#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:28:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179142 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/03/4310358.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_4310358
loop_
_publ_author_name
'Barton H. Hamilton'
'Kathryn A. Kelly'
'Todd A. Wagler'
'Matthew P. Espe'
'Christopher J. Ziegler'
_publ_section_title
;
 Lead Tetrakis(imidazolyl)borate Solids: Anion Exchange, Solvent
 Intercalation, and Self Assembly of an Organic Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              50
_journal_page_last               56
_journal_paper_doi               10.1021/ic035117d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C12 H12 B I N8 Pb'
_chemical_formula_weight         613.20
_chemical_name_systematic
;
 Lead tetrakis(imidazolyl)borate iodide
;
_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                102.070(3)
_cell_angle_beta                 104.408(3)
_cell_angle_gamma                103.875(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5459(16)
_cell_length_b                   10.0336(19)
_cell_length_c                   10.965(2)
_cell_measurement_reflns_used    2194
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.18
_cell_volume                     847.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7608
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    11.789
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.234
_refine_diff_density_min         -3.384
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0434
_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)+(0.0452P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3508
_reflns_number_total             3967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035117dsi20031029_032249_2.cif
_cod_data_source_block           PbBIm4I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310358
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
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.7679(11) 0.3538(9) 0.2265(9) 0.0139(18) Uani 1 1 d . . .
N1 N 0.7084(8) 0.4672(7) 0.3050(6) 0.0124(13) Uani 1 1 d . . .
Pb1 Pb 0.43532(4) 0.82718(3) 0.35165(3) 0.01131(10) Uani 1 1 d . . .
I1 I 0.17283(8) 0.97983(6) 0.24071(6) 0.02703(15) Uani 1 1 d . . .
C1 C 0.6542(9) 0.5703(8) 0.2625(8) 0.0129(15) Uani 1 1 d . . .
H1 H 0.6403 0.5779 0.1776 0.015 Uiso 1 1 calc R . .
N2 N 0.6232(8) 0.6589(7) 0.3541(7) 0.0179(14) Uani 1 1 d . . .
C2 C 0.7133(10) 0.4955(8) 0.4349(8) 0.0155(16) Uani 1 1 d . . .
H2 H 0.7465 0.4435 0.4921 0.019 Uiso 1 1 calc R . .
C3 C 0.6617(10) 0.6113(8) 0.4643(8) 0.0169(17) Uani 1 1 d . . .
H3 H 0.6532 0.6527 0.5456 0.020 Uiso 1 1 calc R . .
N3 N 0.9506(8) 0.4205(6) 0.2282(6) 0.0118(13) Uani 1 1 d . . .
N4 N 1.1904(8) 0.5838(7) 0.2469(7) 0.0158(14) Uani 1 1 d . . .
C4 C 1.0368(9) 0.5628(8) 0.2582(7) 0.0128(15) Uani 1 1 d . . .
H4 H 0.9923 0.6362 0.2836 0.015 Uiso 1 1 calc R . .
N5 N 0.7666(8) 0.2304(6) 0.2917(6) 0.0109(12) Uani 1 1 d . . .
C5 C 1.0593(10) 0.3479(8) 0.1938(8) 0.0178(17) Uani 1 1 d . . .
H5 H 1.0378 0.2492 0.1685 0.021 Uiso 1 1 calc R . .
N6 N 0.6672(8) 0.0382(7) 0.3511(7) 0.0178(14) Uani 1 1 d . . .
C6 C 1.2021(9) 0.4482(8) 0.2040(8) 0.0164(17) Uani 1 1 d . . .
H6 H 1.2958 0.4288 0.1849 0.020 Uiso 1 1 calc R . .
C7 C 0.6361(10) 0.1147(8) 0.2693(8) 0.0183(17) Uani 1 1 d . . .
H7 H 0.5337 0.0905 0.2027 0.022 Uiso 1 1 calc R . .
N7 N 0.6469(8) 0.2986(7) 0.0842(6) 0.0120(13) Uani 1 1 d . . .
C8 C 0.8919(10) 0.2265(9) 0.3961(8) 0.0185(17) Uani 1 1 d . . .
H8 H 0.9994 0.2932 0.4360 0.022 Uiso 1 1 calc R . .
N8 N 0.5554(8) 0.2315(6) -0.1322(7) 0.0140(13) Uani 1 1 d . . .
C9 C 0.8296(10) 0.1082(8) 0.4293(8) 0.0179(17) Uani 1 1 d . . .
H9 H 0.8890 0.0785 0.4963 0.021 Uiso 1 1 calc R . .
C10 C 0.6894(10) 0.2872(8) -0.0259(7) 0.0122(15) Uani 1 1 d . . .
H10 H 0.8006 0.3153 -0.0274 0.015 Uiso 1 1 calc R . .
C11 C 0.4704(9) 0.2466(8) 0.0459(8) 0.0141(16) Uani 1 1 d . . .
H11 H 0.4033 0.2421 0.1008 0.017 Uiso 1 1 calc R . .
C12 C 0.4150(10) 0.2033(8) -0.0885(8) 0.0146(16) Uani 1 1 d . . .
H12 H 0.3025 0.1621 -0.1416 0.017 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 0.0033 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'
B B 0.0013 0.0007 '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'
I I -0.4742 1.8119 '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
N3 B1 N7 110.0(6) . . ?
N3 B1 N1 110.2(6) . . ?
N7 B1 N1 108.1(6) . . ?
N3 B1 N5 108.0(6) . . ?
N7 B1 N5 111.3(6) . . ?
N1 B1 N5 109.3(6) . . ?
C1 N1 C2 105.0(6) . . ?
C1 N1 B1 126.1(7) . . ?
C2 N1 B1 128.7(6) . . ?
N8 Pb1 N6 76.4(2) 2_665 1_565 ?
N8 Pb1 N2 76.6(2) 2_665 . ?
N6 Pb1 N2 93.8(2) 1_565 . ?
N8 Pb1 N4 79.0(2) 2_665 1_455 ?
N6 Pb1 N4 155.3(2) 1_565 1_455 ?
N2 Pb1 N4 82.3(2) . 1_455 ?
N8 Pb1 I1 83.85(15) 2_665 . ?
N6 Pb1 I1 87.46(16) 1_565 . ?
N2 Pb1 I1 159.52(15) . . ?
N4 Pb1 I1 88.05(14) 1_455 . ?
N2 C1 N1 112.8(7) . . ?
C1 N2 C3 105.1(7) . . ?
C1 N2 Pb1 134.5(5) . . ?
C3 N2 Pb1 117.0(5) . . ?
C3 C2 N1 108.1(7) . . ?
C2 C3 N2 109.1(7) . . ?
C4 N3 C5 105.7(6) . . ?
C4 N3 B1 127.4(6) . . ?
C5 N3 B1 126.8(6) . . ?
C4 N4 C6 104.9(6) . . ?
C4 N4 Pb1 124.3(5) . 1_655 ?
C6 N4 Pb1 128.5(5) . 1_655 ?
N4 C4 N3 112.1(7) . . ?
C7 N5 C8 105.3(6) . . ?
C7 N5 B1 127.1(6) . . ?
C8 N5 B1 127.1(6) . . ?
C6 C5 N3 106.6(6) . . ?
C7 N6 C9 104.5(7) . . ?
C7 N6 Pb1 121.0(5) . 1_545 ?
C9 N6 Pb1 134.2(5) . 1_545 ?
C5 C6 N4 110.7(7) . . ?
N6 C7 N5 113.1(7) . . ?
C10 N7 C11 106.7(6) . . ?
C10 N7 B1 127.3(6) . . ?
C11 N7 B1 126.0(6) . . ?
C9 C8 N5 106.8(7) . . ?
C10 N8 C12 106.2(6) . . ?
C10 N8 Pb1 125.1(5) . 2_665 ?
C12 N8 Pb1 128.4(5) . 2_665 ?
C8 C9 N6 110.2(7) . . ?
N8 C10 N7 112.2(7) . . ?
C12 C11 N7 106.5(7) . . ?
C11 C12 N8 108.4(7) . . ?
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
B1 N3 1.539(10) . ?
B1 N7 1.540(11) . ?
B1 N1 1.543(11) . ?
B1 N5 1.553(10) . ?
N1 C1 1.350(9) . ?
N1 C2 1.381(10) . ?
Pb1 N8 2.381(7) 2_665 ?
Pb1 N6 2.531(6) 1_565 ?
Pb1 N2 2.594(7) . ?
Pb1 N4 2.615(6) 1_455 ?
Pb1 I1 3.1507(7) . ?
C1 N2 1.320(10) . ?
N2 C3 1.384(10) . ?
C2 C3 1.344(11) . ?
N3 C4 1.367(9) . ?
N3 C5 1.385(9) . ?
N4 C4 1.321(10) . ?
N4 C6 1.380(10) . ?
N4 Pb1 2.615(6) 1_655 ?
N5 C7 1.332(9) . ?
N5 C8 1.373(10) . ?
C5 C6 1.345(10) . ?
N6 C7 1.316(10) . ?
N6 C9 1.358(10) . ?
N6 Pb1 2.531(6) 1_545 ?
N7 C10 1.335(9) . ?
N7 C11 1.393(10) . ?
C8 C9 1.342(11) . ?
N8 C10 1.318(10) . ?
N8 C12 1.389(10) . ?
N8 Pb1 2.381(7) 2_665 ?
C11 C12 1.368(11) . ?
