# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2007 #======================================================================= data_global #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name 'S. BEAUDET-SAVIGNAT' _publ_contact_author_address 'CEA Le Ripault, BP 16, 37260 MONTS (France)' _publ_contact_author_email sophie.beaudet-savignat@cea.fr _publ_contact_author_phone +(33)247345174 _publ_contact_author_fax +(33)247344852 _journal_name_full 'Journal of Materials Chemistry' _journal_page_first ? _journal_volume ? _journal_year 2006 loop_ _publ_author_name _publ_author_address 'VINCENT, A.' 'CEA Le Ripault, BP16, 37260 MONTS (France)' 'BEAUDET-SAVIGNAT, S.' 'CEA Le Ripault, BP16, 37260 MONTS (France)' 'LAMBERT, S.' 'CEA Le Ripault, BP16, 37260 MONTS (France)' 'GERVAIS, F.' 'LEMA(UMR 6157), 37200 TOURS (France)' #======================================================================= _audit_creation_method 'Jana2000 Version : 25/06/2004' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_issue ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_(I) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'apatite' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'La8.898 O25.96 Si6' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,1/2+z 3 -y,x-y,z 4 -x,-y,1/2+z 5 -x+y,-x,z 6 y,-x+y,1/2+z _cell_length_a 9.725 _cell_length_b 9.725 _cell_length_c 7.189 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 589 _cell_formula_units_Z 1 _cell_measurement_temperature ? _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.1295 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 799 _pd_spec_size_axial ? _pd_spec_size_equat ? _pd_spec_size_thick ? _pd_spec_mounting ? _pd_spec_mount_mode ? _pd_spec_shape ? _pd_char_particle_morphology ? _pd_char_colour ? _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 5.505 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature '300' _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type 'neutron' _diffrn_radiation_wavelength 1.2244 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method ? _pd_meas_special_details ; ? ; _pd_meas_number_of_points 2261 _pd_meas_2theta_range_min 7.000 _pd_meas_2theta_range_max 120.000 _pd_meas_2theta_range_inc 0.05 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_profile_function 'Pseudo-Voigt' _pd_proc_ls_background_function '20 Chebyshev polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0280 _pd_proc_ls_prof_wR_factor 0.0364 _pd_proc_ls_prof_wR_expected 0.0242 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_gt 0.0283 _refine_ls_R_factor_all 0.0179 _refine_ls_wR_factor_ref 0.0228 _refine_ls_number_parameters 30 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.9711 _refine_ls_shift/su_mean 0.2709 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 7 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.05 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_data_reduction ? loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source La 8.240 International_Tables_Vol_C Si 4.149 International_Tables_Vol_C O 5.803 International_Tables_Vol_C _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.3333 0.6667 -0.003 Uani 0.0173 2 0.849 d . . . La2 La 0.6667 0.3333 -0.003 Uani 0.0173 2 0.63 d . . . La3 La 0.231 -0.0132 0.25 Uani 0.0099 6 0.99 d . . . Si Si 0.4009 0.3715 0.25 Uani 0.0087 6 1 d . . . O1 O 0.3216 0.4825 0.25 Uani 0.0261 6 1 d . . . O2 O 0.594 0.4726 0.245 Uani 0.0156 6 1 d . . . O3 O 0.3293 0.2499 0.416 Uani 0.0366 6 1 d . . . O4 O 0.3537 0.2579 0.058 Uani 0.02 6 1 d . . . O5 O 0 0 0.25 Uani 0.0167 2 0.9801 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 La1 La 0.010501 0.010501 0.031003 0.005251 0 0 La2 La 0.010501 0.010501 0.031003 0.005251 0 0 La3 La 0.010601 0.008201 0.010301 0.0042 0 0 Si Si 0.008001 0.007001 0.006 0 0 0 O1 O 0.028003 0.032003 0.033004 0.026002 0.023002 0 O2 O 0.011601 0.007701 0.021002 0 0 0 O3 O 0.081008 0.005001 0.015001 0.015002 0.009001 0.033003 O4 O 0.030003 0.021002 0.012001 0.015002 0 0 O5 O 0.008001 0.008001 0.034004 0.004 0 0 #======================================================================= data_(II) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'Ba doped apatite' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ba1.076 La8.924 O25.869 Si6' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,1/2+z 3 -y,x-y,z 4 -x,-y,1/2+z 5 -x+y,-x,z 6 y,-x+y,1/2+z _cell_length_a 9.740 _cell_length_b 9.740 _cell_length_c 7.267 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 597 _cell_formula_units_Z 1 _cell_measurement_temperature ? _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.4759 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 860 _pd_spec_size_axial ? _pd_spec_size_equat ? _pd_spec_size_thick ? _pd_spec_mounting ? _pd_spec_mount_mode ? _pd_spec_shape ? _pd_char_particle_morphology ? _pd_char_colour ? _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 5.602 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type 'neutron' _diffrn_radiation_wavelength 1.2244 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method ? _pd_meas_special_details ; ? ; _pd_meas_number_of_points 2201 _pd_meas_2theta_range_min 10.000 _pd_meas_2theta_range_max 120.000 _pd_meas_2theta_range_inc 0.05 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function 'Pseudo-Voigt' _pd_proc_ls_background_function '20 Chebyshev polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0173 _pd_proc_ls_prof_wR_factor 0.0225 _pd_proc_ls_prof_wR_expected 0.0220 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_gt 0.0138 _refine_ls_R_factor_all 0.0173 _refine_ls_wR_factor_ref 0.0225 _refine_ls_number_parameters 78 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.6028 _refine_ls_shift/su_mean 0.1211 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.05 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_data_reduction ? loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source La 8.240 International_Tables_Vol_C Ba 5.070 International_Tables_Vol_C Si 4.149 International_Tables_Vol_C O 5.803 International_Tables_Vol_C _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.3333 0.6667 -0.0004(15) Uani 0.0116(6) 2 0.71(7) d . . . Ba1 La 0.3333 0.6667 -0.0004(15) Uani 0.0116(6) 2 0.29(7) d . . . La2 La 0.6667 0.3333 0.0022(14) Uani 0.0116(6) 2 0.75(7) d . . . Ba2 La 0.6667 0.3333 0.0022(14) Uani 0.0116(6) 2 0.25(7) d . . . La3 La 0.22809(17) -0.01172(19) 0.25 Uani 0.0117(6) 6 1 d . . . Si Si 0.4015(3) 0.3720(3) 0.25 Uani 0.0113(9) 6 1 d . . . O1 O 0.3185(3) 0.4824(3) 0.25 Uani 0.0192(11) 6 1 d . . . O2 O 0.5935(2) 0.4728(3) 0.2393(15) Uani 0.0164(8) 6 1 d . . . O3 O 0.3333 0.2509(7) 0.4188(10) Uani 0.021(2) 6 1 d . . . O4 O 0.3524(5) 0.2599(9) 0.0622(11) Uani 0.018(2) 6 1 d . . . O5 O 0 0 0.253(7) Uani 0.067(3) 2 0.935(17) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 La1 La 0.0102(7) 0.0102(7) 0.0143(11) 0.0051(3) 0 0 Ba1 La 0.0102(7) 0.0102(7) 0.0143(11) 0.0051(3) 0 0 La2 La 0.0102(7) 0.0102(7) 0.0143(11) 0.0051(3) 0 0 Ba2 La 0.0102(7) 0.0102(7) 0.0143(11) 0.0051(3) 0 0 La3 La 0.0117(8) 0.0076(7) 0.0166(8) 0.0054(7) 0.0111(14) 0 Si Si 0.0097(12) 0.0023(11) 0.0179(15) 0 0 0 O1 O 0.0268(13) 0.0197(13) 0.0211(14) 0.0190(11) -0.007524 0 O2 O 0.0088(9) 0.0095(9) 0.0249(17) 0 0 0 O3 O 0.046(3) 0.0012(19) 0.013(2) 0.009(2) 0.0134(17) 0 O4 O 0.026(2) 0.029(3) 0.011(3) 0.022(2) 0 0 O5 O 0.0125(17) 0.0125(17) 0.176(9) 0.0063(8) 0 0 #======================================================================= data_(III) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'Sr doped apatite' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'La8.898 O25.886 Si6 Sr1' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,1/2+z 3 -y,x-y,z 4 -x,-y,1/2+z 5 -x+y,-x,z 6 y,-x+y,1/2+z _cell_length_a 9.705 _cell_length_b 9.705 _cell_length_c 7.215 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 588 _cell_formula_units_Z 1 _cell_measurement_temperature ? _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.3775 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 836 _pd_spec_size_axial ? _pd_spec_size_equat ? _pd_spec_size_thick ? _pd_spec_mounting ? _pd_spec_mount_mode ? _pd_spec_shape ? _pd_char_particle_morphology ? _pd_char_colour ? _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 5.593 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type 'neutron' _diffrn_radiation_wavelength 1.2244 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method ? _pd_meas_special_details ; ? ; _pd_meas_number_of_points 2201 _pd_meas_2theta_range_min 10.000 _pd_meas_2theta_range_max 120.000 _pd_meas_2theta_range_inc 0.05 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function 'Pseudo-Voigt' _pd_proc_ls_background_function '20 Chebyshev polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0173 _pd_proc_ls_prof_wR_factor 0.0218 _pd_proc_ls_prof_wR_expected 0.0196 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_gt 0.0170 _refine_ls_R_factor_all 0.0173 _refine_ls_wR_factor_ref 0.0218 _refine_ls_number_parameters 67 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 1.2187 _refine_ls_shift/su_mean 0.1615 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.05 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_data_reduction ? loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source La 8.240 International_Tables_Vol_C Sr 7.020 International_Tables_Vol_C Si 4.149 International_Tables_Vol_C O 5.803 International_Tables_Vol_C _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.3333 0.6667 0.0046(13) Uani 0.0115(4) 2 0.45 d . . . Sr1 La 0.3333 0.6667 0.0046(13) Uani 0.0115(4) 2 0.50 d . . . La2 La 0.6667 0.3333 0.0046(13) Uani 0.0115(4) 2 1 d . . . La3 La 0.22755(13) -0.01219(15) 0.25 Uani 0.0104(4) 6 1 d . . . Si Si 0.4010(2) 0.3723(2) 0.25 Uani 0.0089(6) 6 1 d . . . O1 O 0.32180(18) 0.48327(19) 0.25 Uani 0.0140(5) 6 1 d . . . O2 O 0.59532(19) 0.4729(2) 0.2458(16) Uani 0.0128(5) 6 1 d . . . O3 O 0.3361 0.2534(3) 0.4257(11) Uani 0.026(2) 6 1 d . . . O4 O 0.3494(3) 0.2552 0.0674(11) Uani 0.017(2) 6 1 d . . . O5 O 0 0 0.25 Uani 0.067(2) 2 0.943(13) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 La1 La 0.0124(5) 0.0124(5) 0.0096(8) 0.0062(2) 0 0 Sr1 La 0.0124(5) 0.0124(5) 0.0096(8) 0.0062(2) 0 0 La2 La 0.0124(5) 0.0124(5) 0.0096(8) 0.0062(2) 0 0 La3 La 0.0111(6) 0.0103(5) 0.0095(5) 0.0051(5) 0 0 Si Si 0.0084(8) 0.0044(9) 0.0096(10) 0 0 0 O1 O 0.0110(7) 0.0064(6) 0.0188(10) 0 0 0 O2 O 0.0074(6) 0.0085(6) 0.0173(10) 0 0 0 O3 O 0.052(3) 0.007(2) 0.018(2) 0.013(2) 0.026(2) 0.012(2) O4 O 0.032(2) 0.025(3) 0.008(2) 0.025(2) 0.0036(14) 0.0022(17) O5 O 0.0097(13) 0.0097(13) 0.181(7) 0.0048(6) 0 0 #======================================================================= data_(IV) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'Ca doped apatite' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ca1.258 La8.742 O25.879 Si6' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,1/2+z 3 -y,x-y,z 4 -x,-y,1/2+z 5 -x+y,-x,z 6 y,-x+y,1/2+z _cell_length_a 9.680 _cell_length_b 9.680 _cell_length_c 7.161 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 581 _cell_formula_units_Z 1 _cell_measurement_temperature ? _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.2765 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 814 _pd_spec_size_axial ? _pd_spec_size_equat ? _pd_spec_size_thick ? _pd_spec_mounting ? _pd_spec_mount_mode ? _pd_spec_shape ? _pd_char_particle_morphology ? _pd_char_colour ? _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 5.447 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type 'neutron' _diffrn_radiation_wavelength 1.2244 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method ? _pd_meas_special_details ; ? ; _pd_meas_number_of_points 2201 _pd_meas_2theta_range_min 10.000 _pd_meas_2theta_range_max 120.000 _pd_meas_2theta_range_inc 0.05 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function 'Pseudo-Voigt' _pd_proc_ls_background_function '20 Legendre polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0175 _pd_proc_ls_prof_wR_factor 0.0226 _pd_proc_ls_prof_wR_expected 0.0202 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0133 _refine_ls_wR_factor_gt 0.0141 _refine_ls_R_factor_all 0.0175 _refine_ls_wR_factor_ref 0.0226 _refine_ls_number_parameters 69 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0128 _refine_ls_shift/su_mean 0.0027 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.05 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_data_reduction ? loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source La 8.240 International_Tables_Vol_C Ca 4.700 International_Tables_Vol_C Si 4.149 International_Tables_Vol_C O 5.803 International_Tables_Vol_C _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.3333 0.6667 0.0071(17) Uani 0.0150(6) 2 0.64(6) d . . . Ca1 La 0.3333 0.6667 0.0071(17) Uani 0.0150(6) 2 0.36(6) d . . . La2 La 0.6667 0.3333 0.0081(16) Uani 0.0150(6) 2 0.73(6) d . . . Ca2 La 0.6667 0.3333 0.0081(16) Uani 0.0150(6) 2 0.27(6) d . . . La3 La 0.2263 -0.0132 0.2520(14) Uani 0.0132(6) 6 1 d . . . Si Si 0.4030(3) 0.3736(3) 0.25 Uani 0.0099(8) 6 1 d . . . O1 O 0.3260(2) 0.4881(2) 0.25 Uani 0.0185(10) 6 1 d . . . O2 O 0.5971(2) 0.4713(3) 0.2429(18) Uani 0.0185(10) 6 1 d . . . O3 O 0.3333 0.2528(6) 0.4305(16) Uani 0.036(2) 6 1 d . . . O4 O 0.3546(5) 0.2620(7) 0.0710(17) Uani 0.027(2) 6 1 d . . . O5 O 0 0 0.25 Uani 0.106(4) 2 0.939(16) d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 La1 La 0.0134(7) 0.0134(7) 0.0183(13) 0.0067(3) 0 0 Ca1 La 0.0134(7) 0.0134(7) 0.0183(13) 0.0067(3) 0 0 La2 La 0.0134(7) 0.0134(7) 0.0183(13) 0.0067(3) 0 0 Ca2 La 0.0134(7) 0.0134(7) 0.0183(13) 0.0067(3) 0 0 La3 La 0.0152(7) 0.0104(7) 0.0113(6) 0.0043(6) -0.0109(15) 0 Si Si 0.0053(10) 0.0061(12) 0.0147(13) 0 0 0 O1 O 0.0242(11) 0.0133(12) 0.0232(13) 0.0134(10) 0 0 O2 O 0.0123(11) 0.0093(10) 0.0319(18) 0.0039(10) 0 0 O3 O 0.081(4) 0.0024(18) 0.011(2) 0.011(2) 0.031(2) 0.0172(13) O4 O 0.041(2) 0.039(3) 0.028(3) 0.039(2) 0 0 O5 O 0.0081(17) 0.0081(17) 0.302(11) 0.0040(9) 0 0 #=======================================================================