By-products from the Preparation of Acetone Tosylhydrazone: 4,5-Dihydro-3,5,5-trimethyl-1-[(4-methylphenyl)sulfonyl]-1<i>H</i>-pyrazole and 1,2-Bis(<i>p</i>-toluenesulfono)hydrazide
Charles R. Ojala; William H. Ojala; William B. Gleason; Acta Crystallographica Section C 54 (1998) 60–63; doi:10.1107/S0108270197011670

data_2006966
_publ_section_title
;
 By-products from the Preparation of Acetone Tosylhydrazone:
 4,5-Dihydro-3,5,5-trimethyl-1-[(4-methylphenyl)sulfonyl]-1<i>H</i>-pyrazole
 and 1,2-Bis(<i>p</i>-toluenesulfono)hydrazide
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              60
_journal_page_last               63
_journal_paper_doi               10.1107/S0108270197011670
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C13 H18 N2 O2 S '
_chemical_formula_sum            'C13 H18 N2 O2 S'
_chemical_formula_weight         266.36
_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'
_audit_creation_method           TEXSAN
_cell_angle_alpha                90
_cell_angle_beta                 98.210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.544(2)
_cell_length_b                   9.3080(10)
_cell_length_c                   16.603(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      49.6
_cell_measurement_theta_min      46.4
_cell_volume                     1306.9(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1985)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      173.2
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3612
_diffrn_reflns_theta_max         70.07
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.13
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             568.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.39
_refine_ls_extinction_coef       0.279E-5
_refine_ls_extinction_method     Zachariasen_(1963)_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.62
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2466
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .052
_refine_ls_shift/esd_max         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4Fo^2^/\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .073
_reflns_number_observed          2466
_reflns_number_total             2626
_reflns_observed_criterion       >0.00
_cod_data_source_file            sx1031.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 36 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 4Fo^2^/\s^2^(Fo^2^)' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
4Fo^2^/\s^2^(Fo^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1306.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C13 H18 N2 O2 S '
_cod_database_code               2006966