#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:51:24 +0100 (Fri, 22 May 2026) $ #$Revision: 306072 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721045.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_7721045 loop_ _publ_author_name 'Zuo, Jing' 'Zhang, Jun' 'Li, Hongxiu' 'Hu, Chaojie' 'Zhao, Mei-Xin' _publ_section_title ; Nickel Complexes Supported by a New Class of Fused Imidazonaphthyridine Tridentate N,N,N-Ligands for Ethylene Oligomerization and Isolation of a Key Ni-Al Intermediate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00825A _journal_year 2026 _chemical_formula_moiety 'C40 H43 Cl2 N5 Ni O' _chemical_formula_sum 'C40 H43 Cl2 N5 Ni O' _chemical_formula_weight 739.40 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _audit_creation_date 2026-01-29 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2026-03-31 deposited with the CCDC. 2026-05-19 downloaded from the CCDC. ; _cell_angle_alpha 116.0100(10) _cell_angle_beta 92.7180(10) _cell_angle_gamma 105.9430(10) _cell_formula_units_Z 2 _cell_length_a 9.8014(2) _cell_length_b 15.5910(3) _cell_length_c 16.5325(3) _cell_measurement_reflns_used 9875 _cell_measurement_temperature 200.0 _cell_measurement_theta_max 74.806 _cell_measurement_theta_min 3.032 _cell_volume 2141.59(8) _computing_cell_refinement 'SAINT V8.41 (?, 2016)' _computing_data_reduction 'SAINT V8.41 (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 200.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 44850 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.883 _diffrn_reflns_theta_min 3.340 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.058 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.6851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.147 _exptl_crystal_description needle _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.266 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 485 _refine_ls_number_reflns 8765 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0480P)^2^+0.3177P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.0951 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7284 _reflns_number_total 8765 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00825a2.cif _cod_data_source_block a_CCDC2 _cod_original_cell_volume 2141.58(7) _cod_database_code 7721045 _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 0.980 _shelx_estimated_absorpt_t_min 0.904 _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.058) H3(0.073) H4(0.075) H5(0.08) H6(0.064) H7A(0.045) H7B(0.045) H13(0.061) H1(0.078) H11(0.072) H10(0.059) H9(0.061) H9A(0.063) H13A(0.053) H12A(0.074) H11A(0.078) H10A(0.084) H15(0.044) H19(0.043) H20(0.051) H21A(0.096) H21B(0.096) H21C(0.096) H22A(0.098) H22B(0.098) H22C(0.098) H23(0.063) H24A(0.124) H24B(0.124) H24C(0.124) H25A(0.1) H25B(0.1) H25C(0.1) H27A(0.073) H27B(0.073) H27C(0.073) H29(0.042) H30(0.042) H33(0.043) H34(0.044) H36(0.047) H37(0.045) H38(0.043) H39A(0.098) H39C(0.098) H39B(0.098) H39E(0.098) H39D(0.098) H39F(0.098) H40A(0.086) H40B(0.086) H12(0.086) H38A(0.047) H40D(0.059) H40E(0.059) H40F(0.059) Fixed X: H2(0.406953) H3(0.279064) H4(0.317749) H5(0.484815) H6(0.612697) H7A(0.702204) H7B(0.703194) H13(0.318847) H1(0.193563) H11(0.313141) H10(0.558003) H9(0.68329) H9A(0.731036) H13A(0.334469) H12A(0.237235) H11A(0.3869) H10A(0.633801) H15(0.756001) H19(0.46992) H20(0.802765) H21A(0.958582) H21B(1.012332) H21C(0.998902) H22A(0.634968) H22B(0.791082) H22C(0.737554) H23(0.458954) H24A(0.261343) H24B(0.22228) H24C(0.257546) H25A(0.583879) H25B(0.423522) H25C(0.459845) H27A(0.40168) H27B(0.408168) H27C(0.317537) H29(0.360289) H30(0.403568) H33(0.587393) H34(0.804902) H36(1.057261) H37(1.124508) H38(0.820193) H39A(1.18915) H39C(1.209216) H39B(1.174139) H39E(1.260358) H39D(1.109481) H39F(1.115098) H40A(0.949429) H40B(0.993779) H12(0.838981) H38A(1.030009) H40D(1.303174) H40E(1.153798) H40F(1.204383) Fixed Y: H2(0.691464) H3(0.60779) H4(0.684132) H5(0.845362) H6(0.930269) H7A(0.920153) H7B(0.916265) H13(0.885046) H1(0.987755) H11(1.125306) H10(1.160149) H9(1.057441) H9A(1.051737) H13A(0.886199) H12A(1.003678) H11A(1.145188) H10A(1.169219) H15(0.756671) H19(0.847919) H20(0.587877) H21A(0.714981) H21B(0.634502) H21C(0.731356) H22A(0.502339) H22B(0.492924) H22C(0.570522) H23(0.701972) H24A(0.75257) H24B(0.705945) H24C(0.639526) H25A(0.878679) H25B(0.852015) H25C(0.898883) H27A(0.423776) H27B(0.531464) H27C(0.48897) H29(0.375064) H30(0.316046) H33(0.337317) H34(0.427835) H36(0.602482) H37(0.723968) H38(0.84293) H39A(0.912573) H39C(1.018637) H39B(0.917937) H39E(0.972294) H39D(0.991753) H39F(0.878909) H40A(0.988243) H40B(1.06649) H12(0.979773) H38A(0.831707) H40D(1.013144) H40E(0.997847) H40F(1.079498) Fixed Z: H2(0.022667) H3(-0.127752) H4(-0.221357) H5(-0.163955) H6(-0.013664) H7A(0.122982) H7B(0.120673) H13(0.084871) H1(0.175784) H11(0.318871) H10(0.371046) H9(0.280134) H9A(0.268786) H13A(0.105784) H12A(0.206678) H11A(0.338626) H10A(0.369682) H15(0.093592) H19(0.248224) H20(0.177678) H21A(0.107554) H21B(0.12348) H21C(0.209403) H22A(0.036824) H22B(0.020768) H22C(-0.000293) H23(0.36447) H24A(0.273953) H24B(0.342315) H24C(0.24519) H25A(0.447455) H25B(0.467337) H25C(0.398904) H27A(0.147157) H27B(0.156434) H27C(0.216717) H29(0.274467) H30(0.37763) H33(0.513925) H34(0.612866) H36(0.668649) H37(0.607161) H38(0.387025) H39A(0.416016) H39C(0.417417) H39B(0.321668) H39E(0.387352) H39D(0.37911) H39F(0.330937) H40A(0.303816) H40B(0.411104) H12(0.37035) H38A(0.514286) H40D(0.580337) H40E(0.615984) H40F(0.580122) ; _smtbx_masks_special_details ; A solvent mask was calculated and 84 electrons were found in a volume of 424\%A^3^ in 1 void per unit cell. This is consistent with the presence of 1[C4H8O] per Asymmetric Unit which account for 80 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL A in P-1 #2 a.res created by SHELXL-2018/3 at 21:52:12 on 14-Jan-2026 REM reset to P-1 #2 CELL 1.54178 9.8014 15.591 16.5325 116.01 92.718 105.943 ZERR 2 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H Cl N Ni O UNIT 80 86 4 10 2 2 EADP C13 C8 C9 ISOR 0.002 0.001 C39 SADI N5 C40 N5A C40A EADP C38A N5A C40A L.S. 10 0 0 PLAN 99 SIZE 0.01 0.05 0.01 TEMP -73.15 CONF BOND MORE -1 BOND $H ABIN fmap 2 53 acta OMIT 0 -1 1 REM REM REM WGHT 0.048000 0.317700 FVAR 0.69952 0.33332 0.94238 NI1 5 0.821623 0.662937 0.393505 11.00000 0.02802 0.02567 = 0.03717 0.01974 0.00207 0.00332 CL2 3 0.721627 0.769256 0.508628 11.00000 0.03782 0.03169 = 0.04760 0.02326 0.01278 0.01059 CL3 3 0.933840 0.552736 0.292284 11.00000 0.03621 0.03849 = 0.03534 0.02256 0.00194 0.01275 O1 6 0.964229 0.785480 0.394044 11.00000 0.03500 0.02976 = 0.04908 0.02299 0.00819 0.00375 N1 4 0.638102 0.624116 0.283226 11.00000 0.02972 0.02991 = 0.03607 0.02209 -0.00212 0.00593 N2 4 0.672697 0.540909 0.384515 11.00000 0.02820 0.02559 = 0.03470 0.01959 0.00091 0.00610 N3 4 0.931514 0.643536 0.513033 11.00000 0.03206 0.02972 = 0.03575 0.01864 0.00122 0.00717 N4 4 0.868665 0.532839 0.568173 11.00000 0.03565 0.03486 = 0.03289 0.02242 0.00438 0.01383 PART 1 N5 4 1.002565 0.928930 0.381820 31.00000 0.04049 0.03070 = 0.04832 0.02458 0.00642 0.00409 PART 0 C1 1 0.523619 0.819566 0.020591 11.00000 0.04891 0.03577 = 0.03518 0.02349 0.00881 0.02016 C2 1 0.423680 0.723650 -0.014909 11.00000 0.07136 0.03425 = 0.03924 0.01984 -0.00275 0.01539 AFIX 43 H2 2 0.406953 0.691464 0.022667 11.00000 -1.20000 AFIX 0 C3 1 0.347390 0.673643 -0.104623 11.00000 0.08371 0.04265 = 0.04583 0.01364 -0.01063 0.02178 AFIX 43 H3 2 0.279064 0.607790 -0.127752 11.00000 -1.20000 AFIX 0 C4 1 0.369921 0.718535 -0.159944 11.00000 0.08675 0.07274 = 0.03199 0.01854 0.00287 0.04356 AFIX 43 H4 2 0.317749 0.684132 -0.221357 11.00000 -1.20000 AFIX 0 C5 1 0.468684 0.813810 -0.125845 11.00000 0.08888 0.09232 = 0.04534 0.04884 0.01744 0.03855 AFIX 43 H5 2 0.484815 0.845362 -0.163955 11.00000 -1.20000 AFIX 0 C6 1 0.544962 0.864282 -0.036378 11.00000 0.06711 0.05945 = 0.04960 0.04026 0.01295 0.01896 AFIX 43 H6 2 0.612697 0.930269 -0.013664 11.00000 -1.20000 AFIX 0 C7 1 0.601550 0.880099 0.120481 11.00000 0.04635 0.03126 = 0.03944 0.02506 0.00128 0.00694 PART 1 AFIX 13 H7A 2 0.702204 0.920153 0.122982 21.00000 -1.20000 AFIX 13 PART 2 H7B 2 0.703194 0.916265 0.120673 -21.00000 -1.20000 AFIX 66 PART 1 C8 1 0.512847 0.961586 0.173954 21.00000 0.08917 0.03597 = 0.03429 0.01861 -0.00198 0.03038 C13 1 0.367394 0.940890 0.142962 21.00000 0.08917 0.03597 = 0.03429 0.01861 -0.00198 0.03038 AFIX 43 H13 2 0.318847 0.885046 0.084871 21.00000 -1.20000 AFIX 65 C12 1 0.292974 1.001900 0.196966 21.00000 0.09975 0.05321 = 0.06022 0.02878 0.02763 0.04599 AFIX 43 H12 2 0.193563 0.987755 0.175784 21.00000 -1.20000 AFIX 65 C11 1 0.364005 1.083608 0.281962 21.00000 0.10209 0.03231 = 0.06290 0.03230 0.04449 0.02458 AFIX 43 H11 2 0.313141 1.125306 0.318871 21.00000 -1.20000 AFIX 65 C10 1 0.509457 1.104305 0.312955 21.00000 0.10218 0.02310 = 0.02334 0.01169 0.00954 0.02057 AFIX 43 H10 2 0.558003 1.160149 0.371046 21.00000 -1.20000 AFIX 65 C9 1 0.583879 1.043295 0.258952 21.00000 0.08917 0.03597 = 0.03429 0.01861 -0.00198 0.03038 AFIX 43 H9 2 0.683290 1.057441 0.280134 21.00000 -1.20000 AFIX 66 PART 2 C9A 1 0.630799 1.041982 0.256179 -21.00000 0.07872 0.03370 = 0.04260 0.02057 0.00713 0.00987 AFIX 43 H9A 2 0.731036 1.051737 0.268786 -21.00000 -1.20000 AFIX 65 C8A 1 0.541894 0.957923 0.177800 -21.00000 0.05690 0.02468 = 0.03542 0.02512 0.00718 0.01619 C13A 1 0.395231 0.943649 0.159353 -21.00000 0.06039 0.04594 = 0.04041 0.02571 0.01052 0.02914 AFIX 43 H13A 2 0.334469 0.886199 0.105784 -21.00000 -1.20000 AFIX 65 C12A 1 0.337473 1.013434 0.219286 -21.00000 0.08104 0.06072 = 0.07454 0.04626 0.03417 0.04285 AFIX 43 H12A 2 0.237235 1.003678 0.206678 -21.00000 -1.20000 AFIX 65 C11A 1 0.426376 1.097493 0.297665 -21.00000 0.11337 0.03982 = 0.06203 0.03124 0.04555 0.03604 AFIX 43 H11A 2 0.386900 1.145188 0.338626 -21.00000 -1.20000 AFIX 65 C10A 1 0.573039 1.111768 0.316113 -21.00000 0.10680 0.03934 = 0.05043 0.01995 0.02645 0.00631 AFIX 43 H10A 2 0.633801 1.169219 0.369682 -21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.610946 0.812961 0.164430 11.00000 0.03994 0.02886 = 0.03721 0.02235 -0.00329 0.00438 C15 1 0.699358 0.753340 0.137857 11.00000 0.04414 0.03730 = 0.03373 0.02251 0.00304 0.01087 AFIX 43 H15 2 0.756001 0.756671 0.093592 11.00000 -1.20000 AFIX 0 C16 1 0.707837 0.688761 0.173918 11.00000 0.03880 0.03353 = 0.03124 0.01879 -0.00322 0.00853 C17 1 0.624166 0.684925 0.239721 11.00000 0.02869 0.02996 = 0.03759 0.02358 -0.00604 0.00207 C18 1 0.534614 0.744681 0.268640 11.00000 0.02692 0.03988 = 0.04864 0.03295 0.00164 0.00596 C19 1 0.530625 0.807358 0.229375 11.00000 0.03331 0.03519 = 0.04747 0.02824 0.00006 0.00849 AFIX 43 H19 2 0.469920 0.847919 0.248224 11.00000 -1.20000 AFIX 0 C20 1 0.801354 0.621916 0.138708 11.00000 0.05847 0.04789 = 0.03424 0.02586 0.00654 0.02576 AFIX 13 H20 2 0.802765 0.587877 0.177678 11.00000 -1.20000 AFIX 0 C21 1 0.956500 0.680900 0.145375 11.00000 0.05497 0.06918 = 0.06398 0.02402 0.00798 0.02887 AFIX 137 H21A 2 0.958582 0.714981 0.107554 11.00000 -1.50000 H21B 2 1.012332 0.634502 0.123480 11.00000 -1.50000 H21C 2 0.998902 0.731356 0.209403 11.00000 -1.50000 AFIX 0 C22 1 0.735331 0.539555 0.040185 11.00000 0.08456 0.04540 = 0.05664 0.01510 0.00207 0.02548 AFIX 137 H22A 2 0.634968 0.502339 0.036824 11.00000 -1.50000 H22B 2 0.791082 0.492924 0.020768 11.00000 -1.50000 H22C 2 0.737554 0.570522 -0.000293 11.00000 -1.50000 AFIX 0 C23 1 0.441511 0.747444 0.340305 11.00000 0.04279 0.07379 = 0.08837 0.06861 0.03004 0.03211 AFIX 13 H23 2 0.458954 0.701972 0.364470 11.00000 -1.20000 AFIX 0 C24 1 0.281280 0.707812 0.296507 11.00000 0.03940 0.08271 = 0.16845 0.09118 0.03432 0.02557 AFIX 137 H24A 2 0.261343 0.752570 0.273953 11.00000 -1.50000 H24B 2 0.222280 0.705945 0.342315 11.00000 -1.50000 H24C 2 0.257546 0.639526 0.245190 11.00000 -1.50000 AFIX 0 C25 1 0.480699 0.853778 0.420700 11.00000 0.07915 0.09937 = 0.07034 0.06102 0.03885 0.06023 AFIX 137 H25A 2 0.583879 0.878679 0.447455 11.00000 -1.50000 H25B 2 0.423522 0.852015 0.467337 11.00000 -1.50000 H25C 2 0.459845 0.898883 0.398904 11.00000 -1.50000 AFIX 0 C26 1 0.535811 0.542319 0.264192 11.00000 0.03115 0.03163 = 0.03896 0.02243 -0.00381 0.00453 C27 1 0.404475 0.492322 0.189703 11.00000 0.04561 0.04234 = 0.05344 0.03109 -0.01793 -0.00226 AFIX 137 H27A 2 0.401680 0.423776 0.147157 11.00000 -1.50000 H27B 2 0.408168 0.531464 0.156434 11.00000 -1.50000 H27C 2 0.317537 0.488970 0.216717 11.00000 -1.50000 AFIX 0 C28 1 0.550754 0.493379 0.322507 11.00000 0.03036 0.02578 = 0.03746 0.01941 -0.00064 0.00552 C29 1 0.447780 0.408372 0.318692 11.00000 0.03050 0.02835 = 0.04498 0.02036 -0.00167 0.00314 AFIX 43 H29 2 0.360289 0.375064 0.274467 11.00000 -1.20000 AFIX 0 C30 1 0.473765 0.373038 0.379455 11.00000 0.03265 0.02670 = 0.04812 0.02317 0.00594 0.00495 AFIX 43 H30 2 0.403568 0.316046 0.377630 11.00000 -1.20000 AFIX 0 C31 1 0.604145 0.421655 0.443789 11.00000 0.03377 0.02734 = 0.04039 0.02200 0.00944 0.01181 C32 1 0.699024 0.506140 0.442482 11.00000 0.03005 0.02751 = 0.03332 0.01937 0.00476 0.01001 C33 1 0.649258 0.394330 0.511132 11.00000 0.03942 0.03606 = 0.04672 0.03071 0.01290 0.01443 AFIX 43 H33 2 0.587393 0.337317 0.513925 11.00000 -1.20000 AFIX 0 C34 1 0.776962 0.447948 0.569881 11.00000 0.04476 0.03994 = 0.04316 0.03149 0.01239 0.01894 AFIX 43 H34 2 0.804902 0.427835 0.612866 11.00000 -1.20000 AFIX 0 C35 1 0.832495 0.562326 0.505686 11.00000 0.03304 0.02949 = 0.03240 0.02049 0.00418 0.01160 C36 1 1.001790 0.601541 0.619377 11.00000 0.04075 0.04323 = 0.03588 0.02077 -0.00252 0.01389 AFIX 43 H36 2 1.057261 0.602482 0.668649 11.00000 -1.20000 AFIX 0 C37 1 1.037585 0.668006 0.584720 11.00000 0.03371 0.03668 = 0.03925 0.01789 -0.00166 0.00746 AFIX 43 H37 2 1.124508 0.723968 0.607161 11.00000 -1.20000 AFIX 0 PART 1 C38 1 0.919860 0.850580 0.387673 31.00000 0.03457 0.03145 = 0.03553 0.01650 0.00173 0.00236 AFIX 43 H38 2 0.820193 0.842930 0.387025 31.00000 -1.20000 AFIX 0 PART 0 C39 1 1.156238 0.945896 0.384443 11.00000 0.05330 0.04883 = 0.09917 0.04249 0.02702 0.01047 PART 1 AFIX 137 H39A 2 1.189150 0.912573 0.416016 31.00000 -1.50000 H39C 2 1.209216 1.018637 0.417417 31.00000 -1.50000 H39B 2 1.174139 0.917937 0.321668 31.00000 -1.50000 AFIX 137 PART 2 H39E 2 1.260358 0.972294 0.387352 -31.00000 -1.50000 H39D 2 1.109481 0.991753 0.379110 -31.00000 -1.50000 H39F 2 1.115098 0.878909 0.330937 -31.00000 -1.50000 AFIX 0 PART 1 C40 1 0.941161 0.996382 0.365431 31.00000 0.06523 0.04231 = 0.06820 0.03636 -0.00377 0.00803 AFIX 137 H40A 2 0.949429 0.988243 0.303816 31.00000 -1.50000 H40B 2 0.993779 1.066490 0.411104 31.00000 -1.50000 H40C 2 0.838981 0.979773 0.370350 31.00000 -1.50000 AFIX 0 PART 2 C38A 1 1.035949 0.846073 0.464096 -31.00000 0.04349 0.03785 = 0.05032 0.03262 0.01650 0.01298 AFIX 43 H38A 2 1.030009 0.831707 0.514286 -31.00000 -1.20000 AFIX 0 N5A 4 1.128658 0.936941 0.479534 -31.00000 0.04349 0.03785 = 0.05032 0.03262 0.01650 0.01298 C40A 1 1.203523 1.012971 0.571380 -31.00000 0.04349 0.03785 = 0.05032 0.03262 0.01650 0.01298 AFIX 137 H40D 2 1.303174 1.013144 0.580337 -31.00000 -1.50000 H40E 2 1.153798 0.997847 0.615984 -31.00000 -1.50000 H40F 2 1.204383 1.079498 0.580122 -31.00000 -1.50000 AFIX 0 HKLF 4 REM A in P-1 #2 REM wR2 = 0.0951, GooF = S = 1.069, Restrained GooF = 1.100 for all data REM R1 = 0.0335 for 7284 Fo > 4sig(Fo) and 0.0410 for all 8765 data REM 485 parameters refined using 7 restraints END WGHT 0.0480 0.3177 REM Highest difference peak 0.266, deepest hole -0.332, 1-sigma level 0.040 Q1 1 1.1266 0.9338 0.3395 11.00000 0.05 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0.0020 10 -5 7 -0.2028 -0.0450 10 -5 8 -0.1461 0.0978 10 -5 9 -0.2172 0.0569 10 -5 10 -0.2687 0.0559 10 -4 0 -0.0344 -0.1665 10 -4 1 -0.5949 -0.1498 10 -4 2 -0.6113 0.0435 10 -4 3 0.3171 -0.0473 10 -4 4 1.1719 0.0030 10 -4 5 0.7769 0.0802 10 -4 6 0.0523 -0.0118 10 -4 7 -0.0158 0.0946 10 -4 8 0.0264 0.0779 10 -4 9 -0.0512 -0.0781 10 -3 0 -0.8082 -0.1702 10 -3 1 -0.3763 0.1487 10 -3 2 0.6319 0.0253 10 -3 3 1.2027 -0.1068 10 -3 4 0.5152 0.0402 10 -3 5 -0.5326 -0.0640 10 -3 6 -0.7441 -0.0635 10 -3 7 -0.3955 0.0680 10 -3 8 -0.0782 -0.0700 10 -2 0 0.2074 0.1644 10 -2 1 0.9190 0.1203 10 -2 2 1.0079 -0.1413 10 -2 3 0.3595 0.0340 10 -2 4 -0.3620 0.0602 10 -2 5 -0.4353 -0.0421 10 -2 6 -0.1077 0.1194 10 -2 7 0.1240 0.0138 10 -2 8 0.0283 -0.1165 10 -1 0 0.8656 0.3037 10 -1 1 0.4428 -0.0414 10 -1 2 -0.2344 0.0159 10 -1 3 -0.5555 0.1681 10 -1 4 -0.2710 -0.0462 10 -1 5 0.1001 -0.0060 10 -1 6 0.1875 0.0280 10 -1 7 0.0318 -0.1051 10 0 0 -0.2188 -0.1103 10 0 1 -0.8393 -0.2565 10 0 2 -0.7157 0.0519 10 0 3 0.0457 -0.1095 10 0 4 0.5940 -0.1549 10 0 5 0.4743 0.0671 10 0 6 0.1272 -0.0090 10 1 0 -0.6660 -0.5388 10 1 1 -0.2447 0.0298 10 1 2 0.4242 -0.0081 10 1 3 0.6990 -0.1958 10 1 4 0.3480 0.0552 10 1 5 -0.0365 0.0264 10 2 0 -0.1766 0.5020 10 2 1 0.2977 0.3358 10 2 2 0.3485 -0.0781 10 2 3 0.1265 0.0736 10 2 4 -0.0556 0.1326 10 3 0 0.4329 0.1253 10 3 1 0.1588 -0.1872 10 3 2 -0.0284 -0.0899 10 3 3 -0.0099 0.0655 10 4 0 -0.2899 -0.0250 10 4 1 -0.2721 -0.0730 11 -13 2 -0.0277 -0.0585 11 -13 3 0.0558 -0.1700 11 -13 4 -0.0354 -0.0928 11 -12 0 -0.1200 -0.0455 11 -12 1 -0.1227 0.1141 11 -12 2 0.0068 -0.0536 11 -12 3 0.0576 -0.0088 11 -12 4 0.0379 -0.0031 11 -12 5 0.1741 -0.0728 11 -12 6 0.1269 0.1166 11 -11 0 -0.2043 0.2500 11 -11 1 -0.2011 -0.0435 11 -11 2 -0.0795 -0.0638 11 -11 3 0.0626 0.0782 11 -11 4 0.1462 -0.0634 11 -11 5 -0.0062 0.0231 11 -11 6 -0.2117 0.0873 11 -11 7 -0.0400 -0.1069 11 -10 0 -0.3863 -0.0368 11 -10 1 -0.2186 -0.0854 11 -10 2 0.0105 0.1505 11 -10 3 0.0770 0.0068 11 -10 4 -0.0923 -0.0637 11 -10 5 -0.1516 0.0906 11 -10 6 0.1835 -0.0590 11 -10 7 0.5991 -0.0587 11 -10 8 0.6713 0.0853 11 -9 0 0.2537 -0.2375 11 -9 1 0.3826 -0.0296 11 -9 2 0.3294 -0.0026 11 -9 3 0.0779 -0.1311 11 -9 4 -0.0327 0.0544 11 -9 5 0.2248 0.0102 11 -9 6 0.4753 -0.0829 11 -9 7 0.4093 0.0836 11 -9 8 0.0939 0.0060 11 -8 0 0.2765 -0.0379 11 -8 1 0.1967 0.2531 11 -8 2 -0.1064 0.0095 11 -8 3 -0.3373 0.0294 11 -8 4 -0.1550 0.0769 11 -8 5 0.1137 -0.0758 11 -8 6 0.1372 0.0206 11 -8 7 0.0000 -0.0046 11 -8 8 -0.0671 -0.1516 11 -7 0 0.1076 0.5065 11 -7 1 -0.0057 -0.0072 11 -7 2 -0.1259 -0.1289 11 -7 3 0.0228 0.0935 11 -7 4 0.1673 -0.0126 11 -7 5 0.0844 -0.0117 11 -7 6 -0.0398 0.0811 11 -7 7 -0.1268 -0.0489 11 -7 8 -0.0626 0.0440 11 -6 0 0.2314 -0.3384 11 -6 1 0.3467 -0.2771 11 -6 2 0.3490 0.0869 11 -6 3 0.1189 0.0071 11 -6 4 -0.1764 -0.1224 11 -6 5 -0.1622 0.0580 11 -6 6 -0.0800 -0.0180 11 -6 7 -0.0898 -0.0904 11 -5 0 0.1988 -0.0224 11 -5 1 -0.0259 0.1415 11 -5 2 -0.4147 0.0532 11 -5 3 -0.6083 -0.1483 11 -5 4 -0.2975 0.0312 11 -5 5 0.0100 0.0745 11 -5 6 -0.0868 -0.0894 11 -5 7 -0.1439 0.0987 11 -4 0 -0.2793 -0.0519 11 -4 1 -0.4614 0.0673 11 -4 2 -0.2936 -0.0572 11 -4 3 0.1536 -0.0141 11 -4 4 0.3879 0.1235 11 -4 5 0.1206 -0.0412 11 -4 6 -0.1719 0.0194 11 -3 0 -0.5371 0.1603 11 -3 1 -0.1452 0.0888 11 -3 2 0.1520 -0.1066 11 -3 3 0.1232 0.0348 11 -3 4 -0.1068 -0.0261 11 -3 5 -0.2316 -0.1173 11 -3 6 -0.1497 0.1003 11 -2 0 0.0921 0.1897 11 -2 1 0.2027 -0.1075 11 -2 2 -0.0284 -0.0016 11 -2 3 -0.1364 0.1215 11 -2 4 0.0359 -0.0448 11 -2 5 0.1782 0.0871 11 -1 0 0.2720 -0.1098 11 -1 1 -0.1690 -0.1129 11 -1 2 -0.3622 0.1472 11 -1 3 -0.1007 -0.0214 11 -1 4 0.1970 -0.0813 11 0 0 -0.3042 -0.2772 11 0 1 -0.3792 0.0283 11 0 2 -0.0457 -0.0384 11 0 3 0.3563 -0.2485 11 1 0 -0.2751 0.0116 12 -9 1 0.0537 0.0934 12 -8 0 -0.1252 0.2387 12 -8 1 -0.1410 0.0851 12 -8 2 -0.2247 0.0417 12 -8 3 -0.2558 0.1427 12 -7 0 -0.1659 0.0516 12 -7 1 -0.0226 -0.2114 12 -7 2 0.0256 0.0142 12 -7 3 0.1632 -0.0089 12 -6 0 0.4006 -0.3897 12 -6 1 0.5544 0.0168 12 -6 2 0.4952 0.1126 12 -6 3 0.2748 -0.1363 12 -5 0 0.3567 0.1440 12 -5 1 0.1522 0.1748 12 -5 2 -0.1215 -0.1358 12 -4 0 -0.0998 0.1079 12 -4 1 -0.1308 0.0002 12 -3 0 -0.0193 0.1068 0 0 0 0.0 0.0 ; _shelx_fab_checksum 11583 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.82162(3) 0.66294(2) 0.39350(2) 0.02977(8) Uani 1 1 d . . . . . Cl2 Cl 0.72163(4) 0.76926(3) 0.50863(3) 0.03725(10) Uani 1 1 d . . . . . Cl1 Cl 0.93384(4) 0.55274(3) 0.29228(2) 0.03473(9) Uani 1 1 d . . . . . O1 O 0.96423(12) 0.78548(8) 0.39404(8) 0.0378(2) Uani 1 1 d . . . . . N1 N 0.63810(13) 0.62412(9) 0.28323(9) 0.0305(3) Uani 1 1 d . . . . . N2 N 0.67270(13) 0.54091(9) 0.38451(8) 0.0282(3) Uani 1 1 d . . . . . N3 N 0.93151(13) 0.64354(9) 0.51303(9) 0.0321(3) Uani 1 1 d . . . . . N4 N 0.86867(14) 0.53284(10) 0.56817(9) 0.0315(3) Uani 1 1 d . . . . . N5 N 1.00256(16) 0.92893(11) 0.38182(11) 0.0393(4) Uani 0.942(3) 1 d D . P A 1 C26 C 0.52362(19) 0.81957(12) 0.02059(11) 0.0358(3) Uani 1 1 d . . . . . C31 C 0.4237(2) 0.72365(13) -0.01491(12) 0.0482(4) Uani 1 1 d . . . . . H2 H 0.406953 0.691464 0.022667 0.058 Uiso 1 1 calc R U . . . C30 C 0.3474(3) 0.67364(16) -0.10462(14) 0.0609(6) Uani 1 1 d . . . . . H3 H 0.279064 0.607790 -0.127752 0.073 Uiso 1 1 calc R U . . . C29 C 0.3699(3) 0.71853(18) -0.15994(13) 0.0626(6) Uani 1 1 d . . . . . H4 H 0.317749 0.684132 -0.221357 0.075 Uiso 1 1 calc R U . . . C28 C 0.4687(3) 0.8138(2) -0.12585(15) 0.0669(6) Uani 1 1 d . . . . . H5 H 0.484815 0.845362 -0.163955 0.080 Uiso 1 1 calc R U . . . C27 C 0.5450(2) 0.86428(17) -0.03638(14) 0.0534(5) Uani 1 1 d . . . . . H6 H 0.612697 0.930269 -0.013664 0.064 Uiso 1 1 calc R U . . . C25 C 0.60155(19) 0.88010(12) 0.12048(11) 0.0373(4) Uani 1 1 d . . . . . H7A H 0.702204 0.920153 0.122982 0.045 Uiso 0.33(2) 1 calc R U P B 1 H7B H 0.703194 0.916265 0.120673 0.045 Uiso 0.67(2) 1 calc R U P B 2 C32 C 0.5128(18) 0.9616(7) 0.1740(6) 0.051(2) Uani 0.33(2) 1 d G . P B 1 C33 C 0.3674(18) 0.9409(6) 0.1430(7) 0.051(2) Uani 0.33(2) 1 d G . P B 1 H13 H 0.318847 0.885046 0.084871 0.061 Uiso 0.33(2) 1 calc R U P B 1 C34 C 0.2930(18) 1.0019(7) 0.1970(8) 0.065(3) Uani 0.33(2) 1 d G . P B 1 H1 H 0.193563 0.987755 0.175784 0.078 Uiso 0.33(2) 1 calc R U P B 1 C35 C 0.364(2) 1.0836(8) 0.2820(7) 0.060(3) Uani 0.33(2) 1 d G . P B 1 H11 H 0.313141 1.125306 0.318871 0.072 Uiso 0.33(2) 1 calc R U P B 1 C36 C 0.509(2) 1.1043(7) 0.3130(5) 0.049(4) Uani 0.33(2) 1 d G . P B 1 H10 H 0.558003 1.160149 0.371046 0.059 Uiso 0.33(2) 1 calc R U P B 1 C37 C 0.5839(19) 1.0433(7) 0.2590(6) 0.051(2) Uani 0.33(2) 1 d G . P B 1 H9 H 0.683290 1.057441 0.280134 0.061 Uiso 0.33(2) 1 calc R U P B 1 C37A C 0.6308(8) 1.0420(4) 0.2562(3) 0.0528(12) Uani 0.67(2) 1 d G . P B 2 H9A H 0.731036 1.051737 0.268786 0.063 Uiso 0.67(2) 1 calc R U P B 2 C32A C 0.5419(6) 0.9579(3) 0.1778(2) 0.0341(9) Uani 0.67(2) 1 d G . P B 2 C13A C 0.3952(6) 0.9436(3) 0.1594(4) 0.0441(10) Uani 0.67(2) 1 d G . P B 2 H13A H 0.334469 0.886199 0.105784 0.053 Uiso 0.67(2) 1 calc R U P B 2 C34A C 0.3375(9) 1.0134(4) 0.2193(6) 0.0613(15) Uani 0.67(2) 1 d G . P B 2 H12A H 0.237235 1.003678 0.206678 0.074 Uiso 0.67(2) 1 calc R U P B 2 C35A C 0.4264(13) 1.0975(4) 0.2977(5) 0.065(2) Uani 0.67(2) 1 d G . P B 2 H11A H 0.386900 1.145188 0.338626 0.078 Uiso 0.67(2) 1 calc R U P B 2 C36A C 0.5730(12) 1.1118(3) 0.3161(3) 0.070(2) Uani 0.67(2) 1 d G . P B 2 H10A H 0.633801 1.169219 0.369682 0.084 Uiso 0.67(2) 1 calc R U P B 2 C16 C 0.61095(17) 0.81296(11) 0.16443(11) 0.0347(3) Uani 1 1 d . . . . . C17 C 0.69936(18) 0.75334(12) 0.13786(11) 0.0369(3) Uani 1 1 d . . . . . H15 H 0.756001 0.756671 0.093592 0.044 Uiso 1 1 calc R U . . . C18 C 0.70784(17) 0.68876(12) 0.17392(10) 0.0343(3) Uani 1 1 d . . . . . C13 C 0.62417(16) 0.68493(11) 0.23972(11) 0.0313(3) Uani 1 1 d . . . . . C14 C 0.53461(16) 0.74468(12) 0.26864(12) 0.0351(3) Uani 1 1 d . . . . . C15 C 0.53062(17) 0.80736(12) 0.22937(12) 0.0361(3) Uani 1 1 d . . . . . H19 H 0.469920 0.847919 0.248224 0.043 Uiso 1 1 calc R U . . . C22 C 0.8014(2) 0.62192(14) 0.13871(11) 0.0425(4) Uani 1 1 d . . . . . H20 H 0.802765 0.587877 0.177678 0.051 Uiso 1 1 calc R U . . . C24 C 0.9565(2) 0.68090(18) 0.14538(16) 0.0638(6) Uani 1 1 d . . . . . H21A H 0.958582 0.714981 0.107554 0.096 Uiso 1 1 calc R U . . . H21B H 1.012332 0.634502 0.123480 0.096 Uiso 1 1 calc R U . . . H21C H 0.998902 0.731356 0.209403 0.096 Uiso 1 1 calc R U . . . C23 C 0.7353(3) 0.53955(16) 0.04018(15) 0.0652(6) Uani 1 1 d . . . . . H22A H 0.634968 0.502339 0.036824 0.098 Uiso 1 1 calc R U . . . H22B H 0.791082 0.492924 0.020768 0.098 Uiso 1 1 calc R U . . . H22C H 0.737554 0.570522 -0.000293 0.098 Uiso 1 1 calc R U . . . C19 C 0.4415(2) 0.74744(17) 0.34030(16) 0.0528(5) Uani 1 1 d . . . . . H23 H 0.458954 0.701972 0.364470 0.063 Uiso 1 1 calc R U . . . C20 C 0.2813(2) 0.7078(2) 0.2965(2) 0.0825(9) Uani 1 1 d . . . . . H24A H 0.261343 0.752570 0.273953 0.124 Uiso 1 1 calc R U . . . H24B H 0.222280 0.705945 0.342315 0.124 Uiso 1 1 calc R U . . . H24C H 0.257546 0.639526 0.245190 0.124 Uiso 1 1 calc R U . . . C21 C 0.4807(3) 0.8538(2) 0.42070(16) 0.0667(6) Uani 1 1 d . . . . . H25A H 0.583879 0.878679 0.447455 0.100 Uiso 1 1 calc R U . . . H25B H 0.423522 0.852015 0.467337 0.100 Uiso 1 1 calc R U . . . H25C H 0.459845 0.898883 0.398904 0.100 Uiso 1 1 calc R U . . . C2 C 0.53581(16) 0.54232(12) 0.26419(11) 0.0334(3) Uani 1 1 d . . . . . C1 C 0.4045(2) 0.49232(14) 0.18970(13) 0.0487(5) Uani 1 1 d . . . . . H27A H 0.401680 0.423776 0.147157 0.073 Uiso 1 1 calc R U . . . H27B H 0.408168 0.531464 0.156434 0.073 Uiso 1 1 calc R U . . . H27C H 0.317537 0.488970 0.216717 0.073 Uiso 1 1 calc R U . . . C3 C 0.55075(16) 0.49338(11) 0.32251(11) 0.0306(3) Uani 1 1 d . . . . . C4 C 0.44778(17) 0.40837(11) 0.31869(11) 0.0352(3) Uani 1 1 d . . . . . H29 H 0.360289 0.375064 0.274467 0.042 Uiso 1 1 calc R U . . . C5 C 0.47377(17) 0.37304(11) 0.37946(11) 0.0348(3) Uani 1 1 d . . . . . H30 H 0.403568 0.316046 0.377630 0.042 Uiso 1 1 calc R U . . . C6 C 0.60415(16) 0.42166(11) 0.44379(11) 0.0310(3) Uani 1 1 d . . . . . C12 C 0.69902(15) 0.50614(11) 0.44248(10) 0.0282(3) Uani 1 1 d . . . . . C7 C 0.64926(18) 0.39433(12) 0.51113(11) 0.0357(3) Uani 1 1 d . . . . . H33 H 0.587393 0.337317 0.513925 0.043 Uiso 1 1 calc R U . . . C8 C 0.77696(18) 0.44795(12) 0.56988(11) 0.0367(3) Uani 1 1 d . . . . . H34 H 0.804902 0.427835 0.612866 0.044 Uiso 1 1 calc R U . . . C11 C 0.83250(16) 0.56233(11) 0.50569(10) 0.0291(3) Uani 1 1 d . . . . . C9 C 1.00179(18) 0.60154(13) 0.61938(11) 0.0395(4) Uani 1 1 d . . . . . H36 H 1.057261 0.602482 0.668649 0.047 Uiso 1 1 calc R U . . . C10 C 1.03758(18) 0.66801(13) 0.58472(11) 0.0378(3) Uani 1 1 d . . . . . H37 H 1.124508 0.723968 0.607161 0.045 Uiso 1 1 calc R U . . . C38 C 0.91986(18) 0.85058(12) 0.38767(11) 0.0357(4) Uani 0.942(3) 1 d . . P A 1 H38 H 0.820193 0.842930 0.387025 0.043 Uiso 0.942(3) 1 calc R U P A 1 C39 C 1.1562(2) 0.94590(17) 0.38444(19) 0.0651(6) Uani 1 1 d . U . . . H39A H 1.189150 0.912573 0.416016 0.098 Uiso 0.942(3) 1 calc R U P A 1 H39C H 1.209216 1.018637 0.417417 0.098 Uiso 0.942(3) 1 calc R U P A 1 H39B H 1.174139 0.917937 0.321668 0.098 Uiso 0.942(3) 1 calc R U P A 1 H39E H 1.260358 0.972294 0.387352 0.098 Uiso 0.058(3) 1 calc R U P A 2 H39D H 1.109481 0.991753 0.379110 0.098 Uiso 0.058(3) 1 calc R U P A 2 H39F H 1.115098 0.878909 0.330937 0.098 Uiso 0.058(3) 1 calc R U P A 2 C40 C 0.9412(3) 0.99638(16) 0.36543(17) 0.0574(6) Uani 0.942(3) 1 d D . P A 1 H40A H 0.949429 0.988243 0.303816 0.086 Uiso 0.942(3) 1 calc R U P A 1 H40B H 0.993779 1.066490 0.411104 0.086 Uiso 0.942(3) 1 calc R U P A 1 H12 H 0.838981 0.979773 0.370350 0.086 Uiso 0.942(3) 1 calc R U P A 1 C38A C 1.036(3) 0.846(2) 0.464(2) 0.039(4) Uani 0.058(3) 1 d . . P A 2 H38A H 1.030009 0.831707 0.514286 0.047 Uiso 0.058(3) 1 calc R U P A 2 N5A N 1.129(3) 0.9369(17) 0.4795(15) 0.039(4) Uani 0.058(3) 1 d D . P A 2 C40A C 1.204(3) 1.0130(19) 0.5714(16) 0.039(4) Uani 0.058(3) 1 d D . P A 2 H40D H 1.303174 1.013144 0.580337 0.059 Uiso 0.058(3) 1 calc R U P A 2 H40E H 1.153798 0.997847 0.615984 0.059 Uiso 0.058(3) 1 calc R U P A 2 H40F H 1.204383 1.079498 0.580122 0.059 Uiso 0.058(3) 1 calc R U P A 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 0.02802(14) 0.02567(14) 0.03717(15) 0.01974(11) 0.00207(10) 0.00332(10) Cl2 0.0378(2) 0.03169(19) 0.0476(2) 0.02326(16) 0.01278(16) 0.01059(15) Cl1 0.03621(19) 0.0385(2) 0.03534(19) 0.02256(16) 0.00194(14) 0.01275(15) O1 0.0350(6) 0.0298(5) 0.0491(7) 0.0230(5) 0.0082(5) 0.0038(5) N1 0.0297(6) 0.0299(6) 0.0361(7) 0.0221(5) -0.0021(5) 0.0059(5) N2 0.0282(6) 0.0256(6) 0.0347(6) 0.0196(5) 0.0009(5) 0.0061(5) N3 0.0321(6) 0.0297(6) 0.0357(7) 0.0186(5) 0.0012(5) 0.0072(5) N4 0.0356(7) 0.0349(7) 0.0329(6) 0.0224(6) 0.0044(5) 0.0138(5) N5 0.0405(8) 0.0307(7) 0.0483(9) 0.0246(7) 0.0064(6) 0.0041(6) C26 0.0489(9) 0.0358(8) 0.0352(8) 0.0235(7) 0.0088(7) 0.0202(7) C31 0.0714(12) 0.0343(9) 0.0392(9) 0.0198(7) -0.0028(8) 0.0154(8) C30 0.0837(15) 0.0426(11) 0.0458(11) 0.0136(9) -0.0106(10) 0.0218(10) C29 0.0867(16) 0.0727(15) 0.0320(9) 0.0185(9) 0.0029(9) 0.0436(13) C28 0.0889(17) 0.0923(18) 0.0453(11) 0.0488(12) 0.0174(11) 0.0386(14) C27 0.0671(12) 0.0594(12) 0.0496(11) 0.0403(10) 0.0130(9) 0.0190(10) C25 0.0464(9) 0.0313(8) 0.0394(8) 0.0251(7) 0.0013(7) 0.0069(7) C32 0.089(6) 0.036(2) 0.034(2) 0.0186(19) -0.002(3) 0.030(3) C33 0.089(6) 0.036(2) 0.034(2) 0.0186(19) -0.002(3) 0.030(3) C34 0.100(7) 0.053(5) 0.060(5) 0.029(4) 0.028(5) 0.046(5) C35 0.102(9) 0.032(4) 0.063(5) 0.032(4) 0.044(5) 0.025(5) C36 0.102(11) 0.023(4) 0.023(3) 0.012(3) 0.010(4) 0.021(4) C37 0.089(6) 0.036(2) 0.034(2) 0.0186(19) -0.002(3) 0.030(3) C37A 0.079(3) 0.0337(17) 0.0426(17) 0.0206(14) 0.0071(19) 0.0099(18) C32A 0.057(2) 0.0247(14) 0.0354(15) 0.0251(12) 0.0072(12) 0.0162(12) C13A 0.060(2) 0.0459(18) 0.040(2) 0.0257(16) 0.0105(15) 0.0291(15) C34A 0.081(3) 0.061(3) 0.075(4) 0.046(3) 0.034(3) 0.043(2) C35A 0.113(7) 0.040(3) 0.062(3) 0.031(2) 0.046(4) 0.036(3) C36A 0.107(5) 0.039(2) 0.050(2) 0.0200(18) 0.026(3) 0.006(3) C16 0.0399(8) 0.0289(7) 0.0372(8) 0.0223(7) -0.0033(6) 0.0044(6) C17 0.0441(9) 0.0373(8) 0.0337(8) 0.0225(7) 0.0030(6) 0.0109(7) C18 0.0388(8) 0.0335(8) 0.0312(8) 0.0188(6) -0.0032(6) 0.0085(6) C13 0.0287(7) 0.0300(7) 0.0376(8) 0.0236(6) -0.0060(6) 0.0021(6) C14 0.0269(7) 0.0399(8) 0.0486(9) 0.0329(8) 0.0016(6) 0.0060(6) C15 0.0333(8) 0.0352(8) 0.0475(9) 0.0282(7) 0.0001(6) 0.0085(6) C22 0.0585(11) 0.0479(10) 0.0342(8) 0.0259(8) 0.0065(7) 0.0258(8) C24 0.0550(12) 0.0692(14) 0.0640(13) 0.0240(11) 0.0080(10) 0.0289(11) C23 0.0846(16) 0.0454(11) 0.0566(12) 0.0151(10) 0.0021(11) 0.0255(11) C19 0.0428(10) 0.0738(13) 0.0884(15) 0.0686(13) 0.0300(10) 0.0321(10) C20 0.0394(11) 0.0827(17) 0.168(3) 0.091(2) 0.0343(14) 0.0256(11) C21 0.0792(15) 0.0994(18) 0.0703(14) 0.0610(14) 0.0389(12) 0.0602(14) C2 0.0311(7) 0.0316(8) 0.0390(8) 0.0224(7) -0.0038(6) 0.0045(6) C1 0.0456(10) 0.0423(10) 0.0534(11) 0.0311(9) -0.0179(8) -0.0023(8) C3 0.0304(7) 0.0258(7) 0.0375(8) 0.0194(6) -0.0006(6) 0.0055(6) C4 0.0305(8) 0.0284(8) 0.0450(9) 0.0204(7) -0.0017(6) 0.0031(6) C5 0.0326(8) 0.0267(7) 0.0481(9) 0.0232(7) 0.0059(6) 0.0049(6) C6 0.0338(7) 0.0273(7) 0.0404(8) 0.0220(6) 0.0094(6) 0.0118(6) C12 0.0301(7) 0.0275(7) 0.0333(7) 0.0194(6) 0.0048(6) 0.0100(6) C7 0.0394(8) 0.0361(8) 0.0467(9) 0.0307(7) 0.0129(7) 0.0144(7) C8 0.0448(9) 0.0399(9) 0.0432(9) 0.0315(7) 0.0124(7) 0.0189(7) C11 0.0330(7) 0.0295(7) 0.0324(7) 0.0205(6) 0.0042(6) 0.0116(6) C9 0.0407(9) 0.0432(9) 0.0359(8) 0.0208(7) -0.0025(7) 0.0139(7) C10 0.0337(8) 0.0367(8) 0.0393(8) 0.0179(7) -0.0017(6) 0.0075(7) C38 0.0346(9) 0.0315(8) 0.0355(9) 0.0165(7) 0.0017(7) 0.0024(7) C39 0.0533(10) 0.0488(10) 0.0992(14) 0.0425(10) 0.0270(10) 0.0105(8) C40 0.0652(14) 0.0423(11) 0.0682(14) 0.0364(10) -0.0038(11) 0.0080(10) C38A 0.043(9) 0.038(9) 0.050(9) 0.033(7) 0.017(7) 0.013(7) N5A 0.043(9) 0.038(9) 0.050(9) 0.033(7) 0.017(7) 0.013(7) C40A 0.043(9) 0.038(9) 0.050(9) 0.033(7) 0.017(7) 0.013(7) 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 Cl2 Ni1 Cl1 172.989(16) . . ? Cl2 Ni1 N3 85.50(3) . . ? Cl1 Ni1 N3 87.50(3) . . ? O1 Ni1 Cl2 90.41(4) . . ? O1 Ni1 Cl1 91.88(4) . . ? O1 Ni1 N1 100.85(5) . . ? O1 Ni1 N3 105.49(5) . . ? N1 Ni1 Cl2 91.57(4) . . ? N1 Ni1 Cl1 94.50(4) . . ? N1 Ni1 N3 153.50(5) . . ? N2 Ni1 Cl2 90.40(4) . . ? N2 Ni1 Cl1 87.80(4) . . ? N2 Ni1 O1 175.72(5) . . ? N2 Ni1 N1 74.92(5) . . ? N2 Ni1 N3 78.76(5) . . ? C38 O1 Ni1 119.78(11) . . ? C38A O1 Ni1 115.7(13) . . ? C13 N1 Ni1 126.25(9) . . ? C2 N1 Ni1 113.20(9) . . ? C2 N1 C13 120.42(12) . . ? C3 N2 Ni1 122.00(10) . . ? C3 N2 C12 119.75(12) . . ? C12 N2 Ni1 118.25(10) . . ? C11 N3 Ni1 100.47(9) . . ? C11 N3 C10 103.81(12) . . ? C10 N3 Ni1 155.72(11) . . ? C11 N4 C8 121.01(13) . . ? C11 N4 C9 105.76(12) . . ? C9 N4 C8 133.23(13) . . ? C38 N5 C39 120.55(16) . . ? C38 N5 C40 121.08(16) . . ? C39 N5 C40 118.21(16) . . ? C31 C26 C27 117.84(16) . . ? C31 C26 C25 122.70(14) . . ? C27 C26 C25 119.30(16) . . ? C26 C31 H2 119.5 . . ? C26 C31 C30 121.02(18) . . ? C30 C31 H2 119.5 . . ? C31 C30 H3 119.8 . . ? C29 C30 C31 120.5(2) . . ? C29 C30 H3 119.8 . . ? C30 C29 H4 120.3 . . ? C30 C29 C28 119.35(19) . . ? C28 C29 H4 120.3 . . ? C29 C28 H5 119.7 . . ? C29 C28 C27 120.55(19) . . ? C27 C28 H5 119.7 . . ? C26 C27 H6 119.6 . . ? C28 C27 C26 120.8(2) . . ? C28 C27 H6 119.6 . . ? C26 C25 H7A 108.2 . . ? C26 C25 H7B 106.6 . . ? C26 C25 C32 105.9(5) . . ? C26 C25 C16 112.75(13) . . ? C32 C25 H7A 108.2 . . ? C32A C25 C26 113.8(2) . . ? C32A C25 H7B 106.6 . . ? C32A C25 C16 110.1(2) . . ? C16 C25 H7A 108.2 . . ? C16 C25 H7B 106.6 . . ? C16 C25 C32 113.3(4) . . ? C33 C32 C25 122.1(6) . . ? C33 C32 C37 120.0 . . ? C37 C32 C25 117.1(6) . . ? C32 C33 H13 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H13 120.0 . . ? C33 C34 H1 120.0 . . ? C33 C34 C35 120.0 . . ? C35 C34 H1 120.0 . . ? C34 C35 H11 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H11 120.0 . . ? C35 C36 H10 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H10 120.0 . . ? C32 C37 H9 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H9 120.0 . . ? C32A C37A H9A 120.0 . . ? C32A C37A C36A 120.0 . . ? C36A C37A H9A 120.0 . . ? C37A C32A C25 119.1(3) . . ? C13A C32A C25 120.6(3) . . ? C13A C32A C37A 120.0 . . ? C32A C13A H13A 120.0 . . ? C32A C13A C34A 120.0 . . ? C34A C13A H13A 120.0 . . ? C13A C34A H12A 120.0 . . ? C35A C34A C13A 120.0 . . ? C35A C34A H12A 120.0 . . ? C34A C35A H11A 120.0 . . ? C34A C35A C36A 120.0 . . ? C36A C35A H11A 120.0 . . ? C37A C36A H10A 120.0 . . ? C35A C36A C37A 120.0 . . ? C35A C36A H10A 120.0 . . ? C17 C16 C25 120.29(15) . . ? C15 C16 C25 121.93(15) . . ? C15 C16 C17 117.76(14) . . ? C16 C17 H15 118.9 . . ? C16 C17 C18 122.25(16) . . ? C18 C17 H15 118.9 . . ? C17 C18 C13 118.34(15) . . ? C17 C18 C22 119.64(15) . . ? C13 C18 C22 121.97(13) . . ? C18 C13 N1 119.71(14) . . ? C14 C13 N1 119.24(14) . . ? C14 C13 C18 120.90(13) . . ? C13 C14 C19 125.14(13) . . ? C15 C14 C13 117.82(15) . . ? C15 C14 C19 117.04(15) . . ? C16 C15 C14 122.93(15) . . ? C16 C15 H19 118.5 . . ? C14 C15 H19 118.5 . . ? C18 C22 H20 107.6 . . ? C18 C22 C23 110.50(15) . . ? C24 C22 C18 112.93(15) . . ? C24 C22 H20 107.6 . . ? C24 C22 C23 110.36(18) . . ? C23 C22 H20 107.6 . . ? C22 C24 H21A 109.5 . . ? C22 C24 H21B 109.5 . . ? C22 C24 H21C 109.5 . . ? H21A C24 H21B 109.5 . . ? H21A C24 H21C 109.5 . . ? H21B C24 H21C 109.5 . . ? C22 C23 H22A 109.5 . . ? C22 C23 H22B 109.5 . . ? C22 C23 H22C 109.5 . . ? H22A C23 H22B 109.5 . . ? H22A C23 H22C 109.5 . . ? H22B C23 H22C 109.5 . . ? C14 C19 H23 108.2 . . ? C14 C19 C20 110.20(19) . . ? C14 C19 C21 111.61(16) . . ? C20 C19 H23 108.2 . . ? C21 C19 H23 108.2 . . ? C21 C19 C20 110.32(18) . . ? C19 C20 H24A 109.5 . . ? C19 C20 H24B 109.5 . . ? C19 C20 H24C 109.5 . . ? H24A C20 H24B 109.5 . . ? H24A C20 H24C 109.5 . . ? H24B C20 H24C 109.5 . . ? C19 C21 H25A 109.5 . . ? C19 C21 H25B 109.5 . . ? C19 C21 H25C 109.5 . . ? H25A C21 H25B 109.5 . . ? H25A C21 H25C 109.5 . . ? H25B C21 H25C 109.5 . . ? N1 C2 C1 126.16(14) . . ? N1 C2 C3 116.22(13) . . ? C3 C2 C1 117.61(13) . . ? C2 C1 H27A 109.5 . . ? C2 C1 H27B 109.5 . . ? C2 C1 H27C 109.5 . . ? H27A C1 H27B 109.5 . . ? H27A C1 H27C 109.5 . . ? H27B C1 H27C 109.5 . . ? N2 C3 C2 113.42(12) . . ? N2 C3 C4 120.50(13) . . ? C4 C3 C2 126.03(13) . . ? C3 C4 H29 120.0 . . ? C5 C4 C3 119.90(14) . . ? C5 C4 H29 120.0 . . ? C4 C5 H30 120.1 . . ? C4 C5 C6 119.81(14) . . ? C6 C5 H30 120.1 . . ? C5 C6 C7 127.05(14) . . ? C12 C6 C5 115.83(13) . . ? C12 C6 C7 117.11(14) . . ? N2 C12 C6 124.19(13) . . ? N2 C12 C11 115.13(13) . . ? C6 C12 C11 120.67(13) . . ? C6 C7 H33 119.3 . . ? C8 C7 C6 121.34(14) . . ? C8 C7 H33 119.3 . . ? N4 C8 H34 119.8 . . ? C7 C8 N4 120.46(13) . . ? C7 C8 H34 119.8 . . ? N3 C11 N4 113.22(13) . . ? N3 C11 C12 127.39(13) . . ? N4 C11 C12 119.39(13) . . ? N4 C9 H36 127.1 . . ? C10 C9 N4 105.85(13) . . ? C10 C9 H36 127.1 . . ? N3 C10 H37 124.3 . . ? C9 C10 N3 111.37(14) . . ? C9 C10 H37 124.3 . . ? O1 C38 N5 124.03(16) . . ? O1 C38 H38 118.0 . . ? N5 C38 H38 118.0 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39C 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39C C39 H39B 109.5 . . ? H39E C39 H39D 109.5 . . ? H39E C39 H39F 109.5 . . ? H39D C39 H39F 109.5 . . ? N5A C39 H39E 109.5 . . ? N5A C39 H39D 109.5 . . ? N5A C39 H39F 109.5 . . ? N5 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? N5 C40 H12 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H12 109.5 . . ? H40B C40 H12 109.5 . . ? O1 C38A H38A 117.9 . . ? O1 C38A N5A 124(2) . . ? N5A C38A H38A 117.9 . . ? C38A N5A C39 114.2(19) . . ? C38A N5A C40A 121(2) . . ? C40A N5A C39 125.0(18) . . ? N5A C40A H40D 109.5 . . ? N5A C40A H40E 109.5 . . ? N5A C40A H40F 109.5 . . ? H40D C40A H40E 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 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 Cl2 2.3734(5) . ? Ni1 Cl1 2.3776(5) . ? Ni1 O1 2.0300(11) . ? Ni1 N1 2.2470(12) . ? Ni1 N2 1.9945(12) . ? Ni1 N3 2.3786(12) . ? O1 C38 1.250(2) . ? O1 C38A 1.15(3) . ? N1 C13 1.4473(17) . ? N1 C2 1.283(2) . ? N2 C3 1.3265(18) . ? N2 C12 1.3371(18) . ? N3 C11 1.3186(19) . ? N3 C10 1.378(2) . ? N4 C8 1.394(2) . ? N4 C11 1.3695(18) . ? N4 C9 1.378(2) . ? N5 C38 1.314(2) . ? N5 C39 1.451(3) . ? N5 C40 1.457(2) . ? C26 C31 1.382(3) . ? C26 C27 1.390(2) . ? C26 C25 1.523(2) . ? C31 H2 0.9500 . ? C31 C30 1.388(3) . ? C30 H3 0.9500 . ? C30 C29 1.368(3) . ? C29 H4 0.9500 . ? C29 C28 1.373(3) . ? C28 H5 0.9500 . ? C28 C27 1.385(3) . ? C27 H6 0.9500 . ? C25 H7A 1.0000 . ? C25 H7B 1.0000 . ? C25 C32 1.687(12) . ? C25 C32A 1.465(5) . ? C25 C16 1.5316(19) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 H13 0.9500 . ? C33 C34 1.3900 . ? C34 H1 0.9500 . ? C34 C35 1.3900 . ? C35 H11 0.9500 . ? C35 C36 1.3900 . ? C36 H10 0.9500 . ? C36 C37 1.3900 . ? C37 H9 0.9500 . ? C37A H9A 0.9500 . ? C37A C32A 1.3900 . ? C37A C36A 1.3900 . ? C32A C13A 1.3900 . ? C13A H13A 0.9500 . ? C13A C34A 1.3900 . ? C34A H12A 0.9500 . ? C34A C35A 1.3900 . ? C35A H11A 0.9500 . ? C35A C36A 1.3900 . ? C36A H10A 0.9500 . ? C16 C17 1.389(2) . ? C16 C15 1.380(2) . ? C17 H15 0.9500 . ? C17 C18 1.394(2) . ? C18 C13 1.405(2) . ? C18 C22 1.519(2) . ? C13 C14 1.402(2) . ? C14 C15 1.397(2) . ? C14 C19 1.522(2) . ? C15 H19 0.9500 . ? C22 H20 1.0000 . ? C22 C24 1.516(3) . ? C22 C23 1.526(3) . ? C24 H21A 0.9800 . ? C24 H21B 0.9800 . ? C24 H21C 0.9800 . ? C23 H22A 0.9800 . ? C23 H22B 0.9800 . ? C23 H22C 0.9800 . ? C19 H23 1.0000 . ? C19 C20 1.529(3) . ? C19 C21 1.527(3) . ? C20 H24A 0.9800 . ? C20 H24B 0.9800 . ? C20 H24C 0.9800 . ? C21 H25A 0.9800 . ? C21 H25B 0.9800 . ? C21 H25C 0.9800 . ? C2 C1 1.496(2) . ? C2 C3 1.4921(19) . ? C1 H27A 0.9800 . ? C1 H27B 0.9800 . ? C1 H27C 0.9800 . ? C3 C4 1.402(2) . ? C4 H29 0.9500 . ? C4 C5 1.384(2) . ? C5 H30 0.9500 . ? C5 C6 1.404(2) . ? C6 C12 1.398(2) . ? C6 C7 1.445(2) . ? C12 C11 1.417(2) . ? C7 H33 0.9500 . ? C7 C8 1.344(2) . ? C8 H34 0.9500 . ? C9 H36 0.9500 . ? C9 C10 1.366(2) . ? C10 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39C 0.9800 . ? C39 H39B 0.9800 . ? C39 H39E 0.9800 . ? C39 H39D 0.9800 . ? C39 H39F 0.9800 . ? C39 N5A 1.67(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H12 0.9800 . ? C38A H38A 0.9500 . ? C38A N5A 1.36(4) . ? N5A C40A 1.445(19) . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 O1 C38 N5 -175.68(13) . . . . ? Ni1 O1 C38A N5A -174(2) . . . . ? Ni1 N1 C13 C18 75.60(17) . . . . ? Ni1 N1 C13 C14 -99.99(15) . . . . ? Ni1 N1 C2 C1 -175.24(15) . . . . ? Ni1 N1 C2 C3 4.81(18) . . . . ? Ni1 N2 C3 C2 -2.00(19) . . . . ? Ni1 N2 C3 C4 -179.38(12) . . . . ? Ni1 N2 C12 C6 179.89(11) . . . . ? Ni1 N2 C12 C11 0.66(18) . . . . ? Ni1 N3 C11 N4 179.88(10) . . . . ? Ni1 N3 C11 C12 -0.34(18) . . . . ? Ni1 N3 C10 C9 -180.0(2) . . . . ? O1 C38A N5A C39 -12(4) . . . . ? O1 C38A N5A C40A 173(3) . . . . ? N1 C13 C14 C15 176.02(13) . . . . ? N1 C13 C14 C19 -3.5(2) . . . . ? N1 C2 C3 N2 -2.3(2) . . . . ? N1 C2 C3 C4 174.92(16) . . . . ? N2 C3 C4 C5 -0.6(2) . . . . ? N2 C12 C11 N3 -0.1(2) . . . . ? N2 C12 C11 N4 179.64(13) . . . . ? N4 C9 C10 N3 -0.1(2) . . . . ? C26 C31 C30 C29 0.1(3) . . . . ? C26 C25 C32 C33 27.1(6) . . . . ? C26 C25 C32 C37 -163.0(5) . . . . ? C26 C25 C32A C37A -154.4(2) . . . . ? C26 C25 C32A C13A 31.8(3) . . . . ? C26 C25 C16 C17 69.9(2) . . . . ? C26 C25 C16 C15 -108.56(18) . . . . ? C31 C26 C27 C28 -0.3(3) . . . . ? C31 C26 C25 C32 -99.6(5) . . . . ? C31 C26 C25 C32A -101.4(3) . . . . ? C31 C26 C25 C16 24.9(2) . . . . ? C31 C30 C29 C28 -0.1(3) . . . . ? C30 C29 C28 C27 0.0(4) . . . . ? C29 C28 C27 C26 0.2(4) . . . . ? C27 C26 C31 C30 0.1(3) . . . . ? C27 C26 C25 C32 75.7(5) . . . . ? C27 C26 C25 C32A 73.9(3) . . . . ? C27 C26 C25 C16 -159.85(17) . . . . ? C25 C26 C31 C30 175.44(19) . . . . ? C25 C26 C27 C28 -175.8(2) . . . . ? C25 C32 C33 C34 169.5(8) . . . . ? C25 C32 C37 C36 -170.1(8) . . . . ? C25 C32A C13A C34A 173.7(3) . . . . ? C25 C16 C17 C18 -177.97(14) . . . . ? C25 C16 C15 C14 178.29(15) . . . . ? C32 C25 C16 C17 -169.9(6) . . . . ? C32 C25 C16 C15 11.7(6) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C32 C37 C36 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C32 0.0 . . . . ? C37 C32 C33 C34 0.0 . . . . ? C37A C32A C13A C34A 0.0 . . . . ? C32A C25 C16 C17 -161.9(2) . . . . ? C32A C25 C16 C15 19.7(3) . . . . ? C32A C37A C36A C35A 0.0 . . . . ? C32A C13A C34A C35A 0.0 . . . . ? C13A C34A C35A C36A 0.0 . . . . ? C34A C35A C36A C37A 0.0 . . . . ? C36A C37A C32A C25 -173.8(3) . . . . ? C36A C37A C32A C13A 0.0 . . . . ? C16 C25 C32 C33 -97.0(6) . . . . ? C16 C25 C32 C37 72.9(6) . . . . ? C16 C25 C32A C37A 78.0(3) . . . . ? C16 C25 C32A C13A -95.8(3) . . . . ? C16 C17 C18 C13 -0.4(2) . . . . ? C16 C17 C18 C22 177.17(15) . . . . ? C17 C16 C15 C14 -0.2(2) . . . . ? C17 C18 C13 N1 -175.67(13) . . . . ? C17 C18 C13 C14 -0.2(2) . . . . ? C17 C18 C22 C24 54.7(2) . . . . ? C17 C18 C22 C23 -69.4(2) . . . . ? C18 C13 C14 C15 0.5(2) . . . . ? C18 C13 C14 C19 -179.06(16) . . . . ? C13 N1 C2 C1 8.8(3) . . . . ? C13 N1 C2 C3 -171.15(14) . . . . ? C13 C18 C22 C24 -127.84(17) . . . . ? C13 C18 C22 C23 108.01(19) . . . . ? C13 C14 C15 C16 -0.3(2) . . . . ? C13 C14 C19 C20 -115.73(18) . . . . ? C13 C14 C19 C21 121.34(18) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C15 C14 C19 C20 64.7(2) . . . . ? C15 C14 C19 C21 -58.2(2) . . . . ? C22 C18 C13 N1 6.9(2) . . . . ? C22 C18 C13 C14 -177.62(15) . . . . ? C19 C14 C15 C16 179.26(16) . . . . ? C2 N1 C13 C18 -109.00(17) . . . . ? C2 N1 C13 C14 75.4(2) . . . . ? C2 C3 C4 C5 -177.61(16) . . . . ? C1 C2 C3 N2 177.75(15) . . . . ? C1 C2 C3 C4 -5.0(3) . . . . ? C3 N2 C12 C6 -1.0(2) . . . . ? C3 N2 C12 C11 179.81(14) . . . . ? C3 C4 C5 C6 -0.9(2) . . . . ? C4 C5 C6 C12 1.4(2) . . . . ? C4 C5 C6 C7 -179.29(16) . . . . ? C5 C6 C12 N2 -0.5(2) . . . . ? C5 C6 C12 C11 178.67(14) . . . . ? C5 C6 C7 C8 -179.29(16) . . . . ? C6 C12 C11 N3 -179.39(15) . . . . ? C6 C12 C11 N4 0.4(2) . . . . ? C6 C7 C8 N4 1.0(2) . . . . ? C12 N2 C3 C2 178.88(13) . . . . ? C12 N2 C3 C4 1.5(2) . . . . ? C12 C6 C7 C8 0.0(2) . . . . ? C7 C6 C12 N2 -179.89(14) . . . . ? C7 C6 C12 C11 -0.7(2) . . . . ? C8 N4 C11 N3 -179.54(13) . . . . ? C8 N4 C11 C12 0.7(2) . . . . ? C8 N4 C9 C10 179.61(16) . . . . ? C11 N3 C10 C9 0.19(19) . . . . ? C11 N4 C8 C7 -1.4(2) . . . . ? C11 N4 C9 C10 0.00(18) . . . . ? C9 N4 C8 C7 179.07(17) . . . . ? C9 N4 C11 N3 0.13(18) . . . . ? C9 N4 C11 C12 -179.67(14) . . . . ? C10 N3 C11 N4 -0.20(17) . . . . ? C10 N3 C11 C12 179.59(15) . . . . ? C39 N5 C38 O1 -1.3(3) . . . . ? C40 N5 C38 O1 173.85(18) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 424.4 84.2 '2 THF'