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_7135548
_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
'C47 H111 Cu2 Ge9 Si12, C18 H36 K N2 O6, 0.312[C4H8O1]'
_chemical_formula_sum            'C66.25 H149.5 Cu2 Ge9 K N2 O6.31 Si12'
_chemical_formula_weight         2231.90
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-17
_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                 98.022(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4552(14)
_cell_length_b                   24.525(2)
_cell_length_c                   28.508(2)
_cell_measurement_reflns_used    16162
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.766
_cell_measurement_theta_min      2.036
_cell_volume                     11392.2(16)
_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      150.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            229785
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.766
_diffrn_reflns_theta_max         24.766
_diffrn_reflns_theta_min         2.036
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.366
_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    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             4578
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         19451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0490P)^2^+33.9356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16162
_reflns_number_total             19451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06017f2.cif
_cod_data_source_block           1(3)
_cod_original_cell_volume        11392.2(17)
_cod_original_formula_sum        'C66.25 H149.50 Cu2 Ge9 K N2 O6.31 Si12'
_cod_database_code               7135548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.325
_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.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12856
_shelx_fab_checksum              98339
_olex2_submission_special_instructions 'No special instructions were received'