(<i>S</i>)-Diethyl {(4-fluorophenyl)[5-(4-methoxyphenyl)-1,3,4-thiadiazol-2-ylamino]methyl}phosphonate
Wan, Rong; Han, Feng; Zhang, Jin-jun; Yin, Li-he; Wang, Jin-tang; Acta Crystallographica Section E 63 (2007) o4158–o4158; doi:10.1107/S1600536807046521

data_2215542
_publ_section_title
;(<i>S</i>)-Diethyl
 {(4-fluorophenyl)[5-(4-methoxyphenyl)-1,3,4-thiadiazol-2-ylamino]methyl}phosphonate
;
_journal_coeditor_code           HK2321
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4158
_journal_page_last               o4158
_journal_paper_doi               10.1107/S1600536807046521
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H23 F N3 O4 P S'
_chemical_formula_moiety         'C20 H23 F N3 O4 P S'
_chemical_formula_sum            'C20 H23 F N3 O4 P S'
_chemical_formula_weight         451.44
_chemical_melting_point          465
_chemical_name_systematic
;
(S)-Diethyl {(4-fluorophenyl)[5-(4-methoxyphenyl)-1,3,4-thiadiazol-2-
ylamino]methyl}phosphonate
;
_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           SHELXL-97
_cell_angle_alpha                110.44(3)
_cell_angle_beta                 98.80(3)
_cell_angle_gamma                100.58(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4140(19)
_cell_length_b                   10.227(2)
_cell_length_c                   12.923(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     1113.7(5)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4656
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9505
_exptl_absorpt_correction_T_min  0.9271
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4374
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0497
_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^)+(0.088P)^2^+2.5493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                3276
_reflns_number_total             4374
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2321.cif
_cod_data_source_block           I
_cod_database_code               2215542
_cod_database_fobs_code          2215542