#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:13:31 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230416 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/70/7057054.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_7057054
loop_
_publ_author_name
'Mahmoudi, Ghodrat'
'Zangrando, Ennio'
'Mitoraj, Mariusz P.'
'Gurbanov, Atash V.'
'Zubkov, Fedor I.'
'Moosavifar, Maryam'
'Konyaeva, Irina A.'
'Kirillov, Alexander M.'
'Safin, Damir A.'
_publ_section_title
;
 Extended lead(ii) architectures engineered via tetrel bonding
 interactions
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4959
_journal_paper_doi               10.1039/C8NJ00525G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C15 H16 N10 O13 Pb2'
_chemical_formula_sum            'C15 H16 N10 O13 Pb2'
_chemical_formula_weight         958.76
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-17 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.828(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.620(3)
_cell_length_b                   8.762(2)
_cell_length_c                   11.862(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      3.25
_cell_volume                     2471.9(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2285
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.974
_diffrn_reflns_theta_max         24.974
_diffrn_reflns_theta_min         1.712
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    13.690
_exptl_absorpt_correction_T_max  0.1919
_exptl_absorpt_correction_T_min  0.0932
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.617
_refine_diff_density_min         -2.456
_refine_diff_density_rms         0.348
_refine_ls_extinction_coef       0.00189(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1042P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1760
_reflns_number_total             2165
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj00525g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7057051--7057054.cif.'
_cod_database_code               7057054
_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+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
Pb Pb 0.42835(2) 0.13753(5) 0.56759(4) 0.0278(3) Uani 1 1 d . . .
O1 O 0.5000 0.2890(16) 0.7500 0.048(4) Uani 1 2 d S T P
N1 N 0.3567(4) 0.2614(12) 0.3871(9) 0.028(2) Uani 1 1 d . . .
N2 N 0.4289(4) 0.4298(13) 0.5595(10) 0.034(3) Uani 1 1 d . . .
N3 N 0.4651(5) 0.5120(12) 0.6584(10) 0.038(3) Uani 1 1 d . . .
H3N H 0.4648 0.6101 0.6600 0.046 Uiso 1 1 calc R U .
C1 C 0.3211(6) 0.1735(15) 0.2985(12) 0.031(3) Uani 1 1 d . . .
H1 H 0.3208 0.0690 0.3118 0.038 Uiso 1 1 calc R U .
C2 C 0.2856(6) 0.2307(19) 0.1907(12) 0.040(4) Uani 1 1 d . . .
H2 H 0.2617 0.1662 0.1316 0.048 Uiso 1 1 calc R U .
C3 C 0.2855(7) 0.3837(17) 0.1704(13) 0.044(4) Uani 1 1 d . . .
H3 H 0.2616 0.4243 0.0968 0.052 Uiso 1 1 calc R U .
C4 C 0.3203(6) 0.4772(17) 0.2576(13) 0.041(3) Uani 1 1 d . . .
H4 H 0.3203 0.5821 0.2458 0.049 Uiso 1 1 calc R U .
C5 C 0.3567(5) 0.4092(15) 0.3671(12) 0.030(3) Uani 1 1 d . . .
C6 C 0.3955(5) 0.5058(16) 0.4681(12) 0.032(3) Uani 1 1 d . . .
C7 C 0.5000 0.431(2) 0.7500 0.031(4) Uani 1 2 d S T P
C8 C 0.3929(7) 0.6760(17) 0.4571(15) 0.058(5) Uani 1 1 d . . .
H8A H 0.3672 0.7152 0.4918 0.086 Uiso 1 1 calc R U .
H8B H 0.3803 0.7041 0.3730 0.086 Uiso 1 1 calc R U .
H8C H 0.4297 0.7179 0.4996 0.086 Uiso 1 1 calc R U .
N4 N 0.3209(6) 0.1280(13) 0.6044(13) 0.045(3) Uani 1 1 d . . .
O2 O 0.3597(5) 0.2278(12) 0.6488(10) 0.051(3) Uani 1 1 d . . .
O3 O 0.3285(4) 0.0244(11) 0.5426(10) 0.043(2) Uani 1 1 d . . .
O4 O 0.2772(6) 0.1365(14) 0.6271(18) 0.091(5) Uani 1 1 d . . .
N5 N 0.4511(5) 0.1264(12) 0.3154(12) 0.037(3) Uani 1 1 d . . .
O5 O 0.4709(4) 0.2262(11) 0.3959(9) 0.045(3) Uani 1 1 d . . .
O6 O 0.4394(5) 0.1613(13) 0.2082(10) 0.056(3) Uani 1 1 d . . .
O7 O 0.4434(5) -0.0027(12) 0.3425(12) 0.066(4) Uani 1 1 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'
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
O2 Pb N1 77.8(4) . .
O2 Pb N2 72.8(4) . .
N1 Pb N2 62.9(3) . .
O2 Pb O1 84.0(3) . .
N1 Pb O1 123.7(4) . .
N2 Pb O1 60.8(3) . .
O2 Pb O3 50.0(3) . .
N1 Pb O3 72.3(3) . .
N2 Pb O3 112.8(3) . .
O1 Pb O3 129.2(2) . .
O2 Pb O5 138.1(4) . .
N1 Pb O5 67.0(3) . .
N2 Pb O5 71.4(3) . .
O1 Pb O5 96.8(2) . .
O3 Pb O5 130.7(3) . .
C7 O1 Pb 120.4(3) . .
C7 O1 Pb 120.4(3) . 2_656
Pb O1 Pb 119.1(5) . 2_656
C5 N1 C1 117.9(11) . .
C5 N1 Pb 122.3(8) . .
C1 N1 Pb 119.3(8) . .
C6 N2 N3 117.8(11) . .
C6 N2 Pb 122.4(9) . .
N3 N2 Pb 119.7(7) . .
C7 N3 N2 116.5(11) . .
C7 N3 H3N 121.8 . .
N2 N3 H3N 121.8 . .
N1 C1 C2 123.0(13) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C1 C2 C3 119.0(13) . .
C1 C2 H2 120.5 . .
C3 C2 H2 120.5 . .
C4 C3 C2 120.0(14) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C3 C4 C5 117.7(13) . .
C3 C4 H4 121.1 . .
C5 C4 H4 121.1 . .
N1 C5 C4 122.3(12) . .
N1 C5 C6 117.1(11) . .
C4 C5 C6 120.6(12) . .
N2 C6 C8 125.6(12) . .
N2 C6 C5 114.6(12) . .
C8 C6 C5 119.9(11) . .
O1 C7 N3 122.4(8) . 2_656
O1 C7 N3 122.4(8) . .
N3 C7 N3 115.1(17) 2_656 .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O3 N4 O4 121.9(14) . .
O3 N4 O2 118.5(12) . .
O4 N4 O2 119.5(15) . .
N4 O2 Pb 100.4(8) . .
N4 O3 Pb 91.1(8) . .
O7 N5 O6 120.3(12) . .
O7 N5 O5 120.6(13) . .
O6 N5 O5 119.1(12) . .
N5 O5 Pb 101.9(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb O2 2.430(11) .
Pb N1 2.492(10) .
Pb N2 2.563(11) .
Pb O1 2.619(7) .
Pb O3 2.655(10) .
Pb O5 2.756(10) .
O1 C7 1.24(3) .
O1 Pb 2.619(7) 2_656
N1 C5 1.316(17) .
N1 C1 1.348(16) .
N2 C6 1.289(15) .
N2 N3 1.395(14) .
N3 C7 1.329(14) .
N3 H3N 0.8600 .
C1 C2 1.360(19) .
C1 H1 0.9300 .
C2 C3 1.36(2) .
C2 H2 0.9300 .
C3 C4 1.36(2) .
C3 H3 0.9300 .
C4 C5 1.418(18) .
C4 H4 0.9300 .
C5 C6 1.501(18) .
C6 C8 1.497(19) .
C7 N3 1.329(14) 2_656
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
N4 O3 1.227(15) .
N4 O4 1.247(17) .
N4 O2 1.282(16) .
N5 O7 1.212(14) .
N5 O6 1.231(17) .
N5 O5 1.254(14) .
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
C6 N2 N3 C7 -178.4(12) . .
Pb N2 N3 C7 3.8(15) . .
C5 N1 C1 C2 0.0(19) . .
Pb N1 C1 C2 -171.6(10) . .
N1 C1 C2 C3 0(2) . .
C1 C2 C3 C4 0(2) . .
C2 C3 C4 C5 1(2) . .
C1 N1 C5 C4 1.0(19) . .
Pb N1 C5 C4 172.3(10) . .
C1 N1 C5 C6 178.3(12) . .
Pb N1 C5 C6 -10.4(15) . .
C3 C4 C5 N1 -2(2) . .
C3 C4 C5 C6 -178.8(14) . .
N3 N2 C6 C8 2(2) . .
Pb N2 C6 C8 179.5(12) . .
N3 N2 C6 C5 -178.2(12) . .
Pb N2 C6 C5 -0.4(16) . .
N1 C5 C6 N2 6.8(18) . .
C4 C5 C6 N2 -175.8(13) . .
N1 C5 C6 C8 -173.0(13) . .
C4 C5 C6 C8 4(2) . .
Pb O1 C7 N3 178.8(7) . 2_656
Pb O1 C7 N3 -1.2(7) 2_656 2_656
Pb O1 C7 N3 -1.2(7) . .
Pb O1 C7 N3 178.8(7) 2_656 .
N2 N3 C7 O1 -1.7(14) . .
N2 N3 C7 N3 178.3(14) . 2_656
O3 N4 O2 Pb 1.4(13) . .
O4 N4 O2 Pb 179.9(12) . .
O4 N4 O3 Pb -179.7(14) . .
O2 N4 O3 Pb -1.3(12) . .
O7 N5 O5 Pb -32.4(14) . .
O6 N5 O5 Pb 147.5(10) . .
