Synthesis and Reactivity of Sulfur(II) Dications Stabilized Using Monodentate Ligands
Caleb D. Martin; Paul J. Ragogna; Inorganic Chemistry 49 (2010) 8164–8172; doi:10.1021/ic1012582

data_4316467
_publ_contact_author_address
;
Department of Chemistry, The University of Western Ontario, 
The Chemistry Building, 1151 Richmond Street, London, Ontario N6A 5B7, Canada
;
_publ_contact_author_email       pragogna@uwo.ca
_publ_contact_author_fax         1-519-661-3022
_publ_contact_author_name        'Paul J. Ragogna'
_publ_contact_author_phone       1-519-661-2111x87048
_publ_section_title
;
 Synthesis and Reactivity of Sulfur(II) Dications Stabilized Using
 Monodentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8164
_journal_page_last               8172
_journal_paper_doi               10.1021/ic1012582
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C31 H32 F6 N4 O6 S3'
_chemical_formula_weight         766.79
_space_group_IT_number           2
_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_method           SHELXL-97
_cell_angle_alpha                107.243(4)
_cell_angle_beta                 95.421(4)
_cell_angle_gamma                98.949(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3050(5)
_cell_length_b                   15.0203(10)
_cell_length_c                   15.1251(10)
_cell_measurement_reflns_used    18466
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      1.00
_cell_volume                     1760.2(2)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .938
_diffrn_measured_fraction_theta_max .938
_diffrn_measurement_device_type  'Bruker APEX 11 CCD'
_diffrn_measurement_method       '\f scans, and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9198
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_correction_T_min  0.9523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SAINT
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.976
_refine_diff_density_min         -.571
_refine_diff_density_rms         .079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         5645
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1348P)^2^+2.7080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2322
_reflns_number_gt                4575
_reflns_number_total             5645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1012582_si_002_5.cif
_cod_data_source_block           8Ph
_cod_database_code               4316467