Ethyl 5-(triphenylphosphoranylidene)-1,2,3-thiadiazole-4-carboxylate
Ming-Guo Liu; Yang-Gen Hu; Acta Crystallographica Section E 62 (2006) o3206–o3208; doi:10.1107/S1600536806023403

data_2209874
_publ_section_title
;
 Ethyl 5-(triphenylphosphoranylidene)-1,2,3-thiadiazole-4-carboxylate
;
_journal_coeditor_code           HK2063
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3206
_journal_page_last               o3208
_journal_paper_doi               10.1107/S1600536806023403
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H20 N3 O2 P S'
_chemical_formula_moiety         'C23 H20 N3 O2 P S'
_chemical_formula_sum            'C23 H20 N3 O2 P S'
_chemical_formula_weight         433.45
_chemical_name_systematic
;
Ethyl 5-(triphenylphosphoranylidene)-1,2,3-thiadiazole-4-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.3770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4544(7)
_cell_length_b                   15.8511(10)
_cell_length_c                   13.2195(9)
_cell_measurement_reflns_used    6047
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.34
_cell_volume                     2184.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 4K 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18972
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9299
_exptl_absorpt_correction_T_min  0.9299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0620
_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^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                3901
_reflns_number_total             5188
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2063.cif
_cod_data_source_block           I
_cod_original_cell_volume        2184.3(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209874
_cod_database_fobs_code          2209874