1-{(2<i>E</i>)-2-[(Aminocarbonothioyl)hydrazono]-2-(3-mesityl-3-methylcyclobutyl)ethyl}pyrrolidine-2,5-dione
Karakurt, Tuncay; Dinçer, Muharrem; Yılmaz, İbrahim; Çukurovalı, Alaaddın; Acta Crystallographica Section E 59 (2003) o1997–o1999; doi:10.1107/S1600536803026096

data_2202761
_publ_section_title
1-{(2<i>E</i>)-2-[(Aminocarbonothioyl)hydrazono]-2-(3-mesityl-3-methylcyclobutyl)ethyl}pyrrolidine-2,5-dione
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1997
_journal_page_last               o1999
_journal_paper_doi               10.1107/S1600536803026096
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C21 H28 N4 O2 S'
_chemical_formula_moiety         'C21 H28 N4 O2 S'
_chemical_formula_sum            'C21 H28 N4 O2 S'
_chemical_formula_weight         400.53
_chemical_name_systematic
;
1-{(2E)-2-[(Aminocarbonothioyl)hydrazono]-2-(3-mesityl-3-
methylcyclobutyl)ethyl}pyrrolidine-2,5-dione
;
_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           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8720(7)
_cell_length_b                   10.8100(11)
_cell_length_c                   21.9284(19)
_cell_measurement_reflns_used    4921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      1.15
_cell_volume                     2103.1(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2001)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 1990)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9857
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.18
_refine_ls_abs_structure_details 'Flack (1983), with x Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_coef       0.0032(11)
_refine_ls_extinction_expression
'Fc^*^ = kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.075
_refine_ls_R_factor_gt           0.043
_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^)+(0.0586P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.101
_refine_ls_wR_factor_ref         0.110
_reflns_number_gt                2270
_reflns_number_total             3703
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6266.cif
_cod_data_source_block           I
_cod_depositor_comments
;
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 
;
_cod_database_code               2202761
_cod_database_fobs_code          2202761