Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Franc Meyer' _publ_contact_author_address ; Institut fur Anorganische Chemie Georg August Universitat Gottingen Tammannstrase 4 D-37077 Gottingen Germany ; _publ_contact_author_email franc.meyer@chemie.uni-goettingen.de _publ_contact_author_fax 49(551)393063 _publ_contact_author_phone 49(551)393012 _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Targeted construction of azido-bridged Ni~4~ complexes with decisive effect of \m-1,3 azide torsion on the spin ground state ; loop_ _publ_author_name _publ_author_address S.Demeshko ; Institut fur Anorganische Chemie Georg August Universitat Gottingen Tammannstrase 4 D-37077 Gottingen Germany ; G.Leibeling ; Institut fur Anorganische Chemie Georg August Universitat Gottingen Tammannstrase 4 D-37077 Gottingen Germany ; S.Dechert ; Institut fur Anorganische Chemie Georg August Universitat Gottingen Tammannstrase 4 D-37077 Gottingen Germany ; F.Meyer ; Institut fur Anorganische Chemie Georg August Universitat Gottingen Tammannstrase 4 D-37077 Gottingen Germany ; #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 292198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H35 N11 Ni2 O6, C4 H10 O' _chemical_formula_sum 'C21 H45 N11 Ni2 O7' _chemical_formula_weight 681.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1582(4) _cell_length_b 16.9656(11) _cell_length_c 22.3370(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.861(4) _cell_angle_gamma 90.00 _cell_volume 3062.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 20094 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 24.74 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6608 _exptl_absorpt_correction_T_max 0.7540 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20094 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.74 _reflns_number_total 5203 _reflns_number_gt 4306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+1.0866P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5203 _refine_ls_number_parameters 372 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.72153(4) 0.235280(19) 0.270660(14) 0.02327(10) Uani 1 1 d . . . Ni2 Ni 0.80425(4) 0.343309(18) 0.413293(14) 0.02173(10) Uani 1 1 d . . . O1 O 0.7584(2) 0.27421(11) 0.18510(8) 0.0322(4) Uani 1 1 d . . . O2 O 0.9795(2) 0.26148(13) 0.24856(9) 0.0388(5) Uani 1 1 d . . . O3 O 0.9950(3) 0.30800(15) 0.15861(9) 0.0496(6) Uani 1 1 d . . . O4 O 0.5394(2) 0.38844(11) 0.40893(9) 0.0331(4) Uani 1 1 d . . . O5 O 0.7575(2) 0.46050(10) 0.42963(8) 0.0277(4) Uani 1 1 d . . . O6 O 0.5140(3) 0.51352(12) 0.42882(9) 0.0378(5) Uani 1 1 d . . . N1 N 0.7502(3) 0.19026(13) 0.35097(9) 0.0269(5) Uani 1 1 d . . . N2 N 0.7836(3) 0.23008(12) 0.40364(9) 0.0255(5) Uani 1 1 d . . . N3 N 0.7318(3) 0.10623(13) 0.25316(10) 0.0320(5) Uani 1 1 d . . . N4 N 0.4659(3) 0.24311(14) 0.24961(10) 0.0310(5) Uani 1 1 d . . . N5 N 0.8123(3) 0.30029(13) 0.50849(9) 0.0294(5) Uani 1 1 d . . . N6 N 1.0596(3) 0.36045(13) 0.42081(10) 0.0269(5) Uani 1 1 d . . . N7 N 0.7554(3) 0.34705(13) 0.31596(9) 0.0273(5) Uani 1 1 d . . . N8 N 0.7612(3) 0.40520(13) 0.28553(10) 0.0301(5) Uani 1 1 d . . . N9 N 0.7682(4) 0.45977(15) 0.25498(12) 0.0464(7) Uani 1 1 d . . . N10 N 0.9131(3) 0.28231(14) 0.19619(10) 0.0329(5) Uani 1 1 d . . . N11 N 0.5993(3) 0.45576(13) 0.42253(9) 0.0264(5) Uani 1 1 d . . . C1 C 0.7760(4) 0.10229(17) 0.42586(12) 0.0356(7) Uani 1 1 d . . . H1 H 0.7791 0.0550 0.4471 0.080 Uiso 1 1 calc R . . C2 C 0.7459(4) 0.11359(16) 0.36334(12) 0.0306(6) Uani 1 1 d . . . C3 C 0.8003(3) 0.17832(16) 0.44895(11) 0.0280(6) Uani 1 1 d . . . C4 C 0.6985(4) 0.06224(16) 0.30843(12) 0.0383(7) Uani 1 1 d . . . H4A H 0.7625 0.0139 0.3124 0.080 Uiso 1 1 calc R . . H4B H 0.5822 0.0486 0.3050 0.080 Uiso 1 1 calc R . . C5 C 0.9026(4) 0.08715(18) 0.24271(14) 0.0423(8) Uani 1 1 d . . . H5A H 0.9117 0.0315 0.2363 0.080 Uiso 1 1 calc R . . H5B H 0.9788 0.1026 0.2773 0.080 Uiso 1 1 calc R . . H5C H 0.9280 0.1150 0.2077 0.080 Uiso 1 1 calc R . . C6 C 0.6159(4) 0.08136(18) 0.19906(13) 0.0389(7) Uani 1 1 d . . . H6A H 0.6174 0.0243 0.1965 0.080 Uiso 1 1 calc R . . H6B H 0.6559 0.1019 0.1632 0.080 Uiso 1 1 calc R . . C7 C 0.4378(4) 0.10828(18) 0.19889(14) 0.0415(7) Uani 1 1 d . . . H7A H 0.3701 0.0828 0.1653 0.080 Uiso 1 1 calc R . . H7B H 0.4003 0.0894 0.2357 0.080 Uiso 1 1 calc R . . C8 C 0.4056(4) 0.19642(18) 0.19426(13) 0.0369(7) Uani 1 1 d . . . H8A H 0.4576 0.2169 0.1610 0.080 Uiso 1 1 calc R . . H8B H 0.2873 0.2047 0.1844 0.080 Uiso 1 1 calc R . . C9 C 0.4190(4) 0.32647(18) 0.23608(15) 0.0433(8) Uani 1 1 d . . . H9A H 0.4809 0.3464 0.2058 0.080 Uiso 1 1 calc R . . H9B H 0.4428 0.3574 0.2722 0.080 Uiso 1 1 calc R . . H9C H 0.3028 0.3294 0.2215 0.080 Uiso 1 1 calc R . . C10 C 0.3832(4) 0.2172(2) 0.30126(14) 0.0441(8) Uani 1 1 d . . . H10A H 0.2655 0.2220 0.2908 0.080 Uiso 1 1 calc R . . H10B H 0.4193 0.2497 0.3358 0.080 Uiso 1 1 calc R . . H10C H 0.4111 0.1633 0.3107 0.080 Uiso 1 1 calc R . . C11 C 0.8524(4) 0.21364(16) 0.51035(12) 0.0334(7) Uani 1 1 d . . . H11A H 0.9704 0.2062 0.5220 0.080 Uiso 1 1 calc R . . H11B H 0.7948 0.1876 0.5400 0.080 Uiso 1 1 calc R . . C12 C 0.6459(4) 0.31013(19) 0.52631(13) 0.0391(7) Uani 1 1 d . . . H12A H 0.6457 0.2906 0.5666 0.080 Uiso 1 1 calc R . . H12B H 0.5669 0.2812 0.4990 0.080 Uiso 1 1 calc R . . H12C H 0.6168 0.3650 0.5249 0.080 Uiso 1 1 calc R . . C13 C 0.9324(4) 0.34500(17) 0.55206(12) 0.0366(7) Uani 1 1 d . . . H13A H 0.9369 0.3206 0.5915 0.080 Uiso 1 1 calc R . . H13B H 0.8908 0.3982 0.5552 0.080 Uiso 1 1 calc R . . C14 C 1.1063(4) 0.34973(17) 0.53613(13) 0.0378(7) Uani 1 1 d . . . H14A H 1.1452 0.2965 0.5310 0.080 Uiso 1 1 calc R . . H14B H 1.1768 0.3727 0.5702 0.080 Uiso 1 1 calc R . . C15 C 1.1287(3) 0.39662(16) 0.47999(12) 0.0319(6) Uani 1 1 d . . . H15A H 1.0776 0.4478 0.4829 0.080 Uiso 1 1 calc R . . H15B H 1.2462 0.4053 0.4799 0.080 Uiso 1 1 calc R . . C16 C 1.0951(4) 0.41674(18) 0.37326(13) 0.0358(7) Uani 1 1 d . . . H16A H 1.2102 0.4306 0.3797 0.080 Uiso 1 1 calc R . . H16B H 1.0292 0.4633 0.3751 0.080 Uiso 1 1 calc R . . H16C H 1.0687 0.3926 0.3343 0.080 Uiso 1 1 calc R . . C17 C 1.1473(4) 0.28597(18) 0.41158(14) 0.0369(7) Uani 1 1 d . . . H17A H 1.2638 0.2961 0.4140 0.080 Uiso 1 1 calc R . . H17B H 1.1067 0.2648 0.3725 0.080 Uiso 1 1 calc R . . H17C H 1.1283 0.2488 0.4423 0.080 Uiso 1 1 calc R . . O7A O 0.7293(6) 0.5565(3) 0.01649(19) 0.0528(18) Uiso 0.563(11) 1 d PD A 1 C18A C 0.8448(10) 0.4855(4) 0.1010(4) 0.0483(19) Uiso 0.563(11) 1 d PD A 1 H18A H 0.8543 0.4792 0.1440 0.080 Uiso 0.563(11) 1 calc PR A 1 H18B H 0.9525 0.4941 0.0895 0.080 Uiso 0.563(11) 1 calc PR A 1 H18C H 0.7972 0.4388 0.0815 0.080 Uiso 0.563(11) 1 calc PR A 1 C19A C 0.7413(14) 0.5514(7) 0.0830(4) 0.080(3) Uiso 0.563(11) 1 d PD A 1 H19A H 0.7890 0.5993 0.1016 0.080 Uiso 0.563(11) 1 calc PR A 1 H19B H 0.6325 0.5440 0.0950 0.080 Uiso 0.563(11) 1 calc PR A 1 C20A C 0.611(2) 0.6102(13) -0.0088(7) 0.156(9) Uiso 0.563(11) 1 d PD A 1 H20A H 0.6338 0.6611 0.0104 0.080 Uiso 0.563(11) 1 calc PR A 1 H20B H 0.5031 0.5931 -0.0004 0.080 Uiso 0.563(11) 1 calc PR A 1 C21A C 0.6066(11) 0.6191(5) -0.0737(3) 0.0430(19) Uiso 0.563(11) 1 d PD A 1 H21A H 0.5122 0.6502 -0.0895 0.080 Uiso 0.563(11) 1 calc PR A 1 H21B H 0.5990 0.5681 -0.0925 0.080 Uiso 0.563(11) 1 calc PR A 1 H21C H 0.7058 0.6450 -0.0820 0.080 Uiso 0.563(11) 1 calc PR A 1 O7B O 0.7804(11) 0.6003(7) 0.0186(4) 0.092(3) Uiso 0.437(11) 1 d PD A 2 C18B C 0.822(4) 0.4899(11) 0.0842(12) 0.197(13) Uiso 0.437(11) 1 d PD A 2 H18D H 0.8257 0.4710 0.1249 0.080 Uiso 0.437(11) 1 calc PR A 2 H18E H 0.9264 0.4809 0.0704 0.080 Uiso 0.437(11) 1 calc PR A 2 H18F H 0.7364 0.4625 0.0584 0.080 Uiso 0.437(11) 1 calc PR A 2 C19B C 0.7871(19) 0.5710(8) 0.0825(5) 0.076(4) Uiso 0.437(11) 1 d PD A 2 H19C H 0.8725 0.5990 0.1087 0.080 Uiso 0.437(11) 1 calc PR A 2 H19D H 0.6819 0.5806 0.0969 0.080 Uiso 0.437(11) 1 calc PR A 2 C20B C 0.6184(10) 0.6092(5) -0.0092(3) 0.032(2) Uiso 0.437(11) 1 d PD A 2 H20C H 0.5652 0.6544 0.0064 0.080 Uiso 0.437(11) 1 calc PR A 2 H20D H 0.5529 0.5623 -0.0048 0.080 Uiso 0.437(11) 1 calc PR A 2 C21B C 0.646(3) 0.6214(16) -0.0729(7) 0.146(10) Uiso 0.437(11) 1 d PD A 2 H21D H 0.5425 0.6319 -0.0974 0.080 Uiso 0.437(11) 1 calc PR A 2 H21E H 0.6949 0.5748 -0.0875 0.080 Uiso 0.437(11) 1 calc PR A 2 H21F H 0.7194 0.6653 -0.0751 0.080 Uiso 0.437(11) 1 calc PR 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 0.02527(18) 0.02637(18) 0.01754(17) -0.00299(13) 0.00064(13) 0.00010(13) Ni2 0.02454(18) 0.02231(17) 0.01797(16) -0.00254(12) 0.00154(13) -0.00219(13) O1 0.0321(11) 0.0423(11) 0.0211(9) -0.0011(8) 0.0002(8) -0.0024(9) O2 0.0324(11) 0.0582(13) 0.0243(10) 0.0003(9) -0.0011(8) 0.0055(10) O3 0.0454(13) 0.0742(16) 0.0313(11) 0.0016(11) 0.0123(10) -0.0125(12) O4 0.0286(10) 0.0347(11) 0.0355(11) -0.0059(8) 0.0024(8) -0.0059(8) O5 0.0252(10) 0.0287(10) 0.0283(9) -0.0047(8) 0.0002(8) -0.0012(8) O6 0.0422(12) 0.0390(12) 0.0316(10) 0.0017(9) 0.0033(9) 0.0175(10) N1 0.0355(13) 0.0249(11) 0.0196(10) -0.0057(9) 0.0011(9) -0.0036(9) N2 0.0344(12) 0.0246(11) 0.0170(10) -0.0030(9) 0.0016(9) -0.0026(9) N3 0.0440(14) 0.0294(12) 0.0216(11) -0.0072(9) 0.0007(10) 0.0016(10) N4 0.0267(12) 0.0385(13) 0.0276(12) -0.0090(10) 0.0027(10) -0.0007(10) N5 0.0430(14) 0.0256(12) 0.0198(11) -0.0038(9) 0.0050(10) -0.0025(10) N6 0.0258(11) 0.0312(12) 0.0231(11) -0.0030(9) 0.0010(9) -0.0009(9) N7 0.0340(13) 0.0273(12) 0.0200(11) -0.0017(10) 0.0016(9) -0.0028(9) N8 0.0317(13) 0.0314(14) 0.0259(11) -0.0056(11) -0.0001(10) 0.0017(10) N9 0.0654(19) 0.0319(14) 0.0409(15) 0.0101(12) 0.0037(13) -0.0014(13) N10 0.0339(14) 0.0420(14) 0.0231(12) -0.0022(10) 0.0054(11) 0.0018(11) N11 0.0286(12) 0.0325(13) 0.0176(10) 0.0011(9) 0.0008(9) 0.0043(10) C1 0.0562(19) 0.0254(14) 0.0253(14) -0.0007(11) 0.0057(13) -0.0028(13) C2 0.0428(16) 0.0240(14) 0.0250(14) -0.0040(11) 0.0045(12) -0.0018(12) C3 0.0367(15) 0.0273(14) 0.0206(13) -0.0007(10) 0.0056(11) -0.0016(11) C4 0.061(2) 0.0255(14) 0.0270(15) -0.0032(12) 0.0021(14) -0.0028(13) C5 0.0500(19) 0.0400(17) 0.0361(16) -0.0068(13) 0.0036(14) 0.0166(14) C6 0.0558(19) 0.0345(15) 0.0237(14) -0.0108(12) -0.0041(13) -0.0011(14) C7 0.0469(18) 0.0422(17) 0.0327(16) -0.0112(13) -0.0039(14) -0.0109(14) C8 0.0316(15) 0.0458(17) 0.0312(15) -0.0103(13) -0.0033(12) -0.0036(13) C9 0.0320(16) 0.0436(18) 0.0511(19) -0.0135(15) -0.0053(14) 0.0071(13) C10 0.0309(16) 0.066(2) 0.0367(16) -0.0119(15) 0.0094(13) -0.0056(15) C11 0.0546(18) 0.0255(14) 0.0194(13) -0.0008(10) 0.0032(12) -0.0027(12) C12 0.0516(19) 0.0398(16) 0.0288(15) -0.0010(13) 0.0163(14) -0.0032(14) C13 0.060(2) 0.0318(15) 0.0172(12) -0.0060(11) 0.0003(13) -0.0042(14) C14 0.0482(18) 0.0359(16) 0.0248(14) -0.0051(12) -0.0114(13) -0.0034(13) C15 0.0306(15) 0.0331(15) 0.0296(14) -0.0048(12) -0.0045(12) -0.0037(12) C16 0.0284(15) 0.0472(17) 0.0316(15) 0.0028(13) 0.0029(12) -0.0078(13) C17 0.0289(15) 0.0424(17) 0.0387(16) -0.0114(13) 0.0016(13) 0.0071(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 1.934(2) . ? Ni1 N4 2.079(2) . ? Ni1 O1 2.0824(19) . ? Ni1 N7 2.149(2) . ? Ni1 N3 2.228(2) . ? Ni1 O2 2.270(2) . ? Ni2 N2 1.938(2) . ? Ni2 O5 2.0664(18) . ? Ni2 N6 2.087(2) . ? Ni2 N7 2.157(2) . ? Ni2 N5 2.241(2) . ? Ni2 O4 2.2821(19) . ? Ni1 Ni2 3.6575(5) . ? O1 N10 1.259(3) . ? O2 N10 1.270(3) . ? O3 N10 1.223(3) . ? O4 N11 1.263(3) . ? O5 N11 1.281(3) . ? O6 N11 1.221(3) . ? N1 C2 1.331(3) . ? N1 N2 1.352(3) . ? N2 C3 1.333(3) . ? N3 C5 1.480(4) . ? N3 C6 1.490(3) . ? N3 C4 1.499(4) . ? N4 C10 1.480(4) . ? N4 C9 1.485(4) . ? N4 C8 1.494(3) . ? N5 C12 1.475(4) . ? N5 C13 1.490(3) . ? N5 C11 1.505(3) . ? N6 C17 1.480(4) . ? N6 C16 1.486(4) . ? N6 C15 1.496(3) . ? N7 N8 1.203(3) . ? N8 N9 1.156(3) . ? C1 C3 1.393(4) . ? C1 C2 1.398(4) . ? C2 C4 1.511(4) . ? C3 C11 1.504(4) . ? C6 C7 1.522(4) . ? C7 C8 1.519(4) . ? C13 C14 1.511(5) . ? C14 C15 1.517(4) . ? O7A C20A 1.390(13) . ? O7A C19A 1.478(9) . ? C18A C19A 1.425(10) . ? C20A C21A 1.454(13) . ? O7B C20B 1.390(10) . ? O7B C19B 1.505(11) . ? C18B C19B 1.403(15) . ? C20B C21B 1.486(14) . ? 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 N1 Ni1 N4 103.03(10) . . ? N1 Ni1 O1 164.16(9) . . ? N4 Ni1 O1 92.22(8) . . ? N1 Ni1 N7 85.43(9) . . ? N4 Ni1 N7 96.34(9) . . ? O1 Ni1 N7 97.29(8) . . ? N1 Ni1 N3 76.82(8) . . ? N4 Ni1 N3 94.81(9) . . ? O1 Ni1 N3 97.88(8) . . ? N7 Ni1 N3 160.77(8) . . ? N1 Ni1 O2 106.31(8) . . ? N4 Ni1 O2 150.41(9) . . ? O1 Ni1 O2 58.91(7) . . ? N7 Ni1 O2 82.32(8) . . ? N3 Ni1 O2 95.51(9) . . ? N2 Ni2 O5 163.35(9) . . ? N2 Ni2 N6 102.58(9) . . ? O5 Ni2 N6 93.34(8) . . ? N2 Ni2 N7 85.16(9) . . ? O5 Ni2 N7 97.85(8) . . ? N6 Ni2 N7 97.00(9) . . ? N2 Ni2 N5 76.91(8) . . ? O5 Ni2 N5 97.35(8) . . ? N6 Ni2 N5 93.99(9) . . ? N7 Ni2 N5 160.65(8) . . ? N2 Ni2 O4 105.08(8) . . ? O5 Ni2 O4 59.20(7) . . ? N6 Ni2 O4 152.32(8) . . ? N7 Ni2 O4 84.47(8) . . ? N5 Ni2 O4 93.13(8) . . ? N10 O1 Ni1 96.94(14) . . ? N10 O2 Ni1 87.89(15) . . ? N11 O4 Ni2 87.71(14) . . ? N11 O5 Ni2 97.19(14) . . ? C2 N1 N2 108.4(2) . . ? C2 N1 Ni1 125.11(17) . . ? N2 N1 Ni1 126.47(17) . . ? C3 N2 N1 108.6(2) . . ? C3 N2 Ni2 124.77(17) . . ? N1 N2 Ni2 126.61(17) . . ? C5 N3 C6 108.5(2) . . ? C5 N3 C4 107.5(2) . . ? C6 N3 C4 111.1(2) . . ? C5 N3 Ni1 107.55(18) . . ? C6 N3 Ni1 112.69(17) . . ? C4 N3 Ni1 109.24(16) . . ? C10 N4 C9 108.0(2) . . ? C10 N4 C8 110.7(2) . . ? C9 N4 C8 106.9(2) . . ? C10 N4 Ni1 110.79(18) . . ? C9 N4 Ni1 109.24(18) . . ? C8 N4 Ni1 111.09(17) . . ? C12 N5 C13 108.2(2) . . ? C12 N5 C11 107.9(2) . . ? C13 N5 C11 111.0(2) . . ? C12 N5 Ni2 108.09(17) . . ? C13 N5 Ni2 112.67(17) . . ? C11 N5 Ni2 108.80(15) . . ? C17 N6 C16 107.7(2) . . ? C17 N6 C15 110.0(2) . . ? C16 N6 C15 106.3(2) . . ? C17 N6 Ni2 111.46(17) . . ? C16 N6 Ni2 108.78(16) . . ? C15 N6 Ni2 112.32(17) . . ? N8 N7 Ni1 118.04(17) . . ? N8 N7 Ni2 125.28(17) . . ? Ni1 N7 Ni2 116.28(10) . . ? N9 N8 N7 178.0(3) . . ? O3 N10 O1 122.0(2) . . ? O3 N10 O2 121.8(2) . . ? O1 N10 O2 116.1(2) . . ? O6 N11 O4 123.1(2) . . ? O6 N11 O5 121.0(2) . . ? O4 N11 O5 115.9(2) . . ? C3 C1 C2 103.9(2) . . ? N1 C2 C1 109.6(2) . . ? N1 C2 C4 113.9(2) . . ? C1 C2 C4 136.3(3) . . ? N2 C3 C1 109.5(2) . . ? N2 C3 C11 114.6(2) . . ? C1 C3 C11 135.6(2) . . ? N3 C4 C2 109.1(2) . . ? N3 C6 C7 114.6(2) . . ? C8 C7 C6 116.8(3) . . ? N4 C8 C7 115.6(2) . . ? C3 C11 N5 109.3(2) . . ? N5 C13 C14 115.3(2) . . ? C13 C14 C15 116.5(2) . . ? N6 C15 C14 116.2(2) . . ? C20A O7A C19A 113.2(8) . . ? C18A C19A O7A 106.5(7) . . ? O7A C20A C21A 113.2(12) . . ? C20B O7B C19B 111.7(8) . . ? C18B C19B O7B 109.2(12) . . ? O7B C20B C21B 100.5(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.667 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.056 data_4a _database_code_depnum_ccdc_archive 'CCDC 292199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H70 N24 Ni4 2+, 2(Cl O4 -), 2(C H4 O), 0.5(H2 O)' _chemical_formula_sum 'C36 H79 Cl2 N24 Ni4 O10.50' _chemical_formula_weight 1321.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.537(2) _cell_length_b 16.1276(11) _cell_length_c 15.2760(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.342(6) _cell_angle_gamma 90.00 _cell_volume 6291.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 28794 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 24.66 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2772 _exptl_absorpt_coefficient_mu 1.330 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7047 _exptl_absorpt_correction_T_max 0.7740 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28794 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.66 _reflns_number_total 5305 _reflns_number_gt 3780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1152P)^2^+16.5722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5305 _refine_ls_number_parameters 363 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2027 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.35300(3) 0.65738(5) 0.43561(6) 0.0346(3) Uani 1 1 d . . . Ni2 Ni 0.22745(3) 0.61853(5) 0.33224(6) 0.0325(3) Uani 1 1 d . . . Cl1 Cl 0.11473(9) 0.26041(13) 0.45411(15) 0.0577(6) Uani 1 1 d . . . N1 N 0.3282(2) 0.5515(3) 0.3935(4) 0.0327(13) Uani 1 1 d . . . N2 N 0.2810(2) 0.5369(3) 0.3552(4) 0.0375(14) Uani 1 1 d . . . N3 N 0.3967(2) 0.5754(3) 0.5184(4) 0.0433(15) Uani 1 1 d . . . N4 N 0.4129(2) 0.6887(4) 0.3531(5) 0.0470(16) Uani 1 1 d . . . N5 N 0.1810(2) 0.5087(3) 0.3437(4) 0.0357(13) Uani 1 1 d . . . N6 N 0.2228(3) 0.6301(3) 0.1993(4) 0.0420(15) Uani 1 1 d . . . N7 N 0.2840(2) 0.7052(3) 0.3779(4) 0.0366(14) Uani 1 1 d . . . N8 N 0.2727(2) 0.7785(4) 0.3882(4) 0.0415(15) Uani 1 1 d . . . N9 N 0.2621(3) 0.8471(4) 0.3966(5) 0.0557(19) Uani 1 1 d . . . N10 N 0.3660(2) 0.7573(4) 0.5113(4) 0.0426(15) Uani 1 1 d . . . N11 N 0.3484(2) 0.7803(3) 0.5790(4) 0.0351(14) Uani 1 1 d . . . N12 N 0.3338(2) 0.8042(4) 0.6469(4) 0.0411(14) Uani 1 1 d . . . O1 O 0.1682(2) 0.2801(4) 0.4678(4) 0.0621(16) Uani 1 1 d . . . O2 O 0.1110(3) 0.1854(4) 0.4044(5) 0.089(2) Uani 1 1 d . . . O3 O 0.0899(3) 0.3232(5) 0.4071(7) 0.114(3) Uani 1 1 d . . . O4 O 0.0907(3) 0.2429(7) 0.5350(6) 0.122(4) Uani 1 1 d . . . C1 C 0.3085(3) 0.4181(4) 0.4162(5) 0.0428(18) Uani 1 1 d . . . H1 H 0.3106 0.3632 0.4345 0.080 Uiso 1 1 calc R . . C2 C 0.3442(3) 0.4806(4) 0.4307(5) 0.0437(18) Uani 1 1 d . . . C3 C 0.2686(3) 0.4555(4) 0.3682(5) 0.0365(16) Uani 1 1 d . . . C4 C 0.3959(3) 0.4897(4) 0.4799(6) 0.052(2) Uani 1 1 d . . . H4A H 0.3985 0.4485 0.5259 0.080 Uiso 1 1 calc R . . H4B H 0.4250 0.4824 0.4403 0.080 Uiso 1 1 calc R . . C5 C 0.3680(3) 0.5728(5) 0.6017(6) 0.056(2) Uani 1 1 d . . . H5A H 0.3831 0.5310 0.6389 0.080 Uiso 1 1 calc R . . H5B H 0.3319 0.5598 0.5904 0.080 Uiso 1 1 calc R . . H5C H 0.3704 0.6258 0.6300 0.080 Uiso 1 1 calc R . . C6 C 0.4517(3) 0.6041(5) 0.5334(6) 0.054(2) Uani 1 1 d . . . H6A H 0.4704 0.5613 0.5655 0.080 Uiso 1 1 calc R . . H6B H 0.4509 0.6532 0.5700 0.080 Uiso 1 1 calc R . . C7 C 0.4820(3) 0.6239(5) 0.4523(7) 0.063(3) Uani 1 1 d . . . H7A H 0.4806 0.5761 0.4138 0.080 Uiso 1 1 calc R . . H7B H 0.5183 0.6323 0.4687 0.080 Uiso 1 1 calc R . . C8 C 0.4634(3) 0.6993(5) 0.4012(6) 0.053(2) Uani 1 1 d . . . H8A H 0.4598 0.7453 0.4417 0.080 Uiso 1 1 calc R . . H8B H 0.4902 0.7142 0.3594 0.080 Uiso 1 1 calc R . . C9 C 0.4186(4) 0.6249(6) 0.2838(6) 0.065(3) Uani 1 1 d . . . H9A H 0.3875 0.6237 0.2481 0.080 Uiso 1 1 calc R . . H9B H 0.4238 0.5715 0.3104 0.080 Uiso 1 1 calc R . . H9C H 0.4483 0.6381 0.2481 0.080 Uiso 1 1 calc R . . C10 C 0.3997(4) 0.7686(5) 0.3115(6) 0.059(2) Uani 1 1 d . . . H10A H 0.4262 0.7828 0.2699 0.080 Uiso 1 1 calc R . . H10B H 0.3977 0.8110 0.3554 0.080 Uiso 1 1 calc R . . H10C H 0.3665 0.7641 0.2820 0.080 Uiso 1 1 calc R . . C11 C 0.2152(3) 0.4340(4) 0.3327(5) 0.0392(17) Uani 1 1 d . . . H11A H 0.2174 0.4192 0.2713 0.080 Uiso 1 1 calc R . . H11B H 0.2007 0.3873 0.3644 0.080 Uiso 1 1 calc R . . C12 C 0.1609(3) 0.5104(4) 0.4343(5) 0.0442(18) Uani 1 1 d . . . H12A H 0.1388 0.4632 0.4438 0.080 Uiso 1 1 calc R . . H12B H 0.1411 0.5603 0.4432 0.080 Uiso 1 1 calc R . . H12C H 0.1898 0.5089 0.4748 0.080 Uiso 1 1 calc R . . C13 C 0.1353(3) 0.5047(4) 0.2806(5) 0.0417(17) Uani 1 1 d . . . H13A H 0.1196 0.4500 0.2842 0.080 Uiso 1 1 calc R . . H13B H 0.1091 0.5447 0.2987 0.080 Uiso 1 1 calc R . . C14 C 0.1495(3) 0.5217(4) 0.1865(5) 0.0463(19) Uani 1 1 d . . . H14A H 0.1190 0.5104 0.1503 0.080 Uiso 1 1 calc R . . H14B H 0.1766 0.4828 0.1696 0.080 Uiso 1 1 calc R . . C15 C 0.1686(3) 0.6087(5) 0.1656(5) 0.0467(19) Uani 1 1 d . . . H15A H 0.1682 0.6157 0.1025 0.080 Uiso 1 1 calc R . . H15B H 0.1439 0.6482 0.1898 0.080 Uiso 1 1 calc R . . C16 C 0.2614(3) 0.5797(5) 0.1534(6) 0.055(2) Uani 1 1 d . . . H16A H 0.2582 0.5888 0.0915 0.080 Uiso 1 1 calc R . . H16B H 0.2556 0.5222 0.1661 0.080 Uiso 1 1 calc R . . H16C H 0.2960 0.5952 0.1725 0.080 Uiso 1 1 calc R . . C17 C 0.2327(4) 0.7193(4) 0.1770(6) 0.052(2) Uani 1 1 d . . . H17A H 0.2678 0.7339 0.1939 0.080 Uiso 1 1 calc R . . H17B H 0.2083 0.7538 0.2078 0.080 Uiso 1 1 calc R . . H17C H 0.2284 0.7273 0.1151 0.080 Uiso 1 1 calc R . . C18A C 0.4447(9) 0.6381(15) 0.7912(18) 0.030(6) Uiso 0.25 1 d PD A -1 H18A H 0.4534 0.6544 0.8500 0.080 Uiso 0.25 1 calc PR A -1 H18B H 0.4090 0.6197 0.7889 0.080 Uiso 0.25 1 calc PR A -1 H18C H 0.4491 0.6846 0.7527 0.080 Uiso 0.25 1 calc PR A -1 O5A O 0.4804(8) 0.5684(12) 0.7631(15) 0.047(5) Uiso 0.25 1 d PD A -1 H5D H 0.5110 0.5828 0.7691 0.080 Uiso 0.25 1 calc PR A -1 C18B C 0.4303(11) 0.6706(17) 0.7849(19) 0.036(6) Uiso 0.25 1 d PD B -2 H18D H 0.4530 0.7086 0.8150 0.080 Uiso 0.25 1 calc PR B -2 H18E H 0.3970 0.6688 0.8137 0.080 Uiso 0.25 1 calc PR B -2 H18F H 0.4254 0.6886 0.7255 0.080 Uiso 0.25 1 calc PR B -2 O5B O 0.4542(18) 0.586(2) 0.786(4) 0.145(16) Uiso 0.25 1 d PD B -2 H5E H 0.4585 0.5706 0.7351 0.080 Uiso 0.25 1 calc PR B -2 O6A O 0.4691(12) 0.823(2) 0.756(2) 0.096(10) Uiso 0.25 1 d PD C -3 H6C H 0.4907 0.8213 0.7165 0.080 Uiso 0.25 1 calc PR C -3 C19A C 0.496(4) 0.852(6) 0.839(4) 0.21(2) Uiso 0.25 1 d PD C -3 H19A H 0.5040 0.9093 0.8347 0.080 Uiso 0.25 1 calc PR C -3 H19B H 0.5270 0.8201 0.8483 0.080 Uiso 0.25 1 calc PR C -3 H19C H 0.4723 0.8431 0.8876 0.080 Uiso 0.25 1 calc PR C -3 O6B O 0.494(2) 0.901(4) 0.915(3) 0.21(3) Uiso 0.25 1 d PD D -4 H6D H 0.5071 0.8711 0.9526 0.080 Uiso 0.25 1 calc PR D -4 C19B C 0.4951(18) 0.857(3) 0.828(3) 0.21(2) Uiso 0.25 1 d PD D -4 H19D H 0.5287 0.8638 0.8014 0.080 Uiso 0.25 1 calc PR D -4 H19E H 0.4684 0.8791 0.7907 0.080 Uiso 0.25 1 calc PR D -4 H19F H 0.4886 0.7987 0.8374 0.080 Uiso 0.25 1 calc PR D -4 O7 O 0.5018(18) 1.068(3) 0.697(3) 0.17(2) Uiso 0.25 1 d PRD D -5 H7C H 0.5100 1.0644 0.6433 0.080 Uiso 0.25 1 d PRD D -5 H7D H 0.5031 1.0178 0.7033 0.080 Uiso 0.25 1 d PRD D -5 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 0.0404(5) 0.0196(4) 0.0439(6) -0.0009(4) 0.0020(4) 0.0020(3) Ni2 0.0444(5) 0.0190(4) 0.0340(5) 0.0011(3) 0.0003(4) 0.0032(4) Cl1 0.0703(14) 0.0453(11) 0.0573(14) 0.0035(9) -0.0075(11) -0.0157(10) N1 0.030(3) 0.019(3) 0.049(4) 0.001(2) 0.000(3) 0.004(2) N2 0.047(3) 0.020(3) 0.046(4) 0.002(2) 0.003(3) 0.001(2) N3 0.040(3) 0.027(3) 0.063(4) 0.005(3) -0.007(3) 0.003(2) N4 0.048(4) 0.037(3) 0.057(4) -0.004(3) 0.006(3) 0.001(3) N5 0.048(3) 0.020(3) 0.039(3) 0.000(2) -0.004(3) 0.003(2) N6 0.069(4) 0.021(3) 0.036(3) 0.004(2) 0.004(3) 0.003(3) N7 0.048(3) 0.016(3) 0.046(4) -0.001(2) 0.001(3) 0.003(2) N8 0.049(4) 0.031(4) 0.044(4) 0.006(3) 0.001(3) 0.000(3) N9 0.064(4) 0.020(3) 0.083(5) -0.006(3) -0.004(4) 0.008(3) N10 0.052(4) 0.026(3) 0.050(4) -0.004(3) 0.006(3) 0.005(3) N11 0.037(3) 0.017(3) 0.052(4) 0.001(3) -0.004(3) 0.002(2) N12 0.046(3) 0.033(3) 0.044(4) -0.004(3) 0.000(3) 0.007(3) O1 0.062(4) 0.053(4) 0.071(4) 0.002(3) -0.008(3) -0.012(3) O2 0.137(7) 0.046(4) 0.084(5) -0.010(3) -0.012(5) -0.030(4) O3 0.101(6) 0.054(4) 0.188(10) 0.010(5) -0.062(6) 0.004(4) O4 0.085(6) 0.190(11) 0.091(6) -0.041(7) 0.038(5) -0.034(6) C1 0.050(4) 0.020(3) 0.058(5) -0.003(3) -0.006(4) 0.004(3) C2 0.050(4) 0.021(3) 0.060(5) 0.000(3) -0.004(4) 0.006(3) C3 0.043(4) 0.023(3) 0.044(4) -0.005(3) 0.002(3) 0.001(3) C4 0.050(5) 0.027(4) 0.077(6) 0.003(4) -0.010(4) 0.006(3) C5 0.062(5) 0.038(4) 0.067(6) 0.010(4) -0.013(4) -0.004(4) C6 0.039(4) 0.044(5) 0.079(6) 0.002(4) -0.021(4) -0.005(3) C7 0.041(4) 0.040(4) 0.107(8) -0.004(5) -0.007(5) -0.003(4) C8 0.043(4) 0.047(5) 0.069(6) -0.007(4) 0.005(4) 0.000(4) C9 0.064(6) 0.070(6) 0.060(6) -0.021(5) 0.016(5) -0.007(5) C10 0.073(6) 0.050(5) 0.055(6) 0.019(4) 0.011(4) -0.007(4) C11 0.055(4) 0.012(3) 0.051(5) -0.001(3) 0.001(3) -0.004(3) C12 0.055(5) 0.029(4) 0.049(5) 0.002(3) -0.002(4) -0.004(3) C13 0.043(4) 0.030(4) 0.051(5) 0.002(3) -0.005(3) 0.000(3) C14 0.059(5) 0.036(4) 0.044(5) 0.001(3) -0.007(4) 0.000(3) C15 0.064(5) 0.037(4) 0.039(4) 0.001(3) -0.008(4) 0.005(4) C16 0.074(6) 0.044(5) 0.046(5) 0.003(4) 0.008(4) 0.014(4) C17 0.082(6) 0.025(4) 0.049(5) 0.013(3) 0.003(4) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 1.931(5) . ? Ni1 N10 2.009(6) . ? Ni1 N4 2.050(7) . ? Ni1 N7 2.111(6) . ? Ni1 N3 2.138(6) . ? Ni2 N2 1.929(6) . ? Ni2 N12 2.027(6) 7_566 ? Ni2 N6 2.042(6) . ? Ni2 N7 2.125(6) . ? Ni2 N5 2.140(6) . ? Ni1 Ni2 3.620(1) . ? Ni1 Ni1 6.371(2) 7_566 ? Ni1 Ni2 5.472(1) 7_566 ? Ni2 Ni2 6.746(2) 7_566 ? Cl1 O3 1.393(8) . ? Cl1 O4 1.412(9) . ? Cl1 O1 1.416(6) . ? Cl1 O2 1.432(7) . ? N1 C2 1.339(9) . ? N1 N2 1.357(8) . ? N2 C3 1.366(9) . ? N3 C5 1.471(11) . ? N3 C6 1.496(9) . ? N3 C4 1.502(10) . ? N4 C10 1.476(10) . ? N4 C9 1.485(11) . ? N4 C8 1.491(10) . ? N5 C12 1.479(10) . ? N5 C11 1.497(8) . ? N5 C13 1.511(9) . ? N6 C16 1.460(10) . ? N6 C17 1.501(8) . ? N6 C15 1.513(10) . ? N7 N8 1.227(8) . ? N8 N9 1.146(8) . ? N10 N11 1.190(9) . ? N11 N12 1.169(9) . ? N12 Ni2 2.027(6) 7_566 ? C1 C2 1.376(10) . ? C1 C3 1.388(10) . ? C2 C4 1.522(11) . ? C3 C11 1.507(10) . ? C6 C7 1.498(14) . ? C7 C8 1.520(12) . ? C13 C14 1.510(11) . ? C14 C15 1.520(10) . ? C18A O5A 1.511(10) . ? C18B O5B 1.489(10) . ? O6A C19A 1.505(10) . ? O6B C19B 1.502(10) . ? 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 N1 Ni1 N10 162.5(3) . . ? N1 Ni1 N4 104.9(3) . . ? N10 Ni1 N4 92.0(3) . . ? N1 Ni1 N7 85.0(2) . . ? N10 Ni1 N7 94.7(2) . . ? N4 Ni1 N7 106.1(2) . . ? N1 Ni1 N3 79.6(2) . . ? N10 Ni1 N3 94.1(2) . . ? N4 Ni1 N3 97.3(3) . . ? N7 Ni1 N3 154.6(2) . . ? N2 Ni2 N12 159.7(3) . 7_566 ? N2 Ni2 N6 106.3(3) . . ? N12 Ni2 N6 93.4(3) 7_566 . ? N2 Ni2 N7 84.8(2) . . ? N12 Ni2 N7 93.9(2) 7_566 . ? N6 Ni2 N7 107.6(2) . . ? N2 Ni2 N5 79.2(2) . . ? N12 Ni2 N5 93.9(2) 7_566 . ? N6 Ni2 N5 97.4(2) . . ? N7 Ni2 N5 153.3(2) . . ? O3 Cl1 O4 113.4(7) . . ? O3 Cl1 O1 110.4(5) . . ? O4 Cl1 O1 109.8(5) . . ? O3 Cl1 O2 108.2(5) . . ? O4 Cl1 O2 105.5(6) . . ? O1 Cl1 O2 109.3(5) . . ? C2 N1 N2 107.7(5) . . ? C2 N1 Ni1 121.0(5) . . ? N2 N1 Ni1 125.8(4) . . ? N1 N2 C3 108.0(5) . . ? N1 N2 Ni2 126.0(4) . . ? C3 N2 Ni2 121.2(5) . . ? C5 N3 C6 110.4(7) . . ? C5 N3 C4 107.8(6) . . ? C6 N3 C4 110.7(6) . . ? C5 N3 Ni1 105.6(5) . . ? C6 N3 Ni1 112.7(5) . . ? C4 N3 Ni1 109.3(5) . . ? C10 N4 C9 108.8(7) . . ? C10 N4 C8 107.8(6) . . ? C9 N4 C8 110.0(6) . . ? C10 N4 Ni1 108.1(5) . . ? C9 N4 Ni1 110.2(5) . . ? C8 N4 Ni1 111.8(5) . . ? C12 N5 C11 109.1(5) . . ? C12 N5 C13 109.1(6) . . ? C11 N5 C13 110.0(5) . . ? C12 N5 Ni2 104.9(4) . . ? C11 N5 Ni2 109.5(4) . . ? C13 N5 Ni2 114.2(4) . . ? C16 N6 C17 108.0(6) . . ? C16 N6 C15 109.3(6) . . ? C17 N6 C15 107.2(6) . . ? C16 N6 Ni2 113.0(5) . . ? C17 N6 Ni2 107.7(5) . . ? C15 N6 Ni2 111.4(5) . . ? N8 N7 Ni1 119.6(5) . . ? N8 N7 Ni2 121.1(5) . . ? Ni1 N7 Ni2 117.5(2) . . ? N9 N8 N7 179.1(8) . . ? N11 N10 Ni1 133.5(5) . . ? N12 N11 N10 176.4(7) . . ? N11 N12 Ni2 126.3(5) . 7_566 ? C2 C1 C3 104.5(6) . . ? N1 C2 C1 110.9(6) . . ? N1 C2 C4 112.8(6) . . ? C1 C2 C4 136.3(7) . . ? N2 C3 C1 108.9(6) . . ? N2 C3 C11 112.2(6) . . ? C1 C3 C11 138.6(6) . . ? N3 C4 C2 107.0(6) . . ? N3 C6 C7 115.4(7) . . ? C6 C7 C8 115.7(7) . . ? N4 C8 C7 115.3(7) . . ? N5 C11 C3 107.6(5) . . ? C14 C13 N5 114.3(6) . . ? C13 C14 C15 116.6(6) . . ? N6 C15 C14 115.6(6) . . ? 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 N10 N12 Ni2 -93.0(5) . . . 7_566 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.66 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.053 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.120 data_4b _database_code_depnum_ccdc_archive 'CCDC 292200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H70 N24 Ni4 2+, 2 (Cl O4 -), C3 H6 O, C5 H12' _chemical_formula_sum 'C42 H88 Cl2 N24 Ni4 O9' _chemical_formula_weight 1379.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.875(2) _cell_length_b 15.8835(8) _cell_length_c 15.2957(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.575(6) _cell_angle_gamma 90.00 _cell_volume 6283.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 17877 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 24.75 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6827 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17877 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 24.75 _reflns_number_total 5085 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+8.7725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5085 _refine_ls_number_parameters 399 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.23070(2) 0.61816(3) 0.66721(3) 0.02736(14) Uani 1 1 d . . . Ni2 Ni 0.35391(2) 0.65911(3) 0.56992(3) 0.02989(14) Uani 1 1 d . . . Cl1A Cl 0.38458(8) 0.24184(14) 0.45942(11) 0.0368(5) Uani 0.760(6) 1 d PD A 1 O1A O 0.33246(19) 0.2160(3) 0.4797(3) 0.0456(13) Uani 0.760(6) 1 d PD A 1 O2A O 0.4091(4) 0.1778(6) 0.4096(7) 0.071(2) Uani 0.760(6) 1 d PD A 1 O3A O 0.3820(2) 0.3187(3) 0.4104(3) 0.0617(15) Uani 0.760(6) 1 d PD A 1 O4A O 0.4122(3) 0.2575(4) 0.5403(3) 0.0766(18) Uani 0.760(6) 1 d PD A 1 Cl1B Cl 0.4037(3) 0.2084(5) 0.4782(5) 0.052(2) Uani 0.240(6) 1 d PD A 2 O1B O 0.3487(6) 0.2144(13) 0.4539(11) 0.0456(13) Uani 0.240(6) 1 d PD A 2 O2B O 0.4311(11) 0.1854(19) 0.4009(14) 0.079(11) Uani 0.240(6) 1 d PD A 2 O3B O 0.4113(6) 0.1483(10) 0.5449(10) 0.072(5) Uani 0.240(6) 1 d PD A 2 O4B O 0.4205(10) 0.2870(11) 0.5081(13) 0.0766(18) Uani 0.240(6) 1 d PD A 2 N1 N 0.28425(13) 0.53562(19) 0.6473(2) 0.0318(8) Uani 1 1 d . . . N2 N 0.33059(13) 0.55114(19) 0.6132(2) 0.0344(8) Uani 1 1 d . . . N3 N 0.18544(13) 0.50595(18) 0.6538(2) 0.0313(8) Uani 1 1 d . . . N4 N 0.22665(14) 0.62832(19) 0.8005(2) 0.0344(8) Uani 1 1 d . . . N5 N 0.40002(14) 0.57432(19) 0.4933(2) 0.0387(8) Uani 1 1 d . . . N6 N 0.41172(15) 0.6984(2) 0.6546(2) 0.0427(9) Uani 1 1 d . . . N7 N 0.28486(13) 0.70743(18) 0.6220(2) 0.0321(8) Uani 1 1 d . . . N8 N 0.27232(14) 0.78043(19) 0.6093(2) 0.0338(8) Uani 1 1 d . . . N9 N 0.25983(16) 0.8489(2) 0.5973(3) 0.0482(10) Uani 1 1 d . . . N10 N 0.16960(14) 0.6970(2) 0.6458(2) 0.0370(8) Uani 1 1 d . . . N11 N 0.15355(12) 0.72003(18) 0.5771(2) 0.0275(7) Uani 1 1 d . . . N12 N 0.13489(14) 0.7423(2) 0.5109(2) 0.0391(9) Uani 1 1 d . . . O5 O 0.5000 0.5461(4) 0.2500 0.103(2) Uani 1 2 d S . . C1 C 0.31269(17) 0.4146(2) 0.5925(3) 0.0378(10) Uani 1 1 d . . . H1 H 0.3151 0.3582 0.5766 0.080 Uiso 1 1 calc R . . C2 C 0.27248(16) 0.4539(2) 0.6350(3) 0.0324(9) Uani 1 1 d . . . C3 C 0.34880(17) 0.4787(2) 0.5791(3) 0.0391(10) Uani 1 1 d . . . C4 C 0.21994(15) 0.4302(2) 0.6652(3) 0.0322(9) Uani 1 1 d . . . H4A H 0.2218 0.4134 0.7262 0.080 Uiso 1 1 calc R . . H4B H 0.2063 0.3834 0.6309 0.080 Uiso 1 1 calc R . . C5 C 0.16633(18) 0.5080(2) 0.5611(3) 0.0393(10) Uani 1 1 d . . . H5A H 0.1952 0.5104 0.5231 0.080 Uiso 1 1 calc R . . H5B H 0.1450 0.5567 0.5518 0.080 Uiso 1 1 calc R . . H5C H 0.1465 0.4581 0.5487 0.080 Uiso 1 1 calc R . . C6 C 0.14087(17) 0.5025(3) 0.7125(3) 0.0377(10) Uani 1 1 d . . . H6A H 0.1248 0.4476 0.7071 0.080 Uiso 1 1 calc R . . H6B H 0.1156 0.5442 0.6933 0.080 Uiso 1 1 calc R . . C7 C 0.15487(19) 0.5183(2) 0.8087(3) 0.0414(10) Uani 1 1 d . . . H7A H 0.1814 0.4784 0.8268 0.080 Uiso 1 1 calc R . . H7B H 0.1246 0.5071 0.8429 0.080 Uiso 1 1 calc R . . C8 C 0.17415(19) 0.6070(2) 0.8304(3) 0.0409(10) Uani 1 1 d . . . H8A H 0.1499 0.6471 0.8047 0.080 Uiso 1 1 calc R . . H8B H 0.1737 0.6143 0.8934 0.080 Uiso 1 1 calc R . . C9 C 0.2659(2) 0.5763(3) 0.8467(3) 0.0460(12) Uani 1 1 d . . . H9A H 0.2601 0.5181 0.8330 0.080 Uiso 1 1 calc R . . H9B H 0.2635 0.5847 0.9086 0.080 Uiso 1 1 calc R . . H9C H 0.2997 0.5924 0.8284 0.080 Uiso 1 1 calc R . . C10 C 0.2375(2) 0.7178(2) 0.8241(3) 0.0480(12) Uani 1 1 d . . . H10A H 0.2125 0.7536 0.7952 0.080 Uiso 1 1 calc R . . H10B H 0.2716 0.7327 0.8060 0.080 Uiso 1 1 calc R . . H10C H 0.2355 0.7247 0.8863 0.080 Uiso 1 1 calc R . . C11 C 0.39941(18) 0.4888(2) 0.5359(3) 0.0462(12) Uani 1 1 d . . . H11A H 0.4036 0.4452 0.4923 0.080 Uiso 1 1 calc R . . H11B H 0.4275 0.4843 0.5789 0.080 Uiso 1 1 calc R . . C12 C 0.3732(2) 0.5678(3) 0.4080(3) 0.0484(12) Uani 1 1 d . . . H12A H 0.3385 0.5482 0.4158 0.080 Uiso 1 1 calc R . . H12B H 0.3912 0.5288 0.3718 0.080 Uiso 1 1 calc R . . H12C H 0.3722 0.6221 0.3804 0.080 Uiso 1 1 calc R . . C13 C 0.45378(17) 0.6045(3) 0.4819(4) 0.0499(12) Uani 1 1 d . . . H13A H 0.4529 0.6524 0.4426 0.080 Uiso 1 1 calc R . . H13B H 0.4733 0.5603 0.4543 0.080 Uiso 1 1 calc R . . C14 C 0.48199(19) 0.6300(3) 0.5659(4) 0.0560(14) Uani 1 1 d . . . H14A H 0.5181 0.6390 0.5532 0.080 Uiso 1 1 calc R . . H14B H 0.4804 0.5836 0.6068 0.080 Uiso 1 1 calc R . . C15 C 0.46166(18) 0.7084(3) 0.6101(3) 0.0495(12) Uani 1 1 d . . . H15A H 0.4875 0.7274 0.6528 0.080 Uiso 1 1 calc R . . H15B H 0.4576 0.7524 0.5664 0.080 Uiso 1 1 calc R . . C16 C 0.4171(2) 0.6381(3) 0.7287(3) 0.0595(15) Uani 1 1 d . . . H16A H 0.4266 0.5837 0.7068 0.080 Uiso 1 1 calc R . . H16B H 0.3848 0.6339 0.7578 0.080 Uiso 1 1 calc R . . H16C H 0.4434 0.6577 0.7693 0.080 Uiso 1 1 calc R . . C17 C 0.3973(2) 0.7815(3) 0.6906(3) 0.0550(13) Uani 1 1 d . . . H17A H 0.3650 0.7769 0.7195 0.080 Uiso 1 1 calc R . . H17B H 0.3941 0.8216 0.6438 0.080 Uiso 1 1 calc R . . H17C H 0.4237 0.7999 0.7317 0.080 Uiso 1 1 calc R . . C18 C 0.4529(3) 0.6708(4) 0.2253(4) 0.085(2) Uani 1 1 d . . . H18A H 0.4577 0.6982 0.1702 0.080 Uiso 1 1 calc R . . H18B H 0.4467 0.7124 0.2694 0.080 Uiso 1 1 calc R . . H18C H 0.4237 0.6335 0.2204 0.080 Uiso 1 1 calc R . . C19 C 0.5000 0.6218(5) 0.2500 0.068(2) Uani 1 2 d S . . C20 C 0.5051(15) 0.0928(18) 0.6958(15) 0.257(16) Uiso 0.50 1 d PD B -3 H20A H 0.5055 0.1398 0.7352 0.080 Uiso 0.50 1 calc PR B -3 H20B H 0.5301 0.0518 0.7158 0.080 Uiso 0.50 1 calc PR B -3 H20C H 0.4714 0.0677 0.6940 0.080 Uiso 0.50 1 calc PR B -3 C21 C 0.5189(10) 0.1232(13) 0.6028(12) 0.150(8) Uiso 0.50 1 d PD B -3 H21A H 0.4968 0.1701 0.5857 0.080 Uiso 0.50 1 calc PR B -3 H21B H 0.5545 0.1422 0.6028 0.080 Uiso 0.50 1 calc PR B -3 C22 C 0.5121(11) 0.0578(16) 0.5443(15) 0.179(10) Uiso 0.50 1 d PD B -3 H22A H 0.4750 0.0494 0.5458 0.080 Uiso 0.50 1 calc PR B -3 H22B H 0.5265 0.0110 0.5775 0.080 Uiso 0.50 1 calc PR B -3 C23 C 0.5226(9) 0.0323(16) 0.4557(13) 0.158(8) Uiso 0.50 1 d PD B -3 H23A H 0.5477 -0.0118 0.4685 0.080 Uiso 0.50 1 calc PR B -3 H23B H 0.5436 0.0799 0.4387 0.080 Uiso 0.50 1 calc PR B -3 C24 C 0.5043(14) 0.003(2) 0.3653(17) 0.31(2) Uiso 0.50 1 d PD B -3 H24A H 0.5226 0.0337 0.3216 0.080 Uiso 0.50 1 calc PR B -3 H24B H 0.4679 0.0139 0.3580 0.080 Uiso 0.50 1 calc PR B -3 H24C H 0.5108 -0.0559 0.3592 0.080 Uiso 0.50 1 calc PR B -3 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 0.0378(3) 0.0170(2) 0.0272(3) 0.00022(19) 0.0000(2) 0.0034(2) Ni2 0.0339(3) 0.0184(2) 0.0372(3) 0.0019(2) -0.0025(2) 0.0021(2) Cl1A 0.0475(11) 0.0291(10) 0.0338(8) -0.0033(7) -0.0005(7) -0.0084(8) O1A 0.042(3) 0.049(2) 0.046(3) -0.003(2) 0.022(2) -0.012(2) O2A 0.082(6) 0.051(4) 0.084(5) -0.021(4) 0.043(4) -0.002(3) O3A 0.082(4) 0.039(2) 0.064(3) 0.017(2) 0.011(3) -0.011(2) O4A 0.090(4) 0.085(5) 0.053(4) -0.004(3) -0.028(4) -0.013(3) Cl1B 0.062(5) 0.033(3) 0.062(4) 0.006(3) 0.009(3) -0.013(3) O1B 0.042(3) 0.049(2) 0.046(3) -0.003(2) 0.022(2) -0.012(2) O2B 0.11(3) 0.091(17) 0.033(10) 0.007(9) 0.030(13) 0.005(17) O3B 0.054(10) 0.083(12) 0.080(11) 0.041(9) 0.010(9) 0.003(8) O4B 0.090(4) 0.085(5) 0.053(4) -0.004(3) -0.028(4) -0.013(3) N1 0.037(2) 0.0217(16) 0.0368(18) 0.0021(13) 0.0006(16) 0.0006(13) N2 0.037(2) 0.0193(15) 0.047(2) 0.0016(14) 0.0020(17) 0.0050(14) N3 0.041(2) 0.0216(15) 0.0315(17) -0.0020(13) -0.0002(16) 0.0019(14) N4 0.054(2) 0.0204(15) 0.0292(17) -0.0003(13) 0.0005(17) -0.0008(14) N5 0.038(2) 0.0214(16) 0.057(2) 0.0024(15) 0.0065(18) 0.0022(14) N6 0.044(2) 0.0356(19) 0.048(2) 0.0076(16) -0.0099(19) -0.0002(16) N7 0.043(2) 0.0140(15) 0.0389(18) 0.0014(13) -0.0019(16) 0.0016(13) N8 0.040(2) 0.0261(19) 0.0352(18) -0.0023(14) -0.0027(16) -0.0018(15) N9 0.057(3) 0.0242(19) 0.063(3) 0.0049(17) 0.004(2) 0.0062(17) N10 0.047(2) 0.0297(17) 0.0348(19) 0.0044(15) 0.0036(17) 0.0081(15) N11 0.0286(18) 0.0182(15) 0.0359(19) 0.0024(13) 0.0042(16) 0.0026(12) N12 0.043(2) 0.0302(18) 0.044(2) 0.0081(15) -0.0035(19) 0.0013(15) O5 0.119(6) 0.058(4) 0.134(6) 0.000 0.026(5) 0.000 C1 0.044(3) 0.0168(18) 0.053(3) 0.0007(17) 0.005(2) 0.0026(16) C2 0.042(2) 0.0228(18) 0.032(2) 0.0032(16) -0.0017(19) 0.0013(17) C3 0.044(3) 0.0191(18) 0.055(3) 0.0034(18) 0.006(2) 0.0074(17) C4 0.040(2) 0.0152(17) 0.041(2) 0.0000(15) 0.001(2) 0.0019(15) C5 0.050(3) 0.028(2) 0.039(2) -0.0016(17) -0.006(2) -0.0006(18) C6 0.040(3) 0.029(2) 0.045(2) 0.0001(17) 0.011(2) -0.0028(17) C7 0.054(3) 0.027(2) 0.044(2) 0.0050(18) 0.012(2) -0.0001(19) C8 0.062(3) 0.029(2) 0.032(2) -0.0011(17) 0.012(2) 0.0018(19) C9 0.067(3) 0.037(2) 0.034(2) 0.0057(18) -0.012(2) -0.001(2) C10 0.085(4) 0.024(2) 0.035(2) -0.0096(17) 0.000(2) -0.007(2) C11 0.042(3) 0.022(2) 0.075(3) 0.004(2) 0.014(3) 0.0027(18) C12 0.056(3) 0.036(2) 0.053(3) -0.010(2) 0.009(2) -0.001(2) C13 0.035(3) 0.037(2) 0.079(3) 0.007(2) 0.013(3) 0.0015(19) C14 0.035(3) 0.038(2) 0.095(4) 0.007(2) 0.003(3) 0.003(2) C15 0.039(3) 0.038(2) 0.071(3) 0.008(2) -0.010(3) -0.004(2) C16 0.059(3) 0.062(3) 0.056(3) 0.021(2) -0.025(3) -0.009(2) C17 0.061(3) 0.048(3) 0.055(3) -0.013(2) -0.008(3) -0.010(2) C18 0.111(6) 0.085(5) 0.058(4) 0.013(3) -0.005(4) -0.008(4) C19 0.094(7) 0.061(5) 0.048(4) 0.000 0.009(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 1.938(3) . ? Ni1 N10 2.036(3) . ? Ni1 N4 2.051(3) . ? Ni1 N7 2.123(3) . ? Ni1 N3 2.139(3) . ? Ni2 N2 1.941(3) . ? Ni2 N12 2.021(3) 7_566 ? Ni2 N6 2.049(4) . ? Ni2 N7 2.120(4) . ? Ni2 N5 2.165(4) . ? Ni1 Ni2 3.6141(8) . ? Ni1 Ni1 6.707(1) 7_566 ? Ni1 Ni2 5.4797(7) 7_566 ? Ni2 Ni2 6.418(1) 7_566 ? Cl1A O2A 1.430(7) . ? Cl1A O3A 1.433(5) . ? Cl1A O4A 1.433(5) . ? Cl1A O1A 1.451(5) . ? Cl1B O4B 1.395(14) . ? Cl1B O3B 1.407(13) . ? Cl1B O2B 1.441(15) . ? Cl1B O1B 1.463(14) . ? N1 N2 1.343(5) . ? N1 C2 1.345(5) . ? N2 C3 1.353(5) . ? N3 C6 1.482(6) . ? N3 C5 1.489(5) . ? N3 C4 1.505(5) . ? N4 C9 1.474(5) . ? N4 C8 1.484(6) . ? N4 C10 1.491(5) . ? N5 C12 1.465(6) . ? N5 C13 1.486(6) . ? N5 C11 1.507(5) . ? N6 C17 1.482(6) . ? N6 C15 1.486(6) . ? N6 C16 1.487(6) . ? N7 N8 1.218(4) . ? N8 N9 1.148(4) . ? N10 N11 1.177(4) . ? N11 N12 1.165(4) . ? N12 Ni2 2.021(3) 7_566 ? O5 C19 1.202(10) . ? C1 C2 1.390(6) . ? C1 C3 1.402(6) . ? C2 C4 1.496(6) . ? C3 C11 1.491(6) . ? C6 C7 1.526(6) . ? C7 C8 1.528(6) . ? C13 C14 1.515(7) . ? C14 C15 1.518(7) . ? C18 C19 1.488(8) . ? C19 C18 1.488(8) 2_655 ? C20 C21 1.553(17) . ? C21 C22 1.381(16) . ? C22 C23 1.447(17) . ? C23 C24 1.521(18) . ? 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 N1 Ni1 N10 161.12(14) . . ? N1 Ni1 N4 105.40(14) . . ? N10 Ni1 N4 92.92(14) . . ? N1 Ni1 N7 85.38(13) . . ? N10 Ni1 N7 93.05(13) . . ? N4 Ni1 N7 108.88(13) . . ? N1 Ni1 N3 79.23(13) . . ? N10 Ni1 N3 94.38(14) . . ? N4 Ni1 N3 96.78(13) . . ? N7 Ni1 N3 152.84(13) . . ? N2 Ni2 N12 160.87(14) . 7_566 ? N2 Ni2 N6 106.35(14) . . ? N12 Ni2 N6 92.09(14) 7_566 . ? N2 Ni2 N7 85.32(13) . . ? N12 Ni2 N7 94.92(14) 7_566 . ? N6 Ni2 N7 105.10(14) . . ? N2 Ni2 N5 79.41(14) . . ? N12 Ni2 N5 93.47(14) 7_566 . ? N6 Ni2 N5 97.36(15) . . ? N7 Ni2 N5 155.68(13) . . ? O2A Cl1A O3A 110.0(5) . . ? O2A Cl1A O4A 111.4(6) . . ? O3A Cl1A O4A 108.6(4) . . ? O2A Cl1A O1A 110.0(4) . . ? O3A Cl1A O1A 108.9(3) . . ? O4A Cl1A O1A 108.0(4) . . ? O4B Cl1B O3B 109.4(12) . . ? O4B Cl1B O2B 109.9(15) . . ? O3B Cl1B O2B 111.1(15) . . ? O4B Cl1B O1B 108.5(14) . . ? O3B Cl1B O1B 110.1(10) . . ? O2B Cl1B O1B 107.8(14) . . ? N2 N1 C2 108.9(3) . . ? N2 N1 Ni1 125.9(2) . . ? C2 N1 Ni1 121.0(3) . . ? N1 N2 C3 108.5(3) . . ? N1 N2 Ni2 125.7(2) . . ? C3 N2 Ni2 120.3(3) . . ? C6 N3 C5 109.5(3) . . ? C6 N3 C4 111.7(3) . . ? C5 N3 C4 107.9(3) . . ? C6 N3 Ni1 113.9(2) . . ? C5 N3 Ni1 103.9(2) . . ? C4 N3 Ni1 109.5(2) . . ? C9 N4 C8 110.5(3) . . ? C9 N4 C10 107.2(3) . . ? C8 N4 C10 108.1(3) . . ? C9 N4 Ni1 112.3(3) . . ? C8 N4 Ni1 111.1(2) . . ? C10 N4 Ni1 107.5(2) . . ? C12 N5 C13 109.9(4) . . ? C12 N5 C11 108.1(3) . . ? C13 N5 C11 111.2(3) . . ? C12 N5 Ni2 105.8(3) . . ? C13 N5 Ni2 113.2(3) . . ? C11 N5 Ni2 108.3(3) . . ? C17 N6 C15 107.7(4) . . ? C17 N6 C16 108.1(4) . . ? C15 N6 C16 110.8(4) . . ? C17 N6 Ni2 108.6(3) . . ? C15 N6 Ni2 111.8(3) . . ? C16 N6 Ni2 109.7(3) . . ? N8 N7 Ni2 120.6(3) . . ? N8 N7 Ni1 120.8(3) . . ? Ni2 N7 Ni1 116.83(13) . . ? N9 N8 N7 179.1(4) . . ? N11 N10 Ni1 126.0(3) . . ? N12 N11 N10 176.2(4) . . ? N11 N12 Ni2 134.8(3) . 7_566 ? C2 C1 C3 104.6(3) . . ? N1 C2 C1 109.2(4) . . ? N1 C2 C4 113.8(3) . . ? C1 C2 C4 136.9(3) . . ? N2 C3 C1 108.7(4) . . ? N2 C3 C11 113.5(4) . . ? C1 C3 C11 137.7(4) . . ? C2 C4 N3 107.7(3) . . ? N3 C6 C7 114.2(4) . . ? C6 C7 C8 115.4(3) . . ? N4 C8 C7 116.0(3) . . ? C3 C11 N5 107.9(3) . . ? N5 C13 C14 114.7(4) . . ? C13 C14 C15 115.6(4) . . ? N6 C15 C14 115.6(4) . . ? O5 C19 C18 121.6(4) . . ? O5 C19 C18 121.6(4) . 2_655 ? C18 C19 C18 116.8(8) . 2_655 ? C22 C21 C20 109(2) . . ? C21 C22 C23 143(3) . . ? C22 C23 C24 151(3) . . ? 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 N10 N12 Ni2 -91.4(3) . . . 7_566 ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 24.75 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.508 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.066 data_4c _database_code_depnum_ccdc_archive 'CCDC 292201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H70 N24 Ni4 2+, 2(C24 H20 B -), C3 H6 O' _chemical_formula_sum 'C85 H116 B2 N24 Ni4 O' _chemical_formula_weight 1746.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7053(6) _cell_length_b 18.9522(12) _cell_length_c 26.0462(15) _cell_angle_alpha 83.808(5) _cell_angle_beta 82.862(5) _cell_angle_gamma 75.504(5) _cell_volume 4587.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 41173 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 24.92 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41173 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 24.92 _reflns_number_total 12180 _reflns_number_gt 7193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Crystals of 4c are non-merohedrally twinned (ratio of the two twin components approximately 70 : 30, twin-law -1, 0, -0.002 / -0.883, 0.354, 0.645 / -0.875, 1.358, -0.356) and the reflection data for refinement were prepared using the program X-AREA [X-AREA. (2002) STOE & CIE GmbH, Darmstadt, Germany]. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12180 _refine_ls_number_parameters 1373 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.34011(10) 0.35385(5) 0.51581(3) 0.0348(2) Uani 1 1 d . . . Ni2 Ni 0.51319(10) 0.42799(5) 0.39728(3) 0.0367(2) Uani 1 1 d . . . N1 N 0.2770(6) 0.3655(3) 0.4475(2) 0.0402(14) Uani 1 1 d . . . N2 N 0.3415(6) 0.3933(3) 0.4033(2) 0.0374(14) Uani 1 1 d . . . N3 N 0.1164(8) 0.3527(5) 0.5341(2) 0.061(2) Uani 1 1 d . . . N4 N 0.4259(10) 0.2464(4) 0.5378(3) 0.074(3) Uani 1 1 d . . . N5 N 0.4191(7) 0.4824(3) 0.3282(2) 0.0435(15) Uani 1 1 d . . . N6 N 0.6655(6) 0.3488(3) 0.3611(2) 0.0381(14) Uani 1 1 d . . . N7 N 0.5191(6) 0.3912(4) 0.4775(2) 0.0437(15) Uani 1 1 d . . . N8 N 0.6001(7) 0.4100(4) 0.5020(2) 0.0525(18) Uani 1 1 d . . . N9 N 0.6747(9) 0.4291(6) 0.5257(3) 0.084(3) Uani 1 1 d . . . N10 N 0.3567(7) 0.3873(4) 0.5851(2) 0.0441(15) Uani 1 1 d . . . N11 N 0.3565(6) 0.4479(4) 0.5926(2) 0.0395(14) Uani 1 1 d . . . N12 N 0.3482(8) 0.5074(4) 0.6028(2) 0.0568(19) Uani 1 1 d . . . C1 C 0.1169(9) 0.4010(6) 0.3895(3) 0.062(3) Uani 1 1 d . . . H1 H 0.0325 0.4098 0.3738 0.080 Uiso 1 1 calc R . . C2 C 0.1412(9) 0.3713(5) 0.4396(3) 0.055(2) Uani 1 1 d . . . C3 C 0.2462(8) 0.4145(4) 0.3683(3) 0.0436(18) Uani 1 1 d . . . C4 C 0.0571(11) 0.3415(8) 0.4854(3) 0.085(4) Uani 1 1 d . . . H4A H 0.0653 0.2898 0.4831 0.080 Uiso 1 1 calc R . . H4B H -0.0432 0.3667 0.4861 0.080 Uiso 1 1 calc R . . C5 C 0.0503(10) 0.4284(7) 0.5491(4) 0.077(3) Uani 1 1 d . . . H5A H 0.0727 0.4630 0.5215 0.080 Uiso 1 1 calc R . . H5B H 0.0873 0.4358 0.5801 0.080 Uiso 1 1 calc R . . H5C H -0.0516 0.4353 0.5553 0.080 Uiso 1 1 calc R . . C6 C 0.0844(13) 0.2982(8) 0.5771(3) 0.092(4) Uani 1 1 d . . . H6A H -0.0127 0.2936 0.5764 0.080 Uiso 1 1 calc R . . H6B H 0.0898 0.3162 0.6101 0.080 Uiso 1 1 calc R . . C7 C 0.186(2) 0.2234(7) 0.5735(4) 0.120(6) Uani 1 1 d . . . H7A H 0.1497 0.1894 0.5989 0.080 Uiso 1 1 calc R . . H7B H 0.1847 0.2074 0.5395 0.080 Uiso 1 1 calc R . . C8 C 0.3357(15) 0.2186(5) 0.5818(4) 0.089(4) Uani 1 1 d . . . H8A H 0.3809 0.1678 0.5907 0.080 Uiso 1 1 calc R . . H8B H 0.3353 0.2454 0.6115 0.080 Uiso 1 1 calc R . . C9 C 0.4428(16) 0.2012(5) 0.4933(4) 0.115(5) Uani 1 1 d . . . H9A H 0.5064 0.2172 0.4659 0.080 Uiso 1 1 calc R . . H9B H 0.3512 0.2063 0.4810 0.080 Uiso 1 1 calc R . . H9C H 0.4816 0.1508 0.5042 0.080 Uiso 1 1 calc R . . C10 C 0.5658(14) 0.2391(7) 0.5562(4) 0.109(5) Uani 1 1 d . . . H10A H 0.6030 0.1893 0.5689 0.080 Uiso 1 1 calc R . . H10B H 0.5556 0.2705 0.5837 0.080 Uiso 1 1 calc R . . H10C H 0.6304 0.2528 0.5281 0.080 Uiso 1 1 calc R . . C11 C 0.3052(8) 0.4470(5) 0.3177(3) 0.049(2) Uani 1 1 d . . . H11A H 0.3451 0.4090 0.2942 0.080 Uiso 1 1 calc R . . H11B H 0.2296 0.4829 0.3017 0.080 Uiso 1 1 calc R . . C12 C 0.3487(10) 0.5580(5) 0.3407(3) 0.062(2) Uani 1 1 d . . . H12A H 0.2998 0.5838 0.3118 0.080 Uiso 1 1 calc R . . H12B H 0.4194 0.5824 0.3475 0.080 Uiso 1 1 calc R . . H12C H 0.2811 0.5571 0.3708 0.080 Uiso 1 1 calc R . . C13 C 0.5257(9) 0.4846(4) 0.2815(3) 0.051(2) Uani 1 1 d . . . H13A H 0.5824 0.5185 0.2861 0.080 Uiso 1 1 calc R . . H13B H 0.4745 0.5031 0.2512 0.080 Uiso 1 1 calc R . . C14 C 0.6251(9) 0.4111(5) 0.2714(3) 0.052(2) Uani 1 1 d . . . H14A H 0.5669 0.3771 0.2689 0.080 Uiso 1 1 calc R . . H14B H 0.6789 0.4160 0.2378 0.080 Uiso 1 1 calc R . . C15 C 0.7302(9) 0.3775(5) 0.3104(3) 0.051(2) Uani 1 1 d . . . H15A H 0.8017 0.3377 0.2953 0.080 Uiso 1 1 calc R . . H15B H 0.7788 0.4139 0.3172 0.080 Uiso 1 1 calc R . . C16 C 0.6092(9) 0.2859(4) 0.3525(3) 0.0488(19) Uani 1 1 d . . . H16A H 0.5308 0.3023 0.3315 0.080 Uiso 1 1 calc R . . H16B H 0.5767 0.2642 0.3853 0.080 Uiso 1 1 calc R . . H16C H 0.6835 0.2504 0.3350 0.080 Uiso 1 1 calc R . . C17 C 0.7855(9) 0.3212(5) 0.3946(3) 0.058(2) Uani 1 1 d . . . H17A H 0.7513 0.2976 0.4264 0.080 Uiso 1 1 calc R . . H17B H 0.8209 0.3614 0.4023 0.080 Uiso 1 1 calc R . . H17C H 0.8611 0.2868 0.3768 0.080 Uiso 1 1 calc R . . Ni1A Ni 0.3428(8) 0.1818(6) 0.0043(3) 0.0347(10) Uani 0.629(9) 1 d PD A 1 Ni2A Ni 0.2562(5) 0.03630(18) 0.09497(14) 0.0423(8) Uani 0.629(9) 1 d PD . 1 N1A N 0.1557(11) 0.1751(7) 0.0341(5) 0.036(4) Uani 0.629(9) 1 d PD A 1 N2A N 0.1224(12) 0.1231(7) 0.0681(5) 0.043(3) Uani 0.629(9) 1 d PD A 1 N3A N 0.2127(18) 0.2472(7) -0.0543(5) 0.056(4) Uani 0.629(9) 1 d PD A 1 N5A N 0.0583(15) 0.0015(6) 0.1087(5) 0.058(4) Uani 0.629(9) 1 d PD A 1 N6A N 0.2817(16) 0.0486(6) 0.1707(4) 0.050(3) Uani 0.629(9) 1 d PD A 1 N10A N 0.5280(18) 0.1628(10) -0.0434(7) 0.062(5) Uani 0.629(9) 1 d PD A 1 N11A N 0.572(2) 0.1125(12) -0.0693(9) 0.065(8) Uani 0.629(9) 1 d PD A 1 N12A N 0.619(3) 0.0653(14) -0.0961(9) 0.079(9) Uani 0.629(9) 1 d PD . 1 C1A C -0.0747(14) 0.1785(8) 0.0303(6) 0.059(4) Uani 0.629(9) 1 d PD A 1 H1A H -0.1681 0.1913 0.0213 0.080 Uiso 0.629(9) 1 calc PR A 1 C2A C 0.0359(13) 0.2094(9) 0.0104(6) 0.049(4) Uani 0.629(9) 1 d PD A 1 C3A C -0.0153(15) 0.1226(9) 0.0678(6) 0.046(4) Uani 0.629(9) 1 d PD A 1 C4A C 0.061(2) 0.2692(10) -0.0299(9) 0.062(6) Uani 0.629(9) 1 d PD A 1 H4C H 0.0452 0.3148 -0.0139 0.080 Uiso 0.629(9) 1 calc PR A 1 H4D H -0.0053 0.2760 -0.0561 0.080 Uiso 0.629(9) 1 calc PR A 1 C5A C 0.220(2) 0.1980(8) -0.0940(6) 0.067(4) Uani 0.629(9) 1 d PD A 1 H5D H 0.1704 0.2243 -0.1226 0.080 Uiso 0.629(9) 1 calc PR A 1 H5E H 0.1760 0.1591 -0.0798 0.080 Uiso 0.629(9) 1 calc PR A 1 H5F H 0.3182 0.1779 -0.1060 0.080 Uiso 0.629(9) 1 calc PR A 1 C6A C 0.262(3) 0.3120(8) -0.0784(5) 0.073(6) Uani 0.629(9) 1 d PD A 1 H6C H 0.2007 0.3376 -0.1046 0.080 Uiso 0.629(9) 1 calc PR A 1 H6D H 0.3591 0.2974 -0.0947 0.080 Uiso 0.629(9) 1 calc PR A 1 C11A C -0.0637(15) 0.0650(8) 0.1038(5) 0.061(4) Uani 0.629(9) 1 d PD A 1 H11C H -0.0985 0.0835 0.1375 0.080 Uiso 0.629(9) 1 calc PR A 1 H11D H -0.1409 0.0511 0.0903 0.080 Uiso 0.629(9) 1 calc PR A 1 C12A C 0.064(2) -0.0474(9) 0.0660(6) 0.069(5) Uani 0.629(9) 1 d PD A 1 H12D H -0.0226 -0.0636 0.0691 0.080 Uiso 0.629(9) 1 calc PR A 1 H12E H 0.1441 -0.0890 0.0690 0.080 Uiso 0.629(9) 1 calc PR A 1 H12F H 0.0758 -0.0207 0.0329 0.080 Uiso 0.629(9) 1 calc PR A 1 C13A C 0.038(2) -0.0412(9) 0.1588(6) 0.079(5) Uani 0.629(9) 1 d PD A 1 H13C H 0.1018 -0.0894 0.1578 0.080 Uiso 0.629(9) 1 calc PR A 1 H13D H -0.0597 -0.0472 0.1641 0.080 Uiso 0.629(9) 1 calc PR A 1 C14A C 0.0657(18) -0.0038(9) 0.2046(5) 0.068(5) Uani 0.629(9) 1 d PD A 1 H14C H 0.0109 0.0466 0.2021 0.080 Uiso 0.629(9) 1 calc PR A 1 H14D H 0.0289 -0.0274 0.2364 0.080 Uiso 0.629(9) 1 calc PR A 1 C15A C 0.217(3) -0.0040(10) 0.2092(7) 0.064(6) Uani 0.629(9) 1 d PD A 1 H15C H 0.2746 -0.0532 0.2051 0.080 Uiso 0.629(9) 1 calc PR A 1 H15D H 0.2231 0.0075 0.2440 0.080 Uiso 0.629(9) 1 calc PR A 1 C16A C 0.433(4) 0.0363(18) 0.1771(11) 0.092(11) Uani 0.629(9) 1 d PD A 1 H16D H 0.4723 0.0727 0.1558 0.080 Uiso 0.629(9) 1 calc PR A 1 H16E H 0.4831 -0.0114 0.1668 0.080 Uiso 0.629(9) 1 calc PR A 1 H16F H 0.4448 0.0394 0.2128 0.080 Uiso 0.629(9) 1 calc PR A 1 C17A C 0.209(2) 0.1248(7) 0.1830(5) 0.059(4) Uani 0.629(9) 1 d PD A 1 H17D H 0.2113 0.1297 0.2191 0.080 Uiso 0.629(9) 1 calc PR A 1 H17E H 0.1110 0.1354 0.1753 0.080 Uiso 0.629(9) 1 calc PR A 1 H17F H 0.2566 0.1583 0.1623 0.080 Uiso 0.629(9) 1 calc PR A 1 Ni1B Ni 0.3161(14) 0.1807(10) 0.0075(6) 0.049(3) Uani 0.371(9) 1 d PD A 2 Ni2B Ni 0.3093(8) 0.0330(3) 0.1065(2) 0.0426(13) Uani 0.371(9) 1 d PD . 2 N1B N 0.1565(17) 0.1713(11) 0.0562(8) 0.039(7) Uani 0.371(9) 1 d PD A 2 N2B N 0.1521(16) 0.1169(8) 0.0926(8) 0.037(5) Uani 0.371(9) 1 d PD A 2 N3B N 0.142(3) 0.2468(10) -0.0353(8) 0.056(10) Uani 0.371(9) 1 d PD A 2 N5B N 0.1289(19) -0.0098(8) 0.1392(8) 0.059(6) Uani 0.371(9) 1 d PD A 2 N6B N 0.386(3) 0.0467(12) 0.1743(8) 0.039(8) Uani 0.371(9) 1 d PD A 2 N10B N 0.462(3) 0.1687(15) -0.0560(8) 0.068(11) Uani 0.371(9) 1 d PD A 2 N11B N 0.513(4) 0.1146(17) -0.0767(11) 0.048(10) Uani 0.371(9) 1 d PD A 2 N12B N 0.558(5) 0.0672(19) -0.1033(16) 0.067(15) Uani 0.371(9) 1 d PD . 2 C1B C -0.072(2) 0.1670(15) 0.0760(12) 0.072(9) Uani 0.371(9) 1 d PD A 2 H1B H -0.1708 0.1760 0.0761 0.080 Uiso 0.371(9) 1 calc PR A 2 C2B C 0.0190(19) 0.2031(10) 0.0451(12) 0.051(6) Uani 0.371(9) 1 d PD A 2 C3B C 0.017(2) 0.1130(10) 0.1077(10) 0.058(6) Uani 0.371(9) 1 d PD A 2 C4B C 0.008(3) 0.2631(13) 0.0019(11) 0.059(8) Uani 0.371(9) 1 d PD A 2 H4E H -0.0027 0.3097 0.0160 0.080 Uiso 0.371(9) 1 calc PR A 2 H4F H -0.0754 0.2659 -0.0160 0.080 Uiso 0.371(9) 1 calc PR A 2 C5B C 0.118(4) 0.1983(16) -0.0709(12) 0.097(11) Uani 0.371(9) 1 d PD A 2 H5G H 0.0559 0.2259 -0.0957 0.080 Uiso 0.371(9) 1 calc PR A 2 H5H H 0.0751 0.1617 -0.0519 0.080 Uiso 0.371(9) 1 calc PR A 2 H5I H 0.2081 0.1751 -0.0888 0.080 Uiso 0.371(9) 1 calc PR A 2 C6B C 0.180(3) 0.3146(11) -0.0616(9) 0.093(15) Uani 0.371(9) 1 d PD A 2 H6E H 0.0913 0.3471 -0.0717 0.080 Uiso 0.371(9) 1 calc PR A 2 H6F H 0.2386 0.3006 -0.0935 0.080 Uiso 0.371(9) 1 calc PR A 2 C11B C 0.002(2) 0.0517(12) 0.1476(11) 0.089(11) Uani 0.371(9) 1 d PD A 2 H11E H -0.0041 0.0676 0.1821 0.080 Uiso 0.371(9) 1 calc PR A 2 H11F H -0.0844 0.0363 0.1443 0.080 Uiso 0.371(9) 1 calc PR A 2 C12B C 0.105(4) -0.0548(16) 0.0985(12) 0.096(12) Uani 0.371(9) 1 d PD A 2 H12G H 0.0069 -0.0585 0.1031 0.080 Uiso 0.371(9) 1 calc PR A 2 H12H H 0.1669 -0.1028 0.1018 0.080 Uiso 0.371(9) 1 calc PR A 2 H12I H 0.1244 -0.0317 0.0647 0.080 Uiso 0.371(9) 1 calc PR A 2 C13B C 0.152(3) -0.0562(12) 0.1886(9) 0.068(8) Uani 0.371(9) 1 d PD A 2 H13E H 0.2167 -0.1027 0.1808 0.080 Uiso 0.371(9) 1 calc PR A 2 H13F H 0.0617 -0.0659 0.2037 0.080 Uiso 0.371(9) 1 calc PR A 2 C14B C 0.214(4) -0.023(2) 0.2290(11) 0.085(14) Uani 0.371(9) 1 d PD A 2 H14E H 0.1511 0.0241 0.2356 0.080 Uiso 0.371(9) 1 calc PR A 2 H14F H 0.2121 -0.0543 0.2611 0.080 Uiso 0.371(9) 1 calc PR A 2 C15B C 0.362(3) -0.0135(10) 0.2158(7) 0.061(8) Uani 0.371(9) 1 d PD A 2 H15E H 0.4217 -0.0595 0.2048 0.080 Uiso 0.371(9) 1 calc PR A 2 H15F H 0.3952 -0.0044 0.2475 0.080 Uiso 0.371(9) 1 calc PR A 2 C16B C 0.541(3) 0.0416(14) 0.1658(9) 0.066(8) Uani 0.371(9) 1 d PD A 2 H16G H 0.5578 0.0841 0.1451 0.080 Uiso 0.371(9) 1 calc PR A 2 H16H H 0.5873 -0.0013 0.1482 0.080 Uiso 0.371(9) 1 calc PR A 2 H16I H 0.5780 0.0385 0.1987 0.080 Uiso 0.371(9) 1 calc PR A 2 C17B C 0.310(3) 0.1188(10) 0.1936(8) 0.046(5) Uani 0.371(9) 1 d PD A 2 H17G H 0.3617 0.1548 0.1801 0.080 Uiso 0.371(9) 1 calc PR A 2 H17H H 0.3025 0.1150 0.2309 0.080 Uiso 0.371(9) 1 calc PR A 2 H17I H 0.2155 0.1329 0.1823 0.080 Uiso 0.371(9) 1 calc PR A 2 N104 N 0.3829(7) 0.2681(3) 0.0328(3) 0.0491(16) Uani 1 1 d . . . N107 N 0.4202(7) 0.0870(3) 0.0525(2) 0.0469(16) Uani 1 1 d . . . N108 N 0.5428(9) 0.0539(4) 0.0443(3) 0.066(2) Uani 1 1 d . A . N109 N 0.6591(10) 0.0208(6) 0.0367(5) 0.115(4) Uani 1 1 d . . . C107 C 0.2556(17) 0.3607(5) -0.0357(4) 0.107(5) Uani 1 1 d D . . H10D H 0.294(8) 0.399(3) -0.055(2) 0.080 Uiso 1 1 d D . . H10E H 0.203(5) 0.381(4) -0.0043(17) 0.080 Uiso 1 1 d D . . C108 C 0.3907(13) 0.3287(5) -0.0094(4) 0.083(4) Uani 1 1 d . A . H10F H 0.4672 0.3101 -0.0358 0.080 Uiso 1 1 calc R . . H10G H 0.4164 0.3679 0.0054 0.080 Uiso 1 1 calc R . . C109 C 0.5216(11) 0.2405(6) 0.0537(6) 0.117(5) Uani 1 1 d . A . H10H H 0.5445 0.2788 0.0699 0.080 Uiso 1 1 calc R . . H10I H 0.5942 0.2246 0.0260 0.080 Uiso 1 1 calc R . . H10J H 0.5168 0.2002 0.0789 0.080 Uiso 1 1 calc R . . C110 C 0.2769(10) 0.2981(4) 0.0752(3) 0.058(2) Uani 1 1 d . A . H11G H 0.2815 0.2626 0.1046 0.080 Uiso 1 1 calc R . . H11H H 0.1829 0.3098 0.0639 0.080 Uiso 1 1 calc R . . H11I H 0.2973 0.3416 0.0850 0.080 Uiso 1 1 calc R . . B1 B 0.0486(8) 0.4791(4) 0.1671(3) 0.0336(18) Uani 1 1 d . . . C20 C 0.1569(7) 0.4064(4) 0.1941(2) 0.0329(15) Uani 1 1 d . . . C21 C 0.1046(8) 0.3567(4) 0.2310(3) 0.0402(17) Uani 1 1 d . . . H21 H 0.0063 0.3643 0.2393 0.080 Uiso 1 1 calc R . . C22 C 0.1935(9) 0.2972(4) 0.2552(3) 0.054(2) Uani 1 1 d . . . H22 H 0.1542 0.2669 0.2801 0.080 Uiso 1 1 calc R . . C23 C 0.3399(9) 0.2821(5) 0.2429(3) 0.053(2) Uani 1 1 d . . . H23 H 0.3995 0.2419 0.2592 0.080 Uiso 1 1 calc R . . C24 C 0.3945(8) 0.3271(4) 0.2068(3) 0.0475(19) Uani 1 1 d . . . H24 H 0.4926 0.3165 0.1972 0.080 Uiso 1 1 calc R . . C25 C 0.3065(7) 0.3891(4) 0.1835(3) 0.0394(17) Uani 1 1 d . . . H25 H 0.3486 0.4201 0.1601 0.080 Uiso 1 1 calc R . . C26 C -0.0065(8) 0.5414(4) 0.2095(2) 0.0407(17) Uani 1 1 d . . . C27 C -0.0478(8) 0.5249(5) 0.2617(3) 0.0440(18) Uani 1 1 d . . . H27 H -0.0310 0.4760 0.2743 0.080 Uiso 1 1 calc R . . C28 C -0.1122(11) 0.5774(6) 0.2957(3) 0.068(3) Uani 1 1 d . . . H28 H -0.1454 0.5635 0.3293 0.080 Uiso 1 1 calc R . . C29 C -0.1276(14) 0.6519(6) 0.2793(4) 0.102(4) Uani 1 1 d . . . H29 H -0.1649 0.6880 0.3022 0.080 Uiso 1 1 calc R . . C30 C -0.0858(18) 0.6695(6) 0.2284(4) 0.125(6) Uani 1 1 d . . . H30 H -0.0982 0.7183 0.2162 0.080 Uiso 1 1 calc R . . C31 C -0.0257(14) 0.6157(5) 0.1951(3) 0.082(3) Uani 1 1 d . . . H31 H 0.0036 0.6300 0.1610 0.080 Uiso 1 1 calc R . . C32 C 0.1311(7) 0.5123(4) 0.1153(3) 0.0349(16) Uani 1 1 d . . . C33 C 0.1046(8) 0.5070(4) 0.0646(2) 0.0371(16) Uani 1 1 d . . . H33 H 0.0339 0.4839 0.0595 0.080 Uiso 1 1 calc R . . C34 C 0.1796(8) 0.5348(4) 0.0210(3) 0.0452(19) Uani 1 1 d . . . H34 H 0.1573 0.5301 -0.0120 0.080 Uiso 1 1 calc R . . C35 C 0.2836(9) 0.5681(5) 0.0262(3) 0.057(2) Uani 1 1 d . . . H35 H 0.3333 0.5864 -0.0030 0.080 Uiso 1 1 calc R . . C36 C 0.3155(10) 0.5749(6) 0.0747(4) 0.083(4) Uani 1 1 d . . . H36 H 0.3869 0.5980 0.0789 0.080 Uiso 1 1 calc R . . C37 C 0.2402(10) 0.5469(6) 0.1181(3) 0.068(3) Uani 1 1 d . . . H37 H 0.2643 0.5518 0.1508 0.080 Uiso 1 1 calc R . . C38 C -0.0911(7) 0.4557(4) 0.1519(2) 0.0351(16) Uani 1 1 d . . . C39 C -0.2261(8) 0.5053(4) 0.1521(3) 0.0461(19) Uani 1 1 d . . . H39 H -0.2371 0.5515 0.1633 0.080 Uiso 1 1 calc R . . C40 C -0.3449(8) 0.4870(5) 0.1359(3) 0.050(2) Uani 1 1 d . . . H40 H -0.4325 0.5211 0.1364 0.080 Uiso 1 1 calc R . . C41 C -0.3327(9) 0.4198(5) 0.1193(3) 0.053(2) Uani 1 1 d . . . H41 H -0.4113 0.4084 0.1082 0.080 Uiso 1 1 calc R . . C42 C -0.2030(9) 0.3685(5) 0.1192(3) 0.052(2) Uani 1 1 d . . . H42 H -0.1935 0.3222 0.1084 0.080 Uiso 1 1 calc R . . C43 C -0.0865(8) 0.3879(5) 0.1355(3) 0.0433(19) Uani 1 1 d . . . H43 H 0.0000 0.3529 0.1354 0.080 Uiso 1 1 calc R . . C50 C 0.7462(12) 0.0950(5) 0.2982(4) 0.070(3) Uani 1 1 d . . . C51 C 0.8708(13) 0.1111(5) 0.3051(3) 0.073(3) Uani 1 1 d . B . H51 H 0.9215 0.0854 0.3321 0.080 Uiso 1 1 calc R . . C52 C 0.9278(12) 0.1643(5) 0.2738(4) 0.071(3) Uani 1 1 d . . . H52 H 1.0121 0.1742 0.2811 0.080 Uiso 1 1 calc R B . C53 C 0.8592(12) 0.2013(5) 0.2328(3) 0.063(2) Uani 1 1 d . B . H53 H 0.8950 0.2372 0.2122 0.080 Uiso 1 1 calc R . . C54 C 0.7393(12) 0.1848(5) 0.2228(4) 0.072(3) Uani 1 1 d . . . H54 H 0.6941 0.2079 0.1939 0.080 Uiso 1 1 calc R B . C55 C 0.6810(11) 0.1333(5) 0.2552(4) 0.075(3) Uani 1 1 d . B . H55 H 0.5958 0.1244 0.2479 0.080 Uiso 1 1 calc R . . B2A B 0.707(2) 0.0362(12) 0.3462(9) 0.044(5) Uani 0.486(4) 1 d P B 3 C56A C 0.7349(12) 0.0406(6) 0.4068(3) 0.037(4) Uani 0.486(4) 1 d PG B 3 C57A C 0.7820(12) 0.0963(5) 0.4244(4) 0.050(4) Uani 0.486(4) 1 d PG B 3 H57A H 0.8021 0.1341 0.4012 0.080 Uiso 0.486(4) 1 calc PR B 3 C58A C 0.7990(12) 0.0954(5) 0.4767(4) 0.055(5) Uani 0.486(4) 1 d PG B 3 H58A H 0.8305 0.1327 0.4885 0.080 Uiso 0.486(4) 1 calc PR B 3 C59A C 0.7690(12) 0.0389(6) 0.5114(3) 0.047(4) Uani 0.486(4) 1 d PG B 3 H59A H 0.7803 0.0383 0.5464 0.080 Uiso 0.486(4) 1 calc PR B 3 C60A C 0.7219(12) -0.0168(6) 0.4938(4) 0.054(7) Uani 0.486(4) 1 d PG B 3 H60A H 0.7018 -0.0547 0.5170 0.080 Uiso 0.486(4) 1 calc PR B 3 C61A C 0.7049(12) -0.0160(5) 0.4415(4) 0.047(6) Uani 0.486(4) 1 d PG B 3 H61A H 0.6734 -0.0533 0.4297 0.080 Uiso 0.486(4) 1 calc PR B 3 C62A C 0.5269(11) 0.0488(8) 0.3483(6) 0.054(6) Uani 0.486(4) 1 d PG B 3 C63A C 0.4406(15) 0.1178(7) 0.3568(7) 0.060(7) Uani 0.486(4) 1 d PG B 3 H63A H 0.4813 0.1577 0.3552 0.080 Uiso 0.486(4) 1 calc PR B 3 C64A C 0.2936(14) 0.1274(9) 0.3679(7) 0.118(13) Uani 0.486(4) 1 d PG B 3 H64A H 0.2359 0.1736 0.3736 0.080 Uiso 0.486(4) 1 calc PR B 3 C65A C 0.2328(12) 0.0679(13) 0.3704(7) 0.129(12) Uani 0.486(4) 1 d PG B 3 H65A H 0.1344 0.0743 0.3778 0.080 Uiso 0.486(4) 1 calc PR B 3 C66A C 0.3191(19) -0.0012(11) 0.3619(6) 0.117(12) Uani 0.486(4) 1 d PG B 3 H66A H 0.2784 -0.0410 0.3635 0.080 Uiso 0.486(4) 1 calc PR B 3 C67A C 0.4661(18) -0.0107(8) 0.3508(5) 0.079(7) Uani 0.486(4) 1 d PG B 3 H67A H 0.5238 -0.0570 0.3451 0.080 Uiso 0.486(4) 1 calc PR B 3 C68A C 0.8085(12) -0.0428(5) 0.3218(4) 0.045(4) Uani 0.486(4) 1 d PG B 3 C69A C 0.9389(12) -0.0741(6) 0.3413(4) 0.047(4) Uani 0.486(4) 1 d PG B 3 H69A H 0.9683 -0.0523 0.3670 0.080 Uiso 0.486(4) 1 calc PR B 3 C70A C 1.0256(11) -0.1380(7) 0.3225(5) 0.074(7) Uani 0.486(4) 1 d PG B 3 H70A H 1.1128 -0.1590 0.3355 0.080 Uiso 0.486(4) 1 calc PR B 3 C71A C 0.9817(16) -0.1706(5) 0.2841(5) 0.095(9) Uani 0.486(4) 1 d PG B 3 H71A H 1.0397 -0.2134 0.2714 0.080 Uiso 0.486(4) 1 calc PR B 3 C72A C 0.8512(18) -0.1393(7) 0.2646(4) 0.089(8) Uani 0.486(4) 1 d PG B 3 H72A H 0.8219 -0.1611 0.2389 0.080 Uiso 0.486(4) 1 calc PR B 3 C73A C 0.7646(13) -0.0754(6) 0.2835(4) 0.061(5) Uani 0.486(4) 1 d PG B 3 H73A H 0.6773 -0.0544 0.2704 0.080 Uiso 0.486(4) 1 calc PR B 3 O1A O 1.348(2) -0.2024(10) 0.1961(9) 0.163(7) Uani 0.486(4) 1 d PD B 3 C74A C 1.252(2) -0.2629(11) 0.1451(8) 0.094(5) Uani 0.486(4) 1 d PD B 3 H74A H 1.2416 -0.2204 0.1209 0.080 Uiso 0.486(4) 1 calc PR B 3 H74B H 1.1604 -0.2643 0.1636 0.080 Uiso 0.486(4) 1 calc PR B 3 H74C H 1.2876 -0.3060 0.1266 0.080 Uiso 0.486(4) 1 calc PR B 3 C75A C 1.3508(15) -0.2600(9) 0.1814(6) 0.089(5) Uani 0.486(4) 1 d PD B 3 C76A C 1.453(2) -0.3227(10) 0.2010(10) 0.133(8) Uani 0.486(4) 1 d PD B 3 H76A H 1.5084 -0.3077 0.2240 0.080 Uiso 0.486(4) 1 calc PR B 3 H76B H 1.5156 -0.3450 0.1725 0.080 Uiso 0.486(4) 1 calc PR B 3 H76C H 1.4039 -0.3573 0.2194 0.080 Uiso 0.486(4) 1 calc PR B 3 B2B B 0.653(3) 0.0290(10) 0.3257(9) 0.058(6) Uani 0.514(4) 1 d P B 4 C56B C 0.7239(12) -0.0058(6) 0.3801(4) 0.056(4) Uani 0.514(4) 1 d PG B 4 C57B C 0.6441(10) 0.0004(7) 0.4283(5) 0.060(6) Uani 0.514(4) 1 d PG B 4 H57B H 0.5483 0.0254 0.4306 0.080 Uiso 0.514(4) 1 calc PR B 4 C58B C 0.7076(15) -0.0307(8) 0.4730(4) 0.094(11) Uani 0.514(4) 1 d PG B 4 H58B H 0.6543 -0.0266 0.5052 0.080 Uiso 0.514(4) 1 calc PR B 4 C59B C 0.8509(15) -0.0681(7) 0.4696(4) 0.067(5) Uani 0.514(4) 1 d PG B 4 H59B H 0.8934 -0.0889 0.4995 0.080 Uiso 0.514(4) 1 calc PR B 4 C60B C 0.9306(10) -0.0743(6) 0.4214(5) 0.061(5) Uani 0.514(4) 1 d PG B 4 H60B H 1.0265 -0.0993 0.4191 0.080 Uiso 0.514(4) 1 calc PR B 4 C61B C 0.8671(11) -0.0432(6) 0.3767(4) 0.057(4) Uani 0.514(4) 1 d PG B 4 H61B H 0.9205 -0.0473 0.3445 0.080 Uiso 0.514(4) 1 calc PR B 4 C62B C 0.4804(12) 0.0767(7) 0.3393(6) 0.054(6) Uani 0.514(4) 1 d PG B 4 C63B C 0.4587(15) 0.1436(7) 0.3601(6) 0.065(7) Uani 0.514(4) 1 d PG B 4 H63B H 0.5364 0.1627 0.3633 0.080 Uiso 0.514(4) 1 calc PR B 4 C64B C 0.3209(18) 0.1820(6) 0.3761(6) 0.070(6) Uani 0.514(4) 1 d PG B 4 H64B H 0.3064 0.2268 0.3901 0.080 Uiso 0.514(4) 1 calc PR B 4 C65B C 0.2048(13) 0.1535(9) 0.3714(5) 0.129(12) Uani 0.514(4) 1 d PG B 4 H65B H 0.1126 0.1792 0.3821 0.080 Uiso 0.514(4) 1 calc PR B 4 C66B C 0.2265(13) 0.0866(10) 0.3505(6) 0.085(7) Uani 0.514(4) 1 d PG B 4 H66B H 0.1488 0.0675 0.3474 0.080 Uiso 0.514(4) 1 calc PR B 4 C67B C 0.3643(16) 0.0482(7) 0.3345(5) 0.071(5) Uani 0.514(4) 1 d PG B 4 H67B H 0.3788 0.0034 0.3206 0.080 Uiso 0.514(4) 1 calc PR B 4 C68B C 0.6644(15) -0.0404(6) 0.2874(5) 0.065(6) Uani 0.514(4) 1 d PG B 4 C69B C 0.6012(17) -0.0963(7) 0.3091(5) 0.097(8) Uani 0.514(4) 1 d PG B 4 H69B H 0.5599 -0.0957 0.3433 0.080 Uiso 0.514(4) 1 calc PR B 4 C70B C 0.5998(17) -0.1532(6) 0.2798(7) 0.132(12) Uani 0.514(4) 1 d PG B 4 H70B H 0.5575 -0.1906 0.2944 0.080 Uiso 0.514(4) 1 calc PR B 4 C71B C 0.6615(17) -0.1540(7) 0.2287(7) 0.129(12) Uani 0.514(4) 1 d PG B 4 H71B H 0.6605 -0.1920 0.2091 0.080 Uiso 0.514(4) 1 calc PR B 4 C72B C 0.7247(15) -0.0981(8) 0.2070(5) 0.108(9) Uani 0.514(4) 1 d PG B 4 H72B H 0.7661 -0.0986 0.1728 0.080 Uiso 0.514(4) 1 calc PR B 4 C73B C 0.7262(14) -0.0412(7) 0.2363(5) 0.077(6) Uani 0.514(4) 1 d PG B 4 H73B H 0.7685 -0.0038 0.2217 0.080 Uiso 0.514(4) 1 calc PR B 4 O1B O 0.909(3) 0.2040(13) 0.4968(10) 0.163(7) Uani 0.514(4) 1 d P B 4 C74B C 0.896(3) 0.1158(11) 0.4430(9) 0.094(5) Uani 0.514(4) 1 d P B 4 H74D H 0.9119 0.1525 0.4161 0.080 Uiso 0.514(4) 1 calc PR B 4 H74E H 0.8039 0.1062 0.4411 0.080 Uiso 0.514(4) 1 calc PR B 4 H74F H 0.9690 0.0717 0.4386 0.080 Uiso 0.514(4) 1 calc PR B 4 C75B C 0.899(2) 0.1419(14) 0.4941(10) 0.089(5) Uani 0.514(4) 1 d P B 4 C76B C 0.892(3) 0.0880(13) 0.5386(11) 0.133(8) Uani 0.514(4) 1 d P B 4 H76D H 0.9798 0.0504 0.5373 0.080 Uiso 0.514(4) 1 calc PR B 4 H76E H 0.8133 0.0666 0.5373 0.080 Uiso 0.514(4) 1 calc PR B 4 H76F H 0.8802 0.1116 0.5702 0.080 Uiso 0.514(4) 1 calc PR B 4 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 0.0427(5) 0.0347(5) 0.0287(4) -0.0021(4) 0.0001(4) -0.0142(4) Ni2 0.0429(6) 0.0436(6) 0.0283(4) -0.0065(4) 0.0025(4) -0.0206(4) N1 0.044(4) 0.051(4) 0.031(3) -0.006(3) 0.004(3) -0.026(3) N2 0.042(3) 0.046(4) 0.026(3) -0.002(3) -0.001(3) -0.015(3) N3 0.060(5) 0.110(7) 0.027(3) -0.012(4) 0.004(3) -0.050(5) N4 0.118(7) 0.043(4) 0.040(4) 0.003(3) 0.025(4) -0.001(4) N5 0.058(4) 0.041(4) 0.030(3) -0.002(3) 0.003(3) -0.014(3) N6 0.045(3) 0.042(3) 0.030(3) -0.005(2) 0.002(3) -0.018(3) N7 0.039(3) 0.067(4) 0.031(3) -0.004(3) -0.007(3) -0.020(3) N8 0.040(4) 0.087(5) 0.033(3) -0.015(3) 0.008(3) -0.022(4) N9 0.055(5) 0.165(10) 0.050(4) -0.034(5) -0.003(4) -0.048(6) N10 0.051(4) 0.050(4) 0.035(3) -0.002(3) 0.001(3) -0.022(3) N11 0.039(4) 0.059(5) 0.026(3) -0.009(3) 0.007(2) -0.023(3) N12 0.068(5) 0.067(5) 0.047(4) -0.028(3) 0.019(3) -0.041(4) C1 0.040(5) 0.119(8) 0.036(4) -0.009(5) -0.007(3) -0.036(5) C2 0.050(5) 0.086(7) 0.037(4) -0.010(4) 0.004(4) -0.035(5) C3 0.042(4) 0.062(5) 0.032(4) -0.007(3) -0.006(3) -0.019(4) C4 0.078(7) 0.164(12) 0.039(5) -0.010(6) 0.004(5) -0.080(8) C5 0.041(5) 0.138(11) 0.046(5) -0.007(6) -0.002(4) -0.014(6) C6 0.105(9) 0.166(13) 0.037(5) -0.004(6) 0.017(5) -0.103(9) C7 0.243(19) 0.076(9) 0.058(7) -0.012(6) 0.056(10) -0.105(12) C8 0.160(12) 0.039(5) 0.056(6) 0.005(4) 0.027(7) -0.026(7) C9 0.221(15) 0.038(5) 0.060(6) 0.001(5) 0.049(8) -0.014(7) C10 0.113(10) 0.096(9) 0.074(7) 0.023(6) 0.006(7) 0.037(8) C11 0.049(5) 0.064(5) 0.031(4) -0.003(4) -0.005(3) -0.008(4) C12 0.083(7) 0.048(5) 0.046(5) 0.004(4) 0.003(4) -0.009(5) C13 0.065(5) 0.055(5) 0.033(4) 0.000(3) 0.006(4) -0.021(4) C14 0.068(6) 0.061(5) 0.027(4) -0.006(3) 0.013(4) -0.025(4) C15 0.062(5) 0.062(5) 0.035(4) -0.008(4) 0.012(4) -0.030(4) C16 0.058(5) 0.048(5) 0.042(4) -0.008(3) 0.009(4) -0.020(4) C17 0.043(5) 0.082(7) 0.045(5) -0.012(4) -0.003(4) -0.007(4) Ni1A 0.0408(17) 0.0317(19) 0.0333(18) -0.0077(13) 0.0027(12) -0.0130(15) Ni2A 0.056(2) 0.0337(11) 0.0318(14) -0.0036(9) 0.0022(11) -0.0041(13) N1A 0.040(7) 0.035(6) 0.032(8) 0.002(6) -0.009(5) -0.007(5) N2A 0.041(7) 0.051(8) 0.039(7) 0.001(6) -0.005(6) -0.015(6) N3A 0.075(10) 0.059(9) 0.036(8) -0.009(6) 0.009(6) -0.025(7) N5A 0.100(11) 0.043(8) 0.038(7) -0.010(6) 0.005(7) -0.032(8) N6A 0.061(8) 0.056(7) 0.033(6) -0.005(5) -0.005(6) -0.012(6) N10A 0.066(10) 0.029(8) 0.084(13) -0.018(9) 0.023(9) -0.005(8) N11A 0.078(15) 0.047(13) 0.065(13) 0.022(11) 0.009(11) -0.023(11) N12A 0.14(2) 0.044(10) 0.033(12) -0.011(9) 0.010(12) 0.018(12) C1A 0.048(8) 0.065(10) 0.067(10) -0.003(8) -0.006(7) -0.021(7) C2A 0.043(8) 0.056(10) 0.044(8) -0.011(8) -0.007(7) -0.001(7) C3A 0.042(9) 0.049(9) 0.049(9) -0.006(7) 0.010(7) -0.022(7) C4A 0.068(15) 0.053(13) 0.057(11) -0.007(11) -0.008(10) 0.002(10) C5A 0.098(13) 0.063(10) 0.049(9) -0.001(7) -0.028(9) -0.026(10) C6A 0.130(17) 0.052(10) 0.037(9) 0.002(7) -0.001(9) -0.027(11) C11A 0.066(9) 0.069(10) 0.055(8) -0.013(7) 0.015(7) -0.036(8) C12A 0.090(13) 0.081(12) 0.045(8) -0.011(8) 0.011(8) -0.043(10) C13A 0.129(16) 0.073(11) 0.054(9) -0.009(8) 0.013(10) -0.068(12) C14A 0.098(13) 0.062(10) 0.044(8) -0.007(7) 0.017(8) -0.031(10) C15A 0.104(16) 0.041(13) 0.043(10) -0.010(8) 0.000(10) -0.010(10) C16A 0.09(2) 0.13(2) 0.045(13) -0.007(13) -0.024(14) 0.010(17) C17A 0.080(11) 0.054(9) 0.046(8) -0.018(6) 0.011(8) -0.020(9) Ni1B 0.068(6) 0.036(4) 0.033(3) -0.004(2) -0.003(4) 0.005(4) Ni2B 0.054(3) 0.0289(17) 0.039(2) -0.0023(15) -0.0061(19) 0.000(2) N1B 0.063(14) 0.026(11) 0.032(14) 0.002(11) -0.019(11) -0.017(10) N2B 0.038(11) 0.034(10) 0.041(12) -0.006(9) -0.004(9) -0.008(8) N3B 0.11(3) 0.020(11) 0.026(14) -0.011(9) -0.015(18) 0.008(16) N5B 0.066(14) 0.029(10) 0.086(16) -0.017(10) -0.017(12) -0.008(10) N6B 0.06(2) 0.035(11) 0.025(12) -0.002(9) -0.003(12) -0.013(14) N10B 0.11(3) 0.037(14) 0.027(10) 0.010(10) 0.022(14) 0.016(17) N11B 0.08(2) 0.025(14) 0.023(11) -0.003(9) 0.013(14) 0.014(14) N12B 0.15(4) 0.017(12) 0.027(13) 0.001(10) -0.041(19) 0.013(18) C1B 0.060(19) 0.06(2) 0.10(3) -0.01(2) -0.025(17) -0.024(17) C2B 0.049(16) 0.026(11) 0.083(19) -0.012(13) -0.023(15) -0.011(10) C3B 0.068(18) 0.033(12) 0.070(18) -0.003(11) -0.003(14) -0.012(12) C4B 0.057(18) 0.040(17) 0.08(2) -0.009(16) -0.039(16) 0.009(13) C5B 0.11(3) 0.12(3) 0.07(2) -0.05(2) -0.03(2) -0.02(2) C6B 0.18(4) 0.041(16) 0.028(14) 0.001(12) 0.011(19) 0.03(2) C11B 0.065(18) 0.08(2) 0.12(3) 0.04(2) -0.028(18) -0.017(16) C12B 0.12(3) 0.07(2) 0.12(3) 0.01(2) -0.03(3) -0.07(2) C13B 0.08(2) 0.040(14) 0.079(18) 0.014(13) 0.007(16) -0.028(14) C14B 0.11(3) 0.029(17) 0.10(3) 0.016(19) 0.02(3) -0.019(17) C15B 0.09(2) 0.034(12) 0.035(12) 0.005(9) 0.010(12) 0.012(12) C16B 0.060(17) 0.073(18) 0.048(14) 0.004(12) 0.006(13) 0.007(15) C17B 0.057(15) 0.037(12) 0.042(12) -0.015(9) -0.001(11) -0.003(11) N104 0.048(4) 0.039(4) 0.059(4) -0.009(3) 0.006(3) -0.011(3) N107 0.044(4) 0.040(4) 0.047(4) -0.005(3) -0.002(3) 0.006(3) N108 0.059(5) 0.066(5) 0.065(5) -0.012(4) -0.013(4) 0.007(4) N109 0.058(6) 0.121(9) 0.151(10) -0.041(7) -0.018(6) 0.025(6) C107 0.235(17) 0.032(5) 0.051(6) 0.004(4) -0.024(8) -0.024(8) C108 0.123(9) 0.050(6) 0.076(7) -0.024(5) 0.054(7) -0.045(6) C109 0.064(7) 0.049(6) 0.251(17) -0.036(8) -0.057(9) -0.007(5) C110 0.089(7) 0.037(4) 0.043(4) -0.012(3) 0.006(4) -0.010(4) B1 0.039(5) 0.037(4) 0.027(4) 0.007(3) -0.009(3) -0.014(4) C20 0.038(4) 0.035(4) 0.027(3) -0.006(3) -0.004(3) -0.010(3) C21 0.038(4) 0.039(4) 0.045(4) 0.007(3) -0.006(3) -0.014(3) C22 0.061(6) 0.047(5) 0.056(5) 0.010(4) -0.017(4) -0.015(4) C23 0.057(6) 0.039(5) 0.062(5) -0.008(4) -0.024(4) 0.004(4) C24 0.042(5) 0.051(5) 0.047(4) -0.015(4) -0.010(4) 0.002(4) C25 0.036(4) 0.055(5) 0.029(3) -0.007(3) -0.001(3) -0.013(4) C26 0.048(4) 0.042(4) 0.028(3) -0.002(3) -0.006(3) -0.002(3) C27 0.046(5) 0.050(5) 0.040(4) -0.009(4) -0.001(3) -0.017(4) C28 0.079(7) 0.076(7) 0.047(5) -0.024(5) -0.001(5) -0.008(5) C29 0.142(11) 0.073(8) 0.072(7) -0.041(6) -0.022(7) 0.031(7) C30 0.248(18) 0.048(6) 0.059(7) -0.010(5) -0.043(9) 0.019(9) C31 0.159(11) 0.044(5) 0.040(5) -0.007(4) -0.027(6) -0.008(6) C32 0.031(4) 0.039(4) 0.035(4) 0.005(3) -0.007(3) -0.010(3) C33 0.042(4) 0.037(4) 0.033(4) -0.001(3) -0.001(3) -0.012(3) C34 0.045(5) 0.054(5) 0.036(4) 0.004(3) -0.001(3) -0.015(4) C35 0.049(5) 0.077(6) 0.046(5) 0.023(4) -0.011(4) -0.027(5) C36 0.075(7) 0.131(10) 0.066(6) 0.041(6) -0.032(5) -0.076(7) C37 0.076(6) 0.105(8) 0.043(5) 0.030(5) -0.030(4) -0.062(6) C38 0.032(4) 0.044(4) 0.027(3) 0.000(3) 0.005(3) -0.010(3) C39 0.043(5) 0.052(5) 0.040(4) 0.012(3) -0.005(3) -0.012(4) C40 0.034(4) 0.070(6) 0.043(4) 0.013(4) -0.010(3) -0.013(4) C41 0.042(5) 0.092(7) 0.035(4) 0.007(4) -0.006(3) -0.035(5) C42 0.054(5) 0.076(6) 0.035(4) -0.007(4) 0.003(4) -0.035(5) C43 0.038(4) 0.058(5) 0.036(4) -0.006(4) 0.003(3) -0.016(4) C50 0.077(7) 0.030(5) 0.082(7) 0.008(4) 0.014(5) 0.010(5) C51 0.113(9) 0.051(6) 0.049(5) -0.001(4) -0.014(5) -0.006(6) C52 0.104(8) 0.043(5) 0.068(6) -0.014(5) -0.008(6) -0.020(5) C53 0.083(7) 0.042(5) 0.052(5) -0.007(4) 0.013(5) -0.004(5) C54 0.090(8) 0.046(5) 0.056(5) 0.005(4) -0.001(5) 0.023(5) C55 0.063(6) 0.048(6) 0.098(8) 0.005(5) 0.002(6) 0.006(5) B2A 0.040(12) 0.052(13) 0.048(12) -0.013(11) -0.012(9) -0.017(10) C56A 0.038(8) 0.030(8) 0.045(9) -0.002(7) -0.015(7) -0.006(7) C57A 0.070(12) 0.030(8) 0.050(10) -0.002(7) -0.013(8) -0.006(8) C58A 0.058(11) 0.041(10) 0.065(11) -0.025(9) -0.028(9) 0.011(8) C59A 0.050(10) 0.064(11) 0.033(8) -0.017(8) -0.008(7) -0.018(9) C60A 0.025(10) 0.059(14) 0.064(13) 0.020(11) -0.002(9) 0.002(9) C61A 0.046(13) 0.026(10) 0.069(16) 0.000(10) -0.013(11) -0.008(9) C62A 0.066(15) 0.059(16) 0.045(11) 0.023(10) -0.017(11) -0.039(13) C63A 0.037(12) 0.08(2) 0.056(15) 0.017(13) -0.010(10) -0.004(14) C64A 0.07(2) 0.19(4) 0.10(2) 0.07(2) -0.041(16) -0.05(2) C65A 0.057(12) 0.20(3) 0.122(16) 0.08(2) -0.050(11) -0.047(16) C66A 0.12(2) 0.20(3) 0.067(14) 0.060(18) -0.030(15) -0.14(2) C67A 0.107(17) 0.097(17) 0.053(11) 0.035(11) -0.042(12) -0.066(15) C68A 0.078(12) 0.035(8) 0.033(8) 0.007(6) -0.010(8) -0.034(8) C69A 0.055(11) 0.046(10) 0.039(9) 0.000(8) 0.002(8) -0.011(9) C70A 0.061(12) 0.082(16) 0.062(13) 0.029(12) 0.014(10) -0.010(11) C71A 0.16(3) 0.089(18) 0.053(13) -0.028(12) 0.046(15) -0.078(19) C72A 0.16(2) 0.053(13) 0.065(13) -0.026(10) -0.011(15) -0.035(15) C73A 0.088(15) 0.025(9) 0.075(13) -0.003(9) -0.026(11) -0.017(9) O1A 0.167(15) 0.132(13) 0.213(17) -0.046(13) -0.067(13) -0.043(12) C74A 0.126(14) 0.049(9) 0.109(13) -0.019(8) 0.027(11) -0.039(9) C75A 0.067(10) 0.088(12) 0.106(13) -0.028(10) 0.001(9) -0.006(9) C76A 0.151(19) 0.061(11) 0.16(2) 0.007(12) 0.037(15) -0.014(12) B2B 0.10(2) 0.026(10) 0.052(13) -0.001(9) -0.032(14) -0.016(11) C56B 0.061(11) 0.043(10) 0.065(11) 0.013(9) -0.027(9) -0.013(8) C57B 0.072(17) 0.045(12) 0.069(12) -0.015(10) -0.007(12) -0.019(11) C58B 0.09(2) 0.11(2) 0.10(2) 0.02(2) -0.06(2) -0.053(17) C59B 0.101(16) 0.047(10) 0.061(11) 0.004(9) -0.034(11) -0.025(11) C60B 0.077(12) 0.035(9) 0.080(12) 0.002(8) -0.038(10) -0.015(8) C61B 0.067(12) 0.044(10) 0.067(11) -0.001(8) -0.033(9) -0.013(9) C62B 0.073(16) 0.039(14) 0.063(15) 0.011(11) -0.030(12) -0.030(13) C63B 0.089(18) 0.057(13) 0.063(13) -0.011(10) 0.005(12) -0.046(12) C64B 0.084(16) 0.062(13) 0.055(11) 0.005(10) 0.005(10) -0.010(11) C65B 0.057(12) 0.20(3) 0.122(16) 0.08(2) -0.050(11) -0.047(16) C66B 0.072(17) 0.12(2) 0.067(14) 0.012(14) -0.013(11) -0.025(14) C67B 0.086(15) 0.076(13) 0.055(11) -0.017(10) -0.029(10) -0.011(12) C68B 0.098(15) 0.037(10) 0.069(12) -0.002(8) -0.056(12) -0.008(10) C69B 0.14(2) 0.043(12) 0.116(18) 0.006(12) -0.043(16) -0.037(13) C70B 0.19(3) 0.077(17) 0.11(2) -0.043(16) -0.03(2) 0.025(18) C71B 0.14(2) 0.037(12) 0.21(3) -0.068(16) -0.09(2) 0.042(14) C72B 0.106(19) 0.078(16) 0.15(2) -0.065(16) -0.055(17) 0.010(14) C73B 0.080(14) 0.066(13) 0.083(14) -0.028(11) -0.032(11) 0.006(11) O1B 0.167(15) 0.132(13) 0.213(17) -0.046(13) -0.067(13) -0.043(12) C74B 0.126(14) 0.049(9) 0.109(13) -0.019(8) 0.027(11) -0.039(9) C75B 0.067(10) 0.088(12) 0.106(13) -0.028(10) 0.001(9) -0.006(9) C76B 0.151(19) 0.061(11) 0.16(2) 0.007(12) 0.037(15) -0.014(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N1 1.925(6) . ? Ni1 N10 2.013(6) . ? Ni1 N4 2.047(7) . ? Ni1 N7 2.132(6) . ? Ni1 N3 2.169(7) . ? Ni2 N2 1.922(6) . ? Ni2 N12 2.033(7) 2_666 ? Ni2 N6 2.044(6) . ? Ni2 N7 2.133(6) . ? Ni2 N5 2.161(6) . ? N1 C2 1.335(10) . ? N1 N2 1.360(7) . ? N2 C3 1.338(9) . ? N3 C5 1.490(13) . ? N3 C6 1.498(12) . ? N3 C4 1.513(11) . ? N4 C10 1.465(15) . ? N4 C9 1.484(12) . ? N4 C8 1.485(12) . ? N5 C12 1.477(10) . ? N5 C11 1.494(10) . ? N5 C13 1.502(9) . ? N6 C16 1.477(9) . ? N6 C15 1.496(8) . ? N6 C17 1.499(9) . ? N7 N8 1.212(9) . ? N8 N9 1.152(10) . ? N10 N11 1.185(9) . ? N11 N12 1.167(9) . ? N12 Ni2 2.033(7) 2_666 ? C1 C3 1.380(11) . ? C1 C2 1.387(11) . ? C2 C4 1.502(11) . ? C3 C11 1.503(10) . ? C6 C7 1.515(18) . ? C7 C8 1.475(19) . ? C13 C14 1.510(11) . ? C14 C15 1.508(11) . ? Ni1A N1A 1.913(12) . ? Ni1A N104 2.008(13) . ? Ni1A N10A 2.030(13) . ? Ni1A N107 2.108(10) . ? Ni1A N3A 2.179(14) . ? Ni2A N2A 1.947(13) . ? Ni2A N12A 2.00(2) 2_655 ? Ni2A N6A 2.064(11) . ? Ni2A N5A 2.160(13) . ? Ni2A N107 2.186(8) . ? N1A N2A 1.327(15) . ? N1A C2A 1.368(16) . ? N2A C3A 1.340(16) . ? N3A C5A 1.450(17) . ? N3A C6A 1.478(19) . ? N3A C4A 1.51(2) . ? N5A C11A 1.469(18) . ? N5A C13A 1.479(17) . ? N5A C12A 1.509(18) . ? N6A C16A 1.46(3) . ? N6A C17A 1.489(16) . ? N6A C15A 1.53(2) . ? N10A N11A 1.186(15) . ? N11A N12A 1.162(15) . ? N12A Ni2A 2.00(2) 2_655 ? C1A C2A 1.370(19) . ? C1A C3A 1.42(2) . ? C2A C4A 1.50(2) . ? C3A C11A 1.488(18) . ? C6A C107 1.508(16) . ? C13A C14A 1.53(2) . ? C14A C15A 1.48(3) . ? Ni1B N1B 1.909(16) . ? Ni1B N10B 2.030(17) . ? Ni1B N104 2.12(2) . ? Ni1B N107 2.120(15) . ? Ni1B N3B 2.187(18) . ? Ni2B N2B 1.945(15) . ? Ni2B N12B 2.01(3) 2_655 ? Ni2B N107 2.013(8) . ? Ni2B N6B 2.07(2) . ? Ni2B N5B 2.154(17) . ? Ni1 Ni2 3.645(1) . ? Ni1 Ni1 6.927(2) 2_666 ? Ni1 Ni2 5.478(1) 2_666 ? Ni2 Ni2 6.214(2) 2_666 ? Ni1A Ni2A 3.627(8) . ? Ni1A Ni1A 6.82(2) 2_655 ? Ni1A Ni2A 5.538(11) 2_655 ? Ni2A Ni2A 6.414(6) 2_655 ? Ni1B Ni2B 3.604(14) . ? Ni1B Ni1B 6.91(4) 2_655 ? Ni1B Ni2B 5.567(19) 2_655 ? Ni2B Ni2B 6.336(11) 2_655 ? Ni1A Ni2B 3.712(10) . ? Ni1A Ni1B 6.862(8) 2_655 ? Ni1A Ni2B 5.435(12) 2_655 ? Ni2A Ni1B 5.686(18) 2_655 ? Ni2A Ni2B 6.345(4) 2_655 ? N1B N2B 1.329(18) . ? N1B C2B 1.372(19) . ? N2B C3B 1.34(2) . ? N3B C5B 1.45(2) . ? N3B C6B 1.50(2) . ? N3B C4B 1.51(3) . ? N5B C11B 1.48(2) . ? N5B C13B 1.49(2) . ? N5B C12B 1.50(2) . ? N6B C16B 1.47(3) . ? N6B C17B 1.49(2) . ? N6B C15B 1.53(2) . ? N10B N11B 1.177(18) . ? N11B N12B 1.159(18) . ? N12B Ni2B 2.01(3) 2_655 ? C1B C2B 1.38(2) . ? C1B C3B 1.42(3) . ? C2B C4B 1.51(3) . ? C3B C11B 1.49(2) . ? C6B C107 1.529(17) . ? C13B C14B 1.53(3) . ? C14B C15B 1.48(4) . ? N104 C109 1.467(12) . ? N104 C110 1.471(10) . ? N104 C108 1.511(11) . ? N107 N108 1.202(9) . ? N108 N109 1.151(11) . ? C107 C108 1.513(17) . ? B1 C32 1.632(9) . ? B1 C38 1.632(10) . ? B1 C26 1.649(11) . ? B1 C20 1.656(10) . ? C20 C25 1.405(10) . ? C20 C21 1.413(9) . ? C21 C22 1.382(10) . ? C22 C23 1.381(12) . ? C23 C24 1.350(12) . ? C24 C25 1.398(10) . ? C26 C31 1.389(11) . ? C26 C27 1.393(10) . ? C27 C28 1.380(11) . ? C28 C29 1.407(15) . ? C29 C30 1.366(16) . ? C30 C31 1.379(14) . ? C32 C37 1.390(10) . ? C32 C33 1.396(9) . ? C33 C34 1.396(9) . ? C34 C35 1.345(11) . ? C35 C36 1.365(12) . ? C36 C37 1.397(11) . ? C38 C43 1.385(11) . ? C38 C39 1.409(10) . ? C39 C40 1.407(11) . ? C40 C41 1.360(12) . ? C41 C42 1.385(12) . ? C42 C43 1.399(11) . ? C50 C51 1.355(14) . ? C50 C55 1.397(13) . ? C50 B2A 1.66(2) . ? C50 B2B 1.76(3) . ? C51 C52 1.406(14) . ? C52 C53 1.363(13) . ? C53 C54 1.340(14) . ? C54 C55 1.403(13) . ? B2A C56A 1.65(3) . ? B2A C62A 1.70(2) . ? B2A C68A 1.71(2) . ? C56A C57A 1.3899 . ? C56A C61A 1.3901 . ? C57A C58A 1.3903 . ? C58A C59A 1.3897 . ? C59A C60A 1.3900 . ? C60A C61A 1.3898 . ? C62A C63A 1.3898 . ? C62A C67A 1.3901 . ? C63A C64A 1.3899 . ? C64A C65A 1.3902 . ? C65A C66A 1.3901 . ? C66A C67A 1.3901 . ? C68A C73A 1.3899 . ? C68A C69A 1.3901 . ? C69A C70A 1.3900 . ? C70A C71A 1.3902 . ? C71A C72A 1.3901 . ? C72A C73A 1.3900 . ? O1A C75A 1.187(11) . ? C74A C75A 1.444(11) . ? C75A C76A 1.436(11) . ? B2B C56B 1.65(2) . ? B2B C62B 1.71(3) . ? B2B C68B 1.71(2) . ? C56B C57B 1.3898 . ? C56B C61B 1.3899 . ? C57B C58B 1.3900 . ? C58B C59B 1.3900 . ? C59B C60B 1.3901 . ? C60B C61B 1.3897 . ? C62B C63B 1.3899 . ? C62B C67B 1.3901 . ? C63B C64B 1.3902 . ? C64B C65B 1.3901 . ? C65B C66B 1.3900 . ? C66B C67B 1.3900 . ? C68B C69B 1.3899 . ? C68B C73B 1.3900 . ? C69B C70B 1.3901 . ? C70B C71B 1.3902 . ? C71B C72B 1.3899 . ? C72B C73B 1.3897 . ? O1B C75B 1.21(3) . ? C74B C75B 1.48(3) . ? C75B C76B 1.46(3) . ? 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 N1 Ni1 N10 154.8(3) . . ? N1 Ni1 N4 111.5(3) . . ? N10 Ni1 N4 93.2(3) . . ? N1 Ni1 N7 84.6(2) . . ? N10 Ni1 N7 94.4(2) . . ? N4 Ni1 N7 103.5(3) . . ? N1 Ni1 N3 78.7(2) . . ? N10 Ni1 N3 93.9(3) . . ? N4 Ni1 N3 97.8(4) . . ? N7 Ni1 N3 156.6(3) . . ? N2 Ni2 N12 162.8(3) . 2_666 ? N2 Ni2 N6 104.4(2) . . ? N12 Ni2 N6 92.5(3) 2_666 . ? N2 Ni2 N7 84.6(2) . . ? N12 Ni2 N7 95.0(3) 2_666 . ? N6 Ni2 N7 103.4(2) . . ? N2 Ni2 N5 79.2(2) . . ? N12 Ni2 N5 95.6(3) 2_666 . ? N6 Ni2 N5 96.7(2) . . ? N7 Ni2 N5 156.8(2) . . ? C2 N1 N2 107.2(6) . . ? C2 N1 Ni1 122.8(5) . . ? N2 N1 Ni1 126.4(5) . . ? C3 N2 N1 108.7(6) . . ? C3 N2 Ni2 121.9(5) . . ? N1 N2 Ni2 126.4(4) . . ? C5 N3 C6 110.1(8) . . ? C5 N3 C4 109.1(8) . . ? C6 N3 C4 109.9(7) . . ? C5 N3 Ni1 102.5(5) . . ? C6 N3 Ni1 115.9(6) . . ? C4 N3 Ni1 109.0(5) . . ? C10 N4 C9 109.5(10) . . ? C10 N4 C8 106.5(9) . . ? C9 N4 C8 109.8(9) . . ? C10 N4 Ni1 109.4(7) . . ? C9 N4 Ni1 110.2(6) . . ? C8 N4 Ni1 111.3(6) . . ? C12 N5 C11 107.6(6) . . ? C12 N5 C13 108.9(6) . . ? C11 N5 C13 111.0(6) . . ? C12 N5 Ni2 106.2(5) . . ? C11 N5 Ni2 109.0(4) . . ? C13 N5 Ni2 113.8(5) . . ? C16 N6 C15 109.3(6) . . ? C16 N6 C17 107.8(6) . . ? C15 N6 C17 106.2(6) . . ? C16 N6 Ni2 112.2(5) . . ? C15 N6 Ni2 112.4(5) . . ? C17 N6 Ni2 108.8(5) . . ? N8 N7 Ni1 120.9(5) . . ? N8 N7 Ni2 118.6(5) . . ? Ni1 N7 Ni2 117.4(3) . . ? N9 N8 N7 178.5(9) . . ? N11 N10 Ni1 125.0(5) . . ? N12 N11 N10 175.1(7) . . ? N11 N12 Ni2 136.0(6) . 2_666 ? C3 C1 C2 104.2(7) . . ? N1 C2 C1 110.3(7) . . ? N1 C2 C4 113.0(7) . . ? C1 C2 C4 136.6(8) . . ? N2 C3 C1 109.5(6) . . ? N2 C3 C11 113.5(6) . . ? C1 C3 C11 136.9(7) . . ? C2 C4 N3 108.1(7) . . ? N3 C6 C7 113.0(8) . . ? C8 C7 C6 116.0(10) . . ? C7 C8 N4 116.9(10) . . ? N5 C11 C3 108.5(6) . . ? N5 C13 C14 113.7(6) . . ? C15 C14 C13 117.4(7) . . ? N6 C15 C14 114.8(6) . . ? N1A Ni1A N104 106.6(6) . . ? N1A Ni1A N10A 159.4(9) . . ? N104 Ni1A N10A 93.6(6) . . ? N1A Ni1A N107 86.4(5) . . ? N104 Ni1A N107 109.0(5) . . ? N10A Ni1A N107 91.0(7) . . ? N1A Ni1A N3A 79.3(6) . . ? N104 Ni1A N3A 94.7(6) . . ? N10A Ni1A N3A 95.2(7) . . ? N107 Ni1A N3A 155.1(7) . . ? N2A Ni2A N12A 157.3(7) . 2_655 ? N2A Ni2A N6A 108.9(5) . . ? N12A Ni2A N6A 93.5(7) 2_655 . ? N2A Ni2A N5A 78.9(5) . . ? N12A Ni2A N5A 94.6(11) 2_655 . ? N6A Ni2A N5A 98.6(5) . . ? N2A Ni2A N107 84.6(4) . . ? N12A Ni2A N107 94.8(11) 2_655 . ? N6A Ni2A N107 101.3(4) . . ? N5A Ni2A N107 157.4(4) . . ? N2A N1A C2A 107.7(12) . . ? N2A N1A Ni1A 127.2(9) . . ? C2A N1A Ni1A 121.8(11) . . ? N1A N2A C3A 110.4(13) . . ? N1A N2A Ni2A 125.9(8) . . ? C3A N2A Ni2A 119.8(11) . . ? C5A N3A C6A 108.9(11) . . ? C5A N3A C4A 109.1(17) . . ? C6A N3A C4A 110.7(15) . . ? C5A N3A Ni1A 104.9(10) . . ? C6A N3A Ni1A 114.9(12) . . ? C4A N3A Ni1A 108.0(10) . . ? C11A N5A C13A 109.7(12) . . ? C11A N5A C12A 109.0(13) . . ? C13A N5A C12A 107.6(10) . . ? C11A N5A Ni2A 110.0(8) . . ? C13A N5A Ni2A 115.3(12) . . ? C12A N5A Ni2A 105.0(9) . . ? C16A N6A C17A 108.6(18) . . ? C16A N6A C15A 109.2(17) . . ? C17A N6A C15A 108.3(12) . . ? C16A N6A Ni2A 109.9(15) . . ? C17A N6A Ni2A 108.8(9) . . ? C15A N6A Ni2A 111.9(10) . . ? N11A N10A Ni1A 125.9(16) . . ? N12A N11A N10A 176(3) . . ? N11A N12A Ni2A 141(2) . 2_655 ? C2A C1A C3A 104.7(12) . . ? N1A C2A C1A 109.5(14) . . ? N1A C2A C4A 112.9(13) . . ? C1A C2A C4A 137.6(14) . . ? N2A C3A C1A 107.7(12) . . ? N2A C3A C11A 114.9(14) . . ? C1A C3A C11A 137.4(13) . . ? C2A C4A N3A 108.1(11) . . ? N3A C6A C107 107.1(11) . . ? N5A C11A C3A 108.4(11) . . ? N5A C13A C14A 111.9(11) . . ? C15A C14A C13A 116.9(15) . . ? C14A C15A N6A 116.4(15) . . ? N1B Ni1B N10B 161.7(16) . . ? N1B Ni1B N104 103.5(11) . . ? N10B Ni1B N104 94.5(11) . . ? N1B Ni1B N107 82.2(7) . . ? N10B Ni1B N107 96.7(9) . . ? N104 Ni1B N107 104.5(7) . . ? N1B Ni1B N3B 80.1(9) . . ? N10B Ni1B N3B 94.4(11) . . ? N104 Ni1B N3B 97.4(9) . . ? N107 Ni1B N3B 154.5(10) . . ? N2B Ni2B N12B 160.7(12) . 2_655 ? N2B Ni2B N107 83.1(5) . . ? N12B Ni2B N107 98.3(18) 2_655 . ? N2B Ni2B N6B 108.1(9) . . ? N12B Ni2B N6B 90.5(11) 2_655 . ? N107 Ni2B N6B 102.4(7) . . ? N2B Ni2B N5B 79.3(6) . . ? N12B Ni2B N5B 92.9(19) 2_655 . ? N107 Ni2B N5B 155.4(6) . . ? N6B Ni2B N5B 99.3(9) . . ? N2B N1B C2B 107.9(15) . . ? N2B N1B Ni1B 126.4(13) . . ? C2B N1B Ni1B 121.1(16) . . ? N1B N2B C3B 110.9(16) . . ? N1B N2B Ni2B 125.9(12) . . ? C3B N2B Ni2B 120.0(12) . . ? C5B N3B C6B 114(2) . . ? C5B N3B C4B 106(2) . . ? C6B N3B C4B 112.7(19) . . ? C5B N3B Ni1B 104.6(16) . . ? C6B N3B Ni1B 110.8(17) . . ? C4B N3B Ni1B 108.3(13) . . ? C11B N5B C13B 109.5(17) . . ? C11B N5B C12B 109(2) . . ? C13B N5B C12B 109.6(17) . . ? C11B N5B Ni2B 109.1(11) . . ? C13B N5B Ni2B 114.0(14) . . ? C12B N5B Ni2B 105.1(15) . . ? C16B N6B C17B 110(2) . . ? C16B N6B C15B 108(2) . . ? C17B N6B C15B 108.5(18) . . ? C16B N6B Ni2B 110.6(17) . . ? C17B N6B Ni2B 110.0(16) . . ? C15B N6B Ni2B 109.8(15) . . ? N11B N10B Ni1B 127(3) . . ? N12B N11B N10B 171(4) . . ? N11B N12B Ni2B 143(3) . 2_655 ? C2B C1B C3B 105.5(18) . . ? N1B C2B C1B 108.6(18) . . ? N1B C2B C4B 114.0(17) . . ? C1B C2B C4B 137.3(19) . . ? N2B C3B C1B 106.9(17) . . ? N2B C3B C11B 114.5(18) . . ? C1B C3B C11B 138.2(19) . . ? C2B C4B N3B 108.7(16) . . ? N3B C6B C107 123.0(16) . . ? N5B C11B C3B 108.3(16) . . ? N5B C13B C14B 115.0(17) . . ? C15B C14B C13B 117(3) . . ? C14B C15B N6B 118(2) . . ? C109 N104 C110 108.0(8) . . ? C109 N104 C108 110.3(8) . . ? C110 N104 C108 108.5(6) . . ? C109 N104 Ni1A 105.3(6) . . ? C110 N104 Ni1A 113.6(6) . . ? C108 N104 Ni1A 111.0(6) . . ? C109 N104 Ni1B 109.8(7) . . ? C110 N104 Ni1B 107.0(6) . . ? C108 N104 Ni1B 113.0(7) . . ? Ni1A N104 Ni1B 6.8(6) . . ? N108 N107 Ni2B 112.1(6) . . ? N108 N107 Ni1A 118.8(6) . . ? Ni2B N107 Ni1A 128.5(4) . . ? N108 N107 Ni1B 125.7(7) . . ? Ni2B N107 Ni1B 121.3(5) . . ? Ni1A N107 Ni1B 7.2(5) . . ? N108 N107 Ni2A 122.5(6) . . ? Ni2B N107 Ni2A 16.16(15) . . ? Ni1A N107 Ni2A 115.3(4) . . ? Ni1B N107 Ni2A 108.0(4) . . ? N109 N108 N107 178.4(12) . . ? C6A C107 C108 105.4(12) . . ? C6A C107 C6B 32.7(11) . . ? C108 C107 C6B 123.2(12) . . ? N104 C108 C107 115.9(8) . . ? C32 B1 C38 109.9(5) . . ? C32 B1 C26 110.0(6) . . ? C38 B1 C26 108.2(6) . . ? C32 B1 C20 110.4(6) . . ? C38 B1 C20 109.1(6) . . ? C26 B1 C20 109.2(5) . . ? C25 C20 C21 114.1(6) . . ? C25 C20 B1 124.1(6) . . ? C21 C20 B1 121.8(6) . . ? C22 C21 C20 122.7(7) . . ? C23 C22 C21 120.9(8) . . ? C24 C23 C22 118.5(7) . . ? C23 C24 C25 121.3(7) . . ? C24 C25 C20 122.5(7) . . ? C31 C26 C27 114.4(7) . . ? C31 C26 B1 122.3(6) . . ? C27 C26 B1 123.2(6) . . ? C28 C27 C26 123.3(8) . . ? C27 C28 C29 119.9(9) . . ? C30 C29 C28 117.6(10) . . ? C29 C30 C31 120.9(10) . . ? C30 C31 C26 123.6(9) . . ? C37 C32 C33 113.5(6) . . ? C37 C32 B1 121.9(6) . . ? C33 C32 B1 124.5(6) . . ? C34 C33 C32 122.9(7) . . ? C35 C34 C33 120.9(7) . . ? C34 C35 C36 119.2(7) . . ? C35 C36 C37 119.6(8) . . ? C32 C37 C36 123.8(8) . . ? C43 C38 C39 114.6(7) . . ? C43 C38 B1 123.7(6) . . ? C39 C38 B1 121.6(7) . . ? C40 C39 C38 122.0(8) . . ? C41 C40 C39 120.6(8) . . ? C40 C41 C42 119.8(8) . . ? C41 C42 C43 118.6(8) . . ? C38 C43 C42 124.4(8) . . ? C51 C50 C55 114.3(9) . . ? C51 C50 B2A 109.2(11) . . ? C55 C50 B2A 136.4(13) . . ? C51 C50 B2B 135.5(12) . . ? C55 C50 B2B 109.7(13) . . ? B2A C50 B2B 28.1(8) . . ? C50 C51 C52 123.8(10) . . ? C53 C52 C51 119.9(11) . . ? C54 C53 C52 118.6(9) . . ? C53 C54 C55 121.0(9) . . ? C50 C55 C54 122.3(11) . . ? C56A B2A C50 123.1(15) . . ? C56A B2A C62A 104.0(13) . . ? C50 B2A C62A 104.0(14) . . ? C56A B2A C68A 111.5(14) . . ? C50 B2A C68A 98.8(12) . . ? C62A B2A C68A 116.0(15) . . ? C57A C56A C61A 120.0 . . ? C57A C56A B2A 124.7(10) . . ? C61A C56A B2A 115.3(10) . . ? C56A C57A C58A 120.0 . . ? C59A C58A C57A 120.0 . . ? C58A C59A C60A 120.0 . . ? C61A C60A C59A 120.0 . . ? C60A C61A C56A 120.0 . . ? C63A C62A C67A 120.0 . . ? C63A C62A B2A 118.4(11) . . ? C67A C62A B2A 120.6(11) . . ? C62A C63A C64A 120.0 . . ? C63A C64A C65A 120.0 . . ? C66A C65A C64A 120.0 . . ? C67A C66A C65A 120.0 . . ? C62A C67A C66A 120.0 . . ? C73A C68A C69A 120.0 . . ? C73A C68A B2A 122.1(10) . . ? C69A C68A B2A 117.8(10) . . ? C70A C69A C68A 120.0 . . ? C69A C70A C71A 120.0 . . ? C72A C71A C70A 120.0 . . ? C73A C72A C71A 120.0 . . ? C68A C73A C72A 120.0 . . ? O1A C75A C76A 117.9(10) . . ? O1A C75A C74A 118.1(10) . . ? C76A C75A C74A 124.0(13) . . ? C56B B2B C62B 110.0(15) . . ? C56B B2B C68B 108.8(12) . . ? C62B B2B C68B 111.7(18) . . ? C56B B2B C50 106.4(17) . . ? C62B B2B C50 105.3(11) . . ? C68B B2B C50 114.5(15) . . ? C57B C56B C61B 120.0 . . ? C57B C56B B2B 122.0(12) . . ? C61B C56B B2B 118.0(12) . . ? C56B C57B C58B 120.0 . . ? C57B C58B C59B 120.0 . . ? C58B C59B C60B 120.0 . . ? C61B C60B C59B 120.0 . . ? C60B C61B C56B 120.0 . . ? C63B C62B C67B 120.0 . . ? C63B C62B B2B 117.3(12) . . ? C67B C62B B2B 122.5(12) . . ? C62B C63B C64B 120.0 . . ? C65B C64B C63B 120.0 . . ? C66B C65B C64B 120.0 . . ? C65B C66B C67B 120.0 . . ? C66B C67B C62B 120.0 . . ? C69B C68B C73B 120.0 . . ? C69B C68B B2B 116.3(11) . . ? C73B C68B B2B 123.6(11) . . ? C68B C69B C70B 120.0 . . ? C69B C70B C71B 120.0 . . ? C72B C71B C70B 120.0 . . ? C73B C72B C71B 120.0 . . ? C72B C73B C68B 120.0 . . ? O1B C75B C76B 125(3) . . ? O1B C75B C74B 120(3) . . ? C76B C75B C74B 115(2) . . ? 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 N10 N12 Ni2 -89.6(7) . . . 2_666 ? Ni1A N10A N12A Ni2A -90(3) . . . 2_655 ? Ni1B N10B N12B Ni2B -72(7) . . . 2_655 ? Ni1A N10A N12A Ni2B -64(4) . . . 2_655 ? Ni1B N10B N12B Ni2A -83(5) . . . 2_655 ? Ni1B N10A N12A Ni2B -65(4) . . . 2_655 ? Ni1A N10B N12B Ni2A -77(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.760 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.760 _refine_diff_density_max 0.871 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.083