############################################################################## ### CIF submission form for results of Rietveld refinements (IUCr journals)### ### Version 10 February 2005 ### ############################################################################## # This is an electronic "form" for submitting the results of a Rietveld # refinement of a model against powder diffraction data to an # IUCr journal as a Crystallographic Information File (CIF). Full details # of the CIF format are given in the paper "The Crystallographic Information # File (CIF): a New Standard Archive File for Crystallography" by S. R. Hall, # F. H. Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # The current version of the powder CIF dictionary, which contains definitions # of the terms staring _pd_, may be obtained from # http://www.iucr.org/iucr-top/cif/pd/index.html. Other terms are defined in # the core CIF dictionary at http://www.iucr.org/iucr-top/cif/core/index.html. # # Note that all fields should be numeric or character type EXCEPT those which # are flagged as 'text' - free-form text of any length may be included in # these latter fields provided the text block begins and ends with a semicolon # as the first character of a new line. Note also that the query marks # '?' are significant as placeholders, and should not be deleted where a data # item is not given, UNLESS the accompanying data name is also deleted. # Lines should not exceed 80 characters in length. The comments following # a hash symbol '#' may be deleted if wished. #============================================================================= data_global _audit_update_record ; 2010-06-25 # Formatted by publCIF ; #============================================================================== loop_ _audit_conform.dict_name _audit_conform.dict_version _audit_conform.dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 1. SUBMISSION DETAILS _publ_contact_author_name 'Hiroshi Kojitani' _publ_contact_author_address # Address of author for correspondence ; Department of Chemistry Gakushuin University 1-5-1 Mejiro, Toshima-ku Tokyo 171-8588 Japan ; _publ_contact_author_email hiroshi.kojitani@gakushuin.ac.jp _publ_contact_author_fax +81-3-5992-1029 _publ_contact_author_phone +81-3-3986-0221 _publ_contact_letter ;? ; _publ_requested_journal 'American Mineralogist' _publ_requested_coeditor_name ? _publ_requested_category ? # Acta Cryst. C: one of FI/FM/FO/AD # Acta Cryst. E: one of EI/EM/EO/AD #============================================================================== # 2. 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_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Structure refinement of high-pressure hexagonal aluminous phases K~1.00~Mg~2.00~Al~4.80~Si~1.15~O~12~ and Na~1.04~Mg~1.88~Al~4.64~Si~1.32~O~12~ ; _publ_section_title_footnote . # 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_footnote _publ_author_address 'Kojitani, Hiroshi ' #<--'Last name, firstname' ; ? ; ; Department of Chemistry Gakushuin University 1-5-1 Mejiro, Toshima-ku Tokyo 171-8588 Japan ; 'Iwabuchi, Takemi ' #<--'Last name, firstname' ; ? ; ; Department of Chemistry Gakushuin University 1-5-1 Mejiro, Toshima-ku Tokyo 171-8588 Japan ; 'Kobayashi, Makoto ' #<--'Last name, firstname' ; ? ; ; Department of Chemistry Gakushuin University 1-5-1 Mejiro, Toshima-ku Tokyo 171-8588 Japan ; 'Miura, Hiroyuki ' #<--'Last name, firstname' ; ? ; ; Division of Earth and Planetary Sciences Graduate School of Science Hokkaido University N10-W8, Kita-ku Sapporo 060-0810 Japan ; 'Akaogi, Masaki ' #<--'Last name, firstname' ; ? ; ; Department of Chemistry Gakushuin University 1-5-1 Mejiro, Toshima-ku Tokyo 171-8588 Japan ; #============================================================================== # 4. TEXT (For Acta Cryst. C and E, include the text of your paper in the CIF) _publ_section_synopsis . _publ_section_abstract ; As possible Na- and K-host minerals in the lower mantle, hexagonal aluminous phases with K~1.00~Mg~2.00~Al~4.80~Si~1.15~O~12~ and Na~1.04~Mg~1.88~Al~4.64~Si~1.32~O~12~ compositions were synthesized at 22--25 GPa and 1500\%C. The K-rich hexagonal aluminous phase was synthesized for the first time. Crystal structures of both hexagonal aluminous phases were refined using the Rietveld method. Obtained interatomic distances and bond angles were compared to published data on CaMg~2~Al~6~O~12~ hexagonal aluminous phase. The general chemical formula of the hexagonal aluminous phase is represented as [M3][M2]~2~[M1]~6~O~12~ where the small-, middle-, and large-sized cations occupy the M1, M2, and M3 sites, respectively. Changes of size and shape of M1O~6~ octahedra by the substitution of Si^4+^ for Al^3+^ in the M1 site make it possible to adjust the size of the M2 and the M3 sites to accommodate Na^+^ and Mg^2+^ in the M2 sites and Na^+^ and K^+^ in the M3 sites. Along the NaAlSiO~4~-MgAl~2~O~4~ join, stability of hexagonal aluminous phase in a relatively wide compositional range of 30--50 mol% in NaAlSiO~4~ component can be explained by possible replacement of Mg^2+^ by Na^+^ in the M2 site due to closer ionic radius of Na^+^ to Mg^2+^ than K^+^ and by shrinkage and deformation of M1O~6~ octahedra with the coupled substitution: ^M2^Mg^2+^ + ^M1^Al^3+^ \\rightarrow ^M2^Na^+^ + ^M1^Si^4+^. ; _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; High-pressure high-temperature syntheses of the K- and the Na-hexagonal aluminous phases were made using a Kawai-type multi-anvil high-pressure apparatus at Gakushuin University. In the synthesis of the K-hexagonal aluminous phase, the gel with KMg~2~Al~5~SiO~12~ composition was held for 1 hour at 1500\%C and at 20 GPa. After quenching to room temperature at the pressure, the sample was decompressed to ambient pressure. Similarly, the Na-hexagonal aluminous phase was synthesized by keeping the starting mixture of MgAl~2~O~4~ spinel and NaAlSiO~4~ high carnegieite in the mole ratio of 3:2 at 22 GPa and 1500\%C for 2 hours ; _publ_section_exptl_refinement ; The crystal structure of CaMg~2~Al~6~O~12~ hexagonal aluminous phase (Miura et al. 2000) was adopted as the model structure. ; _publ_section_references ; Kojitani, H., Hisatomi, R. & Akaogi, M. (2007). Am. Mineral., 92, 1112-1118. Izumi, F. & Ikeda, T. (2000). Mater. Sci. Forum, 321/324, 198-204. Miura, H., Hamada, Y., Suzuki, T., Akaogi, M., MIyajima, N. & Fujino, K. (2000). Am. Mineral., 85, 1799-1803. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; This study was partially supported by Grants-in-Aid (No. 18540478 to H. K. and No. 19340166 to M. A.) from Japan Society for the Promotion of Science. ; #============================================================================== # If more than one structure is reported, sections 5-10 should be completed # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== data_K-hex loop_ _audit_conform.dict_name _audit_conform.dict_version _audit_conform.dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'K1.00 Mg2.00 Al4.80 Si1.15 O12' _chemical_formula_structural 'K1.00 Mg2.00 Al4.80 Si1.15 O12' _chemical_formula_analytical 'K1.00 Mg2.00 Al4.80 Si1.15 O12' _chemical_formula_sum 'K1.00 Mg2.00 Al4.80 Si1.15 O12' _chemical_formula_weight 441.51 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system hexagonal _space_group_name_H-M_alt P63/m _space_group_name_Hall -P6c loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 1 x, y, z 2 -y, x-y, z 3 -x;y, -x, z 4 -x, -y, z+1/2 5 y, -x+y, z+1/2 6 x-y, x, z+1/2 _cell_length_a 8.8168(2) _cell_length_b 8.8168(2) _cell_length_c 2.7684(1) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 186.37(1) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; powder were fixed using aceton on a quartz or a Si plate holder. ; _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 ? _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 20000000 _pd_prep_temperature 1773 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The 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 ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source 'rotating target' _diffrn_source_target Cr _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_measurement_device_type 'Rigaku RINT2500V' _diffrn_detector 'NaI scintillation counter' _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method 'cont' # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 2.2897 _diffrn_radiation_monochromator 'pyrolytic graphite monochromator' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 6500 _pd_meas_2theta_range_min 15 _pd_meas_2theta_range_max 145 _pd_meas_2theta_range_inc 0.02 # 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 ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The atomic displacement parameters of two oxygen sites were fixed at 1.0 which was an average for oxides. The site occupancy fractions were based on the results of the chemical analysis. ; # The next three items are given as text. _pd_proc_ls_profile_function 'pseudo-Voigt' _pd_proc_ls_background_function 'Legendre's polynomial' _pd_proc_ls_pref_orient_corr ; March-Dollase function ; _pd_proc_ls_prof_R_factor 0.0754 _pd_proc_ls_prof_wR_factor 0.1011 _pd_proc_ls_prof_wR_expected 0.0757 _refine_ls_R_I_factor 0.0470 _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all 0.0340 _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? # options are 'sigma' (based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_parameters ? _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 ? _refine_ls_restrained_S_all 1.3343 _refine_ls_shift/su_max ? _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 15 _pd_proc_2theta_range_max 145 _pd_proc_2theta_range_inc 0.02 _pd_proc_wavelength 2.2897 # Each refinement must be accompanied by a listing of the powder data # in CIF format. Each listing should be sent as a separate file consisting # of one data block containing a single powder profile. The value of # _pd_block_diffractogram_id is used to associate each refinement with # its corresponding powder profile, since it must match the value # of _pd_block_id in the file containing the powder data. A template # for supplying powder data in CIF format is available by ftp at # ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given # at ftp://ftp.iucr.org/pub/rietdataxmpl.cif. _pd_block_diffractogram_id ? # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection 'RIgaku application software' _computing_cell_refinement 'RIETAN-2000 (Izumi and Ikeda, 2000)' _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'RIETAN-2000 (Izumi and Ikeda, 2000)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_B_iso_or_equiv _atom_site_adp_type K 0 0 0.25 0.5 ? 2a 1.59(11) Biso Mg 0.66667 0.33333 0.25 1.0 ? 2d 0.47(8) Biso Al 0.9915(2) 0.3472(2) 0.25 0.80 ? 6h 0.22(5) Biso Si 0.9915(2) 0.3472(2) 0.25 0.19 ? 6h 0.22(5) Biso O1 0.1318(3) 0.6021(3) 0.25 1.0 ? 6h 1.0 Biso O2 0.3206(4) 0.2074(3) 0.25 1.0 ? 6h 1.0 Biso # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol ? ? ? ? ? ? ? ? #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag K O2 2.483(3) ? ? y K O2 2.843(3) ? ? y Mg O1 2.094(2) ? ? y Al O1 1.949(2) ? ? y Al O1 1.945(2) ? ? y Al O2 1.927(3) ? ? y Al O2 1.837(2) ? ? y O1 O1 2.525(4) ? ? y O2 O2 2.843(2) ? ? y 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al O1 86.1(1) ? ? ? y O1 Al O1 90.7(1) ? ? ? y O2 Al O2 97.8(1) ? ? ? y O1 Al O1 80.8(1) ? ? ? y O1 Al O2 161.4(2) ? ? ? y Al O1 Al 99.2(1) ? ? ? y Al O2 Al 128.8(1) ? ? ? y data_Na-hex loop_ _audit_conform.dict_name _audit_conform.dict_version _audit_conform.dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Na1.04 Mg1.88 Al4.64 Si1.32 O12' _chemical_formula_structural 'Na1.04 Mg1.88 Al4.64 Si1.32 O12' _chemical_formula_analytical 'Na1.04 Mg1.88 Al4.64 Si1.32 O12' _chemical_formula_sum 'Na1.04 Mg1.88 Al4.64 Si1.32 O12' _chemical_formula_weight 423.86 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system hexagonal _space_group_name_H-M_alt P63/m _space_group_name_Hall -P6c loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 1 x, y, z 2 -y, x-y, z 3 -x;y, -x, z 4 -x, -y, z+1/2 5 y, -x+y, z+1/2 6 x-y, x, z+1/2 _cell_length_a 8.7274(2) _cell_length_b 8.7274(2) _cell_length_c 2.7663(1) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 182.47(1) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; powder were fixed using aceton on a quartz or a Si plate holder. ; _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 ? _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 22000000 _pd_prep_temperature 1773 # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The 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 ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source 'rotating target' _diffrn_source_target Cr _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_measurement_device_type 'Rigaku RINT2500V' _diffrn_detector 'NaI scintillation counter' _diffrn_detector_type ? # make or model of detector _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. _diffrn_radiation_wavelength 2.2897 _diffrn_radiation_monochromator 'pyrolytic graphite monochromator' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 6500 _pd_meas_2theta_range_min 10 _pd_meas_2theta_range_max 140 _pd_meas_2theta_range_inc 0.02 # 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 ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The atomic displacement parameters for the two different oxygen sites were fixed at 1.0 for the Na-hexagonal aluminous phase. The atomic displacement parameter for the Na site was fixed at 2.0 which was reasonable and gave the lowest reliability factor. The site occupancy fractions were based on the results of the chemical analysis. ; # The next three items are given as text. _pd_proc_ls_profile_function 'pseudo-Voigt' _pd_proc_ls_background_function 'Legendre's polynomial' _pd_proc_ls_pref_orient_corr ; March-Dollase function ; _pd_proc_ls_prof_R_factor 0.1027 _pd_proc_ls_prof_wR_factor 0.1366 _pd_proc_ls_prof_wR_expected 0.1014 _refine_ls_R_I_factor 0.0375 _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all 0.0225 _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? # options are 'sigma' (based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_parameters ? _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 ? _refine_ls_restrained_S_all 1.35 _refine_ls_shift/su_max ? _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 _pd_proc_2theta_range_max 140 _pd_proc_2theta_range_inc 0.02 _pd_proc_wavelength 2.2897 # Each refinement must be accompanied by a listing of the powder data # in CIF format. Each listing should be sent as a separate file consisting # of one data block containing a single powder profile. The value of # _pd_block_diffractogram_id is used to associate each refinement with # its corresponding powder profile, since it must match the value # of _pd_block_id in the file containing the powder data. A template # for supplying powder data in CIF format is available by ftp at # ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given # at ftp://ftp.iucr.org/pub/rietdataxmpl.cif. _pd_block_diffractogram_id ? # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection 'RIgaku application software' _computing_cell_refinement 'RIETAN-2000 (Izumi and Ikeda, 2000)' _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'RIETAN-2000 (Izumi and Ikeda, 2000)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_B_iso_or_equiv _atom_site_adp_type Na 0 0 0.25 0.46 ? 2a 3.30(29) Biso Mg 0.66667 0.33333 0.25 0.94 ? 2d 1.66(10) Biso Na 0.66667 0.33333 0.25 0.06 ? 2d 1.66(10) Biso Al 0.9892(2) 0.3408(3) 0.25 0.77 ? 6h 0.32(7) Biso Si 0.9892(2) 0.3408(3) 0.25 0.22 ? 6h 0.32(7) Biso O1 0.1224(5) 0.5925(6) 0.25 1.0 ? 6h 1.0 Biso O2 0.3116(3) 0.2045(4) 0.25 1.0 ? 6h 1.0 Biso # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. loop_ _atom_site_aniso_label _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 _atom_site_aniso_type_symbol ? ? ? ? ? ? ? ? #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na O2 2.393(3) ? ? y Na O2 2.764(3) ? ? y Mg O1 2.128(3) ? ? y Al O1 1.903(5) ? ? y Al O1 1.940(3) ? ? y Al O2 1.890(4) ? ? y Al O2 1.817(3) ? ? y O1 O1 2.373(6) ? ? y O2 O2 2.764(3) ? ? y 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al O1 90.7(2) ? ? ? y O1 Al O1 90.9(2) ? ? ? y O2 Al O2 99.2(2) ? ? ? y O1 Al O1 76.3(2) ? ? ? y O1 Al O2 161.2(2) ? ? ? y Al O1 Al 103.7(2) ? ? ? y Al O2 Al 127.5(1) ? ? ? y #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./