# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yahong Li' _publ_contact_author_email LIYAHONG@SUDA.EDU.CN _publ_section_title ; Wheel-like MnII6 and NiII6 complexes from the use of 2-pyidinealdoxime and carboxylates ; loop_ _publ_author_name 'Yahong Li' 'Euan Brechin' 'Wenqian Chen' 'Ross Inglis' 'Konstantis F. Konidaris' 'Kai Li' 'Spyros Perlepes' ; B.Xu ; 'Yong Zhang' 'Su-Yun Zhang' 'Lina Zhen' # Attachment '1.cif' data_aa _database_code_depnum_ccdc_archive 'CCDC 668060' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 N12 Ni6 O19' _chemical_formula_weight 1451.26 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.326(2) _cell_length_b 14.326(2) _cell_length_c 24.550(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4363.5(15) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3992 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.85 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2226 _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6105 _exptl_absorpt_correction_T_max 0.7228 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 8793 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1660 _reflns_number_gt 1399 _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^)+(0.1698P)^2^+42.7978P] 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 1660 _refine_ls_number_parameters 131 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2421 _refine_ls_wR_factor_gt 0.2236 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.056 _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 0.78832(7) 0.82258(7) 0.03871(3) 0.0423(5) Uani 1 1 d . . . O1 O 1.0182(5) 0.8575(5) 0.0431(4) 0.088(2) Uani 1 1 d . . . O2 O 0.7177(5) 0.6595(5) 0.0265(2) 0.0685(17) Uani 1 1 d . . . O3 O 0.8372(7) 0.6395(5) -0.0238(3) 0.080(2) Uani 1 1 d . . . O4 O 0.3333 0.6667 0.1667 0.29(3) Uani 1 6 d S . . H1W H 0.3182 0.7153 0.1704 0.434 Uiso 0.33 1 d PR . . N1 N 0.7536(5) 0.7951(5) 0.1221(3) 0.0513(13) Uani 1 1 d DU . . N2 N 0.9297(6) 0.8340(7) 0.0626(4) 0.0733(19) Uani 1 1 d DU . . C1 C 0.6648(9) 0.7629(6) 0.1474(4) 0.084(2) Uani 1 1 d DU . . H1 H 0.6056 0.7548 0.1279 0.101 Uiso 1 1 calc R . . C2 C 0.6524(10) 0.7391(8) 0.2034(5) 0.095(3) Uani 1 1 d DU . . H2 H 0.5862 0.7154 0.2203 0.114 Uiso 1 1 calc R . . C3 C 0.7356(10) 0.7506(8) 0.2317(5) 0.093(3) Uani 1 1 d DU . . H3 H 0.7269 0.7354 0.2688 0.111 Uiso 1 1 calc R . . C4 C 0.8316(10) 0.7832(8) 0.2093(5) 0.085(2) Uani 1 1 d DU . . H4 H 0.8900 0.7910 0.2295 0.101 Uiso 1 1 calc R . . C5 C 0.8391(8) 0.8050(6) 0.1530(4) 0.0693(19) Uani 1 1 d DU . . C6 C 0.9370(9) 0.8293(9) 0.1187(4) 0.077(2) Uani 1 1 d DU . . H6 H 1.0004 0.8408 0.1351 0.093 Uiso 1 1 calc R . . C7 C 0.7488(8) 0.6056(7) -0.0004(3) 0.062(2) Uani 1 1 d U . . C8 C 0.6699(10) 0.4855(8) -0.0050(4) 0.081(3) Uani 1 1 d U . . H8A H 0.6818 0.4484 0.0243 0.122 Uiso 1 1 calc R . . H8B H 0.6804 0.4595 -0.0392 0.122 Uiso 1 1 calc R . . H8C H 0.5975 0.4728 -0.0032 0.122 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 0.0402(6) 0.0463(6) 0.0274(6) 0.0025(3) 0.0019(3) 0.0119(4) O1 0.045(3) 0.058(3) 0.161(8) 0.020(4) 0.002(4) 0.025(3) O2 0.071(4) 0.051(3) 0.047(3) -0.008(2) 0.014(3) 0.002(3) O3 0.122(6) 0.042(3) 0.065(4) 0.002(3) 0.023(4) 0.034(3) O4 0.20(3) 0.20(3) 0.46(11) 0.000 0.000 0.102(16) N1 0.053(3) 0.049(3) 0.047(3) 0.003(2) 0.005(2) 0.022(2) N2 0.060(4) 0.061(4) 0.102(4) 0.027(3) 0.011(3) 0.032(3) C1 0.070(4) 0.093(5) 0.071(4) 0.010(4) 0.013(4) 0.027(4) C2 0.082(4) 0.108(5) 0.069(4) 0.009(4) 0.017(4) 0.027(4) C3 0.089(5) 0.104(5) 0.070(4) 0.016(4) 0.013(4) 0.037(4) C4 0.085(4) 0.091(5) 0.064(4) 0.006(4) -0.001(4) 0.033(4) C5 0.073(4) 0.067(4) 0.061(4) 0.002(3) -0.002(3) 0.030(3) C6 0.076(4) 0.076(4) 0.075(4) 0.005(4) 0.004(4) 0.034(4) C7 0.083(5) 0.044(3) 0.042(4) 0.003(3) 0.006(3) 0.020(3) C8 0.099(6) 0.054(4) 0.067(5) 0.007(4) -0.017(4) 0.021(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 O1 2.021(6) 3_675 ? Ni1 N2 2.036(8) . ? Ni1 O3 2.036(7) 11_565 ? Ni1 O2 2.052(6) . ? Ni1 N1 2.097(6) . ? Ni1 O1 2.199(10) 11_565 ? O1 N2 1.233(10) . ? O1 Ni1 2.021(6) 2_765 ? O1 Ni1 2.199(10) 12_655 ? O2 C7 1.255(12) . ? O3 C7 1.247(12) . ? O3 Ni1 2.036(7) 12_655 ? O4 H1W 0.8324 . ? N1 C1 1.277(12) . ? N1 C5 1.386(12) . ? N2 C6 1.386(11) . ? C1 C2 1.406(16) . ? C1 H1 0.9300 . ? C2 C3 1.317(18) . ? C2 H2 0.9300 . ? C3 C4 1.329(18) . ? C3 H3 0.9300 . ? C4 C5 1.410(14) . ? C4 H4 0.9300 . ? C5 C6 1.519(15) . ? C6 H6 0.9300 . ? C7 C8 1.518(13) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 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 O1 Ni1 N2 96.3(3) 3_675 . ? O1 Ni1 O3 86.1(3) 3_675 11_565 ? N2 Ni1 O3 172.9(3) . 11_565 ? O1 Ni1 O2 171.0(3) 3_675 . ? N2 Ni1 O2 92.2(3) . . ? O3 Ni1 O2 85.8(3) 11_565 . ? O1 Ni1 N1 94.5(3) 3_675 . ? N2 Ni1 N1 82.3(3) . . ? O3 Ni1 N1 90.9(3) 11_565 . ? O2 Ni1 N1 89.6(2) . . ? O1 Ni1 O1 92.1(3) 3_675 11_565 ? N2 Ni1 O1 83.0(3) . 11_565 ? O3 Ni1 O1 103.5(3) 11_565 11_565 ? O2 Ni1 O1 86.0(2) . 11_565 ? N1 Ni1 O1 164.5(3) . 11_565 ? N2 O1 Ni1 147.3(8) . 2_765 ? N2 O1 Ni1 99.2(6) . 12_655 ? Ni1 O1 Ni1 107.3(4) 2_765 12_655 ? C7 O2 Ni1 130.7(5) . . ? C7 O3 Ni1 134.6(6) . 12_655 ? C1 N1 C5 116.1(8) . . ? C1 N1 Ni1 130.0(7) . . ? C5 N1 Ni1 113.6(6) . . ? O1 N2 C6 108.0(9) . . ? O1 N2 Ni1 139.0(7) . . ? C6 N2 Ni1 112.2(7) . . ? N1 C1 C2 123.1(11) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.2(11) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 122.6(11) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 115.7(12) . . ? C3 C4 H4 122.2 . . ? C5 C4 H4 122.2 . . ? N1 C5 C4 123.3(9) . . ? N1 C5 C6 112.8(8) . . ? C4 C5 C6 123.6(10) . . ? N2 C6 C5 118.6(9) . . ? N2 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? O3 C7 O2 127.3(8) . . ? O3 C7 C8 116.3(9) . . ? O2 C7 C8 116.3(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 O1 Ni1 O2 C7 109(2) 3_675 . . . ? N2 Ni1 O2 C7 -51.7(8) . . . . ? O3 Ni1 O2 C7 135.1(8) 11_565 . . . ? N1 Ni1 O2 C7 -134.0(8) . . . . ? O1 Ni1 O2 C7 31.1(8) 11_565 . . . ? O1 Ni1 N1 C1 94.9(5) 3_675 . . . ? N2 Ni1 N1 C1 -169.3(5) . . . . ? O3 Ni1 N1 C1 8.7(5) 11_565 . . . ? O2 Ni1 N1 C1 -77.1(5) . . . . ? O1 Ni1 N1 C1 -150.4(9) 11_565 . . . ? O1 Ni1 N1 C5 -91.4(4) 3_675 . . . ? N2 Ni1 N1 C5 4.4(5) . . . . ? O3 Ni1 N1 C5 -177.5(5) 11_565 . . . ? O2 Ni1 N1 C5 96.7(5) . . . . ? O1 Ni1 N1 C5 23.4(11) 11_565 . . . ? Ni1 O1 N2 C6 -60.5(14) 2_765 . . . ? Ni1 O1 N2 C6 155.4(7) 12_655 . . . ? Ni1 O1 N2 Ni1 107.7(15) 2_765 . . . ? Ni1 O1 N2 Ni1 -36.4(10) 12_655 . . . ? O1 Ni1 N2 O1 -80.0(10) 3_675 . . . ? O3 Ni1 N2 O1 170(2) 11_565 . . . ? O2 Ni1 N2 O1 97.1(10) . . . . ? N1 Ni1 N2 O1 -173.6(11) . . . . ? O1 Ni1 N2 O1 11.4(10) 11_565 . . . ? O1 Ni1 N2 C6 87.9(7) 3_675 . . . ? O3 Ni1 N2 C6 -22(3) 11_565 . . . ? O2 Ni1 N2 C6 -95.1(7) . . . . ? N1 Ni1 N2 C6 -5.8(7) . . . . ? O1 Ni1 N2 C6 179.2(7) 11_565 . . . ? C5 N1 C1 C2 0.5(3) . . . . ? Ni1 N1 C1 C2 174.1(5) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? C1 N1 C5 C4 -1.1(7) . . . . ? Ni1 N1 C5 C4 -175.7(6) . . . . ? C1 N1 C5 C6 172.5(7) . . . . ? Ni1 N1 C5 C6 -2.2(8) . . . . ? C3 C4 C5 N1 0.8(9) . . . . ? C3 C4 C5 C6 -172.1(9) . . . . ? O1 N2 C6 C5 178.1(8) . . . . ? Ni1 N2 C6 C5 6.4(12) . . . . ? N1 C5 C6 N2 -2.8(12) . . . . ? C4 C5 C6 N2 170.7(8) . . . . ? Ni1 O3 C7 O2 -7.2(16) 12_655 . . . ? Ni1 O3 C7 C8 172.6(7) 12_655 . . . ? Ni1 O2 C7 O3 5.7(15) . . . . ? Ni1 O2 C7 C8 -174.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.395 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.166 # Attachment '4.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 668063' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Mn6 N12 O19' _chemical_formula_weight 1428.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.3210(15) _cell_length_b 14.3210(15) _cell_length_c 25.552(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4538.5(12) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3194 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.19 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 1.293 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7332 _exptl_absorpt_correction_T_max 0.8025 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7299 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.46 _reflns_number_total 1834 _reflns_number_gt 1570 _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^)+(0.1540P)^2^+30.5378P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1834 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2368 _refine_ls_wR_factor_gt 0.2216 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Mn1 Mn 0.14974(7) 0.43711(7) 0.13041(3) 0.0426(4) Uani 1 1 d . . . O1 O 0.1783(5) 0.6762(4) 0.1237(3) 0.0867(18) Uani 1 1 d . . . O2 O -0.0209(4) 0.3629(4) 0.1429(2) 0.0712(14) Uani 1 1 d . . . O3 O -0.0481(4) 0.4772(4) 0.1909(2) 0.0736(14) Uani 1 1 d . . . O4 O 1.0000 0.0000 0.0000 0.28(2) Uani 1 6 d S . . H1W H 0.9636 0.0146 0.0202 0.427 Uiso 0.33 1 d PR . . N1 N 0.1280(4) 0.4152(4) 0.04114(19) 0.0557(13) Uani 1 1 d . . . N2 N 0.1600(5) 0.5904(5) 0.1027(4) 0.090(3) Uani 1 1 d . . . C1 C 0.0839(13) 0.3318(10) 0.0137(4) 0.167(8) Uani 1 1 d . . . H1 H 0.0594 0.2668 0.0312 0.200 Uiso 1 1 calc R . . C2 C 0.0679(10) 0.3256(11) -0.0393(4) 0.126(5) Uani 1 1 d . . . H2 H 0.0393 0.2595 -0.0563 0.151 Uiso 1 1 calc R . . C3 C 0.0920(11) 0.4101(10) -0.0651(3) 0.109(4) Uani 1 1 d . . . H3 H 0.0925 0.4092 -0.1015 0.131 Uiso 1 1 calc R . . C4 C 0.1174(9) 0.5036(9) -0.0384(4) 0.094(3) Uani 1 1 d . . . H4 H 0.1227 0.5633 -0.0557 0.113 Uiso 1 1 calc R . . C5 C 0.1350(6) 0.5055(7) 0.0154(3) 0.0706(19) Uani 1 1 d . . . C6 C 0.1582(7) 0.6008(8) 0.0474(3) 0.080(2) Uani 1 1 d . . . H6 H 0.1710 0.6649 0.0319 0.096 Uiso 1 1 calc R . . C7 C -0.0776(5) 0.3895(5) 0.1686(2) 0.0532(15) Uani 1 1 d . . . C8 C -0.1959(6) 0.3085(7) 0.1716(4) 0.084(2) Uani 1 1 d . . . H8A H -0.2303 0.3340 0.1953 0.126 Uiso 1 1 calc R . . H8B H -0.2054 0.2409 0.1840 0.126 Uiso 1 1 calc R . . H8C H -0.2275 0.2987 0.1375 0.126 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 Mn1 0.0464(6) 0.0437(5) 0.0345(6) -0.0037(3) -0.0024(3) 0.0202(4) O1 0.071(3) 0.056(3) 0.131(5) -0.008(3) -0.017(3) 0.030(3) O2 0.050(2) 0.073(3) 0.077(3) -0.014(3) 0.001(2) 0.021(2) O3 0.050(3) 0.074(3) 0.090(4) -0.015(3) -0.004(2) 0.026(2) O4 0.24(3) 0.24(3) 0.38(7) 0.000 0.000 0.119(14) N1 0.061(3) 0.056(3) 0.035(3) -0.010(2) -0.010(2) 0.018(2) N2 0.064(4) 0.042(3) 0.164(8) -0.016(4) -0.045(4) 0.027(3) C1 0.220(16) 0.091(7) 0.056(5) -0.020(5) -0.006(7) -0.023(8) C2 0.137(10) 0.115(8) 0.058(5) -0.037(6) -0.017(6) 0.012(7) C3 0.147(10) 0.121(9) 0.040(4) -0.019(5) -0.013(5) 0.053(7) C4 0.112(7) 0.101(7) 0.063(5) 0.001(5) -0.003(5) 0.049(6) C5 0.059(4) 0.080(5) 0.062(4) 0.000(4) -0.003(3) 0.027(4) C6 0.083(5) 0.131(7) 0.030(3) 0.003(4) -0.002(3) 0.057(5) C7 0.043(3) 0.056(3) 0.054(4) 0.005(3) -0.005(2) 0.020(3) C8 0.048(4) 0.075(5) 0.116(7) 0.016(5) -0.005(4) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.140(5) 15 ? Mn1 O2 2.147(5) . ? Mn1 O1 2.188(5) 2_665 ? Mn1 N2 2.240(6) . ? Mn1 O1 2.241(7) 15 ? Mn1 N1 2.302(5) . ? O1 N2 1.243(8) . ? O1 Mn1 2.188(5) 3_565 ? O1 Mn1 2.241(7) 14_455 ? O2 C7 1.243(8) . ? O3 C7 1.245(8) . ? O3 Mn1 2.140(5) 14_455 ? O4 H1W 0.8306 . ? N1 C1 1.251(11) . ? N1 C5 1.408(10) . ? N2 C6 1.423(11) . ? C1 C2 1.368(15) . ? C1 H1 0.9300 . ? C2 C3 1.266(17) . ? C2 H2 0.9300 . ? C3 C4 1.379(14) . ? C3 H3 0.9300 . ? C4 C5 1.396(12) . ? C4 H4 0.9300 . ? C5 C6 1.478(12) . ? C6 H6 0.9300 . ? C7 C8 1.501(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 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 Mn1 O2 90.2(2) 15 . ? O3 Mn1 O1 85.2(2) 15 2_665 ? O2 Mn1 O1 174.3(2) . 2_665 ? O3 Mn1 N2 169.8(3) 15 . ? O2 Mn1 N2 91.9(2) . . ? O1 Mn1 N2 93.2(2) 2_665 . ? O3 Mn1 O1 106.6(2) 15 15 ? O2 Mn1 O1 86.5(2) . 15 ? O1 Mn1 O1 91.6(3) 2_665 15 ? N2 Mn1 O1 83.5(3) . 15 ? O3 Mn1 N1 94.0(2) 15 . ? O2 Mn1 N1 92.1(2) . . ? O1 Mn1 N1 91.6(2) 2_665 . ? N2 Mn1 N1 76.0(3) . . ? O1 Mn1 N1 159.4(2) 15 . ? N2 O1 Mn1 146.9(6) . 3_565 ? N2 O1 Mn1 102.2(6) . 14_455 ? Mn1 O1 Mn1 106.0(3) 3_565 14_455 ? C7 O2 Mn1 133.1(4) . . ? C7 O3 Mn1 134.7(4) . 14_455 ? C1 N1 C5 112.7(9) . . ? C1 N1 Mn1 130.9(7) . . ? C5 N1 Mn1 113.3(4) . . ? O1 N2 C6 109.3(7) . . ? O1 N2 Mn1 135.3(7) . . ? C6 N2 Mn1 114.9(6) . . ? N1 C1 C2 127.3(13) . . ? N1 C1 H1 116.4 . . ? C2 C1 H1 116.4 . . ? C3 C2 C1 119.7(11) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.0(9) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 117.6(9) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C4 C5 N1 120.9(8) . . ? C4 C5 C6 121.2(8) . . ? N1 C5 C6 118.0(6) . . ? N2 C6 C5 117.4(8) . . ? N2 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? O2 C7 O3 127.3(6) . . ? O2 C7 C8 116.6(7) . . ? O3 C7 C8 116.0(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 O3 Mn1 O2 C7 135.4(7) 15 . . . ? O1 Mn1 O2 C7 99(2) 2_665 . . . ? N2 Mn1 O2 C7 -54.6(7) . . . . ? O1 Mn1 O2 C7 28.7(6) 15 . . . ? N1 Mn1 O2 C7 -130.7(6) . . . . ? O3 Mn1 N1 C1 25.4(13) 15 . . . ? O2 Mn1 N1 C1 -65.0(13) . . . . ? O1 Mn1 N1 C1 110.7(13) 2_665 . . . ? N2 Mn1 N1 C1 -156.4(13) . . . . ? O1 Mn1 N1 C1 -150.6(13) 15 . . . ? O3 Mn1 N1 C5 -176.5(5) 15 . . . ? O2 Mn1 N1 C5 93.2(5) . . . . ? O1 Mn1 N1 C5 -91.1(5) 2_665 . . . ? N2 Mn1 N1 C5 1.7(5) . . . . ? O1 Mn1 N1 C5 7.6(9) 15 . . . ? Mn1 O1 N2 C6 -57.4(11) 3_565 . . . ? Mn1 O1 N2 C6 154.7(5) 14_455 . . . ? Mn1 O1 N2 Mn1 113.9(11) 3_565 . . . ? Mn1 O1 N2 Mn1 -34.0(8) 14_455 . . . ? O3 Mn1 N2 O1 -166.0(10) 15 . . . ? O2 Mn1 N2 O1 92.2(8) . . . . ? O1 Mn1 N2 O1 -85.3(8) 2_665 . . . ? O1 Mn1 N2 O1 5.9(7) 15 . . . ? N1 Mn1 N2 O1 -176.1(8) . . . . ? O3 Mn1 N2 C6 4.9(16) 15 . . . ? O2 Mn1 N2 C6 -96.9(6) . . . . ? O1 Mn1 N2 C6 85.6(6) 2_665 . . . ? O1 Mn1 N2 C6 176.8(6) 15 . . . ? N1 Mn1 N2 C6 -5.2(5) . . . . ? C5 N1 C1 C2 17(2) . . . . ? Mn1 N1 C1 C2 175.2(12) . . . . ? N1 C1 C2 C3 -5(3) . . . . ? C1 C2 C3 C4 -10(2) . . . . ? C2 C3 C4 C5 11.8(19) . . . . ? C3 C4 C5 N1 0.7(14) . . . . ? C3 C4 C5 C6 -177.4(10) . . . . ? C1 N1 C5 C4 -13.9(13) . . . . ? Mn1 N1 C5 C4 -176.2(7) . . . . ? C1 N1 C5 C6 164.2(11) . . . . ? Mn1 N1 C5 C6 1.9(8) . . . . ? O1 N2 C6 C5 -178.7(7) . . . . ? Mn1 N2 C6 C5 8.1(9) . . . . ? C4 C5 C6 N2 171.4(8) . . . . ? N1 C5 C6 N2 -6.7(11) . . . . ? Mn1 O2 C7 O3 8.3(11) . . . . ? Mn1 O2 C7 C8 -174.0(5) . . . . ? Mn1 O3 C7 O2 -4.3(12) 14_455 . . . ? Mn1 O3 C7 C8 178.0(5) 14_455 . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.463 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.125 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 735792' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H54 Cl6 N12 Ni6 O20' _chemical_formula_weight 2092.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.278(18) _cell_length_b 11.302(5) _cell_length_c 27.664(16) _cell_angle_alpha 90.00 _cell_angle_beta 112.460(13) _cell_angle_gamma 90.00 _cell_volume 8748(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5806 _exptl_absorpt_correction_T_max 0.8625 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20900 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8052 _reflns_number_gt 6016 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0783P)^2^+29.3775P] 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 8052 _refine_ls_number_parameters 572 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1956 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.56674(3) 0.29942(9) 0.54584(3) 0.0406(3) Uani 1 1 d . . . Ni2 Ni 0.59987(3) 0.57173(9) 0.52060(3) 0.0400(3) Uani 1 1 d . . . Ni3 Ni 0.50907(3) 0.58282(9) 0.40370(3) 0.0406(3) Uani 1 1 d . . . Cl1 Cl 0.62852(13) -0.0886(3) 0.83776(10) 0.1114(12) Uani 1 1 d . . . Cl2 Cl 0.85373(8) 0.1483(3) 0.58114(13) 0.0972(10) Uani 1 1 d . . . Cl3 Cl 0.74140(9) 0.8665(3) 0.32829(12) 0.0916(9) Uani 1 1 d . . . O1 O 0.46280(16) 0.3352(4) 0.52509(18) 0.0410(11) Uani 1 1 d . . . O2 O 0.55688(16) 0.4374(4) 0.58672(18) 0.0417(11) Uani 1 1 d . . . O3 O 0.56921(16) 0.4153(4) 0.48607(18) 0.0399(11) Uani 1 1 d . . . O4 O 0.57558(17) 0.1957(5) 0.61023(19) 0.0472(12) Uani 1 1 d . . . O5 O 0.52068(17) 0.2731(5) 0.63828(19) 0.0493(13) Uani 1 1 d . . . O6 O 0.63931(17) 0.3037(5) 0.5744(2) 0.0515(13) Uani 1 1 d . . . O7 O 0.66208(16) 0.4777(5) 0.55260(19) 0.0453(12) Uani 1 1 d . . . O8 O 0.62732(16) 0.6320(5) 0.4690(2) 0.0495(13) Uani 1 1 d . . . O9 O 0.56854(16) 0.6248(5) 0.38833(19) 0.0486(13) Uani 1 1 d . . . N1 N 0.5632(2) 0.1513(6) 0.5001(2) 0.0465(15) Uani 1 1 d . . . N2 N 0.49491(19) 0.2720(5) 0.5130(2) 0.0386(14) Uani 1 1 d . . . N3 N 0.63227(19) 0.7111(5) 0.5702(2) 0.0434(14) Uani 1 1 d . . . N4 N 0.58059(18) 0.5370(5) 0.5824(2) 0.0389(14) Uani 1 1 d . . . N5 N 0.48585(19) 0.4746(6) 0.3382(2) 0.0420(14) Uani 1 1 d . . . N6 N 0.53820(18) 0.4284(5) 0.4360(2) 0.0380(13) Uani 1 1 d . . . C1 C 0.5991(3) 0.0916(7) 0.4930(3) 0.0505(19) Uani 1 1 d . . . H1 H 0.6309 0.1123 0.5133 0.061 Uiso 1 1 calc R . . C2 C 0.5906(3) 0.0017(7) 0.4570(3) 0.055(2) Uani 1 1 d . . . H2 H 0.6163 -0.0370 0.4526 0.067 Uiso 1 1 calc R . . C3 C 0.5447(3) -0.0314(8) 0.4277(3) 0.058(2) Uani 1 1 d . . . H3 H 0.5384 -0.0929 0.4031 0.069 Uiso 1 1 calc R . . C4 C 0.5074(3) 0.0278(7) 0.4349(3) 0.0513(19) Uani 1 1 d . . . H4 H 0.4755 0.0062 0.4156 0.062 Uiso 1 1 calc R . . C5 C 0.5180(2) 0.1198(7) 0.4713(3) 0.0416(16) Uani 1 1 d . . . C6 C 0.4803(2) 0.1864(7) 0.4796(3) 0.0453(18) Uani 1 1 d . . . H6 H 0.4478 0.1685 0.4619 0.054 Uiso 1 1 calc R . . C7 C 0.6592(3) 0.7972(7) 0.5636(3) 0.0480(18) Uani 1 1 d . . . H7 H 0.6630 0.8021 0.5314 0.058 Uiso 1 1 calc R . . C8 C 0.6819(3) 0.8796(8) 0.6015(4) 0.067(2) Uani 1 1 d . . . H8 H 0.7011 0.9386 0.5954 0.080 Uiso 1 1 calc R . . C9 C 0.6763(3) 0.8747(9) 0.6484(4) 0.075(3) Uani 1 1 d . . . H9 H 0.6914 0.9304 0.6748 0.090 Uiso 1 1 calc R . . C10 C 0.6481(3) 0.7868(8) 0.6560(4) 0.065(2) Uani 1 1 d . . . H10 H 0.6435 0.7821 0.6877 0.078 Uiso 1 1 calc R . . C11 C 0.6263(2) 0.7044(7) 0.6159(3) 0.0460(18) Uani 1 1 d . . . C12 C 0.5978(3) 0.6063(7) 0.6218(3) 0.0473(18) Uani 1 1 d . . . H12 H 0.5923 0.5944 0.6526 0.057 Uiso 1 1 calc R . . C13 C 0.4563(3) 0.5015(9) 0.2890(3) 0.059(2) Uani 1 1 d . . . H13 H 0.4476 0.5810 0.2807 0.070 Uiso 1 1 calc R . . C14 C 0.4382(3) 0.4165(9) 0.2502(3) 0.065(2) Uani 1 1 d . . . H14 H 0.4182 0.4382 0.2160 0.078 Uiso 1 1 calc R . . C15 C 0.4503(4) 0.2991(10) 0.2628(4) 0.078(3) Uani 1 1 d . . . H15 H 0.4376 0.2394 0.2376 0.093 Uiso 1 1 calc R . . C16 C 0.4811(3) 0.2711(8) 0.3128(3) 0.061(2) Uani 1 1 d . . . H16 H 0.4905 0.1922 0.3217 0.073 Uiso 1 1 calc R . . C17 C 0.4983(3) 0.3602(7) 0.3498(3) 0.0450(18) Uani 1 1 d . . . C18 C 0.5314(3) 0.3385(7) 0.4041(3) 0.0433(17) Uani 1 1 d . . . H18 H 0.5466 0.2651 0.4150 0.052 Uiso 1 1 calc R . . C19 C 0.5552(3) 0.2041(7) 0.6419(3) 0.0456(18) Uani 1 1 d . . . C20 C 0.5722(3) 0.1271(7) 0.6903(3) 0.0503(19) Uani 1 1 d . . . C21 C 0.5484(3) 0.1259(8) 0.7242(3) 0.064(2) Uani 1 1 d . . . H21 H 0.5204 0.1706 0.7164 0.076 Uiso 1 1 calc R . . C22 C 0.5659(4) 0.0587(10) 0.7697(4) 0.077(3) Uani 1 1 d . . . H22 H 0.5497 0.0575 0.7928 0.093 Uiso 1 1 calc R . . C23 C 0.6068(4) -0.0057(9) 0.7805(3) 0.073(3) Uani 1 1 d . . . C24 C 0.6296(4) -0.0091(8) 0.7474(3) 0.072(3) Uani 1 1 d . . . H24 H 0.6569 -0.0566 0.7552 0.086 Uiso 1 1 calc R . . C25 C 0.6130(3) 0.0570(8) 0.7016(3) 0.063(2) Uani 1 1 d . . . H25 H 0.6290 0.0546 0.6785 0.075 Uiso 1 1 calc R . . C26 C 0.6685(2) 0.3715(8) 0.5656(3) 0.0472(19) Uani 1 1 d . . . C27 C 0.7160(2) 0.3167(7) 0.5719(3) 0.0464(19) Uani 1 1 d . . . C28 C 0.7292(3) 0.2082(8) 0.5956(4) 0.069(3) Uani 1 1 d . . . H28 H 0.7096 0.1690 0.6098 0.082 Uiso 1 1 calc R . . C29 C 0.7725(3) 0.1560(9) 0.5985(4) 0.078(3) Uani 1 1 d . . . H29 H 0.7816 0.0816 0.6143 0.094 Uiso 1 1 calc R . . C30 C 0.8011(3) 0.2133(9) 0.5783(4) 0.068(3) Uani 1 1 d . . . C31 C 0.7882(3) 0.3217(9) 0.5549(3) 0.059(2) Uani 1 1 d . . . H31 H 0.8081 0.3608 0.5410 0.070 Uiso 1 1 calc R . . C32 C 0.7449(2) 0.3745(8) 0.5516(3) 0.0502(19) Uani 1 1 d . . . H32 H 0.7358 0.4488 0.5356 0.060 Uiso 1 1 calc R . . C33 C 0.6102(3) 0.6457(7) 0.4200(3) 0.0462(18) Uani 1 1 d . . . C34 C 0.6445(3) 0.6968(7) 0.3971(3) 0.0439(17) Uani 1 1 d . . . C35 C 0.6884(2) 0.7408(8) 0.4289(3) 0.057(2) Uani 1 1 d . . . H35 H 0.6980 0.7344 0.4654 0.068 Uiso 1 1 calc R . . C36 C 0.7187(3) 0.7944(8) 0.4085(3) 0.056(2) Uani 1 1 d . . . H36 H 0.7479 0.8275 0.4305 0.067 Uiso 1 1 calc R . . C37 C 0.7045(3) 0.7973(8) 0.3556(4) 0.059(2) Uani 1 1 d . . . C38 C 0.6612(3) 0.7509(9) 0.3219(3) 0.066(2) Uani 1 1 d . . . H38 H 0.6525 0.7532 0.2855 0.079 Uiso 1 1 calc R . . C39 C 0.6309(3) 0.7008(8) 0.3436(3) 0.058(2) Uani 1 1 d . . . H39 H 0.6011 0.6697 0.3217 0.069 Uiso 1 1 calc R . . C40 C 0.1936(5) 0.0914(15) 0.2037(6) 0.134(6) Uani 1 1 d D . . C41 C 0.2019(7) 0.0120(19) 0.2509(6) 0.170(7) Uani 1 1 d . A . O10 O 0.1482(5) 0.1439(16) 0.1946(5) 0.125(6) Uani 0.688(16) 1 d PD A 1 O10' O 0.1789(13) 0.213(2) 0.1881(11) 0.125(6) Uani 0.312(16) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0255(4) 0.0568(6) 0.0382(5) 0.0033(4) 0.0108(4) 0.0081(4) Ni2 0.0270(4) 0.0563(6) 0.0359(5) 0.0029(4) 0.0112(4) 0.0075(4) Ni3 0.0285(5) 0.0574(6) 0.0358(5) 0.0044(4) 0.0124(4) 0.0082(4) Cl1 0.154(3) 0.095(2) 0.0477(14) 0.0235(13) -0.0033(16) 0.027(2) Cl2 0.0361(11) 0.106(2) 0.142(3) -0.0463(19) 0.0258(14) 0.0162(13) Cl3 0.0567(14) 0.125(2) 0.100(2) 0.0423(18) 0.0374(14) -0.0066(15) O1 0.033(2) 0.051(3) 0.041(3) 0.002(2) 0.017(2) 0.012(2) O2 0.031(2) 0.051(3) 0.045(3) -0.002(2) 0.017(2) 0.003(2) O3 0.029(2) 0.050(3) 0.039(3) 0.003(2) 0.012(2) 0.004(2) O4 0.042(3) 0.060(3) 0.042(3) 0.003(2) 0.018(2) 0.008(3) O5 0.035(3) 0.064(3) 0.050(3) 0.015(3) 0.017(2) 0.016(3) O6 0.030(3) 0.069(4) 0.055(3) 0.010(3) 0.017(2) 0.013(3) O7 0.028(2) 0.056(3) 0.051(3) 0.002(3) 0.014(2) 0.010(2) O8 0.031(2) 0.070(4) 0.050(3) 0.006(3) 0.018(2) 0.003(3) O9 0.030(3) 0.071(4) 0.044(3) 0.000(3) 0.014(2) 0.001(3) N1 0.034(3) 0.064(4) 0.041(3) 0.010(3) 0.013(3) 0.014(3) N2 0.030(3) 0.047(4) 0.040(3) 0.013(3) 0.015(3) 0.011(3) N3 0.026(3) 0.052(4) 0.048(4) 0.004(3) 0.011(3) 0.006(3) N4 0.022(3) 0.055(4) 0.038(3) -0.004(3) 0.010(2) 0.009(3) N5 0.031(3) 0.055(4) 0.042(3) 0.001(3) 0.016(3) 0.002(3) N6 0.027(3) 0.052(4) 0.037(3) 0.007(3) 0.015(2) 0.008(3) C1 0.042(4) 0.060(5) 0.054(5) 0.007(4) 0.023(4) 0.009(4) C2 0.047(5) 0.060(5) 0.068(6) -0.007(4) 0.032(4) 0.007(4) C3 0.051(5) 0.070(6) 0.060(5) -0.003(4) 0.030(4) 0.008(5) C4 0.040(4) 0.060(5) 0.058(5) -0.003(4) 0.022(4) -0.007(4) C5 0.036(4) 0.047(4) 0.041(4) 0.003(3) 0.014(3) 0.000(3) C6 0.030(4) 0.062(5) 0.043(4) -0.001(4) 0.013(3) 0.003(4) C7 0.035(4) 0.051(5) 0.056(5) 0.001(4) 0.016(3) 0.007(4) C8 0.043(5) 0.066(6) 0.091(7) -0.006(5) 0.026(5) -0.007(5) C9 0.056(5) 0.085(7) 0.090(7) -0.034(6) 0.035(5) -0.014(5) C10 0.057(5) 0.075(6) 0.073(6) -0.015(5) 0.036(5) -0.005(5) C11 0.033(4) 0.061(5) 0.043(4) -0.008(4) 0.013(3) 0.003(4) C12 0.039(4) 0.064(5) 0.046(4) -0.002(4) 0.023(3) 0.003(4) C13 0.052(5) 0.084(6) 0.037(4) 0.004(4) 0.014(4) 0.016(5) C14 0.060(5) 0.089(7) 0.040(5) 0.001(5) 0.012(4) 0.013(5) C15 0.081(7) 0.092(8) 0.048(5) -0.013(5) 0.011(5) -0.003(6) C16 0.070(6) 0.069(6) 0.043(5) -0.004(4) 0.020(4) -0.006(5) C17 0.040(4) 0.058(5) 0.043(4) -0.003(4) 0.023(3) -0.004(4) C18 0.043(4) 0.048(4) 0.042(4) 0.011(3) 0.020(3) 0.012(4) C19 0.042(4) 0.056(5) 0.035(4) 0.006(3) 0.011(3) 0.002(4) C20 0.040(4) 0.066(5) 0.037(4) 0.009(4) 0.007(3) 0.004(4) C21 0.054(5) 0.081(6) 0.052(5) 0.016(5) 0.014(4) 0.018(5) C22 0.079(7) 0.098(8) 0.051(5) 0.017(5) 0.021(5) 0.010(6) C23 0.092(7) 0.076(6) 0.032(5) 0.011(4) 0.004(5) 0.018(6) C24 0.079(6) 0.073(6) 0.046(5) 0.003(4) 0.004(5) 0.037(5) C25 0.060(5) 0.083(6) 0.038(4) 0.006(4) 0.011(4) 0.025(5) C26 0.023(3) 0.068(6) 0.046(4) -0.001(4) 0.009(3) 0.012(4) C27 0.020(3) 0.057(5) 0.058(5) -0.005(4) 0.010(3) 0.000(3) C28 0.032(4) 0.063(6) 0.105(8) 0.010(5) 0.020(5) 0.012(4) C29 0.033(4) 0.067(6) 0.121(9) 0.000(6) 0.016(5) 0.016(5) C30 0.022(4) 0.075(6) 0.094(7) -0.026(5) 0.007(4) 0.012(4) C31 0.031(4) 0.086(7) 0.060(5) -0.020(5) 0.020(4) 0.002(4) C32 0.031(4) 0.072(5) 0.045(4) -0.010(4) 0.012(3) 0.007(4) C33 0.043(4) 0.054(5) 0.045(5) 0.005(4) 0.021(4) 0.012(4) C34 0.040(4) 0.049(4) 0.048(4) 0.007(3) 0.023(3) 0.003(4) C35 0.028(4) 0.090(6) 0.051(5) 0.007(4) 0.013(3) 0.001(4) C36 0.034(4) 0.074(6) 0.056(5) -0.009(4) 0.012(4) -0.005(4) C37 0.033(4) 0.069(6) 0.075(6) 0.020(5) 0.021(4) 0.000(4) C38 0.063(5) 0.089(7) 0.049(5) 0.016(5) 0.025(4) -0.008(5) C39 0.049(5) 0.069(6) 0.059(5) -0.001(4) 0.026(4) -0.012(4) C40 0.138(13) 0.151(14) 0.104(11) 0.006(10) 0.037(10) 0.050(11) C41 0.183(17) 0.21(2) 0.094(12) -0.020(12) 0.026(11) 0.021(15) O10 0.110(11) 0.179(15) 0.078(7) -0.017(9) 0.025(7) 0.056(11) O10' 0.110(11) 0.179(15) 0.078(7) -0.017(9) 0.025(7) 0.056(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 Ni1 O2 2.015(5) . ? Ni1 O6 2.032(5) . ? Ni1 N2 2.035(6) . ? Ni1 O4 2.062(5) . ? Ni1 N1 2.077(7) . ? Ni1 O3 2.133(5) . ? Ni2 O8 2.025(5) . ? Ni2 N4 2.045(6) . ? Ni2 O7 2.046(5) . ? Ni2 O3 2.055(5) . ? Ni2 N3 2.072(6) . ? Ni2 O1 2.114(5) 5_666 ? Ni3 O5 2.003(5) 5_666 ? Ni3 N6 2.005(6) . ? Ni3 O1 2.045(5) 5_666 ? Ni3 O9 2.057(5) . ? Ni3 N5 2.073(6) . ? Ni3 O2 2.125(5) 5_666 ? Cl1 C23 1.738(9) . ? Cl2 C30 1.729(8) . ? Cl3 C37 1.754(8) . ? O1 N2 1.348(7) . ? O1 Ni3 2.045(5) 5_666 ? O1 Ni2 2.115(5) 5_666 ? O2 N4 1.364(7) . ? O2 Ni3 2.125(5) 5_666 ? O3 N6 1.351(7) . ? O4 C19 1.255(8) . ? O5 C19 1.276(9) . ? O5 Ni3 2.003(5) 5_666 ? O6 C26 1.262(9) . ? O7 C26 1.246(10) . ? O8 C33 1.260(8) . ? O9 C33 1.254(9) . ? N1 C5 1.342(9) . ? N1 C1 1.356(9) . ? N2 C6 1.294(9) . ? N3 C7 1.327(9) . ? N3 C11 1.347(9) . ? N4 C12 1.279(9) . ? N5 C17 1.351(10) . ? N5 C13 1.346(9) . ? N6 C18 1.311(9) . ? C1 C2 1.375(11) . ? C1 H1 0.9400 . ? C2 C3 1.366(11) . ? C2 H2 0.9400 . ? C3 C4 1.391(10) . ? C3 H3 0.9400 . ? C4 C5 1.397(11) . ? C4 H4 0.9400 . ? C5 C6 1.454(10) . ? C6 H6 0.9400 . ? C7 C8 1.374(12) . ? C7 H7 0.9400 . ? C8 C9 1.373(13) . ? C8 H8 0.9400 . ? C9 C10 1.378(13) . ? C9 H9 0.9400 . ? C10 C11 1.405(11) . ? C10 H10 0.9400 . ? C11 C12 1.452(11) . ? C12 H12 0.9400 . ? C13 C14 1.388(12) . ? C13 H13 0.9400 . ? C14 C15 1.385(13) . ? C14 H14 0.9400 . ? C15 C16 1.377(12) . ? C15 H15 0.9400 . ? C16 C17 1.388(11) . ? C16 H16 0.9400 . ? C17 C18 1.473(10) . ? C18 H18 0.9400 . ? C19 C20 1.512(10) . ? C20 C21 1.384(11) . ? C20 C25 1.397(11) . ? C21 C22 1.390(12) . ? C21 H21 0.9400 . ? C22 C23 1.368(13) . ? C22 H22 0.9400 . ? C23 C24 1.342(13) . ? C24 C25 1.388(12) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C26 C27 1.515(9) . ? C27 C32 1.372(11) . ? C27 C28 1.375(11) . ? C28 C29 1.411(11) . ? C28 H28 0.9400 . ? C29 C30 1.360(14) . ? C29 H29 0.9400 . ? C30 C31 1.370(13) . ? C31 C32 1.411(10) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.521(10) . ? C34 C35 1.377(10) . ? C34 C39 1.377(11) . ? C35 C36 1.387(11) . ? C35 H35 0.9400 . ? C36 C37 1.360(11) . ? C36 H36 0.9400 . ? C37 C38 1.389(12) . ? C38 C39 1.394(11) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? C40 O10 1.428(14) . ? C40 O10' 1.462(18) . ? C40 C41 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O6 97.7(2) . . ? O2 Ni1 N2 90.4(2) . . ? O6 Ni1 N2 171.8(2) . . ? O2 Ni1 O4 87.3(2) . . ? O6 Ni1 O4 85.0(2) . . ? N2 Ni1 O4 93.6(2) . . ? O2 Ni1 N1 169.1(2) . . ? O6 Ni1 N1 93.0(2) . . ? N2 Ni1 N1 78.9(2) . . ? O4 Ni1 N1 91.6(2) . . ? O2 Ni1 O3 90.94(19) . . ? O6 Ni1 O3 86.20(19) . . ? N2 Ni1 O3 95.47(19) . . ? O4 Ni1 O3 170.77(19) . . ? N1 Ni1 O3 91.8(2) . . ? O8 Ni2 N4 168.4(2) . . ? O8 Ni2 O7 85.5(2) . . ? N4 Ni2 O7 92.8(2) . . ? O8 Ni2 O3 101.3(2) . . ? N4 Ni2 O3 90.1(2) . . ? O7 Ni2 O3 86.1(2) . . ? O8 Ni2 N3 89.6(2) . . ? N4 Ni2 N3 78.9(2) . . ? O7 Ni2 N3 89.1(2) . . ? O3 Ni2 N3 167.7(2) . . ? O8 Ni2 O1 85.84(19) . 5_666 ? N4 Ni2 O1 96.75(19) . 5_666 ? O7 Ni2 O1 169.87(19) . 5_666 ? O3 Ni2 O1 90.41(19) . 5_666 ? N3 Ni2 O1 96.2(2) . 5_666 ? O5 Ni3 N6 171.8(2) 5_666 . ? O5 Ni3 O1 96.9(2) 5_666 5_666 ? N6 Ni3 O1 90.8(2) . 5_666 ? O5 Ni3 O9 85.9(2) 5_666 . ? N6 Ni3 O9 91.3(2) . . ? O1 Ni3 O9 91.1(2) 5_666 . ? O5 Ni3 N5 92.6(2) 5_666 . ? N6 Ni3 N5 79.7(2) . . ? O1 Ni3 N5 170.5(2) 5_666 . ? O9 Ni3 N5 89.3(2) . . ? O5 Ni3 O2 85.65(19) 5_666 5_666 ? N6 Ni3 O2 97.2(2) . 5_666 ? O1 Ni3 O2 89.66(18) 5_666 5_666 ? O9 Ni3 O2 171.5(2) . 5_666 ? N5 Ni3 O2 91.4(2) . 5_666 ? N2 O1 Ni3 113.9(4) . 5_666 ? N2 O1 Ni2 133.1(4) . 5_666 ? Ni3 O1 Ni2 107.4(2) 5_666 5_666 ? N4 O2 Ni1 113.2(4) . . ? N4 O2 Ni3 130.6(4) . 5_666 ? Ni1 O2 Ni3 109.5(2) . 5_666 ? N6 O3 Ni2 113.3(4) . . ? N6 O3 Ni1 130.2(4) . . ? Ni2 O3 Ni1 108.1(2) . . ? C19 O4 Ni1 128.7(5) . . ? C19 O5 Ni3 135.7(5) . 5_666 ? C26 O6 Ni1 132.2(5) . . ? C26 O7 Ni2 129.8(5) . . ? C33 O8 Ni2 133.5(5) . . ? C33 O9 Ni3 128.7(5) . . ? C5 N1 C1 118.3(7) . . ? C5 N1 Ni1 112.2(5) . . ? C1 N1 Ni1 129.2(5) . . ? C6 N2 O1 119.5(6) . . ? C6 N2 Ni1 116.6(5) . . ? O1 N2 Ni1 123.9(4) . . ? C7 N3 C11 118.7(7) . . ? C7 N3 Ni2 128.9(5) . . ? C11 N3 Ni2 112.3(5) . . ? C12 N4 O2 119.2(6) . . ? C12 N4 Ni2 116.1(5) . . ? O2 N4 Ni2 124.0(4) . . ? C17 N5 C13 118.2(7) . . ? C17 N5 Ni3 112.8(5) . . ? C13 N5 Ni3 128.5(6) . . ? C18 N6 O3 118.3(6) . . ? C18 N6 Ni3 116.4(5) . . ? O3 N6 Ni3 124.6(4) . . ? N1 C1 C2 122.2(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 119.9(7) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.7(8) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.1(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.7(7) . . ? N1 C5 C6 116.9(7) . . ? C4 C5 C6 121.3(7) . . ? N2 C6 C5 115.2(6) . . ? N2 C6 H6 122.4 . . ? C5 C6 H6 122.4 . . ? N3 C7 C8 123.2(8) . . ? N3 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C9 C8 C7 119.1(9) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.8(9) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 119.2(8) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N3 C11 C10 120.9(7) . . ? N3 C11 C12 116.5(7) . . ? C10 C11 C12 122.6(7) . . ? N4 C12 C11 116.0(7) . . ? N4 C12 H12 122.0 . . ? C11 C12 H12 122.0 . . ? N5 C13 C14 122.7(8) . . ? N5 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 118.7(8) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 119.0(9) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 119.5(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N5 C17 C16 121.9(7) . . ? N5 C17 C18 114.9(7) . . ? C16 C17 C18 123.2(8) . . ? N6 C18 C17 115.4(7) . . ? N6 C18 H18 122.3 . . ? C17 C18 H18 122.3 . . ? O4 C19 O5 126.7(7) . . ? O4 C19 C20 118.8(7) . . ? O5 C19 C20 114.5(6) . . ? C21 C20 C25 119.1(7) . . ? C21 C20 C19 121.0(7) . . ? C25 C20 C19 119.9(7) . . ? C20 C21 C22 120.3(8) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.1(9) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 121.7(8) . . ? C24 C23 Cl1 119.5(8) . . ? C22 C23 Cl1 118.8(8) . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 119.4(8) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? O7 C26 O6 126.8(6) . . ? O7 C26 C27 117.6(7) . . ? O6 C26 C27 115.6(7) . . ? C32 C27 C28 120.3(7) . . ? C32 C27 C26 118.9(7) . . ? C28 C27 C26 120.8(7) . . ? C27 C28 C29 119.7(9) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.0(9) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.5(7) . . ? C29 C30 Cl2 119.9(8) . . ? C31 C30 Cl2 119.6(8) . . ? C30 C31 C32 120.0(8) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 119.5(8) . . ? C27 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? O9 C33 O8 128.2(7) . . ? O9 C33 C34 116.3(7) . . ? O8 C33 C34 115.4(7) . . ? C35 C34 C39 119.6(7) . . ? C35 C34 C33 121.0(7) . . ? C39 C34 C33 119.3(7) . . ? C34 C35 C36 121.6(8) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 117.6(7) . . ? C37 C36 H36 121.2 . . ? C35 C36 H36 121.2 . . ? C36 C37 C38 122.8(7) . . ? C36 C37 Cl3 118.9(7) . . ? C38 C37 Cl3 118.3(7) . . ? C37 C38 C39 118.2(8) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C34 C39 C38 120.1(8) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? O10 C40 O10' 52.6(14) . . ? O10 C40 C41 103.1(15) . . ? O10' C40 C41 137.7(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 O6 Ni1 O2 N4 51.6(4) . . . . ? N2 Ni1 O2 N4 -130.1(4) . . . . ? O4 Ni1 O2 N4 136.3(4) . . . . ? N1 Ni1 O2 N4 -139.1(11) . . . . ? O3 Ni1 O2 N4 -34.7(4) . . . . ? O6 Ni1 O2 Ni3 -153.8(2) . . . 5_666 ? N2 Ni1 O2 Ni3 24.5(2) . . . 5_666 ? O4 Ni1 O2 Ni3 -69.1(2) . . . 5_666 ? N1 Ni1 O2 Ni3 15.5(13) . . . 5_666 ? O3 Ni1 O2 Ni3 119.9(2) . . . 5_666 ? O8 Ni2 O3 N6 -54.3(4) . . . . ? N4 Ni2 O3 N6 128.2(4) . . . . ? O7 Ni2 O3 N6 -139.0(4) . . . . ? N3 Ni2 O3 N6 153.9(8) . . . . ? O1 Ni2 O3 N6 31.5(4) 5_666 . . . ? O8 Ni2 O3 Ni1 154.0(2) . . . . ? N4 Ni2 O3 Ni1 -23.4(2) . . . . ? O7 Ni2 O3 Ni1 69.4(2) . . . . ? N3 Ni2 O3 Ni1 2.3(10) . . . . ? O1 Ni2 O3 Ni1 -120.1(2) 5_666 . . . ? O2 Ni1 O3 N6 -111.9(5) . . . . ? O6 Ni1 O3 N6 150.4(5) . . . . ? N2 Ni1 O3 N6 -21.5(5) . . . . ? O4 Ni1 O3 N6 169.0(10) . . . . ? N1 Ni1 O3 N6 57.5(5) . . . . ? O2 Ni1 O3 Ni2 33.3(2) . . . . ? O6 Ni1 O3 Ni2 -64.4(2) . . . . ? N2 Ni1 O3 Ni2 123.7(2) . . . . ? O4 Ni1 O3 Ni2 -45.8(13) . . . . ? N1 Ni1 O3 Ni2 -157.3(2) . . . . ? O2 Ni1 O4 C19 34.9(6) . . . . ? O6 Ni1 O4 C19 132.9(6) . . . . ? N2 Ni1 O4 C19 -55.3(6) . . . . ? N1 Ni1 O4 C19 -134.3(6) . . . . ? O3 Ni1 O4 C19 114.2(12) . . . . ? O2 Ni1 O6 C26 -75.2(7) . . . . ? N2 Ni1 O6 C26 117.3(15) . . . . ? O4 Ni1 O6 C26 -161.8(7) . . . . ? N1 Ni1 O6 C26 106.8(7) . . . . ? O3 Ni1 O6 C26 15.3(7) . . . . ? O8 Ni2 O7 C26 -132.4(6) . . . . ? N4 Ni2 O7 C26 59.1(6) . . . . ? O3 Ni2 O7 C26 -30.8(6) . . . . ? N3 Ni2 O7 C26 137.9(6) . . . . ? O1 Ni2 O7 C26 -100.8(13) 5_666 . . . ? N4 Ni2 O8 C33 -142.8(10) . . . . ? O7 Ni2 O8 C33 135.3(7) . . . . ? O3 Ni2 O8 C33 50.2(7) . . . . ? N3 Ni2 O8 C33 -135.6(7) . . . . ? O1 Ni2 O8 C33 -39.4(7) 5_666 . . . ? O5 Ni3 O9 C33 121.5(7) 5_666 . . . ? N6 Ni3 O9 C33 -66.1(7) . . . . ? O1 Ni3 O9 C33 24.7(7) 5_666 . . . ? N5 Ni3 O9 C33 -145.8(7) . . . . ? O2 Ni3 O9 C33 119.8(13) 5_666 . . . ? O2 Ni1 N1 C5 13.1(15) . . . . ? O6 Ni1 N1 C5 -177.6(5) . . . . ? N2 Ni1 N1 C5 3.9(5) . . . . ? O4 Ni1 N1 C5 97.3(5) . . . . ? O3 Ni1 N1 C5 -91.3(5) . . . . ? O2 Ni1 N1 C1 -172.6(10) . . . . ? O6 Ni1 N1 C1 -3.2(6) . . . . ? N2 Ni1 N1 C1 178.3(7) . . . . ? O4 Ni1 N1 C1 -88.4(6) . . . . ? O3 Ni1 N1 C1 83.0(6) . . . . ? Ni3 O1 N2 C6 156.6(5) 5_666 . . . ? Ni2 O1 N2 C6 -53.8(8) 5_666 . . . ? Ni3 O1 N2 Ni1 -21.6(6) 5_666 . . . ? Ni2 O1 N2 Ni1 127.9(4) 5_666 . . . ? O2 Ni1 N2 C6 178.8(5) . . . . ? O6 Ni1 N2 C6 -13.6(18) . . . . ? O4 Ni1 N2 C6 -93.9(5) . . . . ? N1 Ni1 N2 C6 -3.0(5) . . . . ? O3 Ni1 N2 C6 87.8(5) . . . . ? O2 Ni1 N2 O1 -2.9(5) . . . . ? O6 Ni1 N2 O1 164.8(13) . . . . ? O4 Ni1 N2 O1 84.4(5) . . . . ? N1 Ni1 N2 O1 175.4(5) . . . . ? O3 Ni1 N2 O1 -93.9(5) . . . . ? O8 Ni2 N3 C7 -0.1(6) . . . . ? N4 Ni2 N3 C7 178.4(6) . . . . ? O7 Ni2 N3 C7 85.4(6) . . . . ? O3 Ni2 N3 C7 152.2(8) . . . . ? O1 Ni2 N3 C7 -85.9(6) 5_666 . . . ? O8 Ni2 N3 C11 -175.6(5) . . . . ? N4 Ni2 N3 C11 2.9(5) . . . . ? O7 Ni2 N3 C11 -90.1(5) . . . . ? O3 Ni2 N3 C11 -23.3(12) . . . . ? O1 Ni2 N3 C11 98.6(5) 5_666 . . . ? Ni1 O2 N4 C12 -145.3(5) . . . . ? Ni3 O2 N4 C12 66.8(7) 5_666 . . . ? Ni1 O2 N4 Ni2 24.8(5) . . . . ? Ni3 O2 N4 Ni2 -123.0(4) 5_666 . . . ? O8 Ni2 N4 C12 3.7(13) . . . . ? O7 Ni2 N4 C12 84.9(5) . . . . ? O3 Ni2 N4 C12 171.0(5) . . . . ? N3 Ni2 N4 C12 -3.6(5) . . . . ? O1 Ni2 N4 C12 -98.6(5) 5_666 . . . ? O8 Ni2 N4 O2 -166.7(9) . . . . ? O7 Ni2 N4 O2 -85.5(5) . . . . ? O3 Ni2 N4 O2 0.6(4) . . . . ? N3 Ni2 N4 O2 -174.0(5) . . . . ? O1 Ni2 N4 O2 91.0(4) 5_666 . . . ? O5 Ni3 N5 C17 -178.7(5) 5_666 . . . ? N6 Ni3 N5 C17 4.1(4) . . . . ? O1 Ni3 N5 C17 3.2(15) 5_666 . . . ? O9 Ni3 N5 C17 95.5(5) . . . . ? O2 Ni3 N5 C17 -93.0(5) 5_666 . . . ? O5 Ni3 N5 C13 -7.3(6) 5_666 . . . ? N6 Ni3 N5 C13 175.4(7) . . . . ? O1 Ni3 N5 C13 174.6(10) 5_666 . . . ? O9 Ni3 N5 C13 -93.1(6) . . . . ? O2 Ni3 N5 C13 78.4(6) 5_666 . . . ? Ni2 O3 N6 C18 152.9(5) . . . . ? Ni1 O3 N6 C18 -63.3(7) . . . . ? Ni2 O3 N6 Ni3 -17.3(6) . . . . ? Ni1 O3 N6 Ni3 126.5(4) . . . . ? O5 Ni3 N6 C18 -17.7(18) 5_666 . . . ? O1 Ni3 N6 C18 -178.2(5) 5_666 . . . ? O9 Ni3 N6 C18 -87.1(5) . . . . ? N5 Ni3 N6 C18 1.9(5) . . . . ? O2 Ni3 N6 C18 92.0(5) 5_666 . . . ? O5 Ni3 N6 O3 152.7(13) 5_666 . . . ? O1 Ni3 N6 O3 -7.8(5) 5_666 . . . ? O9 Ni3 N6 O3 83.3(5) . . . . ? N5 Ni3 N6 O3 172.3(5) . . . . ? O2 Ni3 N6 O3 -97.6(5) 5_666 . . . ? C5 N1 C1 C2 0.9(11) . . . . ? Ni1 N1 C1 C2 -173.2(6) . . . . ? N1 C1 C2 C3 -1.1(13) . . . . ? C1 C2 C3 C4 0.2(13) . . . . ? C2 C3 C4 C5 0.8(12) . . . . ? C1 N1 C5 C4 0.3(11) . . . . ? Ni1 N1 C5 C4 175.3(6) . . . . ? C1 N1 C5 C6 -179.5(6) . . . . ? Ni1 N1 C5 C6 -4.4(8) . . . . ? C3 C4 C5 N1 -1.1(12) . . . . ? C3 C4 C5 C6 178.6(7) . . . . ? O1 N2 C6 C5 -176.9(5) . . . . ? Ni1 N2 C6 C5 1.5(8) . . . . ? N1 C5 C6 N2 2.1(10) . . . . ? C4 C5 C6 N2 -177.6(7) . . . . ? C11 N3 C7 C8 0.7(11) . . . . ? Ni2 N3 C7 C8 -174.6(6) . . . . ? N3 C7 C8 C9 -0.9(13) . . . . ? C7 C8 C9 C10 0.2(14) . . . . ? C8 C9 C10 C11 0.6(14) . . . . ? C7 N3 C11 C10 0.1(10) . . . . ? Ni2 N3 C11 C10 176.1(6) . . . . ? C7 N3 C11 C12 -178.1(6) . . . . ? Ni2 N3 C11 C12 -2.0(8) . . . . ? C9 C10 C11 N3 -0.8(12) . . . . ? C9 C10 C11 C12 177.3(8) . . . . ? O2 N4 C12 C11 174.5(6) . . . . ? Ni2 N4 C12 C11 3.6(8) . . . . ? N3 C11 C12 N4 -1.0(10) . . . . ? C10 C11 C12 N4 -179.1(7) . . . . ? C17 N5 C13 C14 0.3(11) . . . . ? Ni3 N5 C13 C14 -170.7(6) . . . . ? N5 C13 C14 C15 1.3(14) . . . . ? C13 C14 C15 C16 -2.4(15) . . . . ? C14 C15 C16 C17 2.0(14) . . . . ? C13 N5 C17 C16 -0.7(10) . . . . ? Ni3 N5 C17 C16 171.7(6) . . . . ? C13 N5 C17 C18 178.8(6) . . . . ? Ni3 N5 C17 C18 -8.8(7) . . . . ? C15 C16 C17 N5 -0.5(12) . . . . ? C15 C16 C17 C18 -179.9(8) . . . . ? O3 N6 C18 C17 -178.2(5) . . . . ? Ni3 N6 C18 C17 -7.2(8) . . . . ? N5 C17 C18 N6 10.7(9) . . . . ? C16 C17 C18 N6 -169.7(7) . . . . ? Ni1 O4 C19 O5 7.2(12) . . . . ? Ni1 O4 C19 C20 -172.2(5) . . . . ? Ni3 O5 C19 O4 -15.6(13) 5_666 . . . ? Ni3 O5 C19 C20 163.8(5) 5_666 . . . ? O4 C19 C20 C21 -174.6(8) . . . . ? O5 C19 C20 C21 6.0(11) . . . . ? O4 C19 C20 C25 6.2(12) . . . . ? O5 C19 C20 C25 -173.3(8) . . . . ? C25 C20 C21 C22 2.2(14) . . . . ? C19 C20 C21 C22 -177.1(8) . . . . ? C20 C21 C22 C23 0.1(15) . . . . ? C21 C22 C23 C24 -2.5(16) . . . . ? C21 C22 C23 Cl1 179.6(8) . . . . ? C22 C23 C24 C25 2.5(16) . . . . ? Cl1 C23 C24 C25 -179.6(8) . . . . ? C23 C24 C25 C20 -0.1(15) . . . . ? C21 C20 C25 C24 -2.2(14) . . . . ? C19 C20 C25 C24 177.0(8) . . . . ? Ni2 O7 C26 O6 -19.5(12) . . . . ? Ni2 O7 C26 C27 160.9(5) . . . . ? Ni1 O6 C26 O7 29.4(12) . . . . ? Ni1 O6 C26 C27 -150.9(5) . . . . ? O7 C26 C27 C32 -15.5(11) . . . . ? O6 C26 C27 C32 164.8(7) . . . . ? O7 C26 C27 C28 167.4(8) . . . . ? O6 C26 C27 C28 -12.2(11) . . . . ? C32 C27 C28 C29 -0.5(14) . . . . ? C26 C27 C28 C29 176.5(8) . . . . ? C27 C28 C29 C30 0.5(15) . . . . ? C28 C29 C30 C31 -0.2(15) . . . . ? C28 C29 C30 Cl2 -179.2(8) . . . . ? C29 C30 C31 C32 -0.1(13) . . . . ? Cl2 C30 C31 C32 178.9(6) . . . . ? C28 C27 C32 C31 0.3(12) . . . . ? C26 C27 C32 C31 -176.8(7) . . . . ? C30 C31 C32 C27 0.0(12) . . . . ? Ni3 O9 C33 O8 9.6(12) . . . . ? Ni3 O9 C33 C34 -168.8(5) . . . . ? Ni2 O8 C33 O9 0.6(13) . . . . ? Ni2 O8 C33 C34 179.1(5) . . . . ? O9 C33 C34 C35 169.3(8) . . . . ? O8 C33 C34 C35 -9.3(11) . . . . ? O9 C33 C34 C39 -9.5(11) . . . . ? O8 C33 C34 C39 171.8(7) . . . . ? C39 C34 C35 C36 3.0(13) . . . . ? C33 C34 C35 C36 -175.9(8) . . . . ? C34 C35 C36 C37 -2.9(13) . . . . ? C35 C36 C37 C38 0.9(14) . . . . ? C35 C36 C37 Cl3 179.0(7) . . . . ? C36 C37 C38 C39 0.9(15) . . . . ? Cl3 C37 C38 C39 -177.1(7) . . . . ? C35 C34 C39 C38 -1.0(13) . . . . ? C33 C34 C39 C38 177.9(8) . . . . ? C37 C38 C39 C34 -0.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.586 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.104 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 737330' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H60 N12 Ni6 O20' _chemical_formula_weight 1885.68 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 ? _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.596(4) _cell_length_b 11.2960(11) _cell_length_c 26.483(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.235(3) _cell_angle_gamma 90.00 _cell_volume 8138.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 25.50 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5215 _exptl_absorpt_correction_T_max 0.9315 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20434 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7542 _reflns_number_gt 5534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0371P)^2^+25.7679P] 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 7542 _refine_ls_number_parameters 539 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 0.17349(3) 0.16413(7) 0.03133(3) 0.0382(2) Uani 1 1 d . . . Ni2 Ni 0.28856(3) 0.04915(7) 0.08234(3) 0.0370(2) Uani 1 1 d . . . Ni3 Ni 0.33941(3) 0.31838(7) 0.10183(3) 0.0383(2) Uani 1 1 d . . . O1 O 0.16890(15) 0.3349(3) -0.05888(17) 0.0380(10) Uani 1 1 d . . . O2 O 0.19275(15) 0.0818(4) -0.02393(17) 0.0399(11) Uani 1 1 d . . . O3 O 0.24902(15) 0.1899(4) 0.08827(18) 0.0398(11) Uani 1 1 d . . . O4 O 0.10194(16) 0.1122(4) -0.0179(2) 0.0510(12) Uani 1 1 d . . . O5 O 0.09623(16) 0.1337(4) -0.10489(19) 0.0493(12) Uani 1 1 d . . . O6 O 0.17710(16) 0.0234(4) 0.08006(18) 0.0437(11) Uani 1 1 d . . . O7 O 0.25395(16) -0.0523(4) 0.11777(18) 0.0423(11) Uani 1 1 d . . . O8 O 0.34568(16) 0.0508(4) 0.16126(18) 0.0435(11) Uani 1 1 d . . . O9 O 0.38103(16) 0.2305(4) 0.17654(17) 0.0443(11) Uani 1 1 d . . . N1 N 0.15020(18) 0.2753(5) 0.0774(2) 0.0402(13) Uani 1 1 d . . . N2 N 0.16434(18) 0.3208(5) -0.0109(2) 0.0382(13) Uani 1 1 d . . . N3 N 0.31690(19) -0.0985(4) 0.0598(2) 0.0383(13) Uani 1 1 d . . . N4 N 0.23579(19) 0.0220(5) 0.0017(2) 0.0384(13) Uani 1 1 d . . . N5 N 0.3386(2) 0.4633(5) 0.1486(2) 0.0436(14) Uani 1 1 d . . . N6 N 0.27647(19) 0.2891(5) 0.1071(2) 0.0390(13) Uani 1 1 d . . . C1 C 0.1446(2) 0.2493(7) 0.1238(3) 0.0489(18) Uani 1 1 d . . . H1 H 0.1496 0.1708 0.1370 0.059 Uiso 1 1 calc R . . C2 C 0.1322(3) 0.3321(7) 0.1523(3) 0.060(2) Uani 1 1 d . . . H2 H 0.1279 0.3106 0.1840 0.072 Uiso 1 1 calc R . . C3 C 0.1261(3) 0.4480(7) 0.1339(4) 0.072(2) Uani 1 1 d . . . H3 H 0.1180 0.5066 0.1534 0.086 Uiso 1 1 calc R . . C4 C 0.1320(3) 0.4777(7) 0.0866(3) 0.060(2) Uani 1 1 d . . . H4 H 0.1282 0.5563 0.0736 0.073 Uiso 1 1 calc R . . C5 C 0.1435(2) 0.3879(6) 0.0588(3) 0.0445(17) Uani 1 1 d . . . C6 C 0.1490(2) 0.4083(6) 0.0079(3) 0.0462(17) Uani 1 1 d . . . H6 H 0.1416 0.4821 -0.0105 0.055 Uiso 1 1 calc R . . C7 C 0.3596(3) -0.1533(6) 0.0890(3) 0.0490(18) Uani 1 1 d . . . H7 H 0.3796 -0.1301 0.1268 0.059 Uiso 1 1 calc R . . C8 C 0.3761(3) -0.2432(7) 0.0662(3) 0.0543(19) Uani 1 1 d . . . H8 H 0.4069 -0.2786 0.0881 0.065 Uiso 1 1 calc R . . C9 C 0.3473(3) -0.2795(7) 0.0121(3) 0.058(2) Uani 1 1 d . . . H9 H 0.3574 -0.3416 -0.0038 0.069 Uiso 1 1 calc R . . C10 C 0.3026(3) -0.2228(6) -0.0193(3) 0.0491(18) Uani 1 1 d . . . H10A H 0.2823 -0.2457 -0.0570 0.059 Uiso 1 1 calc R . . C11 C 0.2882(2) -0.1323(6) 0.0051(3) 0.0403(16) Uani 1 1 d . . . C12 C 0.2426(2) -0.0660(6) -0.0247(3) 0.0437(17) Uani 1 1 d . . . H12 H 0.2191 -0.0868 -0.0617 0.052 Uiso 1 1 calc R . . C13 C 0.3717(3) 0.5499(6) 0.1685(3) 0.057(2) Uani 1 1 d . . . H13 H 0.3996 0.5460 0.1622 0.068 Uiso 1 1 calc R . . C14 C 0.3665(3) 0.6457(7) 0.1980(4) 0.074(3) Uani 1 1 d . . . H14 H 0.3898 0.7070 0.2109 0.088 Uiso 1 1 calc R . . C15 C 0.3250(4) 0.6487(8) 0.2082(5) 0.095(3) Uani 1 1 d . . . H15 H 0.3206 0.7115 0.2287 0.114 Uiso 1 1 calc R . . C16 C 0.2915(3) 0.5585(7) 0.1878(4) 0.074(3) Uani 1 1 d . . . H16 H 0.2635 0.5589 0.1938 0.089 Uiso 1 1 calc R . . C17 C 0.2992(3) 0.4666(6) 0.1579(3) 0.0448(17) Uani 1 1 d . . . C18 C 0.2652(3) 0.3665(6) 0.1350(3) 0.0473(18) Uani 1 1 d . . . H18 H 0.2369 0.3592 0.1402 0.057 Uiso 1 1 calc R . . C19 C 0.0802(2) 0.1016(6) -0.0714(3) 0.0424(16) Uani 1 1 d . . . C20 C 0.0297(2) 0.0496(6) -0.0984(3) 0.0439(17) Uani 1 1 d . . . C21 C 0.0015(3) 0.0581(7) -0.1563(3) 0.059(2) Uani 1 1 d . . . H21 H 0.0147 0.0930 -0.1784 0.071 Uiso 1 1 calc R . . C22 C -0.0466(3) 0.0154(9) -0.1825(4) 0.086(3) Uani 1 1 d . . . H22 H -0.0656 0.0237 -0.2219 0.103 Uiso 1 1 calc R . . C23 C -0.0660(3) -0.0381(9) -0.1514(4) 0.085(3) Uani 1 1 d . . . H23 H -0.0982 -0.0682 -0.1693 0.102 Uiso 1 1 calc R . . C24 C -0.0382(3) -0.0477(9) -0.0937(4) 0.081(3) Uani 1 1 d . . . H24 H -0.0517 -0.0837 -0.0719 0.097 Uiso 1 1 calc R . . C25 C 0.0098(3) -0.0045(7) -0.0670(3) 0.062(2) Uani 1 1 d . . . H25 H 0.0286 -0.0124 -0.0275 0.074 Uiso 1 1 calc R . . C26 C 0.2109(3) -0.0416(6) 0.1136(3) 0.0419(16) Uani 1 1 d . . . C27 C 0.2000(2) -0.1189(6) 0.1529(3) 0.0400(16) Uani 1 1 d . . . C28 C 0.1524(3) -0.1501(7) 0.1386(3) 0.066(2) Uani 1 1 d . . . H28 H 0.1265 -0.1226 0.1046 0.079 Uiso 1 1 calc R . . C29 C 0.1426(3) -0.2236(8) 0.1754(4) 0.082(3) Uani 1 1 d . . . H29 H 0.1100 -0.2450 0.1656 0.098 Uiso 1 1 calc R . . C30 C 0.1794(4) -0.2635(8) 0.2244(4) 0.072(3) Uani 1 1 d . . . H30 H 0.1725 -0.3124 0.2487 0.086 Uiso 1 1 calc R . . C31 C 0.2272(3) -0.2316(7) 0.2386(3) 0.066(2) Uani 1 1 d . . . H31 H 0.2531 -0.2595 0.2725 0.080 Uiso 1 1 calc R . . C32 C 0.2372(3) -0.1591(7) 0.2032(3) 0.059(2) Uani 1 1 d . . . H32 H 0.2699 -0.1368 0.2137 0.071 Uiso 1 1 calc R . . C33 C 0.3791(2) 0.1244(6) 0.1892(3) 0.0416(16) Uani 1 1 d . . . C34 C 0.4207(2) 0.0802(6) 0.2435(3) 0.0415(16) Uani 1 1 d . . . C35 C 0.4234(3) -0.0364(7) 0.2594(3) 0.057(2) Uani 1 1 d . . . H35 H 0.3977 -0.0883 0.2371 0.069 Uiso 1 1 calc R . . C36 C 0.4625(3) -0.0786(8) 0.3070(4) 0.072(2) Uani 1 1 d . . . H36 H 0.4636 -0.1591 0.3166 0.086 Uiso 1 1 calc R . . C37 C 0.5002(3) -0.0050(9) 0.3409(4) 0.079(3) Uani 1 1 d . . . H37 H 0.5269 -0.0346 0.3736 0.094 Uiso 1 1 calc R . . C38 C 0.4986(3) 0.1148(9) 0.3262(4) 0.084(3) Uani 1 1 d . . . H38 H 0.5240 0.1667 0.3491 0.101 Uiso 1 1 calc R . . C39 C 0.4590(3) 0.1550(7) 0.2779(3) 0.065(2) Uani 1 1 d . . . H39 H 0.4579 0.2351 0.2678 0.078 Uiso 1 1 calc R . . O10 O 0.4650(9) 0.181(2) 0.0143(10) 0.170(5) Uani 0.454(12) 1 d PD A 1 C40 C 0.5092(13) 0.222(4) 0.0141(18) 0.170(5) Uani 0.454(12) 1 d PD A 1 C41 C 0.5184(19) 0.155(4) -0.029(2) 0.170(5) Uani 0.454(12) 1 d PD A 1 O10' O 0.5134(8) 0.174(2) 0.0405(10) 0.170(5) Uani 0.546(12) 1 d PD A 2 C41' C 0.5497(11) 0.083(3) -0.0203(13) 0.170(5) Uani 0.546(12) 1 d PD A 2 C40' C 0.5220(15) 0.176(3) -0.0086(14) 0.170(5) Uani 0.546(12) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0376(5) 0.0417(5) 0.0362(5) 0.0012(4) 0.0177(4) -0.0029(4) Ni2 0.0382(5) 0.0382(5) 0.0360(5) -0.0004(4) 0.0183(4) -0.0033(4) Ni3 0.0404(5) 0.0402(5) 0.0351(5) -0.0014(4) 0.0178(4) -0.0063(4) O1 0.046(3) 0.039(2) 0.035(2) -0.001(2) 0.024(2) -0.008(2) O2 0.039(3) 0.044(3) 0.033(2) 0.000(2) 0.013(2) 0.002(2) O3 0.040(2) 0.038(3) 0.041(3) -0.006(2) 0.018(2) -0.006(2) O4 0.043(3) 0.066(3) 0.041(3) 0.000(2) 0.016(2) -0.010(3) O5 0.042(3) 0.060(3) 0.045(3) 0.005(2) 0.019(2) -0.012(2) O6 0.038(3) 0.044(3) 0.045(3) 0.014(2) 0.015(2) 0.000(2) O7 0.047(3) 0.040(3) 0.048(3) 0.005(2) 0.028(2) -0.001(2) O8 0.044(3) 0.048(3) 0.035(2) 0.001(2) 0.014(2) -0.009(2) O9 0.052(3) 0.045(3) 0.031(2) 0.001(2) 0.015(2) -0.003(2) N1 0.039(3) 0.045(3) 0.035(3) 0.001(3) 0.015(3) -0.002(3) N2 0.034(3) 0.041(3) 0.040(3) 0.002(3) 0.017(3) -0.003(3) N3 0.040(3) 0.037(3) 0.041(3) 0.004(3) 0.022(3) -0.004(3) N4 0.043(3) 0.040(3) 0.034(3) -0.003(3) 0.019(3) -0.005(3) N5 0.054(4) 0.036(3) 0.035(3) 0.000(3) 0.015(3) -0.002(3) N6 0.040(3) 0.044(3) 0.032(3) 0.002(3) 0.015(3) 0.000(3) C1 0.051(4) 0.055(5) 0.044(4) 0.005(4) 0.024(4) 0.000(4) C2 0.078(6) 0.073(6) 0.044(4) 0.007(4) 0.041(4) 0.014(5) C3 0.105(7) 0.061(5) 0.062(6) 0.000(4) 0.048(5) 0.016(5) C4 0.068(5) 0.060(5) 0.059(5) 0.000(4) 0.034(4) 0.003(4) C5 0.048(4) 0.043(4) 0.050(4) 0.007(3) 0.029(4) 0.011(3) C6 0.047(4) 0.047(4) 0.051(4) 0.006(4) 0.027(4) 0.000(3) C7 0.051(4) 0.054(5) 0.049(4) 0.003(4) 0.028(4) -0.006(4) C8 0.050(4) 0.057(5) 0.057(5) 0.003(4) 0.026(4) 0.006(4) C9 0.068(5) 0.048(4) 0.065(5) -0.007(4) 0.037(5) 0.002(4) C10 0.056(5) 0.045(4) 0.050(4) -0.010(4) 0.028(4) -0.006(4) C11 0.050(4) 0.035(4) 0.040(4) -0.007(3) 0.023(3) -0.008(3) C12 0.044(4) 0.047(4) 0.040(4) -0.004(3) 0.019(3) -0.004(3) C13 0.062(5) 0.048(4) 0.048(4) 0.001(4) 0.014(4) -0.006(4) C14 0.079(6) 0.042(5) 0.071(6) -0.017(4) 0.009(5) -0.010(5) C15 0.079(7) 0.065(6) 0.124(9) -0.051(6) 0.032(6) -0.007(5) C16 0.070(6) 0.070(6) 0.081(6) -0.032(5) 0.034(5) 0.000(5) C17 0.045(4) 0.048(4) 0.031(4) -0.003(3) 0.008(3) -0.002(4) C18 0.047(4) 0.054(4) 0.046(4) -0.007(4) 0.025(4) 0.002(4) C19 0.038(4) 0.038(4) 0.051(5) -0.001(3) 0.020(4) -0.002(3) C20 0.039(4) 0.046(4) 0.043(4) -0.005(3) 0.016(3) -0.011(3) C21 0.043(4) 0.084(6) 0.044(4) 0.000(4) 0.013(4) -0.017(4) C22 0.059(5) 0.128(9) 0.050(5) 0.006(5) 0.006(4) -0.032(6) C23 0.068(6) 0.115(8) 0.058(6) -0.005(5) 0.017(5) -0.049(6) C24 0.068(6) 0.112(8) 0.065(6) 0.005(6) 0.033(5) -0.033(6) C25 0.057(5) 0.076(6) 0.050(5) -0.003(4) 0.021(4) -0.017(4) C26 0.050(4) 0.042(4) 0.039(4) -0.006(3) 0.024(4) -0.014(4) C27 0.047(4) 0.041(4) 0.038(4) 0.005(3) 0.025(3) 0.001(3) C28 0.059(5) 0.078(6) 0.060(5) 0.011(4) 0.026(4) -0.016(5) C29 0.072(6) 0.092(7) 0.095(7) 0.027(6) 0.051(6) -0.010(5) C30 0.101(7) 0.070(6) 0.074(6) 0.013(5) 0.064(6) -0.004(5) C31 0.090(7) 0.062(5) 0.058(5) 0.019(4) 0.043(5) 0.007(5) C32 0.058(5) 0.067(5) 0.064(5) 0.007(4) 0.039(4) 0.003(4) C33 0.046(4) 0.048(4) 0.037(4) -0.001(3) 0.024(3) 0.000(4) C34 0.045(4) 0.048(4) 0.036(4) 0.002(3) 0.023(3) 0.004(3) C35 0.059(5) 0.060(5) 0.049(5) 0.009(4) 0.022(4) 0.006(4) C36 0.083(6) 0.066(6) 0.058(5) 0.013(5) 0.023(5) 0.007(5) C37 0.064(6) 0.107(8) 0.052(5) 0.022(5) 0.015(5) 0.017(6) C38 0.069(6) 0.094(7) 0.052(5) 0.005(5) -0.003(5) -0.009(6) C39 0.066(5) 0.055(5) 0.053(5) -0.003(4) 0.008(4) -0.009(4) O10 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) C40 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) C41 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) O10' 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) C41' 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) C40' 0.174(9) 0.188(10) 0.179(13) -0.022(9) 0.108(11) 0.039(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O6 2.018(4) . ? Ni1 O2 2.035(4) . ? Ni1 N2 2.043(5) . ? Ni1 O4 2.055(4) . ? Ni1 N1 2.090(5) . ? Ni1 O3 2.124(4) . ? Ni2 O8 2.020(4) . ? Ni2 N4 2.027(5) . ? Ni2 O3 2.047(4) . ? Ni2 O7 2.055(4) . ? Ni2 N3 2.089(5) . ? Ni2 O1 2.129(4) 7 ? Ni3 O5 2.008(4) 7 ? Ni3 N6 2.020(5) . ? Ni3 O1 2.023(4) 7 ? Ni3 O9 2.053(4) . ? Ni3 N5 2.061(5) . ? Ni3 O2 2.153(4) 7 ? O1 N2 1.350(6) . ? O1 Ni3 2.023(4) 7 ? O1 Ni2 2.129(4) 7 ? O2 N4 1.354(6) . ? O2 Ni3 2.153(4) 7 ? O3 N6 1.351(6) . ? O4 C19 1.266(8) . ? O5 C19 1.246(8) . ? O5 Ni3 2.008(4) 7 ? O6 C26 1.248(8) . ? O7 C26 1.276(7) . ? O8 C33 1.261(7) . ? O9 C33 1.253(8) . ? N1 C5 1.345(8) . ? N1 C1 1.348(8) . ? N2 C6 1.289(8) . ? N3 C7 1.329(8) . ? N3 C11 1.359(8) . ? N4 C12 1.285(8) . ? N5 C13 1.332(8) . ? N5 C17 1.337(8) . ? N6 C18 1.289(8) . ? C1 C2 1.360(10) . ? C1 H1 0.9400 . ? C2 C3 1.379(10) . ? C2 H2 0.9400 . ? C3 C4 1.388(10) . ? C3 H3 0.9400 . ? C4 C5 1.390(9) . ? C4 H4 0.9400 . ? C5 C6 1.451(9) . ? C6 H6 0.9400 . ? C7 C8 1.388(9) . ? C7 H7 0.9400 . ? C8 C9 1.359(10) . ? C8 H8 0.9400 . ? C9 C10 1.388(10) . ? C9 H9 0.9400 . ? C10 C11 1.386(9) . ? C10 H10A 0.9400 . ? C11 C12 1.457(9) . ? C12 H12 0.9400 . ? C13 C14 1.387(10) . ? C13 H13 0.9400 . ? C14 C15 1.412(12) . ? C14 H14 0.9400 . ? C15 C16 1.370(11) . ? C15 H15 0.9400 . ? C16 C17 1.388(10) . ? C16 H16 0.9400 . ? C17 C18 1.467(9) . ? C18 H18 0.9400 . ? C19 C20 1.495(9) . ? C20 C21 1.376(9) . ? C20 C25 1.379(9) . ? C21 C22 1.392(10) . ? C21 H21 0.9400 . ? C22 C23 1.358(11) . ? C22 H22 0.9400 . ? C23 C24 1.372(11) . ? C23 H23 0.9400 . ? C24 C25 1.394(10) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C26 C27 1.507(9) . ? C27 C32 1.375(9) . ? C27 C28 1.374(9) . ? C28 C29 1.413(10) . ? C28 H28 0.9400 . ? C29 C30 1.347(11) . ? C29 H29 0.9400 . ? C30 C31 1.383(11) . ? C30 H30 0.9400 . ? C31 C32 1.380(10) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.505(9) . ? C34 C35 1.375(9) . ? C34 C39 1.394(9) . ? C35 C36 1.366(10) . ? C35 H35 0.9400 . ? C36 C37 1.372(12) . ? C36 H36 0.9400 . ? C37 C38 1.402(12) . ? C37 H37 0.9400 . ? C38 C39 1.375(10) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? O10 C40 1.430(19) . ? C40 C41 1.494(19) . ? O10' C40' 1.439(18) . ? C41' C40' 1.465(19) . ? 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 O6 Ni1 O2 98.69(18) . . ? O6 Ni1 N2 170.3(2) . . ? O2 Ni1 N2 90.8(2) . . ? O6 Ni1 O4 84.94(18) . . ? O2 Ni1 O4 89.33(18) . . ? N2 Ni1 O4 93.47(19) . . ? O6 Ni1 N1 91.9(2) . . ? O2 Ni1 N1 169.21(19) . . ? N2 Ni1 N1 78.5(2) . . ? O4 Ni1 N1 89.6(2) . . ? O6 Ni1 O3 86.01(17) . . ? O2 Ni1 O3 89.65(16) . . ? N2 Ni1 O3 95.86(18) . . ? O4 Ni1 O3 170.63(18) . . ? N1 Ni1 O3 93.11(18) . . ? O8 Ni2 N4 170.7(2) . . ? O8 Ni2 O3 100.09(17) . . ? N4 Ni2 O3 89.13(19) . . ? O8 Ni2 O7 85.15(17) . . ? N4 Ni2 O7 93.93(19) . . ? O3 Ni2 O7 87.23(17) . . ? O8 Ni2 N3 91.6(2) . . ? N4 Ni2 N3 79.2(2) . . ? O3 Ni2 N3 168.30(19) . . ? O7 Ni2 N3 93.08(18) . . ? O8 Ni2 O1 86.63(17) . 7 ? N4 Ni2 O1 94.82(18) . 7 ? O3 Ni2 O1 90.37(16) . 7 ? O7 Ni2 O1 170.90(17) . 7 ? N3 Ni2 O1 91.05(18) . 7 ? O5 Ni3 N6 171.7(2) 7 . ? O5 Ni3 O1 97.00(18) 7 7 ? N6 Ni3 O1 91.15(19) . 7 ? O5 Ni3 O9 85.82(18) 7 . ? N6 Ni3 O9 92.56(19) . . ? O1 Ni3 O9 89.48(17) 7 . ? O5 Ni3 N5 92.5(2) 7 . ? N6 Ni3 N5 79.3(2) . . ? O1 Ni3 N5 170.2(2) 7 . ? O9 Ni3 N5 88.71(19) . . ? O5 Ni3 O2 84.67(17) 7 7 ? N6 Ni3 O2 96.89(18) . 7 ? O1 Ni3 O2 91.41(16) 7 7 ? O9 Ni3 O2 170.49(17) . 7 ? N5 Ni3 O2 91.97(18) . 7 ? N2 O1 Ni3 112.8(3) . 7 ? N2 O1 Ni2 133.5(3) . 7 ? Ni3 O1 Ni2 107.37(19) 7 7 ? N4 O2 Ni1 113.8(3) . . ? N4 O2 Ni3 130.9(3) . 7 ? Ni1 O2 Ni3 107.11(19) . 7 ? N6 O3 Ni2 112.5(3) . . ? N6 O3 Ni1 131.8(3) . . ? Ni2 O3 Ni1 109.18(18) . . ? C19 O4 Ni1 126.7(4) . . ? C19 O5 Ni3 138.3(4) . 7 ? C26 O6 Ni1 134.8(4) . . ? C26 O7 Ni2 129.4(4) . . ? C33 O8 Ni2 134.3(4) . . ? C33 O9 Ni3 129.4(4) . . ? C5 N1 C1 118.5(6) . . ? C5 N1 Ni1 113.0(4) . . ? C1 N1 Ni1 128.3(5) . . ? C6 N2 O1 119.1(5) . . ? C6 N2 Ni1 115.8(5) . . ? O1 N2 Ni1 124.8(4) . . ? C7 N3 C11 118.3(6) . . ? C7 N3 Ni2 129.2(5) . . ? C11 N3 Ni2 112.2(4) . . ? C12 N4 O2 118.4(5) . . ? C12 N4 Ni2 116.2(5) . . ? O2 N4 Ni2 125.1(4) . . ? C13 N5 C17 119.6(6) . . ? C13 N5 Ni3 127.2(5) . . ? C17 N5 Ni3 113.2(5) . . ? C18 N6 O3 119.3(6) . . ? C18 N6 Ni3 116.2(5) . . ? O3 N6 Ni3 124.2(4) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.0(7) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.1(7) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.0(7) . . ? N1 C5 C6 115.3(6) . . ? C4 C5 C6 122.7(7) . . ? N2 C6 C5 117.0(6) . . ? N2 C6 H6 121.5 . . ? C5 C6 H6 121.5 . . ? N3 C7 C8 122.9(7) . . ? N3 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C9 C8 C7 119.4(7) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 118.5(7) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.8(7) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? N3 C11 C10 121.1(6) . . ? N3 C11 C12 115.2(6) . . ? C10 C11 C12 123.8(6) . . ? N4 C12 C11 117.1(6) . . ? N4 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? N5 C13 C14 122.2(8) . . ? N5 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C15 118.2(8) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C16 C15 C14 118.8(8) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.3(9) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N5 C17 C16 121.8(7) . . ? N5 C17 C18 115.4(6) . . ? C16 C17 C18 122.7(7) . . ? N6 C18 C17 115.8(6) . . ? N6 C18 H18 122.1 . . ? C17 C18 H18 122.1 . . ? O5 C19 O4 126.4(6) . . ? O5 C19 C20 115.6(6) . . ? O4 C19 C20 118.0(6) . . ? C21 C20 C25 118.4(6) . . ? C21 C20 C19 119.4(6) . . ? C25 C20 C19 122.2(6) . . ? C20 C21 C22 120.9(7) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 120.4(8) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.4(8) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 120.5(8) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 120.3(7) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? O6 C26 O7 127.1(6) . . ? O6 C26 C27 117.4(6) . . ? O7 C26 C27 115.5(6) . . ? C32 C27 C28 119.0(7) . . ? C32 C27 C26 121.0(6) . . ? C28 C27 C26 120.0(6) . . ? C27 C28 C29 119.6(8) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.9(8) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 119.2(8) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 120.5(8) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C27 C32 C31 120.8(8) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? O9 C33 O8 126.8(6) . . ? O9 C33 C34 116.7(6) . . ? O8 C33 C34 116.5(6) . . ? C35 C34 C39 117.8(7) . . ? C35 C34 C33 121.1(7) . . ? C39 C34 C33 121.0(6) . . ? C36 C35 C34 121.4(8) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 120.8(8) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 119.4(8) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 118.8(8) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C34 121.8(8) . . ? C38 C39 H39 119.1 . . ? C34 C39 H39 119.1 . . ? O10 C40 C41 110(3) . . ? O10' C40' C41' 123(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 O6 Ni1 O2 N4 -54.1(4) . . . . ? N2 Ni1 O2 N4 127.7(4) . . . . ? O4 Ni1 O2 N4 -138.9(4) . . . . ? N1 Ni1 O2 N4 136.8(9) . . . . ? O3 Ni1 O2 N4 31.8(4) . . . . ? O6 Ni1 O2 Ni3 153.80(18) . . . 7 ? N2 Ni1 O2 Ni3 -24.4(2) . . . 7 ? O4 Ni1 O2 Ni3 69.0(2) . . . 7 ? N1 Ni1 O2 Ni3 -15.4(11) . . . 7 ? O3 Ni1 O2 Ni3 -120.29(19) . . . 7 ? O8 Ni2 O3 N6 52.5(4) . . . . ? N4 Ni2 O3 N6 -129.0(4) . . . . ? O7 Ni2 O3 N6 137.0(4) . . . . ? N3 Ni2 O3 N6 -131.2(8) . . . . ? O1 Ni2 O3 N6 -34.2(4) 7 . . . ? O8 Ni2 O3 Ni1 -152.34(19) . . . . ? N4 Ni2 O3 Ni1 26.2(2) . . . . ? O7 Ni2 O3 Ni1 -67.8(2) . . . . ? N3 Ni2 O3 Ni1 24.0(10) . . . . ? O1 Ni2 O3 Ni1 121.0(2) 7 . . . ? O6 Ni1 O3 N6 -146.5(5) . . . . ? O2 Ni1 O3 N6 114.8(5) . . . . ? N2 Ni1 O3 N6 24.0(5) . . . . ? O4 Ni1 O3 N6 -161.5(10) . . . . ? N1 Ni1 O3 N6 -54.8(5) . . . . ? O6 Ni1 O3 Ni2 64.8(2) . . . . ? O2 Ni1 O3 Ni2 -33.9(2) . . . . ? N2 Ni1 O3 Ni2 -124.7(2) . . . . ? O4 Ni1 O3 Ni2 49.8(12) . . . . ? N1 Ni1 O3 Ni2 156.5(2) . . . . ? O6 Ni1 O4 C19 -132.7(6) . . . . ? O2 Ni1 O4 C19 -33.9(6) . . . . ? N2 Ni1 O4 C19 56.9(6) . . . . ? N1 Ni1 O4 C19 135.3(6) . . . . ? O3 Ni1 O4 C19 -117.7(11) . . . . ? O2 Ni1 O6 C26 66.3(6) . . . . ? N2 Ni1 O6 C26 -124.2(11) . . . . ? O4 Ni1 O6 C26 154.9(6) . . . . ? N1 Ni1 O6 C26 -115.7(6) . . . . ? O3 Ni1 O6 C26 -22.7(6) . . . . ? O8 Ni2 O7 C26 131.8(5) . . . . ? N4 Ni2 O7 C26 -57.6(5) . . . . ? O3 Ni2 O7 C26 31.4(5) . . . . ? N3 Ni2 O7 C26 -136.9(5) . . . . ? O1 Ni2 O7 C26 106.3(11) 7 . . . ? N4 Ni2 O8 C33 127.0(12) . . . . ? O3 Ni2 O8 C33 -62.0(6) . . . . ? O7 Ni2 O8 C33 -148.3(6) . . . . ? N3 Ni2 O8 C33 118.7(6) . . . . ? O1 Ni2 O8 C33 27.7(6) 7 . . . ? O5 Ni3 O9 C33 -126.6(6) 7 . . . ? N6 Ni3 O9 C33 61.6(6) . . . . ? O1 Ni3 O9 C33 -29.5(6) 7 . . . ? N5 Ni3 O9 C33 140.8(6) . . . . ? O2 Ni3 O9 C33 -124.9(10) 7 . . . ? O6 Ni1 N1 C5 178.8(5) . . . . ? O2 Ni1 N1 C5 -11.9(12) . . . . ? N2 Ni1 N1 C5 -2.7(4) . . . . ? O4 Ni1 N1 C5 -96.3(5) . . . . ? O3 Ni1 N1 C5 92.7(5) . . . . ? O6 Ni1 N1 C1 3.5(5) . . . . ? O2 Ni1 N1 C1 172.8(8) . . . . ? N2 Ni1 N1 C1 -178.0(6) . . . . ? O4 Ni1 N1 C1 88.4(5) . . . . ? O3 Ni1 N1 C1 -82.6(5) . . . . ? Ni3 O1 N2 C6 -152.0(5) 7 . . . ? Ni2 O1 N2 C6 60.4(7) 7 . . . ? Ni3 O1 N2 Ni1 21.5(5) 7 . . . ? Ni2 O1 N2 Ni1 -126.1(4) 7 . . . ? O6 Ni1 N2 C6 7.7(14) . . . . ? O2 Ni1 N2 C6 177.3(5) . . . . ? O4 Ni1 N2 C6 87.9(5) . . . . ? N1 Ni1 N2 C6 -1.0(5) . . . . ? O3 Ni1 N2 C6 -93.0(5) . . . . ? O6 Ni1 N2 O1 -166.0(9) . . . . ? O2 Ni1 N2 O1 3.5(4) . . . . ? O4 Ni1 N2 O1 -85.9(4) . . . . ? N1 Ni1 N2 O1 -174.8(4) . . . . ? O3 Ni1 N2 O1 93.2(4) . . . . ? O8 Ni2 N3 C7 -5.9(6) . . . . ? N4 Ni2 N3 C7 175.5(6) . . . . ? O3 Ni2 N3 C7 177.7(8) . . . . ? O7 Ni2 N3 C7 -91.1(6) . . . . ? O1 Ni2 N3 C7 80.7(5) 7 . . . ? O8 Ni2 N3 C11 -179.0(4) . . . . ? N4 Ni2 N3 C11 2.3(4) . . . . ? O3 Ni2 N3 C11 4.5(11) . . . . ? O7 Ni2 N3 C11 95.7(4) . . . . ? O1 Ni2 N3 C11 -92.4(4) 7 . . . ? Ni1 O2 N4 C12 154.1(5) . . . . ? Ni3 O2 N4 C12 -62.1(7) 7 . . . ? Ni1 O2 N4 Ni2 -19.4(5) . . . . ? Ni3 O2 N4 Ni2 124.3(4) 7 . . . ? O8 Ni2 N4 C12 -8.1(15) . . . . ? O3 Ni2 N4 C12 -179.2(5) . . . . ? O7 Ni2 N4 C12 -92.1(5) . . . . ? N3 Ni2 N4 C12 0.3(5) . . . . ? O1 Ni2 N4 C12 90.5(5) 7 . . . ? O8 Ni2 N4 O2 165.6(10) . . . . ? O3 Ni2 N4 O2 -5.5(4) . . . . ? O7 Ni2 N4 O2 81.6(4) . . . . ? N3 Ni2 N4 O2 174.0(5) . . . . ? O1 Ni2 N4 O2 -95.8(4) 7 . . . ? O5 Ni3 N5 C13 1.7(6) 7 . . . ? N6 Ni3 N5 C13 -179.7(6) . . . . ? O1 Ni3 N5 C13 166.9(9) 7 . . . ? O9 Ni3 N5 C13 87.4(6) . . . . ? O2 Ni3 N5 C13 -83.1(6) 7 . . . ? O5 Ni3 N5 C17 -179.4(5) 7 . . . ? N6 Ni3 N5 C17 -0.8(4) . . . . ? O1 Ni3 N5 C17 -14.2(14) 7 . . . ? O9 Ni3 N5 C17 -93.7(5) . . . . ? O2 Ni3 N5 C17 95.8(5) 7 . . . ? Ni2 O3 N6 C18 -151.2(5) . . . . ? Ni1 O3 N6 C18 60.9(7) . . . . ? Ni2 O3 N6 Ni3 22.1(5) . . . . ? Ni1 O3 N6 Ni3 -125.8(4) . . . . ? O5 Ni3 N6 C18 9.3(17) 7 . . . ? O1 Ni3 N6 C18 177.4(5) 7 . . . ? O9 Ni3 N6 C18 87.9(5) . . . . ? N5 Ni3 N6 C18 -0.3(5) . . . . ? O2 Ni3 N6 C18 -91.0(5) 7 . . . ? O5 Ni3 N6 O3 -164.1(12) 7 . . . ? O1 Ni3 N6 O3 3.9(4) 7 . . . ? O9 Ni3 N6 O3 -85.6(4) . . . . ? N5 Ni3 N6 O3 -173.8(5) . . . . ? O2 Ni3 N6 O3 95.5(4) 7 . . . ? C5 N1 C1 C2 0.5(10) . . . . ? Ni1 N1 C1 C2 175.6(6) . . . . ? N1 C1 C2 C3 -1.5(12) . . . . ? C1 C2 C3 C4 0.9(13) . . . . ? C2 C3 C4 C5 0.6(13) . . . . ? C1 N1 C5 C4 1.1(10) . . . . ? Ni1 N1 C5 C4 -174.7(6) . . . . ? C1 N1 C5 C6 -178.6(6) . . . . ? Ni1 N1 C5 C6 5.6(7) . . . . ? C3 C4 C5 N1 -1.6(11) . . . . ? C3 C4 C5 C6 178.0(7) . . . . ? O1 N2 C6 C5 178.5(5) . . . . ? Ni1 N2 C6 C5 4.4(8) . . . . ? N1 C5 C6 N2 -6.8(9) . . . . ? C4 C5 C6 N2 173.5(7) . . . . ? C11 N3 C7 C8 -0.1(10) . . . . ? Ni2 N3 C7 C8 -172.8(5) . . . . ? N3 C7 C8 C9 -1.3(11) . . . . ? C7 C8 C9 C10 1.7(11) . . . . ? C8 C9 C10 C11 -0.8(11) . . . . ? C7 N3 C11 C10 1.0(9) . . . . ? Ni2 N3 C11 C10 174.9(5) . . . . ? C7 N3 C11 C12 -178.4(6) . . . . ? Ni2 N3 C11 C12 -4.4(7) . . . . ? C9 C10 C11 N3 -0.6(10) . . . . ? C9 C10 C11 C12 178.7(7) . . . . ? O2 N4 C12 C11 -177.0(5) . . . . ? Ni2 N4 C12 C11 -2.9(8) . . . . ? N3 C11 C12 N4 5.0(9) . . . . ? C10 C11 C12 N4 -174.4(6) . . . . ? C17 N5 C13 C14 -1.1(10) . . . . ? Ni3 N5 C13 C14 177.8(6) . . . . ? N5 C13 C14 C15 1.6(12) . . . . ? C13 C14 C15 C16 -1.2(14) . . . . ? C14 C15 C16 C17 0.4(15) . . . . ? C13 N5 C17 C16 0.2(10) . . . . ? Ni3 N5 C17 C16 -178.8(6) . . . . ? C13 N5 C17 C18 -179.3(6) . . . . ? Ni3 N5 C17 C18 1.7(7) . . . . ? C15 C16 C17 N5 0.1(13) . . . . ? C15 C16 C17 C18 179.6(8) . . . . ? O3 N6 C18 C17 175.1(5) . . . . ? Ni3 N6 C18 C17 1.3(8) . . . . ? N5 C17 C18 N6 -2.0(9) . . . . ? C16 C17 C18 N6 178.5(7) . . . . ? Ni3 O5 C19 O4 15.6(12) 7 . . . ? Ni3 O5 C19 C20 -166.7(5) 7 . . . ? Ni1 O4 C19 O5 -9.0(10) . . . . ? Ni1 O4 C19 C20 173.3(4) . . . . ? O5 C19 C20 C21 -10.6(10) . . . . ? O4 C19 C20 C21 167.3(7) . . . . ? O5 C19 C20 C25 170.9(7) . . . . ? O4 C19 C20 C25 -11.2(10) . . . . ? C25 C20 C21 C22 1.5(12) . . . . ? C19 C20 C21 C22 -177.1(8) . . . . ? C20 C21 C22 C23 -1.6(15) . . . . ? C21 C22 C23 C24 1.3(16) . . . . ? C22 C23 C24 C25 -0.8(16) . . . . ? C21 C20 C25 C24 -1.0(12) . . . . ? C19 C20 C25 C24 177.5(7) . . . . ? C23 C24 C25 C20 0.7(14) . . . . ? Ni1 O6 C26 O7 -16.6(11) . . . . ? Ni1 O6 C26 C27 165.0(4) . . . . ? Ni2 O7 C26 O6 11.3(10) . . . . ? Ni2 O7 C26 C27 -170.3(4) . . . . ? O6 C26 C27 C32 -156.1(7) . . . . ? O7 C26 C27 C32 25.3(9) . . . . ? O6 C26 C27 C28 23.7(10) . . . . ? O7 C26 C27 C28 -154.9(7) . . . . ? C32 C27 C28 C29 -0.8(12) . . . . ? C26 C27 C28 C29 179.3(7) . . . . ? C27 C28 C29 C30 0.1(14) . . . . ? C28 C29 C30 C31 0.0(14) . . . . ? C29 C30 C31 C32 0.5(13) . . . . ? C28 C27 C32 C31 1.3(11) . . . . ? C26 C27 C32 C31 -178.8(7) . . . . ? C30 C31 C32 C27 -1.2(12) . . . . ? Ni3 O9 C33 O8 -11.7(10) . . . . ? Ni3 O9 C33 C34 168.8(4) . . . . ? Ni2 O8 C33 O9 12.0(11) . . . . ? Ni2 O8 C33 C34 -168.5(4) . . . . ? O9 C33 C34 C35 -176.2(6) . . . . ? O8 C33 C34 C35 4.3(10) . . . . ? O9 C33 C34 C39 0.4(10) . . . . ? O8 C33 C34 C39 -179.1(7) . . . . ? C39 C34 C35 C36 -0.7(11) . . . . ? C33 C34 C35 C36 176.1(7) . . . . ? C34 C35 C36 C37 0.8(13) . . . . ? C35 C36 C37 C38 -0.3(14) . . . . ? C36 C37 C38 C39 -0.3(15) . . . . ? C37 C38 C39 C34 0.5(14) . . . . ? C35 C34 C39 C38 0.0(12) . . . . ? C33 C34 C39 C38 -176.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.607 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.085