#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/63/2226322.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2226322
loop_
_publ_author_name
'Rayner, Matthew Kyle'
'Billing, David Gordon'
_publ_section_title
;
 Poly[1,4-bis(ammoniomethyl)cyclohexane
 [di-μ-bromido-dibromidoplumbate(II)]]
;
_journal_coeditor_code           WM2338
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m658
_journal_paper_doi               10.1107/S1600536810016806
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C8 H20 N2) [Pb Br4]'
_chemical_formula_moiety         'C8 H20 N2 2+, Br4 Pb 2-'
_chemical_formula_sum            'C8 H20 Br4 N2 Pb'
_chemical_formula_weight         671.09
_chemical_name_systematic
;
Poly[1,4-bis(ammoniomethyl)cyclohexane [di-μ-bromido-dibromidoplumbate(II)]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.6930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1042(6)
_cell_length_b                   8.1955(4)
_cell_length_c                   8.2160(4)
_cell_measurement_reflns_used    5293
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      3.01
_cell_volume                     811.01(7)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg,
1999)
;
_computing_publication_material
;
WinGX (Farrugia, 1999) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10495
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    20.233
_exptl_absorpt_correction_T_max  0.6563
_exptl_absorpt_correction_T_min  0.0907
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.784
_refine_diff_density_min         -2.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0349P)²+0.0549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                1742
_reflns_number_total             1966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wm2338.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226322
_cod_database_fobs_code          2226322
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.2360(3) -0.0472(4) 0.4803(5) 0.0262(8) Uani d . 1 . .
H H1A 0.2798 -0.0711 0.5858 0.031 Uiso calc R 1 . .
H H1B 0.2282 -0.1498 0.4166 0.031 Uiso calc R 1 . .
C C2 0.1224(3) 0.0131(4) 0.5124(4) 0.0216(8) Uani d . 1 . .
H H2 0.1325 0.1095 0.5871 0.026 Uiso calc R 1 . .
C C3 0.0636(3) -0.1206(4) 0.6011(4) 0.0257(8) Uani d . 1 . .
H H3A 0.0558 -0.2192 0.5312 0.031 Uiso calc R 1 . .
H H3B 0.1093 -0.1499 0.7035 0.031 Uiso calc R 1 . .
C C4 0.0501(3) 0.0661(5) 0.3589(4) 0.0247(7) Uani d . 1 . .
H H4A 0.0869 0.1569 0.3058 0.030 Uiso calc R 1 . .
H H4B 0.0419 -0.0261 0.2807 0.030 Uiso calc R 1 . .
N N1 0.2966(2) 0.0758(4) 0.3879(4) 0.0230(6) Uani d . 1 . .
H H1C 0.3644 0.0356 0.3700 0.035 Uiso calc R 1 . .
H H1D 0.3054 0.1695 0.4473 0.035 Uiso calc R 1 . .
H H1E 0.2569 0.0972 0.2904 0.035 Uiso calc R 1 . .
Br Br1 0.25157(3) 0.02969(4) -0.01928(4) 0.02426(9) Uani d . 1 . .
Br Br2 0.50023(3) 0.18890(4) -0.31018(4) 0.02370(9) Uani d . 1 . .
Pb Pb1 0.5000 0.0000 0.0000 0.01590(6) Uani d S 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.024(2) 0.0232(17) 0.0322(19) 0.0000(15) 0.0076(16) 0.0042(14)
C2 0.024(2) 0.0206(17) 0.0210(17) -0.0015(13) 0.0039(15) -0.0010(12)
C3 0.0206(19) 0.0285(18) 0.0277(18) 0.0035(15) 0.0011(15) 0.0101(14)
C4 0.0213(19) 0.0285(18) 0.0246(17) -0.0011(15) 0.0040(14) 0.0042(14)
N1 0.0203(16) 0.0229(15) 0.0267(15) -0.0014(12) 0.0065(12) -0.0019(12)
Br1 0.0241(2) 0.02380(17) 0.02478(17) -0.00282(13) 0.00175(14) -0.00035(12)
Br2 0.0311(2) 0.02090(17) 0.01975(16) 0.00481(13) 0.00579(13) 0.00695(12)
Pb1 0.02093(10) 0.01395(9) 0.01320(9) 0.00121(6) 0.00358(6) 0.00007(5)
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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 111.7(3) ?
N1 C1 H1A . . 109.3 ?
C2 C1 H1A . . 109.3 ?
N1 C1 H1B . . 109.3 ?
C2 C1 H1B . . 109.3 ?
H1A C1 H1B . . 108.0 ?
C1 C2 C3 . . 108.9(3) ?
C1 C2 C4 . . 114.0(3) ?
C3 C2 C4 . . 110.0(3) ?
C1 C2 H2 . . 107.9 ?
C3 C2 H2 . . 107.9 ?
C4 C2 H2 . . 107.9 ?
C4 C3 C2 3_556 . 111.6(3) ?
C4 C3 H3A 3_556 . 109.3 ?
C2 C3 H3A . . 109.3 ?
C4 C3 H3B 3_556 . 109.3 ?
C2 C3 H3B . . 109.3 ?
H3A C3 H3B . . 108.0 ?
C3 C4 C2 3_556 . 111.3(3) ?
C3 C4 H4A 3_556 . 109.4 ?
C2 C4 H4A . . 109.4 ?
C3 C4 H4B 3_556 . 109.4 ?
C2 C4 H4B . . 109.4 ?
H4A C4 H4B . . 108.0 ?
C1 N1 H1C . . 109.5 ?
C1 N1 H1D . . 109.5 ?
H1C N1 H1D . . 109.5 ?
C1 N1 H1E . . 109.5 ?
H1C N1 H1E . . 109.5 ?
H1D N1 H1E . . 109.5 ?
Pb1 Br2 Pb1 . 2_654 152.724(12) ?
Br2 Pb1 Br2 3_655 . 180.000(11) ?
Br2 Pb1 Br2 3_655 4_566 89.827(4) ?
Br2 Pb1 Br2 . 4_566 90.173(4) ?
Br2 Pb1 Br2 3_655 2_644 90.173(4) ?
Br2 Pb1 Br2 . 2_644 89.827(4) ?
Br2 Pb1 Br2 4_566 2_644 180.000(15) ?
Br2 Pb1 Br1 3_655 . 90.075(10) ?
Br2 Pb1 Br1 . . 89.925(10) ?
Br2 Pb1 Br1 4_566 . 84.697(10) ?
Br2 Pb1 Br1 2_644 . 95.303(10) ?
Br2 Pb1 Br1 3_655 3_655 89.925(10) ?
Br2 Pb1 Br1 . 3_655 90.075(10) ?
Br2 Pb1 Br1 4_566 3_655 95.303(10) ?
Br2 Pb1 Br1 2_644 3_655 84.697(10) ?
Br1 Pb1 Br1 . 3_655 180.000(13) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.497(4) ?
C1 C2 . 1.509(5) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 C3 . 1.531(4) ?
C2 C4 . 1.526(5) ?
C2 H2 . 1.0000 ?
C3 C4 3_556 1.514(5) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C3 3_556 1.514(5) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
N1 H1C . 0.9100 ?
N1 H1D . 0.9100 ?
N1 H1E . 0.9100 ?
Br1 Pb1 . 3.0054(4) ?
Br2 Pb1 . 2.9821(3) ?
Br2 Pb1 2_654 2.9886(3) ?
Pb1 Br2 3_655 2.9821(3) y
Pb1 Br2 4_566 2.9886(3) y
Pb1 Br2 2_644 2.9886(3) ?
Pb1 Br1 3_655 3.0054(4) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1C Br2 3_655 0.91 2.54 3.387(3) 154.4
N1 H1D Br1 4_566 0.91 2.57 3.378(3) 148.0
N1 H1D Br2 1_556 0.91 2.94 3.446(3) 116.9
N1 H1E Br1 . 0.91 2.60 3.357(3) 141.3
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . 177.9(3) ?
N1 C1 C2 C4 . . . . 54.7(4) ?
C1 C2 C3 C4 . . . 3_556 178.5(3) ?
C4 C2 C3 C4 . . . 3_556 -56.0(4) ?
C1 C2 C4 C3 . . . 3_556 178.4(3) ?
C3 C2 C4 C3 . . . 3_556 55.8(4) ?
Pb1 Br2 Pb1 Br2 2_654 . . 4_566 -0.28(4) ?
Pb1 Br2 Pb1 Br2 2_654 . . 2_644 179.72(4) ?
Pb1 Br2 Pb1 Br1 2_654 . . . 84.42(3) ?
Pb1 Br2 Pb1 Br1 2_654 . . 3_655 -95.58(3) ?
