Base-mediated alkynyl-cubane to Cu<sub>8</sub>-alkynide cluster transformation.
Gupta, Arvind Kumar; Fayet, Océane Y O; Tian, Lei; Berger, Raphael J. F.; Lomoth, Reiner; Orthaber, Andreas; Chemical communications (Cambridge, England) 61 (2025) 18673–18676; doi:10.1039/d5cc00783f

data_7135098
_publ_section_title
;
 Base-mediated alkynyl-cubane to Cu<sub>8</sub>-alkynide cluster
 transformation.
;
_journal_issue                   94
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              18673
_journal_page_last               18676
_journal_paper_doi               10.1039/d5cc00783f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C44 H88 Cl4 Cu4 Si4'
_chemical_formula_sum            'C44 H88 Cl4 Cu4 Si4'
_chemical_formula_weight         1125.46
_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     direct
_audit_creation_date             2025-10-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-16 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                100.646(7)
_cell_angle_beta                 91.838(6)
_cell_angle_gamma                91.599(6)
_cell_formula_units_Z            2
_cell_length_a                   7.4937(8)
_cell_length_b                   13.8967(18)
_cell_length_c                   27.206(3)
_cell_measurement_reflns_used    6307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.49
_cell_volume                     2781.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31691
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.669
_diffrn_reflns_theta_min         0.762
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         11511
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0595P)^2^+17.0913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8692
_reflns_number_total             11511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00783f2.cif
_cod_data_source_block           ag_ag_01_0m
_cod_depositor_comments
'Adding full bibliography for 7135098--7135099.cif.'
_cod_database_code               7135098
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Restrained distances
 Si2-C41 \\sim Si2-C41A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C41-C43 \\sim C41A-C43A
 with sigma of 0.02
 Si2-C42 \\sim Si2-C42A
 with sigma of 0.04
 Si2-C43 \\sim Si2-C43A
 with sigma of 0.04
 C42-C43 \\sim C42A-C43A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C9A \\sim C10A \\sim C14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C9 \\sim C9A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C14A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41A, C42A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43A)=
 Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C61(H61), C71(H71), C81(H81),
 C91(H91), C101(H101), C111(H111), C121(H121), C41A(H41A), C9(H9), C9A(H9A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C7(H7)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C72(H72A,H72B,H72C),
 C73(H73A,H73B,H73C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C92(H92A,H92B,
 H92C), C93(H93A,H93B,H93C), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F),
 C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C122(H12D,H12E,H12F), C123(H12G,
 H12H,H12I), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F), C14(H14A,H14B,H14C),
 C10(H10G,H10H,H10I), C10A(H10J,H10K,H10L), C14A(H14D,H14E,H14F)
;
_shelx_res_checksum              38627
_shelx_hkl_checksum              64740
_olex2_submission_special_instructions 'No special instructions were received'