#------------------------------------------------------------------------------ #$Date: 2025-02-01 04:09:04 +0200 (Sat, 01 Feb 2025) $ #$Revision: 297559 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573826.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_1573826 loop_ _publ_author_name 'Lu, Yuan' 'Ji, Gang' 'Yu, Shuyang' 'Ning, Xiaoshan' 'Sun, Xiu-Li' 'Gao, Yanshan' 'Wang, Xiaoyan' 'Tang, Yong' _publ_section_title ; Binuclear Ni catalyzed ethylene copolymerization with short chain alkenol monomers ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/D4PY01480D _journal_year 2025 _chemical_formula_sum 'C32 H47 Br3 N2 Ni2 O3' _chemical_formula_weight 864.86 _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 2022-06-14 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2024-07-07 deposited with the CCDC. 2025-01-23 downloaded from the CCDC. ; _cell_angle_alpha 97.0810(10) _cell_angle_beta 102.6620(10) _cell_angle_gamma 92.4100(10) _cell_formula_units_Z 2 _cell_length_a 9.1461(2) _cell_length_b 9.5974(2) _cell_length_c 20.7405(5) _cell_measurement_reflns_used 9868 _cell_measurement_temperature 235.00 _cell_measurement_theta_max 55.004 _cell_measurement_theta_min 4.050 _cell_volume 1758.26(7) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_unetI/netI 0.0637 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 19462 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 55.017 _diffrn_reflns_theta_min 4.048 _diffrn_source_current 2.86 _diffrn_source_power 0.1995708 _diffrn_source_voltage 69.78 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.674 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.4483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1466 before and 0.0878 after correction. The Ratio of minimum to maximum transmission is 0.5971. The \l/2 correction factor is Not present. ; _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.634 _exptl_crystal_F_000 876 _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.752 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.126 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 387 _refine_ls_number_reflns 6668 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0463 _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^)+(0.0865P)^2^+0.0173P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1273 _refine_ls_wR_factor_ref 0.1302 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6088 _reflns_number_total 6668 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4py01480d2.cif _cod_data_source_block mj22149_0m _cod_database_code 1573826 _shelx_shelxl_version_number 2018/3 _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 0.671 _shelx_estimated_absorpt_t_min 0.582 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C6(H6) 2.b Secondary CH2 refined with riding coordinates: C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A, H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B) 2.c Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C13(H13), C19(H19), C20(H20), C21(H21) 2.d Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A, H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL mj22149_0m_a.res in P-1 mj22149_0m.res created by SHELXL-2018/3 at 09:13:58 on 14-Jun-2022 REM Old TITL mj22149_0m in P-1 REM SHELXT solution in P-1: R1 0.139, Rweak 0.012, Alpha 0.053 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 N O4 Ni2 Br3 CELL 1.34139 9.1461 9.5974 20.7405 97.081 102.662 92.41 ZERR 2 0.0002 0.0002 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H Br N Ni O DISP Br -0.9338 1.0006 7840.1 DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP N 0.0241 0.0134 109.9 DISP Ni -1.3357 3.2904 25038 DISP O 0.0389 0.0241 193.4 UNIT 64 94 6 4 4 6 L.S. 4 PLAN 12 SIZE 0.05 0.07 0.07 TEMP -38.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT 7 -5 5 OMIT -2 1 1 OMIT 2 2 1 REM REM REM WGHT 0.086500 0.017300 FVAR 0.51829 BR1 3 0.586130 -0.079663 0.376155 11.00000 0.05918 0.02554 = 0.03797 0.01063 0.01295 0.00280 BR2 3 0.728607 0.039100 0.233431 11.00000 0.05107 0.03808 = 0.04345 0.01283 0.02317 0.02128 BR3 3 0.335216 0.232349 0.111718 11.00000 0.03853 0.05921 = 0.04137 0.00641 0.00258 0.01081 NI1 5 0.576916 0.117824 0.313456 11.00000 0.03611 0.01871 = 0.02568 0.00269 0.01006 0.00223 NI2 5 0.586030 0.230636 0.179051 11.00000 0.03280 0.02433 = 0.02624 0.00260 0.00869 0.00628 O1 6 0.538634 0.288019 0.269070 11.00000 0.03301 0.01878 = 0.02830 0.00155 0.01014 0.00208 O2 6 0.370657 0.035895 0.253411 11.00000 0.04975 0.02860 = 0.04426 0.00116 0.00157 -0.00565 O3 6 0.674523 0.170459 0.093321 11.00000 0.05372 0.04955 = 0.03124 0.00610 0.01647 0.02230 N1 4 0.709836 0.264623 0.383750 11.00000 0.03867 0.02565 = 0.02616 0.00363 0.01007 0.00267 N2 4 0.701533 0.419188 0.204741 11.00000 0.03142 0.02430 = 0.03035 0.00868 0.01077 0.00557 C1 1 0.605520 0.416036 0.303751 11.00000 0.03570 0.01799 = 0.02687 0.00156 0.01037 0.00203 C2 1 0.704730 0.392744 0.371584 11.00000 0.03909 0.02658 = 0.02808 0.00026 0.01085 -0.00119 C3 1 0.779485 0.513965 0.422231 11.00000 0.07230 0.02673 = 0.03708 -0.00064 0.00282 -0.00449 AFIX 137 H3A 2 0.779033 0.492065 0.466615 11.00000 -1.50000 H3B 2 0.725526 0.597415 0.414505 11.00000 -1.50000 H3C 2 0.882330 0.530954 0.418388 11.00000 -1.50000 AFIX 0 C4 1 0.700596 0.487405 0.262268 11.00000 0.03288 0.02333 = 0.03113 0.00686 0.01018 0.00612 C5 1 0.780746 0.629312 0.286267 11.00000 0.05650 0.03022 = 0.04681 0.00120 0.02139 -0.00747 AFIX 137 H5A 2 0.878973 0.619183 0.313932 11.00000 -1.50000 H5B 2 0.722961 0.686043 0.312168 11.00000 -1.50000 H5C 2 0.792377 0.674911 0.248294 11.00000 -1.50000 AFIX 0 C6 1 0.480979 0.516824 0.317055 11.00000 0.04277 0.02153 = 0.04302 0.00022 0.01763 0.00576 AFIX 13 H6 2 0.530887 0.606888 0.342298 11.00000 -1.20000 AFIX 0 C7 1 0.382736 0.546785 0.252584 11.00000 0.04998 0.04274 = 0.06055 0.01892 0.02104 0.02127 AFIX 137 H7A 2 0.345606 0.458746 0.224229 11.00000 -1.50000 H7B 2 0.440758 0.603367 0.230091 11.00000 -1.50000 H7C 2 0.298562 0.597541 0.261904 11.00000 -1.50000 AFIX 0 C8 1 0.383314 0.452558 0.358568 11.00000 0.05176 0.04277 = 0.05683 0.00600 0.03083 0.01035 AFIX 137 H8A 2 0.308280 0.516801 0.366765 11.00000 -1.50000 H8B 2 0.445936 0.436148 0.400774 11.00000 -1.50000 H8C 2 0.333814 0.363988 0.334482 11.00000 -1.50000 AFIX 0 C9 1 0.796133 0.233431 0.446871 11.00000 0.05026 0.02327 = 0.02876 0.00242 0.00146 -0.00432 C10 1 0.721251 0.219811 0.497860 11.00000 0.08109 0.03285 = 0.02822 0.00645 0.01493 -0.00001 C11 1 0.804262 0.182950 0.557401 11.00000 0.10657 0.04136 = 0.02829 0.00658 0.00397 -0.00524 AFIX 43 H11 2 0.757107 0.173543 0.592757 11.00000 -1.20000 AFIX 0 C12 1 0.954992 0.160068 0.565097 11.00000 0.11157 0.03681 = 0.03512 0.00719 -0.01706 -0.01250 AFIX 43 H12 2 1.009427 0.134945 0.605448 11.00000 -1.20000 AFIX 0 C13 1 1.025556 0.174016 0.513742 11.00000 0.06455 0.03344 = 0.05412 0.00550 -0.02001 -0.00747 AFIX 43 H13 2 1.127968 0.157777 0.519547 11.00000 -1.20000 AFIX 0 C14 1 0.947684 0.212019 0.452833 11.00000 0.05161 0.02733 = 0.04156 0.00440 -0.00246 -0.00519 C15 1 1.026124 0.224723 0.397902 11.00000 0.04483 0.06812 = 0.06421 0.01272 0.00801 0.00687 AFIX 137 H15A 2 0.974116 0.162541 0.358306 11.00000 -1.50000 H15B 2 1.128659 0.198789 0.411261 11.00000 -1.50000 H15C 2 1.026745 0.321123 0.388319 11.00000 -1.50000 AFIX 0 C16 1 0.558170 0.242074 0.490650 11.00000 0.08590 0.06059 = 0.04716 0.01913 0.03542 0.01011 AFIX 137 H16A 2 0.543267 0.341611 0.490999 11.00000 -1.50000 H16B 2 0.523739 0.208629 0.527419 11.00000 -1.50000 H16C 2 0.501566 0.190446 0.448850 11.00000 -1.50000 AFIX 0 C17 1 0.786033 0.478131 0.161266 11.00000 0.04251 0.03061 = 0.02774 0.00619 0.01323 0.00211 C18 1 0.932971 0.443324 0.165283 11.00000 0.03510 0.03637 = 0.03890 0.00455 0.01431 -0.00027 C19 1 1.010454 0.494609 0.121326 11.00000 0.04679 0.04785 = 0.05252 0.00325 0.02315 -0.00407 AFIX 43 H19 2 1.110198 0.472250 0.123051 11.00000 -1.20000 AFIX 0 C20 1 0.942928 0.577507 0.075448 11.00000 0.06650 0.04673 = 0.04099 0.00467 0.02672 -0.00932 AFIX 43 H20 2 0.996803 0.611636 0.046230 11.00000 -1.20000 AFIX 0 C21 1 0.797645 0.610532 0.072145 11.00000 0.07691 0.04439 = 0.03855 0.01408 0.02420 0.00624 AFIX 43 H21 2 0.752946 0.667596 0.040655 11.00000 -1.20000 AFIX 0 C22 1 0.714584 0.561017 0.114694 11.00000 0.05520 0.04066 = 0.03896 0.01470 0.01869 0.00932 C23 1 0.555428 0.599569 0.110871 11.00000 0.07279 0.08836 = 0.06987 0.05212 0.03037 0.04023 AFIX 137 H23A 2 0.554278 0.678795 0.144620 11.00000 -1.50000 H23B 2 0.495750 0.519808 0.118459 11.00000 -1.50000 H23C 2 0.513654 0.624957 0.067069 11.00000 -1.50000 AFIX 0 C24 1 1.008241 0.355739 0.216364 11.00000 0.03339 0.06889 = 0.06548 0.02671 0.01663 0.00986 AFIX 137 H24A 2 1.093100 0.314327 0.202367 11.00000 -1.50000 H24B 2 0.937175 0.281559 0.220776 11.00000 -1.50000 H24C 2 1.043107 0.414709 0.258972 11.00000 -1.50000 AFIX 0 C25 1 0.243031 0.046726 0.282604 11.00000 0.04304 0.05449 = 0.09386 -0.02183 0.00208 0.01594 AFIX 23 H25A 2 0.190837 0.130794 0.271663 11.00000 -1.20000 H25B 2 0.273754 0.052170 0.331231 11.00000 -1.20000 AFIX 0 C26 1 0.141506 -0.086362 0.252864 11.00000 0.04670 0.07173 = 0.09879 -0.00108 0.01288 -0.00790 AFIX 23 H26A 2 0.163205 -0.161401 0.280883 11.00000 -1.20000 H26B 2 0.035219 -0.067758 0.247201 11.00000 -1.20000 AFIX 0 C27 1 0.180650 -0.123529 0.187740 11.00000 0.08225 0.07528 = 0.06356 -0.00344 -0.00528 -0.02841 AFIX 23 H27A 2 0.127865 -0.067986 0.154444 11.00000 -1.20000 H27B 2 0.156653 -0.223862 0.171264 11.00000 -1.20000 AFIX 0 C28 1 0.349041 -0.086969 0.203889 11.00000 0.07464 0.04649 = 0.04758 -0.01410 0.01657 -0.02275 AFIX 23 H28A 2 0.404121 -0.164421 0.221700 11.00000 -1.20000 H28B 2 0.382590 -0.066068 0.164144 11.00000 -1.20000 AFIX 0 C29 1 0.787103 0.075138 0.084379 11.00000 0.07163 0.08364 = 0.05066 0.00617 0.02837 0.04658 AFIX 23 H29A 2 0.745090 -0.022508 0.078052 11.00000 -1.20000 H29B 2 0.871349 0.088803 0.123499 11.00000 -1.20000 AFIX 0 C30 1 0.838908 0.107129 0.023405 11.00000 0.07281 0.10502 = 0.05926 -0.00236 0.03706 0.02519 AFIX 23 H30A 2 0.938713 0.157247 0.035983 11.00000 -1.20000 H30B 2 0.843436 0.020133 -0.006055 11.00000 -1.20000 AFIX 0 C31 1 0.728328 0.194685 -0.009374 11.00000 0.11278 0.21250 = 0.06370 0.06561 0.05951 0.09526 AFIX 23 H31A 2 0.777017 0.285492 -0.012888 11.00000 -1.20000 H31B 2 0.681537 0.148731 -0.054500 11.00000 -1.20000 AFIX 0 C32 1 0.615735 0.216230 0.029003 11.00000 0.08256 0.07532 = 0.03221 0.01693 0.02289 0.02995 AFIX 23 H32A 2 0.521942 0.161204 0.006257 11.00000 -1.20000 H32B 2 0.595483 0.315914 0.034822 11.00000 -1.20000 AFIX 0 HKLF 4 REM mj22149_0m_a.res in P-1 REM wR2 = 0.1302, GooF = S = 1.079, Restrained GooF = 1.079 for all data REM R1 = 0.0463 for 6088 Fo > 4sig(Fo) and 0.0492 for all 6668 data REM 387 parameters refined using 0 restraints END WGHT 0.0865 0.0174 REM Highest difference peak 0.752, deepest hole -1.088, 1-sigma level 0.126 Q1 1 0.4721 -0.0374 0.3699 11.00000 0.05 0.75 Q2 1 0.2132 0.2702 0.1118 11.00000 0.05 0.74 Q3 1 0.8516 -0.0064 0.2415 11.00000 0.05 0.68 Q4 1 0.7103 -0.1278 0.3838 11.00000 0.05 0.65 Q5 1 0.6754 0.0273 0.2802 11.00000 0.05 0.64 Q6 1 0.6251 0.1236 0.2681 11.00000 0.05 0.62 Q7 1 0.4619 -0.0205 0.4127 11.00000 0.05 0.59 Q8 1 0.4548 0.1971 0.3376 11.00000 0.05 0.59 Q9 1 0.8480 -0.0395 0.2037 11.00000 0.05 0.58 Q10 1 0.7149 -0.1491 0.3477 11.00000 0.05 0.57 Q11 1 0.6309 0.0008 0.2245 11.00000 0.05 0.56 Q12 1 0.4730 0.1748 0.3097 11.00000 0.05 0.55 ; _shelx_res_checksum 75824 _shelx_hkl_file ; -2 0 0 443.76 37.40 -2 0 0 444.46 37.70 2 0 0 426.06 37.40 2 0 0 515.95 42.60 -3 0 0 3078.09 230.48 3 0 0 2320.87 227.38 -4 0 0 6.50 2.20 -4 0 0 12.30 1.80 -4 0 0 14.60 9.80 4 0 0 8.70 1.70 4 0 0 0.30 7.70 -5 0 0 852.91 80.59 -5 0 0 883.81 63.49 -5 0 0 755.32 63.59 -5 0 0 701.03 64.19 5 0 0 627.04 74.49 5 0 0 779.72 63.69 -6 0 0 771.92 63.89 -6 0 0 804.72 63.59 -6 0 0 744.93 64.49 6 0 0 752.82 63.89 -7 0 0 911.31 72.69 -7 0 0 861.71 71.79 7 0 0 817.42 71.89 -8 0 0 189.28 15.60 -8 0 0 155.38 15.10 8 0 0 172.88 16.10 -9 0 0 2.50 3.10 -9 0 0 6.30 8.00 9 0 0 2.50 4.00 10 0 0 14.10 4.00 10 -1 0 3.60 3.60 9 -1 0 64.99 8.50 -9 1 0 69.79 7.80 8 -1 0 492.05 39.60 -8 1 0 504.65 40.40 -8 1 0 420.56 39.10 -8 1 0 453.25 39.00 7 -1 0 1243.58 100.09 -7 1 0 1231.68 99.69 -7 1 0 1155.38 99.79 -7 1 0 1199.58 100.69 6 -1 0 191.58 17.10 -6 1 0 198.88 39.90 -6 1 0 198.28 16.70 -6 1 0 186.48 16.70 -6 1 0 204.98 17.90 5 -1 0 197.88 32.10 5 -1 0 226.68 18.60 -5 1 0 219.48 18.40 -5 1 0 209.38 19.20 -5 1 0 244.28 36.70 -5 1 0 215.38 18.30 4 -1 0 254.97 22.60 4 -1 0 267.67 33.40 -4 1 0 263.17 22.50 -4 1 0 269.77 23.20 -4 1 0 337.97 37.10 3 -1 0 118.79 10.70 3 -1 0 161.88 19.90 -3 1 0 121.39 10.50 -3 1 0 134.59 11.20 -3 1 0 118.39 10.60 2 -1 0 36.10 3.40 2 -1 0 27.30 8.40 2 -1 0 41.60 3.50 -2 1 0 37.40 3.40 -2 1 0 42.10 9.60 1 -1 0 4082.89 367.26 -1 1 0 4782.82 367.96 0 -1 0 2459.95 204.88 0 1 0 2506.85 204.88 -1 -1 0 55.69 6.80 -1 -1 0 67.99 5.50 1 1 0 60.39 6.90 -2 -1 0 812.32 63.19 2 1 0 703.03 62.39 2 1 0 638.94 58.69 -3 -1 0 367.96 26.60 -3 -1 0 296.57 26.10 -3 -1 0 309.77 26.10 -3 -1 0 278.97 25.90 3 1 0 321.67 32.40 3 1 0 309.67 26.00 -4 -1 0 1967.60 155.48 4 1 0 1801.32 164.28 -5 -1 0 2040.90 167.48 -5 -1 0 1898.91 151.38 -5 -1 0 1775.12 152.18 -5 -1 0 1897.21 151.68 5 1 0 1629.44 151.58 -6 -1 0 1323.37 109.99 -6 -1 0 1350.36 110.39 -6 -1 0 1216.18 110.89 6 1 0 1457.15 111.49 -7 -1 0 82.19 9.30 -7 -1 0 63.29 7.20 -7 -1 0 82.19 8.30 7 1 0 71.59 8.30 -8 -1 0 303.27 27.50 -8 -1 0 307.47 26.80 8 1 0 316.77 27.00 -9 -1 0 139.79 14.00 9 1 0 180.28 14.70 9 1 0 133.79 14.30 10 1 0 50.99 7.50 10 -2 0 8.50 3.60 -10 2 0 7.10 3.60 9 -2 0 234.08 19.80 -9 2 0 209.38 19.20 8 -2 0 58.39 7.80 -8 2 0 65.09 7.20 -8 2 0 72.59 9.20 7 -2 0 114.59 10.00 -7 2 0 89.49 10.70 -7 2 0 114.39 9.50 -7 2 0 87.49 9.00 6 -2 0 330.67 26.10 6 -2 0 271.67 50.89 -6 2 0 285.97 25.80 -6 2 0 330.17 25.80 -6 2 0 288.27 26.80 5 -2 0 288.97 23.20 5 -2 0 224.78 36.80 -5 2 0 300.67 23.10 -5 2 0 252.57 22.90 4 -2 0 1249.07 93.79 4 -2 0 962.30 103.99 -4 2 0 1170.08 93.59 -4 2 0 1032.40 93.49 -4 2 0 1272.87 109.99 3 -2 0 30.30 10.70 3 -2 0 44.00 4.00 -3 2 0 41.00 3.80 2 -2 0 1560.34 130.79 2 -2 0 1447.46 123.49 1 -2 0 872.11 76.69 -1 2 0 990.70 76.59 0 -2 0 67.29 5.40 0 -2 0 65.59 7.10 0 -2 0 58.19 5.40 0 2 0 62.19 7.30 0 2 0 66.59 5.40 -1 -2 0 2595.14 205.58 1 2 0 2356.06 205.38 -2 -2 0 50.99 4.70 -2 -2 0 56.89 8.50 2 2 0 51.39 8.50 2 2 0 53.69 4.60 -3 -2 0 369.26 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148.09 18.60 -6 -4 21 208.78 18.40 -5 -4 21 92.19 12.00 -5 -4 21 88.79 10.50 -4 -4 21 55.49 9.00 -4 -4 21 61.79 9.10 3 4 -21 309.07 27.20 -3 -4 21 338.77 28.70 2 4 -21 61.19 7.10 -2 -4 21 70.19 9.70 1 4 -21 10.20 3.10 -1 -4 21 6.70 5.40 0 4 -21 5.90 3.10 0 -4 21 10.10 5.40 -1 4 -21 112.89 11.20 1 -4 21 118.29 12.10 -2 4 -21 55.69 7.00 2 -4 21 54.19 7.40 -3 4 -21 10.30 3.30 3 -4 21 6.30 3.10 -7 -3 21 87.49 10.90 -7 -3 21 70.59 8.20 -6 -3 21 376.66 32.90 -6 -3 21 387.86 33.90 5 3 -21 212.98 18.30 -5 -3 21 217.98 19.60 -5 -3 21 198.78 20.50 4 3 -21 106.99 10.60 -4 -3 21 118.89 12.60 3 3 -21 687.73 59.79 -3 -3 21 751.12 60.79 2 3 -21 558.74 48.20 -2 -3 21 595.84 49.20 1 3 -21 206.28 19.20 -1 -3 21 232.88 20.40 0 3 -21 158.88 14.50 0 -3 21 153.78 15.30 -1 3 -21 13.30 4.10 1 -3 21 19.30 4.80 -2 3 -21 74.89 8.40 2 -3 21 63.49 8.20 -3 3 -21 106.59 12.90 3 -3 21 125.89 11.40 7 2 -21 0.30 2.30 -7 -2 21 -0.30 8.40 -7 -2 21 0.00 3.20 6 2 -21 17.90 3.40 -6 -2 21 12.90 4.10 -6 -2 21 10.90 5.50 5 2 -21 9.40 3.10 -5 -2 21 5.00 4.10 4 2 -21 207.98 18.80 -4 -2 21 222.88 20.10 3 2 -21 532.95 44.70 -3 -2 21 532.95 45.60 2 2 -21 174.68 16.50 -2 -2 21 194.28 17.70 1 2 -21 171.18 15.70 -1 -2 21 171.48 16.70 0 2 -21 32.20 5.10 0 -2 21 29.80 5.40 -1 2 -21 8.40 3.70 1 -2 21 8.20 3.60 -2 2 -21 261.07 21.70 2 -2 21 230.18 21.40 -3 2 -21 308.67 26.00 3 -2 21 289.77 25.80 -4 2 -21 66.89 7.80 8 1 -21 29.50 4.50 -8 -1 21 26.00 4.00 7 1 -21 18.10 4.60 6 1 -21 7.90 3.10 -6 -1 21 11.10 4.20 5 1 -21 86.99 9.20 -5 -1 21 88.39 10.20 4 1 -21 269.27 23.80 -4 -1 21 280.57 24.60 3 1 -21 17.60 3.90 -3 -1 21 16.60 4.90 2 1 -21 474.35 40.70 -2 -1 21 491.25 41.40 1 1 -21 271.07 24.70 -1 -1 21 298.07 25.30 0 1 -21 95.29 10.30 0 -1 21 95.69 10.60 -1 1 -21 110.99 11.30 1 -1 21 109.39 11.20 -2 1 -21 4.80 3.80 2 -1 21 1.00 3.00 -3 1 -21 108.29 11.00 -4 1 -21 23.70 4.20 8 0 -21 143.59 12.40 -8 0 21 128.39 12.40 -7 0 21 3.40 3.60 6 0 -21 57.39 7.20 -6 0 21 59.89 7.90 5 0 -21 5.00 3.30 -5 0 21 -1.50 4.40 4 0 -21 18.70 4.30 -4 0 21 15.70 5.20 3 0 -21 157.38 14.60 -3 0 21 154.18 15.30 2 0 -21 984.60 84.39 -2 0 21 1046.40 84.79 1 0 -21 454.15 40.20 -1 0 21 495.45 40.50 0 0 -21 37.70 5.60 0 0 21 30.80 5.30 -1 0 -21 287.97 25.00 1 0 21 285.17 24.80 -2 0 -21 152.78 13.90 2 0 21 136.89 13.20 7 -1 -21 15.80 4.40 -7 1 21 4.80 3.30 6 -1 -21 286.57 25.40 -6 1 21 302.87 25.70 5 -1 -21 253.67 22.70 -5 1 21 265.87 23.10 4 -1 -21 119.69 12.10 -4 1 21 126.39 12.90 3 -1 -21 224.28 20.00 -3 1 21 222.78 20.40 2 -1 -21 135.59 12.90 -2 1 21 125.19 13.20 1 -1 -21 37.70 5.40 -1 1 21 23.50 4.80 0 -1 -21 233.08 20.50 0 1 21 225.18 20.40 -1 -1 -21 135.79 13.50 1 1 21 140.89 13.10 -2 -1 -21 113.59 11.60 -3 -1 -21 102.59 10.50 7 -2 -21 0.20 3.40 -7 2 21 2.20 3.20 6 -2 -21 58.19 7.80 -6 2 21 61.19 7.90 5 -2 -21 48.20 7.20 -5 2 21 47.30 7.70 4 -2 -21 39.70 5.30 -4 2 21 27.90 4.90 3 -2 -21 52.89 8.00 -3 2 21 57.99 8.20 2 -2 -21 33.20 5.30 -2 2 21 32.20 5.50 1 -2 -21 16.10 4.50 -1 2 21 21.50 4.50 0 -2 -21 133.49 13.20 0 2 21 134.89 12.80 -1 -2 -21 4.10 4.20 1 2 21 6.00 5.30 -2 -2 -21 11.80 4.30 -3 -2 -21 -0.30 3.10 6 -3 -21 0.10 3.50 -6 3 21 2.00 3.20 5 -3 -21 82.69 9.20 -5 3 21 78.29 9.00 4 -3 -21 19.60 4.50 -4 3 21 22.50 4.90 3 -3 -21 209.08 19.10 -3 3 21 214.08 19.20 2 -3 -21 410.66 35.00 -2 3 21 409.26 35.00 1 -3 -21 13.10 4.10 -1 3 21 20.70 4.30 0 -3 -21 99.29 10.90 0 3 21 106.59 10.80 -1 -3 -21 9.10 5.10 -2 -3 -21 8.90 3.70 6 -4 -21 7.40 3.30 -6 4 21 4.10 3.30 5 -4 -21 110.49 11.30 -5 4 21 114.39 11.20 4 -4 -21 36.00 5.50 -4 4 21 26.30 5.10 3 -4 -21 60.19 7.80 -3 4 21 48.50 7.20 2 -4 -21 218.18 20.60 -2 4 21 246.68 20.80 1 -4 -21 18.50 4.30 -1 4 21 20.50 3.80 0 -4 -21 3.60 3.60 0 4 21 -0.50 2.90 -1 -4 -21 15.90 3.90 4 -5 -21 32.70 4.90 -4 5 21 37.80 5.70 3 -5 -21 6.50 3.50 -3 5 21 3.20 3.00 2 -5 -21 14.20 3.70 -2 5 21 14.10 3.30 1 -5 -21 19.10 3.90 -1 5 21 15.80 3.40 -4 -6 22 40.80 6.10 -3 -6 22 16.80 4.90 -2 -6 22 159.08 16.80 -1 -6 22 31.30 6.20 0 -6 22 79.29 9.90 1 -6 22 107.49 11.30 -5 -5 22 33.70 5.50 -5 -5 22 33.80 6.80 -4 -5 22 72.39 9.90 -3 -5 22 107.79 12.40 -2 -5 22 432.66 37.60 -1 -5 22 268.57 24.40 0 5 -22 18.60 3.60 0 -5 22 25.30 5.20 -1 5 -22 6.80 2.80 1 -5 22 7.20 3.80 -2 5 -22 1.40 2.60 2 -5 22 -2.70 2.90 -6 -4 22 27.20 4.70 -6 -4 22 28.10 6.40 -5 -4 22 26.70 5.50 -4 -4 22 55.99 8.80 3 4 -22 -0.20 2.50 -3 -4 22 3.50 4.50 2 4 -22 84.59 9.00 -2 -4 22 100.09 11.50 1 4 -22 60.29 7.20 -1 -4 22 67.39 9.70 0 4 -22 8.20 3.30 0 -4 22 11.40 5.10 1 -4 22 10.70 4.10 -2 4 -22 3.80 3.10 2 -4 22 5.70 3.30 -7 -3 22 3.80 2.80 -7 -3 22 9.00 4.90 6 3 -22 36.30 5.40 -6 -3 22 41.10 5.90 -5 -3 22 154.78 15.20 4 3 -22 110.79 10.90 -4 -3 22 125.69 13.00 3 3 -22 4.90 3.00 -3 -3 22 5.60 5.60 2 3 -22 8.10 3.20 -2 -3 22 8.40 5.90 1 3 -22 12.00 3.60 -1 -3 22 10.10 5.10 0 3 -22 38.70 5.20 0 -3 22 34.90 5.90 -1 3 -22 397.66 34.60 1 -3 22 416.46 35.00 -2 3 -22 374.76 29.80 2 -3 22 312.27 29.20 -3 3 -22 27.40 4.30 7 2 -22 37.40 5.40 -7 -2 22 40.10 6.00 6 2 -22 222.48 19.70 -6 -2 22 231.58 20.30 5 2 -22 394.06 33.30 -5 -2 22 394.16 34.00 4 2 -22 172.28 15.80 -4 -2 22 180.48 17.00 3 2 -22 92.29 9.90 -3 -2 22 103.59 11.60 2 2 -22 257.17 24.10 -2 -2 22 302.87 25.10 1 2 -22 105.19 10.90 -1 -2 22 109.19 12.10 0 2 -22 79.89 8.80 0 -2 22 68.79 9.20 -1 2 -22 125.89 12.70 1 -2 22 132.99 12.80 -2 2 -22 111.89 11.70 2 -2 22 123.39 11.50 -3 2 -22 30.80 4.80 7 1 -22 38.10 4.80 -7 -1 22 39.70 6.20 6 1 -22 1.50 3.20 -6 -1 22 4.00 3.60 5 1 -22 129.89 12.20 -5 -1 22 127.69 13.20 4 1 -22 25.20 4.40 -4 -1 22 27.80 5.80 3 1 -22 235.08 20.40 -3 -1 22 226.08 21.40 2 1 -22 612.04 52.39 -2 -1 22 638.84 52.99 1 1 -22 202.98 18.40 -1 -1 22 204.68 18.90 0 1 -22 0.60 3.50 0 -1 22 1.90 3.60 -1 1 -22 7.40 4.20 1 -1 22 1.80 3.20 -2 1 -22 6.20 3.90 2 -1 22 9.20 3.30 -3 1 -22 20.50 4.30 7 0 -22 256.27 22.00 -7 0 22 255.37 22.20 6 0 -22 151.28 14.60 -6 0 22 168.78 15.10 5 0 -22 8.50 3.50 -5 0 22 17.90 4.90 4 0 -22 13.60 3.90 -4 0 22 22.30 5.70 3 0 -22 2.00 3.70 -3 0 22 1.10 4.10 2 0 -22 38.00 5.80 -2 0 22 49.00 7.00 1 0 -22 146.19 14.00 -1 0 22 143.29 14.30 0 0 -22 24.30 4.90 0 0 22 37.90 5.60 -1 0 -22 33.50 5.30 1 0 22 23.70 4.20 -2 0 -22 45.20 7.80 -3 0 -22 91.49 9.50 7 -1 -22 172.38 15.50 -7 1 22 171.38 15.50 6 -1 -22 137.89 14.90 -6 1 22 160.98 15.00 5 -1 -22 6.50 3.50 -5 1 22 6.80 4.20 4 -1 -22 6.20 3.70 -4 1 22 18.50 5.20 3 -1 -22 102.29 11.10 -3 1 22 107.09 11.50 2 -1 -22 469.55 40.90 -2 1 22 495.15 41.20 1 -1 -22 830.02 69.79 -1 1 22 842.02 69.89 0 -1 -22 262.97 23.50 0 1 22 272.37 23.40 -1 -1 -22 60.09 8.40 1 1 22 61.69 7.20 -2 -1 -22 127.09 12.60 6 -2 -22 18.20 3.90 -6 2 22 16.70 3.90 5 -2 -22 130.99 12.70 4 -2 -22 10.00 4.00 -4 2 22 24.10 4.90 3 -2 -22 13.60 4.40 -3 2 22 12.10 4.30 2 -2 -22 250.27 23.10 -2 2 22 272.77 23.20 1 -2 -22 494.55 41.50 -1 2 22 484.85 41.40 0 -2 -22 20.60 4.40 0 2 22 16.90 6.90 -1 -2 -22 57.49 8.00 1 2 22 46.30 7.20 -2 -2 -22 186.78 16.90 6 -3 -22 43.00 6.90 -6 3 22 56.09 6.90 5 -3 -22 77.49 8.60 -5 3 22 70.59 8.60 4 -3 -22 7.10 3.80 -4 3 22 8.00 4.60 3 -3 -22 52.79 7.80 -3 3 22 50.19 7.30 2 -3 -22 1.60 3.50 -2 3 22 0.70 3.80 1 -3 -22 15.80 4.60 -1 3 22 14.90 3.80 0 -3 -22 14.50 4.10 0 3 22 14.20 3.60 -1 -3 -22 2.40 3.40 4 -4 -22 2.40 3.40 -4 4 22 1.10 3.00 3 -4 -22 6.10 3.60 -3 4 22 4.20 3.50 2 -4 -22 9.40 3.50 -2 4 22 7.40 3.20 1 -4 -22 0.70 3.20 -1 4 22 5.20 3.00 -3 -6 23 53.09 8.10 -2 -6 23 39.80 6.50 -1 -6 23 3.80 3.90 -4 -5 23 36.80 6.40 -3 -5 23 52.49 7.80 -2 -5 23 4.90 6.10 -1 -5 23 29.80 6.20 0 5 -23 19.20 3.70 0 -5 23 20.80 4.90 -5 -4 23 25.20 5.30 -4 -4 23 53.39 9.10 -3 -4 23 -1.10 4.50 2 4 -23 36.50 5.90 -2 -4 23 58.09 7.80 1 4 -23 254.27 24.40 -1 -4 23 324.97 25.90 0 4 -23 47.80 6.30 0 -4 23 30.40 9.20 -1 4 -23 12.30 3.40 1 -4 23 15.00 4.10 -6 -3 23 14.40 4.10 5 3 -23 19.50 3.40 -5 -3 23 25.60 6.30 4 3 -23 243.08 22.60 -4 -3 23 287.37 23.90 3 3 -23 324.27 28.90 -3 -3 23 357.06 30.10 2 3 -23 0.10 3.00 -2 -3 23 0.80 5.00 1 3 -23 172.18 16.10 -1 -3 23 184.98 17.30 0 3 -23 39.00 7.00 0 -3 23 49.70 7.00 -1 3 -23 2.50 3.30 1 -3 23 -2.20 3.20 -2 3 -23 5.10 3.10 2 -3 23 1.00 3.00 6 2 -23 12.80 3.20 -6 -2 23 13.50 4.40 5 2 -23 0.60 2.80 -5 -2 23 1.70 4.30 4 2 -23 353.06 30.70 -4 -2 23 371.96 31.60 3 2 -23 600.74 54.09 -3 -2 23 698.63 54.99 2 2 -23 73.39 8.50 -2 -2 23 74.49 10.40 1 2 -23 19.60 4.00 -1 -2 23 8.80 4.40 0 2 -23 48.10 7.30 0 -2 23 52.09 7.90 -1 2 -23 116.99 14.10 1 -2 23 118.59 11.80 -2 2 -23 84.79 8.80 2 -2 23 76.99 8.50 6 1 -23 7.70 3.00 -6 -1 23 9.50 4.10 -5 -1 23 7.60 3.70 4 1 -23 136.79 12.80 -4 -1 23 129.99 13.70 3 1 -23 46.70 7.00 -3 -1 23 45.20 6.90 2 1 -23 3.90 3.50 -2 -1 23 6.50 4.60 1 1 -23 69.49 8.60 -1 -1 23 69.09 9.50 0 1 -23 27.80 4.80 0 -1 23 21.80 4.60 -1 1 -23 28.80 8.40 1 -1 23 37.80 5.30 -2 1 -23 212.58 18.90 6 0 -23 12.10 3.40 -6 0 23 22.50 4.50 5 0 -23 20.30 4.50 -5 0 23 17.60 4.70 4 0 -23 5.60 3.60 -4 0 23 8.80 4.90 3 0 -23 73.39 9.30 -3 0 23 87.59 10.20 2 0 -23 400.46 35.70 -2 0 23 439.66 36.20 1 0 -23 14.00 4.10 -1 0 23 12.80 4.10 0 0 -23 34.80 5.60 0 0 23 54.69 7.60 -1 0 -23 38.10 6.30 1 0 23 24.90 4.30 -2 0 -23 0.90 3.50 6 -1 -23 230.08 20.60 -6 1 23 241.28 20.80 5 -1 -23 171.98 14.80 -5 1 23 117.99 17.90 4 -1 -23 9.30 3.90 -4 1 23 12.60 4.40 3 -1 -23 19.10 4.80 -3 1 23 25.40 5.50 2 -1 -23 61.29 8.10 -2 1 23 64.79 8.80 1 -1 -23 20.50 4.60 -1 1 23 18.70 4.40 0 -1 -23 205.68 18.10 0 1 23 185.68 17.40 -1 -1 -23 520.75 42.50 1 1 23 485.45 42.20 5 -2 -23 46.90 6.90 -5 2 23 42.80 7.00 4 -2 -23 33.30 6.50 -4 2 23 27.00 6.00 3 -2 -23 32.40 5.30 -3 2 23 26.30 5.80 -2 2 23 13.10 4.40 -1 2 23 183.78 16.70 0 -2 -23 169.18 16.20 0 2 23 186.08 16.90 4 -3 -23 7.40 3.70 -4 3 23 4.70 3.20 3 -3 -23 7.50 3.80 -3 3 23 7.30 3.50 2 -3 -23 23.70 4.50 -2 3 23 20.30 4.20 1 -3 -23 87.49 9.60 -1 3 23 89.69 9.20 -2 -5 24 170.28 16.40 -4 -4 24 3.90 4.50 -3 -4 24 126.99 13.60 -2 -4 24 387.36 33.80 1 4 -24 90.29 9.60 -1 -4 24 112.39 11.50 0 4 -24 30.30 4.20 0 -4 24 26.90 5.20 -5 -3 24 4.50 3.70 4 3 -24 1.70 2.60 -4 -3 24 0.80 4.50 3 3 -24 35.10 5.40 -3 -3 24 33.00 6.40 2 3 -24 84.89 8.90 1 3 -24 15.50 3.70 -1 -3 24 15.20 5.40 0 3 -24 2.90 3.20 0 -3 24 2.50 4.10 5 2 -24 -0.20 2.60 -5 -2 24 2.80 4.10 4 2 -24 3.50 3.00 -4 -2 24 9.80 8.90 3 2 -24 82.69 9.00 -3 -2 24 89.79 10.70 2 2 -24 101.49 11.60 -2 -2 24 88.29 11.10 1 2 -24 7.30 3.60 -1 -2 24 -3.20 5.70 0 2 -24 0.60 3.30 0 -2 24 3.50 3.80 -1 2 -24 5.00 3.20 1 -2 24 3.10 3.20 5 1 -24 26.40 4.10 -5 -1 24 22.50 4.80 4 1 -24 25.80 4.10 -4 -1 24 9.50 5.70 -3 -1 24 291.37 25.80 -2 -1 24 227.98 20.90 -1 -1 24 30.10 6.50 0 1 -24 38.20 5.40 0 -1 24 33.40 5.30 -1 1 -24 9.40 3.80 1 -1 24 6.80 3.20 5 0 -24 93.19 9.60 -5 0 24 98.29 10.30 4 0 -24 3.00 3.40 -4 0 24 5.40 4.40 -3 0 24 38.10 7.30 1 0 -24 3.50 3.70 -1 0 24 4.20 4.20 0 0 -24 25.10 4.80 0 0 24 28.10 4.70 5 -1 -24 52.29 6.80 -5 1 24 56.69 7.40 4 -1 -24 241.78 21.60 -4 1 24 250.17 21.90 3 -1 -24 52.79 7.50 -3 1 24 54.19 7.90 2 -1 -24 24.00 4.50 -2 1 24 16.00 4.30 1 -1 -24 7.60 3.50 -1 1 24 5.90 3.50 0 -1 -24 18.10 4.30 0 1 24 20.10 3.80 4 -2 -24 65.99 8.10 -4 2 24 67.29 8.20 3 -2 -24 84.69 8.70 -3 2 24 68.99 8.70 2 -2 -24 145.69 13.80 -2 2 24 146.09 13.70 3 3 -25 53.79 7.40 2 3 -25 345.37 31.00 -2 -3 25 386.96 31.80 4 2 -25 16.00 3.40 -4 -2 25 25.30 5.10 3 2 -25 0.60 2.80 -3 -2 25 0.20 4.20 2 2 -25 109.69 10.80 -2 -2 25 112.39 11.80 1 2 -25 261.07 23.30 -1 -2 25 275.87 23.80 4 1 -25 40.30 6.20 -4 -1 25 53.29 7.40 3 1 -25 74.19 8.80 -3 -1 25 91.19 10.00 2 1 -25 3.00 3.20 -2 -1 25 3.30 3.80 1 1 -25 92.49 10.10 -1 -1 25 100.79 10.30 3 0 -25 7.50 3.30 -3 0 25 9.70 4.40 2 0 -25 19.70 4.10 -2 0 25 17.30 4.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 72008 _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 _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.58613(5) -0.07966(4) 0.37616(2) 0.04006(13) Uani 1 1 d . . . . . Br2 Br 0.72861(4) 0.03910(4) 0.23343(2) 0.04111(13) Uani 1 1 d . . . . . Br3 Br 0.33522(4) 0.23235(5) 0.11172(2) 0.04720(14) Uani 1 1 d . . . . . Ni1 Ni 0.57692(5) 0.11782(4) 0.31346(2) 0.02638(13) Uani 1 1 d . . . . . Ni2 Ni 0.58603(5) 0.23064(4) 0.17905(2) 0.02742(13) Uani 1 1 d . . . . . O1 O 0.5386(2) 0.2880(2) 0.26907(10) 0.0263(4) Uani 1 1 d . . . . . O2 O 0.3707(3) 0.0359(3) 0.25341(13) 0.0428(6) Uani 1 1 d . . . . . O3 O 0.6745(3) 0.1705(3) 0.09332(12) 0.0432(6) Uani 1 1 d . . . . . N1 N 0.7098(3) 0.2646(3) 0.38375(12) 0.0297(6) Uani 1 1 d . . . . . N2 N 0.7015(3) 0.4192(3) 0.20474(13) 0.0276(5) Uani 1 1 d . . . . . C1 C 0.6055(3) 0.4160(3) 0.30375(15) 0.0265(6) Uani 1 1 d . . . . . C2 C 0.7047(4) 0.3927(3) 0.37158(16) 0.0311(7) Uani 1 1 d . . . . . C3 C 0.7795(5) 0.5140(4) 0.42223(19) 0.0475(9) Uani 1 1 d . . . . . H3A H 0.779033 0.492065 0.466615 0.071 Uiso 1 1 calc R U . . . H3B H 0.725526 0.597415 0.414505 0.071 Uiso 1 1 calc R U . . . H3C H 0.882330 0.530954 0.418388 0.071 Uiso 1 1 calc R U . . . C4 C 0.7006(3) 0.4874(3) 0.26227(16) 0.0283(6) Uani 1 1 d . . . . . C5 C 0.7807(5) 0.6293(4) 0.28627(19) 0.0437(9) Uani 1 1 d . . . . . H5A H 0.878973 0.619183 0.313932 0.065 Uiso 1 1 calc R U . . . H5B H 0.722961 0.686043 0.312168 0.065 Uiso 1 1 calc R U . . . H5C H 0.792377 0.674911 0.248294 0.065 Uiso 1 1 calc R U . . . C6 C 0.4810(4) 0.5168(3) 0.31705(17) 0.0348(7) Uani 1 1 d . . . . . H6 H 0.530887 0.606888 0.342298 0.042 Uiso 1 1 calc R U . . . C7 C 0.3827(5) 0.5468(4) 0.2526(2) 0.0482(9) Uani 1 1 d . . . . . H7A H 0.345606 0.458746 0.224229 0.072 Uiso 1 1 calc R U . . . H7B H 0.440758 0.603367 0.230091 0.072 Uiso 1 1 calc R U . . . H7C H 0.298562 0.597541 0.261904 0.072 Uiso 1 1 calc R U . . . C8 C 0.3833(5) 0.4526(4) 0.3586(2) 0.0474(9) Uani 1 1 d . . . . . H8A H 0.308280 0.516801 0.366765 0.071 Uiso 1 1 calc R U . . . H8B H 0.445936 0.436148 0.400774 0.071 Uiso 1 1 calc R U . . . H8C H 0.333814 0.363988 0.334482 0.071 Uiso 1 1 calc R U . . . C9 C 0.7961(4) 0.2334(3) 0.44687(16) 0.0356(7) Uani 1 1 d . . . . . C10 C 0.7213(5) 0.2198(4) 0.49786(18) 0.0469(9) Uani 1 1 d . . . . . C11 C 0.8043(6) 0.1830(4) 0.55740(19) 0.0606(13) Uani 1 1 d . . . . . H11 H 0.757107 0.173543 0.592757 0.073 Uiso 1 1 calc R U . . . C12 C 0.9550(7) 0.1601(4) 0.5651(2) 0.0667(15) Uani 1 1 d . . . . . H12 H 1.009427 0.134945 0.605448 0.080 Uiso 1 1 calc R U . . . C13 C 1.0256(5) 0.1740(4) 0.5137(2) 0.0563(12) Uani 1 1 d . . . . . H13 H 1.127968 0.157777 0.519547 0.068 Uiso 1 1 calc R U . . . C14 C 0.9477(4) 0.2120(4) 0.45283(18) 0.0424(8) Uani 1 1 d . . . . . C15 C 1.0261(5) 0.2247(5) 0.3979(2) 0.0593(11) Uani 1 1 d . . . . . H15A H 0.974116 0.162541 0.358306 0.089 Uiso 1 1 calc R U . . . H15B H 1.128659 0.198789 0.411261 0.089 Uiso 1 1 calc R U . . . H15C H 1.026745 0.321123 0.388319 0.089 Uiso 1 1 calc R U . . . C16 C 0.5582(6) 0.2421(5) 0.4907(2) 0.0602(12) Uani 1 1 d . . . . . H16A H 0.543267 0.341611 0.490999 0.090 Uiso 1 1 calc R U . . . H16B H 0.523739 0.208629 0.527419 0.090 Uiso 1 1 calc R U . . . H16C H 0.501566 0.190446 0.448850 0.090 Uiso 1 1 calc R U . . . C17 C 0.7860(4) 0.4781(3) 0.16127(16) 0.0326(7) Uani 1 1 d . . . . . C18 C 0.9330(4) 0.4433(4) 0.16528(18) 0.0360(7) Uani 1 1 d . . . . . C19 C 1.0105(5) 0.4946(4) 0.1213(2) 0.0477(9) Uani 1 1 d . . . . . H19 H 1.110198 0.472250 0.123051 0.057 Uiso 1 1 calc R U . . . C20 C 0.9429(5) 0.5775(4) 0.0754(2) 0.0496(10) Uani 1 1 d . . . . . H20 H 0.996803 0.611636 0.046230 0.060 Uiso 1 1 calc R U . . . C21 C 0.7976(5) 0.6105(4) 0.0721(2) 0.0508(10) Uani 1 1 d . . . . . H21 H 0.752946 0.667596 0.040655 0.061 Uiso 1 1 calc R U . . . C22 C 0.7146(5) 0.5610(4) 0.11469(19) 0.0427(8) Uani 1 1 d . . . . . C23 C 0.5554(6) 0.5996(6) 0.1109(3) 0.0702(15) Uani 1 1 d . . . . . H23A H 0.554278 0.678795 0.144620 0.105 Uiso 1 1 calc R U . . . H23B H 0.495750 0.519808 0.118459 0.105 Uiso 1 1 calc R U . . . H23C H 0.513654 0.624957 0.067069 0.105 Uiso 1 1 calc R U . . . C24 C 1.0082(4) 0.3557(5) 0.2164(2) 0.0534(10) Uani 1 1 d . . . . . H24A H 1.093100 0.314327 0.202367 0.080 Uiso 1 1 calc R U . . . H24B H 0.937175 0.281559 0.220776 0.080 Uiso 1 1 calc R U . . . H24C H 1.043107 0.414709 0.258972 0.080 Uiso 1 1 calc R U . . . C25 C 0.2430(5) 0.0467(5) 0.2826(3) 0.0683(14) Uani 1 1 d . . . . . H25A H 0.190837 0.130794 0.271663 0.082 Uiso 1 1 calc R U . . . H25B H 0.273754 0.052170 0.331231 0.082 Uiso 1 1 calc R U . . . C26 C 0.1415(5) -0.0864(6) 0.2529(3) 0.0744(15) Uani 1 1 d . . . . . H26A H 0.163205 -0.161401 0.280883 0.089 Uiso 1 1 calc R U . . . H26B H 0.035219 -0.067758 0.247201 0.089 Uiso 1 1 calc R U . . . C27 C 0.1806(6) -0.1235(6) 0.1877(3) 0.0792(16) Uani 1 1 d . . . . . H27A H 0.127865 -0.067986 0.154444 0.095 Uiso 1 1 calc R U . . . H27B H 0.156653 -0.223862 0.171264 0.095 Uiso 1 1 calc R U . . . C28 C 0.3490(5) -0.0870(5) 0.2039(2) 0.0584(12) Uani 1 1 d . . . . . H28A H 0.404121 -0.164421 0.221700 0.070 Uiso 1 1 calc R U . . . H28B H 0.382590 -0.066068 0.164144 0.070 Uiso 1 1 calc R U . . . C29 C 0.7871(6) 0.0751(6) 0.0844(2) 0.0654(13) Uani 1 1 d . . . . . H29A H 0.745090 -0.022508 0.078052 0.079 Uiso 1 1 calc R U . . . H29B H 0.871349 0.088803 0.123499 0.079 Uiso 1 1 calc R U . . . C30 C 0.8389(6) 0.1071(7) 0.0234(2) 0.0762(15) Uani 1 1 d . . . . . H30A H 0.938713 0.157247 0.035983 0.091 Uiso 1 1 calc R U . . . H30B H 0.843436 0.020133 -0.006055 0.091 Uiso 1 1 calc R U . . . C31 C 0.7283(8) 0.1947(10) -0.0094(3) 0.117(3) Uani 1 1 d . . . . . H31A H 0.777017 0.285492 -0.012888 0.140 Uiso 1 1 calc R U . . . H31B H 0.681537 0.148731 -0.054500 0.140 Uiso 1 1 calc R U . . . C32 C 0.6157(6) 0.2162(5) 0.0290(2) 0.0603(12) Uani 1 1 d . . . . . H32A H 0.521942 0.161204 0.006257 0.072 Uiso 1 1 calc R U . . . H32B H 0.595483 0.315914 0.034822 0.072 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 Br1 0.0592(3) 0.0255(2) 0.0380(2) 0.01063(15) 0.01295(17) 0.00280(16) Br2 0.0511(2) 0.0381(2) 0.0434(2) 0.01283(16) 0.02317(17) 0.02128(17) Br3 0.0385(2) 0.0592(3) 0.0414(2) 0.00641(18) 0.00258(16) 0.01081(18) Ni1 0.0361(3) 0.0187(2) 0.0257(2) 0.00269(17) 0.01006(18) 0.00223(17) Ni2 0.0328(3) 0.0243(2) 0.0262(2) 0.00260(17) 0.00869(18) 0.00628(18) O1 0.0330(11) 0.0188(10) 0.0283(11) 0.0016(8) 0.0101(8) 0.0021(8) O2 0.0497(15) 0.0286(12) 0.0443(14) 0.0012(10) 0.0016(11) -0.0057(10) O3 0.0537(15) 0.0495(15) 0.0312(12) 0.0061(10) 0.0165(11) 0.0223(12) N1 0.0387(14) 0.0256(14) 0.0262(13) 0.0036(10) 0.0101(11) 0.0027(11) N2 0.0314(13) 0.0243(13) 0.0304(13) 0.0087(10) 0.0108(10) 0.0056(10) C1 0.0357(16) 0.0180(14) 0.0269(15) 0.0016(11) 0.0104(12) 0.0020(11) C2 0.0391(17) 0.0266(16) 0.0281(16) 0.0003(12) 0.0109(13) -0.0012(13) C3 0.072(3) 0.0267(18) 0.037(2) -0.0006(14) 0.0028(18) -0.0045(17) C4 0.0329(16) 0.0233(15) 0.0311(16) 0.0069(12) 0.0102(12) 0.0061(12) C5 0.056(2) 0.0302(18) 0.047(2) 0.0012(15) 0.0214(17) -0.0075(16) C6 0.0428(18) 0.0215(15) 0.0430(19) 0.0002(13) 0.0176(15) 0.0058(13) C7 0.050(2) 0.043(2) 0.061(3) 0.0189(18) 0.0210(18) 0.0213(17) C8 0.052(2) 0.043(2) 0.057(2) 0.0060(17) 0.0308(19) 0.0103(17) C9 0.050(2) 0.0233(16) 0.0288(16) 0.0024(12) 0.0015(14) -0.0043(14) C10 0.081(3) 0.0328(19) 0.0282(18) 0.0064(14) 0.0149(18) 0.0000(18) C11 0.107(4) 0.041(2) 0.028(2) 0.0066(16) 0.004(2) -0.005(2) C12 0.112(4) 0.037(2) 0.035(2) 0.0072(17) -0.017(2) -0.013(2) C13 0.065(3) 0.033(2) 0.054(3) 0.0055(17) -0.020(2) -0.0075(18) C14 0.052(2) 0.0273(17) 0.042(2) 0.0044(14) -0.0025(16) -0.0052(15) C15 0.045(2) 0.068(3) 0.064(3) 0.013(2) 0.0080(19) 0.007(2) C16 0.086(3) 0.061(3) 0.047(2) 0.019(2) 0.035(2) 0.010(2) C17 0.0425(18) 0.0306(17) 0.0277(16) 0.0062(12) 0.0132(13) 0.0021(13) C18 0.0351(17) 0.0364(18) 0.0389(18) 0.0046(14) 0.0143(14) -0.0003(14) C19 0.047(2) 0.048(2) 0.053(2) 0.0032(18) 0.0231(18) -0.0041(17) C20 0.067(3) 0.047(2) 0.041(2) 0.0047(16) 0.0267(19) -0.0093(19) C21 0.077(3) 0.044(2) 0.039(2) 0.0141(16) 0.0242(19) 0.006(2) C22 0.055(2) 0.041(2) 0.0390(19) 0.0147(15) 0.0187(16) 0.0093(17) C23 0.073(3) 0.088(4) 0.070(3) 0.052(3) 0.030(3) 0.040(3) C24 0.0334(19) 0.069(3) 0.065(3) 0.027(2) 0.0166(18) 0.0099(18) C25 0.043(2) 0.054(3) 0.094(4) -0.022(2) 0.002(2) 0.0159(19) C26 0.047(3) 0.072(3) 0.099(4) -0.001(3) 0.013(3) -0.008(2) C27 0.082(4) 0.075(4) 0.064(3) -0.003(3) -0.005(3) -0.028(3) C28 0.075(3) 0.046(2) 0.048(2) -0.0141(18) 0.017(2) -0.023(2) C29 0.072(3) 0.084(3) 0.051(2) 0.006(2) 0.028(2) 0.047(3) C30 0.073(3) 0.105(4) 0.059(3) -0.002(3) 0.037(3) 0.025(3) C31 0.113(5) 0.213(9) 0.064(4) 0.066(5) 0.060(4) 0.095(6) C32 0.083(3) 0.075(3) 0.032(2) 0.0169(19) 0.023(2) 0.030(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' Br Br -0.9338 1.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 _geom_angle_publ_flag Ni1 Br2 Ni2 77.619(17) . . ? Br1 Ni1 Br2 100.924(19) . . ? O1 Ni1 Br1 169.83(6) . . ? O1 Ni1 Br2 88.79(6) . . ? O1 Ni1 O2 85.46(9) . . ? O1 Ni1 N1 80.10(9) . . ? O2 Ni1 Br1 90.45(7) . . ? O2 Ni1 Br2 96.23(8) . . ? N1 Ni1 Br1 99.78(8) . . ? N1 Ni1 Br2 106.44(8) . . ? N1 Ni1 O2 152.70(11) . . ? Br3 Ni2 Br2 132.48(2) . . ? O1 Ni2 Br2 85.70(6) . . ? O1 Ni2 Br3 97.69(6) . . ? O1 Ni2 O3 170.29(9) . . ? O3 Ni2 Br2 87.97(7) . . ? O3 Ni2 Br3 92.02(7) . . ? N2 Ni2 Br2 112.06(7) . . ? N2 Ni2 Br3 115.21(7) . . ? N2 Ni2 O1 79.97(9) . . ? N2 Ni2 O3 95.64(10) . . ? Ni1 O1 Ni2 102.79(9) . . ? C1 O1 Ni1 117.77(18) . . ? C1 O1 Ni2 116.39(17) . . ? C25 O2 Ni1 116.8(2) . . ? C25 O2 C28 110.0(3) . . ? C28 O2 Ni1 125.0(3) . . ? C29 O3 Ni2 130.0(2) . . ? C29 O3 C32 107.0(3) . . ? C32 O3 Ni2 122.8(2) . . ? C2 N1 Ni1 116.1(2) . . ? C2 N1 C9 119.9(3) . . ? C9 N1 Ni1 123.8(2) . . ? C4 N2 Ni2 117.6(2) . . ? C4 N2 C17 120.2(3) . . ? C17 N2 Ni2 122.2(2) . . ? O1 C1 C2 109.8(2) . . ? O1 C1 C4 110.2(2) . . ? O1 C1 C6 109.8(2) . . ? C2 C1 C4 110.4(3) . . ? C2 C1 C6 108.5(2) . . ? C4 C1 C6 108.1(2) . . ? N1 C2 C1 116.1(3) . . ? N1 C2 C3 122.2(3) . . ? C3 C2 C1 121.5(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 C1 115.9(3) . . ? N2 C4 C5 122.3(3) . . ? C5 C4 C1 121.8(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6 108.5 . . ? C7 C6 C1 111.1(3) . . ? C7 C6 H6 108.5 . . ? C7 C6 C8 109.3(3) . . ? C8 C6 C1 110.7(3) . . ? C8 C6 H6 108.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 118.2(3) . . ? C14 C9 N1 118.5(3) . . ? C14 C9 C10 123.2(3) . . ? C9 C10 C16 122.7(3) . . ? C11 C10 C9 117.6(4) . . ? C11 C10 C16 119.7(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11 119.6 . . ? C11 C12 H12 119.9 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12 119.9 . . ? C12 C13 H13 119.3 . . ? C12 C13 C14 121.4(5) . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 116.8(4) . . ? C9 C14 C15 122.9(3) . . ? C13 C14 C15 120.3(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N2 118.4(3) . . ? C18 C17 C22 122.2(3) . . ? C22 C17 N2 119.3(3) . . ? C17 C18 C19 118.0(3) . . ? C17 C18 C24 121.3(3) . . ? C19 C18 C24 120.7(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.6 . . ? C19 C20 H20 119.9 . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.9 . . ? C20 C21 H21 119.4 . . ? C20 C21 C22 121.2(4) . . ? C22 C21 H21 119.4 . . ? C17 C22 C23 122.0(3) . . ? C21 C22 C17 117.5(4) . . ? C21 C22 C23 120.5(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 H25A 110.6 . . ? O2 C25 H25B 110.6 . . ? O2 C25 C26 105.6(4) . . ? H25A C25 H25B 108.7 . . ? C26 C25 H25A 110.6 . . ? C26 C25 H25B 110.6 . . ? C25 C26 H26A 111.2 . . ? C25 C26 H26B 111.2 . . ? H26A C26 H26B 109.1 . . ? C27 C26 C25 102.7(4) . . ? C27 C26 H26A 111.2 . . ? C27 C26 H26B 111.2 . . ? C26 C27 H27A 111.2 . . ? C26 C27 H27B 111.2 . . ? C26 C27 C28 102.7(4) . . ? H27A C27 H27B 109.1 . . ? C28 C27 H27A 111.2 . . ? C28 C27 H27B 111.2 . . ? O2 C28 C27 104.0(4) . . ? O2 C28 H28A 111.0 . . ? O2 C28 H28B 111.0 . . ? C27 C28 H28A 111.0 . . ? C27 C28 H28B 111.0 . . ? H28A C28 H28B 109.0 . . ? O3 C29 H29A 110.4 . . ? O3 C29 H29B 110.4 . . ? O3 C29 C30 106.6(4) . . ? H29A C29 H29B 108.6 . . ? C30 C29 H29A 110.4 . . ? C30 C29 H29B 110.4 . . ? C29 C30 H30A 110.6 . . ? C29 C30 H30B 110.6 . . ? H30A C30 H30B 108.8 . . ? C31 C30 C29 105.5(4) . . ? C31 C30 H30A 110.6 . . ? C31 C30 H30B 110.6 . . ? C30 C31 H31A 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? C32 C31 C30 108.9(4) . . ? C32 C31 H31A 109.9 . . ? C32 C31 H31B 109.9 . . ? O3 C32 H32A 110.3 . . ? O3 C32 H32B 110.3 . . ? C31 C32 O3 106.9(4) . . ? C31 C32 H32A 110.3 . . ? C31 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ni1 2.4215(5) . ? Br2 Ni1 2.4574(5) . ? Br2 Ni2 2.5337(5) . ? Br3 Ni2 2.4119(6) . ? Ni1 O1 1.979(2) . ? Ni1 O2 2.081(2) . ? Ni1 N1 2.040(3) . ? Ni2 O1 2.024(2) . ? Ni2 O3 2.137(2) . ? Ni2 N2 2.007(3) . ? O1 C1 1.388(3) . ? O2 C25 1.430(6) . ? O2 C28 1.441(4) . ? O3 C29 1.433(4) . ? O3 C32 1.453(5) . ? N1 C2 1.286(4) . ? N1 C9 1.446(4) . ? N2 C4 1.290(4) . ? N2 C17 1.458(4) . ? C1 C2 1.545(4) . ? C1 C4 1.546(4) . ? C1 C6 1.573(4) . ? C2 C3 1.497(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.493(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6 0.9900 . ? C6 C7 1.506(5) . ? C6 C8 1.530(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.396(5) . ? C9 C14 1.391(5) . ? C10 C11 1.395(6) . ? C10 C16 1.493(6) . ? C11 H11 0.9400 . ? C11 C12 1.383(8) . ? C12 H12 0.9400 . ? C12 C13 1.378(7) . ? C13 H13 0.9400 . ? C13 C14 1.406(5) . ? C14 C15 1.488(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.386(5) . ? C17 C22 1.396(5) . ? C18 C19 1.393(5) . ? C18 C24 1.500(5) . ? C19 H19 0.9400 . ? C19 C20 1.375(6) . ? C20 H20 0.9400 . ? C20 C21 1.368(6) . ? C21 H21 0.9400 . ? C21 C22 1.396(5) . ? C22 C23 1.505(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 C26 1.526(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 C27 1.478(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 C28 1.519(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 C30 1.505(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 C31 1.450(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 C32 1.440(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 O1 C1 C2 2.4(3) . . . . ? Ni1 O1 C1 C4 124.1(2) . . . . ? Ni1 O1 C1 C6 -116.9(2) . . . . ? Ni1 O2 C25 C26 -145.2(3) . . . . ? Ni1 O2 C28 C27 165.8(3) . . . . ? Ni1 N1 C2 C1 -3.3(4) . . . . ? Ni1 N1 C2 C3 171.7(3) . . . . ? Ni1 N1 C9 C10 -79.0(4) . . . . ? Ni1 N1 C9 C14 98.1(3) . . . . ? Ni2 O1 C1 C2 -120.4(2) . . . . ? Ni2 O1 C1 C4 1.4(3) . . . . ? Ni2 O1 C1 C6 120.4(2) . . . . ? Ni2 O3 C29 C30 -162.5(3) . . . . ? Ni2 O3 C32 C31 162.1(5) . . . . ? Ni2 N2 C4 C1 -1.7(3) . . . . ? Ni2 N2 C4 C5 -179.2(3) . . . . ? Ni2 N2 C17 C18 -87.1(3) . . . . ? Ni2 N2 C17 C22 89.5(3) . . . . ? O1 C1 C2 N1 0.7(4) . . . . ? O1 C1 C2 C3 -174.3(3) . . . . ? O1 C1 C4 N2 0.2(4) . . . . ? O1 C1 C4 C5 177.6(3) . . . . ? O1 C1 C6 C7 -61.5(3) . . . . ? O1 C1 C6 C8 60.2(4) . . . . ? O2 C25 C26 C27 -27.2(6) . . . . ? O3 C29 C30 C31 -13.9(7) . . . . ? N1 C9 C10 C11 176.9(3) . . . . ? N1 C9 C10 C16 -2.6(5) . . . . ? N1 C9 C14 C13 -176.5(3) . . . . ? N1 C9 C14 C15 2.2(5) . . . . ? N2 C17 C18 C19 177.0(3) . . . . ? N2 C17 C18 C24 -4.4(5) . . . . ? N2 C17 C22 C21 -177.4(3) . . . . ? N2 C17 C22 C23 4.1(6) . . . . ? C2 N1 C9 C10 95.4(4) . . . . ? C2 N1 C9 C14 -87.6(4) . . . . ? C2 C1 C4 N2 121.6(3) . . . . ? C2 C1 C4 C5 -60.9(4) . . . . ? C2 C1 C6 C7 178.5(3) . . . . ? C2 C1 C6 C8 -59.8(3) . . . . ? C4 N2 C17 C18 92.0(4) . . . . ? C4 N2 C17 C22 -91.4(4) . . . . ? C4 C1 C2 N1 -121.0(3) . . . . ? C4 C1 C2 C3 64.0(4) . . . . ? C4 C1 C6 C7 58.7(3) . . . . ? C4 C1 C6 C8 -179.5(3) . . . . ? C6 C1 C2 N1 120.7(3) . . . . ? C6 C1 C2 C3 -54.3(4) . . . . ? C6 C1 C4 N2 -119.8(3) . . . . ? C6 C1 C4 C5 57.7(4) . . . . ? C9 N1 C2 C1 -178.1(3) . . . . ? C9 N1 C2 C3 -3.2(5) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C10 C9 C14 C13 0.4(5) . . . . ? C10 C9 C14 C15 179.1(4) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C12 C13 C14 C9 -0.6(5) . . . . ? C12 C13 C14 C15 -179.3(4) . . . . ? C14 C9 C10 C11 0.0(5) . . . . ? C14 C9 C10 C16 -179.5(4) . . . . ? C16 C10 C11 C12 179.2(4) . . . . ? C17 N2 C4 C1 179.2(3) . . . . ? C17 N2 C4 C5 1.7(5) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C18 C17 C22 C21 -1.0(6) . . . . ? C18 C17 C22 C23 -179.5(4) . . . . ? C18 C19 C20 C21 -0.3(6) . . . . ? C19 C20 C21 C22 -0.2(6) . . . . ? C20 C21 C22 C17 0.8(6) . . . . ? C20 C21 C22 C23 179.4(4) . . . . ? C22 C17 C18 C19 0.5(5) . . . . ? C22 C17 C18 C24 179.1(4) . . . . ? C24 C18 C19 C20 -178.5(4) . . . . ? C25 O2 C28 C27 18.6(5) . . . . ? C25 C26 C27 C28 37.7(5) . . . . ? C26 C27 C28 O2 -35.3(5) . . . . ? C28 O2 C25 C26 5.0(5) . . . . ? C29 O3 C32 C31 -22.1(6) . . . . ? C29 C30 C31 C32 0.3(8) . . . . ? C30 C31 C32 O3 13.2(8) . . . . ? C32 O3 C29 C30 22.1(5) . . . . ?