Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Rita Delgado' _publ_contact_author_address ; ITQB - Instituto de Tecnologia Quimica e Biologica, UNL Apartado 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email DELGADO@ITQB.UNL.PT _publ_section_title ; Dicopper(II) complexes of a new di-p-xylyldioxatetraazamacrocycle and cascade species with dicarboxylate anions: thermodynamics and structural properties ; loop_ _publ_author_name 'Rita Delgado' 'Silvia Carvalho' 'M. Drew' 'Vitor Felix' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 632448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 Cu2 N4 O18' _chemical_formula_weight 877.80 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' 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 P21/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 11.211(15) _cell_length_b 12.976(17) _cell_length_c 13.812(18) _cell_angle_alpha 90.00 _cell_angle_beta 110.180(10) _cell_angle_gamma 90.00 _cell_volume 1886(4) _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 parallelopiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.786 _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 'Mar-research Image Plate' _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 10199 _diffrn_reflns_av_R_equivalents 0.1075 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.80 _reflns_number_total 3369 _reflns_number_gt 2145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Speck, 1999)' _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^)+(0.0308P)^2^+12.3843P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3369 _refine_ls_number_parameters 256 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1757 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.48847(10) 0.87089(9) 0.15372(7) 0.0432(3) Uani 1 d . . . C11 C 0.8736(10) 0.7648(8) 0.0926(9) 0.071(3) Uani 1 d . . . H11A H 0.9130 0.7182 0.0577 0.085 Uiso 1 calc R . . H11B H 0.9298 0.7720 0.1636 0.085 Uiso 1 calc R . . N12 N 0.7465(8) 0.7221(6) 0.0893(7) 0.056(2) Uani 1 d D . . H12 H 0.717(9) 0.763(6) 0.118(7) 0.067 Uiso 1 d D . . C13 C 0.7555(12) 0.6231(8) 0.1469(11) 0.094(4) Uani 1 d . . . H13A H 0.8065 0.5743 0.1249 0.113 Uiso 1 calc R . . H13B H 0.7972 0.6353 0.2201 0.113 Uiso 1 calc R . . C14 C 0.6273(12) 0.5785(8) 0.1284(11) 0.086(4) Uani 1 d . . . H14A H 0.5857 0.5653 0.0553 0.104 Uiso 1 calc R . . H14B H 0.6355 0.5135 0.1648 0.104 Uiso 1 calc R . . O15 O 0.5526(6) 0.6479(4) 0.1632(5) 0.0494(16) Uani 1 d . . . C16 C 0.4253(9) 0.6077(6) 0.1364(7) 0.052(2) Uani 1 d . . . H16A H 0.4268 0.5427 0.1714 0.062 Uiso 1 calc R . . H16B H 0.3895 0.5959 0.0626 0.062 Uiso 1 calc R . . C17 C 0.3469(9) 0.6838(7) 0.1680(7) 0.052(2) Uani 1 d . . . H17A H 0.3867 0.6977 0.2411 0.062 Uiso 1 calc R . . H17B H 0.2640 0.6539 0.1574 0.062 Uiso 1 calc R . . N18 N 0.3293(7) 0.7840(6) 0.1099(5) 0.0389(17) Uani 1 d D . . H18 H 0.302(7) 0.768(6) 0.0504(19) 0.047 Uiso 1 d D . . C19 C 0.2143(9) 0.8381(7) 0.1169(7) 0.048(2) Uani 1 d . . . H19A H 0.2249 0.8485 0.1889 0.058 Uiso 1 calc R . . H19B H 0.1402 0.7947 0.0866 0.058 Uiso 1 calc R . . C20 C 0.1920(7) 0.9406(7) 0.0627(6) 0.038(2) Uani 1 d . . . C21 C 0.1959(10) 1.0292(8) 0.1158(8) 0.064(3) Uani 1 d . . . H21 H 0.2139 1.0268 0.1867 0.077 Uiso 1 calc R . . C22 C 0.1733(11) 1.1233(9) 0.0656(9) 0.074(3) Uani 1 d . . . H22 H 0.1751 1.1829 0.1034 0.089 Uiso 1 calc R . . C23 C 0.1480(9) 1.1309(9) -0.0398(8) 0.058(3) Uani 1 d . . . C24 C 0.1434(10) 1.0416(9) -0.0936(8) 0.064(3) Uani 1 d . . . H24 H 0.1263 1.0443 -0.1644 0.077 Uiso 1 calc R . . C25 C 0.1641(9) 0.9471(8) -0.0435(7) 0.060(3) Uani 1 d . . . H25 H 0.1592 0.8870 -0.0814 0.072 Uiso 1 calc R . . O41 O 0.5055(6) 0.8659(5) 0.0180(4) 0.0459(14) Uani 1 d . . . O42 O 0.5104(5) 0.9597(4) -0.1174(4) 0.0430(15) Uani 1 d . . . C43 C 0.5044(7) 0.9505(6) -0.0292(6) 0.0347(19) Uani 1 d . . . O51 O 0.4854(6) 0.8811(6) 0.2936(4) 0.0621(19) Uani 1 d . . . C52 C 0.5918(10) 0.8608(8) 0.3640(7) 0.055(2) Uani 1 d . . . O53 O 0.6071(8) 0.8566(7) 0.4565(5) 0.092(3) Uani 1 d . . . C54 C 0.7026(9) 0.8402(6) 0.3257(7) 0.046(2) Uani 1 d . . . O55 O 0.6784(5) 0.8578(5) 0.2297(4) 0.0471(15) Uani 1 d . . . O56 O 0.8047(7) 0.8090(6) 0.3873(5) 0.075(2) Uani 1 d . . . O100 O 0.5474(10) 0.7238(8) -0.1361(7) 0.125(4) Uani 1 d . . . O200 O 0.3226(13) 0.9515(17) 0.4127(10) 0.215(8) Uani 1 d D . . H201 H 0.371(9) 0.95(2) 0.473(3) 0.258 Uiso 1 d D . . H202 H 0.369(10) 0.94(2) 0.380(8) 0.258 Uiso 1 d 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 Cu 0.0489(6) 0.0554(7) 0.0289(5) -0.0039(6) 0.0182(4) -0.0063(7) C11 0.055(7) 0.064(7) 0.110(9) 0.026(7) 0.049(7) 0.018(6) N12 0.069(6) 0.035(5) 0.080(6) 0.016(4) 0.047(5) 0.015(4) C13 0.114(10) 0.051(7) 0.152(12) 0.043(8) 0.091(10) 0.037(8) C14 0.108(10) 0.040(6) 0.142(11) 0.021(7) 0.082(9) 0.014(7) O15 0.065(4) 0.026(3) 0.064(4) 0.004(3) 0.031(3) -0.001(3) C16 0.075(7) 0.022(5) 0.058(6) -0.001(4) 0.022(5) -0.006(5) C17 0.066(7) 0.043(5) 0.047(5) 0.018(5) 0.021(5) -0.010(5) N18 0.044(4) 0.042(4) 0.030(3) 0.006(4) 0.013(3) -0.004(4) C19 0.054(6) 0.045(6) 0.053(5) -0.003(4) 0.029(5) 0.001(5) C20 0.027(5) 0.045(5) 0.050(5) 0.003(4) 0.024(4) -0.006(4) C21 0.094(8) 0.060(7) 0.062(6) 0.003(6) 0.056(6) 0.008(6) C22 0.100(9) 0.054(7) 0.097(8) -0.002(7) 0.071(7) 0.000(7) C23 0.047(6) 0.063(7) 0.076(7) 0.022(7) 0.036(5) 0.007(6) C24 0.076(8) 0.068(8) 0.044(6) 0.003(6) 0.016(5) -0.013(6) C25 0.072(7) 0.055(7) 0.048(6) -0.013(5) 0.014(5) -0.021(6) O41 0.065(4) 0.040(3) 0.038(3) 0.004(3) 0.025(3) -0.002(3) O42 0.064(4) 0.047(4) 0.024(3) -0.001(3) 0.022(3) -0.004(3) C43 0.032(5) 0.045(5) 0.026(4) -0.001(4) 0.009(4) -0.003(4) O51 0.067(5) 0.083(5) 0.040(3) -0.003(4) 0.022(3) 0.007(4) C52 0.065(7) 0.049(6) 0.049(5) 0.005(5) 0.018(5) 0.015(6) O53 0.111(6) 0.133(8) 0.030(3) 0.007(4) 0.021(4) 0.029(6) C54 0.058(6) 0.030(5) 0.041(5) -0.003(4) 0.006(4) 0.000(4) O55 0.050(4) 0.049(4) 0.042(3) 0.002(3) 0.015(3) -0.003(3) O56 0.070(5) 0.092(6) 0.049(4) 0.006(4) 0.004(4) 0.014(5) O100 0.144(9) 0.117(8) 0.142(8) -0.064(7) 0.086(7) -0.027(7) O200 0.191(14) 0.278(18) 0.163(11) -0.041(14) 0.044(10) 0.141(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O51 1.949(6) . ? Cu O41 1.950(6) . ? Cu N18 2.019(7) . ? Cu O55 2.030(6) . ? Cu O42 2.256(6) 3_675 ? C11 N12 1.515(12) . ? C11 C23 1.517(13) 3_675 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N12 C13 1.496(12) . ? N12 H12 0.8000(12) . ? C13 C14 1.487(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O15 1.421(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? O15 C16 1.443(10) . ? C16 C17 1.485(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N18 1.504(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N18 C19 1.500(11) . ? N18 H18 0.8000(14) . ? C19 C20 1.505(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.357(12) . ? C20 C25 1.392(12) . ? C21 C22 1.383(14) . ? C21 H21 0.9300 . ? C22 C23 1.386(14) . ? C22 H22 0.9300 . ? C23 C24 1.367(14) . ? C23 C11 1.517(13) 3_675 ? C24 C25 1.389(13) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O41 C43 1.275(9) . ? O42 C43 1.249(8) . ? O42 Cu 2.256(6) 3_675 ? C43 C43 1.538(16) 3_675 ? O51 C52 1.279(10) . ? C52 O53 1.231(10) . ? C52 C54 1.533(13) . ? C54 O56 1.235(10) . ? C54 O55 1.279(10) . ? O200 H201 0.8200(18) . ? O200 H202 0.820(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 O51 Cu O41 175.3(3) . . ? O51 Cu N18 91.1(3) . . ? O41 Cu N18 93.6(3) . . ? O51 Cu O55 82.4(3) . . ? O41 Cu O55 93.5(2) . . ? N18 Cu O55 140.3(3) . . ? O51 Cu O42 99.1(3) . 3_675 ? O41 Cu O42 79.0(2) . 3_675 ? N18 Cu O42 123.3(3) . 3_675 ? O55 Cu O42 96.4(2) . 3_675 ? N12 C11 C23 108.6(8) . 3_675 ? N12 C11 H11A 110.0 . . ? C23 C11 H11A 110.0 3_675 . ? N12 C11 H11B 110.0 . . ? C23 C11 H11B 110.0 3_675 . ? H11A C11 H11B 108.3 . . ? C13 N12 C11 114.1(8) . . ? C13 N12 H12 106(7) . . ? C11 N12 H12 107(7) . . ? C14 C13 N12 111.1(10) . . ? C14 C13 H13A 109.4 . . ? N12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? N12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? O15 C14 C13 110.0(9) . . ? O15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? O15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C14 O15 C16 109.3(7) . . ? O15 C16 C17 108.6(7) . . ? O15 C16 H16A 110.0 . . ? C17 C16 H16A 110.0 . . ? O15 C16 H16B 110.0 . . ? C17 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C16 C17 N18 113.5(7) . . ? C16 C17 H17A 108.9 . . ? N18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? N18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C19 N18 C17 109.1(6) . . ? C19 N18 Cu 114.2(6) . . ? C17 N18 Cu 112.5(5) . . ? C19 N18 H18 99(6) . . ? C17 N18 H18 105(6) . . ? Cu N18 H18 116(6) . . ? N18 C19 C20 112.4(7) . . ? N18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C25 118.2(9) . . ? C21 C20 C19 120.8(8) . . ? C25 C20 C19 121.0(8) . . ? C20 C21 C22 120.7(9) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 121.6(11) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 117.8(10) . . ? C24 C23 C11 121.6(9) . 3_675 ? C22 C23 C11 120.6(11) . 3_675 ? C23 C24 C25 120.6(9) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 121.1(10) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C43 O41 Cu 118.4(5) . . ? C43 O42 Cu 108.5(5) . 3_675 ? O42 C43 O41 125.9(7) . . ? O42 C43 C43 117.8(9) . 3_675 ? O41 C43 C43 116.3(8) . 3_675 ? C52 O51 Cu 114.1(6) . . ? O53 C52 O51 123.9(9) . . ? O53 C52 C54 120.8(9) . . ? O51 C52 C54 115.4(8) . . ? O56 C54 O55 126.0(9) . . ? O56 C54 C52 119.2(8) . . ? O55 C54 C52 114.8(8) . . ? C54 O55 Cu 111.1(6) . . ? H201 O200 H202 103.7(3) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.80 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.747 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.099 #==END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 632449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 Cl2 Cu2 N4 O10' _chemical_formula_weight 798.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 19.20(2) _cell_length_b 9.219(11) _cell_length_c 20.23(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.080(10) _cell_angle_gamma 90.00 _cell_volume 3572(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour Blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.811 _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 'Marresearch Image Plate' _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 21986 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.74 _reflns_number_total 6576 _reflns_number_gt 5464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Speck, 1999)' _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^)+(0.0326P)^2^+4.8499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6576 _refine_ls_number_parameters 433 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.16977(2) 0.39015(5) 0.21699(2) 0.02548(13) Uani 1 d . . . Cu2 Cu 0.38996(2) 0.80195(5) 0.38265(2) 0.02538(13) Uani 1 d . . . Cl1 Cl 0.49578(6) 0.69986(14) 0.37109(6) 0.0468(3) Uani 1 d . . . Cl2 Cl 0.23521(6) 0.18739(12) 0.19729(6) 0.0437(3) Uani 1 d . . . C11 C 0.1723(2) 0.2312(4) 0.3512(2) 0.0353(10) Uani 1 d . . . H11A H 0.1936 0.1509 0.3292 0.042 Uiso 1 calc R . . H11B H 0.1430 0.1911 0.3838 0.042 Uiso 1 calc R . . N12 N 0.12769(17) 0.3149(3) 0.30131(17) 0.0288(7) Uani 1 d . . . H12 H 0.1133 0.3950 0.3229 0.035 Uiso 1 calc R . . C13 C 0.0629(2) 0.2306(5) 0.2815(2) 0.0383(11) Uani 1 d . . . H13A H 0.0338 0.2248 0.3187 0.046 Uiso 1 calc R . . H13B H 0.0755 0.1326 0.2695 0.046 Uiso 1 calc R . . C14 C 0.0221(2) 0.3018(5) 0.2233(2) 0.0409(11) Uani 1 d . . . H14A H -0.0195 0.2463 0.2101 0.049 Uiso 1 calc R . . H14B H 0.0085 0.3995 0.2345 0.049 Uiso 1 calc R . . O15 O 0.06912(15) 0.3037(3) 0.17120(15) 0.0367(7) Uani 1 d . . . C16 C 0.0503(2) 0.3894(6) 0.1131(2) 0.0438(11) Uani 1 d . . . H16A H 0.0334 0.4842 0.1252 0.053 Uiso 1 calc R . . H16B H 0.0145 0.3413 0.0848 0.053 Uiso 1 calc R . . C17 C 0.1176(2) 0.4021(5) 0.0790(2) 0.0414(11) Uani 1 d . . . H17A H 0.1336 0.3064 0.0672 0.050 Uiso 1 calc R . . H17B H 0.1096 0.4582 0.0386 0.050 Uiso 1 calc R . . N18 N 0.17177(17) 0.4745(4) 0.12395(16) 0.0293(8) Uani 1 d . . . H18 H 0.1571 0.5679 0.1274 0.035 Uiso 1 calc R . . C19 C 0.2406(2) 0.4841(5) 0.0942(2) 0.0362(10) Uani 1 d . . . H19A H 0.2337 0.5172 0.0487 0.043 Uiso 1 calc R . . H19B H 0.2621 0.3889 0.0941 0.043 Uiso 1 calc R . . C20 C 0.2883(2) 0.5888(5) 0.1337(2) 0.0313(9) Uani 1 d . . . C21 C 0.2779(2) 0.7397(5) 0.1255(2) 0.0325(9) Uani 1 d . . . H21 H 0.2420 0.7737 0.0962 0.039 Uiso 1 calc R . . C22 C 0.3208(2) 0.8368(5) 0.1607(2) 0.0334(10) Uani 1 d . . . H22 H 0.3131 0.9358 0.1549 0.040 Uiso 1 calc R . . C23 C 0.3753(2) 0.7907(5) 0.20477(19) 0.0312(9) Uani 1 d . . . C24 C 0.3847(2) 0.6416(5) 0.2138(2) 0.0332(10) Uani 1 d . . . H24 H 0.4199 0.6081 0.2439 0.040 Uiso 1 calc R . . C25 C 0.3420(2) 0.5428(5) 0.1786(2) 0.0362(10) Uani 1 d . . . H25 H 0.3495 0.4440 0.1851 0.043 Uiso 1 calc R . . C26 C 0.4223(2) 0.9014(5) 0.2413(2) 0.0371(10) Uani 1 d . . . H26A H 0.4683 0.8599 0.2510 0.045 Uiso 1 calc R . . H26B H 0.4271 0.9858 0.2134 0.045 Uiso 1 calc R . . N27 N 0.39227(17) 0.9465(4) 0.30475(16) 0.0268(7) Uani 1 d . . . H27 H 0.3467 0.9679 0.2933 0.032 Uiso 1 calc R . . C28 C 0.4241(2) 1.0856(5) 0.3304(2) 0.0391(11) Uani 1 d . . . H28A H 0.4093 1.1644 0.3009 0.047 Uiso 1 calc R . . H28B H 0.4745 1.0787 0.3316 0.047 Uiso 1 calc R . . C29 C 0.4020(2) 1.1172(5) 0.3993(2) 0.0385(11) Uani 1 d . . . H29A H 0.4208 1.2096 0.4151 0.046 Uiso 1 calc R . . H29B H 0.3515 1.1202 0.3994 0.046 Uiso 1 calc R . . O30 O 0.42976(14) 1.0013(3) 0.43978(13) 0.0308(6) Uani 1 d . . . C31 C 0.4044(2) 0.9815(5) 0.5044(2) 0.0366(10) Uani 1 d . . . H31A H 0.3545 0.9990 0.5031 0.044 Uiso 1 calc R . . H31B H 0.4277 1.0474 0.5361 0.044 Uiso 1 calc R . . C32 C 0.4207(2) 0.8273(5) 0.5227(2) 0.0351(10) Uani 1 d . . . H32A H 0.4702 0.8093 0.5201 0.042 Uiso 1 calc R . . H32B H 0.4091 0.8094 0.5679 0.042 Uiso 1 calc R . . N33 N 0.37944(17) 0.7278(4) 0.47651(16) 0.0286(7) Uani 1 d . . . H33 H 0.3339 0.7423 0.4844 0.034 Uiso 1 calc R . . C34 C 0.3936(2) 0.5729(5) 0.4909(2) 0.0385(11) Uani 1 d . . . H34A H 0.3943 0.5560 0.5382 0.046 Uiso 1 calc R . . H34B H 0.4390 0.5466 0.4762 0.046 Uiso 1 calc R . . C35 C 0.3377(2) 0.4813(5) 0.4553(2) 0.0356(10) Uani 1 d . . . C36 C 0.2838(3) 0.4192(6) 0.4885(2) 0.0531(14) Uani 1 d . . . H36 H 0.2835 0.4297 0.5342 0.064 Uiso 1 calc R . . C37 C 0.2308(3) 0.3424(6) 0.4545(2) 0.0495(13) Uani 1 d . . . H37 H 0.1953 0.3032 0.4778 0.059 Uiso 1 calc R . . C38 C 0.2293(2) 0.3223(4) 0.3865(2) 0.0325(9) Uani 1 d . . . C39 C 0.2833(2) 0.3828(5) 0.3528(2) 0.0336(10) Uani 1 d . . . H39 H 0.2837 0.3708 0.3072 0.040 Uiso 1 calc R . . C40 C 0.3360(2) 0.4603(5) 0.3867(2) 0.0342(10) Uani 1 d . . . H40 H 0.3714 0.4996 0.3632 0.041 Uiso 1 calc R . . O51 O 0.16746(18) 0.5815(3) 0.25983(14) 0.0385(8) Uani 1 d . . . O52 O 0.11697(16) 0.7254(3) 0.18130(15) 0.0388(7) Uani 1 d . . . C53 C 0.14848(19) 0.7054(4) 0.23721(19) 0.0241(8) Uani 1 d . . . C54 C 0.1661(2) 0.8342(4) 0.28105(19) 0.0269(9) Uani 1 d D . . H54A H 0.1334 0.9115 0.2688 0.032 Uiso 1 calc R . . H54B H 0.2123 0.8682 0.2721 0.032 Uiso 1 calc R . . C55 C 0.16490(19) 0.8084(5) 0.35510(19) 0.0279(9) Uani 1 d D . . H55A H 0.1355 0.8822 0.3729 0.033 Uiso 1 calc R . . H55B H 0.1425 0.7156 0.3614 0.033 Uiso 1 calc R . . C56 C 0.23367(19) 0.8083(4) 0.39618(19) 0.0268(9) Uani 1 d . . . O57 O 0.23329(15) 0.7865(4) 0.45659(15) 0.0509(9) Uani 1 d . . . O58 O 0.28842(14) 0.8330(4) 0.36555(15) 0.0417(8) Uani 1 d . . . O100 O 0.0424(2) 0.5074(5) 0.3883(2) 0.0718(12) Uani 1 d D . . H101 H 0.0580(18) 0.547(7) 0.4223(18) 0.086 Uiso 1 d D . . H102 H -0.0001(6) 0.510(7) 0.391(2) 0.086 Uiso 1 d D . . O200 O 0.1071(2) 0.9832(4) 0.11724(17) 0.0550(9) Uani 1 d D . . H201 H 0.106(2) 0.914(4) 0.142(2) 0.066 Uiso 1 d D . . H202 H 0.140(2) 1.031(4) 0.133(2) 0.066 Uiso 1 d D . . O300 O 0.1059(2) 0.6720(6) 0.4957(2) 0.0727(13) Uani 1 d D . . H301 H 0.114(2) 0.610(5) 0.524(3) 0.087 Uiso 1 d D . . H302 H 0.1444(12) 0.702(6) 0.488(3) 0.087 Uiso 1 d D . . O400 O 0.0220(4) 0.2246(8) 0.4537(3) 0.135(2) 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 0.0281(3) 0.0214(2) 0.0278(3) -0.00404(19) 0.00805(19) -0.0004(2) Cu2 0.0194(2) 0.0338(3) 0.0232(3) -0.0032(2) 0.00357(18) -0.0031(2) Cl1 0.0307(6) 0.0629(8) 0.0474(7) -0.0073(6) 0.0071(5) 0.0123(5) Cl2 0.0442(7) 0.0279(6) 0.0609(8) -0.0105(5) 0.0162(5) 0.0064(5) C11 0.039(3) 0.022(2) 0.045(3) 0.0078(18) 0.007(2) -0.0054(18) N12 0.0296(18) 0.0198(17) 0.038(2) -0.0010(14) 0.0095(15) -0.0044(14) C13 0.032(2) 0.035(2) 0.050(3) -0.003(2) 0.012(2) -0.0073(19) C14 0.024(2) 0.052(3) 0.048(3) -0.006(2) 0.012(2) -0.004(2) O15 0.0287(16) 0.0423(18) 0.0399(18) -0.0055(14) 0.0068(13) -0.0002(13) C16 0.034(3) 0.055(3) 0.042(3) -0.007(2) -0.003(2) -0.006(2) C17 0.042(3) 0.053(3) 0.029(2) -0.012(2) 0.003(2) -0.009(2) N18 0.0305(19) 0.0335(19) 0.0248(18) -0.0084(14) 0.0075(14) -0.0027(15) C19 0.037(2) 0.046(3) 0.027(2) -0.0115(19) 0.0132(19) -0.006(2) C20 0.033(2) 0.039(2) 0.024(2) -0.0046(17) 0.0148(18) -0.0049(19) C21 0.031(2) 0.042(3) 0.025(2) -0.0024(18) 0.0056(17) 0.0027(19) C22 0.042(3) 0.031(2) 0.028(2) 0.0000(17) 0.0096(19) 0.0037(19) C23 0.034(2) 0.041(2) 0.020(2) -0.0011(17) 0.0143(17) -0.0069(19) C24 0.031(2) 0.042(3) 0.028(2) 0.0033(18) 0.0052(18) -0.0005(18) C25 0.039(3) 0.036(2) 0.035(2) 0.0041(19) 0.011(2) -0.002(2) C26 0.039(2) 0.048(3) 0.026(2) -0.0040(19) 0.0141(19) -0.015(2) N27 0.0208(17) 0.0339(18) 0.0261(18) -0.0028(14) 0.0045(14) -0.0065(14) C28 0.041(3) 0.035(3) 0.042(3) -0.0003(19) 0.004(2) -0.013(2) C29 0.036(2) 0.037(3) 0.041(3) -0.009(2) -0.007(2) -0.003(2) O30 0.0263(15) 0.0363(16) 0.0299(16) -0.0073(12) 0.0015(12) 0.0004(12) C31 0.029(2) 0.050(3) 0.032(2) -0.013(2) 0.0063(18) -0.006(2) C32 0.029(2) 0.050(3) 0.026(2) -0.0065(19) 0.0021(18) -0.0060(19) N33 0.0222(17) 0.039(2) 0.0247(18) -0.0011(14) 0.0012(14) -0.0048(15) C34 0.042(3) 0.044(3) 0.028(2) 0.0034(19) -0.007(2) -0.003(2) C35 0.041(3) 0.033(2) 0.032(2) 0.0031(18) -0.0017(19) -0.0013(19) C36 0.074(4) 0.059(3) 0.027(3) 0.000(2) 0.009(2) -0.021(3) C37 0.059(3) 0.058(3) 0.033(3) 0.004(2) 0.017(2) -0.022(3) C38 0.038(2) 0.025(2) 0.035(2) 0.0075(17) 0.0051(19) 0.0002(18) C39 0.042(3) 0.034(2) 0.025(2) 0.0036(17) 0.0028(18) -0.0028(19) C40 0.036(2) 0.033(2) 0.033(2) 0.0083(18) 0.0023(19) -0.0060(19) O51 0.070(2) 0.0197(15) 0.0267(16) 0.0024(11) 0.0088(15) 0.0058(14) O52 0.0477(19) 0.0361(17) 0.0311(17) -0.0043(13) -0.0085(14) 0.0104(14) C53 0.025(2) 0.025(2) 0.024(2) 0.0008(16) 0.0107(16) 0.0028(16) C54 0.030(2) 0.026(2) 0.024(2) 0.0004(16) -0.0022(17) -0.0037(16) C55 0.020(2) 0.038(2) 0.026(2) -0.0022(17) 0.0034(16) -0.0013(17) C56 0.0177(19) 0.036(2) 0.027(2) 0.0001(17) 0.0045(16) -0.0029(17) O57 0.0289(17) 0.101(3) 0.0235(17) 0.0069(17) 0.0032(13) -0.0098(18) O58 0.0168(14) 0.073(2) 0.0355(17) 0.0193(16) 0.0032(12) -0.0046(14) O100 0.062(3) 0.084(3) 0.072(3) -0.025(2) 0.018(2) -0.008(2) O200 0.075(3) 0.044(2) 0.044(2) 0.0031(16) -0.0130(18) 0.0008(18) O300 0.052(2) 0.122(4) 0.046(2) 0.018(2) 0.0119(19) -0.016(2) O400 0.150(6) 0.152(6) 0.103(5) 0.027(4) 0.001(4) 0.036(5) _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 O51 1.967(3) . ? Cu1 N18 2.040(4) . ? Cu1 N12 2.059(4) . ? Cu1 O15 2.230(4) . ? Cu1 Cl2 2.303(2) . ? Cu2 O58 1.976(4) . ? Cu2 N33 2.042(4) . ? Cu2 N27 2.067(4) . ? Cu2 Cl1 2.267(3) . ? Cu2 O30 2.274(3) . ? C11 N12 1.492(5) . ? C11 C38 1.518(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N12 C13 1.498(5) . ? N12 H12 0.9100 . ? C13 C14 1.516(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O15 1.435(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? O15 C16 1.440(6) . ? C16 C17 1.513(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N18 1.490(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N18 C19 1.493(5) . ? N18 H18 0.9100 . ? C19 C20 1.517(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.392(6) . ? C20 C21 1.413(6) . ? C21 C22 1.380(6) . ? C21 H21 0.9300 . ? C22 C23 1.393(6) . ? C22 H22 0.9300 . ? C23 C24 1.396(6) . ? C23 C26 1.518(6) . ? C24 C25 1.388(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 N27 1.503(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? N27 C28 1.497(5) . ? N27 H27 0.9100 . ? C28 C29 1.513(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O30 1.427(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? O30 C31 1.439(5) . ? C31 C32 1.496(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N33 1.496(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? N33 C34 1.479(6) . ? N33 H33 0.9100 . ? C34 C35 1.508(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.396(7) . ? C35 C40 1.401(6) . ? C36 C37 1.381(7) . ? C36 H36 0.9300 . ? C37 C38 1.386(6) . ? C37 H37 0.9300 . ? C38 C39 1.397(6) . ? C39 C40 1.381(6) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? O51 C53 1.274(5) . ? O52 C53 1.258(5) . ? C53 C54 1.506(5) . ? C54 C55 1.519(6) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.510(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 O57 1.239(5) . ? C56 O58 1.278(5) . ? O100 H101 0.819(10) . ? O100 H102 0.821(10) . ? O200 H201 0.819(10) . ? O200 H202 0.818(10) . ? O300 H301 0.820(10) . ? O300 H302 0.817(10) . ? 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 O51 Cu1 N18 93.85(14) . . ? O51 Cu1 N12 85.09(14) . . ? N18 Cu1 N12 158.02(14) . . ? O51 Cu1 O15 117.21(13) . . ? N18 Cu1 O15 79.95(13) . . ? N12 Cu1 O15 81.05(14) . . ? O51 Cu1 Cl2 146.49(11) . . ? N18 Cu1 Cl2 95.94(11) . . ? N12 Cu1 Cl2 96.96(11) . . ? O15 Cu1 Cl2 96.06(11) . . ? O58 Cu2 N33 92.85(13) . . ? O58 Cu2 N27 81.24(13) . . ? N33 Cu2 N27 159.07(13) . . ? O58 Cu2 Cl1 157.28(11) . . ? N33 Cu2 Cl1 96.07(10) . . ? N27 Cu2 Cl1 96.94(11) . . ? O58 Cu2 O30 105.29(13) . . ? N33 Cu2 O30 81.35(13) . . ? N27 Cu2 O30 80.91(14) . . ? Cl1 Cu2 O30 96.70(10) . . ? N12 C11 C38 113.1(3) . . ? N12 C11 H11A 109.0 . . ? C38 C11 H11A 109.0 . . ? N12 C11 H11B 109.0 . . ? C38 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 N12 C13 109.8(3) . . ? C11 N12 Cu1 119.7(3) . . ? C13 N12 Cu1 108.7(3) . . ? C11 N12 H12 105.9 . . ? C13 N12 H12 105.9 . . ? Cu1 N12 H12 105.9 . . ? N12 C13 C14 110.9(4) . . ? N12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O15 C14 C13 105.0(3) . . ? O15 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? O15 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C14 O15 C16 118.1(3) . . ? C14 O15 Cu1 105.7(3) . . ? C16 O15 Cu1 107.6(2) . . ? O15 C16 C17 104.0(4) . . ? O15 C16 H16A 111.0 . . ? C17 C16 H16A 111.0 . . ? O15 C16 H16B 111.0 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? N18 C17 C16 109.7(3) . . ? N18 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? N18 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C17 N18 C19 112.3(3) . . ? C17 N18 Cu1 109.5(3) . . ? C19 N18 Cu1 118.0(3) . . ? C17 N18 H18 105.3 . . ? C19 N18 H18 105.3 . . ? Cu1 N18 H18 105.3 . . ? N18 C19 C20 110.1(3) . . ? N18 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? N18 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.2 . . ? C25 C20 C21 118.0(4) . . ? C25 C20 C19 122.7(4) . . ? C21 C20 C19 119.3(4) . . ? C22 C21 C20 120.2(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 121.8(4) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C24 117.9(4) . . ? C22 C23 C26 120.0(4) . . ? C24 C23 C26 122.1(4) . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 121.2(4) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? N27 C26 C23 110.6(3) . . ? N27 C26 H26A 109.5 . . ? C23 C26 H26A 109.5 . . ? N27 C26 H26B 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 N27 C26 111.2(3) . . ? C28 N27 Cu2 108.5(3) . . ? C26 N27 Cu2 120.2(3) . . ? C28 N27 H27 105.2 . . ? C26 N27 H27 105.2 . . ? Cu2 N27 H27 105.2 . . ? N27 C28 C29 110.5(3) . . ? N27 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? N27 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? O30 C29 C28 105.5(4) . . ? O30 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O30 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? C29 O30 C31 118.7(3) . . ? C29 O30 Cu2 102.4(2) . . ? C31 O30 Cu2 103.7(2) . . ? O30 C31 C32 105.5(3) . . ? O30 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O30 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.8 . . ? N33 C32 C31 109.6(4) . . ? N33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? N33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 N33 C32 112.8(3) . . ? C34 N33 Cu2 118.5(3) . . ? C32 N33 Cu2 107.1(3) . . ? C34 N33 H33 105.9 . . ? C32 N33 H33 105.9 . . ? Cu2 N33 H33 105.9 . . ? N33 C34 C35 109.4(3) . . ? N33 C34 H34A 109.8 . . ? C35 C34 H34A 109.8 . . ? N33 C34 H34B 109.8 . . ? C35 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C36 C35 C40 117.0(4) . . ? C36 C35 C34 121.9(4) . . ? C40 C35 C34 121.0(4) . . ? C37 C36 C35 121.0(4) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 121.7(4) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C39 117.9(4) . . ? C37 C38 C11 120.3(4) . . ? C39 C38 C11 121.7(4) . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C35 121.9(4) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? C53 O51 Cu1 131.3(3) . . ? O52 C53 O51 124.2(4) . . ? O52 C53 C54 119.1(3) . . ? O51 C53 C54 116.7(4) . . ? C53 C54 C55 116.0(3) . . ? C53 C54 H54A 108.3 . . ? C55 C54 H54A 108.3 . . ? C53 C54 H54B 108.3 . . ? C55 C54 H54B 108.3 . . ? H54A C54 H54B 107.4 . . ? C56 C55 C54 118.0(3) . . ? C56 C55 H55A 107.8 . . ? C54 C55 H55A 107.8 . . ? C56 C55 H55B 107.8 . . ? C54 C55 H55B 107.8 . . ? H55A C55 H55B 107.1 . . ? O57 C56 O58 124.8(4) . . ? O57 C56 C55 118.5(3) . . ? O58 C56 C55 116.8(3) . . ? C56 O58 Cu2 136.4(3) . . ? H101 O100 H102 103.8(13) . . ? H201 O200 H202 104.0(13) . . ? H301 O300 H302 104.0(13) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.362 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.077