#------------------------------------------------------------------------------ #$Date: 2024-07-29 00:37:59 +0300 (Mon, 29 Jul 2024) $ #$Revision: 293579 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/22/1572204.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_1572204 loop_ _publ_author_name 'Norouziyanlakvan, Somayeh' 'Ovens, Jeffrey S.' 'Richeson, Darrin' _publ_section_title ; Electrocatalytic Reduction of Nitrite to Ammonium Ion Using Ni(II) Complexes with Redox-Active Di(imino)pyridine Ligands. ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D4CY00715H _journal_year 2024 _chemical_formula_moiety 'C44 H49 Br2 Cl2 N3 Ni' _chemical_formula_sum 'C44 H49 Br2 Cl2 N3 Ni' _chemical_formula_weight 909.29 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_update_record ; 2024-07-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 93.325(2) _cell_angle_beta 107.464(2) _cell_angle_gamma 114.272(2) _cell_formula_units_Z 1 _cell_length_a 9.5290(6) _cell_length_b 9.7708(6) _cell_length_c 13.6707(9) _cell_measurement_reflns_used 9928 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 26.57 _cell_measurement_theta_min 2.34 _cell_volume 1082.49(12) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution ; SHELXT 2014/5 (Sheldrick, 2014) ; _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_unetI/netI 0.0609 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12372 _diffrn_reflns_point_group_measured_fraction_full 0.934 _diffrn_reflns_point_group_measured_fraction_max 0.908 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.576 _diffrn_reflns_theta_min 1.597 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.395 _exptl_crystal_description plate _exptl_crystal_F_000 466 _exptl_crystal_size_max 0.918 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.236 _refine_diff_density_max 0.743 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Flack x determined using 3246 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.034(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 8201 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0296 _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^)+(0.0170P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.0749 _reflns_Friedel_coverage 0.838 _reflns_Friedel_fraction_full 0.870 _reflns_Friedel_fraction_max 0.828 _reflns_number_gt 7740 _reflns_number_total 8201 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cy00715h2.cif _cod_data_source_block S0928 _cod_database_code 1572204 _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_shelxl_version_number 2018/3 _shelx_res_file ; TITL S0928 S0928_0m_a.res created by SHELXL-2018/3 at 12:50:05 on 23-Aug-2023 CELL 0.71073 9.5290 9.7708 13.6707 93.325 107.464 114.272 ZERR 1.000 0.0006 0.0006 0.0009 0.002 0.002 0.002 LATT -1 SFAC C H N Br Ni Cl UNIT 44 49 3 2 1 2 TEMP -70.000 SIZE 0.236 0.49 0.918 L.S. 10 BOND $H LIST 4 ACTA CONF EQIV $1 x, y+1, z HTAB C23 Br2_$1 HTAB C45 Br1 FMAP 2 PLAN 20 WGHT 0.017000 FVAR 0.75866 BR1 4 0.806832 0.655140 0.596941 11.00000 0.02703 0.03196 = 0.03268 0.00824 0.00903 0.00774 CL1 6 1.030320 0.882060 0.928799 11.00000 0.14234 0.13637 = 0.10904 -0.01927 0.00955 0.10318 NI1 5 0.521244 0.476625 0.489846 11.00000 0.02743 0.01673 = 0.02365 0.00548 0.01050 0.01207 N1 3 0.430017 0.438871 0.620094 11.00000 0.02216 0.01609 = 0.02266 0.00676 0.00786 0.00775 N2 3 0.459184 0.644570 0.504428 11.00000 0.02735 0.01722 = 0.02388 0.00501 0.01070 0.01218 CL2 6 0.767982 0.969999 0.884695 11.00000 0.12732 0.15806 = 0.08868 0.01020 0.00867 0.09772 N3 3 0.530121 0.565838 0.348462 11.00000 0.02802 0.02515 = 0.02336 0.00827 0.01308 0.01488 C1 1 0.381773 0.300952 0.663951 11.00000 0.02867 0.01708 = 0.02462 0.00688 0.01565 0.00933 C2 1 0.501721 0.278918 0.740950 11.00000 0.03159 0.02173 = 0.02922 0.00857 0.01694 0.01450 C3 1 0.449460 0.145249 0.780664 11.00000 0.04657 0.03354 = 0.03662 0.02037 0.02115 0.02688 AFIX 43 H3 2 0.526719 0.129008 0.833824 11.00000 -1.20000 AFIX 0 C4 1 0.287232 0.037419 0.743287 11.00000 0.05113 0.02701 = 0.05553 0.02050 0.03431 0.02149 AFIX 43 H4 2 0.254244 -0.051176 0.771424 11.00000 -1.20000 AFIX 0 C5 1 0.172841 0.058626 0.664807 11.00000 0.03316 0.02226 = 0.05132 0.00724 0.02390 0.00598 AFIX 43 H5 2 0.062759 -0.017425 0.638901 11.00000 -1.20000 AFIX 0 C6 1 0.215964 0.189792 0.622809 11.00000 0.02455 0.02329 = 0.03277 0.00589 0.01376 0.00903 C7 1 0.765315 0.318416 0.723659 11.00000 0.03166 0.04312 = 0.05023 0.00860 0.01751 0.01497 AFIX 137 H7A 2 0.714645 0.302635 0.648265 11.00000 -1.50000 H7B 2 0.751306 0.220802 0.742770 11.00000 -1.50000 H7C 2 0.881864 0.387866 0.745511 11.00000 -1.50000 AFIX 0 C8 1 0.684157 0.387173 0.777534 11.00000 0.02919 0.02553 = 0.03128 0.01081 0.00795 0.01254 AFIX 13 H8 2 0.695916 0.483941 0.753979 11.00000 -1.20000 AFIX 0 C9 1 0.770602 0.427163 0.896283 11.00000 0.04127 0.05672 = 0.03329 0.00782 0.00493 0.02330 AFIX 137 H9A 2 0.765220 0.334926 0.921372 11.00000 -1.50000 H9B 2 0.716630 0.470933 0.928793 11.00000 -1.50000 H9C 2 0.884938 0.501065 0.914214 11.00000 -1.50000 AFIX 0 C10 1 0.012010 0.074788 0.440496 11.00000 0.05032 0.08325 = 0.04238 -0.00341 0.00554 0.01636 AFIX 137 H10A 2 -0.064914 0.091157 0.383316 11.00000 -1.50000 H10B 2 -0.045059 -0.022683 0.458172 11.00000 -1.50000 H10C 2 0.100058 0.073657 0.419320 11.00000 -1.50000 AFIX 0 C11 1 0.084337 0.204236 0.536018 11.00000 0.02666 0.03232 = 0.05253 0.01174 0.01031 0.00356 AFIX 13 H11 2 0.135330 0.303163 0.515207 11.00000 -1.20000 AFIX 0 C12 1 -0.051088 0.204413 0.574143 11.00000 0.03116 0.06670 = 0.07912 0.01187 0.01542 0.02531 AFIX 137 H12A 2 -0.128184 0.225227 0.520133 11.00000 -1.50000 H12B 2 -0.002122 0.283182 0.637274 11.00000 -1.50000 H12C 2 -0.108789 0.104943 0.589185 11.00000 -1.50000 AFIX 0 C13 1 0.344928 0.565952 0.738791 11.00000 0.03359 0.01725 = 0.02439 0.00486 0.01475 0.01065 C14 1 0.429139 0.558338 0.839212 11.00000 0.05408 0.03623 = 0.02886 0.01020 0.01658 0.02830 AFIX 43 H14 2 0.516959 0.532785 0.851247 11.00000 -1.20000 AFIX 0 C15 1 0.382253 0.588828 0.921452 11.00000 0.07800 0.04978 = 0.02601 0.01314 0.02279 0.03558 AFIX 43 H15 2 0.438756 0.583965 0.989525 11.00000 -1.20000 AFIX 0 C16 1 0.253315 0.626239 0.904094 11.00000 0.06732 0.04179 = 0.04668 0.00859 0.03723 0.02719 AFIX 43 H16 2 0.223199 0.647474 0.960516 11.00000 -1.20000 AFIX 0 C17 1 0.169276 0.632629 0.805704 11.00000 0.04690 0.03001 = 0.05360 0.00890 0.03219 0.01555 AFIX 43 H17 2 0.081811 0.658552 0.794465 11.00000 -1.20000 AFIX 0 C18 1 0.212694 0.601058 0.722813 11.00000 0.03279 0.02379 = 0.03393 0.00688 0.01402 0.01193 AFIX 43 H18 2 0.152784 0.603147 0.654820 11.00000 -1.20000 AFIX 0 C19 1 0.402851 0.548731 0.651331 11.00000 0.02225 0.01968 = 0.02172 0.00383 0.00749 0.00781 C20 1 0.435611 0.676872 0.591980 11.00000 0.02613 0.01859 = 0.02275 0.00320 0.01005 0.01022 C21 1 0.444944 0.818875 0.624180 11.00000 0.04562 0.02311 = 0.02885 0.00541 0.01850 0.01997 AFIX 43 H21 2 0.428419 0.841147 0.686436 11.00000 -1.20000 AFIX 0 C22 1 0.479102 0.926616 0.562508 11.00000 0.05360 0.02089 = 0.03980 0.00808 0.02316 0.02117 AFIX 43 H22 2 0.485018 1.023215 0.582091 11.00000 -1.20000 AFIX 0 C23 1 0.504501 0.891486 0.471902 11.00000 0.04741 0.02089 = 0.03033 0.01219 0.01857 0.01868 AFIX 43 H23 2 0.529779 0.964446 0.429987 11.00000 -1.20000 AFIX 0 C24 1 0.492310 0.748051 0.443714 11.00000 0.02650 0.01844 = 0.02659 0.00790 0.01067 0.01076 C25 1 0.515105 0.690348 0.348536 11.00000 0.02504 0.02272 = 0.01981 0.00511 0.00626 0.01012 C26 1 0.512235 0.780134 0.263682 11.00000 0.03980 0.02259 = 0.02226 0.00801 0.01093 0.01471 C27 1 0.393187 0.833055 0.231782 11.00000 0.05176 0.04422 = 0.04297 0.01787 0.02015 0.03196 AFIX 43 H27 2 0.309888 0.806048 0.260666 11.00000 -1.20000 AFIX 0 C28 1 0.396555 0.924560 0.158319 11.00000 0.08183 0.05759 = 0.04307 0.02004 0.01196 0.04965 AFIX 43 H28 2 0.317516 0.961529 0.138549 11.00000 -1.20000 AFIX 0 C29 1 0.515407 0.961023 0.114560 11.00000 0.10185 0.04201 = 0.04091 0.02210 0.02498 0.02964 AFIX 43 H29 2 0.516364 1.021351 0.063416 11.00000 -1.20000 AFIX 0 C30 1 0.635102 0.909548 0.145112 11.00000 0.07108 0.03644 = 0.04702 0.01836 0.03404 0.00950 AFIX 43 H30 2 0.717652 0.936473 0.115590 11.00000 -1.20000 AFIX 0 C31 1 0.632037 0.818072 0.219534 11.00000 0.04192 0.03037 = 0.02990 0.00904 0.01449 0.01404 AFIX 43 H31 2 0.711891 0.782112 0.239707 11.00000 -1.20000 AFIX 0 C32 1 0.523407 0.483170 0.253988 11.00000 0.03124 0.02240 = 0.02333 0.00665 0.01171 0.01355 C33 1 0.669896 0.493482 0.243461 11.00000 0.03973 0.03695 = 0.03313 0.01175 0.01957 0.02533 C34 1 0.653360 0.411151 0.150268 11.00000 0.05906 0.05647 = 0.04296 0.01314 0.03007 0.03941 AFIX 43 H34 2 0.748459 0.416802 0.139690 11.00000 -1.20000 AFIX 0 C35 1 0.501684 0.321862 0.073360 11.00000 0.07805 0.04204 = 0.03234 0.00846 0.02648 0.03549 AFIX 43 H35 2 0.494217 0.270866 0.010171 11.00000 -1.20000 AFIX 0 C36 1 0.362550 0.308096 0.089669 11.00000 0.05453 0.02941 = 0.03058 0.00322 0.01680 0.01681 AFIX 43 H36 2 0.259443 0.242638 0.038408 11.00000 -1.20000 AFIX 0 C37 1 0.368051 0.387755 0.179723 11.00000 0.04022 0.02488 = 0.02748 0.00809 0.01250 0.01225 C38 1 0.969092 0.689521 0.288816 11.00000 0.04125 0.09387 = 0.07846 0.00018 0.03011 0.02673 AFIX 137 H38A 2 0.997225 0.628437 0.246878 11.00000 -1.50000 H38B 2 1.066411 0.757019 0.348473 11.00000 -1.50000 H38C 2 0.927648 0.750440 0.246506 11.00000 -1.50000 AFIX 0 C39 1 0.835966 0.582823 0.327787 11.00000 0.03904 0.06442 = 0.04894 0.00260 0.01917 0.02788 AFIX 13 H39 2 0.823648 0.648431 0.379318 11.00000 -1.20000 AFIX 0 C40 1 0.892627 0.476345 0.385215 11.00000 0.06846 0.12200 = 0.05195 0.02082 0.01768 0.07044 AFIX 137 H40A 2 0.807069 0.408267 0.408375 11.00000 -1.50000 H40B 2 0.992125 0.536458 0.445555 11.00000 -1.50000 H40C 2 0.914988 0.416092 0.338507 11.00000 -1.50000 AFIX 0 C41 1 0.111038 0.421699 0.112684 11.00000 0.04495 0.07525 = 0.05534 0.00363 0.01296 0.03344 AFIX 137 H41A 2 0.088403 0.369861 0.043024 11.00000 -1.50000 H41B 2 0.174551 0.531416 0.120642 11.00000 -1.50000 H41C 2 0.007967 0.400884 0.122404 11.00000 -1.50000 AFIX 0 C42 1 0.207488 0.364218 0.193303 11.00000 0.03536 0.05521 = 0.02976 -0.00107 0.01166 0.01138 AFIX 13 H42 2 0.234771 0.422933 0.263444 11.00000 -1.20000 AFIX 0 C43 1 0.099114 0.191798 0.188424 11.00000 0.04388 0.08186 = 0.05384 0.01870 0.01501 0.00151 AFIX 137 H43A 2 0.056906 0.134242 0.117229 11.00000 -1.50000 H43B 2 0.007792 0.181677 0.210010 11.00000 -1.50000 H43C 2 0.165131 0.152060 0.234993 11.00000 -1.50000 AFIX 0 C45 1 0.905769 0.936399 0.839475 11.00000 0.12081 0.15420 = 0.05437 -0.00386 0.02476 0.05891 AFIX 23 H45A 2 0.843516 0.855898 0.775515 11.00000 -1.20000 H45B 2 0.974378 1.030103 0.821211 11.00000 -1.20000 AFIX 0 BR2 4 0.458560 0.222877 0.423415 11.00000 0.07247 0.02384 = 0.03716 0.00872 0.02157 0.02878 HKLF 4 REM S0928 REM wR2 = 0.0749, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0296 for 7740 Fo > 4sig(Fo) and 0.0321 for all 8201 data REM 477 parameters refined using 3 restraints END WGHT 0.0170 0.0000 REM Highest difference peak 0.743, deepest hole -0.569, 1-sigma level 0.056 Q1 1 0.8916 1.0588 0.8604 11.00000 0.05 0.74 Q2 1 0.9226 0.8141 0.9743 11.00000 0.05 0.65 Q3 1 0.7645 0.8760 0.8744 11.00000 0.05 0.40 Q4 1 0.4420 1.0846 0.2221 11.00000 0.05 0.35 Q5 1 0.0971 0.6572 0.0562 11.00000 0.05 0.33 Q6 1 0.5766 1.1683 0.2019 11.00000 0.05 0.29 Q7 1 0.3662 0.8221 0.1601 11.00000 0.05 0.28 Q8 1 0.3426 1.0704 0.0451 11.00000 0.05 0.28 Q9 1 0.8313 0.8455 0.8701 11.00000 0.05 0.26 Q10 1 0.5629 0.4173 0.2589 11.00000 0.05 0.25 Q11 1 0.5454 0.2738 0.3119 11.00000 0.05 0.25 Q12 1 1.0355 0.8997 1.0023 11.00000 0.05 0.24 Q13 1 0.4873 0.2185 0.3579 11.00000 0.05 0.23 Q14 1 0.5933 0.3404 0.7737 11.00000 0.05 0.23 Q15 1 0.5093 0.5548 0.4113 11.00000 0.05 0.23 Q16 1 0.8662 0.6774 0.5126 11.00000 0.05 0.22 Q17 1 0.2630 0.2380 0.1524 11.00000 0.05 0.22 Q18 1 0.5940 0.4284 0.4049 11.00000 0.05 0.22 Q19 1 0.8222 0.5741 0.6619 11.00000 0.05 0.22 Q20 1 0.7758 0.5469 0.5916 11.00000 0.05 0.22 ; _shelx_res_checksum 66639 _shelx_hkl_file ; -1 0 0 6779.82 424.16 -1 0 0 6272.37 425.26 1 0 0 6239.48 429.66 1 0 0 5910.41 425.86 1 0 0 6073.89 409.16 -2 0 0 4689.83 308.17 -2 0 0 4485.45 307.87 2 0 0 4792.82 308.97 2 0 0 4736.93 308.27 2 0 0 4772.52 307.87 -3 0 0 6225.08 375.66 -3 0 0 5789.92 374.46 3 0 0 4924.71 375.66 3 0 0 5707.43 375.16 3 0 0 5936.41 375.06 -4 0 0 1312.27 78.59 -4 0 0 1299.17 78.69 4 0 0 1170.78 78.59 4 0 0 1035.40 78.89 4 0 0 1150.48 78.59 -5 0 0 76.39 6.50 5 0 0 88.59 7.10 5 0 0 80.99 7.20 5 0 0 94.49 7.00 -6 0 0 285.07 22.70 6 0 0 357.16 23.30 6 0 0 342.77 23.50 6 0 0 364.66 23.30 -7 0 0 468.15 32.10 -7 0 0 473.55 33.50 7 0 0 487.05 32.60 7 0 0 461.45 32.80 7 0 0 492.15 32.70 -8 0 0 81.79 9.40 8 0 0 55.09 7.30 8 0 0 58.59 7.60 -9 0 0 -0.60 4.80 9 0 0 1.70 3.50 -10 0 0 49.20 10.50 10 0 0 61.19 8.40 10 -1 0 76.49 8.60 -10 1 0 64.69 11.30 9 -1 0 24.10 6.80 9 -1 0 26.00 5.90 -9 1 0 36.20 9.00 8 -1 0 193.88 14.80 8 -1 0 188.88 14.40 -8 1 0 189.78 13.70 -8 1 0 183.18 16.10 7 -1 0 701.63 44.90 7 -1 0 684.23 44.90 7 -1 0 693.33 44.90 -7 1 0 589.84 44.40 6 -1 0 84.29 7.20 6 -1 0 89.09 7.20 6 -1 0 87.29 7.50 -6 1 0 78.79 6.90 5 -1 0 787.02 51.89 5 -1 0 795.22 51.79 5 -1 0 804.82 51.99 -5 1 0 782.42 51.79 -5 1 0 736.33 51.69 4 -1 0 616.64 41.70 4 -1 0 611.54 41.80 4 -1 0 629.44 41.90 -4 1 0 545.55 41.90 -4 1 0 680.23 41.80 -4 1 0 696.63 41.70 3 -1 0 1348.67 89.09 3 -1 0 1331.17 89.49 3 -1 0 1286.97 88.99 -3 1 0 1384.66 88.99 -3 1 0 1418.56 89.29 -3 1 0 1377.46 89.09 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-2 0 8.00 3.70 10 -2 0 4.60 4.20 -10 2 0 7.00 5.80 9 -2 0 188.48 14.20 9 -2 0 182.58 14.70 -9 2 0 168.78 16.40 8 -2 0 1062.99 68.79 8 -2 0 1043.90 68.89 -8 2 0 989.10 68.39 7 -2 0 151.68 10.80 7 -2 0 143.69 11.20 7 -2 0 146.19 10.70 -7 2 0 119.69 10.50 6 -2 0 561.44 39.40 6 -2 0 575.54 39.50 6 -2 0 595.74 39.40 -6 2 0 621.74 39.70 5 -2 0 1451.05 95.79 5 -2 0 1485.55 95.59 5 -2 0 1424.06 95.69 -5 2 0 1457.45 95.59 -5 2 0 1453.35 96.09 4 -2 0 233.08 14.20 4 -2 0 222.78 14.40 4 -2 0 221.88 14.50 -4 2 0 185.68 14.00 -4 2 0 190.48 14.40 -4 2 0 191.38 14.30 -3 2 0 132.49 9.30 -3 2 0 131.49 9.40 -3 2 0 131.29 9.00 2 -2 0 2146.69 138.79 2 -2 0 2168.68 138.89 -2 2 0 2055.49 138.59 -2 2 0 2097.79 138.19 -2 2 0 2079.89 138.59 -2 2 0 2112.49 138.29 1 -2 0 1405.26 89.19 1 -2 0 1450.95 89.39 1 -2 0 1226.48 89.29 -1 2 0 1411.96 89.29 -1 2 0 1293.67 89.39 -1 2 0 1384.86 89.09 0 -2 0 143.59 9.60 0 -2 0 135.19 9.80 -1 -2 0 147.79 10.20 -1 -2 0 141.49 10.00 -2 -2 0 132.39 9.40 -2 -2 0 131.89 9.30 -2 -2 0 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120.29 11.80 -6 -1 14 126.89 12.30 5 1 -14 101.79 11.10 5 1 -14 99.49 10.20 -5 -1 14 93.59 10.80 4 1 -14 21.10 4.70 4 1 -14 17.90 5.10 -4 -1 14 14.50 4.90 3 1 -14 59.69 9.70 3 1 -14 57.69 8.10 -3 -1 14 48.70 8.60 2 1 -14 71.59 10.50 2 1 -14 65.59 8.30 -2 -1 14 70.29 9.10 1 1 -14 118.49 13.30 -1 -1 14 117.99 11.60 0 -1 14 60.49 8.90 -1 1 -14 0.20 5.20 1 -1 14 -2.80 4.10 -2 1 -14 76.09 12.30 2 -1 14 81.29 10.20 3 -1 14 92.59 11.50 9 0 -14 77.19 13.60 -9 0 14 49.90 11.90 8 0 -14 9.70 5.40 -8 0 14 15.80 5.30 7 0 -14 46.40 8.90 -7 0 14 48.60 8.80 6 0 -14 22.70 5.30 6 0 -14 19.90 5.80 -6 0 14 18.40 5.20 5 0 -14 124.39 11.90 5 0 -14 117.59 11.10 -5 0 14 104.49 11.60 4 0 -14 124.09 11.30 4 0 -14 126.39 12.20 -4 0 14 87.29 11.20 3 0 -14 55.39 9.40 3 0 -14 51.09 8.20 -3 0 14 46.90 8.60 2 0 -14 374.06 26.90 2 0 -14 353.56 25.10 -2 0 14 330.47 25.60 -2 0 14 344.77 25.10 1 0 -14 351.56 24.90 -1 0 14 299.67 23.30 -1 0 14 292.17 22.30 0 0 -14 22.60 6.10 0 0 14 26.60 7.40 -1 0 -14 163.98 16.60 1 0 14 178.78 15.20 -2 0 -14 264.17 22.50 2 0 14 260.57 20.70 9 -1 -14 80.69 11.60 -9 1 14 84.99 11.50 8 -1 -14 61.69 9.80 -8 1 14 43.40 8.80 7 -1 -14 6.30 4.80 -7 1 14 2.80 4.40 6 -1 -14 202.38 16.30 6 -1 -14 182.78 15.80 -6 1 14 208.58 16.60 5 -1 -14 348.27 25.00 5 -1 -14 339.57 24.80 -5 1 14 315.77 24.90 4 -1 -14 130.49 12.80 4 -1 -14 120.69 12.20 -4 1 14 125.39 12.40 3 -1 -14 300.97 22.70 3 -1 -14 262.57 21.40 -3 1 14 292.47 22.10 -3 1 14 296.87 21.80 2 -1 -14 235.98 19.90 -2 1 14 234.38 18.50 -2 1 14 241.68 18.20 1 -1 -14 35.60 9.60 -1 1 14 30.10 7.30 -1 1 14 27.10 6.40 0 -1 -14 85.79 12.20 0 1 14 91.99 10.20 -1 -1 -14 113.49 14.70 1 1 14 152.08 13.20 2 1 14 18.30 5.40 9 -2 -14 115.59 12.50 -9 2 14 105.69 12.70 8 -2 -14 11.10 5.50 -8 2 14 15.30 5.10 7 -2 -14 241.58 20.80 -7 2 14 288.17 21.10 6 -2 -14 251.87 22.30 6 -2 -14 337.67 23.40 -6 2 14 333.57 23.30 5 -2 -14 17.20 4.90 5 -2 -14 18.80 5.50 -5 2 14 31.40 7.50 4 -2 -14 301.17 23.60 4 -2 -14 304.67 23.00 -4 2 14 317.67 23.40 3 -2 -14 184.68 16.00 -3 2 14 159.58 14.80 -3 2 14 173.88 14.70 2 -2 -14 3.20 4.70 -2 2 14 5.80 4.00 -2 2 14 -0.30 3.70 1 -2 -14 81.59 11.80 -1 2 14 86.59 9.70 -1 2 14 80.79 9.30 0 -2 -14 73.09 11.70 0 2 14 68.19 9.10 -1 -2 -14 34.30 11.80 1 2 14 37.30 8.30 9 -3 -14 3.50 5.50 -9 3 14 -0.10 5.10 8 -3 -14 76.49 11.30 -8 3 14 72.39 10.00 7 -3 -14 130.19 13.30 -7 3 14 102.69 11.80 6 -3 -14 -3.80 3.20 6 -3 -14 -3.90 4.90 -6 3 14 1.90 4.20 5 -3 -14 88.39 10.50 5 -3 -14 63.19 9.30 -4 3 14 76.59 9.90 -4 3 14 68.69 9.50 3 -3 -14 82.19 10.90 -3 3 14 71.99 9.60 -3 3 14 74.49 9.70 2 -3 -14 22.30 6.10 -2 3 14 23.90 7.10 -2 3 14 20.30 5.00 1 -3 -14 14.70 6.00 -1 3 14 20.90 4.90 -1 3 14 18.90 4.80 0 -3 -14 81.09 12.10 0 3 14 63.89 9.30 9 -4 -14 15.10 7.50 8 -4 -14 55.39 10.90 -8 4 14 51.69 9.10 7 -4 -14 9.40 5.80 -7 4 14 5.30 4.60 6 -4 -14 18.00 4.90 6 -4 -14 22.70 6.10 -6 4 14 16.40 5.20 5 -4 -14 4.70 5.30 5 -4 -14 -0.20 3.90 -5 4 14 11.20 5.20 -5 4 14 5.90 4.50 -4 4 14 95.29 10.80 -4 4 14 95.79 11.10 3 -4 -14 70.89 10.80 -3 4 14 76.59 9.50 -3 4 14 75.29 10.00 2 -4 -14 10.40 5.40 -2 4 14 10.20 4.40 -2 4 14 11.00 4.80 1 -4 -14 122.99 14.50 -1 4 14 139.29 12.60 -1 4 14 136.79 12.90 8 -5 -14 53.59 10.80 -8 5 14 57.29 9.40 7 -5 -14 71.69 11.30 -7 5 14 65.29 9.70 6 -5 -14 36.40 9.80 6 -5 -14 42.20 9.20 -6 5 14 45.40 8.50 -6 5 14 47.10 9.80 5 -5 -14 193.08 17.80 -5 5 14 215.98 17.80 -5 5 14 208.18 17.20 4 -5 -14 101.69 13.70 -4 5 14 153.28 13.20 -4 5 14 150.08 13.70 3 -5 -14 6.80 5.60 -3 5 14 22.40 5.80 -3 5 14 18.60 4.70 2 -5 -14 110.69 14.90 -2 5 14 159.18 13.90 -2 5 14 149.69 12.80 7 -6 -14 5.90 6.10 -7 6 14 5.30 5.00 -7 6 14 6.40 5.50 6 -6 -14 107.49 13.10 -6 6 14 123.19 12.20 -6 6 14 119.39 13.30 5 -6 -14 120.99 14.40 -5 6 14 147.49 13.30 -5 6 14 137.39 14.20 4 -6 -14 3.70 5.50 -4 6 14 9.90 4.70 -4 6 14 15.20 5.60 3 6 -15 73.59 13.30 -3 -6 15 54.69 9.60 2 6 -15 42.20 12.60 -2 -6 15 39.60 8.70 1 6 -15 17.10 7.60 -1 -6 15 15.30 5.40 0 6 -15 24.60 8.30 0 -6 15 19.10 5.70 1 -6 15 7.40 5.20 4 5 -15 24.00 7.00 -4 -5 15 26.40 5.90 3 5 -15 36.80 11.40 -3 -5 15 21.80 5.60 2 5 -15 82.79 13.40 -2 -5 15 49.20 9.40 1 5 -15 72.29 14.10 -1 -5 15 50.49 9.30 0 5 -15 12.80 7.80 0 -5 15 13.20 5.20 -1 5 -15 94.99 16.30 1 -5 15 88.79 11.50 5 4 -15 36.40 8.90 -5 -4 15 36.80 9.00 4 4 -15 2.90 5.60 4 4 -15 -0.20 6.00 -4 -4 15 4.40 4.70 3 4 -15 195.88 19.60 -3 -4 15 213.88 17.30 2 4 -15 71.69 13.50 -2 -4 15 77.39 10.10 1 4 -15 13.20 7.30 -1 -4 15 21.00 5.40 0 4 -15 141.09 18.30 0 -4 15 178.08 15.00 -1 4 -15 79.49 15.30 6 3 -15 30.30 8.80 -6 -3 15 29.80 8.50 5 3 -15 13.10 5.00 -5 -3 15 5.30 4.90 4 3 -15 152.88 12.90 4 3 -15 130.59 15.90 -4 -3 15 169.48 14.60 3 3 -15 92.29 13.30 -3 -3 15 82.59 10.60 2 3 -15 7.50 6.20 -2 -3 15 1.60 4.40 1 3 -15 136.19 17.00 -1 -3 15 163.78 14.30 0 3 -15 85.19 14.60 0 -3 15 105.49 11.30 -1 3 -15 1.50 6.60 1 -3 15 5.10 4.90 7 2 -15 81.59 11.00 -7 -2 15 66.59 10.30 6 2 -15 14.50 5.20 -6 -2 15 12.70 5.10 5 2 -15 95.99 10.30 5 2 -15 91.99 11.80 -5 -2 15 84.99 10.90 4 2 -15 118.19 13.80 4 2 -15 127.19 11.70 -4 -2 15 124.49 12.80 3 2 -15 23.20 5.20 3 2 -15 23.10 6.50 -3 -2 15 14.40 5.10 2 2 -15 51.69 11.50 -2 -2 15 59.49 9.20 1 2 -15 69.49 12.50 -1 -2 15 73.09 9.80 0 2 -15 112.69 14.10 0 -2 15 90.69 11.20 -1 2 -15 18.20 6.90 1 -2 15 6.20 4.90 2 -2 15 54.99 10.60 7 1 -15 1.30 5.20 -7 -1 15 0.10 4.50 6 1 -15 66.29 9.60 -6 -1 15 61.69 9.80 5 1 -15 23.60 5.70 5 1 -15 36.60 8.10 -5 -1 15 32.80 8.40 4 1 -15 42.90 8.20 4 1 -15 34.10 8.70 -4 -1 15 22.10 5.90 3 1 -15 12.90 4.70 3 1 -15 10.50 5.10 -3 -1 15 15.30 5.00 2 1 -15 77.99 11.30 -2 -1 15 76.69 9.90 1 1 -15 150.78 15.30 -1 -1 15 143.59 13.60 0 1 -15 63.09 11.60 0 -1 15 67.69 9.70 -1 1 -15 18.10 6.60 1 -1 15 17.60 5.50 8 0 -15 7.40 5.60 -8 0 15 3.60 5.30 7 0 -15 8.30 5.30 -7 0 15 11.80 5.20 6 0 -15 21.50 5.70 -6 0 15 23.90 5.90 5 0 -15 61.79 9.70 5 0 -15 82.39 10.00 -5 0 15 63.69 9.90 4 0 -15 40.60 8.50 4 0 -15 37.90 9.10 -4 0 15 43.40 8.90 3 0 -15 51.39 7.90 3 0 -15 46.50 9.70 -3 0 15 33.30 8.40 2 0 -15 171.68 15.80 -2 0 15 154.28 13.60 -2 0 15 155.18 14.30 1 0 -15 118.49 13.20 -1 0 15 101.29 11.50 0 0 -15 20.30 6.30 0 0 15 24.10 5.60 -1 0 -15 151.98 17.70 1 0 15 176.38 15.30 8 -1 -15 10.10 5.60 -8 1 15 0.90 4.80 7 -1 -15 45.90 9.30 -7 1 15 43.40 9.00 6 -1 -15 211.98 17.30 -6 1 15 191.38 17.10 5 -1 -15 95.79 11.10 5 -1 -15 104.09 11.50 -5 1 15 73.29 10.90 4 -1 -15 137.99 13.60 4 -1 -15 129.99 12.90 -4 1 15 128.19 13.20 3 -1 -15 320.87 23.30 -3 1 15 277.07 22.20 -3 1 15 271.17 21.90 2 -1 -15 236.08 18.90 -2 1 15 196.28 16.60 -2 1 15 201.28 17.20 1 -1 -15 39.80 10.30 -1 1 15 41.00 8.30 0 -1 -15 73.59 12.00 0 1 15 67.89 9.50 1 1 15 21.80 5.80 8 -2 -15 36.80 10.00 -8 2 15 37.40 9.10 7 -2 -15 100.09 12.60 -7 2 15 113.39 12.10 6 -2 -15 75.19 10.40 6 -2 -15 107.39 12.10 -6 2 15 111.39 11.50 5 -2 -15 24.00 6.20 5 -2 -15 19.00 5.30 -5 2 15 40.70 8.60 4 -2 -15 103.59 12.30 4 -2 -15 95.99 11.80 -4 2 15 124.69 12.20 -4 2 15 117.39 12.00 3 -2 -15 31.50 9.60 -3 2 15 52.59 8.40 -3 2 15 52.29 8.80 2 -2 -15 13.40 5.60 -2 2 15 10.60 4.70 -2 2 15 9.90 4.30 1 -2 -15 64.89 11.60 -1 2 15 83.89 9.80 0 2 15 12.50 4.90 8 -3 -15 46.20 10.80 -8 3 15 50.89 11.00 7 -3 -15 20.60 6.60 -7 3 15 24.40 6.00 6 -3 -15 12.90 5.90 6 -3 -15 3.10 4.10 -6 3 15 8.80 5.10 5 -3 -15 24.50 8.20 5 -3 -15 32.40 9.30 -5 3 15 32.30 8.50 -5 3 15 33.30 9.10 4 -3 -15 -2.40 4.30 -4 3 15 2.00 4.50 -4 3 15 3.60 4.70 3 -3 -15 99.39 12.30 -3 3 15 99.39 10.90 -3 3 15 91.89 10.90 2 -3 -15 7.60 5.50 -2 3 15 10.50 4.70 -2 3 15 6.90 4.70 1 -3 -15 20.40 6.90 -1 3 15 34.00 8.00 8 -4 -15 14.10 6.60 7 -4 -15 52.09 11.00 -7 4 15 38.00 9.40 6 -4 -15 8.30 5.90 6 -4 -15 2.60 4.40 -6 4 15 8.70 5.40 -6 4 15 4.40 4.70 5 -4 -15 22.70 5.90 -5 4 15 38.80 8.90 -5 4 15 39.10 8.80 4 -4 -15 173.48 16.60 -4 4 15 186.18 15.90 -4 4 15 173.78 15.80 3 -4 -15 53.99 10.70 -3 4 15 50.29 9.20 -3 4 15 56.99 8.90 2 -4 -15 20.90 7.70 -2 4 15 27.90 8.10 -2 4 15 37.80 7.80 7 -5 -15 70.79 11.90 -7 5 15 62.69 10.10 -7 5 15 60.59 11.20 6 -5 -15 83.79 11.90 -6 5 15 106.39 11.80 -6 5 15 101.49 12.20 -5 5 15 214.98 18.50 -5 5 15 223.78 19.00 4 -5 -15 65.59 12.00 -4 5 15 98.19 11.30 -4 5 15 94.79 11.00 2 5 -16 21.80 8.00 -2 -5 16 21.10 5.90 1 5 -16 9.30 7.50 -1 -5 16 12.40 5.90 4 4 -16 127.29 15.60 -4 -4 16 134.89 13.60 3 4 -16 193.48 19.30 -3 -4 16 184.08 16.60 2 4 -16 49.10 12.60 -2 -4 16 31.20 8.90 1 4 -16 71.19 14.30 -1 -4 16 72.59 10.40 0 4 -16 169.78 19.70 5 3 -16 99.79 11.00 -5 -3 16 83.19 11.90 4 3 -16 115.69 15.00 -4 -3 16 126.29 13.00 3 3 -16 13.80 6.80 -3 -3 16 16.50 5.40 2 3 -16 90.89 14.10 -2 -3 16 74.59 10.50 1 3 -16 110.99 15.30 -1 -3 16 92.19 11.50 0 3 -16 4.40 6.80 0 -3 16 10.30 6.40 6 2 -16 104.59 11.90 -6 -2 16 104.69 12.40 5 2 -16 170.48 14.70 -5 -2 16 170.98 16.00 4 2 -16 9.90 5.80 -4 -2 16 9.30 5.20 3 2 -16 111.29 13.80 -3 -2 16 103.79 11.90 2 2 -16 32.40 10.70 -2 -2 16 25.50 5.80 1 2 -16 11.40 6.40 -1 -2 16 10.50 5.10 0 2 -16 36.80 11.50 0 -2 16 42.60 9.50 6 1 -16 14.30 5.60 -6 -1 16 15.80 5.70 5 1 -16 13.10 5.50 5 1 -16 28.30 8.30 -5 -1 16 19.20 6.00 4 1 -16 49.70 10.20 4 1 -16 68.19 9.80 -4 -1 16 63.49 10.10 3 1 -16 34.00 9.60 -3 -1 16 18.70 5.60 2 1 -16 91.99 12.80 -2 -1 16 105.29 11.60 1 1 -16 119.69 14.10 -1 -1 16 112.49 12.40 0 1 -16 4.40 6.10 0 -1 16 8.40 4.70 7 0 -16 14.60 5.90 6 0 -16 67.29 10.20 -6 0 16 51.09 10.20 5 0 -16 82.99 11.00 5 0 -16 97.59 11.20 -5 0 16 76.89 11.20 4 0 -16 15.90 5.60 4 0 -16 10.90 5.20 -4 0 16 13.80 5.50 3 0 -16 102.99 13.00 -3 0 16 129.79 12.50 2 0 -16 236.68 20.20 -2 0 16 231.28 19.20 1 0 -16 39.30 10.40 -1 0 16 42.30 8.80 0 0 16 73.69 12.40 7 -1 -16 153.68 15.10 6 -1 -16 165.18 15.50 -6 1 16 151.18 15.30 5 -1 -16 34.20 9.00 5 -1 -16 39.90 9.50 -5 1 16 22.40 6.10 4 -1 -16 170.38 15.80 4 -1 -16 166.88 15.10 -4 1 16 157.38 15.60 -4 1 16 168.98 15.10 3 -1 -16 217.58 17.90 -3 1 16 177.18 15.90 -3 1 16 186.38 16.60 2 -1 -16 13.80 5.80 -2 1 16 13.80 5.20 1 -1 -16 39.00 10.80 -1 1 16 38.70 8.80 7 -2 -16 83.79 12.50 6 -2 -16 8.80 6.00 -6 2 16 5.10 5.30 5 -2 -16 26.30 8.90 5 -2 -16 31.60 9.40 -5 2 16 52.49 9.60 4 -2 -16 104.89 13.20 -4 2 16 129.09 13.30 -4 2 16 138.89 12.90 3 -2 -16 42.40 10.10 -3 2 16 43.20 8.80 -3 2 16 42.90 8.70 2 -2 -16 -2.10 5.00 -2 2 16 4.70 4.40 6 -3 -16 2.90 5.70 -6 3 16 10.40 5.60 5 -3 -16 3.80 5.60 5 -3 -16 -3.30 4.20 -5 3 16 4.70 5.00 -5 3 16 -0.40 4.80 4 -3 -16 41.60 9.80 -4 3 16 45.50 9.60 -4 3 16 44.10 9.20 3 -3 -16 40.90 10.10 -3 3 16 29.50 8.60 -3 3 16 34.90 8.60 4 2 -17 -4.00 5.10 3 2 -17 49.90 11.20 2 2 -17 7.00 6.10 4 1 -17 7.30 5.60 3 1 -17 0.70 5.40 2 1 -17 71.39 12.30 5 0 -17 18.60 6.10 5 0 -17 37.70 9.60 4 0 -17 8.70 5.40 3 0 -17 189.18 17.60 5 -1 -17 6.70 5.20 4 -1 -17 129.09 14.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 98787 loop_ _space_group_symop_operation_xyz '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 0.80683(4) 0.65514(4) 0.59694(3) 0.03288(12) Uani 1 1 d . . . . . Cl1 Cl 1.0303(4) 0.8821(4) 0.9288(2) 0.1256(11) Uani 1 1 d . . . . . Ni1 Ni 0.52124(6) 0.47662(5) 0.48985(4) 0.02142(12) Uani 1 1 d . . . . . N1 N 0.4300(4) 0.4389(4) 0.6201(3) 0.0205(7) Uani 1 1 d . . . . . N2 N 0.4592(4) 0.6446(4) 0.5044(3) 0.0216(7) Uani 1 1 d . . . . . Cl2 Cl 0.7680(4) 0.9700(4) 0.8847(2) 0.1208(10) Uani 1 1 d . . . . . N3 N 0.5301(4) 0.5658(4) 0.3485(3) 0.0233(7) Uani 1 1 d . . . . . C1 C 0.3818(5) 0.3010(5) 0.6640(3) 0.0221(9) Uani 1 1 d . . . . . C2 C 0.5017(5) 0.2789(5) 0.7410(3) 0.0249(9) Uani 1 1 d . . . . . C3 C 0.4495(6) 0.1452(5) 0.7807(4) 0.0335(11) Uani 1 1 d . . . . . H3 H 0.526719 0.129008 0.833824 0.040 Uiso 1 1 calc R U . . . C4 C 0.2872(7) 0.0374(6) 0.7433(4) 0.0387(12) Uani 1 1 d . . . . . H4 H 0.254244 -0.051176 0.771424 0.046 Uiso 1 1 calc R U . . . C5 C 0.1728(6) 0.0586(5) 0.6648(4) 0.0357(11) Uani 1 1 d . . . . . H5 H 0.062759 -0.017425 0.638901 0.043 Uiso 1 1 calc R U . . . C6 C 0.2160(5) 0.1898(5) 0.6228(3) 0.0266(9) Uani 1 1 d . . . . . C7 C 0.7653(6) 0.3184(6) 0.7237(4) 0.0417(13) Uani 1 1 d . . . . . H7A H 0.714645 0.302635 0.648265 0.062 Uiso 1 1 calc R U . . . H7B H 0.751306 0.220802 0.742770 0.062 Uiso 1 1 calc R U . . . H7C H 0.881864 0.387866 0.745511 0.062 Uiso 1 1 calc R U . . . C8 C 0.6842(6) 0.3872(5) 0.7775(4) 0.0291(10) Uani 1 1 d . . . . . H8 H 0.695916 0.483941 0.753979 0.035 Uiso 1 1 calc R U . . . C9 C 0.7706(7) 0.4272(7) 0.8963(4) 0.0455(13) Uani 1 1 d . . . . . H9A H 0.765220 0.334926 0.921372 0.068 Uiso 1 1 calc R U . . . H9B H 0.716630 0.470933 0.928793 0.068 Uiso 1 1 calc R U . . . H9C H 0.884938 0.501065 0.914214 0.068 Uiso 1 1 calc R U . . . C10 C 0.0120(8) 0.0748(9) 0.4405(5) 0.0671(19) Uani 1 1 d . . . . . H10A H -0.064914 0.091157 0.383316 0.101 Uiso 1 1 calc R U . . . H10B H -0.045059 -0.022683 0.458172 0.101 Uiso 1 1 calc R U . . . H10C H 0.100058 0.073657 0.419320 0.101 Uiso 1 1 calc R U . . . C11 C 0.0843(6) 0.2042(6) 0.5360(4) 0.0415(12) Uani 1 1 d . . . . . H11 H 0.135330 0.303163 0.515207 0.050 Uiso 1 1 calc R U . . . C12 C -0.0511(7) 0.2044(8) 0.5741(6) 0.0590(16) Uani 1 1 d . . . . . H12A H -0.128184 0.225227 0.520133 0.089 Uiso 1 1 calc R U . . . H12B H -0.002122 0.283182 0.637274 0.089 Uiso 1 1 calc R U . . . H12C H -0.108789 0.104943 0.589185 0.089 Uiso 1 1 calc R U . . . C13 C 0.3449(5) 0.5660(5) 0.7388(3) 0.0242(9) Uani 1 1 d . . . . . C14 C 0.4291(7) 0.5583(6) 0.8392(4) 0.0362(11) Uani 1 1 d . . . . . H14 H 0.516959 0.532785 0.851247 0.043 Uiso 1 1 calc R U . . . C15 C 0.3823(8) 0.5888(6) 0.9215(4) 0.0475(14) Uani 1 1 d . . . . . H15 H 0.438756 0.583965 0.989525 0.057 Uiso 1 1 calc R U . . . C16 C 0.2533(7) 0.6262(6) 0.9041(4) 0.0467(13) Uani 1 1 d . . . . . H16 H 0.223199 0.647474 0.960516 0.056 Uiso 1 1 calc R U . . . C17 C 0.1693(7) 0.6326(6) 0.8057(4) 0.0405(12) Uani 1 1 d . . . . . H17 H 0.081811 0.658552 0.794465 0.049 Uiso 1 1 calc R U . . . C18 C 0.2127(6) 0.6011(5) 0.7228(4) 0.0299(10) Uani 1 1 d . . . . . H18 H 0.152784 0.603147 0.654820 0.036 Uiso 1 1 calc R U . . . C19 C 0.4029(5) 0.5487(5) 0.6513(3) 0.0219(8) Uani 1 1 d . . . . . C20 C 0.4356(5) 0.6769(5) 0.5920(3) 0.0221(8) Uani 1 1 d . . . . . C21 C 0.4449(6) 0.8189(5) 0.6242(4) 0.0296(10) Uani 1 1 d . . . . . H21 H 0.428419 0.841147 0.686436 0.035 Uiso 1 1 calc R U . . . C22 C 0.4791(6) 0.9266(5) 0.5625(4) 0.0348(11) Uani 1 1 d . . . . . H22 H 0.485018 1.023215 0.582091 0.042 Uiso 1 1 calc R U . . . C23 C 0.5045(6) 0.8915(5) 0.4719(3) 0.0302(10) Uani 1 1 d . . . . . H23 H 0.529779 0.964446 0.429987 0.036 Uiso 1 1 calc R U . . . C24 C 0.4923(5) 0.7481(5) 0.4437(3) 0.0231(9) Uani 1 1 d . . . . . C25 C 0.5151(5) 0.6903(5) 0.3485(3) 0.0231(9) Uani 1 1 d . . . . . C26 C 0.5122(6) 0.7801(5) 0.2637(3) 0.0278(9) Uani 1 1 d . . . . . C27 C 0.3932(7) 0.8331(6) 0.2318(4) 0.0413(12) Uani 1 1 d . . . . . H27 H 0.309888 0.806048 0.260666 0.050 Uiso 1 1 calc R U . . . C28 C 0.3966(9) 0.9246(7) 0.1583(5) 0.0564(16) Uani 1 1 d . . . . . H28 H 0.317516 0.961529 0.138549 0.068 Uiso 1 1 calc R U . . . C29 C 0.5154(10) 0.9610(7) 0.1146(5) 0.0621(19) Uani 1 1 d . . . . . H29 H 0.516364 1.021351 0.063416 0.074 Uiso 1 1 calc R U . . . C30 C 0.6351(8) 0.9095(6) 0.1451(4) 0.0531(15) Uani 1 1 d . . . . . H30 H 0.717652 0.936473 0.115590 0.064 Uiso 1 1 calc R U . . . C31 C 0.6320(6) 0.8181(5) 0.2195(4) 0.0343(11) Uani 1 1 d . . . . . H31 H 0.711891 0.782112 0.239707 0.041 Uiso 1 1 calc R U . . . C32 C 0.5234(5) 0.4832(5) 0.2540(3) 0.0245(9) Uani 1 1 d . . . . . C33 C 0.6699(6) 0.4935(6) 0.2435(4) 0.0318(10) Uani 1 1 d . . . . . C34 C 0.6534(7) 0.4112(7) 0.1503(4) 0.0449(13) Uani 1 1 d . . . . . H34 H 0.748459 0.416802 0.139690 0.054 Uiso 1 1 calc R U . . . C35 C 0.5017(8) 0.3219(6) 0.0734(4) 0.0460(14) Uani 1 1 d . . . . . H35 H 0.494217 0.270866 0.010171 0.055 Uiso 1 1 calc R U . . . C36 C 0.3626(7) 0.3081(6) 0.0897(4) 0.0386(12) Uani 1 1 d . . . . . H36 H 0.259443 0.242638 0.038408 0.046 Uiso 1 1 calc R U . . . C37 C 0.3681(6) 0.3878(5) 0.1797(3) 0.0315(10) Uani 1 1 d . . . . . C38 C 0.9691(8) 0.6895(9) 0.2888(6) 0.071(2) Uani 1 1 d . . . . . H38A H 0.997225 0.628437 0.246878 0.107 Uiso 1 1 calc R U . . . H38B H 1.066411 0.757019 0.348473 0.107 Uiso 1 1 calc R U . . . H38C H 0.927648 0.750440 0.246506 0.107 Uiso 1 1 calc R U . . . C39 C 0.8360(7) 0.5828(7) 0.3278(5) 0.0487(14) Uani 1 1 d . . . . . H39 H 0.823648 0.648431 0.379318 0.058 Uiso 1 1 calc R U . . . C40 C 0.8926(9) 0.4763(10) 0.3852(5) 0.072(2) Uani 1 1 d . . . . . H40A H 0.807069 0.408267 0.408375 0.108 Uiso 1 1 calc R U . . . H40B H 0.992125 0.536458 0.445555 0.108 Uiso 1 1 calc R U . . . H40C H 0.914988 0.416092 0.338507 0.108 Uiso 1 1 calc R U . . . C41 C 0.1110(7) 0.4217(8) 0.1127(5) 0.0579(16) Uani 1 1 d . . . . . H41A H 0.088403 0.369861 0.043024 0.087 Uiso 1 1 calc R U . . . H41B H 0.174551 0.531416 0.120642 0.087 Uiso 1 1 calc R U . . . H41C H 0.007967 0.400884 0.122404 0.087 Uiso 1 1 calc R U . . . C42 C 0.2075(6) 0.3642(7) 0.1933(4) 0.0438(13) Uani 1 1 d . . . . . H42 H 0.234771 0.422933 0.263444 0.053 Uiso 1 1 calc R U . . . C43 C 0.0991(8) 0.1918(8) 0.1884(5) 0.070(2) Uani 1 1 d . . . . . H43A H 0.056906 0.134242 0.117229 0.105 Uiso 1 1 calc R U . . . H43B H 0.007792 0.181677 0.210010 0.105 Uiso 1 1 calc R U . . . H43C H 0.165131 0.152060 0.234993 0.105 Uiso 1 1 calc R U . . . C45 C 0.9058(13) 0.9364(13) 0.8395(7) 0.114(4) Uani 1 1 d . . . . . H45A H 0.843516 0.855898 0.775515 0.136 Uiso 1 1 calc R U . . . H45B H 0.974378 1.030103 0.821211 0.136 Uiso 1 1 calc R U . . . Br2 Br 0.45856(6) 0.22288(5) 0.42341(4) 0.04129(14) Uani 1 1 d . . . . . 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 0.0270(2) 0.0320(2) 0.0327(2) 0.00824(18) 0.00903(18) 0.00774(18) Cl1 0.142(2) 0.136(2) 0.109(2) -0.0193(17) 0.0095(17) 0.103(2) Ni1 0.0274(3) 0.0167(3) 0.0236(3) 0.0055(2) 0.0105(2) 0.0121(2) N1 0.0222(17) 0.0161(17) 0.0227(17) 0.0068(13) 0.0079(14) 0.0078(14) N2 0.0273(18) 0.0172(17) 0.0239(17) 0.0050(13) 0.0107(14) 0.0122(14) Cl2 0.127(2) 0.158(3) 0.0887(17) 0.0102(17) 0.0087(15) 0.098(2) N3 0.0280(18) 0.0252(19) 0.0234(18) 0.0083(15) 0.0131(15) 0.0149(16) C1 0.029(2) 0.017(2) 0.025(2) 0.0069(16) 0.0156(18) 0.0093(17) C2 0.032(2) 0.022(2) 0.029(2) 0.0086(17) 0.0169(19) 0.0145(19) C3 0.047(3) 0.034(3) 0.037(3) 0.020(2) 0.021(2) 0.027(2) C4 0.051(3) 0.027(3) 0.056(3) 0.020(2) 0.034(3) 0.021(2) C5 0.033(2) 0.022(2) 0.051(3) 0.007(2) 0.024(2) 0.006(2) C6 0.025(2) 0.023(2) 0.033(2) 0.0059(18) 0.0138(19) 0.0090(18) C7 0.032(3) 0.043(3) 0.050(3) 0.009(3) 0.018(2) 0.015(2) C8 0.029(2) 0.026(2) 0.031(2) 0.0108(19) 0.0080(19) 0.013(2) C9 0.041(3) 0.057(4) 0.033(3) 0.008(2) 0.005(2) 0.023(3) C10 0.050(3) 0.083(5) 0.042(3) -0.003(3) 0.006(3) 0.016(3) C11 0.027(2) 0.032(3) 0.053(3) 0.012(2) 0.010(2) 0.004(2) C12 0.031(3) 0.067(4) 0.079(4) 0.012(3) 0.015(3) 0.025(3) C13 0.034(2) 0.017(2) 0.024(2) 0.0049(16) 0.0147(18) 0.0107(18) C14 0.054(3) 0.036(3) 0.029(2) 0.010(2) 0.017(2) 0.028(2) C15 0.078(4) 0.050(3) 0.026(3) 0.013(2) 0.023(3) 0.036(3) C16 0.067(4) 0.042(3) 0.047(3) 0.009(2) 0.037(3) 0.027(3) C17 0.047(3) 0.030(3) 0.054(3) 0.009(2) 0.032(3) 0.016(2) C18 0.033(2) 0.024(2) 0.034(2) 0.0069(18) 0.014(2) 0.0119(19) C19 0.022(2) 0.020(2) 0.022(2) 0.0038(16) 0.0075(16) 0.0078(17) C20 0.026(2) 0.019(2) 0.023(2) 0.0032(16) 0.0100(17) 0.0102(17) C21 0.046(3) 0.023(2) 0.029(2) 0.0054(18) 0.019(2) 0.020(2) C22 0.054(3) 0.021(2) 0.040(3) 0.008(2) 0.023(2) 0.021(2) C23 0.047(3) 0.021(2) 0.030(2) 0.0122(19) 0.019(2) 0.019(2) C24 0.026(2) 0.018(2) 0.027(2) 0.0079(17) 0.0107(18) 0.0108(17) C25 0.025(2) 0.023(2) 0.020(2) 0.0051(17) 0.0063(16) 0.0101(18) C26 0.040(3) 0.023(2) 0.022(2) 0.0080(17) 0.0109(19) 0.015(2) C27 0.052(3) 0.044(3) 0.043(3) 0.018(2) 0.020(3) 0.032(3) C28 0.082(4) 0.058(4) 0.043(3) 0.020(3) 0.012(3) 0.050(4) C29 0.102(5) 0.042(4) 0.041(3) 0.022(3) 0.025(3) 0.030(4) C30 0.071(4) 0.036(3) 0.047(3) 0.018(3) 0.034(3) 0.009(3) C31 0.042(3) 0.030(3) 0.030(2) 0.009(2) 0.014(2) 0.014(2) C32 0.031(2) 0.022(2) 0.023(2) 0.0066(17) 0.0117(18) 0.0136(19) C33 0.040(3) 0.037(3) 0.033(2) 0.012(2) 0.020(2) 0.025(2) C34 0.059(3) 0.056(4) 0.043(3) 0.013(3) 0.030(3) 0.039(3) C35 0.078(4) 0.042(3) 0.032(3) 0.008(2) 0.026(3) 0.035(3) C36 0.055(3) 0.029(3) 0.031(3) 0.003(2) 0.017(2) 0.017(2) C37 0.040(3) 0.025(2) 0.027(2) 0.0081(19) 0.012(2) 0.012(2) C38 0.041(3) 0.094(6) 0.078(5) 0.000(4) 0.030(3) 0.027(4) C39 0.039(3) 0.064(4) 0.049(3) 0.003(3) 0.019(3) 0.028(3) C40 0.068(4) 0.122(7) 0.052(4) 0.021(4) 0.018(3) 0.070(5) C41 0.045(3) 0.075(5) 0.055(4) 0.004(3) 0.013(3) 0.033(3) C42 0.035(3) 0.055(4) 0.030(3) -0.001(2) 0.012(2) 0.011(3) C43 0.044(3) 0.082(5) 0.054(4) 0.019(4) 0.015(3) 0.002(3) C45 0.121(8) 0.154(10) 0.054(5) -0.004(5) 0.025(5) 0.059(7) Br2 0.0725(4) 0.0238(2) 0.0372(3) 0.00872(19) 0.0216(2) 0.0288(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 '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 N2 Ni1 N3 76.90(13) . . ? N2 Ni1 N1 77.16(13) . . ? N3 Ni1 N1 151.54(13) . . ? N2 Ni1 Br2 152.04(10) . . ? N3 Ni1 Br2 98.00(10) . . ? N1 Ni1 Br2 99.39(9) . . ? N2 Ni1 Br1 89.17(10) . . ? N3 Ni1 Br1 94.86(10) . . ? N1 Ni1 Br1 96.28(9) . . ? Br2 Ni1 Br1 118.77(3) . . ? C19 N1 C1 119.1(3) . . ? C19 N1 Ni1 112.6(3) . . ? C1 N1 Ni1 127.9(3) . . ? C20 N2 C24 121.0(4) . . ? C20 N2 Ni1 117.9(3) . . ? C24 N2 Ni1 117.9(3) . . ? C25 N3 C32 120.8(3) . . ? C25 N3 Ni1 113.4(3) . . ? C32 N3 Ni1 124.9(3) . . ? C2 C1 C6 121.9(4) . . ? C2 C1 N1 119.8(4) . . ? C6 C1 N1 118.2(4) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 C8 119.1(4) . . ? C1 C2 C8 123.2(4) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 117.4(4) . . ? C5 C6 C11 118.7(4) . . ? C1 C6 C11 123.9(4) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 C7 108.8(4) . . ? C2 C8 C9 114.0(4) . . ? C7 C8 C9 111.1(4) . . ? C2 C8 H8 107.6 . . ? C7 C8 H8 107.6 . . ? C9 C8 H8 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 C10 110.6(5) . . ? C6 C11 C12 110.5(5) . . ? C10 C11 C12 110.6(5) . . ? C6 C11 H11 108.3 . . ? C10 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.1(4) . . ? C14 C13 C19 120.3(4) . . ? C18 C13 C19 120.4(4) . . ? C15 C14 C13 119.3(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.9(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.6(5) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? N1 C19 C13 128.3(4) . . ? N1 C19 C20 115.4(4) . . ? C13 C19 C20 116.3(3) . . ? N2 C20 C21 121.2(4) . . ? N2 C20 C19 113.9(3) . . ? C21 C20 C19 124.9(4) . . ? C22 C21 C20 118.4(4) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C23 C22 C21 119.6(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 119.2(4) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? N2 C24 C23 120.5(4) . . ? N2 C24 C25 113.1(4) . . ? C23 C24 C25 126.4(4) . . ? N3 C25 C26 127.5(4) . . ? N3 C25 C24 115.4(4) . . ? C26 C25 C24 117.0(4) . . ? C31 C26 C27 119.2(4) . . ? C31 C26 C25 120.2(4) . . ? C27 C26 C25 120.6(4) . . ? C28 C27 C26 120.8(5) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.6(6) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.5(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.7(5) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C26 C31 C30 120.1(5) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C37 C32 C33 122.6(4) . . ? C37 C32 N3 117.4(4) . . ? C33 C32 N3 119.9(4) . . ? C34 C33 C32 116.5(5) . . ? C34 C33 C39 120.5(5) . . ? C32 C33 C39 123.0(4) . . ? C35 C34 C33 121.9(5) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C36 C35 C34 119.5(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 122.2(5) . . ? C35 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C36 C37 C32 117.1(5) . . ? C36 C37 C42 119.2(4) . . ? C32 C37 C42 123.7(4) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C39 C40 110.8(5) . . ? C33 C39 C38 114.1(5) . . ? C40 C39 C38 110.1(5) . . ? C33 C39 H39 107.2 . . ? C40 C39 H39 107.2 . . ? C38 C39 H39 107.2 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 C42 C37 112.2(4) . . ? C41 C42 C43 109.6(5) . . ? C37 C42 C43 110.8(5) . . ? C41 C42 H42 108.0 . . ? C37 C42 H42 108.0 . . ? C43 C42 H42 108.0 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Cl1 C45 Cl2 113.2(5) . . ? Cl1 C45 H45A 108.9 . . ? Cl2 C45 H45A 108.9 . . ? Cl1 C45 H45B 108.9 . . ? Cl2 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? 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 2.4498(6) . ? Cl1 C45 1.704(10) . ? Ni1 N2 1.978(3) . ? Ni1 N3 2.176(3) . ? Ni1 N1 2.192(3) . ? Ni1 Br2 2.3504(6) . ? N1 C19 1.282(5) . ? N1 C1 1.462(5) . ? N2 C20 1.326(5) . ? N2 C24 1.343(5) . ? Cl2 C45 1.741(10) . ? N3 C25 1.282(5) . ? N3 C32 1.453(5) . ? C1 C2 1.403(6) . ? C1 C6 1.406(6) . ? C2 C3 1.399(6) . ? C2 C8 1.515(6) . ? C3 C4 1.373(7) . ? C3 H3 0.9400 . ? C4 C5 1.375(7) . ? C4 H4 0.9400 . ? C5 C6 1.391(6) . ? C5 H5 0.9400 . ? C6 C11 1.508(7) . ? C7 C8 1.518(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.525(7) . ? C8 H8 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.527(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.530(8) . ? C11 H11 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.391(7) . ? C13 C18 1.397(6) . ? C13 C19 1.487(5) . ? C14 C15 1.387(7) . ? C14 H14 0.9400 . ? C15 C16 1.380(8) . ? C15 H15 0.9400 . ? C16 C17 1.363(8) . ? C16 H16 0.9400 . ? C17 C18 1.377(7) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.507(6) . ? C20 C21 1.390(6) . ? C21 C22 1.382(7) . ? C21 H21 0.9400 . ? C22 C23 1.382(6) . ? C22 H22 0.9400 . ? C23 C24 1.379(6) . ? C23 H23 0.9400 . ? C24 C25 1.498(6) . ? C25 C26 1.495(6) . ? C26 C31 1.377(6) . ? C26 C27 1.399(6) . ? C27 C28 1.382(8) . ? C27 H27 0.9400 . ? C28 C29 1.366(10) . ? C28 H28 0.9400 . ? C29 C30 1.392(10) . ? C29 H29 0.9400 . ? C30 C31 1.392(7) . ? C30 H30 0.9400 . ? C31 H31 0.9400 . ? C32 C37 1.395(6) . ? C32 C33 1.409(6) . ? C33 C34 1.397(7) . ? C33 C39 1.499(8) . ? C34 C35 1.379(8) . ? C34 H34 0.9400 . ? C35 C36 1.364(8) . ? C35 H35 0.9400 . ? C36 C37 1.393(6) . ? C36 H36 0.9400 . ? C37 C42 1.521(7) . ? C38 C39 1.537(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.514(9) . ? C39 H39 0.9900 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 C42 1.504(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C43 1.557(9) . ? C42 H42 0.9900 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C23 H23 Br2 0.94 2.87 3.515(4) 126.7 1_565 yes C45 H45A Br1 0.98 2.88 3.791(9) 154.9 . yes 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 C19 N1 C1 C2 -102.5(5) . . . . ? Ni1 N1 C1 C2 85.3(4) . . . . ? C19 N1 C1 C6 80.9(5) . . . . ? Ni1 N1 C1 C6 -91.3(4) . . . . ? C6 C1 C2 C3 -3.7(6) . . . . ? N1 C1 C2 C3 179.9(4) . . . . ? C6 C1 C2 C8 172.5(4) . . . . ? N1 C1 C2 C8 -4.0(6) . . . . ? C1 C2 C3 C4 1.9(7) . . . . ? C8 C2 C3 C4 -174.4(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 -1.5(8) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? C4 C5 C6 C11 179.3(5) . . . . ? C2 C1 C6 C5 2.8(6) . . . . ? N1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C11 -176.6(4) . . . . ? N1 C1 C6 C11 -0.1(6) . . . . ? C3 C2 C8 C7 75.8(5) . . . . ? C1 C2 C8 C7 -100.3(5) . . . . ? C3 C2 C8 C9 -48.8(6) . . . . ? C1 C2 C8 C9 135.1(5) . . . . ? C5 C6 C11 C10 -61.2(6) . . . . ? C1 C6 C11 C10 118.2(5) . . . . ? C5 C6 C11 C12 61.6(6) . . . . ? C1 C6 C11 C12 -119.0(5) . . . . ? C18 C13 C14 C15 -1.3(7) . . . . ? C19 C13 C14 C15 174.1(5) . . . . ? C13 C14 C15 C16 0.1(8) . . . . ? C14 C15 C16 C17 0.5(9) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C16 C17 C18 C13 -1.5(7) . . . . ? C14 C13 C18 C17 2.1(7) . . . . ? C19 C13 C18 C17 -173.3(4) . . . . ? C1 N1 C19 C13 8.4(6) . . . . ? Ni1 N1 C19 C13 -178.3(3) . . . . ? C1 N1 C19 C20 -172.2(3) . . . . ? Ni1 N1 C19 C20 1.1(4) . . . . ? C14 C13 C19 N1 54.5(6) . . . . ? C18 C13 C19 N1 -130.1(5) . . . . ? C14 C13 C19 C20 -124.9(4) . . . . ? C18 C13 C19 C20 50.5(5) . . . . ? C24 N2 C20 C21 -0.2(6) . . . . ? Ni1 N2 C20 C21 158.9(3) . . . . ? C24 N2 C20 C19 -179.0(4) . . . . ? Ni1 N2 C20 C19 -19.9(5) . . . . ? N1 C19 C20 N2 11.5(5) . . . . ? C13 C19 C20 N2 -169.0(4) . . . . ? N1 C19 C20 C21 -167.1(4) . . . . ? C13 C19 C20 C21 12.4(6) . . . . ? N2 C20 C21 C22 0.2(7) . . . . ? C19 C20 C21 C22 178.7(4) . . . . ? C20 C21 C22 C23 -0.6(7) . . . . ? C21 C22 C23 C24 1.2(8) . . . . ? C20 N2 C24 C23 0.8(6) . . . . ? Ni1 N2 C24 C23 -158.3(3) . . . . ? C20 N2 C24 C25 179.9(4) . . . . ? Ni1 N2 C24 C25 20.8(5) . . . . ? C22 C23 C24 N2 -1.2(7) . . . . ? C22 C23 C24 C25 179.7(4) . . . . ? C32 N3 C25 C26 -8.9(7) . . . . ? Ni1 N3 C25 C26 -178.6(3) . . . . ? C32 N3 C25 C24 168.9(4) . . . . ? Ni1 N3 C25 C24 -0.8(5) . . . . ? N2 C24 C25 N3 -12.3(5) . . . . ? C23 C24 C25 N3 166.8(4) . . . . ? N2 C24 C25 C26 165.8(4) . . . . ? C23 C24 C25 C26 -15.1(6) . . . . ? N3 C25 C26 C31 -49.5(7) . . . . ? C24 C25 C26 C31 132.7(4) . . . . ? N3 C25 C26 C27 133.7(5) . . . . ? C24 C25 C26 C27 -44.1(6) . . . . ? C31 C26 C27 C28 -1.1(8) . . . . ? C25 C26 C27 C28 175.7(5) . . . . ? C26 C27 C28 C29 1.5(9) . . . . ? C27 C28 C29 C30 -1.4(10) . . . . ? C28 C29 C30 C31 1.1(10) . . . . ? C27 C26 C31 C30 0.8(7) . . . . ? C25 C26 C31 C30 -176.1(4) . . . . ? C29 C30 C31 C26 -0.8(8) . . . . ? C25 N3 C32 C37 -81.0(5) . . . . ? Ni1 N3 C32 C37 87.5(4) . . . . ? C25 N3 C32 C33 103.1(5) . . . . ? Ni1 N3 C32 C33 -88.4(5) . . . . ? C37 C32 C33 C34 4.6(7) . . . . ? N3 C32 C33 C34 -179.8(4) . . . . ? C37 C32 C33 C39 -173.4(5) . . . . ? N3 C32 C33 C39 2.2(7) . . . . ? C32 C33 C34 C35 -1.3(8) . . . . ? C39 C33 C34 C35 176.8(5) . . . . ? C33 C34 C35 C36 -2.6(8) . . . . ? C34 C35 C36 C37 3.4(8) . . . . ? C35 C36 C37 C32 -0.2(7) . . . . ? C35 C36 C37 C42 -178.9(5) . . . . ? C33 C32 C37 C36 -3.8(7) . . . . ? N3 C32 C37 C36 -179.6(4) . . . . ? C33 C32 C37 C42 174.7(5) . . . . ? N3 C32 C37 C42 -1.0(7) . . . . ? C34 C33 C39 C40 -74.8(7) . . . . ? C32 C33 C39 C40 103.1(6) . . . . ? C34 C33 C39 C38 50.1(7) . . . . ? C32 C33 C39 C38 -132.0(5) . . . . ? C36 C37 C42 C41 -65.4(6) . . . . ? C32 C37 C42 C41 116.1(5) . . . . ? C36 C37 C42 C43 57.5(6) . . . . ? C32 C37 C42 C43 -121.0(5) . . . . ?