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_1573741
_publ_section_title
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 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
'C2.72 H3.12 Cu0.4 F0.48 N0.16 O0.32 S0.4, 0.08[CH2Cl2]'
_chemical_formula_sum
'C2.8 H3.28 Cl0.16 Cu0.4 F0.48 N0.16 O0.32 S0.4'
_chemical_formula_weight         97.33
_chemical_name_systematic        n/a
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
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2024-11-05 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 102.802(2)
_cell_angle_gamma                90
_cell_formula_units_Z            50
_cell_length_a                   20.5359(10)
_cell_length_b                   15.9060(8)
_cell_length_c                   18.1932(10)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      25.410
_cell_measurement_theta_min      2.296
_cell_volume                     5795.0(5)
_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)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'D8 QUEST'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58049
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.638
_diffrn_reflns_theta_min         2.123
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.8691.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_colour_lustre     Orange
_exptl_crystal_colour_modifier   n/a
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         11971
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0812P)^2^+10.7858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7564
_reflns_number_total             11971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07730j2.cif
_cod_data_source_block           Cu10-dpt
_cod_depositor_comments
'Adding full bibliography for 1573735--1573741.cif.'
_cod_original_formula_sum
'C2.80 H3.28 Cl0.16 Cu0.40 F0.48 N0.16 O0.32 S0.40'
_cod_database_code               1573741
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
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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
 C00Y-F016 \\sim C00Y-F0
 with sigma of 0.02
 F00J-C00Y \\sim F00K-C00Y
 with sigma of 0.02
 F00G-C00Y \\sim F00H-C00Y
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F00J) \\sim Ueq, Uanis(F016) \\sim Ueq, Uanis(F00H) \\sim Ueq,
Uanis(F00G) \\sim Ueq, Uanis(F0) \\sim Ueq, Uanis(F00K) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 F016, F00G, F00J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F0)=1-FVAR(1)
 Sof(F016)=FVAR(1)
 Sof(F00K)=1-FVAR(2)
 Sof(F00J)=FVAR(2)
 Sof(F00H)=1-FVAR(3)
 Sof(F00G)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00O(H00O), C00Q(H00Q), C00T(H00T), C00U(H00U),
 C010(H010), C011(H011), C012(H012), C019(H019), C01F(H01M), C01I(H01T)
6.b Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00V(H00D,H00E,H00F), C00Z(H00G,H00H,H00I), C014(H01A,
 H01B,H01C), C01A(H01D,H01E,H01F), C01B(H01G,H01H,H01I), C01C(H01J,H01K,H01L),
 C01G(H01N,H01O,H01P), C01H(H01Q,H01R,H01S)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 299 electrons were 
found in a volume of 2203\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.08[CH2Cl2] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34986
_shelx_fab_checksum              43263
_olex2_submission_special_instructions 'No special instructions were received'