2-Benzylamino-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphinane-2-thione
Jin-Song Chu; Shi-Guan Wan; Yan Yu; Chang Liu; Xing-Yu Yang; Acta Crystallographica Section E 63 (2007) o1540–o1541; doi:10.1107/S1600536807007076

data_2212856
_publ_section_title
;
 2-Benzylamino-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphinane-2-thione
;
_journal_coeditor_code           ER2014
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1540
_journal_page_last               o1541
_journal_paper_doi               10.1107/S1600536807007076
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C18 H22 N O2 P S'
_chemical_formula_moiety         'C18 H22 N O2 P S'
_chemical_formula_sum            'C18 H22 N O2 P S'
_chemical_formula_weight         347.40
_chemical_melting_point          420
_chemical_name_systematic
;
2-Benzylamino-5,5-dimethyl-4-phenyl-1,3,2-dioxaphosphinane-2-thione
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6955(6)
_cell_length_b                   15.2156(13)
_cell_length_c                   17.7423(15)
_cell_measurement_reflns_used    2389
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      19.58
_cell_measurement_theta_min      2.66
_cell_volume                     1807.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10076
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.145
_refine_ls_abs_structure_details 'Flack (1983), 1718 Friedel pairs'
_refine_ls_abs_structure_Flack   0.60(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4102
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                2602
_reflns_number_total             4102
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            er2014.cif
_cod_data_source_block           I
_cod_database_code               2212856
_cod_database_fobs_code          2212856