#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:41:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179151 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/12/4311265.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_4311265
loop_
_publ_author_name
'Barton H. Hamilton'
'Christopher J. Ziegler'
_publ_section_title
;
 Lead and Thallium Tetrakis(imidazolyl)borates: Modifying Structure by
 Varying Metal and Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4272
_journal_page_last               4277
_journal_paper_doi               10.1021/ic0497984
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C16 H20 B N9 O3 Pb'
_chemical_formula_weight         604.41
_chemical_name_systematic
;
 Lead(II) tetrakis(4-methylimidazolyl)borate nitrate
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 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            2
_cell_length_a                   11.8787(8)
_cell_length_b                   11.8787(8)
_cell_length_c                   7.0539(10)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.42
_cell_volume                     995.33(17)
_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 0.998
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7155
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    8.515
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.736
_refine_diff_density_min         -6.470
_refine_diff_density_rms         0.213
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0572P)²+1.2575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                910
_reflns_number_total             977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497984si20040413_041557_2.cif
_cod_data_source_block           PbBMeIm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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               4311265
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+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
B1 B 0.5000 0.5000 0.5000 0.014(3) Uani 1 4 d S . .
C1 C 0.5224(5) 0.2912(6) 0.3870(9) 0.0161(11) Uani 1 1 d . . .
C2 C 0.4132(5) 0.2899(4) 0.1402(7) 0.0181(11) Uani 1 1 d . . .
C3 C 0.4115(4) 0.3946(5) 0.2122(6) 0.0151(10) Uani 1 1 d . . .
C4 C 0.3531(6) 0.2452(5) -0.0330(8) 0.0242(13) Uani 1 1 d . . .
H1 H 0.578(4) 0.272(4) 0.482(7) 0.009(13) Uiso 1 1 d . . .
H2 H 0.370(5) 0.439(6) 0.166(8) 0.024(16) Uiso 1 1 d . . .
H3 H 0.317(6) 0.299(7) -0.089(12) 0.04(2) Uiso 1 1 d . . .
H4 H 0.316(5) 0.174(5) 0.021(7) 0.015(13) Uiso 1 1 d . . .
H5 H 0.408(5) 0.213(5) -0.114(9) 0.017(14) Uiso 1 1 d . . .
N1 N 0.4840(4) 0.2236(5) 0.248(2) 0.0206(10) Uani 1 1 d . . .
N2 N 0.4791(4) 0.3973(5) 0.3702(7) 0.0142(10) Uani 1 1 d . . .
Pb1 Pb 0.5000 0.0000 0.2500 0.0232(2) Uani 1 4 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.012(5) 0.012(5) 0.018(6) 0.000 0.000 0.000
C1 0.015(2) 0.014(3) 0.019(3) -0.004(2) 0.001(3) 0.001(3)
C2 0.022(3) 0.017(3) 0.015(2) 0.004(2) -0.001(2) -0.006(2)
C3 0.021(3) 0.015(2) 0.009(2) 0.0054(19) -0.0044(19) 0.001(2)
C4 0.038(4) 0.016(3) 0.019(2) -0.002(2) -0.009(2) -0.003(3)
N1 0.022(2) 0.012(2) 0.027(2) -0.012(4) -0.003(4) -0.0006(17)
N2 0.0149(19) 0.014(3) 0.013(2) 0.0009(19) 0.0008(19) -0.001(2)
Pb1 0.0137(2) 0.0137(2) 0.0423(3) 0.000 0.000 -0.00038(11)
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'
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
N2 B1 N2 110.6(2) . 4_656 ?
N2 B1 N2 107.3(4) . 2_665 ?
N2 B1 N2 110.6(2) 4_656 2_665 ?
N2 B1 N2 110.6(2) . 3_566 ?
N2 B1 N2 107.3(4) 4_656 3_566 ?
N2 B1 N2 110.6(2) 2_665 3_566 ?
N1 C1 N2 111.0(6) . . ?
C3 C2 N1 109.3(6) . . ?
C3 C2 C4 128.6(5) . . ?
N1 C2 C4 122.1(6) . . ?
C2 C3 N2 108.7(5) . . ?
C1 N1 C2 105.4(5) . . ?
C1 N1 Pb1 124.4(8) . . ?
C2 N1 Pb1 128.1(6) . . ?
C1 N2 C3 105.6(5) . . ?
C1 N2 B1 128.0(5) . . ?
C3 N2 B1 126.4(5) . . ?
N1 Pb1 N1 98.20(19) 7_545 . ?
N1 Pb1 N1 81.81(19) 7_545 2_655 ?
N1 Pb1 N1 179.3(7) . 2_655 ?
N1 Pb1 N1 179.3(7) 7_545 8 ?
N1 Pb1 N1 81.81(19) . 8 ?
N1 Pb1 N1 98.20(19) 2_655 8 ?
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 N2 1.545(6) . ?
B1 N2 1.545(6) 4_656 ?
B1 N2 1.545(6) 2_665 ?
B1 N2 1.545(6) 3_566 ?
C1 N1 1.350(13) . ?
C1 N2 1.366(9) . ?
C2 C3 1.343(7) . ?
C2 N1 1.379(12) . ?
C2 C4 1.512(7) . ?
C3 N2 1.374(7) . ?
N1 Pb1 2.663(6) . ?
Pb1 N1 2.663(6) 7_545 ?
Pb1 N1 2.663(6) 2_655 ?
Pb1 N1 2.663(6) 8 ?
