#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:52:29 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179676 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/28/4512844.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_4512844
loop_
_publ_author_name
'Gabriel, Catherine'
'Karakosta, Paraskevi'
'Vangelis, Angelos A.'
'Raptopoulou, Catherine P.'
'Terzis, Aris'
'Psycharis, Vassilis'
'Bertmer, Marko'
'Mateescu, Constantin'
'Salifoglou, Athanasios'
_publ_section_title
;
 pH-Specific Crystalline Binary and Ternary Metal--Organic Framework
 Materials of Pb(II) with (Di)Tricarboxylate Ligands
 andN,N′-Aromatic Chelators. Structure, Architecture-Lattice
 Dimensionality, and Electronic Spectroscopic Property Correlations
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1666
_journal_paper_doi               10.1021/cg501628d
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C36 H30 N4 O13 Pb2'
_chemical_formula_weight         1141.02
_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                115.1450(10)
_cell_angle_beta                 98.2720(10)
_cell_angle_gamma                92.3460(10)
_cell_formula_units_Z            1
_cell_length_a                   7.92540(10)
_cell_length_b                   10.74520(10)
_cell_length_c                   11.3467(2)
_cell_measurement_reflns_used    10490
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.75
_cell_measurement_theta_min      6.52
_cell_volume                     859.98(2)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10262
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.53
_exptl_absorpt_coefficient_mu    19.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.078
_refine_diff_density_min         -2.579
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+1.6063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                2602
_reflns_number_total             2688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501628d_si_004.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 4512844--4512847.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4512844
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
Pb1 Pb 0.11274(4) -0.12539(2) 0.10810(2) 0.02056(15) Uani 1 1 d .
N1 N 0.0668(9) 0.0894(6) 0.3087(6) 0.0233(17) Uani 1 1 d .
N2 N 0.2356(9) -0.1224(6) 0.3236(6) 0.0230(16) Uani 1 1 d .
C1 C -0.0182(13) 0.1925(8) 0.3031(9) 0.032(2) Uani 1 1 d .
H1 H -0.0655 0.1861 0.2187 0.042 Uiso 1 1 calc R
C2 C -0.0400(12) 0.3058(8) 0.4123(8) 0.031(2) Uani 1 1 d .
H2 H -0.0995 0.3772 0.4035 0.041 Uiso 1 1 calc R
C3 C 0.0250(13) 0.3164(8) 0.5361(9) 0.036(2) Uani 1 1 d .
H3 H 0.0078 0.3949 0.6124 0.046 Uiso 1 1 calc R
C4 C 0.1139(11) 0.2157(7) 0.5512(8) 0.024(2) Uani 1 1 d .
C5 C 0.1869(12) 0.2168(8) 0.6737(8) 0.031(2) Uani 1 1 d .
H5 H 0.1741 0.2929 0.7536 0.040 Uiso 1 1 calc R
C6 C 0.2715(13) 0.1165(8) 0.6810(8) 0.034(2) Uani 1 1 d .
H6 H 0.3208 0.1234 0.7653 0.044 Uiso 1 1 calc R
C7 C 0.2907(11) -0.0039(8) 0.5628(8) 0.025(2) Uani 1 1 d .
C8 C 0.3812(12) -0.1121(9) 0.5674(8) 0.033(2) Uani 1 1 d .
H8 H 0.4325 -0.1093 0.6496 0.043 Uiso 1 1 calc R
C9 C 0.3936(12) -0.2232(8) 0.4488(9) 0.032(2) Uani 1 1 d .
H9 H 0.4532 -0.2983 0.4485 0.041 Uiso 1 1 calc R
C10 C 0.3183(11) -0.2230(7) 0.3314(8) 0.024(2) Uani 1 1 d .
H10 H 0.3268 -0.3004 0.2512 0.031 Uiso 1 1 calc R
C11 C 0.2205(11) -0.0120(7) 0.4389(7) 0.0223(19) Uani 1 1 d .
C12 C 0.1320(11) 0.0984(7) 0.4306(7) 0.0219(19) Uani 1 1 d .
O21 O 0.3099(8) -0.3065(5) 0.0372(5) 0.0305(15) Uani 1 1 d .
O22 O 0.1449(9) -0.4428(7) -0.1565(6) 0.049(2) Uani 1 1 d .
O23 O 0.8014(9) -0.0778(6) -0.0297(6) 0.0396(17) Uani 1 1 d .
O24 O 0.6273(8) -0.0111(5) -0.1541(5) 0.0306(15) Uani 1 1 d .
O25 O 0.8629(8) -0.3981(6) -0.0699(6) 0.0345(16) Uani 1 1 d .
H25O H 0.931(13) -0.460(10) -0.120(9) 0.045 Uiso 1 1 d .
O26 O 0.7531(9) -0.4188(7) -0.2710(6) 0.0435(17) Uani 1 1 d .
C21 C 0.2879(12) -0.3944(8) -0.0819(8) 0.025(2) Uani 1 1 d .
C22 C 0.4440(11) -0.4429(7) -0.1405(7) 0.0210(18) Uani 1 1 d .
H22A H 0.4123 -0.4870 -0.2382 0.029 Uiso 1 1 calc R
H22B H 0.4869 -0.5135 -0.1130 0.029 Uiso 1 1 calc R
C23 C 0.5866(11) -0.3250(8) -0.0978(8) 0.022(2) Uani 1 1 d .
H23 H 0.6182 -0.2810 0.0009 0.029 Uiso 1 1 calc R
C24 C 0.7445(11) -0.3851(7) -0.1570(8) 0.0232(19) Uani 1 1 d .
C25 C 0.5306(12) -0.2165(7) -0.1416(8) 0.026(2) Uani 1 1 d .
H25A H 0.4283 -0.1808 -0.1030 0.036 Uiso 1 1 calc R
H25B H 0.4950 -0.2615 -0.2390 0.036 Uiso 1 1 calc R
C26 C 0.6648(12) -0.0936(7) -0.1044(7) 0.0249(19) Uani 1 1 d .
O1W O 0.586(2) -0.4931(16) -0.5292(15) 0.063(5) Uani 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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
O24 Pb1 O21 79.35(19) 2_655 .
O24 Pb1 N2 80.67(19) 2_655 .
O21 Pb1 N2 79.14(19) . .
O24 Pb1 N1 79.6(2) 2_655 .
O21 Pb1 N1 141.6(2) . .
N2 Pb1 N1 66.0(2) . .
C1 N1 C12 118.0(6) . .
C1 N1 Pb1 124.8(5) . .
C12 N1 Pb1 117.2(5) . .
C10 N2 C11 118.1(7) . .
C10 N2 Pb1 122.2(5) . .
C11 N2 Pb1 119.7(5) . .
N1 C1 C2 123.2(9) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C1 C2 C3 119.5(9) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C4 C3 C2 121.3(7) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 125.8(7) . .
C3 C4 C12 116.1(8) . .
C5 C4 C12 118.1(7) . .
C6 C5 C4 122.6(7) . .
C6 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
C5 C6 C7 121.1(8) . .
C5 C6 H6 119.4 . .
C7 C6 H6 119.4 . .
C11 C7 C8 118.5(7) . .
C11 C7 C6 119.1(8) . .
C8 C7 C6 122.4(8) . .
C9 C8 C7 118.4(8) . .
C9 C8 H8 120.8 . .
C7 C8 H8 120.8 . .
C10 C9 C8 119.1(8) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
N2 C10 C9 124.0(7) . .
N2 C10 H10 118.0 . .
C9 C10 H10 118.0 . .
N2 C11 C7 121.9(7) . .
N2 C11 C12 118.2(7) . .
C7 C11 C12 119.9(6) . .
N1 C12 C11 119.0(6) . .
N1 C12 C4 121.9(7) . .
C11 C12 C4 119.1(7) . .
C21 O21 Pb1 119.6(6) . .
C26 O24 Pb1 103.4(5) . 2_655
C24 O25 H25O 105(6) . .
O22 C21 O21 125.0(8) . .
O22 C21 C22 117.2(7) . .
O21 C21 C22 117.8(8) . .
C21 C22 C23 112.3(6) . .
C21 C22 H22A 109.1 . .
C23 C22 H22A 109.2 . .
C21 C22 H22B 109.1 . .
C23 C22 H22B 109.1 . .
H22A C22 H22B 107.9 . .
C25 C23 C22 111.5(7) . .
C25 C23 C24 110.2(7) . .
C22 C23 C24 108.7(6) . .
C25 C23 H23 108.8 . .
C22 C23 H23 108.8 . .
C24 C23 H23 108.8 . .
O26 C24 O25 125.1(8) . .
O26 C24 C23 122.4(9) . .
O25 C24 C23 112.5(7) . .
C23 C25 C26 115.8(7) . .
C23 C25 H25A 108.3 . .
C26 C25 H25A 108.3 . .
C23 C25 H25B 108.3 . .
C26 C25 H25B 108.3 . .
H25A C25 H25B 107.4 . .
O23 C26 O24 122.7(7) . .
O23 C26 C25 120.9(7) . .
O24 C26 C25 116.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O24 2.336(5) 2_655
Pb1 O21 2.481(6) .
Pb1 N2 2.485(6) .
Pb1 N1 2.546(6) .
N1 C1 1.340(11) .
N1 C12 1.366(10) .
N2 C10 1.315(10) .
N2 C11 1.367(8) .
C1 C2 1.358(11) .
C1 H1 0.9500 .
C2 C3 1.379(12) .
C2 H2 0.9500 .
C3 C4 1.372(12) .
C3 H3 0.9500 .
C4 C5 1.422(12) .
C4 C12 1.445(9) .
C5 C6 1.318(13) .
C5 H5 0.9500 .
C6 C7 1.448(11) .
C6 H6 0.9500 .
C7 C11 1.400(11) .
C7 C8 1.406(13) .
C8 C9 1.389(11) .
C8 H8 0.9500 .
C9 C10 1.380(12) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.433(11) .
O21 C21 1.258(9) .
O22 C21 1.255(11) .
O23 C26 1.232(10) .
O24 C26 1.262(9) .
O24 Pb1 2.336(5) 2_655
O25 C24 1.318(10) .
O25 H25O 0.92(10) .
O26 C24 1.200(9) .
C21 C22 1.496(11) .
C22 C23 1.523(10) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C25 1.508(11) .
C23 C24 1.541(11) .
C23 H23 1.0000 .
C25 C26 1.528(10) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
O1W O1W 1.62(3) 2_644
