#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/98/2229884.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_2229884
loop_
_publ_author_name
'Trigui, A.'
'Boughzala, H.'
'Driss, A.'
'Abid, Y.'
_publ_section_title
;
 The one-dimensional organic--inorganic hybrid:
 catena-poly[bis[1-(3-ammoniopropyl)-1H-imidazolium]
 [[iodidoplumbate(II)]-tri-μ-iodido-plumbate(II)-tri-μ-iodido-[iodidoplumbate(II)]-di-μ-iodido]]
;
_journal_coeditor_code           YK2002
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m458
_journal_page_last               m459
_journal_paper_doi               10.1107/S160053681100941X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H13 N3)2 [Pb3 I10]'
_chemical_formula_moiety         '2(C6 H13 N3), I10 Pb3'
_chemical_formula_sum            'C12 H26 I10 N6 Pb3'
_chemical_formula_weight         2144.99
_chemical_name_common
'bis[1-(3-ammoniopropyl)-1H-imidazolium] decaiodotriplumbate(II)'
_chemical_name_systematic
;
catena-poly[bis[1-(3-ammoniopropyl)-1H-imidazolium]
[[iodidoplumbate(II)]-tri-μ-iodido-plumbate(II)-tri-μ-iodido-
[iodidoplumbate(II)]-di-μ-iodido]]
;
_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           SHELXL97
_cell_angle_alpha                117.21(3)
_cell_angle_beta                 98.05(2)
_cell_angle_gamma                107.17(3)
_cell_formula_units_Z            1
_cell_length_a                   8.652(3)
_cell_length_b                   11.728(5)
_cell_length_c                   11.972(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      9
_cell_volume                     976.7(9)
_computing_cell_refinement       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_collection       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled ω/2θ'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4950
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    20.812
_exptl_absorpt_correction_T_max  0.6241
_exptl_absorpt_correction_T_min  0.1389
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.166
_refine_diff_density_min         -2.088
_refine_ls_extinction_coef       0.00169(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0363
_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)+(0.0630P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2749
_reflns_number_total             3796
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yk2002.cif
_cod_data_source_block           I
_cod_database_code               2229884
_cod_database_fobs_code          2229884
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pb Pb1 0.45091(5) 0.90517(4) 0.62320(4) 0.03669(15) Uani d . 1 . .
Pb Pb2 0.5000 1.0000 1.0000 0.03708(18) Uani d S 1 . .
I I1 0.76440(9) 0.98779(8) 0.52450(7) 0.0436(2) Uani d . 1 . .
I I2 0.14853(9) 0.82298(7) 0.74775(7) 0.0436(2) Uani d . 1 . .
I I3 0.67368(10) 0.82982(8) 0.79737(7) 0.0432(2) Uani d . 1 . .
I I4 0.59957(11) 1.21598(7) 0.90100(8) 0.0505(2) Uani d . 1 . .
I I5 0.30697(11) 0.59287(8) 0.38118(8) 0.0501(2) Uani d . 1 . .
N N9 0.2562(18) 0.3757(14) 0.5290(12) 0.073(4) Uani d . 1 . .
H H9A 0.2959 0.4198 0.4885 0.109 Uiso calc R 1 . .
H H9B 0.1595 0.3006 0.4732 0.109 Uiso calc R 1 . .
H H9C 0.3332 0.3487 0.5545 0.109 Uiso calc R 1 . .
C C8 0.223(2) 0.4705(14) 0.6451(14) 0.060(4) Uani d . 1 . .
H H8A 0.1398 0.5000 0.6172 0.073 Uiso calc R 1 . .
H H8B 0.3281 0.5534 0.7047 0.073 Uiso calc R 1 . .
C C7 0.1565(18) 0.3985(15) 0.7187(14) 0.057(3) Uani d . 1 . .
H H7A 0.1032 0.4516 0.7762 0.069 Uiso calc R 1 . .
H H7B 0.0682 0.3058 0.6536 0.069 Uiso calc R 1 . .
C C6 0.2864(16) 0.3825(13) 0.8013(12) 0.050(3) Uani d . 1 . .
H H6A 0.3363 0.3245 0.7449 0.060 Uiso calc R 1 . .
H H6B 0.3773 0.4739 0.8663 0.060 Uiso calc R 1 . .
N N1 0.2042(13) 0.3173(9) 0.8694(9) 0.045(2) Uani d . 1 . .
C C2 0.1429(17) 0.1818(12) 0.8230(12) 0.050(3) Uani d . 1 . .
H H2 0.1488 0.1127 0.7458 0.060 Uiso calc R 1 . .
N N3 0.0710(14) 0.1625(10) 0.9077(11) 0.054(3) Uani d . 1 . .
H H3 0.0212 0.0825 0.8993 0.065 Uiso calc R 1 . .
C C4 0.0878(19) 0.2879(14) 1.0096(14) 0.058(3) Uani d . 1 . .
H H4 0.0471 0.3025 1.0808 0.069 Uiso calc R 1 . .
C C5 0.1731(18) 0.3842(14) 0.9870(13) 0.057(3) Uani d . 1 . .
H H5 0.2065 0.4805 1.0411 0.069 Uiso calc R 1 . .
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'
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
6 -1 -3
5 -6 1
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
I5 Pb1 I1 . . 90.09(5) y
I5 Pb1 I3 . . 89.89(5) y
I1 Pb1 I3 . . 88.94(4) y
I5 Pb1 I1 . 2_676 95.96(5) y
I1 Pb1 I1 . 2_676 92.18(4) y
I3 Pb1 I1 . 2_676 174.05(2) y
I5 Pb1 I2 . . 91.62(5) y
I1 Pb1 I2 . . 175.04(2) y
I3 Pb1 I2 . . 86.41(4) y
I1 Pb1 I2 2_676 . 92.27(4) y
I5 Pb1 I4 . . 172.82(3) y
I1 Pb1 I4 . . 94.09(5) y
I3 Pb1 I4 . . 84.36(5) y
I1 Pb1 I4 2_676 . 89.73(5) y
I2 Pb1 I4 . . 83.75(5) y
I4 Pb2 I4 . 2_677 180.0 ?
I4 Pb2 I3 . . 85.76(4) ?
I4 Pb2 I3 2_677 . 94.24(4) y
I3 Pb2 I3 . 2_677 180.0 ?
I4 Pb2 I2 2_677 . 94.02(5) ?
I4 Pb2 I2 . . 85.98(5) y
I3 Pb2 I2 2_677 . 93.10(5) ?
I3 Pb2 I2 . . 86.90(5) y
I2 Pb2 I2 2_677 . 180.0 ?
I3 Pb2 I2 2_677 2_677 86.90(5) ?
I3 Pb2 I2 . 2_677 93.10(5) ?
I4 Pb2 I2 2_677 2_677 85.98(5) ?
I4 Pb2 I2 . 2_677 94.02(5) ?
I4 Pb2 I3 . 2_677 94.24(4) ?
I4 Pb2 I3 2_677 2_677 85.76(4) ?
Pb1 I1 Pb1 . 2_676 87.82(4) y
Pb2 I2 Pb1 . . 76.05(4) y
Pb1 I3 Pb2 . . 77.46(4) y
Pb2 I4 Pb1 . . 76.68(5) y
C8 N9 H9A . . 109.5 ?
C8 N9 H9B . . 109.5 ?
H9A N9 H9B . . 109.5 ?
C8 N9 H9C . . 109.5 ?
H9A N9 H9C . . 109.5 ?
H9B N9 H9C . . 109.5 ?
N9 C8 C7 . . 111.1(11) ?
N9 C8 H8A . . 109.4 ?
C7 C8 H8A . . 109.4 ?
N9 C8 H8B . . 109.4 ?
C7 C8 H8B . . 109.4 ?
H8A C8 H8B . . 108.0 ?
C6 C7 C8 . . 116.4(12) ?
C6 C7 H7A . . 108.2 ?
C8 C7 H7A . . 108.2 ?
C6 C7 H7B . . 108.2 ?
C8 C7 H7B . . 108.2 ?
H7A C7 H7B . . 107.3 ?
N1 C6 C7 . . 109.8(10) ?
N1 C6 H6A . . 109.7 ?
C7 C6 H6A . . 109.7 ?
N1 C6 H6B . . 109.7 ?
C7 C6 H6B . . 109.7 ?
H6A C6 H6B . . 108.2 ?
C2 N1 C5 . . 108.9(12) ?
C2 N1 C6 . . 124.3(10) ?
C5 N1 C6 . . 126.8(10) ?
N1 C2 N3 . . 106.8(10) ?
N1 C2 H2 . . 126.6 ?
N3 C2 H2 . . 126.6 ?
C2 N3 C4 . . 110.1(10) ?
C2 N3 H3 . . 124.9 ?
C4 N3 H3 . . 124.9 ?
C5 C4 N3 . . 106.2(11) ?
C5 C4 H4 . . 126.9 ?
N3 C4 H4 . . 126.9 ?
C4 C5 N1 . . 108.0(12) ?
C4 C5 H5 . . 126.0 ?
N1 C5 H5 . . 126.0 ?
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
Pb1 I5 . 3.155(2) y
Pb1 I1 . 3.1757(13) y
Pb1 I3 . 3.2264(14) y
Pb1 I1 2_676 3.2652(13) y
Pb1 I2 . 3.3039(14) y
Pb1 I4 . 3.309(2) y
Pb2 I4 . 3.2105(15) y
Pb2 I4 2_677 3.2105(14) ?
Pb2 I3 . 3.2388(14) y
Pb2 I3 2_677 3.2388(14) ?
Pb2 I2 2_677 3.263(2) ?
Pb2 I2 . 3.263(2) y
I1 Pb1 2_676 3.2653(13) ?
N9 C8 . 1.460(17) ?
N9 H9A . 0.8900 ?
N9 H9B . 0.8900 ?
N9 H9C . 0.8900 ?
C8 C7 . 1.536(19) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C7 C6 . 1.502(18) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C6 N1 . 1.473(16) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
N1 C2 . 1.315(15) ?
N1 C5 . 1.375(16) ?
C2 N3 . 1.331(17) ?
C2 H2 . 0.9300 ?
N3 C4 . 1.362(16) ?
N3 H3 . 0.8600 ?
C4 C5 . 1.318(19) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
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
N9 H9A I5 1_555 0.89 2.84 3.67(2) 155.8
N9 H9B I2 2_566 0.89 2.90 3.68(2) 146.5
N9 H9C I5 2_666 0.89 2.89 3.64(2) 143.2
