#------------------------------------------------------------------------------ #$Date: 2016-03-22 22:41:36 +0000 (Tue, 22 Mar 2016) $ #$Revision: 179123 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308547.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308547 loop_ _publ_author_name 'Mauricio C. B. de Oliveira' 'Marciela Scarpellini' 'Ademir Neves' 'Hern\'an Terenzi' 'Adailton J. Bortoluzzi' 'Bruno Szpoganics' 'Alessandra Greatti' 'Ant\^onio S. Mangrich' 'Emanuel M. de Souza' 'Pablo M. Fernandez' 'Marcia R. Soares' _publ_contact_author_address ; Depto. Qu\'imica - UFSC 88040 - 900 Florian\'opolis, SC Brazil ; _publ_contact_author_email ademir@qmc.ufsc.br _publ_contact_author_fax 55(48)3316888 _publ_contact_author_name 'Ademir Neves' _publ_contact_author_phone 55(48)3316826 _publ_section_title ; Hydrolytic Protein Cleavage Mediated by Unusual Mononuclear Copper(II) Complexes: X-ray Structures and Solution Studies ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 921 _journal_page_last 929 _journal_paper_doi 10.1021/ic0485864 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C21 H22 Cl Cu N3 O3' _chemical_formula_weight 463.41 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.72(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.311(2) _cell_length_b 12.782(3) _cell_length_c 19.824(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.32 _cell_measurement_theta_min 10.05 _cell_volume 2069.2(8) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 3941 _diffrn_reflns_theta_full 25.07 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_min 2.52 _diffrn_standards_decay_% 1.0 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time '120 min' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_type psi-scan _exptl_crystal_colour olive-green _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular plate' _exptl_crystal_F_000 956 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.263 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.056 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 3669 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0338 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.0962P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.0914 _reflns_number_gt 2521 _reflns_number_total 3669 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0485864rom20041008_111340_1.cif _cod_data_source_block C21H22ClCuN3O3 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.0962P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+1.0962P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4308547 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11463(4) 0.15840(3) 0.536508(18) 0.04005(14) Uani 1 d . . . Cl1 Cl 0.35392(10) 0.07413(7) 0.57845(5) 0.0562(2) Uani 1 d . . . O1 O 0.2216(2) 0.30809(16) 0.52793(10) 0.0414(5) Uani 1 d . . . O2 O 0.5211(3) 0.4150(2) 0.40319(13) 0.0690(8) Uani 1 d . . . N1 N -0.1191(3) 0.2137(2) 0.49923(12) 0.0397(6) Uani 1 d . . . N12 N 0.0298(3) 0.1556(2) 0.62458(12) 0.0453(6) Uani 1 d . . . N32 N 0.1128(3) 0.1300(2) 0.43651(13) 0.0479(7) Uani 1 d . . . C10 C -0.2261(4) 0.1724(3) 0.54528(16) 0.0517(9) Uani 1 d . . . H10A H -0.2629 0.1025 0.5309 0.062 Uiso 1 calc R . . H10B H -0.3218 0.2167 0.5426 0.062 Uiso 1 calc R . . C11 C -0.1332(4) 0.1695(3) 0.61769(16) 0.0473(8) Uani 1 d . . . C13 C 0.1197(5) 0.1463(3) 0.68817(17) 0.0572(9) Uani 1 d . . . H13 H 0.2325 0.1377 0.6934 0.069 Uiso 1 calc R . . C14 C 0.0497(5) 0.1494(3) 0.74552(18) 0.0640(10) Uani 1 d . . . H14 H 0.1143 0.1411 0.7888 0.077 Uiso 1 calc R . . C15 C -0.1156(5) 0.1645(3) 0.73884(19) 0.0682(11) Uani 1 d . . . H15 H -0.1641 0.1675 0.7775 0.082 Uiso 1 calc R . . C16 C -0.2092(5) 0.1752(3) 0.67396(19) 0.0600(10) Uani 1 d . . . H16 H -0.3216 0.1861 0.6682 0.072 Uiso 1 calc R . . C20 C -0.1168(3) 0.3310(2) 0.50330(15) 0.0395(7) Uani 1 d . . . H20A H -0.2280 0.3570 0.4906 0.047 Uiso 1 calc R . . H20B H -0.0753 0.3520 0.5503 0.047 Uiso 1 calc R . . C21 C -0.0133(3) 0.3797(2) 0.45745(14) 0.0339(7) Uani 1 d . . . C22 C 0.1592(3) 0.3628(2) 0.47408(14) 0.0331(7) Uani 1 d . . . C23 C 0.2529(3) 0.4068(2) 0.42831(15) 0.0368(7) Uani 1 d . . . C24 C 0.1781(4) 0.4676(2) 0.37180(15) 0.0407(7) Uani 1 d . . . H24 H 0.2430 0.4964 0.3431 0.049 Uiso 1 calc R . . C25 C 0.0130(3) 0.4853(2) 0.35787(15) 0.0388(7) Uani 1 d . . . C26 C -0.0809(3) 0.4395(2) 0.40187(15) 0.0379(7) Uani 1 d . . . H26 H -0.1936 0.4500 0.3930 0.046 Uiso 1 calc R . . C27 C 0.4256(4) 0.3845(3) 0.43900(17) 0.0532(9) Uani 1 d . . . H27 H 0.4685 0.3431 0.4766 0.064 Uiso 1 calc R . . C28 C -0.0662(4) 0.5531(3) 0.29839(18) 0.0630(10) Uani 1 d . . . H28A H -0.1821 0.5562 0.2971 0.094 Uiso 0.50 calc PR . . H28B H -0.0456 0.5239 0.2562 0.094 Uiso 0.50 calc PR . . H28C H -0.0211 0.6224 0.3041 0.094 Uiso 0.50 calc PR . . H28D H 0.0163 0.5788 0.2745 0.094 Uiso 0.50 calc PR . . H28E H -0.1203 0.6111 0.3154 0.094 Uiso 0.50 calc PR . . H28F H -0.1448 0.5126 0.2675 0.094 Uiso 0.50 calc PR . . C30 C -0.1715(4) 0.1787(3) 0.42686(16) 0.0512(9) Uani 1 d . . . H30A H -0.2390 0.2324 0.4011 0.061 Uiso 1 calc R . . H30B H -0.2368 0.1157 0.4258 0.061 Uiso 1 calc R . . C31 C -0.0260(4) 0.1575(3) 0.39395(16) 0.0491(8) Uani 1 d . . . C33 C 0.2464(5) 0.1068(3) 0.40974(19) 0.0611(10) Uani 1 d . . . H33 H 0.3434 0.0892 0.4392 0.073 Uiso 1 calc R . . C34 C 0.2431(6) 0.1085(3) 0.3406(2) 0.0820(13) Uani 1 d . . . H34 H 0.3365 0.0914 0.3235 0.098 Uiso 1 calc R . . C35 C 0.1016(7) 0.1356(4) 0.2965(2) 0.0886(15) Uani 1 d . . . H35 H 0.0980 0.1369 0.2493 0.106 Uiso 1 calc R . . C36 C -0.0352(5) 0.1610(3) 0.32343(18) 0.0694(11) Uani 1 d . . . H36 H -0.1322 0.1802 0.2946 0.083 Uiso 1 calc R . . O1W O 0.4774(4) 0.3589(3) 0.63038(15) 0.1092(12) Uani 1 d . . . H1WA H 0.3877 0.3392 0.5915 0.131 Uiso 1 d R . . H1WB H 0.5140 0.4235 0.6247 0.131 Uiso 1 d 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 0.0394(2) 0.0417(2) 0.0388(2) 0.00142(19) 0.00648(15) -0.00036(19) Cl1 0.0461(5) 0.0522(5) 0.0692(6) 0.0043(4) 0.0074(4) 0.0071(4) O1 0.0348(11) 0.0450(13) 0.0407(12) 0.0059(10) -0.0023(9) -0.0043(9) O2 0.0340(13) 0.108(2) 0.0680(16) 0.0160(16) 0.0183(12) -0.0002(13) N1 0.0335(13) 0.0466(16) 0.0382(15) 0.0034(12) 0.0042(11) -0.0105(12) N12 0.0470(15) 0.0514(17) 0.0374(14) 0.0081(13) 0.0077(12) 0.0036(13) N32 0.0632(18) 0.0405(16) 0.0418(15) -0.0054(12) 0.0146(14) -0.0075(13) C10 0.0372(17) 0.064(2) 0.054(2) 0.0139(18) 0.0073(15) -0.0143(17) C11 0.051(2) 0.0444(19) 0.0476(19) 0.0100(16) 0.0125(15) -0.0040(16) C13 0.062(2) 0.064(2) 0.0435(19) 0.0052(18) 0.0043(16) 0.0101(19) C14 0.086(3) 0.066(3) 0.0393(19) 0.0115(19) 0.0086(18) 0.009(2) C15 0.094(3) 0.064(2) 0.053(2) 0.008(2) 0.031(2) 0.002(2) C16 0.060(2) 0.064(2) 0.062(2) 0.0132(19) 0.0266(19) 0.0014(19) C20 0.0319(15) 0.0447(18) 0.0425(18) 0.0026(15) 0.0080(13) 0.0023(14) C21 0.0274(14) 0.0355(16) 0.0381(16) -0.0035(13) 0.0043(12) -0.0030(13) C22 0.0312(15) 0.0301(17) 0.0368(16) -0.0047(13) 0.0030(12) -0.0009(12) C23 0.0302(15) 0.0399(18) 0.0403(17) -0.0015(14) 0.0062(13) -0.0014(13) C24 0.0386(17) 0.0458(19) 0.0394(17) 0.0008(15) 0.0118(14) -0.0055(14) C25 0.0376(17) 0.0351(17) 0.0420(18) 0.0037(14) 0.0026(14) -0.0025(14) C26 0.0303(15) 0.0399(17) 0.0420(18) -0.0021(14) 0.0025(13) -0.0012(14) C27 0.0340(17) 0.072(2) 0.053(2) 0.0083(19) 0.0063(15) 0.0004(17) C28 0.053(2) 0.068(3) 0.064(2) 0.026(2) 0.0004(18) -0.0035(19) C30 0.053(2) 0.048(2) 0.0455(19) 0.0000(16) -0.0093(16) -0.0163(16) C31 0.067(2) 0.0406(18) 0.0374(17) -0.0092(16) 0.0036(16) -0.0150(17) C33 0.077(3) 0.052(2) 0.061(2) -0.0059(19) 0.028(2) 0.005(2) C34 0.121(4) 0.071(3) 0.066(3) -0.010(2) 0.048(3) 0.004(3) C35 0.145(5) 0.080(3) 0.049(2) -0.012(2) 0.040(3) -0.009(3) C36 0.098(3) 0.067(3) 0.039(2) -0.010(2) 0.001(2) -0.016(2) O1W 0.105(2) 0.103(3) 0.092(2) 0.0137(19) -0.0535(18) -0.030(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N12 Cu1 N32 156.46(11) . . y N12 Cu1 N1 81.85(10) . . y N32 Cu1 N1 82.84(11) . . y N12 Cu1 O1 107.80(10) . . y N32 Cu1 O1 90.60(9) . . y N1 Cu1 O1 92.45(9) . . y N12 Cu1 Cl1 95.63(8) . . y N32 Cu1 Cl1 96.91(9) . . y N1 Cu1 Cl1 171.52(7) . . y O1 Cu1 Cl1 96.03(6) . . y C22 O1 Cu1 116.10(17) . . y C10 N1 C30 112.6(2) . . ? C10 N1 C20 109.0(2) . . ? C30 N1 C20 110.5(2) . . ? C10 N1 Cu1 106.80(18) . . ? C30 N1 Cu1 109.17(19) . . ? C20 N1 Cu1 108.66(17) . . ? C13 N12 C11 118.6(3) . . ? C13 N12 Cu1 126.5(2) . . ? C11 N12 Cu1 114.8(2) . . ? C31 N32 C33 118.9(3) . . ? C31 N32 Cu1 114.8(2) . . ? C33 N32 Cu1 124.8(3) . . ? N1 C10 C11 109.7(2) . . ? N12 C11 C16 121.8(3) . . ? N12 C11 C10 115.4(3) . . ? C16 C11 C10 122.7(3) . . ? N12 C13 C14 121.8(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 119.1(3) . . ? C15 C16 C11 118.9(4) . . ? C21 C20 N1 112.7(2) . . ? C26 C21 C22 120.9(3) . . ? C26 C21 C20 121.5(3) . . ? C22 C21 C20 117.5(3) . . ? O1 C22 C23 123.8(2) . . ? O1 C22 C21 120.1(3) . . ? C23 C22 C21 116.1(3) . . ? C24 C23 C22 120.9(3) . . ? C24 C23 C27 120.4(3) . . ? C22 C23 C27 118.6(3) . . ? C25 C24 C23 122.0(3) . . ? C24 C25 C26 117.3(3) . . ? C24 C25 C28 121.8(3) . . ? C26 C25 C28 120.8(3) . . ? C21 C26 C25 122.7(3) . . ? O2 C27 C23 126.0(3) . . ? N1 C30 C31 111.0(2) . . ? N32 C31 C36 121.4(3) . . ? N32 C31 C30 116.2(3) . . ? C36 C31 C30 122.3(3) . . ? N32 C33 C34 121.7(4) . . ? C33 C34 C35 119.9(4) . . ? C34 C35 C36 118.8(4) . . ? C35 C36 C31 119.2(4) . . ? 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 N12 2.001(2) . y Cu1 N32 2.013(3) . y Cu1 N1 2.070(2) . y Cu1 O1 2.130(2) . y Cu1 Cl1 2.2784(10) . y O1 C22 1.300(3) . ? O2 C27 1.223(4) . ? N1 C10 1.485(4) . ? N1 C30 1.488(4) . ? N1 C20 1.502(4) . ? N12 C13 1.346(4) . ? N12 C11 1.348(4) . ? N32 C31 1.343(4) . ? N32 C33 1.350(4) . ? C10 C11 1.499(4) . ? C11 C16 1.383(4) . ? C13 C14 1.371(5) . ? C14 C15 1.369(5) . ? C15 C16 1.381(5) . ? C20 C21 1.498(4) . ? C21 C26 1.372(4) . ? C21 C22 1.427(4) . ? C22 C23 1.418(4) . ? C23 C24 1.409(4) . ? C23 C27 1.439(4) . ? C24 C25 1.368(4) . ? C25 C26 1.402(4) . ? C25 C28 1.512(4) . ? C30 C31 1.502(5) . ? C31 C36 1.386(5) . ? C33 C34 1.365(5) . ? C34 C35 1.373(6) . ? C35 C36 1.382(6) . ? 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 _geom_hbond_publ_flag O1W H1WA O1 1.00 1.73 2.732(3) 175.6 . y O1W H1WB O2 0.89 2.14 2.966(4) 152.7 3_666 y