# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2021 data_[CuL4](ClO4)2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; Cu 2+, C18 H28 N6, (Cl O4 1-)2 ; _chemical_formula_structural ; [Cu (C18 H28 N6)] (Cl O4)2 ; _chemical_formula_analytical ? _chemical_formula_sum 'C18 H28 Cl2 Cu N6 O8' _chemical_formula_weight 590.90 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' 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 12.309(9) _cell_length_b 13.834(9) _cell_length_c 14.528(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.74(5) _cell_angle_gamma 90.00 _cell_volume 2451.3(27) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 13 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method ? _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type 'refdelf (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.89 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 Enraf-Nonius' _diffrn_measurement_method '\q/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4474 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.2709 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4290 _reflns_number_observed 1462 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Enraf-Nonius' _computing_cell_refinement 'CAD4 Enraf-Nonius' _computing_data_reduction 'CAD4 Enraf-Nonius' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 (Ver. 1.01\b)(Farrugia,1997)' _computing_publication_material ; SHELXL-93 (Sheldrick, 1993), PARST93 (Nardelli,1993) ; _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2434P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4287 _refine_ls_number_parameters 317 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2966 _refine_ls_R_factor_obs 0.0938 _refine_ls_wR_factor_all 0.3969 _refine_ls_wR_factor_obs 0.2545 _refine_ls_goodness_of_fit_all 0.922 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 0.938 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.028 _refine_ls_shift/esd_mean 0.002 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 Cu Cu 0.1755(2) 0.01110(12) 0.25807(12) 0.0533(7) Uani 1 d . . Cl1 Cl 1.0137(4) 0.3019(4) 0.4169(3) 0.0759(13) Uani 1 d . . O11 O 0.9072(14) 0.2697(13) 0.3728(14) 0.141(6) Uani 1 d . . O12 O 1.0641(19) 0.2247(15) 0.4650(16) 0.185(10) Uani 1 d . . O13 O 0.9995(21) 0.3799(22) 0.4600(22) 0.271(17) Uani 1 d . . O14 O 1.0678(21) 0.3109(24) 0.3430(23) 0.254(15) Uani 1 d . . Cl2 Cl 0.3928(5) -0.3471(5) 0.3380(5) 0.106(2) Uani 1 d D . O21 O 0.3122(15) -0.3073(14) 0.2697(13) 0.161(8) Uani 1 d D . O22 O 0.3982(35) -0.4369(13) 0.3394(20) 0.294(20) Uani 1 d D . O23 O 0.4890(16) -0.3197(26) 0.3212(27) 0.291(21) Uani 1 d D . O24 O 0.3950(28) -0.3009(23) 0.4174(16) 0.273(19) Uani 1 d D . C1 C -0.0483(16) 0.0939(15) 0.2101(17) 0.104(7) Uani 1 d . . H1A H -0.0180 0.1291 0.1626 0.050 Uiso 1 calc . . H1B H -0.1066 0.1307 0.2307 0.050 Uiso 1 calc . . H1C H -0.0764 0.0331 0.1856 0.050 Uiso 1 calc . . N1 N 0.0350(11) 0.0773(11) 0.2864(10) 0.074(4) Uani 1 d . . C2 C -0.0012(20) 0.0254(19) 0.3658(17) 0.109(7) Uani 1 d . . H2A H 0.0500 0.0378 0.4214 0.050 Uiso 1 calc . . H2B H -0.0726 0.0493 0.3763 0.050 Uiso 1 calc . . C3 C -0.0074(15) -0.0739(17) 0.3491(15) 0.090(6) Uani 1 d . . H3A H -0.0661 -0.0866 0.2989 0.050 Uiso 1 calc . . H3B H -0.0252 -0.1065 0.4042 0.050 Uiso 1 calc . . N2 N 0.0979(12) -0.1142(11) 0.3237(10) 0.075(4) Uani 1 d . . C4 C 0.1708(18) -0.1547(13) 0.4031(14) 0.089(6) Uani 1 d . . H4A H 0.2156 -0.2048 0.3806 0.050 Uiso 1 calc . . H4B H 0.1263 -0.1846 0.4454 0.050 Uiso 1 calc . . C5 C 0.2465(14) -0.0793(14) 0.4568(12) 0.072(5) Uani 1 d . . N3 N 0.2591(10) 0.0031(10) 0.4127(7) 0.056(3) Uani 1 d . . C6 C 0.3229(13) 0.0715(13) 0.4507(10) 0.061(4) Uani 1 d . . C7 C 0.3802(14) 0.0585(17) 0.5414(12) 0.084(6) Uani 1 d . . H7 H 0.4270 0.1060 0.5692 0.050 Uiso 1 calc . . C8 C 0.3644(18) -0.0260(21) 0.5865(13) 0.100(7) Uani 1 d . . H8 H 0.4004 -0.0360 0.6462 0.050 Uiso 1 calc . . C9 C 0.2986(19) -0.0932(16) 0.5463(12) 0.090(6) Uani 1 d . . H9 H 0.2872 -0.1500 0.5780 0.050 Uiso 1 calc . . C10 C 0.3294(13) 0.1575(13) 0.3950(12) 0.067(4) Uani 1 d . . N4 N 0.2757(10) 0.1471(9) 0.3056(8) 0.057(3) Uani 1 d . . C11 C 0.2699(14) 0.2205(12) 0.2490(13) 0.068(4) Uani 1 d . . C12 C 0.3142(15) 0.3099(14) 0.2731(14) 0.079(5) Uani 1 d . . H12 H 0.3063 0.3609 0.2310 0.050 Uiso 1 calc . . C13 C 0.3699(19) 0.3221(15) 0.3601(19) 0.095(7) Uani 1 d . . H13 H 0.4010 0.3816 0.3781 0.050 Uiso 1 calc . . C14 C 0.3790(15) 0.2486(19) 0.4185(14) 0.097(8) Uani 1 d . . H14 H 0.4192 0.2566 0.4769 0.050 Uiso 1 calc . . C15 C 0.2094(17) 0.1990(18) 0.1546(13) 0.092(6) Uani 1 d . . H15A H 0.1409 0.2345 0.1471 0.050 Uiso 1 calc . . H15B H 0.2526 0.2224 0.1081 0.050 Uiso 1 calc . . N5 N 0.1856(13) 0.0970(11) 0.1373(9) 0.078(4) Uani 1 d . . C16 C 0.2796(20) 0.0501(22) 0.0949(13) 0.110(8) Uani 1 d . . H16A H 0.2713 0.0641 0.0289 0.050 Uiso 1 calc . . H16B H 0.3486 0.0778 0.1230 0.050 Uiso 1 calc . . C17 C 0.2825(15) -0.0516(17) 0.1082(13) 0.080(5) Uani 1 d . . H17A H 0.3482 -0.0774 0.0872 0.050 Uiso 1 calc . . H17B H 0.2197 -0.0805 0.0706 0.050 Uiso 1 calc . . N6 N 0.2812(13) -0.0787(12) 0.2064(11) 0.085(5) Uani 1 d . . C18 C 0.3921(21) -0.0774(18) 0.2569(18) 0.115(8) Uani 1 d . . H18A H 0.3899 -0.0958 0.3203 0.050 Uiso 1 calc . . H18B H 0.4221 -0.0134 0.2550 0.050 Uiso 1 calc . . H18C H 0.4373 -0.1220 0.2286 0.050 Uiso 1 calc . . 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 Cu 0.0582(11) 0.0501(12) 0.0525(10) 0.0002(9) 0.0106(7) 0.0040(10) Cl1 0.092(4) 0.074(3) 0.060(2) -0.006(2) 0.004(2) 0.013(3) O11 0.099(12) 0.130(14) 0.179(16) -0.012(12) -0.029(11) 0.011(11) O12 0.209(21) 0.130(15) 0.191(19) 0.053(15) -0.069(16) -0.013(15) O13 0.211(25) 0.267(30) 0.305(32) -0.196(29) -0.070(23) 0.102(22) O14 0.190(24) 0.305(36) 0.297(31) 0.114(29) 0.147(24) 0.068(24) Cl2 0.096(4) 0.107(5) 0.118(5) -0.020(4) 0.023(4) -0.009(4) O21 0.145(15) 0.165(16) 0.147(15) -0.012(13) -0.073(13) 0.013(14) O22 0.531(59) 0.071(14) 0.267(32) 0.065(18) 0.003(33) -0.013(23) O23 0.102(17) 0.354(43) 0.432(51) 0.216(40) 0.089(22) 0.058(21) O24 0.338(40) 0.272(32) 0.166(20) -0.104(23) -0.120(24) 0.152(30) C1 0.071(13) 0.084(14) 0.148(19) -0.043(14) -0.017(13) 0.024(12) N1 0.057(9) 0.077(10) 0.091(10) 0.007(8) 0.021(8) -0.006(8) C2 0.109(18) 0.111(19) 0.116(17) 0.022(15) 0.044(14) 0.038(15) C3 0.050(11) 0.100(17) 0.120(16) 0.021(13) 0.014(11) 0.023(11) N2 0.079(10) 0.067(9) 0.080(9) 0.009(8) 0.012(8) -0.002(8) C4 0.120(17) 0.053(11) 0.099(14) 0.016(11) 0.032(12) 0.001(11) C5 0.071(12) 0.075(12) 0.067(10) 0.014(10) 0.002(9) 0.004(10) N3 0.070(8) 0.058(8) 0.040(6) 0.008(7) 0.001(5) 0.016(7) C6 0.050(10) 0.079(12) 0.048(9) -0.004(9) -0.013(7) 0.003(9) C7 0.063(11) 0.123(17) 0.058(10) -0.001(12) -0.023(9) 0.012(12) C8 0.092(15) 0.153(23) 0.048(10) 0.031(13) -0.011(10) 0.008(15) C9 0.129(18) 0.096(15) 0.041(9) 0.030(10) -0.007(11) 0.026(14) C10 0.063(11) 0.068(12) 0.071(11) -0.020(9) 0.017(8) -0.012(9) N4 0.067(9) 0.053(8) 0.051(7) 0.010(6) 0.007(6) 0.009(7) C11 0.062(11) 0.060(11) 0.086(12) -0.006(10) 0.026(9) -0.017(9) C12 0.075(12) 0.078(13) 0.088(13) -0.001(11) 0.026(10) -0.022(11) C13 0.106(17) 0.060(12) 0.134(20) -0.021(13) 0.066(15) -0.047(12) C14 0.073(13) 0.134(20) 0.090(14) -0.069(14) 0.036(10) -0.062(13) C15 0.089(14) 0.118(18) 0.068(11) 0.031(12) 0.010(10) 0.017(13) N5 0.107(13) 0.070(10) 0.052(8) 0.008(7) -0.001(8) -0.024(9) C16 0.112(19) 0.156(24) 0.058(12) -0.006(14) 0.004(12) 0.008(18) C17 0.067(12) 0.094(15) 0.079(13) -0.027(11) 0.012(10) 0.006(11) N6 0.069(10) 0.106(13) 0.080(11) -0.018(9) 0.008(8) 0.009(9) C18 0.110(18) 0.112(19) 0.136(19) 0.031(15) 0.059(16) 0.028(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. Weighted least-squares planes through the starred atoms (Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807). Equation of the plane: m1*X+m2*Y+m3*Z=d Plane 1 m1 = -0.54550(0.00438) m2 = -0.40537(0.00488) m3 = -0.73356(0.00321) D = -3.23839(0.01151) Atom d s d/s (d/s)**2 N1 * -0.1491 0.0147 -10.156 103.136 N2 * 0.1487 0.0147 10.143 102.871 N5 * 0.1446 0.0145 9.947 98.952 N6 * -0.1676 0.0156 -10.711 114.719 Cu -0.4519 0.0018 -250.242 62620.875 ============ Sum((d/s)**2) for starred atoms 419.678 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Weighted least-squares lines through the starred atoms (Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600) m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes. X0,Y0,Z0 are the coordinates of the centroid of the set of atoms. Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3 Line 1 m1 = 0.30979(0.00525) X0 = 2.01815(0.00905) m2 = -0.04715(0.00576) Y0 = 0.09829(0.00947) m3 = 0.94963(0.00175) Z0 = 4.82815(0.00753) Atom d s d/s (d/s)**2 Cu * 0.0000 0.0026 0.004 0.000 N3 * 0.0000 0.0182 0.001 0.000 ============ Sum((d/s)**2) for starred atoms 0.000 Line 2 m1 = 0.49523(0.00486) X0 = 2.22556(0.00915) m2 = 0.81650(0.00305) Y0 = 1.09420(0.00880) m3 = 0.29678(0.00495) Z0 = 4.05698(0.00834) Atom d s d/s (d/s)**2 Cu * 0.0000 0.0026 0.004 0.000 N4 * 0.0000 0.0173 0.001 0.000 ============ Sum((d/s)**2) for starred atoms 0.000 Angles formed by LSQ-lines Line - line angle (e.s.d.) 1 2 66.63( 0.42) Angles formed by lines and normals to planes Line - plane angle (e.s.d.) 1 1 147.83( 0.40) 2 1 144.97( 0.40) ; 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 Cu N6 2.02(2) . ? Cu N1 2.047(14) . ? Cu N5 2.136(13) . ? Cu N2 2.253(14) . ? Cu N4 2.304(13) . ? Cu N3 2.344(11) . ? Cl1 O13 1.27(2) . ? Cl1 O14 1.34(2) . ? Cl1 O12 1.38(2) . ? Cl1 O11 1.45(2) . ? Cl2 O22 1.24(2) . ? Cl2 O23 1.30(2) . ? Cl2 O24 1.32(2) . ? Cl2 O21 1.417(14) . ? C1 N1 1.42(2) . ? N1 C2 1.48(3) . ? C2 C3 1.40(3) . ? C3 N2 1.50(2) . ? N2 C4 1.47(2) . ? C4 C5 1.54(3) . ? C5 N3 1.33(2) . ? C5 C9 1.38(2) . ? N3 C6 1.30(2) . ? C6 C7 1.42(2) . ? C6 C10 1.45(2) . ? C7 C8 1.37(3) . ? C8 C9 1.32(3) . ? C10 N4 1.38(2) . ? C10 C14 1.42(2) . ? N4 C11 1.30(2) . ? C11 C12 1.38(2) . ? C11 C15 1.50(3) . ? C12 C13 1.36(3) . ? C13 C14 1.32(3) . ? C15 N5 1.46(3) . ? N5 C16 1.53(3) . ? C16 C17 1.42(3) . ? C17 N6 1.48(2) . ? N6 C18 1.46(3) . ? 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 N6 Cu N1 162.9(6) . . ? N6 Cu N5 85.7(7) . . ? N1 Cu N5 93.4(6) . . ? N6 Cu N2 90.9(6) . . ? N1 Cu N2 80.9(6) . . ? N5 Cu N2 148.3(6) . . ? N6 Cu N4 105.6(6) . . ? N1 Cu N4 90.4(5) . . ? N5 Cu N4 72.8(5) . . ? N2 Cu N4 137.9(5) . . ? N6 Cu N3 96.1(5) . . ? N1 Cu N3 95.9(5) . . ? N5 Cu N3 138.3(5) . . ? N2 Cu N3 73.4(5) . . ? N4 Cu N3 66.6(4) . . ? O13 Cl1 O14 115.5(24) . . ? O13 Cl1 O12 119.4(17) . . ? O14 Cl1 O12 103.8(17) . . ? O13 Cl1 O11 107.6(14) . . ? O14 Cl1 O11 101.1(17) . . ? O12 Cl1 O11 107.7(12) . . ? O22 Cl2 O23 104.3(25) . . ? O22 Cl2 O24 118.5(21) . . ? O23 Cl2 O24 96.4(23) . . ? O22 Cl2 O21 115.5(18) . . ? O23 Cl2 O21 109.0(17) . . ? O24 Cl2 O21 110.8(14) . . ? C1 N1 C2 115.1(17) . . ? C1 N1 Cu 117.1(12) . . ? C2 N1 Cu 106.9(12) . . ? C3 C2 N1 110.9(19) . . ? C2 C3 N2 112.4(18) . . ? C3 N2 C4 113.9(15) . . ? C3 N2 Cu 104.3(12) . . ? C4 N2 Cu 112.1(11) . . ? N2 C4 C5 113.8(14) . . ? N3 C5 C9 120.2(18) . . ? N3 C5 C4 116.1(14) . . ? C9 C5 C4 123.7(18) . . ? C6 N3 C5 121.5(13) . . ? C6 N3 Cu 122.2(10) . . ? C5 N3 Cu 116.0(11) . . ? N3 C6 C7 119.8(17) . . ? N3 C6 C10 115.8(13) . . ? C7 C6 C10 124.5(17) . . ? C8 C7 C6 118.0(18) . . ? C7 C8 C9 120.6(16) . . ? C8 C9 C5 119.8(19) . . ? N4 C10 C14 116.9(17) . . ? N4 C10 C6 112.6(13) . . ? C14 C10 C6 130.4(17) . . ? C11 N4 C10 119.4(14) . . ? C11 N4 Cu 117.8(11) . . ? C10 N4 Cu 122.3(10) . . ? N4 C11 C12 123.6(17) . . ? N4 C11 C15 113.6(15) . . ? C12 C11 C15 122.8(18) . . ? C13 C12 C11 118.6(18) . . ? C12 C13 C14 119.3(18) . . ? C13 C14 C10 122.2(19) . . ? N5 C15 C11 114.4(15) . . ? C15 N5 C16 109.6(17) . . ? C15 N5 Cu 115.5(11) . . ? C16 N5 Cu 103.1(12) . . ? C17 C16 N5 111.8(20) . . ? C16 C17 N6 112.3(16) . . ? C18 N6 C17 110.6(15) . . ? C18 N6 Cu 114.3(13) . . ? C17 N6 Cu 107.2(12) . . ? _refine_diff_density_max 0.820 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.134 #===END data_[Cu2(HL3)(\m-OH)(ClO4)2Br] _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; (Cu 2+)2, (C20 H29 N6 +1), (O H -1), (Cl O4 -1)3, Br -1, (H2 O)0.5 ; _chemical_formula_structural ; [(Cu)2 (C20 H29 N6) (O H) (BR) (Cl O4)2] (Cl O4) (H2 O)0.5 ; _chemical_formula_analytical ? _chemical_formula_sum 'C20 H31 Br Cl3 Cu2 N6 O13.50' _chemical_formula_weight 884.85 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.450(8) _cell_length_b 22.613(4) _cell_length_c 16.394(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.12(6) _cell_angle_gamma 90.00 _cell_volume 3073.8(34) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 13 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method ? _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 6.301 _exptl_absorpt_correction_type 'refdelf (Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.44 _exptl_absorpt_correction_T_max 0.53 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'P4 Siemens' _diffrn_measurement_method '\q/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3341 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 50.00 _reflns_number_total 3104 _reflns_number_observed 2268 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P4 Siemens' _computing_cell_refinement 'P4 Siemens' _computing_data_reduction 'P4 Siemens' _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 (Ver. 1.01\b)(Farrugia,1997)' _computing_publication_material ; SHELXL-93 (Sheldrick, 1993), PARST93 (Nardelli,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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1819P)^2^+28.4912P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3102 _refine_ls_number_parameters 400 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_obs 0.0920 _refine_ls_wR_factor_all 0.2971 _refine_ls_wR_factor_obs 0.2405 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.030 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.030 _refine_ls_shift/esd_max 0.052 _refine_ls_shift/esd_mean 0.003 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 Br Br -0.1865(3) 0.12535(9) 0.79627(12) 0.0834(8) Uani 1 d . . Cu1 Cu 0.0764(3) 0.05478(8) 0.75105(11) 0.0496(7) Uani 1 d . . Cu2 Cu 0.0027(3) 0.18335(9) 0.73721(14) 0.0662(9) Uani 1 d . . O1 O 0.0243(12) 0.1142(4) 0.6693(5) 0.056(3) Uani 1 d . . Cl1 Cl 0.3625(5) -0.0330(2) 0.6937(2) 0.0669(12) Uani 1 d . . O11 O 0.2853(20) -0.0724(6) 0.7410(9) 0.110(5) Uani 1 d . . O12 O 0.4987(16) -0.0067(8) 0.7443(8) 0.111(5) Uani 1 d . . O13 O 0.4120(15) -0.0622(6) 0.6267(7) 0.087(4) Uani 1 d . . O14 O 0.2525(16) 0.0145(6) 0.6607(7) 0.090(4) Uani 1 d . . Cl2 Cl 0.5891(9) 0.3437(3) -0.0332(3) 0.110(2) Uani 1 d . . O21 O 0.6889(24) 0.3732(9) 0.0310(10) 0.152(7) Uani 1 d . . O22 O 0.6492(32) 0.3329(10) -0.1022(11) 0.180(9) Uani 1 d . . O23 O 0.5477(84) 0.2961(18) -0.0014(23) 0.452(44) Uani 1 d . . O24 O 0.4602(36) 0.3748(23) -0.0559(16) 0.303(27) Uani 1 d . . Cl3 Cl -0.3108(12) 0.2673(3) 0.6157(6) 0.156(3) Uani 1 d . . O31 O -0.2917(33) 0.3047(11) 0.5560(22) 0.235(15) Uani 1 d . . O32 O -0.1910(29) 0.2237(9) 0.6250(10) 0.174(10) Uani 1 d . . O33 O -0.4816(44) 0.2516(13) 0.5843(24) 0.259(15) Uani 1 d . . O34 O -0.3309(66) 0.2919(21) 0.6955(25) 0.479(47) Uani 1 d . . C1 C -0.4197(25) 0.0941(11) 0.5593(13) 0.105(7) Uani 1 d . . H1A H -0.4395(30) 0.1350(12) 0.5694(46) 0.050 Uiso 1 calc R . H1B H -0.4495(32) 0.0703(26) 0.6025(32) 0.050 Uiso 1 calc R . H1C H -0.4827(26) 0.0825(32) 0.5065(20) 0.050 Uiso 1 calc R . N1 N -0.2521(17) 0.0858(6) 0.5585(8) 0.068(4) Uani 1 d . . C2 C -0.1974(26) 0.0219(9) 0.5598(10) 0.088(6) Uani 1 d . . H2A H -0.2597(26) 0.0020(9) 0.5117(10) 0.050 Uiso 1 calc R . H2B H -0.0854(26) 0.0213(9) 0.5538(10) 0.050 Uiso 1 calc R . C3 C -0.2110(25) -0.0118(9) 0.6326(12) 0.099(7) Uani 1 d . . H3A H -0.3045(25) 0.0029(9) 0.6526(12) 0.050 Uiso 1 calc R . H3B H -0.2342(25) -0.0524(9) 0.6152(12) 0.050 Uiso 1 calc R . N2 N -0.0820(19) -0.0129(6) 0.7003(7) 0.073(4) Uani 1 d . . H2 H -0.0118(19) -0.0336(6) 0.6756(7) 0.050 Uiso 1 calc R . C4 C -0.1020(21) -0.0572(7) 0.7627(10) 0.070(5) Uani 1 d . . H4A H -0.0820(21) -0.0964(7) 0.7427(10) 0.050 Uiso 1 calc R . H4B H -0.2117(21) -0.0561(7) 0.7723(10) 0.050 Uiso 1 calc R . C5 C 0.0174(20) -0.0445(7) 0.8449(9) 0.060(4) Uani 1 d . . C6 C 0.0256(21) -0.0803(7) 0.9151(10) 0.065(4) Uani 1 d . . H6 H -0.0398(21) -0.1135(7) 0.9138(10) 0.050 Uiso 1 calc R . C7 C 0.1319(21) -0.0653(8) 0.9855(10) 0.069(5) Uani 1 d . . H7 H 0.1464(21) -0.0905(8) 1.0312(10) 0.050 Uiso 1 calc R . C8 C 0.2194(20) -0.0126(7) 0.9901(9) 0.059(4) Uani 1 d . . C9 C 0.2022(18) 0.0207(6) 0.9158(9) 0.047(4) Uani 1 d . . N3 N 0.1008(13) 0.0032(5) 0.8459(6) 0.041(3) Uani 1 d . . C10 C 0.3301(22) 0.0091(10) 1.0596(9) 0.072(5) Uani 1 d . . H10 H 0.3455(22) -0.0119(10) 1.1093(9) 0.050 Uiso 1 calc R . C11 C 0.4145(23) 0.0600(9) 1.0553(10) 0.077(5) Uani 1 d . . H11 H 0.4817(23) 0.0744(9) 1.1029(10) 0.050 Uiso 1 calc R . C12 C 0.4013(21) 0.0911(7) 0.9798(10) 0.066(4) Uani 1 d . . C13 C 0.2917(18) 0.0734(7) 0.9091(8) 0.051(4) Uani 1 d . . N4 N 0.2714(14) 0.0999(5) 0.8334(7) 0.052(3) Uani 1 d . . C14 C 0.3640(21) 0.1459(6) 0.8241(10) 0.059(4) Uani 1 d . . C15 C 0.4780(19) 0.1673(7) 0.8929(11) 0.067(5) Uani 1 d . . H15 H 0.5448(19) 0.1988(7) 0.8858(11) 0.050 Uiso 1 calc R . C16 C 0.4901(21) 0.1419(8) 0.9692(11) 0.072(5) Uani 1 d . . H16 H 0.5582(21) 0.1585(8) 1.0148(11) 0.050 Uiso 1 calc R . C17 C 0.3561(20) 0.1720(7) 0.7403(11) 0.069(5) Uani 1 d . . H17A H 0.3469(20) 0.1407(7) 0.6992(11) 0.050 Uiso 1 calc R . H17B H 0.4544(20) 0.1938(7) 0.7390(11) 0.050 Uiso 1 calc R . N5 N 0.2146(17) 0.2123(5) 0.7197(9) 0.071(4) Uani 1 d . . H5 H 0.2017(17) 0.2188(5) 0.6640(9) 0.050 Uiso 1 calc R . C18 C 0.2484(29) 0.2720(10) 0.7591(14) 0.107(7) Uiso 1 d D . C19 C 0.0834(45) 0.3002(17) 0.7710(27) 0.097(13) Uiso 0.50 d PD . C19' C 0.1534(53) 0.2801(30) 0.8302(28) 0.151(21) Uiso 0.50 d PD . N6 N -0.0029(26) 0.2560(6) 0.8035(12) 0.110(6) Uani 1 d D . C20 C -0.0097(57) 0.2551(21) 0.8856(32) 0.222(18) Uiso 1 d . . O100 O 0.7763(87) 0.2253(35) 0.0750(44) 0.269(29) Uiso 0.50 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 Br 0.102(2) 0.0851(14) 0.0669(13) 0.0052(10) 0.0264(11) 0.0078(11) Cu1 0.0665(15) 0.0436(13) 0.0334(12) 0.0022(9) -0.0033(10) -0.0003(10) Cu2 0.088(2) 0.0489(15) 0.0591(15) 0.0026(11) 0.0070(12) 0.0063(12) O1 0.075(7) 0.050(6) 0.039(5) 0.016(4) -0.005(5) 0.010(5) Cl1 0.076(3) 0.080(3) 0.042(2) 0.000(2) 0.005(2) 0.009(2) O11 0.155(14) 0.082(9) 0.114(11) 0.021(8) 0.078(11) 0.023(9) O12 0.079(9) 0.166(15) 0.078(9) -0.020(9) -0.009(8) 0.010(9) O13 0.093(9) 0.106(10) 0.065(7) -0.007(7) 0.023(7) 0.026(7) O14 0.108(10) 0.088(9) 0.072(8) 0.009(7) 0.014(7) 0.030(8) Cl2 0.146(6) 0.119(5) 0.069(3) -0.030(3) 0.031(4) -0.026(4) O21 0.162(16) 0.196(19) 0.092(11) -0.045(12) 0.011(11) -0.056(14) O22 0.292(27) 0.172(18) 0.103(12) -0.039(12) 0.106(16) 0.014(18) O23 0.906(112) 0.279(37) 0.252(35) -0.166(32) 0.315(56) -0.418(61) O24 0.160(22) 0.604(80) 0.132(20) -0.059(30) -0.008(17) 0.147(36) Cl3 0.188(8) 0.090(5) 0.167(7) 0.039(5) -0.022(6) 0.037(5) O31 0.213(25) 0.162(19) 0.370(39) 0.143(25) 0.159(27) 0.072(18) O32 0.252(23) 0.147(16) 0.098(11) -0.006(11) -0.030(13) 0.117(17) O33 0.247(35) 0.198(29) 0.328(41) -0.028(28) 0.042(32) 0.010(26) O34 0.637(84) 0.417(57) 0.274(39) -0.191(41) -0.181(46) 0.413(63) C1 0.110(19) 0.121(18) 0.078(14) -0.009(13) 0.004(12) 0.003(15) N1 0.065(10) 0.075(10) 0.058(8) 0.000(7) -0.005(7) 0.004(8) C2 0.109(16) 0.098(15) 0.046(10) -0.018(10) -0.015(10) -0.001(12) C3 0.097(15) 0.090(14) 0.085(14) 0.024(12) -0.046(12) -0.026(12) N2 0.108(12) 0.059(8) 0.044(8) 0.004(6) -0.005(8) -0.031(8) C4 0.075(12) 0.063(11) 0.071(11) -0.008(9) 0.010(9) -0.011(9) C5 0.076(11) 0.061(11) 0.043(9) 0.005(8) 0.014(8) 0.009(10) C6 0.077(12) 0.051(10) 0.066(11) 0.006(9) 0.015(10) 0.000(9) C7 0.072(12) 0.078(13) 0.053(11) 0.019(9) 0.002(9) 0.007(10) C8 0.070(11) 0.069(11) 0.035(9) 0.001(8) 0.002(8) 0.023(9) C9 0.061(10) 0.029(8) 0.047(9) 0.001(7) 0.000(8) 0.011(7) N3 0.051(7) 0.029(6) 0.038(7) 0.006(5) -0.005(6) -0.004(6) C10 0.077(12) 0.112(16) 0.026(9) 0.018(9) 0.003(9) 0.033(12) C11 0.078(13) 0.100(15) 0.039(10) -0.029(10) -0.021(9) 0.008(12) C12 0.075(11) 0.059(11) 0.057(12) -0.014(9) -0.002(9) 0.001(10) C13 0.060(10) 0.055(9) 0.033(9) -0.006(7) -0.002(7) 0.011(8) N4 0.056(8) 0.059(8) 0.036(7) 0.000(6) -0.005(6) 0.010(7) C14 0.083(12) 0.036(8) 0.066(11) -0.008(8) 0.034(9) -0.018(9) C15 0.058(11) 0.062(10) 0.077(13) -0.023(10) 0.001(9) -0.022(9) C16 0.065(11) 0.071(12) 0.068(13) -0.029(10) -0.015(9) 0.008(10) C17 0.062(11) 0.066(11) 0.086(12) -0.026(10) 0.031(9) -0.034(9) N5 0.095(11) 0.022(6) 0.094(10) 0.005(6) 0.012(8) -0.007(7) N6 0.163(18) 0.042(9) 0.124(14) -0.034(9) 0.023(13) -0.020(10) _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. Weighted least-squares planes through the starred atoms (Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807). Equation of the plane: m1*X+m2*Y+m3*Z=d Plane 1 m1 = 0.78100(0.00265) m2 = -0.44497(0.00360) m3 = -0.43821(0.00345) D = -7.28323(0.03954) Atom d s d/s (d/s)**2 N2 * 0.2061 0.0146 14.126 199.540 N3 * -0.1359 0.0109 -12.417 154.183 N4 * 0.1357 0.0120 11.342 128.634 O1 * -0.0763 0.0099 -7.726 59.688 Cu1 0.0871 0.0021 41.577 1728.686 ============ Sum((d/s)**2) for starred atoms 542.045 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Plane 2 m1 = -0.55243(0.00219) m2 = 0.45489(0.00422) m3 = -0.69850(0.00270) D = -5.39160(0.04638) Atom d s d/s (d/s)**2 N5 * -0.2563 0.0140 -18.297 334.795 N6 * 0.4132 0.0193 21.413 458.512 Br * -0.0045 0.0022 -2.081 4.329 O1 * 0.1017 0.0093 10.883 118.449 Cu2 0.2693 0.0024 111.823 12504.299 ============ Sum((d/s)**2) for starred atoms 916.085 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Weighted least-squares lines through the starred atoms (Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600) m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes. X0,Y0,Z0 are the coordinates of the centroid of the set of atoms. Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3 Line 1 m1 = 0.71895(0.00350) X0 = -0.84246(0.00995) m2 = -0.36891(0.00469) Y0 = 0.78365(0.00920) m3 = -0.58908(0.00414) Z0 = 11.35485(0.00831) Atom d s d/s (d/s)**2 Cu1 * 0.0000 0.0027 0.001 0.000 Cu4 * 0.0000 0.0180 0.000 0.000 ============ Sum((d/s)**2) for starred atoms 0.000 Line 2 m1 = -0.53524(0.00847) X0 = -2.94923(0.01753) m2 = 0.38145(0.00781) Y0 = 4.60288(0.01415) m3 = -0.75367(0.00584) Z0 = 10.95640(0.01150) Atom d s d/s (d/s)**2 Cu2 * 0.0000 0.0034 0.003 0.000 O32 * 0.0000 0.0297 0.000 0.000 ============ Sum((d/s)**2) for starred atoms 0.000 Dihedral angles formed by LSQ-planes Plane - plane angle (e.s.d.) 1 2 109.13( 0.25) Angles formed by LSQ-lines Line - line angle (e.s.d.) 1 2 94.68( 0.49) Angles formed by lines and normals to planes Line - plane angle (e.s.d.) 1 1 10.33( 0.32) 1 2 98.83( 0.26) 2 1 104.92( 0.46) 2 2 5.36( 0.46) ; 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 Br Cu2 2.411(4) . ? Cu1 O1 1.889(8) . ? Cu1 N3 1.923(10) . ? Cu1 N2 2.096(12) . ? Cu1 N4 2.173(12) . ? Cu1 Cu2 2.973(3) . ? Cu2 O1 1.949(10) . ? Cu2 N6 1.975(14) . ? Cu2 N5 1.979(14) . ? Cu2 O32 2.39(2) . ? Cl1 O13 1.412(11) . ? Cl1 O12 1.413(14) . ? Cl1 O11 1.419(13) . ? Cl1 O14 1.456(12) . ? Cl2 O23 1.27(3) . ? Cl2 O24 1.29(3) . ? Cl2 O22 1.35(2) . ? Cl2 O21 1.39(2) . ? Cl3 O31 1.33(2) . ? Cl3 O32 1.40(2) . ? Cl3 O34 1.46(4) . ? Cl3 O33 1.48(3) . ? C1 N1 1.43(2) . ? N1 C2 1.52(2) . ? C2 C3 1.44(3) . ? C3 N2 1.40(2) . ? N2 C4 1.47(2) . ? C4 C5 1.55(2) . ? C5 N3 1.29(2) . ? C5 C6 1.40(2) . ? C6 C7 1.36(2) . ? C7 C8 1.40(2) . ? C8 C10 1.41(2) . ? C8 C9 1.42(2) . ? C9 N3 1.35(2) . ? C9 C13 1.43(2) . ? C10 C11 1.36(3) . ? C11 C12 1.41(2) . ? C12 C13 1.40(2) . ? C12 C16 1.40(2) . ? C13 N4 1.36(2) . ? N4 C14 1.33(2) . ? C14 C15 1.42(2) . ? C14 C17 1.48(2) . ? C15 C16 1.36(2) . ? C17 N5 1.49(2) . ? N5 C18 1.50(3) . ? C18 C19' 1.55(4) . ? C18 C19 1.58(4) . ? C19 C19' 1.13(7) . ? C19 N6 1.40(4) . ? C19' N6 1.42(4) . ? C19' C20 1.88(6) . ? N6 C20 1.36(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N3 168.3(5) . . ? O1 Cu1 N2 101.2(5) . . ? N3 Cu1 N2 80.8(5) . . ? O1 Cu1 N4 98.7(4) . . ? N3 Cu1 N4 80.3(5) . . ? N2 Cu1 N4 159.9(5) . . ? O1 Cu1 Cu2 40.0(3) . . ? N3 Cu1 Cu2 130.0(3) . . ? N2 Cu1 Cu2 125.1(4) . . ? N4 Cu1 Cu2 73.2(3) . . ? O1 Cu2 N6 175.3(7) . . ? O1 Cu2 N5 89.7(5) . . ? N6 Cu2 N5 85.6(7) . . ? O1 Cu2 O32 89.6(5) . . ? N6 Cu2 O32 91.2(7) . . ? N5 Cu2 O32 105.4(8) . . ? O1 Cu2 Br 86.3(3) . . ? N6 Cu2 Br 98.2(6) . . ? N5 Cu2 Br 158.0(4) . . ? O32 Cu2 Br 96.2(7) . . ? O1 Cu2 Cu1 38.5(2) . . ? N6 Cu2 Cu1 142.9(6) . . ? N5 Cu2 Cu1 98.8(4) . . ? O32 Cu2 Cu1 122.3(5) . . ? Br Cu2 Cu1 65.33(9) . . ? Cu1 O1 Cu2 101.5(4) . . ? O13 Cl1 O12 108.9(8) . . ? O13 Cl1 O11 111.6(8) . . ? O12 Cl1 O11 110.7(10) . . ? O13 Cl1 O14 108.6(7) . . ? O12 Cl1 O14 107.2(9) . . ? O11 Cl1 O14 109.8(9) . . ? O23 Cl2 O24 107.2(35) . . ? O23 Cl2 O22 111.6(20) . . ? O24 Cl2 O22 106.8(17) . . ? O23 Cl2 O21 105.8(22) . . ? O24 Cl2 O21 108.3(20) . . ? O22 Cl2 O21 116.9(15) . . ? O31 Cl3 O32 109.9(16) . . ? O31 Cl3 O34 118.0(27) . . ? O32 Cl3 O34 112.1(14) . . ? O31 Cl3 O33 98.4(20) . . ? O32 Cl3 O33 120.3(17) . . ? O34 Cl3 O33 97.4(29) . . ? Cl3 O32 Cu2 136.5(11) . . ? C1 N1 C2 115.1(17) . . ? C3 C2 N1 116.3(17) . . ? N2 C3 C2 119.5(17) . . ? C3 N2 C4 112.9(13) . . ? C3 N2 Cu1 130.0(11) . . ? C4 N2 Cu1 111.9(9) . . ? N2 C4 C5 109.7(13) . . ? N3 C5 C6 122.3(15) . . ? N3 C5 C4 115.6(13) . . ? C6 C5 C4 122.0(16) . . ? C7 C6 C5 118.3(16) . . ? C6 C7 C8 120.9(15) . . ? C7 C8 C10 126.9(15) . . ? C7 C8 C9 116.3(14) . . ? C10 C8 C9 116.7(16) . . ? N3 C9 C8 121.1(13) . . ? N3 C9 C13 116.1(12) . . ? C8 C9 C13 122.9(14) . . ? C5 N3 C9 120.9(12) . . ? C5 N3 Cu1 121.6(10) . . ? C9 N3 Cu1 117.3(9) . . ? C11 C10 C8 121.5(15) . . ? C10 C11 C12 120.8(15) . . ? C13 C12 C16 114.6(15) . . ? C13 C12 C11 120.9(16) . . ? C16 C12 C11 124.4(16) . . ? N4 C13 C12 125.4(15) . . ? N4 C13 C9 117.5(12) . . ? C12 C13 C9 116.9(14) . . ? C14 N4 C13 118.5(12) . . ? C14 N4 Cu1 133.5(10) . . ? C13 N4 Cu1 107.9(10) . . ? N4 C14 C15 120.0(14) . . ? N4 C14 C17 119.7(14) . . ? C15 C14 C17 120.2(14) . . ? C16 C15 C14 120.4(16) . . ? C15 C16 C12 120.8(15) . . ? C14 C17 N5 110.1(13) . . ? C17 N5 C18 112.0(14) . . ? C17 N5 Cu2 118.3(9) . . ? C18 N5 Cu2 109.7(12) . . ? N5 C18 C19' 110.4(27) . . ? N5 C18 C19 108.5(22) . . ? C19' C18 C19 42.3(26) . . ? C19' C19 N6 67.2(20) . . ? C19' C19 C18 67.3(18) . . ? N6 C19 C18 107.1(26) . . ? C19 C19' N6 65.6(20) . . ? C19 C19' C18 70.4(20) . . ? N6 C19' C18 108.0(29) . . ? C19 C19' C20 103.0(27) . . ? N6 C19' C20 46.1(20) . . ? C18 C19' C20 149.7(39) . . ? C20 N6 C19 120.7(30) . . ? C20 N6 C19' 85.1(29) . . ? C19 N6 C19' 47.2(28) . . ? C20 N6 Cu2 122.9(23) . . ? C19 N6 Cu2 108.3(21) . . ? C19' N6 Cu2 111.7(26) . . ? N6 C20 C19' 48.8(21) . . ? _refine_diff_density_max 0.773 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.170 #===END