#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:38:48 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132566.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_4132566 loop_ _publ_author_name 'Yuan, Shuai' 'Zhang, Peng' 'Zhang, Liangliang' 'Garcia-Esparza, Angel T' 'Sokaras, Dimosthenis' 'Qin, Jun-Sheng' 'Feng, Liang' 'Day, Gregory S.' 'Chen, Wenmiao' 'Drake, Hannah F.' 'Elumalai, Palani' 'Madrahimov, Sherzod T.' 'Sun, Daofeng' 'Zhou, Hong-Cai' _publ_section_title ; Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10814 _journal_page_last 10819 _journal_paper_doi 10.1021/jacs.8b04886 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C16 H22 Cl2 N2 Ni O6 S2, 2(C2 H6 O S)' _chemical_formula_sum 'C20 H34 Cl2 N2 Ni O8 S4' _chemical_formula_weight 688.34 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-05-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _cell_angle_alpha 73.312(3) _cell_angle_beta 82.332(3) _cell_angle_gamma 75.812(3) _cell_formula_units_Z 1 _cell_length_a 7.1382(9) _cell_length_b 10.4292(12) _cell_length_c 10.7797(13) _cell_measurement_reflns_used 8439 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.629 _cell_measurement_theta_min 2.467 _cell_volume 743.54(16) _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 293(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f 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 0.0297 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10397 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.629 _diffrn_reflns_theta_min 2.467 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6030 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour greenish _exptl_crystal_colour_modifier greenish _exptl_crystal_density_diffrn 1.537 _exptl_crystal_description needle _exptl_crystal_F_000 358 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.344 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 3382 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0319 _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^)+(0.0252P)^2^+0.6965P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0790 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2979 _reflns_number_total 3382 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04886_si_002.cif _cod_data_source_block NiINA2 _cod_database_code 4132566 _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 0.966 _shelx_estimated_absorpt_t_min 0.893 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C4(H4), C6(H6), C3(H3) 2.b Idealised Me refined as rotating group: C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C7(H7a,H7b,H7c) 2.c Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; NiINA2.res created by SHELXL-2014/7 TITL NiINA2_a.res in P-1 REM Old TITL NiINA2 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.070, Rweak 0.005, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C20 Cl2 N4 Ni O6 S4 CELL 0.71073 7.1382 10.4292 10.7797 73.312 82.332 75.812 ZERR 1 0.0009 0.0012 0.0013 0.003 0.003 0.003 LATT 1 SFAC C H Cl N Ni O S UNIT 20 34 2 2 1 8 4 L.S. 99 PLAN 5 SIZE 0.03 0.05 0.1 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.025200 0.696500 FVAR 0.85387 NI1 5 1.000000 0.500000 1.000000 10.50000 0.01092 0.01021 = 0.00760 -0.00138 -0.00132 -0.00235 CL1 3 0.886123 0.310202 0.971804 11.00000 0.01591 0.01319 = 0.01285 -0.00318 -0.00081 -0.00503 S003 7 0.707835 0.641604 1.201315 11.00000 0.01577 0.01327 = 0.01313 -0.00439 -0.00063 -0.00187 S004 7 0.044402 0.986503 0.275872 11.00000 0.01927 0.01876 = 0.01434 -0.00580 -0.00120 -0.00664 O4 6 0.776919 0.518749 1.145110 11.00000 0.01394 0.01299 = 0.01134 -0.00518 0.00098 -0.00224 O1 6 0.523292 0.876201 0.430153 11.00000 0.01866 0.02290 = 0.00979 0.00011 -0.00229 -0.00584 O3 6 0.093698 0.845280 0.371463 11.00000 0.02080 0.02684 = 0.01379 0.00252 -0.00570 -0.00820 O2 6 0.279530 0.808565 0.566547 11.00000 0.01401 0.05539 = 0.01175 0.00012 -0.00382 -0.01057 AFIX 147 H2 2 0.224517 0.828136 0.499342 11.00000 -1.50000 AFIX 0 N1 4 0.817192 0.632618 0.857865 11.00000 0.01250 0.01030 = 0.01091 -0.00270 -0.00177 -0.00232 C5 1 0.625027 0.640427 0.873685 11.00000 0.01484 0.01427 = 0.01103 -0.00130 -0.00031 -0.00453 AFIX 43 H5 2 0.572666 0.599416 0.954888 11.00000 -1.20000 AFIX 0 C4 1 0.889415 0.697403 0.741153 11.00000 0.01218 0.01241 = 0.01361 -0.00202 -0.00038 -0.00335 AFIX 43 H4 2 1.020983 0.697042 0.730139 11.00000 -1.20000 AFIX 0 C2 1 0.579369 0.766817 0.653214 11.00000 0.01426 0.01129 = 0.01089 -0.00369 -0.00210 -0.00094 C6 1 0.501704 0.706256 0.775432 11.00000 0.01180 0.01740 = 0.01182 -0.00388 -0.00050 -0.00364 AFIX 43 H6 2 0.369334 0.710131 0.790483 11.00000 -1.20000 AFIX 0 C3 1 0.776422 0.764534 0.636815 11.00000 0.01467 0.01403 = 0.00954 -0.00232 0.00036 -0.00410 AFIX 43 H3 2 0.831453 0.807284 0.557261 11.00000 -1.20000 AFIX 0 C1 1 0.458342 0.824934 0.538269 11.00000 0.01356 0.01447 = 0.01427 -0.00436 -0.00211 -0.00124 C10 1 -0.141620 0.976164 0.187568 11.00000 0.01957 0.01873 = 0.01741 -0.00150 -0.00517 -0.00428 AFIX 137 H10A 2 -0.097813 0.900017 0.150003 11.00000 -1.50000 H10B 2 -0.173301 1.059438 0.119882 11.00000 -1.50000 H10C 2 -0.254406 0.963443 0.245036 11.00000 -1.50000 AFIX 0 C9 1 0.236188 0.989698 0.151648 11.00000 0.02161 0.02988 = 0.01699 -0.00095 -0.00086 -0.00731 AFIX 137 H9A 2 0.354249 0.986100 0.187265 11.00000 -1.50000 H9B 2 0.205838 1.072656 0.083420 11.00000 -1.50000 H9C 2 0.251790 0.912057 0.117341 11.00000 -1.50000 AFIX 0 C8 1 0.483385 0.613873 1.286925 11.00000 0.01609 0.02719 = 0.02252 -0.01232 0.00204 -0.00350 AFIX 137 H8A 2 0.392798 0.619142 1.226387 11.00000 -1.50000 H8B 2 0.432776 0.682744 1.332908 11.00000 -1.50000 H8C 2 0.503778 0.524809 1.347556 11.00000 -1.50000 AFIX 0 C7 1 0.846722 0.606654 1.337795 11.00000 0.02254 0.02717 = 0.01732 -0.00986 -0.00264 -0.00703 AFIX 137 H7A 2 0.838613 0.518057 1.394286 11.00000 -1.50000 H7B 2 0.796765 0.675371 1.384031 11.00000 -1.50000 H7C 2 0.979507 0.607733 1.308493 11.00000 -1.50000 AFIX 0 HKLF 4 REM NiINA2_a.res in P-1 REM R1 = 0.0319 for 2979 Fo > 4sig(Fo) and 0.0399 for all 3382 data REM 174 parameters refined using 0 restraints END WGHT 0.0252 0.6965 REM Highest difference peak 0.344, deepest hole -0.627, 1-sigma level 0.104 Q1 1 0.5031 0.5893 1.4871 11.00000 0.05 0.34 Q2 1 0.5959 0.4557 1.1638 11.00000 0.05 0.33 Q3 1 -0.1970 0.7992 0.0733 11.00000 0.05 0.32 Q4 1 0.5511 0.7475 0.7181 11.00000 0.05 0.32 Q5 1 1.0095 0.6579 0.7333 11.00000 0.05 0.31 ; _shelx_res_checksum 3687 _shelx_hkl_file ; -1 0 0 1602.38 60.78 -1 0 0 1680.69 60.85 -1 0 0 1670.87 61.16 1 0 0 1654.74 61.15 -2 0 0 302.98 12.34 -2 0 0 310.36 12.99 -2 0 0 298.69 12.35 2 0 0 310.93 13.08 2 0 0 311.87 12.47 -3 0 0 221.51 9.89 -3 0 0 229.74 10.89 -3 0 0 221.91 10.40 3 0 0 226.46 10.13 3 0 0 233.50 10.19 3 0 0 227.98 10.95 -4 0 0 645.34 27.11 -4 0 0 646.28 26.01 -4 0 0 634.34 25.85 4 0 0 628.04 26.05 4 0 0 672.05 27.64 4 0 0 663.31 26.21 -5 0 0 169.07 9.56 -5 0 0 164.10 10.77 -5 0 0 179.18 9.12 5 0 0 192.13 9.93 5 0 0 188.30 11.32 5 0 0 174.77 9.93 6 0 0 19.33 4.13 -7 0 0 148.02 9.28 7 0 0 147.69 12.79 7 0 0 147.55 11.57 -8 0 0 175.18 11.06 8 0 0 146.41 13.84 8 0 0 134.73 15.13 8 -1 0 -1.57 7.29 8 -1 0 7.19 7.22 -8 1 0 15.26 4.64 7 -1 0 35.27 9.95 7 -1 0 36.13 9.25 -7 1 0 32.12 6.26 6 -1 0 58.34 7.67 6 -1 0 49.54 8.77 -6 1 0 59.63 5.65 5 -1 0 88.15 7.38 5 -1 0 110.99 8.40 5 -1 0 101.38 7.51 -5 1 0 85.83 8.04 -5 1 0 99.09 6.23 -5 1 0 89.54 7.18 4 -1 0 376.02 16.21 4 -1 0 369.34 15.96 4 -1 0 372.33 17.17 -4 1 0 349.90 15.32 -4 1 0 357.61 16.99 -4 1 0 357.66 16.02 3 -1 0 709.14 28.05 3 -1 0 721.58 28.85 3 -1 0 708.02 27.71 -3 1 0 718.43 27.98 -3 1 0 673.74 27.38 -3 1 0 717.91 28.74 2 -1 0 134.69 6.58 2 -1 0 127.61 6.09 2 -1 0 122.74 5.76 -2 1 0 122.80 5.64 -2 1 0 119.64 6.37 -2 1 0 127.20 6.09 1 -1 0 347.79 13.86 1 -1 0 361.06 14.12 -1 1 0 363.32 14.15 -1 1 0 344.74 13.82 -1 -1 0 379.15 14.08 -1 -1 0 352.30 13.61 1 1 0 346.22 13.60 1 1 0 351.13 13.78 1 1 0 375.72 14.12 -2 -1 0 994.43 38.82 -2 -1 0 1047.15 39.39 2 1 0 1084.75 39.63 2 1 0 1004.39 38.89 -3 -1 0 177.15 8.46 -3 -1 0 188.41 9.30 3 1 0 186.55 8.88 3 1 0 212.70 9.89 -4 -1 0 66.51 4.77 -4 -1 0 61.71 5.41 -4 -1 0 60.56 4.46 4 1 0 68.32 4.74 4 1 0 64.18 5.13 4 1 0 69.94 5.94 -5 -1 0 78.23 5.71 -5 -1 0 79.58 6.96 -5 -1 0 75.92 6.26 5 1 0 96.25 7.75 5 1 0 81.27 6.92 5 1 0 89.88 6.29 -6 -1 0 546.77 23.18 -6 -1 0 493.40 23.09 6 1 0 540.13 25.98 6 1 0 591.87 23.88 -7 -1 0 556.92 24.32 7 1 0 622.22 31.41 7 1 0 504.56 27.22 -8 -1 0 405.01 18.88 8 1 0 441.88 20.93 8 1 0 326.95 22.63 -9 -1 0 5.44 6.61 9 1 0 -1.02 8.54 9 1 0 10.68 10.52 8 -2 0 52.97 14.05 8 -2 0 62.66 13.54 7 -2 0 11.88 6.04 7 -2 0 14.94 5.86 6 -2 0 205.16 17.77 6 -2 0 242.11 13.67 5 -2 0 793.04 31.97 5 -2 0 785.73 33.12 5 -2 0 759.20 31.12 -5 2 0 733.71 31.75 -5 2 0 774.65 30.49 -5 2 0 691.88 32.41 4 -2 0 267.22 12.44 4 -2 0 283.33 13.84 4 -2 0 272.80 13.11 -4 2 0 261.89 11.86 -4 2 0 260.83 13.62 -4 2 0 245.74 12.55 3 -2 0 2082.86 77.14 3 -2 0 2070.00 76.45 3 -2 0 1985.58 75.62 -3 2 0 1987.14 75.41 -3 2 0 2023.22 76.22 -3 2 0 1984.20 76.94 2 -2 0 499.63 20.45 2 -2 0 499.15 20.12 -2 2 0 487.76 20.54 -2 2 0 509.54 20.62 1 -2 0 1.58 0.59 -1 2 0 0.41 0.81 -1 2 0 2.00 0.68 0 -2 0 16.93 1.75 0 -2 0 21.33 1.65 0 2 0 16.68 1.54 -1 -2 0 7323.38 263.13 -1 -2 0 6902.16 263.26 1 2 0 7533.07 263.15 1 2 0 7020.45 263.33 -2 -2 0 186.33 8.04 -2 -2 0 179.79 8.29 -2 -2 0 202.92 8.82 2 2 0 195.51 8.41 2 2 0 208.38 9.04 2 2 0 203.02 8.12 -3 -2 0 104.62 5.74 -3 -2 0 117.42 6.45 3 2 0 112.15 5.97 3 2 0 115.60 6.70 3 2 0 105.74 5.12 -4 -2 0 2097.94 81.36 -4 -2 0 2028.42 80.34 4 2 0 2153.32 80.72 4 2 0 2288.53 82.51 -5 -2 0 1332.95 55.97 -5 -2 0 1410.66 55.01 5 2 0 1498.97 57.47 5 2 0 1471.41 55.52 -6 -2 0 261.21 12.75 6 2 0 242.69 15.07 -7 -2 0 42.04 6.10 7 2 0 42.44 9.24 -8 -2 0 181.97 11.39 8 2 0 148.16 14.93 -9 -2 0 63.41 9.66 9 2 0 43.34 9.68 8 -3 0 -2.30 8.23 8 -3 0 -1.88 8.55 -8 3 0 -3.83 5.58 7 -3 0 0.24 6.33 7 -3 0 4.52 6.24 -7 3 0 -3.66 3.92 6 -3 0 277.39 16.78 6 -3 0 282.36 15.91 -6 3 0 270.95 13.84 5 -3 0 1092.40 45.46 5 -3 0 1102.61 44.63 4 -3 0 553.92 23.86 4 -3 0 553.91 23.14 -4 3 0 503.86 22.72 -4 3 0 511.35 23.71 3 -3 0 149.54 8.22 -3 3 0 149.86 8.79 -3 3 0 141.68 7.99 2 -3 0 117.85 6.36 -2 3 0 111.25 6.55 -2 3 0 114.55 6.20 -2 3 0 107.10 6.64 1 -3 0 1210.00 44.44 1 -3 0 1142.94 44.25 -1 3 0 1173.38 43.79 -1 3 0 1164.99 44.32 -1 3 0 1167.34 44.56 0 -3 0 1482.24 54.52 0 -3 0 1437.67 54.87 0 3 0 1469.85 54.52 -1 -3 0 59.22 3.35 -1 -3 0 62.52 3.65 1 3 0 62.37 3.41 1 3 0 61.84 3.62 -2 -3 0 500.05 20.02 -2 -3 0 522.83 20.55 -2 -3 0 495.22 19.95 2 3 0 523.70 20.78 2 3 0 522.01 20.05 -3 -3 0 7.11 1.81 -3 -3 0 7.93 1.77 -3 -3 0 11.21 2.15 3 3 0 6.45 1.76 3 3 0 5.28 1.27 3 3 0 7.87 2.00 -4 -3 0 1014.41 40.43 -4 -3 0 1041.97 41.26 -4 -3 0 1027.43 39.47 4 3 0 1019.93 40.60 4 3 0 1109.77 42.35 -5 -3 0 240.47 11.58 -5 -3 0 238.07 12.85 5 3 0 248.74 13.79 5 3 0 241.49 12.41 -6 -3 0 29.96 5.15 -7 -3 0 5.80 3.77 7 3 0 2.64 5.28 -8 -3 0 49.35 7.63 8 3 0 47.65 11.91 -9 -3 0 191.20 13.15 9 3 0 162.14 17.52 7 -4 0 13.21 7.41 6 -4 0 34.99 6.68 -6 4 0 52.71 6.48 5 -4 0 927.25 39.27 4 -4 0 410.04 18.15 -4 4 0 348.58 17.49 -4 4 0 386.51 18.50 -4 4 0 372.20 18.60 3 -4 0 43.13 4.84 -3 4 0 42.64 5.21 -3 4 0 41.55 5.49 -3 4 0 44.85 4.72 2 -4 0 11.39 1.80 2 -4 0 14.52 3.04 -2 4 0 8.21 2.32 -2 4 0 12.92 2.20 -2 4 0 9.50 2.10 -2 4 0 11.30 2.13 1 -4 0 1972.50 73.45 1 -4 0 2022.82 72.99 -1 4 0 1940.38 73.71 -1 4 0 1944.83 72.98 -1 4 0 1919.60 73.38 0 -4 0 180.05 8.23 0 -4 0 162.19 7.58 0 4 0 161.78 7.93 -1 -4 0 1875.10 71.17 -1 -4 0 1914.34 70.92 1 4 0 1897.22 71.28 1 4 0 1911.46 70.90 -2 -4 0 1626.20 60.49 -2 -4 0 1574.28 60.02 2 4 0 1597.36 60.03 2 4 0 1599.56 60.67 -3 -4 0 1165.49 45.05 -3 -4 0 1196.93 45.80 -3 -4 0 1151.53 45.27 3 4 0 1197.84 45.10 3 4 0 1220.06 46.54 -4 -4 0 280.30 13.26 -4 -4 0 269.77 11.93 -4 -4 0 263.81 12.42 4 4 0 269.32 12.65 4 4 0 291.43 14.13 4 4 0 277.91 12.01 -5 -4 0 790.69 32.92 -5 -4 0 769.12 33.75 -5 -4 0 839.94 31.96 5 4 0 876.33 35.49 5 4 0 839.37 32.09 5 4 0 812.28 33.23 -6 -4 0 53.04 5.68 6 4 0 51.04 9.38 -7 -4 0 35.80 6.42 7 4 0 46.42 9.59 -8 -4 0 22.54 4.94 8 4 0 16.80 7.05 -9 -4 0 249.73 17.46 9 4 0 209.13 22.08 7 -5 0 132.01 14.45 -7 5 0 122.18 15.73 6 -5 0 28.77 6.59 -6 5 0 40.47 10.87 5 -5 0 -1.34 4.43 4 -5 0 109.93 8.80 -4 5 0 121.60 9.73 -4 5 0 115.76 9.16 3 -5 0 185.88 10.33 -3 5 0 176.67 11.04 -3 5 0 183.09 10.59 -3 5 0 174.88 9.99 2 -5 0 30.29 4.03 2 -5 0 30.66 2.88 -2 5 0 26.06 5.07 -2 5 0 29.96 3.17 -2 5 0 26.49 3.95 -2 5 0 25.59 3.78 1 -5 0 372.52 15.94 1 -5 0 374.81 15.40 1 -5 0 376.76 16.68 -1 5 0 349.96 15.64 -1 5 0 379.54 15.44 -1 5 0 371.11 16.13 0 -5 0 2.73 1.86 0 -5 0 4.86 1.34 0 5 0 5.27 1.57 0 5 0 5.76 1.57 -1 -5 0 149.18 7.74 -1 -5 0 143.14 7.16 1 5 0 141.28 7.21 1 5 0 143.35 7.50 -2 -5 0 1446.34 54.58 -2 -5 0 1422.18 54.18 2 5 0 1408.18 54.14 2 5 0 1432.62 54.80 -3 -5 0 44.84 3.78 -3 -5 0 44.72 3.91 3 5 0 51.18 4.09 3 5 0 40.96 4.59 -4 -5 0 269.54 12.13 -4 -5 0 257.07 13.04 -4 -5 0 255.67 12.17 4 5 0 278.47 14.01 4 5 0 272.80 12.12 -5 -5 0 4.63 2.03 -5 -5 0 2.95 3.54 -5 -5 0 3.13 2.59 5 5 0 2.34 2.42 5 5 0 0.89 3.43 5 5 0 3.77 3.51 -6 -5 0 40.76 5.14 -6 -5 0 34.64 7.12 6 5 0 28.56 6.34 6 5 0 34.05 5.77 -7 -5 0 52.88 7.24 7 5 0 35.99 10.79 -8 -5 0 78.89 9.48 8 5 0 51.64 12.31 -7 6 0 -1.14 8.08 -7 6 0 -1.10 6.45 -6 6 0 25.96 6.66 5 -6 0 292.35 16.23 -5 6 0 282.13 16.99 4 -6 0 181.58 11.40 -4 6 0 178.34 11.96 3 -6 0 287.89 12.93 3 -6 0 305.91 15.03 -3 6 0 305.19 15.10 -3 6 0 300.32 13.32 -3 6 0 301.01 16.12 2 -6 0 321.54 13.89 2 -6 0 335.95 15.23 -2 6 0 292.25 14.67 -2 6 0 322.43 14.06 -2 6 0 335.65 16.00 -2 6 0 317.32 15.06 1 -6 0 2813.36 102.70 1 -6 0 2809.26 103.21 1 -6 0 2793.33 104.21 -1 6 0 2606.17 102.80 -1 6 0 2788.45 102.69 -1 6 0 2694.59 103.42 0 -6 0 3778.12 138.67 0 -6 0 3745.42 139.45 0 6 0 3732.74 139.23 0 6 0 3688.29 138.58 -1 -6 0 283.89 13.08 -1 -6 0 285.94 12.64 1 6 0 276.78 13.00 1 6 0 277.28 12.64 -2 -6 0 36.85 3.85 -2 -6 0 42.88 4.95 2 6 0 34.41 4.11 2 6 0 45.19 4.25 -3 -6 0 265.05 13.04 -3 -6 0 277.14 12.54 3 6 0 280.45 13.46 3 6 0 263.36 12.48 -4 -6 0 109.55 7.03 -4 -6 0 112.83 7.10 -4 -6 0 112.67 8.12 4 6 0 124.55 8.67 4 6 0 114.97 7.07 -5 -6 0 203.53 10.53 -5 -6 0 203.15 10.86 5 6 0 216.24 13.22 5 6 0 201.46 10.79 -6 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361.43 17.26 -2 -4 -11 120.18 10.44 -2 -4 -11 140.92 9.35 -3 -4 -11 231.18 13.49 -3 -4 -11 220.01 12.57 -3 -4 -11 179.37 18.52 -4 -4 -11 141.44 11.45 -4 -4 -11 155.21 12.16 -5 -4 -11 44.29 12.08 -5 -4 -11 65.51 10.61 -6 -4 -11 374.25 20.04 -6 -4 -11 359.65 22.32 4 -5 -11 88.49 12.04 4 -5 -11 76.85 15.62 -4 5 11 92.74 13.80 3 -5 -11 151.62 11.77 3 -5 -11 109.23 12.55 -3 5 11 144.79 12.61 2 -5 -11 57.22 9.42 2 -5 -11 61.51 9.35 1 -5 -11 113.76 10.38 1 -5 -11 134.29 10.75 -1 5 11 135.00 11.02 0 -5 -11 -2.58 4.10 0 -5 -11 -3.55 3.83 0 5 11 -2.29 4.88 -1 -5 -11 31.42 6.75 -1 -5 -11 27.70 4.81 1 5 11 20.12 4.84 -2 -5 -11 255.21 15.26 2 5 11 280.98 14.65 -3 -5 -11 187.71 12.23 3 5 11 167.52 11.65 -4 -5 -11 -6.77 4.77 -4 -5 -11 6.60 5.08 -5 -5 -11 6.11 5.12 -5 -5 -11 6.18 6.96 -6 -5 -11 150.97 12.68 -6 -5 -11 118.42 15.34 3 -6 -11 260.14 17.53 3 -6 -11 298.52 17.03 -3 6 11 292.41 17.74 2 -6 -11 187.64 13.75 2 -6 -11 183.95 13.76 -2 6 11 205.67 14.21 1 -6 -11 10.90 4.95 1 -6 -11 7.13 4.59 -1 6 11 13.65 5.69 0 -6 -11 350.37 18.35 0 -6 -11 339.99 17.52 0 6 11 353.61 18.43 -1 -6 -11 38.54 8.00 1 6 11 26.53 5.64 -2 -6 -11 204.63 13.53 2 6 11 223.88 13.07 -3 -6 -11 461.48 21.95 3 6 11 430.00 21.24 -4 -6 -11 851.99 36.67 -5 -6 -11 11.75 6.66 -5 -6 -11 2.91 5.22 -6 -6 -11 132.77 14.41 -6 -6 -11 107.50 12.36 -6 -6 -11 119.99 16.21 3 -7 -11 12.10 5.61 3 -7 -11 19.49 7.97 -3 7 11 4.61 8.92 2 -7 -11 8.45 5.22 2 -7 -11 3.23 6.50 -2 7 11 -1.61 6.36 1 -7 -11 322.59 18.51 1 -7 -11 377.59 18.98 -1 7 11 362.08 19.39 0 -7 -11 52.17 9.03 0 7 11 35.24 6.52 -1 -7 -11 23.15 4.93 1 7 11 27.41 5.94 -2 -7 -11 35.20 5.52 2 7 11 50.07 9.13 -3 -7 -11 125.39 10.92 3 7 11 107.36 10.91 -4 -7 -11 714.39 31.60 -5 -7 -11 4.40 5.52 -5 -7 -11 10.82 6.45 -6 -7 -11 53.86 11.78 -6 -7 -11 66.10 13.23 2 -8 -11 210.91 14.59 2 -8 -11 209.32 15.86 -2 8 11 211.50 15.57 1 -8 -11 38.74 10.15 1 -8 -11 37.23 6.05 -1 8 11 59.08 11.17 0 -8 -11 109.88 10.49 0 8 11 102.62 11.92 -1 -8 -11 843.24 37.55 1 8 11 924.25 38.19 -2 -8 -11 649.89 29.95 2 8 11 697.31 30.26 -3 -8 -11 113.76 11.74 3 8 11 147.49 11.78 -4 -8 -11 370.98 19.54 4 8 11 373.67 19.93 -5 -8 -11 91.85 12.51 -5 -8 -11 137.11 12.95 -6 -8 -11 14.89 8.12 -6 -8 -11 11.10 7.05 1 -9 -11 200.76 14.30 -1 9 11 212.15 15.11 0 -9 -11 -1.23 5.28 0 9 11 20.01 6.55 -1 -9 -11 5.06 5.02 1 9 11 -1.27 5.97 2 9 11 49.90 10.10 -3 -9 -11 74.70 10.96 3 9 11 85.44 11.48 -4 -9 -11 83.43 11.77 4 9 11 76.26 12.09 -5 -9 -11 7.17 6.53 0 -10 -11 46.51 11.10 0 10 11 66.09 12.73 -1 -10 -11 14.14 5.74 1 10 11 2.05 6.71 -2 -10 -11 132.92 12.48 2 10 11 146.79 12.79 -3 -10 -11 94.52 12.03 3 10 11 110.82 12.88 -4 -10 -11 8.95 6.44 4 10 11 23.42 7.15 1 3 -12 5.51 6.93 0 3 -12 531.41 28.08 0 3 -12 600.11 30.81 0 -3 12 559.71 29.87 -1 3 -12 15.68 6.78 1 -3 12 12.45 6.15 2 2 -12 10.31 7.17 2 2 -12 13.65 6.48 -2 -2 12 3.98 6.49 1 2 -12 7.82 6.76 -1 -2 12 12.21 6.07 0 2 -12 419.67 21.84 0 2 -12 401.14 20.96 0 -2 12 380.61 21.79 -1 2 -12 274.86 16.46 -1 2 -12 243.39 16.88 1 -2 12 237.57 16.33 -2 2 -12 40.41 7.13 -2 2 -12 49.20 11.61 3 -2 12 31.56 6.65 3 1 -12 51.95 14.44 -3 -1 12 79.50 12.04 2 1 -12 632.82 30.45 2 1 -12 706.04 31.13 -2 -1 12 644.97 31.19 1 1 -12 279.16 17.05 1 1 -12 287.88 16.94 -1 -1 12 298.52 17.79 0 1 -12 194.03 13.23 0 1 -12 166.45 13.51 0 -1 12 182.04 13.80 -1 1 -12 296.38 17.84 -1 1 -12 314.78 17.33 1 -1 12 305.25 17.94 -2 1 -12 46.47 10.65 -2 1 -12 51.82 10.72 2 -1 12 44.32 10.24 -3 1 -12 82.25 11.68 3 -1 12 67.90 11.58 3 0 -12 327.18 19.92 3 0 -12 269.44 17.39 -3 0 12 289.18 18.49 2 0 -12 394.12 20.33 2 0 -12 332.03 19.31 -2 0 12 338.60 19.67 1 0 -12 47.66 9.91 1 0 -12 56.28 9.45 -1 0 12 48.91 10.01 0 0 -12 77.85 10.21 0 0 -12 90.45 9.92 0 0 12 102.03 10.71 -1 0 -12 24.20 5.65 -2 0 -12 2.33 5.41 -2 0 -12 3.01 5.29 2 0 12 0.13 5.13 -3 0 -12 107.47 12.09 -3 0 -12 127.76 13.14 3 0 12 128.00 11.92 -4 0 -12 3.51 6.39 -4 0 -12 8.81 6.59 3 -1 -12 -2.77 10.10 3 -1 -12 0.78 6.27 -3 1 12 8.54 6.47 2 -1 -12 -1.96 6.77 -2 1 12 1.57 5.56 1 -1 -12 244.56 14.92 1 -1 -12 257.00 14.68 -1 1 12 240.58 15.77 0 -1 -12 26.73 8.02 0 1 12 19.86 5.14 -1 -1 -12 73.97 11.09 -1 -1 -12 105.80 9.62 1 1 12 87.04 10.39 -2 -1 -12 344.25 18.94 -2 -1 -12 382.39 18.66 2 1 12 334.39 19.15 -3 -1 -12 1024.60 42.75 -3 -1 -12 996.02 43.26 -4 -1 -12 146.55 14.33 -4 -1 -12 161.42 13.32 -4 -1 -12 141.65 13.31 -5 -1 -12 541.91 27.56 -5 -1 -12 597.43 28.35 -5 -1 -12 554.04 29.36 3 -2 -12 -0.86 6.71 2 -2 -12 3.14 5.90 2 -2 -12 10.98 8.42 1 -2 -12 82.22 9.93 1 -2 -12 88.09 9.66 0 -2 -12 7.13 5.21 0 -2 -12 1.14 4.27 -1 -2 -12 5.47 4.63 -1 -2 -12 3.11 4.29 -2 -2 -12 674.28 29.44 -2 -2 -12 665.60 29.39 -3 -2 -12 125.70 11.85 -3 -2 -12 108.71 11.52 -3 -2 -12 129.32 11.25 -4 -2 -12 23.06 5.89 -4 -2 -12 6.73 6.06 -4 -2 -12 14.75 6.27 -5 -2 -12 19.79 6.21 3 -3 -12 8.29 5.74 2 -3 -12 1.21 5.50 1 -3 -12 210.12 13.24 1 -3 -12 210.11 14.07 0 -3 -12 164.01 12.49 0 -3 -12 167.35 11.76 -1 -3 -12 9.94 4.65 -1 -3 -12 12.44 4.96 -2 -3 -12 337.48 17.33 -2 -3 -12 332.69 17.21 -2 -3 -12 353.57 18.89 -3 -3 -12 747.10 33.59 -3 -3 -12 777.94 33.16 -3 -3 -12 807.46 35.04 -4 -3 -12 187.28 14.10 -4 -3 -12 198.99 14.68 -4 -3 -12 199.45 14.36 -5 -3 -12 11.22 7.08 3 -4 -12 114.01 12.90 -3 4 12 125.06 13.61 2 -4 -12 84.82 11.77 2 -4 -12 100.96 11.22 -2 4 12 95.62 11.75 1 -4 -12 251.92 15.19 1 -4 -12 239.97 15.55 0 -4 -12 997.15 41.49 0 -4 -12 1011.90 43.16 -1 -4 -12 4.95 4.82 -1 -4 -12 19.54 5.16 -2 -4 -12 45.63 6.80 -3 -4 -12 24.28 5.49 -4 -4 -12 5.27 5.80 -4 -4 -12 -5.63 5.47 -5 -4 -12 173.03 14.57 -5 -4 -12 147.06 14.89 3 -5 -12 20.76 7.73 -3 5 12 12.39 7.83 2 -5 -12 325.24 19.17 2 -5 -12 326.56 18.63 -2 5 12 372.56 19.45 1 -5 -12 22.32 6.31 1 -5 -12 26.23 5.53 -1 5 12 24.17 6.42 0 -5 -12 459.42 22.07 0 -5 -12 454.64 23.09 0 5 12 468.97 22.63 -1 -5 -12 21.73 5.10 -2 -5 -12 91.10 10.93 -3 -5 -12 45.29 9.80 -4 -5 -12 597.91 28.34 -4 -5 -12 589.28 27.80 -5 -5 -12 231.65 15.98 -5 -5 -12 223.98 16.86 2 -6 -12 62.89 11.68 2 -6 -12 56.27 11.71 1 -6 -12 2.33 5.52 1 -6 -12 2.98 5.33 -1 6 12 0.06 6.59 0 -6 -12 5.63 5.59 0 -6 -12 5.57 5.12 0 6 12 -3.12 5.94 -1 -6 -12 421.64 21.73 -1 -6 -12 417.00 20.43 1 6 12 434.66 21.54 -2 -6 -12 96.50 10.93 2 6 12 94.60 10.88 -3 -6 -12 4.30 5.17 3 6 12 -5.55 5.68 -4 -6 -12 224.16 15.14 -5 -6 -12 217.02 15.63 2 -7 -12 2.38 7.24 2 -7 -12 7.38 6.28 -2 7 12 2.88 7.53 1 -7 -12 -5.90 6.30 -1 7 12 0.99 6.84 0 -7 -12 24.64 5.63 0 -7 -12 20.51 5.69 0 7 12 10.61 6.61 -1 -7 -12 217.18 15.14 1 7 12 253.97 15.69 -2 -7 -12 479.14 23.37 2 7 12 461.93 22.99 -3 -7 -12 202.44 14.64 3 7 12 209.91 14.85 -4 -7 -12 768.91 34.17 -5 -7 -12 187.05 15.63 -5 -7 -12 211.90 15.88 1 -8 -12 179.23 14.88 1 -8 -12 208.43 14.78 -1 8 12 204.19 15.75 0 -8 -12 151.69 12.94 0 8 12 154.44 14.16 -1 -8 -12 85.89 10.63 1 8 12 84.35 12.03 -2 -8 -12 504.68 24.96 2 8 12 537.13 25.35 -3 -8 -12 5.40 5.49 3 8 12 10.51 6.59 -4 -8 -12 2.57 6.33 4 8 12 18.08 7.21 -5 -8 -12 5.39 6.38 0 -9 -12 19.23 6.65 0 9 12 22.66 9.46 -1 -9 -12 5.54 6.17 1 9 12 14.00 6.84 -2 -9 -12 29.68 6.42 -3 -9 -12 89.42 11.89 3 9 12 114.15 13.16 -4 -9 -12 2.68 6.85 0 1 -13 159.64 14.58 -1 1 -13 125.14 14.02 1 -1 13 147.53 21.59 1 0 -13 21.11 7.09 1 0 -13 15.53 8.64 -1 0 13 11.70 6.58 0 0 -13 129.46 12.53 0 0 -13 107.56 12.76 -1 0 -13 14.90 6.39 1 0 13 16.09 6.18 -2 0 -13 24.75 7.28 2 0 13 19.48 6.43 -2 1 13 103.95 13.62 1 -1 -13 248.21 16.30 -1 1 13 264.93 17.37 0 -1 -13 16.73 6.26 0 1 13 22.93 6.20 -1 -1 -13 0.00 5.59 -1 -1 -13 -0.19 5.71 1 1 13 5.27 5.84 -2 -1 -13 367.31 21.13 -2 -1 -13 405.44 20.67 -3 -1 -13 106.06 12.89 -3 -1 -13 112.76 14.03 1 -2 -13 -6.79 6.36 0 -2 -13 33.01 6.74 -1 -2 -13 17.38 6.16 -2 -2 -13 2.45 5.52 -2 -2 -13 -2.37 5.49 -2 -2 -13 4.76 5.47 -3 -2 -13 703.11 33.13 -3 -2 -13 735.73 32.10 -3 -2 -13 700.45 32.73 -4 -2 -13 105.23 14.08 -4 -2 -13 85.73 14.14 -4 -2 -13 123.53 15.04 2 -3 -13 27.06 6.68 1 -3 -13 300.74 17.97 1 -3 -13 286.10 16.99 0 -3 -13 1124.98 46.35 0 -3 -13 1013.06 44.60 -1 -3 -13 275.70 17.74 -1 -3 -13 297.79 16.92 -2 -3 -13 177.30 12.88 -2 -3 -13 161.94 14.15 -3 -3 -13 218.72 16.38 -3 -3 -13 208.83 16.04 -4 -3 -13 130.30 12.23 -4 -3 -13 99.37 13.36 -4 -3 -13 113.61 14.05 2 -4 -13 48.44 8.29 2 -4 -13 47.09 11.76 0 -4 -13 134.33 11.51 0 -4 -13 112.77 12.58 -1 -4 -13 -7.95 5.40 -1 -4 -13 12.56 5.73 -2 -4 -13 38.46 6.52 -3 -4 -13 219.37 15.74 -3 -4 -13 219.71 14.23 -4 -4 -13 156.70 14.82 1 -5 -13 172.34 14.69 1 -5 -13 196.15 15.14 -1 5 13 210.41 15.26 0 -5 -13 71.76 10.96 0 5 13 86.97 11.59 -1 -5 -13 121.14 11.18 -3 -5 -13 2.79 6.01 -4 -5 -13 331.94 20.30 1 -6 -13 4.66 6.78 1 -6 -13 0.14 6.22 -1 6 13 6.32 7.84 0 -6 -13 2.79 5.80 0 6 13 -0.81 6.87 -1 -6 -13 -0.29 5.83 -2 -6 -13 1.50 6.01 -3 -6 -13 -7.82 6.12 -4 -6 -13 68.64 12.99 0 -7 -13 20.89 6.75 0 7 13 33.16 7.92 -1 -7 -13 555.64 27.93 1 7 13 603.95 28.34 -2 -7 -13 347.93 19.76 2 7 13 343.35 19.85 -3 -7 -13 188.19 15.45 3 7 13 190.32 15.56 -4 -7 -13 6.53 6.89 1 8 13 174.21 15.68 -2 -8 -13 104.84 15.89 2 8 13 78.52 13.27 3 8 13 44.16 8.05 -1 -4 -14 288.19 18.20 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6030 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71103 7.135 10.429 10.803 73.202 82.345 75.927 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 88446 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Ni1 Ni 1.0000 0.5000 1.0000 0.00972(10) Uani 1 2 d S T P Cl1 Cl 0.88612(7) 0.31020(5) 0.97180(5) 0.01372(12) Uani 1 1 d . . . S003 S 0.70783(8) 0.64160(5) 1.20131(5) 0.01413(12) Uani 1 1 d . . . S004 S 0.04440(8) 0.98650(6) 0.27587(5) 0.01670(13) Uani 1 1 d . . . O4 O 0.7769(2) 0.51875(14) 1.14511(13) 0.0126(3) Uani 1 1 d . . . O1 O 0.5233(2) 0.87620(16) 0.43015(14) 0.0177(3) Uani 1 1 d . . . O3 O 0.0937(2) 0.84528(16) 0.37146(14) 0.0212(4) Uani 1 1 d . . . O2 O 0.2795(2) 0.8086(2) 0.56655(15) 0.0282(4) Uani 1 1 d . . . H2 H 0.2245 0.8281 0.4993 0.042 Uiso 1 1 calc GR . . N1 N 0.8172(2) 0.63262(17) 0.85787(16) 0.0112(3) Uani 1 1 d . . . C5 C 0.6250(3) 0.6404(2) 0.87369(19) 0.0136(4) Uani 1 1 d . . . H5 H 0.5727 0.5994 0.9549 0.016 Uiso 1 1 calc R . . C4 C 0.8894(3) 0.6974(2) 0.74115(19) 0.0130(4) Uani 1 1 d . . . H4 H 1.0210 0.6970 0.7301 0.016 Uiso 1 1 calc R . . C2 C 0.5794(3) 0.7668(2) 0.65321(19) 0.0122(4) Uani 1 1 d . . . C6 C 0.5017(3) 0.7063(2) 0.77543(19) 0.0136(4) Uani 1 1 d . . . H6 H 0.3693 0.7101 0.7905 0.016 Uiso 1 1 calc R . . C3 C 0.7764(3) 0.7645(2) 0.63682(19) 0.0129(4) Uani 1 1 d . . . H3 H 0.8315 0.8073 0.5573 0.015 Uiso 1 1 calc R . . C1 C 0.4583(3) 0.8249(2) 0.5383(2) 0.0142(4) Uani 1 1 d . . . C10 C -0.1416(3) 0.9762(2) 0.1876(2) 0.0189(5) Uani 1 1 d . . . H10A H -0.0978 0.9000 0.1500 0.028 Uiso 1 1 calc GR . . H10B H -0.1733 1.0594 0.1199 0.028 Uiso 1 1 calc GR . . H10C H -0.2544 0.9634 0.2450 0.028 Uiso 1 1 calc GR . . C9 C 0.2362(3) 0.9897(3) 0.1516(2) 0.0237(5) Uani 1 1 d . . . H9A H 0.3542 0.9861 0.1873 0.036 Uiso 1 1 calc GR . . H9B H 0.2058 1.0727 0.0834 0.036 Uiso 1 1 calc GR . . H9C H 0.2518 0.9121 0.1173 0.036 Uiso 1 1 calc GR . . C8 C 0.4834(3) 0.6139(2) 1.2869(2) 0.0212(5) Uani 1 1 d . . . H8A H 0.3928 0.6191 1.2264 0.032 Uiso 1 1 calc GR . . H8B H 0.4328 0.6827 1.3329 0.032 Uiso 1 1 calc GR . . H8C H 0.5038 0.5248 1.3476 0.032 Uiso 1 1 calc GR . . C7 C 0.8467(3) 0.6067(2) 1.3378(2) 0.0211(5) Uani 1 1 d . . . H7A H 0.8386 0.5181 1.3943 0.032 Uiso 1 1 calc GR . . H7B H 0.7968 0.6754 1.3840 0.032 Uiso 1 1 calc GR . . H7C H 0.9795 0.6077 1.3085 0.032 Uiso 1 1 calc GR . . 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 0.01092(19) 0.01021(18) 0.00760(17) -0.00138(13) -0.00132(13) -0.00235(14) Cl1 0.0159(3) 0.0132(2) 0.0128(2) -0.00318(18) -0.00081(18) -0.00503(18) S003 0.0158(3) 0.0133(2) 0.0131(2) -0.00439(19) -0.00063(19) -0.00187(19) S004 0.0193(3) 0.0188(3) 0.0143(2) -0.0058(2) -0.0012(2) -0.0066(2) O4 0.0139(7) 0.0130(7) 0.0113(7) -0.0052(6) 0.0010(5) -0.0022(6) O1 0.0187(8) 0.0229(8) 0.0098(7) 0.0001(6) -0.0023(6) -0.0058(6) O3 0.0208(8) 0.0268(9) 0.0138(7) 0.0025(6) -0.0057(6) -0.0082(7) O2 0.0140(8) 0.0554(12) 0.0118(7) 0.0001(8) -0.0038(6) -0.0106(8) N1 0.0125(9) 0.0103(8) 0.0109(8) -0.0027(6) -0.0018(6) -0.0023(6) C5 0.0148(10) 0.0143(10) 0.0110(9) -0.0013(8) -0.0003(8) -0.0045(8) C4 0.0122(10) 0.0124(9) 0.0136(9) -0.0020(8) -0.0004(8) -0.0033(8) C2 0.0143(10) 0.0113(9) 0.0109(9) -0.0037(7) -0.0021(7) -0.0009(8) C6 0.0118(10) 0.0174(10) 0.0118(9) -0.0039(8) -0.0005(7) -0.0036(8) C3 0.0147(10) 0.0140(10) 0.0095(9) -0.0023(7) 0.0004(7) -0.0041(8) C1 0.0136(10) 0.0145(10) 0.0143(10) -0.0044(8) -0.0021(8) -0.0012(8) C10 0.0196(11) 0.0187(11) 0.0174(10) -0.0015(9) -0.0052(8) -0.0043(9) C9 0.0216(12) 0.0299(13) 0.0170(11) -0.0009(9) -0.0009(9) -0.0073(10) C8 0.0161(11) 0.0272(12) 0.0225(11) -0.0123(10) 0.0020(9) -0.0035(9) C7 0.0225(12) 0.0272(12) 0.0173(10) -0.0099(9) -0.0026(9) -0.0070(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl1 Ni1 Cl1 180.0 2_767 . O4 Ni1 Cl1 91.74(4) . 2_767 O4 Ni1 Cl1 88.26(4) . . O4 Ni1 Cl1 91.74(4) 2_767 . O4 Ni1 Cl1 88.26(4) 2_767 2_767 O4 Ni1 O4 180.0 . 2_767 O4 Ni1 N1 90.81(6) 2_767 2_767 O4 Ni1 N1 90.81(6) . . O4 Ni1 N1 89.19(6) 2_767 . O4 Ni1 N1 89.19(6) . 2_767 N1 Ni1 Cl1 88.70(5) 2_767 2_767 N1 Ni1 Cl1 88.70(5) . . N1 Ni1 Cl1 91.30(5) . 2_767 N1 Ni1 Cl1 91.30(5) 2_767 . N1 Ni1 N1 180.00(9) . 2_767 O4 S003 C8 103.00(10) . . O4 S003 C7 106.11(10) . . C8 S003 C7 98.38(11) . . O3 S004 C10 104.46(10) . . O3 S004 C9 105.73(10) . . C10 S004 C9 99.06(11) . . S003 O4 Ni1 125.31(8) . . C1 O2 H2 109.5 . . C5 N1 Ni1 120.55(13) . . C5 N1 C4 117.55(17) . . C4 N1 Ni1 121.24(14) . . N1 C5 H5 118.4 . . N1 C5 C6 123.25(19) . . C6 C5 H5 118.4 . . N1 C4 H4 118.5 . . N1 C4 C3 122.92(19) . . C3 C4 H4 118.5 . . C6 C2 C1 121.50(19) . . C3 C2 C6 118.68(18) . . C3 C2 C1 119.68(18) . . C5 C6 C2 118.69(19) . . C5 C6 H6 120.7 . . C2 C6 H6 120.7 . . C4 C3 C2 118.77(18) . . C4 C3 H3 120.6 . . C2 C3 H3 120.6 . . O1 C1 O2 124.47(19) . . O1 C1 C2 122.82(19) . . O2 C1 C2 112.64(17) . . S004 C10 H10A 109.5 . . S004 C10 H10B 109.5 . . S004 C10 H10C 109.5 . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . S004 C9 H9A 109.5 . . S004 C9 H9B 109.5 . . S004 C9 H9C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . S003 C8 H8A 109.5 . . S003 C8 H8B 109.5 . . S003 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . S003 C7 H7A 109.5 . . S003 C7 H7B 109.5 . . S003 C7 H7C 109.5 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 Cl1 2.4231(5) . Ni1 Cl1 2.4231(5) 2_767 Ni1 O4 2.0926(14) . Ni1 O4 2.0927(14) 2_767 Ni1 N1 2.0964(17) . Ni1 N1 2.0965(17) 2_767 S003 O4 1.5193(14) . S003 C8 1.784(2) . S003 C7 1.784(2) . S004 O3 1.5251(16) . S004 C10 1.774(2) . S004 C9 1.782(2) . O1 C1 1.216(2) . O2 H2 0.8200 . O2 C1 1.313(3) . N1 C5 1.345(3) . N1 C4 1.347(3) . C5 H5 0.9300 . C5 C6 1.379(3) . C4 H4 0.9300 . C4 C3 1.385(3) . C2 C6 1.393(3) . C2 C3 1.389(3) . C2 C1 1.499(3) . C6 H6 0.9300 . C3 H3 0.9300 . C10 H10A 0.9600 . C10 H10B 0.9600 . C10 H10C 0.9600 . C9 H9A 0.9600 . C9 H9B 0.9600 . C9 H9C 0.9600 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 .