Congested C2-symmetric aryliodanes based on an anti-dimethanoanthracene backbone
Stephen J. Murray; Helge Muller-Bunz; Hasim Ibrahim; Chem.Commun. 48 (2012) 6268–; doi:10.1039/c2cc32280c

data_7107862
_publ_section_title
;
 Congested C2-symmetric aryliodanes based on an anti-dimethanoanthracene
 backbone
;
_journal_name_full               Chem.Commun.
_journal_page_first              6268
_journal_paper_doi               10.1039/c2cc32280c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C22 H22 I, C7 H7 O3 S, 2 (C H Cl3)'
_chemical_formula_sum            'C31 H31 Cl6 I O3 S'
_chemical_formula_weight         823.22
_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           SHELXL-97
_cell_angle_alpha                80.086(2)
_cell_angle_beta                 76.784(2)
_cell_angle_gamma                89.133(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4318(9)
_cell_length_b                   11.7919(9)
_cell_length_c                   13.3530(10)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.13
_cell_volume                     1725.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0318
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13766
_diffrn_reflns_theta_full        24.86
_diffrn_reflns_theta_max         24.86
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.7080
_exptl_absorpt_correction_T_min  0.5529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) for selected reflections was 0.047 before and 0.020 after
correction. The Ratio of minimum to maximum transmission is 0.780998.
The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+2.1430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                5321
_reflns_number_total             5891
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc32280c.txt
_cod_data_source_block           has21
_cod_original_formula_sum        'C31 H31 O3 S Cl6 I'
_cod_database_code               7107862