<i>Tert</i>-butylacetylene copper cluster-based metal-organic frameworks exhibit hydrophobic properties.
Liu, Zheng; Fang, Jun-Jie; Wang, Zhi-Yi; Xie, Yun-Peng; Lu, Xing; Chemical communications (Cambridge, England) 61 (2025) 12781–12784; doi:10.1039/d5cc01663k

data_1575136
_publ_section_title
;
 <i>Tert</i>-butylacetylene copper cluster-based metal-organic frameworks
 exhibit hydrophobic properties.
;
_journal_issue                   68
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12781
_journal_page_last               12784
_journal_paper_doi               10.1039/d5cc01663k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C114 H114 Cu14 O12'
_chemical_formula_sum            'C114 H114 Cu14 O12'
_chemical_formula_weight         2565.61
_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
_audit_creation_date             2025-06-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                97.877(4)
_cell_angle_beta                 112.526(4)
_cell_angle_gamma                97.863(4)
_cell_formula_units_Z            1
_cell_length_a                   14.194(2)
_cell_length_b                   14.474(2)
_cell_length_c                   14.986(2)
_cell_measurement_reflns_used    2394
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      18.82
_cell_measurement_theta_min      2.90
_cell_volume                     2756.1(7)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0804
_diffrn_reflns_av_unetI/netI     0.2066
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16369
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_min         2.904
_exptl_absorpt_coefficient_mu    2.696
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.6263.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9911
_refine_ls_number_restraints     554
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.0822
_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^)+(0.0725P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3989
_reflns_number_total             9911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01663k2.cif
_cod_data_source_block           cu14nap
_cod_depositor_comments
'Adding full bibliography for 1575136--1575140.cif.'
_cod_database_code               1575136
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.615
_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
 Cu1-Cu27 \\sim Cu1-Cu
 with sigma of 0.02
 Cu27-O41 \\sim Cu-O41
 with sigma of 0.02
 Cu27-C26 \\sim Cu-C26
 with sigma of 0.02
 Cu27-C2 \\sim Cu-C2
 with sigma of 0.02
3. Rigid bond restraints
 Cu1, Cu2, Cu4, Cu27, Cu5, Cu, Cu3, Cu6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu27, Cu6, Cu3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C11, C10, C15, C14, C13, C19, C18, C17, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40, C32, C33, C34, C35, C36, C37, C38, C39, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C49, C11, C8, C64, C26, C16, C26, C51, C56, C70, C56, C13, C54, C39, C54,
 C68, C42, C25, C42, C24, C20, C46, C20, C15, C58, C18, C58, C38, C48, C44, C48,
  C50, C57, C52, C57, C23, C59, C63, C59, C45, C61, C47, C61, C69, C30, C12,
 C30, C10, C43, C14, C43, C19, C60, C17, C60, C37, C22, C38, C22, C39, C65, C44,
  C65, C49, C2, C50, C2, C68, C66, C52, C66, C51, C62, C23, C62, C25, C67, C63,
 C67, C64, C21, C45, C21, C24, C40, C47, C40, C70, C31, C69, C31, C46, C32, C12,
  C32, C11, C33, C10, C33, C15, C34, C14, C34, C13, C35, C19, C35, C18, C36,
 C17, C36, C16, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu27, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cu6 \\sim C20 \\sim Cu27 \\sim C26: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(Cu1) \\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(Cu4) \\sim Ueq, Uanis(Cu27)
\\sim Ueq, Uanis(Cu5) \\sim Ueq, Uanis(Cu) \\sim Ueq, Uanis(Cu3) \\sim Ueq,
Uanis(Cu6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cu27) \\sim Ueq, Uanis(Cu6) \\sim Ueq, Uanis(Cu3) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C40) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C61) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C65) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C66) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C67) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C26) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cu27) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Cu)=1-FVAR(1)
 Sof(Cu27)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C57(H57), C61(H61), C60(H60), C65(H65), C62(H62), C40(H40), C32(H32),
 C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C63(H63), C64(H64), C12(H12),
  C11(H11), C15(H15), C19(H19), C18(H18), C17(H17), C16(H16)
6.b Naphthalene refined as free rotating group:
 C40(C31,C32,C33,C34,C35,C36,C37,C38,C39), C12(C11,C10,C15,C14,C13,C19,C18,C17,
 C16)
6.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C68(H68A,H68B,H68C), C52(H52A,H52B,H52C), C51(H51A,H51B,
 H51C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C24(H24A,
 H24B,H24C), C47(H47A,H47B,H47C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              5064
_shelx_hkl_checksum              49764
_olex2_submission_special_instructions 'No special instructions were received'