Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email smpeng@mail.ch.ntu.edu.tw _publ_contact_author_name 'Prof Shie-Ming Peng' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Shie-Ming Peng' 'Gene-Hsiang Lee' 'Ting-Bin Tsao' 'Chen-Yu Yeh' data_ic8997 _database_code_CSD 199616 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 N14 Ni3 O4' _chemical_formula_weight 1101.11 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.5862(1) _cell_length_b 16.1383(1) _cell_length_c 18.2700(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.0389(4) _cell_angle_gamma 90.00 _cell_volume 4764.30(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33878 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10901 _reflns_number_gt 8040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0697P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0123(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10901 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.165 _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 0.30415(2) 0.30759(2) 0.168238(18) 0.01946(11) Uani 1 1 d . . . Ni2 Ni 0.43984(2) 0.26783(2) 0.152742(17) 0.01716(11) Uani 1 1 d . . . Ni3 Ni 0.57672(2) 0.22568(2) 0.140235(18) 0.01987(11) Uani 1 1 d . . . O1 O 0.18634(12) 0.34073(12) 0.16471(11) 0.0286(4) Uani 1 1 d . . . O2 O 0.16440(13) 0.35939(15) 0.27970(12) 0.0394(5) Uani 1 1 d . . . O3 O 0.68364(12) 0.19029(12) 0.11434(11) 0.0288(5) Uani 1 1 d . . . O4 O 0.79110(13) 0.20215(14) 0.21240(12) 0.0371(5) Uani 1 1 d . . . N1 N 0.32121(13) 0.40108(13) 0.09316(11) 0.0196(5) Uani 1 1 d . . . N2 N 0.46207(13) 0.37731(13) 0.12627(12) 0.0198(5) Uani 1 1 d . . . N3 N 0.60279(13) 0.35066(14) 0.16217(12) 0.0212(5) Uani 1 1 d . . . N4 N 0.31939(14) 0.20695(14) 0.24136(12) 0.0224(5) Uani 1 1 d . . . N5 N 0.41869(13) 0.15889(13) 0.18000(12) 0.0197(5) Uani 1 1 d . . . N6 N 0.52342(14) 0.10788(14) 0.12690(12) 0.0235(5) Uani 1 1 d . . . N7 N 0.26578(14) 0.22605(14) 0.07874(12) 0.0216(5) Uani 1 1 d . . . N8 N 0.39409(13) 0.24105(14) 0.05065(12) 0.0195(5) Uani 1 1 d . . . N9 N 0.52427(14) 0.25129(14) 0.02516(12) 0.0209(5) Uani 1 1 d . . . N10 N 0.37073(14) 0.38048(14) 0.25281(12) 0.0220(5) Uani 1 1 d . . . N11 N 0.48277(13) 0.29399(13) 0.25470(12) 0.0198(5) Uani 1 1 d . . . N12 N 0.59426(14) 0.20756(14) 0.25529(12) 0.0222(5) Uani 1 1 d . . . N13 N -0.11706(19) 0.3880(2) 0.1124(2) 0.0630(10) Uani 1 1 d . . . N14 N 0.9293(3) 0.1583(3) 0.0002(3) 0.0794(12) Uani 1 1 d . . . C1 C 0.25536(17) 0.44089(17) 0.05144(14) 0.0232(6) Uani 1 1 d . . . H1A H 0.2017 0.4227 0.0543 0.028 Uiso 1 1 calc R . . C2 C 0.26144(18) 0.50637(18) 0.00496(15) 0.0272(6) Uani 1 1 d . . . H2A H 0.2133 0.5327 -0.0237 0.033 Uiso 1 1 calc R . . C3 C 0.33987(18) 0.53290(17) 0.00102(15) 0.0278(6) Uani 1 1 d . . . H3A H 0.3463 0.5781 -0.0306 0.033 Uiso 1 1 calc R . . C4 C 0.40834(18) 0.49350(18) 0.04308(15) 0.0261(6) Uani 1 1 d . . . H4A H 0.4623 0.5120 0.0415 0.031 Uiso 1 1 calc R . . C5 C 0.39816(16) 0.42578(16) 0.08845(14) 0.0204(6) Uani 1 1 d . . . C6 C 0.54129(16) 0.40768(17) 0.15268(14) 0.0217(6) Uani 1 1 d . . . C7 C 0.55906(18) 0.49091(18) 0.17492(16) 0.0277(6) Uani 1 1 d . . . H7A H 0.5157 0.5305 0.1687 0.033 Uiso 1 1 calc R . . C8 C 0.63901(18) 0.51431(19) 0.20538(18) 0.0338(7) Uani 1 1 d . . . H8A H 0.6516 0.5703 0.2196 0.041 Uiso 1 1 calc R . . C9 C 0.70172(19) 0.4549(2) 0.21527(19) 0.0366(7) Uani 1 1 d . . . H9A H 0.7576 0.4696 0.2362 0.044 Uiso 1 1 calc R . . C10 C 0.68097(17) 0.37508(18) 0.19425(16) 0.0287(6) Uani 1 1 d . . . H10A H 0.7236 0.3345 0.2026 0.034 Uiso 1 1 calc R . . C11 C 0.27967(19) 0.20181(19) 0.29797(16) 0.0295(7) Uani 1 1 d . . . H11A H 0.2424 0.2450 0.3031 0.035 Uiso 1 1 calc R . . C12 C 0.2901(2) 0.1378(2) 0.34852(17) 0.0356(7) Uani 1 1 d . . . H12A H 0.2599 0.1359 0.3869 0.043 Uiso 1 1 calc R . . C13 C 0.34621(19) 0.07573(19) 0.34198(16) 0.0332(7) Uani 1 1 d . . . H13A H 0.3546 0.0303 0.3760 0.040 Uiso 1 1 calc R . . C14 C 0.38935(18) 0.08031(18) 0.28622(16) 0.0285(6) Uani 1 1 d . . . H14A H 0.4286 0.0388 0.2820 0.034 Uiso 1 1 calc R . . C15 C 0.37498(16) 0.14677(16) 0.23544(14) 0.0214(6) Uani 1 1 d . . . C16 C 0.45206(17) 0.09284(17) 0.14920(14) 0.0221(6) Uani 1 1 d . . . C17 C 0.41273(18) 0.01556(17) 0.13624(16) 0.0278(6) Uani 1 1 d . . . H17A H 0.3610 0.0067 0.1490 0.033 Uiso 1 1 calc R . . C18 C 0.4494(2) -0.04678(19) 0.10513(17) 0.0350(7) Uani 1 1 d . . . H18A H 0.4237 -0.0996 0.0968 0.042 Uiso 1 1 calc R . . C19 C 0.5244(2) -0.0326(2) 0.08577(19) 0.0390(8) Uani 1 1 d . . . H19A H 0.5518 -0.0759 0.0659 0.047 Uiso 1 1 calc R . . C20 C 0.55789(19) 0.04508(18) 0.09598(17) 0.0311(7) Uani 1 1 d . . . H20A H 0.6079 0.0553 0.0805 0.037 Uiso 1 1 calc R . . C21 C 0.33805(18) 0.45019(18) 0.27443(16) 0.0300(7) Uani 1 1 d . . . H21A H 0.2830 0.4645 0.2500 0.036 Uiso 1 1 calc R . . C22 C 0.3798(2) 0.5014(2) 0.32960(19) 0.0431(8) Uani 1 1 d . . . H22A H 0.3541 0.5493 0.3443 0.052 Uiso 1 1 calc R . . C23 C 0.4617(2) 0.4812(2) 0.36392(19) 0.0449(9) Uani 1 1 d . . . H23A H 0.4925 0.5153 0.4027 0.054 Uiso 1 1 calc R . . C24 C 0.49702(19) 0.41205(19) 0.34124(16) 0.0326(7) Uani 1 1 d . . . H24A H 0.5529 0.3985 0.3635 0.039 Uiso 1 1 calc R . . C25 C 0.45065(16) 0.36135(17) 0.28530(14) 0.0214(6) Uani 1 1 d . . . C26 C 0.54588(16) 0.24659(17) 0.29582(14) 0.0221(6) Uani 1 1 d . . . C27 C 0.55768(19) 0.23323(18) 0.37347(16) 0.0298(7) Uani 1 1 d . . . H27A H 0.5233 0.2601 0.4013 0.036 Uiso 1 1 calc R . . C28 C 0.6195(2) 0.1808(2) 0.40858(17) 0.0368(7) Uani 1 1 d . . . H28A H 0.6294 0.1726 0.4613 0.044 Uiso 1 1 calc R . . C29 C 0.6679(2) 0.1397(2) 0.36702(17) 0.0368(8) Uani 1 1 d . . . H29A H 0.7104 0.1026 0.3905 0.044 Uiso 1 1 calc R . . C30 C 0.65251(18) 0.15417(18) 0.29124(16) 0.0285(6) Uani 1 1 d . . . H30A H 0.6845 0.1251 0.2625 0.034 Uiso 1 1 calc R . . C31 C 0.19196(17) 0.18742(18) 0.06926(15) 0.0261(6) Uani 1 1 d . . . H31A H 0.1575 0.2009 0.1026 0.031 Uiso 1 1 calc R . . C32 C 0.16396(18) 0.12981(19) 0.01433(16) 0.0309(7) Uani 1 1 d . . . H32A H 0.1113 0.1044 0.0093 0.037 Uiso 1 1 calc R . . C33 C 0.21498(18) 0.1097(2) -0.03391(16) 0.0323(7) Uani 1 1 d . . . H33A H 0.1976 0.0701 -0.0727 0.039 Uiso 1 1 calc R . . C34 C 0.29060(18) 0.14767(18) -0.02517(16) 0.0285(6) Uani 1 1 d . . . H34A H 0.3256 0.1346 -0.0582 0.034 Uiso 1 1 calc R . . C35 C 0.31631(16) 0.20612(17) 0.03300(15) 0.0211(6) Uani 1 1 d . . . C36 C 0.44103(17) 0.25240(16) -0.00138(15) 0.0207(6) Uani 1 1 d . . . C37 C 0.40690(18) 0.26967(18) -0.07807(15) 0.0265(6) Uani 1 1 d . . . H37A H 0.3486 0.2727 -0.0961 0.032 Uiso 1 1 calc R . . C38 C 0.45864(19) 0.28200(18) -0.12644(16) 0.0297(7) Uani 1 1 d . . . H38A H 0.4362 0.2917 -0.1783 0.036 Uiso 1 1 calc R . . C39 C 0.5436(2) 0.28016(18) -0.09880(17) 0.0306(7) Uani 1 1 d . . . H39A H 0.5804 0.2884 -0.1312 0.037 Uiso 1 1 calc R . . C40 C 0.57329(19) 0.26601(17) -0.02314(16) 0.0260(6) Uani 1 1 d . . . H40A H 0.6315 0.2667 -0.0039 0.031 Uiso 1 1 calc R . . C41 C 0.14269(18) 0.35421(18) 0.21034(17) 0.0292(7) Uani 1 1 d . . . C42 C -0.0605(2) 0.3872(3) 0.0703(2) 0.0650(12) Uani 1 1 d . . . H42A H -0.0793 0.3952 0.0177 0.078 Uiso 1 1 calc R . . C43 C 0.0227(2) 0.3756(2) 0.09838(19) 0.0463(9) Uani 1 1 d . . . H43A H 0.0599 0.3747 0.0658 0.056 Uiso 1 1 calc R . . C44 C 0.05116(18) 0.36541(18) 0.17473(17) 0.0315(7) Uani 1 1 d . . . C45 C -0.00615(19) 0.3660(2) 0.2190(2) 0.0370(7) Uani 1 1 d . . . H45A H 0.0107 0.3585 0.2718 0.044 Uiso 1 1 calc R . . C46 C -0.0886(2) 0.3778(2) 0.1849(2) 0.0492(9) Uani 1 1 d . . . H46A H -0.1274 0.3786 0.2160 0.059 Uiso 1 1 calc R . . C47 C 0.75961(19) 0.18961(18) 0.14558(17) 0.0296(7) Uani 1 1 d . . . C48 C 0.8474(3) 0.1503(3) -0.0268(3) 0.0754(14) Uani 1 1 d . . . H48A H 0.8280 0.1393 -0.0789 0.090 Uiso 1 1 calc R . . C49 C 0.7894(2) 0.1572(3) 0.0174(2) 0.0541(10) Uani 1 1 d . . . H49A H 0.7320 0.1506 -0.0039 0.065 Uiso 1 1 calc R . . C50 C 0.81763(19) 0.1739(2) 0.09296(19) 0.0354(7) Uani 1 1 d . . . C51 C 0.9019(2) 0.1804(2) 0.1203(2) 0.0507(10) Uani 1 1 d . . . H51A H 0.9238 0.1902 0.1723 0.061 Uiso 1 1 calc R . . C52 C 0.9539(3) 0.1726(3) 0.0722(3) 0.0731(15) Uani 1 1 d . . . H52A H 1.0116 0.1780 0.0925 0.088 Uiso 1 1 calc R . . 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 0.01661(19) 0.0216(2) 0.02036(19) 0.00027(14) 0.00468(13) 0.00151(14) Ni2 0.01576(19) 0.01738(19) 0.01790(18) 0.00011(13) 0.00286(13) 0.00065(13) Ni3 0.01635(19) 0.0211(2) 0.02200(19) 0.00043(14) 0.00399(14) 0.00211(14) O1 0.0254(11) 0.0288(11) 0.0314(11) 0.0018(9) 0.0060(9) 0.0027(9) O2 0.0330(12) 0.0518(14) 0.0331(12) -0.0033(11) 0.0069(9) 0.0093(11) O3 0.0213(11) 0.0340(12) 0.0331(11) -0.0019(9) 0.0099(9) 0.0037(9) O4 0.0284(12) 0.0447(13) 0.0360(13) 0.0048(10) 0.0025(10) 0.0042(10) N1 0.0188(11) 0.0205(11) 0.0193(11) -0.0025(9) 0.0040(9) 0.0020(9) N2 0.0159(11) 0.0196(11) 0.0232(11) 0.0010(9) 0.0029(9) 0.0013(9) N3 0.0170(11) 0.0227(12) 0.0235(11) 0.0022(10) 0.0037(9) 0.0004(9) N4 0.0206(12) 0.0245(12) 0.0225(11) 0.0002(10) 0.0060(9) 0.0002(10) N5 0.0187(11) 0.0177(11) 0.0225(11) 0.0002(9) 0.0041(9) 0.0002(9) N6 0.0225(12) 0.0230(12) 0.0244(11) -0.0002(10) 0.0042(9) 0.0031(10) N7 0.0173(12) 0.0244(12) 0.0229(12) 0.0015(9) 0.0041(9) 0.0002(9) N8 0.0167(11) 0.0221(12) 0.0196(11) -0.0006(9) 0.0040(9) 0.0006(9) N9 0.0193(12) 0.0203(11) 0.0239(12) -0.0011(9) 0.0065(9) 0.0011(9) N10 0.0238(12) 0.0226(12) 0.0203(11) 0.0005(9) 0.0066(9) 0.0028(10) N11 0.0188(12) 0.0207(11) 0.0192(11) 0.0003(9) 0.0031(9) 0.0021(9) N12 0.0194(12) 0.0216(12) 0.0243(12) 0.0026(9) 0.0020(9) 0.0034(9) N13 0.0287(17) 0.080(3) 0.079(2) 0.025(2) 0.0100(16) 0.0182(17) N14 0.069(3) 0.077(3) 0.113(4) -0.005(3) 0.065(3) 0.010(2) C1 0.0197(14) 0.0259(14) 0.0224(13) -0.0047(11) 0.0018(11) 0.0052(11) C2 0.0283(16) 0.0267(15) 0.0240(14) -0.0002(12) 0.0003(11) 0.0091(12) C3 0.0381(17) 0.0215(14) 0.0232(14) 0.0039(12) 0.0059(12) 0.0026(13) C4 0.0269(15) 0.0246(14) 0.0277(14) 0.0036(12) 0.0081(12) 0.0002(12) C5 0.0210(14) 0.0214(13) 0.0191(13) -0.0013(11) 0.0050(10) 0.0010(11) C6 0.0208(14) 0.0235(14) 0.0214(13) 0.0031(11) 0.0063(11) -0.0025(11) C7 0.0249(15) 0.0226(14) 0.0343(16) 0.0003(12) 0.0040(12) 0.0006(12) C8 0.0283(16) 0.0232(15) 0.0483(19) -0.0024(14) 0.0048(14) -0.0035(13) C9 0.0207(15) 0.0320(17) 0.055(2) -0.0033(15) 0.0040(14) -0.0050(13) C10 0.0199(15) 0.0295(16) 0.0351(16) 0.0014(13) 0.0028(12) -0.0015(12) C11 0.0301(16) 0.0321(16) 0.0287(15) 0.0005(13) 0.0117(13) 0.0008(13) C12 0.0400(19) 0.0394(18) 0.0317(16) 0.0075(14) 0.0168(14) 0.0011(15) C13 0.0401(18) 0.0285(16) 0.0320(16) 0.0081(13) 0.0102(13) -0.0004(14) C14 0.0306(16) 0.0241(15) 0.0323(15) 0.0032(12) 0.0101(12) 0.0004(13) C15 0.0189(14) 0.0215(14) 0.0236(13) -0.0014(11) 0.0041(11) -0.0042(11) C16 0.0247(15) 0.0208(14) 0.0197(13) 0.0000(11) 0.0029(11) 0.0023(11) C17 0.0282(16) 0.0244(15) 0.0304(15) -0.0009(12) 0.0063(12) -0.0018(12) C18 0.0415(19) 0.0224(15) 0.0398(17) -0.0067(13) 0.0062(14) -0.0020(14) C19 0.043(2) 0.0280(16) 0.0471(19) -0.0101(15) 0.0129(15) 0.0090(15) C20 0.0288(16) 0.0293(16) 0.0361(16) -0.0057(13) 0.0090(13) 0.0064(13) C21 0.0279(16) 0.0296(16) 0.0330(16) -0.0035(13) 0.0078(12) 0.0060(13) C22 0.046(2) 0.0347(18) 0.0457(19) -0.0182(16) 0.0049(16) 0.0107(16) C23 0.048(2) 0.0389(19) 0.0414(19) -0.0181(16) -0.0032(15) 0.0033(16) C24 0.0329(17) 0.0315(16) 0.0290(15) -0.0071(13) -0.0022(12) 0.0039(14) C25 0.0215(14) 0.0239(14) 0.0188(13) 0.0025(11) 0.0046(10) 0.0014(11) C26 0.0191(14) 0.0231(14) 0.0219(14) 0.0000(11) 0.0003(11) -0.0015(11) C27 0.0336(17) 0.0323(16) 0.0229(14) 0.0004(12) 0.0052(12) 0.0046(13) C28 0.0388(19) 0.0442(19) 0.0248(15) 0.0093(14) 0.0019(13) 0.0086(15) C29 0.0320(17) 0.0410(18) 0.0343(17) 0.0115(15) 0.0010(13) 0.0122(15) C30 0.0250(15) 0.0289(15) 0.0316(16) 0.0057(13) 0.0064(12) 0.0067(12) C31 0.0197(14) 0.0316(16) 0.0262(14) 0.0039(12) 0.0037(11) -0.0021(12) C32 0.0226(15) 0.0379(18) 0.0301(15) -0.0013(13) 0.0019(12) -0.0080(13) C33 0.0270(16) 0.0364(17) 0.0300(15) -0.0091(14) -0.0009(12) -0.0038(14) C34 0.0230(15) 0.0337(16) 0.0280(15) -0.0065(13) 0.0042(12) 0.0006(13) C35 0.0187(14) 0.0208(13) 0.0228(13) 0.0037(11) 0.0025(11) 0.0020(11) C36 0.0229(15) 0.0175(13) 0.0217(13) -0.0029(11) 0.0052(11) -0.0004(11) C37 0.0233(15) 0.0304(16) 0.0244(14) 0.0018(12) 0.0027(11) 0.0041(12) C38 0.0388(18) 0.0292(16) 0.0210(14) 0.0020(12) 0.0065(12) 0.0047(13) C39 0.0365(18) 0.0303(16) 0.0294(15) 0.0029(13) 0.0168(13) 0.0004(13) C40 0.0263(16) 0.0234(15) 0.0307(15) 0.0003(12) 0.0116(12) 0.0002(12) C41 0.0247(16) 0.0262(15) 0.0352(17) 0.0022(13) 0.0038(13) 0.0044(12) C42 0.037(2) 0.097(4) 0.056(2) 0.031(2) 0.0014(18) 0.019(2) C43 0.0300(18) 0.067(3) 0.0423(19) 0.0096(18) 0.0085(14) 0.0053(17) C44 0.0262(16) 0.0281(16) 0.0404(17) 0.0010(13) 0.0078(13) 0.0049(13) C45 0.0275(17) 0.0370(18) 0.0491(19) -0.0018(15) 0.0142(14) 0.0007(14) C46 0.0270(18) 0.058(2) 0.065(2) 0.000(2) 0.0150(17) 0.0083(17) C47 0.0289(17) 0.0228(15) 0.0378(18) 0.0050(13) 0.0090(13) 0.0056(12) C48 0.080(4) 0.093(4) 0.064(3) -0.007(3) 0.037(3) 0.028(3) C49 0.048(2) 0.070(3) 0.048(2) -0.004(2) 0.0176(18) 0.019(2) C50 0.0281(17) 0.0310(17) 0.051(2) 0.0005(14) 0.0169(15) 0.0052(13) C51 0.0310(19) 0.047(2) 0.079(3) -0.014(2) 0.0226(18) 0.0031(16) C52 0.044(2) 0.064(3) 0.126(5) -0.035(3) 0.050(3) -0.009(2) _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 O1 2.013(2) . ? Ni1 N10 2.054(2) . ? Ni1 N4 2.082(2) . ? Ni1 N7 2.083(2) . ? Ni1 N1 2.101(2) . ? Ni1 Ni2 2.4176(4) . ? Ni2 N5 1.882(2) . ? Ni2 N11 1.886(2) . ? Ni2 N2 1.890(2) . ? Ni2 N8 1.898(2) . ? Ni2 Ni3 2.4297(5) . ? Ni3 O3 2.0183(19) . ? Ni3 N12 2.077(2) . ? Ni3 N3 2.083(2) . ? Ni3 N6 2.088(2) . ? Ni3 N9 2.127(2) . ? O1 C41 1.241(3) . ? O2 C41 1.239(3) . ? O3 C47 1.260(4) . ? O4 C47 1.232(4) . ? N1 C1 1.346(3) . ? N1 C5 1.358(3) . ? N2 C5 1.372(3) . ? N2 C6 1.383(3) . ? N3 C10 1.356(3) . ? N3 C6 1.356(3) . ? N4 C11 1.348(3) . ? N4 C15 1.360(3) . ? N5 C16 1.378(3) . ? N5 C15 1.386(3) . ? N6 C20 1.349(3) . ? N6 C16 1.358(4) . ? N7 C35 1.349(3) . ? N7 C31 1.350(3) . ? N8 C36 1.370(3) . ? N8 C35 1.378(3) . ? N9 C40 1.349(3) . ? N9 C36 1.356(3) . ? N10 C21 1.346(3) . ? N10 C25 1.360(3) . ? N11 C26 1.375(3) . ? N11 C25 1.383(3) . ? N12 C30 1.349(3) . ? N12 C26 1.363(3) . ? N13 C46 1.312(5) . ? N13 C42 1.340(5) . ? N14 C52 1.306(6) . ? N14 C48 1.342(6) . ? C1 C2 1.373(4) . ? C2 C3 1.387(4) . ? C3 C4 1.375(4) . ? C4 C5 1.405(4) . ? C6 C7 1.415(4) . ? C7 C8 1.370(4) . ? C8 C9 1.397(4) . ? C9 C10 1.365(4) . ? C11 C12 1.370(4) . ? C12 C13 1.391(4) . ? C13 C14 1.373(4) . ? C14 C15 1.403(4) . ? C16 C17 1.403(4) . ? C17 C18 1.364(4) . ? C18 C19 1.386(5) . ? C19 C20 1.368(4) . ? C21 C22 1.365(4) . ? C22 C23 1.400(5) . ? C23 C24 1.367(4) . ? C24 C25 1.397(4) . ? C26 C27 1.404(4) . ? C27 C28 1.372(4) . ? C28 C29 1.391(4) . ? C29 C30 1.370(4) . ? C31 C32 1.370(4) . ? C32 C33 1.391(4) . ? C33 C34 1.372(4) . ? C34 C35 1.413(4) . ? C36 C37 1.415(4) . ? C37 C38 1.378(4) . ? C38 C39 1.386(4) . ? C39 C40 1.378(4) . ? C41 C44 1.521(4) . ? C42 C43 1.372(5) . ? C43 C44 1.378(4) . ? C44 C45 1.380(4) . ? C45 C46 1.383(5) . ? C47 C50 1.527(4) . ? C48 C49 1.393(5) . ? C49 C50 1.381(5) . ? C50 C51 1.378(5) . ? C51 C52 1.369(5) . ? 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 O1 Ni1 N10 103.01(8) . . ? O1 Ni1 N4 101.79(8) . . ? N10 Ni1 N4 89.84(9) . . ? O1 Ni1 N7 91.16(8) . . ? N10 Ni1 N7 165.72(9) . . ? N4 Ni1 N7 88.98(9) . . ? O1 Ni1 N1 93.50(8) . . ? N10 Ni1 N1 87.20(8) . . ? N4 Ni1 N1 164.70(8) . . ? N7 Ni1 N1 90.20(8) . . ? O1 Ni1 Ni2 171.66(6) . . ? N10 Ni1 Ni2 83.31(6) . . ? N4 Ni1 Ni2 83.49(6) . . ? N7 Ni1 Ni2 82.42(6) . . ? N1 Ni1 Ni2 81.26(6) . . ? N5 Ni2 N11 89.95(9) . . ? N5 Ni2 N2 179.38(10) . . ? N11 Ni2 N2 89.51(9) . . ? N5 Ni2 N8 89.44(9) . . ? N11 Ni2 N8 178.61(9) . . ? N2 Ni2 N8 91.10(9) . . ? N5 Ni2 Ni1 89.02(7) . . ? N11 Ni2 Ni1 88.79(7) . . ? N2 Ni2 Ni1 91.28(6) . . ? N8 Ni2 Ni1 89.95(7) . . ? N5 Ni2 Ni3 89.85(7) . . ? N11 Ni2 Ni3 90.17(7) . . ? N2 Ni2 Ni3 89.84(6) . . ? N8 Ni2 Ni3 91.08(7) . . ? Ni1 Ni2 Ni3 178.466(19) . . ? O3 Ni3 N12 105.52(8) . . ? O3 Ni3 N3 99.43(8) . . ? N12 Ni3 N3 88.05(9) . . ? O3 Ni3 N6 94.95(8) . . ? N12 Ni3 N6 87.06(9) . . ? N3 Ni3 N6 165.57(9) . . ? O3 Ni3 N9 90.48(8) . . ? N12 Ni3 N9 163.88(9) . . ? N3 Ni3 N9 91.31(8) . . ? N6 Ni3 N9 89.63(9) . . ? O3 Ni3 Ni2 172.04(6) . . ? N12 Ni3 Ni2 82.22(6) . . ? N3 Ni3 Ni2 82.45(6) . . ? N6 Ni3 Ni2 83.44(6) . . ? N9 Ni3 Ni2 81.72(6) . . ? C41 O1 Ni1 137.28(19) . . ? C47 O3 Ni3 137.5(2) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Ni1 120.07(18) . . ? C5 N1 Ni1 121.27(17) . . ? C5 N2 C6 122.6(2) . . ? C5 N2 Ni2 119.25(17) . . ? C6 N2 Ni2 117.83(17) . . ? C10 N3 C6 118.5(2) . . ? C10 N3 Ni3 120.11(18) . . ? C6 N3 Ni3 121.02(17) . . ? C11 N4 C15 118.3(2) . . ? C11 N4 Ni1 122.05(19) . . ? C15 N4 Ni1 119.50(17) . . ? C16 N5 C15 120.9(2) . . ? C16 N5 Ni2 119.90(17) . . ? C15 N5 Ni2 118.99(17) . . ? C20 N6 C16 118.2(2) . . ? C20 N6 Ni3 121.65(19) . . ? C16 N6 Ni3 120.19(18) . . ? C35 N7 C31 118.9(2) . . ? C35 N7 Ni1 120.94(18) . . ? C31 N7 Ni1 120.01(18) . . ? C36 N8 C35 122.7(2) . . ? C36 N8 Ni2 119.18(18) . . ? C35 N8 Ni2 117.96(17) . . ? C40 N9 C36 118.6(2) . . ? C40 N9 Ni3 120.56(19) . . ? C36 N9 Ni3 120.83(17) . . ? C21 N10 C25 118.6(2) . . ? C21 N10 Ni1 121.03(19) . . ? C25 N10 Ni1 120.25(17) . . ? C26 N11 C25 122.1(2) . . ? C26 N11 Ni2 119.10(17) . . ? C25 N11 Ni2 118.77(17) . . ? C30 N12 C26 118.4(2) . . ? C30 N12 Ni3 120.26(19) . . ? C26 N12 Ni3 121.31(17) . . ? C46 N13 C42 116.1(3) . . ? C52 N14 C48 116.6(4) . . ? N1 C1 C2 123.6(3) . . ? C1 C2 C3 118.0(3) . . ? C4 C3 C2 119.6(3) . . ? C3 C4 C5 119.7(3) . . ? N1 C5 N2 115.5(2) . . ? N1 C5 C4 120.4(2) . . ? N2 C5 C4 124.0(2) . . ? N3 C6 N2 115.6(2) . . ? N3 C6 C7 120.4(2) . . ? N2 C6 C7 123.8(2) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C9 119.2(3) . . ? C10 C9 C8 118.6(3) . . ? N3 C10 C9 123.5(3) . . ? N4 C11 C12 123.7(3) . . ? C11 C12 C13 118.0(3) . . ? C14 C13 C12 119.7(3) . . ? C13 C14 C15 119.5(3) . . ? N4 C15 N5 115.7(2) . . ? N4 C15 C14 120.7(2) . . ? N5 C15 C14 123.5(2) . . ? N6 C16 N5 116.2(2) . . ? N6 C16 C17 120.8(2) . . ? N5 C16 C17 122.8(3) . . ? C18 C17 C16 119.5(3) . . ? C17 C18 C19 119.7(3) . . ? C20 C19 C18 118.5(3) . . ? N6 C20 C19 123.3(3) . . ? N10 C21 C22 123.5(3) . . ? C21 C22 C23 118.0(3) . . ? C24 C23 C22 119.5(3) . . ? C23 C24 C25 119.8(3) . . ? N10 C25 N11 115.4(2) . . ? N10 C25 C24 120.5(2) . . ? N11 C25 C24 123.9(2) . . ? N12 C26 N11 115.4(2) . . ? N12 C26 C27 120.9(3) . . ? N11 C26 C27 123.6(3) . . ? C28 C27 C26 119.1(3) . . ? C27 C28 C29 120.1(3) . . ? C30 C29 C28 118.1(3) . . ? N12 C30 C29 123.4(3) . . ? N7 C31 C32 123.7(3) . . ? C31 C32 C33 117.9(3) . . ? C34 C33 C32 119.6(3) . . ? C33 C34 C35 119.9(3) . . ? N7 C35 N8 115.9(2) . . ? N7 C35 C34 120.0(2) . . ? N8 C35 C34 123.8(2) . . ? N9 C36 N8 116.2(2) . . ? N9 C36 C37 120.3(2) . . ? N8 C36 C37 123.4(2) . . ? C38 C37 C36 119.7(3) . . ? C37 C38 C39 119.5(3) . . ? C40 C39 C38 118.2(3) . . ? N9 C40 C39 123.6(3) . . ? O2 C41 O1 128.3(3) . . ? O2 C41 C44 117.4(3) . . ? O1 C41 C44 114.3(3) . . ? N13 C42 C43 124.1(4) . . ? C42 C43 C44 118.8(3) . . ? C43 C44 C45 117.9(3) . . ? C43 C44 C41 121.9(3) . . ? C45 C44 C41 120.2(3) . . ? C44 C45 C46 118.6(3) . . ? N13 C46 C45 124.5(3) . . ? O4 C47 O3 127.2(3) . . ? O4 C47 C50 117.7(3) . . ? O3 C47 C50 115.1(3) . . ? N14 C48 C49 123.6(4) . . ? C50 C49 C48 118.2(4) . . ? C51 C50 C49 117.7(3) . . ? C51 C50 C47 119.4(3) . . ? C49 C50 C47 122.8(3) . . ? C52 C51 C50 119.6(4) . . ? N14 C52 C51 124.3(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.319 data_ic9055 _database_code_CSD 199617 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 N14 Ni3 O4' _chemical_formula_weight 1101.11 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.3803(1) _cell_length_b 16.0704(1) _cell_length_c 18.7595(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.4908(5) _cell_angle_gamma 90.00 _cell_volume 4781.12(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.399 _exptl_absorpt_correction_T_max 0.436 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31983 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10965 _reflns_number_gt 8628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0711P)^2^+3.2787P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0125(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10965 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.003 _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 0.29232(2) 0.20020(2) 0.664958(19) 0.02238(11) Uani 1 1 d . . . Ni2 Ni 0.43013(2) 0.23792(2) 0.649879(18) 0.01846(11) Uani 1 1 d . . . Ni3 Ni 0.56766(2) 0.27855(2) 0.637201(18) 0.02057(11) Uani 1 1 d . . . O1 O 0.17155(14) 0.16749(15) 0.66402(14) 0.0374(5) Uani 1 1 d . . . O2 O 0.1603(2) 0.1471(2) 0.77535(17) 0.0619(8) Uani 1 1 d . . . O3 O 0.67300(13) 0.31056(13) 0.60936(11) 0.0307(5) Uani 1 1 d . . . O4 O 0.79026(15) 0.3153(2) 0.70127(13) 0.0510(7) Uani 1 1 d . . . N1 N 0.30624(14) 0.10622(15) 0.58999(12) 0.0219(5) Uani 1 1 d . . . N2 N 0.45032(14) 0.12867(14) 0.61991(12) 0.0212(5) Uani 1 1 d . . . N3 N 0.59371(14) 0.15361(14) 0.65591(12) 0.0217(5) Uani 1 1 d . . . N4 N 0.31465(15) 0.29884(15) 0.74009(13) 0.0259(5) Uani 1 1 d . . . N5 N 0.41326(15) 0.34664(15) 0.68042(13) 0.0233(5) Uani 1 1 d . . . N6 N 0.51559(15) 0.39716(15) 0.62610(13) 0.0254(5) Uani 1 1 d . . . N7 N 0.36163(16) 0.12268(15) 0.74484(13) 0.0256(5) Uani 1 1 d . . . N8 N 0.47749(15) 0.20667(14) 0.74862(12) 0.0217(5) Uani 1 1 d . . . N9 N 0.59141(15) 0.29298(15) 0.75131(13) 0.0230(5) Uani 1 1 d . . . N10 N 0.25075(15) 0.28438(15) 0.57870(13) 0.0229(5) Uani 1 1 d . . . N11 N 0.38017(14) 0.26940(15) 0.55136(12) 0.0219(5) Uani 1 1 d . . . N12 N 0.50906(15) 0.25222(15) 0.52493(12) 0.0217(5) Uani 1 1 d . . . N13 N -0.0769(4) 0.1161(5) 0.5867(4) 0.059(2) Uiso 0.556(10) 1 d P A 1 N13' N -0.0857(6) 0.1603(7) 0.5614(5) 0.065(3) Uiso 0.444(10) 1 d P A 2 N14 N 0.9324(2) 0.3605(3) 0.5495(2) 0.0764(14) Uani 1 1 d . . . C1 C 0.23724(18) 0.06515(19) 0.55182(15) 0.0259(6) Uani 1 1 d . . . H1A H 0.1837 0.0830 0.5568 0.031 Uiso 1 1 calc R . . C2 C 0.2401(2) -0.0008(2) 0.50632(16) 0.0313(7) Uani 1 1 d . . . H2A H 0.1901 -0.0287 0.4811 0.038 Uiso 1 1 calc R . . C3 C 0.3184(2) -0.02572(19) 0.49812(16) 0.0304(7) Uani 1 1 d . . . H3A H 0.3226 -0.0711 0.4667 0.037 Uiso 1 1 calc R . . C4 C 0.38990(19) 0.01536(19) 0.53553(16) 0.0276(6) Uani 1 1 d . . . H4A H 0.4436 -0.0009 0.5297 0.033 Uiso 1 1 calc R . . C5 C 0.38282(18) 0.08184(17) 0.58259(15) 0.0224(6) Uani 1 1 d . . . C6 C 0.53042(18) 0.09650(17) 0.64411(14) 0.0225(6) Uani 1 1 d . . . C7 C 0.54885(19) 0.01271(19) 0.66354(17) 0.0286(6) Uani 1 1 d . . . H7A H 0.5049 -0.0274 0.6549 0.034 Uiso 1 1 calc R . . C8 C 0.6307(2) -0.0111(2) 0.69503(18) 0.0350(7) Uani 1 1 d . . . H8A H 0.6434 -0.0675 0.7083 0.042 Uiso 1 1 calc R . . C9 C 0.6946(2) 0.0483(2) 0.70730(18) 0.0344(7) Uani 1 1 d . . . H9A H 0.7516 0.0332 0.7286 0.041 Uiso 1 1 calc R . . C10 C 0.67327(18) 0.12912(19) 0.68777(16) 0.0273(6) Uani 1 1 d . . . H10A H 0.7166 0.1699 0.6971 0.033 Uiso 1 1 calc R . . C11 C 0.2785(2) 0.3010(2) 0.79726(18) 0.0379(8) Uani 1 1 d . . . H11A H 0.2389 0.2591 0.8009 0.045 Uiso 1 1 calc R . . C12 C 0.2970(3) 0.3620(3) 0.8507(2) 0.0541(10) Uani 1 1 d . . . H12A H 0.2691 0.3631 0.8894 0.065 Uiso 1 1 calc R . . C13 C 0.3570(3) 0.4213(3) 0.8470(2) 0.0510(10) Uani 1 1 d . . . H13A H 0.3713 0.4630 0.8839 0.061 Uiso 1 1 calc R . . C14 C 0.3956(2) 0.4199(2) 0.79027(18) 0.0362(7) Uani 1 1 d . . . H14A H 0.4369 0.4604 0.7873 0.043 Uiso 1 1 calc R . . C15 C 0.37308(18) 0.35717(18) 0.73619(16) 0.0263(6) Uani 1 1 d . . . C16 C 0.44717(18) 0.41336(18) 0.65131(15) 0.0247(6) Uani 1 1 d . . . C17 C 0.4108(2) 0.4933(2) 0.64366(19) 0.0364(7) Uani 1 1 d . . . H17A H 0.3613 0.5040 0.6599 0.044 Uiso 1 1 calc R . . C18 C 0.4475(2) 0.5555(2) 0.6127(2) 0.0443(9) Uani 1 1 d . . . H18A H 0.4237 0.6097 0.6076 0.053 Uiso 1 1 calc R . . C19 C 0.5188(2) 0.5394(2) 0.5889(2) 0.0468(9) Uani 1 1 d . . . H19A H 0.5458 0.5823 0.5686 0.056 Uiso 1 1 calc R . . C20 C 0.5500(2) 0.4598(2) 0.59542(19) 0.0358(7) Uani 1 1 d . . . H20A H 0.5981 0.4481 0.5775 0.043 Uiso 1 1 calc R . . C21 C 0.3273(2) 0.0515(2) 0.76166(17) 0.0346(7) Uani 1 1 d . . . H21A H 0.2694 0.0411 0.7394 0.042 Uiso 1 1 calc R . . C22 C 0.3718(3) -0.0068(2) 0.8094(2) 0.0425(8) Uani 1 1 d . . . H22A H 0.3455 -0.0563 0.8202 0.051 Uiso 1 1 calc R . . C23 C 0.4560(3) 0.0086(2) 0.84130(19) 0.0419(8) Uani 1 1 d . . . H23A H 0.4880 -0.0302 0.8752 0.050 Uiso 1 1 calc R . . C24 C 0.4937(2) 0.0798(2) 0.82429(16) 0.0323(7) Uani 1 1 d . . . H24A H 0.5518 0.0900 0.8455 0.039 Uiso 1 1 calc R . . C25 C 0.44497(19) 0.13739(18) 0.77498(15) 0.0250(6) Uani 1 1 d . . . C26 C 0.54462(18) 0.25108(18) 0.78984(15) 0.0240(6) Uani 1 1 d . . . C27 C 0.5618(2) 0.2595(2) 0.86677(16) 0.0307(7) Uani 1 1 d . . . H27A H 0.5284 0.2306 0.8935 0.037 Uiso 1 1 calc R . . C28 C 0.6269(2) 0.3095(2) 0.90302(17) 0.0371(8) Uani 1 1 d . . . H28A H 0.6400 0.3140 0.9552 0.045 Uiso 1 1 calc R . . C29 C 0.6737(2) 0.3537(2) 0.86323(18) 0.0365(7) Uani 1 1 d . . . H29A H 0.7183 0.3894 0.8873 0.044 Uiso 1 1 calc R . . C30 C 0.65310(19) 0.34409(19) 0.78771(16) 0.0286(6) Uani 1 1 d . . . H30A H 0.6839 0.3750 0.7600 0.034 Uiso 1 1 calc R . . C31 C 0.17552(18) 0.32295(19) 0.56922(17) 0.0285(6) Uani 1 1 d . . . H31A H 0.1397 0.3065 0.5995 0.034 Uiso 1 1 calc R . . C32 C 0.14790(19) 0.3849(2) 0.51802(17) 0.0315(7) Uani 1 1 d . . . H32A H 0.0942 0.4100 0.5126 0.038 Uiso 1 1 calc R . . C33 C 0.20073(19) 0.4092(2) 0.47470(17) 0.0318(7) Uani 1 1 d . . . H33A H 0.1841 0.4524 0.4395 0.038 Uiso 1 1 calc R . . C34 C 0.27701(19) 0.37070(19) 0.48270(16) 0.0279(6) Uani 1 1 d . . . H34A H 0.3133 0.3869 0.4528 0.034 Uiso 1 1 calc R . . C35 C 0.30200(17) 0.30667(17) 0.53553(15) 0.0223(6) Uani 1 1 d . . . C36 C 0.42468(18) 0.25646(17) 0.49924(15) 0.0214(6) Uani 1 1 d . . . C37 C 0.38620(19) 0.24303(19) 0.42372(16) 0.0270(6) Uani 1 1 d . . . H37A H 0.3267 0.2474 0.4058 0.032 Uiso 1 1 calc R . . C38 C 0.4355(2) 0.22368(19) 0.37663(16) 0.0304(7) Uani 1 1 d . . . H38A H 0.4105 0.2154 0.3257 0.037 Uiso 1 1 calc R . . C39 C 0.5226(2) 0.21621(19) 0.40433(17) 0.0300(7) Uani 1 1 d . . . H39A H 0.5578 0.2018 0.3730 0.036 Uiso 1 1 calc R . . C40 C 0.55591(19) 0.23029(18) 0.47794(16) 0.0258(6) Uani 1 1 d . . . H40A H 0.6151 0.2243 0.4970 0.031 Uiso 1 1 calc R . . C41 C 0.1354(3) 0.1554(2) 0.7054(2) 0.0482(10) Uani 1 1 d . A . C43 C 0.0379(3) 0.1498(3) 0.6771(3) 0.0537(11) Uani 1 1 d . . . C42 C 0.0040(4) 0.1292(5) 0.6114(4) 0.0400(17) Uiso 0.556(10) 1 d P A 1 H42A H 0.0390 0.1229 0.5783 0.048 Uiso 0.556(10) 1 calc PR A 1 C44 C -0.0084(5) 0.1527(4) 0.7335(4) 0.0350(16) Uiso 0.556(10) 1 d P A 1 H44A H 0.0181 0.1625 0.7839 0.042 Uiso 0.556(10) 1 calc PR A 1 C45 C -0.0942(5) 0.1401(5) 0.7078(5) 0.043(2) Uiso 0.556(10) 1 d P A 1 H45A H -0.1321 0.1448 0.7385 0.052 Uiso 0.556(10) 1 calc PR A 1 C46 C -0.1184(6) 0.1217(6) 0.6402(5) 0.058(2) Uiso 0.556(10) 1 d P A 1 H46A H -0.1769 0.1096 0.6240 0.070 Uiso 0.556(10) 1 calc PR A 1 C42' C -0.0025(6) 0.1630(7) 0.5890(6) 0.050(3) Uiso 0.444(10) 1 d P A 2 H42B H 0.0336 0.1726 0.5573 0.060 Uiso 0.444(10) 1 calc PR A 2 C44' C -0.0277(9) 0.1483(8) 0.7062(8) 0.068(4) Uiso 0.444(10) 1 d P A 2 H44B H -0.0111 0.1424 0.7582 0.082 Uiso 0.444(10) 1 calc PR A 2 C45' C -0.1099(7) 0.1529(7) 0.6815(7) 0.048(3) Uiso 0.444(10) 1 d P A 2 H45B H -0.1469 0.1553 0.7132 0.058 Uiso 0.444(10) 1 calc PR A 2 C46' C -0.1361(6) 0.1538(6) 0.6124(5) 0.043(2) Uiso 0.444(10) 1 d P A 2 H46B H -0.1953 0.1497 0.5926 0.051 Uiso 0.444(10) 1 calc PR A 2 C47 C 0.7507(2) 0.3218(2) 0.63591(18) 0.0328(7) Uani 1 1 d . . . C48 C 0.8856(2) 0.3466(3) 0.5975(2) 0.0657(14) Uani 1 1 d . . . H48A H 0.9140 0.3400 0.6479 0.079 Uiso 1 1 calc R . . C49 C 0.7986(2) 0.3412(2) 0.57821(18) 0.0361(7) Uani 1 1 d . . . C50 C 0.7580(2) 0.3517(2) 0.50440(19) 0.0395(8) Uani 1 1 d . . . H50A H 0.6982 0.3498 0.4887 0.047 Uiso 1 1 calc R . . C51 C 0.8053(3) 0.3649(3) 0.4541(2) 0.0496(10) Uani 1 1 d . . . H51A H 0.7789 0.3716 0.4033 0.060 Uiso 1 1 calc R . . C52 C 0.8912(3) 0.3680(3) 0.4793(2) 0.0601(12) Uani 1 1 d . . . H52A H 0.9234 0.3762 0.4442 0.072 Uiso 1 1 calc R . . 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 0.0217(2) 0.0230(2) 0.0241(2) -0.00114(14) 0.00884(14) -0.00257(14) Ni2 0.01940(19) 0.01725(19) 0.01874(19) 0.00031(13) 0.00476(13) -0.00070(13) Ni3 0.01958(19) 0.02029(19) 0.02186(19) 0.00050(13) 0.00520(14) -0.00234(13) O1 0.0256(12) 0.0346(13) 0.0483(14) -0.0142(11) 0.0020(10) -0.0004(10) O2 0.070(2) 0.0612(19) 0.0619(19) 0.0083(15) 0.0311(16) -0.0031(16) O3 0.0247(11) 0.0357(12) 0.0333(11) 0.0027(9) 0.0102(9) -0.0059(9) O4 0.0329(13) 0.087(2) 0.0332(13) -0.0085(13) 0.0084(10) -0.0122(13) N1 0.0236(12) 0.0207(12) 0.0232(11) -0.0007(9) 0.0092(9) -0.0027(9) N2 0.0212(11) 0.0190(11) 0.0246(12) -0.0006(9) 0.0081(9) -0.0009(9) N3 0.0224(12) 0.0207(12) 0.0219(11) -0.0012(9) 0.0052(9) 0.0013(9) N4 0.0287(13) 0.0244(13) 0.0263(12) -0.0020(10) 0.0101(10) 0.0014(10) N5 0.0229(12) 0.0197(12) 0.0266(12) 0.0002(9) 0.0051(9) 0.0003(9) N6 0.0256(12) 0.0225(12) 0.0272(12) 0.0021(10) 0.0048(10) -0.0031(10) N7 0.0332(14) 0.0233(12) 0.0239(12) 0.0002(9) 0.0136(10) -0.0036(10) N8 0.0245(12) 0.0219(12) 0.0185(11) 0.0010(9) 0.0052(9) 0.0011(9) N9 0.0225(12) 0.0229(12) 0.0238(12) -0.0009(9) 0.0061(9) 0.0006(10) N10 0.0212(12) 0.0239(12) 0.0227(11) -0.0036(9) 0.0037(9) -0.0010(9) N11 0.0190(12) 0.0243(12) 0.0216(11) 0.0003(9) 0.0038(9) -0.0018(9) N12 0.0228(12) 0.0191(11) 0.0231(12) 0.0010(9) 0.0057(9) -0.0025(9) N14 0.044(2) 0.138(4) 0.055(2) -0.028(2) 0.0271(17) -0.036(2) C1 0.0248(14) 0.0282(15) 0.0245(14) 0.0027(11) 0.0058(11) -0.0027(12) C2 0.0290(16) 0.0337(17) 0.0290(15) -0.0055(13) 0.0031(12) -0.0084(13) C3 0.0366(17) 0.0289(16) 0.0254(15) -0.0073(12) 0.0071(12) -0.0027(13) C4 0.0293(15) 0.0272(15) 0.0283(15) -0.0062(12) 0.0111(12) -0.0020(12) C5 0.0262(14) 0.0195(13) 0.0223(13) 0.0012(11) 0.0077(11) -0.0033(11) C6 0.0274(14) 0.0225(14) 0.0189(13) -0.0009(10) 0.0085(11) 0.0015(11) C7 0.0314(16) 0.0206(14) 0.0352(16) -0.0012(12) 0.0109(13) -0.0006(12) C8 0.0407(18) 0.0233(16) 0.0398(18) 0.0026(13) 0.0079(14) 0.0078(13) C9 0.0285(16) 0.0342(17) 0.0364(17) -0.0001(14) 0.0008(13) 0.0083(13) C10 0.0228(14) 0.0293(16) 0.0292(15) -0.0035(12) 0.0058(12) -0.0003(12) C11 0.044(2) 0.0388(19) 0.0370(18) -0.0051(14) 0.0211(15) 0.0005(15) C12 0.070(3) 0.058(3) 0.047(2) -0.0164(19) 0.036(2) -0.003(2) C13 0.065(3) 0.045(2) 0.047(2) -0.0232(17) 0.0216(19) -0.0034(19) C14 0.0404(18) 0.0285(17) 0.0410(18) -0.0099(14) 0.0124(15) -0.0020(14) C15 0.0242(14) 0.0244(15) 0.0293(15) -0.0009(12) 0.0046(11) 0.0047(12) C16 0.0235(14) 0.0206(14) 0.0274(14) -0.0002(11) 0.0014(11) -0.0010(11) C17 0.0329(17) 0.0259(16) 0.049(2) 0.0036(14) 0.0080(15) 0.0030(13) C18 0.043(2) 0.0211(16) 0.065(2) 0.0079(16) 0.0076(17) 0.0031(15) C19 0.050(2) 0.0271(18) 0.065(2) 0.0129(16) 0.0177(19) -0.0058(16) C20 0.0339(17) 0.0296(17) 0.0445(19) 0.0100(14) 0.0106(14) -0.0056(14) C21 0.0452(19) 0.0294(16) 0.0343(17) 0.0008(13) 0.0194(14) -0.0086(14) C22 0.060(2) 0.0287(18) 0.0438(19) 0.0094(15) 0.0222(17) -0.0065(16) C23 0.062(2) 0.0295(17) 0.0375(18) 0.0151(14) 0.0192(17) 0.0103(16) C24 0.0404(18) 0.0329(17) 0.0247(15) 0.0042(12) 0.0098(13) 0.0069(14) C25 0.0335(16) 0.0228(14) 0.0210(13) -0.0005(11) 0.0108(12) 0.0023(12) C26 0.0240(14) 0.0243(14) 0.0218(14) 0.0001(11) 0.0022(11) 0.0056(11) C27 0.0338(17) 0.0338(17) 0.0240(14) 0.0020(12) 0.0062(12) 0.0010(13) C28 0.0400(18) 0.0424(19) 0.0251(15) -0.0067(14) 0.0011(13) -0.0001(15) C29 0.0300(17) 0.0405(19) 0.0350(18) -0.0104(14) 0.0006(13) -0.0026(14) C30 0.0267(15) 0.0298(16) 0.0286(15) -0.0062(12) 0.0059(12) -0.0015(12) C31 0.0232(14) 0.0303(16) 0.0317(15) -0.0092(12) 0.0067(12) -0.0004(12) C32 0.0255(15) 0.0329(17) 0.0320(16) -0.0078(13) -0.0002(12) 0.0067(13) C33 0.0311(16) 0.0280(16) 0.0308(15) 0.0014(12) -0.0023(12) 0.0026(13) C34 0.0275(15) 0.0257(15) 0.0283(15) 0.0021(12) 0.0027(12) -0.0018(12) C35 0.0212(14) 0.0203(14) 0.0230(13) -0.0017(10) 0.0012(11) -0.0022(11) C36 0.0257(14) 0.0174(13) 0.0217(13) 0.0033(10) 0.0068(11) -0.0024(11) C37 0.0258(15) 0.0278(15) 0.0256(14) 0.0004(12) 0.0028(12) -0.0048(12) C38 0.0417(18) 0.0273(16) 0.0226(14) -0.0018(12) 0.0087(13) -0.0070(13) C39 0.0365(17) 0.0270(15) 0.0303(16) -0.0031(12) 0.0154(13) -0.0029(13) C40 0.0268(15) 0.0233(15) 0.0302(15) -0.0002(11) 0.0123(12) -0.0019(12) C41 0.061(3) 0.0239(17) 0.050(2) -0.0002(16) -0.004(2) -0.0089(17) C43 0.048(2) 0.043(2) 0.080(3) -0.020(2) 0.034(2) -0.0122(18) C47 0.0282(16) 0.0379(18) 0.0339(17) -0.0070(14) 0.0110(13) -0.0087(14) C48 0.032(2) 0.123(4) 0.046(2) -0.023(2) 0.0161(17) -0.032(2) C49 0.0324(17) 0.0431(19) 0.0368(17) -0.0120(15) 0.0159(14) -0.0143(15) C50 0.0373(18) 0.041(2) 0.0421(19) 0.0006(15) 0.0139(15) -0.0103(15) C51 0.059(2) 0.055(2) 0.040(2) -0.0038(17) 0.0211(18) -0.019(2) C52 0.060(3) 0.078(3) 0.054(3) -0.023(2) 0.038(2) -0.031(2) _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 O1 2.043(2) . ? Ni1 N7 2.058(2) . ? Ni1 N10 2.088(2) . ? Ni1 N4 2.092(2) . ? Ni1 N1 2.115(2) . ? Ni1 Ni2 2.4214(5) . ? Ni2 N5 1.880(2) . ? Ni2 N8 1.888(2) . ? Ni2 N11 1.893(2) . ? Ni2 N2 1.898(2) . ? Ni2 Ni3 2.4136(5) . ? Ni3 O3 1.991(2) . ? Ni3 N3 2.064(2) . ? Ni3 N6 2.077(2) . ? Ni3 N9 2.091(2) . ? Ni3 N12 2.127(2) . ? O1 C41 1.106(5) . ? O2 C41 1.280(5) . ? O3 C47 1.259(4) . ? O4 C47 1.239(4) . ? N1 C1 1.349(4) . ? N1 C5 1.354(4) . ? N2 C5 1.375(3) . ? N2 C6 1.377(4) . ? N3 C10 1.349(4) . ? N3 C6 1.361(4) . ? N4 C11 1.349(4) . ? N4 C15 1.355(4) . ? N5 C15 1.379(4) . ? N5 C16 1.381(4) . ? N6 C16 1.346(4) . ? N6 C20 1.351(4) . ? N7 C21 1.347(4) . ? N7 C25 1.361(4) . ? N8 C26 1.375(4) . ? N8 C25 1.378(4) . ? N9 C30 1.348(4) . ? N9 C26 1.357(4) . ? N10 C31 1.351(4) . ? N10 C35 1.353(4) . ? N11 C36 1.374(4) . ? N11 C35 1.377(4) . ? N12 C36 1.347(4) . ? N12 C40 1.352(4) . ? N13 C42 1.306(9) . ? N13 C46 1.348(11) . ? N13' C42' 1.332(13) . ? N13' C46' 1.416(12) . ? N14 C52 1.327(6) . ? N14 C48 1.339(5) . ? C1 C2 1.369(4) . ? C2 C3 1.388(4) . ? C3 C4 1.374(4) . ? C4 C5 1.409(4) . ? C6 C7 1.408(4) . ? C7 C8 1.377(4) . ? C8 C9 1.393(5) . ? C9 C10 1.371(4) . ? C11 C12 1.380(5) . ? C12 C13 1.382(6) . ? C13 C14 1.369(5) . ? C14 C15 1.412(4) . ? C16 C17 1.408(4) . ? C17 C18 1.367(5) . ? C18 C19 1.376(5) . ? C19 C20 1.372(5) . ? C21 C22 1.373(5) . ? C22 C23 1.381(5) . ? C23 C24 1.376(5) . ? C24 C25 1.407(4) . ? C26 C27 1.406(4) . ? C27 C28 1.373(5) . ? C28 C29 1.391(5) . ? C29 C30 1.380(4) . ? C31 C32 1.378(4) . ? C32 C33 1.384(5) . ? C33 C34 1.368(4) . ? C34 C35 1.416(4) . ? C36 C37 1.416(4) . ? C37 C38 1.373(4) . ? C38 C39 1.396(5) . ? C39 C40 1.371(4) . ? C41 C43 1.554(6) . ? C43 C42 1.262(8) . ? C43 C44' 1.322(14) . ? C43 C44 1.448(8) . ? C43 C42' 1.633(12) . ? C44 C45 1.382(11) . ? C45 C46 1.265(12) . ? C44' C45' 1.312(16) . ? C45' C46' 1.259(15) . ? C47 C49 1.520(4) . ? C48 C49 1.382(5) . ? C49 C50 1.388(5) . ? C50 C51 1.378(5) . ? C51 C52 1.369(6) . ? 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 O1 Ni1 N7 101.95(10) . . ? O1 Ni1 N10 91.87(10) . . ? N7 Ni1 N10 165.91(9) . . ? O1 Ni1 N4 101.92(9) . . ? N7 Ni1 N4 89.80(10) . . ? N10 Ni1 N4 89.96(9) . . ? O1 Ni1 N1 94.35(9) . . ? N7 Ni1 N1 85.43(9) . . ? N10 Ni1 N1 90.91(9) . . ? N4 Ni1 N1 163.67(9) . . ? O1 Ni1 Ni2 173.02(7) . . ? N7 Ni1 Ni2 82.88(7) . . ? N10 Ni1 Ni2 83.11(7) . . ? N4 Ni1 Ni2 83.00(7) . . ? N1 Ni1 Ni2 80.92(6) . . ? N5 Ni2 N8 90.22(10) . . ? N5 Ni2 N11 89.35(10) . . ? N8 Ni2 N11 178.67(10) . . ? N5 Ni2 N2 178.46(10) . . ? N8 Ni2 N2 89.16(10) . . ? N11 Ni2 N2 91.31(10) . . ? N5 Ni2 Ni3 89.46(7) . . ? N8 Ni2 Ni3 90.24(7) . . ? N11 Ni2 Ni3 91.01(7) . . ? N2 Ni2 Ni3 89.14(7) . . ? N5 Ni2 Ni1 89.12(7) . . ? N8 Ni2 Ni1 89.14(7) . . ? N11 Ni2 Ni1 89.60(7) . . ? N2 Ni2 Ni1 92.27(7) . . ? Ni3 Ni2 Ni1 178.45(2) . . ? O3 Ni3 N3 98.05(9) . . ? O3 Ni3 N6 95.60(9) . . ? N3 Ni3 N6 166.34(9) . . ? O3 Ni3 N9 106.76(9) . . ? N3 Ni3 N9 87.49(9) . . ? N6 Ni3 N9 88.13(9) . . ? O3 Ni3 N12 89.86(9) . . ? N3 Ni3 N12 89.87(9) . . ? N6 Ni3 N12 90.63(9) . . ? N9 Ni3 N12 163.37(9) . . ? O3 Ni3 Ni2 170.76(6) . . ? N3 Ni3 Ni2 83.02(6) . . ? N6 Ni3 Ni2 83.58(7) . . ? N9 Ni3 Ni2 82.43(7) . . ? N12 Ni3 Ni2 80.95(6) . . ? C41 O1 Ni1 136.7(3) . . ? C47 O3 Ni3 142.2(2) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Ni1 119.14(19) . . ? C5 N1 Ni1 122.12(18) . . ? C5 N2 C6 122.7(2) . . ? C5 N2 Ni2 118.65(18) . . ? C6 N2 Ni2 118.16(18) . . ? C10 N3 C6 119.2(2) . . ? C10 N3 Ni3 119.65(19) . . ? C6 N3 Ni3 120.78(18) . . ? C11 N4 C15 118.8(3) . . ? C11 N4 Ni1 121.2(2) . . ? C15 N4 Ni1 119.66(19) . . ? C15 N5 C16 121.3(2) . . ? C15 N5 Ni2 118.66(19) . . ? C16 N5 Ni2 119.77(19) . . ? C16 N6 C20 118.6(3) . . ? C16 N6 Ni3 119.95(19) . . ? C20 N6 Ni3 121.4(2) . . ? C21 N7 C25 119.0(3) . . ? C21 N7 Ni1 119.9(2) . . ? C25 N7 Ni1 120.70(19) . . ? C26 N8 C25 123.0(2) . . ? C26 N8 Ni2 119.20(19) . . ? C25 N8 Ni2 117.77(19) . . ? C30 N9 C26 119.0(2) . . ? C30 N9 Ni3 120.7(2) . . ? C26 N9 Ni3 120.35(19) . . ? C31 N10 C35 118.8(3) . . ? C31 N10 Ni1 120.6(2) . . ? C35 N10 Ni1 120.31(19) . . ? C36 N11 C35 122.9(2) . . ? C36 N11 Ni2 118.52(18) . . ? C35 N11 Ni2 118.56(18) . . ? C36 N12 C40 118.6(2) . . ? C36 N12 Ni3 120.84(18) . . ? C40 N12 Ni3 120.55(19) . . ? C42 N13 C46 112.4(7) . . ? C42' N13' C46' 116.9(9) . . ? C52 N14 C48 116.6(4) . . ? N1 C1 C2 123.7(3) . . ? C1 C2 C3 118.0(3) . . ? C4 C3 C2 119.8(3) . . ? C3 C4 C5 119.4(3) . . ? N1 C5 N2 115.9(2) . . ? N1 C5 C4 120.5(3) . . ? N2 C5 C4 123.5(3) . . ? N3 C6 N2 115.1(2) . . ? N3 C6 C7 119.9(3) . . ? N2 C6 C7 124.7(3) . . ? C8 C7 C6 119.9(3) . . ? C7 C8 C9 119.5(3) . . ? C10 C9 C8 118.3(3) . . ? N3 C10 C9 123.3(3) . . ? N4 C11 C12 122.5(3) . . ? C11 C12 C13 118.8(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 118.8(3) . . ? N4 C15 N5 115.7(3) . . ? N4 C15 C14 121.1(3) . . ? N5 C15 C14 123.0(3) . . ? N6 C16 N5 116.2(3) . . ? N6 C16 C17 120.6(3) . . ? N5 C16 C17 123.2(3) . . ? C18 C17 C16 119.4(3) . . ? C17 C18 C19 120.0(3) . . ? C20 C19 C18 118.3(3) . . ? N6 C20 C19 123.2(3) . . ? N7 C21 C22 123.2(3) . . ? C21 C22 C23 118.1(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.1(3) . . ? N7 C25 N8 115.4(2) . . ? N7 C25 C24 120.3(3) . . ? N8 C25 C24 124.1(3) . . ? N9 C26 N8 115.9(2) . . ? N9 C26 C27 120.3(3) . . ? N8 C26 C27 123.6(3) . . ? C28 C27 C26 119.7(3) . . ? C27 C28 C29 119.8(3) . . ? C30 C29 C28 117.9(3) . . ? N9 C30 C29 123.2(3) . . ? N10 C31 C32 123.5(3) . . ? C31 C32 C33 118.0(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 120.1(3) . . ? N10 C35 N11 116.0(2) . . ? N10 C35 C34 119.8(3) . . ? N11 C35 C34 123.9(3) . . ? N12 C36 N11 115.7(2) . . ? N12 C36 C37 120.7(3) . . ? N11 C36 C37 123.5(3) . . ? C38 C37 C36 119.5(3) . . ? C37 C38 C39 119.4(3) . . ? C40 C39 C38 118.2(3) . . ? N12 C40 C39 123.5(3) . . ? O1 C41 O2 130.5(4) . . ? O1 C41 C43 117.1(4) . . ? O2 C41 C43 112.4(4) . . ? C42 C43 C44' 101.2(8) . . ? C42 C43 C44 122.6(5) . . ? C44' C43 C44 21.7(6) . . ? C42 C43 C41 120.8(4) . . ? C44' C43 C41 137.0(8) . . ? C44 C43 C41 115.4(5) . . ? C42 C43 C42' 22.8(4) . . ? C44' C43 C42' 104.8(8) . . ? C44 C43 C42' 125.6(6) . . ? C41 C43 C42' 117.4(5) . . ? C43 C42 N13 123.2(6) . . ? C45 C44 C43 114.4(7) . . ? C46 C45 C44 114.8(8) . . ? C45 C46 N13 132.2(8) . . ? N13' C42' C43 120.4(8) . . ? C45' C44' C43 136.2(13) . . ? C46' C45' C44' 114.8(11) . . ? C45' C46' N13' 126.2(9) . . ? O4 C47 O3 127.3(3) . . ? O4 C47 C49 119.1(3) . . ? O3 C47 C49 113.5(3) . . ? N14 C48 C49 124.1(4) . . ? C48 C49 C50 117.3(3) . . ? C48 C49 C47 120.6(3) . . ? C50 C49 C47 122.1(3) . . ? C51 C50 C49 119.3(3) . . ? C52 C51 C50 118.4(4) . . ? N14 C52 C51 124.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.460 _refine_diff_density_min -1.246 _refine_diff_density_rms 0.292 data_ic8999 _database_code_CSD 199618 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C141 H98 Cl2 N22 Ni3 O4 Zn2' _chemical_formula_weight 2542.18 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' Zn Zn 0.2839 1.4301 '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 13.2756(1) _cell_length_b 17.4339(1) _cell_length_c 26.7913(2) _cell_angle_alpha 77.0290(3) _cell_angle_beta 85.9760(3) _cell_angle_gamma 88.9666(3) _cell_volume 6027.59(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 102583 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 27641 _reflns_number_gt 17891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0888P)^2^+0.9287P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0071(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 27641 _refine_ls_number_parameters 1568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn -0.22287(3) -0.00554(2) 0.841939(15) 0.02103(11) Uani 1 1 d . . . Zn2 Zn 0.72693(3) 0.51153(2) 0.142982(15) 0.02266(11) Uani 1 1 d . . . Ni1 Ni 0.07962(3) 0.21911(3) 0.536483(17) 0.02605(12) Uani 1 1 d . . . Ni2 Ni 0.23386(3) 0.25818(2) 0.483801(16) 0.02279(11) Uani 1 1 d . . . Ni3 Ni 0.38746(3) 0.29839(3) 0.432022(17) 0.02690(12) Uani 1 1 d . . . O1 O -0.03269(19) 0.18900(16) 0.59122(10) 0.0380(6) Uani 1 1 d . . . O2 O -0.1768(2) 0.1436(2) 0.56980(10) 0.0541(8) Uani 1 1 d . . . O3 O 0.50578(18) 0.32546(16) 0.38238(9) 0.0368(6) Uani 1 1 d . . . O4 O 0.6362(2) 0.37889(18) 0.41210(10) 0.0456(7) Uani 1 1 d . . . N1 N 0.1428(2) 0.28584(17) 0.58279(10) 0.0297(7) Uani 1 1 d . . . N2 N 0.2989(2) 0.27249(17) 0.54164(10) 0.0277(7) Uani 1 1 d . . . N3 N 0.4549(2) 0.25996(18) 0.49971(11) 0.0307(7) Uani 1 1 d . . . N4 N 0.0501(2) 0.16399(16) 0.47672(11) 0.0273(7) Uani 1 1 d . . . N5 N 0.1726(2) 0.24382(16) 0.42508(11) 0.0246(6) Uani 1 1 d . . . N6 N 0.2895(2) 0.32791(17) 0.37343(10) 0.0267(7) Uani 1 1 d . . . N7 N 0.1692(2) 0.12340(17) 0.56967(11) 0.0276(7) Uani 1 1 d . . . N8 N 0.2771(2) 0.15177(16) 0.49644(11) 0.0261(6) Uani 1 1 d . . . N9 N 0.3863(2) 0.18128(18) 0.42375(11) 0.0307(7) Uani 1 1 d . . . N10 N 0.0232(2) 0.31941(17) 0.49065(11) 0.0273(7) Uani 1 1 d . . . N11 N 0.1879(2) 0.36388(16) 0.47075(10) 0.0250(6) Uani 1 1 d . . . N12 N 0.3528(2) 0.40666(17) 0.45001(11) 0.0279(7) Uani 1 1 d . . . N13 N -0.2035(2) 0.06587(16) 0.76212(11) 0.0255(6) Uani 1 1 d . . . N14 N 0.7072(2) 0.44046(16) 0.22105(11) 0.0273(7) Uani 1 1 d . . . N15 N -0.37557(19) 0.00264(16) 0.86097(11) 0.0238(6) Uani 1 1 d . . . N16 N -0.1958(2) 0.06778(16) 0.89051(11) 0.0232(6) Uani 1 1 d . . . N17 N -0.07304(19) -0.03881(15) 0.84404(10) 0.0225(6) Uani 1 1 d . . . N18 N -0.2529(2) -0.10508(16) 0.81473(10) 0.0226(6) Uani 1 1 d . . . N19 N 0.8796(2) 0.50180(16) 0.12582(11) 0.0242(6) Uani 1 1 d . . . N20 N 0.7003(2) 0.43831(16) 0.09520(11) 0.0257(6) Uani 1 1 d . . . N21 N 0.5746(2) 0.54087(16) 0.14403(11) 0.0248(6) Uani 1 1 d . . . N22 N 0.7550(2) 0.60992(16) 0.17114(11) 0.0243(6) Uani 1 1 d . . . C1 C 0.0827(3) 0.3154(2) 0.61703(14) 0.0362(9) Uani 1 1 d . . . H1A H 0.0118 0.3084 0.6178 0.043 Uiso 1 1 calc R . . C2 C 0.1199(3) 0.3550(2) 0.65055(15) 0.0428(10) Uani 1 1 d . . . H2A H 0.0763 0.3729 0.6752 0.051 Uiso 1 1 calc R . . C3 C 0.2230(4) 0.3683(2) 0.64737(15) 0.0448(11) Uani 1 1 d . . . H3A H 0.2505 0.3963 0.6698 0.054 Uiso 1 1 calc R . . C4 C 0.2854(3) 0.3414(2) 0.61226(14) 0.0363(9) Uani 1 1 d . . . H4A H 0.3559 0.3511 0.6098 0.044 Uiso 1 1 calc R . . C5 C 0.2433(3) 0.2990(2) 0.57974(13) 0.0291(8) Uani 1 1 d . . . C6 C 0.3996(3) 0.2523(2) 0.54512(13) 0.0286(8) Uani 1 1 d . . . C7 C 0.4440(3) 0.2202(2) 0.59147(15) 0.0394(10) Uani 1 1 d . . . H7A H 0.4056 0.2151 0.6233 0.047 Uiso 1 1 calc R . . C8 C 0.5422(3) 0.1966(3) 0.59035(16) 0.0467(11) Uani 1 1 d . . . H8A H 0.5723 0.1747 0.6215 0.056 Uiso 1 1 calc R . . C9 C 0.5985(3) 0.2045(3) 0.54410(17) 0.0472(11) Uani 1 1 d . . . H9A H 0.6675 0.1890 0.5428 0.057 Uiso 1 1 calc R . . C10 C 0.5512(3) 0.2353(2) 0.50027(16) 0.0402(10) Uani 1 1 d . . . H10A H 0.5889 0.2395 0.4683 0.048 Uiso 1 1 calc R . . C11 C -0.0200(3) 0.1064(2) 0.48333(15) 0.0337(9) Uani 1 1 d . . . H11A H -0.0596 0.0939 0.5150 0.040 Uiso 1 1 calc R . . C12 C -0.0366(3) 0.0654(2) 0.44678(16) 0.0400(10) Uani 1 1 d . . . H12A H -0.0888 0.0273 0.4522 0.048 Uiso 1 1 calc R . . C13 C 0.0247(3) 0.0810(2) 0.40146(16) 0.0411(10) Uani 1 1 d . . . H13A H 0.0178 0.0510 0.3763 0.049 Uiso 1 1 calc R . . C14 C 0.0952(3) 0.1396(2) 0.39319(14) 0.0322(8) Uani 1 1 d . . . H14C H 0.1373 0.1509 0.3623 0.039 Uiso 1 1 calc R . . C15 C 0.1044(3) 0.1829(2) 0.43076(13) 0.0268(8) Uani 1 1 d . . . C16 C 0.1976(3) 0.2935(2) 0.37849(13) 0.0251(7) Uani 1 1 d . . . C17 C 0.1314(3) 0.3145(2) 0.33834(13) 0.0295(8) Uani 1 1 d . . . H17A H 0.0668 0.2905 0.3417 0.035 Uiso 1 1 calc R . . C18 C 0.1603(3) 0.3693(2) 0.29481(14) 0.0318(8) Uani 1 1 d . . . H18A H 0.1163 0.3830 0.2677 0.038 Uiso 1 1 calc R . . C19 C 0.2544(3) 0.4048(2) 0.29045(14) 0.0365(9) Uani 1 1 d . . . H19A H 0.2759 0.4431 0.2606 0.044 Uiso 1 1 calc R . . C20 C 0.3151(3) 0.3829(2) 0.33056(14) 0.0337(9) Uani 1 1 d . . . H20A H 0.3789 0.4078 0.3280 0.040 Uiso 1 1 calc R . . C21 C 0.1458(3) 0.0818(2) 0.61791(14) 0.0323(8) Uani 1 1 d . . . H21A H 0.0878 0.0968 0.6363 0.039 Uiso 1 1 calc R . . C22 C 0.2020(3) 0.0190(2) 0.64170(15) 0.0383(9) Uani 1 1 d . . . H22A H 0.1822 -0.0098 0.6754 0.046 Uiso 1 1 calc R . . C23 C 0.2880(3) -0.0014(2) 0.61545(15) 0.0405(10) Uani 1 1 d . . . H23A H 0.3279 -0.0448 0.6310 0.049 Uiso 1 1 calc R . . C24 C 0.3154(3) 0.0405(2) 0.56744(14) 0.0348(9) Uani 1 1 d . . . H24A H 0.3757 0.0277 0.5498 0.042 Uiso 1 1 calc R . . C25 C 0.2533(3) 0.1038(2) 0.54377(13) 0.0267(8) Uani 1 1 d . . . C26 C 0.3334(3) 0.1253(2) 0.45843(14) 0.0283(8) Uani 1 1 d . . . C27 C 0.3321(3) 0.0471(2) 0.45277(15) 0.0367(9) Uani 1 1 d . . . H27A H 0.2932 0.0085 0.4767 0.044 Uiso 1 1 calc R . . C28 C 0.3870(3) 0.0271(3) 0.41265(18) 0.0485(11) Uani 1 1 d . . . H28A H 0.3877 -0.0258 0.4089 0.058 Uiso 1 1 calc R . . C29 C 0.4415(3) 0.0840(3) 0.37744(17) 0.0512(12) Uani 1 1 d . . . H29A H 0.4808 0.0708 0.3496 0.061 Uiso 1 1 calc R . . C30 C 0.4376(3) 0.1599(3) 0.38361(15) 0.0405(10) Uani 1 1 d . . . H30A H 0.4727 0.1993 0.3585 0.049 Uiso 1 1 calc R . . C31 C -0.0758(3) 0.3226(2) 0.48140(14) 0.0321(8) Uani 1 1 d . . . H31A H -0.1186 0.2811 0.4997 0.038 Uiso 1 1 calc R . . C32 C -0.1173(3) 0.3829(2) 0.44673(16) 0.0417(10) Uani 1 1 d . . . H32A H -0.1872 0.3835 0.4410 0.050 Uiso 1 1 calc R . . C33 C -0.0533(3) 0.4431(2) 0.42024(17) 0.0453(10) Uani 1 1 d . . . H33A H -0.0798 0.4862 0.3964 0.054 Uiso 1 1 calc R . . C34 C 0.0472(3) 0.4407(2) 0.42835(15) 0.0381(9) Uani 1 1 d . . . H34A H 0.0906 0.4818 0.4100 0.046 Uiso 1 1 calc R . . C35 C 0.0863(3) 0.3770(2) 0.46412(13) 0.0269(8) Uani 1 1 d . . . C36 C 0.2566(3) 0.4242(2) 0.46392(13) 0.0281(8) Uani 1 1 d . . . C37 C 0.2326(3) 0.4987(2) 0.47318(16) 0.0427(10) Uani 1 1 d . . . H37A H 0.1651 0.5106 0.4830 0.051 Uiso 1 1 calc R . . C38 C 0.3071(3) 0.5545(2) 0.46803(18) 0.0484(11) Uani 1 1 d . . . H38A H 0.2914 0.6052 0.4740 0.058 Uiso 1 1 calc R . . C39 C 0.4050(3) 0.5354(2) 0.45407(17) 0.0463(11) Uani 1 1 d . . . H39A H 0.4576 0.5731 0.4501 0.056 Uiso 1 1 calc R . . C40 C 0.4252(3) 0.4622(2) 0.44615(14) 0.0364(9) Uani 1 1 d . . . H40A H 0.4930 0.4493 0.4375 0.044 Uiso 1 1 calc R . . C41 C -0.1179(3) 0.1555(2) 0.60053(15) 0.0345(9) Uani 1 1 d . . . C42 C -0.1304(3) 0.1188(2) 0.74740(14) 0.0338(9) Uani 1 1 d . . . H42A H -0.0970 0.1362 0.7731 0.041 Uiso 1 1 calc R . . C43 C -0.1002(3) 0.1502(2) 0.69598(14) 0.0345(9) Uani 1 1 d . . . H43A H -0.0471 0.1877 0.6872 0.041 Uiso 1 1 calc R . . C44 C -0.1485(3) 0.1263(2) 0.65778(13) 0.0281(8) Uani 1 1 d . . . C45 C -0.2260(3) 0.0719(2) 0.67338(14) 0.0337(9) Uani 1 1 d . . . H45A H -0.2618 0.0543 0.6486 0.040 Uiso 1 1 calc R . . C46 C -0.2508(3) 0.0437(2) 0.72500(14) 0.0341(9) Uani 1 1 d . . . H46A H -0.3041 0.0066 0.7348 0.041 Uiso 1 1 calc R . . C47 C 0.5895(3) 0.3615(2) 0.37787(14) 0.0346(9) Uani 1 1 d . . . C48 C 0.7493(3) 0.4622(2) 0.26002(14) 0.0304(8) Uani 1 1 d . . . H48A H 0.8053 0.4971 0.2522 0.036 Uiso 1 1 calc R . . C49 C 0.7150(3) 0.4363(2) 0.31080(14) 0.0283(8) Uani 1 1 d . . . H49A H 0.7474 0.4527 0.3371 0.034 Uiso 1 1 calc R . . C50 C 0.6333(2) 0.3863(2) 0.32291(13) 0.0269(8) Uani 1 1 d . . . C51 C 0.5908(3) 0.3624(2) 0.28273(14) 0.0325(9) Uani 1 1 d . . . H51A H 0.5350 0.3272 0.2894 0.039 Uiso 1 1 calc R . . C52 C 0.6307(3) 0.3905(2) 0.23335(14) 0.0300(8) Uani 1 1 d . . . H52A H 0.6017 0.3730 0.2064 0.036 Uiso 1 1 calc R . . C53 C -0.2672(2) 0.10765(19) 0.91466(13) 0.0232(7) Uani 1 1 d . . . C54 C -0.2173(3) 0.1532(2) 0.94429(14) 0.0284(8) Uani 1 1 d . . . H54A H -0.2491 0.1868 0.9642 0.034 Uiso 1 1 calc R . . C55 C -0.1174(3) 0.1395(2) 0.93860(14) 0.0281(8) Uani 1 1 d . . . H55A H -0.0658 0.1616 0.9538 0.034 Uiso 1 1 calc R . . C56 C -0.1031(2) 0.08517(19) 0.90537(13) 0.0242(7) Uani 1 1 d . . . C57 C -0.0111(2) 0.0523(2) 0.89330(13) 0.0245(7) Uani 1 1 d . . . C58 C 0.0025(2) -0.00605(19) 0.86490(13) 0.0246(7) Uani 1 1 d . . . C59 C 0.0984(3) -0.0412(2) 0.85342(14) 0.0283(8) Uani 1 1 d . . . H59A H 0.1622 -0.0298 0.8640 0.034 Uiso 1 1 calc R . . C60 C 0.0799(2) -0.0932(2) 0.82496(14) 0.0289(8) Uani 1 1 d . . . H60A H 0.1287 -0.1246 0.8110 0.035 Uiso 1 1 calc R . . C61 C -0.0274(2) -0.0926(2) 0.81940(13) 0.0243(7) Uani 1 1 d . . . C62 C -0.0768(2) -0.14160(19) 0.79420(13) 0.0236(7) Uani 1 1 d . . . C63 C -0.1821(2) -0.14677(19) 0.79183(12) 0.0225(7) Uani 1 1 d . . . C64 C -0.2319(3) -0.1965(2) 0.76474(13) 0.0272(8) Uani 1 1 d . . . H64A H -0.2003 -0.2307 0.7453 0.033 Uiso 1 1 calc R . . C65 C -0.3326(2) -0.1849(2) 0.77241(13) 0.0256(8) Uani 1 1 d . . . H65A H -0.3849 -0.2103 0.7598 0.031 Uiso 1 1 calc R . . C66 C -0.3456(2) -0.12720(19) 0.80319(13) 0.0225(7) Uani 1 1 d . . . C67 C -0.4390(2) -0.09718(19) 0.81842(12) 0.0236(7) Uani 1 1 d . . . C68 C -0.4519(2) -0.0371(2) 0.84541(13) 0.0243(7) Uani 1 1 d . . . C69 C -0.5480(3) -0.0086(2) 0.86243(13) 0.0278(8) Uani 1 1 d . . . H69A H -0.6126 -0.0259 0.8563 0.033 Uiso 1 1 calc R . . C70 C -0.5301(3) 0.0468(2) 0.88861(13) 0.0279(8) Uani 1 1 d . . . H70A H -0.5793 0.0756 0.9044 0.033 Uiso 1 1 calc R . . C71 C -0.4216(2) 0.0539(2) 0.88804(13) 0.0240(7) Uani 1 1 d . . . C72 C -0.3717(2) 0.10302(19) 0.91314(13) 0.0228(7) Uani 1 1 d . . . C73 C 0.0822(2) 0.0804(2) 0.91265(13) 0.0240(7) Uani 1 1 d . . . C74 C 0.1242(3) 0.0371(2) 0.95584(15) 0.0350(9) Uani 1 1 d . . . H74A H 0.0937 -0.0110 0.9738 0.042 Uiso 1 1 calc R . . C75 C 0.2101(3) 0.0630(2) 0.97331(16) 0.0386(10) Uani 1 1 d . . . H75A H 0.2381 0.0326 1.0032 0.046 Uiso 1 1 calc R . . C76 C 0.2550(3) 0.1319(2) 0.94791(15) 0.0335(9) Uani 1 1 d . . . H76A H 0.3136 0.1497 0.9603 0.040 Uiso 1 1 calc R . . C77 C 0.2151(3) 0.1758(2) 0.90416(15) 0.0336(9) Uani 1 1 d . . . H77A H 0.2468 0.2234 0.8861 0.040 Uiso 1 1 calc R . . C78 C 0.1289(3) 0.1500(2) 0.88690(14) 0.0309(8) Uani 1 1 d . . . H78A H 0.1012 0.1804 0.8570 0.037 Uiso 1 1 calc R . . C79 C -0.0117(2) -0.1937(2) 0.76750(13) 0.0246(7) Uani 1 1 d . . . C80 C -0.0025(3) -0.2737(2) 0.78800(15) 0.0301(8) Uani 1 1 d . . . H80A H -0.0381 -0.2969 0.8196 0.036 Uiso 1 1 calc R . . C81 C 0.0582(3) -0.3200(2) 0.76262(16) 0.0353(9) Uani 1 1 d . . . H81A H 0.0652 -0.3745 0.7774 0.042 Uiso 1 1 calc R . . C82 C 0.1086(3) -0.2881(2) 0.71627(16) 0.0361(10) Uani 1 1 d . . . H82A H 0.1488 -0.3207 0.6987 0.043 Uiso 1 1 calc R . . C83 C 0.1007(3) -0.2077(2) 0.69509(15) 0.0361(9) Uani 1 1 d . . . H83A H 0.1357 -0.1851 0.6632 0.043 Uiso 1 1 calc R . . C84 C 0.0410(3) -0.1613(2) 0.72106(14) 0.0313(8) Uani 1 1 d . . . H84A H 0.0360 -0.1064 0.7069 0.038 Uiso 1 1 calc R . . C85 C -0.5326(2) -0.13425(19) 0.80642(13) 0.0234(7) Uani 1 1 d . . . C86 C -0.5745(3) -0.1087(3) 0.75963(15) 0.0475(11) Uani 1 1 d . . . H86A H -0.5449 -0.0662 0.7347 0.057 Uiso 1 1 calc R . . C87 C -0.6607(3) -0.1458(3) 0.74909(16) 0.0513(12) Uani 1 1 d . . . H87A H -0.6883 -0.1288 0.7167 0.062 Uiso 1 1 calc R . . C88 C -0.7051(3) -0.2054(2) 0.78438(14) 0.0301(8) Uani 1 1 d . . . H88A H -0.7630 -0.2306 0.7767 0.036 Uiso 1 1 calc R . . C89 C -0.6662(3) -0.2290(2) 0.83100(16) 0.0412(10) Uani 1 1 d . . . H89A H -0.6982 -0.2700 0.8562 0.049 Uiso 1 1 calc R . . C90 C -0.5802(3) -0.1936(2) 0.84202(15) 0.0384(9) Uani 1 1 d . . . H90A H -0.5539 -0.2109 0.8748 0.046 Uiso 1 1 calc R . . C91 C -0.4352(2) 0.1502(2) 0.94368(13) 0.0238(7) Uani 1 1 d . . . C92 C -0.4549(3) 0.2289(2) 0.92392(15) 0.0356(9) Uani 1 1 d . . . H92A H -0.4282 0.2535 0.8904 0.043 Uiso 1 1 calc R . . C93 C -0.5140(3) 0.2728(2) 0.95290(17) 0.0429(10) Uani 1 1 d . . . H93A H -0.5279 0.3267 0.9389 0.051 Uiso 1 1 calc R . . C94 C -0.5515(3) 0.2382(2) 1.00126(16) 0.0391(10) Uani 1 1 d . . . H94A H -0.5922 0.2678 1.0207 0.047 Uiso 1 1 calc R . . C95 C -0.5304(3) 0.1598(2) 1.02217(15) 0.0375(9) Uani 1 1 d . . . H95A H -0.5550 0.1361 1.0562 0.045 Uiso 1 1 calc R . . C96 C -0.4729(3) 0.1161(2) 0.99291(14) 0.0325(9) Uani 1 1 d . . . H96A H -0.4595 0.0622 1.0070 0.039 Uiso 1 1 calc R . . C97 C 0.9544(2) 0.53730(19) 0.14495(13) 0.0255(8) Uani 1 1 d . . . C98 C 1.0509(3) 0.5042(2) 0.13244(14) 0.0284(8) Uani 1 1 d . . . H98A H 1.1149 0.5179 0.1417 0.034 Uiso 1 1 calc R . . C99 C 1.0334(3) 0.4503(2) 0.10534(14) 0.0277(8) Uani 1 1 d . . . H99A H 1.0827 0.4192 0.0916 0.033 Uiso 1 1 calc R . . C100 C 0.9258(2) 0.44833(19) 0.10095(13) 0.0245(7) Uani 1 1 d . . . C101 C 0.8765(2) 0.40039(19) 0.07488(13) 0.0231(7) Uani 1 1 d . . . C102 C 0.7714(2) 0.39797(19) 0.07117(13) 0.0243(7) Uani 1 1 d . . . C103 C 0.7218(3) 0.3514(2) 0.04216(13) 0.0280(8) Uani 1 1 d . . . H10B H 0.7538 0.3185 0.0219 0.034 Uiso 1 1 calc R . . C104 C 0.6216(3) 0.36314(19) 0.04916(13) 0.0262(8) Uani 1 1 d . . . H10C H 0.5699 0.3398 0.0348 0.031 Uiso 1 1 calc R . . C105 C 0.6071(2) 0.41728(19) 0.08229(13) 0.0239(7) Uani 1 1 d . . . C106 C 0.5133(2) 0.44512(19) 0.09824(13) 0.0253(8) Uani 1 1 d . . . C107 C 0.4989(3) 0.5025(2) 0.12728(13) 0.0264(8) Uani 1 1 d . . . C108 C 0.4023(3) 0.5290(2) 0.14468(15) 0.0323(9) Uani 1 1 d . . . H10D H 0.3380 0.5126 0.1376 0.039 Uiso 1 1 calc R . . C109 C 0.4206(3) 0.5820(2) 0.17324(15) 0.0329(9) Uani 1 1 d . . . H10E H 0.3715 0.6090 0.1904 0.039 Uiso 1 1 calc R . . C110 C 0.5287(3) 0.5894(2) 0.17259(14) 0.0273(8) Uani 1 1 d . . . C111 C 0.5783(3) 0.6388(2) 0.19738(13) 0.0265(8) Uani 1 1 d . . . C112 C 0.6838(2) 0.64836(19) 0.19602(13) 0.0238(7) Uani 1 1 d . . . C113 C 0.7329(3) 0.6974(2) 0.22390(14) 0.0289(8) Uani 1 1 d . . . H11B H 0.7008 0.7309 0.2437 0.035 Uiso 1 1 calc R . . C114 C 0.8336(3) 0.6863(2) 0.21640(13) 0.0264(8) Uani 1 1 d . . . H11C H 0.8855 0.7108 0.2299 0.032 Uiso 1 1 calc R . . C115 C 0.8474(3) 0.63045(19) 0.18407(13) 0.0245(7) Uani 1 1 d . . . C116 C 0.9400(2) 0.59686(19) 0.17269(13) 0.0244(7) Uani 1 1 d . . . C117 C 0.9397(2) 0.34613(19) 0.04947(13) 0.0232(7) Uani 1 1 d . . . C118 C 0.9502(3) 0.2680(2) 0.07373(15) 0.0328(9) Uani 1 1 d . . . H11D H 0.9170 0.2489 0.1067 0.039 Uiso 1 1 calc R . . C119 C 1.0080(3) 0.2169(2) 0.05091(16) 0.0372(9) Uani 1 1 d . . . H11E H 1.0154 0.1635 0.0684 0.045 Uiso 1 1 calc R . . C120 C 1.0552(3) 0.2435(2) 0.00266(15) 0.0334(9) Uani 1 1 d . . . H12B H 1.0942 0.2083 -0.0133 0.040 Uiso 1 1 calc R . . C121 C 1.0455(3) 0.3207(2) -0.02214(15) 0.0380(9) Uani 1 1 d . . . H12C H 1.0781 0.3391 -0.0553 0.046 Uiso 1 1 calc R . . C122 C 0.9879(3) 0.3722(2) 0.00116(14) 0.0337(9) Uani 1 1 d . . . H12D H 0.9816 0.4257 -0.0162 0.040 Uiso 1 1 calc R . . C123 C 0.4204(2) 0.40938(19) 0.08397(13) 0.0240(7) Uani 1 1 d . . . C124 C 0.3739(3) 0.4430(2) 0.03942(16) 0.0400(10) Uani 1 1 d . . . H12E H 0.4019 0.4889 0.0170 0.048 Uiso 1 1 calc R . . C125 C 0.2872(3) 0.4104(3) 0.02730(16) 0.0457(11) Uani 1 1 d . . . H12F H 0.2562 0.4340 -0.0033 0.055 Uiso 1 1 calc R . . C126 C 0.2457(3) 0.3442(2) 0.05919(15) 0.0326(9) Uani 1 1 d . . . H12G H 0.1865 0.3216 0.0506 0.039 Uiso 1 1 calc R . . C127 C 0.2900(3) 0.3109(2) 0.10339(16) 0.0375(9) Uani 1 1 d . . . H12H H 0.2612 0.2653 0.1258 0.045 Uiso 1 1 calc R . . C128 C 0.3766(3) 0.3435(2) 0.11562(15) 0.0368(9) Uani 1 1 d . . . H12I H 0.4066 0.3198 0.1466 0.044 Uiso 1 1 calc R . . C129 C 0.5145(3) 0.6836(2) 0.22962(14) 0.0323(9) Uani 1 1 d . . . C130 C 0.4778(3) 0.6472(3) 0.27849(16) 0.0473(11) Uani 1 1 d . . . H13B H 0.4930 0.5934 0.2920 0.057 Uiso 1 1 calc R . . C131 C 0.4175(3) 0.6899(3) 0.30836(17) 0.0573(13) Uani 1 1 d . . . H13C H 0.3934 0.6656 0.3424 0.069 Uiso 1 1 calc R . . C132 C 0.3943(3) 0.7667(3) 0.28774(19) 0.0537(13) Uani 1 1 d . . . H13D H 0.3522 0.7951 0.3074 0.064 Uiso 1 1 calc R . . C133 C 0.4298(3) 0.8027(3) 0.2403(2) 0.0535(12) Uani 1 1 d . . . H13E H 0.4126 0.8561 0.2268 0.064 Uiso 1 1 calc R . . C134 C 0.4908(3) 0.7629(2) 0.21094(17) 0.0412(10) Uani 1 1 d . . . H13F H 0.5171 0.7894 0.1778 0.049 Uiso 1 1 calc R . . C135 C 1.0317(2) 0.6251(2) 0.19270(14) 0.0273(8) Uani 1 1 d . . . C136 C 1.0651(3) 0.5861(2) 0.23966(15) 0.0390(9) Uani 1 1 d . . . H13G H 1.0304 0.5407 0.2590 0.047 Uiso 1 1 calc R . . C137 C 1.1494(3) 0.6135(3) 0.25848(17) 0.0505(12) Uani 1 1 d . . . H13H H 1.1728 0.5861 0.2904 0.061 Uiso 1 1 calc R . . C138 C 1.1990(3) 0.6797(3) 0.23119(19) 0.0493(12) Uani 1 1 d . . . H13I H 1.2555 0.6987 0.2446 0.059 Uiso 1 1 calc R . . C139 C 1.1670(3) 0.7184(3) 0.18479(19) 0.0501(12) Uani 1 1 d . . . H13J H 1.2019 0.7639 0.1658 0.060 Uiso 1 1 calc R . . C140 C 1.0834(3) 0.6912(2) 0.16529(16) 0.0385(9) Uani 1 1 d . . . H14D H 1.0618 0.7181 0.1329 0.046 Uiso 1 1 calc R . . C141 C 0.2563(4) 0.0868(3) 0.7673(2) 0.0738(16) Uani 1 1 d . . . H14A H 0.2504 0.0288 0.7768 0.089 Uiso 1 1 calc R . . H14B H 0.2675 0.1052 0.7989 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.14416(12) 0.12645(10) 0.74337(6) 0.0906(5) Uani 1 1 d . . . Cl2 Cl 0.36028(12) 0.11237(10) 0.72371(6) 0.0898(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0174(2) 0.0224(2) 0.0249(2) -0.00923(17) 0.00024(15) -0.00040(15) Zn2 0.0192(2) 0.0222(2) 0.0280(2) -0.00936(17) 0.00107(16) -0.00013(15) Ni1 0.0238(2) 0.0285(3) 0.0242(2) -0.0038(2) 0.00270(18) 0.00048(18) Ni2 0.0220(2) 0.0268(2) 0.0197(2) -0.00564(19) -0.00144(17) 0.00014(17) Ni3 0.0203(2) 0.0385(3) 0.0215(2) -0.0058(2) -0.00071(18) -0.00186(19) O1 0.0349(16) 0.0439(16) 0.0305(15) -0.0024(12) 0.0118(12) -0.0016(12) O2 0.0300(16) 0.097(3) 0.0290(15) 0.0001(16) -0.0045(13) 0.0002(15) O3 0.0244(14) 0.0572(18) 0.0278(14) -0.0083(13) 0.0031(11) -0.0087(12) O4 0.0313(15) 0.078(2) 0.0283(15) -0.0124(15) -0.0003(12) -0.0100(14) N1 0.0381(19) 0.0317(17) 0.0177(15) -0.0032(13) 0.0009(13) 0.0032(13) N2 0.0284(17) 0.0347(17) 0.0204(15) -0.0069(13) -0.0033(12) 0.0005(13) N3 0.0238(16) 0.0397(18) 0.0297(17) -0.0088(14) -0.0053(13) -0.0013(13) N4 0.0209(15) 0.0271(16) 0.0324(17) -0.0033(13) -0.0031(13) -0.0003(12) N5 0.0213(15) 0.0307(16) 0.0241(16) -0.0099(13) -0.0037(12) -0.0013(12) N6 0.0256(16) 0.0350(17) 0.0193(15) -0.0055(13) -0.0013(12) -0.0019(13) N7 0.0259(16) 0.0316(17) 0.0255(16) -0.0059(14) -0.0040(12) -0.0008(13) N8 0.0249(16) 0.0290(16) 0.0253(16) -0.0074(13) -0.0046(12) 0.0031(12) N9 0.0262(17) 0.0450(19) 0.0235(16) -0.0130(15) -0.0027(13) 0.0046(14) N10 0.0248(16) 0.0282(16) 0.0280(16) -0.0058(13) 0.0018(12) 0.0035(12) N11 0.0253(16) 0.0267(16) 0.0220(15) -0.0038(13) 0.0006(12) 0.0002(12) N12 0.0255(16) 0.0336(17) 0.0245(16) -0.0058(13) -0.0028(12) -0.0059(13) N13 0.0216(15) 0.0256(15) 0.0287(16) -0.0057(13) 0.0019(12) 0.0001(12) N14 0.0251(16) 0.0233(15) 0.0320(17) -0.0048(13) 0.0028(13) 0.0020(12) N15 0.0157(14) 0.0287(16) 0.0294(16) -0.0113(13) -0.0011(12) -0.0027(11) N16 0.0193(15) 0.0244(15) 0.0277(16) -0.0096(13) -0.0008(12) 0.0003(11) N17 0.0196(14) 0.0229(15) 0.0273(16) -0.0106(13) -0.0014(12) 0.0001(11) N18 0.0210(15) 0.0235(15) 0.0245(15) -0.0087(13) 0.0014(12) 0.0001(11) N19 0.0218(15) 0.0236(15) 0.0283(16) -0.0091(13) 0.0012(12) -0.0018(11) N20 0.0216(15) 0.0243(15) 0.0321(17) -0.0094(13) 0.0018(12) -0.0001(11) N21 0.0213(15) 0.0246(15) 0.0306(16) -0.0109(13) -0.0013(12) -0.0002(11) N22 0.0228(15) 0.0216(15) 0.0291(16) -0.0073(13) 0.0001(12) 0.0014(11) C1 0.050(2) 0.030(2) 0.026(2) -0.0033(17) 0.0062(17) 0.0035(17) C2 0.065(3) 0.036(2) 0.027(2) -0.0085(18) 0.002(2) 0.010(2) C3 0.077(3) 0.034(2) 0.026(2) -0.0117(19) -0.007(2) 0.002(2) C4 0.050(2) 0.033(2) 0.028(2) -0.0105(18) -0.0058(18) -0.0017(18) C5 0.038(2) 0.0269(19) 0.0218(19) -0.0043(16) -0.0026(15) 0.0018(16) C6 0.033(2) 0.0273(19) 0.027(2) -0.0062(16) -0.0065(16) -0.0020(15) C7 0.047(3) 0.044(2) 0.029(2) -0.0098(19) -0.0105(18) 0.0042(19) C8 0.052(3) 0.052(3) 0.041(3) -0.014(2) -0.028(2) 0.010(2) C9 0.030(2) 0.056(3) 0.057(3) -0.012(2) -0.017(2) 0.0046(19) C10 0.026(2) 0.052(3) 0.043(2) -0.010(2) -0.0060(18) 0.0017(18) C11 0.028(2) 0.029(2) 0.040(2) 0.0014(18) -0.0046(17) -0.0012(15) C12 0.042(2) 0.032(2) 0.046(3) -0.0036(19) -0.014(2) -0.0115(17) C13 0.053(3) 0.034(2) 0.037(2) -0.0059(19) -0.018(2) -0.0064(19) C14 0.041(2) 0.029(2) 0.027(2) -0.0068(17) -0.0078(16) -0.0005(16) C15 0.0231(19) 0.0308(19) 0.0265(19) -0.0045(16) -0.0078(15) 0.0027(14) C16 0.0293(19) 0.0274(18) 0.0201(18) -0.0082(15) -0.0032(14) 0.0020(14) C17 0.026(2) 0.033(2) 0.030(2) -0.0091(17) -0.0086(15) 0.0003(15) C18 0.035(2) 0.031(2) 0.030(2) -0.0057(17) -0.0083(16) 0.0018(16) C19 0.046(2) 0.036(2) 0.023(2) 0.0016(17) -0.0048(17) -0.0029(18) C20 0.032(2) 0.040(2) 0.028(2) -0.0029(18) -0.0007(16) -0.0030(16) C21 0.033(2) 0.038(2) 0.024(2) -0.0038(17) -0.0013(16) -0.0041(16) C22 0.044(2) 0.036(2) 0.029(2) 0.0066(18) -0.0031(18) -0.0047(18) C23 0.042(2) 0.038(2) 0.038(2) 0.0026(19) -0.0077(19) 0.0047(18) C24 0.034(2) 0.035(2) 0.035(2) -0.0071(18) -0.0061(17) 0.0059(17) C25 0.0277(19) 0.0274(19) 0.0256(19) -0.0059(16) -0.0062(15) -0.0019(15) C26 0.0226(19) 0.037(2) 0.028(2) -0.0114(17) -0.0086(15) 0.0047(15) C27 0.035(2) 0.039(2) 0.038(2) -0.0118(19) -0.0065(18) 0.0047(17) C28 0.050(3) 0.047(3) 0.056(3) -0.028(2) -0.009(2) 0.011(2) C29 0.046(3) 0.070(3) 0.046(3) -0.033(3) 0.002(2) 0.014(2) C30 0.032(2) 0.057(3) 0.035(2) -0.016(2) 0.0027(17) 0.0034(19) C31 0.024(2) 0.036(2) 0.035(2) -0.0067(18) 0.0014(16) 0.0033(15) C32 0.030(2) 0.044(2) 0.051(3) -0.009(2) -0.0063(19) 0.0085(18) C33 0.044(3) 0.038(2) 0.051(3) -0.002(2) -0.010(2) 0.0127(19) C34 0.039(2) 0.033(2) 0.040(2) -0.0015(18) -0.0061(18) -0.0008(17) C35 0.029(2) 0.0266(19) 0.0256(19) -0.0081(16) 0.0000(15) 0.0043(15) C36 0.030(2) 0.032(2) 0.0217(18) -0.0044(16) -0.0003(15) -0.0009(15) C37 0.042(2) 0.040(2) 0.049(3) -0.017(2) 0.0030(19) -0.0031(18) C38 0.054(3) 0.034(2) 0.059(3) -0.016(2) 0.003(2) -0.006(2) C39 0.045(3) 0.043(3) 0.052(3) -0.011(2) -0.003(2) -0.017(2) C40 0.034(2) 0.041(2) 0.035(2) -0.0087(19) -0.0056(17) -0.0092(17) C41 0.022(2) 0.042(2) 0.035(2) -0.0017(18) 0.0034(17) 0.0065(16) C42 0.033(2) 0.037(2) 0.032(2) -0.0092(18) -0.0012(17) -0.0037(16) C43 0.029(2) 0.036(2) 0.036(2) -0.0018(18) 0.0026(16) -0.0087(16) C44 0.0207(18) 0.035(2) 0.0277(19) -0.0069(16) 0.0027(15) 0.0052(15) C45 0.029(2) 0.040(2) 0.032(2) -0.0072(18) -0.0036(16) -0.0056(16) C46 0.029(2) 0.037(2) 0.033(2) -0.0002(18) -0.0059(16) -0.0084(16) C47 0.026(2) 0.045(2) 0.030(2) -0.0059(18) 0.0010(16) 0.0015(17) C48 0.0245(19) 0.0285(19) 0.037(2) -0.0042(17) -0.0020(16) -0.0024(15) C49 0.0233(19) 0.031(2) 0.032(2) -0.0094(17) -0.0027(15) 0.0029(15) C50 0.0202(18) 0.034(2) 0.0284(19) -0.0104(16) 0.0004(14) 0.0003(14) C51 0.030(2) 0.035(2) 0.034(2) -0.0102(18) 0.0025(16) -0.0062(16) C52 0.034(2) 0.0287(19) 0.030(2) -0.0123(17) 0.0011(16) -0.0059(15) C53 0.0234(18) 0.0248(18) 0.0245(18) -0.0123(15) 0.0000(14) 0.0002(14) C54 0.0249(19) 0.0298(19) 0.034(2) -0.0155(17) -0.0012(15) 0.0013(15) C55 0.0218(19) 0.031(2) 0.036(2) -0.0171(17) -0.0036(15) 0.0007(14) C56 0.0210(18) 0.0261(18) 0.0278(19) -0.0112(15) -0.0003(14) -0.0004(14) C57 0.0226(18) 0.0266(18) 0.0247(18) -0.0062(15) -0.0026(14) -0.0038(14) C58 0.0231(18) 0.0241(18) 0.0259(19) -0.0038(15) -0.0022(14) -0.0026(14) C59 0.0191(18) 0.031(2) 0.037(2) -0.0122(17) -0.0008(15) -0.0018(14) C60 0.0198(18) 0.0298(19) 0.040(2) -0.0142(17) 0.0008(15) 0.0028(14) C61 0.0201(18) 0.0266(18) 0.0261(19) -0.0065(15) -0.0006(14) 0.0017(14) C62 0.0230(18) 0.0243(18) 0.0234(18) -0.0059(15) 0.0011(14) 0.0022(14) C63 0.0243(18) 0.0219(17) 0.0221(18) -0.0077(14) 0.0011(14) -0.0008(13) C64 0.028(2) 0.0259(19) 0.031(2) -0.0143(16) -0.0007(15) 0.0025(14) C65 0.0234(19) 0.0271(18) 0.0295(19) -0.0129(16) -0.0012(14) -0.0015(14) C66 0.0226(18) 0.0206(17) 0.0252(18) -0.0074(15) 0.0001(14) -0.0029(13) C67 0.0232(18) 0.0262(18) 0.0221(18) -0.0065(15) -0.0010(14) -0.0039(14) C68 0.0217(18) 0.0268(18) 0.0242(18) -0.0052(15) -0.0025(14) -0.0010(14) C69 0.0172(18) 0.035(2) 0.034(2) -0.0138(17) -0.0012(14) 0.0008(14) C70 0.0218(18) 0.033(2) 0.032(2) -0.0161(17) -0.0002(15) 0.0032(15) C71 0.0189(17) 0.0290(19) 0.0250(18) -0.0089(15) 0.0010(14) 0.0015(14) C72 0.0214(18) 0.0233(17) 0.0251(18) -0.0092(15) -0.0002(14) 0.0014(13) C73 0.0164(17) 0.0299(19) 0.0292(19) -0.0135(16) -0.0027(14) 0.0008(14) C74 0.035(2) 0.029(2) 0.039(2) -0.0029(18) -0.0093(18) -0.0027(16) C75 0.032(2) 0.042(2) 0.045(2) -0.011(2) -0.0168(18) 0.0066(18) C76 0.0180(18) 0.047(2) 0.045(2) -0.029(2) -0.0032(16) 0.0019(16) C77 0.029(2) 0.038(2) 0.037(2) -0.0143(18) 0.0023(17) -0.0109(16) C78 0.029(2) 0.035(2) 0.030(2) -0.0103(17) -0.0033(16) -0.0054(16) C79 0.0182(17) 0.0292(19) 0.0293(19) -0.0122(16) -0.0046(14) 0.0024(14) C80 0.0235(19) 0.031(2) 0.038(2) -0.0116(17) -0.0026(16) -0.0023(15) C81 0.028(2) 0.030(2) 0.052(3) -0.0160(19) -0.0063(18) 0.0070(16) C82 0.0211(19) 0.048(2) 0.049(3) -0.031(2) -0.0094(17) 0.0112(17) C83 0.026(2) 0.054(3) 0.031(2) -0.0162(19) -0.0015(16) 0.0082(18) C84 0.028(2) 0.034(2) 0.032(2) -0.0082(17) -0.0042(16) 0.0066(16) C85 0.0186(17) 0.0243(18) 0.0300(19) -0.0119(16) 0.0000(14) 0.0016(13) C86 0.040(2) 0.070(3) 0.028(2) 0.002(2) -0.0080(18) -0.025(2) C87 0.046(3) 0.076(3) 0.031(2) -0.002(2) -0.0176(19) -0.019(2) C88 0.0203(18) 0.034(2) 0.040(2) -0.0169(18) -0.0049(16) -0.0010(15) C89 0.040(2) 0.037(2) 0.044(2) -0.0022(19) -0.0059(19) -0.0149(18) C90 0.036(2) 0.042(2) 0.035(2) -0.0006(19) -0.0147(18) -0.0090(18) C91 0.0164(17) 0.0319(19) 0.0275(19) -0.0156(16) -0.0038(14) 0.0030(14) C92 0.042(2) 0.031(2) 0.035(2) -0.0116(18) 0.0056(17) 0.0031(17) C93 0.045(3) 0.035(2) 0.054(3) -0.020(2) -0.005(2) 0.0102(18) C94 0.0203(19) 0.055(3) 0.055(3) -0.039(2) -0.0029(18) 0.0047(17) C95 0.030(2) 0.057(3) 0.030(2) -0.020(2) 0.0008(16) -0.0032(18) C96 0.032(2) 0.036(2) 0.032(2) -0.0123(18) -0.0045(16) 0.0035(16) C97 0.0228(18) 0.0241(18) 0.0269(19) -0.0005(15) -0.0001(14) -0.0007(14) C98 0.0205(18) 0.031(2) 0.036(2) -0.0114(17) -0.0004(15) -0.0026(14) C99 0.0234(19) 0.0261(19) 0.035(2) -0.0103(16) -0.0006(15) 0.0015(14) C100 0.0199(18) 0.0245(18) 0.0292(19) -0.0079(15) 0.0029(14) 0.0013(13) C101 0.0221(18) 0.0219(17) 0.0247(18) -0.0055(15) 0.0037(14) 0.0013(13) C102 0.0250(19) 0.0225(17) 0.0262(19) -0.0078(15) 0.0004(14) -0.0021(14) C103 0.028(2) 0.0285(19) 0.030(2) -0.0131(16) 0.0000(15) 0.0029(15) C104 0.0249(19) 0.0258(18) 0.029(2) -0.0095(16) -0.0024(15) 0.0010(14) C105 0.0248(19) 0.0219(17) 0.0257(18) -0.0061(15) -0.0033(14) -0.0041(14) C106 0.0219(18) 0.0235(18) 0.0286(19) -0.0026(15) 0.0007(14) -0.0004(14) C107 0.0226(18) 0.0272(19) 0.031(2) -0.0096(16) -0.0010(15) 0.0003(14) C108 0.0223(19) 0.034(2) 0.043(2) -0.0131(18) -0.0014(16) 0.0016(15) C109 0.0224(19) 0.036(2) 0.043(2) -0.0158(19) 0.0009(16) 0.0057(15) C110 0.0235(19) 0.0266(19) 0.034(2) -0.0112(16) -0.0003(15) 0.0039(14) C111 0.029(2) 0.0242(18) 0.0269(19) -0.0073(15) -0.0006(15) 0.0073(14) C112 0.0254(19) 0.0211(17) 0.0255(18) -0.0078(15) 0.0010(14) 0.0014(14) C113 0.029(2) 0.030(2) 0.030(2) -0.0128(16) -0.0016(15) 0.0043(15) C114 0.0269(19) 0.0264(18) 0.0270(19) -0.0082(16) -0.0018(15) -0.0002(14) C115 0.0257(19) 0.0216(17) 0.0270(19) -0.0071(15) -0.0016(14) -0.0009(14) C116 0.0230(18) 0.0235(18) 0.0265(19) -0.0044(15) -0.0026(14) -0.0041(14) C117 0.0168(17) 0.0273(18) 0.0279(19) -0.0113(16) -0.0002(14) -0.0018(13) C118 0.035(2) 0.027(2) 0.035(2) -0.0083(17) 0.0089(17) 0.0015(16) C119 0.037(2) 0.029(2) 0.048(3) -0.0142(19) 0.0004(19) 0.0049(16) C120 0.024(2) 0.046(2) 0.039(2) -0.029(2) -0.0019(16) 0.0036(16) C121 0.035(2) 0.053(3) 0.028(2) -0.014(2) 0.0031(17) 0.0022(18) C122 0.035(2) 0.032(2) 0.033(2) -0.0072(18) 0.0017(17) 0.0048(16) C123 0.0225(18) 0.0245(18) 0.0271(19) -0.0108(15) -0.0004(14) 0.0022(14) C124 0.033(2) 0.036(2) 0.046(2) 0.0044(19) -0.0105(18) -0.0067(17) C125 0.034(2) 0.059(3) 0.042(2) -0.003(2) -0.0139(19) 0.003(2) C126 0.0190(19) 0.043(2) 0.041(2) -0.0215(19) -0.0006(16) 0.0024(16) C127 0.032(2) 0.038(2) 0.043(2) -0.0084(19) -0.0009(18) -0.0123(17) C128 0.034(2) 0.040(2) 0.034(2) -0.0012(18) -0.0094(17) -0.0096(17) C129 0.0217(19) 0.047(2) 0.035(2) -0.0221(19) -0.0073(16) 0.0051(16) C130 0.039(2) 0.068(3) 0.036(2) -0.015(2) 0.0010(19) 0.013(2) C131 0.041(3) 0.101(4) 0.036(3) -0.030(3) -0.003(2) 0.009(3) C132 0.034(2) 0.083(4) 0.063(3) -0.053(3) -0.014(2) 0.015(2) C133 0.046(3) 0.053(3) 0.074(4) -0.038(3) -0.012(2) 0.013(2) C134 0.037(2) 0.039(2) 0.054(3) -0.023(2) -0.0047(19) 0.0090(18) C135 0.0215(18) 0.0289(19) 0.035(2) -0.0158(17) -0.0007(15) 0.0017(14) C136 0.039(2) 0.039(2) 0.039(2) -0.0077(19) -0.0070(18) -0.0008(18) C137 0.043(3) 0.066(3) 0.050(3) -0.020(2) -0.026(2) 0.010(2) C138 0.028(2) 0.059(3) 0.075(3) -0.041(3) -0.012(2) 0.002(2) C139 0.036(2) 0.044(3) 0.074(3) -0.021(2) 0.000(2) -0.0141(19) C140 0.030(2) 0.038(2) 0.047(2) -0.008(2) -0.0082(18) -0.0059(17) C141 0.071(4) 0.079(4) 0.066(4) -0.004(3) -0.009(3) -0.015(3) Cl1 0.0981(12) 0.0999(12) 0.0909(11) -0.0516(10) -0.0340(9) 0.0288(9) Cl2 0.0832(11) 0.0973(12) 0.0828(11) -0.0071(9) 0.0030(8) -0.0325(9) _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 Zn1 N17 2.063(3) . ? Zn1 N15 2.066(3) . ? Zn1 N16 2.070(3) . ? Zn1 N18 2.082(3) . ? Zn1 N13 2.220(3) . ? Zn2 N20 2.051(3) . ? Zn2 N19 2.059(3) . ? Zn2 N22 2.072(3) . ? Zn2 N21 2.077(3) . ? Zn2 N14 2.179(3) . ? Ni1 O1 2.006(2) . ? Ni1 N10 2.060(3) . ? Ni1 N7 2.097(3) . ? Ni1 N1 2.104(3) . ? Ni1 N4 2.105(3) . ? Ni1 Ni2 2.4212(6) . ? Ni2 N5 1.888(3) . ? Ni2 N2 1.891(3) . ? Ni2 N11 1.895(3) . ? Ni2 N8 1.895(3) . ? Ni2 Ni3 2.4067(6) . ? Ni3 O3 1.977(2) . ? Ni3 N3 2.049(3) . ? Ni3 N6 2.079(3) . ? Ni3 N12 2.086(3) . ? Ni3 N9 2.103(3) . ? O1 C41 1.266(4) . ? O2 C41 1.226(5) . ? O3 C47 1.272(4) . ? O4 C47 1.236(4) . ? N1 C5 1.351(5) . ? N1 C1 1.356(4) . ? N2 C5 1.376(4) . ? N2 C6 1.381(4) . ? N3 C10 1.342(5) . ? N3 C6 1.357(5) . ? N4 C11 1.355(4) . ? N4 C15 1.359(4) . ? N5 C16 1.373(4) . ? N5 C15 1.382(4) . ? N6 C20 1.348(5) . ? N6 C16 1.354(4) . ? N7 C21 1.350(5) . ? N7 C25 1.352(4) . ? N8 C25 1.373(4) . ? N8 C26 1.378(4) . ? N9 C30 1.353(5) . ? N9 C26 1.354(5) . ? N10 C31 1.352(4) . ? N10 C35 1.358(4) . ? N11 C36 1.377(4) . ? N11 C35 1.381(4) . ? N12 C36 1.354(4) . ? N12 C40 1.358(4) . ? N13 C42 1.329(4) . ? N13 C46 1.342(4) . ? N14 C52 1.325(4) . ? N14 C48 1.347(4) . ? N15 C68 1.376(4) . ? N15 C71 1.380(4) . ? N16 C53 1.376(4) . ? N16 C56 1.379(4) . ? N17 C61 1.373(4) . ? N17 C58 1.374(4) . ? N18 C66 1.373(4) . ? N18 C63 1.372(4) . ? N19 C97 1.367(4) . ? N19 C100 1.375(4) . ? N20 C102 1.376(4) . ? N20 C105 1.385(4) . ? N21 C110 1.371(4) . ? N21 C107 1.371(4) . ? N22 C112 1.370(4) . ? N22 C115 1.373(4) . ? C1 C2 1.371(5) . ? C2 C3 1.386(6) . ? C3 C4 1.366(5) . ? C4 C5 1.411(5) . ? C6 C7 1.407(5) . ? C7 C8 1.361(6) . ? C8 C9 1.382(6) . ? C9 C10 1.367(6) . ? C11 C12 1.367(5) . ? C12 C13 1.391(6) . ? C13 C14 1.369(5) . ? C14 C15 1.400(5) . ? C16 C17 1.417(5) . ? C17 C18 1.368(5) . ? C18 C19 1.390(5) . ? C19 C20 1.370(5) . ? C21 C22 1.373(5) . ? C22 C23 1.381(5) . ? C23 C24 1.358(5) . ? C24 C25 1.423(5) . ? C26 C27 1.407(5) . ? C27 C28 1.363(5) . ? C28 C29 1.381(6) . ? C29 C30 1.369(6) . ? C31 C32 1.373(5) . ? C32 C33 1.393(6) . ? C33 C34 1.366(5) . ? C34 C35 1.412(5) . ? C36 C37 1.402(5) . ? C37 C38 1.377(5) . ? C38 C39 1.383(6) . ? C39 C40 1.360(6) . ? C41 C44 1.532(5) . ? C42 C43 1.396(5) . ? C43 C44 1.388(5) . ? C44 C45 1.389(5) . ? C45 C46 1.378(5) . ? C47 C50 1.516(5) . ? C48 C49 1.381(5) . ? C49 C50 1.378(5) . ? C50 C51 1.395(5) . ? C51 C52 1.375(5) . ? C53 C72 1.395(4) . ? C53 C54 1.441(5) . ? C54 C55 1.348(5) . ? C55 C56 1.440(5) . ? C56 C57 1.387(5) . ? C57 C58 1.403(5) . ? C57 C73 1.506(4) . ? C58 C59 1.446(5) . ? C59 C60 1.345(5) . ? C60 C61 1.442(5) . ? C61 C62 1.398(5) . ? C62 C63 1.409(5) . ? C62 C79 1.503(4) . ? C63 C64 1.445(4) . ? C64 C65 1.357(5) . ? C65 C66 1.438(5) . ? C66 C67 1.407(4) . ? C67 C68 1.402(5) . ? C67 C85 1.498(4) . ? C68 C69 1.442(5) . ? C69 C70 1.349(5) . ? C70 C71 1.447(5) . ? C71 C72 1.402(4) . ? C72 C91 1.497(4) . ? C73 C74 1.379(5) . ? C73 C78 1.387(5) . ? C74 C75 1.383(5) . ? C75 C76 1.365(5) . ? C76 C77 1.382(5) . ? C77 C78 1.383(5) . ? C79 C80 1.387(5) . ? C79 C84 1.390(5) . ? C80 C81 1.381(5) . ? C81 C82 1.373(6) . ? C82 C83 1.393(6) . ? C83 C84 1.385(5) . ? C85 C90 1.370(5) . ? C85 C86 1.385(5) . ? C86 C87 1.400(5) . ? C87 C88 1.350(5) . ? C88 C89 1.359(5) . ? C89 C90 1.388(5) . ? C91 C96 1.382(5) . ? C91 C92 1.383(5) . ? C92 C93 1.401(5) . ? C93 C94 1.364(6) . ? C94 C95 1.386(6) . ? C95 C96 1.393(5) . ? C97 C116 1.410(5) . ? C97 C98 1.445(5) . ? C98 C99 1.341(5) . ? C99 C100 1.442(5) . ? C100 C101 1.400(5) . ? C101 C102 1.408(5) . ? C101 C117 1.498(4) . ? C102 C103 1.439(5) . ? C103 C104 1.350(5) . ? C104 C105 1.436(5) . ? C105 C106 1.402(5) . ? C106 C107 1.402(5) . ? C106 C123 1.502(5) . ? C107 C108 1.438(5) . ? C108 C109 1.360(5) . ? C109 C110 1.441(5) . ? C110 C111 1.398(5) . ? C111 C112 1.410(5) . ? C111 C129 1.501(5) . ? C112 C113 1.445(5) . ? C113 C114 1.355(5) . ? C114 C115 1.443(5) . ? C115 C116 1.395(5) . ? C116 C135 1.498(4) . ? C117 C118 1.381(5) . ? C117 C122 1.386(5) . ? C118 C119 1.382(5) . ? C119 C120 1.380(5) . ? C120 C121 1.369(6) . ? C121 C122 1.394(5) . ? C123 C128 1.376(5) . ? C123 C124 1.388(5) . ? C124 C125 1.383(5) . ? C125 C126 1.371(6) . ? C126 C127 1.364(5) . ? C127 C128 1.383(5) . ? C129 C130 1.380(6) . ? C129 C134 1.398(5) . ? C130 C131 1.411(6) . ? C131 C132 1.367(7) . ? C132 C133 1.342(7) . ? C133 C134 1.375(6) . ? C135 C140 1.384(5) . ? C135 C136 1.388(5) . ? C136 C137 1.394(5) . ? C137 C138 1.371(6) . ? C138 C139 1.367(6) . ? C139 C140 1.393(5) . ? C141 Cl1 1.733(5) . ? C141 Cl2 1.740(5) . ? 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 N17 Zn1 N15 162.38(11) . . ? N17 Zn1 N16 88.40(10) . . ? N15 Zn1 N16 88.84(10) . . ? N17 Zn1 N18 88.86(10) . . ? N15 Zn1 N18 88.43(10) . . ? N16 Zn1 N18 162.09(11) . . ? N17 Zn1 N13 93.66(10) . . ? N15 Zn1 N13 103.77(11) . . ? N16 Zn1 N13 107.28(11) . . ? N18 Zn1 N13 90.55(10) . . ? N20 Zn2 N19 89.27(11) . . ? N20 Zn2 N22 163.16(11) . . ? N19 Zn2 N22 89.07(11) . . ? N20 Zn2 N21 88.73(11) . . ? N19 Zn2 N21 166.50(11) . . ? N22 Zn2 N21 88.99(11) . . ? N20 Zn2 N14 106.39(11) . . ? N19 Zn2 N14 102.50(11) . . ? N22 Zn2 N14 90.32(11) . . ? N21 Zn2 N14 90.87(11) . . ? O1 Ni1 N10 102.14(11) . . ? O1 Ni1 N7 92.50(11) . . ? N10 Ni1 N7 165.35(11) . . ? O1 Ni1 N1 88.48(11) . . ? N10 Ni1 N1 91.04(11) . . ? N7 Ni1 N1 88.93(11) . . ? O1 Ni1 N4 106.94(11) . . ? N10 Ni1 N4 85.58(11) . . ? N7 Ni1 N4 90.58(11) . . ? N1 Ni1 N4 164.58(11) . . ? O1 Ni1 Ni2 169.06(8) . . ? N10 Ni1 Ni2 83.08(8) . . ? N7 Ni1 Ni2 82.42(8) . . ? N1 Ni1 Ni2 81.77(8) . . ? N4 Ni1 Ni2 82.89(8) . . ? N5 Ni2 N2 178.39(12) . . ? N5 Ni2 N11 89.73(12) . . ? N2 Ni2 N11 90.78(12) . . ? N5 Ni2 N8 89.31(12) . . ? N2 Ni2 N8 90.20(12) . . ? N11 Ni2 N8 178.74(12) . . ? N5 Ni2 Ni3 89.83(9) . . ? N2 Ni2 Ni3 88.63(9) . . ? N11 Ni2 Ni3 90.33(8) . . ? N8 Ni2 Ni3 90.48(9) . . ? N5 Ni2 Ni1 90.73(9) . . ? N2 Ni2 Ni1 90.81(9) . . ? N11 Ni2 Ni1 89.16(8) . . ? N8 Ni2 Ni1 90.03(9) . . ? Ni3 Ni2 Ni1 179.24(2) . . ? O3 Ni3 N3 101.75(11) . . ? O3 Ni3 N6 91.13(11) . . ? N3 Ni3 N6 166.98(11) . . ? O3 Ni3 N12 101.74(11) . . ? N3 Ni3 N12 91.32(12) . . ? N6 Ni3 N12 87.86(11) . . ? O3 Ni3 N9 92.60(11) . . ? N3 Ni3 N9 88.60(12) . . ? N6 Ni3 N9 88.93(11) . . ? N12 Ni3 N9 165.36(11) . . ? O3 Ni3 Ni2 172.33(7) . . ? N3 Ni3 Ni2 84.09(8) . . ? N6 Ni3 Ni2 82.91(8) . . ? N12 Ni3 Ni2 82.93(8) . . ? N9 Ni3 Ni2 82.49(8) . . ? C41 O1 Ni1 142.8(3) . . ? C47 O3 Ni3 139.5(2) . . ? C5 N1 C1 118.8(3) . . ? C5 N1 Ni1 121.1(2) . . ? C1 N1 Ni1 120.0(3) . . ? C5 N2 C6 122.4(3) . . ? C5 N2 Ni2 119.1(2) . . ? C6 N2 Ni2 118.5(2) . . ? C10 N3 C6 118.5(3) . . ? C10 N3 Ni3 121.2(3) . . ? C6 N3 Ni3 120.0(2) . . ? C11 N4 C15 117.8(3) . . ? C11 N4 Ni1 121.5(2) . . ? C15 N4 Ni1 120.6(2) . . ? C16 N5 C15 122.5(3) . . ? C16 N5 Ni2 119.1(2) . . ? C15 N5 Ni2 118.4(2) . . ? C20 N6 C16 119.0(3) . . ? C20 N6 Ni3 120.7(2) . . ? C16 N6 Ni3 120.2(2) . . ? C21 N7 C25 118.7(3) . . ? C21 N7 Ni1 120.7(2) . . ? C25 N7 Ni1 120.6(2) . . ? C25 N8 C26 122.0(3) . . ? C25 N8 Ni2 118.8(2) . . ? C26 N8 Ni2 119.2(2) . . ? C30 N9 C26 118.2(3) . . ? C30 N9 Ni3 121.0(3) . . ? C26 N9 Ni3 120.7(2) . . ? C31 N10 C35 119.6(3) . . ? C31 N10 Ni1 119.1(2) . . ? C35 N10 Ni1 120.6(2) . . ? C36 N11 C35 122.6(3) . . ? C36 N11 Ni2 119.7(2) . . ? C35 N11 Ni2 117.5(2) . . ? C36 N12 C40 118.5(3) . . ? C36 N12 Ni3 120.5(2) . . ? C40 N12 Ni3 121.0(2) . . ? C42 N13 C46 117.1(3) . . ? C42 N13 Zn1 122.0(2) . . ? C46 N13 Zn1 119.2(2) . . ? C52 N14 C48 116.9(3) . . ? C52 N14 Zn2 119.1(2) . . ? C48 N14 Zn2 120.8(2) . . ? C68 N15 C71 106.6(3) . . ? C68 N15 Zn1 126.6(2) . . ? C71 N15 Zn1 126.6(2) . . ? C53 N16 C56 106.9(3) . . ? C53 N16 Zn1 126.4(2) . . ? C56 N16 Zn1 126.6(2) . . ? C61 N17 C58 106.4(3) . . ? C61 N17 Zn1 125.8(2) . . ? C58 N17 Zn1 127.4(2) . . ? C66 N18 C63 106.7(3) . . ? C66 N18 Zn1 126.0(2) . . ? C63 N18 Zn1 125.0(2) . . ? C97 N19 C100 106.7(3) . . ? C97 N19 Zn2 125.9(2) . . ? C100 N19 Zn2 126.4(2) . . ? C102 N20 C105 106.4(3) . . ? C102 N20 Zn2 126.8(2) . . ? C105 N20 Zn2 126.8(2) . . ? C110 N21 C107 106.7(3) . . ? C110 N21 Zn2 125.0(2) . . ? C107 N21 Zn2 126.6(2) . . ? C112 N22 C115 106.7(3) . . ? C112 N22 Zn2 124.6(2) . . ? C115 N22 Zn2 125.2(2) . . ? N1 C1 C2 122.8(4) . . ? C1 C2 C3 118.1(4) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 118.9(4) . . ? N1 C5 N2 115.8(3) . . ? N1 C5 C4 120.7(3) . . ? N2 C5 C4 123.4(3) . . ? N3 C6 N2 115.6(3) . . ? N3 C6 C7 120.0(3) . . ? N2 C6 C7 124.2(3) . . ? C8 C7 C6 119.6(4) . . ? C7 C8 C9 120.4(4) . . ? C10 C9 C8 117.5(4) . . ? N3 C10 C9 124.0(4) . . ? N4 C11 C12 123.4(4) . . ? C11 C12 C13 118.3(4) . . ? C14 C13 C12 119.7(4) . . ? C13 C14 C15 119.3(4) . . ? N4 C15 N5 115.9(3) . . ? N4 C15 C14 121.2(3) . . ? N5 C15 C14 122.9(3) . . ? N6 C16 N5 115.9(3) . . ? N6 C16 C17 119.6(3) . . ? N5 C16 C17 124.3(3) . . ? C18 C17 C16 120.1(3) . . ? C17 C18 C19 119.6(3) . . ? C20 C19 C18 118.0(4) . . ? N6 C20 C19 123.7(4) . . ? N7 C21 C22 123.2(4) . . ? C21 C22 C23 118.3(4) . . ? C24 C23 C22 120.0(4) . . ? C23 C24 C25 119.6(4) . . ? N7 C25 N8 116.0(3) . . ? N7 C25 C24 120.0(3) . . ? N8 C25 C24 123.8(3) . . ? N9 C26 N8 115.5(3) . . ? N9 C26 C27 120.8(3) . . ? N8 C26 C27 123.6(3) . . ? C28 C27 C26 119.5(4) . . ? C27 C28 C29 119.8(4) . . ? C30 C29 C28 118.6(4) . . ? N9 C30 C29 123.1(4) . . ? N10 C31 C32 123.0(4) . . ? C31 C32 C33 117.6(4) . . ? C34 C33 C32 120.5(4) . . ? C33 C34 C35 119.7(4) . . ? N10 C35 N11 115.8(3) . . ? N10 C35 C34 119.5(3) . . ? N11 C35 C34 124.3(3) . . ? N12 C36 N11 115.9(3) . . ? N12 C36 C37 120.4(3) . . ? N11 C36 C37 123.6(3) . . ? C38 C37 C36 120.0(4) . . ? C37 C38 C39 118.9(4) . . ? C40 C39 C38 119.1(4) . . ? C39 C40 N12 123.1(4) . . ? O2 C41 O1 128.2(4) . . ? O2 C41 C44 117.6(3) . . ? O1 C41 C44 114.2(3) . . ? N13 C42 C43 123.1(3) . . ? C44 C43 C42 119.4(3) . . ? C43 C44 C45 117.2(3) . . ? C43 C44 C41 122.9(3) . . ? C45 C44 C41 119.9(3) . . ? C46 C45 C44 119.7(3) . . ? N13 C46 C45 123.5(3) . . ? O4 C47 O3 128.0(4) . . ? O4 C47 C50 118.3(3) . . ? O3 C47 C50 113.6(3) . . ? N14 C48 C49 123.1(3) . . ? C50 C49 C48 119.4(3) . . ? C49 C50 C51 117.7(3) . . ? C49 C50 C47 120.4(3) . . ? C51 C50 C47 121.8(3) . . ? C52 C51 C50 118.9(3) . . ? N14 C52 C51 124.0(3) . . ? N16 C53 C72 126.4(3) . . ? N16 C53 C54 109.1(3) . . ? C72 C53 C54 124.4(3) . . ? C55 C54 C53 107.4(3) . . ? C54 C55 C56 107.6(3) . . ? N16 C56 C57 126.1(3) . . ? N16 C56 C55 108.9(3) . . ? C57 C56 C55 124.9(3) . . ? C56 C57 C58 125.4(3) . . ? C56 C57 C73 117.8(3) . . ? C58 C57 C73 116.7(3) . . ? N17 C58 C57 125.3(3) . . ? N17 C58 C59 109.7(3) . . ? C57 C58 C59 125.1(3) . . ? C60 C59 C58 106.9(3) . . ? C59 C60 C61 107.5(3) . . ? N17 C61 C62 125.7(3) . . ? N17 C61 C60 109.5(3) . . ? C62 C61 C60 124.7(3) . . ? C61 C62 C63 125.9(3) . . ? C61 C62 C79 117.0(3) . . ? C63 C62 C79 117.1(3) . . ? N18 C63 C62 125.2(3) . . ? N18 C63 C64 109.6(3) . . ? C62 C63 C64 125.2(3) . . ? C65 C64 C63 106.8(3) . . ? C64 C65 C66 107.3(3) . . ? N18 C66 C67 125.3(3) . . ? N18 C66 C65 109.5(3) . . ? C67 C66 C65 125.2(3) . . ? C68 C67 C66 125.4(3) . . ? C68 C67 C85 117.2(3) . . ? C66 C67 C85 117.4(3) . . ? N15 C68 C67 125.8(3) . . ? N15 C68 C69 109.2(3) . . ? C67 C68 C69 125.0(3) . . ? C70 C69 C68 107.9(3) . . ? C69 C70 C71 106.8(3) . . ? N15 C71 C72 125.7(3) . . ? N15 C71 C70 109.5(3) . . ? C72 C71 C70 124.8(3) . . ? C53 C72 C71 125.1(3) . . ? C53 C72 C91 117.1(3) . . ? C71 C72 C91 117.6(3) . . ? C74 C73 C78 118.4(3) . . ? C74 C73 C57 121.0(3) . . ? C78 C73 C57 120.6(3) . . ? C73 C74 C75 120.8(4) . . ? C76 C75 C74 120.4(4) . . ? C75 C76 C77 120.0(3) . . ? C76 C77 C78 119.5(4) . . ? C77 C78 C73 121.0(3) . . ? C80 C79 C84 118.8(3) . . ? C80 C79 C62 121.7(3) . . ? C84 C79 C62 119.6(3) . . ? C81 C80 C79 120.3(4) . . ? C82 C81 C80 120.8(4) . . ? C81 C82 C83 119.7(3) . . ? C84 C83 C82 119.3(4) . . ? C83 C84 C79 121.1(4) . . ? C90 C85 C86 118.1(3) . . ? C90 C85 C67 120.6(3) . . ? C86 C85 C67 121.2(3) . . ? C85 C86 C87 119.9(4) . . ? C88 C87 C86 120.9(4) . . ? C87 C88 C89 119.5(3) . . ? C88 C89 C90 120.5(4) . . ? C85 C90 C89 121.0(3) . . ? C96 C91 C92 118.8(3) . . ? C96 C91 C72 120.3(3) . . ? C92 C91 C72 120.9(3) . . ? C91 C92 C93 120.5(4) . . ? C94 C93 C92 120.0(4) . . ? C93 C94 C95 120.3(3) . . ? C94 C95 C96 119.5(4) . . ? C91 C96 C95 120.9(4) . . ? N19 C97 C116 125.4(3) . . ? N19 C97 C98 109.4(3) . . ? C116 C97 C98 125.2(3) . . ? C99 C98 C97 107.2(3) . . ? C98 C99 C100 107.5(3) . . ? N19 C100 C101 125.4(3) . . ? N19 C100 C99 109.1(3) . . ? C101 C100 C99 125.4(3) . . ? C100 C101 C102 125.3(3) . . ? C100 C101 C117 117.9(3) . . ? C102 C101 C117 116.8(3) . . ? N20 C102 C101 125.6(3) . . ? N20 C102 C103 109.6(3) . . ? C101 C102 C103 124.8(3) . . ? C104 C103 C102 107.2(3) . . ? C103 C104 C105 107.6(3) . . ? N20 C105 C106 125.7(3) . . ? N20 C105 C104 109.2(3) . . ? C106 C105 C104 125.1(3) . . ? C107 C106 C105 125.4(3) . . ? C107 C106 C123 117.2(3) . . ? C105 C106 C123 117.4(3) . . ? N21 C107 C106 125.3(3) . . ? N21 C107 C108 109.8(3) . . ? C106 C107 C108 124.9(3) . . ? C109 C108 C107 106.8(3) . . ? C108 C109 C110 107.1(3) . . ? N21 C110 C111 125.6(3) . . ? N21 C110 C109 109.5(3) . . ? C111 C110 C109 124.8(3) . . ? C110 C111 C112 125.6(3) . . ? C110 C111 C129 117.5(3) . . ? C112 C111 C129 116.9(3) . . ? N22 C112 C111 126.0(3) . . ? N22 C112 C113 109.7(3) . . ? C111 C112 C113 124.2(3) . . ? C114 C113 C112 106.8(3) . . ? C113 C114 C115 107.3(3) . . ? N22 C115 C116 125.8(3) . . ? N22 C115 C114 109.4(3) . . ? C116 C115 C114 124.4(3) . . ? C115 C116 C97 125.7(3) . . ? C115 C116 C135 117.3(3) . . ? C97 C116 C135 117.1(3) . . ? C118 C117 C122 118.3(3) . . ? C118 C117 C101 120.2(3) . . ? C122 C117 C101 121.4(3) . . ? C119 C118 C117 121.1(3) . . ? C118 C119 C120 120.0(4) . . ? C121 C120 C119 119.8(3) . . ? C120 C121 C122 120.1(4) . . ? C117 C122 C121 120.6(4) . . ? C128 C123 C124 117.7(3) . . ? C128 C123 C106 120.9(3) . . ? C124 C123 C106 121.3(3) . . ? C125 C124 C123 120.7(4) . . ? C126 C125 C124 120.5(4) . . ? C127 C126 C125 119.5(3) . . ? C126 C127 C128 120.1(4) . . ? C123 C128 C127 121.5(4) . . ? C130 C129 C134 118.6(4) . . ? C130 C129 C111 120.4(4) . . ? C134 C129 C111 121.0(3) . . ? C129 C130 C131 119.9(4) . . ? C132 C131 C130 119.2(4) . . ? C133 C132 C131 121.4(4) . . ? C132 C133 C134 120.5(5) . . ? C133 C134 C129 120.4(4) . . ? C140 C135 C136 118.9(3) . . ? C140 C135 C116 120.8(3) . . ? C136 C135 C116 120.3(3) . . ? C135 C136 C137 120.0(4) . . ? C138 C137 C136 120.4(4) . . ? C139 C138 C137 120.1(4) . . ? C138 C139 C140 120.1(4) . . ? C135 C140 C139 120.5(4) . . ? Cl1 C141 Cl2 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.204 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.270 data_ic8772 _database_code_CSD 199619 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H80 Cl Mn N18 Ni3 O11' _chemical_formula_weight 1964.33 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 35.1566(2) _cell_length_b 18.0237(1) _cell_length_c 16.1465(1) _cell_angle_alpha 90.00 _cell_angle_beta 114.9287(3) _cell_angle_gamma 90.00 _cell_volume 9278.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36342 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10662 _reflns_number_gt 7733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.1090P)^2^+19.9794P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10662 _refine_ls_number_parameters 615 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1975 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.010 _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 0.039839(13) 0.29646(3) 0.41332(3) 0.02519(16) Uani 1 1 d . . . Ni2 Ni 0.0000 0.29656(3) 0.2500 0.02116(17) Uani 1 2 d S . . Mn1 Mn 0.2500 0.2500 1.0000 0.02210(19) Uani 1 2 d S . . O1 O 0.07877(8) 0.29544(16) 0.54818(18) 0.0350(6) Uani 1 1 d . . . O2 O 0.04102(10) 0.2895(2) 0.6290(2) 0.0605(10) Uani 1 1 d . . . N1 N 0.08542(9) 0.24841(17) 0.3789(2) 0.0275(6) Uani 1 1 d . . . N2 N 0.04972(9) 0.29679(16) 0.23335(19) 0.0247(6) Uani 1 1 d . . . N3 N -0.01383(9) 0.34815(18) 0.40960(19) 0.0274(6) Uani 1 1 d . . . N4 N 0.01145(10) 0.19282(18) 0.4017(2) 0.0320(7) Uani 1 1 d . . . N5 N 0.0000 0.1919(2) 0.2500 0.0280(9) Uani 1 2 d S . . N6 N 0.05967(9) 0.39961(17) 0.38604(19) 0.0269(6) Uani 1 1 d . . . N7 N 0.0000 0.4013(2) 0.2500 0.0237(8) Uani 1 2 d S . . N8 N 0.18915(9) 0.27513(18) 0.8660(2) 0.0275(6) Uani 1 1 d . . . N9 N 0.28483(9) 0.25835(16) 0.92862(18) 0.0241(6) Uani 1 1 d . . . N10 N 0.23879(9) 0.14276(16) 0.96255(19) 0.0257(6) Uani 1 1 d . . . C1 C 0.11682(12) 0.2067(2) 0.4397(3) 0.0343(9) Uani 1 1 d . . . H1A H 0.1175 0.1995 0.4986 0.041 Uiso 1 1 calc R . . C2 C 0.14761(13) 0.1744(3) 0.4213(3) 0.0406(10) Uani 1 1 d . . . H2A H 0.1695 0.1466 0.4666 0.049 Uiso 1 1 calc R . . C3 C 0.14602(13) 0.1833(3) 0.3343(3) 0.0400(10) Uani 1 1 d . . . H3A H 0.1667 0.1612 0.3189 0.048 Uiso 1 1 calc R . . C4 C 0.11404(11) 0.2248(2) 0.2709(3) 0.0322(8) Uani 1 1 d . . . H4A H 0.1125 0.2308 0.2111 0.039 Uiso 1 1 calc R . . C5 C 0.08391(11) 0.2579(2) 0.2940(2) 0.0261(7) Uani 1 1 d . . . C6 C -0.05113(10) 0.3392(2) 0.3360(2) 0.0255(7) Uani 1 1 d . . . C7 C -0.08721(11) 0.3772(2) 0.3304(3) 0.0316(8) Uani 1 1 d . . . H7A H -0.1133 0.3706 0.2789 0.038 Uiso 1 1 calc R . . C8 C -0.08439(12) 0.4237(3) 0.3997(3) 0.0411(10) Uani 1 1 d . . . H8A H -0.1086 0.4489 0.3972 0.049 Uiso 1 1 calc R . . C9 C -0.04601(13) 0.4337(3) 0.4735(3) 0.0433(10) Uani 1 1 d . . . H9A H -0.0434 0.4661 0.5220 0.052 Uiso 1 1 calc R . . C10 C -0.01202(12) 0.3959(2) 0.4752(3) 0.0356(9) Uani 1 1 d . . . H10A H 0.0143 0.4038 0.5253 0.043 Uiso 1 1 calc R . . C11 C 0.00474(13) 0.1633(3) 0.4716(3) 0.0402(10) Uani 1 1 d . . . H11A H 0.0144 0.1901 0.5274 0.048 Uiso 1 1 calc R . . C12 C -0.01516(17) 0.0974(3) 0.4661(4) 0.0566(13) Uani 1 1 d . . . H12A H -0.0190 0.0785 0.5170 0.068 Uiso 1 1 calc R . . C13 C -0.02956(18) 0.0586(3) 0.3847(4) 0.0611(14) Uani 1 1 d . . . H13A H -0.0432 0.0122 0.3796 0.073 Uiso 1 1 calc R . . C14 C -0.02424(15) 0.0868(2) 0.3111(3) 0.0468(11) Uani 1 1 d . . . H14A H -0.0343 0.0606 0.2548 0.056 Uiso 1 1 calc R . . C15 C -0.00347(11) 0.1557(2) 0.3211(3) 0.0313(8) Uani 1 1 d . . . C16 C 0.09824(11) 0.4270(2) 0.4406(3) 0.0350(9) Uani 1 1 d . . . H16A H 0.1156 0.3995 0.4932 0.042 Uiso 1 1 calc R . . C17 C 0.11305(13) 0.4924(3) 0.4226(3) 0.0436(10) Uani 1 1 d . . . H17A H 0.1401 0.5101 0.4622 0.052 Uiso 1 1 calc R . . C18 C 0.08806(14) 0.5323(3) 0.3462(3) 0.0459(11) Uani 1 1 d . . . H18A H 0.0978 0.5781 0.3332 0.055 Uiso 1 1 calc R . . C19 C 0.04908(13) 0.5060(2) 0.2885(3) 0.0370(9) Uani 1 1 d . . . H19A H 0.0316 0.5334 0.2359 0.044 Uiso 1 1 calc R . . C20 C 0.03554(11) 0.4377(2) 0.3088(2) 0.0262(7) Uani 1 1 d . . . C21 C 0.07436(13) 0.2895(2) 0.6198(3) 0.0380(9) Uani 1 1 d . . . C22 C 0.11519(12) 0.2834(2) 0.7060(3) 0.0302(8) Uani 1 1 d . . . C23 C 0.15341(12) 0.2765(2) 0.7023(3) 0.0355(9) Uani 1 1 d . . . H23A H 0.1552 0.2747 0.6452 0.043 Uiso 1 1 calc R . . C24 C 0.18940(12) 0.2721(2) 0.7837(3) 0.0341(8) Uani 1 1 d . . . H24A H 0.2156 0.2667 0.7806 0.041 Uiso 1 1 calc R . . C25 C 0.11422(13) 0.2842(2) 0.7910(3) 0.0370(9) Uani 1 1 d . . . H25A H 0.0883 0.2873 0.7959 0.044 Uiso 1 1 calc R . . C26 C 0.15167(12) 0.2805(2) 0.8683(3) 0.0357(9) Uani 1 1 d . . . H26A H 0.1507 0.2819 0.9262 0.043 Uiso 1 1 calc R . . C27 C 0.30700(11) 0.3199(2) 0.9238(2) 0.0276(7) Uani 1 1 d . . . C28 C 0.33023(13) 0.3025(2) 0.8716(3) 0.0378(9) Uani 1 1 d . . . H28A H 0.3482 0.3351 0.8583 0.045 Uiso 1 1 calc R . . C29 C 0.32185(13) 0.2310(2) 0.8449(3) 0.0389(9) Uani 1 1 d . . . H29A H 0.3330 0.2039 0.8098 0.047 Uiso 1 1 calc R . . C30 C 0.29307(11) 0.2036(2) 0.8791(2) 0.0274(7) Uani 1 1 d . . . C31 C 0.27660(11) 0.1318(2) 0.8637(2) 0.0276(7) Uani 1 1 d . . . C32 C 0.25102(11) 0.1041(2) 0.9033(2) 0.0272(7) Uani 1 1 d . . . C33 C 0.23254(13) 0.0310(2) 0.8870(3) 0.0360(9) Uani 1 1 d . . . H33A H 0.2357 -0.0061 0.8486 0.043 Uiso 1 1 calc R . . C34 C 0.20980(13) 0.0251(2) 0.9367(3) 0.0383(9) Uani 1 1 d . . . H34A H 0.1945 -0.0172 0.9405 0.046 Uiso 1 1 calc R . . C35 C 0.21310(11) 0.0949(2) 0.9827(2) 0.0300(8) Uani 1 1 d . . . C36 C 0.19198(11) 0.1112(2) 1.0367(3) 0.0303(8) Uani 1 1 d . . . C37 C 0.28568(12) 0.0831(2) 0.7990(3) 0.0332(8) Uani 1 1 d . . . C38 C 0.27538(17) 0.1064(3) 0.7099(3) 0.0509(12) Uani 1 1 d . . . H38A H 0.2620 0.1530 0.6899 0.061 Uiso 1 1 calc R . . C39 C 0.2843(2) 0.0625(3) 0.6502(4) 0.0705(17) Uani 1 1 d . . . H39A H 0.2778 0.0799 0.5901 0.085 Uiso 1 1 calc R . . C40 C 0.30254(19) -0.0059(3) 0.6763(4) 0.0656(16) Uani 1 1 d . . . H40A H 0.3081 -0.0363 0.6345 0.079 Uiso 1 1 calc R . . C41 C 0.31266(15) -0.0298(3) 0.7641(4) 0.0560(13) Uani 1 1 d . . . H41A H 0.3255 -0.0770 0.7831 0.067 Uiso 1 1 calc R . . C42 C 0.30439(13) 0.0138(2) 0.8252(3) 0.0409(10) Uani 1 1 d . . . H42A H 0.3115 -0.0036 0.8854 0.049 Uiso 1 1 calc R . . C43 C 0.16568(13) 0.0510(2) 1.0516(3) 0.0363(9) Uani 1 1 d . . . C44 C 0.18210(18) 0.0082(3) 1.1296(3) 0.0605(14) Uani 1 1 d . . . H44A H 0.2101 0.0160 1.1735 0.073 Uiso 1 1 calc R . . C45 C 0.1574(2) -0.0466(4) 1.1439(4) 0.0768(18) Uani 1 1 d . . . H45A H 0.1689 -0.0757 1.1979 0.092 Uiso 1 1 calc R . . C46 C 0.11767(19) -0.0589(3) 1.0825(4) 0.0645(16) Uani 1 1 d . . . H46A H 0.1014 -0.0966 1.0932 0.077 Uiso 1 1 calc R . . C47 C 0.10087(17) -0.0168(3) 1.0048(5) 0.0662(16) Uani 1 1 d . . . H47A H 0.0728 -0.0253 0.9616 0.079 Uiso 1 1 calc R . . C48 C 0.12470(15) 0.0384(3) 0.9884(4) 0.0566(13) Uani 1 1 d . . . H48A H 0.1129 0.0673 0.9343 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.26934(6) 0.17500(11) 0.40889(14) 0.0376(4) Uani 0.50 1 d P . . O3 O 0.2439(2) 0.1484(5) 0.3263(5) 0.071(2) Uani 0.50 1 d P . . O4 O 0.2773(3) 0.2457(4) 0.3925(6) 0.072(2) Uani 0.50 1 d P . . O5 O 0.30696(19) 0.1343(4) 0.4570(6) 0.065(2) Uani 0.50 1 d P . . O6 O 0.24719(18) 0.1733(4) 0.4592(5) 0.0539(17) Uani 0.50 1 d P . . O7 O 0.0255(5) 0.1037(10) 0.7705(13) 0.182(7) Uiso 0.50 1 d PD . . H7 H 0.0414 0.1231 0.8210 0.273 Uiso 0.50 1 d P . . C49 C 0.0619(5) 0.1104(9) 0.7491(11) 0.194(4) Uiso 0.50 1 d PD . . H49A H 0.0787 0.0642 0.7666 0.291 Uiso 0.50 1 d P . . H49B H 0.0800 0.1517 0.7841 0.291 Uiso 0.50 1 d P . . H49C H 0.0531 0.1192 0.6840 0.291 Uiso 0.50 1 d P . . O8 O -0.0356(3) 0.2697(6) 0.6344(7) 0.205(4) Uiso 1 1 d D . . H8 H -0.0273 0.3124 0.6406 0.308 Uiso 1 1 d . . . C50 C -0.0683(2) 0.2570(4) 0.5424(5) 0.189(2) Uiso 1 1 d D . . H50A H -0.0903 0.2943 0.5292 0.283 Uiso 1 1 d . . . H50B H -0.0803 0.2073 0.5374 0.283 Uiso 1 1 d . . . H50C H -0.0560 0.2620 0.4980 0.283 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0221(2) 0.0351(3) 0.0178(2) 0.00227(17) 0.00777(18) 0.00331(18) Ni2 0.0198(3) 0.0259(3) 0.0180(3) 0.000 0.0083(2) 0.000 Mn1 0.0234(4) 0.0253(4) 0.0181(3) -0.0006(3) 0.0092(3) 0.0005(3) O1 0.0253(13) 0.0500(18) 0.0303(14) 0.0124(12) 0.0122(11) 0.0074(11) O2 0.0307(16) 0.117(3) 0.0316(16) 0.0102(18) 0.0106(13) 0.0032(17) N1 0.0259(15) 0.0318(16) 0.0248(15) 0.0025(12) 0.0107(12) 0.0042(12) N2 0.0225(14) 0.0303(16) 0.0225(14) 0.0007(12) 0.0105(12) 0.0012(11) N3 0.0252(14) 0.0369(17) 0.0209(14) -0.0004(12) 0.0103(12) 0.0004(12) N4 0.0309(16) 0.0363(18) 0.0307(16) 0.0096(14) 0.0149(14) 0.0058(13) N5 0.027(2) 0.031(2) 0.027(2) 0.000 0.0113(18) 0.000 N6 0.0222(14) 0.0367(17) 0.0199(14) -0.0036(12) 0.0070(12) 0.0007(12) N7 0.0234(19) 0.025(2) 0.0188(18) 0.000 0.0055(16) 0.000 N8 0.0263(15) 0.0318(16) 0.0221(14) 0.0023(12) 0.0080(12) 0.0034(12) N9 0.0238(14) 0.0291(16) 0.0185(13) -0.0006(11) 0.0081(11) 0.0006(12) N10 0.0288(15) 0.0267(15) 0.0235(14) 0.0010(12) 0.0129(12) 0.0015(12) C1 0.033(2) 0.039(2) 0.0273(18) 0.0069(16) 0.0098(16) 0.0084(16) C2 0.035(2) 0.046(2) 0.038(2) 0.0099(19) 0.0135(18) 0.0171(18) C3 0.033(2) 0.050(3) 0.041(2) 0.0034(19) 0.0200(18) 0.0162(18) C4 0.0278(18) 0.042(2) 0.0286(18) -0.0002(16) 0.0137(15) 0.0037(16) C5 0.0237(16) 0.0284(19) 0.0253(17) -0.0001(14) 0.0096(14) 0.0009(14) C6 0.0249(16) 0.0304(19) 0.0225(16) 0.0012(14) 0.0113(14) -0.0013(14) C7 0.0228(17) 0.041(2) 0.0292(18) -0.0017(16) 0.0096(15) 0.0035(15) C8 0.030(2) 0.053(3) 0.042(2) -0.010(2) 0.0166(18) 0.0052(18) C9 0.039(2) 0.057(3) 0.034(2) -0.018(2) 0.0157(18) 0.004(2) C10 0.0311(19) 0.050(2) 0.0237(18) -0.0090(17) 0.0098(15) 0.0001(17) C11 0.043(2) 0.047(3) 0.035(2) 0.0130(19) 0.0207(18) 0.0051(19) C12 0.074(3) 0.053(3) 0.054(3) 0.016(2) 0.038(3) -0.004(3) C13 0.080(4) 0.044(3) 0.070(3) 0.014(3) 0.042(3) -0.014(3) C14 0.054(3) 0.036(2) 0.054(3) 0.005(2) 0.027(2) -0.005(2) C15 0.0320(19) 0.0279(19) 0.036(2) 0.0080(16) 0.0166(16) 0.0034(15) C16 0.0280(18) 0.047(2) 0.0273(18) -0.0083(17) 0.0094(16) -0.0029(17) C17 0.030(2) 0.059(3) 0.036(2) -0.010(2) 0.0087(17) -0.0163(19) C18 0.048(2) 0.042(2) 0.044(2) -0.004(2) 0.015(2) -0.018(2) C19 0.040(2) 0.033(2) 0.035(2) 0.0026(17) 0.0129(17) -0.0043(17) C20 0.0275(17) 0.0294(19) 0.0228(16) -0.0035(14) 0.0116(14) -0.0011(14) C21 0.031(2) 0.051(3) 0.0268(19) 0.0020(17) 0.0072(16) 0.0021(18) C22 0.0287(19) 0.034(2) 0.0238(17) 0.0039(15) 0.0074(15) 0.0022(15) C23 0.036(2) 0.044(2) 0.0258(18) 0.0040(17) 0.0122(16) 0.0011(17) C24 0.0302(19) 0.046(2) 0.0263(18) 0.0043(17) 0.0121(16) 0.0023(17) C25 0.030(2) 0.051(3) 0.0281(19) 0.0039(18) 0.0109(16) 0.0053(17) C26 0.034(2) 0.051(2) 0.0211(17) 0.0013(17) 0.0104(16) 0.0050(18) C27 0.0275(17) 0.0317(19) 0.0246(17) 0.0015(15) 0.0120(14) 0.0006(15) C28 0.042(2) 0.038(2) 0.045(2) -0.0049(18) 0.030(2) -0.0057(17) C29 0.044(2) 0.038(2) 0.048(2) -0.0083(19) 0.032(2) -0.0044(18) C30 0.0255(17) 0.0320(19) 0.0254(17) -0.0002(14) 0.0114(15) 0.0019(14) C31 0.0273(17) 0.0312(19) 0.0239(17) -0.0015(14) 0.0105(14) 0.0017(14) C32 0.0296(18) 0.0287(19) 0.0219(16) -0.0012(14) 0.0093(14) 0.0022(14) C33 0.044(2) 0.034(2) 0.037(2) -0.0081(17) 0.0239(18) -0.0041(17) C34 0.052(2) 0.029(2) 0.044(2) -0.0072(17) 0.030(2) -0.0084(18) C35 0.0346(19) 0.0283(19) 0.0295(18) -0.0008(15) 0.0158(16) -0.0023(15) C36 0.0343(19) 0.031(2) 0.0296(18) -0.0022(15) 0.0169(16) -0.0032(15) C37 0.037(2) 0.036(2) 0.0327(19) -0.0063(16) 0.0202(17) -0.0037(16) C38 0.077(3) 0.044(3) 0.043(2) -0.001(2) 0.035(2) 0.003(2) C39 0.114(5) 0.068(4) 0.051(3) -0.018(3) 0.056(3) -0.015(3) C40 0.084(4) 0.060(3) 0.080(4) -0.032(3) 0.062(3) -0.015(3) C41 0.047(3) 0.043(3) 0.081(4) -0.021(3) 0.030(3) 0.001(2) C42 0.037(2) 0.037(2) 0.049(2) -0.0093(19) 0.0178(19) -0.0001(17) C43 0.044(2) 0.031(2) 0.045(2) -0.0092(17) 0.0297(19) -0.0070(17) C44 0.072(3) 0.062(3) 0.044(3) 0.008(2) 0.022(2) -0.024(3) C45 0.102(5) 0.067(4) 0.067(4) 0.009(3) 0.041(4) -0.034(3) C46 0.082(4) 0.050(3) 0.091(4) -0.023(3) 0.065(4) -0.029(3) C47 0.046(3) 0.056(3) 0.104(5) -0.019(3) 0.039(3) -0.017(2) C48 0.041(2) 0.048(3) 0.079(4) 0.002(3) 0.023(2) -0.006(2) Cl1 0.0318(9) 0.0339(10) 0.0499(11) 0.0033(9) 0.0201(9) 0.0049(8) O3 0.035(3) 0.124(7) 0.042(4) 0.033(4) 0.006(3) 0.030(4) O4 0.073(5) 0.035(4) 0.082(5) 0.006(3) 0.009(4) -0.001(3) O5 0.034(3) 0.057(4) 0.107(6) 0.024(4) 0.032(4) 0.019(3) O6 0.032(3) 0.081(5) 0.052(4) 0.023(4) 0.021(3) 0.016(3) _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 O1 2.025(3) . ? Ni1 N3 2.082(3) . ? Ni1 N4 2.089(3) . ? Ni1 N1 2.093(3) . ? Ni1 N6 2.096(3) . ? Ni1 Ni2 2.4088(4) . ? Ni2 N2 1.877(3) . ? Ni2 N2 1.877(3) 2 ? Ni2 N5 1.886(4) . ? Ni2 N7 1.888(4) . ? Ni2 Ni1 2.4088(4) 2 ? Mn1 N9 2.010(3) . ? Mn1 N9 2.010(3) 7_557 ? Mn1 N10 2.014(3) . ? Mn1 N10 2.014(3) 7_557 ? Mn1 N8 2.358(3) 7_557 ? Mn1 N8 2.358(3) . ? O1 C21 1.235(5) . ? O2 C21 1.242(5) . ? N1 C1 1.355(5) . ? N1 C5 1.360(5) . ? N2 C6 1.373(4) 2 ? N2 C5 1.380(4) . ? N3 C10 1.345(5) . ? N3 C6 1.358(4) . ? N4 C11 1.354(5) . ? N4 C15 1.357(5) . ? N5 C15 1.371(4) 2 ? N5 C15 1.371(4) . ? N6 C16 1.360(5) . ? N6 C20 1.361(5) . ? N7 C20 1.376(4) . ? N7 C20 1.376(4) 2 ? N8 C24 1.333(5) . ? N8 C26 1.337(5) . ? N9 C30 1.376(5) . ? N9 C27 1.377(5) . ? N10 C35 1.383(5) . ? N10 C32 1.390(4) . ? C1 C2 1.368(6) . ? C2 C3 1.390(6) . ? C3 C4 1.379(6) . ? C4 C5 1.397(5) . ? C6 N2 1.373(4) 2 ? C6 C7 1.411(5) . ? C7 C8 1.366(6) . ? C8 C9 1.385(6) . ? C9 C10 1.366(6) . ? C11 C12 1.364(7) . ? C12 C13 1.383(8) . ? C13 C14 1.377(7) . ? C14 C15 1.415(6) . ? C16 C17 1.370(6) . ? C17 C18 1.377(6) . ? C18 C19 1.376(6) . ? C19 C20 1.407(5) . ? C21 C22 1.524(5) . ? C22 C23 1.376(6) . ? C22 C25 1.387(5) . ? C23 C24 1.391(5) . ? C25 C26 1.382(5) . ? C27 C36 1.390(5) 7_557 ? C27 C28 1.433(5) . ? C28 C29 1.351(6) . ? C29 C30 1.430(5) . ? C30 C31 1.397(5) . ? C31 C32 1.396(5) . ? C31 C37 1.498(5) . ? C32 C33 1.444(5) . ? C33 C34 1.354(5) . ? C34 C35 1.440(5) . ? C35 C36 1.395(5) . ? C36 C27 1.390(5) 7_557 ? C36 C43 1.510(5) . ? C37 C42 1.391(6) . ? C37 C38 1.393(6) . ? C38 C39 1.382(7) . ? C39 C40 1.371(9) . ? C40 C41 1.378(8) . ? C41 C42 1.385(6) . ? C43 C44 1.379(7) . ? C43 C48 1.389(6) . ? C44 C45 1.396(7) . ? C45 C46 1.348(9) . ? C46 C47 1.369(9) . ? C47 C48 1.396(7) . ? Cl1 O6 1.342(6) . ? Cl1 O3 1.344(8) . ? Cl1 O4 1.355(7) . ? Cl1 O5 1.423(6) . ? O7 C49 1.464(9) . ? O7 O7 1.63(3) 2_556 ? O8 C50 1.464(8) . ? 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 O1 Ni1 N3 103.21(11) . . ? O1 Ni1 N4 99.73(12) . . ? N3 Ni1 N4 90.26(12) . . ? O1 Ni1 N1 92.06(11) . . ? N3 Ni1 N1 164.49(11) . . ? N4 Ni1 N1 89.80(12) . . ? O1 Ni1 N6 95.75(11) . . ? N3 Ni1 N6 88.55(12) . . ? N4 Ni1 N6 164.33(12) . . ? N1 Ni1 N6 87.22(12) . . ? O1 Ni1 Ni2 174.01(8) . . ? N3 Ni1 Ni2 82.32(8) . . ? N4 Ni1 Ni2 82.36(9) . . ? N1 Ni1 Ni2 82.31(8) . . ? N6 Ni1 Ni2 81.99(8) . . ? N2 Ni2 N2 179.75(19) . 2 ? N2 Ni2 N5 90.13(9) . . ? N2 Ni2 N5 90.13(9) 2 . ? N2 Ni2 N7 89.87(9) . . ? N2 Ni2 N7 89.87(9) 2 . ? N5 Ni2 N7 180.000(1) . . ? N2 Ni2 Ni1 89.43(9) . 2 ? N2 Ni2 Ni1 90.57(9) 2 2 ? N5 Ni2 Ni1 89.958(18) . 2 ? N7 Ni2 Ni1 90.042(18) . 2 ? N2 Ni2 Ni1 90.57(9) . . ? N2 Ni2 Ni1 89.43(9) 2 . ? N5 Ni2 Ni1 89.958(18) . . ? N7 Ni2 Ni1 90.042(18) . . ? Ni1 Ni2 Ni1 179.92(4) 2 . ? N9 Mn1 N9 180.00(9) . 7_557 ? N9 Mn1 N10 89.38(12) . . ? N9 Mn1 N10 90.62(12) 7_557 . ? N9 Mn1 N10 90.62(12) . 7_557 ? N9 Mn1 N10 89.38(12) 7_557 7_557 ? N10 Mn1 N10 180.0 . 7_557 ? N9 Mn1 N8 90.23(11) . 7_557 ? N9 Mn1 N8 89.77(11) 7_557 7_557 ? N10 Mn1 N8 94.48(11) . 7_557 ? N10 Mn1 N8 85.52(11) 7_557 7_557 ? N9 Mn1 N8 89.77(11) . . ? N9 Mn1 N8 90.23(11) 7_557 . ? N10 Mn1 N8 85.52(11) . . ? N10 Mn1 N8 94.48(11) 7_557 . ? N8 Mn1 N8 180.000(1) 7_557 . ? C21 O1 Ni1 135.5(3) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Ni1 121.2(2) . . ? C5 N1 Ni1 120.5(2) . . ? C6 N2 C5 122.8(3) 2 . ? C6 N2 Ni2 118.3(2) 2 . ? C5 N2 Ni2 118.9(2) . . ? C10 N3 C6 118.2(3) . . ? C10 N3 Ni1 121.5(2) . . ? C6 N3 Ni1 120.1(2) . . ? C11 N4 C15 118.2(4) . . ? C11 N4 Ni1 121.4(3) . . ? C15 N4 Ni1 120.3(2) . . ? C15 N5 C15 123.0(5) 2 . ? C15 N5 Ni2 118.5(2) 2 . ? C15 N5 Ni2 118.5(2) . . ? C16 N6 C20 118.4(3) . . ? C16 N6 Ni1 121.0(3) . . ? C20 N6 Ni1 120.4(2) . . ? C20 N7 C20 123.1(4) . 2 ? C20 N7 Ni2 118.4(2) . . ? C20 N7 Ni2 118.4(2) 2 . ? C24 N8 C26 116.8(3) . . ? C24 N8 Mn1 121.5(2) . . ? C26 N8 Mn1 120.8(2) . . ? C30 N9 C27 106.4(3) . . ? C30 N9 Mn1 127.4(2) . . ? C27 N9 Mn1 126.1(2) . . ? C35 N10 C32 105.8(3) . . ? C35 N10 Mn1 126.3(2) . . ? C32 N10 Mn1 127.5(2) . . ? N1 C1 C2 123.8(4) . . ? C1 C2 C3 118.2(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 120.4(4) . . ? N1 C5 N2 115.5(3) . . ? N1 C5 C4 120.3(3) . . ? N2 C5 C4 124.0(3) . . ? N3 C6 N2 115.2(3) . 2 ? N3 C6 C7 120.6(3) . . ? N2 C6 C7 124.0(3) 2 . ? C8 C7 C6 119.5(3) . . ? C7 C8 C9 119.5(4) . . ? C10 C9 C8 118.6(4) . . ? N3 C10 C9 123.6(3) . . ? N4 C11 C12 123.6(4) . . ? C11 C12 C13 118.3(4) . . ? C14 C13 C12 120.4(5) . . ? C13 C14 C15 118.4(5) . . ? N4 C15 N5 115.7(3) . . ? N4 C15 C14 121.0(4) . . ? N5 C15 C14 123.1(4) . . ? N6 C16 C17 122.6(4) . . ? C16 C17 C18 118.9(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 118.8(4) . . ? N6 C20 N7 115.2(3) . . ? N6 C20 C19 120.9(3) . . ? N7 C20 C19 123.6(3) . . ? O1 C21 O2 127.6(4) . . ? O1 C21 C22 114.8(4) . . ? O2 C21 C22 117.6(4) . . ? C23 C22 C25 118.4(3) . . ? C23 C22 C21 121.9(4) . . ? C25 C22 C21 119.7(4) . . ? C22 C23 C24 118.7(4) . . ? N8 C24 C23 123.7(4) . . ? C26 C25 C22 118.8(4) . . ? N8 C26 C25 123.6(4) . . ? N9 C27 C36 126.8(3) . 7_557 ? N9 C27 C28 109.5(3) . . ? C36 C27 C28 123.7(3) 7_557 . ? C29 C28 C27 107.1(3) . . ? C28 C29 C30 107.5(3) . . ? N9 C30 C31 126.6(3) . . ? N9 C30 C29 109.4(3) . . ? C31 C30 C29 124.0(3) . . ? C32 C31 C30 123.2(3) . . ? C32 C31 C37 118.6(3) . . ? C30 C31 C37 118.2(3) . . ? N10 C32 C31 125.6(3) . . ? N10 C32 C33 109.7(3) . . ? C31 C32 C33 124.7(3) . . ? C34 C33 C32 107.2(3) . . ? C33 C34 C35 107.3(3) . . ? N10 C35 C36 126.0(3) . . ? N10 C35 C34 110.0(3) . . ? C36 C35 C34 124.0(3) . . ? C27 C36 C35 123.9(3) 7_557 . ? C27 C36 C43 117.9(3) 7_557 . ? C35 C36 C43 118.1(3) . . ? C42 C37 C38 117.9(4) . . ? C42 C37 C31 121.8(4) . . ? C38 C37 C31 120.4(4) . . ? C39 C38 C37 120.8(5) . . ? C40 C39 C38 120.9(5) . . ? C39 C40 C41 118.8(5) . . ? C40 C41 C42 121.0(5) . . ? C41 C42 C37 120.5(4) . . ? C44 C43 C48 119.0(4) . . ? C44 C43 C36 119.9(4) . . ? C48 C43 C36 121.1(4) . . ? C43 C44 C45 119.8(5) . . ? C46 C45 C44 121.2(6) . . ? C45 C46 C47 119.7(5) . . ? C46 C47 C48 120.4(5) . . ? C43 C48 C47 119.8(5) . . ? O6 Cl1 O3 106.2(4) . . ? O6 Cl1 O4 111.1(5) . . ? O3 Cl1 O4 104.4(5) . . ? O6 Cl1 O5 107.5(4) . . ? O3 Cl1 O5 115.8(5) . . ? O4 Cl1 O5 111.7(5) . . ? C49 O7 O7 146(2) . 2_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.471 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.246 data_ic9386 _database_code_CSD 199620 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H84 Cl4 Mn N18 Ni3 O9.50' _chemical_formula_weight 2098.75 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' Mn Mn 0.3368 0.7283 '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 P2(1)/c 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 21.3217(2) _cell_length_b 24.9858(2) _cell_length_c 18.0492(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.3679(5) _cell_angle_gamma 90.00 _cell_volume 9487.29(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4324 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58673 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21661 _reflns_number_gt 15231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0817P)^2^+7.0188P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00408(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 21661 _refine_ls_number_parameters 1253 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 -0.384791(18) 0.162891(16) 0.18828(2) 0.02094(11) Uani 1 1 d . . . Ni2 Ni -0.273525(17) 0.172702(16) 0.23981(2) 0.01953(11) Uani 1 1 d . . . Ni3 Ni -0.161922(18) 0.185387(17) 0.28877(2) 0.02295(11) Uani 1 1 d . . . Mn1 Mn 0.22866(2) 0.257253(19) 0.49310(2) 0.02066(12) Uani 1 1 d . . . O1 O 0.52168(10) 0.34712(9) 0.65549(12) 0.0274(5) Uani 1 1 d . . . O2 O 0.48955(11) 0.31231(11) 0.54021(13) 0.0375(6) Uani 1 1 d . . . O3 O -0.06823(10) 0.18896(10) 0.31888(13) 0.0316(5) Uani 1 1 d . . . O4 O -0.03825(11) 0.24456(11) 0.41648(14) 0.0415(6) Uani 1 1 d . . . N1 N -0.37259(12) 0.23788(10) 0.14409(14) 0.0230(6) Uani 1 1 d . . . N2 N -0.26493(12) 0.21906(10) 0.15913(14) 0.0225(6) Uani 1 1 d . . . N3 N -0.15655(12) 0.20305(11) 0.17601(15) 0.0250(6) Uani 1 1 d . . . N4 N -0.37274(11) 0.08993(10) 0.24361(14) 0.0223(5) Uani 1 1 d . . . N5 N -0.28254(12) 0.12417(10) 0.31808(14) 0.0223(6) Uani 1 1 d . . . N6 N -0.18956(12) 0.15799(11) 0.38766(14) 0.0247(6) Uani 1 1 d . . . N7 N -0.39602(12) 0.19942(10) 0.28983(14) 0.0227(6) Uani 1 1 d . . . N8 N -0.29366(12) 0.23150(10) 0.29761(14) 0.0222(6) Uani 1 1 d . . . N9 N -0.19102(12) 0.26317(11) 0.30392(15) 0.0257(6) Uani 1 1 d . . . N10 N -0.34682(12) 0.12656(10) 0.10029(14) 0.0232(6) Uani 1 1 d . . . N11 N -0.25266(11) 0.11440(10) 0.18259(14) 0.0217(5) Uani 1 1 d . . . N12 N -0.15643(12) 0.10400(11) 0.26226(15) 0.0261(6) Uani 1 1 d . . . N13 N 0.16078(11) 0.29188(11) 0.54293(14) 0.0230(6) Uani 1 1 d . . . N14 N 0.22076(11) 0.18924(11) 0.55049(14) 0.0232(6) Uani 1 1 d . . . N15 N 0.29646(12) 0.22305(10) 0.44341(14) 0.0229(6) Uani 1 1 d . . . N16 N 0.23673(12) 0.32505(11) 0.43537(15) 0.0247(6) Uani 1 1 d . . . N17 N 0.30604(12) 0.29533(11) 0.58532(15) 0.0266(6) Uani 1 1 d . . . N18 N 0.15124(12) 0.21946(11) 0.40127(14) 0.0242(6) Uani 1 1 d . . . C1 C -0.42172(16) 0.27198(14) 0.12583(19) 0.0293(7) Uani 1 1 d . . . H1A H -0.4618 0.2624 0.1384 0.035 Uiso 1 1 calc R . . C2 C -0.41647(17) 0.31987(14) 0.0900(2) 0.0351(8) Uani 1 1 d . . . H2A H -0.4523 0.3426 0.0771 0.042 Uiso 1 1 calc R . . C3 C -0.35762(18) 0.33411(15) 0.0730(2) 0.0387(9) Uani 1 1 d . . . H3A H -0.3529 0.3665 0.0469 0.046 Uiso 1 1 calc R . . C4 C -0.30631(16) 0.30135(14) 0.09412(19) 0.0323(8) Uani 1 1 d . . . H4A H -0.2656 0.3114 0.0840 0.039 Uiso 1 1 calc R . . C5 C -0.31429(15) 0.25262(13) 0.13090(17) 0.0253(7) Uani 1 1 d . . . C6 C -0.20996(15) 0.21603(13) 0.12799(18) 0.0243(7) Uani 1 1 d . . . C7 C -0.20849(16) 0.22115(14) 0.05073(19) 0.0317(8) Uani 1 1 d . . . H7A H -0.2462 0.2297 0.0170 0.038 Uiso 1 1 calc R . . C8 C -0.15209(17) 0.21375(15) 0.0241(2) 0.0353(8) Uani 1 1 d . . . H8A H -0.1506 0.2174 -0.0280 0.042 Uiso 1 1 calc R . . C9 C -0.09802(16) 0.20109(15) 0.0736(2) 0.0342(8) Uani 1 1 d . . . H9A H -0.0586 0.1962 0.0564 0.041 Uiso 1 1 calc R . . C10 C -0.10205(15) 0.19567(14) 0.14819(19) 0.0307(8) Uani 1 1 d . . . H10A H -0.0647 0.1863 0.1820 0.037 Uiso 1 1 calc R . . C11 C -0.41120(16) 0.04866(14) 0.21844(19) 0.0312(8) Uani 1 1 d . . . H11A H -0.4467 0.0556 0.1805 0.037 Uiso 1 1 calc R . . C12 C -0.40194(17) -0.00287(14) 0.2446(2) 0.0357(8) Uani 1 1 d . . . H12A H -0.4305 -0.0307 0.2257 0.043 Uiso 1 1 calc R . . C13 C -0.34980(17) -0.01296(14) 0.2991(2) 0.0328(8) Uani 1 1 d . . . H13A H -0.3416 -0.0482 0.3179 0.039 Uiso 1 1 calc R . . C14 C -0.31006(16) 0.02827(13) 0.32597(18) 0.0282(7) Uani 1 1 d . . . H14A H -0.2741 0.0215 0.3633 0.034 Uiso 1 1 calc R . . C15 C -0.32237(14) 0.08046(13) 0.29845(17) 0.0238(7) Uani 1 1 d . . . C16 C -0.24264(14) 0.12725(13) 0.38611(17) 0.0240(7) Uani 1 1 d . . . C17 C -0.25484(15) 0.10204(14) 0.45197(18) 0.0293(7) Uani 1 1 d . . . H17A H -0.2928 0.0820 0.4512 0.035 Uiso 1 1 calc R . . C18 C -0.21191(16) 0.10625(15) 0.51777(19) 0.0332(8) Uani 1 1 d . . . H18A H -0.2193 0.0884 0.5620 0.040 Uiso 1 1 calc R . . C19 C -0.15779(17) 0.13704(16) 0.51805(19) 0.0366(9) Uani 1 1 d . . . H19A H -0.1272 0.1403 0.5624 0.044 Uiso 1 1 calc R . . C20 C -0.14912(16) 0.16260(14) 0.45336(18) 0.0304(8) Uani 1 1 d . . . H20A H -0.1128 0.1848 0.4547 0.036 Uiso 1 1 calc R . . C21 C -0.44939(15) 0.19187(15) 0.32024(19) 0.0310(8) Uani 1 1 d . . . H21A H -0.4809 0.1681 0.2958 0.037 Uiso 1 1 calc R . . C22 C -0.45988(16) 0.21678(16) 0.3842(2) 0.0362(8) Uani 1 1 d . . . H22A H -0.4976 0.2101 0.4044 0.043 Uiso 1 1 calc R . . C23 C -0.41426(17) 0.25217(15) 0.4195(2) 0.0347(8) Uani 1 1 d . . . H23A H -0.4208 0.2707 0.4636 0.042 Uiso 1 1 calc R . . C24 C -0.35993(15) 0.25994(14) 0.39011(18) 0.0285(7) Uani 1 1 d . . . H24A H -0.3286 0.2844 0.4133 0.034 Uiso 1 1 calc R . . C25 C -0.35021(14) 0.23179(13) 0.32547(17) 0.0234(7) Uani 1 1 d . . . C26 C -0.25320(15) 0.27486(13) 0.30451(17) 0.0255(7) Uani 1 1 d . . . C27 C -0.27369(17) 0.32850(14) 0.3054(2) 0.0332(8) Uani 1 1 d . . . H27A H -0.3172 0.3364 0.3061 0.040 Uiso 1 1 calc R . . C28 C -0.23071(19) 0.36917(15) 0.3053(2) 0.0414(9) Uani 1 1 d . . . H28A H -0.2442 0.4054 0.3059 0.050 Uiso 1 1 calc R . . C29 C -0.16746(18) 0.35726(16) 0.3042(2) 0.0411(9) Uani 1 1 d . . . H29A H -0.1370 0.3850 0.3039 0.049 Uiso 1 1 calc R . . C30 C -0.14984(16) 0.30446(15) 0.30367(19) 0.0322(8) Uani 1 1 d . . . H30A H -0.1064 0.2964 0.3031 0.039 Uiso 1 1 calc R . . C31 C -0.38121(16) 0.12328(14) 0.03054(18) 0.0302(7) Uani 1 1 d . . . H31A H -0.4224 0.1388 0.0219 0.036 Uiso 1 1 calc R . . C32 C -0.35954(17) 0.09855(15) -0.02850(19) 0.0367(8) Uani 1 1 d . . . H32A H -0.3853 0.0968 -0.0766 0.044 Uiso 1 1 calc R . . C33 C -0.29909(17) 0.07618(15) -0.01609(19) 0.0359(8) Uani 1 1 d . . . H33A H -0.2829 0.0588 -0.0558 0.043 Uiso 1 1 calc R . . C34 C -0.26265(17) 0.07940(14) 0.05440(19) 0.0317(8) Uani 1 1 d . . . H34A H -0.2212 0.0644 0.0635 0.038 Uiso 1 1 calc R . . C35 C -0.28755(15) 0.10516(13) 0.11280(18) 0.0246(7) Uani 1 1 d . . . C36 C -0.20418(14) 0.08074(13) 0.21487(17) 0.0248(7) Uani 1 1 d . . . C37 C -0.20590(16) 0.02500(14) 0.20534(19) 0.0319(8) Uani 1 1 d . . . H37A H -0.2402 0.0086 0.1731 0.038 Uiso 1 1 calc R . . C38 C -0.15719(18) -0.00591(15) 0.2434(2) 0.0407(9) Uani 1 1 d . . . H38A H -0.1575 -0.0436 0.2365 0.049 Uiso 1 1 calc R . . C39 C -0.10820(18) 0.01814(16) 0.2913(2) 0.0436(10) Uani 1 1 d . . . H39A H -0.0742 -0.0024 0.3175 0.052 Uiso 1 1 calc R . . C40 C -0.11018(16) 0.07262(15) 0.2998(2) 0.0345(8) Uani 1 1 d . . . H40A H -0.0773 0.0892 0.3339 0.041 Uiso 1 1 calc R . . C41 C 0.13954(15) 0.34441(13) 0.53459(18) 0.0259(7) Uani 1 1 d . . . C42 C 0.09267(16) 0.35343(15) 0.58178(19) 0.0326(8) Uani 1 1 d . . . H42A H 0.0707 0.3860 0.5867 0.039 Uiso 1 1 calc R . . C43 C 0.08556(16) 0.30724(14) 0.61791(19) 0.0306(8) Uani 1 1 d . . . H43A H 0.0577 0.3014 0.6532 0.037 Uiso 1 1 calc R . . C44 C 0.12754(15) 0.26840(13) 0.59365(17) 0.0259(7) Uani 1 1 d . . . C45 C 0.13404(15) 0.21565(13) 0.61893(17) 0.0258(7) Uani 1 1 d . . . C46 C 0.17723(14) 0.17858(14) 0.59755(17) 0.0257(7) Uani 1 1 d . . . C47 C 0.18185(16) 0.12376(14) 0.62005(19) 0.0320(8) Uani 1 1 d . . . H47A H 0.1568 0.1063 0.6517 0.038 Uiso 1 1 calc R . . C48 C 0.22822(16) 0.10141(14) 0.58823(19) 0.0310(8) Uani 1 1 d . . . H48A H 0.2423 0.0654 0.5940 0.037 Uiso 1 1 calc R . . C49 C 0.25249(14) 0.14152(13) 0.54426(18) 0.0255(7) Uani 1 1 d . . . C50 C 0.30018(14) 0.13297(13) 0.50075(18) 0.0257(7) Uani 1 1 d . . . C51 C 0.31927(15) 0.17148(13) 0.45346(18) 0.0255(7) Uani 1 1 d . . . C52 C 0.36424(16) 0.16174(14) 0.40386(19) 0.0311(8) Uani 1 1 d . . . H52A H 0.3865 0.1293 0.3992 0.037 Uiso 1 1 calc R . . C53 C 0.36902(16) 0.20744(14) 0.36492(19) 0.0306(8) Uani 1 1 d . . . H53A H 0.3954 0.2130 0.3279 0.037 Uiso 1 1 calc R . . C54 C 0.32716(14) 0.24589(13) 0.38962(17) 0.0244(7) Uani 1 1 d . . . C55 C 0.32014(15) 0.29848(14) 0.36375(17) 0.0262(7) Uani 1 1 d . . . C56 C 0.27860(15) 0.33502(14) 0.38642(18) 0.0275(7) Uani 1 1 d . . . C57 C 0.27416(18) 0.39020(15) 0.3639(2) 0.0377(9) Uani 1 1 d . . . H57A H 0.2974 0.4072 0.3298 0.045 Uiso 1 1 calc R . . C58 C 0.23081(18) 0.41323(15) 0.4002(2) 0.0384(9) Uani 1 1 d . . . H58A H 0.2183 0.4498 0.3968 0.046 Uiso 1 1 calc R . . C59 C 0.20702(15) 0.37342(13) 0.44460(18) 0.0272(7) Uani 1 1 d . . . C60 C 0.16053(15) 0.38286(13) 0.48859(18) 0.0280(7) Uani 1 1 d . . . C61 C 0.09235(15) 0.19717(13) 0.67287(18) 0.0271(7) Uani 1 1 d . . . C62 C 0.02659(16) 0.19459(15) 0.65112(19) 0.0334(8) Uani 1 1 d . . . H62A H 0.0081 0.2049 0.6017 0.040 Uiso 1 1 calc R . . C63 C -0.01174(17) 0.17709(16) 0.7009(2) 0.0379(9) Uani 1 1 d . . . H63A H -0.0565 0.1751 0.6855 0.045 Uiso 1 1 calc R . . C64 C 0.01452(18) 0.16242(16) 0.7729(2) 0.0392(9) Uani 1 1 d . . . H64A H -0.0119 0.1499 0.8069 0.047 Uiso 1 1 calc R . . C65 C 0.07926(18) 0.16601(15) 0.7953(2) 0.0368(9) Uani 1 1 d . . . H65A H 0.0973 0.1566 0.8453 0.044 Uiso 1 1 calc R . . C66 C 0.11849(17) 0.18323(15) 0.74601(19) 0.0335(8) Uani 1 1 d . . . H66A H 0.1631 0.1855 0.7621 0.040 Uiso 1 1 calc R . . C67 C 0.33291(16) 0.07982(14) 0.50260(19) 0.0302(8) Uani 1 1 d . . . C68 C 0.30443(18) 0.03695(14) 0.4610(2) 0.0358(8) Uani 1 1 d . . . H68A H 0.2621 0.0401 0.4349 0.043 Uiso 1 1 calc R . . C69 C 0.3377(2) -0.01028(15) 0.4574(2) 0.0437(10) Uani 1 1 d . . . H69A H 0.3183 -0.0391 0.4278 0.052 Uiso 1 1 calc R . . C70 C 0.3984(2) -0.01611(16) 0.4962(2) 0.0435(10) Uani 1 1 d . . . H70A H 0.4206 -0.0489 0.4937 0.052 Uiso 1 1 calc R . . C71 C 0.42661(19) 0.02536(18) 0.5384(2) 0.0452(10) Uani 1 1 d . . . H71A H 0.4682 0.0212 0.5661 0.054 Uiso 1 1 calc R . . C72 C 0.39455(17) 0.07373(16) 0.5407(2) 0.0402(9) Uani 1 1 d . . . H72A H 0.4150 0.1028 0.5687 0.048 Uiso 1 1 calc R . . C73 C 0.36447(16) 0.31581(13) 0.31118(18) 0.0274(7) Uani 1 1 d . . . C74 C 0.34574(18) 0.31300(16) 0.2342(2) 0.0391(9) Uani 1 1 d . . . H74A H 0.3037 0.3023 0.2137 0.047 Uiso 1 1 calc R . . C75 C 0.3888(2) 0.32589(17) 0.1873(2) 0.0452(10) Uani 1 1 d . . . H75A H 0.3765 0.3233 0.1344 0.054 Uiso 1 1 calc R . . C76 C 0.44929(19) 0.34234(17) 0.2164(2) 0.0430(10) Uani 1 1 d . . . H76A H 0.4780 0.3521 0.1836 0.052 Uiso 1 1 calc R . . C77 C 0.46849(18) 0.34475(17) 0.2931(2) 0.0443(10) Uani 1 1 d . . . H77A H 0.5106 0.3554 0.3133 0.053 Uiso 1 1 calc R . . C78 C 0.42587(17) 0.33144(16) 0.3408(2) 0.0377(9) Uani 1 1 d . . . H78A H 0.4388 0.3331 0.3937 0.045 Uiso 1 1 calc R . . C79 C 0.13228(17) 0.43829(14) 0.4863(2) 0.0338(8) Uani 1 1 d . . . C80 C 0.0838(3) 0.4528(2) 0.4301(3) 0.0806(18) Uani 1 1 d . . . H80A H 0.0669 0.4275 0.3929 0.097 Uiso 1 1 calc R . . C81 C 0.0594(3) 0.5043(2) 0.4274(4) 0.102(2) Uani 1 1 d . . . H81A H 0.0260 0.5138 0.3881 0.123 Uiso 1 1 calc R . . C82 C 0.0821(3) 0.54107(19) 0.4795(3) 0.0696(15) Uani 1 1 d . . . H82A H 0.0650 0.5763 0.4770 0.084 Uiso 1 1 calc R . . C83 C 0.1293(3) 0.52742(19) 0.5352(3) 0.0672(14) Uani 1 1 d . . . H83A H 0.1454 0.5530 0.5724 0.081 Uiso 1 1 calc R . . C84 C 0.1550(2) 0.47576(17) 0.5384(3) 0.0538(11) Uani 1 1 d . . . H84A H 0.1887 0.4667 0.5776 0.065 Uiso 1 1 calc R . . C85 C 0.48017(15) 0.32910(14) 0.60193(19) 0.0280(7) Uani 1 1 d . . . C86 C 0.36680(15) 0.29904(13) 0.57384(18) 0.0261(7) Uani 1 1 d . . . H86A H 0.3785 0.2803 0.5323 0.031 Uiso 1 1 calc R . . C87 C 0.41324(15) 0.32848(13) 0.61885(18) 0.0259(7) Uani 1 1 d . . . C88 C 0.39591(16) 0.35629(15) 0.67882(19) 0.0350(8) Uani 1 1 d . . . H88A H 0.4264 0.3768 0.7112 0.042 Uiso 1 1 calc R . . C89 C 0.33345(17) 0.35376(16) 0.6907(2) 0.0377(9) Uani 1 1 d . . . H89A H 0.3203 0.3730 0.7309 0.045 Uiso 1 1 calc R . . C90 C 0.29077(16) 0.32307(15) 0.64366(19) 0.0330(8) Uani 1 1 d . . . H90A H 0.2482 0.3214 0.6528 0.040 Uiso 1 1 calc R . . C91 C -0.02750(15) 0.21325(14) 0.36728(19) 0.0308(8) Uani 1 1 d . . . C92 C 0.08962(14) 0.22762(13) 0.40450(17) 0.0241(7) Uani 1 1 d . . . H92A H 0.0789 0.2536 0.4387 0.029 Uiso 1 1 calc R . . C93 C 0.04070(15) 0.20001(14) 0.36032(18) 0.0265(7) Uani 1 1 d . . . C94 C 0.05636(16) 0.16148(15) 0.3117(2) 0.0337(8) Uani 1 1 d . . . H94A H 0.0241 0.1413 0.2816 0.040 Uiso 1 1 calc R . . C95 C 0.11967(16) 0.15263(16) 0.3074(2) 0.0364(8) Uani 1 1 d . . . H95A H 0.1316 0.1267 0.2738 0.044 Uiso 1 1 calc R . . C96 C 0.16538(15) 0.18242(14) 0.35297(18) 0.0289(7) Uani 1 1 d . . . H96A H 0.2088 0.1763 0.3498 0.035 Uiso 1 1 calc R . . Cl1 Cl 0.22014(5) 0.02486(5) 0.25237(7) 0.0570(3) Uani 1 1 d . . . O5 O 0.24608(19) 0.07211(14) 0.29089(19) 0.0758(10) Uani 1 1 d . . . O6 O 0.25733(16) 0.00968(16) 0.19519(19) 0.0742(10) Uani 1 1 d . . . O7 O 0.22118(18) -0.01801(14) 0.3055(2) 0.0735(10) Uani 1 1 d . . . O8 O 0.15556(17) 0.03542(18) 0.2175(2) 0.0848(12) Uani 1 1 d . . . C97 C 0.6010(2) 0.00382(19) 0.7363(3) 0.0559(11) Uani 1 1 d . . . H97A H 0.6462 -0.0082 0.7412 0.067 Uiso 1 1 calc R . . Cl2 Cl 0.59484(7) 0.06929(5) 0.69994(8) 0.0748(4) Uani 1 1 d . . . Cl3 Cl 0.57824(7) 0.00276(6) 0.82508(7) 0.0755(4) Uani 1 1 d . . . Cl4 Cl 0.55252(6) -0.04065(5) 0.67546(6) 0.0550(3) Uani 1 1 d . . . O9 O 0.04109(15) 0.03239(14) 0.40632(19) 0.0671(9) Uani 1 1 d . . . C98 C 0.0128(3) 0.0884(2) 0.4996(3) 0.0786(16) Uani 1 1 d . . . H98A H 0.0297 0.1088 0.5448 0.118 Uiso 1 1 calc R . . H98B H -0.0174 0.0615 0.5120 0.118 Uiso 1 1 calc R . . H98C H -0.0089 0.1127 0.4612 0.118 Uiso 1 1 calc R . . C99 C 0.0650(2) 0.0615(2) 0.4709(3) 0.0717(15) Uani 1 1 d . . . H99A H 0.0960 0.0884 0.4590 0.086 Uiso 1 1 calc R . . H99B H 0.0873 0.0371 0.5097 0.086 Uiso 1 1 calc R . . C100 C 0.0894(3) 0.0052(2) 0.3787(3) 0.0749(15) Uani 1 1 d . . . H10B H 0.1137 -0.0169 0.4191 0.090 Uiso 1 1 calc R . . H10C H 0.1189 0.0312 0.3614 0.090 Uiso 1 1 calc R . . C101 C 0.0607(3) -0.0302(3) 0.3143(5) 0.121(3) Uani 1 1 d . . . H10D H 0.0947 -0.0493 0.2946 0.181 Uiso 1 1 calc R . . H10E H 0.0369 -0.0081 0.2744 0.181 Uiso 1 1 calc R . . H10F H 0.0320 -0.0561 0.3318 0.181 Uiso 1 1 calc R . . O10 O 0.4920(6) 0.5019(5) 0.5389(6) 0.108(3) Uani 0.50 1 d PD . . C102 C 0.4722(5) 0.4609(5) 0.4824(9) 0.213(7) Uani 1 1 d D . . H10G H 0.4949 0.4298 0.4961 0.255 Uiso 1 1 d . . . H10H H 0.4831 0.4755 0.4367 0.255 Uiso 1 1 d . . . C103 C 0.4068(4) 0.4543(4) 0.4763(5) 0.138(3) Uani 1 1 d D . . H10I H 0.3922 0.4279 0.4371 0.206 Uiso 1 1 calc R . . H10J H 0.3856 0.4886 0.4632 0.206 Uiso 1 1 calc R . . H10K H 0.3966 0.4418 0.5244 0.206 Uiso 1 1 calc R . . 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 0.0143(2) 0.0245(2) 0.0232(2) 0.00179(16) 0.00056(15) 0.00017(15) Ni2 0.0144(2) 0.0219(2) 0.0220(2) -0.00064(15) 0.00201(15) -0.00055(15) Ni3 0.0139(2) 0.0295(2) 0.0249(2) -0.00425(17) 0.00153(15) -0.00252(16) Mn1 0.0140(2) 0.0247(3) 0.0229(2) 0.00078(19) 0.00185(18) 0.00016(18) O1 0.0144(11) 0.0360(13) 0.0297(12) -0.0051(10) -0.0026(9) -0.0003(9) O2 0.0217(12) 0.0581(17) 0.0325(13) -0.0111(12) 0.0041(10) -0.0052(11) O3 0.0172(11) 0.0425(14) 0.0340(13) -0.0101(11) 0.0005(10) -0.0051(10) O4 0.0209(12) 0.0619(18) 0.0420(14) -0.0212(13) 0.0060(11) -0.0039(12) N1 0.0181(13) 0.0256(14) 0.0252(13) 0.0018(11) 0.0033(10) 0.0036(11) N2 0.0183(13) 0.0233(14) 0.0262(14) 0.0010(11) 0.0045(11) -0.0014(11) N3 0.0194(13) 0.0277(14) 0.0284(14) -0.0034(12) 0.0051(11) -0.0004(11) N4 0.0159(13) 0.0243(14) 0.0259(13) 0.0006(11) 0.0007(10) -0.0016(10) N5 0.0177(13) 0.0237(14) 0.0247(13) 0.0031(11) 0.0008(10) 0.0002(10) N6 0.0179(13) 0.0312(15) 0.0240(13) -0.0035(11) 0.0007(11) 0.0014(11) N7 0.0183(13) 0.0263(14) 0.0236(13) 0.0042(11) 0.0032(10) 0.0030(11) N8 0.0183(13) 0.0244(14) 0.0248(13) -0.0022(11) 0.0059(10) -0.0016(11) N9 0.0208(14) 0.0298(15) 0.0269(14) -0.0054(12) 0.0054(11) -0.0045(11) N10 0.0174(13) 0.0248(14) 0.0264(13) 0.0006(11) 0.0006(10) -0.0003(11) N11 0.0146(12) 0.0242(14) 0.0255(13) -0.0028(11) 0.0003(10) 0.0003(10) N12 0.0168(13) 0.0341(16) 0.0269(14) -0.0039(12) 0.0020(11) 0.0025(11) N13 0.0164(13) 0.0276(14) 0.0245(13) -0.0001(11) 0.0020(10) -0.0008(11) N14 0.0144(12) 0.0302(15) 0.0249(13) 0.0020(11) 0.0031(10) 0.0019(11) N15 0.0178(13) 0.0263(14) 0.0245(13) 0.0001(11) 0.0036(10) -0.0029(11) N16 0.0181(13) 0.0282(15) 0.0278(14) 0.0017(11) 0.0036(11) 0.0003(11) N17 0.0176(13) 0.0338(16) 0.0274(14) -0.0010(12) 0.0005(11) -0.0020(11) N18 0.0162(13) 0.0307(15) 0.0245(13) 0.0008(12) -0.0003(10) -0.0005(11) C1 0.0224(17) 0.0330(19) 0.0326(18) 0.0006(15) 0.0052(14) 0.0043(14) C2 0.0309(19) 0.0297(19) 0.046(2) 0.0078(16) 0.0086(16) 0.0121(15) C3 0.043(2) 0.0305(19) 0.047(2) 0.0116(17) 0.0188(18) 0.0060(16) C4 0.0270(18) 0.0314(19) 0.041(2) 0.0064(16) 0.0138(15) 0.0011(15) C5 0.0259(17) 0.0253(17) 0.0252(16) -0.0010(13) 0.0059(13) 0.0004(13) C6 0.0224(16) 0.0225(16) 0.0283(17) -0.0004(13) 0.0051(13) -0.0024(13) C7 0.0288(18) 0.037(2) 0.0294(18) 0.0023(15) 0.0060(14) 0.0040(15) C8 0.037(2) 0.040(2) 0.0310(18) 0.0002(16) 0.0117(16) 0.0000(16) C9 0.0258(18) 0.040(2) 0.039(2) -0.0068(17) 0.0138(15) -0.0011(15) C10 0.0184(16) 0.038(2) 0.0359(19) -0.0046(16) 0.0059(14) -0.0009(14) C11 0.0230(17) 0.0323(19) 0.0363(19) 0.0032(15) -0.0010(14) -0.0042(14) C12 0.033(2) 0.0286(19) 0.044(2) 0.0020(16) 0.0013(16) -0.0095(15) C13 0.0341(19) 0.0247(18) 0.0395(19) 0.0081(15) 0.0057(16) 0.0009(15) C14 0.0251(17) 0.0300(18) 0.0288(17) 0.0065(14) 0.0020(13) 0.0017(14) C15 0.0183(15) 0.0266(17) 0.0264(16) 0.0014(13) 0.0032(13) -0.0017(13) C16 0.0172(15) 0.0278(17) 0.0269(16) -0.0019(13) 0.0035(12) 0.0027(13) C17 0.0216(17) 0.037(2) 0.0298(17) 0.0012(15) 0.0046(14) 0.0008(14) C18 0.0284(18) 0.044(2) 0.0273(17) -0.0008(15) 0.0034(14) 0.0029(16) C19 0.0285(19) 0.051(2) 0.0282(18) -0.0062(17) -0.0009(14) 0.0040(17) C20 0.0218(17) 0.040(2) 0.0284(17) -0.0068(15) 0.0011(13) 0.0007(14) C21 0.0182(16) 0.042(2) 0.0330(18) -0.0001(16) 0.0034(14) -0.0029(15) C22 0.0199(17) 0.054(2) 0.037(2) 0.0011(18) 0.0106(15) -0.0010(16) C23 0.0307(19) 0.044(2) 0.0314(18) -0.0050(16) 0.0113(15) 0.0034(16) C24 0.0238(17) 0.0331(19) 0.0284(17) -0.0042(14) 0.0039(14) 0.0005(14) C25 0.0196(16) 0.0253(16) 0.0247(16) 0.0027(13) 0.0019(12) 0.0026(13) C26 0.0240(17) 0.0283(17) 0.0248(16) -0.0037(13) 0.0065(13) -0.0025(14) C27 0.0304(19) 0.0295(19) 0.041(2) -0.0049(16) 0.0093(16) -0.0024(15) C28 0.046(2) 0.0283(19) 0.054(2) -0.0028(17) 0.0187(19) -0.0020(17) C29 0.038(2) 0.035(2) 0.053(2) -0.0080(18) 0.0149(18) -0.0151(17) C30 0.0261(18) 0.038(2) 0.0341(18) -0.0063(16) 0.0102(14) -0.0092(15) C31 0.0232(17) 0.0335(19) 0.0320(18) 0.0006(15) -0.0007(14) 0.0008(14) C32 0.039(2) 0.042(2) 0.0266(17) -0.0033(16) -0.0039(15) 0.0008(17) C33 0.039(2) 0.042(2) 0.0268(18) -0.0078(16) 0.0049(15) 0.0051(17) C34 0.0287(18) 0.0349(19) 0.0316(18) -0.0039(15) 0.0053(14) 0.0030(15) C35 0.0211(16) 0.0236(16) 0.0284(16) 0.0015(13) 0.0018(13) -0.0035(13) C36 0.0152(15) 0.0302(18) 0.0289(16) -0.0022(14) 0.0032(12) 0.0015(13) C37 0.0272(18) 0.0307(19) 0.0358(19) -0.0055(15) -0.0005(15) 0.0015(14) C38 0.039(2) 0.0294(19) 0.051(2) -0.0001(17) -0.0026(18) 0.0093(16) C39 0.033(2) 0.043(2) 0.049(2) 0.0010(18) -0.0091(17) 0.0174(17) C40 0.0222(17) 0.041(2) 0.0372(19) -0.0015(16) -0.0037(14) 0.0064(15) C41 0.0190(16) 0.0299(18) 0.0274(17) -0.0022(14) -0.0001(13) 0.0015(13) C42 0.0279(18) 0.034(2) 0.0370(19) -0.0043(16) 0.0095(15) 0.0052(15) C43 0.0254(17) 0.037(2) 0.0316(18) -0.0043(16) 0.0120(14) 0.0026(15) C44 0.0176(15) 0.0343(19) 0.0250(16) -0.0034(14) 0.0013(13) -0.0004(13) C45 0.0188(16) 0.0326(18) 0.0254(16) 0.0014(14) 0.0017(13) -0.0018(13) C46 0.0170(16) 0.0345(18) 0.0256(16) 0.0043(14) 0.0033(13) -0.0008(13) C47 0.0257(18) 0.036(2) 0.0357(19) 0.0078(16) 0.0087(15) 0.0008(15) C48 0.0265(18) 0.0289(18) 0.0374(19) 0.0064(15) 0.0048(15) 0.0051(14) C49 0.0185(16) 0.0283(17) 0.0284(16) 0.0050(14) 0.0001(13) 0.0027(13) C50 0.0190(16) 0.0280(17) 0.0289(17) 0.0006(14) 0.0002(13) 0.0020(13) C51 0.0171(15) 0.0295(17) 0.0292(17) -0.0015(14) 0.0017(13) 0.0012(13) C52 0.0283(18) 0.0315(19) 0.0352(19) -0.0020(15) 0.0100(15) 0.0041(15) C53 0.0240(17) 0.039(2) 0.0298(17) -0.0010(15) 0.0072(14) 0.0016(15) C54 0.0159(15) 0.0333(18) 0.0234(15) -0.0010(14) 0.0012(12) 0.0001(13) C55 0.0201(16) 0.0357(19) 0.0224(16) 0.0002(14) 0.0020(12) -0.0027(14) C56 0.0210(16) 0.0337(19) 0.0278(17) 0.0027(14) 0.0043(13) -0.0009(14) C57 0.038(2) 0.034(2) 0.044(2) 0.0140(17) 0.0167(17) 0.0021(16) C58 0.040(2) 0.0268(18) 0.051(2) 0.0094(17) 0.0147(18) 0.0046(16) C59 0.0227(17) 0.0275(17) 0.0311(17) 0.0030(14) 0.0031(13) 0.0011(13) C60 0.0259(17) 0.0268(17) 0.0304(17) -0.0017(14) 0.0014(14) 0.0016(14) C61 0.0227(17) 0.0298(18) 0.0301(17) 0.0006(14) 0.0081(13) 0.0000(14) C62 0.0272(18) 0.043(2) 0.0298(18) 0.0006(16) 0.0046(14) 0.0008(16) C63 0.0225(18) 0.054(2) 0.038(2) -0.0005(18) 0.0079(15) -0.0011(16) C64 0.037(2) 0.046(2) 0.039(2) 0.0026(17) 0.0200(17) -0.0006(17) C65 0.037(2) 0.046(2) 0.0285(18) 0.0057(16) 0.0069(15) 0.0031(17) C66 0.0245(18) 0.043(2) 0.0326(19) 0.0019(16) 0.0042(14) 0.0009(15) C67 0.0281(18) 0.0314(19) 0.0327(18) 0.0075(15) 0.0093(14) 0.0048(14) C68 0.0312(19) 0.034(2) 0.043(2) 0.0025(17) 0.0100(16) 0.0000(16) C69 0.049(2) 0.029(2) 0.057(2) 0.0020(18) 0.019(2) 0.0015(17) C70 0.049(2) 0.033(2) 0.054(2) 0.0088(19) 0.025(2) 0.0126(18) C71 0.036(2) 0.057(3) 0.043(2) 0.009(2) 0.0085(18) 0.0207(19) C72 0.033(2) 0.046(2) 0.041(2) -0.0048(18) 0.0027(16) 0.0103(17) C73 0.0258(17) 0.0281(18) 0.0296(17) 0.0056(14) 0.0088(14) 0.0015(14) C74 0.031(2) 0.053(2) 0.0325(19) 0.0059(17) 0.0037(16) -0.0074(17) C75 0.052(3) 0.055(3) 0.0300(19) 0.0061(18) 0.0121(18) -0.002(2) C76 0.040(2) 0.050(2) 0.045(2) 0.0088(19) 0.0226(19) 0.0025(18) C77 0.027(2) 0.060(3) 0.047(2) 0.008(2) 0.0084(17) -0.0083(18) C78 0.031(2) 0.053(2) 0.0301(18) 0.0032(17) 0.0057(15) -0.0080(17) C79 0.034(2) 0.0304(19) 0.039(2) 0.0008(16) 0.0130(16) 0.0032(15) C80 0.099(4) 0.056(3) 0.074(3) -0.019(3) -0.026(3) 0.042(3) C81 0.133(6) 0.074(4) 0.087(4) -0.008(3) -0.021(4) 0.068(4) C82 0.080(4) 0.036(3) 0.099(4) 0.005(3) 0.035(3) 0.018(3) C83 0.067(3) 0.040(3) 0.098(4) -0.026(3) 0.023(3) -0.001(2) C84 0.052(3) 0.040(2) 0.066(3) -0.016(2) 0.003(2) 0.003(2) C85 0.0193(16) 0.0337(19) 0.0295(18) -0.0014(15) -0.0008(13) -0.0017(14) C86 0.0189(16) 0.0327(18) 0.0261(16) -0.0009(14) 0.0019(13) 0.0021(13) C87 0.0193(16) 0.0286(17) 0.0280(17) -0.0025(14) -0.0017(13) -0.0010(13) C88 0.0246(18) 0.044(2) 0.0332(19) -0.0127(16) -0.0038(14) 0.0014(16) C89 0.0281(19) 0.053(2) 0.0315(19) -0.0131(17) 0.0021(15) 0.0005(17) C90 0.0180(16) 0.051(2) 0.0300(18) -0.0042(16) 0.0035(14) 0.0033(15) C91 0.0224(17) 0.039(2) 0.0313(18) -0.0023(16) 0.0048(14) -0.0032(15) C92 0.0169(15) 0.0291(17) 0.0258(16) -0.0006(13) 0.0016(12) -0.0006(13) C93 0.0173(16) 0.0342(19) 0.0271(16) -0.0017(14) 0.0009(13) -0.0028(13) C94 0.0216(17) 0.041(2) 0.0359(19) -0.0104(16) -0.0036(14) -0.0014(15) C95 0.0266(18) 0.048(2) 0.0334(19) -0.0137(17) -0.0001(15) 0.0045(16) C96 0.0184(16) 0.039(2) 0.0288(17) -0.0016(15) 0.0037(13) 0.0035(14) Cl1 0.0479(6) 0.0564(7) 0.0643(7) -0.0067(6) 0.0021(5) 0.0045(5) O5 0.096(3) 0.062(2) 0.069(2) -0.0059(18) 0.014(2) -0.024(2) O6 0.058(2) 0.100(3) 0.064(2) -0.010(2) 0.0101(17) 0.0202(19) O7 0.088(3) 0.055(2) 0.078(2) 0.0024(18) 0.015(2) -0.0100(18) O8 0.054(2) 0.115(3) 0.082(3) -0.012(2) 0.0022(19) 0.026(2) C97 0.047(3) 0.060(3) 0.059(3) 0.009(2) 0.006(2) 0.003(2) Cl2 0.0900(10) 0.0501(7) 0.0902(9) 0.0031(7) 0.0325(8) 0.0057(7) Cl3 0.0934(10) 0.0811(9) 0.0498(7) -0.0078(6) 0.0054(7) -0.0154(8) Cl4 0.0695(7) 0.0524(6) 0.0418(5) 0.0042(5) 0.0055(5) 0.0120(5) O9 0.052(2) 0.075(2) 0.073(2) -0.0050(19) 0.0056(17) 0.0098(17) C98 0.107(5) 0.063(3) 0.064(3) -0.009(3) 0.011(3) 0.009(3) C99 0.057(3) 0.076(4) 0.076(3) -0.013(3) -0.009(3) -0.002(3) C100 0.056(3) 0.081(4) 0.091(4) -0.009(3) 0.022(3) 0.003(3) C101 0.089(5) 0.100(5) 0.187(8) -0.064(5) 0.064(5) -0.023(4) O10 0.132(9) 0.079(6) 0.112(7) 0.013(6) 0.017(7) 0.003(6) C102 0.145(11) 0.241(17) 0.265(19) 0.106(16) 0.075(12) 0.032(11) C103 0.127(7) 0.141(8) 0.142(7) -0.059(6) 0.012(6) -0.008(6) _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 O1 2.001(2) 4_465 ? Ni1 N1 2.069(3) . ? Ni1 N4 2.074(3) . ? Ni1 N7 2.096(3) . ? Ni1 N10 2.103(3) . ? Ni1 Ni2 2.4156(5) . ? Ni2 N11 1.881(3) . ? Ni2 N8 1.891(3) . ? Ni2 N2 1.893(3) . ? Ni2 N5 1.895(2) . ? Ni2 Ni3 2.4206(5) . ? Ni3 O3 1.985(2) . ? Ni3 N9 2.072(3) . ? Ni3 N6 2.084(3) . ? Ni3 N12 2.097(3) . ? Ni3 N3 2.104(3) . ? Mn1 N16 2.011(3) . ? Mn1 N15 2.012(3) . ? Mn1 N14 2.011(3) . ? Mn1 N13 2.019(3) . ? Mn1 N18 2.339(3) . ? Mn1 N17 2.346(3) . ? O1 C85 1.281(4) . ? O1 Ni1 2.001(2) 4_666 ? O2 C85 1.237(4) . ? O3 C91 1.280(4) . ? O4 C91 1.233(4) . ? N1 C1 1.349(4) . ? N1 C5 1.354(4) . ? N2 C5 1.377(4) . ? N2 C6 1.382(4) . ? N3 C10 1.351(4) . ? N3 C6 1.353(4) . ? N4 C11 1.349(4) . ? N4 C15 1.358(4) . ? N5 C16 1.377(4) . ? N5 C15 1.393(4) . ? N6 C20 1.353(4) . ? N6 C16 1.364(4) . ? N7 C25 1.348(4) . ? N7 C21 1.355(4) . ? N8 C26 1.378(4) . ? N8 C25 1.380(4) . ? N9 C30 1.355(4) . ? N9 C26 1.359(4) . ? N10 C31 1.352(4) . ? N10 C35 1.357(4) . ? N11 C35 1.374(4) . ? N11 C36 1.385(4) . ? N12 C36 1.350(4) . ? N12 C40 1.352(4) . ? N13 C44 1.377(4) . ? N13 C41 1.389(4) . ? N14 C46 1.382(4) . ? N14 C49 1.384(4) . ? N15 C51 1.379(4) . ? N15 C54 1.380(4) . ? N16 C56 1.377(4) . ? N16 C59 1.387(4) . ? N17 C90 1.344(4) . ? N17 C86 1.348(4) . ? N18 C96 1.339(4) . ? N18 C92 1.340(4) . ? C1 C2 1.374(5) . ? C2 C3 1.385(5) . ? C3 C4 1.370(5) . ? C4 C5 1.410(5) . ? C6 C7 1.406(5) . ? C7 C8 1.378(5) . ? C8 C9 1.375(5) . ? C9 C10 1.370(5) . ? C11 C12 1.374(5) . ? C12 C13 1.383(5) . ? C13 C14 1.371(5) . ? C14 C15 1.405(4) . ? C16 C17 1.407(5) . ? C17 C18 1.380(5) . ? C18 C19 1.386(5) . ? C19 C20 1.370(5) . ? C21 C22 1.362(5) . ? C22 C23 1.390(5) . ? C23 C24 1.364(5) . ? C24 C25 1.406(4) . ? C26 C27 1.410(5) . ? C27 C28 1.369(5) . ? C28 C29 1.384(5) . ? C29 C30 1.372(5) . ? C31 C32 1.375(5) . ? C32 C33 1.389(5) . ? C33 C34 1.381(5) . ? C34 C35 1.410(5) . ? C36 C37 1.403(5) . ? C37 C38 1.384(5) . ? C38 C39 1.380(5) . ? C39 C40 1.371(5) . ? C41 C60 1.391(5) . ? C41 C42 1.433(5) . ? C42 C43 1.346(5) . ? C43 C44 1.436(5) . ? C44 C45 1.394(5) . ? C45 C46 1.404(5) . ? C45 C61 1.494(4) . ? C46 C47 1.427(5) . ? C47 C48 1.343(5) . ? C48 C49 1.427(5) . ? C49 C50 1.399(4) . ? C50 C51 1.390(5) . ? C50 C67 1.498(5) . ? C51 C52 1.435(5) . ? C52 C53 1.353(5) . ? C53 C54 1.431(5) . ? C54 C55 1.394(5) . ? C55 C56 1.380(5) . ? C55 C73 1.508(4) . ? C56 C57 1.436(5) . ? C57 C58 1.346(5) . ? C58 C59 1.422(5) . ? C59 C60 1.387(5) . ? C60 C79 1.508(5) . ? C61 C66 1.391(5) . ? C61 C62 1.395(5) . ? C62 C63 1.380(5) . ? C63 C64 1.379(5) . ? C64 C65 1.377(5) . ? C65 C66 1.386(5) . ? C67 C72 1.389(5) . ? C67 C68 1.390(5) . ? C68 C69 1.384(5) . ? C69 C70 1.375(6) . ? C70 C71 1.366(6) . ? C71 C72 1.393(5) . ? C73 C74 1.384(5) . ? C73 C78 1.387(5) . ? C74 C75 1.385(5) . ? C75 C76 1.373(6) . ? C76 C77 1.380(6) . ? C77 C78 1.389(5) . ? C79 C84 1.360(5) . ? C79 C80 1.374(6) . ? C80 C81 1.385(7) . ? C81 C82 1.347(8) . ? C82 C83 1.345(7) . ? C83 C84 1.399(6) . ? C85 C87 1.507(4) . ? C86 C87 1.385(4) . ? C87 C88 1.386(5) . ? C88 C89 1.384(5) . ? C89 C90 1.373(5) . ? C91 C93 1.516(4) . ? C92 C93 1.389(4) . ? C93 C94 1.380(5) . ? C94 C95 1.383(5) . ? C95 C96 1.386(5) . ? Cl1 O5 1.435(4) . ? Cl1 O7 1.436(4) . ? Cl1 O8 1.442(4) . ? Cl1 O6 1.450(3) . ? C97 Cl3 1.748(5) . ? C97 Cl2 1.760(5) . ? C97 Cl4 1.772(5) . ? O9 C100 1.391(6) . ? O9 C99 1.399(6) . ? C98 C99 1.465(7) . ? C100 C101 1.509(8) . ? O10 C102 1.300(15) 3_666 ? O10 C102 1.458(9) . ? O10 O10 1.50(2) 3_666 ? C102 O10 1.300(15) 3_666 ? C102 C103 1.390(8) . ? 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 O1 Ni1 N1 100.42(10) 4_465 . ? O1 Ni1 N4 94.13(9) 4_465 . ? N1 Ni1 N4 165.42(10) . . ? O1 Ni1 N7 93.61(9) 4_465 . ? N1 Ni1 N7 88.98(10) . . ? N4 Ni1 N7 89.11(10) . . ? O1 Ni1 N10 102.14(9) 4_465 . ? N1 Ni1 N10 90.67(10) . . ? N4 Ni1 N10 87.22(10) . . ? N7 Ni1 N10 164.04(10) . . ? O1 Ni1 Ni2 174.52(7) 4_465 . ? N1 Ni1 Ni2 83.07(7) . . ? N4 Ni1 Ni2 82.35(7) . . ? N7 Ni1 Ni2 82.18(7) . . ? N10 Ni1 Ni2 81.94(7) . . ? N11 Ni2 N8 179.45(11) . . ? N11 Ni2 N2 89.44(11) . . ? N8 Ni2 N2 90.47(11) . . ? N11 Ni2 N5 88.60(11) . . ? N8 Ni2 N5 91.50(11) . . ? N2 Ni2 N5 177.90(11) . . ? N11 Ni2 Ni1 90.87(7) . . ? N8 Ni2 Ni1 89.67(8) . . ? N2 Ni2 Ni1 88.73(8) . . ? N5 Ni2 Ni1 90.55(8) . . ? N11 Ni2 Ni3 89.75(7) . . ? N8 Ni2 Ni3 89.71(8) . . ? N2 Ni2 Ni3 89.32(8) . . ? N5 Ni2 Ni3 91.41(8) . . ? Ni1 Ni2 Ni3 177.96(2) . . ? O3 Ni3 N9 103.37(10) . . ? O3 Ni3 N6 101.10(10) . . ? N9 Ni3 N6 93.59(10) . . ? O3 Ni3 N12 90.86(10) . . ? N9 Ni3 N12 165.70(10) . . ? N6 Ni3 N12 84.89(10) . . ? O3 Ni3 N3 92.56(10) . . ? N9 Ni3 N3 89.74(10) . . ? N6 Ni3 N3 164.76(10) . . ? N12 Ni3 N3 88.22(10) . . ? O3 Ni3 Ni2 172.53(7) . . ? N9 Ni3 Ni2 82.72(7) . . ? N6 Ni3 Ni2 82.61(7) . . ? N12 Ni3 Ni2 82.98(7) . . ? N3 Ni3 Ni2 83.07(7) . . ? N16 Mn1 N15 89.92(10) . . ? N16 Mn1 N14 179.74(11) . . ? N15 Mn1 N14 89.84(10) . . ? N16 Mn1 N13 89.88(11) . . ? N15 Mn1 N13 179.77(11) . . ? N14 Mn1 N13 90.37(10) . . ? N16 Mn1 N18 94.76(10) . . ? N15 Mn1 N18 89.31(10) . . ? N14 Mn1 N18 85.14(10) . . ? N13 Mn1 N18 90.82(10) . . ? N16 Mn1 N17 85.21(10) . . ? N15 Mn1 N17 90.87(10) . . ? N14 Mn1 N17 94.89(10) . . ? N13 Mn1 N17 89.00(10) . . ? N18 Mn1 N17 179.81(10) . . ? C85 O1 Ni1 135.4(2) . 4_666 ? C91 O3 Ni3 138.5(2) . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Ni1 121.6(2) . . ? C5 N1 Ni1 119.4(2) . . ? C5 N2 C6 122.0(3) . . ? C5 N2 Ni2 119.6(2) . . ? C6 N2 Ni2 118.3(2) . . ? C10 N3 C6 118.7(3) . . ? C10 N3 Ni3 121.1(2) . . ? C6 N3 Ni3 119.8(2) . . ? C11 N4 C15 118.5(3) . . ? C11 N4 Ni1 119.3(2) . . ? C15 N4 Ni1 121.7(2) . . ? C16 N5 C15 122.2(3) . . ? C16 N5 Ni2 120.4(2) . . ? C15 N5 Ni2 116.3(2) . . ? C20 N6 C16 118.3(3) . . ? C20 N6 Ni3 119.6(2) . . ? C16 N6 Ni3 121.1(2) . . ? C25 N7 C21 118.8(3) . . ? C25 N7 Ni1 120.1(2) . . ? C21 N7 Ni1 121.1(2) . . ? C26 N8 C25 122.3(3) . . ? C26 N8 Ni2 117.8(2) . . ? C25 N8 Ni2 119.7(2) . . ? C30 N9 C26 118.0(3) . . ? C30 N9 Ni3 120.4(2) . . ? C26 N9 Ni3 121.1(2) . . ? C31 N10 C35 118.7(3) . . ? C31 N10 Ni1 120.8(2) . . ? C35 N10 Ni1 120.5(2) . . ? C35 N11 C36 122.6(3) . . ? C35 N11 Ni2 119.5(2) . . ? C36 N11 Ni2 117.8(2) . . ? C36 N12 C40 118.7(3) . . ? C36 N12 Ni3 119.9(2) . . ? C40 N12 Ni3 120.7(2) . . ? C44 N13 C41 106.3(3) . . ? C44 N13 Mn1 126.7(2) . . ? C41 N13 Mn1 127.0(2) . . ? C46 N14 C49 105.7(3) . . ? C46 N14 Mn1 126.9(2) . . ? C49 N14 Mn1 127.1(2) . . ? C51 N15 C54 106.4(3) . . ? C51 N15 Mn1 127.0(2) . . ? C54 N15 Mn1 126.6(2) . . ? C56 N16 C59 106.0(3) . . ? C56 N16 Mn1 127.2(2) . . ? C59 N16 Mn1 126.3(2) . . ? C90 N17 C86 116.5(3) . . ? C90 N17 Mn1 122.2(2) . . ? C86 N17 Mn1 120.1(2) . . ? C96 N18 C92 117.4(3) . . ? C96 N18 Mn1 122.2(2) . . ? C92 N18 Mn1 119.4(2) . . ? N1 C1 C2 123.1(3) . . ? C1 C2 C3 118.3(3) . . ? C4 C3 C2 119.8(3) . . ? C3 C4 C5 119.6(3) . . ? N1 C5 N2 116.0(3) . . ? N1 C5 C4 120.1(3) . . ? N2 C5 C4 123.8(3) . . ? N3 C6 N2 115.7(3) . . ? N3 C6 C7 120.3(3) . . ? N2 C6 C7 123.8(3) . . ? C8 C7 C6 119.7(3) . . ? C9 C8 C7 119.4(3) . . ? C10 C9 C8 118.7(3) . . ? N3 C10 C9 123.2(3) . . ? N4 C11 C12 123.7(3) . . ? C11 C12 C13 118.0(3) . . ? C14 C13 C12 119.6(3) . . ? C13 C14 C15 120.2(3) . . ? N4 C15 N5 115.2(3) . . ? N4 C15 C14 120.0(3) . . ? N5 C15 C14 124.5(3) . . ? N6 C16 N5 116.1(3) . . ? N6 C16 C17 120.1(3) . . ? N5 C16 C17 123.8(3) . . ? C18 C17 C16 120.3(3) . . ? C17 C18 C19 118.7(3) . . ? C20 C19 C18 118.9(3) . . ? N6 C20 C19 123.5(3) . . ? N7 C21 C22 123.0(3) . . ? C21 C22 C23 118.7(3) . . ? C24 C23 C22 119.2(3) . . ? C23 C24 C25 120.0(3) . . ? N7 C25 N8 115.5(3) . . ? N7 C25 C24 120.2(3) . . ? N8 C25 C24 124.1(3) . . ? N9 C26 N8 115.3(3) . . ? N9 C26 C27 120.6(3) . . ? N8 C26 C27 123.9(3) . . ? C28 C27 C26 119.8(3) . . ? C27 C28 C29 119.6(4) . . ? C30 C29 C28 118.4(3) . . ? N9 C30 C29 123.6(3) . . ? N10 C31 C32 123.3(3) . . ? C31 C32 C33 118.4(3) . . ? C34 C33 C32 119.6(3) . . ? C33 C34 C35 119.4(3) . . ? N10 C35 N11 115.9(3) . . ? N10 C35 C34 120.6(3) . . ? N11 C35 C34 123.3(3) . . ? N12 C36 N11 116.0(3) . . ? N12 C36 C37 120.5(3) . . ? N11 C36 C37 123.2(3) . . ? C38 C37 C36 119.4(3) . . ? C39 C38 C37 119.9(4) . . ? C40 C39 C38 117.9(3) . . ? N12 C40 C39 123.5(3) . . ? N13 C41 C60 125.9(3) . . ? N13 C41 C42 109.3(3) . . ? C60 C41 C42 124.7(3) . . ? C43 C42 C41 107.3(3) . . ? C42 C43 C44 107.9(3) . . ? N13 C44 C45 125.9(3) . . ? N13 C44 C43 109.2(3) . . ? C45 C44 C43 124.9(3) . . ? C44 C45 C46 124.6(3) . . ? C44 C45 C61 117.9(3) . . ? C46 C45 C61 117.5(3) . . ? N14 C46 C45 125.3(3) . . ? N14 C46 C47 109.7(3) . . ? C45 C46 C47 124.9(3) . . ? C48 C47 C46 107.4(3) . . ? C47 C48 C49 107.7(3) . . ? N14 C49 C50 125.9(3) . . ? N14 C49 C48 109.5(3) . . ? C50 C49 C48 124.6(3) . . ? C51 C50 C49 123.4(3) . . ? C51 C50 C67 116.5(3) . . ? C49 C50 C67 120.1(3) . . ? N15 C51 C50 126.5(3) . . ? N15 C51 C52 109.5(3) . . ? C50 C51 C52 123.9(3) . . ? C53 C52 C51 107.2(3) . . ? C52 C53 C54 107.5(3) . . ? N15 C54 C55 126.0(3) . . ? N15 C54 C53 109.5(3) . . ? C55 C54 C53 124.5(3) . . ? C56 C55 C54 124.3(3) . . ? C56 C55 C73 119.7(3) . . ? C54 C55 C73 115.9(3) . . ? N16 C56 C55 125.8(3) . . ? N16 C56 C57 109.6(3) . . ? C55 C56 C57 124.5(3) . . ? C58 C57 C56 106.9(3) . . ? C57 C58 C59 108.2(3) . . ? N16 C59 C60 126.8(3) . . ? N16 C59 C58 109.3(3) . . ? C60 C59 C58 123.9(3) . . ? C59 C60 C41 123.6(3) . . ? C59 C60 C79 117.4(3) . . ? C41 C60 C79 119.0(3) . . ? C66 C61 C62 119.0(3) . . ? C66 C61 C45 120.4(3) . . ? C62 C61 C45 120.6(3) . . ? C63 C62 C61 120.4(3) . . ? C64 C63 C62 120.4(3) . . ? C65 C64 C63 119.6(3) . . ? C64 C65 C66 120.9(3) . . ? C65 C66 C61 119.8(3) . . ? C72 C67 C68 118.6(3) . . ? C72 C67 C50 120.5(3) . . ? C68 C67 C50 120.7(3) . . ? C69 C68 C67 120.0(4) . . ? C70 C69 C68 120.9(4) . . ? C71 C70 C69 119.8(4) . . ? C70 C71 C72 120.1(4) . . ? C67 C72 C71 120.6(4) . . ? C74 C73 C78 120.1(3) . . ? C74 C73 C55 120.6(3) . . ? C78 C73 C55 119.2(3) . . ? C75 C74 C73 119.4(4) . . ? C76 C75 C74 120.7(4) . . ? C75 C76 C77 120.3(3) . . ? C76 C77 C78 119.6(4) . . ? C73 C78 C77 120.0(3) . . ? C84 C79 C80 118.0(4) . . ? C84 C79 C60 121.2(4) . . ? C80 C79 C60 120.8(4) . . ? C79 C80 C81 120.2(5) . . ? C82 C81 C80 121.3(5) . . ? C83 C82 C81 119.2(5) . . ? C82 C83 C84 120.3(5) . . ? C79 C84 C83 120.9(5) . . ? O2 C85 O1 127.3(3) . . ? O2 C85 C87 118.4(3) . . ? O1 C85 C87 114.3(3) . . ? N17 C86 C87 124.0(3) . . ? C86 C87 C88 117.9(3) . . ? C86 C87 C85 119.8(3) . . ? C88 C87 C85 122.3(3) . . ? C89 C88 C87 118.9(3) . . ? C90 C89 C88 119.2(3) . . ? N17 C90 C89 123.5(3) . . ? O4 C91 O3 127.4(3) . . ? O4 C91 C93 119.4(3) . . ? O3 C91 C93 113.2(3) . . ? N18 C92 C93 123.3(3) . . ? C94 C93 C92 118.4(3) . . ? C94 C93 C91 122.6(3) . . ? C92 C93 C91 119.0(3) . . ? C93 C94 C95 119.1(3) . . ? C94 C95 C96 118.7(3) . . ? N18 C96 C95 123.1(3) . . ? O5 Cl1 O7 109.1(2) . . ? O5 Cl1 O8 109.1(2) . . ? O7 Cl1 O8 109.8(2) . . ? O5 Cl1 O6 110.3(2) . . ? O7 Cl1 O6 109.3(2) . . ? O8 Cl1 O6 109.3(2) . . ? Cl3 C97 Cl2 109.9(3) . . ? Cl3 C97 Cl4 109.8(3) . . ? Cl2 C97 Cl4 110.5(2) . . ? C100 O9 C99 111.2(4) . . ? O9 C99 C98 109.7(4) . . ? O9 C100 C101 109.4(5) . . ? C102 O10 C102 114.4(11) 3_666 . ? C102 O10 O10 62.3(8) 3_666 3_666 ? C102 O10 O10 52.1(8) . 3_666 ? O10 C102 C103 133.6(12) 3_666 . ? O10 C102 O10 65.6(11) 3_666 . ? C103 C102 O10 108.1(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.484 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.218