#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:16:42 +0100 (vie 05 de feb de 2021) $
#$Revision: 261682 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/60/7706098.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_7706098
loop_
_publ_author_name
'Zhang, Ying-Ying'
'Liu, Qing'
'Zhang, Lin-Yan'
'Bao, Yu-Mei'
'Tan, Jing-Yi'
'Zhang, Na'
'Zhang, Jian-Yong'
'Liu, Zhen-Jiang'
_publ_section_title
;
 MOFs assembled from C₃ symmetric ligands: structure,
 iodine capture and role as bifunctional catalysts towards the
 oxidation-Knoevenagel cascade reaction.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              647
_journal_page_last               659
_journal_paper_doi               10.1039/d0dt03565c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C54 H45 N12 Ni3 O19.5'
_chemical_formula_weight         1350.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-11-10 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.362(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.144(2)
_cell_length_b                   26.077(5)
_cell_length_c                   15.602(3)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.35
_cell_volume                     4046.2(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83056
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.006
_diffrn_reflns_theta_min         2.346
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.753
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       rod
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.591
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7969
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.591
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0518
_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)+(0.1617P)²+15.2976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6645
_reflns_number_total             7969
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03565c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7706096--7706098.cif.'
_cod_original_cell_volume        4046.2(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C54 H45 N12 Ni3 O19.50'
_cod_database_code               7706098
_shelx_shelxl_version_number     2014/7
_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   0.817
_shelx_estimated_absorpt_t_max   0.929
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_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 0.20616(3) 0.19089(2) 0.79684(2) 0.02806(13) Uani 1 1 d . . . . .
Ni2 Ni 0.0000 0.0000 0.0000 0.03725(16) Uani 1 2 d S . P . .
O2 O 0.0074(2) 0.18620(8) 0.81493(14) 0.0362(5) Uani 1 1 d . . . . .
O1 O 0.0526(2) 0.22797(8) 0.70267(13) 0.0348(4) Uani 1 1 d . . . . .
O7 O 0.3027(2) 0.15047(9) 0.90355(15) 0.0403(5) Uani 1 1 d D . . . .
N1 N 0.1904(3) 0.12499(9) 0.71927(17) 0.0357(5) Uani 1 1 d . . . . .
C1 C -0.1728(3) 0.23138(11) 0.7263(2) 0.0327(6) Uani 1 1 d . . . . .
N4 N 0.1588(3) 0.00603(10) 0.46276(17) 0.0401(6) Uani 1 1 d . . . . .
O6 O -0.2903(3) 0.35649(9) 0.55732(17) 0.0513(6) Uani 1 1 d . . . . .
C26 C 0.1593(3) -0.03546(11) 0.41224(19) 0.0358(6) Uani 1 1 d . . . . .
N5 N 0.1825(3) -0.08313(10) 0.44163(17) 0.0397(6) Uani 1 1 d . . . . .
N6 N 0.2067(3) -0.04941(10) 0.58462(17) 0.0432(6) Uani 1 1 d . . . . .
O9 O -0.1124(3) 0.06271(9) 0.01923(18) 0.0497(6) Uani 1 1 d D . . . .
C7 C -0.0306(3) 0.21377(11) 0.74939(19) 0.0310(6) Uani 1 1 d . . . . .
C6 C -0.2085(3) 0.27240(11) 0.6684(2) 0.0351(6) Uani 1 1 d . . . . .
H6A H -0.1437 0.2879 0.6425 0.042 Uiso 1 1 calc R U . . .
N2 N 0.0535(3) -0.01202(10) 0.13614(17) 0.0438(7) Uani 1 1 d . . . . .
O5 O -0.4964(3) 0.35181(11) 0.5822(2) 0.0700(9) Uani 1 1 d . . . . .
C4 C -0.4373(3) 0.26560(12) 0.6867(2) 0.0386(7) Uani 1 1 d . . . . .
H4A H -0.5261 0.2766 0.6731 0.046 Uiso 1 1 calc R U . . .
C17 C 0.1265(3) -0.02741(11) 0.3162(2) 0.0378(7) Uani 1 1 d . . . . .
C27 C 0.2048(3) -0.08800(11) 0.5281(2) 0.0376(7) Uani 1 1 d . . . . .
O8 O 0.1679(3) 0.04526(10) 0.0051(2) 0.0561(7) Uani 1 1 d D . . . .
C5 C -0.3404(3) 0.28994(11) 0.64953(19) 0.0338(6) Uani 1 1 d . . . . .
C12 C 0.1865(3) 0.04125(11) 0.6077(2) 0.0373(7) Uani 1 1 d . . . . .
C2 C -0.2698(3) 0.20824(12) 0.7645(2) 0.0371(7) Uani 1 1 d . . . . .
H2A H -0.2459 0.1815 0.8040 0.045 Uiso 1 1 calc R U . . .
C3 C -0.4022(3) 0.22466(12) 0.7445(2) 0.0378(7) Uani 1 1 d . . . . .
C13 C 0.2182(4) 0.03527(12) 0.6978(2) 0.0456(8) Uani 1 1 d . . . . .
H13A H 0.2386 0.0030 0.7223 0.055 Uiso 1 1 calc R U . . .
C25 C 0.1846(3) -0.00340(11) 0.5484(2) 0.0376(7) Uani 1 1 d . . . . .
C16 C 0.1070(4) -0.06815(12) 0.2587(2) 0.0418(7) Uani 1 1 d . . . . .
H16A H 0.1195 -0.1016 0.2794 0.050 Uiso 1 1 calc R U . . .
C15 C 0.0690(4) -0.05905(12) 0.1707(2) 0.0454(8) Uani 1 1 d . . . . .
H15A H 0.0532 -0.0870 0.1331 0.055 Uiso 1 1 calc R U . . .
C9 C -0.3794(3) 0.33606(12) 0.5911(2) 0.0410(7) Uani 1 1 d . . . . .
C11 C 0.1570(4) 0.09024(12) 0.5746(2) 0.0452(8) Uani 1 1 d . . . . .
H11A H 0.1362 0.0958 0.5146 0.054 Uiso 1 1 calc R U . . .
C10 C 0.1591(4) 0.13042(12) 0.6317(2) 0.0457(8) Uani 1 1 d . . . . .
H10A H 0.1379 0.1630 0.6089 0.055 Uiso 1 1 calc R U . . .
C18 C 0.1092(4) 0.02189(13) 0.2815(2) 0.0503(9) Uani 1 1 d . . . . .
H18A H 0.1212 0.0504 0.3180 0.060 Uiso 1 1 calc R U . . .
C21 C 0.2353(5) -0.14823(13) 0.6546(2) 0.0571(10) Uani 1 1 d . . . . .
H21A H 0.2274 -0.1208 0.6914 0.068 Uiso 1 1 calc R U . . .
C22 C 0.2271(4) -0.14018(11) 0.5660(2) 0.0395(7) Uani 1 1 d . . . . .
C14 C 0.2193(4) 0.07788(12) 0.7510(2) 0.0444(8) Uani 1 1 d . . . . .
H14A H 0.2410 0.0735 0.8113 0.053 Uiso 1 1 calc R U . . .
C19 C 0.0740(5) 0.02746(13) 0.1922(2) 0.0547(10) Uani 1 1 d . . . . .
H19A H 0.0638 0.0605 0.1694 0.066 Uiso 1 1 calc R U . . .
C23 C 0.2401(5) -0.18260(13) 0.5153(2) 0.0561(10) Uani 1 1 d . . . . .
H23A H 0.2352 -0.1790 0.4554 0.067 Uiso 1 1 calc R U . . .
C24 C 0.2604(5) -0.22995(12) 0.5537(2) 0.0521(9) Uani 1 1 d . . . . .
H24A H 0.2684 -0.2580 0.5184 0.062 Uiso 1 1 calc R U . . .
C20 C 0.2553(5) -0.19701(13) 0.6877(2) 0.0547(10) Uani 1 1 d . . . . .
H20A H 0.2594 -0.2018 0.7473 0.066 Uiso 1 1 calc R U . . .
N3 N 0.2692(3) -0.23789(9) 0.63887(16) 0.0350(5) Uani 1 1 d . . . . .
C8 C -0.5082(3) 0.19983(13) 0.7867(2) 0.0443(8) Uani 1 1 d . . . . .
O3 O -0.4708(3) 0.17372(17) 0.8533(3) 0.0983(14) Uani 1 1 d . . . . .
O4 O -0.6269(2) 0.20888(9) 0.75101(15) 0.0403(5) Uani 1 1 d . . . . .
H9A H -0.081(6) 0.0897(13) 0.037(4) 0.095(19) Uiso 1 1 d D . . . .
H7A H 0.381(2) 0.1565(16) 0.915(3) 0.054(12) Uiso 1 1 d D . . . .
H9B H -0.191(2) 0.060(2) -0.002(4) 0.10(2) Uiso 1 1 d D . . . .
H7B H 0.263(4) 0.1507(17) 0.945(2) 0.058(12) Uiso 1 1 d D . . . .
H8B H 0.234(5) 0.037(3) -0.009(6) 0.17(4) Uiso 1 1 d D . . . .
H8A H 0.152(7) 0.0739(11) 0.013(5) 0.14(3) Uiso 1 1 d D . . . .
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
O4 Ni1 O7 96.15(9) 1_655 . ?
O4 Ni1 N1 87.70(10) 1_655 . ?
O7 Ni1 N1 90.99(10) . . ?
O4 Ni1 O2 163.44(9) 1_655 . ?
O7 Ni1 O2 100.33(9) . . ?
N1 Ni1 O2 93.67(9) . . ?
O4 Ni1 N3 86.24(10) 1_655 2_556 ?
O7 Ni1 N3 94.24(10) . 2_556 ?
N1 Ni1 N3 172.39(10) . 2_556 ?
O2 Ni1 N3 90.84(9) . 2_556 ?
O4 Ni1 O1 101.48(8) 1_655 . ?
O7 Ni1 O1 162.34(9) . . ?
N1 Ni1 O1 90.66(9) . . ?
O2 Ni1 O1 62.02(8) . . ?
N3 Ni1 O1 86.04(9) 2_556 . ?
O4 Ni1 C7 132.76(9) 1_655 . ?
O7 Ni1 C7 130.97(10) . . ?
N1 Ni1 C7 93.83(10) . . ?
O2 Ni1 C7 30.69(9) . . ?
N3 Ni1 C7 86.93(10) 2_556 . ?
O1 Ni1 C7 31.37(9) . . ?
O9 Ni2 O9 180.0 . 3 ?
O9 Ni2 O8 90.96(12) . . ?
O9 Ni2 O8 89.04(12) 3 . ?
O9 Ni2 O8 89.04(12) . 3 ?
O9 Ni2 O8 90.96(12) 3 3 ?
O8 Ni2 O8 180.0 . 3 ?
O9 Ni2 N2 90.64(11) . . ?
O9 Ni2 N2 89.36(11) 3 . ?
O8 Ni2 N2 89.98(12) . . ?
O8 Ni2 N2 90.02(12) 3 . ?
O9 Ni2 N2 89.36(11) . 3 ?
O9 Ni2 N2 90.64(11) 3 3 ?
O8 Ni2 N2 90.02(12) . 3 ?
O8 Ni2 N2 89.98(12) 3 3 ?
N2 Ni2 N2 180.0 . 3 ?
C7 O2 Ni1 90.33(17) . . ?
C7 O1 Ni1 87.16(17) . . ?
C14 N1 C10 117.6(3) . . ?
C14 N1 Ni1 123.8(2) . . ?
C10 N1 Ni1 118.5(2) . . ?
C2 C1 C6 119.7(3) . . ?
C2 C1 C7 119.9(3) . . ?
C6 C1 C7 120.4(3) . . ?
C25 N4 C26 114.7(3) . . ?
N5 C26 N4 125.0(3) . . ?
N5 C26 C17 118.0(3) . . ?
N4 C26 C17 117.0(3) . . ?
C27 N5 C26 115.0(3) . . ?
C25 N6 C27 114.9(3) . . ?
O2 C7 O1 120.3(3) . . ?
O2 C7 C1 120.3(3) . . ?
O1 C7 C1 119.4(3) . . ?
O2 C7 Ni1 58.98(15) . . ?
O1 C7 Ni1 61.46(15) . . ?
C1 C7 Ni1 175.0(2) . . ?
C5 C6 C1 120.2(3) . . ?
C15 N2 C19 116.8(3) . . ?
C15 N2 Ni2 121.9(2) . . ?
C19 N2 Ni2 121.3(2) . . ?
C5 C4 C3 120.5(3) . . ?
C16 C17 C18 117.9(3) . . ?
C16 C17 C26 121.5(3) . . ?
C18 C17 C26 120.6(3) . . ?
N5 C27 N6 125.1(3) . . ?
N5 C27 C22 118.3(3) . . ?
N6 C27 C22 116.5(3) . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 C9 119.5(3) . . ?
C6 C5 C9 121.0(3) . . ?
C11 C12 C13 118.0(3) . . ?
C11 C12 C25 121.0(3) . . ?
C13 C12 C25 121.0(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 C8 120.7(3) . . ?
C4 C3 C8 119.7(3) . . ?
C14 C13 C12 119.3(3) . . ?
N6 C25 N4 125.2(3) . . ?
N6 C25 C12 117.6(3) . . ?
N4 C25 C12 117.1(3) . . ?
C15 C16 C17 119.6(3) . . ?
N2 C15 C16 123.4(3) . . ?
O5 C9 O6 124.6(3) . . ?
O5 C9 C5 117.5(3) . . ?
O6 C9 C5 117.8(3) . . ?
C10 C11 C12 119.1(3) . . ?
N1 C10 C11 123.2(3) . . ?
C19 C18 C17 118.6(3) . . ?
C20 C21 C22 119.5(3) . . ?
C23 C22 C21 117.2(3) . . ?
C23 C22 C27 122.0(3) . . ?
C21 C22 C27 120.8(3) . . ?
N1 C14 C13 122.8(3) . . ?
N2 C19 C18 123.7(3) . . ?
C24 C23 C22 119.6(3) . . ?
N3 C24 C23 123.5(3) . . ?
N3 C20 C21 123.3(3) . . ?
C24 N3 C20 116.9(3) . . ?
C24 N3 Ni1 126.3(2) . 2_546 ?
C20 N3 Ni1 116.7(2) . 2_546 ?
O3 C8 O4 126.1(3) . . ?
O3 C8 C3 118.3(3) . . ?
O4 C8 C3 115.6(3) . . ?
C8 O4 Ni1 127.0(2) . 1_455 ?
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 O4 2.019(2) 1_655 ?
Ni1 O7 2.049(2) . ?
Ni1 N1 2.090(2) . ?
Ni1 O2 2.094(2) . ?
Ni1 N3 2.102(2) 2_556 ?
Ni1 O1 2.149(2) . ?
Ni1 C7 2.443(3) . ?
Ni2 O9 2.049(3) . ?
Ni2 O9 2.049(3) 3 ?
Ni2 O8 2.061(3) . ?
Ni2 O8 2.061(3) 3 ?
Ni2 N2 2.109(3) . ?
Ni2 N2 2.109(3) 3 ?
O2 C7 1.247(4) . ?
O1 C7 1.274(3) . ?
N1 C14 1.335(4) . ?
N1 C10 1.347(4) . ?
C1 C2 1.386(4) . ?
C1 C6 1.401(4) . ?
C1 C7 1.489(4) . ?
N4 C25 1.333(4) . ?
N4 C26 1.339(4) . ?
O6 C9 1.252(4) . ?
C26 N5 1.330(4) . ?
C26 C17 1.484(4) . ?
N5 C27 1.330(4) . ?
N6 C25 1.326(4) . ?
N6 C27 1.335(4) . ?
C6 C5 1.390(4) . ?
N2 C15 1.336(4) . ?
N2 C19 1.340(4) . ?
O5 C9 1.238(4) . ?
C4 C5 1.389(4) . ?
C4 C3 1.397(4) . ?
C17 C16 1.380(4) . ?
C17 C18 1.392(4) . ?
C27 C22 1.483(4) . ?
C5 C9 1.514(4) . ?
C12 C11 1.388(4) . ?
C12 C13 1.388(5) . ?
C12 C25 1.485(4) . ?
C2 C3 1.385(4) . ?
C3 C8 1.513(4) . ?
C13 C14 1.385(4) . ?
C16 C15 1.372(5) . ?
C11 C10 1.372(5) . ?
C18 C19 1.377(5) . ?
C21 C20 1.373(5) . ?
C21 C22 1.384(5) . ?
C22 C23 1.382(5) . ?
C23 C24 1.371(5) . ?
C24 N3 1.330(4) . ?
C20 N3 1.334(4) . ?
N3 Ni1 2.102(2) 2_546 ?
C8 O3 1.238(4) . ?
C8 O4 1.245(4) . ?
O4 Ni1 2.019(2) 1_455 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.154 0.345 0.008 1667 375 ' '
