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_1573737
_publ_section_title
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 Tunable structural rearrangement in Cu cluster assemblies through linker
 and solvent alterations.
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_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
'C68 H72 Cu7 F6 N12 O10 S4, C4 H9 N O, 1[CF3COO], 2[C4H9NO]'
_chemical_formula_sum            'C82 H99 Cu7 F9 N15 O15 S4'
_chemical_formula_weight         2278.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-10-02
_audit_creation_method
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Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
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_audit_update_record
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2024-11-05 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.171(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.186(2)
_cell_length_b                   17.9336(10)
_cell_length_c                   43.303(2)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      21.58
_cell_measurement_theta_min      2.32
_cell_volume                     29651(3)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1258
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            163726
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.090
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_min         1.898
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0869 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.8841.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       block
_exptl_crystal_F_000             9312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         26252
_refine_ls_number_restraints     954
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1426P)^2^+8.6547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2368
_refine_ls_wR_factor_ref         0.2649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14537
_reflns_number_total             26252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07730j2.cif
_cod_data_source_block           Cu7-tpbt
_cod_depositor_comments
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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_database_code               1573737
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Restrained distances
 F3-C71 = F5-C71 = F2-C71
 1.35 with sigma of 0.01
 F5-F3 = F3-F2
 2.2 with sigma of 0.02
 F5-F2
 2.2 with sigma of 0.02
2. 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
3. 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
Uanis(O9) = Uanis(O7)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N7(H7), N8(H8), N10(H10), N11(H11), C7(H7A), C8(H8A),
 C10(H10A), C11(H11A), C19(H19), C21(H21), C22(H22), C26(H26), C28(H28),
 C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50),
 C58(H58), C59(H59), C60(H60), C62(H62), C68(H68), C72(H72)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C31(H31A,H31B,
 H31C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C57(H57A,
 H57B,H57C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C),
 C70(H70A,H70B,H70C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C69(H69A,H69B,
 H69C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 1216 electrons were 
found in a volume of 16331\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C4H9NO] per formula unit 
which account for 1152 electrons 
per unit cell.
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_shelx_res_checksum              57740
_shelx_fab_checksum              34183
_olex2_submission_special_instructions 'No special instructions were received'