5,8,13,13-Tetrachloro-13<i>H</i>-dibenzo[<i>a</i>,<i>i</i>]fluorene cyclohexane hemisolvate
Detert, Heiner; Schollmeyer, Dieter; IUCrData 4 (2019) x190236–; doi:10.1107/S2414314619002360

data_1556953
_publ_section_title
;
 5,8,13,13-Tetrachloro-13<i>H</i>-dibenzo[<i>a</i>,<i>i</i>]fluorene
 cyclohexane hemisolvate
;
_journal_coden_ASTM              IUCRBK
_journal_coeditor_code           BT4083
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x190236
_journal_paper_doi               10.1107/S2414314619002360
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          'C21 H10 Cl4, 0.5C6 H12'
_chemical_formula_moiety         'C21 H10 Cl4, 0.5(C6 H12)'
_chemical_formula_sum            'C24 H16 Cl4'
_chemical_formula_weight         446.17
_chemical_name_systematic
;
5,8,13,13-Tetrachloro-13<i>H</i>-dibenzo[<i>a</i>,<i>i</i>]fluorene
cyclohexane hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 99.901(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7822(6)
_cell_length_b                   10.7752(4)
_cell_length_c                   27.0787(13)
_cell_measurement_reflns_used    17812
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.04
_cell_volume                     3961.5(3)
_computing_cell_refinement
;
X-RED and X-AREA (Stoe & Cie, 1996)
;
_computing_data_collection
;
X-RED and X-AREA (Stoe & Cie, 1996)
;
_computing_data_reduction
;
X-RED and X-AREA (Stoe & Cie, 1996)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11344
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_min         2.038
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.7360
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED and X-AREA; Stoe & Cie, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.505
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4935
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+6.8104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                4194
_reflns_number_total             4935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4083sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding '_space_group_symop_id'.'
_cod_original_sg_symbol_H-M      'I 2/c'
_cod_database_code               1556953
_cod_database_fobs_code          1556953
_shelx_estimated_absorpt_t_min   0.612
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              77891
_shelx_res_checksum              3281