#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309196.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_4309196
loop_
_publ_author_name
'Barton H. Hamilton'
'Todd A. Wagler'
'Matthew P. Espe'
'Christopher J. Ziegler'
_publ_section_title
;
Sequestering Perrhenate with a Borate-Based Coordination Polymer: A Model
for Pertechnetate Separation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4891
_journal_page_last               4893
_journal_paper_doi               10.1021/ic050213v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H12 B N8 O4 Pb Re'
_chemical_formula_weight         736.50
_chemical_name_systematic
;
 Lead(II) tetrakis(imidazolyl)borate perrhenate
;
_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                73.8860(10)
_cell_angle_beta                 79.1570(10)
_cell_angle_gamma                70.9930(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4923(7)
_cell_length_b                   10.2828(9)
_cell_length_c                   11.1011(10)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.53
_cell_volume                     875.43(13)
_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 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7064
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    16.549
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.944
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0194P)²+1.2243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3521
_reflns_number_total             3926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050213vsi20050208_115816.cif
_cod_data_source_block           pbbim4reo4
_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               4309196
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
N8 N 0.5412(5) 0.4710(4) 0.7773(3) 0.0071(8) Uani 1 1 d . . .
C10 C 0.4587(6) 0.6071(5) 0.7265(4) 0.0124(10) Uani 1 1 d . . .
N7 N 0.3112(5) 0.6186(4) 0.6943(4) 0.0118(8) Uani 1 1 d . . .
C11 C 0.2985(6) 0.4821(5) 0.7243(5) 0.0139(10) Uani 1 1 d . . .
C12 C 0.4374(6) 0.3919(6) 0.7749(5) 0.0128(10) Uani 1 1 d . . .
B1 B 0.7246(6) 0.4170(6) 0.8075(5) 0.0085(10) Uani 1 1 d . . .
H10 H 0.500(7) 0.681(7) 0.716(5) 0.024(16) Uiso 1 1 d . . .
H12 H 0.465(6) 0.304(6) 0.801(5) 0.005(12) Uiso 1 1 d . . .
H11 H 0.196(8) 0.463(7) 0.713(6) 0.040(19) Uiso 1 1 d . . .
N5 N 0.9106(5) 0.7093(4) 0.7593(4) 0.0097(8) Uani 1 1 d . . .
N6 N 0.7767(5) 0.5449(4) 0.8110(3) 0.0091(8) Uani 1 1 d . . .
C7 C 0.8893(6) 0.6003(5) 0.7289(4) 0.0093(9) Uani 1 1 d . . .
C9 C 0.7172(6) 0.6278(5) 0.8991(5) 0.0119(10) Uani 1 1 d . . .
C8 C 0.7996(6) 0.7286(5) 0.8666(4) 0.0101(9) Uani 1 1 d . . .
H8 H 0.784(5) 0.796(5) 0.909(4) 0.000(11) Uiso 1 1 d . . .
H9 H 0.632(6) 0.614(5) 0.965(5) 0.005(12) Uiso 1 1 d . . .
H7 H 0.949(7) 0.564(6) 0.663(5) 0.025(16) Uiso 1 1 d . . .
Pb1 Pb 0.90053(2) 0.155841(18) 0.351087(15) 0.00826(5) Uani 1 1 d . . .
N1 N 0.9195(5) 0.2720(4) 0.5221(4) 0.0103(8) Uani 1 1 d . . .
N2 N 0.8336(4) 0.3464(4) 0.7015(3) 0.0080(8) Uani 1 1 d . . .
C2 C 1.0517(6) 0.2262(5) 0.5942(4) 0.0095(9) Uani 1 1 d . . .
C3 C 1.0026(6) 0.2691(5) 0.7018(5) 0.0110(9) Uani 1 1 d . . .
C1 C 0.7925(6) 0.3437(5) 0.5896(4) 0.0099(9) Uani 1 1 d . . .
H1 H 0.683(6) 0.393(5) 0.565(4) 0.000(11) Uiso 1 1 d . . .
H3 H 1.053(6) 0.252(5) 0.766(5) 0.002(12) Uiso 1 1 d . . .
H2 H 1.151(6) 0.172(6) 0.567(5) 0.011(13) Uiso 1 1 d . . .
N3 N 0.8546(5) 0.1893(4) 1.1176(4) 0.0149(9) Uani 1 1 d . . .
N4 N 0.7520(5) 0.3058(4) 0.9336(3) 0.0094(8) Uani 1 1 d . . .
C5 C 0.7847(6) 0.1045(5) 1.0789(5) 0.0127(10) Uani 1 1 d . . .
C4 C 0.8329(6) 0.3055(6) 1.0290(5) 0.0140(10) Uani 1 1 d . . .
C6 C 0.7252(7) 0.1738(6) 0.9678(5) 0.0176(11) Uani 1 1 d . . .
H6 H 0.666(7) 0.157(7) 0.924(6) 0.029(17) Uiso 1 1 d . . .
H5 H 0.791(6) 0.005(6) 1.120(5) 0.008(13) Uiso 1 1 d . . .
H H 0.869(7) 0.376(7) 1.026(6) 0.029(17) Uiso 1 1 d . . .
Re1 Re 0.54986(2) 0.053082(19) 0.647628(16) 0.00955(6) Uani 1 1 d . . .
O4 O 0.7603(4) -0.0060(4) 0.5914(3) 0.0172(8) Uani 1 1 d . . .
O3 O 0.5360(4) 0.0572(4) 0.8039(3) 0.0165(7) Uani 1 1 d . . .
O2 O 0.4643(4) 0.2223(4) 0.5649(3) 0.0177(8) Uani 1 1 d . . .
O1 O 0.4360(4) -0.0561(4) 0.6383(3) 0.0166(8) 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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
C10 N8 C12 105.6(4) . . ?
C10 N8 B1 125.5(4) . . ?
C12 N8 B1 128.0(4) . . ?
N7 C10 N8 111.9(4) . . ?
C10 N7 C11 105.7(4) . . ?
C10 N7 Pb1 121.7(3) . 2_666 ?
C11 N7 Pb1 130.6(3) . 2_666 ?
C12 C11 N7 109.2(4) . . ?
C11 C12 N8 107.6(4) . . ?
N6 B1 N8 107.6(4) . . ?
N6 B1 N4 109.6(4) . . ?
N8 B1 N4 113.5(4) . . ?
N6 B1 N2 110.5(4) . . ?
N8 B1 N2 108.1(3) . . ?
N4 B1 N2 107.5(4) . . ?
C7 N5 C8 105.5(4) . . ?
C7 N5 Pb1 126.7(3) . 2_766 ?
C8 N5 Pb1 127.9(3) . 2_766 ?
C7 N6 C9 106.0(4) . . ?
C7 N6 B1 126.8(4) . . ?
C9 N6 B1 127.2(4) . . ?
N5 C7 N6 112.5(4) . . ?
C8 C9 N6 107.1(4) . . ?
C9 C8 N5 108.8(4) . . ?
N5 Pb1 N7 83.79(13) 2_766 2_666 ?
N5 Pb1 N1 79.27(12) 2_766 . ?
N7 Pb1 N1 77.45(13) 2_666 . ?
N5 Pb1 N3 78.71(12) 2_766 1_554 ?
N7 Pb1 N3 76.18(13) 2_666 1_554 ?
N1 Pb1 N3 147.14(13) . 1_554 ?
C1 N1 C2 104.6(4) . . ?
C1 N1 Pb1 126.6(3) . . ?
C2 N1 Pb1 124.3(3) . . ?
C1 N2 C3 104.2(4) . . ?
C1 N2 B1 129.9(4) . . ?
C3 N2 B1 125.8(4) . . ?
C3 C2 N1 110.3(4) . . ?
C2 C3 N2 107.9(4) . . ?
N1 C1 N2 113.1(4) . . ?
C4 N3 C5 104.9(4) . . ?
C4 N3 Pb1 127.5(3) . 1_556 ?
C5 N3 Pb1 123.4(3) . 1_556 ?
C4 N4 C6 103.7(4) . . ?
C4 N4 B1 127.5(4) . . ?
C6 N4 B1 128.1(4) . . ?
C6 C5 N3 108.9(4) . . ?
N3 C4 N4 113.7(4) . . ?
C5 C6 N4 108.6(4) . . ?
O2 Re1 O3 107.70(17) . . ?
O2 Re1 O1 110.02(16) . . ?
O3 Re1 O1 108.23(16) . . ?
O2 Re1 O4 109.49(17) . . ?
O3 Re1 O4 108.86(16) . . ?
O1 Re1 O4 112.42(17) . . ?
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
N8 C10 1.356(6) . ?
N8 C12 1.388(6) . ?
N8 B1 1.541(6) . ?
C10 N7 1.326(6) . ?
N7 C11 1.385(6) . ?
N7 Pb1 2.417(4) 2_666 ?
C11 C12 1.347(7) . ?
B1 N6 1.530(6) . ?
B1 N4 1.544(6) . ?
B1 N2 1.547(6) . ?
N5 C7 1.329(6) . ?
N5 C8 1.390(6) . ?
N5 Pb1 2.401(4) 2_766 ?
N6 C7 1.345(6) . ?
N6 C9 1.390(6) . ?
C9 C8 1.366(7) . ?
Pb1 N5 2.401(4) 2_766 ?
Pb1 N7 2.417(4) 2_666 ?
Pb1 N1 2.560(4) . ?
Pb1 N3 2.606(4) 1_554 ?
N1 C1 1.324(6) . ?
N1 C2 1.381(6) . ?
N2 C1 1.362(6) . ?
N2 C3 1.396(6) . ?
C2 C3 1.334(7) . ?
N3 C4 1.304(6) . ?
N3 C5 1.392(6) . ?
N3 Pb1 2.606(4) 1_556 ?
N4 C4 1.364(6) . ?
N4 C6 1.386(6) . ?
C5 C6 1.340(7) . ?
Re1 O2 1.714(4) . ?
Re1 O3 1.728(3) . ?
Re1 O1 1.737(3) . ?
Re1 O4 1.743(3) . ?
