A neutral homoaromatic heavy allene as a platform for selective conversion to a germylene-coordinated digermavinylidene.
Uchida, Daichi; Yamada, Hiroko; Mizuhata, Yoshiyuki; Chemical science 16 (2025) 22597–22602; doi:10.1039/d5sc07177a

data_1576068
_publ_section_title
;
 A neutral homoaromatic heavy allene as a platform for selective
 conversion to a germylene-coordinated digermavinylidene.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              22597
_journal_page_last               22602
_journal_paper_doi               10.1039/d5sc07177a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C56 H110 Ge3 N2 Si8, C6 H6'
_chemical_formula_sum            'C62 H116 Ge3 N2 Si8'
_chemical_formula_weight         1332.05
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-04 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.6150(10)
_cell_angle_beta                 97.1890(10)
_cell_angle_gamma                109.0370(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6987(5)
_cell_length_b                   16.2715(6)
_cell_length_c                   19.6919(7)
_cell_measurement_reflns_used    9170
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.390
_cell_measurement_theta_min      2.498
_cell_volume                     3792.6(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            118938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.008
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0774 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.8958.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         17355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0379P)^2^+2.9687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14901
_reflns_number_total             17355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07177a3.cif
_cod_data_source_block           Tbb2Ge3CH2_dmap
_cod_depositor_comments
'Adding full bibliography for 1576066--1576068.cif.'
_cod_database_code               1576068
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C9(H9), C8(H8), C32(H32), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C28(H28), C30(H30), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60)
2.d Fitted hexagon refined as free rotating group:
 C50(C51,C52,C53,C54,C55)
2.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C17(H17A,H17B,
 H17C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C13(H13A,
 H13B,H13C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C19(H19A,H19B,H19C), C15(H15A,H15B,
 H15C), C43(H43A,H43B,H43C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C49(H49A,H49B,
 H49C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              94915
_olex2_submission_special_instructions 'No special instructions were received'