Bis(2-carboxy-<i>N</i>-{[1-(2-hydroxyethyl)-3,3-dimethylindolin-2-ylidene]methylimino}anilinium) sulfate monohydrate
Gainsford, Graeme J.; Ashraf, Mohamed; Kay, Andrew J.; Acta Crystallographica Section E 69 (2013) o343–o344; doi:10.1107/S1600536813003188

data_2237574
_publ_section_title
;
 Bis(2-carboxy-<i>N</i>-{[1-(2-hydroxyethyl)-3,3-dimethylindolin-2-ylidene]methylimino}anilinium)
 sulfate monohydrate
;
_journal_coeditor_code           WM2718
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o343
_journal_page_last               o344
_journal_paper_doi               10.1107/S1600536813003188
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2C20 H22 N3 O3 +, S O4 2-, H2 O'
_chemical_formula_moiety         '2(C20 H22 N3 O3 +), (O4 S 2-), H2 O'
_chemical_formula_sum            'C40 H46 N6 O11 S'
_chemical_formula_weight         816.88
_chemical_name_systematic
'Bis(2-carboxy-<i>N</i>-{[1-(2-hydroxyethyl)-3,3-dimethylindolin-2-ylidene]methylimino}anilinium) sulfate monohydrate'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.6810(10)
_cell_angle_beta                 87.688(2)
_cell_angle_gamma                82.627(7)
_cell_formula_units_Z            4
_cell_length_a                   12.2530(9)
_cell_length_b                   14.6114(3)
_cell_length_c                   23.2442(4)
_cell_measurement_reflns_used    11451
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.7
_cell_volume                     3917.9(3)
_computing_cell_refinement
;
<i>FSProcess</i> in PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction
;
<i>FSProcess</i> in PROCESS-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
WinGX (Farrugia, 2012) and <i>Mercury</i> (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.744
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type
;
Rigaku Spider
;
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator
;
Rigaku VariMax-HF Confocal Optical System
;
_diffrn_radiation_source
;
 Rigaku MM007 rotating anode
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24005
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_min         6.701
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.526
_refine_ls_extinction_coef       0.00137(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         10558
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0892P)^2^+0.4584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                9283
_reflns_number_total             10558
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2718.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C40 H46 N6 O11 S1'
_cod_database_code               2237574
_cod_database_fobs_code          2237574