#------------------------------------------------------------------------------ #$Date: 2021-10-15 02:04:43 +0300 (Fri, 15 Oct 2021) $ #$Revision: 269958 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708561.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_7708561 loop_ _publ_author_name 'Peng, Min' 'Wu, Xiao-Fan' 'Wang, Li-Xin' 'Chen, Si-Huai' 'Xiang, Jing' 'Jin, Xin-Xin' 'Yiu, Shek-Man' 'Wang, Bing-Wu' 'Gao, Song' 'Lau, Tai-Chu' _publ_section_title ; Slow magnetic relaxation in high-coordinate Co(II) and Fe(II) compounds bearing neutral tetradentate ligands. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt02575a _journal_year 2021 _chemical_formula_moiety 'C44 H52 N8 Ni O4, 2(Cl O4)' _chemical_formula_sum 'C44 H52 Cl2 N8 Ni O12' _chemical_formula_weight 1014.54 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-09-14 _audit_creation_method ; Olex2 1.5 (compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380) ; _audit_update_record ; 2021-09-14 deposited with the CCDC. 2021-09-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.070(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.9339(9) _cell_length_b 13.2633(6) _cell_length_c 16.2274(5) _cell_measurement_reflns_used 4545 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 73.3590 _cell_measurement_theta_min 4.7020 _cell_volume 4488.0(3) _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 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0299 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.949 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8259 _diffrn_reflns_point_group_measured_fraction_full 0.571 _diffrn_reflns_point_group_measured_fraction_max 0.549 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.646 _diffrn_reflns_theta_min 3.950 _exptl_absorpt_coefficient_mu 2.341 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.502 _exptl_crystal_description needle _exptl_crystal_F_000 2120 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.438 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.66(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 695 _refine_ls_number_reflns 4985 _refine_ls_number_restraints 242 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0461 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+7.4626P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.1240 _reflns_Friedel_coverage 0.157 _reflns_Friedel_fraction_full 0.163 _reflns_Friedel_fraction_max 0.149 _reflns_number_gt 4817 _reflns_number_total 4985 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02575a2.cif _cod_data_source_block 04 _cod_database_code 7708561 _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 0.783 _shelx_estimated_absorpt_t_min 0.766 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.34(3) 0.66(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 3. Uiso/Uaniso restraints and constraints C43 \\sim C44 \\sim C45 \\sim C46 \\sim C43' \\sim C44' \\sim C45' \\sim C46': within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3.8A O5 \\sim O6' \\sim O7' \\sim O8': within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3.8A O9 \\sim O10' \\sim O11' \\sim O12': within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3.8A Uanis(O7') \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(O5') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 4. Others Sof(C43')=Sof(H43C)=Sof(H43D)=Sof(C44')=Sof(H44C)=Sof(H44D)=Sof(C45')= Sof(H45C)=Sof(H45D)=Sof(C46')=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1) Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)= Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1) Sof(O11')=Sof(O10')=Sof(O12')=1-FVAR(2) Sof(O10)=Sof(O11)=Sof(O12)=FVAR(2) Sof(O5')=Sof(O8')=Sof(O7')=Sof(O6')=1-FVAR(3) Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3) U11(C13)=U11(C14)=U11(C15)=U11(C16)=U11(C17)=U11(C18)=U11(C19)=U11(C20)= U11(C24)=FVAR(4) U11(C1)=U11(C2)=U11(C3)=U11(C4)=U11(C7)=U11(C8)=U11(C9)=U11(C10)=U11(C11)= U11(C12)=FVAR(5) 5.a Riding coordinates: N8(H8), C43(H43A,H43B), C43'(H43C,H43D) 5.b Secondary CH2 refined with riding coordinates: C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A, H34B), C35(H35A,H35B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C44(H44A,H44B), C45(H45A,H45B), C44'(H44C,H44D), C45'(H45C,H45D) 5.c Aromatic/amide H refined with riding coordinates: N1(H1), N4(H4), N5(H5), C2(H2), C3(H3), C5(H5A), C6(H6), C8(H8A), C9(H9), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21) 5.d Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C46(H46A,H46B, H46C), C46'(H46D,H46E,H46F) ; _shelx_res_file ; TITL 04 in Cc 04.res created by SHELXL-2018/3 at 08:20:27 on 14-Sep-2021 CELL 1.54178 20.9339 13.2633 16.2274 90 95.07 90 ZERR 4 0.0009 0.0006 0.0005 0 0.003 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C H Cl N Ni O UNIT 176 208 8 32 4 48 EQIV $1 +X,1+Y,+Z EQIV $2 0.5+X,0.5+Y,+Z EQIV $3 +X,2-Y,-0.5+Z SIMU 0.02 0.04 3.8 C43 C44 C45 C46 C43' C44' C45' C46' SIMU 0.02 0.04 3.8 O5 O6' O7' O8' SIMU 0.02 0.04 3.8 O9 O10' O11' O12' ISOR 0.002 0.004 O7' ISOR 0.001 0.002 O5' L.S. 9 PLAN 2 SIZE 0.12 0.11 0.11 TEMP 20(2) CONF HTAB C45' O12'_$1 HTAB N1 O12 HTAB N4 O5_$2 HTAB N5 O10' HTAB N8 O7_$3 MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -1 5 -1 REM REM REM WGHT 0.075400 7.462600 BASF 0.66082 FVAR 0.06701 0.64843 0.86969 0.81313 0.05522 0.02513 NI1 5 0.573179 0.926321 0.292760 11.00000 0.02536 0.02149 = 0.01378 -0.00014 -0.00099 -0.00154 CL1 3 0.324419 0.716039 0.563032 11.00000 0.04251 0.02980 = 0.03203 -0.00688 0.00497 -0.00768 CL2 3 0.580830 0.413899 0.294297 11.00000 0.06427 0.04579 = 0.03363 -0.00196 -0.00802 0.02338 N1 4 0.482891 0.642070 0.198286 11.00000 0.03130 0.03133 = 0.02558 -0.00711 -0.00383 0.00533 AFIX 43 H1 2 0.504335 0.596355 0.226290 11.00000 -1.20000 AFIX 0 N2 4 0.525510 0.804836 0.356106 11.00000 0.02355 0.01856 = 0.01958 0.00014 0.00041 -0.00154 N3 4 0.611396 0.941683 0.408234 11.00000 0.02227 0.02481 = 0.02008 0.00204 0.00125 0.00043 N4 4 0.718262 1.134716 0.355904 11.00000 0.02835 0.03306 = 0.02187 -0.00091 -0.00358 -0.00731 AFIX 43 H4 2 0.736911 1.149785 0.403667 11.00000 -1.20000 AFIX 0 N5 4 0.670256 0.643496 0.382451 11.00000 0.05278 0.03781 = 0.03444 0.00361 -0.00342 0.00756 AFIX 43 H5 2 0.657797 0.593082 0.351799 11.00000 -1.20000 AFIX 0 N6 4 0.623179 0.809977 0.227259 11.00000 0.03530 0.02491 = 0.02221 -0.00076 0.00332 0.00072 N7 4 0.534236 0.943498 0.177719 11.00000 0.02584 0.02173 = 0.01632 0.00135 -0.00161 -0.00252 N8 4 0.432173 1.140907 0.232136 11.00000 0.05590 0.05098 = 0.02633 0.01332 0.00634 0.02732 AFIX 3 H8 2 0.409693 1.153577 0.186376 11.00000 -1.20000 AFIX 0 O1 6 0.440173 0.799671 0.203271 11.00000 0.03465 0.02560 = 0.02194 0.00084 0.00140 -0.00096 O2 6 0.643163 1.042281 0.282632 11.00000 0.02889 0.02578 = 0.01470 0.00007 -0.00112 -0.00644 O3 6 0.707062 0.805733 0.381478 11.00000 0.03876 0.04142 = 0.04507 -0.01228 -0.00297 0.00708 O4 6 0.501269 1.038671 0.305793 11.00000 0.02967 0.02408 = 0.02176 0.00118 0.00033 0.00335 PART 1 O5 6 0.321614 0.658066 0.489196 41.00000 0.03489 0.04239 = 0.02648 -0.00786 -0.00879 -0.00308 O6 6 0.290976 0.665497 0.624911 41.00000 0.04573 0.03586 = 0.03677 0.00527 0.00623 -0.00464 O7 6 0.391501 0.728396 0.591996 41.00000 0.04057 0.10774 = 0.04158 -0.03099 0.00837 -0.03834 O8 6 0.298870 0.813603 0.547051 41.00000 0.15672 0.02377 = 0.06925 0.00870 0.06006 0.00862 PART 2 O5' 6 0.335404 0.632419 0.509575 -41.00000 0.03718 0.03674 = 0.03702 -0.00008 0.00305 0.00046 O8' 6 0.267012 0.763533 0.520642 -41.00000 0.04119 0.03562 = 0.04713 0.00813 -0.00032 0.01565 O7' 6 0.376151 0.791355 0.558640 -41.00000 0.03467 0.03732 = 0.03840 -0.00417 -0.00373 -0.00656 O6' 6 0.314915 0.688946 0.643865 -41.00000 0.06514 0.08914 = 0.05000 0.01105 0.02319 -0.01809 PART 0 O9 6 0.589752 0.308191 0.294316 11.00000 0.08817 0.04697 = 0.03996 -0.00714 0.00021 0.02887 PART 1 O10 6 0.579115 0.450062 0.377580 31.00000 0.12998 0.05129 = 0.04153 -0.01428 0.00305 0.01784 O11 6 0.633634 0.467309 0.261552 31.00000 0.16199 0.06616 = 0.07482 0.01861 0.05450 0.01662 O12 6 0.522252 0.438430 0.247892 31.00000 0.09523 0.06843 = 0.11141 -0.01204 -0.05992 0.03827 PART 2 O11' 6 0.570735 0.452559 0.199178 -31.00000 0.06070 0.03257 = 0.04804 0.00246 -0.00863 0.03112 O10' 6 0.631302 0.434755 0.342658 -31.00000 0.08468 0.03018 = 0.09524 0.01403 -0.01215 0.00063 O12' 6 0.521778 0.449881 0.311904 -31.00000 0.04742 0.06226 = 0.05409 -0.00720 0.01041 0.03797 PART 0 C1 1 0.487944 0.728373 0.327737 11.00000 61.00000 0.02274 = 0.02344 -0.00345 -0.00247 -0.00262 C2 1 0.468165 0.653275 0.380885 11.00000 61.00000 0.02996 = 0.03229 0.00107 0.00162 -0.00604 AFIX 43 H2 2 0.443397 0.599702 0.359240 11.00000 -1.20000 AFIX 0 C3 1 0.484849 0.658072 0.463679 11.00000 61.00000 0.02454 = 0.03035 0.00302 0.00322 -0.00136 AFIX 43 H3 2 0.469801 0.609992 0.498926 11.00000 -1.20000 AFIX 0 C4 1 0.525133 0.736504 0.495623 11.00000 61.00000 0.02638 = 0.02164 0.00104 -0.00069 0.00388 C5 1 0.548450 0.744888 0.581392 11.00000 0.03500 0.03111 = 0.01897 0.00549 0.00125 0.00374 AFIX 43 H5A 2 0.533570 0.700212 0.619513 11.00000 -1.20000 AFIX 0 C6 1 0.592196 0.817427 0.608166 11.00000 0.03621 0.02866 = 0.01500 0.00361 0.00131 0.00576 AFIX 43 H6 2 0.606466 0.821859 0.663969 11.00000 -1.20000 AFIX 0 C7 1 0.615854 0.886302 0.550079 11.00000 61.00000 0.02793 = 0.02163 0.00227 -0.00482 0.00231 C8 1 0.664069 0.959637 0.569709 11.00000 61.00000 0.02985 = 0.01707 -0.00518 -0.00514 0.00128 AFIX 43 H8A 2 0.681703 0.966891 0.624025 11.00000 -1.20000 AFIX 0 C9 1 0.684947 1.020452 0.508201 11.00000 61.00000 0.02966 = 0.02513 -0.00403 -0.00463 -0.00127 AFIX 43 H9 2 0.716763 1.068378 0.520694 11.00000 -1.20000 AFIX 0 C10 1 0.657421 1.008794 0.426643 11.00000 61.00000 0.02473 = 0.01658 -0.00118 -0.00060 -0.00270 C11 1 0.591321 0.881215 0.467453 11.00000 61.00000 0.02283 = 0.01423 0.00082 -0.00094 0.00153 C12 1 0.544974 0.806270 0.438006 11.00000 61.00000 0.02443 = 0.01792 0.00048 -0.00090 0.00192 C13 1 0.663090 0.735582 0.252698 11.00000 51.00000 0.02274 = 0.02942 0.00125 0.01124 0.00594 C14 1 0.685761 0.663161 0.198635 11.00000 51.00000 0.03303 = 0.04126 -0.00371 0.01563 0.01131 AFIX 43 H14 2 0.713266 0.612220 0.219143 11.00000 -1.20000 AFIX 0 C15 1 0.666815 0.668481 0.115097 11.00000 51.00000 0.03388 = 0.04198 -0.00672 0.02117 0.00401 AFIX 43 H15 2 0.682898 0.623014 0.078507 11.00000 -1.20000 AFIX 0 C16 1 0.622732 0.743715 0.085734 11.00000 51.00000 0.02905 = 0.02746 -0.00301 0.01580 -0.00157 C17 1 0.597738 0.753218 0.000652 11.00000 51.00000 0.03043 = 0.02872 -0.00822 0.01496 -0.00902 AFIX 43 H17 2 0.611891 0.709498 -0.038683 11.00000 -1.20000 AFIX 0 C18 1 0.554160 0.824504 -0.022792 11.00000 51.00000 0.03900 = 0.01946 -0.00078 0.00380 -0.01466 AFIX 43 H18 2 0.540142 0.830673 -0.078562 11.00000 -1.20000 AFIX 0 C19 1 0.528659 0.891284 0.035611 11.00000 51.00000 0.02918 = 0.01318 0.00055 0.00589 -0.01249 C20 1 0.480722 0.964146 0.018105 11.00000 51.00000 0.03541 = 0.01646 0.00696 -0.00589 -0.01387 AFIX 43 H20 2 0.462564 0.972041 -0.035911 11.00000 -1.20000 AFIX 0 C21 1 0.460407 1.023588 0.079382 11.00000 0.03520 0.03726 = 0.01928 0.00683 -0.00249 -0.00687 AFIX 43 H21 2 0.428503 1.071477 0.067277 11.00000 -1.20000 AFIX 0 C22 1 0.488060 1.011775 0.160630 11.00000 0.02605 0.02641 = 0.02369 0.00454 -0.00354 -0.00529 C23 1 0.554563 0.884033 0.118893 11.00000 0.03809 0.02560 = 0.02132 0.00316 0.00465 -0.00917 C24 1 0.602132 0.810745 0.144030 11.00000 51.00000 0.02432 = 0.01220 -0.00341 0.00976 -0.00681 C27 1 0.468131 0.726863 0.236170 11.00000 0.02267 0.03172 = 0.02086 -0.00035 0.00280 -0.00278 C28 1 0.463765 0.623955 0.110193 11.00000 0.03217 0.04583 = 0.02500 -0.01070 0.00385 0.00280 AFIX 23 H28A 2 0.500498 0.599662 0.083545 11.00000 -1.20000 H28B 2 0.450018 0.687016 0.084041 11.00000 -1.20000 AFIX 0 C29 1 0.409605 0.547264 0.097778 11.00000 0.03838 0.03067 = 0.02583 -0.00739 -0.00092 0.00123 AFIX 23 H29A 2 0.422913 0.485395 0.126193 11.00000 -1.20000 H29B 2 0.402099 0.532026 0.039260 11.00000 -1.20000 AFIX 0 C30 1 0.346939 0.582945 0.129248 11.00000 0.03353 0.02749 = 0.02983 -0.00669 0.00212 -0.00026 AFIX 23 H30A 2 0.317813 0.526148 0.130088 11.00000 -1.20000 H30B 2 0.355525 0.606831 0.185636 11.00000 -1.20000 AFIX 0 C31 1 0.314611 0.666256 0.077222 11.00000 0.03816 0.03632 = 0.03493 -0.00419 -0.00090 0.00467 AFIX 137 H31A 2 0.307580 0.644244 0.020792 11.00000 -1.50000 H31B 2 0.341529 0.724975 0.080123 11.00000 -1.50000 H31C 2 0.274218 0.682393 0.097752 11.00000 -1.50000 AFIX 0 C32 1 0.673030 1.065629 0.350297 11.00000 0.02198 0.02529 = 0.02449 0.00165 -0.00129 -0.00067 C33 1 0.737544 1.186715 0.281899 11.00000 0.02721 0.03669 = 0.02185 0.00432 0.00238 -0.00744 AFIX 23 H33A 2 0.702717 1.229514 0.259311 11.00000 -1.20000 H33B 2 0.745919 1.137196 0.240202 11.00000 -1.20000 AFIX 0 C34 1 0.797426 1.250751 0.302143 11.00000 0.02585 0.03321 = 0.02929 0.00238 0.00082 -0.00818 AFIX 23 H34A 2 0.828606 1.211287 0.336151 11.00000 -1.20000 H34B 2 0.816023 1.266616 0.251028 11.00000 -1.20000 AFIX 0 C35 1 0.785322 1.348323 0.346862 11.00000 0.03859 0.03851 = 0.04530 -0.00412 0.01381 -0.00662 AFIX 23 H35A 2 0.763308 1.333632 0.395623 11.00000 -1.20000 H35B 2 0.757724 1.391386 0.310904 11.00000 -1.20000 AFIX 0 C36 1 0.847593 1.403743 0.372562 11.00000 0.04605 0.05080 = 0.04674 -0.01581 0.00913 -0.01658 AFIX 137 H36A 2 0.872349 1.409891 0.325760 11.00000 -1.50000 H36B 2 0.871670 1.366610 0.415575 11.00000 -1.50000 H36C 2 0.838029 1.469676 0.392560 11.00000 -1.50000 AFIX 0 C37 1 0.683690 0.732188 0.344967 11.00000 0.03684 0.03020 = 0.03632 -0.00227 -0.00285 0.01144 C38 1 0.676050 0.630108 0.472364 11.00000 0.04297 0.04514 = 0.03328 0.00127 0.00687 0.00804 AFIX 23 H38A 2 0.641733 0.586340 0.487129 11.00000 -1.20000 H38B 2 0.670369 0.695050 0.498218 11.00000 -1.20000 AFIX 0 C39 1 0.738919 0.586249 0.506684 11.00000 0.04564 0.03226 = 0.02781 -0.00186 0.00706 0.00351 AFIX 23 H39A 2 0.773836 0.627466 0.490047 11.00000 -1.20000 H39B 2 0.743704 0.518930 0.484694 11.00000 -1.20000 AFIX 0 C40 1 0.741902 0.581710 0.601297 11.00000 0.05419 0.02623 = 0.02703 -0.00278 0.00419 -0.00571 AFIX 23 H40A 2 0.737155 0.649257 0.622843 11.00000 -1.20000 H40B 2 0.706450 0.541336 0.617475 11.00000 -1.20000 AFIX 0 C41 1 0.804020 0.537240 0.638761 11.00000 0.04505 0.05123 = 0.04819 -0.00764 -0.00216 -0.00089 AFIX 137 H41A 2 0.839123 0.578837 0.625176 11.00000 -1.50000 H41B 2 0.809123 0.470602 0.617202 11.00000 -1.50000 H41C 2 0.803405 0.533940 0.697783 11.00000 -1.50000 AFIX 0 C42 1 0.472542 1.065906 0.237260 11.00000 0.03551 0.02656 = 0.01825 0.00771 0.00299 0.00238 PART 1 C43 1 0.426079 1.206539 0.310328 21.00000 0.04218 0.03630 = 0.02504 -0.00400 0.00150 0.01255 AFIX 3 H43A 2 0.468169 1.231169 0.330678 21.00000 -1.20000 H43B 2 0.409849 1.165629 0.353438 21.00000 -1.20000 AFIX 0 C44 1 0.381362 1.294414 0.291658 21.00000 0.03927 0.03393 = 0.02325 -0.00206 0.00183 0.00472 AFIX 23 H44A 2 0.339158 1.269231 0.272412 21.00000 -1.20000 H44B 2 0.396917 1.334640 0.247686 21.00000 -1.20000 AFIX 0 C45 1 0.376162 1.360100 0.366895 21.00000 0.04381 0.04730 = 0.02625 -0.00385 0.00349 0.01390 AFIX 23 H45A 2 0.359347 1.320122 0.410128 21.00000 -1.20000 H45B 2 0.418669 1.382980 0.387233 21.00000 -1.20000 AFIX 0 C46 1 0.333513 1.450547 0.349236 21.00000 0.03326 0.03156 = 0.04214 -0.00621 -0.00045 0.01237 AFIX 137 H46A 2 0.290312 1.428479 0.334679 21.00000 -1.50000 H46B 2 0.348375 1.488295 0.304205 21.00000 -1.50000 H46C 2 0.334697 1.492459 0.397579 21.00000 -1.50000 AFIX 0 PART 2 C43' 1 0.398117 1.188956 0.291584 -21.00000 0.03428 0.03303 = 0.02678 0.01290 -0.00391 -0.00064 AFIX 3 H43C 2 0.353807 1.201496 0.271504 -21.00000 -1.20000 H43D 2 0.399647 1.150446 0.342544 -21.00000 -1.20000 AFIX 0 C44' 1 0.435944 1.284214 0.301677 -21.00000 0.04209 0.04012 = 0.03042 0.00283 -0.00120 0.01187 AFIX 23 H44C 2 0.431644 1.320283 0.249481 -21.00000 -1.20000 H44D 2 0.480840 1.266724 0.313161 -21.00000 -1.20000 AFIX 0 C45' 1 0.417010 1.356614 0.370613 -21.00000 0.04579 0.03746 = 0.03272 -0.00045 0.00436 -0.00492 AFIX 23 H45C 2 0.410472 1.317800 0.419829 -21.00000 -1.20000 H45D 2 0.451885 1.403476 0.384475 -21.00000 -1.20000 AFIX 0 C46' 1 0.355217 1.416640 0.343859 -21.00000 0.04768 0.03733 = 0.04019 0.00201 0.00369 0.02946 AFIX 137 H46D 2 0.319150 1.371655 0.339487 -21.00000 -1.50000 H46E 2 0.359300 1.447829 0.291198 -21.00000 -1.50000 H46F 2 0.348880 1.467661 0.384301 -21.00000 -1.50000 AFIX 0 HKLF 4 REM 04 in Cc REM wR2 = 0.1240, GooF = S = 1.030, Restrained GooF = 1.007 for all data REM R1 = 0.0461 for 4817 Fo > 4sig(Fo) and 0.0477 for all 4985 data REM 695 parameters refined using 242 restraints END WGHT 0.0754 7.4071 REM Highest difference peak 0.438, deepest hole -0.704, 1-sigma level 0.065 Q1 1 0.6125 0.4279 0.2125 11.00000 0.05 0.44 Q2 1 0.5706 0.8430 0.2895 11.00000 0.05 0.39 ; _shelx_res_checksum 9745 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.57318(4) 0.92632(5) 0.29276(5) 0.02037(17) Uani 1 1 d . . . . . Cl1 Cl 0.32442(6) 0.71604(9) 0.56303(9) 0.0347(3) Uani 1 1 d . . . . . Cl2 Cl 0.58083(9) 0.41390(11) 0.29430(12) 0.0486(4) Uani 1 1 d . . . . . N1 N 0.4829(2) 0.6421(4) 0.1983(3) 0.0298(9) Uani 1 1 d . . . . . H1 H 0.504335 0.596355 0.226290 0.036 Uiso 1 1 calc R U . . . N2 N 0.52551(18) 0.8048(3) 0.3561(3) 0.0207(8) Uani 1 1 d . . . . . N3 N 0.61140(19) 0.9417(3) 0.4082(3) 0.0224(8) Uani 1 1 d . . . . . N4 N 0.7183(2) 1.1347(3) 0.3559(3) 0.0281(9) Uani 1 1 d . . . . . H4 H 0.736911 1.149785 0.403667 0.034 Uiso 1 1 calc R U . . . N5 N 0.6703(3) 0.6435(4) 0.3825(3) 0.0421(12) Uani 1 1 d . . . . . H5 H 0.657797 0.593082 0.351799 0.051 Uiso 1 1 calc R U . . . N6 N 0.6232(2) 0.8100(3) 0.2273(3) 0.0274(9) Uani 1 1 d . . . . . N7 N 0.53424(19) 0.9435(3) 0.1777(3) 0.0215(8) Uani 1 1 d . . . . . N8 N 0.4322(3) 1.1409(4) 0.2321(3) 0.0442(13) Uani 1 1 d . . . . . H8 H 0.409693 1.153577 0.186376 0.053 Uiso 1 1 d R U . C . O1 O 0.44017(17) 0.7997(3) 0.2033(2) 0.0275(7) Uani 1 1 d . . . . . O2 O 0.64316(16) 1.0423(3) 0.2826(2) 0.0233(7) Uani 1 1 d . . . . . O3 O 0.7071(2) 0.8057(3) 0.3815(3) 0.0421(10) Uani 1 1 d . . . . . O4 O 0.50127(16) 1.0387(3) 0.3058(2) 0.0253(7) Uani 1 1 d . . . . . O5 O 0.3216(3) 0.6581(6) 0.4892(4) 0.0353(13) Uani 0.813(14) 1 d . U P A 1 O6 O 0.2910(3) 0.6655(5) 0.6249(4) 0.0393(15) Uani 0.813(14) 1 d . . P A 1 O7 O 0.3915(3) 0.7284(7) 0.5920(4) 0.063(3) Uani 0.813(14) 1 d . . P A 1 O8 O 0.2989(5) 0.8136(5) 0.5471(5) 0.080(3) Uani 0.813(14) 1 d . . P A 1 O5' O 0.3354(14) 0.632(2) 0.510(2) 0.037(7) Uani 0.187(14) 1 d . U P A 2 O8' O 0.2670(11) 0.764(2) 0.5206(16) 0.042(7) Uani 0.187(14) 1 d . U P A 2 O7' O 0.3762(10) 0.7914(18) 0.5586(15) 0.037(6) Uani 0.187(14) 1 d . U P A 2 O6' O 0.315(2) 0.689(3) 0.644(3) 0.067(9) Uani 0.187(14) 1 d . U P A 2 O9 O 0.5898(3) 0.3082(4) 0.2943(3) 0.0587(14) Uani 1 1 d . U . . . O10 O 0.5791(4) 0.4501(5) 0.3776(4) 0.075(2) Uani 0.870(12) 1 d . . P B 1 O11 O 0.6336(5) 0.4673(6) 0.2616(6) 0.098(3) Uani 0.870(12) 1 d . . P B 1 O12 O 0.5223(4) 0.4384(6) 0.2479(7) 0.096(4) Uani 0.870(12) 1 d . . P B 1 O11' O 0.5707(19) 0.453(3) 0.199(2) 0.048(10) Uani 0.130(12) 1 d . U P B 2 O10' O 0.631(2) 0.435(3) 0.343(4) 0.071(12) Uani 0.130(12) 1 d . U P B 2 O12' O 0.5218(18) 0.450(3) 0.312(3) 0.054(10) Uani 0.130(12) 1 d . U P B 2 C1 C 0.4879(2) 0.7284(4) 0.3277(3) 0.0240(9) Uani 1 1 d . . . . . C2 C 0.4682(2) 0.6533(4) 0.3809(4) 0.0292(10) Uani 1 1 d . . . . . H2 H 0.443397 0.599702 0.359240 0.035 Uiso 1 1 calc R U . . . C3 C 0.4848(2) 0.6581(4) 0.4637(4) 0.0266(10) Uani 1 1 d . . . . . H3 H 0.469801 0.609992 0.498926 0.032 Uiso 1 1 calc R U . . . C4 C 0.5251(2) 0.7365(4) 0.4956(3) 0.0245(9) Uani 1 1 d . . . . . C5 C 0.5485(3) 0.7449(4) 0.5814(3) 0.0284(10) Uani 1 1 d . . . . . H5A H 0.533570 0.700212 0.619513 0.034 Uiso 1 1 calc R U . . . C6 C 0.5922(3) 0.8174(4) 0.6082(3) 0.0267(10) Uani 1 1 d . . . . . H6 H 0.606466 0.821859 0.663969 0.032 Uiso 1 1 calc R U . . . C7 C 0.6159(2) 0.8863(4) 0.5501(3) 0.0253(10) Uani 1 1 d . . . . . C8 C 0.6641(2) 0.9596(4) 0.5697(3) 0.0244(9) Uani 1 1 d . . . . . H8A H 0.681703 0.966891 0.624025 0.029 Uiso 1 1 calc R U . . . C9 C 0.6849(2) 1.0205(4) 0.5082(3) 0.0270(10) Uani 1 1 d . . . . . H9 H 0.716763 1.068378 0.520694 0.032 Uiso 1 1 calc R U . . . C10 C 0.6574(2) 1.0088(4) 0.4266(3) 0.0223(9) Uani 1 1 d . . . . . C11 C 0.5913(2) 0.8812(4) 0.4675(3) 0.0209(9) Uani 1 1 d . . . . . C12 C 0.5450(2) 0.8063(4) 0.4380(3) 0.0227(9) Uani 1 1 d . . . . . C13 C 0.6631(3) 0.7356(4) 0.2527(4) 0.0353(10) Uani 1 1 d . . . . . C14 C 0.6858(3) 0.6632(5) 0.1986(4) 0.0425(13) Uani 1 1 d . . . . . H14 H 0.713266 0.612220 0.219143 0.051 Uiso 1 1 calc R U . . . C15 C 0.6668(3) 0.6685(5) 0.1151(4) 0.0427(13) Uani 1 1 d . . . . . H15 H 0.682898 0.623014 0.078507 0.051 Uiso 1 1 calc R U . . . C16 C 0.6227(3) 0.7437(4) 0.0857(4) 0.0365(11) Uani 1 1 d . . . . . C17 C 0.5977(3) 0.7532(4) 0.0007(4) 0.0375(11) Uani 1 1 d . . . . . H17 H 0.611891 0.709498 -0.038683 0.045 Uiso 1 1 calc R U . . . C18 C 0.5542(3) 0.8245(4) -0.0228(4) 0.0379(12) Uani 1 1 d . . . . . H18 H 0.540142 0.830673 -0.078562 0.045 Uiso 1 1 calc R U . . . C19 C 0.5287(3) 0.8913(4) 0.0356(3) 0.0324(10) Uani 1 1 d . . . . . C20 C 0.4807(3) 0.9641(4) 0.0181(3) 0.0362(11) Uani 1 1 d . . . . . H20 H 0.462564 0.972041 -0.035911 0.043 Uiso 1 1 calc R U . . . C21 C 0.4604(3) 1.0236(4) 0.0794(3) 0.0309(11) Uani 1 1 d . . . . . H21 H 0.428503 1.071477 0.067277 0.037 Uiso 1 1 calc R U . . . C22 C 0.4881(2) 1.0118(4) 0.1606(3) 0.0257(10) Uani 1 1 d . . . . . C23 C 0.5546(3) 0.8840(4) 0.1189(3) 0.0282(11) Uani 1 1 d . . . . . C24 C 0.6021(3) 0.8107(4) 0.1440(3) 0.0302(9) Uani 1 1 d . . . . . C27 C 0.4681(2) 0.7269(4) 0.2362(3) 0.0250(10) Uani 1 1 d . . . . . C28 C 0.4638(3) 0.6240(5) 0.1102(4) 0.0343(12) Uani 1 1 d . . . . . H28A H 0.500498 0.599662 0.083545 0.041 Uiso 1 1 calc R U . . . H28B H 0.450018 0.687016 0.084041 0.041 Uiso 1 1 calc R U . . . C29 C 0.4096(3) 0.5473(4) 0.0978(3) 0.0318(10) Uani 1 1 d . . . . . H29A H 0.422913 0.485395 0.126193 0.038 Uiso 1 1 calc R U . . . H29B H 0.402099 0.532026 0.039260 0.038 Uiso 1 1 calc R U . . . C30 C 0.3469(2) 0.5829(4) 0.1292(3) 0.0303(10) Uani 1 1 d . . . . . H30A H 0.317813 0.526148 0.130088 0.036 Uiso 1 1 calc R U . . . H30B H 0.355525 0.606831 0.185636 0.036 Uiso 1 1 calc R U . . . C31 C 0.3146(3) 0.6663(4) 0.0772(4) 0.0367(12) Uani 1 1 d . . . . . H31A H 0.307580 0.644244 0.020792 0.055 Uiso 1 1 calc R U . . . H31B H 0.341529 0.724975 0.080123 0.055 Uiso 1 1 calc R U . . . H31C H 0.274218 0.682393 0.097752 0.055 Uiso 1 1 calc R U . . . C32 C 0.6730(2) 1.0656(4) 0.3503(3) 0.0241(10) Uani 1 1 d . . . . . C33 C 0.7375(2) 1.1867(4) 0.2819(3) 0.0286(11) Uani 1 1 d . . . . . H33A H 0.702717 1.229514 0.259311 0.034 Uiso 1 1 calc R U . . . H33B H 0.745919 1.137196 0.240202 0.034 Uiso 1 1 calc R U . . . C34 C 0.7974(2) 1.2508(4) 0.3021(3) 0.0295(10) Uani 1 1 d . . . . . H34A H 0.828606 1.211287 0.336151 0.035 Uiso 1 1 calc R U . . . H34B H 0.816023 1.266616 0.251028 0.035 Uiso 1 1 calc R U . . . C35 C 0.7853(3) 1.3483(4) 0.3469(4) 0.0402(12) Uani 1 1 d . . . . . H35A H 0.763308 1.333632 0.395623 0.048 Uiso 1 1 calc R U . . . H35B H 0.757724 1.391386 0.310904 0.048 Uiso 1 1 calc R U . . . C36 C 0.8476(3) 1.4037(5) 0.3726(4) 0.0476(14) Uani 1 1 d . . . . . H36A H 0.872349 1.409891 0.325760 0.071 Uiso 1 1 calc R U . . . H36B H 0.871670 1.366610 0.415575 0.071 Uiso 1 1 calc R U . . . H36C H 0.838029 1.469676 0.392560 0.071 Uiso 1 1 calc R U . . . C37 C 0.6837(3) 0.7322(4) 0.3450(4) 0.0348(12) Uani 1 1 d . . . . . C38 C 0.6761(3) 0.6301(5) 0.4724(4) 0.0403(13) Uani 1 1 d . . . . . H38A H 0.641733 0.586340 0.487129 0.048 Uiso 1 1 calc R U . . . H38B H 0.670369 0.695050 0.498218 0.048 Uiso 1 1 calc R U . . . C39 C 0.7389(3) 0.5862(4) 0.5067(3) 0.0350(12) Uani 1 1 d . . . . . H39A H 0.773836 0.627466 0.490047 0.042 Uiso 1 1 calc R U . . . H39B H 0.743704 0.518930 0.484694 0.042 Uiso 1 1 calc R U . . . C40 C 0.7419(3) 0.5817(4) 0.6013(3) 0.0358(11) Uani 1 1 d . . . . . H40A H 0.737155 0.649257 0.622843 0.043 Uiso 1 1 calc R U . . . H40B H 0.706450 0.541336 0.617475 0.043 Uiso 1 1 calc R U . . . C41 C 0.8040(3) 0.5372(5) 0.6388(4) 0.0485(15) Uani 1 1 d . . . . . H41A H 0.839123 0.578837 0.625176 0.073 Uiso 1 1 calc R U . . . H41B H 0.809123 0.470602 0.617202 0.073 Uiso 1 1 calc R U . . . H41C H 0.803405 0.533940 0.697783 0.073 Uiso 1 1 calc R U . . . C42 C 0.4725(3) 1.0659(4) 0.2373(3) 0.0267(11) Uani 1 1 d . . . . . C43 C 0.4261(6) 1.2065(8) 0.3103(6) 0.035(2) Uani 0.648(12) 1 d . U P C 1 H43A H 0.468169 1.231169 0.330678 0.042 Uiso 0.648(12) 1 d R U P C 1 H43B H 0.409849 1.165629 0.353438 0.042 Uiso 0.648(12) 1 d R U P C 1 C44 C 0.3814(4) 1.2944(6) 0.2917(5) 0.0322(18) Uani 0.648(12) 1 d . U P C 1 H44A H 0.339158 1.269231 0.272412 0.039 Uiso 0.648(12) 1 calc R U P C 1 H44B H 0.396917 1.334640 0.247686 0.039 Uiso 0.648(12) 1 calc R U P C 1 C45 C 0.3762(5) 1.3601(8) 0.3669(6) 0.039(2) Uani 0.648(12) 1 d . U P C 1 H45A H 0.359347 1.320122 0.410128 0.047 Uiso 0.648(12) 1 calc R U P C 1 H45B H 0.418669 1.382980 0.387233 0.047 Uiso 0.648(12) 1 calc R U P C 1 C46 C 0.3335(5) 1.4505(8) 0.3492(6) 0.036(2) Uani 0.648(12) 1 d . U P C 1 H46A H 0.290312 1.428479 0.334679 0.054 Uiso 0.648(12) 1 calc R U P C 1 H46B H 0.348375 1.488295 0.304205 0.054 Uiso 0.648(12) 1 calc R U P C 1 H46C H 0.334697 1.492459 0.397579 0.054 Uiso 0.648(12) 1 calc R U P C 1 C43' C 0.3981(10) 1.1890(14) 0.2916(12) 0.032(3) Uani 0.352(12) 1 d . U P C 2 H43C H 0.353807 1.201496 0.271504 0.038 Uiso 0.352(12) 1 d R U P C 2 H43D H 0.399647 1.150446 0.342544 0.038 Uiso 0.352(12) 1 d R U P C 2 C44' C 0.4359(8) 1.2842(13) 0.3017(10) 0.038(3) Uani 0.352(12) 1 d . U P C 2 H44C H 0.431644 1.320283 0.249481 0.045 Uiso 0.352(12) 1 calc R U P C 2 H44D H 0.480840 1.266724 0.313161 0.045 Uiso 0.352(12) 1 calc R U P C 2 C45' C 0.4170(10) 1.3566(13) 0.3706(11) 0.039(3) Uani 0.352(12) 1 d . U P C 2 H45C H 0.410472 1.317800 0.419829 0.046 Uiso 0.352(12) 1 calc R U P C 2 H45D H 0.451885 1.403476 0.384475 0.046 Uiso 0.352(12) 1 calc R U P C 2 C46' C 0.3552(11) 1.4166(16) 0.3439(12) 0.042(4) Uani 0.352(12) 1 d . U P C 2 H46D H 0.319150 1.371655 0.339487 0.063 Uiso 0.352(12) 1 calc R U P C 2 H46E H 0.359300 1.447829 0.291198 0.063 Uiso 0.352(12) 1 calc R U P C 2 H46F H 0.348880 1.467661 0.384301 0.063 Uiso 0.352(12) 1 calc R U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0254(3) 0.0215(3) 0.0138(3) -0.0001(4) -0.0010(2) -0.0015(3) Cl1 0.0425(6) 0.0298(6) 0.0320(6) -0.0069(5) 0.0050(5) -0.0077(5) Cl2 0.0643(10) 0.0458(7) 0.0336(6) -0.0020(7) -0.0080(6) 0.0234(7) N1 0.031(2) 0.031(2) 0.026(2) -0.0071(19) -0.0038(17) 0.0053(17) N2 0.0235(18) 0.0186(17) 0.0196(19) 0.0001(15) 0.0004(14) -0.0015(14) N3 0.0223(19) 0.0248(19) 0.020(2) 0.0020(17) 0.0012(15) 0.0004(15) N4 0.028(2) 0.033(2) 0.022(2) -0.0009(18) -0.0036(16) -0.0073(18) N5 0.053(3) 0.038(3) 0.034(3) 0.004(2) -0.003(2) 0.008(2) N6 0.035(2) 0.025(2) 0.022(2) -0.0008(17) 0.0033(17) 0.0007(17) N7 0.026(2) 0.0217(19) 0.0163(19) 0.0014(16) -0.0016(15) -0.0025(15) N8 0.056(3) 0.051(3) 0.026(3) 0.013(2) 0.006(2) 0.027(3) O1 0.0346(17) 0.0256(17) 0.0219(17) 0.0008(14) 0.0014(14) -0.0010(14) O2 0.0289(16) 0.0258(17) 0.0147(15) 0.0001(13) -0.0011(12) -0.0064(13) O3 0.039(2) 0.041(2) 0.045(3) -0.012(2) -0.0030(18) 0.0071(18) O4 0.0297(17) 0.0241(16) 0.0218(17) 0.0012(14) 0.0003(13) 0.0033(13) O5 0.035(3) 0.042(3) 0.026(3) -0.008(2) -0.009(2) -0.003(2) O6 0.046(4) 0.036(3) 0.037(3) 0.005(2) 0.006(3) -0.005(2) O7 0.041(3) 0.108(7) 0.042(3) -0.031(4) 0.008(3) -0.038(3) O8 0.157(9) 0.024(3) 0.069(5) 0.009(3) 0.060(6) 0.009(4) O5' 0.037(8) 0.037(8) 0.037(8) 0.000(2) 0.003(2) 0.000(2) O8' 0.041(12) 0.036(13) 0.047(12) 0.008(10) 0.000(9) 0.016(10) O7' 0.035(7) 0.037(7) 0.038(7) -0.004(4) -0.004(4) -0.007(4) O6' 0.065(18) 0.09(2) 0.050(17) 0.011(15) 0.023(14) -0.018(15) O9 0.088(4) 0.047(2) 0.040(2) -0.007(2) 0.000(2) 0.029(2) O10 0.130(7) 0.051(4) 0.042(3) -0.014(3) 0.003(4) 0.018(4) O11 0.162(9) 0.066(5) 0.075(5) 0.019(4) 0.055(5) 0.017(5) O12 0.095(6) 0.068(5) 0.111(8) -0.012(5) -0.060(6) 0.038(4) O11' 0.061(19) 0.033(14) 0.048(17) 0.002(13) -0.009(14) 0.031(13) O10' 0.08(2) 0.030(16) 0.10(2) 0.014(17) -0.01(2) 0.001(15) O12' 0.047(17) 0.062(18) 0.05(2) -0.007(16) 0.010(15) 0.038(14) C1 0.0251(7) 0.023(2) 0.023(2) -0.0034(19) -0.0025(17) -0.0026(17) C2 0.0251(7) 0.030(2) 0.032(3) 0.001(2) 0.0016(19) -0.0060(18) C3 0.0251(7) 0.025(2) 0.030(3) 0.003(2) 0.0032(19) -0.0014(17) C4 0.0251(7) 0.026(2) 0.022(2) 0.0010(19) -0.0007(17) 0.0039(18) C5 0.035(2) 0.031(3) 0.019(2) 0.005(2) 0.0012(19) 0.004(2) C6 0.036(2) 0.029(2) 0.015(2) 0.0036(19) 0.0013(19) 0.0058(19) C7 0.0251(7) 0.028(2) 0.022(2) 0.002(2) -0.0048(18) 0.0023(19) C8 0.0251(7) 0.030(2) 0.017(2) -0.005(2) -0.0051(18) 0.0013(19) C9 0.0251(7) 0.030(2) 0.025(2) -0.004(2) -0.0046(19) -0.0013(19) C10 0.0251(7) 0.025(2) 0.017(2) -0.0012(18) -0.0006(17) -0.0027(18) C11 0.0251(7) 0.023(2) 0.014(2) 0.0008(17) -0.0009(17) 0.0015(17) C12 0.0251(7) 0.024(2) 0.018(2) 0.0005(19) -0.0009(17) 0.0019(18) C13 0.0552(12) 0.023(2) 0.029(3) 0.001(2) 0.011(2) 0.006(2) C14 0.0552(12) 0.033(3) 0.041(4) -0.004(2) 0.016(3) 0.011(2) C15 0.0552(12) 0.034(3) 0.042(4) -0.007(3) 0.021(3) 0.004(2) C16 0.0552(12) 0.029(3) 0.027(3) -0.003(2) 0.016(2) -0.002(2) C17 0.0552(12) 0.030(3) 0.029(3) -0.008(2) 0.015(2) -0.009(2) C18 0.0552(12) 0.039(3) 0.019(3) -0.001(2) 0.004(2) -0.015(3) C19 0.0552(12) 0.029(3) 0.013(2) 0.001(2) 0.006(2) -0.012(2) C20 0.0552(12) 0.035(3) 0.016(2) 0.007(2) -0.006(2) -0.014(3) C21 0.035(2) 0.037(3) 0.019(2) 0.007(2) -0.002(2) -0.007(2) C22 0.026(2) 0.026(2) 0.024(3) 0.005(2) -0.0035(19) -0.0053(18) C23 0.038(2) 0.026(2) 0.021(3) 0.0032(19) 0.005(2) -0.009(2) C24 0.0552(12) 0.024(2) 0.012(2) -0.0034(18) 0.010(2) -0.007(2) C27 0.023(2) 0.032(2) 0.021(2) -0.0003(19) 0.0028(17) -0.0028(18) C28 0.032(3) 0.046(3) 0.025(3) -0.011(2) 0.004(2) 0.003(2) C29 0.038(3) 0.031(2) 0.026(2) -0.007(2) -0.001(2) 0.001(2) C30 0.034(2) 0.027(2) 0.030(2) -0.0067(19) 0.0021(19) -0.0003(18) C31 0.038(3) 0.036(3) 0.035(3) -0.004(2) -0.001(2) 0.005(2) C32 0.022(2) 0.025(2) 0.024(3) 0.0016(19) -0.0013(18) -0.0007(17) C33 0.027(2) 0.037(3) 0.022(2) 0.004(2) 0.0024(19) -0.007(2) C34 0.026(2) 0.033(3) 0.029(2) 0.0024(19) 0.0008(18) -0.0082(19) C35 0.039(3) 0.039(3) 0.045(3) -0.004(2) 0.014(2) -0.007(2) C36 0.046(3) 0.051(3) 0.047(4) -0.016(3) 0.009(3) -0.017(3) C37 0.037(3) 0.030(3) 0.036(3) -0.002(2) -0.003(2) 0.011(2) C38 0.043(3) 0.045(3) 0.033(3) 0.001(3) 0.007(2) 0.008(3) C39 0.046(3) 0.032(3) 0.028(3) -0.002(2) 0.007(2) 0.004(2) C40 0.054(3) 0.026(2) 0.027(3) -0.003(2) 0.004(2) -0.006(2) C41 0.045(3) 0.051(4) 0.048(4) -0.008(3) -0.002(3) -0.001(3) C42 0.036(3) 0.027(2) 0.018(2) 0.0077(19) 0.003(2) 0.0024(19) C43 0.042(5) 0.036(5) 0.025(4) -0.004(4) 0.002(4) 0.013(4) C44 0.039(4) 0.034(4) 0.023(4) -0.002(3) 0.002(3) 0.005(3) C45 0.044(5) 0.047(5) 0.026(4) -0.004(4) 0.003(4) 0.014(4) C46 0.033(5) 0.032(5) 0.042(5) -0.006(4) 0.000(4) 0.012(4) C43' 0.034(7) 0.033(7) 0.027(7) 0.013(5) -0.004(6) -0.001(6) C44' 0.042(7) 0.040(7) 0.030(6) 0.003(5) -0.001(5) 0.012(6) C45' 0.046(7) 0.037(6) 0.033(6) 0.000(5) 0.004(6) -0.005(6) C46' 0.048(10) 0.037(10) 0.040(8) 0.002(8) 0.004(8) 0.029(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 N3 Ni1 N2 78.18(17) . . ? N3 Ni1 N6 111.15(17) . . ? N3 Ni1 N7 167.49(14) . . ? N3 Ni1 O2 77.11(15) . . ? N3 Ni1 O4 93.65(16) . . ? N6 Ni1 N2 88.09(13) . . ? N7 Ni1 N2 111.02(16) . . ? N7 Ni1 N6 78.38(18) . . ? N7 Ni1 O2 94.15(15) . . ? N7 Ni1 O4 77.23(16) . . ? O2 Ni1 N2 154.81(14) . . ? O2 Ni1 N6 96.27(15) . . ? O2 Ni1 O4 89.97(11) . . ? O4 Ni1 N2 96.42(14) . . ? O4 Ni1 N6 155.19(16) . . ? O5 Cl1 O6 110.5(4) . . ? O5 Cl1 O7 107.5(4) . . ? O6 Cl1 O7 110.1(4) . . ? O8 Cl1 O5 110.7(5) . . ? O8 Cl1 O6 110.8(4) . . ? O8 Cl1 O7 107.2(6) . . ? O5' Cl1 O8' 102.4(16) . . ? O5' Cl1 O7' 109.6(14) . . ? O8' Cl1 O7' 105.0(14) . . ? O6' Cl1 O5' 114(2) . . ? O6' Cl1 O8' 112(2) . . ? O6' Cl1 O7' 113(2) . . ? O9 Cl2 O10 110.2(4) . . ? O9 Cl2 O11 112.3(4) . . ? O9 Cl2 O12 109.6(4) . . ? O9 Cl2 O11' 108.6(12) . . ? O10 Cl2 O11 105.3(5) . . ? O12 Cl2 O10 109.3(6) . . ? O12 Cl2 O11 110.1(7) . . ? O10' Cl2 O9 96.4(17) . . ? O10' Cl2 O11' 123(3) . . ? O10' Cl2 O12' 120(3) . . ? O12' Cl2 O9 117.6(19) . . ? O12' Cl2 O11' 93(2) . . ? C27 N1 H1 118.9 . . ? C27 N1 C28 122.2(5) . . ? C28 N1 H1 118.9 . . ? C1 N2 Ni1 132.2(3) . . ? C1 N2 C12 117.6(4) . . ? C12 N2 Ni1 109.8(3) . . ? C10 N3 Ni1 120.4(3) . . ? C10 N3 C11 120.3(4) . . ? C11 N3 Ni1 119.2(3) . . ? C32 N4 H4 119.4 . . ? C32 N4 C33 121.2(4) . . ? C33 N4 H4 119.4 . . ? C37 N5 H5 118.4 . . ? C37 N5 C38 123.1(6) . . ? C38 N5 H5 118.4 . . ? C13 N6 Ni1 133.1(4) . . ? C13 N6 C24 116.4(5) . . ? C24 N6 Ni1 110.1(4) . . ? C22 N7 Ni1 120.2(3) . . ? C22 N7 C23 121.5(4) . . ? C23 N7 Ni1 118.3(4) . . ? C42 N8 H8 120.4 . . ? C42 N8 C43 118.4(6) . . ? C42 N8 C43' 132.0(9) . . ? C43 N8 H8 121.2 . . ? C43' N8 H8 103.4 . . ? C32 O2 Ni1 113.7(3) . . ? C42 O4 Ni1 113.2(3) . . ? N2 C1 C2 121.5(5) . . ? N2 C1 C27 116.8(4) . . ? C2 C1 C27 121.7(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2 119.7 . . ? C2 C3 H3 120.3 . . ? C2 C3 C4 119.4(5) . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 123.7(5) . . ? C12 C4 C3 116.4(5) . . ? C12 C4 C5 119.9(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 C4 121.4(5) . . ? C6 C5 H5A 119.3 . . ? C5 C6 H6 120.0 . . ? C5 C6 C7 119.9(5) . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 124.8(5) . . ? C11 C7 C6 118.9(5) . . ? C11 C7 C8 116.3(5) . . ? C7 C8 H8A 119.9 . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8A 119.9 . . ? C8 C9 H9 120.5 . . ? C8 C9 C10 119.1(5) . . ? C10 C9 H9 120.5 . . ? N3 C10 C9 121.0(5) . . ? N3 C10 C32 110.8(4) . . ? C9 C10 C32 128.1(4) . . ? N3 C11 C7 123.1(4) . . ? N3 C11 C12 114.7(4) . . ? C7 C11 C12 122.2(4) . . ? N2 C12 C4 124.2(4) . . ? N2 C12 C11 118.0(4) . . ? C4 C12 C11 117.6(4) . . ? N6 C13 C14 123.1(6) . . ? N6 C13 C37 116.2(5) . . ? C14 C13 C37 120.7(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.5(6) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 120.3 . . ? C14 C15 C16 119.3(6) . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 123.8(5) . . ? C24 C16 C15 117.0(6) . . ? C24 C16 C17 119.2(5) . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.9(5) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.0 . . ? C17 C18 C19 122.0(6) . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 126.3(5) . . ? C20 C19 C23 116.5(5) . . ? C23 C19 C18 117.1(6) . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.9(5) . . ? C21 C20 H20 119.6 . . ? C20 C21 H21 120.3 . . ? C20 C21 C22 119.4(5) . . ? C22 C21 H21 120.3 . . ? N7 C22 C21 120.2(5) . . ? N7 C22 C42 111.0(4) . . ? C21 C22 C42 128.8(5) . . ? N7 C23 C19 121.5(5) . . ? N7 C23 C24 117.2(5) . . ? C19 C23 C24 121.3(5) . . ? N6 C24 C16 124.5(5) . . ? N6 C24 C23 116.0(5) . . ? C16 C24 C23 119.4(5) . . ? N1 C27 C1 114.3(4) . . ? O1 C27 N1 125.8(5) . . ? O1 C27 C1 119.9(5) . . ? N1 C28 H28A 109.2 . . ? N1 C28 H28B 109.2 . . ? N1 C28 C29 111.9(5) . . ? H28A C28 H28B 107.9 . . ? C29 C28 H28A 109.2 . . ? C29 C28 H28B 109.2 . . ? C28 C29 H29A 108.8 . . ? C28 C29 H29B 108.8 . . ? C28 C29 C30 113.6(4) . . ? H29A C29 H29B 107.7 . . ? C30 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? C29 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C31 C30 C29 113.3(5) . . ? C31 C30 H30A 108.9 . . ? C31 C30 H30B 108.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 C10 119.8(4) . . ? O2 C32 N4 122.2(5) . . ? O2 C32 C10 117.9(4) . . ? N4 C33 H33A 109.4 . . ? N4 C33 H33B 109.4 . . ? N4 C33 C34 111.4(4) . . ? H33A C33 H33B 108.0 . . ? C34 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C33 C34 H34A 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C35 C34 C33 114.2(4) . . ? C35 C34 H34A 108.7 . . ? C35 C34 H34B 108.7 . . ? C34 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C34 C35 C36 111.6(5) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C13 114.4(5) . . ? O3 C37 N5 124.2(6) . . ? O3 C37 C13 121.4(6) . . ? N5 C38 H38A 108.7 . . ? N5 C38 H38B 108.7 . . ? N5 C38 C39 114.2(5) . . ? H38A C38 H38B 107.6 . . ? C39 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C38 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C38 C39 C40 110.1(5) . . ? H39A C39 H39B 108.2 . . ? C40 C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? C39 C40 H40A 109.2 . . ? C39 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? C41 C40 C39 112.2(5) . . ? C41 C40 H40A 109.2 . . ? C41 C40 H40B 109.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N8 C42 C22 120.0(5) . . ? O4 C42 N8 121.8(5) . . ? O4 C42 C22 118.1(4) . . ? N8 C43 H43A 109.2 . . ? N8 C43 H43B 109.6 . . ? H43A C43 H43B 108.0 . . ? C44 C43 N8 111.3(7) . . ? C44 C43 H43A 109.7 . . ? C44 C43 H43B 109.0 . . ? C43 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C43 C44 C45 111.8(7) . . ? H44A C44 H44B 107.9 . . ? C45 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? C44 C45 H45A 109.0 . . ? C44 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? C46 C45 C44 112.9(8) . . ? C46 C45 H45A 109.0 . . ? C46 C45 H45B 109.0 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N8 C43' H43C 112.1 . . ? N8 C43' H43D 111.5 . . ? N8 C43' C44' 99.4(13) . . ? H43C C43' H43D 109.6 . . ? C44' C43' H43C 112.0 . . ? C44' C43' H43D 112.0 . . ? C43' C44' H44C 108.3 . . ? C43' C44' H44D 108.3 . . ? C43' C44' C45' 115.9(15) . . ? H44C C44' H44D 107.4 . . ? C45' C44' H44C 108.3 . . ? C45' C44' H44D 108.3 . . ? C44' C45' H45C 109.2 . . ? C44' C45' H45D 109.2 . . ? H45C C45' H45D 107.9 . . ? C46' C45' C44' 112.1(15) . . ? C46' C45' H45C 109.2 . . ? C46' C45' H45D 109.2 . . ? C45' C46' H46D 109.5 . . ? C45' C46' H46E 109.5 . . ? C45' C46' H46F 109.5 . . ? H46D C46' H46E 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? 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 Ni1 N2 2.198(4) . ? Ni1 N3 1.982(4) . ? Ni1 N6 2.192(4) . ? Ni1 N7 1.983(4) . ? Ni1 O2 2.140(3) . ? Ni1 O4 2.142(3) . ? Cl1 O5 1.421(5) . ? Cl1 O6 1.439(7) . ? Cl1 O7 1.450(6) . ? Cl1 O8 1.415(7) . ? Cl1 O5' 1.44(3) . ? Cl1 O8' 1.47(2) . ? Cl1 O7' 1.48(2) . ? Cl1 O6' 1.39(4) . ? Cl2 O9 1.414(5) . ? Cl2 O10 1.437(7) . ? Cl2 O11 1.453(9) . ? Cl2 O12 1.419(7) . ? Cl2 O11' 1.62(4) . ? Cl2 O10' 1.29(5) . ? Cl2 O12' 1.38(3) . ? N1 H1 0.8600 . ? N1 C27 1.331(7) . ? N1 C28 1.470(7) . ? N2 C1 1.340(6) . ? N2 C12 1.355(6) . ? N3 C10 1.326(6) . ? N3 C11 1.347(6) . ? N4 H4 0.8600 . ? N4 C32 1.315(7) . ? N4 C33 1.472(7) . ? N5 H5 0.8600 . ? N5 C37 1.365(8) . ? N5 C38 1.464(8) . ? N6 C13 1.335(7) . ? N6 C24 1.383(7) . ? N7 C22 1.336(7) . ? N7 C23 1.336(7) . ? N8 H8 0.8598 . ? N8 C42 1.303(7) . ? N8 C43 1.553(11) . ? N8 C43' 1.40(2) . ? O1 C27 1.227(7) . ? O2 C32 1.253(6) . ? O3 C37 1.221(7) . ? O4 C42 1.269(6) . ? C1 C2 1.404(7) . ? C1 C27 1.507(7) . ? C2 H2 0.9300 . ? C2 C3 1.359(8) . ? C3 H3 0.9300 . ? C3 C4 1.409(7) . ? C4 C5 1.438(7) . ? C4 C12 1.404(7) . ? C5 H5A 0.9300 . ? C5 C6 1.372(8) . ? C6 H6 0.9300 . ? C6 C7 1.432(7) . ? C7 C8 1.418(7) . ? C7 C11 1.394(7) . ? C8 H8A 0.9300 . ? C8 C9 1.384(8) . ? C9 H9 0.9300 . ? C9 C10 1.405(7) . ? C10 C32 1.510(7) . ? C11 C12 1.441(7) . ? C13 C14 1.411(8) . ? C13 C37 1.522(8) . ? C14 H14 0.9300 . ? C14 C15 1.380(10) . ? C15 H15 0.9300 . ? C15 C16 1.413(9) . ? C16 C17 1.438(9) . ? C16 C24 1.394(7) . ? C17 H17 0.9300 . ? C17 C18 1.345(9) . ? C18 H18 0.9300 . ? C18 C19 1.434(8) . ? C19 C20 1.404(9) . ? C19 C23 1.414(8) . ? C20 H20 0.9300 . ? C20 C21 1.366(9) . ? C21 H21 0.9300 . ? C21 C22 1.401(7) . ? C22 C42 1.496(7) . ? C23 C24 1.425(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.523(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.524(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.514(7) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.526(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 C35 1.516(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 C36 1.522(8) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 C39 1.500(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 C40 1.532(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 C41 1.506(8) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C43 H43A 0.9699 . ? C43 H43B 0.9702 . ? C43 C44 1.509(12) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 C45 1.512(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 C46 1.508(14) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C43' H43C 0.9700 . ? C43' H43D 0.9701 . ? C43' C44' 1.49(3) . ? C44' H44C 0.9700 . ? C44' H44D 0.9700 . ? C44' C45' 1.55(2) . ? C45' H45C 0.9700 . ? C45' H45D 0.9700 . ? C45' C46' 1.55(3) . ? C46' H46D 0.9600 . ? C46' H46E 0.9600 . ? C46' H46F 0.9600 . ? 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 N1 H1 O12 0.86 2.15 2.916(9) 148.0 . yes N4 H4 O5 0.86 2.16 2.937(7) 150.9 3 yes N5 H5 O10' 0.86 2.17 2.94(4) 148.6 . yes N8 H8 O7 0.86 2.20 2.926(8) 142.0 2_574 yes C45' H45D O12' 0.97 2.05 2.76(5) 128.3 1_565 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 Ni1 N2 C1 C2 173.3(4) . . . . ? Ni1 N2 C1 C27 -6.5(7) . . . . ? Ni1 N2 C12 C4 -177.9(4) . . . . ? Ni1 N2 C12 C11 -0.9(5) . . . . ? Ni1 N3 C10 C9 -180.0(4) . . . . ? Ni1 N3 C10 C32 0.3(6) . . . . ? Ni1 N3 C11 C7 179.5(4) . . . . ? Ni1 N3 C11 C12 3.1(5) . . . . ? Ni1 N6 C13 C14 174.5(5) . . . . ? Ni1 N6 C13 C37 -5.6(8) . . . . ? Ni1 N6 C24 C16 -177.6(5) . . . . ? Ni1 N6 C24 C23 0.3(6) . . . . ? Ni1 N7 C22 C21 -179.8(4) . . . . ? Ni1 N7 C22 C42 -0.7(5) . . . . ? Ni1 N7 C23 C19 179.4(4) . . . . ? Ni1 N7 C23 C24 1.3(6) . . . . ? Ni1 O2 C32 N4 179.3(4) . . . . ? Ni1 O2 C32 C10 1.6(5) . . . . ? Ni1 O4 C42 N8 -172.6(5) . . . . ? Ni1 O4 C42 C22 5.1(6) . . . . ? N1 C28 C29 C30 65.1(6) . . . . ? N2 C1 C2 C3 2.4(8) . . . . ? N2 C1 C27 N1 124.4(5) . . . . ? N2 C1 C27 O1 -56.5(6) . . . . ? N3 C10 C32 N4 -179.1(4) . . . . ? N3 C10 C32 O2 -1.3(6) . . . . ? N3 C11 C12 N2 -1.2(6) . . . . ? N3 C11 C12 C4 175.9(4) . . . . ? N4 C33 C34 C35 -75.7(6) . . . . ? N5 C38 C39 C40 176.3(5) . . . . ? N6 C13 C14 C15 0.5(10) . . . . ? N6 C13 C37 N5 123.0(6) . . . . ? N6 C13 C37 O3 -53.4(8) . . . . ? N7 C22 C42 N8 174.6(5) . . . . ? N7 C22 C42 O4 -3.1(7) . . . . ? N7 C23 C24 N6 -1.0(7) . . . . ? N7 C23 C24 C16 177.0(5) . . . . ? N8 C43 C44 C45 -178.8(8) . . . . ? N8 C43' C44' C45' -174.4(13) . . . . ? C1 N2 C12 C4 -4.1(7) . . . . ? C1 N2 C12 C11 172.8(4) . . . . ? C1 C2 C3 C4 -3.3(8) . . . . ? C2 C1 C27 N1 -55.5(6) . . . . ? C2 C1 C27 O1 123.7(6) . . . . ? C2 C3 C4 C5 -176.3(5) . . . . ? C2 C3 C4 C12 0.7(7) . . . . ? C3 C4 C5 C6 174.0(5) . . . . ? C3 C4 C12 N2 3.2(7) . . . . ? C3 C4 C12 C11 -173.8(4) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C5 C4 C12 N2 -179.8(4) . . . . ? C5 C4 C12 C11 3.3(7) . . . . ? C5 C6 C7 C8 -175.6(5) . . . . ? C5 C6 C7 C11 3.1(8) . . . . ? C6 C7 C8 C9 177.9(5) . . . . ? C6 C7 C11 N3 -178.9(5) . . . . ? C6 C7 C11 C12 -2.7(7) . . . . ? C7 C8 C9 C10 0.4(8) . . . . ? C7 C11 C12 N2 -177.7(4) . . . . ? C7 C11 C12 C4 -0.5(7) . . . . ? C8 C7 C11 N3 0.0(7) . . . . ? C8 C7 C11 C12 176.2(4) . . . . ? C8 C9 C10 N3 0.9(8) . . . . ? C8 C9 C10 C32 -179.4(5) . . . . ? C9 C10 C32 N4 1.2(8) . . . . ? C9 C10 C32 O2 179.0(5) . . . . ? C10 N3 C11 C7 1.4(7) . . . . ? C10 N3 C11 C12 -175.1(4) . . . . ? C11 N3 C10 C9 -1.8(7) . . . . ? C11 N3 C10 C32 178.5(4) . . . . ? C11 C7 C8 C9 -0.9(7) . . . . ? C12 N2 C1 C2 1.3(7) . . . . ? C12 N2 C1 C27 -178.6(4) . . . . ? C12 C4 C5 C6 -2.9(8) . . . . ? C13 N6 C24 C16 -4.0(8) . . . . ? C13 N6 C24 C23 173.8(5) . . . . ? C13 C14 C15 C16 -2.8(10) . . . . ? C14 C13 C37 N5 -57.1(8) . . . . ? C14 C13 C37 O3 126.6(6) . . . . ? C14 C15 C16 C17 -177.2(6) . . . . ? C14 C15 C16 C24 1.7(9) . . . . ? C15 C16 C17 C18 177.7(6) . . . . ? C15 C16 C24 N6 1.8(9) . . . . ? C15 C16 C24 C23 -176.0(5) . . . . ? C16 C17 C18 C19 -2.6(9) . . . . ? C17 C16 C24 N6 -179.2(5) . . . . ? C17 C16 C24 C23 3.0(8) . . . . ? C17 C18 C19 C20 -176.3(6) . . . . ? C17 C18 C19 C23 4.3(8) . . . . ? C18 C19 C20 C21 -179.9(5) . . . . ? C18 C19 C23 N7 179.5(5) . . . . ? C18 C19 C23 C24 -2.4(8) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? C19 C23 C24 N6 -179.1(5) . . . . ? C19 C23 C24 C16 -1.2(8) . . . . ? C20 C19 C23 N7 0.1(8) . . . . ? C20 C19 C23 C24 178.2(5) . . . . ? C20 C21 C22 N7 0.5(8) . . . . ? C20 C21 C22 C42 -178.3(5) . . . . ? C21 C22 C42 N8 -6.4(9) . . . . ? C21 C22 C42 O4 175.8(5) . . . . ? C22 N7 C23 C19 0.7(7) . . . . ? C22 N7 C23 C24 -177.4(4) . . . . ? C23 N7 C22 C21 -1.0(7) . . . . ? C23 N7 C22 C42 178.0(4) . . . . ? C23 C19 C20 C21 -0.6(8) . . . . ? C24 N6 C13 C14 2.8(9) . . . . ? C24 N6 C13 C37 -177.3(5) . . . . ? C24 C16 C17 C18 -1.2(9) . . . . ? C27 N1 C28 C29 -106.7(6) . . . . ? C27 C1 C2 C3 -177.8(5) . . . . ? C28 N1 C27 O1 -3.1(8) . . . . ? C28 N1 C27 C1 176.0(5) . . . . ? C28 C29 C30 C31 70.5(6) . . . . ? C32 N4 C33 C34 -171.0(5) . . . . ? C33 N4 C32 O2 -1.7(8) . . . . ? C33 N4 C32 C10 175.9(5) . . . . ? C33 C34 C35 C36 174.5(5) . . . . ? C37 N5 C38 C39 -95.0(7) . . . . ? C37 C13 C14 C15 -179.4(6) . . . . ? C38 N5 C37 O3 6.8(9) . . . . ? C38 N5 C37 C13 -169.4(5) . . . . ? C38 C39 C40 C41 179.5(5) . . . . ? C42 N8 C43 C44 175.5(7) . . . . ? C42 N8 C43' C44' 105.4(12) . . . . ? C43 N8 C42 O4 7.9(10) . . . . ? C43 N8 C42 C22 -169.7(6) . . . . ? C43 C44 C45 C46 178.0(9) . . . . ? C43' N8 C42 O4 -19.2(16) . . . . ? C43' N8 C42 C22 163.2(13) . . . . ? C43' C44' C45' C46' -77.4(19) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.34(3) 2 0.66(3)