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_7135546
_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         'C37 H96 Cu Ge9 Si12, C18 H36 K N2 O6'
_chemical_formula_sum            'C55 H132 Cu Ge9 K N2 O6 Si12'
_chemical_formula_weight         2010.65
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 90.100(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2014(16)
_cell_length_b                   25.5890(19)
_cell_length_c                   20.2737(17)
_cell_measurement_reflns_used    14967
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.709
_cell_measurement_theta_min      2.009
_cell_volume                     9442.6(13)
_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 0.999
_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  0.1018
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            519655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         2.009
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  0.270
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.070
_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     984
_refine_ls_number_reflns         16067
_refine_ls_number_restraints     586
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0322P)^2^+4.6232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14967
_reflns_number_total             16067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06017f2.cif
_cod_data_source_block           4amended
_cod_database_code               7135546
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5799(5)
 0.4201(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C4-C10 \\sim C4A-C10A
 with sigma of 0.02
 Si9-C29 \\sim Si9A-C29A
 with sigma of 0.04
 C7A-C1A \\sim C7-C1 \\sim C8A-C2A \\sim C8-C2 \\sim C9A-C3A \\sim C9-C3 \\sim
C4A-C10A \\sim C4-C10 \\sim C6A-
 C5A \\sim C6-C5
 with sigma of 0.01
 Si9-C30 \\sim Si9A-C30A
 with sigma of 0.04
 Si4-C18 \\sim Si4A-C18A
 with sigma of 0.02
 Cu1-C10 \\sim Cu1-C10A
 with sigma of 0.04
 C3-C10 \\sim C3A-C10A
 with sigma of 0.04
 Si9-C31 \\sim Si9A-C31A
 with sigma of 0.04
 C5-C10 \\sim C5A-C10A
 with sigma of 0.04
 Si1-C18 \\sim Si1-C18A
 with sigma of 0.04
 Si9-C32 \\sim Si9A-C32A
 with sigma of 0.04
 C17-C18 \\sim C17A-C18A
 with sigma of 0.04
 Si9-C33 \\sim Si9A-C33A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 Si9-C34 \\sim Si9A-C34A
 with sigma of 0.04
 C1-C5 \\sim C1A-C5A
 with sigma of 0.02
 Si9-C35 \\sim Si9A-C35A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.04
 Si9-C36 \\sim Si9A-C36A
 with sigma of 0.04
 Si9-C37 \\sim Si9A-C37A
 with sigma of 0.04
 Si4-C19 \\sim Si4A-C19A \\sim Si4-C18 \\sim Si4A-C18A \\sim Si4-C17 \\sim
Si4A-C17A
 with sigma of 0.01
 Si9A-Si13 \\sim Si9-Si11 \\sim Si9A-Si14 \\sim Si9-Si12 \\sim Si9A-Si \\sim
Si9-Si10
 with sigma of 0.01
 Ge5-Si9A \\sim Ge5-Si9
 with sigma of 0.01
 Ge5-Si10 \\sim Ge5-Si
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 Ge5-Si11 \\sim Ge5-Si13
 with sigma of 0.04
 Ge5-Si12 \\sim Ge5-Si14
 with sigma of 0.04
 C1-C7 \\sim C1A-C7A
 with sigma of 0.02
 Si10-Si11 \\sim Si-Si13
 with sigma of 0.04
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 Si10-Si12 \\sim Si-Si14
 with sigma of 0.04
 Si11-Si12 \\sim Si13-Si14
 with sigma of 0.04
 Cu1-C4 \\sim Cu1-C4A
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.04
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 C2-C8 \\sim C2A-C8A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.04
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 C1-C4 \\sim C1A-C4A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C35-C36 \\sim C35A-C36A
 with sigma of 0.04
 C3-C9 \\sim C3A-C9A
 with sigma of 0.02
 C35-C37 \\sim C35A-C37A
 with sigma of 0.04
 C36-C37 \\sim C36A-C37A
 with sigma of 0.04
 C4-C9 \\sim C4A-C9A
 with sigma of 0.04
 Si11-C33 \\sim Si11-C34 \\sim Si11-C32 \\sim Si14-C35A \\sim Si14-C36A \\sim
Si14-C37A \\sim Si12-C35
 \\sim Si12-C36 \\sim Si12-C37 \\sim Si-C29A \\sim Si-C30A \\sim Si-C31A \\sim
Si10-C29 \\sim Si10-C30 ~
 Si10-C31 \\sim Si13-C32A \\sim Si13-C33A \\sim Si13-C34A
 with sigma of 0.01
 C1-C2 \\sim C3-C4 \\sim C5-C1A \\sim C2A-C3A \\sim C4A-C5A
 with sigma of 0.01
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 Cu1-C1 \\sim Cu1-C1A
 with sigma of 0.04
 Cu1-C2 \\sim Cu1-C2A
 with sigma of 0.04
 Cu1-C3 \\sim Cu1-C3A
 with sigma of 0.04
 Cu1-C5 \\sim Cu1-C5A
 with sigma of 0.04
 Cu1-C6 \\sim Cu1-C6A
 with sigma of 0.04
 Cu1-C7 \\sim Cu1-C7A
 with sigma of 0.04
 Cu1-C8 \\sim Cu1-C8A
 with sigma of 0.04
 Cu1-C9 \\sim Cu1-C9A
 with sigma of 0.04
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C1-C6 \\sim C1A-C6A
 with sigma of 0.04
 C1-C8 \\sim C1A-C8A
 with sigma of 0.04
 C2-C5 \\sim C2A-C5A
 with sigma of 0.04
 C2-C7 \\sim C2A-C7A
 with sigma of 0.04
 C2-C9 \\sim C2A-C9A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C3-C8 \\sim C3A-C8A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 Si1-Si4 \\sim Si1-Si4A
 with sigma of 0.02
 Si4-C17 \\sim Si4A-C17A
 with sigma of 0.02
 Si4-C19 \\sim Si4A-C19A
 with sigma of 0.02
 Si1-C17 \\sim Si1-C17A
 with sigma of 0.04
 Si1-C19 \\sim Si1-C19A
 with sigma of 0.04
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2A \\sim C2 \\sim C3A \\sim C3 \\sim C4 \\sim C4A \\sim C5A \\sim C5
\\sim C1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C1A) \\sim Ueq,
Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq,
Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) = Uanis(O6A)
Uanis(Si9) = Uanis(Si9A)
Uanis(C18) = Uanis(C18A)
Uanis(C35A) = Uanis(C34)
Uanis(C37A) = Uanis(C35)
Uanis(C37) = Uanis(C30A)
Uanis(C29A) = Uanis(C29)
Uanis(C31A) = Uanis(C30)
Uanis(C31) = Uanis(C33A)
Uanis(C33) = Uanis(C34A)
Uanis(C32) = Uanis(C32A)
Uanis(Si4) = Uanis(Si4A)
Uanis(C19A) = Uanis(C19)
Uanis(C17) = Uanis(C17A)
5. Rigid body (RIGU) restrains
 Si13, Si11, Si14, Si12, Si, Si10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C37A, C35, C29A, C37, C30A, C29, C31A, C30, C31, C32A, C33A, C34A, C33,
 C35A, C34, C36A, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(Si9A)=Sof(Si)=Sof(Si13)=Sof(Si14)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=
 Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
 Sof(Si9)=Sof(Si10)=Sof(Si11)=Sof(Si12)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 FVAR(2)
 Sof(O6)=Sof(H53C)=Sof(H53D)=Sof(H54C)=Sof(H54D)=1-FVAR(3)
 Sof(O6A)=Sof(H53A)=Sof(H53B)=Sof(H54A)=Sof(H54B)=FVAR(3)
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(Si4A)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(4)
 Sof(Si4)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53C,H53D), C53(H53A,H53B), C54(H54A,H54B), C54(H54C,
 H54D), C55(H55A,H55B)
7.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C18(H18A,H18B,H18C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C35A(H35D,H35E,
 H35F), C18A(H18D,H18E,H18F)
7.c Idealised Me refined as rotating group:
 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), 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), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F),
 C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F), C36A(H36D,
 H36E,H36F), C37A(H37D,H37E,H37F), C19A(H19D,H19E,H19F), C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              86755
_olex2_submission_special_instructions 'No special instructions were received'