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_1573739
_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         'C40 H43 Cu6 F3 N4 O2 S8, 2.5[CH2Cl2]'
_chemical_formula_sum            'C42.5 H48 Cl5 Cu6 F3 N4 O2 S8'
_chemical_formula_weight         1518.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-27
_audit_creation_method
;
Olex2 1.5
(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            4
_cell_length_a                   24.6205(9)
_cell_length_b                   17.0084(7)
_cell_length_c                   22.4482(9)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.908
_cell_measurement_theta_min      2.325
_cell_volume                     9400.3(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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48189
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.672
_diffrn_reflns_theta_min         2.326
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0948 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.9275.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.045
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4702
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.003
_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          0.1768
_refine_ls_wR_factor_ref         0.1862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3525
_reflns_number_total             4702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07730j2.cif
_cod_data_source_block           Cu6-dpp
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Orange' was changed
to 'orange' 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_formula_sum        'C42.50 H48 Cl5 Cu6 F3 N4 O2 S8'
_cod_database_code               1573739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.786
_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
 O3-C16
 1.23 with sigma of 0.001
 O3-O3_$1
 2 with sigma of 0.001
 O3-Cu3
 2.05 with sigma of 0.001
 C59-C16
 1.53 with sigma of 0.001
 F2-C32 = F2-C32
 1.4 with sigma of 0.001
 F3-C32 = F2-C32 = F1-C32
 1.4 with sigma of 0.01
 F2-C32 = F3-C32 = F1-C32
 1.4 with sigma of 0.0001
 F2-F3 = F3-F1
 2.3 with sigma of 0.02
 F1-F2
 2.3 with sigma of 0.02
 O1-C15
 1.23 with sigma of 0.0001
 O2-C15
 1.23 with sigma of 0.0001
 C32-C15
 1.53 with sigma of 0.0001
 Cu2-O1
 2.05 with sigma of 0.0001
 O2-O1
 2 with sigma of 0.02
 F6-C59
 1.4 with sigma of 0.01
 O2-C32
 2.5 with sigma of 0.02
 F4-C59 = F5-C59
 1.4 with sigma of 0.001
 C59-F6
 1.4 with sigma of 0.001
 O4-O3
 2 with sigma of 0.02
 O4-C59
 2.4 with sigma of 0.02
 C59-O3
 2.4 with sigma of 0.02
 O4-C16
 1.23 with sigma of 0.001
 F5-F6 = F5-F4
 2.3 with sigma of 0.02
 F6-F4
 2.3 with sigma of 0.02
 C4-C1 = C3-C1 = C2-C1
 1.53 with sigma of 0.01
 C2-C4 = C4-C3
 2.5 with sigma of 0.02
 C2-C3
 2.5 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
Uanis(F5) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H5C(0.5) H5B(0.5) H5A(0.5) F1(0.125) F2(0.125) F3(0.125) F4(0.125)
 F5(0.125) F6(0.125) O1(0.125) O2(0.125) O3(0.125) O4(0.125) C1(0.25) C2(0.25)
 H2A(0.25) H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25)
 H4A(0.25) H4B(0.25) H4C(0.25) C15(0.125) C16(0.125) C32(0.125) C59(0.125)
6.a Me refined with riding coordinates:
 C5(H5C,H5B,H5A)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12)
6.c Fitted hexagon refined as free rotating group:
 N1(C8,C9,C10,C11,C12)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 456 electrons were 
found in a volume of 4224\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.75[CH2Cl2] per formula unit 
which account for 462 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97252
_shelx_fab_checksum              80097
_olex2_submission_special_instructions 'No special instructions were received'