# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'P. Shiv Halasyamani' 'Alex Gittens' 'Kang Min Ok' 'Lei Zhang' _publ_contact_author_name 'Halasyamani, P. Shiv' _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_phone 1(713)7433278 _publ_requested_journal 'Journal of Materials Chemistry' #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; Synthesis, characterization, and dielectric properties of two new antimony oxides – LaSb3O9 and LaSb5O12: Transformation of three-dimensional LaSb3O9 to two-dimensional LaSb5O12 ; data_compound_1 _database_code_CSD 218480 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Lanthanum antimony oxide ; _chemical_formula_sum 'La O9 Sb3' _chemical_formula_weight 648.16 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 5.5210(8) _cell_length_b 11.8274(17) _cell_length_c 5.5250(8) _cell_angle_alpha 90 _cell_angle_beta 107.257(2) _cell_angle_gamma 90 _cell_volume 344.54(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 3.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 282 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.868 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_number 2107 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.83 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _reflns_number_total 812 _reflns_number_gt 805 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0650P)^2^+6.5982P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.104(7) _refine_ls_number_reflns 812 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.135 _refine_ls_goodness_of_fit_ref 1.304 _refine_ls_restrained_S_all 1.304 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 2.735 _refine_diff_density_min -2.845 _refine_diff_density_rms 0.638 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' Sb Sb -0.5866 1.5461 '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_ _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 0.25512(17) 0.25 0.74499(17) 0.0122(4) Uani 1 2 d S . . Sb1 Sb 0.37803(11) 0.59158(6) 0.62145(11) 0.0074(4) Uani 1 1 d . . . Sb2 Sb 0 0.5 1 0.0074(4) Uani 1 2 d S . . O1 O 0.6921(14) 0.5986(7) 0.9130(14) 0.0109(15) Uani 1 1 d . . . O2 O 0.0857(13) 0.5985(7) 0.3080(14) 0.0109(15) Uani 1 1 d . . . O3 O 0.3992(14) 0.4254(7) 0.6046(14) 0.0092(15) Uani 1 1 d . . . O4 O 0.439(2) 0.75 0.562(2) 0.008(2) Uani 1 2 d S . . O5 O 0.1627(15) 0.6150(7) 0.8300(15) 0.0124(15) 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 0.0148(6) 0.0081(6) 0.0157(6) 0 0.0078(4) 0 Sb1 0.0074(5) 0.0068(5) 0.0078(5) -0.0004(2) 0.0020(3) -0.0004(2) Sb2 0.0073(6) 0.0072(6) 0.0075(6) 0.0002(3) 0.0020(4) 0.0003(3) O1 0.008(3) 0.011(4) 0.011(3) -0.004(3) -0.003(3) 0.002(3) O2 0.007(3) 0.014(4) 0.010(3) 0.002(3) 0.001(3) 0.005(3) O3 0.010(3) 0.005(3) 0.012(3) -0.004(3) 0.003(3) -0.003(3) O4 0.006(4) 0.001(4) 0.019(5) 0 0.003(4) 0 O5 0.015(3) 0.007(4) 0.014(3) 0.003(3) 0.004(3) 0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 La1 O3 2.429(9) 4_565 ? La1 O3 2.429(9) . ? La1 O2 2.552(8) 2_546 ? La1 O2 2.552(7) 3_566 ? La1 O1 2.556(7) 3_667 ? La1 O1 2.556(7) 2_647 ? La1 O4 2.725(11) 3_666 ? La1 Sb2 3.7268(7) 2_547 ? La1 Sb2 3.7268(7) . ? La1 Sb1 3.7610(10) 2_646 ? La1 Sb1 3.7610(10) 3_666 ? Sb1 O5 1.905(9) . ? Sb1 O4 1.949(3) . ? Sb1 O3 1.973(9) . ? Sb1 O1 1.988(7) . ? Sb1 O2 1.988(7) . ? Sb1 O3 2.006(8) 3_666 ? Sb1 Sb1 3.0626(13) 3_666 ? Sb1 La1 3.7610(10) 3_666 ? Sb2 O1 1.999(7) 3_667 ? Sb2 O1 1.999(7) 1_455 ? Sb2 O2 2.000(8) 3_566 ? Sb2 O2 2.000(8) 1_556 ? Sb2 O5 2.010(9) 3_567 ? Sb2 O5 2.010(9) . ? Sb2 La1 3.7268(7) 3_567 ? O1 Sb2 1.999(7) 1_655 ? O1 La1 2.556(7) 3_667 ? O2 Sb2 2.000(8) 1_554 ? O2 La1 2.552(7) 3_566 ? O3 Sb1 2.006(7) 3_666 ? O4 Sb1 1.949(3) 4_575 ? O4 La1 2.725(11) 3_666 ? 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 O3 La1 O3 117.2(4) 4_565 . ? O3 La1 O2 70.4(2) 4_565 2_546 ? O3 La1 O2 149.7(2) . 2_546 ? O3 La1 O2 149.7(2) 4_565 3_566 ? O3 La1 O2 70.4(2) . 3_566 ? O2 La1 O2 89.2(4) 2_546 3_566 ? O3 La1 O1 149.0(2) 4_565 3_667 ? O3 La1 O1 70.2(2) . 3_667 ? O2 La1 O1 119.7(2) 2_546 3_667 ? O2 La1 O1 60.8(3) 3_566 3_667 ? O3 La1 O1 70.2(2) 4_565 2_647 ? O3 La1 O1 149.0(2) . 2_647 ? O2 La1 O1 60.8(3) 2_546 2_647 ? O2 La1 O1 119.7(2) 3_566 2_647 ? O1 La1 O1 88.9(3) 3_667 2_647 ? O3 La1 O4 58.62(18) 4_565 3_666 ? O3 La1 O4 58.62(18) . 3_666 ? O2 La1 O4 120.0(2) 2_546 3_666 ? O2 La1 O4 120.0(2) 3_566 3_666 ? O1 La1 O4 120.3(2) 3_667 3_666 ? O1 La1 O4 120.3(2) 2_647 3_666 ? O3 La1 Sb2 68.88(18) 4_565 2_547 ? O3 La1 Sb2 173.88(18) . 2_547 ? O2 La1 Sb2 30.42(17) 2_546 2_547 ? O2 La1 Sb2 104.60(18) 3_566 2_547 ? O1 La1 Sb2 104.43(18) 3_667 2_547 ? O1 La1 Sb2 30.44(17) 2_647 2_547 ? O4 La1 Sb2 127.496(12) 3_666 2_547 ? O3 La1 Sb2 173.88(18) 4_565 . ? O3 La1 Sb2 68.88(18) . . ? O2 La1 Sb2 104.60(18) 2_546 . ? O2 La1 Sb2 30.42(17) 3_566 . ? O1 La1 Sb2 30.44(17) 3_667 . ? O1 La1 Sb2 104.43(18) 2_647 . ? O4 La1 Sb2 127.496(12) 3_666 . ? Sb2 La1 Sb2 105.01(2) 2_547 . ? O3 La1 Sb1 28.74(18) 4_565 2_646 ? O3 La1 Sb1 88.50(18) . 2_646 ? O2 La1 Sb1 94.87(17) 2_546 2_646 ? O2 La1 Sb1 141.69(17) 3_566 2_646 ? O1 La1 Sb1 141.76(17) 3_667 2_646 ? O1 La1 Sb1 95.02(18) 2_647 2_646 ? O4 La1 Sb1 29.882(13) 3_666 2_646 ? Sb2 La1 Sb1 97.615(14) 2_547 2_646 ? Sb2 La1 Sb1 157.38(2) . 2_646 ? O3 La1 Sb1 88.50(18) 4_565 3_666 ? O3 La1 Sb1 28.74(18) . 3_666 ? O2 La1 Sb1 141.69(17) 2_546 3_666 ? O2 La1 Sb1 94.87(17) 3_566 3_666 ? O1 La1 Sb1 95.02(18) 3_667 3_666 ? O1 La1 Sb1 141.76(17) 2_647 3_666 ? O4 La1 Sb1 29.882(13) 3_666 3_666 ? Sb2 La1 Sb1 157.38(2) 2_547 3_666 ? Sb2 La1 Sb1 97.615(14) . 3_666 ? Sb1 La1 Sb1 59.76(3) 2_646 3_666 ? O5 Sb1 O4 97.6(4) . . ? O5 Sb1 O3 103.3(3) . . ? O4 Sb1 O3 159.1(4) . . ? O5 Sb1 O1 93.1(3) . . ? O4 Sb1 O1 86.7(4) . . ? O3 Sb1 O1 91.7(3) . . ? O5 Sb1 O2 91.7(3) . . ? O4 Sb1 O2 87.2(4) . . ? O3 Sb1 O2 92.5(3) . . ? O1 Sb1 O2 172.6(3) . . ? O5 Sb1 O3 177.2(3) . 3_666 ? O4 Sb1 O3 79.8(4) . 3_666 ? O3 Sb1 O3 79.4(4) . 3_666 ? O1 Sb1 O3 87.7(3) . 3_666 ? O2 Sb1 O3 87.2(3) . 3_666 ? O5 Sb1 Sb1 143.3(3) . 3_666 ? O4 Sb1 Sb1 119.1(3) . 3_666 ? O3 Sb1 Sb1 40.1(2) . 3_666 ? O1 Sb1 Sb1 89.6(2) . 3_666 ? O2 Sb1 Sb1 89.8(2) . 3_666 ? O3 Sb1 Sb1 39.3(2) 3_666 3_666 ? O5 Sb1 La1 141.7(3) . 3_666 ? O4 Sb1 La1 44.2(3) . 3_666 ? O3 Sb1 La1 115.0(2) . 3_666 ? O1 Sb1 La1 86.3(2) . 3_666 ? O2 Sb1 La1 86.5(2) . 3_666 ? O3 Sb1 La1 35.6(2) 3_666 3_666 ? Sb1 Sb1 La1 74.90(3) 3_666 3_666 ? O1 Sb2 O1 180.000(2) 3_667 1_455 ? O1 Sb2 O2 80.5(3) 3_667 3_566 ? O1 Sb2 O2 99.5(3) 1_455 3_566 ? O1 Sb2 O2 99.5(3) 3_667 1_556 ? O1 Sb2 O2 80.5(3) 1_455 1_556 ? O2 Sb2 O2 180.000(2) 3_566 1_556 ? O1 Sb2 O5 87.6(3) 3_667 3_567 ? O1 Sb2 O5 92.4(3) 1_455 3_567 ? O2 Sb2 O5 88.7(3) 3_566 3_567 ? O2 Sb2 O5 91.3(3) 1_556 3_567 ? O1 Sb2 O5 92.4(3) 3_667 . ? O1 Sb2 O5 87.6(3) 1_455 . ? O2 Sb2 O5 91.3(3) 3_566 . ? O2 Sb2 O5 88.7(3) 1_556 . ? O5 Sb2 O5 180.0(4) 3_567 . ? O1 Sb2 La1 139.6(2) 3_667 3_567 ? O1 Sb2 La1 40.4(2) 1_455 3_567 ? O2 Sb2 La1 139.8(2) 3_566 3_567 ? O2 Sb2 La1 40.2(2) 1_556 3_567 ? O5 Sb2 La1 95.1(2) 3_567 3_567 ? O5 Sb2 La1 84.9(2) . 3_567 ? O1 Sb2 La1 40.4(2) 3_667 . ? O1 Sb2 La1 139.6(2) 1_455 . ? O2 Sb2 La1 40.2(2) 3_566 . ? O2 Sb2 La1 139.8(2) 1_556 . ? O5 Sb2 La1 84.9(2) 3_567 . ? O5 Sb2 La1 95.1(2) . . ? La1 Sb2 La1 180 3_567 . ? Sb1 O1 Sb2 130.2(4) . 1_655 ? Sb1 O1 La1 120.6(3) . 3_667 ? Sb2 O1 La1 109.2(3) 1_655 3_667 ? Sb1 O2 Sb2 130.0(4) . 1_554 ? Sb1 O2 La1 120.6(3) . 3_566 ? Sb2 O2 La1 109.3(3) 1_554 3_566 ? Sb1 O3 Sb1 100.6(4) . 3_666 ? Sb1 O3 La1 143.7(4) . . ? Sb1 O3 La1 115.6(4) 3_666 . ? Sb1 O4 Sb1 148.1(6) 4_575 . ? Sb1 O4 La1 106.0(3) 4_575 3_666 ? Sb1 O4 La1 106.0(3) . 3_666 ? Sb1 O5 Sb2 129.0(5) . . ? #===END data_compound_2 _database_code_CSD 218481 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Lanthanum antimony oxide ; _chemical_formula_sum 'La O12 Sb5' _chemical_formula_weight 939.66 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 7.2707(7) _cell_length_b 7.2707(7) _cell_length_c 16.4673(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 753.89(12) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 6.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 17.466 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_number 1549 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 251 _reflns_number_gt 251 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0183P)^2^+20.2026P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0158(8) _refine_ls_number_reflns 251 _refine_ls_number_parameters 23 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.023 _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.481 _refine_ls_restrained_S_all 1.481 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.669 _refine_diff_density_min -2.277 _refine_diff_density_rms 0.304 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' Sb Sb -0.5866 1.5461 '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_ _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 0.3333 0.6667 0.1667 0.0071(3) Uani 1 12 d S . . Sb1 Sb 0 0 0.15170(5) 0.0073(3) Uani 1 6 d S . . Sb2 Sb 0.1667 0.3333 0.3333 0.0055(3) Uani 1 4 d S . . O1 O 0.2513(10) 0.1256(5) 0.3657(3) 0.0096(12) Uani 1 2 d S . . O2 O 0.1315(5) 0.2629(10) 0.2168(3) 0.0110(12) Uani 1 2 d S . . 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 0.0083(4) 0.0083(4) 0.0047(5) 0 0 0.0041(2) Sb1 0.0080(4) 0.0080(4) 0.0058(5) 0 0 0.00401(19) Sb2 0.0064(4) 0.0050(4) 0.0048(4) 0.0003(2) 0.00017(12) 0.0025(2) O1 0.015(3) 0.0083(19) 0.008(2) 0.0000(11) 0.000(2) 0.0076(16) O2 0.014(2) 0.009(3) 0.008(2) 0.000(2) -0.0001(11) 0.0043(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 La1 O2 2.673(6) 27 ? La1 O2 2.673(6) 3_565 ? La1 O2 2.673(6) 2_665 ? La1 O2 2.673(6) 26_455 ? La1 O2 2.673(6) . ? La1 O2 2.673(6) 25_565 ? La1 O1 2.720(6) 33 ? La1 O1 2.720(6) 31 ? La1 O1 2.720(6) 32 ? La1 O1 2.720(6) 14_554 ? La1 O1 2.720(6) 15_554 ? La1 O1 2.720(6) 13_554 ? Sb1 O2 1.972(6) . ? Sb1 O2 1.972(6) 3 ? Sb1 O2 1.972(6) 2 ? Sb2 O1 1.968(2) 31 ? Sb2 O1 1.968(2) . ? Sb2 O1 1.968(2) 2 ? Sb2 O1 1.968(2) 32 ? Sb2 O2 1.970(6) 31 ? Sb2 O2 1.970(6) . ? Sb2 La1 3.4551(2) 7_445 ? O1 Sb2 1.968(2) 3 ? O1 La1 2.720(6) 7_445 ? 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 O2 La1 O2 180 27 3_565 ? O2 La1 O2 69.08(11) 27 2_665 ? O2 La1 O2 110.92(11) 3_565 2_665 ? O2 La1 O2 110.92(11) 27 26_455 ? O2 La1 O2 69.08(11) 3_565 26_455 ? O2 La1 O2 180 2_665 26_455 ? O2 La1 O2 69.08(11) 27 . ? O2 La1 O2 110.92(11) 3_565 . ? O2 La1 O2 110.92(11) 2_665 . ? O2 La1 O2 69.08(11) 26_455 . ? O2 La1 O2 110.92(11) 27 25_565 ? O2 La1 O2 69.08(11) 3_565 25_565 ? O2 La1 O2 69.08(11) 2_665 25_565 ? O2 La1 O2 110.92(11) 26_455 25_565 ? O2 La1 O2 180 . 25_565 ? O2 La1 O1 121.85(10) 27 33 ? O2 La1 O1 58.15(10) 3_565 33 ? O2 La1 O1 58.15(10) 2_665 33 ? O2 La1 O1 121.85(10) 26_455 33 ? O2 La1 O1 107.59(18) . 33 ? O2 La1 O1 72.41(18) 25_565 33 ? O2 La1 O1 121.85(10) 27 31 ? O2 La1 O1 58.15(10) 3_565 31 ? O2 La1 O1 107.59(18) 2_665 31 ? O2 La1 O1 72.41(17) 26_455 31 ? O2 La1 O1 58.15(10) . 31 ? O2 La1 O1 121.85(10) 25_565 31 ? O1 La1 O1 60.5(2) 33 31 ? O2 La1 O1 72.41(17) 27 32 ? O2 La1 O1 107.59(17) 3_565 32 ? O2 La1 O1 58.15(10) 2_665 32 ? O2 La1 O1 121.85(10) 26_455 32 ? O2 La1 O1 58.15(10) . 32 ? O2 La1 O1 121.85(10) 25_565 32 ? O1 La1 O1 60.5(2) 33 32 ? O1 La1 O1 60.5(2) 31 32 ? O2 La1 O1 107.59(17) 27 14_554 ? O2 La1 O1 72.41(17) 3_565 14_554 ? O2 La1 O1 121.85(10) 2_665 14_554 ? O2 La1 O1 58.15(10) 26_455 14_554 ? O2 La1 O1 121.85(10) . 14_554 ? O2 La1 O1 58.15(10) 25_565 14_554 ? O1 La1 O1 119.5(2) 33 14_554 ? O1 La1 O1 119.5(2) 31 14_554 ? O1 La1 O1 180 32 14_554 ? O2 La1 O1 58.15(10) 27 15_554 ? O2 La1 O1 121.85(10) 3_565 15_554 ? O2 La1 O1 121.85(10) 2_665 15_554 ? O2 La1 O1 58.15(10) 26_455 15_554 ? O2 La1 O1 72.41(18) . 15_554 ? O2 La1 O1 107.59(17) 25_565 15_554 ? O1 La1 O1 180 33 15_554 ? O1 La1 O1 119.5(2) 31 15_554 ? O1 La1 O1 119.5(2) 32 15_554 ? O1 La1 O1 60.5(2) 14_554 15_554 ? O2 La1 O1 58.15(10) 27 13_554 ? O2 La1 O1 121.85(10) 3_565 13_554 ? O2 La1 O1 72.41(18) 2_665 13_554 ? O2 La1 O1 107.59(17) 26_455 13_554 ? O2 La1 O1 121.85(10) . 13_554 ? O2 La1 O1 58.15(10) 25_565 13_554 ? O1 La1 O1 119.5(2) 33 13_554 ? O1 La1 O1 180 31 13_554 ? O1 La1 O1 119.5(2) 32 13_554 ? O1 La1 O1 60.5(2) 14_554 13_554 ? O1 La1 O1 60.5(2) 15_554 13_554 ? O2 Sb1 O2 93.3(2) . 3 ? O2 Sb1 O2 93.3(2) . 2 ? O2 Sb1 O2 93.3(2) 3 2 ? O1 Sb2 O1 179.999(2) 31 . ? O1 Sb2 O1 91.7(4) 31 2 ? O1 Sb2 O1 88.3(4) . 2 ? O1 Sb2 O1 88.3(4) 31 32 ? O1 Sb2 O1 91.7(4) . 32 ? O1 Sb2 O1 180 2 32 ? O1 Sb2 O2 96.6(2) 31 31 ? O1 Sb2 O2 83.4(2) . 31 ? O1 Sb2 O2 83.4(2) 2 31 ? O1 Sb2 O2 96.6(2) 32 31 ? O1 Sb2 O2 83.4(2) 31 . ? O1 Sb2 O2 96.6(2) . . ? O1 Sb2 O2 96.6(2) 2 . ? O1 Sb2 O2 83.4(2) 32 . ? O2 Sb2 O2 179.9990(10) 31 . ? O1 Sb2 La1 51.77(17) 31 . ? O1 Sb2 La1 128.23(17) . . ? O1 Sb2 La1 128.23(17) 2 . ? O1 Sb2 La1 51.77(17) 32 . ? O2 Sb2 La1 129.59(18) 31 . ? O2 Sb2 La1 50.41(18) . . ? O1 Sb2 La1 128.23(17) 31 7_445 ? O1 Sb2 La1 51.78(17) . 7_445 ? O1 Sb2 La1 51.77(17) 2 7_445 ? O1 Sb2 La1 128.23(17) 32 7_445 ? O2 Sb2 La1 50.41(18) 31 7_445 ? O2 Sb2 La1 129.59(18) . 7_445 ? La1 Sb2 La1 180 . 7_445 ? Sb2 O1 Sb2 135.0(3) . 3 ? Sb2 O1 La1 93.59(18) . 7_445 ? Sb2 O1 La1 93.59(18) 3 7_445 ? Sb2 O2 Sb1 135.9(3) . . ? Sb2 O2 La1 95.0(2) . . ? Sb1 O2 La1 129.1(3) . . ?