A [CuII24] truncated octahedron and its [CuII8] building block.
Wilson, Lucinda R. B.; Nichol, Gary S.; Dalgarno, Scott J.; Brechin, Euan K.; Chemical communications (Cambridge, England) 61 (2025) 4722–4725; doi:10.1039/d5cc00532a

data_7134282
_publ_section_title
;
 A [CuII24] truncated octahedron and its [CuII8] building block.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4722
_journal_page_last               4725
_journal_paper_doi               10.1039/d5cc00532a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C123 H132 Cl3 Cu12 O24 S12, C123 H129 Cl3 Cu12 O24 S12, 2.25(O), 5(C3 H7 N O), 22[C3H7NO]'
_chemical_formula_sum            'C327 H450 Cl6 Cu24 N27 O77.25 S24'
_chemical_formula_weight         8502.21
_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     dual
_audit_creation_date             2025-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-20 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                75.7320(10)
_cell_angle_beta                 84.1880(10)
_cell_angle_gamma                89.7150(10)
_cell_formula_units_Z            2
_cell_length_a                   22.2855(4)
_cell_length_b                   22.2953(3)
_cell_length_c                   40.7937(7)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.79
_cell_volume                     19538.4(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.631
_diffrn_measured_fraction_theta_max 0.599
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.3696
_diffrn_reflns_Laue_measured_fraction_full 0.631
_diffrn_reflns_Laue_measured_fraction_max 0.599
_diffrn_reflns_number            46213
_diffrn_reflns_point_group_measured_fraction_full 0.631
_diffrn_reflns_point_group_measured_fraction_max 0.599
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.239
_diffrn_reflns_theta_min         1.993
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1034 before and 0.0537 after correction.
 
For component 2:
 wR2(int) was 0.1436 before and 0.0627 after correction.
 The Ratio of minimum to maximum transmission is 0.70.

Final HKLF 4 output contains 517771 reflections, Rint = 0.0600
 (295061 with I > 3sig(I), Rint = 0.0463)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             8802
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3043
_refine_ls_number_reflns         46213
_refine_ls_number_restraints     1015
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.1017
_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^)+(0.1786P)^2^+34.0364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2993
_refine_ls_wR_factor_ref         0.3222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27281
_reflns_number_total             46213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00532a2.cif
_cod_data_source_block           cu_8v00886_0m_4_a
_cod_depositor_comments
'Adding full bibliography for 7134282--7134283.cif.'
_cod_database_code               7134282
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O100-C302
 1.2 with sigma of 0.02
 O104-C314
 1.2 with sigma of 0.02
 N100-C300 = N100-C302 = N100-C301
 1.45 with sigma of 0.02
 N102-C307 = N102-C306 = N102-C308
 1.45 with sigma of 0.02
 C47-C45
 2.54 with sigma of 0.04
 C43-C44
 2.54 with sigma of 0.04
 C46-C47
 2.54 with sigma of 0.04
 C44-C42
 2.54 with sigma of 0.04
 C42-C43
 2.54 with sigma of 0.04
 C45-C46
 2.54 with sigma of 0.04
 C257-C256
 2.54 with sigma of 0.04
 C255-C256
 2.54 with sigma of 0.04
 C257-C255
 2.54 with sigma of 0.04
 C220-C219
 2.54 with sigma of 0.04
 C219-C221
 2.54 with sigma of 0.04
 C220-C221
 2.54 with sigma of 0.04
 C47-C45 \\sim C46-C45
 with sigma of 0.04
 C41-C44 \\sim C41-C42 \\sim C41-C47 \\sim C41-C43 \\sim C41-C46 \\sim C41-C45
\\sim C41-C21
 with sigma of 0.02
 C25-C3 \\sim C25-C26 \\sim C25-C27 \\sim C25-C28
 with sigma of 0.02
 C31-C32 \\sim C31-C30 \\sim C32-C30
 with sigma of 0.04
 C29-C3 \\sim C29-C31 \\sim C29-C32 \\sim C29-C30
 with sigma of 0.02
 C26-C27 \\sim C26-C28 \\sim C27-C28
 with sigma of 0.04
 C119-C117 \\sim C119-C118 \\sim C119-C96 \\sim C117-C118 \\sim C117-C96 \\sim
C118-C96
 with sigma of 0.04
 C116-C119 \\sim C116-C117 \\sim C116-C118 \\sim C116-C96
 with sigma of 0.02
 C108-C127 \\sim C108-C126 \\sim C108-C125 \\sim C127-C126 \\sim C127-C125
\\sim C126-C125
 with sigma of 0.04
 C124-C108 \\sim C124-C127 \\sim C124-C126 \\sim C124-C125
 with sigma of 0.02
 C266-C268 \\sim C266-C270 \\sim C266-C272 \\sim C266-C271 \\sim C266-C269
\\sim C266-C267 \\sim C266-
 C250
 with sigma of 0.02
 C268-C270 \\sim C270-C272 \\sim C271-C269 \\sim C271-C267 \\sim C269-C267
 with sigma of 0.04
 C221-C220 \\sim C221-C219 \\sim C221-C198 \\sim C219-C198
 with sigma of 0.04
 C218-C221 \\sim C218-C220 \\sim C218-C219 \\sim C218-C198
 with sigma of 0.02
 C300-C302 \\sim C302-C301
 with sigma of 0.02
3. Restrained planarity
 O102, N102, C306, C307, C308
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23)
Uanis(C241) = Uanis(C240) = Uanis(C236) = Uanis(C239) = Uanis(C237) =
Uanis(C238)
Uanis(O29) = Uanis(O28) = Uanis(O26) = Uanis(O27) = Uanis(O31) = Uanis(O30) =
Uanis(C130)
Uanis(O19) = Uanis(O18) = Uanis(O14) = Uanis(O15) = Uanis(C128) = Uanis(O17) =
Uanis(O16)
Uanis(O20) = Uanis(O21) = Uanis(O22) = Uanis(O23) = Uanis(C129) = Uanis(O24) =
Uanis(O25)
Uanis(C41) = Uanis(C44) = Uanis(C42) = Uanis(C47) = Uanis(C43) = Uanis(C46) =
Uanis(C45)
Uanis(C40) = Uanis(C37) = Uanis(C38) = Uanis(C39)
Uanis(C77) = Uanis(C78) = Uanis(C76) = Uanis(C79)
Uanis(C48) = Uanis(C50) = Uanis(C52) = Uanis(C49) = Uanis(C51) = Uanis(C53)
Uanis(O67) = Uanis(O66) = Uanis(C273) = Uanis(O64) = Uanis(O65) = Uanis(O63) =
Uanis(O62)
Uanis(O36) = Uanis(O38) = Uanis(O35) = Uanis(O34) = Uanis(O37)
Uanis(C76) = Uanis(C77) = Uanis(C78) = Uanis(C79)
Uanis(O32) = Uanis(O43) = Uanis(C131) = Uanis(O33) = Uanis(O13) = Uanis(O13A)
Uanis(C186) = Uanis(C189) = Uanis(C187) = Uanis(C188)
Uanis(C174) = Uanis(C175) = Uanis(C176) = Uanis(C177)
Uanis(C226) = Uanis(C227) = Uanis(C228) = Uanis(C229)
Uanis(C214) = Uanis(C216) = Uanis(C215) = Uanis(C217)
Uanis(C260) = Uanis(C258) = Uanis(C261) = Uanis(C259)
Uanis(C218) = Uanis(C221) = Uanis(C220) = Uanis(C219)
Uanis(O78) = Uanis(O77) = Uanis(O84) = Uanis(O76) = Uanis(O75) = Uanis(C275) =
Uanis(O74) = Uanis(O73)
Uanis(O71) = Uanis(O72) = Uanis(O85) = Uanis(C274) = Uanis(O68) = Uanis(O70) =
Uanis(O69)
Uanis(O79) = Uanis(C276) = Uanis(O80) = Uanis(O81) = Uanis(O82) = Uanis(O83) =
Uanis(O87)
Uanis(O85) = Uanis(O88) = Uanis(O84) = Uanis(O87) = Uanis(O86)
Uanis(C155) = Uanis(C150) = Uanis(C152) = Uanis(C154) = Uanis(C151) =
Uanis(C153)
Uanis(O57) = Uanis(O54) = Uanis(O55) = Uanis(O56)
Uanis(C12) = Uanis(C7) = Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8)
Uanis(O52) = Uanis(C162) = Uanis(C163) = Uanis(C166) = Uanis(C167) =
Uanis(C165) = Uanis(C164)
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O100, N100, C300, C301, C302
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C66, C67, C68, C69, C70, C71
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C84, C85, C86, C87
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C88, C89, C90, C91, C92, C93
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C112, C113, C114, C115
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C94, C95, C96, C97, C98, C99
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C116, C117, C118, C119
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C124, C125, C126, C127
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O103, N103, C309, C310, C311
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O102, N102, C306, C307, C308
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C120, C121, C122, C123
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C162, C163, C164, C165, C166, C167
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C230, C231, C232, C233, C234, C235
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C190, C191, C192, C193, C194, C195, O38, O100, O101, N100, N101, C300, C301,
 C302, C303, C304, C305, O36, O34, O37, O35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C156, C157, C158, C159, C160, C161
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C182, C183, C184, C185
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C266, C268, C270, C272, C267, C269, C271
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C254, C255, C256, C257
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C262, C263, C264, C265
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C248, C249, C250, C251, C252, C253
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C168, C169, C170, C171, C172, C173
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C196, C197, C198, C199, C200, C201
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O57, C208, C209, C210, C211, C212, C213
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O104, N104, C312, C313, C314
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C29, C30, C31, C32, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C262, C263, C264, C265
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: O63(0.75) O64(0.75) O66(0.75) O70(0.25) O72(0.25) O73(0.25)
 O76(0.25) O78(0.25) O83(0.25) O87(0.25) C268(0.5) H26S(0.5) H26T(0.5)
 H26U(0.5) C270(0.5) H27D(0.5) H27E(0.5) H27F(0.5) C272(0.5) H27G(0.5)
 H27H(0.5) H27I(0.5) C273(0.75) O62(0.25) O67(0.25) O69(0.75) O71(0.75)
 O74(0.75) O75(0.75) O77(0.75) O80(0.75) O82(0.75) C267(0.5) H26V(0.5)
 H26W(0.5) H26X(0.5) C269(0.5) H26Y(0.5) H(0.5) HA(0.5) C271(0.5) H27J(0.5)
 H27K(0.5) H27L(0.5) C274(0.75) C275(0.75) C276(0.75) O38(0.125) O88(0.125)
 O13(0.75) O14(0.25) O17(0.25) O19(0.25) O20(0.25) O23(0.25) O25(0.25)
 O27(0.75) O28(0.75) O30(0.75) O32(0.75) O36(0.25) O81(0.25) O84(0.25)
 O85(0.25) C29(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) C130(0.75) C131(0.75) O13A(0.25) O15(0.75) O16(0.75)
 O18(0.75) O21(0.75) O22(0.75) O24(0.75) O26(0.25) O29(0.25) O31(0.25)
 O34(0.25) O37(0.25) O43(0.25) O65(0.25) O86(0.25) C25(0.5) C26(0.5) H26A(0.5)
 H26B(0.5) H26C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C128(0.75)
 C129(0.75) O35(0.25)
7.a Me refined with riding coordinates:
 C268(H26S,H26T,H26U), C270(H27D,H27E,H27F), C272(H27G,H27H,H27I), C267(H26V,
 H26W,H26X), C269(H26Y,H,HA), C271(H27J,H27K,H27L), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
7.b Aromatic/amide H refined with riding coordinates:
 C151(H151), C153(H153), C157(H157), C159(H159), C163(H163), C165(H165),
 C169(H169), C171(H171), C191(H191), C193(H193), C197(H197), C199(H199),
 C203(H203), C205(H205), C209(H209), C211(H211), C231(H231), C233(H233),
 C237(H237), C239(H239), C243(H243), C245(H245), C249(H249), C251(H251), C2(H2),
  C4(H4), C8(H8), C10(H10), C14(H14), C16(H16), C20(H20), C22(H22), C49(H49),
 C51(H51), C55(H55), C57(H57), C61(H61), C63(H63), C67(H67), C69(H69), C89(H89),
  C91(H91), C95(H95), C97(H97), C101(H101), C103(H103), C107(H107), C109(H109),
 C302(H302), C305(H305), C308(H308), C311(H311), C314(H314)
7.c Idealised Me refined as rotating group:
 C175(H17A,H17B,H17C), C176(H17D,H17E,H17F), C177(H17G,H17H,H17I), C179(H17J,
 H17K,H17L), C180(H18A,H18B,H18C), C181(H18D,H18E,H18F), C183(H18G,H18H,H18I),
 C184(H18J,H18K,H18L), C185(H18M,H18N,H18O), C187(H18P,H18Q,H18R), C188(H18S,
 H18T,H18U), C189(H18V,H18W,H18X), C215(H21A,H21B,H21C), C216(H21D,H21E,H21F),
 C217(H21G,H21H,H21I), C219(H21J,H21K,H21L), C220(H22A,H22B,H22C), C221(H22D,
 H22E,H22F), C223(H22G,H22H,H22I), C224(H22J,H22K,H22L), C225(H22M,H22N,H22O),
 C227(H22P,H22Q,H22R), C228(H22S,H22T,H22U), C229(H22V,H22W,H22X), C256(H25A,
 H25B,H25C), C257(H25D,H25E,H25F), C259(H25G,H25H,H25I), C260(H26D,H26E,H26F),
 C261(H26G,H26H,H26I), C263(H26J,H26K,H26L), C264(H26M,H26N,H26O), C265(H26P,
 H26Q,H26R), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C113(H11A,H11B,H11C), C114(H11D,H11E,H11F), C115(H11G,
 H11H,H11I), C117(H11J,H11K,H11L), C118(H11M,H11N,H11O), C119(H11P,H11Q,H11R),
 C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C125(H12J,
 H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R), C300(H30D,H30E,H30F),
 C301(H30G,H30H,H30I), C303(H30J,H30K,H30L), C304(H30M,H30N,H30O), C306(H30P,
 H30Q,H30R), C307(H30S,H30T,H30U), C309(H30V,H30W,H30X), C310(H31D,H31E,H31F),
 C312(H31G,H31H,H31I), C313(H31J,H31K,H31L), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C77(H77A,H77B,H77C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3314
_shelx_hkl_checksum              50864
_shelx_fab_checksum              67125
_olex2_submission_special_instructions 'No special instructions were received'