Cage Hydrocarbons Derived from Dibenzosuberenone
Marcus Pillekamp; Wasim Alachraf; Iris M. Oppel; Gerald Dyker; Journal of Organic Chemistry 74 (2009) 8355–8358; doi:10.1021/jo9018057

data_4024968
_publ_section_title
;
Cage Hydrocarbons Derived from Dibenzosuberenone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8355
_journal_page_last               8358
_journal_paper_doi               10.1021/jo9018057
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C30 H20 Cl2'
_chemical_formula_weight         451.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.193(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.9075(6)
_cell_length_b                   15.3500(10)
_cell_length_c                   31.4301(19)
_cell_measurement_reflns_used    27235
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.58
_cell_volume                     4285.9(5)
_computing_cell_refinement       'CrysAlis RED Oxford diffraction'
_computing_data_collection       'CrysAlis CCD Oxford diffraction'
_computing_data_reduction        'CrysAlis RED Oxford diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford diffraction'
_diffrn_measurement_method       '1505 images at 1.0 deg in \w and 25 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            53074
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.557
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9687
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+5.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                7579
_reflns_number_total             9687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9018057_si_003.cif
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4024968