#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:00:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180407 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/76/7207632.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_7207632
loop_
_publ_author_name
'Martínez Casado, Francisco Javier'
'Cañadillas-Delgado, Laura'
'Cucinotta, Fabio'
'Guerrero-Martínez, Andrés'
'Ramos Riesco, Miguel'
'Marchese, Leonardo'
'Rodríguez Cheda, José Antonio'
_publ_section_title
;
 Luminescent lead(ii) complexes: new three-dimensional mixed ligand MOFs
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2660
_journal_paper_doi               10.1039/c2ce06546k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         2(Pb+2),4(C4O2H7-),(C12H10N2),(H2O)
_chemical_formula_sum            'C28 H40 N2 O9 Pb2'
_chemical_formula_weight         963.03
_chemical_name_common
;
aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate
;
_chemical_name_systematic
;
aqua-1,2-bis(4-pyridyl)ethene-dilead(II) tetrabutyrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.479(4)
_cell_length_b                   22.360(5)
_cell_length_c                   8.2480(16)
_cell_measurement_temperature    298(2)
_cell_volume                     3349.4(13)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'CCD Server Software Huber'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Mercury 1.4.2. and ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9.77
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  ADSCq210rCCD-HUBER
_diffrn_measurement_method       'f\ scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.73790
_diffrn_reflns_av_R_equivalents  0.1154
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            42581
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    10.736
_exptl_absorpt_correction_T_max  0.7742
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1831
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.00227(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3973
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0309
_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)+(0.0411P)²+5.8167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                3691
_reflns_number_total             3973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06546k.txt
_cod_data_source_block           PbC4_4,4'-bipy_298K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3349.4(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7207632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
O4 O 0.4910(2) 0.3911(2) 0.4525(4) 0.0725(10) Uani 1 1 d .
O1 O 0.33472(19) 0.47824(16) 0.4567(5) 0.0660(9) Uani 1 1 d .
O3 O 0.4022(2) 0.33695(15) 0.3107(4) 0.0671(9) Uani 1 1 d .
O2 O 0.2677(2) 0.4251(2) 0.2647(5) 0.0737(10) Uani 1 1 d .
C6 C 0.2602(3) 0.3401(2) -0.0376(6) 0.0602(11) Uani 1 1 d .
H6 H 0.2408 0.3393 0.0587 0.072 Uiso 1 1 calc R
C11 C 0.2745(3) 0.4558(2) 0.3927(6) 0.0555(10) Uani 1 1 d .
C15 C 0.4597(3) 0.3416(2) 0.4169(6) 0.0634(12) Uani 1 1 d .
C16 C 0.5016(8) 0.2913(4) 0.5088(12) 0.186(7) Uani 1 1 d D
H16A H 0.5532 0.2996 0.5099 0.223 Uiso 1 1 calc R
H16B H 0.4946 0.2950 0.6221 0.223 Uiso 1 1 calc R
C12 C 0.2081(3) 0.4659(4) 0.4708(9) 0.092(2) Uani 1 1 d .
H12A H 0.2202 0.4517 0.5836 0.111 Uiso 1 1 calc R
H12B H 0.2007 0.5088 0.4760 0.111 Uiso 1 1 calc R
C17 C 0.4914(8) 0.2298(4) 0.4679(18) 0.319(14) Uani 1 1 d D
H17A H 0.4894 0.2254 0.3501 0.383 Uiso 1 1 calc R
H17B H 0.4441 0.2173 0.4914 0.383 Uiso 1 1 calc R
C13 C 0.1394(6) 0.4401(7) 0.399(2) 0.214(10) Uani 1 1 d .
H13A H 0.1435 0.3969 0.4077 0.257 Uiso 1 1 calc R
H13B H 0.1289 0.4500 0.2821 0.257 Uiso 1 1 calc R
C18 C 0.5478(7) 0.1901(5) 0.5539(18) 0.192(7) Uani 1 1 d D
H18A H 0.5304 0.1496 0.5429 0.288 Uiso 1 1 calc R
H18B H 0.5589 0.2007 0.6686 0.288 Uiso 1 1 calc R
H18C H 0.5915 0.1936 0.5071 0.288 Uiso 1 1 calc R
C14 C 0.0786(9) 0.4597(12) 0.473(4) 0.43(3) Uani 1 1 d .
H14A H 0.0359 0.4360 0.4315 0.652 Uiso 1 1 calc R
H14B H 0.0683 0.5010 0.4470 0.652 Uiso 1 1 calc R
H14C H 0.0913 0.4550 0.5908 0.652 Uiso 1 1 calc R
Pb1 Pb 0.386328(8) 0.437554(6) 0.195282(15) 0.04209(10) Uani 1 1 d .
O1W O 0.5000 0.5399(2) 0.2500 0.0612(11) Uani 1 2 d S
C5 C 0.2371(2) 0.2531(2) -0.4310(5) 0.0522(9) Uani 1 1 d .
H5 H 0.2005 0.2269 -0.4118 0.063 Uiso 1 1 calc R
C3 C 0.2627(2) 0.29900(18) -0.3061(5) 0.0454(8) Uani 1 1 d .
C2 C 0.3148(2) 0.34214(19) -0.3202(5) 0.0493(9) Uani 1 1 d .
H2 H 0.3339 0.3452 -0.4167 0.059 Uiso 1 1 calc R
C1 C 0.3384(2) 0.38063(19) -0.1907(5) 0.0515(9) Uani 1 1 d .
H1 H 0.3739 0.4089 -0.2023 0.062 Uiso 1 1 calc R
N1 N 0.3129(2) 0.37945(17) -0.0494(4) 0.0514(8) Uani 1 1 d .
C4 C 0.2332(3) 0.3009(2) -0.1610(6) 0.0589(11) Uani 1 1 d .
H4 H 0.1950 0.2752 -0.1488 0.071 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 0.0030 0.0020 '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 0.0070 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0120 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.1460 10.7510 '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
C15 O4 Pb1 85.7(3) . .
C11 O1 Pb1 86.9(3) . .
C11 O1 Pb1 137.7(3) . 6_566
Pb1 O1 Pb1 132.75(14) . 6_566
C15 O3 Pb1 102.8(3) . .
C11 O2 Pb1 100.7(3) . .
N1 C6 C4 122.8(4) . .
N1 C6 H6 118.6 . .
C4 C6 H6 118.6 . .
O1 C11 O2 121.5(5) . .
O1 C11 C12 119.6(5) . .
O2 C11 C12 118.9(5) . .
O1 C11 Pb1 67.6(3) . .
O2 C11 Pb1 54.2(3) . .
C12 C11 Pb1 171.2(4) . .
O3 C15 O4 122.1(4) . .
O3 C15 C16 125.9(7) . .
O4 C15 C16 111.9(7) . .
O3 C15 Pb1 53.0(2) . .
O4 C15 Pb1 69.3(3) . .
C16 C15 Pb1 172.2(5) . .
C17 C16 C15 125.2(9) . .
C17 C16 H16A 106.0 . .
C15 C16 H16A 106.0 . .
C17 C16 H16B 106.0 . .
C15 C16 H16B 106.0 . .
H16A C16 H16B 106.3 . .
C13 C12 C11 119.7(7) . .
C13 C12 H12A 107.4 . .
C11 C12 H12A 107.4 . .
C13 C12 H12B 107.4 . .
C11 C12 H12B 107.4 . .
H12A C12 H12B 106.9 . .
C16 C17 C18 115.1(8) . .
C16 C17 H17A 108.5 . .
C18 C17 H17A 108.5 . .
C16 C17 H17B 108.5 . .
C18 C17 H17B 108.5 . .
H17A C17 H17B 107.5 . .
C12 C13 C14 113.7(12) . .
C12 C13 H13A 108.8 . .
C14 C13 H13A 108.8 . .
C12 C13 H13B 108.8 . .
C14 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O2 Pb1 O3 81.23(15) . .
O2 Pb1 N1 75.73(12) . .
O3 Pb1 N1 81.27(12) . .
O2 Pb1 O1 50.57(11) . .
O3 Pb1 O1 91.94(12) . .
N1 Pb1 O1 126.22(12) . .
O2 Pb1 O1 92.24(14) . 6_565
O3 Pb1 O1 155.13(12) . 6_565
N1 Pb1 O1 73.86(12) . 6_565
O1 Pb1 O1 102.41(7) . 6_565
O2 Pb1 O4 108.22(14) . .
O3 Pb1 O4 49.04(13) . .
N1 Pb1 O4 126.89(13) . .
O1 Pb1 O4 79.27(12) . .
O1 Pb1 O4 153.34(12) 6_565 .
O2 Pb1 C11 25.10(13) . .
O3 Pb1 C11 87.53(13) . .
N1 Pb1 C11 100.69(13) . .
O1 Pb1 C11 25.53(12) . .
O1 Pb1 C11 96.69(12) 6_565 .
O4 Pb1 C11 95.25(13) . .
O2 Pb1 C15 95.93(16) . .
O3 Pb1 C15 24.19(14) . .
N1 Pb1 C15 103.46(15) . .
O1 Pb1 C15 86.57(12) . .
O1 Pb1 C15 170.50(12) 6_565 .
O4 Pb1 C15 24.92(14) . .
C11 Pb1 C15 92.76(13) . .
C5 C5 C3 123.8(5) 7_554 .
C5 C5 H5 118.1 7_554 .
C3 C5 H5 118.1 . .
C2 C3 C4 115.9(4) . .
C2 C3 C5 124.6(4) . .
C4 C3 C5 119.5(4) . .
C1 C2 C3 119.7(4) . .
C1 C2 H2 120.2 . .
C3 C2 H2 120.2 . .
N1 C1 C2 123.5(4) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C6 N1 C1 117.3(3) . .
C6 N1 Pb1 124.4(3) . .
C1 N1 Pb1 117.1(3) . .
C6 C4 C3 120.6(4) . .
C6 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 C15 1.258(7) .
O4 Pb1 2.794(4) .
O1 C11 1.246(6) .
O1 Pb1 2.673(4) .
O1 Pb1 2.763(3) 6_566
O3 C15 1.251(7) .
O3 Pb1 2.439(3) .
O2 C11 1.246(6) .
O2 Pb1 2.382(4) .
C6 N1 1.329(6) .
C6 C4 1.366(6) .
C6 H6 0.9300 .
C11 C12 1.504(7) .
C11 Pb1 2.887(5) .
C15 C16 1.492(9) .
C15 Pb1 2.977(5) .
C16 C17 1.4190(11) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C12 C13 1.421(11) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C17 C18 1.452(2) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C13 C14 1.446(18) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
Pb1 N1 2.568(3) .
Pb1 O1 2.763(3) 6_565
C5 C5 1.321(9) 7_554
C5 C3 1.469(5) .
C5 H5 0.9300 .
C3 C2 1.383(5) .
C3 C4 1.404(6) .
C2 C1 1.379(5) .
C2 H2 0.9300 .
C1 N1 1.335(5) .
C1 H1 0.9300 .
C4 H4 0.9300 .
