Crystal structure of 1,5-diethyl-3',5'-diphenyl-1,5-dihydro-3'<i>H</i>-spiro[pyrazolo[3,4-<i>d</i>]pyrimidine-4,2'-[1,3,4]thiadiazole]
El Fal, Mohammed; Ramli, Youssef; Essassi, El Mokhtar; Saadi, Mohamed; El Ammari, Lahcen; Acta Crystallographica Section E 71 (2015) o769–o770; doi:10.1107/S2056989015017405

data_2241124
_publ_section_title
;
 Crystal structure of
 1,5-diethyl-3',5'-diphenyl-1,5-dihydro-3'<i>H</i>-spiro[pyrazolo[3,4-<i>d</i>]pyrimidine-4,2'-[1,3,4]thiadiazole]
;
_journal_coeditor_code           TK5387
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o769
_journal_page_last               o770
_journal_paper_doi               10.1107/S2056989015017405
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C22 H22 N6 S'
_chemical_formula_moiety         'C22 H22 N6 S'
_chemical_formula_sum            'C22 H22 N6 S'
_chemical_formula_weight         402.51
_chemical_melting_point          468
_chemical_name_systematic
1,5-Diethyl-3',5'-diphenyl-1,5-dihydro-3'<i>H</i>-spiro[pyrazolo[3,4-<i>d</i>]pyrimidine-4,2'-[1,3,4]thiadiazole]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.501(5)
_cell_length_b                   22.898(5)
_cell_length_c                   12.468(4)
_cell_measurement_reflns_used    4224
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.364
_cell_measurement_theta_min      2.331
_cell_volume                     4140(2)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXL2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\f and \w 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  0.0786
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25025
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.331
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0625P)^2^+0.7320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2566
_reflns_number_total             4224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk5387sup1.cif
_cod_data_source_block           I
_cod_database_code               2241124
_cod_database_fobs_code          2241124
_shelx_hkl_checksum              35094
_shelx_res_checksum              39117
_shelxl_version_number           .2013