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#$Date: 2025-11-26 23:20:16 +0100 (Wed 26 de Nov de 2025) $
#$Revision: 303435 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/52/7135224.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_7135224
loop_
_publ_author_name
'Sheng, Daopeng'
'Zhai, Fuwan'
'Li, Baoyu'
'Guo, Chenglong'
'Hou, Minglei'
'Jin, Yusheng'
'Zhang, Yugang'
'Zhang, Mingxing'
'Shen, Nannan'
'Diwu, Juan'
'Li, Jie'
'Wang, Shuao'
_publ_section_title
;
 Correlation between coordination environments and sorption selectivity to
 ⁹⁹TcO₄⁻ in two-dimensional metal-organic
 frameworks.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16082
_journal_page_last               16085
_journal_paper_doi               10.1039/d5cc03326h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C64 H46 N14 Ni'
_chemical_formula_weight         1069.86
_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
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V144 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-04-10 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.651(4)
_cell_length_b                   18.651(4)
_cell_length_c                   23.358(7)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.9215
_cell_measurement_theta_min      2.616
_cell_volume                     7037(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker BIS V6.2.10/2018-10-03'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1509
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17306
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.616
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    0.757
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.2255
_refine_ls_R_factor_gt           0.1344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.3416
_refine_ls_wR_factor_ref         0.3921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1606
_reflns_number_total             3598
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc03326h2.cif
_cod_data_source_block           mo_20230925j2_sq
_cod_database_code               7135224
_shelx_shelxl_version_number     2019/1
_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.
;
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.976
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 1000'
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
Ni1 Ni 0.666667 0.333333 0.333333 0.0703(7) Uani 1 6 d S T P . .
N1 N 0.6897(3) 0.4357(3) 0.2808(2) 0.0849(15) Uani 1 1 d . U . . .
N2 N 0.7436(3) 0.5654(3) 0.2508(2) 0.0859(15) Uani 1 1 d . . . . .
C1 C 0.7481(4) 0.5147(4) 0.2899(3) 0.0808(17) Uani 1 1 d . . . . .
H7 H 0.786780 0.532252 0.319383 0.097 Uiso 1 1 calc R U . . .
C2 C 0.6786(5) 0.5167(5) 0.2155(4) 0.114(3) Uani 1 1 d . . . . .
H2 H 0.659725 0.534485 0.184811 0.137 Uiso 1 1 calc R U . . .
C3 C 0.6471(5) 0.4376(4) 0.2338(3) 0.099(2) Uani 1 1 d . U . . .
H1 H 0.602940 0.391507 0.216859 0.119 Uiso 1 1 calc R U . . .
C4 C 0.7961(4) 0.6536(4) 0.2484(3) 0.0872(19) Uani 1 1 d . . . . .
C5 C 0.7678(4) 0.7011(4) 0.2254(3) 0.106(2) Uani 1 1 d . . . . .
H6 H 0.714890 0.676727 0.209724 0.127 Uiso 1 1 calc R U . . .
C6 C 0.8187(4) 0.7878(4) 0.2252(4) 0.110(2) Uani 1 1 d . . . . .
H5 H 0.798901 0.820531 0.209685 0.132 Uiso 1 1 calc R U . . .
C7 C 0.8975(4) 0.8248(4) 0.2476(3) 0.0892(19) Uani 1 1 d . . . . .
C8 C 0.9510(4) 0.9162(3) 0.2459(3) 0.0787(17) Uani 1 1 d . . . . .
C9 C 0.9251(4) 0.7744(4) 0.2694(4) 0.117(3) Uani 1 1 d . . . . .
H4 H 0.978513 0.797985 0.284096 0.140 Uiso 1 1 calc R U . . .
C10 C 0.8751(4) 0.6895(4) 0.2697(4) 0.117(3) Uani 1 1 d . . . . .
H3 H 0.895056 0.656445 0.284348 0.140 Uiso 1 1 calc R U . . .
C11 C 0.9156(3) 0.9650(3) 0.2461(3) 0.0820(17) Uani 0.6667 1 d . . P . .
N3 N 0.9156(3) 0.9650(3) 0.2461(3) 0.0820(17) Uani 0.3333 1 d . . P . .
H11 H 0.862608 0.942982 0.246293 0.098 Uiso 0.6667 1 calc R U P . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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 Ni1 N1 180.0(3) 18_545 3_665 ?
N1 Ni1 N1 90.0(2) 18_545 17 ?
N1 Ni1 N1 90.0(2) 3_665 17 ?
N1 Ni1 N1 90.0(2) 18_545 . ?
N1 Ni1 N1 90.0(2) 3_665 . ?
N1 Ni1 N1 90.0(2) 17 . ?
N1 Ni1 N1 90.0(2) 18_545 2_655 ?
N1 Ni1 N1 90.0(2) 3_665 2_655 ?
N1 Ni1 N1 180.0 17 2_655 ?
N1 Ni1 N1 90.0(2) . 2_655 ?
N1 Ni1 N1 90.0(2) 18_545 16_655 ?
N1 Ni1 N1 90.0(2) 3_665 16_655 ?
N1 Ni1 N1 90.0(2) 17 16_655 ?
N1 Ni1 N1 180.0 . 16_655 ?
N1 Ni1 N1 90.0(2) 2_655 16_655 ?
C1 N1 C3 105.2(5) . . ?
C1 N1 Ni1 125.7(5) . . ?
C3 N1 Ni1 129.0(4) . . ?
C1 N2 C2 106.8(6) . . ?
C1 N2 C4 125.8(6) . . ?
C2 N2 C4 127.4(6) . . ?
N1 C1 N2 111.2(6) . . ?
N1 C1 H7 124.4 . . ?
N2 C1 H7 124.4 . . ?
C3 C2 N2 106.9(7) . . ?
C3 C2 H2 126.5 . . ?
N2 C2 H2 126.5 . . ?
C2 C3 N1 109.9(6) . . ?
C2 C3 H1 125.1 . . ?
N1 C3 H1 125.1 . . ?
C5 C4 C10 120.1(6) . . ?
C5 C4 N2 120.1(6) . . ?
C10 C4 N2 119.8(5) . . ?
C4 C5 C6 119.7(7) . . ?
C4 C5 H6 120.2 . . ?
C6 C5 H6 120.2 . . ?
C7 C6 C5 120.8(6) . . ?
C7 C6 H5 119.6 . . ?
C5 C6 H5 119.6 . . ?
C9 C7 C6 118.0(6) . . ?
C9 C7 C8 121.8(6) . . ?
C6 C7 C8 120.1(6) . . ?
C11 C8 N3 120.7(6) 2_765 . ?
C11 C8 C7 119.7(5) 2_765 . ?
N3 C8 C7 119.6(5) . . ?
C7 C9 C10 121.1(7) . . ?
C7 C9 H4 119.4 . . ?
C10 C9 H4 119.4 . . ?
C4 C10 C9 120.3(6) . . ?
C4 C10 H3 119.9 . . ?
C9 C10 H3 119.9 . . ?
C8 N3 C8 119.3(6) 3_675 . ?
C8 N3 H11 120.3 3_675 . ?
C8 N3 H11 120.3 . . ?
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
Ni1 N1 2.125(5) 18_545 ?
Ni1 N1 2.125(5) 3_665 ?
Ni1 N1 2.125(5) 17 ?
Ni1 N1 2.125(5) . ?
Ni1 N1 2.125(5) 2_655 ?
Ni1 N1 2.125(5) 16_655 ?
N1 C1 1.341(7) . ?
N1 C3 1.367(8) . ?
N2 C1 1.347(8) . ?
N2 C2 1.368(9) . ?
N2 C4 1.435(8) . ?
C1 H7 0.9300 . ?
C2 C3 1.355(10) . ?
C2 H2 0.9300 . ?
C3 H1 0.9300 . ?
C4 C5 1.350(8) . ?
C4 C10 1.372(9) . ?
C5 C6 1.407(9) . ?
C5 H6 0.9300 . ?
C6 C7 1.376(9) . ?
C6 H5 0.9300 . ?
C7 C9 1.377(9) . ?
C7 C8 1.484(8) . ?
C8 C11 1.364(7) 2_765 ?
C8 N3 1.366(7) . ?
C9 C10 1.378(9) . ?
C9 H4 0.9300 . ?
C10 H3 0.9300 . ?
N3 H11 0.8600 . ?
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
C3 N1 C1 N2 0.0(7) . . . . ?
Ni1 N1 C1 N2 -176.3(4) . . . . ?
C2 N2 C1 N1 0.8(7) . . . . ?
C4 N2 C1 N1 179.3(5) . . . . ?
C1 N2 C2 C3 -1.3(9) . . . . ?
C4 N2 C2 C3 -179.8(6) . . . . ?
N2 C2 C3 N1 1.4(9) . . . . ?
C1 N1 C3 C2 -0.9(8) . . . . ?
Ni1 N1 C3 C2 175.3(5) . . . . ?
C1 N2 C4 C5 -152.1(7) . . . . ?
C2 N2 C4 C5 26.1(11) . . . . ?
C1 N2 C4 C10 27.9(10) . . . . ?
C2 N2 C4 C10 -154.0(8) . . . . ?
C10 C4 C5 C6 -2.3(12) . . . . ?
N2 C4 C5 C6 177.7(7) . . . . ?
C4 C5 C6 C7 0.7(12) . . . . ?
C5 C6 C7 C9 1.0(12) . . . . ?
C5 C6 C7 C8 178.6(7) . . . . ?
C9 C7 C8 C11 23.6(11) . . . 2_765 ?
C6 C7 C8 C11 -154.0(7) . . . 2_765 ?
C9 C7 C8 N3 -154.2(7) . . . . ?
C6 C7 C8 N3 28.2(10) . . . . ?
C6 C7 C9 C10 -1.2(13) . . . . ?
C8 C7 C9 C10 -178.8(7) . . . . ?
C5 C4 C10 C9 2.1(13) . . . . ?
N2 C4 C10 C9 -177.8(7) . . . . ?
C7 C9 C10 C4 -0.4(14) . . . . ?
C11 C8 N3 C8 0.6(13) 2_765 . . 3_675 ?
C7 C8 N3 C8 178.4(4) . . . 3_675 ?
