Crossover Point between Dialkoxy Disulfides (ROSSOR) and Thionosulfites ((RO)2SS): Prediction, Synthesis, and Structure
Eli Zysman-Colman; Neysa Nevins; Nicolas Eghbali; James P. Snyder; David N. Harpp; Journal of the American Chemical Society 128 (2006) 291–304; doi:10.1021/ja0559395

data_4110333
_publ_contact_author_address
;
      University of McGill
      Department of Chemistry
      Otto Maass Chemistry Building
      801 Sherbrooke St. West
      Montr\'eal, Qu\'ebec
      Canada H3A 2K6

;
_publ_contact_author_email       david.harpp@mcgill.ca
_publ_contact_author_fax         '+1 514 343 2382'
_publ_contact_author_name        'Dr. David N. Harpp'
_publ_contact_author_phone       '+1 514 343 6685'
_publ_section_title
;
 Crossover Point between Dialkoxy Disulfides (ROSSOR) and Thionosulfites
 ((RO)2SS): Prediction, Synthesis, and Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              291
_journal_page_last               304
_journal_paper_doi               10.1021/ja0559395
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C8 H8 O3 S'
_chemical_formula_sum            'C8 H8 O3 S'
_chemical_formula_weight         184.20
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.2787(2)
_cell_length_b                   8.8934(2)
_cell_length_c                   16.4636(3)
_cell_measurement_reflns_used    6628
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      54.90
_cell_measurement_theta_min      2.68
_cell_volume                     1651.40(6)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SAINT (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10293
_diffrn_reflns_theta_full        55.16
_diffrn_reflns_theta_max         55.16
_diffrn_reflns_theta_min         5.37
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         119
_exptl_absorpt_coefficient_mu    3.200
_exptl_absorpt_correction_T_max  0.8300
_exptl_absorpt_correction_T_min  0.2400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         1037
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0811P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                859
_reflns_number_total             1037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0559395si20050906_100251.cif
_cod_data_source_block           harp74
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4110333