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#$Date: 2016-03-25 09:18:57 +0100 (vie 25 de mar de 2016) $
#$Revision: 179747 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/43/7004308.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_7004308
loop_
_publ_author_name
'Aslani, Alireza'
'Morsali, Ali'
'Zeller, Matthias'
_publ_section_title
;
 Dynamic crystal-to-crystal conversion of a 3D--3D coordination polymer
 by de- and re-hydration
;
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              5173
_journal_page_last               5177
_journal_paper_doi               10.1039/b805367g
_journal_year                    2008
_chemical_formula_moiety         '(C6 H4 N O2)2 Pb'
_chemical_formula_sum            'C12 H8 N2 O4 Pb'
_chemical_formula_weight         451.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.595(1)
_cell_length_b                   10.028(1)
_cell_length_c                   14.635(1)
_cell_measurement_reflns_used    19872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2435.5(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Nonius kappa-CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37528
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    13.866
_exptl_absorpt_correction_T_max  0.0905
_exptl_absorpt_correction_T_min  0.0305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav, Blessing Acta A51 33-70'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needdle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.723
_refine_diff_density_rms         .238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0277
_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)+(0.0308P)²+2.4500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                2736
_reflns_number_total             3553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805367g.txt
_cod_data_source_block           SH-542
_cod_original_sg_symbol_H-M      'P bcn'
_cod_database_code               7004308
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb -0.435654(8) 0.379691(14) -0.384065(10) 0.02561(6) Uani 1 1 d . . .
O1 O -0.31492(17) 0.3274(3) -0.2955(2) 0.0336(7) Uani 1 1 d . . .
O2 O -0.41167(19) 0.3575(3) -0.1938(2) 0.0403(7) Uani 1 1 d . . .
O3 O -0.3906(3) 0.6154(3) -0.3450(3) 0.0535(10) Uani 1 1 d . . .
O4 O -0.4899(2) 0.6336(3) -0.4451(2) 0.0422(8) Uani 1 1 d . . .
N1 N -0.1797(2) 0.1780(4) -0.0082(3) 0.0353(8) Uani 1 1 d . . .
N2 N -0.4439(3) 0.1097(4) -0.3574(4) 0.0441(10) Uani 1 1 d . . .
C1 C -0.3422(2) 0.3237(4) -0.2154(3) 0.0294(9) Uani 1 1 d . . .
C2 C -0.2858(2) 0.2701(4) -0.1424(3) 0.0283(9) Uani 1 1 d . . .
C3 C -0.2217(3) 0.1889(4) -0.1641(3) 0.0329(9) Uani 1 1 d . . .
H3 H -0.2127 0.1644 -0.2245 0.040 Uiso 1 1 calc R . .
C4 C -0.1712(3) 0.1444(5) -0.0965(3) 0.0348(10) Uani 1 1 d . . .
H4 H -0.1289 0.0882 -0.1127 0.042 Uiso 1 1 calc R . .
C5 C -0.2423(3) 0.2562(5) 0.0123(3) 0.0382(10) Uani 1 1 d . . .
H5 H -0.2499 0.2802 0.0731 0.046 Uiso 1 1 calc R . .
C6 C -0.2962(3) 0.3035(5) -0.0518(3) 0.0351(10) Uani 1 1 d . . .
H6 H -0.3391 0.3573 -0.0340 0.042 Uiso 1 1 calc R . .
C7 C -0.4428(3) 0.6830(5) -0.3877(3) 0.0314(9) Uani 1 1 d . . .
C8 C -0.4455(3) 0.8305(5) -0.3719(3) 0.0311(9) Uani 1 1 d . . .
C9 C -0.3783(3) 0.8985(4) -0.3416(4) 0.0400(11) Uani 1 1 d . . .
H9 H -0.3324 0.8517 -0.3243 0.048 Uiso 1 1 calc R . .
C10 C -0.3792(3) 0.0358(4) -0.3371(4) 0.0445(12) Uani 1 1 d . . .
H10 H -0.3324 0.0793 -0.3190 0.053 Uiso 1 1 calc R . .
C11 C -0.5111(3) 0.0431(5) -0.3829(4) 0.0456(12) Uani 1 1 d . . .
H11 H -0.5577 0.0916 -0.3947 0.055 Uiso 1 1 calc R . .
C12 C -0.5135(3) 0.9062(5) -0.3921(4) 0.0433(12) Uani 1 1 d . . .
H12 H -0.5605 0.8646 -0.4118 0.052 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 .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .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
O1 Pb O3 80.73(11) . . ?
O1 Pb N1 74.32(10) . 2_454 ?
O3 Pb N1 98.14(14) . 2_454 ?
O1 Pb N2 75.73(12) . . ?
O3 Pb N2 154.30(13) . . ?
N1 Pb N2 85.40(13) 2_454 . ?
C1 O1 Pb 101.9(2) . . ?
C7 O3 Pb 100.7(3) . . ?
C5 N1 C4 116.4(4) . . ?
C5 N1 Pb 121.7(3) . 2_455 ?
C4 N1 Pb 121.3(3) . 2_455 ?
C10 N2 C11 116.6(4) . . ?
C10 N2 Pb 122.6(3) . . ?
C11 N2 Pb 119.4(3) . . ?
O2 C1 O1 124.3(4) . . ?
O2 C1 C2 119.3(4) . . ?
O1 C1 C2 116.4(4) . . ?
C3 C2 C6 117.6(4) . . ?
C3 C2 C1 121.5(4) . . ?
C6 C2 C1 120.9(4) . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
N1 C4 C3 123.3(4) . . ?
N1 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
N1 C5 C6 123.6(4) . . ?
N1 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C2 C6 C5 119.3(4) . . ?
C2 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
O4 C7 O3 123.2(4) . . ?
O4 C7 C8 118.4(4) . . ?
O3 C7 C8 118.3(4) . . ?
C9 C8 C12 117.0(4) . . ?
C9 C8 C7 120.9(4) . . ?
C12 C8 C7 122.0(4) . . ?
C10 C9 C8 120.0(5) 1_565 . ?
C10 C9 H9 120.0 1_565 . ?
C8 C9 H9 120.0 . . ?
N2 C10 C9 123.5(5) . 1_545 ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 1_545 . ?
N2 C11 C12 122.9(5) . 1_545 ?
N2 C11 H11 118.6 . . ?
C12 C11 H11 118.6 1_545 . ?
C11 C12 C8 119.8(5) 1_565 . ?
C11 C12 H12 120.1 1_565 . ?
C8 C12 H12 120.1 . . ?
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
Pb O1 2.443(3) . ?
Pb O3 2.544(3) . ?
Pb N1 2.701(4) 2_454 ?
Pb N2 2.739(4) . ?
O1 C1 1.258(5) . ?
O2 C1 1.242(5) . ?
O3 C7 1.265(6) . ?
O4 C7 1.251(5) . ?
N1 C5 1.336(6) . ?
N1 C4 1.343(6) . ?
N1 Pb 2.701(4) 2_455 ?
N2 C10 1.338(6) . ?
N2 C11 1.351(7) . ?
C1 C2 1.519(6) . ?
C2 C3 1.377(6) . ?
C2 C6 1.378(6) . ?
C3 C4 1.371(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.380(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.497(6) . ?
C8 C9 1.381(6) . ?
C8 C12 1.392(7) . ?
C9 C10 1.378(6) 1_565 ?
C9 H9 0.9300 . ?
C10 C9 1.378(6) 1_545 ?
C10 H10 0.9300 . ?
C11 C12 1.380(6) 1_545 ?
C11 H11 0.9300 . ?
C12 C11 1.380(6) 1_565 ?
C12 H12 0.9300 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Pb O1 C1 87.5(3) . . . . ?
N1 Pb O1 C1 -171.3(3) 2_454 . . . ?
N2 Pb O1 C1 -82.1(3) . . . . ?
O1 Pb O3 C7 176.9(3) . . . . ?
N1 Pb O3 C7 104.4(3) 2_454 . . . ?
N2 Pb O3 C7 -159.3(3) . . . . ?
O1 Pb N2 C10 -21.1(4) . . . . ?
O3 Pb N2 C10 -45.4(7) . . . . ?
N1 Pb N2 C10 53.9(5) 2_454 . . . ?
O1 Pb N2 C11 172.6(4) . . . . ?
O3 Pb N2 C11 148.3(4) . . . . ?
N1 Pb N2 C11 -112.5(4) 2_454 . . . ?
Pb O1 C1 O2 -8.3(5) . . . . ?
Pb O1 C1 C2 169.9(3) . . . . ?
O2 C1 C2 C3 156.5(4) . . . . ?
O1 C1 C2 C3 -21.9(6) . . . . ?
O2 C1 C2 C6 -24.9(6) . . . . ?
O1 C1 C2 C6 156.8(4) . . . . ?
C6 C2 C3 C4 0.1(6) . . . . ?
C1 C2 C3 C4 178.8(4) . . . . ?
C5 N1 C4 C3 1.6(7) . . . . ?
Pb N1 C4 C3 -169.7(3) 2_455 . . . ?
C2 C3 C4 N1 -1.3(7) . . . . ?
C4 N1 C5 C6 -0.7(7) . . . . ?
Pb N1 C5 C6 170.5(4) 2_455 . . . ?
C3 C2 C6 C5 0.7(7) . . . . ?
C1 C2 C6 C5 -178.0(4) . . . . ?
N1 C5 C6 C2 -0.4(8) . . . . ?
Pb O3 C7 O4 -11.8(6) . . . . ?
Pb O3 C7 C8 171.3(3) . . . . ?
O4 C7 C8 C9 -153.0(5) . . . . ?
O3 C7 C8 C9 24.0(7) . . . . ?
O4 C7 C8 C12 23.1(7) . . . . ?
O3 C7 C8 C12 -159.9(5) . . . . ?
C12 C8 C9 C10 -3.4(7) . . . 1_565 ?
C7 C8 C9 C10 172.9(5) . . . 1_565 ?
C11 N2 C10 C9 0.4(9) . . . 1_545 ?
Pb N2 C10 C9 -166.3(4) . . . 1_545 ?
C10 N2 C11 C12 -2.9(8) . . . 1_545 ?
Pb N2 C11 C12 164.3(4) . . . 1_545 ?
C9 C8 C12 C11 1.1(7) . . . 1_565 ?
C7 C8 C12 C11 -175.2(5) . . . 1_565 ?
