S-(2-pyridinyl)-1,1,3,3-tetramethylthiouronium hexafluorophosphate. A new reagent for the synthesis of 2-pyridinethiol esters.
Scardovi, Noemi; Garner, Philip P.; Protasiewicz, John D.; Organic letters 5 (2003) 1633–1635; doi:10.1021/ol034253j

data_1507286
_publ_section_title
;
 S-(2-pyridinyl)-1,1,3,3-tetramethylthiouronium hexafluorophosphate. A new
 reagent for the synthesis of 2-pyridinethiol esters.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              1633
_journal_page_last               1635
_journal_paper_doi               10.1021/ol034253j
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C10 H16 F6 N3 P S'
_chemical_formula_weight         355.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_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                 110.508(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6428(13)
_cell_length_b                   28.593(4)
_cell_length_c                   8.7453(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1555.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3181
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.369
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1452P)^2^+1.8700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2556
_reflns_number_gt                1613
_reflns_number_total             2387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol034253j.cif
_cod_data_source_block           ns1
_cod_database_code               1507286