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_4302912
_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            'C33 H50 Ge N4 Si'
_chemical_formula_weight         603.45
_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                107.113(3)
_cell_angle_beta                 94.231(4)
_cell_angle_gamma                109.254(3)
_cell_formula_units_Z            2
_cell_length_a                   10.778(3)
_cell_length_b                   12.040(4)
_cell_length_c                   14.445(4)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.785
_cell_measurement_theta_min      2.2175
_cell_volume                     1660.7(9)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL vers 4.10'
_computing_publication_material  'XSHELL vers 4.10'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24779
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.95008
_exptl_absorpt_correction_T_min  0.76466
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0242P)^2^+0.9117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                5650
_reflns_number_total             6039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900341r_si_001_3.cif
_cod_data_source_block           p-1
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1660.7(8)
_cod_database_code               4302912