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#$Date: 2024-10-06 09:06:15 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295140 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/37/7133707.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_7133707
loop_
_publ_author_name
'Shao, Zhen-Wu'
'Xiong, Chaozhi'
'Yang, Jiajie'
'Mei, Zhewei'
'Xiong, Li'
'Wu, Wenjing'
'Liu, Chong'
_publ_section_title
;
 A Zr-hydroxamate metal-organic framework with intrinsic chelating sites
 for postsynthetic Pd metalation and Suzuki-Miyaura catalysis.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11100
_journal_page_last               11103
_journal_paper_doi               10.1039/d4cc03895a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C12 H8 N8 O8 Zr, 7[C3H7NO]'
_chemical_formula_sum            'C33 H57 N15 O15 Zr'
_chemical_formula_weight         995.136
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_symmetry_Int_Tables_number      192
_audit_creation_date             2024-08-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-08-30 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.8945(4)
_cell_length_b                   22.8945(4)
_cell_length_c                   16.5284(5)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      60.37
_cell_measurement_theta_min      3.36
_cell_volume                     7502.8(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9899
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.9958
_diffrn_reflns_Laue_measured_fraction_max 0.9899
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55736
_diffrn_reflns_point_group_measured_fraction_full 0.9958
_diffrn_reflns_point_group_measured_fraction_max 0.9899
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         60.38
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1343 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8819.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             3126.372
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6047
_refine_diff_density_min         -0.7097
_refine_diff_density_rms         0.0873
_refine_ls_d_res_high            0.7715
_refine_ls_d_res_low             19.8272
_refine_ls_goodness_of_fit_ref   1.0037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2947
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.9996
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1064P)²+2.3173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2166
_reflns_number_total             2947
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03895a2.cif
_cod_data_source_block           SUM-1-pz
_cod_depositor_comments          'Adding full bibliography for 7133707.cif.'
_cod_original_formula_sum        'C33 H57 N15 O15 Zr1'
_cod_database_code               7133707
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
N2 \\sim C2 \\sim C3: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1662 electrons were 
found in a volume of 5578Å³ in 1 void per unit cell. 
This is consistent with the presence of 7[C3H7NO] per Formula Unit 
which account for 1680 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x-y,x,z
3 y,-x+y,z
4 -y,x-y,z
5 -x+y,-x,z
6 x-y,-y,-z+1/2
7 -x,-x+y,-z+1/2
8 -x,-y,z
9 y,x,-z+1/2
10 -y,-x,-z+1/2
11 -x+y,y,-z+1/2
12 x,x-y,-z+1/2
13 -x,-y,-z
14 -x+y,-x,-z
15 -y,x-y,-z
16 y,-x+y,-z
17 x-y,x,-z
18 -x+y,y,z-1/2
19 x,x-y,z-1/2
20 x,y,-z
21 -y,-x,z-1/2
22 y,x,z-1/2
23 x-y,-y,z-1/2
24 -x,-x+y,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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zr1 Zr 0.5 0.5 0.25 0.02029(17) Uani 1.000000 4 S T P
O2 O 0.39876(9) 0.48478(9) 0.28301(12) 0.0348(4) Uani 1.000000 1 . . .
O1 O 0.43802(8) 0.47639(9) 0.14186(11) 0.0290(4) Uani 1.000000 1 . . .
N1 N 0.37801(10) 0.47454(12) 0.15195(13) 0.0328(5) Uani 1.000000 1 . . .
H1 H 0.35222(10) 0.47030(12) 0.11032(13) 0.0394(6) Uiso 1.000000 1 R . .
N2 N 0.26224(14) 0.47771(18) 0.17356(17) 0.0617(7) Uani 1.000000 1 . U .
C2 C 0.29546(14) 0.47751(19) 0.23769(17) 0.0456(6) Uani 1.000000 1 . U .
C1 C 0.36041(12) 0.47921(14) 0.22470(16) 0.0318(6) Uani 1.000000 1 . . .
C3 C 0.27324(16) 0.4780(2) 0.3144(2) 0.0564(7) Uani 1.000000 1 . U .
H3 H 0.29922(16) 0.4786(2) 0.3595(2) 0.0677(9) Uiso 1.000000 1 R . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01370 0.00670 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.02410 0.01340 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.03890 0.02410 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Zr -0.37500 1.76120 17.87650 10.94800 5.41732 3.65721 1.27618 11.91600 0.11762
87.66270 2.06929 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
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 Zr1 O2 106.67(10) . 9 y
O2 Zr1 O2 151.70(10) 8_665 . y
O2 Zr1 O2 80.37(10) 8_665 9 y
O2 Zr1 O2 80.37(10) 10_665 . y
O2 Zr1 O2 151.70(10) 10_665 9 y
O2 Zr1 O2 106.67(10) 10_665 8_665 y
O1 Zr1 O2 78.31(7) 8_665 10_665 y
O1 Zr1 O2 78.52(7) 8_665 9 y
O1 Zr1 O2 78.31(7) 10_665 8_665 y
O1 Zr1 O2 78.31(7) 9 . y
O1 Zr1 O2 78.52(7) 9 8_665 y
O1 Zr1 O2 137.47(6) 9 10_665 y
O1 Zr1 O2 78.31(7) . 9 y
O1 Zr1 O2 70.41(7) 8_665 8_665 y
O1 Zr1 O2 70.41(7) . . y
O1 Zr1 O2 70.41(7) 10_665 10_665 y
O1 Zr1 O2 137.47(6) . 8_665 y
O1 Zr1 O2 78.52(7) 10_665 . y
O1 Zr1 O2 78.52(7) . 10_665 y
O1 Zr1 O2 70.41(7) 9 9 y
O1 Zr1 O2 137.47(6) 8_665 . y
O1 Zr1 O2 137.47(6) 10_665 9 y
O1 Zr1 O1 69.52(9) 8_665 . y
O1 Zr1 O1 126.47(9) 10_665 8_665 y
O1 Zr1 O1 126.47(9) 9 . y
O1 Zr1 O1 69.52(9) 10_665 9 y
O1 Zr1 O1 139.06(8) 10_665 . y
O1 Zr1 O1 139.06(8) 9 8_665 y
C1 O2 Zr1 116.30(16) . 9 ?
N1 O1 Zr1 115.41(14) . . ?
H1 N1 O1 121.20(12) . . ?
C1 N1 O1 117.6(2) . . ?
C1 N1 H1 121.20(13) . . ?
C3 N2 C2 117.1(3) 11 . ?
C1 C2 N2 117.4(2) . . ?
C3 C2 N2 122.2(3) . . ?
C3 C2 C1 120.4(2) . . ?
N1 C1 O2 119.2(2) . . ?
C2 C1 O2 121.9(2) . . ?
C2 C1 N1 118.9(2) . . ?
C2 C3 N2 120.7(3) . 11 ?
H3 C3 N2 119.65(18) . 11 ?
H3 C3 C2 119.65(16) . . ?
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
Zr1 O2 2.2324(16) 8_665 y
Zr1 O2 2.2324(16) 9 y
Zr1 O2 2.2324(16) . y
Zr1 O2 2.2324(16) 10_665 y
Zr1 O1 2.1756(17) 8_665 y
Zr1 O1 2.1756(17) 9 y
Zr1 O1 2.1756(17) 10_665 y
Zr1 O1 2.1756(17) . y
O2 C1 1.267(3) . ?
O1 N1 1.363(2) . ?
N1 H1 0.8800 . ?
N1 C1 1.289(3) . ?
N2 C2 1.306(4) . ?
N2 C3 1.334(4) 11 ?
C2 C1 1.483(3) . ?
C2 C3 1.368(4) . ?
C3 H3 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O2 C1 N1 8.13(19) 9 . . . ?
Zr1 O2 C1 N1 8.13(19) 10_665 . . . ?
Zr1 O2 C1 N1 8.13(19) 8_665 . . . ?
Zr1 O2 C1 N1 8.13(19) . . . . ?
Zr1 O2 C1 C2 -172.2(2) 10_665 . . . ?
Zr1 O2 C1 C2 -172.2(2) 8_665 . . . ?
Zr1 O2 C1 C2 -172.2(2) . . . . ?
Zr1 O2 C1 C2 -172.2(2) 9 . . . ?
Zr1 O1 N1 C1 -7.57(19) . . . . ?
Zr1 O1 N1 C1 -7.57(19) 9 . . . ?
Zr1 O1 N1 C1 -7.57(19) 10_665 . . . ?
Zr1 O1 N1 C1 -7.57(19) 8_665 . . . ?
O2 C1 N1 O1 -0.5(3) . . . . ?
O2 C1 C2 N2 174.0(3) . . . . ?
O2 C1 C2 C3 -3.8(4) . . . . ?
O1 N1 C1 C2 179.9(3) . . . . ?
N1 C1 C2 N2 -6.3(3) . . . . ?
N1 C1 C2 C3 175.8(3) . . . . ?
N2 C2 C3 N2 1.0(5) . . . 11 ?
N2 C3 C2 N2 1.0(5) 11 . . . ?
N2 C3 C2 C1 178.8(3) 11 . . . ?
loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
N2 0.0100
C3 0.0050
loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
N2 C2 0.0040
C2 C3 0.0020
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 -0.597 -0.231 -0.921 5577.5 1662.2 '42 DMF'
