#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:36:32 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229140 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/11/7231178.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_7231178
loop_
_publ_author_name
'Seth, Saikat Kumar'
'Bauzá, Antonio'
'Mahmoudi, Ghodrat'
'Stilinović, Vladimir'
'López-Torres, Elena'
'Zaragoza, Guillermo'
'Keramidas, Anastasios D.'
'Frontera, Antonio'
_publ_section_title
;
 On the importance of Pb⋯X (X = O, N, S, Br) tetrel bonding
 interactions in a series of tetra- and hexa-coordinated Pb(ii) compounds
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5033
_journal_paper_doi               10.1039/C8CE00919H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C62 H56 N16 O2 Pb2 S4'
_chemical_formula_weight         1599.84
_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
;
2018-04-29 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                105.607(7)
_cell_angle_beta                 91.747(6)
_cell_angle_gamma                101.222(6)
_cell_formula_units_Z            1
_cell_length_a                   9.7763(6)
_cell_length_b                   11.3341(7)
_cell_length_c                   15.0580(10)
_cell_measurement_reflns_used    4486
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.6792
_cell_measurement_theta_min      4.0346
_cell_volume                     1570.19(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.833
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.833
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5941
_diffrn_reflns_point_group_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         4.050
_exptl_absorpt_coefficient_mu    5.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.679
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1087P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3967
_reflns_number_total             4605
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00919h2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7231176--7231180.cif.'
_cod_original_cell_volume        1570.19(18)
_cod_database_code               7231178
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.090(2) 0.334(2) 0.8611(17) 0.231(9) Uani 1 1 d D U . .
C31 C -0.169(3) 0.4077(18) 0.829(2) 0.27(2) Uani 1 1 d D U A 1
Pb1 Pb 0.60106(3) 0.43273(3) 0.68632(2) 0.04442(16) Uani 1 1 d . . . .
C10 C 0.1678(10) -0.0384(9) 0.6650(7) 0.048(2) Uani 1 1 d . . . .
H10 H 0.2065 -0.0570 0.6085 0.058 Uiso 1 1 calc R U . .
C11 C 0.0380(11) -0.1004(11) 0.6732(9) 0.064(3) Uani 1 1 d . . . .
H11 H -0.0111 -0.1624 0.6225 0.076 Uiso 1 1 calc R U . .
C17 C 0.5354(12) -0.0216(10) 0.8214(7) 0.054(3) Uani 1 1 d . . . .
H17 H 0.4814 -0.0584 0.7653 0.065 Uiso 1 1 calc R U . .
N3 N 0.4305(7) 0.1091(7) 0.6542(5) 0.0397(16) Uani 1 1 d . . . .
C20 C 0.6916(13) 0.0760(15) 0.9843(9) 0.082(4) Uani 1 1 d . . . .
H20 H 0.7477 0.1104 1.0398 0.099 Uiso 1 1 calc R U . .
N2 N 0.5659(7) 0.1772(7) 0.6521(5) 0.0401(17) Uani 1 1 d . . . .
C28 C 0.3499(12) 0.6077(11) 0.6760(9) 0.069(3) Uani 1 1 d . . . .
H28 H 0.3976 0.6152 0.6246 0.082 Uiso 1 1 calc R U . .
N5 N 0.4403(7) 0.3676(7) 0.8097(5) 0.0388(16) Uani 1 1 d . . . .
C7 C 0.6326(12) -0.0245(10) 0.5882(8) 0.062(3) Uani 1 1 d . . . .
H7A H 0.7158 -0.0483 0.5636 0.093 Uiso 1 1 calc R U . .
H7B H 0.6131 -0.0556 0.6408 0.093 Uiso 1 1 calc R U . .
H7C H 0.5553 -0.0592 0.5416 0.093 Uiso 1 1 calc R U . .
C23 C 0.3166(12) 0.4477(13) 0.9430(9) 0.073(3) Uani 1 1 d . . . .
H23A H 0.2606 0.5099 0.9585 0.109 Uiso 1 1 calc R U . .
H23B H 0.2618 0.3678 0.9433 0.109 Uiso 1 1 calc R U . .
H23C H 0.3963 0.4703 0.9876 0.109 Uiso 1 1 calc R U . .
N4 N 0.4978(7) 0.2999(7) 0.8602(5) 0.0413(17) Uani 1 1 d . . . .
C9 C 0.2440(9) 0.0530(8) 0.7406(6) 0.041(2) Uani 1 1 d . . . .
N6 N 0.3872(8) 0.5353(8) 0.7256(6) 0.0489(19) Uani 1 1 d . . . .
C29 C 0.3735(12) 0.3507(10) 0.4759(8) 0.059(3) Uani 1 1 d . . . .
N1 N 0.7997(9) 0.3066(9) 0.6060(8) 0.063(2) Uani 1 1 d . . . .
C21 C 0.6222(12) 0.1534(11) 0.9502(6) 0.068(3) Uani 1 1 d D . . .
H21 H 0.6265 0.2362 0.9835 0.082 Uiso 1 1 calc R U . .
C16 C 0.5460(8) 0.1010(8) 0.8640(5) 0.044(2) Uani 1 1 d D . . .
C12 C -0.0211(11) -0.0734(11) 0.7538(9) 0.064(3) Uani 1 1 d . . . .
H12 H -0.1123 -0.1134 0.7578 0.077 Uiso 1 1 calc R U . .
C8 C 0.3859(8) 0.1177(8) 0.7341(6) 0.0348(18) Uani 1 1 d . . . .
C13 C 0.0538(10) 0.0132(10) 0.8295(9) 0.071(3) Uani 1 1 d D . . .
H13 H 0.0159 0.0265 0.8864 0.085 Uiso 1 1 calc R U . .
C6 C 0.6538(10) 0.1144(8) 0.6170(6) 0.041(2) Uani 1 1 d . . . .
C26 C 0.1756(15) 0.6595(14) 0.7725(12) 0.087(4) Uani 1 1 d . . . .
H26 H 0.1024 0.7007 0.7875 0.104 Uiso 1 1 calc R U . .
C3 C 1.0367(13) 0.2076(17) 0.5918(10) 0.084(4) Uani 1 1 d . . . .
H3 H 1.1171 0.1748 0.5879 0.101 Uiso 1 1 calc R U . .
C5 C 0.7902(11) 0.1870(10) 0.6059(7) 0.050(2) Uani 1 1 d . . . .
C14 C 0.1840(10) 0.0808(11) 0.8233(8) 0.058(3) Uani 1 1 d . . . .
H14 H 0.2309 0.1442 0.8740 0.070 Uiso 1 1 calc R U . .
C4 C 0.9117(13) 0.1373(12) 0.5993(8) 0.067(3) Uani 1 1 d . . . .
H4 H 0.9058 0.0547 0.6001 0.080 Uiso 1 1 calc R U . .
C15 C 0.4782(8) 0.1820(8) 0.8210(6) 0.0374(19) Uani 1 1 d . . . .
C27 C 0.2474(13) 0.6695(12) 0.6975(11) 0.078(4) Uani 1 1 d . . . .
H27 H 0.2246 0.7192 0.6615 0.093 Uiso 1 1 calc R U . .
C18 C 0.6040(13) -0.0923(13) 0.8604(9) 0.073(3) Uani 1 1 d . . . .
H18 H 0.5965 -0.1765 0.8296 0.088 Uiso 1 1 calc R U . .
C25 C 0.2145(12) 0.5858(11) 0.8265(10) 0.071(3) Uani 1 1 d . . . .
H25 H 0.1690 0.5789 0.8788 0.085 Uiso 1 1 calc R U . .
C19 C 0.6812(13) -0.0436(14) 0.9414(9) 0.071(3) Uani 1 1 d . . . .
H19 H 0.7267 -0.0931 0.9671 0.085 Uiso 1 1 calc R U . .
C24 C 0.3201(9) 0.5245(9) 0.8008(7) 0.047(2) Uani 1 1 d . . . .
C22 C 0.3643(9) 0.4404(9) 0.8507(6) 0.043(2) Uani 1 1 d . . . .
S1 S 0.2776(3) 0.3451(3) 0.3857(3) 0.0835(11) Uani 1 1 d . . . .
C1 C 0.9210(12) 0.3745(14) 0.5972(11) 0.086(4) Uani 1 1 d . . . .
H1 H 0.9258 0.4567 0.5956 0.104 Uiso 1 1 calc R U . .
C2 C 1.0418(14) 0.3274(19) 0.5901(11) 0.095(5) Uani 1 1 d . . . .
H2 H 1.1264 0.3778 0.5843 0.114 Uiso 1 1 calc R U . .
N7 N 0.4412(15) 0.3477(12) 0.5369(8) 0.094(4) Uani 1 1 d . . . .
S2 S 0.9301(7) 0.7442(7) 0.9401(4) 0.1412(19) Uani 1 1 d . U . .
C30 C 0.8083(16) 0.6534(17) 0.8671(12) 0.100(4) Uani 1 1 d . U . .
N8 N 0.6878(15) 0.6232(14) 0.8481(9) 0.107(4) Uani 1 1 d . 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'
S S 0.1246 0.1234 '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_3
N7 Pb1 N6 76.7(4) .
N7 Pb1 N5 103.1(3) .
N6 Pb1 N5 61.4(2) .
N7 Pb1 N2 76.7(3) .
N6 Pb1 N2 119.0(2) .
N5 Pb1 N2 72.9(2) .
N7 Pb1 N1 90.9(4) .
N6 Pb1 N1 167.5(3) .
N5 Pb1 N1 124.4(2) .
N2 Pb1 N1 58.4(2) .
N7 Pb1 N8 148.0(4) .
N6 Pb1 N8 74.7(4) .
N5 Pb1 N8 75.2(3) .
N2 Pb1 N8 130.5(3) .
N1 Pb1 N8 116.9(4) .
N7 Pb1 S1 86.9(3) 2_666
N6 Pb1 S1 87.02(19) 2_666
N5 Pb1 S1 142.72(18) 2_666
N2 Pb1 S1 144.01(17) 2_666
N1 Pb1 S1 90.65(19) 2_666
N8 Pb1 S1 77.7(3) 2_666
C11 C10 C9 120.4(11) .
C12 C11 C10 120.9(12) .
C16 C17 C18 120.2(10) .
C8 N3 N2 116.4(7) .
C19 C20 C21 123.0(12) .
C6 N2 N3 116.4(8) .
C6 N2 Pb1 124.7(6) .
N3 N2 Pb1 117.3(5) .
C27 C28 N6 122.6(11) .
C22 N5 N4 117.6(7) .
C22 N5 Pb1 119.3(5) .
N4 N5 Pb1 113.9(5) .
C15 N4 N5 115.0(7) .
C14 C9 C10 118.9(9) .
C14 C9 C8 119.8(9) .
C10 C9 C8 121.2(8) .
C28 N6 C24 119.4(8) .
C28 N6 Pb1 120.3(7) .
C24 N6 Pb1 120.0(6) .
N7 C29 S1 176.1(13) .
C1 N1 C5 119.8(10) .
C1 N1 Pb1 117.2(9) .
C5 N1 Pb1 119.2(6) .
C20 C21 C16 117.0(11) .
C17 C16 C21 119.2(9) .
C17 C16 C15 121.4(7) .
C21 C16 C15 119.4(8) .
C11 C12 C13 119.5(10) .
N3 C8 C9 119.0(8) .
N3 C8 C15 122.1(7) .
C9 C8 C15 118.7(7) .
C12 C13 C14 121.3(11) .
N2 C6 C5 115.9(9) .
N2 C6 C7 126.2(9) .
C5 C6 C7 117.8(8) .
C27 C26 C25 118.7(10) .
C2 C3 C4 118.2(11) .
N1 C5 C4 119.2(10) .
N1 C5 C6 118.5(8) .
C4 C5 C6 122.3(10) .
C9 C14 C13 118.8(11) .
C3 C4 C5 121.0(12) .
N4 C15 C8 123.3(7) .
N4 C15 C16 120.0(7) .
C8 C15 C16 116.6(7) .
C28 C27 C26 119.7(11) .
C19 C18 C17 121.8(13) .
C24 C25 C26 118.8(12) .
C20 C19 C18 118.6(11) .
N6 C24 C25 120.7(10) .
N6 C24 C22 116.4(8) .
C25 C24 C22 122.8(10) .
N5 C22 C23 125.5(9) .
N5 C22 C24 117.0(8) .
C23 C22 C24 117.5(9) .
C29 S1 Pb1 109.0(4) 2_666
N1 C1 C2 122.0(14) .
C3 C2 C1 119.9(13) .
C29 N7 Pb1 157.4(11) .
N8 C30 S2 145.5(18) .
C30 N8 Pb1 115.7(15) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C31 1.401(2) .
Pb1 N7 2.543(13) .
Pb1 N6 2.593(7) .
Pb1 N5 2.633(6) .
Pb1 N2 2.752(7) .
Pb1 N1 2.751(8) .
Pb1 N8 2.766(14) .
Pb1 S1 3.051(3) 2_666
C10 C11 1.352(15) .
C10 C9 1.392(13) .
C11 C12 1.345(17) .
C17 C16 1.347(14) .
C17 C18 1.368(14) .
N3 C8 1.278(11) .
N3 N2 1.402(10) .
C20 C19 1.32(2) .
C20 C21 1.395(16) .
N2 C6 1.260(11) .
C28 C27 1.330(15) .
C28 N6 1.339(12) .
N5 C22 1.268(11) .
N5 N4 1.392(9) .
C7 C6 1.487(13) .
C23 C22 1.465(14) .
N4 C15 1.281(12) .
C9 C14 1.378(15) .
C9 C8 1.457(11) .
N6 C24 1.349(12) .
C29 N7 1.128(15) .
C29 S1 1.606(12) .
N1 C1 1.313(15) .
N1 C5 1.340(13) .
C21 C16 1.395(2) .
C16 C15 1.495(11) .
C12 C13 1.367(17) .
C8 C15 1.489(12) .
C13 C14 1.372(14) .
C6 C5 1.464(14) .
C26 C27 1.367(19) .
C26 C25 1.405(18) .
C3 C2 1.36(2) .
C3 C4 1.349(19) .
C5 C4 1.406(14) .
C18 C19 1.335(19) .
C25 C24 1.362(14) .
C24 C22 1.478(13) .
S1 Pb1 3.051(3) 2_666
C1 C2 1.383(18) .
S2 C30 1.59(2) .
C30 N8 1.165(18) .
