#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:19:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180034 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/28/7032847.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_7032847
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            'C20 H16 N12 O8 Pb2'
_chemical_formula_weight         966.83
_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                85.184(2)
_cell_angle_beta                 86.853(2)
_cell_angle_gamma                67.1140(10)
_cell_formula_units_Z            1
_cell_length_a                   7.7520(3)
_cell_length_b                   7.8081(3)
_cell_length_c                   11.2756(5)
_cell_measurement_reflns_used    6206
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.85
_cell_volume                     626.36(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0182
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7136
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    13.496
_exptl_absorpt_correction_T_max  0.06
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_description       Block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0214
_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)+(0.0310P)²+0.8235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2475
_reflns_number_total             2550
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02316a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7032845--7032850.cif.'
_cod_database_code               7032847
#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   0.103
_shelx_estimated_absorpt_t_max   0.173
_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 0.43976(2) 0.18447(2) 0.13204(2) 0.02970(7) Uani 1 1 d . .
O2 O 0.0894(4) 0.0714(4) -0.1343(3) 0.0360(6) Uani 1 1 d . .
O3 O 0.3917(5) -0.0533(4) 0.2392(3) 0.0391(7) Uani 1 1 d . .
O1 O 0.3182(4) 0.0853(4) -0.0290(3) 0.0356(6) Uani 1 1 d . .
N1 N 0.0759(4) 0.3166(5) 0.1192(3) 0.0264(6) Uani 1 1 d . .
N2 N -0.3064(4) 0.4731(5) 0.0816(3) 0.0304(7) Uani 1 1 d . .
N3 N -0.2672(5) 0.3149(5) -0.0873(3) 0.0366(8) Uani 1 1 d . .
H3A H -0.3858 0.3703 -0.0975 0.055 Uiso 1 1 calc R U
H3B H -0.1985 0.2375 -0.1372 0.055 Uiso 1 1 calc R U
O4 O 0.3016(7) -0.1785(5) 0.4030(4) 0.0601(11) Uani 1 1 d . .
N4 N 0.3389(5) 0.2574(5) 0.3506(3) 0.0337(7) Uani 1 1 d . .
C3 C -0.1891(5) 0.3494(5) 0.0068(3) 0.0259(7) Uani 1 1 d . .
C2 C 0.0070(5) 0.2687(5) 0.0274(3) 0.0243(7) Uani 1 1 d . .
C5 C -0.0414(6) 0.4391(6) 0.1926(4) 0.0304(8) Uani 1 1 d . .
H5 H 0.0052 0.4728 0.2572 0.036 Uiso 1 1 calc R U
C1 C 0.1457(5) 0.1313(5) -0.0525(3) 0.0274(7) Uani 1 1 d . .
N5 N 0.2069(7) 0.3087(6) 0.5826(4) 0.0460(10) Uani 1 1 d . .
C4 C -0.2323(6) 0.5154(6) 0.1723(4) 0.0315(8) Uani 1 1 d . .
H4 H -0.3112 0.5997 0.2243 0.038 Uiso 1 1 calc R U
N6 N 0.1973(7) 0.0178(6) 0.6006(4) 0.0542(11) Uani 1 1 d . .
H6A H 0.1592 0.0372 0.6732 0.081 Uiso 1 1 calc R U
H6B H 0.2123 -0.0860 0.5721 0.081 Uiso 1 1 calc R U
C6 C 0.3322(6) -0.0495(6) 0.3483(4) 0.0349(9) Uani 1 1 d . .
C7 C 0.3006(6) 0.1234(6) 0.4127(4) 0.0310(8) Uani 1 1 d . .
C8 C 0.2332(6) 0.1484(6) 0.5324(4) 0.0362(9) Uani 1 1 d . .
C10 C 0.3146(7) 0.4139(6) 0.4004(4) 0.0410(10) Uani 1 1 d . .
H10 H 0.3416 0.5077 0.3572 0.049 Uiso 1 1 calc R U
C9 C 0.2487(8) 0.4362(7) 0.5170(4) 0.0485(12) Uani 1 1 d . .
H9 H 0.2331 0.5461 0.5508 0.058 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 84.05(11) . .
O3 Pb1 O1 81.26(11) . 2_655
O1 Pb1 O1 66.26(11) . 2_655
O3 Pb1 N4 67.29(11) . .
O1 Pb1 N4 135.70(11) . .
O1 Pb1 N4 135.42(11) 2_655 .
O3 Pb1 N1 82.31(11) . .
O1 Pb1 N1 64.12(9) . .
O1 Pb1 N1 128.90(9) 2_655 .
N4 Pb1 N1 78.62(11) . .
C6 O3 Pb1 125.2(3) . .
C1 O1 Pb1 126.9(2) . .
C1 O1 Pb1 118.2(2) . 2_655
Pb1 O1 Pb1 113.74(11) . 2_655
C2 N1 C5 119.4(3) . .
C2 N1 Pb1 116.4(2) . .
C5 N1 Pb1 124.0(3) . .
C4 N2 C3 117.9(3) . .
C7 N4 C10 120.1(4) . .
C7 N4 Pb1 113.3(3) . .
C10 N4 Pb1 126.5(3) . .
N3 C3 N2 116.6(3) . .
N3 C3 C2 123.3(3) . .
N2 C3 C2 120.1(3) . .
N1 C2 C3 120.1(3) . .
N1 C2 C1 117.0(3) . .
C3 C2 C1 122.9(3) . .
N1 C5 C4 120.0(4) . .
O2 C1 O1 124.6(4) . .
O2 C1 C2 120.0(3) . .
O1 C1 C2 115.4(3) . .
C9 N5 C8 117.6(4) . .
N2 C4 C5 122.6(4) . .
O4 C6 O3 123.8(4) . .
O4 C6 C7 118.6(4) . .
O3 C6 C7 117.7(4) . .
N4 C7 C8 119.7(4) . .
N4 C7 C6 116.3(4) . .
C8 C7 C6 124.0(4) . .
N6 C8 N5 117.1(4) . .
N6 C8 C7 122.8(4) . .
N5 C8 C7 120.1(4) . .
N4 C10 C9 119.5(4) . .
N5 C9 C10 123.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O3 2.271(3) .
Pb1 O1 2.403(3) .
Pb1 O1 2.531(3) 2_655
Pb1 N4 2.585(3) .
Pb1 N1 2.608(3) .
O2 C1 1.239(5) .
O3 C6 1.288(5) .
O1 C1 1.279(5) .
O1 Pb1 2.531(3) 2_655
N1 C2 1.333(5) .
N1 C5 1.342(5) .
N2 C4 1.325(5) .
N2 C3 1.356(5) .
N3 C3 1.346(5) .
O4 C6 1.231(6) .
N4 C7 1.330(5) .
N4 C10 1.331(5) .
C3 C2 1.425(5) .
C2 C1 1.509(5) .
C5 C4 1.388(6) .
N5 C9 1.321(7) .
N5 C8 1.355(6) .
N6 C8 1.332(6) .
C6 C7 1.515(6) .
C7 C8 1.421(6) .
C10 C9 1.384(7) .
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
N3 H3A N2 0.86 2.22 3.067(5) 167.2 2_465
N3 H3B O2 0.86 2.10 2.731(5) 129.6 .
C5 H5 N4 0.93 2.69 3.282(5) 122.1 .
C5 H5 N5 0.93 2.62 3.235(6) 123.7 2_566
C4 H4 N5 0.93 2.61 3.236(6) 125.2 2_566
N6 H6A O2 0.86 2.22 3.078(5) 174.4 1_556
N6 H6B O4 0.86 2.08 2.716(6) 130.1 .
C10 H10 O4 0.93 2.44 3.147(5) 132.5 1_565
