Synthesis and large crystal growth of a family of mixed-anionic methanesulfonate salts by anionic site-substitution: Na<sub>5</sub>(SO<sub>3</sub>CH<sub>3</sub>)<sub>4</sub>(X) (X = BF<sub>4</sub><sup>-</sup>, ClO<sub>4</sub><sup>-</sup>, PF<sub>6</sub><sup>-</sup>, I<sup>-</sup>).
Gabilondo, Eric A.; Halasyamani, P. Shiv; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5301–5310; doi:10.1039/d5dt00223k

data_7718274
_publ_section_title
;
 Synthesis and large crystal growth of a family of mixed-anionic
 methanesulfonate salts by anionic site-substitution:
 Na<sub>5</sub>(SO<sub>3</sub>CH<sub>3</sub>)<sub>4</sub>(X) (X =
 BF<sub>4</sub><sup>-</sup>, ClO<sub>4</sub><sup>-</sup>,
 PF<sub>6</sub><sup>-</sup>, I<sup>-</sup>).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5301
_journal_page_last               5310
_journal_paper_doi               10.1039/d5dt00223k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C4 H12 F6 Na5 O12 P S4'
_chemical_formula_sum            'C4 H12 F6 Na5 O12 P S4'
_chemical_formula_weight         640.30
_chemical_name_common            'Sodium Methanesulfonate Hexafluorophosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-02-23 deposited with the CCDC.	2025-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.946(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9030(3)
_cell_length_b                   5.54490(10)
_cell_length_c                   15.1892(6)
_cell_measurement_reflns_used    2861
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.37
_cell_volume                     1054.69(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8438
_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         26.724
_diffrn_reflns_theta_min         1.863
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0509 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.9108.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       Plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1246
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0290P)^2^+2.1465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1043
_reflns_number_total             1246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00223k2.cif
_cod_data_source_block           int1_a_pl
_cod_depositor_comments
'Adding full bibliography for 7718273--7718276.cif.'
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               7718274
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              16938
_shelx_hkl_checksum              38488