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_7718276
_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 Cl Na5 O16 S4'
_chemical_formula_sum            'C4 H12 Cl Na5 O16 S4'
_chemical_formula_weight         594.78
_chemical_name_common            'Sodium Methanesulfonate Perchlorate'
_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             2025-02-19
_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                 103.263(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6653(7)
_cell_length_b                   5.5400(3)
_cell_length_c                   15.0037(9)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.39
_cell_volume                     1024.67(10)
_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      298.19
_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       Rotation
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0104
_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       -16
_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            35337
_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         28.312
_diffrn_reflns_theta_min         1.902
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0473 before and 0.0379 after correction.
The Ratio of minimum to maximum transmission is 0.9348.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_description       Plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0277(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2567
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0473P)^2^+0.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2379
_reflns_number_total             2567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00223k2.cif
_cod_data_source_block           attachedstandardfile_test_a_ccdc2417058
_cod_depositor_comments
'Adding full bibliography for 7718273--7718276.cif.'
_cod_database_code               7718276
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O7 = Cl1-O10 = Cl1A-O7A = Cl1A-O10A = Cl1A-O9A = Cl1-O9 = Cl1-O8 = Cl1A-O8
 1.42 with sigma of 0.01
 O7A-O10A = O10A-O9A = O9A-O7A = O10A-O8A = O9A-O8A = O7A-O8A
 2.3 with sigma of 0.02
 O7-O9 = O9-O10 = O10-O7 = O7-O8 = O9-O8 = O10-O8
 2.3 with sigma of 0.02
 Na3-O7A \\sim Na3-O7
 with sigma of 0.01
 Cl1A-O7A \\sim Cl1-O7 \\sim Cl1-O8 \\sim Cl1A-O8A \\sim Cl1-O10 \\sim
Cl1A-O10A \\sim Cl1-O9 \\sim Cl1A-O9A
 with sigma of 0.01
 Na3-O7A \\sim Na3-O9_$1 \\sim Na3-O9A_$1 \\sim Na3-O7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim O7A \\sim O10 \\sim O9A \\sim O8A \\sim O8 \\sim O9 \\sim Cl1A \\sim
Cl1 \\sim O10A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O7) = Uanis(O9) = Uanis(O9A) = Uanis(O7A)
Uanis(O8) = Uanis(O8A)
4. Others
 Sof(O10A)=Sof(O9A)=Sof(O7A)=Sof(Cl1A)=Sof(O8A)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(O7)=Sof(O8)=Sof(O10)=Sof(O9)=0.5*FVAR(2)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'