#------------------------------------------------------------------------------
#$Date: 2022-09-10 04:16:53 +0300 (Sat, 10 Sep 2022) $
#$Revision: 277758 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/90/2109071.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2109071
loop_
_publ_author_name
'Matsuura, Mimiko'
'Okudera, Hiroki'
_publ_section_title
;
 Structures of Ca₅(VO₄)₃Cl and
 Ca~4.78(1)~Na~0.22~(PO₄)₃Cl~0.78~: positions of channel anions and
 repulsion on the anion in apatite-type compounds
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622008095
_journal_volume                  78
_journal_year                    2022
_chemical_compound_source        synthetic
_chemical_formula_structural     'Ca4.78(1) Na0.22 (P O4)3 Cl0.78'
_chemical_formula_sum            'Ca4.78 Cl0.78 Na0.22 O12 P3'
_chemical_formula_weight         509.20
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.5773(5)
_cell_length_b                   9.5773(5)
_cell_length_c                   6.8033(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    294
_cell_measurement_theta_max      54.97
_cell_measurement_theta_min      45.20
_cell_volume                     540.43(6)
_computing_cell_refinement       'Rigaku Control software, corrected with Si'
_computing_data_collection       'AFC-5S control'
_computing_data_reduction        'AFCPHI, SORT6 (parts of LSGCEX)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2011)'
_computing_publication_material  none
_computing_structure_refinement  'LSGCEX (Kihara, 1990)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Rigaku AFC5S diffractometer'
_diffrn_measurement_method       'integrated with \v/2θ scans'
_diffrn_radiation_monochromator  'graphite (002)'
_diffrn_radiation_source         'X-ray tube, 50kV 25mA'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23197
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.0760
_exptl_absorpt_correction_T_max  0.0083
_exptl_absorpt_correction_T_min  0.0079
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'spherical absorption correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.1292
_exptl_crystal_description       sphere
_exptl_crystal_F_000             504.6
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_crystal_size_rad          0.055
_pd_phase_name                   Ca4.78(1)Na0.22(PO4)3Cl0.78
_refine_diff_density_max         1.1932
_refine_diff_density_min         -1.3455
_refine_ls_extinction_coef       0.17(3)
_refine_ls_extinction_method     'B-C type 1 Lorenzian isotropic'
_refine_ls_goodness_of_fit_ref   0.8593
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     43
_refine_ls_number_reflns         1020
_refine_ls_number_restraints     10
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'weight proportional to sigma⁻²'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0286
_reflns_number_gt                1154
_reflns_number_total             1994
_reflns_observed_criterion       F>3u(F)
_reflns_threshold_expression
'F>3u(F) & (|Fobs.max|-|Fobs.min|)/|Fobs.min| < 1.0 among equivalents'
_cod_data_source_file            yh5022sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        540.43(7)
_cod_original_sg_symbol_Hall     '-P 6 c'
_cod_database_code               2109071
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
'-y, x-y, z'
'y, -x+y, -z'
'-x+y, -x, z'
'x-y, x, -z'
'-x, -y, z+1/2'
'x, y, -z+1/2'
'y, -x+y, z+1/2'
'-y, x-y, -z+1/2'
'x-y, x, z+1/2'
'-x+y, -x, -z+1/2'
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
Ca1 0.01426(10) 0.01426 0.00744(14) 0.00713 0.00000 0.00000
Na1 0.01426 0.01426 0.00744 0.00713 0.00000 0.00000
Ca2 0.01415(15) 0.01431(15) 0.00897(12) 0.00633(13) 0.00000 0.00000
Na2 0.01415 0.01431 0.00897 0.00633 0.00000 0.00000
P 0.00981(17) 0.00803(16) 0.00701(15) 0.00572(14) 0.00000 0.00000
O1 0.0245(7) 0.0175(6) 0.0142(6) 0.0172(6) 0.00000 0.00000
O2 0.0112(6) 0.0137(6) 0.0377(10) 0.0058(5) 0.00000 0.00000
O3a 0.048(4) 0.023(2) 0.0088(19) 0.026(3) -0.017(3) -0.010(2)
O3b 0.048 0.023 0.0088 0.026 -0.017 -0.010
Cl 0.0134(3) 0.0134 0.298(11) 0.00671 0.00000 0.00000
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Ca1 0.956 0.333333 0.666667 0.00283(7) Ueq 0.01199(9) Ca
Na1 0.044 0.333333 0.666667 0.00283 Ueq 0.01199 Na
Ca2 0.956 0.25873(5) -0.00275(5) 0.250000 Ueq 0.01283(12) Ca
Na2 0.044 0.25873 -0.00275 0.250000 Ueq 0.01283 Na
P 1.0 0.40282(6) 0.37130(5) 0.250000 Ueq 0.00773(13) P
O1 1.0 0.3367(2) 0.48791(19) 0.250000 Ueq 0.0158(5) O
O2 1.0 0.58862(19) 0.46376(19) 0.250000 Ueq 0.0210(6) O
O3a 0.5 0.359(3) 0.271(2) 0.0526(10) Ueq 0.023(2) O
O3b 0.5 0.343(3) 0.257(2) 0.0841(10) Ueq 0.023 O
Cl 0.39 0.000000 0.000000 0.0526 Ueq 0.108 Cl
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca 0 9.56 0.226 0.306 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.3'
Na 0 0.44 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.3'
P 0 6 0.102 0.095 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.3'
O 0 24 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.3'
Cl 0 1.56 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.3'
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
O1 P O2 111.10(11) 1_555 1_555 1_555
O1 P O3a 111.3(12) 1_555 1_555 1_555
O1 P O3b 113.0(13) 1_555 1_555 1_555
O2 P O3a 103.1(9) 1_555 1_555 1_555
O2 P O3b 109.5(10) 1_555 1_555 1_555
O3a P O3b 108.2(8) 1_555 1_555 8_555
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_multiplicity
Ca1 O1 1_555 2.4113(16) 3
Ca1 O2 6_555 2.4518(16) 3
Ca1 O3a 6_555 2.72(3) 3
Ca1 O3b 6_555 2.87(3) 3
Na1 O1 1_555 2.4113 3
Na1 O2 6_555 2.4518 3
Na1 O3a 6_555 2.72 3
Na1 O3b 6_555 2.87 3
Ca2 O1 5_555 2.828(2) 1
Ca2 O2 3_655 2.3043(17) 1
Ca2 O3a 1_555 2.659(19) 2
Ca2 O3a 4_555 2.241(16) 2
Ca2 O3b 1_555 2.47(2) 2
Ca2 O3b 4_555 2.407(14) 2
Ca2 Cl 1_555 2.8301(5) 2
Na2 O1 5_555 2.828 1
Na2 O2 3_655 2.3043 1
Na2 O3a 1_555 2.659 2
Na2 O3a 4_555 2.241 2
Na2 O3b 1_555 2.47 2
Na2 O3b 4_555 2.407 2
Na2 Cl 1_555 2.8301 2
P O1 1_555 1.535(2) 1
P O2 1_555 1.5411(17) 1
P O3a 1_555 1.582(12) 2
P O3b 1_555 1.472(13) 2

_cod_database_fobs_code 2109071
