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#$Date: 2019-11-23 07:45:00 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232466 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/77/4347719.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_4347719
loop_
_publ_author_name
'Aboutorabi, Leila'
'Morsali, Ali'
'Tahmasebi, Elham'
'Büyükgüngor, Orhan'
_publ_section_title
;
 Metal-Organic Framework Based on Isonicotinate N-Oxide for Fast and
 Highly Efficient Aqueous Phase Cr(VI) Adsorption.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5507
_journal_page_last               5513
_journal_paper_doi               10.1021/acs.inorgchem.6b00522
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '2(C12 H8 N2 O6 Pb), C2 H4 N O'
_chemical_formula_sum            'C26 H20 N5 O13 Pb2'
_chemical_formula_weight         1024.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 137.543(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.722(3)
_cell_length_b                   7.3936(6)
_cell_length_c                   21.633(2)
_cell_measurement_reflns_used    8233
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      1.89
_cell_volume                     2993.1(6)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'w scan,rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8233
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.491
_diffrn_reflns_theta_min         1.887
_exptl_absorpt_coefficient_mu    11.311
_exptl_absorpt_correction_T_max  0.4228
_exptl_absorpt_correction_T_min  0.0403
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.764
_refine_diff_density_min         -3.628
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0528
_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)+(0.0746P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2541
_reflns_number_total             3084
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00522_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2993.0(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347719
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.3893(4) 0.8549(16) 0.3767(5) 0.031(2) Uani 1 1 d . . . . .
C2 C 0.4614(4) 0.7786(15) 0.4608(5) 0.0291(19) Uani 1 1 d . . . . .
C3 C 0.4762(5) 0.7057(17) 0.5330(6) 0.039(2) Uani 1 1 d . . . . .
H3 H 0.4394 0.6882 0.5265 0.047 Uiso 1 1 calc R U . . .
C4 C 0.5449(5) 0.6598(17) 0.6136(7) 0.039(2) Uani 1 1 d . . . . .
H4 H 0.5550 0.6149 0.6624 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5840(5) 0.7326(17) 0.5504(6) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.6208 0.7340 0.5563 0.045 Uiso 1 1 calc R U . . .
C6 C 0.5159(5) 0.7841(18) 0.4692(6) 0.041(3) Uani 1 1 d . . . . .
H6 H 0.5066 0.8225 0.4203 0.049 Uiso 1 1 calc R U . . .
C7 C 0.2197(7) 1.0340(16) 0.0404(8) 0.041(2) Uani 1 1 d . . . . .
C8 C 0.2248(7) 0.9848(15) -0.0236(8) 0.039(2) Uani 1 1 d . . . . .
C9 C 0.2832(7) 1.0248(19) -0.0003(7) 0.047(3) Uani 1 1 d . . . . .
H9 H 0.3193 1.0929 0.0520 0.056 Uiso 1 1 calc R U . . .
C10 C 0.2905(7) 0.9637(16) -0.0551(8) 0.043(3) Uani 1 1 d . . . . .
H10 H 0.3318 0.9910 -0.0381 0.052 Uiso 1 1 calc R U . . .
C11 C 0.1777(5) 0.8368(19) -0.1577(6) 0.045(3) Uani 1 1 d . . . . .
H11 H 0.1409 0.7745 -0.2121 0.054 Uiso 1 1 calc R U . . .
C12 C 0.1695(6) 0.8964(19) -0.1055(7) 0.047(3) Uani 1 1 d . . . . .
H12 H 0.1266 0.8771 -0.1255 0.057 Uiso 1 1 calc R U . . .
N1 N 0.5968(4) 0.6802(12) 0.6213(5) 0.0348(18) Uani 1 1 d . . . . .
N2 N 0.2600(5) 0.6302(12) 0.1291(5) 0.0348(19) Uani 1 1 d . . . . .
O1 O 0.3828(4) 0.9389(11) 0.3217(4) 0.0380(17) Uani 1 1 d . . . . .
O2 O 0.3397(3) 0.8350(13) 0.3696(4) 0.0430(19) Uani 1 1 d . . . . .
O3 O 0.6646(3) 0.6442(14) 0.7018(4) 0.0478(19) Uani 1 1 d . . . . .
O4 O 0.2769(6) 1.0822(14) 0.1192(6) 0.057(2) Uani 1 1 d . . . . .
O5 O 0.1608(6) 1.0103(16) 0.0116(7) 0.065(3) Uani 1 1 d . . . . .
O6 O 0.2494(4) 0.7019(11) 0.1737(4) 0.0390(17) Uani 1 1 d . . . . .
Pb1 Pb 0.25695(2) 1.04638(5) 0.21168(2) 0.02988(15) Uani 1 1 d . . . . .
C13 C 0.544(2) 0.264(5) 0.283(3) 0.111(13) Uani 0.5 1 d D U P A -1
H13A H 0.5296 0.3525 0.2998 0.166 Uiso 0.5 1 calc R U P A -1
H13B H 0.5363 0.3110 0.2353 0.166 Uiso 0.5 1 calc R U P A -1
H13C H 0.5931 0.2342 0.3354 0.166 Uiso 0.5 1 calc R U P A -1
O7 O 0.5083(15) -0.168(4) 0.2129(18) 0.118(10) Uiso 0.5 1 d D . P A -1
C14 C 0.5332(14) -0.014(4) 0.2349(18) 0.060(7) Uani 0.5 1 d D U P A -1
H14 H 0.5685 0.0248 0.2411 0.072 Uiso 0.5 1 calc R U P A -1
N3 N 0.5000 0.099(4) 0.2500 0.099(7) Uani 1 2 d DS TU 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
O1 C1 O2 124.5(8) . .
O1 C1 C2 118.4(8) . .
O2 C1 C2 117.1(9) . .
C6 C2 C3 118.2(8) . .
C6 C2 C1 119.7(8) . .
C3 C2 C1 122.1(8) . .
C4 C3 C2 120.3(9) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
N1 C4 C3 119.3(9) . .
N1 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
N1 C5 C6 119.3(9) . .
N1 C5 H5 120.3 . .
C6 C5 H5 120.3 . .
C5 C6 C2 119.8(9) . .
C5 C6 H6 120.1 . .
C2 C6 H6 120.1 . .
O4 C7 O5 126.5(10) . .
O4 C7 C8 115.3(10) . .
O5 C7 C8 118.0(10) . .
C9 C8 C12 118.8(10) . .
C9 C8 C7 120.2(10) . .
C12 C8 C7 121.0(10) . .
C8 C9 C10 120.0(11) . .
C8 C9 H9 120.0 . .
C10 C9 H9 120.0 . .
N2 C10 C9 120.6(11) 7_565 .
N2 C10 H10 119.7 7_565 .
C9 C10 H10 119.7 . .
N2 C11 C12 119.4(10) 7_565 .
N2 C11 H11 120.3 7_565 .
C12 C11 H11 120.3 . .
C11 C12 C8 120.3(11) . .
C11 C12 H12 119.8 . .
C8 C12 H12 119.8 . .
C4 N1 O3 119.2(8) . .
C4 N1 C5 122.5(8) . .
O3 N1 C5 118.3(8) . .
C10 N2 O6 120.0(9) 7_565 .
C10 N2 C11 120.5(9) 7_565 7_565
O6 N2 C11 119.4(9) . 7_565
C1 O1 Pb1 100.7(5) . .
N1 O3 Pb1 111.5(7) . 5_676
C7 O4 Pb1 104.9(7) . .
N2 O6 Pb1 127.7(6) . .
O4 Pb1 O1 79.2(3) . .
O4 Pb1 O6 82.1(3) . .
O1 Pb1 O6 73.9(2) . .
O4 Pb1 O3 85.6(3) . 5_676
O1 Pb1 O3 76.5(2) . 5_676
O6 Pb1 O3 149.6(2) . 5_676
N3 C13 H13A 109.5 . .
N3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
O7 C14 N3 111(3) . .
O7 C14 H14 124.6 . .
N3 C14 H14 124.6 . .
C14 N3 C13 99(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.233(12) .
C1 O2 1.273(11) .
C1 C2 1.502(11) .
C2 C6 1.383(13) .
C2 C3 1.397(13) .
C3 C4 1.371(13) .
C3 H3 0.9300 .
C4 N1 1.331(13) .
C4 H4 0.9300 .
C5 N1 1.351(13) .
C5 C6 1.380(13) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O4 1.248(15) .
C7 O5 1.257(16) .
C7 C8 1.537(14) .
C8 C9 1.324(17) .
C8 C12 1.381(17) .
C9 C10 1.417(15) .
C9 H9 0.9300 .
C10 N2 1.303(15) 7_565
C10 H10 0.9300 .
C11 N2 1.361(14) 7_565
C11 C12 1.378(15) .
C11 H11 0.9300 .
C12 H12 0.9300 .
N1 O3 1.344(10) .
N2 C10 1.303(15) 7_565
N2 O6 1.308(10) .
N2 C11 1.361(14) 7_565
O1 Pb1 2.494(7) .
O3 Pb1 2.732(10) 5_676
O4 Pb1 2.454(8) .
O6 Pb1 2.637(8) .
Pb1 O3 2.732(10) 5_676
C13 N3 1.472(19) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
O7 C14 1.230(19) .
C14 N3 1.448(17) .
C14 H14 0.9300 .
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_4
O1 C1 C2 C6 -8.0(16) . .
O2 C1 C2 C6 175.2(10) . .
O1 C1 C2 C3 170.2(10) . .
O2 C1 C2 C3 -6.6(16) . .
C6 C2 C3 C4 7.0(17) . .
C1 C2 C3 C4 -171.2(11) . .
C2 C3 C4 N1 -2.1(18) . .
N1 C5 C6 C2 -1.1(18) . .
C3 C2 C6 C5 -5.4(17) . .
C1 C2 C6 C5 172.9(11) . .
O4 C7 C8 C9 -12.0(16) . .
O5 C7 C8 C9 172.9(13) . .
O4 C7 C8 C12 167.2(12) . .
O5 C7 C8 C12 -8.0(17) . .
C12 C8 C9 C10 -5.3(18) . .
C7 C8 C9 C10 173.8(12) . .
C8 C9 C10 N2 0.7(19) . 7_565
N2 C11 C12 C8 -1.7(19) 7_565 .
C9 C8 C12 C11 5.8(19) . .
C7 C8 C12 C11 -173.3(11) . .
C3 C4 N1 O3 176.5(11) . .
C3 C4 N1 C5 -4.8(17) . .
C6 C5 N1 C4 6.4(17) . .
C6 C5 N1 O3 -174.9(11) . .
O2 C1 O1 Pb1 1.6(12) . .
C2 C1 O1 Pb1 -175.0(8) . .
C4 N1 O3 Pb1 -107.4(9) . 5_676
C5 N1 O3 Pb1 73.9(10) . 5_676
O5 C7 O4 Pb1 13.5(15) . .
C8 C7 O4 Pb1 -161.1(8) . .
C10 N2 O6 Pb1 -121.5(10) 7_565 .
C11 N2 O6 Pb1 54.8(11) 7_565 .
O7 C14 N3 C13 175(3) . .
