#------------------------------------------------------------------------------
#$Date: 2019-07-06 06:56:05 +0300 (Sat, 06 Jul 2019) $
#$Revision: 216788 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021700.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2021700
loop_
_publ_author_name
'Marandi, Farzin'
'Moeini, Keyvan'
'Mardani, Zahra'
'Krautscheid, Harald'
_publ_section_title
;
Spectral, structural and theoretical study of the effects of thiocyanato
and dicyanamido ligands on the geometry of PbII complexes containing a
triazinic ligand
;
_journal_coeditor_code YP3186
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229619008301
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Pb2 (C2 N3)2 (N O3)2 (C16 H10 N4 O2)4]'
_chemical_formula_moiety 'C68 H40 N24 O14 Pb2'
_chemical_formula_sum 'C68 H40 N24 O14 Pb2'
_chemical_formula_weight 1831.62
_chemical_name_systematic
Di-\m-dicyanamido-\k^2^N^1^:N^5^;\k^2^N^5^:N^1^-bis{[5,6-bis(furan-2-yl)-3-(pyridin-2-yl-\kN)-1,2,4-triazine-\kN^2^](nitrato-\k^2^O,O')lead(II)}
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 66.834(5)
_cell_angle_beta 80.260(6)
_cell_angle_gamma 67.514(5)
_cell_formula_units_Z 1
_cell_length_a 10.5123(8)
_cell_length_b 12.2682(8)
_cell_length_c 15.6379(10)
_cell_measurement_reflns_used 22877
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 29.5
_cell_measurement_theta_min 1.9
_cell_volume 1712.8(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2016)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996),
ORTEP-3 for Windows (Farrugia, 2012) and
DIAMOND (Bergerhof et al., 1996)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Stoe IPDS-2T'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0259
_diffrn_reflns_av_unetI/netI 0.0326
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 22922
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.998
_diffrn_reflns_theta_min 1.926
_diffrn_source 'sealed tube'
_exptl_absorpt_coefficient_mu 4.994
_exptl_absorpt_correction_T_max 0.4511
_exptl_absorpt_correction_T_min 0.3103
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details '(X-AREA; Stoe & Cie, 2016)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.776
_exptl_crystal_description 'block, fragment'
_exptl_crystal_F_000 892
_exptl_crystal_size_max 0.330
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.210
_refine_diff_density_max 0.847
_refine_diff_density_min -0.767
_refine_ls_extinction_coef 0.00200(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 0.931
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 488
_refine_ls_number_reflns 7484
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.931
_refine_ls_R_factor_all 0.0345
_refine_ls_R_factor_gt 0.0259
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0557
_refine_ls_wR_factor_ref 0.0573
_reflns_number_gt 6299
_reflns_number_total 7484
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yp3186sup1.cif
_cod_data_source_block 2
_cod_database_code 2021700
_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 0.290
_shelx_estimated_absorpt_t_max 0.420
_shelx_hkl_file
;
0 1 13 71.39 7.36 0
0 4 13 92.30 6.01 0
0 5 6 358.97 6.81 0
0 5 12 245.77 6.20 0
1 -6 0 391.65 7.50 0
1 -6 7 162.64 8.16 0
1 4 17 19.93 6.19 0
1 5 17 5.28 5.75 0
1 6 2 56.27 4.33 0
1 7 4 291.93 6.53 0
1 8 7 1.91 5.09 0
1 8 14 26.26 5.56 0
2 -7 -2 66.01 5.83 0
2 -4 -5 136.77 6.13 0
2 -3 15 18.18 13.95 0
2 2 19 1.74 8.35 0
2 5 -2 742.49 13.16 0
2 8 2 337.23 6.92 0
2 9 4 299.39 6.39 0
2 9 18 -0.48 4.30 0
2 10 7 361.43 6.54 0
2 10 16 58.40 5.89 0
3 -8 -2 313.55 6.73 0
3 -7 -4 163.49 4.66 0
3 -3 -7 314.87 7.28 0
3 -2 -7 124.30 6.67 0
3 -1 -7 100.02 5.96 0
3 6 -3 361.21 10.60 0
3 9 21 16.77 6.95 0
3 10 20 2.12 6.53 0
3 11 5 100.21 5.75 0
3 11 19 16.63 6.22 0
3 12 8 153.26 5.83 0
3 12 16 67.68 6.09 0
3 12 17 0.74 4.09 0
4 -9 -1 119.28 4.89 0
4 -9 6 0.70 7.35 0
4 -8 -4 16.26 3.99 0
4 -7 -6 536.35 7.56 0
4 -7 12 6.72 8.35 0
4 -6 -7 6.50 5.22 0
4 -4 -8 310.50 7.18 0
4 11 2 170.39 7.26 0
4 12 4 112.46 5.92 0
4 13 19 25.69 6.59 0
4 14 11 12.95 5.41 0
4 14 12 74.46 5.99 0
4 14 13 1.01 5.46 0
4 14 14 59.66 6.09 0
4 14 15 47.45 5.91 0
4 14 16 1.63 4.24 0
5 -9 -3 19.39 4.19 0
5 -7 -7 339.56 6.86 0
5 -6 -8 18.31 5.70 0
5 -4 -9 197.46 6.50 0
5 9 -3 128.91 7.78 0
5 14 6 111.89 6.12 0
5 15 9 20.79 4.03 0
5 15 10 18.62 5.68 0
6 -10 -1 0.10 5.95 0
6 -10 0 21.83 6.20 0
6 -10 1 1.20 4.35 0
6 -10 2 5.50 4.56 0
6 -10 3 18.54 6.38 0
6 -3 -10 82.06 6.28 0
6 -2 -10 82.55 6.48 0
6 -1 -10 37.95 5.78 0
6 0 -10 86.28 6.53 0
6 3 -9 173.89 8.57 0
6 15 6 9.22 5.84 0
6 16 9 27.86 5.90 0
7 -10 -2 1.92 6.26 0
7 -9 -5 8.15 4.17 0
7 -8 -7 8.47 5.63 0
7 -6 -9 103.67 4.93 0
7 16 6 24.44 6.18 0
8 -9 -6 8.47 6.08 0
8 -3 -11 5.31 6.54 0
8 1 -11 37.99 6.90 0
8 4 -10 26.25 8.26 0
8 12 -3 0.95 7.30 0
8 14 0 8.95 7.59 0
9 -7 -9 4.83 6.42 0
9 -4 -11 11.25 6.99 0
9 5 -10 11.83 7.96 0
9 12 -4 0.73 7.68 0
10 -4 -11 0.41 6.96 0
0 3 13 71.73 5.81 0
0 4 4 1021.88 10.42 0
0 4 12 405.60 7.09 0
0 5 7 310.93 6.66 0
0 5 10 369.58 6.84 0
0 5 11 67.53 4.13 0
1 -5 -2 55.10 4.44 0
1 -4 -3 1586.62 12.64 0
1 1 16 103.02 8.14 0
1 5 1 1317.60 12.45 0
1 6 16 52.54 5.73 0
1 7 15 58.88 5.70 0
1 8 8 346.74 6.39 0
1 8 12 24.55 5.27 0
1 8 13 199.99 4.75 0
2 -8 1 157.05 5.94 0
2 -8 2 226.73 6.71 0
2 -8 3 6.70 5.82 0
2 -7 8 37.08 6.02 0
2 -6 -4 1033.73 9.47 0
2 -1 17 9.92 9.29 0
2 6 19 33.05 6.43 0
2 7 19 21.02 4.52 0
2 8 18 8.58 5.94 0
2 9 17 103.32 6.28 0
2 10 8 0.54 4.98 0
2 10 15 47.67 5.75 0
3 -8 -3 45.02 5.59 0
3 -8 8 62.63 8.12 0
3 -6 -6 7.91 5.18 0
3 -4 -7 396.40 7.45 0
3 0 -7 54.76 5.54 0
3 1 20 1.85 8.87 0
3 8 21 29.93 7.14 0
3 9 1 285.00 6.84 0
3 10 3 210.72 6.26 0
3 11 18 80.14 6.40 0
3 12 9 57.99 5.59 0
3 12 10 160.37 6.11 0
3 12 15 29.46 5.69 0
4 -9 -2 15.53 3.74 0
4 -8 -5 117.55 6.00 0
4 -8 10 7.49 7.94 0
4 1 -8 4.19 7.00 0
4 3 -7 347.92 10.69 0
4 12 20 29.66 6.64 0
4 13 7 145.31 4.56 0
4 13 18 0.82 6.30 0
5 -10 0 1.45 5.78 0
5 -10 1 49.94 6.15 0
5 -10 2 12.02 6.02 0
5 -10 3 4.98 6.17 0
5 -9 -4 60.23 4.38 0
5 -8 -6 32.36 4.02 0
5 -5 -9 189.03 6.77 0
5 1 -9 76.42 6.58 0
5 8 -4 23.40 8.63 0
5 11 0 20.40 5.51 0
5 13 4 84.74 5.74 0
5 15 11 77.94 6.27 0
5 15 12 6.22 5.89 0
5 15 15 8.62 6.11 0
5 15 16 59.91 6.22 0
6 -10 -2 37.50 5.99 0
6 -9 -5 67.13 4.74 0
6 -8 -7 57.39 5.82 0
6 -7 -8 77.59 4.53 0
6 -6 -9 15.61 5.95 0
6 -4 -10 109.12 6.20 0
6 10 -3 24.09 7.90 0
6 16 10 45.45 6.33 0
6 16 11 3.75 5.88 0
7 -10 -3 18.50 4.34 0
7 -9 -6 37.30 6.26 0
7 -7 -9 21.85 6.21 0
7 -5 -10 1.16 4.38 0
7 -2 -11 30.63 6.44 0
7 -1 -11 35.62 6.52 0
7 11 -3 63.58 8.72 0
7 13 0 21.59 7.24 0
7 15 4 34.67 6.25 0
8 -8 -8 -2.58 6.03 0
8 -7 -9 19.63 4.52 0
8 -6 -10 27.70 6.36 0
8 -4 -11 7.49 6.38 0
8 15 2 -0.26 6.10 0
8 16 4 5.29 6.12 0
9 -6 -10 6.30 4.83 0
9 3 -11 13.55 8.11 0
9 11 -5 15.22 10.44 0
9 14 -1 8.61 7.69 0
10 -2 -12 16.17 7.49 0
10 -1 -12 9.84 7.34 0
10 0 -12 7.38 7.29 0
10 4 -11 5.34 8.70 0
10 6 -10 7.90 9.43 0
0 -4 1 456.93 9.49 0
0 -3 0 1087.72 14.15 0
0 0 12 239.34 8.49 0
0 3 12 319.61 6.98 0
0 5 8 69.15 4.00 0
0 5 9 282.00 5.30 0
1 -6 -1 186.19 5.31 0
1 -5 10 24.70 10.35 0
1 5 16 182.24 6.33 0
1 7 5 319.41 6.50 0
1 7 14 93.18 5.57 0
1 8 9 235.32 4.66 0
1 8 10 207.66 4.70 0
1 8 11 158.05 4.44 0
2 -8 0 54.57 5.62 0
2 -8 4 81.65 6.09 0
2 -8 5 2.90 6.72 0
2 -7 -3 265.15 6.76 0
2 -5 -5 134.87 4.66 0
2 -2 16 33.40 10.88 0
2 1 -5 532.30 11.70 0
2 3 19 4.22 6.65 0
2 5 19 28.91 6.47 0
2 9 5 421.21 6.96 0
2 9 16 24.97 5.60 0
2 10 9 345.81 6.46 0
2 10 10 112.94 5.47 0
2 10 11 28.47 5.14 0
2 10 12 240.59 5.98 0
2 10 13 2.10 5.23 0
2 10 14 158.84 4.73 0
3 -9 0 100.62 5.89 0
3 -9 1 54.43 4.27 0
3 -9 2 17.03 4.17 0
3 -9 3 82.39 6.14 0
3 -9 4 5.18 5.55 0
3 -7 -5 339.28 5.56 0
3 -5 -7 335.41 7.05 0
3 4 21 21.78 7.35 0
3 5 21 18.84 8.90 0
3 6 21 20.59 7.12 0
3 7 21 21.64 7.16 0
3 9 20 5.99 4.62 0
3 10 19 40.34 4.47 0
3 11 6 194.84 5.76 0
3 11 17 1.16 5.77 0
3 12 11 210.33 4.91 0
3 12 12 2.47 5.23 0
3 12 13 86.09 4.23 0
3 12 14 27.50 3.86 0
4 -9 -3 119.94 4.91 0
4 -9 7 11.34 6.14 0
4 -5 -8 248.29 5.20 0
4 9 -1 21.00 5.48 0
4 12 5 157.23 6.00 0
4 13 8 27.76 3.98 0
4 13 17 61.91 6.34 0
5 -10 -2 53.69 5.87 0
5 -10 -1 33.46 4.58 0
5 -10 4 20.25 6.34 0
5 -10 5 3.48 6.29 0
5 -9 -5 10.45 5.66 0
5 -8 -7 78.29 5.90 0
5 -7 -8 7.21 5.64 0
5 12 2 84.12 5.88 0
5 14 7 22.12 4.06 0
5 15 13 41.98 4.48 0
5 15 14 45.34 4.31 0
6 -10 -4 17.46 5.97 0
6 -10 -3 13.35 4.14 0
6 -9 -6 8.00 5.81 0
6 -5 -10 126.30 6.85 0
6 1 -10 29.42 6.27 0
6 5 -8 40.70 8.79 0
6 12 0 72.48 6.09 0
6 13 2 63.11 7.32 0
6 14 4 7.53 5.61 0
6 15 7 39.41 6.01 0
6 16 12 37.45 6.19 0
6 16 13 10.66 6.27 0
6 16 14 12.18 6.22 0
7 -10 -4 6.48 4.21 0
7 -9 -7 1.82 5.85 0
7 -8 -8 29.92 4.33 0
7 -6 -10 5.06 6.07 0
7 -4 -11 66.56 6.44 0
7 -3 -11 56.00 6.55 0
7 0 -11 12.81 6.35 0
7 3 -10 51.09 7.91 0
7 14 2 54.19 6.21 0
7 16 7 16.18 6.08 0
8 -9 -7 18.25 6.27 0
8 -5 -11 -2.55 6.36 0
8 2 -11 20.69 6.45 0
9 -7 -10 10.44 6.76 0
9 -5 -11 23.27 4.70 0
9 -2 -12 1.64 6.68 0
9 -1 -12 6.00 6.82 0
9 0 -12 3.53 6.85 0
10 -3 -12 1.16 7.24 0
10 1 -12 7.36 7.23 0
0 -1 11 14.37 7.67 0
0 1 12 161.80 7.57 0
0 3 3 479.27 8.94 0
0 4 5 654.42 7.85 0
0 4 10 569.37 7.87 0
0 4 11 226.54 4.99 0
1 -7 1 4.63 5.24 0
1 -7 2 226.77 6.85 0
1 -7 3 32.87 5.60 0
1 -7 4 227.75 7.17 0
1 -6 -2 292.16 7.03 0
1 -6 8 9.11 7.56 0
1 -5 -3 662.89 8.92 0
1 2 16 111.71 6.59 0
1 4 0 6.35 5.46 0
1 4 16 120.63 6.47 0
1 6 3 497.91 6.95 0
1 6 15 34.80 4.13 0
1 7 6 209.28 5.83 0
1 7 13 198.35 5.98 0
2 -8 -1 252.90 6.81 0
2 -6 11 75.89 9.83 0
2 -3 -6 470.78 8.16 0
2 -2 -6 355.92 8.05 0
2 1 18 53.46 8.20 0
2 7 1 77.63 5.42 0
2 7 18 17.42 4.32 0
2 8 3 114.09 5.85 0
2 8 17 67.79 6.05 0
2 9 15 79.02 5.80 0
3 -9 -2 199.95 6.42 0
3 -9 -1 42.74 4.20 0
3 -9 5 39.64 6.00 0
3 -8 -4 18.81 4.07 0
3 -7 11 13.57 7.79 0
3 -6 13 12.06 11.49 0
3 8 0 44.72 6.95 0
3 8 20 1.08 6.41 0
3 9 19 39.02 6.59 0
3 10 4 125.04 5.79 0
3 10 18 49.21 6.13 0
3 11 7 6.61 5.30 0
3 11 16 123.97 6.18 0
4 -10 0 39.10 6.07 0
4 -10 1 5.97 5.76 0
4 -10 2 50.62 6.19 0
4 -10 3 6.83 5.95 0
4 -9 -4 5.26 4.04 0
4 -9 8 4.11 7.69 0
4 -8 -6 169.63 6.38 0
4 -7 -7 91.56 4.42 0
4 -6 -8 187.77 6.38 0
4 -3 -9 184.17 6.24 0
4 -2 -9 317.40 6.99 0
4 10 21 7.01 6.82 0
4 11 3 49.17 5.44 0
4 11 20 48.14 6.76 0
4 12 19 17.56 4.41 0
4 13 9 59.58 4.20 0
4 13 10 79.98 5.81 0
4 13 15 55.20 5.59 0
4 13 16 10.27 4.10 0
5 -10 -3 22.57 5.87 0
5 -9 -6 88.47 6.04 0
5 -6 -9 42.69 5.84 0
5 -3 -10 216.18 6.76 0
5 -2 -10 202.21 6.92 0
5 5 -7 61.63 12.88 0
5 7 -5 180.35 12.04 0
5 13 5 2.89 5.34 0
5 14 8 39.84 5.49 0
5 14 18 8.67 6.47 0
6 -10 -5 34.77 5.95 0
6 -9 -7 53.61 5.92 0
6 -8 -8 32.11 4.13 0
6 -7 -9 8.73 4.12 0
6 15 8 33.32 5.95 0
7 -10 -5 8.18 4.14 0
7 -5 -11 15.01 6.28 0
7 5 -9 15.31 8.46 0
7 16 8 4.89 5.98 0
8 -9 -8 -3.96 6.07 0
8 -8 -9 12.60 4.56 0
8 -7 -10 12.48 6.41 0
8 -2 -12 22.50 6.74 0
8 6 -9 10.05 8.97 0
8 11 -4 37.06 8.81 0
8 16 5 23.05 6.38 0
9 -6 -11 9.74 6.74 0
9 -4 -12 5.42 6.76 0
9 -3 -12 -1.75 4.81 0
9 1 -12 10.82 8.66 0
9 15 1 1.44 6.44 0
10 2 -12 4.17 7.05 0
0 -5 2 4.58 6.17 0
0 -5 3 568.99 10.03 0
0 -5 4 122.79 7.97 0
0 -2 10 258.99 12.03 0
0 3 11 3.68 5.22 0
0 4 6 5.45 5.21 0
0 4 7 1419.55 11.00 0
0 4 8 272.60 6.54 0
0 4 9 636.51 7.99 0
1 -7 0 528.24 8.00 0
1 -7 5 195.68 8.36 0
1 -3 -4 464.75 8.61 0
1 -2 -4 670.23 10.36 0
1 0 15 9.00 7.31 0
1 5 15 143.35 6.32 0
1 6 14 74.78 5.62 0
1 7 7 -1.32 4.91 0
1 7 12 20.09 5.13 0
2 -8 -2 21.80 5.39 0
2 -8 6 86.35 6.33 0
2 -7 -4 200.39 6.39 0
2 -7 9 53.36 7.73 0
2 -6 -5 6.23 3.75 0
2 -4 -6 932.23 8.66 0
2 -1 -6 254.55 7.32 0
2 2 18 28.16 8.03 0
2 6 18 23.56 6.29 0
2 7 17 108.60 6.15 0
2 8 16 9.02 5.44 0
2 9 6 25.69 3.81 0
2 9 14 225.43 6.26 0
3 -9 -3 6.35 5.52 0
3 -9 6 32.94 7.54 0
3 -8 -5 215.24 6.51 0
3 -8 9 0.23 7.52 0
3 -7 -6 51.36 3.92 0
3 -6 -7 332.44 6.69 0
3 -3 -8 151.28 6.40 0
3 0 19 11.19 9.03 0
3 2 20 0.85 8.77 0
3 7 20 0.57 6.56 0
3 9 2 25.29 5.05 0
3 10 17 0.07 5.74 0
3 11 8 139.11 5.74 0
3 11 15 58.86 5.69 0
4 -10 -2 20.96 5.86 0
4 -10 -1 85.53 4.64 0
4 -10 4 19.80 6.23 0
4 -9 -5 60.76 5.83 0
4 -4 -9 225.76 6.66 0
4 -1 -9 526.52 8.54 0
4 10 1 38.34 5.17 0
4 12 6 7.93 5.16 0
4 12 18 12.18 4.43 0
4 13 11 -0.16 3.83 0
4 13 12 126.81 5.89 0
4 13 13 17.77 5.56 0
4 13 14 62.42 4.25 0
5 -10 -4 76.86 6.20 0
5 -8 -8 16.75 5.70 0
5 -4 -10 135.64 6.62 0
5 -1 -10 456.12 8.10 0
5 2 -9 19.97 7.11 0
5 10 -1 185.75 7.72 0
5 14 9 97.96 5.84 0
5 14 10 16.74 5.62 0
5 14 16 28.77 6.10 0
5 14 17 3.82 4.24 0
6 -11 -2 4.56 5.97 0
6 -11 -1 4.54 6.19 0
6 -6 -10 53.18 4.61 0
6 -4 -11 35.16 6.08 0
6 -3 -11 89.20 6.72 0
6 -2 -11 62.17 6.25 0
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11 1 6 18.82 6.52 0
11 1 7 18.73 6.93 0
11 1 8 1.48 6.48 0
11 1 9 19.09 6.91 0
11 1 10 5.00 6.68 0
12 -3 -3 4.42 7.19 0
12 -1 1 32.14 6.76 0
12 0 4 6.37 4.65 0
12 0 5 9.76 6.83 0
-12 -12 -4 15.46 6.80 0
-12 -11 1 7.83 6.86 0
-12 -11 2 2.40 6.93 0
-11 -14 -11 8.61 7.25 0
-11 -12 -8 10.56 6.58 0
-11 -11 -6 15.47 6.33 0
-11 -10 -3 57.05 6.35 0
-10 -14 -13 8.82 7.33 0
-10 -9 -4 90.57 4.96 0
-10 -8 0 26.27 4.33 0
-10 -8 6 40.47 4.86 0
-10 -8 7 6.35 6.42 0
-9 -8 -5 104.11 6.39 0
-9 -7 9 19.77 6.76 0
-8 -7 -5 2.47 5.72 0
-8 -7 12 -4.48 5.17 0
-8 -6 -2 150.45 6.34 0
-8 -6 10 9.40 4.73 0
-7 -6 -5 280.19 7.15 0
-7 -6 13 1.41 5.37 0
-7 -5 -2 133.21 6.20 0
-7 -5 11 3.32 4.59 0
-7 -4 4 264.69 6.71 0
-7 -4 5 475.60 7.52 0
-7 -4 6 4.57 5.73 0
-6 -7 -9 191.53 7.42 0
-6 -6 -7 13.07 5.80 0
-6 -5 14 14.59 7.17 0
-6 -4 12 17.64 6.28 0
-6 -3 5 3.59 5.38 0
-6 -3 6 309.42 7.16 0
-6 -3 7 17.65 5.67 0
-5 -4 -4 369.48 7.93 0
-5 -3 12 39.20 6.33 0
-4 -2 12 51.78 6.23 0
-3 -1 11 229.36 6.85 0
-2 -2 16 0.73 6.74 0
-2 -1 14 147.73 6.96 0
-2 0 6 75.86 6.16 0
-2 0 7 814.75 10.16 0
-2 0 8 28.72 5.25 0
-2 0 9 414.65 8.18 0
0 1 10 518.16 9.80 0
1 -9 -16 10.30 6.95 0
1 -8 -15 238.55 8.20 0
1 -1 -4 635.93 11.64 0
2 -9 -16 57.83 7.63 0
2 -7 -14 259.31 7.93 0
2 0 -2 386.30 9.52 0
3 -9 -16 12.27 7.38 0
3 -8 -15 44.06 7.14 0
3 -7 -14 38.99 6.62 0
3 -2 -7 117.71 6.70 0
3 -1 -5 777.18 10.10 0
4 -7 -14 4.29 4.59 0
4 -2 -7 52.51 5.87 0
4 1 0 110.41 5.17 0
5 -4 -10 129.45 7.09 0
5 -2 -7 533.16 8.11 0
5 0 -3 586.08 7.19 0
5 1 0 999.65 10.36 0
6 -5 -11 64.02 6.78 0
6 -1 -5 80.43 4.68 0
6 1 0 101.07 5.96 0
6 2 4 465.67 8.25 0
7 -3 -8 16.24 6.18 0
8 -7 -12 18.01 7.80 0
8 -6 -11 -2.08 7.26 0
8 -5 -10 67.54 7.09 0
8 -1 -4 5.13 5.76 0
8 1 1 15.31 5.61 0
8 2 6 39.19 5.72 0
9 -4 -8 41.43 6.97 0
9 -2 -5 35.25 6.14 0
9 -1 -3 86.94 6.00 0
9 0 -1 156.41 5.31 0
9 1 2 15.17 5.76 0
10 -5 -8 -0.31 7.37 0
10 -4 -7 21.20 6.79 0
10 -2 -4 19.42 6.12 0
10 -1 -2 59.32 6.24 0
10 1 4 0.09 6.12 0
11 -3 -4 2.32 6.55 0
11 0 2 31.59 4.61 0
12 -2 -1 5.82 4.67 0
12 -1 2 0.21 6.66 0
12 0 6 15.07 4.90 0
12 0 7 -1.08 6.82 0
12 0 8 15.61 7.19 0
12 0 9 11.84 7.05 0
-12 -11 0 9.61 4.84 0
-10 -8 -1 7.34 4.44 0
-9 -7 -2 40.79 4.10 0
-8 -5 4 137.73 4.86 0
-8 -5 5 31.87 4.21 0
-8 -5 6 34.58 4.41 0
-7 -4 3 170.61 4.82 0
-7 -4 7 196.28 5.31 0
-6 -3 4 504.07 6.57 0
-3 -2 -2 1802.76 16.77 0
4 -1 -5 40.04 4.34 0
5 -1 -5 424.93 6.40 0
6 -8 -14 6.48 5.18 0
9 -6 -10 8.34 5.39 0
9 -5 -9 11.91 4.87 0
11 -1 0 15.63 4.56 0
11 0 3 4.14 4.45 0
12 -3 -2 5.89 4.97 0
;
_shelx_hkl_checksum 32430
_shelx_res_file
;
ip2-2429n.res created by SHELXL-2014/7
TITL FG8 = ip2-2429 in P-1: [Pb(C16H10N4O2)2(NO3)(C2N3)]2
CELL 0.71073 10.5123 12.2682 15.6379 66.834 80.260 67.514
ZERR 1 0.0008 0.0008 0.0010 0.005 0.006 0.005
LATT 1
SFAC C H N O Pb
UNIT 68 40 24 14 2
TEMP -73
SIZE 0.21 0.21 0.33
OMIT -2 54
L.S. 6
PLAN -10
BOND $H
LIST 6
FMAP 2
ACTA
WGHT 0.035700
EXTI 0.001997
FVAR 0.27404
PB1 5 0.196475 0.521103 0.701642 11.00000 0.04834 0.03619 =
0.04197 -0.01954 -0.00107 -0.01221
O1 4 0.740319 -0.109852 0.956210 11.00000 0.04648 0.04241 =
0.04971 -0.02107 -0.00819 -0.00948
O2 4 0.450994 -0.106717 0.766528 11.00000 0.06989 0.04943 =
0.04559 -0.02261 0.00089 -0.03081
O3 4 -0.255675 1.200704 0.636494 11.00000 0.07499 0.06341 =
0.09135 -0.01757 -0.01730 -0.01783
O4 4 0.121791 1.049655 0.801378 11.00000 0.06251 0.05039 =
0.06965 -0.02840 -0.00577 -0.02251
O5 4 0.036754 0.379090 0.751083 11.00000 0.13014 0.11259 =
0.15108 -0.09969 0.07144 -0.07640
O6 4 -0.019233 0.507754 0.817705 11.00000 0.13899 0.16751 =
0.17687 -0.14555 0.08884 -0.10133
O7 4 -0.109455 0.364138 0.864655 11.00000 0.10870 0.12627 =
0.08545 -0.04130 0.03100 -0.06942
N1 3 0.312629 0.434102 0.870102 11.00000 0.05838 0.03453 =
0.04512 -0.01901 0.00090 -0.01104
N2 3 0.374221 0.274382 0.777962 11.00000 0.05084 0.04140 =
0.04743 -0.02304 -0.00809 -0.00852
N3 3 0.392377 0.193664 0.734866 11.00000 0.05116 0.04372 =
0.04968 -0.02542 -0.00793 -0.00928
N4 3 0.540887 0.117738 0.890639 11.00000 0.04191 0.03617 =
0.03955 -0.01750 0.00110 -0.01591
N5 3 0.021274 0.698542 0.562372 11.00000 0.06790 0.05184 =
0.05222 -0.02390 -0.01360 -0.02111
N6 3 0.070414 0.763513 0.697355 11.00000 0.04862 0.04212 =
0.04627 -0.02059 -0.00984 -0.01127
N7 3 0.107461 0.796935 0.758602 11.00000 0.04648 0.03958 =
0.04333 -0.01872 -0.00818 -0.00968
N8 3 -0.094702 0.968368 0.633338 11.00000 0.03853 0.03993 =
0.04088 -0.01230 -0.00392 -0.01299
C1 1 0.277393 0.512441 0.916731 11.00000 0.06919 0.03521 =
0.05278 -0.02219 -0.00399 -0.01004
AFIX 43
H1 2 0.208591 0.593338 0.891670 11.00000 -1.20000
AFIX 0
C2 1 0.335743 0.481983 0.999443 11.00000 0.07312 0.04219 =
0.05007 -0.02445 0.00072 -0.02236
AFIX 43
H2 2 0.305560 0.539361 1.031589 11.00000 -1.20000
AFIX 0
C3 1 0.439006 0.366218 1.034455 11.00000 0.06619 0.04708 =
0.04188 -0.01996 -0.00107 -0.02464
AFIX 43
H3 2 0.482983 0.343632 1.090343 11.00000 -1.20000
AFIX 0
C4 1 0.477735 0.283458 0.987243 11.00000 0.04849 0.03933 =
0.04326 -0.01734 0.00012 -0.01822
AFIX 43
H4 2 0.548646 0.203331 1.009951 11.00000 -1.20000
AFIX 0
C5 1 0.410593 0.320162 0.905867 11.00000 0.04200 0.03736 =
0.04001 -0.01717 0.00331 -0.01804
C6 1 0.442998 0.232669 0.855204 11.00000 0.03645 0.03538 =
0.03955 -0.01662 0.00350 -0.01332
C7 1 0.482998 0.077594 0.767930 11.00000 0.04135 0.03640 =
0.04020 -0.01580 -0.00059 -0.01386
C8 1 0.565478 0.038858 0.844947 11.00000 0.04025 0.03651 =
0.03606 -0.01629 0.00360 -0.01679
C9 1 0.678097 -0.081473 0.876249 11.00000 0.03722 0.03519 =
0.03731 -0.01442 0.00123 -0.01484
C10 1 0.740568 -0.175931 0.841917 11.00000 0.04369 0.03956 =
0.04912 -0.02410 0.00644 -0.01406
AFIX 43
H10 2 0.717361 -0.179629 0.787230 11.00000 -1.20000
AFIX 0
C11 1 0.847632 -0.268129 0.904248 11.00000 0.04248 0.03772 =
0.06203 -0.02052 0.00680 -0.01250
AFIX 43
H11 2 0.910233 -0.345524 0.899370 11.00000 -1.20000
AFIX 0
C12 1 0.842580 -0.224375 0.970637 11.00000 0.04175 0.03971 =
0.05864 -0.01203 -0.00981 -0.00727
AFIX 43
H12 2 0.902776 -0.267565 1.021795 11.00000 -1.20000
AFIX 0
C13 1 0.493064 -0.005213 0.717933 11.00000 0.04525 0.03668 =
0.04245 -0.01635 -0.00595 -0.01211
C14 1 0.538790 -0.004478 0.632604 11.00000 0.07291 0.04980 =
0.03931 -0.01899 -0.00137 -0.02447
AFIX 43
H14 2 0.573102 0.055908 0.585850 11.00000 -1.20000
AFIX 0
C15 1 0.525851 -0.112376 0.625657 11.00000 0.08560 0.05403 =
0.05019 -0.02893 -0.00935 -0.01957
AFIX 43
H15 2 0.549984 -0.138114 0.573434 11.00000 -1.20000
AFIX 0
C16 1 0.472961 -0.170046 0.707349 11.00000 0.08324 0.04720 =
0.05509 -0.02547 -0.01006 -0.02627
AFIX 43
H16 2 0.453307 -0.244973 0.722232 11.00000 -1.20000
AFIX 0
C17 1 -0.003104 0.665608 0.495814 11.00000 0.08376 0.05972 =
0.06372 -0.03201 -0.01670 -0.02211
AFIX 43
H17 2 0.048866 0.583112 0.495538 11.00000 -1.20000
AFIX 0
C18 1 -0.099452 0.745372 0.428202 11.00000 0.07196 0.07518 =
0.05113 -0.02716 -0.00802 -0.03565
AFIX 43
H18 2 -0.114278 0.717946 0.382970 11.00000 -1.20000
AFIX 0
C19 1 -0.174004 0.865668 0.427267 11.00000 0.05314 0.08061 =
0.04130 -0.02003 -0.00667 -0.02650
AFIX 43
H19 2 -0.240669 0.922793 0.381012 11.00000 -1.20000
AFIX 0
C20 1 -0.150540 0.902452 0.494771 11.00000 0.04582 0.05972 =
0.04445 -0.01962 -0.00290 -0.01649
AFIX 43
H20 2 -0.200572 0.985072 0.495407 11.00000 -1.20000
AFIX 0
C21 1 -0.053146 0.816687 0.560920 11.00000 0.04327 0.05021 =
0.04119 -0.01956 0.00093 -0.02156
C22 1 -0.023444 0.851845 0.634453 11.00000 0.03873 0.03941 =
0.03962 -0.01495 -0.00305 -0.01411
C23 1 0.045541 0.913500 0.759042 11.00000 0.03903 0.03387 =
0.03998 -0.01549 0.00072 -0.01202
C24 1 -0.065932 1.001225 0.698052 11.00000 0.03931 0.03440 =
0.03977 -0.01288 0.00031 -0.01453
C25 1 -0.155987 1.122523 0.701364 11.00000 0.03822 0.03470 =
0.05138 -0.01151 -0.00254 -0.00992
C26 1 -0.160797 1.170765 0.765652 11.00000 0.03807 0.06345 =
0.06151 -0.04085 0.00417 -0.01566
AFIX 43
H26 2 -0.104854 1.133314 0.818652 11.00000 -1.20000
AFIX 0
C27 1 -0.268618 1.290899 0.736828 11.00000 0.07442 0.07972 =
0.15142 -0.08336 0.04626 -0.04309
AFIX 43
H27 2 -0.295067 1.350890 0.766486 11.00000 -1.20000
AFIX 0
C28 1 -0.324496 1.305083 0.664039 11.00000 0.05925 0.03183 =
0.13803 -0.00983 0.00557 -0.00376
AFIX 43
H28 2 -0.401220 1.376003 0.633467 11.00000 -1.20000
AFIX 0
C29 1 0.097229 0.938261 0.828351 11.00000 0.04155 0.03637 =
0.04109 -0.01674 -0.00213 -0.01253
C30 1 0.131652 0.867759 0.917959 11.00000 0.04582 0.06111 =
0.05010 -0.00219 0.00080 -0.01172
AFIX 43
H30 2 0.129692 0.785340 0.953682 11.00000 -1.20000
AFIX 0
C31 1 0.173312 0.950609 0.946971 11.00000 0.05020 0.07889 =
0.05127 -0.03704 -0.00380 -0.01816
AFIX 43
H31 2 0.200089 0.931762 1.007700 11.00000 -1.20000
AFIX 0
C32 1 0.167247 1.051861 0.876609 11.00000 0.06238 0.07876 =
0.06994 -0.04970 0.00290 -0.02853
AFIX 43
H32 2 0.191186 1.118825 0.877139 11.00000 -1.20000
AFIX 0
N9 3 -0.033996 0.418229 0.811030 11.00000 0.07130 0.06727 =
0.05677 -0.03117 0.00677 -0.03082
N10 3 0.295791 0.449074 0.558753 11.00000 0.10437 0.06567 =
0.05513 -0.02625 0.00500 -0.01532
N11 3 0.471044 0.314853 0.482081 11.00000 0.10338 0.04871 =
0.07393 -0.02772 0.01896 -0.02926
N12 3 0.601540 0.390911 0.341504 11.00000 0.08961 0.09125 =
0.09784 -0.05744 0.02979 -0.04861
C33 1 0.378226 0.390229 0.520267 11.00000 0.08752 0.04722 =
0.04725 -0.01975 -0.00231 -0.02269
C34 1 0.540144 0.358939 0.409345 11.00000 0.07170 0.05456 =
0.06954 -0.03855 0.00647 -0.02598
HKLF 4
REM FG8 = ip2-2429 in P-1: [Pb(C16H10N4O2)2(NO3)(C2N3)]2
REM R1 = 0.0259 for 6299 Fo > 4sig(Fo) and 0.0345 for all 7484 data
REM 488 parameters refined using 0 restraints
END
WGHT 0.0358 0.0000
REM Highest difference peak 0.847, deepest hole -0.767, 1-sigma level 0.082
Q1 1 0.1858 0.8564 0.9654 11.00000 0.05 0.85
Q2 1 0.1395 0.8034 0.9079 11.00000 0.05 0.83
Q3 1 -0.1636 1.1390 0.7971 11.00000 0.05 0.57
Q4 1 -0.1934 1.2134 0.7451 11.00000 0.05 0.54
Q5 1 -0.1354 1.1667 0.7381 11.00000 0.05 0.54
Q6 1 0.1410 0.6416 0.7126 11.00000 0.05 0.51
Q7 1 -0.1196 1.1528 0.7744 11.00000 0.05 0.51
Q8 1 0.2634 0.5377 0.6717 11.00000 0.05 0.45
Q9 1 0.1423 0.6444 0.6551 11.00000 0.05 0.45
Q10 1 0.0007 0.4581 0.8438 11.00000 0.05 0.42
;
_shelx_res_checksum 26639
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Pb Pb1 0.19647(2) 0.52110(2) 0.70164(2) 0.04116(5) Uani d 1
O O1 0.7403(2) -0.1099(2) 0.95621(18) 0.0457(6) Uani d 1
O O2 0.4510(3) -0.1067(2) 0.76653(18) 0.0502(6) Uani d 1
O O3 -0.2557(4) 1.2007(3) 0.6365(3) 0.0800(10) Uani d 1
O O4 0.1218(3) 1.0497(2) 0.8014(2) 0.0571(7) Uani d 1
O O5 0.0368(5) 0.3791(4) 0.7511(4) 0.1130(16) Uani d 1
O O6 -0.0192(5) 0.5078(5) 0.8177(4) 0.130(2) Uani d 1
O O7 -0.1095(5) 0.3641(4) 0.8647(3) 0.1011(13) Uani d 1
N N1 0.3126(3) 0.4341(3) 0.8701(2) 0.0464(7) Uani d 1
N N2 0.3742(3) 0.2744(3) 0.7780(2) 0.0457(7) Uani d 1
N N3 0.3924(3) 0.1937(3) 0.7349(2) 0.0468(7) Uani d 1
N N4 0.5409(3) 0.1177(2) 0.89064(19) 0.0375(6) Uani d 1
N N5 0.0213(4) 0.6985(3) 0.5624(2) 0.0539(8) Uani d 1
N N6 0.0704(3) 0.7635(3) 0.6974(2) 0.0444(7) Uani d 1
N N7 0.1075(3) 0.7969(3) 0.7586(2) 0.0426(6) Uani d 1
N N8 -0.0947(3) 0.9684(3) 0.6333(2) 0.0404(6) Uani d 1
C C1 0.2774(4) 0.5124(3) 0.9167(3) 0.0526(9) Uani d 1
H H1 0.2086 0.5933 0.8917 0.063 Uiso calc 1
C C2 0.3357(4) 0.4820(3) 0.9994(3) 0.0521(9) Uani d 1
H H2 0.3056 0.5394 1.0316 0.063 Uiso calc 1
C C3 0.4390(4) 0.3662(3) 1.0345(3) 0.0489(8) Uani d 1
H H3 0.4830 0.3436 1.0903 0.059 Uiso calc 1
C C4 0.4777(4) 0.2835(3) 0.9872(2) 0.0421(7) Uani d 1
H H4 0.5486 0.2033 1.0100 0.051 Uiso calc 1
C C5 0.4106(3) 0.3202(3) 0.9059(2) 0.0379(7) Uani d 1
C C6 0.4430(3) 0.2327(3) 0.8552(2) 0.0364(7) Uani d 1
C C7 0.4830(3) 0.0776(3) 0.7679(2) 0.0386(7) Uani d 1
C C8 0.5655(3) 0.0389(3) 0.8449(2) 0.0360(7) Uani d 1
C C9 0.6781(3) -0.0815(3) 0.8762(2) 0.0357(7) Uani d 1
C C10 0.7406(4) -0.1759(3) 0.8419(3) 0.0426(8) Uani d 1
H H10 0.7174 -0.1796 0.7872 0.051 Uiso calc 1
C C11 0.8476(4) -0.2681(3) 0.9042(3) 0.0481(8) Uani d 1
H H11 0.9102 -0.3455 0.8994 0.058 Uiso calc 1
C C12 0.8426(4) -0.2244(3) 0.9706(3) 0.0497(9) Uani d 1
H H12 0.9028 -0.2676 1.0218 0.060 Uiso calc 1
C C13 0.4931(4) -0.0052(3) 0.7179(2) 0.0408(7) Uani d 1
C C14 0.5388(4) -0.0045(4) 0.6326(3) 0.0520(9) Uani d 1
H H14 0.5731 0.0559 0.5859 0.062 Uiso calc 1
C C15 0.5259(5) -0.1124(4) 0.6257(3) 0.0604(11) Uani d 1
H H15 0.5500 -0.1381 0.5734 0.072 Uiso calc 1
C C16 0.4730(5) -0.1700(4) 0.7073(3) 0.0573(10) Uani d 1
H H16 0.4533 -0.2450 0.7222 0.069 Uiso calc 1
C C17 -0.0031(5) 0.6656(4) 0.4958(3) 0.0648(11) Uani d 1
H H17 0.0489 0.5831 0.4955 0.078 Uiso calc 1
C C18 -0.0995(5) 0.7454(4) 0.4282(3) 0.0606(11) Uani d 1
H H18 -0.1143 0.7179 0.3830 0.073 Uiso calc 1
C C19 -0.1740(4) 0.8657(4) 0.4273(3) 0.0572(10) Uani d 1
H H19 -0.2407 0.9228 0.3810 0.069 Uiso calc 1
C C20 -0.1505(4) 0.9025(4) 0.4948(3) 0.0501(9) Uani d 1
H H20 -0.2006 0.9851 0.4954 0.060 Uiso calc 1
C C21 -0.0531(4) 0.8167(3) 0.5609(2) 0.0424(8) Uani d 1
C C22 -0.0234(3) 0.8518(3) 0.6345(2) 0.0386(7) Uani d 1
C C23 0.0455(3) 0.9135(3) 0.7590(2) 0.0373(7) Uani d 1
C C24 -0.0659(3) 1.0012(3) 0.6981(2) 0.0376(7) Uani d 1
C C25 -0.1560(4) 1.1225(3) 0.7014(3) 0.0435(8) Uani d 1
C C26 -0.1608(4) 1.1708(4) 0.7657(3) 0.0496(9) Uani d 1
H H26 -0.1049 1.1333 0.8187 0.060 Uiso calc 1
C C27 -0.2686(6) 1.2909(5) 0.7368(5) 0.0893(19) Uani d 1
H H27 -0.2951 1.3509 0.7665 0.107 Uiso calc 1
C C28 -0.3245(5) 1.3051(4) 0.6640(5) 0.0882(19) Uani d 1
H H28 -0.4012 1.3760 0.6335 0.106 Uiso calc 1
C C29 0.0972(3) 0.9383(3) 0.8284(2) 0.0389(7) Uani d 1
C C30 0.1317(4) 0.8678(4) 0.9180(3) 0.0607(11) Uani d 1
H H30 0.1297 0.7853 0.9537 0.073 Uiso calc 1
C C31 0.1733(4) 0.9506(4) 0.9470(3) 0.0567(10) Uani d 1
H H31 0.2001 0.9318 1.0077 0.068 Uiso calc 1
C C32 0.1672(4) 1.0519(5) 0.8766(3) 0.0621(11) Uani d 1
H H32 0.1912 1.1188 0.8771 0.075 Uiso calc 1
N N9 -0.0340(4) 0.4182(4) 0.8110(3) 0.0612(9) Uani d 1
N N10 0.2958(5) 0.4491(4) 0.5588(3) 0.0791(12) Uani d 1
N N11 0.4710(5) 0.3149(3) 0.4821(3) 0.0754(11) Uani d 1
N N12 0.6015(5) 0.3909(4) 0.3415(4) 0.0839(13) Uani d 1
C C33 0.3782(5) 0.3902(4) 0.5203(3) 0.0599(10) Uani d 1
C C34 0.5401(5) 0.3589(4) 0.4093(3) 0.0597(11) Uani d 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 0.04834(8) 0.03619(7) 0.04197(8) -0.01221(5) -0.00107(5) -0.01954(5)
O1 0.0465(13) 0.0424(12) 0.0497(15) -0.0095(10) -0.0082(11) -0.0211(11)
O2 0.0699(17) 0.0494(14) 0.0456(15) -0.0308(13) 0.0009(12) -0.0226(12)
O3 0.075(2) 0.0634(19) 0.091(3) -0.0178(17) -0.0173(19) -0.0176(18)
O4 0.0625(17) 0.0504(14) 0.0697(19) -0.0225(13) -0.0058(14) -0.0284(14)
O5 0.130(3) 0.113(3) 0.151(4) -0.076(3) 0.071(3) -0.100(3)
O6 0.139(4) 0.168(4) 0.177(5) -0.101(4) 0.089(4) -0.146(4)
O7 0.109(3) 0.126(3) 0.085(3) -0.069(3) 0.031(2) -0.041(3)
N1 0.0584(18) 0.0345(14) 0.0451(17) -0.0110(13) 0.0009(14) -0.0190(13)
N2 0.0508(17) 0.0414(15) 0.0474(18) -0.0085(13) -0.0081(14) -0.0230(14)
N3 0.0512(17) 0.0437(15) 0.0497(18) -0.0093(13) -0.0079(14) -0.0254(14)
N4 0.0419(15) 0.0362(13) 0.0395(16) -0.0159(11) 0.0011(12) -0.0175(12)
N5 0.068(2) 0.0518(17) 0.0522(19) -0.0211(16) -0.0136(16) -0.0239(15)
N6 0.0486(17) 0.0421(15) 0.0463(17) -0.0113(13) -0.0098(13) -0.0206(13)
N7 0.0465(16) 0.0396(14) 0.0433(17) -0.0097(12) -0.0082(13) -0.0187(13)
N8 0.0385(15) 0.0399(14) 0.0409(16) -0.0130(12) -0.0039(12) -0.0123(13)
C1 0.069(2) 0.0352(17) 0.053(2) -0.0100(16) -0.0040(19) -0.0222(16)
C2 0.073(3) 0.0422(18) 0.050(2) -0.0224(18) 0.0007(19) -0.0245(17)
C3 0.066(2) 0.0471(19) 0.042(2) -0.0246(17) -0.0011(17) -0.0200(16)
C4 0.0485(19) 0.0393(17) 0.043(2) -0.0182(15) 0.0001(15) -0.0173(15)
C5 0.0420(17) 0.0374(16) 0.0400(18) -0.0180(14) 0.0033(14) -0.0172(14)
C6 0.0364(17) 0.0354(15) 0.0395(18) -0.0133(13) 0.0035(14) -0.0166(14)
C7 0.0414(18) 0.0364(16) 0.0402(19) -0.0139(14) -0.0006(14) -0.0158(15)
C8 0.0402(17) 0.0365(16) 0.0361(18) -0.0168(13) 0.0036(14) -0.0163(14)
C9 0.0372(16) 0.0352(15) 0.0373(18) -0.0148(13) 0.0012(13) -0.0144(14)
C10 0.0437(18) 0.0396(17) 0.049(2) -0.0141(14) 0.0064(15) -0.0241(16)
C11 0.0425(19) 0.0377(17) 0.062(2) -0.0125(15) 0.0068(17) -0.0205(17)
C12 0.0417(19) 0.0397(18) 0.059(2) -0.0073(15) -0.0098(17) -0.0120(17)
C13 0.0453(19) 0.0367(16) 0.0425(19) -0.0121(14) -0.0060(15) -0.0163(15)
C14 0.073(3) 0.050(2) 0.039(2) -0.0245(19) -0.0014(18) -0.0190(17)
C15 0.086(3) 0.054(2) 0.050(2) -0.020(2) -0.009(2) -0.029(2)
C16 0.083(3) 0.047(2) 0.055(2) -0.026(2) -0.010(2) -0.0255(19)
C17 0.084(3) 0.060(2) 0.064(3) -0.022(2) -0.017(2) -0.032(2)
C18 0.072(3) 0.075(3) 0.051(2) -0.036(2) -0.008(2) -0.027(2)
C19 0.053(2) 0.081(3) 0.041(2) -0.026(2) -0.0067(17) -0.020(2)
C20 0.046(2) 0.060(2) 0.044(2) -0.0165(17) -0.0029(16) -0.0196(18)
C21 0.0433(19) 0.0502(19) 0.0412(19) -0.0216(16) 0.0009(15) -0.0196(16)
C22 0.0387(17) 0.0394(16) 0.0396(18) -0.0141(14) -0.0030(14) -0.0149(14)
C23 0.0390(17) 0.0339(15) 0.0400(18) -0.0120(13) 0.0007(14) -0.0155(14)
C24 0.0393(17) 0.0344(15) 0.0398(18) -0.0145(13) 0.0003(14) -0.0129(14)
C25 0.0382(18) 0.0347(16) 0.051(2) -0.0099(14) -0.0025(15) -0.0115(15)
C26 0.0381(18) 0.063(2) 0.062(2) -0.0157(16) 0.0042(16) -0.041(2)
C27 0.074(3) 0.080(3) 0.151(6) -0.043(3) 0.046(4) -0.083(4)
C28 0.059(3) 0.032(2) 0.138(6) -0.0038(19) 0.006(3) -0.010(3)
C29 0.0415(18) 0.0364(16) 0.0411(19) -0.0125(14) -0.0021(14) -0.0167(15)
C30 0.046(2) 0.061(2) 0.050(2) -0.0117(18) 0.0008(18) -0.002(2)
C31 0.050(2) 0.079(3) 0.051(2) -0.018(2) -0.0038(18) -0.037(2)
C32 0.062(3) 0.079(3) 0.070(3) -0.029(2) 0.003(2) -0.050(3)
N9 0.071(2) 0.067(2) 0.057(2) -0.0308(19) 0.0068(18) -0.0312(19)
N10 0.104(3) 0.066(2) 0.055(2) -0.015(2) 0.005(2) -0.026(2)
N11 0.103(3) 0.0487(19) 0.074(3) -0.029(2) 0.019(2) -0.0277(19)
N12 0.090(3) 0.091(3) 0.098(3) -0.049(3) 0.030(3) -0.057(3)
C33 0.088(3) 0.047(2) 0.047(2) -0.023(2) -0.002(2) -0.0198(19)
C34 0.072(3) 0.055(2) 0.070(3) -0.026(2) 0.006(2) -0.039(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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N12 Pb1 N10 2_666 . 82.91(14)
N12 Pb1 O6 2_666 . 142.91(12)
N10 Pb1 O6 . . 134.11(14)
N12 Pb1 O5 2_666 . 166.63(14)
N10 Pb1 O5 . . 90.29(13)
O6 Pb1 O5 . . 45.60(11)
N12 Pb1 N5 2_666 . 99.36(14)
N10 Pb1 N5 . . 76.57(12)
O6 Pb1 N5 . . 89.53(16)
O5 Pb1 N5 . . 90.17(14)
N12 Pb1 N1 2_666 . 77.78(13)
N10 Pb1 N1 . . 128.61(12)
O6 Pb1 N1 . . 78.36(15)
O5 Pb1 N1 . . 97.86(14)
N5 Pb1 N1 . . 153.18(9)
N12 Pb1 N6 2_666 . 76.89(12)
N10 Pb1 N6 . . 127.02(11)
O6 Pb1 N6 . . 76.95(12)
O5 Pb1 N6 . . 116.24(11)
N5 Pb1 N6 . . 59.63(9)
N1 Pb1 N6 . . 94.10(8)
N12 Pb1 N2 2_666 . 92.11(13)
N10 Pb1 N2 . . 75.13(11)
O6 Pb1 N2 . . 99.26(15)
O5 Pb1 N2 . . 74.98(13)
N5 Pb1 N2 . . 147.80(9)
N1 Pb1 N2 . . 58.74(8)
N6 Pb1 N2 . . 152.54(9)
C12 O1 C9 . . 105.9(3)
C16 O2 C13 . . 105.6(3)
C25 O3 C28 . . 104.2(4)
C32 O4 C29 . . 107.5(3)
N9 O5 Pb1 . . 98.1(3)
N9 O6 Pb1 . . 99.2(3)
C1 N1 C5 . . 117.9(3)
C1 N1 Pb1 . . 118.2(2)
C5 N1 Pb1 . . 123.8(2)
C6 N2 N3 . . 118.7(3)
C6 N2 Pb1 . . 122.7(2)
N3 N2 Pb1 . . 118.6(2)
C7 N3 N2 . . 119.0(3)
C8 N4 C6 . . 116.2(3)
C17 N5 C21 . . 117.3(3)
C17 N5 Pb1 . . 119.4(3)
C21 N5 Pb1 . . 123.0(2)
C22 N6 N7 . . 118.3(3)
C22 N6 Pb1 . . 122.8(2)
N7 N6 Pb1 . . 118.8(2)
C23 N7 N6 . . 119.9(3)
C22 N8 C24 . . 117.3(3)
N1 C1 C2 . . 123.4(3)
N1 C1 H1 . . 118.3
C2 C1 H1 . . 118.3
C1 C2 C3 . . 118.5(3)
C1 C2 H2 . . 120.8
C3 C2 H2 . . 120.8
C2 C3 C4 . . 119.2(4)
C2 C3 H3 . . 120.4
C4 C3 H3 . . 120.4
C3 C4 C5 . . 118.5(3)
C3 C4 H4 . . 120.7
C5 C4 H4 . . 120.7
N1 C5 C4 . . 122.5(3)
N1 C5 C6 . . 116.8(3)
C4 C5 C6 . . 120.7(3)
N2 C6 N4 . . 125.4(3)
N2 C6 C5 . . 117.3(3)
N4 C6 C5 . . 117.3(3)
N3 C7 C8 . . 121.4(3)
N3 C7 C13 . . 115.2(3)
C8 C7 C13 . . 123.4(3)
N4 C8 C7 . . 118.9(3)
N4 C8 C9 . . 117.7(3)
C7 C8 C9 . . 123.4(3)
C10 C9 O1 . . 109.9(3)
C10 C9 C8 . . 133.7(3)
O1 C9 C8 . . 116.4(3)
C9 C10 C11 . . 106.3(3)
C9 C10 H10 . . 126.8
C11 C10 H10 . . 126.8
C12 C11 C10 . . 106.3(3)
C12 C11 H11 . . 126.8
C10 C11 H11 . . 126.8
C11 C12 O1 . . 111.6(3)
C11 C12 H12 . . 124.2
O1 C12 H12 . . 124.2
C14 C13 O2 . . 110.7(3)
C14 C13 C7 . . 132.9(3)
O2 C13 C7 . . 116.3(3)
C13 C14 C15 . . 106.4(4)
C13 C14 H14 . . 126.8
C15 C14 H14 . . 126.8
C16 C15 C14 . . 106.3(3)
C16 C15 H15 . . 126.8
C14 C15 H15 . . 126.8
C15 C16 O2 . . 110.9(3)
C15 C16 H16 . . 124.5
O2 C16 H16 . . 124.5
N5 C17 C18 . . 123.3(4)
N5 C17 H17 . . 118.3
C18 C17 H17 . . 118.3
C17 C18 C19 . . 118.8(4)
C17 C18 H18 . . 120.6
C19 C18 H18 . . 120.6
C18 C19 C20 . . 119.2(4)
C18 C19 H19 . . 120.4
C20 C19 H19 . . 120.4
C21 C20 C19 . . 118.7(4)
C21 C20 H20 . . 120.6
C19 C20 H20 . . 120.6
N5 C21 C20 . . 122.8(3)
N5 C21 C22 . . 116.5(3)
C20 C21 C22 . . 120.8(3)
N8 C22 N6 . . 125.1(3)
N8 C22 C21 . . 117.2(3)
N6 C22 C21 . . 117.7(3)
N7 C23 C24 . . 120.2(3)
N7 C23 C29 . . 114.3(3)
C24 C23 C29 . . 125.4(3)
N8 C24 C23 . . 118.5(3)
N8 C24 C25 . . 115.5(3)
C23 C24 C25 . . 125.9(3)
C26 C25 O3 . . 111.8(3)
C26 C25 C24 . . 127.6(3)
O3 C25 C24 . . 120.5(3)
C25 C26 C27 . . 104.6(4)
C25 C26 H26 . . 127.7
C27 C26 H26 . . 127.7
C28 C27 C26 . . 109.1(4)
C28 C27 H27 . . 125.5
C26 C27 H27 . . 125.5
C27 C28 O3 . . 110.2(4)
C27 C28 H28 . . 124.9
O3 C28 H28 . . 124.9
C30 C29 O4 . . 110.3(3)
C30 C29 C23 . . 131.4(3)
O4 C29 C23 . . 118.2(3)
C29 C30 C31 . . 102.9(4)
C29 C30 H30 . . 128.5
C31 C30 H30 . . 128.5
C32 C31 C30 . . 108.8(4)
C32 C31 H31 . . 125.6
C30 C31 H31 . . 125.6
C31 C32 O4 . . 110.3(4)
C31 C32 H32 . . 124.9
O4 C32 H32 . . 124.9
O6 N9 O5 . . 116.4(4)
O6 N9 O7 . . 122.2(4)
O5 N9 O7 . . 121.2(4)
C33 N10 Pb1 . . 153.9(4)
C34 N11 C33 . . 120.7(4)
C34 N12 Pb1 . 2_666 133.8(4)
N10 C33 N11 . . 175.2(5)
N12 C34 N11 . . 174.2(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb1 N12 2_666 2.612(4)
Pb1 N10 . 2.631(4)
Pb1 O6 . 2.668(4)
Pb1 O5 . 2.682(4)
Pb1 N5 . 2.727(3)
Pb1 N1 . 2.729(3)
Pb1 N6 . 2.732(3)
Pb1 N2 . 2.768(3)
O1 C12 . 1.363(4)
O1 C9 . 1.368(4)
O2 C16 . 1.367(4)
O2 C13 . 1.374(4)
O3 C25 . 1.368(5)
O3 C28 . 1.403(6)
O4 C32 . 1.356(5)
O4 C29 . 1.375(4)
O5 N9 . 1.228(5)
O6 N9 . 1.211(5)
O7 N9 . 1.230(5)
N1 C1 . 1.334(4)
N1 C5 . 1.344(4)
N2 C6 . 1.330(4)
N2 N3 . 1.345(4)
N3 C7 . 1.324(4)
N4 C8 . 1.343(4)
N4 C6 . 1.350(4)
N5 C17 . 1.346(5)
N5 C21 . 1.351(5)
N6 C22 . 1.337(4)
N6 N7 . 1.340(4)
N7 C23 . 1.328(4)
N8 C22 . 1.331(4)
N8 C24 . 1.340(4)
C1 C2 . 1.379(6)
C1 H1 . 0.9500
C2 C3 . 1.380(6)
C2 H2 . 0.9500
C3 C4 . 1.383(5)
C3 H3 . 0.9500
C4 C5 . 1.389(5)
C4 H4 . 0.9500
C5 C6 . 1.481(4)
C7 C8 . 1.420(5)
C7 C13 . 1.473(4)
C8 C9 . 1.453(4)
C9 C10 . 1.360(4)
C10 C11 . 1.423(5)
C10 H10 . 0.9500
C11 C12 . 1.329(5)
C11 H11 . 0.9500
C12 H12 . 0.9500
C13 C14 . 1.337(5)
C14 C15 . 1.428(5)
C14 H14 . 0.9500
C15 C16 . 1.338(6)
C15 H15 . 0.9500
C16 H16 . 0.9500
C17 C18 . 1.375(6)
C17 H17 . 0.9500
C18 C19 . 1.376(6)
C18 H18 . 0.9500
C19 C20 . 1.388(5)
C19 H19 . 0.9500
C20 C21 . 1.380(5)
C20 H20 . 0.9500
C21 C22 . 1.490(5)
C23 C24 . 1.431(5)
C23 C29 . 1.465(5)
C24 C25 . 1.442(5)
C25 C26 . 1.338(5)
C26 C27 . 1.426(7)
C26 H26 . 0.9500
C27 C28 . 1.290(9)
C27 H27 . 0.9500
C28 H28 . 0.9500
C29 C30 . 1.350(5)
C30 C31 . 1.484(6)
C30 H30 . 0.9500
C31 C32 . 1.283(6)
C31 H31 . 0.9500
C32 H32 . 0.9500
N10 C33 . 1.149(6)
N11 C34 . 1.285(6)
N11 C33 . 1.308(6)
N12 C34 . 1.153(6)
N12 Pb1 2_666 2.612(4)
_cod_database_fobs_code 2021700