#------------------------------------------------------------------------------ #$Date: 2019-11-17 04:59:05 +0200 (Sun, 17 Nov 2019) $ #$Revision: 227998 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121137.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_7121137 loop_ _publ_author_name 'Koner, Abhishek' 'Kelemen, Zsolt' 'Schnakenburg, Gregor' 'Nyul\'aszi, L\'aszl\'o' 'Streubel, Rainer' _publ_section_title ; 1,4-Additions of tricyclic 1,4-diphosphinines - a novel system to study \s-bond activation and \p-\p dispersion interactions. ; _journal_issue 10 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1182 _journal_page_last 1184 _journal_paper_doi 10.1039/c7cc09349g _journal_volume 54 _journal_year 2018 _chemical_formula_moiety 'C34 H46 N4 P2 S4' _chemical_formula_sum 'C34 H46 N4 P2 S4' _chemical_formula_weight 700.93 _chemical_name_systematic ABK-465 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-04-05 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292) ; _audit_update_record ; 2017-12-05 deposited with the CCDC. 2018-01-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.230(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.465(3) _cell_length_b 13.1095(18) _cell_length_c 15.633(2) _cell_measurement_reflns_used 7641 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.44 _cell_measurement_theta_min 2.49 _cell_volume 3683.8(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 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method 'fine slicing \w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_unetI/netI 0.0589 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 50325 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.000 _diffrn_reflns_theta_min 1.133 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_correction_T_min 0.4664 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1032 before and 0.0734 after correction. The Ratio of minimum to maximum transmission is 0.6253. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.264 _exptl_crystal_description plate _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.537 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 8895 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0466 _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^)+(0.0246P)^2^+2.5985P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.0975 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7330 _reflns_number_total 8895 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09349g2.cif _cod_data_source_block 3a _cod_depositor_comments 'Adding full bibliography for 7121136--7121139.cif.' _cod_database_code 7121137 _shelx_shelxl_version_number 2014/7 _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 0.982 _shelx_estimated_absorpt_t_min 0.936 _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.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C3'(H3'A,H3'B), C4'(H4'A,H4'B), C5'(H5'A,H5'B), C8'(H8'A,H8'B), C9'(H9'A,H9'B), C10'(H10D,H10E) 2.b Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17') 2.c Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C6'(H6'A,H6'B,H6'C), C11'(H11A,H11B,H11C) ; _shelx_res_file ; 5109f.res created by SHELXL-2014/7 TITL 5109f in P21/c #14 REM reset to P21/c #14 CELL 0.71073 18.4651 13.1095 15.6329 90 103.2303 90 ZERR 4 0.0028 0.0018 0.0022 0 0.0049 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N P S UNIT 136 184 16 8 16 L.S. 4 PLAN 5 SIZE 0.05 0.14 0.18 TEMP -173.15 BOND fmap 2 ACTA OMIT -2 56 OMIT 0 1 1 OMIT 0 0 2 REM REM REM WGHT 0.024600 2.598500 FVAR 0.12068 S1 5 0.376674 0.747319 0.683488 11.00000 0.02905 0.01815 = 0.02087 -0.00496 0.01168 0.00502 S2 5 0.562175 0.698645 0.417020 11.00000 0.02392 0.01221 = 0.01311 0.00220 0.00641 -0.00316 P 4 0.474081 0.587614 0.402273 11.00000 0.01792 0.00949 = 0.00855 0.00090 0.00328 0.00134 N1 3 0.416496 0.675186 0.535865 11.00000 0.01639 0.00958 = 0.01202 -0.00023 0.00366 0.00075 N2 3 0.446895 0.573899 0.648448 11.00000 0.01566 0.01277 = 0.00962 -0.00104 0.00434 0.00015 C1 1 0.454308 0.593446 0.509921 11.00000 0.01556 0.00764 = 0.01104 -0.00066 0.00342 -0.00161 C2 1 0.412992 0.664718 0.622061 11.00000 0.01426 0.01373 = 0.01426 -0.00247 0.00374 -0.00196 C3 1 0.383070 0.760497 0.479715 11.00000 0.01854 0.00943 = 0.01862 0.00174 0.00463 0.00153 AFIX 23 H3A 2 0.417344 0.781716 0.442712 11.00000 -1.20000 H3B 2 0.376852 0.819093 0.517339 11.00000 -1.20000 AFIX 0 C4 1 0.307859 0.733717 0.420557 11.00000 0.01913 0.01949 = 0.02088 0.00195 0.00169 -0.00065 AFIX 23 H4A 2 0.314529 0.678800 0.379573 11.00000 -1.20000 H4B 2 0.274592 0.707662 0.457060 11.00000 -1.20000 AFIX 0 C5 1 0.271699 0.825167 0.368131 11.00000 0.02447 0.02645 = 0.02210 0.00518 0.00512 0.00854 AFIX 23 H5A 2 0.307338 0.855553 0.336753 11.00000 -1.20000 H5B 2 0.260503 0.877170 0.409183 11.00000 -1.20000 AFIX 0 C6 1 0.200383 0.798342 0.301748 11.00000 0.02826 0.05748 = 0.03329 0.00947 -0.00468 0.01249 AFIX 137 H6A 2 0.165180 0.766881 0.332174 11.00000 -1.50000 H6B 2 0.211579 0.750368 0.258453 11.00000 -1.50000 H6C 2 0.178397 0.860475 0.271807 11.00000 -1.50000 AFIX 0 C7 1 0.454416 0.530861 0.736929 11.00000 0.01961 0.01618 = 0.00736 -0.00005 0.00510 -0.00221 AFIX 23 H7A 2 0.445775 0.456343 0.731992 11.00000 -1.20000 H7B 2 0.415750 0.560845 0.763915 11.00000 -1.20000 AFIX 0 C8 1 0.530633 0.550723 0.796641 11.00000 0.01867 0.01213 = 0.01077 -0.00071 0.00523 -0.00186 AFIX 23 H8A 2 0.569091 0.515424 0.772703 11.00000 -1.20000 H8B 2 0.541286 0.624785 0.797769 11.00000 -1.20000 AFIX 0 C9 1 0.534629 0.513614 0.889821 11.00000 0.01955 0.01893 = 0.01126 0.00085 0.00295 -0.00106 AFIX 23 H9A 2 0.521064 0.440465 0.888242 11.00000 -1.20000 H9B 2 0.498076 0.551757 0.914881 11.00000 -1.20000 AFIX 0 C10 1 0.612089 0.527712 0.948833 11.00000 0.02142 0.01727 = 0.01774 0.00052 0.00046 0.00151 AFIX 137 H10A 2 0.611694 0.506565 1.008852 11.00000 -1.50000 H10B 2 0.626469 0.599672 0.948857 11.00000 -1.50000 H10C 2 0.647866 0.485956 0.926701 11.00000 -1.50000 AFIX 0 C11 1 0.525948 0.470268 0.419172 11.00000 0.01168 0.01061 = 0.01098 -0.00209 0.00336 -0.00218 C12 1 0.610408 0.682940 0.528727 11.00000 0.01628 0.01250 = 0.01428 0.00164 0.00517 -0.00443 C13 1 0.592686 0.747326 0.592192 11.00000 0.01839 0.01118 = 0.02001 -0.00115 0.00719 -0.00066 AFIX 43 H13 2 0.556693 0.799685 0.575230 11.00000 -1.20000 AFIX 0 C14 1 0.627734 0.734667 0.680000 11.00000 0.02497 0.01884 = 0.01662 -0.00500 0.00921 -0.00260 AFIX 43 H14 2 0.615556 0.778098 0.723296 11.00000 -1.20000 AFIX 0 C15 1 0.680616 0.658482 0.704551 11.00000 0.02237 0.02380 = 0.01532 -0.00021 0.00357 -0.00431 AFIX 43 H15 2 0.704251 0.649473 0.764767 11.00000 -1.20000 AFIX 0 C16 1 0.699101 0.595421 0.641486 11.00000 0.01627 0.01931 = 0.02290 0.00248 0.00440 0.00257 AFIX 43 H16 2 0.735748 0.543914 0.658577 11.00000 -1.20000 AFIX 0 C17 1 0.664017 0.607474 0.553102 11.00000 0.01780 0.01574 = 0.01895 -0.00197 0.00888 -0.00200 AFIX 43 H17 2 0.676668 0.564412 0.509860 11.00000 -1.20000 AFIX 0 S1' 5 0.000141 0.156400 0.663195 11.00000 0.03656 0.01252 = 0.01574 0.00625 0.00534 -0.00101 S2' 5 -0.095473 0.605917 0.624063 11.00000 0.01605 0.01543 = 0.00959 -0.00239 0.00537 0.00038 P' 4 0.015137 0.570341 0.608062 11.00000 0.01410 0.01049 = 0.00596 -0.00057 0.00309 -0.00098 N1' 3 0.007992 0.363501 0.646773 11.00000 0.01660 0.01205 = 0.00701 0.00181 0.00319 -0.00035 N2' 3 0.012716 0.717158 0.478057 11.00000 0.01676 0.00981 = 0.00958 0.00029 0.00523 -0.00092 C1' 1 0.005460 0.436741 0.581300 11.00000 0.01073 0.01117 = 0.00872 0.00205 0.00322 0.00032 C2' 1 -0.001886 0.268035 0.610824 11.00000 0.01611 0.01514 = 0.01094 0.00262 0.00416 0.00020 C3' 1 0.028823 0.382568 0.741766 11.00000 0.01900 0.01669 = 0.00586 0.00189 0.00442 0.00040 AFIX 23 H3'A 2 0.005232 0.330735 0.772608 11.00000 -1.20000 H3'B 2 0.010343 0.450516 0.754441 11.00000 -1.20000 AFIX 0 C4' 1 0.113026 0.378411 0.775721 11.00000 0.01744 0.01848 = 0.01023 0.00109 0.00540 -0.00002 AFIX 23 H4'A 2 0.136263 0.429690 0.743958 11.00000 -1.20000 H4'B 2 0.131089 0.310292 0.762827 11.00000 -1.20000 AFIX 0 C5' 1 0.137641 0.398613 0.874376 11.00000 0.01799 0.01983 = 0.01274 -0.00164 0.00115 0.00170 AFIX 23 H5'A 2 0.125131 0.469712 0.886765 11.00000 -1.20000 H5'B 2 0.110360 0.352466 0.906102 11.00000 -1.20000 AFIX 0 C6' 1 0.221091 0.381858 0.907574 11.00000 0.02144 0.03110 = 0.02412 -0.00423 -0.00036 -0.00223 AFIX 137 H6'A 2 0.235624 0.398078 0.970372 11.00000 -1.50000 H6'B 2 0.248140 0.426278 0.875199 11.00000 -1.50000 H6'C 2 0.233133 0.310451 0.898483 11.00000 -1.50000 AFIX 0 C7' 1 0.008141 0.614241 0.496886 11.00000 0.01066 0.00994 = 0.00980 0.00132 0.00294 -0.00040 C8' 1 0.030212 0.800600 0.542004 11.00000 0.02094 0.00968 = 0.01246 -0.00231 0.00528 0.00059 AFIX 23 H8'A 2 0.017339 0.779273 0.597443 11.00000 -1.20000 H8'B 2 -0.000809 0.860547 0.519092 11.00000 -1.20000 AFIX 0 C9' 1 0.111437 0.831170 0.561216 11.00000 0.02077 0.01914 = 0.01805 -0.00338 0.00699 -0.00310 AFIX 23 H9'A 2 0.125318 0.849721 0.505692 11.00000 -1.20000 H9'B 2 0.142699 0.772746 0.587501 11.00000 -1.20000 AFIX 0 C10' 1 0.125729 0.921428 0.624181 11.00000 0.03247 0.02330 = 0.02911 -0.01034 0.00652 -0.01084 AFIX 23 H10D 2 0.089952 0.976501 0.600897 11.00000 -1.20000 H10E 2 0.116928 0.900035 0.681686 11.00000 -1.20000 AFIX 0 C11' 1 0.204129 0.962679 0.637511 11.00000 0.04539 0.05251 = 0.04449 -0.01117 0.00295 -0.02988 AFIX 137 H11A 2 0.209895 1.022031 0.676602 11.00000 -1.50000 H11B 2 0.213475 0.982973 0.580668 11.00000 -1.50000 H11C 2 0.239749 0.909726 0.663889 11.00000 -1.50000 AFIX 0 C12' 1 -0.153384 0.570545 0.520794 11.00000 0.01214 0.02058 = 0.01064 -0.00171 0.00499 0.00007 C13' 1 -0.178576 0.645928 0.458062 11.00000 0.01695 0.01904 = 0.01851 0.00189 0.00705 0.00079 AFIX 43 H13' 2 -0.162860 0.714608 0.469334 11.00000 -1.20000 AFIX 0 C14' 1 -0.226948 0.619973 0.378713 11.00000 0.01702 0.03791 = 0.01518 0.00670 0.00443 0.00415 AFIX 43 H14' 2 -0.244816 0.671303 0.336227 11.00000 -1.20000 AFIX 0 C15' 1 -0.249009 0.519703 0.361654 11.00000 0.01466 0.04325 = 0.01407 -0.00638 0.00293 -0.00124 AFIX 43 H15' 2 -0.281563 0.502361 0.307243 11.00000 -1.20000 AFIX 0 C16' 1 -0.223787 0.444405 0.423669 11.00000 0.01800 0.02690 = 0.02333 -0.01148 0.00935 -0.00512 AFIX 43 H16' 2 -0.238877 0.375615 0.411584 11.00000 -1.20000 AFIX 0 C17' 1 -0.176365 0.469686 0.503603 11.00000 0.01476 0.01786 = 0.01910 -0.00104 0.00663 0.00017 AFIX 43 H17' 2 -0.159646 0.418324 0.546439 11.00000 -1.20000 AFIX 0 HKLF 4 REM 5109f in P21/c #14 REM R1 = 0.0466 for 7330 Fo > 4sig(Fo) and 0.0630 for all 8895 data REM 401 parameters refined using 0 restraints END WGHT 0.0237 2.6986 REM Highest difference peak 0.537, deepest hole -0.401, 1-sigma level 0.072 Q1 1 0.0226 0.5805 0.5506 11.00000 0.05 0.54 Q2 1 0.4626 0.5919 0.4557 11.00000 0.05 0.48 Q3 1 0.5016 0.5267 0.4107 11.00000 0.05 0.45 Q4 1 0.0308 0.5022 0.5955 11.00000 0.05 0.40 Q5 1 0.3470 0.7381 0.4552 11.00000 0.05 0.37 ; _shelx_res_checksum 5090 _shelx_hkl_file ; 0 0 -1 -0.34 0.04 0 0 1 -0.37 0.01 0 0 1 -0.38 0.01 0 0 1 -0.39 0.03 0 0 1 -0.37 0.01 0 0 -1 -0.35 0.03 0 0 -1 -0.38 0.04 0 0 2 245.94 12.21 0 0 3 0.02 0.21 0 0 -3 0.21 0.27 0 0 -3 -0.03 0.14 0 0 3 0.08 0.11 0 0 -3 0.21 0.28 0 0 3 0.12 0.12 0 0 4 675.63 34.55 0 0 4 725.74 34.54 0 0 -4 704.89 34.50 0 0 4 747.96 34.79 0 0 -4 670.35 34.57 0 0 -4 730.88 34.83 0 0 5 0.09 0.18 0 0 5 0.02 0.26 0 0 -5 -0.35 0.31 0 0 -5 -0.17 0.32 0 0 -5 0.34 0.31 0 0 5 -0.16 0.25 0 0 5 -0.17 0.26 0 0 5 0.16 0.39 0 0 6 29.43 2.31 0 0 6 30.25 2.26 0 0 6 30.78 1.70 0 0 -6 28.65 2.04 0 0 6 31.65 2.16 0 0 -6 26.49 2.09 0 0 6 26.87 2.11 0 0 -6 30.41 2.41 0 0 -7 -0.12 0.35 0 0 7 0.49 0.56 0 0 7 0.07 0.49 0 0 7 0.72 0.54 0 0 -7 0.05 0.25 0 0 7 0.07 0.35 0 0 7 0.22 0.22 0 0 -7 -0.04 0.43 0 0 -8 86.69 5.80 0 0 8 89.19 5.62 0 0 8 96.16 4.76 0 0 8 96.30 5.53 0 0 8 95.14 5.45 0 0 -8 85.28 5.46 0 0 9 0.06 0.40 0 0 9 0.10 0.16 0 0 -9 0.14 0.34 0 0 9 -0.52 0.43 0 0 -9 0.17 0.36 0 0 9 0.06 0.49 0 0 10 60.32 4.19 0 0 10 61.48 3.25 0 0 10 55.30 4.29 0 0 10 64.27 4.19 0 0 11 0.70 0.83 0 0 11 0.29 0.65 0 0 11 -0.40 0.45 0 0 11 -0.09 0.11 0 0 12 2.28 1.11 0 0 12 1.02 0.78 0 0 12 2.60 0.30 0 0 12 2.15 1.01 0 0 13 -0.31 0.54 0 0 13 0.34 0.72 0 0 13 -0.60 0.62 0 0 14 27.84 3.70 0 0 14 25.29 3.19 0 0 14 31.66 3.63 0 0 15 0.75 0.75 0 0 15 1.17 0.89 0 0 15 -0.93 0.43 0 0 16 1.12 0.85 0 0 16 1.19 0.86 0 0 17 -0.53 0.59 0 0 17 1.04 0.99 0 0 17 0.05 0.73 0 0 18 2.00 0.86 0 0 18 1.48 1.04 0 0 18 4.15 1.35 0 0 19 2.80 1.13 0 0 19 0.26 0.79 0 0 19 1.40 0.92 0 0 20 2.55 1.42 0 0 20 1.60 1.02 0 0 21 -1.41 0.36 0 0 21 -1.25 0.84 0 1 0 -0.01 0.01 0 1 0 -0.01 0.01 0 1 0 -0.01 0.05 0 1 0 0.00 0.02 0 -1 0 0.05 0.05 0 -1 0 0.03 0.04 0 -1 0 -0.01 0.00 0 1 -1 0.03 0.04 0 1 -1 0.00 0.03 0 1 1 0.01 0.01 0 1 1 0.00 0.01 0 -1 1 0.06 0.06 0 -1 1 -0.01 0.02 0 -1 1 0.01 0.04 0 1 -2 22.61 1.34 0 1 -2 24.53 1.65 0 -1 -2 22.63 1.40 0 -1 -2 21.02 1.27 0 -1 2 22.21 1.39 0 -1 -2 21.26 1.27 0 1 4 12.67 1.09 0 1 -4 15.20 1.18 0 1 -4 14.35 1.33 0 1 -4 13.24 1.26 0 1 4 16.41 1.34 0 1 4 14.73 1.15 0 1 -4 13.79 1.46 0 -1 4 15.53 1.37 0 -1 4 14.28 1.22 0 -1 4 14.97 1.47 0 -1 -4 16.07 1.16 0 -1 4 16.38 1.31 0 -1 -4 14.15 1.12 0 1 -5 76.58 4.48 0 1 5 84.32 4.72 0 1 -5 79.24 4.75 0 1 5 82.71 4.46 0 1 -5 86.92 4.78 0 1 -5 85.07 5.02 0 1 5 80.14 4.46 0 1 5 85.20 4.37 0 -1 5 83.48 4.56 0 -1 -5 73.20 4.40 0 -1 -5 80.13 4.68 0 -1 5 86.14 4.76 0 -1 5 82.15 4.68 0 -1 5 81.00 4.99 0 -1 -5 70.63 4.40 0 1 6 9.90 1.17 0 1 6 9.58 1.32 0 1 6 7.33 1.06 0 1 6 9.42 0.98 0 1 -6 8.59 1.30 0 1 -6 7.46 1.43 0 1 -6 8.67 1.36 0 1 -6 7.95 1.13 0 -1 6 10.06 1.35 0 -1 6 8.35 1.53 0 -1 -6 7.77 1.06 0 -1 6 7.62 1.21 0 -1 -6 9.09 1.16 0 -1 6 9.87 1.26 0 -1 -6 9.89 1.37 0 1 7 24.61 1.64 0 1 7 24.03 2.25 0 1 7 20.05 1.74 0 1 -7 22.08 1.96 0 1 -7 19.68 2.15 0 1 7 21.78 2.01 0 1 7 19.54 1.76 0 -1 7 22.25 2.02 0 -1 -7 22.51 2.03 0 -1 7 23.03 2.33 0 -1 -7 18.11 1.71 0 -1 7 24.85 1.91 0 -1 7 23.37 2.02 0 -1 -7 19.54 1.70 0 1 -8 1.34 0.78 0 1 8 2.47 0.72 0 1 8 1.32 0.51 0 1 8 1.95 0.72 0 1 8 2.38 0.81 0 -1 8 1.02 0.74 0 -1 8 2.61 0.94 0 -1 -8 2.48 0.76 0 -1 -8 1.93 0.77 0 -1 8 1.57 0.74 0 -1 8 1.06 0.61 0 1 9 92.90 4.81 0 1 9 82.65 5.52 0 1 9 82.61 5.19 0 1 9 86.61 5.24 0 -1 9 86.44 5.50 0 -1 9 86.04 5.51 0 -1 -9 89.48 5.32 0 -1 -9 86.87 5.64 0 -1 9 82.38 5.30 0 1 10 28.26 1.94 0 1 10 30.16 2.76 0 1 10 24.01 2.27 0 1 10 28.28 2.42 0 -1 10 29.04 3.19 0 -1 10 25.99 2.54 0 -1 10 27.63 2.45 0 1 11 8.61 1.77 0 1 11 7.69 1.52 0 1 11 9.91 1.10 0 1 11 7.75 1.54 0 -1 11 10.85 1.91 0 -1 11 9.65 1.80 0 -1 11 9.76 1.72 0 1 12 8.43 1.70 0 1 12 8.96 1.73 0 1 12 7.37 1.75 0 1 12 9.07 1.02 0 -1 12 7.27 1.58 0 -1 12 10.77 2.00 0 -1 12 7.52 1.70 0 1 13 0.23 0.22 0 1 13 0.76 0.77 0 1 13 -0.47 0.73 0 1 13 -0.90 0.64 0 -1 13 0.57 0.83 0 -1 13 0.35 0.70 0 -1 13 0.38 0.88 0 1 14 87.85 5.81 0 1 14 85.58 5.84 0 1 14 77.93 6.08 0 -1 14 83.42 6.16 0 -1 14 83.43 5.92 0 -1 14 79.07 5.87 0 1 15 0.88 0.96 0 1 15 0.89 0.77 0 1 15 0.64 0.80 0 -1 15 0.96 1.09 0 -1 15 1.24 0.99 0 -1 15 -0.16 0.86 0 1 16 15.24 2.53 0 1 16 13.83 2.77 0 1 16 11.69 2.34 0 -1 16 18.31 2.97 0 -1 16 15.35 2.75 0 -1 16 10.89 2.37 0 1 17 1.53 1.24 0 1 17 1.25 0.96 0 1 17 2.96 1.21 0 -1 17 1.36 0.80 0 -1 17 0.82 0.85 0 -1 17 0.62 1.17 0 1 18 14.11 2.63 0 1 18 13.37 2.74 0 1 18 17.47 3.36 0 -1 18 14.83 2.94 0 -1 18 15.39 2.94 0 -1 18 14.04 2.79 0 1 19 4.03 1.56 0 1 19 4.91 1.59 0 -1 19 2.90 1.56 0 -1 19 3.17 1.20 0 -1 19 3.73 1.55 0 1 20 0.04 0.67 0 1 20 1.85 1.01 0 -1 20 0.12 0.98 0 -1 20 2.28 1.12 0 -1 20 2.04 0.86 0 1 21 3.95 1.36 0 1 21 9.57 2.49 0 -1 21 7.00 2.28 0 -1 21 5.21 1.61 0 2 0 5.90 0.93 0 -2 0 6.74 0.94 0 2 -1 25.38 1.53 0 2 -1 25.98 1.98 0 2 -1 23.42 1.67 0 -2 -1 24.70 1.89 0 -2 -1 31.94 1.62 0 -2 1 32.57 1.80 0 -2 1 31.34 1.58 0 2 -2 -0.21 0.38 0 2 -2 -0.24 0.17 0 2 2 -0.04 0.09 0 2 -2 0.53 0.25 0 2 2 -0.05 0.06 0 -2 2 -0.11 0.19 0 -2 -2 -0.19 0.18 0 -2 2 -0.20 0.08 0 -2 2 0.26 0.23 0 2 3 14.54 1.20 0 2 -3 17.64 1.18 0 2 -3 13.84 1.18 0 2 -3 15.23 1.56 0 -2 -3 14.47 1.17 0 -2 -3 12.66 0.99 0 -2 3 16.10 1.21 0 -2 3 14.56 1.56 0 -2 -3 17.61 1.08 0 -2 3 16.23 1.19 0 2 4 51.97 3.26 0 2 4 54.69 3.03 0 2 -4 52.29 3.68 0 2 -4 55.98 3.32 0 2 4 58.02 3.05 0 2 -4 53.59 3.13 0 -2 4 55.21 3.25 0 -2 -4 52.28 3.01 0 -2 4 52.78 3.68 0 -2 4 54.32 3.19 0 -2 4 55.27 3.46 0 -2 -4 51.12 3.00 0 2 -5 131.39 7.18 0 2 -5 129.14 7.61 0 2 5 127.88 7.11 0 2 -5 124.68 6.91 0 2 5 126.49 6.81 0 2 -5 131.13 6.48 0 2 5 133.39 6.82 0 -2 -5 119.10 6.77 0 -2 5 131.38 7.08 0 -2 5 130.46 7.63 0 -2 -5 150.66 6.89 0 -2 5 131.95 6.99 0 -2 5 127.50 7.26 0 2 6 60.16 3.64 0 2 -6 61.41 3.74 0 2 6 64.12 3.66 0 2 6 60.39 3.93 0 2 -6 59.99 3.99 0 2 -6 63.64 4.45 0 -2 6 65.17 4.49 0 -2 -6 56.04 3.59 0 -2 6 64.37 3.85 0 -2 6 69.23 4.21 0 -2 -6 66.28 3.68 0 -2 6 61.10 3.88 0 2 7 101.54 5.40 0 2 7 97.12 5.71 0 2 7 99.40 5.36 0 2 -7 91.98 5.74 0 2 -7 93.57 6.18 0 2 7 83.97 5.23 0 -2 7 91.17 5.57 0 -2 -7 89.27 5.27 0 -2 -7 96.95 5.63 0 -2 7 98.77 6.27 0 -2 -7 95.91 5.33 0 -2 7 98.09 5.52 0 -2 7 92.66 5.79 0 2 8 225.38 10.83 0 2 8 201.13 10.83 0 2 -8 190.47 11.29 0 2 8 201.56 10.79 0 2 8 206.70 11.27 0 -2 8 209.98 11.05 0 -2 8 239.19 12.15 0 -2 -8 212.71 11.23 0 -2 8 196.72 11.29 0 -2 -8 183.87 10.76 0 2 9 38.06 2.55 0 2 -9 34.54 3.07 0 2 9 36.01 2.67 0 2 9 32.11 2.89 0 2 9 28.70 2.46 0 -2 9 35.17 2.89 0 -2 9 35.52 2.76 0 -2 -9 33.09 2.57 0 -2 9 40.06 3.14 0 -2 -9 33.14 2.80 0 -2 9 37.42 3.49 0 2 10 0.36 0.66 0 2 10 0.19 0.50 0 2 10 -0.50 0.42 0 2 10 -0.10 0.49 0 -2 -10 0.64 0.49 0 -2 10 -0.02 0.70 0 -2 10 0.15 0.77 0 -2 -10 0.07 0.37 0 -2 10 -0.26 0.27 0 2 11 12.24 1.84 0 2 11 15.19 2.08 0 2 11 15.66 1.73 0 2 11 16.59 2.57 0 -2 11 12.31 1.95 0 -2 11 16.07 2.31 0 -2 11 15.83 2.42 0 2 12 6.82 1.77 0 2 12 9.78 1.75 0 2 12 8.97 1.64 0 2 12 8.81 1.34 0 -2 12 10.14 2.03 0 -2 12 7.38 1.71 0 -2 12 10.59 1.90 0 2 13 8.45 1.68 0 2 13 7.70 1.89 0 2 13 11.80 1.95 0 -2 13 10.56 2.03 0 -2 13 8.19 1.94 0 -2 13 7.73 1.84 0 2 14 8.60 2.01 0 2 14 12.52 2.13 0 2 14 7.16 1.61 0 -2 14 10.88 2.12 0 -2 14 8.57 2.07 0 -2 14 9.33 2.12 0 2 15 12.91 2.63 0 2 15 13.23 2.31 0 2 15 12.67 2.20 0 -2 15 18.95 3.07 0 -2 15 10.57 2.23 0 -2 15 13.03 2.53 0 2 16 1.36 0.88 0 2 16 -1.21 0.71 0 2 16 0.53 0.68 0 -2 16 0.87 0.92 0 -2 16 -0.58 0.93 0 -2 16 -0.33 0.65 0 2 17 -0.08 0.58 0 2 17 1.60 1.13 0 2 17 0.24 0.56 0 -2 17 0.52 0.95 0 -2 17 -0.08 0.32 0 -2 17 0.61 0.81 0 2 18 14.58 2.96 0 2 18 12.66 2.48 0 -2 18 9.91 2.28 0 -2 18 10.31 2.54 0 -2 18 13.25 2.74 0 2 19 18.14 3.43 0 2 19 22.36 3.50 0 -2 19 21.75 3.75 0 -2 19 23.07 3.79 0 -2 19 23.64 3.80 0 2 20 21.61 3.52 0 2 20 14.11 3.08 0 -2 20 20.91 3.73 0 -2 20 17.55 3.22 0 -2 20 14.52 2.95 0 3 0 -0.44 0.41 0 3 0 -0.34 0.08 0 3 0 -0.32 0.16 0 3 0 -0.19 0.14 0 -3 0 -0.18 0.16 0 -3 0 -0.20 0.14 0 -3 0 -0.51 0.35 0 3 -1 85.05 4.09 0 3 -1 81.72 4.44 0 3 -1 67.33 4.69 0 -3 -1 83.11 4.14 0 -3 -1 67.04 4.61 0 -3 1 81.48 4.45 0 -3 1 83.25 4.06 0 -3 1 74.97 4.76 0 -3 1 82.78 4.11 0 3 -2 195.52 9.36 0 3 2 174.84 9.41 0 3 -2 174.76 10.09 0 3 -2 190.49 9.63 0 -3 2 191.17 9.65 0 -3 2 186.48 10.15 0 -3 2 189.40 9.38 0 -3 -2 189.98 9.43 0 3 -3 27.06 1.97 0 3 3 28.15 1.66 0 3 -3 27.35 1.82 0 3 3 28.24 1.93 0 3 -3 27.68 2.42 0 -3 -3 28.07 1.91 0 -3 3 34.89 2.62 0 -3 3 29.82 2.02 0 -3 3 29.18 1.88 0 3 -4 119.26 7.47 0 3 4 125.25 6.53 0 3 -4 119.17 6.69 0 3 -4 128.48 6.94 0 3 4 122.18 6.85 0 -3 4 130.79 6.92 0 -3 4 139.02 7.70 0 -3 -4 132.86 6.60 0 -3 -4 131.46 6.90 0 -3 4 128.44 6.77 0 3 -5 24.27 2.48 0 3 -5 25.49 1.90 0 3 -5 26.43 2.09 0 3 5 25.99 2.06 0 3 5 26.46 1.76 0 -3 5 26.65 2.33 0 -3 5 26.48 2.01 0 -3 5 27.34 2.63 0 -3 -5 26.82 1.77 0 -3 5 27.31 1.96 0 -3 -5 23.84 1.71 0 3 -6 119.33 6.11 0 3 -6 121.17 6.91 0 3 6 121.34 6.43 0 3 6 120.03 6.40 0 3 6 124.54 6.86 0 3 -6 114.42 6.55 0 3 -6 115.13 7.43 0 -3 6 117.41 6.64 0 -3 6 123.52 7.12 0 -3 -6 137.39 6.48 0 -3 6 118.80 6.74 0 -3 6 128.24 7.62 0 -3 -6 104.17 6.33 0 3 -7 0.45 0.17 0 3 7 1.33 0.72 0 3 -7 0.46 0.53 0 3 7 0.70 0.47 0 3 7 0.34 0.45 0 -3 7 0.41 0.77 0 -3 7 0.60 0.35 0 -3 7 0.88 0.95 0 -3 -7 0.77 0.38 0 -3 7 0.37 0.42 0 -3 -7 0.46 0.40 0 3 -8 -0.17 0.59 0 3 8 -0.49 0.35 0 3 8 0.30 0.41 0 3 8 -0.51 0.35 0 3 8 0.55 0.53 0 3 -8 0.17 0.12 0 -3 8 -0.05 0.85 0 -3 -8 -0.40 0.18 0 -3 -8 -0.27 0.18 0 -3 8 0.18 0.73 0 -3 8 0.14 0.43 0 3 9 18.29 1.99 0 3 9 19.36 2.08 0 3 9 16.55 1.63 0 3 -9 15.27 2.26 0 3 9 16.78 2.26 0 -3 -9 15.09 1.79 0 -3 9 20.01 3.04 0 -3 -9 15.69 1.72 0 -3 9 16.71 2.10 0 -3 9 15.91 2.41 0 3 10 130.77 8.28 0 3 10 137.90 7.83 0 3 10 149.40 7.94 0 3 -10 129.18 8.41 0 3 10 126.74 7.68 0 -3 10 141.64 8.15 0 -3 10 139.77 8.55 0 -3 -10 147.88 8.26 0 -3 10 138.92 8.25 0 -3 10 151.86 9.37 0 -3 -10 135.62 7.78 0 3 11 3.41 1.01 0 3 11 2.73 0.99 0 3 -11 1.48 1.10 0 3 11 3.85 1.06 0 3 11 2.02 1.10 0 -3 11 2.92 1.02 0 -3 11 3.99 1.64 0 -3 11 2.42 1.21 0 -3 11 2.36 1.12 0 3 12 3.28 1.12 0 3 12 3.63 1.17 0 3 12 5.56 1.29 0 3 12 4.83 1.45 0 -3 12 3.00 1.24 0 -3 12 6.79 1.59 0 -3 12 3.15 1.23 0 3 13 29.33 3.72 0 3 13 29.64 2.75 0 3 13 34.79 3.04 0 -3 13 31.38 4.02 0 -3 13 37.46 4.04 0 -3 13 38.57 3.34 0 3 14 2.26 1.13 0 3 14 3.20 1.16 0 3 14 0.23 0.73 0 -3 14 1.89 0.89 0 -3 14 1.16 1.07 0 -3 14 2.62 1.32 0 3 15 7.03 1.85 0 3 15 5.68 1.60 0 3 15 6.04 1.54 0 -3 15 7.63 2.03 0 -3 15 7.24 1.88 0 -3 15 11.47 2.29 0 3 16 9.21 1.84 0 3 16 11.48 2.26 0 3 16 7.04 2.08 0 -3 16 11.52 2.36 0 -3 16 8.62 2.32 0 -3 16 10.12 2.21 0 3 17 4.32 1.58 0 3 17 1.70 1.19 0 3 17 6.21 1.47 0 -3 17 4.47 1.63 0 -3 17 4.16 1.50 0 -3 17 4.70 1.81 0 3 18 16.13 3.42 0 3 18 22.48 3.26 0 -3 18 20.97 3.49 0 -3 18 19.56 3.44 0 -3 18 20.64 3.47 0 3 19 3.13 1.23 0 3 19 2.33 1.41 0 -3 19 2.83 1.08 0 -3 19 2.19 1.56 0 -3 19 5.17 1.74 0 3 20 19.60 3.39 0 3 20 12.42 2.92 0 -3 20 18.44 3.53 0 -3 20 21.51 3.65 0 -3 20 21.55 3.83 0 4 0 79.82 4.11 0 4 0 81.70 4.69 0 4 0 81.44 4.00 0 4 0 63.60 4.82 0 -4 0 77.58 4.04 0 -4 0 80.37 5.02 0 -4 0 80.10 4.07 0 4 -1 1.14 0.69 0 4 -1 2.12 0.38 0 4 1 1.31 0.36 0 4 1 1.03 0.25 0 4 1 0.50 0.64 0 4 -1 1.45 0.51 0 -4 1 1.29 0.35 0 -4 1 1.72 0.34 0 -4 1 1.49 0.83 0 -4 1 0.86 0.42 0 -4 -1 0.75 0.67 0 -4 -1 1.46 0.36 0 4 2 0.31 0.29 0 4 -2 1.12 0.75 0 4 -2 0.14 0.29 0 4 -2 -0.03 0.22 0 -4 2 0.70 0.35 0 -4 2 0.45 0.33 0 -4 -2 0.15 0.25 0 -4 2 0.32 0.57 0 -4 -2 0.37 0.55 0 4 3 129.79 6.85 0 4 3 126.38 6.46 0 4 -3 114.34 7.61 0 4 -3 131.84 7.07 0 4 -3 128.87 6.71 0 -4 3 134.52 7.83 0 -4 -3 130.61 6.84 0 -4 3 126.89 6.75 0 -4 3 135.79 7.12 0 4 4 59.53 3.68 0 4 -4 58.82 3.53 0 4 4 61.24 3.32 0 4 -4 56.38 4.41 0 4 -4 60.84 3.82 0 -4 4 61.66 3.61 0 -4 4 61.51 4.54 0 -4 -4 62.60 3.47 0 -4 4 61.01 3.82 0 -4 -4 66.30 3.74 0 4 5 111.25 5.81 0 4 -5 97.38 6.93 0 4 5 109.13 6.23 0 4 -5 105.65 6.03 0 4 -5 109.78 6.34 0 -4 5 112.64 6.15 0 -4 -5 115.63 5.91 0 -4 5 111.36 6.75 0 -4 -5 113.15 6.27 0 -4 5 112.57 6.32 0 -4 5 116.83 7.25 0 4 6 1.27 0.61 0 4 6 1.43 0.52 0 4 -6 2.73 0.78 0 -4 6 1.11 0.76 0 -4 6 1.35 0.96 0 -4 6 1.35 0.57 0 -4 6 2.91 0.72 0 -4 -6 1.00 0.46 0 4 -7 12.26 0.98 0 4 7 13.07 1.80 0 4 7 12.64 1.40 0 4 -7 12.24 1.77 0 -4 7 11.08 1.54 0 -4 7 11.30 1.95 0 -4 7 15.63 2.62 0 -4 -7 13.29 1.20 0 4 -8 134.39 8.22 0 4 8 132.33 8.08 0 4 8 141.14 7.62 0 4 8 142.31 7.58 0 4 -8 142.17 7.16 0 -4 8 142.97 7.98 0 -4 -8 135.72 7.56 0 -4 8 146.58 9.18 0 -4 8 148.59 8.65 0 4 9 1.46 0.79 0 4 9 1.03 0.70 0 4 -9 3.17 1.05 0 4 -9 1.74 0.30 0 4 9 2.43 0.76 0 4 9 2.12 0.72 0 -4 9 2.97 1.28 0 -4 9 2.40 1.42 0 -4 -9 2.66 0.66 0 -4 9 1.97 0.80 0 4 10 29.48 2.34 0 4 10 26.20 3.14 0 4 -10 24.67 3.08 0 4 10 24.46 2.15 0 -4 10 27.72 2.99 0 -4 -10 23.53 2.06 0 -4 -10 29.22 2.47 0 -4 10 29.81 4.13 0 -4 10 30.38 3.63 0 4 11 -0.25 0.52 0 4 11 -0.18 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20 2.25 1.15 0 4 20 4.29 1.74 0 -4 20 4.14 1.22 0 -4 20 5.47 1.96 0 -4 20 5.88 1.83 0 5 0 -0.02 0.21 0 5 0 0.16 0.49 0 5 0 -0.15 0.18 0 5 0 0.17 0.31 0 -5 0 0.37 0.70 0 -5 0 0.11 0.18 0 -5 0 0.29 0.25 0 5 -1 103.88 5.33 0 5 1 105.89 5.19 0 5 -1 104.81 6.04 0 5 1 103.18 5.45 0 5 1 100.78 6.17 0 -5 1 98.68 5.98 0 -5 1 103.08 5.32 0 -5 -1 95.93 6.35 0 -5 1 108.17 6.63 0 -5 -1 104.11 5.42 0 -5 1 103.06 5.40 0 5 2 133.18 7.00 0 5 -2 134.34 7.45 0 5 -2 112.92 7.93 0 5 -2 134.60 6.88 0 -5 -2 137.42 7.00 0 -5 -2 110.49 7.67 0 -5 2 137.67 7.52 0 -5 2 140.64 6.84 0 -5 2 133.36 6.94 0 -5 2 160.47 8.46 0 5 -3 21.23 1.61 0 5 -3 23.98 1.99 0 5 3 22.82 1.39 0 5 3 24.88 1.80 0 5 -3 22.90 3.04 0 -5 3 24.54 2.66 0 -5 3 24.23 1.74 0 -5 -3 26.69 1.81 0 -5 -3 17.94 2.12 0 -5 3 24.68 2.02 0 5 -4 131.13 9.85 0 5 -4 164.00 8.83 0 5 4 163.81 8.59 0 5 -4 156.60 8.37 0 5 4 156.69 8.05 0 -5 4 159.41 8.83 0 -5 4 167.87 8.50 0 -5 -4 166.38 8.57 0 -5 4 174.21 9.88 0 5 5 28.03 2.17 0 5 -5 24.76 2.16 0 5 5 24.55 1.68 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9 9 5.09 0.86 0 9 9 3.31 1.18 0 9 -9 4.83 1.40 0 -9 -9 4.95 0.94 0 -9 9 3.60 1.74 0 -9 -9 2.90 1.03 0 -9 9 2.36 1.05 0 -9 9 7.21 2.65 0 9 -10 107.93 7.44 0 9 10 102.27 5.97 0 9 10 107.77 7.09 0 9 -10 108.92 6.34 0 -9 10 117.63 9.24 0 -9 10 107.52 8.15 0 -9 10 105.22 6.94 0 9 11 -0.30 0.36 0 9 -11 0.06 0.51 0 9 11 -1.13 0.40 0 -9 11 -0.51 0.65 0 -9 11 1.24 0.42 0 -9 -11 0.85 0.43 0 -9 11 -0.28 0.92 0 -9 11 -0.14 0.84 0 9 12 9.86 2.10 0 9 12 11.67 1.55 0 9 -12 8.54 2.14 0 -9 12 13.01 2.31 0 -9 12 12.16 3.43 0 -9 12 10.20 2.82 0 -9 -12 5.27 1.31 0 -9 12 11.24 1.86 0 9 13 3.43 1.38 0 9 13 3.02 1.30 0 -9 13 3.52 2.00 0 -9 13 4.23 1.91 0 -9 13 3.11 1.29 0 -9 13 4.33 1.10 0 9 -14 14.98 3.06 0 9 14 11.68 2.50 0 -9 14 14.17 2.27 0 -9 14 13.03 2.60 0 -9 14 16.98 4.16 0 -9 14 17.00 3.70 0 9 -15 5.17 1.85 0 9 15 9.60 2.35 0 -9 15 9.02 1.86 0 -9 15 7.04 2.51 0 -9 15 10.81 3.42 0 -9 15 5.51 1.71 0 9 -16 3.09 1.66 0 9 16 5.67 1.75 0 -9 16 4.27 1.99 0 -9 16 4.76 1.43 0 -9 16 5.04 1.27 0 9 -17 5.64 2.23 0 9 17 8.65 2.34 0 -9 17 10.16 2.00 0 -9 17 13.33 3.39 0 -9 17 9.92 2.32 0 9 18 2.50 1.09 0 -9 18 0.96 0.89 0 -9 18 0.56 0.88 0 10 0 -0.71 0.49 0 10 0 -0.12 0.22 0 -10 0 2.25 1.32 0 -10 0 0.50 0.24 0 10 -1 10.92 2.18 0 10 1 12.94 2.42 0 10 1 13.90 1.00 0 10 -1 15.35 1.21 0 10 1 15.76 1.72 0 -10 -1 12.67 2.76 0 -10 -1 14.97 1.30 0 -10 1 17.95 3.39 0 -10 1 15.41 1.19 0 10 2 52.65 3.52 0 10 -2 53.96 4.44 0 10 2 57.92 4.85 0 10 -2 53.37 3.24 0 10 2 54.09 2.79 0 -10 2 57.97 5.32 0 -10 2 52.51 3.43 0 -10 2 56.65 3.15 0 -10 -2 52.83 3.40 0 -10 -2 50.83 4.79 0 10 -3 1.19 0.81 0 10 3 1.10 0.94 0 10 -3 1.98 0.50 0 10 3 1.29 0.75 0 -10 3 1.59 0.69 0 -10 3 2.59 0.48 0 -10 -3 1.81 1.19 0 -10 -3 2.80 0.65 0 -10 3 1.75 1.57 0 10 -4 6.53 1.63 0 10 4 5.85 1.22 0 10 4 3.35 1.40 0 -10 -4 4.55 1.56 0 -10 4 5.00 2.15 0 -10 4 5.31 1.15 0 -10 4 5.96 0.81 0 10 -5 7.79 1.71 0 10 5 8.94 1.57 0 -10 5 8.80 1.12 0 -10 5 6.60 1.38 0 -10 -5 8.67 2.09 0 -10 5 7.44 2.37 0 10 6 50.81 2.73 0 10 6 54.88 2.70 0 10 -6 48.89 4.20 0 10 6 49.54 3.78 0 -10 6 51.35 3.25 0 -10 6 55.70 3.84 0 -10 -6 41.79 4.15 0 -10 6 53.22 5.60 0 10 7 0.04 0.57 0 10 7 1.11 0.32 0 10 -7 1.83 0.81 0 -10 7 2.94 1.91 0 -10 7 0.70 0.67 0 -10 7 1.35 0.33 0 -10 -7 1.40 0.91 0 -10 7 1.83 1.32 0 10 8 42.78 3.64 0 10 -8 52.71 4.25 0 10 8 46.30 2.64 0 -10 8 50.90 5.49 0 -10 8 47.63 3.66 0 -10 -8 32.91 3.60 0 -10 8 51.26 4.87 0 10 -9 40.37 3.66 0 10 9 38.50 3.37 0 10 9 33.25 2.34 0 -10 9 46.63 6.51 0 -10 9 42.04 5.37 0 -10 -9 23.80 2.92 0 -10 9 43.41 3.41 0 10 -10 3.13 1.13 0 10 10 2.25 1.11 0 -10 -10 2.17 0.86 0 -10 10 4.24 2.17 0 -10 10 3.69 1.14 0 -10 10 1.35 1.24 0 10 -11 5.49 1.77 0 10 -11 5.68 1.03 0 10 11 7.35 1.85 0 -10 11 5.84 1.28 0 -10 11 5.49 2.18 0 -10 11 5.18 1.53 0 -10 -11 3.85 1.08 0 -10 11 6.95 2.82 0 10 12 8.22 2.06 0 10 -12 9.64 2.25 0 -10 12 9.92 2.10 0 -10 12 11.51 3.46 0 -10 12 8.15 1.51 0 -10 12 9.68 2.80 0 10 -13 0.66 0.91 0 10 13 1.59 0.94 0 -10 13 2.17 1.94 0 -10 13 0.14 1.34 0 -10 13 2.21 1.13 0 10 14 4.60 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-2 -5 -4 135.67 7.46 2 -5 4 132.10 7.49 2 -5 4 146.84 8.13 2 -5 4 137.57 7.09 2 5 5 105.17 5.36 -2 5 -5 96.71 6.18 2 5 5 98.94 6.01 2 -5 5 102.98 5.58 -2 -5 -5 109.46 5.88 2 -5 5 96.68 5.90 2 -5 5 96.21 6.38 2 -5 5 109.30 7.05 -2 5 -6 44.84 2.93 -2 5 -6 47.10 3.52 2 5 6 46.93 2.75 2 5 6 45.88 3.36 -2 -5 -6 46.95 3.09 -2 -5 -6 37.99 2.62 2 -5 6 43.43 3.22 2 -5 6 53.90 4.40 2 -5 6 48.75 3.00 2 -5 6 46.20 3.76 -2 5 -7 31.69 2.24 -2 5 -7 30.71 2.87 2 5 7 32.73 2.20 2 5 7 32.58 2.74 -2 -5 -7 35.47 2.51 2 -5 7 32.07 3.06 -2 -5 -7 28.84 2.10 2 -5 7 30.65 2.64 2 -5 7 35.11 2.48 2 -5 7 35.56 3.58 -2 5 -8 52.13 4.10 -2 5 -8 49.22 3.18 2 5 8 57.71 3.37 2 5 8 51.96 3.91 -2 -5 -8 56.38 3.58 2 -5 8 52.15 3.57 -2 -5 -8 46.21 3.16 2 -5 8 53.08 4.83 2 -5 8 51.45 3.77 2 -5 8 53.18 4.33 2 5 9 71.00 5.22 -2 5 -9 70.96 5.41 2 5 9 77.26 4.62 -2 5 -9 74.56 4.33 2 -5 9 80.11 6.33 2 -5 9 81.10 4.98 2 -5 9 76.98 5.16 2 -5 9 75.06 5.60 2 5 10 17.42 2.57 -2 5 -10 18.28 2.80 2 5 10 17.39 2.03 -2 5 -10 17.40 1.40 2 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5 3.00 1.32 -2 -6 5 4.42 0.94 2 -6 -5 2.43 0.78 -2 6 4 15.18 1.40 2 6 -4 18.46 1.71 2 6 -4 15.90 1.35 -2 -6 4 16.13 1.44 -2 -6 4 15.61 2.79 2 -6 -4 13.47 1.56 -2 -6 4 18.26 1.73 -2 -6 4 14.89 1.35 2 6 -3 50.07 3.08 -2 6 3 55.41 3.21 -2 6 3 51.09 3.98 2 6 -3 53.19 3.62 -2 -6 3 52.93 4.68 2 -6 -3 55.67 3.70 -2 -6 3 53.02 3.28 -2 -6 3 48.90 3.58 -2 -6 3 57.81 3.18 2 6 -2 8.02 0.87 -2 6 2 6.27 1.33 -2 6 2 7.39 0.92 2 6 -2 6.79 1.22 -2 6 2 7.48 0.89 2 6 -2 5.74 1.87 -2 6 2 6.49 1.52 -2 -6 2 8.60 0.91 2 -6 -2 9.28 1.52 -2 -6 2 8.51 1.11 -2 -6 2 10.84 2.43 2 6 -1 1.32 0.62 -2 6 1 1.10 0.66 2 6 -1 0.13 0.57 2 6 -1 0.50 0.45 -2 6 1 0.73 0.37 2 6 -1 0.39 0.24 -2 6 1 0.36 0.63 -2 6 1 1.05 0.31 2 -6 -1 0.45 0.66 -2 -6 1 1.22 0.34 -2 -6 1 1.13 0.44 -2 -6 1 0.73 0.92 -2 6 0 39.26 2.38 -2 6 0 37.05 2.00 2 6 0 37.56 2.55 2 6 0 38.75 3.04 -2 6 0 30.54 3.05 -2 6 0 41.68 3.10 -2 -6 0 38.57 2.48 2 -6 0 41.72 3.27 -2 -6 0 38.13 2.00 -2 -6 0 32.76 3.64 -2 6 -1 17.38 2.11 -2 6 -1 18.77 2.66 2 6 1 16.78 1.57 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0.67 -4 -4 5 2.45 1.46 -4 -4 5 2.16 0.54 -4 4 4 8.06 0.73 4 4 -4 10.15 1.24 4 4 -4 10.23 0.91 4 4 -4 6.48 1.79 -4 -4 4 10.44 0.96 -4 -4 4 9.70 1.11 -4 -4 4 9.97 2.26 4 -4 -4 5.63 0.47 4 4 -3 0.09 0.41 -4 4 3 0.03 0.35 4 4 -3 0.21 0.27 4 4 -3 -0.79 0.33 -4 4 3 -0.24 0.30 -4 -4 3 -0.65 0.56 -4 -4 3 -0.25 0.24 4 -4 -3 -0.31 0.17 -4 -4 3 -0.18 0.21 -4 4 2 15.58 1.41 4 4 -2 15.60 1.38 4 4 -2 17.43 1.55 -4 4 2 13.53 1.69 -4 -4 2 16.50 1.44 -4 -4 2 16.01 1.20 4 -4 -2 16.32 1.23 -4 -4 2 15.71 2.87 -4 4 1 158.54 8.61 -4 4 1 155.52 8.51 -4 4 1 148.65 8.26 4 4 -1 155.18 8.46 4 4 -1 162.42 8.59 4 -4 -1 146.57 8.58 4 -4 -1 189.41 8.36 4 -4 -1 174.69 8.58 -4 -4 1 125.91 9.64 -4 -4 1 152.25 8.38 4 4 0 85.83 4.98 -4 4 0 76.82 4.95 -4 4 0 81.74 4.92 -4 4 0 78.58 4.64 4 4 0 81.61 4.80 -4 4 0 82.38 4.11 4 -4 0 89.59 5.08 4 -4 0 83.14 4.97 4 -4 0 80.35 4.71 -4 -4 0 81.73 4.74 4 4 1 104.30 5.91 -4 4 -1 101.56 5.89 -4 4 -1 103.29 5.73 -4 4 -1 101.53 5.93 4 4 1 109.71 6.12 -4 4 -1 97.13 6.16 -4 4 -1 106.06 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37.50 2.26 -4 -4 -5 38.69 2.78 4 -4 5 34.85 2.76 4 4 6 54.55 3.98 4 4 6 56.89 3.48 -4 4 -6 57.71 4.29 -4 4 -6 59.82 3.64 4 -4 6 63.12 3.70 4 -4 6 58.92 4.00 -4 -4 -6 58.43 3.41 4 -4 6 50.40 4.15 -4 4 -7 7.82 1.66 4 4 7 7.54 1.48 4 4 7 7.47 1.14 -4 4 -7 7.43 1.10 4 4 7 8.64 1.47 4 -4 7 6.28 1.31 -4 -4 -7 6.80 1.02 4 -4 7 7.57 1.70 4 -4 7 7.34 1.24 -4 4 -8 0.07 0.23 4 4 8 0.10 0.50 4 4 8 -1.05 0.47 -4 4 -8 0.44 0.77 4 4 8 0.52 0.74 4 -4 8 -0.01 0.50 4 -4 8 -0.21 0.76 4 -4 8 -0.47 0.31 4 4 9 0.13 0.74 4 4 9 -0.14 0.61 4 4 9 0.34 0.54 -4 4 -9 -0.03 0.27 -4 4 -9 0.38 0.70 4 -4 9 0.58 0.80 4 -4 9 0.08 0.83 4 -4 9 0.42 0.51 4 4 10 41.40 3.17 4 4 10 45.45 3.54 -4 4 -10 43.11 4.12 4 4 10 38.68 3.58 -4 4 -10 43.59 2.84 4 -4 10 42.52 3.39 4 -4 10 38.29 4.47 4 -4 10 43.55 3.61 -4 4 -11 3.35 1.56 4 4 11 3.15 1.07 4 4 11 1.25 0.84 -4 4 -11 2.00 0.66 4 4 11 3.97 1.24 4 -4 11 2.77 1.05 4 -4 11 3.51 1.25 4 -4 11 3.33 1.52 4 4 12 69.49 4.89 4 4 12 67.10 5.24 -4 4 -12 62.40 5.55 -4 4 -12 62.22 3.81 4 4 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9 22.24 3.49 10 -7 9 27.48 4.03 -10 7 -10 -0.47 0.33 -10 7 -10 0.66 1.38 10 7 10 0.11 0.77 10 -7 10 0.58 0.29 10 -7 10 -0.41 0.63 10 -7 10 1.05 1.03 10 7 11 -0.24 0.61 -10 7 -11 3.01 1.59 -10 7 -11 -0.16 0.47 10 -7 11 2.62 0.67 10 -7 11 0.56 1.03 10 -7 11 1.41 0.98 -10 7 -12 0.05 0.92 10 7 12 -0.62 0.70 10 -7 12 -0.73 1.05 10 -7 12 0.28 0.98 10 -7 12 3.43 0.85 10 7 13 6.16 1.93 -10 7 -13 7.34 2.41 10 -7 13 7.65 1.78 10 -7 13 8.19 2.12 10 -7 13 10.91 2.93 -10 7 -14 11.30 3.47 10 7 14 19.78 3.80 10 -7 14 19.90 3.53 10 -7 14 21.83 4.24 -10 7 -15 6.82 3.13 10 7 15 11.51 2.98 10 -7 15 2.58 1.53 10 -7 15 8.96 2.31 -10 8 19 1.54 0.91 -10 8 19 2.34 1.29 -10 -8 19 3.12 1.58 -10 -8 19 2.49 1.97 -10 -8 19 1.65 1.09 -10 8 18 0.73 0.98 -10 8 18 0.58 0.60 -10 -8 18 3.39 2.53 -10 -8 18 2.22 1.49 -10 -8 18 5.33 1.50 -10 8 17 1.73 1.20 -10 8 17 2.97 1.35 -10 8 17 0.99 0.85 -10 -8 17 1.62 1.36 -10 -8 17 1.62 0.84 -10 -8 17 1.06 1.73 -10 8 16 1.54 1.07 -10 8 16 2.14 1.03 -10 8 16 2.05 0.85 -10 8 16 3.48 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0.68 -23 -7 2 -1.41 1.42 -23 -7 2 1.73 1.36 -23 7 1 6.15 2.11 -23 -7 1 5.72 2.16 -23 7 0 6.58 2.14 -23 7 0 5.71 2.63 -23 -7 0 9.55 3.14 -23 -8 5 5.42 2.69 -23 -8 4 7.75 3.48 -24 0 10 25.47 4.49 -24 0 9 -2.38 1.31 -24 0 8 8.97 2.67 -24 0 8 5.51 1.95 -24 0 7 -1.93 0.69 -24 0 6 65.91 6.29 -24 0 5 -0.10 1.52 -24 0 4 -0.91 1.36 -24 0 3 -0.21 1.08 -24 0 2 9.66 3.11 -24 0 1 -1.58 1.22 -24 0 0 -3.09 1.10 -24 0 -1 -4.11 1.05 -24 0 -2 -4.08 0.97 -24 1 11 3.68 2.30 -24 -1 11 6.78 2.61 -24 1 10 24.96 4.13 -24 -1 10 23.68 4.26 -24 1 9 7.94 2.69 -24 -1 9 6.34 2.38 -24 -1 9 4.02 2.41 -24 1 8 0.25 1.68 -24 -1 8 3.02 1.19 -24 -1 8 -3.39 1.25 -24 1 7 -0.96 1.27 -24 -1 7 2.74 1.53 -24 -1 7 -3.32 1.25 -24 1 6 1.55 1.56 -24 -1 6 -0.50 1.68 -24 1 5 9.45 2.73 -24 -1 5 7.03 2.83 -24 1 4 -1.05 1.57 -24 -1 4 -2.18 0.81 -24 1 3 6.95 2.52 -24 -1 3 3.18 2.37 -24 1 2 0.62 1.81 -24 -1 2 -1.04 1.84 -24 1 1 12.39 3.09 -24 -1 1 7.45 2.71 -24 1 0 -0.66 1.33 -24 1 -1 -2.96 1.14 -24 -1 -1 -2.81 1.22 -24 1 -2 0.05 1.57 -24 -1 -2 -2.77 1.41 -24 2 11 24.31 4.10 -24 -2 11 27.47 4.59 -24 2 10 -0.76 1.10 -24 -2 10 2.50 1.42 -24 -2 10 -3.97 1.20 -24 2 9 4.19 2.09 -24 -2 9 9.39 3.31 -24 -2 9 1.88 2.05 -24 2 8 -1.72 1.08 -24 -2 8 5.74 2.19 -24 -2 8 -1.51 1.01 -24 2 7 6.11 2.55 -24 -2 7 11.09 3.23 -24 -2 7 8.05 2.58 -24 2 6 -0.18 1.35 -24 2 5 0.47 1.15 -24 -2 5 0.27 1.48 -24 2 4 8.93 2.73 -24 -2 4 8.79 2.99 -24 2 3 0.71 1.29 -24 -2 3 -1.71 1.64 -24 2 2 -0.40 1.49 -24 -2 2 1.62 1.90 -24 2 1 -1.02 0.91 -24 -2 1 -1.86 1.43 -24 2 0 -2.25 1.18 -24 -2 0 -0.77 1.23 -24 2 -1 3.30 2.08 -24 -2 -1 0.27 1.19 24 2 2 2.16 0.96 -24 2 -2 -4.06 0.93 -24 3 11 0.81 1.50 -24 -3 11 -3.69 1.48 -24 -3 11 1.61 2.11 -24 3 10 -0.96 0.96 -24 -3 10 -4.32 1.10 -24 -3 10 0.74 1.41 -24 3 9 -1.21 1.08 -24 -3 9 1.66 1.29 -24 -3 9 -3.79 1.35 -24 3 8 -0.15 1.22 -24 -3 8 1.94 1.33 -24 -3 8 -0.96 1.85 -24 3 7 3.85 2.07 -24 -3 7 -0.51 1.83 -24 -3 7 1.32 0.91 -24 3 6 2.21 1.55 -24 -3 6 5.46 2.23 -24 -3 6 -0.91 1.99 -24 3 5 -0.23 1.02 -24 -3 5 -3.49 1.40 -24 3 4 2.25 1.75 -24 -3 4 -0.69 1.70 -24 3 3 0.58 1.17 -24 -3 3 -1.48 1.09 -24 3 2 3.98 2.17 -24 -3 2 5.81 2.69 -24 3 1 -1.35 0.44 -24 -3 1 -1.07 1.04 -24 3 0 2.17 1.51 -24 -3 0 -0.87 1.63 -24 -3 -1 -0.40 1.26 -24 4 10 1.48 1.61 -24 -4 10 2.89 2.28 -24 -4 10 -2.17 1.39 -24 4 9 -0.73 1.25 -24 -4 9 1.68 1.22 -24 -4 9 -3.92 1.17 -24 4 8 -0.83 1.01 -24 -4 8 1.17 1.56 -24 -4 8 -1.76 1.42 -24 4 7 -1.50 0.87 -24 -4 7 0.73 1.02 -24 -4 7 -2.42 0.85 -24 4 6 7.50 2.57 -24 -4 6 10.00 3.67 -24 -4 6 5.78 2.43 -24 4 5 0.89 1.04 -24 -4 5 -0.68 1.25 -24 -4 5 3.24 1.32 -24 4 4 -0.05 1.10 -24 -4 4 0.88 1.54 -24 4 3 9.96 2.77 -24 -4 3 7.81 2.87 -24 4 2 -0.93 1.34 -24 -4 2 -1.63 1.46 -24 4 1 12.69 3.30 -24 -4 1 12.72 3.37 -24 4 0 2.80 1.62 -24 -4 0 -2.08 1.45 -24 4 -1 -1.01 0.86 -24 -4 -1 -1.30 1.55 -24 5 9 3.28 1.79 -24 -5 9 4.27 2.17 -24 -5 9 8.95 2.75 -24 5 8 -0.53 1.17 -24 -5 8 3.13 1.46 -24 -5 8 -2.44 1.15 -24 5 7 0.04 1.30 -24 -5 7 3.18 1.87 -24 -5 7 -0.84 1.56 -24 5 6 6.23 2.38 -24 -5 6 5.13 2.46 -24 -5 6 2.55 2.31 -24 5 5 1.53 1.47 -24 -5 5 3.44 1.74 -24 -5 5 1.22 1.95 -24 5 4 -0.46 1.28 -24 -5 4 2.07 1.16 -24 -5 4 -1.20 1.58 -24 5 3 5.41 2.22 -24 -5 3 2.31 2.17 -24 5 2 8.93 2.57 -24 -5 2 4.99 2.29 -24 5 1 0.67 1.48 -24 -5 1 -2.10 1.28 -24 -6 7 0.95 1.45 -24 6 6 6.25 2.45 -24 -6 6 4.76 2.47 -24 -6 6 9.23 2.74 -24 6 5 -0.81 1.04 -24 -6 5 0.56 1.61 -24 -6 5 2.20 1.55 -24 6 4 2.76 1.61 -24 -6 4 2.07 1.70 -24 -6 4 7.51 3.02 -24 6 3 -1.38 1.01 -24 -6 3 3.81 1.45 -25 0 9 -1.06 1.05 -25 0 8 4.77 2.11 -25 0 7 -2.86 0.71 -25 0 6 5.60 2.36 -25 0 5 -1.39 1.55 -25 0 4 0.11 1.81 -25 0 3 -2.80 0.67 -25 0 2 -3.04 1.30 -25 0 1 -1.79 0.87 -25 1 9 -0.51 1.68 -25 -1 9 -1.58 1.57 -25 1 8 -2.20 1.38 -25 -1 8 2.62 1.39 -25 -1 8 -3.42 1.13 -25 1 7 -1.24 1.71 -25 -1 7 0.80 2.21 -25 -1 7 7.61 2.76 -25 1 6 -0.52 1.33 -25 1 5 -2.00 0.89 -25 -1 5 -2.17 1.58 -25 1 4 -2.11 1.35 -25 -1 4 0.40 1.99 -25 1 3 2.46 1.71 -25 -1 3 2.36 1.80 -25 1 2 13.03 3.51 -25 -1 2 13.03 3.65 -25 1 1 -1.81 0.83 -25 -1 1 -0.85 1.18 -25 2 8 2.45 2.08 -25 -2 8 -1.39 1.85 -25 2 7 -1.68 1.33 -25 -2 7 3.72 1.98 -25 -2 7 -1.93 1.64 -25 2 6 -0.91 1.32 -25 -2 6 -4.88 1.44 -25 2 5 1.43 1.52 -25 -2 5 -0.33 1.82 -25 2 4 4.67 2.35 -25 -2 4 3.11 2.05 -25 2 3 25.78 4.55 -25 -2 3 18.13 4.22 -25 2 2 -0.47 1.75 -25 -2 2 -3.49 1.26 -25 2 1 5.47 2.31 -25 -2 1 0.23 2.01 -25 3 7 -2.20 1.09 -25 -3 7 2.89 1.61 -25 -3 7 -2.09 0.93 -25 3 6 2.74 1.77 -25 -3 6 8.17 2.66 -25 -3 6 5.03 2.29 -25 3 5 -0.62 0.74 -25 -3 5 -2.26 0.94 -25 3 4 16.07 3.66 -25 -3 4 11.10 3.49 -25 3 3 -2.27 0.56 -25 -3 3 -1.31 1.77 -25 3 2 1.88 1.87 -25 -3 2 1.84 1.70 -25 -4 5 2.68 1.42 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 45526 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 S1 S 0.37667(3) 0.74732(4) 0.68349(4) 0.02173(13) Uani 1 1 d . S2 S 0.56217(3) 0.69865(4) 0.41702(3) 0.01606(12) Uani 1 1 d . P P 0.47408(3) 0.58761(4) 0.40227(3) 0.01195(11) Uani 1 1 d . N1 N 0.41650(10) 0.67519(12) 0.53587(10) 0.0126(3) Uani 1 1 d . N2 N 0.44690(9) 0.57390(12) 0.64845(10) 0.0125(3) Uani 1 1 d . C1 C 0.45431(11) 0.59345(14) 0.50992(12) 0.0114(4) Uani 1 1 d . C2 C 0.41299(12) 0.66472(15) 0.62206(13) 0.0140(4) Uani 1 1 d . C3 C 0.38307(12) 0.76050(15) 0.47972(13) 0.0155(4) Uani 1 1 d . H3A H 0.4173 0.7817 0.4427 0.019 Uiso 1 1 calc R H3B H 0.3769 0.8191 0.5173 0.019 Uiso 1 1 calc R C4 C 0.30786(12) 0.73372(16) 0.42056(14) 0.0203(5) Uani 1 1 d . H4A H 0.3145 0.6788 0.3796 0.024 Uiso 1 1 calc R H4B H 0.2746 0.7077 0.4571 0.024 Uiso 1 1 calc R C5 C 0.27170(13) 0.82517(18) 0.36813(15) 0.0244(5) Uani 1 1 d . H5A H 0.3073 0.8556 0.3368 0.029 Uiso 1 1 calc R H5B H 0.2605 0.8772 0.4092 0.029 Uiso 1 1 calc R C6 C 0.20038(15) 0.7983(2) 0.30175(17) 0.0416(7) Uani 1 1 d . H6A H 0.1652 0.7669 0.3322 0.062 Uiso 1 1 calc GR H6B H 0.2116 0.7504 0.2585 0.062 Uiso 1 1 calc GR H6C H 0.1784 0.8605 0.2718 0.062 Uiso 1 1 calc GR C7 C 0.45442(12) 0.53086(16) 0.73693(12) 0.0141(4) Uani 1 1 d . H7A H 0.4458 0.4563 0.7320 0.017 Uiso 1 1 calc R H7B H 0.4157 0.5608 0.7639 0.017 Uiso 1 1 calc R C8 C 0.53063(12) 0.55072(15) 0.79664(12) 0.0136(4) Uani 1 1 d . H8A H 0.5691 0.5154 0.7727 0.016 Uiso 1 1 calc R H8B H 0.5413 0.6248 0.7978 0.016 Uiso 1 1 calc R C9 C 0.53463(12) 0.51361(16) 0.88982(12) 0.0167(4) Uani 1 1 d . H9A H 0.5211 0.4405 0.8882 0.020 Uiso 1 1 calc R H9B H 0.4981 0.5518 0.9149 0.020 Uiso 1 1 calc R C10 C 0.61209(12) 0.52771(16) 0.94883(14) 0.0195(5) Uani 1 1 d . H10A H 0.6117 0.5066 1.0089 0.029 Uiso 1 1 calc GR H10B H 0.6265 0.5997 0.9489 0.029 Uiso 1 1 calc GR H10C H 0.6479 0.4860 0.9267 0.029 Uiso 1 1 calc GR C11 C 0.52595(11) 0.47027(14) 0.41917(12) 0.0110(4) Uani 1 1 d . C12 C 0.61041(12) 0.68294(15) 0.52873(13) 0.0141(4) Uani 1 1 d . C13 C 0.59269(12) 0.74733(15) 0.59219(13) 0.0161(4) Uani 1 1 d . H13 H 0.5567 0.7997 0.5752 0.019 Uiso 1 1 calc R C14 C 0.62773(13) 0.73467(16) 0.68000(14) 0.0194(5) Uani 1 1 d . H14 H 0.6156 0.7781 0.7233 0.023 Uiso 1 1 calc R C15 C 0.68062(13) 0.65848(17) 0.70455(14) 0.0206(5) Uani 1 1 d . H15 H 0.7043 0.6495 0.7648 0.025 Uiso 1 1 calc R C16 C 0.69910(12) 0.59542(16) 0.64149(14) 0.0195(5) Uani 1 1 d . H16 H 0.7357 0.5439 0.6586 0.023 Uiso 1 1 calc R C17 C 0.66402(12) 0.60747(16) 0.55310(13) 0.0167(4) Uani 1 1 d . H17 H 0.6767 0.5644 0.5099 0.020 Uiso 1 1 calc R S1' S 0.00014(4) 0.15640(4) 0.66319(3) 0.02171(13) Uani 1 1 d . S2' S -0.09547(3) 0.60592(4) 0.62406(3) 0.01330(11) Uani 1 1 d . P' P 0.01514(3) 0.57034(4) 0.60806(3) 0.01006(11) Uani 1 1 d . N1' N 0.00799(9) 0.36350(12) 0.64677(10) 0.0118(3) Uani 1 1 d . N2' N 0.01272(10) 0.71716(12) 0.47806(10) 0.0117(3) Uani 1 1 d . C1' C 0.00546(11) 0.43674(14) 0.58130(12) 0.0100(4) Uani 1 1 d . C2' C -0.00189(12) 0.26803(15) 0.61082(12) 0.0139(4) Uani 1 1 d . C3' C 0.02882(12) 0.38257(15) 0.74177(12) 0.0136(4) Uani 1 1 d . H3'A H 0.0052 0.3307 0.7726 0.016 Uiso 1 1 calc R H3'B H 0.0103 0.4505 0.7544 0.016 Uiso 1 1 calc R C4' C 0.11303(12) 0.37841(16) 0.77572(12) 0.0150(4) Uani 1 1 d . H4'A H 0.1363 0.4297 0.7440 0.018 Uiso 1 1 calc R H4'B H 0.1311 0.3103 0.7628 0.018 Uiso 1 1 calc R C5' C 0.13764(12) 0.39861(16) 0.87438(13) 0.0172(4) Uani 1 1 d . H5'A H 0.1251 0.4697 0.8868 0.021 Uiso 1 1 calc R H5'B H 0.1104 0.3525 0.9061 0.021 Uiso 1 1 calc R C6' C 0.22109(13) 0.38186(19) 0.90757(15) 0.0265(5) Uani 1 1 d . H6'A H 0.2356 0.3981 0.9704 0.040 Uiso 1 1 calc GR H6'B H 0.2481 0.4263 0.8752 0.040 Uiso 1 1 calc GR H6'C H 0.2331 0.3105 0.8985 0.040 Uiso 1 1 calc GR C7' C 0.00814(11) 0.61424(14) 0.49689(12) 0.0100(4) Uani 1 1 d . C8' C 0.03021(12) 0.80060(15) 0.54200(13) 0.0141(4) Uani 1 1 d . H8'A H 0.0173 0.7793 0.5974 0.017 Uiso 1 1 calc R H8'B H -0.0008 0.8605 0.5191 0.017 Uiso 1 1 calc R C9' C 0.11144(12) 0.83117(16) 0.56122(14) 0.0189(5) Uani 1 1 d . H9'A H 0.1253 0.8497 0.5057 0.023 Uiso 1 1 calc R H9'B H 0.1427 0.7727 0.5875 0.023 Uiso 1 1 calc R C10' C 0.12573(14) 0.92143(18) 0.62418(16) 0.0284(6) Uani 1 1 d . H10D H 0.0900 0.9765 0.6009 0.034 Uiso 1 1 calc R H10E H 0.1169 0.9000 0.6817 0.034 Uiso 1 1 calc R C11' C 0.20413(17) 0.9627(2) 0.6375(2) 0.0486(8) Uani 1 1 d . H11A H 0.2099 1.0220 0.6766 0.073 Uiso 1 1 calc GR H11B H 0.2135 0.9830 0.5807 0.073 Uiso 1 1 calc GR H11C H 0.2397 0.9097 0.6639 0.073 Uiso 1 1 calc GR C12' C -0.15338(11) 0.57054(16) 0.52079(12) 0.0141(4) Uani 1 1 d . C13' C -0.17858(12) 0.64593(17) 0.45806(13) 0.0177(4) Uani 1 1 d . H13' H -0.1629 0.7146 0.4693 0.021 Uiso 1 1 calc R C14' C -0.22695(13) 0.61997(19) 0.37871(14) 0.0233(5) Uani 1 1 d . H14' H -0.2448 0.6713 0.3362 0.028 Uiso 1 1 calc R C15' C -0.24901(13) 0.51970(19) 0.36165(14) 0.0240(5) Uani 1 1 d . H15' H -0.2816 0.5024 0.3072 0.029 Uiso 1 1 calc R C16' C -0.22379(13) 0.44441(18) 0.42367(14) 0.0220(5) Uani 1 1 d . H16' H -0.2389 0.3756 0.4116 0.026 Uiso 1 1 calc R C17' C -0.17636(12) 0.46969(16) 0.50360(14) 0.0168(4) Uani 1 1 d . H17' H -0.1596 0.4183 0.5464 0.020 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 S1 0.0291(3) 0.0181(3) 0.0209(3) -0.0050(2) 0.0117(2) 0.0050(2) S2 0.0239(3) 0.0122(2) 0.0131(2) 0.00220(18) 0.0064(2) -0.0032(2) P 0.0179(3) 0.0095(2) 0.0086(2) 0.00090(18) 0.0033(2) 0.0013(2) N1 0.0164(9) 0.0096(8) 0.0120(8) -0.0002(6) 0.0037(7) 0.0008(7) N2 0.0157(9) 0.0128(8) 0.0096(8) -0.0010(6) 0.0043(7) 0.0002(7) C1 0.0156(11) 0.0076(9) 0.0110(9) -0.0007(7) 0.0034(8) -0.0016(7) C2 0.0143(11) 0.0137(10) 0.0143(9) -0.0025(7) 0.0037(8) -0.0020(8) C3 0.0185(11) 0.0094(9) 0.0186(10) 0.0017(8) 0.0046(8) 0.0015(8) C4 0.0191(12) 0.0195(11) 0.0209(11) 0.0019(8) 0.0017(9) -0.0006(9) C5 0.0245(13) 0.0264(12) 0.0221(11) 0.0052(9) 0.0051(10) 0.0085(10) C6 0.0283(16) 0.0575(19) 0.0333(15) 0.0095(13) -0.0047(12) 0.0125(13) C7 0.0196(12) 0.0162(10) 0.0074(9) -0.0001(7) 0.0051(8) -0.0022(8) C8 0.0187(11) 0.0121(10) 0.0108(9) -0.0007(7) 0.0052(8) -0.0019(8) C9 0.0195(12) 0.0189(11) 0.0113(9) 0.0008(8) 0.0029(8) -0.0011(9) C10 0.0214(12) 0.0173(11) 0.0177(10) 0.0005(8) 0.0005(9) 0.0015(9) C11 0.0117(10) 0.0106(9) 0.0110(9) -0.0021(7) 0.0034(7) -0.0022(7) C12 0.0163(11) 0.0125(10) 0.0143(10) 0.0016(7) 0.0052(8) -0.0044(8) C13 0.0184(11) 0.0112(10) 0.0200(10) -0.0011(8) 0.0072(9) -0.0007(8) C14 0.0250(13) 0.0188(11) 0.0166(10) -0.0050(8) 0.0092(9) -0.0026(9) C15 0.0224(13) 0.0238(12) 0.0153(10) -0.0002(8) 0.0036(9) -0.0043(9) C16 0.0163(12) 0.0193(11) 0.0229(11) 0.0025(9) 0.0044(9) 0.0026(9) C17 0.0178(12) 0.0157(10) 0.0190(10) -0.0020(8) 0.0089(9) -0.0020(8) S1' 0.0366(4) 0.0125(3) 0.0157(3) 0.00625(19) 0.0053(2) -0.0010(2) S2' 0.0161(3) 0.0154(2) 0.0096(2) -0.00239(18) 0.00537(19) 0.0004(2) P' 0.0141(3) 0.0105(2) 0.0060(2) -0.00057(17) 0.00309(19) -0.00098(19) N1' 0.0166(9) 0.0120(8) 0.0070(7) 0.0018(6) 0.0032(6) -0.0004(7) N2' 0.0168(9) 0.0098(8) 0.0096(8) 0.0003(6) 0.0052(7) -0.0009(7) C1' 0.0107(10) 0.0112(9) 0.0087(9) 0.0020(7) 0.0032(7) 0.0003(7) C2' 0.0161(11) 0.0151(10) 0.0109(9) 0.0026(7) 0.0042(8) 0.0002(8) C3' 0.0190(11) 0.0167(10) 0.0059(8) 0.0019(7) 0.0044(8) 0.0004(8) C4' 0.0174(11) 0.0185(10) 0.0102(9) 0.0011(7) 0.0054(8) 0.0000(8) C5' 0.0180(12) 0.0198(11) 0.0127(10) -0.0016(8) 0.0011(8) 0.0017(9) C6' 0.0214(13) 0.0311(13) 0.0241(12) -0.0042(10) -0.0004(10) -0.0022(10) C7' 0.0107(10) 0.0099(9) 0.0098(9) 0.0013(7) 0.0029(7) -0.0004(7) C8' 0.0209(12) 0.0097(9) 0.0125(9) -0.0023(7) 0.0053(8) 0.0006(8) C9' 0.0208(12) 0.0191(11) 0.0181(10) -0.0034(8) 0.0070(9) -0.0031(9) C10' 0.0325(15) 0.0233(12) 0.0291(13) -0.0103(10) 0.0065(11) -0.0108(10) C11' 0.0454(19) 0.0525(19) 0.0445(17) -0.0112(14) 0.0030(14) -0.0299(15) C12' 0.0121(11) 0.0206(11) 0.0106(9) -0.0017(8) 0.0050(8) 0.0001(8) C13' 0.0170(12) 0.0190(11) 0.0185(10) 0.0019(8) 0.0071(9) 0.0008(9) C14' 0.0170(12) 0.0379(14) 0.0152(10) 0.0067(9) 0.0044(9) 0.0042(10) C15' 0.0147(12) 0.0433(15) 0.0141(10) -0.0064(9) 0.0029(9) -0.0012(10) C16' 0.0180(12) 0.0269(12) 0.0233(11) -0.0115(9) 0.0094(9) -0.0051(9) C17' 0.0148(11) 0.0179(11) 0.0191(10) -0.0010(8) 0.0066(8) 0.0002(8) 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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 C12 S2 P 102.86(7) . . C1 P S2 100.40(7) . . C11 P S2 101.44(7) . . C11 P C1 96.54(9) . . C1 N1 C3 125.72(16) . . C2 N1 C1 110.47(16) . . C2 N1 C3 123.80(17) . . C2 N2 C7 123.86(17) . . C2 N2 C11 110.65(16) . 3_666 C11 N2 C7 125.48(16) 3_666 . N1 C1 P 121.85(14) . . C11 C1 P 131.03(15) 3_666 . C11 C1 N1 107.02(16) 3_666 . N1 C2 S1 127.62(15) . . N2 C2 S1 127.12(15) . . N2 C2 N1 105.25(17) . . N1 C3 C4 112.81(17) . . C5 C4 C3 111.91(18) . . C4 C5 C6 113.0(2) . . N2 C7 C8 112.71(17) . . C9 C8 C7 111.58(17) . . C8 C9 C10 111.94(18) . . N2 C11 P 121.00(14) 3_666 . C1 C11 P 132.42(15) 3_666 . C1 C11 N2 106.56(17) 3_666 3_666 C13 C12 S2 118.71(16) . . C17 C12 S2 121.07(16) . . C17 C12 C13 120.21(19) . . C14 C13 C12 119.9(2) . . C13 C14 C15 119.9(2) . . C16 C15 C14 120.3(2) . . C15 C16 C17 120.2(2) . . C12 C17 C16 119.52(19) . . C12' S2' P' 103.04(7) . . C1' P' S2' 100.98(7) . . C1' P' C7' 96.02(8) . . C7' P' S2' 100.42(7) . . C1' N1' C3' 125.56(16) . . C2' N1' C1' 110.44(15) . . C2' N1' C3' 123.46(16) . . C2' N2' C7' 110.53(16) 3_566 . C2' N2' C8' 122.89(16) 3_566 . C7' N2' C8' 126.51(16) . . N1' C1' P' 120.92(13) . . C7' C1' P' 132.27(14) 3_566 . C7' C1' N1' 106.74(16) 3_566 . N1' C2' S1' 127.86(15) . . N1' C2' N2' 105.17(16) . 3_566 N2' C2' S1' 126.96(15) 3_566 . N1' C3' C4' 110.88(16) . . C3' C4' C5' 112.91(17) . . C6' C5' C4' 111.25(18) . . N2' C7' P' 121.28(14) . . C1' C7' P' 131.55(15) 3_566 . C1' C7' N2' 107.08(16) 3_566 . N2' C8' C9' 112.71(17) . . C8' C9' C10' 110.55(18) . . C11' C10' C9' 112.7(2) . . C13' C12' S2' 119.15(16) . . C13' C12' C17' 119.86(19) . . C17' C12' S2' 120.93(16) . . C14' C13' C12' 119.7(2) . . C15' C14' C13' 120.2(2) . . C14' C15' C16' 120.3(2) . . C15' C16' C17' 120.0(2) . . C16' C17' C12' 120.0(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 S1 C2 1.685(2) . S2 P 2.1555(8) . S2 C12 1.781(2) . P C1 1.803(2) . P C11 1.799(2) . N1 C1 1.389(2) . N1 C2 1.371(2) . N1 C3 1.468(2) . N2 C2 1.364(3) . N2 C7 1.471(2) . N2 C11 1.395(2) 3_666 C1 C11 1.369(3) 3_666 C3 C4 1.523(3) . C4 C5 1.518(3) . C5 C6 1.520(3) . C7 C8 1.523(3) . C8 C9 1.521(3) . C9 C10 1.525(3) . C11 N2 1.395(2) 3_666 C11 C1 1.369(3) 3_666 C12 C13 1.397(3) . C12 C17 1.390(3) . C13 C14 1.387(3) . C14 C15 1.388(3) . C15 C16 1.388(3) . C16 C17 1.394(3) . S1' C2' 1.673(2) . S2' P' 2.1646(8) . S2' C12' 1.782(2) . P' C1' 1.800(2) . P' C7' 1.8071(19) . N1' C1' 1.396(2) . N1' C2' 1.367(2) . N1' C3' 1.468(2) . N2' C2' 1.372(2) 3_566 N2' C7' 1.388(2) . N2' C8' 1.467(2) . C1' C7' 1.365(3) 3_566 C2' N2' 1.372(2) 3_566 C3' C4' 1.525(3) . C4' C5' 1.528(3) . C5' C6' 1.525(3) . C7' C1' 1.365(3) 3_566 C8' C9' 1.515(3) . C9' C10' 1.523(3) . C10' C11' 1.514(4) . C12' C13' 1.395(3) . C12' C17' 1.396(3) . C13' C14' 1.395(3) . C14' C15' 1.384(3) . C15' C16' 1.387(3) . C16' C17' 1.392(3) .