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#$Date: 2019-11-17 09:15:03 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/91/1549181.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_1549181
loop_
_publ_author_name
'Mahmoudi, Ghodrat'
'Seth, Saikat Kumar'
'Bauzá, Antonio'
'Zubkov, Fedor I.'
'Gurbanov, Atash V.'
'White, Jonathan'
'Stilinović, Vladimir'
'Doert, Thomas'
'Frontera, Antonio'
_publ_section_title
;
 Pb⋯X (X = N, S, I) tetrel bonding interactions in Pb(ii)
 complexes: X-ray characterization, Hirshfeld surfaces and DFT
 calculations
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              2812
_journal_paper_doi               10.1039/C8CE00110C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C16 H12 N6 O3 Pb2 S2'
_chemical_formula_weight         814.82
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-23 deposited with the CCDC.
2018-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                72.684(7)
_cell_angle_beta                 80.451(9)
_cell_angle_gamma                82.758(7)
_cell_formula_units_Z            2
_cell_length_a                   8.5997(9)
_cell_length_b                   10.9376(7)
_cell_length_c                   11.7938(12)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      27.7347
_cell_measurement_theta_min      2.9735
_cell_volume                     1040.90(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13256
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.978
_exptl_absorpt_coefficient_mu    16.384
_exptl_absorpt_correction_T_max  0.170
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.600
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.3829
_exptl_crystal_size_mid          0.1692
_exptl_crystal_size_min          0.1349
_refine_diff_density_max         1.552
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0238P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4048
_reflns_number_total             4469
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00110c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1549180--1549183.cif.'
_cod_database_code               1549181
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Pb1 Pb 0.10073(2) 0.21178(2) 0.36241(2) 0.01754(6) Uani 1 1 d . .
Pb2 Pb 0.34642(2) 0.02446(2) 0.66310(2) 0.01624(6) Uani 1 1 d . .
C15 C -0.0313(6) -0.0071(5) 0.2103(5) 0.0225(11) Uani 1 1 d . .
S2 S -0.17395(17) 0.25199(13) 0.53658(12) 0.0285(3) Uani 1 1 d . .
S5 S 0.57488(18) 0.13362(15) 0.09260(12) 0.0344(4) Uani 1 1 d . .
O1 O 0.2579(4) 0.2178(3) 0.5214(3) 0.0210(8) Uani 1 1 d . .
O3 O -0.0672(4) 0.0729(4) 0.2693(4) 0.0344(10) Uani 1 1 d . .
O2 O -0.1239(4) -0.0866(3) 0.2097(3) 0.0237(8) Uani 1 1 d . .
N1 N 0.4176(5) 0.2245(4) 0.6966(4) 0.0175(9) Uani 1 1 d . .
N2 N 0.2099(5) 0.4396(4) 0.4699(4) 0.0173(9) Uani 1 1 d . .
N3 N 0.1263(5) 0.4232(4) 0.3844(4) 0.0164(9) Uani 1 1 d . .
N4 N -0.0476(5) 0.4013(4) 0.2197(3) 0.0184(9) Uani 1 1 d . .
C14 C -0.2519(6) 0.1174(5) 0.5536(4) 0.0209(11) Uani 1 1 d . .
N7 N 0.3476(6) 0.2858(5) 0.2013(4) 0.0332(11) Uani 1 1 d . .
N5 N -0.3113(5) 0.0237(4) 0.5654(4) 0.0268(10) Uani 1 1 d . .
C1 C 0.3668(5) 0.3370(5) 0.6249(4) 0.0159(10) Uani 1 1 d . .
C2 C 0.4013(6) 0.4543(5) 0.6343(4) 0.0177(10) Uani 1 1 d . .
H2 H 0.3625 0.5312 0.5845 0.021 Uiso 1 1 calc R U
C3 C 0.4939(6) 0.4539(5) 0.7189(4) 0.0210(11) Uani 1 1 d . .
H3 H 0.5216 0.5307 0.7257 0.025 Uiso 1 1 calc R U
C4 C 0.5452(6) 0.3375(5) 0.7935(4) 0.0224(11) Uani 1 1 d . .
H4 H 0.6072 0.3350 0.8518 0.027 Uiso 1 1 calc R U
C5 C 0.5036(6) 0.2253(5) 0.7807(5) 0.0221(11) Uani 1 1 d . .
H5 H 0.5365 0.1475 0.8325 0.026 Uiso 1 1 calc R U
C6 C 0.2711(6) 0.3295(5) 0.5317(4) 0.0170(10) Uani 1 1 d . .
C7 C 0.0688(6) 0.5261(5) 0.3155(4) 0.0181(10) Uani 1 1 d . .
H7 H 0.0854 0.6054 0.3234 0.022 Uiso 1 1 calc R U
C8 C -0.0241(6) 0.5197(5) 0.2235(4) 0.0187(10) Uani 1 1 d . .
C9 C -0.0856(6) 0.6299(5) 0.1478(4) 0.0221(11) Uani 1 1 d . .
H9 H -0.0667 0.7101 0.1521 0.026 Uiso 1 1 calc R U
C10 C -0.1768(6) 0.6192(5) 0.0646(4) 0.0230(11) Uani 1 1 d . .
H10 H -0.2190 0.6922 0.0117 0.028 Uiso 1 1 calc R U
C11 C -0.2033(6) 0.4993(5) 0.0620(4) 0.0233(11) Uani 1 1 d . .
H11 H -0.2653 0.4897 0.0083 0.028 Uiso 1 1 calc R U
C12 C -0.1355(6) 0.3913(5) 0.1416(4) 0.0217(11) Uani 1 1 d . .
H12 H -0.1530 0.3099 0.1394 0.026 Uiso 1 1 calc R U
C13 C 0.4425(6) 0.2239(5) 0.1561(4) 0.0245(12) Uani 1 1 d . .
C16 C 0.1270(6) -0.0056(6) 0.1322(5) 0.0331(13) Uani 1 1 d . .
H16B H 0.1672 -0.0921 0.1343 0.050 Uiso 1 1 calc R U
H16A H 0.1998 0.0336 0.1614 0.050 Uiso 1 1 calc R U
H16C H 0.1144 0.0427 0.0512 0.050 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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N3 Pb1 O1 63.27(12) . .
N3 Pb1 N4 65.30(13) . .
O1 Pb1 N4 128.54(12) . .
N3 Pb1 N7 78.67(14) . .
O1 Pb1 N7 88.56(13) . .
N4 Pb1 N7 83.07(13) . .
N3 Pb1 S2 75.70(10) . .
O1 Pb1 S2 84.13(9) . .
N4 Pb1 S2 82.09(9) . .
N7 Pb1 S2 153.94(11) . .
O2 Pb2 O1 82.40(12) 2_556 .
O2 Pb2 N1 75.28(12) 2_556 .
O1 Pb2 N1 66.47(12) . .
O2 Pb2 O3 51.39(11) 2_556 2_556
O1 Pb2 O3 96.29(12) . 2_556
N1 Pb2 O3 126.15(12) . 2_556
O2 Pb2 S5 78.88(9) 2_556 2_656
O1 Pb2 S5 154.01(8) . 2_656
N1 Pb2 S5 91.28(10) . 2_656
O3 Pb2 S5 85.98(9) 2_556 2_656
O3 C15 O2 122.7(5) . .
O3 C15 C16 119.4(5) . .
O2 C15 C16 117.8(5) . .
C14 S2 Pb1 96.76(18) . .
C13 S5 Pb2 89.84(18) . 2_656
C6 O1 Pb2 121.9(3) . .
C6 O1 Pb1 116.1(3) . .
Pb2 O1 Pb1 121.40(13) . .
C15 O3 Pb2 86.7(3) . 2_556
C15 O2 Pb2 99.2(3) . 2_556
C5 N1 C1 118.4(4) . .
C5 N1 Pb2 124.0(3) . .
C1 N1 Pb2 117.6(3) . .
C6 N2 N3 111.0(4) . .
C7 N3 N2 115.6(4) . .
C7 N3 Pb1 122.0(3) . .
N2 N3 Pb1 122.4(3) . .
C12 N4 C8 118.7(4) . .
C12 N4 Pb1 125.7(3) . .
C8 N4 Pb1 115.5(3) . .
N5 C14 S2 178.1(5) . .
C13 N7 Pb1 128.7(4) . .
N1 C1 C2 122.5(4) . .
N1 C1 C6 115.8(4) . .
C2 C1 C6 121.7(4) . .
C3 C2 C1 118.6(5) . .
C3 C2 H2 120.7 . .
C1 C2 H2 120.7 . .
C2 C3 C4 118.8(5) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 119.4(4) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
N1 C5 C4 122.2(5) . .
N1 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
O1 C6 N2 127.2(4) . .
O1 C6 C1 117.6(4) . .
N2 C6 C1 115.2(4) . .
N3 C7 C8 120.0(4) . .
N3 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
N4 C8 C9 122.5(4) . .
N4 C8 C7 116.8(4) . .
C9 C8 C7 120.7(5) . .
C8 C9 C10 118.7(5) . .
C8 C9 H9 120.6 . .
C10 C9 H9 120.6 . .
C11 C10 C9 118.8(5) . .
C11 C10 H10 120.6 . .
C9 C10 H10 120.6 . .
C10 C11 C12 119.1(5) . .
C10 C11 H11 120.5 . .
C12 C11 H11 120.5 . .
N4 C12 C11 122.1(5) . .
N4 C12 H12 118.9 . .
C11 C12 H12 118.9 . .
N7 C13 S5 178.9(5) . .
C15 C16 H16B 109.5 . .
C15 C16 H16A 109.5 . .
H16B C16 H16A 109.5 . .
C15 C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N3 2.442(4) .
Pb1 O1 2.507(3) .
Pb1 N4 2.593(4) .
Pb1 N7 2.637(5) .
Pb1 S2 2.9426(15) .
Pb2 O2 2.387(3) 2_556
Pb2 O1 2.399(3) .
Pb2 N1 2.499(4) .
Pb2 O3 2.653(4) 2_556
Pb2 S5 3.0224(14) 2_656
C15 O3 1.253(6) .
C15 O2 1.253(6) .
C15 C16 1.511(7) .
S2 C14 1.639(5) .
S5 C13 1.644(6) .
S5 Pb2 3.0224(14) 2_656
O1 C6 1.284(6) .
O3 Pb2 2.654(4) 2_556
O2 Pb2 2.387(3) 2_556
N1 C5 1.335(6) .
N1 C1 1.337(6) .
N2 C6 1.305(6) .
N2 N3 1.395(5) .
N3 C7 1.273(6) .
N4 C12 1.320(6) .
N4 C8 1.350(6) .
C14 N5 1.163(6) .
N7 C13 1.159(7) .
C1 C2 1.392(6) .
C1 C6 1.504(6) .
C2 C3 1.374(6) .
C2 H2 0.9300 .
C3 C4 1.382(7) .
C3 H3 0.9300 .
C4 C5 1.376(7) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C7 C8 1.473(6) .
C7 H7 0.9300 .
C8 C9 1.373(7) .
C9 C10 1.393(7) .
C9 H9 0.9300 .
C10 C11 1.368(7) .
C10 H10 0.9300 .
C11 C12 1.402(7) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C16 H16B 0.9600 .
C16 H16A 0.9600 .
C16 H16C 0.9600 .
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_4
O2 C15 O3 Pb2 -1.1(5) 2_556
C16 C15 O3 Pb2 176.2(4) 2_556
O3 C15 O2 Pb2 1.3(5) 2_556
C16 C15 O2 Pb2 -176.1(4) 2_556
C6 N2 N3 C7 -176.6(4) .
C6 N2 N3 Pb1 0.9(5) .
C5 N1 C1 C2 0.5(7) .
Pb2 N1 C1 C2 -179.1(3) .
C5 N1 C1 C6 179.8(4) .
Pb2 N1 C1 C6 0.2(5) .
N1 C1 C2 C3 1.5(7) .
C6 C1 C2 C3 -177.8(4) .
C1 C2 C3 C4 -1.9(7) .
C2 C3 C4 C5 0.6(7) .
C1 N1 C5 C4 -2.0(7) .
Pb2 N1 C5 C4 177.6(4) .
C3 C4 C5 N1 1.4(8) .
Pb2 O1 C6 N2 -170.6(4) .
Pb1 O1 C6 N2 1.1(6) .
Pb2 O1 C6 C1 9.2(6) .
Pb1 O1 C6 C1 -179.1(3) .
N3 N2 C6 O1 -1.4(7) .
N3 N2 C6 C1 178.8(4) .
N1 C1 C6 O1 -6.0(6) .
C2 C1 C6 O1 173.3(4) .
N1 C1 C6 N2 173.8(4) .
C2 C1 C6 N2 -6.9(7) .
N2 N3 C7 C8 -178.9(4) .
Pb1 N3 C7 C8 3.5(6) .
C12 N4 C8 C9 -1.2(7) .
Pb1 N4 C8 C9 175.5(4) .
C12 N4 C8 C7 177.3(4) .
Pb1 N4 C8 C7 -5.9(5) .
N3 C7 C8 N4 2.0(7) .
N3 C7 C8 C9 -179.4(5) .
N4 C8 C9 C10 0.5(7) .
C7 C8 C9 C10 -178.0(5) .
C8 C9 C10 C11 0.7(7) .
C9 C10 C11 C12 -1.1(8) .
C8 N4 C12 C11 0.7(7) .
Pb1 N4 C12 C11 -175.7(3) .
C10 C11 C12 N4 0.4(8) .
