3-Methyl-4-(4-nitrophenyl)-1-phenyl-1,7-dihydro-6<i>H</i>-pyrazolo[3,4-<i>b</i>]thiazolo[5,4-<i>e</i>]pyridine-6-thione‒dimethylformamide (1/1)
Delgado, Paula; Cruz, Silvia; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section E 61 (2005) o3998–o4000; doi:10.1107/S1600536805035270

data_2207593
_publ_section_title
;3-Methyl-4-(4-nitrophenyl)-1-phenyl-1,7-dihydro-6<i>H</i>-pyrazolo[3,4-<i>b</i>]thiazolo[5,4-<i>e</i>]pyridine-6-thione--dimethylformamide
 (1/1)
;
_journal_coeditor_code           LH6537
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3998
_journal_page_last               o4000
_journal_paper_doi               10.1107/S1600536805035270
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C20 H13 N5 O2 S2, C3 H7 N O'
_chemical_formula_moiety         'C20 H13 N5 O2 S2, C3 H7 N O'
_chemical_formula_sum            'C23 H20 N6 O3 S2'
_chemical_formula_weight         492.57
_chemical_name_systematic
;
3-Methyl-4-(4-nitrophenyl)-1-phenyl-1,7-dihydro-6H-
pyrazolo[3,4-b]thiazolo[5,4-e]pyridine-6-
thione--dimethylformamide (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 113.7660(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3023(2)
_cell_length_b                   25.5447(7)
_cell_length_c                   10.3794(2)
_cell_measurement_reflns_used    5163
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.38
_cell_volume                     2257.25(9)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and  PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'OSCAIL and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR91 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0039
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25526
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,  2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.800
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5163
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+2.3558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                4088
_reflns_number_total             5163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6537.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2207593
_cod_database_fobs_code          2207593