#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:09:00 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303727 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/88/7718885.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7718885
loop_
_publ_author_name
'Martí-Rujas, Javier'
'Elli, Stefano'
'Famulari, Antonino'
_publ_section_title
;
 In situ X-ray study of breathing-like effect in interlocked
 metal-organic nanocages.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10761
_journal_page_last               10768
_journal_paper_doi               10.1039/d5dt01186h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C174 H144 I24 N24 O6 Zn12'
_chemical_formula_weight         6497.16
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2025-05-19 deposited with the CCDC.	2025-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   38.8170(7)
_cell_length_b                   38.8170(7)
_cell_length_c                   16.0500(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      73.3890
_cell_measurement_theta_min      3.8060
_cell_volume                     20943.5(7)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24715
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.205
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    22.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04300
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless"
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             9108
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.704
_refine_diff_density_min         -2.771
_refine_diff_density_rms         0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         9158
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.1154
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3192
_refine_ls_wR_factor_ref         0.3357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6913
_reflns_number_total             9158
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01186h2.cif
_cod_data_source_block           2_200K
_cod_depositor_comments
'Adding full bibliography for 7718884--7718892.cif.'
_cod_original_cell_volume        20943.5(9)
_cod_database_code               7718885
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.36944(3) 0.29600(3) 0.14795(5) 0.0446(3) Uani 1 1 d . . . . .
I4 I 0.42237(3) 0.49669(3) 0.89048(6) 0.0559(3) Uani 1 1 d . . . . .
I3 I 0.31458(3) 0.43148(3) 0.73284(7) 0.0550(3) Uani 1 1 d . . . . .
I2 I 0.42831(4) 0.36877(5) -0.07879(6) 0.0722(4) Uani 1 1 d . . . . .
Zn1 Zn 0.38879(4) 0.35670(5) 0.05556(9) 0.0321(4) Uani 1 1 d . . . . .
Zn2 Zn 0.37939(5) 0.49484(5) 0.76851(11) 0.0394(4) Uani 1 1 d . . . . .
N1 N 0.4192(3) 0.4067(3) 0.1284(6) 0.0305(19) Uani 1 1 d . . . . .
N2 N 0.6462(3) 0.6708(3) 0.3023(5) 0.0279(18) Uiso 1 1 d . . . . .
N3 N 0.4134(3) 0.5124(3) 0.6630(6) 0.036(2) Uani 1 1 d . . . . .
C19 C 0.4576(3) 0.4729(4) 0.2348(8) 0.036(3) Uani 1 1 d . . . . .
C25 C 0.4543(3) 0.5271(3) 0.5113(8) 0.035(3) Uani 1 1 d . . . . .
C17 C 0.6378(4) 0.6358(4) 0.2690(8) 0.038(3) Uani 1 1 d . . . . .
H17 H 0.657602 0.633952 0.237920 0.046 Uiso 1 1 calc R U . . .
C20 C 0.4636(4) 0.4769(4) 0.1499(8) 0.041(3) Uani 1 1 d . . . . .
H20 H 0.480117 0.502353 0.126012 0.049 Uiso 1 1 calc R U . . .
C11 C 0.4768(3) 0.5059(4) 0.2958(8) 0.037(3) Uani 1 1 d . . . . .
N4 N 0.3654(4) 0.5395(4) 0.7769(8) 0.050(3) Uani 1 1 d . . . . .
C23 C 0.4132(4) 0.4024(4) 0.2116(8) 0.044(3) Uani 1 1 d . . . . .
H23 H 0.395348 0.376748 0.233201 0.053 Uiso 1 1 calc R U . . .
C9 C 0.4754(4) 0.5328(3) 0.4316(7) 0.034(2) Uani 1 1 d . . . . .
C24 C 0.4316(4) 0.4334(4) 0.2658(8) 0.047(3) Uani 1 1 d . . . . .
H24 H 0.427202 0.428926 0.324029 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5145(3) 0.5396(3) 0.2817(7) 0.030(2) Uani 1 1 d . . . . .
H12 H 0.527542 0.542461 0.229937 0.036 Uiso 1 1 calc R U . . .
C8 C 0.5142(3) 0.5650(4) 0.4176(8) 0.039(3) Uani 1 1 d . . . . .
H8 H 0.527533 0.584260 0.460069 0.047 Uiso 1 1 calc R U . . .
C7 C 0.5327(4) 0.5685(3) 0.3423(7) 0.034(2) Uani 1 1 d . . . . .
C21 C 0.4452(4) 0.4431(4) 0.0993(8) 0.046(3) Uani 1 1 d . . . . .
H21 H 0.451251 0.446078 0.041467 0.055 Uiso 1 1 calc R U . . .
C10 C 0.4574(4) 0.5036(4) 0.3712(8) 0.041(3) Uani 1 1 d . . . . .
H10 H 0.431511 0.481672 0.380901 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6186(3) 0.6731(3) 0.3462(8) 0.039(3) Uani 1 1 d . . . . .
H15 H 0.624328 0.698114 0.368578 0.047 Uiso 1 1 calc R U . . .
C13 C 0.5723(3) 0.6041(3) 0.3273(7) 0.032(2) Uani 1 1 d . . . . .
C14 C 0.5817(4) 0.6403(4) 0.3604(8) 0.040(3) Uani 1 1 d . . . . .
H14 H 0.562778 0.642755 0.393366 0.048 Uiso 1 1 calc R U . . .
C18 C 0.6002(4) 0.6018(3) 0.2793(7) 0.033(2) Uani 1 1 d . . . . .
H18 H 0.594221 0.577429 0.253189 0.039 Uiso 1 1 calc R U . . .
C26 C 0.4144(4) 0.5149(4) 0.5122(9) 0.047(3) Uani 1 1 d . . . . .
H26 H 0.400329 0.512440 0.461969 0.057 Uiso 1 1 calc R U . . .
C29 C 0.4537(4) 0.5271(4) 0.6606(8) 0.041(3) Uani 1 1 d . . . . .
H29 H 0.468008 0.532592 0.711525 0.049 Uiso 1 1 calc R U . . .
C30 C 0.4738(4) 0.5341(4) 0.5878(8) 0.039(3) Uani 1 1 d . . . . .
H30 H 0.501679 0.543867 0.588745 0.047 Uiso 1 1 calc R U . . .
C27 C 0.3950(4) 0.5063(4) 0.5897(9) 0.046(3) Uani 1 1 d . . . . .
H27 H 0.366974 0.495415 0.589991 0.055 Uiso 1 1 calc R U . . .
C33 C 0.3897(4) 0.5737(4) 0.8155(12) 0.058(4) Uani 1 1 d . . . . .
H33 H 0.413208 0.576578 0.840473 0.069 Uiso 1 1 calc R U . . .
C32 C 0.3825(4) 0.6051(5) 0.8210(14) 0.067(5) Uani 1 1 d . . . . .
H32 H 0.400132 0.628195 0.851700 0.081 Uiso 1 1 calc R U . . .
C35 C 0.3333(5) 0.5366(5) 0.7386(12) 0.063(4) Uani 1 1 d . . . . .
H35 H 0.315357 0.512360 0.711482 0.075 Uiso 1 1 calc R U . . .
C38 C 0.3411(4) 0.6358(4) 0.7819(10) 0.049(3) Uani 1 1 d . . . . .
C37 C 0.3022(4) 0.6275(4) 0.7831(10) 0.049(3) Uani 1 1 d . . . . .
H37 H 0.280870 0.600814 0.784834 0.058 Uiso 1 1 calc R U . . .
C31 C 0.3496(4) 0.6028(4) 0.7819(11) 0.051(4) Uani 1 1 d . . . . .
C36 C 0.3256(5) 0.5672(5) 0.7373(12) 0.061(4) Uani 1 1 d . . . . .
H36 H 0.303728 0.564542 0.705857 0.074 Uiso 1 1 calc R U . . .
O1 O 0.5039(11) 0.6216(11) 0.846(2) 0.192(12) Uiso 1 1 d D . . . .
H1 H 0.492838 0.606763 0.805155 0.289 Uiso 1 1 calc DR U . . .
C1S C 0.4853(13) 0.6461(12) 0.863(2) 0.155(13) Uiso 1 1 d D . . . .
H1SA H 0.480818 0.655930 0.809788 0.233 Uiso 1 1 calc DR U . . .
H1SB H 0.502863 0.668764 0.898053 0.233 Uiso 1 1 calc R U . . .
H1SC H 0.459758 0.629956 0.891035 0.233 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N2 101.1(4) . 14_455 ?
N1 Zn1 I2 107.4(3) . . ?
N2 Zn1 I2 109.6(2) 14_455 . ?
N1 Zn1 I1 107.8(3) . . ?
N2 Zn1 I1 106.9(3) 14_455 . ?
I2 Zn1 I1 122.13(7) . . ?
N3 Zn2 N4 99.8(5) . . ?
N3 Zn2 I4 108.9(3) . . ?
N4 Zn2 I4 111.7(4) . . ?
N3 Zn2 I3 107.2(3) . . ?
N4 Zn2 I3 106.1(4) . . ?
I4 Zn2 I3 121.00(7) . . ?
C23 N1 C21 117.6(10) . . ?
C23 N1 Zn1 117.6(8) . . ?
C21 N1 Zn1 124.7(8) . . ?
C17 N2 C15 119.0(10) . . ?
C17 N2 Zn1 121.9(8) . 15 ?
C15 N2 Zn1 118.8(8) . 15 ?
C27 N3 C29 116.5(10) . . ?
C27 N3 Zn2 118.3(8) . . ?
C29 N3 Zn2 125.0(9) . . ?
C20 C19 C24 116.8(11) . . ?
C20 C19 C11 124.9(11) . . ?
C24 C19 C11 118.3(11) . . ?
C26 C25 C30 117.9(11) . . ?
C26 C25 C9 120.4(12) . . ?
C30 C25 C9 121.7(11) . . ?
N2 C17 C18 121.4(11) . . ?
C19 C20 C21 119.4(12) . . ?
C10 C11 C12 118.2(11) . . ?
C10 C11 C19 119.4(11) . . ?
C12 C11 C19 122.4(11) . . ?
C33 N4 C35 117.4(13) . . ?
C33 N4 Zn2 120.9(10) . . ?
C35 N4 Zn2 121.5(10) . . ?
N1 C23 C24 122.8(12) . . ?
C10 C9 C8 119.5(11) . . ?
C10 C9 C25 118.0(10) . . ?
C8 C9 C25 122.4(11) . . ?
C23 C24 C19 119.9(12) . . ?
C7 C12 C11 120.8(10) . . ?
C7 C8 C9 119.8(12) . . ?
C8 C7 C12 120.6(11) . . ?
C8 C7 C13 118.6(10) . . ?
C12 C7 C13 120.8(10) . . ?
N1 C21 C20 123.2(12) . . ?
C9 C10 C11 121.0(11) . . ?
N2 C15 C14 121.7(11) . . ?
C14 C13 C18 118.1(10) . . ?
C14 C13 C7 120.9(11) . . ?
C18 C13 C7 121.0(10) . . ?
C13 C14 C15 120.5(11) . . ?
C13 C18 C17 119.2(11) . . ?
C25 C26 C27 117.8(14) . . ?
N3 C29 C30 122.0(12) . . ?
C29 C30 C25 121.1(12) . . ?
N3 C27 C26 124.4(13) . . ?
N4 C33 C32 123.6(14) . . ?
C33 C32 C31 120.1(14) . . ?
N4 C35 C36 122.2(15) . . ?
C37 C38 C37 121.3(13) . 2_665 ?
C37 C38 C31 119.5(12) . . ?
C37 C38 C31 119.1(12) 2_665 . ?
C38 C37 C38 118.6(13) . 3_565 ?
C32 C31 C36 115.1(13) . . ?
C32 C31 C38 123.0(13) . . ?
C36 C31 C38 121.8(13) . . ?
C35 C36 C31 121.5(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Zn1 2.5583(19) . ?
I4 Zn2 2.550(2) . ?
I3 Zn2 2.553(2) . ?
I2 Zn1 2.5502(18) . ?
Zn1 N1 2.057(9) . ?
Zn1 N2 2.054(9) 14_455 ?
Zn2 N3 2.043(9) . ?
Zn2 N4 2.062(13) . ?
N1 C23 1.352(17) . ?
N1 C21 1.346(17) . ?
N2 C17 1.339(16) . ?
N2 C15 1.324(14) . ?
N3 C27 1.333(18) . ?
N3 C29 1.375(15) . ?
C19 C20 1.378(18) . ?
C19 C24 1.439(17) . ?
C19 C11 1.483(17) . ?
C25 C26 1.376(17) . ?
C25 C30 1.396(19) . ?
C25 C9 1.477(16) . ?
C17 C18 1.405(16) . ?
C20 C21 1.396(19) . ?
C11 C10 1.405(18) . ?
C11 C12 1.409(15) . ?
N4 C33 1.34(2) . ?
N4 C35 1.34(2) . ?
C23 C24 1.361(18) . ?
C9 C10 1.386(17) . ?
C9 C8 1.414(15) . ?
C12 C7 1.382(16) . ?
C8 C7 1.377(17) . ?
C7 C13 1.486(15) . ?
C15 C14 1.379(16) . ?
C13 C14 1.369(17) . ?
C13 C18 1.369(17) . ?
C26 C27 1.41(2) . ?
C29 C30 1.355(18) . ?
C33 C32 1.383(19) . ?
C32 C31 1.39(2) . ?
C35 C36 1.36(2) . ?
C38 C37 1.376(18) . ?
C38 C37 1.386(18) 2_665 ?
C38 C31 1.476(17) . ?
C31 C36 1.41(2) . ?
O1 C1S 1.480(18) . ?
