All-metal σ-antiaromaticity in dimeric cluster anion {[CuGe<sub>9</sub>Mes]<sub>2</sub>}<sup>4</sup>.
Wang, Zi-Chuan; Tkachenko, Nikolay V.; Qiao, Lei; Matito, Eduard; Muñoz-Castro, Alvaro; Boldyrev, Alexander I.; Sun, Zhong-Ming; Chemical communications (Cambridge, England) 56 (2020) 6583–6586; doi:10.1039/d0cc02525a

data_7126516
_publ_section_title
;
 All-metal \s-antiaromaticity in dimeric cluster anion
 {[CuGe<sub>9</sub>Mes]<sub>2</sub>}<sup>4</sup>.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6583
_journal_page_last               6586
_journal_paper_doi               10.1039/d0cc02525a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C18 H22 Cu2 Ge18, 3(C18 H36 K N2 O6), C18 H35 K N2 O6, 2(C3 H7 N O), C3 H7 N O0.907'
_chemical_formula_sum            'C99 H186 Cu2 Ge18 K4 N11 O27'
_chemical_formula_weight         3551.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_block_doi                 10.5517/ccdc.csd.cc248ww6
_audit_creation_date             2020-03-23
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                100.0676(7)
_cell_angle_beta                 101.7388(7)
_cell_angle_gamma                105.5044(7)
_cell_formula_units_Z            2
_cell_length_a                   15.32218(12)
_cell_length_b                   19.01622(16)
_cell_length_c                   25.9169(2)
_cell_measurement_reflns_used    27909
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      73.3340
_cell_measurement_theta_min      2.7380
_cell_volume                     6911.00(11)
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78365
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.655
_diffrn_reflns_theta_min         2.690
_exptl_absorpt_coefficient_mu    6.224
_exptl_absorpt_correction_T_max  0.4710
_exptl_absorpt_correction_T_min  0.4160
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3564
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         26992
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0469P)^2^+18.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23725
_reflns_number_total             26992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02525a2.cif
_cod_data_source_block           wzc
_cod_depositor_comments          'Adding full bibliography for 7126516.cif.'
_cod_original_cell_volume        6910.99(10)
_cod_database_code               7126516
_shelx_shelxl_version_number     2014/7
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.400
_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. Rigid bond restraints
 Ge3, Ge5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Others
 Sof(C100)=Sof(H100)=1-FVAR(1)
 Sof(C98)=Sof(H98)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C10(H10A,H10B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B), 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), C58(H58A,H58B), C59(H59A,
 H59B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B),
 C81(H81B,H81A), C82(H82A,H82B), C84(H84A,H84B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C90(H90A,H90B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C40(H40), C57(H57), C83(H83), C86(H86), C98(H98), C100(H100)
4.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C46(H46A,H46B,H46C), C60(H60A,H60B,
 H60C), C68(H68A,H68B,H68C), C77(H77A,H77B,H77C), C85(H85A,H85B,H85C), C91(H91A,
 H91B,H91C), C92(H92A,H92B,H92C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C),
 C99(H99A,H99B,H99C)
;
_shelx_res_checksum              89769
_shelx_hkl_checksum              85123
_olex2_submission_special_instructions 'No special instructions were received'