# ic0109905.cif data_mn1138 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cu(PEA)(H2O)Cl _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 Cl Cu N4 O2' _chemical_formula_weight 420.35 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' 'O' 'O' 0.0492 0.0322 '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' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.8580(7) _cell_length_b 17.1000(14) _cell_length_c 23.528(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3563.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.9 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 3.286 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3842 _exptl_absorpt_correction_T_max 0.7790 _exptl_absorpt_process_details ;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28 (1995) 53-56. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens rotating Cu anode' _diffrn_radiation_monochromator 'nickel filter' _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method 2\q-\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.9 _diffrn_reflns_number 5100 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 56.35 _reflns_number_total 2353 _reflns_number_gt 1993 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _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^)+(0.0720P)^2^+3.0493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2353 _refine_ls_number_parameters 243 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.87282(5) 0.54110(3) 0.13391(2) 0.0152(2) Uani 1 1 d . . . Cl1 Cl 0.85660(10) 0.50355(6) 0.22521(4) 0.0219(3) Uani 1 1 d . . . O1 O 1.0921(3) 0.62518(15) -0.00414(10) 0.0228(6) Uani 1 1 d . . . O2 O 0.7572(3) 0.43872(16) 0.09299(11) 0.0200(6) Uani 1 1 d D . . H2A H 0.742(5) 0.4042(17) 0.1177(13) 0.022(12) Uiso 1 1 d D . . H2B H 0.808(5) 0.417(3) 0.0673(17) 0.068(19) Uiso 1 1 d D . . N1 N 1.0831(3) 0.49930(18) 0.11619(13) 0.0165(7) Uani 1 1 d . . . N2 N 0.9215(3) 0.60369(18) 0.06818(12) 0.0155(7) Uani 1 1 d . . . N3 N 0.6828(3) 0.60547(17) 0.12907(12) 0.0152(7) Uani 1 1 d . . . N5 N 0.8545(3) 0.81596(18) 0.15948(13) 0.0185(7) Uani 1 1 d . . . C1 C 1.1616(5) 0.4466(2) 0.14601(17) 0.0253(10) Uani 1 1 d . . . H1 H 1.1218 0.4280 0.1810 0.030 Uiso 1 1 calc R . . C2 C 1.2996(5) 0.4186(3) 0.12718(17) 0.0292(10) Uani 1 1 d . . . H2 H 1.3547 0.3819 0.1493 0.035 Uiso 1 1 calc R . . C3 C 1.3556(4) 0.4445(3) 0.07626(18) 0.0288(11) Uani 1 1 d . . . H3 H 1.4491 0.4253 0.0623 0.035 Uiso 1 1 calc R . . C4 C 1.2734(4) 0.4992(2) 0.04533(17) 0.0226(9) Uani 1 1 d . . . H4 H 1.3102 0.5182 0.0100 0.027 Uiso 1 1 calc R . . C5 C 1.1388(4) 0.5252(2) 0.06666(16) 0.0167(9) Uani 1 1 d . . . C6 C 1.0465(4) 0.5906(2) 0.03934(15) 0.0166(8) Uani 1 1 d . . . C7 C 0.8271(4) 0.6707(2) 0.05545(15) 0.0158(8) Uani 1 1 d . . . H7 H 0.8034 0.6706 0.0139 0.019 Uiso 1 1 calc R . . C8 C 0.6814(4) 0.6601(2) 0.08848(15) 0.0167(8) Uani 1 1 d . . . C9 C 0.5555(4) 0.7067(2) 0.07904(16) 0.0211(9) Uani 1 1 d . . . H9 H 0.5578 0.7465 0.0509 0.025 Uiso 1 1 calc R . . C10 C 0.4275(4) 0.6946(2) 0.11091(17) 0.0261(10) Uani 1 1 d . . . H10 H 0.3402 0.7258 0.1050 0.031 Uiso 1 1 calc R . . C11 C 0.4275(4) 0.6362(2) 0.15190(17) 0.0240(9) Uani 1 1 d . . . H11 H 0.3395 0.6260 0.1738 0.029 Uiso 1 1 calc R . . C12 C 0.5569(4) 0.5935(2) 0.16028(16) 0.0201(9) Uani 1 1 d . . . H12 H 0.5578 0.5543 0.1889 0.024 Uiso 1 1 calc R . . C13 C 0.9053(4) 0.7489(2) 0.07059(15) 0.0167(8) Uani 1 1 d . . . H13A H 1.0024 0.7520 0.0499 0.020 Uiso 1 1 calc R . . H13B H 0.8410 0.7925 0.0572 0.020 Uiso 1 1 calc R . . C14 C 0.9355(4) 0.7597(2) 0.13330(15) 0.0172(9) Uani 1 1 d . . . C15 C 1.0408(4) 0.7149(2) 0.16268(16) 0.0203(9) Uani 1 1 d . . . H15 H 1.0953 0.6748 0.1437 0.024 Uiso 1 1 calc R . . C16 C 1.0655(4) 0.7294(2) 0.21995(17) 0.0240(10) Uani 1 1 d . . . H16 H 1.1366 0.6991 0.2406 0.029 Uiso 1 1 calc R . . C17 C 0.9864(4) 0.7880(2) 0.24647(16) 0.0248(10) Uani 1 1 d . . . H17 H 1.0027 0.7996 0.2855 0.030 Uiso 1 1 calc R . . C18 C 0.8819(4) 0.8297(3) 0.21463(17) 0.0249(10) Uani 1 1 d . . . H18 H 0.8269 0.8702 0.2329 0.030 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 0.0145(3) 0.0146(4) 0.0166(3) 0.0023(2) 0.0013(2) 0.0009(2) Cl1 0.0226(5) 0.0261(6) 0.0171(5) 0.0044(4) -0.0007(4) -0.0023(4) O1 0.0290(15) 0.0191(14) 0.0202(14) 0.0056(13) 0.0101(12) 0.0053(13) O2 0.0252(15) 0.0159(14) 0.0190(15) 0.0000(12) 0.0052(13) -0.0028(13) N1 0.0156(16) 0.0139(17) 0.0201(16) -0.0009(14) 0.0008(14) 0.0015(14) N2 0.0141(15) 0.0147(17) 0.0176(16) -0.0003(13) 0.0017(13) 0.0027(14) N3 0.0169(16) 0.0109(16) 0.0179(15) -0.0011(13) -0.0010(14) 0.0030(14) N5 0.0181(16) 0.0180(18) 0.0195(17) 0.0006(14) 0.0018(14) -0.0023(14) C1 0.027(2) 0.026(2) 0.022(2) 0.0065(19) 0.0000(18) 0.006(2) C2 0.027(2) 0.029(2) 0.032(2) 0.002(2) -0.0054(19) 0.010(2) C3 0.018(2) 0.032(3) 0.036(3) 0.001(2) 0.0057(19) 0.009(2) C4 0.021(2) 0.024(2) 0.0229(19) 0.0006(18) 0.0026(18) 0.0054(19) C5 0.017(2) 0.016(2) 0.0172(19) -0.0005(17) -0.0001(16) -0.0070(17) C6 0.020(2) 0.0102(19) 0.0197(19) -0.0023(17) -0.0028(17) -0.0025(17) C7 0.0206(19) 0.0133(19) 0.0134(18) 0.0015(16) 0.0001(16) 0.0024(17) C8 0.0190(19) 0.0122(19) 0.0188(19) -0.0035(16) -0.0006(17) -0.0029(18) C9 0.021(2) 0.019(2) 0.023(2) -0.0010(18) -0.0016(18) 0.0036(19) C10 0.017(2) 0.027(2) 0.034(2) 0.000(2) 0.0001(19) 0.0081(19) C11 0.014(2) 0.028(2) 0.030(2) -0.001(2) 0.0031(17) 0.0013(18) C12 0.022(2) 0.018(2) 0.021(2) 0.0011(17) 0.0036(18) -0.0047(18) C13 0.0177(19) 0.0137(19) 0.019(2) 0.0055(16) 0.0021(15) 0.0002(18) C14 0.0148(19) 0.015(2) 0.0215(19) 0.0027(17) 0.0026(17) -0.0050(17) C15 0.0122(18) 0.019(2) 0.030(2) -0.0011(18) 0.0038(18) -0.0002(17) C16 0.021(2) 0.025(2) 0.026(2) 0.0043(19) -0.0044(18) 0.0005(19) C17 0.027(2) 0.026(2) 0.021(2) -0.0008(19) -0.0012(18) -0.001(2) C18 0.026(2) 0.025(2) 0.024(2) -0.0042(19) 0.0045(18) 0.0011(19) _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 N2 1.930(3) . ? Cu1 N3 2.014(3) . ? Cu1 N1 2.038(3) . ? Cu1 O2 2.245(3) . ? Cu1 Cl1 2.2466(10) . ? O1 C6 1.249(4) . ? N1 C1 1.337(5) . ? N1 C5 1.341(5) . ? N2 C6 1.318(5) . ? N2 C7 1.450(5) . ? N3 C8 1.336(5) . ? N3 C12 1.351(5) . ? N5 C18 1.341(5) . ? N5 C14 1.349(5) . ? C1 C2 1.386(6) . ? C2 C3 1.370(6) . ? C3 C4 1.391(6) . ? C4 C5 1.368(5) . ? C5 C6 1.527(5) . ? C7 C8 1.518(5) . ? C7 C13 1.547(5) . ? C8 C9 1.388(5) . ? C9 C10 1.376(6) . ? C10 C11 1.388(6) . ? C11 C12 1.374(6) . ? C13 C14 1.511(5) . ? C14 C15 1.391(5) . ? C15 C16 1.387(5) . ? C16 C17 1.372(6) . ? C17 C18 1.388(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 80.70(12) . . ? N2 Cu1 N1 80.00(12) . . ? N3 Cu1 N1 160.68(12) . . ? N2 Cu1 O2 101.00(11) . . ? N3 Cu1 O2 91.18(11) . . ? N1 Cu1 O2 93.20(11) . . ? N2 Cu1 Cl1 159.91(10) . . ? N3 Cu1 Cl1 99.02(9) . . ? N1 Cu1 Cl1 98.84(9) . . ? O2 Cu1 Cl1 99.09(7) . . ? C1 N1 C5 119.2(3) . . ? C1 N1 Cu1 127.2(3) . . ? C5 N1 Cu1 113.5(2) . . ? C6 N2 C7 120.8(3) . . ? C6 N2 Cu1 120.4(3) . . ? C7 N2 Cu1 118.4(2) . . ? C8 N3 C12 119.1(3) . . ? C8 N3 Cu1 115.5(2) . . ? C12 N3 Cu1 125.2(2) . . ? C18 N5 C14 118.1(3) . . ? N1 C1 C2 121.6(4) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 119.1(4) . . ? C5 C4 C3 118.9(4) . . ? N1 C5 C4 122.1(4) . . ? N1 C5 C6 114.2(3) . . ? C4 C5 C6 123.4(3) . . ? O1 C6 N2 127.8(3) . . ? O1 C6 C5 121.2(3) . . ? N2 C6 C5 111.0(3) . . ? N2 C7 C8 106.9(3) . . ? N2 C7 C13 112.2(3) . . ? C8 C7 C13 111.5(3) . . ? N3 C8 C9 121.6(4) . . ? N3 C8 C7 116.2(3) . . ? C9 C8 C7 122.2(3) . . ? C10 C9 C8 119.3(4) . . ? C9 C10 C11 119.1(4) . . ? C12 C11 C10 118.9(4) . . ? N3 C12 C11 122.0(4) . . ? C14 C13 C7 114.2(3) . . ? N5 C14 C15 121.5(3) . . ? N5 C14 C13 116.0(3) . . ? C15 C14 C13 122.5(4) . . ? C16 C15 C14 119.3(4) . . ? C17 C16 C15 119.4(4) . . ? C16 C17 C18 118.1(4) . . ? N5 C18 C17 123.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A N5 0.839(10) 1.993(17) 2.799(4) 161(4) 8_755 O2 H2B O1 0.841(10) 1.873(13) 2.710(3) 174(6) 5_765 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 56.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.446 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.085 #===END data_mn1119 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Cu2PEA2](ClO4)2.2.5CH3CN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37.50 Cl2 Cu2 N10.50 O10' _chemical_formula_weight 1035.30 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 '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 12.4124(7) _cell_length_b 13.6347(8) _cell_length_c 25.7106(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.8930(10) _cell_angle_gamma 90.00 _cell_volume 4350.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6246 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 31.1 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5864 _exptl_absorpt_correction_T_max 0.6985 _exptl_absorpt_process_details 'SADABS 2.0 (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames remeasured' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 57964 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 31.47 _reflns_number_total 13676 _reflns_number_gt 11406 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _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. One of the the perchlorate anions is disordered and has two sets of three of the oxygen atoms {O(4), O(5), and O(6) were refined to 60.7(11)% occupancy while {O(4B), O(5B), and O(6B) are at 39.3(11) % occupancy. One of the acetonitrile molecules is disordered with respect to an inversion center and is at half occupancy. Hydrogen atoms were not added for this latter molecule. ; _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^)+(0.0609P)^2^+7.6655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13676 _refine_ls_number_parameters 584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.029 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 0.37879(2) 0.58765(2) 0.164364(10) 0.01943(7) Uani 1 1 d . A . Cu2 Cu 0.33294(2) 0.79788(2) 0.081828(11) 0.02318(8) Uani 1 1 d . A . O1 O 0.60822(15) 0.59612(15) 0.05845(7) 0.0289(4) Uani 1 1 d . . . N1 N 0.51969(17) 0.65167(15) 0.18603(8) 0.0216(4) Uani 1 1 d . A . N2 N 0.44017(16) 0.59417(14) 0.09656(7) 0.0188(3) Uani 1 1 d . A . N3 N 0.28920(16) 0.48226(15) 0.13119(7) 0.0199(4) Uani 1 1 d . A . N4 N 0.38432(17) 0.76821(16) 0.01063(7) 0.0222(4) Uani 1 1 d . A . C1 C 0.5545(2) 0.6842(2) 0.23292(10) 0.0297(5) Uani 1 1 d . . . H1 H 0.5050 0.6872 0.2607 0.036 Uiso 1 1 calc R A . C2 C 0.6601(3) 0.7135(2) 0.24195(11) 0.0367(6) Uani 1 1 d . A . H2 H 0.6826 0.7358 0.2754 0.044 Uiso 1 1 calc R . . C3 C 0.7323(2) 0.7098(2) 0.20145(12) 0.0375(6) Uani 1 1 d . . . H3 H 0.8054 0.7286 0.2068 0.045 Uiso 1 1 calc R A . C4 C 0.6961(2) 0.6781(2) 0.15258(11) 0.0300(5) Uani 1 1 d . A . H4 H 0.7438 0.6764 0.1240 0.036 Uiso 1 1 calc R . . C5 C 0.59022(19) 0.64941(17) 0.14625(9) 0.0215(4) Uani 1 1 d . . . C6 C 0.54634(19) 0.61056(17) 0.09497(9) 0.0202(4) Uani 1 1 d . A . C7 C 0.38846(19) 0.53612(17) 0.05555(8) 0.0202(4) Uani 1 1 d . . . H7 H 0.4444 0.5013 0.0349 0.024 Uiso 1 1 calc R A . C8 C 0.31549(19) 0.46160(17) 0.08154(9) 0.0213(4) Uani 1 1 d . A . C9 C 0.2755(2) 0.3794(2) 0.05599(10) 0.0285(5) Uani 1 1 d . . . H9 H 0.2953 0.3654 0.0212 0.034 Uiso 1 1 calc R A . C10 C 0.2055(2) 0.3177(2) 0.08244(12) 0.0326(6) Uani 1 1 d . A . H10 H 0.1769 0.2610 0.0658 0.039 Uiso 1 1 calc R . . C11 C 0.1777(2) 0.3396(2) 0.13330(11) 0.0308(5) Uani 1 1 d . . . H11 H 0.1293 0.2988 0.1517 0.037 Uiso 1 1 calc R A . C12 C 0.2219(2) 0.42185(19) 0.15660(10) 0.0253(5) Uani 1 1 d . A . H12 H 0.2043 0.4364 0.1916 0.030 Uiso 1 1 calc R . . C13 C 0.3166(2) 0.59879(19) 0.01894(9) 0.0242(4) Uani 1 1 d . A . H13A H 0.2802 0.5547 -0.0064 0.029 Uiso 1 1 calc R . . H13B H 0.2600 0.6305 0.0398 0.029 Uiso 1 1 calc R . . C14 C 0.3754(2) 0.67712(18) -0.01064(9) 0.0223(4) Uani 1 1 d . . . C15 C 0.4164(2) 0.65786(19) -0.05965(9) 0.0270(5) Uani 1 1 d . A . H15 H 0.4102 0.5939 -0.0741 0.032 Uiso 1 1 calc R . . C16 C 0.4662(2) 0.7318(2) -0.08753(9) 0.0294(5) Uani 1 1 d . . . H16 H 0.4951 0.7189 -0.1208 0.035 Uiso 1 1 calc R A . C17 C 0.4732(2) 0.82488(19) -0.06599(9) 0.0271(5) Uani 1 1 d . A . H17 H 0.5061 0.8770 -0.0844 0.033 Uiso 1 1 calc R . . C18 C 0.4313(2) 0.84010(18) -0.01717(9) 0.0229(4) Uani 1 1 d . . . H18 H 0.4356 0.9040 -0.0025 0.028 Uiso 1 1 calc R A . O2 O 0.32968(19) 0.85776(17) 0.23387(8) 0.0388(5) Uani 1 1 d . . . N5 N 0.47104(17) 0.85369(15) 0.11447(8) 0.0215(4) Uani 1 1 d . . . N6 N 0.28769(17) 0.79628(17) 0.15216(8) 0.0257(4) Uani 1 1 d . . . N7 N 0.17222(18) 0.79066(17) 0.06731(9) 0.0271(4) Uani 1 1 d . . . N8 N 0.29713(17) 0.60090(15) 0.22984(7) 0.0217(4) Uani 1 1 d . A . C19 C 0.5638(2) 0.8807(2) 0.09274(10) 0.0283(5) Uani 1 1 d . A . H19 H 0.5765 0.8636 0.0575 0.034 Uiso 1 1 calc R . . C20 C 0.6420(3) 0.9330(3) 0.12035(13) 0.0403(7) Uani 1 1 d . . . H20 H 0.7067 0.9522 0.1039 0.048 Uiso 1 1 calc R A . C21 C 0.6253(3) 0.9568(3) 0.17169(14) 0.0491(9) Uani 1 1 d . A . H21 H 0.6779 0.9927 0.1910 0.059 Uiso 1 1 calc R . . C22 C 0.5292(3) 0.9271(2) 0.19485(12) 0.0378(7) Uani 1 1 d . . . H22 H 0.5154 0.9422 0.2302 0.045 Uiso 1 1 calc R A . C23 C 0.4555(2) 0.87556(18) 0.16519(9) 0.0242(4) Uani 1 1 d . A . C24 C 0.3498(2) 0.84157(19) 0.18766(9) 0.0257(5) Uani 1 1 d . A . C25 C 0.1731(2) 0.7821(2) 0.16161(11) 0.0298(5) Uani 1 1 d . A . H25 H 0.1472 0.8316 0.1873 0.036 Uiso 1 1 calc R . . C26 C 0.1120(2) 0.7937(2) 0.10995(12) 0.0348(6) Uani 1 1 d . A . C27 C -0.0005(3) 0.7982(3) 0.10644(15) 0.0520(10) Uani 1 1 d . . . H27 H -0.0426 0.7981 0.1370 0.062 Uiso 1 1 calc R A . C28 C -0.0500(3) 0.8029(3) 0.05716(15) 0.0498(9) Uani 1 1 d . A . H28 H -0.1263 0.8055 0.0537 0.060 Uiso 1 1 calc R . . C29 C 0.0134(3) 0.8036(3) 0.01406(14) 0.0449(8) Uani 1 1 d . . . H29 H -0.0182 0.8080 -0.0197 0.054 Uiso 1 1 calc R A . C30 C 0.1238(2) 0.7977(2) 0.02032(11) 0.0321(6) Uani 1 1 d . A . H30 H 0.1673 0.7987 -0.0097 0.039 Uiso 1 1 calc R . . C31 C 0.1472(2) 0.6775(2) 0.18062(11) 0.0314(5) Uani 1 1 d . . . H31A H 0.0682 0.6719 0.1845 0.038 Uiso 1 1 calc R A . H31B H 0.1686 0.6304 0.1533 0.038 Uiso 1 1 calc R . . C32 C 0.2010(2) 0.6472(2) 0.23148(10) 0.0290(5) Uani 1 1 d . A . C33 C 0.1485(2) 0.6614(2) 0.27829(11) 0.0355(6) Uani 1 1 d . . . H33 H 0.0826 0.6967 0.2790 0.043 Uiso 1 1 calc R A . C34 C 0.1927(2) 0.6240(2) 0.32376(10) 0.0302(5) Uani 1 1 d . A . H34 H 0.1587 0.6348 0.3561 0.036 Uiso 1 1 calc R . . C35 C 0.2873(2) 0.5704(2) 0.32140(9) 0.0294(5) Uani 1 1 d . . . H35 H 0.3172 0.5408 0.3518 0.035 Uiso 1 1 calc R A . C36 C 0.3373(2) 0.56080(19) 0.27406(9) 0.0250(5) Uani 1 1 d . A . H36 H 0.4026 0.5246 0.2726 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.57792(5) 0.39065(5) 0.22493(2) 0.02593(12) Uani 1 1 d . . . O3 O 0.48945(19) 0.42460(16) 0.19264(8) 0.0378(5) Uani 1 1 d . A 1 O4 O 0.6233(9) 0.3044(8) 0.2052(4) 0.062(3) Uani 0.607(11) 1 d P A 1 O5 O 0.5299(4) 0.3634(5) 0.27533(17) 0.0478(14) Uani 0.607(11) 1 d P A 1 O6 O 0.6547(4) 0.4651(4) 0.2354(3) 0.058(2) Uani 0.607(11) 1 d P A 1 O4B O 0.5923(15) 0.2890(12) 0.2185(7) 0.076(6) Uani 0.393(11) 1 d P A 2 O5B O 0.5780(9) 0.4247(11) 0.2735(3) 0.080(5) Uani 0.393(11) 1 d P A 2 O6B O 0.6723(7) 0.4285(9) 0.1971(5) 0.089(4) Uani 0.393(11) 1 d P A 2 Cl2 Cl 0.24581(5) 1.04296(4) 0.02723(2) 0.02313(11) Uani 1 1 d . A . O7 O 0.32435(15) 0.99461(14) 0.06095(7) 0.0277(4) Uani 1 1 d . . . O8 O 0.22875(18) 0.98453(16) -0.01893(7) 0.0352(4) Uani 1 1 d . . . O9 O 0.14667(16) 1.05514(19) 0.05437(8) 0.0390(5) Uani 1 1 d . . . O10 O 0.28632(18) 1.13776(15) 0.01212(9) 0.0358(4) Uani 1 1 d . . . N9 N 0.9282(4) 0.2225(4) 0.1241(2) 0.0925(15) Uiso 1 1 d . . . C37 C 0.8844(5) 0.4852(5) 0.1576(2) 0.0798(15) Uiso 1 1 d . . . C38 C 0.8196(8) 0.4431(7) 0.1204(4) 0.133(3) Uiso 1 1 d . . . H38A H 0.7652 0.4838 0.0975 0.050 Uiso 1 1 d . . . H38B H 0.7739 0.3945 0.1378 0.060 Uiso 1 1 d . . . H38C H 0.8624 0.4066 0.0969 0.060 Uiso 1 1 d . . . N10 N 0.9390(6) 0.5304(5) 0.1866(3) 0.122(2) Uiso 1 1 d . . . C39 C 0.9284(4) 0.1419(3) 0.12419(17) 0.0566(9) Uiso 1 1 d . . . C40 C 0.9303(4) 0.0380(3) 0.12280(17) 0.0575(10) Uiso 1 1 d . . . H40A H 0.8882 0.0096 0.0935 0.050 Uiso 1 1 d . . . H40B H 0.9064 0.0141 0.1540 0.050 Uiso 1 1 d . . . H40C H 1.0035 0.0070 0.1236 0.050 Uiso 1 1 d . . . N11 N 1.0483(9) 0.5603(8) 0.0661(4) 0.087(3) Uiso 0.50 1 d P . . C41 C 1.0205(10) 0.5257(9) 0.0279(4) 0.164(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02363(14) 0.02405(14) 0.01069(12) -0.00126(9) 0.00240(9) -0.00229(10) Cu2 0.02322(14) 0.03144(16) 0.01492(13) -0.00403(11) 0.00172(10) 0.00052(11) O1 0.0275(9) 0.0351(10) 0.0243(9) -0.0096(7) 0.0083(7) -0.0076(7) N1 0.0270(9) 0.0221(9) 0.0157(8) -0.0003(7) -0.0023(7) -0.0005(7) N2 0.0229(9) 0.0225(9) 0.0112(7) -0.0013(6) 0.0014(6) -0.0030(7) N3 0.0244(9) 0.0204(9) 0.0151(8) 0.0019(7) 0.0028(7) -0.0006(7) N4 0.0274(9) 0.0253(10) 0.0139(8) -0.0013(7) 0.0001(7) 0.0005(8) C1 0.0371(13) 0.0349(13) 0.0171(10) -0.0021(9) -0.0037(9) -0.0057(11) C2 0.0441(16) 0.0426(16) 0.0232(12) -0.0033(11) -0.0090(11) -0.0111(13) C3 0.0329(14) 0.0462(17) 0.0332(14) -0.0037(12) -0.0079(11) -0.0109(12) C4 0.0265(12) 0.0347(13) 0.0286(12) -0.0023(10) -0.0008(9) -0.0062(10) C5 0.0253(10) 0.0204(10) 0.0189(10) -0.0003(8) -0.0004(8) -0.0016(8) C6 0.0246(10) 0.0193(10) 0.0166(9) -0.0015(8) 0.0016(8) -0.0021(8) C7 0.0257(10) 0.0214(10) 0.0136(9) -0.0021(7) 0.0020(8) -0.0028(8) C8 0.0254(10) 0.0204(10) 0.0182(10) -0.0010(8) 0.0031(8) -0.0010(8) C9 0.0351(13) 0.0257(12) 0.0249(12) -0.0071(9) 0.0060(10) -0.0058(10) C10 0.0386(14) 0.0236(12) 0.0357(14) -0.0071(10) 0.0058(11) -0.0082(10) C11 0.0355(13) 0.0244(12) 0.0325(13) 0.0031(10) 0.0071(10) -0.0071(10) C12 0.0322(12) 0.0247(11) 0.0191(10) 0.0035(9) 0.0050(9) -0.0028(9) C13 0.0290(11) 0.0277(12) 0.0158(10) 0.0013(8) -0.0016(8) -0.0043(9) C14 0.0272(11) 0.0237(11) 0.0159(10) 0.0007(8) -0.0008(8) -0.0004(9) C15 0.0405(14) 0.0239(11) 0.0166(10) -0.0033(8) 0.0010(9) -0.0019(10) C16 0.0446(15) 0.0292(12) 0.0146(10) -0.0015(9) 0.0050(10) -0.0018(11) C17 0.0401(13) 0.0252(11) 0.0160(10) 0.0019(9) 0.0034(9) -0.0012(10) C18 0.0300(11) 0.0212(10) 0.0177(10) -0.0001(8) 0.0003(8) 0.0003(9) O2 0.0524(13) 0.0453(12) 0.0191(9) -0.0078(8) 0.0126(8) -0.0030(10) N5 0.0259(9) 0.0229(9) 0.0159(8) 0.0020(7) 0.0018(7) 0.0017(7) N6 0.0248(10) 0.0309(11) 0.0216(9) -0.0040(8) 0.0085(8) -0.0024(8) N7 0.0261(10) 0.0338(11) 0.0214(10) 0.0037(8) -0.0018(8) 0.0011(8) N8 0.0279(10) 0.0252(10) 0.0121(8) 0.0012(7) 0.0024(7) 0.0004(8) C19 0.0299(12) 0.0333(13) 0.0218(11) 0.0053(10) 0.0024(9) -0.0022(10) C20 0.0370(15) 0.0475(18) 0.0366(15) 0.0067(13) 0.0026(12) -0.0152(13) C21 0.0508(19) 0.058(2) 0.0382(17) -0.0042(15) -0.0045(14) -0.0283(17) C22 0.0498(17) 0.0395(16) 0.0239(12) -0.0062(11) -0.0025(12) -0.0128(13) C23 0.0322(12) 0.0236(11) 0.0168(10) -0.0001(8) 0.0018(8) -0.0025(9) C24 0.0346(12) 0.0259(11) 0.0169(10) -0.0010(8) 0.0064(9) 0.0014(10) C25 0.0292(12) 0.0337(13) 0.0266(12) 0.0057(10) 0.0059(10) 0.0052(10) C26 0.0313(13) 0.0425(16) 0.0308(13) 0.0134(12) 0.0015(10) 0.0067(11) C27 0.0306(15) 0.079(3) 0.0461(19) 0.0295(18) 0.0063(13) 0.0136(16) C28 0.0271(14) 0.065(2) 0.057(2) 0.0260(18) -0.0072(13) 0.0031(14) C29 0.0373(16) 0.060(2) 0.0373(16) 0.0186(15) -0.0130(13) 0.0010(14) C30 0.0329(13) 0.0374(14) 0.0260(12) 0.0111(11) -0.0041(10) 0.0003(11) C31 0.0301(12) 0.0347(14) 0.0295(13) 0.0039(11) 0.0025(10) 0.0004(10) C32 0.0341(13) 0.0333(13) 0.0198(11) 0.0040(9) 0.0058(9) 0.0045(10) C33 0.0378(14) 0.0433(16) 0.0258(12) 0.0056(11) 0.0129(11) 0.0112(12) C34 0.0361(13) 0.0381(14) 0.0167(10) 0.0008(10) 0.0105(9) 0.0012(11) C35 0.0386(14) 0.0353(13) 0.0143(10) 0.0028(9) 0.0034(9) 0.0037(11) C36 0.0307(12) 0.0296(12) 0.0146(10) 0.0001(8) 0.0008(8) 0.0051(9) Cl1 0.0274(3) 0.0262(3) 0.0242(3) 0.0001(2) -0.0027(2) 0.0035(2) O3 0.0470(12) 0.0328(10) 0.0333(11) -0.0048(8) -0.0162(9) 0.0155(9) O4 0.081(6) 0.069(7) 0.037(3) -0.022(3) -0.018(3) 0.057(5) O5 0.040(2) 0.078(4) 0.0261(18) 0.007(2) 0.0041(16) 0.001(2) O6 0.050(3) 0.046(3) 0.078(5) 0.021(3) -0.029(3) -0.023(2) O4B 0.086(10) 0.031(4) 0.111(14) -0.008(7) -0.072(9) 0.010(6) O5B 0.077(7) 0.137(12) 0.025(3) -0.037(5) -0.019(4) 0.057(8) O6B 0.059(5) 0.108(8) 0.101(9) 0.016(7) 0.048(5) -0.013(5) Cl2 0.0268(3) 0.0255(3) 0.0171(2) -0.00102(19) 0.00051(19) 0.0040(2) O7 0.0327(9) 0.0290(9) 0.0212(8) -0.0024(7) -0.0050(7) 0.0075(7) O8 0.0503(12) 0.0367(11) 0.0184(8) -0.0052(8) -0.0054(8) 0.0000(9) O9 0.0266(9) 0.0643(15) 0.0263(10) 0.0042(10) 0.0052(7) 0.0100(9) O10 0.0463(12) 0.0246(9) 0.0367(11) 0.0032(8) 0.0025(9) 0.0014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.9154(18) . ? Cu1 N8 1.9868(19) . ? Cu1 N3 2.000(2) . ? Cu1 N1 2.025(2) . ? Cu1 O3 2.707(2) . ? Cu2 N6 1.902(2) . ? Cu2 N4 1.9895(19) . ? Cu2 N7 2.026(2) . ? Cu2 N5 2.044(2) . ? Cu2 O7 2.737(2) . ? O1 C6 1.238(3) . ? N1 C1 1.350(3) . ? N1 C5 1.357(3) . ? N2 C6 1.338(3) . ? N2 C7 1.459(3) . ? N3 C12 1.349(3) . ? N3 C8 1.352(3) . ? N4 C18 1.350(3) . ? N4 C14 1.361(3) . ? C1 C2 1.386(4) . ? C2 C3 1.385(4) . ? C3 C4 1.397(4) . ? C4 C5 1.378(3) . ? C5 C6 1.514(3) . ? C7 C8 1.523(3) . ? C7 C13 1.545(3) . ? C8 C9 1.388(3) . ? C9 C10 1.394(4) . ? C10 C11 1.390(4) . ? C11 C12 1.381(4) . ? C13 C14 1.506(3) . ? C14 C15 1.391(3) . ? C15 C16 1.388(4) . ? C16 C17 1.387(4) . ? C17 C18 1.382(3) . ? O2 C24 1.238(3) . ? N5 C19 1.339(3) . ? N5 C23 1.354(3) . ? N6 C24 1.337(3) . ? N6 C25 1.460(3) . ? N7 C26 1.337(4) . ? N7 C30 1.344(3) . ? N8 C36 1.350(3) . ? N8 C32 1.352(3) . ? C19 C20 1.391(4) . ? C20 C21 1.378(5) . ? C21 C22 1.401(5) . ? C22 C23 1.376(4) . ? C23 C24 1.514(4) . ? C25 C26 1.527(4) . ? C25 C31 1.543(4) . ? C26 C27 1.399(4) . ? C27 C28 1.401(5) . ? C28 C29 1.369(5) . ? C29 C30 1.380(4) . ? C31 C32 1.516(4) . ? C32 C33 1.391(4) . ? C33 C34 1.381(4) . ? C34 C35 1.384(4) . ? C35 C36 1.382(3) . ? Cl1 O5B 1.332(6) . ? Cl1 O4 1.402(9) . ? Cl1 O4B 1.407(16) . ? Cl1 O6 1.416(4) . ? Cl1 O3 1.443(2) . ? Cl1 O6B 1.475(7) . ? Cl1 O5 1.482(4) . ? Cl2 O9 1.434(2) . ? Cl2 O8 1.442(2) . ? Cl2 O10 1.442(2) . ? Cl2 O7 1.4528(19) . ? N9 C39 1.099(6) . ? C37 N10 1.174(8) . ? C37 C38 1.366(10) . ? C39 C40 1.418(6) . ? N11 C41 1.138(13) . ? C41 C41 1.67(2) 3_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N8 169.23(9) . . ? N2 Cu1 N3 82.62(8) . . ? N8 Cu1 N3 98.00(8) . . ? N2 Cu1 N1 82.89(8) . . ? N8 Cu1 N1 100.23(8) . . ? N3 Cu1 N1 154.05(8) . . ? N2 Cu1 O3 94.31(8) . . ? N8 Cu1 O3 96.35(8) . . ? N3 Cu1 O3 78.52(7) . . ? N1 Cu1 O3 81.24(8) . . ? N6 Cu2 N4 167.46(9) . . ? N6 Cu2 N7 82.53(9) . . ? N4 Cu2 N7 98.59(9) . . ? N6 Cu2 N5 82.65(9) . . ? N4 Cu2 N5 100.07(8) . . ? N7 Cu2 N5 155.61(9) . . ? N6 Cu2 O7 100.75(8) . . ? N4 Cu2 O7 91.77(7) . . ? N7 Cu2 O7 88.64(8) . . ? N5 Cu2 O7 75.26(7) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Cu1 130.62(18) . . ? C5 N1 Cu1 110.33(15) . . ? C6 N2 C7 119.40(19) . . ? C6 N2 Cu1 116.20(15) . . ? C7 N2 Cu1 117.11(14) . . ? C6 N2 Cu2 105.53(14) . . ? C7 N2 Cu2 102.39(13) . . ? Cu1 N2 Cu2 88.67(7) . . ? C12 N3 C8 119.4(2) . . ? C12 N3 Cu1 125.20(16) . . ? C8 N3 Cu1 114.31(15) . . ? C18 N4 C14 118.9(2) . . ? C18 N4 Cu2 119.11(16) . . ? C14 N4 Cu2 122.00(16) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 Cu1 29.95(12) . . ? C2 C1 Cu1 151.5(2) . . ? C3 C2 C1 119.0(3) . . ? C2 C3 C4 119.0(3) . . ? C5 C4 C3 119.2(3) . . ? N1 C5 C4 122.0(2) . . ? N1 C5 C6 115.9(2) . . ? C4 C5 C6 122.1(2) . . ? N1 C5 Cu1 42.66(11) . . ? C4 C5 Cu1 163.62(19) . . ? C6 C5 Cu1 73.41(12) . . ? O1 C6 N2 128.3(2) . . ? O1 C6 C5 119.8(2) . . ? N2 C6 C5 111.89(19) . . ? O1 C6 Cu1 161.52(17) . . ? N2 C6 Cu1 38.20(10) . . ? C5 C6 Cu1 75.10(12) . . ? N2 C7 C8 107.62(18) . . ? N2 C7 C13 112.56(19) . . ? C8 C7 C13 107.14(19) . . ? N2 C7 Cu1 36.17(9) . . ? C8 C7 Cu1 72.74(12) . . ? C13 C7 Cu1 115.04(15) . . ? N3 C8 C9 121.7(2) . . ? N3 C8 C7 115.4(2) . . ? C9 C8 C7 122.8(2) . . ? N3 C8 Cu1 39.96(11) . . ? C9 C8 Cu1 159.64(18) . . ? C7 C8 Cu1 76.44(12) . . ? C8 C9 C10 118.5(2) . . ? C11 C10 C9 119.7(2) . . ? C12 C11 C10 118.7(2) . . ? N3 C12 C11 122.0(2) . . ? N3 C12 Cu1 33.15(11) . . ? C11 C12 Cu1 153.78(18) . . ? C14 C13 C7 114.9(2) . . ? C14 C13 Cu2 67.79(13) . . ? C7 C13 Cu2 97.55(13) . . ? N4 C14 C15 120.5(2) . . ? N4 C14 C13 118.8(2) . . ? C15 C14 C13 120.7(2) . . ? N4 C14 Cu2 34.94(11) . . ? C15 C14 Cu2 155.35(18) . . ? C13 C14 Cu2 83.96(13) . . ? C14 C15 C16 120.2(2) . . ? C17 C16 C15 119.0(2) . . ? C18 C17 C16 118.5(2) . . ? N4 C18 C17 122.9(2) . . ? N4 C18 Cu2 36.86(11) . . ? C17 C18 Cu2 159.68(18) . . ? C19 N5 C23 118.5(2) . . ? C19 N5 Cu2 130.69(17) . . ? C23 N5 Cu2 110.24(16) . . ? C24 N6 C25 120.1(2) . . ? C24 N6 Cu2 117.90(17) . . ? C25 N6 Cu2 117.56(18) . . ? C24 N6 Cu1 98.65(16) . . ? C25 N6 Cu1 102.60(15) . . ? Cu2 N6 Cu1 89.66(8) . . ? C26 N7 C30 119.1(2) . . ? C26 N7 Cu2 114.13(19) . . ? C30 N7 Cu2 125.95(19) . . ? C36 N8 C32 118.6(2) . . ? C36 N8 Cu1 119.34(17) . . ? C32 N8 Cu1 122.10(16) . . ? N5 C19 C20 121.7(3) . . ? N5 C19 Cu2 30.12(12) . . ? C20 C19 Cu2 150.9(2) . . ? C21 C20 C19 119.7(3) . . ? C20 C21 C22 118.7(3) . . ? C23 C22 C21 118.4(3) . . ? N5 C23 C22 122.8(2) . . ? N5 C23 C24 115.9(2) . . ? C22 C23 C24 121.2(2) . . ? N5 C23 Cu2 42.93(12) . . ? C22 C23 Cu2 164.0(2) . . ? C24 C23 Cu2 73.41(13) . . ? O2 C24 N6 127.9(3) . . ? O2 C24 C23 120.0(2) . . ? N6 C24 C23 112.0(2) . . ? O2 C24 Cu2 163.9(2) . . ? N6 C24 Cu2 37.05(11) . . ? C23 C24 Cu2 75.26(13) . . ? N6 C25 C26 108.3(2) . . ? N6 C25 C31 112.6(2) . . ? C26 C25 C31 105.6(2) . . ? N6 C25 Cu2 35.78(11) . . ? C26 C25 Cu2 73.22(15) . . ? C31 C25 Cu2 116.32(17) . . ? N7 C26 C27 121.2(3) . . ? N7 C26 C25 115.7(2) . . ? C27 C26 C25 122.8(3) . . ? N7 C26 Cu2 40.50(13) . . ? C27 C26 Cu2 161.2(2) . . ? C25 C26 Cu2 75.89(15) . . ? C26 C27 C28 118.9(3) . . ? C29 C28 C27 118.8(3) . . ? C28 C29 C30 119.2(3) . . ? N7 C30 C29 122.6(3) . . ? N7 C30 Cu2 32.92(13) . . ? C29 C30 Cu2 154.9(2) . . ? C32 C31 C25 115.7(2) . . ? C32 C31 Cu1 67.60(14) . . ? C25 C31 Cu1 97.01(16) . . ? N8 C32 C33 121.2(2) . . ? N8 C32 C31 118.5(2) . . ? C33 C32 C31 120.2(3) . . ? N8 C32 Cu1 34.96(11) . . ? C33 C32 Cu1 155.9(2) . . ? C31 C32 Cu1 83.89(15) . . ? C34 C33 C32 119.7(3) . . ? C35 C34 C33 118.9(2) . . ? C34 C35 C36 118.8(2) . . ? N8 C36 C35 122.6(2) . . ? N8 C36 Cu1 36.70(11) . . ? C35 C36 Cu1 159.17(19) . . ? O5B Cl1 O4 129.6(6) . . ? O5B Cl1 O4B 117.1(9) . . ? O4 Cl1 O4B 22.9(9) . . ? O5B Cl1 O6 65.2(7) . . ? O4 Cl1 O6 113.4(5) . . ? O4B Cl1 O6 130.0(7) . . ? O5B Cl1 O3 114.6(3) . . ? O4 Cl1 O3 111.6(5) . . ? O4B Cl1 O3 110.2(7) . . ? O6 Cl1 O3 112.6(2) . . ? O5B Cl1 O6B 110.1(8) . . ? O4 Cl1 O6B 78.0(7) . . ? O4B Cl1 O6B 100.6(9) . . ? O6 Cl1 O6B 45.9(5) . . ? O3 Cl1 O6B 102.2(5) . . ? O5B Cl1 O5 42.5(6) . . ? O4 Cl1 O5 106.0(5) . . ? O4B Cl1 O5 84.9(8) . . ? O6 Cl1 O5 107.0(3) . . ? O3 Cl1 O5 105.7(2) . . ? O6B Cl1 O5 147.7(6) . . ? Cl1 O3 Cu1 142.81(13) . . ? O9 Cl2 O8 110.39(14) . . ? O9 Cl2 O10 109.44(14) . . ? O8 Cl2 O10 108.71(13) . . ? O9 Cl2 O7 109.58(12) . . ? O8 Cl2 O7 109.20(12) . . ? O10 Cl2 O7 109.51(13) . . ? Cl2 O7 Cu2 125.84(11) . . ? N10 C37 C38 172.9(8) . . ? N9 C39 C40 178.3(6) . . ? N11 C41 C41 179.7(19) . 3_765 ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 31.47 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.707 _refine_diff_density_min -1.319 _refine_diff_density_rms 0.097 #===END