# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2075 data_dinuclear[Zn2L3Cl2] #1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Cl2 N4 O2 Zn2' _chemical_formula_weight 684.25 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.740(8) _cell_length_b 15.318(2) _cell_length_c 11.285(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.34(4) _cell_angle_gamma 90.00 _cell_volume 1457.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf-Nonius MACH-3' _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 2652 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2652 _reflns_number_gt 2076 _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 w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.5579P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(2) _refine_ls_number_reflns 2652 _refine_ls_number_parameters 363 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.012 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.28493(9) 0.33442(4) 0.33575(7) 0.0391(3) Uani 1 d . . . Zn2 Zn 0.21985(9) 0.50876(4) 0.17560(7) 0.0379(2) Uani 1 d . . . Cl1 Cl 0.2629(3) 0.3282(2) 0.52934(18) 0.0633(6) Uani 1 d . . . Cl2 Cl 0.2630(3) 0.5218(2) -0.0097(2) 0.0729(8) Uani 1 d . . . O1 O 0.3898(7) 0.4474(4) 0.2976(6) 0.0598(19) Uani 1 d . . . O2 O 0.1090(6) 0.4046(4) 0.2176(5) 0.0471(15) Uani 1 d . . . N1 N 0.4939(7) 0.2795(5) 0.3173(6) 0.0375(16) Uani 1 d . . . N2 N 0.1878(7) 0.2294(4) 0.2409(5) 0.0336(15) Uani 1 d . . . N3 N 0.0075(7) 0.5733(4) 0.1639(5) 0.0352(15) Uani 1 d . . . N4 N 0.3090(8) 0.6202(5) 0.2832(6) 0.0382(16) Uani 1 d . . . C1 C 0.5384(10) 0.4711(6) 0.3428(8) 0.040(2) Uani 1 d . . . C2 C 0.5723(10) 0.5616(6) 0.3627(7) 0.034(2) Uani 1 d . . . C3 C 0.7313(8) 0.5838(6) 0.4181(6) 0.0330(19) Uani 1 d . . . H3 H 0.7562 0.6422 0.4360 0.040 Uiso 1 calc R . . C4 C 0.8529(8) 0.5228(6) 0.4474(6) 0.039(2) Uani 1 d . . . C5 C 0.8152(9) 0.4364(6) 0.4193(6) 0.0369(19) Uani 1 d . . . H5 H 0.8959 0.3950 0.4335 0.044 Uiso 1 calc R . . C6 C 0.6580(9) 0.4098(6) 0.3697(6) 0.0353(19) Uani 1 d . . . C7 C 1.0209(9) 0.5491(7) 0.5127(8) 0.059(3) Uani 1 d . . . H7A H 1.0208 0.6072 0.5448 0.088 Uiso 1 calc R . . H7B H 1.0853 0.5476 0.4558 0.088 Uiso 1 calc R . . H7C H 1.0631 0.5093 0.5790 0.088 Uiso 1 calc R . . C8 C 0.4540(9) 0.6297(6) 0.3447(6) 0.0356(18) Uani 1 d . . . H8 H 0.4850 0.6839 0.3801 0.043 Uiso 1 calc R . . C9 C 0.6301(9) 0.3169(6) 0.3366(6) 0.0371(18) Uani 1 d . . . H9 H 0.7159 0.2835 0.3293 0.044 Uiso 1 calc R . . C10 C 0.4665(8) 0.1897(5) 0.2654(6) 0.0390(16) Uani 1 d . . . H10 H 0.4609 0.1933 0.1776 0.047 Uiso 1 calc R . . C11 C 0.5939(11) 0.1233(6) 0.3230(8) 0.047(2) Uani 1 d . . . H11A H 0.6032 0.1193 0.4104 0.057 Uiso 1 calc R . . H11B H 0.6952 0.1427 0.3126 0.057 Uiso 1 calc R . . C12 C 0.5540(10) 0.0331(5) 0.2639(7) 0.053(2) Uani 1 d . . . H12A H 0.5578 0.0356 0.1789 0.063 Uiso 1 calc R . . H12B H 0.6328 -0.0087 0.3063 0.063 Uiso 1 calc R . . C13 C 0.3886(8) 0.0024(6) 0.2694(7) 0.0486(17) Uani 1 d . . . H13A H 0.3626 -0.0517 0.2238 0.058 Uiso 1 calc R . . H13B H 0.3896 -0.0090 0.3541 0.058 Uiso 1 calc R . . C14 C 0.2629(9) 0.0701(6) 0.2162(7) 0.046(2) Uani 1 d . . . H14A H 0.2528 0.0761 0.1289 0.055 Uiso 1 calc R . . H14B H 0.1616 0.0504 0.2262 0.055 Uiso 1 calc R . . C15 C 0.3024(7) 0.1580(4) 0.2775(6) 0.0343(14) Uani 1 d . . . H15 H 0.3146 0.1484 0.3653 0.041 Uiso 1 calc R . . C16 C -0.0346(9) 0.3787(6) 0.1610(7) 0.0304(19) Uani 1 d . . . C17 C -0.0755(10) 0.2901(6) 0.1374(8) 0.037(2) Uani 1 d . . . C18 C -0.2295(9) 0.2669(7) 0.0746(7) 0.042(2) Uani 1 d . . . H18 H -0.2539 0.2081 0.0598 0.051 Uiso 1 calc R . . C19 C -0.3478(8) 0.3285(7) 0.0336(6) 0.0405(18) Uani 1 d . . . C20 C -0.3096(9) 0.4153(6) 0.0594(6) 0.0372(19) Uani 1 d . . . H20 H -0.3895 0.4566 0.0344 0.045 Uiso 1 calc R . . C21 C -0.1586(8) 0.4445(6) 0.1205(6) 0.0305(17) Uani 1 d . . . C22 C -0.5150(9) 0.3015(6) -0.0385(8) 0.057(2) Uani 1 d . . . H22A H -0.5916 0.3306 -0.0052 0.085 Uiso 1 calc R . . H22B H -0.5265 0.2395 -0.0324 0.085 Uiso 1 calc R . . H22C H -0.5317 0.3175 -0.1233 0.085 Uiso 1 calc R . . C23 C 0.0445(9) 0.2193(6) 0.1751(6) 0.0365(19) Uani 1 d . . . H23 H 0.0129 0.1630 0.1488 0.044 Uiso 1 calc R . . C24 C -0.1270(9) 0.5367(5) 0.1368(6) 0.0318(17) Uani 1 d . . . H24 H -0.2147 0.5731 0.1263 0.038 Uiso 1 calc R . . C25 C 0.0370(7) 0.6669(4) 0.1753(6) 0.0329(15) Uani 1 d . . . H25 H 0.0695 0.6837 0.1017 0.039 Uiso 1 calc R . . C26 C -0.1030(11) 0.7249(6) 0.1764(8) 0.049(2) Uani 1 d . . . H26A H -0.1421 0.7110 0.2470 0.059 Uiso 1 calc R . . H26B H -0.1881 0.7149 0.1027 0.059 Uiso 1 calc R . . C27 C -0.0513(9) 0.8209(5) 0.1824(7) 0.052(2) Uani 1 d . . . H27A H -0.0232 0.8360 0.1073 0.063 Uiso 1 calc R . . H27B H -0.1394 0.8577 0.1881 0.063 Uiso 1 calc R . . C28 C 0.0875(8) 0.8380(6) 0.2903(7) 0.0547(19) Uani 1 d . . . H28A H 0.0566 0.8270 0.3654 0.066 Uiso 1 calc R . . H28B H 0.1174 0.8990 0.2901 0.066 Uiso 1 calc R . . C29 C 0.2313(9) 0.7809(6) 0.2891(7) 0.042(2) Uani 1 d . . . H29A H 0.2695 0.7951 0.2182 0.051 Uiso 1 calc R . . H29B H 0.3163 0.7914 0.3626 0.051 Uiso 1 calc R . . C30 C 0.1807(7) 0.6853(4) 0.2836(6) 0.0363(15) Uani 1 d . . . H30 H 0.1466 0.6741 0.3583 0.044 Uiso 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 Zn1 0.0288(5) 0.0261(6) 0.0559(5) 0.0014(4) -0.0002(4) 0.0019(4) Zn2 0.0262(5) 0.0247(5) 0.0579(5) 0.0008(4) 0.0023(4) 0.0022(4) Cl1 0.0849(16) 0.0457(13) 0.0584(11) -0.0038(11) 0.0173(10) 0.0137(13) Cl2 0.0967(18) 0.0555(18) 0.0820(15) -0.0016(13) 0.0510(13) 0.0113(15) O1 0.034(3) 0.021(3) 0.106(5) 0.010(3) -0.014(3) -0.008(3) O2 0.022(3) 0.030(3) 0.075(4) 0.014(3) -0.012(2) 0.000(3) N1 0.028(3) 0.031(4) 0.051(4) 0.007(3) 0.006(3) 0.005(3) N2 0.030(3) 0.020(3) 0.045(3) 0.003(3) -0.001(3) 0.007(3) N3 0.033(4) 0.022(3) 0.046(3) 0.002(3) 0.003(3) -0.001(3) N4 0.033(4) 0.030(4) 0.049(3) 0.001(3) 0.007(3) -0.005(3) C1 0.025(4) 0.032(5) 0.051(5) 0.006(3) -0.010(4) -0.006(4) C2 0.031(5) 0.028(5) 0.042(4) 0.000(3) 0.011(4) -0.011(4) C3 0.024(4) 0.036(5) 0.039(4) 0.005(3) 0.008(3) 0.002(4) C4 0.025(4) 0.044(5) 0.044(4) 0.008(4) 0.004(3) -0.013(4) C5 0.027(4) 0.040(5) 0.043(4) 0.006(3) 0.008(3) -0.001(4) C6 0.030(4) 0.031(4) 0.040(4) 0.007(3) 0.001(3) -0.003(4) C7 0.032(4) 0.064(7) 0.067(5) 0.002(5) -0.007(4) -0.010(4) C8 0.030(4) 0.031(5) 0.043(4) 0.003(3) 0.004(3) 0.002(3) C9 0.031(4) 0.040(5) 0.039(4) 0.004(3) 0.006(3) -0.001(3) C10 0.043(4) 0.032(4) 0.040(4) -0.001(3) 0.007(3) 0.007(3) C11 0.032(5) 0.047(6) 0.061(5) 0.006(4) 0.010(4) -0.001(4) C12 0.058(5) 0.039(4) 0.066(5) 0.004(4) 0.023(4) 0.012(4) C13 0.048(4) 0.036(4) 0.060(4) -0.002(4) 0.011(3) 0.003(3) C14 0.050(6) 0.030(5) 0.056(5) -0.008(4) 0.010(4) 0.001(4) C15 0.035(3) 0.025(3) 0.042(4) -0.002(3) 0.007(3) 0.002(3) C16 0.022(4) 0.036(5) 0.034(4) 0.005(3) 0.009(3) -0.001(4) C17 0.028(5) 0.037(5) 0.040(4) 0.011(4) -0.001(3) 0.008(4) C18 0.037(5) 0.039(5) 0.045(5) -0.004(4) 0.002(4) -0.016(4) C19 0.028(4) 0.043(5) 0.047(4) -0.005(4) 0.003(3) -0.001(4) C20 0.029(4) 0.042(5) 0.036(4) 0.006(3) 0.000(3) 0.006(4) C21 0.022(4) 0.032(4) 0.036(4) 0.004(3) 0.006(3) 0.000(3) C22 0.032(4) 0.042(5) 0.083(6) 0.004(4) -0.009(4) -0.007(4) C23 0.043(5) 0.028(5) 0.035(4) 0.001(3) 0.005(3) -0.008(4) C24 0.029(4) 0.031(4) 0.033(3) 0.002(3) 0.005(3) 0.010(3) C25 0.029(3) 0.025(3) 0.041(4) 0.002(3) 0.004(3) 0.007(3) C26 0.038(5) 0.028(5) 0.075(6) -0.006(4) 0.001(4) 0.011(4) C27 0.052(4) 0.031(4) 0.069(5) -0.004(4) 0.008(4) 0.017(3) C28 0.048(4) 0.035(4) 0.078(5) -0.009(4) 0.012(4) 0.005(4) C29 0.042(5) 0.033(5) 0.050(5) -0.003(4) 0.008(4) -0.001(4) C30 0.033(3) 0.033(3) 0.041(4) -0.004(3) 0.006(3) 0.005(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 Zn1 N2 1.994(6) . ? Zn1 O2 2.052(5) . ? Zn1 O1 2.057(6) . ? Zn1 N1 2.070(7) . ? Zn1 Cl1 2.246(2) . ? Zn2 O1 1.975(6) . ? Zn2 O2 1.989(6) . ? Zn2 N3 2.076(7) . ? Zn2 N4 2.120(7) . ? Zn2 Cl2 2.229(2) . ? O1 C1 1.315(9) . ? O2 C16 1.310(9) . ? N1 C9 1.287(9) . ? N1 C10 1.490(10) . ? N2 C23 1.286(9) . ? N2 C15 1.466(9) . ? N3 C24 1.265(9) . ? N3 C25 1.456(9) . ? N4 C8 1.282(9) . ? N4 C30 1.502(9) . ? C1 C6 1.378(12) . ? C1 C2 1.423(11) . ? C2 C3 1.407(10) . ? C2 C8 1.444(12) . ? C3 C4 1.388(11) . ? C4 C5 1.380(13) . ? C4 C7 1.513(10) . ? C5 C6 1.401(10) . ? C6 C9 1.475(12) . ? C10 C11 1.520(11) . ? C10 C15 1.554(9) . ? C11 C12 1.534(12) . ? C12 C13 1.537(10) . ? C13 C14 1.515(11) . ? C14 C15 1.511(10) . ? C16 C17 1.411(12) . ? C16 C21 1.462(11) . ? C17 C18 1.391(11) . ? C17 C23 1.490(12) . ? C18 C19 1.387(12) . ? C19 C20 1.382(14) . ? C19 C22 1.529(10) . ? C20 C21 1.391(10) . ? C21 C24 1.442(11) . ? C25 C26 1.515(10) . ? C25 C30 1.529(8) . ? C26 C27 1.534(12) . ? C27 C28 1.498(9) . ? C28 C29 1.534(10) . ? C29 C30 1.526(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 O2 86.2(3) . . ? N2 Zn1 O1 135.8(3) . . ? O2 Zn1 O1 73.9(2) . . ? N2 Zn1 N1 83.1(3) . . ? O2 Zn1 N1 132.6(2) . . ? O1 Zn1 N1 82.3(3) . . ? N2 Zn1 Cl1 110.8(2) . . ? O2 Zn1 Cl1 114.30(19) . . ? O1 Zn1 Cl1 113.4(2) . . ? N1 Zn1 Cl1 112.70(19) . . ? O1 Zn2 O2 77.1(2) . . ? O1 Zn2 N3 140.0(3) . . ? O2 Zn2 N3 85.0(2) . . ? O1 Zn2 N4 83.6(3) . . ? O2 Zn2 N4 129.6(3) . . ? N3 Zn2 N4 80.8(3) . . ? O1 Zn2 Cl2 114.4(2) . . ? O2 Zn2 Cl2 120.6(2) . . ? N3 Zn2 Cl2 105.53(19) . . ? N4 Zn2 Cl2 109.7(2) . . ? C1 O1 Zn2 128.5(6) . . ? C1 O1 Zn1 126.9(5) . . ? Zn2 O1 Zn1 104.6(3) . . ? C16 O2 Zn2 126.2(5) . . ? C16 O2 Zn1 127.9(5) . . ? Zn2 O2 Zn1 104.3(2) . . ? C9 N1 C10 121.5(7) . . ? C9 N1 Zn1 127.1(6) . . ? C10 N1 Zn1 111.2(5) . . ? C23 N2 C15 124.2(7) . . ? C23 N2 Zn1 128.2(6) . . ? C15 N2 Zn1 106.8(4) . . ? C24 N3 C25 126.1(6) . . ? C24 N3 Zn2 124.2(6) . . ? C25 N3 Zn2 109.2(4) . . ? C8 N4 C30 123.7(7) . . ? C8 N4 Zn2 124.2(6) . . ? C30 N4 Zn2 112.0(4) . . ? O1 C1 C6 120.7(8) . . ? O1 C1 C2 118.3(8) . . ? C6 C1 C2 121.0(8) . . ? C3 C2 C1 116.4(8) . . ? C3 C2 C8 118.4(8) . . ? C1 C2 C8 124.7(8) . . ? C4 C3 C2 123.2(8) . . ? C3 C4 C5 118.0(7) . . ? C3 C4 C7 121.3(9) . . ? C5 C4 C7 120.7(8) . . ? C4 C5 C6 121.4(8) . . ? C1 C6 C5 119.8(8) . . ? C1 C6 C9 122.5(7) . . ? C5 C6 C9 117.4(8) . . ? N4 C8 C2 124.3(8) . . ? N1 C9 C6 123.8(8) . . ? N1 C10 C11 115.2(6) . . ? N1 C10 C15 108.0(5) . . ? C11 C10 C15 110.0(6) . . ? C10 C11 C12 111.1(6) . . ? C13 C12 C11 111.5(7) . . ? C14 C13 C12 111.5(7) . . ? C15 C14 C13 112.0(6) . . ? N2 C15 C14 118.6(6) . . ? N2 C15 C10 108.7(6) . . ? C14 C15 C10 110.0(6) . . ? O2 C16 C17 123.1(8) . . ? O2 C16 C21 118.6(8) . . ? C17 C16 C21 118.3(8) . . ? C18 C17 C16 120.3(8) . . ? C18 C17 C23 118.2(9) . . ? C16 C17 C23 121.5(8) . . ? C17 C18 C19 122.1(9) . . ? C20 C19 C18 117.8(7) . . ? C20 C19 C22 121.1(8) . . ? C18 C19 C22 121.1(9) . . ? C19 C20 C21 123.9(8) . . ? C20 C21 C24 120.2(7) . . ? C20 C21 C16 117.5(8) . . ? C24 C21 C16 122.3(7) . . ? N2 C23 C17 125.6(8) . . ? N3 C24 C21 126.9(7) . . ? N3 C25 C26 117.0(6) . . ? N3 C25 C30 109.9(5) . . ? C26 C25 C30 112.3(6) . . ? C25 C26 C27 109.5(7) . . ? C28 C27 C26 111.7(7) . . ? C27 C28 C29 112.4(6) . . ? C30 C29 C28 108.6(6) . . ? N4 C30 C25 109.3(5) . . ? N4 C30 C29 115.4(6) . . ? C25 C30 C29 112.1(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.401 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.064 data_[Cu2L3(OAc)]ClO4CH3CN #2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H40 Cl Cu2 N5 O8' _chemical_formula_weight 809.24 _chemical_melting_point ? _chemical_compound_source 'Hodgson (MSU) 1996' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.042(11) _cell_length_b 19.769(9) _cell_length_c 12.477(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.56(5) _cell_angle_gamma 90.00 _cell_volume 3728.5(36) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description 'flat, prismatic' _exptl_crystal_colour 'brown (transmission), black (reflectance)' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas na _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method na _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min na _exptl_absorpt_correction_T_max na _exptl_special_details ; crystal mounted on fine glass fibre; crystals lost solvent (acetonitrile and/or water) over the course of the data collection. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'scintillation counter, PH analysis' _diffrn_measurement_method 'omega scans, 2.0 deg' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time 1.5h _diffrn_standards_decay_% ' mean -10.3 (min -39.4; max +3.9), solvent loss' _diffrn_reflns_number 6341 _diffrn_reflns_av_R_equivalents 0.1821 _diffrn_reflns_av_sigmaI/netI 0.1734 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5227 _reflns_number_observed 2226 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3 (Siemens Analytical Xray Inc.)' _computing_cell_refinement 'P3 (Siemens Analytical Xray Inc.)' _computing_data_reduction 'XDISK (Siemens Analytical Xray Inc.)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP (Siemens Analytical Xray Inc.)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Disorder in the cyclohexyl rings (carbons and hydrogens) was modelled with the major conformers contributing 0.56(5) and 0.53(4). U(iso) for H's was assigned as 1.2 times U(eq) of the attached atom. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated, fixed, riding' _refine_ls_extinction_method none _refine_ls_extinction_coef na _refine_ls_number_reflns 5225 _refine_ls_number_parameters 528 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.2134 _refine_ls_R_factor_obs 0.0835 _refine_ls_wR_factor_all 0.2157 _refine_ls_wR_factor_obs 0.1809 _refine_ls_goodness_of_fit_all 1.221 _refine_ls_goodness_of_fit_obs 1.742 _refine_ls_restrained_S_all 1.246 _refine_ls_restrained_S_obs 1.689 _refine_ls_shift/esd_max 0.020 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.29424(9) 0.48433(6) 0.03319(12) 0.0622(5) Uani 1 d . . Cu2 Cu 0.25192(9) 0.34320(6) 0.03407(13) 0.0642(5) Uani 1 d . . O1 O 0.3614(5) 0.3478(4) 0.1918(7) 0.091(3) Uani 1 d . . O2 O 0.3998(5) 0.4554(4) 0.1858(7) 0.088(3) Uani 1 d . . O3 O 0.2102(5) 0.4285(3) 0.0702(7) 0.081(3) Uani 1 d . . O4 O 0.3047(5) 0.4031(3) -0.0459(7) 0.077(3) Uani 1 d . . N1 N 0.2399(6) 0.5641(4) 0.0601(8) 0.060(3) Uani 1 d . . N2 N 0.1600(6) 0.2946(4) 0.0646(7) 0.059(2) Uani 1 d . . N3 N 0.2690(6) 0.2668(4) -0.0479(8) 0.056(2) Uani 1 d . . N4 N 0.3520(6) 0.5362(4) -0.0487(8) 0.061(3) Uani 1 d . . Cl1 Cl 0.0780(3) 0.7669(2) -0.2732(4) 0.1009(12) Uani 1 d . . O1A O 0.0066(11) 0.7819(8) -0.2470(15) 0.288(11) Uani 1 d . . O2A O 0.1488(7) 0.8118(5) -0.2267(9) 0.150(4) Uani 1 d . . O3A O 0.1018(10) 0.7006(6) -0.2582(13) 0.235(7) Uani 1 d . . O4A O 0.0576(7) 0.7782(6) -0.3878(11) 0.168(5) Uani 1 d . . C1 C 0.4096(8) 0.3980(6) 0.2296(10) 0.076(4) Uani 1 d . . C2 C 0.4851(9) 0.3913(7) 0.3445(13) 0.153(7) Uani 1 d . . H2A H 0.4875(9) 0.3456(7) 0.3714(13) 0.183 Uiso 1 calc R . H2B H 0.4746(9) 0.4215(7) 0.3989(13) 0.183 Uiso 1 calc R . H2C H 0.5403(9) 0.4026(7) 0.3347(13) 0.183 Uiso 1 calc R . C3 C 0.1433(7) 0.4432(5) 0.1026(9) 0.052(3) Uani 1 d . . C4 C 0.1256(7) 0.5105(5) 0.1183(9) 0.052(3) Uani 1 d . . C5 C 0.0553(7) 0.5261(5) 0.1561(8) 0.056(3) Uani 1 d . . H5A H 0.0444(7) 0.5711(5) 0.1680(8) 0.068 Uiso 1 calc R . C6 C 0.0008(7) 0.4762(6) 0.1766(8) 0.055(3) Uani 1 d . . C7 C 0.0199(7) 0.4097(5) 0.1581(8) 0.055(3) Uani 1 d . . H7A H -0.0156(7) 0.3756(5) 0.1707(8) 0.066 Uiso 1 calc R . C8 C 0.0890(7) 0.3921(5) 0.1221(8) 0.046(3) Uani 1 d . . C9 C 0.0981(7) 0.3206(5) 0.0960(9) 0.061(3) Uani 1 d . . H9A H 0.0550(7) 0.2911(5) 0.1028(9) 0.074 Uiso 1 calc R . C10 C 0.1718(8) 0.5675(5) 0.0943(9) 0.071(4) Uani 1 d . . H10A H 0.1513(8) 0.6104(5) 0.1040(9) 0.085 Uiso 1 calc R . C11 C -0.0714(7) 0.4933(6) 0.2200(10) 0.090(4) Uani 1 d . . H11A H -0.0746(7) 0.5415(6) 0.2271(10) 0.108 Uiso 1 calc R . H11B H -0.0603(7) 0.4727(6) 0.2931(10) 0.108 Uiso 1 calc R . H11C H -0.1265(7) 0.4769(6) 0.1681(10) 0.108 Uiso 1 calc R . C12 C 0.1961(40) 0.2179(23) 0.0675(38) 0.064(15) Uani 0.44(5) d PU 1 H12A H 0.2544(40) 0.2079(23) 0.1233(38) 0.077 Uiso 0.44(5) calc PR 1 C14 C 0.1590(40) 0.0959(19) 0.0638(43) 0.072(15) Uani 0.44(5) d PU 1 H14A H 0.2169(40) 0.0924(19) 0.1219(43) 0.086 Uiso 0.44(5) calc PR 1 H14B H 0.1214(40) 0.0606(19) 0.0766(43) 0.086 Uiso 0.44(5) calc PR 1 C15 C 0.1670(40) 0.0884(27) -0.0575(49) 0.057(16) Uani 0.44(5) d PU 1 H15A H 0.1865(40) 0.0432(27) -0.0681(49) 0.068 Uiso 0.44(5) calc PR 1 H15B H 0.1105(40) 0.0970(27) -0.1161(49) 0.068 Uiso 0.44(5) calc PR 1 C17 C 0.1871(43) 0.2113(25) -0.0538(53) 0.077(17) Uani 0.44(5) d PU 1 H17A H 0.1287(43) 0.2201(25) -0.1099(53) 0.092 Uiso 0.44(5) calc PR 1 C13 C 0.1160(7) 0.1703(5) 0.0689(10) 0.069(3) Uani 1 d U . H13A H 0.0635(7) 0.1782(5) 0.0032(10) 0.083 Uiso 0.44(5) calc PR 1 H13B H 0.1016(7) 0.1762(5) 0.1379(10) 0.083 Uiso 0.44(5) calc PR 1 H13C H 0.0568(7) 0.1822(5) 0.0668(10) 0.083 Uiso 0.56(5) calc PR 2 H13D H 0.1528(7) 0.1662(5) 0.1480(10) 0.083 Uiso 0.56(5) calc PR 2 C16 C 0.2335(8) 0.1395(5) -0.0626(10) 0.079(4) Uani 1 d U . H16A H 0.2456(8) 0.1361(5) -0.1335(10) 0.095 Uiso 0.44(5) calc PR 1 H16B H 0.2884(8) 0.1338(5) 0.0003(10) 0.095 Uiso 0.44(5) calc PR 1 H16C H 0.2019(8) 0.1401(5) -0.1438(10) 0.095 Uiso 0.56(5) calc PR 2 H16D H 0.2946(8) 0.1281(5) -0.0518(10) 0.095 Uiso 0.56(5) calc PR 2 C12A C 0.1505(25) 0.2244(15) 0.0166(45) 0.057(11) Uani 0.56(5) d PU 2 H12B H 0.1035(108) 0.2300(86) -0.0571(149) 0.069 Uiso 0.56 calc P 2 C14A C 0.1127(25) 0.1019(15) 0.0098(41) 0.080(12) Uani 0.56(5) d PU 2 H14C H 0.1007(25) 0.0667(15) 0.0568(41) 0.096 Uiso 0.56(5) calc PR 2 H14D H 0.0642(25) 0.1023(15) -0.0620(41) 0.096 Uiso 0.56(5) calc PR 2 C15A C 0.1959(32) 0.0849(25) -0.0123(37) 0.068(14) Uani 0.56(5) d PU 2 H15C H 0.2399(32) 0.0715(25) 0.0590(37) 0.081 Uiso 0.56(5) calc PR 2 H15D H 0.1846(32) 0.0462(25) -0.0629(37) 0.081 Uiso 0.56(5) calc PR 2 C17A C 0.2316(25) 0.2087(16) -0.0183(38) 0.051(10) Uani 0.56(5) d PU 2 H17B H 0.2747(25) 0.2020(16) 0.0579(38) 0.061 Uiso 0.56(5) calc PR 2 C18 C 0.3513(7) 0.3916(5) -0.1105(9) 0.052(3) Uani 1 d . . C19 C 0.3566(6) 0.3235(5) -0.1489(9) 0.047(3) Uani 1 d . . C20 C 0.4048(7) 0.3131(5) -0.2247(9) 0.060(3) Uani 1 d . . H20A H 0.4080(7) 0.2696(5) -0.2512(9) 0.072 Uiso 1 calc R . C21 C 0.4460(7) 0.3639(6) -0.2598(9) 0.061(3) Uani 1 d . . C22 C 0.4390(7) 0.4298(5) -0.2215(10) 0.061(3) Uani 1 d . . H22A H 0.4664(7) 0.4651(5) -0.2460(10) 0.073 Uiso 1 calc R . C23 C 0.3924(7) 0.4438(5) -0.1482(9) 0.048(3) Uani 1 d . . C24 C 0.3113(7) 0.2652(5) -0.1202(10) 0.056(3) Uani 1 d . . H24A H 0.3131(7) 0.2243(5) -0.1562(10) 0.067 Uiso 1 calc R . C25 C 0.4972(8) 0.3494(6) -0.3422(10) 0.099(4) Uani 1 d . . H25A H 0.5220(8) 0.3907(6) -0.3584(10) 0.119 Uiso 1 calc R . H25B H 0.4575(8) 0.3307(6) -0.4116(10) 0.119 Uiso 1 calc R . H25C H 0.5438(8) 0.3177(6) -0.3079(10) 0.119 Uiso 1 calc R . C26 C 0.3896(7) 0.5141(6) -0.1195(11) 0.069(3) Uani 1 d . . H26A H 0.4162(7) 0.5454(6) -0.1535(11) 0.083 Uiso 1 calc R . C27 C 0.3639(30) 0.6076(18) 0.0056(44) 0.053(12) Uani 0.47(4) d PU 1 H27A H 0.4029(30) 0.6068(18) 0.0851(44) 0.064 Uiso 0.47(4) calc PR 1 C29 C 0.3991(30) 0.7256(22) 0.0014(44) 0.087(16) Uani 0.47(4) d PU 1 H29A H 0.4221(30) 0.7612(22) -0.0343(44) 0.104 Uiso 0.47(4) calc PR 1 H29B H 0.4388(30) 0.7201(22) 0.0789(44) 0.104 Uiso 0.47(4) calc PR 1 C30 C 0.3040(25) 0.7445(17) 0.0007(38) 0.038(10) Uani 0.47(4) d PU 1 H30A H 0.3065(25) 0.7879(17) 0.0378(38) 0.046 Uiso 0.47(4) calc PR 1 H30B H 0.2652(25) 0.7491(17) -0.0775(38) 0.046 Uiso 0.47(4) calc PR 1 C32 C 0.2640(30) 0.6224(17) -0.0052(44) 0.047(10) Uani 0.47(4) d PU 1 H32A H 0.2250(30) 0.6243(17) -0.0846(44) 0.057 Uiso 0.47(4) calc PR 1 C28 C 0.3923(7) 0.6607(5) -0.0632(10) 0.066(3) Uani 1 d U . H28A H 0.4490(7) 0.6489(5) -0.0702(10) 0.079 Uiso 0.47(4) calc PR 1 H28B H 0.3490(7) 0.6647(5) -0.1388(10) 0.079 Uiso 0.47(4) calc PR 1 H28C H 0.3972(7) 0.6559(5) -0.1383(10) 0.079 Uiso 0.53(4) calc PR 2 H28D H 0.4499(7) 0.6520(5) -0.0069(10) 0.079 Uiso 0.53(4) calc PR 2 C31 C 0.2652(7) 0.6926(5) 0.0599(10) 0.077(4) Uani 1 d U . H31A H 0.2057(7) 0..7054(5) 0.0552(10) 0.093 Uiso 0.47(4) calc PR 1 H31B H 0.3012(7) 0.6887(5) 0.1394(10) 0.093 Uiso 0.47(4) calc PR 1 H31C H 0.2487(7) 0.6983(5) 0.1275(10) 0.093 Uiso 0.53(4) calc PR 2 H31D H 0.2128(7) 0.6991(5) -0.0064(10) 0.093 Uiso 0.53(4) calc PR 2 C27A C 0.3229(30) 0.6102(15) -0.0481(36) 0.046(10) Uani 0.53(4) d PU 2 H27B H 0.2682(30) 0.6163(15) -0.1127(36) 0.056 Uiso 0.53(4) calc PR 2 C29A C 0.3605(30) 0.7332(14) -0.0477(36) 0.061(11) Uani 0.53(4) d PU 2 H29C H 0.4065(30) 0.7650(14) -0.0483(36) 0.073 Uiso 0.53(4) calc PR 2 H29D H 0.3087(30) 0.7435(14) -0.1129(36) 0.073 Uiso 0.53(4) calc PR 2 C30A C 0.3377(29) 0.7451(19) 0.0598(40) 0.075(13) Uani 0.53(4) d PU 2 H30C H 0.3157(29) 0.7908(19) 0.0604(40) 0.090 Uiso 0.53(4) calc PR 2 H30D H 0.3898(29) 0.7391(19) 0.1266(40) 0.090 Uiso 0.53(4) calc PR 2 C32A C 0.3021(27) 0.6237(15) 0.0582(41) 0.051(10) Uani 0.53(4) d PU 2 H32B H 0.3567(27) 0.6193(15) 0.1235(41) 0.062 Uiso 0.53(4) calc PR 2 C1S C 0.1315(11) 0.6131(7) -0.4909(15) 0.142(6) Uani 1 d . . H1SA H 0.0822(11) 0.5900(7) -0.4803(15) 0.171 Uiso 1 d R . H1SB H 0.1263(11) 0.6609(7) -0.4806(15) 0.171 Uiso 1 d R . H1SD H 0.1322(11) 0.6045(7) -0.5664(15) 0.171 Uiso 1 d R . C2S C 0.2088(15) 0.5896(9) -0.4140(18) 0.129(6) Uani 1 d . . N1S N 0.2743(14) 0.5736(9) -0.3512(18) 0.232(11) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0829(10) 0.0312(7) 0.0904(12) 0.0032(8) 0.0526(9) 0.0007(7) Cu2 0.0806(10) 0.0347(7) 0.0934(12) -0.0058(8) 0.0508(9) -0.0080(7) O1 0.105(6) 0.061(5) 0.076(7) 0.027(5) -0.012(5) -0.019(5) O2 0.102(6) 0.060(5) 0.079(7) 0.027(5) -0.003(5) -0.014(5) O3 0.094(6) 0.030(4) 0.154(8) -0.005(4) 0.090(6) -0.008(4) O4 0.133(7) 0.019(4) 0.124(7) -0.011(4) 0.102(6) -0.015(4) N1 0.073(7) 0.025(5) 0.099(8) 0.008(5) 0.052(6) 0.009(5) N2 0.072(7) 0.033(5) 0.079(7) -0.003(5) 0.032(6) -0.016(5) N3 0.070(7) 0.026(5) 0.075(7) -0.001(5) 0.026(6) -0.001(4) N4 0.075(7) 0.032(5) 0.087(8) 0.001(5) 0.041(6) -0.008(4) Cl1 0.128(4) 0.081(3) 0.090(3) 0.006(3) 0.032(3) -0.018(3) O1A 0.246(15) 0.319(21) 0.419(25) -0.191(18) 0.270(18) -0.133(14) O2A 0.148(9) 0.128(9) 0.155(10) 0.019(8) 0.024(8) -0.024(8) O3A 0.315(18) 0.102(10) 0.322(19) 0.068(11) 0.149(15) 0.003(10) O4A 0.176(11) 0.191(12) 0.119(10) 0.004(9) 0.025(9) -0.026(9) C1 0.101(11) 0.057(9) 0.044(9) 0.012(8) -0.011(8) -0.021(8) C2 0.145(14) 0.126(13) 0.134(15) 0.074(11) -0.025(13) -0.059(11) C3 0.064(8) 0.039(7) 0.070(9) 0.003(6) 0.045(7) -0.007(6) C4 0.062(8) 0.039(7) 0.067(9) 0.006(6) 0.038(7) 0.000(6) C5 0.069(8) 0.050(7) 0.049(8) 0.009(6) 0.019(7) -0.001(6) C6 0.056(8) 0.068(8) 0.052(8) -0.005(7) 0.031(7) 0.005(7) C7 0.058(8) 0.059(8) 0.050(8) 0.007(6) 0.022(7) -0.005(6) C8 0.065(8) 0.037(6) 0.044(7) 0.004(5) 0.028(7) 0.007(6) C9 0.059(8) 0.055(8) 0.077(9) 0.018(7) 0.030(7) -0.009(6) C10 0.105(10) 0.037(7) 0.087(10) -0.007(6) 0.054(9) 0.021(7) C11 0.087(9) 0.092(9) 0.107(11) -0.022(8) 0.055(9) -0.016(7) C12 0.081(29) 0.057(20) 0.040(27) -0.008(18) 0.000(21) -0.013(22) C14 0.096(30) 0.034(18) 0.067(29) -0.014(20) 0.003(23) -0.048(21) C15 0.065(28) 0.036(19) 0.059(35) -0.024(24) 0.008(25) -0.016(19) C17 0.059(28) 0.054(21) 0.115(35) 0.019(22) 0.025(26) -0.040(23) C13 0.076(8) 0.063(8) 0.064(8) 0.011(7) 0.016(7) -0.013(7) C16 0.125(11) 0.040(7) 0.081(10) -0.020(7) 0.048(9) -0.013(7) C12A 0.058(22) 0.039(14) 0.091(28) 0.001(19) 0.045(20) -0.018(16) C14A 0.081(23) 0.028(12) 0.100(27) -0.021(16) -0.012(20) -0.019(15) C15A 0.104(31) 0.065(18) 0.022(23) 0.010(18) 0.005(20) -0.002(20) C17A 0.033(17) 0.035(13) 0.083(24) -0.031(15) 0.017(17) -0.018(14) C18 0.072(8) 0.040(7) 0.057(8) -0.011(6) 0.041(7) 0.000(6) C19 0.043(7) 0.054(8) 0.043(8) 0.005(6) 0.012(6) 0.005(6) C20 0.063(8) 0.051(8) 0.058(9) -0.019(7) 0.008(7) 0.010(6) C21 0.064(8) 0.060(8) 0.063(9) 0.006(7) 0.026(7) -0.006(6) C22 0.059(8) 0.054(8) 0.069(9) -0.006(7) 0.022(8) -0.009(6) C23 0.053(7) 0.052(8) 0.044(8) -0.005(7) 0.023(7) 0.001(6) C24 0.065(8) 0.039(7) 0.065(9) -0.011(6) 0.023(7) 0.012(6) C25 0.119(11) 0.098(10) 0.111(11) -0.039(9) 0.077(10) -0.007(8) C26 0.082(9) 0.046(7) 0.095(10) 0.009(7) 0.050(8) -0.004(7) C27 0.051(22) 0.044(15) 0.057(23) -0.011(18) 0.007(17) -0.023(16) C29 0.096(27) 0.081(22) 0.077(26) 0.007(19) 0.020(20) 0.003(19) C30 0.045(19) 0.027(13) 0.043(21) 0.000(16) 0.014(16) -0.003(14) C32 0.057(21) 0.036(14) 0.053(22) 0.009(17) 0.022(17) 0.006(15) C28 0.074(8) 0.043(6) 0.091(9) 0.004(7) 0.042(7) -0.009(6) C31 0.103(9) 0.035(6) 0.116(11) -0.009(7) 0.067(8) 0.001(6) C27A 0.056(20) 0.026(12) 0.053(21) -0.009(15) 0.013(16) -0.011(14) C29A 0.078(22) 0.030(13) 0.085(24) 0.021(15) 0.042(19) -0.021(14) C30A 0.080(23) 0.049(14) 0.081(25) -0.001(19) 0.009(18) -0.025(16) C32A 0.055(19) 0.033(13) 0.065(23) 0.017(16) 0.019(16) 0.010(13) C1S 0.138(15) 0.130(14) 0.166(18) 0.017(13) 0.060(14) 0.041(12) C2S 0.135(19) 0.098(13) 0.138(21) 0.014(13) 0.026(16) -0.013(13) N1S 0.234(23) 0.149(15) 0.206(22) 0.027(13) -0.069(16) -0.005(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.886(8) . ? Cu1 N4 1.895(8) . ? Cu1 O3 1.915(7) . ? Cu1 O4 1.922(7) . ? Cu1 O2 2.159(8) . ? Cu1 Cu2 2.872(2) . ? Cu2 N3 1.894(8) . ? Cu2 N2 1.902(8) . ? Cu2 O4 1.918(7) . ? Cu2 O3 1.922(7) . ? Cu2 O1 2.156(8) . ? O1 C1 1.250(11) . ? O2 C1 1.245(11) . ? O3 C3 1.301(11) . ? O4 C18 1.290(11) . ? N1 C10 1.302(12) . ? N1 C32 1.53(4) . ? N1 C32A 1.55(3) . ? N2 C9 1.290(11) . ? N2 C12A 1.50(3) . ? N2 C12 1.62(5) . ? N3 C24 1.298(11) . ? N3 C17A 1.40(3) . ? N3 C17 1.69(5) . ? N4 C26 1.301(12) . ? N4 C27A 1.54(3) . ? N4 C27 1.55(4) . ? Cl1 O1A 1.325(13) . ? Cl1 O3A 1.361(12) . ? Cl1 O4A 1.375(11) . ? Cl1 O2A 1.405(10) . ? C1 C2 1.542(15) . ? C3 C4 1.386(12) . ? C3 C8 1.408(12) . ? C4 C5 1.395(12) . ? C4 C10 1.435(13) . ? C5 C6 1.396(13) . ? C6 C7 1.386(13) . ? C6 C11 1.474(12) . ? C7 C8 1.374(12) . ? C8 C9 1.469(13) . ? C12 C13 1.60(5) . ? C12 C17 1.48(8) . ? C14 C15 1.57(8) . ? C14 C13 1.63(5) . ? C15 C16 1.48(6) . ? C17 C16 1.62(6) . ? C13 C12A 1.46(3) . ? C13 C14A 1.53(3) . ? C16 C15A 1.47(5) . ? C16 C17A 1.48(3) . ? C12A C17A 1.54(6) . ? C14A C15A 1.49(7) . ? C18 C23 1.389(13) . ? C18 C19 1.440(13) . ? C19 C20 1.421(13) . ? C19 C24 1.470(13) . ? C20 C21 1.353(13) . ? C21 C22 1.405(13) . ? C21 C25 1.541(13) . ? C22 C23 1.390(13) . ? C23 C26 1.439(13) . ? C27 C28 1.52(4) . ? C27 C32 1.59(7) . ? C29 C28 1.50(4) . ? C29 C30 1.57(6) . ? C30 C31 1.51(3) . ? C32 C31 1.60(4) . ? C28 C27A 1.55(3) . ? C28 C29A 1.56(4) . ? C31 C32A 1.49(3) . ? C31 C30A 1.56(3) . ? C27A C32A 1.50(6) . ? C29A C30A 1.52(6) . ? C1S C2S 1.37(2) . ? C2S N1S 1.12(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 N1 Cu1 N4 88.9(4) . . ? N1 Cu1 O3 92.0(3) . . ? N4 Cu1 O3 162.4(4) . . ? N1 Cu1 O4 156.3(4) . . ? N4 Cu1 O4 91.9(4) . . ? O3 Cu1 O4 80.3(3) . . ? N1 Cu1 O2 109.7(3) . . ? N4 Cu1 O2 103.8(3) . . ? O3 Cu1 O2 92.4(3) . . ? O4 Cu1 O2 93.1(3) . . ? N1 Cu1 Cu2 133.5(3) . . ? N4 Cu1 Cu2 133.4(3) . . ? O3 Cu1 Cu2 41.6(2) . . ? O4 Cu1 Cu2 41.5(2) . . ? O2 Cu1 Cu2 81.7(2) . . ? N3 Cu2 N2 88.2(4) . . ? N3 Cu2 O4 92.4(4) . . ? N2 Cu2 O4 157.3(4) . . ? N3 Cu2 O3 161.9(4) . . ? N2 Cu2 O3 92.4(4) . . ? O4 Cu2 O3 80.2(3) . . ? N3 Cu2 O1 107.8(3) . . ? N2 Cu2 O1 106.7(3) . . ? O4 Cu2 O1 94.7(3) . . ? O3 Cu2 O1 89.4(3) . . ? N3 Cu2 Cu1 134.0(3) . . ? N2 Cu2 Cu1 133.7(3) . . ? O4 Cu2 Cu1 41.6(2) . . ? O3 Cu2 Cu1 41.4(2) . . ? O1 Cu2 Cu1 80.9(2) . . ? C1 O1 Cu2 126.1(7) . . ? C1 O2 Cu1 125.1(7) . . ? C3 O3 Cu1 131.8(6) . . ? C3 O3 Cu2 131.1(6) . . ? Cu1 O3 Cu2 97.0(3) . . ? C18 O4 Cu2 131.7(6) . . ? C18 O4 Cu1 129.6(6) . . ? Cu2 O4 Cu1 96.8(3) . . ? C10 N1 C32 121.6(16) . . ? C10 N1 C32A 125.6(14) . . ? C10 N1 Cu1 126.2(7) . . ? C32 N1 Cu1 108.7(14) . . ? C32A N1 Cu1 107.2(12) . . ? C9 N2 C12A 120.3(15) . . ? C9 N2 C12 132.2(21) . . ? C9 N2 Cu2 126.0(7) . . ? C12A N2 Cu2 111.7(14) . . ? C12 N2 Cu2 100.5(21) . . ? C24 N3 C17A 122.1(16) . . ? C24 N3 C17 122.1(22) . . ? C24 N3 Cu2 126.8(7) . . ? C17A N3 Cu2 111.0(15) . . ? C17 N3 Cu2 106.8(22) . . ? C26 N4 C27A 122.3(15) . . ? C26 N4 C27 125.9(16) . . ? C26 N4 Cu1 127.3(7) . . ? C27A N4 Cu1 108.0(13) . . ? C27 N4 Cu1 105.6(15) . . ? O1A Cl1 O3A 114.0(10) . . ? O1A Cl1 O4A 107.3(10) . . ? O3A Cl1 O4A 104.9(9) . . ? O1A Cl1 O2A 113.8(8) . . ? O3A Cl1 O2A 113.6(8) . . ? O4A Cl1 O2A 101.8(7) . . ? O2 C1 O1 125.9(11) . . ? O2 C1 C2 115.6(10) . . ? O1 C1 C2 118.4(11) . . ? O3 C3 C4 119.2(9) . . ? O3 C3 C8 121.0(9) . . ? C4 C3 C8 119.7(10) . . ? C3 C4 C5 119.1(10) . . ? C3 C4 C10 125.5(10) . . ? C5 C4 C10 115.4(10) . . ? C4 C5 C6 122.2(10) . . ? C7 C6 C5 116.9(9) . . ? C7 C6 C11 121.5(10) . . ? C5 C6 C11 121.6(10) . . ? C8 C7 C6 122.8(10) . . ? C7 C8 C3 119.3(9) . . ? C7 C8 C9 117.9(10) . . ? C3 C8 C9 122.6(9) . . ? N2 C9 C8 126.4(9) . . ? N1 C10 C4 125.2(9) . . ? C13 C12 C17 99.0(39) . . ? C13 C12 N2 105.6(36) . . ? C17 C12 N2 98.5(38) . . ? C15 C14 C13 107.1(40) . . ? C16 C15 C14 105..6(37) . . ? C12 C17 C16 104.8(45) . . ? C12 C17 N3 95.2(40) . . ? C16 C17 N3 101.8(36) . . ? C12A C13 C14A 112.9(23) . . ? C12 C13 C14 100.2(29) . . ? C15A C16 C17A 117.1(25) . . ? C15 C16 C17 103.9(31) . . ? C13 C12A C17A 117.6(27) . . ? C13 C12A N2 120.3(30) . . ? C17A C12A N2 108.6(24) . . ? C15A C14A C13 113.6(32) . . ? C16 C15A C14A 115.7(35) . . ? N3 C17A C16 126.6(26) . . ? N3 C17A C12A 112.7(24) . . ? C16 C17A C12A 114.7(26) . . ? O4 C18 C23 121.4(9) . . ? O4 C18 C19 119.0(10) . . ? C23 C18 C19 119.6(10) . . ? C20 C19 C18 117.5(10) . . ? C20 C19 C24 118.2(10) . . ? C18 C19 C24 124.2(10) . . ? C21 C20 C19 122.8(10) . . ? C20 C21 C22 118.3(10) . . ? C20 C21 C25 120.4(11) . . ? C22 C21 C25 121.3(10) . . ? C23 C22 C21 122.0(10) . . ? C22 C23 C18 119.7(10) . . ? C22 C23 C26 115.1(11) . . ? C18 C23 C26 125.1(10) . . ? N3 C24 C19 124.5(9) . . ? N4 C26 C23 123.6(10) . . ? C28 C27 N4 113.5(28) . . ? C28 C27 C32 108.0(36) . . ? N4 C27 C32 99.1(30) . . ? C28 C29 C30 107.8(34) . . ? C31 C30 C29 113.3(30) . . ? N1 C32 C27 104.0(32) . . ? N1 C32 C31 110.1(26) . . ? C27 C32 C31 106.0(33) . . ? C29 C28 C27 105.6(26) . . ? C27A C28 C29A 107.4(19) . . ? C32A C31 C30A 107.9(22) . . ? C30 C31 C32 106.0(21) . . ? C32A C27A N4 109.4(27) . . ? C32A C27A C28 112.0(31) . . ? N4 C27A C28 112.3(24) . . ? C30A C29A C28 115.9(30) . . ? C29A C30A C31 107.3(31) . . ? C31 C32A C27A 112.6(31) . . ? C31 C32A N1 115.7(22) . . ? C27A C32A N1 102.3(31) . . ? N1S C2S C1S 176.2(22) . . ? 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 N1 Cu1 Cu2 N3 148.2(5) . . . . ? N4 Cu1 Cu2 N3 -1.2(5) . . . . ? O3 Cu1 Cu2 N3 154.4(5) . . . . ? O4 Cu1 Cu2 N3 1.8(5) . . . . ? O2 Cu1 Cu2 N3 -102.4(4) . . . . ? N1 Cu1 Cu2 N2 -1.4(5) . . . . ? N4 Cu1 Cu2 N2 -150.8(5) . . . . ? O3 Cu1 Cu2 N2 4.9(5) . . . . ? O4 Cu1 Cu2 N2 -147.7(5) . . . . ? O2 Cu1 Cu2 N2 108.0(4) . . . . ? N1 Cu1 Cu2 O4 146.4(5) . . . . ? N4 Cu1 Cu2 O4 -3.1(5) . . . . ? O3 Cu1 Cu2 O4 152.6(5) . . . . ? O4 Cu1 Cu2 O4 0.0 . . . . ? O2 Cu1 Cu2 O4 -104.3(4) . . . . ? N1 Cu1 Cu2 O3 -6.2(5) . . . . ? N4 Cu1 Cu2 O3 -155.7(5) . . . . ? O3 Cu1 Cu2 O3 0.0 . . . . ? O4 Cu1 Cu2 O3 -152.6(5) . . . . ? O2 Cu1 Cu2 O3 103.1(4) . . . . ? N1 Cu1 Cu2 O1 -105.8(5) . . . . ? N4 Cu1 Cu2 O1 104.7(4) . . . . ? O3 Cu1 Cu2 O1 -99.6(4) . . . . ? O4 Cu1 Cu2 O1 107.8(4) . . . . ? O2 Cu1 Cu2 O1 3.5(3) . . . . ? N3 Cu2 O1 C1 128.1(10) . . . . ? N2 Cu2 O1 C1 -138.4(10) . . . . ? O4 Cu2 O1 C1 34.0(11) . . . . ? O3 Cu2 O1 C1 -46.1(11) . . . . ? Cu1 Cu2 O1 C1 -5.3(10) . . . . ? N1 Cu1 O2 C1 129.2(10) . . . . ? N4 Cu1 O2 C1 -136.9(10) . . . . ? O3 Cu1 O2 C1 36.2(10) . . . . ? O4 Cu1 O2 C1 -44.2(10) . . . . ? Cu2 Cu1 O2 C1 -4.1(10) . . . . ? N1 Cu1 O3 C3 -0.8(10) . . . . ? N4 Cu1 O3 C3 -93.7(15) . . . . ? O4 Cu1 O3 C3 -158.3(10) . . . . ? O2 Cu1 O3 C3 109.0(10) . . . . ? Cu2 Cu1 O3 C3 -176.3(12) . . . . ? N1 Cu1 O3 Cu2 175.5(4) . . . . ? N4 Cu1 O3 Cu2 82.7(12) . . . . ? O4 Cu1 O3 Cu2 18.0(3) . . . . ? O2 Cu1 O3 Cu2 -74.7(4) . . . . ? Cu2 Cu1 O3 Cu2 0.0 . . . . ? N3 Cu2 O3 C3 91.3(15) . . . . ? N2 Cu2 O3 C3 -0.1(10) . . . . ? O4 Cu2 O3 C3 158.3(10) . . . . ? O1 Cu2 O3 C3 -106.8(10) . . . . ? Cu1 Cu2 O3 C3 176.4(12) . . . . ? N3 Cu2 O3 Cu1 -85.1(12) . . . . ? N2 Cu2 O3 Cu1 -176.5(4) . . . . ? O4 Cu2 O3 Cu1 -18.1(3) . . . . ? O1 Cu2 O3 Cu1 76.8(4) . . . . ? Cu1 Cu2 O3 Cu1 0.0 . . . . ? N3 Cu2 O4 C18 -13.6(10) . . . . ? N2 Cu2 O4 C18 -104.6(12) . . . . ? O3 Cu2 O4 C18 -176.9(10) . . . . ? O1 Cu2 O4 C18 94.5(10) . . . . ? Cu1 Cu2 O4 C18 165.1(12) . . . . ? N3 Cu2 O4 Cu1 -178.7(4) . . . . ? N2 Cu2 O4 Cu1 90.4(9) . . . . ? O3 Cu2 O4 Cu1 18.0(3) . . . . ? O1 Cu2 O4 Cu1 -70.6(4) . . . . ? Cu1 Cu2 O4 Cu1 0.0 . . . . ? N1 Cu1 O4 C18 103.9(12) . . . . ? N4 Cu1 O4 C18 12.2(10) . . . . ? O3 Cu1 O4 C18 176.4(10) . . . . ? O2 Cu1 O4 C18 -91.7(9) . . . . ? Cu2 Cu1 O4 C18 -165.6(11) . . . . ? N1 Cu1 O4 Cu2 -90.5(9) . . . . ? N4 Cu1 O4 Cu2 177.8(4) . . . . ? O3 Cu1 O4 Cu2 -18.1(3) . . . . ? O2 Cu1 O4 Cu2 73.8(3) . . . . ? Cu2 Cu1 O4 Cu2 0.0 . . . . ? N4 Cu1 N1 C10 164.0(10) . . . . ? O3 Cu1 N1 C10 1.6(10) . . . . ? O4 Cu1 N1 C10 71.7(14) . . . . ? O2 Cu1 N1 C10 -91.7(10) . . . . ? Cu2 Cu1 N1 C10 5.7(12) . . . . ? N4 Cu1 N1 C32 5.1(22) . . . . ? O3 Cu1 N1 C32 -157.3(22) . . . . ? O4 Cu1 N1 C32 -87.2(23) . . . . ? O2 Cu1 N1 C32 109.5(21) . . . . ? Cu2 Cu1 N1 C32 -153.2(21) . . . . ? N4 Cu1 N1 C32A -27.3(20) . . . . ? O3 Cu1 N1 C32A 170.2(20) . . . . ? O4 Cu1 N1 C32A -119.7(20) . . . . ? O2 Cu1 N1 C32A 77.0(20) . . . . ? Cu2 Cu1 N1 C32A 174.3(19) . . . . ? N3 Cu2 N2 C9 -161.1(9) . . . . ? O4 Cu2 N2 C9 -69.3(14) . . . . ? O3 Cu2 N2 C9 0.7(9) . . . . ? O1 Cu2 N2 C9 90.9(9) . . . . ? Cu1 Cu2 N2 C9 -2.5(11) . . . . ? N3 Cu2 N2 C12A 2.4(22) . . . . ? O4 Cu2 N2 C12A 94.2(23) . . . . ? O3 Cu2 N2 C12A 164.2(22) . . . . ? O1 Cu2 N2 C12A -105.6(22) . . . . ? Cu1 Cu2 N2 C12A 161.0(21) . . . . ? N3 Cu2 N2 C12 30.9(17) . . . . ? O4 Cu2 N2 C12 122.7(18) . . . . ? O3 Cu2 N2 C12 -167.3(17) . . . . ? O1 Cu2 N2 C12 -77.1(17) . . . . ? Cu1 Cu2 N2 C12 -170.5(16) . . . . ? N2 Cu2 N3 C24 163.3(9) . . . . ? O4 Cu2 N3 C24 6.0(9) . . . . ? O3 Cu2 N3 C24 71.2(15) . . . . ? O1 Cu2 N3 C24 -89.7(9) . . . . ? Cu1 Cu2 N3 C24 4.8(11) . . . . ? N2 Cu2 N3 C17A -18.6(20) . . . . ? O4 Cu2 N3 C17A -175.9(20) . . . . ? O3 Cu2 N3 C17A -110.7(23) . . . . ? O1 Cu2 N3 C17A 88.3(20) . . . . ? Cu1 Cu2 N3 C17A -177.2(19) . . . . ? N2 Cu2 N3 C17 6.3(23) . . . . ? O4 Cu2 N3 C17 -151.0(22) . . . . ? O3 Cu2 N3 C17 -85.8(26) . . . . ? O1 Cu2 N3 C17 113.3(22) . . . . ? Cu1 Cu2 N3 C17 -152.2(22) . . . . ? N1 Cu1 N4 C26 -162.9(10) . . . . ? O3 Cu1 N4 C26 -69.6(16) . . . . ? O4 Cu1 N4 C26 -6.6(10) . . . . ? O2 Cu1 N4 C26 87.0(10) . . . . ? Cu2 Cu1 N4 C26 -4.6(11) . . . . ? N1 Cu1 N4 C27A -0.5(19) . . . . ? O3 Cu1 N4 C27A 92.8(22) . . . . ? O4 Cu1 N4 C27A 155.8(19) . . . . ? O2 Cu1 N4 C27A -110.5(19) . . . . ? Cu2 Cu1 N4 C27A 157.9(19) . . . . ? N1 Cu1 N4 C27 29.5(20) . . . . ? O3 Cu1 N4 C27 122.9(22) . . . . ? O4 Cu1 N4 C27 -174.1(20) . . . . ? O2 Cu1 N4 C27 -80.5(20) . . . . ? Cu2 Cu1 N4 C27 -172.1(20) . . . . ? Cu1 O2 C1 O1 1.4(19) . . . . ? Cu1 O2 C1 C2 -174.7(9) . . . . ? Cu2 O1 C1 O2 4.1(19) . . . . ? Cu2 O1 C1 C2 -179.8(9) . . . . ? Cu1 O3 C3 C4 -1.9(16) . . . . ? Cu2 O3 C3 C4 -177.0(7) . . . . ? Cu1 O3 C3 C8 178.2(7) . . . . ? Cu2 O3 C3 C8 3.1(16) . . . . ? O3 C3 C4 C5 -178.2(9) . . . . ? C8 C3 C4 C5 1.7(16) . . . . ? O3 C3 C4 C10 4.5(17) . . . . ? C8 C3 C4 C10 -175.6(10) . . . . ? C3 C4 C5 C6 -1.3(16) . . . . ? C10 C4 C5 C6 176.2(9) . . . . ? C4 C5 C6 C7 0.3(15) . . . . ? C4 C5 C6 C11 178.0(9) . . . . ? C5 C6 C7 C8 0.4(15) . . . . ? C11 C6 C7 C8 -177.3(9) . . . . ? C6 C7 C8 C3 0.0(15) . . . . ? C6 C7 C8 C9 -174.8(9) . . . . ? O3 C3 C8 C7 178.9(9) . . . . ? C4 C3 C8 C7 -1.0(16) . . . . ? O3 C3 C8 C9 -6.6(16) . . . . ? C4 C3 C8 C9 173.5(9) . . . . ? C12A N2 C9 C8 -166.6(24) . . . . ? C12 N2 C9 C8 159.6(24) . . . . ? Cu2 N2 C9 C8 -4.4(16) . . . . ? C7 C8 C9 N2 -177.8(10) . . . . ? C3 C8 C9 N2 7.6(17) . . . . ? C32 N1 C10 C4 156.7(24) . . . . ? C32A N1 C10 C4 -166.3(24) . . . . ? Cu1 N1 C10 C4 0.3(17) . . . . ? C3 C4 C10 N1 -3.8(18) . . . . ? C5 C4 C10 N1 178.8(10) . . . . ? C9 N2 C12 C13 23.7(38) . . . . ? C12A N2 C12 C13 -53.5(53) . . . . ? Cu2 N2 C12 C13 -169.4(19) . . . . ? C9 N2 C12 C17 125.6(37) . . . . ? C12A N2 C12 C17 48.3(43) . . . . ? Cu2 N2 C12 C17 -67.6(44) . . . . ? C13 C14 C15 C16 66.3(56) . . . . ? C13 C12 C17 C16 -80.0(50) . . . . ? N2 C12 C17 C16 172.7(19) . . . . ? C13 C12 C17 N3 176.4(21) . . . . ? N2 C12 C17 N3 69.0(46) . . . . ? C24 N3 C17 C12 156.2(33) . . . . ? C17A N3 C17 C12 58.5(68) . . . . ? Cu2 N3 C17 C12 -45.6(47) . . . . ? C24 N3 C17 C16 49.8(38) . . . . ? C17A N3 C17 C16 -47.9(66) . . . . ? Cu2 N3 C17 C16 -151.9(22) . . . . ? C17 C12 C13 C12A -46.9(45) . . . . ? N2 C12 C13 C12A 54.6(53) . . . . ? C17 C12 C13 C14A 47.3(59) . . . . ? N2 C12 C13 C14A 148.8(22) . . . . ? C17 C12 C13 C14 75.2(54) . . . . ? N2 C12 C13 C14 176.7(21) . . . . ? C15 C14 C13 C12A -41.5(57) . . . . ? C15 C14 C13 C14A 52.4(49) . . . . ? C15 C14 C13 C12 -69.3(48) . . . . ? C14 C15 C16 C15A 44.8(81) . . . . ? C14 C15 C16 C17A -43.4(67) . . . . ? C14 C15 C16 C17 -64.7(61) . . . . ? C12 C17 C16 C15A 52.8(58) . . . . ? N3 C17 C16 C15A 151.5(23) . . . . ? C12 C17 C16 C17A -57.4(68) . . . . ? N3 C17 C16 C17A 41.2(56) . . . . ? C12 C17 C16 C15 76.5(59) . . . . ? N3 C17 C16 C15 175.1(26) . . . . ? C14A C13 C12A C17A -42.6(62) . . . . ? C12 C13 C12A C17A 56.7(48) . . . . ? C14 C13 C12A C17A -9.8(67) . . . . ? C14A C13 C12A N2 -178.8(21) . . . . ? C12 C13 C12A N2 -79.5(72) . . . . ? C14 C13 C12A N2 -146.0(22) . . . . ? C9 N2 C12A C13 -43.0(43) . . . . ? C12 N2 C12A C13 80.2(75) . . . . ? Cu2 N2 C12A C13 152.4(25) . . . . ? C9 N2 C12A C17A 177.3(30) . . . . ? C12 N2 C12A C17A -59.5(48) . . . . ? Cu2 N2 C12A C17A 12.7(47) . . . . ? C12A C13 C14A C15A 47.3(55) . . . . ? C12 C13 C14A C15A 14.4(56) . . . . ? C14 C13 C14A C15A -52.4(45) . . . . ? C17A C16 C15A C14A 40.8(59) . . . . ? C15 C16 C15A C14A -63.9(88) . . . . ? C17 C16 C15A C14A 13.7(62) . . . . ? C13 C14A C15A C16 -46.6(60) . . . . ? C24 N3 C17A C16 -0.3(48) . . . . ? C17 N3 C17A C16 97.3(96) . . . . ? Cu2 N3 C17A C16 -178.5(29) . . . . ? C24 N3 C17A C12A -151.5(33) . . . . ? C17 N3 C17A C12A -53.8(70) . . . . ? Cu2 N3 C17A C12A 30.3(48) . . . . ? C15A C16 C17A N3 175.2(28) . . . . ? C15 C16 C17A N3 -158.2(29) . . . . ? C17 C16 C17A N3 -103.9(93) . . . . ? C15A C16 C17A C12A -34.2(61) . . . . ? C15 C16 C17A C12A -7.6(69) . . . . ? C17 C16 C17A C12A 46.7(61) . . . . ? C13 C12A C17A N3 -168.9(22) . . . . ? N2 C12A C17A N3 -28.0(61) . . . . ? C13 C12A C17A C16 36.3(68) . . . . ? N2 C12A C17A C16 177.3(20) . . . . ? Cu2 O4 C18 C23 -171.7(7) . . . . ? Cu1 O4 C18 C23 -11.1(16) . . . . ? Cu2 O4 C18 C19 11.7(15) . . . . ? Cu1 O4 C18 C19 172.3(7) . . . . ? O4 C18 C19 C20 176.9(9) . . . . ? C23 C18 C19 C20 0.2(14) . . . . ? O4 C18 C19 C24 0.6(15) . . . . ? C23 C18 C19 C24 -176.1(9) . . . . ? C18 C19 C20 C21 1.0(15) . . . . ? C24 C19 C20 C21 177.5(9) . . . . ? C19 C20 C21 C22 -1.5(15) . . . . ? C19 C20 C21 C25 -179.9(9) . . . . ? C20 C21 C22 C23 0.9(16) . . . . ? C25 C21 C22 C23 179.3(10) . . . . ? C21 C22 C23 C18 0.2(16) . . . . ? C21 C22 C23 C26 -178.4(10) . . . . ? O4 C18 C23 C22 -177.3(10) . . . . ? C19 C18 C23 C22 -0.7(15) . . . . ? O4 C18 C23 C26 1.1(17) . . . . ? C19 C18 C23 C26 177.7(9) . . . . ? C17A N3 C24 C19 -175.9(22) . . . . ? C17 N3 C24 C19 155.7(26) . . . . ? Cu2 N3 C24 C19 1.9(15) . . . . ? C20 C19 C24 N3 176.3(9) . . . . ? C18 C19 C24 N3 -7.4(16) . . . . ? C27A N4 C26 C23 -159.6(22) . . . . ? C27 N4 C26 C23 165.7(25) . . . . ? Cu1 N4 C26 C23 0.6(16) . . . . ? C22 C23 C26 N4 -177.3(10) . . . . ? C18 C23 C26 N4 4.2(18) . . . . ? C26 N4 C27 C28 23.9(43) . . . . ? C27A N4 C27 C28 -69.2(52) . . . . ? Cu1 N4 C27 C28 -168.4(24) . . . . ? C26 N4 C27 C32 138.1(24) . . . . ? C27A N4 C27 C32 45.1(43) . . . . ? Cu1 N4 C27 C32 -54.1(37) . . . . ? C28 C29 C30 C31 62.4(54) . . . . ? C10 N1 C32 C27 162.5(25) . . . . ? C32A N1 C32 C27 54.9(45) . . . . ? Cu1 N1 C32 C27 -37.4(40) . . . . ? C10 N1 C32 C31 49.3(38) . . . . ? C32A N1 C32 C31 -58.3(40) . . . . ? Cu1 N1 C32 C31 -150.7(20) . . . . ? C28 C27 C32 N1 176.5(19) . . . . ? N4 C27 C32 N1 58.1(43) . . . . ? C28 C27 C32 C31 -67.4(47) . . . . ? N4 C27 C32 C31 174.2(18) . . . . ? C30 C29 C28 C27 -64.8(52) . . . . ? C30 C29 C28 C27A -35.4(55) . . . . ? C30 C29 C28 C29A 45.6(45) . . . . ? N4 C27 C28 C29 179.3(21) . . . . ? C32 C27 C28 C29 70.5(52) . . . . ? N4 C27 C28 C27A 67.2(48) . . . . ? C32 C27 C28 C27A -41.6(44) . . . . ? N4 C27 C28 C29A 151.3(21) . . . . ? C32 C27 C28 C29A 42.5(55) . . . . ? C29 C30 C31 C32A -26.5(59) . . . . ? C29 C30 C31 C30A 59.9(48) . . . . ? C29 C30 C31 C32 -58.2(54) . . . . ? N1 C32 C31 C32A 63.7(42) . . . . ? C27 C32 C31 C32A -48.3(43) . . . . ? N1 C32 C31 C30 170.8(18) . . . . ? C27 C32 C31 C30 58.9(50) . . . . ? N1 C32 C31 C30A 142.7(20) . . . . ? C27 C32 C31 C30A 30.8(58) . . . . ? C26 N4 C27A C32A -166.8(29) . . . . ? C27 N4 C27A C32A -60.0(49) . . . . ? Cu1 N4 C27A C32A 29.7(44) . . . . ? C26 N4 C27A C28 -41.7(37) . . . . ? C27 N4 C27A C28 65.1(49) . . . . ? Cu1 N4 C27A C28 154.8(20) . . . . ? C29 C28 C27A C32A -21.7(59) . . . . ? C27 C28 C27A C32A 56.5(50) . . . . ? C29A C28 C27A C32A -50.2(53) . . . . ? C29 C28 C27A N4 -145.4(21) . . . . ? C27 C28 C27A N4 -67.2(49) . . . . ? C29A C28 C27A N4 -173.8(20) . . . . ? C29 C28 C29A C30A -57.6(56) . . . . ? C27 C28 C29A C30A 21.4(61) . . . . ? C27A C28 C29A C30A 51.7(56) . . . . ? C28 C29A C30A C31 -57.0(56) . . . . ? C32A C31 C30A C29A 59.5(56) . . . . ? C30 C31 C30A C29A -44.5(43) . . . . ? C32 C31 C30A C29A 27.9(61) . . . . ? C30 C31 C32A C27A -33.9(60) . . . . ? C30A C31 C32A C27A -63.8(58) . . . . ? C32 C31 C32A C27A 49.7(46) . . . . ? C30 C31 C32A N1 -151.1(19) . . . . ? C30A C31 C32A N1 179.0(19) . . . . ? C32 C31 C32A N1 -67.6(45) . . . . ? N4 C27A C32A C31 -174.5(16) . . . . ? C28 C27A C32A C31 60.2(55) . . . . ? N4 C27A C32A N1 -49.6(47) . . . . ? C28 C27A C32A N1 -174.8(17) . . . . ? C10 N1 C32A C31 -20.4(44) . . . . ? C32 N1 C32A C31 73.0(45) . . . . ? Cu1 N1 C32A C31 170.9(25) . . . . ? C10 N1 C32A C27A -143.2(24) . . . . ? C32 N1 C32A C27A -49.9(45) . . . . ? Cu1 N1 C32A C27A 48.0(38) . . . . ? _refine_diff_density_max 0.476 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.090 data_[Ni2L3](ClO4)2CH3CNCH3OH #3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 Cl2 N5 Ni2 O11' _chemical_formula_weight 871.02 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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.00(3) _cell_length_b 19.014(4) _cell_length_c 11.518(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.33(12) _cell_angle_gamma 90.00 _cell_volume 1892(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour range _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf-Nonius MACH3 ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3419 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3419 _reflns_number_gt 2887 _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 w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+1.3140P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 3419 _refine_ls_number_parameters 477 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 1.471 _refine_ls_shift/su_mean 0.295 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.00637(14) 0.06339(5) 0.80263(11) 0.0446(3) Uani 1 d . . . Ni2 Ni 1.02558(14) -0.07729(6) 0.73408(12) 0.0451(3) Uani 1 d . . . Cl1 Cl 1.4853(4) 0.31552(18) 0.5993(3) 0.0717(8) Uani 1 d . . . Cl2 Cl 0.4665(4) 0.1685(2) 0.1150(3) 0.0815(10) Uani 1 d D . . O1 O 0.9085(10) -0.0212(4) 0.8018(8) 0.063(2) Uani 1 d . . . O2 O 1.1375(9) 0.0046(4) 0.7480(7) 0.0557(19) Uani 1 d . . . O3 O 1.3735(17) 0.2887(8) 0.6443(16) 0.141(6) Uani 1 d . . . O4 O 1.603(2) 0.2655(17) 0.6175(18) 0.217(13) Uani 1 d . . . O5 O 1.565(3) 0.3670(11) 0.672(2) 0.201(9) Uani 1 d . . . O6 O 1.4421(18) 0.3256(12) 0.4807(15) 0.182(9) Uani 1 d . . . O7 O 0.546(2) 0.1097(8) 0.1568(19) 0.195(9) Uani 1 d D . . O8 O 0.337(2) 0.1922(10) 0.137(2) 0.213(11) Uani 1 d D . . O9 O 0.426(4) 0.137(3) 0.010(3) 0.43(4) Uani 1 d D . . O10 O 0.564(3) 0.2228(10) 0.099(4) 0.28(2) Uani 1 d D . . O11 O -0.203(4) 0.5232(12) 0.764(4) 0.40(3) Uani 1 d D . . N1 N 0.9045(10) -0.1536(4) 0.7217(7) 0.0456(19) Uani 1 d . . . N2 N 1.1583(9) -0.1288(4) 0.6739(7) 0.0404(17) Uani 1 d . . . N3 N 1.1018(9) 0.1451(4) 0.7820(7) 0.0454(19) Uani 1 d . . . N4 N 0.8845(9) 0.1135(5) 0.8752(7) 0.0463(18) Uani 1 d . . . N5 N 0.044(2) 0.4739(10) 0.5336(15) 0.127(5) Uani 1 d . . . C1 C 0.5428(11) -0.0723(7) 0.9369(9) 0.051(2) Uani 1 d . . . C2 C 0.5981(11) -0.0045(6) 0.9442(9) 0.051(2) Uani 1 d . . . H2 H 0.5529 0.0294 0.9816 0.061 Uiso 1 calc R . . C3 C 0.7206(11) 0.0157(6) 0.8972(9) 0.046(2) Uani 1 d . . . C4 C 0.7866(11) -0.0369(5) 0.8425(9) 0.045(2) Uani 1 d . . . C5 C 0.7306(11) -0.1051(5) 0.8317(9) 0.044(2) Uani 1 d . . . C6 C 0.6093(12) -0.1218(5) 0.8810(9) 0.051(2) Uani 1 d . . . H6 H 0.5729 -0.1678 0.8756 0.061 Uiso 1 calc R . . C7 C 0.4154(14) -0.0909(8) 0.9898(12) 0.071(3) Uani 1 d . . . H7A H 0.4271 -0.1388 1.0170 0.106 Uiso 1 calc R . . H7B H 0.3178 -0.0854 0.9296 0.106 Uiso 1 calc R . . H7C H 0.4190 -0.0605 1.0570 0.106 Uiso 1 calc R . . C8 C 0.7853(11) -0.1597(5) 0.7641(9) 0.046(2) Uani 1 d . . . H8 H 0.7310 -0.2019 0.7505 0.056 Uiso 1 calc R . . C9 C 0.7730(11) 0.0874(6) 0.9102(9) 0.045(2) Uani 1 d . . . H9 H 0.7207 0.1180 0.9479 0.055 Uiso 1 calc R . . C10 C 0.9444(11) -0.2086(5) 0.6447(9) 0.047(2) Uani 1 d . . . H10 H 0.8988 -0.1947 0.5602 0.056 Uiso 1 calc R . . C11 C 0.8929(14) -0.2843(6) 0.6582(11) 0.059(3) Uani 1 d . . . H11A H 0.9397 -0.3013 0.7397 0.071 Uiso 1 calc R . . H11B H 0.7812 -0.2867 0.6415 0.071 Uiso 1 calc R . . C12 C 0.9469(17) -0.3284(7) 0.5665(13) 0.078(4) Uani 1 d . . . H12A H 0.9164 -0.3770 0.5716 0.094 Uiso 1 calc R . . H12B H 0.8963 -0.3117 0.4854 0.094 Uiso 1 calc R . . C13 C 1.1115(15) -0.3250(6) 0.5873(14) 0.072(3) Uani 1 d . . . H13A H 1.1408 -0.3530 0.5269 0.086 Uiso 1 calc R . . H13B H 1.1622 -0.3447 0.6662 0.086 Uiso 1 calc R . . C14 C 1.1656(15) -0.2509(7) 0.5819(12) 0.065(3) Uani 1 d . . . H14A H 1.2776 -0.2502 0.6001 0.078 Uiso 1 calc R . . H14B H 1.1228 -0.2325 0.5008 0.078 Uiso 1 calc R . . C15 C 1.1171(11) -0.2063(5) 0.6690(9) 0.045(2) Uani 1 d . . . H15 H 1.1628 -0.2259 0.7498 0.054 Uiso 1 calc R . . C16 C 1.2715(12) -0.1048(6) 0.6418(10) 0.048(2) Uani 1 d . . . H16 H 1.3304 -0.1366 0.6120 0.057 Uiso 1 calc R . . C17 C 1.3166(12) -0.0306(6) 0.6483(9) 0.045(2) Uani 1 d . . . C18 C 1.4422(11) -0.0117(5) 0.6036(9) 0.046(2) Uani 1 d . . . H18 H 1.4907 -0.0463 0.5701 0.055 Uiso 1 calc R . . C19 C 1.4942(10) 0.0563(6) 0.6084(9) 0.050(2) Uani 1 d . . . C20 C 1.4242(12) 0.1069(6) 0.6578(9) 0.050(2) Uani 1 d . . . H20 H 1.4589 0.1531 0.6593 0.060 Uiso 1 calc R . . C21 C 1.3014(12) 0.0919(6) 0.7067(9) 0.046(2) Uani 1 d . . . C22 C 1.2502(11) 0.0223(6) 0.7001(9) 0.046(2) Uani 1 d . . . C23 C 1.6251(13) 0.0760(8) 0.5535(12) 0.070(3) Uani 1 d . . . H23A H 1.5820 0.0891 0.4704 0.106 Uiso 1 calc R . . H23B H 1.6927 0.0364 0.5584 0.106 Uiso 1 calc R . . H23C H 1.6827 0.1148 0.5975 0.106 Uiso 1 calc R . . C24 C 1.2253(12) 0.1499(5) 0.7465(8) 0.044(2) Uani 1 d . . . H24 H 1.2686 0.1943 0.7467 0.052 Uiso 1 calc R . . C25 C 1.0152(12) 0.2070(5) 0.8039(9) 0.047(2) Uani 1 d . . . H25 H 0.9285 0.2135 0.7310 0.057 Uiso 1 calc R . . C26 C 1.0974(12) 0.2762(6) 0.8293(11) 0.058(3) Uani 1 d . . . H26A H 1.1349 0.2893 0.7612 0.069 Uiso 1 calc R . . H26B H 1.1860 0.2718 0.9001 0.069 Uiso 1 calc R . . C27 C 0.9906(13) 0.3326(6) 0.8510(12) 0.062(3) Uani 1 d . . . H27A H 1.0497 0.3754 0.8760 0.074 Uiso 1 calc R . . H27B H 0.9123 0.3424 0.7756 0.074 Uiso 1 calc R . . C28 C 0.9123(15) 0.3131(7) 0.9449(13) 0.070(3) Uani 1 d . . . H28A H 0.8361 0.3488 0.9467 0.084 Uiso 1 calc R . . H28B H 0.9887 0.3128 1.0234 0.084 Uiso 1 calc R . . C29 C 0.8312(14) 0.2409(6) 0.9236(12) 0.064(3) Uani 1 d . . . H29A H 0.7956 0.2283 0.9929 0.077 Uiso 1 calc R . . H29B H 0.7422 0.2429 0.8529 0.077 Uiso 1 calc R . . C30 C 0.9455(11) 0.1862(5) 0.9051(8) 0.043(2) Uani 1 d . . . H30 H 1.0303 0.1836 0.9801 0.051 Uiso 1 calc R . . C31 C 0.266(2) 0.4656(12) 0.7327(16) 0.104(5) Uani 1 d . . . H31A H 0.2904 0.4172 0.7528 0.156 Uiso 1 calc R . . H31B H 0.2355 0.4879 0.7974 0.156 Uiso 1 calc R . . H31C H 0.3546 0.4891 0.7209 0.156 Uiso 1 calc R . . C32 C 0.1400(18) 0.4695(8) 0.6233(13) 0.082(4) Uani 1 d . . . C33 C -0.076(5) 0.532(3) 0.831(5) 0.32(3) Uiso 1 d D . . H33A H -0.0773 0.5246 0.9127 0.479 Uiso 1 calc R . . H33B H -0.0431 0.5795 0.8219 0.479 Uiso 1 calc R . . H33C H -0.0052 0.4997 0.8106 0.479 Uiso 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 0.0532(7) 0.0341(6) 0.0571(7) -0.0018(5) 0.0330(5) 0.0008(5) Ni2 0.0535(7) 0.0337(6) 0.0578(7) -0.0017(5) 0.0318(5) 0.0013(5) Cl1 0.0793(19) 0.0623(18) 0.0776(19) 0.0088(14) 0.0288(16) -0.0191(15) Cl2 0.085(2) 0.066(2) 0.096(2) -0.0035(17) 0.0298(18) 0.0254(17) O1 0.080(5) 0.036(4) 0.099(6) -0.005(4) 0.068(5) -0.001(4) O2 0.066(5) 0.039(4) 0.083(5) 0.000(3) 0.055(4) -0.002(3) O3 0.157(12) 0.087(9) 0.231(16) 0.034(10) 0.141(12) -0.008(8) O4 0.144(13) 0.34(4) 0.194(18) 0.05(2) 0.090(13) 0.10(2) O5 0.212(19) 0.138(16) 0.202(17) -0.055(15) -0.024(15) -0.060(15) O6 0.147(14) 0.24(2) 0.124(11) 0.067(13) -0.016(10) -0.092(15) O7 0.220(19) 0.129(14) 0.211(18) 0.006(13) 0.022(16) 0.102(15) O8 0.236(19) 0.107(13) 0.39(3) 0.030(16) 0.24(2) 0.047(14) O9 0.32(4) 0.63(9) 0.27(3) -0.28(5) -0.04(3) 0.17(5) O10 0.21(2) 0.130(16) 0.60(6) 0.06(3) 0.26(3) 0.020(16) O11 0.68(7) 0.104(17) 0.66(7) 0.09(3) 0.57(6) 0.13(3) N1 0.058(5) 0.034(4) 0.048(4) -0.006(4) 0.020(4) -0.001(4) N2 0.043(4) 0.033(4) 0.050(4) -0.002(3) 0.021(4) 0.004(3) N3 0.050(4) 0.039(4) 0.059(5) -0.005(4) 0.034(4) -0.001(4) N4 0.051(4) 0.040(4) 0.053(5) 0.000(3) 0.024(4) 0.004(4) N5 0.128(12) 0.130(14) 0.118(13) -0.030(11) 0.026(10) -0.015(11) C1 0.044(5) 0.060(6) 0.054(5) -0.006(5) 0.021(4) 0.000(5) C2 0.053(5) 0.062(7) 0.046(5) -0.002(4) 0.028(5) -0.007(5) C3 0.046(5) 0.051(6) 0.051(5) 0.002(5) 0.030(4) -0.006(4) C4 0.055(6) 0.038(5) 0.050(5) 0.004(4) 0.028(5) 0.003(4) C5 0.043(5) 0.041(5) 0.052(6) 0.005(4) 0.022(4) 0.001(4) C6 0.060(6) 0.037(5) 0.065(6) 0.002(4) 0.035(5) -0.002(4) C7 0.065(7) 0.081(10) 0.077(7) 0.000(7) 0.038(6) -0.011(7) C8 0.043(5) 0.039(5) 0.057(5) 0.005(4) 0.014(4) -0.004(4) C9 0.053(5) 0.044(6) 0.049(5) -0.005(4) 0.030(4) 0.004(4) C10 0.057(5) 0.036(5) 0.053(5) -0.010(4) 0.024(4) -0.003(4) C11 0.067(7) 0.040(6) 0.079(7) -0.009(5) 0.035(6) -0.003(5) C12 0.094(9) 0.049(6) 0.097(9) -0.026(6) 0.036(8) -0.003(6) C13 0.073(7) 0.045(6) 0.108(10) -0.027(6) 0.044(7) -0.006(6) C14 0.073(7) 0.049(7) 0.081(8) -0.024(6) 0.035(6) -0.005(6) C15 0.051(5) 0.033(5) 0.053(5) -0.003(4) 0.016(4) -0.003(4) C16 0.051(6) 0.044(5) 0.048(5) -0.009(4) 0.013(5) 0.005(4) C17 0.050(5) 0.045(5) 0.044(5) 0.001(4) 0.022(4) 0.009(4) C18 0.047(5) 0.048(5) 0.050(5) -0.007(4) 0.025(4) 0.008(4) C19 0.041(4) 0.060(7) 0.058(5) 0.001(5) 0.029(4) -0.005(5) C20 0.051(5) 0.051(6) 0.050(5) 0.005(4) 0.017(4) -0.011(5) C21 0.055(6) 0.044(6) 0.047(5) 0.004(4) 0.026(4) 0.007(5) C22 0.046(5) 0.047(6) 0.050(5) 0.002(4) 0.024(4) -0.001(4) C23 0.063(6) 0.074(8) 0.091(8) -0.017(7) 0.050(6) -0.019(6) C24 0.058(6) 0.030(5) 0.048(5) 0.002(4) 0.025(4) 0.002(4) C25 0.059(6) 0.034(5) 0.051(5) 0.001(4) 0.019(5) 0.012(4) C26 0.052(6) 0.040(6) 0.088(7) -0.008(5) 0.031(5) -0.006(5) C27 0.056(6) 0.044(6) 0.093(8) -0.005(6) 0.032(6) -0.008(5) C28 0.076(8) 0.046(7) 0.100(9) -0.030(6) 0.043(7) -0.003(6) C29 0.060(7) 0.053(6) 0.096(8) -0.011(6) 0.047(6) 0.003(5) C30 0.046(5) 0.041(5) 0.044(4) -0.004(4) 0.017(4) 0.004(4) C31 0.099(11) 0.109(14) 0.106(12) -0.013(11) 0.031(10) -0.013(11) C32 0.079(9) 0.078(9) 0.077(9) -0.019(8) 0.002(8) -0.025(8) _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 N3 1.822(8) . ? Ni1 N4 1.824(9) . ? Ni1 O1 1.833(8) . ? Ni1 O2 1.860(8) . ? Ni1 Ni2 2.8080(15) . ? Ni2 N1 1.797(9) . ? Ni2 O1 1.821(8) . ? Ni2 N2 1.826(8) . ? Ni2 O2 1.837(8) . ? Cl1 O6 1.325(15) . ? Cl1 O3 1.355(11) . ? Cl1 O5 1.356(16) . ? Cl1 O4 1.39(2) . ? Cl2 O9 1.303(17) . ? Cl2 O7 1.341(12) . ? Cl2 O8 1.341(13) . ? Cl2 O10 1.405(15) . ? O1 C4 1.343(12) . ? O2 C22 1.326(12) . ? O7 O9 1.81(4) . ? O11 C33 1.19(2) . ? N1 C8 1.302(13) . ? N1 C10 1.480(12) . ? N2 C16 1.262(14) . ? N2 C15 1.516(12) . ? N3 C24 1.292(13) . ? N3 C25 1.471(12) . ? N4 C9 1.282(13) . ? N4 C30 1.491(13) . ? N5 C32 1.148(19) . ? C1 C6 1.368(15) . ? C1 C2 1.377(17) . ? C1 C7 1.484(14) . ? C2 C3 1.410(13) . ? C3 C4 1.400(15) . ? C3 C9 1.438(15) . ? C4 C5 1.384(14) . ? C5 C6 1.401(14) . ? C5 C8 1.463(14) . ? C10 C15 1.500(14) . ? C10 C11 1.534(14) . ? C11 C12 1.532(15) . ? C12 C13 1.435(18) . ? C13 C14 1.497(18) . ? C14 C15 1.471(15) . ? C16 C17 1.464(15) . ? C17 C22 1.389(15) . ? C17 C18 1.413(14) . ? C18 C19 1.373(16) . ? C19 C20 1.359(15) . ? C19 C23 1.532(13) . ? C20 C21 1.403(14) . ? C21 C22 1.395(15) . ? C21 C24 1.439(14) . ? C25 C26 1.498(15) . ? C25 C30 1.523(13) . ? C26 C27 1.508(15) . ? C27 C28 1.494(18) . ? C28 C29 1.542(17) . ? C29 C30 1.518(14) . ? C31 C32 1.44(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 N3 Ni1 N4 88.9(4) . . ? N3 Ni1 O1 172.2(4) . . ? N4 Ni1 O1 96.4(4) . . ? N3 Ni1 O2 95.8(4) . . ? N4 Ni1 O2 172.0(4) . . ? O1 Ni1 O2 79.6(3) . . ? N3 Ni1 Ni2 135.0(3) . . ? N4 Ni1 Ni2 136.0(3) . . ? O1 Ni1 Ni2 39.6(2) . . ? O2 Ni1 Ni2 40.3(2) . . ? N1 Ni2 O1 95.5(4) . . ? N1 Ni2 N2 89.1(4) . . ? O1 Ni2 N2 174.7(4) . . ? N1 Ni2 O2 175.8(4) . . ? O1 Ni2 O2 80.6(4) . . ? N2 Ni2 O2 94.9(4) . . ? N1 Ni2 Ni1 135.1(3) . . ? O1 Ni2 Ni1 39.9(3) . . ? N2 Ni2 Ni1 135.8(3) . . ? O2 Ni2 Ni1 40.9(2) . . ? O6 Cl1 O3 114.5(11) . . ? O6 Cl1 O5 118.9(14) . . ? O3 Cl1 O5 111.0(14) . . ? O6 Cl1 O4 104.1(14) . . ? O3 Cl1 O4 107.5(12) . . ? O5 Cl1 O4 98.6(15) . . ? O9 Cl2 O7 86(3) . . ? O9 Cl2 O8 107.5(19) . . ? O7 Cl2 O8 128.0(14) . . ? O9 Cl2 O10 103(3) . . ? O7 Cl2 O10 111.7(14) . . ? O8 Cl2 O10 113.0(12) . . ? C4 O1 Ni2 130.4(7) . . ? C4 O1 Ni1 129.2(7) . . ? Ni2 O1 Ni1 100.4(4) . . ? C22 O2 Ni2 130.1(7) . . ? C22 O2 Ni1 128.3(7) . . ? Ni2 O2 Ni1 98.9(4) . . ? Cl2 O7 O9 45.9(13) . . ? Cl2 O9 O7 47.7(14) . . ? C8 N1 C10 121.8(8) . . ? C8 N1 Ni2 126.0(7) . . ? C10 N1 Ni2 112.0(6) . . ? C16 N2 C15 123.3(8) . . ? C16 N2 Ni2 125.9(7) . . ? C15 N2 Ni2 110.8(6) . . ? C24 N3 C25 122.8(8) . . ? C24 N3 Ni1 125.5(7) . . ? C25 N3 Ni1 111.6(6) . . ? C9 N4 C30 123.8(8) . . ? C9 N4 Ni1 124.5(8) . . ? C30 N4 Ni1 111.2(6) . . ? C6 C1 C2 118.3(9) . . ? C6 C1 C7 121.4(11) . . ? C2 C1 C7 120.4(11) . . ? C1 C2 C3 122.6(10) . . ? C4 C3 C2 117.1(9) . . ? C4 C3 C9 123.8(9) . . ? C2 C3 C9 119.1(10) . . ? O1 C4 C5 119.3(9) . . ? O1 C4 C3 119.4(9) . . ? C5 C4 C3 121.3(9) . . ? C4 C5 C6 118.7(9) . . ? C4 C5 C8 123.0(9) . . ? C6 C5 C8 118.2(9) . . ? C1 C6 C5 122.0(10) . . ? N1 C8 C5 124.9(9) . . ? N4 C9 C3 126.7(9) . . ? N1 C10 C15 106.3(8) . . ? N1 C10 C11 118.1(8) . . ? C15 C10 C11 109.6(8) . . ? C12 C11 C10 106.3(9) . . ? C13 C12 C11 111.9(11) . . ? C12 C13 C14 111.6(11) . . ? C15 C14 C13 110.6(10) . . ? C14 C15 C10 110.2(9) . . ? C14 C15 N2 118.0(9) . . ? C10 C15 N2 105.4(8) . . ? N2 C16 C17 124.6(9) . . ? C22 C17 C18 117.2(9) . . ? C22 C17 C16 125.0(10) . . ? C18 C17 C16 117.7(10) . . ? C19 C18 C17 121.6(9) . . ? C20 C19 C18 119.4(9) . . ? C20 C19 C23 120.1(11) . . ? C18 C19 C23 120.4(10) . . ? C19 C20 C21 122.3(10) . . ? C22 C21 C20 117.2(10) . . ? C22 C21 C24 124.3(10) . . ? C20 C21 C24 118.1(10) . . ? O2 C22 C17 117.8(9) . . ? O2 C22 C21 119.9(10) . . ? C17 C22 C21 122.3(10) . . ? N3 C24 C21 125.2(10) . . ? N3 C25 C26 118.7(8) . . ? N3 C25 C30 106.0(8) . . ? C26 C25 C30 111.4(8) . . ? C25 C26 C27 110.8(8) . . ? C28 C27 C26 113.3(11) . . ? C27 C28 C29 113.9(10) . . ? C30 C29 C28 108.8(9) . . ? N4 C30 C29 116.6(8) . . ? N4 C30 C25 105.5(7) . . ? C29 C30 C25 111.8(9) . . ? N5 C32 C31 177.1(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.873 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.102 data_[MNL4(OH)2]PF6CH3OH #7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 F6 Mn N4 O8 P' _chemical_formula_weight 1008.81 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 20.117(4) _cell_length_b 58.207(12) _cell_length_c 9.730(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11393(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 0.327 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Rigaku AFC7R' _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 3589 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 75 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3589 _reflns_number_gt 1466 _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 w=1/[\s^2^(Fo^2^)+(0.1747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(17) _refine_ls_number_reflns 3589 _refine_ls_number_parameters 383 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.2138 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2986 _refine_ls_wR_factor_gt 0.2380 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 1.737 _refine_ls_shift/su_max 0.570 _refine_ls_shift/su_mean 0.021 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.44070(6) 0.0000 0.0676(13) Uani 1 d S . . Mn2 Mn 0.2500 0.30914(6) 0.2500 0.0674(14) Uani 1 d S . . O1W O 0.4246(8) 0.4392(2) 0.1790(17) 0.098(5) Uani 1 d . . . O2W O 0.3124(8) 0.3111(3) 0.0641(16) 0.097(5) Uani 1 d . . . O1 O 0.4464(8) 0.46320(19) -0.0869(14) 0.077(5) Uani 1 d D . . O2 O 0.3654(10) 0.5203(3) -0.234(3) 0.121(8) Uani 1 d D . . N1 N 0.4515(7) 0.4142(2) -0.0921(15) 0.056(4) Uani 1 d D . . C1 C 0.4016(9) 0.4605(3) -0.181(2) 0.081(7) Uani 1 d D . . C2 C 0.3791(7) 0.4389(3) -0.2313(15) 0.065(5) Uani 1 d D . . C3 C 0.3310(9) 0.4383(3) -0.3344(19) 0.078(6) Uani 1 d D . . H3A H 0.3150 0.4234 -0.3605 0.100 Uiso 1 d R . . C4 C 0.3048(9) 0.4576(3) -0.396(2) 0.070(6) Uani 1 d D . . C5 C 0.3284(12) 0.4792(3) -0.348(2) 0.086(8) Uani 1 d D . . H5A H 0.3103 0.4932 -0.3850 0.100 Uiso 1 d R . . C6 C 0.3743(11) 0.4801(3) -0.241(2) 0.082(8) Uani 1 d D . . C7 C 0.4024(10) 0.4178(4) -0.176(2) 0.083(7) Uani 1 d D . . H7A H 0.3830 0.4041 -0.2138 0.100 Uiso 1 d R . . C8 C 0.2534(16) 0.4563(3) -0.510(3) 0.088(6) Uani 1 d D . . H8A H 0.2451 0.4406 -0.5354 0.120 Uiso 1 d R . . H8B H 0.2133 0.4630 -0.4744 0.120 Uiso 1 d R . . H8C H 0.2674 0.4647 -0.5899 0.120 Uiso 1 d R . . C9 C 0.3931(12) 0.5035(3) -0.193(2) 0.090(8) Uani 1 d D . . H9A H 0.4294 0.5043 -0.1293 0.100 Uiso 1 d R . . C10 C 0.4840(17) 0.3920(2) -0.078(2) 0.090(8) Uani 1 d . . . H10A H 0.5212 0.3912 -0.1391 0.100 Uiso 1 d R . . C11 C 0.4404(16) 0.3709(3) -0.105(2) 0.107(10) Uani 1 d . . . H11A H 0.4286 0.3699 -0.1999 0.100 Uiso 1 d R . . H11B H 0.4006 0.3719 -0.0504 0.100 Uiso 1 d R . . C12 C 0.4816(14) 0.3510(3) -0.059(2) 0.099(9) Uani 1 d . . . H12A H 0.5130 0.3483 -0.1317 0.100 Uiso 1 d R . . H12B H 0.4527 0.3378 -0.0567 0.100 Uiso 1 d R . . O3 O 0.3042(8) 0.28681(19) 0.3285(17) 0.080(5) Uani 1 d D . . O4 O 0.3776(9) 0.2287(2) 0.494(2) 0.097(6) Uani 1 d D . . N2 N 0.3019(11) 0.3338(3) 0.323(2) 0.096(7) Uani 1 d D . . C13 C 0.3481(8) 0.2889(2) 0.4324(16) 0.053(5) Uani 1 d D . . C14 C 0.3695(9) 0.3112(3) 0.480(2) 0.092(8) Uani 1 d D . . C15 C 0.4172(9) 0.3131(3) 0.5866(19) 0.066(6) Uani 1 d D . . H15A H 0.4304 0.3280 0.6189 0.100 Uiso 1 d R . . C16 C 0.4446(10) 0.2939(3) 0.644(2) 0.080(7) Uani 1 d D . . C17 C 0.4252(9) 0.2725(3) 0.5922(19) 0.066(6) Uani 1 d D . . H17A H 0.4452 0.2587 0.6278 0.100 Uiso 1 d R . . C18 C 0.3773(10) 0.2695(3) 0.4908(19) 0.057(6) Uani 1 d D . . C19 C 0.3428(13) 0.3333(3) 0.421(2) 0.093(9) Uani 1 d D . . H19A H 0.3611 0.3474 0.4553 0.100 Uiso 1 d R . . C20 C 0.4920(16) 0.2958(3) 0.757(3) 0.097(8) Uani 1 d D . . H20A H 0.5006 0.3116 0.7778 0.120 Uiso 1 d R . . H20B H 0.4734 0.2884 0.8367 0.120 Uiso 1 d R . . H20C H 0.5328 0.2883 0.7324 0.120 Uiso 1 d R . . C21 C 0.3545(9) 0.2470(4) 0.453(2) 0.075(7) Uani 1 d D . . H21A H 0.3196 0.2456 0.3858 0.100 Uiso 1 d R . . C22 C 0.2874(10) 0.3569(3) 0.256(2) 0.076(6) Uani 1 d . . . H22A H 0.3046 0.3565 0.1645 0.100 Uiso 1 d R . . C23 C 0.3113(12) 0.3779(3) 0.316(2) 0.072(6) Uani 1 d . . . H23A H 0.3589 0.3771 0.3199 0.100 Uiso 1 d R . . H23B H 0.2951 0.3782 0.4084 0.100 Uiso 1 d R . . C24 C 0.2903(11) 0.3997(3) 0.252(4) 0.114(9) Uani 1 d . . . H24A H 0.3085 0.4006 0.1609 0.100 Uiso 1 d R . . H24B H 0.3065 0.4125 0.3049 0.100 Uiso 1 d R . . P1 P 0.5000 0.38937(7) 0.5000 0.151(6) Uani 1 d SDU . . F1 F 0.42780(19) 0.3897(3) 0.5638(9) 0.135(12) Uani 0.50 d PDU . . F2 F 0.4761(6) 0.40830(14) 0.3953(9) 0.182(19) Uani 0.50 d PDU . . F3 F 0.4799(7) 0.37011(14) 0.3940(9) 0.23(2) Uani 0.50 d PDU . . P2 P 0.2500 0.36449(7) -0.2500 0.167(7) Uani 1 d SDU . . F4 F 0.32098(19) 0.3645(2) -0.3194(9) 0.153(14) Uani 0.50 d PDU . . F5 F 0.2741(5) 0.34539(13) -0.1459(9) 0.173(18) Uani 0.50 d PDU . . F6 F 0.2739(6) 0.38376(14) -0.1468(9) 0.139(14) Uani 0.50 d PDU . . O5 O 0.5000 0.4877(5) 0.5000 0.074(10) Uani 0.50 d SPDU . . C25 C 0.5000 0.4635(5) 0.5000 0.10(2) Uani 0.50 d SPDU . . O6 O 0.2500 0.2434(4) 0.7500 0.108(15) Uani 0.50 d SPDU . . C26 C 0.2500 0.2191(5) 0.7500 0.13(3) Uani 0.50 d SPDU . . 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 0.094(3) 0.046(2) 0.062(3) 0.000 0.009(3) 0.000 Mn2 0.096(3) 0.0403(19) 0.066(3) 0.000 -0.005(3) 0.000 O1W 0.119(12) 0.057(7) 0.117(13) 0.006(9) 0.040(12) 0.006(8) O2W 0.119(13) 0.108(11) 0.064(9) 0.003(9) 0.021(9) 0.024(10) O1 0.123(13) 0.050(7) 0.058(8) -0.006(7) -0.003(10) 0.001(8) O2 0.169(19) 0.063(10) 0.131(16) -0.027(12) -0.031(17) -0.008(11) N1 0.071(9) 0.042(7) 0.056(8) 0.003(6) -0.021(8) -0.004(7) C1 0.089(17) 0.075(15) 0.078(17) -0.003(13) 0.037(15) 0.006(13) C2 0.084(13) 0.050(9) 0.062(11) -0.018(10) -0.043(11) 0.019(10) C3 0.101(16) 0.067(12) 0.066(13) -0.019(12) 0.019(14) -0.006(13) C4 0.063(12) 0.054(10) 0.092(16) -0.003(11) 0.012(14) 0.010(10) C5 0.12(2) 0.069(13) 0.069(14) -0.027(12) 0.003(16) -0.002(14) C6 0.090(17) 0.071(14) 0.083(17) -0.033(14) -0.003(17) 0.030(13) C7 0.095(17) 0.072(13) 0.081(16) -0.021(12) -0.013(15) 0.000(13) C8 0.083(13) 0.078(11) 0.104(17) 0.015(16) 0.009(19) 0.006(17) C9 0.16(2) 0.026(9) 0.086(16) -0.008(10) -0.009(17) -0.008(12) C10 0.17(3) 0.035(7) 0.066(12) 0.011(8) 0.016(16) 0.006(12) C11 0.21(3) 0.047(10) 0.067(13) 0.000(10) 0.012(18) -0.016(14) C12 0.12(2) 0.076(12) 0.099(18) 0.001(12) 0.000(16) -0.017(14) O3 0.096(10) 0.049(7) 0.095(11) 0.003(8) -0.036(10) 0.003(7) O4 0.112(13) 0.054(8) 0.125(13) -0.007(10) -0.070(13) 0.021(9) N2 0.163(19) 0.033(8) 0.091(14) -0.004(9) 0.006(15) 0.013(11) C13 0.071(13) 0.032(8) 0.057(12) -0.011(8) -0.013(11) -0.005(8) C14 0.14(2) 0.055(11) 0.085(16) -0.004(13) 0.067(17) -0.018(14) C15 0.075(14) 0.062(11) 0.061(13) -0.005(11) -0.006(13) 0.001(11) C16 0.090(16) 0.097(16) 0.053(12) -0.005(12) 0.012(14) -0.020(14) C17 0.063(12) 0.066(11) 0.068(12) 0.022(11) 0.004(12) 0.000(10) C18 0.076(14) 0.051(10) 0.043(9) 0.005(9) -0.001(12) -0.020(10) C19 0.17(3) 0.034(9) 0.073(15) 0.002(11) 0.030(18) -0.007(14) C20 0.110(18) 0.095(13) 0.084(15) -0.031(15) -0.027(18) -0.029(17) C21 0.067(11) 0.069(13) 0.089(16) -0.011(13) -0.017(12) 0.017(13) C22 0.123(16) 0.051(8) 0.055(10) -0.015(10) 0.028(15) -0.012(10) C23 0.103(16) 0.046(9) 0.066(12) 0.002(9) 0.001(12) 0.003(10) C24 0.136(19) 0.045(9) 0.16(2) 0.008(16) 0.03(3) -0.030(11) P1 0.123(10) 0.274(18) 0.055(6) 0.000 0.004(8) 0.000 F1 0.15(3) 0.20(3) 0.053(15) 0.029(19) 0.046(19) 0.03(2) F2 0.24(5) 0.25(4) 0.057(16) 0.03(2) 0.02(2) -0.08(4) F3 0.23(5) 0.26(4) 0.20(4) -0.09(3) 0.13(4) 0.02(4) P2 0.105(9) 0.31(2) 0.087(8) 0.000 -0.003(10) 0.000 F4 0.14(3) 0.22(3) 0.10(2) -0.08(2) -0.04(2) 0.07(3) F5 0.18(4) 0.16(3) 0.18(3) 0.12(3) -0.07(3) 0.01(2) F6 0.11(2) 0.21(3) 0.09(2) 0.02(2) 0.004(19) -0.08(2) O5 0.07(2) 0.08(2) 0.08(2) 0.000 0.00(2) 0.000 C25 0.13(5) 0.11(4) 0.04(3) 0.000 0.02(4) 0.000 O6 0.17(4) 0.04(2) 0.12(3) 0.000 -0.07(4) 0.000 C26 0.09(5) 0.15(6) 0.16(7) 0.000 -0.03(7) 0.000 _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 O1 1.895(14) 3_655 ? Mn1 O1 1.895(14) . ? Mn1 N1 2.033(14) . ? Mn1 N1 2.033(14) 3_655 ? Mn1 O1W 2.311(15) 3_655 ? Mn1 O1W 2.311(15) . ? Mn2 O3 1.860(13) 11 ? Mn2 O3 1.860(13) . ? Mn2 N2 1.91(2) 11 ? Mn2 N2 1.91(2) . ? Mn2 O2W 2.205(15) . ? Mn2 O2W 2.205(15) 11 ? O1 C1 1.29(2) . ? O2 C9 1.20(3) . ? N1 C7 1.30(2) . ? N1 C10 1.46(2) . ? C1 C6 1.40(2) . ? C1 C2 1.42(2) . ? C2 C3 1.39(2) . ? C2 C7 1.42(2) . ? C3 C4 1.38(2) . ? C4 C5 1.42(2) . ? C4 C8 1.52(4) . ? C5 C6 1.39(2) . ? C6 C9 1.49(2) . ? C10 C11 1.53(3) . ? C10 C10 1.64(4) 3_655 ? C11 C12 1.49(3) . ? C12 C12 1.37(5) 3_655 ? O3 C13 1.35(2) . ? O4 C21 1.23(2) . ? N2 C19 1.26(3) . ? N2 C22 1.52(3) . ? C13 C18 1.393(19) . ? C13 C14 1.442(19) . ? C14 C15 1.42(2) . ? C14 C19 1.51(3) . ? C15 C16 1.36(2) . ? C16 C17 1.40(2) . ? C16 C20 1.46(3) . ? C17 C18 1.39(2) . ? C18 C21 1.44(3) . ? C22 C23 1.43(2) . ? C22 C22 1.51(4) 11 ? C23 C24 1.47(3) . ? C24 C24 1.62(4) 11 ? P1 F2 1.5752(14) 3_656 ? P1 F2 1.5752(14) . ? P1 F3 1.5756(13) . ? P1 F3 1.5756(13) 3_656 ? P1 F1 1.5796(13) . ? P1 F1 1.5796(13) 3_656 ? P2 F4 1.5796(13) 11_554 ? P2 F4 1.5796(13) . ? P2 F5 1.5799(13) 11_554 ? P2 F5 1.5799(13) . ? P2 F6 1.5800(14) . ? P2 F6 1.5800(14) 11_554 ? O5 C25 1.408(18) . ? O5 O5 1.43(6) 2_665 ? O6 O6 0.76(5) 14 ? O6 C26 1.416(18) . ? 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 Mn1 O1 92.6(8) 3_655 . ? O1 Mn1 N1 173.6(6) 3_655 . ? O1 Mn1 N1 93.1(5) . . ? O1 Mn1 N1 93.1(5) 3_655 3_655 ? O1 Mn1 N1 173.6(6) . 3_655 ? N1 Mn1 N1 81.3(8) . 3_655 ? O1 Mn1 O1W 89.4(6) 3_655 3_655 ? O1 Mn1 O1W 93.6(6) . 3_655 ? N1 Mn1 O1W 87.4(6) . 3_655 ? N1 Mn1 O1W 89.3(6) 3_655 3_655 ? O1 Mn1 O1W 93.6(6) 3_655 . ? O1 Mn1 O1W 89.4(6) . . ? N1 Mn1 O1W 89.3(6) . . ? N1 Mn1 O1W 87.4(6) 3_655 . ? O1W Mn1 O1W 175.7(7) 3_655 . ? O3 Mn2 O3 91.4(8) 11 . ? O3 Mn2 N2 93.0(7) 11 11 ? O3 Mn2 N2 175.5(8) . 11 ? O3 Mn2 N2 175.5(8) 11 . ? O3 Mn2 N2 93.0(7) . . ? N2 Mn2 N2 82.6(12) 11 . ? O3 Mn2 O2W 91.9(7) 11 . ? O3 Mn2 O2W 92.3(7) . . ? N2 Mn2 O2W 88.1(7) 11 . ? N2 Mn2 O2W 87.3(8) . . ? O3 Mn2 O2W 92.3(7) 11 11 ? O3 Mn2 O2W 91.9(7) . 11 ? N2 Mn2 O2W 87.3(8) 11 11 ? N2 Mn2 O2W 88.1(7) . 11 ? O2W Mn2 O2W 173.9(9) . 11 ? C1 O1 Mn1 128.8(12) . . ? C7 N1 C10 123.0(17) . . ? C7 N1 Mn1 121.4(13) . . ? C10 N1 Mn1 114.5(14) . . ? O1 C1 C6 118.1(17) . . ? O1 C1 C2 125.0(17) . . ? C6 C1 C2 116.8(18) . . ? C3 C2 C7 118.8(16) . . ? C3 C2 C1 119.3(16) . . ? C7 C2 C1 121.9(15) . . ? C4 C3 C2 124.2(17) . . ? C3 C4 C5 116.4(18) . . ? C3 C4 C8 122.4(16) . . ? C5 C4 C8 121.1(16) . . ? C6 C5 C4 120.0(18) . . ? C5 C6 C1 123.2(18) . . ? C5 C6 C9 115.8(18) . . ? C1 C6 C9 121.1(19) . . ? N1 C7 C2 128.8(18) . . ? O2 C9 C6 122(2) . . ? N1 C10 C11 116(2) . . ? N1 C10 C10 105.4(12) . 3_655 ? C11 C10 C10 112.5(16) . 3_655 ? C12 C11 C10 105(2) . . ? C12 C12 C11 123.3(16) 3_655 . ? C13 O3 Mn2 128.9(10) . . ? C19 N2 C22 117.8(19) . . ? C19 N2 Mn2 128.3(16) . . ? C22 N2 Mn2 113.8(16) . . ? O3 C13 C18 120.5(13) . . ? O3 C13 C14 121.2(15) . . ? C18 C13 C14 118.1(15) . . ? C15 C14 C13 120.5(17) . . ? C15 C14 C19 117.1(17) . . ? C13 C14 C19 122.4(19) . . ? C16 C15 C14 120.7(17) . . ? C15 C16 C17 117.8(17) . . ? C15 C16 C20 121.0(18) . . ? C17 C16 C20 121.3(19) . . ? C18 C17 C16 124.0(16) . . ? C17 C18 C13 118.8(15) . . ? C17 C18 C21 121.1(16) . . ? C13 C18 C21 120.0(16) . . ? N2 C19 C14 123(2) . . ? O4 C21 C18 125.7(17) . . ? C23 C22 C22 111.6(15) . 11 ? C23 C22 N2 121(2) . . ? C22 C22 N2 103.1(14) 11 . ? C22 C23 C24 118(2) . . ? C23 C24 C24 107.2(18) . 11 ? F2 P1 F2 91.2(7) 3_656 . ? F2 P1 F3 177.1(6) 3_656 . ? F2 P1 F3 89.8(5) . . ? F2 P1 F3 89.8(5) 3_656 3_656 ? F2 P1 F3 177.1(7) . 3_656 ? F3 P1 F3 89.3(8) . 3_656 ? F2 P1 F1 91.0(6) 3_656 . ? F2 P1 F1 88.0(6) . . ? F3 P1 F1 91.7(7) . . ? F3 P1 F1 89.3(6) 3_656 . ? F2 P1 F1 88.0(6) 3_656 3_656 ? F2 P1 F1 91.0(6) . 3_656 ? F3 P1 F1 89.3(6) . 3_656 ? F3 P1 F1 91.7(7) 3_656 3_656 ? F1 P1 F1 178.6(11) . 3_656 ? F4 P2 F4 179.8(11) 11_554 . ? F4 P2 F5 89.8(6) 11_554 11_554 ? F4 P2 F5 90.3(5) . 11_554 ? F4 P2 F5 90.3(5) 11_554 . ? F4 P2 F5 89.8(6) . . ? F5 P2 F5 90.6(7) 11_554 . ? F4 P2 F6 90.1(5) 11_554 . ? F4 P2 F6 89.8(6) . . ? F5 P2 F6 179.5(5) 11_554 . ? F5 P2 F6 89.9(5) . . ? F4 P2 F6 89.8(6) 11_554 11_554 ? F4 P2 F6 90.1(5) . 11_554 ? F5 P2 F6 89.9(5) 11_554 11_554 ? F5 P2 F6 179.5(6) . 11_554 ? F6 P2 F6 89.6(8) . 11_554 ? C25 O5 O5 180.000(3) . 2_665 ? O6 O6 C26 180.000(3) 14 . ? _diffrn_measured_fraction_theta_max 0.249 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.249 _refine_diff_density_max 0.745 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.083