Deacetyl tenuazonic acid <i>p</i>-toluenesulfonylhydrazone
Siegel, David; Blaske, Franziska; Koch, Matthias; Emmerling, Franziska; Nehls, Irene; Acta Crystallographica Section E 65 (2009) o3136–; doi:10.1107/S1600536809048958

data_2224442
_publ_section_title
;
 Deacetyl tenuazonic acid <i>p</i>-toluenesulfonylhydrazone
;
_journal_coeditor_code           SJ2674
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3136
_journal_paper_doi               10.1107/S1600536809048958
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C15 H21 N3 O3 S'
_chemical_formula_moiety         'C15 H21 N3 O3 S'
_chemical_formula_sum            'C15 H21 N3 O3 S'
_chemical_formula_weight         323.41
_chemical_name_common
;
deacetyl tenuazonic acid <i>p</i>-toluenesulfonylhydrazone
;
_chemical_name_systematic
;
4-methyl-<i>N</i>'-[(3<i>E</i>)-2-(1-methylpropyl)-5-oxopyrrolidin-3-
ylidene]benzenesulfonohydrazide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.1286(16)
_cell_length_b                   8.285(3)
_cell_length_c                   38.430(12)
_cell_measurement_reflns_used    122
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      4
_cell_volume                     1632.9(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.1343
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            13112
_diffrn_reflns_theta_full        31.10
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
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_refine_diff_density_min         -0.285
_refine_ls_abs_structure_details 'Flack (1983), 1905 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.11(10)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.771
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                2233
_reflns_number_total             4755
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2674.cif
_cod_data_source_block           I
_cod_original_cell_volume        1633.0(9)
_cod_database_code               2224442
_cod_database_fobs_code          2224442