2-(<i>p</i>-Methoxyphenyl)-3-[<i>o</i>-(methylaminothiocarbonyl)phenyl]-1,3,2-oxazaphospholidine 2-sulfide
Sheng-Lou Deng; Dong-Zhi Liu; Wei Li; Acta Crystallographica Section E 58 (2002) o1430–o1431; doi:10.1107/S1600536802021219

data_2201593
_publ_section_title
;2-(<i>p</i>-Methoxyphenyl)-3-[<i>o</i>-(methylaminothiocarbonyl)phenyl]-1,3,2-oxazaphospholidine
 2-sulfide
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1430
_journal_page_last               o1431
_journal_paper_doi               10.1107/S1600536802021219
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C17 H19 N2 O2 P S2'
_chemical_formula_moiety         'C17 H19 N2 O2 P S2'
_chemical_formula_sum            'C17 H19 N2 O2 P S2'
_chemical_formula_weight         378.43
_chemical_melting_point          373
_chemical_name_systematic
;
2-(p-Methoxyphenyl)-3-[o-(methylaminothiocarbonyl)phenyl]-1,3,2-
oxazaphospholidine 2-sulfide
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.180(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.905(3)
_cell_length_b                   19.091(5)
_cell_length_c                   20.384(5)
_cell_measurement_reflns_used    874
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.10
_cell_measurement_theta_min      2.43
_cell_volume                     3805.2(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15649
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.242
_refine_ls_abs_structure_details 'Flack (1983), 3497 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         10230
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.04P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                6200
_reflns_number_total             10230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6189.cif
_cod_data_source_block           2
_cod_original_cell_volume        3805.0(17)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2201593
_cod_database_fobs_code          2201593