# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Pb I4, C5 H16 N2'
_chemical_formula_sum            'C5 H16 I4 N2 Pb'
_chemical_formula_weight         818.99

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'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'Pbca '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.4679(6)
_cell_length_b                   8.6405(3)
_cell_length_c                   20.7717(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3314.6(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3355
_cell_measurement_theta_min      3.2330
_cell_measurement_theta_max      30.6010

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2832
_exptl_absorpt_coefficient_mu    17.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1267
_exptl_absorpt_correction_T_max  0.3333
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9114
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         25.99
_reflns_number_total             3255
_reflns_number_gt                2752
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00174(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3255
_refine_ls_number_parameters     113
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Pb1 Pb 0.377339(12) 0.12825(3) 0.729838(14) 0.02966(11) Uani 1 1 d . . .
I1 I 0.39908(3) 0.12302(6) 0.58059(3) 0.04642(16) Uani 1 1 d . . .
I2 I 0.26589(3) -0.15191(6) 0.71599(3) 0.04874(17) Uani 1 1 d . . .
I3 I 0.48918(3) 0.40828(6) 0.74422(3) 0.04711(18) Uani 1 1 d . . .
I4 I 0.34557(3) 0.16366(7) 0.88608(3) 0.05500(18) Uani 1 1 d . . .
N1 N 0.1223(3) 0.2896(8) 1.0509(4) 0.0464(17) Uani 1 1 d . . .
H1A H 0.1322 0.1915 1.0642 0.056 Uiso 1 1 calc R . .
N2 N 0.1605(4) 0.0688(8) 0.8382(4) 0.059(2) Uani 1 1 d . . .
H2A H 0.2050 0.1081 0.8396 0.088 Uiso 1 1 calc R . .
H2B H 0.1435 0.0753 0.7982 0.088 Uiso 1 1 calc R . .
H2C H 0.1616 -0.0299 0.8503 0.088 Uiso 1 1 calc R . .
C1 C 0.1909(6) 0.3770(12) 1.0527(7) 0.086(3) Uani 1 1 d U . .
H1B H 0.1846 0.4746 1.0314 0.129 Uiso 1 1 calc R . .
H1C H 0.2281 0.3187 1.0313 0.129 Uiso 1 1 calc R . .
H1D H 0.2047 0.3945 1.0967 0.129 Uiso 1 1 calc R . .
C2 C 0.0709(6) 0.3574(11) 1.0977(6) 0.078(3) Uani 1 1 d U . .
H2D H 0.0577 0.4597 1.0839 0.117 Uiso 1 1 calc R . .
H2E H 0.0934 0.3627 1.1393 0.117 Uiso 1 1 calc R . .
H2F H 0.0284 0.2939 1.1001 0.117 Uiso 1 1 calc R . .
C3 C 0.0918(4) 0.2787(11) 0.9859(4) 0.059(2) Uani 1 1 d D . .
H3A H 0.0858 0.3815 0.9679 0.070 Uiso 1 1 calc R . .
H3B H 0.0446 0.2293 0.9876 0.070 Uiso 1 1 calc R . .
C4 C 0.1426(6) 0.1846(13) 0.9439(5) 0.083(3) Uani 1 1 d DU . .
H4A H 0.1881 0.2397 0.9396 0.100 Uiso 1 1 calc R . .
H4B H 0.1525 0.0867 0.9650 0.100 Uiso 1 1 calc R . .
C5 C 0.1140(6) 0.1548(15) 0.8810(6) 0.097(4) Uani 1 1 d DU . .
H5A H 0.1026 0.2532 0.8609 0.116 Uiso 1 1 calc R . .
H5B H 0.0689 0.0983 0.8857 0.116 Uiso 1 1 calc R . .

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
Pb1 0.02481(16) 0.02517(16) 0.0390(2) -0.00013(12) -0.00126(12) -0.00037(9)
I1 0.0443(3) 0.0560(3) 0.0390(3) -0.0001(3) 0.0007(3) -0.0083(2)
I2 0.0434(3) 0.0373(3) 0.0655(4) -0.0043(3) 0.0079(3) -0.0189(2)
I3 0.0405(3) 0.0369(3) 0.0640(4) -0.0068(3) -0.0004(3) -0.0169(2)
I4 0.0504(3) 0.0741(4) 0.0405(3) 0.0056(3) -0.0021(3) 0.0008(3)
N1 0.042(4) 0.043(4) 0.054(5) 0.005(4) 0.009(4) 0.004(3)
N2 0.062(4) 0.066(4) 0.049(5) -0.018(4) 0.003(4) -0.007(4)
C1 0.074(6) 0.105(7) 0.079(7) 0.011(6) -0.019(6) -0.023(5)
C2 0.086(6) 0.081(6) 0.066(6) -0.010(5) 0.004(6) 0.010(5)
C3 0.039(5) 0.091(6) 0.046(6) -0.015(5) 0.004(4) -0.016(4)
C4 0.070(6) 0.105(7) 0.075(7) -0.009(6) 0.009(6) 0.000(5)
C5 0.082(7) 0.114(7) 0.093(8) -0.024(6) 0.002(6) 0.006(5)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Pb1 I1 3.1264(7) . ?
Pb1 I3 3.1590(5) 3_646 ?
Pb1 I2 3.1904(5) . ?
Pb1 I3 3.1953(5) . ?
Pb1 I2 3.2692(5) 8_665 ?
Pb1 I4 3.3121(7) . ?
I2 Pb1 3.2692(5) 8_655 ?
I3 Pb1 3.1590(5) 3_656 ?
N1 C3 1.467(11) . ?
N1 C1 1.476(11) . ?
N1 C2 1.479(12) . ?
N2 C5 1.442(13) . ?
C3 C4 1.517(11) . ?
C4 C5 1.433(13) . ?

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
I1 Pb1 I3 93.453(17) . 3_646 ?
I1 Pb1 I2 88.998(16) . . ?
I3 Pb1 I2 93.570(15) 3_646 . ?
I1 Pb1 I3 91.182(16) . . ?
I3 Pb1 I3 86.286(6) 3_646 . ?
I2 Pb1 I3 179.78(2) . . ?
I1 Pb1 I2 91.439(17) . 8_665 ?
I3 Pb1 I2 174.848(19) 3_646 8_665 ?
I2 Pb1 I2 84.891(6) . 8_665 ?
I3 Pb1 I2 95.237(14) . 8_665 ?
I1 Pb1 I4 174.691(16) . . ?
I3 Pb1 I4 91.527(17) 3_646 . ?
I2 Pb1 I4 92.530(17) . . ?
I3 Pb1 I4 87.302(17) . . ?
I2 Pb1 I4 83.638(17) 8_665 . ?
Pb1 I2 Pb1 162.73(2) . 8_655 ?
Pb1 I3 Pb1 167.41(2) 3_656 . ?
C3 N1 C1 112.8(8) . . ?
C3 N1 C2 112.6(7) . . ?
C1 N1 C2 109.3(8) . . ?
N1 C3 C4 109.0(7) . . ?
C5 C4 C3 113.1(10) . . ?
C4 C5 N2 115.8(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A I4 0.89 2.81 3.653(7) 158.5 .
N1 H1A I1 0.91 2.80 3.640(7) 154.2 2
N2 H2B I3 0.89 3.06 3.657(7) 126.5 8_655
N2 H2C I4 0.89 2.75 3.641(7) 175.8 8_655

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.232
_database_code_depnum_ccdc_archive 'CCDC 995699'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Pb5 I18, 4(C7 H20 N2)'
_chemical_formula_sum            'C28 H80 I18 N8 Pb5'
_chemical_formula_weight         3849.15

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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7958(3)
_cell_length_b                   12.3844(6)
_cell_length_c                   18.7377(10)
_cell_angle_alpha                85.377(4)
_cell_angle_beta                 88.212(3)
_cell_angle_gamma                78.755(4)
_cell_volume                     1995.16(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5226
_cell_measurement_theta_min      2.8510
_cell_measurement_theta_max      28.7570

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1668
_exptl_absorpt_coefficient_mu    17.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1276
_exptl_absorpt_correction_T_max  0.2735
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16218
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7821
_reflns_number_gt                6037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0287P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7821
_refine_ls_number_parameters     274
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000

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
Pb1 Pb 0.0000 0.5000 0.5000 0.03335(5) Uani 1 2 d SU . .
Pb2 Pb 0.574333(12) 0.296397(11) 0.301944(6) 0.03766(3) Uani 1 1 d U . .
Pb3 Pb 0.543122(13) 0.364185(12) 0.084471(7) 0.04614(4) Uani 1 1 d U . .
I1 I -0.16374(2) 0.37492(2) 0.392154(13) 0.05472(7) Uani 1 1 d U . .
I2 I 0.31995(2) 0.41568(2) 0.420190(11) 0.05098(7) Uani 1 1 d U . .
I3 I -0.06990(3) 0.70725(2) 0.379477(13) 0.05666(8) Uani 1 1 d U . .
I4 I 0.62608(3) 0.06404(2) 0.378903(14) 0.06302(8) Uani 1 1 d U . .
I5 I 0.47982(2) 0.55943(2) 0.215910(12) 0.05025(7) Uani 1 1 d U . .
I6 I 0.82929(2) 0.24151(2) 0.184823(12) 0.05613(8) Uani 1 1 d U . .
I7 I 0.31717(2) 0.24909(2) 0.200735(13) 0.05963(8) Uani 1 1 d U . .
I8 I 0.58400(3) 0.17582(2) -0.013941(15) 0.07447(9) Uani 1 1 d U . .
I9 I 0.23593(2) 0.51224(2) 0.013665(12) 0.05328(7) Uani 1 1 d U . .
C1 C 0.9603(4) 0.5487(3) 0.1928(2) 0.0663(12) Uani 1 1 d U . .
H1D H 0.8608 0.5408 0.2141 0.080 Uiso 1 1 calc R . .
H1E H 0.9793 0.5030 0.1525 0.080 Uiso 1 1 calc R . .
C2 C 0.9539(3) 0.6687(3) 0.16598(17) 0.0509(10) Uani 1 1 d U . .
H2A H 0.9479 0.7139 0.2063 0.061 Uiso 1 1 calc R . .
H2B H 1.0471 0.6757 0.1384 0.061 Uiso 1 1 calc R . .
C3 C 0.8133(3) 0.7072(3) 0.11983(19) 0.0577(10) Uani 1 1 d U . .
H3D H 0.8164 0.6553 0.0835 0.069 Uiso 1 1 calc R . .
H3E H 0.7220 0.7033 0.1496 0.069 Uiso 1 1 calc R . .
C4 C 0.9146(5) 0.8134(4) 0.0234(2) 0.1201(15) Uani 1 1 d DU . .
H4A H 1.0103 0.8256 0.0427 0.144 Uiso 1 1 calc R . .
H4B H 0.9351 0.7398 0.0066 0.144 Uiso 1 1 calc R . .
C5 C 0.8742(5) 0.8906(4) -0.0364(2) 0.1136(16) Uani 1 1 d DU . .
H5A H 0.7764 0.8827 -0.0545 0.170 Uiso 1 1 calc R . .
H5B H 0.9526 0.8773 -0.0731 0.170 Uiso 1 1 calc R . .
H5C H 0.8663 0.9642 -0.0219 0.170 Uiso 1 1 calc R . .
C6 C 0.7901(5) 0.9070(4) 0.1271(3) 0.1026(13) Uani 1 1 d U . .
H6A H 0.7809 0.9743 0.0959 0.123 Uiso 1 1 calc R . .
H6B H 0.8877 0.8966 0.1519 0.123 Uiso 1 1 calc R . .
C7 C 0.6626(6) 0.9203(5) 0.1802(3) 0.1393(17) Uani 1 1 d U . .
H7A H 0.5682 0.9563 0.1571 0.209 Uiso 1 1 calc R . .
H7B H 0.6855 0.9642 0.2169 0.209 Uiso 1 1 calc R . .
H7C H 0.6507 0.8490 0.2012 0.209 Uiso 1 1 calc R . .
C8 C 0.4292(5) 0.7145(4) 0.4206(2) 0.0944(16) Uani 1 1 d U . .
H8A H 0.3370 0.6835 0.4304 0.113 Uiso 1 1 calc R . .
H8B H 0.4607 0.7375 0.4652 0.113 Uiso 1 1 calc R . .
C9 C 0.3917(5) 0.8108(3) 0.3699(2) 0.0811(15) Uani 1 1 d U . .
H9A H 0.3583 0.7889 0.3253 0.097 Uiso 1 1 calc R . .
H9B H 0.4831 0.8427 0.3599 0.097 Uiso 1 1 calc R . .
C10 C 0.2643(4) 0.8954(3) 0.4004(2) 0.0790(13) Uani 1 1 d U . .
H10A H 0.1689 0.8669 0.4040 0.095 Uiso 1 1 calc R . .
H10B H 0.2915 0.9089 0.4482 0.095 Uiso 1 1 calc R . .
C11 C 0.2485(5) 0.9814(5) 0.2716(3) 0.1536(7) Uani 1 1 d DU . .
H11A H 0.2522 1.0508 0.2442 0.184 Uiso 1 1 calc R . .
H11B H 0.3417 0.9288 0.2607 0.184 Uiso 1 1 calc R . .
C12 C 0.1193(5) 0.9425(5) 0.2535(3) 0.1369(9) Uani 1 1 d DU . .
H12A H 0.0284 0.9855 0.2743 0.205 Uiso 1 1 calc R . .
H12B H 0.1292 0.8666 0.2713 0.205 Uiso 1 1 calc R . .
H12C H 0.1103 0.9483 0.2023 0.205 Uiso 1 1 calc R . .
C13 C 0.1285(6) 1.0844(5) 0.3726(3) 0.1165(12) Uani 1 1 d U . .
H13A H 0.0274 1.0648 0.3702 0.140 Uiso 1 1 calc R . .
H13B H 0.1313 1.1479 0.3390 0.140 Uiso 1 1 calc R . .
C14 C 0.1545(6) 1.1116(5) 0.4448(3) 0.1221(13) Uani 1 1 d U . .
H14A H 0.2498 1.0672 0.4623 0.183 Uiso 1 1 calc R . .
H14B H 0.0702 1.0974 0.4756 0.183 Uiso 1 1 calc R . .
H14C H 0.1605 1.1883 0.4441 0.183 Uiso 1 1 calc R . .
N1 N 1.0837(3) 0.5095(3) 0.24650(16) 0.0701(11) Uani 1 1 d U . .
H1A H 1.1737 0.5229 0.2286 0.105 Uiso 1 1 calc R . .
H1B H 1.0916 0.4373 0.2570 0.105 Uiso 1 1 calc R . .
H1C H 1.0597 0.5449 0.2860 0.105 Uiso 1 1 calc R . .
N2 N 0.7938(3) 0.8168(3) 0.08433(15) 0.0654(9) Uani 1 1 d DU . .
H2C H 0.7000 0.8290 0.0628 0.078 Uiso 1 1 calc R . .
N3 N 0.5527(3) 0.6292(2) 0.39477(15) 0.0573(10) Uani 1 1 d U . .
H3A H 0.5314 0.6152 0.3507 0.086 Uiso 1 1 calc R . .
H3B H 0.5595 0.5679 0.4237 0.086 Uiso 1 1 calc R . .
H3C H 0.6423 0.6524 0.3942 0.086 Uiso 1 1 calc R . .
N4 N 0.2396(3) 0.9991(3) 0.3553(2) 0.0875(11) Uani 1 1 d U . .
H4C H 0.3279 1.0247 0.3619 0.105 Uiso 1 1 calc R . .

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
Pb1 0.02884(7) 0.03872(9) 0.03299(8) -0.00782(7) -0.00005(6) -0.00574(6)
Pb2 0.03185(5) 0.04459(7) 0.03731(6) -0.00968(6) -0.00006(5) -0.00666(5)
Pb3 0.03937(6) 0.05648(8) 0.04154(6) -0.00624(6) -0.00414(5) -0.00516(6)
I1 0.04505(10) 0.04779(13) 0.07304(14) -0.02266(11) -0.02200(10) -0.00257(9)
I2 0.03571(9) 0.06778(16) 0.04641(11) -0.01161(12) 0.01018(9) -0.00125(10)
I3 0.06965(13) 0.04595(13) 0.05417(13) 0.00040(12) -0.00119(11) -0.01231(11)
I4 0.06232(12) 0.05183(14) 0.07564(16) 0.01034(13) -0.01696(12) -0.01646(10)
I5 0.05308(11) 0.05359(13) 0.04574(12) -0.00161(11) 0.00144(10) -0.01560(9)
I6 0.03589(10) 0.07927(18) 0.04624(12) -0.00977(13) 0.00335(9) 0.00747(11)
I7 0.04288(10) 0.07521(16) 0.06676(14) -0.01663(13) -0.00847(10) -0.02028(10)
I8 0.06304(13) 0.07366(18) 0.08653(17) -0.03303(15) -0.02110(13) 0.00130(13)
I9 0.03673(10) 0.06597(16) 0.05559(13) -0.00907(12) -0.00120(9) -0.00424(10)
C1 0.0565(18) 0.060(2) 0.085(2) -0.0157(19) -0.0006(16) -0.0129(16)
C2 0.0476(15) 0.0626(19) 0.0430(17) -0.0080(15) 0.0060(13) -0.0115(15)
C3 0.0513(16) 0.0693(17) 0.0584(19) -0.0097(16) -0.0045(14) -0.0238(14)
C4 0.103(2) 0.131(3) 0.120(2) 0.0247(18) 0.0176(17) -0.026(2)
C5 0.119(3) 0.131(3) 0.091(2) -0.007(2) 0.017(2) -0.029(2)
C6 0.104(2) 0.0836(19) 0.123(2) -0.0076(18) -0.0367(17) -0.0207(19)
C7 0.160(3) 0.149(3) 0.112(2) -0.041(2) -0.016(2) -0.021(2)
C8 0.104(3) 0.063(2) 0.094(3) -0.010(2) -0.015(2) 0.041(2)
C9 0.097(3) 0.055(2) 0.085(3) -0.011(2) -0.010(2) 0.0026(18)
C10 0.063(2) 0.0491(19) 0.119(3) -0.0132(19) -0.028(2) 0.0106(17)
C11 0.1819(4) 0.1437(12) 0.1404(18) -0.0061(11) -0.0009(7) -0.0461(4)
C12 0.1406(5) 0.1380(15) 0.118(2) 0.0214(13) -0.0266(9) -0.0026(5)
C13 0.120(2) 0.0867(19) 0.1252(18) 0.0166(17) -0.0040(18) 0.0136(17)
C14 0.130(2) 0.094(2) 0.1308(19) -0.0069(17) -0.0296(19) 0.0099(19)
N1 0.0648(17) 0.067(2) 0.0696(19) -0.0057(17) 0.0096(14) 0.0063(16)
N2 0.0532(13) 0.0717(16) 0.0755(17) 0.0139(13) -0.0176(12) -0.0280(12)
N3 0.0525(15) 0.0535(18) 0.0600(17) -0.0071(16) -0.0109(13) 0.0073(13)
N4 0.0630(17) 0.0628(18) 0.134(2) 0.0076(16) 0.0013(17) -0.0114(14)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Pb1 I2 3.1764(2) 2_566 ?
Pb1 I2 3.1764(2) . ?
Pb1 I1 3.1802(3) 2_566 ?
Pb1 I1 3.1802(3) . ?
Pb1 I3 3.2561(3) . ?
Pb1 I3 3.2561(3) 2_566 ?
Pb2 I4 3.0706(3) . ?
Pb2 I6 3.1058(3) . ?
Pb2 I7 3.1654(3) . ?
Pb2 I1 3.2392(3) 1_655 ?
Pb2 I2 3.3207(3) . ?
Pb2 I5 3.4759(3) . ?
Pb3 I8 3.0490(4) . ?
Pb3 I9 3.1597(3) 2_665 ?
Pb3 I9 3.2128(3) . ?
Pb3 I6 3.2439(3) . ?
Pb3 I7 3.3259(3) . ?
Pb3 I5 3.5456(3) . ?
I1 Pb2 3.2392(3) 1_455 ?
I9 Pb3 3.1597(3) 2_665 ?
C1 N1 1.487(4) . ?
C1 C2 1.520(5) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 C3 1.508(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.444(5) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C4 C5 1.419(6) . ?
C4 N2 1.533(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N2 1.421(6) . ?
C6 C7 1.470(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.455(6) . ?
C8 N3 1.460(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.509(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N4 1.462(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.380(7) . ?
C11 N4 1.599(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N4 1.344(6) . ?
C13 C14 1.456(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N4 H4C 0.9100 . ?

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
I2 Pb1 I2 180.0 2_566 . ?
I2 Pb1 I1 88.434(7) 2_566 2_566 ?
I2 Pb1 I1 91.566(7) . 2_566 ?
I2 Pb1 I1 91.566(7) 2_566 . ?
I2 Pb1 I1 88.434(7) . . ?
I1 Pb1 I1 180.0 2_566 . ?
I2 Pb1 I3 91.173(7) 2_566 . ?
I2 Pb1 I3 88.827(7) . . ?
I1 Pb1 I3 95.222(7) 2_566 . ?
I1 Pb1 I3 84.778(7) . . ?
I2 Pb1 I3 88.827(7) 2_566 2_566 ?
I2 Pb1 I3 91.173(7) . 2_566 ?
I1 Pb1 I3 84.778(7) 2_566 2_566 ?
I1 Pb1 I3 95.222(7) . 2_566 ?
I3 Pb1 I3 180.0 . 2_566 ?
I4 Pb2 I6 96.060(8) . . ?
I4 Pb2 I7 93.647(9) . . ?
I6 Pb2 I7 91.393(7) . . ?
I4 Pb2 I1 93.862(8) . 1_655 ?
I6 Pb2 I1 86.515(7) . 1_655 ?
I7 Pb2 I1 172.378(8) . 1_655 ?
I4 Pb2 I2 96.189(8) . . ?
I6 Pb2 I2 166.209(8) . . ?
I7 Pb2 I2 94.128(7) . . ?
I1 Pb2 I2 86.362(7) 1_655 . ?
I4 Pb2 I5 174.788(7) . . ?
I6 Pb2 I5 87.609(8) . . ?
I7 Pb2 I5 82.540(8) . . ?
I1 Pb2 I5 90.046(8) 1_655 . ?
I2 Pb2 I5 80.603(7) . . ?
I8 Pb3 I9 91.614(9) . 2_665 ?
I8 Pb3 I9 97.786(8) . . ?
I9 Pb3 I9 92.696(7) 2_665 . ?
I8 Pb3 I6 93.022(8) . . ?
I9 Pb3 I6 91.616(7) 2_665 . ?
I9 Pb3 I6 168.240(8) . . ?
I8 Pb3 I7 93.741(9) . . ?
I9 Pb3 I7 174.305(8) 2_665 . ?
I9 Pb3 I7 88.502(7) . . ?
I6 Pb3 I7 86.171(7) . . ?
I8 Pb3 I5 172.667(8) . . ?
I9 Pb3 I5 95.293(8) 2_665 . ?
I9 Pb3 I5 84.368(7) . . ?
I6 Pb3 I5 84.344(7) . . ?
I7 Pb3 I5 79.276(7) . . ?
Pb1 I1 Pb2 162.051(8) . 1_455 ?
Pb1 I2 Pb2 160.651(9) . . ?
Pb2 I5 Pb3 71.454(7) . . ?
Pb2 I6 Pb3 80.416(7) . . ?
Pb2 I7 Pb3 78.308(7) . . ?
Pb3 I9 Pb3 87.304(7) 2_665 . ?
N1 C1 C2 112.0(3) . . ?
N1 C1 H1D 109.2 . . ?
C2 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
C2 C1 H1E 109.2 . . ?
H1D C1 H1E 107.9 . . ?
C3 C2 C1 109.0(3) . . ?
C3 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
C3 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C2 117.4(3) . . ?
N2 C3 H3D 108.0 . . ?
C2 C3 H3D 108.0 . . ?
N2 C3 H3E 108.0 . . ?
C2 C3 H3E 108.0 . . ?
H3D C3 H3E 107.2 . . ?
C5 C4 N2 116.0(3) . . ?
C5 C4 H4A 108.3 . . ?
N2 C4 H4A 108.3 . . ?
C5 C4 H4B 108.3 . . ?
N2 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 113.8(4) . . ?
N2 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N3 113.0(3) . . ?
C9 C8 H8A 109.0 . . ?
N3 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
N3 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 C10 110.0(4) . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N4 C10 C9 111.1(3) . . ?
N4 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N4 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 N4 108.8(4) . . ?
C12 C11 H11A 109.9 . . ?
N4 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
N4 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 109.1(4) . . ?
N4 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
N4 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 N2 C3 118.1(3) . . ?
C6 N2 C4 112.7(3) . . ?
C3 N2 C4 107.5(3) . . ?
C6 N2 H2C 105.9 . . ?
C3 N2 H2C 105.9 . . ?
C4 N2 H2C 105.9 . . ?
C8 N3 H3A 109.5 . . ?
C8 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C8 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C13 N4 C10 120.3(4) . . ?
C13 N4 C11 113.3(4) . . ?
C10 N4 C11 113.1(4) . . ?
C13 N4 H4C 102.4 . . ?
C10 N4 H4C 102.4 . . ?
C11 N4 H4C 102.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A I5 0.89 2.75 3.634(3) 176.2 .
N3 H3B I2 0.89 3.09 3.641(3) 121.6 .
N1 H1A I5 0.89 2.82 3.675(3) 162.7 1_655
N1 H1B I7 0.89 2.99 3.620(3) 129.3 1_655
N1 H1C I3 0.89 2.82 3.676(3) 161.7 1_655
N3 H3C I3 0.89 2.75 3.631(3) 173.1 1_655
N3 H3B I1 0.89 3.14 3.618(3) 116.0 1_655
N2 H2C I8 0.91 2.70 3.595(3) 167.8 2_665
N3 H3B I2 0.89 3.18 3.643(3) 115.0 2_666
N4 H4C I4 0.91 2.79 3.690(3) 169.6 1_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.211
_database_code_depnum_ccdc_archive 'CCDC 995700'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Pb3 I8, C6 H18 N2'
_chemical_formula_sum            'C6 H18 I8 N2 Pb3'
_chemical_formula_weight         1754.99

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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '
_symmetry_space_group_name_Hall  '-P 2ybc'


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'

_cell_length_a                   11.2041(6)
_cell_length_b                   8.0665(4)
_cell_length_c                   15.7101(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.179(6)
_cell_angle_gamma                90.00
_cell_volume                     1387.89(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1941
_cell_measurement_theta_min      3.1350
_cell_measurement_theta_max      27.9790

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_absorpt_coefficient_mu    27.042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0744
_exptl_absorpt_correction_T_max  0.2209
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5413
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2717
_reflns_number_gt                2015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0740P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00196(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2717
_refine_ls_number_parameters     91
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1687
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Pb1 Pb 1.0000 0.5000 1.0000 0.03766(11) Uani 1 2 d S . .
Pb2 Pb 0.88270(2) 0.01657(3) 0.850949(18) 0.03934(8) Uani 1 1 d . . .
I1 I 1.24767(4) 0.30933(6) 1.09045(3) 0.04422(14) Uani 1 1 d . . .
I2 I 0.97778(5) 0.64544(6) 1.18488(3) 0.05129(14) Uani 1 1 d . . .
I3 I 0.84499(4) 0.17481(6) 1.02945(3) 0.04088(13) Uani 1 1 d . . .
I4 I 0.64961(4) 0.14456(7) 0.74320(3) 0.05288(16) Uani 1 1 d . . .
C1 C 0.4780(7) -0.0041(8) 0.9523(5) 0.0475(19) Uani 1 1 d U . .
H1B H 0.4286 -0.1027 0.9367 0.057 Uiso 1 1 calc R . .
H1C H 0.5467 -0.0090 0.9237 0.057 Uiso 1 1 calc R . .
C2 C 0.3389(8) 0.1348(12) 0.8293(4) 0.075(2) Uani 1 1 d DU . .
H2A H 0.2898 0.2310 0.8109 0.112 Uiso 1 1 calc R . .
H2B H 0.2879 0.0381 0.8224 0.112 Uiso 1 1 calc R . .
H2C H 0.3994 0.1236 0.7945 0.112 Uiso 1 1 calc R . .
C3 C 0.4817(7) 0.3078(10) 0.9401(5) 0.060(2) Uani 1 1 d U . .
H3A H 0.5388 0.3071 0.9023 0.090 Uiso 1 1 calc R . .
H3B H 0.5254 0.3078 0.9996 0.090 Uiso 1 1 calc R . .
H3C H 0.4317 0.4053 0.9291 0.090 Uiso 1 1 calc R . .
N1 N 0.4007(5) 0.1532(7) 0.9229(3) 0.0484(16) Uani 1 1 d DU . .
H1A H 0.3422 0.1611 0.9550 0.058 Uiso 1 1 calc R . .

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
Pb1 0.04064(17) 0.03161(18) 0.0402(2) 0.00025(13) 0.00737(15) -0.00146(14)
Pb2 0.03987(13) 0.04187(14) 0.03670(14) -0.00144(10) 0.00902(11) 0.00025(10)
I1 0.0411(2) 0.0424(2) 0.0470(3) 0.0041(2) 0.0045(2) 0.00292(19)
I2 0.0690(2) 0.0509(3) 0.0399(2) -0.0031(2) 0.02500(18) -0.0158(2)
I3 0.0428(2) 0.0436(2) 0.0377(2) -0.00445(17) 0.01201(18) -0.00614(19)
I4 0.0459(2) 0.0599(3) 0.0499(3) 0.0002(2) 0.0036(2) 0.0052(2)
C1 0.058(3) 0.042(3) 0.040(3) 0.013(3) 0.005(3) -0.001(3)
C2 0.070(4) 0.076(4) 0.079(4) 0.002(3) 0.020(3) 0.001(3)
C3 0.078(4) 0.050(3) 0.049(3) -0.010(3) 0.009(3) -0.004(3)
N1 0.041(2) 0.055(3) 0.049(3) -0.009(2) 0.009(2) 0.000(2)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Pb1 I2 3.1905(5) . ?
Pb1 I2 3.1905(5) 3_767 ?
Pb1 I1 3.2282(5) . ?
Pb1 I1 3.2282(5) 3_767 ?
Pb1 I3 3.2327(5) 3_767 ?
Pb1 I3 3.2327(5) . ?
Pb2 I4 2.9810(6) . ?
Pb2 I3 3.1894(6) . ?
Pb2 I1 3.2341(6) 3_757 ?
Pb2 I2 3.2504(6) 3_767 ?
Pb2 I2 3.2897(6) 4_565 ?
I1 Pb2 3.2341(6) 3_757 ?
I2 Pb2 3.2504(6) 3_767 ?
I2 Pb2 3.2897(6) 4_566 ?
C1 C1 1.477(14) 3_657 ?
C1 N1 1.550(9) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 N1 1.494(8) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N1 1.533(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
N1 H1A 0.9100 . ?

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
I2 Pb1 I2 180.0 . 3_767 ?
I2 Pb1 I1 89.965(14) . . ?
I2 Pb1 I1 90.035(14) 3_767 . ?
I2 Pb1 I1 90.035(14) . 3_767 ?
I2 Pb1 I1 89.965(14) 3_767 3_767 ?
I1 Pb1 I1 180.0 . 3_767 ?
I2 Pb1 I3 88.819(13) . 3_767 ?
I2 Pb1 I3 91.181(13) 3_767 3_767 ?
I1 Pb1 I3 90.673(12) . 3_767 ?
I1 Pb1 I3 89.327(12) 3_767 3_767 ?
I2 Pb1 I3 91.181(13) . . ?
I2 Pb1 I3 88.819(13) 3_767 . ?
I1 Pb1 I3 89.327(12) . . ?
I1 Pb1 I3 90.673(12) 3_767 . ?
I3 Pb1 I3 180.0 3_767 . ?
I4 Pb2 I3 95.622(16) . . ?
I4 Pb2 I1 92.807(15) . 3_757 ?
I3 Pb2 I1 85.609(15) . 3_757 ?
I4 Pb2 I2 90.393(16) . 3_767 ?
I3 Pb2 I2 88.529(14) . 3_767 ?
I1 Pb2 I2 173.569(16) 3_757 3_767 ?
I4 Pb2 I2 94.516(16) . 4_565 ?
I3 Pb2 I2 168.948(14) . 4_565 ?
I1 Pb2 I2 98.287(15) 3_757 4_565 ?
I2 Pb2 I2 87.011(10) 3_767 4_565 ?
Pb1 I1 Pb2 96.584(13) . 3_757 ?
Pb1 I2 Pb2 91.035(14) . 3_767 ?
Pb1 I2 Pb2 132.565(17) . 4_566 ?
Pb2 I2 Pb2 135.936(17) 3_767 4_566 ?
Pb2 I3 Pb1 91.378(13) . . ?
C1 C1 N1 108.2(7) 3_657 . ?
C1 C1 H1B 110.1 3_657 . ?
N1 C1 H1B 110.1 . . ?
C1 C1 H1C 110.1 3_657 . ?
N1 C1 H1C 110.1 . . ?
H1B C1 H1C 108.4 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 N1 C3 112.8(6) . . ?
C2 N1 C1 109.0(6) . . ?
C3 N1 C1 109.9(5) . . ?
C2 N1 H1A 108.3 . . ?
C3 N1 H1A 108.3 . . ?
C1 N1 H1A 108.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A I1 0.91 2.83 3.655(6) 150.8 1_455

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.971
_refine_diff_density_min         -3.298
_refine_diff_density_rms         0.547
_database_code_depnum_ccdc_archive 'CCDC 995701'
