# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2296 data_hphpepcu _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(S)-3-(Imidazol-4-yl)-2-[(6-{[(S)-2-(imidazol-4-yl)-1- methoxycarbonylethylimino]carbonyl}pyridine- 2-carbonyl)imino]propionic acid methyl ester]Copper(II) Dihydrate ; _chemical_name_common hphpepcu _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 Cu N7 O5, 2(H2 O)' _chemical_formula_sum 'C21 H25 Cu N7 O8' _chemical_formula_weight 567.0 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P43212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 16.854(5) _cell_length_b 16.854(5) _cell_length_c 19.824(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5631(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 14.2 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 1.626 _exptl_absorpt_correction_type ?f-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details ? _exptl_special_details ; none ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK?a _diffrn_radiation_source 'Rigaku RU200' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method 2?q-?w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.001 _diffrn_reflns_number 2548 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0030 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 62.22 _reflns_number_total 2548 _reflns_number_gt 2375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Control Software' _computing_cell_refinement 'MSC/AFC Control Software' _computing_data_reduction 'MSC/AFC Control Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1574P)^2^+7.3531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^?l^3^/sin(2?q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.16(9) _refine_ls_number_reflns 2548 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2162 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.30118(7) 0.02946(6) 0.24703(6) 0.0444(5) Uani 1 1 d . . . N1 N 0.2647(4) -0.0619(4) 0.1974(3) 0.0431(14) Uani 1 1 d . . . C2 C 0.2949(5) -0.1337(4) 0.2130(4) 0.0439(17) Uani 1 1 d . . . C3 C 0.2684(5) -0.2004(5) 0.1808(4) 0.0493(19) Uani 1 1 d . . . H3 H 0.2884 -0.2501 0.1920 0.059 Uiso 1 1 calc R . . C4 C 0.2110(6) -0.1921(5) 0.1313(4) 0.059(2) Uani 1 1 d . . . H4 H 0.1917 -0.2368 0.1093 0.071 Uiso 1 1 calc R . . C5 C 0.1827(6) -0.1187(6) 0.1144(4) 0.058(2) Uani 1 1 d . . . H5 H 0.1445 -0.1132 0.0809 0.069 Uiso 1 1 calc R . . C6 C 0.2121(5) -0.0517(5) 0.1485(4) 0.0464(18) Uani 1 1 d . . . C7 C 0.3555(5) -0.1289(4) 0.2682(4) 0.0409(16) Uani 1 1 d . . . O7 O 0.3911(4) -0.1900(3) 0.2861(3) 0.0575(15) Uani 1 1 d . . . N8 N 0.3640(4) -0.0560(4) 0.2925(3) 0.0461(15) Uani 1 1 d . . . C9 C 0.4275(5) -0.0464(5) 0.3434(4) 0.0475(18) Uani 1 1 d . . . H9 H 0.4778 -0.0648 0.3242 0.057 Uiso 1 1 calc R . . C9A C 0.4111(5) -0.0909(5) 0.4054(4) 0.0494(19) Uani 1 1 d . . . O9B O 0.3474(4) -0.1076(4) 0.4290(3) 0.0632(17) Uani 1 1 d . . . O9C C 0.4790(4) -0.1094(5) 0.4380(4) 0.0422(17) Uani 1 1 d . . . C9D C 0.4738(6) -0.1494(8) 0.5013(5) 0.079(3) Uani 1 1 d . . . H91 H 0.4580 -0.1125 0.5356 0.119 Uiso 1 1 calc R . . H92 H 0.5246 -0.1714 0.5126 0.119 Uiso 1 1 calc R . . H93 H 0.4353 -0.1913 0.4983 0.119 Uiso 1 1 calc R . . C10 C 0.4350(5) 0.0421(5) 0.3620(4) 0.0509(19) Uani 1 1 d . . . H11 H 0.3868 0.0587 0.3847 0.061 Uiso 1 1 calc R . . H12 H 0.4785 0.0483 0.3936 0.061 Uiso 1 1 calc R . . C11 C 0.4491(5) 0.0961(5) 0.3025(5) 0.052(2) Uani 1 1 d . . . N12 N 0.3968(4) 0.1023(4) 0.2503(4) 0.0502(15) Uani 1 1 d . . . C13 C 0.4243(6) 0.1588(6) 0.2109(5) 0.062(2) Uani 1 1 d . . . H13 H 0.3986 0.1772 0.1725 0.074 Uiso 1 1 calc R . . N14 N 0.4951(5) 0.1868(5) 0.2335(5) 0.073(2) Uani 1 1 d . . . H14 H 0.5234 0.2232 0.2148 0.087 Uiso 1 1 calc R . . C15 C 0.5130(6) 0.1468(6) 0.2908(6) 0.064(2) Uani 1 1 d . . . H15 H 0.5585 0.1521 0.3169 0.077 Uiso 1 1 calc R . . C7' C 0.1881(6) 0.0322(6) 0.1396(4) 0.054(2) Uani 1 1 d . . . O7' O 0.1355(5) 0.0491(4) 0.0963(3) 0.0725(19) Uani 1 1 d . . . N8' N 0.2237(5) 0.0800(4) 0.1817(3) 0.0513(17) Uani 1 1 d . . . C9' C 0.1932(6) 0.1614(5) 0.1850(4) 0.055(2) Uani 1 1 d . . . H9' H 0.1354 0.1592 0.1799 0.065 Uiso 1 1 calc R . . C9A' C 0.2249(7) 0.2120(5) 0.1302(5) 0.063(2) Uani 1 1 d . . . O9B' O 0.2823(6) 0.1992(5) 0.0954(4) 0.091(3) Uani 1 1 d . . . O9C' O 0.1822(6) 0.2795(4) 0.1245(4) 0.090(3) Uani 1 1 d . . . C9D' C 0.2065(11) 0.3341(7) 0.0749(6) 0.098(5) Uani 1 1 d . . . H94 H 0.2633 0.3342 0.0721 0.148 Uiso 1 1 calc R . . H95 H 0.1882 0.3862 0.0868 0.148 Uiso 1 1 calc R . . H96 H 0.1845 0.3191 0.0321 0.148 Uiso 1 1 calc R . . C10' C 0.2116(6) 0.1981(5) 0.2544(4) 0.058(2) Uani 1 1 d . . . H1A H 0.2681 0.2089 0.2573 0.070 Uiso 1 1 calc R . . H1B H 0.1839 0.2483 0.2584 0.070 Uiso 1 1 calc R . . C11' C 0.1885(6) 0.1466(5) 0.3109(4) 0.0506(19) Uani 1 1 d . . . N12' N 0.2289(4) 0.0765(4) 0.3248(3) 0.0510(17) Uani 1 1 d . . . C13' C 0.1969(6) 0.0442(6) 0.3762(5) 0.063(2) Uani 1 1 d . . . H13' H 0.2130 -0.0032 0.3960 0.076 Uiso 1 1 calc R . . N14' C 0.1341(6) 0.0911(6) 0.3979(4) 0.057(2) Uani 1 1 d . . . H14' H 0.1015 0.0806 0.4347 0.068 Uiso 1 1 calc R . . C15' C 0.1285(6) 0.1532(7) 0.3573(5) 0.071(3) Uani 1 1 d . . . H15' H 0.0910 0.1936 0.3597 0.085 Uiso 1 1 calc R . . O1W O 0.2508(8) -0.0405(6) 0.5395(6) 0.131(5) Uani 1 1 d . . . H1W H 0.2756 0.0029 0.5390 0.197 Uiso 1 1 d . . . H2W H 0.2796 -0.0509 0.5045 0.197 Uiso 1 1 d . . . O2W O 0.1551(9) 0.0313(11) -0.0457(7) 0.189(8) Uani 1 1 d . . . H3W H 0.1162 0.0592 -0.0635 0.284 Uiso 1 1 d . . . H4W H 0.1464 0.0350 -0.0060 0.284 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 Cu 0.0503(7) 0.0323(6) 0.0507(7) -0.0022(5) -0.0062(5) 0.0034(5) N1 0.054(4) 0.033(3) 0.041(3) -0.002(3) -0.001(3) -0.002(3) C2 0.049(4) 0.034(4) 0.048(4) 0.006(3) 0.013(3) -0.001(3) C3 0.064(5) 0.037(4) 0.047(4) -0.004(3) 0.003(4) 0.005(4) C4 0.077(6) 0.046(5) 0.054(4) -0.016(4) 0.008(4) -0.011(4) C5 0.065(6) 0.053(5) 0.056(5) -0.010(4) -0.013(4) -0.006(4) C6 0.046(4) 0.048(4) 0.045(4) -0.002(3) 0.001(3) -0.002(3) C7 0.044(4) 0.032(4) 0.047(4) 0.003(3) 0.007(3) 0.002(3) O7 0.062(4) 0.036(3) 0.074(4) -0.002(3) -0.007(3) 0.005(3) N8 0.044(3) 0.042(3) 0.052(3) -0.001(3) -0.003(3) 0.003(3) C9 0.037(4) 0.041(4) 0.065(5) -0.002(4) -0.006(4) 0.000(3) C9A 0.044(5) 0.051(5) 0.054(4) -0.005(4) -0.008(4) -0.001(4) O9B 0.052(4) 0.072(4) 0.065(4) 0.001(3) -0.003(3) -0.006(3) O9C 0.021(3) 0.057(5) 0.048(4) 0.021(3) -0.011(3) -0.002(3) C9D 0.056(6) 0.106(9) 0.075(6) 0.030(7) -0.023(5) -0.010(5) C10 0.050(5) 0.049(5) 0.054(4) -0.009(4) -0.011(4) -0.003(4) C11 0.052(5) 0.034(4) 0.069(5) -0.004(4) -0.001(4) -0.006(3) N12 0.056(4) 0.036(3) 0.059(3) 0.003(3) -0.001(3) -0.006(3) C13 0.076(6) 0.046(5) 0.063(5) 0.006(4) -0.001(5) 0.001(4) N14 0.056(5) 0.057(5) 0.104(6) 0.013(5) 0.001(5) -0.013(4) C15 0.053(5) 0.048(5) 0.091(6) -0.001(5) -0.001(5) -0.013(4) C7' 0.053(5) 0.055(5) 0.053(4) 0.002(4) -0.008(4) 0.010(4) O7' 0.085(5) 0.062(4) 0.070(4) 0.002(3) -0.021(4) 0.012(4) N8' 0.061(4) 0.041(4) 0.051(3) -0.006(3) -0.008(3) 0.008(3) C9' 0.072(6) 0.037(4) 0.055(4) -0.004(3) -0.009(4) 0.015(4) C9A' 0.090(7) 0.042(5) 0.056(5) 0.000(4) -0.017(5) 0.016(4) O9B' 0.108(6) 0.077(5) 0.086(5) 0.021(4) 0.033(5) 0.034(5) O9C' 0.143(8) 0.046(4) 0.081(4) 0.013(4) 0.013(5) 0.035(5) C9D' 0.164(14) 0.054(6) 0.077(7) 0.014(5) -0.005(8) 0.031(8) C10' 0.062(5) 0.044(4) 0.068(5) -0.005(4) -0.008(5) 0.014(4) C11' 0.056(5) 0.044(4) 0.051(4) -0.003(4) -0.006(4) 0.004(4) N12' 0.056(4) 0.043(4) 0.054(4) -0.005(3) 0.002(3) 0.002(3) C13' 0.067(6) 0.063(5) 0.060(5) 0.006(4) 0.004(5) 0.000(5) N14' 0.058(5) 0.080(6) 0.034(4) 0.005(4) 0.011(4) 0.007(5) C15' 0.054(5) 0.084(7) 0.075(6) -0.027(6) -0.001(5) 0.022(5) O1W 0.170(12) 0.084(6) 0.140(8) -0.013(6) 0.069(9) -0.034(7) O2W 0.153(11) 0.257(19) 0.158(10) 0.053(12) -0.027(10) 0.116(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 1.929(6) . ? Cu N8 2.002(7) . ? Cu N12 2.027(7) . ? Cu N8' 2.027(7) . ? Cu N12' 2.119(7) . ? N1 C6 1.324(10) . ? N1 C2 1.349(10) . ? C2 C3 1.367(12) . ? C2 C7 1.498(11) . ? C3 C4 1.385(13) . ? C4 C5 1.368(14) . ? C5 C6 1.407(12) . ? C6 C7' 1.481(13) . ? C7 O7 1.244(9) . ? C7 N8 1.328(10) . ? N8 C9 1.479(10) . ? C9 C9A 1.466(12) . ? C9 C10 1.542(12) . ? C9A O9B 1.204(11) . ? C9A O9C 1.351(11) . ? O9C C9D 1.428(13) . ? C10 C11 1.509(12) . ? C11 N12 1.363(11) . ? C11 C15 1.395(13) . ? N12 C13 1.316(12) . ? C13 N14 1.359(13) . ? N14 C15 1.354(14) . ? C7' O7' 1.266(11) . ? C7' N8' 1.305(12) . ? N8' C9' 1.467(10) . ? C9' C9A' 1.480(14) . ? C9' C10' 1.540(12) . ? C9A' O9B' 1.207(13) . ? C9A' O9C' 1.352(12) . ? O9C' C9D' 1.406(14) . ? C10' C11' 1.469(13) . ? C11' C15' 1.372(13) . ? C11' N12' 1.391(11) . ? N12' C13' 1.274(12) . ? C13' N14' 1.390(14) . ? N14' C15' 1.324(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu N8 79.9(3) . . ? N1 Cu N12 138.9(3) . . ? N8 Cu N12 90.0(3) . . ? N1 Cu N8' 78.7(3) . . ? N8 Cu N8' 158.6(3) . . ? N12 Cu N8' 106.2(3) . . ? N1 Cu N12' 119.2(3) . . ? N8 Cu N12' 104.2(3) . . ? N12 Cu N12' 101.9(3) . . ? N8' Cu N12' 86.4(3) . . ? C6 N1 C2 122.6(7) . . ? C6 N1 Cu 118.8(5) . . ? C2 N1 Cu 118.6(5) . . ? N1 C2 C3 120.4(7) . . ? N1 C2 C7 112.1(7) . . ? C3 C2 C7 127.5(7) . . ? C2 C3 C4 118.5(8) . . ? C5 C4 C3 120.5(8) . . ? C4 C5 C6 119.1(8) . . ? N1 C6 C5 118.8(8) . . ? N1 C6 C7' 113.3(7) . . ? C5 C6 C7' 127.8(8) . . ? O7 C7 N8 127.7(7) . . ? O7 C7 C2 119.5(7) . . ? N8 C7 C2 112.9(6) . . ? C7 N8 C9 115.2(6) . . ? C7 N8 Cu 116.4(5) . . ? C9 N8 Cu 127.7(5) . . ? C9A C9 N8 112.3(7) . . ? C9A C9 C10 108.0(7) . . ? N8 C9 C10 109.1(6) . . ? O9B C9A O9C 121.0(8) . . ? O9B C9A C9 127.9(8) . . ? O9C C9A C9 111.0(7) . . ? C9A O9C C9D 118.5(8) . . ? C11 C10 C9 114.2(7) . . ? N12 C11 C15 109.0(8) . . ? N12 C11 C10 122.5(7) . . ? C15 C11 C10 128.4(9) . . ? C13 N12 C11 106.1(8) . . ? C13 N12 Cu 134.4(7) . . ? C11 N12 Cu 119.5(5) . . ? N12 C13 N14 111.5(9) . . ? C15 N14 C13 107.4(8) . . ? N14 C15 C11 105.8(9) . . ? O7' C7' N8' 128.0(9) . . ? O7' C7' C6 119.1(8) . . ? N8' C7' C6 112.8(7) . . ? C7' N8' C9' 116.4(7) . . ? C7' N8' Cu 116.4(6) . . ? C9' N8' Cu 126.2(5) . . ? N8' C9' C9A' 112.3(8) . . ? N8' C9' C10' 110.1(7) . . ? C9A' C9' C10' 110.6(7) . . ? O9B' C9A' O9C' 121.9(10) . . ? O9B' C9A' C9' 127.3(9) . . ? O9C' C9A' C9' 110.8(9) . . ? C9A' O9C' C9D' 117.0(10) . . ? C11' C10' C9' 113.0(7) . . ? C15' C11' N12' 107.2(8) . . ? C15' C11' C10' 131.2(9) . . ? N12' C11' C10' 121.6(8) . . ? C13' N12' C11' 108.4(8) . . ? C13' N12' Cu 131.7(7) . . ? C11' N12' Cu 117.0(6) . . ? N12' C13' N14' 109.0(9) . . ? C15' N14' C13' 108.4(8) . . ? N14' C15' C11' 106.9(8) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 62.22 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.173 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.125 #===END data_Me2hphpepcu #---------------------------------------------------------------------------- _audit_creation_date 'Thu May 27 09:39:57 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #--------------------------------------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _chemical_compound_source synthesis _chemical_name_common [CuII(MeNHPH-Pep]CH3OH _chemical_formula_weight 318.06 _chemical_formula_analytical ? _chemical_formula_sum 'C12.50 H16 Cu0.50 N4 O4 ' _chemical_formula_moiety '0.5(C23 H26 Cu1 N8 O6), C1 H4 O1' _chemical_formula_structural ? _chemical_melting_point ? #--------------------------------------------------------------------------- _cell_length_a 14.178(3) _cell_length_b 16.111(2) _cell_length_c 13.676(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3123.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.1 #--------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' _symmetry_Int_Tables_number 20 _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 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 #--------------------------------------------------------------------------- _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324.00 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.995 _exptl_special_details ; none ; #--------------------------------------------------------------------------- _diffrn_special_details ; none ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K?a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method ?w-2?q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -4.79 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 -3 0 2 -3 0 4 -2 _diffrn_reflns_number 2008 _reflns_number_total 2008 _reflns_number_gt 1294 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.105 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02759 _diffrn_orient_matrix_UB_12 0.05364 _diffrn_orient_matrix_UB_13 -0.02315 _diffrn_orient_matrix_UB_21 0.04029 _diffrn_orient_matrix_UB_22 0.03089 _diffrn_orient_matrix_UB_23 0.04772 _diffrn_orient_matrix_UB_31 0.05090 _diffrn_orient_matrix_UB_32 0.00462 _diffrn_orient_matrix_UB_33 -0.05033 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'CuCu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #-------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.0000 -0.2540(2) -0.2500 0.0346(5) Uani 1.00 d S.. O(7) O -0.1418(7) -0.3856(6) -0.0400(6) 0.044(3) Uani 1.00 d ... O(9B) O -0.2752(7) -0.2248(7) -0.1480(7) 0.066(4) Uani 1.00 d ... O(9C) O -0.2599(7) -0.1576(7) -0.0034(9) 0.067(3) Uani 1.00 d ... O(17) O -0.394(2) -0.392(2) -0.258(2) 0.31(1) Uiso 1.00 d ... N(1) N 0.0000 -0.3723(8) -0.2500 0.032(3) Uiso 1.00 d S.. N(4A) N 0.0000 -0.6286(9) -0.2500 0.043(4) Uani 1.00 d S.. N(8) N -0.0848(7) -0.2754(7) -0.1372(7) 0.035(3) Uani 1.00 d ... N(12) N 0.0798(7) -0.1768(8) -0.1638(7) 0.041(3) Uani 1.00 d ... N(14) N 0.1857(8) -0.1352(8) -0.0566(9) 0.053(4) Uani 1.00 d ... C(2) C -0.0475(8) -0.4134(8) -0.1814(9) 0.030(3) Uani 1.00 d ... C(3) C -0.0488(8) -0.4974(9) -0.1786(9) 0.039(4) Uani 1.00 d ... C(4) C 0.0000 -0.545(1) -0.2500 0.035(5) Uani 1.00 d S.. C(4A) C -0.054(1) -0.6761(9) -0.179(1) 0.059(5) Uani 1.00 d ... C(7) C -0.0969(10) -0.3563(10) -0.1132(10) 0.039(4) Uani 1.00 d ... C(9) C -0.1207(9) -0.2152(9) -0.0698(9) 0.041(4) Uani 1.00 d ... C(9A) C -0.2285(10) -0.202(1) -0.080(1) 0.053(5) Uani 1.00 d ... C(9D) C -0.357(1) -0.135(1) -0.001(2) 0.080(7) Uani 1.00 d ... C(10) C -0.072(1) -0.129(1) -0.082(1) 0.044(5) Uani 1.00 d ... C(11) C 0.0341(9) -0.1360(10) -0.085(1) 0.040(4) Uani 1.00 d ... C(13) C 0.1712(9) -0.1741(10) -0.144(1) 0.048(5) Uani 1.00 d ... C(15) C 0.100(1) -0.110(1) -0.017(1) 0.059(6) Uani 1.00 d ... C(16) C -0.298(2) -0.447(2) -0.265(2) 0.18(1) Uiso 1.00 d ... H(3) H -0.0819 -0.5242 -0.1270 0.0475 Uiso 1.00 calc ... H(4A2) H -0.0322 -0.6620 -0.1147 0.0698 Uiso 1.00 calc ... H(4A3) H -0.0450 -0.7330 -0.1902 0.0698 Uiso 1.00 calc ... H(4A1) H -0.1186 -0.6619 -0.1844 0.0698 Uiso 1.00 calc ... H(9) H -0.1091 -0.2351 -0.0015 0.0450 Uiso 1.00 calc ... H(9D3) H -0.3957 -0.1850 -0.0006 0.1037 Uiso 1.00 calc ... H(9D1) H -0.3740 -0.1038 -0.0573 0.1037 Uiso 1.00 calc ... H(9D2) H -0.3716 -0.1043 0.0561 0.1037 Uiso 1.00 calc ... H(13) H 0.2205 -0.1963 -0.1848 0.0597 Uiso 1.00 calc ... H(14) H 0.2461 -0.1263 -0.0271 0.0604 Uiso 1.00 calc ... H(15) H 0.0893 -0.0827 0.0439 0.0759 Uiso 1.00 calc ... H(17) H -0.3567 -0.3586 -0.2125 0.0722 Uiso 1.00 calc ... H(101) H -0.0898 -0.0951 -0.0284 0.0545 Uiso 1.00 calc ... H(102) H -0.0945 -0.1075 -0.1408 0.0545 Uiso 1.00 calc ... H(161) H -0.3102 -0.4877 -0.3102 0.2072 Uiso 1.00 calc ... H(162) H -0.2894 -0.4680 -0.2012 0.2072 Uiso 1.00 calc ... H(163) H -0.2499 -0.4107 -0.2828 0.2072 Uiso 1.00 calc ... N(8*) N 0.0848(7) -0.2754(7) -0.3628(7) 0.035(3) Uani 1.00 d ... N(12*) N -0.0798(7) -0.1768(8) -0.3362(7) 0.041(3) Uani 1.00 d ... C(2*) C 0.0475(8) -0.4134(8) -0.3186(9) 0.030(3) Uani 1.00 d ... C(4A*) C 0.054(1) -0.6761(9) -0.321(1) 0.059(5) Uani 1.00 d ... C(3*) C 0.0488(8) -0.4974(9) -0.3214(9) 0.039(4) Uani 1.00 d ... C(7*) C 0.0969(10) -0.3563(10) -0.3868(10) 0.039(4) Uani 1.00 d ... C(9*) C 0.1207(9) -0.2152(9) -0.4302(9) 0.041(4) Uani 1.00 d ... C(11*) C -0.0341(9) -0.1360(10) -0.415(1) 0.040(4) Uani 1.00 d ... C(13*) C -0.1712(9) -0.1741(10) -0.356(1) 0.048(5) Uani 1.00 d ... H(4A2*) H 0.0322 -0.6620 -0.3853 0.0698 Uiso 1.00 calc ... H(4A3*) H 0.0450 -0.7330 -0.3098 0.0698 Uiso 1.00 calc ... H(4A1*) H 0.1186 -0.6619 -0.3156 0.0698 Uiso 1.00 calc ... H(3*) H 0.0819 -0.5242 -0.3730 0.0475 Uiso 1.00 calc ... O(7*) O 0.1418(7) -0.3856(6) -0.4600(6) 0.044(3) Uani 1.00 d ... C(9A*) C 0.2285(10) -0.202(1) -0.420(1) 0.053(5) Uani 1.00 d ... C(10*) C 0.072(1) -0.129(1) -0.418(1) 0.044(5) Uani 1.00 d ... H(9*) H 0.1091 -0.2351 -0.4985 0.0450 Uiso 1.00 calc ... C(15*) C -0.100(1) -0.110(1) -0.483(1) 0.059(6) Uani 1.00 d ... N(14*) N -0.1856(8) -0.1352(8) -0.4434(9) 0.053(4) Uani 1.00 d ... H(13*) H -0.2205 -0.1963 -0.3152 0.0597 Uiso 1.00 calc ... O(9B*) O 0.2752(7) -0.2248(7) -0.3520(7) 0.066(4) Uani 1.00 d ... O(9C*) O 0.2599(7) -0.1576(7) -0.4966(9) 0.067(3) Uani 1.00 d ... H(101*) H 0.0898 -0.0951 -0.4715 0.0545 Uiso 1.00 calc ... H(102*) H 0.0945 -0.1075 -0.3592 0.0545 Uiso 1.00 calc ... H(15*) H -0.0893 -0.0827 -0.5439 0.0759 Uiso 1.00 calc ... H(14*) H -0.2461 -0.1263 -0.4729 0.0604 Uiso 1.00 calc ... C(9D*) C 0.357(1) -0.135(1) -0.499(2) 0.080(7) Uani 1.00 d ... H(9D3*) H 0.3957 -0.1850 -0.4994 0.1037 Uiso 1.00 calc ... H(9D1*) H 0.3740 -0.1038 -0.4427 0.1037 Uiso 1.00 calc ... H(9D2*) H 0.3716 -0.1043 -0.5561 0.1037 Uiso 1.00 calc ... loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0347(10) 0.040(1) 0.0292(9) 0.0000 0.005(1) 0.0000 O(7) 0.045(6) 0.056(7) 0.030(5) 0.010(5) 0.021(5) -0.002(5) O(9B) 0.037(6) 0.10(1) 0.059(7) 0.009(6) -0.010(5) -0.008(7) O(9C) 0.039(6) 0.082(8) 0.079(7) 0.012(6) 0.008(6) -0.020(8) N(4A) 0.045(9) 0.046(9) 0.039(8) 0.0000 0.02(1) 0.0000 N(8) 0.039(6) 0.040(7) 0.025(5) 0.007(6) 0.003(5) -0.007(5) N(12) 0.034(7) 0.058(8) 0.030(6) 0.001(6) 0.000(5) -0.004(6) N(14) 0.034(7) 0.068(10) 0.058(9) 0.004(7) -0.015(7) -0.004(8) C(2) 0.026(6) 0.037(8) 0.027(6) 0.001(6) 0.006(6) -0.011(6) C(3) 0.032(7) 0.057(9) 0.027(7) 0.006(8) 0.007(6) -0.007(7) C(4) 0.026(8) 0.05(1) 0.032(8) 0.0000 0.00(1) 0.0000 C(4A) 0.07(1) 0.047(10) 0.061(10) 0.002(9) 0.020(9) 0.016(9) C(7) 0.029(8) 0.06(1) 0.029(7) 0.004(8) -0.005(7) -0.006(8) C(9) 0.033(8) 0.056(10) 0.034(7) 0.004(7) -0.009(7) 0.004(7) C(9A) 0.031(8) 0.07(1) 0.06(1) 0.013(9) 0.020(8) 0.025(10) C(9D) 0.05(1) 0.10(2) 0.10(2) 0.03(1) 0.02(1) -0.01(1) C(10) 0.033(9) 0.05(1) 0.048(10) 0.020(8) -0.005(8) -0.002(9) C(11) 0.038(9) 0.044(10) 0.038(8) -0.013(7) -0.006(7) 0.007(8) C(13) 0.032(8) 0.07(1) 0.041(8) -0.006(8) -0.004(7) 0.001(9) C(15) 0.045(10) 0.08(1) 0.06(1) -0.011(9) -0.011(9) 0.000(10) N(8*) 0.039(6) 0.040(7) 0.025(5) -0.007(6) 0.003(5) 0.007(5) N(12*) 0.034(7) 0.058(8) 0.030(6) -0.001(6) 0.000(5) 0.004(6) C(2*) 0.026(6) 0.037(8) 0.027(6) -0.001(6) 0.006(6) 0.011(6) C(4A*) 0.07(1) 0.047(10) 0.061(10) -0.002(9) 0.020(9) -0.016(9) C(3*) 0.032(7) 0.057(9) 0.027(7) -0.006(8) 0.007(6) 0.007(7) C(7*) 0.029(8) 0.06(1) 0.029(7) -0.004(8) -0.005(7) 0.006(8) C(9*) 0.033(8) 0.056(10) 0.034(7) -0.004(7) -0.009(7) -0.004(7) C(11*) 0.038(9) 0.044(10) 0.038(8) 0.013(7) -0.006(7) -0.007(8) C(13*) 0.032(8) 0.07(1) 0.041(8) 0.006(8) -0.004(7) -0.001(9) O(7*) 0.045(6) 0.056(7) 0.030(5) -0.010(5) 0.021(5) 0.002(5) C(9A*) 0.031(8) 0.07(1) 0.06(1) -0.013(9) 0.020(8) -0.025(10) C(10*) 0.033(9) 0.05(1) 0.048(10) -0.020(8) -0.005(8) 0.002(9) C(15*) 0.045(10) 0.08(1) 0.06(1) 0.011(9) -0.011(9) 0.000(10) N(14*) 0.034(7) 0.068(10) 0.058(9) -0.004(7) -0.015(7) 0.004(8) O(9B*) 0.037(6) 0.10(1) 0.059(7) -0.009(6) -0.010(5) 0.008(7) O(9C*) 0.039(6) 0.082(8) 0.079(7) -0.012(6) 0.008(6) 0.020(8) C(9D*) 0.05(1) 0.10(2) 0.10(2) -0.03(1) 0.02(1) 0.01(1) #--------------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[?s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_abs_structure_details none? _refine_ls_abs_structure_Flack none? _refine_ls_number_reflns 1294 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 3.129 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.41 _refine_diff_density_max 0.59 #--------------------------------------------------------------------------- _geom_special_details ; The copper complex belongs C2 symmetry and the crystakkographic 2-fold Axis passes Cu(1), N(1), N(4A), and C(4) atoms. ; 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) 1.91(1) 1_555 1_555 yes Cu(1) N(8) 1.99(1) 1_555 1_555 yes Cu(1) N(8) 1.99(1) 1_555 4_554 yes Cu(1) N(12) 2.05(1) 1_555 1_555 yes Cu(1) N(12) 2.05(1) 1_555 4_554 yes O(7) C(7) 1.28(2) 1_555 1_555 yes O(9B) C(9A) 1.20(2) 1_555 1_555 yes O(9C) C(9A) 1.35(2) 1_555 1_555 yes O(9C) C(9D) 1.43(2) 1_555 1_555 yes O(17) C(16) 1.63(3) 1_555 1_555 yes N(1) C(2) 1.33(1) 1_555 1_555 yes N(1) C(2) 1.33(1) 1_555 4_554 yes N(4A) C(4) 1.35(2) 1_555 1_555 yes N(4A) C(4A) 1.45(1) 1_555 1_555 yes N(4A) C(4A) 1.45(1) 1_555 4_554 yes N(8) C(7) 1.36(2) 1_555 1_555 yes N(8) C(9) 1.43(1) 1_555 1_555 yes N(12) C(11) 1.42(2) 1_555 1_555 yes N(12) C(13) 1.32(2) 1_555 1_555 yes N(14) C(13) 1.37(2) 1_555 1_555 yes N(14) C(15) 1.40(2) 1_555 1_555 yes C(2) C(3) 1.35(2) 1_555 1_555 yes C(2) C(7) 1.48(2) 1_555 1_555 yes C(3) C(4) 1.42(1) 1_555 1_555 yes C(9) C(9A) 1.55(2) 1_555 1_555 yes C(9) C(10) 1.56(2) 1_555 1_555 yes C(10) C(11) 1.50(2) 1_555 1_555 yes C(11) C(15) 1.38(2) 1_555 1_555 yes #-------------------------------------------------------------------------- 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(8) 80.0(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(8) 80.0(3) 1_555 1_555 4_554 yes N(1) Cu(1) N(12) 127.3(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(12) 127.3(3) 1_555 1_555 4_554 yes N(8) Cu(1) N(8) 160.0(6) 1_555 1_555 4_554 yes N(8) Cu(1) N(12) 89.6(4) 1_555 1_555 1_555 yes N(8) Cu(1) N(12) 102.6(4) 1_555 1_555 4_554 yes N(8) Cu(1) N(12) 102.6(4) 4_554 1_555 1_555 yes N(8) Cu(1) N(12) 89.6(4) 4_554 1_555 4_554 yes N(12) Cu(1) N(12) 105.4(7) 1_555 1_555 4_554 yes C(9A) O(9C) C(9D) 118(1) 1_555 1_555 1_555 yes C(16) O(17) H(17) 82(1) 1_555 1_555 1_555 no Cu(1) N(1) C(2) 119.8(7) 1_555 1_555 1_555 yes Cu(1) N(1) C(2) 119.8(7) 1_555 1_555 4_554 yes C(2) N(1) C(2) 120(1) 1_555 1_555 4_554 yes C(4) N(4A) C(4A) 121.9(8) 1_555 1_555 1_555 yes C(4) N(4A) C(4A) 121.9(8) 1_555 1_555 4_554 yes C(4A) N(4A) C(4A) 116(1) 1_555 1_555 4_554 yes Cu(1) N(8) C(7) 115.5(9) 1_555 1_555 1_555 yes Cu(1) N(8) C(9) 126.7(9) 1_555 1_555 1_555 yes C(7) N(8) C(9) 116(1) 1_555 1_555 1_555 yes Cu(1) N(12) C(11) 117.7(8) 1_555 1_555 1_555 yes Cu(1) N(12) C(13) 132(1) 1_555 1_555 1_555 yes C(11) N(12) C(13) 106(1) 1_555 1_555 1_555 yes C(13) N(14) C(15) 109(1) 1_555 1_555 1_555 yes C(13) N(14) H(14) 124(1) 1_555 1_555 1_555 no C(15) N(14) H(14) 125(1) 1_555 1_555 1_555 no N(1) C(2) C(3) 121(1) 1_555 1_555 1_555 yes N(1) C(2) C(7) 111(1) 1_555 1_555 1_555 yes C(3) C(2) C(7) 126(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120(1) 1_555 1_555 1_555 yes C(2) C(3) H(3) 118(1) 1_555 1_555 1_555 no C(4) C(3) H(3) 120(1) 1_555 1_555 1_555 no N(4A) C(4) C(3) 122.5(8) 1_555 1_555 1_555 yes N(4A) C(4) C(3) 122.5(8) 1_555 1_555 4_554 yes C(3) C(4) C(3) 115(1) 1_555 1_555 4_554 yes N(4A) C(4A) H(4A2) 108(1) 1_555 1_555 1_555 no N(4A) C(4A) H(4A3) 110(1) 1_555 1_555 1_555 no N(4A) C(4A) H(4A1) 109(1) 1_555 1_555 1_555 no H(4A2) C(4A) H(4A3) 109(1) 1_555 1_555 1_555 no H(4A2) C(4A) H(4A1) 108(1) 1_555 1_555 1_555 no H(4A3) C(4A) H(4A1) 110(1) 1_555 1_555 1_555 no O(7) C(7) N(8) 127(1) 1_555 1_555 1_555 yes O(7) C(7) C(2) 119(1) 1_555 1_555 1_555 yes N(8) C(7) C(2) 112(1) 1_555 1_555 1_555 yes N(8) C(9) C(9A) 112(1) 1_555 1_555 1_555 yes N(8) C(9) C(10) 111(1) 1_555 1_555 1_555 yes N(8) C(9) H(9) 108(1) 1_555 1_555 1_555 no C(9A) C(9) C(10) 107(1) 1_555 1_555 1_555 yes C(9A) C(9) H(9) 107(1) 1_555 1_555 1_555 no C(10) C(9) H(9) 108(1) 1_555 1_555 1_555 no O(9B) C(9A) O(9C) 125(1) 1_555 1_555 1_555 yes O(9B) C(9A) C(9) 125(1) 1_555 1_555 1_555 yes O(9C) C(9A) C(9) 109(1) 1_555 1_555 1_555 yes O(9C) C(9D) H(9D3) 109(1) 1_555 1_555 1_555 no O(9C) C(9D) H(9D1) 110(1) 1_555 1_555 1_555 no O(9C) C(9D) H(9D2) 111(1) 1_555 1_555 1_555 no H(9D3) C(9D) H(9D1) 107(1) 1_555 1_555 1_555 no H(9D3) C(9D) H(9D2) 108(1) 1_555 1_555 1_555 no H(9D1) C(9D) H(9D2) 109(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 112(1) 1_555 1_555 1_555 yes C(9) C(10) H(101) 108(1) 1_555 1_555 1_555 no C(9) C(10) H(102) 105(1) 1_555 1_555 1_555 no C(11) C(10) H(101) 109(1) 1_555 1_555 1_555 no C(11) C(10) H(102) 110(1) 1_555 1_555 1_555 no H(101) C(10) H(102) 110(1) 1_555 1_555 1_555 no N(12) C(11) C(10) 120(1) 1_555 1_555 1_555 yes N(12) C(11) C(15) 110(1) 1_555 1_555 1_555 yes C(10) C(11) C(15) 129(1) 1_555 1_555 1_555 yes N(12) C(13) N(14) 109(1) 1_555 1_555 1_555 yes N(12) C(13) H(13) 125(1) 1_555 1_555 1_555 no N(14) C(13) H(13) 124(1) 1_555 1_555 1_555 no N(14) C(15) C(11) 103(1) 1_555 1_555 1_555 yes N(14) C(15) H(15) 127(1) 1_555 1_555 1_555 no C(11) C(15) H(15) 128(1) 1_555 1_555 1_555 no O(17) C(16) H(161) 105(2) 1_555 1_555 1_555 no O(17) C(16) H(162) 104(2) 1_555 1_555 1_555 no O(17) C(16) H(163) 106(2) 1_555 1_555 1_555 no H(161) C(16) H(162) 112(2) 1_555 1_555 1_555 no H(161) C(16) H(163) 114(3) 1_555 1_555 1_555 no H(162) C(16) H(163) 112(2) 1_555 1_555 1_555 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(2) C(3) -179.6(9) 1_555 1_555 1_555 1_555 yes Cu(1) N(1) C(2) C(7) 1(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(1) C(2) C(3) -179.6(9) 1_555 1_555 4_554 4_554 yes Cu(1) N(1) C(2) C(7) 1(1) 1_555 1_555 4_554 4_554 yes Cu(1) N(8) C(7) O(7) 174(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(8) C(7) C(2) -3(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(8) C(9) C(9A) 111(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(8) C(9) C(10) -10(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(8) C(7) O(7) 174(1) 1_555 4_554 4_554 4_554 yes Cu(1) N(8) C(7) C(2) -3(1) 1_555 4_554 4_554 4_554 yes Cu(1) N(8) C(9) C(9A) 111(1) 1_555 4_554 4_554 4_554 yes Cu(1) N(8) C(9) C(10) -10(1) 1_555 4_554 4_554 4_554 yes Cu(1) N(12) C(11) C(10) -17(2) 1_555 1_555 1_555 1_555 yes Cu(1) N(12) C(11) C(15) 160(1) 1_555 1_555 1_555 1_555 yes Cu(1) N(12) C(13) N(14) -156.0(10) 1_555 1_555 1_555 1_555 yes Cu(1) N(12) C(11) C(10) -17(2) 1_555 4_554 4_554 4_554 yes Cu(1) N(12) C(11) C(15) 160(1) 1_555 4_554 4_554 4_554 yes Cu(1) N(12) C(13) N(14) -156.0(10) 1_555 4_554 4_554 4_554 yes O(7) C(7) N(8) C(9) 4(2) 1_555 1_555 1_555 1_555 yes O(7) C(7) C(2) N(1) -176(1) 1_555 1_555 1_555 1_555 yes O(7) C(7) C(2) C(3) 4(2) 1_555 1_555 1_555 1_555 yes O(9B) C(9A) O(9C) C(9D) 0(2) 1_555 1_555 1_555 1_555 yes O(9B) C(9A) C(9) N(8) -14(2) 1_555 1_555 1_555 1_555 yes O(9B) C(9A) C(9) C(10) 109(1) 1_555 1_555 1_555 1_555 yes O(9C) C(9A) C(9) N(8) 168(1) 1_555 1_555 1_555 1_555 yes O(9C) C(9A) C(9) C(10) -68(1) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(8) C(7) 3.1(9) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(8) C(9) 171.7(10) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(8) C(7) 3.1(9) 1_555 1_555 4_554 4_554 yes N(1) Cu(1) N(8) C(9) 171.7(10) 1_555 1_555 4_554 4_554 yes N(1) Cu(1) N(12) C(11) -104.8(10) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(12) C(13) 50(1) 1_555 1_555 1_555 1_555 yes N(1) Cu(1) N(12) C(11) -104.8(10) 1_555 1_555 4_554 4_554 yes N(1) Cu(1) N(12) C(13) 50(1) 1_555 1_555 4_554 4_554 yes N(1) C(2) C(3) C(4) 0(1) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(7) N(8) 1(1) 1_555 1_555 1_555 1_555 yes N(1) C(2) C(3) C(4) 0(1) 1_555 4_554 4_554 1_555 yes N(1) C(2) C(7) N(8) 1(1) 1_555 4_554 4_554 4_554 yes N(4A) C(4) C(3) C(2) -179.6(9) 1_555 1_555 1_555 1_555 yes N(4A) C(4) C(3) C(2) -179.6(9) 1_555 1_555 4_554 4_554 yes N(8) Cu(1) N(1) C(2) -2.2(7) 1_555 1_555 1_555 1_555 yes N(8) Cu(1) N(1) C(2) 177.8(7) 1_555 1_555 1_555 4_554 yes N(8) Cu(1) N(8) C(7) 3.1(9) 1_555 1_555 4_554 4_554 yes N(8) Cu(1) N(8) C(9) 171.7(10) 1_555 1_555 4_554 4_554 yes N(8) Cu(1) N(12) C(11) -27(1) 1_555 1_555 1_555 1_555 yes N(8) Cu(1) N(12) C(13) 127(1) 1_555 1_555 1_555 1_555 yes N(8) Cu(1) N(12) C(11) 168(1) 1_555 1_555 4_554 4_554 yes N(8) Cu(1) N(12) C(13) -36(1) 1_555 1_555 4_554 4_554 yes N(8) C(7) C(2) C(3) -177(1) 1_555 1_555 1_555 1_555 yes N(8) C(9) C(10) C(11) -49(1) 1_555 1_555 1_555 1_555 yes N(12) Cu(1) N(1) C(2) 79.5(7) 1_555 1_555 1_555 1_555 yes N(12) Cu(1) N(1) C(2) -100.5(7) 1_555 1_555 1_555 4_554 yes N(12) Cu(1) N(8) C(7) -125.0(10) 1_555 1_555 1_555 1_555 yes N(12) Cu(1) N(8) C(9) 43(1) 1_555 1_555 1_555 1_555 yes N(12) Cu(1) N(8) C(7) 129.3(10) 1_555 1_555 4_554 4_554 yes N(12) Cu(1) N(8) C(9) -62(1) 1_555 1_555 4_554 4_554 yes N(12) Cu(1) N(12) C(11) 75.2(10) 1_555 1_555 4_554 4_554 yes N(12) Cu(1) N(12) C(13) -129(1) 1_555 1_555 4_554 4_554 yes N(12) C(11) C(10) C(9) 66(2) 1_555 1_555 1_555 1_555 yes N(12) C(11) C(15) N(14) 0(1) 1_555 1_555 1_555 1_555 yes N(12) C(13) N(14) C(15) -1(1) 1_555 1_555 1_555 1_555 yes N(14) C(13) N(12) C(11) 1(1) 1_555 1_555 1_555 1_555 yes N(14) C(15) C(11) C(10) 177(1) 1_555 1_555 1_555 1_555 yes C(2) N(1) C(2) C(3) 0.4(9) 1_555 1_555 4_554 4_554 yes C(2) N(1) C(2) C(7) -178(1) 1_555 1_555 4_554 4_554 yes C(2) C(3) C(4) C(3) 0.4(9) 1_555 1_555 1_555 4_554 yes C(2) C(7) N(8) C(9) -173(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) N(4A) C(4A) 2(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) N(4A) C(4A) -177(1) 1_555 1_555 1_555 4_554 yes C(4) C(3) C(2) C(7) 178(1) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(7) 178(1) 1_555 4_554 4_554 4_554 yes C(7) N(8) C(9) C(9A) -80(1) 1_555 1_555 1_555 1_555 yes C(7) N(8) C(9) C(10) 158(1) 1_555 1_555 1_555 1_555 yes C(9) C(9A) O(9C) C(9D) 177(1) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(15) -111(2) 1_555 1_555 1_555 1_555 yes C(9A) C(9) C(10) C(11) -173(1) 1_555 1_555 1_555 1_555 yes C(10) C(11) N(12) C(13) -178(1) 1_555 1_555 1_555 1_555 yes C(11) C(15) N(14) C(13) 0(1) 1_555 1_555 1_555 1_555 yes C(13) N(12) C(11) C(15) 0(1) 1_555 1_555 1_555 1_555 yes #-------------------------------------------------------------------------- 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 O(7) N(14) 2.80(2) 1_555 6_445 ? O(7) C(4A) 3.40(2) 1_555 2_545 ? O(9B) C(4A) 3.48(2) 1_555 8_454 ? O(9B) O(17) 3.51(3) 1_555 1_555 ? O(9C) C(13) 3.52(2) 1_555 6_445 ? O(9C) N(14) 3.52(2) 1_555 6_445 ? O(17) O(17) 3.01(5) 1_555 4_454 ? N(14) C(9A) 3.45(2) 1_555 6_545 ? C(15) C(15) 3.57(3) 1_555 2_555 ? #-------------------------------------------------------------------------- _publ_contact_author_name ' Masafumi Goto' _publ_contact_author_address ; Faculty of Pharmaceutical Sciences, Kumamoto University, 5-1 Oe-honmchi, Kumamoto 862-0973, Japan ; _publ_contact_author_email ' gotomphi@gpo.kumamoto-u.ac.jp ' _publ_contact_author_fax ' +81-96-371-4314 ' _publ_contact_author_phone ' +81-96-371-4310 ' #===END