1,2,3,4,5,6,7,8,13,13,14,14-Dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-1,4:5,8-dimethanotriphenylene at 90K
Jenkins, Brandon W.; Fronczek, Frank R.; Watkins, Steven F.; Acta Crystallographica Section E 68 (2012) o2538–; doi:10.1107/S1600536812032540

data_2236043
_publ_section_title
;
 1,2,3,4,5,6,7,8,13,13,14,14-Dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-1,4:5,8-dimethanotriphenylene
 at 90K
;
_journal_coeditor_code           ZJ2089
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2538
_journal_paper_doi               10.1107/S1600536812032540
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C20 H8 Cl12'
_chemical_formula_moiety         'C20 H8 Cl12'
_chemical_formula_sum            'C20 H8 Cl12'
_chemical_formula_weight         673.66
_chemical_name_systematic
;
1,2,3,4,5,6,7,8,13,13,14,14-Dodecachloro-1,4,4a,4b,5,8,8a,12b-
octahydro-1,4:5,8-dimethanotriphenylene
;
_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                92.1948(6)
_cell_angle_beta                 98.2331(7)
_cell_angle_gamma                91.3097(6)
_cell_formula_units_Z            4
_cell_length_a                   9.64340(10)
_cell_length_b                   15.4287(2)
_cell_length_c                   16.4161(2)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    27797
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.546
_cell_volume                     2414.53(5)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_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)'
_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 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            111692
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         40.28
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.6069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.633
_refine_ls_extinction_coef       0.0013(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   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     578
_refine_ls_number_reflns         30125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.2577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                24699
_reflns_number_total             30125
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zj2089.cif
_cod_data_source_block           I
_cod_database_code               2236043
_cod_database_fobs_code          2236043