Silylene- and Germylene-Mediated C−H Activation: Reaction with Alkanes, Ethers, and Amines
Walker, Randon H.; Miller, Karla A.; Scott, Sara L.; Cygan, Zuzanna T.; Bartolin, Jeffrey M.; Kampf, Jeff W.; Banaszak Holl, Mark M.; Organometallics 28 (2009) 2744–; doi:10.1021/om900182z

data_4069408
_publ_section_title
;
 Silylene- and Germylene-Mediated C&#x2212;H Activation: Reaction with
 Alkanes, Ethers, and Amines
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2744
_journal_paper_doi               10.1021/om900182z
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C22 H48 Ge I N Si4'
_chemical_formula_sum            'C22 H48 Ge I N Si4'
_chemical_formula_weight         638.46
_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                102.125(4)
_cell_angle_beta                 93.528(4)
_cell_angle_gamma                109.538(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5644(18)
_cell_length_b                   10.362(2)
_cell_length_c                   16.856(3)
_cell_measurement_reflns_used    4518
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      3.13
_cell_volume                     1523.4(5)
_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      118(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14401
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  0.8445
_exptl_absorpt_correction_T_min  0.3538
_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    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         7426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0380P)^2^+2.3931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                6274
_reflns_number_total             7426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900182z_si_002.cif
_cod_data_source_block           ss119_-_Compound_(16)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069408