# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Samiran Mitra' C.R.Choudhury R.Karmakar C.-Z.Lu C.-D.Wu _publ_contact_author_name 'Dr Samiran Mitra' _publ_contact_author_address ; Dr Samiran Mitra Department of Chemistry Jadavpur University Calcutta 700 032 INDIA ; _publ_contact_author_email SMITRA_2002@YAHOO.COM _publ_section_title ; First report of singly phenoxo-bridged copper(II) dimeric complexes: synthesis, crystal structure and low-temperature magnetic behaviour study ; data_CR4 _database_code_CSD 214016 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 Cl Cu2 N5 O9 S' _chemical_formula_weight 745.18 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' S S 0.1246 0.1234 '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' _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 16.6049(3) _cell_length_b 13.7745(3) _cell_length_c 13.7888(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.184(1) _cell_angle_gamma 90.00 _cell_volume 3082.8(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1945 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 23.00 _exptl_crystal_description ? _exptl_crystal_colour Blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6221 _exptl_absorpt_correction_T_max 0.8878 _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 'SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 8518 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 23.00 _reflns_number_total 4281 _reflns_number_gt 2450 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+23.9900P] 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 SHELXL _refine_ls_extinction_coef 0.00000(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4281 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.1646 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.70135(7) 0.56431(9) 0.01697(9) 0.0438(4) Uani 1 1 d . . . Cu2 Cu 0.76605(7) 0.39657(9) 0.18528(9) 0.0430(4) Uani 1 1 d . . . S1 S 0.53919(17) 0.5661(2) 0.2535(2) 0.0556(8) Uani 1 1 d . . . Cl1 Cl 1.1298(3) 0.1552(4) -0.1259(3) 0.1023(14) Uani 1 1 d . . . O1 O 0.6059(4) 0.2303(5) -0.0638(6) 0.060(2) Uani 1 1 d . . . O2 O 0.8755(4) 0.3130(5) 0.1418(6) 0.060(2) Uani 1 1 d . . . O3 O 0.6864(4) 0.3203(5) 0.0936(5) 0.0490(18) Uani 1 1 d . . . O4 O 0.6380(4) 0.4363(5) -0.0694(5) 0.057(2) Uani 1 1 d . . . H4AO H 0.5952 0.4545 -0.1061 0.069 Uiso 1 1 calc R . . H4BO H 0.6607 0.3768 -0.0601 0.069 Uiso 1 1 d R . . O5 O 0.7922(4) 0.4725(4) 0.0735(5) 0.0398(17) Uani 1 1 d . . . O6 O 1.1685(13) 0.239(2) -0.120(2) 0.354(16) Uani 1 1 d . . . O7 O 1.0769(8) 0.1634(13) -0.2125(9) 0.197(7) Uani 1 1 d . . . O8 O 1.0916(10) 0.1618(13) -0.0511(10) 0.213(8) Uani 1 1 d . . . O9 O 1.1859(12) 0.0929(15) -0.1187(15) 0.304(13) Uani 1 1 d . . . N1 N 0.6523(5) 0.5433(6) 0.1321(7) 0.053(2) Uani 1 1 d . . . N2 N 0.6160(5) 0.6703(6) -0.0417(6) 0.048(2) Uani 1 1 d . . . N3 N 0.8397(5) 0.4808(6) 0.2931(6) 0.050(2) Uani 1 1 d . . . N4 N 0.7548(5) 0.3133(7) 0.2948(6) 0.051(2) Uani 1 1 d . . . N5 N 0.7613(5) 0.6101(6) -0.0799(6) 0.052(2) Uani 1 1 d . . . C1 C 0.6274(6) 0.1762(7) 0.0205(8) 0.047(3) Uani 1 1 d . . . C2 C 0.7292(6) 0.2250(8) 0.2848(8) 0.055(3) Uani 1 1 d . . . H2A H 0.7358 0.1884 0.3425 0.067 Uiso 1 1 calc R . . C3 C 0.7924(7) 0.3537(9) 0.3922(8) 0.070(4) Uani 1 1 d . . . H3A H 0.8103 0.3019 0.4395 0.084 Uiso 1 1 calc R . . H3B H 0.7531 0.3940 0.4167 0.084 Uiso 1 1 calc R . . C4 C 0.9715(7) 0.3684(9) -0.0676(10) 0.068(4) Uani 1 1 d . . . H4A H 1.0129 0.3454 -0.0976 0.081 Uiso 1 1 calc R . . C5 C 0.9279(7) 0.4487(9) -0.1042(8) 0.061(3) Uani 1 1 d . . . H5A H 0.9389 0.4801 -0.1597 0.074 Uiso 1 1 calc R . . C6 C 0.7252(8) 0.6963(8) -0.1332(9) 0.077(4) Uani 1 1 d . . . H6A H 0.7376 0.6984 -0.1988 0.093 Uiso 1 1 calc R . . H6B H 0.7469 0.7545 -0.0975 0.093 Uiso 1 1 calc R . . C7 C 0.6703(6) 0.2290(8) 0.1058(8) 0.044(3) Uani 1 1 d . . . C8 C 0.6056(6) 0.5531(7) 0.1833(7) 0.043(3) Uani 1 1 d . . . C9 C 0.9546(6) 0.3210(8) 0.0136(9) 0.058(3) Uani 1 1 d . . . H9A H 0.9835 0.2648 0.0367 0.069 Uiso 1 1 calc R . . C10 C 0.6742(7) 0.0777(8) 0.1984(10) 0.064(3) Uani 1 1 d . . . H10A H 0.6907 0.0449 0.2582 0.076 Uiso 1 1 calc R . . C11 C 0.6910(6) 0.1764(7) 0.1935(8) 0.049(3) Uani 1 1 d . . . C12 C 0.8661(6) 0.4841(7) -0.0581(7) 0.041(2) Uani 1 1 d . . . C13 C 0.5594(7) 0.1836(8) -0.1493(8) 0.072(4) Uani 1 1 d . . . H13A H 0.5486 0.2287 -0.2036 0.108 Uiso 1 1 calc R . . H13B H 0.5083 0.1610 -0.1357 0.108 Uiso 1 1 calc R . . H13C H 0.5901 0.1294 -0.1665 0.108 Uiso 1 1 calc R . . C14 C 0.8486(6) 0.4392(7) 0.0262(7) 0.038(2) Uani 1 1 d . . . C15 C 0.8237(6) 0.5704(8) -0.1020(8) 0.053(3) Uani 1 1 d . . . H15A H 0.8447 0.5999 -0.1520 0.063 Uiso 1 1 calc R . . C16 C 0.6343(8) 0.0293(8) 0.1177(10) 0.072(4) Uani 1 1 d . . . H16A H 0.6231 -0.0366 0.1216 0.087 Uiso 1 1 calc R . . C17 C 0.8959(6) 0.3554(7) 0.0609(8) 0.046(3) Uani 1 1 d . . . C18 C 0.6339(7) 0.6895(9) -0.1408(9) 0.072(4) Uani 1 1 d . . . H18A H 0.6079 0.7498 -0.1670 0.087 Uiso 1 1 calc R . . H18B H 0.6114 0.6376 -0.1860 0.087 Uiso 1 1 calc R . . C19 C 0.8653(7) 0.4136(9) 0.3783(9) 0.085(4) Uani 1 1 d . . . H19A H 0.8866 0.4506 0.4381 0.103 Uiso 1 1 calc R . . H19B H 0.9087 0.3712 0.3661 0.103 Uiso 1 1 calc R . . C20 C 0.7982(9) 0.5638(10) 0.3228(11) 0.130(7) Uani 1 1 d . . . H20A H 0.8357 0.5994 0.3728 0.195 Uiso 1 1 calc R . . H20B H 0.7520 0.5426 0.3491 0.195 Uiso 1 1 calc R . . H20C H 0.7792 0.6049 0.2664 0.195 Uiso 1 1 calc R . . C22 C 0.6100(7) 0.0791(8) 0.0276(10) 0.066(3) Uani 1 1 d . . . H22A H 0.5817 0.0461 -0.0281 0.079 Uiso 1 1 calc R . . C23 C 0.9103(7) 0.2201(8) 0.1726(9) 0.073(4) Uani 1 1 d . . . H23A H 0.9554 0.2073 0.1408 0.110 Uiso 1 1 calc R . . H23B H 0.8691 0.1707 0.1544 0.110 Uiso 1 1 calc R . . H23C H 0.9300 0.2198 0.2433 0.110 Uiso 1 1 calc R . . C24 C 0.9157(8) 0.5157(11) 0.2666(10) 0.105(5) Uani 1 1 d . . . H24A H 0.9465 0.5537 0.3202 0.158 Uiso 1 1 calc R . . H24B H 0.9021 0.5551 0.2080 0.158 Uiso 1 1 calc R . . H24C H 0.9482 0.4613 0.2543 0.158 Uiso 1 1 calc R . . C25 C 0.6280(7) 0.7570(7) 0.0222(9) 0.080(4) Uani 1 1 d . . . H25A H 0.5883 0.8056 -0.0053 0.120 Uiso 1 1 calc R . . H25B H 0.6826 0.7821 0.0263 0.120 Uiso 1 1 calc R . . H25C H 0.6210 0.7398 0.0875 0.120 Uiso 1 1 calc R . . C26 C 0.5298(7) 0.6383(8) -0.0572(9) 0.073(4) Uani 1 1 d . . . H26A H 0.4940 0.6908 -0.0844 0.109 Uiso 1 1 calc R . . H26B H 0.5178 0.6187 0.0051 0.109 Uiso 1 1 calc R . . H26C H 0.5211 0.5845 -0.1024 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0398(8) 0.0424(7) 0.0471(8) 0.0045(6) 0.0042(6) 0.0029(6) Cu2 0.0397(7) 0.0459(7) 0.0415(8) 0.0017(6) 0.0045(6) 0.0001(6) S1 0.0552(18) 0.0553(18) 0.0586(19) -0.0026(16) 0.0171(15) 0.0001(15) Cl1 0.059(3) 0.165(4) 0.076(3) -0.029(3) -0.002(2) 0.025(3) O1 0.070(5) 0.040(4) 0.062(5) -0.001(4) -0.007(4) -0.004(4) O2 0.054(5) 0.057(5) 0.069(6) 0.015(4) 0.016(4) 0.016(4) O3 0.052(5) 0.040(4) 0.050(5) 0.003(4) -0.001(4) -0.005(4) O4 0.058(5) 0.042(4) 0.063(5) -0.003(4) -0.008(4) 0.006(4) O5 0.035(4) 0.039(4) 0.044(4) 0.007(3) 0.006(3) 0.010(3) O6 0.169(19) 0.46(4) 0.40(4) 0.01(3) -0.03(2) -0.08(2) O7 0.125(10) 0.35(2) 0.096(9) -0.048(11) -0.024(8) 0.022(12) O8 0.220(17) 0.32(2) 0.115(11) 0.040(12) 0.072(11) 0.154(16) O9 0.27(2) 0.30(2) 0.33(2) -0.054(19) 0.041(18) 0.23(2) N1 0.045(6) 0.058(6) 0.053(6) -0.011(5) 0.003(5) 0.010(5) N2 0.040(5) 0.043(5) 0.053(6) 0.005(5) -0.004(4) 0.002(4) N3 0.052(6) 0.060(6) 0.032(5) 0.000(5) -0.004(4) -0.005(5) N4 0.040(5) 0.062(6) 0.048(6) 0.001(5) 0.004(4) -0.004(5) N5 0.045(6) 0.051(5) 0.052(6) 0.013(5) -0.004(5) 0.006(5) C1 0.055(7) 0.041(7) 0.046(7) -0.002(6) 0.014(6) 0.002(6) C2 0.058(8) 0.057(8) 0.056(8) 0.013(6) 0.022(6) 0.003(6) C3 0.067(8) 0.092(9) 0.045(7) 0.006(7) -0.001(6) -0.023(7) C4 0.052(8) 0.078(10) 0.079(10) -0.016(8) 0.025(7) -0.002(7) C5 0.069(8) 0.079(9) 0.040(7) -0.001(7) 0.022(6) -0.002(7) C6 0.086(10) 0.064(8) 0.079(9) 0.036(7) 0.011(8) 0.002(7) C7 0.041(6) 0.041(7) 0.047(7) 0.009(6) 0.004(5) 0.007(5) C8 0.040(6) 0.042(6) 0.040(7) -0.002(5) -0.004(5) 0.006(5) C9 0.040(7) 0.063(8) 0.069(9) -0.014(7) 0.009(6) 0.012(6) C10 0.078(9) 0.039(8) 0.080(9) 0.012(7) 0.028(7) 0.003(6) C11 0.045(7) 0.041(7) 0.064(8) -0.005(6) 0.020(6) 0.003(5) C12 0.034(6) 0.048(6) 0.037(6) -0.009(5) 0.001(5) -0.001(5) C13 0.065(8) 0.073(8) 0.065(8) -0.016(7) -0.013(7) -0.008(7) C14 0.030(6) 0.052(6) 0.032(6) -0.007(5) 0.006(5) -0.007(5) C15 0.043(7) 0.064(8) 0.051(7) 0.010(6) 0.011(6) -0.013(6) C16 0.105(11) 0.032(7) 0.083(10) -0.005(7) 0.029(9) -0.007(7) C17 0.039(6) 0.046(7) 0.054(7) -0.004(6) 0.014(6) 0.007(5) C18 0.073(9) 0.062(8) 0.074(10) 0.023(7) -0.003(7) 0.016(7) C19 0.068(9) 0.099(11) 0.077(10) -0.011(9) -0.012(7) -0.016(8) C20 0.123(13) 0.109(12) 0.131(14) -0.084(11) -0.036(10) 0.050(10) C22 0.060(8) 0.058(9) 0.082(10) 0.002(7) 0.019(7) -0.010(6) C23 0.065(8) 0.066(8) 0.088(10) 0.027(7) 0.016(7) 0.026(7) C24 0.079(10) 0.144(14) 0.086(11) -0.030(10) 0.006(8) -0.056(10) C25 0.075(9) 0.045(7) 0.109(11) -0.021(7) -0.007(8) 0.012(6) C26 0.054(8) 0.066(8) 0.088(10) 0.001(7) -0.012(7) 0.014(6) _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 N5 1.933(9) . ? Cu1 N1 1.952(10) . ? Cu1 O5 1.996(6) . ? Cu1 N2 2.077(8) . ? Cu1 O4 2.260(6) . ? Cu2 O3 1.936(6) . ? Cu2 N4 1.937(9) . ? Cu2 O5 1.985(6) . ? Cu2 N3 2.070(8) . ? Cu2 O2 2.334(7) . ? S1 C8 1.623(12) . ? Cl1 O9 1.255(13) . ? Cl1 O6 1.31(3) . ? Cl1 O8 1.322(13) . ? Cl1 O7 1.330(12) . ? O1 C1 1.363(11) . ? O1 C13 1.420(11) . ? O2 C17 1.364(12) . ? O2 C23 1.431(11) . ? O3 C7 1.303(11) . ? O5 C14 1.331(10) . ? N1 C8 1.162(11) . ? N2 C26 1.470(12) . ? N2 C25 1.472(12) . ? N2 C18 1.482(13) . ? N3 C20 1.438(13) . ? N3 C24 1.467(13) . ? N3 C19 1.485(14) . ? N4 C2 1.285(12) . ? N4 C3 1.466(13) . ? N5 C15 1.264(12) . ? N5 C6 1.458(12) . ? C1 C22 1.376(14) . ? C1 C7 1.438(13) . ? C2 C11 1.448(14) . ? C3 C19 1.510(15) . ? C4 C5 1.360(15) . ? C4 C9 1.375(15) . ? C5 C12 1.404(13) . ? C6 C18 1.501(15) . ? C7 C11 1.390(13) . ? C9 C17 1.368(13) . ? C10 C16 1.345(15) . ? C10 C11 1.393(14) . ? C12 C14 1.400(13) . ? C12 C15 1.447(13) . ? C14 C17 1.420(13) . ? C16 C22 1.403(15) . ? 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 N5 Cu1 N1 167.0(4) . . ? N5 Cu1 O5 91.1(3) . . ? N1 Cu1 O5 89.9(3) . . ? N5 Cu1 N2 84.9(4) . . ? N1 Cu1 N2 93.1(4) . . ? O5 Cu1 N2 174.2(3) . . ? N5 Cu1 O4 98.1(3) . . ? N1 Cu1 O4 94.9(3) . . ? O5 Cu1 O4 86.6(2) . . ? N2 Cu1 O4 98.0(3) . . ? O3 Cu2 N4 91.3(3) . . ? O3 Cu2 O5 90.6(3) . . ? N4 Cu2 O5 172.1(3) . . ? O3 Cu2 N3 172.8(3) . . ? N4 Cu2 N3 84.9(3) . . ? O5 Cu2 N3 94.0(3) . . ? O3 Cu2 O2 91.5(3) . . ? N4 Cu2 O2 96.7(3) . . ? O5 Cu2 O2 75.6(3) . . ? N3 Cu2 O2 95.0(3) . . ? O9 Cl1 O6 104.4(15) . . ? O9 Cl1 O8 117.2(13) . . ? O6 Cl1 O8 101.7(15) . . ? O9 Cl1 O7 117.9(12) . . ? O6 Cl1 O7 101.6(14) . . ? O8 Cl1 O7 111.1(9) . . ? C1 O1 C13 117.3(8) . . ? C17 O2 C23 118.1(8) . . ? C17 O2 Cu2 109.8(6) . . ? C23 O2 Cu2 130.8(6) . . ? C7 O3 Cu2 124.7(6) . . ? C14 O5 Cu2 119.4(6) . . ? C14 O5 Cu1 125.4(6) . . ? Cu2 O5 Cu1 111.5(3) . . ? C8 N1 Cu1 157.4(8) . . ? C26 N2 C25 109.6(9) . . ? C26 N2 C18 107.3(8) . . ? C25 N2 C18 112.3(9) . . ? C26 N2 Cu1 114.2(6) . . ? C25 N2 Cu1 110.0(6) . . ? C18 N2 Cu1 103.4(6) . . ? C20 N3 C24 107.4(11) . . ? C20 N3 C19 110.1(10) . . ? C24 N3 C19 106.5(9) . . ? C20 N3 Cu2 113.9(7) . . ? C24 N3 Cu2 114.5(7) . . ? C19 N3 Cu2 104.2(6) . . ? C2 N4 C3 121.7(10) . . ? C2 N4 Cu2 124.1(8) . . ? C3 N4 Cu2 113.4(7) . . ? C15 N5 C6 120.2(10) . . ? C15 N5 Cu1 126.4(7) . . ? C6 N5 Cu1 113.4(7) . . ? O1 C1 C22 124.8(10) . . ? O1 C1 C7 114.5(9) . . ? C22 C1 C7 120.6(11) . . ? N4 C2 C11 127.2(10) . . ? N4 C3 C19 106.8(9) . . ? C5 C4 C9 120.4(11) . . ? C4 C5 C12 119.8(11) . . ? N5 C6 C18 106.7(9) . . ? O3 C7 C11 126.5(10) . . ? O3 C7 C1 117.6(9) . . ? C11 C7 C1 115.9(10) . . ? N1 C8 S1 179.1(10) . . ? C17 C9 C4 120.7(11) . . ? C16 C10 C11 120.9(12) . . ? C7 C11 C10 122.4(11) . . ? C7 C11 C2 119.9(10) . . ? C10 C11 C2 117.7(11) . . ? C14 C12 C5 121.5(10) . . ? C14 C12 C15 122.9(9) . . ? C5 C12 C15 115.6(10) . . ? O5 C14 C12 123.0(9) . . ? O5 C14 C17 120.8(9) . . ? C12 C14 C17 116.2(9) . . ? N5 C15 C12 127.3(10) . . ? C10 C16 C22 119.3(11) . . ? O2 C17 C9 124.5(10) . . ? O2 C17 C14 114.1(9) . . ? C9 C17 C14 121.4(11) . . ? N2 C18 C6 110.1(9) . . ? N3 C19 C3 109.7(9) . . ? C1 C22 C16 120.9(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.650 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.110 data_CR10 _database_code_CSD 214017 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 Cl Cu2 N5 O10' _chemical_formula_weight 729.12 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 16.738(1) _cell_length_b 13.286(1) _cell_length_c 14.082(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.88 _cell_angle_gamma 90.00 _cell_volume 3026.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5758 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.04 _exptl_crystal_description ? _exptl_crystal_colour Blue _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5484 _exptl_absorpt_correction_T_max 0.6936 _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 'SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 9793 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5279 _reflns_number_gt 4361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+7.8950P] 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 SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5279 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0664 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.69658(3) 0.57159(4) 0.01212(4) 0.03667(18) Uani 1 1 d . . . Cu2 Cu 0.76589(3) 0.40240(4) 0.17899(4) 0.03432(17) Uani 1 1 d . . . Cl1 Cl 1.13606(11) 0.15547(17) -0.11949(13) 0.0807(5) Uani 1 1 d . . . O1 O 0.6117(2) 0.2160(3) -0.0675(2) 0.0567(9) Uani 1 1 d . . . O2 O 0.8746(2) 0.3135(3) 0.1373(3) 0.0529(9) Uani 1 1 d . . . O3 O 0.6882(2) 0.3179(2) 0.0864(2) 0.0437(8) Uani 1 1 d . . . O4 O 0.6267(2) 0.4362(3) -0.0760(3) 0.0542(9) Uani 1 1 d . . . H4AO H 0.5833 0.4559 -0.1130 0.065 Uiso 1 1 calc R . . H4BO H 0.6495 0.3767 -0.0668 0.065 Uiso 1 1 d R . . O5 O 0.78870(18) 0.4773(2) 0.0665(2) 0.0361(7) Uani 1 1 d . . . O6 O 1.1861(8) 0.2288(15) -0.1203(10) 0.373(12) Uani 1 1 d . . . O7 O 1.0836(5) 0.1643(8) -0.2124(5) 0.190(4) Uani 1 1 d . . . O8 O 1.0932(7) 0.1686(9) -0.0548(6) 0.234(6) Uani 1 1 d . . . O9 O 1.1815(10) 0.0773(9) -0.0933(13) 0.315(9) Uani 1 1 d . . . O10 O 0.5539(3) 0.5739(4) 0.2140(3) 0.0803(13) Uani 1 1 d . . . N1 N 0.6560(3) 0.5456(3) 0.1285(3) 0.0473(10) Uani 1 1 d . . . N2 N 0.6083(2) 0.6800(3) -0.0483(3) 0.0481(10) Uani 1 1 d . . . N3 N 0.8459(2) 0.4885(3) 0.2863(3) 0.0439(9) Uani 1 1 d . . . N4 N 0.7550(2) 0.3216(3) 0.2892(3) 0.0412(9) Uani 1 1 d . . . N5 N 0.7508(3) 0.6167(3) -0.0863(3) 0.0454(10) Uani 1 1 d . . . C1 C 0.6292(3) 0.1649(4) 0.0204(4) 0.0446(11) Uani 1 1 d . . . C2 C 0.7282(3) 0.2305(4) 0.2847(3) 0.0462(12) Uani 1 1 d . . . H2A H 0.7343 0.1961 0.3436 0.055 Uiso 1 1 calc R . . C3 C 0.7943(3) 0.3658(4) 0.3860(4) 0.0535(13) Uani 1 1 d . . . H3A H 0.8094 0.3136 0.4355 0.064 Uiso 1 1 calc R . . H3B H 0.7570 0.4126 0.4057 0.064 Uiso 1 1 calc R . . C4 C 0.9652(3) 0.3705(5) -0.0684(4) 0.0592(15) Uani 1 1 d . . . H4A H 1.0057 0.3469 -0.0972 0.071 Uiso 1 1 calc R . . C5 C 0.9195(3) 0.4523(4) -0.1063(4) 0.0541(13) Uani 1 1 d . . . H5A H 0.9288 0.4838 -0.1615 0.065 Uiso 1 1 calc R . . C6 C 0.7116(4) 0.7049(5) -0.1405(5) 0.0723(18) Uani 1 1 d . . . H6A H 0.7350 0.7658 -0.1066 0.087 Uiso 1 1 calc R . . H6B H 0.7208 0.7056 -0.2057 0.087 Uiso 1 1 calc R . . C7 C 0.6709(3) 0.2242(3) 0.1016(3) 0.0375(10) Uani 1 1 d . . . C8 C 0.6059(3) 0.5602(4) 0.1704(4) 0.0468(12) Uani 1 1 d . . . C9 C 0.9517(3) 0.3220(4) 0.0132(4) 0.0517(13) Uani 1 1 d . . . H9A H 0.9829 0.2658 0.0387 0.062 Uiso 1 1 calc R . . C10 C 0.6681(4) 0.0763(4) 0.2045(4) 0.0594(15) Uani 1 1 d . . . H10A H 0.6799 0.0463 0.2663 0.071 Uiso 1 1 calc R . . C11 C 0.6895(3) 0.1776(3) 0.1956(4) 0.0419(11) Uani 1 1 d . . . C12 C 0.8581(3) 0.4906(4) -0.0637(3) 0.0424(11) Uani 1 1 d . . . C13 C 0.5642(4) 0.1660(5) -0.1523(4) 0.0711(17) Uani 1 1 d . . . H13A H 0.5532 0.2115 -0.2072 0.107 Uiso 1 1 calc R . . H13B H 0.5129 0.1439 -0.1408 0.107 Uiso 1 1 calc R . . H13C H 0.5944 0.1089 -0.1665 0.107 Uiso 1 1 calc R . . C14 C 0.8441(3) 0.4426(3) 0.0203(3) 0.0359(10) Uani 1 1 d . . . C15 C 0.8131(3) 0.5763(4) -0.1087(4) 0.0490(12) Uani 1 1 d . . . H15A H 0.8308 0.6063 -0.1594 0.059 Uiso 1 1 calc R . . C16 C 0.6299(4) 0.0213(4) 0.1232(5) 0.0695(17) Uani 1 1 d . . . H16A H 0.6173 -0.0461 0.1299 0.083 Uiso 1 1 calc R . . C17 C 0.8918(3) 0.3570(4) 0.0569(3) 0.0423(11) Uani 1 1 d . . . C18 C 0.6238(4) 0.7001(5) -0.1472(5) 0.0765(19) Uani 1 1 d . . . H18A H 0.5989 0.6470 -0.1925 0.092 Uiso 1 1 calc R . . H18B H 0.5981 0.7632 -0.1729 0.092 Uiso 1 1 calc R . . C19 C 0.8703(4) 0.4198(5) 0.3732(4) 0.0677(17) Uani 1 1 d . . . H19A H 0.8952 0.4584 0.4318 0.081 Uiso 1 1 calc R . . H19B H 0.9106 0.3712 0.3631 0.081 Uiso 1 1 calc R . . C20 C 0.8081(5) 0.5798(5) 0.3111(5) 0.086(2) Uani 1 1 d . . . H20A H 0.8472 0.6150 0.3622 0.129 Uiso 1 1 calc R . . H20B H 0.7603 0.5627 0.3335 0.129 Uiso 1 1 calc R . . H20C H 0.7920 0.6219 0.2541 0.129 Uiso 1 1 calc R . . C22 C 0.6099(4) 0.0660(4) 0.0304(5) 0.0585(14) Uani 1 1 d . . . H22A H 0.5835 0.0286 -0.0246 0.070 Uiso 1 1 calc R . . C23 C 0.9096(4) 0.2181(4) 0.1696(5) 0.0688(17) Uani 1 1 d . . . H23A H 0.9538 0.2040 0.1395 0.103 Uiso 1 1 calc R . . H23B H 0.8679 0.1670 0.1514 0.103 Uiso 1 1 calc R . . H23C H 0.9308 0.2188 0.2397 0.103 Uiso 1 1 calc R . . C24 C 0.9233(4) 0.5164(6) 0.2611(5) 0.086(2) Uani 1 1 d . . . H24A H 0.9572 0.5556 0.3134 0.128 Uiso 1 1 calc R . . H24B H 0.9106 0.5552 0.2016 0.128 Uiso 1 1 calc R . . H24C H 0.9525 0.4565 0.2519 0.128 Uiso 1 1 calc R . . C25 C 0.6163(5) 0.7686(5) 0.0148(6) 0.090(2) Uani 1 1 d . . . H25A H 0.5750 0.8172 -0.0150 0.135 Uiso 1 1 calc R . . H25B H 0.6703 0.7974 0.0231 0.135 Uiso 1 1 calc R . . H25C H 0.6090 0.7493 0.0777 0.135 Uiso 1 1 calc R . . C26 C 0.5231(3) 0.6430(5) -0.0682(5) 0.0694(17) Uani 1 1 d . . . H26A H 0.4856 0.6963 -0.0962 0.104 Uiso 1 1 calc R . . H26B H 0.5119 0.6210 -0.0080 0.104 Uiso 1 1 calc R . . H26C H 0.5159 0.5878 -0.1135 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0381(3) 0.0353(3) 0.0366(3) 0.0063(2) 0.0097(2) 0.0038(2) Cu2 0.0385(3) 0.0336(3) 0.0301(3) 0.0009(2) 0.0074(2) -0.0009(2) Cl1 0.0610(9) 0.1101(14) 0.0677(10) -0.0186(10) 0.0106(8) 0.0060(10) O1 0.071(2) 0.053(2) 0.0392(19) -0.0046(16) 0.0010(17) -0.0105(18) O2 0.059(2) 0.050(2) 0.054(2) 0.0134(17) 0.0227(17) 0.0220(17) O3 0.0540(19) 0.0335(17) 0.0381(17) 0.0040(13) 0.0015(15) -0.0064(14) O4 0.065(2) 0.0405(19) 0.048(2) 0.0027(16) -0.0012(17) -0.0020(17) O5 0.0381(16) 0.0366(16) 0.0354(16) 0.0060(13) 0.0124(13) 0.0063(13) O6 0.214(12) 0.51(3) 0.291(15) 0.212(17) -0.118(11) -0.211(15) O7 0.165(7) 0.284(12) 0.095(5) -0.024(6) -0.017(5) -0.047(8) O8 0.282(12) 0.335(14) 0.110(6) 0.038(7) 0.092(7) 0.188(11) O9 0.349(17) 0.197(11) 0.46(2) 0.092(12) 0.216(17) 0.188(12) O10 0.073(3) 0.101(3) 0.083(3) -0.018(3) 0.048(3) -0.003(2) N1 0.048(2) 0.052(3) 0.043(2) 0.0065(19) 0.014(2) 0.003(2) N2 0.045(2) 0.040(2) 0.058(3) 0.0119(19) 0.0103(19) 0.0075(18) N3 0.046(2) 0.040(2) 0.042(2) -0.0032(18) 0.0055(18) -0.0021(18) N4 0.045(2) 0.045(2) 0.031(2) 0.0015(17) 0.0064(16) -0.0017(18) N5 0.052(2) 0.044(2) 0.042(2) 0.0126(18) 0.0163(19) -0.0002(19) C1 0.045(3) 0.039(3) 0.049(3) -0.005(2) 0.011(2) -0.002(2) C2 0.055(3) 0.049(3) 0.037(3) 0.015(2) 0.015(2) 0.007(2) C3 0.065(3) 0.060(3) 0.032(3) 0.000(2) 0.006(2) -0.010(3) C4 0.053(3) 0.070(4) 0.063(4) -0.016(3) 0.029(3) 0.005(3) C5 0.053(3) 0.070(4) 0.046(3) -0.005(3) 0.024(2) -0.002(3) C6 0.084(4) 0.060(4) 0.081(4) 0.033(3) 0.035(4) 0.017(3) C7 0.039(2) 0.029(2) 0.047(3) 0.0030(19) 0.014(2) 0.0028(18) C8 0.050(3) 0.045(3) 0.045(3) -0.003(2) 0.012(2) -0.004(2) C9 0.044(3) 0.054(3) 0.057(3) -0.012(3) 0.014(2) 0.006(2) C10 0.084(4) 0.040(3) 0.058(3) 0.011(3) 0.026(3) -0.005(3) C11 0.045(3) 0.038(2) 0.045(3) 0.004(2) 0.015(2) 0.001(2) C12 0.041(2) 0.048(3) 0.039(2) -0.003(2) 0.013(2) -0.006(2) C13 0.071(4) 0.082(4) 0.052(3) -0.016(3) 0.002(3) -0.024(3) C14 0.030(2) 0.041(2) 0.035(2) -0.0047(19) 0.0072(18) -0.0030(18) C15 0.051(3) 0.057(3) 0.043(3) 0.009(2) 0.019(2) -0.008(2) C16 0.097(5) 0.033(3) 0.083(4) 0.002(3) 0.031(4) -0.016(3) C17 0.043(3) 0.045(3) 0.040(3) -0.004(2) 0.012(2) 0.004(2) C18 0.081(5) 0.076(4) 0.068(4) 0.029(3) 0.012(3) 0.016(4) C19 0.073(4) 0.072(4) 0.047(3) -0.005(3) -0.005(3) -0.003(3) C20 0.095(5) 0.064(4) 0.079(5) -0.029(3) -0.012(4) 0.017(4) C22 0.066(4) 0.045(3) 0.065(4) -0.012(3) 0.019(3) -0.012(3) C23 0.087(4) 0.057(3) 0.065(4) 0.019(3) 0.023(3) 0.029(3) C24 0.065(4) 0.101(5) 0.090(5) -0.021(4) 0.019(4) -0.029(4) C25 0.086(5) 0.044(3) 0.118(6) -0.025(4) -0.012(4) 0.017(3) C26 0.044(3) 0.070(4) 0.084(4) 0.001(3) -0.001(3) 0.013(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 Cu1 N5 1.936(4) . ? Cu1 N1 1.959(4) . ? Cu1 O5 1.982(3) . ? Cu1 N2 2.082(4) . ? Cu1 O4 2.324(3) . ? Cu1 Cu2 3.2436(7) . ? Cu2 N4 1.934(4) . ? Cu2 O3 1.944(3) . ? Cu2 O5 1.989(3) . ? Cu2 N3 2.085(4) . ? Cu2 O2 2.367(3) . ? Cl1 O9 1.284(9) . ? Cl1 O6 1.287(12) . ? Cl1 O8 1.308(8) . ? Cl1 O7 1.381(7) . ? O1 C1 1.376(6) . ? O1 C13 1.419(6) . ? O2 C17 1.366(6) . ? O2 C23 1.422(6) . ? O3 C7 1.308(5) . ? O5 C14 1.344(5) . ? O10 C8 1.202(6) . ? N1 C8 1.158(6) . ? N2 C25 1.459(7) . ? N2 C26 1.466(7) . ? N2 C18 1.505(7) . ? N3 C20 1.451(7) . ? N3 C24 1.476(7) . ? N3 C19 1.497(7) . ? N4 C2 1.287(6) . ? N4 C3 1.474(6) . ? N5 C15 1.282(6) . ? N5 C6 1.459(7) . ? C1 C22 1.370(7) . ? C1 C7 1.416(7) . ? C2 C11 1.438(7) . ? C3 C19 1.511(8) . ? C4 C5 1.358(8) . ? C4 C9 1.385(8) . ? C5 C12 1.412(7) . ? C6 C18 1.449(9) . ? C7 C11 1.423(6) . ? C9 C17 1.383(7) . ? C10 C16 1.370(8) . ? C10 C11 1.407(7) . ? C12 C14 1.415(6) . ? C12 C15 1.421(7) . ? C14 C17 1.409(7) . ? C16 C22 1.395(8) . ? 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 N5 Cu1 N1 168.62(18) . . ? N5 Cu1 O5 90.65(15) . . ? N1 Cu1 O5 88.16(15) . . ? N5 Cu1 N2 84.68(17) . . ? N1 Cu1 N2 95.82(17) . . ? O5 Cu1 N2 174.42(14) . . ? N5 Cu1 O4 96.94(16) . . ? N1 Cu1 O4 94.31(16) . . ? O5 Cu1 O4 87.25(13) . . ? N2 Cu1 O4 96.33(15) . . ? N5 Cu1 Cu2 125.94(12) . . ? N1 Cu1 Cu2 53.72(12) . . ? O5 Cu1 Cu2 35.29(8) . . ? N2 Cu1 Cu2 149.27(12) . . ? O4 Cu1 Cu2 83.56(9) . . ? N4 Cu2 O3 91.91(15) . . ? N4 Cu2 O5 173.64(14) . . ? O3 Cu2 O5 89.25(13) . . ? N4 Cu2 N3 84.14(16) . . ? O3 Cu2 N3 175.86(15) . . ? O5 Cu2 N3 94.81(14) . . ? N4 Cu2 O2 99.15(14) . . ? O3 Cu2 O2 88.31(14) . . ? O5 Cu2 O2 74.63(12) . . ? N3 Cu2 O2 93.52(15) . . ? N4 Cu2 Cu1 151.21(12) . . ? O3 Cu2 Cu1 82.01(9) . . ? O5 Cu2 Cu1 35.15(8) . . ? N3 Cu2 Cu1 100.88(11) . . ? O2 Cu2 Cu1 108.71(8) . . ? O9 Cl1 O6 106.0(11) . . ? O9 Cl1 O8 107.4(8) . . ? O6 Cl1 O8 112.3(11) . . ? O9 Cl1 O7 121.7(9) . . ? O6 Cl1 O7 100.6(7) . . ? O8 Cl1 O7 108.6(6) . . ? C1 O1 C13 118.1(4) . . ? C17 O2 C23 119.0(4) . . ? C17 O2 Cu2 109.5(3) . . ? C23 O2 Cu2 130.2(3) . . ? C7 O3 Cu2 125.3(3) . . ? C14 O5 Cu1 126.5(3) . . ? C14 O5 Cu2 120.8(3) . . ? Cu1 O5 Cu2 109.56(13) . . ? C8 N1 Cu1 148.0(4) . . ? C25 N2 C26 108.6(5) . . ? C25 N2 C18 114.2(5) . . ? C26 N2 C18 105.8(5) . . ? C25 N2 Cu1 111.4(4) . . ? C26 N2 Cu1 113.6(3) . . ? C18 N2 Cu1 103.2(3) . . ? C20 N3 C24 108.2(5) . . ? C20 N3 C19 110.9(5) . . ? C24 N3 C19 106.2(5) . . ? C20 N3 Cu2 113.2(3) . . ? C24 N3 Cu2 113.8(4) . . ? C19 N3 Cu2 104.3(3) . . ? C2 N4 C3 119.2(4) . . ? C2 N4 Cu2 125.8(3) . . ? C3 N4 Cu2 114.2(3) . . ? C15 N5 C6 119.5(4) . . ? C15 N5 Cu1 127.4(3) . . ? C6 N5 Cu1 113.1(4) . . ? C22 C1 O1 124.4(5) . . ? C22 C1 C7 122.2(5) . . ? O1 C1 C7 113.5(4) . . ? N4 C2 C11 125.2(4) . . ? N4 C3 C19 105.5(4) . . ? C5 C4 C9 120.2(5) . . ? C4 C5 C12 121.3(5) . . ? C18 C6 N5 108.1(5) . . ? O3 C7 C1 118.9(4) . . ? O3 C7 C11 124.2(4) . . ? C1 C7 C11 116.9(4) . . ? N1 C8 O10 179.0(6) . . ? C17 C9 C4 120.2(5) . . ? C16 C10 C11 120.7(5) . . ? C10 C11 C7 120.0(5) . . ? C10 C11 C2 117.2(5) . . ? C7 C11 C2 122.7(4) . . ? C5 C12 C14 119.2(5) . . ? C5 C12 C15 117.3(4) . . ? C14 C12 C15 123.5(4) . . ? O5 C14 C17 119.8(4) . . ? O5 C14 C12 122.2(4) . . ? C17 C14 C12 118.0(4) . . ? N5 C15 C12 126.6(4) . . ? C10 C16 C22 120.3(5) . . ? O2 C17 C9 123.8(5) . . ? O2 C17 C14 115.1(4) . . ? C9 C17 C14 121.1(5) . . ? C6 C18 N2 111.1(5) . . ? N3 C19 C3 109.0(5) . . ? C1 C22 C16 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.804 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.083 data_cr11a _database_code_CSD 214955 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 Cl Cu2 N7 O9' _chemical_formula_weight 729.13 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' Cl Cl 0.1484 0.1585 '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 16.6748(4) _cell_length_b 13.3188(3) _cell_length_c 14.0639(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.699(1) _cell_angle_gamma 90.00 _cell_volume 3021.2(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5754 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.10 _exptl_crystal_description ? _exptl_crystal_colour Blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7795 _exptl_absorpt_correction_T_max 1.0000 _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 'SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 _diffrn_reflns_number 9445 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5272 _reflns_number_gt 4322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+11.5028P] 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 SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5272 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_r_factor_ref 0.0731 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.69593(4) 0.56795(5) 0.01243(4) 0.03571(19) Uani 1 1 d . . . Cu2 Cu 0.76553(4) 0.39886(5) 0.17891(4) 0.03328(19) Uani 1 1 d . . . Cl1 Cl 1.13702(12) 0.1558(2) -0.11991(15) 0.0828(6) Uani 1 1 d . . . O1 O 0.6133(3) 0.2120(3) -0.0689(3) 0.0546(11) Uani 1 1 d . . . O2 O 0.8768(2) 0.3138(3) 0.1373(3) 0.0507(10) Uani 1 1 d . . . O3 O 0.6904(2) 0.3129(3) 0.0857(2) 0.0414(9) Uani 1 1 d . . . O4 O 0.6291(2) 0.4318(3) -0.0761(3) 0.0492(10) Uani 1 1 d . . . H4A H 0.5855 0.4505 -0.1134 0.059 Uiso 1 1 calc R . . H4B H 0.6519 0.3724 -0.0669 0.059 Uiso 1 1 d R . . O5 O 0.7890(2) 0.4757(2) 0.0666(2) 0.0344(8) Uani 1 1 d . . . O6 O 1.1867(8) 0.2286(16) -0.1254(11) 0.362(13) Uani 1 1 d . . . O7 O 1.0835(6) 0.1607(10) -0.2112(6) 0.214(5) Uani 1 1 d . . . O8 O 1.0960(8) 0.1724(10) -0.0535(7) 0.239(7) Uani 1 1 d . . . O9 O 1.1836(11) 0.0807(10) -0.0898(13) 0.311(9) Uani 1 1 d . . . N1 N 0.6596(3) 0.5326(4) 0.1311(3) 0.0439(11) Uani 1 1 d . . . N2 N 0.6062(3) 0.6732(3) -0.0461(3) 0.0452(11) Uani 1 1 d . . . N3 N 0.8447(3) 0.4856(3) 0.2870(3) 0.0418(10) Uani 1 1 d . . . N4 N 0.7553(3) 0.3159(3) 0.2892(3) 0.0403(10) Uani 1 1 d . . . N5 N 0.7511(3) 0.6164(3) -0.0849(3) 0.0419(10) Uani 1 1 d . . . N6 N 0.6069(3) 0.5626(3) 0.1666(3) 0.0426(11) Uani 1 1 d . . . N7 N 0.5559(3) 0.5894(5) 0.2038(4) 0.0675(16) Uani 1 1 d . . . C1 C 0.6296(3) 0.1611(4) 0.0186(4) 0.0416(12) Uani 1 1 d . . . C2 C 0.7286(3) 0.2257(4) 0.2829(4) 0.0441(13) Uani 1 1 d . . . H2A H 0.7350 0.1905 0.3415 0.053 Uiso 1 1 calc R . . C3 C 0.7946(4) 0.3600(5) 0.3855(4) 0.0513(15) Uani 1 1 d . . . H3A H 0.8108 0.3077 0.4347 0.062 Uiso 1 1 calc R . . H3B H 0.7565 0.4052 0.4060 0.062 Uiso 1 1 calc R . . C4 C 0.9669(4) 0.3716(5) -0.0697(5) 0.0577(16) Uani 1 1 d . . . H4A' H 1.0074 0.3486 -0.0993 0.069 Uiso 1 1 calc R . . C5 C 0.9202(4) 0.4531(5) -0.1067(4) 0.0534(15) Uani 1 1 d . . . H5A H 0.9293 0.4852 -0.1617 0.064 Uiso 1 1 calc R . . C6 C 0.7108(4) 0.7056(5) -0.1366(5) 0.0652(18) Uani 1 1 d . . . H6A H 0.7208 0.7097 -0.2015 0.078 Uiso 1 1 calc R . . H6B H 0.7326 0.7658 -0.1003 0.078 Uiso 1 1 calc R . . C7 C 0.6720(3) 0.2195(4) 0.1003(4) 0.0361(11) Uani 1 1 d . . . C9 C 0.9539(3) 0.3228(5) 0.0124(4) 0.0502(14) Uani 1 1 d . . . H9A H 0.9857 0.2670 0.0379 0.060 Uiso 1 1 calc R . . C10 C 0.6686(4) 0.0718(4) 0.2019(5) 0.0564(16) Uani 1 1 d . . . H10A H 0.6817 0.0411 0.2633 0.068 Uiso 1 1 calc R . . C11 C 0.6897(3) 0.1734(4) 0.1939(4) 0.0391(12) Uani 1 1 d . . . C12 C 0.8586(3) 0.4899(4) -0.0637(4) 0.0402(12) Uani 1 1 d . . . C13 C 0.5656(4) 0.1625(6) -0.1546(5) 0.0678(19) Uani 1 1 d . . . H13A H 0.5548 0.2083 -0.2091 0.102 Uiso 1 1 calc R . . H13B H 0.5141 0.1402 -0.1434 0.102 Uiso 1 1 calc R . . H13C H 0.5960 0.1057 -0.1691 0.102 Uiso 1 1 calc R . . C14 C 0.8444(3) 0.4422(4) 0.0205(4) 0.0351(11) Uani 1 1 d . . . C15 C 0.8133(3) 0.5770(4) -0.1070(4) 0.0464(14) Uani 1 1 d . . . H15A H 0.8316 0.6081 -0.1568 0.056 Uiso 1 1 calc R . . C16 C 0.6294(4) 0.0182(5) 0.1215(5) 0.0647(18) Uani 1 1 d . . . H16A H 0.6159 -0.0487 0.1285 0.078 Uiso 1 1 calc R . . C17 C 0.8934(3) 0.3574(4) 0.0562(4) 0.0406(12) Uani 1 1 d . . . C18 C 0.6209(4) 0.6961(5) -0.1444(5) 0.0637(18) Uani 1 1 d . . . H18A H 0.5979 0.6428 -0.1903 0.076 Uiso 1 1 calc R . . H18B H 0.5932 0.7582 -0.1695 0.076 Uiso 1 1 calc R . . C19 C 0.8698(4) 0.4164(5) 0.3730(5) 0.0645(18) Uani 1 1 d . . . H19A H 0.8940 0.4546 0.4320 0.077 Uiso 1 1 calc R . . H19B H 0.9111 0.3693 0.3624 0.077 Uiso 1 1 calc R . . C20 C 0.8043(5) 0.5751(5) 0.3127(6) 0.083(2) Uani 1 1 d . . . H20A H 0.8426 0.6113 0.3637 0.125 Uiso 1 1 calc R . . H20B H 0.7569 0.5557 0.3354 0.125 Uiso 1 1 calc R . . H20C H 0.7868 0.6172 0.2558 0.125 Uiso 1 1 calc R . . C22 C 0.6093(4) 0.0622(4) 0.0288(5) 0.0544(15) Uani 1 1 d . . . H22A H 0.5822 0.0251 -0.0259 0.065 Uiso 1 1 calc R . . C23 C 0.9121(5) 0.2185(5) 0.1688(5) 0.070(2) Uani 1 1 d . . . H23A H 0.9563 0.2049 0.1382 0.105 Uiso 1 1 calc R . . H23B H 0.8704 0.1675 0.1504 0.105 Uiso 1 1 calc R . . H23C H 0.9335 0.2187 0.2389 0.105 Uiso 1 1 calc R . . C24 C 0.9209(4) 0.5172(6) 0.2614(6) 0.080(2) Uani 1 1 d . . . H24A H 0.9543 0.5563 0.3141 0.120 Uiso 1 1 calc R . . H24B H 0.9069 0.5570 0.2026 0.120 Uiso 1 1 calc R . . H24C H 0.9515 0.4590 0.2507 0.120 Uiso 1 1 calc R . . C25 C 0.6149(5) 0.7629(5) 0.0167(6) 0.074(2) Uani 1 1 d . . . H25A H 0.5736 0.8114 -0.0131 0.111 Uiso 1 1 calc R . . H25B H 0.6691 0.7913 0.0242 0.111 Uiso 1 1 calc R . . H25C H 0.6078 0.7445 0.0801 0.111 Uiso 1 1 calc R . . C26 C 0.5207(3) 0.6355(5) -0.0647(5) 0.0577(16) Uani 1 1 d . . . H26A H 0.4827 0.6881 -0.0927 0.087 Uiso 1 1 calc R . . H26B H 0.5102 0.6138 -0.0039 0.087 Uiso 1 1 calc R . . H26C H 0.5135 0.5800 -0.1096 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0366(4) 0.0346(4) 0.0357(3) 0.0063(3) 0.0088(3) 0.0030(3) Cu2 0.0361(3) 0.0333(3) 0.0295(3) 0.0014(2) 0.0066(2) -0.0005(3) Cl1 0.0603(11) 0.1144(17) 0.0701(12) -0.0219(12) 0.0097(9) 0.0100(11) O1 0.067(3) 0.053(2) 0.037(2) -0.0021(18) 0.0007(19) -0.012(2) O2 0.051(2) 0.051(2) 0.054(2) 0.0135(19) 0.0197(19) 0.0226(19) O3 0.049(2) 0.035(2) 0.0351(19) 0.0020(15) 0.0021(16) -0.0071(16) O4 0.057(2) 0.038(2) 0.048(2) 0.0032(17) 0.0038(18) 0.0011(18) O5 0.0347(18) 0.0369(19) 0.0340(18) 0.0044(15) 0.0132(14) 0.0038(15) O6 0.198(12) 0.50(3) 0.296(17) 0.203(18) -0.103(12) -0.191(16) O7 0.170(9) 0.350(16) 0.098(6) -0.052(8) -0.011(6) -0.058(10) O8 0.290(14) 0.334(16) 0.116(7) 0.033(8) 0.092(8) 0.185(13) O9 0.362(19) 0.209(12) 0.43(2) 0.113(14) 0.223(18) 0.198(13) N1 0.040(2) 0.050(3) 0.044(3) 0.008(2) 0.017(2) 0.007(2) N2 0.045(3) 0.038(2) 0.050(3) 0.008(2) 0.008(2) 0.007(2) N3 0.042(2) 0.042(3) 0.039(2) -0.002(2) 0.0054(19) -0.001(2) N4 0.044(2) 0.044(3) 0.031(2) 0.0023(19) 0.0052(19) -0.003(2) N5 0.044(3) 0.040(3) 0.043(2) 0.010(2) 0.013(2) -0.004(2) N6 0.042(3) 0.045(3) 0.038(2) -0.005(2) 0.006(2) -0.002(2) N7 0.056(3) 0.086(4) 0.067(4) -0.015(3) 0.028(3) 0.007(3) C1 0.043(3) 0.037(3) 0.044(3) -0.004(2) 0.009(2) -0.003(2) C2 0.052(3) 0.047(3) 0.036(3) 0.010(2) 0.015(2) 0.002(3) C3 0.060(4) 0.062(4) 0.029(3) 0.001(3) 0.006(3) -0.008(3) C4 0.047(3) 0.075(5) 0.056(4) -0.015(3) 0.022(3) 0.006(3) C5 0.048(3) 0.074(4) 0.045(3) -0.009(3) 0.024(3) -0.009(3) C6 0.078(5) 0.054(4) 0.068(4) 0.028(3) 0.025(4) 0.007(3) C7 0.032(3) 0.030(3) 0.047(3) 0.000(2) 0.011(2) 0.003(2) C9 0.041(3) 0.054(4) 0.057(4) -0.010(3) 0.016(3) 0.012(3) C10 0.078(4) 0.041(3) 0.055(4) 0.009(3) 0.025(3) -0.002(3) C11 0.042(3) 0.034(3) 0.041(3) 0.004(2) 0.012(2) 0.000(2) C12 0.038(3) 0.047(3) 0.036(3) -0.006(2) 0.011(2) -0.006(2) C13 0.071(4) 0.077(5) 0.047(4) -0.016(3) 0.001(3) -0.020(4) C14 0.032(3) 0.041(3) 0.032(3) -0.007(2) 0.008(2) -0.004(2) C15 0.045(3) 0.055(4) 0.042(3) 0.008(3) 0.015(3) -0.012(3) C16 0.089(5) 0.036(3) 0.070(4) -0.002(3) 0.023(4) -0.018(3) C17 0.038(3) 0.043(3) 0.039(3) -0.001(2) 0.007(2) 0.001(2) C18 0.064(4) 0.062(4) 0.061(4) 0.024(3) 0.009(3) 0.011(3) C19 0.067(4) 0.071(5) 0.049(4) -0.001(3) 0.001(3) -0.004(3) C20 0.093(6) 0.056(4) 0.084(5) -0.025(4) -0.008(4) 0.017(4) C22 0.055(4) 0.044(3) 0.065(4) -0.013(3) 0.016(3) -0.011(3) C23 0.085(5) 0.061(4) 0.064(4) 0.016(3) 0.020(4) 0.028(4) C24 0.065(5) 0.093(6) 0.079(5) -0.018(4) 0.014(4) -0.032(4) C25 0.076(5) 0.041(4) 0.093(5) -0.006(4) -0.003(4) 0.011(3) C26 0.037(3) 0.058(4) 0.072(4) 0.002(3) 0.001(3) 0.011(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 Cu1 N5 1.944(4) . ? Cu1 N1 1.971(4) . ? Cu1 O5 1.975(3) . ? Cu1 N2 2.064(4) . ? Cu1 O4 2.318(4) . ? Cu1 Cu2 3.2438(8) . ? Cu2 O3 1.941(3) . ? Cu2 N4 1.946(4) . ? Cu2 O5 2.003(3) . ? Cu2 N3 2.090(4) . ? Cu2 O2 2.370(4) . ? Cu2 N1 2.479(4) . ? Cl1 O9 1.272(10) . ? Cl1 O6 1.290(13) . ? Cl1 O8 1.308(9) . ? Cl1 O7 1.366(8) . ? O1 C1 1.370(6) . ? O1 C13 1.426(7) . ? O2 C17 1.371(6) . ? O2 C23 1.422(7) . ? O3 C7 1.310(6) . ? O5 C14 1.332(6) . ? N1 N6 1.184(6) . ? N2 C26 1.470(7) . ? N2 C25 1.471(8) . ? N2 C18 1.496(8) . ? N3 C20 1.459(8) . ? N3 C24 1.468(8) . ? N3 C19 1.493(8) . ? N4 C2 1.277(7) . ? N4 C3 1.469(7) . ? N5 C15 1.269(7) . ? N5 C6 1.463(7) . ? N6 N7 1.163(7) . ? C1 C22 1.376(8) . ? C1 C7 1.419(7) . ? C2 C11 1.435(7) . ? C3 C19 1.511(9) . ? C4 C5 1.360(9) . ? C4 C9 1.389(9) . ? C5 C12 1.405(7) . ? C6 C18 1.480(9) . ? C7 C11 1.414(7) . ? C9 C17 1.386(7) . ? C10 C16 1.356(9) . ? C10 C11 1.410(8) . ? C12 C14 1.417(7) . ? C12 C15 1.433(8) . ? C14 C17 1.410(7) . ? C16 C22 1.391(9) . ? 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 N5 Cu1 N1 167.88(19) . . ? N5 Cu1 O5 90.67(16) . . ? N1 Cu1 O5 84.58(16) . . ? N5 Cu1 N2 85.32(19) . . ? N1 Cu1 N2 98.77(19) . . ? O5 Cu1 N2 175.01(16) . . ? N5 Cu1 O4 97.49(17) . . ? N1 Cu1 O4 93.38(17) . . ? O5 Cu1 O4 86.81(14) . . ? N2 Cu1 O4 96.65(16) . . ? N5 Cu1 Cu2 126.33(13) . . ? N1 Cu1 Cu2 49.74(13) . . ? O5 Cu1 Cu2 35.66(9) . . ? N2 Cu1 Cu2 148.23(13) . . ? O4 Cu1 Cu2 83.11(9) . . ? O3 Cu2 N4 91.81(16) . . ? O3 Cu2 O5 89.44(14) . . ? N4 Cu2 O5 173.09(16) . . ? O3 Cu2 N3 176.10(16) . . ? N4 Cu2 N3 84.31(18) . . ? O5 Cu2 N3 94.45(16) . . ? O3 Cu2 O2 87.83(15) . . ? N4 Cu2 O2 99.05(16) . . ? O5 Cu2 O2 74.21(13) . . ? N3 Cu2 O2 93.12(16) . . ? O3 Cu2 N1 86.99(15) . . ? N4 Cu2 N1 115.07(17) . . ? O5 Cu2 N1 71.78(14) . . ? N3 Cu2 N1 94.32(17) . . ? O2 Cu2 N1 145.62(14) . . ? O3 Cu2 Cu1 82.56(10) . . ? N4 Cu2 Cu1 151.83(13) . . ? O5 Cu2 Cu1 35.07(9) . . ? N3 Cu2 Cu1 100.70(12) . . ? O2 Cu2 Cu1 108.24(9) . . ? N1 Cu2 Cu1 37.37(10) . . ? O9 Cl1 O6 105.3(11) . . ? O9 Cl1 O8 106.3(8) . . ? O6 Cl1 O8 112.1(12) . . ? O9 Cl1 O7 123.3(10) . . ? O6 Cl1 O7 100.6(8) . . ? O8 Cl1 O7 109.1(7) . . ? C1 O1 C13 118.1(5) . . ? C17 O2 C23 118.8(5) . . ? C17 O2 Cu2 109.9(3) . . ? C23 O2 Cu2 129.7(4) . . ? C7 O3 Cu2 126.2(3) . . ? C14 O5 Cu1 126.5(3) . . ? C14 O5 Cu2 120.7(3) . . ? Cu1 O5 Cu2 109.27(15) . . ? N6 N1 Cu1 134.1(4) . . ? N6 N1 Cu2 133.0(4) . . ? Cu1 N1 Cu2 92.89(17) . . ? C26 N2 C25 109.2(5) . . ? C26 N2 C18 106.6(5) . . ? C25 N2 C18 112.0(5) . . ? C26 N2 Cu1 114.3(4) . . ? C25 N2 Cu1 111.1(4) . . ? C18 N2 Cu1 103.6(3) . . ? C20 N3 C24 108.0(6) . . ? C20 N3 C19 110.9(5) . . ? C24 N3 C19 107.1(5) . . ? C20 N3 Cu2 112.7(4) . . ? C24 N3 Cu2 114.0(4) . . ? C19 N3 Cu2 104.1(3) . . ? C2 N4 C3 120.4(5) . . ? C2 N4 Cu2 125.3(4) . . ? C3 N4 Cu2 113.6(3) . . ? C15 N5 C6 121.0(5) . . ? C15 N5 Cu1 126.6(4) . . ? C6 N5 Cu1 112.3(4) . . ? N7 N6 N1 177.6(6) . . ? O1 C1 C22 124.7(5) . . ? O1 C1 C7 113.6(5) . . ? C22 C1 C7 121.7(5) . . ? N4 C2 C11 126.1(5) . . ? N4 C3 C19 106.2(5) . . ? C5 C4 C9 119.8(5) . . ? C4 C5 C12 121.6(6) . . ? N5 C6 C18 107.3(5) . . ? O3 C7 C11 123.8(5) . . ? O3 C7 C1 118.8(5) . . ? C11 C7 C1 117.4(5) . . ? C17 C9 C4 119.9(6) . . ? C16 C10 C11 121.1(6) . . ? C10 C11 C7 119.5(5) . . ? C10 C11 C2 117.6(5) . . ? C7 C11 C2 122.9(5) . . ? C5 C12 C14 119.9(5) . . ? C5 C12 C15 117.6(5) . . ? C14 C12 C15 122.4(5) . . ? O5 C14 C17 120.5(4) . . ? O5 C14 C12 122.7(5) . . ? C17 C14 C12 116.8(5) . . ? N5 C15 C12 127.4(5) . . ? C10 C16 C22 120.6(6) . . ? O2 C17 C9 123.6(5) . . ? O2 C17 C14 114.4(4) . . ? C9 C17 C14 122.0(5) . . ? C6 C18 N2 110.4(5) . . ? N3 C19 C3 109.3(5) . . ? C1 C22 C16 119.7(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.665 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.090