Tunable structural rearrangement in Cu cluster assemblies through linker and solvent alterations.
Das, Saikat; Sakai, Jin; Nakatani, Riki; Kondo, Ayumu; Tomioka, Rina; Das, Subhabrata; Takahashi, Shuntaro; Kawawaki, Tokuhisa; Biswas, Sourav; Negishi, Yuichi; Chemical science 16 (2025) 2600–2608; doi:10.1039/d4sc07730j

data_1573736
_publ_section_title
;
 Tunable structural rearrangement in Cu cluster assemblies through linker
 and solvent alterations.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2600
_journal_page_last               2608
_journal_paper_doi               10.1039/d4sc07730j
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C82 H84 Cu6 N8 S4, 10.5[C4H9NO]'
_chemical_formula_sum            'C124 H178.5 Cu6 N18.5 O10.5 S4'
_chemical_formula_weight         2605.82
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-05 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.9370(4)
_cell_length_b                   30.9370(4)
_cell_length_c                   30.9370(4)
_cell_measurement_reflns_used    2436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.3270
_cell_measurement_theta_min      3.1820
_cell_volume                     29609.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.107a 64-bit (release 07-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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     46.00 111.00   0.50   24.60    --   54.83  73.00 154.00  130
  2  \w     25.00  60.00   0.50   24.60    --  109.67 -48.00-151.00   70
  3  \w     21.00  51.00   0.50   24.60    --  109.67 -40.00  92.00   60
  4  \w     42.00  68.00   0.50    6.15    --    0.00-125.00 -88.00   52
  5  \w     22.00  48.00   0.50   24.60    --  109.67 -37.00-120.00   52
  6  \w     25.00  60.00   0.50   24.60    --  109.67 -50.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0493938000
_diffrn_orient_matrix_UB_12      -0.0065756000
_diffrn_orient_matrix_UB_13      -0.0001394000
_diffrn_orient_matrix_UB_21      0.0037549000
_diffrn_orient_matrix_UB_22      0.0285687000
_diffrn_orient_matrix_UB_23      -0.0406221000
_diffrn_orient_matrix_UB_31      0.0054070000
_diffrn_orient_matrix_UB_32      0.0402241000
_diffrn_orient_matrix_UB_33      0.0287837000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20402
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        63.818
_diffrn_reflns_theta_max         63.818
_diffrn_reflns_theta_min         4.287
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             10992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.2063
_refine_ls_R_factor_gt           0.1048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.2430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1863
_reflns_number_total             7963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07730j2.cif
_cod_data_source_block           Cu6-tppa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Yellow' was changed
to 'yellow' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1573735--1573741.cif.
;
_cod_original_cell_volume        29609.8(10)
_cod_original_formula_sum        'C124 H178.50 Cu6 N18.50 O10.50 S4'
_cod_database_code               1573736
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHCuSONF
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.764
_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
 S1-C12
 1.9 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C11(H11), C10(H10), C18(H18), C19(H19), C21(H21), C22(H22),
 C5(H5), C6(H6), C2(H2), C3(H3), C28(H28), C27(H27), C25(H25), C24(H24)
5.c Fitted hexagon refined as free rotating group:
 N1(C9,C8,C7,C11,C10), N3(C18,C19,C20,C21,C22), C4(C5,C6,C1,C2,C3), C23(C28,
 C27,C26,C25,C24)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 3968 electrons were 
found in a volume of 17694\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
10.5[C4H9NO] per formula unit 
which account for 4032 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20439
_shelx_fab_checksum              6172
_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 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.858