Isolation and structures of sulfonium salts derived from thioethers: [{o-C6H4(CH2SMe)2}H][NbF6] and [{[9]aneS3}H][NbF6]
Jura, Marek; Levason, William; Reid, Gillian; Webster, Michael; Dalton Transactions  (2009) 7610–7612; doi:10.1039/b914120k

data_7002295
_publ_section_title
;
 Isolation and structures of sulfonium salts derived from thioethers:
 [{o-C6H4(CH2SMe)2}H][NbF6] and [{[9]aneS3}H][NbF6]
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7610
_journal_page_last               7612
_journal_paper_doi               10.1039/b914120k
_journal_year                    2009
_chemical_formula_moiety         'C6 H13 S3 1+, F6 Nb 1-'
_chemical_formula_sum            'C6 H13 F6 Nb S3'
_chemical_formula_weight         388.25
_chemical_name_common            '1,4,7-trithionan-1-ium hexafluoroniobate(V)'
_chemical_name_systematic
;
1,4,7-trithionan-1-ium hexafluoroniobate(V)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-04-20
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record
'2009-05-12 Added comment about H1 in _refine_special_details'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.929(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0262(15)
_cell_length_b                   9.8162(10)
_cell_length_c                   11.3884(10)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1286.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18517
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0291P)^2^+1.0913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                2706
_reflns_number_total             2948
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b914120k.txt
_cod_data_source_block           09mj18
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002295