Stepwise coordination of {Cu(C<sub>5</sub>Me<sub>5</sub>)} with a tri-silylated Ge<sub>9</sub> cluster.
Chen, Tianzi; Wang, Xinyue; Han, Yulin; Guo, Chenxi; Duan, Dongyu; Tang, Yu; Pan, Fuxing; Chemical communications (Cambridge, England) 62 (2026) 3541–3544; doi:10.1039/d5cc06017f

data_7135547
_publ_section_title
;
 Stepwise coordination of {Cu(C<sub>5</sub>Me<sub>5</sub>)} with a
 tri-silylated Ge<sub>9</sub> cluster.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3541
_journal_page_last               3544
_journal_paper_doi               10.1039/d5cc06017f
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C54 H162 Cu Ge18 Si24, C24 H48 K O6'
_chemical_formula_sum            'C78 H210 Cu Ge18 K O6 Si24'
_chemical_formula_weight         3327.87
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-26
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-12-26 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.6847(4)
_cell_length_b                   23.6847(4)
_cell_length_c                   23.4153(6)
_cell_measurement_reflns_used    4339
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.997
_cell_measurement_theta_min      2.610
_cell_volume                     11375.4(4)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.610
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             5058
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0540P)^2^+35.8964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4339
_reflns_number_total             4974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06017f2.cif
_cod_data_source_block           ctz25111401_1_auto
_cod_original_cell_volume        11375.4(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7135547
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.443
_shelx_estimated_absorpt_t_min   0.305
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 H9C(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 H7C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C9A(H9AA,H9AB,H9AC), C9(H9A,H9B,H9C), C8A(H8AA,H8AB,
 H8AC), C8(H8A,H8B,H8C), C7A(H7AA,H7AB,H7AC), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              40673
_olex2_submission_special_instructions 'No special instructions were received'