#------------------------------------------------------------------------------
#$Date: 2020-03-07 04:35:34 +0200 (Sat, 07 Mar 2020) $
#$Revision: 249166 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/00/7240086.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_7240086
loop_
_publ_author_name
'Safin, Damir'
'Mahmoudi, Ghodrat'
'Akbari Afkhami, Farhad'
'Gupta, Arunava'
'Qu, Fengrui'
'Kose, Muhammet'
'Zubkov, Fedor Ivanovich'
'Zangrando, Ennio'
'Alkorta, Ibon'
_publ_section_title
;
 Supramolecular lead(II) architectures engineered by tetrel bonds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00102C
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 N6 O7 Pb'
_chemical_formula_sum            'C12 H10 N6 O7 Pb'
_chemical_formula_weight         557.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-10-22 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.710(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2085(6)
_cell_length_b                   12.9123(5)
_cell_length_c                   7.4057(2)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.5991
_cell_measurement_theta_min      2.3947
_cell_volume                     1626.58(10)
_computing_cell_refinement       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_data_collection       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_data_reduction        'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            52795
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.711
_diffrn_reflns_theta_min         1.980
_diffrn_source                   'fine focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.424
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0172
_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/[σ²(Fo²)+(0.0182P)²+1.3523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4053
_reflns_number_total             4616
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00102c1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7240086
_shelx_shelxl_version_number     2017/1
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pb Pb 0.26086(2) 0.58286(2) 0.35383(2) 0.02067(3) Uani 1 1 d . . . . .
O1 O 0.37809(11) 0.60972(15) 0.6370(2) 0.0283(4) Uani 1 1 d . . . . .
O2 O 0.32140(13) 0.39837(16) 0.3781(3) 0.0395(5) Uani 1 1 d . . . . .
O3 O 0.24745(11) 0.42391(15) 0.1187(2) 0.0305(4) Uani 1 1 d . . . . .
O4 O 0.2926(2) 0.2711(2) 0.1910(4) 0.0789(10) Uani 1 1 d . . . . .
N1 N 0.13639(12) 0.47534(17) 0.3814(3) 0.0255(4) Uani 1 1 d . . . . .
N2 N 0.24528(12) 0.51345(17) 0.6749(3) 0.0229(4) Uani 1 1 d . . . . .
N3 N 0.30084(12) 0.53494(18) 0.8211(3) 0.0248(4) Uani 1 1 d . . . . .
H3 H 0.294228 0.517117 0.931024 0.030 Uiso 1 1 calc R U . . .
N4 N 0.40596(13) 0.57964(17) 1.1205(3) 0.0271(4) Uani 1 1 d . . . . .
N5 N 0.28759(14) 0.36217(19) 0.2288(3) 0.0322(5) Uani 1 1 d . . . . .
C1 C 0.08150(16) 0.4548(2) 0.2375(4) 0.0333(6) Uani 1 1 d . . . . .
H1 H 0.087399 0.483698 0.123846 0.040 Uiso 1 1 calc R U . . .
C2 C 0.01659(17) 0.3932(2) 0.2476(4) 0.0378(7) Uani 1 1 d . . . . .
H2 H -0.020506 0.380589 0.143099 0.045 Uiso 1 1 calc R U . . .
C3 C 0.00724(18) 0.3509(3) 0.4121(4) 0.0421(7) Uani 1 1 d . . . . .
H3A H -0.036828 0.309625 0.422950 0.051 Uiso 1 1 calc R U . . .
C4 C 0.06388(18) 0.3698(3) 0.5629(4) 0.0400(7) Uani 1 1 d . . . . .
H4 H 0.059355 0.340431 0.676981 0.048 Uiso 1 1 calc R U . . .
C5 C 0.12756(15) 0.4331(2) 0.5424(3) 0.0266(5) Uani 1 1 d . . . . .
C6 C 0.18774(16) 0.4554(2) 0.6991(3) 0.0288(5) Uani 1 1 d . . . . .
H6 H 0.184100 0.427763 0.814967 0.035 Uiso 1 1 calc R U . . .
C7 C 0.36622(14) 0.58451(18) 0.7906(3) 0.0222(5) Uani 1 1 d . . . . .
C8 C 0.42588(15) 0.60455(18) 0.9574(3) 0.0222(5) Uani 1 1 d . . . . .
C9 C 0.49836(15) 0.64213(19) 0.9326(3) 0.0266(5) Uani 1 1 d . . . . .
H9 H 0.509150 0.657989 0.815015 0.032 Uiso 1 1 calc R U . . .
C10 C 0.55545(16) 0.6562(2) 1.0856(4) 0.0313(6) Uani 1 1 d . . . . .
H10 H 0.605450 0.682294 1.074074 0.038 Uiso 1 1 calc R U . . .
C11 C 0.53637(16) 0.6306(2) 1.2544(4) 0.0305(6) Uani 1 1 d . . . . .
H11 H 0.573499 0.638382 1.360463 0.037 Uiso 1 1 calc R U . . .
C12 C 0.46212(17) 0.5934(2) 1.2654(3) 0.0321(6) Uani 1 1 d . . . . .
H12 H 0.450087 0.576558 1.381523 0.039 Uiso 1 1 calc R U . . .
O5 O 0.24844(12) 0.75589(17) 0.5647(3) 0.0422(5) Uani 1 1 d . . . . .
O6 O 0.14215(12) 0.72807(16) 0.3769(3) 0.0389(5) Uani 1 1 d . . . . .
O7 O 0.16014(12) 0.87514(15) 0.5178(3) 0.0328(4) Uani 1 1 d . . . . .
N6 N 0.18297(12) 0.78658(16) 0.4856(3) 0.0244(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
_geom_angle_publ_flag
N1 Pb N2 62.63(6) . . ?
N1 Pb O2 80.24(7) . . ?
N2 Pb O2 73.47(7) . . ?
N1 Pb O3 69.47(6) . . ?
N2 Pb O3 108.70(6) . . ?
O2 Pb O3 48.39(6) . . ?
N1 Pb O1 122.50(6) . . ?
N2 Pb O1 60.10(6) . . ?
O2 Pb O1 79.60(6) . . ?
O3 Pb O1 125.69(6) . . ?
N1 Pb O5 104.75(7) . . ?
N2 Pb O5 74.49(7) . . ?
O2 Pb O5 140.41(6) . . ?
O3 Pb O5 169.80(6) . . ?
O1 Pb O5 64.44(6) . . ?
C7 O1 Pb 118.34(16) . . ?
N5 O2 Pb 98.79(15) . . ?
N5 O3 Pb 94.51(14) . . ?
C1 N1 C5 117.8(2) . . ?
C1 N1 Pb 122.44(17) . . ?
C5 N1 Pb 119.70(16) . . ?
C6 N2 N3 118.3(2) . . ?
C6 N2 Pb 121.50(15) . . ?
N3 N2 Pb 120.12(15) . . ?
C7 N3 N2 117.97(19) . . ?
C7 N3 H3 121.0 . . ?
N2 N3 H3 121.0 . . ?
C12 N4 C8 115.8(2) . . ?
O4 N5 O2 121.5(2) . . ?
O4 N5 O3 120.7(2) . . ?
O2 N5 O3 117.8(2) . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.2(2) . . ?
N1 C5 C6 117.6(2) . . ?
C4 C5 C6 120.2(2) . . ?
N2 C6 C5 118.4(2) . . ?
N2 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
O1 C7 N3 122.9(2) . . ?
O1 C7 C8 121.7(2) . . ?
N3 C7 C8 115.4(2) . . ?
N4 C8 C9 124.4(2) . . ?
N4 C8 C7 117.5(2) . . ?
C9 C8 C7 118.1(2) . . ?
C8 C9 C10 118.6(2) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 118.0(3) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C12 C11 C10 119.1(2) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N4 C12 C11 124.1(3) . . ?
N4 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
N6 O5 Pb 97.64(14) . . ?
O6 N6 O7 121.3(2) . . ?
O6 N6 O5 119.4(2) . . ?
O7 N6 O5 119.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb N1 2.586(2) . ?
Pb N2 2.5923(19) . ?
Pb O2 2.595(2) . ?
Pb O3 2.6790(19) . ?
Pb O1 2.7032(17) . ?
Pb O5 2.753(2) . ?
O1 C7 1.229(3) . ?
O2 N5 1.259(3) . ?
O3 N5 1.268(3) . ?
O4 N5 1.214(3) . ?
N1 C1 1.339(3) . ?
N1 C5 1.341(3) . ?
N2 C6 1.276(3) . ?
N2 N3 1.360(3) . ?
N3 C7 1.343(3) . ?
N3 H3 0.8700 . ?
N4 C12 1.343(3) . ?
N4 C8 1.344(3) . ?
C1 C2 1.383(4) . ?
C1 H1 0.9400 . ?
C2 C3 1.366(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.388(4) . ?
C3 H3A 0.9400 . ?
C4 C5 1.393(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.463(3) . ?
C6 H6 0.9400 . ?
C7 C8 1.505(3) . ?
C8 C9 1.376(4) . ?
C9 C10 1.395(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9400 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
O5 N6 1.253(3) . ?
O6 N6 1.241(3) . ?
O7 N6 1.244(3) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 N3 C7 171.5(2) . . . . ?
Pb N2 N3 C7 -5.8(3) . . . . ?
Pb O2 N5 O4 -171.9(3) . . . . ?
Pb O2 N5 O3 7.6(3) . . . . ?
Pb O3 N5 O4 172.2(3) . . . . ?
Pb O3 N5 O2 -7.3(3) . . . . ?
C5 N1 C1 C2 0.4(4) . . . . ?
Pb N1 C1 C2 176.6(2) . . . . ?
N1 C1 C2 C3 0.1(5) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C1 N1 C5 C4 -0.1(4) . . . . ?
Pb N1 C5 C4 -176.4(2) . . . . ?
C1 N1 C5 C6 179.8(3) . . . . ?
Pb N1 C5 C6 3.5(3) . . . . ?
C3 C4 C5 N1 -0.7(5) . . . . ?
C3 C4 C5 C6 179.3(3) . . . . ?
N3 N2 C6 C5 179.4(2) . . . . ?
Pb N2 C6 C5 -3.3(3) . . . . ?
N1 C5 C6 N2 -0.2(4) . . . . ?
C4 C5 C6 N2 179.8(3) . . . . ?
Pb O1 C7 N3 6.9(3) . . . . ?
Pb O1 C7 C8 -175.11(16) . . . . ?
N2 N3 C7 O1 -1.0(4) . . . . ?
N2 N3 C7 C8 -179.1(2) . . . . ?
C12 N4 C8 C9 0.0(4) . . . . ?
C12 N4 C8 C7 176.5(2) . . . . ?
O1 C7 C8 N4 176.3(2) . . . . ?
N3 C7 C8 N4 -5.5(3) . . . . ?
O1 C7 C8 C9 -6.9(4) . . . . ?
N3 C7 C8 C9 171.3(2) . . . . ?
N4 C8 C9 C10 -0.3(4) . . . . ?
C7 C8 C9 C10 -176.9(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C10 C11 C12 -0.6(4) . . . . ?
C8 N4 C12 C11 0.1(4) . . . . ?
C10 C11 C12 N4 0.2(4) . . . . ?
Pb O5 N6 O6 12.7(3) . . . . ?
Pb O5 N6 O7 -167.42(19) . . . . ?
