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_4134382
_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_moiety         'C47 H51 Ge I N4'
_chemical_formula_sum            'C47 H51 Ge I N4'
_chemical_formula_weight         871.41
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                75.451(2)
_cell_angle_beta                 77.193(2)
_cell_angle_gamma                74.606(3)
_cell_formula_units_Z            4
_cell_length_a                   11.1696(6)
_cell_length_b                   18.5499(10)
_cell_length_c                   22.1637(11)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.28
_cell_volume                     4226.0(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            147737
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         0.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_preparation
'heating germylone with PhI in benzene at 40oC for 1 day'
_exptl_crystal_recrystallization_method
'from a mixture of benzene/hexane at room temperature'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         21189
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+16.4554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                17030
_reflns_number_total             21189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0c01283_si_005.cif
_cod_data_source_block           mt29_0m_a
_cod_depositor_comments
'Adding full bibliography for 4134378--4134383.cif.'
_cod_database_code               4134382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 I1, Ge1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C39(H39), C36(H36), C67(H67), C64(H64), C86(H86), C84(H84)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C2(H2), C1(H1), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C34(H34),
 C33(H33), C32(H32), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C62(H62),
  C61(H61), C60(H60), C57(H57), C56(H56), C55(H55), C54(H54), C53(H53),
 C49(H49), C48(H48), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C81(H81), C80(H80), C79(H79)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C21(H21A,H21B,
 H21C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C37(H37A,
 H37B,H37C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C88(H88A,H88B,H88C), C87(H87A,H87B,H87C), C83(H83A,H83B,
 H83C), C85(H85A,H85B,H85C)
;
_olex2_date_sample_completion    2019-11-03
_olex2_date_sample_data_collection 2019-11-01
_olex2_date_sample_submission    2019-11-01
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop with paratone oil '
_olex2_submission_original_sample_id 'MT29_0m_a.res '
_olex2_submission_special_instructions 'No special instructions were received'