Ethyl 5-amino-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-1<i>H</i>-pyrazole-4-carboxylate dimethyl sulfoxide hemisolvate
Abu Thaher, Bassam; Koch, Pierre; Schollmeyer, Dieter; Laufer, Stefan; Acta Crystallographica Section E 68 (2012) o917–o918; doi:10.1107/S1600536812008264

data_2233761
_publ_section_title
;
 Ethyl
 5-amino-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-1<i>H</i>-pyrazole-4-carboxylate
 dimethyl sulfoxide hemisolvate
;
_journal_coeditor_code           BT5829
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o917
_journal_page_last               o918
_journal_paper_doi               10.1107/S1600536812008264
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C17 H13 Cl3 N4 O2, 0.5C2 H6 O S'
_chemical_formula_moiety         'C17 H13 Cl3 N4 O2, 0.5(C2 H6 O S)'
_chemical_formula_sum            'C18 H16 Cl3 N4 O2.5 S0.5'
_chemical_formula_weight         450.73
_chemical_name_systematic
;
Ethyl 5-amino-3-(pyridin-4-yl)-1-(2,4,6-trichlorophenyl)-1<i>H</i>-pyrazole-4-
carboxylate dimethyl sulfoxide hemisolvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.453(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.501(2)
_cell_length_b                   10.3222(15)
_cell_length_c                   14.889(2)
_cell_measurement_reflns_used    3021
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.2
_cell_volume                     2040.5(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>a</i>)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'CCD scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1618
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9562
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2008<i>b</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.393
_refine_ls_abs_structure_details 'Flack (1983), 4289 Friedel pairs'
_refine_ls_abs_structure_Flack   0.61(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9562
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1075
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                5575
_reflns_number_total             9562
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5829.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233761
_cod_database_fobs_code          2233761