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#$Date: 2025-05-30 04:24:57 +0300 (Fri, 30 May 2025) $
#$Revision: 299875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/04/7250486.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_7250486
loop_
_publ_author_name
'Zhang, Tao'
'Liang, Shujun'
'Jia, Shuai'
'Cui, Haibo'
'Wang, Xinyi'
'Zhang, Xiutang'
_publ_section_title
;
 Nanoporous [Ho2(CO2)7(H2O)2]-organic frameworks for excellent catalytic
 performance on the cycloaddition of CO2 into epoxides and the
 deacetalization-Knoevenagel condensation
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              17811
_journal_page_last               17818
_journal_paper_doi               10.1039/D5RA02269J
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety
'0.25(C120 H40 Ho8 N4 O64), 4(C3 H7 N O), 8(H2 O)'
_chemical_formula_sum            'C41 H55 Ho2 N5 O24'
_chemical_formula_weight         1331.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-03-31 deposited with the CCDC.	2025-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8580(5)
_cell_length_b                   21.8580(5)
_cell_length_c                   14.4715(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.51
_cell_volume                     6914.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.12
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40545
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.514
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    2.308
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0824 before and 0.0695 after correction. The Ratio of minimum to maximum transmission is 0.8073. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.505(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         6157
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0380
_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)+(0.0663P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5065
_reflns_number_total             6157
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ra02269j2.cif
_cod_data_source_block           z
_cod_original_cell_volume        6914.1(5)
_cod_database_code               7250486
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.681
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.495(19)
 0.505(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O2-C1 \\sim C1-O1
 with sigma of 0.02
4. Rigid bond restraints
 C1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C12(H12), C14(H14), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'
'x, -y, -z+1/2'
'y, x, -z+1/4'
'-x, y, -z'
'-y, -x, -z+3/4'
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
C1 C 0.1170(7) 0.4726(7) 0.4324(14) 0.125(5) Uani 1 1 d D U . . .
C2 C 0.0939(5) 0.4813(6) 0.3317(8) 0.083(3) Uani 1 1 d . U . . .
C3 C 0.0330(4) 0.4825(6) 0.3293(7) 0.082(4) Uani 1 1 d . . . . .
H3 H 0.011790 0.471210 0.382347 0.098 Uiso 1 1 calc R . . . .
C4 C -0.0014(5) 0.500000 0.250000 0.069(4) Uani 1 2 d S T P . .
C5 C -0.0674(6) 0.500000 0.250000 0.086(5) Uani 1 2 d S T P . .
C6 C 0.1284(9) 0.500000 0.250000 0.097(5) Uani 1 2 d S TU P . .
C7 C 0.1953(5) 0.500000 0.250000 0.065(4) Uani 1 2 d S T P . .
C8 C 0.2265(3) 0.4525(5) 0.2896(7) 0.067(3) Uani 1 1 d . . . . .
H8 H 0.204991 0.420003 0.315235 0.080 Uiso 1 1 calc R . . . .
C9 C 0.2890(3) 0.4522(4) 0.2918(5) 0.0469(19) Uani 1 1 d . . . . .
C10 C 0.3249(4) 0.4023(4) 0.3357(5) 0.054(2) Uani 1 1 d . . . . .
C11 C 0.3104(4) 0.3775(4) 0.4203(5) 0.051(2) Uani 1 1 d . . . . .
C12 C 0.3440(4) 0.3272(4) 0.4543(6) 0.057(2) Uani 1 1 d . . . . .
H12 H 0.333774 0.309997 0.511002 0.068 Uiso 1 1 calc R . . . .
C13 C 0.3914(5) 0.3037(4) 0.4045(7) 0.066(3) Uani 1 1 d . . . . .
C14 C 0.4030(5) 0.3252(5) 0.3183(7) 0.076(3) Uani 1 1 d . . . . .
H14 H 0.432870 0.306367 0.282564 0.092 Uiso 1 1 calc R . . . .
C15 C 0.3716(4) 0.3740(5) 0.2830(8) 0.076(3) Uani 1 1 d . . . . .
H15 H 0.380998 0.388619 0.224281 0.092 Uiso 1 1 calc R . . . .
C16 C 0.2653(4) 0.4018(4) 0.4852(7) 0.058(2) Uani 1 1 d . U . . .
C17 C 0.4276(6) 0.2501(5) 0.4426(7) 0.073(3) Uani 1 1 d . . . . .
Ho1 Ho 0.17715(2) 0.44867(2) 0.60549(3) 0.05447(16) Uani 1 1 d . . . . .
N1 N 0.3223(5) 0.500000 0.250000 0.069(3) Uani 1 2 d S T P . .
O1 O 0.1017(5) 0.4220(7) 0.4912(8) 0.161(5) Uani 1 1 d D . . . .
O2 O 0.1449(5) 0.5188(6) 0.4872(9) 0.154(4) Uani 1 1 d D U . . .
O3 O -0.0950(3) 0.4842(5) 0.3172(7) 0.114(3) Uani 1 1 d . U . . .
O4 O 0.2604(4) 0.4565(4) 0.4971(7) 0.111(3) Uani 1 1 d . U . . .
O5 O 0.2319(4) 0.3675(4) 0.5332(6) 0.098(3) Uani 1 1 d . U . . .
O6 O 0.4217(5) 0.2374(4) 0.5251(6) 0.117(3) Uani 1 1 d . . . . .
O7 O 0.4610(4) 0.2218(4) 0.3967(6) 0.095(2) Uani 1 1 d . . . . .
O8 O 0.1302(7) 0.3608(7) 0.6689(9) 0.183(6) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ho Ho -0.2175 4.6783 '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'
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
O1 C1 C2 125.2(12) . . ?
O2 C1 C2 125.1(14) . . ?
O2 C1 O1 108.4(15) . . ?
C3 C2 C1 110.5(10) . . ?
C3 C2 C6 119.4(11) . . ?
C6 C2 C1 128.7(11) . . ?
C2 C3 H3 118.2 . . ?
C2 C3 C4 123.6(10) . . ?
C4 C3 H3 118.2 . . ?
C3 C4 C3 116.3(11) . 5_565 ?
C3 C4 C5 121.8(6) . . ?
C3 C4 C5 121.8(6) 5_565 . ?
O3 C5 C4 120.3(7) 5_565 . ?
O3 C5 C4 120.3(7) . . ?
O3 C5 O3 119.4(15) 5_565 . ?
C2 C6 C2 117.7(16) 5_565 . ?
C7 C6 C2 121.1(8) . . ?
C7 C6 C2 121.1(8) . 5_565 ?
C8 C7 C6 120.0(5) 5_565 . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 C8 120.1(11) . 5_565 ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.8(9) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C10 122.7(8) . . ?
C8 C9 N1 120.2(8) . . ?
N1 C9 C10 117.1(7) . . ?
C11 C10 C9 123.3(7) . . ?
C11 C10 C15 118.2(8) . . ?
C15 C10 C9 118.1(7) . . ?
C10 C11 C12 119.9(8) . . ?
C10 C11 C16 125.7(8) . . ?
C12 C11 C16 114.2(7) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(8) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C17 119.8(9) . . ?
C14 C13 C12 119.8(9) . . ?
C14 C13 C17 120.2(9) . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C15 121.4(10) . . ?
C15 C14 H14 119.3 . . ?
C10 C15 H15 120.0 . . ?
C14 C15 C10 120.0(9) . . ?
C14 C15 H15 120.0 . . ?
O4 C16 C11 120.6(9) . . ?
O4 C16 O5 117.3(10) . . ?
O5 C16 C11 122.1(9) . . ?
O6 C17 C13 118.1(10) . . ?
O7 C17 C13 122.0(10) . . ?
O7 C17 O6 119.9(11) . . ?
O1 Ho1 O4 95.0(4) . . ?
O2 Ho1 O1 57.6(4) . . ?
O2 Ho1 O4 73.3(4) . . ?
O3 Ho1 O1 83.0(4) 7_556 . ?
O3 Ho1 O2 84.3(4) 7_556 . ?
O3 Ho1 O4 154.3(4) 7_556 . ?
O3 Ho1 O5 151.0(3) 7_556 . ?
O3 Ho1 O7 85.0(3) 7_556 4_565 ?
O3 Ho1 O8 75.0(5) 7_556 . ?
O5 Ho1 O1 82.1(4) . . ?
O5 Ho1 O2 108.0(4) . . ?
O5 Ho1 O4 52.2(3) . . ?
O6 Ho1 O1 149.9(5) 6_556 . ?
O6 Ho1 O2 152.3(4) 6_556 . ?
O6 Ho1 O3 100.1(3) 6_556 7_556 ?
O6 Ho1 O4 94.4(4) 6_556 . ?
O6 Ho1 O5 81.3(3) 6_556 . ?
O6 Ho1 O7 77.0(4) 6_556 4_565 ?
O6 Ho1 O8 75.1(5) 6_556 . ?
O7 Ho1 O1 133.0(4) 4_565 . ?
O7 Ho1 O2 76.1(4) 4_565 . ?
O7 Ho1 O4 77.6(3) 4_565 . ?
O7 Ho1 O5 123.0(3) 4_565 . ?
O7 Ho1 O8 141.9(4) 4_565 . ?
O8 Ho1 O1 76.9(5) . . ?
O8 Ho1 O2 131.9(5) . . ?
O8 Ho1 O4 129.7(5) . . ?
O8 Ho1 O5 77.5(5) . . ?
C9 N1 C9 117.8(10) . 5_565 ?
C1 O1 Ho1 93.6(9) . . ?
C1 O2 Ho1 94.0(10) . . ?
C5 O3 Ho1 154.9(9) . 7_556 ?
C16 O4 Ho1 95.2(7) . . ?
C16 O5 Ho1 95.2(6) . . ?
C17 O6 Ho1 148.0(9) . 6_556 ?
C17 O7 Ho1 156.7(9) . 2_654 ?
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
C1 C2 1.55(2) . ?
C1 O1 1.433(17) . ?
C1 O2 1.422(16) . ?
C2 C3 1.331(14) . ?
C2 C6 1.461(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.424(11) . ?
C4 C5 1.443(19) . ?
C5 O3 1.197(10) 5_565 ?
C5 O3 1.197(10) . ?
C6 C7 1.46(2) . ?
C7 C8 1.368(10) . ?
C7 C8 1.368(10) 5_565 ?
C8 H8 0.9300 . ?
C8 C9 1.366(11) . ?
C9 C10 1.487(11) . ?
C9 N1 1.409(10) . ?
C10 C11 1.377(11) . ?
C10 C15 1.418(13) . ?
C11 C12 1.410(12) . ?
C11 C16 1.461(12) . ?
C12 H12 0.9300 . ?
C12 C13 1.362(13) . ?
C13 C14 1.357(13) . ?
C13 C17 1.517(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.367(15) . ?
C15 H15 0.9300 . ?
C16 O4 1.213(12) . ?
C16 O5 1.255(11) . ?
C17 O6 1.234(12) . ?
C17 O7 1.163(12) . ?
Ho1 O1 2.406(9) . ?
Ho1 O2 2.403(11) . ?
Ho1 O3 2.253(7) 7_556 ?
Ho1 O4 2.408(8) . ?
Ho1 O5 2.383(8) . ?
Ho1 O6 2.251(8) 6_556 ?
Ho1 O7 2.283(8) 4_565 ?
Ho1 O8 2.364(12) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.495(19)
2 0.505(19)
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.291 3972.2 80.1 ?
2 0.500 0.500 -0.291 545.4 0.0 ?
