<i>syn</i>-5,10,15-Tris(dichloromethyl)-5,10,15-trihydroxy-5<i>H</i>-diindeno[1,2-<i>a</i>:1',2'-<i>c</i>]fluorene dichloromethane 0.82-solvate
Morrison, Gregory W.; Fronczek, Frank R.; Watkins, Steven F.; Acta Crystallographica Section E 68 (2012) o1755–o1756; doi:10.1107/S1600536812020703

data_2235117
_publ_section_title
;
 <i>syn</i>-5,10,15-Tris(dichloromethyl)-5,10,15-trihydroxy-5<i>H</i>-diindeno[1,2-<i>a</i>:1',2'-<i>c</i>]fluorene
 dichloromethane 0.82-solvate
;
_journal_coeditor_code           KJ2201
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1755
_journal_page_last               o1756
_journal_paper_doi               10.1107/S1600536812020703
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C30 H18 Cl6 O3, 0.82C H2 Cl2'
_chemical_formula_moiety         'C30 H18 Cl6 O3, 0.82(C H2 Cl2)'
_chemical_formula_sum            'C30.82 H19.64 Cl7.64 O3'
_chemical_formula_weight         708.78
_chemical_name_systematic
;
<i>syn</i>-5,10,15-Tris(dichloromethyl)-5,10,15-trihydroxy-
5<i>H</i>-diindeno[1,2-<i>a</i>:1',2'-<i>c</i>]fluorene dichloromethane
0.82-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
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.009(2)
_cell_angle_beta                 85.291(2)
_cell_angle_gamma                68.798(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9719(4)
_cell_length_b                   11.6186(3)
_cell_length_c                   14.0431(5)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    5548
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.546
_cell_volume                     1576.88(9)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2004)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type
'Nonius KappaCCD diffractometer with an Oxford Cryostream cooler'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            10851
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.8137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             717
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Procedure SQUEEZE, as implemented in PLATON (Spek, 2003), was used
to account for some of the residual electron density found in the solvent
accessible space (330 \%A^3^). In total, 69 electrons were subtracted
from the solvent channel parallel to b and centered at 1/2a, corresponding
to 1.64 dichloromethane molecules per cell or 0.82 per truxene molecule. The
solvent is included in the formula, density, etc., but in not in the model.
;
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       0.0066(17)
_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   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                3608
_reflns_number_total             5744
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kj2201.cif
_cod_data_source_block           I
_cod_database_code               2235117
_cod_database_fobs_code          2235117