#------------------------------------------------------------------------------ #$Date: 2019-11-11 16:46:56 +0200 (Mon, 11 Nov 2019) $ #$Revision: 226611 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/51/4035126.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_4035126 loop_ _publ_author_name 'Gillen, Dermot M.' 'Hawes, Chris S.' 'Gunnlaugsson, Thorfinnur' _publ_section_title ; Solution-State Anion Recognition, and Structural Studies, of a Series of Electron-Rich meta-Phenylene Bis(phenylurea) Receptors and Their Self-Assembled Structures. ; _journal_issue 17 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 10398 _journal_page_last 10408 _journal_paper_doi 10.1021/acs.joc.8b01481 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety '6(C22 H22 N4 O4), 6(C16 H36 N), 2(C0.5 H0.5 Cl1.5), 4(H1.5 O4 P1)' _chemical_formula_sum 'C229 H355 Cl3 N30 O40 P4' _chemical_formula_weight 4398.64 _space_group_crystal_system trigonal _space_group_IT_number 161 _space_group_name_Hall 'R 3 -2"c' _space_group_name_H-M_alt 'R 3 c :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2015-06-27 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 22.0110(7) _cell_length_b 22.0110(7) _cell_length_c 42.9761(14) _cell_measurement_reflns_used 9515 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.35 _cell_measurement_theta_min 2.84 _cell_volume 18031.7(10) _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 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_number 70836 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.330 _diffrn_reflns_theta_min 1.850 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_T_max 0.4311 _exptl_absorpt_correction_T_min 0.3676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0647 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.8781. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 7110 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.429 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.058 _refine_ls_abs_structure_details ; Flack x determined using 3146 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.11(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 474 _refine_ls_number_reflns 9954 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0550 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+9.3580P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1422 _refine_ls_wR_factor_ref 0.1612 _reflns_Friedel_coverage 0.993 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 7602 _reflns_number_total 9954 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b01481_si_001.cif _cod_data_source_block 3(TBA3H3P2O8) _cod_original_cell_volume 18031.7(13) _cod_original_sg_symbol_H-M 'R 3 c' _cod_database_code 4035126 _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. ; _shelx_estimated_absorpt_t_max 0.975 _shelx_estimated_absorpt_t_min 0.955 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances H6-O7 1.74 with sigma of 0.01 H7A-O6 1.74 with sigma of 0.01 3. Others Fixed Sof: Cl1(0.5) H7A(0.5) H6(0.5) C39(0.16667) H39(0.16667) 4.a Ternary CH refined with riding coordinates: C39(H39) 4.b Secondary CH2 refined with riding coordinates: C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A, H28B), C29(H29A,H29B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B) 4.c Aromatic/amide H refined with riding coordinates: N1(H1), N2(H2), C3(H3), N3(H3A), C4(H4), N4(H4A), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14), C17(H17), C19(H19), C20(H20), C21(H21) 4.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C30(H30A,H30B, H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C) 4.e Idealised tetrahedral OH refined as rotating group: O7(H7A), O6(H6) ; _shelx_res_file ; mo_csh001_0m.res created by SHELXL-2014/7 TITL mo_csh001_0m_a.res in R3c REM Old TITL mo_CSH001_0m in R3c #161 REM SHELXT solution in R3c REM R1 0.146, Rweak 0.018, Alpha 0.002, Orientation as input REM Flack x = 0.285 ( 0.021 ) from Parsons' quotients REM Formula found by SHELXT: C117 N15 O20 Cl2 CELL 0.71073 22.011 22.011 42.9761 90 90 120 ZERR 3 0.0007 0.0007 0.0014 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -Y,-X,0.5+Z SYMM +Y-X,+Y,0.5+Z SYMM +X,+X-Y,0.5+Z SFAC C H Cl N O P UNIT 687 1065 9 90 120 12 EQIV $1 1+Y-X,1-X,+Z DFIX 1.74 0.01 H6 O7 DFIX 1.74 0.01 H7a O6 L.S. 20 PLAN 40 SIZE 0.18 0.28 0.33 TEMP -173 HTAB O7 O6 HTAB N2 O6_$1 HTAB N3 O7 HTAB C7 O2 HTAB C17 O3 HTAB N4 O8 HTAB N1 O5 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT -2 57 OMIT 0 8 4 REM REM REM WGHT 0.096000 9.358006 FVAR 0.06815 C1 1 0.707947 0.592444 0.263814 11.00000 0.08156 0.06267 = 0.02426 0.01179 0.01762 0.03358 AFIX 137 H1A 2 0.674033 0.547309 0.254571 11.00000 -1.50000 H1B 2 0.755614 0.603765 0.258164 11.00000 -1.50000 H1C 2 0.699161 0.629189 0.256011 11.00000 -1.50000 AFIX 0 N1 4 0.691768 0.479435 0.394267 11.00000 0.04479 0.04590 = 0.02814 0.00260 0.00286 0.02937 AFIX 43 H1 2 0.697585 0.447175 0.403658 11.00000 -1.20000 AFIX 0 O1 5 0.700705 0.588172 0.296908 11.00000 0.08320 0.05660 = 0.02555 0.00925 0.01671 0.04029 C2 1 0.710581 0.538945 0.311974 11.00000 0.04801 0.04013 = 0.02828 0.00531 0.01143 0.02036 N2 4 0.668160 0.499824 0.443331 11.00000 0.04930 0.04884 = 0.02417 0.00013 0.00003 0.03261 AFIX 43 H2 2 0.684434 0.471568 0.447775 11.00000 -1.20000 AFIX 0 O2 5 0.656651 0.560905 0.403116 11.00000 0.07363 0.06546 = 0.02664 0.00483 0.00680 0.05097 C3 1 0.729539 0.494489 0.297806 11.00000 0.04957 0.04460 = 0.02958 -0.00378 0.01232 0.01586 AFIX 43 H3 2 0.737726 0.496744 0.276022 11.00000 -1.20000 AFIX 0 N3 4 0.603313 0.452035 0.548268 11.00000 0.05607 0.04655 = 0.02463 -0.00086 0.00303 0.02900 AFIX 43 H3A 2 0.609524 0.416692 0.543376 11.00000 -1.20000 AFIX 0 O3 5 0.571654 0.496733 0.589025 11.00000 0.06736 0.06510 = 0.02633 0.00315 0.00768 0.04157 C4 1 0.736300 0.446390 0.316303 11.00000 0.05409 0.04214 = 0.04141 -0.00355 0.01171 0.02371 AFIX 43 H4 2 0.749144 0.415394 0.306874 11.00000 -1.20000 AFIX 0 N4 4 0.586925 0.401994 0.595495 11.00000 0.04908 0.05589 = 0.02456 0.00082 0.00218 0.02694 AFIX 43 H4A 2 0.603058 0.377846 0.585705 11.00000 -1.20000 AFIX 0 O4 5 0.495092 0.419790 0.696742 11.00000 0.12120 0.12450 = 0.05009 0.03972 0.04699 0.09193 C5 1 0.724846 0.442463 0.348009 11.00000 0.04601 0.03885 = 0.04136 0.00036 0.00713 0.02175 AFIX 43 H5 2 0.730484 0.409661 0.360237 11.00000 -1.20000 AFIX 0 C6 1 0.704786 0.487389 0.362023 11.00000 0.03415 0.03943 = 0.02699 -0.00243 0.00369 0.01591 C7 1 0.698501 0.535512 0.344059 11.00000 0.04624 0.04375 = 0.02815 0.00367 0.00867 0.02535 AFIX 43 H7 2 0.685869 0.566687 0.353468 11.00000 -1.20000 AFIX 0 C8 1 0.670833 0.517038 0.412630 11.00000 0.03973 0.04695 = 0.02563 0.00228 0.00160 0.02568 C9 1 0.643066 0.520887 0.468851 11.00000 0.03398 0.04666 = 0.02420 -0.00423 -0.00177 0.02382 C10 1 0.630087 0.576730 0.469400 11.00000 0.05034 0.05527 = 0.02779 0.00094 -0.00111 0.03481 AFIX 43 H10 2 0.635064 0.603104 0.451121 11.00000 -1.20000 AFIX 0 C11 1 0.609672 0.592826 0.497388 11.00000 0.05618 0.05646 = 0.03232 -0.00084 0.00061 0.04012 AFIX 43 H11 2 0.601710 0.631434 0.498018 11.00000 -1.20000 AFIX 0 C12 1 0.600374 0.554340 0.524711 11.00000 0.05158 0.05417 = 0.02694 -0.00644 -0.00046 0.03263 AFIX 43 H12 2 0.586254 0.566386 0.543517 11.00000 -1.20000 AFIX 0 C13 1 0.612308 0.498346 0.523564 11.00000 0.03898 0.04351 = 0.02462 -0.00282 -0.00318 0.01788 C14 1 0.633539 0.482405 0.495762 11.00000 0.03763 0.03909 = 0.02782 -0.00312 -0.00164 0.02008 AFIX 43 H14 2 0.641768 0.443967 0.495192 11.00000 -1.20000 AFIX 0 C15 1 0.586254 0.454516 0.578801 11.00000 0.04368 0.04527 = 0.02737 -0.00165 0.00097 0.02063 C16 1 0.564891 0.381652 0.626569 11.00000 0.04046 0.05818 = 0.02835 0.00406 0.00327 0.02249 C17 1 0.540576 0.415606 0.645632 11.00000 0.05144 0.06817 = 0.03161 0.01115 0.00976 0.03266 AFIX 43 H17 2 0.538111 0.455093 0.638386 11.00000 -1.20000 AFIX 0 C18 1 0.519696 0.390057 0.675935 11.00000 0.07349 0.09144 = 0.04023 0.02243 0.02482 0.05317 C19 1 0.522641 0.333003 0.686574 11.00000 0.10587 0.11898 = 0.05160 0.04179 0.04384 0.07850 AFIX 43 H19 2 0.508145 0.316439 0.707178 11.00000 -1.20000 AFIX 0 C20 1 0.546629 0.299868 0.667334 11.00000 0.08912 0.09227 = 0.05528 0.03094 0.02726 0.06275 AFIX 43 H20 2 0.547901 0.259755 0.674598 11.00000 -1.20000 AFIX 0 C21 1 0.568957 0.324136 0.637523 11.00000 0.05439 0.06233 = 0.04064 0.00859 0.00949 0.03298 AFIX 43 H21 2 0.586957 0.301834 0.624566 11.00000 -1.20000 AFIX 0 C22 1 0.496184 0.482602 0.687640 11.00000 0.11369 0.11453 = 0.04907 0.02239 0.03747 0.08259 AFIX 137 H22A 2 0.543905 0.517833 0.681472 11.00000 -1.50000 H22B 2 0.481157 0.500478 0.705146 11.00000 -1.50000 H22C 2 0.464240 0.472679 0.670043 11.00000 -1.50000 AFIX 0 N5 4 0.392516 0.268325 0.509150 11.00000 0.03940 0.04463 = 0.03760 0.00691 0.00900 0.01984 C23 1 0.441474 0.358208 0.397247 11.00000 0.14757 0.08594 = 0.04263 0.02111 0.01840 0.06415 AFIX 137 H23A 2 0.479519 0.380059 0.381978 11.00000 -1.50000 H23B 2 0.421332 0.388546 0.400689 11.00000 -1.50000 H23C 2 0.405038 0.312564 0.389405 11.00000 -1.50000 AFIX 0 C24 1 0.470528 0.347947 0.428083 11.00000 0.09672 0.08696 = 0.04853 0.02952 0.03207 0.06464 AFIX 23 H24A 2 0.493492 0.319753 0.424343 11.00000 -1.20000 H24B 2 0.506315 0.394199 0.436313 11.00000 -1.20000 AFIX 0 C25 1 0.412014 0.310860 0.452089 11.00000 0.05891 0.05375 = 0.04007 0.01212 0.00837 0.02641 AFIX 23 H25A 2 0.390908 0.340277 0.456982 11.00000 -1.20000 H25B 2 0.374824 0.265637 0.443571 11.00000 -1.20000 AFIX 0 C26 1 0.442353 0.298039 0.481393 11.00000 0.04456 0.05288 = 0.03785 0.01520 0.01481 0.02168 AFIX 23 H26A 2 0.483564 0.342993 0.487797 11.00000 -1.20000 H26B 2 0.459370 0.265245 0.476276 11.00000 -1.20000 AFIX 0 C27 1 0.432785 0.255206 0.534347 11.00000 0.03980 0.05470 = 0.03931 0.00791 0.00784 0.02458 AFIX 23 H27A 2 0.477848 0.299176 0.537600 11.00000 -1.20000 H27B 2 0.443996 0.219611 0.526559 11.00000 -1.20000 AFIX 0 C28 1 0.396878 0.230669 0.565803 11.00000 0.04526 0.06454 = 0.03624 0.00690 0.00929 0.03150 AFIX 23 H28A 2 0.346722 0.195516 0.562784 11.00000 -1.20000 H28B 2 0.399798 0.270924 0.577386 11.00000 -1.20000 AFIX 0 C29 1 0.432716 0.198388 0.584246 11.00000 0.05279 0.07104 = 0.03734 0.00615 0.00145 0.03519 AFIX 23 H29A 2 0.427466 0.156897 0.572888 11.00000 -1.20000 H29B 2 0.483468 0.232863 0.585726 11.00000 -1.20000 AFIX 0 C30 1 0.403123 0.176253 0.616834 11.00000 0.06821 0.09035 = 0.04099 0.01496 0.00575 0.04495 AFIX 137 H30A 2 0.351857 0.148015 0.615762 11.00000 -1.50000 H30B 2 0.416582 0.218053 0.629551 11.00000 -1.50000 H30C 2 0.421832 0.148406 0.626220 11.00000 -1.50000 AFIX 0 C31 1 0.384325 0.420719 0.574268 11.00000 0.08161 0.08324 = 0.11706 -0.02129 0.03489 0.02151 AFIX 137 H31A 2 0.348746 0.370948 0.575898 11.00000 -1.50000 H31B 2 0.365519 0.449314 0.582734 11.00000 -1.50000 H31C 2 0.426107 0.429703 0.586072 11.00000 -1.50000 AFIX 0 C32 1 0.403494 0.439263 0.540954 11.00000 0.07757 0.05754 = 0.09744 -0.00507 0.01105 0.02649 AFIX 23 H32A 2 0.440324 0.489254 0.539452 11.00000 -1.20000 H32B 2 0.361881 0.433054 0.529374 11.00000 -1.20000 AFIX 0 C33 1 0.429856 0.394518 0.526184 11.00000 0.06299 0.05608 = 0.05657 -0.00338 0.00134 0.02315 AFIX 23 H33A 2 0.464553 0.392528 0.540173 11.00000 -1.20000 H33B 2 0.453818 0.416346 0.506378 11.00000 -1.20000 AFIX 0 C34 1 0.370118 0.319983 0.519798 11.00000 0.04598 0.05216 = 0.04751 0.00773 0.00855 0.02555 AFIX 23 H34A 2 0.341990 0.301563 0.539034 11.00000 -1.20000 H34B 2 0.339184 0.322245 0.503675 11.00000 -1.20000 AFIX 0 C35 1 0.325998 0.201468 0.500686 11.00000 0.04264 0.04492 = 0.03788 0.00643 0.00516 0.02106 AFIX 23 H35A 2 0.301539 0.212460 0.484208 11.00000 -1.20000 H35B 2 0.294980 0.185352 0.519159 11.00000 -1.20000 AFIX 0 C36 1 0.335627 0.141146 0.489393 11.00000 0.06207 0.04793 = 0.04784 0.00725 0.00739 0.02821 AFIX 23 H36A 2 0.351627 0.123284 0.506852 11.00000 -1.20000 H36B 2 0.371899 0.158097 0.472917 11.00000 -1.20000 AFIX 0 C37 1 0.266477 0.082154 0.476608 11.00000 0.06980 0.05156 = 0.04899 -0.00094 -0.00356 0.02237 AFIX 23 H37A 2 0.269936 0.039172 0.474630 11.00000 -1.20000 H37B 2 0.228611 0.072251 0.491681 11.00000 -1.20000 AFIX 0 C38 1 0.247027 0.098659 0.445646 11.00000 0.13092 0.06480 = 0.05017 -0.00984 -0.02336 0.04354 AFIX 137 H38A 2 0.284661 0.109466 0.430662 11.00000 -1.50000 H38B 2 0.240245 0.139220 0.447699 11.00000 -1.50000 H38C 2 0.203442 0.058096 0.438309 11.00000 -1.50000 AFIX 0 CL1 3 0.646943 0.397310 0.735637 10.50000 0.08318 0.07666 = 0.05121 -0.01405 -0.00878 0.04282 P2 6 0.666667 0.333333 0.535792 10.33333 0.04447 0.04447 = 0.02668 0.00000 0.00000 0.02223 O7 5 0.598274 0.327825 0.522790 11.00000 0.04713 0.04519 = 0.02923 -0.00121 0.00054 0.02404 PART 1 AFIX 147 H7A 2 0.595480 0.319559 0.503604 10.50000 -1.50000 AFIX 0 PART 0 O8 5 0.666667 0.333333 0.570487 10.33333 0.05210 0.05210 = 0.03052 0.00000 0.00000 0.02605 P1 6 0.666667 0.333333 0.450212 10.33333 0.03799 0.03799 = 0.02559 0.00000 0.00000 0.01900 O5 5 0.666667 0.333333 0.415621 10.33333 0.04881 0.04881 = 0.02265 0.00000 0.00000 0.02441 O6 5 0.592496 0.311225 0.463257 11.00000 0.04144 0.04396 = 0.03023 -0.00190 0.00077 0.02161 PART 2 AFIX 147 H6 2 0.593529 0.310770 0.482791 10.50000 -1.50000 AFIX 0 PART 0 C39 1 0.666667 0.333333 0.722990 10.16667 0.08719 0.08719 = 0.03087 0.00000 0.00000 0.04360 AFIX 13 H39 2 0.666667 0.333332 0.699721 10.16667 -1.20000 AFIX 0 HKLF 4 REM mo_csh001_0m_a.res in R3c REM R1 = 0.0550 for 7602 Fo > 4sig(Fo) and 0.0792 for all 9954 data REM 474 parameters refined using 3 restraints END WGHT 0.0950 9.6172 REM Highest difference peak 0.429, deepest hole -0.493, 1-sigma level 0.058 Q1 1 0.3997 0.4906 0.5495 11.00000 0.05 0.43 Q2 1 0.6399 0.2806 0.5382 11.00000 0.05 0.32 Q3 1 0.5350 0.4629 0.7005 11.00000 0.05 0.28 Q4 1 0.7378 0.5274 0.3037 11.00000 0.05 0.26 Q5 1 0.5516 0.4202 0.6798 11.00000 0.05 0.25 Q6 1 0.6115 0.5306 0.5257 11.00000 0.05 0.24 Q7 1 0.6121 0.2907 0.4512 11.00000 0.05 0.24 Q8 1 0.6802 0.5009 0.3535 11.00000 0.05 0.24 Q9 1 0.5503 0.4499 0.5801 11.00000 0.05 0.24 Q10 1 0.4257 0.3132 0.4695 11.00000 0.05 0.24 Q11 1 0.5558 0.3681 0.6909 11.00000 0.05 0.24 Q12 1 0.4743 0.4181 0.6908 11.00000 0.05 0.23 Q13 1 0.4066 0.2745 0.4677 11.00000 0.05 0.23 Q14 1 0.3869 0.3836 0.5291 11.00000 0.05 0.23 Q15 1 0.6135 0.5646 0.5092 11.00000 0.05 0.23 Q16 1 0.4982 0.4052 0.6854 11.00000 0.05 0.23 Q17 1 0.3612 0.2226 0.5040 11.00000 0.05 0.22 Q18 1 0.6369 0.5250 0.4062 11.00000 0.05 0.22 Q19 1 0.5629 0.3355 0.6767 11.00000 0.05 0.22 Q20 1 0.6476 0.3441 0.7411 11.00000 0.05 0.22 Q21 1 0.4260 0.3790 0.5441 11.00000 0.05 0.22 Q22 1 0.6124 0.3047 0.5301 11.00000 0.05 0.22 Q23 1 0.6535 0.3541 0.4329 11.00000 0.05 0.22 Q24 1 0.6177 0.5351 0.4710 11.00000 0.05 0.21 Q25 1 0.5365 0.3398 0.6720 11.00000 0.05 0.20 Q26 1 0.3441 0.1819 0.4975 11.00000 0.05 0.20 Q27 1 0.6002 0.5740 0.4806 11.00000 0.05 0.20 Q28 1 0.2655 0.0138 0.4688 11.00000 0.05 0.19 Q29 1 0.7103 0.3488 0.5788 11.00000 0.05 0.19 Q30 1 0.4027 0.2022 0.5725 11.00000 0.05 0.19 Q31 1 0.5495 0.3935 0.6374 11.00000 0.05 0.19 Q32 1 0.6332 0.3363 0.4638 11.00000 0.05 0.18 Q33 1 0.3867 0.3069 0.5161 11.00000 0.05 0.18 Q34 1 0.2332 0.0405 0.4967 11.00000 0.05 0.18 Q35 1 0.6043 0.4754 0.5024 11.00000 0.05 0.18 Q36 1 0.6949 0.4535 0.3535 11.00000 0.05 0.18 Q37 1 0.6639 0.4815 0.3320 11.00000 0.05 0.18 Q38 1 0.5564 0.4134 0.5845 11.00000 0.05 0.18 Q39 1 0.6945 0.5561 0.3047 11.00000 0.05 0.18 Q40 1 0.7439 0.5798 0.3062 11.00000 0.05 0.18 ; _shelx_res_checksum 81861 _shelx_hkl_file ; -2 1 0 762.02 37.00 1 1 0 761.42 37.10 2 -1 0 781.92 37.00 -1 -1 0 815.52 37.10 -3 3 0 124.19 6.00 3 0 0 116.39 6.10 3 -3 0 133.29 6.00 -4 2 0 16.50 1.30 2 2 0 19.00 1.30 -2 -2 0 18.10 1.20 4 -2 0 16.70 1.30 -5 1 0 905.71 43.90 1 4 0 940.81 43.80 -4 5 0 916.01 43.70 5 -1 0 934.61 43.90 -5 4 0 894.61 44.50 4 1 0 967.20 44.60 5 -4 0 924.01 44.50 -4 -1 0 970.60 44.60 3 3 0 21.20 1.60 -6 3 0 16.30 1.60 -3 -3 0 20.40 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1.20 8 -17 4 7.00 1.00 9 8 4 5.20 0.90 14 -9 -4 1.10 0.80 -5 14 -4 1.30 0.50 14 -9 -4 0.80 0.70 -9 -5 -4 1.00 0.80 -9 -5 -4 1.00 0.80 -14 9 4 2.00 0.80 9 5 4 -0.50 0.70 9 5 4 -0.40 0.80 5 -14 4 -0.10 0.70 5 -14 4 1.30 0.60 11 -9 -4 207.08 9.90 11 -9 -4 203.28 9.70 -9 -2 -4 205.28 9.90 -9 -2 -4 201.88 9.90 -2 11 -4 198.38 9.80 9 2 4 203.98 9.80 9 2 4 204.38 9.80 2 -11 4 204.68 9.80 1 8 -4 356.66 17.10 8 -9 -4 378.96 17.20 -9 1 -4 355.06 17.20 -9 1 -4 364.16 17.10 -1 -8 4 344.47 17.10 -1 -8 4 357.36 17.10 9 -1 4 357.86 17.10 9 -1 4 359.76 17.10 4 5 -4 300.27 14.90 5 -9 -4 325.77 14.90 4 5 -4 303.77 14.90 -4 -5 4 309.77 14.90 9 -4 4 318.37 14.90 -4 -5 4 314.47 14.90 9 -4 4 316.27 14.90 7 2 -4 57.89 3.10 7 2 -4 57.79 3.10 -7 -2 4 62.69 3.20 9 -7 4 59.99 3.10 9 -7 4 65.29 3.20 -7 -2 4 61.89 3.20 9 -7 4 61.09 3.20 -1 -9 -4 18.20 1.20 -1 -9 -4 18.60 1.30 10 -1 -4 16.90 1.20 10 -1 -4 16.80 1.30 10 -1 -4 14.60 1.20 9 -10 4 15.60 1.30 -10 1 4 15.50 1.30 9 -10 4 18.30 1.30 1 9 4 16.60 1.20 -10 1 4 17.50 1.30 -4 -9 -4 8.10 0.90 13 -4 -4 7.50 0.90 13 -4 -4 8.40 0.90 -4 -9 -4 8.50 0.90 13 -4 -4 8.40 0.90 9 -13 4 8.80 1.00 4 9 4 8.70 0.80 -13 4 4 8.60 1.00 -13 4 4 8.50 0.90 9 -13 4 8.20 0.90 4 9 4 7.80 0.90 16 -7 -4 16.00 1.40 -7 -9 -4 17.10 1.50 16 -7 -4 17.70 1.50 -7 -9 -4 17.00 1.60 16 -7 -4 16.10 1.40 -16 7 4 15.50 1.40 9 -16 4 16.00 1.50 9 -16 4 18.00 1.50 7 9 4 14.70 1.40 7 9 4 16.20 1.40 19 -10 -4 13.30 1.40 -10 -9 -4 11.60 1.50 -10 -9 -4 11.90 1.50 19 -10 -4 13.50 1.50 9 -19 4 13.10 1.40 -19 10 4 13.10 1.50 9 -19 4 13.80 1.50 10 9 4 15.40 1.60 10 9 4 15.60 1.40 -10 -6 -4 13.30 1.30 16 -10 -4 15.20 1.40 16 -10 -4 13.20 1.30 -10 -6 -4 10.80 1.30 10 6 4 12.40 1.20 6 -16 4 13.60 1.20 -16 10 4 15.60 1.30 10 6 4 11.00 1.30 6 -16 4 11.30 1.10 13 -10 -4 84.59 4.00 -10 -3 -4 73.89 4.10 13 -10 -4 89.19 4.10 -10 -3 -4 76.59 4.10 -3 13 -4 76.89 3.90 3 -13 4 74.99 3.90 10 3 4 74.29 4.10 3 -13 4 79.49 3.90 3 -13 4 82.19 4.10 10 3 4 76.39 4.10 -10 0 -4 21.00 1.40 10 -10 -4 19.50 1.50 -10 0 -4 19.70 1.50 0 10 -4 21.10 1.40 10 0 4 17.20 1.40 0 -10 4 20.40 1.40 10 0 4 19.90 1.40 0 -10 4 23.50 1.50 10 0 4 19.60 1.50 7 -10 -4 459.95 22.30 -10 3 -4 477.75 22.30 3 7 -4 472.85 22.30 -10 3 -4 463.05 22.20 -3 -7 4 468.15 22.30 -3 -7 4 477.25 22.30 10 -3 4 450.75 22.20 10 -3 4 468.55 22.30 10 -3 4 473.15 22.30 6 4 -4 63.09 3.30 4 -10 -4 65.99 3.40 6 4 -4 63.39 3.40 -6 -4 4 67.09 3.40 10 -6 4 67.59 3.40 -6 -4 4 68.19 3.40 10 -6 4 67.69 3.40 1 -10 -4 19.10 1.30 9 1 -4 15.70 1.30 9 1 -4 20.10 1.40 1 -10 -4 19.20 1.30 10 -9 4 17.40 1.40 10 -9 4 18.80 1.40 -1 10 4 17.30 1.20 -9 -1 4 19.40 1.40 -9 -1 4 19.10 1.40 12 -2 -4 17.00 1.40 12 -2 -4 17.90 1.30 -2 -10 -4 16.30 1.30 12 -2 -4 16.80 1.30 -2 -10 -4 16.10 1.30 10 -12 4 18.90 1.40 -12 2 4 18.60 1.40 10 -12 4 16.10 1.40 2 10 4 17.80 1.30 -12 2 4 18.50 1.40 15 -5 -4 33.40 2.10 15 -5 -4 28.10 1.90 -5 -10 -4 30.30 2.00 -5 -10 -4 29.30 2.00 15 -5 -4 28.30 2.00 -15 5 4 29.90 1.90 -15 5 4 31.40 2.10 10 -15 4 32.30 2.00 5 10 4 29.30 1.90 10 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207.98 9.70 -2 -9 4 202.08 9.70 11 -2 4 200.38 9.70 6 -11 -4 11.00 1.00 5 6 -4 13.00 1.00 -11 5 -4 11.90 1.00 5 6 -4 12.60 1.10 -5 -6 4 12.70 1.10 11 -5 4 12.30 1.10 11 -5 4 12.40 1.10 11 -5 4 11.90 1.00 -5 -6 4 13.00 1.20 8 3 -4 29.10 1.70 8 3 -4 27.20 1.70 3 -11 -4 26.40 1.60 3 -11 -4 28.90 1.60 -8 -3 4 27.80 1.80 -8 -3 4 29.10 1.80 11 -8 4 27.10 1.80 0 -11 -4 77.69 4.00 11 0 -4 79.69 4.00 0 -11 -4 78.09 4.00 11 0 -4 75.99 3.90 11 0 -4 80.19 4.00 11 -11 4 76.69 4.10 -11 0 4 78.89 4.00 0 11 4 80.99 4.00 -11 0 4 77.79 4.10 11 -11 4 81.59 4.10 14 -3 -4 40.90 2.30 14 -3 -4 37.40 2.20 -3 -11 -4 36.50 2.20 14 -3 -4 39.40 2.20 -3 -11 -4 33.30 2.20 11 -14 4 38.60 2.30 -14 3 4 40.20 2.40 3 11 4 33.70 2.20 11 -14 4 35.60 2.30 -14 3 4 37.60 2.20 17 -6 -4 6.70 1.10 -6 -11 -4 10.70 1.20 -6 -11 -4 9.00 1.20 17 -6 -4 7.20 1.10 17 -6 -4 7.20 1.00 -17 6 4 6.90 1.00 6 11 4 8.20 1.10 11 -17 4 5.70 1.10 6 11 4 9.00 1.20 11 -17 4 6.10 1.10 -17 6 4 6.20 1.20 -9 -11 -4 3.10 1.20 -9 -11 -4 3.70 1.30 20 -9 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85.29 4.10 -4 -8 4 78.49 4.10 -4 -8 4 79.69 4.20 12 -4 4 81.99 4.10 12 -4 4 84.99 4.10 12 -4 4 81.09 4.10 7 5 -4 14.10 1.30 5 -12 -4 12.60 1.10 5 -12 -4 15.10 1.10 7 5 -4 15.00 1.20 12 -7 4 15.10 1.30 -7 -5 4 15.60 1.30 -7 -5 4 15.20 1.30 12 -7 4 14.40 1.20 2 -12 -4 16.80 1.30 10 2 -4 21.00 1.40 2 -12 -4 16.60 1.30 10 2 -4 19.90 1.50 -10 -2 4 18.70 1.50 12 -10 4 18.30 1.30 -2 12 4 17.40 1.30 -10 -2 4 21.30 1.50 12 -10 4 19.90 1.50 -1 -12 -4 1.80 0.70 -1 -12 -4 1.80 0.70 13 -1 -4 1.30 0.80 13 -1 -4 2.10 0.80 13 -1 -4 2.10 0.70 12 -13 4 0.50 0.70 12 -13 4 0.40 0.80 -13 1 4 1.30 0.80 -13 1 4 -0.10 0.70 1 12 4 2.00 0.70 -4 -12 -4 14.70 1.30 16 -4 -4 13.30 1.20 -4 -12 -4 14.10 1.30 16 -4 -4 14.40 1.30 16 -4 -4 13.90 1.40 12 -16 4 13.40 1.40 -16 4 4 13.10 1.40 4 12 4 14.80 1.30 12 -16 4 12.00 1.30 -16 4 4 13.30 1.20 19 -7 -4 38.00 2.50 19 -7 -4 38.30 2.50 -7 -12 -4 34.80 2.50 -7 -12 -4 32.80 2.50 7 12 4 30.20 2.50 12 -19 4 33.70 2.40 12 -19 4 31.60 2.30 -19 7 4 35.20 2.50 -19 7 4 34.20 2.40 22 -10 -4 1.90 1.30 -10 -12 -4 0.60 1.30 -10 -12 -4 0.70 1.30 22 -10 -4 0.60 1.40 10 12 4 1.70 1.40 -22 10 4 1.20 1.30 12 -22 4 0.20 1.70 12 -22 4 0.00 1.20 -13 -12 -4 9.80 1.80 -13 -12 -4 8.90 1.80 25 -13 -4 10.00 1.90 -25 13 4 5.60 1.70 13 12 4 10.40 1.80 22 -13 -4 10.90 1.60 -13 -9 -4 7.50 1.50 -13 -9 -4 9.50 1.60 13 9 4 7.50 1.40 -22 13 4 8.50 1.60 9 -22 4 8.50 1.40 13 9 4 6.10 1.50 19 -13 -4 45.30 3.00 -13 -6 -4 45.50 3.00 -13 -6 -4 51.99 3.10 13 6 4 49.20 2.90 -19 13 4 44.30 3.00 13 6 4 45.10 3.00 6 -19 4 42.10 2.90 -13 -3 -4 9.90 1.20 16 -13 -4 8.60 1.30 -3 16 -4 7.80 0.90 -13 -3 -4 9.00 1.20 13 3 4 9.40 1.20 13 3 4 7.60 1.20 3 -16 4 9.10 1.10 -13 0 -4 74.29 3.80 -13 0 -4 73.89 3.70 0 13 -4 67.39 3.60 13 -13 -4 68.09 3.70 13 0 4 74.39 3.70 13 0 4 74.69 3.70 13 0 4 68.89 3.60 0 -13 4 63.49 3.60 0 -13 4 61.39 3.60 3 10 -4 82.19 4.00 -13 3 -4 76.49 4.20 3 10 -4 88.69 4.20 -13 3 -4 77.89 4.20 10 -13 -4 77.99 4.20 10 -13 -4 72.69 4.10 13 -3 4 82.69 4.20 -3 -10 4 94.49 4.30 -3 -10 4 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22 38.60 2.20 9 1 -22 55.99 3.10 1 -10 -22 54.29 3.10 -10 9 -22 53.19 2.90 1 -10 -22 53.69 3.00 9 1 -22 52.49 3.10 9 1 -22 54.99 3.00 10 -9 22 51.59 2.90 10 -9 22 54.19 3.10 10 -9 22 53.79 3.10 -9 -1 22 54.69 3.00 12 -2 -22 8.40 1.10 -10 12 -22 7.80 1.00 12 -2 -22 7.30 1.10 12 -2 -22 5.50 1.10 12 -2 -22 7.00 1.20 -2 -10 -22 7.00 1.10 10 -12 22 6.50 1.10 10 -12 22 6.50 1.20 10 -12 22 7.60 0.90 -12 2 22 7.90 1.10 15 -5 -22 27.70 2.10 15 -5 -22 25.40 2.20 15 -5 -22 26.70 2.10 15 -5 -22 26.30 2.30 -5 -10 -22 22.50 2.00 -10 15 -22 29.10 2.30 -15 5 22 24.20 2.00 10 -15 22 30.10 2.20 10 -15 22 28.20 2.20 18 -8 -22 17.50 1.90 18 -8 -22 17.40 1.90 18 -8 -22 13.80 1.60 -8 -10 -22 14.20 1.80 10 -18 22 17.70 1.80 10 -18 22 15.10 1.80 8 10 22 19.10 1.70 -11 -10 -22 15.70 1.90 21 -11 -22 17.30 2.00 11 10 22 16.10 1.80 10 -21 22 19.50 2.00 11 10 22 14.10 1.90 18 -11 -22 10.40 1.50 18 -11 -22 5.40 1.50 -11 -7 -22 7.00 1.50 11 7 22 10.10 1.50 7 -18 22 10.60 1.60 15 -11 -22 9.30 1.30 -11 -4 -22 10.40 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7.30 1.20 -7 -6 -28 10.30 1.50 13 -7 -28 9.00 1.40 7 6 28 7.40 1.20 6 -13 28 6.00 1.40 6 -13 28 7.20 1.30 -3 10 -28 67.39 3.60 -3 10 -28 58.49 3.50 -7 -3 -28 63.29 3.70 10 -7 -28 65.49 3.70 -3 10 -28 66.09 3.70 10 -7 -28 66.49 3.60 10 -7 -28 64.19 3.50 10 -7 -28 63.99 3.70 -7 -3 -28 63.69 3.70 3 -10 28 69.29 3.70 7 3 28 65.19 3.60 3 -10 28 65.29 3.60 0 7 -28 8.40 1.10 0 7 -28 7.60 1.10 7 -7 -28 9.10 1.10 7 -7 -28 10.40 1.00 7 -7 -28 8.60 1.20 0 7 -28 8.30 1.10 -7 0 -28 7.20 1.10 7 -7 -28 8.60 1.10 -7 0 -28 6.90 1.10 0 -7 28 9.20 1.20 0 -7 28 9.90 1.20 7 0 28 7.30 1.20 -7 3 -28 57.49 3.10 3 4 -28 55.89 3.10 3 4 -28 52.89 3.10 3 4 -28 50.29 3.10 4 -7 -28 56.59 3.10 4 -7 -28 52.59 3.10 -7 3 -28 58.39 3.10 7 -3 28 57.09 3.20 7 -3 28 58.09 3.10 -3 -4 28 50.89 3.10 -3 -4 28 52.59 3.10 6 1 -28 45.60 2.60 1 -7 -28 41.30 2.60 1 -7 -28 40.70 2.60 6 1 -28 43.10 2.60 -7 6 -28 40.40 2.40 -7 6 -28 43.60 2.60 6 1 -28 42.20 2.50 7 -6 28 44.50 2.70 -6 -1 28 41.80 2.50 7 -6 28 42.40 2.50 -2 -7 -28 20.70 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5.40 8 1 28 105.59 5.40 1 -9 28 102.89 5.40 2 6 -28 29.00 1.90 6 -8 -28 24.80 2.00 6 -8 -28 27.00 1.90 2 6 -28 29.40 1.90 6 -8 -28 24.60 1.80 2 6 -28 26.10 2.00 -8 2 -28 26.20 1.90 -8 2 -28 24.60 2.00 8 -2 28 27.60 2.00 -2 -6 28 26.80 1.90 -2 -6 28 27.40 1.90 -8 5 -28 0.50 0.80 5 3 -28 2.70 1.00 3 -8 -28 1.40 0.90 -8 5 -28 2.40 0.90 3 -8 -28 1.40 0.90 5 3 -28 2.20 0.90 5 3 -28 1.40 0.90 8 -5 28 2.80 1.00 8 -5 28 1.50 0.90 -5 -3 28 2.30 0.80 8 0 -28 124.59 6.20 -8 8 -28 123.09 6.20 -8 8 -28 116.09 6.10 8 0 -28 113.29 6.20 8 0 -28 116.59 6.20 0 -8 -28 126.99 6.20 0 -8 -28 132.29 6.20 8 -8 28 125.39 6.20 8 -8 28 124.29 6.30 -8 0 28 117.89 6.10 11 -3 -28 86.49 4.50 11 -3 -28 81.89 4.50 11 -3 -28 89.39 4.60 -3 -8 -28 77.09 4.50 -3 -8 -28 77.19 4.50 11 -3 -28 87.59 4.50 -8 11 -28 85.29 4.50 -8 11 -28 89.19 4.50 8 -11 28 79.49 4.50 8 -11 28 85.09 4.60 3 8 28 82.69 4.50 14 -6 -28 27.40 2.30 -8 14 -28 28.80 2.40 -8 14 -28 26.40 2.20 14 -6 -28 29.60 2.20 14 -6 -28 29.30 2.40 -6 -8 -28 25.50 2.40 14 -6 -28 28.00 2.30 8 -14 28 26.40 2.20 8 -14 28 27.50 2.40 17 -9 -28 8.30 1.30 -9 -8 -28 10.40 1.60 17 -9 -28 9.10 1.60 17 -9 -28 7.40 1.50 8 -17 28 6.90 1.50 8 -17 28 6.20 1.50 9 8 28 11.40 1.50 14 -9 -28 21.10 2.00 -5 14 -28 19.90 1.70 -5 14 -28 18.20 1.70 14 -9 -28 19.10 1.60 -9 -5 -28 21.70 1.90 14 -9 -28 19.50 1.90 5 -14 28 20.70 1.80 9 5 28 24.60 1.90 5 -14 28 19.70 1.90 -2 11 -28 4.80 1.20 -9 -2 -28 9.20 1.30 11 -9 -28 4.70 1.00 -2 11 -28 4.50 1.00 -2 11 -28 5.20 1.10 11 -9 -28 6.40 1.10 -9 -2 -28 9.90 1.30 -9 -2 -28 11.10 1.20 11 -9 -28 6.70 1.30 11 -9 -28 6.20 1.30 2 -11 28 6.40 1.30 2 -11 28 4.20 1.10 9 2 28 7.20 1.20 8 -9 -28 109.49 5.50 8 -9 -28 104.79 5.50 8 -9 -28 99.99 5.40 8 -9 -28 97.39 5.30 -9 1 -28 112.29 5.50 1 8 -28 101.89 5.50 1 8 -28 107.29 5.50 -9 1 -28 110.49 5.50 1 8 -28 104.69 5.40 9 -1 28 105.39 5.50 -1 -8 28 109.79 5.50 -1 -8 28 105.89 5.40 -9 4 -28 2.60 1.00 4 5 -28 2.70 1.00 5 -9 -28 3.60 1.00 -9 4 -28 2.40 0.90 4 5 -28 2.50 0.90 4 5 -28 3.70 1.00 5 -9 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16 -10 -28 -0.90 1.30 16 -10 -28 -0.20 1.30 -10 -6 -28 1.80 1.30 6 -16 28 0.60 1.30 6 -16 28 1.90 1.20 10 6 28 0.70 1.30 -10 -3 -28 12.30 1.60 -3 13 -28 13.20 1.40 13 -10 -28 13.10 1.60 13 -10 -28 14.60 1.60 -10 -3 -28 14.10 1.60 -3 13 -28 12.40 1.50 -10 -3 -28 11.00 1.70 3 -13 28 11.80 1.60 10 3 28 16.30 1.60 3 -13 28 10.20 1.40 10 3 28 11.50 1.40 10 -10 -28 5.70 1.00 0 10 -28 4.80 1.10 0 10 -28 3.40 1.00 -10 0 -28 5.20 1.20 -10 0 -28 3.70 1.20 10 -10 -28 7.00 1.20 0 10 -28 5.70 1.20 10 -10 -28 6.40 1.30 0 -10 28 7.10 1.20 0 -10 28 6.10 1.10 10 0 28 1.20 1.10 10 0 28 5.10 1.20 3 7 -28 62.59 3.60 3 7 -28 65.49 3.80 3 7 -28 69.89 3.70 7 -10 -28 66.49 3.70 -10 3 -28 67.09 3.70 -10 3 -28 70.79 3.70 7 -10 -28 65.29 3.60 7 -10 -28 68.49 3.80 -3 -7 28 64.09 3.60 -3 -7 28 62.59 3.70 10 -3 28 61.19 3.70 -10 6 -28 33.80 2.20 4 -10 -28 28.10 2.20 6 4 -28 26.90 2.20 6 4 -28 27.50 2.20 4 -10 -28 33.70 2.10 6 4 -28 28.70 2.20 -10 6 -28 35.80 2.10 10 -6 28 31.10 2.20 10 -6 28 29.90 2.20 -6 -4 28 27.20 2.10 10 -6 28 29.40 2.30 9 1 -28 13.30 1.50 1 -10 -28 16.10 1.50 9 1 -28 14.70 1.60 9 1 -28 14.40 1.50 -10 9 -28 16.60 1.40 1 -10 -28 15.30 1.40 10 -9 28 13.40 1.60 10 -9 28 15.90 1.40 10 -9 28 15.80 1.60 -9 -1 28 15.00 1.40 -2 -10 -28 87.19 4.80 12 -2 -28 96.89 5.00 -2 -10 -28 86.69 4.90 12 -2 -28 96.19 4.90 12 -2 -28 91.79 4.80 -10 12 -28 91.69 4.80 12 -2 -28 98.59 4.90 2 10 28 82.29 4.80 10 -12 28 87.09 4.70 10 -12 28 93.19 4.90 10 -12 28 85.29 4.90 -12 2 28 94.49 4.80 15 -5 -28 6.10 1.30 -5 -10 -28 3.40 1.30 -10 15 -28 6.60 1.30 15 -5 -28 6.10 1.30 15 -5 -28 4.90 1.40 15 -5 -28 6.00 1.50 10 -15 28 6.90 1.40 10 -15 28 6.10 1.40 -8 -10 -28 9.80 1.70 18 -8 -28 9.00 1.80 18 -8 -28 7.80 1.40 18 -8 -28 10.30 1.70 10 -18 28 11.00 1.60 8 10 28 9.80 1.60 10 -18 28 9.00 1.70 21 -11 -28 4.30 1.70 21 -11 -28 8.10 1.90 -11 -10 -28 4.60 1.60 11 10 28 3.80 1.60 10 -21 28 3.30 1.70 11 10 28 4.40 1.60 -11 -7 -28 1.60 1.40 18 -11 -28 1.00 1.40 18 -11 -28 1.00 1.40 11 7 28 -1.50 1.30 7 -18 28 -0.50 1.40 -4 15 -28 7.50 1.40 -11 -4 -28 6.90 1.50 15 -11 -28 6.60 1.40 15 -11 -28 4.60 1.40 -4 15 -28 5.90 1.50 4 -15 28 9.10 1.50 11 4 28 7.20 1.50 -1 12 -28 50.09 3.30 -11 -1 -28 52.39 3.20 12 -11 -28 52.69 3.20 -1 12 -28 53.69 3.20 -11 -1 -28 48.70 3.10 12 -11 -28 55.29 3.30 -11 -1 -28 55.79 3.20 -1 12 -28 51.79 3.10 1 -12 28 47.00 3.00 1 -12 28 51.59 3.20 11 1 28 51.09 3.20 11 1 28 48.30 3.10 -11 2 -28 9.00 1.30 2 9 -28 4.70 1.10 2 9 -28 6.80 1.30 9 -11 -28 8.20 1.10 2 9 -28 5.40 1.10 9 -11 -28 9.30 1.30 9 -11 -28 6.60 1.20 -11 2 -28 6.40 1.20 11 -2 28 7.40 1.30 -2 -9 28 4.70 1.20 11 -2 28 9.20 1.30 -2 -9 28 4.10 1.10 -11 5 -28 157.28 7.70 5 6 -28 159.48 7.80 6 -11 -28 147.19 7.70 5 6 -28 153.58 7.70 -11 5 -28 154.78 7.70 6 -11 -28 149.29 7.60 5 6 -28 156.08 7.70 6 -11 -28 154.18 7.70 11 -5 28 155.88 7.80 -5 -6 28 155.88 7.70 -5 -6 28 146.29 7.60 11 -5 28 155.38 7.70 -11 8 -28 81.99 4.50 8 3 -28 86.09 4.60 3 -11 -28 87.19 4.60 8 3 -28 89.49 4.70 8 3 -28 88.89 4.70 3 -11 -28 85.99 4.60 -8 -3 28 91.79 4.60 11 -8 28 80.99 4.50 11 -8 28 85.99 4.70 11 -8 28 79.89 4.70 11 0 -28 33.40 2.50 11 0 -28 32.60 2.50 0 -11 -28 30.20 2.40 0 -11 -28 32.40 2.40 -11 11 -28 31.20 2.20 11 0 -28 33.10 2.40 -11 0 28 29.80 2.30 11 -11 28 28.80 2.20 11 -11 28 30.60 2.40 11 -11 28 31.10 2.40 -3 -11 -28 3.50 1.30 14 -3 -28 3.70 1.30 14 -3 -28 2.60 1.20 14 -3 -28 5.90 1.30 14 -3 -28 4.60 1.40 11 -14 28 3.80 1.30 11 -14 28 7.50 1.50 17 -6 -28 6.80 1.50 17 -6 -28 4.60 1.40 17 -6 -28 5.00 1.30 -6 -11 -28 6.10 1.50 17 -6 -28 8.00 1.60 11 -17 28 6.20 1.50 11 -17 28 7.70 1.60 20 -9 -28 7.50 1.70 20 -9 -28 7.50 1.50 -9 -11 -28 7.70 1.70 20 -9 -28 6.90 1.70 11 -20 28 4.80 1.60 11 -20 28 6.80 1.70 9 11 28 9.30 1.70 -12 -11 -28 5.70 1.80 23 -12 -28 3.50 1.80 12 11 28 3.40 1.70 11 -23 28 5.00 1.90 12 11 28 3.60 1.70 -12 -8 -28 0.60 1.50 20 -12 -28 0.10 1.60 20 -12 -28 0.00 1.60 12 8 28 2.00 1.50 8 -20 28 -1.50 1.50 -12 -5 -28 8.60 1.60 17 -12 -28 6.90 1.50 17 -12 -28 8.60 1.70 12 5 28 8.80 1.60 5 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54 2.90 1.70 7 -5 54 2.50 1.80 -2 7 54 4.00 1.80 -1 -7 -54 0.80 1.60 -1 -7 -54 1.60 1.90 -7 8 -54 -0.90 1.60 8 -1 -54 2.50 1.60 8 -1 -54 -0.20 1.40 8 -1 -54 4.90 1.90 1 7 54 0.50 1.80 7 -8 54 4.80 1.80 -8 1 54 2.80 1.80 7 -8 -54 3.70 2.00 -8 1 -54 1.90 1.70 1 7 -54 1.00 1.70 7 -8 -54 1.20 1.50 -8 1 -54 2.30 1.80 1 7 -54 1.80 1.50 1 7 -54 1.60 1.70 -7 8 54 1.30 1.80 8 -1 54 1.40 1.70 -1 -7 54 0.90 1.70 4 -8 -54 4.40 2.00 -8 4 -54 3.40 2.00 4 4 -54 5.20 1.70 4 4 -54 4.10 1.60 4 4 -54 4.60 1.90 4 -8 -54 4.30 1.70 -8 4 -54 4.10 1.80 -4 8 54 4.20 1.90 8 -4 54 4.30 1.80 -4 -4 54 3.40 1.80 7 1 -54 2.20 2.00 -8 7 -54 1.60 1.70 1 -8 -54 2.10 1.70 1 -8 -54 0.00 1.90 7 1 -54 2.20 1.50 7 1 -54 -1.50 1.50 -1 8 54 1.00 1.70 -7 -1 54 1.70 1.70 8 -7 54 -0.20 1.70 3 6 -54 0.80 1.60 -9 3 -54 -1.40 1.60 3 6 -54 2.70 1.70 -9 3 -54 0.90 1.60 3 6 -54 1.50 1.80 6 -9 -54 0.50 2.00 6 -9 -54 0.00 1.50 -6 9 54 1.00 1.80 9 -3 54 0.90 1.70 -3 -6 54 -0.60 1.80 6 3 -54 0.10 1.60 3 -9 -54 3.20 1.60 6 3 -54 0.10 1.70 6 3 -54 -0.40 1.80 -9 6 -54 1.00 1.70 3 -9 -54 2.30 2.00 9 -6 54 0.30 1.80 -3 9 54 -1.30 1.70 -6 -3 54 -2.00 1.60 1 -1 -55 -0.40 1.50 -1 0 -55 2.10 1.60 0 1 -55 -3.00 1.70 1 -1 -55 -0.30 1.80 0 1 -55 0.80 1.50 -1 0 -55 1.80 1.80 -1 1 55 -0.90 1.60 1 0 55 0.80 1.70 0 -1 55 3.00 1.80 3 -2 -55 1.10 1.50 3 -2 -55 0.00 1.80 -1 3 -55 -1.40 1.70 -1 3 -55 2.40 1.60 -2 -1 -55 -2.10 1.80 -2 -1 -55 -1.10 1.60 -3 2 55 -1.70 1.70 1 -3 55 -1.90 1.60 2 1 55 0.10 1.70 0 -2 -55 -0.40 1.60 2 0 -55 1.70 1.80 2 0 -55 -2.70 1.50 2 0 -55 0.20 1.40 -2 2 -55 6.20 1.90 -2 2 -55 -0.80 1.50 0 -2 -55 2.40 1.90 -2 0 55 -0.40 1.70 2 -2 55 -1.80 1.60 0 2 55 0.70 1.70 5 -3 -55 0.00 1.60 5 -3 -55 -0.50 1.40 -3 -2 -55 -0.30 1.80 -2 5 -55 -0.10 1.60 -2 5 -55 -1.00 1.50 -3 -2 -55 -0.60 1.60 5 -3 -55 1.20 1.80 3 2 55 0.80 1.70 -5 3 55 0.30 1.70 2 -5 55 -3.20 1.60 1 2 -55 -1.60 1.40 2 -3 -55 1.30 1.60 1 2 -55 -0.40 1.70 -3 1 -55 1.70 1.80 -3 1 -55 1.50 1.60 1 2 -55 0.40 1.40 2 -3 -55 -2.20 1.70 -1 -2 55 0.40 1.70 3 -1 55 0.80 1.70 -2 3 55 0.70 1.70 4 -1 -55 2.80 1.80 -3 4 -55 -1.90 1.60 -1 -3 -55 0.90 1.80 -1 -3 -55 0.20 1.60 -3 4 -55 3.50 1.70 4 -1 -55 1.30 1.60 4 -1 -55 -0.90 1.40 3 -4 55 3.70 1.80 1 3 55 2.50 1.80 -4 1 55 1.40 1.80 7 -4 -55 0.40 1.40 -3 7 -55 1.30 1.50 -4 -3 -55 2.70 1.80 -3 7 -55 -0.20 1.60 7 -4 -55 4.10 1.90 -4 -3 -55 2.70 1.70 7 -4 -55 -1.00 1.50 3 -7 55 1.20 1.70 -7 4 55 1.90 1.80 4 3 55 0.70 1.70 0 4 -55 -0.30 1.40 0 4 -55 -0.10 1.60 4 -4 -55 0.40 1.50 0 4 -55 1.90 1.70 -4 0 -55 -0.40 1.80 4 -4 -55 0.30 1.80 -4 0 -55 -1.40 1.60 4 0 55 -2.70 1.60 0 -4 55 -0.30 1.70 -4 4 55 0.70 1.70 1 -4 -55 2.60 1.90 3 1 -55 0.80 1.60 -4 3 -55 -0.90 1.70 3 1 -55 0.30 1.40 1 -4 -55 0.00 1.60 3 1 -55 1.20 1.80 -4 3 -55 1.40 1.70 -1 4 55 1.60 1.70 4 -3 55 2.30 1.70 -3 -1 55 0.00 1.70 -4 6 -55 3.60 1.70 6 -2 -55 -0.30 1.40 -2 -4 -55 1.30 1.90 6 -2 -55 5.60 1.90 -2 -4 -55 0.50 1.60 6 -2 -55 -0.50 1.60 4 -6 55 2.00 1.80 2 4 55 -0.30 1.70 -6 2 55 2.90 1.80 -1 6 -55 1.80 1.70 -1 6 -55 2.10 1.60 -5 -1 -55 2.40 1.60 -5 -1 -55 5.40 1.90 6 -5 -55 -0.10 1.50 -1 6 -55 3.40 1.80 6 -5 -55 2.40 1.90 1 -6 55 3.70 1.80 -6 5 55 0.60 1.70 5 1 55 0.90 1.70 3 -5 -55 -1.20 1.50 -5 2 -55 -0.60 1.60 2 3 -55 0.70 1.60 2 3 -55 0.50 1.40 -5 2 -55 -0.70 1.70 2 3 -55 -0.10 1.70 3 -5 -55 0.80 1.80 -3 5 55 0.40 1.70 -2 -3 55 1.20 1.70 5 -2 55 -1.50 1.70 5 0 -55 0.10 1.40 -5 5 -55 -0.60 1.60 5 0 -55 -2.30 1.50 0 -5 -55 -0.80 1.60 -5 5 -55 0.10 1.60 0 -5 -55 1.40 1.90 5 0 -55 -3.40 1.70 -5 0 55 2.40 1.80 0 5 55 0.90 1.70 5 -5 55 0.20 1.80 -3 -5 -55 5.90 1.90 8 -3 -55 5.50 1.80 8 -3 -55 9.50 2.10 8 -3 -55 7.20 1.60 -3 -5 -55 4.80 2.00 -5 8 -55 8.00 1.90 -2 8 -55 -0.10 1.60 -6 -2 -55 0.40 1.70 8 -6 -55 1.90 1.60 -6 1 -55 4.30 1.70 -6 1 -55 4.30 1.90 5 -6 -55 2.60 1.60 1 5 -55 2.00 1.80 5 -6 -55 4.20 2.00 1 5 -55 4.50 1.80 1 5 -55 2.90 1.50 -5 6 55 1.10 1.80 6 -1 55 4.10 1.80 -1 -5 55 2.00 1.70 -6 4 -55 0.40 1.70 2 -6 -55 1.20 1.60 4 2 -55 0.60 1.50 -6 4 -55 2.60 1.70 2 -6 -55 5.10 2.00 4 2 -55 4.50 1.70 4 2 -55 2.30 1.80 -2 6 55 4.50 1.80 -4 -2 55 0.80 1.70 6 -4 55 0.30 1.70 7 -1 -55 3.20 1.50 -1 -6 -55 2.40 2.00 -6 7 -55 4.10 1.70 7 -1 -55 3.30 1.70 7 -1 -55 4.60 2.00 -1 -6 -55 5.00 1.70 1 6 55 1.80 1.80 -7 1 55 1.90 1.80 6 -7 55 2.60 1.70 0 7 -55 0.00 1.50 -7 0 -55 -0.40 1.70 7 -7 -55 -0.90 1.60 7 -7 -55 -2.10 1.90 0 7 -55 1.60 1.70 -7 0 -55 1.50 1.80 0 7 -55 1.40 1.80 3 4 -55 1.80 1.60 3 4 -55 0.00 1.80 -7 3 -55 1.70 1.80 4 -7 -55 -1.20 1.90 3 4 -55 2.10 1.60 -7 3 -55 0.40 1.70 4 -7 -55 -0.20 1.50 -3 -4 55 2.00 1.70 -4 7 55 1.50 1.80 7 -3 55 0.30 1.70 1 -7 -55 -0.80 1.60 1 -7 -55 6.80 2.00 6 1 -55 3.90 1.70 -7 6 -55 3.70 1.80 6 1 -55 1.00 1.50 6 1 -55 2.90 1.90 -6 -1 55 1.70 1.80 7 -6 55 1.80 1.80 -1 7 55 2.00 1.80 2 6 -55 3.40 1.70 6 -8 -55 3.10 1.60 2 6 -55 2.00 1.80 -8 2 -55 -0.10 1.70 5 3 -55 7.70 1.80 5 3 -55 4.40 2.00 3 -8 -55 3.50 1.70 -8 5 -55 9.20 1.90 3 -8 -55 2.90 2.00 5 3 -55 6.50 1.70 1 0 -56 10.20 2.10 0 -1 -56 5.50 1.80 0 -1 -56 9.20 2.00 -1 1 -56 6.00 1.80 -1 1 -56 10.60 2.00 1 0 -56 4.40 1.70 -1 0 56 11.10 2.00 0 1 56 5.50 1.90 1 -1 56 5.30 1.90 2 -2 -56 19.20 2.40 2 -2 -56 17.30 2.20 0 2 -56 23.50 2.50 -2 0 -56 21.60 2.50 0 2 -56 16.80 2.20 -2 0 -56 18.20 2.30 0 -2 56 17.40 2.30 -2 2 56 13.90 2.20 2 0 56 15.30 2.30 -1 -2 -56 4.10 1.90 3 -1 -56 5.80 1.80 -1 -2 -56 3.00 1.60 -2 3 -56 7.40 1.90 3 -1 -56 7.60 2.00 -2 3 -56 1.70 1.70 2 -3 56 3.10 1.80 1 2 56 2.20 1.90 -3 1 56 3.80 1.80 -3 -1 -56 2.20 1.70 -3 -1 -56 5.30 2.00 -1 4 -56 4.30 1.90 4 -3 -56 1.70 1.90 -1 4 -56 4.60 1.70 4 -3 -56 1.70 1.60 3 1 56 4.80 1.80 1 -4 56 2.60 1.80 -4 3 56 0.30 1.80 2 1 -56 2.60 1.60 2 1 -56 0.20 1.40 1 -3 -56 3.80 1.80 -3 2 -56 4.70 2.00 1 -3 -56 1.70 1.90 2 1 -56 6.10 1.90 -3 2 -56 1.20 1.70 3 -2 56 3.10 1.80 -2 -1 56 3.30 1.80 -1 3 56 4.40 1.80 -3 5 -56 4.00 1.80 -2 -3 -56 1.60 1.70 -2 -3 -56 7.10 2.10 5 -2 -56 4.00 1.60 5 -2 -56 1.70 1.50 5 -2 -56 2.40 1.80 -3 5 -56 1.50 1.80 2 3 56 2.50 1.80 -5 2 56 2.70 1.80 3 -5 56 3.50 1.80 6 -4 -56 0.10 1.60 6 -4 -56 4.10 2.00 -4 -2 -56 1.90 1.70 -2 6 -56 3.00 1.80 -2 6 -56 1.80 1.70 -4 -2 -56 2.90 1.90 -4 1 -56 5.30 1.80 1 3 -56 3.80 1.90 -4 1 -56 2.30 1.80 3 -4 -56 4.80 1.70 3 -4 -56 2.10 1.90 1 3 -56 4.40 1.60 1 3 -56 3.70 1.60 -1 -3 56 5.50 1.90 -3 4 56 2.70 1.80 4 -1 56 3.30 1.80 0 -4 -56 3.20 1.90 -4 4 -56 5.20 1.70 0 -4 -56 7.00 1.80 4 0 -56 5.80 1.60 -4 4 -56 5.50 1.90 4 0 -56 4.40 1.70 4 0 -56 5.70 2.00 0 4 56 4.20 1.90 -4 0 56 2.40 1.80 4 -4 56 3.70 1.80 -5 0 -56 10.50 1.90 5 -5 -56 10.10 1.80 5 -5 -56 13.00 2.20 0 5 -56 5.90 1.70 0 5 -56 7.10 1.80 0 5 -56 7.40 2.00 -5 0 -56 8.20 2.00 -5 5 56 6.50 2.00 0 -5 56 7.90 1.90 5 0 56 9.90 2.10 -5 3 -56 -0.10 1.70 3 2 -56 3.60 1.60 2 -5 -56 1.70 1.90 2 -5 -56 -0.20 1.50 3 2 -56 4.40 1.70 3 2 -56 1.70 1.90 -5 3 -56 3.40 1.70 -2 5 56 3.70 1.80 5 -3 56 2.20 1.80 -3 -2 56 5.60 1.80 6 -1 -56 5.50 1.80 -1 -5 -56 5.00 1.80 -5 6 -56 7.40 1.80 4 -6 -56 1.50 1.60 2 4 -56 2.90 1.90 2 4 -56 1.20 1.60 4 -6 -56 3.70 1.90 -6 2 -56 -0.20 1.60 -6 2 -56 0.60 1.80 5 1 -56 7.60 1.80 -6 5 -56 8.30 1.90 1 -6 -56 5.00 1.80 0 0 -57 -1.00 1.50 0 0 -57 0.50 1.90 0 0 57 -1.30 1.70 -1 2 -57 0.30 1.60 -1 -1 -57 3.50 2.00 -1 -1 -57 1.80 1.70 2 -1 -57 5.70 1.80 2 -1 -57 4.00 1.90 -1 2 -57 4.20 1.90 -2 1 57 3.10 1.80 1 -2 57 2.70 1.80 1 1 57 1.70 1.80 -2 1 -57 4.20 1.80 1 -2 -57 3.80 2.00 -2 1 -57 0.70 1.90 1 1 -57 0.40 1.90 1 1 -57 3.00 1.60 1 -2 -57 2.60 1.70 -1 -1 57 5.10 1.80 2 -1 57 2.20 1.80 -1 2 57 0.20 1.80 0 3 -57 2.20 1.70 -3 0 -57 -0.80 1.70 3 -3 -57 0.20 1.60 -3 3 -57 0.90 1.60 0 -3 -57 -1.10 1.60 3 0 -57 -0.30 1.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 14604 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' 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 C1 C 0.7079(3) 0.5924(3) 0.26381(9) 0.0573(12) Uani 1 1 d . . . . . H1A H 0.6740 0.5473 0.2546 0.086 Uiso 1 1 calc GR . . . . H1B H 0.7556 0.6038 0.2582 0.086 Uiso 1 1 calc GR . . . . H1C H 0.6992 0.6292 0.2560 0.086 Uiso 1 1 calc GR . . . . N1 N 0.69177(17) 0.47944(17) 0.39427(7) 0.0366(7) Uani 1 1 d . . . . . H1 H 0.6976 0.4472 0.4037 0.044 Uiso 1 1 calc R . . . . O1 O 0.70071(19) 0.58817(17) 0.29691(6) 0.0527(8) Uani 1 1 d . . . . . C2 C 0.7106(2) 0.5389(2) 0.31197(8) 0.0396(8) Uani 1 1 d . . . . . N2 N 0.66816(17) 0.49982(18) 0.44333(7) 0.0372(7) Uani 1 1 d . . . . . H2 H 0.6844 0.4716 0.4478 0.045 Uiso 1 1 calc R . . . . O2 O 0.65665(18) 0.56091(17) 0.40312(6) 0.0480(7) Uani 1 1 d . . . . . C3 C 0.7295(2) 0.4945(2) 0.29781(9) 0.0447(9) Uani 1 1 d . . . . . H3 H 0.7377 0.4967 0.2760 0.054 Uiso 1 1 calc R . . . . N3 N 0.60331(19) 0.45203(18) 0.54827(7) 0.0409(7) Uani 1 1 d . . . . . H3A H 0.6095 0.4167 0.5434 0.049 Uiso 1 1 calc R . . . . O3 O 0.57165(18) 0.49673(17) 0.58903(6) 0.0492(7) Uani 1 1 d . . . . . C4 C 0.7363(2) 0.4464(2) 0.31630(10) 0.0460(10) Uani 1 1 d . . . . . H4 H 0.7491 0.4154 0.3069 0.055 Uiso 1 1 calc R . . . . N4 N 0.58693(18) 0.40199(19) 0.59550(7) 0.0429(8) Uani 1 1 d . . . . . H4A H 0.6031 0.3778 0.5857 0.051 Uiso 1 1 calc R . . . . O4 O 0.4951(3) 0.4198(3) 0.69674(9) 0.0850(14) Uani 1 1 d . . . . . C5 C 0.7248(2) 0.4425(2) 0.34801(9) 0.0418(9) Uani 1 1 d . . . . . H5 H 0.7305 0.4097 0.3602 0.050 Uiso 1 1 calc R . . . . C6 C 0.70479(19) 0.4874(2) 0.36202(8) 0.0346(7) Uani 1 1 d . . . . . C7 C 0.6985(2) 0.5355(2) 0.34406(8) 0.0381(8) Uani 1 1 d . . . . . H7 H 0.6859 0.5667 0.3535 0.046 Uiso 1 1 calc R . . . . C8 C 0.6708(2) 0.5170(2) 0.41263(8) 0.0357(8) Uani 1 1 d . . . . . C9 C 0.64307(19) 0.5209(2) 0.46885(8) 0.0333(7) Uani 1 1 d . . . . . C10 C 0.6301(2) 0.5767(2) 0.46940(8) 0.0407(9) Uani 1 1 d . . . . . H10 H 0.6351 0.6031 0.4511 0.049 Uiso 1 1 calc R . . . . C11 C 0.6097(2) 0.5928(2) 0.49739(9) 0.0430(9) Uani 1 1 d . . . . . H11 H 0.6017 0.6314 0.4980 0.052 Uiso 1 1 calc R . . . . C12 C 0.6004(2) 0.5543(2) 0.52471(8) 0.0415(9) Uani 1 1 d . . . . . H12 H 0.5863 0.5664 0.5435 0.050 Uiso 1 1 calc R . . . . C13 C 0.6123(2) 0.4983(2) 0.52356(8) 0.0369(8) Uani 1 1 d . . . . . C14 C 0.6335(2) 0.4824(2) 0.49576(8) 0.0344(7) Uani 1 1 d . . . . . H14 H 0.6418 0.4440 0.4952 0.041 Uiso 1 1 calc R . . . . C15 C 0.5863(2) 0.4545(2) 0.57880(8) 0.0395(8) Uani 1 1 d . . . . . C16 C 0.5649(2) 0.3817(2) 0.62657(8) 0.0433(9) Uani 1 1 d . . . . . C17 C 0.5406(2) 0.4156(3) 0.64563(9) 0.0492(10) Uani 1 1 d . . . . . H17 H 0.5381 0.4551 0.6384 0.059 Uiso 1 1 calc R . . . . C18 C 0.5197(3) 0.3901(3) 0.67594(11) 0.0631(14) Uani 1 1 d . . . . . C19 C 0.5226(4) 0.3330(4) 0.68657(13) 0.082(2) Uani 1 1 d . . . . . H19 H 0.5081 0.3164 0.7072 0.099 Uiso 1 1 calc R . . . . C20 C 0.5466(3) 0.2999(4) 0.66733(12) 0.0712(16) Uani 1 1 d . . . . . H20 H 0.5479 0.2598 0.6746 0.085 Uiso 1 1 calc R . . . . C21 C 0.5690(3) 0.3241(3) 0.63752(10) 0.0508(10) Uani 1 1 d . . . . . H21 H 0.5870 0.3018 0.6246 0.061 Uiso 1 1 calc R . . . . C22 C 0.4962(4) 0.4826(4) 0.68764(13) 0.0811(19) Uani 1 1 d . . . . . H22A H 0.5439 0.5178 0.6815 0.122 Uiso 1 1 calc GR . . . . H22B H 0.4812 0.5005 0.7051 0.122 Uiso 1 1 calc GR . . . . H22C H 0.4642 0.4727 0.6700 0.122 Uiso 1 1 calc GR . . . . N5 N 0.39252(18) 0.26832(18) 0.50915(8) 0.0411(7) Uani 1 1 d . . . . . C23 C 0.4415(5) 0.3582(4) 0.39725(13) 0.089(2) Uani 1 1 d . . . . . H23A H 0.4795 0.3801 0.3820 0.134 Uiso 1 1 calc GR . . . . H23B H 0.4213 0.3885 0.4007 0.134 Uiso 1 1 calc GR . . . . H23C H 0.4050 0.3126 0.3894 0.134 Uiso 1 1 calc GR . . . . C24 C 0.4705(4) 0.3479(4) 0.42808(12) 0.0691(16) Uani 1 1 d . . . . . H24A H 0.4935 0.3198 0.4243 0.083 Uiso 1 1 calc R . . . . H24B H 0.5063 0.3942 0.4363 0.083 Uiso 1 1 calc R . . . . C25 C 0.4120(3) 0.3109(3) 0.45209(10) 0.0517(10) Uani 1 1 d . . . . . H25A H 0.3909 0.3403 0.4570 0.062 Uiso 1 1 calc R . . . . H25B H 0.3748 0.2656 0.4436 0.062 Uiso 1 1 calc R . . . . C26 C 0.4424(2) 0.2980(2) 0.48139(10) 0.0463(9) Uani 1 1 d . . . . . H26A H 0.4836 0.3430 0.4878 0.056 Uiso 1 1 calc R . . . . H26B H 0.4594 0.2652 0.4763 0.056 Uiso 1 1 calc R . . . . C27 C 0.4328(2) 0.2552(2) 0.53435(9) 0.0442(9) Uani 1 1 d . . . . . H27A H 0.4778 0.2992 0.5376 0.053 Uiso 1 1 calc R . . . . H27B H 0.4440 0.2196 0.5266 0.053 Uiso 1 1 calc R . . . . C28 C 0.3969(2) 0.2307(3) 0.56580(9) 0.0469(9) Uani 1 1 d . . . . . H28A H 0.3467 0.1955 0.5628 0.056 Uiso 1 1 calc R . . . . H28B H 0.3998 0.2709 0.5774 0.056 Uiso 1 1 calc R . . . . C29 C 0.4327(3) 0.1984(3) 0.58425(10) 0.0518(10) Uani 1 1 d . . . . . H29A H 0.4275 0.1569 0.5729 0.062 Uiso 1 1 calc R . . . . H29B H 0.4835 0.2329 0.5857 0.062 Uiso 1 1 calc R . . . . C30 C 0.4031(3) 0.1763(3) 0.61683(11) 0.0642(13) Uani 1 1 d . . . . . H30A H 0.3519 0.1480 0.6158 0.096 Uiso 1 1 calc GR . . . . H30B H 0.4166 0.2181 0.6296 0.096 Uiso 1 1 calc GR . . . . H30C H 0.4218 0.1484 0.6262 0.096 Uiso 1 1 calc GR . . . . C31 C 0.3843(4) 0.4207(4) 0.5743(2) 0.103(3) Uani 1 1 d . . . . . H31A H 0.3487 0.3709 0.5759 0.154 Uiso 1 1 calc GR . . . . H31B H 0.3655 0.4493 0.5827 0.154 Uiso 1 1 calc GR . . . . H31C H 0.4261 0.4297 0.5861 0.154 Uiso 1 1 calc GR . . . . C32 C 0.4035(4) 0.4393(3) 0.54095(18) 0.0808(18) Uani 1 1 d . . . . . H32A H 0.4403 0.4893 0.5395 0.097 Uiso 1 1 calc R . . . . H32B H 0.3619 0.4331 0.5294 0.097 Uiso 1 1 calc R . . . . C33 C 0.4299(3) 0.3945(3) 0.52618(13) 0.0615(12) Uani 1 1 d . . . . . H33A H 0.4646 0.3925 0.5402 0.074 Uiso 1 1 calc R . . . . H33B H 0.4538 0.4163 0.5064 0.074 Uiso 1 1 calc R . . . . C34 C 0.3701(2) 0.3200(2) 0.51980(11) 0.0481(10) Uani 1 1 d . . . . . H34A H 0.3420 0.3016 0.5390 0.058 Uiso 1 1 calc R . . . . H34B H 0.3392 0.3222 0.5037 0.058 Uiso 1 1 calc R . . . . C35 C 0.3260(2) 0.2015(2) 0.50069(9) 0.0422(9) Uani 1 1 d . . . . . H35A H 0.3015 0.2125 0.4842 0.051 Uiso 1 1 calc R . . . . H35B H 0.2950 0.1854 0.5192 0.051 Uiso 1 1 calc R . . . . C36 C 0.3356(3) 0.1411(2) 0.48939(11) 0.0523(10) Uani 1 1 d . . . . . H36A H 0.3516 0.1233 0.5069 0.063 Uiso 1 1 calc R . . . . H36B H 0.3719 0.1581 0.4729 0.063 Uiso 1 1 calc R . . . . C37 C 0.2665(3) 0.0822(3) 0.47661(12) 0.0603(12) Uani 1 1 d . . . . . H37A H 0.2699 0.0392 0.4746 0.072 Uiso 1 1 calc R . . . . H37B H 0.2286 0.0723 0.4917 0.072 Uiso 1 1 calc R . . . . C38 C 0.2470(4) 0.0987(3) 0.44565(13) 0.084(2) Uani 1 1 d . . . . . H38A H 0.2847 0.1095 0.4307 0.127 Uiso 1 1 calc GR . . . . H38B H 0.2402 0.1392 0.4477 0.127 Uiso 1 1 calc GR . . . . H38C H 0.2034 0.0581 0.4383 0.127 Uiso 1 1 calc GR . . . . Cl1 Cl 0.64694(17) 0.39731(16) 0.73564(6) 0.0691(7) Uani 0.5 1 d . . . . . P2 P 0.6667 0.3333 0.53579(4) 0.0385(4) Uani 1 3 d S T P . . O7 O 0.59827(15) 0.32783(15) 0.52279(6) 0.0401(6) Uani 1 1 d D . . . . H7A H 0.5955 0.3196 0.5036 0.060 Uiso 0.5 1 calc DGR . . A 1 O8 O 0.6667 0.3333 0.57049(11) 0.0449(11) Uani 1 3 d S T P . . P1 P 0.6667 0.3333 0.45021(4) 0.0339(3) Uani 1 3 d S T P . . O5 O 0.6667 0.3333 0.41562(10) 0.0401(11) Uani 1 3 d S T P . . O6 O 0.59250(14) 0.31122(14) 0.46326(6) 0.0384(6) Uani 1 1 d D . . . . H6 H 0.5935 0.3108 0.4828 0.058 Uiso 0.5 1 calc DGR . . B 2 C39 C 0.6667 0.3333 0.7230(4) 0.068(5) Uani 0.5 3 d S T P . . H39 H 0.6667 0.3333 0.6997 0.082 Uiso 0.5 3 calc RS T P . . 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 C1 0.082(3) 0.063(3) 0.0243(17) 0.0118(17) 0.0176(19) 0.034(3) N1 0.0448(17) 0.0459(18) 0.0281(13) 0.0026(12) 0.0029(12) 0.0294(15) O1 0.083(2) 0.0566(18) 0.0256(12) 0.0093(12) 0.0167(13) 0.0403(17) C2 0.048(2) 0.040(2) 0.0283(16) 0.0053(14) 0.0114(15) 0.0204(17) N2 0.0493(18) 0.0488(18) 0.0242(13) 0.0001(12) 0.0000(13) 0.0326(16) O2 0.074(2) 0.0655(19) 0.0266(12) 0.0048(12) 0.0068(13) 0.0510(17) C3 0.050(2) 0.045(2) 0.0296(17) -0.0038(15) 0.0123(16) 0.0159(19) N3 0.056(2) 0.0466(19) 0.0246(13) -0.0009(13) 0.0030(13) 0.0290(17) O3 0.067(2) 0.0651(19) 0.0263(12) 0.0031(12) 0.0077(12) 0.0416(17) C4 0.054(2) 0.042(2) 0.041(2) -0.0036(17) 0.0117(18) 0.0237(19) N4 0.0491(19) 0.056(2) 0.0246(14) 0.0008(14) 0.0022(13) 0.0269(17) O4 0.121(4) 0.125(4) 0.0501(19) 0.040(2) 0.047(2) 0.092(3) C5 0.046(2) 0.039(2) 0.0414(19) 0.0004(16) 0.0071(16) 0.0217(18) C6 0.0342(18) 0.0394(19) 0.0270(15) -0.0024(14) 0.0037(13) 0.0159(15) C7 0.046(2) 0.044(2) 0.0281(16) 0.0037(14) 0.0087(14) 0.0254(18) C8 0.0397(19) 0.047(2) 0.0256(15) 0.0023(14) 0.0016(13) 0.0257(17) C9 0.0340(18) 0.047(2) 0.0242(15) -0.0042(13) -0.0018(13) 0.0238(16) C10 0.050(2) 0.055(2) 0.0278(17) 0.0009(15) -0.0011(15) 0.035(2) C11 0.056(2) 0.056(2) 0.0323(17) -0.0008(17) 0.0006(16) 0.040(2) C12 0.052(2) 0.054(2) 0.0269(16) -0.0064(16) -0.0005(15) 0.033(2) C13 0.0390(19) 0.044(2) 0.0246(15) -0.0028(14) -0.0032(14) 0.0179(17) C14 0.0376(18) 0.0391(19) 0.0278(15) -0.0031(14) -0.0016(13) 0.0201(16) C15 0.044(2) 0.045(2) 0.0274(15) -0.0017(15) 0.0010(14) 0.0206(18) C16 0.040(2) 0.058(3) 0.0283(18) 0.0041(16) 0.0033(15) 0.0225(19) C17 0.051(2) 0.068(3) 0.0316(18) 0.0111(18) 0.0098(17) 0.033(2) C18 0.073(3) 0.091(4) 0.040(2) 0.022(2) 0.025(2) 0.053(3) C19 0.106(5) 0.119(5) 0.052(3) 0.042(3) 0.044(3) 0.079(4) C20 0.089(4) 0.092(4) 0.055(3) 0.031(3) 0.027(3) 0.063(4) C21 0.054(3) 0.062(3) 0.041(2) 0.0086(19) 0.0095(18) 0.033(2) C22 0.114(5) 0.115(5) 0.049(3) 0.022(3) 0.037(3) 0.083(5) N5 0.0394(17) 0.0446(18) 0.0376(16) 0.0069(13) 0.0090(14) 0.0198(15) C23 0.148(7) 0.086(4) 0.043(3) 0.021(3) 0.018(3) 0.064(5) C24 0.097(4) 0.087(4) 0.049(3) 0.030(3) 0.032(3) 0.065(4) C25 0.059(3) 0.054(2) 0.040(2) 0.0121(19) 0.0084(19) 0.026(2) C26 0.045(2) 0.053(2) 0.0379(18) 0.0152(17) 0.0148(17) 0.0217(19) C27 0.040(2) 0.055(2) 0.0393(19) 0.0079(17) 0.0078(16) 0.0246(19) C28 0.045(2) 0.065(3) 0.0362(19) 0.0069(18) 0.0093(16) 0.032(2) C29 0.053(3) 0.071(3) 0.0373(19) 0.0061(19) 0.0014(18) 0.035(2) C30 0.068(3) 0.090(4) 0.041(2) 0.015(2) 0.006(2) 0.045(3) C31 0.082(5) 0.083(5) 0.117(6) -0.021(4) 0.035(4) 0.022(4) C32 0.078(4) 0.058(3) 0.097(5) -0.005(3) 0.011(3) 0.026(3) C33 0.063(3) 0.056(3) 0.057(3) -0.003(2) 0.001(2) 0.023(2) C34 0.046(2) 0.052(2) 0.048(2) 0.0077(18) 0.0085(17) 0.026(2) C35 0.043(2) 0.045(2) 0.0379(19) 0.0064(16) 0.0052(16) 0.0211(18) C36 0.062(3) 0.048(2) 0.048(2) 0.0073(18) 0.007(2) 0.028(2) C37 0.070(3) 0.052(3) 0.049(2) -0.001(2) -0.004(2) 0.022(2) C38 0.131(6) 0.065(4) 0.050(3) -0.010(2) -0.023(3) 0.044(4) Cl1 0.0832(18) 0.0767(17) 0.0512(12) -0.0141(12) -0.0088(12) 0.0428(15) P2 0.0445(6) 0.0445(6) 0.0267(7) 0.000 0.000 0.0222(3) O7 0.0471(15) 0.0452(15) 0.0292(12) -0.0012(11) 0.0005(11) 0.0240(13) O8 0.0521(18) 0.0521(18) 0.031(2) 0.000 0.000 0.0261(9) P1 0.0380(5) 0.0380(5) 0.0256(6) 0.000 0.000 0.0190(3) O5 0.0488(17) 0.0488(17) 0.0227(19) 0.000 0.000 0.0244(9) O6 0.0414(14) 0.0440(15) 0.0302(12) -0.0019(11) 0.0008(10) 0.0216(12) C39 0.087(8) 0.087(8) 0.031(6) 0.000 0.000 0.044(4) 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 '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 H1A C1 H1B 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . O1 C1 H1A 109.5 . . O1 C1 H1B 109.5 . . O1 C1 H1C 109.5 . . C6 N1 H1 116.7 . . C8 N1 H1 116.7 . . C8 N1 C6 126.6(3) . . C2 O1 C1 117.8(3) . . O1 C2 C3 125.1(3) . . O1 C2 C7 114.0(3) . . C3 C2 C7 120.8(4) . . C8 N2 H2 115.4 . . C8 N2 C9 129.1(3) . . C9 N2 H2 115.4 . . C2 C3 H3 120.9 . . C2 C3 C4 118.2(3) . . C4 C3 H3 120.9 . . C13 N3 H3A 115.5 . . C15 N3 H3A 115.5 . . C15 N3 C13 129.1(4) . . C3 C4 H4 119.1 . . C5 C4 C3 121.8(4) . . C5 C4 H4 119.1 . . C15 N4 H4A 116.0 . . C15 N4 C16 128.0(4) . . C16 N4 H4A 116.0 . . C18 O4 C22 117.7(4) . . C4 C5 H5 120.3 . . C4 C5 C6 119.4(4) . . C6 C5 H5 120.3 . . C5 C6 N1 116.8(3) . . C7 C6 N1 123.8(3) . . C7 C6 C5 119.4(3) . . C2 C7 H7 119.8 . . C6 C7 C2 120.4(4) . . C6 C7 H7 119.8 . . N2 C8 N1 111.5(3) . . O2 C8 N1 125.2(3) . . O2 C8 N2 123.3(3) . . C10 C9 N2 126.2(3) . . C14 C9 N2 114.4(3) . . C14 C9 C10 119.3(3) . . C9 C10 H10 120.9 . . C11 C10 C9 118.3(3) . . C11 C10 H10 120.9 . . C10 C11 H11 118.7 . . C10 C11 C12 122.6(4) . . C12 C11 H11 118.7 . . C11 C12 H12 120.9 . . C13 C12 C11 118.2(3) . . C13 C12 H12 120.9 . . C12 C13 N3 126.5(3) . . C12 C13 C14 119.5(3) . . C14 C13 N3 114.0(3) . . C9 C14 C13 122.0(4) . . C9 C14 H14 119.0 . . C13 C14 H14 119.0 . . O3 C15 N3 124.2(4) . . O3 C15 N4 125.4(3) . . N4 C15 N3 110.4(3) . . C17 C16 N4 123.5(4) . . C17 C16 C21 120.5(4) . . C21 C16 N4 116.0(4) . . C16 C17 H17 121.0 . . C16 C17 C18 118.1(5) . . C18 C17 H17 121.0 . . O4 C18 C17 122.9(5) . . C19 C18 O4 115.6(4) . . C19 C18 C17 121.5(5) . . C18 C19 H19 120.2 . . C18 C19 C20 119.6(5) . . C20 C19 H19 120.2 . . C19 C20 H20 119.6 . . C19 C20 C21 120.7(5) . . C21 C20 H20 119.6 . . C16 C21 H21 120.2 . . C20 C21 C16 119.5(4) . . C20 C21 H21 120.2 . . O4 C22 H22A 109.5 . . O4 C22 H22B 109.5 . . O4 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C27 N5 C26 106.0(3) . . C27 N5 C34 111.5(3) . . C34 N5 C26 110.3(3) . . C35 N5 C26 111.5(3) . . C35 N5 C27 111.1(3) . . C35 N5 C34 106.4(3) . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C24 C23 H23A 109.5 . . C24 C23 H23B 109.5 . . C24 C23 H23C 109.5 . . C23 C24 H24A 109.4 . . C23 C24 H24B 109.4 . . H24A C24 H24B 108.0 . . C25 C24 C23 111.0(5) . . C25 C24 H24A 109.4 . . C25 C24 H24B 109.4 . . C24 C25 H25A 109.9 . . C24 C25 H25B 109.9 . . H25A C25 H25B 108.3 . . C26 C25 C24 109.1(4) . . C26 C25 H25A 109.9 . . C26 C25 H25B 109.9 . . N5 C26 H26A 108.3 . . N5 C26 H26B 108.3 . . C25 C26 N5 116.0(4) . . C25 C26 H26A 108.3 . . C25 C26 H26B 108.3 . . H26A C26 H26B 107.4 . . N5 C27 H27A 108.1 . . N5 C27 H27B 108.1 . . N5 C27 C28 116.9(3) . . H27A C27 H27B 107.3 . . C28 C27 H27A 108.1 . . C28 C27 H27B 108.1 . . C27 C28 H28A 109.8 . . C27 C28 H28B 109.8 . . C27 C28 C29 109.3(3) . . H28A C28 H28B 108.3 . . C29 C28 H28A 109.8 . . C29 C28 H28B 109.8 . . C28 C29 H29A 109.0 . . C28 C29 H29B 109.0 . . H29A C29 H29B 107.8 . . C30 C29 C28 113.0(4) . . C30 C29 H29A 109.0 . . C30 C29 H29B 109.0 . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . H31A C31 H31B 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C32 C31 H31A 109.5 . . C32 C31 H31B 109.5 . . C32 C31 H31C 109.5 . . C31 C32 H32A 109.2 . . C31 C32 H32B 109.2 . . C31 C32 C33 111.9(6) . . H32A C32 H32B 107.9 . . C33 C32 H32A 109.2 . . C33 C32 H32B 109.2 . . C32 C33 H33A 109.3 . . C32 C33 H33B 109.3 . . C32 C33 C34 111.7(5) . . H33A C33 H33B 107.9 . . C34 C33 H33A 109.3 . . C34 C33 H33B 109.3 . . N5 C34 C33 115.5(4) . . N5 C34 H34A 108.4 . . N5 C34 H34B 108.4 . . C33 C34 H34A 108.4 . . C33 C34 H34B 108.4 . . H34A C34 H34B 107.5 . . N5 C35 H35A 108.3 . . N5 C35 H35B 108.3 . . N5 C35 C36 115.8(4) . . H35A C35 H35B 107.4 . . C36 C35 H35A 108.3 . . C36 C35 H35B 108.3 . . C35 C36 H36A 109.7 . . C35 C36 H36B 109.7 . . C35 C36 C37 110.0(4) . . H36A C36 H36B 108.2 . . C37 C36 H36A 109.7 . . C37 C36 H36B 109.7 . . C36 C37 H37A 108.9 . . C36 C37 H37B 108.9 . . H37A C37 H37B 107.7 . . C38 C37 C36 113.5(5) . . C38 C37 H37A 108.9 . . C38 C37 H37B 108.9 . . C37 C38 H38A 109.5 . . C37 C38 H38B 109.5 . . C37 C38 H38C 109.5 . . H38A C38 H38B 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . O7 P2 O7 107.80(11) 2_655 . O7 P2 O7 107.80(11) 3_665 . O7 P2 O7 107.80(11) 2_655 3_665 O8 P2 O7 111.09(10) . 2_655 O8 P2 O7 111.09(11) . 3_665 O8 P2 O7 111.09(11) . . P2 O7 H7A 109.5 . . O5 P1 O6 111.11(11) . . O5 P1 O6 111.11(11) . 3_665 O5 P1 O6 111.11(11) . 2_655 O6 P1 O6 107.78(11) 2_655 . O6 P1 O6 107.78(11) 3_665 . O6 P1 O6 107.78(11) 2_655 3_665 P1 O6 H6 109.5 . . Cl1 C39 Cl1 110.9(5) 3_665 . Cl1 C39 Cl1 110.9(5) 2_655 . Cl1 C39 Cl1 110.9(5) 3_665 2_655 Cl1 C39 H39 108.0 3_665 . Cl1 C39 H39 108.0 2_655 . Cl1 C39 H39 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C1 O1 1.429(4) . N1 H1 0.8800 . N1 C6 1.408(4) . N1 C8 1.379(5) . O1 C2 1.370(5) . C2 C3 1.382(6) . C2 C7 1.399(5) . N2 H2 0.8800 . N2 C8 1.366(4) . N2 C9 1.407(5) . O2 C8 1.224(5) . C3 H3 0.9500 . C3 C4 1.390(7) . N3 H3A 0.8800 . N3 C13 1.415(5) . N3 C15 1.373(5) . O3 C15 1.208(5) . C4 H4 0.9500 . C4 C5 1.381(6) . N4 H4A 0.8800 . N4 C15 1.367(6) . N4 C16 1.415(5) . O4 C18 1.370(6) . O4 C22 1.425(7) . C5 H5 0.9500 . C5 C6 1.404(5) . C6 C7 1.372(5) . C7 H7 0.9500 . C9 C10 1.394(6) . C9 C14 1.386(5) . C10 H10 0.9500 . C10 C11 1.390(5) . C11 H11 0.9500 . C11 C12 1.402(6) . C12 H12 0.9500 . C12 C13 1.384(6) . C13 C14 1.390(5) . C14 H14 0.9500 . C16 C17 1.384(6) . C16 C21 1.395(7) . C17 H17 0.9500 . C17 C18 1.402(6) . C18 C19 1.368(8) . C19 H19 0.9500 . C19 C20 1.371(8) . C20 H20 0.9500 . C20 C21 1.380(6) . C21 H21 0.9500 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . N5 C26 1.529(5) . N5 C27 1.516(5) . N5 C34 1.519(6) . N5 C35 1.512(5) . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C23 C24 1.536(8) . C24 H24A 0.9900 . C24 H24B 0.9900 . C24 C25 1.529(7) . C25 H25A 0.9900 . C25 H25B 0.9900 . C25 C26 1.517(6) . C26 H26A 0.9900 . C26 H26B 0.9900 . C27 H27A 0.9900 . C27 H27B 0.9900 . C27 C28 1.522(5) . C28 H28A 0.9900 . C28 H28B 0.9900 . C28 C29 1.522(6) . C29 H29A 0.9900 . C29 H29B 0.9900 . C29 C30 1.518(6) . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C31 C32 1.491(11) . C32 H32A 0.9900 . C32 H32B 0.9900 . C32 C33 1.510(9) . C33 H33A 0.9900 . C33 H33B 0.9900 . C33 C34 1.529(7) . C34 H34A 0.9900 . C34 H34B 0.9900 . C35 H35A 0.9900 . C35 H35B 0.9900 . C35 C36 1.525(6) . C36 H36A 0.9900 . C36 H36B 0.9900 . C36 C37 1.526(7) . C37 H37A 0.9900 . C37 H37B 0.9900 . C37 C38 1.497(8) . C38 H38A 0.9800 . C38 H38B 0.9800 . C38 H38C 0.9800 . Cl1 C39 1.754(6) . P2 O7 1.553(3) . P2 O7 1.553(3) 2_655 P2 O7 1.553(3) 3_665 P2 O8 1.491(5) . O7 H7A 0.8400 . P1 O5 1.487(4) . P1 O6 1.556(3) 2_655 P1 O6 1.556(3) 3_665 P1 O6 1.556(3) . O6 H6 0.8400 . C39 Cl1 1.754(6) 3_665 C39 Cl1 1.754(6) 2_655 C39 H39 1.0000 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O5 0.88 2.30 3.116(3) 153.8 . N2 H2 O6 0.88 2.02 2.892(4) 173.2 3_665 N3 H3A O7 0.88 2.05 2.895(4) 161.9 . N4 H4A O8 0.88 2.17 3.029(4) 164.2 . C7 H7 O2 0.95 2.21 2.849(4) 123.4 . C17 H17 O3 0.95 2.28 2.890(5) 121.1 . O7 H7A O6 0.84 1.74 2.579(3) 174.3 . 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 C1 O1 C2 C3 2.4(6) C1 O1 C2 C7 -176.4(4) N1 C6 C7 C2 -178.3(4) O1 C2 C3 C4 -178.9(4) O1 C2 C7 C6 178.4(4) C2 C3 C4 C5 -0.2(7) N2 C9 C10 C11 -175.8(4) N2 C9 C14 C13 176.8(3) C3 C2 C7 C6 -0.5(6) C3 C4 C5 C6 1.0(7) N3 C13 C14 C9 178.2(3) C4 C5 C6 N1 178.1(4) C4 C5 C6 C7 -1.5(6) N4 C16 C17 C18 179.5(5) N4 C16 C21 C20 -178.3(5) O4 C18 C19 C20 -180.0(6) C5 C6 C7 C2 1.3(6) C6 N1 C8 N2 -175.3(4) C6 N1 C8 O2 4.2(7) C7 C2 C3 C4 0.0(6) C8 N1 C6 C5 -179.2(4) C8 N1 C6 C7 0.4(6) C8 N2 C9 C10 -15.8(7) C8 N2 C9 C14 166.6(4) C9 N2 C8 N1 -173.2(4) C9 N2 C8 O2 7.3(7) C9 C10 C11 C12 -1.3(6) C10 C9 C14 C13 -0.9(6) C10 C11 C12 C13 0.2(6) C11 C12 C13 N3 -177.6(4) C11 C12 C13 C14 0.6(6) C12 C13 C14 C9 -0.2(6) C13 N3 C15 O3 4.8(7) C13 N3 C15 N4 -176.3(4) C14 C9 C10 C11 1.6(6) C15 N3 C13 C12 -5.2(7) C15 N3 C13 C14 176.5(4) C15 N4 C16 C17 -2.4(7) C15 N4 C16 C21 177.7(4) C16 N4 C15 N3 -172.2(4) C16 N4 C15 O3 6.6(7) C16 C17 C18 O4 179.8(5) C16 C17 C18 C19 -0.4(9) C17 C16 C21 C20 1.8(7) C17 C18 C19 C20 0.1(11) C18 C19 C20 C21 1.1(11) C19 C20 C21 C16 -2.1(9) C21 C16 C17 C18 -0.6(7) C22 O4 C18 C17 -5.0(9) C22 O4 C18 C19 175.2(7) N5 C27 C28 C29 162.0(4) N5 C35 C36 C37 -170.5(3) C23 C24 C25 C26 176.7(5) C24 C25 C26 N5 173.7(4) C26 N5 C27 C28 175.3(4) C26 N5 C34 C33 -52.4(5) C26 N5 C35 C36 60.0(4) C27 N5 C26 C25 175.9(4) C27 N5 C34 C33 65.1(5) C27 N5 C35 C36 -58.0(4) C27 C28 C29 C30 176.6(4) C31 C32 C33 C34 74.3(7) C32 C33 C34 N5 -171.8(5) C34 N5 C26 C25 -63.2(5) C34 N5 C27 C28 55.2(5) C34 N5 C35 C36 -179.6(3) C35 N5 C26 C25 54.8(5) C35 N5 C27 C28 -63.4(5) C35 N5 C34 C33 -173.5(4) C35 C36 C37 C38 73.4(6)