6-Benzyl-2-[(triphenyl-λ^5^-phosphanylidene)amino]-4,5,6,7-tetrahydrothieno[2,3-<i>c</i>]pyridine-3-carbonitrile
Chen, Hong; Yan, Kai; Acta Crystallographica Section E 67 (2011) o2548–; doi:10.1107/S1600536811035082

data_2231797
_publ_section_title
;
 6-Benzyl-2-[(triphenyl-\l^5^-phosphanylidene)amino]-4,5,6,7-tetrahydrothieno[2,3-<i>c</i>]pyridine-3-carbonitrile
;
_journal_coeditor_code           AA2019
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2548
_journal_paper_doi               10.1107/S1600536811035082
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C33 H28 N3 P S'
_chemical_formula_moiety         'C33 H28 N3 P S'
_chemical_formula_sum            'C33 H28 N3 P S'
_chemical_formula_weight         529.61
_chemical_melting_point          463
_chemical_name_systematic
;
6-Benzyl-2-[(triphenyl-\l^5^-phosphanylidene)amino]-4,5,6,7-
tetrahydrothieno[2,3-<i>c</i>]pyridine-3-carbonitrile
;
_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                 101.970(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.926(4)
_cell_length_b                   27.537(12)
_cell_length_c                   11.719(5)
_cell_measurement_reflns_used    6648
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.73
_cell_volume                     2818(2)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'CCD Profile fitting scans'
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25582
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0593P)^2^+0.6222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                5506
_reflns_number_total             6415
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            aa2019.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231797
_cod_database_fobs_code          2231797