#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:55:48 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179604 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/68/4506823.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_4506823
loop_
_publ_author_name
'Deng, Dongsheng'
'Liu, Leilei'
'Ji, Bao-Ming'
'Yin, Guojie'
'Du, Chenxia'
_publ_section_title
;
 Temperature, Cooling Rate, and Additive-Controlled Supramolecular
 Isomerism in Four Pb(II) Coordination Polymers with an in Situ Ligand
 Transformation Reaction
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5338
_journal_paper_doi               10.1021/cg300900m
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C15 H12 N2 O4 Pb'
_chemical_formula_sum            'C15 H12 N2 O4 Pb'
_chemical_formula_weight         491.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.2347(12)
_cell_length_b                   19.772(2)
_cell_length_c                   10.8817(10)
_cell_measurement_reflns_used    2986
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.57
_cell_volume                     3062.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6854
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.036
_exptl_absorpt_correction_T_max  0.3280
_exptl_absorpt_correction_T_min  0.1056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1875
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0254
_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)+(0.0000P)²+9.8675P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                1648
_reflns_number_total             1875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300900m_si_002.cif
_cod_data_source_block           3
_cod_database_code               4506823
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'
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 0.0000 -0.5000 -1.12408(9) 0.04547(9) Uani 1 2 d S
O1 O 0.0941(3) -0.4045(2) -1.0553(5) 0.0680(13) Uani 1 1 d .
O2 O 0.0881(3) -0.3025(2) -0.9692(5) 0.0669(13) Uani 1 1 d .
N1 N -0.0708(3) -0.4401(2) -0.9464(4) 0.0437(11) Uani 1 1 d .
C1 C -0.2500 -0.2500 -0.7698(10) 0.077(3) Uani 1 2 d S
H1A H -0.2027 -0.2297 -0.8224 0.092 Uiso 0.50 1 calc PR
H1B H -0.2973 -0.2703 -0.8224 0.092 Uiso 0.50 1 calc PR
C2 C -0.2036(5) -0.3061(3) -0.6921(6) 0.0560(16) Uani 1 1 d .
H2A H -0.1578 -0.2865 -0.6365 0.067 Uiso 1 1 calc R
H2B H -0.2508 -0.3294 -0.6437 0.067 Uiso 1 1 calc R
C3 C -0.1562(4) -0.3551(3) -0.7776(6) 0.0451(13) Uani 1 1 d .
C4 C -0.1897(4) -0.4192(3) -0.7986(6) 0.0493(14) Uani 1 1 d .
H4 H -0.2412 -0.4353 -0.7548 0.059 Uiso 1 1 calc R
C5 C -0.1463(4) -0.4598(3) -0.8854(6) 0.0494(14) Uani 1 1 d .
H5 H -0.1713 -0.5024 -0.9015 0.059 Uiso 1 1 calc R
C6 C -0.0342(4) -0.3790(3) -0.9215(5) 0.0411(12) Uani 1 1 d .
C7 C -0.0742(5) -0.3359(3) -0.8396(5) 0.0490(15) Uani 1 1 d .
H7 H -0.0472 -0.2938 -0.8247 0.059 Uiso 1 1 calc R
C8 C 0.0580(4) -0.3598(3) -0.9877(6) 0.0526(16) Uani 1 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
O1 Pb1 O1 144.2(3) 2_545 .
O1 Pb1 N1 67.25(16) 2_545 2_545
O1 Pb1 N1 84.66(17) . 2_545
O1 Pb1 N1 84.66(17) 2_545 .
O1 Pb1 N1 67.25(16) . .
N1 Pb1 N1 77.6(2) 2_545 .
O1 Pb1 O2 106.64(16) 2_545 7_544
O1 Pb1 O2 86.96(16) . 7_544
N1 Pb1 O2 76.79(15) 2_545 7_544
N1 Pb1 O2 145.02(17) . 7_544
O1 Pb1 O2 86.96(16) 2_545 8_434
O1 Pb1 O2 106.64(16) . 8_434
N1 Pb1 O2 145.02(17) 2_545 8_434
N1 Pb1 O2 76.79(15) . 8_434
O2 Pb1 O2 135.5(2) 7_544 8_434
C8 O1 Pb1 119.9(4) . .
C8 O2 Pb1 135.0(4) . 3
C5 N1 C6 118.7(5) . .
C5 N1 Pb1 125.5(4) . .
C6 N1 Pb1 115.4(4) . .
C2 C1 C2 113.6(8) 14_445 .
C2 C1 H1A 108.8 14_445 .
C2 C1 H1A 108.8 . .
C2 C1 H1B 108.8 14_445 .
C2 C1 H1B 108.8 . .
H1A C1 H1B 107.7 . .
C3 C2 C1 108.5(6) . .
C3 C2 H2A 110.0 . .
C1 C2 H2A 110.0 . .
C3 C2 H2B 110.0 . .
C1 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
C4 C3 C7 117.4(5) . .
C4 C3 C2 122.8(6) . .
C7 C3 C2 119.8(6) . .
C3 C4 C5 119.6(5) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N1 C5 C4 122.3(5) . .
N1 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
N1 C6 C7 122.3(5) . .
N1 C6 C8 117.2(5) . .
C7 C6 C8 120.5(5) . .
C6 C7 C3 119.6(6) . .
C6 C7 H7 120.2 . .
C3 C7 H7 120.2 . .
O2 C8 O1 126.9(6) . .
O2 C8 C6 116.6(6) . .
O1 C8 C6 116.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.434(5) 2_545
Pb1 O1 2.434(5) .
Pb1 N1 2.481(5) 2_545
Pb1 N1 2.481(5) .
Pb1 O2 2.731(5) 7_544
Pb1 O2 2.731(5) 8_434
O1 C8 1.259(8) .
O2 C8 1.229(8) .
O2 Pb1 2.731(5) 3
N1 C5 1.322(7) .
N1 C6 1.343(7) .
C1 C2 1.544(9) 14_445
C1 C2 1.544(9) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.502(8) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.373(8) .
C3 C7 1.401(8) .
C4 C5 1.385(9) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.359(8) .
C6 C8 1.544(8) .
C7 H7 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
O1 Pb1 O1 C8 -58.5(5) 2_545
N1 Pb1 O1 C8 -96.1(5) 2_545
N1 Pb1 O1 C8 -17.3(5) .
O2 Pb1 O1 C8 -173.1(5) 7_544
O2 Pb1 O1 C8 50.1(5) 8_434
O1 Pb1 N1 C5 -16.6(5) 2_545
O1 Pb1 N1 C5 -173.9(5) .
N1 Pb1 N1 C5 -84.5(5) 2_545
O2 Pb1 N1 C5 -128.2(5) 7_544
O2 Pb1 N1 C5 71.5(5) 8_434
O1 Pb1 N1 C6 171.4(4) 2_545
O1 Pb1 N1 C6 14.2(4) .
N1 Pb1 N1 C6 103.6(5) 2_545
O2 Pb1 N1 C6 59.8(5) 7_544
O2 Pb1 N1 C6 -100.5(4) 8_434
C2 C1 C2 C3 -176.6(6) 14_445
C1 C2 C3 C4 -108.4(7) .
C1 C2 C3 C7 71.6(7) .
C7 C3 C4 C5 -4.8(9) .
C2 C3 C4 C5 175.2(6) .
C6 N1 C5 C4 1.0(9) .
Pb1 N1 C5 C4 -170.7(5) .
C3 C4 C5 N1 2.7(10) .
C5 N1 C6 C7 -2.6(9) .
Pb1 N1 C6 C7 170.0(5) .
C5 N1 C6 C8 175.7(5) .
Pb1 N1 C6 C8 -11.7(7) .
N1 C6 C7 C3 0.3(9) .
C8 C6 C7 C3 -178.0(6) .
C4 C3 C7 C6 3.4(9) .
C2 C3 C7 C6 -176.7(6) .
Pb1 O2 C8 O1 -60.2(10) 3
Pb1 O2 C8 C6 120.2(6) 3
Pb1 O1 C8 O2 -161.9(6) .
Pb1 O1 C8 C6 17.7(7) .
N1 C6 C8 O2 176.3(6) .
C7 C6 C8 O2 -5.4(9) .
N1 C6 C8 O1 -3.4(8) .
C7 C6 C8 O1 174.9(6) .
