###############################################################################
### 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 Crystallogr., Sect. A, 47 (1991) 655-685].
#
# The current version of the powder CIF dictionary, which contains definitions
# 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
#===============================================================================
# 1. GLOBAL DATA
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
_audit_creation_method
; from .lst and *.dst using lst2cif (Dilanian and Izumi, 2011)
;
_audit_creation_date
_audit_author_name '?'
_audit_update_record
; ?
;
# SUBMISSION DETAILS
_publ_contact_author_name '?'
_publ_contact_author_address
; ?
;
_publ_contact_author_email ?
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_contact_letter
; ?
;
_publ_requested_journal '?'
_publ_requested_coeditor_name '?'
_publ_requested_category ?
#===============================================================================
# 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
; ?
;
_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
? #<--'Last name, first name'
; ?
;
; ?
;
#===============================================================================
# 4. TEXT
_publ_section_synopsis
; ?
;
_publ_section_abstract
; ?
;
_publ_section_comment
; ?
;
_publ_section_exptl_prep # Details of the preparation of the sample(s)
# should be given here.
; ?
;
_publ_section_exptl_refinement
; ?
;
_publ_section_references
; ?
;
_publ_section_figure_captions
; ?
;
_publ_section_acknowledgements
; ?
;
# Pointers to the data blocks containing information on phases
loop_
_pd_phase_block_id
_phase_1
_phase_2
#===============================================================================
# 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_phase_1
_pd_block_id _phase_1
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common '?'
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety '?'
_chemical_formula_structural '?'
_chemical_formula_analytical '?'
_chemical_formula_sum 'Ca3 O9 Rh3'
_chemical_formula_weight 572.945
_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
Rh Rh3+ -1.0723 1.0749 'International Tables for Crystallography, Vol. C'
Ca Ca2+ 0.2288 0.3629 'International Tables for Crystallography, Vol. C'
O O- 0.0103 0.0073 'International Tables for Crystallography, Vol. C'
#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/m 1'
_symmetry_space_group_name_Hall '-P 2yb'
_symmetry_Int_Tables_number 11
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-y+1/2,z
_cell_length_a 12.51140(12)
_cell_length_b 3.12406(3)
_cell_length_c 8.85794(8)
_cell_angle_alpha 90
_cell_angle_beta 103.9510(6)
_cell_angle_gamma 90
_cell_volume 336.012(5)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z 2
_cell_measurement_temperature ?
_cell_special_details
?
_exptl_crystal_density_diffrn 5.6629
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 534.00
# 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.
; ?
;
_pd_spec_mount_mode transmission
_pd_spec_shape cylinder
_pd_char_particle_morphology ?
_pd_char_colour ?
# 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 ?
_exptl_absorpt_coefficient_mu 11.4969
# The next four fields are normally only needed for transmission experiments.
_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 ?
_diffrn_source 'synchrotron'
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_radiation_type ?
_diffrn_measurement_device_type '?'
_diffrn_detector '?'
_diffrn_detector_type ?
_pd_meas_scan_method step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details
; ?
;
_diffrn_radiation_wavelength 0.77462
_diffrn_radiation_monochromator ?
# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.
_pd_meas_number_of_points 7201
_pd_meas_2theta_range_min 3.0000
_pd_meas_2theta_range_max 75.0000
_pd_meas_2theta_range_inc 0.0100
# 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 next three items are given as text.
_pd_calc_method 'Rietveld Refinement'
_pd_proc_ls_profile_function 'split pseudo-Voigt function'
_pd_proc_ls_background_function 'Legendre polynomials'
_pd_proc_ls_pref_orient_corr
; ?
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and r = 1.0(0)
_pd_proc_ls_prof_R_factor 0.04721
_pd_proc_ls_prof_wR_factor 0.06228
_pd_proc_ls_prof_wR_expected 0.04119
_refine_ls_R_I_factor 0.00909
_refine_ls_R_Fsqd_factor 0.00474
_refine_ls_R_factor_all 0.00476
_refine_special_details
; ?
;
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details 1/y~i~
# The following line must be commented out in the absence of H atoms.
#_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_parameters 80
_refine_ls_number_restraints 0
_refine_ls_number_constraints 4
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all 1.5118
_refine_ls_restrained_S_all ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max 0.0
_refine_ls_shift/su_mean ?
_refine_diff_density_max 0.0
_refine_diff_density_min 0.0
# 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 3.0000
_pd_proc_2theta_range_max 74.7500
_pd_proc_2theta_range_inc 0.0100
_pd_proc_wavelength ?
loop_
_pd_phase_id
_pd_phase_block_id
_pd_phase_mass_%
1 _phase_1 85.32
2 _phase_2 14.68
# 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 ?
_computing_cell_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction ?
_computing_structure_solution ?
_computing_structure_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics 'VESTA (Momma and Izumi, 2008)'
_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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
O1 0.8215(6) 0.75 0.8756(10) 1 2 e Uiso 0.01267 O
O2 0.6152(6) 0.25 0.7842(9) 1 2 e Uiso 0.01267 O
O3 0.5488(6) 0.25 0.1325(9) 1 2 e Uiso 0.01267 O
O4 0.5535(6) 0.25 0.4159(10) 1 2 e Uiso 0.01267 O
O5 0.7031(6) 0.75 0.3271(10) 1 2 e Uiso 0.01267 O
O6 0.8115(6) 0.25 0.5802(9) 1 2 e Uiso 0.01267 O
O7 0.7878(6) 0.25 0.1278(9) 1 2 e Uiso 0.01267 O
O8 0.9118(6) 0.75 0.3879(9) 1 2 e Uiso 0.01267 O
O9 0.9890(6) 0.75 0.1170(9) 1 2 e Uiso 0.01267 O
Ca1 0.6718(2) 0.75 0.6175(3) 1 2 e Uiso 0.0111(7) Ca
Ca2 0.6505(2) 0.75 0.9941(3) 1 2 e Uiso 0.0096(7) Ca
Ca3 0.0521(2) 0.25 0.3318(3) 1 2 e Uiso 0.0115(7) Ca
Rh1 0.54318(8) 0.75 0.27037(13) 1 2 e Uiso 0.0043(3) Rh
Rh2 0.89248(9) 0.25 0.99875(12) 1 2 e Uiso 0.0045(3) Rh
Rh3 0.19426(8) 0.75 0.64612(13) 1 2 e Uiso 0.0049(3) Rh
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_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
O1 Rh2 1.988(5) . 1_555 ?
O1 Rh2 1.988(5) . 1_565 ?
O1 Ca1 2.584(8) . 1_555 ?
O1 Ca2 2.600(8) . 1_555 ?
O1 O9 2.61(1) . 1_556 ?
O1 Ca3 2.697(8) . 2_656 ?
O1 O7 2.84(1) . 1_556 ?
O1 O7 2.84(1) . 1_566 ?
O1 O2 2.958(9) . 1_555 ?
O1 O2 2.958(9) . 1_565 ?
O1 O6 3.02(1) . 1_555 ?
O1 O6 3.02(1) . 1_565 ?
O2 Rh1 1.923(7) . 2_646 ?
O2 Ca1 2.372(6) . 1_555 ?
O2 Ca1 2.372(6) . 1_545 ?
O2 Ca2 2.387(6) . 1_555 ?
O2 Ca2 2.387(6) . 1_545 ?
O2 O3 2.814(9) . 2_646 ?
O2 O3 2.814(9) . 2_656 ?
O2 O4 2.869(9) . 2_646 ?
O2 O4 2.869(9) . 2_656 ?
O2 O1 2.958(9) . 1_555 ?
O2 O1 2.958(9) . 1_545 ?
O3 Rh1 1.995(5) . 1_555 ?
O3 Rh1 1.995(5) . 1_545 ?
O3 Ca2 2.475(7) . 2_646 ?
O3 O4 2.50(1) . 1_555 ?
O3 Ca2 2.513(7) . 1_554 ?
O3 Ca2 2.513(7) . 1_544 ?
O3 O5 2.745(8) . 1_555 ?
O3 O5 2.745(8) . 1_545 ?
O3 O2 2.814(9) . 2_646 ?
O3 O2 2.814(9) . 2_656 ?
O3 O3 2.84(1) . 2_645 ?
O3 O3 2.84(1) . 2_655 ?
O3 O7 3.00(1) . 1_555 ?
O4 Rh1 2.010(5) . 1_555 ?
O4 Rh1 2.010(5) . 1_545 ?
O4 O3 2.50(1) . 1_555 ?
O4 Ca1 2.558(7) . 1_555 ?
O4 Ca1 2.558(7) . 1_545 ?
O4 O5 2.697(9) . 1_555 ?
O4 O5 2.697(9) . 1_545 ?
O4 O4 2.72(1) . 2_646 ?
O4 O4 2.72(1) . 2_656 ?
O4 Ca1 2.762(8) . 2_646 ?
O4 O2 2.869(9) . 2_646 ?
O4 O2 2.869(9) . 2_656 ?
O5 Rh1 1.942(7) . 1_555 ?
O5 Rh3 2.000(5) . 2_646 ?
O5 Rh3 2.000(5) . 2_656 ?
O5 O8 2.536(9) . 1_555 ?
O5 Ca1 2.694(8) . 1_555 ?
O5 O4 2.697(9) . 1_555 ?
O5 O4 2.697(9) . 1_565 ?
O5 O3 2.745(8) . 1_555 ?
O5 O3 2.745(8) . 1_565 ?
O5 O7 2.754(9) . 1_555 ?
O5 O7 2.754(9) . 1_565 ?
O5 O6 2.800(9) . 1_555 ?
O5 O6 2.800(9) . 1_565 ?
O5 Ca2 2.863(9) . 1_554 ?
O6 Rh3 1.989(8) . 2_646 ?
O6 Ca3 2.306(6) . 2_646 ?
O6 Ca3 2.306(6) . 2_656 ?
O6 Ca1 2.426(6) . 1_555 ?
O6 Ca1 2.426(6) . 1_545 ?
O6 O5 2.800(9) . 1_555 ?
O6 O5 2.800(9) . 1_545 ?
O6 O8 2.819(9) . 1_555 ?
O6 O8 2.819(9) . 1_545 ?
O6 O1 3.02(1) . 1_555 ?
O6 O1 3.02(1) . 1_545 ?
O7 Rh2 1.935(8) . 1_554 ?
O7 Rh3 1.961(8) . 2_646 ?
O7 Ca2 2.411(6) . 1_554 ?
O7 Ca2 2.411(6) . 1_544 ?
O7 O5 2.754(9) . 1_555 ?
O7 O5 2.754(9) . 1_545 ?
O7 O1 2.84(1) . 1_554 ?
O7 O1 2.84(1) . 1_544 ?
O7 O8 2.904(9) . 1_555 ?
O7 O8 2.904(9) . 1_545 ?
O7 O9 2.98(1) . 1_555 ?
O7 O9 2.98(1) . 1_545 ?
O7 O3 3.00(1) . 1_555 ?
O8 Rh3 2.025(5) . 2_646 ?
O8 Rh3 2.025(5) . 2_656 ?
O8 Ca3 2.415(8) . 2_656 ?
O8 Ca3 2.488(6) . 1_655 ?
O8 Ca3 2.488(6) . 1_665 ?
O8 O5 2.536(9) . 1_555 ?
O8 O9 2.79(1) . 1_555 ?
O8 O6 2.819(9) . 1_555 ?
O8 O6 2.819(9) . 1_565 ?
O8 O7 2.904(9) . 1_555 ?
O8 O7 2.904(9) . 1_565 ?
O9 Rh2 2.094(5) . 1_554 ?
O9 Rh2 2.094(5) . 1_564 ?
O9 Ca3 2.441(6) . 1_655 ?
O9 Ca3 2.441(6) . 1_665 ?
O9 O1 2.61(1) . 1_554 ?
O9 O9 2.66(1) . 2_755 ?
O9 O8 2.79(1) . 1_555 ?
O9 O7 2.98(1) . 1_555 ?
O9 O7 2.98(1) . 1_565 ?
Ca1 O2 2.372(6) . 1_555 ?
Ca1 O2 2.372(6) . 1_565 ?
Ca1 O6 2.426(6) . 1_555 ?
Ca1 O6 2.426(6) . 1_565 ?
Ca1 O4 2.558(7) . 1_555 ?
Ca1 O4 2.558(7) . 1_565 ?
Ca1 O1 2.584(8) . 1_555 ?
Ca1 O5 2.694(8) . 1_555 ?
Ca1 O4 2.762(8) . 2_656 ?
Ca2 O2 2.387(6) . 1_555 ?
Ca2 O2 2.387(6) . 1_565 ?
Ca2 O7 2.411(6) . 1_556 ?
Ca2 O7 2.411(6) . 1_566 ?
Ca2 O3 2.475(7) . 2_656 ?
Ca2 O3 2.513(7) . 1_556 ?
Ca2 O3 2.513(7) . 1_566 ?
Ca2 O1 2.600(8) . 1_555 ?
Ca2 O5 2.863(9) . 1_556 ?
Ca2 Rh1 3.062(3) . 1_556 ?
Ca3 O6 2.306(6) . 2_646 ?
Ca3 O6 2.306(6) . 2_656 ?
Ca3 O8 2.415(8) . 2_646 ?
Ca3 O9 2.441(6) . 1_455 ?
Ca3 O9 2.441(6) . 1_445 ?
Ca3 O8 2.488(6) . 1_455 ?
Ca3 O8 2.488(6) . 1_445 ?
Ca3 O1 2.697(8) . 2_646 ?
Rh1 O2 1.923(7) . 2_656 ?
Rh1 O5 1.942(7) . 1_555 ?
Rh1 O3 1.995(5) . 1_555 ?
Rh1 O3 1.995(5) . 1_565 ?
Rh1 O4 2.010(5) . 1_555 ?
Rh1 O4 2.010(5) . 1_565 ?
Rh1 Ca2 3.062(3) . 1_554 ?
Rh2 O7 1.935(8) . 1_556 ?
Rh2 O1 1.988(5) . 1_555 ?
Rh2 O1 1.988(5) . 1_545 ?
Rh2 O9 2.094(5) . 1_546 ?
Rh2 O9 2.094(5) . 1_556 ?
Rh3 O7 1.961(8) . 2_656 ?
Rh3 O6 1.989(8) . 2_656 ?
Rh3 O5 2.000(5) . 2_646 ?
Rh3 O5 2.000(5) . 2_656 ?
Rh3 O8 2.025(5) . 2_646 ?
Rh3 O8 2.025(5) . 2_656 ?
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
O3 O4 O1 133.3(3) 1_555 . 1_555 ?
O3 O4 O2 167.6(4) 1_555 . 1_555 ?
#===============================================================================
data_phase_2
_pd_block_id _phase_2
#11. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common '?'
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety '?'
_chemical_formula_structural '?'
_chemical_formula_analytical '?'
_chemical_formula_sum ''
_chemical_formula_weight 134.904
_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
Rh Rh3+ -1.0723 1.0749 'International Tables for Crystallography, Vol. C'
Ca Ca2+ 0.2288 0.3629 'International Tables for Crystallography, Vol. C'
O O- 0.0103 0.0073 'International Tables for Crystallography, Vol. C'
#===============================================================================
#12. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting cubic
_symmetry_space_group_name_H-M 'P a -3'
_symmetry_space_group_name_Hall '-P 2ac 2ab 3'
_symmetry_Int_Tables_number 205
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,-y,z+1/2
3 -x,y+1/2,-z+1/2
4 x+1/2,-y+1/2,-z
5 z,x,y
6 z+1/2,-x+1/2,-y
7 -z+1/2,-x,y+1/2
8 -z,x+1/2,-y+1/2
9 y,z,x
10 -y,z+1/2,-x+1/2
11 y+1/2,-z+1/2,-x
12 -y+1/2,-z,x+1/2
13 -x,-y,-z
14 x+1/2,y,-z+1/2
15 x,-y+1/2,z+1/2
16 -x+1/2,y+1/2,z
17 -z,-x,-y
18 -z+1/2,x+1/2,y
19 z+1/2,x,-y+1/2
20 z,-x+1/2,y+1/2
21 -y,-z,-x
22 y,-z+1/2,x+1/2
23 -y+1/2,z+1/2,x
24 y+1/2,z,-x+1/2
_cell_length_a 4.8440(1)
_cell_length_b 4.8440(1)
_cell_length_c 4.8440(1)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 113.66(1)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z 4
_cell_measurement_temperature ?
_cell_special_details
?
_exptl_crystal_density_diffrn 7.8837
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 244.00
# 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.
; ?
;
_pd_spec_mount_mode transmission
_pd_spec_shape cylinder
_pd_char_particle_morphology ?
_pd_char_colour ?
# 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 ?
_exptl_absorpt_coefficient_mu 16.9001
# The next four fields are normally only needed for transmission experiments.
_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
#===============================================================================
#13. 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 ?
_diffrn_source 'synchrotron'
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_radiation_type ?
_diffrn_measurement_device_type '?'
_diffrn_detector '?'
_diffrn_detector_type ?
_pd_meas_scan_method step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details
; ?
;
_diffrn_radiation_wavelength 0.77462
_diffrn_radiation_monochromator ?
# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.
_pd_meas_number_of_points 7201
_pd_meas_2theta_range_min 3.0000
_pd_meas_2theta_range_max 75.0000
_pd_meas_2theta_range_inc 0.0100
# 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 ?
#===============================================================================
#14. 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_calc_method 'Rietveld Refinement'
_pd_proc_ls_profile_function 'split pseudo-Voigt function'
_pd_proc_ls_background_function 'Legendre polynomials'
_pd_proc_ls_pref_orient_corr
; ?
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and r = 1.0(0)
_pd_proc_ls_prof_R_factor 0.04721
_pd_proc_ls_prof_wR_factor 0.06228
_pd_proc_ls_prof_wR_expected 0.04119
_refine_ls_R_I_factor 0.00651
_refine_ls_R_Fsqd_factor 0.00466
_refine_ls_R_factor_all 0.00466
_refine_special_details
; ?
;
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details 1/y~i~
# The following line must be commented out in the absence of H atoms.
#_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_parameters 80
_refine_ls_number_restraints 0
_refine_ls_number_constraints 4
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all 1.5118
_refine_ls_restrained_S_all ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max 0.0
_refine_ls_shift/su_mean ?
_refine_diff_density_max 0.0
_refine_diff_density_min 0.0
# 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 3.0000
_pd_proc_2theta_range_max 74.7500
_pd_proc_2theta_range_inc 0.0100
_pd_proc_wavelength ?
loop_
_pd_phase_id
_pd_phase_block_id
_pd_phase_mass_%
1 _phase_1 85.32
2 _phase_2 14.68
# 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 ?
_computing_cell_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction ?
_computing_structure_solution ?
_computing_structure_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics 'VESTA (Momma and Izumi, 2008)'
_computing_publication_material ?
#===============================================================================
#15. 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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
O10 0.351(1) 0.351(1) 0.351(1) 1 8 c Uiso 0.013(4) O
Rh4 0 0 0 1 4 a Uiso 0.0042(5) Rh
#===============================================================================
#16. GEOMETRICAL PARAMETERS
_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
? ? ? ? ? ?
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
? ? ? ? ? ? ? ?