Selective crystallization of indigo B by a modified sublimation method and its redetermined structure
Kettner, Florian; Hüter, Lucie; Schäfer, Johanna; Röder, Konstantin; Purgahn, Uta; Krautscheid, Harald; Acta Crystallographica Section E 67 (2011) o2867–; doi:10.1107/S1600536811040220

data_2232260
_publ_section_title
;
 Selective crystallization of indigo B by a modified sublimation method
 and its redetermined structure
;
_journal_coeditor_code           HB6323
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2867
_journal_paper_doi               10.1107/S1600536811040220
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H10 N2 O2'
_chemical_formula_moiety         'C16 H10 N2 O2'
_chemical_formula_sum            'C16 H10 N2 O2'
_chemical_formula_weight         262.26
_chemical_name_common
;
indigo B
;
_chemical_name_systematic
;
2-(3-oxoindolin-2-ylidene)indolin-3-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.781(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.799(2)
_cell_length_b                   5.9064(10)
_cell_length_c                   10.755(3)
_cell_measurement_reflns_used    3816
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.9
_cell_volume                     596.0(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2004)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 1'
_diffrn_measurement_method       '\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  0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4479
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment of long platelet'
_exptl_crystal_F_000             272
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                896
_reflns_number_total             1115
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6323.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2232260
_cod_database_fobs_code          2232260