Stabilization of a Transient Diorganogermylene by an N-Heterocyclic Carbene
Rupar, Paul A.; Jennings, Michael C.; Ragogna, Paul J.; Baines, Kim M.; Organometallics 26 (2007) 4109–; doi:10.1021/om7006198

data_4073775
_publ_section_title
;
 Stabilization of a Transient Diorganogermylene by an N-Heterocyclic
 Carbene
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4109
_journal_paper_doi               10.1021/om7006198
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '2(C29 H42 Ge N2), C7 H8'
_chemical_formula_sum            'C32.5 H46 Ge N2'
_chemical_formula_weight         537.30
_chemical_melting_point          144
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                63.736(5)
_cell_angle_beta                 80.017(7)
_cell_angle_gamma                81.165(8)
_cell_formula_units_Z            2
_cell_length_a                   8.8091(9)
_cell_length_b                   13.7282(17)
_cell_length_c                   14.061(2)
_cell_measurement_reflns_used    48088
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.70
_cell_volume                     1496.1(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12668
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.66
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.5970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             574
_exptl_crystal_recrystallization_method 'toluene, -30C'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0665P)^2^+2.0055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                4075
_reflns_number_total             4990
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om7006198-file001.cif
_cod_data_source_block           Compound4
_cod_original_formula_sum        'C32.50 H46 Ge N2'
_cod_database_code               4073775