Thionations Using a P4S10-Pyridine Complex in Solvents Such as Acetonitrile and Dimethyl Sulfone
Jan Bergman; Birgitta Pettersson; Vedran Hasimbegovic; Per H. Svensson; Journal of Organic Chemistry 76 (2011) 1546–1553; doi:10.1021/jo101865y

data_4026096
_publ_contact_author_address
;
Department of Biosciences and Nutrition
Karolinska Institutet
SE 141 57 Huddinge,
Sweden
;
_publ_contact_author_email       jan.bergman@ki.se
_publ_contact_author_name        'Prof. Jan Bergman'
_publ_section_title
;
 Thionations Using a P4S10-Pyridine Complex in Solvents Such as
 Acetonitrile and Dimethyl Sulfone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1546
_journal_page_last               1553
_journal_paper_doi               10.1021/jo101865y
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C10 H10 N2 P2 S5'
_chemical_formula_sum            'C10 H10 N2 P2 S5'
_chemical_formula_weight         380.49
_chemical_name_systematic
; 
pentathiodiphosphoric acid-P,P-bis(pyridiniumbetain)
;
_space_group_IT_number           2
_symmetry_Int_Tables_number      2
_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                89.09(3)
_cell_angle_beta                 88.04(2)
_cell_angle_gamma                86.02(3)
_cell_formula_units_Z            4
_cell_length_a                   9.3820(19)
_cell_length_b                   12.916(3)
_cell_length_c                   13.290(3)
_cell_measurement_temperature    200(2)
_cell_volume                     1605.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5627
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_type   emperical
_exptl_crystal_colour            Needle
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       Plate
_exptl_crystal_F_000             776.0
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                5060
_reflns_number_total             5626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101865y_si_001.cif
_cod_data_source_block
pentathiodiphosphoricacid-P,P-bis(pyridiniumbetain)
_cod_database_code               4026096