# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Yaqiu Sun' _publ_contact_author_email hxxysyq@mail.tjnu.edu.cn _publ_author_name 'Yaqiu Sun' #===End data_091022c _database_code_depnum_ccdc_archive 'CCDC 800812' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 N4 Ni O11 Zn2' _chemical_formula_weight 781.96 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' 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 10.1145(5) _cell_length_b 12.3815(6) _cell_length_c 13.7981(6) _cell_angle_alpha 100.4750(10) _cell_angle_beta 107.9830(10) _cell_angle_gamma 109.2310(10) _cell_volume 1472.49(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3302 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.09 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4892 _exptl_absorpt_correction_T_max 0.6296 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _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_% ? _diffrn_reflns_number 7648 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5166 _reflns_number_gt 4155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0392P)^2^+1.0504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5166 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33230(5) 0.76344(4) 0.54465(3) 0.03446(12) Uani 1 1 d . . . Zn1 Zn 0.08150(4) 0.54954(3) 0.12315(3) 0.02634(10) Uani 1 1 d . . . Zn2 Zn 0.21615(4) 0.74730(3) 0.00559(3) 0.02781(11) Uani 1 1 d . . . O1 O 0.2927(3) 0.6841(2) 0.24516(17) 0.0364(6) Uani 1 1 d . . . O2 O 0.0343(3) 0.5509(2) 0.26031(17) 0.0367(6) Uani 1 1 d . . . O3 O 0.4352(2) 0.8341(2) 0.0600(2) 0.0380(6) Uani 1 1 d . . . O4 O 0.4550(3) 0.6611(2) 0.0143(2) 0.0479(7) Uani 1 1 d . . . O5 O 0.9803(3) 0.6758(2) 0.1166(2) 0.0357(6) Uani 1 1 d . . . O6 O 1.1485(2) 0.83388(19) 0.09968(18) 0.0318(5) Uani 1 1 d . . . O7 O 1.0930(3) 1.2179(2) 0.1647(3) 0.0562(8) Uani 1 1 d . . . O8 O 0.8604(3) 1.2140(2) 0.12596(19) 0.0369(6) Uani 1 1 d . . . O9 O 0.1302(2) 0.57729(17) -0.00923(16) 0.0222(4) Uani 1 1 d . . . H9A H 0.1982 0.5541 -0.0160 0.033 Uiso 1 1 d R . . O10 O 0.1836(3) 0.4314(2) 0.1405(2) 0.0482(7) Uani 1 1 d . . . H10' H 0.1398 0.3647 0.1495 0.072 Uiso 1 1 d R . . H10" H 0.2758 0.4493 0.1484 0.072 Uiso 1 1 d R . . O11 O 0.4667(4) 0.4916(3) 0.1251(3) 0.0731(9) Uani 1 1 d . . . H11' H 0.4238 0.4233 0.0724 0.110 Uiso 1 1 d R . . H11" H 0.4374 0.5463 0.1062 0.110 Uiso 1 1 d R . . N1 N 0.3982(3) 0.7798(2) 0.4304(2) 0.0328(6) Uani 1 1 d . . . N2 N 0.1368(3) 0.6693(3) 0.4378(2) 0.0358(7) Uani 1 1 d . . . N3 N 0.2718(4) 0.7051(3) 0.6483(2) 0.0433(8) Uani 1 1 d . . . N4 N 0.5101(3) 0.8875(3) 0.6520(2) 0.0392(7) Uani 1 1 d . . . C1 C 0.2897(4) 0.7024(3) 0.3358(3) 0.0316(7) Uani 1 1 d . . . C2 C 0.1395(4) 0.6314(3) 0.3427(3) 0.0314(7) Uani 1 1 d . . . C3 C -0.0002(4) 0.6457(3) 0.4529(3) 0.0379(8) Uani 1 1 d . . . C4 C -0.1343(5) 0.6303(4) 0.3727(3) 0.0501(10) Uani 1 1 d . . . H4 H -0.1375 0.6286 0.3043 0.060 Uiso 1 1 calc R . . C5 C -0.2631(5) 0.6174(4) 0.3934(4) 0.0630(12) Uani 1 1 d . . . H5 H -0.3514 0.6089 0.3392 0.076 Uiso 1 1 calc R . . C6 C -0.2618(6) 0.6169(5) 0.4935(4) 0.0750(15) Uani 1 1 d . . . H6 H -0.3491 0.6080 0.5066 0.090 Uiso 1 1 calc R . . C7 C -0.1319(5) 0.6298(4) 0.5738(4) 0.0620(12) Uani 1 1 d . . . H7 H -0.1322 0.6274 0.6407 0.074 Uiso 1 1 calc R . . C8 C 0.0014(5) 0.6465(3) 0.5557(3) 0.0459(9) Uani 1 1 d . . . C9 C 0.1356(5) 0.6599(3) 0.6427(3) 0.0478(10) Uani 1 1 d . . . H9 H 0.1216 0.6334 0.6992 0.057 Uiso 1 1 calc R . . C10 C 0.3950(5) 0.7023(4) 0.7375(3) 0.0604(12) Uani 1 1 d . . . H10A H 0.4501 0.6636 0.7087 0.072 Uiso 1 1 calc R . . H10B H 0.3511 0.6548 0.7773 0.072 Uiso 1 1 calc R . . C11 C 0.5050(5) 0.8279(4) 0.8126(3) 0.0647(13) Uani 1 1 d . . . H11A H 0.4779 0.8451 0.8735 0.078 Uiso 1 1 calc R . . H11B H 0.6072 0.8309 0.8397 0.078 Uiso 1 1 calc R . . C12 C 0.5046(5) 0.9234(4) 0.7588(3) 0.0540(11) Uani 1 1 d . . . H12A H 0.4132 0.9370 0.7503 0.065 Uiso 1 1 calc R . . H12B H 0.5921 0.9984 0.8038 0.065 Uiso 1 1 calc R . . C13 C 0.6227(4) 0.9555(3) 0.6375(3) 0.0424(9) Uani 1 1 d . . . H13 H 0.6964 1.0212 0.6964 0.051 Uiso 1 1 calc R . . C14 C 0.6490(4) 0.9422(3) 0.5400(3) 0.0369(8) Uani 1 1 d . . . C15 C 0.7910(4) 1.0233(4) 0.5481(3) 0.0480(10) Uani 1 1 d . . . H15 H 0.8590 1.0808 0.6141 0.058 Uiso 1 1 calc R . . C16 C 0.8319(4) 1.0204(4) 0.4637(3) 0.0512(10) Uani 1 1 d . . . H16 H 0.9256 1.0755 0.4708 0.061 Uiso 1 1 calc R . . C17 C 0.7312(5) 0.9336(4) 0.3667(3) 0.0565(11) Uani 1 1 d . . . H17 H 0.7590 0.9289 0.3084 0.068 Uiso 1 1 calc R . . C18 C 0.5907(4) 0.8539(4) 0.3542(3) 0.0502(10) Uani 1 1 d . . . H18 H 0.5253 0.7971 0.2872 0.060 Uiso 1 1 calc R . . C19 C 0.5435(4) 0.8559(3) 0.4390(3) 0.0332(8) Uani 1 1 d . . . C20 C 0.6792(3) 0.8436(3) 0.0839(2) 0.0254(7) Uani 1 1 d . . . C21 C 0.7753(3) 0.7845(3) 0.0921(2) 0.0251(7) Uani 1 1 d . . . H21 H 0.7373 0.7024 0.0835 0.030 Uiso 1 1 calc R . . C22 C 0.9283(3) 0.8477(3) 0.1133(2) 0.0239(6) Uani 1 1 d . . . C23 C 0.9856(3) 0.9707(3) 0.1291(2) 0.0258(7) Uani 1 1 d . . . H23 H 1.0877 1.0129 0.1425 0.031 Uiso 1 1 calc R . . C24 C 0.8908(3) 1.0313(3) 0.1248(2) 0.0254(7) Uani 1 1 d . . . C25 C 0.7381(3) 0.9673(3) 0.1008(2) 0.0268(7) Uani 1 1 d . . . H25 H 0.6740 1.0073 0.0960 0.032 Uiso 1 1 calc R . . C26 C 0.5115(4) 0.7727(3) 0.0509(3) 0.0296(7) Uani 1 1 d . . . C27 C 1.0254(3) 0.7793(3) 0.1103(2) 0.0252(7) Uani 1 1 d . . . C28 C 0.9549(4) 1.1644(3) 0.1399(3) 0.0324(8) 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 Ni1 0.0380(3) 0.0308(3) 0.0211(2) 0.00435(18) 0.00706(19) 0.0047(2) Zn1 0.0274(2) 0.0222(2) 0.02314(19) 0.00522(15) 0.00740(16) 0.00629(16) Zn2 0.02203(19) 0.0208(2) 0.0413(2) 0.00947(16) 0.01514(17) 0.00752(15) O1 0.0335(13) 0.0362(14) 0.0251(12) 0.0037(10) 0.0087(10) 0.0033(11) O2 0.0364(13) 0.0324(13) 0.0243(12) 0.0025(10) 0.0093(11) 0.0000(11) O3 0.0184(11) 0.0337(13) 0.0614(16) 0.0109(12) 0.0185(11) 0.0100(10) O4 0.0254(13) 0.0321(15) 0.079(2) 0.0110(13) 0.0199(13) 0.0080(11) O5 0.0321(13) 0.0238(13) 0.0583(16) 0.0139(11) 0.0230(12) 0.0144(11) O6 0.0240(12) 0.0250(12) 0.0468(14) 0.0062(10) 0.0187(11) 0.0090(10) O7 0.0372(15) 0.0270(14) 0.107(2) 0.0282(15) 0.0292(16) 0.0117(12) O8 0.0484(15) 0.0350(14) 0.0456(14) 0.0202(11) 0.0258(12) 0.0282(12) O9 0.0188(10) 0.0190(11) 0.0290(11) 0.0064(9) 0.0098(9) 0.0084(9) O10 0.0379(14) 0.0378(15) 0.082(2) 0.0347(14) 0.0270(14) 0.0198(12) O11 0.078(2) 0.066(2) 0.082(2) 0.0227(18) 0.0364(19) 0.0323(19) N1 0.0344(16) 0.0294(15) 0.0226(14) 0.0040(12) 0.0063(12) 0.0060(13) N2 0.0373(17) 0.0323(16) 0.0241(14) 0.0040(12) 0.0100(13) 0.0027(13) N3 0.057(2) 0.0361(18) 0.0263(15) 0.0093(13) 0.0135(15) 0.0097(16) N4 0.0434(18) 0.0362(17) 0.0234(15) 0.0030(13) 0.0077(13) 0.0078(15) C1 0.0357(19) 0.0253(18) 0.0262(17) 0.0070(14) 0.0081(15) 0.0080(15) C2 0.0358(19) 0.0262(18) 0.0252(17) 0.0079(15) 0.0089(15) 0.0078(15) C3 0.040(2) 0.0269(19) 0.0341(19) 0.0012(15) 0.0141(17) 0.0039(16) C4 0.049(2) 0.047(2) 0.046(2) 0.0071(19) 0.018(2) 0.014(2) C5 0.048(3) 0.066(3) 0.068(3) 0.010(2) 0.021(2) 0.022(2) C6 0.062(3) 0.082(4) 0.080(4) 0.010(3) 0.044(3) 0.021(3) C7 0.068(3) 0.058(3) 0.056(3) 0.007(2) 0.039(3) 0.012(2) C8 0.052(2) 0.035(2) 0.039(2) 0.0017(17) 0.0204(19) 0.0067(18) C9 0.066(3) 0.037(2) 0.0289(19) 0.0069(16) 0.024(2) 0.005(2) C10 0.074(3) 0.059(3) 0.037(2) 0.021(2) 0.010(2) 0.022(2) C11 0.065(3) 0.078(3) 0.030(2) 0.015(2) 0.008(2) 0.014(3) C12 0.054(3) 0.048(3) 0.029(2) -0.0048(18) 0.0100(18) 0.000(2) C13 0.037(2) 0.037(2) 0.0293(19) -0.0004(16) 0.0022(16) 0.0024(17) C14 0.0330(19) 0.033(2) 0.0315(18) 0.0043(15) 0.0052(15) 0.0076(16) C15 0.035(2) 0.043(2) 0.041(2) 0.0038(18) 0.0041(18) 0.0016(18) C16 0.035(2) 0.049(3) 0.055(3) 0.014(2) 0.012(2) 0.0060(19) C17 0.044(2) 0.069(3) 0.044(2) 0.015(2) 0.020(2) 0.007(2) C18 0.040(2) 0.054(3) 0.033(2) 0.0050(18) 0.0093(17) 0.0016(19) C19 0.0309(18) 0.0311(19) 0.0274(17) 0.0071(15) 0.0058(15) 0.0071(15) C20 0.0212(16) 0.0280(17) 0.0278(16) 0.0097(14) 0.0105(13) 0.0099(14) C21 0.0233(16) 0.0207(16) 0.0319(17) 0.0087(13) 0.0130(14) 0.0076(13) C22 0.0234(16) 0.0215(16) 0.0262(16) 0.0048(13) 0.0092(13) 0.0104(13) C23 0.0200(15) 0.0250(17) 0.0305(17) 0.0081(14) 0.0096(13) 0.0077(13) C24 0.0253(16) 0.0238(17) 0.0272(16) 0.0078(13) 0.0105(13) 0.0104(14) C25 0.0264(17) 0.0312(18) 0.0296(17) 0.0108(14) 0.0131(14) 0.0173(15) C26 0.0233(17) 0.033(2) 0.0348(18) 0.0128(15) 0.0140(15) 0.0117(15) C27 0.0197(16) 0.0238(17) 0.0262(16) 0.0021(13) 0.0065(13) 0.0077(13) C28 0.036(2) 0.0263(18) 0.0391(19) 0.0145(15) 0.0185(16) 0.0128(16) _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 N4 1.869(3) . ? Ni1 N2 1.871(3) . ? Ni1 N3 1.888(3) . ? Ni1 N1 1.910(3) . ? Zn1 O10 2.058(2) . ? Zn1 O9 2.0811(19) 2_565 ? Zn1 O2 2.088(2) . ? Zn1 O9 2.090(2) . ? Zn1 O5 2.133(2) 1_455 ? Zn1 O1 2.142(2) . ? Zn1 Zn1 3.0764(7) 2_565 ? Zn2 O3 1.933(2) . ? Zn2 O9 1.9382(19) . ? Zn2 O8 1.954(2) 2_675 ? Zn2 O6 1.957(2) 1_455 ? O1 C1 1.241(4) . ? O2 C2 1.249(4) . ? O3 C26 1.266(4) . ? O4 C26 1.240(4) . ? O5 C27 1.239(4) . ? O5 Zn1 2.133(2) 1_655 ? O6 C27 1.274(4) . ? O6 Zn2 1.957(2) 1_655 ? O7 C28 1.233(4) . ? O8 C28 1.282(4) . ? O8 Zn2 1.954(2) 2_675 ? O9 Zn1 2.0811(19) 2_565 ? O9 H9A 0.8502 . ? O10 H10' 0.8501 . ? O10 H10" 0.8504 . ? O11 H11' 0.8789 . ? O11 H11" 0.8740 . ? N1 C1 1.340(4) . ? N1 C19 1.414(4) . ? N2 C2 1.323(4) . ? N2 C3 1.408(4) . ? N3 C9 1.276(5) . ? N3 C10 1.472(5) . ? N4 C13 1.272(5) . ? N4 C12 1.484(4) . ? C1 C2 1.526(5) . ? C3 C4 1.387(5) . ? C3 C8 1.412(5) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C6 1.378(7) . ? C5 H5 0.9300 . ? C6 C7 1.371(7) . ? C6 H6 0.9300 . ? C7 C8 1.401(6) . ? C7 H7 0.9300 . ? C8 C9 1.444(6) . ? C9 H9 0.9300 . ? C10 C11 1.515(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.507(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.440(5) . ? C13 H13 0.9300 . ? C14 C15 1.412(5) . ? C14 C19 1.419(5) . ? C15 C16 1.349(5) . ? C15 H15 0.9300 . ? C16 C17 1.378(6) . ? C16 H16 0.9300 . ? C17 C18 1.373(5) . ? C17 H17 0.9300 . ? C18 C19 1.394(5) . ? C18 H18 0.9300 . ? C20 C21 1.388(4) . ? C20 C25 1.392(4) . ? C20 C26 1.501(4) . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.387(4) . ? C22 C27 1.498(4) . ? C23 C24 1.393(4) . ? C23 H23 0.9300 . ? C24 C25 1.381(4) . ? C24 C28 1.506(4) . ? C25 H25 0.9300 . ? 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 N4 Ni1 N2 165.86(13) . . ? N4 Ni1 N3 91.21(13) . . ? N2 Ni1 N3 90.92(13) . . ? N4 Ni1 N1 95.22(12) . . ? N2 Ni1 N1 86.49(11) . . ? N3 Ni1 N1 163.72(13) . . ? O10 Zn1 O9 96.41(9) . 2_565 ? O10 Zn1 O2 94.85(10) . . ? O9 Zn1 O2 98.60(8) 2_565 . ? O10 Zn1 O9 93.56(9) . . ? O9 Zn1 O9 84.97(8) 2_565 . ? O2 Zn1 O9 170.43(9) . . ? O10 Zn1 O5 176.12(10) . 1_455 ? O9 Zn1 O5 85.91(8) 2_565 1_455 ? O2 Zn1 O5 81.71(9) . 1_455 ? O9 Zn1 O5 89.73(8) . 1_455 ? O10 Zn1 O1 85.89(10) . . ? O9 Zn1 O1 176.71(8) 2_565 . ? O2 Zn1 O1 78.84(9) . . ? O9 Zn1 O1 97.25(8) . . ? O5 Zn1 O1 91.66(9) 1_455 . ? O10 Zn1 Zn1 96.76(8) . 2_565 ? O9 Zn1 Zn1 42.60(5) 2_565 2_565 ? O2 Zn1 Zn1 140.46(6) . 2_565 ? O9 Zn1 Zn1 42.37(5) . 2_565 ? O5 Zn1 Zn1 87.05(7) 1_455 2_565 ? O1 Zn1 Zn1 139.57(6) . 2_565 ? O3 Zn2 O9 119.22(9) . . ? O3 Zn2 O8 104.22(10) . 2_675 ? O9 Zn2 O8 114.62(9) . 2_675 ? O3 Zn2 O6 106.25(10) . 1_455 ? O9 Zn2 O6 109.29(9) . 1_455 ? O8 Zn2 O6 101.52(9) 2_675 1_455 ? C1 O1 Zn1 112.5(2) . . ? C2 O2 Zn1 112.8(2) . . ? C26 O3 Zn2 117.1(2) . . ? C27 O5 Zn1 132.1(2) . 1_655 ? C27 O6 Zn2 120.5(2) . 1_655 ? C28 O8 Zn2 122.0(2) . 2_675 ? Zn2 O9 Zn1 125.41(10) . 2_565 ? Zn2 O9 Zn1 111.47(9) . . ? Zn1 O9 Zn1 95.03(8) 2_565 . ? Zn2 O9 H9A 103.7 . . ? Zn1 O9 H9A 108.4 2_565 . ? Zn1 O9 H9A 112.9 . . ? Zn1 O10 H10' 121.3 . . ? Zn1 O10 H10" 123.0 . . ? H10' O10 H10" 115.1 . . ? H11' O11 H11" 112.3 . . ? C1 N1 C19 121.5(3) . . ? C1 N1 Ni1 111.2(2) . . ? C19 N1 Ni1 127.2(2) . . ? C2 N2 C3 122.5(3) . . ? C2 N2 Ni1 112.3(2) . . ? C3 N2 Ni1 125.1(2) . . ? C9 N3 C10 118.6(3) . . ? C9 N3 Ni1 126.3(3) . . ? C10 N3 Ni1 114.8(3) . . ? C13 N4 C12 117.3(3) . . ? C13 N4 Ni1 125.8(2) . . ? C12 N4 Ni1 115.8(2) . . ? O1 C1 N1 129.6(3) . . ? O1 C1 C2 116.8(3) . . ? N1 C1 C2 113.5(3) . . ? O2 C2 N2 128.0(3) . . ? O2 C2 C1 118.6(3) . . ? N2 C2 C1 113.3(3) . . ? C4 C3 N2 122.5(3) . . ? C4 C3 C8 118.6(4) . . ? N2 C3 C8 118.8(3) . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 119.6(4) . . ? C7 C8 C9 118.5(4) . . ? C3 C8 C9 121.8(4) . . ? N3 C9 C8 125.2(3) . . ? N3 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? N3 C10 C11 111.6(4) . . ? N3 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 112.6(3) . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N4 C12 C11 111.3(4) . . ? N4 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? N4 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N4 C13 C14 127.3(3) . . ? N4 C13 H13 116.3 . . ? C14 C13 H13 116.3 . . ? C15 C14 C19 119.0(3) . . ? C15 C14 C13 116.1(3) . . ? C19 C14 C13 124.9(3) . . ? C16 C15 C14 122.5(4) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 118.2(4) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.7(4) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 N1 124.5(3) . . ? C18 C19 C14 116.9(3) . . ? N1 C19 C14 118.6(3) . . ? C21 C20 C25 119.6(3) . . ? C21 C20 C26 119.7(3) . . ? C25 C20 C26 120.6(3) . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 C27 121.2(3) . . ? C21 C22 C27 118.9(3) . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 C28 121.0(3) . . ? C23 C24 C28 119.2(3) . . ? C24 C25 C20 120.6(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? O4 C26 O3 124.0(3) . . ? O4 C26 C20 120.2(3) . . ? O3 C26 C20 115.8(3) . . ? O5 C27 O6 125.6(3) . . ? O5 C27 C22 118.7(3) . . ? O6 C27 C22 115.7(3) . . ? O7 C28 O8 124.7(3) . . ? O7 C28 C24 118.4(3) . . ? O8 C28 C24 116.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Zn1 O1 C1 -97.3(2) . . . . ? O9 Zn1 O1 C1 37.3(16) 2_565 . . . ? O2 Zn1 O1 C1 -1.5(2) . . . . ? O9 Zn1 O1 C1 169.6(2) . . . . ? O5 Zn1 O1 C1 79.7(2) 1_455 . . . ? Zn1 Zn1 O1 C1 167.08(18) 2_565 . . . ? O10 Zn1 O2 C2 90.3(2) . . . . ? O9 Zn1 O2 C2 -172.4(2) 2_565 . . . ? O9 Zn1 O2 C2 -61.2(6) . . . . ? O5 Zn1 O2 C2 -87.9(2) 1_455 . . . ? O1 Zn1 O2 C2 5.5(2) . . . . ? Zn1 Zn1 O2 C2 -162.93(19) 2_565 . . . ? O9 Zn2 O3 C26 22.7(3) . . . . ? O8 Zn2 O3 C26 -106.6(2) 2_675 . . . ? O6 Zn2 O3 C26 146.6(2) 1_455 . . . ? O3 Zn2 O9 Zn1 -149.94(12) . . . 2_565 ? O8 Zn2 O9 Zn1 -25.47(15) 2_675 . . 2_565 ? O6 Zn2 O9 Zn1 87.68(13) 1_455 . . 2_565 ? O3 Zn2 O9 Zn1 96.77(12) . . . . ? O8 Zn2 O9 Zn1 -138.76(10) 2_675 . . . ? O6 Zn2 O9 Zn1 -25.60(12) 1_455 . . . ? O10 Zn1 O9 Zn2 -132.59(11) . . . . ? O9 Zn1 O9 Zn2 131.27(13) 2_565 . . . ? O2 Zn1 O9 Zn2 18.9(5) . . . . ? O5 Zn1 O9 Zn2 45.35(10) 1_455 . . . ? O1 Zn1 O9 Zn2 -46.28(11) . . . . ? Zn1 Zn1 O9 Zn2 131.27(13) 2_565 . . . ? O10 Zn1 O9 Zn1 96.13(9) . . . 2_565 ? O9 Zn1 O9 Zn1 0.0 2_565 . . 2_565 ? O2 Zn1 O9 Zn1 -112.3(5) . . . 2_565 ? O5 Zn1 O9 Zn1 -85.92(8) 1_455 . . 2_565 ? O1 Zn1 O9 Zn1 -177.56(9) . . . 2_565 ? N4 Ni1 N1 C1 -178.0(2) . . . . ? N2 Ni1 N1 C1 -12.1(2) . . . . ? N3 Ni1 N1 C1 69.1(5) . . . . ? N4 Ni1 N1 C19 5.8(3) . . . . ? N2 Ni1 N1 C19 171.8(3) . . . . ? N3 Ni1 N1 C19 -107.0(5) . . . . ? N4 Ni1 N2 C2 114.3(5) . . . . ? N3 Ni1 N2 C2 -147.0(2) . . . . ? N1 Ni1 N2 C2 16.9(2) . . . . ? N4 Ni1 N2 C3 -62.0(6) . . . . ? N3 Ni1 N2 C3 36.6(3) . . . . ? N1 Ni1 N2 C3 -159.5(3) . . . . ? N4 Ni1 N3 C9 143.7(3) . . . . ? N2 Ni1 N3 C9 -22.3(3) . . . . ? N1 Ni1 N3 C9 -102.9(5) . . . . ? N4 Ni1 N3 C10 -42.7(3) . . . . ? N2 Ni1 N3 C10 151.3(3) . . . . ? N1 Ni1 N3 C10 70.7(5) . . . . ? N2 Ni1 N4 C13 -93.0(6) . . . . ? N3 Ni1 N4 C13 168.4(3) . . . . ? N1 Ni1 N4 C13 3.3(3) . . . . ? N2 Ni1 N4 C12 74.5(6) . . . . ? N3 Ni1 N4 C12 -24.1(3) . . . . ? N1 Ni1 N4 C12 170.9(3) . . . . ? Zn1 O1 C1 N1 -179.2(3) . . . . ? Zn1 O1 C1 C2 -2.0(4) . . . . ? C19 N1 C1 O1 -0.9(6) . . . . ? Ni1 N1 C1 O1 -177.3(3) . . . . ? C19 N1 C1 C2 -178.1(3) . . . . ? Ni1 N1 C1 C2 5.5(3) . . . . ? Zn1 O2 C2 N2 168.2(3) . . . . ? Zn1 O2 C2 C1 -8.3(4) . . . . ? C3 N2 C2 O2 -17.7(5) . . . . ? Ni1 N2 C2 O2 165.8(3) . . . . ? C3 N2 C2 C1 159.0(3) . . . . ? Ni1 N2 C2 C1 -17.5(3) . . . . ? O1 C1 C2 O2 7.3(5) . . . . ? N1 C1 C2 O2 -175.1(3) . . . . ? O1 C1 C2 N2 -169.7(3) . . . . ? N1 C1 C2 N2 7.9(4) . . . . ? C2 N2 C3 C4 -28.6(5) . . . . ? Ni1 N2 C3 C4 147.4(3) . . . . ? C2 N2 C3 C8 156.2(3) . . . . ? Ni1 N2 C3 C8 -27.8(5) . . . . ? N2 C3 C4 C5 -174.5(4) . . . . ? C8 C3 C4 C5 0.8(6) . . . . ? C3 C4 C5 C6 -1.4(7) . . . . ? C4 C5 C6 C7 0.2(8) . . . . ? C5 C6 C7 C8 1.7(8) . . . . ? C6 C7 C8 C3 -2.3(7) . . . . ? C6 C7 C8 C9 179.9(4) . . . . ? C4 C3 C8 C7 1.1(6) . . . . ? N2 C3 C8 C7 176.5(3) . . . . ? C4 C3 C8 C9 178.8(4) . . . . ? N2 C3 C8 C9 -5.7(5) . . . . ? C10 N3 C9 C8 -174.4(4) . . . . ? Ni1 N3 C9 C8 -1.0(6) . . . . ? C7 C8 C9 N3 -161.2(4) . . . . ? C3 C8 C9 N3 21.0(6) . . . . ? C9 N3 C10 C11 -113.9(4) . . . . ? Ni1 N3 C10 C11 72.0(4) . . . . ? N3 C10 C11 C12 -23.9(6) . . . . ? C13 N4 C12 C11 -120.1(4) . . . . ? Ni1 N4 C12 C11 71.3(4) . . . . ? C10 C11 C12 N4 -45.7(5) . . . . ? C12 N4 C13 C14 -177.0(4) . . . . ? Ni1 N4 C13 C14 -9.6(6) . . . . ? N4 C13 C14 C15 -173.7(4) . . . . ? N4 C13 C14 C19 6.8(6) . . . . ? C19 C14 C15 C16 -1.3(6) . . . . ? C13 C14 C15 C16 179.2(4) . . . . ? C14 C15 C16 C17 -0.9(6) . . . . ? C15 C16 C17 C18 2.0(7) . . . . ? C16 C17 C18 C19 -0.7(7) . . . . ? C17 C18 C19 N1 177.3(4) . . . . ? C17 C18 C19 C14 -1.6(6) . . . . ? C1 N1 C19 C18 -3.6(5) . . . . ? Ni1 N1 C19 C18 172.2(3) . . . . ? C1 N1 C19 C14 175.2(3) . . . . ? Ni1 N1 C19 C14 -9.0(5) . . . . ? C15 C14 C19 C18 2.6(5) . . . . ? C13 C14 C19 C18 -178.0(4) . . . . ? C15 C14 C19 N1 -176.4(3) . . . . ? C13 C14 C19 N1 3.1(5) . . . . ? C25 C20 C21 C22 -2.4(5) . . . . ? C26 C20 C21 C22 174.3(3) . . . . ? C20 C21 C22 C23 1.7(5) . . . . ? C20 C21 C22 C27 -173.6(3) . . . . ? C21 C22 C23 C24 0.7(5) . . . . ? C27 C22 C23 C24 176.0(3) . . . . ? C22 C23 C24 C25 -2.5(5) . . . . ? C22 C23 C24 C28 -178.7(3) . . . . ? C23 C24 C25 C20 1.8(5) . . . . ? C28 C24 C25 C20 178.0(3) . . . . ? C21 C20 C25 C24 0.6(5) . . . . ? C26 C20 C25 C24 -176.1(3) . . . . ? Zn2 O3 C26 O4 -3.6(5) . . . . ? Zn2 O3 C26 C20 174.2(2) . . . . ? C21 C20 C26 O4 -11.9(5) . . . . ? C25 C20 C26 O4 164.8(3) . . . . ? C21 C20 C26 O3 170.3(3) . . . . ? C25 C20 C26 O3 -13.1(4) . . . . ? Zn1 O5 C27 O6 4.5(5) 1_655 . . . ? Zn1 O5 C27 C22 -176.7(2) 1_655 . . . ? Zn2 O6 C27 O5 39.7(4) 1_655 . . . ? Zn2 O6 C27 C22 -139.1(2) 1_655 . . . ? C23 C22 C27 O5 166.5(3) . . . . ? C21 C22 C27 O5 -18.2(4) . . . . ? C23 C22 C27 O6 -14.6(4) . . . . ? C21 C22 C27 O6 160.7(3) . . . . ? Zn2 O8 C28 O7 78.2(4) 2_675 . . . ? Zn2 O8 C28 C24 -102.0(3) 2_675 . . . ? C25 C24 C28 O7 177.6(3) . . . . ? C23 C24 C28 O7 -6.2(5) . . . . ? C25 C24 C28 O8 -2.1(5) . . . . ? C23 C24 C28 O8 174.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.744 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.068 #===End data_091105d _database_code_depnum_ccdc_archive 'CCDC 800813' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.50 H22 Cd Cu N4 O8.50' _chemical_formula_weight 732.44 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' Cu Cu 0.3201 1.2651 '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)/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 10.021(3) _cell_length_b 13.739(4) _cell_length_c 18.812(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.981(4) _cell_angle_gamma 90.00 _cell_volume 2588.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.53 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5629 _exptl_absorpt_correction_T_max 0.7050 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16858 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.73 _reflns_number_total 7003 _reflns_number_gt 5305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0297P)^2^+1.2346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7003 _refine_ls_number_parameters 426 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd -0.108717(16) 0.587543(12) 0.048500(9) 0.02912(6) Uani 1 1 d . . . Cu1 Cu 0.16271(3) 0.53171(2) 0.310660(17) 0.03523(8) Uani 1 1 d . A . O1 O -0.0215(2) 0.67072(12) 0.15036(10) 0.0440(5) Uani 1 1 d . . . O2 O -0.0655(2) 0.48033(13) 0.13695(10) 0.0431(5) Uani 1 1 d . . . O3 O 0.14209(17) 0.55091(13) 0.02191(10) 0.0385(4) Uani 1 1 d . . . O4 O 0.03466(16) 0.68306(14) -0.01371(11) 0.0443(5) Uani 1 1 d . . . O5 O 0.2740(2) 0.97341(15) -0.08762(13) 0.0601(6) Uani 1 1 d . . . O6 O 0.49544(19) 0.97498(14) -0.08962(11) 0.0495(5) Uani 1 1 d . . . O7 O 0.74230(16) 0.70360(15) 0.01812(11) 0.0478(5) Uani 1 1 d . . . O8 O 0.64200(19) 0.57267(14) 0.05599(12) 0.0500(5) Uani 1 1 d . . . N1 N 0.0778(2) 0.64251(15) 0.26133(11) 0.0344(5) Uani 1 1 d . . . N2 N 0.0431(2) 0.45489(15) 0.24539(11) 0.0330(4) Uani 1 1 d . . . N3 N 0.2475(2) 0.41066(17) 0.34861(13) 0.0441(5) Uani 1 1 d D . . N4 N 0.2956(2) 0.6236(2) 0.35818(14) 0.0523(6) Uani 1 1 d D . . C1 C 0.0191(2) 0.61724(17) 0.19951(14) 0.0333(5) Uani 1 1 d . . . C2 C -0.0024(2) 0.50834(17) 0.19111(13) 0.0323(5) Uani 1 1 d . . . C3 C 0.0067(3) 0.35680(18) 0.25171(13) 0.0364(6) Uani 1 1 d . A . C4 C -0.1020(3) 0.3149(2) 0.21472(16) 0.0479(7) Uani 1 1 d . . . H4 H -0.1497 0.3514 0.1808 0.058 Uiso 1 1 calc R . . C5 C -0.1397(4) 0.2202(2) 0.22768(17) 0.0573(8) Uani 1 1 d . . . H5A H -0.2133 0.1943 0.2029 0.069 Uiso 1 1 calc R . . C6 C -0.0714(4) 0.1639(2) 0.27606(19) 0.0692(11) Uani 1 1 d . . . H6 H -0.0990 0.1007 0.2855 0.083 Uiso 1 1 calc R . . C7 C 0.0385(4) 0.2024(2) 0.31036(17) 0.0633(10) Uani 1 1 d . A . H7 H 0.0879 0.1632 0.3418 0.076 Uiso 1 1 calc R . . C8 C 0.0795(3) 0.29781(19) 0.30009(14) 0.0420(6) Uani 1 1 d . . . C9 C 0.1973(3) 0.3276(2) 0.33996(15) 0.0482(7) Uani 1 1 d . A . H9 H 0.2437 0.2774 0.3630 0.058 Uiso 1 1 calc R . . C10 C 0.3663(12) 0.4146(9) 0.3981(9) 0.061(4) Uani 0.516(10) 1 d PD A 1 H10A H 0.4159 0.3543 0.3946 0.073 Uiso 0.516(10) 1 calc PR A 1 H10B H 0.3369 0.4204 0.4465 0.073 Uiso 0.516(10) 1 calc PR A 1 C11 C 0.4557(6) 0.4977(6) 0.3824(4) 0.056(2) Uani 0.516(10) 1 d PD A 1 H11A H 0.5427 0.4857 0.4048 0.068 Uiso 0.516(10) 1 calc PR A 1 H11B H 0.4671 0.5007 0.3314 0.068 Uiso 0.516(10) 1 calc PR A 1 C12 C 0.4069(13) 0.5916(9) 0.4064(8) 0.087(6) Uani 0.516(10) 1 d PD A 1 H12A H 0.4784 0.6392 0.4063 0.105 Uiso 0.516(10) 1 calc PR A 1 H12B H 0.3762 0.5860 0.4546 0.105 Uiso 0.516(10) 1 calc PR A 1 C10' C 0.3812(13) 0.4067(10) 0.3856(10) 0.073(6) Uani 0.484(10) 1 d PD A 2 H10C H 0.3875 0.3486 0.4149 0.087 Uiso 0.484(10) 1 calc PR A 2 H10D H 0.4500 0.4033 0.3507 0.087 Uiso 0.484(10) 1 calc PR A 2 C11' C 0.4029(7) 0.4942(6) 0.4310(4) 0.063(3) Uani 0.484(10) 1 d PD A 2 H11C H 0.3269 0.5031 0.4608 0.076 Uiso 0.484(10) 1 calc PR A 2 H11D H 0.4815 0.4847 0.4617 0.076 Uiso 0.484(10) 1 calc PR A 2 C12' C 0.4203(11) 0.5809(10) 0.3875(10) 0.093(6) Uani 0.484(10) 1 d PD A 2 H12C H 0.4768 0.5645 0.3484 0.111 Uiso 0.484(10) 1 calc PR A 2 H12D H 0.4668 0.6298 0.4162 0.111 Uiso 0.484(10) 1 calc PR A 2 C13 C 0.2865(3) 0.7155(2) 0.35801(15) 0.0466(7) Uani 1 1 d . A . H13 H 0.3578 0.7489 0.3796 0.056 Uiso 1 1 calc R . . C14 C 0.1805(3) 0.7748(2) 0.32877(14) 0.0390(6) Uani 1 1 d . . . C15 C 0.1788(4) 0.8714(2) 0.35211(15) 0.0530(8) Uani 1 1 d . A . H15 H 0.2513 0.8960 0.3786 0.064 Uiso 1 1 calc R . . C16 C 0.0714(4) 0.9303(2) 0.3364(2) 0.0686(10) Uani 1 1 d . . . H16 H 0.0690 0.9938 0.3534 0.082 Uiso 1 1 calc R A . C17 C -0.0322(4) 0.8940(2) 0.2951(2) 0.0713(11) Uani 1 1 d . A . H17 H -0.1069 0.9326 0.2857 0.086 Uiso 1 1 calc R . . C18 C -0.0279(3) 0.8019(2) 0.26742(18) 0.0535(8) Uani 1 1 d . . . H18 H -0.0971 0.7807 0.2370 0.064 Uiso 1 1 calc R A . C19 C 0.0775(3) 0.74006(19) 0.28382(14) 0.0372(6) Uani 1 1 d . A . C20 C 0.2694(2) 0.68823(18) -0.01414(13) 0.0298(5) Uani 1 1 d . . . C21 C 0.3899(2) 0.64550(17) 0.00708(13) 0.0303(5) Uani 1 1 d . . . H21 H 0.3913 0.5821 0.0243 0.036 Uiso 1 1 calc R . . C22 C 0.5083(2) 0.69725(18) 0.00258(13) 0.0306(5) Uani 1 1 d . . . C23 C 0.5062(2) 0.79015(18) -0.02495(13) 0.0328(5) Uani 1 1 d . B . H23 H 0.5857 0.8244 -0.0284 0.039 Uiso 1 1 calc R . . C24 C 0.3870(2) 0.83345(18) -0.04771(13) 0.0313(5) Uani 1 1 d . . . C25 C 0.2687(2) 0.78213(17) -0.04137(13) 0.0310(5) Uani 1 1 d . B . H25 H 0.1881 0.8110 -0.0555 0.037 Uiso 1 1 calc R . . C26 C 0.1398(2) 0.63650(19) -0.00252(13) 0.0328(5) Uani 1 1 d . . . C27 C 0.6385(2) 0.65369(19) 0.02780(14) 0.0345(5) Uani 1 1 d . . . C28 C 0.3931(3) 0.93324(19) -0.07690(14) 0.0372(6) Uani 1 1 d . B . C29 C 0.2782(8) 1.0796(6) -0.1148(5) 0.074(2) Uani 0.50 1 d P B 1 H29A H 0.2056 1.1156 -0.0957 0.111 Uiso 0.50 1 calc PR B 1 H29B H 0.2704 1.0800 -0.1658 0.111 Uiso 0.50 1 calc PR B 1 H29C H 0.3613 1.1091 -0.0997 0.111 Uiso 0.50 1 calc PR B 1 O9 O 0.2495(5) 1.1509(3) -0.1217(3) 0.0641(13) Uani 0.50 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02345(8) 0.02833(9) 0.03511(10) 0.00476(7) -0.00565(6) -0.00129(7) Cu1 0.03284(16) 0.03587(17) 0.03619(17) 0.00498(14) -0.01006(12) 0.00057(13) O1 0.0588(12) 0.0295(9) 0.0423(11) 0.0061(8) -0.0204(9) -0.0019(8) O2 0.0595(12) 0.0311(10) 0.0375(10) 0.0043(8) -0.0163(9) -0.0084(8) O3 0.0377(10) 0.0353(10) 0.0423(10) -0.0001(8) -0.0004(8) -0.0114(8) O4 0.0211(8) 0.0517(11) 0.0601(12) 0.0077(10) 0.0003(8) -0.0016(8) O5 0.0410(11) 0.0444(12) 0.0942(18) 0.0226(12) -0.0053(11) 0.0038(9) O6 0.0433(11) 0.0429(11) 0.0627(13) 0.0105(10) 0.0062(9) -0.0103(9) O7 0.0206(8) 0.0539(12) 0.0685(14) 0.0101(10) -0.0031(8) 0.0018(8) O8 0.0367(10) 0.0382(11) 0.0742(15) 0.0031(10) -0.0129(10) 0.0050(8) N1 0.0362(11) 0.0288(11) 0.0375(12) 0.0018(9) -0.0100(9) -0.0024(8) N2 0.0377(11) 0.0289(11) 0.0320(11) 0.0045(9) -0.0050(9) 0.0011(9) N3 0.0429(13) 0.0459(14) 0.0429(13) 0.0060(11) -0.0082(10) 0.0107(11) N4 0.0426(14) 0.0562(16) 0.0563(16) 0.0055(13) -0.0236(12) -0.0069(11) C1 0.0303(12) 0.0288(12) 0.0400(14) 0.0029(11) -0.0074(10) -0.0006(9) C2 0.0332(12) 0.0287(12) 0.0346(13) 0.0029(10) -0.0051(10) -0.0011(10) C3 0.0490(15) 0.0274(12) 0.0331(13) -0.0001(11) 0.0031(11) 0.0010(11) C4 0.0603(18) 0.0356(15) 0.0473(17) 0.0067(13) -0.0058(14) -0.0065(13) C5 0.082(2) 0.0379(16) 0.0513(19) 0.0008(14) -0.0039(16) -0.0180(15) C6 0.117(3) 0.0312(16) 0.058(2) 0.0098(15) -0.007(2) -0.0171(18) C7 0.110(3) 0.0316(16) 0.0475(18) 0.0102(14) -0.0145(18) 0.0029(17) C8 0.0637(18) 0.0304(13) 0.0319(14) 0.0035(11) 0.0016(12) 0.0053(12) C9 0.0629(19) 0.0438(17) 0.0372(15) 0.0102(13) -0.0082(13) 0.0174(14) C10 0.053(6) 0.055(7) 0.073(7) 0.024(6) -0.026(5) -0.001(5) C11 0.026(3) 0.084(6) 0.058(5) 0.000(4) -0.007(3) 0.009(3) C12 0.098(10) 0.051(6) 0.107(9) -0.010(6) -0.085(7) 0.018(5) C10' 0.049(7) 0.086(11) 0.081(9) 0.005(7) -0.022(6) 0.030(7) C11' 0.036(4) 0.103(7) 0.049(5) 0.011(4) -0.015(3) 0.008(4) C12' 0.052(7) 0.099(13) 0.124(12) 0.017(9) -0.050(6) -0.025(7) C13 0.0438(15) 0.0542(19) 0.0411(16) -0.0002(14) -0.0068(12) -0.0168(13) C14 0.0448(15) 0.0413(15) 0.0308(13) 0.0005(11) -0.0001(11) -0.0098(12) C15 0.079(2) 0.0427(17) 0.0367(15) -0.0049(13) -0.0029(15) -0.0219(16) C16 0.105(3) 0.0351(18) 0.065(2) -0.0106(16) -0.009(2) -0.0020(18) C17 0.085(3) 0.0419(19) 0.086(3) -0.0064(18) -0.015(2) 0.0123(17) C18 0.0599(19) 0.0335(15) 0.066(2) -0.0025(14) -0.0148(15) 0.0027(13) C19 0.0430(14) 0.0337(13) 0.0345(13) -0.0002(11) -0.0022(11) -0.0055(11) C20 0.0219(11) 0.0332(12) 0.0340(13) -0.0033(10) -0.0010(9) -0.0011(9) C21 0.0270(11) 0.0284(12) 0.0354(13) -0.0012(10) -0.0017(9) 0.0001(9) C22 0.0218(11) 0.0345(13) 0.0355(13) -0.0036(10) -0.0025(9) 0.0024(9) C23 0.0227(11) 0.0366(13) 0.0391(14) -0.0025(11) 0.0008(9) -0.0050(9) C24 0.0264(11) 0.0322(13) 0.0352(13) 0.0023(10) -0.0004(9) -0.0018(9) C25 0.0219(11) 0.0331(13) 0.0379(13) 0.0011(10) -0.0028(9) 0.0014(9) C26 0.0262(12) 0.0379(14) 0.0342(13) -0.0048(11) -0.0008(9) -0.0075(10) C27 0.0242(11) 0.0398(14) 0.0393(14) -0.0081(12) -0.0034(10) 0.0043(10) C28 0.0376(14) 0.0362(14) 0.0374(14) 0.0009(11) -0.0027(11) -0.0003(11) C29 0.057(4) 0.078(6) 0.087(6) 0.027(5) -0.008(4) -0.001(4) O9 0.091(4) 0.026(2) 0.074(3) 0.009(2) -0.023(3) 0.002(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 Cd1 O7 2.2448(18) 1_455 ? Cd1 O2 2.2531(18) . ? Cd1 O4 2.2962(18) . ? Cd1 O3 2.3355(18) 3_565 ? Cd1 O1 2.3718(18) . ? Cd1 O8 2.515(2) 1_455 ? Cd1 O3 2.6283(19) . ? Cd1 C27 2.706(2) 1_455 ? Cu1 N1 1.962(2) . ? Cu1 N3 1.989(2) . ? Cu1 N2 1.989(2) . ? Cu1 N4 2.021(2) . ? O1 C1 1.239(3) . ? O2 C2 1.241(3) . ? O3 C26 1.263(3) . ? O3 Cd1 2.3354(18) 3_565 ? O4 C26 1.244(3) . ? O5 C28 1.323(3) . ? O5 C29 1.547(8) . ? O6 C28 1.207(3) . ? O7 C27 1.264(3) . ? O7 Cd1 2.2448(18) 1_655 ? O8 C27 1.233(3) . ? O8 Cd1 2.515(2) 1_655 ? N1 C1 1.331(3) . ? N1 C19 1.405(3) . ? N2 C2 1.326(3) . ? N2 C3 1.402(3) . ? N3 C9 1.256(4) . ? N3 C10 1.487(8) . ? N3 C10' 1.490(9) . ? N4 C13 1.266(4) . ? N4 C12' 1.471(8) . ? N4 C12 1.480(8) . ? C1 C2 1.519(3) . ? C3 C4 1.397(4) . ? C3 C8 1.404(4) . ? C4 C5 1.378(4) . ? C4 H4 0.9300 . ? C5 C6 1.362(5) . ? C5 H5A 0.9300 . ? C6 C7 1.364(5) . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 C9 1.436(4) . ? C9 H9 0.9300 . ? C10 C11 1.488(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.457(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10' C11' 1.486(10) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' C12' 1.459(9) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C13 C14 1.433(4) . ? C13 H13 0.9300 . ? C14 C19 1.396(4) . ? C14 C15 1.399(4) . ? C15 C16 1.370(5) . ? C15 H15 0.9300 . ? C16 C17 1.368(5) . ? C16 H16 0.9300 . ? C17 C18 1.370(4) . ? C17 H17 0.9300 . ? C18 C19 1.382(4) . ? C18 H18 0.9300 . ? C20 C25 1.388(3) . ? C20 C21 1.389(3) . ? C20 C26 1.503(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9300 . ? C22 C23 1.377(3) . ? C22 C27 1.498(3) . ? C23 C24 1.389(3) . ? C23 H23 0.9300 . ? C24 C25 1.388(3) . ? C24 C28 1.479(3) . ? C25 H25 0.9300 . ? C27 Cd1 2.706(2) 1_655 ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 O2 139.61(8) 1_455 . ? O7 Cd1 O4 83.49(7) 1_455 . ? O2 Cd1 O4 129.96(7) . . ? O7 Cd1 O3 110.69(7) 1_455 3_565 ? O2 Cd1 O3 84.63(7) . 3_565 ? O4 Cd1 O3 104.85(7) . 3_565 ? O7 Cd1 O1 94.97(7) 1_455 . ? O2 Cd1 O1 70.27(6) . . ? O4 Cd1 O1 85.23(7) . . ? O3 Cd1 O1 153.15(6) 3_565 . ? O7 Cd1 O8 54.47(6) 1_455 1_455 ? O2 Cd1 O8 94.11(7) . 1_455 ? O4 Cd1 O8 135.66(6) . 1_455 ? O3 Cd1 O8 80.94(6) 3_565 1_455 ? O1 Cd1 O8 109.44(7) . 1_455 ? O7 Cd1 O3 136.02(6) 1_455 . ? O2 Cd1 O3 81.64(7) . . ? O4 Cd1 O3 52.63(6) . . ? O3 Cd1 O3 81.68(6) 3_565 . ? O1 Cd1 O3 85.30(6) . . ? O8 Cd1 O3 162.42(6) 1_455 . ? O7 Cd1 C27 27.62(7) 1_455 1_455 ? O2 Cd1 C27 118.75(8) . 1_455 ? O4 Cd1 C27 109.50(7) . 1_455 ? O3 Cd1 C27 94.41(7) 3_565 1_455 ? O1 Cd1 C27 105.74(7) . 1_455 ? O8 Cd1 C27 27.00(7) 1_455 1_455 ? O3 Cd1 C27 158.95(7) . 1_455 ? N1 Cu1 N3 172.61(9) . . ? N1 Cu1 N2 82.96(8) . . ? N3 Cu1 N2 91.07(9) . . ? N1 Cu1 N4 89.59(9) . . ? N3 Cu1 N4 95.56(10) . . ? N2 Cu1 N4 168.05(10) . . ? C1 O1 Cd1 114.81(15) . . ? C2 O2 Cd1 118.87(16) . . ? C26 O3 Cd1 123.49(16) . 3_565 ? C26 O3 Cd1 83.41(14) . . ? Cd1 O3 Cd1 98.32(6) 3_565 . ? C26 O4 Cd1 99.27(16) . . ? C28 O5 C29 114.2(3) . . ? C27 O7 Cd1 96.96(16) . 1_655 ? C27 O8 Cd1 85.17(15) . 1_655 ? C1 N1 C19 120.4(2) . . ? C1 N1 Cu1 112.47(16) . . ? C19 N1 Cu1 127.09(16) . . ? C2 N2 C3 120.9(2) . . ? C2 N2 Cu1 111.43(16) . . ? C3 N2 Cu1 127.63(16) . . ? C9 N3 C10 115.0(5) . . ? C9 N3 C10' 112.1(6) . . ? C10 N3 C10' 11.7(13) . . ? C9 N3 Cu1 123.34(19) . . ? C10 N3 Cu1 121.1(5) . . ? C10' N3 Cu1 124.4(6) . . ? C13 N4 C12' 117.3(6) . . ? C13 N4 C12 110.5(5) . . ? C12' N4 C12 16.0(12) . . ? C13 N4 Cu1 125.16(19) . . ? C12' N4 Cu1 117.1(6) . . ? C12 N4 Cu1 123.8(5) . . ? O1 C1 N1 128.4(2) . . ? O1 C1 C2 117.7(2) . . ? N1 C1 C2 113.9(2) . . ? O2 C2 N2 127.7(2) . . ? O2 C2 C1 117.2(2) . . ? N2 C2 C1 114.9(2) . . ? C4 C3 N2 123.7(2) . . ? C4 C3 C8 117.6(2) . . ? N2 C3 C8 118.6(2) . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 118.3(3) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C8 122.5(3) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C3 119.0(3) . . ? C7 C8 C9 116.0(3) . . ? C3 C8 C9 125.0(2) . . ? N3 C9 C8 130.2(3) . . ? N3 C9 H9 114.9 . . ? C8 C9 H9 114.9 . . ? N3 C10 C11 112.2(8) . . ? N3 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N3 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 114.0(11) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.6 . . ? C11 C12 N4 109.1(8) . . ? C11 C12 H12A 109.9 . . ? N4 C12 H12A 109.9 . . ? C11 C12 H12B 109.9 . . ? N4 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C11' C10' N3 110.5(9) . . ? C11' C10' H10C 109.6 . . ? N3 C10' H10C 109.6 . . ? C11' C10' H10D 109.6 . . ? N3 C10' H10D 109.6 . . ? H10C C10' H10D 108.1 . . ? C12' C11' C10' 111.0(13) . . ? C12' C11' H11C 109.4 . . ? C10' C11' H11C 109.4 . . ? C12' C11' H11D 109.4 . . ? C10' C11' H11D 109.4 . . ? H11C C11' H11D 108.0 . . ? C11' C12' N4 114.8(9) . . ? C11' C12' H12C 108.6 . . ? N4 C12' H12C 108.6 . . ? C11' C12' H12D 108.6 . . ? N4 C12' H12D 108.6 . . ? H12C C12' H12D 107.6 . . ? N4 C13 C14 128.3(3) . . ? N4 C13 H13 115.9 . . ? C14 C13 H13 115.9 . . ? C19 C14 C15 119.8(3) . . ? C19 C14 C13 124.2(3) . . ? C15 C14 C13 115.8(3) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 118.9(3) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 121.3(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C19 121.1(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 117.9(3) . . ? C18 C19 N1 121.9(2) . . ? C14 C19 N1 119.9(2) . . ? C25 C20 C21 119.5(2) . . ? C25 C20 C26 120.0(2) . . ? C21 C20 C26 120.4(2) . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 C27 119.4(2) . . ? C21 C22 C27 120.9(2) . . ? C22 C23 C24 121.0(2) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 118.9(2) . . ? C25 C24 C28 123.3(2) . . ? C23 C24 C28 117.7(2) . . ? C24 C25 C20 120.7(2) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? O4 C26 O3 123.0(2) . . ? O4 C26 C20 117.6(2) . . ? O3 C26 C20 119.2(2) . . ? O8 C27 O7 122.7(2) . . ? O8 C27 C22 120.5(2) . . ? O7 C27 C22 116.7(2) . . ? O8 C27 Cd1 67.83(14) . 1_655 ? O7 C27 Cd1 55.42(12) . 1_655 ? C22 C27 Cd1 168.69(19) . 1_655 ? O6 C28 O5 122.7(2) . . ? O6 C28 C24 124.1(2) . . ? O5 C28 C24 113.3(2) . . ? O5 C29 H29A 109.5 . . ? O5 C29 H29B 109.5 . . ? O5 C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cd1 O1 C1 148.82(19) 1_455 . . . ? O2 Cd1 O1 C1 7.46(18) . . . . ? O4 Cd1 O1 C1 -128.16(19) . . . . ? O3 Cd1 O1 C1 -14.3(3) 3_565 . . . ? O8 Cd1 O1 C1 94.82(19) 1_455 . . . ? O3 Cd1 O1 C1 -75.33(19) . . . . ? C27 Cd1 O1 C1 122.91(19) 1_455 . . . ? O7 Cd1 O2 C2 -83.5(2) 1_455 . . . ? O4 Cd1 O2 C2 55.7(2) . . . . ? O3 Cd1 O2 C2 160.6(2) 3_565 . . . ? O1 Cd1 O2 C2 -9.77(19) . . . . ? O8 Cd1 O2 C2 -119.0(2) 1_455 . . . ? O3 Cd1 O2 C2 78.2(2) . . . . ? C27 Cd1 O2 C2 -107.3(2) 1_455 . . . ? O7 Cd1 O3 C26 11.73(18) 1_455 . . . ? O2 Cd1 O3 C26 -151.26(14) . . . . ? O4 Cd1 O3 C26 7.03(14) . . . . ? O3 Cd1 O3 C26 122.98(16) 3_565 . . . ? O1 Cd1 O3 C26 -80.55(14) . . . . ? O8 Cd1 O3 C26 131.7(2) 1_455 . . . ? C27 Cd1 O3 C26 42.4(2) 1_455 . . . ? O7 Cd1 O3 Cd1 -111.25(10) 1_455 . . 3_565 ? O2 Cd1 O3 Cd1 85.75(7) . . . 3_565 ? O4 Cd1 O3 Cd1 -115.96(10) . . . 3_565 ? O3 Cd1 O3 Cd1 0.0 3_565 . . 3_565 ? O1 Cd1 O3 Cd1 156.46(7) . . . 3_565 ? O8 Cd1 O3 Cd1 8.7(2) 1_455 . . 3_565 ? C27 Cd1 O3 Cd1 -80.58(19) 1_455 . . 3_565 ? O7 Cd1 O4 C26 176.10(17) 1_455 . . . ? O2 Cd1 O4 C26 21.3(2) . . . . ? O3 Cd1 O4 C26 -74.17(16) 3_565 . . . ? O1 Cd1 O4 C26 80.54(16) . . . . ? O8 Cd1 O4 C26 -166.36(14) 1_455 . . . ? O3 Cd1 O4 C26 -7.18(14) . . . . ? C27 Cd1 O4 C26 -174.44(15) 1_455 . . . ? N3 Cu1 N1 C1 17.8(8) . . . . ? N2 Cu1 N1 C1 -18.54(18) . . . . ? N4 Cu1 N1 C1 152.10(19) . . . . ? N3 Cu1 N1 C19 -160.4(7) . . . . ? N2 Cu1 N1 C19 163.2(2) . . . . ? N4 Cu1 N1 C19 -26.1(2) . . . . ? N1 Cu1 N2 C2 17.41(18) . . . . ? N3 Cu1 N2 C2 -158.22(19) . . . . ? N4 Cu1 N2 C2 -34.4(6) . . . . ? N1 Cu1 N2 C3 -162.8(2) . . . . ? N3 Cu1 N2 C3 21.6(2) . . . . ? N4 Cu1 N2 C3 145.4(4) . . . . ? N1 Cu1 N3 C9 -52.1(9) . . . . ? N2 Cu1 N3 C9 -16.1(3) . . . . ? N4 Cu1 N3 C9 173.9(3) . . . . ? N1 Cu1 N3 C10 136.6(11) . . . . ? N2 Cu1 N3 C10 172.6(9) . . . . ? N4 Cu1 N3 C10 2.6(9) . . . . ? N1 Cu1 N3 C10' 123.2(12) . . . . ? N2 Cu1 N3 C10' 159.2(9) . . . . ? N4 Cu1 N3 C10' -10.8(9) . . . . ? N1 Cu1 N4 C13 11.5(3) . . . . ? N3 Cu1 N4 C13 -173.8(3) . . . . ? N2 Cu1 N4 C13 62.8(6) . . . . ? N1 Cu1 N4 C12' -160.5(8) . . . . ? N3 Cu1 N4 C12' 14.2(8) . . . . ? N2 Cu1 N4 C12' -109.3(9) . . . . ? N1 Cu1 N4 C12 -177.4(9) . . . . ? N3 Cu1 N4 C12 -2.7(9) . . . . ? N2 Cu1 N4 C12 -126.1(9) . . . . ? Cd1 O1 C1 N1 176.9(2) . . . . ? Cd1 O1 C1 C2 -5.1(3) . . . . ? C19 N1 C1 O1 12.5(4) . . . . ? Cu1 N1 C1 O1 -165.8(2) . . . . ? C19 N1 C1 C2 -165.6(2) . . . . ? Cu1 N1 C1 C2 16.1(3) . . . . ? Cd1 O2 C2 N2 -173.2(2) . . . . ? Cd1 O2 C2 C1 10.8(3) . . . . ? C3 N2 C2 O2 -9.2(4) . . . . ? Cu1 N2 C2 O2 170.6(2) . . . . ? C3 N2 C2 C1 166.9(2) . . . . ? Cu1 N2 C2 C1 -13.3(3) . . . . ? O1 C1 C2 O2 -3.5(4) . . . . ? N1 C1 C2 O2 174.8(2) . . . . ? O1 C1 C2 N2 -180.0(2) . . . . ? N1 C1 C2 N2 -1.6(3) . . . . ? C2 N2 C3 C4 -17.1(4) . . . . ? Cu1 N2 C3 C4 163.2(2) . . . . ? C2 N2 C3 C8 165.8(2) . . . . ? Cu1 N2 C3 C8 -14.0(3) . . . . ? N2 C3 C4 C5 -174.4(3) . . . . ? C8 C3 C4 C5 2.8(4) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C4 C5 C6 C7 -1.8(6) . . . . ? C5 C6 C7 C8 2.9(6) . . . . ? C6 C7 C8 C3 -1.1(5) . . . . ? C6 C7 C8 C9 -179.9(3) . . . . ? C4 C3 C8 C7 -1.7(4) . . . . ? N2 C3 C8 C7 175.6(3) . . . . ? C4 C3 C8 C9 177.0(3) . . . . ? N2 C3 C8 C9 -5.7(4) . . . . ? C10 N3 C9 C8 175.9(9) . . . . ? C10' N3 C9 C8 -171.7(9) . . . . ? Cu1 N3 C9 C8 4.1(5) . . . . ? C7 C8 C9 N3 -169.9(3) . . . . ? C3 C8 C9 N3 11.4(5) . . . . ? C9 N3 C10 C11 153.9(9) . . . . ? C10' N3 C10 C11 75(5) . . . . ? Cu1 N3 C10 C11 -34.1(16) . . . . ? N3 C10 C11 C12 76.5(14) . . . . ? C10 C11 C12 N4 -74.6(13) . . . . ? C13 N4 C12 C11 -153.6(9) . . . . ? C12' N4 C12 C11 -35(3) . . . . ? Cu1 N4 C12 C11 34.2(16) . . . . ? C9 N3 C10' C11' -147.0(10) . . . . ? C10 N3 C10' C11' -41(4) . . . . ? Cu1 N3 C10' C11' 37.2(17) . . . . ? N3 C10' C11' C12' -70.4(15) . . . . ? C10' C11' C12' N4 79.9(16) . . . . ? C13 N4 C12' C11' 139.6(11) . . . . ? C12 N4 C12' C11' 71(4) . . . . ? Cu1 N4 C12' C11' -47.7(17) . . . . ? C12' N4 C13 C14 175.8(9) . . . . ? C12 N4 C13 C14 -168.4(8) . . . . ? Cu1 N4 C13 C14 3.7(5) . . . . ? N4 C13 C14 C19 -11.7(5) . . . . ? N4 C13 C14 C15 163.6(3) . . . . ? C19 C14 C15 C16 5.6(5) . . . . ? C13 C14 C15 C16 -169.9(3) . . . . ? C14 C15 C16 C17 -2.4(5) . . . . ? C15 C16 C17 C18 -2.5(6) . . . . ? C16 C17 C18 C19 4.2(6) . . . . ? C17 C18 C19 C14 -0.9(5) . . . . ? C17 C18 C19 N1 174.0(3) . . . . ? C15 C14 C19 C18 -3.9(4) . . . . ? C13 C14 C19 C18 171.3(3) . . . . ? C15 C14 C19 N1 -178.9(2) . . . . ? C13 C14 C19 N1 -3.7(4) . . . . ? C1 N1 C19 C18 33.0(4) . . . . ? Cu1 N1 C19 C18 -148.9(2) . . . . ? C1 N1 C19 C14 -152.2(3) . . . . ? Cu1 N1 C19 C14 25.9(4) . . . . ? C25 C20 C21 C22 1.5(4) . . . . ? C26 C20 C21 C22 -173.8(2) . . . . ? C20 C21 C22 C23 -1.9(4) . . . . ? C20 C21 C22 C27 177.7(2) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C27 C22 C23 C24 -178.9(2) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C22 C23 C24 C28 -179.8(2) . . . . ? C23 C24 C25 C20 -1.4(4) . . . . ? C28 C24 C25 C20 179.4(2) . . . . ? C21 C20 C25 C24 0.2(4) . . . . ? C26 C20 C25 C24 175.4(2) . . . . ? Cd1 O4 C26 O3 14.3(3) . . . . ? Cd1 O4 C26 C20 -161.35(18) . . . . ? Cd1 O3 C26 O4 83.3(3) 3_565 . . . ? Cd1 O3 C26 O4 -12.4(2) . . . . ? Cd1 O3 C26 C20 -101.2(2) 3_565 . . . ? Cd1 O3 C26 C20 163.2(2) . . . . ? C25 C20 C26 O4 -4.6(3) . . . . ? C21 C20 C26 O4 170.6(2) . . . . ? C25 C20 C26 O3 179.6(2) . . . . ? C21 C20 C26 O3 -5.2(3) . . . . ? Cd1 O8 C27 O7 -7.9(3) 1_655 . . . ? Cd1 O8 C27 C22 171.5(2) 1_655 . . . ? Cd1 O7 C27 O8 8.9(3) 1_655 . . . ? Cd1 O7 C27 C22 -170.52(18) 1_655 . . . ? C23 C22 C27 O8 176.3(2) . . . . ? C21 C22 C27 O8 -3.3(4) . . . . ? C23 C22 C27 O7 -4.3(4) . . . . ? C21 C22 C27 O7 176.2(2) . . . . ? C23 C22 C27 Cd1 -48.1(10) . . . 1_655 ? C21 C22 C27 Cd1 132.4(8) . . . 1_655 ? C29 O5 C28 O6 -2.4(5) . . . . ? C29 O5 C28 C24 177.3(4) . . . . ? C25 C24 C28 O6 -172.0(3) . . . . ? C23 C24 C28 O6 8.8(4) . . . . ? C25 C24 C28 O5 8.3(4) . . . . ? C23 C24 C28 O5 -170.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.572 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.075 #===End data_091213a _database_code_depnum_ccdc_archive 'CCDC 800814' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H31 N4 Ni2.50 O13' _chemical_formula_weight 790.35 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7772(6) _cell_length_b 12.0096(7) _cell_length_c 14.0441(9) _cell_angle_alpha 88.6690(10) _cell_angle_beta 82.8440(10) _cell_angle_gamma 71.6580(10) _cell_volume 1552.87(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3106 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.7427 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _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_% ? _diffrn_reflns_number 8054 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5464 _reflns_number_gt 4487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0345P)^2^+1.2225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5464 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.0000 0.0000 0.0000 0.02049(12) Uani 1 2 d S . . Ni2 Ni 0.79320(4) 0.23358(3) 0.17967(3) 0.02684(11) Uani 1 1 d . . . Ni3 Ni 0.78599(5) 0.26286(4) 0.55230(3) 0.03575(12) Uani 1 1 d . . . O1 O 0.9205(2) 0.15518(18) 0.28484(14) 0.0352(5) Uani 1 1 d . . . O2 O 0.6463(2) 0.29219(18) 0.30142(14) 0.0336(5) Uani 1 1 d . . . O3 O 1.1929(2) -0.06514(17) 0.05688(14) 0.0289(4) Uani 1 1 d . . . O4 O 1.2077(2) 0.09801(18) 0.12120(17) 0.0410(6) Uani 1 1 d . . . O5 O 1.6976(2) 0.10959(17) 0.16894(15) 0.0342(5) Uani 1 1 d . . . O6 O 1.8885(2) -0.04774(16) 0.12103(14) 0.0284(4) Uani 1 1 d . . . O7 O 1.8034(2) -0.43337(19) 0.0966(2) 0.0565(7) Uani 1 1 d . . . O8 O 1.5772(3) -0.4359(2) 0.1063(3) 0.0965(13) Uani 1 1 d . . . O9 O 0.95741(19) 0.16878(16) 0.06604(13) 0.0262(4) Uani 1 1 d . . . H9A H 1.0393 0.1414 0.0868 0.039 Uiso 1 1 d R . . H9B H 0.9501 0.2255 0.0276 0.039 Uiso 1 1 d R . . O10 O 0.6602(2) 0.33655(19) 0.08845(16) 0.0439(6) Uani 1 1 d . . . H10A H 0.6356 0.4110 0.0899 0.066 Uiso 1 1 d R . . H10B H 0.5916 0.3064 0.0908 0.066 Uiso 1 1 d R . . O11 O 0.8738(2) 0.37180(18) 0.20189(15) 0.0409(5) Uani 1 1 d . . . H11A H 0.8398 0.4275 0.1643 0.061 Uiso 1 1 d R . . H11B H 0.9613 0.3601 0.2116 0.061 Uiso 1 1 d R . . O12 O 0.9550(2) 0.36628(19) 0.96669(16) 0.0453(6) Uani 1 1 d . . . H12A H 0.8926 0.4164 1.0048 0.068 Uiso 1 1 d R . . H12B H 1.0352 0.3792 0.9501 0.068 Uiso 1 1 d R . . O13 O 0.1693(4) 0.3044(3) 0.2195(3) 0.1139(14) Uani 1 1 d . . . H13 H 0.1786 0.2344 0.2144 0.171 Uiso 1 1 d R . . N1 N 0.9224(3) 0.1782(2) 0.44930(18) 0.0334(6) Uani 1 1 d . . . N2 N 0.6458(3) 0.2933(2) 0.46686(17) 0.0348(6) Uani 1 1 d . . . N3 N 0.6621(4) 0.3814(2) 0.63743(19) 0.0463(7) Uani 1 1 d . . . N4 N 0.9087(3) 0.2038(3) 0.64684(19) 0.0429(7) Uani 1 1 d . . . C1 C 0.8641(3) 0.1947(3) 0.3670(2) 0.0315(7) Uani 1 1 d . . . C2 C 0.7053(3) 0.2671(3) 0.3765(2) 0.0313(7) Uani 1 1 d . . . C3 C 0.4939(3) 0.3306(3) 0.4918(2) 0.0362(7) Uani 1 1 d . . . C4 C 0.3996(4) 0.3032(3) 0.4368(3) 0.0436(8) Uani 1 1 d . . . H4 H 0.4365 0.2620 0.3791 0.052 Uiso 1 1 calc R . . C5 C 0.2523(4) 0.3362(3) 0.4663(3) 0.0554(10) Uani 1 1 d . . . H5 H 0.1913 0.3158 0.4291 0.066 Uiso 1 1 calc R . . C6 C 0.1945(5) 0.3995(4) 0.5512(3) 0.0674(12) Uani 1 1 d . . . H6 H 0.0950 0.4224 0.5707 0.081 Uiso 1 1 calc R . . C7 C 0.2852(5) 0.4278(4) 0.6058(3) 0.0624(11) Uani 1 1 d . . . H7 H 0.2462 0.4714 0.6622 0.075 Uiso 1 1 calc R . . C8 C 0.4354(4) 0.3929(3) 0.5791(2) 0.0429(8) Uani 1 1 d . . . C9 C 0.5244(5) 0.4265(3) 0.6399(2) 0.0504(10) Uani 1 1 d . . . H9 H 0.4778 0.4861 0.6850 0.061 Uiso 1 1 calc R . . C10 C 0.7367(5) 0.4358(4) 0.6983(3) 0.0613(11) Uani 1 1 d . . . H10 H 0.6683 0.5074 0.7277 0.074 Uiso 1 1 calc R . . H10' H 0.8137 0.4564 0.6590 0.074 Uiso 1 1 calc R . . C11 C 0.8003(5) 0.3530(4) 0.7761(3) 0.0691(12) Uani 1 1 d . . . H11 H 0.8868 0.3683 0.7913 0.083 Uiso 1 1 calc R . . H11' H 0.7306 0.3685 0.8336 0.083 Uiso 1 1 calc R . . C12 C 0.8388(5) 0.2254(4) 0.7473(2) 0.0583(11) Uani 1 1 d . . . H12 H 0.9042 0.1775 0.7897 0.070 Uiso 1 1 calc R . . H12' H 0.7514 0.2025 0.7544 0.070 Uiso 1 1 calc R . . C13 C 1.0376(4) 0.1321(3) 0.6329(2) 0.0471(9) Uani 1 1 d . . . H13' H 1.0815 0.1044 0.6876 0.057 Uiso 1 1 calc R . . C14 C 1.1228(4) 0.0895(3) 0.5424(2) 0.0397(8) Uani 1 1 d . . . C15 C 1.2667(4) 0.0191(3) 0.5471(3) 0.0499(9) Uani 1 1 d . . . H15 H 1.3006 0.0052 0.6066 0.060 Uiso 1 1 calc R . . C16 C 1.3581(4) -0.0296(3) 0.4669(3) 0.0511(9) Uani 1 1 d . . . H16 H 1.4528 -0.0766 0.4715 0.061 Uiso 1 1 calc R . . C17 C 1.3075(4) -0.0078(3) 0.3794(3) 0.0532(10) Uani 1 1 d . . . H17 H 1.3696 -0.0395 0.3242 0.064 Uiso 1 1 calc R . . C18 C 1.1660(4) 0.0603(3) 0.3713(3) 0.0477(9) Uani 1 1 d . . . H18 H 1.1347 0.0729 0.3110 0.057 Uiso 1 1 calc R . . C19 C 1.0691(3) 0.1107(3) 0.4529(2) 0.0368(7) Uani 1 1 d . . . C20 C 1.4150(3) -0.0710(2) 0.1098(2) 0.0255(6) Uani 1 1 d . . . C21 C 1.5067(3) -0.0084(2) 0.1278(2) 0.0263(6) Uani 1 1 d . . . H21 H 1.4700 0.0727 0.1355 0.032 Uiso 1 1 calc R . . C22 C 1.6522(3) -0.0652(2) 0.13437(19) 0.0239(6) Uani 1 1 d . . . C23 C 1.7048(3) -0.1867(2) 0.1265(2) 0.0307(7) Uani 1 1 d . . . H23 H 1.8021 -0.2254 0.1317 0.037 Uiso 1 1 calc R . . C24 C 1.6141(3) -0.2512(2) 0.1110(2) 0.0331(7) Uani 1 1 d . . . C25 C 1.4697(3) -0.1922(2) 0.1012(2) 0.0298(7) Uani 1 1 d . . . H25 H 1.4088 -0.2346 0.0888 0.036 Uiso 1 1 calc R . . C26 C 1.2601(3) -0.0083(2) 0.0955(2) 0.0265(6) Uani 1 1 d . . . C27 C 1.7549(3) 0.0039(2) 0.14247(19) 0.0258(6) Uani 1 1 d . . . C28 C 1.6685(4) -0.3836(3) 0.1036(3) 0.0494(9) Uani 1 1 d . . . C29 C 0.2713(18) 0.3375(7) 0.1409(6) 0.311(10) Uani 1 1 d . . . H29A H 0.2415 0.4212 0.1346 0.466 Uiso 1 1 calc R . . H29B H 0.2680 0.3017 0.0812 0.466 Uiso 1 1 calc R . . H29C H 0.3686 0.3103 0.1575 0.466 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 0.0154(2) 0.0188(2) 0.0249(3) -0.00351(19) -0.00105(19) -0.0023(2) Ni2 0.0268(2) 0.0222(2) 0.0290(2) -0.00576(15) -0.00011(15) -0.00487(16) Ni3 0.0428(3) 0.0356(2) 0.0263(2) 0.00034(17) -0.00350(17) -0.00899(19) O1 0.0320(12) 0.0357(12) 0.0298(12) -0.0039(9) -0.0013(9) -0.0001(10) O2 0.0327(12) 0.0336(12) 0.0273(11) -0.0049(9) -0.0021(9) -0.0006(10) O3 0.0234(11) 0.0278(11) 0.0351(11) 0.0010(9) -0.0077(9) -0.0061(9) O4 0.0265(11) 0.0317(12) 0.0604(15) -0.0149(11) -0.0124(10) 0.0007(10) O5 0.0263(11) 0.0260(11) 0.0476(13) -0.0116(9) 0.0055(9) -0.0076(9) O6 0.0188(10) 0.0269(11) 0.0369(11) 0.0026(9) -0.0011(8) -0.0043(9) O7 0.0275(13) 0.0244(12) 0.111(2) 0.0024(13) 0.0025(13) -0.0028(10) O8 0.0395(16) 0.0281(14) 0.223(4) -0.0140(19) -0.018(2) -0.0099(13) O9 0.0210(10) 0.0239(10) 0.0299(11) -0.0016(8) -0.0026(8) -0.0017(8) O10 0.0470(14) 0.0307(12) 0.0561(15) 0.0006(11) -0.0172(12) -0.0111(11) O11 0.0455(14) 0.0342(12) 0.0448(13) -0.0045(10) -0.0080(11) -0.0138(11) O12 0.0439(14) 0.0397(13) 0.0494(14) -0.0039(11) 0.0042(11) -0.0126(11) O13 0.110(3) 0.078(3) 0.156(4) -0.033(3) -0.053(3) -0.016(2) N1 0.0361(15) 0.0298(14) 0.0323(14) 0.0025(11) -0.0052(11) -0.0076(12) N2 0.0362(15) 0.0323(14) 0.0297(14) -0.0031(11) 0.0016(11) -0.0038(12) N3 0.066(2) 0.0394(17) 0.0305(15) -0.0026(12) -0.0034(14) -0.0129(16) N4 0.0513(19) 0.0493(17) 0.0309(15) 0.0074(13) -0.0078(13) -0.0195(15) C1 0.0325(17) 0.0259(16) 0.0337(17) 0.0021(13) -0.0025(13) -0.0065(13) C2 0.0350(17) 0.0255(15) 0.0311(17) -0.0020(13) -0.0001(13) -0.0075(13) C3 0.0387(19) 0.0273(16) 0.0350(17) 0.0022(13) 0.0029(14) -0.0027(14) C4 0.040(2) 0.0390(19) 0.047(2) -0.0024(15) 0.0026(16) -0.0074(16) C5 0.042(2) 0.052(2) 0.067(3) 0.003(2) 0.0009(19) -0.0111(18) C6 0.040(2) 0.073(3) 0.073(3) 0.002(2) 0.016(2) -0.004(2) C7 0.057(3) 0.061(3) 0.050(2) -0.007(2) 0.015(2) 0.001(2) C8 0.046(2) 0.0343(18) 0.0368(18) -0.0016(14) 0.0069(15) -0.0010(16) C9 0.070(3) 0.038(2) 0.0308(18) -0.0047(15) 0.0018(17) -0.0016(19) C10 0.088(3) 0.055(2) 0.043(2) -0.0094(18) -0.016(2) -0.022(2) C11 0.088(3) 0.083(3) 0.038(2) -0.008(2) -0.014(2) -0.026(3) C12 0.065(3) 0.075(3) 0.0312(19) 0.0139(18) -0.0066(17) -0.018(2) C13 0.055(2) 0.052(2) 0.039(2) 0.0153(16) -0.0175(17) -0.022(2) C14 0.044(2) 0.0370(18) 0.0429(19) 0.0090(15) -0.0128(15) -0.0170(16) C15 0.048(2) 0.049(2) 0.058(2) 0.0172(18) -0.0212(19) -0.0182(18) C16 0.034(2) 0.042(2) 0.077(3) 0.0069(19) -0.0151(19) -0.0093(17) C17 0.035(2) 0.056(2) 0.063(3) -0.0025(19) -0.0050(18) -0.0060(18) C18 0.039(2) 0.053(2) 0.044(2) 0.0014(17) -0.0081(16) -0.0039(17) C19 0.0377(18) 0.0337(17) 0.0409(19) 0.0051(14) -0.0080(14) -0.0129(15) C20 0.0213(14) 0.0270(15) 0.0263(15) -0.0003(12) -0.0019(11) -0.0049(12) C21 0.0221(15) 0.0236(15) 0.0289(15) -0.0012(12) -0.0001(12) -0.0022(12) C22 0.0203(14) 0.0266(15) 0.0238(14) -0.0005(11) -0.0002(11) -0.0068(12) C23 0.0207(15) 0.0264(16) 0.0418(18) -0.0016(13) -0.0027(13) -0.0030(13) C24 0.0260(16) 0.0215(15) 0.0487(19) -0.0012(13) -0.0028(14) -0.0036(13) C25 0.0236(15) 0.0264(16) 0.0403(17) -0.0046(13) -0.0030(13) -0.0090(13) C26 0.0234(15) 0.0293(16) 0.0242(15) 0.0012(12) -0.0005(12) -0.0055(13) C27 0.0273(16) 0.0272(16) 0.0221(14) 0.0017(12) -0.0013(12) -0.0083(13) C28 0.0319(19) 0.0252(17) 0.087(3) -0.0036(17) -0.0035(18) -0.0047(15) C29 0.71(3) 0.104(6) 0.101(7) 0.002(5) -0.015(12) -0.111(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.0558(19) 2_755 ? Ni1 O3 2.0558(19) . ? Ni1 O6 2.0718(18) 1_455 ? Ni1 O6 2.0718(18) 2_855 ? Ni1 O9 2.1452(18) . ? Ni1 O9 2.1452(18) 2_755 ? Ni2 O5 2.009(2) 1_455 ? Ni2 O10 2.047(2) . ? Ni2 O1 2.067(2) . ? Ni2 O2 2.0714(19) . ? Ni2 O9 2.0888(18) . ? Ni2 O11 2.093(2) . ? Ni3 N4 1.877(3) . ? Ni3 N2 1.878(3) . ? Ni3 N3 1.886(3) . ? Ni3 N1 1.908(3) . ? O1 C1 1.250(3) . ? O2 C2 1.250(4) . ? O3 C26 1.256(3) . ? O4 C26 1.259(3) . ? O5 C27 1.259(3) . ? O5 Ni2 2.009(2) 1_655 ? O6 C27 1.258(3) . ? O6 Ni1 2.0718(18) 1_655 ? O7 C28 1.257(4) . ? O8 C28 1.240(4) . ? O9 H9A 0.8501 . ? O9 H9B 0.8501 . ? O10 H10A 0.8501 . ? O10 H10B 0.8540 . ? O11 H11A 0.8500 . ? O11 H11B 0.8502 . ? O12 H12A 0.8499 . ? O12 H12B 0.8500 . ? O13 C29 1.525(12) . ? O13 H13 0.8200 . ? N1 C1 1.336(4) . ? N1 C19 1.414(4) . ? N2 C2 1.329(4) . ? N2 C3 1.409(4) . ? N3 C9 1.279(5) . ? N3 C10 1.474(5) . ? N4 C13 1.277(4) . ? N4 C12 1.480(4) . ? C1 C2 1.512(4) . ? C3 C4 1.391(5) . ? C3 C8 1.410(4) . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 C6 1.387(6) . ? C5 H5 0.9300 . ? C6 C7 1.364(6) . ? C6 H6 0.9300 . ? C7 C8 1.399(5) . ? C7 H7 0.9300 . ? C8 C9 1.440(5) . ? C9 H9 0.9300 . ? C10 C11 1.516(5) . ? C10 H10 0.9700 . ? C10 H10' 0.9700 . ? C11 C12 1.510(6) . ? C11 H11 0.9700 . ? C11 H11' 0.9700 . ? C12 H12 0.9700 . ? C12 H12' 0.9700 . ? C13 C14 1.438(5) . ? C13 H13' 0.9300 . ? C14 C15 1.404(5) . ? C14 C19 1.410(4) . ? C15 C16 1.364(5) . ? C15 H15 0.9300 . ? C16 C17 1.370(5) . ? C16 H16 0.9300 . ? C17 C18 1.385(5) . ? C17 H17 0.9300 . ? C18 C19 1.406(5) . ? C18 H18 0.9300 . ? C20 C25 1.386(4) . ? C20 C21 1.387(4) . ? C20 C26 1.501(4) . ? C21 C22 1.385(4) . ? C21 H21 0.9300 . ? C22 C23 1.388(4) . ? C22 C27 1.506(4) . ? C23 C24 1.386(4) . ? C23 H23 0.9300 . ? C24 C25 1.389(4) . ? C24 C28 1.511(4) . ? C25 H25 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 O3 Ni1 O3 180.00(16) 2_755 . ? O3 Ni1 O6 89.02(7) 2_755 1_455 ? O3 Ni1 O6 90.98(7) . 1_455 ? O3 Ni1 O6 90.98(7) 2_755 2_855 ? O3 Ni1 O6 89.02(7) . 2_855 ? O6 Ni1 O6 180.00(13) 1_455 2_855 ? O3 Ni1 O9 88.34(7) 2_755 . ? O3 Ni1 O9 91.66(7) . . ? O6 Ni1 O9 88.69(7) 1_455 . ? O6 Ni1 O9 91.31(7) 2_855 . ? O3 Ni1 O9 91.66(7) 2_755 2_755 ? O3 Ni1 O9 88.34(7) . 2_755 ? O6 Ni1 O9 91.31(7) 1_455 2_755 ? O6 Ni1 O9 88.69(7) 2_855 2_755 ? O9 Ni1 O9 180.00(10) . 2_755 ? O5 Ni2 O10 89.64(9) 1_455 . ? O5 Ni2 O1 97.37(9) 1_455 . ? O10 Ni2 O1 170.43(8) . . ? O5 Ni2 O2 86.29(8) 1_455 . ? O10 Ni2 O2 94.31(9) . . ? O1 Ni2 O2 79.72(8) . . ? O5 Ni2 O9 95.62(8) 1_455 . ? O10 Ni2 O9 91.11(8) . . ? O1 Ni2 O9 94.66(8) . . ? O2 Ni2 O9 174.27(8) . . ? O5 Ni2 O11 173.79(8) 1_455 . ? O10 Ni2 O11 89.47(9) . . ? O1 Ni2 O11 82.86(9) . . ? O2 Ni2 O11 87.65(8) . . ? O9 Ni2 O11 90.54(8) . . ? N4 Ni3 N2 166.56(12) . . ? N4 Ni3 N3 91.07(13) . . ? N2 Ni3 N3 90.96(12) . . ? N4 Ni3 N1 94.54(12) . . ? N2 Ni3 N1 86.94(11) . . ? N3 Ni3 N1 164.49(12) . . ? C1 O1 Ni2 112.48(18) . . ? C2 O2 Ni2 111.88(18) . . ? C26 O3 Ni1 127.60(18) . . ? C27 O5 Ni2 128.75(18) . 1_655 ? C27 O6 Ni1 120.07(17) . 1_655 ? Ni2 O9 Ni1 122.74(9) . . ? Ni2 O9 H9A 110.4 . . ? Ni1 O9 H9A 87.2 . . ? Ni2 O9 H9B 105.3 . . ? Ni1 O9 H9B 115.5 . . ? H9A O9 H9B 115.1 . . ? Ni2 O10 H10A 122.8 . . ? Ni2 O10 H10B 102.7 . . ? H10A O10 H10B 116.6 . . ? Ni2 O11 H11A 109.6 . . ? Ni2 O11 H11B 122.1 . . ? H11A O11 H11B 115.7 . . ? H12A O12 H12B 116.5 . . ? C29 O13 H13 109.5 . . ? C1 N1 C19 121.6(3) . . ? C1 N1 Ni3 110.9(2) . . ? C19 N1 Ni3 127.5(2) . . ? C2 N2 C3 121.4(3) . . ? C2 N2 Ni3 112.1(2) . . ? C3 N2 Ni3 126.3(2) . . ? C9 N3 C10 117.8(3) . . ? C9 N3 Ni3 126.8(3) . . ? C10 N3 Ni3 115.0(3) . . ? C13 N4 C12 117.2(3) . . ? C13 N4 Ni3 126.1(2) . . ? C12 N4 Ni3 115.6(2) . . ? O1 C1 N1 129.2(3) . . ? O1 C1 C2 116.1(3) . . ? N1 C1 C2 114.6(3) . . ? O2 C2 N2 128.4(3) . . ? O2 C2 C1 117.9(3) . . ? N2 C2 C1 113.6(3) . . ? C4 C3 N2 123.0(3) . . ? C4 C3 C8 118.4(3) . . ? N2 C3 C8 118.6(3) . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 121.6(4) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C3 119.2(4) . . ? C7 C8 C9 118.6(3) . . ? C3 C8 C9 122.2(3) . . ? N3 C9 C8 125.7(3) . . ? N3 C9 H9 117.1 . . ? C8 C9 H9 117.1 . . ? N3 C10 C11 110.9(3) . . ? N3 C10 H10 109.4 . . ? C11 C10 H10 109.4 . . ? N3 C10 H10' 109.4 . . ? C11 C10 H10' 109.4 . . ? H10 C10 H10' 108.0 . . ? C12 C11 C10 112.9(3) . . ? C12 C11 H11 109.0 . . ? C10 C11 H11 109.0 . . ? C12 C11 H11' 109.0 . . ? C10 C11 H11' 109.0 . . ? H11 C11 H11' 107.8 . . ? N4 C12 C11 111.4(3) . . ? N4 C12 H12 109.3 . . ? C11 C12 H12 109.3 . . ? N4 C12 H12' 109.3 . . ? C11 C12 H12' 109.3 . . ? H12 C12 H12' 108.0 . . ? N4 C13 C14 127.5(3) . . ? N4 C13 H13' 116.2 . . ? C14 C13 H13' 116.2 . . ? C15 C14 C19 119.8(3) . . ? C15 C14 C13 115.9(3) . . ? C19 C14 C13 124.3(3) . . ? C16 C15 C14 121.9(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.6(3) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C16 C17 C18 121.5(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C19 121.1(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 117.0(3) . . ? C18 C19 N1 123.6(3) . . ? C14 C19 N1 119.4(3) . . ? C25 C20 C21 119.2(3) . . ? C25 C20 C26 120.2(3) . . ? C21 C20 C26 120.5(2) . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 C27 120.5(2) . . ? C23 C22 C27 120.1(2) . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 118.9(3) . . ? C23 C24 C28 121.8(3) . . ? C25 C24 C28 119.3(3) . . ? C20 C25 C24 120.9(3) . . ? C20 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? O3 C26 O4 124.8(3) . . ? O3 C26 C20 117.5(2) . . ? O4 C26 C20 117.7(3) . . ? O6 C27 O5 126.1(3) . . ? O6 C27 C22 117.7(2) . . ? O5 C27 C22 116.2(2) . . ? O8 C28 O7 124.4(3) . . ? O8 C28 C24 117.9(3) . . ? O7 C28 C24 117.7(3) . . ? O13 C29 H29A 109.5 . . ? O13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Ni2 O1 C1 -97.2(2) 1_455 . . . ? O10 Ni2 O1 C1 39.6(6) . . . . ? O2 Ni2 O1 C1 -12.4(2) . . . . ? O9 Ni2 O1 C1 166.5(2) . . . . ? O11 Ni2 O1 C1 76.5(2) . . . . ? O5 Ni2 O2 C2 106.5(2) 1_455 . . . ? O10 Ni2 O2 C2 -164.1(2) . . . . ? O1 Ni2 O2 C2 8.3(2) . . . . ? O9 Ni2 O2 C2 -3.2(9) . . . . ? O11 Ni2 O2 C2 -74.9(2) . . . . ? O3 Ni1 O3 C26 -174(100) 2_755 . . . ? O6 Ni1 O3 C26 -101.9(2) 1_455 . . . ? O6 Ni1 O3 C26 78.1(2) 2_855 . . . ? O9 Ni1 O3 C26 -13.2(2) . . . . ? O9 Ni1 O3 C26 166.8(2) 2_755 . . . ? O5 Ni2 O9 Ni1 -11.26(12) 1_455 . . . ? O10 Ni2 O9 Ni1 -101.01(11) . . . . ? O1 Ni2 O9 Ni1 86.64(11) . . . . ? O2 Ni2 O9 Ni1 98.0(8) . . . . ? O11 Ni2 O9 Ni1 169.51(11) . . . . ? O3 Ni1 O9 Ni2 69.95(11) 2_755 . . . ? O3 Ni1 O9 Ni2 -110.05(11) . . . . ? O6 Ni1 O9 Ni2 -19.11(11) 1_455 . . . ? O6 Ni1 O9 Ni2 160.89(11) 2_855 . . . ? O9 Ni1 O9 Ni2 -124(100) 2_755 . . . ? N4 Ni3 N1 C1 175.8(2) . . . . ? N2 Ni3 N1 C1 9.2(2) . . . . ? N3 Ni3 N1 C1 -73.3(5) . . . . ? N4 Ni3 N1 C19 -7.5(3) . . . . ? N2 Ni3 N1 C19 -174.1(3) . . . . ? N3 Ni3 N1 C19 103.4(5) . . . . ? N4 Ni3 N2 C2 -109.6(5) . . . . ? N3 Ni3 N2 C2 151.8(2) . . . . ? N1 Ni3 N2 C2 -12.8(2) . . . . ? N4 Ni3 N2 C3 65.6(6) . . . . ? N3 Ni3 N2 C3 -33.1(3) . . . . ? N1 Ni3 N2 C3 162.3(3) . . . . ? N4 Ni3 N3 C9 -147.5(3) . . . . ? N2 Ni3 N3 C9 19.2(3) . . . . ? N1 Ni3 N3 C9 101.2(5) . . . . ? N4 Ni3 N3 C10 40.5(3) . . . . ? N2 Ni3 N3 C10 -152.8(2) . . . . ? N1 Ni3 N3 C10 -70.8(5) . . . . ? N2 Ni3 N4 C13 96.3(6) . . . . ? N3 Ni3 N4 C13 -165.1(3) . . . . ? N1 Ni3 N4 C13 0.5(3) . . . . ? N2 Ni3 N4 C12 -71.6(6) . . . . ? N3 Ni3 N4 C12 27.1(3) . . . . ? N1 Ni3 N4 C12 -167.4(3) . . . . ? Ni2 O1 C1 N1 -169.2(3) . . . . ? Ni2 O1 C1 C2 13.9(3) . . . . ? C19 N1 C1 O1 2.0(5) . . . . ? Ni3 N1 C1 O1 178.9(3) . . . . ? C19 N1 C1 C2 178.9(3) . . . . ? Ni3 N1 C1 C2 -4.2(3) . . . . ? Ni2 O2 C2 N2 178.0(3) . . . . ? Ni2 O2 C2 C1 -3.8(3) . . . . ? C3 N2 C2 O2 16.1(5) . . . . ? Ni3 N2 C2 O2 -168.5(3) . . . . ? C3 N2 C2 C1 -162.1(3) . . . . ? Ni3 N2 C2 C1 13.3(3) . . . . ? O1 C1 C2 O2 -7.2(4) . . . . ? N1 C1 C2 O2 175.6(3) . . . . ? O1 C1 C2 N2 171.3(3) . . . . ? N1 C1 C2 N2 -6.0(4) . . . . ? C2 N2 C3 C4 24.2(5) . . . . ? Ni3 N2 C3 C4 -150.5(3) . . . . ? C2 N2 C3 C8 -159.3(3) . . . . ? Ni3 N2 C3 C8 26.0(4) . . . . ? N2 C3 C4 C5 176.6(3) . . . . ? C8 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 1.2(6) . . . . ? C4 C5 C6 C7 -0.7(6) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? C6 C7 C8 C3 2.3(6) . . . . ? C6 C7 C8 C9 179.7(4) . . . . ? C4 C3 C8 C7 -1.8(5) . . . . ? N2 C3 C8 C7 -178.4(3) . . . . ? C4 C3 C8 C9 -179.1(3) . . . . ? N2 C3 C8 C9 4.3(5) . . . . ? C10 N3 C9 C8 173.6(3) . . . . ? Ni3 N3 C9 C8 1.7(5) . . . . ? C7 C8 C9 N3 163.8(4) . . . . ? C3 C8 C9 N3 -18.9(5) . . . . ? C9 N3 C10 C11 114.1(4) . . . . ? Ni3 N3 C10 C11 -73.1(4) . . . . ? N3 C10 C11 C12 28.1(5) . . . . ? C13 N4 C12 C11 119.4(4) . . . . ? Ni3 N4 C12 C11 -71.6(4) . . . . ? C10 C11 C12 N4 41.9(5) . . . . ? C12 N4 C13 C14 174.2(3) . . . . ? Ni3 N4 C13 C14 6.5(5) . . . . ? N4 C13 C14 C15 174.6(3) . . . . ? N4 C13 C14 C19 -7.7(6) . . . . ? C19 C14 C15 C16 0.5(5) . . . . ? C13 C14 C15 C16 178.3(3) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? C16 C17 C18 C19 0.6(6) . . . . ? C17 C18 C19 C14 0.5(5) . . . . ? C17 C18 C19 N1 -178.1(3) . . . . ? C15 C14 C19 C18 -1.0(5) . . . . ? C13 C14 C19 C18 -178.6(3) . . . . ? C15 C14 C19 N1 177.7(3) . . . . ? C13 C14 C19 N1 0.0(5) . . . . ? C1 N1 C19 C18 2.7(5) . . . . ? Ni3 N1 C19 C18 -173.7(3) . . . . ? C1 N1 C19 C14 -175.8(3) . . . . ? Ni3 N1 C19 C14 7.8(4) . . . . ? C25 C20 C21 C22 2.0(4) . . . . ? C26 C20 C21 C22 -175.5(2) . . . . ? C20 C21 C22 C23 -2.5(4) . . . . ? C20 C21 C22 C27 172.9(2) . . . . ? C21 C22 C23 C24 0.8(4) . . . . ? C27 C22 C23 C24 -174.6(3) . . . . ? C22 C23 C24 C25 1.5(5) . . . . ? C22 C23 C24 C28 -179.1(3) . . . . ? C21 C20 C25 C24 0.4(4) . . . . ? C26 C20 C25 C24 177.8(3) . . . . ? C23 C24 C25 C20 -2.0(5) . . . . ? C28 C24 C25 C20 178.5(3) . . . . ? Ni1 O3 C26 O4 13.1(4) . . . . ? Ni1 O3 C26 C20 -165.34(17) . . . . ? C25 C20 C26 O3 -14.4(4) . . . . ? C21 C20 C26 O3 163.0(3) . . . . ? C25 C20 C26 O4 167.0(3) . . . . ? C21 C20 C26 O4 -15.6(4) . . . . ? Ni1 O6 C27 O5 -67.0(3) 1_655 . . . ? Ni1 O6 C27 C22 111.8(2) 1_655 . . . ? Ni2 O5 C27 O6 3.6(4) 1_655 . . . ? Ni2 O5 C27 C22 -175.24(17) 1_655 . . . ? C21 C22 C27 O6 -160.2(3) . . . . ? C23 C22 C27 O6 15.2(4) . . . . ? C21 C22 C27 O5 18.8(4) . . . . ? C23 C22 C27 O5 -165.9(3) . . . . ? C23 C24 C28 O8 167.9(4) . . . . ? C25 C24 C28 O8 -12.7(6) . . . . ? C23 C24 C28 O7 -11.1(5) . . . . ? C25 C24 C28 O7 168.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.545 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.062 #===End data_100106a _database_code_depnum_ccdc_archive 'CCDC 800815' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H82 Cd4 N16 Ni4 O30' _chemical_formula_weight 2708.29 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' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 18.4200(7) _cell_length_b 14.3984(6) _cell_length_c 18.8098(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.4300(10) _cell_angle_gamma 90.00 _cell_volume 4946.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9883 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 1.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6507 _exptl_absorpt_correction_T_max 0.7301 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _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_% ? _diffrn_reflns_number 25658 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13515 _reflns_number_gt 12511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0485P)^2^+3.6106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.489(16) _refine_ls_number_reflns 13515 _refine_ls_number_parameters 1424 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.52843(2) 0.03125(3) 0.653039(19) 0.02669(9) Uani 1 1 d . . . Cd2 Cd 0.38395(2) 0.08320(3) 0.78137(2) 0.02949(10) Uani 1 1 d . . . Cd3 Cd 0.12150(2) 0.47190(3) 0.71122(2) 0.03059(10) Uani 1 1 d . . . Cd4 Cd -0.02563(2) 0.52218(3) 0.85955(2) 0.03271(10) Uani 1 1 d . . . Ni1 Ni 0.73507(4) 0.14091(8) 0.88264(4) 0.0479(2) Uani 1 1 d . . . Ni2 Ni 0.58183(4) -0.01101(6) 1.01360(4) 0.03443(18) Uani 1 1 d . . . Ni3 Ni -0.22093(4) 0.36755(8) 0.63708(4) 0.0472(2) Uani 1 1 d . . . Ni4 Ni -0.08414(4) 0.53490(7) 0.48218(4) 0.03673(18) Uani 1 1 d . . . O1 O 0.5866(2) 0.1615(3) 0.7136(2) 0.0421(11) Uani 1 1 d . . . O2 O 0.6041(2) -0.0151(4) 0.7514(2) 0.0435(11) Uani 1 1 d . . . O3 O 0.4710(2) 0.1444(3) 0.8675(2) 0.0420(11) Uani 1 1 d . . . O4 O 0.4546(2) -0.0369(3) 0.8348(2) 0.0363(10) Uani 1 1 d . . . O5 O -0.0780(2) 0.3796(3) 0.8114(2) 0.0418(10) Uani 1 1 d . . . O6 O -0.1062(3) 0.5501(3) 0.7602(3) 0.0504(13) Uani 1 1 d . . . O7 O 0.0308(2) 0.3963(3) 0.6360(2) 0.0403(11) Uani 1 1 d . . . O8 O 0.0404(2) 0.5789(3) 0.6621(2) 0.0357(9) Uani 1 1 d . . . O9 O 0.4676(2) 0.1451(3) 0.5911(2) 0.0386(10) Uani 1 1 d . . . O10 O 0.4262(2) 0.1665(4) 0.6959(2) 0.0451(12) Uani 1 1 d . . . O11 O 0.2128(2) 0.3739(3) 0.6925(2) 0.0391(10) Uani 1 1 d . . . O12 O 0.1907(2) 0.4808(4) 0.6100(2) 0.0446(11) Uani 1 1 d . . . O13 O 0.3659(3) 0.5122(4) 0.4224(3) 0.0584(14) Uani 1 1 d . . . O14 O 0.4665(2) 0.4310(4) 0.4388(2) 0.0479(12) Uani 1 1 d . . . O15 O 0.4394(2) -0.0644(4) 0.6795(3) 0.0514(12) Uani 1 1 d . . . O16 O 0.3306(2) -0.0239(3) 0.7100(3) 0.0489(11) Uani 1 1 d . . . O17 O 0.1665(3) -0.2803(4) 0.7722(3) 0.0678(16) Uani 1 1 d . . . O18 O 0.2021(3) -0.4259(4) 0.7635(3) 0.0536(12) Uani 1 1 d . . . O19 O 0.4419(3) -0.4908(4) 0.6653(3) 0.0585(13) Uani 1 1 d . . . O20 O 0.4830(3) -0.3745(5) 0.6054(4) 0.083(2) Uani 1 1 d . . . H20 H 0.5093 -0.4150 0.5918 0.124 Uiso 1 1 d R . . O21 O 0.2907(3) 0.0465(5) 0.8644(3) 0.079(2) Uani 1 1 d . . . O22 O 0.2919(2) 0.1758(3) 0.8034(3) 0.0440(11) Uani 1 1 d . . . O23 O 0.0851(3) 0.4069(4) 0.8063(3) 0.0565(14) Uani 1 1 d . . . O24 O 0.0488(2) 0.4159(4) 0.9133(2) 0.0439(11) Uani 1 1 d . . . O25 O 0.0338(3) 0.1275(4) 1.0520(3) 0.0737(18) Uani 1 1 d . . . O26 O 0.1155(3) 0.0221(5) 1.0495(3) 0.0717(17) Uani 1 1 d . . . O27 O 0.0397(3) 0.6424(4) 0.8186(2) 0.0579(14) Uani 1 1 d . . . H27A H 0.0410 0.6807 0.8543 0.087 Uiso 1 1 d R . . H27B H 0.0805 0.6262 0.8030 0.087 Uiso 1 1 d R . . O28 O 0.5658(4) 0.5277(7) 0.5391(4) 0.122(3) Uani 1 1 d . . . O29 O 0.8316(5) 0.3992(6) 0.1679(5) 0.127(3) Uani 1 1 d . . . N1 N 0.6747(3) 0.2036(4) 0.8092(3) 0.0387(13) Uani 1 1 d . . . N2 N 0.6948(3) 0.0302(5) 0.8422(3) 0.0439(13) Uani 1 1 d . . . N3 N 0.7714(3) 0.0808(7) 0.9694(3) 0.069(2) Uani 1 1 d . . . N4 N 0.7953(3) 0.2448(7) 0.9060(3) 0.064(2) Uani 1 1 d . . . N5 N 0.5551(3) 0.1006(4) 0.9652(3) 0.0339(12) Uani 1 1 d . . . N6 N 0.5491(3) -0.0710(4) 0.9266(3) 0.0324(11) Uani 1 1 d . . . N7 N 0.6216(4) -0.1178(5) 1.0591(3) 0.0604(18) Uani 1 1 d . . . N8 N 0.5856(3) 0.0481(5) 1.1048(3) 0.0533(16) Uani 1 1 d . . . N9 N -0.1575(3) 0.3204(4) 0.7147(3) 0.0384(12) Uani 1 1 d . . . N10 N -0.1857(3) 0.4868(5) 0.6666(3) 0.0456(14) Uani 1 1 d . . . N11 N -0.2602(3) 0.4073(7) 0.5459(3) 0.072(3) Uani 1 1 d . . . N12 N -0.2762(3) 0.2569(7) 0.6244(3) 0.062(2) Uani 1 1 d . . . N13 N -0.0549(3) 0.4280(4) 0.5372(3) 0.0341(12) Uani 1 1 d . . . N14 N -0.0515(3) 0.6028(4) 0.5672(3) 0.0337(12) Uani 1 1 d . . . N15 N -0.1259(4) 0.6378(6) 0.4321(3) 0.0640(19) Uani 1 1 d . . . N16 N -0.0918(4) 0.4641(6) 0.3956(3) 0.0645(18) Uani 1 1 d . . . C1 C 0.6314(3) 0.1440(5) 0.7674(3) 0.0338(14) Uani 1 1 d . . . C2 C 0.6427(3) 0.0437(5) 0.7879(3) 0.0370(15) Uani 1 1 d . . . C3 C 0.7204(4) -0.0612(7) 0.8597(4) 0.057(2) Uani 1 1 d . . . C4 C 0.7118(4) -0.1354(7) 0.8142(5) 0.069(2) Uani 1 1 d . . . H4 H 0.6890 -0.1262 0.7677 0.082 Uiso 1 1 calc R . . C5 C 0.7354(5) -0.2222(7) 0.8340(6) 0.081(3) Uani 1 1 d . . . H5 H 0.7275 -0.2704 0.8010 0.097 Uiso 1 1 calc R . . C6 C 0.7691(6) -0.2400(10) 0.8987(7) 0.101(4) Uani 1 1 d U . . H6 H 0.7843 -0.2998 0.9121 0.121 Uiso 1 1 calc R . . C7 C 0.7810(6) -0.1670(9) 0.9455(6) 0.100(4) Uani 1 1 d . . . H7 H 0.8051 -0.1787 0.9912 0.120 Uiso 1 1 calc R . . C8 C 0.7591(5) -0.0768(8) 0.9286(4) 0.076(3) Uani 1 1 d . . . C9 C 0.7753(5) -0.0078(10) 0.9802(5) 0.085(3) Uani 1 1 d . . . H9 H 0.7903 -0.0274 1.0269 0.102 Uiso 1 1 calc R . . C10 C 0.7871(5) 0.1470(9) 1.0323(4) 0.088(3) Uani 1 1 d . . . H10A H 0.7928 0.1119 1.0767 0.105 Uiso 1 1 calc R . . H10B H 0.7459 0.1889 1.0331 0.105 Uiso 1 1 calc R . . C11 C 0.8577(5) 0.2042(8) 1.0270(5) 0.085(3) Uani 1 1 d U . . H11A H 0.8557 0.2615 1.0539 0.102 Uiso 1 1 calc R . . H11B H 0.8999 0.1692 1.0484 0.102 Uiso 1 1 calc R . . C12 C 0.8668(4) 0.2274(9) 0.9490(5) 0.089(4) Uani 1 1 d . . . H12A H 0.8975 0.2821 0.9479 0.107 Uiso 1 1 calc R . . H12B H 0.8910 0.1762 0.9282 0.107 Uiso 1 1 calc R . . C13 C 0.7850(4) 0.3274(8) 0.8834(5) 0.070(3) Uani 1 1 d . . . H13 H 0.8203 0.3712 0.9000 0.084 Uiso 1 1 calc R . . C14 C 0.7225(4) 0.3600(6) 0.8335(4) 0.053(2) Uani 1 1 d . . . C15 C 0.7182(5) 0.4559(7) 0.8183(5) 0.075(3) Uani 1 1 d . . . H15 H 0.7549 0.4945 0.8403 0.090 Uiso 1 1 calc R . . C16 C 0.6636(6) 0.4943(7) 0.7736(6) 0.080(3) Uani 1 1 d . . . H16 H 0.6628 0.5577 0.7639 0.096 Uiso 1 1 calc R . . C17 C 0.6100(5) 0.4375(6) 0.7434(5) 0.067(2) Uani 1 1 d . . . H17 H 0.5709 0.4633 0.7137 0.080 Uiso 1 1 calc R . . C18 C 0.6109(4) 0.3430(6) 0.7547(4) 0.0546(19) Uani 1 1 d . . . H18 H 0.5721 0.3071 0.7332 0.066 Uiso 1 1 calc R . . C19 C 0.6681(4) 0.3004(5) 0.7974(4) 0.0455(16) Uani 1 1 d . . . C20 C 0.5075(3) 0.0856(5) 0.9058(3) 0.0321(13) Uani 1 1 d . . . C21 C 0.5003(3) -0.0163(5) 0.8852(3) 0.0307(13) Uani 1 1 d . . . C22 C 0.5570(3) -0.1637(5) 0.9088(3) 0.0369(14) Uani 1 1 d . . . C23 C 0.5400(4) -0.1975(6) 0.8384(4) 0.0523(18) Uani 1 1 d . . . H23 H 0.5209 -0.1576 0.8018 0.063 Uiso 1 1 calc R . . C24 C 0.5516(5) -0.2902(6) 0.8236(5) 0.069(2) Uani 1 1 d . . . H24 H 0.5399 -0.3114 0.7768 0.083 Uiso 1 1 calc R . . C25 C 0.5798(5) -0.3520(6) 0.8757(5) 0.070(2) Uani 1 1 d . . . H25 H 0.5869 -0.4140 0.8646 0.084 Uiso 1 1 calc R . . C26 C 0.5971(5) -0.3203(5) 0.9448(5) 0.056(2) Uani 1 1 d . . . H26 H 0.6151 -0.3617 0.9808 0.068 Uiso 1 1 calc R . . C27 C 0.5881(4) -0.2262(5) 0.9621(4) 0.0437(17) Uani 1 1 d . . . C28 C 0.6192(5) -0.1993(6) 1.0331(4) 0.062(2) Uani 1 1 d . . . H28 H 0.6397 -0.2464 1.0631 0.074 Uiso 1 1 calc R . . C29 C 0.6673(5) -0.1055(7) 1.1326(5) 0.079(3) Uani 1 1 d . . . H29A H 0.6952 -0.1616 1.1451 0.095 Uiso 1 1 calc R . . H29B H 0.7016 -0.0548 1.1304 0.095 Uiso 1 1 calc R . . C30 C 0.6204(5) -0.0860(6) 1.1868(4) 0.073(3) Uani 1 1 d . . . H30A H 0.6503 -0.0653 1.2302 0.088 Uiso 1 1 calc R . . H30B H 0.5959 -0.1428 1.1980 0.088 Uiso 1 1 calc R . . C31 C 0.5630(5) -0.0119(7) 1.1631(4) 0.070(2) Uani 1 1 d . . . H31A H 0.5168 -0.0419 1.1461 0.084 Uiso 1 1 calc R . . H31B H 0.5556 0.0266 1.2039 0.084 Uiso 1 1 calc R . . C32 C 0.5938(4) 0.1359(6) 1.1158(4) 0.0553(19) Uani 1 1 d . . . H32 H 0.5935 0.1568 1.1625 0.066 Uiso 1 1 calc R . . C33 C 0.6037(4) 0.2066(5) 1.0610(4) 0.0438(16) Uani 1 1 d . . . C34 C 0.6289(4) 0.2949(6) 1.0830(4) 0.0527(19) Uani 1 1 d . . . H34 H 0.6452 0.3049 1.1312 0.063 Uiso 1 1 calc R . . C35 C 0.6304(4) 0.3668(5) 1.0363(4) 0.0493(17) Uani 1 1 d . . . H35 H 0.6477 0.4250 1.0517 0.059 Uiso 1 1 calc R . . C36 C 0.6052(4) 0.3499(5) 0.9649(4) 0.0490(18) Uani 1 1 d . . . H36 H 0.6061 0.3982 0.9322 0.059 Uiso 1 1 calc R . . C37 C 0.5788(4) 0.2646(5) 0.9403(4) 0.0416(16) Uani 1 1 d . . . H37 H 0.5619 0.2565 0.8920 0.050 Uiso 1 1 calc R . . C38 C 0.5775(3) 0.1901(5) 0.9880(3) 0.0363(15) Uani 1 1 d . . . C39 C -0.1211(3) 0.3859(5) 0.7542(3) 0.0341(14) Uani 1 1 d . . . C40 C -0.1379(3) 0.4842(5) 0.7262(3) 0.0339(14) Uani 1 1 d . . . C41 C -0.2140(3) 0.5722(7) 0.6391(4) 0.058(2) Uani 1 1 d . . . C42 C -0.2080(4) 0.6539(7) 0.6779(6) 0.078(3) Uani 1 1 d . . . H42 H -0.1838 0.6537 0.7245 0.094 Uiso 1 1 calc R . . C43 C -0.2379(5) 0.7379(9) 0.6481(7) 0.104(4) Uani 1 1 d . . . H43 H -0.2350 0.7925 0.6747 0.125 Uiso 1 1 calc R . . C44 C -0.2716(6) 0.7357(10) 0.5782(7) 0.098(3) Uani 1 1 d U . . H44 H -0.2912 0.7905 0.5577 0.118 Uiso 1 1 calc R . . C45 C -0.2772(6) 0.6586(9) 0.5391(6) 0.093(3) Uani 1 1 d U . . H45 H -0.2987 0.6610 0.4916 0.111 Uiso 1 1 calc R . . C46 C -0.2509(4) 0.5733(9) 0.5684(5) 0.083(4) Uani 1 1 d . . . C47 C -0.2650(4) 0.4912(12) 0.5254(5) 0.090(4) Uani 1 1 d . . . H47 H -0.2792 0.5008 0.4767 0.107 Uiso 1 1 calc R . . C48 C -0.2777(4) 0.3344(10) 0.4915(4) 0.098(4) Uani 1 1 d . . . H48A H -0.2367 0.2919 0.4930 0.117 Uiso 1 1 calc R . . H48B H -0.2851 0.3626 0.4443 0.117 Uiso 1 1 calc R . . C49 C -0.3458(4) 0.2807(10) 0.5036(4) 0.096(4) Uani 1 1 d . . . H49A H -0.3449 0.2201 0.4811 0.115 Uiso 1 1 calc R . . H49B H -0.3888 0.3135 0.4814 0.115 Uiso 1 1 calc R . . C50 C -0.3502(4) 0.2687(8) 0.5830(4) 0.082(3) Uani 1 1 d . . . H50A H -0.3738 0.3227 0.6007 0.099 Uiso 1 1 calc R . . H50B H -0.3800 0.2148 0.5901 0.099 Uiso 1 1 calc R . . C51 C -0.2587(5) 0.1767(7) 0.6538(5) 0.067(3) Uani 1 1 d . . . H51 H -0.2918 0.1282 0.6434 0.080 Uiso 1 1 calc R . . C52 C -0.1944(4) 0.1571(6) 0.6996(4) 0.0525(19) Uani 1 1 d . . . C53 C -0.1802(6) 0.0624(6) 0.7185(6) 0.076(3) Uani 1 1 d . . . H53 H -0.2140 0.0178 0.7000 0.091 Uiso 1 1 calc R . . C54 C -0.1201(6) 0.0342(7) 0.7620(6) 0.087(3) Uani 1 1 d . . . H54 H -0.1133 -0.0282 0.7739 0.105 Uiso 1 1 calc R . . C55 C -0.0695(5) 0.0995(6) 0.7884(5) 0.074(2) Uani 1 1 d . . . H55 H -0.0270 0.0812 0.8171 0.089 Uiso 1 1 calc R . . C56 C -0.0815(5) 0.1926(6) 0.7725(4) 0.058(2) Uani 1 1 d . . . H56 H -0.0465 0.2356 0.7913 0.069 Uiso 1 1 calc R . . C57 C -0.1434(4) 0.2245(5) 0.7297(4) 0.0461(17) Uani 1 1 d . . . C58 C -0.0074(3) 0.4494(4) 0.5948(3) 0.0303(13) Uani 1 1 d . . . C59 C -0.0038(3) 0.5525(4) 0.6111(3) 0.0300(13) Uani 1 1 d . . . C60 C -0.0628(3) 0.6972(5) 0.5801(4) 0.0423(16) Uani 1 1 d . . . C61 C -0.0473(4) 0.7374(5) 0.6479(4) 0.0488(17) Uani 1 1 d . . . H61 H -0.0272 0.7008 0.6862 0.059 Uiso 1 1 calc R . . C62 C -0.0609(4) 0.8296(6) 0.6598(4) 0.058(2) Uani 1 1 d . . . H62 H -0.0522 0.8538 0.7059 0.070 Uiso 1 1 calc R . . C63 C -0.0878(5) 0.8866(6) 0.6028(5) 0.067(2) Uani 1 1 d . . . H63 H -0.0946 0.9497 0.6103 0.080 Uiso 1 1 calc R . . C64 C -0.1040(4) 0.8499(5) 0.5360(4) 0.0526(19) Uani 1 1 d . . . H64 H -0.1230 0.8882 0.4983 0.063 Uiso 1 1 calc R . . C65 C -0.0928(4) 0.7566(5) 0.5229(4) 0.0468(17) Uani 1 1 d . . . C66 C -0.1226(5) 0.7229(7) 0.4540(4) 0.067(2) Uani 1 1 d . . . H66 H -0.1420 0.7674 0.4210 0.081 Uiso 1 1 calc R . . C67 C -0.1771(5) 0.6131(9) 0.3621(5) 0.091(3) Uani 1 1 d U . . H67A H -0.2094 0.5624 0.3710 0.109 Uiso 1 1 calc R . . H67B H -0.2069 0.6664 0.3458 0.109 Uiso 1 1 calc R . . C68 C -0.1309(6) 0.5858(8) 0.3068(4) 0.096(3) Uani 1 1 d . . . H68A H -0.1621 0.5605 0.2660 0.116 Uiso 1 1 calc R . . H68B H -0.1075 0.6410 0.2908 0.116 Uiso 1 1 calc R . . C69 C -0.0742(5) 0.5175(10) 0.3312(4) 0.096(4) Uani 1 1 d . . . H69A H -0.0278 0.5491 0.3431 0.116 Uiso 1 1 calc R . . H69B H -0.0692 0.4744 0.2925 0.116 Uiso 1 1 calc R . . C70 C -0.0998(4) 0.3749(7) 0.3909(4) 0.068(2) Uani 1 1 d . . . H70 H -0.1056 0.3496 0.3451 0.081 Uiso 1 1 calc R . . C71 C -0.1006(4) 0.3130(6) 0.4480(4) 0.0461(18) Uani 1 1 d . . . C72 C -0.1224(4) 0.2198(6) 0.4332(5) 0.061(2) Uani 1 1 d . . . H72 H -0.1384 0.2033 0.3860 0.073 Uiso 1 1 calc R . . C73 C -0.1209(4) 0.1537(6) 0.4845(5) 0.061(2) Uani 1 1 d . . . H73 H -0.1369 0.0935 0.4733 0.073 Uiso 1 1 calc R . . C74 C -0.0953(4) 0.1778(5) 0.5529(4) 0.054(2) Uani 1 1 d . . . H74 H -0.0940 0.1327 0.5884 0.065 Uiso 1 1 calc R . . C75 C -0.0714(4) 0.2656(5) 0.5720(4) 0.0429(16) Uani 1 1 d . . . H75 H -0.0527 0.2782 0.6193 0.051 Uiso 1 1 calc R . . C76 C -0.0753(3) 0.3367(5) 0.5201(3) 0.0358(15) Uani 1 1 d . . . C77 C 0.3933(3) 0.2758(4) 0.6039(3) 0.0246(12) Uani 1 1 d . . . C78 C 0.4160(3) 0.3229(4) 0.5451(3) 0.0283(13) Uani 1 1 d . . . H78 H 0.4558 0.3012 0.5241 0.034 Uiso 1 1 calc R . . C79 C 0.3789(3) 0.4015(4) 0.5184(3) 0.0277(12) Uani 1 1 d . . . C80 C 0.3169(3) 0.4308(4) 0.5472(3) 0.0297(12) Uani 1 1 d . . . H80 H 0.2904 0.4816 0.5274 0.036 Uiso 1 1 calc R . . C81 C 0.2945(3) 0.3847(4) 0.6052(3) 0.0286(12) Uani 1 1 d . . . C82 C 0.3335(3) 0.3078(4) 0.6340(3) 0.0295(13) Uani 1 1 d . . . H82 H 0.3192 0.2777 0.6736 0.035 Uiso 1 1 calc R . . C83 C 0.4314(3) 0.1896(4) 0.6330(3) 0.0298(13) Uani 1 1 d . . . C84 C 0.4039(4) 0.4525(4) 0.4556(3) 0.0381(15) Uani 1 1 d . . . C85 C 0.2276(3) 0.4166(5) 0.6375(3) 0.0338(14) Uani 1 1 d . . . C86 C 0.3565(3) -0.1835(4) 0.6935(3) 0.0341(13) Uani 1 1 d . . . C87 C 0.2928(3) -0.2133(4) 0.7192(3) 0.0359(13) Uani 1 1 d . . . H87 H 0.2603 -0.1699 0.7335 0.043 Uiso 1 1 calc R . . C88 C 0.2776(3) -0.3071(4) 0.7236(3) 0.0356(13) Uani 1 1 d . . . C89 C 0.3255(3) -0.3710(5) 0.6990(3) 0.0364(14) Uani 1 1 d . . . H89 H 0.3151 -0.4341 0.7007 0.044 Uiso 1 1 calc R . . C90 C 0.3884(3) -0.3417(4) 0.6720(3) 0.0353(13) Uani 1 1 d . . . C91 C 0.4035(3) -0.2479(4) 0.6700(3) 0.0359(13) Uani 1 1 d . . . H91 H 0.4458 -0.2279 0.6526 0.043 Uiso 1 1 calc R . . C92 C 0.3769(3) -0.0825(4) 0.6931(3) 0.0353(13) Uani 1 1 d . . . C93 C 0.2091(3) -0.3405(5) 0.7555(3) 0.0417(15) Uani 1 1 d . . . C94 C 0.4397(3) -0.4112(5) 0.6478(3) 0.0390(13) Uani 1 1 d . . . C95 C 0.1987(3) 0.1601(5) 0.8784(3) 0.0333(14) Uani 1 1 d . . . C96 C 0.1668(3) 0.2431(4) 0.8541(3) 0.0314(13) Uani 1 1 d . . . H96 H 0.1840 0.2749 0.8166 0.038 Uiso 1 1 calc R . . C97 C 0.1085(3) 0.2789(4) 0.8862(3) 0.0307(13) Uani 1 1 d . . . C98 C 0.0822(3) 0.2283(4) 0.9405(3) 0.0295(13) Uani 1 1 d . . . H98 H 0.0431 0.2518 0.9615 0.035 Uiso 1 1 calc R . . C99 C 0.1123(3) 0.1445(5) 0.9640(3) 0.0351(13) Uani 1 1 d . . . C100 C 0.1724(3) 0.1098(5) 0.9328(3) 0.0373(14) Uani 1 1 d . . . H100 H 0.1942 0.0539 0.9484 0.045 Uiso 1 1 calc R . . C101 C 0.2654(3) 0.1244(5) 0.8465(3) 0.0406(16) Uani 1 1 d . . . C102 C 0.0786(3) 0.3741(4) 0.8667(3) 0.0308(13) Uani 1 1 d . . . C103 C 0.0862(3) 0.0938(5) 1.0261(3) 0.0390(15) Uani 1 1 d . . . O30 O 0.0173(18) 0.902(2) 0.9047(12) 0.251(17) Uani 0.50 1 d P A 1 O30' O -0.0042(14) 0.8283(17) 0.8435(7) 0.217(15) Uani 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02832(19) 0.0253(2) 0.02616(19) -0.00090(18) 0.00232(14) 0.00141(18) Cd2 0.0350(2) 0.0281(2) 0.0265(2) 0.00090(17) 0.00827(16) 0.00364(18) Cd3 0.0324(2) 0.0293(2) 0.0305(2) 0.00092(18) 0.00526(16) 0.00206(18) Cd4 0.0342(2) 0.0312(2) 0.0327(2) -0.0050(2) 0.00416(16) 0.0042(2) Ni1 0.0312(4) 0.0801(7) 0.0306(4) -0.0123(4) -0.0029(3) 0.0041(4) Ni2 0.0376(4) 0.0332(4) 0.0309(4) 0.0014(3) -0.0016(3) 0.0059(3) Ni3 0.0362(4) 0.0776(7) 0.0274(4) -0.0041(4) 0.0022(3) -0.0137(4) Ni4 0.0347(4) 0.0462(5) 0.0281(3) 0.0023(4) -0.0004(3) 0.0037(4) O1 0.046(2) 0.035(3) 0.041(2) -0.003(2) -0.012(2) 0.001(2) O2 0.043(2) 0.044(3) 0.040(2) 0.007(2) -0.0073(19) -0.001(2) O3 0.063(3) 0.025(2) 0.034(2) 0.004(2) -0.009(2) 0.004(2) O4 0.047(2) 0.026(2) 0.035(2) -0.0061(19) -0.0010(19) 0.003(2) O5 0.046(2) 0.040(3) 0.036(2) -0.001(2) -0.0072(19) 0.006(2) O6 0.057(3) 0.034(3) 0.055(3) 0.005(2) -0.010(2) -0.001(2) O7 0.048(3) 0.032(3) 0.038(2) 0.003(2) -0.006(2) -0.004(2) O8 0.042(2) 0.029(2) 0.035(2) -0.003(2) -0.0008(18) 0.002(2) O9 0.051(2) 0.035(3) 0.029(2) -0.0019(19) 0.0018(18) 0.017(2) O10 0.043(2) 0.051(3) 0.042(2) 0.022(2) 0.0093(19) 0.006(2) O11 0.042(2) 0.039(3) 0.040(2) 0.011(2) 0.0174(19) 0.012(2) O12 0.047(2) 0.047(3) 0.042(2) 0.010(2) 0.0134(19) 0.024(2) O13 0.063(3) 0.057(4) 0.058(3) 0.038(3) 0.019(2) 0.012(3) O14 0.050(3) 0.055(3) 0.044(2) 0.020(2) 0.025(2) 0.005(2) O15 0.055(3) 0.046(3) 0.058(3) 0.000(2) 0.027(2) -0.018(2) O16 0.045(2) 0.033(3) 0.066(3) -0.006(2) 0.002(2) 0.002(2) O17 0.053(3) 0.066(4) 0.091(4) -0.005(3) 0.035(3) -0.010(3) O18 0.064(3) 0.044(3) 0.051(3) -0.001(2) 0.004(2) -0.028(2) O19 0.060(3) 0.049(3) 0.067(3) -0.002(3) 0.015(2) 0.009(2) O20 0.100(4) 0.057(4) 0.104(5) 0.017(4) 0.062(4) 0.025(3) O21 0.081(4) 0.078(4) 0.091(4) 0.042(4) 0.057(3) 0.056(3) O22 0.041(2) 0.038(3) 0.059(3) 0.002(2) 0.028(2) 0.004(2) O23 0.057(3) 0.063(4) 0.053(3) 0.033(3) 0.021(2) 0.012(3) O24 0.050(2) 0.042(3) 0.038(2) 0.002(2) -0.003(2) 0.016(2) O25 0.100(4) 0.057(4) 0.079(4) 0.026(3) 0.069(3) 0.024(3) O26 0.074(3) 0.071(4) 0.078(4) 0.041(4) 0.038(3) 0.019(3) O27 0.056(3) 0.075(4) 0.046(3) -0.005(3) 0.019(2) -0.023(3) O28 0.098(5) 0.153(8) 0.110(6) 0.021(6) -0.011(4) -0.018(5) O29 0.139(6) 0.080(6) 0.178(9) 0.024(6) 0.080(6) -0.002(5) N1 0.030(3) 0.055(4) 0.030(3) -0.012(2) 0.000(2) 0.000(2) N2 0.035(3) 0.062(4) 0.034(3) 0.000(3) -0.002(2) 0.008(3) N3 0.046(3) 0.121(7) 0.036(3) -0.024(4) -0.008(3) 0.020(4) N4 0.035(3) 0.109(7) 0.047(4) -0.028(4) 0.002(3) -0.008(4) N5 0.040(3) 0.029(3) 0.030(3) 0.000(2) -0.003(2) 0.000(2) N6 0.036(3) 0.031(3) 0.030(2) 0.000(2) 0.005(2) 0.007(2) N7 0.094(5) 0.040(4) 0.045(3) 0.010(3) -0.002(3) 0.020(4) N8 0.066(4) 0.050(4) 0.040(3) 0.002(3) -0.008(3) 0.004(3) N9 0.039(3) 0.045(3) 0.031(3) -0.007(2) 0.006(2) -0.008(2) N10 0.031(3) 0.065(4) 0.040(3) 0.013(3) 0.001(2) -0.003(3) N11 0.034(3) 0.151(8) 0.030(3) 0.008(4) 0.001(2) -0.023(4) N12 0.042(3) 0.113(7) 0.031(3) -0.037(4) 0.010(2) -0.027(4) N13 0.036(3) 0.038(3) 0.027(2) -0.003(2) -0.001(2) -0.002(2) N14 0.038(3) 0.037(3) 0.026(2) 0.001(2) 0.002(2) 0.010(2) N15 0.073(4) 0.072(5) 0.043(3) 0.007(3) -0.005(3) 0.018(4) N16 0.079(4) 0.078(6) 0.032(3) 0.000(3) -0.008(3) 0.012(4) C1 0.027(3) 0.044(4) 0.031(3) -0.007(3) 0.006(2) 0.002(3) C2 0.029(3) 0.056(4) 0.026(3) -0.001(3) 0.002(2) 0.000(3) C3 0.043(4) 0.082(7) 0.043(4) 0.013(4) -0.005(3) 0.015(4) C4 0.062(5) 0.070(6) 0.068(5) 0.003(5) -0.014(4) 0.019(5) C5 0.076(6) 0.068(7) 0.094(7) 0.015(5) -0.009(5) 0.026(5) C6 0.103(5) 0.099(5) 0.099(5) 0.010(4) 0.004(4) 0.022(4) C7 0.101(7) 0.123(10) 0.066(6) 0.022(7) -0.024(5) 0.049(7) C8 0.069(5) 0.110(8) 0.042(4) 0.007(5) -0.017(4) 0.037(5) C9 0.071(6) 0.137(11) 0.041(4) 0.002(6) -0.012(4) 0.046(7) C10 0.080(6) 0.145(10) 0.034(4) -0.031(5) -0.009(4) 0.019(6) C11 0.079(4) 0.101(5) 0.069(4) -0.016(4) -0.014(4) -0.002(4) C12 0.033(4) 0.158(11) 0.072(6) -0.039(7) -0.010(4) -0.004(5) C13 0.052(5) 0.105(8) 0.058(5) -0.044(6) 0.026(4) -0.032(5) C14 0.042(4) 0.071(6) 0.051(4) -0.026(4) 0.020(3) -0.016(4) C15 0.075(6) 0.067(6) 0.091(6) -0.039(5) 0.045(5) -0.033(5) C16 0.090(7) 0.046(6) 0.111(8) -0.028(5) 0.040(6) -0.008(5) C17 0.075(5) 0.044(5) 0.081(6) -0.005(4) 0.011(4) 0.009(4) C18 0.065(5) 0.045(4) 0.054(4) -0.012(4) 0.006(4) -0.005(4) C19 0.048(4) 0.051(4) 0.041(4) -0.012(3) 0.019(3) -0.007(3) C20 0.040(3) 0.033(3) 0.024(3) -0.001(3) 0.008(2) 0.003(3) C21 0.040(3) 0.027(3) 0.027(3) 0.001(2) 0.010(2) -0.001(3) C22 0.038(3) 0.028(3) 0.045(4) -0.004(3) 0.006(3) 0.005(3) C23 0.062(4) 0.041(4) 0.052(4) -0.007(3) -0.001(3) 0.015(4) C24 0.088(6) 0.045(5) 0.071(5) -0.025(4) 0.002(5) 0.012(4) C25 0.084(6) 0.040(5) 0.083(6) -0.018(4) 0.004(5) 0.017(4) C26 0.065(5) 0.031(4) 0.072(5) 0.001(4) 0.006(4) 0.016(4) C27 0.045(4) 0.041(4) 0.047(4) 0.000(3) 0.011(3) 0.006(3) C28 0.089(6) 0.044(5) 0.050(4) 0.009(4) -0.002(4) 0.012(4) C29 0.091(6) 0.059(6) 0.075(6) 0.011(5) -0.040(5) 0.008(5) C30 0.114(7) 0.057(5) 0.043(4) 0.011(4) -0.011(4) 0.019(5) C31 0.087(6) 0.084(7) 0.041(4) 0.011(4) 0.016(4) -0.002(5) C32 0.064(4) 0.061(5) 0.037(4) -0.002(4) -0.010(3) -0.002(4) C33 0.053(4) 0.036(4) 0.040(4) -0.002(3) -0.001(3) 0.003(3) C34 0.052(4) 0.052(5) 0.049(4) -0.017(4) -0.009(3) 0.006(4) C35 0.051(4) 0.037(4) 0.060(4) -0.015(4) 0.011(3) -0.006(3) C36 0.059(4) 0.034(4) 0.059(4) -0.004(3) 0.025(4) -0.004(3) C37 0.050(4) 0.037(4) 0.040(4) 0.000(3) 0.013(3) 0.000(3) C38 0.035(3) 0.033(4) 0.041(3) -0.010(3) 0.008(3) -0.003(3) C39 0.030(3) 0.042(4) 0.031(3) 0.000(3) 0.008(2) 0.001(3) C40 0.027(3) 0.045(4) 0.029(3) 0.005(3) 0.002(2) 0.004(3) C41 0.027(3) 0.081(7) 0.066(5) 0.038(5) 0.005(3) 0.004(4) C42 0.045(4) 0.073(7) 0.117(8) 0.052(7) 0.014(5) 0.021(4) C43 0.059(5) 0.096(9) 0.157(11) 0.076(8) 0.009(6) 0.023(6) C44 0.084(5) 0.100(5) 0.108(5) 0.032(4) 0.001(4) 0.010(4) C45 0.080(4) 0.103(5) 0.091(5) 0.027(4) -0.003(4) 0.002(4) C46 0.045(4) 0.120(9) 0.078(6) 0.067(7) -0.010(4) -0.004(5) C47 0.038(4) 0.181(14) 0.046(5) 0.046(7) -0.010(3) -0.011(6) C48 0.058(5) 0.204(14) 0.030(4) -0.020(6) 0.007(3) -0.021(6) C49 0.053(5) 0.179(13) 0.052(5) -0.031(6) -0.004(4) -0.030(6) C50 0.043(4) 0.149(10) 0.053(5) -0.039(6) 0.001(3) -0.035(5) C51 0.065(5) 0.079(7) 0.064(5) -0.030(5) 0.033(4) -0.033(5) C52 0.056(4) 0.056(5) 0.051(4) -0.020(4) 0.027(3) -0.016(4) C53 0.098(7) 0.045(5) 0.098(7) -0.032(5) 0.059(6) -0.035(5) C54 0.128(9) 0.043(5) 0.101(7) -0.014(6) 0.055(7) 0.002(6) C55 0.108(7) 0.040(5) 0.077(6) -0.009(4) 0.021(5) 0.017(5) C56 0.077(5) 0.044(5) 0.053(4) -0.007(4) 0.014(4) -0.002(4) C57 0.071(5) 0.036(4) 0.036(3) -0.011(3) 0.025(3) -0.006(4) C58 0.034(3) 0.032(3) 0.025(3) -0.002(2) 0.004(2) -0.004(3) C59 0.027(3) 0.033(4) 0.031(3) -0.002(2) 0.007(2) -0.001(2) C60 0.037(3) 0.047(4) 0.044(4) 0.009(3) 0.009(3) 0.006(3) C61 0.060(4) 0.038(4) 0.047(4) 0.001(3) 0.005(3) 0.012(3) C62 0.072(5) 0.040(4) 0.060(5) -0.007(4) 0.000(4) 0.011(4) C63 0.080(6) 0.031(4) 0.088(6) 0.006(4) 0.007(5) 0.017(4) C64 0.059(4) 0.039(4) 0.060(5) 0.010(4) 0.005(4) 0.010(4) C65 0.045(4) 0.041(4) 0.054(4) 0.006(3) 0.004(3) 0.007(3) C66 0.097(6) 0.057(6) 0.048(5) 0.023(4) 0.003(4) 0.028(5) C67 0.085(4) 0.102(5) 0.078(4) -0.002(4) -0.016(4) 0.019(4) C68 0.139(9) 0.101(8) 0.042(4) 0.007(5) -0.013(5) 0.041(8) C69 0.081(6) 0.165(12) 0.043(4) 0.030(6) 0.008(4) 0.017(7) C70 0.071(5) 0.079(7) 0.046(4) -0.020(4) -0.022(4) 0.007(5) C71 0.036(3) 0.057(5) 0.042(4) -0.014(3) -0.007(3) 0.002(3) C72 0.043(4) 0.064(6) 0.071(5) -0.044(5) -0.005(4) 0.000(4) C73 0.054(4) 0.053(5) 0.079(6) -0.030(5) 0.022(4) -0.014(4) C74 0.066(5) 0.035(4) 0.065(5) -0.017(4) 0.023(4) -0.009(4) C75 0.044(4) 0.046(4) 0.041(3) -0.012(3) 0.015(3) -0.011(3) C76 0.031(3) 0.042(4) 0.036(3) -0.015(3) 0.009(3) -0.007(3) C77 0.023(3) 0.025(3) 0.025(3) 0.001(2) -0.001(2) 0.003(2) C78 0.028(3) 0.033(3) 0.025(3) -0.002(2) 0.006(2) -0.001(2) C79 0.029(3) 0.028(3) 0.026(3) 0.002(2) 0.003(2) -0.001(2) C80 0.035(3) 0.026(3) 0.027(3) 0.003(2) 0.002(2) 0.007(2) C81 0.028(3) 0.028(3) 0.030(3) 0.002(2) 0.003(2) 0.007(2) C82 0.032(3) 0.033(3) 0.024(3) 0.001(2) 0.006(2) 0.001(3) C83 0.024(3) 0.031(3) 0.033(3) 0.006(3) 0.000(2) -0.004(2) C84 0.054(4) 0.028(3) 0.033(3) 0.002(3) 0.010(3) -0.007(3) C85 0.038(3) 0.031(3) 0.034(3) -0.009(3) 0.011(3) 0.003(3) C86 0.040(3) 0.032(3) 0.029(3) 0.002(3) 0.001(2) -0.008(3) C87 0.035(3) 0.037(4) 0.035(3) -0.010(3) 0.001(2) -0.007(3) C88 0.037(3) 0.043(4) 0.026(3) -0.002(3) 0.002(2) -0.012(3) C89 0.042(3) 0.031(3) 0.033(3) 0.000(3) -0.006(3) -0.008(3) C90 0.044(3) 0.035(3) 0.025(3) -0.001(2) -0.004(2) -0.001(3) C91 0.037(3) 0.041(4) 0.030(3) -0.002(3) 0.005(2) -0.009(3) C92 0.043(3) 0.031(3) 0.030(3) -0.007(3) 0.001(3) -0.007(3) C93 0.041(3) 0.047(4) 0.037(3) -0.009(3) 0.006(3) -0.014(3) C94 0.050(3) 0.033(4) 0.033(3) -0.005(3) -0.001(3) 0.002(3) C95 0.038(3) 0.035(4) 0.029(3) -0.003(3) 0.011(2) 0.001(3) C96 0.035(3) 0.034(4) 0.027(3) 0.002(2) 0.010(2) -0.002(3) C97 0.030(3) 0.036(4) 0.026(3) -0.004(3) 0.003(2) -0.004(3) C98 0.026(3) 0.036(4) 0.028(3) -0.004(3) 0.009(2) -0.002(3) C99 0.042(3) 0.032(3) 0.033(3) 0.000(3) 0.011(2) -0.006(3) C100 0.043(3) 0.034(4) 0.037(3) -0.001(3) 0.011(3) 0.008(3) C101 0.046(4) 0.043(4) 0.035(3) 0.004(3) 0.015(3) 0.008(3) C102 0.023(3) 0.034(3) 0.035(3) -0.001(3) 0.001(2) 0.002(2) C103 0.038(3) 0.044(4) 0.037(3) 0.005(3) 0.009(3) -0.007(3) O30 0.40(4) 0.22(3) 0.122(17) -0.016(18) -0.04(2) 0.21(3) O30' 0.36(3) 0.25(3) 0.029(6) -0.012(10) -0.018(11) 0.26(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 Cd1 O9 2.228(4) . ? Cd1 O15 2.246(4) . ? Cd1 O14 2.262(4) 2_646 ? Cd1 O2 2.269(4) . ? Cd1 O1 2.376(4) . ? Cd1 O13 2.567(5) 2_646 ? Cd2 O16 2.193(5) . ? Cd2 O10 2.225(4) . ? Cd2 O22 2.237(4) . ? Cd2 O3 2.303(4) . ? Cd2 O4 2.314(4) . ? Cd2 O21 2.521(5) . ? Cd2 C101 2.704(6) . ? Cd3 O23 2.198(4) . ? Cd3 O18 2.227(4) 1_565 ? Cd3 O11 2.257(4) . ? Cd3 O8 2.259(4) . ? Cd3 O7 2.317(4) . ? Cd3 O12 2.428(4) . ? Cd3 C85 2.661(5) . ? Cd4 O24 2.211(4) . ? Cd4 O6 2.267(5) . ? Cd4 O25 2.270(5) 2_557 ? Cd4 O27 2.297(5) . ? Cd4 O5 2.396(5) . ? Cd4 O26 2.529(5) 2_557 ? Cd4 C103 2.749(6) 2_557 ? Ni1 N2 1.878(7) . ? Ni1 N4 1.880(8) . ? Ni1 N1 1.888(5) . ? Ni1 N3 1.892(8) . ? Ni2 N7 1.863(6) . ? Ni2 N6 1.880(5) . ? Ni2 N5 1.881(5) . ? Ni2 N8 1.908(6) . ? Ni3 N11 1.863(7) . ? Ni3 N9 1.876(5) . ? Ni3 N12 1.888(8) . ? Ni3 N10 1.893(7) . ? Ni4 N15 1.867(7) . ? Ni4 N13 1.893(5) . ? Ni4 N14 1.903(5) . ? Ni4 N16 1.912(7) . ? O1 C1 1.246(7) . ? O2 C2 1.253(8) . ? O3 C20 1.250(8) . ? O4 C21 1.220(7) . ? O5 C39 1.256(7) . ? O6 C40 1.246(8) . ? O7 C58 1.240(7) . ? O8 C59 1.235(7) . ? O9 C83 1.269(7) . ? O10 C83 1.245(7) . ? O11 C85 1.264(7) . ? O12 C85 1.222(8) . ? O13 C84 1.227(8) . ? O13 Cd1 2.567(5) 2_656 ? O14 C84 1.272(7) . ? O14 Cd1 2.262(4) 2_656 ? O15 C92 1.239(7) . ? O16 C92 1.269(7) . ? O17 C93 1.238(9) . ? O18 C93 1.248(8) . ? O18 Cd3 2.227(4) 1_545 ? O19 C94 1.192(8) . ? O20 C94 1.309(8) . ? O20 H20 0.8200 . ? O21 C101 1.244(9) . ? O22 C101 1.243(8) . ? O23 C102 1.251(7) . ? O24 C102 1.249(7) . ? O25 C103 1.236(8) . ? O25 Cd4 2.270(5) 2_547 ? O26 C103 1.220(9) . ? O26 Cd4 2.529(5) 2_547 ? O27 H27A 0.8676 . ? O27 H27B 0.8716 . ? N1 C1 1.352(8) . ? N1 C19 1.414(9) . ? N2 C2 1.321(7) . ? N2 C3 1.423(11) . ? N3 C9 1.292(14) . ? N3 C10 1.518(11) . ? N4 C13 1.269(13) . ? N4 C12 1.475(10) . ? N5 C20 1.346(8) . ? N5 C38 1.403(8) . ? N6 C21 1.361(8) . ? N6 C22 1.388(8) . ? N7 C28 1.270(10) . ? N7 C29 1.533(10) . ? N8 C32 1.287(10) . ? N8 C31 1.498(10) . ? N9 C39 1.327(8) . ? N9 C57 1.425(9) . ? N10 C40 1.334(8) . ? N10 C41 1.408(10) . ? N11 C47 1.268(16) . ? N11 C48 1.472(13) . ? N12 C51 1.303(12) . ? N12 C50 1.491(10) . ? N13 C58 1.338(7) . ? N13 C76 1.394(9) . ? N14 C59 1.339(8) . ? N14 C60 1.401(9) . ? N15 C66 1.292(12) . ? N15 C67 1.559(11) . ? N16 C70 1.294(12) . ? N16 C69 1.504(11) . ? C1 C2 1.501(9) . ? C3 C4 1.365(13) . ? C3 C8 1.415(10) . ? C4 C5 1.359(13) . ? C4 H4 0.9300 . ? C5 C6 1.318(14) . ? C5 H5 0.9300 . ? C6 C7 1.370(17) . ? C6 H6 0.9300 . ? C7 C8 1.385(16) . ? C7 H7 0.9300 . ? C8 C9 1.394(15) . ? C9 H9 0.9300 . ? C10 C11 1.554(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.535(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.466(13) . ? C13 H13 0.9300 . ? C14 C15 1.411(13) . ? C14 C19 1.423(10) . ? C15 C16 1.343(14) . ? C15 H15 0.9300 . ? C16 C17 1.350(13) . ? C16 H16 0.9300 . ? C17 C18 1.377(12) . ? C17 H17 0.9300 . ? C18 C19 1.383(10) . ? C18 H18 0.9300 . ? C20 C21 1.520(9) . ? C22 C23 1.407(9) . ? C22 C27 1.412(9) . ? C23 C24 1.386(11) . ? C23 H23 0.9300 . ? C24 C25 1.376(12) . ? C24 H24 0.9300 . ? C25 C26 1.375(12) . ? C25 H25 0.9300 . ? C26 C27 1.408(11) . ? C26 H26 0.9300 . ? C27 C28 1.437(11) . ? C28 H28 0.9300 . ? C29 C30 1.447(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.528(12) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.476(11) . ? C32 H32 0.9300 . ? C33 C34 1.399(10) . ? C33 C38 1.415(9) . ? C34 C35 1.360(11) . ? C34 H34 0.9300 . ? C35 C36 1.383(11) . ? C35 H35 0.9300 . ? C36 C37 1.380(10) . ? C36 H36 0.9300 . ? C37 C38 1.400(10) . ? C37 H37 0.9300 . ? C39 C40 1.528(9) . ? C41 C42 1.381(14) . ? C41 C46 1.412(12) . ? C42 C43 1.414(13) . ? C42 H42 0.9300 . ? C43 C44 1.379(17) . ? C43 H43 0.9300 . ? C44 C45 1.330(17) . ? C44 H44 0.9300 . ? C45 C46 1.407(14) . ? C45 H45 0.9300 . ? C46 C47 1.437(17) . ? C47 H47 0.9300 . ? C48 C49 1.515(13) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.516(11) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.401(12) . ? C51 H51 0.9300 . ? C52 C57 1.417(10) . ? C52 C53 1.425(13) . ? C53 C54 1.351(14) . ? C53 H53 0.9300 . ? C54 C55 1.371(14) . ? C54 H54 0.9300 . ? C55 C56 1.386(12) . ? C55 H55 0.9300 . ? C56 C57 1.385(11) . ? C56 H56 0.9300 . ? C58 C59 1.516(9) . ? C60 C61 1.397(10) . ? C60 C65 1.428(10) . ? C61 C62 1.374(11) . ? C61 H61 0.9300 . ? C62 C63 1.390(11) . ? C62 H62 0.9300 . ? C63 C64 1.360(12) . ? C63 H63 0.9300 . ? C64 C65 1.386(11) . ? C64 H64 0.9300 . ? C65 C66 1.427(12) . ? C66 H66 0.9300 . ? C67 C68 1.479(14) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.464(14) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.396(12) . ? C70 H70 0.9300 . ? C71 C76 1.418(9) . ? C71 C72 1.418(11) . ? C72 C73 1.354(12) . ? C72 H72 0.9300 . ? C73 C74 1.355(11) . ? C73 H73 0.9300 . ? C74 C75 1.371(10) . ? C74 H74 0.9300 . ? C75 C76 1.411(10) . ? C75 H75 0.9300 . ? C77 C82 1.381(8) . ? C77 C78 1.407(8) . ? C77 C83 1.495(8) . ? C78 C79 1.381(8) . ? C78 H78 0.9300 . ? C79 C80 1.390(8) . ? C79 C84 1.514(8) . ? C80 C81 1.385(8) . ? C80 H80 0.9300 . ? C81 C82 1.391(8) . ? C81 C85 1.512(7) . ? C82 H82 0.9300 . ? C86 C91 1.379(9) . ? C86 C87 1.393(8) . ? C86 C92 1.503(9) . ? C87 C88 1.384(9) . ? C87 H87 0.9300 . ? C88 C89 1.393(9) . ? C88 C93 1.542(8) . ? C89 C90 1.389(8) . ? C89 H89 0.9300 . ? C90 C91 1.380(9) . ? C90 C94 1.489(9) . ? C91 H91 0.9300 . ? C95 C96 1.384(9) . ? C95 C100 1.390(8) . ? C95 C101 1.525(8) . ? C96 C97 1.397(8) . ? C96 H96 0.9300 . ? C97 C98 1.391(8) . ? C97 C102 1.504(9) . ? C98 C99 1.377(9) . ? C98 H98 0.9300 . ? C99 C100 1.409(8) . ? C99 C103 1.508(8) . ? C100 H100 0.9300 . ? C103 Cd4 2.749(6) 2_547 ? 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 O9 Cd1 O15 103.58(18) . . ? O9 Cd1 O14 97.91(17) . 2_646 ? O15 Cd1 O14 83.20(17) . 2_646 ? O9 Cd1 O2 149.05(18) . . ? O15 Cd1 O2 91.60(18) . . ? O14 Cd1 O2 110.72(19) 2_646 . ? O9 Cd1 O1 80.52(16) . . ? O15 Cd1 O1 132.39(17) . . ? O14 Cd1 O1 144.01(16) 2_646 . ? O2 Cd1 O1 69.48(17) . . ? O9 Cd1 O13 98.95(17) . 2_646 ? O15 Cd1 O13 133.20(17) . 2_646 ? O14 Cd1 O13 53.18(15) 2_646 2_646 ? O2 Cd1 O13 89.41(17) . 2_646 ? O1 Cd1 O13 91.28(16) . 2_646 ? O16 Cd2 O10 96.21(19) . . ? O16 Cd2 O22 104.00(17) . . ? O10 Cd2 O22 99.03(17) . . ? O16 Cd2 O3 156.44(17) . . ? O10 Cd2 O3 91.42(17) . . ? O22 Cd2 O3 96.72(17) . . ? O16 Cd2 O4 85.59(16) . . ? O10 Cd2 O4 119.16(15) . . ? O22 Cd2 O4 139.60(16) . . ? O3 Cd2 O4 71.27(15) . . ? O16 Cd2 O21 86.8(2) . . ? O10 Cd2 O21 152.84(16) . . ? O22 Cd2 O21 54.32(17) . . ? O3 Cd2 O21 96.5(2) . . ? O4 Cd2 O21 87.95(16) . . ? O16 Cd2 C101 96.14(19) . . ? O10 Cd2 C101 125.95(19) . . ? O22 Cd2 C101 27.07(19) . . ? O3 Cd2 C101 97.32(19) . . ? O4 Cd2 C101 114.12(18) . . ? O21 Cd2 C101 27.25(19) . . ? O23 Cd3 O18 100.3(2) . 1_565 ? O23 Cd3 O11 99.95(17) . . ? O18 Cd3 O11 90.85(18) 1_565 . ? O23 Cd3 O8 111.55(16) . . ? O18 Cd3 O8 95.60(18) 1_565 . ? O11 Cd3 O8 146.03(14) . . ? O23 Cd3 O7 91.44(19) . . ? O18 Cd3 O7 165.27(17) 1_565 . ? O11 Cd3 O7 95.94(17) . . ? O8 Cd3 O7 71.60(16) . . ? O23 Cd3 O12 155.07(18) . . ? O18 Cd3 O12 85.65(17) 1_565 . ? O11 Cd3 O12 55.50(15) . . ? O8 Cd3 O12 91.72(15) . . ? O7 Cd3 O12 87.46(16) . . ? O23 Cd3 C85 128.2(2) . . ? O18 Cd3 C85 86.30(19) 1_565 . ? O11 Cd3 C85 28.29(18) . . ? O8 Cd3 C85 118.86(18) . . ? O7 Cd3 C85 93.50(18) . . ? O12 Cd3 C85 27.30(18) . . ? O24 Cd4 O6 143.25(18) . . ? O24 Cd4 O25 102.9(2) . 2_557 ? O6 Cd4 O25 112.8(2) . 2_557 ? O24 Cd4 O27 110.74(19) . . ? O6 Cd4 O27 84.59(18) . . ? O25 Cd4 O27 80.21(19) 2_557 . ? O24 Cd4 O5 77.03(16) . . ? O6 Cd4 O5 69.60(16) . . ? O25 Cd4 O5 141.99(17) 2_557 . ? O27 Cd4 O5 136.17(17) . . ? O24 Cd4 O26 96.4(2) . 2_557 ? O6 Cd4 O26 98.1(2) . 2_557 ? O25 Cd4 O26 52.66(18) 2_557 2_557 ? O27 Cd4 O26 130.1(2) . 2_557 ? O5 Cd4 O26 89.37(17) . 2_557 ? O24 Cd4 C103 101.09(18) . 2_557 ? O6 Cd4 C103 106.81(18) . 2_557 ? O25 Cd4 C103 26.37(19) 2_557 2_557 ? O27 Cd4 C103 105.3(2) . 2_557 ? O5 Cd4 C103 115.66(18) . 2_557 ? O26 Cd4 C103 26.29(19) 2_557 2_557 ? N2 Ni1 N4 163.8(3) . . ? N2 Ni1 N1 86.8(2) . . ? N4 Ni1 N1 93.7(3) . . ? N2 Ni1 N3 92.2(3) . . ? N4 Ni1 N3 91.7(4) . . ? N1 Ni1 N3 163.6(2) . . ? N7 Ni2 N6 94.8(3) . . ? N7 Ni2 N5 172.0(3) . . ? N6 Ni2 N5 86.4(2) . . ? N7 Ni2 N8 89.4(3) . . ? N6 Ni2 N8 163.4(2) . . ? N5 Ni2 N8 91.8(2) . . ? N11 Ni3 N9 163.1(3) . . ? N11 Ni3 N12 90.2(4) . . ? N9 Ni3 N12 93.7(3) . . ? N11 Ni3 N10 94.0(3) . . ? N9 Ni3 N10 86.8(2) . . ? N12 Ni3 N10 163.9(2) . . ? N15 Ni4 N13 171.9(3) . . ? N15 Ni4 N14 94.6(3) . . ? N13 Ni4 N14 85.5(2) . . ? N15 Ni4 N16 90.8(3) . . ? N13 Ni4 N16 91.0(3) . . ? N14 Ni4 N16 165.9(3) . . ? C1 O1 Cd1 116.1(4) . . ? C2 O2 Cd1 119.6(4) . . ? C20 O3 Cd2 114.8(4) . . ? C21 O4 Cd2 116.7(4) . . ? C39 O5 Cd4 116.2(4) . . ? C40 O6 Cd4 120.1(4) . . ? C58 O7 Cd3 113.4(4) . . ? C59 O8 Cd3 116.2(4) . . ? C83 O9 Cd1 108.4(4) . . ? C83 O10 Cd2 155.2(4) . . ? C85 O11 Cd3 93.9(4) . . ? C85 O12 Cd3 87.0(4) . . ? C84 O13 Cd1 86.1(4) . 2_656 ? C84 O14 Cd1 99.4(4) . 2_656 ? C92 O15 Cd1 154.0(5) . . ? C92 O16 Cd2 110.9(4) . . ? C93 O18 Cd3 132.2(4) . 1_545 ? C94 O20 H20 109.5 . . ? C101 O21 Cd2 84.6(4) . . ? C101 O22 Cd2 97.9(4) . . ? C102 O23 Cd3 167.1(4) . . ? C102 O24 Cd4 108.4(4) . . ? C103 O25 Cd4 99.0(5) . 2_547 ? C103 O26 Cd4 87.0(4) . 2_547 ? Cd4 O27 H27A 100.5 . . ? Cd4 O27 H27B 115.0 . . ? H27A O27 H27B 119.4 . . ? C1 N1 C19 120.2(5) . . ? C1 N1 Ni1 111.6(5) . . ? C19 N1 Ni1 128.1(4) . . ? C2 N2 C3 120.1(7) . . ? C2 N2 Ni1 113.4(6) . . ? C3 N2 Ni1 126.2(4) . . ? C9 N3 C10 119.8(8) . . ? C9 N3 Ni1 126.4(6) . . ? C10 N3 Ni1 113.3(7) . . ? C13 N4 C12 115.2(9) . . ? C13 N4 Ni1 127.6(6) . . ? C12 N4 Ni1 116.8(8) . . ? C20 N5 C38 122.3(6) . . ? C20 N5 Ni2 111.5(4) . . ? C38 N5 Ni2 126.1(4) . . ? C21 N6 C22 120.0(5) . . ? C21 N6 Ni2 110.2(4) . . ? C22 N6 Ni2 128.3(4) . . ? C28 N7 C29 116.2(7) . . ? C28 N7 Ni2 126.4(6) . . ? C29 N7 Ni2 117.1(5) . . ? C32 N8 C31 119.2(7) . . ? C32 N8 Ni2 124.9(5) . . ? C31 N8 Ni2 114.8(5) . . ? C39 N9 C57 120.8(5) . . ? C39 N9 Ni3 113.3(4) . . ? C57 N9 Ni3 125.8(4) . . ? C40 N10 C41 120.4(7) . . ? C40 N10 Ni3 112.7(5) . . ? C41 N10 Ni3 126.0(5) . . ? C47 N11 C48 117.8(9) . . ? C47 N11 Ni3 125.2(8) . . ? C48 N11 Ni3 116.4(8) . . ? C51 N12 C50 118.8(8) . . ? C51 N12 Ni3 126.5(6) . . ? C50 N12 Ni3 114.3(7) . . ? C58 N13 C76 122.2(6) . . ? C58 N13 Ni4 111.5(4) . . ? C76 N13 Ni4 126.2(4) . . ? C59 N14 C60 121.1(5) . . ? C59 N14 Ni4 110.6(4) . . ? C60 N14 Ni4 127.3(4) . . ? C66 N15 C67 118.9(8) . . ? C66 N15 Ni4 126.4(6) . . ? C67 N15 Ni4 114.2(7) . . ? C70 N16 C69 119.2(8) . . ? C70 N16 Ni4 125.6(6) . . ? C69 N16 Ni4 114.4(7) . . ? O1 C1 N1 128.5(6) . . ? O1 C1 C2 117.3(6) . . ? N1 C1 C2 114.2(5) . . ? O2 C2 N2 128.9(7) . . ? O2 C2 C1 117.3(5) . . ? N2 C2 C1 113.8(6) . . ? C4 C3 C8 117.0(9) . . ? C4 C3 N2 124.8(7) . . ? C8 C3 N2 118.1(8) . . ? C5 C4 C3 122.7(9) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C6 C5 C4 121.8(12) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 117.5(12) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C6 C7 C8 123.6(9) . . ? C6 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 118.6(8) . . ? C7 C8 C3 117.2(10) . . ? C9 C8 C3 124.2(10) . . ? N3 C9 C8 126.3(9) . . ? N3 C9 H9 116.9 . . ? C8 C9 H9 116.9 . . ? N3 C10 C11 111.0(7) . . ? N3 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N3 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 111.9(7) . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11B 109.2 . . ? C10 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N4 C12 C11 111.1(7) . . ? N4 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? N4 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? N4 C13 C14 125.8(8) . . ? N4 C13 H13 117.1 . . ? C14 C13 H13 117.1 . . ? C15 C14 C19 118.4(8) . . ? C15 C14 C13 117.5(8) . . ? C19 C14 C13 124.0(8) . . ? C16 C15 C14 123.2(8) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C15 C16 C17 117.5(9) . . ? C15 C16 H16 121.3 . . ? C17 C16 H16 121.3 . . ? C16 C17 C18 122.7(9) . . ? C16 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C17 C18 C19 121.4(8) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 N1 124.8(6) . . ? C18 C19 C14 116.5(7) . . ? N1 C19 C14 118.6(7) . . ? O3 C20 N5 127.9(6) . . ? O3 C20 C21 119.0(5) . . ? N5 C20 C21 113.1(6) . . ? O4 C21 N6 130.0(6) . . ? O4 C21 C20 117.4(6) . . ? N6 C21 C20 112.6(5) . . ? N6 C22 C23 122.8(6) . . ? N6 C22 C27 119.1(6) . . ? C23 C22 C27 117.9(6) . . ? C24 C23 C22 120.1(8) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 122.2(8) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26 C25 C24 118.6(8) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 121.2(8) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C22 119.9(7) . . ? C26 C27 C28 115.4(7) . . ? C22 C27 C28 124.4(7) . . ? N7 C28 C27 126.6(8) . . ? N7 C28 H28 116.7 . . ? C27 C28 H28 116.7 . . ? C30 C29 N7 110.5(7) . . ? C30 C29 H29A 109.6 . . ? N7 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? N7 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 112.6(7) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? N8 C31 C30 111.6(7) . . ? N8 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? N8 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? N8 C32 C33 126.0(7) . . ? N8 C32 H32 117.0 . . ? C33 C32 H32 117.0 . . ? C34 C33 C38 119.8(7) . . ? C34 C33 C32 119.1(7) . . ? C38 C33 C32 120.3(6) . . ? C35 C34 C33 122.3(7) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C34 C35 C36 117.5(7) . . ? C34 C35 H35 121.3 . . ? C36 C35 H35 121.3 . . ? C37 C36 C35 122.7(7) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 120.1(7) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 N5 122.5(6) . . ? C37 C38 C33 117.5(6) . . ? N5 C38 C33 120.0(6) . . ? O5 C39 N9 130.2(6) . . ? O5 C39 C40 116.0(6) . . ? N9 C39 C40 113.7(5) . . ? O6 C40 N10 128.7(7) . . ? O6 C40 C39 117.9(5) . . ? N10 C40 C39 113.4(6) . . ? C42 C41 N10 123.3(7) . . ? C42 C41 C46 119.0(9) . . ? N10 C41 C46 117.7(10) . . ? C41 C42 C43 121.2(11) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 117.6(14) . . ? C44 C43 H43 121.2 . . ? C42 C43 H43 121.2 . . ? C45 C44 C43 122.6(12) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C44 C45 C46 120.9(11) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C45 C46 C41 118.6(12) . . ? C45 C46 C47 117.9(9) . . ? C41 C46 C47 123.5(9) . . ? N11 C47 C46 127.7(8) . . ? N11 C47 H47 116.2 . . ? C46 C47 H47 116.2 . . ? N11 C48 C49 111.7(7) . . ? N11 C48 H48A 109.3 . . ? C49 C48 H48A 109.3 . . ? N11 C48 H48B 109.3 . . ? C49 C48 H48B 109.3 . . ? H48A C48 H48B 107.9 . . ? C48 C49 C50 110.9(6) . . ? C48 C49 H49A 109.5 . . ? C50 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 108.0 . . ? N12 C50 C49 111.4(6) . . ? N12 C50 H50A 109.3 . . ? C49 C50 H50A 109.3 . . ? N12 C50 H50B 109.3 . . ? C49 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? N12 C51 C52 125.6(8) . . ? N12 C51 H51 117.2 . . ? C52 C51 H51 117.2 . . ? C51 C52 C57 124.9(8) . . ? C51 C52 C53 117.3(8) . . ? C57 C52 C53 117.7(8) . . ? C54 C53 C52 123.2(9) . . ? C54 C53 H53 118.4 . . ? C52 C53 H53 118.4 . . ? C53 C54 C55 118.6(10) . . ? C53 C54 H54 120.7 . . ? C55 C54 H54 120.7 . . ? C54 C55 C56 120.2(10) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C57 C56 C55 122.9(8) . . ? C57 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? C56 C57 C52 117.3(7) . . ? C56 C57 N9 123.5(7) . . ? C52 C57 N9 119.3(7) . . ? O7 C58 N13 128.5(6) . . ? O7 C58 C59 118.1(5) . . ? N13 C58 C59 113.3(5) . . ? O8 C59 N14 128.9(6) . . ? O8 C59 C58 117.8(5) . . ? N14 C59 C58 113.3(5) . . ? C61 C60 N14 123.0(6) . . ? C61 C60 C65 116.9(7) . . ? N14 C60 C65 120.1(6) . . ? C62 C61 C60 121.9(7) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C63 120.0(8) . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 119.8(7) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 121.3(7) . . ? C63 C64 H64 119.3 . . ? C65 C64 H64 119.3 . . ? C64 C65 C66 116.2(7) . . ? C64 C65 C60 120.0(7) . . ? C66 C65 C60 123.2(7) . . ? N15 C66 C65 127.5(7) . . ? N15 C66 H66 116.2 . . ? C65 C66 H66 116.2 . . ? C68 C67 N15 108.3(7) . . ? C68 C67 H67A 110.0 . . ? N15 C67 H67A 110.0 . . ? C68 C67 H67B 110.0 . . ? N15 C67 H67B 110.0 . . ? H67A C67 H67B 108.4 . . ? C69 C68 C67 114.3(8) . . ? C69 C68 H68A 108.7 . . ? C67 C68 H68A 108.7 . . ? C69 C68 H68B 108.7 . . ? C67 C68 H68B 108.7 . . ? H68A C68 H68B 107.6 . . ? C68 C69 N16 112.2(8) . . ? C68 C69 H69A 109.2 . . ? N16 C69 H69A 109.2 . . ? C68 C69 H69B 109.2 . . ? N16 C69 H69B 109.2 . . ? H69A C69 H69B 107.9 . . ? N16 C70 C71 126.5(7) . . ? N16 C70 H70 116.8 . . ? C71 C70 H70 116.8 . . ? C70 C71 C76 123.2(7) . . ? C70 C71 C72 119.0(7) . . ? C76 C71 C72 117.6(7) . . ? C73 C72 C71 123.2(7) . . ? C73 C72 H72 118.4 . . ? C71 C72 H72 118.4 . . ? C72 C73 C74 117.9(8) . . ? C72 C73 H73 121.0 . . ? C74 C73 H73 121.0 . . ? C73 C74 C75 123.1(8) . . ? C73 C74 H74 118.5 . . ? C75 C74 H74 118.5 . . ? C74 C75 C76 120.1(7) . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? N13 C76 C75 122.5(6) . . ? N13 C76 C71 119.6(6) . . ? C75 C76 C71 118.0(6) . . ? C82 C77 C78 119.7(5) . . ? C82 C77 C83 119.3(5) . . ? C78 C77 C83 121.0(5) . . ? C79 C78 C77 119.8(5) . . ? C79 C78 H78 120.1 . . ? C77 C78 H78 120.1 . . ? C78 C79 C80 120.0(5) . . ? C78 C79 C84 119.6(5) . . ? C80 C79 C84 120.3(5) . . ? C81 C80 C79 120.3(5) . . ? C81 C80 H80 119.9 . . ? C79 C80 H80 119.9 . . ? C80 C81 C82 119.7(5) . . ? C80 C81 C85 120.8(5) . . ? C82 C81 C85 119.5(5) . . ? C77 C82 C81 120.4(5) . . ? C77 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? O10 C83 O9 124.6(6) . . ? O10 C83 C77 118.6(5) . . ? O9 C83 C77 116.8(5) . . ? O13 C84 O14 121.3(6) . . ? O13 C84 C79 121.7(6) . . ? O14 C84 C79 117.0(5) . . ? O12 C85 O11 123.1(5) . . ? O12 C85 C81 119.9(5) . . ? O11 C85 C81 117.0(5) . . ? O12 C85 Cd3 65.7(3) . . ? O11 C85 Cd3 57.8(3) . . ? C81 C85 Cd3 172.2(4) . . ? C91 C86 C87 119.6(6) . . ? C91 C86 C92 118.9(5) . . ? C87 C86 C92 121.4(6) . . ? C88 C87 C86 120.5(6) . . ? C88 C87 H87 119.7 . . ? C86 C87 H87 119.7 . . ? C87 C88 C89 118.8(5) . . ? C87 C88 C93 120.7(6) . . ? C89 C88 C93 120.5(6) . . ? C90 C89 C88 120.9(6) . . ? C90 C89 H89 119.5 . . ? C88 C89 H89 119.5 . . ? C91 C90 C89 119.2(6) . . ? C91 C90 C94 120.8(6) . . ? C89 C90 C94 120.1(6) . . ? C86 C91 C90 120.8(5) . . ? C86 C91 H91 119.6 . . ? C90 C91 H91 119.6 . . ? O15 C92 O16 125.8(6) . . ? O15 C92 C86 116.3(6) . . ? O16 C92 C86 117.8(5) . . ? O17 C93 O18 125.4(6) . . ? O17 C93 C88 117.3(6) . . ? O18 C93 C88 117.3(6) . . ? O19 C94 O20 123.6(6) . . ? O19 C94 C90 124.2(6) . . ? O20 C94 C90 112.1(6) . . ? C96 C95 C100 121.3(5) . . ? C96 C95 C101 119.4(5) . . ? C100 C95 C101 119.3(6) . . ? C95 C96 C97 119.5(5) . . ? C95 C96 H96 120.2 . . ? C97 C96 H96 120.2 . . ? C98 C97 C96 119.0(6) . . ? C98 C97 C102 120.3(5) . . ? C96 C97 C102 120.5(5) . . ? C99 C98 C97 122.0(5) . . ? C99 C98 H98 119.0 . . ? C97 C98 H98 119.0 . . ? C98 C99 C100 118.9(5) . . ? C98 C99 C103 121.2(5) . . ? C100 C99 C103 119.8(6) . . ? C95 C100 C99 119.2(6) . . ? C95 C100 H100 120.4 . . ? C99 C100 H100 120.4 . . ? O22 C101 O21 123.2(6) . . ? O22 C101 C95 117.4(6) . . ? O21 C101 C95 119.4(6) . . ? O22 C101 Cd2 55.0(3) . . ? O21 C101 Cd2 68.2(4) . . ? C95 C101 Cd2 172.4(5) . . ? O24 C102 O23 123.9(6) . . ? O24 C102 C97 116.6(5) . . ? O23 C102 C97 119.4(5) . . ? O26 C103 O25 121.4(6) . . ? O26 C103 C99 121.3(6) . . ? O25 C103 C99 117.3(6) . . ? O26 C103 Cd4 66.7(4) . 2_547 ? O25 C103 Cd4 54.7(3) . 2_547 ? C99 C103 Cd4 172.0(5) . 2_547 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Cd1 O1 C1 174.5(4) . . . . ? O15 Cd1 O1 C1 74.7(5) . . . . ? O14 Cd1 O1 C1 -95.1(5) 2_646 . . . ? O2 Cd1 O1 C1 2.2(4) . . . . ? O13 Cd1 O1 C1 -86.7(4) 2_646 . . . ? O9 Cd1 O2 C2 -19.0(6) . . . . ? O15 Cd1 O2 C2 -139.2(4) . . . . ? O14 Cd1 O2 C2 137.4(4) 2_646 . . . ? O1 Cd1 O2 C2 -4.0(4) . . . . ? O13 Cd1 O2 C2 87.6(4) 2_646 . . . ? O16 Cd2 O3 C20 -19.0(7) . . . . ? O10 Cd2 O3 C20 -128.1(4) . . . . ? O22 Cd2 O3 C20 132.7(4) . . . . ? O4 Cd2 O3 C20 -7.7(4) . . . . ? O21 Cd2 O3 C20 78.0(4) . . . . ? C101 Cd2 O3 C20 105.4(4) . . . . ? O16 Cd2 O4 C21 -179.7(4) . . . . ? O10 Cd2 O4 C21 85.7(4) . . . . ? O22 Cd2 O4 C21 -73.2(5) . . . . ? O3 Cd2 O4 C21 4.8(4) . . . . ? O21 Cd2 O4 C21 -92.7(4) . . . . ? C101 Cd2 O4 C21 -84.9(4) . . . . ? O24 Cd4 O5 C39 -161.2(4) . . . . ? O6 Cd4 O5 C39 3.2(4) . . . . ? O25 Cd4 O5 C39 104.5(5) 2_557 . . . ? O27 Cd4 O5 C39 -54.6(5) . . . . ? O26 Cd4 O5 C39 102.1(4) 2_557 . . . ? C103 Cd4 O5 C39 102.6(4) 2_557 . . . ? O24 Cd4 O6 C40 24.2(6) . . . . ? O25 Cd4 O6 C40 -141.0(5) 2_557 . . . ? O27 Cd4 O6 C40 142.0(5) . . . . ? O5 Cd4 O6 C40 -1.9(4) . . . . ? O26 Cd4 O6 C40 -88.2(5) 2_557 . . . ? C103 Cd4 O6 C40 -113.6(5) 2_557 . . . ? O23 Cd3 O7 C58 126.9(4) . . . . ? O18 Cd3 O7 C58 -15.9(9) 1_565 . . . ? O11 Cd3 O7 C58 -132.9(4) . . . . ? O8 Cd3 O7 C58 14.7(4) . . . . ? O12 Cd3 O7 C58 -78.0(4) . . . . ? C85 Cd3 O7 C58 -104.6(4) . . . . ? O23 Cd3 O8 C59 -96.8(4) . . . . ? O18 Cd3 O8 C59 159.8(4) 1_565 . . . ? O11 Cd3 O8 C59 59.9(5) . . . . ? O7 Cd3 O8 C59 -12.7(4) . . . . ? O12 Cd3 O8 C59 74.0(4) . . . . ? C85 Cd3 O8 C59 71.0(4) . . . . ? O15 Cd1 O9 C83 67.1(4) . . . . ? O14 Cd1 O9 C83 151.9(4) 2_646 . . . ? O2 Cd1 O9 C83 -50.2(5) . . . . ? O1 Cd1 O9 C83 -64.4(4) . . . . ? O13 Cd1 O9 C83 -154.2(4) 2_646 . . . ? O16 Cd2 O10 C83 11.3(10) . . . . ? O22 Cd2 O10 C83 -94.0(10) . . . . ? O3 Cd2 O10 C83 169.0(10) . . . . ? O4 Cd2 O10 C83 99.7(10) . . . . ? O21 Cd2 O10 C83 -83.8(12) . . . . ? C101 Cd2 O10 C83 -90.9(10) . . . . ? O23 Cd3 O11 C85 178.9(4) . . . . ? O18 Cd3 O11 C85 -80.6(4) 1_565 . . . ? O8 Cd3 O11 C85 20.8(5) . . . . ? O7 Cd3 O11 C85 86.3(4) . . . . ? O12 Cd3 O11 C85 3.6(3) . . . . ? O23 Cd3 O12 C85 -14.7(7) . . . . ? O18 Cd3 O12 C85 90.4(4) 1_565 . . . ? O11 Cd3 O12 C85 -3.7(4) . . . . ? O8 Cd3 O12 C85 -174.2(4) . . . . ? O7 Cd3 O12 C85 -102.7(4) . . . . ? O9 Cd1 O15 C92 -30.5(10) . . . . ? O14 Cd1 O15 C92 -127.0(10) 2_646 . . . ? O2 Cd1 O15 C92 122.3(10) . . . . ? O1 Cd1 O15 C92 59.0(10) . . . . ? O13 Cd1 O15 C92 -147.0(9) 2_646 . . . ? O10 Cd2 O16 C92 79.4(4) . . . . ? O22 Cd2 O16 C92 -179.6(4) . . . . ? O3 Cd2 O16 C92 -28.7(7) . . . . ? O4 Cd2 O16 C92 -39.5(4) . . . . ? O21 Cd2 O16 C92 -127.6(4) . . . . ? C101 Cd2 O16 C92 -153.3(4) . . . . ? O16 Cd2 O21 C101 -110.0(5) . . . . ? O10 Cd2 O21 C101 -12.6(8) . . . . ? O22 Cd2 O21 C101 -0.2(4) . . . . ? O3 Cd2 O21 C101 93.4(5) . . . . ? O4 Cd2 O21 C101 164.3(5) . . . . ? O16 Cd2 O22 C101 75.8(4) . . . . ? O10 Cd2 O22 C101 174.5(4) . . . . ? O3 Cd2 O22 C101 -92.9(4) . . . . ? O4 Cd2 O22 C101 -24.1(5) . . . . ? O21 Cd2 O22 C101 0.2(4) . . . . ? O18 Cd3 O23 C102 -31(2) 1_565 . . . ? O11 Cd3 O23 C102 62(2) . . . . ? O8 Cd3 O23 C102 -131(2) . . . . ? O7 Cd3 O23 C102 158(2) . . . . ? O12 Cd3 O23 C102 71(2) . . . . ? C85 Cd3 O23 C102 63(2) . . . . ? O6 Cd4 O24 C102 38.3(6) . . . . ? O25 Cd4 O24 C102 -155.8(4) 2_557 . . . ? O27 Cd4 O24 C102 -71.5(4) . . . . ? O5 Cd4 O24 C102 63.3(4) . . . . ? O26 Cd4 O24 C102 151.1(4) 2_557 . . . ? C103 Cd4 O24 C102 177.3(4) 2_557 . . . ? N2 Ni1 N1 C1 2.9(4) . . . . ? N4 Ni1 N1 C1 166.7(4) . . . . ? N3 Ni1 N1 C1 -84.1(13) . . . . ? N2 Ni1 N1 C19 179.2(5) . . . . ? N4 Ni1 N1 C19 -17.0(5) . . . . ? N3 Ni1 N1 C19 92.2(13) . . . . ? N4 Ni1 N2 C2 -96.5(11) . . . . ? N1 Ni1 N2 C2 -4.1(4) . . . . ? N3 Ni1 N2 C2 159.6(4) . . . . ? N4 Ni1 N2 C3 76.5(13) . . . . ? N1 Ni1 N2 C3 168.8(6) . . . . ? N3 Ni1 N2 C3 -27.5(6) . . . . ? N2 Ni1 N3 C9 12.1(8) . . . . ? N4 Ni1 N3 C9 -152.2(8) . . . . ? N1 Ni1 N3 C9 98.3(13) . . . . ? N2 Ni1 N3 C10 -159.4(5) . . . . ? N4 Ni1 N3 C10 36.3(6) . . . . ? N1 Ni1 N3 C10 -73.2(14) . . . . ? N2 Ni1 N4 C13 100.7(12) . . . . ? N1 Ni1 N4 C13 9.3(7) . . . . ? N3 Ni1 N4 C13 -155.3(7) . . . . ? N2 Ni1 N4 C12 -72.0(13) . . . . ? N1 Ni1 N4 C12 -163.4(5) . . . . ? N3 Ni1 N4 C12 32.1(6) . . . . ? N7 Ni2 N5 C20 118.0(18) . . . . ? N6 Ni2 N5 C20 19.6(4) . . . . ? N8 Ni2 N5 C20 -143.9(4) . . . . ? N7 Ni2 N5 C38 -65(2) . . . . ? N6 Ni2 N5 C38 -163.5(5) . . . . ? N8 Ni2 N5 C38 33.0(5) . . . . ? N7 Ni2 N6 C21 164.9(4) . . . . ? N5 Ni2 N6 C21 -23.1(4) . . . . ? N8 Ni2 N6 C21 61.0(11) . . . . ? N7 Ni2 N6 C22 -1.3(6) . . . . ? N5 Ni2 N6 C22 170.8(6) . . . . ? N8 Ni2 N6 C22 -105.2(10) . . . . ? N6 Ni2 N7 C28 -3.0(9) . . . . ? N5 Ni2 N7 C28 -101(2) . . . . ? N8 Ni2 N7 C28 160.9(9) . . . . ? N6 Ni2 N7 C29 171.6(6) . . . . ? N5 Ni2 N7 C29 74(2) . . . . ? N8 Ni2 N7 C29 -24.6(7) . . . . ? N7 Ni2 N8 C32 150.3(7) . . . . ? N6 Ni2 N8 C32 -105.0(11) . . . . ? N5 Ni2 N8 C32 -21.7(7) . . . . ? N7 Ni2 N8 C31 -41.7(6) . . . . ? N6 Ni2 N8 C31 63.0(11) . . . . ? N5 Ni2 N8 C31 146.2(5) . . . . ? N11 Ni3 N9 C39 95.4(12) . . . . ? N12 Ni3 N9 C39 -161.7(4) . . . . ? N10 Ni3 N9 C39 2.2(4) . . . . ? N11 Ni3 N9 C57 -80.2(13) . . . . ? N12 Ni3 N9 C57 22.7(5) . . . . ? N10 Ni3 N9 C57 -173.4(5) . . . . ? N11 Ni3 N10 C40 -165.6(4) . . . . ? N9 Ni3 N10 C40 -2.5(4) . . . . ? N12 Ni3 N10 C40 89.7(11) . . . . ? N11 Ni3 N10 C41 25.5(6) . . . . ? N9 Ni3 N10 C41 -171.4(6) . . . . ? N12 Ni3 N10 C41 -79.2(12) . . . . ? N9 Ni3 N11 C47 -100.3(14) . . . . ? N12 Ni3 N11 C47 156.3(7) . . . . ? N10 Ni3 N11 C47 -8.1(7) . . . . ? N9 Ni3 N11 C48 71.1(13) . . . . ? N12 Ni3 N11 C48 -32.4(5) . . . . ? N10 Ni3 N11 C48 163.2(5) . . . . ? N11 Ni3 N12 C51 151.4(7) . . . . ? N9 Ni3 N12 C51 -12.1(7) . . . . ? N10 Ni3 N12 C51 -103.4(12) . . . . ? N11 Ni3 N12 C50 -35.9(5) . . . . ? N9 Ni3 N12 C50 160.6(5) . . . . ? N10 Ni3 N12 C50 69.3(12) . . . . ? N15 Ni4 N13 C58 -111.2(19) . . . . ? N14 Ni4 N13 C58 -20.0(4) . . . . ? N16 Ni4 N13 C58 146.4(4) . . . . ? N15 Ni4 N13 C76 72(2) . . . . ? N14 Ni4 N13 C76 163.6(5) . . . . ? N16 Ni4 N13 C76 -30.0(5) . . . . ? N15 Ni4 N14 C59 -166.4(4) . . . . ? N13 Ni4 N14 C59 21.8(4) . . . . ? N16 Ni4 N14 C59 -54.1(14) . . . . ? N15 Ni4 N14 C60 2.6(6) . . . . ? N13 Ni4 N14 C60 -169.2(6) . . . . ? N16 Ni4 N14 C60 114.9(12) . . . . ? N13 Ni4 N15 C66 96(2) . . . . ? N14 Ni4 N15 C66 5.2(8) . . . . ? N16 Ni4 N15 C66 -161.8(8) . . . . ? N13 Ni4 N15 C67 -76(2) . . . . ? N14 Ni4 N15 C67 -166.7(6) . . . . ? N16 Ni4 N15 C67 26.4(6) . . . . ? N15 Ni4 N16 C70 -150.7(8) . . . . ? N13 Ni4 N16 C70 21.4(8) . . . . ? N14 Ni4 N16 C70 96.5(14) . . . . ? N15 Ni4 N16 C69 39.8(6) . . . . ? N13 Ni4 N16 C69 -148.2(6) . . . . ? N14 Ni4 N16 C69 -73.0(13) . . . . ? Cd1 O1 C1 N1 176.2(5) . . . . ? Cd1 O1 C1 C2 -0.6(7) . . . . ? C19 N1 C1 O1 5.2(9) . . . . ? Ni1 N1 C1 O1 -178.2(5) . . . . ? C19 N1 C1 C2 -178.0(5) . . . . ? Ni1 N1 C1 C2 -1.3(6) . . . . ? Cd1 O2 C2 N2 -172.8(5) . . . . ? Cd1 O2 C2 C1 5.2(7) . . . . ? C3 N2 C2 O2 8.9(10) . . . . ? Ni1 N2 C2 O2 -177.7(5) . . . . ? C3 N2 C2 C1 -169.2(6) . . . . ? Ni1 N2 C2 C1 4.2(6) . . . . ? O1 C1 C2 O2 -3.0(8) . . . . ? N1 C1 C2 O2 179.8(5) . . . . ? O1 C1 C2 N2 175.3(5) . . . . ? N1 C1 C2 N2 -1.9(7) . . . . ? C2 N2 C3 C4 19.8(12) . . . . ? Ni1 N2 C3 C4 -152.7(7) . . . . ? C2 N2 C3 C8 -161.7(7) . . . . ? Ni1 N2 C3 C8 25.8(10) . . . . ? C8 C3 C4 C5 3.5(14) . . . . ? N2 C3 C4 C5 -178.0(9) . . . . ? C3 C4 C5 C6 -0.9(17) . . . . ? C4 C5 C6 C7 -1.2(18) . . . . ? C5 C6 C7 C8 0.5(19) . . . . ? C6 C7 C8 C9 -178.9(12) . . . . ? C6 C7 C8 C3 2.1(18) . . . . ? C4 C3 C8 C7 -3.9(13) . . . . ? N2 C3 C8 C7 177.5(9) . . . . ? C4 C3 C8 C9 177.1(9) . . . . ? N2 C3 C8 C9 -1.5(14) . . . . ? C10 N3 C9 C8 176.7(8) . . . . ? Ni1 N3 C9 C8 5.7(15) . . . . ? C7 C8 C9 N3 166.1(11) . . . . ? C3 C8 C9 N3 -14.9(16) . . . . ? C9 N3 C10 C11 113.7(10) . . . . ? Ni1 N3 C10 C11 -74.1(8) . . . . ? N3 C10 C11 C12 35.0(12) . . . . ? C13 N4 C12 C11 113.7(10) . . . . ? Ni1 N4 C12 C11 -72.7(10) . . . . ? C10 C11 C12 N4 35.5(13) . . . . ? C12 N4 C13 C14 173.0(6) . . . . ? Ni1 N4 C13 C14 0.2(12) . . . . ? N4 C13 C14 C15 175.9(8) . . . . ? N4 C13 C14 C19 -7.0(12) . . . . ? C19 C14 C15 C16 2.8(12) . . . . ? C13 C14 C15 C16 -179.9(8) . . . . ? C14 C15 C16 C17 1.4(13) . . . . ? C15 C16 C17 C18 -2.3(14) . . . . ? C16 C17 C18 C19 -1.1(13) . . . . ? C17 C18 C19 N1 -177.1(7) . . . . ? C17 C18 C19 C14 5.1(11) . . . . ? C1 N1 C19 C18 13.2(9) . . . . ? Ni1 N1 C19 C18 -162.9(5) . . . . ? C1 N1 C19 C14 -169.1(5) . . . . ? Ni1 N1 C19 C14 14.9(8) . . . . ? C15 C14 C19 C18 -5.8(9) . . . . ? C13 C14 C19 C18 177.1(6) . . . . ? C15 C14 C19 N1 176.3(6) . . . . ? C13 C14 C19 N1 -0.9(9) . . . . ? Cd2 O3 C20 N5 -171.0(5) . . . . ? Cd2 O3 C20 C21 9.7(7) . . . . ? C38 N5 C20 O3 -8.2(10) . . . . ? Ni2 N5 C20 O3 168.8(5) . . . . ? C38 N5 C20 C21 171.1(5) . . . . ? Ni2 N5 C20 C21 -11.9(6) . . . . ? Cd2 O4 C21 N6 -179.9(5) . . . . ? Cd2 O4 C21 C20 -1.9(7) . . . . ? C22 N6 C21 O4 7.1(9) . . . . ? Ni2 N6 C21 O4 -160.3(5) . . . . ? C22 N6 C21 C20 -171.0(5) . . . . ? Ni2 N6 C21 C20 21.5(6) . . . . ? O3 C20 C21 O4 -5.5(8) . . . . ? N5 C20 C21 O4 175.1(5) . . . . ? O3 C20 C21 N6 172.9(5) . . . . ? N5 C20 C21 N6 -6.5(7) . . . . ? C21 N6 C22 C23 25.0(9) . . . . ? Ni2 N6 C22 C23 -170.0(5) . . . . ? C21 N6 C22 C27 -159.4(6) . . . . ? Ni2 N6 C22 C27 5.5(9) . . . . ? N6 C22 C23 C24 177.7(7) . . . . ? C27 C22 C23 C24 2.0(11) . . . . ? C22 C23 C24 C25 -0.1(14) . . . . ? C23 C24 C25 C26 -0.2(14) . . . . ? C24 C25 C26 C27 -1.5(14) . . . . ? C25 C26 C27 C22 3.5(12) . . . . ? C25 C26 C27 C28 -170.2(8) . . . . ? N6 C22 C27 C26 -179.4(7) . . . . ? C23 C22 C27 C26 -3.7(10) . . . . ? N6 C22 C27 C28 -6.4(10) . . . . ? C23 C22 C27 C28 169.4(8) . . . . ? C29 N7 C28 C27 -171.7(8) . . . . ? Ni2 N7 C28 C27 2.8(15) . . . . ? C26 C27 C28 N7 175.6(10) . . . . ? C22 C27 C28 N7 2.3(14) . . . . ? C28 N7 C29 C30 -111.0(10) . . . . ? Ni2 N7 C29 C30 73.9(9) . . . . ? N7 C29 C30 C31 -46.5(11) . . . . ? C32 N8 C31 C30 -119.3(9) . . . . ? Ni2 N8 C31 C30 72.0(8) . . . . ? C29 C30 C31 N8 -22.3(11) . . . . ? C31 N8 C32 C33 -169.1(7) . . . . ? Ni2 N8 C32 C33 -1.7(12) . . . . ? N8 C32 C33 C34 -165.0(8) . . . . ? N8 C32 C33 C38 24.6(12) . . . . ? C38 C33 C34 C35 -1.0(11) . . . . ? C32 C33 C34 C35 -171.4(7) . . . . ? C33 C34 C35 C36 0.5(11) . . . . ? C34 C35 C36 C37 0.3(11) . . . . ? C35 C36 C37 C38 -0.7(11) . . . . ? C36 C37 C38 N5 -176.4(6) . . . . ? C36 C37 C38 C33 0.2(10) . . . . ? C20 N5 C38 C37 -27.4(9) . . . . ? Ni2 N5 C38 C37 156.0(5) . . . . ? C20 N5 C38 C33 156.1(6) . . . . ? Ni2 N5 C38 C33 -20.5(9) . . . . ? C34 C33 C38 C37 0.6(10) . . . . ? C32 C33 C38 C37 170.9(6) . . . . ? C34 C33 C38 N5 177.3(6) . . . . ? C32 C33 C38 N5 -12.4(10) . . . . ? Cd4 O5 C39 N9 179.2(5) . . . . ? Cd4 O5 C39 C40 -4.0(6) . . . . ? C57 N9 C39 O5 -8.6(10) . . . . ? Ni3 N9 C39 O5 175.5(5) . . . . ? C57 N9 C39 C40 174.5(5) . . . . ? Ni3 N9 C39 C40 -1.4(6) . . . . ? Cd4 O6 C40 N10 -178.9(5) . . . . ? Cd4 O6 C40 C39 0.7(7) . . . . ? C41 N10 C40 O6 -8.5(10) . . . . ? Ni3 N10 C40 O6 -178.1(5) . . . . ? C41 N10 C40 C39 171.9(5) . . . . ? Ni3 N10 C40 C39 2.3(6) . . . . ? O5 C39 C40 O6 2.4(8) . . . . ? N9 C39 C40 O6 179.8(6) . . . . ? O5 C39 C40 N10 -178.0(5) . . . . ? N9 C39 C40 N10 -0.6(7) . . . . ? C40 N10 C41 C42 -14.5(10) . . . . ? Ni3 N10 C41 C42 153.6(6) . . . . ? C40 N10 C41 C46 166.1(6) . . . . ? Ni3 N10 C41 C46 -25.8(9) . . . . ? N10 C41 C42 C43 -179.4(7) . . . . ? C46 C41 C42 C43 0.0(12) . . . . ? C41 C42 C43 C44 -1.7(14) . . . . ? C42 C43 C44 C45 0.5(17) . . . . ? C43 C44 C45 C46 2.5(18) . . . . ? C44 C45 C46 C41 -4.2(15) . . . . ? C44 C45 C46 C47 174.1(11) . . . . ? C42 C41 C46 C45 2.9(12) . . . . ? N10 C41 C46 C45 -177.6(8) . . . . ? C42 C41 C46 C47 -175.3(8) . . . . ? N10 C41 C46 C47 4.2(12) . . . . ? C48 N11 C47 C46 179.8(8) . . . . ? Ni3 N11 C47 C46 -8.9(13) . . . . ? C45 C46 C47 N11 -163.9(9) . . . . ? C41 C46 C47 N11 14.3(15) . . . . ? C47 N11 C48 C49 -114.0(10) . . . . ? Ni3 N11 C48 C49 74.0(10) . . . . ? N11 C48 C49 C50 -36.0(14) . . . . ? C51 N12 C50 C49 -111.6(10) . . . . ? Ni3 N12 C50 C49 75.0(10) . . . . ? C48 C49 C50 N12 -34.9(15) . . . . ? C50 N12 C51 C52 -173.8(6) . . . . ? Ni3 N12 C51 C52 -1.3(11) . . . . ? N12 C51 C52 C57 10.0(12) . . . . ? N12 C51 C52 C53 -171.5(7) . . . . ? C51 C52 C53 C54 179.8(8) . . . . ? C57 C52 C53 C54 -1.6(12) . . . . ? C52 C53 C54 C55 -1.2(14) . . . . ? C53 C54 C55 C56 2.2(14) . . . . ? C54 C55 C56 C57 -0.4(13) . . . . ? C55 C56 C57 C52 -2.3(11) . . . . ? C55 C56 C57 N9 178.0(7) . . . . ? C51 C52 C57 C56 -178.3(7) . . . . ? C53 C52 C57 C56 3.2(9) . . . . ? C51 C52 C57 N9 1.4(10) . . . . ? C53 C52 C57 N9 -177.1(6) . . . . ? C39 N9 C57 C56 -16.2(9) . . . . ? Ni3 N9 C57 C56 159.2(5) . . . . ? C39 N9 C57 C52 164.2(6) . . . . ? Ni3 N9 C57 C52 -20.5(8) . . . . ? Cd3 O7 C58 N13 167.1(5) . . . . ? Cd3 O7 C58 C59 -15.3(6) . . . . ? C76 N13 C58 O7 8.4(10) . . . . ? Ni4 N13 C58 O7 -168.1(5) . . . . ? C76 N13 C58 C59 -169.3(5) . . . . ? Ni4 N13 C58 C59 14.2(6) . . . . ? Cd3 O8 C59 N14 -171.5(5) . . . . ? Cd3 O8 C59 C58 9.9(6) . . . . ? C60 N14 C59 O8 -7.4(9) . . . . ? Ni4 N14 C59 O8 162.4(5) . . . . ? C60 N14 C59 C58 171.3(5) . . . . ? Ni4 N14 C59 C58 -18.9(6) . . . . ? O7 C58 C59 O8 4.2(8) . . . . ? N13 C58 C59 O8 -177.8(5) . . . . ? O7 C58 C59 N14 -174.7(5) . . . . ? N13 C58 C59 N14 3.3(7) . . . . ? C59 N14 C60 C61 -22.9(10) . . . . ? Ni4 N14 C60 C61 169.2(5) . . . . ? C59 N14 C60 C65 158.4(6) . . . . ? Ni4 N14 C60 C65 -9.6(9) . . . . ? N14 C60 C61 C62 -178.0(7) . . . . ? C65 C60 C61 C62 0.8(11) . . . . ? C60 C61 C62 C63 -3.0(13) . . . . ? C61 C62 C63 C64 3.3(13) . . . . ? C62 C63 C64 C65 -1.5(13) . . . . ? C63 C64 C65 C66 170.1(8) . . . . ? C63 C64 C65 C60 -0.8(12) . . . . ? C61 C60 C65 C64 1.1(10) . . . . ? N14 C60 C65 C64 179.9(7) . . . . ? C61 C60 C65 C66 -169.2(7) . . . . ? N14 C60 C65 C66 9.7(11) . . . . ? C67 N15 C66 C65 165.2(9) . . . . ? Ni4 N15 C66 C65 -6.3(15) . . . . ? C64 C65 C66 N15 -172.3(9) . . . . ? C60 C65 C66 N15 -1.7(15) . . . . ? C66 N15 C67 C68 112.4(10) . . . . ? Ni4 N15 C67 C68 -75.1(10) . . . . ? N15 C67 C68 C69 48.9(14) . . . . ? C67 C68 C69 N16 21.2(15) . . . . ? C70 N16 C69 C68 119.0(11) . . . . ? Ni4 N16 C69 C68 -70.8(10) . . . . ? C69 N16 C70 C71 165.5(8) . . . . ? Ni4 N16 C70 C71 -3.6(13) . . . . ? N16 C70 C71 C76 -15.7(13) . . . . ? N16 C70 C71 C72 169.3(8) . . . . ? C70 C71 C72 C73 176.1(7) . . . . ? C76 C71 C72 C73 0.9(11) . . . . ? C71 C72 C73 C74 -1.9(12) . . . . ? C72 C73 C74 C75 0.2(12) . . . . ? C73 C74 C75 C76 2.4(11) . . . . ? C58 N13 C76 C75 24.7(9) . . . . ? Ni4 N13 C76 C75 -159.3(5) . . . . ? C58 N13 C76 C71 -155.0(6) . . . . ? Ni4 N13 C76 C71 21.0(8) . . . . ? C74 C75 C76 N13 177.0(6) . . . . ? C74 C75 C76 C71 -3.3(10) . . . . ? C70 C71 C76 N13 6.4(10) . . . . ? C72 C71 C76 N13 -178.5(6) . . . . ? C70 C71 C76 C75 -173.3(7) . . . . ? C72 C71 C76 C75 1.7(9) . . . . ? C82 C77 C78 C79 1.0(8) . . . . ? C83 C77 C78 C79 178.8(5) . . . . ? C77 C78 C79 C80 -3.6(8) . . . . ? C77 C78 C79 C84 179.3(5) . . . . ? C78 C79 C80 C81 3.7(8) . . . . ? C84 C79 C80 C81 -179.2(5) . . . . ? C79 C80 C81 C82 -1.1(9) . . . . ? C79 C80 C81 C85 179.4(5) . . . . ? C78 C77 C82 C81 1.6(8) . . . . ? C83 C77 C82 C81 -176.2(5) . . . . ? C80 C81 C82 C77 -1.5(9) . . . . ? C85 C81 C82 C77 178.0(5) . . . . ? Cd2 O10 C83 O9 -77.0(11) . . . . ? Cd2 O10 C83 C77 103.5(10) . . . . ? Cd1 O9 C83 O10 -6.3(7) . . . . ? Cd1 O9 C83 C77 173.2(4) . . . . ? C82 C77 C83 O10 -24.2(8) . . . . ? C78 C77 C83 O10 158.0(5) . . . . ? C82 C77 C83 O9 156.2(5) . . . . ? C78 C77 C83 O9 -21.6(8) . . . . ? Cd1 O13 C84 O14 -1.1(6) 2_656 . . . ? Cd1 O13 C84 C79 178.7(5) 2_656 . . . ? Cd1 O14 C84 O13 1.2(7) 2_656 . . . ? Cd1 O14 C84 C79 -178.5(4) 2_656 . . . ? C78 C79 C84 O13 167.2(6) . . . . ? C80 C79 C84 O13 -9.9(9) . . . . ? C78 C79 C84 O14 -13.1(8) . . . . ? C80 C79 C84 O14 169.8(6) . . . . ? Cd3 O12 C85 O11 6.5(6) . . . . ? Cd3 O12 C85 C81 -173.8(5) . . . . ? Cd3 O11 C85 O12 -7.0(7) . . . . ? Cd3 O11 C85 C81 173.3(5) . . . . ? C80 C81 C85 O12 3.7(9) . . . . ? C82 C81 C85 O12 -175.8(6) . . . . ? C80 C81 C85 O11 -176.6(6) . . . . ? C82 C81 C85 O11 3.9(8) . . . . ? C80 C81 C85 Cd3 -130(3) . . . . ? C82 C81 C85 Cd3 51(4) . . . . ? O23 Cd3 C85 O12 172.2(4) . . . . ? O18 Cd3 C85 O12 -87.7(4) 1_565 . . . ? O11 Cd3 C85 O12 173.6(6) . . . . ? O8 Cd3 C85 O12 6.7(4) . . . . ? O7 Cd3 C85 O12 77.6(4) . . . . ? O23 Cd3 C85 O11 -1.4(5) . . . . ? O18 Cd3 C85 O11 98.7(4) 1_565 . . . ? O8 Cd3 C85 O11 -166.9(3) . . . . ? O7 Cd3 C85 O11 -96.0(4) . . . . ? O12 Cd3 C85 O11 -173.6(6) . . . . ? O23 Cd3 C85 C81 -51(3) . . . . ? O18 Cd3 C85 C81 49(3) 1_565 . . . ? O11 Cd3 C85 C81 -50(3) . . . . ? O8 Cd3 C85 C81 143(3) . . . . ? O7 Cd3 C85 C81 -146(3) . . . . ? O12 Cd3 C85 C81 136(4) . . . . ? C91 C86 C87 C88 2.2(9) . . . . ? C92 C86 C87 C88 -175.5(5) . . . . ? C86 C87 C88 C89 -2.7(9) . . . . ? C86 C87 C88 C93 177.0(5) . . . . ? C87 C88 C89 C90 1.5(8) . . . . ? C93 C88 C89 C90 -178.2(5) . . . . ? C88 C89 C90 C91 0.3(8) . . . . ? C88 C89 C90 C94 178.5(5) . . . . ? C87 C86 C91 C90 -0.4(9) . . . . ? C92 C86 C91 C90 177.4(5) . . . . ? C89 C90 C91 C86 -0.9(9) . . . . ? C94 C90 C91 C86 -179.0(5) . . . . ? Cd1 O15 C92 O16 -14.0(14) . . . . ? Cd1 O15 C92 C86 169.6(7) . . . . ? Cd2 O16 C92 O15 -39.4(8) . . . . ? Cd2 O16 C92 C86 137.0(4) . . . . ? C91 C86 C92 O15 -8.3(8) . . . . ? C87 C86 C92 O15 169.5(5) . . . . ? C91 C86 C92 O16 175.0(5) . . . . ? C87 C86 C92 O16 -7.2(8) . . . . ? Cd3 O18 C93 O17 68.4(9) 1_545 . . . ? Cd3 O18 C93 C88 -113.1(6) 1_545 . . . ? C87 C88 C93 O17 4.7(9) . . . . ? C89 C88 C93 O17 -175.6(6) . . . . ? C87 C88 C93 O18 -174.0(6) . . . . ? C89 C88 C93 O18 5.7(8) . . . . ? C91 C90 C94 O19 158.5(6) . . . . ? C89 C90 C94 O19 -19.7(9) . . . . ? C91 C90 C94 O20 -20.7(8) . . . . ? C89 C90 C94 O20 161.1(6) . . . . ? C100 C95 C96 C97 2.1(9) . . . . ? C101 C95 C96 C97 -176.2(5) . . . . ? C95 C96 C97 C98 -2.2(8) . . . . ? C95 C96 C97 C102 172.8(5) . . . . ? C96 C97 C98 C99 0.6(9) . . . . ? C102 C97 C98 C99 -174.4(5) . . . . ? C97 C98 C99 C100 1.1(9) . . . . ? C97 C98 C99 C103 176.0(5) . . . . ? C96 C95 C100 C99 -0.4(9) . . . . ? C101 C95 C100 C99 177.8(5) . . . . ? C98 C99 C100 C95 -1.2(9) . . . . ? C103 C99 C100 C95 -176.1(6) . . . . ? Cd2 O22 C101 O21 -0.5(8) . . . . ? Cd2 O22 C101 C95 179.3(5) . . . . ? Cd2 O21 C101 O22 0.4(7) . . . . ? Cd2 O21 C101 C95 -179.4(6) . . . . ? C96 C95 C101 O22 5.6(9) . . . . ? C100 C95 C101 O22 -172.7(6) . . . . ? C96 C95 C101 O21 -174.6(7) . . . . ? C100 C95 C101 O21 7.1(10) . . . . ? C96 C95 C101 Cd2 10(4) . . . . ? C100 C95 C101 Cd2 -168(3) . . . . ? O16 Cd2 C101 O22 -108.9(4) . . . . ? O10 Cd2 C101 O22 -6.7(5) . . . . ? O3 Cd2 C101 O22 90.5(4) . . . . ? O4 Cd2 C101 O22 163.2(4) . . . . ? O21 Cd2 C101 O22 -179.6(7) . . . . ? O16 Cd2 C101 O21 70.7(5) . . . . ? O10 Cd2 C101 O21 172.9(4) . . . . ? O22 Cd2 C101 O21 179.6(7) . . . . ? O3 Cd2 C101 O21 -90.0(5) . . . . ? O4 Cd2 C101 O21 -17.2(5) . . . . ? O16 Cd2 C101 C95 -113(3) . . . . ? O10 Cd2 C101 C95 -11(4) . . . . ? O22 Cd2 C101 C95 -5(3) . . . . ? O3 Cd2 C101 C95 86(3) . . . . ? O4 Cd2 C101 C95 159(3) . . . . ? O21 Cd2 C101 C95 176(4) . . . . ? Cd4 O24 C102 O23 22.4(7) . . . . ? Cd4 O24 C102 C97 -158.0(4) . . . . ? Cd3 O23 C102 O24 99(2) . . . . ? Cd3 O23 C102 C97 -80(2) . . . . ? C98 C97 C102 O24 21.9(8) . . . . ? C96 C97 C102 O24 -153.1(5) . . . . ? C98 C97 C102 O23 -158.5(6) . . . . ? C96 C97 C102 O23 26.5(8) . . . . ? Cd4 O26 C103 O25 -1.4(7) 2_547 . . . ? Cd4 O26 C103 C99 179.2(6) 2_547 . . . ? Cd4 O25 C103 O26 1.5(8) 2_547 . . . ? Cd4 O25 C103 C99 -179.0(5) 2_547 . . . ? C98 C99 C103 O26 -176.0(7) . . . . ? C100 C99 C103 O26 -1.2(10) . . . . ? C98 C99 C103 O25 4.5(9) . . . . ? C100 C99 C103 O25 179.4(6) . . . . ? C98 C99 C103 Cd4 -1(3) . . . 2_547 ? C100 C99 C103 Cd4 174(3) . . . 2_547 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.012 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.079 data_100110c _database_code_depnum_ccdc_archive 'CCDC 800816' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Co2 N4 Ni O11' _chemical_formula_weight 769.08 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' Co Co 0.3494 0.9721 '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 10.149(7) _cell_length_b 12.422(9) _cell_length_c 13.888(10) _cell_angle_alpha 100.960(13) _cell_angle_beta 108.179(12) _cell_angle_gamma 109.137(12) _cell_volume 1485.8(18) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2005 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 25.76 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.167268 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _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_% ? _diffrn_reflns_number 7420 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5175 _reflns_number_gt 3217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5175 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33347(12) 0.26375(8) 0.54512(8) 0.0429(3) Uani 1 1 d . . . Co1 Co 0.08183(11) 0.05192(8) 0.12402(7) 0.0312(3) Uani 1 1 d . . . Co2 Co 0.21131(12) 0.24400(8) 0.00026(9) 0.0400(3) Uani 1 1 d . . . O1 O 0.2927(6) 0.1800(4) 0.2461(4) 0.0426(12) Uani 1 1 d . . . O2 O 0.0349(6) 0.0482(4) 0.2599(4) 0.0416(12) Uani 1 1 d . . . O3 O 0.4327(6) 0.3292(5) 0.0608(5) 0.0534(15) Uani 1 1 d . . . O4 O 0.4518(6) 0.1574(5) 0.0100(5) 0.0576(16) Uani 1 1 d . . . O5 O 0.9828(6) 0.1759(4) 0.1216(4) 0.0427(13) Uani 1 1 d . . . O6 O 1.1461(6) 0.3303(4) 0.0979(5) 0.0431(13) Uani 1 1 d . . . O7 O 1.0930(7) 0.7182(5) 0.1692(6) 0.0658(19) Uani 1 1 d . . . O8 O 0.8577(6) 0.7105(4) 0.1265(5) 0.0493(14) Uani 1 1 d . . . O9 O 0.1298(5) 0.0755(4) -0.0082(4) 0.0304(10) Uani 1 1 d . . . H9A H 0.1979 0.0600 -0.0234 0.046 Uiso 1 1 d R . . O10 O 0.1753(6) -0.0741(5) 0.1335(5) 0.0559(16) Uani 1 1 d . . . H10' H 0.2662 -0.0545 0.1387 0.084 Uiso 1 1 d R . . H10" H 0.1371 -0.1367 0.1493 0.084 Uiso 1 1 d R . . O11 O 0.4620(8) -0.0083(6) 0.1243(6) 0.078(2) Uani 1 1 d . . . H11' H 0.3735 -0.0453 0.1217 0.117 Uiso 1 1 d R . . H11" H 0.4783 0.0545 0.1056 0.117 Uiso 1 1 d R . . N1 N 0.3995(7) 0.2799(5) 0.4320(5) 0.0417(15) Uani 1 1 d . . . N2 N 0.1367(8) 0.1675(5) 0.4372(5) 0.0436(16) Uani 1 1 d . . . N3 N 0.2723(9) 0.2071(6) 0.6481(5) 0.0506(18) Uani 1 1 d . . . N4 N 0.5117(8) 0.3895(5) 0.6532(5) 0.0457(16) Uani 1 1 d . . . C1 C 0.2917(9) 0.1991(6) 0.3373(6) 0.0385(17) Uani 1 1 d . . . C2 C 0.1396(9) 0.1296(6) 0.3430(6) 0.0414(18) Uani 1 1 d . . . C3 C 0.0012(10) 0.1445(6) 0.4532(6) 0.0451(19) Uani 1 1 d . . . C4 C -0.1342(10) 0.1287(7) 0.3714(8) 0.056(2) Uani 1 1 d . . . H4 H -0.1365 0.1282 0.3038 0.068 Uiso 1 1 calc R . . C5 C -0.2658(12) 0.1137(9) 0.3908(9) 0.072(3) Uani 1 1 d . . . H5 H -0.3548 0.1025 0.3358 0.087 Uiso 1 1 calc R . . C6 C -0.2639(14) 0.1155(10) 0.4904(10) 0.080(3) Uani 1 1 d . . . H6 H -0.3504 0.1079 0.5034 0.096 Uiso 1 1 calc R . . C7 C -0.1326(12) 0.1287(8) 0.5714(9) 0.069(3) Uani 1 1 d . . . H7 H -0.1330 0.1256 0.6377 0.083 Uiso 1 1 calc R . . C8 C 0.0000(11) 0.1466(7) 0.5541(7) 0.053(2) Uani 1 1 d . . . C9 C 0.1375(11) 0.1597(7) 0.6417(7) 0.053(2) Uani 1 1 d . . . H9 H 0.1241 0.1308 0.6967 0.064 Uiso 1 1 calc R . . C10 C 0.3979(12) 0.2057(8) 0.7389(7) 0.067(3) Uani 1 1 d . . . H10A H 0.4524 0.1663 0.7105 0.081 Uiso 1 1 calc R . . H10B H 0.3546 0.1596 0.7789 0.081 Uiso 1 1 calc R . . C11 C 0.5085(13) 0.3318(10) 0.8134(8) 0.079(3) Uani 1 1 d . . . H11B H 0.6106 0.3350 0.8405 0.095 Uiso 1 1 calc R . . H11A H 0.4823 0.3504 0.8741 0.095 Uiso 1 1 calc R . . C12 C 0.5069(12) 0.4258(8) 0.7578(7) 0.066(3) Uani 1 1 d . . . H12A H 0.4153 0.4390 0.7490 0.079 Uiso 1 1 calc R . . H12B H 0.5940 0.5014 0.8026 0.079 Uiso 1 1 calc R . . C13 C 0.6243(10) 0.4573(7) 0.6379(7) 0.052(2) Uani 1 1 d . . . H13 H 0.6984 0.5235 0.6967 0.063 Uiso 1 1 calc R . . C14 C 0.6502(9) 0.4434(7) 0.5409(7) 0.0452(19) Uani 1 1 d . . . C15 C 0.7910(10) 0.5259(7) 0.5504(7) 0.056(2) Uani 1 1 d . . . H15 H 0.8576 0.5849 0.6163 0.067 Uiso 1 1 calc R . . C16 C 0.8330(10) 0.5217(8) 0.4650(8) 0.059(2) Uani 1 1 d . . . H16 H 0.9270 0.5764 0.4729 0.071 Uiso 1 1 calc R . . C17 C 0.7336(11) 0.4354(9) 0.3685(8) 0.065(3) Uani 1 1 d . . . H17 H 0.7608 0.4311 0.3104 0.078 Uiso 1 1 calc R . . C18 C 0.5896(10) 0.3523(8) 0.3555(7) 0.056(2) Uani 1 1 d . . . H18 H 0.5240 0.2942 0.2890 0.067 Uiso 1 1 calc R . . C19 C 0.5447(9) 0.3565(6) 0.4406(6) 0.0418(18) Uani 1 1 d . . . C20 C 0.6785(8) 0.3404(6) 0.0842(6) 0.0333(16) Uani 1 1 d . . . C21 C 0.7745(8) 0.2820(6) 0.0927(6) 0.0347(16) Uani 1 1 d . . . H21 H 0.7370 0.2002 0.0842 0.042 Uiso 1 1 calc R . . C22 C 0.9284(8) 0.3464(6) 0.1142(6) 0.0330(16) Uani 1 1 d . . . C23 C 0.9852(8) 0.4688(6) 0.1301(6) 0.0366(17) Uani 1 1 d . . . H23 H 1.0870 0.5111 0.1434 0.044 Uiso 1 1 calc R . . C24 C 0.8897(8) 0.5293(6) 0.1262(6) 0.0349(16) Uani 1 1 d . . . C25 C 0.7372(8) 0.4642(6) 0.1023(6) 0.0340(16) Uani 1 1 d . . . H25 H 0.6730 0.5037 0.0982 0.041 Uiso 1 1 calc R . . C26 C 0.5087(9) 0.2685(7) 0.0492(6) 0.0396(18) Uani 1 1 d . . . C27 C 1.0267(8) 0.2778(6) 0.1124(6) 0.0323(16) Uani 1 1 d . . . C28 C 0.9545(10) 0.6625(7) 0.1425(7) 0.0447(19) 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 Ni1 0.0501(7) 0.0426(6) 0.0248(6) 0.0066(4) 0.0118(5) 0.0118(5) Co1 0.0354(6) 0.0301(5) 0.0254(5) 0.0065(4) 0.0115(5) 0.0125(4) Co2 0.0402(6) 0.0357(5) 0.0508(7) 0.0146(5) 0.0237(6) 0.0182(5) O1 0.040(3) 0.048(3) 0.027(3) 0.004(2) 0.011(3) 0.009(3) O2 0.041(3) 0.040(3) 0.028(3) 0.005(2) 0.012(3) 0.004(3) O3 0.042(3) 0.047(3) 0.081(5) 0.018(3) 0.033(3) 0.024(3) O4 0.038(3) 0.046(3) 0.081(5) 0.010(3) 0.023(3) 0.016(3) O5 0.045(3) 0.034(3) 0.056(4) 0.014(2) 0.025(3) 0.022(3) O6 0.037(3) 0.038(3) 0.060(4) 0.013(2) 0.025(3) 0.019(2) O7 0.045(4) 0.038(3) 0.114(6) 0.028(3) 0.031(4) 0.016(3) O8 0.064(4) 0.051(3) 0.062(4) 0.029(3) 0.038(3) 0.040(3) O9 0.034(3) 0.028(2) 0.031(3) 0.009(2) 0.016(2) 0.013(2) O10 0.055(4) 0.053(3) 0.086(5) 0.040(3) 0.037(4) 0.036(3) O11 0.082(5) 0.078(4) 0.093(6) 0.032(4) 0.048(5) 0.039(4) N1 0.046(4) 0.042(3) 0.025(4) 0.004(3) 0.008(3) 0.014(3) N2 0.051(4) 0.043(3) 0.030(4) 0.008(3) 0.018(3) 0.012(3) N3 0.070(5) 0.049(4) 0.028(4) 0.013(3) 0.018(4) 0.022(4) N4 0.053(4) 0.042(3) 0.029(4) 0.006(3) 0.011(3) 0.013(3) C1 0.042(5) 0.040(4) 0.038(5) 0.016(3) 0.017(4) 0.020(4) C2 0.056(5) 0.035(4) 0.025(4) 0.009(3) 0.016(4) 0.011(4) C3 0.052(5) 0.040(4) 0.035(5) 0.005(3) 0.019(4) 0.012(4) C4 0.061(6) 0.056(5) 0.052(6) 0.011(4) 0.027(5) 0.024(5) C5 0.065(7) 0.081(7) 0.070(8) 0.016(6) 0.026(6) 0.034(6) C6 0.079(8) 0.094(8) 0.081(9) 0.022(6) 0.048(7) 0.040(7) C7 0.082(8) 0.073(6) 0.059(7) 0.018(5) 0.048(7) 0.025(6) C8 0.063(6) 0.046(5) 0.043(5) 0.004(4) 0.027(5) 0.016(4) C9 0.073(7) 0.042(4) 0.034(5) 0.010(4) 0.029(5) 0.005(5) C10 0.090(8) 0.069(6) 0.035(5) 0.017(4) 0.015(5) 0.032(6) C11 0.077(7) 0.098(8) 0.033(6) 0.013(5) 0.010(5) 0.017(6) C12 0.072(7) 0.065(6) 0.029(5) -0.001(4) 0.013(5) 0.008(5) C13 0.050(5) 0.048(5) 0.039(5) 0.005(4) 0.008(4) 0.012(4) C14 0.048(5) 0.044(4) 0.038(5) 0.012(4) 0.010(4) 0.019(4) C15 0.048(5) 0.046(5) 0.046(6) 0.003(4) 0.005(5) 0.007(4) C16 0.044(5) 0.063(6) 0.062(7) 0.023(5) 0.019(5) 0.015(5) C17 0.058(6) 0.078(6) 0.043(6) 0.015(5) 0.022(5) 0.010(5) C18 0.046(5) 0.063(5) 0.041(5) 0.012(4) 0.012(4) 0.010(4) C19 0.044(5) 0.038(4) 0.037(5) 0.014(3) 0.014(4) 0.011(4) C20 0.032(4) 0.040(4) 0.027(4) 0.006(3) 0.012(3) 0.015(3) C21 0.039(4) 0.034(4) 0.037(4) 0.010(3) 0.021(4) 0.018(3) C22 0.029(4) 0.035(4) 0.032(4) 0.006(3) 0.012(3) 0.013(3) C23 0.039(4) 0.039(4) 0.034(4) 0.011(3) 0.018(4) 0.015(3) C24 0.043(5) 0.036(4) 0.032(4) 0.010(3) 0.019(4) 0.019(4) C25 0.036(4) 0.043(4) 0.034(4) 0.014(3) 0.020(4) 0.022(3) C26 0.040(5) 0.046(4) 0.038(5) 0.016(4) 0.021(4) 0.019(4) C27 0.031(4) 0.034(4) 0.027(4) 0.002(3) 0.011(3) 0.011(3) C28 0.057(6) 0.039(4) 0.044(5) 0.014(4) 0.028(5) 0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.878(7) . ? Ni1 N2 1.884(7) . ? Ni1 N3 1.892(7) . ? Ni1 N1 1.910(6) . ? Co1 O10 2.084(5) . ? Co1 O9 2.086(5) 2 ? Co1 O9 2.089(5) . ? Co1 O2 2.091(5) . ? Co1 O5 2.097(5) 1_455 ? Co1 O1 2.113(5) . ? Co2 O8 1.944(6) 2_665 ? Co2 O9 1.946(4) . ? Co2 O3 1.949(6) . ? Co2 O6 1.975(5) 1_455 ? O1 C1 1.247(9) . ? O2 C2 1.253(9) . ? O3 C26 1.266(8) . ? O4 C26 1.237(9) . ? O5 C27 1.242(8) . ? O5 Co1 2.097(5) 1_655 ? O6 C27 1.272(8) . ? O6 Co2 1.975(5) 1_655 ? O7 C28 1.238(10) . ? O8 C28 1.292(9) . ? O8 Co2 1.944(6) 2_665 ? O9 Co1 2.086(5) 2 ? O9 H9A 0.8499 . ? O10 H10' 0.8488 . ? O10 H10" 0.8506 . ? O11 H11' 0.8500 . ? O11 H11" 0.8500 . ? N1 C1 1.347(10) . ? N1 C19 1.421(10) . ? N2 C2 1.316(9) . ? N2 C3 1.407(10) . ? N3 C9 1.267(10) . ? N3 C10 1.494(11) . ? N4 C13 1.285(10) . ? N4 C12 1.457(10) . ? C1 C2 1.537(11) . ? C3 C8 1.401(11) . ? C3 C4 1.408(12) . ? C4 C5 1.404(13) . ? C4 H4 0.9300 . ? C5 C6 1.374(15) . ? C5 H5 0.9300 . ? C6 C7 1.385(15) . ? C6 H6 0.9300 . ? C7 C8 1.395(12) . ? C7 H7 0.9300 . ? C8 C9 1.473(13) . ? C9 H9 0.9300 . ? C10 C11 1.513(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.520(14) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.441(12) . ? C13 H13 0.9300 . ? C14 C15 1.407(11) . ? C14 C19 1.411(11) . ? C15 C16 1.377(12) . ? C15 H15 0.9300 . ? C16 C17 1.365(13) . ? C16 H16 0.9300 . ? C17 C18 1.417(12) . ? C17 H17 0.9300 . ? C18 C19 1.391(11) . ? C18 H18 0.9300 . ? C20 C21 1.383(9) . ? C20 C25 1.394(9) . ? C20 C26 1.519(10) . ? C21 C22 1.402(9) . ? C21 H21 0.9300 . ? C22 C23 1.383(9) . ? C22 C27 1.513(9) . ? C23 C24 1.404(9) . ? C23 H23 0.9300 . ? C24 C25 1.384(10) . ? C24 C28 1.508(10) . ? C25 H25 0.9300 . ? 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 N4 Ni1 N2 165.8(3) . . ? N4 Ni1 N3 91.3(3) . . ? N2 Ni1 N3 90.7(3) . . ? N4 Ni1 N1 95.0(3) . . ? N2 Ni1 N1 86.7(3) . . ? N3 Ni1 N1 164.3(3) . . ? O10 Co1 O9 93.4(2) . 2 ? O10 Co1 O9 91.5(2) . . ? O9 Co1 O9 84.02(18) 2 . ? O10 Co1 O2 94.4(2) . . ? O9 Co1 O2 98.43(19) 2 . ? O9 Co1 O2 173.45(17) . . ? O10 Co1 O5 176.5(2) . 1_455 ? O9 Co1 O5 86.5(2) 2 1_455 ? O9 Co1 O5 92.02(19) . 1_455 ? O2 Co1 O5 82.1(2) . 1_455 ? O10 Co1 O1 86.9(2) . . ? O9 Co1 O1 177.69(18) 2 . ? O9 Co1 O1 98.27(19) . . ? O2 Co1 O1 79.3(2) . . ? O5 Co1 O1 93.2(2) 1_455 . ? O8 Co2 O9 120.0(2) 2_665 . ? O8 Co2 O3 104.5(2) 2_665 . ? O9 Co2 O3 116.4(2) . . ? O8 Co2 O6 102.1(2) 2_665 1_455 ? O9 Co2 O6 107.10(19) . 1_455 ? O3 Co2 O6 104.9(2) . 1_455 ? C1 O1 Co1 113.3(5) . . ? C2 O2 Co1 112.2(4) . . ? C26 O3 Co2 117.8(5) . . ? C27 O5 Co1 130.9(5) . 1_655 ? C27 O6 Co2 122.2(4) . 1_655 ? C28 O8 Co2 123.0(5) . 2_665 ? Co2 O9 Co1 122.9(2) . 2 ? Co2 O9 Co1 112.7(2) . . ? Co1 O9 Co1 95.98(18) 2 . ? Co2 O9 H9A 95.6 . . ? Co1 O9 H9A 107.5 2 . ? Co1 O9 H9A 124.5 . . ? Co1 O10 H10' 119.0 . . ? Co1 O10 H10" 122.6 . . ? H10' O10 H10" 116.2 . . ? H11' O11 H11" 117.3 . . ? C1 N1 C19 121.3(6) . . ? C1 N1 Ni1 110.8(5) . . ? C19 N1 Ni1 127.7(5) . . ? C2 N2 C3 123.4(7) . . ? C2 N2 Ni1 112.2(5) . . ? C3 N2 Ni1 124.3(5) . . ? C9 N3 C10 118.2(8) . . ? C9 N3 Ni1 127.0(6) . . ? C10 N3 Ni1 114.3(6) . . ? C13 N4 C12 117.9(7) . . ? C13 N4 Ni1 125.1(6) . . ? C12 N4 Ni1 116.0(6) . . ? O1 C1 N1 130.1(7) . . ? O1 C1 C2 116.1(7) . . ? N1 C1 C2 113.5(7) . . ? O2 C2 N2 128.3(7) . . ? O2 C2 C1 118.1(6) . . ? N2 C2 C1 113.6(7) . . ? C8 C3 N2 120.8(8) . . ? C8 C3 C4 117.6(8) . . ? N2 C3 C4 121.4(7) . . ? C5 C4 C3 120.7(9) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.4(10) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.8(10) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.4(10) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 121.0(9) . . ? C7 C8 C9 119.0(8) . . ? C3 C8 C9 119.9(8) . . ? N3 C9 C8 125.1(8) . . ? N3 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? N3 C10 C11 111.7(8) . . ? N3 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 112.1(8) . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? H11B C11 H11A 107.9 . . ? N4 C12 C11 112.1(8) . . ? N4 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N4 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C14 128.0(8) . . ? N4 C13 H13 116.0 . . ? C14 C13 H13 116.0 . . ? C15 C14 C19 120.0(8) . . ? C15 C14 C13 115.4(8) . . ? C19 C14 C13 124.6(8) . . ? C16 C15 C14 121.9(8) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C17 C16 C15 118.5(8) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 C18 121.1(9) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 121.0(8) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C14 117.4(7) . . ? C18 C19 N1 124.0(7) . . ? C14 C19 N1 118.6(7) . . ? C21 C20 C25 119.7(6) . . ? C21 C20 C26 119.9(6) . . ? C25 C20 C26 120.3(6) . . ? C20 C21 C22 119.9(6) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.1(6) . . ? C23 C22 C27 121.2(6) . . ? C21 C22 C27 118.6(6) . . ? C22 C23 C24 120.1(6) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.2(6) . . ? C25 C24 C28 121.9(6) . . ? C23 C24 C28 118.8(6) . . ? C24 C25 C20 120.9(6) . . ? C24 C25 H25 119.5 . . ? C20 C25 H25 119.5 . . ? O4 C26 O3 123.8(7) . . ? O4 C26 C20 120.1(6) . . ? O3 C26 C20 116.0(6) . . ? O5 C27 O6 126.3(6) . . ? O5 C27 C22 118.3(6) . . ? O6 C27 C22 115.4(6) . . ? O7 C28 O8 124.5(7) . . ? O7 C28 C24 119.6(7) . . ? O8 C28 C24 116.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Co1 O1 C1 -98.5(5) . . . . ? O9 Co1 O1 C1 -3(5) 2 . . . ? O9 Co1 O1 C1 170.5(5) . . . . ? O2 Co1 O1 C1 -3.4(5) . . . . ? O5 Co1 O1 C1 78.0(5) 1_455 . . . ? O10 Co1 O2 C2 94.4(5) . . . . ? O9 Co1 O2 C2 -171.6(5) 2 . . . ? O9 Co1 O2 C2 -60.0(19) . . . . ? O5 Co1 O2 C2 -86.4(5) 1_455 . . . ? O1 Co1 O2 C2 8.4(5) . . . . ? O8 Co2 O3 C26 -105.4(6) 2_665 . . . ? O9 Co2 O3 C26 29.4(6) . . . . ? O6 Co2 O3 C26 147.6(5) 1_455 . . . ? O8 Co2 O9 Co1 -24.2(3) 2_665 . . 2 ? O3 Co2 O9 Co1 -151.7(3) . . . 2 ? O6 Co2 O9 Co1 91.3(3) 1_455 . . 2 ? O8 Co2 O9 Co1 -138.1(2) 2_665 . . . ? O3 Co2 O9 Co1 94.4(3) . . . . ? O6 Co2 O9 Co1 -22.6(3) 1_455 . . . ? O10 Co1 O9 Co2 -137.3(3) . . . . ? O9 Co1 O9 Co2 129.5(3) 2 . . . ? O2 Co1 O9 Co2 17.2(18) . . . . ? O5 Co1 O9 Co2 43.3(3) 1_455 . . . ? O1 Co1 O9 Co2 -50.2(3) . . . . ? O10 Co1 O9 Co1 93.2(2) . . . 2 ? O9 Co1 O9 Co1 0.0 2 . . 2 ? O2 Co1 O9 Co1 -112.3(17) . . . 2 ? O5 Co1 O9 Co1 -86.2(2) 1_455 . . 2 ? O1 Co1 O9 Co1 -179.72(18) . . . 2 ? N4 Ni1 N1 C1 -179.5(5) . . . . ? N2 Ni1 N1 C1 -13.6(5) . . . . ? N3 Ni1 N1 C1 67.2(13) . . . . ? N4 Ni1 N1 C19 5.9(6) . . . . ? N2 Ni1 N1 C19 171.8(6) . . . . ? N3 Ni1 N1 C19 -107.4(11) . . . . ? N4 Ni1 N2 C2 114.3(11) . . . . ? N3 Ni1 N2 C2 -147.7(5) . . . . ? N1 Ni1 N2 C2 16.8(5) . . . . ? N4 Ni1 N2 C3 -62.0(14) . . . . ? N3 Ni1 N2 C3 36.0(6) . . . . ? N1 Ni1 N2 C3 -159.5(6) . . . . ? N4 Ni1 N3 C9 145.3(7) . . . . ? N2 Ni1 N3 C9 -20.7(7) . . . . ? N1 Ni1 N3 C9 -100.9(12) . . . . ? N4 Ni1 N3 C10 -42.8(6) . . . . ? N2 Ni1 N3 C10 151.3(6) . . . . ? N1 Ni1 N3 C10 71.0(13) . . . . ? N2 Ni1 N4 C13 -93.5(13) . . . . ? N3 Ni1 N4 C13 168.6(7) . . . . ? N1 Ni1 N4 C13 3.0(7) . . . . ? N2 Ni1 N4 C12 74.4(13) . . . . ? N3 Ni1 N4 C12 -23.5(6) . . . . ? N1 Ni1 N4 C12 170.8(6) . . . . ? Co1 O1 C1 N1 -174.4(6) . . . . ? Co1 O1 C1 C2 -1.4(7) . . . . ? C19 N1 C1 O1 -3.7(12) . . . . ? Ni1 N1 C1 O1 -178.7(6) . . . . ? C19 N1 C1 C2 -176.8(6) . . . . ? Ni1 N1 C1 C2 8.1(7) . . . . ? Co1 O2 C2 N2 166.4(7) . . . . ? Co1 O2 C2 C1 -11.8(8) . . . . ? C3 N2 C2 O2 -17.8(12) . . . . ? Ni1 N2 C2 O2 165.9(7) . . . . ? C3 N2 C2 C1 160.4(7) . . . . ? Ni1 N2 C2 C1 -15.9(8) . . . . ? O1 C1 C2 O2 9.3(10) . . . . ? N1 C1 C2 O2 -176.5(6) . . . . ? O1 C1 C2 N2 -169.1(6) . . . . ? N1 C1 C2 N2 5.1(9) . . . . ? C2 N2 C3 C8 156.7(7) . . . . ? Ni1 N2 C3 C8 -27.5(10) . . . . ? C2 N2 C3 C4 -28.7(11) . . . . ? Ni1 N2 C3 C4 147.2(6) . . . . ? C8 C3 C4 C5 -1.0(12) . . . . ? N2 C3 C4 C5 -175.8(8) . . . . ? C3 C4 C5 C6 0.7(14) . . . . ? C4 C5 C6 C7 -1.9(16) . . . . ? C5 C6 C7 C8 3.4(16) . . . . ? C6 C7 C8 C3 -3.8(14) . . . . ? C6 C7 C8 C9 -179.7(9) . . . . ? N2 C3 C8 C7 177.4(8) . . . . ? C4 C3 C8 C7 2.5(12) . . . . ? N2 C3 C8 C9 -6.8(11) . . . . ? C4 C3 C8 C9 178.4(7) . . . . ? C10 N3 C9 C8 -176.0(8) . . . . ? Ni1 N3 C9 C8 -4.4(12) . . . . ? C7 C8 C9 N3 -160.1(8) . . . . ? C3 C8 C9 N3 23.9(12) . . . . ? C9 N3 C10 C11 -115.7(9) . . . . ? Ni1 N3 C10 C11 71.6(9) . . . . ? N3 C10 C11 C12 -23.9(12) . . . . ? C13 N4 C12 C11 -119.9(9) . . . . ? Ni1 N4 C12 C11 71.3(10) . . . . ? C10 C11 C12 N4 -46.1(12) . . . . ? C12 N4 C13 C14 -176.9(8) . . . . ? Ni1 N4 C13 C14 -9.3(12) . . . . ? N4 C13 C14 C15 -174.5(8) . . . . ? N4 C13 C14 C19 6.6(14) . . . . ? C19 C14 C15 C16 -2.7(13) . . . . ? C13 C14 C15 C16 178.4(8) . . . . ? C14 C15 C16 C17 0.7(14) . . . . ? C15 C16 C17 C18 0.6(14) . . . . ? C16 C17 C18 C19 0.2(14) . . . . ? C17 C18 C19 C14 -2.2(12) . . . . ? C17 C18 C19 N1 176.9(8) . . . . ? C15 C14 C19 C18 3.4(11) . . . . ? C13 C14 C19 C18 -177.8(8) . . . . ? C15 C14 C19 N1 -175.7(7) . . . . ? C13 C14 C19 N1 3.0(11) . . . . ? C1 N1 C19 C18 -2.2(11) . . . . ? Ni1 N1 C19 C18 171.9(6) . . . . ? C1 N1 C19 C14 176.9(7) . . . . ? Ni1 N1 C19 C14 -9.0(10) . . . . ? C25 C20 C21 C22 -3.2(10) . . . . ? C26 C20 C21 C22 173.4(7) . . . . ? C20 C21 C22 C23 2.0(10) . . . . ? C20 C21 C22 C27 -174.2(6) . . . . ? C21 C22 C23 C24 0.8(10) . . . . ? C27 C22 C23 C24 176.9(6) . . . . ? C22 C23 C24 C25 -2.4(10) . . . . ? C22 C23 C24 C28 -179.2(7) . . . . ? C23 C24 C25 C20 1.2(10) . . . . ? C28 C24 C25 C20 177.9(7) . . . . ? C21 C20 C25 C24 1.6(10) . . . . ? C26 C20 C25 C24 -175.0(7) . . . . ? Co2 O3 C26 O4 -6.4(10) . . . . ? Co2 O3 C26 C20 172.2(5) . . . . ? C21 C20 C26 O4 -13.0(11) . . . . ? C25 C20 C26 O4 163.6(7) . . . . ? C21 C20 C26 O3 168.4(7) . . . . ? C25 C20 C26 O3 -15.1(10) . . . . ? Co1 O5 C27 O6 2.7(11) 1_655 . . . ? Co1 O5 C27 C22 -179.7(4) 1_655 . . . ? Co2 O6 C27 O5 40.9(10) 1_655 . . . ? Co2 O6 C27 C22 -136.8(5) 1_655 . . . ? C23 C22 C27 O5 164.4(7) . . . . ? C21 C22 C27 O5 -19.5(10) . . . . ? C23 C22 C27 O6 -17.8(10) . . . . ? C21 C22 C27 O6 158.4(7) . . . . ? Co2 O8 C28 O7 74.7(10) 2_665 . . . ? Co2 O8 C28 C24 -105.1(6) 2_665 . . . ? C25 C24 C28 O7 176.3(8) . . . . ? C23 C24 C28 O7 -7.0(11) . . . . ? C25 C24 C28 O8 -4.0(11) . . . . ? C23 C24 C28 O8 172.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.590 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.171 #===End data_91208c _database_code_depnum_ccdc_archive 'CCDC 800817' #TrackingRef '- 100110C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Cu N4 O11 Zn2' _chemical_formula_weight 786.79 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' Cu Cu 0.3201 1.2651 '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 10.1376(6) _cell_length_b 12.3611(8) _cell_length_c 13.8352(8) _cell_angle_alpha 100.5220(10) _cell_angle_beta 107.4860(10) _cell_angle_gamma 109.1880(10) _cell_volume 1483.59(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4748 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.81 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 2.382 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6472 _exptl_absorpt_correction_T_max 0.8323 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _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_% ? _diffrn_reflns_number 7594 _diffrn_reflns_av_R_equivalents 0.0115 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5196 _reflns_number_gt 4404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0337P)^2^+1.0381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5196 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.16932(4) 0.23395(3) -0.04447(3) 0.03981(11) Uani 1 1 d . . . Zn1 Zn 0.41887(3) 0.44846(3) 0.37712(2) 0.02889(9) Uani 1 1 d . . . Zn2 Zn 0.28280(3) 0.25279(3) 0.49456(3) 0.03085(9) Uani 1 1 d . . . O1 O 0.2089(2) 0.31161(19) 0.25692(15) 0.0412(5) Uani 1 1 d . . . O2 O 0.4649(2) 0.44512(18) 0.24109(15) 0.0415(5) Uani 1 1 d . . . O3 O 0.0649(2) 0.16498(18) 0.44321(18) 0.0435(5) Uani 1 1 d . . . O4 O 0.0442(2) 0.33795(19) 0.48701(19) 0.0484(6) Uani 1 1 d . . . O5 O -0.3610(2) -0.21652(18) 0.37373(16) 0.0402(5) Uani 1 1 d . . . O6 O -0.5923(3) -0.21990(19) 0.3330(2) 0.0628(7) Uani 1 1 d . . . O7 O -0.6470(2) 0.16531(17) 0.40252(16) 0.0349(4) Uani 1 1 d . . . O8 O -0.4775(2) 0.32458(17) 0.38705(17) 0.0380(5) Uani 1 1 d . . . O9 O 0.36921(19) 0.42288(15) 0.50889(13) 0.0256(4) Uani 1 1 d . . . H9A H 0.3019 0.4476 0.5140 0.038 Uiso 1 1 d R . . O10 O 0.3156(2) 0.5656(2) 0.3573(2) 0.0523(6) Uani 1 1 d . . . H10" H 0.3615 0.6321 0.3488 0.079 Uiso 1 1 d R . . H10' H 0.2263 0.5500 0.3549 0.079 Uiso 1 1 d R . . O11 O 0.0366(3) 0.5072(2) 0.3754(2) 0.0703(7) Uani 1 1 d . . . H11" H 0.0338 0.4496 0.4011 0.105 Uiso 1 1 d R . . H11' H 0.0116 0.5599 0.4041 0.105 Uiso 1 1 d R . . N1 N 0.0984(3) 0.2229(2) 0.07220(18) 0.0375(6) Uani 1 1 d . . . N2 N 0.3686(3) 0.3259(2) 0.06545(18) 0.0397(6) Uani 1 1 d . . . N3 N 0.2347(3) 0.2973(2) -0.15081(19) 0.0464(7) Uani 1 1 d . . . N4 N -0.0125(3) 0.1055(2) -0.15216(19) 0.0463(7) Uani 1 1 d . . . C1 C 0.2105(3) 0.2962(3) 0.1661(2) 0.0353(6) Uani 1 1 d . . . C2 C 0.3623(3) 0.3642(3) 0.1590(2) 0.0352(6) Uani 1 1 d . . . C3 C 0.5059(3) 0.3555(3) 0.0501(2) 0.0414(7) Uani 1 1 d . . . C4 C 0.6411(4) 0.3732(3) 0.1295(3) 0.0526(8) Uani 1 1 d . . . H4 H 0.6442 0.3724 0.1972 0.063 Uiso 1 1 calc R . . C5 C 0.7702(4) 0.3917(4) 0.1088(3) 0.0684(11) Uani 1 1 d . . . H5 H 0.8589 0.4019 0.1624 0.082 Uiso 1 1 calc R . . C6 C 0.7698(5) 0.3954(4) 0.0100(4) 0.0771(13) Uani 1 1 d . . . H6 H 0.8575 0.4082 -0.0032 0.093 Uiso 1 1 calc R . . C7 C 0.6389(5) 0.3801(4) -0.0689(3) 0.0651(11) Uani 1 1 d . . . H7 H 0.6392 0.3844 -0.1352 0.078 Uiso 1 1 calc R . . C8 C 0.5045(4) 0.3582(3) -0.0517(3) 0.0462(8) Uani 1 1 d . . . C9 C 0.3715(4) 0.3418(3) -0.1417(2) 0.0494(8) Uani 1 1 d . . . H9 H 0.3887 0.3664 -0.1981 0.059 Uiso 1 1 calc R . . C10 C 0.1167(5) 0.2927(4) -0.2470(3) 0.0692(11) Uani 1 1 d . . . H10A H 0.1643 0.3228 -0.2935 0.083 Uiso 1 1 calc R . . H10B H 0.0716 0.3463 -0.2258 0.083 Uiso 1 1 calc R . . C11 C -0.0060(5) 0.1705(5) -0.3084(3) 0.0982(18) Uani 1 1 d . . . H11A H -0.1022 0.1773 -0.3234 0.118 Uiso 1 1 calc R . . H11B H 0.0019 0.1455 -0.3763 0.118 Uiso 1 1 calc R . . C12 C -0.0111(5) 0.0729(4) -0.2595(3) 0.0747(13) Uani 1 1 d . . . H12A H -0.1013 0.0006 -0.3049 0.090 Uiso 1 1 calc R . . H12B H 0.0764 0.0550 -0.2551 0.090 Uiso 1 1 calc R . . C13 C -0.1250(4) 0.0415(3) -0.1350(3) 0.0486(8) Uani 1 1 d . . . H13 H -0.2010 -0.0234 -0.1928 0.058 Uiso 1 1 calc R . . C14 C -0.1489(3) 0.0577(3) -0.0357(2) 0.0410(7) Uani 1 1 d . . . C15 C -0.2891(4) -0.0233(3) -0.0428(3) 0.0523(9) Uani 1 1 d . . . H15 H -0.3559 -0.0813 -0.1080 0.063 Uiso 1 1 calc R . . C16 C -0.3308(4) -0.0201(3) 0.0411(3) 0.0605(10) Uani 1 1 d . . . H16 H -0.4224 -0.0770 0.0348 0.073 Uiso 1 1 calc R . . C17 C -0.2338(4) 0.0699(4) 0.1369(3) 0.0662(11) Uani 1 1 d . . . H17 H -0.2631 0.0762 0.1945 0.079 Uiso 1 1 calc R . . C18 C -0.0946(4) 0.1501(3) 0.1477(3) 0.0580(10) Uani 1 1 d . . . H18 H -0.0312 0.2089 0.2132 0.070 Uiso 1 1 calc R . . C19 C -0.0454(3) 0.1459(3) 0.0635(2) 0.0386(7) Uani 1 1 d . . . C20 C -0.1781(3) 0.1556(2) 0.4190(2) 0.0276(6) Uani 1 1 d . . . C21 C -0.2373(3) 0.0314(2) 0.4010(2) 0.0306(6) Uani 1 1 d . . . H21 H -0.1735 -0.0086 0.4057 0.037 Uiso 1 1 calc R . . C22 C -0.3903(3) -0.0332(2) 0.3762(2) 0.0282(6) Uani 1 1 d . . . C23 C -0.4841(3) 0.0286(2) 0.3722(2) 0.0285(6) Uani 1 1 d . . . H23 H -0.5861 -0.0134 0.3579 0.034 Uiso 1 1 calc R . . C24 C -0.4264(3) 0.1517(2) 0.3895(2) 0.0264(5) Uani 1 1 d . . . C25 C -0.2738(3) 0.2148(2) 0.4111(2) 0.0281(6) Uani 1 1 d . . . H25 H -0.2358 0.2971 0.4204 0.034 Uiso 1 1 calc R . . C26 C -0.0119(3) 0.2260(3) 0.4511(2) 0.0316(6) Uani 1 1 d . . . C27 C -0.4546(3) -0.1663(3) 0.3596(2) 0.0368(7) Uani 1 1 d . . . C28 C -0.5236(3) 0.2203(2) 0.3924(2) 0.0280(6) 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 Cu1 0.0409(2) 0.0387(2) 0.02419(18) 0.00408(15) 0.00814(16) 0.00490(17) Zn1 0.03008(17) 0.02595(17) 0.02461(16) 0.00574(13) 0.00852(13) 0.00735(13) Zn2 0.02500(17) 0.02240(16) 0.0468(2) 0.01088(14) 0.01804(15) 0.00792(13) O1 0.0418(12) 0.0432(12) 0.0260(10) 0.0060(9) 0.0112(9) 0.0069(10) O2 0.0420(12) 0.0380(12) 0.0267(10) 0.0038(9) 0.0092(9) 0.0024(10) O3 0.0248(10) 0.0373(12) 0.0698(15) 0.0131(10) 0.0223(10) 0.0128(9) O4 0.0281(11) 0.0338(12) 0.0772(16) 0.0116(11) 0.0207(11) 0.0082(9) O5 0.0530(13) 0.0382(11) 0.0501(12) 0.0237(10) 0.0293(11) 0.0294(10) O6 0.0409(13) 0.0302(12) 0.119(2) 0.0291(13) 0.0330(14) 0.0112(10) O7 0.0247(10) 0.0285(10) 0.0508(12) 0.0068(9) 0.0195(9) 0.0088(8) O8 0.0337(11) 0.0274(11) 0.0591(13) 0.0139(9) 0.0239(10) 0.0145(9) O9 0.0241(9) 0.0213(9) 0.0326(10) 0.0071(8) 0.0131(8) 0.0094(7) O10 0.0427(12) 0.0429(13) 0.0853(17) 0.0362(12) 0.0305(12) 0.0202(11) O11 0.0795(19) 0.0645(17) 0.0837(19) 0.0288(15) 0.0443(16) 0.0348(15) N1 0.0370(13) 0.0344(13) 0.0274(12) 0.0049(10) 0.0073(11) 0.0056(11) N2 0.0402(14) 0.0393(14) 0.0261(12) 0.0051(11) 0.0097(11) 0.0061(11) N3 0.0571(18) 0.0413(15) 0.0282(13) 0.0081(11) 0.0119(13) 0.0107(13) N4 0.0478(16) 0.0454(16) 0.0265(13) 0.0031(11) 0.0075(12) 0.0071(13) C1 0.0418(16) 0.0313(15) 0.0279(15) 0.0084(12) 0.0114(13) 0.0115(13) C2 0.0391(16) 0.0303(15) 0.0273(15) 0.0092(12) 0.0076(13) 0.0084(13) C3 0.0433(18) 0.0318(16) 0.0391(17) 0.0037(13) 0.0164(14) 0.0070(14) C4 0.049(2) 0.051(2) 0.048(2) 0.0088(16) 0.0161(17) 0.0152(17) C5 0.050(2) 0.072(3) 0.070(3) 0.009(2) 0.016(2) 0.023(2) C6 0.058(3) 0.087(3) 0.084(3) 0.013(3) 0.037(2) 0.023(2) C7 0.068(3) 0.063(2) 0.059(2) 0.0095(19) 0.038(2) 0.014(2) C8 0.0515(19) 0.0352(17) 0.0408(18) 0.0034(14) 0.0218(16) 0.0058(15) C9 0.066(2) 0.0385(18) 0.0331(17) 0.0079(14) 0.0229(17) 0.0079(17) C10 0.087(3) 0.063(3) 0.039(2) 0.0161(18) 0.005(2) 0.027(2) C11 0.077(3) 0.123(4) 0.043(2) 0.035(3) -0.004(2) -0.002(3) C12 0.075(3) 0.065(3) 0.0331(19) -0.0123(18) 0.0179(19) -0.015(2) C13 0.0406(18) 0.0438(19) 0.0356(17) 0.0020(14) 0.0036(14) 0.0024(15) C14 0.0376(16) 0.0372(17) 0.0373(17) 0.0087(13) 0.0086(14) 0.0091(14) C15 0.0405(18) 0.047(2) 0.048(2) 0.0096(16) 0.0082(16) 0.0039(15) C16 0.043(2) 0.062(2) 0.060(2) 0.0182(19) 0.0185(18) 0.0052(18) C17 0.053(2) 0.080(3) 0.051(2) 0.016(2) 0.0255(19) 0.009(2) C18 0.049(2) 0.066(2) 0.0386(19) 0.0061(17) 0.0152(16) 0.0057(18) C19 0.0377(16) 0.0376(17) 0.0340(16) 0.0106(13) 0.0100(13) 0.0114(14) C20 0.0252(13) 0.0310(14) 0.0287(14) 0.0106(11) 0.0134(11) 0.0107(11) C21 0.0305(14) 0.0368(15) 0.0338(15) 0.0135(12) 0.0173(12) 0.0190(12) C22 0.0301(14) 0.0258(14) 0.0315(14) 0.0110(11) 0.0143(12) 0.0114(11) C23 0.0221(13) 0.0292(14) 0.0326(14) 0.0092(12) 0.0112(11) 0.0081(11) C24 0.0215(12) 0.0285(14) 0.0285(14) 0.0069(11) 0.0099(11) 0.0102(11) C25 0.0261(13) 0.0244(13) 0.0329(14) 0.0082(11) 0.0135(11) 0.0079(11) C26 0.0271(14) 0.0370(16) 0.0358(15) 0.0139(13) 0.0169(12) 0.0135(13) C27 0.0410(17) 0.0297(15) 0.0454(17) 0.0160(13) 0.0211(14) 0.0151(14) C28 0.0231(13) 0.0256(14) 0.0283(14) 0.0020(11) 0.0078(11) 0.0072(11) _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 Cu1 N2 1.923(2) . ? Cu1 N4 1.924(2) . ? Cu1 N1 1.963(2) . ? Cu1 N3 1.970(3) . ? Zn1 O10 2.058(2) . ? Zn1 O2 2.0674(19) . ? Zn1 O9 2.0820(17) . ? Zn1 O9 2.1057(17) 2_666 ? Zn1 O8 2.1245(19) 1_655 ? Zn1 O1 2.153(2) . ? Zn1 Zn1 3.0934(6) 2_666 ? Zn2 O9 1.9390(17) . ? Zn2 O3 1.9391(19) . ? Zn2 O5 1.953(2) 2_556 ? Zn2 O7 1.9608(18) 1_655 ? O1 C1 1.242(3) . ? O2 C2 1.250(3) . ? O3 C26 1.263(3) . ? O4 C26 1.244(3) . ? O5 C27 1.281(3) . ? O5 Zn2 1.953(2) 2_556 ? O6 C27 1.232(4) . ? O7 C28 1.276(3) . ? O7 Zn2 1.9608(18) 1_455 ? O8 C28 1.243(3) . ? O8 Zn1 2.1245(19) 1_455 ? O9 Zn1 2.1057(17) 2_666 ? O9 H9A 0.8497 . ? O10 H10" 0.8502 . ? O10 H10' 0.8504 . ? O11 H11" 0.8493 . ? O11 H11' 0.8497 . ? N1 C1 1.344(4) . ? N1 C19 1.409(4) . ? N2 C2 1.323(4) . ? N2 C3 1.410(4) . ? N3 C9 1.269(4) . ? N3 C10 1.476(4) . ? N4 C13 1.274(4) . ? N4 C12 1.472(4) . ? C1 C2 1.535(4) . ? C3 C4 1.395(5) . ? C3 C8 1.411(4) . ? C4 C5 1.378(5) . ? C4 H4 0.9300 . ? C5 C6 1.375(6) . ? C5 H5 0.9300 . ? C6 C7 1.370(6) . ? C6 H6 0.9300 . ? C7 C8 1.400(5) . ? C7 H7 0.9300 . ? C8 C9 1.458(5) . ? C9 H9 0.9300 . ? C10 C11 1.487(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.480(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.454(4) . ? C13 H13 0.9300 . ? C14 C15 1.407(4) . ? C14 C19 1.418(4) . ? C15 C16 1.347(5) . ? C15 H15 0.9300 . ? C16 C17 1.386(5) . ? C16 H16 0.9300 . ? C17 C18 1.377(5) . ? C17 H17 0.9300 . ? C18 C19 1.397(4) . ? C18 H18 0.9300 . ? C20 C25 1.386(4) . ? C20 C21 1.394(4) . ? C20 C26 1.496(4) . ? C21 C22 1.389(4) . ? C21 H21 0.9300 . ? C22 C23 1.396(4) . ? C22 C27 1.501(4) . ? C23 C24 1.383(4) . ? C23 H23 0.9300 . ? C24 C25 1.391(3) . ? C24 C28 1.501(3) . ? C25 H25 0.9300 . ? 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 N2 Cu1 N4 163.91(12) . . ? N2 Cu1 N1 86.09(10) . . ? N4 Cu1 N1 94.82(10) . . ? N2 Cu1 N3 91.48(11) . . ? N4 Cu1 N3 92.79(11) . . ? N1 Cu1 N3 160.70(11) . . ? O10 Zn1 O2 94.38(9) . . ? O10 Zn1 O9 93.58(8) . . ? O2 Zn1 O9 170.63(8) . . ? O10 Zn1 O9 96.87(8) . 2_666 ? O2 Zn1 O9 99.16(7) . 2_666 ? O9 Zn1 O9 84.76(7) . 2_666 ? O10 Zn1 O8 176.35(9) . 1_655 ? O2 Zn1 O8 82.24(8) . 1_655 ? O9 Zn1 O8 89.68(7) . 1_655 ? O9 Zn1 O8 85.07(7) 2_666 1_655 ? O10 Zn1 O1 85.82(9) . . ? O2 Zn1 O1 78.71(8) . . ? O9 Zn1 O1 96.97(7) . . ? O9 Zn1 O1 176.72(7) 2_666 . ? O8 Zn1 O1 92.15(8) 1_655 . ? O10 Zn1 Zn1 97.09(7) . 2_666 ? O2 Zn1 Zn1 140.58(6) . 2_666 ? O9 Zn1 Zn1 42.68(5) . 2_666 ? O9 Zn1 Zn1 42.09(5) 2_666 2_666 ? O8 Zn1 Zn1 86.43(6) 1_655 2_666 ? O1 Zn1 Zn1 139.58(5) . 2_666 ? O9 Zn2 O3 120.14(8) . . ? O9 Zn2 O5 113.59(8) . 2_556 ? O3 Zn2 O5 104.06(9) . 2_556 ? O9 Zn2 O7 109.39(7) . 1_655 ? O3 Zn2 O7 106.98(8) . 1_655 ? O5 Zn2 O7 100.76(8) 2_556 1_655 ? C1 O1 Zn1 112.23(18) . . ? C2 O2 Zn1 113.97(18) . . ? C26 O3 Zn2 117.22(18) . . ? C27 O5 Zn2 122.52(18) . 2_556 ? C28 O7 Zn2 120.20(17) . 1_455 ? C28 O8 Zn1 131.60(17) . 1_455 ? Zn2 O9 Zn1 110.95(8) . . ? Zn2 O9 Zn1 125.83(9) . 2_666 ? Zn1 O9 Zn1 95.24(7) . 2_666 ? Zn2 O9 H9A 105.0 . . ? Zn1 O9 H9A 111.3 . . ? Zn1 O9 H9A 108.2 2_666 . ? Zn1 O10 H10" 119.9 . . ? Zn1 O10 H10' 123.1 . . ? H10" O10 H10' 117.0 . . ? H11" O11 H11' 117.1 . . ? C1 N1 C19 122.9(2) . . ? C1 N1 Cu1 110.32(19) . . ? C19 N1 Cu1 126.69(19) . . ? C2 N2 C3 122.9(2) . . ? C2 N2 Cu1 111.4(2) . . ? C3 N2 Cu1 125.56(19) . . ? C9 N3 C10 118.1(3) . . ? C9 N3 Cu1 124.2(2) . . ? C10 N3 Cu1 117.7(2) . . ? C13 N4 C12 118.9(3) . . ? C13 N4 Cu1 125.0(2) . . ? C12 N4 Cu1 115.8(2) . . ? O1 C1 N1 128.8(3) . . ? O1 C1 C2 116.5(2) . . ? N1 C1 C2 114.7(2) . . ? O2 C2 N2 128.0(3) . . ? O2 C2 C1 117.5(2) . . ? N2 C2 C1 114.4(2) . . ? C4 C3 N2 122.4(3) . . ? C4 C3 C8 118.5(3) . . ? N2 C3 C8 118.9(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 119.4(4) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 121.4(4) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 119.0(3) . . ? C7 C8 C9 116.7(3) . . ? C3 C8 C9 124.3(3) . . ? N3 C9 C8 126.5(3) . . ? N3 C9 H9 116.7 . . ? C8 C9 H9 116.7 . . ? N3 C10 C11 114.4(3) . . ? N3 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N3 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 118.0(3) . . ? C12 C11 H11A 107.8 . . ? C10 C11 H11A 107.8 . . ? C12 C11 H11B 107.8 . . ? C10 C11 H11B 107.8 . . ? H11A C11 H11B 107.1 . . ? N4 C12 C11 112.2(4) . . ? N4 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? N4 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C14 127.7(3) . . ? N4 C13 H13 116.1 . . ? C14 C13 H13 116.1 . . ? C15 C14 C19 119.2(3) . . ? C15 C14 C13 114.8(3) . . ? C19 C14 C13 126.0(3) . . ? C16 C15 C14 122.7(3) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 118.4(3) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 122.1(3) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C18 C19 N1 124.1(3) . . ? C18 C19 C14 116.6(3) . . ? N1 C19 C14 119.3(3) . . ? C25 C20 C21 119.4(2) . . ? C25 C20 C26 119.9(2) . . ? C21 C20 C26 120.7(2) . . ? C22 C21 C20 120.8(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.0(2) . . ? C21 C22 C27 121.3(2) . . ? C23 C22 C27 119.6(2) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.9(2) . . ? C23 C24 C28 121.1(2) . . ? C25 C24 C28 119.0(2) . . ? C20 C25 C24 120.3(2) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? O4 C26 O3 123.6(2) . . ? O4 C26 C20 120.2(2) . . ? O3 C26 C20 116.2(2) . . ? O6 C27 O5 124.5(3) . . ? O6 C27 C22 118.4(3) . . ? O5 C27 C22 117.1(2) . . ? O8 C28 O7 125.7(2) . . ? O8 C28 C24 118.6(2) . . ? O7 C28 C24 115.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Zn1 O1 C1 94.0(2) . . . . ? O2 Zn1 O1 C1 -1.4(2) . . . . ? O9 Zn1 O1 C1 -172.9(2) . . . . ? O9 Zn1 O1 C1 -51.1(14) 2_666 . . . ? O8 Zn1 O1 C1 -83.0(2) 1_655 . . . ? Zn1 Zn1 O1 C1 -170.02(16) 2_666 . . . ? O10 Zn1 O2 C2 -90.2(2) . . . . ? O9 Zn1 O2 C2 57.9(5) . . . . ? O9 Zn1 O2 C2 172.1(2) 2_666 . . . ? O8 Zn1 O2 C2 88.4(2) 1_655 . . . ? O1 Zn1 O2 C2 -5.4(2) . . . . ? Zn1 Zn1 O2 C2 163.04(16) 2_666 . . . ? O9 Zn2 O3 C26 -21.1(2) . . . . ? O5 Zn2 O3 C26 107.4(2) 2_556 . . . ? O7 Zn2 O3 C26 -146.5(2) 1_655 . . . ? O3 Zn2 O9 Zn1 -97.91(10) . . . . ? O5 Zn2 O9 Zn1 138.02(8) 2_556 . . . ? O7 Zn2 O9 Zn1 26.31(11) 1_655 . . . ? O3 Zn2 O9 Zn1 148.70(10) . . . 2_666 ? O5 Zn2 O9 Zn1 24.62(13) 2_556 . . 2_666 ? O7 Zn2 O9 Zn1 -87.08(11) 1_655 . . 2_666 ? O10 Zn1 O9 Zn2 131.78(9) . . . . ? O2 Zn1 O9 Zn2 -16.4(5) . . . . ? O9 Zn1 O9 Zn2 -131.65(11) 2_666 . . . ? O8 Zn1 O9 Zn2 -46.57(9) 1_655 . . . ? O1 Zn1 O9 Zn2 45.56(10) . . . . ? Zn1 Zn1 O9 Zn2 -131.65(11) 2_666 . . . ? O10 Zn1 O9 Zn1 -96.58(8) . . . 2_666 ? O2 Zn1 O9 Zn1 115.3(4) . . . 2_666 ? O9 Zn1 O9 Zn1 0.0 2_666 . . 2_666 ? O8 Zn1 O9 Zn1 85.08(7) 1_655 . . 2_666 ? O1 Zn1 O9 Zn1 177.20(7) . . . 2_666 ? N2 Cu1 N1 C1 9.6(2) . . . . ? N4 Cu1 N1 C1 173.5(2) . . . . ? N3 Cu1 N1 C1 -73.7(4) . . . . ? N2 Cu1 N1 C19 -167.2(3) . . . . ? N4 Cu1 N1 C19 -3.4(3) . . . . ? N3 Cu1 N1 C19 109.5(4) . . . . ? N4 Cu1 N2 C2 -109.8(4) . . . . ? N1 Cu1 N2 C2 -16.0(2) . . . . ? N3 Cu1 N2 C2 144.8(2) . . . . ? N4 Cu1 N2 C3 73.2(5) . . . . ? N1 Cu1 N2 C3 167.0(3) . . . . ? N3 Cu1 N2 C3 -32.2(3) . . . . ? N2 Cu1 N3 C9 21.1(3) . . . . ? N4 Cu1 N3 C9 -143.3(3) . . . . ? N1 Cu1 N3 C9 103.5(4) . . . . ? N2 Cu1 N3 C10 -158.7(3) . . . . ? N4 Cu1 N3 C10 36.8(3) . . . . ? N1 Cu1 N3 C10 -76.3(4) . . . . ? N2 Cu1 N4 C13 89.3(5) . . . . ? N1 Cu1 N4 C13 -3.2(3) . . . . ? N3 Cu1 N4 C13 -165.5(3) . . . . ? N2 Cu1 N4 C12 -84.0(5) . . . . ? N1 Cu1 N4 C12 -176.6(3) . . . . ? N3 Cu1 N4 C12 21.2(3) . . . . ? Zn1 O1 C1 N1 -176.8(3) . . . . ? Zn1 O1 C1 C2 6.8(3) . . . . ? C19 N1 C1 O1 -1.6(5) . . . . ? Cu1 N1 C1 O1 -178.6(3) . . . . ? C19 N1 C1 C2 174.8(3) . . . . ? Cu1 N1 C1 C2 -2.1(3) . . . . ? Zn1 O2 C2 N2 -167.2(3) . . . . ? Zn1 O2 C2 C1 10.5(3) . . . . ? C3 N2 C2 O2 13.3(5) . . . . ? Cu1 N2 C2 O2 -163.8(3) . . . . ? C3 N2 C2 C1 -164.4(3) . . . . ? Cu1 N2 C2 C1 18.5(3) . . . . ? O1 C1 C2 O2 -12.1(4) . . . . ? N1 C1 C2 O2 170.9(3) . . . . ? O1 C1 C2 N2 165.9(3) . . . . ? N1 C1 C2 N2 -11.1(4) . . . . ? C2 N2 C3 C4 32.1(5) . . . . ? Cu1 N2 C3 C4 -151.2(3) . . . . ? C2 N2 C3 C8 -152.9(3) . . . . ? Cu1 N2 C3 C8 23.8(4) . . . . ? N2 C3 C4 C5 174.4(3) . . . . ? C8 C3 C4 C5 -0.7(5) . . . . ? C3 C4 C5 C6 1.2(6) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C5 C6 C7 C8 -1.3(7) . . . . ? C6 C7 C8 C3 1.8(6) . . . . ? C6 C7 C8 C9 -179.2(4) . . . . ? C4 C3 C8 C7 -0.8(5) . . . . ? N2 C3 C8 C7 -176.0(3) . . . . ? C4 C3 C8 C9 -179.7(3) . . . . ? N2 C3 C8 C9 5.1(5) . . . . ? C10 N3 C9 C8 177.7(3) . . . . ? Cu1 N3 C9 C8 -2.1(5) . . . . ? C7 C8 C9 N3 164.3(3) . . . . ? C3 C8 C9 N3 -16.8(5) . . . . ? C9 N3 C10 C11 124.6(4) . . . . ? Cu1 N3 C10 C11 -55.6(5) . . . . ? N3 C10 C11 C12 9.6(7) . . . . ? C13 N4 C12 C11 119.4(4) . . . . ? Cu1 N4 C12 C11 -66.8(4) . . . . ? C10 C11 C12 N4 53.7(6) . . . . ? C12 N4 C13 C14 -180.0(4) . . . . ? Cu1 N4 C13 C14 6.9(5) . . . . ? N4 C13 C14 C15 176.2(4) . . . . ? N4 C13 C14 C19 -3.6(6) . . . . ? C19 C14 C15 C16 0.7(5) . . . . ? C13 C14 C15 C16 -179.2(4) . . . . ? C14 C15 C16 C17 2.8(6) . . . . ? C15 C16 C17 C18 -3.6(6) . . . . ? C16 C17 C18 C19 0.9(7) . . . . ? C17 C18 C19 N1 -177.3(4) . . . . ? C17 C18 C19 C14 2.5(6) . . . . ? C1 N1 C19 C18 9.9(5) . . . . ? Cu1 N1 C19 C18 -173.6(3) . . . . ? C1 N1 C19 C14 -169.9(3) . . . . ? Cu1 N1 C19 C14 6.6(4) . . . . ? C15 C14 C19 C18 -3.3(5) . . . . ? C13 C14 C19 C18 176.6(3) . . . . ? C15 C14 C19 N1 176.6(3) . . . . ? C13 C14 C19 N1 -3.6(5) . . . . ? C25 C20 C21 C22 -0.5(4) . . . . ? C26 C20 C21 C22 176.9(2) . . . . ? C20 C21 C22 C23 -1.7(4) . . . . ? C20 C21 C22 C27 -178.3(2) . . . . ? C21 C22 C23 C24 2.0(4) . . . . ? C27 C22 C23 C24 178.7(2) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C22 C23 C24 C28 -176.1(2) . . . . ? C21 C20 C25 C24 2.4(4) . . . . ? C26 C20 C25 C24 -175.0(2) . . . . ? C23 C24 C25 C20 -2.1(4) . . . . ? C28 C24 C25 C20 173.9(2) . . . . ? Zn2 O3 C26 O4 1.9(4) . . . . ? Zn2 O3 C26 C20 -175.33(18) . . . . ? C25 C20 C26 O4 11.5(4) . . . . ? C21 C20 C26 O4 -165.9(3) . . . . ? C25 C20 C26 O3 -171.2(2) . . . . ? C21 C20 C26 O3 11.5(4) . . . . ? Zn2 O5 C27 O6 -81.0(4) 2_556 . . . ? Zn2 O5 C27 C22 99.4(3) 2_556 . . . ? C21 C22 C27 O6 -176.8(3) . . . . ? C23 C22 C27 O6 6.6(4) . . . . ? C21 C22 C27 O5 2.9(4) . . . . ? C23 C22 C27 O5 -173.7(2) . . . . ? Zn1 O8 C28 O7 -6.6(4) 1_455 . . . ? Zn1 O8 C28 C24 174.98(17) 1_455 . . . ? Zn2 O7 C28 O8 -38.4(4) 1_455 . . . ? Zn2 O7 C28 C24 140.04(18) 1_455 . . . ? C23 C24 C28 O8 -166.1(3) . . . . ? C25 C24 C28 O8 17.9(4) . . . . ? C23 C24 C28 O7 15.3(4) . . . . ? C25 C24 C28 O7 -160.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.494 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.059