#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/24/8102474.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_8102474
loop_
_publ_author_name
'Zhan-Lin Xu'
'Xiu-Mei Li'
'Qing-Wei Wang'
_publ_section_title
;
 Crystal structure of poly[(4,5-imidazoledicarboxylato)lead(II)],
 [Pb3(C10H2N4O8)]n
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              481
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C10 H2 N4 O8 Pb3'
_chemical_formula_sum            'C10 H2 N4 O8 Pb3'
_chemical_formula_weight         927.73
_chemical_name_systematic
; 
[(4,5-imidazoledicarboxylate)lead(II)], 
[Pb₃(C₁₀H₂N₄O₈)₂]ₙ
;
_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                 113.9120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.853(2)
_cell_length_b                   4.7321(4)
_cell_length_c                   14.4504(12)
_cell_measurement_reflns_used    2517
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.90
_cell_volume                     1428.6(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3627
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         4.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    35.323
_exptl_absorpt_correction_T_max  0.2257
_exptl_absorpt_correction_T_min  0.2257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS (Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0157
_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)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0333
_reflns_number_gt                1257
_reflns_number_total             1310
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            1267-2658.cff
_cod_data_source_block           2
_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_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               8102474
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.43941(6) 0.7500 0.01882(11) Uani 1 2 d S . .
Pb2 Pb 0.302118(10) 0.36347(4) 0.396826(15) 0.00983(10) Uani 1 1 d . . .
C1 C 0.4178(3) 0.0060(11) 0.8440(5) 0.0184(13) Uani 1 1 d . . .
H1 H 0.4385 0.0696 0.9103 0.022 Uiso 1 1 calc R . .
C2 C 0.3539(2) -0.2262(11) 0.7138(4) 0.0089(11) Uani 1 1 d . . .
C3 C 0.3911(3) -0.0478(10) 0.6837(4) 0.0079(11) Uani 1 1 d . . .
C4 C 0.3036(3) -0.4363(11) 0.6605(4) 0.0099(12) Uani 1 1 d U . .
C5 C 0.3905(3) 0.0447(11) 0.5849(4) 0.0114(12) Uani 1 1 d U . .
N1 N 0.4316(2) 0.1002(9) 0.7679(4) 0.0129(10) Uani 1 1 d . . .
N2 N 0.3716(2) -0.1869(10) 0.8159(3) 0.0156(10) Uani 1 1 d . . .
O1 O 0.3493(2) -0.0523(8) 0.5029(3) 0.0156(9) Uani 1 1 d . . .
O2 O 0.43061(18) 0.2318(8) 0.5864(3) 0.0162(9) Uani 1 1 d . . .
O3 O 0.2981(2) -0.5517(8) 0.5810(3) 0.0167(9) Uani 1 1 d . . .
O4 O 0.2681(2) -0.5011(8) 0.7067(3) 0.0166(9) 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
Pb Pb -3.3944 10.1111 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N1 Pb1 N1 92.7(2) 2_656 . ?
N1 Pb1 O2 79.50(16) 2_656 . ?
N1 Pb1 O2 68.29(15) . . ?
N1 Pb1 O2 68.29(14) 2_656 2_656 ?
N1 Pb1 O2 79.50(15) . 2_656 ?
O2 Pb1 O2 132.82(18) . 2_656 ?
O4 Pb2 N2 81.91(15) 7_546 6 ?
O4 Pb2 O1 80.26(14) 7_546 . ?
N2 Pb2 O1 79.68(14) 6 . ?
O4 Pb2 O4 71.66(8) 7_546 6 ?
N2 Pb2 O4 63.97(14) 6 6 ?
O1 Pb2 O4 136.26(12) . 6 ?
O4 Pb2 O3 115.66(12) 7_546 1_565 ?
N2 Pb2 O3 142.57(15) 6 1_565 ?
O1 Pb2 O3 71.91(12) . 1_565 ?
O4 Pb2 O3 150.94(12) 6 1_565 ?
N1 C1 N2 113.6(6) . . ?
N1 C1 H1 123.2 . . ?
N2 C1 H1 123.2 . . ?
N2 C2 C3 107.6(5) . . ?
N2 C2 C4 118.6(4) . . ?
C3 C2 C4 133.8(5) . . ?
C2 C3 C5 135.3(5) . . ?
C2 C3 N1 108.0(4) . . ?
C5 C3 N1 115.9(5) . . ?
O3 C4 O4 122.3(5) . . ?
O3 C4 C2 123.2(5) . . ?
O4 C4 C2 114.4(4) . . ?
O1 C5 O2 121.9(5) . . ?
O1 C5 C3 120.4(5) . . ?
O2 C5 C3 117.6(5) . . ?
C1 N1 C3 104.9(5) . . ?
C1 N1 Pb1 135.6(4) . . ?
C3 N1 Pb1 119.5(3) . . ?
C2 N2 C1 105.9(4) . . ?
C2 N2 Pb2 119.7(4) . 6_556 ?
C1 N2 Pb2 132.2(4) . 6_556 ?
C5 O1 Pb2 105.4(3) . . ?
C5 O2 Pb1 118.4(3) . . ?
C4 O3 Pb2 160.7(4) . 1_545 ?
C4 O4 Pb2 104.5(3) . 7_546 ?
C4 O4 Pb2 120.4(3) . 6_556 ?
Pb2 O4 Pb2 131.98(15) 7_546 6_556 ?
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 N1 2.326(5) 2_656 ?
Pb1 N1 2.326(5) . ?
Pb1 O2 2.455(4) . ?
Pb1 O2 2.455(4) 2_656 ?
Pb2 O4 2.410(4) 7_546 ?
Pb2 N2 2.469(5) 6 ?
Pb2 O1 2.458(4) . ?
Pb2 O4 2.616(4) 6 ?
Pb2 O3 2.729(4) 1_565 ?
C1 N1 1.338(7) . ?
C1 N2 1.327(8) . ?
C1 H1 0.9300 . ?
C2 N2 1.374(7) . ?
C2 C3 1.388(8) . ?
C2 C4 1.478(8) . ?
C3 C5 1.488(7) . ?
C3 N1 1.384(7) . ?
C4 O3 1.232(6) . ?
C4 O4 1.279(7) . ?
C5 O1 1.265(7) . ?
C5 O2 1.268(7) . ?
N2 Pb2 2.469(5) 6_556 ?
O3 Pb2 2.729(4) 1_545 ?
O4 Pb2 2.410(4) 7_546 ?
O4 Pb2 2.616(4) 6_556 ?
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
N2 C2 C3 C5 -169.4(6) . . . . ?
C4 C2 C3 C5 11.7(11) . . . . ?
N2 C2 C3 N1 0.0(6) . . . . ?
C4 C2 C3 N1 -178.9(6) . . . . ?
N2 C2 C4 O3 -156.3(5) . . . . ?
C3 C2 C4 O3 22.4(9) . . . . ?
N2 C2 C4 O4 20.0(7) . . . . ?
C3 C2 C4 O4 -161.3(6) . . . . ?
C2 C3 C5 O1 -2.0(9) . . . . ?
N1 C3 C5 O1 -170.8(5) . . . . ?
C2 C3 C5 O2 174.8(6) . . . . ?
N1 C3 C5 O2 6.0(7) . . . . ?
N2 C1 N1 C3 -0.6(7) . . . . ?
N2 C1 N1 Pb1 176.6(4) . . . . ?
C2 C3 N1 C1 0.4(6) . . . . ?
C5 C3 N1 C1 172.1(5) . . . . ?
C2 C3 N1 Pb1 -177.4(3) . . . . ?
C5 C3 N1 Pb1 -5.7(6) . . . . ?
N1 Pb1 N1 C1 108.4(6) 2_656 . . . ?
O2 Pb1 N1 C1 -174.0(6) . . . . ?
O2 Pb1 N1 C1 41.1(6) 2_656 . . . ?
N1 Pb1 N1 C3 -74.6(4) 2_656 . . . ?
O2 Pb1 N1 C3 2.9(4) . . . . ?
O2 Pb1 N1 C3 -142.0(4) 2_656 . . . ?
C3 C2 N2 C1 -0.3(6) . . . . ?
C4 C2 N2 C1 178.7(5) . . . . ?
C3 C2 N2 Pb2 164.7(3) . . . 6_556 ?
C4 C2 N2 Pb2 -16.2(6) . . . 6_556 ?
N1 C1 N2 C2 0.6(7) . . . . ?
N1 C1 N2 Pb2 -161.8(4) . . . 6_556 ?
O2 C5 O1 Pb2 -47.0(6) . . . . ?
C3 C5 O1 Pb2 129.6(4) . . . . ?
O4 Pb2 O1 C5 -172.1(4) 7_546 . . . ?
N2 Pb2 O1 C5 104.4(4) 6 . . . ?
O4 Pb2 O1 C5 137.8(3) 6 . . . ?
O3 Pb2 O1 C5 -50.9(3) 1_565 . . . ?
O1 C5 O2 Pb1 173.2(4) . . . . ?
C3 C5 O2 Pb1 -3.5(6) . . . . ?
N1 Pb1 O2 C5 97.7(4) 2_656 . . . ?
N1 Pb1 O2 C5 0.5(4) . . . . ?
O2 Pb1 O2 C5 50.9(4) 2_656 . . . ?
O4 C4 O3 Pb2 152.7(9) . . . 1_545 ?
C2 C4 O3 Pb2 -31.3(15) . . . 1_545 ?
O3 C4 O4 Pb2 -0.2(6) . . . 7_546 ?
C2 C4 O4 Pb2 -176.6(4) . . . 7_546 ?
O3 C4 O4 Pb2 162.1(4) . . . 6_556 ?
C2 C4 O4 Pb2 -14.2(6) . . . 6_556 ?
