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_4118573
_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         '(C67 H86 Ge2), 0.5(C5 H12)'
_chemical_formula_sum            'C69.5 H92 Ge2'
_chemical_formula_weight         1072.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.826(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5795(16)
_cell_length_b                   13.4167(10)
_cell_length_c                   22.7242(17)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      71.79
_cell_measurement_theta_min      7.72
_cell_volume                     5902.5(8)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II Duo CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27667
_diffrn_reflns_theta_full        67.75
_diffrn_reflns_theta_max         67.75
_diffrn_reflns_theta_min         7.72
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.7236
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       Block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10462
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0330P)^2^+3.6935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                10390
_reflns_number_total             10462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305853d_si_002.cif
_cod_data_source_block           ots28jcff
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C69.50 H92 Ge2'
_cod_database_code               4118573