#------------------------------------------------------------------------------
#$Date: 2025-11-26 23:20:16 +0100 (Wed 26 de Nov de 2025) $
#$Revision: 303435 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/52/7135223.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_7135223
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            'C66 H48 N12 Ni O8 Re2'
_chemical_formula_weight         1568.27
_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 V118 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                   18.7166(7)
_cell_length_b                   18.7166(7)
_cell_length_c                   23.4717(15)
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.128
_cell_measurement_theta_min      2.176
_cell_volume                     7120.8(6)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS 8.5.0.27 Release/2023-03-20 && APEX5 2023.9-2'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5759
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_min         2.659
_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    2.783
_exptl_absorpt_correction_T_max  0.74521
_exptl_absorpt_correction_T_min  0.447162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L.,
Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       block
_exptl_crystal_F_000             2310
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.805
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.1189
_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)+(0.0700P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2690
_refine_ls_wR_factor_ref         0.3025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1892
_reflns_number_total             2884
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  -1.00001
_twin_individual_twin_matrix_12  -0.0002
_twin_individual_twin_matrix_13  -2e-05
_twin_individual_twin_matrix_21  0.99999
_twin_individual_twin_matrix_22  0.00013
_twin_individual_twin_matrix_23  1.00001
_twin_individual_twin_matrix_31  -0.00034
_twin_individual_twin_matrix_32  1.0
_twin_individual_twin_matrix_33  -5e-05
_cod_data_source_file            d5cc03326h2.cif
_cod_data_source_block           mo_20240707h1_re_0m_4_sq
_cod_original_cell_volume        7120.8(7)
_cod_database_code               7135223
_shelx_shelxl_version_number     2019/2
_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.
;
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
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
C1 C 0.5123(4) 0.7469(4) 0.7098(4) 0.0598(18) Uani 1 1 d . U . . .
H1 H 0.529934 0.785456 0.680506 0.072 Uiso 1 1 calc R U . . .
Ni1 Ni 0.333333 0.666667 0.666667 0.0509(7) Uani 1 6 d S T P . .
O1 O 0.5805(15) 0.5566(16) 0.7452(11) 0.215(11) Uani 0.2557(19) 1 d D U P A 1
O2 O 0.4080(11) 0.4562(19) 0.7561(12) 0.187(7) Uani 0.2557(19) 1 d D U P A 1
O3 O 0.5064(17) 0.5298(18) 0.8534(8) 0.193(11) Uani 0.2557(19) 1 d D U P A 1
O4 O 0.513(2) 0.4006(13) 0.7968(15) 0.230(9) Uani 0.2557(19) 1 d D U P A 1
Re1 Re 0.5014(2) 0.4853(2) 0.7876(2) 0.201(2) Uani 0.2557(19) 1 d D U P A 1
C2 C 0.4359(5) 0.6479(5) 0.7648(4) 0.070(2) Uani 1 1 d . U . . .
H2 H 0.389543 0.603199 0.780624 0.084 Uiso 1 1 calc R U . . .
C3 C 0.5154(5) 0.6810(5) 0.7859(4) 0.072(2) Uani 1 1 d . U . . .
H3 H 0.531927 0.664035 0.818029 0.087 Uiso 1 1 calc R U . . .
C4 C 0.6517(4) 0.7963(4) 0.7506(4) 0.0621(18) Uani 1 1 d . U . . .
C5 C 0.6989(5) 0.7703(5) 0.7794(4) 0.074(2) Uani 1 1 d . U . . .
H5 H 0.673957 0.719943 0.798293 0.089 Uiso 1 1 calc R U . . .
C6 C 0.7835(5) 0.8202(5) 0.7797(4) 0.076(2) Uani 1 1 d . U . . .
H6 H 0.815085 0.801918 0.798525 0.091 Uiso 1 1 calc R U . . .
C7 C 0.8229(4) 0.8958(4) 0.7532(4) 0.0650(18) Uani 1 1 d . U . . .
C8 C 0.7740(5) 0.9216(5) 0.7271(4) 0.080(2) Uani 1 1 d . U . . .
H8 H 0.798253 0.972454 0.708815 0.096 Uiso 1 1 calc R U . . .
C9 C 0.6873(5) 0.8715(5) 0.7277(4) 0.081(2) Uani 1 1 d . U . . .
H9 H 0.654765 0.891118 0.711965 0.097 Uiso 1 1 calc R U . . .
C10 C 0.9133(4) 0.9491(4) 0.7541(4) 0.0621(18) Uani 1 1 d . U . . .
C11 C 0.9502(4) 1.0351(4) 0.7542(4) 0.0595(19) Uani 1 1 d . U . . .
H11 H 0.916746 1.058716 0.754283 0.071 Uiso 1 1 calc R U . . .
N1 N 0.4350(3) 0.6902(3) 0.7175(3) 0.0510(14) Uani 1 1 d . U . . .
N2 N 0.5646(3) 0.7439(3) 0.7493(3) 0.0574(15) Uani 1 1 d . U . . .
O1A O 0.399(6) 0.315(3) 0.725(4) 0.220(17) Uani 0.0777(19) 1 d G U P A 2
O2A O 0.430(7) 0.396(7) 0.8304(10) 0.217(11) Uani 0.0777(19) 1 d G U P A 2
O3A O 0.394(6) 0.462(6) 0.734(5) 0.201(12) Uani 0.0777(19) 1 d G U P A 2
O4A O 0.5455(19) 0.465(5) 0.741(5) 0.215(9) Uani 0.0777(19) 1 d G U P A 2
Re1A Re 0.4421(10) 0.4095(10) 0.7579(8) 0.224(4) Uani 0.0777(19) 1 d G U P A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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 C1 N2 113.4(7) . . ?
N1 Ni1 N1 180.0(3) 14_456 2_665 ?
N1 Ni1 N1 90.9(2) 14_456 15_556 ?
N1 Ni1 N1 89.1(2) 2_665 15_556 ?
N1 Ni1 N1 89.1(2) 14_456 . ?
N1 Ni1 N1 90.9(2) 2_665 . ?
N1 Ni1 N1 89.1(2) 15_556 . ?
N1 Ni1 N1 89.1(2) 14_456 3_565 ?
N1 Ni1 N1 90.9(2) 2_665 3_565 ?
N1 Ni1 N1 180.0 15_556 3_565 ?
N1 Ni1 N1 90.9(2) . 3_565 ?
N1 Ni1 N1 90.9(2) 14_456 13_566 ?
N1 Ni1 N1 89.1(2) 2_665 13_566 ?
N1 Ni1 N1 90.9(2) 15_556 13_566 ?
N1 Ni1 N1 180.0 . 13_566 ?
N1 Ni1 N1 89.1(2) 3_565 13_566 ?
O2 Re1 O4 110.1(6) . . ?
O2 Re1 O1 109.9(6) . . ?
O4 Re1 O1 109.1(6) . . ?
O2 Re1 O3 109.8(6) . . ?
O4 Re1 O3 109.1(6) . . ?
O1 Re1 O3 108.8(6) . . ?
N1 C2 C3 110.6(7) . . ?
N2 C3 C2 105.7(7) . . ?
C9 C4 C5 119.9(7) . . ?
C9 C4 N2 121.1(7) . . ?
C5 C4 N2 118.9(7) . . ?
C6 C5 C4 119.1(7) . . ?
C7 C6 C5 122.6(7) . . ?
C6 C7 C8 117.0(7) . . ?
C6 C7 C10 122.4(7) . . ?
C8 C7 C10 120.6(7) . . ?
C7 C8 C9 120.6(8) . . ?
C4 C9 C8 120.5(7) . . ?
C11 C10 C11 117.9(8) 2_765 . ?
C11 C10 C7 120.9(7) 2_765 . ?
C11 C10 C7 121.2(7) . . ?
C10 C11 C10 122.1(8) 3_675 . ?
C1 N1 C2 104.6(6) . . ?
C1 N1 Ni1 127.6(5) . . ?
C2 N1 Ni1 127.7(5) . . ?
C1 N2 C3 105.7(6) . . ?
C1 N2 C4 125.6(7) . . ?
C3 N2 C4 128.7(6) . . ?
O2A Re1A O3A 109.6 . . ?
O2A Re1A O1A 109.53(5) . . ?
O3A Re1A O1A 109.5 . . ?
O2A Re1A O4A 109.52(5) . . ?
O3A Re1A O4A 109.4 . . ?
O1A Re1A O4A 109.3 . . ?
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
C1 N1 1.310(8) . ?
C1 N2 1.369(9) . ?
Ni1 N1 2.098(5) 14_456 ?
Ni1 N1 2.098(5) 2_665 ?
Ni1 N1 2.098(6) 15_556 ?
Ni1 N1 2.098(6) . ?
Ni1 N1 2.098(6) 3_565 ?
Ni1 N1 2.098(6) 13_566 ?
O1 Re1 1.727(10) . ?
O2 Re1 1.715(10) . ?
O3 Re1 1.734(10) . ?
O4 Re1 1.725(10) . ?
C2 N1 1.368(9) . ?
C2 C3 1.385(10) . ?
C3 N2 1.374(10) . ?
C4 C9 1.332(11) . ?
C4 C5 1.379(10) . ?
C4 N2 1.421(9) . ?
C5 C6 1.379(10) . ?
C6 C7 1.374(11) . ?
C7 C8 1.375(10) . ?
C7 C10 1.473(10) . ?
C8 C9 1.411(10) . ?
C10 C11 1.396(9) 2_765 ?
C10 C11 1.399(9) . ?
O1A Re1A 1.7213 . ?
O2A Re1A 1.7187 . ?
O3A Re1A 1.7203 . ?
O4A Re1A 1.7228 . ?
