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_7718275
_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 I Na5 O12 S4'
_chemical_formula_sum            'C4 H12 I Na5 O12 S4'
_chemical_formula_weight         622.23
_chemical_name_common            'Sodium Methanesulfonate Iodide'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-23 deposited with the CCDC.	2025-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.489(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4118(4)
_cell_length_b                   5.5158(2)
_cell_length_c                   14.9258(5)
_cell_measurement_reflns_used    2734
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      29.321
_cell_measurement_theta_min      1.939
_cell_volume                     997.66(6)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       Rotation
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31164
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.321
_diffrn_reflns_theta_min         1.939
_diffrn_source                   Mo
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing R.H. Acta Crystallogr A, 1995, 51, 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.6800
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.7321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1840
_reflns_number_total             2734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00223k2.cif
_cod_data_source_block           int2_a
_cod_depositor_comments
'Adding full bibliography for 7718273--7718276.cif.'
_cod_database_code               7718275
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.780
_exptl_crystal_lustre            clear
_exptl_crystal_primary           yellow
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'