Isolation of Transient Acyclic Germanium(I) Radicals Stabilized by Cyclic Alkyl(amino) Carbenes.
Siddiqui, Mujahuddin M.; Sarkar, Samir Kumar; Sinhababu, Soumen; Ruth, Paul Niklas; Herbst-Irmer, Regine; Stalke, Dietmar; Ghosh, Munmun; Fu, Mingxing; Zhao, Lili; Casanova, David; Frenking, Gernot; Schwederski, Brigitte; Kaim, Wolfgang; Roesky, Herbert W.; Journal of the American Chemical Society 141 (2019) 1908–1912; doi:10.1021/jacs.8b13434

data_4127917
_publ_section_title
;
 Isolation of Transient Acyclic Germanium(I) Radicals Stabilized by Cyclic
 Alkyl(amino) Carbenes.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1908
_journal_page_last               1912
_journal_paper_doi               10.1021/jacs.8b13434
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C47 H57 Ge N2 Si'
_chemical_formula_sum            'C47 H57 Ge N2 Si'
_chemical_formula_weight         750.62
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                112.83(2)
_cell_angle_beta                 100.59(2)
_cell_angle_gamma                108.21(3)
_cell_formula_units_Z            2
_cell_length_a                   13.375(2)
_cell_length_b                   13.416(2)
_cell_length_c                   14.015(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      2.198
_cell_volume                     2063.8(10)
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.38A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.580
_diffrn_reflns_theta_min         1.496
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.4254
_exptl_absorpt_correction_T_min  0.3786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.166
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0486P)^2^+3.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6776
_reflns_number_total             8474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13434_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        2063.8(8)
_cod_database_code               4127917
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              89509
_shelx_hkl_checksum              13497