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_7134283
_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
'C90 H112 Br5 Cu8 N3 O16 S8, 2(C3 H7 N O), [+ solvents]1.5[C3H7NO]'
_chemical_formula_sum            'C96 H126 Br5 Cu8 N5 O18 S8'
_chemical_formula_weight         2802.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-09
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-15 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4990(4)
_cell_length_b                   25.0057(5)
_cell_length_c                   43.0467(8)
_cell_measurement_reflns_used    27775
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      72.4000
_cell_measurement_theta_min      3.6530
_cell_volume                     25294.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2792
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -78.00  30.00   1.00   15.00    --  -42.50  89.00-107.00  108
  2  \w    103.00 178.00   1.00   30.00    --  110.76  89.00-107.00   75
  3  \w     31.00 106.00   1.00   30.00    --  110.76 -89.00 137.00   75
  4  \w   -113.00 -16.00   1.00   15.00    --  -42.50 -57.00 150.00   97
  5  \w   -113.00 -16.00   1.00   15.00    --  -42.50 -57.00  60.00   97
  6  \w    -87.00  -6.00   1.00   15.00    --  -42.50 125.00 -30.00   81
  7  \w      6.00  81.00   1.00   15.00    --   42.50 -99.00 -30.00   75
  8  \w     -9.00  78.00   1.00   15.00    --   42.50 -89.00 137.00   87
  9  \w    103.00 178.00   1.00   30.00    --  110.76  77.00-180.00   75
 10  \w     41.00 113.00   1.00   30.00    --  110.76-125.00 150.00   72
 11  \w     87.00 178.00   1.00   30.00    --  110.76  45.00  90.00   91
 12  \w     41.00 113.00   1.00   30.00    --  110.76-125.00  60.00   72
 13  \w     36.00 135.00   1.00   30.00    --  110.76 -30.00  90.00   99
 14  \w     29.00 106.00   1.00   30.00    --  110.76 -94.00-120.00   77
 15  \w     87.00 178.00   1.00   30.00    --  110.76  30.00   0.00   91
 16  \w   -113.00 -16.00   1.00   15.00    --  -42.50 -57.00   0.00   97
 17  \w   -113.00 -16.00   1.00   15.00    --  -42.50 -57.00-150.00   97
 18  \w   -121.00  -6.00   1.00   15.00    --  -42.50 -19.00-120.00  115
 19  \w   -113.00 -54.00   1.00   15.00    --  -42.50 -57.00 120.00   59
 20  \w   -113.00 -16.00   1.00   15.00    --  -42.50 -57.00 -90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0114866000
_diffrn_orient_matrix_UB_12      0.0271947000
_diffrn_orient_matrix_UB_13      -0.0315075000
_diffrn_orient_matrix_UB_21      0.0636681000
_diffrn_orient_matrix_UB_22      -0.0042192000
_diffrn_orient_matrix_UB_23      -0.0081548000
_diffrn_orient_matrix_UB_31      -0.0105480000
_diffrn_orient_matrix_UB_32      -0.0551175000
_diffrn_orient_matrix_UB_33      -0.0149028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            177307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        50.436
_diffrn_reflns_theta_max         50.436
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.984
_exptl_absorpt_correction_T_max  0.44731
_exptl_absorpt_correction_T_min  0.41659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             11328
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DMF and methanol  by slow evaporation'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.038
_refine_diff_density_max         1.834
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         13238
_refine_ls_number_restraints     1390
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0906
_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^)+(0.1233P)^2^+325.5473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2358
_refine_ls_wR_factor_ref         0.2607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9465
_reflns_number_total             13238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00532a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7134282--7134283.cif.'
_cod_database_code               7134283
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cl Cu S'
_chemical_oxdiff_usercomment     '@ 120 K LW-1040'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O16-H16B = O16-H16A
 0.84 with sigma of 0.001
 O12-H12
 0.84 with sigma of 0.02
 C91-O17
 1.22 with sigma of 0.02
 C91-N4
 1.36 with sigma of 0.02
 N4-C93
 1.45 with sigma of 0.02
 N4-C92
 1.46 with sigma of 0.02
 C94-O18
 1.22 with sigma of 0.02
 C94-N5
 1.36 with sigma of 0.02
 N5-C96
 1.45 with sigma of 0.02
 N5-C95
 1.46 with sigma of 0.02
 H16A-H16B
 1.35 with sigma of 0.002
 C91-C93
 2.46 with sigma of 0.04
 C91-C92
 2.45 with sigma of 0.04
 C94-C96
 2.46 with sigma of 0.04
 C94-C95
 2.45 with sigma of 0.04
 C67-C68 \\sim C67-C68A
 with sigma of 0.02
 C67-C69 \\sim C67-C69A
 with sigma of 0.02
 C67-C70 \\sim C67-C70A
 with sigma of 0.02
 N4-C93 \\sim N4-C92
 with sigma of 0.02
 N5-C96 \\sim N5-C95
 with sigma of 0.02
 C79-C77 \\sim C78-C77 \\sim C80-C77
 with sigma of 0.02
3. Restrained planarity
 O17, N4, C91, C92, C93
 with sigma of 0.1
 O18, N5, C94, C95, C96
 with sigma of 0.1
4. Rigid bond restraints
 C67, C68, C69, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C67, C68A, C69A, C70A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C67 \\sim C68 \\sim C69 \\sim C70: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C67 \\sim C68A \\sim C69A \\sim C70A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O17 \\sim N4 \\sim C91 \\sim C92 \\sim C93: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O18 \\sim N5 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C70) = Uanis(C67)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C61, C62, C63, C64, C65, C66, C67, C68, C69, C70}
8. Others
 Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=
 Sof(H69F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(1)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(1)
 Fixed Sof: Br5(0.5) Br6(0.5)
9.a Everything fixed:
 H12
9.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C68A(H68D,H68E,H68F),
 C69A(H69D,H69E,H69F), C70A(H70D,H70E,H70F), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C93(H93A,H93B,H93C), C92(H92A,H92B,H92C), C96(H96A,
 H96B,H96C), C95(H95A,H95B,H95C)
9.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C23(H23), C25(H25), C33(H33), C35(H35),
 C43(H43), C45(H45), C53(H53), C55(H55), C63(H63), C65(H65), C73(H73), C75(H75),
  C82(H82), C85(H85), C88(H88), C91(H91), C94(H94)
9.d Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56054
_shelx_hkl_checksum              58646
_shelx_fab_checksum              75190
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id LW-1040
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.693