C-H Activation of Ethers and Alkanes by Germylene-Aryl Halide Complexes
Karla A. Miller; Jeffrey M. Bartolin; Rory M. O'Neill; Ryan D. Sweeder; Thomas M. Owens; Jeff W. Kampf; Mark M. Banaszak Holl; Norman J. Wells; Journal of the American Chemical Society 125 (2003) 8986–8987; doi:10.1021/ja0357285

data_4113987
_publ_section_title
;
 C-H Activation of Ethers and Alkanes by Germylene-Aryl Halide Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8986
_journal_page_last               8987
_journal_paper_doi               10.1021/ja0357285
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C20 H49 Ge I Si4'
_chemical_formula_weight         601.44
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.381(3)
_cell_angle_beta                 82.483(3)
_cell_angle_gamma                74.544(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2704(19)
_cell_length_b                   11.857(2)
_cell_length_c                   12.554(2)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      3.03
_cell_volume                     1460.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0087
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14707
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0326P)^2^+0.4078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                6783
_reflns_number_total             7088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0357285si20030603_114929.cif
_cod_data_source_block           km264
_cod_original_cell_volume        1460.3(5)
_cod_database_code               4113987