Cleavage of a N-H Bond of Ammonia at Room Temperature by a Germylene
Anukul Jana; Ina Objartel; Herbert W. Roesky; Dietmar Stalke; Inorganic Chemistry 48 (2009) 798–800; doi:10.1021/ic801964u

data_4301346
_publ_contact_author             'Prof. Dr. H. W. Roesky'
_publ_contact_author_email
'hroesky@gwdg.de, dstalke@chemie.uni-goettingen.de'
_publ_section_title
;
Cleavage of a N-H Bond of Ammonia at Room Temperature by a Germylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              798
_journal_page_last               800
_journal_paper_doi               10.1021/ic801964u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C29 H43 Ge N3'
_chemical_formula_weight         506.25
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 95.261(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.902(5)
_cell_length_b                   15.167(3)
_cell_length_c                   14.672(3)
_cell_measurement_reflns_used    7163
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.304
_cell_measurement_theta_min      2.686
_cell_volume                     5518.1(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25829
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0498
_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^)+(0.0638P)^2^+1.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                4141
_reflns_number_total             5069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801964u_si_001.cif
_cod_data_source_block           c2cneu
_cod_original_cell_volume        5518.0(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4301346