#------------------------------------------------------------------------------ #$Date: 2014-07-11 19:31:04 +0200 (Fri, 11 Jul 2014) $ #$Revision: 120073 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001454.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_4001454 loop_ _publ_author_name 'Kim, Jun-Ho' 'Baek, Jaewook' 'Halasyamani, P. Shiv' _publ_section_title ; (NH4)2Te2WO8:  A New Polar Oxide with Second-Harmonic Generating, Ferroelectric, and Pyroelectric Properties ; _journal_issue 23 _journal_name_full 'Chemistry of Materials' _journal_page_first 5637 _journal_volume 19 _journal_year 2007 _chemical_formula_sum 'H8 N2 O8 Te2 W' _chemical_formula_weight 603.13 _chemical_name_systematic ; Ammonium tungsten tellurite ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 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 99.188(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.9716(9) _cell_length_b 7.0279(9) _cell_length_c 9.4593(13) _cell_measurement_reflns_used 1342 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.14 _cell_measurement_theta_min 2.96 _cell_volume 457.52(10) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _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 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2840 _diffrn_reflns_theta_full 28.33 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_min 2.18 _exptl_absorpt_coefficient_mu 18.895 _exptl_absorpt_correction_T_max 0.9875 _exptl_absorpt_correction_T_min 0.5042 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'psi-scan, (north et al., 1968)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 4.378 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal plates' _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.502 _refine_diff_density_min -1.784 _refine_diff_density_rms 0.299 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.062(11) _refine_ls_extinction_coef 0.0028(2) _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 0.922 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 2025 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.922 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0318 _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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.0607 _reflns_number_gt 1851 _reflns_number_total 2025 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm7019334-file003.cif _[local]_cod_data_source_block 4onab _[local]_cod_cif_authors_sg_H-M P2(1) _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4001454 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -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 W1 W 0.16845(7) 0.07474(6) 0.74068(5) 0.01234(13) Uani 1 1 d Te1 Te -0.03569(11) 0.27601(10) 1.00186(9) 0.01212(19) Uani 1 1 d Te2 Te 0.05225(12) 0.01449(10) 1.35861(9) 0.01436(19) Uani 1 1 d O1 O 0.3107(14) 0.2405(12) 0.6699(11) 0.024(2) Uani 1 1 d O2 O 0.3387(13) -0.0877(12) 0.8292(10) 0.022(2) Uani 1 1 d O3 O 0.0791(14) -0.0649(11) 0.5798(10) 0.018(2) Uani 1 1 d O4 O 0.1977(12) 0.2345(11) 0.9302(9) 0.0132(19) Uani 1 1 d O5 O 0.0734(12) -0.2437(11) 1.3125(9) 0.0143(18) Uani 1 1 d O6 O 0.0502(12) 0.4463(11) 1.1534(9) 0.0137(19) Uani 1 1 d O7 O 0.0199(13) 0.0566(13) 1.1307(8) 0.022(2) Uani 1 1 d O8 O 0.3093(12) 0.0806(15) 1.3772(9) 0.0238(19) Uani 1 1 d N1 N 0.4977(15) -0.4540(15) 0.8629(11) 0.020(2) Uani 1 1 d N2 N 0.6160(16) -0.0198(17) 1.5959(13) 0.028(3) Uani 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 W1 0.0149(3) 0.0126(2) 0.0095(2) 0.0000(2) 0.00207(18) 0.0012(2) Te1 0.0149(4) 0.0115(4) 0.0096(4) -0.0014(3) 0.0010(3) 0.0003(3) Te2 0.0163(4) 0.0110(4) 0.0151(4) -0.0026(3) 0.0003(3) -0.0001(3) O1 0.024(5) 0.020(5) 0.028(6) 0.000(4) 0.007(4) -0.004(4) O2 0.028(6) 0.022(5) 0.011(5) -0.001(4) -0.009(4) 0.004(4) O3 0.031(6) 0.007(4) 0.019(5) 0.001(4) 0.008(4) -0.001(4) O4 0.012(4) 0.015(5) 0.013(5) -0.004(4) 0.005(3) -0.004(4) O5 0.018(5) 0.004(4) 0.017(5) -0.006(4) -0.006(4) 0.005(4) O6 0.019(5) 0.014(4) 0.006(4) -0.004(3) -0.002(3) 0.005(4) O7 0.044(6) 0.014(5) 0.008(4) -0.002(4) 0.007(4) -0.001(5) O8 0.021(5) 0.024(4) 0.025(5) 0.006(5) 0.001(4) -0.010(5) N1 0.018(5) 0.016(7) 0.021(6) -0.002(5) -0.012(4) 0.010(5) N2 0.020(7) 0.029(7) 0.033(7) -0.002(6) 0.001(5) 0.011(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' 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 O1 W1 O2 103.6(4) . . O1 W1 O3 100.3(4) . . O2 W1 O3 99.3(4) . . O1 W1 O4 89.3(4) . . O2 W1 O4 88.5(4) . . O3 W1 O4 165.8(3) . . O1 W1 O5 89.2(4) . 2_557 O2 W1 O5 163.4(4) . 2_557 O3 W1 O5 88.5(4) . 2_557 O4 W1 O5 81.1(3) . 2_557 O1 W1 O6 162.5(4) . 2_547 O2 W1 O6 88.9(4) . 2_547 O3 W1 O6 89.4(3) . 2_547 O4 W1 O6 78.8(3) . 2_547 O5 W1 O6 76.5(3) 2_557 2_547 O4 Te1 O6 100.6(4) . . O4 Te1 O7 90.3(3) . . O6 Te1 O7 91.1(3) . . O4 Te1 O7 79.7(3) . 2_557 O6 Te1 O7 80.6(3) . 2_557 O7 Te1 O7 165.55(13) . 2_557 O8 Te2 O5 98.9(4) . . O8 Te2 O3 92.3(4) . 1_556 O5 Te2 O3 88.7(3) . 1_556 O8 Te2 O7 90.3(3) . . O5 Te2 O7 84.2(3) . . O3 Te2 O7 172.8(3) 1_556 . W1 O3 Te2 129.5(4) . 1_554 Te1 O4 W1 114.8(4) . . Te2 O5 W1 123.4(4) . 2_547 Te1 O6 W1 117.2(4) . 2_557 Te1 O7 Te2 135.1(4) . . Te1 O7 Te1 110.4(3) . 2_547 Te2 O7 Te1 114.4(4) . 2_547 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W1 O1 1.733(9) . W1 O2 1.759(9) . W1 O3 1.834(9) . W1 O4 2.097(8) . W1 O5 2.110(8) 2_557 W1 O6 2.151(8) 2_547 Te1 O4 1.882(8) . Te1 O6 1.890(8) . Te1 O7 1.965(9) . Te1 O7 2.349(9) 2_557 Te2 O8 1.832(8) . Te2 O5 1.878(7) . Te2 O3 2.145(9) 1_556 Te2 O7 2.152(8) . O3 Te2 2.145(9) 1_554 O5 W1 2.110(8) 2_547 O6 W1 2.151(8) 2_557 O7 Te1 2.349(9) 2_547 _journal_paper_doi 10.1021/cm7019334