#------------------------------------------------------------------------------ #$Date: 2021-09-29 10:47:37 +0300 (Wed, 29 Sep 2021) $ #$Revision: 269364 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564742.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_1564742 loop_ _publ_author_name 'Mou, Wen-Yu' 'Li, Tao' 'Xie, Bin' 'Zhang, Dong-Liang' 'Lai, Chuan' 'Deng, Cheng-Long' 'Cao, Jia-Xi' 'Bai, Xiao-Xue' 'Liu, Xiao-Qiang' _publ_section_title ; Neutral heteroleptic nickel complexes incorporating maleonitriledithiolate and bis(diphenylphosphanyl)amine as robust molecular electrocatalysts for hydrogen evolution ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119587 _journal_paper_doi 10.1016/j.ica.2020.119587 _journal_volume 507 _journal_year 2020 _chemical_formula_sum 'C32 H29 N3 Ni O P2 S2' _chemical_formula_weight 656.35 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 101.1550(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1362(8) _cell_length_b 14.3940(12) _cell_length_c 21.3439(16) _cell_measurement_reflns_used 5766 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.277 _cell_measurement_theta_min 2.490 _cell_volume 3055.3(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15257 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.995 _diffrn_reflns_theta_min 1.717 _exptl_absorpt_coefficient_mu 0.907 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.427 _exptl_crystal_description block _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.359 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 371 _refine_ls_number_reflns 5357 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0281 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+1.6940P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.0766 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4546 _reflns_number_total 5357 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-507-119587.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564742 _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 0.854 _shelx_estimated_absorpt_t_max 0.883 _shelxl_version_number 2013-2 _shelx_res_file ; TITL cc1_a.res in P2(1)/n CELL 0.71073 10.1362 14.394 21.3439 90 101.155 90 ZERR 4 0.0008 0.0012 0.0016 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S Ni P UNIT 128 116 12 4 8 4 8 OMIT -3 50 REM Old TITL cc1 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.078, Rweak 0.003, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C32 N3 O S4 Ni REM REM REM L.S. 20 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.18 0.16 0.14 TEMP -173 WGHT 0.034600 1.694000 FVAR 0.37140 NI1 6 0.369141 0.649732 0.698907 11.00000 0.01075 0.01333 = 0.01095 0.00102 0.00096 0.00017 S2 5 0.583413 0.661490 0.708359 11.00000 0.01185 0.01992 = 0.01249 0.00193 0.00086 -0.00025 P2 7 0.320464 0.692723 0.600155 11.00000 0.01162 0.01301 = 0.01177 0.00091 0.00178 -0.00010 P1 7 0.153614 0.660931 0.674762 11.00000 0.01117 0.01266 = 0.01238 -0.00034 0.00206 -0.00040 S1 5 0.378605 0.606261 0.796361 11.00000 0.01505 0.02487 = 0.01432 0.00441 0.00319 0.00283 O1 4 -0.229522 0.751079 0.483129 11.00000 0.01453 0.02413 = 0.02262 0.00827 -0.00369 -0.00295 N1 3 0.153036 0.696912 0.599154 11.00000 0.01087 0.01759 = 0.01179 0.00031 0.00175 -0.00056 N3 3 0.890053 0.660915 0.836141 11.00000 0.01924 0.03442 = 0.02516 0.00465 -0.00191 0.00099 C6 1 -0.075261 0.753869 0.695840 11.00000 0.01849 0.01638 = 0.02294 -0.00108 0.00809 -0.00246 AFIX 43 H6 2 -0.125901 0.708079 0.669489 11.00000 -1.20000 AFIX 0 C1 1 0.064348 0.746314 0.712258 11.00000 0.01941 0.01227 = 0.01311 0.00291 0.00678 0.00045 C32 1 0.639116 0.633171 0.788375 11.00000 0.01598 0.01357 = 0.01449 -0.00066 0.00041 0.00428 C13 1 0.387144 0.805583 0.587338 11.00000 0.01732 0.01525 = 0.00992 0.00070 -0.00266 -0.00231 C7 1 0.064910 0.552296 0.673553 11.00000 0.01002 0.01306 = 0.02052 -0.00086 0.00102 -0.00031 C30 1 0.550962 0.607088 0.825908 11.00000 0.01665 0.01602 = 0.01347 -0.00021 -0.00104 0.00628 C31 1 0.779344 0.645954 0.814924 11.00000 0.02201 0.01888 = 0.01458 0.00272 0.00314 0.00577 C12 1 0.066410 0.488088 0.624771 11.00000 0.01862 0.02106 = 0.01786 -0.00068 0.00221 -0.00064 AFIX 43 H12 2 0.096421 0.506370 0.587112 11.00000 -1.20000 AFIX 0 C2 1 0.137530 0.812483 0.752070 11.00000 0.02290 0.01722 = 0.01890 -0.00023 0.00266 -0.00146 AFIX 43 H2 2 0.232595 0.807523 0.763635 11.00000 -1.20000 AFIX 0 C26 1 -0.017835 0.808800 0.539369 11.00000 0.01908 0.01821 = 0.01823 0.00316 -0.00044 -0.00046 AFIX 23 H26A 2 -0.054868 0.823626 0.577843 11.00000 -1.20000 H26B 2 0.055022 0.853676 0.536942 11.00000 -1.20000 AFIX 0 N2 3 0.638293 0.553218 0.942038 11.00000 0.03701 0.06315 = 0.01902 0.00858 0.00489 0.02166 C8 1 0.018843 0.525000 0.728323 11.00000 0.01982 0.02059 = 0.01874 -0.00131 0.00381 -0.00408 AFIX 43 H8 2 0.016551 0.568472 0.761586 11.00000 -1.20000 AFIX 0 C25 1 0.039471 0.710921 0.545210 11.00000 0.01505 0.02233 = 0.01356 -0.00115 -0.00130 0.00124 AFIX 23 H25A 2 -0.033297 0.667093 0.549851 11.00000 -1.20000 H25B 2 0.069664 0.695165 0.505082 11.00000 -1.20000 AFIX 0 C14 1 0.325931 0.886176 0.604136 11.00000 0.01854 0.02020 = 0.01380 -0.00040 -0.00330 0.00017 AFIX 43 H14 2 0.242852 0.882539 0.618336 11.00000 -1.20000 AFIX 0 C5 1 -0.140006 0.828176 0.717981 11.00000 0.02194 0.02189 = 0.03192 0.00621 0.01259 0.00517 AFIX 43 H5 2 -0.234922 0.834022 0.706137 11.00000 -1.20000 AFIX 0 C18 1 0.512293 0.811092 0.568994 11.00000 0.01891 0.02243 = 0.01663 0.00056 0.00193 -0.00279 AFIX 43 H18 2 0.555826 0.756218 0.558846 11.00000 -1.20000 AFIX 0 C27 1 -0.127564 0.818549 0.480570 11.00000 0.01607 0.01979 = 0.02025 0.00421 -0.00070 -0.00276 AFIX 23 H27A 2 -0.166575 0.881765 0.478863 11.00000 -1.20000 H27B 2 -0.089582 0.809021 0.441670 11.00000 -1.20000 AFIX 0 C20 1 0.333774 0.526429 0.535597 11.00000 0.01850 0.01733 = 0.01974 0.00252 0.00536 0.00339 AFIX 43 H20 2 0.337913 0.497650 0.575986 11.00000 -1.20000 AFIX 0 C9 1 -0.023626 0.434183 0.734093 11.00000 0.02265 0.02537 = 0.02664 0.00787 0.00035 -0.00723 AFIX 43 H9 2 -0.055405 0.415634 0.771240 11.00000 -1.20000 AFIX 0 C19 1 0.336866 0.623363 0.531146 11.00000 0.00888 0.01744 = 0.01577 -0.00136 0.00238 -0.00021 C15 1 0.386863 0.971667 0.600021 11.00000 0.03567 0.01505 = 0.01983 -0.00094 -0.00345 0.00006 AFIX 43 H15 2 0.344615 1.026789 0.610689 11.00000 -1.20000 AFIX 0 C24 1 0.334529 0.664801 0.471826 11.00000 0.01568 0.01765 = 0.01767 -0.00042 0.00340 0.00017 AFIX 43 H24 2 0.336619 0.730557 0.468323 11.00000 -1.20000 AFIX 0 C21 1 0.324684 0.472271 0.481198 11.00000 0.01980 0.01651 = 0.03134 -0.00372 0.00659 0.00208 AFIX 43 H21 2 0.319941 0.406545 0.484152 11.00000 -1.20000 AFIX 0 C29 1 0.599084 0.578116 0.890789 11.00000 0.02043 0.03141 = 0.02083 0.00125 0.00636 0.00850 C11 1 0.024216 0.397770 0.631185 11.00000 0.02920 0.01736 = 0.02705 -0.00688 -0.00629 0.00035 AFIX 43 H11 2 0.025449 0.354179 0.597884 11.00000 -1.20000 AFIX 0 C23 1 0.329140 0.609742 0.417847 11.00000 0.02071 0.02863 = 0.01441 -0.00058 0.00444 0.00039 AFIX 43 H23 2 0.330007 0.637903 0.377675 11.00000 -1.20000 AFIX 0 C10 1 -0.019697 0.370666 0.685773 11.00000 0.02854 0.01461 = 0.03480 0.00574 -0.00568 -0.00623 AFIX 43 H10 2 -0.047258 0.308313 0.690167 11.00000 -1.20000 AFIX 0 C17 1 0.572413 0.897131 0.565714 11.00000 0.02638 0.03255 = 0.01825 0.00096 0.00302 -0.01297 AFIX 43 H17 2 0.657349 0.901137 0.553327 11.00000 -1.20000 AFIX 0 C4 1 -0.066538 0.893832 0.757310 11.00000 0.04114 0.01437 = 0.02388 0.00423 0.01793 0.00729 AFIX 43 H4 2 -0.111088 0.944831 0.772384 11.00000 -1.20000 AFIX 0 C16 1 0.509182 0.976846 0.580390 11.00000 0.03977 0.02014 = 0.01722 0.00173 -0.00374 -0.01436 AFIX 43 H16 2 0.549767 1.035657 0.577014 11.00000 -1.20000 AFIX 0 C22 1 0.322520 0.514089 0.422512 11.00000 0.01999 0.02768 = 0.02376 -0.00983 0.00483 0.00083 AFIX 43 H22 2 0.316461 0.476862 0.385311 11.00000 -1.20000 AFIX 0 C3 1 0.071474 0.885520 0.774767 11.00000 0.04126 0.01709 = 0.01978 -0.00307 0.00401 -0.00228 AFIX 43 H3 2 0.121260 0.930177 0.802493 11.00000 -1.20000 AFIX 0 C28 1 -0.334256 0.757604 0.428713 11.00000 0.01974 0.03474 = 0.02773 0.00504 -0.00738 -0.00774 AFIX 137 H28A 2 -0.295909 0.755662 0.389960 11.00000 -1.50000 H28B 2 -0.382798 0.816218 0.430093 11.00000 -1.50000 H28C 2 -0.396499 0.705443 0.428449 11.00000 -1.50000 AFIX 0 HKLF 4 REM cc1_a.res in P2(1)/n REM R1 = 0.0281 for 4546 Fo > 4sig(Fo) and 0.0371 for all 5357 data REM 371 parameters refined using 0 restraints END WGHT 0.0344 1.7285 REM Highest difference peak 0.359, deepest hole -0.321, 1-sigma level 0.066 Q1 1 0.0970 0.5995 0.6686 11.00000 0.05 0.36 Q2 1 0.1027 0.7168 0.6918 11.00000 0.05 0.33 Q3 1 0.3547 0.7528 0.5881 11.00000 0.05 0.29 Q4 1 0.3221 0.6576 0.5591 11.00000 0.05 0.29 Q5 1 -0.0689 0.8158 0.5106 11.00000 0.05 0.28 Q6 1 0.6698 0.6001 0.9467 11.00000 0.05 0.28 Q7 1 -0.0106 0.7613 0.5497 11.00000 0.05 0.27 Q8 1 0.2236 0.6941 0.5962 11.00000 0.05 0.26 Q9 1 0.3420 0.8366 0.5822 11.00000 0.05 0.25 Q10 1 0.5569 0.9362 0.5914 11.00000 0.05 0.25 Q11 1 0.6173 0.6486 0.7569 11.00000 0.05 0.24 Q12 1 0.0015 0.7637 0.6879 11.00000 0.05 0.24 Q13 1 0.5577 0.8542 0.5828 11.00000 0.05 0.24 Q14 1 0.7023 0.6097 0.7991 11.00000 0.05 0.23 Q15 1 0.4551 0.8107 0.5869 11.00000 0.05 0.23 Q16 1 0.0966 0.7846 0.7151 11.00000 0.05 0.23 Q17 1 -0.0863 0.9220 0.5806 11.00000 0.05 0.23 Q18 1 0.5155 0.9376 0.5540 11.00000 0.05 0.22 Q19 1 -0.1536 0.9663 0.7376 11.00000 0.05 0.22 Q20 1 0.8336 0.6591 0.8533 11.00000 0.05 0.22 ; _shelx_res_checksum 58757 _shelx_hkl_file ; -1 0 0 -1.90 0.30 -2 0 0 1358.16 22.50 2 0 0 1348.97 23.10 3 0 0 0.70 2.30 -3 0 0 0.20 1.70 -4 0 0 9720.53 144.89 4 0 0 9999.00 146.69 -5 0 0 7.50 2.70 6 0 0 1089.09 26.50 -6 0 0 1094.79 24.40 7 0 0 4.90 5.30 -7 0 0 -1.10 3.00 8 0 0 253.47 15.40 -8 0 0 224.28 11.50 9 0 0 0.90 6.70 -9 0 0 -1.90 3.60 -10 0 0 219.08 13.10 10 0 0 217.68 17.40 -11 0 0 0.70 4.60 -12 0 0 18.20 6.40 0 -1 0 -3.90 0.20 -1 -1 0 235.48 5.00 -1 1 0 204.68 4.70 -2 -1 0 1117.89 19.40 2 1 0 1147.29 21.10 -2 1 0 1122.09 19.20 -3 -1 0 7608.94 111.49 3 -1 0 7614.44 111.19 3 1 0 7467.85 113.69 -3 1 0 7601.64 111.29 4 -1 0 1730.13 31.20 -4 -1 0 1751.92 31.30 -4 1 0 1783.22 31.30 4 1 0 1772.32 34.00 -5 -1 0 686.53 16.80 5 -1 0 689.93 17.40 5 1 0 684.73 19.20 -5 1 0 692.53 16.80 -6 -1 0 543.25 15.70 6 -1 0 547.45 16.80 6 1 0 552.94 18.80 -6 1 0 541.75 15.60 -7 -1 0 137.19 8.70 7 -1 0 150.48 10.80 -7 1 0 134.79 8.60 7 1 0 147.49 11.50 -8 -1 0 16.00 4.80 8 -1 0 12.20 6.40 8 1 0 4.40 6.80 -8 1 0 20.00 4.90 9 -1 0 -2.40 6.10 -9 -1 0 9.10 4.50 -9 1 0 0.40 3.70 9 1 0 13.20 7.80 -10 -1 0 433.66 18.10 -10 1 0 402.66 17.60 10 1 0 356.66 20.90 -11 -1 0 6.30 5.00 -11 1 0 2.00 4.70 -12 -1 0 88.59 11.60 -12 1 0 74.79 10.50 0 -2 0 2538.55 38.00 -1 -2 0 3502.05 50.99 -1 2 0 3445.36 50.79 1 2 0 3317.77 52.89 -2 -2 0 477.75 10.60 2 2 0 522.75 13.40 -2 2 0 497.75 10.70 -3 -2 0 426.66 10.80 3 -2 0 434.56 10.00 -3 2 0 446.76 10.80 3 2 0 429.06 13.50 -4 -2 0 333.47 10.30 4 -2 0 340.97 9.70 -4 2 0 340.97 10.20 4 2 0 347.77 12.80 5 -2 0 2829.02 47.60 -5 -2 0 2804.02 48.20 -5 2 0 2732.53 47.70 5 2 0 2845.92 52.49 6 -2 0 0.60 3.10 -6 -2 0 2.80 2.90 -6 2 0 3.60 3.30 6 2 0 4.30 4.90 7 -2 0 235.88 11.90 -7 -2 0 233.38 11.00 -7 2 0 221.98 10.70 7 2 0 259.37 15.90 -8 -2 0 24.20 5.70 8 -2 0 15.40 5.90 8 2 0 13.60 7.30 -8 2 0 25.40 5.40 -9 -2 0 1085.09 29.10 -9 2 0 1127.99 29.20 9 2 0 1168.68 36.00 -10 -2 0 31.20 6.60 -10 2 0 35.90 6.90 10 2 0 41.70 11.40 -11 -2 0 -2.50 4.40 -11 2 0 5.40 4.90 11 2 0 -9.30 9.80 -12 -2 0 1.80 5.40 -12 2 0 11.30 6.40 0 -3 0 -5.10 1.10 1 -3 0 3790.02 56.39 -1 -3 0 3705.83 56.49 -2 -3 0 181.38 6.30 2 3 0 198.58 9.10 -2 3 0 173.18 6.10 -3 -3 0 290.77 9.10 3 3 0 305.47 11.90 -3 3 0 305.37 8.90 -4 -3 0 325.37 10.40 4 -3 0 316.57 9.10 4 3 0 313.17 13.20 -4 3 0 342.77 10.50 -5 -3 0 1057.29 23.40 5 -3 0 1078.69 22.20 5 3 0 1096.29 28.00 -5 3 0 1071.09 23.20 6 -3 0 438.66 13.70 -6 -3 0 428.36 14.40 -6 3 0 438.16 14.20 6 3 0 429.46 18.20 -7 -3 0 12.90 4.50 7 -3 0 10.90 4.50 -7 3 0 29.70 5.40 7 3 0 11.80 7.30 8 -3 0 81.49 8.80 -8 -3 0 83.59 8.80 -8 3 0 74.59 8.00 8 3 0 90.39 11.80 -9 -3 0 71.59 9.00 9 3 0 62.89 11.50 -9 3 0 72.39 8.80 -10 -3 0 71.09 9.10 -10 3 0 71.09 9.00 10 3 0 60.19 13.40 -11 -3 0 9.50 6.20 -11 3 0 11.60 6.40 11 3 0 -8.70 9.30 -12 -3 0 10.50 5.90 -12 3 0 4.80 6.00 0 -4 0 4814.52 72.19 1 -4 0 1796.02 29.80 -1 -4 0 1769.02 29.90 -2 -4 0 30.20 3.40 -2 4 0 30.80 3.40 2 4 0 35.70 5.40 -3 -4 0 -0.70 1.90 -3 4 0 0.80 1.90 3 4 0 3.90 4.30 -4 -4 0 2727.03 47.50 -4 4 0 2866.31 47.60 4 4 0 2815.52 53.19 5 -4 0 1648.14 30.20 -5 -4 0 1624.14 32.50 -5 4 0 1674.13 32.30 5 4 0 1629.74 37.80 6 -4 0 14.70 3.60 -6 -4 0 18.60 4.70 -6 4 0 21.20 4.40 6 4 0 18.40 7.40 7 -4 0 397.76 14.20 -7 -4 0 405.46 15.30 -7 4 0 371.36 14.30 7 4 0 423.86 20.60 -8 -4 0 597.04 19.60 -8 4 0 569.74 19.30 8 4 0 607.04 25.90 -9 -4 0 327.87 15.30 -9 4 0 364.96 15.90 9 4 0 338.57 22.90 -10 -4 0 41.80 7.90 -10 4 0 40.20 7.80 10 4 0 38.50 12.80 -11 -4 0 22.20 7.30 -11 4 0 14.50 6.30 11 4 0 1.80 10.90 -12 -4 0 89.29 11.50 -12 4 0 84.49 11.00 12 4 0 78.49 17.60 0 -5 0 1.90 1.80 1 -5 0 680.13 14.80 -1 -5 0 674.63 14.90 -2 -5 0 1635.94 29.70 2 -5 0 1651.03 29.50 -3 -5 0 40.30 4.50 -3 5 0 43.40 4.40 3 5 0 27.20 6.00 -4 -5 0 152.88 7.70 -4 -5 0 149.99 4.60 -4 5 0 144.69 7.40 4 5 0 155.98 11.70 -5 -5 0 711.43 19.00 5 -5 0 694.93 16.40 -5 5 0 720.13 18.60 5 5 0 744.63 24.50 -6 -5 0 280.27 12.10 6 -5 0 281.67 10.50 -6 5 0 283.47 11.80 6 5 0 313.67 18.00 -7 -5 0 60.99 7.40 7 5 0 56.29 10.80 -7 5 0 77.89 8.00 -8 -5 0 177.68 11.60 -8 5 0 174.48 11.20 8 5 0 147.29 16.40 -9 -5 0 102.79 10.80 -9 5 0 87.79 9.30 9 5 0 77.79 13.60 -10 -5 0 408.86 18.20 10 5 0 367.06 26.60 -10 5 0 370.86 17.30 -11 -5 0 222.08 14.60 -11 5 0 215.28 14.10 11 5 0 188.88 21.90 -12 -5 0 12.30 6.90 -12 5 0 5.10 5.30 12 5 0 5.80 12.40 0 -6 0 3903.21 61.89 1 -6 0 29.10 3.60 -1 -6 0 34.20 3.80 -2 -6 0 142.09 6.80 2 -6 0 135.69 6.60 3 -6 0 176.88 7.90 -3 -6 0 187.78 8.30 -3 6 0 184.28 8.00 -4 -6 0 1835.72 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23.00 8.70 4 5 23 -8.80 9.00 -8 -6 23 10.10 9.20 -8 6 23 22.90 11.00 -7 -6 23 346.87 21.10 -7 6 23 335.87 22.60 -6 -6 23 -10.90 7.10 -6 6 23 6.30 9.30 -5 -6 23 5.90 8.00 -5 6 23 10.20 9.20 -4 -6 23 144.79 14.70 -4 6 23 149.29 16.50 -3 -6 23 52.99 10.50 -3 6 23 71.19 13.00 -2 -6 23 4.90 6.70 -2 6 23 17.20 10.70 -1 -6 23 282.87 18.10 -1 6 23 318.87 21.60 0 -6 23 583.64 24.70 0 6 23 536.65 25.10 1 -6 23 0.10 6.60 1 6 23 -3.80 8.50 2 -6 23 1.50 7.00 2 6 23 -4.40 7.80 3 -6 23 562.24 24.50 3 6 23 621.84 30.40 -7 -7 23 79.89 12.90 -7 7 23 79.49 15.00 -6 -7 23 -3.70 7.70 -6 7 23 -7.00 9.90 -5 -7 23 8.10 8.20 -5 7 23 25.10 10.60 -4 -7 23 3.20 7.20 -4 7 23 -9.10 7.80 -3 -7 23 223.48 17.70 -3 7 23 224.18 19.70 -2 -7 23 11.20 7.30 -2 7 23 -8.10 8.60 -1 -7 23 19.20 7.80 -1 7 23 17.20 9.40 0 -7 23 45.90 9.70 0 7 23 61.99 12.60 1 -7 23 6.30 6.90 1 7 23 21.60 10.00 2 -7 23 12.50 7.20 3 -7 23 31.50 8.80 3 7 23 22.40 11.70 -6 -8 23 346.57 21.10 -6 8 23 362.96 23.50 -5 -8 23 -11.00 6.90 -5 8 23 9.10 10.80 -4 -8 23 145.09 15.30 -4 8 23 170.58 18.60 -3 -8 23 24.70 8.90 -3 8 23 42.80 11.60 -2 -8 23 255.97 17.60 -2 8 23 253.67 19.60 -1 -8 23 44.70 10.00 -1 8 23 53.39 11.60 0 -8 23 32.40 9.80 0 8 23 38.30 10.90 1 -8 23 122.39 14.10 1 8 23 88.19 14.20 2 -8 23 203.28 17.90 -5 -9 23 -12.50 6.30 -5 9 23 -3.70 8.90 -4 -9 23 -1.60 7.80 -4 9 23 16.00 10.10 -3 -9 23 -5.40 7.00 -3 9 23 5.00 9.20 -2 -9 23 16.80 8.30 -2 9 23 12.10 9.40 -1 -9 23 55.29 11.20 -1 9 23 51.49 12.30 0 -9 23 10.00 7.60 0 9 23 26.10 10.50 1 -9 23 23.40 9.10 -4 -10 23 1.00 7.10 -4 10 23 18.90 10.80 -3 -10 23 147.69 15.50 -3 10 23 165.38 18.30 -2 -10 23 217.38 19.10 -2 10 23 306.57 22.10 -1 -10 23 -3.60 7.20 -1 10 23 1.60 9.30 0 -10 23 11.20 8.00 0 10 23 21.80 10.00 -8 0 24 175.38 18.50 -7 0 24 -12.50 7.50 -6 0 24 404.06 22.70 -5 0 24 -1.30 8.50 -4 0 24 252.27 19.50 -3 0 24 3.30 7.70 -2 0 24 527.55 25.00 -1 0 24 2.90 7.40 0 0 24 108.49 12.40 0 0 24 115.19 14.60 1 0 24 -5.30 7.40 1 0 24 0.40 5.80 2 0 24 -11.20 7.60 2 0 24 4.70 6.70 3 0 24 2.70 12.00 3 0 24 1.90 7.20 4 0 24 56.69 12.10 -8 -1 24 45.40 12.80 -8 1 24 24.90 11.40 -7 -1 24 15.90 9.20 -7 1 24 26.80 10.60 -6 -1 24 5.40 8.10 -6 1 24 -4.40 7.90 -5 -1 24 29.90 10.70 -5 1 24 38.60 10.70 -4 -1 24 -0.90 7.30 -4 1 24 -6.10 7.60 -3 -1 24 -4.30 8.10 -3 1 24 2.90 7.70 -2 -1 24 110.69 13.50 -2 1 24 136.09 15.10 -1 -1 24 27.10 9.00 -1 1 24 19.80 6.40 -1 1 24 11.90 9.30 0 -1 24 -0.90 7.10 0 1 24 19.60 8.10 0 1 24 12.00 9.10 1 -1 24 59.99 10.60 1 -1 24 55.49 10.60 1 1 24 52.09 10.20 1 1 24 70.19 12.00 2 -1 24 2.00 8.20 2 -1 24 -6.80 5.60 2 1 24 -1.20 6.40 2 1 24 1.70 8.50 3 -1 24 -8.00 6.00 3 -1 24 -2.80 6.90 3 1 24 1.30 7.30 4 -1 24 16.60 9.30 4 1 24 23.90 9.70 -8 -2 24 20.50 10.10 -8 2 24 24.60 10.90 -7 -2 24 176.28 17.80 -7 2 24 186.38 18.50 -6 -2 24 107.19 14.00 -6 2 24 105.19 15.00 -5 -2 24 -5.50 7.80 -5 2 24 -8.20 7.40 -4 -2 24 -6.90 6.80 -4 2 24 7.60 9.80 -3 -2 24 55.89 11.10 -3 2 24 37.30 10.80 -2 -2 24 230.78 17.00 -2 2 24 260.27 18.80 -1 -2 24 78.59 12.00 -1 2 24 61.79 12.30 0 -2 24 -0.50 7.70 0 2 24 -10.70 8.00 0 2 24 6.40 6.20 1 -2 24 112.59 13.90 1 2 24 100.39 12.30 1 2 24 81.29 12.40 2 -2 24 -10.50 6.40 2 -2 24 -6.00 5.30 2 2 24 -2.10 7.50 2 2 24 9.10 7.90 3 -2 24 228.18 17.80 3 -2 24 229.38 18.60 3 2 24 227.38 19.00 4 -2 24 8.20 8.10 4 2 24 10.10 9.20 -8 -3 24 -15.70 8.70 -8 3 24 1.10 9.00 -7 -3 24 231.38 19.80 -7 3 24 222.38 20.00 -6 -3 24 52.19 11.90 -6 3 24 52.99 12.30 -5 -3 24 55.79 12.00 -5 3 24 43.40 11.90 -4 -3 24 11.30 7.90 -4 3 24 19.70 10.20 -3 -3 24 75.59 11.90 -3 3 24 53.99 12.60 -2 -3 24 168.48 15.80 -2 3 24 180.98 17.10 -1 -3 24 24.90 8.90 -1 3 24 23.70 10.60 0 -3 24 21.00 9.30 0 3 24 30.40 13.20 0 3 24 1.70 9.60 1 -3 24 111.29 13.70 1 3 24 114.79 14.10 1 3 24 98.69 13.10 2 -3 24 82.09 11.90 2 3 24 67.99 12.40 2 3 24 76.09 12.90 3 -3 24 0.00 6.90 3 -3 24 -3.70 7.30 3 3 24 -6.30 8.10 -8 -4 24 168.68 17.00 -8 4 24 164.18 18.00 -7 -4 24 32.90 10.20 -7 4 24 37.70 12.50 -6 -4 24 90.79 13.70 -6 4 24 84.99 13.80 -5 -4 24 401.26 21.50 -5 4 24 418.86 23.80 -4 -4 24 402.16 22.30 -4 4 24 416.06 24.60 -3 -4 24 3.90 8.30 -3 4 24 0.50 9.50 -2 -4 24 21.50 8.60 -2 4 24 2.40 8.60 -1 -4 24 453.15 22.40 -1 4 24 463.85 25.00 0 -4 24 122.59 14.70 0 4 24 90.69 14.00 1 -4 24 63.99 12.00 1 4 24 79.69 13.60 1 4 24 58.29 11.30 2 -4 24 35.70 9.60 2 4 24 41.00 16.80 2 4 24 52.69 11.50 3 -4 24 272.57 18.20 3 4 24 239.48 19.70 -7 -5 24 61.99 12.50 -7 5 24 68.79 14.20 -6 -5 24 13.90 9.10 -6 5 24 10.70 10.60 -5 -5 24 30.70 10.80 -5 5 24 29.50 11.60 -4 -5 24 78.49 12.30 -4 5 24 68.49 13.20 -3 -5 24 291.77 18.80 -3 5 24 267.37 20.00 -2 -5 24 187.88 17.30 -2 5 24 144.59 16.40 -1 -5 24 88.79 12.90 -1 5 24 87.49 14.00 0 -5 24 65.99 11.60 0 5 24 47.40 11.60 1 -5 24 22.80 9.10 1 5 24 24.50 9.90 2 -5 24 5.20 7.60 2 5 24 0.30 8.60 3 -5 24 -4.10 7.70 3 5 24 4.70 8.50 -7 -6 24 27.50 10.50 -7 6 24 33.30 11.80 -6 -6 24 486.55 23.90 -6 6 24 469.45 26.00 -5 -6 24 106.79 13.60 -5 6 24 90.49 14.70 -4 -6 24 56.99 11.60 -4 6 24 55.09 12.10 -3 -6 24 49.80 11.20 -3 6 24 51.79 12.00 -2 -6 24 203.58 17.80 -2 6 24 247.18 20.60 -1 -6 24 28.00 9.20 -1 6 24 25.90 10.60 0 -6 24 51.79 11.20 0 6 24 50.09 12.70 1 -6 24 81.59 12.70 1 6 24 97.89 14.70 2 -6 24 35.30 9.50 -6 -7 24 68.19 12.00 -6 7 24 84.89 15.00 -5 -7 24 65.69 11.50 -5 7 24 60.29 14.00 -4 -7 24 -1.80 7.80 -4 7 24 9.30 10.30 -3 -7 24 -13.70 7.40 -3 7 24 12.80 9.60 -2 -7 24 178.78 16.80 -2 7 24 198.98 19.20 -1 -7 24 160.88 16.30 -1 7 24 174.88 17.40 0 7 24 47.00 12.40 1 -7 24 -10.30 6.90 1 7 24 2.20 8.20 2 -7 24 51.29 10.50 -5 -8 24 8.20 9.10 -5 8 24 5.30 9.30 -4 -8 24 151.98 16.50 -4 8 24 185.38 19.10 -3 -8 24 30.00 9.90 -3 8 24 53.29 13.00 -2 -8 24 -1.50 7.80 -2 8 24 -0.30 9.50 -1 -8 24 149.09 16.20 -1 8 24 156.58 16.90 0 -8 24 42.90 10.20 0 8 24 38.30 10.80 1 -8 24 134.99 15.10 -4 -9 24 14.90 9.80 -4 9 24 14.50 10.40 -3 -9 24 295.87 20.90 -3 9 24 307.57 23.30 -2 -9 24 4.80 7.50 -2 9 24 2.40 10.10 -1 -9 24 -2.00 6.80 -1 9 24 -6.20 7.90 -7 0 25 205.08 19.90 -6 0 25 -3.20 9.30 -5 0 25 82.79 14.30 -4 0 25 -15.00 8.30 -3 0 25 123.29 14.70 -2 0 25 5.30 8.40 -1 0 25 43.80 10.60 0 0 25 -2.30 7.60 0 0 25 4.60 6.70 1 0 25 145.19 15.10 1 0 25 159.28 16.70 2 0 25 -11.80 8.00 2 0 25 0.80 6.50 3 0 25 105.79 14.40 -7 -1 25 375.56 24.10 -7 1 25 392.96 24.80 -6 -1 25 -14.90 7.40 -6 1 25 -0.10 9.70 -5 -1 25 13.70 9.00 -5 1 25 21.10 10.70 -4 -1 25 -0.60 7.90 -4 1 25 -6.90 9.00 -3 -1 25 14.00 9.70 -3 1 25 1.70 8.40 -2 -1 25 50.69 11.80 -2 1 25 82.69 13.20 -1 -1 25 -1.20 7.80 -1 1 25 -6.60 8.40 0 -1 25 35.20 10.80 0 1 25 35.00 8.50 0 1 25 24.40 10.50 1 -1 25 23.10 9.00 1 -1 25 10.90 6.80 1 1 25 33.00 9.50 1 1 25 8.10 8.40 2 -1 25 76.29 12.80 2 -1 25 68.99 11.60 2 1 25 64.99 12.00 2 1 25 55.59 12.10 3 -1 25 4.20 8.70 3 -1 25 11.60 8.90 3 1 25 -0.30 7.00 -7 -2 25 -9.80 7.90 -7 2 25 -1.20 10.10 -6 -2 25 99.99 14.20 -6 2 25 111.59 15.10 -5 -2 25 80.19 13.40 -5 2 25 61.69 12.80 -4 -2 25 159.38 16.30 -4 2 25 154.88 16.80 -3 -2 25 11.70 9.10 -3 2 25 -5.30 8.40 -2 -2 25 218.28 18.60 -2 2 25 190.08 17.80 -1 -2 25 -8.40 7.50 -1 2 25 3.80 9.20 0 -2 25 188.98 17.50 0 2 25 222.98 16.50 0 2 25 201.38 18.70 1 -2 25 7.30 9.20 1 2 25 27.40 8.80 1 2 25 1.10 8.00 2 -2 25 13.40 7.90 2 -2 25 -3.40 8.40 2 2 25 -5.10 9.20 2 2 25 10.60 8.60 3 -2 25 57.89 11.80 3 -2 25 58.59 11.80 3 2 25 38.70 10.40 -7 -3 25 83.19 14.40 -7 3 25 75.79 15.00 -6 -3 25 40.20 11.70 -6 3 25 38.00 11.80 -5 -3 25 6.90 8.40 -5 3 25 -2.20 8.90 -4 -3 25 -5.20 8.20 -4 3 25 -2.20 10.00 -3 -3 25 4.90 8.00 -3 3 25 2.40 8.70 -2 -3 25 250.97 19.40 -2 3 25 270.87 21.30 -1 -3 25 11.40 9.30 -1 3 25 -2.70 8.80 0 -3 25 -9.50 7.70 0 3 25 -9.60 8.70 1 -3 25 -9.10 7.50 1 3 25 -0.90 9.40 1 3 25 5.40 7.50 2 -3 25 45.30 10.50 2 3 25 44.10 11.30 2 3 25 63.49 14.00 -7 -4 25 26.50 9.90 -7 4 25 38.80 13.10 -6 -4 25 228.38 18.30 -6 4 25 227.78 20.70 -5 -4 25 10.10 8.20 -5 4 25 -0.80 9.50 -4 -4 25 -6.00 7.00 -4 4 25 -1.40 8.90 -3 -4 25 -2.60 7.20 -3 4 25 1.20 9.10 -2 -4 25 53.29 11.10 -2 4 25 71.49 14.20 -1 -4 25 97.99 13.20 -1 4 25 97.19 14.30 0 -4 25 35.30 10.70 0 4 25 39.10 12.10 1 -4 25 26.80 10.00 1 4 25 35.30 11.90 2 -4 25 -3.20 7.20 2 4 25 5.90 7.90 -6 -5 25 240.78 20.50 -6 5 25 258.87 22.70 -5 -5 25 124.79 15.00 -5 5 25 119.69 16.10 -4 -5 25 1.80 8.70 -4 5 25 10.20 10.90 -3 -5 25 287.47 19.10 -3 5 25 246.28 21.50 -2 -5 25 61.69 12.10 -2 5 25 61.89 12.70 -1 -5 25 18.00 9.80 -1 5 25 13.90 9.80 0 -5 25 37.40 10.10 0 5 25 28.10 11.80 1 -5 25 2.20 7.70 1 5 25 2.20 9.50 2 -5 25 -12.80 7.90 2 5 25 -6.90 7.10 -6 -6 25 0.20 8.80 -6 6 25 -9.80 9.70 -5 -6 25 13.30 9.10 -5 6 25 13.60 10.20 -4 -6 25 142.29 16.30 -4 6 25 150.38 17.30 -3 -6 25 1.50 8.10 -3 6 25 6.90 9.20 -2 -6 25 34.20 10.10 -2 6 25 27.60 11.00 -1 -6 25 113.99 14.30 -1 6 25 166.98 17.60 0 -6 25 22.00 9.30 0 6 25 19.00 11.00 1 -6 25 121.89 14.80 1 6 25 122.59 15.30 -5 -7 25 16.70 8.80 -5 7 25 31.30 12.60 -4 -7 25 148.09 16.90 -4 7 25 159.78 18.70 -3 -7 25 50.19 11.90 -3 7 25 74.39 14.00 -2 -7 25 13.70 9.50 -2 7 25 26.70 11.20 -1 -7 25 10.40 9.40 -1 7 25 11.30 9.90 0 -7 25 161.28 16.80 0 7 25 176.78 18.00 -3 -8 25 3.00 8.10 -3 8 25 -7.90 9.90 -2 -8 25 348.37 22.70 -2 8 25 359.76 24.70 -6 0 26 61.59 14.10 -5 0 26 -12.30 8.20 -4 0 26 267.47 21.70 -3 0 26 -4.20 8.30 -2 0 26 99.39 13.90 -1 0 26 10.90 9.50 -1 0 26 8.00 6.50 0 0 26 257.47 18.00 0 0 26 241.48 20.40 1 0 26 -14.60 7.00 1 0 26 -1.50 6.90 2 0 26 19.10 8.90 2 0 26 -12.90 7.10 -6 -1 26 208.38 20.40 -6 1 26 230.98 21.00 -5 -1 26 -12.40 7.50 -5 1 26 -2.60 9.00 -4 -1 26 -10.00 8.80 -4 1 26 2.30 10.40 -3 -1 26 3.30 8.80 -3 1 26 13.20 9.90 -2 -1 26 264.67 19.40 -2 1 26 300.97 21.90 -1 -1 26 11.80 10.00 -1 1 26 -1.20 8.40 0 -1 26 18.00 7.60 0 -1 26 -4.70 7.50 0 1 26 -3.80 8.20 0 1 26 6.60 7.20 1 -1 26 22.90 8.30 1 -1 26 9.80 9.50 1 1 26 26.10 8.70 1 1 26 30.40 11.30 2 -1 26 54.69 12.40 2 -1 26 74.39 12.30 2 1 26 68.39 12.60 2 1 26 49.20 12.60 -6 -2 26 -5.00 8.50 -6 2 26 8.10 9.80 -5 -2 26 -7.90 9.10 -5 2 26 5.50 9.90 -4 -2 26 -9.10 8.40 -4 2 26 -11.80 8.30 -3 -2 26 33.90 10.80 -3 2 26 50.19 12.80 -2 -2 26 13.50 8.80 -2 2 26 -7.50 8.50 -1 -2 26 61.29 12.40 -1 2 26 45.20 12.90 0 -2 26 98.39 13.60 0 2 26 85.79 14.70 1 -2 26 34.30 9.20 1 -2 26 33.50 11.20 1 2 26 31.60 10.10 1 2 26 40.20 12.60 -6 -3 26 -4.30 9.30 -6 3 26 2.40 9.20 -5 -3 26 49.50 11.80 -5 3 26 52.29 14.20 -4 -3 26 30.00 10.60 -4 3 26 20.90 10.40 -3 -3 26 -14.90 8.20 -3 3 26 -6.90 8.90 -2 -3 26 14.50 8.80 -2 3 26 11.00 11.20 -1 -3 26 -3.50 8.70 -1 3 26 4.10 9.10 0 -3 26 10.70 8.50 0 3 26 27.50 11.50 1 -3 26 2.00 8.90 1 3 26 -1.70 9.70 1 3 26 4.10 8.20 -5 -4 26 22.10 11.00 -5 4 26 -0.30 10.70 -4 -4 26 21.80 10.80 -4 4 26 25.90 12.40 -3 -4 26 3.30 8.50 -3 4 26 20.10 11.60 -2 -4 26 28.20 10.90 -2 4 26 4.50 9.30 -1 -4 26 0.10 7.70 -1 4 26 11.70 10.00 0 -4 26 17.60 10.10 0 4 26 21.70 11.70 1 -4 26 92.09 13.50 1 4 26 116.59 16.20 -5 -5 26 14.80 10.60 -5 5 26 30.80 11.60 -4 -5 26 35.20 10.80 -4 5 26 17.20 10.80 -3 -5 26 46.90 12.10 -3 5 26 45.50 12.50 -2 -5 26 147.79 16.80 -2 5 26 157.58 18.60 -1 -5 26 8.80 9.00 -1 5 26 12.00 11.10 0 -5 26 93.99 13.60 0 5 26 87.59 15.40 -4 -6 26 236.08 20.20 -4 6 26 172.98 19.10 -3 -6 26 15.50 9.90 -3 6 26 8.50 11.20 -2 -6 26 45.50 11.10 -2 6 26 68.49 14.60 -1 -6 26 44.50 12.00 -1 6 26 59.89 14.10 -5 0 27 0.10 9.40 -4 0 27 -15.80 9.50 -3 0 27 158.88 17.50 -2 0 27 -23.40 8.60 -1 0 27 4.20 9.20 0 0 27 -3.20 8.50 0 0 27 9.80 7.70 -5 -1 27 -12.50 9.20 -5 1 27 -3.20 9.50 -4 -1 27 6.20 10.30 -4 1 27 13.90 11.60 -3 -1 27 96.89 14.40 -3 1 27 93.19 14.60 -2 -1 27 174.38 18.70 -2 1 27 135.09 17.30 -1 -1 27 8.10 9.40 -1 1 27 -8.10 8.30 0 -1 27 10.00 7.80 0 -1 27 -4.00 8.40 0 1 27 6.40 7.00 0 1 27 -0.80 9.80 -5 -2 27 -3.80 8.70 -5 2 27 -8.60 9.10 -4 -2 27 3.60 9.20 -4 2 27 3.00 10.60 -3 -2 27 4.80 10.10 -3 2 27 -0.40 10.50 -2 -2 27 5.70 9.60 -2 2 27 23.90 11.40 -1 -2 27 7.40 8.80 -1 2 27 10.20 11.10 0 -2 27 44.80 11.40 0 2 27 59.79 13.00 -4 -3 27 0.60 10.00 -4 3 27 33.20 12.90 -3 -3 27 14.90 9.60 -3 3 27 -4.10 9.30 -2 -3 27 137.69 16.00 -2 3 27 131.79 16.70 -1 -3 27 16.50 10.20 -1 3 27 9.40 10.10 -3 -4 27 103.59 15.20 -3 4 27 66.69 14.20 -2 -4 27 -7.10 9.10 -2 4 27 7.80 10.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 92841 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 0.36914(3) 0.64973(2) 0.69891(2) 0.01183(9) Uani 1 1 d . . . . . S2 S 0.58341(5) 0.66149(4) 0.70836(3) 0.01495(13) Uani 1 1 d . . . . . P2 P 0.32046(6) 0.69272(4) 0.60016(3) 0.01220(13) Uani 1 1 d . . . . . P1 P 0.15361(6) 0.66093(4) 0.67476(3) 0.01210(13) Uani 1 1 d . . . . . S1 S 0.37860(6) 0.60626(4) 0.79636(3) 0.01803(14) Uani 1 1 d . . . . . O1 O -0.22952(15) 0.75108(12) 0.48313(8) 0.0214(4) Uani 1 1 d . . . . . N1 N 0.15304(18) 0.69691(13) 0.59915(8) 0.0135(4) Uani 1 1 d . . . . . N3 N 0.8901(2) 0.66091(16) 0.83614(10) 0.0271(5) Uani 1 1 d . . . . . C6 C -0.0753(2) 0.75387(16) 0.69584(11) 0.0187(5) Uani 1 1 d . . . . . H6 H -0.1259 0.7081 0.6695 0.022 Uiso 1 1 calc R U . . . C1 C 0.0643(2) 0.74631(15) 0.71226(10) 0.0144(5) Uani 1 1 d . . . . . C32 C 0.6391(2) 0.63317(15) 0.78838(11) 0.0150(5) Uani 1 1 d . . . . . C13 C 0.3871(2) 0.80558(16) 0.58734(10) 0.0149(5) Uani 1 1 d . . . . . C7 C 0.0649(2) 0.55230(15) 0.67355(11) 0.0148(5) Uani 1 1 d . . . . . C30 C 0.5510(2) 0.60709(16) 0.82591(11) 0.0159(5) Uani 1 1 d . . . . . C31 C 0.7793(2) 0.64595(16) 0.81492(11) 0.0185(5) Uani 1 1 d . . . . . C12 C 0.0664(2) 0.48809(17) 0.62477(11) 0.0194(5) Uani 1 1 d . . . . . H12 H 0.0964 0.5064 0.5871 0.023 Uiso 1 1 calc R U . . . C2 C 0.1375(2) 0.81248(16) 0.75207(11) 0.0199(5) Uani 1 1 d . . . . . H2 H 0.2326 0.8075 0.7636 0.024 Uiso 1 1 calc R U . . . C26 C -0.0178(2) 0.80880(16) 0.53937(11) 0.0190(5) Uani 1 1 d . . . . . H26A H -0.0549 0.8236 0.5778 0.023 Uiso 1 1 calc R U . . . H26B H 0.0550 0.8537 0.5369 0.023 Uiso 1 1 calc R U . . . N2 N 0.6383(2) 0.55322(19) 0.94204(11) 0.0398(6) Uani 1 1 d . . . . . C8 C 0.0188(2) 0.52500(17) 0.72832(11) 0.0197(5) Uani 1 1 d . . . . . H8 H 0.0166 0.5685 0.7616 0.024 Uiso 1 1 calc R U . . . C25 C 0.0395(2) 0.71092(17) 0.54521(11) 0.0175(5) Uani 1 1 d . . . . . H25A H -0.0333 0.6671 0.5499 0.021 Uiso 1 1 calc R U . . . H25B H 0.0697 0.6952 0.5051 0.021 Uiso 1 1 calc R U . . . C14 C 0.3259(2) 0.88618(17) 0.60414(11) 0.0184(5) Uani 1 1 d . . . . . H14 H 0.2429 0.8825 0.6183 0.022 Uiso 1 1 calc R U . . . C5 C -0.1400(3) 0.82818(17) 0.71798(13) 0.0243(6) Uani 1 1 d . . . . . H5 H -0.2349 0.8340 0.7061 0.029 Uiso 1 1 calc R U . . . C18 C 0.5123(2) 0.81109(17) 0.56899(11) 0.0195(5) Uani 1 1 d . . . . . H18 H 0.5558 0.7562 0.5588 0.023 Uiso 1 1 calc R U . . . C27 C -0.1276(2) 0.81855(17) 0.48057(11) 0.0193(5) Uani 1 1 d . . . . . H27A H -0.1666 0.8818 0.4789 0.023 Uiso 1 1 calc R U . . . H27B H -0.0896 0.8090 0.4417 0.023 Uiso 1 1 calc R U . . . C20 C 0.3338(2) 0.52643(16) 0.53560(11) 0.0183(5) Uani 1 1 d . . . . . H20 H 0.3379 0.4976 0.5760 0.022 Uiso 1 1 calc R U . . . C9 C -0.0236(2) 0.43418(18) 0.73409(12) 0.0255(6) Uani 1 1 d . . . . . H9 H -0.0554 0.4156 0.7712 0.031 Uiso 1 1 calc R U . . . C19 C 0.3369(2) 0.62336(16) 0.53115(11) 0.0140(5) Uani 1 1 d . . . . . C15 C 0.3869(3) 0.97167(17) 0.60002(11) 0.0247(6) Uani 1 1 d . . . . . H15 H 0.3446 1.0268 0.6107 0.030 Uiso 1 1 calc R U . . . C24 C 0.3345(2) 0.66480(17) 0.47183(11) 0.0170(5) Uani 1 1 d . . . . . H24 H 0.3366 0.7306 0.4683 0.020 Uiso 1 1 calc R U . . . C21 C 0.3247(2) 0.47227(17) 0.48120(12) 0.0223(6) Uani 1 1 d . . . . . H21 H 0.3199 0.4065 0.4842 0.027 Uiso 1 1 calc R U . . . C29 C 0.5991(2) 0.57812(18) 0.89079(12) 0.0239(6) Uani 1 1 d . . . . . C11 C 0.0242(3) 0.39777(17) 0.63118(12) 0.0261(6) Uani 1 1 d . . . . . H11 H 0.0254 0.3542 0.5979 0.031 Uiso 1 1 calc R U . . . C23 C 0.3291(2) 0.60974(18) 0.41785(11) 0.0211(5) Uani 1 1 d . . . . . H23 H 0.3300 0.6379 0.3777 0.025 Uiso 1 1 calc R U . . . C10 C -0.0197(3) 0.37067(18) 0.68577(13) 0.0276(6) Uani 1 1 d . . . . . H10 H -0.0473 0.3083 0.6902 0.033 Uiso 1 1 calc R U . . . C17 C 0.5724(3) 0.89713(19) 0.56571(11) 0.0259(6) Uani 1 1 d . . . . . H17 H 0.6573 0.9011 0.5533 0.031 Uiso 1 1 calc R U . . . C4 C -0.0665(3) 0.89383(17) 0.75731(12) 0.0249(6) Uani 1 1 d . . . . . H4 H -0.1111 0.9448 0.7724 0.030 Uiso 1 1 calc R U . . . C16 C 0.5092(3) 0.97685(18) 0.58039(11) 0.0270(6) Uani 1 1 d . . . . . H16 H 0.5498 1.0357 0.5770 0.032 Uiso 1 1 calc R U . . . C22 C 0.3225(2) 0.51409(18) 0.42251(12) 0.0237(6) Uani 1 1 d . . . . . H22 H 0.3165 0.4769 0.3853 0.028 Uiso 1 1 calc R U . . . C3 C 0.0715(3) 0.88552(17) 0.77477(12) 0.0263(6) Uani 1 1 d . . . . . H3 H 0.1213 0.9302 0.8025 0.032 Uiso 1 1 calc R U . . . C28 C -0.3343(2) 0.7576(2) 0.42871(12) 0.0290(6) Uani 1 1 d . . . . . H28A H -0.2959 0.7557 0.3900 0.044 Uiso 1 1 calc R U . . . H28B H -0.3828 0.8162 0.4301 0.044 Uiso 1 1 calc R U . . . H28C H -0.3965 0.7054 0.4284 0.044 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 0.01075(15) 0.01333(16) 0.01095(16) 0.00102(11) 0.00096(11) 0.00017(12) S2 0.0118(3) 0.0199(3) 0.0125(3) 0.0019(2) 0.0009(2) -0.0002(2) P2 0.0116(3) 0.0130(3) 0.0118(3) 0.0009(2) 0.0018(2) -0.0001(2) P1 0.0112(3) 0.0127(3) 0.0124(3) -0.0003(2) 0.0021(2) -0.0004(2) S1 0.0151(3) 0.0249(3) 0.0143(3) 0.0044(2) 0.0032(2) 0.0028(2) O1 0.0145(8) 0.0241(9) 0.0226(9) 0.0083(7) -0.0037(7) -0.0030(7) N1 0.0109(9) 0.0176(10) 0.0118(10) 0.0003(8) 0.0018(8) -0.0006(8) N3 0.0192(12) 0.0344(13) 0.0252(12) 0.0046(10) -0.0019(10) 0.0010(10) C6 0.0185(12) 0.0164(12) 0.0229(13) -0.0011(10) 0.0081(10) -0.0025(10) C1 0.0194(12) 0.0123(12) 0.0131(12) 0.0029(9) 0.0068(9) 0.0005(9) C32 0.0160(12) 0.0136(12) 0.0145(12) -0.0007(9) 0.0004(9) 0.0043(9) C13 0.0173(12) 0.0152(12) 0.0099(11) 0.0007(9) -0.0027(9) -0.0023(10) C7 0.0100(11) 0.0131(12) 0.0205(13) -0.0009(9) 0.0010(9) -0.0003(9) C30 0.0166(12) 0.0160(12) 0.0135(12) -0.0002(9) -0.0010(9) 0.0063(10) C31 0.0220(14) 0.0189(13) 0.0146(12) 0.0027(10) 0.0031(10) 0.0058(10) C12 0.0186(12) 0.0211(13) 0.0179(13) -0.0007(10) 0.0022(10) -0.0006(10) C2 0.0229(13) 0.0172(13) 0.0189(13) -0.0002(10) 0.0027(10) -0.0015(10) C26 0.0191(13) 0.0182(13) 0.0182(13) 0.0032(10) -0.0004(10) -0.0005(10) N2 0.0370(14) 0.0631(18) 0.0190(13) 0.0086(12) 0.0049(11) 0.0217(13) C8 0.0198(13) 0.0206(13) 0.0187(13) -0.0013(10) 0.0038(10) -0.0041(10) C25 0.0150(12) 0.0223(13) 0.0136(12) -0.0011(10) -0.0013(9) 0.0012(10) C14 0.0185(12) 0.0202(13) 0.0138(12) -0.0004(10) -0.0033(10) 0.0002(10) C5 0.0219(13) 0.0219(14) 0.0319(15) 0.0062(11) 0.0126(11) 0.0052(11) C18 0.0189(13) 0.0224(13) 0.0166(13) 0.0006(10) 0.0019(10) -0.0028(10) C27 0.0161(12) 0.0198(13) 0.0203(13) 0.0042(10) -0.0007(10) -0.0028(10) C20 0.0185(12) 0.0173(12) 0.0197(13) 0.0025(10) 0.0054(10) 0.0034(10) C9 0.0227(13) 0.0254(14) 0.0266(14) 0.0079(11) 0.0004(11) -0.0072(11) C19 0.0089(11) 0.0174(12) 0.0158(12) -0.0014(9) 0.0024(9) -0.0002(9) C15 0.0357(15) 0.0150(13) 0.0198(13) -0.0009(10) -0.0035(11) 0.0001(11) C24 0.0157(12) 0.0176(12) 0.0177(13) -0.0004(10) 0.0034(10) 0.0002(10) C21 0.0198(13) 0.0165(13) 0.0313(15) -0.0037(11) 0.0066(11) 0.0021(10) C29 0.0204(13) 0.0314(15) 0.0208(15) 0.0012(11) 0.0064(11) 0.0085(11) C11 0.0292(15) 0.0174(13) 0.0271(15) -0.0069(11) -0.0063(12) 0.0003(11) C23 0.0207(13) 0.0286(14) 0.0144(13) -0.0006(10) 0.0044(10) 0.0004(11) C10 0.0285(15) 0.0146(13) 0.0348(16) 0.0057(11) -0.0057(12) -0.0062(11) C17 0.0264(14) 0.0326(16) 0.0182(14) 0.0010(11) 0.0030(11) -0.0130(12) C4 0.0411(16) 0.0144(13) 0.0239(14) 0.0042(10) 0.0179(12) 0.0073(12) C16 0.0398(16) 0.0201(14) 0.0172(14) 0.0017(10) -0.0037(12) -0.0144(12) C22 0.0200(13) 0.0277(15) 0.0238(14) -0.0098(11) 0.0048(11) 0.0008(11) C3 0.0413(16) 0.0171(13) 0.0198(14) -0.0031(10) 0.0040(12) -0.0023(12) C28 0.0197(13) 0.0347(16) 0.0277(15) 0.0050(12) -0.0074(11) -0.0077(12) 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' 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' 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' 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 S2 Ni1 P1 167.88(3) . . S2 Ni1 S1 94.40(2) . . P1 Ni1 S1 96.11(2) . . S2 Ni1 P2 96.02(2) . . P1 Ni1 P2 73.45(2) . . S1 Ni1 P2 169.55(3) . . C32 S2 Ni1 101.76(8) . . N1 P2 C13 111.75(10) . . N1 P2 C19 104.97(10) . . C13 P2 C19 106.09(10) . . N1 P2 Ni1 93.53(7) . . C13 P2 Ni1 112.65(7) . . C19 P2 Ni1 126.53(8) . . N1 P2 P1 40.44(6) . . C13 P2 P1 124.35(8) . . C19 P2 P1 125.32(8) . . Ni1 P2 P1 53.12(2) . . N1 P1 C7 110.00(10) . . N1 P1 C1 107.76(10) . . C7 P1 C1 107.83(10) . . N1 P1 Ni1 93.86(7) . . C7 P1 Ni1 114.79(7) . . C1 P1 Ni1 121.22(8) . . N1 P1 P2 40.45(6) . . C7 P1 P2 122.03(8) . . C1 P1 P2 126.78(8) . . Ni1 P1 P2 53.43(2) . . C30 S1 Ni1 101.65(8) . . C28 O1 C27 110.91(18) . . C25 N1 P1 130.05(15) . . C25 N1 P2 130.01(15) . . P1 N1 P2 99.11(10) . . C5 C6 C1 119.9(2) . . C5 C6 H6 120.0 . . C1 C6 H6 120.0 . . C2 C1 C6 119.7(2) . . C2 C1 P1 118.93(18) . . C6 C1 P1 120.90(18) . . C30 C32 C31 121.0(2) . . C30 C32 S2 121.07(17) . . C31 C32 S2 117.74(17) . . C14 C13 C18 119.8(2) . . C14 C13 P2 120.84(18) . . C18 C13 P2 118.72(18) . . C12 C7 C8 119.5(2) . . C12 C7 P1 120.56(18) . . C8 C7 P1 118.62(17) . . C32 C30 C29 120.5(2) . . C32 C30 S1 121.04(17) . . C29 C30 S1 118.49(18) . . N3 C31 C32 176.5(3) . . C11 C12 C7 120.0(2) . . C11 C12 H12 120.0 . . C7 C12 H12 120.0 . . C3 C2 C1 119.8(2) . . C3 C2 H2 120.1 . . C1 C2 H2 120.1 . . C27 C26 C25 111.2(2) . . C27 C26 H26A 109.4 . . C25 C26 H26A 109.4 . . C27 C26 H26B 109.4 . . C25 C26 H26B 109.4 . . H26A C26 H26B 108.0 . . C9 C8 C7 119.9(2) . . C9 C8 H8 120.1 . . C7 C8 H8 120.1 . . N1 C25 C26 114.75(19) . . N1 C25 H25A 108.6 . . C26 C25 H25A 108.6 . . N1 C25 H25B 108.6 . . C26 C25 H25B 108.6 . . H25A C25 H25B 107.6 . . C15 C14 C13 119.7(2) . . C15 C14 H14 120.1 . . C13 C14 H14 120.1 . . C4 C5 C6 120.0(2) . . C4 C5 H5 120.0 . . C6 C5 H5 120.0 . . C17 C18 C13 119.7(2) . . C17 C18 H18 120.2 . . C13 C18 H18 120.2 . . O1 C27 C26 109.06(19) . . O1 C27 H27A 109.9 . . C26 C27 H27A 109.9 . . O1 C27 H27B 109.9 . . C26 C27 H27B 109.9 . . H27A C27 H27B 108.3 . . C21 C20 C19 120.2(2) . . C21 C20 H20 119.9 . . C19 C20 H20 119.9 . . C10 C9 C8 120.1(2) . . C10 C9 H9 120.0 . . C8 C9 H9 120.0 . . C24 C19 C20 119.4(2) . . C24 C19 P2 120.89(18) . . C20 C19 P2 119.15(17) . . C16 C15 C14 120.2(2) . . C16 C15 H15 119.9 . . C14 C15 H15 119.9 . . C23 C24 C19 119.9(2) . . C23 C24 H24 120.0 . . C19 C24 H24 120.0 . . C22 C21 C20 120.0(2) . . C22 C21 H21 120.0 . . C20 C21 H21 120.0 . . N2 C29 C30 178.5(3) . . C10 C11 C12 120.3(2) . . C10 C11 H11 119.8 . . C12 C11 H11 119.8 . . C22 C23 C24 120.2(2) . . C22 C23 H23 119.9 . . C24 C23 H23 119.9 . . C11 C10 C9 120.1(2) . . C11 C10 H10 119.9 . . C9 C10 H10 119.9 . . C16 C17 C18 120.2(2) . . C16 C17 H17 119.9 . . C18 C17 H17 119.9 . . C3 C4 C5 120.2(2) . . C3 C4 H4 119.9 . . C5 C4 H4 119.9 . . C17 C16 C15 120.4(2) . . C17 C16 H16 119.8 . . C15 C16 H16 119.8 . . C23 C22 C21 120.3(2) . . C23 C22 H22 119.8 . . C21 C22 H22 119.8 . . C4 C3 C2 120.3(2) . . C4 C3 H3 119.8 . . C2 C3 H3 119.8 . . O1 C28 H28A 109.5 . . O1 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . O1 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 S2 2.1487(6) . Ni1 P1 2.1514(7) . Ni1 S1 2.1564(6) . Ni1 P2 2.1602(7) . S2 C32 1.740(2) . P2 N1 1.6942(18) . P2 C13 1.801(2) . P2 C19 1.813(2) . P2 P1 2.5783(8) . P1 N1 1.6938(19) . P1 C7 1.801(2) . P1 C1 1.803(2) . S1 C30 1.739(2) . O1 C28 1.417(3) . O1 C27 1.427(3) . N1 C25 1.476(3) . N3 C31 1.146(3) . C6 C5 1.385(3) . C6 C1 1.395(3) . C6 H6 0.9500 . C1 C2 1.391(3) . C32 C30 1.363(3) . C32 C31 1.437(3) . C13 C14 1.395(3) . C13 C18 1.400(3) . C7 C12 1.394(3) . C7 C8 1.397(3) . C30 C29 1.438(3) . C12 C11 1.384(3) . C12 H12 0.9500 . C2 C3 1.383(3) . C2 H2 0.9500 . C26 C27 1.514(3) . C26 C25 1.520(3) . C26 H26A 0.9900 . C26 H26B 0.9900 . N2 C29 1.147(3) . C8 C9 1.389(3) . C8 H8 0.9500 . C25 H25A 0.9900 . C25 H25B 0.9900 . C14 C15 1.387(3) . C14 H14 0.9500 . C5 C4 1.382(4) . C5 H5 0.9500 . C18 C17 1.388(3) . C18 H18 0.9500 . C27 H27A 0.9900 . C27 H27B 0.9900 . C20 C21 1.387(3) . C20 C19 1.399(3) . C20 H20 0.9500 . C9 C10 1.385(4) . C9 H9 0.9500 . C19 C24 1.396(3) . C15 C16 1.385(4) . C15 H15 0.9500 . C24 C23 1.391(3) . C24 H24 0.9500 . C21 C22 1.386(4) . C21 H21 0.9500 . C11 C10 1.381(4) . C11 H11 0.9500 . C23 C22 1.383(4) . C23 H23 0.9500 . C10 H10 0.9500 . C17 C16 1.380(4) . C17 H17 0.9500 . C4 C3 1.381(4) . C4 H4 0.9500 . C16 H16 0.9500 . C22 H22 0.9500 . C3 H3 0.9500 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 .