Unusual formation of a N-heterocyclic germylene via homolytic cleavage of a C-C bond
Yan Li; Kartik Chandra Mondal; Peter Stollberg; Hongping Zhu; Herbert W. Roesky; Regine Herbst-Irmer; Dietmar Stalke; Heike Fliegl; Chem.Commun. 50 (2014) 3356–; doi:10.1039/c4cc00251b

data_7112103
_publ_section_title
;
 Unusual formation of a N-heterocyclic germylene via homolytic cleavage of
 a C-C bond
;
_journal_name_full               Chem.Commun.
_journal_page_first              3356
_journal_paper_doi               10.1039/c4cc00251b
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C18 H22 Ge N2'
_chemical_formula_sum            'C18 H22 Ge N2'
_chemical_formula_weight         338.96
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 114.96(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.693(3)
_cell_length_b                   10.903(2)
_cell_length_c                   27.840(3)
_cell_measurement_reflns_used    9372
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.707
_cell_measurement_theta_min      2.254
_cell_volume                     6795(2)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52365
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.827
_diffrn_reflns_theta_min         1.273
_diffrn_source                   'INCOATEC Ag Microsource'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.7816
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7215
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+18.1063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6140
_reflns_number_total             7215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00251b2.cif
_cod_data_source_block           c2c
_cod_original_cell_volume        6795.3(19)
_cod_database_code               7112103
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.914
_shelxl_version_number           2013-4
_shelx_res_checksum              17910
_shelx_hkl_checksum              85042