Intermolecular C-H Insertions and Cyclization Reactions Involving a Stable Germylene
Karla A. Miller; Thomas W. Watson; John E. Bender; Mark M. Banaszak Holl; Jeff W. Kampf; Journal of the American Chemical Society 123 (2001) 982–983; doi:10.1021/ja0026408

data_4115433
_publ_section_title
;
 Intermolecular C-H Insertions and Cyclization Reactions Involving a
 Stable Germylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              982
_journal_page_last               983
_journal_paper_doi               10.1021/ja0026408
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C16 H41 Ge N Si4'
_chemical_formula_weight         432.45
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2877(2)
_cell_length_b                   21.2552(4)
_cell_length_c                   8.2422(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.85
_cell_volume                     2503.06(8)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11019
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            needles
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       colorless
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.553
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.33(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2521
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                2160
_reflns_number_total             2521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0026408.cif
_cod_data_source_block           kma1
_cod_database_code               4115433