#------------------------------------------------------------------------------ #$Date: 2010-09-26 12:00:33 +0100 (Sun, 26 Sep 2010) $ #$Revision: 1526 $ #$URL: svn://www.crystallography.net/cod/cif/4/4308966.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_4308966 loop_ _publ_author_name 'Kang Min Ok' 'P. Shiv Halasyamani' _publ_contact_author_address ; Department of Chemistry University of Houston 4800 Calhoun TX 77204-5003 USA ; _publ_contact_author_email psh@uh.edu _publ_contact_author_fax 1(713)7432787 _publ_contact_author_name 'P. Shiv Halasyamani' _publ_contact_author_phone 1(713)7433278 _publ_section_title ; New d0 Transition Metal Iodates: Synthesis, Structure, and Characterization of BaTi(IO3)6, LaTiO(IO3)5, Ba2VO2(IO3)4.(IO3), K2MoO2(IO3)4, and BaMoO2(IO3)4.H2O ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2263 _journal_page_last 2271 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'I5 La O16 Ti' _chemical_formula_weight 1077.31 _chemical_name_systematic ; Lathanum Titanium Iodate ; _space_group_IT_number 14 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 91.742(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.4798(10) _cell_length_b 18.065(2) _cell_length_c 10.4843(14) _cell_measurement_temperature 293.0(2) _cell_volume 1416.0(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293.0(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.941 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8650 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_min 2.25 _exptl_absorpt_coefficient_mu 14.528 _exptl_absorpt_correction_T_max 0.175 _exptl_absorpt_correction_T_min 0.077 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 5.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1888 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.576 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.245 _refine_ls_extinction_coef 0.00212(10) _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 1.186 _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 3215 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.186 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0286 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+87.5275P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.0768 _reflns_number_gt 3093 _reflns_number_total 3215 _reflns_threshold_expression >2\(I) _[local]_cod_data_source_file ic048428csi20041110_031926_3.cif _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 4308966 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 La1 La -0.25928(5) 0.26623(2) 0.76010(4) 0.01100(11) Uani 1 1 d . . . I1 I 0.09448(6) 0.37663(2) 0.56406(4) 0.01151(11) Uani 1 1 d . . . I2 I 0.27673(6) 0.17715(2) 0.60130(4) 0.01218(12) Uani 1 1 d . . . I3 I 0.57132(6) 0.36894(2) 0.45025(4) 0.01167(11) Uani 1 1 d . . . I4 I 0.22839(6) 0.50487(2) 0.24450(4) 0.01161(11) Uani 1 1 d . . . I5 I 0.22870(6) -0.16274(2) 0.56431(4) 0.01241(12) Uani 1 1 d . . . Ti1 Ti 0.26756(16) 0.50166(6) 0.76437(12) 0.0119(2) Uani 1 1 d . . . O1 O 0.2960(6) 0.4124(3) 0.6479(5) 0.0138(9) Uani 1 1 d . . . O2 O 0.2127(7) 0.3058(3) 0.4745(5) 0.0173(10) Uani 1 1 d . . . O3 O -0.0035(6) 0.5230(3) 0.3007(5) 0.0184(10) Uani 1 1 d . . . O4 O 0.0335(7) 0.3139(3) 0.6891(5) 0.0167(10) Uani 1 1 d . . . O5 O 0.3959(7) 0.1764(3) 0.4533(5) 0.0165(10) Uani 1 1 d . . . O6 O 0.3442(7) 0.0824(3) 0.6402(5) 0.0237(12) Uani 1 1 d . . . O7 O 0.4295(7) 0.2268(3) 0.7051(5) 0.0212(11) Uani 1 1 d . . . O8 O 0.7245(7) 0.3013(3) 0.5215(5) 0.0196(11) Uani 1 1 d . . . O9 O 0.7429(7) 0.4306(3) 0.3916(5) 0.0211(11) Uani 1 1 d . . . O10 O 0.5215(7) 0.3176(3) 0.3063(5) 0.0147(10) Uani 1 1 d . . . O11 O 0.3036(7) 0.5950(3) 0.2977(5) 0.0182(10) Uani 1 1 d . . . O12 O 0.2819(7) 0.4480(3) 0.3801(5) 0.0243(12) Uani 1 1 d . . . O13 O 0.4890(6) 0.5149(3) 0.7956(5) 0.0194(11) Uani 1 1 d . . . O14 O 0.2281(7) -0.1590(3) 0.3925(5) 0.0182(10) Uani 1 1 d . . . O15 O 0.2715(7) -0.0642(3) 0.5873(5) 0.0189(10) Uani 1 1 d . . . O16 O -0.0103(7) -0.1672(3) 0.5886(5) 0.0210(11) 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 La1 0.01158(19) 0.01088(19) 0.01048(19) -0.00016(13) -0.00049(13) -0.00081(13) I1 0.0120(2) 0.0099(2) 0.0126(2) -0.00035(14) 0.00021(15) 0.00010(14) I2 0.0120(2) 0.0132(2) 0.0113(2) 0.00027(15) -0.00009(15) -0.00166(15) I3 0.0132(2) 0.0105(2) 0.0112(2) -0.00044(14) -0.00018(15) 0.00026(14) I4 0.0113(2) 0.0104(2) 0.0130(2) -0.00040(14) 0.00004(15) 0.00071(14) I5 0.0133(2) 0.0120(2) 0.0119(2) -0.00142(14) -0.00122(15) -0.00051(15) Ti1 0.0122(6) 0.0096(5) 0.0139(6) -0.0001(4) 0.0013(4) -0.0005(4) O1 0.012(2) 0.012(2) 0.017(2) -0.0005(18) 0.0001(18) 0.0017(17) O2 0.022(3) 0.012(2) 0.017(2) -0.0037(19) 0.004(2) 0.002(2) O3 0.011(2) 0.018(3) 0.026(3) -0.006(2) 0.0072(19) 0.0025(19) O4 0.018(2) 0.012(2) 0.021(3) 0.0070(19) 0.005(2) -0.0008(18) O5 0.020(3) 0.019(2) 0.010(2) 0.0041(18) 0.0042(19) 0.0023(19) O6 0.023(3) 0.017(3) 0.031(3) 0.012(2) 0.005(2) 0.001(2) O7 0.017(2) 0.026(3) 0.020(3) -0.010(2) -0.004(2) -0.006(2) O8 0.029(3) 0.011(2) 0.018(2) -0.0027(19) -0.007(2) 0.004(2) O9 0.024(3) 0.018(3) 0.022(3) 0.007(2) -0.004(2) -0.004(2) O10 0.018(2) 0.012(2) 0.014(2) -0.0035(18) -0.0005(18) -0.0013(19) O11 0.019(3) 0.009(2) 0.026(3) -0.0030(19) -0.001(2) -0.0027(19) O12 0.024(3) 0.023(3) 0.026(3) 0.015(2) 0.009(2) 0.008(2) O13 0.010(2) 0.022(3) 0.025(3) -0.001(2) -0.002(2) -0.003(2) O14 0.027(3) 0.017(3) 0.011(2) 0.0009(18) -0.003(2) 0.003(2) O15 0.024(3) 0.015(2) 0.018(2) -0.0048(19) 0.007(2) -0.004(2) O16 0.013(2) 0.027(3) 0.023(3) 0.002(2) -0.002(2) -0.005(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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 O7 La1 O4 148.93(17) 1_455 . ? O7 La1 O5 135.05(17) 1_455 4_566 ? O4 La1 O5 73.19(17) . 4_566 ? O7 La1 O14 74.78(17) 1_455 3_556 ? O4 La1 O14 88.68(17) . 3_556 ? O5 La1 O14 140.61(16) 4_566 3_556 ? O7 La1 O8 80.17(17) 1_455 1_455 ? O4 La1 O8 68.95(17) . 1_455 ? O5 La1 O8 133.14(16) 4_566 1_455 ? O14 La1 O8 65.00(16) 3_556 1_455 ? O7 La1 O11 96.33(17) 1_455 3_566 ? O4 La1 O11 72.75(16) . 3_566 ? O5 La1 O11 81.01(16) 4_566 3_566 ? O14 La1 O11 127.26(16) 3_556 3_566 ? O8 La1 O11 62.27(16) 1_455 3_566 ? O7 La1 O2 87.57(17) 1_455 4_566 ? O4 La1 O2 121.63(16) . 4_566 ? O5 La1 O2 63.96(16) 4_566 4_566 ? O14 La1 O2 100.03(16) 3_556 4_566 ? O8 La1 O2 162.64(16) 1_455 4_566 ? O11 La1 O2 131.97(16) 3_566 4_566 ? O7 La1 O10 128.06(17) 1_455 4_566 ? O4 La1 O10 63.12(16) . 4_566 ? O5 La1 O10 75.11(16) 4_566 4_566 ? O14 La1 O10 65.49(16) 3_556 4_566 ? O8 La1 O10 109.56(16) 1_455 4_566 ? O11 La1 O10 134.12(16) 3_566 4_566 ? O2 La1 O10 68.79(15) 4_566 4_566 ? O7 La1 O16 69.45(17) 1_455 2_456 ? O4 La1 O16 127.82(17) . 2_456 ? O5 La1 O16 68.12(16) 4_566 2_456 ? O14 La1 O16 142.79(17) 3_556 2_456 ? O8 La1 O16 117.00(16) 1_455 2_456 ? O11 La1 O16 67.87(17) 3_566 2_456 ? O2 La1 O16 69.02(16) 4_566 2_456 ? O10 La1 O16 132.83(16) 4_566 2_456 ? O4 I1 O2 94.0(2) . . ? O4 I1 O1 95.5(2) . . ? O2 I1 O1 95.1(2) . . ? O4 I1 O3 87.9(2) . 3_566 ? O2 I1 O3 167.5(2) . 3_566 ? O1 I1 O3 72.36(19) . 3_566 ? O7 I2 O5 101.7(2) . . ? O7 I2 O6 99.6(3) . . ? O5 I2 O6 92.6(2) . . ? O10 I3 O8 96.3(2) . . ? O10 I3 O9 99.3(2) . . ? O8 I3 O9 96.2(2) . . ? O12 I4 O11 102.2(3) . . ? O12 I4 O3 92.1(2) . . ? O11 I4 O3 91.6(2) . . ? O12 I4 O13 82.3(2) . 3_666 ? O11 I4 O13 85.0(2) . 3_666 ? O3 I4 O13 172.7(2) . 3_666 ? O14 I5 O16 99.8(2) . . ? O14 I5 O15 95.2(2) . . ? O16 I5 O15 101.2(2) . . ? O13 Ti1 O6 103.0(2) . 2_556 ? O13 Ti1 O15 95.7(2) . 2_556 ? O6 Ti1 O15 88.4(2) 2_556 2_556 ? O13 Ti1 O1 96.2(2) . . ? O6 Ti1 O1 160.8(2) 2_556 . ? O15 Ti1 O1 90.9(2) 2_556 . ? O13 Ti1 O9 94.8(2) . 3_666 ? O6 Ti1 O9 87.5(2) 2_556 3_666 ? O15 Ti1 O9 169.3(2) 2_556 3_666 ? O1 Ti1 O9 89.8(2) . 3_666 ? O13 Ti1 O3 171.2(2) . 3_566 ? O6 Ti1 O3 85.0(2) 2_556 3_566 ? O15 Ti1 O3 88.2(2) 2_556 3_566 ? O1 Ti1 O3 75.75(19) . 3_566 ? O9 Ti1 O3 81.7(2) 3_666 3_566 ? I1 O1 Ti1 117.7(2) . . ? I1 O2 La1 147.4(3) . 4_665 ? I4 O3 Ti1 136.4(3) . 3_566 ? I4 O3 I1 126.5(2) . 3_566 ? Ti1 O3 I1 94.04(18) 3_566 3_566 ? I1 O4 La1 132.8(3) . . ? I2 O5 La1 117.2(2) . 4_665 ? I2 O6 Ti1 133.5(3) . 2_546 ? I2 O7 La1 149.2(3) . 1_655 ? I3 O8 La1 125.0(3) . 1_655 ? I3 O9 Ti1 128.8(3) . 3_666 ? I3 O10 La1 126.6(2) . 4_665 ? I4 O11 La1 139.6(3) . 3_566 ? Ti1 O13 I4 151.6(3) . 3_666 ? I5 O14 La1 127.3(2) . 3_556 ? I5 O15 Ti1 131.2(3) . 2_546 ? I5 O16 La1 139.6(3) . 2_446 ? 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 La1 O7 2.486(5) 1_455 ? La1 O4 2.488(5) . ? La1 O5 2.526(5) 4_566 ? La1 O14 2.528(5) 3_556 ? La1 O8 2.580(5) 1_455 ? La1 O11 2.597(5) 3_566 ? La1 O2 2.611(5) 4_566 ? La1 O10 2.622(5) 4_566 ? La1 O16 2.664(5) 2_456 ? I1 O4 1.802(5) . ? I1 O2 1.831(5) . ? I1 O1 1.839(5) . ? I1 O3 2.412(5) 3_566 ? I2 O7 1.794(5) . ? I2 O5 1.812(5) . ? I2 O6 1.826(5) . ? I3 O10 1.801(5) . ? I3 O8 1.819(5) . ? I3 O9 1.820(5) . ? I4 O12 1.789(5) . ? I4 O11 1.806(5) . ? I4 O3 1.878(5) . ? I4 O13 2.197(5) 3_666 ? I5 O14 1.803(5) . ? I5 O16 1.815(5) . ? I5 O15 1.823(5) . ? Ti1 O13 1.695(5) . ? Ti1 O6 1.970(5) 2_556 ? Ti1 O15 1.987(5) 2_556 ? Ti1 O1 2.038(5) . ? Ti1 O9 2.042(5) 3_666 ? Ti1 O3 2.117(5) 3_566 ? O2 La1 2.611(5) 4_665 ? O3 Ti1 2.117(5) 3_566 ? O3 I1 2.412(5) 3_566 ? O5 La1 2.526(5) 4_665 ? O6 Ti1 1.970(5) 2_546 ? O7 La1 2.486(5) 1_655 ? O8 La1 2.580(5) 1_655 ? O9 Ti1 2.042(5) 3_666 ? O10 La1 2.622(5) 4_665 ? O11 La1 2.597(5) 3_566 ? O13 I4 2.197(5) 3_666 ? O14 La1 2.528(5) 3_556 ? O15 Ti1 1.987(5) 2_546 ? O16 La1 2.664(5) 2_446 ?