# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_x1
_database_code_depnum_ccdc_archive 'CCDC 1570129'
_audit_update_record             
;
2017-08-22 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H6 I3 N Pb'
_chemical_formula_weight         631.93

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           Hexagonal
_symmetry_space_group_name_H-M   P63/mmc

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

_cell_length_a                   8.7490(12)
_cell_length_b                   8.7490(12)
_cell_length_c                   8.2061(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     543.98(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3141
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      27.61

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    23.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0154
_exptl_absorpt_correction_T_max  0.0968
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4989
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         24.97
_reflns_number_total             212
_reflns_number_gt                205
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0380P)²+3.0548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         212
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0688
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_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
Pb01 Pb 0.0000 0.0000 0.5000 0.0423(4) Uani 1 12 d S . .
I002 I 0.16454(6) 0.32908(13) 0.7500 0.0794(5) Uani 1 4 d S . .
C1 C 0.3333 0.6667 0.111(4) 0.158(17) Uani 1 6 d S . .
N2 N 0.242(7) 0.621(4) 0.2500 0.15(3) Uani 0.33 4 d SP . .

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
Pb01 0.0405(4) 0.0405(4) 0.0458(6) 0.000 0.000 0.0202(2)
I002 0.0924(8) 0.0345(6) 0.0919(9) 0.000 0.000 0.0173(3)
C1 0.20(3) 0.20(3) 0.069(17) 0.000 0.000 0.101(14)
N2 0.05(3) 0.14(4) 0.23(8) 0.000 0.000 0.023(13)

_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
Pb01 I002 3.2289(8) 13_556 ?
Pb01 I002 3.2289(8) 14_556 ?
Pb01 I002 3.2289(8) . ?
Pb01 I002 3.2289(8) 2 ?
Pb01 I002 3.2289(8) 15_556 ?
Pb01 I002 3.2289(8) 3 ?
I002 Pb01 3.2289(8) 4 ?
C1 N2 1.34(4) . ?
C1 N2 1.34(4) 3_565 ?
C1 N2 1.34(4) 2_665 ?
N2 N2 1.20(9) 2_665 ?
N2 N2 1.20(9) 3_565 ?
N2 C1 1.34(4) 16_556 ?

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
I002 Pb01 I002 83.943(18) 13_556 14_556 ?
I002 Pb01 I002 180.0 13_556 . ?
I002 Pb01 I002 96.057(18) 14_556 . ?
I002 Pb01 I002 96.057(18) 13_556 2 ?
I002 Pb01 I002 180.0 14_556 2 ?
I002 Pb01 I002 83.942(18) . 2 ?
I002 Pb01 I002 83.943(18) 13_556 15_556 ?
I002 Pb01 I002 83.943(18) 14_556 15_556 ?
I002 Pb01 I002 96.057(18) . 15_556 ?
I002 Pb01 I002 96.058(18) 2 15_556 ?
I002 Pb01 I002 96.058(18) 13_556 3 ?
I002 Pb01 I002 96.058(18) 14_556 3 ?
I002 Pb01 I002 83.942(18) . 3 ?
I002 Pb01 I002 83.942(18) 2 3 ?
I002 Pb01 I002 180.0 15_556 3 ?
Pb01 I002 Pb01 78.89(2) . 4 ?
N2 C1 N2 54(4) . 3_565 ?
N2 C1 N2 54(4) . 2_665 ?
N2 C1 N2 54(4) 3_565 2_665 ?
N2 N2 N2 60.000(11) 2_665 3_565 ?
N2 N2 C1 63.2(18) 2_665 . ?
N2 N2 C1 63.2(18) 3_565 . ?
N2 N2 C1 63.2(18) 2_665 16_556 ?
N2 N2 C1 63.2(18) 3_565 16_556 ?
C1 N2 C1 117(4) . 16_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.133
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_x
_database_code_depnum_ccdc_archive 'CCDC 1570130'
_audit_update_record             
;
2017-08-22 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C1 H6 I3 N1 Pb'
_chemical_formula_weight         619.91

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'
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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pm-3m

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

_cell_length_a                   6.3026(13)
_cell_length_b                   6.3026(13)
_cell_length_c                   6.3026(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     250.36(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1076
_cell_measurement_theta_min      3.23
_cell_measurement_theta_max      27.26

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             248
_exptl_absorpt_coefficient_mu    26.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.005
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1387
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         27.26
_reflns_number_total             85
_reflns_number_gt                85
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0875P)²+2.6257P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.012(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         85
_refine_ls_number_parameters     6
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_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 0.0000 0.0000 0.0319(9) Uani 1 48 d S . .
I2 I 0.5000 0.0000 0.0000 0.131(2) Uani 1 16 d S . .
N1 N 0.5000 0.5000 0.5000 0.07(2) Uiso 1 48 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
Pb1 0.0319(9) 0.0319(9) 0.0319(9) 0.000 0.000 0.000
I2 0.0268(14) 0.183(3) 0.183(3) 0.000 0.000 0.000

_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 3.1513(6) 17 ?
Pb1 I2 3.1513(6) . ?
Pb1 I2 3.1513(6) 1_455 ?
Pb1 I2 3.1513(6) 2_545 ?
Pb1 I2 3.1513(6) 2 ?
Pb1 I2 3.1513(6) 17_554 ?
I2 Pb1 3.1513(6) 1_655 ?

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 90.0 17 . ?
I2 Pb1 I2 90.0 17 1_455 ?
I2 Pb1 I2 180.0 . 1_455 ?
I2 Pb1 I2 90.0 17 2_545 ?
I2 Pb1 I2 90.0 . 2_545 ?
I2 Pb1 I2 90.0 1_455 2_545 ?
I2 Pb1 I2 90.0 17 2 ?
I2 Pb1 I2 90.0 . 2 ?
I2 Pb1 I2 90.0 1_455 2 ?
I2 Pb1 I2 180.0 2_545 2 ?
I2 Pb1 I2 180.0 17 17_554 ?
I2 Pb1 I2 90.0 . 17_554 ?
I2 Pb1 I2 90.0 1_455 17_554 ?
I2 Pb1 I2 90.0 2_545 17_554 ?
I2 Pb1 I2 90.0 2 17_554 ?
Pb1 I2 Pb1 180.0 1_655 . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I2 Pb1 I2 Pb1 0.0 17 . . 1_655 ?
I2 Pb1 I2 Pb1 0.0 1_455 . . 1_655 ?
I2 Pb1 I2 Pb1 0.0 2_545 . . 1_655 ?
I2 Pb1 I2 Pb1 0.0 2 . . 1_655 ?
I2 Pb1 I2 Pb1 0.0 17_554 . . 1_655 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.26
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.041
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.292
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_x1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1570131'
_audit_update_record             
;
2017-08-22 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H6 I3 N Pb'
_chemical_formula_weight         631.93

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           Hexagonal
_symmetry_space_group_name_H-M   P63/mmc

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

_cell_length_a                   8.778(2)
_cell_length_b                   8.778(2)
_cell_length_c                   8.212(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     547.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1559
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      26.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    23.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2833
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         25.99
_reflns_number_total             233
_reflns_number_gt                218
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0863P)²+1.1140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         233
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1142
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_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
Pb01 Pb 1.0000 1.0000 0.5000 0.0432(6) Uani 1 12 d S . .
I002 I 0.83577(6) 0.67154(12) 0.2500 0.0809(8) Uani 1 4 d S . .
C1 C 0.6667 0.3333 0.888(7) 0.19(3) Uani 1 6 d S . .
N1 N 0.620(4) 0.240(9) 0.7500 0.17(6) Uani 0.33 4 d SP . .

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
Pb01 0.0388(7) 0.0388(7) 0.0521(9) 0.000 0.000 0.0194(3)
I002 0.0927(10) 0.0326(8) 0.0973(13) 0.000 0.000 0.0163(4)
C1 0.23(5) 0.23(5) 0.10(3) 0.000 0.000 0.11(2)
N1 0.12(4) 0.03(3) 0.33(18) 0.000 0.000 0.016(13)

_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
Pb01 I002 3.2325(9) 3_675 ?
Pb01 I002 3.2325(9) 14_566 ?
Pb01 I002 3.2325(9) 15_656 ?
Pb01 I002 3.2325(9) . ?
Pb01 I002 3.2325(9) 2_765 ?
Pb01 I002 3.2325(9) 13_776 ?
I002 Pb01 3.2325(9) 4_774 ?
C1 N1 1.34(6) 2_655 ?
C1 N1 1.34(6) 3_665 ?
C1 N1 1.34(6) . ?
N1 N1 1.23(11) 2_655 ?
N1 N1 1.23(11) 3_665 ?
N1 C1 1.34(6) 16_557 ?

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
I002 Pb01 I002 96.03(2) 3_675 14_566 ?
I002 Pb01 I002 180.0 3_675 15_656 ?
I002 Pb01 I002 83.97(2) 14_566 15_656 ?
I002 Pb01 I002 83.97(2) 3_675 . ?
I002 Pb01 I002 96.03(2) 14_566 . ?
I002 Pb01 I002 96.03(2) 15_656 . ?
I002 Pb01 I002 83.97(2) 3_675 2_765 ?
I002 Pb01 I002 180.0 14_566 2_765 ?
I002 Pb01 I002 96.03(2) 15_656 2_765 ?
I002 Pb01 I002 83.97(2) . 2_765 ?
I002 Pb01 I002 96.03(2) 3_675 13_776 ?
I002 Pb01 I002 83.97(2) 14_566 13_776 ?
I002 Pb01 I002 83.97(2) 15_656 13_776 ?
I002 Pb01 I002 180.0 . 13_776 ?
I002 Pb01 I002 96.03(2) 2_765 13_776 ?
Pb01 I002 Pb01 78.85(3) 4_774 . ?
N1 C1 N1 54(5) 2_655 3_665 ?
N1 C1 N1 54(5) 2_655 . ?
N1 C1 N1 54(5) 3_665 . ?
N1 N1 N1 60.000(1) 2_655 3_665 ?
N1 N1 C1 63(2) 2_655 16_557 ?
N1 N1 C1 63(2) 3_665 16_557 ?
N1 N1 C1 63(2) 2_655 . ?
N1 N1 C1 63(2) 3_665 . ?
C1 N1 C1 116(6) 16_557 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         3.258
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.289
