<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_1575138
_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         'C51 H51 Cu7 O6, [+ solvents]'
_chemical_formula_sum            'C51 H51 Cu7 O6'
_chemical_formula_weight         1204.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.018(6)
_cell_length_b                   20.018(6)
_cell_length_c                   32.569(10)
_cell_measurement_reflns_used    3228
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      16.30
_cell_measurement_theta_min      2.88
_cell_volume                     13051(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.1458
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28481
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        16.810
_diffrn_reflns_theta_max         16.810
_diffrn_reflns_theta_min         2.359
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.4075
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.5477.
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    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     662
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.1022
_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^)+(0.2500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2904
_refine_ls_wR_factor_ref         0.3318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2321
_reflns_number_total             3615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01663k2.cif
_cod_data_source_block           cu14btb
_cod_depositor_comments
'Adding full bibliography for 1575136--1575140.cif.'
_cod_database_code               1575138
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.805
_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
 O32-C21 = O22-C21
 1.25 with sigma of 0.02
 O5-C3 = O4-C3
 1.25 with sigma of 0.02
 O62-C39 = O40-C39
 1.25 with sigma of 0.02
 C44-C43 = C47-C44 = C46-C44 = C45-C44 = C55-C54 = C54-C51 = C54-C4 = C54-C52 =
  C58-C57 = C61-C58 = C60-C58 = C59-C58
 1.54 with sigma of 0.02
 C6-C25 = C6-C22 = C6-C23 = C6-C24
 1.54 with sigma of 0.02
 O22-C21 = O32-C21
 1.25 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.02
 O30-C39 = O10-C39
 1.25 with sigma of 0.01
 O1-C21 = O21-C21
 1.25 with sigma of 0.01
 O2-C3 = O3-C3
 1.25 with sigma of 0.01
3. Rigid bond restraints
 C1, C10, C2, C7, C8, C9, C11, C12, C13, C14, C15, C16, C17, C34, C33, C20,
 C19, C18, C35, C36, C37, C38, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu7, Cu5, Cu9, Cu8, Cu6, Cu3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39, C21, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, C43, C44, C46, C45, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C57, C59, C58, C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C5, C24, C6, C23, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O62, O40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O40, O62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu23, Cu2, Cu24, Cu4, Cu1, Cu41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, O5, C1, C10, C2, C7, C8, C9, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O22, O32, C17, C34, C33, C20, C19, C18, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O40, O62, C11, C12, C13, C14, C15, C16, C35, C36, C37, C38, C63, C64, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C63, C39, O10, O30, C11, C12, C13, C14, C15, C16, C35, C36, C37, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C34, C33, C20, C19, C18, C21, O1, O21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C10, C2, C7, C8, C9, C3, O3, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50, C51, C52, C54, C55, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C57, C58, C59, C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C5, C6, C22, C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu49, Cu9, Cu6, Cu23, Cu7, Cu24, Cu8, Cu41, Cu3, Cu1, Cu5, Cu4, Cu2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cu7 \\sim Cu5 \\sim Cu9 \\sim Cu8 \\sim Cu6 \\sim Cu3: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(Cu7) \\sim Ueq, Uanis(Cu5) \\sim Ueq, Uanis(Cu9) \\sim Ueq, Uanis(Cu8)
\\sim Ueq, Uanis(Cu6) \\sim Ueq, Uanis(Cu3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C25) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(O40) \\sim Ueq, Uanis(O62) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(Cu23) \\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(Cu24) \\sim Ueq, Uanis(Cu4)
\\sim Ueq, Uanis(Cu1) \\sim Ueq, Uanis(Cu41) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O22) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O40) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cu23(0.88) Cu24(0.88) Cu41(0.88) O4(0.88) O5(0.88) O22(0.88)
 O32(0.88) O40(0.88) O62(0.88) Cu1(0.88) Cu4(0.88) Cu2(0.88) Cu8(0.12)
 Cu9(0.12) Cu3(0.12) Cu7(0.12) Cu5(0.12) Cu6(0.12) O10(0.12) O30(0.12) O1(0.12)
 O21(0.12) O3(0.12) O2(0.12)
6.a Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C52(H52A,H52B,
 H52C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C4(H4A,H4B,H4C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C7(H7), C8(H8), C12(H12), C14(H14), C16(H16), C34(H34),
 C33(H33), C19(H19), C18(H18), C36(H36), C37(H37), C63(H63), C64(H64)
6.c Fitted hexagon refined as free rotating group:
 C1(C10,C2,C7,C8,C9), C11(C12,C13,C14,C15,C16), C17(C34,C33,C20,C19,C18),
 C35(C36,C37,C38,C63,C64)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20479
_shelx_hkl_checksum              94210
_shelx_fab_checksum              28249
_olex2_submission_special_instructions 'No special instructions were received'