#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318810.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_4318810
loop_
_publ_author_name
'Joaquín Sanchiz'
'Pedro Esparza'
'Diego Villagra'
'Sixto Domínguez'
'Alfredo Mederos'
'Felipe Brito'
'Lorena Araujo'
'Agustin Sánchez'
'Juan Manuel Arrieta'
_publ_section_title
;
 Holo- and Hemidirected Lead(II) in the Polymeric
 [Pb4(μ-3,4-TDTA)2(H2O)2].4H2O Complex. N,N,N',N'-Tetraacetate Ligands
 Derived fromo-Phenylenediamines as Sequestering Agents for Lead(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6048
_journal_page_last               6055
_journal_paper_doi               10.1021/ic0201304
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H20 N2 O11 Pb2'
_chemical_formula_weight         818.73
_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
_cell_angle_alpha                74.410(10)
_cell_angle_beta                 75.26(2)
_cell_angle_gamma                69.61(2)
_cell_formula_units_Z            2
_cell_length_a                   8.911(3)
_cell_length_b                   9.601(2)
_cell_length_c                   13.052(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      5.
_cell_volume                     992.1(4)
_computing_cell_refinement       cad4
_computing_data_collection       cad4
_computing_data_reduction        xtal
_computing_molecular_graphics    ortep
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Cad4
_diffrn_measurement_method       'omega/2theta scans (0.8+0.35tg(theta))'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12301
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '1 hour'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.011
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prismatic Triangular'
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2mm
_refine_diff_density_max         2.602
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.134
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0344P)²+1.8955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4912
_reflns_number_total             5781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201304.cif
_cod_data_source_block           plomo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        ' C15 H20 N2 O11 Pb2'
_cod_database_code               4318810
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.11875(2) 0.59649(2) 0.365584(15) 0.02909(6) Uani 1 d . . .
C1 C 0.7163(8) 0.8431(9) -0.0603(6) 0.0517(17) Uani 1 d . . .
H1A H 0.7809 0.8344 -0.0089 0.053(6) Uiso 1 calc R . .
H1B H 0.6815 0.9468 -0.0970 0.053(6) Uiso 1 calc R . .
H1C H 0.7800 0.7806 -0.1119 0.053(6) Uiso 1 calc R . .
C2 C 0.5704(7) 0.7922(7) -0.0026(5) 0.0379(12) Uani 1 d . . .
C3 C 0.5400(6) 0.7488(6) 0.1095(5) 0.0318(10) Uani 1 d . . .
H3 H 0.6153 0.7462 0.1484 0.053(6) Uiso 1 calc R . .
C4 C 0.4008(6) 0.7093(5) 0.1652(4) 0.0238(8) Uani 1 d . . .
C5 C 0.2874(6) 0.7119(6) 0.1068(4) 0.0269(9) Uani 1 d . . .
C6 C 0.3203(7) 0.7538(7) -0.0061(4) 0.0367(12) Uani 1 d . . .
H6 H 0.2471 0.7545 -0.0460 0.053(6) Uiso 1 calc R . .
C7 C 0.4586(8) 0.7942(8) -0.0598(5) 0.0405(13) Uani 1 d . . .
H7 H 0.4766 0.8229 -0.1347 0.053(6) Uiso 1 calc R . .
N1 N 0.3763(5) 0.6682(5) 0.2822(3) 0.0237(7) Uani 1 d . . .
C8 C 0.3730(7) 0.7964(6) 0.3278(4) 0.0312(10) Uani 1 d . . .
H8A H 0.3181 0.8912 0.2845 0.053(6) Uiso 1 calc R . .
H8B H 0.4839 0.7955 0.3225 0.053(6) Uiso 1 calc R . .
C9 C 0.2882(8) 0.7901(7) 0.4448(5) 0.0359(11) Uani 1 d . . .
O1 O 0.2404(6) 0.6787(5) 0.4961(4) 0.0421(10) Uani 1 d . . .
O2 O 0.2742(8) 0.9007(6) 0.4850(4) 0.0587(14) Uani 1 d . . .
C10 C 0.5047(6) 0.5280(6) 0.3186(5) 0.0306(10) Uani 1 d . . .
H10A H 0.5003 0.5157 0.3954 0.053(6) Uiso 1 calc R . .
H10B H 0.6104 0.5386 0.2813 0.053(6) Uiso 1 calc R . .
C11 C 0.4866(6) 0.3885(6) 0.2975(4) 0.0296(10) Uani 1 d . . .
O3 O 0.3485(5) 0.3915(5) 0.2902(4) 0.0362(8) Uani 1 d . . .
O4 O 0.6111(5) 0.2763(5) 0.2903(4) 0.0447(11) Uani 1 d . . .
N2 N 0.1352(5) 0.6786(5) 0.1603(3) 0.0236(7) Uani 1 d . . .
C12 C -0.0053(6) 0.8186(6) 0.1446(5) 0.0288(10) Uani 1 d . . .
H12A H -0.1050 0.7907 0.1629 0.053(6) Uiso 1 calc R . .
H12B H 0.0071 0.8684 0.0691 0.053(6) Uiso 1 calc R . .
C13 C -0.0190(6) 0.9293(6) 0.2140(5) 0.0309(10) Uani 1 d . . .
O5 O 0.0237(6) 0.8782(5) 0.3039(4) 0.0403(9) Uani 1 d . . .
O6 O -0.0721(6) 1.0656(5) 0.1771(4) 0.0460(11) Uani 1 d . . .
C14 C 0.1158(6) 0.5591(6) 0.1171(4) 0.0300(10) Uani 1 d . . .
H14A H 0.2193 0.4805 0.1086 0.053(6) Uiso 1 calc R . .
H14B H 0.0863 0.6027 0.0461 0.053(6) Uiso 1 calc R . .
C15 C -0.0121(7) 0.4879(6) 0.1890(5) 0.0323(11) Uani 1 d . . .
O7 O -0.0674(6) 0.5095(6) 0.2839(4) 0.0454(11) Uani 1 d . . .
O8 O -0.0526(6) 0.4015(6) 0.1510(4) 0.0509(12) Uani 1 d . . .
Pb2 Pb -0.10737(2) 1.21033(2) 0.318057(16) 0.03023(6) Uani 1 d . . .
O1W O 0.2677(10) 0.3447(9) 0.5402(6) 0.091(2) Uani 1 d . . .
O2W O 0.1885(8) 1.1725(7) 0.3491(7) 0.081(2) Uani 1 d . . .
O3W O 0.3990(11) 0.0370(10) 0.6179(10) 0.122(4) Uani 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
O5 Pb1 O3 132.86(15) . . ?
O5 Pb1 N1 75.52(15) . . ?
O3 Pb1 N1 65.77(13) . . ?
O5 Pb1 N2 67.06(13) . . ?
O3 Pb1 N2 75.32(13) . . ?
N1 Pb1 N2 70.76(13) . . ?
O5 Pb1 O7 101.72(16) . . ?
O3 Pb1 O7 85.78(14) . . ?
N1 Pb1 O7 131.58(13) . . ?
N2 Pb1 O7 64.32(14) . . ?
O5 Pb1 O1 80.29(14) . . ?
O3 Pb1 O1 104.81(14) . . ?
N1 Pb1 O1 64.63(14) . . ?
N2 Pb1 O1 129.80(14) . . ?
O7 Pb1 O1 163.76(14) . . ?
C7 C2 C3 118.5(5) . . ?
C7 C2 C1 120.2(6) . . ?
C3 C2 C1 121.2(6) . . ?
C2 C3 C4 122.3(5) . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 N1 119.0(4) . . ?
C5 C4 N1 121.9(4) . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 N2 121.9(4) . . ?
C6 C5 N2 119.9(4) . . ?
C7 C6 C5 121.8(5) . . ?
C6 C7 C2 120.3(5) . . ?
C4 N1 C10 110.9(4) . . ?
C4 N1 C8 109.9(4) . . ?
C10 N1 C8 110.9(4) . . ?
C4 N1 Pb1 113.4(3) . . ?
C10 N1 Pb1 102.7(3) . . ?
C8 N1 Pb1 108.8(3) . . ?
N1 C8 C9 113.5(4) . . ?
O1 C9 O2 123.9(6) . . ?
O1 C9 C8 120.3(5) . . ?
O2 C9 C8 115.8(5) . . ?
C9 O1 Pb1 108.3(4) . . ?
C9 O1 Pb2 95.1(4) . 2_576 ?
Pb1 O1 Pb2 133.04(19) . 2_576 ?
C9 O2 Pb2 93.3(4) . 2_576 ?
N1 C10 C11 112.6(4) . . ?
O3 C11 O4 124.5(5) . . ?
O3 C11 C10 117.9(5) . . ?
O4 C11 C10 117.6(5) . . ?
C11 O3 Pb1 115.0(3) . . ?
C11 O4 Pb2 135.5(4) . 1_645 ?
C5 N2 C14 110.7(4) . . ?
C5 N2 C12 110.1(4) . . ?
C14 N2 C12 109.6(4) . . ?
C5 N2 Pb1 111.7(3) . . ?
C14 N2 Pb1 109.7(3) . . ?
C12 N2 Pb1 104.9(3) . . ?
N2 C12 C13 112.2(4) . . ?
O6 C13 O5 123.5(5) . . ?
O6 C13 C12 117.5(5) . . ?
O5 C13 C12 119.0(5) . . ?
C13 O5 Pb1 118.0(4) . . ?
C13 O6 Pb2 108.9(4) . . ?
N2 C14 C15 113.2(4) . . ?
O7 C15 O8 122.4(6) . . ?
O7 C15 C14 120.5(5) . . ?
O8 C15 C14 117.0(5) . . ?
C15 O7 Pb1 114.7(4) . . ?
C15 O8 Pb2 101.1(4) . 1_545 ?
O4 Pb2 O6 78.23(15) 1_465 . ?
O4 Pb2 O8 89.73(17) 1_465 1_565 ?
O6 Pb2 O8 80.00(16) . 1_565 ?
O4 Pb2 O2W 173.38(17) 1_465 . ?
O6 Pb2 O2W 106.7(2) . . ?
O8 Pb2 O2W 86.90(19) 1_565 . ?
O4 Pb2 O1 86.18(15) 1_465 2_576 ?
O6 Pb2 O1 158.08(16) . 2_576 ?
O8 Pb2 O1 115.56(15) 1_565 2_576 ?
O2W Pb2 O1 90.1(2) . 2_576 ?
O4 Pb2 O2 74.98(18) 1_465 2_576 ?
O6 Pb2 O2 112.61(16) . 2_576 ?
O8 Pb2 O2 156.99(18) 1_565 2_576 ?
O2W Pb2 O2 106.4(2) . 2_576 ?
O1 Pb2 O2 47.55(14) 2_576 2_576 ?
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
Pb1 O5 2.502(5) . ?
Pb1 O3 2.498(4) . ?
Pb1 N1 2.520(4) . ?
Pb1 N2 2.562(4) . ?
Pb1 O7 2.633(4) . ?
Pb1 O1 2.638(4) . ?
C1 C2 1.498(9) . ?
C2 C7 1.381(9) . ?
C2 C3 1.391(8) . ?
C3 C4 1.390(7) . ?
C4 C5 1.404(6) . ?
C4 N1 1.450(6) . ?
C5 C6 1.400(7) . ?
C5 N2 1.459(6) . ?
C6 C7 1.381(9) . ?
N1 C10 1.485(6) . ?
N1 C8 1.494(6) . ?
C8 C9 1.517(8) . ?
C9 O1 1.249(7) . ?
C9 O2 1.261(7) . ?
O1 Pb2 2.733(4) 2_576 ?
O2 Pb2 2.764(6) 2_576 ?
C10 C11 1.506(7) . ?
C11 O3 1.248(6) . ?
C11 O4 1.252(6) . ?
O4 Pb2 2.461(4) 1_645 ?
N2 C14 1.484(6) . ?
N2 C12 1.492(6) . ?
C12 C13 1.528(7) . ?
C13 O6 1.230(7) . ?
C13 O5 1.245(7) . ?
O6 Pb2 2.488(4) . ?
C14 C15 1.517(8) . ?
C15 O7 1.255(7) . ?
C15 O8 1.259(6) . ?
O8 Pb2 2.509(6) 1_545 ?
Pb2 O4 2.461(4) 1_465 ?
Pb2 O8 2.509(6) 1_565 ?
Pb2 O2W 2.654(6) . ?
Pb2 O1 2.733(4) 2_576 ?
Pb2 O2 2.764(6) 2_576 ?
