#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100162.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_1100162 _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 'C14 H22 N4 O6 Zn' _chemical_formula_weight 407.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 10.7634(9) _cell_length_b 10.7634(9) _cell_length_c 16.442(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1904.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.11 _exptl_crystal_description octahedral _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type MULTISCAN _exptl_absorpt_correction_T_min 0.9429 _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 8295 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1366 _reflns_number_gt 1276 _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^)+(0.0477P)^2^+0.5646P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(3) _refine_ls_number_reflns 1366 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _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 Zn Zn 0.25021(3) 0.74979(3) 0.2500 0.0288(2) Uani 1 2 d S . . O11 O 0.2538(2) 0.5604(2) 0.28451(13) 0.0410(6) Uani 1 1 d . . . O12 O 0.2248(2) 0.3656(2) 0.24867(14) 0.0437(6) Uani 1 1 d . . . O13 O 0.1980(3) 0.6502(2) 0.14469(15) 0.0461(7) Uani 1 1 d . . . C11 C 0.2317(3) 0.4799(3) 0.23344(19) 0.0304(8) Uani 1 1 d . . . C12 C 0.2078(4) 0.5175(3) 0.1450(2) 0.0426(10) Uani 1 1 d . . . C13 C 0.3161(5) 0.4769(5) 0.0941(3) 0.0815(17) Uani 1 1 d . . . H13A H 0.3045 0.5048 0.0391 0.122 Uiso 1 1 calc R . . H13B H 0.3218 0.3879 0.0949 0.122 Uiso 1 1 calc R . . H13C H 0.3912 0.5120 0.1156 0.122 Uiso 1 1 calc R . . C14 C 0.0862(5) 0.4616(4) 0.1159(3) 0.0783(16) Uani 1 1 d . . . H14A H 0.0203 0.4865 0.1517 0.117 Uiso 1 1 calc R . . H14B H 0.0927 0.3727 0.1157 0.117 Uiso 1 1 calc R . . H14C H 0.0688 0.4904 0.0618 0.117 Uiso 1 1 calc R . . N1 N 0.0739(2) 0.7635(3) 0.30306(17) 0.0418(7) Uani 1 1 d . . . N2 N -0.1284(3) 0.7657(4) 0.3111(2) 0.0582(10) Uani 1 1 d . . . C1 C -0.0305(3) 0.7539(4) 0.2636(2) 0.0462(9) Uani 1 1 d . . . H1 H -0.0355 0.7402 0.2078 0.055 Uiso 1 1 calc R . . C2 C 0.0388(4) 0.7857(6) 0.3799(3) 0.087(2) Uani 1 1 d . . . H2 H 0.0930 0.7988 0.4231 0.104 Uiso 1 1 calc R . . C3 C -0.0855(4) 0.7864(6) 0.3858(3) 0.095(2) Uani 1 1 d . . . H3 H -0.1322 0.7989 0.4327 0.114 Uiso 1 1 calc R . . H13 H 0.181(5) 0.680(5) 0.090(4) 0.105(18) Uiso 1 1 d . . . H20 H -0.194(4) 0.782(4) 0.286(3) 0.065(13) 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 Zn 0.0282(2) 0.0282(2) 0.0302(3) -0.00220(15) -0.00220(15) 0.0000(3) O11 0.0603(16) 0.0320(13) 0.0307(12) 0.0011(10) -0.0066(12) -0.0004(13) O12 0.0653(18) 0.0294(13) 0.0363(12) 0.0018(10) 0.0007(14) -0.0008(12) O13 0.0758(19) 0.0285(14) 0.0341(13) 0.0020(12) -0.0154(12) -0.0021(12) C11 0.038(2) 0.0239(17) 0.0296(16) 0.0003(14) 0.0007(17) 0.0017(15) C12 0.065(3) 0.027(2) 0.0364(19) -0.0006(16) -0.0056(17) -0.0016(16) C13 0.131(5) 0.058(3) 0.056(3) 0.004(2) 0.035(3) 0.019(3) C14 0.102(4) 0.052(3) 0.080(3) 0.013(3) -0.045(3) -0.024(3) N1 0.0310(16) 0.0494(19) 0.0449(18) 0.0011(16) 0.0000(13) 0.0006(15) N2 0.0265(17) 0.091(3) 0.058(2) -0.003(2) -0.0049(16) 0.005(2) C1 0.0315(19) 0.063(3) 0.0438(19) 0.001(2) -0.0057(16) 0.0058(19) C2 0.036(3) 0.176(7) 0.047(3) -0.027(3) -0.002(2) -0.008(3) C3 0.047(3) 0.185(7) 0.054(3) -0.019(3) 0.006(2) 0.003(4) _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 Zn N1 2.094(3) 8_665 ? Zn N1 2.094(3) . ? Zn O13 2.113(2) 8_665 ? Zn O13 2.113(2) . ? Zn O11 2.117(2) . ? Zn O11 2.117(2) 8_665 ? O11 C11 1.230(4) . ? O12 C11 1.258(4) . ? O13 C12 1.432(4) . ? C11 C12 1.531(5) . ? C12 C13 1.500(6) . ? C12 C14 1.518(6) . ? N1 C1 1.302(4) . ? N1 C2 1.341(5) . ? N2 C1 1.318(5) . ? N2 C3 1.331(6) . ? C2 C3 1.341(6) . ? 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 Zn N1 92.63(16) 8_665 . ? N1 Zn O13 97.83(11) 8_665 8_665 ? N1 Zn O13 95.73(10) . 8_665 ? N1 Zn O13 95.73(10) 8_665 . ? N1 Zn O13 97.83(11) . . ? O13 Zn O13 160.32(14) 8_665 . ? N1 Zn O11 170.40(10) 8_665 . ? N1 Zn O11 88.44(10) . . ? O13 Zn O11 91.55(9) 8_665 . ? O13 Zn O11 74.68(9) . . ? N1 Zn O11 88.44(10) 8_665 8_665 ? N1 Zn O11 170.40(10) . 8_665 ? O13 Zn O11 74.68(9) 8_665 8_665 ? O13 Zn O11 91.55(9) . 8_665 ? O11 Zn O11 92.09(14) . 8_665 ? C11 O11 Zn 119.46(19) . . ? C12 O13 Zn 118.9(2) . . ? O11 C11 O12 124.4(3) . . ? O11 C11 C12 119.7(3) . . ? O12 C11 C12 116.0(3) . . ? O13 C12 C13 110.2(4) . . ? O13 C12 C14 109.3(3) . . ? C13 C12 C14 112.2(4) . . ? O13 C12 C11 106.2(3) . . ? C13 C12 C11 108.8(3) . . ? C14 C12 C11 109.9(3) . . ? C1 N1 C2 103.9(3) . . ? C1 N1 Zn 124.7(2) . . ? C2 N1 Zn 131.4(3) . . ? C1 N2 C3 106.6(3) . . ? N1 C1 N2 112.8(3) . . ? N1 C2 C3 110.5(4) . . ? N2 C3 C2 106.2(4) . . ? 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 C2 H2 O12 0.93 2.45 3.346(5) 161.2 7 O13 H13 O12 0.98(6) 1.65(6) 2.623(3) 173(5) 2_554 N2 H20 O12 0.84(5) 1.93(5) 2.737(4) 160(4) 8_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.662 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.057 _cod_database_code 1100162