#------------------------------------------------------------------------------
#$Date: 2025-11-26 23:20:16 +0100 (Wed 26 de Nov de 2025) $
#$Revision: 303435 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/52/7135221.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_7135221
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            'C33 H24 N6 Ni O3'
_chemical_formula_weight         611.29
_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
_audit_creation_method           SHELXL-2018/3
_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            6
_cell_length_a                   18.4326(5)
_cell_length_b                   18.4326(5)
_cell_length_c                   19.6463(12)
_cell_measurement_reflns_used    2960
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.413
_cell_volume                     5780.8(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.425
_diffrn_reflns_theta_min         2.210
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             1896
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.922
_exptl_transmission_factor_min   0.898
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0833
_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          0.2430
_refine_ls_wR_factor_ref         0.2864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1466
_reflns_number_total             2631
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc03326h2.cif
_cod_data_source_block           a_a_sq
_cod_original_cell_volume        5780.8(5)
_cod_database_code               7135221
_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.
;
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 0.46547(5) 0.0570(5) Uani 1 3 d S T P . .
N2 N 0.8288(2) 0.5608(2) 0.56291(19) 0.0537(10) Uiso 1 1 d . . . . .
N1 N 0.7535(2) 0.4332(2) 0.5215(2) 0.0558(10) Uiso 1 1 d . . . . .
C4 C 0.8614(3) 0.6489(3) 0.5714(2) 0.0513(11) Uani 1 1 d . . . . .
C7 C 0.9268(3) 0.8199(3) 0.5858(2) 0.0526(11) Uani 1 1 d . . . . .
C6 C 0.9687(3) 0.7811(3) 0.6121(3) 0.0627(13) Uani 1 1 d . . . . .
H6 H 1.019529 0.813436 0.634301 0.075 Uiso 1 1 calc R U . . .
O1 O 0.7628(3) 0.3497(3) 0.3977(2) 0.0975(14) Uani 1 1 d . . . . .
C5 C 0.9369(3) 0.6960(3) 0.6061(3) 0.0642(14) Uani 1 1 d . . . . .
H5 H 0.965111 0.670602 0.624726 0.077 Uiso 1 1 calc R U . . .
C10 C 0.9634(3) 0.9127(3) 0.5896(2) 0.0507(11) Uani 1 1 d . . . . .
C11 C 0.9143(3) 0.9482(3) 0.5901(2) 0.0526(12) Uani 1 1 d . . . . .
H11 H 0.856331 0.913924 0.590691 0.063 Uiso 1 1 calc R U . . .
C9 C 0.8195(3) 0.6859(3) 0.5465(3) 0.0644(14) Uani 1 1 d . . . . .
H9 H 0.768192 0.654114 0.524851 0.077 Uiso 1 1 calc R U . . .
C8 C 0.8536(3) 0.7711(3) 0.5537(3) 0.0621(14) Uani 1 1 d . . . . .
H8 H 0.824859 0.796097 0.535505 0.074 Uiso 1 1 calc R U . . .
C1 C 0.7716(3) 0.5119(3) 0.5157(3) 0.0695(15) Uani 1 1 d . . . . .
H1 H 0.748136 0.531134 0.483545 0.083 Uiso 1 1 calc R U . . .
C2 C 0.8491(4) 0.5104(3) 0.5987(3) 0.0760(16) Uani 1 1 d . . . . .
H2 H 0.887570 0.526427 0.634153 0.091 Uiso 1 1 calc R U . . .
C3 C 0.8031(3) 0.4335(3) 0.5731(3) 0.0748(16) Uani 1 1 d . . . . .
H3 H 0.804718 0.386567 0.588354 0.090 Uiso 1 1 calc R 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'
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'
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 93.92(15) 3_665 . ?
N1 Ni1 N1 93.92(15) 3_665 2_655 ?
N1 Ni1 N1 93.92(15) . 2_655 ?
N1 Ni1 O1 91.89(17) 3_665 . ?
N1 Ni1 O1 89.29(18) . . ?
N1 Ni1 O1 173.15(16) 2_655 . ?
N1 Ni1 O1 89.29(18) 3_665 3_665 ?
N1 Ni1 O1 173.15(16) . 3_665 ?
N1 Ni1 O1 91.89(17) 2_655 3_665 ?
O1 Ni1 O1 84.55(19) . 3_665 ?
N1 Ni1 O1 173.15(16) 3_665 2_655 ?
N1 Ni1 O1 91.89(17) . 2_655 ?
N1 Ni1 O1 89.29(18) 2_655 2_655 ?
O1 Ni1 O1 84.55(19) . 2_655 ?
O1 Ni1 O1 84.55(19) 3_665 2_655 ?
C1 N2 C2 106.8(4) . . ?
C1 N2 C4 125.5(4) . . ?
C2 N2 C4 127.8(4) . . ?
C1 N1 C3 105.0(4) . . ?
C1 N1 Ni1 126.3(3) . . ?
C3 N1 Ni1 128.6(3) . . ?
C9 C4 C5 120.4(4) . . ?
C9 C4 N2 120.6(4) . . ?
C5 C4 N2 119.0(4) . . ?
C8 C7 C6 117.4(4) . . ?
C8 C7 C10 121.1(4) . . ?
C6 C7 C10 121.4(4) . . ?
C7 C6 C5 121.7(4) . . ?
C4 C5 C6 118.3(4) . . ?
C11 C10 C11 118.5(5) . 2_765 ?
C11 C10 C7 121.6(4) . . ?
C11 C10 C7 119.9(4) 2_765 . ?
C10 C11 C10 121.5(5) . 3_675 ?
C4 C9 C8 119.3(4) . . ?
C7 C8 C9 122.9(4) . . ?
N1 C1 N2 110.9(4) . . ?
C3 C2 N2 106.6(5) . . ?
N1 C3 C2 110.7(5) . . ?
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 2.054(4) 3_665 ?
Ni1 N1 2.054(4) . ?
Ni1 N1 2.054(4) 2_655 ?
Ni1 O1 2.113(4) . ?
Ni1 O1 2.113(4) 3_665 ?
Ni1 O1 2.113(4) 2_655 ?
N2 C1 1.354(6) . ?
N2 C2 1.358(6) . ?
N2 C4 1.431(6) . ?
N1 C1 1.322(6) . ?
N1 C3 1.362(6) . ?
C4 C9 1.352(7) . ?
C4 C5 1.396(7) . ?
C7 C8 1.347(7) . ?
C7 C6 1.387(6) . ?
C7 C10 1.495(6) . ?
C6 C5 1.379(7) . ?
C10 C11 1.358(6) . ?
C10 C11 1.420(6) 2_765 ?
C9 C8 1.377(7) . ?
C2 C3 1.334(7) . ?
