5-(4-Chlorophenyl)-1-methyl-3-phenyl-3,6,8,9-tetrahydropyrazolo[3,4-<i>b</i>]thiopyrano[4,3-<i>d</i>]pyridine
Jia, Runhong; Peng, Juhua; Acta Crystallographica Section E 67 (2011) o2421–o2422; doi:10.1107/S1600536811033514

data_2231782
_publ_section_title
;
 5-(4-Chlorophenyl)-1-methyl-3-phenyl-3,6,8,9-tetrahydropyrazolo[3,4-<i>b</i>]thiopyrano[4,3-<i>d</i>]pyridine
;
_journal_coeditor_code           ZQ2115
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2421
_journal_page_last               o2422
_journal_paper_doi               10.1107/S1600536811033514
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C22 H18 Cl N3 S'
_chemical_formula_moiety         'C22 H18 Cl N3 S'
_chemical_formula_sum            'C22 H18 Cl N3 S'
_chemical_formula_weight         391.90
_chemical_melting_point_gt       473
_chemical_melting_point_lt       475
_chemical_name_systematic
;
5-(4-Chlorophenyl)-1-methyl-3-phenyl-3,6,8,9-
tetrahydropyrazolo[3,4-<i>b</i>]thiopyrano[4,3-<i>d</i>]pyridine
;
_space_group_IT_number           14
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.6890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8731(9)
_cell_length_b                   19.9044(18)
_cell_length_c                   10.5292(11)
_cell_measurement_reflns_used    2113
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.697
_cell_measurement_theta_min      2.2
_cell_volume                     1846.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9193
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9427
_exptl_absorpt_correction_T_min  0.8569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       solid
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0492P)^2^+0.3375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                1988
_reflns_number_total             3264
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zq2115.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231782
_cod_database_fobs_code          2231782