#------------------------------------------------------------------------------
#$Date: 2025-10-06 09:40:48 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302502 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/51/1575195.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_1575195
loop_
_publ_author_name
'Xiao, Zongjing'
'Li, Pengfei'
'Sun, Beibei'
'Bao, Xinrui'
'Gan, Lei'
'Yang, Huajun'
_publ_section_title
;
 Water-mediated synthesis of hydrogen-bonded metal-organic frameworks.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              14919
_journal_page_last               14923
_journal_paper_doi               10.1039/d5sc02337h
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C72 H100 Cu4 I0 N4 O24'
_chemical_formula_weight         1659.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-03-25 deposited with the CCDC.	2025-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.610(3)
_cell_length_b                   10.687(4)
_cell_length_c                   20.153(7)
_cell_measurement_reflns_used    8676
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.16
_cell_volume                     2069.8(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13114
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.003
_diffrn_reflns_theta_min         2.021
_exptl_absorpt_coefficient_mu    1.086
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       rod
_exptl_crystal_F_000             868
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1265
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0211
_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/[σ²(Fo²)+(0.0444P)²+1.1917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1208
_reflns_number_total             1265
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc02337h2.cif
_cod_data_source_block           aa_a
_cod_depositor_comments
'Adding full bibliography for 1575195--1575196.cif.'
_cod_database_code               1575195
_shelx_shelxl_version_number     2014/7
_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'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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
Cu1 Cu 0.63711(3) 0.5000 0.5000 0.01703(11) Uani 1 4 d S TU P C .
O2 O 0.61509(14) 0.31831(13) 0.5000 0.0446(4) Uani 1 2 d S TU P . .
O3 O 0.61509(15) 0.5000 0.40293(7) 0.0464(4) Uani 1 2 d S TU P . .
O005 O 0.5000 0.39706(17) 0.06516(8) 0.0688(6) Uani 1 2 d S TU P . .
H005 H 0.5000 0.4090 0.0250 0.103 Uiso 0.5 2 calc R U P . .
C6 C 0.5000 0.2647(2) 0.5000 0.0250(5) Uani 1 4 d S TU P B .
C22 C 0.5000 0.1219(2) 0.5000 0.0260(5) Uani 1 4 d S TU P . .
C11 C 0.5000 0.5000 0.37459(12) 0.0285(5) Uani 1 4 d S TU P A .
C12 C 0.5000 0.5000 0.29892(13) 0.0327(6) Uani 1 4 d S TU P . .
C11A C 0.4594(8) 0.6262(8) 0.2743(4) 0.045(2) Uani 0.25 1 d . U P A -1
H11A H 0.5248 0.6878 0.2910 0.054 Uiso 0.25 1 calc R U P A -1
H11B H 0.3679 0.6472 0.2913 0.054 Uiso 0.25 1 calc R U P A -1
C11B C 0.6435(8) 0.4622(8) 0.2702(4) 0.044(2) Uani 0.25 1 d . U P A -1
H11C H 0.7142 0.5200 0.2857 0.053 Uiso 0.25 1 calc R U P A -1
H11D H 0.6680 0.3790 0.2855 0.053 Uiso 0.25 1 calc R U P A -1
C11C C 0.3922(9) 0.4006(9) 0.2723(4) 0.0391(19) Uani 0.25 1 d . U P A -1
H11E H 0.4196 0.3175 0.2865 0.047 Uiso 0.25 1 calc R U P A -1
H11F H 0.3007 0.4182 0.2904 0.047 Uiso 0.25 1 calc R U P A -1
C12A C 0.3867(10) 0.4056(9) 0.1963(4) 0.042(2) Uani 0.25 1 d . U P A -1
H12A H 0.2950 0.4325 0.1820 0.051 Uiso 0.25 1 calc R U P A -1
H12B H 0.4038 0.3230 0.1782 0.051 Uiso 0.25 1 calc R U P A -1
C12B C 0.6379(10) 0.4642(8) 0.1939(5) 0.044(2) Uani 0.25 1 d . U P A -1
H12C H 0.7065 0.5229 0.1773 0.053 Uiso 0.25 1 calc R U P A -1
H12D H 0.6613 0.3818 0.1771 0.053 Uiso 0.25 1 calc R U P A -1
C12C C 0.4569(9) 0.6316(7) 0.1979(4) 0.048(2) Uani 0.25 1 d . U P A -1
H12E H 0.5212 0.6951 0.1823 0.058 Uiso 0.25 1 calc R U P A -1
H12F H 0.3643 0.6533 0.1826 0.058 Uiso 0.25 1 calc R U P A -1
C13A C 0.4618(9) 0.0714(12) 0.5653(7) 0.037(4) Uani 0.25 1 d . U P B -1
H13B H 0.5274 0.1003 0.5978 0.056 Uiso 0.25 1 d R U P B -1
H13C H 0.3703 0.1003 0.5768 0.056 Uiso 0.25 1 d R U P B -1
C13B C 0.4016(13) 0.0725(9) 0.4456(6) 0.038(3) Uani 0.25 1 d . U P B -1
H13E H 0.3095 0.1021 0.4552 0.057 Uiso 0.25 1 d R U P B -1
H13F H 0.4296 0.1021 0.4026 0.057 Uiso 0.25 1 d R U P B -1
C13C C 0.6491(7) 0.0718(7) 0.4814(5) 0.042(3) Uani 0.25 1 d . U P B -1
H13H H 0.6746 0.1012 0.4381 0.064 Uiso 0.25 1 d R U P B -1
H13I H 0.7154 0.1012 0.5134 0.064 Uiso 0.25 1 d R U P B -1
C17 C 0.5000 0.5000 0.16969(13) 0.0395(7) Uani 1 4 d S TU P . .
C18 C 0.5000 0.5000 0.09467(14) 0.0411(7) Uani 1 4 d S TU P A .
N1 N 0.86598(19) 0.5000 0.5000 0.0216(4) Uani 1 4 d DS TU P . .
C24 C 0.9189(10) 0.6243(6) 0.4836(4) 0.041(4) Uani 0.25 1 d D U P C -1
H24A H 0.8851 0.6848 0.5156 0.049 Uiso 0.25 1 d R U P C -1
H24B H 0.8851 0.6486 0.4401 0.049 Uiso 0.25 1 d R U P C -1
C25 C 0.9213(11) 0.4602(8) 0.5652(3) 0.037(3) Uani 0.25 1 d D U P C -1
H25A H 0.8874 0.3775 0.5766 0.044 Uiso 0.25 1 d R U P C -1
H25B H 0.8874 0.5188 0.5982 0.044 Uiso 0.25 1 d R U P C -1
C23 C 0.9195(9) 0.4076(6) 0.4517(4) 0.035(3) Uani 0.25 1 d D U P C -1
H23A H 0.8854 0.4301 0.4080 0.043 Uiso 0.25 1 d R U P C -1
H23B H 0.8854 0.3246 0.4624 0.043 Uiso 0.25 1 d R U P C -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
O2 Cu1 O2 167.56(8) . 11_565 ?
O2 Cu1 O3 89.333(7) . . ?
O2 Cu1 O3 89.333(7) 11_565 . ?
O2 Cu1 O3 89.333(7) . 10_556 ?
O2 Cu1 O3 89.333(7) 11_565 10_556 ?
O3 Cu1 O3 167.66(9) . 10_556 ?
O2 Cu1 N1 96.22(4) . . ?
O2 Cu1 N1 96.22(4) 11_565 . ?
O3 Cu1 N1 96.17(4) . . ?
O3 Cu1 N1 96.17(4) 10_556 . ?
O2 Cu1 Cu1 83.78(4) . 9_666 ?
O2 Cu1 Cu1 83.78(4) 11_565 9_666 ?
O3 Cu1 Cu1 83.83(4) . 9_666 ?
O3 Cu1 Cu1 83.83(4) 10_556 9_666 ?
N1 Cu1 Cu1 180.0 . 9_666 ?
C6 O2 Cu1 123.59(13) . . ?
C11 O3 Cu1 123.48(14) . . ?
C18 O005 H005 109.5 . . ?
O2 C6 O2 125.2(2) 3_656 . ?
O2 C6 C22 117.38(11) 3_656 . ?
O2 C6 C22 117.38(11) . . ?
C13A C22 C6 111.6(5) . . ?
C13A C22 C13B 111.0(6) . . ?
C6 C22 C13B 110.0(4) . . ?
C13A C22 C13C 108.4(4) . . ?
C6 C22 C13C 109.9(3) . . ?
C13B C22 C13C 105.8(6) . . ?
O3 C11 O3 125.4(2) . 2_665 ?
O3 C11 C12 117.31(12) . . ?
O3 C11 C12 117.31(12) 2_665 . ?
C11A C12 C11 109.4(3) . . ?
C11A C12 C11B 110.2(4) . . ?
C11 C12 C11B 111.9(3) . . ?
C11A C12 C11C 108.9(5) . . ?
C11 C12 C11C 109.9(3) . . ?
C11B C12 C11C 106.4(5) . . ?
C12 C11A C12C 111.7(6) . . ?
C12 C11A H11A 109.3 . . ?
C12C C11A H11A 109.3 . . ?
C12 C11A H11B 109.3 . . ?
C12C C11A H11B 109.3 . . ?
H11A C11A H11B 107.9 . . ?
C12B C11B C12 109.8(6) . . ?
C12B C11B H11C 109.7 . . ?
C12 C11B H11C 109.7 . . ?
C12B C11B H11D 109.7 . . ?
C12 C11B H11D 109.7 . . ?
H11C C11B H11D 108.2 . . ?
C12A C11C C12 109.8(6) . . ?
C12A C11C H11E 109.7 . . ?
C12 C11C H11E 109.7 . . ?
C12A C11C H11F 109.7 . . ?
C12 C11C H11F 109.7 . . ?
H11E C11C H11F 108.2 . . ?
C11C C12A C17 109.7(6) . . ?
C11C C12A H12A 109.7 . . ?
C17 C12A H12A 109.7 . . ?
C11C C12A H12B 109.7 . . ?
C17 C12A H12B 109.7 . . ?
H12A C12A H12B 108.2 . . ?
C17 C12B C11B 111.6(6) . . ?
C17 C12B H12C 109.3 . . ?
C11B C12B H12C 109.3 . . ?
C17 C12B H12D 109.3 . . ?
C11B C12B H12D 109.3 . . ?
H12C C12B H12D 108.0 . . ?
C11A C12C C17 108.9(6) . . ?
C11A C12C H12E 109.9 . . ?
C17 C12C H12E 109.9 . . ?
C11A C12C H12F 109.9 . . ?
C17 C12C H12F 109.9 . . ?
H12E C12C H12F 108.3 . . ?
C22 C13A H13B 109.2 . . ?
C22 C13A H13C 109.1 . . ?
H13B C13A H13C 109.5 . . ?
C22 C13B H13E 108.0 . . ?
C22 C13B H13F 110.9 . . ?
H13E C13B H13F 109.5 . . ?
C22 C13C H13H 109.7 . . ?
C22 C13C H13I 109.4 . . ?
H13H C13C H13I 109.5 . . ?
C12B C17 C18 109.5(4) . . ?
C12B C17 C12C 110.6(4) . . ?
C18 C17 C12C 111.2(3) . . ?
C12B C17 C12A 110.1(5) . . ?
C18 C17 C12A 109.8(3) . . ?
C12C C17 C12A 105.5(5) . . ?
O005 C18 O005 123.2(3) . 11_565 ?
O005 C18 C17 118.39(14) . . ?
O005 C18 C17 118.39(14) 11_565 . ?
C24 N1 C23 109.7(5) . . ?
C24 N1 C25 109.7(4) . . ?
C23 N1 C25 105.5(6) . . ?
C24 N1 Cu1 110.4(4) . . ?
C23 N1 Cu1 110.4(3) . . ?
C25 N1 Cu1 111.1(4) . . ?
N1 C24 H24A 109.8 . . ?
N1 C24 H24B 109.4 . . ?
H24A C24 H24B 108.2 . . ?
N1 C25 H25A 110.6 . . ?
N1 C25 H25B 107.6 . . ?
H25A C25 H25B 108.2 . . ?
N1 C23 H23A 108.4 . . ?
N1 C23 H23B 110.3 . . ?
H23A C23 H23B 108.3 . . ?
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
Cu1 O2 1.9532(15) . ?
Cu1 O2 1.9532(15) 11_565 ?
Cu1 O3 1.9676(16) . ?
Cu1 O3 1.9677(16) 10_556 ?
Cu1 N1 2.199(2) . ?
Cu1 Cu1 2.6352(10) 9_666 ?
O2 C6 1.2455(17) . ?
O3 C11 1.2448(18) . ?
O005 C18 1.251(2) . ?
O005 H005 0.8200 . ?
C6 O2 1.2455(17) 3_656 ?
C6 C22 1.527(3) . ?
C22 C13A 1.469(15) . ?
C22 C13B 1.541(13) . ?
C22 C13C 1.575(7) . ?
C11 O3 1.2448(18) 2_665 ?
C11 C12 1.525(3) . ?
C12 C11A 1.489(9) . ?
C12 C11B 1.549(8) . ?
C12 C11C 1.578(9) . ?
C11A C12C 1.542(10) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11B C12B 1.539(11) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C11C C12A 1.534(12) . ?
C11C H11E 0.9700 . ?
C11C H11F 0.9700 . ?
C12A C17 1.578(10) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12B C17 1.464(9) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C12C C17 1.572(8) . ?
C12C H12E 0.9700 . ?
C12C H12F 0.9700 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9599 . ?
C13B H13E 0.9600 . ?
C13B H13F 0.9599 . ?
C13C H13H 0.9600 . ?
C13C H13I 0.9600 . ?
C17 C18 1.512(4) . ?
C18 O005 1.251(2) 11_565 ?
N1 C24 1.460(6) . ?
N1 C23 1.480(6) . ?
N1 C25 1.479(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9701 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9699 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
