#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:19:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180034 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/28/7032848.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_7032848
loop_
_publ_author_name
'Karmakar, Anirban'
'Hazra, Susanta'
'Guedes da Silva, M Fátima C'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Synthesis, structure and catalytic application of lead(II) complexes in
 cyanosilylation reactions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              268
_journal_page_last               280
_journal_paper_doi               10.1039/c4dt02316a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C14 H16 N8 O10 Pb2'
_chemical_formula_weight         870.73
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                102.495(2)
_cell_angle_beta                 99.181(2)
_cell_angle_gamma                112.272(3)
_cell_formula_units_Z            1
_cell_length_a                   7.6846(4)
_cell_length_b                   8.0250(4)
_cell_length_c                   10.1201(5)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.88
_cell_volume                     543.33(5)
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(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       'φ and ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    15.544
_exptl_absorpt_correction_T_max  0.065
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_description       Block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.756
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0187
_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)+(0.0258P)²+0.6103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2167
_reflns_number_total             2225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02316a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7032845--7032850.cif.'
_cod_database_code               7032848
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.093
_shelx_estimated_absorpt_t_max   0.178
_shelxl_version_number           2014-1
#END Tags that were not found in dictionaries
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 0.10389(2) 0.25480(2) 0.16115(2) 0.02922(6) Uani 1 1 d . .
O2 O 0.3680(4) 0.0044(4) -0.1473(3) 0.0404(7) Uani 1 1 d . .
O3 O 0.2444(5) 0.1096(4) 0.2924(3) 0.0432(7) Uani 1 1 d . .
O4 O 0.0334(6) 0.1589(6) 0.4021(4) 0.0614(9) Uani 1 1 d . .
O1 O 0.1695(4) 0.0748(4) -0.0328(3) 0.0331(6) Uani 1 1 d . .
O5 O 0.3006(7) 0.5605(6) 0.3878(4) 0.0823(14) Uani 1 1 d . .
N4 N 0.3189(6) 0.7635(6) 0.5840(5) 0.0574(11) Uani 1 1 d . .
H4A H 0.4387 0.7936 0.6242 0.069 Uiso 1 1 calc R U
H4B H 0.2542 0.8140 0.6262 0.069 Uiso 1 1 calc R U
N1 N 0.4647(4) 0.3885(4) 0.1452(3) 0.0283(6) Uani 1 1 d . .
N2 N 0.8364(4) 0.5240(5) 0.1070(4) 0.0346(7) Uani 1 1 d . .
N3 N 0.7424(5) 0.2692(5) -0.0865(4) 0.0390(8) Uani 1 1 d . .
H3A H 0.8591 0.3168 -0.0955 0.047 Uiso 1 1 calc R U
H3B H 0.6565 0.1636 -0.1452 0.047 Uiso 1 1 calc R U
C2 C 0.5033(5) 0.2904(5) 0.0396(3) 0.0246(6) Uani 1 1 d . .
C1 C 0.3373(5) 0.1089(5) -0.0550(4) 0.0271(7) Uani 1 1 d . .
C4 C 0.7915(5) 0.6158(5) 0.2120(4) 0.0368(8) Uani 1 1 d . .
H4 H 0.8887 0.7286 0.2744 0.044 Uiso 1 1 calc R U
C3 C 0.6075(6) 0.5518(6) 0.2329(4) 0.0351(8) Uani 1 1 d . .
H3 H 0.5823 0.6215 0.3074 0.042 Uiso 1 1 calc R U
C6 C 0.1623(7) 0.1074(6) 0.3924(5) 0.0440(10) Uani 1 1 d . .
H6 H 0.2038 0.0631 0.4632 0.053 Uiso 1 1 calc R U
C5 C 0.6946(5) 0.3590(5) 0.0186(4) 0.0277(7) Uani 1 1 d . .
C7 C 0.2385(9) 0.6456(10) 0.4634(5) 0.0628(14) Uani 1 1 d . .
H7 H 0.1091 0.6208 0.4274 0.075 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'
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
O3 Pb1 O1 84.03(10) . .
O3 Pb1 O1 86.68(10) . 2
O1 Pb1 O1 65.25(9) . 2
O3 Pb1 N1 76.68(10) . .
O1 Pb1 N1 64.03(9) . .
O1 Pb1 N1 127.78(8) 2 .
O3 Pb1 O5 84.13(15) . .
O1 Pb1 O5 138.76(11) . .
O1 Pb1 O5 152.58(11) 2 .
N1 Pb1 O5 74.82(11) . .
C6 O3 Pb1 102.2(3) . .
C1 O1 Pb1 126.0(2) . .
C1 O1 Pb1 117.1(2) . 2
Pb1 O1 Pb1 114.75(9) . 2
C7 O5 Pb1 128.9(4) . .
C7 N4 H4A 120.0 . .
C7 N4 H4B 120.0 . .
H4A N4 H4B 120.0 . .
C2 N1 C3 119.3(3) . .
C2 N1 Pb1 116.7(2) . .
C3 N1 Pb1 123.9(2) . .
C4 N2 C5 117.8(3) . .
C5 N3 H3A 120.0 . .
C5 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
N1 C2 C5 120.3(3) . .
N1 C2 C1 116.8(3) . .
C5 C2 C1 122.9(3) . .
O2 C1 O1 124.2(3) . .
O2 C1 C2 119.7(3) . .
O1 C1 C2 116.1(3) . .
N2 C4 C3 123.0(3) . .
N2 C4 H4 118.5 . .
C3 C4 H4 118.5 . .
N1 C3 C4 119.8(4) . .
N1 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
O4 C6 O3 124.9(4) . .
O4 C6 H6 117.5 . .
O3 C6 H6 117.5 . .
N3 C5 N2 116.9(3) . .
N3 C5 C2 123.4(3) . .
N2 C5 C2 119.7(3) . .
O5 C7 N4 130.7(6) . .
O5 C7 H7 114.6 . .
N4 C7 H7 114.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O3 2.335(3) .
Pb1 O1 2.415(2) .
Pb1 O1 2.555(2) 2
Pb1 N1 2.613(3) .
Pb1 O5 2.686(4) .
O2 C1 1.230(4) .
O3 C6 1.275(5) .
O4 C6 1.219(6) .
O1 C1 1.281(4) .
O1 Pb1 2.555(2) 2
O5 C7 1.190(6) .
N4 C7 1.258(7) .
N4 H4A 0.8600 .
N4 H4B 0.8600 .
N1 C2 1.328(4) .
N1 C3 1.344(5) .
N2 C4 1.327(5) .
N2 C5 1.350(5) .
N3 C5 1.334(5) .
N3 H3A 0.8600 .
N3 H3B 0.8600 .
C2 C5 1.430(5) .
C2 C1 1.505(4) .
C4 C3 1.378(5) .
C4 H4 0.9300 .
C3 H3 0.9300 .
C6 H6 0.9300 .
C7 H7 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A O3 0.86 2.21 3.063(5) 172.7 2_666
N4 H4B O2 0.86 2.28 2.850(5) 124.1 1_566
N4 H4B O4 0.86 2.28 3.016(6) 143.6 2_566
N3 H3A N2 0.86 2.24 3.093(4) 172.9 2_765
N3 H3B O2 0.86 2.09 2.721(4) 129.5 .
C3 H3 O5 0.93 2.35 3.047(6) 131.5 .
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
C3 N1 C2 C5 -0.7(5) .
Pb1 N1 C2 C5 176.6(2) .
C3 N1 C2 C1 -179.9(3) .
Pb1 N1 C2 C1 -2.7(4) .
Pb1 O1 C1 O2 172.9(3) .
Pb1 O1 C1 O2 10.6(5) 2
Pb1 O1 C1 C2 -7.5(4) .
Pb1 O1 C1 C2 -169.8(2) 2
N1 C2 C1 O2 -174.0(3) .
C5 C2 C1 O2 6.7(5) .
N1 C2 C1 O1 6.4(5) .
C5 C2 C1 O1 -172.8(3) .
C5 N2 C4 C3 -1.0(6) .
C2 N1 C3 C4 0.3(6) .
Pb1 N1 C3 C4 -176.7(3) .
N2 C4 C3 N1 0.6(7) .
Pb1 O3 C6 O4 4.6(5) .
C4 N2 C5 N3 179.8(4) .
C4 N2 C5 C2 0.6(5) .
N1 C2 C5 N3 -178.9(4) .
C1 C2 C5 N3 0.3(6) .
N1 C2 C5 N2 0.2(5) .
C1 C2 C5 N2 179.4(3) .
Pb1 O5 C7 N4 164.1(6) .
