#------------------------------------------------------------------------------ #$Date: 2021-07-04 04:32:23 +0300 (Sun, 04 Jul 2021) $ #$Revision: 266957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/88/4518828.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4518828 loop_ _publ_author_name 'Goryunov, Georgy P.' 'Sharikov, Mikhail I.' 'Iashin, Andrei N.' 'Canich, Jo Ann M.' 'Mattler, Sarah J.' 'Hagadorn, John R.' 'Uborsky, Dmitry V.' 'Voskoboynikov, Alexander Z.' _publ_section_title ; Rigid Postmetallocene Catalysts for Propylene Polymerization: Ligand Design Prevents the Temperature-Dependent Loss of Stereo- and Regioselectivities ; _journal_issue 13 _journal_name_full 'ACS Catalysis' _journal_page_first 8079 _journal_page_last 8086 _journal_paper_doi 10.1021/acscatal.1c01611 _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'C55 H61 Hf N O2' _chemical_formula_sum 'C55 H61 Hf N O2' _chemical_formula_weight 946.53 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-02-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 102.4480(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 29.0406(16) _cell_length_b 16.9643(9) _cell_length_c 19.5677(11) _cell_measurement_reflns_used 9918 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.57 _cell_measurement_theta_min 2.30 _cell_volume 9413.5(9) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 120 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 56610 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.997 _diffrn_reflns_theta_min 1.436 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.257 _exptl_absorpt_correction_T_max 0.4330 _exptl_absorpt_correction_T_min 0.3489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0884 before and 0.0412 after correction. The Ratio of minimum to maximum transmission is 0.8150. The \l/2 correction factor is 0.0015.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.336 _exptl_crystal_description prism _exptl_crystal_F_000 3888 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.281 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 532 _refine_ls_number_reflns 12484 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0218 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+17.1659P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.0517 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10986 _reflns_number_total 12484 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c01611_si_002.cif _cod_data_source_block sad _cod_depositor_comments 'Adding full bibliography for 4518828.cif.' _cod_database_code 4518828 _shelxl_version_number 2014/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O1) = Uanis(O2) 3.a Ternary CH refined with riding coordinates: C15(H15), C17(H17), C19(H19), C42(H42), C44(H44), C46(H46) 3.b Secondary CH2 refined with riding coordinates: C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A, H21B), C22(H22A,H22B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B), C55(H55A,H55B) 3.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C8(H8), C9(H9), C11(H11), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C33(H33), C36(H36), C38(H38) 3.d Idealised Me refined as rotating group: C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B, H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C) ; _shelx_res_file ; TITL sad_a.res in C2/c REM Old TITL sad in C2/c REM SHELXT solution in C2/c REM R1 0.063, Rweak 0.002, Alpha 0.022, Orientation as input REM Formula found by SHELXT: C55 N2 O2 Hf CELL 0.71073 29.0406 16.9643 19.5677 90 102.448 90 ZERR 8 0.0016 0.0009 0.0011 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Hf N O UNIT 440 488 8 8 16 EADP O1 O2 L.S. 99 0 0 PLAN 20 TEMP 23 conf BOND $H list 4 ABIN fmap 2 53 acta OMIT -2 58 OMIT 1 1 0 OMIT -4 0 2 OMIT -13 1 9 OMIT -11 3 6 OMIT 11 1 5 OMIT -5 5 6 OMIT 30 0 10 OMIT 9 5 4 OMIT -3 9 1 OMIT 4 8 0 OMIT -3 7 1 OMIT 13 1 1 OMIT -3 7 3 OMIT 16 0 0 OMIT 29 1 2 OMIT 22 4 6 OMIT -2 6 4 OMIT -7 1 7 OMIT -7 3 8 OMIT -10 4 8 OMIT 8 6 3 OMIT -4 0 10 OMIT 22 4 7 OMIT 1 7 0 OMIT 1 7 3 REM REM REM WGHT 0.020000 17.165899 FVAR 0.09302 HF1 3 0.283127 0.635000 0.254529 11.00000 0.01256 0.01312 = 0.01228 -0.00121 0.00259 -0.00198 O1 5 0.216498 0.603010 0.251641 11.00000 0.00880 0.01435 = 0.01370 0.00056 0.00182 -0.00284 O2 5 0.340628 0.700857 0.264086 11.00000 0.00880 0.01435 = 0.01370 0.00056 0.00182 -0.00284 N1 4 0.263378 0.747981 0.309980 11.00000 0.01330 0.01517 = 0.01126 -0.00077 0.00166 -0.00162 C1 1 0.179103 0.617638 0.281872 11.00000 0.01370 0.01620 = 0.01222 0.00199 0.00041 -0.00222 C2 1 0.132369 0.618577 0.242500 11.00000 0.02498 0.01529 = 0.01009 -0.00156 -0.00239 0.00507 C3 1 0.096965 0.639681 0.278134 11.00000 0.01333 0.02098 = 0.01751 0.00022 0.00244 -0.00066 AFIX 43 H3 2 0.066042 0.642583 0.252615 11.00000 -1.20000 AFIX 0 C4 1 0.105615 0.656511 0.349610 11.00000 0.01987 0.02136 = 0.02025 -0.00134 0.00834 -0.00138 C5 1 0.151468 0.648662 0.387624 11.00000 0.02083 0.02255 = 0.01354 -0.00232 0.00455 -0.00380 AFIX 43 H5 2 0.157944 0.656253 0.435820 11.00000 -1.20000 AFIX 0 C6 1 0.188207 0.629486 0.354640 11.00000 0.01467 0.01581 = 0.01463 0.00000 0.00290 -0.00481 C7 1 0.235784 0.613908 0.399936 11.00000 0.01580 0.02115 = 0.01006 -0.00066 0.00272 -0.00192 C8 1 0.243339 0.541327 0.434832 11.00000 0.02246 0.01994 = 0.01587 -0.00133 0.00427 -0.00581 AFIX 43 H8 2 0.220640 0.501996 0.423835 11.00000 -1.20000 AFIX 0 C9 1 0.283785 0.526896 0.485240 11.00000 0.02618 0.01975 = 0.01705 0.00411 0.00560 0.00096 AFIX 43 H9 2 0.288016 0.477865 0.506949 11.00000 -1.20000 AFIX 0 C10 1 0.318353 0.584798 0.504029 11.00000 0.01950 0.02878 = 0.01483 0.00515 0.00200 0.00061 C11 1 0.311971 0.655786 0.468276 11.00000 0.01914 0.02539 = 0.01337 0.00156 0.00257 -0.00485 AFIX 43 H11 2 0.334980 0.694614 0.479342 11.00000 -1.20000 AFIX 0 C12 1 0.271735 0.670623 0.415850 11.00000 0.01642 0.01825 = 0.01089 -0.00046 0.00347 -0.00258 C13 1 0.118825 0.592594 0.165535 11.00000 0.01255 0.02129 = 0.01366 -0.00161 0.00057 0.00078 C14 1 0.064908 0.591701 0.136907 11.00000 0.01557 0.04071 = 0.02104 -0.00701 0.00115 0.00096 AFIX 23 H14A 2 0.050308 0.556086 0.164738 11.00000 -1.20000 H14B 2 0.052273 0.644077 0.140623 11.00000 -1.20000 AFIX 0 C15 1 0.053032 0.565008 0.059783 11.00000 0.01336 0.05846 = 0.02433 -0.01438 -0.00639 0.00427 AFIX 13 H15 2 0.018716 0.564812 0.042884 11.00000 -1.20000 AFIX 0 C16 1 0.071961 0.481826 0.054020 11.00000 0.02371 0.05179 = 0.03069 -0.02017 -0.00119 -0.00786 AFIX 23 H16A 2 0.064066 0.464441 0.005677 11.00000 -1.20000 H16B 2 0.057693 0.445617 0.081772 11.00000 -1.20000 AFIX 0 C17 1 0.125634 0.482205 0.080454 11.00000 0.02163 0.02894 = 0.02152 -0.01108 -0.00151 -0.00129 AFIX 13 H17 2 0.138127 0.429124 0.076528 11.00000 -1.20000 AFIX 0 C18 1 0.147579 0.539939 0.036174 11.00000 0.02236 0.04049 = 0.01735 -0.00648 0.00090 0.00501 AFIX 23 H18A 2 0.181599 0.540055 0.052220 11.00000 -1.20000 H18B 2 0.140214 0.523284 -0.012388 11.00000 -1.20000 AFIX 0 C19 1 0.128379 0.622863 0.042171 11.00000 0.02993 0.03864 = 0.01382 0.00360 0.00418 0.00733 AFIX 13 H19 2 0.142639 0.659409 0.013912 11.00000 -1.20000 AFIX 0 C20 1 0.074907 0.622458 0.015681 11.00000 0.03392 0.06092 = 0.01584 -0.00151 -0.00320 0.02039 AFIX 23 H20A 2 0.067108 0.606491 -0.033052 11.00000 -1.20000 H20B 2 0.062436 0.675002 0.019145 11.00000 -1.20000 AFIX 0 C21 1 0.140304 0.649376 0.119034 11.00000 0.02224 0.02402 = 0.01642 0.00235 0.00381 0.00367 AFIX 23 H21A 2 0.128145 0.702117 0.122641 11.00000 -1.20000 H21B 2 0.174275 0.651013 0.135523 11.00000 -1.20000 AFIX 0 C22 1 0.137506 0.508698 0.157542 11.00000 0.01895 0.01982 = 0.01927 -0.00180 0.00072 -0.00206 AFIX 23 H22A 2 0.171419 0.507756 0.174817 11.00000 -1.20000 H22B 2 0.123545 0.472220 0.185445 11.00000 -1.20000 AFIX 0 C23 1 0.266878 0.748483 0.380011 11.00000 0.01206 0.01829 = 0.01278 -0.00074 0.00181 -0.00247 C24 1 0.267134 0.818560 0.416437 11.00000 0.02332 0.02117 = 0.01247 -0.00417 0.00408 -0.00378 AFIX 43 H24 2 0.269653 0.818148 0.464629 11.00000 -1.20000 AFIX 0 C25 1 0.263596 0.889223 0.380266 11.00000 0.02606 0.01728 = 0.02007 -0.00506 0.00553 -0.00225 AFIX 43 H25 2 0.263759 0.936764 0.403984 11.00000 -1.20000 AFIX 0 C26 1 0.259814 0.888562 0.308545 11.00000 0.01952 0.01581 = 0.01804 -0.00070 0.00203 -0.00112 AFIX 43 H26 2 0.257250 0.935559 0.283539 11.00000 -1.20000 AFIX 0 C27 1 0.259898 0.816860 0.274420 11.00000 0.01067 0.01657 = 0.01289 -0.00024 0.00203 -0.00123 C28 1 0.253462 0.813257 0.196557 11.00000 0.01508 0.01077 = 0.01390 0.00053 0.00180 0.00027 C29 1 0.291692 0.812800 0.163084 11.00000 0.01476 0.01489 = 0.01500 0.00050 0.00208 -0.00052 C30 1 0.280692 0.815822 0.089491 11.00000 0.02108 0.02047 = 0.01411 0.00065 0.00533 -0.00034 AFIX 43 H30 2 0.305024 0.812874 0.065512 11.00000 -1.20000 AFIX 0 C31 1 0.234774 0.823045 0.051714 11.00000 0.02482 0.01756 = 0.01164 0.00085 -0.00040 -0.00194 AFIX 43 H31 2 0.228978 0.825001 0.003112 11.00000 -1.20000 AFIX 0 C32 1 0.197151 0.827432 0.085040 11.00000 0.01934 0.01579 = 0.01817 0.00179 -0.00191 -0.00054 C33 1 0.207357 0.820195 0.157761 11.00000 0.01513 0.01606 = 0.01745 0.00114 0.00276 -0.00075 AFIX 43 H33 2 0.182643 0.819990 0.181096 11.00000 -1.20000 AFIX 0 C34 1 0.364945 0.764294 0.249723 11.00000 0.01509 0.01374 = 0.01437 -0.00065 0.00432 -0.00257 C35 1 0.341984 0.818706 0.199446 11.00000 0.01377 0.01758 = 0.01245 -0.00127 0.00349 -0.00016 C36 1 0.367885 0.880542 0.178292 11.00000 0.01649 0.01730 = 0.01595 0.00229 0.00443 0.00089 AFIX 43 H36 2 0.352678 0.915450 0.144149 11.00000 -1.20000 AFIX 0 C37 1 0.415187 0.890960 0.206688 11.00000 0.01671 0.01609 = 0.01751 -0.00087 0.00617 -0.00038 C38 1 0.436629 0.838330 0.259309 11.00000 0.01272 0.01847 = 0.01705 -0.00101 0.00388 -0.00009 AFIX 43 H38 2 0.468237 0.846127 0.280141 11.00000 -1.20000 AFIX 0 C39 1 0.413281 0.775008 0.282175 11.00000 0.01372 0.01672 = 0.01300 -0.00066 0.00205 -0.00035 C40 1 0.440103 0.719826 0.339262 11.00000 0.01359 0.01906 = 0.01588 0.00327 0.00089 -0.00024 C41 1 0.491754 0.745984 0.366271 11.00000 0.01368 0.02669 = 0.02054 0.00408 0.00134 -0.00161 AFIX 23 H41A 2 0.507745 0.746799 0.327571 11.00000 -1.20000 H41B 2 0.492258 0.799069 0.384836 11.00000 -1.20000 AFIX 0 C42 1 0.518236 0.690522 0.423605 11.00000 0.01516 0.03624 = 0.02319 0.00844 -0.00208 -0.00086 AFIX 13 H42 2 0.550810 0.708848 0.439250 11.00000 -1.20000 AFIX 0 C43 1 0.518361 0.606987 0.395031 11.00000 0.02524 0.03453 = 0.03415 0.01025 0.00039 0.00972 AFIX 23 H43A 2 0.534863 0.572006 0.431385 11.00000 -1.20000 H43B 2 0.534557 0.606062 0.356557 11.00000 -1.20000 AFIX 0 C44 1 0.467395 0.579167 0.369635 11.00000 0.02922 0.02097 = 0.03582 0.00532 -0.00307 0.00388 AFIX 13 H44 2 0.467286 0.525430 0.351220 11.00000 -1.20000 AFIX 0 C45 1 0.442499 0.579955 0.431205 11.00000 0.02782 0.03180 = 0.03325 0.01701 -0.00598 -0.00519 AFIX 23 H45A 2 0.410282 0.561706 0.415690 11.00000 -1.20000 H45B 2 0.458595 0.544671 0.467619 11.00000 -1.20000 AFIX 0 C46 1 0.442635 0.663646 0.460249 11.00000 0.02029 0.04099 = 0.01910 0.00911 0.00069 -0.00416 AFIX 13 H46 2 0.426728 0.663752 0.499622 11.00000 -1.20000 AFIX 0 C47 1 0.493667 0.691413 0.485754 11.00000 0.02125 0.04167 = 0.01994 0.00724 -0.00322 -0.00511 AFIX 23 H47A 2 0.510089 0.656729 0.522420 11.00000 -1.20000 H47B 2 0.494115 0.744315 0.504698 11.00000 -1.20000 AFIX 0 C48 1 0.416330 0.719034 0.402779 11.00000 0.01727 0.02800 = 0.01679 0.00257 0.00364 -0.00193 AFIX 23 H48A 2 0.416161 0.771994 0.421411 11.00000 -1.20000 H48B 2 0.383877 0.701753 0.387832 11.00000 -1.20000 AFIX 0 C49 1 0.065907 0.678290 0.384724 11.00000 0.02240 0.03875 = 0.02501 -0.00417 0.00978 0.00186 AFIX 137 H49A 2 0.054107 0.729571 0.369203 11.00000 -1.50000 H49B 2 0.077365 0.678909 0.434551 11.00000 -1.50000 H49C 2 0.041004 0.640238 0.372742 11.00000 -1.50000 AFIX 0 C50 1 0.147823 0.843745 0.044289 11.00000 0.02036 0.03461 = 0.02272 0.00618 -0.00408 0.00242 AFIX 137 H50A 2 0.140695 0.898622 0.048077 11.00000 -1.50000 H50B 2 0.125797 0.812532 0.062850 11.00000 -1.50000 H50C 2 0.145560 0.830472 -0.004014 11.00000 -1.50000 AFIX 0 C51 1 0.278901 0.608466 0.142510 11.00000 0.02660 0.02313 = 0.01949 -0.00391 0.00788 -0.00509 AFIX 137 H51A 2 0.272454 0.553387 0.134163 11.00000 -1.50000 H51B 2 0.308342 0.621471 0.130497 11.00000 -1.50000 H51C 2 0.254075 0.639040 0.114322 11.00000 -1.50000 AFIX 0 C52 1 0.318613 0.530827 0.309403 11.00000 0.02176 0.01848 = 0.02572 0.00230 0.00352 -0.00013 AFIX 137 H52A 2 0.334709 0.545535 0.355786 11.00000 -1.50000 H52B 2 0.340985 0.510593 0.284186 11.00000 -1.50000 H52C 2 0.295597 0.490994 0.312131 11.00000 -1.50000 AFIX 0 C53 1 0.442915 0.956625 0.182254 11.00000 0.01743 0.01830 = 0.02471 0.00373 0.00568 -0.00289 AFIX 137 H53A 2 0.467414 0.934487 0.162200 11.00000 -1.50000 H53B 2 0.456703 0.989348 0.221346 11.00000 -1.50000 H53C 2 0.422240 0.987752 0.147695 11.00000 -1.50000 AFIX 0 C54 1 0.360847 0.569574 0.562563 11.00000 0.02671 0.04516 = 0.02641 0.01631 -0.00540 -0.00659 AFIX 137 H54A 2 0.384379 0.541686 0.544413 11.00000 -1.50000 H54B 2 0.351544 0.538488 0.598301 11.00000 -1.50000 H54C 2 0.373563 0.618895 0.582090 11.00000 -1.50000 AFIX 0 C55 1 0.441264 0.634526 0.311410 11.00000 0.02164 0.01913 = 0.02197 0.00026 0.00074 0.00255 AFIX 23 H55A 2 0.409274 0.615782 0.294550 11.00000 -1.20000 H55B 2 0.457051 0.634040 0.272487 11.00000 -1.20000 AFIX 0 HKLF 4 REM sad_a.res in C2/c REM R1 = 0.0218 for 10986 Fo > 4sig(Fo) and 0.0270 for all 12484 data REM 532 parameters refined using 0 restraints END WGHT 0.0200 17.1550 REM Highest difference peak 1.281, deepest hole -0.887, 1-sigma level 0.076 Q1 1 0.1589 0.6383 0.2413 11.00000 0.05 1.28 Q2 1 0.2242 0.6339 0.2549 11.00000 0.05 0.63 Q3 1 0.1213 0.6411 0.2461 11.00000 0.05 0.61 Q4 1 0.1431 0.5973 0.2604 11.00000 0.05 0.52 Q5 1 0.3156 0.7023 0.2513 11.00000 0.05 0.44 Q6 1 0.3645 0.7080 0.2600 11.00000 0.05 0.43 Q7 1 0.1208 0.6059 0.2065 11.00000 0.05 0.41 Q8 1 0.1835 0.6333 0.3185 11.00000 0.05 0.39 Q9 1 0.2554 0.8163 0.2362 11.00000 0.05 0.37 Q10 1 0.4226 0.7206 0.3623 11.00000 0.05 0.36 Q11 1 0.2998 0.5602 0.4994 11.00000 0.05 0.36 Q12 1 0.2377 0.5800 0.4167 11.00000 0.05 0.35 Q13 1 0.3615 0.8412 0.1834 11.00000 0.05 0.34 Q14 1 0.0192 0.6404 0.2231 11.00000 0.05 0.34 Q15 1 0.2689 0.7820 0.3963 11.00000 0.05 0.34 Q16 1 0.2591 0.8481 0.2978 11.00000 0.05 0.34 Q17 1 0.3179 0.6147 0.4790 11.00000 0.05 0.34 Q18 1 0.2835 0.8062 0.1212 11.00000 0.05 0.33 Q19 1 0.4201 0.8521 0.2299 11.00000 0.05 0.33 Q20 1 0.4212 0.8724 0.2375 11.00000 0.05 0.32 ; _shelx_res_checksum 93908 _shelx_hkl_file ; 2 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93.89 5.50 18 -6 0 99.09 5.80 -18 -6 0 96.39 4.80 18 6 0 86.09 5.90 -18 6 0 94.39 6.10 20 -6 0 0.90 1.00 -20 -6 0 1.20 1.30 20 -6 0 0.80 1.70 -20 -6 0 2.20 1.90 -20 6 0 -0.10 1.40 20 6 0 -1.50 1.70 22 -6 0 22.10 2.20 22 -6 0 15.10 3.50 -22 -6 0 17.30 3.30 -22 -6 0 18.40 2.40 22 6 0 15.60 3.60 -22 6 0 21.00 3.90 -24 -6 0 3.00 2.10 24 -6 0 0.00 1.90 -24 6 0 2.80 2.40 24 6 0 1.90 2.90 -26 -6 0 8.70 3.20 26 -6 0 11.00 3.50 -26 6 0 14.20 3.70 26 6 0 19.80 4.70 28 -6 0 73.59 7.40 -28 -6 0 73.89 7.10 -28 6 0 78.39 7.90 28 6 0 83.49 8.20 30 -6 0 45.50 6.60 -30 -6 0 37.80 5.60 -30 6 0 43.10 6.10 30 6 0 34.60 6.20 32 -6 0 72.79 8.30 -32 -6 0 77.39 7.90 -32 6 0 81.89 8.90 32 6 0 89.39 9.70 -34 -6 0 67.69 8.00 34 -6 0 52.49 7.10 34 6 0 57.99 8.00 -34 6 0 45.40 6.80 -36 -6 0 -1.50 3.10 36 -6 0 -2.00 2.90 36 6 0 -4.70 3.50 -36 6 0 -2.00 2.70 -38 -6 0 -5.70 2.60 38 -6 0 0.50 4.00 38 6 0 2.70 4.10 -38 6 0 7.60 3.70 1 -7 0 31.10 2.70 -1 -7 0 35.80 2.90 1 7 0 36.10 1.50 -1 7 0 34.10 1.60 1 7 0 38.50 2.60 1 7 0 36.10 1.40 -1 7 0 34.60 2.40 3 -7 0 170.88 6.40 -3 -7 0 172.38 6.60 -3 7 0 165.98 5.00 3 7 0 163.28 5.90 3 7 0 167.78 4.30 -3 7 0 168.38 5.90 3 7 0 167.48 4.30 -5 -7 0 1659.43 35.00 5 -7 0 1638.54 38.20 -5 -7 0 1659.63 38.90 -5 7 0 1644.24 37.00 5 7 0 1654.93 37.30 -5 7 0 1642.24 36.20 -7 -7 0 2593.24 58.59 -7 -7 0 2538.05 54.29 7 -7 0 2545.65 57.69 7 7 0 2599.44 56.79 -7 7 0 2598.84 55.99 -7 7 0 2584.64 56.49 9 -7 0 1522.75 35.50 -9 -7 0 1482.95 36.40 -9 -7 0 1525.15 33.40 -9 7 0 1531.15 35.10 9 7 0 1572.94 35.70 -9 7 0 1522.85 35.20 11 -7 0 843.62 20.70 -11 -7 0 807.02 21.60 -11 -7 0 845.82 19.80 -11 7 0 829.52 21.50 11 7 0 812.52 21.40 -11 7 0 829.52 21.10 13 -7 0 127.29 5.20 -13 -7 0 125.69 5.20 -13 -7 0 125.39 5.90 -13 7 0 120.99 5.70 -13 7 0 124.19 6.30 13 7 0 108.29 5.90 -15 -7 0 4.70 1.60 -15 -7 0 3.40 1.60 15 -7 0 4.90 1.50 -15 7 0 1.90 1.70 -15 7 0 3.70 1.80 15 7 0 -0.60 1.70 17 -7 0 109.89 4.80 -17 -7 0 113.09 5.60 17 -7 0 108.49 6.00 -17 -7 0 101.19 5.40 17 7 0 104.29 6.30 -17 7 0 102.19 6.30 -19 -7 0 608.04 17.90 -19 -7 0 655.93 17.50 19 -7 0 590.94 18.50 19 -7 0 623.24 16.20 19 7 0 600.84 19.20 -19 7 0 643.74 19.50 -21 -7 0 700.63 20.40 -21 -7 0 709.53 19.10 21 -7 0 700.63 21.00 21 -7 0 699.93 17.90 -21 7 0 682.43 21.50 21 7 0 705.83 21.80 -23 -7 0 595.64 18.70 -23 -7 0 603.44 16.70 23 -7 0 581.64 19.20 -23 7 0 602.04 19.90 23 7 0 589.54 20.00 25 -7 0 358.76 14.60 -25 -7 0 376.06 14.10 -25 7 0 390.16 15.30 25 7 0 374.26 15.40 -27 -7 0 169.58 9.50 27 -7 0 152.18 9.50 -27 7 0 188.08 10.40 27 7 0 185.38 10.70 -29 -7 0 85.09 7.10 29 -7 0 63.19 7.20 -29 7 0 85.29 8.40 29 7 0 72.79 8.10 -31 -7 0 26.40 5.00 31 -7 0 27.70 5.60 31 7 0 38.90 6.40 -31 7 0 29.50 5.30 -33 -7 0 140.59 9.70 33 -7 0 132.09 9.60 -33 7 0 123.79 9.40 33 7 0 123.89 10.30 -35 -7 0 120.59 9.30 35 -7 0 108.99 10.50 -35 7 0 113.59 10.90 35 7 0 105.89 10.50 37 -7 0 204.98 13.20 -37 -7 0 230.08 12.80 -37 7 0 241.18 13.70 37 7 0 235.08 14.70 0 -8 0 1675.93 38.80 0 8 0 1616.34 36.80 0 8 0 1591.04 34.40 2 -8 0 874.51 22.00 -2 -8 0 832.52 22.10 2 8 0 874.31 18.30 -2 8 0 818.82 20.60 2 8 0 849.41 18.30 2 8 0 849.41 20.80 -2 8 0 843.52 19.00 -4 -8 0 99.99 5.20 4 -8 0 102.39 5.10 -4 8 0 101.69 3.90 4 8 0 95.99 3.00 4 8 0 105.99 4.80 -4 8 0 98.09 4.50 6 -8 0 218.68 7.90 -6 -8 0 216.68 8.30 -6 -8 0 224.68 5.80 -6 8 0 213.88 7.00 6 8 0 208.68 7.50 -6 8 0 207.28 7.30 8 -8 0 30.10 3.00 -8 -8 0 31.40 3.60 -8 -8 0 31.60 1.90 -8 8 0 27.90 2.80 -8 8 0 33.40 2.70 8 8 0 31.20 3.20 -10 -8 0 462.15 14.30 10 -8 0 446.36 13.20 -10 -8 0 474.05 11.80 10 8 0 456.75 13.70 -10 8 0 471.45 13.40 -10 8 0 477.05 13.70 12 -8 0 652.63 17.60 -12 -8 0 666.63 18.80 -12 -8 0 685.33 16.60 -12 8 0 673.83 18.10 -12 8 0 645.84 18.40 12 8 0 670.13 18.50 14 -8 0 909.31 22.60 -14 -8 0 886.81 23.80 -14 -8 0 880.91 22.00 -14 8 0 933.31 24.20 -14 8 0 921.61 23.50 14 8 0 867.91 23.80 16 -8 0 520.95 14.70 -16 -8 0 513.55 15.70 -16 -8 0 544.55 15.10 16 8 0 523.25 16.50 -16 8 0 559.64 17.00 -16 8 0 520.05 15.90 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170.78 6.80 4 -10 0 78.49 5.00 -4 -10 0 92.89 5.50 -4 10 0 87.09 3.80 -4 10 0 83.39 4.60 4 10 0 84.69 4.70 4 10 0 85.19 2.70 6 -10 0 34.10 3.60 -6 -10 0 35.00 4.10 6 10 0 32.20 1.70 6 10 0 25.60 3.10 -6 10 0 35.00 2.60 -6 10 0 31.30 3.20 8 -10 0 15.50 2.60 -8 -10 0 14.70 1.50 -8 -10 0 14.60 2.80 -8 10 0 12.90 2.10 -8 10 0 11.50 2.10 8 10 0 15.90 2.60 -10 -10 0 16.60 1.70 10 -10 0 14.50 2.50 -10 -10 0 20.10 3.20 -10 10 0 18.90 2.90 -10 10 0 12.60 2.20 10 10 0 16.10 2.80 -12 -10 0 200.88 9.00 -12 -10 0 210.28 6.70 12 -10 0 214.18 8.30 12 10 0 218.38 8.90 -12 10 0 221.58 8.70 -12 10 0 206.08 8.50 -14 -10 0 187.78 6.70 14 -10 0 184.58 7.70 -14 -10 0 197.28 8.80 -14 10 0 193.68 8.20 14 10 0 190.08 8.70 -14 10 0 194.58 8.60 -16 -10 0 232.18 8.10 -16 -10 0 225.58 9.60 16 -10 0 233.48 8.80 -16 10 0 214.18 9.60 16 10 0 217.98 9.90 -16 10 0 232.58 9.50 -18 -10 0 150.58 7.70 18 -10 0 150.48 6.90 -18 -10 0 160.28 6.90 18 10 0 153.18 8.50 -18 10 0 161.18 8.10 -18 10 0 181.38 8.80 20 -10 0 3.00 2.50 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11 0 311.77 7.50 -3 11 0 304.57 10.30 -5 -11 0 762.02 21.80 5 -11 0 751.22 21.10 -5 11 0 747.73 18.30 5 11 0 730.03 20.00 5 11 0 742.13 16.50 -5 11 0 761.42 20.00 -7 -11 0 1641.64 41.20 7 -11 0 1593.64 40.20 -7 11 0 1640.54 37.60 7 11 0 1671.73 39.20 -7 11 0 1664.53 38.90 7 11 0 1670.13 35.20 -9 -11 0 1022.70 22.80 -9 -11 0 1007.70 27.70 9 -11 0 987.30 26.60 -9 11 0 1025.40 25.30 -9 11 0 1024.70 25.90 9 11 0 1024.50 26.20 -11 -11 0 701.43 21.60 11 -11 0 751.72 20.80 -11 -11 0 756.92 17.60 -11 11 0 737.53 20.20 11 11 0 752.82 20.90 -11 11 0 753.02 20.40 -13 -11 0 275.37 11.20 -13 -11 0 264.67 8.10 13 -11 0 276.57 10.20 13 11 0 272.87 10.70 -13 11 0 256.77 10.00 -13 11 0 274.17 10.40 -15 -11 0 1.10 1.20 -15 -11 0 0.10 1.50 15 -11 0 1.50 1.70 -15 11 0 0.80 1.50 15 11 0 2.80 2.10 -15 11 0 0.70 2.00 -17 -11 0 33.80 4.40 17 -11 0 36.90 4.00 -17 -11 0 40.00 3.70 -17 11 0 32.40 4.20 -17 11 0 37.50 4.60 17 11 0 37.20 4.80 19 -11 0 454.55 14.20 -19 -11 0 437.46 15.30 -19 -11 0 450.35 13.70 -19 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5.80 20 -12 0 97.19 6.00 20 12 0 103.39 7.50 -20 12 0 110.89 7.50 -20 12 0 99.19 6.80 22 -12 0 3.00 2.30 -22 -12 0 3.70 2.10 -22 -12 0 2.50 2.10 22 -12 0 5.70 2.80 -22 12 0 4.70 2.70 22 12 0 5.50 3.30 24 -12 0 91.19 7.40 -24 -12 0 99.89 6.30 -24 -12 0 93.39 6.50 -24 12 0 100.19 7.40 24 12 0 81.79 8.30 -26 -12 0 192.48 9.40 26 -12 0 185.58 10.80 26 12 0 190.68 11.80 -26 12 0 201.38 10.90 28 -12 0 135.99 9.60 -28 12 0 143.19 9.40 28 12 0 129.39 10.10 30 -12 0 333.17 15.60 -30 12 0 285.17 14.20 30 12 0 295.97 15.80 32 -12 0 180.08 11.70 32 12 0 192.18 12.80 -32 12 0 196.58 11.70 34 -12 0 87.59 9.60 34 12 0 93.29 10.00 -34 12 0 88.69 9.40 -1 -13 0 1.60 1.90 1 -13 0 1.10 1.80 -1 13 0 6.60 2.10 1 13 0 3.70 2.10 1 13 0 6.50 0.90 -1 13 0 5.00 1.00 -3 -13 0 13.30 3.10 3 -13 0 19.10 3.40 3 13 0 11.60 2.50 -3 13 0 19.70 2.00 -3 13 0 13.90 2.70 5 -13 0 23.40 3.70 -5 -13 0 17.70 3.50 -5 13 0 29.80 3.60 5 13 0 21.30 3.20 -5 13 0 25.00 2.60 7 -13 0 85.99 6.00 -7 -13 0 74.39 5.90 -7 13 0 82.49 5.40 -7 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278.87 9.70 -4 -10 -4 158.58 7.90 4 -10 4 160.28 7.50 -4 10 -4 162.78 6.20 -4 10 -4 165.68 6.30 4 10 4 168.38 7.20 -6 -10 -4 69.79 5.30 6 -10 4 80.29 5.20 -6 10 -4 80.09 4.30 6 10 4 91.79 5.30 -6 10 -4 88.49 4.60 8 -10 4 60.89 4.70 -8 -10 -4 62.59 4.90 -8 -10 -4 55.49 2.20 8 10 4 59.39 4.40 -8 10 -4 61.99 3.90 -8 10 -4 55.99 3.90 10 -10 4 96.79 5.70 -10 -10 -4 86.49 6.00 -10 -10 -4 96.89 3.70 -10 10 -4 98.29 5.10 10 10 4 95.09 5.80 -10 10 -4 95.49 5.40 12 -10 4 467.35 14.80 -12 -10 -4 463.95 12.30 -12 -10 -4 465.85 15.90 -12 10 -4 472.55 14.00 12 10 4 460.25 15.00 -12 10 -4 465.15 14.70 14 -10 4 405.66 13.30 -14 -10 -4 383.26 14.10 -14 -10 -4 390.76 11.40 14 10 4 363.76 13.40 -14 10 -4 382.16 13.50 -14 10 -4 398.06 12.80 16 -10 4 189.58 8.40 -16 -10 -4 197.08 7.50 16 -10 4 192.98 8.50 -16 -10 -4 203.78 9.50 16 10 4 175.88 9.00 -16 10 -4 194.48 9.30 18 -10 4 131.89 7.10 18 -10 4 124.09 6.80 -18 -10 -4 128.79 6.40 -18 -10 -4 122.39 7.20 18 10 4 115.99 7.50 -18 10 -4 135.69 7.90 -20 -10 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3.80 -29 -11 4 25.70 4.70 29 -11 -4 28.00 5.50 29 11 -4 16.70 4.80 -29 11 4 21.70 4.60 -27 -11 4 292.97 12.40 27 -11 -4 275.67 13.50 -27 11 4 301.47 13.40 27 11 -4 289.77 14.20 -25 -11 4 317.87 12.40 25 -11 -4 292.17 13.50 25 11 -4 289.87 13.70 -25 11 4 307.87 13.10 -23 -11 4 190.38 8.70 -23 -11 4 184.78 8.70 23 -11 -4 185.28 10.00 -23 11 4 176.38 9.40 23 11 -4 171.78 10.00 -21 -11 4 476.35 16.10 21 -11 -4 470.55 14.70 -21 -11 4 487.45 15.40 -21 11 4 534.85 17.80 -21 11 4 516.25 17.00 21 11 -4 502.85 17.70 -19 -11 4 198.38 9.00 -19 -11 4 191.78 8.00 19 -11 -4 183.48 7.80 19 11 -4 170.08 9.00 -19 11 4 199.88 9.60 -19 11 4 171.38 8.50 17 -11 -4 101.69 5.70 -17 -11 4 100.69 6.30 -17 -11 4 105.59 5.50 -17 11 4 106.09 6.70 -17 11 4 98.69 6.00 17 11 -4 92.89 6.40 -15 -11 4 1.70 1.40 15 -11 -4 2.70 1.80 -15 -11 4 1.10 1.50 -15 11 4 4.50 2.50 15 11 -4 1.10 1.80 -15 11 4 3.50 1.50 -13 -11 4 327.27 12.40 -13 -11 4 325.87 10.20 13 -11 -4 335.17 11.60 -13 11 4 339.27 12.20 13 11 -4 335.37 11.80 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1487.25 37.20 -5 11 -4 1485.25 34.20 -5 11 -4 1469.65 34.60 5 11 4 1483.45 36.00 7 -11 4 940.21 25.20 -7 -11 -4 877.21 25.90 -7 11 -4 894.81 22.90 7 11 4 925.71 24.30 -7 11 -4 930.71 23.10 -9 -11 -4 814.12 17.90 9 -11 4 844.62 23.10 -9 -11 -4 782.32 23.80 9 11 4 842.82 22.60 -9 11 -4 790.32 21.40 -9 11 -4 809.32 21.10 11 -11 4 507.15 15.90 -11 -11 -4 492.05 12.00 -11 -11 -4 450.15 16.40 -11 11 -4 470.25 14.40 -11 11 -4 483.85 15.00 11 11 4 504.55 15.70 13 -11 4 3.00 1.90 -13 -11 -4 6.20 2.30 -13 -11 -4 3.90 1.20 -13 11 -4 0.90 1.50 -13 11 -4 6.60 2.20 13 11 4 4.50 2.40 15 -11 4 41.30 4.60 -15 -11 -4 32.00 4.60 -15 -11 -4 39.70 3.10 15 11 4 32.40 4.40 -15 11 -4 33.80 4.00 -15 11 -4 31.20 4.40 -17 -11 -4 256.47 11.10 17 -11 4 229.98 9.80 -17 -11 -4 216.18 8.40 17 -11 4 253.07 10.20 -17 11 -4 233.28 10.60 17 11 4 221.08 10.50 19 -11 4 633.44 19.40 -19 -11 -4 645.64 18.30 -19 -11 -4 679.53 21.00 19 -11 4 632.84 19.80 19 11 4 673.43 21.40 -19 11 -4 633.14 20.90 -21 -11 -4 577.44 19.10 -21 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10.80 -35 1 -5 158.88 11.50 37 -1 5 198.28 12.40 -37 -1 -5 190.08 12.30 -37 1 -5 185.48 12.40 37 1 5 196.38 12.40 40 -2 -5 23.80 5.90 -40 -2 5 32.70 6.80 40 2 -5 29.80 6.60 -40 2 5 29.60 5.90 38 -2 -5 8.60 4.40 -38 -2 5 13.40 5.10 38 2 -5 17.40 5.60 -38 2 5 18.60 5.10 -36 -2 5 92.99 9.50 36 -2 -5 74.79 8.60 36 2 -5 100.59 10.10 -36 2 5 91.49 9.60 -34 -2 5 363.66 16.40 34 -2 -5 361.66 16.60 34 2 -5 392.36 17.50 -34 2 5 376.56 16.60 -32 -2 5 497.45 19.20 32 -2 -5 526.05 20.00 32 2 -5 497.95 19.80 -32 2 5 513.95 19.50 30 -2 -5 488.25 18.70 -30 -2 5 462.35 18.10 -30 2 5 528.65 19.00 30 2 -5 498.65 19.00 28 -2 -5 247.48 12.20 -28 -2 5 265.67 12.20 28 2 -5 240.98 12.20 -28 2 5 268.87 12.40 26 -2 -5 579.94 19.90 -26 -2 5 599.34 19.80 -26 2 5 584.84 19.80 26 2 -5 633.14 20.80 24 -2 -5 227.18 11.00 -24 -2 5 250.77 11.00 -24 2 5 263.77 11.30 24 2 -5 253.07 11.50 -22 -2 5 30.10 4.20 22 -2 -5 34.70 4.60 22 2 -5 48.50 5.60 -22 2 5 35.30 4.50 -20 -2 5 504.15 15.90 20 -2 -5 529.65 16.80 -20 2 5 473.45 15.80 20 2 -5 529.65 16.90 -18 -2 5 630.64 14.90 18 -2 -5 619.44 18.70 -18 -2 5 661.43 18.60 18 2 -5 641.34 19.10 -18 2 5 672.03 18.80 18 2 -5 673.23 15.10 16 -2 -5 1875.81 44.00 -16 -2 5 1858.51 43.20 16 -2 -5 1916.71 40.20 -16 -2 5 1867.31 41.10 16 -2 -5 1897.91 40.20 -16 2 5 1814.82 43.30 16 2 -5 1887.31 44.40 -14 -2 5 1756.02 40.30 14 -2 -5 1750.62 38.20 14 -2 -5 1769.22 40.90 -14 -2 5 1785.92 38.90 -14 2 5 1769.72 40.40 14 2 -5 1732.23 41.30 -12 -2 5 721.53 16.90 12 -2 -5 706.03 18.30 -12 -2 5 701.83 17.80 12 2 -5 681.33 18.50 -12 2 5 718.43 18.10 -10 -2 5 442.36 12.00 10 -2 -5 449.76 12.30 -10 -2 5 453.25 11.60 -10 2 5 455.25 12.10 10 2 -5 448.16 12.60 -10 2 5 457.25 11.30 -8 -2 5 34.90 2.30 -8 -2 5 28.80 2.20 -8 2 5 34.30 2.20 -8 2 5 29.90 2.20 8 2 -5 30.10 2.30 -8 2 5 32.60 2.10 -6 -2 5 474.25 11.90 -6 -2 5 462.45 12.20 -6 2 5 463.35 11.50 6 2 -5 472.85 11.70 -6 2 5 463.35 11.70 -6 2 5 478.85 12.20 -4 -2 5 1941.01 41.10 -4 -2 5 1859.01 42.40 -4 2 5 1837.22 40.80 4 2 -5 1918.11 40.40 -4 2 5 1909.01 42.60 -4 2 5 1912.71 40.50 -2 -2 5 4437.86 100.19 -2 -2 5 4822.52 103.49 2 2 -5 4864.41 100.59 -2 2 5 4722.53 103.69 -2 2 5 5042.90 99.69 2 2 -5 4817.02 99.99 -2 2 5 4824.42 100.29 0 -2 -5 1746.13 37.30 0 -2 5 1738.33 39.70 0 2 -5 1768.72 37.90 0 2 5 1685.33 39.90 0 2 5 1821.12 37.70 2 -2 5 855.51 18.10 -2 -2 -5 859.41 19.10 2 -2 5 840.72 18.00 2 -2 5 862.61 20.80 2 2 5 803.72 21.00 2 2 5 881.21 19.20 -2 2 -5 850.31 19.60 4 -2 5 849.61 18.60 4 -2 5 841.92 20.90 -4 -2 -5 841.62 19.30 4 -2 5 844.02 18.80 -4 2 -5 880.51 20.00 4 2 5 831.02 21.20 4 2 5 844.12 19.30 -6 -2 -5 10.20 1.60 6 -2 5 14.40 1.70 6 -2 5 11.00 1.90 -6 2 -5 9.60 1.70 6 2 5 8.10 1.80 6 2 5 12.60 1.70 -8 -2 -5 38.40 2.60 8 -2 5 38.70 2.50 8 -2 5 43.60 3.00 -8 2 -5 39.60 2.90 8 2 5 42.70 2.70 8 2 5 40.70 3.00 -10 -2 -5 541.95 14.80 10 -2 5 565.14 14.70 10 -2 5 575.04 15.30 -10 2 -5 522.65 15.00 10 2 5 562.94 15.40 10 2 5 572.94 14.80 12 -2 5 1497.75 35.50 12 -2 5 1532.95 35.20 -12 -2 -5 1501.75 35.30 -12 2 -5 1496.85 35.60 12 2 5 1499.25 35.70 12 2 5 1507.95 35.20 -14 -2 -5 1424.76 35.00 14 -2 5 1504.55 34.90 14 -2 5 1528.65 34.80 -14 2 -5 1389.06 35.30 14 2 5 1468.85 34.90 14 2 5 1437.56 34.90 16 -2 5 926.31 22.80 16 -2 5 866.11 23.30 -16 -2 -5 904.41 24.00 16 2 5 872.01 23.50 16 2 5 885.61 22.80 -16 2 -5 850.81 24.00 18 -2 5 1069.09 26.10 -18 -2 -5 1011.50 27.70 18 -2 5 1032.70 27.20 18 2 5 1064.79 27.70 -18 2 -5 1008.60 27.90 18 2 5 1044.20 26.10 20 -2 5 59.59 3.90 20 -2 5 49.99 4.90 -20 -2 -5 50.49 5.40 20 2 5 54.09 5.30 -20 2 -5 51.99 5.60 20 2 5 52.79 3.80 -22 -2 -5 11.40 3.10 22 -2 5 18.20 2.60 22 -2 5 17.90 3.30 -22 2 -5 22.90 4.10 22 2 5 22.30 3.80 22 2 5 21.50 2.80 24 -2 5 199.48 9.70 -24 -2 -5 173.88 9.60 -24 2 -5 196.58 10.50 24 2 5 184.38 9.80 -26 -2 -5 427.46 16.40 26 -2 5 437.16 16.20 26 2 5 427.06 16.40 -26 2 -5 409.26 16.60 28 -2 5 421.86 16.10 -28 -2 -5 381.96 15.90 -28 2 -5 382.96 16.60 28 2 5 387.66 15.90 30 -2 5 618.74 21.50 -30 -2 -5 588.24 21.50 30 2 5 638.84 22.20 -30 2 -5 626.44 22.60 32 -2 5 241.28 12.70 -32 -2 -5 236.88 13.00 32 2 5 255.67 13.30 -32 2 -5 260.37 13.80 -34 -2 -5 129.09 9.70 34 -2 5 135.09 9.80 34 2 5 123.99 9.80 -34 2 -5 134.39 10.20 36 -2 5 -1.00 3.70 -36 -2 -5 2.40 3.40 -36 2 -5 3.20 3.60 36 2 5 -0.90 3.10 38 -2 5 54.29 7.50 -38 -2 -5 43.50 7.30 38 2 5 50.29 7.50 -38 2 -5 48.20 7.80 -41 -3 5 36.00 7.00 41 -3 -5 29.10 6.30 41 3 -5 36.90 7.10 -41 3 5 28.50 6.30 39 -3 -5 52.89 8.00 -39 -3 5 63.39 8.30 -39 3 5 59.29 8.30 39 3 -5 63.59 8.50 -37 -3 5 37.90 6.50 37 -3 -5 45.30 7.30 -37 3 5 32.50 6.00 37 3 -5 30.70 6.30 -35 -3 5 50.39 7.10 35 -3 -5 38.80 6.70 35 3 -5 42.80 7.40 -35 3 5 50.89 7.00 33 -3 -5 24.90 5.30 -33 -3 5 23.70 5.00 33 3 -5 14.70 4.70 -33 3 5 15.40 4.50 31 -3 -5 2.00 3.00 -31 -3 5 0.60 2.60 31 3 -5 -2.70 3.00 -31 3 5 -2.90 2.50 29 -3 -5 71.49 7.30 -29 -3 5 71.49 7.30 29 3 -5 82.19 8.10 -29 3 5 72.59 7.50 -27 -3 5 250.77 11.70 27 -3 -5 264.57 12.30 27 3 -5 265.07 12.50 -27 3 5 237.18 11.60 -25 -3 5 130.09 7.90 25 -3 -5 116.89 7.90 -25 3 5 118.79 7.70 25 3 -5 133.99 8.40 -23 -3 5 67.59 5.40 23 -3 -5 64.89 6.30 -23 3 5 64.29 6.30 23 3 -5 53.89 5.90 21 -3 -5 280.37 11.30 -21 -3 5 258.57 10.60 -21 -3 5 277.07 7.00 -21 3 5 259.37 10.80 21 3 -5 277.17 11.60 -19 -3 5 136.69 4.50 19 -3 -5 151.98 7.50 -19 -3 5 144.69 7.10 19 3 -5 141.09 7.70 -19 3 5 148.69 7.30 -17 -3 5 7.10 1.90 17 -3 -5 5.70 2.00 17 -3 -5 9.50 1.00 -17 -3 5 7.90 1.20 17 -3 -5 8.40 0.80 17 3 -5 10.40 2.60 -17 3 5 11.50 2.30 -15 -3 5 12.20 1.50 -15 -3 5 8.10 1.90 15 -3 -5 9.60 1.10 15 -3 -5 11.80 2.30 15 3 -5 11.40 2.60 -15 3 5 6.00 1.90 13 -3 -5 4.60 1.60 13 -3 -5 7.20 1.00 -13 -3 5 9.90 1.80 -13 -3 5 11.10 1.50 -13 3 5 7.20 1.50 13 3 -5 4.30 1.60 -11 -3 5 103.09 4.50 11 -3 -5 101.79 3.80 -11 -3 5 109.09 4.20 -11 3 5 105.39 4.70 -11 3 5 105.59 4.60 11 3 -5 93.69 4.70 -9 -3 5 852.91 20.60 -9 -3 5 852.81 20.80 -9 3 5 900.01 20.70 -9 3 5 859.61 20.90 9 3 -5 891.51 21.10 -9 3 5 874.21 20.50 -7 -3 5 1887.11 40.60 -7 -3 5 1843.82 41.80 -7 3 5 1805.12 40.80 -7 3 5 1881.11 40.20 -7 3 5 1891.01 41.70 7 3 -5 1838.32 40.70 -5 -3 5 290.47 8.60 -5 -3 5 291.07 8.10 -5 3 5 283.77 7.50 -5 3 5 296.27 8.70 5 3 -5 284.77 7.50 -5 3 5 291.87 8.00 -3 -3 5 147.49 5.40 3 3 -5 149.49 4.80 3 3 -5 144.49 4.00 -3 3 5 149.59 4.40 -3 3 5 145.39 5.50 -3 3 5 139.79 4.70 -1 -3 5 46.10 2.90 1 -3 -5 43.80 1.90 -1 -3 5 47.90 1.60 1 3 -5 49.10 2.50 -1 3 5 43.70 3.00 -1 3 5 50.09 2.30 1 3 -5 49.30 1.60 1 -3 5 32.80 2.40 1 -3 5 33.50 1.20 -1 -3 -5 36.30 1.80 1 3 5 31.10 2.00 -1 3 -5 32.90 1.20 1 3 5 31.90 2.60 -1 3 -5 32.90 2.10 3 -3 5 114.29 3.10 3 -3 5 117.49 3.30 3 -3 5 115.79 4.80 -3 -3 -5 111.79 3.70 3 3 5 114.09 4.10 3 3 5 112.49 5.00 -3 3 -5 111.79 4.30 5 -3 5 388.26 11.30 5 -3 5 402.46 9.70 -5 -3 -5 382.46 10.00 5 3 5 398.76 10.40 5 3 5 378.26 11.60 -5 3 -5 412.26 10.90 7 -3 5 423.36 12.00 -7 -3 -5 408.66 11.00 7 -3 5 424.16 10.90 -7 3 -5 427.96 11.80 7 3 5 423.76 12.50 7 3 5 417.36 11.30 9 -3 5 85.89 4.10 9 -3 5 102.29 4.70 -9 -3 -5 90.19 4.20 9 3 5 97.59 4.80 9 3 5 89.39 4.20 -9 3 -5 95.29 4.60 11 -3 5 2.00 1.10 -11 -3 -5 4.70 1.60 11 -3 5 2.00 1.10 -11 3 -5 2.10 1.40 11 3 5 3.40 1.50 11 3 5 3.20 1.50 13 -3 5 51.89 3.50 13 -3 5 53.49 3.80 -13 -3 -5 50.19 3.80 13 3 5 44.10 3.50 -13 3 -5 52.59 4.00 13 3 5 49.50 3.80 15 -3 5 7.60 1.90 -15 -3 -5 7.00 2.20 15 -3 5 8.60 2.20 -15 3 -5 7.20 2.10 15 3 5 9.80 2.40 15 3 5 8.30 2.00 17 -3 5 11.00 2.40 -17 -3 -5 6.50 2.20 17 -3 5 12.60 2.30 17 3 5 10.30 2.70 17 3 5 8.20 2.00 -17 3 -5 8.10 2.50 19 -3 5 368.16 13.10 19 -3 5 378.46 11.80 -19 -3 -5 373.86 13.50 19 3 5 392.06 12.10 -19 3 -5 376.46 14.00 19 3 5 379.86 13.60 21 -3 5 245.18 8.90 21 -3 5 248.18 10.50 -21 -3 -5 267.07 9.30 -21 -3 -5 247.88 11.00 21 3 5 248.88 10.90 -21 3 -5 223.78 10.90 -23 -3 -5 151.08 8.70 23 -3 5 145.59 6.50 23 -3 5 146.89 8.30 -23 -3 -5 152.98 6.70 23 3 5 162.08 9.00 -23 3 -5 162.38 9.30 -25 -3 -5 78.89 6.50 25 -3 5 57.59 6.10 -25 3 -5 70.69 7.50 25 3 5 58.19 6.60 27 -3 5 15.70 3.90 -27 -3 -5 19.60 4.20 27 3 5 11.60 4.00 -27 3 -5 9.00 3.90 29 -3 5 1.40 2.50 -29 -3 -5 2.50 2.50 -29 3 -5 1.90 3.30 29 3 5 2.80 3.30 31 -3 5 9.30 3.40 -31 -3 -5 14.90 4.60 31 3 5 8.90 3.90 -31 3 -5 15.80 4.60 33 -3 5 82.69 8.60 -33 -3 -5 88.99 9.00 -33 3 -5 94.69 9.80 33 3 5 75.09 8.60 -35 -3 -5 49.00 7.20 35 -3 5 35.00 6.30 -35 3 -5 43.00 7.20 35 3 5 41.30 6.90 37 -3 5 12.90 4.50 -37 -3 -5 14.70 4.90 37 3 5 8.30 4.80 -37 3 -5 19.70 5.70 -40 -4 5 1.80 4.00 40 -4 -5 7.90 4.40 -40 4 5 -0.30 2.90 40 4 -5 1.20 3.50 -38 -4 5 0.60 3.30 38 -4 -5 -2.60 3.60 -38 4 5 1.80 3.50 38 4 -5 -1.30 4.10 -36 -4 5 -1.30 2.70 36 -4 -5 6.80 4.10 -36 4 5 -2.90 2.70 36 4 -5 5.90 4.30 34 -4 -5 33.40 6.10 -34 -4 5 43.50 6.60 34 4 -5 50.49 7.30 -34 4 5 45.60 6.60 32 -4 -5 5.10 3.30 -32 -4 5 5.40 3.40 32 4 -5 4.30 3.60 -32 4 5 9.30 3.30 -30 -4 5 11.50 3.70 30 -4 -5 13.20 3.90 30 4 -5 13.60 4.40 -30 4 5 10.50 3.80 28 -4 -5 36.20 5.50 -28 -4 5 30.10 5.00 28 4 -5 40.10 5.90 -28 4 5 35.70 5.30 -26 -4 5 18.80 3.90 26 -4 -5 22.10 4.30 26 4 -5 19.60 4.40 -26 4 5 23.60 4.30 24 -4 -5 125.39 7.90 -24 -4 5 112.89 7.20 24 4 -5 119.39 7.90 -24 4 5 120.69 7.40 -22 -4 5 39.30 4.70 22 -4 -5 38.90 4.80 -22 -4 5 46.40 2.50 22 4 -5 47.20 5.50 -22 4 5 51.69 5.50 20 -4 -5 259.97 10.60 -20 -4 5 260.87 7.40 20 -4 -5 253.77 6.20 20 -4 -5 247.88 6.00 -20 -4 5 261.17 10.10 -20 4 5 236.88 10.20 20 4 -5 244.38 10.80 -18 -4 5 77.69 3.50 18 -4 -5 74.19 2.70 18 -4 -5 76.69 5.20 -18 -4 5 77.99 4.90 18 4 -5 69.29 5.40 -18 4 5 80.59 5.20 -16 -4 5 219.28 6.90 16 -4 -5 202.88 8.40 16 -4 -5 219.48 6.10 -16 -4 5 219.28 8.20 16 4 -5 213.38 8.80 -16 4 5 217.28 8.50 14 -4 -5 150.38 4.90 -14 -4 5 153.58 6.30 -14 -4 5 158.58 5.60 14 -4 -5 140.49 6.40 -14 4 5 163.58 6.70 14 4 -5 150.98 6.80 -14 4 5 156.28 6.60 -12 -4 5 34.30 2.70 12 -4 -5 36.50 2.20 -12 -4 5 34.40 2.40 -12 4 5 35.10 2.90 12 4 -5 34.00 3.30 -12 4 5 27.80 2.80 10 -4 -5 434.56 11.50 -10 -4 5 428.86 11.80 -10 -4 5 426.76 11.70 10 4 -5 441.76 12.20 -10 4 5 447.06 12.30 -10 4 5 424.86 11.60 -8 -4 5 238.78 7.70 -8 -4 5 244.88 7.40 8 -4 -5 242.38 7.50 8 4 -5 240.08 7.40 -8 4 5 237.68 7.10 -8 4 5 236.68 7.60 6 -4 -5 90.49 4.00 -6 -4 5 84.09 3.70 -6 -4 5 83.09 3.90 6 4 -5 80.09 3.30 -6 4 5 79.19 3.20 -6 4 5 81.09 3.80 -4 -4 5 8.30 1.60 -4 -4 5 10.50 1.50 -4 4 5 9.00 1.40 -4 4 5 10.10 1.70 -4 4 5 8.80 1.10 4 4 -5 9.70 1.20 -2 -4 5 12.60 1.80 -2 4 5 10.30 1.90 -2 4 5 11.90 1.20 2 4 -5 11.40 1.40 2 4 -5 12.60 1.10 -2 4 5 12.30 1.60 0 -4 5 22.70 2.50 0 -4 5 22.70 1.40 0 -4 -5 20.70 1.30 0 4 -5 25.40 1.90 0 4 5 20.30 1.80 0 4 5 21.40 2.60 0 4 -5 24.50 1.20 -2 -4 -5 72.19 2.60 2 -4 5 76.99 3.90 2 4 5 80.89 4.30 -2 4 -5 76.89 3.40 2 4 5 70.99 3.20 -2 4 -5 74.59 2.40 4 -4 5 9.50 1.70 -4 -4 -5 11.10 1.30 -4 4 -5 9.70 1.60 -4 4 -5 13.50 1.10 4 4 5 10.20 1.90 4 4 5 10.70 1.60 6 -4 5 153.58 6.20 6 -4 5 172.38 5.10 -6 -4 -5 159.58 5.30 6 4 5 145.69 6.40 -6 4 -5 163.38 6.00 6 4 5 167.48 5.80 8 -4 5 26.40 2.80 8 -4 5 28.60 2.10 -8 -4 -5 29.00 2.30 8 4 5 33.10 3.30 8 4 5 25.00 2.50 -8 4 -5 27.10 2.80 -10 -4 -5 94.69 4.60 10 -4 5 96.09 4.40 10 -4 5 98.69 4.80 10 4 5 97.89 5.10 10 4 5 90.19 4.60 -10 4 -5 87.59 4.80 12 -4 5 105.29 5.20 -12 -4 -5 114.39 5.50 12 -4 5 104.09 5.10 12 4 5 117.69 5.50 12 4 5 116.69 5.70 -12 4 -5 112.69 5.70 14 -4 5 61.39 4.10 14 -4 5 59.49 3.90 -14 -4 -5 57.39 4.20 14 4 5 61.09 4.20 -14 4 -5 50.49 4.80 14 4 5 65.09 4.60 -16 -4 -5 85.59 5.50 16 -4 5 84.89 5.20 16 -4 5 80.99 4.70 16 4 5 77.89 4.80 16 4 5 88.39 5.50 -16 4 -5 84.29 5.80 18 -4 5 5.30 2.00 -18 -4 -5 6.40 1.90 -18 -4 -5 7.40 2.30 18 -4 5 7.50 2.00 -18 4 -5 5.80 2.40 18 4 5 8.00 2.40 -20 -4 -5 -0.50 1.90 20 -4 5 0.60 1.40 -20 -4 -5 1.40 1.20 20 -4 5 -1.60 1.50 -20 4 -5 1.20 1.80 20 4 5 -0.50 2.10 -22 -4 -5 5.70 2.40 22 -4 5 3.70 2.50 -22 -4 -5 5.40 1.80 22 -4 5 5.30 1.80 -22 4 -5 5.20 2.70 22 4 5 6.50 2.90 24 -4 5 8.10 2.90 -24 -4 -5 5.10 2.50 24 4 5 9.90 3.40 -24 4 -5 3.90 2.70 26 -4 5 3.60 2.50 -26 -4 -5 1.20 2.20 -26 4 -5 3.30 2.50 26 4 5 2.70 2.90 -28 -4 -5 16.00 4.10 28 -4 5 14.80 3.80 28 4 5 16.80 4.30 -28 4 -5 12.70 4.10 -30 -4 -5 30.10 5.20 30 -4 5 21.80 4.50 -30 4 -5 34.30 6.00 30 4 5 33.90 5.70 32 -4 5 45.10 6.20 -32 -4 -5 49.60 6.80 32 4 5 52.19 7.00 -32 4 -5 56.59 7.80 34 -4 5 7.50 3.50 -34 -4 -5 14.50 4.30 34 4 5 10.90 4.90 -34 4 -5 7.80 4.10 -36 -4 -5 -0.40 2.80 36 -4 5 0.70 3.10 36 4 5 4.90 4.40 -36 4 -5 0.10 3.70 -39 -5 5 210.88 13.00 39 -5 -5 222.48 14.20 39 5 -5 205.68 13.60 -39 5 5 210.68 13.10 -37 -5 5 167.28 11.20 37 -5 -5 179.38 12.00 37 5 -5 139.49 11.30 -37 5 5 175.38 11.60 35 -5 -5 94.49 9.90 -35 -5 5 98.09 9.70 -35 5 5 120.59 9.30 35 5 -5 101.29 10.40 33 -5 -5 74.49 8.40 -33 -5 5 103.79 8.30 33 5 -5 86.99 9.30 -33 5 5 72.79 8.10 -31 -5 5 0.40 2.70 31 -5 -5 -0.10 2.80 -31 5 5 3.30 2.80 31 5 -5 -1.00 2.90 -29 -5 5 45.70 6.00 29 -5 -5 50.49 6.50 -29 5 5 50.49 6.40 29 5 -5 60.59 7.30 -27 -5 5 394.56 15.40 27 -5 -5 441.46 16.80 27 5 -5 396.46 16.30 -27 5 5 409.96 15.90 -25 -5 5 689.73 21.90 25 -5 -5 734.63 23.10 -25 5 5 730.53 22.70 25 5 -5 749.33 23.50 -23 -5 5 206.88 9.70 23 -5 -5 218.88 10.30 23 5 -5 197.18 10.30 -23 5 5 258.17 10.80 -21 -5 5 499.15 15.80 21 -5 -5 485.95 16.40 -21 -5 5 515.45 13.10 21 -5 -5 489.85 11.60 21 5 -5 479.65 16.70 -21 5 5 487.15 16.20 19 -5 -5 451.35 11.00 -19 -5 5 448.36 12.10 19 -5 -5 449.66 14.70 -19 -5 5 446.76 14.10 19 5 -5 425.46 14.90 -19 5 5 425.66 14.40 17 -5 -5 9.80 1.40 -17 -5 5 11.50 1.80 -17 -5 5 5.80 1.90 17 -5 -5 8.40 2.20 17 5 -5 9.00 2.70 -17 5 5 11.80 2.40 15 -5 -5 13.10 1.60 -15 -5 5 13.50 1.90 -15 -5 5 10.80 2.00 -15 5 5 11.20 2.20 -15 5 5 13.30 2.40 15 5 -5 15.30 2.70 13 -5 -5 514.45 13.10 -13 -5 5 513.35 13.80 -13 -5 5 515.05 14.00 -13 5 5 483.15 14.40 13 5 -5 508.45 14.70 -13 5 5 510.45 14.20 -11 -5 5 1094.79 25.20 -11 -5 5 1008.70 25.60 11 -5 -5 1093.59 25.30 11 5 -5 1070.49 25.80 -11 5 5 1056.39 25.10 -11 5 5 1072.99 25.90 -9 -5 5 948.21 23.60 9 -5 -5 969.70 23.20 -9 -5 5 968.80 22.70 -9 5 5 993.80 23.50 9 5 -5 936.91 22.90 -9 5 5 967.30 22.40 -7 -5 5 1956.50 42.70 -7 -5 5 1910.61 44.50 7 -5 -5 1938.61 44.20 7 5 -5 1965.80 42.80 -7 5 5 1992.40 43.50 -7 5 5 1940.71 42.00 -5 -5 5 1650.63 39.50 5 -5 -5 1778.92 39.80 -5 -5 5 1731.13 37.90 -5 5 5 1709.53 36.80 -5 5 5 1725.53 38.40 5 5 -5 1718.63 37.50 -3 -5 5 435.96 12.40 3 -5 -5 440.26 12.50 3 5 -5 444.96 10.60 3 5 -5 429.36 11.10 -3 5 5 436.06 11.50 -3 5 5 424.06 10.10 -1 -5 5 139.49 5.70 1 -5 -5 144.59 3.90 1 -5 -5 155.38 6.20 1 5 -5 139.59 4.20 -1 5 5 143.69 5.10 1 5 -5 134.99 4.90 -1 -5 -5 249.97 6.10 1 -5 5 228.78 8.00 1 5 5 243.08 8.50 1 5 5 237.38 7.30 -1 5 -5 250.77 7.30 -1 5 -5 246.98 6.30 3 -5 5 167.18 6.50 -3 -5 -5 174.48 4.80 -3 5 -5 182.98 5.00 -3 5 -5 174.78 6.00 3 5 5 177.98 7.10 3 5 5 169.78 5.90 -5 -5 -5 2324.17 49.40 5 -5 5 2398.26 52.79 5 5 5 2145.09 53.09 -5 5 -5 2308.57 50.79 5 5 5 2419.76 51.19 -5 5 -5 2326.67 49.70 7 -5 5 1361.06 31.90 -7 -5 -5 1338.27 29.80 -7 5 -5 1329.57 29.70 7 5 5 1267.17 32.40 7 5 5 1319.97 30.80 -7 5 -5 1345.87 30.90 9 -5 5 673.23 17.90 9 -5 5 670.13 16.70 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4 10 1399.76 33.00 -12 -4 10 657.93 18.80 -12 -4 10 690.43 18.50 -12 4 10 661.63 17.70 12 4 -10 691.33 17.80 -12 4 10 678.33 18.60 -12 4 10 667.73 18.10 -10 -4 10 157.48 6.70 -10 -4 10 155.48 7.00 -10 4 10 147.89 6.70 10 4 -10 153.38 5.70 -10 4 10 141.49 6.00 -10 4 10 149.79 6.00 -8 -4 10 1.50 1.40 -8 -4 10 2.10 1.50 -8 4 10 2.30 1.30 -8 4 10 1.10 1.20 8 4 -10 3.00 1.00 -8 4 10 -0.80 1.00 -6 -4 10 261.57 10.00 6 4 -10 258.57 7.00 -6 4 10 269.87 8.40 -6 4 10 274.17 8.50 6 4 -10 264.77 8.90 -6 4 10 276.97 10.20 -4 -4 10 759.62 21.20 4 -4 -10 751.72 18.30 -4 4 10 769.12 18.60 4 4 -10 726.83 16.40 4 4 -10 755.12 19.30 4 4 -10 781.12 16.40 -4 4 10 723.53 21.10 2 -4 -10 1857.81 41.20 -2 -4 10 1872.71 45.10 -2 4 10 1931.21 45.80 2 4 -10 1797.42 42.20 -2 4 10 1895.41 41.60 0 -4 -10 1303.87 29.70 0 -4 10 1284.67 33.10 0 4 10 1334.17 29.90 0 4 -10 1328.67 30.90 0 4 10 1256.57 33.40 -2 -4 -10 971.40 22.90 2 -4 10 976.70 26.10 -2 4 -10 950.40 23.90 2 4 10 1004.40 23.00 2 4 10 920.51 26.30 -4 -4 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19.20 2 2 -23 381.16 15.70 0 -2 -23 210.18 10.90 0 -2 23 233.48 14.20 0 2 -23 200.08 10.90 0 2 23 176.38 12.80 2 -2 23 94.79 10.70 -2 -2 -23 96.09 7.70 -2 2 -23 96.09 7.80 2 2 23 92.19 10.40 4 -2 23 -0.60 3.90 -4 -2 -23 -0.30 3.00 -4 2 -23 0.60 2.90 4 2 23 2.70 3.80 -6 -2 -23 36.00 5.90 6 -2 23 40.50 7.70 6 2 23 34.80 7.20 -6 2 -23 40.00 6.30 -8 -2 -23 59.49 7.10 8 -2 23 58.49 9.10 -8 2 -23 49.10 6.80 8 2 23 62.79 8.90 10 -2 23 119.39 12.20 -10 -2 -23 96.59 9.20 10 2 23 92.49 10.80 -10 2 -23 99.69 9.50 12 -2 23 324.97 17.70 -12 -2 -23 321.77 15.50 12 2 23 374.26 19.20 -12 2 -23 350.36 16.30 -14 -2 -23 226.38 13.10 14 -2 23 248.78 15.60 -14 2 -23 222.58 13.20 14 2 23 233.18 15.10 -29 -3 23 38.10 6.80 -29 3 23 51.09 7.30 -27 -3 23 48.70 7.30 -27 3 23 77.69 8.90 25 3 -23 38.00 6.40 -25 3 23 44.40 6.80 23 -3 -23 43.30 6.10 23 3 -23 37.70 6.20 21 -3 -23 21.30 4.70 -21 -3 23 16.80 4.40 21 3 -23 14.00 4.50 -19 -3 23 -2.70 2.10 19 -3 -23 -0.50 2.50 19 3 -23 -0.90 2.80 -19 3 23 1.40 2.50 17 -3 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7 1 -1.9515 0.1003 29 7 2 -0.7754 0.3867 29 7 3 0.8345 0.1171 29 7 4 0.7377 -0.4549 29 7 5 1.0409 -0.1725 29 7 6 0.7154 0.5638 29 7 7 0.6720 -0.5170 29 7 8 -0.2104 -0.1079 29 7 9 -2.1966 -0.0063 29 7 10 -0.8350 -0.7398 29 7 11 0.8198 0.1550 29 9 0 -1.3895 0.6271 29 9 1 -1.6458 0.3923 29 9 2 1.9186 -0.2634 29 9 3 0.3827 -0.2602 29 9 4 -0.0254 0.1820 29 9 5 1.3185 -0.1079 29 9 6 -0.3006 -0.2931 29 9 7 -2.2810 -0.3678 29 9 8 1.1472 -0.4484 29 9 9 0.7552 -0.8713 29 9 10 -0.2023 0.7020 29 11 0 2.2487 0.1991 29 11 1 -2.6223 -0.1581 29 11 2 -1.9179 -0.3503 29 11 3 3.9871 0.7453 29 11 4 -1.3466 0.3972 29 11 5 -0.6074 -0.2605 29 11 6 3.1526 0.5266 29 11 7 -4.2460 -1.3254 29 11 8 -0.6225 0.1392 29 13 0 -1.2621 1.1304 29 13 1 1.9431 0.8050 29 13 2 2.6919 -0.7372 29 13 3 -0.8545 -0.0784 29 13 4 -3.2716 1.3686 29 13 5 -0.7035 -0.5618 29 15 0 -2.7607 1.2021 29 15 1 -3.4440 -0.2752 30 0 0 0.4813 0.1838 30 0 2 -0.0110 -0.3794 30 0 4 3.5430 0.0648 30 0 6 -6.5438 0.0268 30 0 8 4.1824 0.0837 30 0 10 -2.4768 0.1978 30 0 12 4.5610 0.6271 30 2 0 1.0277 -0.6800 30 2 1 -0.3248 0.0557 30 2 2 0.3579 0.7187 30 2 3 -1.2372 -0.2138 30 2 4 -0.2867 -0.6058 30 2 5 3.8053 0.1644 30 2 6 -0.7758 0.4450 30 2 7 -3.1695 -0.2475 30 2 8 1.3311 -0.2911 30 2 9 3.3028 0.2406 30 2 10 -3.8310 0.0205 30 2 11 -3.3682 1.3306 30 2 12 3.4843 0.6720 30 4 0 -0.8037 -0.1391 30 4 1 0.8059 -0.0163 30 4 2 1.1017 0.1271 30 4 3 0.0346 0.5660 30 4 4 -1.5155 0.2736 30 4 5 0.5493 -0.4306 30 4 6 0.7247 -0.3410 30 4 7 -0.5614 -0.3679 30 4 8 -1.7754 -0.5405 30 4 9 2.0135 0.6298 30 4 10 1.3004 0.4488 30 4 11 -2.4057 -0.0704 30 4 12 0.6092 0.6495 30 6 0 -1.0729 -0.6135 30 6 1 -2.0505 0.9260 30 6 2 -0.1409 0.1031 30 6 3 1.1678 -0.3019 30 6 4 0.6172 -0.6283 30 6 5 1.7947 0.0478 30 6 6 0.5104 0.1872 30 6 7 -0.8782 -0.9512 30 6 8 -2.3463 0.4607 30 6 9 -2.3225 0.0720 30 6 10 1.8131 -0.3394 30 6 11 1.5285 0.9822 30 8 0 -0.5824 0.4219 30 8 1 -0.6851 0.0787 30 8 2 0.8506 -0.3650 30 8 3 -0.9559 0.0555 30 8 4 -1.2166 0.9062 30 8 5 1.1530 -0.3808 30 8 6 2.7755 -0.4853 30 8 7 0.3778 0.1155 30 8 8 0.0675 -0.9819 30 8 9 -1.8974 -0.3243 30 8 10 -1.3724 0.4439 30 10 0 -0.8027 0.2222 30 10 1 -3.8647 0.2922 30 10 2 0.8030 0.1311 30 10 3 4.6678 0.2355 30 10 4 -1.7963 -0.0481 30 10 5 -0.5113 0.1972 30 10 6 2.8768 -0.6170 30 10 7 -2.4231 -1.3564 30 10 8 0.1470 0.8236 30 12 0 0.6668 0.7511 30 12 1 0.9720 -0.3276 30 12 2 -0.4498 -1.0050 30 12 3 -0.8122 0.9474 30 12 4 -0.6691 1.9109 30 12 5 0.6472 -0.7169 30 14 0 -4.1615 0.1026 30 14 1 -1.1292 -0.4955 30 14 2 4.1238 0.1710 31 1 0 1.3235 0.0406 31 1 1 -0.7638 0.2664 31 1 2 0.4884 -0.0670 31 1 3 -0.1959 -0.0952 31 1 4 1.4278 -0.2407 31 1 5 0.8508 -0.0187 31 1 6 -3.6803 0.3217 31 1 7 -1.5228 -0.0584 31 1 8 1.8143 -0.3858 31 1 9 1.8702 0.4409 31 1 10 -1.9801 1.1413 31 1 11 -0.0826 0.4588 31 3 0 0.2589 -1.0338 31 3 1 1.4353 -0.3274 31 3 2 1.4470 0.5374 31 3 3 -0.9244 0.2041 31 3 4 -1.7932 0.1005 31 3 5 2.4628 -0.6322 31 3 6 0.0439 0.0214 31 3 7 -1.7600 -0.1076 31 3 8 0.2289 -0.5196 31 3 9 1.9447 1.0187 31 3 10 -1.9164 0.1988 31 3 11 -2.1528 0.8053 31 5 0 -2.1975 0.1119 31 5 1 -1.2114 0.0734 31 5 2 1.8263 -0.2600 31 5 3 1.7797 0.6635 31 5 4 -1.7745 0.2020 31 5 5 0.9219 0.1066 31 5 6 1.2218 -0.8293 31 5 7 -1.4564 -0.9768 31 5 8 -2.4269 0.1647 31 5 9 -0.2003 -0.3760 31 5 10 2.1542 0.8596 31 7 0 0.6598 0.2341 31 7 1 -0.6141 0.3611 31 7 2 -1.1095 -0.3850 31 7 3 -0.0433 0.1399 31 7 4 -0.3390 0.3160 31 7 5 0.6096 -0.9530 31 7 6 3.3732 -0.4036 31 7 7 0.8734 -0.3068 31 7 8 -1.5157 -0.2324 31 7 9 -3.5086 0.9042 31 9 0 -1.3348 -0.0341 31 9 1 -1.0541 0.5587 31 9 2 2.6760 0.0396 31 9 3 1.8465 -0.1518 31 9 4 -2.8970 0.8431 31 9 5 -0.5933 0.5375 31 9 6 2.9293 -1.2834 31 9 7 -0.2132 -0.2301 31 9 8 0.9826 -0.2587 31 11 0 -1.1501 0.6002 31 11 1 -2.0874 -0.1374 31 11 2 -1.6211 -0.3805 31 11 3 1.6668 1.1232 31 11 4 1.2724 1.0053 31 11 5 0.9611 -0.7765 31 13 0 -2.6148 -1.2968 31 13 1 0.8699 -1.0549 31 13 2 4.0144 0.8489 32 0 0 1.8741 0.1397 32 0 2 -0.7529 -0.1431 32 0 4 2.0628 -0.2442 32 0 6 -2.7172 0.3444 32 0 8 0.9012 -0.1280 32 0 10 -0.8565 0.7902 32 2 0 2.0819 -0.2658 32 2 1 1.6141 -0.2214 32 2 2 0.8875 -0.4179 32 2 3 -1.4432 0.0947 32 2 4 -0.8168 0.4546 32 2 5 1.6366 -0.7216 32 2 6 -1.3334 -0.0677 32 2 7 -2.2838 -0.0435 32 2 8 -0.1461 -0.0515 32 2 9 1.9242 0.8992 32 2 10 -1.0593 0.8934 32 4 0 -3.8602 -0.3424 32 4 1 0.8597 -0.2303 32 4 2 4.0899 0.1216 32 4 3 0.5267 0.1657 32 4 4 -3.4338 0.2522 32 4 5 1.8576 -0.0155 32 4 6 1.0282 -0.7382 32 4 7 -1.1671 -0.2767 32 4 8 -0.8622 -0.2842 32 4 9 -0.5120 0.0761 32 4 10 0.5605 1.3132 32 6 0 1.0573 0.5575 32 6 1 -1.6679 -0.4477 32 6 2 -0.6494 -0.5363 32 6 3 2.5999 1.0688 32 6 4 -2.0484 0.1977 32 6 5 -0.9100 -0.6477 32 6 6 4.3244 -0.8253 32 6 7 -0.0383 -0.9040 32 6 8 -2.9091 0.2653 32 6 9 -2.2007 0.2353 32 8 0 0.0795 -0.2960 32 8 1 1.1512 0.7323 32 8 2 0.6865 0.1985 32 8 3 0.3775 -0.2963 32 8 4 -0.5663 0.7877 32 8 5 -1.8959 -0.2732 32 8 6 1.4777 -1.5107 32 8 7 2.2283 0.1724 32 10 0 -1.1417 0.2654 32 10 1 -0.9484 0.2690 32 10 2 -0.3898 -0.2212 32 10 3 1.6984 1.2998 32 10 4 0.7182 0.4513 32 10 5 0.8046 -0.6400 32 12 0 -3.4632 -1.3940 32 12 1 -0.0286 -0.1136 32 12 2 1.8898 1.1327 33 1 0 3.8398 -0.3446 33 1 1 2.1759 -0.5110 33 1 2 -2.2074 0.0281 33 1 3 -2.6617 0.3653 33 1 4 1.3214 0.1027 33 1 5 1.6845 -0.8364 33 1 6 -0.9037 -0.4274 33 1 7 -2.1584 0.7083 33 1 8 -0.1706 0.8032 33 1 9 1.4794 1.0547 33 3 0 -2.6769 0.6800 33 3 1 3.7385 0.3145 33 3 2 4.5733 -1.0939 33 3 3 -1.3982 -0.8079 33 3 4 -3.6828 0.6601 33 3 5 1.6357 -0.2452 33 3 6 0.2948 -0.3858 33 3 7 -1.0567 0.0231 33 3 8 -1.4900 -0.0626 33 3 9 -0.5192 0.6843 33 5 0 -2.6428 -0.3463 33 5 1 -2.0815 -0.9363 33 5 2 2.5795 0.4613 33 5 3 3.2050 1.0021 33 5 4 -3.7885 -0.5349 33 5 5 -0.1529 0.0387 33 5 6 3.4171 -0.7260 33 5 7 -0.6880 -0.5782 33 5 8 -1.4766 0.3833 33 7 0 2.0451 0.0907 33 7 1 0.9063 0.4842 33 7 2 -1.3066 0.0072 33 7 3 2.1512 -0.1416 33 7 4 -0.3660 0.8019 33 7 5 -4.1582 -0.9217 33 7 6 2.9465 -1.6282 33 7 7 2.9205 0.0996 33 9 0 1.2635 -0.6593 33 9 1 0.3402 -0.2836 33 9 2 -1.0682 0.5346 33 9 3 0.8406 1.7145 33 9 4 2.1963 -0.8952 33 9 5 -0.4121 -0.3834 33 11 0 -3.1919 -0.5288 33 11 1 1.9878 1.8013 33 11 2 0.4786 0.3580 34 0 0 6.4231 -0.6024 34 0 2 -6.0955 0.0318 34 0 4 3.1265 0.3640 34 0 6 0.8572 -0.4882 34 0 8 -0.1972 0.5891 34 2 0 1.1777 0.2745 34 2 1 5.6275 -0.0263 34 2 2 1.0879 -0.6619 34 2 3 -4.5618 -0.1510 34 2 4 -1.9292 0.3405 34 2 5 2.3157 -0.7933 34 2 6 -0.1612 -0.2443 34 2 7 -1.3657 0.0657 34 2 8 -0.7577 0.8440 34 4 0 -5.7691 0.5093 34 4 1 0.8476 0.0445 34 4 2 5.4831 0.1754 34 4 3 1.9791 -0.6522 34 4 4 -3.9818 -1.0241 34 4 5 -0.1470 0.2936 34 4 6 1.3079 -0.5724 34 4 7 -0.2360 0.4362 34 6 0 0.5293 -0.9127 34 6 1 -1.4927 -0.1653 34 6 2 -0.7193 0.3297 34 6 3 3.8094 0.2987 34 6 4 -1.2998 0.4425 34 6 5 -3.0795 -0.7623 34 6 6 3.6816 -0.7173 34 8 0 2.7835 -0.5797 34 8 1 0.1028 -0.0603 34 8 2 -2.1939 1.4805 34 8 3 1.0530 0.7358 34 8 4 2.4988 -1.6573 34 10 0 1.2965 -0.3738 34 10 1 3.4530 1.1468 34 10 2 -1.6377 -0.4361 35 1 0 4.8980 -0.3054 35 1 1 2.7236 0.7999 35 1 2 -4.0950 -0.0254 35 1 3 -3.3712 -0.0005 35 1 4 1.1045 -0.3984 35 1 5 0.9499 -0.2588 35 1 6 1.1971 0.1612 35 1 7 1.1886 0.1936 35 3 0 -2.5284 -0.2713 35 3 1 5.0644 -0.0810 35 3 2 3.5155 0.5739 35 3 3 -2.1170 -0.4359 35 3 4 -2.5434 -0.8500 35 3 5 0.6946 -0.6834 35 3 6 -1.2016 -0.2207 35 5 0 -4.2517 -0.0371 35 5 1 -2.3584 0.4479 35 5 2 2.1747 0.2420 35 5 3 4.9890 -0.3345 35 5 4 -1.1647 -0.7849 35 5 5 -1.9986 -0.4761 35 7 0 2.1381 -1.3572 35 7 1 -1.0948 0.1159 35 7 2 -2.9598 1.5688 35 7 3 0.9916 -0.4691 35 7 4 2.0148 -0.8078 35 9 0 4.7921 0.4714 35 9 1 1.5762 0.5042 36 0 0 2.2600 0.6187 36 0 2 -2.0142 0.2075 36 0 4 0.0688 -0.3189 36 2 0 3.1835 -1.8968 36 2 1 2.1357 1.2903 36 2 2 -2.6507 0.9393 36 2 3 -2.6695 0.5369 36 2 4 1.1529 -1.1053 36 2 5 -0.3033 -1.3606 36 4 0 -3.9334 0.4422 36 4 1 2.0973 -0.6588 36 4 2 3.2302 0.8049 36 4 3 1.8368 -0.0608 36 4 4 -0.9701 -1.3463 36 6 0 -1.3040 -1.5546 36 6 1 -4.0574 1.5395 36 6 2 -2.6231 0.7223 36 6 3 3.4195 -1.2883 36 8 0 4.4192 1.6466 37 1 0 -0.2643 0.1418 37 1 1 -3.7378 -0.2399 37 1 2 -0.5608 -0.2284 37 1 3 0.8000 1.7449 37 3 0 3.6126 -2.0826 37 3 1 2.7141 -0.4100 37 3 2 -2.7018 1.7105 37 3 3 -1.3846 0.7273 37 5 0 -3.8289 0.0529 37 5 1 -2.8745 1.4803 37 5 2 0.6667 0.1283 38 0 0 -6.7954 -0.6489 38 2 0 3.6378 -0.6970 38 2 1 -4.3836 -0.2803 38 4 0 1.2001 -0.7127 0 0 0 0.0 0.0 ; _shelx_fab_checksum 1517 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.28313(2) 0.63500(2) 0.25453(2) 0.01267(3) Uani 1 1 d . . . . . O1 O 0.21650(4) 0.60301(7) 0.25164(6) 0.01237(16) Uani 1 1 d . . . . . O2 O 0.34063(4) 0.70086(7) 0.26409(6) 0.01237(16) Uani 1 1 d . . . . . N1 N 0.26338(5) 0.74798(9) 0.30998(8) 0.0134(3) Uani 1 1 d . . . . . C1 C 0.17910(6) 0.61764(10) 0.28187(9) 0.0144(3) Uani 1 1 d . . . . . C2 C 0.13237(7) 0.61858(11) 0.24250(9) 0.0177(4) Uani 1 1 d . . . . . C3 C 0.09696(7) 0.63968(11) 0.27813(10) 0.0174(4) Uani 1 1 d . . . . . H3 H 0.0660 0.6426 0.2526 0.021 Uiso 1 1 calc R . . . . C4 C 0.10562(7) 0.65651(12) 0.34961(10) 0.0199(4) Uani 1 1 d . . . . . C5 C 0.15147(7) 0.64866(11) 0.38762(10) 0.0188(4) Uani 1 1 d . . . . . H5 H 0.1579 0.6563 0.4358 0.023 Uiso 1 1 calc R . . . . C6 C 0.18821(6) 0.62949(10) 0.35464(9) 0.0151(3) Uani 1 1 d . . . . . C7 C 0.23578(6) 0.61391(11) 0.39994(9) 0.0157(3) Uani 1 1 d . . . . . C8 C 0.24334(7) 0.54133(11) 0.43483(10) 0.0194(4) Uani 1 1 d . . . . . H8 H 0.2206 0.5020 0.4238 0.023 Uiso 1 1 calc R . . . . C9 C 0.28379(7) 0.52690(12) 0.48524(10) 0.0209(4) Uani 1 1 d . . . . . H9 H 0.2880 0.4779 0.5069 0.025 Uiso 1 1 calc R . . . . C10 C 0.31835(7) 0.58480(12) 0.50403(10) 0.0213(4) Uani 1 1 d . . . . . C11 C 0.31197(7) 0.65579(12) 0.46828(10) 0.0194(4) Uani 1 1 d . . . . . H11 H 0.3350 0.6946 0.4793 0.023 Uiso 1 1 calc R . . . . C12 C 0.27174(6) 0.67062(11) 0.41585(9) 0.0151(3) Uani 1 1 d . . . . . C13 C 0.11882(6) 0.59259(11) 0.16554(9) 0.0162(3) Uani 1 1 d . . . . . C14 C 0.06491(7) 0.59170(14) 0.13691(11) 0.0262(4) Uani 1 1 d . . . . . H14A H 0.0503 0.5561 0.1647 0.031 Uiso 1 1 calc R . . . . H14B H 0.0523 0.6441 0.1406 0.031 Uiso 1 1 calc R . . . . C15 C 0.05303(7) 0.56501(16) 0.05978(12) 0.0336(5) Uani 1 1 d . . . . . H15 H 0.0187 0.5648 0.0429 0.040 Uiso 1 1 calc R . . . . C16 C 0.07196(8) 0.48183(16) 0.05402(13) 0.0365(6) Uani 1 1 d . . . . . H16A H 0.0641 0.4644 0.0057 0.044 Uiso 1 1 calc R . . . . H16B H 0.0577 0.4456 0.0818 0.044 Uiso 1 1 calc R . . . . C17 C 0.12563(7) 0.48220(13) 0.08045(11) 0.0250(4) Uani 1 1 d . . . . . H17 H 0.1381 0.4291 0.0765 0.030 Uiso 1 1 calc R . . . . C18 C 0.14758(8) 0.53994(14) 0.03617(11) 0.0272(5) Uani 1 1 d . . . . . H18A H 0.1816 0.5401 0.0522 0.033 Uiso 1 1 calc R . . . . H18B H 0.1402 0.5233 -0.0124 0.033 Uiso 1 1 calc R . . . . C19 C 0.12838(8) 0.62286(14) 0.04217(11) 0.0275(5) Uani 1 1 d . . . . . H19 H 0.1426 0.6594 0.0139 0.033 Uiso 1 1 calc R . . . . C20 C 0.07491(9) 0.62246(17) 0.01568(12) 0.0382(6) Uani 1 1 d . . . . . H20A H 0.0671 0.6065 -0.0331 0.046 Uiso 1 1 calc R . . . . H20B H 0.0624 0.6750 0.0191 0.046 Uiso 1 1 calc R . . . . C21 C 0.14030(7) 0.64938(12) 0.11903(10) 0.0209(4) Uani 1 1 d . . . . . H21A H 0.1281 0.7021 0.1226 0.025 Uiso 1 1 calc R . . . . H21B H 0.1743 0.6510 0.1355 0.025 Uiso 1 1 calc R . . . . C22 C 0.13751(7) 0.50870(11) 0.15754(10) 0.0199(4) Uani 1 1 d . . . . . H22A H 0.1714 0.5078 0.1748 0.024 Uiso 1 1 calc R . . . . H22B H 0.1235 0.4722 0.1854 0.024 Uiso 1 1 calc R . . . . C23 C 0.26688(6) 0.74848(11) 0.38001(9) 0.0145(3) Uani 1 1 d . . . . . C24 C 0.26713(7) 0.81856(11) 0.41644(10) 0.0190(4) Uani 1 1 d . . . . . H24 H 0.2697 0.8181 0.4646 0.023 Uiso 1 1 calc R . . . . C25 C 0.26360(7) 0.88922(12) 0.38027(10) 0.0211(4) Uani 1 1 d . . . . . H25 H 0.2638 0.9368 0.4040 0.025 Uiso 1 1 calc R . . . . C26 C 0.25981(7) 0.88856(11) 0.30854(10) 0.0181(4) Uani 1 1 d . . . . . H26 H 0.2572 0.9356 0.2835 0.022 Uiso 1 1 calc R . . . . C27 C 0.25990(6) 0.81686(10) 0.27442(9) 0.0135(3) Uani 1 1 d . . . . . C28 C 0.25346(6) 0.81326(10) 0.19656(9) 0.0134(3) Uani 1 1 d . . . . . C29 C 0.29169(6) 0.81280(10) 0.16308(9) 0.0151(3) Uani 1 1 d . . . . . C30 C 0.28069(7) 0.81582(11) 0.08949(10) 0.0183(4) Uani 1 1 d . . . . . H30 H 0.3050 0.8129 0.0655 0.022 Uiso 1 1 calc R . . . . C31 C 0.23477(7) 0.82304(11) 0.05171(10) 0.0187(4) Uani 1 1 d . . . . . H31 H 0.2290 0.8250 0.0031 0.022 Uiso 1 1 calc R . . . . C32 C 0.19715(7) 0.82743(11) 0.08504(10) 0.0187(4) Uani 1 1 d . . . . . C33 C 0.20736(6) 0.82019(11) 0.15776(10) 0.0163(3) Uani 1 1 d . . . . . H33 H 0.1826 0.8200 0.1811 0.020 Uiso 1 1 calc R . . . . C34 C 0.36495(6) 0.76429(10) 0.24972(9) 0.0142(3) Uani 1 1 d . . . . . C35 C 0.34198(6) 0.81871(11) 0.19945(9) 0.0145(3) Uani 1 1 d . . . . . C36 C 0.36789(7) 0.88054(11) 0.17829(10) 0.0164(3) Uani 1 1 d . . . . . H36 H 0.3527 0.9154 0.1441 0.020 Uiso 1 1 calc R . . . . C37 C 0.41519(7) 0.89096(11) 0.20669(10) 0.0164(3) Uani 1 1 d . . . . . C38 C 0.43663(6) 0.83833(11) 0.25931(10) 0.0160(3) Uani 1 1 d . . . . . H38 H 0.4682 0.8461 0.2801 0.019 Uiso 1 1 calc R . . . . C39 C 0.41328(6) 0.77501(11) 0.28217(9) 0.0146(3) Uani 1 1 d . . . . . C40 C 0.44010(6) 0.71983(11) 0.33926(10) 0.0165(3) Uani 1 1 d . . . . . C41 C 0.49175(7) 0.74598(12) 0.36627(10) 0.0207(4) Uani 1 1 d . . . . . H41A H 0.5077 0.7468 0.3276 0.025 Uiso 1 1 calc R . . . . H41B H 0.4923 0.7991 0.3848 0.025 Uiso 1 1 calc R . . . . C42 C 0.51824(7) 0.69052(13) 0.42360(11) 0.0258(4) Uani 1 1 d . . . . . H42 H 0.5508 0.7088 0.4393 0.031 Uiso 1 1 calc R . . . . C43 C 0.51836(8) 0.60699(14) 0.39503(13) 0.0322(5) Uani 1 1 d . . . . . H43A H 0.5349 0.5720 0.4314 0.039 Uiso 1 1 calc R . . . . H43B H 0.5346 0.6061 0.3566 0.039 Uiso 1 1 calc R . . . . C44 C 0.46739(8) 0.57917(13) 0.36963(12) 0.0302(5) Uani 1 1 d . . . . . H44 H 0.4673 0.5254 0.3512 0.036 Uiso 1 1 calc R . . . . C45 C 0.44250(8) 0.57995(14) 0.43120(12) 0.0328(5) Uani 1 1 d . . . . . H45A H 0.4103 0.5617 0.4157 0.039 Uiso 1 1 calc R . . . . H45B H 0.4586 0.5447 0.4676 0.039 Uiso 1 1 calc R . . . . C46 C 0.44263(7) 0.66365(14) 0.46025(11) 0.0273(5) Uani 1 1 d . . . . . H46 H 0.4267 0.6638 0.4996 0.033 Uiso 1 1 calc R . . . . C47 C 0.49367(8) 0.69141(15) 0.48575(11) 0.0288(5) Uani 1 1 d . . . . . H47A H 0.5101 0.6567 0.5224 0.035 Uiso 1 1 calc R . . . . H47B H 0.4941 0.7443 0.5047 0.035 Uiso 1 1 calc R . . . . C48 C 0.41633(7) 0.71903(12) 0.40278(10) 0.0207(4) Uani 1 1 d . . . . . H48A H 0.4162 0.7720 0.4214 0.025 Uiso 1 1 calc R . . . . H48B H 0.3839 0.7018 0.3878 0.025 Uiso 1 1 calc R . . . . C49 C 0.06591(8) 0.67829(14) 0.38472(11) 0.0280(5) Uani 1 1 d . . . . . H49A H 0.0541 0.7296 0.3692 0.042 Uiso 1 1 calc GR . . . . H49B H 0.0774 0.6789 0.4346 0.042 Uiso 1 1 calc GR . . . . H49C H 0.0410 0.6402 0.3727 0.042 Uiso 1 1 calc GR . . . . C50 C 0.14782(7) 0.84375(14) 0.04429(11) 0.0272(4) Uani 1 1 d . . . . . H50A H 0.1407 0.8986 0.0481 0.041 Uiso 1 1 calc GR . . . . H50B H 0.1258 0.8125 0.0628 0.041 Uiso 1 1 calc GR . . . . H50C H 0.1456 0.8305 -0.0040 0.041 Uiso 1 1 calc GR . . . . C51 C 0.27890(7) 0.60847(12) 0.14251(10) 0.0226(4) Uani 1 1 d . . . . . H51A H 0.2725 0.5534 0.1342 0.034 Uiso 1 1 calc GR . . . . H51B H 0.3083 0.6215 0.1305 0.034 Uiso 1 1 calc GR . . . . H51C H 0.2541 0.6390 0.1143 0.034 Uiso 1 1 calc GR . . . . C52 C 0.31861(7) 0.53083(11) 0.30940(11) 0.0222(4) Uani 1 1 d . . . . . H52A H 0.3347 0.5455 0.3558 0.033 Uiso 1 1 calc GR . . . . H52B H 0.3410 0.5106 0.2842 0.033 Uiso 1 1 calc GR . . . . H52C H 0.2956 0.4910 0.3121 0.033 Uiso 1 1 calc GR . . . . C53 C 0.44291(7) 0.95662(11) 0.18225(10) 0.0200(4) Uani 1 1 d . . . . . H53A H 0.4674 0.9345 0.1622 0.030 Uiso 1 1 calc GR . . . . H53B H 0.4567 0.9893 0.2213 0.030 Uiso 1 1 calc GR . . . . H53C H 0.4222 0.9878 0.1477 0.030 Uiso 1 1 calc GR . . . . C54 C 0.36085(8) 0.56957(15) 0.56256(12) 0.0344(5) Uani 1 1 d . . . . . H54A H 0.3844 0.5417 0.5444 0.052 Uiso 1 1 calc GR . . . . H54B H 0.3515 0.5385 0.5983 0.052 Uiso 1 1 calc GR . . . . H54C H 0.3736 0.6189 0.5821 0.052 Uiso 1 1 calc GR . . . . C55 C 0.44126(7) 0.63453(11) 0.31141(11) 0.0215(4) Uani 1 1 d . . . . . H55A H 0.4093 0.6158 0.2946 0.026 Uiso 1 1 calc R . . . . H55B H 0.4571 0.6340 0.2725 0.026 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.01256(4) 0.01312(4) 0.01228(4) -0.00121(3) 0.00259(3) -0.00198(3) O1 0.0088(4) 0.0143(4) 0.0137(4) 0.0006(3) 0.0018(3) -0.0028(3) O2 0.0088(4) 0.0143(4) 0.0137(4) 0.0006(3) 0.0018(3) -0.0028(3) N1 0.0133(7) 0.0152(7) 0.0113(7) -0.0008(5) 0.0017(5) -0.0016(5) C1 0.0137(8) 0.0162(8) 0.0122(8) 0.0020(6) 0.0004(6) -0.0022(6) C2 0.0250(10) 0.0153(8) 0.0101(8) -0.0016(6) -0.0024(7) 0.0051(7) C3 0.0133(8) 0.0210(9) 0.0175(9) 0.0002(7) 0.0024(7) -0.0007(7) C4 0.0199(9) 0.0214(9) 0.0203(9) -0.0013(7) 0.0083(7) -0.0014(7) C5 0.0208(9) 0.0226(10) 0.0135(8) -0.0023(7) 0.0045(7) -0.0038(7) C6 0.0147(8) 0.0158(8) 0.0146(8) 0.0000(6) 0.0029(6) -0.0048(7) C7 0.0158(8) 0.0212(9) 0.0101(8) -0.0007(6) 0.0027(6) -0.0019(7) C8 0.0225(10) 0.0199(9) 0.0159(9) -0.0013(7) 0.0043(7) -0.0058(7) C9 0.0262(10) 0.0197(9) 0.0171(9) 0.0041(7) 0.0056(8) 0.0010(7) C10 0.0195(9) 0.0288(10) 0.0148(9) 0.0052(7) 0.0020(7) 0.0006(8) C11 0.0191(9) 0.0254(10) 0.0134(8) 0.0016(7) 0.0026(7) -0.0048(7) C12 0.0164(9) 0.0182(9) 0.0109(8) -0.0005(6) 0.0035(6) -0.0026(7) C13 0.0125(8) 0.0213(9) 0.0137(8) -0.0016(7) 0.0006(6) 0.0008(7) C14 0.0156(9) 0.0407(12) 0.0210(10) -0.0070(9) 0.0012(7) 0.0010(9) C15 0.0134(9) 0.0585(16) 0.0243(11) -0.0144(10) -0.0064(8) 0.0043(9) C16 0.0237(11) 0.0518(15) 0.0307(12) -0.0202(11) -0.0012(9) -0.0079(10) C17 0.0216(10) 0.0289(11) 0.0215(10) -0.0111(8) -0.0015(8) -0.0013(8) C18 0.0224(10) 0.0405(13) 0.0173(9) -0.0065(9) 0.0009(8) 0.0050(9) C19 0.0299(11) 0.0386(13) 0.0138(9) 0.0036(8) 0.0042(8) 0.0073(9) C20 0.0339(13) 0.0609(17) 0.0158(10) -0.0015(10) -0.0032(9) 0.0204(12) C21 0.0222(10) 0.0240(10) 0.0164(9) 0.0023(7) 0.0038(7) 0.0037(8) C22 0.0189(9) 0.0198(9) 0.0193(9) -0.0018(7) 0.0007(7) -0.0021(7) C23 0.0121(8) 0.0183(9) 0.0128(8) -0.0007(6) 0.0018(6) -0.0025(6) C24 0.0233(10) 0.0212(9) 0.0125(8) -0.0042(7) 0.0041(7) -0.0038(7) C25 0.0261(10) 0.0173(9) 0.0201(9) -0.0051(7) 0.0055(8) -0.0022(7) C26 0.0195(9) 0.0158(8) 0.0180(9) -0.0007(7) 0.0020(7) -0.0011(7) C27 0.0107(8) 0.0166(8) 0.0129(8) -0.0002(6) 0.0020(6) -0.0012(6) C28 0.0151(8) 0.0108(8) 0.0139(8) 0.0005(6) 0.0018(6) 0.0003(6) C29 0.0148(8) 0.0149(8) 0.0150(8) 0.0005(6) 0.0021(7) -0.0005(6) C30 0.0211(9) 0.0205(9) 0.0141(9) 0.0006(7) 0.0053(7) -0.0003(7) C31 0.0248(10) 0.0176(9) 0.0116(8) 0.0009(7) -0.0004(7) -0.0019(7) C32 0.0193(9) 0.0158(9) 0.0182(9) 0.0018(7) -0.0019(7) -0.0005(7) C33 0.0151(8) 0.0161(8) 0.0174(9) 0.0011(7) 0.0028(7) -0.0007(7) C34 0.0151(8) 0.0137(8) 0.0144(8) -0.0007(6) 0.0043(6) -0.0026(6) C35 0.0138(8) 0.0176(8) 0.0124(8) -0.0013(6) 0.0035(6) -0.0002(6) C36 0.0165(9) 0.0173(9) 0.0160(8) 0.0023(7) 0.0044(7) 0.0009(7) C37 0.0167(9) 0.0161(8) 0.0175(9) -0.0009(7) 0.0062(7) -0.0004(7) C38 0.0127(8) 0.0185(9) 0.0171(9) -0.0010(7) 0.0039(7) -0.0001(7) C39 0.0137(8) 0.0167(8) 0.0130(8) -0.0007(6) 0.0021(6) -0.0003(6) C40 0.0136(8) 0.0191(9) 0.0159(8) 0.0033(7) 0.0009(7) -0.0002(7) C41 0.0137(9) 0.0267(10) 0.0205(9) 0.0041(8) 0.0013(7) -0.0016(7) C42 0.0152(9) 0.0362(12) 0.0232(10) 0.0084(9) -0.0021(8) -0.0009(8) C43 0.0252(11) 0.0345(12) 0.0342(12) 0.0102(10) 0.0004(9) 0.0097(9) C44 0.0292(11) 0.0210(10) 0.0358(12) 0.0053(9) -0.0031(9) 0.0039(8) C45 0.0278(11) 0.0318(12) 0.0333(12) 0.0170(10) -0.0060(9) -0.0052(9) C46 0.0203(10) 0.0410(12) 0.0191(10) 0.0091(9) 0.0007(8) -0.0042(9) C47 0.0212(10) 0.0417(13) 0.0199(10) 0.0072(9) -0.0032(8) -0.0051(9) C48 0.0173(9) 0.0280(10) 0.0168(9) 0.0026(8) 0.0036(7) -0.0019(8) C49 0.0224(10) 0.0387(13) 0.0250(11) -0.0042(9) 0.0098(8) 0.0019(9) C50 0.0204(10) 0.0346(12) 0.0227(10) 0.0062(9) -0.0041(8) 0.0024(8) C51 0.0266(10) 0.0231(10) 0.0195(9) -0.0039(8) 0.0079(8) -0.0051(8) C52 0.0218(10) 0.0185(9) 0.0257(10) 0.0023(8) 0.0035(8) -0.0001(7) C53 0.0174(9) 0.0183(9) 0.0247(10) 0.0037(7) 0.0057(7) -0.0029(7) C54 0.0267(11) 0.0452(14) 0.0264(11) 0.0163(10) -0.0054(9) -0.0066(10) C55 0.0216(10) 0.0191(9) 0.0220(10) 0.0003(7) 0.0007(7) 0.0025(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Hf1 N1 84.42(5) . . ? O1 Hf1 C51 94.02(6) . . ? O1 Hf1 C52 98.29(6) . . ? O2 Hf1 O1 161.00(5) . . ? O2 Hf1 N1 77.29(5) . . ? O2 Hf1 C51 94.23(6) . . ? O2 Hf1 C52 96.31(6) . . ? C51 Hf1 N1 131.31(7) . . ? C52 Hf1 N1 124.59(7) . . ? C52 Hf1 C51 103.85(8) . . ? C1 O1 Hf1 142.49(11) . . ? C34 O2 Hf1 153.75(11) . . ? C23 N1 Hf1 120.26(12) . . ? C23 N1 C27 119.80(15) . . ? C27 N1 Hf1 117.96(11) . . ? O1 C1 C2 121.80(16) . . ? O1 C1 C6 118.10(15) . . ? C6 C1 C2 120.07(17) . . ? C1 C2 C13 123.06(17) . . ? C3 C2 C1 116.90(17) . . ? C3 C2 C13 119.90(17) . . ? C2 C3 H3 118.1 . . ? C4 C3 C2 123.74(17) . . ? C4 C3 H3 118.1 . . ? C3 C4 C49 121.05(18) . . ? C5 C4 C3 117.58(17) . . ? C5 C4 C49 121.29(18) . . ? C4 C5 H5 119.5 . . ? C4 C5 C6 121.01(17) . . ? C6 C5 H5 119.5 . . ? C1 C6 C7 121.54(16) . . ? C5 C6 C1 120.33(17) . . ? C5 C6 C7 117.82(16) . . ? C8 C7 C6 118.13(16) . . ? C8 C7 C12 117.57(17) . . ? C12 C7 C6 123.92(17) . . ? C7 C8 H8 119.3 . . ? C9 C8 C7 121.50(18) . . ? C9 C8 H8 119.3 . . ? C8 C9 H9 119.5 . . ? C8 C9 C10 121.01(18) . . ? C10 C9 H9 119.5 . . ? C9 C10 C54 120.12(18) . . ? C11 C10 C9 117.93(18) . . ? C11 C10 C54 121.94(19) . . ? C10 C11 H11 119.1 . . ? C10 C11 C12 121.71(18) . . ? C12 C11 H11 119.1 . . ? C7 C12 C23 120.88(16) . . ? C11 C12 C7 120.12(17) . . ? C11 C12 C23 118.93(16) . . ? C2 C13 C14 112.54(16) . . ? C2 C13 C21 110.34(16) . . ? C2 C13 C22 110.03(15) . . ? C14 C13 C21 107.38(16) . . ? C22 C13 C14 107.77(16) . . ? C22 C13 C21 108.65(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C15 C14 C13 110.68(16) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C14 C15 H15 109.1 . . ? C16 C15 C14 109.6(2) . . ? C16 C15 H15 109.1 . . ? C16 C15 C20 110.3(2) . . ? C20 C15 C14 109.5(2) . . ? C20 C15 H15 109.1 . . ? C15 C16 H16A 109.9 . . ? C15 C16 H16B 109.9 . . ? C15 C16 C17 109.10(18) . . ? H16A C16 H16B 108.3 . . ? C17 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? C16 C17 H17 109.7 . . ? C16 C17 C18 109.15(19) . . ? C16 C17 C22 109.17(17) . . ? C18 C17 H17 109.7 . . ? C18 C17 C22 109.53(17) . . ? C22 C17 H17 109.7 . . ? C17 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C19 C18 C17 109.98(17) . . ? C19 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? C18 C19 H19 109.5 . . ? C18 C19 C20 109.3(2) . . ? C18 C19 C21 109.63(17) . . ? C20 C19 H19 109.5 . . ? C20 C19 C21 109.37(18) . . ? C21 C19 H19 109.5 . . ? C15 C20 H20A 109.9 . . ? C15 C20 H20B 109.9 . . ? C19 C20 C15 109.10(18) . . ? C19 C20 H20A 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C13 C21 H21A 109.4 . . ? C13 C21 H21B 109.4 . . ? C19 C21 C13 111.07(17) . . ? C19 C21 H21A 109.4 . . ? C19 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C13 C22 H22A 109.4 . . ? C13 C22 H22B 109.4 . . ? C17 C22 C13 111.04(16) . . ? C17 C22 H22A 109.4 . . ? C17 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N1 C23 C12 116.80(15) . . ? N1 C23 C24 121.18(17) . . ? C24 C23 C12 122.00(16) . . ? C23 C24 H24 120.4 . . ? C25 C24 C23 119.23(17) . . ? C25 C24 H24 120.4 . . ? C24 C25 H25 120.3 . . ? C26 C25 C24 119.49(18) . . ? C26 C25 H25 120.3 . . ? C25 C26 H26 120.4 . . ? C25 C26 C27 119.14(18) . . ? C27 C26 H26 120.4 . . ? N1 C27 C26 121.15(16) . . ? N1 C27 C28 117.89(15) . . ? C26 C27 C28 120.87(16) . . ? C29 C28 C27 122.49(16) . . ? C33 C28 C27 116.46(16) . . ? C33 C28 C29 120.60(16) . . ? C28 C29 C30 116.67(16) . . ? C28 C29 C35 124.82(16) . . ? C30 C29 C35 118.11(16) . . ? C29 C30 H30 119.0 . . ? C31 C30 C29 122.00(18) . . ? C31 C30 H30 119.0 . . ? C30 C31 H31 119.4 . . ? C30 C31 C32 121.24(17) . . ? C32 C31 H31 119.4 . . ? C31 C32 C33 117.27(17) . . ? C31 C32 C50 121.01(18) . . ? C33 C32 C50 121.63(18) . . ? C28 C33 C32 122.05(17) . . ? C28 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? O2 C34 C35 118.56(16) . . ? O2 C34 C39 121.29(16) . . ? C35 C34 C39 120.10(16) . . ? C34 C35 C29 124.05(16) . . ? C36 C35 C29 116.33(16) . . ? C36 C35 C34 119.52(16) . . ? C35 C36 H36 119.1 . . ? C37 C36 C35 121.86(17) . . ? C37 C36 H36 119.1 . . ? C36 C37 C38 117.42(17) . . ? C36 C37 C53 121.33(17) . . ? C38 C37 C53 121.25(17) . . ? C37 C38 H38 118.1 . . ? C39 C38 C37 123.78(17) . . ? C39 C38 H38 118.1 . . ? C34 C39 C40 122.97(16) . . ? C38 C39 C34 117.17(16) . . ? C38 C39 C40 119.85(16) . . ? C39 C40 C41 112.15(15) . . ? C39 C40 C48 110.23(15) . . ? C39 C40 C55 111.09(15) . . ? C41 C40 C48 107.24(15) . . ? C41 C40 C55 107.20(16) . . ? C48 C40 C55 108.78(16) . . ? C40 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? C42 C41 C40 111.72(16) . . ? C42 C41 H41A 109.3 . . ? C42 C41 H41B 109.3 . . ? C41 C42 H42 109.3 . . ? C43 C42 C41 109.99(18) . . ? C43 C42 H42 109.3 . . ? C43 C42 C47 109.74(19) . . ? C47 C42 C41 109.08(17) . . ? C47 C42 H42 109.3 . . ? C42 C43 H43A 109.9 . . ? C42 C43 H43B 109.9 . . ? C42 C43 C44 109.10(18) . . ? H43A C43 H43B 108.3 . . ? C44 C43 H43A 109.9 . . ? C44 C43 H43B 109.9 . . ? C43 C44 H44 109.4 . . ? C43 C44 C45 109.21(19) . . ? C43 C44 C55 109.82(18) . . ? C45 C44 H44 109.4 . . ? C45 C44 C55 109.55(18) . . ? C55 C44 H44 109.4 . . ? C44 C45 H45A 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C46 C45 C44 109.66(18) . . ? C46 C45 H45A 109.7 . . ? C46 C45 H45B 109.7 . . ? C45 C46 H46 109.3 . . ? C45 C46 C47 109.35(19) . . ? C45 C46 C48 109.56(17) . . ? C47 C46 H46 109.3 . . ? C47 C46 C48 110.10(18) . . ? C48 C46 H46 109.3 . . ? C42 C47 H47A 110.0 . . ? C42 C47 H47B 109.9 . . ? C46 C47 C42 108.70(17) . . ? C46 C47 H47A 110.0 . . ? C46 C47 H47B 110.0 . . ? H47A C47 H47B 108.3 . . ? C40 C48 H48A 109.5 . . ? C40 C48 H48B 109.5 . . ? C46 C48 C40 110.85(16) . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? C4 C49 H49A 109.5 . . ? C4 C49 H49B 109.5 . . ? C4 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C32 C50 H50A 109.5 . . ? C32 C50 H50B 109.5 . . ? C32 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Hf1 C51 H51A 109.5 . . ? Hf1 C51 H51B 109.5 . . ? Hf1 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Hf1 C52 H52A 109.5 . . ? Hf1 C52 H52B 109.5 . . ? Hf1 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C37 C53 H53A 109.5 . . ? C37 C53 H53B 109.5 . . ? C37 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C10 C54 H54A 109.5 . . ? C10 C54 H54B 109.5 . . ? C10 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C40 C55 H55A 109.5 . . ? C40 C55 H55B 109.5 . . ? C44 C55 C40 110.68(16) . . ? C44 C55 H55A 109.5 . . ? C44 C55 H55B 109.5 . . ? H55A C55 H55B 108.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 O1 1.9986(12) . ? Hf1 O2 1.9842(12) . ? Hf1 N1 2.3341(15) . ? Hf1 C51 2.2150(19) . ? Hf1 C52 2.2048(19) . ? O1 C1 1.367(2) . ? O2 C34 1.350(2) . ? N1 C23 1.352(2) . ? N1 C27 1.353(2) . ? C1 C2 1.409(3) . ? C1 C6 1.406(2) . ? C2 C3 1.407(3) . ? C2 C13 1.537(2) . ? C3 H3 0.9300 . ? C3 C4 1.396(3) . ? C4 C5 1.385(3) . ? C4 C49 1.510(3) . ? C5 H5 0.9300 . ? C5 C6 1.399(3) . ? C6 C7 1.495(3) . ? C7 C8 1.402(3) . ? C7 C12 1.404(3) . ? C8 H8 0.9300 . ? C8 C9 1.383(3) . ? C9 H9 0.9300 . ? C9 C10 1.396(3) . ? C10 C11 1.385(3) . ? C10 C54 1.514(3) . ? C11 H11 0.9300 . ? C11 C12 1.402(3) . ? C12 C23 1.488(3) . ? C13 C14 1.545(3) . ? C13 C21 1.546(3) . ? C13 C22 1.543(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.542(3) . ? C15 H15 0.9800 . ? C15 C16 1.527(4) . ? C15 C20 1.528(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.533(3) . ? C17 H17 0.9800 . ? C17 C18 1.534(3) . ? C17 C22 1.540(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.527(3) . ? C19 H19 0.9800 . ? C19 C20 1.527(3) . ? C19 C21 1.536(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.385(3) . ? C24 H24 0.9300 . ? C24 C25 1.385(3) . ? C25 H25 0.9300 . ? C25 C26 1.384(3) . ? C26 H26 0.9300 . ? C26 C27 1.388(3) . ? C27 C28 1.496(2) . ? C28 C29 1.405(2) . ? C28 C33 1.395(2) . ? C29 C30 1.407(3) . ? C29 C35 1.484(2) . ? C30 H30 0.9300 . ? C30 C31 1.384(3) . ? C31 H31 0.9300 . ? C31 C32 1.390(3) . ? C32 C33 1.395(3) . ? C32 C50 1.507(3) . ? C33 H33 0.9300 . ? C34 C35 1.408(2) . ? C34 C39 1.422(2) . ? C35 C36 1.404(2) . ? C36 H36 0.9300 . ? C36 C37 1.378(3) . ? C37 C38 1.403(3) . ? C37 C53 1.511(3) . ? C38 H38 0.9300 . ? C38 C39 1.395(2) . ? C39 C40 1.535(2) . ? C40 C41 1.544(3) . ? C40 C48 1.546(3) . ? C40 C55 1.549(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 C42 1.537(3) . ? C42 H42 0.9800 . ? C42 C43 1.524(3) . ? C42 C47 1.537(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.531(3) . ? C44 H44 0.9800 . ? C44 C45 1.533(3) . ? C44 C55 1.544(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 C46 1.529(3) . ? C46 H46 0.9800 . ? C46 C47 1.532(3) . ? C46 C48 1.536(3) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Hf1 O1 C1 C2 141.85(16) . . . . ? Hf1 O1 C1 C6 -40.1(3) . . . . ? Hf1 O2 C34 C35 -3.6(4) . . . . ? Hf1 O2 C34 C39 178.98(18) . . . . ? Hf1 N1 C23 C12 -14.9(2) . . . . ? Hf1 N1 C23 C24 163.45(14) . . . . ? Hf1 N1 C27 C26 -164.08(13) . . . . ? Hf1 N1 C27 C28 19.2(2) . . . . ? O1 C1 C2 C3 -175.69(16) . . . . ? O1 C1 C2 C13 8.5(3) . . . . ? O1 C1 C6 C5 176.70(16) . . . . ? O1 C1 C6 C7 -9.8(3) . . . . ? O2 C34 C35 C29 2.9(3) . . . . ? O2 C34 C35 C36 -173.32(16) . . . . ? O2 C34 C39 C38 174.19(16) . . . . ? O2 C34 C39 C40 -4.9(3) . . . . ? N1 C23 C24 C25 0.2(3) . . . . ? N1 C27 C28 C29 -90.4(2) . . . . ? N1 C27 C28 C33 97.3(2) . . . . ? C1 C2 C3 C4 -2.4(3) . . . . ? C1 C2 C13 C14 174.44(18) . . . . ? C1 C2 C13 C21 -65.6(2) . . . . ? C1 C2 C13 C22 54.2(2) . . . . ? C1 C6 C7 C8 -97.4(2) . . . . ? C1 C6 C7 C12 89.9(2) . . . . ? C2 C1 C6 C5 -5.3(3) . . . . ? C2 C1 C6 C7 168.21(17) . . . . ? C2 C3 C4 C5 -2.7(3) . . . . ? C2 C3 C4 C49 -179.59(19) . . . . ? C2 C13 C14 C15 -179.77(18) . . . . ? C2 C13 C21 C19 178.27(16) . . . . ? C2 C13 C22 C17 -178.34(16) . . . . ? C3 C2 C13 C14 -1.2(3) . . . . ? C3 C2 C13 C21 118.71(19) . . . . ? C3 C2 C13 C22 -121.41(18) . . . . ? C3 C4 C5 C6 4.0(3) . . . . ? C4 C5 C6 C1 -0.1(3) . . . . ? C4 C5 C6 C7 -173.83(17) . . . . ? C5 C6 C7 C8 76.2(2) . . . . ? C5 C6 C7 C12 -96.4(2) . . . . ? C6 C1 C2 C3 6.3(3) . . . . ? C6 C1 C2 C13 -169.43(17) . . . . ? C6 C7 C8 C9 -170.53(18) . . . . ? C6 C7 C12 C11 168.55(17) . . . . ? C6 C7 C12 C23 -8.6(3) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? C7 C12 C23 N1 -62.8(2) . . . . ? C7 C12 C23 C24 118.9(2) . . . . ? C8 C7 C12 C11 -4.2(3) . . . . ? C8 C7 C12 C23 178.71(16) . . . . ? C8 C9 C10 C11 -3.1(3) . . . . ? C8 C9 C10 C54 176.1(2) . . . . ? C9 C10 C11 C12 1.5(3) . . . . ? C10 C11 C12 C7 2.2(3) . . . . ? C10 C11 C12 C23 179.38(18) . . . . ? C11 C12 C23 N1 120.06(19) . . . . ? C11 C12 C23 C24 -58.3(2) . . . . ? C12 C7 C8 C9 2.6(3) . . . . ? C12 C23 C24 C25 178.48(18) . . . . ? C13 C2 C3 C4 173.50(18) . . . . ? C13 C14 C15 C16 60.4(3) . . . . ? C13 C14 C15 C20 -60.7(2) . . . . ? C14 C13 C21 C19 -58.7(2) . . . . ? C14 C13 C22 C17 58.6(2) . . . . ? C14 C15 C16 C17 -60.5(3) . . . . ? C14 C15 C20 C19 60.5(2) . . . . ? C15 C16 C17 C18 -59.3(2) . . . . ? C15 C16 C17 C22 60.4(3) . . . . ? C16 C15 C20 C19 -60.2(2) . . . . ? C16 C17 C18 C19 60.0(2) . . . . ? C16 C17 C22 C13 -60.5(2) . . . . ? C17 C18 C19 C20 -60.3(2) . . . . ? C17 C18 C19 C21 59.6(2) . . . . ? C18 C17 C22 C13 59.0(2) . . . . ? C18 C19 C20 C15 59.7(2) . . . . ? C18 C19 C21 C13 -59.3(2) . . . . ? C20 C15 C16 C17 60.1(2) . . . . ? C20 C19 C21 C13 60.6(2) . . . . ? C21 C13 C14 C15 58.6(2) . . . . ? C21 C13 C22 C17 -57.4(2) . . . . ? C21 C19 C20 C15 -60.3(2) . . . . ? C22 C13 C14 C15 -58.3(2) . . . . ? C22 C13 C21 C19 57.6(2) . . . . ? C22 C17 C18 C19 -59.5(2) . . . . ? C23 N1 C27 C26 0.0(3) . . . . ? C23 N1 C27 C28 -176.74(15) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C24 C25 C26 C27 -0.3(3) . . . . ? C25 C26 C27 N1 0.3(3) . . . . ? C25 C26 C27 C28 176.91(17) . . . . ? C26 C27 C28 C29 92.9(2) . . . . ? C26 C27 C28 C33 -79.4(2) . . . . ? C27 N1 C23 C12 -178.58(15) . . . . ? C27 N1 C23 C24 -0.2(3) . . . . ? C27 C28 C29 C30 -174.93(16) . . . . ? C27 C28 C29 C35 -2.4(3) . . . . ? C27 C28 C33 C32 172.02(17) . . . . ? C28 C29 C30 C31 3.3(3) . . . . ? C28 C29 C35 C34 60.1(3) . . . . ? C28 C29 C35 C36 -123.60(19) . . . . ? C29 C28 C33 C32 -0.4(3) . . . . ? C29 C30 C31 C32 -0.2(3) . . . . ? C29 C35 C36 C37 -178.17(17) . . . . ? C30 C29 C35 C34 -127.42(19) . . . . ? C30 C29 C35 C36 48.9(2) . . . . ? C30 C31 C32 C33 -3.2(3) . . . . ? C30 C31 C32 C50 173.58(19) . . . . ? C31 C32 C33 C28 3.5(3) . . . . ? C33 C28 C29 C30 -2.9(3) . . . . ? C33 C28 C29 C35 169.62(17) . . . . ? C34 C35 C36 C37 -1.7(3) . . . . ? C34 C39 C40 C41 -178.94(17) . . . . ? C34 C39 C40 C48 -59.5(2) . . . . ? C34 C39 C40 C55 61.1(2) . . . . ? C35 C29 C30 C31 -169.80(17) . . . . ? C35 C34 C39 C38 -3.2(3) . . . . ? C35 C34 C39 C40 177.73(16) . . . . ? C35 C36 C37 C38 -1.6(3) . . . . ? C35 C36 C37 C53 178.56(17) . . . . ? C36 C37 C38 C39 2.5(3) . . . . ? C37 C38 C39 C34 -0.1(3) . . . . ? C37 C38 C39 C40 178.93(17) . . . . ? C38 C39 C40 C41 2.0(2) . . . . ? C38 C39 C40 C48 121.45(18) . . . . ? C38 C39 C40 C55 -117.90(19) . . . . ? C39 C34 C35 C29 -179.65(16) . . . . ? C39 C34 C35 C36 4.2(3) . . . . ? C39 C40 C41 C42 179.78(16) . . . . ? C39 C40 C48 C46 179.68(16) . . . . ? C39 C40 C55 C44 -178.80(16) . . . . ? C40 C41 C42 C43 59.7(2) . . . . ? C40 C41 C42 C47 -60.7(2) . . . . ? C41 C40 C48 C46 -58.0(2) . . . . ? C41 C40 C55 C44 58.4(2) . . . . ? C41 C42 C43 C44 -59.1(2) . . . . ? C41 C42 C47 C46 59.8(2) . . . . ? C42 C43 C44 C45 -60.2(2) . . . . ? C42 C43 C44 C55 59.9(2) . . . . ? C43 C42 C47 C46 -60.8(2) . . . . ? C43 C44 C45 C46 60.2(2) . . . . ? C43 C44 C55 C40 -60.8(2) . . . . ? C44 C45 C46 C47 -60.3(2) . . . . ? C44 C45 C46 C48 60.4(2) . . . . ? C45 C44 C55 C40 59.1(2) . . . . ? C45 C46 C47 C42 60.1(2) . . . . ? C45 C46 C48 C40 -59.7(2) . . . . ? C47 C42 C43 C44 60.9(2) . . . . ? C47 C46 C48 C40 60.6(2) . . . . ? C48 C40 C41 C42 58.6(2) . . . . ? C48 C40 C55 C44 -57.3(2) . . . . ? C48 C46 C47 C42 -60.3(2) . . . . ? C49 C4 C5 C6 -179.15(19) . . . . ? C50 C32 C33 C28 -173.23(18) . . . . ? C53 C37 C38 C39 -177.60(17) . . . . ? C54 C10 C11 C12 -177.7(2) . . . . ? C55 C40 C41 C42 -58.0(2) . . . . ? C55 C40 C48 C46 57.7(2) . . . . ? C55 C44 C45 C46 -60.2(2) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.095 0.250 335.1 49.8 0.5(C6H14) 2 0.000 0.095 0.750 335.1 49.8 ? 3 0.500 0.405 0.250 335.1 49.8 ? 4 0.500 0.595 0.750 335.1 49.8 ?