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_4134378
_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         '4(C41 H47 Cl Ge N4), 0.5(C8 H20 O2)'
_chemical_formula_sum            'C168 H198 Cl4 Ge4 N16 O'
_chemical_formula_weight         2889.58
_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             2020-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                92.772(6)
_cell_angle_beta                 97.630(3)
_cell_angle_gamma                96.140(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8382(7)
_cell_length_b                   15.3641(16)
_cell_length_c                   28.9948(19)
_cell_measurement_reflns_used    9321
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.44
_cell_volume                     3872.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'Bruker XT'
_diffrn_ambient_temperature      152.1
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24627
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         0.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         24634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0838
_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^)+(0.0667P)^2^+16.8595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                20729
_reflns_number_total             24634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0c01283_si_004.cif
_cod_data_source_block           twin5
_cod_depositor_comments
'Adding full bibliography for 4134378--4134383.cif.'
_cod_database_code               4134378
_exptl_absorpt_special_details
;
twinabs 2012/1 bruer AXS Madison WI, USA
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5635(8)
 0.4365(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C85, C85A}
4. Uiso/Uaniso restraints and constraints
Uanis(C85) = Uanis(C85A)
Uanis(C58) = Uanis(C61)
Uanis(C60) = Uanis(C59) = Uanis(C63) = Uanis(C62)
5. Others
 Fixed Sof: C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5)
 C85A(0.5) H85A(0.5) H85B(0.5) H85C(0.5) C85(0.5) H85D(0.5) H85E(0.5) H85F(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C17(H17), C20(H20), C36(H36), C39(H39), C44(H44), C58(H58), C61(H61),
 C77(H77), C80(H80)
6.b Secondary CH2 refined with riding coordinates:
 C83(H83A,H83B), C84(H84A,H84B)
6.c Me refined with everything fixed:
 C85A(H85A,H85B,H85C), C85(H85D,H85E,H85F)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
  C34(H34), C42(H42), C43(H43), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C54(H54), C55(H55), C56(H56), C66(H66), C67(H67), C68(H68), C69(H69),
  C70(H70), C73(H73), C74(H74), C75(H75)
6.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C)
;
_olex2_submission_special_instructions 'No special instructions were received'