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_4127916
_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         'C38 H61 Ge N2 Si'
_chemical_formula_sum            'C38 H61 Ge N2 Si'
_chemical_formula_weight         646.56
_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                104.34(2)
_cell_angle_beta                 93.68(2)
_cell_angle_gamma                108.63(3)
_cell_formula_units_Z            2
_cell_length_a                   9.570(2)
_cell_length_b                   11.955(2)
_cell_length_c                   17.699(3)
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.676
_cell_measurement_theta_min      2.1565
_cell_volume                     1836.3(7)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
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_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
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_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.0712
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62594
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.823
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.274
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0644P)^2^+1.4296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6643
_reflns_number_total             7706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13434_si_002.cif
_cod_data_source_block           1
_cod_database_code               4127916
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              6925
_shelx_hkl_checksum              39939