Galeite, Na15(SO4)5ClF4, and Schairerite, Na21(SO4)7ClF6: Phase Transitions, Thermal Expansion and Thermal Stability
Avdontceva, Margarita S.; Zolotarev, Andrey A.; Shablinskii, Andrey P.; Bocharov, Vladimir N.; Kasatkin, Anatoly V.; Krivovichev, Sergey V.; Symmetry 15 (2023) 1871–; doi:10.3390/sym15101871

data_1570282
_publ_section_title
;
 Galeite, Na15(SO4)5ClF4, and Schairerite, Na21(SO4)7ClF6: Phase
 Transitions, Thermal Expansion and Thermal Stability
;
_journal_issue                   10
_journal_name_full               Symmetry
_journal_page_first              1871
_journal_paper_doi               10.3390/sym15101871
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'Cl F6 Na21 O28 S7'
_chemical_formula_sum            'Cl F6 Na21 O28 S7'
_chemical_formula_weight         1304.66
_space_group_crystal_system      trigonal
_space_group_IT_number           157
_space_group_name_Hall           'P 3 -2'
_space_group_name_H-M_alt        'P 3 1 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.1859(3)
_cell_length_b                   12.1859(3)
_cell_length_c                   19.3080(6)
_cell_measurement_reflns_used    10062
_cell_measurement_temperature    300.1(6)
_cell_measurement_theta_max      29.2730
_cell_measurement_theta_min      3.3370
_cell_volume                     2483.04(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.1(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -23.00  43.00   0.50    2.50    --   14.80  38.00  60.00  132
  2  \w    -26.00  43.00   0.50    2.50    --   14.80  19.00 150.00  138
  3  \w    -10.00  25.00   0.50    2.50    --   14.80  77.00-120.00   70
  4  \w    -15.00  37.00   0.50    2.50    --   14.80  57.00  90.00  104
  5  \w    -21.00  41.00   0.50    2.50    --   14.80  38.00 -30.00  124
  6  \w     -3.00  42.00   0.50    2.50    --   14.80  19.00-120.00   90
  7  \w    -10.00  17.00   0.50    2.50    --   14.80  57.00 -90.00   54
  8  \w     -6.00  19.00   0.50    2.50    --   14.80  77.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0572116000
_diffrn_orient_matrix_UB_12      -0.0018493000
_diffrn_orient_matrix_UB_13      0.0014085000
_diffrn_orient_matrix_UB_21      -0.0016672000
_diffrn_orient_matrix_UB_22      -0.0074124000
_diffrn_orient_matrix_UB_23      -0.0364937000
_diffrn_orient_matrix_UB_31      0.0352288000
_diffrn_orient_matrix_UB_32      0.0667732000
_diffrn_orient_matrix_UB_33      -0.0040087000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20070
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.629
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             1914
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                3578
_reflns_number_total             4396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            schairerite_300K.cif
_cod_data_source_block           sh_300k_auto
_cod_original_cell_volume        2483.04(14)
_cod_database_code               1570282
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Na21 S7 O28 Cl1 F1'
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61(13)
 0.39(13)
2. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O3)
;
_shelx_res_checksum              86654
_shelx_hkl_checksum              33057
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.321
_oxdiff_exptl_absorpt_empirical_full_min 0.787