<i>N</i>'-(3,3,7,7-Tetramethyl-1,5-dioxaspiro[5,5]undecane-8-ylidene)-<i>p</i>-toluenesulfonohydrazide
Zhu, Xiaolei; Zou, Liwei; Xu, Yongting; Han, Jing; Zhang, Chenglu; Acta Crystallographica Section E 63 (2007) o4931–o4931; doi:10.1107/S160053680705893X

data_2216777
_publ_section_title
<i>N</i>'-(3,3,7,7-Tetramethyl-1,5-dioxaspiro[5,5]undecane-8-ylidene)-<i>p</i>-toluenesulfonohydrazide
_journal_coeditor_code           SJ2404
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4931
_journal_page_last               o4931
_journal_paper_doi               10.1107/S160053680705893X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H30 N2 O4 S'
_chemical_formula_moiety         'C20 H30 N2 O4 S'
_chemical_formula_sum            'C20 H30 N2 O4 S'
_chemical_formula_weight         394.52
_chemical_melting_point          416.1(5)
_chemical_name_systematic
;
N'-(3,3,7,7-Tetramethyl-1,5-dioxaspiro[5,5]undecane-8-ylidene)-
p-toluenesulfonohydrazide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                98.397(4)
_cell_angle_beta                 92.789(4)
_cell_angle_gamma                98.676(3)
_cell_formula_units_Z            2
_cell_length_a                   7.437(2)
_cell_length_b                   10.045(3)
_cell_length_c                   14.299(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2.08
_cell_volume                     1041.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       \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  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5883
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.9784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.068P)^2^+0.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                3556
_reflns_number_total             4212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2404.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '415.65-416.55' was changed to
'416.1(5)' - the average value was taken and precision was estimated.

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

The following automatic conversions were performed:

'_chemical_melting_point' value '415.65-416.55' was changed to
'416.1(5)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2216777
_cod_database_fobs_code          2216777