NaCo7.38(PO4)4Cl4 in a series of homeotype compounds with stable cationic substructures derived from the sulphohalite archetype
Yakubovich, Olga; Kiriukhina, Galina; Simonov, Sergei; Volkov, Anatoliy; Dimitrova, Olga; CrystEngComm 25 (2023) 6006–6016; doi:10.1039/D3CE00819C

data_7247463
_publ_section_title
;
 NaCo7.38(PO4)4Cl4 in a series of homeotype compounds with stable cationic
 substructures derived from the sulphohalite archetype
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6006
_journal_page_last               6016
_journal_paper_doi               10.1039/D3CE00819C
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Cl8 Co14.76 O32 P8, 2(Na)'
_chemical_formula_sum            'Cl4 Co7.38 Na O16 P4'
_chemical_formula_weight         979.57
_chemical_name_systematic        'sodium cobalt (II, III) posphate cloride'
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-08-05 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1150(4)
_cell_length_b                   9.1150(4)
_cell_length_c                   10.2056(6)
_cell_measurement_reflns_used    1696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.723
_cell_measurement_theta_min      2.975
_cell_volume                     847.91(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.2283
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.987
_diffrn_reflns_theta_min         2.996
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.157
_exptl_absorpt_correction_T_max  1.272
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.837
_exptl_crystal_description       irregular
_exptl_crystal_F_000             933
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.012
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.789
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0164
_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^)+(0.0140P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0360
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                638
_reflns_number_total             651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00819c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7247463.cif.'
_cod_original_cell_volume        847.91(9)
_cod_database_code               7247463
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.908
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              10454