2-[(5-Chloro-2-hydroxybenzylidene)amino]-3',6'-bis(diethylamino)spiro[isoindoline-1,9'-xanthen]-3-one
Xu, Zhi-hong; Guo, Wei-yun; Su, Bo-wei; Shen, Xu-Ke; Yang, Feng-ling; Acta Crystallographica Section E 66 (2010) o1500–; doi:10.1107/S1600536810019549

data_2226083
_publ_section_title
;
 2-[(5-Chloro-2-hydroxybenzylidene)amino]-3',6'-bis(diethylamino)spiro[isoindoline-1,9'-xanthen]-3-one
;
_journal_coeditor_code           CS2127
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1500
_journal_paper_doi               10.1107/S1600536810019549
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C35 H35 Cl N4 O3'
_chemical_formula_moiety         'C35 H35 Cl N4 O3'
_chemical_formula_sum            'C35 H35 Cl N4 O3'
_chemical_formula_weight         595.12
_chemical_name_systematic
;
2-[(5-Chloro-2-hydroxybenzylidene)amino]-3',6'-
bis(diethylamino)spiro[isoindoline-1,9'-xanthen]-3-one
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.609(9)
_cell_length_b                   11.892(5)
_cell_length_c                   12.355(5)
_cell_measurement_reflns_used    1377
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.55
_cell_measurement_theta_min      2.50
_cell_volume                     3175(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16073
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.9548
_exptl_absorpt_correction_T_min  0.9458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details 'Flack (1983), 2521 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_coef       0.0018(2)
_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   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5528
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0200P)^2^+0.0114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                2820
_reflns_number_total             5528
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cs2127.cif
_cod_data_source_block           I
_cod_database_code               2226083
_cod_database_fobs_code          2226083