Ge(0) Compound Stabilized by a Diimino-Carbene Ligand: Synthesis and Ambiphilic Reactivity.
Nguyen, Minh Tho; Gusev, Dmitry; Dmitrienko, Anton; Gabidullin, Bulat M.; Spasyuk, Denis; Pilkington, Melanie; Nikonov, Georgii I.; Journal of the American Chemical Society 142 (2020) 5852–5861; doi:10.1021/jacs.0c01283

data_4134380
_publ_section_title
;
 Ge(0) Compound Stabilized by a Diimino-Carbene Ligand: Synthesis and
 Ambiphilic Reactivity.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5852
_journal_page_last               5861
_journal_paper_doi               10.1021/jacs.0c01283
_journal_volume                  142
_journal_year                    2020
_chemical_formula_sum            'C55 H50 Cl12 Ge N4 O4'
_chemical_formula_weight         1328.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                85.175(3)
_cell_angle_beta                 82.476(3)
_cell_angle_gamma                78.104(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0522(6)
_cell_length_b                   12.8275(9)
_cell_length_c                   25.9222(19)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.34
_cell_volume                     2914.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            101054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.665
_diffrn_reflns_theta_min         0.794
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.228
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         14820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0344P)^2^+7.0305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12581
_reflns_number_total             14820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01283_si_007.cif
_cod_data_source_block           TT_0m_a
_cod_depositor_comments
'Adding full bibliography for 4134378--4134383.cif.'
_cod_database_code               4134380
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              8294
_shelx_hkl_checksum              96137