Synthesis of [N(CH3)4]2O3SOSO2(s) and [N(CH3)4]2[(O2SO)2SO2].SO2(s) Containing (SO4)(SO2)x2- x= 1, 2, Members of a New Class of Sulfur Oxydianions
Pablo Bruna; Andreas Decken; Friedrich Grein; Jack Passmore; J. Mikko Rautiainen; Stephanie Richardson; Tom Whidden; Inorganic Chemistry 52 (2013) 7193–7202; doi:10.1021/ic400805c

data_4335242
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 5A3
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
 Synthesis of [N(CH3)4]2O3SOSO2(s) and [N(CH3)4]2[(O2SO)2SO2].SO2(s)
 Containing (SO4)(SO2)x2- x= 1, 2, Members of a New Class of Sulfur
 Oxydianions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7193
_journal_page_last               7202
_journal_paper_doi               10.1021/ic400805c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C4 H12 N), O4 S, 3(O2 S)'
_chemical_formula_sum            'C8 H24 N2 O10 S4'
_chemical_formula_weight         436.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.117(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.270(3)
_cell_length_b                   15.265(4)
_cell_length_c                   13.278(5)
_cell_measurement_reflns_used    7012
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.4165
_cell_measurement_theta_min      2.538
_cell_volume                     1928.4(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.8132
_exptl_absorpt_correction_T_min  0.7380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             920
_exptl_crystal_recrystallization_method SO2
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+0.5498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                3023
_reflns_number_total             4327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400805c_si_002.cif
_cod_data_source_block           jp110146
_cod_original_cell_volume        1928.5(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335242