# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xinxin Xu' _publ_contact_author_email xuxx@mail.neu.edu.cn loop_ _publ_author_name 'Xinxin Xu' 'Xia Zhang' 'Xiaoxia Liu' 'Linshan Wang' 'Enbo Wang' # Attachment 'Complex 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 842568' #TrackingRef 'Complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Cd2 N4 O12' _chemical_formula_weight 1089.64 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' Cd Cd -0.8075 1.2024 '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 23.7711(16) _cell_length_b 18.2299(12) _cell_length_c 10.4033(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.183(2) _cell_angle_gamma 90.00 _cell_volume 4507.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26667 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 26.31 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.547 _exptl_crystal_size_mid 0.521 _exptl_crystal_size_min 0.177 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26667 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.31 _reflns_number_total 8883 _reflns_number_gt 7563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0650P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8883 _refine_ls_number_parameters 656 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.004 _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 Cd1 Cd 0.179158(7) 0.467023(12) 0.586916(16) 0.02189(7) Uani 1 1 d . . . Cd2 Cd 0.318552(7) 0.505817(12) 0.402059(16) 0.02155(7) Uani 1 1 d . . . O6 O 0.36240(7) 0.57789(11) 0.55149(18) 0.0308(5) Uani 1 1 d . . . O1 O 0.23065(7) 0.54628(10) 0.47109(17) 0.0268(4) Uani 1 1 d . . . O5 O 0.41020(8) 0.47765(11) 0.5053(2) 0.0334(5) Uani 1 1 d . . . C1 C 0.22761(10) 0.60420(15) 0.4006(2) 0.0227(5) Uani 1 1 d . . . O2 O 0.26776(7) 0.62064(11) 0.32951(18) 0.0317(4) Uani 1 1 d . . . N1 N 0.20789(9) 0.53234(13) 0.7684(2) 0.0276(5) Uani 1 1 d . . . N3 N 0.28909(9) 0.44873(13) 0.2137(2) 0.0276(5) Uani 1 1 d . . . C13 C 0.40709(11) 0.53968(16) 0.5560(3) 0.0261(6) Uani 1 1 d . . . N4 N 0.38061(9) 0.53926(13) 0.2341(2) 0.0274(5) Uani 1 1 d . . . C4 C 0.11943(11) 0.75427(15) 0.3219(2) 0.0266(6) Uani 1 1 d . . . N2 N 0.11390(9) 0.44555(13) 0.7551(2) 0.0275(5) Uani 1 1 d . . . C3 C 0.17085(11) 0.71098(16) 0.3420(3) 0.0285(6) Uani 1 1 d D . . C14 C 0.45814(11) 0.57129(16) 0.6188(3) 0.0281(6) Uani 1 1 d D . . C35 C 0.17539(12) 0.52543(16) 0.8736(3) 0.0279(6) Uani 1 1 d . . . C47 C 0.32147(11) 0.45887(15) 0.1092(3) 0.0280(6) Uani 1 1 d . . . C2 C 0.17508(10) 0.64740(16) 0.4025(2) 0.0245(6) Uani 1 1 d D . . C43 C 0.40492(13) 0.51741(19) 0.0114(3) 0.0366(7) Uani 1 1 d . . . C19 C 0.59160(10) 0.75401(16) 0.8558(2) 0.0269(6) Uani 1 1 d . . . C25 C 0.25382(12) 0.57428(17) 0.7754(3) 0.0341(7) Uani 1 1 d . . . H25A H 0.2759 0.5789 0.7032 0.041 Uiso 1 1 calc R . . C31 C 0.09079(13) 0.47179(18) 0.9760(3) 0.0355(7) Uani 1 1 d . . . C20 C 0.60220(11) 0.69436(16) 0.7754(3) 0.0294(6) Uani 1 1 d . . . H20A H 0.6392 0.6825 0.7567 0.035 Uiso 1 1 calc R . . C15 C 0.45563(11) 0.63182(17) 0.6904(3) 0.0286(6) Uani 1 1 d D . . C9 C 0.12219(10) 0.81497(16) 0.2403(3) 0.0293(6) Uani 1 1 d . . . H9A H 0.1569 0.8298 0.2100 0.035 Uiso 1 1 calc R . . C34 C 0.06881(11) 0.40310(18) 0.7487(3) 0.0351(7) Uani 1 1 d . . . H34A H 0.0607 0.3793 0.6715 0.042 Uiso 1 1 calc R . . C21 C 0.55915(11) 0.65291(16) 0.7233(3) 0.0282(6) Uani 1 1 d . . . H21A H 0.5672 0.6133 0.6704 0.034 Uiso 1 1 calc R . . C5 C 0.06700(11) 0.73519(17) 0.3724(3) 0.0341(7) Uani 1 1 d . . . H5A H 0.0645 0.6967 0.4306 0.041 Uiso 1 1 calc R . . C16 C 0.50300(10) 0.67036(16) 0.7500(2) 0.0271(6) Uani 1 1 d . . . C8 C 0.07483(11) 0.85313(16) 0.2040(2) 0.0277(6) Uani 1 1 d . . . H8A H 0.0776 0.8934 0.1496 0.033 Uiso 1 1 calc R . . C29 C 0.15029(15) 0.5538(2) 1.0983(3) 0.0485(9) Uani 1 1 d . . . H29A H 0.1583 0.5791 1.1740 0.058 Uiso 1 1 calc R . . C37 C 0.24321(12) 0.40669(17) 0.2036(3) 0.0346(7) Uani 1 1 d . . . H37A H 0.2212 0.3994 0.2754 0.042 Uiso 1 1 calc R . . C45 C 0.45979(13) 0.5997(2) 0.1401(3) 0.0438(8) Uani 1 1 d . . . H45A H 0.4895 0.6325 0.1507 0.053 Uiso 1 1 calc R . . C42 C 0.39228(15) 0.4803(2) -0.1063(3) 0.0475(9) Uani 1 1 d . . . H42A H 0.4155 0.4862 -0.1764 0.057 Uiso 1 1 calc R . . C40 C 0.30967(13) 0.42544(18) -0.0106(3) 0.0363(7) Uani 1 1 d . . . C32 C 0.04345(13) 0.42627(19) 0.9655(3) 0.0410(8) Uani 1 1 d . . . H32A H 0.0200 0.4197 1.0350 0.049 Uiso 1 1 calc R . . C18 C 0.53574(11) 0.76923(18) 0.8864(3) 0.0349(7) Uani 1 1 d . . . H18A H 0.5279 0.8072 0.9430 0.042 Uiso 1 1 calc R . . C26 C 0.26975(13) 0.61143(19) 0.8875(3) 0.0435(8) Uani 1 1 d . . . H26A H 0.3023 0.6397 0.8905 0.052 Uiso 1 1 calc R . . C30 C 0.10445(16) 0.5107(2) 1.0915(3) 0.0476(9) Uani 1 1 d . . . H30A H 0.0815 0.5063 1.1624 0.057 Uiso 1 1 calc R . . C17 C 0.49212(11) 0.72834(18) 0.8331(3) 0.0352(7) Uani 1 1 d . . . H17A H 0.4552 0.7397 0.8530 0.042 Uiso 1 1 calc R . . C33 C 0.03248(13) 0.39184(19) 0.8516(3) 0.0413(8) Uani 1 1 d . . . H33A H 0.0014 0.3613 0.8421 0.050 Uiso 1 1 calc R . . C36 C 0.12562(11) 0.47951(16) 0.8676(3) 0.0269(6) Uani 1 1 d . . . C39 C 0.26054(14) 0.38228(18) -0.0172(3) 0.0449(8) Uani 1 1 d . . . H39A H 0.2504 0.3594 -0.0942 0.054 Uiso 1 1 calc R . . C46 C 0.42396(12) 0.58461(18) 0.2436(3) 0.0378(7) Uani 1 1 d . . . H46A H 0.4312 0.6076 0.3220 0.045 Uiso 1 1 calc R . . C38 C 0.22757(13) 0.37346(18) 0.0875(3) 0.0414(8) Uani 1 1 d . . . H38A H 0.1949 0.3455 0.0815 0.050 Uiso 1 1 calc R . . C28 C 0.18780(13) 0.56180(18) 0.9899(3) 0.0385(7) Uani 1 1 d . . . C27 C 0.23642(14) 0.60561(19) 0.9940(3) 0.0453(8) Uani 1 1 d . . . H27A H 0.2462 0.6308 1.0689 0.054 Uiso 1 1 calc R . . C44 C 0.45058(14) 0.5660(2) 0.0249(3) 0.0444(8) Uani 1 1 d . . . H44A H 0.4741 0.5749 -0.0437 0.053 Uiso 1 1 calc R . . C41 C 0.34657(15) 0.4364(2) -0.1160(3) 0.0496(9) Uani 1 1 d . . . H41A H 0.3388 0.4126 -0.1934 0.060 Uiso 1 1 calc R . . C48 C 0.37032(11) 0.50624(16) 0.1192(3) 0.0272(6) Uani 1 1 d . . . O3W O 0.15809(14) 0.25466(17) 0.7493(3) 0.0719(8) Uani 1 1 d D . . O2W O 0.36530(12) 0.72983(15) 0.4999(3) 0.0556(6) Uani 1 1 d D . . O4W O 0.11278(11) 0.25785(15) 0.5005(3) 0.0552(6) Uani 1 1 d D . . O1W O 0.32741(16) 0.74204(18) 0.2465(3) 0.0823(10) Uani 1 1 d D . . C22 C 0.63602(11) 0.80223(16) 0.9049(3) 0.0292(6) Uani 1 1 d D . . C23 C 0.68961(11) 0.80137(16) 0.8721(3) 0.0274(6) Uani 1 1 d D . . C24 C 0.72925(11) 0.85985(16) 0.9120(2) 0.0279(6) Uani 1 1 d . . . O7 O 0.77466(8) 0.86499(13) 0.84837(19) 0.0389(5) Uani 1 1 d . . . O8 O 0.71786(8) 0.90234(13) 1.0005(2) 0.0462(6) Uani 1 1 d . . . C6 C 0.01959(11) 0.77331(17) 0.3360(3) 0.0330(7) Uani 1 1 d . . . H6A H -0.0148 0.7601 0.3700 0.040 Uiso 1 1 calc R . . C7 C 0.02185(10) 0.83148(15) 0.2492(2) 0.0259(6) Uani 1 1 d . . . C10 C -0.03015(11) 0.86467(16) 0.2003(2) 0.0267(6) Uani 1 1 d D . . C11 C -0.03389(11) 0.92484(16) 0.1277(3) 0.0282(6) Uani 1 1 d D . . C12 C -0.08767(11) 0.94975(17) 0.0685(2) 0.0273(6) Uani 1 1 d . . . O3 O -0.12917(7) 0.90536(11) 0.06508(18) 0.0306(4) Uani 1 1 d . . . O4 O -0.08975(8) 1.01177(12) 0.0173(2) 0.0334(5) Uani 1 1 d . . . H4 H -0.0020(8) 0.9511(13) 0.102(2) 0.021(7) Uiso 1 1 d D . . H5 H 0.4908(8) 0.5447(15) 0.604(3) 0.033(8) Uiso 1 1 d D . . H7 H 0.6255(12) 0.8396(12) 0.961(2) 0.039(9) Uiso 1 1 d D . . H1 H 0.1444(7) 0.6268(14) 0.444(2) 0.024(7) Uiso 1 1 d D . . H8 H 0.7045(12) 0.7690(14) 0.814(2) 0.042(9) Uiso 1 1 d D . . H3 H -0.0631(8) 0.8392(15) 0.215(3) 0.038(8) Uiso 1 1 d D . . H2 H 0.2013(8) 0.7308(16) 0.300(2) 0.034(8) Uiso 1 1 d D . . H6 H 0.4204(7) 0.6517(16) 0.708(3) 0.036(8) Uiso 1 1 d D . . H10 H 0.3046(13) 0.7075(15) 0.250(3) 0.068(13) Uiso 1 1 d D . . H13 H 0.1496(13) 0.2567(19) 0.8275(14) 0.061(12) Uiso 1 1 d D . . H15 H 0.1271(14) 0.2970(12) 0.472(3) 0.061 Uiso 1 1 d D . . H16 H 0.1232(15) 0.2551(19) 0.5802(14) 0.068(14) Uiso 1 1 d D . . H11 H 0.3521(14) 0.7368(17) 0.4264(16) 0.056(12) Uiso 1 1 d D . . H12 H 0.3561(15) 0.6889(11) 0.528(3) 0.059(13) Uiso 1 1 d D . . H9 H 0.3362(14) 0.7495(18) 0.1695(14) 0.059 Uiso 1 1 d D . . H14 H 0.1821(12) 0.2878(15) 0.734(3) 0.059 Uiso 1 1 d 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 Cd1 0.01791(11) 0.02575(14) 0.02193(11) -0.00096(7) -0.00160(7) -0.00166(7) Cd2 0.01591(11) 0.02568(13) 0.02300(11) -0.00101(7) -0.00111(7) -0.00034(7) O6 0.0200(9) 0.0372(12) 0.0349(10) -0.0067(9) -0.0048(7) -0.0008(9) O1 0.0203(9) 0.0261(10) 0.0341(10) 0.0076(8) -0.0012(7) 0.0040(8) O5 0.0277(10) 0.0310(12) 0.0412(11) -0.0085(10) -0.0090(9) -0.0022(9) C1 0.0214(12) 0.0231(14) 0.0235(12) -0.0032(11) -0.0051(10) -0.0010(11) O2 0.0244(9) 0.0325(12) 0.0382(10) 0.0104(9) 0.0055(8) 0.0036(9) N1 0.0258(12) 0.0274(14) 0.0294(12) -0.0003(10) -0.0036(9) -0.0004(10) N3 0.0251(11) 0.0278(13) 0.0298(11) -0.0004(10) -0.0021(9) -0.0004(10) C13 0.0201(13) 0.0336(17) 0.0245(13) 0.0015(12) -0.0029(10) -0.0061(12) N4 0.0254(11) 0.0307(14) 0.0261(11) -0.0004(10) 0.0010(9) -0.0005(10) C4 0.0242(13) 0.0263(15) 0.0292(13) 0.0000(12) -0.0034(10) 0.0030(11) N2 0.0233(11) 0.0305(14) 0.0288(11) -0.0029(10) 0.0020(9) -0.0007(10) C3 0.0231(13) 0.0299(17) 0.0323(14) 0.0006(12) -0.0033(11) 0.0001(12) C14 0.0216(13) 0.0321(17) 0.0304(14) -0.0011(12) -0.0042(11) -0.0042(12) C35 0.0318(15) 0.0262(15) 0.0254(13) 0.0007(12) -0.0037(11) 0.0027(12) C47 0.0285(14) 0.0247(15) 0.0306(14) 0.0002(12) -0.0043(11) 0.0041(12) C2 0.0211(12) 0.0286(15) 0.0238(12) 0.0017(11) -0.0005(10) 0.0010(11) C43 0.0397(17) 0.0415(19) 0.0288(15) 0.0033(14) 0.0036(13) 0.0035(15) C19 0.0235(13) 0.0297(16) 0.0273(13) -0.0003(12) -0.0019(10) -0.0037(11) C25 0.0310(15) 0.0339(18) 0.0372(15) -0.0018(13) -0.0036(12) -0.0049(13) C31 0.0377(17) 0.0396(19) 0.0294(15) 0.0035(13) 0.0052(12) 0.0055(14) C20 0.0201(12) 0.0309(16) 0.0371(15) -0.0048(13) -0.0041(11) 0.0033(12) C15 0.0219(13) 0.0335(17) 0.0303(14) -0.0003(12) 0.0004(11) -0.0028(12) C9 0.0202(12) 0.0305(16) 0.0372(15) 0.0041(13) -0.0001(11) -0.0025(12) C34 0.0293(14) 0.0408(19) 0.0355(15) -0.0042(14) 0.0045(12) -0.0055(14) C21 0.0267(13) 0.0241(15) 0.0338(14) -0.0056(12) -0.0022(11) -0.0014(12) C5 0.0307(15) 0.0340(17) 0.0377(15) 0.0127(13) 0.0014(12) 0.0015(13) C16 0.0235(13) 0.0302(16) 0.0275(13) -0.0014(12) -0.0033(10) -0.0056(12) C8 0.0283(13) 0.0258(15) 0.0289(13) 0.0070(12) -0.0011(11) 0.0029(12) C29 0.059(2) 0.064(3) 0.0223(14) -0.0092(15) 0.0013(14) 0.0023(19) C37 0.0318(14) 0.0347(18) 0.0372(15) 0.0007(14) -0.0040(12) -0.0036(13) C45 0.0374(17) 0.047(2) 0.0471(18) 0.0028(16) 0.0083(14) -0.0119(16) C42 0.053(2) 0.066(2) 0.0238(15) -0.0027(15) 0.0101(14) 0.0014(19) C40 0.0437(17) 0.0390(19) 0.0258(14) -0.0031(13) -0.0061(12) 0.0012(14) C32 0.0384(16) 0.047(2) 0.0377(16) 0.0073(15) 0.0131(13) -0.0016(15) C18 0.0284(14) 0.0408(19) 0.0355(15) -0.0144(14) 0.0022(12) -0.0034(13) C26 0.0417(17) 0.041(2) 0.0468(18) -0.0052(16) -0.0138(14) -0.0101(15) C30 0.057(2) 0.063(2) 0.0232(15) 0.0018(15) 0.0099(14) 0.0053(19) C17 0.0223(13) 0.0439(19) 0.0394(15) -0.0090(14) 0.0025(11) -0.0023(13) C33 0.0341(16) 0.043(2) 0.0471(18) 0.0026(15) 0.0107(13) -0.0080(15) C36 0.0287(14) 0.0270(15) 0.0249(13) 0.0003(12) -0.0019(11) 0.0049(12) C39 0.0550(19) 0.042(2) 0.0369(16) -0.0071(15) -0.0146(14) -0.0080(17) C46 0.0351(16) 0.0415(19) 0.0367(16) -0.0043(14) 0.0012(12) -0.0076(14) C38 0.0415(17) 0.0378(19) 0.0443(18) -0.0018(15) -0.0133(14) -0.0124(15) C28 0.0469(18) 0.0386(19) 0.0296(15) -0.0038(13) -0.0070(13) 0.0027(15) C27 0.0505(18) 0.048(2) 0.0364(17) -0.0134(16) -0.0121(14) -0.0035(17) C44 0.0409(17) 0.053(2) 0.0398(17) 0.0085(16) 0.0129(14) -0.0039(16) C41 0.065(2) 0.057(2) 0.0263(15) -0.0112(16) -0.0029(15) -0.0016(19) C48 0.0255(14) 0.0295(16) 0.0266(13) 0.0018(12) 0.0010(11) 0.0055(12) O3W 0.102(2) 0.061(2) 0.0529(17) 0.0003(14) 0.0188(16) -0.0194(17) O2W 0.0702(18) 0.0426(17) 0.0541(16) -0.0015(13) 0.0042(14) -0.0039(14) O4W 0.0606(16) 0.0444(16) 0.0606(17) 0.0000(13) 0.0041(13) -0.0045(13) O1W 0.129(3) 0.062(2) 0.0564(17) 0.0021(15) 0.0217(18) -0.048(2) C22 0.0298(14) 0.0300(16) 0.0276(13) -0.0053(12) -0.0048(11) -0.0018(13) C23 0.0267(13) 0.0243(15) 0.0309(14) -0.0071(12) -0.0026(11) 0.0001(12) C24 0.0292(14) 0.0244(15) 0.0296(14) 0.0035(12) -0.0132(11) -0.0003(12) O7 0.0300(10) 0.0494(14) 0.0373(11) -0.0004(10) -0.0010(8) -0.0127(10) O8 0.0383(11) 0.0407(13) 0.0590(14) -0.0248(12) -0.0179(10) 0.0066(11) C6 0.0225(13) 0.0365(18) 0.0402(15) 0.0076(14) 0.0038(11) 0.0055(13) C7 0.0246(13) 0.0245(15) 0.0284(13) -0.0010(12) -0.0031(10) 0.0040(11) C10 0.0229(13) 0.0294(16) 0.0278(13) -0.0014(12) -0.0032(10) 0.0025(12) C11 0.0213(13) 0.0312(16) 0.0319(14) 0.0012(12) -0.0041(11) 0.0022(12) C12 0.0241(13) 0.0332(17) 0.0244(13) -0.0004(12) -0.0025(10) 0.0077(12) O3 0.0227(9) 0.0354(12) 0.0335(10) 0.0050(9) -0.0067(8) 0.0006(9) O4 0.0269(10) 0.0336(12) 0.0393(11) 0.0099(10) -0.0039(9) 0.0077(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 Cd1 O7 2.256(2) 2_646 ? Cd1 O3 2.2579(18) 2_545 ? Cd1 O1 2.2581(18) . ? Cd1 N1 2.323(2) . ? Cd1 N2 2.395(2) . ? Cd1 O4 2.503(2) 2_545 ? Cd1 C12 2.702(3) 2_545 ? Cd2 O6 2.2720(18) . ? Cd2 N3 2.314(2) . ? Cd2 O8 2.318(2) 2_646 ? Cd2 O1 2.3425(17) . ? Cd2 N4 2.389(2) . ? Cd2 O5 2.4629(19) . ? Cd2 O2 2.5242(19) . ? Cd2 C13 2.690(3) . ? O6 C13 1.270(3) . ? O1 C1 1.287(3) . ? O5 C13 1.251(3) . ? C1 O2 1.256(3) . ? C1 C2 1.477(3) . ? N1 C25 1.334(3) . ? N1 C35 1.359(4) . ? N3 C37 1.335(4) . ? N3 C47 1.358(4) . ? C13 C14 1.483(3) . ? N4 C46 1.323(4) . ? N4 C48 1.356(3) . ? C4 C9 1.397(4) . ? C4 C5 1.406(4) . ? C4 C3 1.467(4) . ? N2 C34 1.322(3) . ? N2 C36 1.348(3) . ? C3 C2 1.322(4) . ? C14 C15 1.334(4) . ? C35 C28 1.405(4) . ? C35 C36 1.449(4) . ? C47 C40 1.410(4) . ? C47 C48 1.449(4) . ? C43 C44 1.405(5) . ? C43 C48 1.419(4) . ? C43 C42 1.426(4) . ? C19 C18 1.399(4) . ? C19 C20 1.398(4) . ? C19 C22 1.458(4) . ? C25 C26 1.394(4) . ? C31 C32 1.400(4) . ? C31 C36 1.420(4) . ? C31 C30 1.427(4) . ? C20 C21 1.374(4) . ? C15 C16 1.455(3) . ? C9 C8 1.370(4) . ? C34 C33 1.404(4) . ? C21 C16 1.406(4) . ? C5 C6 1.370(4) . ? C16 C17 1.393(4) . ? C8 C7 1.409(4) . ? C29 C30 1.343(5) . ? C29 C28 1.459(4) . ? C37 C38 1.395(4) . ? C45 C44 1.360(4) . ? C45 C46 1.414(4) . ? C42 C41 1.351(5) . ? C40 C39 1.409(4) . ? C40 C41 1.432(5) . ? C32 C33 1.362(4) . ? C18 C17 1.384(4) . ? C26 C27 1.379(5) . ? C39 C38 1.365(5) . ? C28 C27 1.405(4) . ? C22 C23 1.326(4) . ? C23 C24 1.477(4) . ? C24 O8 1.238(3) . ? C24 O7 1.281(3) . ? O7 Cd1 2.256(2) 2_656 ? O8 Cd2 2.318(2) 2_656 ? C6 C7 1.395(4) . ? C7 C10 1.458(3) . ? C10 C11 1.334(4) . ? C11 C12 1.479(3) . ? C12 O4 1.250(3) . ? C12 O3 1.276(3) . ? C12 Cd1 2.702(3) 2 ? O3 Cd1 2.2579(18) 2 ? O4 Cd1 2.503(2) 2 ? 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 O7 Cd1 O3 92.54(7) 2_646 2_545 ? O7 Cd1 O1 114.90(7) 2_646 . ? O3 Cd1 O1 103.18(7) 2_545 . ? O7 Cd1 N1 92.70(8) 2_646 . ? O3 Cd1 N1 165.04(7) 2_545 . ? O1 Cd1 N1 87.25(7) . . ? O7 Cd1 N2 88.04(8) 2_646 . ? O3 Cd1 N2 95.21(7) 2_545 . ? O1 Cd1 N2 149.44(8) . . ? N1 Cd1 N2 70.97(8) . . ? O7 Cd1 O4 143.31(7) 2_646 2_545 ? O3 Cd1 O4 55.18(7) 2_545 2_545 ? O1 Cd1 O4 91.44(6) . 2_545 ? N1 Cd1 O4 114.70(7) . 2_545 ? N2 Cd1 O4 79.20(7) . 2_545 ? O7 Cd1 C12 117.61(8) 2_646 2_545 ? O3 Cd1 C12 28.03(8) 2_545 2_545 ? O1 Cd1 C12 101.17(7) . 2_545 ? N1 Cd1 C12 139.98(8) . 2_545 ? N2 Cd1 C12 83.84(8) . 2_545 ? O4 Cd1 C12 27.46(8) 2_545 2_545 ? O6 Cd2 N3 164.98(8) . . ? O6 Cd2 O8 109.98(8) . 2_646 ? N3 Cd2 O8 83.97(8) . 2_646 ? O6 Cd2 O1 90.44(6) . . ? N3 Cd2 O1 98.33(7) . . ? O8 Cd2 O1 77.21(7) 2_646 . ? O6 Cd2 N4 94.10(7) . . ? N3 Cd2 N4 71.10(8) . . ? O8 Cd2 N4 140.29(8) 2_646 . ? O1 Cd2 N4 135.40(7) . . ? O6 Cd2 O5 55.47(7) . . ? N3 Cd2 O5 121.66(7) . . ? O8 Cd2 O5 88.55(7) 2_646 . ? O1 Cd2 O5 135.93(6) . . ? N4 Cd2 O5 79.53(7) . . ? O6 Cd2 O2 86.27(7) . . ? N3 Cd2 O2 89.16(7) . . ? O8 Cd2 O2 128.69(7) 2_646 . ? O1 Cd2 O2 53.58(6) . . ? N4 Cd2 O2 82.44(7) . . ? O5 Cd2 O2 135.77(7) . . ? O6 Cd2 C13 28.08(8) . . ? N3 Cd2 C13 145.76(8) . . ? O8 Cd2 C13 102.78(8) 2_646 . ? O1 Cd2 C13 115.91(7) . . ? N4 Cd2 C13 83.67(8) . . ? O5 Cd2 C13 27.65(8) . . ? O2 Cd2 C13 110.56(8) . . ? C13 O6 Cd2 94.57(16) . . ? C1 O1 Cd1 143.56(16) . . ? C1 O1 Cd2 97.10(15) . . ? Cd1 O1 Cd2 117.32(8) . . ? C13 O5 Cd2 86.34(15) . . ? O2 C1 O1 119.8(2) . . ? O2 C1 C2 122.3(2) . . ? O1 C1 C2 117.9(2) . . ? C1 O2 Cd2 89.46(16) . . ? C25 N1 C35 119.2(2) . . ? C25 N1 Cd1 124.43(19) . . ? C35 N1 Cd1 116.41(18) . . ? C37 N3 C47 119.4(2) . . ? C37 N3 Cd2 123.87(19) . . ? C47 N3 Cd2 116.76(18) . . ? O5 C13 O6 122.5(2) . . ? O5 C13 C14 118.8(2) . . ? O6 C13 C14 118.7(3) . . ? O5 C13 Cd2 66.02(14) . . ? O6 C13 Cd2 57.34(13) . . ? C14 C13 Cd2 167.0(2) . . ? C46 N4 C48 118.0(2) . . ? C46 N4 Cd2 126.60(19) . . ? C48 N4 Cd2 115.38(18) . . ? C9 C4 C5 118.4(2) . . ? C9 C4 C3 117.6(2) . . ? C5 C4 C3 123.8(3) . . ? C34 N2 C36 117.7(2) . . ? C34 N2 Cd1 126.55(18) . . ? C36 N2 Cd1 115.71(18) . . ? C2 C3 C4 126.5(3) . . ? C15 C14 C13 121.5(3) . . ? N1 C35 C28 122.5(3) . . ? N1 C35 C36 119.7(2) . . ? C28 C35 C36 117.8(3) . . ? N3 C47 C40 122.9(3) . . ? N3 C47 C48 119.3(2) . . ? C40 C47 C48 117.8(3) . . ? C3 C2 C1 121.1(2) . . ? C44 C43 C48 118.1(3) . . ? C44 C43 C42 122.3(3) . . ? C48 C43 C42 119.7(3) . . ? C18 C19 C20 118.3(2) . . ? C18 C19 C22 119.0(3) . . ? C20 C19 C22 122.7(2) . . ? N1 C25 C26 122.2(3) . . ? C32 C31 C36 118.6(3) . . ? C32 C31 C30 121.9(3) . . ? C36 C31 C30 119.5(3) . . ? C21 C20 C19 121.4(2) . . ? C14 C15 C16 126.5(3) . . ? C8 C9 C4 121.4(2) . . ? N2 C34 C33 123.9(3) . . ? C20 C21 C16 120.0(3) . . ? C6 C5 C4 120.1(3) . . ? C17 C16 C21 118.9(2) . . ? C17 C16 C15 118.6(2) . . ? C21 C16 C15 122.4(2) . . ? C9 C8 C7 120.1(3) . . ? C30 C29 C28 121.7(3) . . ? N3 C37 C38 121.4(3) . . ? C44 C45 C46 119.6(3) . . ? C41 C42 C43 120.0(3) . . ? C39 C40 C47 115.7(3) . . ? C39 C40 C41 124.1(3) . . ? C47 C40 C41 120.2(3) . . ? C33 C32 C31 118.7(3) . . ? C17 C18 C19 120.6(3) . . ? C27 C26 C25 118.9(3) . . ? C29 C30 C31 120.3(3) . . ? C18 C17 C16 120.7(3) . . ? C32 C33 C34 119.1(3) . . ? N2 C36 C31 122.0(3) . . ? N2 C36 C35 117.2(2) . . ? C31 C36 C35 120.8(3) . . ? C38 C39 C40 121.1(3) . . ? N4 C46 C45 123.0(3) . . ? C39 C38 C37 119.5(3) . . ? C35 C28 C27 116.9(3) . . ? C35 C28 C29 119.8(3) . . ? C27 C28 C29 123.3(3) . . ? C26 C27 C28 120.4(3) . . ? C45 C44 C43 118.9(3) . . ? C42 C41 C40 122.0(3) . . ? N4 C48 C43 122.4(3) . . ? N4 C48 C47 117.2(2) . . ? C43 C48 C47 120.4(3) . . ? C23 C22 C19 126.5(3) . . ? C22 C23 C24 122.0(3) . . ? O8 C24 O7 122.6(3) . . ? O8 C24 C23 120.9(3) . . ? O7 C24 C23 116.5(2) . . ? C24 O7 Cd1 108.43(18) . 2_656 ? C24 O8 Cd2 157.6(2) . 2_656 ? C5 C6 C7 121.5(3) . . ? C6 C7 C8 118.4(2) . . ? C6 C7 C10 119.8(2) . . ? C8 C7 C10 121.6(2) . . ? C11 C10 C7 125.8(3) . . ? C10 C11 C12 122.4(3) . . ? O4 C12 O3 122.5(2) . . ? O4 C12 C11 118.8(3) . . ? O3 C12 C11 118.6(3) . . ? O4 C12 Cd1 67.37(14) . 2 ? O3 C12 Cd1 56.26(13) . 2 ? C11 C12 Cd1 164.4(2) . 2 ? C12 O3 Cd1 95.71(16) . 2 ? C12 O4 Cd1 85.16(16) . 2 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.883 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.080 data_1 _database_code_depnum_ccdc_archive 'CCDC 854463' #TrackingRef 'Complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C125 H134 N10 Ni5 O32' _chemical_formula_weight 2581.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 27.3120(5) _cell_length_b 27.3120(5) _cell_length_c 34.5543(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25775.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60735 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10800 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _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 60735 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11207 _reflns_number_gt 6706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0600P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11207 _refine_ls_number_parameters 858 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.927 _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 Ni3 Ni 0.0000 0.7500 0.09568(2) 0.03047(18) Uani 1 2 d S . . Ni2 Ni 0.775865(17) 0.298543(16) 0.093527(14) 0.02736(13) Uani 1 1 d . . . Ni1 Ni 0.384327(17) 0.548555(16) 0.096428(14) 0.02928(14) Uani 1 1 d . . . O10 O 0.01931(9) 0.82103(8) 0.08331(7) 0.0338(6) Uani 1 1 d . . . O6 O 0.79112(9) 0.36759(8) 0.07481(7) 0.0307(6) Uani 1 1 d . . . O5 O 0.72898(9) 0.32916(8) 0.04826(7) 0.0312(6) Uani 1 1 d . . . O2 O 0.40264(9) 0.62000(8) 0.08264(7) 0.0348(7) Uani 1 1 d . . . O1 O 0.34307(9) 0.58363(9) 0.05120(7) 0.0330(6) Uani 1 1 d . . . O9 O -0.04254(9) 0.78763(9) 0.05241(7) 0.0360(7) Uani 1 1 d . . . N2 N 0.72706(11) 0.32645(10) 0.13353(9) 0.0302(7) Uani 1 1 d . . . C1 C 0.36996(14) 0.62072(13) 0.05647(11) 0.0299(9) Uani 1 1 d . . . N3 N 0.33109(13) 0.56691(11) 0.13523(9) 0.0383(8) Uani 1 1 d . . . N5 N 0.83295(11) 0.29017(11) 0.13112(9) 0.0327(8) Uani 1 1 d . . . N1 N 0.43911(12) 0.53423(11) 0.13502(9) 0.0337(8) Uani 1 1 d . . . N4 N 0.05317(12) 0.73328(11) 0.13615(9) 0.0348(8) Uani 1 1 d . . . C2 C 0.36327(14) 0.66451(13) 0.03195(11) 0.0298(9) Uani 1 1 d D . . C28 C 0.00246(14) 0.95477(13) 0.01920(11) 0.0333(9) Uani 1 1 d . . . C9 C 0.35192(14) 0.75759(13) -0.01494(12) 0.0389(10) Uani 1 1 d . . . H9A H 0.3299 0.7328 -0.0211 0.047 Uiso 1 1 calc R . . C20 C 0.73832(14) 0.55050(13) -0.03808(11) 0.0347(10) Uani 1 1 d . . . H20A H 0.7185 0.5551 -0.0597 0.042 Uiso 1 1 calc R . . C13 C 0.75517(13) 0.36726(13) 0.05134(10) 0.0271(9) Uani 1 1 d . . . C27 C 0.00608(16) 0.90819(14) 0.03973(11) 0.0352(10) Uani 1 1 d D . . C26 C -0.02249(15) 0.86956(14) 0.03585(11) 0.0326(9) Uani 1 1 d D . . C16 C 0.76631(14) 0.49898(13) 0.01373(11) 0.0313(9) Uani 1 1 d . . . C4 C 0.38512(14) 0.75082(13) 0.01525(11) 0.0342(10) Uani 1 1 d . . . C21 C 0.73682(13) 0.50646(13) -0.01842(11) 0.0326(9) Uani 1 1 d . . . H21A H 0.7159 0.4817 -0.0268 0.039 Uiso 1 1 calc R . . C14 C 0.74528(14) 0.41100(13) 0.02769(11) 0.0281(9) Uani 1 1 d D . . C3 C 0.38769(16) 0.70545(14) 0.03778(12) 0.0378(10) Uani 1 1 d D . . C15 C 0.76791(14) 0.45252(13) 0.03518(11) 0.0305(9) Uani 1 1 d D . . C18 C 0.79886(16) 0.58056(14) 0.00602(12) 0.0483(12) Uani 1 1 d . . . H18A H 0.8200 0.6051 0.0143 0.058 Uiso 1 1 calc R . . C25 C -0.01530(14) 0.82432(13) 0.05789(11) 0.0309(9) Uani 1 1 d . . . C31 C 0.51973(15) 0.50265(14) 0.17814(12) 0.0374(10) Uani 1 1 d . . . C5 C 0.41650(17) 0.78869(15) 0.02404(13) 0.0533(13) Uani 1 1 d . . . H5A H 0.4384 0.7849 0.0444 0.064 Uiso 1 1 calc R . . C33 C 0.48433(16) 0.54901(14) 0.12703(12) 0.0413(11) Uani 1 1 d . . . H33A H 0.4888 0.5703 0.1063 0.050 Uiso 1 1 calc R . . C60 C 0.83748(16) 0.25122(15) 0.15375(12) 0.0451(11) Uani 1 1 d . . . H60A H 0.8125 0.2280 0.1533 0.054 Uiso 1 1 calc R . . C34 C 0.43377(15) 0.50403(15) 0.16475(12) 0.0431(11) Uani 1 1 d . . . H34A H 0.4024 0.4933 0.1710 0.052 Uiso 1 1 calc R . . C29 C 0.03982(15) 0.98862(14) 0.02233(12) 0.0430(11) Uani 1 1 d . . . H29A H 0.0669 0.9813 0.0376 0.052 Uiso 1 1 calc R . . C54 C 0.09809(16) 0.75260(14) 0.13257(12) 0.0412(11) Uani 1 1 d . . . H54A H 0.1045 0.7731 0.1117 0.049 Uiso 1 1 calc R . . C19 C 0.76922(14) 0.58823(13) -0.02597(11) 0.0342(10) Uani 1 1 d . . . C30 C -0.03811(15) 0.96683(14) -0.00332(12) 0.0426(11) Uani 1 1 d . . . H30A H -0.0640 0.9449 -0.0056 0.051 Uiso 1 1 calc R . . C48 C 0.24516(17) 0.57107(15) 0.14873(13) 0.0486(12) Uani 1 1 d . . . H48A H 0.2138 0.5604 0.1424 0.058 Uiso 1 1 calc R . . C8 C 0.35146(15) 0.80088(13) -0.03576(12) 0.0400(10) Uani 1 1 d . . . H8A H 0.3297 0.8044 -0.0563 0.048 Uiso 1 1 calc R . . C58 C 0.90927(16) 0.31757(17) 0.15635(15) 0.0581(13) Uani 1 1 d . . . H58A H 0.9336 0.3414 0.1564 0.070 Uiso 1 1 calc R . . C35 C 0.47287(16) 0.48776(15) 0.18699(12) 0.0450(11) Uani 1 1 d . . . H35A H 0.4674 0.4669 0.2078 0.054 Uiso 1 1 calc R . . C36 C 0.56349(15) 0.48292(15) 0.19943(12) 0.0450(11) Uani 1 1 d . . . H36A H 0.5534 0.4716 0.2248 0.054 Uiso 1 1 calc R . . H36B H 0.5872 0.5090 0.2030 0.054 Uiso 1 1 calc R . . C57 C 0.91342(16) 0.27612(17) 0.18012(12) 0.0479(12) Uani 1 1 d . . . C37 C 0.58747(14) 0.44081(14) 0.17760(11) 0.0389(10) Uani 1 1 d . . . H37A H 0.5637 0.4148 0.1740 0.047 Uiso 1 1 calc R . . H37B H 0.5975 0.4521 0.1522 0.047 Uiso 1 1 calc R . . C17 C 0.79710(16) 0.53658(14) 0.02569(12) 0.0453(11) Uani 1 1 d . . . H17A H 0.8169 0.5320 0.0473 0.054 Uiso 1 1 calc R . . C56 C 0.08120(17) 0.69296(16) 0.19299(13) 0.0507(12) Uani 1 1 d . . . H56A H 0.0741 0.6719 0.2134 0.061 Uiso 1 1 calc R . . C53 C 0.13471(16) 0.74338(15) 0.15840(12) 0.0435(11) Uani 1 1 d . . . H53A H 0.1653 0.7576 0.1546 0.052 Uiso 1 1 calc R . . C59 C 0.86930(16) 0.32253(16) 0.13319(13) 0.0524(12) Uani 1 1 d . . . H59A H 0.8672 0.3504 0.1178 0.063 Uiso 1 1 calc R . . C55 C 0.04531(16) 0.70349(15) 0.16597(12) 0.0448(11) Uani 1 1 d . . . H55A H 0.0146 0.6892 0.1688 0.054 Uiso 1 1 calc R . . C47 C 0.28477(16) 0.55325(14) 0.12887(12) 0.0451(11) Uani 1 1 d . . . H47A H 0.2790 0.5301 0.1097 0.054 Uiso 1 1 calc R . . C42 C 0.67899(14) 0.32747(13) 0.12669(11) 0.0351(10) Uani 1 1 d . . . H42A H 0.6665 0.3074 0.1073 0.042 Uiso 1 1 calc R . . C43 C 0.64710(15) 0.35666(14) 0.14688(11) 0.0383(10) Uani 1 1 d . . . H43A H 0.6139 0.3564 0.1408 0.046 Uiso 1 1 calc R . . C44 C 0.25133(17) 0.60436(16) 0.17776(13) 0.0494(12) Uani 1 1 d . . . C32 C 0.52457(15) 0.53476(15) 0.14745(12) 0.0448(11) Uani 1 1 d . . . H32A H 0.5553 0.5467 0.1407 0.054 Uiso 1 1 calc R . . C41 C 0.74302(16) 0.35468(16) 0.16220(12) 0.0479(12) Uani 1 1 d . . . H41A H 0.7762 0.3541 0.1681 0.057 Uiso 1 1 calc R . . C52 C 0.12716(16) 0.71325(15) 0.19016(12) 0.0410(11) Uani 1 1 d . . . C39 C 0.66406(15) 0.38652(14) 0.17630(11) 0.0366(10) Uani 1 1 d . . . C38 C 0.63155(16) 0.42081(16) 0.19874(12) 0.0525(12) Uani 1 1 d . . . H38A H 0.6513 0.4483 0.2074 0.063 Uiso 1 1 calc R . . H38B H 0.6201 0.4038 0.2217 0.063 Uiso 1 1 calc R . . C61 C 0.87636(17) 0.24302(16) 0.17762(13) 0.0529(12) Uani 1 1 d . . . H61A H 0.8776 0.2145 0.1923 0.063 Uiso 1 1 calc R . . C46 C 0.33751(17) 0.59786(18) 0.16381(14) 0.0625(14) Uani 1 1 d . . . H46A H 0.3693 0.6072 0.1700 0.075 Uiso 1 1 calc R . . C51 C 0.16629(16) 0.70472(17) 0.22012(13) 0.0562(13) Uani 1 1 d . . . H51A H 0.1530 0.6838 0.2402 0.067 Uiso 1 1 calc R . . H51B H 0.1744 0.7359 0.2320 0.067 Uiso 1 1 calc R . . C40 C 0.71312(15) 0.38465(15) 0.18360(12) 0.0484(12) Uani 1 1 d . . . H40A H 0.7264 0.4038 0.2032 0.058 Uiso 1 1 calc R . . C50 C 0.21323(16) 0.68160(17) 0.20490(14) 0.0586(13) Uani 1 1 d . . . H50A H 0.2222 0.6972 0.1807 0.070 Uiso 1 1 calc R . . H50B H 0.2394 0.6874 0.2233 0.070 Uiso 1 1 calc R . . C62 C 0.95682(11) 0.26748(13) 0.20581(9) 0.0659(15) Uani 1 1 d . . . H62A H 0.9490 0.2429 0.2251 0.079 Uiso 1 1 calc R . . H62B H 0.9655 0.2975 0.2191 0.079 Uiso 1 1 calc R . . C63 C 0.99995(11) 0.24997(13) 0.18079(9) 0.067(2) Uani 1 2 d SR . . H63A H 0.9892 0.2233 0.1643 0.067 Uiso 0.50 1 calc PR . . H63B H 1.0107 0.2766 0.1642 0.067 Uiso 0.50 1 calc PR . . C49 C 0.20823(11) 0.62801(13) 0.19845(9) 0.0654(15) Uani 1 1 d R . . H49A H 0.1788 0.6221 0.1834 0.078 Uiso 1 1 calc R . . H49B H 0.2040 0.6121 0.2233 0.078 Uiso 1 1 calc R . . C45 C 0.2993(2) 0.6174(2) 0.18535(15) 0.0764(17) Uani 1 1 d . . . H45A H 0.3060 0.6394 0.2051 0.092 Uiso 1 1 calc R . . O4W O 0.10528(15) 1.00117(16) 0.10480(11) 0.0737(11) Uani 1 1 d D . . O5W O 0.11688(12) 0.83947(12) 0.05838(11) 0.0582(9) Uani 1 1 d D . . O6W O 0.12632(13) 0.75302(13) 0.01660(11) 0.0699(10) Uani 1 1 d D . . O1W O 0.15431(14) 0.91242(14) 0.10612(11) 0.0612(9) Uani 1 1 d D . . O2W O 0.45690(14) 0.69181(14) 0.12666(11) 0.0777(11) Uani 1 1 d D . . O3W O 0.88256(14) 0.41250(18) 0.05761(16) 0.0851(12) Uani 1 1 d D . . C7 C 0.38287(14) 0.83902(13) -0.02656(12) 0.0365(10) Uani 1 1 d . . . C10 C 0.37963(16) 0.88520(14) -0.04770(12) 0.0374(10) Uani 1 1 d D . . C6 C 0.41649(16) 0.83189(15) 0.00360(13) 0.0492(12) Uani 1 1 d . . . H6A H 0.4388 0.8564 0.0098 0.059 Uiso 1 1 calc R . . C11 C 0.40315(15) 0.92585(14) -0.04042(12) 0.0361(10) Uani 1 1 d D . . C12 C 0.39739(14) 0.97220(14) -0.06182(11) 0.0322(9) Uani 1 1 d . . . O3 O 0.36561(9) 0.97583(8) -0.08873(7) 0.0318(6) Uani 1 1 d . . . O4 O 0.42356(10) 1.00859(9) -0.05315(7) 0.0362(7) Uani 1 1 d . . . C22 C 0.76880(15) 0.63503(14) -0.04659(11) 0.0344(10) Uani 1 1 d D . . C23 C 0.79602(15) 0.67405(14) -0.04032(11) 0.0346(10) Uani 1 1 d D . . C24 C 0.78960(14) 0.72027(13) -0.06088(11) 0.0304(9) Uani 1 1 d . . . O8 O 0.75903(9) 0.72441(8) -0.08857(7) 0.0320(6) Uani 1 1 d . . . O7 O 0.81431(9) 0.75743(9) -0.05064(7) 0.0356(7) Uani 1 1 d . . . H1 H 0.1769(13) 0.9040(15) 0.1212(12) 0.09(2) Uiso 1 1 d D . . H11 H 0.1020(9) 0.7364(12) 0.0234(10) 0.047(13) Uiso 1 1 d D . . H10 H 0.1233(12) 0.8149(10) 0.0449(11) 0.055(16) Uiso 1 1 d D . . H9 H 0.0873(6) 0.8390(14) 0.0648(12) 0.067(17) Uiso 1 1 d D . . H7 H 0.0825(15) 0.9999(18) 0.1212(13) 0.12(3) Uiso 1 1 d D . . H12 H 0.1360(15) 0.7436(16) -0.0053(7) 0.09(2) Uiso 1 1 d D . . H2 H 0.1425(18) 0.8871(10) 0.0958(15) 0.11(3) Uiso 1 1 d D . . H5 H 0.8854(18) 0.433(2) 0.0759(14) 0.14(4) Uiso 1 1 d D . . H6 H 0.8534(7) 0.4022(17) 0.0576(14) 0.09(2) Uiso 1 1 d D . . H8 H 0.1211(18) 0.9746(12) 0.1055(17) 0.13(3) Uiso 1 1 d D . . H3 H 0.441(2) 0.672(2) 0.1129(19) 0.195 Uiso 1 1 d D . . H4 H 0.4866(8) 0.691(3) 0.120(2) 0.195 Uiso 1 1 d D . . H23A H 0.8202(10) 0.6751(13) -0.0214(8) 0.042(12) Uiso 1 1 d D . . H3A H 0.4078(11) 0.7062(12) 0.0595(7) 0.036(11) Uiso 1 1 d D . . H10A H 0.3591(10) 0.8854(12) -0.0691(6) 0.030(10) Uiso 1 1 d D . . H14A H 0.7236(9) 0.4073(11) 0.0071(6) 0.019(9) Uiso 1 1 d D . . H11A H 0.4243(9) 0.9264(11) -0.0196(6) 0.022(9) Uiso 1 1 d D . . H26A H -0.0486(8) 0.8700(11) 0.0188(8) 0.024(10) Uiso 1 1 d D . . H2A H 0.3393(8) 0.6604(11) 0.0134(7) 0.020(9) Uiso 1 1 d D . . H22A H 0.7443(9) 0.6386(12) -0.0650(7) 0.034(10) Uiso 1 1 d D . . H27A H 0.0333(9) 0.9048(14) 0.0554(9) 0.050(13) Uiso 1 1 d D . . H15A H 0.7902(10) 0.4510(13) 0.0554(7) 0.043(12) Uiso 1 1 d 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 Ni3 0.0408(4) 0.0213(4) 0.0293(4) 0.000 0.000 -0.0053(3) Ni2 0.0333(3) 0.0185(3) 0.0303(3) -0.0006(2) -0.0017(2) 0.0004(2) Ni1 0.0396(3) 0.0194(3) 0.0288(3) 0.0001(2) -0.0040(2) 0.0008(2) O10 0.0391(16) 0.0240(15) 0.0382(16) 0.0004(12) -0.0060(13) -0.0086(12) O6 0.0285(15) 0.0193(14) 0.0443(17) 0.0010(12) -0.0067(13) -0.0041(11) O5 0.0384(16) 0.0226(14) 0.0326(16) 0.0001(11) -0.0021(12) -0.0056(12) O2 0.0440(17) 0.0208(14) 0.0395(17) 0.0033(12) -0.0102(13) -0.0047(12) O1 0.0439(17) 0.0236(14) 0.0315(16) 0.0031(12) -0.0038(12) -0.0048(12) O9 0.0445(17) 0.0267(15) 0.0370(17) 0.0027(12) -0.0030(13) -0.0077(13) N2 0.038(2) 0.0233(18) 0.0289(19) 0.0007(14) -0.0003(15) 0.0023(14) C1 0.036(2) 0.027(2) 0.026(2) 0.0005(17) -0.0005(18) 0.0052(18) N3 0.054(2) 0.032(2) 0.029(2) -0.0018(15) -0.0042(17) 0.0078(17) N5 0.037(2) 0.0244(18) 0.037(2) 0.0015(15) -0.0037(16) 0.0021(15) N1 0.043(2) 0.0253(18) 0.033(2) -0.0019(15) -0.0050(16) 0.0008(15) N4 0.047(2) 0.0243(18) 0.033(2) -0.0005(15) 0.0049(16) 0.0015(16) C2 0.030(2) 0.029(2) 0.030(2) 0.0049(18) 0.0004(18) 0.0006(18) C28 0.042(2) 0.025(2) 0.033(2) 0.0004(17) -0.0034(19) -0.0027(19) C9 0.044(3) 0.023(2) 0.050(3) 0.0024(19) -0.006(2) -0.0044(18) C20 0.041(2) 0.031(2) 0.033(2) 0.0057(18) -0.0075(19) -0.0005(19) C13 0.031(2) 0.026(2) 0.025(2) -0.0023(16) 0.0058(17) -0.0030(17) C27 0.045(3) 0.031(2) 0.030(2) 0.0006(18) -0.002(2) 0.000(2) C26 0.039(3) 0.030(2) 0.029(2) 0.0038(18) -0.0042(19) -0.0001(19) C16 0.038(2) 0.023(2) 0.033(2) 0.0039(17) -0.0053(19) 0.0012(17) C4 0.047(3) 0.022(2) 0.034(2) 0.0020(17) -0.0048(19) -0.0044(19) C21 0.036(2) 0.019(2) 0.043(3) 0.0045(18) -0.0016(19) -0.0057(17) C14 0.034(2) 0.025(2) 0.025(2) 0.0003(17) -0.0005(18) -0.0006(17) C3 0.050(3) 0.029(2) 0.034(3) 0.0018(19) -0.007(2) -0.001(2) C15 0.038(2) 0.024(2) 0.030(2) 0.0020(17) -0.0060(19) 0.0038(18) C18 0.066(3) 0.026(2) 0.053(3) 0.002(2) -0.026(2) -0.014(2) C25 0.037(2) 0.027(2) 0.029(2) 0.0001(17) 0.0067(19) -0.0053(19) C31 0.048(3) 0.031(2) 0.034(3) -0.0123(19) -0.007(2) 0.010(2) C5 0.069(3) 0.042(3) 0.049(3) 0.013(2) -0.026(2) -0.005(2) C33 0.053(3) 0.037(3) 0.034(3) 0.0018(19) -0.002(2) -0.003(2) C60 0.054(3) 0.044(3) 0.037(3) 0.014(2) -0.013(2) -0.009(2) C34 0.040(3) 0.048(3) 0.041(3) 0.012(2) -0.005(2) 0.001(2) C29 0.045(3) 0.036(3) 0.048(3) 0.008(2) -0.014(2) -0.003(2) C54 0.055(3) 0.033(2) 0.035(3) 0.0063(19) -0.005(2) -0.009(2) C19 0.039(2) 0.024(2) 0.039(3) 0.0060(18) -0.0057(19) -0.0003(18) C30 0.043(3) 0.029(2) 0.056(3) 0.009(2) -0.012(2) -0.0088(19) C48 0.053(3) 0.041(3) 0.053(3) -0.002(2) 0.011(2) -0.005(2) C8 0.046(3) 0.029(2) 0.044(3) 0.012(2) -0.015(2) 0.001(2) C58 0.041(3) 0.052(3) 0.081(4) 0.012(3) -0.024(3) -0.009(2) C35 0.055(3) 0.044(3) 0.036(3) 0.011(2) -0.007(2) 0.003(2) C36 0.047(3) 0.048(3) 0.040(3) -0.012(2) -0.011(2) 0.016(2) C57 0.043(3) 0.060(3) 0.041(3) 0.000(2) -0.007(2) 0.012(2) C37 0.044(3) 0.038(2) 0.034(2) -0.0043(19) -0.0054(19) 0.008(2) C17 0.061(3) 0.030(2) 0.045(3) 0.007(2) -0.024(2) -0.010(2) C56 0.063(3) 0.047(3) 0.042(3) 0.022(2) 0.007(2) 0.017(2) C53 0.049(3) 0.041(3) 0.041(3) 0.005(2) -0.002(2) -0.001(2) C59 0.055(3) 0.038(3) 0.064(3) 0.014(2) -0.020(3) -0.003(2) C55 0.049(3) 0.043(3) 0.043(3) 0.012(2) 0.009(2) 0.001(2) C47 0.055(3) 0.030(2) 0.050(3) -0.009(2) 0.008(2) -0.003(2) C42 0.039(3) 0.031(2) 0.035(2) -0.0016(18) 0.0013(19) -0.0063(19) C43 0.032(2) 0.041(3) 0.042(3) -0.006(2) 0.0007(19) -0.0006(19) C44 0.053(3) 0.048(3) 0.047(3) -0.003(2) 0.011(2) 0.001(2) C32 0.037(3) 0.048(3) 0.049(3) -0.002(2) -0.005(2) 0.000(2) C41 0.042(3) 0.056(3) 0.046(3) -0.019(2) -0.012(2) 0.010(2) C52 0.047(3) 0.038(3) 0.038(3) 0.003(2) 0.003(2) 0.019(2) C39 0.046(3) 0.034(2) 0.030(2) -0.0011(19) -0.001(2) 0.009(2) C38 0.059(3) 0.060(3) 0.039(3) -0.014(2) -0.007(2) 0.024(2) C61 0.065(3) 0.037(3) 0.057(3) 0.013(2) -0.019(3) -0.001(2) C46 0.048(3) 0.078(4) 0.061(3) -0.025(3) -0.009(3) 0.012(3) C51 0.061(3) 0.062(3) 0.046(3) 0.007(2) 0.001(2) 0.024(3) C40 0.047(3) 0.054(3) 0.044(3) -0.022(2) -0.014(2) 0.012(2) C50 0.055(3) 0.058(3) 0.063(3) 0.009(3) 0.001(3) 0.009(2) C62 0.048(3) 0.086(4) 0.064(4) 0.016(3) -0.008(3) 0.009(3) C63 0.054(5) 0.110(6) 0.037(4) 0.000 0.000 -0.016(4) C49 0.072(4) 0.053(3) 0.070(4) -0.014(3) 0.036(3) -0.007(3) C45 0.085(4) 0.087(4) 0.058(4) -0.046(3) -0.006(3) 0.016(3) O4W 0.061(3) 0.109(4) 0.051(2) 0.000(2) 0.007(2) 0.020(2) O5W 0.042(2) 0.052(2) 0.080(3) 0.002(2) 0.0066(19) -0.0073(16) O6W 0.061(3) 0.081(3) 0.068(3) -0.021(2) 0.027(2) -0.033(2) O1W 0.053(2) 0.079(3) 0.052(2) 0.007(2) -0.0082(18) 0.005(2) O2W 0.089(3) 0.074(3) 0.070(3) -0.005(2) -0.024(2) -0.021(2) O3W 0.038(2) 0.085(3) 0.132(4) 0.030(3) 0.005(2) -0.009(2) C7 0.044(3) 0.025(2) 0.040(3) 0.0053(19) -0.002(2) 0.0002(19) C10 0.049(3) 0.030(2) 0.033(3) 0.0048(19) 0.000(2) 0.002(2) C6 0.064(3) 0.030(2) 0.054(3) 0.012(2) -0.024(2) -0.012(2) C11 0.044(3) 0.031(2) 0.034(3) 0.0055(19) -0.003(2) 0.004(2) C12 0.037(2) 0.027(2) 0.033(2) 0.0014(18) 0.0083(19) 0.0066(19) O3 0.0399(16) 0.0213(14) 0.0342(16) 0.0023(11) -0.0012(13) 0.0014(11) O4 0.0478(18) 0.0275(15) 0.0335(16) 0.0022(12) -0.0030(13) -0.0064(13) C22 0.039(3) 0.030(2) 0.034(2) 0.0087(19) -0.011(2) 0.0022(19) C23 0.047(3) 0.026(2) 0.031(2) 0.0030(18) -0.005(2) -0.003(2) C24 0.035(2) 0.023(2) 0.034(2) 0.0028(18) -0.0014(19) -0.0026(18) O8 0.0391(16) 0.0234(14) 0.0334(16) 0.0029(12) -0.0057(13) -0.0020(12) O7 0.0429(17) 0.0226(15) 0.0414(17) 0.0027(12) -0.0086(13) -0.0028(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni3 O10 2.055(2) 6_464 ? Ni3 O10 2.055(2) . ? Ni3 N4 2.067(3) . ? Ni3 N4 2.067(3) 6_464 ? Ni3 O9 2.154(3) 6_464 ? Ni3 O9 2.154(3) . ? Ni3 C25 2.449(4) 6_464 ? Ni3 C25 2.449(4) . ? Ni2 O6 2.037(2) . ? Ni2 N5 2.042(3) . ? Ni2 N2 2.066(3) . ? Ni2 O8 2.083(2) 14_545 ? Ni2 O7 2.135(2) 14_545 ? Ni2 O5 2.188(2) . ? Ni2 C13 2.443(4) . ? Ni2 C24 2.446(4) 14_545 ? Ni1 N3 2.040(3) . ? Ni1 N1 2.042(3) . ? Ni1 O3 2.068(2) 14_545 ? Ni1 O2 2.070(2) . ? Ni1 O4 2.139(3) 14_545 ? Ni1 O1 2.152(2) . ? Ni1 C12 2.430(4) 14_545 ? Ni1 C1 2.438(4) . ? O10 C25 1.294(4) . ? O6 C13 1.273(4) . ? O5 C13 1.267(4) . ? O2 C1 1.271(4) . ? O1 C1 1.264(4) . ? O9 C25 1.262(4) . ? N2 C41 1.329(5) . ? N2 C42 1.334(4) . ? C1 C2 1.477(5) . ? N3 C46 1.312(5) . ? N3 C47 1.337(5) . ? N5 C60 1.326(4) . ? N5 C59 1.331(5) . ? N1 C34 1.325(5) . ? N1 C33 1.328(5) . ? N4 C55 1.330(5) . ? N4 C54 1.341(5) . ? C2 C3 1.317(5) . ? C2 H2A 0.924(10) . ? C28 C29 1.381(5) . ? C28 C30 1.394(5) . ? C28 C27 1.460(5) . ? C9 C8 1.384(5) . ? C9 C4 1.395(5) . ? C9 H9A 0.9300 . ? C20 C21 1.382(5) . ? C20 C19 1.396(5) . ? C20 H20A 0.9300 . ? C13 C14 1.472(5) . ? C27 C26 1.319(5) . ? C27 H27A 0.925(10) . ? C26 C25 1.465(5) . ? C26 H26A 0.925(10) . ? C16 C21 1.387(5) . ? C16 C17 1.390(5) . ? C16 C15 1.470(5) . ? C4 C5 1.377(5) . ? C4 C3 1.465(5) . ? C21 H21A 0.9300 . ? C14 C15 1.317(5) . ? C14 H14A 0.930(10) . ? C3 H3A 0.930(10) . ? C15 H15A 0.929(10) . ? C18 C17 1.381(5) . ? C18 C19 1.386(5) . ? C18 H18A 0.9300 . ? C31 C35 1.377(5) . ? C31 C32 1.382(5) . ? C31 C36 1.503(5) . ? C5 C6 1.375(5) . ? C5 H5A 0.9300 . ? C33 C32 1.363(5) . ? C33 H33A 0.9300 . ? C60 C61 1.363(5) . ? C60 H60A 0.9300 . ? C34 C35 1.389(5) . ? C34 H34A 0.9300 . ? C29 C30 1.384(5) 9_575 ? C29 H29A 0.9300 . ? C54 C53 1.364(5) . ? C54 H54A 0.9300 . ? C19 C22 1.463(5) . ? C30 C29 1.384(5) 9_575 ? C30 H30A 0.9300 . ? C48 C44 1.364(6) . ? C48 C47 1.370(5) . ? C48 H48A 0.9300 . ? C8 C7 1.387(5) . ? C8 H8A 0.9300 . ? C58 C59 1.360(6) . ? C58 C57 1.403(6) . ? C58 H58A 0.9300 . ? C35 H35A 0.9300 . ? C36 C37 1.523(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C57 C61 1.360(6) . ? C57 C62 1.500(5) . ? C37 C38 1.511(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C17 H17A 0.9300 . ? C56 C52 1.376(6) . ? C56 C55 1.384(6) . ? C56 H56A 0.9300 . ? C53 C52 1.387(5) . ? C53 H53A 0.9300 . ? C59 H59A 0.9300 . ? C55 H55A 0.9300 . ? C47 H47A 0.9300 . ? C42 C43 1.372(5) . ? C42 H42A 0.9300 . ? C43 C39 1.383(5) . ? C43 H43A 0.9300 . ? C44 C45 1.381(6) . ? C44 C49 1.521(5) . ? C32 H32A 0.9300 . ? C41 C40 1.372(5) . ? C41 H41A 0.9300 . ? C52 C51 1.506(6) . ? C39 C40 1.364(5) . ? C39 C38 1.505(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C61 H61A 0.9300 . ? C46 C45 1.389(6) . ? C46 H46A 0.9300 . ? C51 C50 1.523(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C40 H40A 0.9300 . ? C50 C49 1.487(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C62 C63 1.5374 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C62 1.539(5) 6_654 ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C45 H45A 0.9300 . ? O4W H7 0.843(10) . ? O4W H8 0.844(10) . ? O5W H10 0.835(10) . ? O5W H9 0.838(10) . ? O6W H11 0.838(10) . ? O6W H12 0.840(10) . ? O1W H1 0.840(10) . ? O1W H2 0.843(10) . ? O2W H3 0.839(10) . ? O2W H4 0.842(10) . ? O3W H5 0.846(10) . ? O3W H6 0.845(10) . ? C7 C6 1.403(5) . ? C7 C10 1.460(5) . ? C10 C11 1.307(5) . ? C10 H10A 0.928(10) . ? C6 H6A 0.9300 . ? C11 C12 1.475(5) . ? C11 H11A 0.923(10) . ? C12 O4 1.260(4) . ? C12 O3 1.276(4) . ? C12 Ni1 2.430(4) 14 ? O3 Ni1 2.068(2) 14 ? O4 Ni1 2.139(3) 14 ? C22 C23 1.317(5) . ? C22 H22A 0.929(10) . ? C23 C24 1.459(5) . ? C23 H23A 0.929(10) . ? C24 O7 1.269(4) . ? C24 O8 1.275(4) . ? C24 Ni2 2.446(4) 14 ? O8 Ni2 2.083(2) 14 ? O7 Ni2 2.135(2) 14 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Ni3 O10 155.99(14) 6_464 . ? O10 Ni3 N4 96.46(11) 6_464 . ? O10 Ni3 N4 99.72(11) . . ? O10 Ni3 N4 99.72(11) 6_464 6_464 ? O10 Ni3 N4 96.46(11) . 6_464 ? N4 Ni3 N4 94.86(18) . 6_464 ? O10 Ni3 O9 62.86(9) 6_464 6_464 ? O10 Ni3 O9 99.65(10) . 6_464 ? N4 Ni3 O9 89.15(11) . 6_464 ? N4 Ni3 O9 162.50(11) 6_464 6_464 ? O10 Ni3 O9 99.65(10) 6_464 . ? O10 Ni3 O9 62.86(10) . . ? N4 Ni3 O9 162.50(11) . . ? N4 Ni3 O9 89.15(11) 6_464 . ? O9 Ni3 O9 92.11(14) 6_464 . ? O10 Ni3 C25 31.87(10) 6_464 6_464 ? O10 Ni3 C25 128.87(12) . 6_464 ? N4 Ni3 C25 93.31(12) . 6_464 ? N4 Ni3 C25 131.57(13) 6_464 6_464 ? O9 Ni3 C25 30.99(10) 6_464 6_464 ? O9 Ni3 C25 96.74(11) . 6_464 ? O10 Ni3 C25 128.87(12) 6_464 . ? O10 Ni3 C25 31.87(10) . . ? N4 Ni3 C25 131.57(13) . . ? N4 Ni3 C25 93.31(12) 6_464 . ? O9 Ni3 C25 96.74(11) 6_464 . ? O9 Ni3 C25 30.99(10) . . ? C25 Ni3 C25 115.57(18) 6_464 . ? O6 Ni2 N5 98.60(11) . . ? O6 Ni2 N2 90.16(11) . . ? N5 Ni2 N2 96.22(12) . . ? O6 Ni2 O8 156.77(10) . 14_545 ? N5 Ni2 O8 96.43(11) . 14_545 ? N2 Ni2 O8 105.74(11) . 14_545 ? O6 Ni2 O7 99.55(10) . 14_545 ? N5 Ni2 O7 90.41(11) . 14_545 ? N2 Ni2 O7 167.32(11) . 14_545 ? O8 Ni2 O7 62.64(9) 14_545 14_545 ? O6 Ni2 O5 62.53(9) . . ? N5 Ni2 O5 160.82(11) . . ? N2 Ni2 O5 87.69(10) . . ? O8 Ni2 O5 100.57(9) 14_545 . ? O7 Ni2 O5 89.57(9) 14_545 . ? O6 Ni2 C13 31.39(10) . . ? N5 Ni2 C13 129.96(12) . . ? N2 Ni2 C13 88.08(11) . . ? O8 Ni2 C13 130.28(11) 14_545 . ? O7 Ni2 C13 95.95(11) 14_545 . ? O5 Ni2 C13 31.15(10) . . ? O6 Ni2 C24 129.16(12) . 14_545 ? N5 Ni2 C24 94.49(12) . 14_545 ? N2 Ni2 C24 136.88(12) . 14_545 ? O8 Ni2 C24 31.41(10) 14_545 14_545 ? O7 Ni2 C24 31.24(10) 14_545 14_545 ? O5 Ni2 C24 95.40(11) . 14_545 ? C13 Ni2 C24 115.58(12) . 14_545 ? N3 Ni1 N1 98.05(13) . . ? N3 Ni1 O3 98.30(12) . 14_545 ? N1 Ni1 O3 94.65(11) . 14_545 ? N3 Ni1 O2 95.27(11) . . ? N1 Ni1 O2 98.85(11) . . ? O3 Ni1 O2 159.30(10) 14_545 . ? N3 Ni1 O4 160.34(12) . 14_545 ? N1 Ni1 O4 89.53(11) . 14_545 ? O3 Ni1 O4 62.86(10) 14_545 14_545 ? O2 Ni1 O4 101.48(10) . 14_545 ? N3 Ni1 O1 89.70(11) . . ? N1 Ni1 O1 160.62(11) . . ? O3 Ni1 O1 101.82(10) 14_545 . ? O2 Ni1 O1 62.59(9) . . ? O4 Ni1 O1 88.96(10) 14_545 . ? N3 Ni1 C12 129.70(14) . 14_545 ? N1 Ni1 C12 92.83(12) . 14_545 ? O3 Ni1 C12 31.67(11) 14_545 14_545 ? O2 Ni1 C12 131.31(12) . 14_545 ? O4 Ni1 C12 31.20(11) 14_545 14_545 ? O1 Ni1 C12 95.83(11) . 14_545 ? N3 Ni1 C1 93.38(12) . . ? N1 Ni1 C1 129.99(13) . . ? O3 Ni1 C1 131.59(11) 14_545 . ? O2 Ni1 C1 31.41(10) . . ? O4 Ni1 C1 95.58(11) 14_545 . ? O1 Ni1 C1 31.19(10) . . ? C12 Ni1 C1 116.01(13) 14_545 . ? C25 O10 Ni3 91.1(2) . . ? C13 O6 Ni2 92.2(2) . . ? C13 O5 Ni2 85.6(2) . . ? C1 O2 Ni1 90.5(2) . . ? C1 O1 Ni1 87.0(2) . . ? C25 O9 Ni3 87.5(2) . . ? C41 N2 C42 116.3(3) . . ? C41 N2 Ni2 120.1(3) . . ? C42 N2 Ni2 121.6(3) . . ? O1 C1 O2 119.9(3) . . ? O1 C1 C2 119.6(3) . . ? O2 C1 C2 120.5(3) . . ? O1 C1 Ni1 61.80(19) . . ? O2 C1 Ni1 58.10(18) . . ? C2 C1 Ni1 177.8(3) . . ? C46 N3 C47 115.5(4) . . ? C46 N3 Ni1 123.9(3) . . ? C47 N3 Ni1 119.8(3) . . ? C60 N5 C59 115.5(3) . . ? C60 N5 Ni2 122.4(3) . . ? C59 N5 Ni2 122.0(3) . . ? C34 N1 C33 116.9(4) . . ? C34 N1 Ni1 123.0(3) . . ? C33 N1 Ni1 119.2(3) . . ? C55 N4 C54 117.4(4) . . ? C55 N4 Ni3 123.1(3) . . ? C54 N4 Ni3 119.6(3) . . ? C3 C2 C1 122.5(4) . . ? C3 C2 H2A 125(2) . . ? C1 C2 H2A 113(2) . . ? C29 C28 C30 118.2(4) . . ? C29 C28 C27 119.7(4) . . ? C30 C28 C27 122.1(4) . . ? C8 C9 C4 120.5(4) . . ? C8 C9 H9A 119.7 . . ? C4 C9 H9A 119.7 . . ? C21 C20 C19 120.9(4) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? O5 C13 O6 119.6(3) . . ? O5 C13 C14 121.1(3) . . ? O6 C13 C14 119.3(3) . . ? O5 C13 Ni2 63.24(19) . . ? O6 C13 Ni2 56.42(17) . . ? C14 C13 Ni2 175.6(3) . . ? C26 C27 C28 127.4(4) . . ? C26 C27 H27A 117(2) . . ? C28 C27 H27A 115(2) . . ? C27 C26 C25 122.9(4) . . ? C27 C26 H26A 121(2) . . ? C25 C26 H26A 116(2) . . ? C21 C16 C17 118.7(3) . . ? C21 C16 C15 123.2(3) . . ? C17 C16 C15 118.0(3) . . ? C5 C4 C9 118.0(4) . . ? C5 C4 C3 119.2(4) . . ? C9 C4 C3 122.7(3) . . ? C20 C21 C16 120.3(3) . . ? C20 C21 H21A 119.9 . . ? C16 C21 H21A 119.9 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14A 122.8(19) . . ? C13 C14 H14A 116.9(19) . . ? C2 C3 C4 127.8(4) . . ? C2 C3 H3A 116(2) . . ? C4 C3 H3A 116(2) . . ? C14 C15 C16 129.1(4) . . ? C14 C15 H15A 115(2) . . ? C16 C15 H15A 116(2) . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? O9 C25 O10 118.5(3) . . ? O9 C25 C26 120.8(4) . . ? O10 C25 C26 120.6(3) . . ? O9 C25 Ni3 61.49(19) . . ? O10 C25 Ni3 57.03(18) . . ? C26 C25 Ni3 177.6(3) . . ? C35 C31 C32 116.5(4) . . ? C35 C31 C36 121.6(4) . . ? C32 C31 C36 121.8(4) . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? N1 C33 C32 123.7(4) . . ? N1 C33 H33A 118.1 . . ? C32 C33 H33A 118.1 . . ? N5 C60 C61 124.1(4) . . ? N5 C60 H60A 117.9 . . ? C61 C60 H60A 117.9 . . ? N1 C34 C35 122.9(4) . . ? N1 C34 H34A 118.5 . . ? C35 C34 H34A 118.5 . . ? C28 C29 C30 121.8(4) . 9_575 ? C28 C29 H29A 119.1 . . ? C30 C29 H29A 119.1 9_575 . ? N4 C54 C53 122.6(4) . . ? N4 C54 H54A 118.7 . . ? C53 C54 H54A 118.7 . . ? C18 C19 C20 118.7(3) . . ? C18 C19 C22 121.7(4) . . ? C20 C19 C22 119.6(3) . . ? C29 C30 C28 120.0(4) 9_575 . ? C29 C30 H30A 120.0 9_575 . ? C28 C30 H30A 120.0 . . ? C44 C48 C47 120.5(4) . . ? C44 C48 H48A 119.8 . . ? C47 C48 H48A 119.8 . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C59 C58 C57 119.3(4) . . ? C59 C58 H58A 120.3 . . ? C57 C58 H58A 120.3 . . ? C31 C35 C34 119.8(4) . . ? C31 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C31 C36 C37 111.7(3) . . ? C31 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C31 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C61 C57 C58 116.0(4) . . ? C61 C57 C62 121.4(4) . . ? C58 C57 C62 122.5(4) . . ? C38 C37 C36 112.1(3) . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C52 C56 C55 121.0(4) . . ? C52 C56 H56A 119.5 . . ? C55 C56 H56A 119.5 . . ? C54 C53 C52 121.2(4) . . ? C54 C53 H53A 119.4 . . ? C52 C53 H53A 119.4 . . ? N5 C59 C58 124.3(4) . . ? N5 C59 H59A 117.8 . . ? C58 C59 H59A 117.8 . . ? N4 C55 C56 122.4(4) . . ? N4 C55 H55A 118.8 . . ? C56 C55 H55A 118.8 . . ? N3 C47 C48 124.4(4) . . ? N3 C47 H47A 117.8 . . ? C48 C47 H47A 117.8 . . ? N2 C42 C43 123.2(4) . . ? N2 C42 H42A 118.4 . . ? C43 C42 H42A 118.4 . . ? C42 C43 C39 120.3(4) . . ? C42 C43 H43A 119.9 . . ? C39 C43 H43A 119.9 . . ? C48 C44 C45 115.3(4) . . ? C48 C44 C49 122.2(4) . . ? C45 C44 C49 122.3(4) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? N2 C41 C40 123.5(4) . . ? N2 C41 H41A 118.2 . . ? C40 C41 H41A 118.2 . . ? C56 C52 C53 115.5(4) . . ? C56 C52 C51 122.4(4) . . ? C53 C52 C51 122.0(4) . . ? C40 C39 C43 116.3(4) . . ? C40 C39 C38 120.5(4) . . ? C43 C39 C38 123.2(4) . . ? C39 C38 C37 116.5(3) . . ? C39 C38 H38A 108.2 . . ? C37 C38 H38A 108.2 . . ? C39 C38 H38B 108.2 . . ? C37 C38 H38B 108.2 . . ? H38A C38 H38B 107.3 . . ? C60 C61 C57 120.6(4) . . ? C60 C61 H61A 119.7 . . ? C57 C61 H61A 119.7 . . ? N3 C46 C45 123.4(5) . . ? N3 C46 H46A 118.3 . . ? C45 C46 H46A 118.3 . . ? C52 C51 C50 115.1(4) . . ? C52 C51 H51A 108.5 . . ? C50 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? C50 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C39 C40 C41 120.5(4) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C49 C50 C51 112.5(4) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C57 C62 C63 108.8(2) . . ? C57 C62 H62A 109.9 . . ? C63 C62 H62A 109.9 . . ? C57 C62 H62B 109.9 . . ? C63 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C62 C63 C62 111.61(13) 6_654 . ? C62 C63 H63A 109.3 6_654 . ? C62 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 6_654 . ? C62 C63 H63B 109.3 . . ? H63A C63 H63B 108.0 . . ? C50 C49 C44 114.7(3) . . ? C50 C49 H49A 108.6 . . ? C44 C49 H49A 108.6 . . ? C50 C49 H49B 108.6 . . ? C44 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C44 C45 C46 120.8(4) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? H7 O4W H8 108.8(18) . . ? H10 O5W H9 109.7(17) . . ? H11 O6W H12 109.6(17) . . ? H1 O1W H2 108.6(17) . . ? H3 O2W H4 108.9(18) . . ? H5 O3W H6 107.7(17) . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C10 119.8(4) . . ? C6 C7 C10 122.1(4) . . ? C11 C10 C7 127.4(4) . . ? C11 C10 H10A 116(2) . . ? C7 C10 H10A 116(2) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C10 C11 C12 125.5(4) . . ? C10 C11 H11A 118(2) . . ? C12 C11 H11A 116(2) . . ? O4 C12 O3 119.9(3) . . ? O4 C12 C11 119.8(4) . . ? O3 C12 C11 120.3(4) . . ? O4 C12 Ni1 61.55(19) . 14 ? O3 C12 Ni1 58.33(18) . 14 ? C11 C12 Ni1 177.6(3) . 14 ? C12 O3 Ni1 90.0(2) . 14 ? C12 O4 Ni1 87.2(2) . 14 ? C23 C22 C19 128.5(4) . . ? C23 C22 H22A 116(2) . . ? C19 C22 H22A 115(2) . . ? C22 C23 C24 123.5(4) . . ? C22 C23 H23A 123(2) . . ? C24 C23 H23A 114(2) . . ? O7 C24 O8 119.1(3) . . ? O7 C24 C23 119.5(3) . . ? O8 C24 C23 121.4(3) . . ? O7 C24 Ni2 60.74(18) . 14 ? O8 C24 Ni2 58.40(18) . 14 ? C23 C24 Ni2 177.5(3) . 14 ? C24 O8 Ni2 90.2(2) . 14 ? C24 O7 Ni2 88.0(2) . 14 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.520 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.064