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_7002296
_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         'C20 H28 F4 Nb S4 1+, F11 Nb2 1-, C H2 Cl2'
_chemical_formula_structural
'((C6 H4 (C2 H5 S)2)2 Nb F4) (Nb2 F11) (C H2 Cl2)'
_chemical_formula_sum            'C21 H30 Cl2 F15 Nb3 S4'
_chemical_formula_weight         1045.32
_chemical_name_common
;
catena-(tetrafluorobis(mu-1,2-bis(methylthiomethyl)benzene-
S,S')niobium(V)) undecafluoro-diniobate(V) dichloromethane solvate
;
_chemical_name_systematic
;
catena-(tetrafluorobis(\m-1,2-bis(methylthiomethyl)benzene-S,S')niobium(V))
undecafluoro-diniobate(V) dichloromethane solvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-05-11
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record
'2009-05-12 Added comment about refinement in _refine_special_details'
_cell_angle_alpha                114.254(6)
_cell_angle_beta                 109.892(6)
_cell_angle_gamma                97.279(6)
_cell_formula_units_Z            2
_cell_length_a                   12.5263(10)
_cell_length_b                   13.3180(15)
_cell_length_c                   14.3186(15)
_cell_measurement_reflns_used    66433
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1946.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39177
_diffrn_reflns_theta_full        27.77
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         3.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7935
_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    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.132
_refine_diff_density_min         -3.199
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8948
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+28.2339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2026
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                7883
_reflns_number_total             8948
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b914120k.txt
_cod_data_source_block           09mj17
_cod_database_code               7002296