#------------------------------------------------------------------------------ #$Date: 2019-11-17 06:37:57 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228452 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/13/7121308.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_7121308 loop_ _publ_author_name 'Terada, Misaki' 'Nishii, Yuji' 'Miura, Masahiro' _publ_section_title ; Synthesis, crystal structure and reactivity of \h2-thiophyne Ni complexes. ; _journal_issue 23 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 2918 _journal_page_last 2921 _journal_paper_doi 10.1039/c8cc00705e _journal_volume 54 _journal_year 2018 _chemical_formula_sum 'C30 H50 Ni P2 S' _chemical_formula_weight 563.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc1nb1mn _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-01-23 deposited with the CCDC. 2018-02-21 downloaded from the CCDC. ; _cell_angle_alpha 90.000(11) _cell_angle_beta 92.402(10) _cell_angle_gamma 90.000(8) _cell_formula_units_Z 4 _cell_length_a 9.9110(16) _cell_length_b 16.711(3) _cell_length_c 18.048(2) _cell_measurement_reflns_used 3005 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.40 _cell_measurement_theta_min 3.20 _cell_volume 2986.5(8) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 13.653 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku XtaLAB mini' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.2229 _diffrn_reflns_av_unetI/netI 0.1653 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 25694 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.997 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_min 3.190 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.838 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.096 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 335 _refine_ls_number_reflns 5244 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.1856 _refine_ls_R_factor_gt 0.0950 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+8.5137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1638 _refine_ls_wR_factor_ref 0.2047 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2728 _reflns_number_total 5244 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8cc00705e2.cif _cod_data_source_block shelxl _cod_depositor_comments ; The following automatic conversions were performed: data name '__diffrn_measurement_method' replaced with '_diffrn_measurement_method'. Automatic conversion script Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas Adding full bibliography for 7121308--7121314.cif. ; _cod_original_cell_volume 2986.6(8) _cod_database_code 7121308 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.936 _shelx_estimated_absorpt_t_max 0.951 _shelx_res_file ; TITL 83-01 shelxl.res created by SHELXL-2016/6 at 10:06:49 on 09-Nov-2016 CELL 0.71075 9.91100 16.71130 18.04810 90.000 92.402 90.000 ZERR 4 0.00162 0.00307 0.00210 0.0107 0.0103 0.0079 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H NI P S UNIT 120 200 4 8 4 DELU S5 C2 C32 DELU S28 C46 C30 SIMU S5 C2 C32 SIMU S28 C46 C30 OMIT -2 50 L.S. 30 FMAP 2 PLAN -25 WPDB -2 BOND $H CONF LIST 4 TEMP -100.0 ACTA SIZE 0.060 0.070 0.080 HTAB WGHT 0.047600 8.513700 FVAR 0.66098 0.41805 NI1 3 0.590213 0.391358 0.223413 11.00000 0.03584 0.03844 = 0.02857 -0.00292 -0.00164 0.00104 PART 1 S5 5 0.623568 0.248458 0.078828 21.00000 0.07489 0.03156 = 0.03712 -0.00556 -0.00026 0.00213 C2 1 0.800940 0.254786 0.091662 21.00000 0.07739 0.06110 = 0.09211 0.00227 0.00410 0.01820 AFIX 43 H2 2 0.859999 0.222099 0.064655 21.00000 -1.20000 AFIX 0 C32 1 0.849454 0.310936 0.144098 21.00000 0.07978 0.07206 = 0.12150 0.01331 -0.03136 -0.00958 AFIX 43 H32 2 0.940338 0.326490 0.154952 21.00000 -1.20000 AFIX 0 Part 2 S28 5 0.854953 0.286424 0.133923 -21.00000 0.04208 0.05646 = 0.05410 -0.00811 0.00779 0.00684 C46 1 0.744003 0.242190 0.073776 -21.00000 0.06076 0.03913 = 0.02613 -0.00288 -0.00060 0.01393 AFIX 43 H46 2 0.769434 0.202870 0.039000 -21.00000 -1.20000 AFIX 0 C30 1 0.607913 0.269207 0.079801 -21.00000 0.05704 0.01121 = 0.04646 0.01222 -0.01825 0.00479 AFIX 43 H30 2 0.532646 0.257326 0.047340 -21.00000 -1.20000 AFIX 0 Part 0 P3 4 0.382773 0.424248 0.230497 11.00000 0.03583 0.04536 = 0.02863 -0.00277 -0.00266 -0.00113 P25 4 0.649153 0.470557 0.313108 11.00000 0.03426 0.04074 = 0.02821 -0.00308 -0.00430 0.00254 C6 1 0.728974 0.339510 0.177661 11.00000 0.03296 0.04439 = 0.03403 -0.00262 -0.00115 0.00144 C7 1 0.737660 0.428225 0.395360 11.00000 0.02914 0.03900 = 0.03167 0.00093 0.00049 0.00435 AFIX 13 H7 2 0.828739 0.411586 0.379140 11.00000 -1.20000 AFIX 0 C8 1 0.981061 0.604484 0.248876 11.00000 0.03385 0.04463 = 0.04302 -0.01281 -0.00498 0.00159 AFIX 23 H8A 2 0.984210 0.647881 0.286248 11.00000 -1.20000 H8B 2 1.074800 0.586723 0.241375 11.00000 -1.20000 AFIX 0 C9 1 0.288932 0.458301 0.146052 11.00000 0.03411 0.03291 = 0.03837 -0.00288 -0.00456 0.00001 AFIX 13 H9 2 0.205782 0.486454 0.161722 11.00000 -1.20000 AFIX 0 C10 1 0.774106 0.662600 0.185309 11.00000 0.06256 0.04338 = 0.04595 0.00697 -0.01594 -0.00282 AFIX 23 H10A 2 0.734566 0.679713 0.136575 11.00000 -1.20000 H10B 2 0.772316 0.708917 0.219455 11.00000 -1.20000 AFIX 0 C11 1 0.750279 0.558037 0.287266 11.00000 0.03795 0.03973 = 0.02852 -0.00515 -0.00680 0.00861 AFIX 13 H11 2 0.746626 0.598819 0.327680 11.00000 -1.20000 AFIX 0 C12 1 0.690249 0.594602 0.215758 11.00000 0.03945 0.04788 = 0.03868 -0.00453 -0.00224 0.00502 AFIX 23 H12A 2 0.680764 0.552099 0.177685 11.00000 -1.20000 H12B 2 0.598708 0.614988 0.225055 11.00000 -1.20000 AFIX 0 C13 1 0.609145 0.319155 0.146722 11.00000 0.04348 0.02513 = 0.02870 0.00206 -0.00153 -0.00119 C14 1 0.899503 0.534991 0.277231 11.00000 0.03518 0.04447 = 0.04541 -0.00464 -0.01118 0.00393 AFIX 23 H14A 2 0.940072 0.516786 0.325381 11.00000 -1.20000 H14B 2 0.903441 0.489902 0.241808 11.00000 -1.20000 AFIX 0 C15 1 0.778067 0.370008 0.549825 11.00000 0.04629 0.06446 = 0.03378 -0.00029 -0.00694 0.00096 AFIX 23 H15A 2 0.837436 0.343855 0.588089 11.00000 -1.20000 H15B 2 0.691861 0.383494 0.572659 11.00000 -1.20000 AFIX 0 C16 1 0.750753 0.312407 0.486236 11.00000 0.05547 0.04780 = 0.05076 0.01100 -0.01193 0.00512 AFIX 23 H16A 2 0.700129 0.265675 0.504177 11.00000 -1.20000 H16B 2 0.837670 0.292877 0.468044 11.00000 -1.20000 AFIX 0 C17 1 0.493239 0.515233 0.350139 11.00000 0.04261 0.05619 = 0.03089 -0.00631 -0.00852 0.00573 AFIX 23 H17A 2 0.467015 0.485063 0.394496 11.00000 -1.20000 H17B 2 0.511152 0.571342 0.365152 11.00000 -1.20000 AFIX 0 C18 1 0.919604 0.635954 0.176632 11.00000 0.04756 0.03681 = 0.05121 0.00058 0.00149 -0.01108 AFIX 23 H18A 2 0.922069 0.593568 0.138390 11.00000 -1.20000 H18B 2 0.973614 0.681787 0.159717 11.00000 -1.20000 AFIX 0 C19 1 0.763435 0.486893 0.460742 11.00000 0.04421 0.05037 = 0.03884 -0.00204 -0.00857 -0.00132 AFIX 23 H19A 2 0.813485 0.534141 0.443429 11.00000 -1.20000 H19B 2 0.675980 0.505585 0.478903 11.00000 -1.20000 AFIX 0 C20 1 0.372128 0.518245 0.102327 11.00000 0.06481 0.03949 = 0.02894 0.00979 -0.00817 -0.00713 AFIX 23 H20A 2 0.398708 0.563751 0.134889 11.00000 -1.20000 H20B 2 0.455593 0.491877 0.086480 11.00000 -1.20000 AFIX 0 C21 1 0.245786 0.481557 -0.015625 11.00000 0.07452 0.05706 = 0.02779 0.00793 -0.01163 -0.01084 AFIX 23 H21A 2 0.325553 0.454847 -0.035741 11.00000 -1.20000 H21B 2 0.190125 0.503012 -0.057913 11.00000 -1.20000 AFIX 0 C22 1 0.164095 0.420862 0.025739 11.00000 0.06191 0.05475 = 0.03510 -0.00722 -0.01637 -0.00586 AFIX 23 H22A 2 0.140019 0.375535 -0.007572 11.00000 -1.20000 H22B 2 0.079307 0.445957 0.041248 11.00000 -1.20000 AFIX 0 C23 1 0.669641 0.352036 0.422429 11.00000 0.04334 0.04649 = 0.04036 -0.00495 -0.01011 0.00252 AFIX 23 H23A 2 0.578398 0.365427 0.439010 11.00000 -1.20000 H23B 2 0.659093 0.313764 0.380718 11.00000 -1.20000 AFIX 0 C24 1 0.244412 0.389629 0.094371 11.00000 0.04366 0.05063 = 0.03220 0.00439 -0.01151 -0.00427 AFIX 23 H24A 2 0.187754 0.351757 0.121577 11.00000 -1.20000 H24B 2 0.325040 0.360318 0.078467 11.00000 -1.20000 AFIX 0 C26 1 0.272618 0.344939 0.269719 11.00000 0.01954 0.13209 = 0.03686 0.03709 -0.00138 -0.00757 AFIX 13 H26 2 0.273728 0.298912 0.234341 11.00000 -1.20000 AFIX 0 C27 1 0.292037 0.549628 0.034003 11.00000 0.09124 0.03325 = 0.04591 0.00612 -0.01831 -0.01195 AFIX 23 H27A 2 0.212540 0.579996 0.049944 11.00000 -1.20000 H27B 2 0.349393 0.586467 0.006082 11.00000 -1.20000 AFIX 0 C29 1 0.376515 0.512811 0.290469 11.00000 0.03594 0.06382 = 0.03563 -0.00938 -0.01114 0.01105 AFIX 23 H29A 2 0.380533 0.561517 0.259414 11.00000 -1.20000 H29B 2 0.289333 0.513340 0.315307 11.00000 -1.20000 AFIX 0 C31 1 0.844804 0.446379 0.524112 11.00000 0.06217 0.05613 = 0.04132 -0.00149 -0.01320 -0.00782 AFIX 23 H31A 2 0.936246 0.433655 0.507429 11.00000 -1.20000 H31B 2 0.854832 0.483953 0.566392 11.00000 -1.20000 AFIX 0 C34 1 0.327264 0.314010 0.342120 11.00000 0.07221 0.09876 = 0.08438 0.01258 -0.01352 -0.00763 AFIX 23 H34A 2 0.324255 0.356993 0.379763 11.00000 -1.20000 H34B 2 0.422822 0.298297 0.337363 11.00000 -1.20000 AFIX 0 C38 1 0.127202 0.366893 0.276975 11.00000 0.06478 0.07394 = 0.07490 0.01245 0.00540 0.01408 AFIX 23 H38A 2 0.088268 0.385098 0.228451 11.00000 -1.20000 H38B 2 0.119801 0.411247 0.312940 11.00000 -1.20000 AFIX 0 C39 1 0.103844 0.262536 0.373747 11.00000 0.05809 0.14040 = 0.06325 0.03512 -0.00795 -0.00096 AFIX 23 H39A 2 0.051197 0.215831 0.389982 11.00000 -1.20000 H39B 2 0.096883 0.304919 0.411721 11.00000 -1.20000 AFIX 0 C40 1 0.244065 0.239472 0.368913 11.00000 0.07610 0.05227 = 0.10811 0.03485 -0.00149 -0.00057 AFIX 23 H40A 2 0.251825 0.194763 0.333355 11.00000 -1.20000 H40B 2 0.280321 0.221339 0.418031 11.00000 -1.20000 AFIX 0 C41 1 0.046401 0.291274 0.304511 11.00000 0.05600 0.11407 = 0.10647 0.03002 0.00864 -0.01846 AFIX 23 H41A 2 -0.049239 0.306045 0.310577 11.00000 -1.20000 H41B 2 0.049104 0.248296 0.266850 11.00000 -1.20000 AFIX 0 HKLF 4 REM 83-01 REM R1 = 0.0950 for 2728 Fo > 4sig(Fo) and 0.1856 for all 5244 data REM 335 parameters refined using 30 restraints END WGHT 0.0474 8.5407 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.838, deepest hole -0.453, 1-sigma level 0.096 Q1 1 0.3127 0.2745 0.2628 11.00000 0.05 0.84 Q2 1 0.1368 0.3425 0.3891 11.00000 0.05 0.75 Q3 1 0.2723 0.3843 0.3748 11.00000 0.05 0.55 Q4 1 0.2424 0.3914 0.3570 11.00000 0.05 0.54 Q5 1 0.1354 0.2301 0.2868 11.00000 0.05 0.48 Q6 1 0.2472 0.2070 0.3090 11.00000 0.05 0.44 Q7 1 0.2461 0.3659 0.2546 11.00000 0.05 0.38 Q8 1 0.7041 0.3986 0.2375 11.00000 0.05 0.35 Q9 1 0.3167 0.3642 0.2865 11.00000 0.05 0.34 Q10 1 0.0855 0.4765 0.0582 11.00000 0.05 0.33 Q11 1 0.5056 0.4195 0.2013 11.00000 0.05 0.32 Q12 1 0.6758 0.5433 0.2686 11.00000 0.05 0.32 Q13 1 0.6887 0.3762 0.2043 11.00000 0.05 0.31 Q14 1 0.4082 0.5363 0.3220 11.00000 0.05 0.31 Q15 1 0.7252 0.4584 0.4253 11.00000 0.05 0.30 Q16 1 0.9079 0.3782 0.0961 11.00000 0.05 0.30 Q17 1 0.1527 0.3561 0.1092 11.00000 0.05 0.30 Q18 1 0.5636 0.3913 0.4900 11.00000 0.05 0.29 Q19 1 0.4950 0.3563 0.1645 11.00000 0.05 0.29 Q20 1 1.0633 0.2997 0.0993 11.00000 0.05 0.29 Q21 1 0.7221 0.4607 0.3263 11.00000 0.05 0.29 Q22 1 0.3726 0.3455 0.2387 11.00000 0.05 0.29 Q23 1 0.6126 0.4397 0.2882 11.00000 0.05 0.29 Q24 1 0.9450 0.3022 0.4060 11.00000 0.05 0.29 Q25 1 0.5961 0.3846 0.1479 11.00000 0.05 0.28 ; _shelx_res_checksum 3895 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.59021(11) 0.39136(6) 0.22341(6) 0.0344(3) Uani 1 1 d . . . . . S5 S 0.624(2) 0.2485(12) 0.0788(12) 0.048(4) Uani 0.418(13) 1 d . U P A 1 C2 C 0.801(4) 0.255(3) 0.092(3) 0.077(10) Uani 0.418(13) 1 d . U P A 1 H2 H 0.859999 0.222099 0.064655 0.092 Uiso 0.418(13) 1 calc R U P A 1 C32 C 0.849(6) 0.311(3) 0.144(4) 0.092(17) Uani 0.418(13) 1 d . U P A 1 H32 H 0.940338 0.326490 0.154952 0.111 Uiso 0.418(13) 1 calc R U P A 1 S28 S 0.8550(9) 0.2864(5) 0.1339(5) 0.051(2) Uani 0.582(13) 1 d . U P A 2 C46 C 0.744(3) 0.2422(14) 0.0738(11) 0.042(5) Uani 0.582(13) 1 d . U P A 2 H46 H 0.769434 0.202870 0.039000 0.050 Uiso 0.582(13) 1 calc R U P A 2 C30 C 0.608(6) 0.269(2) 0.080(3) 0.039(10) Uani 0.582(13) 1 d . U P A 2 H30 H 0.532646 0.257326 0.047340 0.047 Uiso 0.582(13) 1 calc R U P A 2 P3 P 0.3828(2) 0.42425(14) 0.23050(12) 0.0367(6) Uani 1 1 d . . . . . P25 P 0.6492(2) 0.47056(13) 0.31311(11) 0.0346(6) Uani 1 1 d . . . . . C6 C 0.7290(9) 0.3395(5) 0.1777(4) 0.037(2) Uani 1 1 d . . . . . C7 C 0.7377(8) 0.4282(5) 0.3954(4) 0.0333(19) Uani 1 1 d . . . . . H7 H 0.828739 0.411586 0.379140 0.040 Uiso 1 1 calc R U . . . C8 C 0.9811(8) 0.6045(5) 0.2489(4) 0.041(2) Uani 1 1 d . . . . . H8A H 0.984210 0.647881 0.286248 0.049 Uiso 1 1 calc R U . . . H8B H 1.074800 0.586723 0.241375 0.049 Uiso 1 1 calc R U . . . C9 C 0.2889(8) 0.4583(5) 0.1461(4) 0.035(2) Uani 1 1 d . . . . . H9 H 0.205782 0.486454 0.161722 0.042 Uiso 1 1 calc R U . . . C10 C 0.7741(9) 0.6626(5) 0.1853(5) 0.051(3) Uani 1 1 d . . . . . H10A H 0.734566 0.679713 0.136575 0.061 Uiso 1 1 calc R U . . . H10B H 0.772316 0.708917 0.219455 0.061 Uiso 1 1 calc R U . . . C11 C 0.7503(8) 0.5580(5) 0.2873(4) 0.036(2) Uani 1 1 d . . . . . H11 H 0.746626 0.598819 0.327680 0.043 Uiso 1 1 calc R U . . . C12 C 0.6902(8) 0.5946(5) 0.2158(4) 0.042(2) Uani 1 1 d . . . . . H12A H 0.680764 0.552099 0.177685 0.051 Uiso 1 1 calc R U . . . H12B H 0.598708 0.614988 0.225055 0.051 Uiso 1 1 calc R U . . . C13 C 0.6091(8) 0.3192(5) 0.1467(4) 0.0325(19) Uani 1 1 d . . . . . C14 C 0.8995(8) 0.5350(5) 0.2772(5) 0.042(2) Uani 1 1 d . . . . . H14A H 0.940072 0.516786 0.325381 0.050 Uiso 1 1 calc R U . . . H14B H 0.903441 0.489902 0.241808 0.050 Uiso 1 1 calc R U . . . C15 C 0.7781(9) 0.3700(5) 0.5498(4) 0.048(2) Uani 1 1 d . . . . . H15A H 0.837436 0.343855 0.588089 0.058 Uiso 1 1 calc R U . . . H15B H 0.691861 0.383494 0.572659 0.058 Uiso 1 1 calc R U . . . C16 C 0.7508(9) 0.3124(5) 0.4862(5) 0.052(3) Uani 1 1 d . . . . . H16A H 0.700129 0.265675 0.504177 0.062 Uiso 1 1 calc R U . . . H16B H 0.837670 0.292877 0.468044 0.062 Uiso 1 1 calc R U . . . C17 C 0.4932(8) 0.5152(5) 0.3501(4) 0.044(2) Uani 1 1 d . . . . . H17A H 0.467015 0.485063 0.394496 0.052 Uiso 1 1 calc R U . . . H17B H 0.511152 0.571342 0.365152 0.052 Uiso 1 1 calc R U . . . C18 C 0.9196(9) 0.6360(5) 0.1766(5) 0.045(2) Uani 1 1 d . . . . . H18A H 0.922069 0.593568 0.138390 0.054 Uiso 1 1 calc R U . . . H18B H 0.973614 0.681787 0.159717 0.054 Uiso 1 1 calc R U . . . C19 C 0.7634(9) 0.4869(5) 0.4607(4) 0.045(2) Uani 1 1 d . . . . . H19A H 0.813485 0.534141 0.443429 0.054 Uiso 1 1 calc R U . . . H19B H 0.675980 0.505585 0.478903 0.054 Uiso 1 1 calc R U . . . C20 C 0.3721(9) 0.5182(5) 0.1023(4) 0.045(2) Uani 1 1 d . . . . . H20A H 0.398708 0.563751 0.134889 0.054 Uiso 1 1 calc R U . . . H20B H 0.455593 0.491877 0.086480 0.054 Uiso 1 1 calc R U . . . C21 C 0.2458(10) 0.4816(6) -0.0156(5) 0.054(3) Uani 1 1 d . . . . . H21A H 0.325553 0.454847 -0.035741 0.064 Uiso 1 1 calc R U . . . H21B H 0.190125 0.503012 -0.057913 0.064 Uiso 1 1 calc R U . . . C22 C 0.1641(9) 0.4209(5) 0.0257(5) 0.051(3) Uani 1 1 d . . . . . H22A H 0.140019 0.375535 -0.007572 0.061 Uiso 1 1 calc R U . . . H22B H 0.079307 0.445957 0.041248 0.061 Uiso 1 1 calc R U . . . C23 C 0.6696(8) 0.3520(5) 0.4224(5) 0.044(2) Uani 1 1 d . . . . . H23A H 0.578398 0.365427 0.439010 0.052 Uiso 1 1 calc R U . . . H23B H 0.659093 0.313764 0.380718 0.052 Uiso 1 1 calc R U . . . C24 C 0.2444(8) 0.3896(5) 0.0944(4) 0.043(2) Uani 1 1 d . . . . . H24A H 0.187754 0.351757 0.121577 0.051 Uiso 1 1 calc R U . . . H24B H 0.325040 0.360318 0.078467 0.051 Uiso 1 1 calc R U . . . C26 C 0.2726(8) 0.3449(7) 0.2697(5) 0.063(3) Uani 1 1 d . . . . . H26 H 0.273728 0.298912 0.234341 0.075 Uiso 1 1 calc R U . . . C27 C 0.2920(10) 0.5496(5) 0.0340(5) 0.057(3) Uani 1 1 d . . . . . H27A H 0.212540 0.579996 0.049944 0.069 Uiso 1 1 calc R U . . . H27B H 0.349393 0.586467 0.006082 0.069 Uiso 1 1 calc R U . . . C29 C 0.3765(8) 0.5128(5) 0.2905(4) 0.045(2) Uani 1 1 d . . . . . H29A H 0.380533 0.561517 0.259414 0.055 Uiso 1 1 calc R U . . . H29B H 0.289333 0.513340 0.315307 0.055 Uiso 1 1 calc R U . . . C31 C 0.8448(10) 0.4464(5) 0.5241(5) 0.054(3) Uani 1 1 d . . . . . H31A H 0.936246 0.433655 0.507429 0.064 Uiso 1 1 calc R U . . . H31B H 0.854832 0.483953 0.566392 0.064 Uiso 1 1 calc R U . . . C34 C 0.3273(11) 0.3140(7) 0.3421(6) 0.086(4) Uani 1 1 d . . . . . H34A H 0.324255 0.356993 0.379763 0.103 Uiso 1 1 calc R U . . . H34B H 0.422822 0.298297 0.337363 0.103 Uiso 1 1 calc R U . . . C38 C 0.1272(10) 0.3669(6) 0.2770(6) 0.071(3) Uani 1 1 d . . . . . H38A H 0.088268 0.385098 0.228451 0.085 Uiso 1 1 calc R U . . . H38B H 0.119801 0.411247 0.312940 0.085 Uiso 1 1 calc R U . . . C39 C 0.1038(11) 0.2625(8) 0.3737(6) 0.088(4) Uani 1 1 d . . . . . H39A H 0.051197 0.215831 0.389982 0.105 Uiso 1 1 calc R U . . . H39B H 0.096883 0.304919 0.411721 0.105 Uiso 1 1 calc R U . . . C40 C 0.2441(11) 0.2395(6) 0.3689(7) 0.079(4) Uani 1 1 d . . . . . H40A H 0.251825 0.194763 0.333355 0.095 Uiso 1 1 calc R U . . . H40B H 0.280321 0.221339 0.418031 0.095 Uiso 1 1 calc R U . . . C41 C 0.0464(11) 0.2913(8) 0.3045(7) 0.092(4) Uani 1 1 d . . . . . H41A H -0.049239 0.306045 0.310577 0.110 Uiso 1 1 calc R U . . . H41B H 0.049104 0.248296 0.266850 0.110 Uiso 1 1 calc R U . . . 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 Ni1 0.0358(6) 0.0384(6) 0.0286(6) -0.0029(5) -0.0016(4) 0.0010(6) S5 0.075(9) 0.032(9) 0.037(5) -0.006(6) 0.000(5) 0.002(6) C2 0.077(13) 0.06(2) 0.09(2) 0.002(18) 0.004(19) 0.018(18) C32 0.08(3) 0.07(3) 0.12(3) 0.01(2) -0.03(2) -0.01(2) S28 0.042(3) 0.056(5) 0.054(4) -0.008(3) 0.008(3) 0.007(3) C46 0.061(14) 0.039(11) 0.026(9) -0.003(7) -0.001(8) 0.014(10) C30 0.057(12) 0.011(19) 0.046(17) 0.012(14) -0.018(11) 0.005(12) P3 0.0358(13) 0.0454(14) 0.0286(12) -0.0028(10) -0.0027(10) -0.0011(11) P25 0.0343(13) 0.0407(14) 0.0282(12) -0.0031(10) -0.0043(9) 0.0025(11) C6 0.033(5) 0.044(6) 0.034(5) -0.003(4) -0.001(4) 0.001(4) C7 0.029(5) 0.039(5) 0.032(5) 0.001(4) 0.000(4) 0.004(4) C8 0.034(5) 0.045(5) 0.043(5) -0.013(5) -0.005(4) 0.002(4) C9 0.034(5) 0.033(5) 0.038(5) -0.003(4) -0.005(4) 0.000(4) C10 0.063(7) 0.043(6) 0.046(6) 0.007(5) -0.016(5) -0.003(5) C11 0.038(5) 0.040(5) 0.029(4) -0.005(4) -0.007(4) 0.009(4) C12 0.039(5) 0.048(6) 0.039(5) -0.005(4) -0.002(4) 0.005(4) C13 0.043(5) 0.025(4) 0.029(4) 0.002(4) -0.002(4) -0.001(4) C14 0.035(5) 0.044(5) 0.045(5) -0.005(5) -0.011(4) 0.004(5) C15 0.046(6) 0.064(7) 0.034(5) 0.000(5) -0.007(4) 0.001(5) C16 0.055(6) 0.048(6) 0.051(6) 0.011(5) -0.012(5) 0.005(5) C17 0.043(5) 0.056(6) 0.031(5) -0.006(4) -0.009(4) 0.006(5) C18 0.048(6) 0.037(5) 0.051(6) 0.001(4) 0.001(5) -0.011(4) C19 0.044(6) 0.050(6) 0.039(5) -0.002(4) -0.009(4) -0.001(5) C20 0.065(6) 0.039(5) 0.029(5) 0.010(4) -0.008(4) -0.007(5) C21 0.075(7) 0.057(6) 0.028(5) 0.008(4) -0.012(5) -0.011(5) C22 0.062(7) 0.055(6) 0.035(5) -0.007(5) -0.016(5) -0.006(5) C23 0.043(5) 0.046(6) 0.040(5) -0.005(4) -0.010(4) 0.003(5) C24 0.044(5) 0.051(6) 0.032(5) 0.004(4) -0.012(4) -0.004(5) C26 0.020(5) 0.132(10) 0.037(5) 0.037(6) -0.001(4) -0.008(5) C27 0.091(8) 0.033(5) 0.046(6) 0.006(4) -0.018(5) -0.012(5) C29 0.036(5) 0.064(6) 0.036(5) -0.009(4) -0.011(4) 0.011(5) C31 0.062(7) 0.056(6) 0.041(6) -0.001(5) -0.013(5) -0.008(5) C34 0.072(8) 0.099(10) 0.084(9) 0.013(7) -0.014(7) -0.008(7) C38 0.065(8) 0.074(8) 0.075(8) 0.012(6) 0.005(6) 0.014(6) C39 0.058(8) 0.140(12) 0.063(8) 0.035(8) -0.008(6) -0.001(8) C40 0.076(8) 0.052(7) 0.108(10) 0.035(7) -0.001(7) -0.001(6) C41 0.056(8) 0.114(11) 0.106(10) 0.030(9) 0.009(7) -0.018(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 C6 Ni1 C13 42.3(3) C6 Ni1 P3 152.0(3) C13 Ni1 P3 109.9(3) C6 Ni1 P25 116.1(3) C13 Ni1 P25 158.4(3) P3 Ni1 P25 91.62(9) C13 S5 C2 89(2) C32 C2 S5 116(4) C32 C2 H2 122.0 S5 C2 H2 122.0 C2 C32 C6 104(5) C2 C32 H32 128.1 C6 C32 H32 128.1 C46 S28 C6 93.1(11) C30 C46 S28 114(3) C30 C46 H46 123.1 S28 C46 H46 123.1 C46 C30 C13 105(4) C46 C30 H30 127.3 C13 C30 H30 127.3 C29 P3 C9 102.1(4) C29 P3 C26 108.2(5) C9 P3 C26 104.4(4) C29 P3 Ni1 107.4(3) C9 P3 Ni1 118.9(3) C26 P3 Ni1 114.7(3) C7 P25 C11 105.3(4) C7 P25 C17 103.9(4) C11 P25 C17 103.9(4) C7 P25 Ni1 118.5(3) C11 P25 Ni1 115.5(3) C17 P25 Ni1 108.2(3) C13 C6 C32 119(3) C13 C6 S28 108.8(7) C13 C6 Ni1 69.0(5) C32 C6 Ni1 171(3) S28 C6 Ni1 177.2(6) C23 C7 C19 110.2(6) C23 C7 P25 112.2(5) C19 C7 P25 115.5(6) C23 C7 H7 106.1 C19 C7 H7 106.1 P25 C7 H7 106.1 C18 C8 C14 110.9(7) C18 C8 H8A 109.5 C14 C8 H8A 109.5 C18 C8 H8B 109.5 C14 C8 H8B 109.5 H8A C8 H8B 108.0 C24 C9 C20 108.8(7) C24 C9 P3 113.3(5) C20 C9 P3 111.3(5) C24 C9 H9 107.8 C20 C9 H9 107.8 P3 C9 H9 107.8 C18 C10 C12 110.6(7) C18 C10 H10A 109.5 C12 C10 H10A 109.5 C18 C10 H10B 109.5 C12 C10 H10B 109.5 H10A C10 H10B 108.1 C12 C11 C14 110.0(7) C12 C11 P25 109.6(5) C14 C11 P25 111.4(5) C12 C11 H11 108.6 C14 C11 H11 108.6 P25 C11 H11 108.6 C10 C12 C11 113.9(7) C10 C12 H12A 108.8 C11 C12 H12A 108.8 C10 C12 H12B 108.8 C11 C12 H12B 108.8 H12A C12 H12B 107.7 C6 C13 C30 118(2) C6 C13 S5 112.1(10) C6 C13 Ni1 68.8(5) C30 C13 Ni1 171(2) S5 C13 Ni1 176.9(9) C8 C14 C11 112.0(7) C8 C14 H14A 109.2 C11 C14 H14A 109.2 C8 C14 H14B 109.2 C11 C14 H14B 109.2 H14A C14 H14B 107.9 C16 C15 C31 111.7(7) C16 C15 H15A 109.3 C31 C15 H15A 109.3 C16 C15 H15B 109.3 C31 C15 H15B 109.3 H15A C15 H15B 108.0 C15 C16 C23 111.6(7) C15 C16 H16A 109.3 C23 C16 H16A 109.3 C15 C16 H16B 109.3 C23 C16 H16B 109.3 H16A C16 H16B 108.0 C29 C17 P25 110.3(5) C29 C17 H17A 109.6 P25 C17 H17A 109.6 C29 C17 H17B 109.6 P25 C17 H17B 109.6 H17A C17 H17B 108.1 C8 C18 C10 111.2(7) C8 C18 H18A 109.4 C10 C18 H18A 109.4 C8 C18 H18B 109.4 C10 C18 H18B 109.4 H18A C18 H18B 108.0 C31 C19 C7 110.8(7) C31 C19 H19A 109.5 C7 C19 H19A 109.5 C31 C19 H19B 109.5 C7 C19 H19B 109.5 H19A C19 H19B 108.1 C27 C20 C9 111.5(7) C27 C20 H20A 109.3 C9 C20 H20A 109.3 C27 C20 H20B 109.3 C9 C20 H20B 109.3 H20A C20 H20B 108.0 C27 C21 C22 111.6(7) C27 C21 H21A 109.3 C22 C21 H21A 109.3 C27 C21 H21B 109.3 C22 C21 H21B 109.3 H21A C21 H21B 108.0 C21 C22 C24 110.8(7) C21 C22 H22A 109.5 C24 C22 H22A 109.5 C21 C22 H22B 109.5 C24 C22 H22B 109.5 H22A C22 H22B 108.1 C16 C23 C7 112.1(7) C16 C23 H23A 109.2 C7 C23 H23A 109.2 C16 C23 H23B 109.2 C7 C23 H23B 109.2 H23A C23 H23B 107.9 C9 C24 C22 111.3(7) C9 C24 H24A 109.4 C22 C24 H24A 109.4 C9 C24 H24B 109.4 C22 C24 H24B 109.4 H24A C24 H24B 108.0 C34 C26 C38 109.0(8) C34 C26 P3 112.4(7) C38 C26 P3 115.9(8) C34 C26 H26 106.3 C38 C26 H26 106.3 P3 C26 H26 106.3 C21 C27 C20 110.8(7) C21 C27 H27A 109.5 C20 C27 H27A 109.5 C21 C27 H27B 109.5 C20 C27 H27B 109.5 H27A C27 H27B 108.1 C17 C29 P3 112.9(6) C17 C29 H29A 109.0 P3 C29 H29A 109.0 C17 C29 H29B 109.0 P3 C29 H29B 109.0 H29A C29 H29B 107.8 C15 C31 C19 112.2(7) C15 C31 H31A 109.2 C19 C31 H31A 109.2 C15 C31 H31B 109.2 C19 C31 H31B 109.2 H31A C31 H31B 107.9 C26 C34 C40 111.6(9) C26 C34 H34A 109.3 C40 C34 H34A 109.3 C26 C34 H34B 109.3 C40 C34 H34B 109.3 H34A C34 H34B 108.0 C26 C38 C41 109.4(9) C26 C38 H38A 109.8 C41 C38 H38A 109.8 C26 C38 H38B 109.8 C41 C38 H38B 109.8 H38A C38 H38B 108.2 C41 C39 C40 112.6(10) C41 C39 H39A 109.1 C40 C39 H39A 109.1 C41 C39 H39B 109.1 C40 C39 H39B 109.1 H39A C39 H39B 107.8 C39 C40 C34 108.8(9) C39 C40 H40A 109.9 C34 C40 H40A 109.9 C39 C40 H40B 109.9 C34 C40 H40B 109.9 H40A C40 H40B 108.3 C39 C41 C38 110.6(10) C39 C41 H41A 109.5 C38 C41 H41A 109.5 C39 C41 H41B 109.5 C38 C41 H41B 109.5 H41A C41 H41B 108.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 C6 1.849(9) Ni1 C13 1.852(8) Ni1 P3 2.137(3) Ni1 P25 2.153(2) S5 C13 1.71(2) S5 C2 1.77(4) C2 C32 1.40(7) C2 H2 0.9500 C32 C6 1.44(6) C32 H32 0.9500 S28 C46 1.68(2) S28 C6 1.747(11) C46 C30 1.43(5) C46 H46 0.9500 C30 C13 1.47(5) C30 H30 0.9500 P3 C29 1.836(8) P3 C9 1.842(8) P3 C26 1.875(9) P25 C7 1.834(8) P25 C11 1.843(8) P25 C17 1.865(8) C6 C13 1.335(10) C7 C23 1.530(11) C7 C19 1.547(11) C7 H7 1.0000 C8 C18 1.510(11) C8 C14 1.516(11) C8 H8A 0.9900 C8 H8B 0.9900 C9 C24 1.532(10) C9 C20 1.536(11) C9 H9 1.0000 C10 C18 1.524(11) C10 C12 1.524(11) C10 H10A 0.9900 C10 H10B 0.9900 C11 C12 1.526(10) C11 C14 1.546(10) C11 H11 1.0000 C12 H12A 0.9900 C12 H12B 0.9900 C14 H14A 0.9900 C14 H14B 0.9900 C15 C16 1.514(11) C15 C31 1.519(12) C15 H15A 0.9900 C15 H15B 0.9900 C16 C23 1.528(10) C16 H16A 0.9900 C16 H16B 0.9900 C17 C29 1.548(10) C17 H17A 0.9900 C17 H17B 0.9900 C18 H18A 0.9900 C18 H18B 0.9900 C19 C31 1.530(11) C19 H19A 0.9900 C19 H19B 0.9900 C20 C27 1.531(11) C20 H20A 0.9900 C20 H20B 0.9900 C21 C27 1.507(11) C21 C22 1.514(12) C21 H21A 0.9900 C21 H21B 0.9900 C22 C24 1.535(10) C22 H22A 0.9900 C22 H22B 0.9900 C23 H23A 0.9900 C23 H23B 0.9900 C24 H24A 0.9900 C24 H24B 0.9900 C26 C34 1.486(12) C26 C38 1.498(12) C26 H26 1.0000 C27 H27A 0.9900 C27 H27B 0.9900 C29 H29A 0.9900 C29 H29B 0.9900 C31 H31A 0.9900 C31 H31B 0.9900 C34 C40 1.581(14) C34 H34A 0.9900 C34 H34B 0.9900 C38 C41 1.587(14) C38 H38A 0.9900 C38 H38B 0.9900 C39 C41 1.434(13) C39 C40 1.448(13) C39 H39A 0.9900 C39 H39B 0.9900 C40 H40A 0.9900 C40 H40B 0.9900 C41 H41A 0.9900 C41 H41B 0.9900 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 C13 S5 C2 C32 -2(4) S5 C2 C32 C6 7(5) C6 S28 C46 C30 4(3) S28 C46 C30 C13 -9(4) C2 C32 C6 C13 -10(5) C46 S28 C6 C13 2.3(11) P3 Ni1 C6 C13 -8.7(9) P25 Ni1 C6 C13 -179.9(4) C11 P25 C7 C23 -177.5(6) C17 P25 C7 C23 73.6(6) Ni1 P25 C7 C23 -46.5(6) C11 P25 C7 C19 55.1(7) C17 P25 C7 C19 -53.8(7) Ni1 P25 C7 C19 -173.8(5) C29 P3 C9 C24 -164.1(6) C26 P3 C9 C24 -51.4(7) Ni1 P3 C9 C24 78.0(6) C29 P3 C9 C20 73.0(7) C26 P3 C9 C20 -174.4(6) Ni1 P3 C9 C20 -45.0(7) C7 P25 C11 C12 176.1(5) C17 P25 C11 C12 -75.0(6) Ni1 P25 C11 C12 43.4(6) C7 P25 C11 C14 54.2(6) C17 P25 C11 C14 163.1(5) Ni1 P25 C11 C14 -78.5(6) C18 C10 C12 C11 53.5(10) C14 C11 C12 C10 -51.6(9) P25 C11 C12 C10 -174.4(6) S28 C6 C13 C30 -8(2) Ni1 C6 C13 C30 173(2) C32 C6 C13 S5 9(3) Ni1 C6 C13 S5 -176.8(9) C32 C6 C13 Ni1 -174(3) S28 C6 C13 Ni1 178.3(6) C46 C30 C13 C6 11(4) C2 S5 C13 C6 -3.9(18) P3 Ni1 C13 C6 175.6(4) P25 Ni1 C13 C6 0.3(9) C18 C8 C14 C11 -56.9(9) C12 C11 C14 C8 52.9(9) P25 C11 C14 C8 174.6(5) C31 C15 C16 C23 -54.0(10) C7 P25 C17 C29 -149.9(6) C11 P25 C17 C29 100.1(7) Ni1 P25 C17 C29 -23.2(7) C14 C8 C18 C10 58.1(9) C12 C10 C18 C8 -55.7(9) C23 C7 C19 C31 55.0(9) P25 C7 C19 C31 -176.7(6) C24 C9 C20 C27 57.1(9) P3 C9 C20 C27 -177.4(6) C27 C21 C22 C24 -55.8(11) C15 C16 C23 C7 55.1(10) C19 C7 C23 C16 -55.3(9) P25 C7 C23 C16 174.5(6) C20 C9 C24 C22 -56.9(9) P3 C9 C24 C22 178.8(6) C21 C22 C24 C9 56.8(10) C29 P3 C26 C34 -67.4(9) C9 P3 C26 C34 -175.7(8) Ni1 P3 C26 C34 52.4(9) C29 P3 C26 C38 58.8(8) C9 P3 C26 C38 -49.4(9) Ni1 P3 C26 C38 178.7(6) C22 C21 C27 C20 55.9(11) C9 C20 C27 C21 -57.1(11) P25 C17 C29 P3 33.9(8) C9 P3 C29 C17 -156.0(6) C26 P3 C29 C17 94.2(7) Ni1 P3 C29 C17 -30.1(7) C16 C15 C31 C19 54.7(10) C7 C19 C31 C15 -55.2(10) C38 C26 C34 C40 57.8(13) P3 C26 C34 C40 -172.3(8) C34 C26 C38 C41 -56.7(13) P3 C26 C38 C41 175.3(7) C41 C39 C40 C34 58.2(15) C26 C34 C40 C39 -57.5(14) C40 C39 C41 C38 -59.4(15) C26 C38 C41 C39 57.7(13)