#------------------------------------------------------------------------------ #$Date: 2019-06-01 03:26:27 +0300 (Sat, 01 Jun 2019) $ #$Revision: 215644 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/11/1551192.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_1551192 loop_ _publ_author_name 'Fataftah, Majed S.' 'Krzyaniak, Matthew D.' 'Vlaisavljevich, Bess' 'Wasielewski, Michael R.' 'Zadrozny, Joseph' 'Freedman, Danna' _publ_section_title ; Metal-Ligand Covalency Enables Room Temperature Molecular Qubit Candidates ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00074G _journal_year 2019 _chemical_formula_moiety 'C12 H8 Ni S4, 2(C24 H20 P)' _chemical_formula_sum 'C60 H48 Ni P2 S4' _chemical_formula_weight 1017.87 _chemical_name_systematic 'tetraphenyl phosphonium nickel bis(dithiocatecholate)' _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 _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc210dcv _audit_creation_date 2018-03-06 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-11-05 deposited with the CCDC. 2019-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.168(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.1212(6) _cell_length_b 14.6404(8) _cell_length_c 14.8691(8) _cell_measurement_reflns_used 9898 _cell_measurement_temperature 100 _cell_measurement_theta_max 30.37 _cell_measurement_theta_min 2.39 _cell_volume 2411.1(2) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 99.95 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 78942 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.841 _diffrn_reflns_theta_min 1.956 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0943 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.9410. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'dull dark red' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.402 _exptl_crystal_description plate _exptl_crystal_F_000 1060 _exptl_crystal_preparation 'Made in DMF with NBu4OH, CuCl2, dithiocatechol, and Ph4PBr,' _exptl_crystal_recrystallization_method 'Crystallized by layering a solution of DMF under Et2O at -35' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.409 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef 0.0005(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 305 _refine_ls_number_reflns 7503 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0346 _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^)+(0.0233P)^2^+1.6804P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0764 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5850 _reflns_number_total 7503 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00074g2.cif _cod_data_source_block msf6_39_0m _cod_database_code 1551192 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C005(H005), C006(H006), C008(H008), C00A(H00A), C00C(H00C), C00F(H00F), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y) ; _shelx_res_file ; TITL msf6_39_0m_a.res in P2(1)/n msf6_39_0m.res created by SHELXL-2016/6 at 08:05:54 on 06-Mar-2018 REM Old TITL MSF6_39_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.081, Rweak 0.005, Alpha 0.020, Orientation as input REM Formula found by SHELXT: C60 P2 S4 Ni CELL 0.71073 11.1212 14.6404 14.8691 90 95.168 90 ZERR 2 0.0006 0.0008 0.0008 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ni P S UNIT 120 96 2 4 8 L.S. 4 PLAN 20 TEMP -173.2 BOND $H list 4 fmap 2 acta OMIT 0 6 0 OMIT 0 6 6 OMIT 6 6 3 REM REM REM WGHT 0.023300 1.680400 EXTI 0.000480 FVAR 0.41955 NI01 3 0.500000 1.000000 0.500000 10.50000 0.01608 0.00954 = 0.01313 -0.00196 0.00028 0.00015 S002 5 0.615568 0.981905 0.389642 11.00000 0.01803 0.01318 = 0.01722 -0.00330 0.00194 -0.00117 P003 4 0.478500 0.534817 0.296307 11.00000 0.01312 0.00952 = 0.01432 -0.00099 0.00060 0.00026 S004 5 0.366728 0.906129 0.435560 11.00000 0.01818 0.01609 = 0.01736 -0.00519 0.00243 -0.00267 C005 1 0.600213 0.592715 0.153345 11.00000 0.02178 0.01400 = 0.01598 0.00000 0.00301 0.00147 AFIX 43 H005 2 0.669803 0.591350 0.195357 11.00000 -1.20000 AFIX 0 C006 1 0.615914 0.681756 0.356491 11.00000 0.01501 0.01352 = 0.01610 0.00098 0.00105 0.00162 AFIX 43 H006 2 0.557561 0.716760 0.320862 11.00000 -1.20000 AFIX 0 C007 1 0.533029 0.910872 0.311625 11.00000 0.01977 0.01048 = 0.01398 -0.00010 -0.00159 0.00299 C008 1 0.798527 0.672692 0.455448 11.00000 0.01427 0.02393 = 0.01334 -0.00218 0.00157 -0.00272 AFIX 43 H008 2 0.864704 0.702143 0.488388 11.00000 -1.20000 AFIX 0 C009 1 0.341789 0.573853 0.339919 11.00000 0.01449 0.00997 = 0.01939 0.00021 0.00341 0.00131 C00A 1 0.691937 0.534589 0.410755 11.00000 0.01712 0.01426 = 0.01656 0.00190 0.00115 0.00192 AFIX 43 H00A 2 0.684670 0.469993 0.412992 11.00000 -1.20000 AFIX 0 C00B 1 0.487443 0.568209 0.180750 11.00000 0.01975 0.00975 = 0.01564 -0.00130 -0.00010 0.00244 C00C 1 0.712000 0.724697 0.405154 11.00000 0.01736 0.01389 = 0.01715 -0.00122 0.00271 -0.00272 AFIX 43 H00C 2 0.718736 0.789369 0.404165 11.00000 -1.20000 AFIX 0 C00D 1 0.491212 0.413274 0.307868 11.00000 0.01725 0.01133 = 0.01498 -0.00149 0.00048 0.00013 C00E 1 0.420996 0.876473 0.332686 11.00000 0.01932 0.01004 = 0.01464 -0.00024 -0.00153 0.00374 C00F 1 0.429527 0.366574 0.371517 11.00000 0.02044 0.01516 = 0.01926 -0.00192 0.00506 -0.00014 AFIX 43 H00F 2 0.372953 0.397871 0.404536 11.00000 -1.20000 AFIX 0 C00G 1 0.573407 0.366753 0.258884 11.00000 0.02536 0.01517 = 0.01858 0.00048 0.00655 0.00227 AFIX 43 H00G 2 0.614600 0.398095 0.214882 11.00000 -1.20000 AFIX 0 C00H 1 0.346279 0.636208 0.411194 11.00000 0.01716 0.01461 = 0.01805 -0.00069 0.00305 -0.00073 AFIX 43 H00H 2 0.421997 0.656759 0.438463 11.00000 -1.20000 AFIX 0 C00I 1 0.605235 0.586530 0.360082 11.00000 0.01311 0.01405 = 0.01204 -0.00137 0.00167 -0.00045 C00J 1 0.354043 0.820796 0.270126 11.00000 0.02061 0.01112 = 0.01847 0.00016 -0.00387 0.00197 AFIX 43 H00J 2 0.278226 0.797383 0.284022 11.00000 -1.20000 AFIX 0 C00K 1 0.575804 0.888543 0.228766 11.00000 0.02469 0.01522 = 0.01718 0.00108 0.00302 0.00252 AFIX 43 H00K 2 0.651673 0.911436 0.214382 11.00000 -1.20000 AFIX 0 C00L 1 0.397341 0.799437 0.187938 11.00000 0.03014 0.01369 = 0.01577 -0.00224 -0.00580 0.00393 AFIX 43 H00L 2 0.351043 0.761766 0.145872 11.00000 -1.20000 AFIX 0 C00M 1 0.239978 0.668117 0.442141 11.00000 0.02401 0.01506 = 0.02481 -0.00250 0.00831 0.00054 AFIX 43 H00M 2 0.242888 0.710019 0.491072 11.00000 -1.20000 AFIX 0 C00N 1 0.385805 0.568221 0.118193 11.00000 0.02244 0.01328 = 0.02190 -0.00215 -0.00586 0.00284 AFIX 43 H00N 2 0.309354 0.550336 0.136040 11.00000 -1.20000 AFIX 0 C00O 1 0.451356 0.274052 0.386291 11.00000 0.02955 0.01457 = 0.02098 0.00182 0.00379 -0.00275 AFIX 43 H00O 2 0.409199 0.242050 0.429310 11.00000 -1.20000 AFIX 0 C00P 1 0.789148 0.578280 0.457984 11.00000 0.01619 0.02210 = 0.01592 0.00268 -0.00028 0.00363 AFIX 43 H00P 2 0.849220 0.543400 0.492034 11.00000 -1.20000 AFIX 0 C00Q 1 0.397552 0.594528 0.030005 11.00000 0.04007 0.01400 = 0.01932 -0.00373 -0.01026 0.00698 AFIX 43 H00Q 2 0.328800 0.594571 -0.012828 11.00000 -1.20000 AFIX 0 C00R 1 0.508295 0.833125 0.167217 11.00000 0.03320 0.01683 = 0.01351 -0.00146 0.00122 0.00503 AFIX 43 H00R 2 0.538047 0.818344 0.111092 11.00000 -1.20000 AFIX 0 C00S 1 0.124317 0.576318 0.331596 11.00000 0.01414 0.02251 = 0.03864 -0.00112 0.00216 -0.00312 AFIX 43 H00S 2 0.048297 0.556315 0.304396 11.00000 -1.20000 AFIX 0 C00T 1 0.229839 0.542851 0.301078 11.00000 0.01684 0.01604 = 0.03028 -0.00619 0.00136 -0.00244 AFIX 43 H00T 2 0.226244 0.498938 0.253875 11.00000 -1.20000 AFIX 0 C00U 1 0.129459 0.638817 0.401613 11.00000 0.01902 0.01741 = 0.03584 0.00246 0.01041 0.00258 AFIX 43 H00U 2 0.056838 0.661821 0.422073 11.00000 -1.20000 AFIX 0 C00V 1 0.534174 0.228294 0.338671 11.00000 0.03153 0.01334 = 0.02229 0.00036 0.00168 0.00403 AFIX 43 H00V 2 0.549643 0.165280 0.349694 11.00000 -1.20000 AFIX 0 C00W 1 0.610077 0.619003 0.064660 11.00000 0.03297 0.01524 = 0.01965 0.00022 0.00863 0.00357 AFIX 43 H00W 2 0.686480 0.635749 0.045911 11.00000 -1.20000 AFIX 0 C00X 1 0.594603 0.274518 0.274810 11.00000 0.03497 0.01682 = 0.02448 -0.00010 0.01094 0.00872 AFIX 43 H00X 2 0.650820 0.242812 0.241802 11.00000 -1.20000 AFIX 0 C00Y 1 0.508977 0.620829 0.003711 11.00000 0.04826 0.01277 = 0.01449 -0.00033 0.00142 0.00828 AFIX 43 H00Y 2 0.515698 0.640207 -0.056606 11.00000 -1.20000 AFIX 0 HKLF 4 REM msf6_39_0m_a.res in P2(1)/n REM R1 = 0.0346 for 5850 Fo > 4sig(Fo) and 0.0562 for all 7503 data REM 305 parameters refined using 0 restraints END WGHT 0.0231 1.6837 REM Highest difference peak 0.409, deepest hole -0.363, 1-sigma level 0.071 Q1 1 0.3408 0.6078 0.3744 11.00000 0.05 0.41 Q2 1 0.6596 0.5600 0.3775 11.00000 0.05 0.38 Q3 1 0.6157 0.6367 0.3634 11.00000 0.05 0.38 Q4 1 0.1788 0.5591 0.3181 11.00000 0.05 0.38 Q5 1 0.3867 0.8601 0.2918 11.00000 0.05 0.38 Q6 1 0.5586 0.6004 0.0346 11.00000 0.05 0.36 Q7 1 0.7388 0.5581 0.4334 11.00000 0.05 0.35 Q8 1 0.2875 0.5655 0.3226 11.00000 0.05 0.35 Q9 1 0.5827 0.3227 0.2738 11.00000 0.05 0.33 Q10 1 0.4031 0.5511 0.3283 11.00000 0.05 0.33 Q11 1 0.5104 0.3851 0.2804 11.00000 0.05 0.33 Q12 1 0.7963 0.6221 0.4373 11.00000 0.05 0.32 Q13 1 0.4689 0.2565 0.3473 11.00000 0.05 0.32 Q14 1 0.4403 0.5609 0.1504 11.00000 0.05 0.32 Q15 1 0.4008 0.5792 0.0711 11.00000 0.05 0.32 Q16 1 0.5498 0.9152 0.2649 11.00000 0.05 0.31 Q17 1 0.1849 0.6693 0.4070 11.00000 0.05 0.31 Q18 1 0.4836 0.4620 0.3008 11.00000 0.05 0.31 Q19 1 0.1288 0.5953 0.3788 11.00000 0.05 0.31 Q20 1 0.5985 0.6082 0.1045 11.00000 0.05 0.31 ; _shelx_res_checksum 30959 _olex2_exptl_crystal_mounting_method 'Mounted under paratone' _olex2_submission_special_instructions 'No special instructions were received' 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 Ni01 Ni 0.500000 1.000000 0.500000 0.01298(7) Uani 1 2 d S T P S002 S 0.61557(4) 0.98191(3) 0.38964(3) 0.01612(8) Uani 1 1 d . . . P003 P 0.47850(3) 0.53482(3) 0.29631(3) 0.01236(8) Uani 1 1 d . . . S004 S 0.36673(4) 0.90613(3) 0.43556(3) 0.01716(9) Uani 1 1 d . . . C005 C 0.60021(15) 0.59272(11) 0.15334(10) 0.0172(3) Uani 1 1 d . . . H005 H 0.669803 0.591350 0.195357 0.021 Uiso 1 1 calc R . . C006 C 0.61591(14) 0.68176(10) 0.35649(10) 0.0149(3) Uani 1 1 d . . . H006 H 0.557561 0.716760 0.320862 0.018 Uiso 1 1 calc R . . C007 C 0.53303(14) 0.91087(10) 0.31162(10) 0.0149(3) Uani 1 1 d . . . C008 C 0.79853(14) 0.67269(11) 0.45545(10) 0.0172(3) Uani 1 1 d . . . H008 H 0.864704 0.702143 0.488388 0.021 Uiso 1 1 calc R . . C009 C 0.34179(14) 0.57385(10) 0.33992(10) 0.0145(3) Uani 1 1 d . . . C00A C 0.69194(14) 0.53459(11) 0.41075(10) 0.0160(3) Uani 1 1 d . . . H00A H 0.684670 0.469993 0.412992 0.019 Uiso 1 1 calc R . . C00B C 0.48744(14) 0.56821(10) 0.18075(10) 0.0151(3) Uani 1 1 d . . . C00C C 0.71200(14) 0.72470(11) 0.40515(10) 0.0161(3) Uani 1 1 d . . . H00C H 0.718736 0.789369 0.404165 0.019 Uiso 1 1 calc R . . C00D C 0.49121(14) 0.41327(10) 0.30787(10) 0.0146(3) Uani 1 1 d . . . C00E C 0.42100(14) 0.87647(10) 0.33269(10) 0.0149(3) Uani 1 1 d . . . C00F C 0.42953(15) 0.36657(11) 0.37152(11) 0.0181(3) Uani 1 1 d . . . H00F H 0.372953 0.397871 0.404536 0.022 Uiso 1 1 calc R . . C00G C 0.57341(15) 0.36675(11) 0.25888(11) 0.0194(3) Uani 1 1 d . . . H00G H 0.614600 0.398095 0.214882 0.023 Uiso 1 1 calc R . . C00H C 0.34628(14) 0.63621(10) 0.41119(10) 0.0165(3) Uani 1 1 d . . . H00H H 0.421997 0.656759 0.438463 0.020 Uiso 1 1 calc R . . C00I C 0.60523(13) 0.58653(10) 0.36008(9) 0.0130(3) Uani 1 1 d . . . C00J C 0.35404(15) 0.82080(10) 0.27013(10) 0.0171(3) Uani 1 1 d . . . H00J H 0.278226 0.797383 0.284022 0.020 Uiso 1 1 calc R . . C00K C 0.57580(16) 0.88854(11) 0.22877(10) 0.0190(3) Uani 1 1 d . . . H00K H 0.651673 0.911436 0.214382 0.023 Uiso 1 1 calc R . . C00L C 0.39734(16) 0.79944(11) 0.18794(10) 0.0203(3) Uani 1 1 d . . . H00L H 0.351043 0.761766 0.145872 0.024 Uiso 1 1 calc R . . C00M C 0.23998(15) 0.66812(11) 0.44214(11) 0.0209(3) Uani 1 1 d . . . H00M H 0.242888 0.710019 0.491072 0.025 Uiso 1 1 calc R . . C00N C 0.38580(15) 0.56822(11) 0.11819(11) 0.0197(3) Uani 1 1 d . . . H00N H 0.309354 0.550336 0.136040 0.024 Uiso 1 1 calc R . . C00O C 0.45136(16) 0.27405(11) 0.38629(11) 0.0216(3) Uani 1 1 d . . . H00O H 0.409199 0.242050 0.429310 0.026 Uiso 1 1 calc R . . C00P C 0.78915(14) 0.57828(11) 0.45798(10) 0.0182(3) Uani 1 1 d . . . H00P H 0.849220 0.543400 0.492034 0.022 Uiso 1 1 calc R . . C00Q C 0.39755(18) 0.59453(11) 0.03000(11) 0.0252(4) Uani 1 1 d . . . H00Q H 0.328800 0.594571 -0.012828 0.030 Uiso 1 1 calc R . . C00R C 0.50829(16) 0.83312(11) 0.16722(11) 0.0212(3) Uani 1 1 d . . . H00R H 0.538047 0.818344 0.111092 0.025 Uiso 1 1 calc R . . C00S C 0.12432(15) 0.57632(12) 0.33160(13) 0.0251(4) Uani 1 1 d . . . H00S H 0.048297 0.556315 0.304396 0.030 Uiso 1 1 calc R . . C00T C 0.22984(15) 0.54285(11) 0.30108(12) 0.0211(3) Uani 1 1 d . . . H00T H 0.226244 0.498938 0.253875 0.025 Uiso 1 1 calc R . . C00U C 0.12946(16) 0.63882(12) 0.40161(12) 0.0236(4) Uani 1 1 d . . . H00U H 0.056838 0.661821 0.422073 0.028 Uiso 1 1 calc R . . C00V C 0.53417(16) 0.22829(11) 0.33867(11) 0.0224(3) Uani 1 1 d . . . H00V H 0.549643 0.165280 0.349694 0.027 Uiso 1 1 calc R . . C00W C 0.61008(17) 0.61900(11) 0.06466(11) 0.0222(3) Uani 1 1 d . . . H00W H 0.686480 0.635749 0.045911 0.027 Uiso 1 1 calc R . . C00X C 0.59460(17) 0.27452(12) 0.27481(12) 0.0249(4) Uani 1 1 d . . . H00X H 0.650820 0.242812 0.241802 0.030 Uiso 1 1 calc R . . C00Y C 0.50898(18) 0.62083(11) 0.00371(11) 0.0253(4) Uani 1 1 d . . . H00Y H 0.515698 0.640207 -0.056606 0.030 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 Ni01 0.01608(14) 0.00954(13) 0.01313(13) -0.00196(10) 0.00028(10) 0.00015(10) S002 0.01803(18) 0.01318(18) 0.01722(17) -0.00330(13) 0.00194(14) -0.00117(14) P003 0.01312(18) 0.00952(17) 0.01432(17) -0.00099(13) 0.00060(14) 0.00026(14) S004 0.01818(19) 0.01609(19) 0.01736(18) -0.00519(14) 0.00243(14) -0.00267(15) C005 0.0218(8) 0.0140(7) 0.0160(7) 0.0000(6) 0.0030(6) 0.0015(6) C006 0.0150(7) 0.0135(7) 0.0161(7) 0.0010(5) 0.0011(6) 0.0016(6) C007 0.0198(8) 0.0105(7) 0.0140(7) -0.0001(5) -0.0016(6) 0.0030(6) C008 0.0143(7) 0.0239(8) 0.0133(7) -0.0022(6) 0.0016(6) -0.0027(6) C009 0.0145(7) 0.0100(7) 0.0194(7) 0.0002(5) 0.0034(6) 0.0013(5) C00A 0.0171(7) 0.0143(7) 0.0166(7) 0.0019(5) 0.0011(6) 0.0019(6) C00B 0.0197(8) 0.0098(7) 0.0156(7) -0.0013(5) -0.0001(6) 0.0024(6) C00C 0.0174(7) 0.0139(7) 0.0171(7) -0.0012(6) 0.0027(6) -0.0027(6) C00D 0.0173(7) 0.0113(7) 0.0150(7) -0.0015(5) 0.0005(6) 0.0001(5) C00E 0.0193(7) 0.0100(7) 0.0146(7) -0.0002(5) -0.0015(6) 0.0037(6) C00F 0.0204(8) 0.0152(7) 0.0193(7) -0.0019(6) 0.0051(6) -0.0001(6) C00G 0.0254(9) 0.0152(8) 0.0186(7) 0.0005(6) 0.0065(6) 0.0023(6) C00H 0.0172(7) 0.0146(7) 0.0181(7) -0.0007(6) 0.0030(6) -0.0007(6) C00I 0.0131(7) 0.0141(7) 0.0120(6) -0.0014(5) 0.0017(5) -0.0004(5) C00J 0.0206(8) 0.0111(7) 0.0185(7) 0.0002(5) -0.0039(6) 0.0020(6) C00K 0.0247(8) 0.0152(7) 0.0172(7) 0.0011(6) 0.0030(6) 0.0025(6) C00L 0.0301(9) 0.0137(7) 0.0158(7) -0.0022(6) -0.0058(6) 0.0039(6) C00M 0.0240(8) 0.0151(8) 0.0248(8) -0.0025(6) 0.0083(7) 0.0005(6) C00N 0.0224(8) 0.0133(7) 0.0219(8) -0.0021(6) -0.0059(6) 0.0028(6) C00O 0.0296(9) 0.0146(8) 0.0210(8) 0.0018(6) 0.0038(7) -0.0027(7) C00P 0.0162(7) 0.0221(8) 0.0159(7) 0.0027(6) -0.0003(6) 0.0036(6) C00Q 0.0401(10) 0.0140(8) 0.0193(8) -0.0037(6) -0.0103(7) 0.0070(7) C00R 0.0332(9) 0.0168(8) 0.0135(7) -0.0015(6) 0.0012(6) 0.0050(7) C00S 0.0141(8) 0.0225(9) 0.0386(10) -0.0011(7) 0.0022(7) -0.0031(6) C00T 0.0168(8) 0.0160(8) 0.0303(9) -0.0062(6) 0.0014(6) -0.0024(6) C00U 0.0190(8) 0.0174(8) 0.0358(9) 0.0025(7) 0.0104(7) 0.0026(6) C00V 0.0315(9) 0.0133(7) 0.0223(8) 0.0004(6) 0.0017(7) 0.0040(7) C00W 0.0330(10) 0.0152(8) 0.0197(8) 0.0002(6) 0.0086(7) 0.0036(7) C00X 0.0350(10) 0.0168(8) 0.0245(8) -0.0001(6) 0.0109(7) 0.0087(7) C00Y 0.0483(11) 0.0128(7) 0.0145(7) -0.0003(6) 0.0014(7) 0.0083(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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 S002 Ni01 S002 180.000(19) 3_676 . S004 Ni01 S002 90.922(15) . . S004 Ni01 S002 90.923(15) 3_676 3_676 S004 Ni01 S002 89.078(15) . 3_676 S004 Ni01 S002 89.078(15) 3_676 . S004 Ni01 S004 180.0 . 3_676 C007 S002 Ni01 105.06(6) . . C00B P003 C009 112.30(7) . . C00D P003 C009 110.05(7) . . C00D P003 C00B 110.55(7) . . C00D P003 C00I 108.48(7) . . C00I P003 C009 108.95(7) . . C00I P003 C00B 106.38(7) . . C00E S004 Ni01 105.46(5) . . C00B C005 H005 120.1 . . C00W C005 H005 120.1 . . C00W C005 C00B 119.82(15) . . C00C C006 H006 120.1 . . C00C C006 C00I 119.71(14) . . C00I C006 H006 120.1 . . C00E C007 S002 119.13(11) . . C00K C007 S002 121.45(13) . . C00K C007 C00E 119.42(14) . . C00C C008 H008 119.7 . . C00P C008 H008 119.7 . . C00P C008 C00C 120.66(14) . . C00H C009 P003 120.51(12) . . C00H C009 C00T 119.65(14) . . C00T C009 P003 119.83(12) . . C00I C00A H00A 120.3 . . C00P C00A H00A 120.3 . . C00P C00A C00I 119.35(15) . . C005 C00B P003 118.43(11) . . C00N C00B P003 121.67(13) . . C00N C00B C005 119.89(14) . . C006 C00C C008 119.72(14) . . C006 C00C H00C 120.1 . . C008 C00C H00C 120.1 . . C00F C00D P003 120.78(12) . . C00G C00D P003 118.94(12) . . C00G C00D C00F 119.95(14) . . C007 C00E S004 119.26(11) . . C00J C00E S004 121.40(13) . . C00J C00E C007 119.33(14) . . C00D C00F H00F 120.2 . . C00O C00F C00D 119.65(15) . . C00O C00F H00F 120.2 . . C00D C00G H00G 120.2 . . C00X C00G C00D 119.66(15) . . C00X C00G H00G 120.2 . . C009 C00H H00H 120.0 . . C00M C00H C009 119.90(15) . . C00M C00H H00H 120.0 . . C006 C00I P003 117.72(11) . . C00A C00I P003 121.84(12) . . C00A C00I C006 120.43(14) . . C00E C00J H00J 119.7 . . C00L C00J C00E 120.66(16) . . C00L C00J H00J 119.7 . . C007 C00K H00K 119.7 . . C00R C00K C007 120.63(16) . . C00R C00K H00K 119.7 . . C00J C00L H00L 120.0 . . C00R C00L C00J 120.04(15) . . C00R C00L H00L 120.0 . . C00H C00M H00M 120.0 . . C00U C00M C00H 119.99(15) . . C00U C00M H00M 120.0 . . C00B C00N H00N 120.3 . . C00Q C00N C00B 119.40(17) . . C00Q C00N H00N 120.3 . . C00F C00O H00O 119.8 . . C00V C00O C00F 120.37(16) . . C00V C00O H00O 119.8 . . C008 C00P C00A 120.10(14) . . C008 C00P H00P 119.9 . . C00A C00P H00P 119.9 . . C00N C00Q H00Q 119.8 . . C00N C00Q C00Y 120.48(16) . . C00Y C00Q H00Q 119.8 . . C00K C00R H00R 120.0 . . C00L C00R C00K 119.91(15) . . C00L C00R H00R 120.0 . . C00T C00S H00S 119.9 . . C00U C00S H00S 119.9 . . C00U C00S C00T 120.11(16) . . C009 C00T H00T 120.1 . . C00S C00T C009 119.89(15) . . C00S C00T H00T 120.1 . . C00M C00U H00U 119.8 . . C00S C00U C00M 120.42(16) . . C00S C00U H00U 119.8 . . C00O C00V H00V 120.0 . . C00O C00V C00X 119.97(15) . . C00X C00V H00V 120.0 . . C005 C00W H00W 120.0 . . C00Y C00W C005 120.02(17) . . C00Y C00W H00W 120.0 . . C00G C00X C00V 120.40(16) . . C00G C00X H00X 119.8 . . C00V C00X H00X 119.8 . . C00Q C00Y H00Y 119.8 . . C00W C00Y C00Q 120.36(16) . . C00W C00Y H00Y 119.8 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni01 S002 2.1897(4) 3_676 Ni01 S002 2.1897(4) . Ni01 S004 2.1789(4) . Ni01 S004 2.1789(4) 3_676 S002 C007 1.7544(15) . P003 C009 1.7990(16) . P003 C00B 1.7978(16) . P003 C00D 1.7921(15) . P003 C00I 1.7939(15) . S004 C00E 1.7490(16) . C005 H005 0.9500 . C005 C00B 1.400(2) . C005 C00W 1.387(2) . C006 H006 0.9500 . C006 C00C 1.386(2) . C006 C00I 1.401(2) . C007 C00E 1.405(2) . C007 C00K 1.399(2) . C008 H008 0.9500 . C008 C00C 1.391(2) . C008 C00P 1.387(2) . C009 C00H 1.396(2) . C009 C00T 1.400(2) . C00A H00A 0.9500 . C00A C00I 1.395(2) . C00A C00P 1.391(2) . C00B C00N 1.398(2) . C00C H00C 0.9500 . C00D C00F 1.397(2) . C00D C00G 1.396(2) . C00E C00J 1.400(2) . C00F H00F 0.9500 . C00F C00O 1.390(2) . C00G H00G 0.9500 . C00G C00X 1.387(2) . C00H H00H 0.9500 . C00H C00M 1.388(2) . C00J H00J 0.9500 . C00J C00L 1.389(2) . C00K H00K 0.9500 . C00K C00R 1.391(2) . C00L H00L 0.9500 . C00L C00R 1.389(3) . C00M H00M 0.9500 . C00M C00U 1.387(2) . C00N H00N 0.9500 . C00N C00Q 1.384(2) . C00O H00O 0.9500 . C00O C00V 1.384(2) . C00P H00P 0.9500 . C00Q H00Q 0.9500 . C00Q C00Y 1.387(3) . C00R H00R 0.9500 . C00S H00S 0.9500 . C00S C00T 1.385(2) . C00S C00U 1.383(3) . C00T H00T 0.9500 . C00U H00U 0.9500 . C00V H00V 0.9500 . C00V C00X 1.388(2) . C00W H00W 0.9500 . C00W C00Y 1.379(2) . C00X H00X 0.9500 . C00Y H00Y 0.9500 .