The Role of Group 14 Element Hydrides in the Activation of C-H Bonds in Cyclic Olefins
Owen T. Summerscales; Christine A. Caputo; Caroline E. Knapp; James C. Fettinger; Philip P. Power; Journal of the American Chemical Society 134 (2012) 14595–14603; doi:10.1021/ja305853d

data_4118572
_publ_section_title
;
 The Role of Group 14 Element Hydrides in the Activation of C-H Bonds in
 Cyclic Olefins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14595
_journal_page_last               14603
_journal_paper_doi               10.1021/ja305853d
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'(C65 H84 Ge2)0.94, (C65 H86 Ge2)0.06, (C6 H14)'
_chemical_formula_sum            'C71 H98.12 Ge2'
_chemical_formula_weight         1096.79
_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                 90.478(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.5869(6)
_cell_length_b                   14.9231(4)
_cell_length_c                   39.6876(12)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      70.80
_cell_measurement_theta_min      4.46
_cell_volume                     12784.7(6)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker APEXII DUO CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            18113
_diffrn_reflns_theta_full        68.50
_diffrn_reflns_theta_max         68.50
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.8552
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       Block
_exptl_crystal_F_000             4705
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         10458
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+21.1613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                9593
_reflns_number_total             10458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305853d_si_001.cif
_cod_data_source_block           ots26fmi
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118572