#------------------------------------------------------------------------------
#$Date: 2016-08-06 03:57:24 +0300 (Sat, 06 Aug 2016) $
#$Revision: 185045 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/61/7226171.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_7226171
loop_
_publ_author_name
'Mahmoudi, Ghodrat'
'Bauzá, Antonio'
'Frontera, Antonio'
'Garczarek, Piotr'
'Stilinović, Vladimir'
'Kirillov, Alexander M.'
'Kennedy, Alan'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Metal--organic and supramolecular lead(ii) networks assembled from
 isomeric nicotinoylhydrazone blocks: the effects of ligand geometry and
 counter-ion on topology and supramolecular assembly
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5375
_journal_paper_doi               10.1039/C6CE00900J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C13 H12 Cl2 N4 O Pb'
_chemical_formula_sum            'C13 H12 Cl2 N4 O Pb'
_chemical_formula_weight         518.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                100.321(4)
_cell_angle_beta                 92.891(5)
_cell_angle_gamma                95.189(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8658(7)
_cell_length_b                   8.6864(7)
_cell_length_c                   11.0020(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      2.61
_cell_measurement_theta_min      37.99
_cell_volume                     734.82(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18736
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    11.846
_exptl_absorpt_correction_T_max  0.4868
_exptl_absorpt_correction_T_min  0.2283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+0.5894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0439
_reflns_number_gt                3524
_reflns_number_total             3653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00900j2.cif
_cod_data_source_block           4
_cod_database_code               7226171
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C17 C 0.0653(4) 0.8567(3) 0.3425(3) 0.0172(5) Uani 1 1 d .
H17 H 0.1804 0.8481 0.3222 0.021 Uiso 1 1 calc R
C16 C 0.0056(3) 0.7833(3) 0.4371(2) 0.0147(5) Uani 1 1 d .
C15 C -0.1637(4) 0.7989(3) 0.4662(3) 0.0174(5) Uani 1 1 d .
H15 H -0.2095 0.7524 0.5309 0.021 Uiso 1 1 calc R
C14 C -0.2641(4) 0.8825(3) 0.4001(3) 0.0195(5) Uani 1 1 d .
H14 H -0.3797 0.8932 0.4182 0.023 Uiso 1 1 calc R
C13 C -0.1932(4) 0.9507(3) 0.3067(3) 0.0179(5) Uani 1 1 d .
H13 H -0.2625 1.0076 0.2611 0.022 Uiso 1 1 calc R
N3 N -0.0310(3) 0.9389(3) 0.2787(2) 0.0183(5) Uani 1 1 d .
Pb1 Pb 0.123191(11) 0.154650(10) 1.158861(8) 0.01335(5) Uani 1 1 d .
Cl1 Cl 0.18937(9) -0.11471(8) 1.00360(7) 0.02072(14) Uani 1 1 d .
Cl3 Cl 0.44384(9) 0.19037(10) 1.28796(7) 0.02732(16) Uani 1 1 d .
O1 O -0.0287(2) 0.5389(2) 0.80024(18) 0.0178(4) Uani 1 1 d .
N1 N 0.2655(3) 0.2843(3) 0.9902(2) 0.0174(5) Uani 1 1 d .
N5 N 0.0736(3) 0.6780(3) 0.6137(2) 0.0158(4) Uani 1 1 d .
N6 N 0.1843(3) 0.6022(3) 0.6801(2) 0.0167(5) Uani 1 1 d .
H6 H 0.2893 0.6108 0.6685 0.020 Uiso 1 1 d R
C1 C 0.4283(4) 0.2691(3) 0.9630(3) 0.0179(5) Uani 1 1 d .
H1 H 0.4925 0.2044 1.0048 0.022 Uiso 1 1 calc R
C2 C 0.5065(4) 0.3444(3) 0.8760(3) 0.0187(5) Uani 1 1 d .
H2 H 0.6225 0.3326 0.8598 0.022 Uiso 1 1 calc R
C3 C 0.2420(3) 0.4515(3) 0.8397(2) 0.0133(5) Uani 1 1 d .
C4 C 0.1755(3) 0.3729(3) 0.9286(2) 0.0147(5) Uani 1 1 d .
H4 H 0.0597 0.3824 0.9468 0.018 Uiso 1 1 calc R
C5 C 0.4127(4) 0.4369(3) 0.8135(3) 0.0170(5) Uani 1 1 d .
H5 H 0.4635 0.4896 0.7538 0.020 Uiso 1 1 calc R
C6 C 0.1213(3) 0.5370(3) 0.7743(2) 0.0131(5) Uani 1 1 d .
C23 C 0.1197(3) 0.6977(3) 0.5060(2) 0.0149(5) Uani 1 1 d .
C24 C 0.2761(4) 0.6394(4) 0.4473(3) 0.0211(6) Uani 1 1 d .
H24A H 0.3728 0.7209 0.4691 0.032 Uiso 1 1 calc R
H24B H 0.2540 0.6148 0.3571 0.032 Uiso 1 1 calc R
H24C H 0.3035 0.5444 0.4776 0.032 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 '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
N3 C17 C16 123.6(3) . .
N3 C17 H17 118.2 . .
C16 C17 H17 118.2 . .
C17 C16 C15 117.2(2) . .
C17 C16 C23 120.9(2) . .
C15 C16 C23 121.9(2) . .
C14 C15 C16 119.5(3) . .
C14 C15 H15 120.2 . .
C16 C15 H15 120.2 . .
C15 C14 C13 119.0(3) . .
C15 C14 H14 120.5 . .
C13 C14 H14 120.5 . .
N3 C13 C14 122.3(3) . .
N3 C13 H13 118.9 . .
C14 C13 H13 118.9 . .
C13 N3 C17 118.4(3) . .
C13 N3 Pb1 118.65(18) . 1_564
C17 N3 Pb1 119.53(19) . 1_564
N1 Pb1 N3 162.10(8) . 1_546
N1 Pb1 Cl1 81.80(5) . .
N3 Pb1 Cl1 80.93(5) 1_546 .
N1 Pb1 Cl3 88.25(6) . .
N3 Pb1 Cl3 97.45(6) 1_546 .
Cl1 Pb1 Cl3 93.36(2) . .
N1 Pb1 Cl1 85.63(6) . 2_557
N3 Pb1 Cl1 87.43(6) 1_546 2_557
Cl1 Pb1 Cl1 82.40(2) . 2_557
Cl3 Pb1 Cl1 172.99(2) . 2_557
Pb1 Cl1 Pb1 97.60(2) . 2_557
C4 N1 C1 118.1(2) . .
C4 N1 Pb1 119.22(18) . .
C1 N1 Pb1 122.70(18) . .
C23 N5 N6 115.7(2) . .
C6 N6 N5 117.8(2) . .
C6 N6 H6 122.2 . .
N5 N6 H6 119.2 . .
N1 C1 C2 122.5(3) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C5 C2 C1 119.0(3) . .
C5 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C4 C3 C5 117.8(2) . .
C4 C3 C6 116.7(2) . .
C5 C3 C6 125.3(2) . .
N1 C4 C3 123.6(2) . .
N1 C4 H4 118.2 . .
C3 C4 H4 118.2 . .
C2 C5 C3 119.0(3) . .
C2 C5 H5 120.5 . .
C3 C5 H5 120.5 . .
O1 C6 N6 122.8(2) . .
O1 C6 C3 121.0(2) . .
N6 C6 C3 116.1(2) . .
N5 C23 C16 115.8(2) . .
N5 C23 C24 125.1(3) . .
C16 C23 C24 119.1(2) . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C17 N3 1.341(4) .
C17 C16 1.394(4) .
C17 H17 0.9500 .
C16 C15 1.398(4) .
C16 C23 1.479(4) .
C15 C14 1.384(4) .
C15 H15 0.9500 .
C14 C13 1.391(4) .
C14 H14 0.9500 .
C13 N3 1.336(4) .
C13 H13 0.9500 .
N3 Pb1 2.712(2) 1_564
Pb1 N1 2.588(2) .
Pb1 N3 2.712(2) 1_546
Pb1 Cl1 2.7461(7) .
Pb1 Cl3 2.7954(8) .
Pb1 Cl1 2.9223(7) 2_557
Cl1 Pb1 2.9223(7) 2_557
O1 C6 1.229(3) .
N1 C4 1.337(3) .
N1 C1 1.342(4) .
N5 C23 1.292(4) .
N5 N6 1.391(3) .
N6 C6 1.361(3) .
N6 H6 0.8409 .
C1 C2 1.390(4) .
C1 H1 0.9500 .
C2 C5 1.384(4) .
C2 H2 0.9500 .
C3 C4 1.387(4) .
C3 C5 1.400(4) .
C3 C6 1.489(4) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C23 C24 1.504(4) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
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
N3 C17 C16 C15 -0.6(4) . .
N3 C17 C16 C23 -178.5(2) . .
C17 C16 C15 C14 1.0(4) . .
C23 C16 C15 C14 178.9(2) . .
C16 C15 C14 C13 -0.6(4) . .
C15 C14 C13 N3 -0.3(4) . .
C14 C13 N3 C17 0.8(4) . .
C14 C13 N3 Pb1 -158.3(2) . 1_564
C16 C17 N3 C13 -0.3(4) . .
C16 C17 N3 Pb1 158.6(2) . 1_564
N1 Pb1 Cl1 Pb1 -86.65(6) . 2_557
N3 Pb1 Cl1 Pb1 88.59(6) 1_546 2_557
Cl3 Pb1 Cl1 Pb1 -174.39(2) . 2_557
Cl1 Pb1 Cl1 Pb1 0.0 2_557 2_557
N3 Pb1 N1 C4 103.7(3) 1_546 .
Cl1 Pb1 N1 C4 119.1(2) . .
Cl3 Pb1 N1 C4 -147.2(2) . .
Cl1 Pb1 N1 C4 36.20(19) 2_557 .
N3 Pb1 N1 C1 -77.6(3) 1_546 .
Cl1 Pb1 N1 C1 -62.2(2) . .
Cl3 Pb1 N1 C1 31.5(2) . .
Cl1 Pb1 N1 C1 -145.1(2) 2_557 .
C23 N5 N6 C6 -160.8(2) . .
C4 N1 C1 C2 1.5(4) . .
Pb1 N1 C1 C2 -177.2(2) . .
N1 C1 C2 C5 -1.0(4) . .
C1 N1 C4 C3 -1.0(4) . .
Pb1 N1 C4 C3 177.8(2) . .
C5 C3 C4 N1 -0.1(4) . .
C6 C3 C4 N1 176.3(2) . .
C1 C2 C5 C3 -0.1(4) . .
C4 C3 C5 C2 0.6(4) . .
C6 C3 C5 C2 -175.4(2) . .
N5 N6 C6 O1 1.9(4) . .
N5 N6 C6 C3 177.6(2) . .
C4 C3 C6 O1 1.2(4) . .
C5 C3 C6 O1 177.2(3) . .
C4 C3 C6 N6 -174.6(2) . .
C5 C3 C6 N6 1.5(4) . .
N6 N5 C23 C16 -177.8(2) . .
N6 N5 C23 C24 2.9(4) . .
C17 C16 C23 N5 158.7(3) . .
C15 C16 C23 N5 -19.1(4) . .
C17 C16 C23 C24 -22.0(4) . .
C15 C16 C23 C24 160.2(3) . .
