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_1576066
_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         'C49 H100 Ge3 Si8'
_chemical_formula_sum            'C49 H100 Ge3 Si8'
_chemical_formula_weight         1131.77
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 103.920(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.202(3)
_cell_length_b                   9.5466(8)
_cell_length_c                   23.1505(17)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.24
_cell_volume                     6478.9(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0909
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50202
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         2.001
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1761 before and 0.0841 after correction.
The Ratio of minimum to maximum transmission is 0.7153.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       plate
_exptl_crystal_F_000             2408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0644P)^2^+29.9657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5622
_reflns_number_total             7429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07177a3.cif
_cod_data_source_block           Tbb2Ge3CH2
_cod_depositor_comments
'Adding full bibliography for 1576066--1576068.cif.'
_cod_original_cell_volume        6478.8(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1576066
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.785
_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. Uiso/Uaniso restraints and constraints
Uanis(Ge1) = Uanis(Ge3)
3. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) Ge1(0.5) Ge2(0.5) Ge3(0.5)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              89950
_olex2_submission_special_instructions 'No special instructions were received'