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_7112102
_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         '2(C36 H44 Cl2 Ge2 N4), 3(C7 H8)'
_chemical_formula_sum            'C93 H112 Cl4 Ge4 N8'
_chemical_formula_weight         1774.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.61(2)
_cell_angle_beta                 102.61(2)
_cell_angle_gamma                113.07(3)
_cell_formula_units_Z            1
_cell_length_a                   12.692(2)
_cell_length_b                   12.839(2)
_cell_length_c                   15.409(3)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.726
_cell_measurement_theta_min      2.246
_cell_volume                     2175.6(9)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP Version 5.1'
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_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64131
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.835
_diffrn_reflns_theta_min         1.445
_diffrn_source                   'INCOATEC Ag Microsource'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.8618
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9244
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.3017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8098
_reflns_number_total             9244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00251b2.cif
_cod_data_source_block           p-1_a
_cod_original_cell_volume        2175.6(8)
_cod_database_code               7112102
_shelxl_version_number           2013-4
_shelx_res_checksum              10547
_shelx_hkl_checksum              31634