2-(4-Methoxyphenyl)-4<i>H</i>-1,3,2-benzoxathiaphosphinine 2-sulfide
Osyanin, Vitaly A.; Ivleva, Elena A.; Rybakov, Victor B.; Klimochkin, Yurij N.; Acta Crystallographica Section E 67 (2011) o388–o389; doi:10.1107/S1600536810053146

data_2229254
_publ_section_title
;
 2-(4-Methoxyphenyl)-4<i>H</i>-1,3,2-benzoxathiaphosphinine 2-sulfide
;
_journal_coeditor_code           VM2065
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o388
_journal_page_last               o389
_journal_paper_doi               10.1107/S1600536810053146
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H13 O2 P S2'
_chemical_formula_moiety         'C14 H13 O2 P S2'
_chemical_formula_sum            'C14 H13 O2 P S2'
_chemical_formula_weight         308.35
_chemical_melting_point_gt       357
_chemical_melting_point_lt       358
_chemical_name_systematic
;
2-(4-Methoxyphenyl)-4<i>H</i>-1,3,2-benzoxathiaphosphinine 2-sulfide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL97
_cell_angle_alpha                94.322(4)
_cell_angle_beta                 91.121(4)
_cell_angle_gamma                111.675(4)
_cell_formula_units_Z            4
_cell_length_a                   10.0548(5)
_cell_length_b                   10.0804(5)
_cell_length_c                   14.8913(7)
_cell_measurement_reflns_used    11905
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.2294
_cell_measurement_theta_min      2.9775
_cell_volume                     1396.79(12)
_computing_cell_refinement
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_collection
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_reduction
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material  '<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27233
_diffrn_reflns_theta_full        67.36
_diffrn_reflns_theta_max         67.36
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[<i>CrysAlis PRO</i> (Oxford Diffraction, 2010); based on expressions
derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0361P)^2^+0.5302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                4175
_reflns_number_total             4926
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            vm2065.cif
_cod_data_source_block           I
_cod_database_code               2229254
_cod_database_fobs_code          2229254