# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1-250K
_database_code_depnum_ccdc_archive 'CCDC 1523555'
_audit_update_record             
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.8294(7)
_cell_length_b                   10.3796(9)
_cell_length_c                   18.2256(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1481.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.4635
_cell_measurement_theta_max      25.7823

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
__exptl_crystal_size_max         0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    17.613
_shelx_estimated_absorpt_T_min   0.249
_shelx_estimated_absorpt_T_max   0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19298
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.832
_diffrn_reflns_theta_max         27.651
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1804
_reflns_number_gt                1546
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0513P)²+5.5026P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00160(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1804
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4574(12) 0.250000 0.6528(6) 0.041(2) Uani 1 2 d S T P . .
C2 C 0.5281(10) 0.1359(8) 0.6264(5) 0.0496(19) Uani 1 1 d . . . . .
H2 H 0.485557 0.056232 0.642681 0.060 Uiso 1 1 calc R U . . .
C3 C 0.6558(11) 0.1393(9) 0.5780(5) 0.058(2) Uani 1 1 d . . . . .
H3 H 0.699142 0.061238 0.559701 0.070 Uiso 1 1 calc R U . . .
C4 C 0.8647(19) 0.250000 0.4988(7) 0.094(6) Uani 1 2 d S T P . .
H4A H 0.852255 0.173770 0.467545 0.112 Uiso 0.5 1 calc R U P . .
H4B H 0.852255 0.326230 0.467545 0.112 Uiso 0.5 1 calc R U P . .
C5 C 1.0294(17) 0.250000 0.5295(9) 0.088(6) Uani 1 2 d S T P . .
H5A H 1.032882 0.309332 0.570620 0.132 Uiso 0.5 1 calc R U P . .
H5B H 1.111565 0.276744 0.492732 0.132 Uiso 0.5 1 calc R U P . .
H5C H 1.057329 0.163924 0.546420 0.132 Uiso 0.5 1 calc R U P . .
I1 I 0.95897(5) 0.03902(5) 0.31874(3) 0.04451(17) Uani 1 1 d . . . . .
I2 I 0.44915(7) 0.250000 0.38943(3) 0.03830(19) Uani 1 2 d S T P . .
N1 N 0.3309(14) 0.250000 0.7042(6) 0.064(3) Uani 1 2 d S T P . .
H1A H 0.292118 0.177433 0.721321 0.077 Uiso 0.5 1 calc R U P . .
H1B H 0.288858 0.322567 0.719838 0.077 Uiso 0.5 1 calc R U P . .
N2 N 0.7245(12) 0.250000 0.5546(5) 0.058(3) Uani 1 2 d S T P . .
Pb1 Pb 0.70965(4) 0.250000 0.24924(2) 0.02988(15) Uani 1 2 d S T P . .

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
C1 0.042(6) 0.042(5) 0.039(5) 0.000 -0.002(4) 0.000
C2 0.064(5) 0.036(4) 0.049(4) 0.004(3) 0.001(4) 0.004(3)
C3 0.066(5) 0.062(5) 0.047(4) -0.003(4) -0.001(4) 0.023(5)
C4 0.068(9) 0.174(18) 0.038(7) 0.000 0.012(7) 0.000
C5 0.052(8) 0.151(17) 0.062(9) 0.000 0.008(7) 0.000
I1 0.0410(3) 0.0411(3) 0.0514(3) 0.0065(2) -0.0003(2) -0.00188(19)
I2 0.0353(3) 0.0478(4) 0.0318(3) 0.000 -0.0007(2) 0.000
N1 0.068(7) 0.045(5) 0.078(7) 0.000 0.030(6) 0.000
N2 0.045(5) 0.093(8) 0.037(5) 0.000 0.006(4) 0.000
Pb1 0.0207(2) 0.0350(2) 0.0339(2) 0.000 0.00050(12) 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
C1 N1 1.363(14) . ?
C1 C2 1.393(9) . ?
C1 C2 1.393(9) 7_565 ?
C2 C3 1.334(12) . ?
C2 H2 0.9400 . ?
C3 N2 1.338(10) . ?
C3 H3 0.9400 . ?
C4 C5 1.41(2) . ?
C4 N2 1.496(16) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5A 0.97(16) 7_565 ?
C5 H5B 0.97(9) 7_565 ?
C5 H5C 0.97(7) 7_565 ?
I1 Pb1 3.1910(5) 6_656 ?
I1 Pb1 3.1954(5) . ?
I2 Pb1 3.1469(7) 6_556 ?
I2 Pb1 3.2692(7) . ?
N1 H1A 0.8700 . ?
N1 H1B 0.8700 . ?

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
N1 C1 C2 121.8(5) . . ?
N1 C1 C2 121.8(5) . 7_565 ?
C2 C1 C2 116.4(10) . 7_565 ?
C3 C2 C1 120.3(8) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 N2 122.3(8) . . ?
C2 C3 H3 118.8 . . ?
N2 C3 H3 118.8 . . ?
C5 C4 N2 113.7(11) . . ?
C5 C4 H4A 108.8 . . ?
N2 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
N2 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
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 . . ?
C4 C5 H5A 109(3) . 7_565 ?
H5A C5 H5A 78.8 . 7_565 ?
H5B C5 H5A 134.2 . 7_565 ?
H5C C5 H5A 33.3 . 7_565 ?
C4 C5 H5B 109(2) . 7_565 ?
H5A C5 H5B 134.2 . 7_565 ?
H5B C5 H5B 33.3 . 7_565 ?
H5C C5 H5B 78.8 . 7_565 ?
H5A C5 H5B 109.5 7_565 7_565 ?
C4 C5 H5C 109.5(14) . 7_565 ?
H5A C5 H5C 33.3 . 7_565 ?
H5B C5 H5C 78.8 . 7_565 ?
H5C C5 H5C 134.2 . 7_565 ?
H5A C5 H5C 109.5 7_565 7_565 ?
H5B C5 H5C 109.5 7_565 7_565 ?
Pb1 I1 Pb1 75.612(12) 6_656 . ?
Pb1 I2 Pb1 75.173(15) 6_556 . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C3 N2 C3 118.3(10) 7_565 . ?
C3 N2 C4 120.8(5) 7_565 . ?
C3 N2 C4 120.8(5) . . ?
I2 Pb1 I1 93.134(14) 6_656 6_556 ?
I2 Pb1 I1 93.134(14) 6_656 4_455 ?
I1 Pb1 I1 86.67(2) 6_556 4_455 ?
I2 Pb1 I1 87.383(14) 6_656 . ?
I1 Pb1 I1 93.401(16) 6_556 . ?
I1 Pb1 I1 179.473(13) 4_455 . ?
I2 Pb1 I1 87.383(14) 6_656 7_565 ?
I1 Pb1 I1 179.473(13) 6_556 7_565 ?
I1 Pb1 I1 93.401(16) 4_455 7_565 ?
I1 Pb1 I1 86.523(19) . 7_565 ?
I2 Pb1 I2 177.974(19) 6_656 . ?
I1 Pb1 I2 85.395(14) 6_556 . ?
I1 Pb1 I2 85.395(14) 4_455 . ?
I1 Pb1 I2 94.090(14) . . ?
I1 Pb1 I2 94.090(14) 7_565 . ?

_refine_diff_density_max         1.539
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.191

_structure_special_details       
;
 This structure is part of a multi-temperature experiment.
;

_shelx_res_file                  
;
TITL 13 in Pnma
    13.res
    created by SHELXL-2016/6 at 16:00:03 on 18-Dec-2016
CELL 0.71073   7.8294  10.3796  18.2256  90.000  90.000  90.000
ZERR   4.00   0.0007   0.0009   0.0016   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC C  H  N  I  Pb
UNIT 28  44  8  12  4
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 20
TEMP -23.560
WGHT    0.051300    5.502600
EXTI    0.001604
FVAR       0.06133
MOLE 1
C1    1    0.457424    0.250000    0.652842    10.50000    0.04154    0.04175 =
         0.03896    0.00000   -0.00226    0.00000
C2    1    0.528080    0.135938    0.626377    11.00000    0.06390    0.03583 =
         0.04919    0.00395    0.00077    0.00362
AFIX  43
H2    2    0.485557    0.056232    0.642681    11.00000   -1.20000
AFIX   0
C3    1    0.655814    0.139348    0.577998    11.00000    0.06569    0.06208 =
         0.04719   -0.00307   -0.00132    0.02308
AFIX  43
H3    2    0.699142    0.061238    0.559701    11.00000   -1.20000
AFIX   0
C4    1    0.864660    0.250000    0.498821    10.50000    0.06849    0.17435 =
         0.03772    0.00000    0.01217    0.00000
AFIX  23
H4A   2    0.852255    0.173770    0.467545    10.50000   -1.20000
H4B   2    0.852255    0.326230    0.467545    10.50000   -1.20000
AFIX   0
C5    1    1.029375    0.250000    0.529528    10.50000    0.05175    0.15137 =
         0.06155    0.00000    0.00849    0.00000
AFIX 137
H5A   2    1.032882    0.309332    0.570620    10.50000   -1.50000
H5B   2    1.111565    0.276744    0.492732    10.50000   -1.50000
H5C   2    1.057329    0.163924    0.546420    10.50000   -1.50000
AFIX   0
I1    4    0.958970    0.039022    0.318738    11.00000    0.04100    0.04112 =
         0.05140    0.00648   -0.00028   -0.00188
I2    4    0.449146    0.250000    0.389426    10.50000    0.03526    0.04782 =
         0.03183    0.00000   -0.00074    0.00000
N1    3    0.330878    0.250000    0.704190    10.50000    0.06843    0.04528 =
         0.07840    0.00000    0.02969    0.00000
AFIX  93
H1A   2    0.292118    0.177433    0.721321    10.50000   -1.20000
H1B   2    0.288858    0.322567    0.719838    10.50000   -1.20000
AFIX   0
N2    3    0.724472    0.250000    0.554585    10.50000    0.04540    0.09296 =
         0.03662    0.00000    0.00606    0.00000
PB1   5    0.709648    0.250000    0.249240    10.50000    0.02075    0.03500 =
         0.03389    0.00000    0.00050    0.00000
HKLF 4




REM  13 in Pnma
REM R1 =  0.0301 for    1546 Fo > 4sig(Fo)  and  0.0378 for all    1804 data
REM     72 parameters refined using      0 restraints

END

WGHT      0.0508      5.0720

REM Highest difference peak  1.539,  deepest hole -1.191,  1-sigma level  0.191
Q1    1   0.7923  0.2500  0.2495  10.50000  0.05    1.54
Q2    1   0.7136  0.2500  0.2830  10.50000  0.05    1.54
Q3    1   0.7054  0.2500  0.2133  10.50000  0.05    1.52
Q4    1   0.7172  0.1877  0.2485  11.00000  0.05    1.35
Q5    1   0.6274  0.2500  0.2499  10.50000  0.05    1.21
Q6    1   0.5631  0.2500  0.3935  10.50000  0.05    0.86
Q7    1   0.5171  0.2500  0.3329  10.50000  0.05    0.71
Q8    1   0.8321  0.0511  0.3215  11.00000  0.05    0.69
Q9    1   0.6214  0.2500  0.1906  10.50000  0.05    0.63
Q10   1   1.0809  0.0797  0.3190  11.00000  0.05    0.62
Q11   1   0.8923  0.1953  0.2509  11.00000  0.05    0.62
Q12   1   0.2373  0.2500  0.3963  10.50000  0.05    0.60
Q13   1   0.6214  0.2500  0.3080  10.50000  0.05    0.60
Q14   1   1.2028  0.0605  0.3147  11.00000  0.05    0.60
Q15   1   0.5407  0.2500  0.4516  10.50000  0.05    0.58
Q16   1   0.9351  0.2500  0.3918  10.50000  0.05    0.58
Q17   1   0.7468  0.2500  0.3974  10.50000  0.05    0.58
Q18   1   0.3728  0.1884  0.3917  11.00000  0.05    0.57
Q19   1   0.9152  0.1303  0.3175  11.00000  0.05    0.55
Q20   1   1.0645  0.2500  0.5436  10.50000  0.05    0.53
;
_shelx_res_checksum              40040
####################################################################### 
# 
# 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_15
_database_code_depnum_ccdc_archive 'CCDC 1523557'
_audit_update_record             
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_15                  
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
_vrf_PLAT020_15                  
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.573 Report
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
_vrf_PLAT971_15                  
;
PROBLEM: Check Calcd Residual Density  0.86A From     Pb1       4.39 eA-3
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
_vrf_PLAT973_15                  
;
PROBLEM: Check Calcd Positive Residual Density on     Pb1       3.77 eA-3
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
# Added during the CSD deposition process: Sunday 15 January 2017 08:06 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H11 I3 N2 Pb'
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.8530(15)
_cell_length_b                   10.418(2)
_cell_length_c                   18.343(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1500.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.4635
_cell_measurement_theta_max      25.7823

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    17.384
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_T_max  0.240
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15166
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_av_R_equivalents  0.5734
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.822
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1403
_reflns_number_gt                1102
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1074P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0034(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1403
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2016
_refine_ls_wR_factor_gt          0.1928
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.460(3) 0.250000 0.6509(12) 0.057(5) Uani 1 2 d S T P . .
C2 C 0.538(3) 0.1349(18) 0.6240(11) 0.088(6) Uani 1 1 d . . . . .
H2 H 0.499358 0.055408 0.640081 0.105 Uiso 1 1 calc R U . . .
C3 C 0.658(2) 0.1403(17) 0.5794(10) 0.080(5) Uani 1 1 d . . . . .
H3 H 0.706125 0.064256 0.562663 0.096 Uiso 1 1 calc R U . . .
C4 C 0.865(3) 0.250000 0.5020(16) 0.128(14) Uani 1 2 d S T P . .
H4A H 0.853371 0.175023 0.470994 0.153 Uiso 0.5 1 calc R U P . .
H4B H 0.853371 0.324977 0.470994 0.153 Uiso 0.5 1 calc R U P . .
C5 C 1.032(3) 0.250000 0.5320(19) 0.17(2) Uani 1 2 d S T P . .
H5A H 1.047141 0.174009 0.562882 0.252 Uiso 0.5 1 d R U P . .
H5B H 1.048582 0.327602 0.561422 0.252 Uiso 0.5 1 d R U P . .
H5C H 1.116534 0.250000 0.492563 0.252 Uiso 1 2 d R U P . .
I1 I 0.95724(12) 0.04008(10) 0.31816(5) 0.0640(5) Uani 1 1 d . . . . .
I2 I 0.44821(16) 0.250000 0.38854(7) 0.0562(5) Uani 1 2 d S T P . .
N1 N 0.338(3) 0.250000 0.7005(12) 0.080(6) Uani 1 2 d S T P . .
H1A H 0.301701 0.321381 0.718257 0.095 Uiso 0.5 1 calc R U P . .
H1B H 0.294392 0.178619 0.714963 0.095 Uiso 0.5 1 calc R U P . .
N2 N 0.718(3) 0.250000 0.5552(9) 0.090(7) Uani 1 2 d S T P . .
Pb1 Pb 0.70833(9) 0.250000 0.24909(3) 0.0448(4) Uani 1 2 d S T P . .

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
C1 0.057(15) 0.043(11) 0.070(13) 0.000 -0.009(10) 0.000
C2 0.13(2) 0.036(9) 0.100(13) 0.003(9) 0.013(13) -0.004(9)
C3 0.086(12) 0.057(11) 0.096(11) 0.011(9) 0.021(11) 0.026(9)
C4 0.053(16) 0.26(5) 0.074(15) 0.000 0.011(13) 0.000
C5 0.023(15) 0.36(7) 0.13(3) 0.000 0.014(13) 0.000
I1 0.0583(8) 0.0479(7) 0.0857(9) 0.0112(5) -0.0008(5) -0.0017(4)
I2 0.0512(9) 0.0563(9) 0.0609(9) 0.000 -0.0013(6) 0.000
N1 0.071(13) 0.043(10) 0.125(16) 0.000 0.022(13) 0.000
N2 0.055(12) 0.17(2) 0.050(10) 0.000 0.004(9) 0.000
Pb1 0.0304(6) 0.0406(6) 0.0633(7) 0.000 -0.0001(3) 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
C1 N1 1.32(3) . ?
C1 C2 1.44(2) 7_565 ?
C1 C2 1.44(2) . ?
C2 C3 1.25(2) . ?
C2 H2 0.9300 . ?
C3 N2 1.313(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.43(4) . ?
C4 N2 1.51(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9799 . ?
I1 Pb1 3.1925(11) 6_656 ?
I1 Pb1 3.1950(11) . ?
I2 Pb1 3.1500(15) 6_556 ?
I2 Pb1 3.2734(15) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?

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
N1 C1 C2 123.2(11) . 7_565 ?
N1 C1 C2 123.2(11) . . ?
C2 C1 C2 113(2) 7_565 . ?
C3 C2 C1 120.7(18) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 N2 122.1(18) . . ?
C2 C3 H3 119.0 . . ?
N2 C3 H3 119.0 . . ?
C5 C4 N2 117(2) . . ?
C5 C4 H4A 108.0 . . ?
N2 C4 H4A 108.0 . . ?
C5 C4 H4B 108.0 . . ?
N2 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.7 . . ?
H5A C5 H5C 110.3 . . ?
H5B C5 H5C 108.6 . . ?
Pb1 I1 Pb1 75.87(3) 6_656 . ?
Pb1 I2 Pb1 75.34(3) 6_556 . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C3 N2 C3 121(2) 7_565 . ?
C3 N2 C4 119.5(11) 7_565 . ?
C3 N2 C4 119.4(11) . . ?
I2 Pb1 I1 93.42(3) 6_656 6_556 ?
I2 Pb1 I1 93.42(3) 6_656 4_455 ?
I1 Pb1 I1 86.47(4) 6_556 4_455 ?
I2 Pb1 I1 87.24(3) 6_656 . ?
I1 Pb1 I1 93.57(4) 6_556 . ?
I1 Pb1 I1 179.33(3) 4_455 . ?
I2 Pb1 I1 87.24(3) 6_656 7_565 ?
I1 Pb1 I1 179.33(3) 6_556 7_565 ?
I1 Pb1 I1 93.57(4) 4_455 7_565 ?
I1 Pb1 I1 86.39(4) . 7_565 ?
I2 Pb1 I2 178.12(4) 6_656 . ?
I1 Pb1 I2 85.21(3) 6_556 . ?
I1 Pb1 I2 85.21(3) 4_455 . ?
I1 Pb1 I2 94.13(3) . . ?
I1 Pb1 I2 94.13(3) 7_565 . ?

_refine_diff_density_max         4.040
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.463

_structure_special_details       
;
 This structure is part of a multi-temperature experiment.
;

_shelx_res_file                  
;
TITL 15 in Pnma
    15.res
    created by SHELXL-2016/6 at 21:18:12 on 09-Jan-2017
CELL 0.71073   7.8530  10.4176  18.3429  90.000  90.000  90.000
ZERR   4.00   0.0015   0.0021   0.0037   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC C  H  N  I  Pb
UNIT 28  44  8  12  4
OMIT 0 50
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 20
TEMP 77
WGHT    0.107400
EXTI    0.003374
FVAR       0.05861
MOLE 1
C1    1    0.459739    0.250000    0.650861    10.50000    0.05722    0.04294 =
         0.06962    0.00000   -0.00893    0.00000
C2    1    0.538148    0.134879    0.624028    11.00000    0.12656    0.03646 =
         0.10030    0.00280    0.01339   -0.00398
AFIX  43
H2    2    0.499358    0.055408    0.640081    11.00000   -1.20000
AFIX   0
C3    1    0.657888    0.140303    0.579359    11.00000    0.08598    0.05680 =
         0.09634    0.01122    0.02072    0.02567
AFIX  43
H3    2    0.706125    0.064256    0.562663    11.00000   -1.20000
AFIX   0
C4    1    0.864571    0.250000    0.501982    10.50000    0.05321    0.25607 =
         0.07409    0.00000    0.01125    0.00000
AFIX  23
H4A   2    0.853371    0.175023    0.470994    10.50000   -1.20000
H4B   2    0.853371    0.324977    0.470994    10.50000   -1.20000
AFIX   0
C5    1    1.032434    0.250000    0.532025    10.50000    0.02337    0.35623 =
         0.12535    0.00000    0.01353    0.00000
AFIX   3
H5A   2    1.047141    0.174009    0.562882    10.50000   -1.50000
H5B   2    1.048582    0.327602    0.561422    10.50000   -1.50000
H5C   2    1.116534    0.250000    0.492563    10.50000   -1.50000
AFIX   0
I1    4    0.957237    0.040080    0.318155    11.00000    0.05827    0.04794 =
         0.08567    0.01118   -0.00077   -0.00174
I2    4    0.448213    0.250000    0.388544    10.50000    0.05121    0.05634 =
         0.06093    0.00000   -0.00133    0.00000
N1    3    0.337749    0.250000    0.700466    10.50000    0.07104    0.04269 =
         0.12502    0.00000    0.02236    0.00000
AFIX  93
H1A   2    0.301701    0.321381    0.718257    10.50000   -1.20000
H1B   2    0.294392    0.178619    0.714963    10.50000   -1.20000
AFIX   0
N2    3    0.717844    0.250000    0.555216    10.50000    0.05520    0.16625 =
         0.04962    0.00000    0.00445    0.00000
PB1   5    0.708329    0.250000    0.249095    10.50000    0.03041    0.04061 =
         0.06334    0.00000   -0.00007    0.00000
HKLF 4




REM  15 in Pnma
REM R1 =  0.0729 for    1102 Fo > 4sig(Fo)  and  0.0842 for all    1403 data
REM     71 parameters refined using      0 restraints

END

WGHT      0.1074      0.0000

REM Highest difference peak  4.040,  deepest hole -2.370,  1-sigma level  0.463
Q1    1   0.7066  0.2500  0.2895  10.50000  0.05    4.04
Q2    1   0.6983  0.2500  0.2078  10.50000  0.05    3.91
Q3    1   0.4531  0.2332  0.3418  11.00000  0.05    2.32
Q4    1   0.9486  0.0623  0.3707  11.00000  0.05    1.84
Q5    1   0.4215  0.2500  0.4398  10.50000  0.05    1.81
Q6    1   0.8559  0.2500  0.1995  10.50000  0.05    1.34
Q7    1   0.9552  0.0079  0.2716  11.00000  0.05    1.21
Q8    1   0.9552  0.0727  0.2712  11.00000  0.05    1.14
Q9    1   0.9560  0.1891  0.2324  11.00000  0.05    1.03
Q10   1   0.7043  0.0850  0.2437  11.00000  0.05    0.98
Q11   1   0.7169  0.1060  0.1848  11.00000  0.05    0.86
Q12   1   0.7419  0.2500  0.4027  10.50000  0.05    0.86
Q13   1   0.5211  0.2500  0.2433  10.50000  0.05    0.86
Q14   1   0.5045  0.1461  0.6318  11.00000  0.05    0.80
Q15   1   0.4786  0.2500  0.7714  10.50000  0.05    0.79
Q16   1   0.4799  0.2500  0.7418  10.50000  0.05    0.79
Q17   1   0.7791  0.2500  0.5387  10.50000  0.05    0.77
Q18   1   0.7189  0.2500  0.5190  10.50000  0.05    0.75
Q19   1   0.2405  0.2500  0.4017  10.50000  0.05    0.74
Q20   1   0.3405  0.1156  0.3194  11.00000  0.05    0.72
;
_shelx_res_checksum              24776
####################################################################### 
# 
# 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_1-200K
_database_code_depnum_ccdc_archive 'CCDC 1523554'
_audit_update_record             
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.8158(8)
_cell_length_b                   10.3604(10)
_cell_length_c                   18.1750(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1471.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.4635
_cell_measurement_theta_max      25.7823

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.209
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    17.726
_shelx_estimated_absorpt_T_min   0.249
_shelx_estimated_absorpt_T_max   0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19146
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.837
_diffrn_reflns_theta_max         27.653
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1804
_reflns_number_gt                1586
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²+9.6792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1804
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4555(12) 0.2500 0.6535(6) 0.033(2) Uani 1 2 d S T P . .
C2 C 0.5268(10) 0.1347(8) 0.6270(5) 0.0403(18) Uani 1 1 d . . . . .
H2 H 0.4837 0.0540 0.6436 0.048 Uiso 1 1 calc R U . . .
C3 C 0.6560(11) 0.1382(9) 0.5783(4) 0.047(2) Uani 1 1 d . . . . .
H3 H 0.7009 0.0592 0.5601 0.056 Uiso 1 1 calc R U . . .
C4 C 0.8639(17) 0.2500 0.4987(6) 0.070(5) Uani 1 2 d S T P . .
H4A H 0.8515 0.1728 0.4670 0.084 Uiso 0.5 1 calc R U P . .
H4B H 0.8515 0.3272 0.4670 0.084 Uiso 0.5 1 calc R U P . .
C5 C 1.0301(16) 0.2500 0.5300(9) 0.072(5) Uani 1 2 d S T P . .
H5A H 1.0326 0.3086 0.5723 0.108 Uiso 0.5 1 calc R U P . .
H5B H 1.1132 0.2789 0.4931 0.108 Uiso 0.5 1 calc R U P . .
H5C H 1.0593 0.1625 0.5461 0.108 Uiso 0.5 1 calc R U P . .
I1 I 0.95981(5) 0.03855(5) 0.31900(3) 0.03533(15) Uani 1 1 d . . . . .
I2 I 0.44957(7) 0.2500 0.38981(3) 0.02990(17) Uani 1 2 d S T P . .
N1 N 0.3297(13) 0.2500 0.7049(6) 0.048(3) Uani 1 2 d S T P . .
H1A H 0.2909 0.1765 0.7225 0.058 Uiso 0.5 1 calc R U P . .
H1B H 0.2869 0.3235 0.7207 0.058 Uiso 0.5 1 calc R U P . .
N2 N 0.7236(12) 0.2500 0.5545(5) 0.048(3) Uani 1 2 d S T P . .
Pb1 Pb 0.71045(4) 0.2500 0.24930(2) 0.02276(13) Uani 1 2 d S T P . .

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
C1 0.033(5) 0.034(5) 0.033(5) 0.000 -0.003(4) 0.000
C2 0.051(5) 0.029(3) 0.040(4) 0.002(3) 0.003(3) 0.002(3)
C3 0.050(5) 0.053(5) 0.037(4) -0.004(4) -0.001(4) 0.020(4)
C4 0.045(7) 0.142(15) 0.022(5) 0.000 0.005(5) 0.000
C5 0.033(7) 0.125(15) 0.057(9) 0.000 0.013(6) 0.000
I1 0.0319(3) 0.0332(3) 0.0409(3) 0.00428(19) 0.00000(19) -0.00154(17)
I2 0.0271(3) 0.0382(3) 0.0245(3) 0.000 -0.0007(2) 0.000
N1 0.048(6) 0.039(5) 0.058(6) 0.000 0.023(5) 0.000
N2 0.035(5) 0.081(8) 0.028(5) 0.000 0.005(4) 0.000
Pb1 0.01522(19) 0.02766(19) 0.0254(2) 0.000 0.00049(12) 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
C1 N1 1.357(14) . ?
C1 C2 1.403(9) . ?
C1 C2 1.403(9) 7_565 ?
C2 C3 1.343(12) . ?
C3 N2 1.345(10) . ?
C4 C5 1.418(19) . ?
C4 N2 1.495(15) . ?
I1 Pb1 3.1902(5) 6_656 ?
I1 Pb1 3.1941(5) . ?
I2 Pb1 3.1441(7) 6_556 ?
I2 Pb1 3.2680(7) . ?
N2 C3 1.345(10) 7_565 ?
Pb1 I2 3.1441(7) 6_656 ?
Pb1 I1 3.1902(5) 6_556 ?
Pb1 I1 3.1902(5) 4_455 ?
Pb1 I1 3.1941(5) 7_565 ?

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
N1 C1 C2 121.6(5) . . ?
N1 C1 C2 121.6(5) . 7_565 ?
C2 C1 C2 116.7(10) . 7_565 ?
C3 C2 C1 120.1(8) . . ?
C2 C3 N2 122.0(8) . . ?
C5 C4 N2 113.6(11) . . ?
Pb1 I1 Pb1 75.485(13) 6_656 . ?
Pb1 I2 Pb1 75.075(16) 6_556 . ?
C3 N2 C3 119.0(10) . 7_565 ?
C3 N2 C4 120.4(5) . . ?
C3 N2 C4 120.4(5) 7_565 . ?
I2 Pb1 I1 92.987(15) 6_656 6_556 ?
I2 Pb1 I1 92.987(15) 6_656 4_455 ?
I1 Pb1 I1 86.74(2) 6_556 4_455 ?
I2 Pb1 I1 87.493(14) 6_656 7_565 ?
I1 Pb1 I1 179.511(13) 6_556 7_565 ?
I1 Pb1 I1 93.327(16) 4_455 7_565 ?
I2 Pb1 I1 87.493(14) 6_656 . ?
I1 Pb1 I1 93.327(16) 6_556 . ?
I1 Pb1 I1 179.511(13) 4_455 . ?
I1 Pb1 I1 86.61(2) 7_565 . ?
I2 Pb1 I2 177.867(19) 6_656 . ?
I1 Pb1 I2 85.466(14) 6_556 . ?
I1 Pb1 I2 85.466(14) 4_455 . ?
I1 Pb1 I2 94.056(15) 7_565 . ?
I1 Pb1 I2 94.056(15) . . ?

_refine_diff_density_max         1.086
_refine_diff_density_min         -2.136
_refine_diff_density_rms         0.294

_structure_special_details       
;
 This structure is part of a multi-temperature experiment.
;
_shelx_res_file                  
;

    12.res created by SHELXL-2014/7

TITL 12 in Pnma
CELL 0.71073   7.8158  10.3604  18.1750  90.000  90.000  90.000
ZERR   14.00   0.0008   0.0010   0.0018   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC C  H  N  I  Pb
UNIT 13 13 13 13 13
L.S. 88
ACTA
BOND
FMAP 2
PLAN 20
TEMP -123.560
WGHT    0.049500    9.679200
FVAR       0.05831
MOLE 1
C1    1    0.455499    0.250000    0.653515    10.50000    0.03264    0.03391 =
         0.03266    0.00000   -0.00322    0.00000
C2    1    0.526827    0.134689    0.627030    11.00000    0.05104    0.02942 =
         0.04032    0.00154    0.00262    0.00226
AFIX  43
H2    2    0.483696    0.054035    0.643593    11.00000   -1.20000
AFIX   0
C3    1    0.655962    0.138159    0.578306    11.00000    0.05007    0.05292 =
         0.03691   -0.00413   -0.00062    0.02010
AFIX  43
H3    2    0.700915    0.059190    0.560085    11.00000   -1.20000
AFIX   0
C4    1    0.863938    0.250000    0.498684    10.50000    0.04539    0.14246 =
         0.02163    0.00000    0.00549    0.00000
AFIX  23
H4A   2    0.851525    0.172840    0.466999    10.50000   -1.20000
H4B   2    0.851525    0.327160    0.466999    10.50000   -1.20000
AFIX   0
C5    1    1.030094    0.250000    0.529969    10.50000    0.03277    0.12534 =
         0.05740    0.00000    0.01288    0.00000
AFIX 137
H5A   2    1.032649    0.308623    0.572271    10.50000   -1.50000
H5B   2    1.113238    0.278890    0.493121    10.50000   -1.50000
H5C   2    1.059253    0.162487    0.546142    10.50000   -1.50000
AFIX   0
I1    4    0.959811    0.038551    0.319001    11.00000    0.03190    0.03320 =
         0.04088    0.00428    0.00000   -0.00154
I2    4    0.449573    0.250000    0.389813    10.50000    0.02709    0.03816 =
         0.02445    0.00000   -0.00065    0.00000
N1    3    0.329693    0.250000    0.704934    10.50000    0.04786    0.03895 =
         0.05817    0.00000    0.02280    0.00000
AFIX  93
H1A   2    0.290862    0.176473    0.722506    10.50000   -1.20000
H1B   2    0.286911    0.323527    0.720718    10.50000   -1.20000
AFIX   0
N2    3    0.723567    0.250000    0.554528    10.50000    0.03451    0.08099 =
         0.02751    0.00000    0.00494    0.00000
PB1   5    0.710453    0.250000    0.249296    10.50000    0.01522    0.02766 =
         0.02540    0.00000    0.00049    0.00000
HKLF 4

REM  12 in Pnma
REM R1 =  0.0333 for    1586 Fo > 4sig(Fo)  and  0.0391 for all    1804 data
REM     71 parameters refined using      0 restraints

END

WGHT      0.0495      9.6771

REM Highest difference peak  1.086,  deepest hole -2.136,  1-sigma level  0.294
Q1    1   0.7083  0.2500  0.2874  10.50000  0.05    1.09
Q2    1   0.7065  0.2500  0.2106  10.50000  0.05    1.07
Q3    1   0.6111  0.2500  0.2496  10.50000  0.05    1.00
Q4    1   0.7142  0.1573  0.3040  11.00000  0.05    0.85
Q5    1   0.7019  0.1830  0.2484  11.00000  0.05    0.82
Q6    1   0.7905  0.2500  0.2508  10.50000  0.05    0.82
Q7    1   0.5950  0.2127  0.1861  11.00000  0.05    0.79
Q8    1   0.7266  0.1656  0.1936  11.00000  0.05    0.76
Q9    1   0.5194  0.2500  0.3233  10.50000  0.05    0.71
Q10   1   1.0221  0.1463  0.2541  11.00000  0.05    0.71
Q11   1   0.6185  0.2500  0.3135  10.50000  0.05    0.70
Q12   1   0.9839  0.1271  0.2548  11.00000  0.05    0.69
Q13   1   0.9849  0.2249  0.3187  11.00000  0.05    0.66
Q14   1   0.8312  0.2069  0.3132  11.00000  0.05    0.66
Q15   1   0.8202  0.2157  0.1801  11.00000  0.05    0.65
Q16   1   0.7813  0.1181  0.3274  11.00000  0.05    0.64
Q17   1   0.6946  0.0766  0.2463  11.00000  0.05    0.63
Q18   1   0.8267  0.0492  0.3210  11.00000  0.05    0.63
Q19   1   0.5965  0.1978  0.3118  11.00000  0.05    0.62
Q20   1   0.2680  0.1382  0.3937  11.00000  0.05    0.62
;
_shelx_res_checksum              96404
####################################################################### 
# 
# 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_1-300K
_database_code_depnum_ccdc_archive 'CCDC 1523556'
_audit_update_record             
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_1-300K              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
_vrf_PLAT971_1-300K              
;
PROBLEM: Check Calcd Residual Density  0.85A From     Pb1       3.73 eA-3
RESPONSE: However, when the temperature is higher than 300K, the single crystal X-ray diffraction data is bad due to intense thermal motion of organic cation. 
;
# Added during the CSD deposition process: Sunday 15 January 2017 08:06 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H11 I3 N2 Pb'
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.8382(6)
_cell_length_b                   10.3922(7)
_cell_length_c                   18.2707(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1488.26(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.4635
_cell_measurement_theta_max      25.7823

_exptl_crystal_description       needele
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.174
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    17.528
_shelx_estimated_absorpt_T_min   0.249
_shelx_estimated_absorpt_T_max   0.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16469
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_av_R_equivalents  0.2793
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.425
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1393
_reflns_number_gt                1249
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1381P)²+6.2294P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1393
_refine_ls_number_parameters     96
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1941
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.041
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4579(19) 0.250000 0.6518(12) 0.047(5) Uani 1 2 d S T P . .
C2 C 0.530(2) 0.1335(15) 0.6266(8) 0.062(4) Uani 1 1 d . . . . .
H2 H 0.488765 0.054629 0.642835 0.074 Uiso 1 1 calc R U . . .
C3 C 0.659(2) 0.1396(16) 0.5789(8) 0.065(4) Uani 1 1 d . . . . .
H3 H 0.703781 0.063019 0.561087 0.078 Uiso 1 1 calc R U . . .
C4A C 0.874(4) 0.287(7) 0.5035(18) 0.073(6) Uani 0.37(2) 1 d D U P A -1
H4A1 H 0.854709 0.247941 0.456055 0.088 Uiso 0.37(2) 1 calc R U P A -1
H4A2 H 0.874753 0.379698 0.496874 0.088 Uiso 0.37(2) 1 calc R U P A -1
C5A C 1.034(3) 0.248(19) 0.5295(17) 0.073(7) Uani 0.37(2) 1 d D U P A -1
H5A1 H 1.061772 0.296081 0.572918 0.110 Uiso 0.37(2) 1 calc R U P A -1
H5A2 H 1.119086 0.264277 0.492729 0.110 Uiso 0.37(2) 1 calc R U P A -1
H5A3 H 1.031465 0.158129 0.540728 0.110 Uiso 0.37(2) 1 calc R U P A -1
C4B C 0.850(13) 0.223(14) 0.492(4) 0.073(6) Uani 0.13(2) 1 d D U P A -2
H4B1 H 0.785681 0.200446 0.448221 0.087 Uiso 0.13(2) 1 calc R U P A -2
H4B2 H 0.914882 0.300323 0.481013 0.087 Uiso 0.13(2) 1 calc R U P A -2
C5B C 0.963(10) 0.123(12) 0.508(6) 0.075(8) Uani 0.13(2) 1 d D U P A -2
H5B1 H 1.072225 0.138812 0.486270 0.112 Uiso 0.13(2) 1 d R U P A -2
H5B2 H 0.917814 0.043184 0.490196 0.112 Uiso 0.13(2) 1 d R U P A -2
H5B3 H 0.976594 0.117108 0.560611 0.112 Uiso 0.13(2) 1 d R U P A -2
I1 I 0.95827(10) 0.03946(9) 0.31848(5) 0.0522(4) Uani 1 1 d . . . . .
I2 I 0.44858(13) 0.250000 0.38895(6) 0.0453(4) Uani 1 2 d S T P . .
N1 N 0.334(2) 0.250000 0.7028(10) 0.064(4) Uani 1 2 d S T P . .
H1A H 0.297799 0.321584 0.720520 0.076 Uiso 0.5 1 calc R U P . .
H1B H 0.291437 0.178416 0.717677 0.076 Uiso 0.5 1 calc R U P . .
N2 N 0.7252(18) 0.250000 0.5557(8) 0.072(5) Uani 1 2 d DS TU P . .
Pb1 Pb 0.70892(7) 0.250000 0.24918(3) 0.0357(4) Uani 1 2 d S T P . .

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
C1 0.040(11) 0.036(10) 0.066(11) 0.000 -0.003(7) 0.000
C2 0.096(13) 0.027(7) 0.063(8) 0.001(6) -0.004(7) 0.012(7)
C3 0.064(9) 0.062(9) 0.070(8) 0.005(7) 0.015(8) 0.029(8)
C4A 0.034(9) 0.135(18) 0.051(9) 0.001(8) 0.010(7) 0.003(7)
C5A 0.034(9) 0.13(2) 0.053(11) 0.002(14) 0.014(8) 0.003(13)
C4B 0.034(9) 0.135(18) 0.049(9) 0.001(8) 0.007(8) 0.001(8)
C5B 0.037(13) 0.13(2) 0.053(14) 0.003(13) 0.007(12) 0.001(10)
I1 0.0460(7) 0.0391(6) 0.0716(7) 0.0085(4) -0.0002(3) -0.0016(3)
I2 0.0403(7) 0.0466(8) 0.0490(7) 0.000 -0.0018(4) 0.000
N1 0.057(10) 0.045(9) 0.089(11) 0.000 0.012(9) 0.000
N2 0.034(7) 0.136(16) 0.047(7) 0.000 0.004(6) 0.000
Pb1 0.0225(5) 0.0329(5) 0.0517(5) 0.000 0.0002(2) 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
C1 N1 1.34(3) . ?
C1 C2 1.413(17) 7_565 ?
C1 C2 1.413(17) . ?
C2 C3 1.33(2) . ?
C2 H2 0.9300 . ?
C3 N2 1.330(17) . ?
C3 H3 0.9300 . ?
C4A C5A 1.40(2) . ?
C4A N2 1.557(18) . ?
C4A H4A1 0.9700 . ?
C4A H4A2 0.9700 . ?
C5A H5A1 0.9600 . ?
C5A H5A2 0.9600 . ?
C5A H5A3 0.9600 . ?
C4B C5B 1.40(2) . ?
C4B N2 1.55(2) . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C5B H5B1 0.9600 . ?
C5B H5B2 0.9600 . ?
C5B H5B3 0.9600 . ?
I1 Pb1 3.1900(9) 6_656 ?
I1 Pb1 3.1954(9) . ?
I2 Pb1 3.1461(12) 6_556 ?
I2 Pb1 3.2688(12) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?

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
N1 C1 C2 121.0(10) . 7_565 ?
N1 C1 C2 121.0(10) . . ?
C2 C1 C2 117.9(19) 7_565 . ?
C3 C2 C1 118.4(15) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
N2 C3 C2 123.1(15) . . ?
N2 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C5A C4A N2 113(2) . . ?
C5A C4A H4A1 108.9 . . ?
N2 C4A H4A1 108.9 . . ?
C5A C4A H4A2 108.9 . . ?
N2 C4A H4A2 108.9 . . ?
H4A1 C4A H4A2 107.8 . . ?
C4A C5A H5A1 109.5 . . ?
C4A C5A H5A2 109.5 . . ?
H5A1 C5A H5A2 109.5 . . ?
C4A C5A H5A3 109.5 . . ?
H5A1 C5A H5A3 109.5 . . ?
H5A2 C5A H5A3 109.5 . . ?
C5B C4B N2 112(3) . . ?
C5B C4B H4B1 109.3 . . ?
N2 C4B H4B1 109.3 . . ?
C5B C4B H4B2 109.3 . . ?
N2 C4B H4B2 109.3 . . ?
H4B1 C4B H4B2 108.0 . . ?
C4B C5B H5B1 109.9 . . ?
C4B C5B H5B2 109.2 . . ?
H5B1 C5B H5B2 109.5 . . ?
C4B C5B H5B3 109.3 . . ?
H5B1 C5B H5B3 109.5 . . ?
H5B2 C5B H5B3 109.5 . . ?
Pb1 I1 Pb1 75.73(2) 6_656 . ?
Pb1 I2 Pb1 75.29(3) 6_556 . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C3 N2 C3 119.3(16) . 7_565 ?
C3 N2 C4B 109(6) . . ?
C3 N2 C4B 130(5) 7_565 . ?
C3 N2 C4A 135(3) . . ?
C3 N2 C4A 106(3) 7_565 . ?
I2 Pb1 I1 93.26(2) 6_656 6_556 ?
I2 Pb1 I1 93.26(2) 6_656 4_455 ?
I1 Pb1 I1 86.62(4) 6_556 4_455 ?
I2 Pb1 I1 87.29(2) 6_656 . ?
I1 Pb1 I1 93.47(3) 6_556 . ?
I1 Pb1 I1 179.44(2) 4_455 . ?
I2 Pb1 I1 87.29(2) 6_656 7_565 ?
I1 Pb1 I1 179.44(2) 6_556 7_565 ?
I1 Pb1 I1 93.47(3) 4_455 7_565 ?
I1 Pb1 I1 86.43(4) . 7_565 ?
I2 Pb1 I2 178.03(3) 6_656 . ?
I1 Pb1 I2 85.31(2) 6_556 . ?
I1 Pb1 I2 85.31(2) 4_455 . ?
I1 Pb1 I2 94.14(2) . . ?
I1 Pb1 I2 94.14(2) 7_565 . ?

_refine_diff_density_max         3.533
_refine_diff_density_min         -2.710
_refine_diff_density_rms         0.541

_structure_special_details       
;
 This structure is part of a multi-temperature experiment.
;
_shelx_res_file                  
;
TITL 14 in Pnma
    14.res
    created by SHELXL-2016/6 at 22:09:24 on 09-Jan-2017
CELL 0.71073   7.8382  10.3922  18.2707  90.000  90.000  90.000
ZERR   4.00   0.0006   0.0007   0.0013   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC C  H  N  I  Pb
UNIT 28  44  8  12  4
OMIT 0 50
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 20
size 0.11 0.10 0.10
dang 2.45 n2 c5a n2 c5b
DFIX 1.55 N2 C4A N2 C4B
DFIX 1.40 C4A C5A C4B C5B
DELU 0.01  N2 C4A C5A C4B C5B
SIMU 0.01  N2 C4A C5A C4B C5B
TEMP 27.00
WGHT    0.138100    6.229400
FVAR       0.05823   0.73075
MOLE 1
C1    1    0.457922    0.250000    0.651842    10.50000    0.03981    0.03622 =
         0.06555    0.00000   -0.00341    0.00000
C2    1    0.529988    0.133543    0.626603    11.00000    0.09583    0.02705 =
         0.06258    0.00108   -0.00430    0.01202
AFIX  43
H2    2    0.488765    0.054629    0.642835    11.00000   -1.20000
AFIX   0
C3    1    0.658569    0.139578    0.578933    11.00000    0.06366    0.06189 =
         0.07012    0.00543    0.01455    0.02941
AFIX  43
H3    2    0.703781    0.063019    0.561087    11.00000   -1.20000
PART -1
AFIX   0
C4A   1    0.874323    0.287091    0.503509    20.50000    0.03405    0.13512 =
         0.05064    0.00112    0.01038    0.00315
AFIX  23
H4A1  2    0.854709    0.247941    0.456055    20.50000   -1.20000
H4A2  2    0.874753    0.379698    0.496874    20.50000   -1.20000
AFIX   0
C5A   1    1.034213    0.248354    0.529512    20.50000    0.03386    0.13279 =
         0.05257    0.00230    0.01366    0.00307
AFIX 137
H5A1  2    1.061772    0.296081    0.572918    20.50000   -1.50000
H5A2  2    1.119086    0.264277    0.492729    20.50000   -1.50000
H5A3  2    1.031465    0.158129    0.540728    20.50000   -1.50000
PART -2
AFIX   0
C4B   1    0.850306    0.222928    0.491654   -20.50000    0.03411    0.13500 =
         0.04889    0.00138    0.00745    0.00082
AFIX  23
H4B1  2    0.785681    0.200446    0.448221   -20.50000   -1.20000
H4B2  2    0.914882    0.300323    0.481013   -20.50000   -1.20000
AFIX   0
C5B   1    0.963296    0.122707    0.508476   -20.50000    0.03680    0.13447 =
         0.05328    0.00299    0.00708    0.00107
AFIX   3
H5B1  2    1.072225    0.138812    0.486270   -20.50000   -1.50000
H5B2  2    0.917814    0.043184    0.490196   -20.50000   -1.50000
H5B3  2    0.976594    0.117108    0.560611   -20.50000   -1.50000
PART 0
AFIX   0
I1    4    0.958265    0.039456    0.318482    11.00000    0.04603    0.03910 =
         0.07159    0.00852   -0.00015   -0.00163
I2    4    0.448578    0.250000    0.388946    10.50000    0.04035    0.04655 =
         0.04900    0.00000   -0.00181    0.00000
N1    3    0.334193    0.250000    0.702800    10.50000    0.05719    0.04480 =
         0.08888    0.00000    0.01246    0.00000
AFIX  93
H1A   2    0.297799    0.321584    0.720520    10.50000   -1.20000
H1B   2    0.291437    0.178416    0.717677    10.50000   -1.20000
AFIX   0
N2    3    0.725165    0.250000    0.555722    10.50000    0.03433    0.13590 =
         0.04699    0.00000    0.00431    0.00000
PB1   5    0.708923    0.250000    0.249181    10.50000    0.02249    0.03287 =
         0.05171    0.00000    0.00016    0.00000
HKLF 4




REM  14 in Pnma
REM R1 =  0.0666 for    1249 Fo > 4sig(Fo)  and  0.0708 for all    1393 data
REM     96 parameters refined using     60 restraints

END

WGHT      0.1391      6.5367

REM Highest difference peak  3.533,  deepest hole -2.710,  1-sigma level  0.541
Q1    1   0.7004  0.2500  0.2035  10.50000  0.05    3.53
Q2    1   0.7286  0.2500  0.2950  10.50000  0.05    3.38
Q3    1   0.4608  0.2500  0.3381  10.50000  0.05    2.40
Q4    1   0.4115  0.2500  0.4397  10.50000  0.05    1.65
Q5    1   0.3238  0.1536  0.3226  11.00000  0.05    1.59
Q6    1   0.9604  0.2500  0.3229  10.50000  0.05    1.55
Q7    1   0.9315  0.0721  0.3729  11.00000  0.05    1.49
Q8    1   0.5817  0.1417  0.3183  11.00000  0.05    1.25
Q9    1   0.7098  0.0896  0.2475  11.00000  0.05    1.21
Q10   1   0.7098  0.0478  0.2473  11.00000  0.05    1.21
Q11   1   0.9582  0.0845  0.2680  11.00000  0.05    1.11
Q12   1   0.8072  0.1358  0.3817  11.00000  0.05    1.04
Q13   1   0.8993  0.0313  0.2680  11.00000  0.05    1.00
Q14   1   0.9631  0.1816  0.2545  11.00000  0.05    0.98
Q15   1   0.8140  0.2500  0.4988  10.50000  0.05    0.93
Q16   1   1.0385  0.0243  0.2639  11.00000  0.05    0.87
Q17   1   1.2978  0.3361  0.4522  11.00000  0.05    0.86
Q18   1   1.0585  0.3374  0.6172  11.00000  0.05    0.83
Q19   1   1.0480  0.3204  0.6732  11.00000  0.05    0.83
Q20   1   1.1185  0.1364  0.3926  11.00000  0.05    0.82
;
_shelx_res_checksum              50977
####################################################################### 
# 
# 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_1-150K
_database_code_depnum_ccdc_archive 'CCDC 1523553'
_audit_update_record             
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.8023(9)
_cell_length_b                   10.3378(12)
_cell_length_c                   18.120(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1461.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.4635
_cell_measurement_theta_max      25.7823

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.232
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    17.849
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18875
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.842
_diffrn_reflns_theta_max         27.674
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1790
_reflns_number_gt                1620
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+11.6745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1790
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4530(11) 0.2500 0.6543(6) 0.023(2) Uani 1 2 d S T P . .
C2 C 0.5251(10) 0.1342(8) 0.6277(4) 0.0318(16) Uani 1 1 d . . . . .
H2 H 0.4821 0.0534 0.6443 0.038 Uiso 1 1 calc R U . . .
C3 C 0.6558(11) 0.1379(8) 0.5783(4) 0.0366(18) Uani 1 1 d . . . . .
H3 H 0.7015 0.0589 0.5601 0.044 Uiso 1 1 calc R U . . .
C4 C 0.8641(17) 0.2500 0.4990(7) 0.060(4) Uani 1 2 d S T P . .
H4A H 0.8519 0.1727 0.4672 0.072 Uiso 0.5 1 calc R U P . .
H4B H 0.8519 0.3273 0.4672 0.072 Uiso 0.5 1 calc R U P . .
C5 C 1.0311(14) 0.2500 0.5304(8) 0.056(4) Uani 1 2 d S T P . .
H5A H 1.0340 0.3094 0.5726 0.084 Uiso 0.5 1 calc R U P . .
H5B H 1.1144 0.2782 0.4933 0.084 Uiso 0.5 1 calc R U P . .
H5C H 1.0599 0.1625 0.5471 0.084 Uiso 0.5 1 calc R U P . .
I1 I 0.96060(5) 0.03819(5) 0.31926(3) 0.02777(15) Uani 1 1 d . . . . .
I2 I 0.44986(7) 0.2500 0.39019(3) 0.02297(16) Uani 1 2 d S T P . .
N1 N 0.3282(13) 0.2500 0.7053(5) 0.037(2) Uani 1 2 d S T P . .
H1A H 0.2895 0.1763 0.7229 0.045 Uiso 0.5 1 calc R U P . .
H1B H 0.2852 0.3237 0.7210 0.045 Uiso 0.5 1 calc R U P . .
N2 N 0.7222(12) 0.2500 0.5546(5) 0.037(2) Uani 1 2 d S T P . .
Pb1 Pb 0.71119(4) 0.2500 0.24937(2) 0.01696(13) Uani 1 2 d S T P . .

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
C1 0.020(5) 0.027(5) 0.022(5) 0.000 0.000(3) 0.000
C2 0.040(4) 0.025(3) 0.030(4) 0.003(3) 0.001(3) 0.003(3)
C3 0.043(4) 0.045(5) 0.022(3) -0.005(3) 0.000(3) 0.018(4)
C4 0.038(7) 0.123(14) 0.019(5) 0.000 0.007(5) 0.000
C5 0.024(6) 0.108(13) 0.036(7) 0.000 0.009(5) 0.000
I1 0.0246(3) 0.0268(3) 0.0319(3) 0.00266(18) 0.00000(17) -0.00149(16)
I2 0.0201(3) 0.0302(3) 0.0186(3) 0.000 -0.0004(2) 0.000
N1 0.038(5) 0.031(5) 0.043(6) 0.000 0.018(4) 0.000
N2 0.029(5) 0.066(7) 0.016(4) 0.000 0.003(3) 0.000
Pb1 0.01114(19) 0.02143(19) 0.01830(19) 0.000 0.00052(11) 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
C1 N1 1.342(13) . ?
C1 C2 1.407(9) . ?
C1 C2 1.407(9) 7_565 ?
C2 C3 1.357(11) . ?
C3 N2 1.340(10) . ?
C4 C5 1.422(18) . ?
C4 N2 1.497(14) . ?
I1 Pb1 3.1881(5) 6_656 ?
I1 Pb1 3.1914(5) . ?
I2 Pb1 3.1404(7) 6_556 ?
I2 Pb1 3.2663(7) . ?
N2 C3 1.340(10) 7_565 ?
Pb1 I2 3.1405(7) 6_656 ?
Pb1 I1 3.1881(5) 6_556 ?
Pb1 I1 3.1881(5) 4_455 ?
Pb1 I1 3.1914(5) 7_565 ?

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
N1 C1 C2 121.7(5) . . ?
N1 C1 C2 121.7(5) . 7_565 ?
C2 C1 C2 116.5(9) . 7_565 ?
C3 C2 C1 120.2(8) . . ?
N2 C3 C2 121.7(8) . . ?
C5 C4 N2 114.1(10) . . ?
Pb1 I1 Pb1 75.400(13) 6_656 . ?
Pb1 I2 Pb1 74.995(16) 6_556 . ?
C3 N2 C3 119.7(9) . 7_565 ?
C3 N2 C4 120.1(5) . . ?
C3 N2 C4 120.1(5) 7_565 . ?
I2 Pb1 I1 92.839(15) 6_656 6_556 ?
I2 Pb1 I1 92.839(15) 6_656 4_455 ?
I1 Pb1 I1 86.76(2) 6_556 4_455 ?
I2 Pb1 I1 87.594(14) 6_656 . ?
I1 Pb1 I1 93.299(17) 6_556 . ?
I1 Pb1 I1 179.560(13) 4_455 . ?
I2 Pb1 I1 87.595(14) 6_656 7_565 ?
I1 Pb1 I1 179.559(13) 6_556 7_565 ?
I1 Pb1 I1 93.299(17) 4_455 7_565 ?
I1 Pb1 I1 86.64(2) . 7_565 ?
I2 Pb1 I2 177.739(19) 6_656 . ?
I1 Pb1 I2 85.520(14) 6_556 . ?
I1 Pb1 I2 85.520(14) 4_455 . ?
I1 Pb1 I2 94.048(15) . . ?
I1 Pb1 I2 94.048(14) 7_565 . ?

_refine_diff_density_max         1.176
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.313

_structure_special_details       
;
 This structure is part of a multi-temperature experiment.
;
_shelx_res_file                  
;

    11.res created by SHELXL-2014/7

TITL 11 in Pnma
CELL 0.71073   7.8023  10.3378  18.1202  90.000  90.000  90.000
ZERR   13.00   0.0009   0.0012   0.0021   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC C  H  N  I  Pb
UNIT 13 13 13 13 13
L.S. 88
ACTA
BOND
FMAP 2
PLAN 20
TEMP -123.560
WGHT    0.049100   11.674500
FVAR       0.05625
MOLE 1
C1    1    0.452977    0.250000    0.654275    10.50000    0.02047    0.02735 =
         0.02159    0.00000   -0.00008    0.00000
C2    1    0.525086    0.134250    0.627665    11.00000    0.04035    0.02541 =
         0.02969    0.00256    0.00112    0.00255
AFIX  43
H2    2    0.482109    0.053351    0.644279    11.00000   -1.20000
AFIX   0
C3    1    0.655845    0.137924    0.578335    11.00000    0.04292    0.04504 =
         0.02189   -0.00477   -0.00003    0.01781
AFIX  43
H3    2    0.701529    0.058944    0.560132    11.00000   -1.20000
AFIX   0
C4    1    0.864079    0.250000    0.499012    10.50000    0.03793    0.12298 =
         0.01929    0.00000    0.00671    0.00000
AFIX  23
H4A   2    0.851902    0.172702    0.467188    10.50000   -1.20000
H4B   2    0.851903    0.327298    0.467188    10.50000   -1.20000
AFIX   0
C5    1    1.031082    0.250000    0.530438    10.50000    0.02386    0.10793 =
         0.03588    0.00000    0.00946    0.00000
AFIX 137
H5A   2    1.033996    0.309362    0.572586    10.50000   -1.50000
H5B   2    1.114449    0.278182    0.493317    10.50000   -1.50000
H5C   2    1.059896    0.162455    0.547068    10.50000   -1.50000
AFIX   0
I1    4    0.960595    0.038194    0.319265    11.00000    0.02458    0.02684 =
         0.03189    0.00266    0.00000   -0.00149
I2    4    0.449857    0.250000    0.390188    10.50000    0.02012    0.03016 =
         0.01864    0.00000   -0.00036    0.00000
N1    3    0.328240    0.250000    0.705264    10.50000    0.03819    0.03071 =
         0.04317    0.00000    0.01828    0.00000
AFIX  93
H1A   2    0.289457    0.176317    0.722942    10.50000   -1.20000
H1B   2    0.285226    0.323683    0.721022    10.50000   -1.20000
AFIX   0
N2    3    0.722236    0.250000    0.554620    10.50000    0.02881    0.06560 =
         0.01618    0.00000    0.00304    0.00000
PB1   5    0.711193    0.250000    0.249367    10.50000    0.01114    0.02143 =
         0.01830    0.00000    0.00052    0.00000
HKLF 4

REM  11 in Pnma
REM R1 =  0.0330 for    1620 Fo > 4sig(Fo)  and  0.0371 for all    1790 data
REM     71 parameters refined using      0 restraints

END

WGHT      0.0491     11.6668

REM Highest difference peak  1.176,  deepest hole -2.320,  1-sigma level  0.313
Q1    1   0.7048  0.2500  0.2107  10.50000  0.05    1.18
Q2    1   0.6053  0.2500  0.2501  10.50000  0.05    1.14
Q3    1   0.6053  0.2500  0.1889  10.50000  0.05    1.09
Q4    1   0.6956  0.1859  0.2505  11.00000  0.05    1.03
Q5    1   0.7130  0.2500  0.2865  10.50000  0.05    1.00
Q6    1   0.7982  0.2132  0.2486  11.00000  0.05    0.91
Q7    1   0.8393  0.1848  0.2484  11.00000  0.05    0.91
Q8    1   0.8311  0.2500  0.1817  10.50000  0.05    0.87
Q9    1   0.6095  0.2500  0.3110  10.50000  0.05    0.84
Q10   1   0.4898  0.2500  0.1823  10.50000  0.05    0.83
Q11   1   0.8293  0.0429  0.3196  11.00000  0.05    0.80
Q12   1   0.9566  0.1314  0.3595  11.00000  0.05    0.77
Q13   1   0.5199  0.2500  0.3262  10.50000  0.05    0.75
Q14   1   0.8319  0.2069  0.3105  11.00000  0.05    0.74
Q15   1   0.4894  0.2500  0.5318  10.50000  0.05    0.74
Q16   1   0.7183  0.1618  0.1975  11.00000  0.05    0.72
Q17   1   0.7037  0.0644  0.2490  11.00000  0.05    0.72
Q18   1   1.0192  0.1391  0.2507  11.00000  0.05    0.72
Q19   1   0.8532  0.0347  0.2567  11.00000  0.05    0.71
Q20   1   1.0522  0.1658  0.3383  11.00000  0.05    0.68
;
_shelx_res_checksum              57874
