3-<i>tert</i>-Butyl-4-(4-chlorophenyl)-1-phenyl-1<i>H</i>-pyrazolo[3,4-<i>e</i>][1,4]thiazepin-7(4<i>H</i>,6<i>H</i>,8<i>H</i>)-one
Moreno-Fuquen, Rodolfo; Castillo, Juan C.; Abonia, Rodrigo; Tenorio, Juan C.; Ellena, Javier; IUCrData 1 (2016) x160608–; doi:10.1107/S2414314616006088

data_1543166
_publ_section_title
;
 3-<i>tert</i>-Butyl-4-(4-chlorophenyl)-1-phenyl-1<i>H</i>-pyrazolo[3,4-<i>e</i>][1,4]thiazepin-7(4<i>H</i>,6<i>H</i>,8<i>H</i>)-one
;
_journal_coeditor_code           HG4005
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x160608
_journal_paper_doi               10.1107/S2414314616006088
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C22 H22 Cl N3 O S'
_chemical_formula_moiety         'C22 H22 Cl N3 O S'
_chemical_formula_sum            'C22 H22 Cl N3 O S'
_chemical_formula_weight         411.94
_chemical_melting_point          518.0(10)
_chemical_name_common
(+-)-3-<i>tert</i>-Butyl-4-(4-chlorophenyl)-1-phenyl-1<i>H</i>-pyrazolo[3,4-<i>e</i>][1,4]thiazepin-7(4<i>H</i>,6<i>H</i>,8<i>H</i>)-one
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7478(3)
_cell_length_b                   25.2229(8)
_cell_length_c                   8.6354(2)
_cell_measurement_reflns_used    7625
_cell_measurement_temperature    295
_cell_measurement_theta_max      26.378
_cell_measurement_theta_min      3.229
_cell_volume                     2078.80(10)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 2000)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega 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
_diffrn_reflns_av_sigmaI/netI    0.1152
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4362
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         3.229
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.379
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                2417
_reflns_number_total             4251
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg4005sup1.cif
_cod_data_source_block           I
_cod_database_code               1543166
_cod_database_fobs_code          1543166
_shelx_hkl_checksum              39477
_shelx_res_checksum              18602
_shelxl_version_number           2.014