Ethyl 4-[1-(4-bromophenyl)-3-methyl-5-oxo-4,5-dihydro-1<i>H</i>-1,2,4-triazol-4-yliminomethyl]phenoxyacetate
Thamotharan, S; Parthasarathi, V; Sunagar, Vinay; Badami, Bharati; Schenk, Kurt J.; Acta Crystallographica Section E 59 (2003) o1272–o1274; doi:10.1107/S1600536803016969

data_2202565
_publ_section_title
;Ethyl
 4-[1-(4-bromophenyl)-3-methyl-5-oxo-4,5-dihydro-1<i>H</i>-1,2,4-triazol-4-yliminomethyl]phenoxyacetate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1272
_journal_page_last               o1274
_journal_paper_doi               10.1107/S1600536803016969
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C20 H19 Br N4 O4'
_chemical_formula_moiety         'C20 H19 Br N4 O4'
_chemical_formula_sum            'C20 H19 Br N4 O4'
_chemical_formula_weight         459.30
_chemical_melting_point          428
_chemical_name_systematic
;
Ethyl 4-[1-(4-bromophenyl)-3-methyl-5-oxo-4,5-dihydro-
1H-1,2,4-triazol-4-yliminomethyl]phenoxyacetate
;
_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   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.407(6)
_cell_angle_beta                 94.601(7)
_cell_angle_gamma                103.763(6)
_cell_formula_units_Z            4
_cell_length_a                   8.5176(7)
_cell_length_b                   15.5566(12)
_cell_length_c                   17.2643(15)
_cell_measurement_reflns_used    15908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.37
_cell_volume                     1999.5(3)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'Plane graphite'
_diffrn_radiation_source         'sealed LFF X-ray tube, 12 x 0.4 mm'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19783
_diffrn_reflns_theta_full        29.48
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.8606
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED in IPDS; Stoe & Cie, 1997)'
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       obelisk
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.419
_refine_ls_extinction_coef       0.0045(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         10124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.6771P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                6462
_reflns_number_total             10124
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6214.cif
_cod_data_source_block           I
_cod_database_code               2202565
_cod_database_fobs_code          2202565