Hydroalumination and Hydrogallation of 1,2-Bis(trimethylsilylethynyl)benzene: Formation of Molecular Capsules and C−C Bond Activation
Uhl, Werner; Hepp, Alexander; Westenberg, Hauke; Zemke, Sarina; Würthwein, Ernst-Ulrich; Hellmann, Johannes; Organometallics 29 (2010) 1406–; doi:10.1021/om901058a

data_4067643
_publ_section_title
;
 Hydroalumination and Hydrogallation of
 1,2-Bis(trimethylsilylethynyl)benzene: Formation of Molecular Capsules
 and C&#x2212;C Bond Activation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1406
_journal_paper_doi               10.1021/om901058a
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C80 H110 Al2 F8 N2 Si6'
_chemical_formula_weight         1474.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.474(6)
_cell_length_b                   15.050(3)
_cell_length_c                   19.347(4)
_cell_measurement_reflns_used    20065
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.505
_cell_measurement_theta_min      1.74
_cell_volume                     8489(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20671
_diffrn_reflns_theta_full        29.33
_diffrn_reflns_theta_max         29.33
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9325
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         11518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.2175
_reflns_number_gt                5205
_reflns_number_total             11518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901058a_si_001.cif
_cod_data_source_block           sad2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4067643