Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Nolan, Kevin B.' 'Gaynor, Declan' 'Haase, Wolfgang' 'Ostrovsky, Sergei' 'Starikova, Zoya' _publ_contact_author_name 'Prof Kevin B Nolan' _publ_contact_author_address ; Chemistry Royal College of Surgeons in Ireland St. Stephen's Green Dublin 2 REPUBLIC OF IRELAND ; _publ_contact_author_email 'KBNOLAN@RCSI.IE' _publ_section_title ; Synthesis and structure of a heptanuclear nickel(II) complex uniquely exhibiting four distinct binding modes, three of which are novel, for a hydroxamate ligand. ; publ_section_references ; Bruker (1998a). SHELXTL, Version 5.10. Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART and SAINT, Version 5.05, Bruker AXS, Madison, Wisconsin, USA. Flack, H.D. (1983). Acta Cryst. A39, 876-881. ; data_exp2-38d _database_code_CSD 175233 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu5 (C9 H10 N2 O2)4 (H S O4 )2 (C H4 O)2, 2(C H4 O)' _chemical_formula_sum 'C40 H58 Cu5 N8 O20 S2' _chemical_formula_weight 1352.76 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' 'S' 'S' 0.1246 0.1234 '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' _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 11.002(4) _cell_length_b 11.393(4) _cell_length_c 11.863(4) _cell_angle_alpha 81.989(7) _cell_angle_beta 64.844(6) _cell_angle_gamma 68.106(6) _cell_volume 1248.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour black-green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 691 _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4312 _exptl_absorpt_correction_T_max 0.9356 _exptl_absorpt_process_details 'Sadabs program' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 14707 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7140 _reflns_number_gt 5646 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7140 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.004 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 0.0000 0.5000 0.0000 0.01286(10) Uani 1 2 d S . . Cu2 Cu -0.20140(3) 0.42600(3) 0.26954(2) 0.01291(8) Uani 1 1 d . . . Cu3 Cu 0.28293(3) 0.31777(3) 0.04720(3) 0.01410(8) Uani 1 1 d . . . O1 O 0.22523(17) 0.23260(17) 0.20247(15) 0.0172(3) Uani 1 1 d . . . O2 O 0.08271(17) 0.41592(16) 0.11340(15) 0.0146(3) Uani 1 1 d . . . O3 O 0.38758(17) 0.52967(17) -0.26556(15) 0.0166(3) Uani 1 1 d . . . O4 O 0.18361(17) 0.45263(16) -0.13583(15) 0.0143(3) Uani 1 1 d . . . N1 N -0.2258(2) 0.2850(2) 0.39617(18) 0.0158(4) Uani 1 1 d . . . N2 N 0.0026(2) 0.36780(19) 0.22334(17) 0.0135(4) Uani 1 1 d . . . N3 N 0.5006(2) 0.23834(19) -0.01380(18) 0.0152(4) Uani 1 1 d . . . N4 N 0.30288(19) 0.40875(19) -0.10472(18) 0.0130(4) Uani 1 1 d . . . C1 C -0.1222(2) 0.2330(2) 0.4529(2) 0.0152(4) Uani 1 1 d . . . C2 C 0.0222(3) 0.2230(2) 0.3877(2) 0.0158(4) Uani 1 1 d . . . C3 C 0.1164(3) 0.1677(2) 0.4462(2) 0.0189(5) Uani 1 1 d . . . H3 H 0.218(3) 0.156(3) 0.394(3) 0.013(7) Uiso 1 1 d . . . C4 C 0.0704(3) 0.1271(3) 0.5672(2) 0.0214(5) Uani 1 1 d . . . H4 H 0.126(4) 0.100(3) 0.610(3) 0.032(9) Uiso 1 1 d . . . C5 C -0.0714(3) 0.1357(3) 0.6309(2) 0.0229(5) Uani 1 1 d . . . H5 H -0.102(3) 0.105(3) 0.714(3) 0.013(7) Uiso 1 1 d . . . C6 C -0.1648(3) 0.1871(3) 0.5736(2) 0.0221(5) Uani 1 1 d . . . H6 H -0.262(3) 0.196(3) 0.618(3) 0.018(7) Uiso 1 1 d . . . C7 C 0.0864(2) 0.2740(2) 0.2632(2) 0.0148(4) Uani 1 1 d . . . C8 C -0.3762(3) 0.3357(3) 0.4919(3) 0.0221(5) Uani 1 1 d . . . H8A H -0.436(4) 0.379(3) 0.450(3) 0.032(9) Uiso 1 1 d . . . H8B H -0.412(4) 0.267(4) 0.544(3) 0.043(11) Uiso 1 1 d . . . H8C H -0.378(4) 0.399(3) 0.548(3) 0.027(9) Uiso 1 1 d . . . C9 C -0.2152(3) 0.1828(3) 0.3224(3) 0.0217(5) Uani 1 1 d . . . H9A H -0.248(4) 0.119(3) 0.385(3) 0.032(9) Uiso 1 1 d . . . H9B H -0.276(3) 0.223(3) 0.279(3) 0.017(7) Uiso 1 1 d . . . H9C H -0.125(4) 0.151(3) 0.266(3) 0.035(10) Uiso 1 1 d . . . C10 C 0.5797(2) 0.3245(2) -0.0781(2) 0.0143(4) Uani 1 1 d . . . C11 C 0.5365(2) 0.4177(2) -0.1581(2) 0.0137(4) Uani 1 1 d . . . C12 C 0.6246(3) 0.4877(2) -0.2268(2) 0.0159(4) Uani 1 1 d . . . H12 H 0.592(3) 0.545(3) -0.274(3) 0.017(7) Uiso 1 1 d . . . C13 C 0.7508(3) 0.4687(2) -0.2154(2) 0.0185(5) Uani 1 1 d . . . H13 H 0.804(4) 0.520(3) -0.253(3) 0.034(9) Uiso 1 1 d . . . C14 C 0.7908(3) 0.3792(2) -0.1342(2) 0.0190(5) Uani 1 1 d . . . H14 H 0.867(4) 0.376(3) -0.122(3) 0.026(8) Uiso 1 1 d . . . C15 C 0.7067(3) 0.3073(2) -0.0668(2) 0.0171(5) Uani 1 1 d . . . H15 H 0.736(3) 0.245(3) -0.018(3) 0.012(7) Uiso 1 1 d . . . C16 C 0.4026(2) 0.4532(2) -0.1783(2) 0.0134(4) Uani 1 1 d . . . C17 C 0.5342(3) 0.1752(3) 0.0940(2) 0.0209(5) Uani 1 1 d . . . H17A H 0.628(3) 0.116(3) 0.072(3) 0.009(6) Uiso 1 1 d . . . H17B H 0.522(3) 0.240(3) 0.146(2) 0.005(6) Uiso 1 1 d . . . H17C H 0.475(4) 0.121(3) 0.140(3) 0.030(9) Uiso 1 1 d . . . C18 C 0.5438(3) 0.1370(2) -0.1054(2) 0.0192(5) Uani 1 1 d . . . H18A H 0.630(5) 0.088(5) -0.124(4) 0.063(14) Uiso 1 1 d . . . H18B H 0.482(4) 0.093(3) -0.073(3) 0.027(8) Uiso 1 1 d . . . H18C H 0.538(3) 0.174(3) -0.178(3) 0.022(8) Uiso 1 1 d . . . S1 S 0.09660(6) 0.13083(6) -0.01543(5) 0.01665(13) Uani 1 1 d . . . O5 O 0.23002(19) 0.15489(18) -0.05920(17) 0.0211(4) Uani 1 1 d . . . O6 O 0.09280(19) 0.02655(18) 0.07255(17) 0.0214(4) Uani 1 1 d . . . O7 O -0.0296(2) 0.24271(19) 0.02859(18) 0.0244(4) Uani 1 1 d . . . O8 O 0.1045(2) 0.0803(2) -0.13670(17) 0.0248(4) Uani 1 1 d . . . H8O H 0.054(4) 0.051(3) -0.119(3) 0.029(10) Uiso 1 1 d . . . O1S O -0.2717(2) 0.5745(2) 0.41962(18) 0.0211(4) Uani 1 1 d . . . H1SO H -0.295(3) 0.626(3) 0.391(3) 0.011(8) Uiso 1 1 d . . . C1S C -0.1652(3) 0.5816(3) 0.4532(3) 0.0313(6) Uani 1 1 d . . . H1SA H -0.084(5) 0.606(4) 0.372(4) 0.057(12) Uiso 1 1 d . . . H1SB H -0.206(4) 0.653(4) 0.517(4) 0.038(10) Uiso 1 1 d . . . H1SC H -0.120(4) 0.486(4) 0.479(3) 0.035(9) Uiso 1 1 d . . . O2S O 0.3655(2) 0.2093(2) -0.30450(19) 0.0266(4) Uani 1 1 d . . . H2SO H 0.327(3) 0.207(3) -0.237(3) 0.017(8) Uiso 1 1 d . . . C2S C 0.4272(4) 0.0883(3) -0.3596(3) 0.0343(7) Uani 1 1 d . . . H2SA H 0.511(6) 0.027(5) -0.350(5) 0.080(16) Uiso 1 1 d . . . H2SB H 0.364(5) 0.031(4) -0.332(4) 0.056(12) Uiso 1 1 d . . . H2SC H 0.446(6) 0.106(5) -0.447(5) 0.091(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00829(18) 0.0174(2) 0.01174(18) 0.00278(15) -0.00367(14) -0.00467(15) Cu2 0.00961(14) 0.01495(15) 0.01277(14) 0.00347(10) -0.00384(10) -0.00476(11) Cu3 0.00918(14) 0.01678(16) 0.01360(14) 0.00410(11) -0.00362(10) -0.00414(11) O1 0.0111(7) 0.0203(9) 0.0167(8) 0.0062(7) -0.0048(6) -0.0046(7) O2 0.0082(7) 0.0186(8) 0.0137(7) 0.0060(6) -0.0026(6) -0.0051(6) O3 0.0108(7) 0.0222(9) 0.0163(8) 0.0064(7) -0.0058(6) -0.0068(7) O4 0.0094(7) 0.0196(8) 0.0138(7) 0.0046(6) -0.0055(6) -0.0056(6) N1 0.0128(9) 0.0179(10) 0.0142(9) 0.0021(8) -0.0030(7) -0.0063(8) N2 0.0099(8) 0.0174(10) 0.0115(8) 0.0041(7) -0.0027(7) -0.0061(7) N3 0.0108(9) 0.0153(10) 0.0170(9) 0.0042(8) -0.0053(7) -0.0040(7) N4 0.0071(8) 0.0151(9) 0.0148(9) 0.0024(7) -0.0042(7) -0.0028(7) C1 0.0142(10) 0.0123(10) 0.0151(10) 0.0007(8) -0.0045(8) -0.0024(8) C2 0.0184(11) 0.0169(11) 0.0117(10) 0.0032(8) -0.0054(8) -0.0076(9) C3 0.0193(12) 0.0166(12) 0.0206(11) 0.0041(9) -0.0093(9) -0.0058(10) C4 0.0234(13) 0.0220(13) 0.0205(12) 0.0056(10) -0.0120(10) -0.0078(10) C5 0.0253(13) 0.0240(13) 0.0164(11) 0.0054(10) -0.0074(10) -0.0084(11) C6 0.0217(12) 0.0234(13) 0.0154(11) 0.0041(10) -0.0022(9) -0.0094(10) C7 0.0093(9) 0.0163(11) 0.0192(11) -0.0025(9) -0.0044(8) -0.0053(8) C8 0.0134(11) 0.0235(13) 0.0215(12) 0.0083(10) -0.0029(9) -0.0056(10) C9 0.0257(13) 0.0184(12) 0.0237(12) 0.0014(10) -0.0116(11) -0.0092(11) C10 0.0108(10) 0.0155(11) 0.0143(10) -0.0006(8) -0.0030(8) -0.0043(8) C11 0.0106(10) 0.0142(11) 0.0146(10) -0.0010(8) -0.0037(8) -0.0039(8) C12 0.0144(10) 0.0178(11) 0.0157(10) 0.0027(9) -0.0060(9) -0.0069(9) C13 0.0156(11) 0.0211(12) 0.0214(11) 0.0015(9) -0.0079(9) -0.0090(10) C14 0.0152(11) 0.0202(12) 0.0253(12) 0.0030(10) -0.0112(9) -0.0074(10) C15 0.0146(11) 0.0170(12) 0.0195(11) 0.0010(9) -0.0074(9) -0.0051(9) C16 0.0104(10) 0.0139(11) 0.0148(10) -0.0004(8) -0.0043(8) -0.0040(8) C17 0.0183(12) 0.0246(13) 0.0216(12) 0.0074(10) -0.0106(10) -0.0089(11) C18 0.0157(11) 0.0165(12) 0.0239(12) 0.0011(10) -0.0055(9) -0.0070(10) S1 0.0152(3) 0.0190(3) 0.0173(3) 0.0017(2) -0.0073(2) -0.0073(2) O5 0.0182(8) 0.0251(10) 0.0238(9) 0.0036(7) -0.0092(7) -0.0117(7) O6 0.0186(8) 0.0252(10) 0.0222(9) 0.0055(7) -0.0094(7) -0.0100(8) O7 0.0198(9) 0.0254(10) 0.0271(9) -0.0008(8) -0.0116(8) -0.0041(8) O8 0.0272(10) 0.0361(12) 0.0179(9) 0.0007(8) -0.0072(8) -0.0205(9) O1S 0.0207(9) 0.0200(10) 0.0229(9) -0.0004(8) -0.0080(8) -0.0082(8) C1S 0.0316(15) 0.0352(17) 0.0339(15) -0.0046(13) -0.0164(13) -0.0134(13) O2S 0.0321(11) 0.0241(10) 0.0166(9) -0.0006(8) -0.0033(8) -0.0098(9) C2S 0.0322(16) 0.0273(16) 0.0357(17) -0.0077(13) -0.0029(13) -0.0122(13) _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 O2 1.8939(17) 2_565 ? Cu1 O2 1.8939(17) . ? Cu1 O4 1.9054(17) . ? Cu1 O4 1.9054(17) 2_565 ? Cu1 O7 3.0255(22) . ? Cu2 N2 1.929(2) . ? Cu2 O3 1.9383(17) 2_565 ? Cu2 O4 1.9476(17) 2_565 ? Cu2 O7 3.1986(22) . ? Cu2 N1 2.053(2) . ? Cu2 O1S 2.307(2) . ? Cu3 O2 1.9122(17) . ? Cu3 O5 2.7311(20) . ? Cu3 N4 1.9192(19) . ? Cu3 O1 1.9248(17) . ? Cu3 N3 2.042(2) . ? O1 C7 1.303(3) . ? O2 N2 1.401(2) . ? O3 C16 1.282(3) . ? O3 Cu2 1.9383(17) 2_565 ? O4 N4 1.407(2) . ? O4 Cu2 1.9476(17) 2_565 ? N1 C1 1.464(3) . ? N1 C9 1.494(3) . ? N1 C8 1.495(3) . ? N2 C7 1.308(3) . ? N3 C10 1.473(3) . ? N3 C17 1.495(3) . ? N3 C18 1.496(3) . ? N4 C16 1.303(3) . ? C1 C6 1.395(3) . ? C1 C2 1.407(3) . ? C2 C3 1.399(3) . ? C2 C7 1.482(3) . ? C3 C4 1.379(3) . ? C4 C5 1.386(4) . ? C5 C6 1.377(4) . ? C10 C15 1.398(3) . ? C10 C11 1.407(3) . ? C11 C12 1.401(3) . ? C11 C16 1.491(3) . ? C12 C13 1.386(3) . ? C13 C14 1.383(4) . ? C14 C15 1.386(3) . ? S1 O7 1.440(2) . ? S1 O5 1.4532(18) . ? S1 O6 1.4687(19) . ? S1 O8 1.579(2) . ? O1S C1S 1.420(4) . ? O2S C2S 1.401(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O2 180.00(6) 2_565 . ? O2 Cu1 O4 88.86(7) 2_565 . ? O2 Cu1 O4 91.14(7) . . ? O2 Cu1 O4 91.14(7) 2_565 2_565 ? O2 Cu1 O4 88.86(7) . 2_565 ? O4 Cu1 O4 180.00(9) . 2_565 ? N2 Cu2 O3 163.13(8) . 2_565 ? N2 Cu2 O4 90.27(7) . 2_565 ? O3 Cu2 O4 80.71(7) 2_565 2_565 ? N2 Cu2 N1 92.31(8) . . ? O3 Cu2 N1 94.92(8) 2_565 . ? O4 Cu2 N1 172.20(8) 2_565 . ? N2 Cu2 O1S 98.29(8) . . ? O3 Cu2 O1S 96.47(7) 2_565 . ? O4 Cu2 O1S 93.48(8) 2_565 . ? N1 Cu2 O1S 93.44(8) . . ? O2 Cu3 N4 88.54(7) . . ? O2 Cu3 O1 81.62(7) . . ? N4 Cu3 O1 168.64(7) . . ? O2 Cu3 N3 170.22(8) . . ? N4 Cu3 N3 90.53(8) . . ? O1 Cu3 N3 100.13(7) . . ? C7 O1 Cu3 111.38(15) . . ? N2 O2 Cu1 120.08(13) . . ? N2 O2 Cu3 113.40(13) . . ? Cu1 O2 Cu3 118.06(8) . . ? C16 O3 Cu2 112.63(14) . 2_565 ? N4 O4 Cu1 116.30(13) . . ? N4 O4 Cu2 112.59(12) . 2_565 ? Cu1 O4 Cu2 114.18(8) . 2_565 ? C1 N1 C9 109.1(2) . . ? C1 N1 C8 111.86(19) . . ? C9 N1 C8 108.3(2) . . ? C1 N1 Cu2 117.95(15) . . ? C9 N1 Cu2 103.16(15) . . ? C8 N1 Cu2 105.81(15) . . ? C7 N2 O2 110.99(18) . . ? C7 N2 Cu2 131.46(16) . . ? O2 N2 Cu2 116.35(14) . . ? C10 N3 C17 112.78(19) . . ? C10 N3 C18 107.80(18) . . ? C17 N3 C18 107.7(2) . . ? C10 N3 Cu3 115.28(15) . . ? C17 N3 Cu3 108.00(15) . . ? C18 N3 Cu3 104.78(15) . . ? C16 N4 O4 111.74(18) . . ? C16 N4 Cu3 130.65(16) . . ? O4 N4 Cu3 116.89(13) . . ? C6 C1 C2 118.2(2) . . ? C6 C1 N1 119.7(2) . . ? C2 C1 N1 122.0(2) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 C7 114.4(2) . . ? C1 C2 C7 126.6(2) . . ? C4 C3 C2 121.8(2) . . ? C3 C4 C5 119.3(2) . . ? C6 C5 C4 119.6(2) . . ? C5 C6 C1 122.2(2) . . ? O1 C7 N2 121.9(2) . . ? O1 C7 C2 119.1(2) . . ? N2 C7 C2 118.6(2) . . ? C15 C10 C11 119.1(2) . . ? C15 C10 N3 119.2(2) . . ? C11 C10 N3 121.5(2) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 C16 114.4(2) . . ? C10 C11 C16 126.8(2) . . ? C13 C12 C11 121.4(2) . . ? C12 C13 C14 119.5(2) . . ? C13 C14 C15 120.2(2) . . ? C14 C15 C10 121.0(2) . . ? O3 C16 N4 122.1(2) . . ? O3 C16 C11 118.7(2) . . ? N4 C16 C11 119.1(2) . . ? O7 S1 O5 113.77(12) . . ? O7 S1 O6 113.47(12) . . ? O5 S1 O6 111.93(11) . . ? O7 S1 O8 107.82(12) . . ? O5 S1 O8 103.06(11) . . ? O6 S1 O8 105.82(12) . . ? C1S O1S Cu2 117.76(18) . . ? 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 O2 Cu3 O1 C7 6.32(16) . . . . ? N4 Cu3 O1 C7 -23.8(5) . . . . ? N3 Cu3 O1 C7 176.58(16) . . . . ? O2 Cu1 O2 N2 145(100) 2_565 . . . ? O4 Cu1 O2 N2 -152.42(16) . . . . ? O4 Cu1 O2 N2 27.58(16) 2_565 . . . ? O2 Cu1 O2 Cu3 -69(100) 2_565 . . . ? O4 Cu1 O2 Cu3 -6.44(10) . . . . ? O4 Cu1 O2 Cu3 173.56(10) 2_565 . . . ? N4 Cu3 O2 N2 166.84(15) . . . . ? O1 Cu3 O2 N2 -7.48(14) . . . . ? N3 Cu3 O2 N2 -108.6(4) . . . . ? N4 Cu3 O2 Cu1 18.68(11) . . . . ? O1 Cu3 O2 Cu1 -155.64(11) . . . . ? N3 Cu3 O2 Cu1 103.3(4) . . . . ? O2 Cu1 O4 N4 164.81(15) 2_565 . . . ? O2 Cu1 O4 N4 -15.19(15) . . . . ? O4 Cu1 O4 N4 -122(100) 2_565 . . . ? O2 Cu1 O4 Cu2 31.06(9) 2_565 . . 2_565 ? O2 Cu1 O4 Cu2 -148.94(9) . . . 2_565 ? O4 Cu1 O4 Cu2 104(100) 2_565 . . 2_565 ? N2 Cu2 N1 C1 27.14(17) . . . . ? O3 Cu2 N1 C1 -168.11(17) 2_565 . . . ? O4 Cu2 N1 C1 136.4(5) 2_565 . . . ? O1S Cu2 N1 C1 -71.31(17) . . . . ? N2 Cu2 N1 C9 -93.16(16) . . . . ? O3 Cu2 N1 C9 71.58(16) 2_565 . . . ? O4 Cu2 N1 C9 16.1(6) 2_565 . . . ? O1S Cu2 N1 C9 168.38(15) . . . . ? N2 Cu2 N1 C8 153.19(17) . . . . ? O3 Cu2 N1 C8 -42.07(17) 2_565 . . . ? O4 Cu2 N1 C8 -97.6(6) 2_565 . . . ? O1S Cu2 N1 C8 54.73(17) . . . . ? Cu1 O2 N2 C7 154.68(16) . . . . ? Cu3 O2 N2 C7 7.2(2) . . . . ? Cu1 O2 N2 Cu2 -14.2(2) . . . . ? Cu3 O2 N2 Cu2 -161.68(10) . . . . ? O3 Cu2 N2 C7 -116.3(3) 2_565 . . . ? O4 Cu2 N2 C7 -173.6(2) 2_565 . . . ? N1 Cu2 N2 C7 -0.9(2) . . . . ? O1S Cu2 N2 C7 92.9(2) . . . . ? O3 Cu2 N2 O2 49.8(4) 2_565 . . . ? O4 Cu2 N2 O2 -7.44(16) 2_565 . . . ? N1 Cu2 N2 O2 165.19(16) . . . . ? O1S Cu2 N2 O2 -101.00(16) . . . . ? O2 Cu3 N3 C10 -43.0(5) . . . . ? N4 Cu3 N3 C10 41.40(16) . . . . ? O1 Cu3 N3 C10 -142.54(16) . . . . ? O2 Cu3 N3 C17 84.1(5) . . . . ? N4 Cu3 N3 C17 168.53(17) . . . . ? O1 Cu3 N3 C17 -15.41(17) . . . . ? O2 Cu3 N3 C18 -161.3(4) . . . . ? N4 Cu3 N3 C18 -76.91(15) . . . . ? O1 Cu3 N3 C18 99.15(15) . . . . ? Cu1 O4 N4 C16 -138.68(16) . . . . ? Cu2 O4 N4 C16 -4.2(2) 2_565 . . . ? Cu1 O4 N4 Cu3 32.6(2) . . . . ? Cu2 O4 N4 Cu3 167.09(9) 2_565 . . . ? O2 Cu3 N4 C16 139.3(2) . . . . ? O1 Cu3 N4 C16 169.1(3) . . . . ? N3 Cu3 N4 C16 -31.0(2) . . . . ? O2 Cu3 N4 O4 -30.08(16) . . . . ? O1 Cu3 N4 O4 -0.3(5) . . . . ? N3 Cu3 N4 O4 159.65(16) . . . . ? C9 N1 C1 C6 -93.4(3) . . . . ? C8 N1 C1 C6 26.4(3) . . . . ? Cu2 N1 C1 C6 149.4(2) . . . . ? C9 N1 C1 C2 84.0(3) . . . . ? C8 N1 C1 C2 -156.2(2) . . . . ? Cu2 N1 C1 C2 -33.2(3) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? N1 C1 C2 C3 -177.5(2) . . . . ? C6 C1 C2 C7 -175.2(2) . . . . ? N1 C1 C2 C7 7.4(4) . . . . ? C1 C2 C3 C4 -2.3(4) . . . . ? C7 C2 C3 C4 173.4(2) . . . . ? C2 C3 C4 C5 3.1(4) . . . . ? C3 C4 C5 C6 -1.5(4) . . . . ? C4 C5 C6 C1 -0.9(4) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? N1 C1 C6 C5 179.1(2) . . . . ? Cu3 O1 C7 N2 -4.2(3) . . . . ? Cu3 O1 C7 C2 -177.57(17) . . . . ? O2 N2 C7 O1 -1.9(3) . . . . ? Cu2 N2 C7 O1 164.79(17) . . . . ? O2 N2 C7 C2 171.44(19) . . . . ? Cu2 N2 C7 C2 -21.9(3) . . . . ? C3 C2 C7 O1 20.7(3) . . . . ? C1 C2 C7 O1 -164.0(2) . . . . ? C3 C2 C7 N2 -152.8(2) . . . . ? C1 C2 C7 N2 22.5(4) . . . . ? C17 N3 C10 C15 22.5(3) . . . . ? C18 N3 C10 C15 -96.2(3) . . . . ? Cu3 N3 C10 C15 147.14(19) . . . . ? C17 N3 C10 C11 -162.4(2) . . . . ? C18 N3 C10 C11 78.9(3) . . . . ? Cu3 N3 C10 C11 -37.7(3) . . . . ? C15 C10 C11 C12 2.0(3) . . . . ? N3 C10 C11 C12 -173.2(2) . . . . ? C15 C10 C11 C16 -177.4(2) . . . . ? N3 C10 C11 C16 7.5(4) . . . . ? C10 C11 C12 C13 -1.4(4) . . . . ? C16 C11 C12 C13 178.0(2) . . . . ? C11 C12 C13 C14 -0.3(4) . . . . ? C12 C13 C14 C15 1.4(4) . . . . ? C13 C14 C15 C10 -0.8(4) . . . . ? C11 C10 C15 C14 -0.9(4) . . . . ? N3 C10 C15 C14 174.4(2) . . . . ? Cu2 O3 C16 N4 2.2(3) 2_565 . . . ? Cu2 O3 C16 C11 -175.77(16) 2_565 . . . ? O4 N4 C16 O3 1.4(3) . . . . ? Cu3 N4 C16 O3 -168.38(17) . . . . ? O4 N4 C16 C11 179.31(19) . . . . ? Cu3 N4 C16 C11 9.5(3) . . . . ? C12 C11 C16 O3 8.9(3) . . . . ? C10 C11 C16 O3 -171.7(2) . . . . ? C12 C11 C16 N4 -169.1(2) . . . . ? C10 C11 C16 N4 10.3(4) . . . . ? N2 Cu2 O1S C1S -6.3(2) . . . . ? O3 Cu2 O1S C1S -178.1(2) 2_565 . . . ? O4 Cu2 O1S C1S -97.1(2) 2_565 . . . ? N1 Cu2 O1S C1S 86.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.534 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.141 #------------------------------------------------------------ data_exp2.56(b) _database_code_CSD 175234 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H120 N20 Ni7 O26 2+, S O4 2-, 15(H2 O)' _chemical_formula_sum 'C90 H150 N20 Ni7 O45 S' _chemical_formula_weight 2675.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 16.398(9) _cell_length_b 23.996(14) _cell_length_c 30.666(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12067(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 70 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20.0 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5608 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7987 _exptl_absorpt_correction_T_max 0.9435 _exptl_absorpt_process_details 'SADABS (Bruker, 1998b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'SMART 1000 CCD' _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 41850 _diffrn_reflns_av_R_equivalents 0.1354 _diffrn_reflns_av_sigmaI/netI 0.4306 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.10 _reflns_number_total 20598 _reflns_number_gt 6247 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Bruker SMART (Bruker, 1998b)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998b)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998b)' _computing_structure_solution 'SHELXL PLUS ver. 5.10 (Bruker, 1998a)' _computing_structure_refinement 'SHELXL PLUS ver. 5.10 (Bruker, 1998a)' _computing_molecular_graphics 'SHELXL PLUS ver. 5.10 (Bruker,1998a)' _computing_publication_material 'SHELXL PLUS ver. 5.10 (Bruker, 1998a)' _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^)+(0.0033P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983)' _refine_ls_abs_structure_Flack 0.059(15) _refine_ls_number_reflns 20598 _refine_ls_number_parameters 1452 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1878 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.649 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.95688(11) -0.97220(7) -0.56041(5) 0.0428(5) Uani 1 1 d . . . Ni2 Ni -0.79116(10) -0.92747(6) -0.57567(5) 0.0350(4) Uani 1 1 d . . . Ni3 Ni -0.87469(10) -0.82766(6) -0.65076(5) 0.0334(4) Uani 1 1 d . . . Ni4 Ni -0.66581(10) -0.85516(6) -0.62707(5) 0.0333(4) Uani 1 1 d . . . Ni5 Ni -0.80764(10) -0.94668(6) -0.67990(5) 0.0350(4) Uani 1 1 d . . . Ni6 Ni -0.72383(10) -0.81726(6) -0.71902(5) 0.0332(4) Uani 1 1 d . . . Ni7 Ni -0.83664(10) -0.81950(6) -0.79370(5) 0.0362(4) Uani 1 1 d . . . O1A O -0.8835(5) -0.9119(3) -0.5326(2) 0.038(2) Uani 1 1 d . . . O2A O -0.9446(5) -1.0082(3) -0.5022(3) 0.046(3) Uani 1 1 d . . . N1A N -0.8690(6) -0.9271(4) -0.4893(3) 0.041(3) Uani 1 1 d . . . H1A H -0.8553 -0.8937 -0.4588 0.050 Uiso 1 1 d . . . N2A N -0.7968(6) -0.9139(4) -0.4105(3) 0.038(3) Uani 1 1 d . . . C1A C -0.9022(8) -0.9767(6) -0.4759(5) 0.049(4) Uani 1 1 d . . . C2A C -0.8865(8) -0.9918(5) -0.4275(4) 0.042(4) Uani 1 1 d . . . C3A C -0.8447(9) -0.9612(5) -0.3977(5) 0.046(4) Uani 1 1 d . . . C4A C -0.8501(7) -0.9764(5) -0.3540(5) 0.046(4) Uani 1 1 d . . . H4A H -0.8225 -0.9541 -0.3331 0.055 Uiso 1 1 calc R . . C5A C -0.8907(8) -1.0193(6) -0.3402(4) 0.050(4) Uani 1 1 d . . . H5A H -0.8934 -1.0265 -0.3097 0.059 Uiso 1 1 calc R . . C6A C -0.9328(8) -1.0571(6) -0.3708(5) 0.062(4) Uani 1 1 d . . . H6A H -0.9597 -1.0904 -0.3622 0.074 Uiso 1 1 calc R . . C7A C -0.9287(8) -1.0381(5) -0.4141(4) 0.046(4) Uani 1 1 d . . . H7A H -0.9572 -1.0589 -0.4356 0.056 Uiso 1 1 calc R . . C8A C -0.7180(8) -0.9331(4) -0.4264(4) 0.048(4) Uani 1 1 d . . . H8AA H -0.7258 -0.9655 -0.4454 0.072 Uiso 1 1 calc R . . H8AB H -0.6835 -0.9436 -0.4016 0.072 Uiso 1 1 calc R . . H9AC H -0.6915 -0.9031 -0.4429 0.072 Uiso 1 1 calc R . . C9A C -0.7855(8) -0.8706(4) -0.3782(3) 0.050(4) Uani 1 1 d . . . H9AA H -0.8371 -0.8507 -0.3738 0.075 Uiso 1 1 calc R . . H9AB H -0.7438 -0.8443 -0.3884 0.075 Uiso 1 1 calc R . . H9AC' H -0.7680 -0.8873 -0.3506 0.075 Uiso 1 1 calc R . . O1B O -0.8422(5) -1.0061(3) -0.5777(2) 0.036(2) Uani 1 1 d . . . O2B O -0.7141(5) -0.9672(3) -0.5349(2) 0.039(2) Uani 1 1 d . . . N1B N -0.7931(7) -1.0401(4) -0.5524(3) 0.043(3) Uani 1 1 d . . . H1B H -0.7813 -1.0888 -0.5495 0.050 Uiso 1 1 d . . . N2B N -0.7536(8) -1.1412(4) -0.5145(3) 0.049(3) Uani 1 1 d . . . C1B C -0.7280(9) -1.0190(5) -0.5325(4) 0.039(4) Uani 1 1 d . . . C2B C -0.6660(8) -1.0561(6) -0.5099(4) 0.039(3) Uani 1 1 d . . . C3B C -0.6740(10) -1.1150(6) -0.5047(4) 0.048(4) Uani 1 1 d . . . C4B C -0.6092(9) -1.1451(6) -0.4918(4) 0.050(4) Uani 1 1 d . . . H4B H -0.6130 -1.1846 -0.4913 0.060 Uiso 1 1 calc R . . C5B C -0.5381(10) -1.1203(6) -0.4793(4) 0.051(4) Uani 1 1 d . . . H5B H -0.4944 -1.1426 -0.4689 0.061 Uiso 1 1 calc R . . C6B C -0.5289(8) -1.0631(6) -0.4817(4) 0.052(4) Uani 1 1 d . . . H6B H -0.4793 -1.0462 -0.4727 0.062 Uiso 1 1 calc R . . C7B C -0.5944(10) -1.0297(5) -0.4977(3) 0.049(4) Uani 1 1 d . . . H7B H -0.5891 -0.9904 -0.5000 0.059 Uiso 1 1 calc R . . C8B C -0.8122(8) -1.1332(5) -0.4807(4) 0.054(4) Uani 1 1 d . . . H8BA H -0.8205 -1.0932 -0.4760 0.081 Uiso 1 1 calc R . . H8BB H -0.7923 -1.1503 -0.4537 0.081 Uiso 1 1 calc R . . H8BC H -0.8640 -1.1505 -0.4892 0.081 Uiso 1 1 calc R . . C9B C -0.7453(9) -1.1980(4) -0.5284(4) 0.073(6) Uani 1 1 d . . . H9BA H -0.7083 -1.1997 -0.5535 0.110 Uiso 1 1 calc R . . H9BB H -0.7988 -1.2126 -0.5367 0.110 Uiso 1 1 calc R . . H9BC H -0.7230 -1.2203 -0.5045 0.110 Uiso 1 1 calc R . . O1C O -0.8685(5) -0.9077(3) -0.6256(2) 0.034(2) Uani 1 1 d . . . O2C O -0.9884(5) -0.8544(3) -0.6587(2) 0.038(2) Uani 1 1 d . . . N1C N -0.9498(6) -0.9273(4) -0.6153(3) 0.036(3) Uani 1 1 d . . . N2C N -1.0771(7) -0.9330(4) -0.5490(3) 0.047(3) Uani 1 1 d . . . C1C C -1.0036(8) -0.8946(5) -0.6329(4) 0.036(3) Uani 1 1 d . . . C2C C -1.0924(8) -0.9126(5) -0.6267(4) 0.035(3) Uani 1 1 d . . . C3C C -1.1220(9) -0.9331(5) -0.5893(4) 0.045(4) Uani 1 1 d . . . C4C C -1.2031(9) -0.9495(5) -0.5889(4) 0.053(4) Uani 1 1 d . . . H4C H -1.2253 -0.9639 -0.5626 0.064 Uiso 1 1 calc R . . C5C C -1.2535(8) -0.9460(5) -0.6255(4) 0.041(3) Uani 1 1 d . . . H5C H -1.3080 -0.9592 -0.6240 0.049 Uiso 1 1 calc R . . C6C C -1.2254(8) -0.9242(4) -0.6625(4) 0.039(4) Uani 1 1 d . . . H6C H -1.2589 -0.9208 -0.6876 0.046 Uiso 1 1 calc R . . C7C C -1.1448(8) -0.9066(4) -0.6627(4) 0.037(3) Uani 1 1 d . . . H7C H -1.1240 -0.8897 -0.6884 0.044 Uiso 1 1 calc R . . C8C C -1.0673(9) -0.8746(6) -0.5326(4) 0.074(5) Uani 1 1 d . . . H8CA H -1.1206 -0.8600 -0.5237 0.111 Uiso 1 1 calc R . . H8CB H -1.0449 -0.8511 -0.5559 0.111 Uiso 1 1 calc R . . H8CC H -1.0301 -0.8743 -0.5076 0.111 Uiso 1 1 calc R . . C9C C -1.1146(8) -0.9650(6) -0.5117(4) 0.080(6) Uani 1 1 d . . . H9CA H -1.1545 -0.9413 -0.4967 0.120 Uiso 1 1 calc R . . H9CB H -1.0718 -0.9760 -0.4911 0.120 Uiso 1 1 calc R . . H9CC H -1.1419 -0.9983 -0.5230 0.120 Uiso 1 1 calc R . . O1D O -0.7208(5) -0.9333(3) -0.6331(2) 0.031(2) Uani 1 1 d . . . O2D O -0.5756(5) -0.9034(3) -0.6041(2) 0.040(2) Uani 1 1 d . . . N1D N -0.6540(7) -0.9722(4) -0.6296(3) 0.036(3) Uani 1 1 d . . . H1D H -0.6731 -1.0093 -0.6303 0.050 Uiso 1 1 d . . . N2D N -0.5966(8) -1.0749(4) -0.6343(3) 0.048(3) Uani 1 1 d . . . C1D C -0.5885(9) -0.9544(5) -0.6117(4) 0.049(4) Uani 1 1 d . . . C2D C -0.5241(9) -0.9985(6) -0.6009(4) 0.050(4) Uani 1 1 d . . . C3D C -0.5258(9) -1.0535(6) -0.6092(4) 0.042(4) Uani 1 1 d . . . C4D C -0.4664(10) -1.0889(6) -0.5939(4) 0.058(4) Uani 1 1 d . . . H4D H -0.4691 -1.1275 -0.6006 0.069 Uiso 1 1 calc R . . C5D C -0.4021(9) -1.0684(7) -0.5686(4) 0.064(5) Uani 1 1 d . . . H5D H -0.3611 -1.0926 -0.5577 0.076 Uiso 1 1 calc R . . C6D C -0.3999(9) -1.0115(7) -0.5599(5) 0.073(5) Uani 1 1 d . . . H6D H -0.3574 -0.9963 -0.5426 0.088 Uiso 1 1 calc R . . C7D C -0.4583(9) -0.9780(5) -0.5763(4) 0.054(4) Uani 1 1 d . . . H7D H -0.4549 -0.9390 -0.5710 0.064 Uiso 1 1 calc R . . C8D C -0.5745(9) -1.0734(5) -0.6802(4) 0.079(5) Uani 1 1 d . . . H8DA H -0.5696 -1.0345 -0.6897 0.119 Uiso 1 1 calc R . . H8DB H -0.6167 -1.0921 -0.6975 0.119 Uiso 1 1 calc R . . H8DB' H -0.5222 -1.0925 -0.6844 0.119 Uiso 1 1 calc R . . C9D C -0.6298(9) -1.1278(5) -0.6211(4) 0.072(5) Uani 1 1 d . . . H9DA H -0.6346 -1.1288 -0.5893 0.107 Uiso 1 1 calc R . . H9DB H -0.5936 -1.1578 -0.6308 0.107 Uiso 1 1 calc R . . H9DC H -0.6838 -1.1327 -0.6342 0.107 Uiso 1 1 calc R . . O1E O -0.8189(5) -0.8680(3) -0.7076(2) 0.032(2) Uani 1 1 d . . . O2E O -0.9067(5) -0.9584(3) -0.7184(2) 0.031(2) Uani 1 1 d . . . N1E N -0.8712(6) -0.8708(3) -0.7454(3) 0.022(2) Uani 1 1 d . . . N2E N -0.8709(7) -0.8857(4) -0.8372(3) 0.047(3) Uani 1 1 d . . . C1E C -0.9137(8) -0.9165(5) -0.7472(4) 0.035(3) Uani 1 1 d . . . C2E C -0.9685(7) -0.9243(4) -0.7822(4) 0.029(3) Uani 1 1 d . . . C3E C -0.9518(8) -0.9066(5) -0.8269(4) 0.037(3) Uani 1 1 d . . . C4E C -1.0126(10) -0.9098(6) -0.8584(4) 0.074(5) Uani 1 1 d . . . H4E H -1.0035 -0.8955 -0.8869 0.089 Uiso 1 1 calc R . . C5E C -1.0891(10) -0.9350(5) -0.8475(4) 0.059(5) Uani 1 1 d . . . H5E H -1.1289 -0.9400 -0.8697 0.071 Uiso 1 1 calc R . . C6E C -1.1062(9) -0.9517(5) -0.8068(4) 0.056(4) Uani 1 1 d . . . H6E H -1.1585 -0.9657 -0.7994 0.067 Uiso 1 1 calc R . . C7E C -1.0418(8) -0.9477(4) -0.7742(4) 0.036(3) Uani 1 1 d . . . H7H H -1.0519 -0.9622 -0.7459 0.043 Uiso 1 1 calc R . . C8E C -0.8122(8) -0.9331(4) -0.8333(3) 0.051(4) Uani 1 1 d . . . H8EA H -0.8275 -0.9627 -0.8538 0.077 Uiso 1 1 calc R . . H8EB H -0.8136 -0.9478 -0.8035 0.077 Uiso 1 1 calc R . . H8EC H -0.7570 -0.9201 -0.8400 0.077 Uiso 1 1 calc R . . C9E C -0.8657(8) -0.8643(5) -0.8827(3) 0.063(5) Uani 1 1 d . . . H9EA H -0.8818 -0.8938 -0.9031 0.094 Uiso 1 1 calc R . . H9EB H -0.8096 -0.8527 -0.8889 0.094 Uiso 1 1 calc R . . H9EC H -0.9024 -0.8323 -0.8860 0.094 Uiso 1 1 calc R . . O1F O -0.8054(5) -0.7593(3) -0.7448(2) 0.042(2) Uani 1 1 d . . . O2F O -0.6482(5) -0.7531(3) -0.7244(2) 0.035(2) Uani 1 1 d . . . N1F N -0.7569(7) -0.7096(4) -0.7512(3) 0.037(3) Uani 1 1 d . . . H1F H -0.7826 -0.6843 -0.7716 0.050 Uiso 1 1 d . . . N2F N -0.7363(8) -0.6058(4) -0.7848(4) 0.056(3) Uani 1 1 d . . . C1F C -0.6807(8) -0.7112(5) -0.7388(3) 0.025(3) Uani 1 1 d . . . C2F C -0.6359(10) -0.6566(6) -0.7428(4) 0.053(4) Uani 1 1 d . . . C3F C -0.6664(12) -0.6079(7) -0.7606(4) 0.070(6) Uani 1 1 d . . . C4F C -0.6129(10) -0.5558(6) -0.7572(5) 0.068(5) Uani 1 1 d . . . H4F H -0.6272 -0.5222 -0.7716 0.081 Uiso 1 1 calc R . . C5F C -0.5441(11) -0.5595(7) -0.7327(4) 0.062(5) Uani 1 1 d . . . H5F H -0.5154 -0.5257 -0.7278 0.074 Uiso 1 1 calc R . . C6F C -0.5105(10) -0.6071(7) -0.7140(4) 0.077(5) Uani 1 1 d . . . H6F H -0.4602 -0.6074 -0.6987 0.093 Uiso 1 1 calc R . . C7F C -0.5612(10) -0.6565(6) -0.7205(4) 0.063(5) Uani 1 1 d . . . H7F H -0.5422 -0.6909 -0.7090 0.076 Uiso 1 1 calc R . . C8F C -0.7276(10) -0.6206(5) -0.8303(4) 0.102(7) Uani 1 1 d . . . H8FA H -0.6948 -0.6546 -0.8327 0.153 Uiso 1 1 calc R . . H8FB H -0.7005 -0.5902 -0.8459 0.153 Uiso 1 1 calc R . . H8FC H -0.7816 -0.6271 -0.8430 0.153 Uiso 1 1 calc R . . C9F C -0.7859(10) -0.5571(5) -0.7853(4) 0.090(6) Uani 1 1 d . . . H9FA H -0.7772 -0.5359 -0.7584 0.135 Uiso 1 1 calc R . . H9FB H -0.8434 -0.5678 -0.7874 0.135 Uiso 1 1 calc R . . H9FC H -0.7712 -0.5340 -0.8105 0.135 Uiso 1 1 calc R . . O1G O -0.6405(5) -0.8660(3) -0.6920(2) 0.035(2) Uani 1 1 d . . . O2G O -0.5470(5) -0.9410(3) -0.7353(2) 0.041(2) Uani 1 1 d . . . N1G N -0.5593(6) -0.8562(4) -0.7056(3) 0.032(3) Uani 1 1 d . . . H1G H -0.5445 -0.8201 -0.6910 0.050 Uiso 1 1 d . . . N2G N -0.4194(6) -0.8014(4) -0.6861(4) 0.051(3) Uani 1 1 d . . . C1G C -0.5167(8) -0.8953(5) -0.7261(4) 0.033(3) Uani 1 1 d . . . C2G C -0.4313(9) -0.8787(5) -0.7378(4) 0.041(4) Uani 1 1 d . . . C3G C -0.3843(8) -0.8362(5) -0.7206(4) 0.042(4) Uani 1 1 d . . . C4G C -0.3043(9) -0.8240(6) -0.7382(4) 0.069(5) Uani 1 1 d . . . H4G H -0.2734 -0.7931 -0.7281 0.083 Uiso 1 1 calc R . . C5G C -0.2747(9) -0.8592(5) -0.7703(4) 0.053(4) Uani 1 1 d . . . H5G H -0.2218 -0.8526 -0.7818 0.064 Uiso 1 1 calc R . . C6G C -0.3185(8) -0.9031(5) -0.7861(4) 0.049(4) Uani 1 1 d . . . H6G H -0.2953 -0.9264 -0.8079 0.059 Uiso 1 1 calc R . . C7G C -0.3973(8) -0.9143(5) -0.7708(4) 0.037(4) Uani 1 1 d . . . H7G H -0.4276 -0.9449 -0.7820 0.045 Uiso 1 1 calc R . . C8G C -0.4187(8) -0.8319(5) -0.6440(3) 0.057(4) Uani 1 1 d . . . H8GA H -0.4374 -0.8702 -0.6487 0.086 Uiso 1 1 calc R . . H8GB H -0.4552 -0.8132 -0.6233 0.086 Uiso 1 1 calc R . . H8GC H -0.3632 -0.8324 -0.6323 0.086 Uiso 1 1 calc R . . C9G C -0.3815(8) -0.7431(5) -0.6824(5) 0.083(5) Uani 1 1 d . . . H9GA H -0.3840 -0.7246 -0.7108 0.124 Uiso 1 1 calc R . . H9GB H -0.3245 -0.7465 -0.6732 0.124 Uiso 1 1 calc R . . H9GC H -0.4119 -0.7212 -0.6609 0.124 Uiso 1 1 calc R . . O1H O -0.7204(5) -0.8456(3) -0.7832(2) 0.034(2) Uani 1 1 d . . . O2H O -0.7779(6) -0.7724(3) -0.8391(3) 0.046(3) Uani 1 1 d . . . N1H N -0.6692(6) -0.8166(3) -0.8129(3) 0.036(3) Uani 1 1 d . . . H1H H -0.6207 -0.8484 -0.8229 0.050 Uiso 1 1 d . . . N2H N -0.5183(7) -0.7912(4) -0.8464(3) 0.040(3) Uani 1 1 d . . . C1H C -0.7015(10) -0.7857(5) -0.8415(4) 0.046(4) Uani 1 1 d . . . C2H C -0.6499(8) -0.7602(5) -0.8783(4) 0.033(3) Uani 1 1 d . . . C3H C -0.5615(9) -0.7663(5) -0.8808(5) 0.049(4) Uani 1 1 d . . . C4H C -0.5232(10) -0.7525(5) -0.9203(4) 0.065(5) Uani 1 1 d . . . H4H H -0.4675 -0.7617 -0.9250 0.077 Uiso 1 1 calc R . . C5H C -0.5666(10) -0.7263(6) -0.9514(5) 0.060(5) Uani 1 1 d . . . H5H H -0.5386 -0.7123 -0.9762 0.072 Uiso 1 1 calc R . . C6H C -0.6485(11) -0.7188(5) -0.9489(4) 0.062(5) Uani 1 1 d . . . H6H H -0.6770 -0.7029 -0.9728 0.074 Uiso 1 1 calc R . . C7H C -0.6902(8) -0.7341(4) -0.9120(4) 0.037(4) Uani 1 1 d . . . H7H' H -0.7469 -0.7266 -0.9098 0.045 Uiso 1 1 calc R . . C8H C -0.5126(8) -0.7511(5) -0.8097(4) 0.063(5) Uani 1 1 d . . . H8HA H -0.5628 -0.7291 -0.8082 0.095 Uiso 1 1 calc R . . H8HB H -0.4660 -0.7263 -0.8143 0.095 Uiso 1 1 calc R . . H8HC H -0.5053 -0.7716 -0.7823 0.095 Uiso 1 1 calc R . . C9H C -0.4389(8) -0.8127(6) -0.8577(4) 0.082(5) Uani 1 1 d . . . H9HA H -0.4439 -0.8379 -0.8827 0.123 Uiso 1 1 calc R . . H9HB H -0.4163 -0.8331 -0.8328 0.123 Uiso 1 1 calc R . . H9HC H -0.4026 -0.7817 -0.8653 0.123 Uiso 1 1 calc R . . O1J O -0.7372(4) -0.8537(3) -0.5733(2) 0.030(2) Uani 1 1 d . . . O2J O -0.7803(5) -0.7582(3) -0.5317(2) 0.041(2) Uani 1 1 d . . . N1J N -0.7036(6) -0.8377(3) -0.5334(3) 0.028(3) Uani 1 1 d . . . H1J H -0.6583 -0.8649 -0.5195 0.050 Uiso 1 1 d . . . N2J N -0.5669(6) -0.8323(4) -0.4854(3) 0.044(3) Uani 1 1 d . . . C1J C -0.7274(8) -0.7909(5) -0.5162(4) 0.037(3) Uani 1 1 d . . . C2J C -0.6844(8) -0.7726(5) -0.4741(4) 0.034(3) Uani 1 1 d . . . C3J C -0.6123(8) -0.7933(5) -0.4587(4) 0.036(3) Uani 1 1 d . . . C4J C -0.5839(8) -0.7776(5) -0.4177(4) 0.046(4) Uani 1 1 d . . . H4J H -0.5354 -0.7937 -0.4064 0.055 Uiso 1 1 calc R . . C5J C -0.6261(9) -0.7389(5) -0.3939(4) 0.046(4) Uani 1 1 d . . . H5J H -0.6040 -0.7271 -0.3668 0.056 Uiso 1 1 calc R . . C6J C -0.6968(9) -0.7168(5) -0.4068(4) 0.051(4) Uani 1 1 d . . . H6J H -0.7258 -0.6908 -0.3894 0.062 Uiso 1 1 calc R . . C7J C -0.7267(8) -0.7347(5) -0.4486(4) 0.043(4) Uani 1 1 d . . . H7J H -0.7769 -0.7201 -0.4591 0.051 Uiso 1 1 calc R . . C8J C -0.5200(8) -0.8016(6) -0.5206(4) 0.070(5) Uani 1 1 d . . . H7JA H -0.5582 -0.7808 -0.5390 0.105 Uiso 1 1 calc R . . H8JB H -0.4900 -0.8285 -0.5385 0.105 Uiso 1 1 calc R . . H8JC H -0.4814 -0.7757 -0.5070 0.105 Uiso 1 1 calc R . . C9J C -0.5098(9) -0.8693(5) -0.4617(4) 0.065(5) Uani 1 1 d . . . H9JA H -0.5392 -0.8888 -0.4384 0.097 Uiso 1 1 calc R . . H9JB H -0.4657 -0.8471 -0.4490 0.097 Uiso 1 1 calc R . . H9JC H -0.4868 -0.8967 -0.4820 0.097 Uiso 1 1 calc R . . O1K O -0.7525(5) -0.8028(3) -0.6541(2) 0.032(2) Uani 1 1 d . . . O2K O -0.6119(5) -0.7811(3) -0.6172(2) 0.033(2) Uani 1 1 d . . . N1K N -0.7376(6) -0.7501(4) -0.6389(3) 0.026(2) Uani 1 1 d . . . H1K H -0.7943 -0.7161 -0.6405 0.050 Uiso 1 1 d . . . N2K N -0.7686(6) -0.6400(4) -0.6351(3) 0.039(3) Uani 1 1 d . . . C1K C -0.6624(9) -0.7398(5) -0.6235(4) 0.039(3) Uani 1 1 d . . . C2K C -0.6356(8) -0.6825(5) -0.6138(3) 0.036(3) Uani 1 1 d . . . C3K C -0.6848(7) -0.6337(5) -0.6217(3) 0.028(3) Uani 1 1 d . . . C4K C -0.6483(8) -0.5810(5) -0.6185(4) 0.045(4) Uani 1 1 d . . . H4K H -0.6784 -0.5483 -0.6253 0.054 Uiso 1 1 calc R . . C5K C -0.5691(9) -0.5775(6) -0.6055(4) 0.048(4) Uani 1 1 d . . . H5K H -0.5454 -0.5414 -0.6037 0.058 Uiso 1 1 calc R . . C6K C -0.5203(9) -0.6229(5) -0.5947(4) 0.044(4) Uani 1 1 d . . . H6K H -0.4661 -0.6188 -0.5843 0.053 Uiso 1 1 calc R . . C7K C -0.5552(8) -0.6720(5) -0.6002(3) 0.037(3) Uani 1 1 d . . . H7K H -0.5224 -0.7037 -0.5942 0.044 Uiso 1 1 calc R . . C8K C -0.8242(8) -0.6467(5) -0.5967(3) 0.057(4) Uani 1 1 d . . . H8KA H -0.7991 -0.6720 -0.5755 0.085 Uiso 1 1 calc R . . H8KB H -0.8764 -0.6623 -0.6064 0.085 Uiso 1 1 calc R . . H8KC H -0.8335 -0.6103 -0.5831 0.085 Uiso 1 1 calc R . . C9K C -0.8005(7) -0.5967(4) -0.6648(3) 0.042(4) Uani 1 1 d . . . H9KA H -0.7629 -0.5919 -0.6894 0.064 Uiso 1 1 calc R . . H9KB H -0.8056 -0.5613 -0.6490 0.064 Uiso 1 1 calc R . . H9KC H -0.8541 -0.6080 -0.6758 0.064 Uiso 1 1 calc R . . S1 S -0.9270(3) -1.16716(18) -0.68784(16) 0.164(3) Uani 1 1 d D . . O1SS O -0.8932 -1.1978 -0.6517 0.533 Uani 1 1 d D . . O2SS O -1.0147 -1.1605 -0.6765 0.296 Uani 1 1 d D . . O3SS O -0.9104 -1.1082 -0.6935 0.201 Uani 1 1 d D . . O4SS O -0.9035 -1.1745 -0.7329 0.661 Uani 1 1 d D . . O1 O -1.0172(5) -1.0409(4) -0.5858(2) 0.065(3) Uani 1 1 d . . . H1A' H -0.9808 -1.0648 -0.5845 0.050 Uiso 1 1 d . . . H1B' H -0.9982 -1.0258 -0.6091 0.050 Uiso 1 1 d . . . O2 O -0.8945(5) -0.7524(3) -0.6762(2) 0.040(2) Uani 1 1 d . . . H2A H -0.9316 -0.7270 -0.6796 0.050 Uiso 1 1 d . . . H2B H -0.8675 -0.7249 -0.6893 0.050 Uiso 1 1 d . . . O3 O -0.8950(5) -0.7991(3) -0.5880(2) 0.044(2) Uani 1 1 d . . . H3A H -0.8604 -0.7793 -0.5737 0.050 Uiso 1 1 d . . . H3B H -0.9364 -0.8158 -0.5780 0.050 Uiso 1 1 d . . . O4 O -0.8106(5) -1.0258(3) -0.6582(2) 0.050(2) Uani 1 1 d . . . H4A' H -0.8477 -1.0514 -0.6592 0.050 Uiso 1 1 d . . . H4B' H -0.7789 -1.0535 -0.6394 0.050 Uiso 1 1 d . . . O5 O -0.9528(6) -0.7846(4) -0.8002(3) 0.071(3) Uani 1 1 d . . . H5BB H -0.9925 -0.7910 -0.8178 0.050 Uiso 1 1 d . . . H5AA H -0.9444 -0.7562 -0.7855 0.050 Uiso 1 1 d . . . O6 O -0.7237(5) -0.9675(3) -0.7265(2) 0.046(2) Uani 1 1 d . . . H6A' H -0.6812 -0.9488 -0.7341 0.050 Uiso 1 1 d . . . H6B' H -0.6998 -0.9963 -0.7351 0.050 Uiso 1 1 d . . . O7 O -1.0233(7) -1.0323(4) -0.6728(4) 0.115(4) Uani 1 1 d . . . H7A' H -1.0019 -1.0615 -0.6736 0.050 Uiso 1 1 d . . . H7B' H -0.9901 -1.0086 -0.6870 0.050 Uiso 1 1 d . . . O8 O -1.1626(8) -1.1053(4) -0.5646(3) 0.128(5) Uani 1 1 d . . . H8A H -1.1540 -1.1210 -0.5395 0.050 Uiso 1 1 d . . . H8B H -1.1544 -1.0759 -0.5798 0.050 Uiso 1 1 d . . . O9 O -0.9635(6) -1.0648(4) -0.8460(3) 0.085(3) Uani 1 1 d . . . H9A H -0.9821 -1.0403 -0.8642 0.050 Uiso 1 1 d . . . H9B H -0.9416 -1.0736 -0.8226 0.050 Uiso 1 1 d . . . O10 O -1.1116(8) -1.2016(5) -0.6145(3) 0.123(5) Uani 1 1 d . . . H10A H -1.0874 -1.1940 -0.6401 0.050 Uiso 1 1 d . . . H10B H -1.1507 -1.1738 -0.6206 0.050 Uiso 1 1 d . . . O11 O -0.8922(6) -1.0578(4) -0.7674(3) 0.093(4) Uani 1 1 d . . . H11A H -0.9144 -1.0316 -0.7837 0.050 Uiso 1 1 d . . . H11B H -0.8244 -1.0608 -0.7739 0.050 Uiso 1 1 d . . . O12 O -0.7264(6) -1.0722(4) -0.7621(2) 0.073(3) Uani 1 1 d . . . H12A H -0.7232 -1.0997 -0.7451 0.050 Uiso 1 1 d . . . H12B H -0.7810 -1.0638 -0.7685 0.050 Uiso 1 1 d . . . O13 O -0.9796(6) -1.1749(4) -0.8171(3) 0.079(3) Uani 1 1 d . . . H13A H -1.0104 -1.1395 -0.8401 0.050 Uiso 1 1 d . . . H13B H -0.9435 -1.1891 -0.8094 0.050 Uiso 1 1 d . . . O14 O -0.9398(5) -1.3105(3) -0.7646(2) 0.055(3) Uani 1 1 d . . . H14A H -0.9113 -1.2826 -0.7695 0.050 Uiso 1 1 d . . . H14B H -0.9690 -1.2815 -0.7589 0.050 Uiso 1 1 d . . . O15 O -0.9149(8) -1.1311(4) -0.5787(4) 0.135(5) Uani 1 1 d . . . H15A H -0.8729 -1.1415 -0.5987 0.050 Uiso 1 1 d . . . H15B H -0.9442 -1.1259 -0.5607 0.050 Uiso 1 1 d . . . O16 O -0.7324(9) -1.1792(5) -0.7307(4) 0.171(6) Uani 1 1 d . . . H16A H -0.7509 -1.1750 -0.7063 0.050 Uiso 1 1 d . . . H16B H -0.6759 -1.1888 -0.7338 0.050 Uiso 1 1 d . . . O17 O -1.0212(10) -1.2186(6) -0.5464(4) 0.165(6) Uani 1 1 d . . . H17A H -0.9782 -1.2420 -0.5513 0.050 Uiso 1 1 d . . . H17B H -1.0643 -1.2104 -0.5383 0.050 Uiso 1 1 d . . . O18 O -0.4216(12) -1.2175(6) -0.4156(7) 0.258(10) Uani 1 1 d . . . H18A H -0.3905 -1.1955 -0.4266 0.050 Uiso 1 1 d . . . H18B H -0.4271 -1.2126 -0.3864 0.050 Uiso 1 1 d . . . O19 O -1.1354(15) -1.1659(7) -0.4853(4) 0.345(16) Uani 1 1 d . . . H19A H -1.0913 -1.1415 -0.4865 0.593 Uiso 1 1 d . . . H19B H -1.1761 -1.1426 -0.4844 0.675 Uiso 1 1 d . . . O20 O -0.7749(15) -1.3276(6) -0.5772(4) 0.307(13) Uani 1 1 d . . . H20A H -0.7600 -1.3051 -0.6000 0.050 Uiso 1 1 d . . . H20B H -0.7273 -1.3154 -0.5607 0.050 Uiso 1 1 d . . . O21 O -0.7463(11) -1.2489(9) -0.6530(6) 0.307(12) Uani 1 1 d . . . H21A H -0.7998 -1.2428 -0.6536 0.050 Uiso 1 1 d . . . H21B H -0.7556 -1.2728 -0.6322 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0382(12) 0.0486(12) 0.0415(11) 0.0137(9) -0.0038(10) -0.0097(9) Ni2 0.0341(12) 0.0378(10) 0.0332(10) 0.0051(7) -0.0015(9) -0.0001(8) Ni3 0.0351(11) 0.0350(10) 0.0301(10) -0.0004(8) 0.0031(9) -0.0019(8) Ni4 0.0328(11) 0.0333(9) 0.0339(10) 0.0009(8) 0.0022(9) 0.0005(8) Ni5 0.0399(12) 0.0323(9) 0.0326(10) 0.0004(7) 0.0004(9) 0.0000(8) Ni6 0.0386(12) 0.0306(9) 0.0304(10) 0.0019(8) 0.0031(9) 0.0006(9) Ni7 0.0392(12) 0.0389(10) 0.0304(10) 0.0041(8) -0.0003(9) 0.0014(9) O1A 0.039(6) 0.051(6) 0.025(5) 0.024(4) 0.004(5) 0.011(5) O2A 0.027(6) 0.058(6) 0.052(6) 0.010(5) 0.000(5) -0.023(5) N1A 0.040(8) 0.045(7) 0.037(7) 0.010(5) 0.005(6) -0.014(6) N2A 0.028(7) 0.058(8) 0.028(6) 0.011(5) 0.007(6) -0.003(6) C1A 0.026(9) 0.050(10) 0.071(12) 0.009(9) 0.009(9) 0.024(8) C2A 0.039(10) 0.048(9) 0.040(10) 0.032(8) 0.031(8) 0.019(7) C3A 0.046(11) 0.039(9) 0.052(10) -0.006(8) -0.009(9) 0.008(8) C4A 0.025(9) 0.037(8) 0.075(11) 0.005(8) 0.006(9) 0.003(7) C5A 0.044(11) 0.076(11) 0.028(9) 0.025(8) 0.007(8) -0.005(9) C6A 0.048(11) 0.054(10) 0.083(12) 0.043(9) 0.004(10) 0.014(8) C7A 0.055(11) 0.039(9) 0.045(10) 0.005(7) -0.003(8) 0.025(8) C8A 0.059(11) 0.042(8) 0.042(8) 0.006(6) -0.013(8) -0.009(8) C9A 0.093(12) 0.031(8) 0.025(8) -0.006(6) 0.014(8) -0.018(8) O1B 0.027(5) 0.031(5) 0.050(6) 0.011(4) -0.018(5) -0.015(4) O2B 0.048(6) 0.030(5) 0.040(5) 0.002(4) 0.010(5) -0.007(5) N1B 0.056(9) 0.042(7) 0.030(7) 0.005(5) 0.005(6) 0.021(7) N2B 0.075(10) 0.030(7) 0.042(8) -0.002(5) 0.000(7) 0.013(7) C1B 0.045(10) 0.032(8) 0.039(9) 0.019(7) 0.000(8) -0.017(8) C2B 0.029(9) 0.061(10) 0.027(8) -0.014(7) 0.005(7) 0.018(8) C3B 0.079(14) 0.039(9) 0.027(8) 0.007(7) 0.006(9) 0.006(9) C4B 0.062(12) 0.051(10) 0.038(9) -0.002(7) -0.017(9) 0.019(9) C5B 0.068(13) 0.048(10) 0.037(9) 0.015(7) 0.000(9) 0.023(9) C6B 0.041(10) 0.079(12) 0.034(9) -0.005(8) 0.008(8) 0.025(9) C7B 0.096(14) 0.039(9) 0.012(8) -0.001(6) -0.013(8) 0.021(9) C8B 0.053(11) 0.065(10) 0.044(9) -0.025(7) -0.007(8) 0.035(8) C9B 0.140(17) 0.022(8) 0.058(10) -0.009(7) -0.015(10) 0.007(9) O1C 0.044(6) 0.038(5) 0.019(5) 0.015(4) 0.005(5) 0.000(4) O2C 0.041(6) 0.042(5) 0.031(5) 0.005(4) -0.003(5) -0.010(5) N1C 0.021(7) 0.032(6) 0.056(8) 0.000(5) 0.009(6) -0.024(5) N2C 0.047(9) 0.057(8) 0.036(7) 0.017(6) 0.012(6) -0.006(6) C1C 0.035(10) 0.041(9) 0.033(9) 0.003(7) 0.005(8) 0.008(7) C2C 0.037(10) 0.035(8) 0.034(9) -0.002(6) 0.004(8) -0.011(7) C3C 0.042(10) 0.049(9) 0.043(10) 0.018(7) -0.020(9) 0.001(8) C4C 0.052(12) 0.070(10) 0.038(9) 0.011(7) 0.022(9) 0.000(9) C5C 0.035(9) 0.043(8) 0.045(9) -0.001(7) -0.013(8) -0.002(7) C6C 0.038(9) 0.035(8) 0.043(9) 0.011(6) -0.001(7) -0.029(7) C7C 0.039(10) 0.045(8) 0.027(8) 0.008(6) 0.001(7) -0.005(7) C8C 0.051(12) 0.123(15) 0.049(10) -0.017(10) -0.010(9) 0.031(11) C9C 0.028(10) 0.177(17) 0.036(9) 0.060(10) 0.019(8) 0.038(10) O1D 0.022(5) 0.038(5) 0.032(5) 0.003(4) -0.001(4) -0.001(4) O2D 0.028(6) 0.054(6) 0.040(6) 0.008(5) -0.009(4) -0.005(5) N1D 0.049(8) 0.022(6) 0.038(7) 0.014(5) -0.013(6) -0.004(6) N2D 0.076(10) 0.046(8) 0.023(7) 0.007(5) 0.034(7) 0.010(7) C1D 0.030(10) 0.031(9) 0.087(12) -0.012(8) -0.010(9) -0.008(7) C2D 0.021(10) 0.052(10) 0.076(12) 0.015(8) 0.017(8) 0.000(8) C3D 0.054(11) 0.039(9) 0.033(9) 0.011(7) 0.018(8) 0.020(8) C4D 0.052(12) 0.069(11) 0.053(11) 0.003(8) 0.030(9) 0.021(10) C5D 0.038(11) 0.093(14) 0.060(11) 0.024(10) 0.008(9) 0.011(10) C6D 0.027(10) 0.095(14) 0.098(13) 0.039(11) -0.016(9) 0.015(10) C7D 0.056(11) 0.041(9) 0.064(11) 0.044(8) 0.035(9) 0.009(9) C8D 0.119(16) 0.068(11) 0.050(11) 0.023(8) -0.008(10) 0.011(10) C9D 0.119(15) 0.045(9) 0.050(9) -0.023(7) 0.065(10) -0.010(9) O1E 0.038(6) 0.035(5) 0.022(5) 0.006(4) -0.006(4) 0.010(4) O2E 0.036(6) 0.027(5) 0.029(5) 0.003(4) -0.014(4) -0.011(4) N1E 0.027(6) 0.019(5) 0.021(6) -0.002(4) -0.016(5) -0.002(5) N2E 0.035(8) 0.063(8) 0.044(8) 0.014(6) 0.005(6) -0.007(6) C1E 0.030(9) 0.055(10) 0.019(8) -0.018(7) -0.003(7) 0.005(8) C2E 0.023(8) 0.026(7) 0.039(9) 0.007(6) -0.005(7) -0.003(6) C3E 0.029(9) 0.052(9) 0.029(9) -0.008(7) -0.007(8) -0.002(7) C4E 0.081(15) 0.093(14) 0.049(12) 0.021(9) 0.006(11) 0.012(11) C5E 0.081(13) 0.074(11) 0.022(9) 0.005(7) 0.007(9) -0.035(10) C6E 0.049(11) 0.057(10) 0.061(11) -0.024(8) 0.013(9) -0.026(8) C7E 0.045(10) 0.028(7) 0.036(8) -0.016(6) 0.009(8) -0.011(7) C8E 0.060(11) 0.049(9) 0.045(9) -0.013(7) 0.013(8) -0.016(8) C9E 0.067(12) 0.078(11) 0.043(9) 0.032(8) -0.020(8) -0.035(9) O1F 0.052(7) 0.027(5) 0.045(5) 0.015(4) 0.020(5) 0.007(5) O2F 0.036(6) 0.036(5) 0.032(5) 0.003(4) 0.001(4) -0.011(5) N1F 0.058(9) 0.026(6) 0.027(6) 0.012(5) 0.018(6) -0.001(6) N2F 0.074(11) 0.054(8) 0.039(9) 0.012(7) 0.017(8) 0.006(7) C1F 0.032(9) 0.031(8) 0.013(7) -0.008(6) 0.005(7) -0.010(7) C2F 0.047(11) 0.070(12) 0.043(10) -0.018(8) 0.022(9) -0.015(9) C3F 0.110(17) 0.066(12) 0.033(10) 0.010(8) 0.015(11) 0.051(13) C4F 0.074(14) 0.043(10) 0.086(14) 0.023(9) 0.034(11) 0.019(10) C5F 0.077(15) 0.072(12) 0.037(10) 0.021(8) 0.019(9) -0.027(11) C6F 0.088(15) 0.109(14) 0.035(10) -0.011(10) 0.030(10) -0.035(12) C7F 0.085(14) 0.050(10) 0.055(10) -0.011(8) 0.019(10) -0.018(10) C8F 0.19(2) 0.041(10) 0.076(13) -0.004(8) 0.025(13) -0.028(11) C9F 0.152(18) 0.059(10) 0.059(10) 0.003(8) -0.024(11) 0.054(12) O1G 0.040(6) 0.025(5) 0.041(5) -0.005(4) -0.002(5) -0.006(4) O2G 0.047(6) 0.033(5) 0.043(6) 0.002(4) 0.020(5) -0.004(5) N1G 0.024(7) 0.022(6) 0.049(7) -0.012(5) 0.008(6) -0.002(5) N2G 0.041(8) 0.036(7) 0.077(9) -0.010(6) 0.004(7) -0.003(6) C1G 0.044(10) 0.027(8) 0.026(8) 0.006(6) -0.011(7) 0.006(7) C2G 0.046(11) 0.036(9) 0.042(9) -0.002(7) 0.003(8) -0.011(7) C3G 0.023(9) 0.048(9) 0.054(9) 0.027(7) 0.002(8) 0.004(7) C4G 0.046(11) 0.053(10) 0.108(13) 0.020(9) 0.015(10) 0.002(9) C5G 0.040(10) 0.061(10) 0.058(10) 0.014(8) 0.024(8) 0.036(9) C6G 0.045(11) 0.056(9) 0.047(9) -0.012(7) 0.022(8) -0.017(8) C7G 0.052(10) 0.023(7) 0.038(8) 0.006(6) 0.015(7) -0.001(7) C8G 0.074(12) 0.070(11) 0.028(9) 0.014(7) -0.001(8) 0.016(9) C9G 0.033(10) 0.053(10) 0.162(15) -0.059(10) 0.026(11) -0.015(8) O1H 0.035(6) 0.032(5) 0.036(5) 0.010(4) 0.018(5) 0.011(4) O2H 0.054(7) 0.036(5) 0.048(6) 0.012(4) -0.009(6) 0.021(5) N1H 0.044(7) 0.020(5) 0.043(7) 0.018(5) 0.007(6) 0.000(5) N2H 0.057(9) 0.044(7) 0.019(7) -0.004(5) 0.017(6) 0.015(6) C1H 0.078(13) 0.017(7) 0.043(9) 0.007(6) -0.019(10) -0.005(8) C2H 0.045(10) 0.030(7) 0.023(8) -0.008(6) 0.010(8) -0.004(7) C3H 0.052(11) 0.036(9) 0.057(11) -0.002(7) 0.005(9) 0.028(8) C4H 0.131(17) 0.037(9) 0.025(9) 0.021(7) 0.046(11) 0.013(9) C5H 0.069(13) 0.058(11) 0.053(12) -0.004(8) 0.054(11) -0.036(10) C6H 0.095(16) 0.062(10) 0.029(10) 0.012(7) -0.013(10) -0.048(11) C7H 0.038(10) 0.030(7) 0.044(9) 0.009(6) -0.006(8) 0.014(7) C8H 0.067(12) 0.068(11) 0.055(10) 0.038(8) 0.003(9) -0.024(9) C9H 0.057(12) 0.120(15) 0.070(12) 0.024(10) 0.028(10) 0.020(11) O1J 0.019(5) 0.050(5) 0.021(5) -0.008(4) -0.004(4) -0.011(4) O2J 0.027(6) 0.045(6) 0.050(6) -0.007(4) -0.006(5) 0.009(5) N1J 0.029(7) 0.020(5) 0.035(6) -0.012(4) 0.004(6) 0.003(5) N2J 0.034(8) 0.062(8) 0.035(7) 0.004(6) -0.009(6) 0.004(6) C1J 0.014(8) 0.056(10) 0.042(9) 0.004(7) 0.004(7) -0.007(7) C2J 0.037(10) 0.025(7) 0.040(9) 0.010(6) 0.013(8) -0.005(7) C3J 0.023(9) 0.042(8) 0.042(9) -0.004(7) -0.008(8) -0.020(7) C4J 0.049(10) 0.042(9) 0.046(9) 0.002(7) -0.005(9) 0.002(7) C5J 0.037(10) 0.058(10) 0.044(10) -0.001(8) -0.007(8) 0.000(8) C6J 0.067(13) 0.047(9) 0.040(10) -0.006(7) 0.015(9) 0.002(9) C7J 0.044(10) 0.050(9) 0.035(9) -0.001(7) -0.003(8) -0.024(8) C8J 0.068(13) 0.099(13) 0.042(10) -0.005(8) 0.022(9) -0.013(10) C9J 0.078(13) 0.081(12) 0.036(9) -0.016(8) -0.011(9) -0.021(10) O1K 0.038(6) 0.022(5) 0.038(5) -0.003(4) -0.006(4) -0.010(4) O2K 0.023(5) 0.044(5) 0.032(5) 0.008(4) -0.003(4) -0.003(4) N1K 0.017(6) 0.028(6) 0.033(7) -0.003(5) -0.005(5) -0.006(5) N2K 0.034(7) 0.024(6) 0.059(8) -0.003(5) 0.006(6) -0.008(5) C1K 0.037(10) 0.057(10) 0.022(8) -0.016(7) 0.018(8) -0.002(8) C2K 0.043(10) 0.037(8) 0.029(8) -0.032(6) -0.005(7) -0.024(7) C3K 0.029(9) 0.034(8) 0.022(7) 0.009(6) 0.003(7) -0.003(6) C4K 0.061(12) 0.017(7) 0.057(9) -0.002(6) 0.022(9) -0.003(7) C5K 0.045(11) 0.077(12) 0.022(8) -0.012(7) -0.013(7) -0.047(9) C6K 0.057(12) 0.035(9) 0.040(9) -0.010(7) 0.000(8) -0.010(8) C7K 0.049(10) 0.045(9) 0.016(7) 0.004(6) -0.010(7) 0.016(8) C8K 0.069(12) 0.061(9) 0.041(8) 0.008(7) 0.028(9) 0.000(9) C9K 0.028(9) 0.051(9) 0.047(9) 0.012(6) 0.015(7) 0.002(7) S1 0.187(7) 0.090(4) 0.215(6) -0.040(4) 0.103(5) -0.064(4) O1SS 0.214 1.347 0.039 0.181 0.017 0.216 O2SS 0.200 0.530 0.158 0.223 0.023 0.190 O3SS 0.287 0.153 0.162 0.026 -0.055 -0.111 O4SS 0.572 1.229 0.182 -0.175 0.277 -0.522 O1 0.045(7) 0.101(8) 0.048(6) 0.028(5) -0.013(5) -0.023(6) O2 0.047(6) 0.023(5) 0.050(5) 0.019(4) -0.001(5) 0.002(4) O3 0.033(6) 0.069(6) 0.029(5) -0.018(4) 0.005(4) -0.015(5) O4 0.053(7) 0.031(5) 0.065(6) 0.007(4) 0.003(5) -0.007(5) O5 0.037(7) 0.097(8) 0.078(7) -0.002(6) -0.005(6) 0.025(6) O6 0.061(7) 0.038(5) 0.039(5) 0.002(4) 0.014(5) 0.008(5) O7 0.101(11) 0.088(9) 0.156(11) 0.052(8) -0.025(9) -0.028(7) O8 0.160(13) 0.120(9) 0.105(9) 0.024(7) -0.031(9) -0.055(9) O9 0.110(10) 0.063(7) 0.083(7) 0.019(6) 0.002(7) -0.011(7) O10 0.129(12) 0.129(11) 0.112(9) -0.052(7) 0.055(9) -0.043(9) O11 0.078(9) 0.086(8) 0.115(9) 0.009(6) 0.007(7) 0.029(7) O12 0.083(8) 0.083(7) 0.053(6) -0.007(5) -0.009(6) 0.006(7) O13 0.072(8) 0.087(8) 0.078(7) -0.009(6) 0.004(6) -0.008(6) O14 0.045(6) 0.058(6) 0.061(6) -0.001(5) 0.006(5) 0.013(5) O15 0.114(12) 0.092(9) 0.200(13) -0.019(9) -0.034(10) -0.033(8) O16 0.188(16) 0.115(10) 0.210(13) -0.039(10) 0.002(12) -0.046(11) O17 0.222(19) 0.159(14) 0.115(11) 0.013(9) -0.012(11) -0.040(12) O18 0.19(2) 0.152(15) 0.43(3) 0.073(17) 0.13(2) 0.057(14) O19 0.66(5) 0.27(2) 0.098(11) 0.045(12) 0.066(19) -0.16(3) O20 0.58(4) 0.174(15) 0.169(13) -0.066(12) -0.15(2) 0.11(2) O21 0.168(19) 0.45(3) 0.30(2) 0.23(2) 0.022(16) 0.008(19) _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 O2A 1.993(8) . ? Ni1 N1C 2.001(9) . ? Ni1 O1A 2.066(8) . ? Ni1 O1 2.074(9) . ? Ni1 O1B 2.116(8) . ? Ni1 N2C 2.211(11) . ? Ni1 Ni2 2.959(3) . ? Ni2 O1J 1.981(7) . ? Ni2 O2B 2.017(8) . ? Ni2 O1A 2.043(8) . ? Ni2 O1C 2.044(7) . ? Ni2 O1B 2.064(7) . ? Ni2 O1D 2.111(7) . ? Ni3 O2C 1.987(8) . ? Ni3 O2 1.994(6) . ? Ni3 O3 2.070(7) . ? Ni3 O1C 2.073(7) . ? Ni3 O1K 2.093(8) . ? Ni3 O1E 2.193(7) . ? Ni4 O2D 2.007(8) . ? Ni4 O2K 2.008(8) . ? Ni4 O1J 2.023(7) . ? Ni4 O1G 2.052(7) . ? Ni4 O1K 2.069(7) . ? Ni4 O1D 2.090(7) . ? Ni5 O4 2.011(7) . ? Ni5 O2E 2.027(7) . ? Ni5 O1D 2.045(7) . ? Ni5 O6 2.047(8) . ? Ni5 O1E 2.079(6) . ? Ni5 O1C 2.155(7) . ? Ni6 O1G 1.980(8) . ? Ni6 O2F 1.983(7) . ? Ni6 O1E 2.008(8) . ? Ni6 O1K 2.076(7) . ? Ni6 O1H 2.084(7) . ? Ni6 O1F 2.085(7) . ? Ni6 Ni7 2.944(2) . ? Ni7 N1E 2.008(9) . ? Ni7 O1H 2.033(8) . ? Ni7 O2H 2.036(8) . ? Ni7 O5 2.090(9) . ? Ni7 O1F 2.144(8) . ? Ni7 N2E 2.149(10) . ? O1A N1A 1.399(10) . ? O2A C1A 1.307(14) . ? N1A C1A 1.371(15) . ? N2A C3A 1.437(15) . ? N2A C9A 1.448(12) . ? N2A C8A 1.456(14) . ? C1A C2A 1.548(16) . ? C2A C3A 1.359(16) . ? C2A C7A 1.372(15) . ? C3A C4A 1.390(15) . ? C4A C5A 1.297(15) . ? C5A C6A 1.477(16) . ? C6A C7A 1.405(15) . ? O1B N1B 1.385(11) . ? O2B C1B 1.266(12) . ? N1B C1B 1.329(15) . ? N2B C8B 1.427(14) . ? N2B C9B 1.433(12) . ? N2B C3B 1.480(17) . ? C1B C2B 1.519(16) . ? C2B C7B 1.385(17) . ? C2B C3B 1.429(16) . ? C3B C4B 1.344(17) . ? C4B C5B 1.363(17) . ? C5B C6B 1.383(15) . ? C6B C7B 1.428(16) . ? O1C N1C 1.449(11) . ? O2C C1C 1.272(13) . ? N1C C1C 1.298(13) . ? N2C C3C 1.439(14) . ? N2C C8C 1.499(14) . ? N2C C9C 1.508(13) . ? C1C C2C 1.531(16) . ? C2C C3C 1.340(15) . ? C2C C7C 1.406(14) . ? C3C C4C 1.386(17) . ? C4C C5C 1.396(15) . ? C5C C6C 1.331(14) . ? C6C C7C 1.387(15) . ? O1D N1D 1.443(11) . ? O2D C1D 1.262(13) . ? N1D C1D 1.280(14) . ? N2D C9D 1.438(13) . ? N2D C8D 1.454(13) . ? N2D C3D 1.486(16) . ? C1D C2D 1.531(17) . ? C2D C3D 1.344(16) . ? C2D C7D 1.407(17) . ? C3D C4D 1.375(17) . ? C4D C5D 1.399(17) . ? C5D C6D 1.393(18) . ? C6D C7D 1.346(16) . ? O1E N1E 1.443(10) . ? O2E C1E 1.344(13) . ? N1E C1E 1.300(13) . ? N2E C3E 1.453(15) . ? N2E C9E 1.487(12) . ? N2E C8E 1.497(14) . ? C1E C2E 1.412(15) . ? C2E C7E 1.349(15) . ? C2E C3E 1.461(14) . ? C3E C4E 1.391(16) . ? C4E C5E 1.433(18) . ? C5E C6E 1.341(14) . ? C6E C7E 1.457(16) . ? O1F N1F 1.446(11) . ? O2F C1F 1.221(13) . ? N1F C1F 1.307(14) . ? N2F C3F 1.366(18) . ? N2F C9F 1.424(14) . ? N2F C8F 1.446(14) . ? C1F C2F 1.507(16) . ? C2F C3F 1.385(17) . ? C2F C7F 1.401(18) . ? C3F C4F 1.53(2) . ? C4F C5F 1.357(18) . ? C5F C6F 1.391(19) . ? C6F C7F 1.462(17) . ? O1G N1G 1.413(11) . ? O2G C1G 1.235(12) . ? N1G C1G 1.329(13) . ? N2G C3G 1.468(14) . ? N2G C8G 1.482(12) . ? N2G C9G 1.533(13) . ? C1G C2G 1.500(17) . ? C2G C3G 1.385(15) . ? C2G C7G 1.437(15) . ? C3G C4G 1.446(16) . ? C4G C5G 1.388(15) . ? C5G C6G 1.363(16) . ? C6G C7G 1.400(16) . ? O1H N1H 1.420(10) . ? O2H C1H 1.295(16) . ? N1H C1H 1.266(13) . ? N2H C3H 1.405(15) . ? N2H C9H 1.442(14) . ? N2H C8H 1.482(14) . ? C1H C2H 1.535(16) . ? C2H C7H 1.378(14) . ? C2H C3H 1.459(16) . ? C3H C4H 1.404(16) . ? C4H C5H 1.347(18) . ? C5H C6H 1.357(19) . ? C6H C7H 1.371(16) . ? O1J N1J 1.395(9) . ? O2J C1J 1.264(13) . ? N1J C1J 1.300(13) . ? N2J C3J 1.447(14) . ? N2J C9J 1.482(14) . ? N2J C8J 1.517(13) . ? C1J C2J 1.536(16) . ? C2J C3J 1.367(16) . ? C2J C7J 1.384(15) . ? C3J C4J 1.392(14) . ? C4J C5J 1.371(15) . ? C5J C6J 1.334(16) . ? C6J C7J 1.438(14) . ? O1K N1K 1.370(9) . ? O2K C1K 1.306(13) . ? N1K C1K 1.344(14) . ? N2K C3K 1.443(13) . ? N2K C9K 1.479(12) . ? N2K C8K 1.497(13) . ? C1K C2K 1.474(15) . ? C2K C7K 1.405(15) . ? C2K C3K 1.442(15) . ? C3K C4K 1.401(14) . ? C4K C5K 1.361(16) . ? C5K C6K 1.392(17) . ? C6K C7K 1.322(15) . ? S1 O1SS 1.441(5) . ? S1 O4SS 1.445(5) . ? S1 O3SS 1.452(4) . ? S1 O2SS 1.487(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2A Ni1 N1C 168.7(4) . . ? O2A Ni1 O1A 82.8(3) . . ? N1C Ni1 O1A 86.4(3) . . ? O2A Ni1 O1 92.3(3) . . ? N1C Ni1 O1 98.0(3) . . ? O1A Ni1 O1 171.6(3) . . ? O2A Ni1 O1B 88.2(3) . . ? N1C Ni1 O1B 86.8(4) . . ? O1A Ni1 O1B 81.6(3) . . ? O1 Ni1 O1B 91.4(3) . . ? O2A Ni1 N2C 97.6(4) . . ? N1C Ni1 N2C 87.5(4) . . ? O1A Ni1 N2C 99.0(4) . . ? O1 Ni1 N2C 88.4(4) . . ? O1B Ni1 N2C 174.2(3) . . ? O2A Ni1 Ni2 101.9(2) . . ? N1C Ni1 Ni2 67.6(3) . . ? O1A Ni1 Ni2 43.6(2) . . ? O1 Ni1 Ni2 131.8(3) . . ? O1B Ni1 Ni2 44.23(18) . . ? N2C Ni1 Ni2 133.6(3) . . ? O1J Ni2 O2B 96.9(3) . . ? O1J Ni2 O1A 98.3(3) . . ? O2B Ni2 O1A 98.6(3) . . ? O1J Ni2 O1C 95.6(3) . . ? O2B Ni2 O1C 164.3(3) . . ? O1A Ni2 O1C 89.0(3) . . ? O1J Ni2 O1B 177.3(3) . . ? O2B Ni2 O1B 80.8(3) . . ? O1A Ni2 O1B 83.4(3) . . ? O1C Ni2 O1B 86.4(3) . . ? O1J Ni2 O1D 81.2(3) . . ? O2B Ni2 O1D 98.2(3) . . ? O1A Ni2 O1D 163.1(3) . . ? O1C Ni2 O1D 74.3(3) . . ? O1B Ni2 O1D 97.8(3) . . ? O1J Ni2 Ni1 136.8(2) . . ? O2B Ni2 Ni1 107.8(2) . . ? O1A Ni2 Ni1 44.2(2) . . ? O1C Ni2 Ni1 68.5(2) . . ? O1B Ni2 Ni1 45.6(2) . . ? O1D Ni2 Ni1 127.6(2) . . ? O2C Ni3 O2 95.3(3) . . ? O2C Ni3 O3 94.0(3) . . ? O2 Ni3 O3 92.2(3) . . ? O2C Ni3 O1C 78.0(3) . . ? O2 Ni3 O1C 173.3(3) . . ? O3 Ni3 O1C 88.2(3) . . ? O2C Ni3 O1K 170.0(3) . . ? O2 Ni3 O1K 83.0(3) . . ? O3 Ni3 O1K 96.0(3) . . ? O1C Ni3 O1K 103.6(3) . . ? O2C Ni3 O1E 98.8(3) . . ? O2 Ni3 O1E 99.0(3) . . ? O3 Ni3 O1E 162.2(3) . . ? O1C Ni3 O1E 82.3(3) . . ? O1K Ni3 O1E 71.8(3) . . ? O2D Ni4 O2K 97.6(3) . . ? O2D Ni4 O1J 98.6(3) . . ? O2K Ni4 O1J 96.7(3) . . ? O2D Ni4 O1G 96.8(3) . . ? O2K Ni4 O1G 99.7(3) . . ? O1J Ni4 O1G 155.7(3) . . ? O2D Ni4 O1K 175.6(3) . . ? O2K Ni4 O1K 80.0(3) . . ? O1J Ni4 O1K 85.3(3) . . ? O1G Ni4 O1K 80.1(3) . . ? O2D Ni4 O1D 80.3(3) . . ? O2K Ni4 O1D 176.4(3) . . ? O1J Ni4 O1D 80.7(3) . . ? O1G Ni4 O1D 83.6(3) . . ? O1K Ni4 O1D 102.3(3) . . ? O4 Ni5 O2E 92.4(3) . . ? O4 Ni5 O1D 86.2(3) . . ? O2E Ni5 O1D 170.8(3) . . ? O4 Ni5 O6 90.9(3) . . ? O2E Ni5 O6 95.7(3) . . ? O1D Ni5 O6 93.4(3) . . ? O4 Ni5 O1E 171.9(3) . . ? O2E Ni5 O1E 79.4(3) . . ? O1D Ni5 O1E 101.9(3) . . ? O6 Ni5 O1E 89.8(3) . . ? O4 Ni5 O1C 98.2(3) . . ? O2E Ni5 O1C 97.9(3) . . ? O1D Ni5 O1C 73.3(3) . . ? O6 Ni5 O1C 163.2(3) . . ? O1E Ni5 O1C 83.1(3) . . ? O1G Ni6 O2F 93.5(3) . . ? O1G Ni6 O1E 96.1(3) . . ? O2F Ni6 O1E 165.9(3) . . ? O1G Ni6 O1K 81.6(3) . . ? O2F Ni6 O1K 95.3(3) . . ? O1E Ni6 O1K 76.0(3) . . ? O1G Ni6 O1H 100.6(3) . . ? O2F Ni6 O1H 99.1(3) . . ? O1E Ni6 O1H 89.3(3) . . ? O1K Ni6 O1H 165.3(3) . . ? O1G Ni6 O1F 174.3(3) . . ? O2F Ni6 O1F 81.5(3) . . ? O1E Ni6 O1F 88.4(3) . . ? O1K Ni6 O1F 96.2(3) . . ? O1H Ni6 O1F 82.9(3) . . ? O1G Ni6 Ni7 138.4(2) . . ? O2F Ni6 Ni7 110.0(2) . . ? O1E Ni6 Ni7 68.7(2) . . ? O1K Ni6 Ni7 127.4(2) . . ? O1H Ni6 Ni7 43.6(2) . . ? O1F Ni6 Ni7 46.7(2) . . ? N1E Ni7 O1H 87.7(3) . . ? N1E Ni7 O2H 168.1(4) . . ? O1H Ni7 O2H 80.5(3) . . ? N1E Ni7 O5 93.4(4) . . ? O1H Ni7 O5 173.4(3) . . ? O2H Ni7 O5 98.3(3) . . ? N1E Ni7 O1F 87.9(3) . . ? O1H Ni7 O1F 82.7(3) . . ? O2H Ni7 O1F 89.5(3) . . ? O5 Ni7 O1F 90.8(3) . . ? N1E Ni7 N2E 86.1(4) . . ? O1H Ni7 N2E 96.6(4) . . ? O2H Ni7 N2E 96.3(4) . . ? O5 Ni7 N2E 89.9(4) . . ? O1F Ni7 N2E 174.0(3) . . ? N1E Ni7 Ni6 67.3(3) . . ? O1H Ni7 Ni6 45.1(2) . . ? O2H Ni7 Ni6 102.9(3) . . ? O5 Ni7 Ni6 129.7(2) . . ? O1F Ni7 Ni6 45.0(2) . . ? N2E Ni7 Ni6 131.4(3) . . ? N1A O1A Ni2 116.2(6) . . ? N1A O1A Ni1 108.0(6) . . ? Ni2 O1A Ni1 92.1(3) . . ? C1A O2A Ni1 110.9(8) . . ? C1A N1A O1A 116.3(10) . . ? C3A N2A C9A 116.7(10) . . ? C3A N2A C8A 109.1(10) . . ? C9A N2A C8A 110.0(10) . . ? O2A C1A N1A 121.9(12) . . ? O2A C1A C2A 123.0(13) . . ? N1A C1A C2A 115.1(12) . . ? C3A C2A C7A 119.3(12) . . ? C3A C2A C1A 127.1(13) . . ? C7A C2A C1A 113.2(14) . . ? C2A C3A C4A 118.4(13) . . ? C2A C3A N2A 121.2(13) . . ? C4A C3A N2A 120.4(12) . . ? C5A C4A C3A 123.7(14) . . ? C4A C5A C6A 121.3(13) . . ? C7A C6A C5A 112.3(12) . . ? C2A C7A C6A 124.8(13) . . ? N1B O1B Ni2 106.6(6) . . ? N1B O1B Ni1 127.1(6) . . ? Ni2 O1B Ni1 90.1(3) . . ? C1B O2B Ni2 112.8(8) . . ? C1B N1B O1B 119.9(10) . . ? C8B N2B C9B 114.1(11) . . ? C8B N2B C3B 112.8(10) . . ? C9B N2B C3B 112.3(12) . . ? O2B C1B N1B 119.5(12) . . ? O2B C1B C2B 118.8(12) . . ? N1B C1B C2B 121.6(11) . . ? C7B C2B C3B 120.0(13) . . ? C7B C2B C1B 115.0(12) . . ? C3B C2B C1B 124.7(13) . . ? C4B C3B C2B 119.5(15) . . ? C4B C3B N2B 122.0(13) . . ? C2B C3B N2B 118.5(13) . . ? C3B C4B C5B 121.6(15) . . ? C4B C5B C6B 120.9(14) . . ? C5B C6B C7B 119.5(14) . . ? C2B C7B C6B 118.3(13) . . ? N1C O1C Ni2 109.4(6) . . ? N1C O1C Ni3 109.7(6) . . ? Ni2 O1C Ni3 121.6(4) . . ? N1C O1C Ni5 117.0(6) . . ? Ni2 O1C Ni5 101.0(3) . . ? Ni3 O1C Ni5 97.9(3) . . ? C1C O2C Ni3 110.7(8) . . ? C1C N1C O1C 109.7(9) . . ? C1C N1C Ni1 129.6(9) . . ? O1C N1C Ni1 114.3(7) . . ? C3C N2C C8C 110.0(10) . . ? C3C N2C C9C 116.2(11) . . ? C8C N2C C9C 105.4(10) . . ? C3C N2C Ni1 108.7(8) . . ? C8C N2C Ni1 110.9(8) . . ? C9C N2C Ni1 105.6(7) . . ? O2C C1C N1C 125.8(13) . . ? O2C C1C C2C 118.5(11) . . ? N1C C1C C2C 115.1(12) . . ? C3C C2C C7C 119.2(12) . . ? C3C C2C C1C 123.7(13) . . ? C7C C2C C1C 117.1(12) . . ? C2C C3C C4C 117.3(13) . . ? C2C C3C N2C 123.3(13) . . ? C4C C3C N2C 119.0(13) . . ? C3C C4C C5C 123.0(12) . . ? C6C C5C C4C 120.2(12) . . ? C5C C6C C7C 117.0(12) . . ? C6C C7C C2C 123.2(11) . . ? N1D O1D Ni5 118.7(6) . . ? N1D O1D Ni4 104.2(6) . . ? Ni5 O1D Ni4 120.2(3) . . ? N1D O1D Ni2 113.3(5) . . ? Ni5 O1D Ni2 102.5(3) . . ? Ni4 O1D Ni2 95.8(3) . . ? C1D O2D Ni4 111.7(8) . . ? C1D N1D O1D 117.0(10) . . ? C9D N2D C8D 113.0(10) . . ? C9D N2D C3D 117.1(11) . . ? C8D N2D C3D 107.3(11) . . ? O2D C1D N1D 122.9(13) . . ? O2D C1D C2D 120.9(12) . . ? N1D C1D C2D 116.1(12) . . ? C3D C2D C7D 117.4(14) . . ? C3D C2D C1D 128.6(14) . . ? C7D C2D C1D 113.8(13) . . ? C2D C3D C4D 121.9(15) . . ? C2D C3D N2D 117.0(13) . . ? C4D C3D N2D 121.1(14) . . ? C3D C4D C5D 120.4(15) . . ? C6D C5D C4D 118.0(15) . . ? C7D C6D C5D 119.8(16) . . ? C6D C7D C2D 122.4(15) . . ? N1E O1E Ni6 110.5(5) . . ? N1E O1E Ni5 109.7(5) . . ? Ni6 O1E Ni5 123.6(4) . . ? N1E O1E Ni3 114.3(6) . . ? Ni6 O1E Ni3 101.3(3) . . ? Ni5 O1E Ni3 96.5(3) . . ? C1E O2E Ni5 110.4(7) . . ? C1E N1E O1E 113.2(9) . . ? C1E N1E Ni7 129.5(8) . . ? O1E N1E Ni7 113.3(6) . . ? C3E N2E C9E 112.0(10) . . ? C3E N2E C8E 107.8(10) . . ? C9E N2E C8E 107.5(10) . . ? C3E N2E Ni7 111.0(8) . . ? C9E N2E Ni7 108.2(7) . . ? C8E N2E Ni7 110.1(7) . . ? N1E C1E O2E 123.8(11) . . ? N1E C1E C2E 119.1(12) . . ? O2E C1E C2E 117.1(11) . . ? C7E C2E C1E 118.9(12) . . ? C7E C2E C3E 117.4(12) . . ? C1E C2E C3E 123.7(12) . . ? C4E C3E N2E 121.5(12) . . ? C4E C3E C2E 120.1(13) . . ? N2E C3E C2E 118.4(11) . . ? C3E C4E C5E 119.3(13) . . ? C6E C5E C4E 121.7(14) . . ? C5E C6E C7E 117.9(13) . . ? C2E C7E C6E 123.2(12) . . ? N1F O1F Ni6 104.4(6) . . ? N1F O1F Ni7 126.3(6) . . ? Ni6 O1F Ni7 88.2(3) . . ? C1F O2F Ni6 113.4(8) . . ? C1F N1F O1F 117.5(10) . . ? C3F N2F C9F 121.0(13) . . ? C3F N2F C8F 115.6(13) . . ? C9F N2F C8F 104.3(11) . . ? O2F C1F N1F 123.1(12) . . ? O2F C1F C2F 122.2(13) . . ? N1F C1F C2F 114.7(13) . . ? C3F C2F C7F 120.4(16) . . ? C3F C2F C1F 126.1(16) . . ? C7F C2F C1F 112.9(14) . . ? N2F C3F C2F 123.3(18) . . ? N2F C3F C4F 119.2(14) . . ? C2F C3F C4F 117.1(16) . . ? C5F C4F C3F 117.4(14) . . ? C4F C5F C6F 127.6(16) . . ? C5F C6F C7F 112.6(16) . . ? C2F C7F C6F 124.4(15) . . ? N1G O1G Ni6 115.4(6) . . ? N1G O1G Ni4 117.1(6) . . ? Ni6 O1G Ni4 101.0(3) . . ? C1G N1G O1G 121.1(9) . . ? C3G N2G C8G 110.1(9) . . ? C3G N2G C9G 114.3(10) . . ? C8G N2G C9G 112.6(10) . . ? O2G C1G N1G 121.6(13) . . ? O2G C1G C2G 123.8(12) . . ? N1G C1G C2G 114.6(11) . . ? C3G C2G C7G 119.3(13) . . ? C3G C2G C1G 128.7(12) . . ? C7G C2G C1G 112.0(11) . . ? C2G C3G C4G 120.9(13) . . ? C2G C3G N2G 118.4(12) . . ? C4G C3G N2G 120.6(13) . . ? C5G C4G C3G 117.3(14) . . ? C6G C5G C4G 122.6(14) . . ? C5G C6G C7G 121.1(12) . . ? C6G C7G C2G 118.7(12) . . ? N1H O1H Ni7 107.6(5) . . ? N1H O1H Ni6 117.6(6) . . ? Ni7 O1H Ni6 91.3(3) . . ? C1H O2H Ni7 111.2(8) . . ? C1H N1H O1H 119.0(11) . . ? C3H N2H C9H 115.3(10) . . ? C3H N2H C8H 109.1(10) . . ? C9H N2H C8H 111.0(11) . . ? N1H C1H O2H 120.5(13) . . ? N1H C1H C2H 120.8(14) . . ? O2H C1H C2H 118.5(11) . . ? C7H C2H C3H 118.8(12) . . ? C7H C2H C1H 118.0(12) . . ? C3H C2H C1H 123.1(12) . . ? C4H C3H N2H 121.5(14) . . ? C4H C3H C2H 117.8(13) . . ? N2H C3H C2H 120.3(13) . . ? C5H C4H C3H 119.0(15) . . ? C4H C5H C6H 122.9(14) . . ? C5H C6H C7H 120.4(14) . . ? C6H C7H C2H 120.1(13) . . ? N1J O1J Ni2 117.1(5) . . ? N1J O1J Ni4 119.4(6) . . ? Ni2 O1J Ni4 102.3(3) . . ? C1J N1J O1J 118.4(10) . . ? C3J N2J C9J 115.9(10) . . ? C3J N2J C8J 110.4(10) . . ? C9J N2J C8J 108.6(10) . . ? O2J C1J N1J 126.2(12) . . ? O2J C1J C2J 117.0(12) . . ? N1J C1J C2J 116.8(12) . . ? C3J C2J C7J 118.7(13) . . ? C3J C2J C1J 125.6(12) . . ? C7J C2J C1J 115.6(12) . . ? C2J C3J C4J 120.1(13) . . ? C2J C3J N2J 119.1(12) . . ? C4J C3J N2J 120.8(12) . . ? C5J C4J C3J 119.8(13) . . ? C6J C5J C4J 123.3(13) . . ? C5J C6J C7J 116.3(13) . . ? C2J C7J C6J 121.8(13) . . ? N1K O1K Ni4 107.6(6) . . ? N1K O1K Ni6 116.1(5) . . ? Ni4 O1K Ni6 97.3(3) . . ? N1K O1K Ni3 114.7(6) . . ? Ni4 O1K Ni3 117.7(3) . . ? Ni6 O1K Ni3 102.4(3) . . ? C1K O2K Ni4 111.7(8) . . ? C1K N1K O1K 117.0(9) . . ? C3K N2K C9K 116.0(9) . . ? C3K N2K C8K 111.6(10) . . ? C9K N2K C8K 110.2(9) . . ? O2K C1K N1K 119.6(11) . . ? O2K C1K C2K 119.3(13) . . ? N1K C1K C2K 121.1(12) . . ? C7K C2K C3K 115.4(11) . . ? C7K C2K C1K 120.4(13) . . ? C3K C2K C1K 123.9(12) . . ? C4K C3K C2K 118.8(12) . . ? C4K C3K N2K 121.4(11) . . ? C2K C3K N2K 119.7(10) . . ? C5K C4K C3K 118.9(12) . . ? C4K C5K C6K 124.7(13) . . ? C7K C6K C5K 114.8(14) . . ? C6K C7K C2K 127.1(13) . . ? O1SS S1 O4SS 124.7(4) . . ? O1SS S1 O3SS 121.2(4) . . ? O4SS S1 O3SS 87.4(2) . . ? O1SS S1 O2SS 104.3(3) . . ? O4SS S1 O2SS 119.6(4) . . ? O3SS S1 O2SS 96.0(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.312 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.089