# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Unprecedented 10-connected three-dimensional bct nets and their magnetic behavior ; loop_ _publ_author_name 'Wei-Yin Sun.' 'Zhengshuai Bai.' 'Jian Fan.' 'Guang-Xiang Liu.' 'You Song.' ; Zhi Su ; data_1 _database_code_depnum_ccdc_archive 'CCDC 764874' #TrackingRef 'C002366C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Co3 N12 O12, 2(H2 O)' _chemical_formula_sum 'C48 H46 Co3 N12 O14' _chemical_formula_weight 1191.76 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5941(19) _cell_length_b 8.5724(9) _cell_length_c 16.3844(18) _cell_angle_alpha 90.00 _cell_angle_beta 106.052(2) _cell_angle_gamma 90.00 _cell_volume 2374.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6775 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.21 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7299 _exptl_absorpt_correction_T_max 0.8070 _exptl_absorpt_process_details 'sadabs, bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11404 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4166 _reflns_number_gt 3773 _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^)+(0.0448P)^2^+0.9922P] 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 4166 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.63190(14) -0.0069(3) 0.18134(16) 0.0272(5) Uani 1 1 d . . . C2 C 0.55970(14) 0.0289(3) 0.19416(16) 0.0298(6) Uani 1 1 d . . . H2 H 0.5563 0.0972 0.2371 0.036 Uiso 1 1 calc R . . C3 C 0.49258(14) -0.0388(3) 0.14191(16) 0.0266(5) Uani 1 1 d . . . C4 C 0.49712(14) -0.1430(3) 0.07923(16) 0.0303(6) Uani 1 1 d . . . H4 H 0.4517 -0.1906 0.0457 0.036 Uiso 1 1 calc R . . C5 C 0.56985(14) -0.1755(3) 0.06698(15) 0.0273(5) Uani 1 1 d . . . C6 C 0.63829(14) -0.1072(3) 0.11763(16) 0.0288(5) Uani 1 1 d . . . H6 H 0.6873 -0.1285 0.1088 0.035 Uiso 1 1 calc R . . C7 C 0.77757(18) 0.0073(4) 0.2498(3) 0.0684(12) Uani 1 1 d . . . H7 H 0.7941 -0.0800 0.2256 0.082 Uiso 1 1 calc R . . C8 C 0.82322(16) 0.1059(4) 0.3058(2) 0.0528(9) Uani 1 1 d . . . H8 H 0.8778 0.0974 0.3270 0.063 Uiso 1 1 calc R . . C9 C 0.70689(14) 0.1882(3) 0.28326(16) 0.0319(6) Uani 1 1 d . . . H9 H 0.6634 0.2484 0.2851 0.038 Uiso 1 1 calc R . . C10 C 0.40319(16) 0.0632(3) 0.22576(18) 0.0400(7) Uani 1 1 d . . . H10 H 0.4404 0.0961 0.2749 0.048 Uiso 1 1 calc R . . C11 C 0.32438(15) 0.0697(3) 0.20965(18) 0.0373(6) Uani 1 1 d . . . H11 H 0.2976 0.1085 0.2469 0.045 Uiso 1 1 calc R . . C12 C 0.34605(14) -0.0306(3) 0.09927(16) 0.0281(5) Uani 1 1 d . . . H12 H 0.3389 -0.0743 0.0457 0.034 Uiso 1 1 calc R . . C13 C 0.64371(17) -0.3261(4) -0.0161(2) 0.0550(9) Uani 1 1 d . . . H13 H 0.6950 -0.2956 0.0121 0.066 Uiso 1 1 calc R . . C14 C 0.6220(2) -0.4239(4) -0.0821(2) 0.0654(11) Uani 1 1 d . . . H14 H 0.6569 -0.4730 -0.1073 0.078 Uiso 1 1 calc R . . C15 C 0.51640(17) -0.3519(4) -0.05727(18) 0.0476(8) Uani 1 1 d . . . H15 H 0.4631 -0.3380 -0.0612 0.057 Uiso 1 1 calc R . . C16 C 0.90864(13) 0.7901(2) 0.59180(14) 0.0211(5) Uani 1 1 d . . . H16 H 0.9647 0.7699 0.5977 0.025 Uiso 1 1 calc R . . C17 C 0.89759(13) 0.8150(3) 0.67921(13) 0.0216(5) Uani 1 1 d . . . H17A H 0.9167 0.7241 0.7141 0.026 Uiso 1 1 calc R . . H17B H 0.8417 0.8263 0.6743 0.026 Uiso 1 1 calc R . . C18 C 0.94146(13) 0.9591(3) 0.72242(14) 0.0199(5) Uani 1 1 d . . . H18 H 0.9981 0.9450 0.7291 0.024 Uiso 1 1 calc R . . C19 C 0.91310(14) 1.1035(2) 0.66707(14) 0.0229(5) Uani 1 1 d . . . H19A H 0.8574 1.1208 0.6616 0.028 Uiso 1 1 calc R . . H19B H 0.9421 1.1944 0.6943 0.028 Uiso 1 1 calc R . . C20 C 0.92539(14) 1.0829(2) 0.57898(14) 0.0228(5) Uani 1 1 d . . . H20 H 0.9822 1.0733 0.5848 0.027 Uiso 1 1 calc R . . C21 C 0.88339(15) 0.9346(3) 0.53627(14) 0.0253(5) Uani 1 1 d . . . H21A H 0.8267 0.9483 0.5246 0.030 Uiso 1 1 calc R . . H21B H 0.8954 0.9191 0.4825 0.030 Uiso 1 1 calc R . . C22 C 0.86071(13) 0.6539(2) 0.54593(14) 0.0200(5) Uani 1 1 d . . . C23 C 0.92871(13) 0.9797(2) 0.80960(14) 0.0188(5) Uani 1 1 d . . . C24 C 0.89285(14) 1.2189(2) 0.52079(14) 0.0218(5) Uani 1 1 d . . . Co1 Co 0.824232(17) 0.41747(3) 0.410400(18) 0.01902(11) Uani 1 1 d . . . Co2 Co 1.0000 0.5000 0.5000 0.01639(12) Uani 1 2 d S . . N1 N 0.77916(11) 0.2193(2) 0.32730(12) 0.0273(4) Uani 1 1 d . . . N2 N 0.70205(12) 0.0604(2) 0.23518(14) 0.0300(5) Uani 1 1 d . . . N3 N 0.28870(11) 0.0108(2) 0.13013(13) 0.0255(4) Uani 1 1 d . . . N4 N 0.41795(12) -0.0021(2) 0.15466(13) 0.0286(5) Uani 1 1 d . . . N5 N 0.54230(17) -0.4420(3) -0.10763(18) 0.0588(8) Uani 1 1 d . . . N6 N 0.57612(12) -0.2802(3) 0.00183(13) 0.0333(5) Uani 1 1 d . . . O1 O 0.88734(9) 0.58733(16) 0.48854(9) 0.0195(3) Uani 1 1 d . . . O2 O 0.79823(10) 0.6166(2) 0.55974(11) 0.0318(4) Uani 1 1 d . . . O3 O 0.98798(9) 0.97629(19) 0.87280(10) 0.0254(4) Uani 1 1 d . . . O4 O 0.85858(10) 0.9995(2) 0.81118(10) 0.0319(4) Uani 1 1 d . . . O5 O 0.93428(9) 1.27919(17) 0.47697(10) 0.0241(4) Uani 1 1 d . . . O6 O 0.82307(9) 1.26401(19) 0.51168(10) 0.0291(4) Uani 1 1 d . . . O7 O 0.68450(15) 0.2139(4) 0.56387(18) 0.0907(9) Uani 1 1 d . . . H7C H 0.6882 0.2704 0.6074 0.109 Uiso 1 1 d R . . H7D H 0.7258 0.2274 0.5474 0.109 Uiso 1 1 d 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 C1 0.0199(12) 0.0318(13) 0.0270(13) -0.0059(11) 0.0018(10) -0.0051(10) C2 0.0246(13) 0.0342(13) 0.0294(14) -0.0107(11) 0.0055(11) -0.0036(11) C3 0.0198(12) 0.0305(12) 0.0285(13) -0.0006(11) 0.0050(10) -0.0018(10) C4 0.0247(13) 0.0331(13) 0.0293(13) -0.0064(11) 0.0009(10) -0.0066(11) C5 0.0287(13) 0.0281(12) 0.0254(13) -0.0054(10) 0.0080(10) -0.0048(10) C6 0.0230(12) 0.0348(13) 0.0297(13) -0.0069(11) 0.0093(10) -0.0032(10) C7 0.0231(15) 0.078(2) 0.094(3) -0.060(2) 0.0006(16) 0.0068(15) C8 0.0195(14) 0.067(2) 0.064(2) -0.0372(17) -0.0008(13) 0.0008(14) C9 0.0233(13) 0.0320(13) 0.0377(15) -0.0105(12) 0.0042(11) -0.0018(10) C10 0.0286(14) 0.0564(18) 0.0319(15) -0.0195(13) 0.0032(12) -0.0023(13) C11 0.0270(14) 0.0477(16) 0.0351(15) -0.0147(13) 0.0054(12) -0.0021(12) C12 0.0198(12) 0.0361(13) 0.0259(13) -0.0024(11) 0.0022(10) -0.0045(10) C13 0.0316(15) 0.070(2) 0.065(2) -0.0363(18) 0.0145(14) -0.0055(15) C14 0.051(2) 0.080(3) 0.070(2) -0.045(2) 0.0250(18) -0.0091(18) C15 0.0388(16) 0.0607(19) 0.0422(17) -0.0233(15) 0.0094(13) -0.0144(14) C16 0.0242(12) 0.0188(11) 0.0212(12) -0.0024(9) 0.0077(9) 0.0008(9) C17 0.0276(12) 0.0195(11) 0.0169(11) 0.0019(9) 0.0048(9) 0.0025(9) C18 0.0221(12) 0.0224(11) 0.0148(11) 0.0002(9) 0.0044(9) 0.0017(9) C19 0.0325(13) 0.0179(11) 0.0182(11) -0.0024(9) 0.0066(10) -0.0024(9) C20 0.0275(12) 0.0205(11) 0.0212(12) 0.0009(9) 0.0080(10) -0.0004(9) C21 0.0361(14) 0.0219(11) 0.0170(11) 0.0002(9) 0.0056(10) -0.0009(10) C22 0.0221(12) 0.0187(11) 0.0175(11) 0.0016(9) 0.0028(9) 0.0033(9) C23 0.0245(12) 0.0149(10) 0.0176(11) -0.0006(9) 0.0066(10) 0.0012(9) C24 0.0301(13) 0.0169(10) 0.0178(11) -0.0033(9) 0.0056(10) -0.0021(9) Co1 0.01664(18) 0.02115(17) 0.01761(17) 0.00045(12) 0.00196(12) -0.00184(12) Co2 0.0155(2) 0.0191(2) 0.0137(2) -0.00088(16) 0.00265(17) -0.00079(16) N1 0.0217(10) 0.0301(11) 0.0278(11) -0.0056(9) 0.0028(8) -0.0048(8) N2 0.0192(10) 0.0375(12) 0.0317(12) -0.0133(10) 0.0043(9) -0.0044(9) N3 0.0196(10) 0.0286(11) 0.0252(11) 0.0004(9) 0.0011(9) -0.0011(8) N4 0.0189(10) 0.0353(12) 0.0285(11) -0.0066(9) 0.0012(9) -0.0019(8) N5 0.0542(17) 0.0738(19) 0.0501(17) -0.0368(15) 0.0171(14) -0.0188(15) N6 0.0302(12) 0.0375(12) 0.0319(12) -0.0135(10) 0.0080(9) -0.0074(9) O1 0.0192(8) 0.0207(8) 0.0177(8) -0.0051(6) 0.0036(6) 0.0002(6) O2 0.0248(9) 0.0379(10) 0.0354(10) -0.0090(8) 0.0125(8) -0.0057(8) O3 0.0225(9) 0.0362(9) 0.0156(8) -0.0021(7) 0.0024(7) -0.0002(7) O4 0.0272(10) 0.0495(11) 0.0185(9) -0.0046(8) 0.0055(7) 0.0078(8) O5 0.0303(9) 0.0204(8) 0.0237(8) 0.0003(7) 0.0112(7) -0.0026(7) O6 0.0267(9) 0.0288(9) 0.0322(10) 0.0079(7) 0.0084(7) 0.0018(7) O7 0.0666(18) 0.125(3) 0.091(2) 0.0225(19) 0.0398(16) 0.0246(17) _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 C1 C2 1.378(3) . ? C1 C6 1.381(3) . ? C1 N2 1.426(3) . ? C2 C3 1.380(3) . ? C2 H2 0.9300 . ? C3 C4 1.380(3) . ? C3 N4 1.421(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 C6 1.389(3) . ? C5 N6 1.422(3) . ? C6 H6 0.9300 . ? C7 C8 1.339(4) . ? C7 N2 1.362(4) . ? C7 H7 0.9300 . ? C8 N1 1.349(3) . ? C8 H8 0.9300 . ? C9 N1 1.304(3) . ? C9 N2 1.338(3) . ? C9 H9 0.9300 . ? C10 C11 1.339(4) . ? C10 N4 1.380(3) . ? C10 H10 0.9300 . ? C11 N3 1.376(3) . ? C11 H11 0.9300 . ? C12 N3 1.297(3) . ? C12 N4 1.360(3) . ? C12 H12 0.9300 . ? C13 C14 1.338(4) . ? C13 N6 1.359(3) . ? C13 H13 0.9300 . ? C14 N5 1.356(4) . ? C14 H14 0.9300 . ? C15 N5 1.301(4) . ? C15 N6 1.363(3) . ? C15 H15 0.9300 . ? C16 C17 1.513(3) . ? C16 C22 1.513(3) . ? C16 C21 1.529(3) . ? C16 H16 0.9800 . ? C17 C18 1.523(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.516(3) . ? C18 C19 1.534(3) . ? C18 H18 0.9800 . ? C19 C20 1.527(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C24 1.514(3) . ? C20 C21 1.538(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O2 1.224(3) . ? C22 O1 1.293(3) . ? C23 O3 1.250(3) . ? C23 O4 1.253(3) . ? C24 O6 1.256(3) . ? C24 O5 1.266(3) . ? Co1 O4 2.0145(17) 4_575 ? Co1 O1 2.0508(15) . ? Co1 N3 2.0733(19) 2_655 ? Co1 O6 2.1221(16) 1_545 ? Co1 N1 2.1847(19) . ? Co1 O5 2.2751(16) 1_545 ? Co2 O3 2.0460(15) 4_575 ? Co2 O3 2.0460(15) 2_746 ? Co2 O1 2.0782(15) . ? Co2 O1 2.0782(15) 3_766 ? Co2 O5 2.1957(15) 1_545 ? Co2 O5 2.1957(15) 3_776 ? N3 Co1 2.0733(19) 2_645 ? O3 Co2 2.0460(15) 2_756 ? O4 Co1 2.0145(17) 4_576 ? O5 Co2 2.1957(15) 1_565 ? O5 Co1 2.2751(16) 1_565 ? O6 Co1 2.1221(16) 1_565 ? O7 H7C 0.8500 . ? O7 H7D 0.8500 . ? 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 C2 C1 C6 121.7(2) . . ? C2 C1 N2 119.5(2) . . ? C6 C1 N2 118.8(2) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 121.2(2) . . ? C4 C3 N4 119.9(2) . . ? C2 C3 N4 118.9(2) . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.0(2) . . ? C4 C5 N6 120.3(2) . . ? C6 C5 N6 118.7(2) . . ? C1 C6 C5 118.4(2) . . ? C1 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C8 C7 N2 106.3(3) . . ? C8 C7 H7 126.9 . . ? N2 C7 H7 126.9 . . ? C7 C8 N1 110.8(2) . . ? C7 C8 H8 124.6 . . ? N1 C8 H8 124.6 . . ? N1 C9 N2 112.7(2) . . ? N1 C9 H9 123.6 . . ? N2 C9 H9 123.6 . . ? C11 C10 N4 106.1(2) . . ? C11 C10 H10 127.0 . . ? N4 C10 H10 127.0 . . ? C10 C11 N3 110.4(2) . . ? C10 C11 H11 124.8 . . ? N3 C11 H11 124.8 . . ? N3 C12 N4 111.8(2) . . ? N3 C12 H12 124.1 . . ? N4 C12 H12 124.1 . . ? C14 C13 N6 106.5(3) . . ? C14 C13 H13 126.7 . . ? N6 C13 H13 126.7 . . ? C13 C14 N5 111.2(3) . . ? C13 C14 H14 124.4 . . ? N5 C14 H14 124.4 . . ? N5 C15 N6 112.5(3) . . ? N5 C15 H15 123.8 . . ? N6 C15 H15 123.8 . . ? C17 C16 C22 112.31(19) . . ? C17 C16 C21 110.89(18) . . ? C22 C16 C21 107.44(18) . . ? C17 C16 H16 108.7 . . ? C22 C16 H16 108.7 . . ? C21 C16 H16 108.7 . . ? C16 C17 C18 111.93(18) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C23 C18 C17 110.14(18) . . ? C23 C18 C19 110.76(18) . . ? C17 C18 C19 109.83(18) . . ? C23 C18 H18 108.7 . . ? C17 C18 H18 108.7 . . ? C19 C18 H18 108.7 . . ? C20 C19 C18 110.95(18) . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C24 C20 C19 112.23(18) . . ? C24 C20 C21 107.40(18) . . ? C19 C20 C21 110.48(19) . . ? C24 C20 H20 108.9 . . ? C19 C20 H20 108.9 . . ? C21 C20 H20 108.9 . . ? C16 C21 C20 112.03(18) . . ? C16 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C16 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O2 C22 O1 122.9(2) . . ? O2 C22 C16 121.0(2) . . ? O1 C22 C16 115.93(19) . . ? O3 C23 O4 125.9(2) . . ? O3 C23 C18 118.1(2) . . ? O4 C23 C18 116.0(2) . . ? O6 C24 O5 120.2(2) . . ? O6 C24 C20 119.9(2) . . ? O5 C24 C20 119.6(2) . . ? O4 Co1 O1 91.23(7) 4_575 . ? O4 Co1 N3 94.58(8) 4_575 2_655 ? O1 Co1 N3 103.39(7) . 2_655 ? O4 Co1 O6 156.93(7) 4_575 1_545 ? O1 Co1 O6 94.16(6) . 1_545 ? N3 Co1 O6 105.90(7) 2_655 1_545 ? O4 Co1 N1 84.84(7) 4_575 . ? O1 Co1 N1 169.06(7) . . ? N3 Co1 N1 87.12(8) 2_655 . ? O6 Co1 N1 85.69(7) 1_545 . ? O4 Co1 O5 99.53(6) 4_575 1_545 ? O1 Co1 O5 80.13(6) . 1_545 ? N3 Co1 O5 165.40(7) 2_655 1_545 ? O6 Co1 O5 59.54(6) 1_545 1_545 ? N1 Co1 O5 90.44(6) . 1_545 ? O3 Co2 O3 180 4_575 2_746 ? O3 Co2 O1 92.57(6) 4_575 . ? O3 Co2 O1 87.43(6) 2_746 . ? O3 Co2 O1 87.43(6) 4_575 3_766 ? O3 Co2 O1 92.57(6) 2_746 3_766 ? O1 Co2 O1 180 . 3_766 ? O3 Co2 O5 90.54(6) 4_575 1_545 ? O3 Co2 O5 89.46(6) 2_746 1_545 ? O1 Co2 O5 81.44(6) . 1_545 ? O1 Co2 O5 98.56(6) 3_766 1_545 ? O3 Co2 O5 89.46(6) 4_575 3_776 ? O3 Co2 O5 90.54(6) 2_746 3_776 ? O1 Co2 O5 98.56(6) . 3_776 ? O1 Co2 O5 81.44(6) 3_766 3_776 ? O5 Co2 O5 180 1_545 3_776 ? C9 N1 C8 104.5(2) . . ? C9 N1 Co1 129.35(17) . . ? C8 N1 Co1 125.96(16) . . ? C9 N2 C7 105.7(2) . . ? C9 N2 C1 126.8(2) . . ? C7 N2 C1 127.5(2) . . ? C12 N3 C11 105.6(2) . . ? C12 N3 Co1 123.36(17) . 2_645 ? C11 N3 Co1 126.21(17) . 2_645 ? C12 N4 C10 106.2(2) . . ? C12 N4 C3 126.1(2) . . ? C10 N4 C3 127.7(2) . . ? C15 N5 C14 104.5(2) . . ? C13 N6 C15 105.3(2) . . ? C13 N6 C5 126.8(2) . . ? C15 N6 C5 127.8(2) . . ? C22 O1 Co1 121.64(14) . . ? C22 O1 Co2 128.42(14) . . ? Co1 O1 Co2 97.98(6) . . ? C23 O3 Co2 131.99(15) . 2_756 ? C23 O4 Co1 125.55(15) . 4_576 ? C24 O5 Co2 127.81(14) . 1_565 ? C24 O5 Co1 86.42(13) . 1_565 ? Co2 O5 Co1 88.35(5) 1_565 1_565 ? C24 O6 Co1 93.64(13) . 1_565 ? H7C O7 H7D 108.4 . . ? 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 C6 C1 C2 C3 0.5(4) . . . . ? N2 C1 C2 C3 -179.3(2) . . . . ? C1 C2 C3 C4 1.4(4) . . . . ? C1 C2 C3 N4 -179.9(2) . . . . ? C2 C3 C4 C5 -2.2(4) . . . . ? N4 C3 C4 C5 179.1(2) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C3 C4 C5 N6 -178.9(2) . . . . ? C2 C1 C6 C5 -1.5(4) . . . . ? N2 C1 C6 C5 178.3(2) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? N6 C5 C6 C1 -179.3(2) . . . . ? N2 C7 C8 N1 0.2(5) . . . . ? N4 C10 C11 N3 -0.2(3) . . . . ? N6 C13 C14 N5 0.2(5) . . . . ? C22 C16 C17 C18 -176.00(18) . . . . ? C21 C16 C17 C18 -55.8(3) . . . . ? C16 C17 C18 C23 179.94(18) . . . . ? C16 C17 C18 C19 57.7(2) . . . . ? C23 C18 C19 C20 -179.67(19) . . . . ? C17 C18 C19 C20 -57.8(2) . . . . ? C18 C19 C20 C24 176.09(19) . . . . ? C18 C19 C20 C21 56.3(3) . . . . ? C17 C16 C21 C20 53.9(3) . . . . ? C22 C16 C21 C20 176.98(19) . . . . ? C24 C20 C21 C16 -177.05(19) . . . . ? C19 C20 C21 C16 -54.3(3) . . . . ? C17 C16 C22 O2 29.4(3) . . . . ? C21 C16 C22 O2 -92.8(2) . . . . ? C17 C16 C22 O1 -154.65(19) . . . . ? C21 C16 C22 O1 83.2(2) . . . . ? C17 C18 C23 O3 119.1(2) . . . . ? C19 C18 C23 O3 -119.2(2) . . . . ? C17 C18 C23 O4 -61.2(3) . . . . ? C19 C18 C23 O4 60.5(3) . . . . ? C19 C20 C24 O6 -51.4(3) . . . . ? C21 C20 C24 O6 70.3(3) . . . . ? C19 C20 C24 O5 133.6(2) . . . . ? C21 C20 C24 O5 -104.7(2) . . . . ? N2 C9 N1 C8 0.5(3) . . . . ? N2 C9 N1 Co1 176.09(16) . . . . ? C7 C8 N1 C9 -0.4(4) . . . . ? C7 C8 N1 Co1 -176.2(3) . . . . ? O4 Co1 N1 C9 -101.0(2) 4_575 . . . ? O1 Co1 N1 C9 -170.3(3) . . . . ? N3 Co1 N1 C9 -6.1(2) 2_655 . . . ? O6 Co1 N1 C9 100.1(2) 1_545 . . . ? O5 Co1 N1 C9 159.5(2) 1_545 . . . ? O4 Co1 N1 C8 73.7(2) 4_575 . . . ? O1 Co1 N1 C8 4.4(5) . . . . ? N3 Co1 N1 C8 168.6(3) 2_655 . . . ? O6 Co1 N1 C8 -85.2(2) 1_545 . . . ? O5 Co1 N1 C8 -25.8(2) 1_545 . . . ? N1 C9 N2 C7 -0.4(3) . . . . ? N1 C9 N2 C1 178.5(2) . . . . ? C8 C7 N2 C9 0.1(4) . . . . ? C8 C7 N2 C1 -178.7(3) . . . . ? C2 C1 N2 C9 -19.9(4) . . . . ? C6 C1 N2 C9 160.4(3) . . . . ? C2 C1 N2 C7 158.8(3) . . . . ? C6 C1 N2 C7 -21.0(4) . . . . ? N4 C12 N3 C11 0.2(3) . . . . ? N4 C12 N3 Co1 -156.49(16) . . . 2_645 ? C10 C11 N3 C12 0.0(3) . . . . ? C10 C11 N3 Co1 155.8(2) . . . 2_645 ? N3 C12 N4 C10 -0.3(3) . . . . ? N3 C12 N4 C3 177.5(2) . . . . ? C11 C10 N4 C12 0.3(3) . . . . ? C11 C10 N4 C3 -177.5(2) . . . . ? C4 C3 N4 C12 -16.2(4) . . . . ? C2 C3 N4 C12 165.0(2) . . . . ? C4 C3 N4 C10 161.1(3) . . . . ? C2 C3 N4 C10 -17.6(4) . . . . ? N6 C15 N5 C14 -2.2(4) . . . . ? C13 C14 N5 C15 1.2(5) . . . . ? C14 C13 N6 C15 -1.5(4) . . . . ? C14 C13 N6 C5 -179.7(3) . . . . ? N5 C15 N6 C13 2.4(4) . . . . ? N5 C15 N6 C5 -179.5(3) . . . . ? C4 C5 N6 C13 -178.2(3) . . . . ? C6 C5 N6 C13 1.8(4) . . . . ? C4 C5 N6 C15 4.0(4) . . . . ? C6 C5 N6 C15 -176.0(3) . . . . ? O2 C22 O1 Co1 2.9(3) . . . . ? C16 C22 O1 Co1 -172.96(13) . . . . ? O2 C22 O1 Co2 -131.30(19) . . . . ? C16 C22 O1 Co2 52.9(2) . . . . ? O4 Co1 O1 C22 141.86(16) 4_575 . . . ? N3 Co1 O1 C22 46.85(17) 2_655 . . . ? O6 Co1 O1 C22 -60.59(16) 1_545 . . . ? N1 Co1 O1 C22 -149.4(3) . . . . ? O5 Co1 O1 C22 -118.68(15) 1_545 . . . ? O4 Co1 O1 Co2 -72.72(7) 4_575 . . . ? N3 Co1 O1 Co2 -167.72(7) 2_655 . . . ? O6 Co1 O1 Co2 84.84(6) 1_545 . . . ? N1 Co1 O1 Co2 -4.0(4) . . . . ? O5 Co1 O1 Co2 26.75(6) 1_545 . . . ? O3 Co2 O1 C22 -155.59(17) 4_575 . . . ? O3 Co2 O1 C22 24.41(17) 2_746 . . . ? O5 Co2 O1 C22 114.25(17) 1_545 . . . ? O5 Co2 O1 C22 -65.75(17) 3_776 . . . ? O3 Co2 O1 Co1 62.47(7) 4_575 . . . ? O3 Co2 O1 Co1 -117.53(7) 2_746 . . . ? O5 Co2 O1 Co1 -27.69(6) 1_545 . . . ? O5 Co2 O1 Co1 152.31(6) 3_776 . . . ? O4 C23 O3 Co2 -0.3(3) . . . 2_756 ? C18 C23 O3 Co2 179.40(14) . . . 2_756 ? O3 C23 O4 Co1 15.9(3) . . . 4_576 ? C18 C23 O4 Co1 -163.74(14) . . . 4_576 ? O6 C24 O5 Co2 81.3(3) . . . 1_565 ? C20 C24 O5 Co2 -103.7(2) . . . 1_565 ? O6 C24 O5 Co1 -3.8(2) . . . 1_565 ? C20 C24 O5 Co1 171.18(18) . . . 1_565 ? O5 C24 O6 Co1 4.1(2) . . . 1_565 ? C20 C24 O6 Co1 -170.89(17) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.611 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.067 data_2 _database_code_depnum_ccdc_archive 'CCDC 764875' #TrackingRef 'C002366C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H47.82 Mn3 N12 O14.92' _chemical_formula_sum 'C48 H47.82 Mn3 N12 O14.92' _chemical_formula_weight 1196.34 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.3958(16) _cell_length_b 8.4767(7) _cell_length_c 16.6419(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.4240(10) _cell_angle_gamma 90.00 _cell_volume 2462.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6752 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7863 _exptl_absorpt_correction_T_max 0.9206 _exptl_absorpt_process_details sadabs,bruker(2000) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12096 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4444 _reflns_number_gt 4052 _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^)+(0.0529P)^2^+2.0993P] 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 4444 _refine_ls_number_parameters 359 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.111 _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 C1 C 0.58135(17) 0.6970(4) 0.06652(18) 0.0308(7) Uani 1 1 d . . . C2 C 0.64670(17) 0.6322(3) 0.12371(18) 0.0299(6) Uani 1 1 d . . . H2 H 0.6950 0.6547 0.1200 0.036 Uiso 1 1 calc R . . C3 C 0.63837(16) 0.5341(3) 0.18589(17) 0.0264(6) Uani 1 1 d . . . C4 C 0.56753(16) 0.4983(3) 0.19231(18) 0.0282(6) Uani 1 1 d . . . H4 H 0.5631 0.4320 0.2351 0.034 Uiso 1 1 calc R . . C5 C 0.50317(16) 0.5618(3) 0.13453(18) 0.0283(6) Uani 1 1 d . . . C6 C 0.50963(17) 0.6627(4) 0.07173(19) 0.0346(7) Uani 1 1 d . . . H6 H 0.4661 0.7069 0.0334 0.042 Uiso 1 1 calc R . . C7 C 0.6569(3) 0.8472(6) -0.0084(3) 0.0752(12) Uani 1 1 d U . . H7 H 0.7059 0.8136 0.0225 0.090 Uiso 1 1 calc R . . C8 C 0.6387(3) 0.9508(6) -0.0728(3) 0.0774(12) Uani 1 1 d U . . H8 H 0.6741 1.0034 -0.0925 0.093 Uiso 1 1 calc R . . C9 C 0.5348(2) 0.8753(5) -0.0587(2) 0.0518(9) Uani 1 1 d U . . H9 H 0.4827 0.8621 -0.0676 0.062 Uiso 1 1 calc R . . C10 C 0.77319(17) 0.5427(4) 0.2853(2) 0.0360(7) Uani 1 1 d . . . H10 H 0.7867 0.6454 0.2766 0.043 Uiso 1 1 calc R . . C11 C 0.81656(17) 0.4361(4) 0.3386(2) 0.0359(7) Uani 1 1 d . . . H11 H 0.8663 0.4542 0.3738 0.043 Uiso 1 1 calc R . . C12 C 0.71042(16) 0.3211(3) 0.27765(18) 0.0292(6) Uani 1 1 d . . . H12 H 0.6717 0.2459 0.2613 0.035 Uiso 1 1 calc R . . C13 C 0.4166(2) 0.4475(5) 0.2092(3) 0.0530(9) Uani 1 1 d U . . H13 H 0.4531 0.4078 0.2573 0.064 Uiso 1 1 calc R . . C14 C 0.34051(19) 0.4402(4) 0.1906(2) 0.0495(8) Uani 1 1 d U . . H14 H 0.3151 0.3909 0.2240 0.059 Uiso 1 1 calc R . . C15 C 0.36080(17) 0.5663(4) 0.0898(2) 0.0356(7) Uani 1 1 d U . . H15 H 0.3534 0.6243 0.0404 0.043 Uiso 1 1 calc R . . C16 C 0.07696(15) 0.4456(3) 0.25312(15) 0.0185(5) Uani 1 1 d . . . H16 H 0.0220 0.4253 0.2276 0.022 Uiso 1 1 calc R . . C17 C 0.11483(16) 0.3005(3) 0.30272(16) 0.0216(6) Uani 1 1 d . . . H17A H 0.1027 0.2094 0.2656 0.026 Uiso 1 1 calc R . . H17B H 0.1700 0.3146 0.3209 0.026 Uiso 1 1 calc R . . C18 C 0.08994(14) 0.2678(3) 0.38001(15) 0.0178(5) Uani 1 1 d . . . H18 H 0.0357 0.2379 0.3609 0.021 Uiso 1 1 calc R . . C19 C 0.09990(16) 0.4145(3) 0.43650(16) 0.0224(6) Uani 1 1 d . . . H19A H 0.0794 0.3930 0.4824 0.027 Uiso 1 1 calc R . . H19B H 0.1541 0.4375 0.4611 0.027 Uiso 1 1 calc R . . C20 C 0.05930(15) 0.5577(3) 0.38686(15) 0.0202(5) Uani 1 1 d . . . H20 H 0.0042 0.5360 0.3655 0.024 Uiso 1 1 calc R . . C21 C 0.08797(16) 0.5899(3) 0.31118(15) 0.0212(6) Uani 1 1 d . . . H21A H 0.0602 0.6788 0.2791 0.025 Uiso 1 1 calc R . . H21B H 0.1419 0.6175 0.3317 0.025 Uiso 1 1 calc R . . C22 C 0.11071(15) 0.4856(3) 0.18387(15) 0.0191(5) Uani 1 1 d . . . C23 C 0.13611(15) 0.1346(3) 0.43326(15) 0.0194(5) Uani 1 1 d . . . C24 C 0.07253(15) 0.7031(3) 0.44347(15) 0.0211(6) Uani 1 1 d . . . Mn1 Mn 0.18325(2) 0.58726(5) 0.07876(2) 0.01861(13) Uani 1 1 d . . . Mn2 Mn 0.0000 0.5000 0.0000 0.01674(15) Uani 1 2 d S . . N1 N 0.5622(2) 0.9681(4) -0.1048(2) 0.0616(8) Uani 1 1 d U . . N2 N 0.58959(16) 0.8007(3) 0.00291(17) 0.0423(7) Uani 1 1 d U . . N3 N 0.77761(13) 0.2963(3) 0.33434(15) 0.0293(5) Uani 1 1 d . . . N4 N 0.70436(13) 0.4687(3) 0.24595(15) 0.0269(5) Uani 1 1 d . . . N5 N 0.30507(13) 0.5156(3) 0.11529(16) 0.0315(5) Uani 1 1 d U . . N6 N 0.43021(13) 0.5261(3) 0.14246(16) 0.0323(6) Uani 1 1 d U . . O1 O 0.17597(11) 0.4389(2) 0.18789(12) 0.0285(4) Uani 1 1 d . . . O2 O 0.07313(10) 0.5766(2) 0.12392(10) 0.0206(4) Uani 1 1 d . . . O3 O 0.19646(12) 0.0899(3) 0.42381(14) 0.0383(5) Uani 1 1 d . . . O4 O 0.11086(10) 0.0778(2) 0.49057(11) 0.0214(4) Uani 1 1 d . . . O5 O 0.01508(11) 0.7786(2) 0.44553(13) 0.0314(5) Uani 1 1 d . . . O6 O 0.14090(11) 0.7364(2) 0.48479(12) 0.0279(4) Uani 1 1 d . . . O7 O 0.2650(2) 0.7912(4) 0.41723(19) 0.0766(9) Uani 1 1 d . . . O8 O 0.3574(8) 0.613(2) 0.3883(10) 0.227(12) Uani 0.461(16) 1 d P . . 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 C1 0.0308(16) 0.0330(16) 0.0285(15) 0.0085(12) 0.0091(12) 0.0065(12) C2 0.0242(14) 0.0335(16) 0.0338(15) 0.0081(13) 0.0116(12) 0.0046(12) C3 0.0221(14) 0.0296(15) 0.0261(14) 0.0057(12) 0.0058(12) 0.0057(11) C4 0.0248(15) 0.0325(16) 0.0272(14) 0.0086(12) 0.0082(12) 0.0035(12) C5 0.0218(14) 0.0326(16) 0.0301(15) 0.0003(12) 0.0077(12) 0.0027(12) C6 0.0248(15) 0.0423(18) 0.0333(16) 0.0122(14) 0.0041(12) 0.0103(13) C7 0.0494(19) 0.100(3) 0.076(2) 0.054(2) 0.0190(18) 0.006(2) C8 0.067(2) 0.096(3) 0.074(2) 0.053(2) 0.029(2) 0.008(2) C9 0.0495(18) 0.062(2) 0.0428(17) 0.0244(16) 0.0134(15) 0.0170(16) C10 0.0253(15) 0.0368(17) 0.0430(18) 0.0146(14) 0.0069(14) -0.0062(13) C11 0.0207(15) 0.0433(18) 0.0383(17) 0.0115(14) 0.0016(13) -0.0034(13) C12 0.0248(15) 0.0281(15) 0.0319(15) 0.0045(12) 0.0049(12) 0.0000(12) C13 0.0278(15) 0.067(2) 0.0619(19) 0.0321(17) 0.0107(14) 0.0070(15) C14 0.0279(15) 0.057(2) 0.0618(19) 0.0280(16) 0.0123(14) 0.0032(14) C15 0.0214(13) 0.0524(18) 0.0315(14) 0.0059(13) 0.0061(11) 0.0049(12) C16 0.0200(13) 0.0205(13) 0.0151(12) -0.0006(10) 0.0057(10) -0.0011(10) C17 0.0296(14) 0.0186(13) 0.0188(12) -0.0004(10) 0.0110(11) 0.0021(11) C18 0.0209(12) 0.0173(12) 0.0159(12) 0.0013(10) 0.0069(10) -0.0007(10) C19 0.0319(15) 0.0198(13) 0.0169(12) -0.0005(10) 0.0099(11) 0.0023(11) C20 0.0234(13) 0.0205(13) 0.0173(12) -0.0015(10) 0.0071(11) 0.0017(10) C21 0.0303(15) 0.0172(13) 0.0171(12) 0.0017(10) 0.0088(11) 0.0020(11) C22 0.0222(13) 0.0180(13) 0.0163(12) -0.0029(10) 0.0049(10) -0.0033(10) C23 0.0221(13) 0.0160(12) 0.0195(12) -0.0024(10) 0.0057(10) -0.0011(10) C24 0.0295(15) 0.0195(13) 0.0158(12) 0.0028(10) 0.0095(11) 0.0031(11) Mn1 0.0159(2) 0.0212(2) 0.0176(2) 0.00091(15) 0.00377(16) -0.00244(15) Mn2 0.0162(3) 0.0180(3) 0.0156(3) 0.0015(2) 0.0045(2) -0.0033(2) N1 0.0698(19) 0.0666(19) 0.0508(17) 0.0345(15) 0.0223(15) 0.0224(16) N2 0.0377(14) 0.0519(16) 0.0394(14) 0.0245(12) 0.0154(11) 0.0123(12) N3 0.0227(12) 0.0321(14) 0.0287(12) 0.0063(11) 0.0020(10) 0.0032(10) N4 0.0204(12) 0.0304(13) 0.0286(12) 0.0091(10) 0.0060(10) 0.0037(10) N5 0.0211(11) 0.0391(14) 0.0336(12) -0.0010(11) 0.0077(10) 0.0028(10) N6 0.0187(11) 0.0403(14) 0.0359(13) 0.0087(11) 0.0057(10) 0.0042(10) O1 0.0244(10) 0.0354(11) 0.0290(10) 0.0081(9) 0.0133(8) 0.0067(8) O2 0.0258(10) 0.0206(9) 0.0141(8) 0.0004(7) 0.0046(7) -0.0006(7) O3 0.0306(12) 0.0441(13) 0.0477(13) 0.0191(10) 0.0231(10) 0.0162(10) O4 0.0221(9) 0.0224(10) 0.0207(9) 0.0076(7) 0.0081(8) 0.0019(7) O5 0.0314(11) 0.0259(11) 0.0387(11) -0.0104(9) 0.0137(9) 0.0049(8) O6 0.0302(11) 0.0246(10) 0.0258(10) -0.0063(8) 0.0045(8) 0.0026(8) O7 0.092(2) 0.074(2) 0.0611(18) -0.0174(16) 0.0197(17) -0.0184(18) O8 0.182(15) 0.28(2) 0.27(2) 0.178(16) 0.134(14) 0.141(14) _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 C1 C6 1.380(4) . ? C1 C2 1.389(4) . ? C1 N2 1.421(4) . ? C2 C3 1.373(4) . ? C2 H2 0.9300 . ? C3 C4 1.375(4) . ? C3 N4 1.419(3) . ? C4 C5 1.377(4) . ? C4 H4 0.9300 . ? C5 C6 1.384(4) . ? C5 N6 1.422(4) . ? C6 H6 0.9300 . ? C7 C8 1.343(6) . ? C7 N2 1.369(5) . ? C7 H7 0.9300 . ? C8 N1 1.346(6) . ? C8 H8 0.9300 . ? C9 N1 1.306(5) . ? C9 N2 1.347(4) . ? C9 H9 0.9300 . ? C10 C11 1.339(4) . ? C10 N4 1.379(4) . ? C10 H10 0.9300 . ? C11 N3 1.375(4) . ? C11 H11 0.9300 . ? C12 N3 1.313(4) . ? C12 N4 1.349(4) . ? C12 H12 0.9300 . ? C13 C14 1.336(5) . ? C13 N6 1.385(4) . ? C13 H13 0.9300 . ? C14 N5 1.375(4) . ? C14 H14 0.9300 . ? C15 N5 1.300(4) . ? C15 N6 1.344(4) . ? C15 H15 0.9300 . ? C16 C22 1.510(3) . ? C16 C17 1.522(4) . ? C16 C21 1.532(3) . ? C16 H16 0.9800 . ? C17 C18 1.521(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.519(3) . ? C18 C19 1.534(3) . ? C18 H18 0.9800 . ? C19 C20 1.525(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C24 1.523(3) . ? C20 C21 1.536(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O1 1.246(3) . ? C22 O2 1.277(3) . ? C23 O3 1.229(3) . ? C23 O4 1.279(3) . ? C24 O5 1.245(3) . ? C24 O6 1.260(3) . ? Mn1 O6 2.1250(18) 4_575 ? Mn1 O4 2.1565(17) 4_565 ? Mn1 N5 2.213(2) . ? Mn1 O1 2.2478(19) . ? Mn1 N3 2.256(2) 2_655 ? Mn1 O2 2.3746(19) . ? Mn2 O5 2.1401(19) 4_575 ? Mn2 O5 2.1401(19) 2_545 ? Mn2 O2 2.1749(17) . ? Mn2 O2 2.1749(17) 3_565 ? Mn2 O4 2.1958(18) 4_565 ? Mn2 O4 2.1958(18) 2 ? N3 Mn1 2.256(2) 2_645 ? O4 Mn1 2.1565(17) 4_566 ? O4 Mn2 2.1958(18) 2_545 ? O5 Mn2 2.1401(19) 2 ? O6 Mn1 2.1250(18) 4_576 ? 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 C6 C1 C2 120.7(3) . . ? C6 C1 N2 120.4(3) . . ? C2 C1 N2 118.8(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 121.8(3) . . ? C2 C3 N4 119.5(3) . . ? C4 C3 N4 118.7(2) . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 N6 118.7(3) . . ? C6 C5 N6 120.7(3) . . ? C1 C6 C5 119.3(3) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 N2 106.8(4) . . ? C8 C7 H7 126.6 . . ? N2 C7 H7 126.6 . . ? C7 C8 N1 110.7(4) . . ? C7 C8 H8 124.7 . . ? N1 C8 H8 124.7 . . ? N1 C9 N2 113.3(4) . . ? N1 C9 H9 123.4 . . ? N2 C9 H9 123.4 . . ? C11 C10 N4 105.9(3) . . ? C11 C10 H10 127.1 . . ? N4 C10 H10 127.1 . . ? C10 C11 N3 110.8(3) . . ? C10 C11 H11 124.6 . . ? N3 C11 H11 124.6 . . ? N3 C12 N4 111.8(3) . . ? N3 C12 H12 124.1 . . ? N4 C12 H12 124.1 . . ? C14 C13 N6 106.2(3) . . ? C14 C13 H13 126.9 . . ? N6 C13 H13 126.9 . . ? C13 C14 N5 110.5(3) . . ? C13 C14 H14 124.8 . . ? N5 C14 H14 124.8 . . ? N5 C15 N6 112.8(3) . . ? N5 C15 H15 123.6 . . ? N6 C15 H15 123.6 . . ? C22 C16 C17 111.5(2) . . ? C22 C16 C21 107.3(2) . . ? C17 C16 C21 110.9(2) . . ? C22 C16 H16 109.0 . . ? C17 C16 H16 109.0 . . ? C21 C16 H16 109.0 . . ? C18 C17 C16 113.4(2) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C23 C18 C17 111.5(2) . . ? C23 C18 C19 107.98(19) . . ? C17 C18 C19 111.2(2) . . ? C23 C18 H18 108.7 . . ? C17 C18 H18 108.7 . . ? C19 C18 H18 108.7 . . ? C20 C19 C18 111.7(2) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C24 C20 C19 110.7(2) . . ? C24 C20 C21 109.5(2) . . ? C19 C20 C21 110.5(2) . . ? C24 C20 H20 108.7 . . ? C19 C20 H20 108.7 . . ? C21 C20 H20 108.7 . . ? C16 C21 C20 111.3(2) . . ? C16 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C16 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O1 C22 O2 120.6(2) . . ? O1 C22 C16 120.6(2) . . ? O2 C22 C16 118.7(2) . . ? O3 C23 O4 122.4(2) . . ? O3 C23 C18 121.0(2) . . ? O4 C23 C18 116.5(2) . . ? O5 C24 O6 125.4(2) . . ? O5 C24 C20 117.5(2) . . ? O6 C24 C20 117.1(2) . . ? O6 Mn1 O4 87.23(7) 4_575 4_565 ? O6 Mn1 N5 119.92(9) 4_575 . ? O4 Mn1 N5 111.27(8) 4_565 . ? O6 Mn1 O1 152.45(7) 4_575 . ? O4 Mn1 O1 90.29(7) 4_565 . ? N5 Mn1 O1 86.46(8) . . ? O6 Mn1 N3 83.56(8) 4_575 2_655 ? O4 Mn1 N3 161.65(8) 4_565 2_655 ? N5 Mn1 N3 87.08(9) . 2_655 ? O1 Mn1 N3 90.57(8) . 2_655 ? O6 Mn1 O2 96.25(7) 4_575 . ? O4 Mn1 O2 77.62(6) 4_565 . ? N5 Mn1 O2 142.52(8) . . ? O1 Mn1 O2 56.51(6) . . ? N3 Mn1 O2 87.62(8) 2_655 . ? O5 Mn2 O5 180 4_575 2_545 ? O5 Mn2 O2 90.90(7) 4_575 . ? O5 Mn2 O2 89.10(7) 2_545 . ? O5 Mn2 O2 89.10(7) 4_575 3_565 ? O5 Mn2 O2 90.90(7) 2_545 3_565 ? O2 Mn2 O2 180 . 3_565 ? O5 Mn2 O4 89.17(7) 4_575 4_565 ? O5 Mn2 O4 90.83(7) 2_545 4_565 ? O2 Mn2 O4 81.22(6) . 4_565 ? O2 Mn2 O4 98.78(6) 3_565 4_565 ? O5 Mn2 O4 90.83(7) 4_575 2 ? O5 Mn2 O4 89.17(7) 2_545 2 ? O2 Mn2 O4 98.78(6) . 2 ? O2 Mn2 O4 81.22(6) 3_565 2 ? O4 Mn2 O4 180 4_565 2 ? C9 N1 C8 104.6(3) . . ? C9 N2 C7 104.6(3) . . ? C9 N2 C1 128.9(3) . . ? C7 N2 C1 126.6(3) . . ? C12 N3 C11 104.8(2) . . ? C12 N3 Mn1 128.6(2) . 2_645 ? C11 N3 Mn1 126.02(18) . 2_645 ? C12 N4 C10 106.6(2) . . ? C12 N4 C3 125.8(2) . . ? C10 N4 C3 127.6(3) . . ? C15 N5 C14 104.8(3) . . ? C15 N5 Mn1 130.8(2) . . ? C14 N5 Mn1 121.7(2) . . ? C15 N6 C13 105.7(3) . . ? C15 N6 C5 128.0(3) . . ? C13 N6 C5 126.3(3) . . ? C22 O1 Mn1 94.64(15) . . ? C22 O2 Mn2 125.48(15) . . ? C22 O2 Mn1 87.99(15) . . ? Mn2 O2 Mn1 92.59(6) . . ? C23 O4 Mn1 117.37(16) . 4_566 ? C23 O4 Mn2 136.92(16) . 2_545 ? Mn1 O4 Mn2 98.28(7) 4_566 2_545 ? C24 O5 Mn2 133.41(18) . 2 ? C24 O6 Mn1 129.04(17) . 4_576 ? 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 C6 C1 C2 C3 -0.5(5) . . . . ? N2 C1 C2 C3 178.9(3) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 N4 -178.9(3) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? N4 C3 C4 C5 179.7(3) . . . . ? C3 C4 C5 C6 -1.2(5) . . . . ? C3 C4 C5 N6 -179.0(3) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? N2 C1 C6 C5 -179.7(3) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? N6 C5 C6 C1 179.0(3) . . . . ? N2 C7 C8 N1 -2.1(7) . . . . ? N4 C10 C11 N3 0.2(4) . . . . ? N6 C13 C14 N5 -1.8(5) . . . . ? C22 C16 C17 C18 172.7(2) . . . . ? C21 C16 C17 C18 53.1(3) . . . . ? C16 C17 C18 C23 -173.1(2) . . . . ? C16 C17 C18 C19 -52.5(3) . . . . ? C23 C18 C19 C20 176.5(2) . . . . ? C17 C18 C19 C20 53.9(3) . . . . ? C18 C19 C20 C24 -177.9(2) . . . . ? C18 C19 C20 C21 -56.4(3) . . . . ? C22 C16 C21 C20 -176.9(2) . . . . ? C17 C16 C21 C20 -54.8(3) . . . . ? C24 C20 C21 C16 179.1(2) . . . . ? C19 C20 C21 C16 56.9(3) . . . . ? C17 C16 C22 O1 -22.2(3) . . . . ? C21 C16 C22 O1 99.5(3) . . . . ? C17 C16 C22 O2 162.2(2) . . . . ? C21 C16 C22 O2 -76.1(3) . . . . ? C17 C18 C23 O3 15.9(3) . . . . ? C19 C18 C23 O3 -106.5(3) . . . . ? C17 C18 C23 O4 -167.5(2) . . . . ? C19 C18 C23 O4 70.1(3) . . . . ? C19 C20 C24 O5 -127.6(3) . . . . ? C21 C20 C24 O5 110.4(3) . . . . ? C19 C20 C24 O6 52.1(3) . . . . ? C21 C20 C24 O6 -70.0(3) . . . . ? N2 C9 N1 C8 1.3(5) . . . . ? C7 C8 N1 C9 0.5(6) . . . . ? N1 C9 N2 C7 -2.5(5) . . . . ? N1 C9 N2 C1 177.2(3) . . . . ? C8 C7 N2 C9 2.7(6) . . . . ? C8 C7 N2 C1 -177.0(4) . . . . ? C6 C1 N2 C9 -1.1(5) . . . . ? C2 C1 N2 C9 179.5(4) . . . . ? C6 C1 N2 C7 178.6(4) . . . . ? C2 C1 N2 C7 -0.8(6) . . . . ? N4 C12 N3 C11 -0.2(3) . . . . ? N4 C12 N3 Mn1 171.28(19) . . . 2_645 ? C10 C11 N3 C12 0.0(4) . . . . ? C10 C11 N3 Mn1 -171.8(2) . . . 2_645 ? N3 C12 N4 C10 0.4(3) . . . . ? N3 C12 N4 C3 -177.7(3) . . . . ? C11 C10 N4 C12 -0.3(4) . . . . ? C11 C10 N4 C3 177.7(3) . . . . ? C2 C3 N4 C12 -141.6(3) . . . . ? C4 C3 N4 C12 39.1(4) . . . . ? C2 C3 N4 C10 40.7(5) . . . . ? C4 C3 N4 C10 -138.6(3) . . . . ? N6 C15 N5 C14 1.4(4) . . . . ? N6 C15 N5 Mn1 162.7(2) . . . . ? C13 C14 N5 C15 0.3(4) . . . . ? C13 C14 N5 Mn1 -163.1(3) . . . . ? O6 Mn1 N5 C15 1.7(3) 4_575 . . . ? O4 Mn1 N5 C15 101.1(3) 4_565 . . . ? O1 Mn1 N5 C15 -169.9(3) . . . . ? N3 Mn1 N5 C15 -79.2(3) 2_655 . . . ? O2 Mn1 N5 C15 -161.4(2) . . . . ? O6 Mn1 N5 C14 160.3(2) 4_575 . . . ? O4 Mn1 N5 C14 -100.2(3) 4_565 . . . ? O1 Mn1 N5 C14 -11.3(3) . . . . ? N3 Mn1 N5 C14 79.4(3) 2_655 . . . ? O2 Mn1 N5 C14 -2.8(3) . . . . ? N5 C15 N6 C13 -2.5(4) . . . . ? N5 C15 N6 C5 -179.8(3) . . . . ? C14 C13 N6 C15 2.5(4) . . . . ? C14 C13 N6 C5 179.9(3) . . . . ? C4 C5 N6 C15 -174.8(3) . . . . ? C6 C5 N6 C15 7.3(5) . . . . ? C4 C5 N6 C13 8.3(5) . . . . ? C6 C5 N6 C13 -169.5(3) . . . . ? O2 C22 O1 Mn1 5.5(2) . . . . ? C16 C22 O1 Mn1 -170.0(2) . . . . ? O6 Mn1 O1 C22 6.6(3) 4_575 . . . ? O4 Mn1 O1 C22 -77.97(16) 4_565 . . . ? N5 Mn1 O1 C22 170.74(17) . . . . ? N3 Mn1 O1 C22 83.70(16) 2_655 . . . ? O2 Mn1 O1 C22 -3.06(14) . . . . ? O1 C22 O2 Mn2 86.5(3) . . . . ? C16 C22 O2 Mn2 -97.9(2) . . . . ? O1 C22 O2 Mn1 -5.2(2) . . . . ? C16 C22 O2 Mn1 170.4(2) . . . . ? O5 Mn2 O2 C22 -155.4(2) 4_575 . . . ? O5 Mn2 O2 C22 24.6(2) 2_545 . . . ? O4 Mn2 O2 C22 -66.4(2) 4_565 . . . ? O4 Mn2 O2 C22 113.6(2) 2 . . . ? O5 Mn2 O2 Mn1 -66.02(7) 4_575 . . . ? O5 Mn2 O2 Mn1 113.98(7) 2_545 . . . ? O4 Mn2 O2 Mn1 23.01(6) 4_565 . . . ? O4 Mn2 O2 Mn1 -156.99(6) 2 . . . ? O6 Mn1 O2 C22 -172.54(14) 4_575 . . . ? O4 Mn1 O2 C22 101.69(14) 4_565 . . . ? N5 Mn1 O2 C22 -7.2(2) . . . . ? O1 Mn1 O2 C22 2.98(13) . . . . ? N3 Mn1 O2 C22 -89.28(15) 2_655 . . . ? O6 Mn1 O2 Mn2 62.02(7) 4_575 . . . ? O4 Mn1 O2 Mn2 -23.75(6) 4_565 . . . ? N5 Mn1 O2 Mn2 -132.65(12) . . . . ? O1 Mn1 O2 Mn2 -122.46(9) . . . . ? N3 Mn1 O2 Mn2 145.28(8) 2_655 . . . ? O3 C23 O4 Mn1 5.2(3) . . . 4_566 ? C18 C23 O4 Mn1 -171.36(15) . . . 4_566 ? O3 C23 O4 Mn2 -137.1(2) . . . 2_545 ? C18 C23 O4 Mn2 46.3(3) . . . 2_545 ? O6 C24 O5 Mn2 8.9(4) . . . 2 ? C20 C24 O5 Mn2 -171.51(17) . . . 2 ? O5 C24 O6 Mn1 6.2(4) . . . 4_576 ? C20 C24 O6 Mn1 -173.38(16) . . . 4_576 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.748 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.072 data_3 _database_code_depnum_ccdc_archive 'CCDC 764876' #TrackingRef 'C002366C.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 N12 Ni3 O12, 2(H2O)' _chemical_formula_sum 'C48 H46 N12 Ni3 O14' _chemical_formula_weight 1191.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4216(15) _cell_length_b 8.5070(7) _cell_length_c 16.3463(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.5660(10) _cell_angle_gamma 90.00 _cell_volume 2322.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8379 _cell_measurement_theta_min 2.394 _cell_measurement_theta_max 28.268 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6664 _exptl_absorpt_correction_T_max 0.7824 _exptl_absorpt_process_details sadabs,bruker(2000) _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 11427 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4187 _reflns_number_gt 3888 _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^)+(0.0588P)^2^+1.4695P] 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 4187 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.173977(16) 0.91575(3) 0.090259(18) 0.01435(12) Uani 1 1 d . . . Ni2 Ni 0.0000 1.0000 0.0000 0.01315(13) Uani 1 2 d S . . C1 C 0.49119(15) 0.9638(3) 0.14126(17) 0.0236(5) Uani 1 1 d . . . C2 C 0.55957(16) 1.0318(3) 0.19428(18) 0.0261(6) Uani 1 1 d . . . H2 H 0.5563 1.1006 0.2374 0.031 Uiso 1 1 calc R . . C3 C 0.63285(16) 0.9956(3) 0.18207(18) 0.0244(6) Uani 1 1 d . . . C4 C 0.63879(15) 0.8938(3) 0.11799(17) 0.0250(6) Uani 1 1 d . . . H4 H 0.6882 0.8718 0.1094 0.030 Uiso 1 1 calc R . . C5 C 0.56945(15) 0.8256(3) 0.06703(16) 0.0243(5) Uani 1 1 d . . . C6 C 0.49528(15) 0.8578(3) 0.07866(17) 0.0262(6) Uani 1 1 d . . . H6 H 0.4493 0.8091 0.0450 0.031 Uiso 1 1 calc R . . C7 C 0.40111(18) 1.0682(4) 0.22445(19) 0.0341(7) Uani 1 1 d . . . H7 H 0.4391 1.1035 0.2733 0.041 Uiso 1 1 calc R . . C8 C 0.32149(17) 1.0731(3) 0.20894(19) 0.0318(6) Uani 1 1 d . . . H8 H 0.2947 1.1118 0.2464 0.038 Uiso 1 1 calc R . . C9 C 0.34285(15) 0.9714(3) 0.09805(17) 0.0235(5) Uani 1 1 d . . . H9 H 0.3353 0.9276 0.0442 0.028 Uiso 1 1 calc R . . C10 C 0.78067(19) 1.0110(4) 0.2498(3) 0.0569(11) Uani 1 1 d . . . H10 H 0.7973 0.9249 0.2242 0.068 Uiso 1 1 calc R . . C11 C 0.82711(18) 1.1082(4) 0.3068(2) 0.0449(9) Uani 1 1 d . . . H11 H 0.8825 1.0998 0.3278 0.054 Uiso 1 1 calc R . . C12 C 0.70872(16) 1.1899(3) 0.28605(17) 0.0266(6) Uani 1 1 d . . . H12 H 0.6647 1.2490 0.2889 0.032 Uiso 1 1 calc R . . C13 C 0.51510(18) 0.6466(4) -0.0578(2) 0.0417(8) Uani 1 1 d . . . H13 H 0.4611 0.6600 -0.0620 0.050 Uiso 1 1 calc R . . C14 C 0.54081(19) 0.5576(4) -0.1076(2) 0.0391(8) Uani 1 1 d . . . H14A H 0.5105 0.4954 -0.1519 0.047 Uiso 1 1 calc R . . C15 C 0.64422(19) 0.6724(4) -0.0154(2) 0.0475(9) Uani 1 1 d . . . H15 H 0.6962 0.7030 0.0132 0.057 Uiso 1 1 calc R . . C16 C 0.07351(15) 0.5894(3) -0.08072(15) 0.0186(5) Uani 1 1 d . . . H16 H 0.0160 0.5820 -0.0871 0.022 Uiso 1 1 calc R . . C17 C 0.11508(16) 0.4401(3) -0.03637(15) 0.0205(5) Uani 1 1 d . . . H17A H 0.1726 0.4527 -0.0237 0.025 Uiso 1 1 calc R . . H17B H 0.1025 0.4264 0.0173 0.025 Uiso 1 1 calc R . . C18 C 0.08932(14) 0.2931(3) -0.09123(14) 0.0171(5) Uani 1 1 d . . . H18 H 0.0326 0.2726 -0.0974 0.021 Uiso 1 1 calc R . . C19 C 0.10080(15) 0.3156(3) -0.17915(14) 0.0179(5) Uani 1 1 d . . . H19A H 0.0812 0.2234 -0.2137 0.022 Uiso 1 1 calc R . . H19B H 0.1575 0.3261 -0.1737 0.022 Uiso 1 1 calc R . . C20 C 0.05667(14) 0.4607(3) -0.22366(14) 0.0158(5) Uani 1 1 d . . . H20 H -0.0008 0.4477 -0.2308 0.019 Uiso 1 1 calc R . . C21 C 0.08632(15) 0.6067(3) -0.16888(15) 0.0185(5) Uani 1 1 d . . . H21A H 0.1429 0.6220 -0.1628 0.022 Uiso 1 1 calc R . . H21B H 0.0577 0.6985 -0.1971 0.022 Uiso 1 1 calc R . . C22 C 0.10780(14) 0.7255(3) -0.02280(14) 0.0170(5) Uani 1 1 d . . . C23 C 0.13870(14) 0.1561(3) -0.04458(14) 0.0164(5) Uani 1 1 d . . . C24 C 0.06998(14) 0.4783(2) -0.31126(15) 0.0150(5) Uani 1 1 d . . . N1 N 0.28492(13) 1.0122(2) 0.12901(14) 0.0209(4) Uani 1 1 d . . . N2 N 0.41566(13) 1.0003(2) 0.15358(14) 0.0245(5) Uani 1 1 d . . . N3 N 0.78207(12) 1.2215(2) 0.33007(13) 0.0225(4) Uani 1 1 d . . . N4 N 0.70365(13) 1.0629(3) 0.23611(15) 0.0257(5) Uani 1 1 d . . . N5 N 0.6216(2) 0.5733(5) -0.0821(3) 0.0789(12) Uani 1 1 d . . . N6 N 0.57534(13) 0.7191(3) 0.00192(15) 0.0293(5) Uani 1 1 d . . . O1 O 0.06812(10) 0.78385(17) 0.02481(10) 0.0172(3) Uani 1 1 d . . . O2 O 0.17725(10) 0.7734(2) -0.01572(11) 0.0223(4) Uani 1 1 d . . . O3 O 0.20163(11) 0.1199(2) -0.05862(12) 0.0272(4) Uani 1 1 d . . . O4 O 0.11231(10) 0.08988(17) 0.01362(10) 0.0159(3) Uani 1 1 d . . . O5 O 0.00988(10) 0.4760(2) -0.37512(10) 0.0197(4) Uani 1 1 d . . . O6 O 0.14133(11) 0.4961(2) -0.31155(11) 0.0233(4) Uani 1 1 d . . . O7 O 0.31473(16) 0.7119(4) 0.9326(2) 0.0748(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01432(18) 0.01599(18) 0.01221(19) 0.00021(10) 0.00293(14) 0.00124(11) Ni2 0.0142(2) 0.0152(2) 0.0098(2) 0.00031(14) 0.00317(17) 0.00072(15) C1 0.0187(13) 0.0268(12) 0.0250(14) -0.0008(11) 0.0057(11) -0.0010(10) C2 0.0218(13) 0.0304(13) 0.0254(14) -0.0097(11) 0.0057(11) -0.0035(11) C3 0.0203(13) 0.0282(13) 0.0227(14) -0.0063(10) 0.0028(11) -0.0046(10) C4 0.0199(13) 0.0302(13) 0.0264(14) -0.0067(11) 0.0088(11) -0.0026(10) C5 0.0264(13) 0.0240(12) 0.0228(14) -0.0057(10) 0.0073(11) -0.0047(10) C6 0.0207(13) 0.0306(13) 0.0254(14) -0.0074(11) 0.0033(11) -0.0062(11) C7 0.0263(15) 0.0473(17) 0.0269(15) -0.0177(13) 0.0048(12) -0.0029(13) C8 0.0239(14) 0.0407(16) 0.0293(16) -0.0120(12) 0.0049(12) -0.0009(12) C9 0.0186(12) 0.0309(13) 0.0196(13) -0.0039(10) 0.0029(11) -0.0042(11) C10 0.0226(16) 0.064(2) 0.077(3) -0.048(2) 0.0027(17) 0.0053(15) C11 0.0170(14) 0.0550(19) 0.056(2) -0.0299(17) -0.0002(14) 0.0024(13) C12 0.0220(13) 0.0254(13) 0.0314(15) -0.0098(11) 0.0060(11) -0.0002(10) C13 0.0306(16) 0.0552(19) 0.0368(18) -0.0187(15) 0.0057(14) -0.0120(14) C14 0.0341(16) 0.0513(18) 0.0324(17) -0.0314(15) 0.0103(14) -0.0156(14) C15 0.0303(16) 0.059(2) 0.054(2) -0.0294(17) 0.0126(15) -0.0030(15) C16 0.0234(13) 0.0164(11) 0.0166(13) -0.0019(9) 0.0068(10) -0.0007(9) C17 0.0309(14) 0.0173(11) 0.0126(12) 0.0003(9) 0.0048(10) 0.0011(10) C18 0.0208(12) 0.0155(11) 0.0152(12) 0.0013(9) 0.0056(10) 0.0001(9) C19 0.0261(12) 0.0144(11) 0.0133(12) 0.0000(9) 0.0057(10) -0.0003(9) C20 0.0177(11) 0.0178(11) 0.0114(11) 0.0011(9) 0.0034(9) -0.0004(9) C21 0.0275(13) 0.0147(11) 0.0135(12) 0.0011(9) 0.0061(10) 0.0006(9) C22 0.0233(12) 0.0143(11) 0.0126(11) 0.0029(9) 0.0039(10) 0.0017(9) C23 0.0195(12) 0.0153(11) 0.0141(11) -0.0019(9) 0.0042(9) -0.0032(9) C24 0.0219(12) 0.0096(10) 0.0149(12) 0.0006(8) 0.0076(10) 0.0002(9) N1 0.0181(10) 0.0223(10) 0.0207(11) 0.0005(8) 0.0027(9) -0.0010(8) N2 0.0180(11) 0.0312(12) 0.0230(12) -0.0060(9) 0.0040(9) -0.0016(8) N3 0.0211(10) 0.0241(10) 0.0214(11) -0.0047(9) 0.0047(9) -0.0033(9) N4 0.0168(11) 0.0316(12) 0.0270(12) -0.0116(10) 0.0035(9) -0.0035(9) N5 0.075(3) 0.085(3) 0.082(3) -0.043(2) 0.031(2) -0.006(2) N6 0.0270(12) 0.0333(12) 0.0283(12) -0.0132(10) 0.0092(10) -0.0063(10) O1 0.0217(8) 0.0154(8) 0.0155(8) -0.0007(6) 0.0071(7) 0.0017(6) O2 0.0223(9) 0.0232(9) 0.0235(9) -0.0060(7) 0.0098(7) -0.0019(7) O3 0.0229(10) 0.0329(10) 0.0290(10) 0.0097(8) 0.0128(8) 0.0060(8) O4 0.0184(8) 0.0170(8) 0.0128(8) 0.0036(6) 0.0051(7) -0.0003(6) O5 0.0218(9) 0.0264(9) 0.0101(8) 0.0008(7) 0.0033(7) -0.0002(7) O6 0.0202(9) 0.0356(10) 0.0135(9) 0.0039(7) 0.0040(7) -0.0041(7) O7 0.0517(16) 0.096(2) 0.085(2) -0.0201(18) 0.0324(16) -0.0120(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O6 1.9956(17) 4_576 ? Ni1 N1 2.028(2) . ? Ni1 O4 2.0372(16) 1_565 ? Ni1 N3 2.109(2) 2_645 ? Ni1 O2 2.1275(16) . ? Ni1 O1 2.1632(16) . ? Ni2 O5 2.0095(16) 2_554 ? Ni2 O5 2.0095(16) 4_576 ? Ni2 O4 2.0528(16) 1_565 ? Ni2 O4 2.0528(16) 3_565 ? Ni2 O1 2.1632(15) 3_575 ? Ni2 O1 2.1632(15) . ? C1 C6 1.381(4) . ? C1 C2 1.384(4) . ? C1 N2 1.421(3) . ? C2 C3 1.382(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 N4 1.417(3) . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 C6 1.386(4) . ? C5 N6 1.423(3) . ? C6 H6 0.9300 . ? C7 C8 1.338(4) . ? C7 N2 1.381(3) . ? C7 H7 0.9300 . ? C8 N1 1.381(4) . ? C8 H8 0.9300 . ? C9 N1 1.299(3) . ? C9 N2 1.355(3) . ? C9 H9 0.9300 . ? C10 C11 1.333(4) . ? C10 N4 1.369(4) . ? C10 H10 0.9300 . ? C11 N3 1.364(4) . ? C11 H11 0.9300 . ? C12 N3 1.303(3) . ? C12 N4 1.342(3) . ? C12 H12 0.9300 . ? C13 C14 1.283(4) . ? C13 N6 1.360(4) . ? C13 H13 0.9300 . ? C14 N5 1.356(5) . ? C14 H14A 0.9300 . ? C15 N5 1.346(5) . ? C15 N6 1.368(4) . ? C15 H15 0.9300 . ? C16 C22 1.507(3) . ? C16 C21 1.527(3) . ? C16 C17 1.538(3) . ? C16 H16 0.9800 . ? C17 C18 1.529(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.519(3) . ? C18 C23 1.519(3) . ? C18 H18 0.9800 . ? C19 C20 1.525(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C24 1.522(3) . ? C20 C21 1.532(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O2 1.251(3) . ? C22 O1 1.280(3) . ? C23 O3 1.222(3) . ? C23 O4 1.297(3) . ? C24 O5 1.250(3) . ? C24 O6 1.254(3) . ? N3 Ni1 2.109(2) 2_655 ? O4 Ni1 2.0372(16) 1_545 ? O4 Ni2 2.0528(16) 1_545 ? O5 Ni2 2.0095(16) 2_544 ? O6 Ni1 1.9956(17) 4_575 ? 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 N1 93.53(8) 4_576 . ? O6 Ni1 O4 90.00(7) 4_576 1_565 ? N1 Ni1 O4 100.75(7) . 1_565 ? O6 Ni1 N3 86.24(8) 4_576 2_645 ? N1 Ni1 N3 88.75(8) . 2_645 ? O4 Ni1 N3 169.99(7) 1_565 2_645 ? O6 Ni1 O2 161.57(7) 4_576 . ? N1 Ni1 O2 103.89(7) . . ? O4 Ni1 O2 92.57(7) 1_565 . ? N3 Ni1 O2 88.14(8) 2_645 . ? O6 Ni1 O1 101.21(7) 4_576 . ? N1 Ni1 O1 165.15(7) . . ? O4 Ni1 O1 81.21(6) 1_565 . ? N3 Ni1 O1 90.41(7) 2_645 . ? O2 Ni1 O1 61.26(6) . . ? O5 Ni2 O5 180 2_554 4_576 ? O5 Ni2 O4 87.18(7) 2_554 1_565 ? O5 Ni2 O4 92.82(7) 4_576 1_565 ? O5 Ni2 O4 92.82(7) 2_554 3_565 ? O5 Ni2 O4 87.18(7) 4_576 3_565 ? O4 Ni2 O4 180 1_565 3_565 ? O5 Ni2 O1 90.70(6) 2_554 3_575 ? O5 Ni2 O1 89.30(6) 4_576 3_575 ? O4 Ni2 O1 99.13(6) 1_565 3_575 ? O4 Ni2 O1 80.87(6) 3_565 3_575 ? O5 Ni2 O1 89.30(6) 2_554 . ? O5 Ni2 O1 90.70(6) 4_576 . ? O4 Ni2 O1 80.87(6) 1_565 . ? O4 Ni2 O1 99.13(6) 3_565 . ? O1 Ni2 O1 180 3_575 . ? C6 C1 C2 121.3(2) . . ? C6 C1 N2 119.6(2) . . ? C2 C1 N2 119.1(2) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 121.3(2) . . ? C2 C3 N4 119.7(2) . . ? C4 C3 N4 119.0(2) . . ? C5 C4 C3 118.4(2) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 N6 118.7(2) . . ? C6 C5 N6 119.8(2) . . ? C1 C6 C5 118.6(2) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 N2 106.4(2) . . ? C8 C7 H7 126.8 . . ? N2 C7 H7 126.8 . . ? C7 C8 N1 110.0(2) . . ? C7 C8 H8 125.0 . . ? N1 C8 H8 125.0 . . ? N1 C9 N2 111.9(2) . . ? N1 C9 H9 124.0 . . ? N2 C9 H9 124.0 . . ? C11 C10 N4 106.6(3) . . ? C11 C10 H10 126.7 . . ? N4 C10 H10 126.7 . . ? C10 C11 N3 110.5(3) . . ? C10 C11 H11 124.7 . . ? N3 C11 H11 124.7 . . ? N3 C12 N4 112.7(2) . . ? N3 C12 H12 123.6 . . ? N4 C12 H12 123.6 . . ? C14 C13 N6 112.7(3) . . ? C14 C13 H13 123.7 . . ? N6 C13 H13 123.7 . . ? C13 C14 N5 105.4(3) . . ? C13 C14 H14A 127.3 . . ? N5 C14 H14A 127.3 . . ? N5 C15 N6 106.1(3) . . ? N5 C15 H15 126.9 . . ? N6 C15 H15 126.9 . . ? C22 C16 C21 112.39(19) . . ? C22 C16 C17 106.81(19) . . ? C21 C16 C17 110.38(19) . . ? C22 C16 H16 109.1 . . ? C21 C16 H16 109.1 . . ? C17 C16 H16 109.1 . . ? C18 C17 C16 112.26(19) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C23 111.28(18) . . ? C19 C18 C17 110.88(18) . . ? C23 C18 C17 107.66(18) . . ? C19 C18 H18 109.0 . . ? C23 C18 H18 109.0 . . ? C17 C18 H18 109.0 . . ? C18 C19 C20 111.63(18) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C24 C20 C19 109.71(18) . . ? C24 C20 C21 110.71(18) . . ? C19 C20 C21 109.71(19) . . ? C24 C20 H20 108.9 . . ? C19 C20 H20 108.9 . . ? C21 C20 H20 108.9 . . ? C16 C21 C20 110.99(18) . . ? C16 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C16 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O2 C22 O1 119.5(2) . . ? O2 C22 C16 120.6(2) . . ? O1 C22 C16 119.6(2) . . ? O3 C23 O4 123.6(2) . . ? O3 C23 C18 120.6(2) . . ? O4 C23 C18 115.66(19) . . ? O5 C24 O6 126.4(2) . . ? O5 C24 C20 117.9(2) . . ? O6 C24 C20 115.6(2) . . ? C9 N1 C8 105.6(2) . . ? C9 N1 Ni1 123.22(18) . . ? C8 N1 Ni1 126.08(18) . . ? C9 N2 C7 106.1(2) . . ? C9 N2 C1 126.4(2) . . ? C7 N2 C1 127.5(2) . . ? C12 N3 C11 104.6(2) . . ? C12 N3 Ni1 128.97(17) . 2_655 ? C11 N3 Ni1 126.13(18) . 2_655 ? C12 N4 C10 105.6(2) . . ? C12 N4 C3 126.8(2) . . ? C10 N4 C3 127.6(2) . . ? C15 N5 C14 110.5(3) . . ? C13 N6 C15 105.2(2) . . ? C13 N6 C5 128.3(2) . . ? C15 N6 C5 126.4(2) . . ? C22 O1 Ni2 125.36(14) . . ? C22 O1 Ni1 88.28(13) . . ? Ni2 O1 Ni1 89.80(6) . . ? C22 O2 Ni1 90.65(13) . . ? C23 O4 Ni1 122.11(15) . 1_545 ? C23 O4 Ni2 127.47(15) . 1_545 ? Ni1 O4 Ni2 96.61(6) 1_545 1_545 ? C24 O5 Ni2 130.95(15) . 2_544 ? C24 O6 Ni1 123.96(16) . 4_575 ? 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 C6 C1 C2 C3 1.9(4) . . . . ? N2 C1 C2 C3 179.9(2) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C2 C3 N4 -179.5(3) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? N4 C3 C4 C5 178.3(2) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C3 C4 C5 N6 -179.1(2) . . . . ? C2 C1 C6 C5 -2.9(4) . . . . ? N2 C1 C6 C5 179.1(2) . . . . ? C4 C5 C6 C1 1.7(4) . . . . ? N6 C5 C6 C1 -178.8(2) . . . . ? N2 C7 C8 N1 -1.0(3) . . . . ? N4 C10 C11 N3 -0.2(5) . . . . ? N6 C13 C14 N5 -1.5(5) . . . . ? C22 C16 C17 C18 -176.50(19) . . . . ? C21 C16 C17 C18 -54.0(3) . . . . ? C16 C17 C18 C19 53.6(3) . . . . ? C16 C17 C18 C23 175.52(19) . . . . ? C23 C18 C19 C20 -175.49(18) . . . . ? C17 C18 C19 C20 -55.7(3) . . . . ? C18 C19 C20 C24 179.9(2) . . . . ? C18 C19 C20 C21 58.1(2) . . . . ? C22 C16 C21 C20 175.6(2) . . . . ? C17 C16 C21 C20 56.4(3) . . . . ? C24 C20 C21 C16 -179.7(2) . . . . ? C19 C20 C21 C16 -58.5(3) . . . . ? C21 C16 C22 O2 -47.7(3) . . . . ? C17 C16 C22 O2 73.5(3) . . . . ? C21 C16 C22 O1 138.1(2) . . . . ? C17 C16 C22 O1 -100.7(2) . . . . ? C19 C18 C23 O3 29.4(3) . . . . ? C17 C18 C23 O3 -92.3(3) . . . . ? C19 C18 C23 O4 -155.0(2) . . . . ? C17 C18 C23 O4 83.3(2) . . . . ? C19 C20 C24 O5 120.0(2) . . . . ? C21 C20 C24 O5 -118.8(2) . . . . ? C19 C20 C24 O6 -60.9(3) . . . . ? C21 C20 C24 O6 60.3(3) . . . . ? N2 C9 N1 C8 0.7(3) . . . . ? N2 C9 N1 Ni1 -155.25(17) . . . . ? C7 C8 N1 C9 0.2(3) . . . . ? C7 C8 N1 Ni1 155.3(2) . . . . ? O6 Ni1 N1 C9 166.4(2) 4_576 . . . ? O4 Ni1 N1 C9 -103.0(2) 1_565 . . . ? N3 Ni1 N1 C9 80.2(2) 2_645 . . . ? O2 Ni1 N1 C9 -7.6(2) . . . . ? O1 Ni1 N1 C9 -6.7(4) . . . . ? O6 Ni1 N1 C8 15.4(2) 4_576 . . . ? O4 Ni1 N1 C8 106.0(2) 1_565 . . . ? N3 Ni1 N1 C8 -70.8(2) 2_645 . . . ? O2 Ni1 N1 C8 -158.6(2) . . . . ? O1 Ni1 N1 C8 -157.7(2) . . . . ? N1 C9 N2 C7 -1.4(3) . . . . ? N1 C9 N2 C1 177.2(2) . . . . ? C8 C7 N2 C9 1.4(3) . . . . ? C8 C7 N2 C1 -177.1(3) . . . . ? C6 C1 N2 C9 -16.6(4) . . . . ? C2 C1 N2 C9 165.4(3) . . . . ? C6 C1 N2 C7 161.6(3) . . . . ? C2 C1 N2 C7 -16.3(4) . . . . ? N4 C12 N3 C11 0.2(3) . . . . ? N4 C12 N3 Ni1 174.19(17) . . . 2_655 ? C10 C11 N3 C12 0.0(4) . . . . ? C10 C11 N3 Ni1 -174.2(3) . . . 2_655 ? N3 C12 N4 C10 -0.4(4) . . . . ? N3 C12 N4 C3 178.5(3) . . . . ? C11 C10 N4 C12 0.3(4) . . . . ? C11 C10 N4 C3 -178.5(3) . . . . ? C2 C3 N4 C12 -18.1(4) . . . . ? C4 C3 N4 C12 162.2(3) . . . . ? C2 C3 N4 C10 160.5(3) . . . . ? C4 C3 N4 C10 -19.2(5) . . . . ? N6 C15 N5 C14 0.6(5) . . . . ? C13 C14 N5 C15 0.5(5) . . . . ? C14 C13 N6 C15 1.8(4) . . . . ? C14 C13 N6 C5 179.8(3) . . . . ? N5 C15 N6 C13 -1.4(4) . . . . ? N5 C15 N6 C5 -179.4(3) . . . . ? C4 C5 N6 C13 -176.0(3) . . . . ? C6 C5 N6 C13 4.6(4) . . . . ? C4 C5 N6 C15 1.6(4) . . . . ? C6 C5 N6 C15 -177.9(3) . . . . ? O2 C22 O1 Ni2 83.4(3) . . . . ? C16 C22 O1 Ni2 -102.3(2) . . . . ? O2 C22 O1 Ni1 -5.1(2) . . . . ? C16 C22 O1 Ni1 169.16(19) . . . . ? O5 Ni2 O1 C22 23.90(18) 2_554 . . . ? O5 Ni2 O1 C22 -156.10(18) 4_576 . . . ? O4 Ni2 O1 C22 -63.36(18) 1_565 . . . ? O4 Ni2 O1 C22 116.64(18) 3_565 . . . ? O5 Ni2 O1 Ni1 111.65(6) 2_554 . . . ? O5 Ni2 O1 Ni1 -68.35(6) 4_576 . . . ? O4 Ni2 O1 Ni1 24.39(6) 1_565 . . . ? O4 Ni2 O1 Ni1 -155.61(6) 3_565 . . . ? O6 Ni1 O1 C22 -170.94(13) 4_576 . . . ? N1 Ni1 O1 C22 2.0(3) . . . . ? O4 Ni1 O1 C22 100.82(13) 1_565 . . . ? N3 Ni1 O1 C22 -84.69(13) 2_645 . . . ? O2 Ni1 O1 C22 2.97(12) . . . . ? O6 Ni1 O1 Ni2 63.68(7) 4_576 . . . ? N1 Ni1 O1 Ni2 -123.4(3) . . . . ? O4 Ni1 O1 Ni2 -24.57(6) 1_565 . . . ? N3 Ni1 O1 Ni2 149.93(7) 2_645 . . . ? O2 Ni1 O1 Ni2 -122.42(8) . . . . ? O1 C22 O2 Ni1 5.2(2) . . . . ? C16 C22 O2 Ni1 -169.02(19) . . . . ? O6 Ni1 O2 C22 16.2(3) 4_576 . . . ? N1 Ni1 O2 C22 176.70(14) . . . . ? O4 Ni1 O2 C22 -81.56(14) 1_565 . . . ? N3 Ni1 O2 C22 88.45(14) 2_645 . . . ? O1 Ni1 O2 C22 -3.04(12) . . . . ? O3 C23 O4 Ni1 0.4(3) . . . 1_545 ? C18 C23 O4 Ni1 -175.04(14) . . . 1_545 ? O3 C23 O4 Ni2 -130.3(2) . . . 1_545 ? C18 C23 O4 Ni2 54.2(2) . . . 1_545 ? O6 C24 O5 Ni2 -0.6(3) . . . 2_544 ? C20 C24 O5 Ni2 178.38(14) . . . 2_544 ? O5 C24 O6 Ni1 18.0(3) . . . 4_575 ? C20 C24 O6 Ni1 -160.96(15) . . . 4_575 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.645 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.085