1-Benzoyl-6-methyl-3-methylsulfanyl-6,7-dihydro-1<i>H</i>-pyrano[4,3-<i>c</i>]pyrazol-4-one
Hao, Jing-Jun; Gao, Feng; Wang, You-Ming; Li, Zheng-Ming; Acta Crystallographica Section E 61 (2005) o3470–o3471; doi:10.1107/S1600536805025547

data_2207095
_publ_section_title
1-Benzoyl-6-methyl-3-methylsulfanyl-6,7-dihydro-1<i>H</i>-pyrano[4,3-<i>c</i>]pyrazol-4-one
_journal_coeditor_code           WW6380
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3470
_journal_page_last               o3471
_journal_paper_doi               10.1107/S1600536805025547
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C15 H14 N2 O3 S1'
_chemical_formula_moiety         'C15 H14 N2 O3 S1'
_chemical_formula_sum            'C15 H14 N2 O3 S'
_chemical_formula_weight         302.35
_chemical_melting_point          409
_chemical_name_systematic
;
1-Benzoyl-6-methyl-3-methylsulfanyl-6,7-dihydro-1H-pyrano[4,3-c]pyrazol-4-one
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 117.765(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.083(3)
_cell_length_b                   7.3930(10)
_cell_length_c                   18.820(3)
_cell_measurement_reflns_used    2146
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      2.30
_cell_volume                     2965.0(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7700
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.724761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.154
_refine_ls_abs_structure_details 'Flack (1983), 436 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0203P)^2^+0.9288P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                3298
_reflns_number_total             3972
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww6380.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2965.2(7)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C15 H14 N2 O3 S1'
_cod_database_code               2207095
_cod_database_fobs_code          2207095