#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013277.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013277 loop_ _publ_author_name 'Baggio, Ricardo' 'Perec, Mireille' 'Garland, Maria Teresa' _publ_section_title ; Polymeric hexaaquahexakis(\m~3~-2,2'-oxydiacetato)trizinc(II)digadolinium(III) dodecahydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m175 _journal_page_last m177 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Zn3 Gd2 (C4 H4 O5)6 (H2 O)6], 12H2 O' _chemical_formula_moiety 'C24 H36 Gd2 O36 Zn3, 12H2 O' _chemical_formula_sum 'C24 H60 Gd2 O48 Zn3' _chemical_formula_weight 1627.33 _chemical_name_systematic ; hexaaquahexakis(\m~3~-2,2'-oxydiacetato)trizinc(II)digadolinium(III) dodecahydrate ; _space_group_IT_number 192 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6 2c' _symmetry_space_group_name_H-M 'P 6/m c c' _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 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 14.5104(11) _cell_length_b 14.5104(11) _cell_length_c 15.7725(16) _cell_measurement_reflns_used 15357 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.01 _cell_measurement_theta_min 1.62 _cell_volume 2876.0(4) _computing_cell_refinement SMART-NT _computing_data_collection 'SMART-NT (Bruker, 1999)' _computing_data_reduction 'SAINT-NT (Bruker, 1999)' _computing_molecular_graphics 'XP in SHELXTL (Bruker, 1999)' _computing_publication_material 'XP in SHELXTL' _computing_structure_refinement 'XL in SHELXTL (Bruker, 1999)' _computing_structure_solution 'XS in SHELXTL (Bruker, 1999)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-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 0.0911 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 15357 _diffrn_reflns_theta_full 28.01 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 1.62 _diffrn_standards_decay_% <2 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.620 _exptl_absorpt_correction_T_max 0.47 _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker, 1999c)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_description polyhedra _exptl_crystal_F_000 1612 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.779 _refine_diff_density_min -0.722 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 74 _refine_ls_number_reflns 1180 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0316 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ' w = 1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.947P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.0962 _reflns_number_gt 962 _reflns_number_total 1180 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ga1010.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2013277 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' 'y, x, -z-1/2' 'x-y, -y, -z-1/2' '-x, -x+y, -z-1/2' '-y, -x, -z-1/2' '-x+y, y, -z-1/2' 'x, x-y, -z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Gd 0.6667 0.3333 0.2500 0.02765(17) Uani d S 1 Gd Zn 1.0000 0.5000 0.5000 0.0302(2) Uani d S 1 Zn O1 0.80431(19) 0.41954(17) 0.35441(15) 0.0412(5) Uani d . 1 O O2 0.9450(2) 0.56231(18) 0.40957(17) 0.0623(8) Uani d . 1 O O3 0.76513(13) 0.5303(3) 0.2500 0.0407(7) Uani d S 1 O C1 0.8681(3) 0.5181(2) 0.3600(2) 0.0432(7) Uani d . 1 C C2 0.8491(3) 0.5902(3) 0.3049(3) 0.0733(14) Uani d . 1 C H2A 0.8324 0.6350 0.3398 0.088 Uiso calc R 1 H H2B 0.9128 0.6358 0.2726 0.088 Uiso calc R 1 H O1W 0.8555(2) 0.3483(2) 0.5000 0.0408(7) Uiso d S 1 O H1W 0.829(4) 0.367(4) 0.543(3) 0.111(18) Uiso d . 1 H O2WA 0.803(3) 1.033(3) 0.5000 0.150(7) Uiso d SP 0.29(2) O O2WB 0.733(3) 0.920(4) 0.5000 0.150(7) Uiso d SP 0.241(19) O O2WC 0.769(3) 0.977(3) 0.451(3) 0.150(7) Uiso d P 0.198(15) O O2WD 0.845(3) 0.984(2) 0.311(3) 0.150(7) Uiso d P 0.167(11) O O2WE 0.923(3) 1.073(3) 0.379(3) 0.150(7) Uiso d P 0.148(14) O 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 Gd 0.03199(19) 0.03199(19) 0.0190(2) 0.01599(10) 0.000 0.000 Zn 0.0271(3) 0.0366(4) 0.0237(4) 0.0135(3) 0.000 0.000 O1 0.0421(12) 0.0409(11) 0.0356(12) 0.0169(10) -0.0127(10) 0.0003(9) O2 0.0581(16) 0.0468(13) 0.0652(16) 0.0136(12) -0.0350(13) 0.0054(12) O3 0.0461(14) 0.0360(16) 0.0366(17) 0.0180(8) -0.0157(10) 0.000 C1 0.0402(16) 0.0432(17) 0.0387(16) 0.0153(14) -0.0145(13) -0.0004(14) C2 0.071(3) 0.0424(19) 0.085(3) 0.0120(18) -0.052(2) 0.0013(19) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Gd O1 24_556 3_665 126.37(10) O1 Gd O1 24_556 . 87.85(12) O1 Gd O1 3_665 . 78.15(9) O1 Gd O1 24_556 22_666 78.15(9) O1 Gd O1 3_665 22_666 87.85(12) O1 Gd O1 . 22_666 148.78(11) O1 Gd O1 24_556 23_656 78.15(9) O1 Gd O1 3_665 23_656 148.78(11) O1 Gd O1 . 23_656 126.37(10) O1 Gd O1 22_666 23_656 78.15(9) O1 Gd O1 24_556 2_655 148.78(11) O1 Gd O1 3_665 2_655 78.15(9) O1 Gd O1 . 2_655 78.15(9) O1 Gd O1 22_666 2_655 126.37(10) O1 Gd O1 23_656 2_655 87.85(12) O1 Gd O3 24_556 3_665 63.19(5) O1 Gd O3 3_665 3_665 63.19(5) O1 Gd O3 . 3_665 74.39(5) O1 Gd O3 22_666 3_665 74.39(5) O1 Gd O3 23_656 3_665 136.07(6) O1 Gd O3 2_655 3_665 136.07(6) O1 Gd O3 24_556 2_655 136.07(6) O1 Gd O3 3_665 2_655 74.39(5) O1 Gd O3 . 2_655 136.07(6) O1 Gd O3 22_666 2_655 63.19(5) O1 Gd O3 23_656 2_655 74.39(5) O1 Gd O3 2_655 2_655 63.19(5) O3 Gd O3 3_665 2_655 120.0 O1 Gd O3 24_556 . 74.39(5) O1 Gd O3 3_665 . 136.07(6) O1 Gd O3 . . 63.19(5) O1 Gd O3 22_666 . 136.07(6) O1 Gd O3 23_656 . 63.19(5) O1 Gd O3 2_655 . 74.39(5) O3 Gd O3 3_665 . 120.0 O3 Gd O3 2_655 . 120.0 O2 Zn O2 16_556 . 88.08(17) O2 Zn O2 16_556 4_765 180.0 O2 Zn O2 . 4_765 91.92(17) O2 Zn O2 16_556 13_766 91.92(17) O2 Zn O2 . 13_766 180.0 O2 Zn O2 4_765 13_766 88.08(17) O2 Zn O1W 16_556 13_766 86.79(9) O2 Zn O1W . 13_766 86.79(9) O2 Zn O1W 4_765 13_766 93.21(9) O2 Zn O1W 13_766 13_766 93.21(9) O2 Zn O1W 16_556 . 93.21(9) O2 Zn O1W . . 93.21(9) O2 Zn O1W 4_765 . 86.79(9) O2 Zn O1W 13_766 . 86.79(9) O1W Zn O1W 13_766 . 180.0 C2 O3 C2 . 23_656 114.4(4) O2 C1 O1 . . 126.1(3) O2 C1 C2 . . 115.9(3) O1 C1 C2 . . 117.9(3) O3 C2 C1 . . 109.7(3) O3 C2 H2A . . 109.7 C1 C2 H2A . . 109.7 O3 C2 H2B . . 109.7 C1 C2 H2B . . 109.7 H2A C2 H2B . . 108.2 H1W O1W H1W . 16_556 100(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd O1 24_556 2.402(2) ? Gd O1 3_665 2.402(2) ? Gd O1 . 2.402(2) y Gd O1 22_666 2.402(2) ? Gd O1 23_656 2.402(2) ? Gd O1 2_655 2.402(2) ? Gd O3 3_665 2.475(3) ? Gd O3 2_655 2.475(3) ? Gd O3 . 2.475(3) y Zn O2 16_556 2.052(2) ? Zn O2 . 2.052(2) y Zn O2 4_765 2.052(2) ? Zn O2 13_766 2.052(2) ? Zn O1W 13_766 2.152(3) ? Zn O1W . 2.152(3) y O1 C1 . 1.259(4) y O2 C1 . 1.246(3) y O3 C2 . 1.390(4) y O3 C2 23_656 1.390(4) ? C1 C2 . 1.488(4) y C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? O1W H1W . 0.88(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1W O1 16_556 0.88(5) 1.90(5) 2.768(3) 167(4)