4,11-Bis(4-chlorophenyl)-3,10-bis(2,6-dichlorophenyl)-1,8-dioxa-2,9-diazadispiro[4.1.4.2]trideca-2,9-dien-6-one‒chloroform‒methanol (1/1/0.75)
Li, Xiao-Fang; Feng, Ya-Qing; Hu Xiao-Fen; Acta Crystallographica Section E 59 (2003) o670–o671; doi:10.1107/S1600536803005543

data_2202227
_publ_section_title
;4,11-Bis(4-chlorophenyl)-3,10-bis(2,6-dichlorophenyl)-1,8-dioxa-2,9-diazadispiro[4.1.4.2]trideca-2,9-dien-6-one--chloroform--methanol
 (1/1/0.75)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o670
_journal_page_last               o671
_journal_paper_doi               10.1107/S1600536803005543
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C33 H20 Cl6 N2 O3, C H Cl3, 0.75C H4 O'
_chemical_formula_moiety         'C33 H20 Cl6 N2 O3, C H Cl3, 0.75C H4 O'
_chemical_formula_sum            'C34.75 H24 Cl9 N2 O3.75'
_chemical_formula_weight         848.61
_chemical_melting_point          .535E-305
_chemical_name_systematic
;
4,11-Bis(4-chlorophenyl)-3,10-bis(2,6-dichlorophenyl)-1,8-dioxa-2,9-
diazadispiro[4.1.4.2]trideca-2,9-dien-6-one chloroform 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'
_cell_angle_alpha                111.815(5)
_cell_angle_beta                 101.814(5)
_cell_angle_gamma                103.510(5)
_cell_formula_units_Z            2
_cell_length_a                   9.896(3)
_cell_length_b                   14.724(4)
_cell_length_c                   15.550(5)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      3.17
_cell_volume                     1935.7(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT and SHELXTL (Bruker, 1998)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10032
_diffrn_reflns_reduction_process 'SAINT (Bruker, 1998)'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             859
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6787
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0560
_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^)+(0.084P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                4617
_reflns_number_total             6787
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww6065.cif
_cod_data_source_block           I
_cod_original_cell_volume        1935.5(10)
_cod_database_code               2202227
_cod_database_fobs_code          2202227