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_1573738
_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
'C3.048 H3.714 Cu0.476 F0.571 N0.19 O0.381 S0.286, 0.095(H), 0.162[CHCl3]'
_chemical_formula_sum
'C3.21 H3.97 Cl0.49 Cu0.48 F0.57 N0.19 O0.38 S0.29'
_chemical_formula_weight         118.92
_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             2024-09-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-05 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                82.041(3)
_cell_angle_beta                 82.058(3)
_cell_angle_gamma                75.543(3)
_cell_formula_units_Z            21
_cell_length_a                   13.4577(14)
_cell_length_b                   13.9427(13)
_cell_length_c                   13.9994(14)
_cell_measurement_reflns_used    3372
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      21.59
_cell_measurement_theta_min      2.23
_cell_volume                     2504.4(4)
_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 n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16723
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        22.212
_diffrn_reflns_theta_max         22.212
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    2.545
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5474
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.7350.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6182
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0881P)^2^+14.2246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4250
_reflns_number_total             6182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07730j2.cif
_cod_data_source_block           Cu10-dpb
_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_database_code               1573738
_shelx_shelxl_version_number     2019/2
_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
 Cu03-S07
 2.25 with sigma of 0.005
 C01B-C01J
 1.54 with sigma of 0.01
 C01B-C01H
 1.54 with sigma of 0.005
 C01H-C01B
 1.541 with sigma of 0.0001
 C01F-C01B
 1.541 with sigma of 0.0001
3. Rigid body (RIGU) restrains
 S07, Cu03
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Cu03, S07
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O), C00S(H00S),
 C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C019(H019)
4.b Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,H01H,H01I), C01A(H01J,
 H01K,H01L), C01C(H01M,H01N,H01O), C01E(H01P,H01Q,H01R), C01F(H01S,H01T,H01U),
 C01H(H01V,H01W,H01X), C01J(H01Y,H,HA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35988
_shelx_fab_checksum              73963
_olex2_submission_special_instructions 'No special instructions were received'