# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1730 data_x536a #(1) _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 Cu2 N16 O16.15' _chemical_formula_weight 930.14 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 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 11.3954(7) _cell_length_b 14.062(1) _cell_length_c 22.994(1) _cell_angle_alpha 90.00 _cell_angle_beta 101.167(4) _cell_angle_gamma 90.00 _cell_volume 3614.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 511 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1901 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details 'SHELXTL V5.1 (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART-CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24639 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8282 _reflns_number_gt 6489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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. As describer below except that hydrogens on waters were located in diff maps but ; _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^)+(0.0084P)^2^+8.4993P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8282 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.813 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.091 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 -0.14521(3) -0.13584(3) -0.253632(16) 0.01679(9) Uani 1 1 d . . . Cu2 Cu 0.00886(4) -0.28140(3) -0.116658(16) 0.01835(10) Uani 1 1 d . . . O1 O -0.0653(2) -0.0635(2) -0.31197(11) 0.0242(5) Uani 1 1 d . . . N1 N 0.1873(2) -0.2907(2) -0.10266(11) 0.0220(6) Uani 1 1 d . . . H1A H -0.050(3) -0.012(3) -0.3016(17) 0.024(11) Uiso 1 1 d . . . H1B H -0.009(4) -0.086(3) -0.3210(19) 0.036(13) Uiso 1 1 d . . . C1 C 0.2551(4) -0.3608(3) -0.07415(16) 0.0299(8) Uani 1 1 d . . . H1 H 0.215(3) -0.409(3) -0.0578(17) 0.031(10) Uiso 1 1 d . . . O2 O -0.0084(3) -0.42118(18) -0.09391(11) 0.0301(6) Uani 1 1 d . . . H2C H -0.078(6) -0.433(5) -0.082(3) 0.12(3) Uiso 1 1 d . . . H2D H -0.0148 -0.4530 -0.1061 0.060 Uiso 1 1 d . . . N2 N 0.1942(3) -0.0768(2) -0.18900(13) 0.0228(6) Uani 1 1 d . . . H2B H 0.271(4) -0.071(3) -0.1916(16) 0.027(10) Uiso 1 1 d . . . H2A H 0.153(3) -0.032(3) -0.1987(15) 0.018(10) Uiso 1 1 d . . . C2 C 0.3776(4) -0.3641(3) -0.07103(16) 0.0322(8) Uani 1 1 d . . . H2 H 0.416(4) -0.410(3) -0.0522(17) 0.036(11) Uiso 1 1 d . . . N3 N 0.0479(2) -0.15455(18) -0.14823(11) 0.0167(5) Uani 1 1 d . . . C3 C 0.4319(3) -0.2937(3) -0.09744(16) 0.0301(8) Uani 1 1 d . . . H3 H 0.517(4) -0.295(3) -0.0947(17) 0.036(11) Uiso 1 1 d . . . N4 N -0.0373(2) -0.09064(18) -0.18007(11) 0.0163(5) Uani 1 1 d . . . C4 C 0.3625(3) -0.2205(3) -0.12688(15) 0.0256(7) Uani 1 1 d . . . H4 H 0.396(3) -0.170(3) -0.1441(16) 0.028(10) Uiso 1 1 d . . . N5 N -0.0398(3) -0.0123(2) -0.09036(12) 0.0223(6) Uani 1 1 d . . . H5A H -0.071(4) 0.026(3) -0.0735(17) 0.028(11) Uiso 1 1 d . . . H5B H 0.027(5) -0.043(4) -0.070(2) 0.063(15) Uiso 1 1 d . . . C5 C 0.2413(3) -0.2207(2) -0.12857(13) 0.0181(6) Uani 1 1 d . . . N6 N -0.2342(2) -0.00225(19) -0.23363(11) 0.0197(6) Uani 1 1 d . . . C6 C 0.1569(3) -0.1457(2) -0.15739(13) 0.0173(6) Uani 1 1 d . . . N7 N -0.0584(2) -0.2523(2) -0.03333(11) 0.0225(6) Uani 1 1 d . . . C7 C -0.0797(3) -0.0268(2) -0.14795(13) 0.0161(6) Uani 1 1 d . . . N8 N -0.3221(3) -0.1579(2) -0.12725(14) 0.0239(6) Uani 1 1 d . . . H8B H -0.351(3) -0.154(3) -0.1624(18) 0.029(11) Uiso 1 1 d . . . H8A H -0.354(4) -0.126(3) -0.1044(18) 0.032(11) Uiso 1 1 d . . . C8 C -0.1808(3) 0.0327(2) -0.18020(13) 0.0169(6) Uani 1 1 d . . . N9 N -0.1652(2) -0.25468(19) -0.14541(10) 0.0172(5) Uani 1 1 d . . . C9 C -0.2158(3) 0.1172(2) -0.15792(15) 0.0235(7) Uani 1 1 d . . . H9 H -0.181(3) 0.140(3) -0.1192(16) 0.025(10) Uiso 1 1 d . . . N10 N -0.2084(2) -0.23691(18) -0.20684(10) 0.0166(5) Uani 1 1 d . . . C10 C -0.3099(3) 0.1678(3) -0.19162(16) 0.0268(8) Uani 1 1 d . . . H10 H 0.336(3) -0.225(3) 0.1768(15) 0.023(9) Uiso 1 1 d . . . N11 N -0.3089(3) -0.3831(2) -0.21540(13) 0.0227(6) Uani 1 1 d . . . H11A H -0.350(4) -0.425(3) -0.2374(17) 0.030(11) Uiso 1 1 d . . . H11B H -0.290(4) -0.394(3) -0.180(2) 0.052(14) Uiso 1 1 d . . . C11 C -0.3650(3) 0.1324(3) -0.24635(16) 0.0264(7) Uani 1 1 d . . . H11 H -0.429(4) 0.165(3) -0.2686(17) 0.038(11) Uiso 1 1 d . . . N12 N -0.2651(2) -0.19684(19) -0.31752(11) 0.0182(5) Uani 1 1 d . . . C12 C -0.3244(3) 0.0470(2) -0.26530(15) 0.0232(7) Uani 1 1 d . . . H12 H -0.359(3) 0.020(2) -0.2996(15) 0.020(9) Uiso 1 1 d . . . C13 C -0.0038(3) -0.2625(3) 0.02349(15) 0.0278(8) Uani 1 1 d . . . H13 H 0.075(4) -0.293(3) 0.0300(17) 0.032(11) Uiso 1 1 d . . . C14 C -0.0529(3) -0.2284(3) 0.07032(15) 0.0280(8) Uani 1 1 d . . . H14 H -0.017(3) -0.235(2) 0.1098(16) 0.020(9) Uiso 1 1 d . . . C15 C -0.1599(3) -0.1814(3) 0.05778(15) 0.0263(8) Uani 1 1 d . . . H15 H -0.200(3) -0.155(3) 0.0880(16) 0.028(10) Uiso 1 1 d . . . C16 C -0.2202(3) -0.1739(3) -0.00096(14) 0.0249(7) Uani 1 1 d . . . H16 H -0.295(3) -0.149(3) -0.0095(15) 0.023(10) Uiso 1 1 d . . . C17 C -0.1662(3) -0.2107(2) -0.04498(13) 0.0185(6) Uani 1 1 d . . . C18 C -0.2226(3) -0.2070(2) -0.10988(13) 0.0175(6) Uani 1 1 d . . . C19 C -0.2739(3) -0.3032(2) -0.23722(13) 0.0173(6) Uani 1 1 d . . . C20 C -0.3142(3) -0.2780(2) -0.30139(13) 0.0174(6) Uani 1 1 d . . . C21 C -0.4010(3) -0.3271(2) -0.34031(14) 0.0212(7) Uani 1 1 d . . . H21 H -0.432(3) -0.383(2) -0.3275(14) 0.016(8) Uiso 1 1 d . . . C22 C -0.4420(3) -0.2894(3) -0.39652(15) 0.0302(8) Uani 1 1 d . . . H22 H -0.505(4) -0.319(3) -0.4225(18) 0.044(12) Uiso 1 1 d . . . C23 C -0.3948(3) -0.2057(3) -0.41259(15) 0.0281(8) Uani 1 1 d . . . H23 H -0.420(4) -0.178(3) -0.4488(19) 0.047(13) Uiso 1 1 d . . . C24 C -0.3036(3) -0.1617(3) -0.37218(14) 0.0230(7) Uani 1 1 d . . . H24 H -0.266(3) -0.108(2) -0.3820(14) 0.016(9) Uiso 1 1 d . . . N100 N 0.0113(2) 0.33871(19) 0.26221(11) 0.0203(6) Uani 1 1 d . . . O101 O 0.0770(2) 0.38793(17) 0.30069(10) 0.0264(5) Uani 1 1 d . . . O102 O -0.0156(2) 0.25559(16) 0.27275(10) 0.0255(5) Uani 1 1 d . . . O103 O -0.0270(2) 0.37419(17) 0.21127(10) 0.0326(6) Uani 1 1 d . . . N200 N 0.2652(4) -0.5445(3) 0.04075(19) 0.0559(11) Uani 1 1 d . . . O201 O 0.1702(4) -0.4959(4) 0.0328(2) 0.1121(19) Uani 1 1 d . . . O202 O 0.2913(5) -0.5850(3) 0.08775(15) 0.0871(15) Uani 1 1 d . . . O203 O 0.3250(4) -0.5501(3) 0.00281(16) 0.0748(12) Uani 1 1 d . . . O303 O 0.4362(2) -0.45648(17) 0.28500(11) 0.0281(5) Uani 1 1 d . . . O302 O 0.5233(2) -0.33316(18) 0.25540(11) 0.0331(6) Uani 1 1 d . . . N300 N 0.4520(2) -0.4002(2) 0.24400(12) 0.0233(6) Uani 1 1 d . . . O301 O 0.3954(3) -0.4134(2) 0.19254(12) 0.0456(8) Uani 1 1 d . . . N400 N -0.2472(3) 0.0772(3) 0.00263(14) 0.0406(9) Uani 1 1 d . . . O401 O -0.3251(3) 0.0928(5) -0.04074(19) 0.134(3) Uani 1 1 d . . . O402 O -0.2760(3) 0.0454(2) 0.04810(12) 0.0399(7) Uani 1 1 d . . . O403 O -0.1408(2) 0.0912(2) -0.00098(11) 0.0350(6) Uani 1 1 d . . . O1W O 0.4757(3) 0.0602(3) 0.05763(16) 0.0677(11) Uani 1 1 d . . . H1WB H 0.5634 0.0568 0.0527 0.050 Uiso 1 1 d . . . H1WA H 0.4449 -0.0016 0.0481 0.050 Uiso 1 1 d . . . O2W O 0.1417(3) -0.3911(2) 0.14551(14) 0.0513(8) Uani 1 1 d . . . H2WB H 0.2115 -0.3853 0.1742 0.050 Uiso 1 1 d . . . H2WA H 0.1442 -0.4397 0.1614 0.050 Uiso 1 1 d . . . O3W O 0.276(2) -0.334(2) 0.0782(11) 0.076(8) Uani 0.15 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02085(19) 0.01581(19) 0.01312(17) 0.00000(14) 0.00185(14) -0.00188(16) Cu2 0.0206(2) 0.0186(2) 0.01633(18) 0.00195(15) 0.00467(15) 0.00102(16) O1 0.0330(15) 0.0167(13) 0.0243(12) -0.0006(10) 0.0085(11) -0.0029(11) N1 0.0238(14) 0.0238(15) 0.0177(13) 0.0003(11) 0.0022(11) 0.0058(12) C1 0.036(2) 0.0252(19) 0.0266(18) 0.0066(15) 0.0006(15) 0.0064(17) O2 0.0425(16) 0.0215(13) 0.0288(13) -0.0011(10) 0.0132(12) -0.0027(12) N2 0.0182(15) 0.0215(15) 0.0296(16) 0.0069(12) 0.0066(12) 0.0029(13) C2 0.034(2) 0.027(2) 0.0309(19) 0.0071(16) -0.0032(16) 0.0133(17) N3 0.0176(13) 0.0157(13) 0.0159(12) -0.0015(10) 0.0011(10) 0.0035(10) C3 0.0227(18) 0.035(2) 0.0314(19) 0.0026(16) 0.0018(15) 0.0120(16) N4 0.0161(13) 0.0171(13) 0.0154(12) 0.0006(10) 0.0024(10) 0.0011(10) C4 0.0252(18) 0.0274(19) 0.0247(17) 0.0026(14) 0.0060(14) 0.0044(15) N5 0.0226(15) 0.0254(16) 0.0183(14) -0.0053(12) 0.0025(12) 0.0041(13) C5 0.0234(16) 0.0179(15) 0.0136(14) -0.0006(12) 0.0049(12) 0.0035(13) N6 0.0187(13) 0.0198(14) 0.0198(13) 0.0017(11) 0.0018(11) 0.0010(11) C6 0.0206(15) 0.0176(16) 0.0138(14) -0.0033(12) 0.0031(12) 0.0022(13) N7 0.0248(15) 0.0265(15) 0.0162(13) 0.0024(11) 0.0043(11) 0.0015(12) C7 0.0148(14) 0.0141(15) 0.0193(15) -0.0009(12) 0.0031(12) -0.0036(12) N8 0.0238(15) 0.0326(17) 0.0153(14) -0.0012(12) 0.0035(12) 0.0067(13) C8 0.0160(15) 0.0169(15) 0.0183(14) 0.0012(12) 0.0047(12) -0.0024(12) N9 0.0192(13) 0.0223(14) 0.0101(11) 0.0018(10) 0.0027(10) -0.0015(11) C9 0.0214(17) 0.0216(17) 0.0269(17) -0.0032(14) 0.0029(14) 0.0001(14) N10 0.0195(13) 0.0192(14) 0.0106(12) 0.0006(10) 0.0018(10) -0.0022(11) C10 0.0253(18) 0.0198(17) 0.037(2) -0.0030(15) 0.0090(15) 0.0041(14) N11 0.0268(16) 0.0224(15) 0.0177(14) -0.0002(12) 0.0014(12) -0.0076(13) C11 0.0205(17) 0.0268(18) 0.0326(18) 0.0067(15) 0.0068(14) 0.0061(15) N12 0.0199(13) 0.0200(14) 0.0149(12) 0.0000(10) 0.0036(10) 0.0005(11) C12 0.0216(17) 0.0241(18) 0.0228(17) 0.0023(14) 0.0017(14) -0.0004(14) C13 0.0308(19) 0.033(2) 0.0185(16) 0.0034(14) 0.0022(14) 0.0024(16) C14 0.036(2) 0.033(2) 0.0144(15) -0.0003(14) 0.0038(14) -0.0047(16) C15 0.033(2) 0.0305(19) 0.0168(16) -0.0040(14) 0.0095(14) -0.0060(16) C16 0.0266(19) 0.0310(19) 0.0181(16) -0.0003(14) 0.0068(14) -0.0023(15) C17 0.0240(16) 0.0190(16) 0.0132(14) -0.0001(12) 0.0050(12) -0.0021(13) C18 0.0196(15) 0.0168(15) 0.0162(14) 0.0019(12) 0.0035(12) -0.0041(13) C19 0.0171(15) 0.0205(16) 0.0148(14) 0.0006(12) 0.0043(12) -0.0011(13) C20 0.0165(15) 0.0203(16) 0.0158(14) -0.0022(12) 0.0039(12) 0.0023(12) C21 0.0207(16) 0.0233(17) 0.0193(15) -0.0021(13) 0.0031(13) -0.0047(14) C22 0.0247(18) 0.043(2) 0.0214(17) -0.0043(16) -0.0003(14) -0.0048(17) C23 0.0276(19) 0.037(2) 0.0174(16) 0.0039(15) -0.0005(14) 0.0008(16) C24 0.0258(18) 0.0249(18) 0.0190(16) 0.0037(13) 0.0059(13) 0.0009(14) N100 0.0246(14) 0.0180(14) 0.0202(14) -0.0004(11) 0.0093(11) 0.0049(11) O101 0.0297(13) 0.0221(13) 0.0255(12) -0.0047(10) 0.0008(10) -0.0007(10) O102 0.0345(14) 0.0174(12) 0.0266(12) 0.0009(9) 0.0112(10) -0.0018(10) O103 0.0545(17) 0.0228(13) 0.0180(11) 0.0027(10) 0.0004(11) 0.0099(12) N200 0.078(3) 0.042(2) 0.061(3) 0.0116(19) 0.048(2) -0.003(2) O201 0.093(3) 0.134(4) 0.131(4) 0.049(4) 0.076(3) 0.027(3) O202 0.175(5) 0.058(2) 0.0357(19) 0.0067(17) 0.040(2) -0.026(3) O203 0.112(3) 0.059(2) 0.070(2) 0.0292(19) 0.060(2) 0.036(2) O303 0.0313(14) 0.0237(13) 0.0327(13) 0.0032(10) 0.0148(11) -0.0030(11) O302 0.0313(14) 0.0290(14) 0.0360(14) 0.0066(11) -0.0008(11) -0.0132(12) N300 0.0178(14) 0.0247(15) 0.0275(15) -0.0002(12) 0.0043(12) -0.0004(12) O301 0.0538(19) 0.0466(18) 0.0290(14) -0.0015(13) -0.0105(13) -0.0120(15) N400 0.0305(18) 0.061(2) 0.0275(17) 0.0027(16) -0.0003(14) 0.0159(17) O401 0.033(2) 0.289(8) 0.073(3) 0.100(4) -0.0056(19) 0.017(3) O402 0.0397(16) 0.0478(18) 0.0342(15) -0.0074(13) 0.0123(13) -0.0023(14) O403 0.0257(14) 0.0510(17) 0.0286(13) -0.0032(12) 0.0061(11) 0.0069(13) O1W 0.0449(19) 0.085(3) 0.075(2) -0.033(2) 0.0172(18) 0.0058(19) O2W 0.0328(16) 0.067(2) 0.0506(18) -0.0019(16) -0.0019(14) -0.0079(15) O3W 0.063(16) 0.10(2) 0.060(15) -0.020(14) 0.008(13) -0.020(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cu2 3.8794(5) . ? Cu1 N4 1.993(2) . ? Cu1 N12 1.996(3) . ? Cu1 N10 1.999(3) . ? Cu1 O1 2.033(3) . ? Cu1 N6 2.225(3) . ? Cu2 N1 2.001(3) . ? Cu2 N9 2.001(3) . ? Cu2 N3 2.008(3) . ? Cu2 O2 2.053(3) . ? Cu2 N7 2.235(3) . ? Cu1 O102 2.588(2) 3 ? Cu2 O103 2.579(2) 3 ? O1 H1A 0.77(4) . ? O1 H1B 0.78(4) . ? N1 C1 1.342(4) . ? N1 C5 1.358(4) . ? C1 C2 1.386(5) . ? C1 H1 0.94(4) . ? O2 H2C 0.91(7) . ? O2 H2D 0.5257 . ? N2 C6 1.330(4) . ? N2 H2B 0.90(4) . ? N2 H2A 0.79(4) . ? C2 C3 1.370(6) . ? C2 H2 0.85(4) . ? N3 C6 1.305(4) . ? N3 N4 1.419(3) . ? C3 C4 1.391(5) . ? C3 H3 0.96(4) . ? N4 C7 1.312(4) . ? C4 C5 1.375(5) . ? C4 H4 0.93(4) . ? N5 C7 1.330(4) . ? N5 H5A 0.79(4) . ? N5 H5B 0.92(5) . ? C5 C6 1.493(4) . ? N6 C12 1.333(4) . ? N6 C8 1.354(4) . ? N7 C17 1.340(4) . ? N7 C13 1.342(4) . ? C7 C8 1.499(4) . ? N8 C18 1.321(4) . ? N8 H8B 0.81(4) . ? N8 H8A 0.83(4) . ? C8 C9 1.383(4) . ? N9 C18 1.323(4) . ? N9 N10 1.425(3) . ? C9 C10 1.391(5) . ? C9 H9 0.95(4) . ? N10 C19 1.309(4) . ? C10 C11 1.385(5) . ? N11 C19 1.322(4) . ? N11 H11A 0.85(4) . ? N11 H11B 0.81(5) . ? C11 C12 1.388(5) . ? C11 H11 0.93(4) . ? N12 C24 1.343(4) . ? N12 C20 1.354(4) . ? C12 H12 0.90(3) . ? C13 C14 1.392(5) . ? C13 H13 0.98(4) . ? C14 C15 1.368(5) . ? C14 H14 0.93(3) . ? C15 C16 1.396(5) . ? C15 H15 0.98(4) . ? C16 C17 1.383(4) . ? C16 H16 0.91(4) . ? C17 C18 1.507(4) . ? C19 C20 1.500(4) . ? C20 C21 1.383(4) . ? C21 C22 1.391(5) . ? C21 H21 0.93(3) . ? C22 C23 1.375(5) . ? C22 H22 0.93(4) . ? C23 C24 1.396(5) . ? C23 H23 0.91(4) . ? C24 H24 0.92(3) . ? N100 O102 1.244(3) . ? N100 O101 1.251(3) . ? N100 O103 1.270(3) . ? N200 O202 1.207(5) . ? N200 O203 1.209(5) . ? N200 O201 1.264(6) . ? O303 N300 1.270(4) . ? O302 N300 1.239(4) . ? N300 O301 1.247(4) . ? N400 O401 1.220(4) . ? N400 O402 1.239(4) . ? N400 O403 1.247(4) . ? O1W H1WB 1.0286 . ? O1W H1WA 0.9469 . ? O2W H2WB 0.9335 . ? O2W H2WA 0.7723 . ? 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 N4 Cu1 N12 169.65(11) . . ? N4 Cu1 N10 89.84(10) . . ? N12 Cu1 N10 79.86(10) . . ? N4 Cu1 O1 96.84(10) . . ? N12 Cu1 O1 93.41(10) . . ? N10 Cu1 O1 164.69(11) . . ? N4 Cu1 N6 77.65(10) . . ? N12 Cu1 N6 103.92(10) . . ? N10 Cu1 N6 105.25(10) . . ? O1 Cu1 N6 89.67(11) . . ? N1 Cu2 N9 167.69(11) . . ? N1 Cu2 N3 80.01(11) . . ? N9 Cu2 N3 89.36(10) . . ? N1 Cu2 O2 92.34(11) . . ? N9 Cu2 O2 97.26(11) . . ? N3 Cu2 O2 168.92(10) . . ? N1 Cu2 N7 112.37(10) . . ? N9 Cu2 N7 76.49(10) . . ? N3 Cu2 N7 106.50(10) . . ? O2 Cu2 N7 83.77(10) . . ? Cu1 O1 H1A 112(3) . . ? Cu1 O1 H1B 118(3) . . ? H1A O1 H1B 109(4) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Cu2 126.7(3) . . ? C5 N1 Cu2 114.5(2) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 H1 117(2) . . ? C2 C1 H1 121(2) . . ? Cu2 O2 H2C 112(4) . . ? Cu2 O2 H2D 133.6 . . ? H2C O2 H2D 88.3 . . ? C6 N2 H2B 122(2) . . ? C6 N2 H2A 120(3) . . ? H2B N2 H2A 116(4) . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 123(3) . . ? C1 C2 H2 118(3) . . ? C6 N3 N4 115.7(3) . . ? C6 N3 Cu2 115.3(2) . . ? N4 N3 Cu2 124.87(19) . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 119(2) . . ? C4 C3 H3 121(2) . . ? C7 N4 N3 115.6(2) . . ? C7 N4 Cu1 117.5(2) . . ? N3 N4 Cu1 118.96(18) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4 119(2) . . ? C3 C4 H4 122(2) . . ? C7 N5 H5A 120(3) . . ? C7 N5 H5B 121(3) . . ? H5A N5 H5B 119(4) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 113.6(3) . . ? C4 C5 C6 124.6(3) . . ? C12 N6 C8 118.1(3) . . ? C12 N6 Cu1 131.3(2) . . ? C8 N6 Cu1 110.6(2) . . ? N3 C6 N2 124.9(3) . . ? N3 C6 C5 114.3(3) . . ? N2 C6 C5 120.7(3) . . ? C17 N7 C13 118.4(3) . . ? C17 N7 Cu2 111.21(19) . . ? C13 N7 Cu2 130.1(2) . . ? N4 C7 N5 124.9(3) . . ? N4 C7 C8 115.8(3) . . ? N5 C7 C8 119.3(3) . . ? C18 N8 H8B 119(3) . . ? C18 N8 H8A 123(3) . . ? H8B N8 H8A 117(4) . . ? N6 C8 C9 122.5(3) . . ? N6 C8 C7 114.4(3) . . ? C9 C8 C7 123.1(3) . . ? C18 N9 N10 114.0(2) . . ? C18 N9 Cu2 117.9(2) . . ? N10 N9 Cu2 119.34(18) . . ? C8 C9 C10 118.7(3) . . ? C8 C9 H9 122(2) . . ? C10 C9 H9 119(2) . . ? C19 N10 N9 117.1(2) . . ? C19 N10 Cu1 116.6(2) . . ? N9 N10 Cu1 124.56(19) . . ? C11 C10 C9 119.2(3) . . ? C19 N11 H11A 122(3) . . ? C19 N11 H11B 120(3) . . ? H11A N11 H11B 118(4) . . ? C10 C11 C12 118.4(3) . . ? C10 C11 H11 120(3) . . ? C12 C11 H11 122(3) . . ? C24 N12 C20 119.3(3) . . ? C24 N12 Cu1 125.7(2) . . ? C20 N12 Cu1 114.9(2) . . ? N6 C12 C11 123.2(3) . . ? N6 C12 H12 115(2) . . ? C11 C12 H12 122(2) . . ? N7 C13 C14 122.4(3) . . ? N7 C13 H13 116(2) . . ? C14 C13 H13 122(2) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 118(2) . . ? C13 C14 H14 124(2) . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 124(2) . . ? C16 C15 H15 117(2) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 H16 121(2) . . ? C15 C16 H16 120(2) . . ? N7 C17 C16 122.5(3) . . ? N7 C17 C18 114.3(3) . . ? C16 C17 C18 123.1(3) . . ? N8 C18 N9 125.1(3) . . ? N8 C18 C17 119.6(3) . . ? N9 C18 C17 115.3(3) . . ? N10 C19 N11 125.8(3) . . ? N10 C19 C20 113.0(3) . . ? N11 C19 C20 121.1(3) . . ? N12 C20 C21 121.7(3) . . ? N12 C20 C19 113.9(3) . . ? C21 C20 C19 124.2(3) . . ? C20 C21 C22 118.7(3) . . ? C20 C21 H21 119(2) . . ? C22 C21 H21 122(2) . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 120(3) . . ? C22 C23 C24 118.7(3) . . ? C22 C23 H23 123(3) . . ? C24 C23 H23 119(3) . . ? N12 C24 C23 121.8(3) . . ? N12 C24 H24 117(2) . . ? C23 C24 H24 122(2) . . ? O102 N100 O101 121.2(3) . . ? O102 N100 O103 119.7(3) . . ? O101 N100 O103 119.1(3) . . ? O202 N200 O203 122.7(5) . . ? O202 N200 O201 116.1(4) . . ? O203 N200 O201 121.2(4) . . ? O302 N300 O301 120.7(3) . . ? O302 N300 O303 119.9(3) . . ? O301 N300 O303 119.3(3) . . ? O401 N400 O402 119.0(4) . . ? O401 N400 O403 118.7(4) . . ? O402 N400 O403 122.2(3) . . ? H1WB O1W H1WA 104.8 . . ? H2WB O2W H2WA 78.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 N9 N10 C19 -104.7(3) . . . . ? C6 N3 N4 C7 -111.9(3) . . . . ? Cu1 N10 N9 Cu2 -55.8(3) . . . . ? Cu1 N4 N3 Cu2 -56.4(3) . . . . ? 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 O1 H1A O103 0.77(4) 1.97(4) 2.734(4) 170(4) 4_565 O1 H1B O2W 0.78(4) 2.04(5) 2.797(4) 164(4) 4 O2 H2C O201 0.91(7) 1.96(7) 2.781(5) 150(6) 3_545 N11 H11B O202 0.81(5) 2.15(5) 2.938(4) 164(5) 3_545 N2 H2B O303 0.90(4) 2.09(4) 2.969(4) 168(3) 4 N2 H2A O101 0.79(4) 2.20(4) 2.961(4) 161(3) 4_565 N5 H5A O403 0.79(4) 2.18(4) 2.930(4) 158(4) . N5 H5B O403 0.92(5) 2.00(5) 2.864(4) 156(4) 3 N8 H8B O302 0.81(4) 2.15(4) 2.926(4) 160(4) 4_455 N8 H8A O1W 0.83(4) 2.12(4) 2.933(4) 166(4) 3 N11 H11A O303 0.85(4) 2.13(4) 2.976(4) 172(4) 3_545 O2W H2WB O301 0.93 2.09 2.901(4) 143.9 . O1W H1WB O402 1.03 1.86 2.888(4) 176.2 1_655 O1W H1WA O401 0.95 1.86 2.732(7) 152.6 3 #===END data_x539 #(2) _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H31 Cu2 N14 O15' _chemical_formula_weight 906.74 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.938(4) _cell_length_b 14.887(3) _cell_length_c 14.372(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.43(3) _cell_angle_gamma 90.00 _cell_volume 3557.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 392 _cell_measurement_theta_min 13.71 _cell_measurement_theta_max 23.31 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART-CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21146 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.46 _reflns_number_total 9330 _reflns_number_gt 8445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.253(9) _refine_ls_number_reflns 9330 _refine_ls_number_parameters 639 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.003 _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 30.46 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.531 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.064 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 0.064891(15) 0.27084(2) 0.308740(19) 0.01618(8) Uani 1 1 d . . . Cu2 Cu -0.101540(14) 0.27146(2) 0.355572(19) 0.01542(8) Uani 1 1 d . . . N1 N -0.07452(18) 0.33314(17) 0.4988(2) 0.0194(5) Uani 1 1 d . . . N2 N 0.02804(17) 0.26282(17) 0.4731(2) 0.0159(5) Uani 1 1 d . . . N3 N 0.07524(18) 0.22361(16) 0.4451(2) 0.0164(5) Uani 1 1 d . . . N4 N 0.06051(18) 0.08714(19) 0.5105(3) 0.0234(6) Uani 1 1 d . . . N5 N 0.11074(17) 0.14835(18) 0.3199(2) 0.0191(5) Uani 1 1 d . . . N6 N 0.03159(18) 0.32062(18) 0.1568(2) 0.0197(5) Uani 1 1 d . . . N7 N -0.06536(16) 0.24578(18) 0.1917(2) 0.0157(5) Uani 1 1 d . . . N8 N -0.11002(18) 0.21109(17) 0.2269(2) 0.0154(5) Uani 1 1 d . . . N9 N -0.09797(18) 0.0654(2) 0.1739(2) 0.0224(5) Uani 1 1 d . . . N10 N -0.14517(17) 0.15074(17) 0.3588(2) 0.0166(5) Uani 1 1 d . . . N11 N 0.1480(2) 0.42151(19) 0.4243(3) 0.0243(6) Uani 1 1 d . . . O1 O 0.07320(15) 0.39819(16) 0.3682(2) 0.0245(5) Uani 1 1 d . . . O2 O 0.19409(17) 0.36810(18) 0.4261(3) 0.0330(6) Uani 1 1 d . . . O3 O 0.1695(2) 0.4952(2) 0.4718(3) 0.0423(8) Uani 1 1 d . . . N12 N -0.18767(19) 0.41904(18) 0.2357(3) 0.0210(6) Uani 1 1 d . . . O4 O -0.11546(15) 0.39701(17) 0.2817(2) 0.0239(5) Uani 1 1 d . . . O5 O -0.23197(19) 0.36302(18) 0.2363(3) 0.0354(7) Uani 1 1 d . . . O6 O -0.2113(2) 0.49484(19) 0.1940(3) 0.0384(7) Uani 1 1 d . . . C1 C -0.1283(2) 0.3610(2) 0.5129(3) 0.0238(7) Uani 1 1 d . . . C2 C -0.1065(3) 0.4126(2) 0.6100(3) 0.0296(8) Uani 1 1 d . . . C3 C -0.0279(3) 0.4355(2) 0.6900(3) 0.0323(8) Uani 1 1 d . . . C4 C 0.0287(3) 0.4057(2) 0.6772(3) 0.0287(8) Uani 1 1 d . . . C5 C 0.0040(2) 0.3539(2) 0.5802(3) 0.0191(6) Uani 1 1 d . . . C6 C 0.0608(2) 0.3148(2) 0.5616(3) 0.0193(6) Uani 1 1 d . . . C7 C 0.1485(2) 0.3352(3) 0.6442(3) 0.0300(8) Uani 1 1 d . . . C8 C 0.08079(19) 0.1357(2) 0.4548(3) 0.0175(6) Uani 1 1 d . . . C9 C 0.11185(19) 0.0937(2) 0.3960(3) 0.0183(6) Uani 1 1 d . . . C10 C 0.1411(2) 0.0060(2) 0.4165(3) 0.0263(7) Uani 1 1 d . . . C11 C 0.1689(2) -0.0240(2) 0.3562(4) 0.0329(8) Uani 1 1 d . . . C12 C 0.1693(2) 0.0317(3) 0.2806(3) 0.0316(8) Uani 1 1 d . . . C13 C 0.1384(2) 0.1179(2) 0.2625(3) 0.0238(7) Uani 1 1 d . . . C14 C 0.0817(2) 0.3503(2) 0.1344(3) 0.0266(7) Uani 1 1 d . . . C15 C 0.0555(3) 0.3984(3) 0.0353(3) 0.0330(8) Uani 1 1 d . . . C16 C -0.0250(2) 0.4173(2) -0.0445(3) 0.0296(8) Uani 1 1 d . . . C17 C -0.0778(2) 0.3859(2) -0.0240(3) 0.0247(7) Uani 1 1 d . . . C18 C -0.0487(2) 0.3362(2) 0.0760(3) 0.0178(6) Uani 1 1 d . . . C19 C -0.1016(2) 0.2969(2) 0.1014(3) 0.0185(6) Uani 1 1 d . . . C20 C -0.1892(2) 0.3175(3) 0.0233(3) 0.0299(8) Uani 1 1 d . . . C21 C -0.11748(19) 0.12289(19) 0.2244(3) 0.0157(6) Uani 1 1 d . . . C22 C -0.15018(19) 0.0902(2) 0.2851(3) 0.0168(6) Uani 1 1 d . . . C23 C -0.1833(2) 0.0060(2) 0.2691(3) 0.0226(7) Uani 1 1 d . . . C24 C -0.2108(2) -0.0165(2) 0.3331(3) 0.0260(7) Uani 1 1 d . . . C25 C -0.2048(2) 0.0445(2) 0.4095(3) 0.0253(7) Uani 1 1 d . . . C26 C -0.1717(2) 0.1290(2) 0.4200(3) 0.0215(6) Uani 1 1 d . . . N100 N 0.20854(19) 0.25300(18) 0.9886(3) 0.0397(6) Uani 1 1 d . . . O101 O 0.2663(2) 0.2953(3) 1.0663(3) 0.0959(14) Uani 1 1 d . . . O102 O 0.1880(2) 0.2496(2) 0.8868(3) 0.0467(8) Uani 1 1 d . . . O103 O 0.1746(4) 0.2099(4) 1.0166(5) 0.161(3) Uani 1 1 d . . . N200 N -0.03197(14) -0.11188(16) 0.4831(2) 0.0303(5) Uani 1 1 d . . . O201 O 0.01047(16) -0.09643(15) 0.4495(2) 0.0386(5) Uani 1 1 d . . . O202 O -0.02268(13) -0.06365(18) 0.56080(19) 0.0414(5) Uani 1 1 d . . . O203 O -0.08105(19) -0.17367(19) 0.4384(3) 0.0609(9) Uani 1 1 d . . . H1 H -0.186(2) 0.346(2) 0.442(3) 0.037(11) Uiso 1 1 d . . . H2 H -0.144(2) 0.429(2) 0.615(3) 0.017(8) Uiso 1 1 d . . . H3 H -0.016(2) 0.473(2) 0.753(3) 0.038(10) Uiso 1 1 d . . . H4 H 0.072(2) 0.416(2) 0.720(3) 0.027(10) Uiso 1 1 d . . . H4A H 0.045(2) 0.107(3) 0.548(3) 0.036(11) Uiso 1 1 d . . . H4B H 0.055(5) 0.043(5) 0.494(7) 0.14(3) Uiso 1 1 d . . . H7A H 0.157(3) 0.407(3) 0.649(4) 0.074(18) Uiso 1 1 d . . . H7B H 0.168(3) 0.320(3) 0.716(4) 0.038(12) Uiso 1 1 d . . . H7C H 0.1746(18) 0.309(2) 0.614(3) 0.014(7) Uiso 1 1 d . . . H9A H -0.088(2) 0.090(2) 0.135(3) 0.017(9) Uiso 1 1 d . . . H9B H -0.0981(19) 0.014(2) 0.174(3) 0.020(8) Uiso 1 1 d . . . H10 H 0.141(3) -0.027(3) 0.471(4) 0.055(14) Uiso 1 1 d . . . H11 H 0.188(4) -0.071(4) 0.373(5) 0.10(2) Uiso 1 1 d . . . H12 H 0.188(2) 0.015(2) 0.243(3) 0.022(8) Uiso 1 1 d . . . H13 H 0.1399(19) 0.156(2) 0.218(3) 0.009(7) Uiso 1 1 d . . . H14 H 0.135(2) 0.338(2) 0.188(3) 0.017(8) Uiso 1 1 d . . . H15 H 0.094(2) 0.412(3) 0.019(3) 0.037(11) Uiso 1 1 d . . . H16 H -0.0452(19) 0.450(2) -0.115(3) 0.020(8) Uiso 1 1 d . . . H17 H -0.1369(17) 0.3998(18) -0.083(2) 0.008(6) Uiso 1 1 d . . . H20A H -0.220(3) 0.275(3) 0.037(4) 0.051(13) Uiso 1 1 d . . . H20B H -0.195(2) 0.381(3) 0.024(4) 0.040(11) Uiso 1 1 d . . . H20C H -0.207(3) 0.298(3) -0.049(4) 0.037(11) Uiso 1 1 d . . . H23 H -0.188(2) -0.033(2) 0.206(3) 0.016(8) Uiso 1 1 d . . . H24 H -0.2325(18) -0.075(2) 0.318(3) 0.013(7) Uiso 1 1 d . . . H25 H -0.2234(18) 0.033(2) 0.457(3) 0.018(7) Uiso 1 1 d . . . H26 H -0.1661(19) 0.176(2) 0.475(3) 0.020(8) Uiso 1 1 d . . . O2W O 0.03975(19) 0.16738(19) 0.6805(3) 0.0378(6) Uani 1 1 d . . . H2WA H 0.075(3) 0.190(3) 0.747(4) 0.050(13) Uiso 1 1 d . . . H2WB H -0.001(2) 0.130(3) 0.630(3) 0.032(9) Uiso 1 1 d . . . O1W O -0.2374(2) -0.2454(3) 0.2663(3) 0.0453(8) Uani 1 1 d . . . H1WA H -0.197(5) -0.237(5) 0.273(7) 0.17(4) Uiso 1 1 d . . . O3W O -0.07888(19) -0.12943(17) 0.2105(3) 0.0417(6) Uani 1 1 d . . . H3WA H -0.121(3) -0.165(3) 0.178(4) 0.056(12) Uiso 1 1 d . . . H3WB H -0.045(3) -0.146(3) 0.287(5) 0.093(19) 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 0.0170(2) 0.01596(16) 0.01688(17) 0.00176(14) 0.01095(16) 0.00056(14) Cu2 0.0172(2) 0.01530(16) 0.01655(17) -0.00101(14) 0.01168(17) -0.00020(14) N1 0.0219(14) 0.0198(11) 0.0202(12) -0.0001(9) 0.0147(11) -0.0002(10) N2 0.0165(12) 0.0176(11) 0.0172(11) 0.0016(8) 0.0121(10) 0.0013(9) N3 0.0154(13) 0.0170(11) 0.0148(11) 0.0012(8) 0.0082(10) 0.0004(9) N4 0.0262(14) 0.0189(12) 0.0266(13) 0.0037(10) 0.0168(12) 0.0015(10) N5 0.0131(13) 0.0207(12) 0.0216(12) -0.0054(10) 0.0094(11) -0.0003(10) N6 0.0216(14) 0.0209(11) 0.0196(12) 0.0009(9) 0.0141(11) -0.0032(10) N7 0.0149(12) 0.0176(10) 0.0139(11) 0.0004(8) 0.0084(10) -0.0007(9) N8 0.0163(13) 0.0166(10) 0.0180(12) -0.0011(9) 0.0129(11) -0.0037(9) N9 0.0282(14) 0.0194(13) 0.0254(13) -0.0036(10) 0.0193(12) -0.0038(10) N10 0.0147(13) 0.0173(11) 0.0173(11) 0.0016(9) 0.0095(10) 0.0009(9) N11 0.0310(19) 0.0216(14) 0.0298(15) -0.0016(12) 0.0235(15) -0.0019(12) O1 0.0235(13) 0.0208(11) 0.0304(12) 0.0023(9) 0.0170(11) -0.0003(9) O2 0.0252(15) 0.0339(14) 0.0448(16) -0.0037(12) 0.0239(14) 0.0022(11) O3 0.054(2) 0.0297(14) 0.065(2) -0.0234(14) 0.0477(19) -0.0219(13) N12 0.0248(17) 0.0189(13) 0.0202(13) 0.0030(10) 0.0141(13) 0.0056(11) O4 0.0185(12) 0.0258(11) 0.0252(11) -0.0034(9) 0.0121(10) 0.0019(9) O5 0.0415(18) 0.0295(13) 0.0427(16) -0.0004(12) 0.0295(15) -0.0086(12) O6 0.048(2) 0.0307(14) 0.0496(18) 0.0223(12) 0.0365(16) 0.0192(13) C1 0.0294(19) 0.0245(14) 0.0263(15) -0.0003(11) 0.0215(15) 0.0038(12) C2 0.040(2) 0.0296(16) 0.0360(18) -0.0039(13) 0.0318(17) 0.0012(14) C3 0.054(2) 0.0248(15) 0.0308(17) -0.0081(13) 0.0327(18) -0.0050(14) C4 0.035(2) 0.0284(16) 0.0220(15) -0.0092(12) 0.0173(15) -0.0123(14) C5 0.0249(15) 0.0185(12) 0.0190(13) -0.0007(10) 0.0160(12) -0.0005(10) C6 0.0227(16) 0.0191(13) 0.0137(12) -0.0005(10) 0.0098(12) -0.0032(10) C7 0.0190(17) 0.044(2) 0.0214(15) -0.0084(14) 0.0091(14) -0.0067(14) C8 0.0099(13) 0.0219(13) 0.0154(12) -0.0001(10) 0.0050(11) 0.0000(10) C9 0.0131(14) 0.0146(12) 0.0201(13) -0.0028(10) 0.0064(12) -0.0017(10) C10 0.0193(15) 0.0190(13) 0.0311(17) -0.0010(12) 0.0104(13) 0.0012(11) C11 0.0243(17) 0.0198(14) 0.044(2) -0.0087(13) 0.0149(16) 0.0014(12) C12 0.0208(16) 0.0360(18) 0.0348(18) -0.0192(15) 0.0154(15) -0.0003(13) C13 0.0157(15) 0.0294(15) 0.0263(15) -0.0053(12) 0.0128(13) -0.0037(11) C14 0.0232(17) 0.0298(16) 0.0290(16) -0.0004(13) 0.0170(14) -0.0029(13) C15 0.045(2) 0.0317(16) 0.0377(19) 0.0008(14) 0.0328(18) -0.0075(15) C16 0.042(2) 0.0269(16) 0.0271(15) 0.0071(12) 0.0247(15) 0.0033(13) C17 0.0308(18) 0.0229(14) 0.0255(15) 0.0054(11) 0.0197(14) 0.0037(12) C18 0.0202(14) 0.0172(12) 0.0140(12) 0.0003(9) 0.0094(11) 0.0005(10) C19 0.0165(14) 0.0232(13) 0.0175(13) -0.0025(10) 0.0113(12) -0.0024(10) C20 0.0236(19) 0.0413(19) 0.0222(16) 0.0080(14) 0.0125(15) 0.0024(14) C21 0.0152(14) 0.0134(11) 0.0142(12) -0.0024(9) 0.0067(11) -0.0002(9) C22 0.0123(14) 0.0188(12) 0.0167(12) 0.0028(10) 0.0075(11) -0.0001(10) C23 0.0199(15) 0.0163(12) 0.0280(15) 0.0009(11) 0.0127(13) -0.0010(10) C24 0.0194(15) 0.0209(14) 0.0358(17) 0.0086(12) 0.0158(14) -0.0002(11) C25 0.0185(15) 0.0318(15) 0.0279(15) 0.0101(12) 0.0153(13) 0.0029(11) C26 0.0189(15) 0.0242(14) 0.0229(14) 0.0070(12) 0.0135(13) 0.0026(11) N100 0.0513(18) 0.0322(14) 0.0497(17) -0.0037(12) 0.0381(16) -0.0058(12) O101 0.068(2) 0.179(4) 0.0495(18) -0.041(2) 0.0405(18) -0.052(2) O102 0.058(2) 0.0443(15) 0.0372(16) 0.0011(13) 0.0288(16) -0.0079(15) O103 0.266(7) 0.161(5) 0.156(4) -0.093(4) 0.180(5) -0.148(5) N200 0.0211(12) 0.0315(12) 0.0304(13) 0.0127(10) 0.0115(11) 0.0000(9) O201 0.0521(15) 0.0299(11) 0.0508(14) -0.0070(10) 0.0401(13) -0.0079(10) O202 0.0319(12) 0.0682(16) 0.0276(11) 0.0045(11) 0.0199(10) 0.0031(11) O203 0.0452(18) 0.0350(14) 0.067(2) 0.0148(13) 0.0155(16) -0.0150(12) O2W 0.0421(16) 0.0384(13) 0.0366(14) 0.0061(11) 0.0259(13) 0.0012(11) O1W 0.0321(16) 0.0660(19) 0.0412(17) -0.0041(14) 0.0241(14) -0.0044(13) O3W 0.0563(17) 0.0339(12) 0.0438(14) -0.0005(11) 0.0351(14) 0.0019(12) _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 Cu2 3.9303(8) . ? Cu1 N3 1.967(3) . yes Cu1 N6 1.988(3) . yes Cu1 N5 2.021(3) . yes Cu1 O1 2.043(3) . yes Cu1 O2 2.591(3) . ? Cu1 N7 2.198(3) . yes Cu2 N8 1.965(3) . yes Cu2 N1 1.996(3) . yes Cu2 N10 2.029(3) . yes Cu2 O4 2.081(3) . yes Cu2 O5 2.562(3) . ? Cu2 N2 2.159(3) . yes N1 C1 1.327(4) . ? N1 C5 1.353(5) . ? N2 C6 1.276(4) . ? N2 N3 1.401(4) . yes N3 C8 1.314(4) . ? N4 C8 1.325(4) . ? N4 H4A 0.83(4) . ? N4 H4B 0.69(8) . ? N5 C13 1.342(4) . ? N5 C9 1.352(4) . ? N6 C14 1.346(5) . ? N6 C18 1.363(4) . ? N7 C19 1.281(4) . ? N7 N8 1.404(4) . ? N8 C21 1.320(4) . ? N9 C21 1.336(4) . ? N9 H9A 0.80(4) . ? N9 H9B 0.77(4) . ? N10 C26 1.335(4) . ? N10 C22 1.346(4) . ? N11 O3 1.224(4) . ? N11 O2 1.239(4) . ? N11 O1 1.299(4) . ? N12 O6 1.231(4) . ? N12 O5 1.252(4) . ? N12 O4 1.271(4) . ? C1 C2 1.402(5) . ? C1 H1 1.03(4) . ? C2 C3 1.360(6) . ? C2 H2 0.86(3) . ? C3 C4 1.378(5) . ? C3 H3 0.96(4) . ? C4 C5 1.390(4) . ? C4 H4 0.75(4) . ? C5 C6 1.485(5) . ? C6 C7 1.492(5) . ? C7 H7A 1.08(5) . ? C7 H7B 0.88(4) . ? C7 H7C 0.96(3) . ? C8 C9 1.482(4) . ? C9 C10 1.395(4) . ? C10 C11 1.379(5) . ? C10 H10 0.93(5) . ? C11 C12 1.370(6) . ? C11 H11 0.78(6) . ? C12 C13 1.388(5) . ? C12 H12 0.88(3) . ? C13 H13 0.87(3) . ? C14 C15 1.376(5) . ? C14 H14 0.90(3) . ? C15 C16 1.374(6) . ? C15 H15 0.99(4) . ? C16 C17 1.388(5) . ? C16 H16 0.96(3) . ? C17 C18 1.385(4) . ? C17 H17 1.01(3) . ? C18 C19 1.481(4) . ? C19 C20 1.488(5) . ? C20 H20A 0.99(4) . ? C20 H20B 0.95(4) . ? C20 H20C 0.90(4) . ? C21 C22 1.481(4) . ? C22 C23 1.381(4) . ? C23 C24 1.391(4) . ? C23 H23 1.03(3) . ? C24 C25 1.371(5) . ? C24 H24 0.94(3) . ? C25 C26 1.399(5) . ? C25 H25 0.98(3) . ? C26 H26 1.01(3) . ? N100 O103 1.194(4) . ? N100 O101 1.210(4) . ? N100 O102 1.251(4) . ? O101 H3WA 1.98(5) 3_556 ? O102 H2WA 2.16(4) . ? N200 O203 1.230(4) . ? N200 O202 1.239(4) . ? N200 O201 1.264(3) . ? O201 H3WB 2.01(5) . ? O201 H4B 2.20(8) . ? O202 H9A 2.21(4) 2 ? O203 H1WA 2.33(8) . ? O2W H4A 2.17(4) . ? O2W H2WA 0.84(4) . ? O2W H2WB 0.90(4) . ? O1W H1WA 0.80(8) . ? O3W H9B 2.17(4) . ? O3W H3WA 0.88(4) . ? O3W H3WB 0.91(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N6 168.71(13) . . yes N3 Cu1 N5 80.75(11) . . yes N6 Cu1 N5 104.82(11) . . yes N3 Cu1 O1 89.15(10) . . yes N6 Cu1 O1 89.85(11) . . yes N5 Cu1 O1 152.68(11) . . yes N3 Cu1 N7 92.07(12) . . yes N6 Cu1 N7 77.21(11) . . yes N5 Cu1 N7 102.48(11) . . yes O1 Cu1 N7 103.20(10) . . yes N8 Cu2 N1 171.07(12) . . yes N8 Cu2 N10 80.32(10) . . yes N1 Cu2 N10 103.49(11) . . yes N8 Cu2 O4 91.50(10) . . yes N1 Cu2 O4 88.67(11) . . yes N10 Cu2 O4 151.86(11) . . yes N8 Cu2 N2 93.49(12) . . yes N1 Cu2 N2 77.69(12) . . yes N10 Cu2 N2 107.36(10) . . yes O4 Cu2 N2 99.93(10) . . yes C1 N1 C5 119.7(3) . . ? C1 N1 Cu2 124.5(3) . . ? C5 N1 Cu2 115.5(2) . . ? C6 N2 N3 119.6(3) . . ? C6 N2 Cu2 113.7(2) . . ? N3 N2 Cu2 124.8(2) . . ? C8 N3 N2 114.6(3) . . ? C8 N3 Cu1 114.3(2) . . ? N2 N3 Cu1 117.9(2) . . ? C8 N4 H4A 127(3) . . ? C8 N4 H4B 111(7) . . ? H4A N4 H4B 121(7) . . ? C13 N5 C9 119.5(3) . . ? C13 N5 Cu1 128.1(2) . . ? C9 N5 Cu1 112.4(2) . . ? C14 N6 C18 118.6(3) . . ? C14 N6 Cu1 125.5(3) . . ? C18 N6 Cu1 115.3(2) . . ? C19 N7 N8 117.9(3) . . ? C19 N7 Cu1 111.7(2) . . ? N8 N7 Cu1 125.07(19) . . ? C21 N8 N7 116.7(3) . . ? C21 N8 Cu2 115.0(2) . . ? N7 N8 Cu2 118.2(2) . . ? C21 N9 H9A 113(3) . . ? C21 N9 H9B 129(2) . . ? H9A N9 H9B 117(4) . . ? C26 N10 C22 119.4(3) . . ? C26 N10 Cu2 127.1(2) . . ? C22 N10 Cu2 113.4(2) . . ? O3 N11 O2 123.0(3) . . ? O3 N11 O1 118.8(3) . . ? O2 N11 O1 118.1(3) . . ? N11 O1 Cu1 105.77(19) . . ? O6 N12 O5 122.3(3) . . ? O6 N12 O4 119.2(3) . . ? O5 N12 O4 118.5(3) . . ? N12 O4 Cu2 104.5(2) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 112(2) . . ? C2 C1 H1 126(2) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 123(2) . . ? C1 C2 H2 118(2) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 116(2) . . ? C4 C3 H3 124(2) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 123(3) . . ? C5 C4 H4 118(3) . . ? N1 C5 C4 120.6(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 123.2(3) . . ? N2 C6 C5 114.4(3) . . ? N2 C6 C7 124.9(3) . . ? C5 C6 C7 120.7(3) . . ? C6 C7 H7A 109(3) . . ? C6 C7 H7B 110(3) . . ? H7A C7 H7B 103(4) . . ? C6 C7 H7C 108.6(18) . . ? H7A C7 H7C 109(3) . . ? H7B C7 H7C 116(3) . . ? N3 C8 N4 124.6(3) . . ? N3 C8 C9 113.6(3) . . ? N4 C8 C9 121.8(3) . . ? N5 C9 C10 121.6(3) . . ? N5 C9 C8 114.2(3) . . ? C10 C9 C8 124.2(3) . . ? C11 C10 C9 117.9(3) . . ? C11 C10 H10 125(3) . . ? C9 C10 H10 117(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 122(4) . . ? C10 C11 H11 117(4) . . ? C11 C12 C13 118.8(3) . . ? C11 C12 H12 123(2) . . ? C13 C12 H12 119(2) . . ? N5 C13 C12 121.5(3) . . ? N5 C13 H13 117(2) . . ? C12 C13 H13 121(2) . . ? N6 C14 C15 122.7(4) . . ? N6 C14 H14 118(2) . . ? C15 C14 H14 120(2) . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 122(2) . . ? C14 C15 H15 119(2) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 121.1(19) . . ? C17 C16 H16 119.8(19) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 121.4(16) . . ? C16 C17 H17 118.9(16) . . ? N6 C18 C17 120.8(3) . . ? N6 C18 C19 116.3(3) . . ? C17 C18 C19 122.9(3) . . ? N7 C19 C18 114.4(3) . . ? N7 C19 C20 125.9(3) . . ? C18 C19 C20 119.7(3) . . ? C19 C20 H20A 111(2) . . ? C19 C20 H20B 107(3) . . ? H20A C20 H20B 122(4) . . ? C19 C20 H20C 105(3) . . ? H20A C20 H20C 99(3) . . ? H20B C20 H20C 111(4) . . ? N8 C21 N9 125.5(3) . . ? N8 C21 C22 113.6(3) . . ? N9 C21 C22 120.8(3) . . ? N10 C22 C23 122.0(3) . . ? N10 C22 C21 113.6(3) . . ? C23 C22 C21 124.4(3) . . ? C22 C23 C24 118.5(3) . . ? C22 C23 H23 114.9(19) . . ? C24 C23 H23 126.6(18) . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 126.4(19) . . ? C23 C24 H24 113.8(19) . . ? C24 C25 C26 118.7(3) . . ? C24 C25 H25 124.0(18) . . ? C26 C25 H25 117.2(18) . . ? N10 C26 C25 121.6(3) . . ? N10 C26 H26 116.6(18) . . ? C25 C26 H26 121.8(18) . . ? O103 N100 O101 115.8(4) . . ? O103 N100 O102 121.3(4) . . ? O101 N100 O102 122.7(3) . . ? N100 O101 H3WA 159.6(13) . 3_556 ? N100 O102 H2WA 120.6(12) . . ? O203 N200 O202 121.9(3) . . ? O203 N200 O201 119.6(3) . . ? O202 N200 O201 118.5(2) . . ? N200 O201 H3WB 109.2(16) . . ? N200 O201 H4B 110(2) . . ? H3WB O201 H4B 122(3) . . ? N200 O202 H9A 121.7(10) . 2 ? N200 O203 H1WA 149(2) . . ? H4A O2W H2WA 133(3) . . ? H4A O2W H2WB 64(2) . . ? H2WA O2W H2WB 155(4) . . ? H9B O3W H3WA 119(3) . . ? H9B O3W H3WB 116(3) . . ? H3WA O3W H3WB 105(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 N3 N2 Cu2 57.2(3) . . . . ? Cu1 N7 N8 Cu2 53.4(3) . . . . ? #===END data_x532 #(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 Cu2 N14 O13.50' _chemical_formula_weight 876.68 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.709(1) _cell_length_b 17.688(2) _cell_length_c 19.155(2) _cell_angle_alpha 91.691(4) _cell_angle_beta 95.085(3) _cell_angle_gamma 97.501(3) _cell_volume 3245.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 401 _cell_measurement_theta_min 13.67 _cell_measurement_theta_max 19.02 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 150(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 'Bruker SMART-CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39180 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 28.27 _reflns_number_total 15964 _reflns_number_gt 12464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+5.2459P] 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 15964 _refine_ls_number_parameters 1056 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.148 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.084 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 0.59046(3) 0.769079(18) 0.201435(17) 0.01852(7) Uani 1 1 d . . . Cu2 Cu 0.24671(3) 0.778673(18) 0.078963(17) 0.01786(7) Uani 1 1 d . . . Cu3 Cu 0.17867(3) 0.275331(17) 0.312593(17) 0.01582(7) Uani 1 1 d . . . Cu4 Cu -0.15378(3) 0.225508(17) 0.414524(16) 0.01475(7) Uani 1 1 d . . . N1 N 0.7151(2) 0.69016(12) 0.22216(12) 0.0180(4) Uani 1 1 d . . . N2 N 0.4753(2) 0.67782(12) 0.14623(11) 0.0164(4) Uani 1 1 d . . . N3 N 0.3454(2) 0.67899(12) 0.11741(11) 0.0176(4) Uani 1 1 d . . . N4 N 0.0912(2) 0.69412(13) 0.05732(12) 0.0200(5) Uani 1 1 d . . . N5 N 0.2873(2) 0.80535(12) -0.01948(11) 0.0169(4) Uani 1 1 d . . . N6 N 0.4188(2) 0.84770(12) 0.09992(11) 0.0156(4) Uani 1 1 d . . . N7 N 0.4918(2) 0.85066(12) 0.16682(11) 0.0151(4) Uani 1 1 d . . . N8 N 0.6052(2) 0.83434(12) 0.29117(11) 0.0165(4) Uani 1 1 d . . . N9 N 0.6080(2) 0.91757(14) 0.05225(14) 0.0218(5) Uani 1 1 d . . . H1N H 0.638(3) 0.9364(19) 0.0185(18) 0.024(9) Uiso 1 1 d . . . H2N H 0.656(4) 0.927(2) 0.093(2) 0.039(10) Uiso 1 1 d . . . N10 N 0.3847(3) 0.95584(14) 0.19909(14) 0.0221(5) Uani 1 1 d . . . H3N H 0.341(3) 0.9577(18) 0.1574(19) 0.027(9) Uiso 1 1 d . . . H4N H 0.373(4) 0.988(2) 0.228(2) 0.035(10) Uiso 1 1 d . . . N11 N 0.3280(2) 0.36335(12) 0.31853(11) 0.0170(4) Uani 1 1 d . . . N12 N 0.0868(2) 0.35125(12) 0.37115(11) 0.0145(4) Uani 1 1 d . . . N13 N -0.0376(2) 0.33690(12) 0.39594(11) 0.0154(4) Uani 1 1 d . . . N14 N -0.2822(2) 0.29501(12) 0.44598(11) 0.0149(4) Uani 1 1 d . . . N15 N -0.1070(2) 0.17974(12) 0.50774(11) 0.0145(4) Uani 1 1 d . . . N16 N -0.0065(2) 0.16927(11) 0.38900(11) 0.0131(4) Uani 1 1 d . . . N17 N 0.0612(2) 0.18209(11) 0.32748(11) 0.0135(4) Uani 1 1 d . . . N18 N 0.1983(2) 0.21758(12) 0.22207(11) 0.0147(4) Uani 1 1 d . . . N19 N 0.1589(2) 0.09131(13) 0.42976(13) 0.0188(5) Uani 1 1 d . . . H5N H 0.190(3) 0.0662(18) 0.4609(17) 0.018(8) Uiso 1 1 d . . . H6N H 0.200(3) 0.0944(19) 0.3899(19) 0.030(9) Uiso 1 1 d . . . N20 N -0.0662(2) 0.07142(13) 0.27397(13) 0.0188(5) Uani 1 1 d . . . H7N H -0.120(4) 0.0633(19) 0.3074(19) 0.033(9) Uiso 1 1 d . . . H8N H -0.081(4) 0.038(2) 0.2388(19) 0.034(9) Uiso 1 1 d . . . N21 N 0.5767(3) 0.36762(15) 0.06960(14) 0.0305(6) Uani 1 1 d . . . N22 N 0.8522(2) 0.65871(12) 0.45434(12) 0.0214(5) Uani 1 1 d . . . N23 N 0.3433(3) 0.68759(13) 0.31262(12) 0.0230(5) Uani 1 1 d . . . N24 N 0.7002(2) 0.04939(12) 0.43195(12) 0.0192(5) Uani 1 1 d . . . N25 N 0.0748(3) 0.39004(14) 0.17852(13) 0.0265(5) Uani 1 1 d . . . N26 N 0.1632(2) 0.95140(12) 0.02802(12) 0.0187(4) Uani 1 1 d . . . N27 N 0.8701(2) 0.89266(13) 0.17879(12) 0.0198(5) Uani 1 1 d . . . N28 N 0.3988(2) 0.13226(13) 0.30964(12) 0.0203(5) Uani 1 1 d . . . O1 O 0.1671(2) 0.79574(14) 0.17180(12) 0.0276(5) Uani 1 1 d . . . H12W H 0.200(4) 0.775(2) 0.208(2) 0.049(12) Uiso 1 1 d . . . H11W H 0.124(4) 0.825(2) 0.1799(19) 0.030(10) Uiso 1 1 d . . . O2 O -0.2495(2) 0.21476(12) 0.31403(10) 0.0196(4) Uani 1 1 d . . . H22W H -0.318(5) 0.192(3) 0.309(2) 0.059(15) Uiso 1 1 d . . . H21W H -0.252(4) 0.258(2) 0.291(2) 0.050(12) Uiso 1 1 d . . . O3 O 0.7545(3) 0.34065(13) 0.23686(13) 0.0315(5) Uani 1 1 d . . . H32W H 0.703(4) 0.342(2) 0.200(2) 0.048(12) Uiso 1 1 d . . . H31W H 0.830(5) 0.343(2) 0.224(2) 0.053(13) Uiso 1 1 d . . . O4 O 0.6930(4) 0.4035(2) 0.06237(16) 0.0759(11) Uani 1 1 d . . . O5 O 0.5447(3) 0.35892(18) 0.13108(13) 0.0524(7) Uani 1 1 d . . . O6 O 0.4984(3) 0.34082(19) 0.01842(14) 0.0565(8) Uani 1 1 d . . . O7 O 0.7688(3) 0.60204(13) 0.46626(18) 0.0572(9) Uani 1 1 d . . . O8 O 0.8190(2) 0.72373(12) 0.46276(15) 0.0413(6) Uani 1 1 d . . . O9 O 0.9711(2) 0.64938(12) 0.43769(13) 0.0350(5) Uani 1 1 d . . . O10 O 0.3203(3) 0.74379(14) 0.27689(15) 0.0505(7) Uani 1 1 d . . . O11 O 0.4568(2) 0.66306(13) 0.30893(16) 0.0472(7) Uani 1 1 d . . . O12 O 0.2577(2) 0.65948(12) 0.35208(13) 0.0344(5) Uani 1 1 d . . . O13 O 0.1146(3) 0.45451(16) 0.20845(14) 0.0543(7) Uani 1 1 d . . . O14 O 0.0784(4) 0.38201(16) 0.11608(14) 0.0728(10) Uani 1 1 d . . . O15 O 0.0246(2) 0.33685(13) 0.21582(12) 0.0352(5) Uani 1 1 d . . . O16 O 0.6314(2) 0.10323(11) 0.41923(11) 0.0290(5) Uani 1 1 d . . . O17 O 0.7687(2) 0.02444(11) 0.38575(11) 0.0254(4) Uani 1 1 d . . . O18 O 0.7018(2) 0.02037(11) 0.49114(10) 0.0226(4) Uani 1 1 d . . . O19 O 0.1270(2) 0.97116(13) -0.03149(11) 0.0323(5) Uani 1 1 d . . . O20 O 0.0992(2) 0.89512(11) 0.05494(11) 0.0277(4) Uani 1 1 d . . . O21 O 0.2710(2) 0.98934(11) 0.06228(10) 0.0228(4) Uani 1 1 d . . . O22 O 0.9932(2) 0.90096(13) 0.20702(11) 0.0303(5) Uani 1 1 d . . . O23 O 0.8042(2) 0.94948(11) 0.17676(11) 0.0248(4) Uani 1 1 d . . . O24 O 0.8130(2) 0.82885(11) 0.15381(11) 0.0279(5) Uani 1 1 d . . . O25 O 0.4928(2) 0.13329(16) 0.26947(12) 0.0415(6) Uani 1 1 d . . . O26 O 0.3912(2) 0.18900(11) 0.34927(11) 0.0268(4) Uani 1 1 d . . . O27 O 0.30908(19) 0.07349(10) 0.30922(10) 0.0213(4) Uani 1 1 d . . . C1 C 0.8429(3) 0.70249(17) 0.25655(15) 0.0235(6) Uani 1 1 d . . . H11 H 0.8776 0.7525 0.2749 0.028 Uiso 1 1 calc R . . C2 C 0.9269(3) 0.64493(18) 0.26646(16) 0.0284(6) Uani 1 1 d . . . H21 H 1.0159 0.6550 0.2923 0.034 Uiso 1 1 calc R . . C3 C 0.8773(3) 0.57252(18) 0.23770(16) 0.0282(6) Uani 1 1 d . . . H31 H 0.9328 0.5323 0.2431 0.034 Uiso 1 1 calc R . . C4 C 0.7454(3) 0.55917(16) 0.20087(15) 0.0234(6) Uani 1 1 d . . . H41 H 0.7102 0.5101 0.1806 0.028 Uiso 1 1 calc R . . C5 C 0.6665(3) 0.61922(15) 0.19447(13) 0.0175(5) Uani 1 1 d . . . C6 C 0.5248(3) 0.61150(15) 0.15690(14) 0.0183(5) Uani 1 1 d . . . C7 C 0.4440(3) 0.54154(15) 0.13634(15) 0.0227(6) Uani 1 1 d . . . H71 H 0.4811 0.4948 0.1424 0.027 Uiso 1 1 calc R . . C8 C 0.3103(3) 0.54251(16) 0.10733(15) 0.0236(6) Uani 1 1 d . . . H81 H 0.2516 0.4964 0.0931 0.028 Uiso 1 1 calc R . . C9 C 0.2622(3) 0.61386(15) 0.09925(14) 0.0189(5) Uani 1 1 d . . . C10 C 0.1165(3) 0.62270(15) 0.07290(14) 0.0199(5) Uani 1 1 d . . . C11 C 0.0091(3) 0.56199(16) 0.06831(14) 0.0236(6) Uani 1 1 d . . . H111 H 0.0279 0.5120 0.0790 0.028 Uiso 1 1 calc R . . C12 C -0.1265(3) 0.57566(17) 0.04779(15) 0.0265(6) Uani 1 1 d . . . H121 H -0.2013 0.5349 0.0443 0.032 Uiso 1 1 calc R . . C13 C -0.1515(3) 0.64850(18) 0.03256(15) 0.0267(6) Uani 1 1 d . . . H131 H -0.2433 0.6587 0.0184 0.032 Uiso 1 1 calc R . . C14 C -0.0401(3) 0.70669(17) 0.03831(15) 0.0246(6) Uani 1 1 d . . . H141 H -0.0572 0.7571 0.0285 0.030 Uiso 1 1 calc R . . C15 C 0.2061(3) 0.78441(15) -0.07858(14) 0.0205(5) Uani 1 1 d . . . H151 H 0.1293 0.7455 -0.0773 0.025 Uiso 1 1 calc R . . C16 C 0.2305(3) 0.81775(16) -0.14178(14) 0.0217(6) Uani 1 1 d . . . H161 H 0.1712 0.8019 -0.1831 0.026 Uiso 1 1 calc R . . C17 C 0.3423(3) 0.87447(16) -0.14362(14) 0.0225(6) Uani 1 1 d . . . H171 H 0.3591 0.8991 -0.1860 0.027 Uiso 1 1 calc R . . C18 C 0.4304(3) 0.89517(16) -0.08260(14) 0.0210(5) Uani 1 1 d . . . H181 H 0.5095 0.9329 -0.0829 0.025 Uiso 1 1 calc R . . C19 C 0.3995(3) 0.85935(14) -0.02162(13) 0.0153(5) Uani 1 1 d . . . C20 C 0.4831(3) 0.87686(14) 0.04756(14) 0.0164(5) Uani 1 1 d . . . C21 C 0.4625(3) 0.90116(14) 0.21322(14) 0.0165(5) Uani 1 1 d . . . C22 C 0.5189(3) 0.88888(14) 0.28635(13) 0.0152(5) Uani 1 1 d . . . C23 C 0.4731(3) 0.92227(14) 0.34497(14) 0.0177(5) Uani 1 1 d . . . H231 H 0.4139 0.9609 0.3401 0.021 Uiso 1 1 calc R . . C24 C 0.5152(3) 0.89826(15) 0.41101(14) 0.0194(5) Uani 1 1 d . . . H241 H 0.4820 0.9184 0.4519 0.023 Uiso 1 1 calc R . . C25 C 0.6069(3) 0.84435(15) 0.41599(14) 0.0200(5) Uani 1 1 d . . . H251 H 0.6404 0.8285 0.4606 0.024 Uiso 1 1 calc R . . C26 C 0.6493(3) 0.81370(15) 0.35510(14) 0.0192(5) Uani 1 1 d . . . H261 H 0.7119 0.7767 0.3590 0.023 Uiso 1 1 calc R . . C27 C 0.4584(3) 0.36401(15) 0.30031(14) 0.0182(5) Uani 1 1 d . . . H271 H 0.4861 0.3177 0.2836 0.022 Uiso 1 1 calc R . . C28 C 0.5540(3) 0.42969(15) 0.30497(15) 0.0208(5) Uani 1 1 d . . . H281 H 0.6458 0.4282 0.2920 0.025 Uiso 1 1 calc R . . C29 C 0.5142(3) 0.49765(15) 0.32882(15) 0.0211(5) Uani 1 1 d . . . H291 H 0.5777 0.5435 0.3317 0.025 Uiso 1 1 calc R . . C30 C 0.3796(3) 0.49751(15) 0.34836(14) 0.0189(5) Uani 1 1 d . . . H301 H 0.3497 0.5433 0.3648 0.023 Uiso 1 1 calc R . . C31 C 0.2901(3) 0.42961(14) 0.34343(13) 0.0158(5) Uani 1 1 d . . . C32 C 0.1495(3) 0.42310(14) 0.36795(13) 0.0148(5) Uani 1 1 d . . . C33 C 0.0841(3) 0.48560(14) 0.38814(14) 0.0183(5) Uani 1 1 d . . . H331 H 0.1271 0.5365 0.3841 0.022 Uiso 1 1 calc R . . C34 C -0.0437(3) 0.47092(14) 0.41381(14) 0.0179(5) Uani 1 1 d . . . H341 H -0.0918 0.5113 0.4281 0.022 Uiso 1 1 calc R . . C35 C -0.1015(3) 0.39436(14) 0.41843(13) 0.0144(5) Uani 1 1 d . . . C36 C -0.2378(3) 0.37120(14) 0.44680(13) 0.0150(5) Uani 1 1 d . . . C37 C -0.3191(3) 0.42399(15) 0.47046(14) 0.0193(5) Uani 1 1 d . . . H371 H -0.2863 0.4771 0.4719 0.023 Uiso 1 1 calc R . . C38 C -0.4494(3) 0.39780(15) 0.49202(14) 0.0197(5) Uani 1 1 d . . . H381 H -0.5060 0.4330 0.5088 0.024 Uiso 1 1 calc R . . C39 C -0.4964(3) 0.32051(15) 0.48905(14) 0.0198(5) Uani 1 1 d . . . H391 H -0.5863 0.3019 0.5022 0.024 Uiso 1 1 calc R . . C40 C -0.4085(3) 0.27042(15) 0.46616(14) 0.0181(5) Uani 1 1 d . . . H401 H -0.4392 0.2171 0.4648 0.022 Uiso 1 1 calc R . . C41 C -0.1618(3) 0.18987(15) 0.56847(14) 0.0188(5) Uani 1 1 d . . . H411 H -0.2280 0.2247 0.5710 0.023 Uiso 1 1 calc R . . C42 C -0.1249(3) 0.15098(16) 0.62803(14) 0.0237(6) Uani 1 1 d . . . H421 H -0.1641 0.1600 0.6707 0.028 Uiso 1 1 calc R . . C43 C -0.0308(3) 0.09916(16) 0.62438(14) 0.0224(6) Uani 1 1 d . . . H431 H -0.0071 0.0706 0.6639 0.027 Uiso 1 1 calc R . . C44 C 0.0286(3) 0.08955(15) 0.56174(14) 0.0183(5) Uani 1 1 d . . . H441 H 0.0955 0.0553 0.5581 0.022 Uiso 1 1 calc R . . C45 C -0.0111(2) 0.13055(13) 0.50517(13) 0.0137(5) Uani 1 1 d . . . C46 C 0.0520(2) 0.12905(13) 0.43723(13) 0.0134(5) Uani 1 1 d . . . C47 C 0.0273(2) 0.13279(14) 0.27445(13) 0.0138(5) Uani 1 1 d . . . C48 C 0.1049(2) 0.15258(14) 0.21181(13) 0.0140(5) Uani 1 1 d . . . C49 C 0.0816(3) 0.11160(15) 0.14835(14) 0.0182(5) Uani 1 1 d . . . H491 H 0.0164 0.0664 0.1427 0.022 Uiso 1 1 calc R . . C50 C 0.1557(3) 0.13804(16) 0.09275(14) 0.0208(5) Uani 1 1 d . . . H501 H 0.1400 0.1118 0.0482 0.025 Uiso 1 1 calc R . . C51 C 0.2526(3) 0.20311(16) 0.10344(14) 0.0217(5) Uani 1 1 d . . . H511 H 0.3063 0.2212 0.0668 0.026 Uiso 1 1 calc R . . C52 C 0.2700(3) 0.24160(15) 0.16866(14) 0.0191(5) Uani 1 1 d . . . H521 H 0.3354 0.2867 0.1755 0.023 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 0.01861(16) 0.01651(15) 0.02037(17) -0.00217(12) -0.00324(12) 0.00618(12) Cu2 0.01576(15) 0.02039(16) 0.01622(16) 0.00241(12) 0.00068(12) -0.00193(12) Cu3 0.01479(15) 0.01364(14) 0.01898(16) -0.00271(12) 0.00631(12) -0.00078(11) Cu4 0.01567(15) 0.01423(14) 0.01626(15) 0.00220(11) 0.00520(11) 0.00633(11) N1 0.0150(10) 0.0195(11) 0.0203(11) 0.0027(9) 0.0042(8) 0.0034(8) N2 0.0164(10) 0.0170(10) 0.0162(11) -0.0002(8) 0.0029(8) 0.0028(8) N3 0.0151(10) 0.0198(11) 0.0180(11) 0.0003(9) 0.0020(8) 0.0020(8) N4 0.0171(11) 0.0226(11) 0.0192(11) 0.0023(9) 0.0015(9) -0.0021(9) N5 0.0177(11) 0.0159(10) 0.0171(11) -0.0003(8) 0.0013(8) 0.0027(8) N6 0.0166(10) 0.0166(10) 0.0130(10) 0.0008(8) -0.0002(8) 0.0011(8) N7 0.0151(10) 0.0166(10) 0.0133(10) 0.0004(8) -0.0013(8) 0.0029(8) N8 0.0159(10) 0.0162(10) 0.0173(11) 0.0010(8) 0.0011(8) 0.0019(8) N9 0.0198(12) 0.0253(12) 0.0194(12) 0.0036(10) 0.0017(10) -0.0015(9) N10 0.0276(13) 0.0199(12) 0.0198(12) -0.0017(10) -0.0030(10) 0.0108(10) N11 0.0152(10) 0.0157(10) 0.0202(11) 0.0005(8) 0.0047(8) 0.0004(8) N12 0.0145(10) 0.0142(10) 0.0155(10) 0.0012(8) 0.0042(8) 0.0023(8) N13 0.0145(10) 0.0148(10) 0.0176(11) 0.0014(8) 0.0027(8) 0.0036(8) N14 0.0153(10) 0.0139(10) 0.0163(10) 0.0011(8) 0.0046(8) 0.0030(8) N15 0.0128(10) 0.0150(10) 0.0150(10) 0.0001(8) 0.0018(8) -0.0005(8) N16 0.0131(10) 0.0134(9) 0.0136(10) 0.0015(8) 0.0043(8) 0.0030(8) N17 0.0135(10) 0.0141(10) 0.0139(10) 0.0019(8) 0.0039(8) 0.0029(8) N18 0.0138(10) 0.0156(10) 0.0155(10) 0.0004(8) 0.0031(8) 0.0035(8) N19 0.0204(11) 0.0217(11) 0.0168(11) 0.0062(9) 0.0055(9) 0.0089(9) N20 0.0208(11) 0.0157(11) 0.0194(12) -0.0020(9) 0.0046(9) -0.0010(9) N21 0.0318(14) 0.0313(14) 0.0298(14) 0.0037(11) 0.0096(11) 0.0049(11) N22 0.0218(12) 0.0158(11) 0.0259(12) 0.0023(9) 0.0005(9) 0.0005(9) N23 0.0266(12) 0.0193(11) 0.0230(12) 0.0008(9) 0.0016(10) 0.0029(9) N24 0.0147(10) 0.0135(10) 0.0282(12) 0.0005(9) -0.0003(9) -0.0005(8) N25 0.0284(13) 0.0272(13) 0.0248(13) 0.0042(10) 0.0023(10) 0.0064(10) N26 0.0169(11) 0.0191(11) 0.0208(11) -0.0010(9) 0.0017(9) 0.0053(9) N27 0.0199(11) 0.0222(11) 0.0176(11) 0.0017(9) 0.0028(9) 0.0028(9) N28 0.0155(11) 0.0268(12) 0.0188(11) 0.0049(9) -0.0006(9) 0.0040(9) O1 0.0295(12) 0.0338(12) 0.0245(11) 0.0077(9) 0.0092(9) 0.0166(10) O2 0.0162(10) 0.0231(10) 0.0188(10) 0.0019(8) 0.0012(8) 0.0003(8) O3 0.0294(12) 0.0352(12) 0.0342(13) 0.0075(10) 0.0113(11) 0.0135(10) O4 0.075(2) 0.087(2) 0.0521(19) 0.0036(17) 0.0142(16) -0.0484(19) O5 0.0376(14) 0.086(2) 0.0362(14) 0.0208(14) 0.0147(11) 0.0077(14) O6 0.0351(14) 0.089(2) 0.0420(16) -0.0068(15) -0.0007(12) 0.0004(14) O7 0.0378(14) 0.0165(11) 0.122(3) 0.0034(13) 0.0416(16) -0.0001(10) O8 0.0223(11) 0.0147(10) 0.087(2) 0.0031(11) 0.0000(12) 0.0048(8) O9 0.0261(11) 0.0282(11) 0.0516(15) -0.0038(10) 0.0128(10) 0.0018(9) O10 0.0496(16) 0.0396(14) 0.0574(17) 0.0279(13) -0.0166(13) -0.0036(12) O11 0.0336(13) 0.0267(12) 0.087(2) 0.0050(12) 0.0311(13) 0.0074(10) O12 0.0334(12) 0.0244(11) 0.0495(14) 0.0054(10) 0.0229(11) 0.0050(9) O13 0.075(2) 0.0443(15) 0.0408(16) -0.0023(12) 0.0014(14) 0.0032(14) O14 0.141(3) 0.0418(16) 0.0286(15) -0.0001(12) 0.0084(17) -0.0119(18) O15 0.0254(11) 0.0398(13) 0.0445(14) 0.0223(11) 0.0100(10) 0.0108(10) O16 0.0312(11) 0.0222(10) 0.0350(12) 0.0013(9) -0.0046(9) 0.0141(9) O17 0.0235(10) 0.0232(10) 0.0320(11) 0.0051(8) 0.0128(8) 0.0040(8) O18 0.0242(10) 0.0205(9) 0.0231(10) 0.0030(8) 0.0010(8) 0.0033(8) O19 0.0295(11) 0.0449(13) 0.0195(10) 0.0073(9) -0.0036(9) -0.0036(10) O20 0.0236(10) 0.0236(10) 0.0367(12) 0.0090(9) 0.0072(9) 0.0013(8) O21 0.0219(10) 0.0209(9) 0.0240(10) 0.0008(8) -0.0045(8) 0.0012(8) O22 0.0229(10) 0.0414(12) 0.0266(11) -0.0074(9) -0.0045(8) 0.0113(9) O23 0.0253(10) 0.0198(9) 0.0287(11) -0.0034(8) -0.0046(8) 0.0068(8) O24 0.0287(11) 0.0157(9) 0.0389(12) -0.0031(8) 0.0068(9) 0.0000(8) O25 0.0235(11) 0.0707(17) 0.0276(12) -0.0075(12) 0.0132(9) -0.0089(11) O26 0.0268(11) 0.0204(10) 0.0318(11) -0.0032(8) -0.0039(9) 0.0034(8) O27 0.0198(9) 0.0178(9) 0.0263(10) -0.0002(8) 0.0057(8) 0.0006(7) C1 0.0195(13) 0.0256(14) 0.0253(14) 0.0039(11) -0.0004(11) 0.0043(11) C2 0.0203(14) 0.0364(17) 0.0306(16) 0.0089(13) 0.0031(12) 0.0089(12) C3 0.0300(16) 0.0309(15) 0.0286(16) 0.0074(12) 0.0076(12) 0.0180(13) C4 0.0279(15) 0.0226(13) 0.0222(14) 0.0042(11) 0.0077(11) 0.0087(11) C5 0.0205(13) 0.0187(12) 0.0150(12) 0.0039(10) 0.0055(10) 0.0059(10) C6 0.0212(13) 0.0175(12) 0.0174(13) 0.0010(10) 0.0061(10) 0.0042(10) C7 0.0297(15) 0.0174(13) 0.0218(14) 0.0018(10) 0.0025(11) 0.0053(11) C8 0.0300(15) 0.0195(13) 0.0204(14) 0.0011(11) 0.0027(11) -0.0008(11) C9 0.0205(13) 0.0191(12) 0.0163(12) 0.0004(10) 0.0040(10) -0.0014(10) C10 0.0205(13) 0.0227(13) 0.0154(12) -0.0001(10) 0.0007(10) -0.0005(10) C11 0.0259(14) 0.0243(14) 0.0186(13) -0.0001(11) 0.0024(11) -0.0046(11) C12 0.0219(14) 0.0331(16) 0.0212(14) -0.0008(12) 0.0030(11) -0.0084(12) C13 0.0178(13) 0.0373(16) 0.0231(14) 0.0018(12) 0.0004(11) -0.0023(12) C14 0.0190(13) 0.0296(15) 0.0247(14) 0.0048(12) 0.0011(11) 0.0010(11) C15 0.0191(13) 0.0193(13) 0.0228(14) -0.0034(10) -0.0003(10) 0.0042(10) C16 0.0211(13) 0.0283(14) 0.0163(13) -0.0046(11) -0.0004(10) 0.0087(11) C17 0.0263(14) 0.0294(14) 0.0146(12) 0.0017(11) 0.0062(11) 0.0109(12) C18 0.0189(13) 0.0244(13) 0.0198(13) 0.0021(11) 0.0037(10) 0.0021(11) C19 0.0131(11) 0.0158(11) 0.0174(12) -0.0001(9) 0.0013(9) 0.0040(9) C20 0.0170(12) 0.0136(11) 0.0193(13) 0.0008(9) 0.0030(10) 0.0036(9) C21 0.0148(12) 0.0155(12) 0.0189(13) 0.0019(10) 0.0022(9) 0.0001(9) C22 0.0142(11) 0.0146(11) 0.0161(12) 0.0030(9) 0.0009(9) -0.0008(9) C23 0.0172(12) 0.0161(12) 0.0199(13) -0.0004(10) 0.0019(10) 0.0023(10) C24 0.0200(13) 0.0183(12) 0.0182(13) -0.0008(10) 0.0040(10) -0.0047(10) C25 0.0208(13) 0.0185(12) 0.0187(13) 0.0041(10) -0.0012(10) -0.0032(10) C26 0.0179(12) 0.0178(12) 0.0212(13) 0.0030(10) -0.0018(10) 0.0019(10) C27 0.0145(12) 0.0185(12) 0.0223(13) -0.0013(10) 0.0051(10) 0.0025(10) C28 0.0145(12) 0.0229(13) 0.0253(14) 0.0020(11) 0.0063(10) 0.0012(10) C29 0.0176(13) 0.0182(12) 0.0272(15) 0.0025(11) 0.0057(11) -0.0016(10) C30 0.0182(12) 0.0161(12) 0.0232(14) 0.0021(10) 0.0051(10) 0.0024(10) C31 0.0152(12) 0.0154(11) 0.0176(12) 0.0022(10) 0.0035(9) 0.0031(9) C32 0.0151(12) 0.0141(11) 0.0156(12) 0.0013(9) 0.0023(9) 0.0020(9) C33 0.0183(12) 0.0142(12) 0.0233(13) 0.0025(10) 0.0041(10) 0.0034(10) C34 0.0185(12) 0.0128(11) 0.0237(13) -0.0001(10) 0.0047(10) 0.0050(10) C35 0.0138(11) 0.0133(11) 0.0167(12) 0.0008(9) 0.0025(9) 0.0028(9) C36 0.0150(12) 0.0140(11) 0.0172(12) 0.0017(9) 0.0053(9) 0.0039(9) C37 0.0178(12) 0.0154(12) 0.0255(14) -0.0004(10) 0.0028(10) 0.0048(10) C38 0.0187(13) 0.0186(12) 0.0240(14) 0.0003(10) 0.0070(10) 0.0074(10) C39 0.0151(12) 0.0211(13) 0.0249(14) 0.0028(11) 0.0074(10) 0.0048(10) C40 0.0170(12) 0.0158(12) 0.0218(13) 0.0015(10) 0.0036(10) 0.0024(10) C41 0.0181(12) 0.0196(12) 0.0185(13) -0.0010(10) 0.0050(10) 0.0000(10) C42 0.0260(14) 0.0301(15) 0.0146(13) -0.0008(11) 0.0054(11) 0.0006(12) C43 0.0245(14) 0.0253(14) 0.0167(13) 0.0065(11) 0.0002(10) 0.0005(11) C44 0.0192(13) 0.0172(12) 0.0186(13) 0.0029(10) 0.0009(10) 0.0027(10) C45 0.0130(11) 0.0117(11) 0.0157(12) -0.0005(9) 0.0018(9) -0.0009(9) C46 0.0121(11) 0.0105(11) 0.0167(12) -0.0024(9) 0.0009(9) -0.0008(9) C47 0.0126(11) 0.0143(11) 0.0154(12) 0.0019(9) 0.0012(9) 0.0047(9) C48 0.0141(11) 0.0142(11) 0.0148(12) 0.0011(9) 0.0025(9) 0.0051(9) C49 0.0178(12) 0.0177(12) 0.0195(13) 0.0001(10) 0.0026(10) 0.0031(10) C50 0.0231(13) 0.0235(13) 0.0171(13) 0.0004(10) 0.0029(10) 0.0079(11) C51 0.0214(13) 0.0266(14) 0.0190(13) 0.0039(11) 0.0074(10) 0.0066(11) C52 0.0159(12) 0.0199(12) 0.0221(13) 0.0023(10) 0.0056(10) 0.0016(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N7 1.935(2) . ? Cu1 N1 1.990(2) . ? Cu1 N8 2.027(2) . ? Cu1 N2 2.048(2) . ? Cu2 N6 1.940(2) . ? Cu2 N4 1.988(2) . ? Cu2 N5 2.018(2) . ? Cu2 O1 2.032(2) . ? Cu2 N3 2.228(2) . ? Cu3 N17 1.923(2) . ? Cu3 N11 1.978(2) . ? Cu3 N18 2.024(2) . ? Cu3 N12 2.064(2) . ? Cu4 N16 1.935(2) . ? Cu4 N14 1.980(2) . ? Cu4 N15 2.022(2) . ? Cu4 O2 2.055(2) . ? Cu4 N13 2.194(2) . ? N1 C1 1.341(3) . ? N1 C5 1.357(3) . ? N2 N3 1.335(3) . ? N2 C6 1.340(3) . ? N3 C9 1.336(3) . ? N4 C14 1.343(3) . ? N4 C10 1.355(3) . ? N5 C15 1.335(3) . ? N5 C19 1.356(3) . ? N6 C20 1.311(3) . ? N6 N7 1.405(3) . ? N7 C21 1.317(3) . ? N8 C26 1.338(3) . ? N8 C22 1.358(3) . ? N9 C20 1.322(3) . ? N9 H1N 0.80(3) . ? N9 H2N 0.88(4) . ? N10 C21 1.322(3) . ? N10 H3N 0.87(4) . ? N10 H4N 0.82(4) . ? N11 C27 1.342(3) . ? N11 C31 1.360(3) . ? N12 N13 1.334(3) . ? N12 C32 1.341(3) . ? N13 C35 1.338(3) . ? N14 C40 1.341(3) . ? N14 C36 1.360(3) . ? N15 C41 1.339(3) . ? N15 C45 1.358(3) . ? N16 C46 1.317(3) . ? N16 N17 1.409(3) . ? N17 C47 1.310(3) . ? N18 C52 1.337(3) . ? N18 C48 1.366(3) . ? N19 C46 1.321(3) . ? N19 H5N 0.81(3) . ? N19 H6N 0.89(4) . ? N20 C47 1.321(3) . ? N20 H7N 0.87(4) . ? N20 H8N 0.87(4) . ? N21 O6 1.230(4) . ? N21 O4 1.242(4) . ? N21 O5 1.254(3) . ? N22 O7 1.244(3) . ? N22 O8 1.245(3) . ? N22 O9 1.255(3) . ? N23 O12 1.239(3) . ? N23 O11 1.243(3) . ? N23 O10 1.256(3) . ? N24 O16 1.251(3) . ? N24 O17 1.257(3) . ? N24 O18 1.258(3) . ? N25 O14 1.205(4) . ? N25 O13 1.260(4) . ? N25 O15 1.271(3) . ? N26 O19 1.237(3) . ? N26 O20 1.253(3) . ? N26 O21 1.283(3) . ? N27 O24 1.253(3) . ? N27 O22 1.256(3) . ? N27 O23 1.260(3) . ? N28 O25 1.244(3) . ? N28 O26 1.255(3) . ? N28 O27 1.266(3) . ? O1 H12W 0.85(4) . ? O1 H11W 0.74(4) . ? O2 H22W 0.73(5) . ? O2 H21W 0.89(4) . ? O3 H32W 0.83(4) . ? O3 H31W 0.79(5) . ? C1 C2 1.392(4) . ? C1 H11 0.9500 . ? C2 C3 1.388(4) . ? C2 H21 0.9500 . ? C3 C4 1.394(4) . ? C3 H31 0.9500 . ? C4 C5 1.391(4) . ? C4 H41 0.9500 . ? C5 C6 1.483(4) . ? C6 C7 1.402(4) . ? C7 C8 1.369(4) . ? C7 H71 0.9500 . ? C8 C9 1.410(4) . ? C8 H81 0.9500 . ? C9 C10 1.489(4) . ? C10 C11 1.391(4) . ? C11 C12 1.395(4) . ? C11 H111 0.9500 . ? C12 C13 1.377(4) . ? C12 H121 0.9500 . ? C13 C14 1.387(4) . ? C13 H131 0.9500 . ? C14 H141 0.9500 . ? C15 C16 1.388(4) . ? C15 H151 0.9500 . ? C16 C17 1.383(4) . ? C16 H161 0.9500 . ? C17 C18 1.396(4) . ? C17 H171 0.9500 . ? C18 C19 1.383(4) . ? C18 H181 0.9500 . ? C19 C20 1.494(4) . ? C21 C22 1.491(3) . ? C22 C23 1.388(4) . ? C23 C24 1.391(4) . ? C23 H231 0.9500 . ? C24 C25 1.387(4) . ? C24 H241 0.9500 . ? C25 C26 1.390(4) . ? C25 H251 0.9500 . ? C26 H261 0.9500 . ? C27 C28 1.385(4) . ? C27 H271 0.9500 . ? C28 C29 1.387(4) . ? C28 H281 0.9500 . ? C29 C30 1.391(4) . ? C29 H291 0.9500 . ? C30 C31 1.384(3) . ? C30 H301 0.9500 . ? C31 C32 1.474(3) . ? C32 C33 1.407(3) . ? C33 C34 1.371(4) . ? C33 H331 0.9500 . ? C34 C35 1.405(3) . ? C34 H341 0.9500 . ? C35 C36 1.488(3) . ? C36 C37 1.391(3) . ? C37 C38 1.392(4) . ? C37 H371 0.9500 . ? C38 C39 1.382(4) . ? C38 H381 0.9500 . ? C39 C40 1.396(3) . ? C39 H391 0.9500 . ? C40 H401 0.9500 . ? C41 C42 1.394(4) . ? C41 H411 0.9500 . ? C42 C43 1.381(4) . ? C42 H421 0.9500 . ? C43 C44 1.393(4) . ? C43 H431 0.9500 . ? C44 C45 1.377(3) . ? C44 H441 0.9500 . ? C45 C46 1.488(3) . ? C47 C48 1.499(3) . ? C48 C49 1.383(4) . ? C49 C50 1.397(4) . ? C49 H491 0.9500 . ? C50 C51 1.386(4) . ? C50 H501 0.9500 . ? C51 C52 1.392(4) . ? C51 H511 0.9500 . ? C52 H521 0.9500 . ? 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 N7 Cu1 N1 168.94(9) . . ? N7 Cu1 N8 81.04(9) . . ? N1 Cu1 N8 105.02(9) . . ? N7 Cu1 N2 100.03(9) . . ? N1 Cu1 N2 80.68(9) . . ? N8 Cu1 N2 143.65(9) . . ? N6 Cu2 N4 170.28(9) . . ? N6 Cu2 N5 80.60(9) . . ? N4 Cu2 N5 99.53(9) . . ? N6 Cu2 O1 96.63(9) . . ? N4 Cu2 O1 87.46(9) . . ? N5 Cu2 O1 154.02(9) . . ? N6 Cu2 N3 92.31(8) . . ? N4 Cu2 N3 78.67(9) . . ? N5 Cu2 N3 113.39(8) . . ? O1 Cu2 N3 92.47(9) . . ? N17 Cu3 N11 165.33(9) . . ? N17 Cu3 N18 81.03(9) . . ? N11 Cu3 N18 105.27(9) . . ? N17 Cu3 N12 100.02(8) . . ? N11 Cu3 N12 80.67(8) . . ? N18 Cu3 N12 152.22(8) . . ? N16 Cu4 N14 171.56(9) . . ? N16 Cu4 N15 80.80(8) . . ? N14 Cu4 N15 98.14(8) . . ? N16 Cu4 O2 92.00(8) . . ? N14 Cu4 O2 92.93(8) . . ? N15 Cu4 O2 150.19(9) . . ? N16 Cu4 N13 93.81(8) . . ? N14 Cu4 N13 79.13(8) . . ? N15 Cu4 N13 116.67(8) . . ? O2 Cu4 N13 92.52(8) . . ? C1 N1 C5 118.9(2) . . ? C1 N1 Cu1 125.80(19) . . ? C5 N1 Cu1 115.20(17) . . ? N3 N2 C6 120.7(2) . . ? N3 N2 Cu1 123.29(16) . . ? C6 N2 Cu1 113.84(17) . . ? N2 N3 C9 120.4(2) . . ? N2 N3 Cu2 128.35(16) . . ? C9 N3 Cu2 110.64(17) . . ? C14 N4 C10 119.4(2) . . ? C14 N4 Cu2 122.37(19) . . ? C10 N4 Cu2 117.43(18) . . ? C15 N5 C19 119.0(2) . . ? C15 N5 Cu2 127.00(18) . . ? C19 N5 Cu2 113.20(17) . . ? C20 N6 N7 119.0(2) . . ? C20 N6 Cu2 118.52(17) . . ? N7 N6 Cu2 120.35(15) . . ? C21 N7 N6 117.2(2) . . ? C21 N7 Cu1 117.50(17) . . ? N6 N7 Cu1 123.06(15) . . ? C26 N8 C22 118.2(2) . . ? C26 N8 Cu1 125.75(18) . . ? C22 N8 Cu1 111.91(16) . . ? C20 N9 H1N 120(2) . . ? C20 N9 H2N 120(2) . . ? H1N N9 H2N 119(3) . . ? C21 N10 H3N 120(2) . . ? C21 N10 H4N 123(3) . . ? H3N N10 H4N 117(3) . . ? C27 N11 C31 118.3(2) . . ? C27 N11 Cu3 127.16(18) . . ? C31 N11 Cu3 114.52(16) . . ? N13 N12 C32 120.8(2) . . ? N13 N12 Cu3 125.52(16) . . ? C32 N12 Cu3 111.88(16) . . ? N12 N13 C35 120.2(2) . . ? N12 N13 Cu4 127.96(15) . . ? C35 N13 Cu4 111.63(16) . . ? C40 N14 C36 119.5(2) . . ? C40 N14 Cu4 123.26(17) . . ? C36 N14 Cu4 117.27(16) . . ? C41 N15 C45 118.2(2) . . ? C41 N15 Cu4 128.35(18) . . ? C45 N15 Cu4 113.36(16) . . ? C46 N16 N17 117.58(19) . . ? C46 N16 Cu4 118.06(17) . . ? N17 N16 Cu4 122.88(15) . . ? C47 N17 N16 118.1(2) . . ? C47 N17 Cu3 118.11(17) . . ? N16 N17 Cu3 123.08(15) . . ? C52 N18 C48 118.3(2) . . ? C52 N18 Cu3 128.15(18) . . ? C48 N18 Cu3 112.33(16) . . ? C46 N19 H5N 122(2) . . ? C46 N19 H6N 119(2) . . ? H5N N19 H6N 119(3) . . ? C47 N20 H7N 122(2) . . ? C47 N20 H8N 122(2) . . ? H7N N20 H8N 116(3) . . ? O6 N21 O4 121.0(3) . . ? O6 N21 O5 122.0(3) . . ? O4 N21 O5 117.0(3) . . ? O7 N22 O8 119.4(2) . . ? O7 N22 O9 119.3(2) . . ? O8 N22 O9 121.2(2) . . ? O12 N23 O11 121.3(2) . . ? O12 N23 O10 121.0(3) . . ? O11 N23 O10 117.7(3) . . ? O16 N24 O17 120.0(2) . . ? O16 N24 O18 120.1(2) . . ? O17 N24 O18 119.8(2) . . ? O14 N25 O13 119.7(3) . . ? O14 N25 O15 122.7(3) . . ? O13 N25 O15 117.5(3) . . ? O19 N26 O20 122.0(2) . . ? O19 N26 O21 118.5(2) . . ? O20 N26 O21 119.5(2) . . ? O24 N27 O22 120.7(2) . . ? O24 N27 O23 120.4(2) . . ? O22 N27 O23 118.9(2) . . ? O25 N28 O26 120.7(2) . . ? O25 N28 O27 119.0(2) . . ? O26 N28 O27 120.2(2) . . ? Cu2 O1 H12W 119(3) . . ? Cu2 O1 H11W 126(3) . . ? H12W O1 H11W 113(4) . . ? Cu4 O2 H22W 117(4) . . ? Cu4 O2 H21W 117(3) . . ? H22W O2 H21W 108(4) . . ? H32W O3 H31W 104(4) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H11 118.7 . . ? C2 C1 H11 118.7 . . ? C3 C2 C1 118.4(3) . . ? C3 C2 H21 120.8 . . ? C1 C2 H21 120.8 . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H31 120.2 . . ? C4 C3 H31 120.2 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H41 120.7 . . ? C3 C4 H41 120.7 . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C6 114.8(2) . . ? C4 C5 C6 123.3(2) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 114.4(2) . . ? C7 C6 C5 124.3(2) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 H71 120.9 . . ? C6 C7 H71 120.9 . . ? C7 C8 C9 118.1(3) . . ? C7 C8 H81 121.0 . . ? C9 C8 H81 121.0 . . ? N3 C9 C8 121.3(2) . . ? N3 C9 C10 115.2(2) . . ? C8 C9 C10 123.5(2) . . ? N4 C10 C11 121.1(3) . . ? N4 C10 C9 116.7(2) . . ? C11 C10 C9 122.1(2) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H111 120.5 . . ? C12 C11 H111 120.5 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H121 120.2 . . ? C11 C12 H121 120.2 . . ? C12 C13 C14 118.7(3) . . ? C12 C13 H131 120.6 . . ? C14 C13 H131 120.6 . . ? N4 C14 C13 122.2(3) . . ? N4 C14 H141 118.9 . . ? C13 C14 H141 118.9 . . ? N5 C15 C16 122.1(3) . . ? N5 C15 H151 119.0 . . ? C16 C15 H151 119.0 . . ? C17 C16 C15 119.0(3) . . ? C17 C16 H161 120.5 . . ? C15 C16 H161 120.5 . . ? C16 C17 C18 119.4(3) . . ? C16 C17 H171 120.3 . . ? C18 C17 H171 120.3 . . ? C19 C18 C17 118.3(3) . . ? C19 C18 H181 120.9 . . ? C17 C18 H181 120.9 . . ? N5 C19 C18 122.2(2) . . ? N5 C19 C20 113.8(2) . . ? C18 C19 C20 123.9(2) . . ? N6 C20 N9 126.1(3) . . ? N6 C20 C19 112.7(2) . . ? N9 C20 C19 121.2(2) . . ? N7 C21 N10 124.9(2) . . ? N7 C21 C22 113.6(2) . . ? N10 C21 C22 121.4(2) . . ? N8 C22 C23 122.4(2) . . ? N8 C22 C21 114.0(2) . . ? C23 C22 C21 123.1(2) . . ? C22 C23 C24 118.9(2) . . ? C22 C23 H231 120.6 . . ? C24 C23 H231 120.6 . . ? C25 C24 C23 118.6(2) . . ? C25 C24 H241 120.7 . . ? C23 C24 H241 120.7 . . ? C24 C25 C26 119.3(2) . . ? C24 C25 H251 120.3 . . ? C26 C25 H251 120.3 . . ? N8 C26 C25 122.5(2) . . ? N8 C26 H261 118.8 . . ? C25 C26 H261 118.8 . . ? N11 C27 C28 122.4(2) . . ? N11 C27 H271 118.8 . . ? C28 C27 H271 118.8 . . ? C27 C28 C29 119.2(2) . . ? C27 C28 H281 120.4 . . ? C29 C28 H281 120.4 . . ? C28 C29 C30 118.9(2) . . ? C28 C29 H291 120.6 . . ? C30 C29 H291 120.6 . . ? C31 C30 C29 118.9(2) . . ? C31 C30 H301 120.6 . . ? C29 C30 H301 120.6 . . ? N11 C31 C30 122.3(2) . . ? N11 C31 C32 115.2(2) . . ? C30 C31 C32 122.4(2) . . ? N12 C32 C33 121.1(2) . . ? N12 C32 C31 114.5(2) . . ? C33 C32 C31 124.3(2) . . ? C34 C33 C32 118.0(2) . . ? C34 C33 H331 121.0 . . ? C32 C33 H331 121.0 . . ? C33 C34 C35 118.1(2) . . ? C33 C34 H341 120.9 . . ? C35 C34 H341 120.9 . . ? N13 C35 C34 121.6(2) . . ? N13 C35 C36 115.3(2) . . ? C34 C35 C36 123.1(2) . . ? N14 C36 C37 121.1(2) . . ? N14 C36 C35 116.4(2) . . ? C37 C36 C35 122.5(2) . . ? C36 C37 C38 118.9(2) . . ? C36 C37 H371 120.6 . . ? C38 C37 H371 120.6 . . ? C39 C38 C37 120.0(2) . . ? C39 C38 H381 120.0 . . ? C37 C38 H381 120.0 . . ? C38 C39 C40 118.3(2) . . ? C38 C39 H391 120.9 . . ? C40 C39 H391 120.9 . . ? N14 C40 C39 122.2(2) . . ? N14 C40 H401 118.9 . . ? C39 C40 H401 118.9 . . ? N15 C41 C42 122.1(2) . . ? N15 C41 H411 118.9 . . ? C42 C41 H411 118.9 . . ? C43 C42 C41 119.3(2) . . ? C43 C42 H421 120.3 . . ? C41 C42 H421 120.3 . . ? C42 C43 C44 118.8(2) . . ? C42 C43 H431 120.6 . . ? C44 C43 H431 120.6 . . ? C45 C44 C43 118.9(2) . . ? C45 C44 H441 120.6 . . ? C43 C44 H441 120.6 . . ? N15 C45 C44 122.6(2) . . ? N15 C45 C46 113.6(2) . . ? C44 C45 C46 123.7(2) . . ? N16 C46 N19 125.7(2) . . ? N16 C46 C45 113.7(2) . . ? N19 C46 C45 120.6(2) . . ? N17 C47 N20 124.9(2) . . ? N17 C47 C48 113.4(2) . . ? N20 C47 C48 121.7(2) . . ? N18 C48 C49 122.4(2) . . ? N18 C48 C47 113.5(2) . . ? C49 C48 C47 124.1(2) . . ? C48 C49 C50 118.6(2) . . ? C48 C49 H491 120.7 . . ? C50 C49 H491 120.7 . . ? C51 C50 C49 119.1(2) . . ? C51 C50 H501 120.5 . . ? C49 C50 H501 120.5 . . ? C50 C51 C52 119.1(2) . . ? C50 C51 H511 120.5 . . ? C52 C51 H511 120.5 . . ? N18 C52 C51 122.5(2) . . ? N18 C52 H521 118.7 . . ? C51 C52 H521 118.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Cu1 N1 C1 79.0(5) . . . . ? N8 Cu1 N1 C1 -43.2(2) . . . . ? N2 Cu1 N1 C1 173.6(2) . . . . ? N7 Cu1 N1 C5 -96.7(5) . . . . ? N8 Cu1 N1 C5 141.14(18) . . . . ? N2 Cu1 N1 C5 -2.09(18) . . . . ? N7 Cu1 N2 N3 -20.2(2) . . . . ? N1 Cu1 N2 N3 171.0(2) . . . . ? N8 Cu1 N2 N3 68.3(3) . . . . ? N7 Cu1 N2 C6 176.64(18) . . . . ? N1 Cu1 N2 C6 7.83(18) . . . . ? N8 Cu1 N2 C6 -94.9(2) . . . . ? C6 N2 N3 C9 0.6(4) . . . . ? Cu1 N2 N3 C9 -161.48(19) . . . . ? C6 N2 N3 Cu2 -169.85(18) . . . . ? Cu1 N2 N3 Cu2 28.1(3) . . . . ? N6 Cu2 N3 N2 2.8(2) . . . . ? N4 Cu2 N3 N2 179.2(2) . . . . ? N5 Cu2 N3 N2 83.6(2) . . . . ? O1 Cu2 N3 N2 -93.9(2) . . . . ? N6 Cu2 N3 C9 -168.31(18) . . . . ? N4 Cu2 N3 C9 8.03(18) . . . . ? N5 Cu2 N3 C9 -87.56(19) . . . . ? O1 Cu2 N3 C9 94.94(18) . . . . ? N6 Cu2 N4 C14 -169.4(5) . . . . ? N5 Cu2 N4 C14 -79.4(2) . . . . ? O1 Cu2 N4 C14 75.4(2) . . . . ? N3 Cu2 N4 C14 168.4(2) . . . . ? N6 Cu2 N4 C10 20.8(7) . . . . ? N5 Cu2 N4 C10 110.7(2) . . . . ? O1 Cu2 N4 C10 -94.4(2) . . . . ? N3 Cu2 N4 C10 -1.42(19) . . . . ? N6 Cu2 N5 C15 -174.6(2) . . . . ? N4 Cu2 N5 C15 15.2(2) . . . . ? O1 Cu2 N5 C15 -88.8(3) . . . . ? N3 Cu2 N5 C15 96.9(2) . . . . ? N6 Cu2 N5 C19 -5.11(17) . . . . ? N4 Cu2 N5 C19 -175.26(17) . . . . ? O1 Cu2 N5 C19 80.7(3) . . . . ? N3 Cu2 N5 C19 -93.56(18) . . . . ? N4 Cu2 N6 C20 89.6(6) . . . . ? N5 Cu2 N6 C20 -1.99(19) . . . . ? O1 Cu2 N6 C20 -155.90(19) . . . . ? N3 Cu2 N6 C20 111.34(19) . . . . ? N4 Cu2 N6 N7 -73.8(6) . . . . ? N5 Cu2 N6 N7 -165.34(18) . . . . ? O1 Cu2 N6 N7 40.75(18) . . . . ? N3 Cu2 N6 N7 -52.01(18) . . . . ? C20 N6 N7 C21 104.7(3) . . . . ? Cu2 N6 N7 C21 -92.0(2) . . . . ? C20 N6 N7 Cu1 -92.8(2) . . . . ? Cu2 N6 N7 Cu1 70.5(2) . . . . ? N1 Cu1 N7 C21 -133.0(4) . . . . ? N8 Cu1 N7 C21 -8.83(19) . . . . ? N2 Cu1 N7 C21 134.31(19) . . . . ? N1 Cu1 N7 N6 64.6(5) . . . . ? N8 Cu1 N7 N6 -171.28(19) . . . . ? N2 Cu1 N7 N6 -28.1(2) . . . . ? N7 Cu1 N8 C26 169.4(2) . . . . ? N1 Cu1 N8 C26 -20.1(2) . . . . ? N2 Cu1 N8 C26 74.6(3) . . . . ? N7 Cu1 N8 C22 12.87(17) . . . . ? N1 Cu1 N8 C22 -176.59(16) . . . . ? N2 Cu1 N8 C22 -81.9(2) . . . . ? N17 Cu3 N11 C27 75.1(4) . . . . ? N18 Cu3 N11 C27 -38.8(2) . . . . ? N12 Cu3 N11 C27 169.0(2) . . . . ? N17 Cu3 N11 C31 -105.6(4) . . . . ? N18 Cu3 N11 C31 140.54(17) . . . . ? N12 Cu3 N11 C31 -11.66(18) . . . . ? N17 Cu3 N12 N13 -13.6(2) . . . . ? N11 Cu3 N12 N13 -178.7(2) . . . . ? N18 Cu3 N12 N13 76.2(3) . . . . ? N17 Cu3 N12 C32 -178.51(17) . . . . ? N11 Cu3 N12 C32 16.35(17) . . . . ? N18 Cu3 N12 C32 -88.7(2) . . . . ? C32 N12 N13 C35 -0.4(3) . . . . ? Cu3 N12 N13 C35 -164.02(18) . . . . ? C32 N12 N13 Cu4 -174.64(18) . . . . ? Cu3 N12 N13 Cu4 21.7(3) . . . . ? N16 Cu4 N13 N12 3.7(2) . . . . ? N14 Cu4 N13 N12 179.0(2) . . . . ? N15 Cu4 N13 N12 85.3(2) . . . . ? O2 Cu4 N13 N12 -88.5(2) . . . . ? N16 Cu4 N13 C35 -170.98(17) . . . . ? N14 Cu4 N13 C35 4.34(17) . . . . ? N15 Cu4 N13 C35 -89.38(18) . . . . ? O2 Cu4 N13 C35 96.84(17) . . . . ? N16 Cu4 N14 C40 -151.2(5) . . . . ? N15 Cu4 N14 C40 -69.1(2) . . . . ? O2 Cu4 N14 C40 83.2(2) . . . . ? N13 Cu4 N14 C40 175.2(2) . . . . ? N16 Cu4 N14 C36 28.7(7) . . . . ? N15 Cu4 N14 C36 110.88(19) . . . . ? O2 Cu4 N14 C36 -96.87(19) . . . . ? N13 Cu4 N14 C36 -4.86(18) . . . . ? N16 Cu4 N15 C41 177.7(2) . . . . ? N14 Cu4 N15 C41 6.2(2) . . . . ? O2 Cu4 N15 C41 -104.5(2) . . . . ? N13 Cu4 N15 C41 88.1(2) . . . . ? N16 Cu4 N15 C45 -5.05(16) . . . . ? N14 Cu4 N15 C45 -176.58(17) . . . . ? O2 Cu4 N15 C45 72.7(2) . . . . ? N13 Cu4 N15 C45 -94.70(17) . . . . ? N14 Cu4 N16 C46 84.6(6) . . . . ? N15 Cu4 N16 C46 1.14(18) . . . . ? O2 Cu4 N16 C46 -149.77(19) . . . . ? N13 Cu4 N16 C46 117.56(18) . . . . ? N14 Cu4 N16 N17 -81.2(6) . . . . ? N15 Cu4 N16 N17 -164.67(19) . . . . ? O2 Cu4 N16 N17 44.42(18) . . . . ? N13 Cu4 N16 N17 -48.24(18) . . . . ? C46 N16 N17 C47 90.6(3) . . . . ? Cu4 N16 N17 C47 -103.5(2) . . . . ? C46 N16 N17 Cu3 -99.1(2) . . . . ? Cu4 N16 N17 Cu3 66.8(2) . . . . ? N11 Cu3 N17 C47 -127.8(3) . . . . ? N18 Cu3 N17 C47 -11.03(18) . . . . ? N12 Cu3 N17 C47 140.82(18) . . . . ? N11 Cu3 N17 N16 61.9(4) . . . . ? N18 Cu3 N17 N16 178.62(18) . . . . ? N12 Cu3 N17 N16 -29.54(18) . . . . ? N17 Cu3 N18 C52 178.1(2) . . . . ? N11 Cu3 N18 C52 -15.5(2) . . . . ? N12 Cu3 N18 C52 83.6(3) . . . . ? N17 Cu3 N18 C48 10.97(16) . . . . ? N11 Cu3 N18 C48 177.41(16) . . . . ? N12 Cu3 N18 C48 -83.5(2) . . . . ? C5 N1 C1 C2 -1.5(4) . . . . ? Cu1 N1 C1 C2 -177.1(2) . . . . ? N1 C1 C2 C3 1.9(4) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C1 N1 C5 C4 0.1(4) . . . . ? Cu1 N1 C5 C4 176.1(2) . . . . ? C1 N1 C5 C6 -179.4(2) . . . . ? Cu1 N1 C5 C6 -3.4(3) . . . . ? C3 C4 C5 N1 0.9(4) . . . . ? C3 C4 C5 C6 -179.6(3) . . . . ? N3 N2 C6 C7 2.0(4) . . . . ? Cu1 N2 C6 C7 165.6(2) . . . . ? N3 N2 C6 C5 -175.3(2) . . . . ? Cu1 N2 C6 C5 -11.7(3) . . . . ? N1 C5 C6 N2 10.2(3) . . . . ? C4 C5 C6 N2 -169.4(2) . . . . ? N1 C5 C6 C7 -167.1(2) . . . . ? C4 C5 C6 C7 13.4(4) . . . . ? N2 C6 C7 C8 -2.5(4) . . . . ? C5 C6 C7 C8 174.5(3) . . . . ? C6 C7 C8 C9 0.6(4) . . . . ? N2 N3 C9 C8 -2.5(4) . . . . ? Cu2 N3 C9 C8 169.5(2) . . . . ? N2 N3 C9 C10 175.4(2) . . . . ? Cu2 N3 C9 C10 -12.7(3) . . . . ? C7 C8 C9 N3 1.9(4) . . . . ? C7 C8 C9 C10 -175.8(3) . . . . ? C14 N4 C10 C11 1.2(4) . . . . ? Cu2 N4 C10 C11 171.3(2) . . . . ? C14 N4 C10 C9 -175.1(2) . . . . ? Cu2 N4 C10 C9 -5.0(3) . . . . ? N3 C9 C10 N4 12.4(4) . . . . ? C8 C9 C10 N4 -169.8(3) . . . . ? N3 C9 C10 C11 -163.8(3) . . . . ? C8 C9 C10 C11 14.0(4) . . . . ? N4 C10 C11 C12 -0.5(4) . . . . ? C9 C10 C11 C12 175.6(3) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? C10 N4 C14 C13 -1.4(4) . . . . ? Cu2 N4 C14 C13 -171.0(2) . . . . ? C12 C13 C14 N4 0.9(4) . . . . ? C19 N5 C15 C16 -1.9(4) . . . . ? Cu2 N5 C15 C16 167.03(19) . . . . ? N5 C15 C16 C17 0.0(4) . . . . ? C15 C16 C17 C18 1.9(4) . . . . ? C16 C17 C18 C19 -1.9(4) . . . . ? C15 N5 C19 C18 2.0(4) . . . . ? Cu2 N5 C19 C18 -168.5(2) . . . . ? C15 N5 C19 C20 -179.1(2) . . . . ? Cu2 N5 C19 C20 10.5(3) . . . . ? C17 C18 C19 N5 0.0(4) . . . . ? C17 C18 C19 C20 -178.9(2) . . . . ? N7 N6 C20 N9 -8.3(4) . . . . ? Cu2 N6 C20 N9 -171.9(2) . . . . ? N7 N6 C20 C19 171.6(2) . . . . ? Cu2 N6 C20 C19 8.0(3) . . . . ? N5 C19 C20 N6 -12.1(3) . . . . ? C18 C19 C20 N6 166.8(2) . . . . ? N5 C19 C20 N9 167.8(2) . . . . ? C18 C19 C20 N9 -13.3(4) . . . . ? N6 N7 C21 N10 -9.8(4) . . . . ? Cu1 N7 C21 N10 -173.3(2) . . . . ? N6 N7 C21 C22 166.7(2) . . . . ? Cu1 N7 C21 C22 3.3(3) . . . . ? C26 N8 C22 C23 -1.4(4) . . . . ? Cu1 N8 C22 C23 157.0(2) . . . . ? C26 N8 C22 C21 -173.1(2) . . . . ? Cu1 N8 C22 C21 -14.7(3) . . . . ? N7 C21 C22 N8 8.0(3) . . . . ? N10 C21 C22 N8 -175.2(2) . . . . ? N7 C21 C22 C23 -163.6(2) . . . . ? N10 C21 C22 C23 13.2(4) . . . . ? N8 C22 C23 C24 -1.0(4) . . . . ? C21 C22 C23 C24 169.9(2) . . . . ? C22 C23 C24 C25 3.0(4) . . . . ? C23 C24 C25 C26 -2.6(4) . . . . ? C22 N8 C26 C25 1.9(4) . . . . ? Cu1 N8 C26 C25 -153.3(2) . . . . ? C24 C25 C26 N8 0.2(4) . . . . ? C31 N11 C27 C28 -1.1(4) . . . . ? Cu3 N11 C27 C28 178.3(2) . . . . ? N11 C27 C28 C29 -0.5(4) . . . . ? C27 C28 C29 C30 0.9(4) . . . . ? C28 C29 C30 C31 0.1(4) . . . . ? C27 N11 C31 C30 2.1(4) . . . . ? Cu3 N11 C31 C30 -177.3(2) . . . . ? C27 N11 C31 C32 -175.0(2) . . . . ? Cu3 N11 C31 C32 5.6(3) . . . . ? C29 C30 C31 N11 -1.6(4) . . . . ? C29 C30 C31 C32 175.3(2) . . . . ? N13 N12 C32 C33 -2.4(4) . . . . ? Cu3 N12 C32 C33 163.35(19) . . . . ? N13 N12 C32 C31 176.4(2) . . . . ? Cu3 N12 C32 C31 -17.8(3) . . . . ? N11 C31 C32 N12 8.7(3) . . . . ? C30 C31 C32 N12 -168.4(2) . . . . ? N11 C31 C32 C33 -172.5(2) . . . . ? C30 C31 C32 C33 10.3(4) . . . . ? N12 C32 C33 C34 2.5(4) . . . . ? C31 C32 C33 C34 -176.2(2) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? N12 N13 C35 C34 2.9(4) . . . . ? Cu4 N13 C35 C34 178.1(2) . . . . ? N12 N13 C35 C36 -178.3(2) . . . . ? Cu4 N13 C35 C36 -3.2(3) . . . . ? C33 C34 C35 N13 -2.7(4) . . . . ? C33 C34 C35 C36 178.6(2) . . . . ? C40 N14 C36 C37 2.2(4) . . . . ? Cu4 N14 C36 C37 -177.73(19) . . . . ? C40 N14 C36 C35 -175.3(2) . . . . ? Cu4 N14 C36 C35 4.7(3) . . . . ? N13 C35 C36 N14 -0.7(3) . . . . ? C34 C35 C36 N14 178.1(2) . . . . ? N13 C35 C36 C37 -178.2(2) . . . . ? C34 C35 C36 C37 0.6(4) . . . . ? N14 C36 C37 C38 -1.5(4) . . . . ? C35 C36 C37 C38 175.9(2) . . . . ? C36 C37 C38 C39 -0.6(4) . . . . ? C37 C38 C39 C40 1.9(4) . . . . ? C36 N14 C40 C39 -0.8(4) . . . . ? Cu4 N14 C40 C39 179.1(2) . . . . ? C38 C39 C40 N14 -1.2(4) . . . . ? C45 N15 C41 C42 -0.9(4) . . . . ? Cu4 N15 C41 C42 176.2(2) . . . . ? N15 C41 C42 C43 -1.2(4) . . . . ? C41 C42 C43 C44 2.5(4) . . . . ? C42 C43 C44 C45 -1.6(4) . . . . ? C41 N15 C45 C44 1.7(4) . . . . ? Cu4 N15 C45 C44 -175.77(19) . . . . ? C41 N15 C45 C46 -174.8(2) . . . . ? Cu4 N15 C45 C46 7.7(2) . . . . ? C43 C44 C45 N15 -0.5(4) . . . . ? C43 C44 C45 C46 175.7(2) . . . . ? N17 N16 C46 N19 -9.2(4) . . . . ? Cu4 N16 C46 N19 -175.7(2) . . . . ? N17 N16 C46 C45 169.23(19) . . . . ? Cu4 N16 C46 C45 2.7(3) . . . . ? N15 C45 C46 N16 -6.9(3) . . . . ? C44 C45 C46 N16 176.6(2) . . . . ? N15 C45 C46 N19 171.6(2) . . . . ? C44 C45 C46 N19 -4.9(4) . . . . ? N16 N17 C47 N20 0.1(4) . . . . ? Cu3 N17 C47 N20 -170.76(19) . . . . ? N16 N17 C47 C48 179.52(19) . . . . ? Cu3 N17 C47 C48 8.7(3) . . . . ? C52 N18 C48 C49 -0.6(4) . . . . ? Cu3 N18 C48 C49 167.95(19) . . . . ? C52 N18 C48 C47 -178.0(2) . . . . ? Cu3 N18 C48 C47 -9.5(2) . . . . ? N17 C47 C48 N18 1.1(3) . . . . ? N20 C47 C48 N18 -179.4(2) . . . . ? N17 C47 C48 C49 -176.3(2) . . . . ? N20 C47 C48 C49 3.2(4) . . . . ? N18 C48 C49 C50 -0.4(4) . . . . ? C47 C48 C49 C50 176.8(2) . . . . ? C48 C49 C50 C51 1.7(4) . . . . ? C49 C50 C51 C52 -2.0(4) . . . . ? C48 N18 C52 C51 0.2(4) . . . . ? Cu3 N18 C52 C51 -166.2(2) . . . . ? C50 C51 C52 N18 1.1(4) . . . . ? #===END data_x549 #(5) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 Cu2 N8 O13' _chemical_formula_weight 743.64 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 'P 2(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 17.226(3) _cell_length_b 12.260(2) _cell_length_c 14.795(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.208(3) _cell_angle_gamma 90.00 _cell_volume 3075.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 13.73 _cell_measurement_theta_max 24.94 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Bruker SMART-CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31674 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7039 _reflns_number_gt 6042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Bruker, 1998)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+2.4486P] 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 7039 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.355 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.064 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 0.357994(12) 0.948524(17) 0.196854(13) 0.01415(6) Uani 1 1 d . . . Cu2 Cu 0.181953(12) 1.042779(17) 0.360720(14) 0.01556(6) Uani 1 1 d . . . N1 N 0.46247(8) 0.93420(11) 0.28069(10) 0.0143(3) Uani 1 1 d . . . N2 N 0.36232(10) 0.87587(13) 0.46985(10) 0.0171(3) Uani 1 1 d . . . H21N H 0.3976(14) 0.865(2) 0.5107(17) 0.028(6) Uiso 1 1 d . . . H22N H 0.3161(14) 0.8684(19) 0.4787(15) 0.025(6) Uiso 1 1 d . . . N3 N 0.32268(8) 0.91778(12) 0.31433(9) 0.0135(3) Uani 1 1 d . . . N4 N 0.24415(8) 0.91538(12) 0.32878(9) 0.0134(3) Uani 1 1 d . . . N5 N 0.23282(10) 0.74470(13) 0.25642(11) 0.0189(3) Uani 1 1 d . . . H51N H 0.2036(15) 0.702(2) 0.2247(17) 0.034(7) Uiso 1 1 d . . . H52N H 0.2789(15) 0.7469(19) 0.2446(16) 0.028(6) Uiso 1 1 d . . . N6 N 0.09663(9) 0.92819(13) 0.33692(10) 0.0185(3) Uani 1 1 d . . . N7 N 0.19262(9) 0.93975(13) 0.57690(11) 0.0213(3) Uani 1 1 d . . . N8 N 0.45033(9) 0.69594(12) 0.19327(10) 0.0172(3) Uani 1 1 d . . . O1 O 0.40568(7) 0.94638(11) 0.08942(8) 0.0202(3) Uani 1 1 d . . . O2 O 0.25177(7) 0.94327(10) 0.12794(8) 0.0185(3) Uani 1 1 d . . . O3 O 0.35232(9) 1.13921(11) 0.22070(10) 0.0213(3) Uani 1 1 d . . . H31W H 0.3961(16) 1.154(2) 0.2273(17) 0.034(7) Uiso 1 1 d . . . H32W H 0.3390(16) 1.144(2) 0.271(2) 0.043(8) Uiso 1 1 d . . . O4 O 0.27013(7) 1.14443(10) 0.37762(8) 0.0184(3) Uani 1 1 d . . . O5 O 0.10835(7) 1.14606(11) 0.39440(9) 0.0217(3) Uani 1 1 d . . . O6 O 0.15222(8) 1.09022(13) 0.19806(10) 0.0235(3) Uani 1 1 d . . . H61W H 0.1689(17) 1.147(3) 0.186(2) 0.048(9) Uiso 1 1 d . . . H62W H 0.1771(16) 1.047(2) 0.1759(18) 0.037(7) Uiso 1 1 d . . . O7 O 0.22473(10) 1.21066(14) 0.67336(12) 0.0337(4) Uani 1 1 d . . . H71W H 0.2648(17) 1.239(2) 0.6719(18) 0.039(8) Uiso 1 1 d . . . H72W H 0.2177(17) 1.167(3) 0.630(2) 0.050(8) Uiso 1 1 d . . . O8 O 0.15976(10) 0.93787(13) 0.64604(11) 0.0386(4) Uani 1 1 d . . . O9 O 0.21023(9) 1.02986(11) 0.54502(10) 0.0282(3) Uani 1 1 d . . . O10 O 0.20816(9) 0.85352(12) 0.53972(10) 0.0319(3) Uani 1 1 d . . . O11 O 0.37797(8) 0.71416(12) 0.17909(10) 0.0275(3) Uani 1 1 d . . . O12 O 0.48949(8) 0.69422(11) 0.27288(8) 0.0222(3) Uani 1 1 d . . . O13 O 0.48474(8) 0.67860(12) 0.12645(9) 0.0260(3) Uani 1 1 d . . . C1 C 0.53286(10) 0.94441(14) 0.25581(12) 0.0173(3) Uani 1 1 d . . . H11 H 0.5351 0.9596 0.1947 0.015(5) Uiso 1 1 calc R . . C2 C 0.60294(10) 0.93314(15) 0.31789(13) 0.0191(4) Uani 1 1 d . . . H21 H 0.6513 0.9423 0.2991 0.026(6) Uiso 1 1 calc R . . C3 C 0.59958(10) 0.90812(15) 0.40820(12) 0.0187(3) Uani 1 1 d . . . H31 H 0.6457 0.8997 0.4510 0.026(6) Uiso 1 1 calc R . . C4 C 0.52619(10) 0.89562(14) 0.43429(12) 0.0168(3) Uani 1 1 d . . . H41 H 0.5225 0.8781 0.4945 0.016(5) Uiso 1 1 calc R . . C5 C 0.45909(10) 0.90976(13) 0.36900(11) 0.0133(3) Uani 1 1 d . . . C6 C 0.37679(10) 0.90040(13) 0.38710(11) 0.0128(3) Uani 1 1 d . . . C7 C 0.20381(10) 0.83014(14) 0.29422(11) 0.0141(3) Uani 1 1 d . . . C8 C 0.11899(10) 0.83347(14) 0.30289(11) 0.0161(3) Uani 1 1 d . . . C9 C 0.06723(11) 0.74784(16) 0.27939(13) 0.0227(4) Uani 1 1 d . . . H91 H 0.0840 0.6834 0.2557 0.027(6) Uiso 1 1 calc R . . C10 C -0.01058(12) 0.76009(19) 0.29191(15) 0.0303(5) Uani 1 1 d . . . H101 H -0.0465 0.7034 0.2777 0.038(7) Uiso 1 1 calc R . . C11 C -0.03355(12) 0.85764(19) 0.32566(16) 0.0324(5) Uani 1 1 d . . . H111 H -0.0854 0.8679 0.3335 0.046(7) Uiso 1 1 calc R . . C12 C 0.02164(11) 0.94013(17) 0.34777(15) 0.0268(4) Uani 1 1 d . . . H121 H 0.0061 1.0056 0.3708 0.031(6) Uiso 1 1 calc R . . C13 C 0.42311(13) 0.89210(18) -0.05753(13) 0.0289(4) Uani 1 1 d . . . H131 H 0.4557 0.9548 -0.0617 0.036(7) Uiso 1 1 calc R . . H132 H 0.3915 0.8777 -0.1165 0.037(7) Uiso 1 1 calc R . . H133 H 0.4559 0.8300 -0.0383 0.056(9) Uiso 1 1 calc R . . C14 C 0.37036(12) 0.91361(15) 0.01116(12) 0.0201(4) Uani 1 1 d . . . C15 C 0.28903(12) 0.89717(15) -0.01397(12) 0.0223(4) Uani 1 1 d . . . H151 H 0.2702 0.8733 -0.0735 0.024(6) Uiso 1 1 calc R . . C16 C 0.23420(11) 0.91392(14) 0.04337(12) 0.0188(3) Uani 1 1 d . . . C17 C 0.14791(12) 0.89595(18) 0.00804(14) 0.0281(4) Uani 1 1 d . . . H171 H 0.1177 0.9488 0.0348 0.055(8) Uiso 1 1 calc R . . H172 H 0.1334 0.8239 0.0243 0.067(10) Uiso 1 1 calc R . . H173 H 0.1375 0.9037 -0.0576 0.070(10) Uiso 1 1 calc R . . C18 C 0.34051(13) 1.30898(17) 0.41764(17) 0.0320(5) Uani 1 1 d . . . H181 H 0.3824 1.2649 0.4025 0.067(10) Uiso 1 1 calc R . . H182 H 0.3550 1.3354 0.4794 0.091(12) Uiso 1 1 calc R . . H183 H 0.3313 1.3697 0.3761 0.096(13) Uiso 1 1 calc R . . C19 C 0.26648(11) 1.24145(15) 0.40968(13) 0.0213(4) Uani 1 1 d . . . C20 C 0.20044(12) 1.28806(16) 0.43692(15) 0.0279(4) Uani 1 1 d . . . H201 H 0.2065 1.3571 0.4633 0.036(6) Uiso 1 1 calc R . . C21 C 0.12616(11) 1.24007(16) 0.42795(13) 0.0229(4) Uani 1 1 d . . . C22 C 0.05968(13) 1.30230(19) 0.45830(17) 0.0354(5) Uani 1 1 d . . . H221 H 0.0175 1.2530 0.4640 0.064(9) Uiso 1 1 calc R . . H222 H 0.0408 1.3573 0.4136 0.068(10) Uiso 1 1 calc R . . H223 H 0.0785 1.3362 0.5166 0.056(8) 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 0.01221(10) 0.01842(11) 0.01208(10) 0.00080(8) 0.00288(7) 0.00107(8) Cu2 0.01213(10) 0.01377(10) 0.02148(11) -0.00196(8) 0.00490(8) 0.00046(8) N1 0.0145(7) 0.0132(7) 0.0157(7) -0.0004(5) 0.0045(5) 0.0006(5) N2 0.0132(7) 0.0246(8) 0.0138(7) 0.0013(6) 0.0031(6) -0.0002(6) N3 0.0104(6) 0.0158(7) 0.0148(6) -0.0003(5) 0.0036(5) 0.0000(5) N4 0.0097(6) 0.0164(7) 0.0147(6) -0.0005(5) 0.0035(5) -0.0002(5) N5 0.0169(8) 0.0172(8) 0.0235(8) -0.0053(6) 0.0064(6) -0.0022(6) N6 0.0141(7) 0.0191(7) 0.0230(7) -0.0005(6) 0.0054(6) -0.0008(6) N7 0.0195(8) 0.0216(8) 0.0232(8) 0.0041(6) 0.0054(6) 0.0029(6) N8 0.0188(7) 0.0147(7) 0.0194(7) -0.0022(6) 0.0068(6) -0.0010(6) O1 0.0207(6) 0.0249(7) 0.0159(6) -0.0006(5) 0.0060(5) -0.0019(5) O2 0.0161(6) 0.0232(7) 0.0156(6) -0.0011(5) 0.0015(5) 0.0014(5) O3 0.0183(7) 0.0203(7) 0.0255(7) 0.0010(5) 0.0042(6) 0.0001(5) O4 0.0164(6) 0.0159(6) 0.0235(6) -0.0015(5) 0.0053(5) -0.0010(5) O5 0.0178(6) 0.0200(6) 0.0277(7) -0.0039(5) 0.0054(5) 0.0031(5) O6 0.0230(7) 0.0221(7) 0.0268(7) 0.0017(6) 0.0082(6) 0.0058(6) O7 0.0242(8) 0.0315(8) 0.0475(10) -0.0143(7) 0.0121(7) -0.0070(7) O8 0.0523(10) 0.0338(9) 0.0378(9) 0.0143(7) 0.0298(8) 0.0174(7) O9 0.0354(8) 0.0206(7) 0.0293(7) 0.0051(6) 0.0078(6) -0.0042(6) O10 0.0396(9) 0.0212(7) 0.0386(8) -0.0026(6) 0.0168(7) 0.0001(6) O11 0.0146(6) 0.0350(8) 0.0341(8) -0.0043(6) 0.0071(6) 0.0037(6) O12 0.0295(7) 0.0220(7) 0.0147(6) -0.0016(5) 0.0033(5) 0.0019(5) O13 0.0213(7) 0.0409(8) 0.0176(6) -0.0053(6) 0.0081(5) 0.0010(6) C1 0.0166(8) 0.0182(9) 0.0184(8) 0.0020(7) 0.0064(7) 0.0002(7) C2 0.0131(8) 0.0199(9) 0.0256(9) 0.0013(7) 0.0075(7) -0.0001(7) C3 0.0122(8) 0.0209(9) 0.0219(9) -0.0002(7) 0.0000(7) 0.0012(7) C4 0.0166(8) 0.0191(8) 0.0149(8) 0.0005(6) 0.0033(6) -0.0003(7) C5 0.0130(8) 0.0113(7) 0.0163(8) -0.0014(6) 0.0041(6) -0.0008(6) C6 0.0134(8) 0.0104(7) 0.0150(7) -0.0017(6) 0.0032(6) -0.0003(6) C7 0.0138(8) 0.0155(8) 0.0132(7) 0.0024(6) 0.0030(6) 0.0005(6) C8 0.0132(8) 0.0185(8) 0.0167(8) 0.0011(6) 0.0030(6) -0.0006(7) C9 0.0205(9) 0.0235(9) 0.0251(9) -0.0048(8) 0.0067(7) -0.0064(7) C10 0.0191(9) 0.0368(12) 0.0357(11) -0.0069(9) 0.0071(8) -0.0139(9) C11 0.0155(9) 0.0391(12) 0.0449(12) -0.0053(10) 0.0119(9) -0.0056(8) C12 0.0175(9) 0.0280(10) 0.0374(11) -0.0029(8) 0.0116(8) 0.0006(8) C13 0.0381(12) 0.0308(11) 0.0219(9) -0.0062(8) 0.0160(9) -0.0097(9) C14 0.0306(10) 0.0150(8) 0.0163(8) 0.0025(7) 0.0084(7) -0.0010(7) C15 0.0292(10) 0.0222(9) 0.0153(8) -0.0021(7) 0.0029(7) -0.0008(8) C16 0.0223(9) 0.0135(8) 0.0188(8) 0.0010(6) -0.0018(7) 0.0006(7) C17 0.0225(10) 0.0305(11) 0.0286(10) -0.0047(8) -0.0032(8) 0.0014(8) C18 0.0283(11) 0.0207(10) 0.0486(13) -0.0076(9) 0.0111(10) -0.0063(8) C19 0.0247(9) 0.0173(9) 0.0219(9) -0.0006(7) 0.0044(7) -0.0011(7) C20 0.0293(10) 0.0184(9) 0.0373(11) -0.0099(8) 0.0098(9) -0.0001(8) C21 0.0241(9) 0.0219(9) 0.0232(9) -0.0026(7) 0.0052(7) 0.0055(8) C22 0.0297(11) 0.0336(12) 0.0448(13) -0.0141(10) 0.0114(10) 0.0056(9) _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 O1 1.9144(12) . ? Cu1 O2 1.9315(13) . ? Cu1 N3 1.9769(14) . ? Cu1 N1 2.0043(15) . ? Cu1 O3 2.3688(14) . ? Cu2 O5 1.9191(13) . ? Cu2 O4 1.9463(13) . ? Cu2 N4 1.9975(14) . ? Cu2 N6 2.0185(15) . ? N1 C1 1.334(2) . ? N1 C5 1.352(2) . ? N2 C6 1.327(2) . ? N2 H21N 0.79(3) . ? N2 H22N 0.83(2) . ? N3 C6 1.311(2) . ? N3 N4 1.4068(19) . ? N4 C7 1.308(2) . ? N5 C7 1.326(2) . ? N5 H51N 0.81(3) . ? N5 H52N 0.84(2) . ? N6 C12 1.338(2) . ? N6 C8 1.349(2) . ? N7 O10 1.243(2) . ? N7 O8 1.254(2) . ? N7 O9 1.259(2) . ? N8 O11 1.247(2) . ? N8 O12 1.2494(19) . ? N8 O13 1.2576(19) . ? O1 C14 1.274(2) . ? O2 C16 1.285(2) . ? O3 H31W 0.76(3) . ? O3 H32W 0.82(3) . ? O4 C19 1.286(2) . ? O5 C21 1.271(2) . ? O6 H61W 0.78(3) . ? O6 H62W 0.78(3) . ? O7 H71W 0.78(3) . ? O7 H72W 0.84(3) . ? C1 C2 1.388(3) . ? C1 H11 0.9300 . ? C2 C3 1.382(3) . ? C2 H21 0.9300 . ? C3 C4 1.394(2) . ? C3 H31 0.9300 . ? C4 C5 1.380(2) . ? C4 H41 0.9300 . ? C5 C6 1.493(2) . ? C7 C8 1.490(2) . ? C8 C9 1.381(2) . ? C9 C10 1.393(3) . ? C9 H91 0.9300 . ? C10 C11 1.381(3) . ? C10 H101 0.9300 . ? C11 C12 1.387(3) . ? C11 H111 0.9300 . ? C12 H121 0.9300 . ? C13 C14 1.502(3) . ? C13 H131 0.9600 . ? C13 H132 0.9600 . ? C13 H133 0.9600 . ? C14 C15 1.399(3) . ? C15 C16 1.392(3) . ? C15 H151 0.9300 . ? C16 C17 1.502(3) . ? C17 H171 0.9600 . ? C17 H172 0.9600 . ? C17 H173 0.9600 . ? C18 C19 1.508(3) . ? C18 H181 0.9600 . ? C18 H182 0.9600 . ? C18 H183 0.9600 . ? C19 C20 1.395(3) . ? C20 C21 1.393(3) . ? C20 H201 0.9300 . ? C21 C22 1.509(3) . ? C22 H221 0.9600 . ? C22 H222 0.9600 . ? C22 H223 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O2 93.84(5) . . ? O1 Cu1 N3 166.31(6) . . ? O2 Cu1 N3 92.72(6) . . ? O1 Cu1 N1 92.42(6) . . ? O2 Cu1 N1 170.58(5) . . ? N3 Cu1 N1 79.73(6) . . ? O1 Cu1 O3 99.92(5) . . ? O2 Cu1 O3 92.94(5) . . ? N3 Cu1 O3 91.72(6) . . ? N1 Cu1 O3 92.89(5) . . ? O5 Cu2 O4 94.63(6) . . ? O5 Cu2 N4 169.75(6) . . ? O4 Cu2 N4 95.28(5) . . ? O5 Cu2 N6 90.59(6) . . ? O4 Cu2 N6 174.62(6) . . ? N4 Cu2 N6 79.57(6) . . ? C1 N1 C5 118.98(15) . . ? C1 N1 Cu1 125.55(12) . . ? C5 N1 Cu1 115.45(11) . . ? C6 N2 H21N 120.0(17) . . ? C6 N2 H22N 120.7(15) . . ? H21N N2 H22N 119(2) . . ? C6 N3 N4 115.77(13) . . ? C6 N3 Cu1 117.93(11) . . ? N4 N3 Cu1 126.27(10) . . ? C7 N4 N3 114.58(13) . . ? C7 N4 Cu2 116.57(11) . . ? N3 N4 Cu2 126.16(11) . . ? C7 N5 H51N 120.5(18) . . ? C7 N5 H52N 120.1(16) . . ? H51N N5 H52N 114(2) . . ? C12 N6 C8 119.00(16) . . ? C12 N6 Cu2 126.28(13) . . ? C8 N6 Cu2 114.65(11) . . ? O10 N7 O8 120.62(16) . . ? O10 N7 O9 119.69(15) . . ? O8 N7 O9 119.68(16) . . ? O11 N8 O12 121.22(14) . . ? O11 N8 O13 119.63(15) . . ? O12 N8 O13 119.16(15) . . ? C14 O1 Cu1 123.57(12) . . ? C16 O2 Cu1 124.11(12) . . ? Cu1 O3 H31W 101(2) . . ? Cu1 O3 H32W 103(2) . . ? H31W O3 H32W 107(3) . . ? C19 O4 Cu2 123.47(12) . . ? C21 O5 Cu2 125.09(12) . . ? H61W O6 H62W 104(3) . . ? H71W O7 H72W 106(3) . . ? N1 C1 C2 122.31(16) . . ? N1 C1 H11 118.8 . . ? C2 C1 H11 118.8 . . ? C3 C2 C1 118.76(16) . . ? C3 C2 H21 120.6 . . ? C1 C2 H21 120.6 . . ? C2 C3 C4 119.18(16) . . ? C2 C3 H31 120.4 . . ? C4 C3 H31 120.4 . . ? C5 C4 C3 118.73(16) . . ? C5 C4 H41 120.6 . . ? C3 C4 H41 120.6 . . ? N1 C5 C4 122.03(15) . . ? N1 C5 C6 113.29(14) . . ? C4 C5 C6 124.69(15) . . ? N3 C6 N2 124.92(16) . . ? N3 C6 C5 113.57(14) . . ? N2 C6 C5 121.51(15) . . ? N4 C7 N5 125.61(16) . . ? N4 C7 C8 113.93(15) . . ? N5 C7 C8 120.43(16) . . ? N6 C8 C9 122.27(16) . . ? N6 C8 C7 113.90(15) . . ? C9 C8 C7 123.83(16) . . ? C8 C9 C10 118.55(18) . . ? C8 C9 H91 120.7 . . ? C10 C9 H91 120.7 . . ? C11 C10 C9 119.05(18) . . ? C11 C10 H101 120.5 . . ? C9 C10 H101 120.5 . . ? C10 C11 C12 119.25(18) . . ? C10 C11 H111 120.4 . . ? C12 C11 H111 120.4 . . ? N6 C12 C11 121.88(19) . . ? N6 C12 H121 119.1 . . ? C11 C12 H121 119.1 . . ? C14 C13 H131 109.5 . . ? C14 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? C14 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? O1 C14 C15 125.56(16) . . ? O1 C14 C13 114.95(17) . . ? C15 C14 C13 119.50(17) . . ? C16 C15 C14 124.92(17) . . ? C16 C15 H151 117.5 . . ? C14 C15 H151 117.5 . . ? O2 C16 C15 124.50(17) . . ? O2 C16 C17 115.31(16) . . ? C15 C16 C17 120.18(16) . . ? C16 C17 H171 109.5 . . ? C16 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C16 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? C19 C18 H181 109.5 . . ? C19 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? C19 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? O4 C19 C20 125.53(17) . . ? O4 C19 C18 116.15(16) . . ? C20 C19 C18 118.32(17) . . ? C21 C20 C19 125.58(18) . . ? C21 C20 H201 117.2 . . ? C19 C20 H201 117.2 . . ? O5 C21 C20 125.06(17) . . ? O5 C21 C22 115.55(17) . . ? C20 C21 C22 119.39(18) . . ? C21 C22 H221 109.5 . . ? C21 C22 H222 109.5 . . ? H221 C22 H222 109.5 . . ? C21 C22 H223 109.5 . . ? H221 C22 H223 109.5 . . ? H222 C22 H223 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 N1 C1 11.29(14) . . . . ? O2 Cu1 N1 C1 143.0(3) . . . . ? N3 Cu1 N1 C1 180.00(15) . . . . ? O3 Cu1 N1 C1 -88.78(14) . . . . ? O1 Cu1 N1 C5 -167.19(12) . . . . ? O2 Cu1 N1 C5 -35.5(4) . . . . ? N3 Cu1 N1 C5 1.52(12) . . . . ? O3 Cu1 N1 C5 92.74(12) . . . . ? O1 Cu1 N3 C6 54.1(3) . . . . ? O2 Cu1 N3 C6 172.67(13) . . . . ? N1 Cu1 N3 C6 -1.67(12) . . . . ? O3 Cu1 N3 C6 -94.30(13) . . . . ? O1 Cu1 N3 N4 -127.7(2) . . . . ? O2 Cu1 N3 N4 -9.14(13) . . . . ? N1 Cu1 N3 N4 176.52(14) . . . . ? O3 Cu1 N3 N4 83.89(13) . . . . ? C6 N3 N4 C7 -108.63(17) . . . . ? Cu1 N3 N4 C7 73.15(17) . . . . ? C6 N3 N4 Cu2 90.75(16) . . . . ? Cu1 N3 N4 Cu2 -87.47(14) . . . . ? O5 Cu2 N4 C7 27.6(4) . . . . ? O4 Cu2 N4 C7 -167.40(12) . . . . ? N6 Cu2 N4 C7 11.04(12) . . . . ? O5 Cu2 N4 N3 -172.1(3) . . . . ? O4 Cu2 N4 N3 -7.12(13) . . . . ? N6 Cu2 N4 N3 171.32(13) . . . . ? O5 Cu2 N6 C12 -1.14(17) . . . . ? O4 Cu2 N6 C12 -167.2(6) . . . . ? N4 Cu2 N6 C12 175.95(17) . . . . ? O5 Cu2 N6 C8 175.64(13) . . . . ? O4 Cu2 N6 C8 9.5(7) . . . . ? N4 Cu2 N6 C8 -7.27(12) . . . . ? O2 Cu1 O1 C14 -19.71(15) . . . . ? N3 Cu1 O1 C14 98.8(3) . . . . ? N1 Cu1 O1 C14 153.26(14) . . . . ? O3 Cu1 O1 C14 -113.37(14) . . . . ? O1 Cu1 O2 C16 17.48(14) . . . . ? N3 Cu1 O2 C16 -150.49(14) . . . . ? N1 Cu1 O2 C16 -114.1(3) . . . . ? O3 Cu1 O2 C16 117.64(14) . . . . ? O5 Cu2 O4 C19 5.17(14) . . . . ? N4 Cu2 O4 C19 -172.18(14) . . . . ? N6 Cu2 O4 C19 171.2(6) . . . . ? O4 Cu2 O5 C21 -8.70(15) . . . . ? N4 Cu2 O5 C21 156.3(3) . . . . ? N6 Cu2 O5 C21 172.59(15) . . . . ? C5 N1 C1 C2 -1.4(3) . . . . ? Cu1 N1 C1 C2 -179.86(13) . . . . ? N1 C1 C2 C3 1.4(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C1 N1 C5 C4 0.4(2) . . . . ? Cu1 N1 C5 C4 178.94(13) . . . . ? C1 N1 C5 C6 -179.78(14) . . . . ? Cu1 N1 C5 C6 -1.19(18) . . . . ? C3 C4 C5 N1 0.7(3) . . . . ? C3 C4 C5 C6 -179.18(16) . . . . ? N4 N3 C6 N2 3.6(2) . . . . ? Cu1 N3 C6 N2 -178.04(13) . . . . ? N4 N3 C6 C5 -176.90(13) . . . . ? Cu1 N3 C6 C5 1.48(18) . . . . ? N1 C5 C6 N3 -0.2(2) . . . . ? C4 C5 C6 N3 179.71(16) . . . . ? N1 C5 C6 N2 179.38(15) . . . . ? C4 C5 C6 N2 -0.8(3) . . . . ? N3 N4 C7 N5 6.9(2) . . . . ? Cu2 N4 C7 N5 169.47(14) . . . . ? N3 N4 C7 C8 -174.94(13) . . . . ? Cu2 N4 C7 C8 -12.37(18) . . . . ? C12 N6 C8 C9 -0.5(3) . . . . ? Cu2 N6 C8 C9 -177.50(14) . . . . ? C12 N6 C8 C7 -179.90(16) . . . . ? Cu2 N6 C8 C7 3.07(18) . . . . ? N4 C7 C8 N6 6.0(2) . . . . ? N5 C7 C8 N6 -175.78(16) . . . . ? N4 C7 C8 C9 -173.46(17) . . . . ? N5 C7 C8 C9 4.8(3) . . . . ? N6 C8 C9 C10 -0.3(3) . . . . ? C7 C8 C9 C10 179.03(17) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C9 C10 C11 C12 -1.1(3) . . . . ? C8 N6 C12 C11 0.5(3) . . . . ? Cu2 N6 C12 C11 177.12(16) . . . . ? C10 C11 C12 N6 0.3(3) . . . . ? Cu1 O1 C14 C15 14.6(3) . . . . ? Cu1 O1 C14 C13 -165.44(13) . . . . ? O1 C14 C15 C16 -0.2(3) . . . . ? C13 C14 C15 C16 179.83(18) . . . . ? Cu1 O2 C16 C15 -9.7(2) . . . . ? Cu1 O2 C16 C17 169.27(12) . . . . ? C14 C15 C16 O2 -2.4(3) . . . . ? C14 C15 C16 C17 178.60(18) . . . . ? Cu2 O4 C19 C20 0.1(3) . . . . ? Cu2 O4 C19 C18 -179.74(13) . . . . ? O4 C19 C20 C21 -4.7(3) . . . . ? C18 C19 C20 C21 175.1(2) . . . . ? Cu2 O5 C21 C20 7.1(3) . . . . ? Cu2 O5 C21 C22 -173.85(14) . . . . ? C19 C20 C21 O5 0.8(3) . . . . ? C19 C20 C21 C22 -178.3(2) . . . . ? #===END #============================================================================== data__x612 #(6) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 16.965(3) _cell_length_b 16.040(9) _cell_length_c 17.045(3) _cell_angle_alpha 90 _cell_angle_beta 100.72(1) _cell_angle_gamma 90 _cell_volume 4557(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 18.3 _cell_measurement_theta_max 22.6 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2-y, -z' '1/2-x,1/2-y, -z' '1/2+x,1/2-y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'irregular' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1231.02 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H48 Cu4 N20 O18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2512.00 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.810 _exptl_special_details ; The scan width was (1.31+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 7 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.76 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 3 4 2 2 2 2 2 _diffrn_reflns_number 5636 _reflns_number_total 5452 _reflns_number_gt 4135 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.01900 _diffrn_reflns_av_sigmaI/netI 0.059 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02125 _diffrn_orient_matrix_UB_12 0.03412 _diffrn_orient_matrix_UB_13 0.04842 _diffrn_orient_matrix_UB_21 -0.03844 _diffrn_orient_matrix_UB_22 -0.02796 _diffrn_orient_matrix_UB_23 0.02944 _diffrn_orient_matrix_UB_31 0.04086 _diffrn_orient_matrix_UB_32 -0.04405 _diffrn_orient_matrix_UB_33 0.01882 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 120 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 192 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 80 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 72 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cu 0 16 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.44288(1) 0.02580(2) 0.57709(1) 0.02547(7) 1.000 . Uani d ? Cu(2) 0.33542(2) -0.05078(2) 0.71258(2) 0.02791(7) 1.000 . Uani d ? O(1) 0.33877(8) 0.03893(8) 0.64105(8) 0.0246(4) 1.000 . Uani d ? O(2) 0.3407(1) 0.3262(1) 0.7140(1) 0.0506(6) 1.000 . Uani d ? O(3) 0.2538(1) 0.3904(1) 0.6295(1) 0.0836(8) 1.000 . Uani d ? O(4) 0.2555(1) 0.2568(1) 0.6284(1) 0.0712(8) 1.000 . Uani d ? O(5) 0.1755(2) 0.3014(2) 0.0725(2) 0.073(1) 0.800 S Uani d ? O(5) 0.1863(9) 0.218(1) 0.0768(8) 0.101(6) 0.200 S Uani d ? O(6) 0.126(1) 0.3067(8) -0.005(1) 0.082(5) 0.200 S Uani d ? O(6) 0.1195(3) 0.2665(3) -0.0441(2) 0.087(1) 0.800 S Uani d ? O(7) 0.1566(2) 0.1721(2) 0.0406(2) 0.077(1) 0.800 S Uani d ? O(7) 0.1149(8) 0.180(1) -0.0335(8) 0.090(5) 0.200 S Uani d ? O(8) 0.9221(2) 0.0118(2) 0.2019(2) 0.110(1) 1.000 . Uani d ? O(9) 0.9583(3) 0.0499(3) 0.5549(2) 0.103(1) 1.000 . Uani d ? N(1) 0.4505(1) 0.1514(1) 0.5692(1) 0.0273(5) 1.000 . Uani d ? N(2) 0.6147(1) 0.1482(1) 0.7383(1) 0.0349(6) 1.000 . Uani d ? N(3) 0.5357(1) 0.0458(1) 0.6612(1) 0.0238(5) 1.000 . Uani d ? N(4) 0.5750(1) -0.0246(1) 0.6982(1) 0.0237(5) 1.000 . Uani d ? N(5) 0.4787(1) -0.0873(1) 0.6027(1) 0.0320(5) 1.000 . Uani d ? N(6) 0.3535(1) -0.0013(1) 0.4846(1) 0.0310(6) 1.000 . Uani d ? N(7) 0.2191(1) -0.0595(2) 0.6657(1) 0.0397(6) 1.000 . Uani d ? N(8) 0.3613(1) -0.1664(1) 0.7459(1) 0.0291(5) 1.000 . Uani d ? N(9) 0.2828(1) 0.3244(2) 0.6559(1) 0.0451(7) 1.000 . Uani d ? N(10) 0.1497(1) 0.2445(2) 0.0220(1) 0.0467(8) 1.000 . Uani d ? C(1) 0.4031(1) 0.2031(2) 0.5202(1) 0.0351(7) 1.000 . Uani d ? C(2) 0.4099(2) 0.2880(2) 0.5255(2) 0.0405(8) 1.000 . Uani d ? C(3) 0.4670(2) 0.3215(2) 0.5842(2) 0.0431(8) 1.000 . Uani d ? C(4) 0.5165(1) 0.2691(1) 0.6363(1) 0.0336(7) 1.000 . Uani d ? C(5) 0.5073(1) 0.1847(1) 0.6274(1) 0.0244(6) 1.000 . Uani d ? C(6) 0.5570(1) 0.1224(1) 0.6801(1) 0.0236(6) 1.000 . Uani d ? C(7) 0.5396(1) -0.0928(1) 0.6617(1) 0.0248(6) 1.000 . Uani d ? C(8) 0.2786(1) -0.0200(2) 0.5144(1) 0.0290(6) 1.000 . Uani d ? C(9) 0.2686(1) 0.0403(1) 0.5805(1) 0.0272(6) 1.000 . Uani d ? C(10) 0.1977(1) 0.0176(2) 0.6184(2) 0.0378(7) 1.000 . Uani d ? C(11) 0.3274(2) -0.2355(2) 0.7108(2) 0.0391(7) 1.000 . Uani d ? C(12) 0.3554(2) -0.3141(2) 0.7339(2) 0.0442(8) 1.000 . Uani d ? C(13) 0.4191(2) -0.3213(2) 0.7958(2) 0.0412(8) 1.000 . Uani d ? C(14) 0.4546(1) -0.2505(1) 0.8329(2) 0.0337(7) 1.000 . Uani d ? C(15) 0.4251(1) -0.1738(1) 0.8058(1) 0.0252(6) 1.000 . Uani d ? H(1) 0.364(1) 0.178(1) 0.482(1) 0.038 1.000 . Uiso d ? H(2) 0.374(1) 0.319(1) 0.490(1) 0.044 1.000 . Uiso d ? H(3) 0.473(1) 0.378(2) 0.588(1) 0.048 1.000 . Uiso d ? H(4) 0.555(1) 0.290(1) 0.676(1) 0.040 1.000 . Uiso d ? H(5) 0.236(1) -0.015(1) 0.474(1) 0.032 1.000 . Uiso d ? H(6) 0.282(1) -0.077(1) 0.534(1) 0.032 1.000 . Uiso d ? H(7) 0.261(1) 0.099(1) 0.559(1) 0.032 1.000 . Uiso d ? H(8) 0.151(1) 0.007(1) 0.584(1) 0.045 1.000 . Uiso d ? H(9) 0.187(1) 0.064(2) 0.656(1) 0.045 1.000 . Uiso d ? H(10) 0.288(1) -0.224(2) 0.671(1) 0.047 1.000 . Uiso d ? H(11) 0.330(1) -0.361(2) 0.707(1) 0.048 1.000 . Uiso d ? H(12) 0.438(1) -0.370(2) 0.812(1) 0.046 1.000 . Uiso d ? H(13) 0.496(1) -0.253(1) 0.872(1) 0.039 1.000 . Uiso d ? H(14) 0.370(1) -0.043(1) 0.464(1) 0.036 1.000 . Uiso d ? H(15) 0.348(1) 0.041(1) 0.450(1) 0.036 1.000 . Uiso d ? H(16) 0.208(1) -0.106(2) 0.637(1) 0.046 1.000 . Uiso d ? H(17) 0.192(1) -0.067(1) 0.701(1) 0.024 1.000 . Uiso d ? H(18) 0.637(1) 0.115(1) 0.778(1) 0.041 1.000 . Uiso d ? H(19) 0.623(1) 0.197(2) 0.746(1) 0.041 1.000 . Uiso d ? H(20) 0.459(1) -0.130(1) 0.587(1) 0.038 1.000 . Uiso d ? H(21) 0.889(3) 0.051(3) 0.194(3) 0.134 1.000 . Uiso d ? H(22) 0.963(3) 0.014(3) 0.205(3) 0.134 1.000 . Uiso d ? H(23) 0.968(4) 0.042(4) 0.530(3) 0.121 1.000 . Uiso d ? H(24) 0.931(3) 0.044(3) 0.588(3) 0.121 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0246(1) 0.0259(1) 0.0231(1) 0.0001(1) -0.0028(1) 0.0009(1) Cu(2) 0.0279(1) 0.0274(2) 0.0249(1) -0.0048(1) -0.0043(1) 0.0020(1) O(1) 0.0258(8) 0.0249(8) 0.0204(7) -0.0007(6) -0.0028(6) -0.0001(6) O(2) 0.050(1) 0.052(1) 0.043(1) 0.0148(9) -0.0097(9) 0.0015(9) O(3) 0.075(2) 0.075(2) 0.090(2) 0.018(1) -0.011(1) 0.047(1) O(4) 0.068(1) 0.078(2) 0.064(2) -0.010(1) 0.003(1) -0.017(1) O(5) 0.070(2) 0.082(2) 0.065(2) -0.012(2) 0.010(2) -0.014(2) O(5) 0.10(1) 0.11(1) 0.07(1) 0.02(1) -0.060(8) 0.035(9) O(6) 0.082(9) 0.042(8) 0.11(1) 0.007(8) -0.01(1) 0.055(8) O(6) 0.103(3) 0.085(3) 0.057(2) 0.031(3) -0.028(2) 0.012(2) O(7) 0.085(3) 0.049(2) 0.098(3) 0.027(2) 0.018(2) 0.030(2) O(7) 0.09(1) 0.10(1) 0.08(1) -0.022(8) -0.003(8) -0.028(8) O(8) 0.159(4) 0.065(2) 0.115(2) 0.031(2) 0.048(3) 0.034(2) O(9) 0.117(3) 0.103(2) 0.085(3) -0.029(2) 0.012(2) 0.009(2) N(1) 0.028(1) 0.026(1) 0.026(1) 0.0005(8) 0.0009(8) 0.0062(8) N(2) 0.043(1) 0.022(1) 0.033(1) -0.0059(9) -0.0100(9) 0.0053(9) N(3) 0.0252(9) 0.0206(9) 0.0232(9) 0.0016(7) -0.0020(7) 0.0013(7) N(4) 0.0260(9) 0.0199(9) 0.0225(9) 0.0021(7) -0.0027(7) 0.0012(7) N(5) 0.033(1) 0.024(1) 0.034(1) 0.0006(8) -0.0076(9) -0.0053(9) N(6) 0.031(1) 0.035(1) 0.025(1) 0.0019(9) -0.0002(8) 0.0014(9) N(7) 0.031(1) 0.057(1) 0.030(1) -0.013(1) 0.0014(9) 0.006(1) N(8) 0.035(1) 0.024(1) 0.026(1) -0.0054(8) 0.0008(8) -0.0006(8) N(9) 0.041(1) 0.058(2) 0.036(1) 0.007(1) 0.006(1) 0.008(1) N(10) 0.038(1) 0.057(2) 0.045(2) 0.013(1) 0.009(1) 0.014(1) C(1) 0.032(1) 0.038(1) 0.031(1) 0.002(1) -0.003(1) 0.009(1) C(2) 0.046(2) 0.036(1) 0.038(2) 0.012(1) 0.003(1) 0.014(1) C(3) 0.055(2) 0.024(1) 0.050(2) 0.006(1) 0.010(1) 0.005(1) C(4) 0.037(1) 0.027(1) 0.035(1) 0.001(1) 0.003(1) 0.000(1) C(5) 0.023(1) 0.026(1) 0.024(1) 0.0010(9) 0.0036(9) 0.0042(9) C(6) 0.024(1) 0.026(1) 0.020(1) -0.0003(9) 0.0029(9) 0.0017(9) C(7) 0.025(1) 0.024(1) 0.025(1) 0.0016(9) 0.0028(9) -0.0006(9) C(8) 0.026(1) 0.036(1) 0.023(1) -0.003(1) -0.0029(9) -0.002(1) C(9) 0.027(1) 0.025(1) 0.026(1) 0.0036(9) -0.0039(9) 0.0018(9) C(10) 0.024(1) 0.053(2) 0.035(1) 0.005(1) 0.001(1) -0.002(1) C(11) 0.045(2) 0.036(1) 0.033(1) -0.010(1) -0.000(1) -0.003(1) C(12) 0.057(2) 0.026(1) 0.049(2) -0.011(1) 0.008(1) -0.008(1) C(13) 0.049(2) 0.024(1) 0.053(2) -0.001(1) 0.014(1) 0.003(1) C(14) 0.033(1) 0.029(1) 0.038(1) -0.001(1) 0.004(1) 0.002(1) C(15) 0.028(1) 0.022(1) 0.026(1) -0.0035(9) 0.0067(9) -0.0006(9) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000059(3) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4135 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_all 0.0330 _refine_ls_wR_factor_ref 0.0310 _refine_ls_goodness_of_fit_all 1.459 _refine_ls_goodness_of_fit_ref 1.560 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.33 _refine_diff_density_max 0.00 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) O(1) 2.251(2) . . ? Cu(1) N(1) 2.025(2) . . ? Cu(1) N(3) 1.950(2) . . ? Cu(1) N(5) 1.936(2) . . ? Cu(1) N(6) 2.020(2) . . ? Cu(2) O(1) 1.894(2) . . ? Cu(2) N(4) 1.984(2) . . ? Cu(2) N(7) 1.991(3) . . ? Cu(2) N(8) 1.966(2) . . ? O(1) C(9) 1.424(3) . . ? O(2) N(9) 1.257(3) . . ? O(3) N(9) 1.219(3) . . ? O(4) N(9) 1.237(4) . . ? O(5) O(5a) 1.35(2) . . ? O(5) O(6a) 1.43(2) . . ? O(5) N(10) 1.274(4) . . ? O(5a) O(7) 1.03(2) . . ? O(5a) N(10) 1.10(1) . . ? O(6a) O(6) 0.92(2) . . ? O(6a) N(10) 1.14(1) . . ? O(6) O(7a) 1.41(2) . . ? O(6) N(10) 1.200(5) . . ? O(7) O(7a) 1.33(2) . . ? O(7) N(10) 1.204(4) . . ? O(7a) N(10) 1.46(1) . . ? O(8) H(21) 0.84(5) . . no O(8) H(22) 0.68(6) . . no O(9) H(23) 0.50(6) . . no O(9) H(24) 0.79(5) . . no N(1) C(1) 1.335(3) . . ? N(1) C(5) 1.357(3) . . ? N(2) C(6) 1.324(3) . . ? N(2) H(18) 0.88(3) . . no N(2) H(19) 0.81(3) . . no N(3) N(4) 1.400(3) . . ? N(3) C(6) 1.303(3) . . ? N(4) C(7) 1.342(3) . . ? N(5) C(7) 1.304(3) . . ? N(5) H(20) 0.79(3) . . no N(6) C(8) 1.486(4) . . ? N(6) H(14) 0.83(3) . . no N(6) H(15) 0.90(3) . . no N(7) C(10) 1.484(4) . . ? N(7) H(16) 0.89(3) . . no N(7) H(17) 0.83(3) . . no N(8) C(11) 1.338(4) . . ? N(8) C(15) 1.348(3) . . ? C(1) C(2) 1.368(4) . . ? C(1) H(1) 0.93(3) . . no C(2) C(3) 1.367(5) . . ? C(2) H(2) 0.92(3) . . no C(3) C(4) 1.387(4) . . ? C(3) H(3) 0.92(3) . . no C(4) C(5) 1.368(4) . . ? C(4) H(4) 0.92(3) . . no C(5) C(6) 1.495(3) . . ? C(7) C(15) 1.493(4) . . ? C(8) C(9) 1.519(4) . . ? C(8) H(5) 0.90(3) . . no C(8) H(6) 0.97(3) . . no C(9) C(10) 1.512(4) . . ? C(9) H(7) 1.01(3) . . no C(10) H(8) 0.91(3) . . no C(10) H(9) 1.02(3) . . no C(11) C(12) 1.377(4) . . ? C(11) H(10) 0.88(3) . . no C(12) C(13) 1.368(5) . . ? C(12) H(11) 0.94(3) . . no C(13) C(14) 1.383(4) . . ? C(13) H(12) 0.87(3) . . no C(14) C(15) 1.375(4) . . ? C(14) H(13) 0.87(3) . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cu(1) N(1) 90.27(8) . . . ? O(1) Cu(1) N(3) 103.17(8) . . . ? O(1) Cu(1) N(5) 102.72(9) . . . ? O(1) Cu(1) N(6) 81.71(8) . . . ? N(1) Cu(1) N(3) 80.33(9) . . . ? N(1) Cu(1) N(5) 157.7(1) . . . ? N(1) Cu(1) N(6) 102.1(1) . . . ? N(3) Cu(1) N(5) 79.12(9) . . . ? N(3) Cu(1) N(6) 174.6(1) . . . ? N(5) Cu(1) N(6) 97.7(1) . . . ? O(1) Cu(2) N(4) 102.86(8) . . . ? O(1) Cu(2) N(7) 86.6(1) . . . ? O(1) Cu(2) N(8) 150.60(9) . . . ? N(4) Cu(2) N(7) 152.0(1) 2_656 2_656 2_656 ? N(4) Cu(2) N(8) 83.09(9) 2_656 2_656 2_656 ? N(7) Cu(2) N(8) 101.6(1) . . . ? Cu(1) O(1) Cu(2) 111.15(8) . . . ? Cu(1) O(1) C(9) 106.0(2) . . . ? Cu(2) O(1) C(9) 110.9(2) . . . ? O(5a) O(5) O(6a) 99.2(9) . . . ? O(5a) O(5) N(10) 49.7(6) . . . ? O(6a) O(5) N(10) 49.5(7) . . . ? O(5) O(5a) O(7) 129(1) . . . ? O(5) O(5a) N(10) 62(1) . . . ? O(7) O(5a) N(10) 69(1) . . . ? O(5) O(6a) O(6) 127(2) . . . ? O(5) O(6a) N(10) 58.0(8) . . . ? O(6) O(6a) N(10) 70(1) . . . ? O(6a) O(6) O(7a) 127(2) . . . ? O(6a) O(6) N(10) 64(1) . . . ? O(7a) O(6) N(10) 67.3(7) . . . ? O(5a) O(7) O(7a) 128(1) . . . ? O(5a) O(7) N(10) 58.6(9) . . . ? O(7a) O(7) N(10) 69.9(8) . . . ? O(6) O(7a) O(7) 100(1) . . . ? O(6) O(7a) N(10) 49.5(6) . . . ? O(7) O(7a) N(10) 50.9(5) . . . ? H(21) O(8) H(22) 128(7) . . . no H(23) O(9) H(24) 153(11) . . . no Cu(1) N(1) C(1) 128.4(2) . . . ? Cu(1) N(1) C(5) 112.9(2) . . . ? C(1) N(1) C(5) 118.4(2) . . . ? C(6) N(2) H(18) 123(2) . . . no C(6) N(2) H(19) 121(2) . . . no H(18) N(2) H(19) 115(3) . . . no Cu(1) N(3) N(4) 116.7(2) . . . ? Cu(1) N(3) C(6) 119.0(2) . . . ? N(4) N(3) C(6) 124.2(2) . . . ? Cu(2) N(4) N(3) 138.4(2) 2_656 2_656 2_656 ? Cu(2) N(4) C(7) 113.3(2) 2_656 2_656 2_656 ? N(3) N(4) C(7) 108.3(2) . . . ? Cu(1) N(5) C(7) 114.1(2) . . . ? Cu(1) N(5) H(20) 129(2) . . . no C(7) N(5) H(20) 116(2) . . . no Cu(1) N(6) C(8) 110.0(2) . . . ? Cu(1) N(6) H(14) 104(2) . . . no Cu(1) N(6) H(15) 109(2) . . . no C(8) N(6) H(14) 111(2) . . . no C(8) N(6) H(15) 113(2) . . . no H(14) N(6) H(15) 109(3) . . . no Cu(2) N(7) C(10) 106.5(2) . . . ? Cu(2) N(7) H(16) 112(2) . . . no Cu(2) N(7) H(17) 111(2) . . . no C(10) N(7) H(16) 113(2) . . . no C(10) N(7) H(17) 114(2) . . . no H(16) N(7) H(17) 101(3) . . . no Cu(2) N(8) C(11) 126.7(2) . . . ? Cu(2) N(8) C(15) 114.0(2) . . . ? C(11) N(8) C(15) 119.0(3) . . . ? O(2) N(9) O(3) 118.3(3) . . . ? O(2) N(9) O(4) 120.1(3) . . . ? O(3) N(9) O(4) 121.6(3) . . . ? O(5) N(10) O(5a) 69(1) . . . ? O(5) N(10) O(6a) 72(1) . . . ? O(5) N(10) O(6) 117.1(4) . . . ? O(5) N(10) O(7) 120.6(4) . . . ? O(5) N(10) O(7a) 175.9(7) . . . ? O(5a) N(10) O(6a) 141(2) . . . ? O(5a) N(10) O(6) 169(1) . . . ? O(5a) N(10) O(7) 53(1) . . . ? O(5a) N(10) O(7a) 112(1) . . . ? O(6a) N(10) O(6) 46(1) . . . ? O(6a) N(10) O(7) 164(1) . . . ? O(6a) N(10) O(7a) 107(1) . . . ? O(6) N(10) O(7) 122.2(5) . . . ? O(6) N(10) O(7a) 63.2(8) . . . ? O(7) N(10) O(7a) 59.2(8) . . . ? N(1) C(1) C(2) 122.9(3) . . . ? N(1) C(1) H(1) 116(2) . . . no C(2) C(1) H(1) 121(2) . . . no C(1) C(2) C(3) 118.6(3) . . . ? C(1) C(2) H(2) 117(2) . . . no C(3) C(2) H(2) 124(2) . . . no C(2) C(3) C(4) 119.5(3) . . . ? C(2) C(3) H(3) 120(2) . . . no C(4) C(3) H(3) 120(2) . . . no C(3) C(4) C(5) 119.0(3) . . . ? C(3) C(4) H(4) 121(2) . . . no C(5) C(4) H(4) 120(2) . . . no N(1) C(5) C(4) 121.5(2) . . . ? N(1) C(5) C(6) 114.8(2) . . . ? C(4) C(5) C(6) 123.7(2) . . . ? N(2) C(6) N(3) 127.7(2) . . . ? N(2) C(6) C(5) 119.8(2) . . . ? N(3) C(6) C(5) 112.5(2) . . . ? N(4) C(7) N(5) 121.6(2) . . . ? N(4) C(7) C(15) 115.1(2) . . . ? N(5) C(7) C(15) 123.3(2) . . . ? N(6) C(8) C(9) 110.2(2) . . . ? N(6) C(8) H(5) 110(2) . . . no N(6) C(8) H(6) 107(2) . . . no C(9) C(8) H(5) 109(2) . . . no C(9) C(8) H(6) 111(2) . . . no H(5) C(8) H(6) 109(2) . . . no O(1) C(9) C(8) 109.5(2) . . . ? O(1) C(9) C(10) 108.1(2) . . . ? O(1) C(9) H(7) 108(2) . . . no C(8) C(9) C(10) 111.8(2) . . . ? C(8) C(9) H(7) 111(2) . . . no C(10) C(9) H(7) 109(2) . . . no N(7) C(10) C(9) 107.4(2) . . . ? N(7) C(10) H(8) 107(2) . . . no N(7) C(10) H(9) 109(2) . . . no C(9) C(10) H(8) 115(2) . . . no C(9) C(10) H(9) 110(2) . . . no H(8) C(10) H(9) 108(2) . . . no N(8) C(11) C(12) 122.3(3) . . . ? N(8) C(11) H(10) 112(2) . . . no C(12) C(11) H(10) 125(2) . . . no C(11) C(12) C(13) 118.6(3) . . . ? C(11) C(12) H(11) 119(2) . . . no C(13) C(12) H(11) 122(2) . . . no C(12) C(13) C(14) 119.8(3) . . . ? C(12) C(13) H(12) 121(2) . . . no C(14) C(13) H(12) 119(2) . . . no C(13) C(14) C(15) 118.8(3) . . . ? C(13) C(14) H(13) 122(2) . . . no C(15) C(14) H(13) 119(2) . . . no N(8) C(15) C(7) 114.4(2) . . . ? N(8) C(15) C(14) 121.5(3) . . . ? C(7) C(15) C(14) 124.0(3) 2_656 2_656 2_656 ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(2) O(3) 3.457(3) . 6_546 no O(2) O(8) 2.968(5) . 8_455 no O(2) N(2) 3.026(4) . 2_656 no O(2) N(7) 3.061(4) . 6_556 no O(2) C(4) 3.304(4) . 2_656 no O(2) C(3) 3.355(4) . . no O(2) C(11) 3.481(4) . 6_556 no O(3) N(6) 2.990(4) . 7_556 no O(3) C(8) 3.183(4) . 7_556 no O(3) N(8) 3.272(4) . 6_556 no O(3) O(8) 3.290(5) . 8_455 no O(3) N(7) 3.529(4) . 6_556 no O(3) C(15) 3.569(4) . 6_556 no O(4) C(11) 3.309(4) . 6_556 no O(4) N(2) 3.345(4) . 2_656 no O(4) C(1) 3.397(4) . 7_556 no O(4) N(8) 3.409(4) . 6_556 no O(4) C(2) 3.449(4) . . no O(4) C(12) 3.463(4) . 6_556 no O(4) C(1) 3.482(4) . . no O(4) C(2) 3.540(4) . 7_556 no O(4) C(9) 3.583(4) . . no O(5) C(5) 3.173(4) . 8_454 no O(5) C(6) 3.206(4) . 8_454 no O(5) N(2) 3.285(4) . 8_454 no O(5) C(4) 3.290(5) . 8_454 no O(5) N(6) 3.320(5) . 6 no O(5) C(11) 3.326(5) . 4_554 no O(5) C(8) 3.380(5) . 6 no O(5a) N(7) 2.96(2) . 4_554 no O(5a) C(11) 3.00(1) . 4_554 no O(5a) C(4) 3.23(2) . 8_454 no O(5a) O(6) 3.45(2) . 7 no O(5a) N(10) 3.56(2) . 7 no O(6a) N(5) 2.78(2) . 6 no O(6a) N(6) 3.11(2) . 6 no O(6a) C(8) 3.24(2) . 6 no O(6a) C(5) 3.30(2) . 8_454 no O(6a) N(1) 3.51(2) . 8_454 no O(6a) C(4) 3.52(2) . 8_454 no O(6) N(5) 2.943(5) . 6 no O(6) C(11) 3.137(6) . 6 no O(6) C(14) 3.181(6) . 5_454 no O(6) C(12) 3.582(6) . 6 no O(7) N(7) 2.845(5) . 4_554 no O(7) O(9) 3.018(9) . 2_655 no O(7) C(4) 3.262(5) . 8_454 no O(7) C(8) 3.282(5) . 4_554 no O(7) C(10) 3.341(5) . 4_554 no O(7) C(3) 3.435(6) . 8_454 no O(7a) O(9) 2.41(2) . 2_655 no O(7a) C(14) 3.40(2) . 5_454 no O(7a) C(3) 3.49(2) . 8_454 no O(7a) C(12) 3.55(2) . 6 no O(8) O(8) 2.84(1) . 2_755 no O(8) O(9) 2.866(7) . 4_554 no O(8) C(12) 3.444(6) . 8_544 no O(8) C(13) 3.453(5) . 8_544 no O(8) C(3) 3.511(5) . 8_554 no O(8) N(9) 3.523(5) . 8_554 no O(9) O(9) 3.01(1) . 3_756 no O(9) C(3) 3.549(6) . 7_656 no N(1) N(5) 3.521(4) . 3_656 no N(3) N(6) 3.457(3) . 3_656 no N(4) N(6) 3.571(3) . 3_656 no N(7) N(9) 3.571(4) . 6_546 no N(8) N(9) 3.214(4) . 6_546 no N(9) C(11) 3.342(4) . 6_556 no N(9) C(2) 3.423(4) . . no N(9) C(3) 3.561(4) . . no N(10) C(4) 3.254(4) . 8_454 no N(10) C(5) 3.460(4) . 8_454 no C(1) C(14) 3.546(4) . 4_554 no C(2) C(14) 3.555(5) . 4_554 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cu(1) O(1) Cu(2) N(4) . . . . 74.2(1) no Cu(1) O(1) Cu(2) N(7) . . . . -132.4(1) no Cu(1) O(1) Cu(2) N(8) . . . . -24.6(2) no Cu(1) O(1) C(9) C(8) . . . . 37.7(2) no Cu(1) O(1) C(9) C(10) . . . . 159.7(2) no Cu(1) N(1) C(1) C(2) . . . . 173.8(2) no Cu(1) N(1) C(5) C(4) . . . . -174.2(2) no Cu(1) N(1) C(5) C(6) . . . . 5.3(3) no Cu(1) N(3) N(4) Cu(2) . . . . -175.7(2) no Cu(1) N(3) N(4) C(7) . . . . 3.4(3) no Cu(1) N(3) C(6) N(2) . . . . 175.6(2) no Cu(1) N(3) C(6) C(5) . . . . -4.2(3) no Cu(1) N(5) C(7) N(4) . . . . -2.5(4) no Cu(1) N(5) C(7) C(15) . . . . 177.1(2) no Cu(1) N(6) C(8) C(9) . . . . 41.2(3) no Cu(2) O(1) Cu(1) N(1) . . . . -149.91(9) no Cu(2) O(1) Cu(1) N(3) . . . . -69.8(1) no Cu(2) O(1) Cu(1) N(5) . . . . 11.8(1) no Cu(2) O(1) Cu(1) N(6) . . . . 107.9(1) no Cu(2) O(1) C(9) C(8) . . . . -83.1(2) no Cu(2) O(1) C(9) C(10) . . . . 38.9(3) no Cu(2) N(4) N(3) C(6) . . . . 3.7(4) no Cu(2) N(4) C(7) N(5) . . . . 178.8(2) no Cu(2) N(4) C(7) C(15) . . . . -0.9(3) no Cu(2) N(7) C(10) C(9) . . . . 36.3(3) no Cu(2) N(8) C(11) C(12) . . . . 173.3(3) no Cu(2) N(8) C(15) C(7) . . . . 3.5(3) no Cu(2) N(8) C(15) C(14) . . . . -175.7(2) no O(1) Cu(1) N(1) C(1) . . . . -75.7(3) no O(1) Cu(1) N(1) C(5) . . . . 97.5(2) no O(1) Cu(1) N(3) N(4) . . . . 97.0(2) no O(1) Cu(1) N(3) C(6) . . . . -82.4(2) no O(1) Cu(1) N(5) C(7) . . . . -98.0(2) no O(1) Cu(1) N(6) C(8) . . . . -15.5(2) no O(1) Cu(2) N(4) N(3) . . . . 30.4(3) no O(1) Cu(2) N(4) C(7) . . . . -148.6(2) no O(1) Cu(2) N(7) C(10) . . . . -13.0(2) no O(1) Cu(2) N(8) C(11) . . . . -72.6(3) no O(1) Cu(2) N(8) C(15) . . . . 100.8(2) no O(1) C(9) C(8) N(6) . . . . -54.1(3) no O(1) C(9) C(10) N(7) . . . . -49.7(3) no O(5) O(5a) O(7) O(7a) . . . . 21(4) no O(5) O(5a) O(7) N(10) . . . . 12(2) no O(5) O(5a) N(10) O(6a) . . . . -1(3) no O(5) O(5a) N(10) O(6) . . . . 123(6) no O(5) O(5a) N(10) O(7) . . . . -169(1) no O(5) O(5a) N(10) O(7a) . . . . -175.6(8) no O(5) O(6a) O(6) O(7a) . . . . 39(4) no O(5) O(6a) O(6) N(10) . . . . 15(2) no O(5) O(6a) N(10) O(5a) . . . . 1(3) no O(5) O(6a) N(10) O(6) . . . . -166(2) no O(5) O(6a) N(10) O(7) . . . . 145(4) no O(5) O(6a) N(10) O(7a) . . . . 175.8(8) no O(5) N(10) O(5a) O(7) . . . . 169(1) no O(5) N(10) O(6a) O(6) . . . . 166(2) no O(5) N(10) O(6) O(6a) . . . . -15(2) no O(5) N(10) O(6) O(7a) . . . . -175.5(8) no O(5) N(10) O(7) O(5a) . . . . -12(2) no O(5) N(10) O(7) O(7a) . . . . 175.3(9) no O(5) N(10) O(7a) O(6) . . . . 96(13) no O(5) N(10) O(7a) O(7) . . . . -89(13) no O(5a) O(5) O(6a) O(6) . . . . -18(3) no O(5a) O(5) O(6a) N(10) . . . . -1(1) no O(5a) O(5) N(10) O(6a) . . . . 179(2) no O(5a) O(5) N(10) O(6) . . . . -169(1) no O(5a) O(5) N(10) O(7) . . . . 10(1) no O(5a) O(5) N(10) O(7a) . . . . 97(13) no O(5a) O(7) O(7a) O(6) . . . . -4(2) no O(5a) O(7) O(7a) N(10) . . . . -8(2) no O(5a) O(7) N(10) O(6a) . . . . -152(5) no O(5a) O(7) N(10) O(6) . . . . 167(2) no O(5a) O(7) N(10) O(7a) . . . . 173(2) no O(5a) N(10) O(5) O(6a) . . . . -179(2) no O(5a) N(10) O(6a) O(6) . . . . 167(2) no O(5a) N(10) O(6) O(6a) . . . . -134(7) no O(5a) N(10) O(6) O(7a) . . . . 66(7) no O(5a) N(10) O(7) O(7a) . . . . -173(2) no O(5a) N(10) O(7a) O(6) . . . . -169(1) no O(5a) N(10) O(7a) O(7) . . . . 6(2) no O(6a) O(5) O(5a) O(7) . . . . -12(3) no O(6a) O(5) O(5a) N(10) . . . . 1(1) no O(6a) O(5) N(10) O(6) . . . . 12(1) no O(6a) O(5) N(10) O(7) . . . . -169(1) no O(6a) O(5) N(10) O(7a) . . . . -83(13) no O(6a) O(6) O(7a) O(7) . . . . -27(3) no O(6a) O(6) O(7a) N(10) . . . . -23(2) no O(6a) O(6) N(10) O(7) . . . . 165(2) no O(6a) O(6) N(10) O(7a) . . . . 160(2) no O(6a) N(10) O(5a) O(7) . . . . 168(2) no O(6a) N(10) O(6) O(7a) . . . . -160(2) no O(6a) N(10) O(7) O(7a) . . . . 35(5) no O(6a) N(10) O(7a) O(6) . . . . 15(2) no O(6a) N(10) O(7a) O(7) . . . . -170(1) no O(6) O(6a) O(5) N(10) . . . . -17(2) no O(6) O(6a) N(10) O(7) . . . . -49(5) no O(6) O(6a) N(10) O(7a) . . . . -19(2) no O(6) O(7a) O(7) N(10) . . . . 4.0(7) no O(6) O(7a) N(10) O(7) . . . . -174.8(9) no O(6) N(10) O(5a) O(7) . . . . -68(7) no O(6) N(10) O(7) O(7a) . . . . -5.5(9) no O(6) N(10) O(7a) O(7) . . . . 174.8(9) no O(7) O(5a) O(5) N(10) . . . . -13(2) no O(7) O(5a) N(10) O(7a) . . . . -6(2) no O(7) O(7a) O(6) N(10) . . . . -4.1(7) no O(7) N(10) O(6) O(7a) . . . . 5.3(9) no O(7a) O(6) O(6a) N(10) . . . . 23(2) no O(7a) O(7) O(5a) N(10) . . . . 8(2) no N(1) Cu(1) O(1) C(9) . . . . 89.4(2) no N(1) Cu(1) N(3) N(4) . . . . -175.0(2) no N(1) Cu(1) N(3) C(6) . . . . 5.6(2) no N(1) Cu(1) N(5) C(7) . . . . 26.3(4) no N(1) Cu(1) N(6) C(8) . . . . -104.0(2) no N(1) C(1) C(2) C(3) . . . . -1.0(5) no N(1) C(5) C(4) C(3) . . . . -0.4(5) no N(1) C(5) C(6) N(2) . . . . 179.2(3) no N(1) C(5) C(6) N(3) . . . . -1.1(3) no N(2) C(6) N(3) N(4) . . . . -3.8(5) no N(2) C(6) C(5) C(4) . . . . -1.3(4) no N(3) Cu(1) O(1) C(9) . . . . 169.6(2) no N(3) Cu(1) N(1) C(1) . . . . -179.0(3) no N(3) Cu(1) N(1) C(5) . . . . -5.8(2) no N(3) Cu(1) N(5) C(7) . . . . 3.3(2) no N(3) Cu(1) N(6) C(8) . . . . 139(1) no N(3) N(4) Cu(2) N(7) . . . . -77.1(3) no N(3) N(4) Cu(2) N(8) . . . . -178.8(3) no N(3) N(4) C(7) N(5) . . . . -0.5(4) no N(3) N(4) C(7) C(15) . . . . 179.8(2) no N(3) C(6) C(5) C(4) . . . . 178.4(3) no N(4) Cu(2) O(1) C(9) . . . . -168.1(2) no N(4) Cu(2) N(7) C(10) . . . . 98.3(3) no N(4) Cu(2) N(8) C(11) . . . . -176.6(3) no N(4) Cu(2) N(8) C(15) . . . . -3.1(2) no N(4) N(3) Cu(1) N(5) . . . . -3.7(2) no N(4) N(3) Cu(1) N(6) . . . . -57(1) no N(4) N(3) C(6) C(5) . . . . 176.5(2) no N(4) C(7) C(15) N(8) . . . . -1.7(4) no N(4) C(7) C(15) C(14) . . . . 177.5(3) no N(5) Cu(1) O(1) C(9) . . . . -108.8(2) no N(5) Cu(1) N(1) C(1) . . . . 158.0(3) no N(5) Cu(1) N(1) C(5) . . . . -28.8(4) no N(5) Cu(1) N(3) C(6) . . . . 176.9(2) no N(5) Cu(1) N(6) C(8) . . . . 86.3(2) no N(5) C(7) C(15) N(8) . . . . 178.6(3) no N(5) C(7) C(15) C(14) . . . . -2.2(5) no N(6) Cu(1) O(1) C(9) . . . . -12.8(2) no N(6) Cu(1) N(1) C(1) . . . . 5.9(3) no N(6) Cu(1) N(1) C(5) . . . . 179.1(2) no N(6) Cu(1) N(3) C(6) . . . . 123(1) no N(6) Cu(1) N(5) C(7) . . . . 178.9(2) no N(6) C(8) C(9) C(10) . . . . -173.9(2) no N(7) Cu(2) O(1) C(9) . . . . -14.7(2) no N(7) Cu(2) N(4) C(7) . . . . 103.9(3) no N(7) Cu(2) N(8) C(11) . . . . 31.4(3) no N(7) Cu(2) N(8) C(15) . . . . -155.1(2) no N(7) C(10) C(9) C(8) . . . . 71.0(3) no N(8) Cu(2) O(1) C(9) . . . . 93.1(2) no N(8) Cu(2) N(4) C(7) . . . . 2.2(2) no N(8) Cu(2) N(7) C(10) . . . . -164.6(2) no N(8) C(11) C(12) C(13) . . . . 1.2(5) no N(8) C(15) C(14) C(13) . . . . 2.0(5) no C(1) N(1) C(5) C(4) . . . . -0.2(4) no C(1) N(1) C(5) C(6) . . . . 179.3(2) no C(1) C(2) C(3) C(4) . . . . 0.3(5) no C(2) C(1) N(1) C(5) . . . . 0.9(5) no C(2) C(3) C(4) C(5) . . . . 0.3(5) no C(3) C(4) C(5) C(6) . . . . -179.8(3) no C(6) N(3) N(4) C(7) . . . . -177.3(3) no C(7) C(15) N(8) C(11) . . . . 177.5(3) no C(7) C(15) C(14) C(13) . . . . -177.1(3) no C(11) N(8) C(15) C(14) . . . . -1.7(4) no C(11) C(12) C(13) C(14) . . . . -0.9(5) no C(12) C(11) N(8) C(15) . . . . 0.1(5) no C(12) C(13) C(14) C(15) . . . . -0.6(5) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #===END data__cjm2-36 #(7) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 10.757(4) _cell_length_b 10.993(3) _cell_length_c 10.590(3) _cell_angle_alpha 110.80(2) _cell_angle_beta 99.77(3) _cell_angle_gamma 90.34(3) _cell_volume 1150.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 634.47 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H17 Cu2 N11 O9 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 640.00 _exptl_absorpt_coefficient_mu 1.923 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.768 _exptl_special_details ; The scan width was (1.26+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 6 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.64 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 1 3 -1 0 2 -2 0 _diffrn_reflns_number 5569 _reflns_number_total 5289 _reflns_number_gt 3369 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02810 _diffrn_reflns_av_sigmaI/netI 0.096 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02486 _diffrn_orient_matrix_UB_12 -0.05063 _diffrn_orient_matrix_UB_13 0.06118 _diffrn_orient_matrix_UB_21 0.01609 _diffrn_orient_matrix_UB_22 -0.07573 _diffrn_orient_matrix_UB_23 -0.08072 _diffrn_orient_matrix_UB_31 0.08982 _diffrn_orient_matrix_UB_32 0.03496 _diffrn_orient_matrix_UB_33 0.01741 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 34 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 22 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 18 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cu 0 4 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.69030(4) 0.03687(4) 0.54580(4) 0.0388(1) 1.000 . Uani d ? Cu(2) 1.03189(5) 0.28613(5) 0.83044(5) 0.0469(1) 1.000 . Uani d ? O(1) 1.0656(3) 0.2761(3) 0.6451(3) 0.060(1) 1.000 . Uani d ? O(2) 1.1119(3) 0.0918(3) 0.6657(4) 0.077(1) 1.000 . Uani d ? O(3) 1.1212(3) 0.1178(4) 0.4761(3) 0.089(1) 1.000 . Uani d ? O(4) 1.2043(3) 0.3624(3) 0.9234(3) 0.071(1) 1.000 . Uani d ? O(5) 1.0967(4) 0.5168(3) 0.8941(4) 0.099(1) 1.000 . Uani d ? O(6) 1.2972(3) 0.5523(4) 0.9743(4) 0.101(1) 1.000 . Uani d ? O(7) 0.6316(3) -0.1467(3) 0.8435(3) 0.066(1) 1.000 . Uani d ? O(8) 0.5974(3) -0.3481(3) 0.7168(3) 0.080(1) 1.000 . Uani d ? O(9) 0.5081(3) -0.2689(3) 0.8923(3) 0.076(1) 1.000 . Uani d ? N(1) 0.6004(3) -0.1371(3) 0.4364(3) 0.0400(9) 1.000 . Uani d ? N(2) 0.5818(3) -0.0481(3) 0.1406(3) 0.055(1) 1.000 . Uani d ? N(3) 0.6480(3) 0.0616(3) 0.3748(3) 0.0407(9) 1.000 . Uani d ? N(4) 0.6768(3) 0.1653(3) 0.3387(3) 0.046(1) 1.000 . Uani d ? N(5) 0.7890(3) 0.2054(3) 0.6264(3) 0.0388(8) 1.000 . Uani d ? N(6) 0.8509(3) 0.2295(3) 0.7605(3) 0.0388(8) 1.000 . Uani d ? N(7) 0.7268(3) 0.0475(3) 0.7348(3) 0.0431(9) 1.000 . Uani d ? N(8) 0.9988(3) 0.2226(3) 0.9752(3) 0.0428(9) 1.000 . Uani d ? N(9) 1.1003(3) 0.1579(4) 0.5928(4) 0.061(1) 1.000 . Uani d ? N(10) 1.1997(4) 0.4828(4) 0.9306(4) 0.068(1) 1.000 . Uani d ? N(11) 0.5800(3) -0.2558(3) 0.8172(3) 0.049(1) 1.000 . Uani d ? C(1) 0.5782(4) -0.2337(4) 0.4792(4) 0.045(1) 1.000 . Uani d ? C(2) 0.5297(4) -0.3554(4) 0.3889(4) 0.050(1) 1.000 . Uani d ? C(3) 0.5034(4) -0.3792(4) 0.2512(4) 0.055(1) 1.000 . Uani d ? C(4) 0.5246(4) -0.2805(4) 0.2055(4) 0.049(1) 1.000 . Uani d ? C(5) 0.5731(3) -0.1599(3) 0.3002(3) 0.038(1) 1.000 . Uani d ? C(6) 0.6017(3) -0.0439(4) 0.2662(4) 0.042(1) 1.000 . Uani d ? C(7) 0.7348(4) 0.2713(4) 0.4298(4) 0.046(1) 1.000 . Uani d ? C(8) 0.7580(5) 0.3773(4) 0.3758(5) 0.067(2) 1.000 . Uani d ? C(9) 0.7857(3) 0.2990(3) 0.5789(4) 0.043(1) 1.000 . Uani d ? C(10) 0.8313(4) 0.4365(4) 0.6691(4) 0.058(1) 1.000 . Uani d ? C(11) 0.8147(3) 0.1381(3) 0.8065(3) 0.038(1) 1.000 . Uani d ? C(12) 0.8884(3) 0.1531(3) 0.9437(4) 0.040(1) 1.000 . Uani d ? C(13) 0.8496(4) 0.0991(4) 1.0318(4) 0.051(1) 1.000 . Uani d ? C(14) 0.9291(4) 0.1197(4) 1.1566(4) 0.056(1) 1.000 . Uani d ? C(15) 1.0424(4) 0.1910(4) 1.1894(4) 0.058(1) 1.000 . Uani d ? C(16) 1.0752(4) 0.2416(4) 1.0966(4) 0.052(1) 1.000 . Uani d ? H(1) 0.5959 -0.2182 0.5747 0.055 1.000 . Uiso c ? H(2) 0.5148 -0.4228 0.4217 0.061 1.000 . Uiso c ? H(3) 0.4707 -0.4630 0.1880 0.067 1.000 . Uiso c ? H(4) 0.5065 -0.2951 0.1107 0.060 1.000 . Uiso c ? H(5) 0.7772 0.4584 0.4502 0.081 1.000 . Uiso c ? H(6) 0.8269 0.3577 0.3281 0.081 1.000 . Uiso c ? H(7) 0.6843 0.3827 0.3146 0.081 1.000 . Uiso c ? H(8) 0.8361 0.4462 0.7627 0.069 1.000 . Uiso c ? H(9) 0.9128 0.4556 0.6545 0.069 1.000 . Uiso c ? H(10) 0.7741 0.4948 0.6476 0.069 1.000 . Uiso c ? H(11) 0.7718 0.0485 1.0077 0.062 1.000 . Uiso c ? H(12) 0.9051 0.0851 1.2194 0.068 1.000 . Uiso c ? H(13) 1.0973 0.2055 1.2745 0.070 1.000 . Uiso c ? H(14) 1.1542 0.2914 1.1191 0.062 1.000 . Uiso c ? H(15) 0.5631 -0.1072 0.0765 0.066 1.000 . Uiso c ? H(16) 0.5986 0.0258 0.1308 0.066 1.000 . Uiso c ? H(17) 0.7105 -0.0025 0.7652 0.052 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0428(3) 0.0366(2) 0.0337(2) -0.0010(2) 0.0049(2) 0.0095(2) Cu(2) 0.0431(3) 0.0484(3) 0.0474(3) -0.0020(2) 0.0048(2) 0.0167(2) O(1) 0.058(2) 0.063(2) 0.066(2) 0.010(2) 0.019(2) 0.029(2) O(2) 0.080(2) 0.074(2) 0.085(3) 0.026(2) 0.023(2) 0.035(2) O(3) 0.069(2) 0.132(3) 0.056(2) 0.019(2) 0.023(2) 0.015(2) O(4) 0.050(2) 0.086(2) 0.079(2) -0.011(2) -0.003(2) 0.040(2) O(5) 0.070(3) 0.063(2) 0.128(3) 0.008(2) -0.001(2) -0.002(2) O(6) 0.083(3) 0.105(3) 0.093(3) -0.046(2) -0.005(2) 0.019(2) O(7) 0.084(2) 0.051(2) 0.064(2) -0.016(2) 0.015(2) 0.022(2) O(8) 0.124(3) 0.048(2) 0.064(2) 0.011(2) 0.021(2) 0.013(2) O(9) 0.091(2) 0.089(2) 0.045(2) -0.039(2) 0.007(2) 0.023(2) N(1) 0.042(2) 0.039(2) 0.036(2) 0.001(1) 0.005(1) 0.010(1) N(2) 0.077(3) 0.048(2) 0.035(2) -0.005(2) 0.002(2) 0.013(2) N(3) 0.046(2) 0.038(2) 0.038(2) 0.004(1) 0.006(1) 0.013(1) N(4) 0.049(2) 0.042(2) 0.046(2) 0.002(2) 0.005(2) 0.019(2) N(5) 0.038(2) 0.035(2) 0.037(2) -0.001(1) 0.004(1) 0.007(1) N(6) 0.039(2) 0.038(2) 0.034(2) 0.002(1) 0.003(1) 0.009(1) N(7) 0.049(2) 0.044(2) 0.034(2) -0.006(1) 0.010(1) 0.011(1) N(8) 0.045(2) 0.038(2) 0.038(2) -0.001(1) 0.002(1) 0.008(1) N(9) 0.041(2) 0.082(3) 0.056(2) 0.010(2) 0.012(2) 0.018(2) N(10) 0.061(3) 0.068(3) 0.057(2) -0.019(2) 0.005(2) 0.005(2) N(11) 0.059(2) 0.043(2) 0.042(2) -0.005(2) -0.003(2) 0.019(2) C(1) 0.049(2) 0.050(2) 0.036(2) -0.002(2) 0.005(2) 0.016(2) C(2) 0.056(3) 0.041(2) 0.055(3) -0.005(2) 0.007(2) 0.021(2) C(3) 0.061(3) 0.045(2) 0.048(2) -0.011(2) 0.001(2) 0.006(2) C(4) 0.055(3) 0.049(2) 0.035(2) -0.001(2) 0.002(2) 0.008(2) C(5) 0.036(2) 0.041(2) 0.033(2) 0.002(2) 0.007(2) 0.009(2) C(6) 0.039(2) 0.048(2) 0.036(2) 0.006(2) 0.005(2) 0.013(2) C(7) 0.048(2) 0.041(2) 0.052(2) 0.006(2) 0.007(2) 0.020(2) C(8) 0.086(4) 0.054(3) 0.063(3) -0.007(2) -0.002(3) 0.030(2) C(9) 0.037(2) 0.036(2) 0.052(2) 0.004(2) 0.008(2) 0.012(2) C(10) 0.072(3) 0.033(2) 0.060(3) 0.000(2) -0.002(2) 0.012(2) C(11) 0.042(2) 0.037(2) 0.032(2) 0.004(2) 0.013(2) 0.007(2) C(12) 0.042(2) 0.034(2) 0.038(2) 0.002(2) 0.006(2) 0.005(2) C(13) 0.054(3) 0.054(2) 0.043(2) -0.005(2) 0.013(2) 0.012(2) C(14) 0.071(3) 0.059(3) 0.042(2) 0.010(2) 0.016(2) 0.021(2) C(15) 0.063(3) 0.059(3) 0.047(2) 0.008(2) 0.000(2) 0.017(2) C(16) 0.052(3) 0.042(2) 0.051(3) 0.003(2) -0.003(2) 0.009(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3369 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_all 0.0490 _refine_ls_wR_factor_ref 0.0430 _refine_ls_goodness_of_fit_all 1.419 _refine_ls_goodness_of_fit_ref 1.620 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.44 _refine_diff_density_max 0.00 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 1.990(4) . . ? Cu(1) N(3) 1.905(4) . . ? Cu(1) N(5) 1.958(4) . . ? Cu(1) N(7) 1.934(4) . . ? Cu(2) O(1) 2.021(4) . . ? Cu(2) O(4) 1.971(4) . . ? Cu(2) N(6) 1.974(4) . . ? Cu(2) N(8) 1.977(4) . . ? O(1) N(9) 1.303(5) . . ? O(2) N(9) 1.227(6) . . ? O(3) N(9) 1.217(5) . . ? O(4) N(10) 1.301(6) . . ? O(5) N(10) 1.216(6) . . ? O(6) N(10) 1.213(6) . . ? O(7) N(11) 1.236(5) . . ? O(8) N(11) 1.224(5) . . ? O(9) N(11) 1.241(5) . . ? N(1) C(1) 1.328(6) . . ? N(1) C(5) 1.352(5) . . ? N(2) C(6) 1.296(5) . . ? N(2) H(15) 0.75 . . no N(2) H(16) 0.88 . . no N(3) N(4) 1.374(5) . . ? N(3) C(6) 1.329(5) . . ? N(4) C(7) 1.291(6) . . ? N(5) N(6) 1.392(5) . . ? N(5) C(9) 1.294(6) . . ? N(6) C(11) 1.345(5) . . ? N(7) C(11) 1.292(5) . . ? N(7) H(17) 0.76 . . no N(8) C(12) 1.334(5) . . ? N(8) C(16) 1.349(6) . . ? C(1) C(2) 1.375(6) . . ? C(1) H(1) 0.95 . . no C(2) C(3) 1.365(7) . . ? C(2) H(2) 0.95 . . no C(3) C(4) 1.368(7) . . ? C(3) H(3) 0.95 . . no C(4) C(5) 1.380(6) . . ? C(4) H(4) 0.94 . . no C(5) C(6) 1.486(6) . . ? C(7) C(8) 1.506(7) . . ? C(7) C(9) 1.499(7) . . ? C(8) H(5) 0.95 . . no C(8) H(6) 0.95 . . no C(8) H(7) 0.95 . . no C(9) C(10) 1.498(6) . . ? C(10) H(8) 0.95 . . no C(10) H(9) 0.95 . . no C(10) H(10) 0.95 . . no C(11) C(12) 1.485(6) . . ? C(12) C(13) 1.386(6) . . ? C(13) C(14) 1.389(7) . . ? C(13) H(11) 0.95 . . no C(14) C(15) 1.368(7) . . ? C(14) H(12) 0.94 . . no C(15) C(16) 1.380(7) . . ? C(15) H(13) 0.95 . . no C(16) H(14) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(3) 82.3(2) . . . ? N(1) Cu(1) N(5) 170.8(2) . . . ? N(1) Cu(1) N(7) 106.7(2) . . . ? N(3) Cu(1) N(5) 90.3(2) . . . ? N(3) Cu(1) N(7) 168.7(2) . . . ? N(5) Cu(1) N(7) 81.4(2) . . . ? O(1) Cu(2) O(4) 92.5(2) . . . ? O(1) Cu(2) N(6) 93.6(2) . . . ? O(1) Cu(2) N(8) 157.8(2) . . . ? O(4) Cu(2) N(6) 171.5(2) . . . ? O(4) Cu(2) N(8) 95.3(2) . . . ? N(6) Cu(2) N(8) 81.2(2) . . . ? Cu(2) O(1) N(9) 103.2(3) . . . ? Cu(2) O(4) N(10) 103.0(3) . . . ? Cu(1) N(1) C(1) 128.0(3) . . . ? Cu(1) N(1) C(5) 113.0(3) . . . ? C(1) N(1) C(5) 118.6(4) . . . ? C(6) N(2) H(15) 127.1 . . . no C(6) N(2) H(16) 115.1 . . . no H(15) N(2) H(16) 117.5 . . . no Cu(1) N(3) N(4) 130.5(3) . . . ? Cu(1) N(3) C(6) 116.1(3) . . . ? N(4) N(3) C(6) 112.4(4) . . . ? N(3) N(4) C(7) 120.6(4) . . . ? Cu(1) N(5) N(6) 112.3(3) . . . ? Cu(1) N(5) C(9) 127.6(3) . . . ? N(6) N(5) C(9) 119.1(4) . . . ? Cu(2) N(6) N(5) 124.9(3) . . . ? Cu(2) N(6) C(11) 111.3(3) . . . ? N(5) N(6) C(11) 111.0(4) . . . ? Cu(1) N(7) C(11) 111.0(3) . . . ? Cu(1) N(7) H(17) 129.0 . . . no C(11) N(7) H(17) 117.8 . . . no Cu(2) N(8) C(12) 113.7(3) . . . ? Cu(2) N(8) C(16) 127.0(3) . . . ? C(12) N(8) C(16) 119.3(4) . . . ? O(1) N(9) O(2) 117.6(5) . . . ? O(1) N(9) O(3) 119.7(6) . . . ? O(2) N(9) O(3) 122.6(6) . . . ? O(4) N(10) O(5) 116.7(5) . . . ? O(4) N(10) O(6) 117.9(6) . . . ? O(5) N(10) O(6) 125.4(6) . . . ? O(7) N(11) O(8) 120.2(5) . . . ? O(7) N(11) O(9) 118.8(4) . . . ? O(8) N(11) O(9) 121.0(4) . . . ? N(1) C(1) C(2) 121.8(4) . . . ? N(1) C(1) H(1) 119.1 . . . no C(2) C(1) H(1) 119.1 . . . no C(1) C(2) C(3) 119.8(5) . . . ? C(1) C(2) H(2) 120.3 . . . no C(3) C(2) H(2) 119.9 . . . no C(2) C(3) C(4) 119.2(5) . . . ? C(2) C(3) H(3) 120.5 . . . no C(4) C(3) H(3) 120.4 . . . no C(3) C(4) C(5) 118.9(5) . . . ? C(3) C(4) H(4) 120.3 . . . no C(5) C(4) H(4) 120.9 . . . no N(1) C(5) C(4) 121.8(4) . . . ? N(1) C(5) C(6) 113.2(4) . . . ? C(4) C(5) C(6) 125.0(4) . . . ? N(2) C(6) N(3) 124.2(5) . . . ? N(2) C(6) C(5) 121.6(4) . . . ? N(3) C(6) C(5) 114.2(4) . . . ? N(4) C(7) C(8) 114.7(5) . . . ? N(4) C(7) C(9) 128.4(4) . . . ? C(8) C(7) C(9) 116.9(4) . . . ? C(7) C(8) H(5) 109.5 . . . no C(7) C(8) H(6) 109.5 . . . no C(7) C(8) H(7) 109.5 . . . no H(5) C(8) H(6) 109.5 . . . no H(5) C(8) H(7) 109.5 . . . no H(6) C(8) H(7) 109.4 . . . no N(5) C(9) C(7) 120.0(4) . . . ? N(5) C(9) C(10) 121.8(5) . . . ? C(7) C(9) C(10) 118.2(4) . . . ? C(9) C(10) H(8) 109.4 . . . no C(9) C(10) H(9) 109.5 . . . no C(9) C(10) H(10) 109.6 . . . no H(8) C(10) H(9) 109.4 . . . no H(8) C(10) H(10) 109.5 . . . no H(9) C(10) H(10) 109.6 . . . no N(6) C(11) N(7) 122.0(4) . . . ? N(6) C(11) C(12) 112.4(4) . . . ? N(7) C(11) C(12) 125.7(4) . . . ? N(8) C(12) C(11) 113.7(4) . . . ? N(8) C(12) C(13) 122.0(5) . . . ? C(11) C(12) C(13) 124.3(4) . . . ? C(12) C(13) C(14) 118.1(5) . . . ? C(12) C(13) H(11) 121.4 . . . no C(14) C(13) H(11) 120.5 . . . no C(13) C(14) C(15) 120.1(5) . . . ? C(13) C(14) H(12) 120.3 . . . no C(15) C(14) H(12) 119.6 . . . no C(14) C(15) C(16) 118.7(5) . . . ? C(14) C(15) H(13) 120.6 . . . no C(16) C(15) H(13) 120.7 . . . no N(8) C(16) C(15) 121.8(5) . . . ? N(8) C(16) H(14) 119.2 . . . no C(15) C(16) H(14) 119.0 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu(1) O(3) 2.641(4) . 2_756 no Cu(1) N(9) 3.280(5) . 2_756 no Cu(1) O(2) 3.308(4) . 2_756 no Cu(1) N(1) 3.335(4) . 2_656 no Cu(1) C(5) 3.544(4) . 2_656 no Cu(2) O(5) 3.468(5) . 2_767 no O(2) N(3) 3.100(5) . 2_756 no O(2) C(6) 3.134(6) . 2_756 no O(2) O(3) 3.170(6) . 2_756 no O(2) C(5) 3.396(6) . 2_756 no O(2) N(1) 3.534(6) . 2_756 no O(2) C(14) 3.539(7) . 2_757 no O(2) N(9) 3.565(6) . 2_756 no O(3) N(1) 2.964(6) . 2_756 no O(3) N(7) 3.058(5) . 2_756 no O(3) C(1) 3.362(7) . 2_756 no O(3) C(15) 3.384(7) . 1_554 no O(3) C(11) 3.476(6) . 2_756 no O(3) N(5) 3.521(6) . 2_756 no O(4) C(4) 3.419(7) . 2_756 no O(5) N(8) 2.979(6) . 2_767 no O(5) C(16) 3.228(7) . 2_767 no O(5) C(12) 3.409(6) . 2_767 no O(5) O(5) 3.41(1) . 2_767 no O(6) C(4) 3.174(7) . 1_666 no O(6) C(3) 3.207(7) . 1_666 no O(6) O(9) 3.405(6) . 1_665 no O(6) C(3) 3.533(7) . 2_756 no O(6) N(6) 3.599(6) . 2_767 no O(7) N(7) 3.009(5) . . no O(7) N(2) 3.085(5) . 1_556 no O(7) N(2) 3.133(6) . 2_656 no O(7) C(16) 3.357(7) . 2_757 no O(7) C(13) 3.359(6) . . no O(7) N(4) 3.508(6) . 2_656 no O(7) C(1) 3.571(6) . . no O(7) C(6) 3.583(6) . 2_656 no O(8) C(1) 3.167(6) . . no O(8) C(2) 3.253(6) . 2_646 no O(8) C(3) 3.329(7) . 2_646 no O(8) C(2) 3.397(7) . . no O(8) C(10) 3.441(7) . 1_545 no O(9) N(2) 2.858(5) . 1_556 no O(9) C(4) 3.338(6) . 1_556 no O(9) N(4) 3.404(6) . 2_656 no O(9) C(8) 3.531(7) . 2_656 no N(1) N(9) 3.288(6) . 2_756 no N(1) N(3) 3.534(5) . 2_656 no N(2) N(11) 3.371(6) . 1_554 no N(3) C(1) 3.339(6) . 2_656 no N(4) N(11) 3.316(6) . 2_656 no N(4) C(14) 3.527(7) . 1_554 no N(4) C(1) 3.550(6) . 2_656 no N(7) C(5) 3.470(6) . 2_656 no N(7) C(6) 3.533(6) . 2_656 no N(9) C(5) 3.502(6) . 2_756 no C(2) C(9) 3.504(7) . 2_656 no C(10) C(16) 3.544(7) . 2_767 no C(12) C(14) 3.533(7) . 2_757 no C(13) C(15) 3.559(7) . 2_757 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cu(1) N(1) C(1) C(2) . . . . -171.1(4) no Cu(1) N(1) C(5) C(4) . . . . 172.2(4) no Cu(1) N(1) C(5) C(6) . . . . -7.3(5) no Cu(1) N(3) N(4) C(7) . . . . -5.1(6) no Cu(1) N(3) C(6) N(2) . . . . -171.7(4) no Cu(1) N(3) C(6) C(5) . . . . 8.5(5) no Cu(1) N(5) N(6) Cu(2) . . . . 130.3(2) no Cu(1) N(5) N(6) C(11) . . . . -7.6(4) no Cu(1) N(5) C(9) C(7) . . . . -20.4(6) no Cu(1) N(5) C(9) C(10) . . . . 159.4(4) no Cu(1) N(7) C(11) N(6) . . . . 14.5(5) no Cu(1) N(7) C(11) C(12) . . . . -164.1(3) no Cu(2) O(1) N(9) O(2) . . . . -4.9(5) no Cu(2) O(1) N(9) O(3) . . . . 176.0(4) no Cu(2) O(4) N(10) O(5) . . . . 6.6(6) no Cu(2) O(4) N(10) O(6) . . . . -174.3(4) no Cu(2) N(6) N(5) C(9) . . . . -60.3(5) no Cu(2) N(6) C(11) N(7) . . . . -148.5(4) no Cu(2) N(6) C(11) C(12) . . . . 30.3(4) no Cu(2) N(8) C(12) C(11) . . . . 0.2(5) no Cu(2) N(8) C(12) C(13) . . . . 179.2(4) no Cu(2) N(8) C(16) C(15) . . . . -179.3(4) no O(1) Cu(2) O(4) N(10) . . . . 76.1(3) no O(1) Cu(2) N(6) N(5) . . . . -3.5(3) no O(1) Cu(2) N(6) C(11) . . . . 134.3(3) no O(1) Cu(2) N(8) C(12) . . . . -65.0(6) no O(1) Cu(2) N(8) C(16) . . . . 114.3(5) no O(4) Cu(2) O(1) N(9) . . . . 94.0(3) no O(4) Cu(2) N(6) N(5) . . . . 132(1) no O(4) Cu(2) N(6) C(11) . . . . -90(1) no O(4) Cu(2) N(8) C(12) . . . . -175.2(3) no O(4) Cu(2) N(8) C(16) . . . . 4.1(4) no N(1) Cu(1) N(3) N(4) . . . . -177.3(4) no N(1) Cu(1) N(3) C(6) . . . . -9.9(3) no N(1) Cu(1) N(5) N(6) . . . . -139.3(9) no N(1) Cu(1) N(5) C(9) . . . . 52(1) no N(1) Cu(1) N(7) C(11) . . . . 161.5(3) no N(1) C(1) C(2) C(3) . . . . 0.1(8) no N(1) C(5) C(4) C(3) . . . . 0.2(8) no N(1) C(5) C(6) N(2) . . . . 179.8(4) no N(1) C(5) C(6) N(3) . . . . -0.4(6) no N(2) C(6) N(3) N(4) . . . . -2.1(7) no N(2) C(6) C(5) C(4) . . . . 0.3(8) no N(3) Cu(1) N(1) C(1) . . . . -178.5(4) no N(3) Cu(1) N(1) C(5) . . . . 9.4(3) no N(3) Cu(1) N(5) N(6) . . . . -175.9(3) no N(3) Cu(1) N(5) C(9) . . . . 15.8(4) no N(3) Cu(1) N(7) C(11) . . . . -57(1) no N(3) N(4) C(7) C(8) . . . . -179.0(4) no N(3) N(4) C(7) C(9) . . . . 3.8(8) no N(3) C(6) C(5) C(4) . . . . -179.9(5) no N(4) N(3) Cu(1) N(5) . . . . -2.8(4) no N(4) N(3) Cu(1) N(7) . . . . 39(1) no N(4) N(3) C(6) C(5) . . . . 178.2(4) no N(4) C(7) C(9) N(5) . . . . 9.3(8) no N(4) C(7) C(9) C(10) . . . . -170.5(5) no N(5) Cu(1) N(1) C(1) . . . . 144.5(9) no N(5) Cu(1) N(1) C(5) . . . . -28(1) no N(5) Cu(1) N(3) C(6) . . . . 164.5(3) no N(5) Cu(1) N(7) C(11) . . . . -13.8(3) no N(5) N(6) Cu(2) N(8) . . . . -161.8(4) no N(5) N(6) C(11) N(7) . . . . -4.6(6) no N(5) N(6) C(11) C(12) . . . . 174.1(3) no N(5) C(9) C(7) C(8) . . . . -167.9(5) no N(6) Cu(2) O(1) N(9) . . . . -91.9(3) no N(6) Cu(2) O(4) N(10) . . . . -60(1) no N(6) Cu(2) N(8) C(12) . . . . 12.6(3) no N(6) Cu(2) N(8) C(16) . . . . -168.1(4) no N(6) N(5) Cu(1) N(7) . . . . 11.8(3) no N(6) N(5) C(9) C(7) . . . . 172.0(4) no N(6) N(5) C(9) C(10) . . . . -8.2(7) no N(6) C(11) C(12) N(8) . . . . -20.4(6) no N(6) C(11) C(12) C(13) . . . . 160.6(4) no N(7) Cu(1) N(1) C(1) . . . . -5.5(4) no N(7) Cu(1) N(1) C(5) . . . . -177.6(3) no N(7) Cu(1) N(3) C(6) . . . . -153.2(7) no N(7) Cu(1) N(5) C(9) . . . . -156.5(4) no N(7) C(11) C(12) N(8) . . . . 158.3(4) no N(7) C(11) C(12) C(13) . . . . -20.7(7) no N(8) Cu(2) O(1) N(9) . . . . -16.7(6) no N(8) Cu(2) O(4) N(10) . . . . -124.7(3) no N(8) Cu(2) N(6) C(11) . . . . -24.0(3) no N(8) C(12) C(13) C(14) . . . . 0.3(7) no N(8) C(16) C(15) C(14) . . . . -0.0(8) no C(1) N(1) C(5) C(4) . . . . -0.7(7) no C(1) N(1) C(5) C(6) . . . . 179.7(4) no C(1) C(2) C(3) C(4) . . . . -0.7(8) no C(2) C(1) N(1) C(5) . . . . 0.6(7) no C(2) C(3) C(4) C(5) . . . . 0.5(8) no C(3) C(4) C(5) C(6) . . . . 179.6(5) no C(6) N(3) N(4) C(7) . . . . -172.8(4) no C(8) C(7) C(9) C(10) . . . . 12.3(7) no C(9) N(5) N(6) C(11) . . . . 161.8(4) no C(11) C(12) N(8) C(16) . . . . -179.1(4) no C(11) C(12) C(13) C(14) . . . . 179.2(4) no C(12) N(8) C(16) C(15) . . . . 0.0(7) no C(12) C(13) C(14) C(15) . . . . -0.3(8) no C(13) C(12) N(8) C(16) . . . . -0.2(7) no C(13) C(14) C(15) C(16) . . . . 0.2(8) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================