Bis(4-formyl-3-methyl-1-phenyl-1<i>H</i>-pyrazol-5-yl) sulfide
Li-Min Yang; Hong-Qing Wang; Zhao-Jie Liu; Hai-Bin Song; Acta Crystallographica Section E 60 (2004) o1898–o1899; doi:10.1107/S1600536804024043

data_2204408
_publ_section_title
;
 Bis(4-formyl-3-methyl-1-phenyl-1<i>H</i>-pyrazol-5-yl) sulfide
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1898
_journal_page_last               o1899
_journal_paper_doi               10.1107/S1600536804024043
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C22 H18 N4 O2 S'
_chemical_formula_moiety         'C22 H18 N4 O2 S'
_chemical_formula_sum            'C22 H18 N4 O2 S'
_chemical_formula_weight         402.46
_chemical_melting_point          468
_chemical_name_systematic
;
Bis(4-formyl-3-methyl-1-phenyl-1H-pyrazol-5-yl) sulfide
;
_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                 99.855(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.853(4)
_cell_length_b                   6.918(2)
_cell_length_c                   20.723(6)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      3.37
_cell_volume                     1956.7(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997--2002)'
_computing_data_reduction        'SAINT (Bruker, 1997--2002)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997--2002)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens 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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10858
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.194
_refine_ls_extinction_coef       0.0124(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.045P)^2^+0.5946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                2913
_reflns_number_total             4015
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6277.cif
_cod_data_source_block           I
_cod_original_cell_volume        1956.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204408
_cod_database_fobs_code          2204408