#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100158.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_1100158 loop_ _publ_author_name 'Carballo, Rosa' 'Vazquez-Lopez, Ezequiel M.' 'Covelo, Berta' 'Garcia-Martinez, Emilia' 'Castineiras, Alfonso' 'Niclos, Juan' _publ_section_title ; 'Solid state coordination chemistry of mononuclear mixed-ligand complexes of Ni(II), Cu(II) and Zn(II) with \a-hydroxycarboxylic acids and imidazole' ; _journal_name_full Polyhedron _journal_page_first 1505 _journal_page_last 1518 _journal_paper_doi 10.1016/j.poly.2004.02.028 _journal_volume 23 _journal_year 2004 _chemical_formula_sum 'C7 H10 Cu N2 O6' _chemical_formula_weight 281.71 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 75.045(5) _cell_angle_beta 85.826(6) _cell_angle_gamma 75.613(7) _cell_formula_units_Z 2 _cell_length_a 5.528(2) _cell_length_b 7.267(3) _cell_length_c 13.626(5) _cell_measurement_reflns_used 451 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.80 _cell_measurement_theta_min 2.99 _cell_volume 512.2(3) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.795 _diffrn_measured_fraction_theta_max 0.795 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 2335 _diffrn_reflns_theta_full 28.07 _diffrn_reflns_theta_max 28.07 _diffrn_reflns_theta_min 1.55 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 286 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.666 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.103 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 1984 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0675 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.3732P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1157 _refine_ls_wR_factor_ref 0.1259 _reflns_number_gt 1472 _reflns_number_total 1984 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'multiscan' changed to 'multi-scan' 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 ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1100158 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.85489(16) 0.17931(12) 0.24638(6) 0.0339(2) Uani 1 1 d . . . O11 O 1.1010(8) 0.1569(6) 0.3482(3) 0.0355(10) Uani 1 1 d . . . O12 O 1.2067(8) 0.2078(7) 0.4906(3) 0.0453(12) Uani 1 1 d . . . O13 O 0.6099(8) 0.3058(7) 0.3762(4) 0.0441(12) Uani 1 1 d . . . C11 C 1.0453(11) 0.2179(8) 0.4281(4) 0.0284(13) Uani 1 1 d . . . C12 C 0.7774(12) 0.3070(11) 0.4509(5) 0.0438(16) Uani 1 1 d . . . H12A H 0.7306 0.2345 0.5168 0.053 Uiso 1 1 calc R . . H12B H 0.7620 0.4412 0.4543 0.053 Uiso 1 1 calc R . . O21 O 0.6140(9) 0.1710(6) 0.1514(3) 0.0425(11) Uani 1 1 d . . . O22 O 0.3233(9) 0.0174(7) 0.1353(3) 0.0513(13) Uani 1 1 d . . . O23 O 0.8172(9) -0.0923(7) 0.3088(4) 0.0383(11) Uani 1 1 d . . . C21 C 0.5043(12) 0.0325(9) 0.1778(4) 0.0348(14) Uani 1 1 d . . . C22 C 0.6013(12) -0.1304(9) 0.2729(4) 0.0341(14) Uani 1 1 d . . . H22A H 0.4727 -0.1330 0.3253 0.041 Uiso 1 1 calc R . . H22B H 0.6450 -0.2568 0.2565 0.041 Uiso 1 1 calc R . . N1 N 0.9023(9) 0.4332(7) 0.1657(3) 0.0304(11) Uani 1 1 d . . . N2 N 0.8416(11) 0.7075(8) 0.0454(4) 0.0380(13) Uani 1 1 d . . . C1 C 0.7598(12) 0.5469(8) 0.0879(4) 0.0324(13) Uani 1 1 d . . . H1 H 0.6213 0.5180 0.0660 0.039 Uiso 1 1 calc R . . C2 C 1.0842(12) 0.5292(9) 0.1720(5) 0.0364(15) Uani 1 1 d . . . H2 H 1.2116 0.4843 0.2196 0.044 Uiso 1 1 calc R . . C3 C 1.0492(13) 0.6997(9) 0.0981(5) 0.0393(15) Uani 1 1 d . . . H3 H 1.1453 0.7919 0.0857 0.047 Uiso 1 1 calc R . . H20 H 0.785(12) 0.801(9) -0.009(5) 0.035(17) Uiso 1 1 d . . . H23 H 0.814(13) -0.112(10) 0.363(5) 0.04(2) Uiso 1 1 d . . . H13 H 0.505(13) 0.252(9) 0.407(5) 0.04(2) 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 0.0388(4) 0.0377(4) 0.0255(4) -0.0017(3) -0.0103(3) -0.0131(3) O11 0.031(2) 0.049(3) 0.028(2) -0.0096(19) -0.0045(18) -0.009(2) O12 0.043(3) 0.075(3) 0.024(2) -0.009(2) -0.008(2) -0.026(3) O13 0.028(2) 0.065(3) 0.042(3) -0.011(2) -0.003(2) -0.016(2) C11 0.033(3) 0.030(3) 0.021(3) 0.001(2) 0.001(2) -0.013(3) C12 0.039(4) 0.060(4) 0.037(3) -0.018(3) 0.002(3) -0.015(3) O21 0.052(3) 0.044(3) 0.032(2) 0.0026(19) -0.017(2) -0.022(2) O22 0.059(3) 0.044(3) 0.056(3) 0.002(2) -0.029(3) -0.027(2) O23 0.046(3) 0.043(3) 0.026(2) -0.002(2) -0.011(2) -0.015(2) C21 0.040(4) 0.038(3) 0.028(3) -0.007(3) -0.008(3) -0.011(3) C22 0.035(3) 0.037(3) 0.030(3) -0.007(3) -0.001(3) -0.009(3) N1 0.031(3) 0.034(3) 0.027(2) -0.004(2) -0.004(2) -0.010(2) N2 0.042(3) 0.039(3) 0.030(3) -0.003(2) -0.004(2) -0.008(3) C1 0.035(3) 0.033(3) 0.028(3) -0.005(2) -0.005(3) -0.009(3) C2 0.035(4) 0.045(4) 0.033(3) -0.011(3) -0.008(3) -0.013(3) C3 0.046(4) 0.036(4) 0.043(3) -0.010(3) -0.001(3) -0.021(3) 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' Cu Cu 0.3201 1.2651 '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' 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 O21 Cu N1 92.56(19) . . ? O21 Cu O11 173.74(19) . . ? N1 Cu O11 93.45(19) . . ? O21 Cu O23 82.06(18) . . ? N1 Cu O23 171.2(2) . . ? O11 Cu O23 91.76(18) . . ? O21 Cu O13 105.03(18) . . ? N1 Cu O13 95.42(19) . . ? O11 Cu O13 76.14(16) . . ? O23 Cu O13 92.66(19) . . ? C11 O11 Cu 123.5(4) . . ? C12 O13 Cu 107.6(4) . . ? O12 C11 O11 122.4(6) . . ? O12 C11 C12 117.4(5) . . ? O11 C11 C12 120.2(5) . . ? O13 C12 C11 112.4(5) . . ? C21 O21 Cu 116.6(4) . . ? C22 O23 Cu 112.6(4) . . ? O22 C21 O21 126.0(6) . . ? O22 C21 C22 116.8(5) . . ? O21 C21 C22 117.2(5) . . ? O23 C22 C21 108.7(5) . . ? C1 N1 C2 105.6(5) . . ? C1 N1 Cu 124.6(4) . . ? C2 N1 Cu 129.8(4) . . ? C1 N2 C3 107.9(5) . . ? N1 C1 N2 111.2(5) . . ? C3 C2 N1 109.6(5) . . ? C2 C3 N2 105.7(5) . . ? 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 O21 1.945(4) . ? Cu N1 1.958(5) . ? Cu O11 1.962(4) . ? Cu O23 1.993(5) . ? Cu O13 2.383(5) . ? O11 C11 1.268(6) . ? O12 C11 1.254(7) . ? O13 C12 1.429(7) . ? C11 C12 1.507(9) . ? O21 C21 1.263(7) . ? O22 C21 1.233(7) . ? O23 C22 1.435(7) . ? C21 C22 1.536(8) . ? N1 C1 1.332(7) . ? N1 C2 1.378(7) . ? N2 C1 1.333(7) . ? N2 C3 1.379(8) . ? C2 C3 1.362(9) . ? 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 N2 H20 O22 0.88(6) 1.91(6) 2.787(7) 174(6) 2_665 O23 H23 O12 0.71(6) 1.94(7) 2.648(6) 170(7) 2_756 O13 H13 O12 0.81(6) 1.98(7) 2.760(6) 161(6) 1_455 C1 H1 O21 0.93 2.50 2.938(7) 109.1 . C3 H3 O22 0.93 2.36 3.215(7) 152.3 1_665