#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100158.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 _journal_name_full 'Polyhedron' _journal_volume 23 _journal_page_first 1505 _journal_page_last 1518 _journal_year 2004 _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' ; loop_ _publ_author_name 'Carballo, Rosa' 'Vazquez-Lopez, Ezequiel M.' 'Covelo, Berta' 'Garcia-Martinez, Emilia' 'Castineiras, Alfonso' 'Niclos, Juan' _chemical_formula_sum 'C7 H10 Cu N2 O6' _chemical_formula_weight 281.71 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' _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 5.528(2) _cell_length_b 7.267(3) _cell_length_c 13.626(5) _cell_angle_alpha 75.045(5) _cell_angle_beta 85.826(6) _cell_angle_gamma 75.613(7) _cell_volume 512.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 451 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 22.80 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 286 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6652 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2335 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.07 _reflns_number_total 1984 _reflns_number_gt 1472 _reflns_threshold_expression >2sigma(I) _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^)+(0.0385P)^2^+1.3732P] 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 1984 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1157 _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 0.85489(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) _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 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_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_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 _diffrn_measured_fraction_theta_max 0.795 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.795 _refine_diff_density_max 0.666 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.103 _cod_database_code 1100158