Collapse or capture? Guest-induced response of two structurally distinct pillared-MOFs upon exposure to pyridines and quinolines.
Giovanardi, Dario; Cagossi, Giorgio; Zolotarev, Pavel N.; Mazzeo, Paolo P.; Bacchi, Alessia; Carlucci, Lucia; Proserpio, Davide M.; Pelagatti, Paolo; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13540–13548; doi:10.1039/d5dt01321f

data_1575406
_publ_section_title
;
 Collapse or capture? Guest-induced response of two structurally distinct
 pillared-MOFs upon exposure to pyridines and quinolines.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13540
_journal_page_last               13548
_journal_paper_doi               10.1039/d5dt01321f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C93 H58 N7 O19 Zn4, 2(C3 H7 N O)'
_chemical_formula_sum            'C99 H72 N9 O21 Zn4'
_chemical_formula_weight         1985.13
_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     iterative
_audit_creation_date             2025-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                87.768(2)
_cell_angle_beta                 87.468(2)
_cell_angle_gamma                86.876(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1342(9)
_cell_length_b                   13.1346(8)
_cell_length_c                   31.665(2)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.021
_cell_measurement_theta_min      2.269
_cell_volume                     5445.5(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 PhotonII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1175
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            110594
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.933
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1365 before and 0.0905 after correction.
The Ratio of minimum to maximum transmission is 0.7892.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       plate
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.053
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         19068
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0984
_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^)+(0.1352P)^2^+21.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2507
_refine_ls_wR_factor_ref         0.2760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13004
_reflns_number_total             19068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01321f2.cif
_cod_data_source_block           pum210@(quino)1
_cod_depositor_comments
'Adding full bibliography for 1575404--1575407.cif.'
_cod_original_cell_volume        5445.6(6)
_cod_database_code               1575406
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6560(19)
 0.3440(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C59-C59_$1
 1.54 with sigma of 0.02
4. Rigid bond restraints
 C11, C12, C9, C8, C7, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C7 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.008
Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of
0.07 and sigma for terminal atoms of 0.08
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(C83) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C82) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.005
Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C71) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.005
Uanis(C25) = Uanis(C26) = Uanis(O5) = Uanis(O4)
Uanis(C60) = Uanis(C61) = Uanis(C70) = Uanis(C69) = Uanis(C68) = Uanis(C66) =
Uanis(C67)
Uanis(C83) = Uanis(O18) = Uanis(O19)
Uanis(C66) = Uanis(C65) = Uanis(C64)
Uanis(C22) = Uanis(C21) = Uanis(N4)
Uanis(O15) = Uanis(C71) = Uanis(O14)
Uanis(C49) = Uanis(C48) = Uanis(C52)
6. Rigid body (RIGU) restrains
 C84, C85, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Aromatic/amide H refined with riding coordinates:
 C67(H67), C79(H79), C70(H70), C23(H23), C77(H77), C62(H62), C81(H81),
 C69(H69), C65(H65), C64(H64), C74(H74), C82(H82), C24(H24), C76(H76), C22(H22),
  C21(H21), C46(H46), C44(H44), C34(H34), C17(H17), C16(H16), C14(H14),
 C15(H15), C50(H50), C01R(H01R), C84(H84), C42(H42), C39(H39), C32(H32), N3(H3),
  C51(H51), C3(H3A), C4(H4), C2(H2), C1(H1), C27(H27), C86(H86), C30(H30),
 C31(H31), C93(H93), C90(H90), C85(H85), C48(H48), C88(H88), C41(H41), C29(H29),
  C49(H49), N6(H6), C11(H11), C10(H10), C8(H8), C9(H9), C91(H91), C89(H89),
 N2(H2A), C96(H96), C58(H58), C57(H57), C55(H55), C56(H56)
7.b Fitted hexagon refined as free rotating group:
 C17(C16,C13,C14,C15,C18), N1(C3,C4,C5,C2,C1), C12(C11,C10,C7,C8,C9), C59(C58,
 C57,C54,C55,C56)
7.c Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C98(H98A,H98B,H98C), C97(H97A,H97B,
 H97C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11794
_shelx_fab_checksum              90199
_olex2_submission_special_instructions 'No special instructions were received'