2,4-Bis(4-methoxyphenyl)-3-phenyl-1,3,2,4-thiazadiphosphetidine 2,4-disulfide
Rothenberger, Alexander; Shi, Weifeng; Acta Crystallographica Section E 63 (2007) o1798–o1799; doi:10.1107/S1600536807011191

data_2212997
_publ_section_title
;
 2,4-Bis(4-methoxyphenyl)-3-phenyl-1,3,2,4-thiazadiphosphetidine
 2,4-disulfide
;
_journal_coeditor_code           SG2146
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1798
_journal_page_last               o1799
_journal_paper_doi               10.1107/S1600536807011191
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H19 N O2 P2 S3'
_chemical_formula_moiety         'C20 H19 N O2 P2 S3'
_chemical_formula_sum            'C20 H19 N O2 P2 S3'
_chemical_formula_weight         463.48
_chemical_name_systematic
;
2,4-Bis(4-methoxyphenyl)-3-phenyl-1,3,2,4-thiazadiphosphetidine 2,4-disulfide
;
_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                 97.326(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.406(2)
_cell_length_b                   15.8954(17)
_cell_length_c                   13.0056(18)
_cell_measurement_reflns_used    7382
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      54.13
_cell_measurement_theta_min      4.03
_cell_volume                     2133.7(6)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, ????)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Stoe IPDSII'
_diffrn_measurement_method       rotation
_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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7973
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.771
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1728
_reflns_number_gt                2411
_reflns_number_total             4423
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2146.cif
_cod_data_source_block           I
_cod_original_cell_volume        2133.8(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212997
_cod_database_fobs_code          2212997