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_4026097
_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         'C5 H6 N, H2 O3 P S'
_chemical_formula_sum            'C5 H8 N O3 P S'
_chemical_formula_weight         193.16
_chemical_name_systematic
; 
Pyridinium dihydrogenmonothiophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.514(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9234(4)
_cell_length_b                   11.0214(5)
_cell_length_c                   9.0941(3)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.58
_cell_volume                     790.49(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f 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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20537
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.036(2)
_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   1.041
_refine_ls_hydrogen_treatment    const.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.3826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                1711
_reflns_number_total             1820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101865y_si_002.cif
_cod_data_source_block           Pyridiniumdihydrogenmonothiophosphate
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_formula_sum        'C5 H8 N O3 P S '
_cod_database_code               4026097