3-(2-Amino-5-nitroanilino)-5,5-dimethylcyclohex-2-en-1-one 0.25-hydrate
Mehdi, Sayed Hasan; Hashim, Rokiah; Ghalib, Raza Murad; Goh, Jia Hao; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o2414–o2415; doi:10.1107/S1600536810033933

data_2227322
_publ_section_title
;
 3-(2-Amino-5-nitroanilino)-5,5-dimethylcyclohex-2-en-1-one
 0.25-hydrate
;
_journal_coeditor_code           CI5160
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2414
_journal_page_last               o2415
_journal_paper_doi               10.1107/S1600536810033933
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C14 H17 N3 O3, 0.25H2 O'
_chemical_formula_moiety         'C14 H17 N3 O3, 0.25(H2 O)'
_chemical_formula_sum            'C14 H17.5 N3 O3.25'
_chemical_formula_weight         279.81
_chemical_name_systematic
;
3-(2-Amino-5-nitroanilino)-5,5-dimethylcyclohex-2-en-1-one 0.25-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.4430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   18.90430(10)
_cell_length_b                   16.70480(10)
_cell_length_c                   17.8806(2)
_cell_measurement_reflns_used    6071
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.21
_cell_volume                     5513.93(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector diffractometer
;
_diffrn_measurement_method       '\f and \w scans'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58072
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+2.5234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                5448
_reflns_number_total             8086
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci5160.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C14 H17.50 N3 O3.25'
_cod_database_code               2227322
_cod_database_fobs_code          2227322