2,3,4-Trichloro-6-(diethylamino)-9-oxo-9<i>H</i>-xanthene-1-carboxylic acid methanol solvate
Zhang, Hai-Feng; Sun, Bao-Sheng; Zhao, Xin-Hua; Yan, Fan-Yong; Acta Crystallographica Section E 63 (2007) o863–o864; doi:10.1107/S1600536807002437

data_2212219
_publ_section_title
;
 2,3,4-Trichloro-6-(diethylamino)-9-oxo-9<i>H</i>-xanthene-1-carboxylic
 acid methanol solvate
;
_journal_coeditor_code           HG2164
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o863
_journal_page_last               o864
_journal_paper_doi               10.1107/S1600536807002437
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C18 H14 Cl3 N O4 , C H4 O'
_chemical_formula_moiety         'C18 H14 Cl3 N O4 , C H4 O'
_chemical_formula_sum            'C19 H18 Cl3 N O5'
_chemical_formula_weight         446.69
_chemical_melting_point          441
_chemical_name_systematic
;
2,3,4-Trichloro-6-(diethylamino)-9-oxo-9H-xanthene-1-carboxylic acid
methanol solvate
;
_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
_cell_angle_alpha                105.305(5)
_cell_angle_beta                 95.552(9)
_cell_angle_gamma                101.563(6)
_cell_formula_units_Z            2
_cell_length_a                   8.5125(12)
_cell_length_b                   10.0649(14)
_cell_length_c                   12.4028(17)
_cell_measurement_reflns_used    2223
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.7
_cell_volume                     991.5(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXL97
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12536
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9616
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0388P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                1969
_reflns_number_total             4699
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2164.cif
_cod_data_source_block           I
_cod_database_code               2212219
_cod_database_fobs_code          2212219