Dehydrogenation of LGeH by a Lewis N-Heterocyclic Carbene Borane Pair under the Formation of L'Ge and its Reactions with B(C6F5)3 and Trimethylsilyl Diazomethane: An Unprecedented Rearrangement of a Diazocompound to an Isonitrile
Anukul Jana; Ina Objartel; Herbert W. Roesky; Dietmar Stalke; Inorganic Chemistry 48 (2009) 7645–7649; doi:10.1021/ic900341r

data_4302910
_publ_contact_author             'Prof. Dr. H. W. Roesky'
_publ_contact_author_email
'hroesky@gwdg.de, dstalke@chemie.uni-goettingen.de'
_publ_section_title
;
Dehydrogenation of LGeH by a Lewis N-Heterocyclic Carbene Borane Pair under
the Formation of L'Ge and its Reactions with B(C6F5)3 and Trimethylsilyl
Diazomethane: An Unprecedented Rearrangement of a Diazocompound to an
Isonitrile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7645
_journal_page_last               7649
_journal_paper_doi               10.1021/ic900341r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C47 H40 B F15 Ge N2'
_chemical_formula_weight         1001.21
_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                109.9890(10)
_cell_angle_beta                 91.1810(10)
_cell_angle_gamma                108.7890(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1690(13)
_cell_length_b                   13.7136(15)
_cell_length_c                   15.0404(16)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.261
_cell_measurement_theta_min      2.466
_cell_volume                     2208.8(4)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL ver. 4.01'
_computing_publication_material  'XSHELL ver. 4.01'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.10'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.10'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker TXS-Mo rotating anode'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43135
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.8473
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0541P)^2^+0.5573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                6298
_reflns_number_total             8111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900341r_si_001_1.cif
_cod_data_source_block           AJ58
_cod_database_code               4302910