# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 #TrackingRef '- ksrbodytm.txt' #============================================================================== _audit_creation_method 'encifer (version 1.1)' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _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_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Li Wu' _publ_contact_author_address ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; _publ_contact_author_email lwu@nankai.edu.cn _publ_contact_author_fax 86(22)23505409 _publ_contact_author_phone 86(22)23506257 #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Luminescence and Energy Transfer of a Color Tunable Phosphor: Dy^3+^-, Tm^3+^-, and Eu^3+^-Coactivated KSr~4~(BO~3~)~3~ for Warm White-Light UVLED ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Li Wu' ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; 'Yi Zhang' ; Institute of photo-electronic thin film devices and technology Nankai University, Tianjin 300071 People's Republic of China ; 'Mingyuan Gui' ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; 'Shu Tian' ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; 'Yongfa Kong' ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; 'Jingjun Xu' ; The MOE Key Laboratory of Weak-Light Nonlinear Photonics School of Physics Nankai University, Tianjin 300457 People's Republic of China ; #============================================================================== # TEXT _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_acknowledgements ; This work is financially supported by National Natural Science Foundation of China (50902074, 90922037 and 60906033), and Natural Science Foundation of Tianjin (09JCYBJC02500). The work is also supported through a Grant-in-Aid from the International Centre for Diffraction Data (ICDD). We thank Mrs. Y. P. Xu of N01 group, Institute of Physics, Chinese Academy of Science; Dr. J. W. Qi and Dr. Z. H. Wang of Applied Physics School, Nankai University; and Dr. M. Jiang of Tsinghua University for their great help in collecting powder X-ray diffraction data, PL spectra, and ESR measurements. ; _publ_section_references ; J.Rodriguez-Carvajal (2003), FULLPROF version 2.45, ILL, France. PANalytical(2004). X'Pert Pro. PANalytical Corporation, Nertherland. CCDC (2003). enCIFer. Version 1.0. Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge, England. Kang, S. J. & Ozawa, T.C. (2003). Balls & Sticks. URL: http://www.softbug.com/ toycrate/. March (1932), Toraya, 1986. ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_ksrbodydata _database_code_depnum_ccdc_archive 'CCDC 852615' #TrackingRef '- ksrbodytm.txt' # start Validation Reply Form _vrf_WEIGH01_ksrbodydata ; PROBLEM: The weighting scheme should be one of the following RESPONSE: The structure was refined by Rietveld method with powder diffraction data in Fullprof program, in which the weights of the observations are calculated as: 1/Y~i~ ; _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: All the authors have contribution to the paper. ; # end Validation Reply Form # CHEMICAL DATA _chemical_name_systematic ; dysprosium doped potassium strontium borate ; _chemical_name_common ? _chemical_formula_moiety '3(B O3), 4(Sr0.98 Dy0.02), K' _chemical_formula_structural 'Sr3.92 Dy0.08 K (B O3)3' _chemical_formula_analytical ? _chemical_formula_iupac 'K Sr3.92 Dy0.08 (B O3)3' _chemical_formula_sum 'B3 Sr3.92 Dy0.08 K O9' _chemical_formula_weight 571.992 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -0.3528 1.8200 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ama2 _symmetry_space_group_name_Hall 'A a -2a' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x+1/2,y,z x+1/2,-y,z -x,-y,z x,y+1/2,z+1/2 -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z+1/2 -x,-y+1/2,z+1/2 _cell_length_a 11.0101(1) _cell_length_b 11.9831(1) _cell_length_c 6.8838(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 908.22(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.182 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1041 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 35 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour white # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature 1073 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 295 _diffrn_source 'rotating-anode x-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type "X'pert Pro" _diffrn_detector X'celerator _diffrn_detector_type RTMS _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a 1.5418 _diffrn_radiation_monochromator none # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7352 _pd_meas_2theta_range_min 10.008 _pd_meas_2theta_range_max 134.975 _pd_meas_2theta_range_inc 0.017 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection "X'Pert Data Collector 2.2f" _computing_cell_refinement 'Highscore1.0b (Philips Electronics 2002)' _computing_data_reduction 'Highscore1.0b (Philips Electronics 2002)' _computing_structure_solution SHEXLS97(Sheldric,1997) _computing_structure_refinement 'FULLPROF(J. Rodriguez-Carvajal,2003)' _computing_molecular_graphics 'Balls & sticks(Kang & Ozawa,2003)' _computing_publication_material 'enCIFer(CCDC, 2003)' #============================================================================== # REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function pseudo-Voigt _pd_proc_ls_background_function 'square polynomial for each range' _pd_proc_ls_pref_orient_corr ; I~corr~ = I~obs~[G~2~+(1-G~2~)exp(G~1~a^2^)], axis (001), (March, 1932) ; _pd_proc_ls_prof_R_factor 0.0350 _pd_proc_ls_prof_wR_factor 0.0506 _pd_proc_ls_prof_wR_expected 0.0282 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/Y~i~ _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 58 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.8 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 10.008 _pd_proc_2theta_range_max 134.975 _pd_proc_2theta_range_inc 0.017 loop_ _pd_proc_wavelength 1.5418 _pd_block_diffractogram_id ksrbodyprofile # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction ? #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_type_symbol Sr1 .2500 .3555(1) .0624(6) .0126(8) Uiso 1 Sr Sr2 -.0281(1) .2145(1) .9294(4) .0103(4) Uiso 0.968(11) Sr Dy -.0281(1) .2145(1) .9294(4) .0103(4) Uiso 0.032(11) Dy Sr3 .0000 .0000 .2829 .0111(7) Uiso 1 Sr K .2500 .5839(5) .328(1) .038(2) Uiso 1 K O1 .2500 .349(1) .449(3) .008(5) Uiso 1 O O2 .2500 .563(1) .907(3) .019(5) Uiso 1 O O3 .137(1) .6720(9) .669(1) .003(3) Uiso 1 O O4 .0289(7) .402(1) .108(1) .004(2) Uiso 1 O O5 .857(1) .1944(9) .238(2) .005(3) Uiso 1 O O6 .0000 .5000 .407(4) .012(5) Uiso 1 O B1 .2500 .637(3) .754(5) .015(9) Uiso 1 B B2 .2500 .336(2) .651(5) .005(9) Uiso 1 B B3 .0000 .5000 .211(5) .024(9) Uiso 1 B #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ? 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 Sr1 O1 . 2.66(2) yes Sr1 O2 1_554 2.71(1) yes Sr1 O3 5_544 2.63(1) yes Sr1 O3 6_544 2.63(1) yes Sr1 O4 . 2.518(9) yes Sr1 O4 2_555 2.518(9) yes Sr1 O5 7_454 2.59(1) yes Sr1 O5 8_654 2.59(1) yes Sr2 O1 7_455 2.563(4) yes Sr2 O3 4_565 2.54(1) yes Sr2 O3 5_545 2.51(1) yes Sr2 O4 1_556 2.64(1) yes Sr2 O4 8_555 2.61(1) yes Sr2 O5 1_456 2.48(1) yes Sr2 O5 8_655 2.53(1) yes Sr2 O6 5_545 2.593(2) yes Dy2 O1 7_455 2.563(4) yes Dy2 O3 4_565 2.54(1) yes Dy2 O3 5_545 2.51(1) yes Dy2 O4 1_556 2.64(1) yes Dy2 O4 8_555 2.61(1) yes Dy2 O5 1_456 2.48(1) yes Dy2 O5 8_655 2.53(1) yes Dy2 O6 5_545 2.593(2) yes Sr3 O2 5_544 2.982(7) yes Sr3 O2 7_454 2.982(7) yes Sr3 O3 5_544 2.67(1) yes Sr3 O3 8_554 2.67(1) yes Sr3 O4 5_545 2.54(1) yes Sr3 O4 8_555 2.54(1) yes Sr3 O5 1_455 2.82(1) yes Sr3 O5 4_655 2.82(1) yes Sr3 O6 5_544 2.58(2) yes K O1 . 2.93(1) yes K O2 1_554 2.90(2) yes K O3 . 2.86(1) yes K O3 2_555 2.86(1) yes K O5 3_465 2.97(1) yes K O5 4_665 2.97(1) yes K O6 . 2.981(5) yes K O6 2_555 2.981(5) yes B1 O2 . 1.37(4) yes B1 O3 . 1.43(2) yes B1 O3 2_555 1.43(2) yes B2 O1 . 1.39(4) yes B2 O5 7_455 1.37(2) yes B2 O5 8_655 1.37(2) yes B3 O4 . 1.40(2) yes B3 O4 4_565 1.40(2) yes B3 O6 . 1.34(4) yes 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 _geom_angle_publ_flag O2 B1 O3 . . 119.7(2) yes O2 B1 O3 . 2_555 119.7(2) yes O3 B1 O3 . 2_555 120.3(1) yes O1 B2 O5 . 7_455 117.5(2) yes O1 B2 O5 . 8_655 117.5(2) yes O5 B2 O5 7_455 8_655 118.6(2) yes O4 B3 O4 . 4_565 118.9(1) yes O4 B3 O6 . . 120.5(2) yes O4 B3 O6 4_565 . 120.5(2) yes data_ksrbotmdata _database_code_depnum_ccdc_archive 'CCDC 852616' #TrackingRef '- ksrbodytm.txt' # start Validation Reply Form _vrf_WEIGH01_ksrbotmdata ; PROBLEM: The weighting scheme should be one of the following RESPONSE: The structure was refined by Rietveld method with powder diffraction data in Fullprof program, in which the weights of the observations are calculated as: 1/Y~i~ ; # end Validation Reply Form # CHEMICAL DATA _chemical_name_systematic ; thulium doped potassium strontium borate ; _chemical_name_common ? _chemical_formula_moiety '3(B O3), 4(Sr0.985 Tm0.015), K' _chemical_formula_structural 'Sr3.94 Tm0.06 K (B O3)3' _chemical_formula_analytical ? _chemical_formula_iupac 'K Sr3.94 Tm0.06 (B O3)3' _chemical_formula_sum 'B3 Sr3.94 Tm0.06 K O9' _chemical_formula_weight 570.880 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -0.3528 1.8200 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -8.0393 4.1821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ama2 _symmetry_space_group_name_Hall 'A a -2a' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x+1/2,y,z x+1/2,-y,z -x,-y,z x,y+1/2,z+1/2 -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z+1/2 -x,-y+1/2,z+1/2 _cell_length_a 11.0324(1) _cell_length_b 11.9915(1) _cell_length_c 6.8888(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 911.36(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.159 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1039 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 35 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour white # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature 1073 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 295 _diffrn_source 'rotating-anode x-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type "X'pert Pro" _diffrn_detector X'celerator _diffrn_detector_type RTMS _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a 1.5418 _diffrn_radiation_monochromator none # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7352 _pd_meas_2theta_range_min 10.008 _pd_meas_2theta_range_max 134.975 _pd_meas_2theta_range_inc 0.017 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection "X'Pert Data Collector 2.2f" _computing_cell_refinement 'Highscore1.0b (Philips Electronics 2002)' _computing_data_reduction 'Highscore1.0b (Philips Electronics 2002)' _computing_structure_solution SHEXLS97(Sheldric,1997) _computing_structure_refinement 'FULLPROF(J. Rodriguez-Carvajal,2003)' _computing_molecular_graphics 'Balls & sticks(Kang & Ozawa,2003)' _computing_publication_material 'enCIFer(CCDC, 2003)' #============================================================================== # REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function pseudo-Voigt _pd_proc_ls_background_function 'square polynomial for each range' _pd_proc_ls_pref_orient_corr ; I~corr~ = I~obs~[G~2~+(1-G~2~)exp(G~1~a^2^)], axis (001), (March, 1932) ; _pd_proc_ls_prof_R_factor 0.0375 _pd_proc_ls_prof_wR_factor 0.0538 _pd_proc_ls_prof_wR_expected 0.0278 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/Y~i~ _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 58 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.9 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 10.008 _pd_proc_2theta_range_max 134.975 _pd_proc_2theta_range_inc 0.017 loop_ _pd_proc_wavelength 1.5418 _pd_block_diffractogram_id ksrbotmprofile # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction ? #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_type_symbol Sr1 .2500 .3553(2) .0643(6) .0125(8) Uiso 1 Sr Sr2 -.0284(1) .2148(1) .9312(4) .0098(5) Uiso 0.985(7) Sr Tm -.0284(1) .2148(1) .9312(4) .0098(5) Uiso 0.015(7) Dy Sr3 .0000 .0000 .2829 .0106(7) Uiso 1 Sr K .2500 .5837(5) .331(1) .029(2) Uiso 1 K O1 .2500 .347(1) .451(3) .008(5) Uiso 1 O O2 .2500 .565(1) .911(3) .018(5) Uiso 1 O O3 .136(1) .672(1) .668(1) .006(3) Uiso 1 O O4 .0292(8) .403(1) .108(2) .005(3) Uiso 1 O O5 .857(1) .1959(9) .239(2) .006(4) Uiso 1 O O6 .0000 .5000 .407(4) .008(5) Uiso 1 O B1 .2500 .641(3) .754(5) .013(9) Uiso 1 B B2 .2500 .330(3) .647(5) .010(9) Uiso 1 B B3 .0000 .5000 .208(6) .021(9) Uiso 1 B #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ? 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 Sr1 O1 . 2.67(2) yes Sr1 O2 1_554 2.73(1) yes Sr1 O3 5_544 2.63(1) yes Sr1 O3 6_544 2.63(1) yes Sr1 O4 . 2.520(9) yes Sr1 O4 2_555 2.520(9) yes Sr1 O5 7_454 2.60(1) yes Sr1 O5 8_654 2.60(1) yes Sr2 O1 7_455 2.558(4) yes Sr2 O3 4_565 2.55(1) yes Sr2 O3 5_545 2.49(1) yes Sr2 O4 1_556 2.64(1) yes Sr2 O4 8_555 2.63(1) yes Sr2 O5 1_456 2.47(1) yes Sr2 O5 8_655 2.54(1) yes Sr2 O6 5_545 2.600(2) yes Tm2 O1 7_455 2.558(4) yes Tm2 O3 4_565 2.55(1) yes Tm2 O3 5_545 2.49(1) yes Tm2 O4 1_556 2.64(1) yes Tm2 O4 8_555 2.63(1) yes Tm2 O5 1_456 2.47(1) yes Tm2 O5 8_655 2.54(1) yes Tm2 O6 5_545 2.600(2) yes Sr3 O2 5_544 2.992(7) yes Sr3 O2 7_454 2.992(7) yes Sr3 O3 5_544 2.67(1) yes Sr3 O3 8_554 2.67(1) yes Sr3 O4 5_545 2.54(1) yes Sr3 O4 8_555 2.54(1) yes Sr3 O5 1_455 2.84(1) yes Sr3 O5 4_655 2.84(1) yes Sr3 O6 5_544 2.58(2) yes K O1 . 2.95(1) yes K O2 1_554 2.89(2) yes K O3 . 2.84(1) yes K O3 2_555 2.84(1) yes K O5 3_465 2.96(1) yes K O5 4_665 2.96(1) yes K O6 . 2.982(5) yes K O6 2_555 2.982(5) yes B1 O2 . 1.41(4) yes B1 O3 . 1.43(2) yes B1 O3 2_555 1.43(2) yes B2 O1 . 1.36(4) yes B2 O5 7_455 1.38(2) yes B2 O5 8_655 1.38(2) yes B3 O4 . 1.38(2) yes B3 O4 4_565 1.38(2) yes B3 O6 . 1.37(4) yes 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 _geom_angle_publ_flag O2 B1 O3 . . 118.8(2) yes O2 B1 O3 . 2_555 118.8(2) yes O3 B1 O3 . 2_555 121.5(1) yes O1 B2 O5 . 7_455 119.2(2) yes O1 B2 O5 . 8_655 119.2(2) yes O5 B2 O5 7_455 8_655 118.0(2) yes O4 B3 O4 . 4_565 120.7(1) yes O4 B3 O6 . . 119.6(3) yes O4 B3 O6 4_565 . 119.6(3) yes data_ksrbodytmdata _database_code_depnum_ccdc_archive 'CCDC 852617' #TrackingRef '- ksrbodytm.txt' # start Validation Reply Form _vrf_WEIGH01_ksrbodytmdata ; PROBLEM: The weighting scheme should be one of the following RESPONSE: The structure was refined by Rietveld method with powder diffraction data in Fullprof program, in which the weights of the observations are calculated as: 1/Y~i~ ; # end Validation Reply Form # CHEMICAL DATA _chemical_name_systematic ; dysprosium thulium codoped potassium strontium borate ; _chemical_name_common ? _chemical_formula_moiety '3(B O3), 4(Sr0.985 Dy0.01 Tm0.005), K' _chemical_formula_structural 'Sr3.94 Dy0.04 Tm0.02 K (B O3)3' _chemical_formula_analytical ? _chemical_formula_iupac 'K Sr3.94 Dy0.04 Tm0.02 (B O3)3' _chemical_formula_sum 'B3 Sr3.94 Dy0.04 Tm0.02 K O9' _chemical_formula_weight 570.623 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -0.3528 1.8200 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -8.0393 4.1821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ama2 _symmetry_space_group_name_Hall 'A a -2a' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x+1/2,y,z x+1/2,-y,z -x,-y,z x,y+1/2,z+1/2 -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z+1/2 -x,-y+1/2,z+1/2 _cell_length_a 11.0300(1) _cell_length_b 11.9923(1) _cell_length_c 6.8880(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 911.11(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.158 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1039 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 35 # parallel to # scattering vector # in transmission _pd_spec_size_thick 1 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour white # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature 1073 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 295 _diffrn_source 'rotating-anode x-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type "X'pert Pro" _diffrn_detector X'celerator _diffrn_detector_type RTMS _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a 1.5418 _diffrn_radiation_monochromator none # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7352 _pd_meas_2theta_range_min 10.008 _pd_meas_2theta_range_max 134.975 _pd_meas_2theta_range_inc 0.017 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection "X'Pert Data Collector 2.2f" _computing_cell_refinement 'Highscore1.0b (Philips Electronics 2002)' _computing_data_reduction 'Highscore1.0b (Philips Electronics 2002)' _computing_structure_solution SHEXLS97(Sheldric,1997) _computing_structure_refinement 'FULLPROF(J. Rodriguez-Carvajal,2003)' _computing_molecular_graphics 'Balls & sticks(Kang & Ozawa,2003)' _computing_publication_material 'enCIFer(CCDC, 2003)' #============================================================================== # REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text _pd_proc_ls_profile_function pseudo-Voigt _pd_proc_ls_background_function 'square polynomial for each range' _pd_proc_ls_pref_orient_corr ; I~corr~ = I~obs~[G~2~+(1-G~2~)exp(G~1~a^2^)], axis (001), (March, 1932) ; _pd_proc_ls_prof_R_factor 0.0316 _pd_proc_ls_prof_wR_factor 0.0418 _pd_proc_ls_prof_wR_expected 0.0268 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/Y~i~ _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 59 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.5 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 10.008 _pd_proc_2theta_range_max 134.975 _pd_proc_2theta_range_inc 0.017 loop_ _pd_proc_wavelength 1.5418 _pd_block_diffractogram_id ksrbodytmprofile # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions none _pd_proc_info_data_reduction ? #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_type_symbol Sr1 .2500 .3550(1) .0629(4) .0126(7) Uiso 1 Sr Sr2 -.0282(1) .2147(1) .9304(4) .0103(4) Uiso 0.988(1) Sr Dy1 -.0282(1) .2147(1) .9304(4) .0103(4) Uiso 0.007(1) Dy Tm -.0282(1) .2147(1) .9304(4) .0103(4) Uiso 0.005(1) Tm Sr3 .0000 .0000 .2829 .0111(6) Uiso 0.996(6) Sr Dy2 .0000 .0000 .2829 .0111(6) Uiso 0.004(6) Dy K .2500 .5834(4) .3262(9) .032(2) Uiso 1 K O1 .2500 .348(1) .448(3) .011(4) Uiso 1 O O2 .2500 .557(1) .910(3) .029(4) Uiso 1 O O3 .137(1) .6711(8) .670(1) .006(3) Uiso 1 O O4 .0277(6) .4040(9) .109(1) .005(2) Uiso 1 O O5 .857(1) .1927(8) .238(1) .010(3) Uiso 1 O O6 .0000 .5000 .402(3) .005(4) Uiso 1 O B1 .2500 .635(2) .763(4) .016(8) Uiso 1 B B2 .2500 .330(2) .647(4) .005(7) Uiso 1 B B3 .0000 .5000 .203(4) .022(8) Uiso 1 B #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ? 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 Sr1 O1 . 2.65(1) yes Sr1 O2 1_554 2.64(1) yes Sr1 O3 5_544 2.63(1) yes Sr1 O3 6_544 2.63(1) yes Sr1 O4 . 2.540(7) yes Sr1 O4 2_555 2.540(7) yes Sr1 O5 7_454 2.59(1) yes Sr1 O5 8_654 2.59(1) yes Sr2 O1 7_455 2.564(4) yes Sr2 O3 4_565 2.55(1) yes Sr2 O3 5_545 2.52(1) yes Sr2 O4 1_556 2.65(1) yes Sr2 O4 8_555 2.63(1) yes Sr2 O5 1_456 2.48(1) yes Sr2 O5 8_655 2.55(1) yes Sr2 O6 5_545 2.601(2) yes Dy1 O1 7_455 2.564(4) yes Dy1 O3 4_565 2.55(1) yes Dy1 O3 5_545 2.52(1) yes Dy1 O4 1_556 2.65(1) yes Dy1 O4 8_555 2.63(1) yes Dy1 O5 1_456 2.48(1) yes Dy1 O5 8_655 2.55(1) yes Dy1 O6 5_545 2.601(2) yes Tm O1 7_455 2.564(4) yes Tm O3 4_565 2.55(1) yes Tm O3 5_545 2.52(1) yes Tm O4 1_556 2.65(1) yes Tm O4 8_555 2.63(1) yes Tm O5 1_456 2.48(1) yes Tm O5 8_655 2.55(1) yes Tm O6 5_545 2.601(2) yes Sr3 O2 5_544 2.973(6) yes Sr3 O2 7_454 2.973(6) yes Sr3 O3 5_544 2.66(1) yes Sr3 O3 8_554 2.66(1) yes Sr3 O4 5_545 2.54(1) yes Sr3 O4 8_555 2.54(1) yes Sr3 O5 1_455 2.81(1) yes Sr3 O5 4_655 2.81(1) yes Sr3 O6 5_544 2.61(2) yes Dy2 O2 5_544 2.973(6) yes Dy2 O2 7_454 2.973(6) yes Dy2 O3 5_544 2.66(1) yes Dy2 O3 8_554 2.66(1) yes Dy2 O4 5_545 2.54(1) yes Dy2 O4 8_555 2.54(1) yes Dy2 O5 1_455 2.81(1) yes Dy2 O5 4_655 2.81(1) yes Dy2 O6 5_544 2.61(2) yes K O1 . 2.93(1) yes K O2 1_554 2.88(2) yes K O3 . 2.87(1) yes K O3 2_555 2.87(1) yes K O5 3_465 2.99(1) yes K O5 4_665 2.99(1) yes K O6 . 2.980(4) yes K O6 2_555 2.980(4) yes B1 O2 . 1.37(3) yes B1 O3 . 1.45(2) yes B1 O3 2_555 1.45(2) yes B2 O1 . 1.38(3) yes B2 O5 7_455 1.36(1) yes B2 O5 8_655 1.36(1) yes B3 O4 . 1.35(1) yes B3 O4 4_565 1.35(1) yes B3 O6 . 1.37(3) yes 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 _geom_angle_publ_flag O2 B1 O3 . . 121.4(2) yes O2 B1 O3 . 2_555 121.4(2) yes O3 B1 O3 . 2_555 116.3(2) yes O1 B2 O5 . 7_455 118.9(2) yes O1 B2 O5 . 8_655 118.9(2) yes O5 B2 O5 7_455 8_655 119.6(1) yes O4 B3 O4 . 4_565 122.9(1) yes O4 B3 O6 . . 118.5(2) yes O4 B3 O6 4_565 . 118.5(2) yes #===END