 
data_1_a
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H24 I6 N4 Pb' 
_chemical_formula_weight          1144.90

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            13
_space_group_name_H-M_alt         'P 2/n'
_space_group_name_Hall            '-P 2yac'
 
_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, -z'
 'x-1/2, -y, z-1/2'
 
_cell_length_a                    9.8118(2)
_cell_length_b                    9.2671(2)
_cell_length_c                    12.4194(3)
_cell_angle_alpha                 90
_cell_angle_beta                  93.5610(10)
_cell_angle_gamma                 90
_cell_volume                      1127.08(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     9699
_cell_measurement_theta_min       2.73
_cell_measurement_theta_max       26.39
 
_exptl_crystal_description        irregular
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.374          
_exptl_crystal_F_000              1000
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.39
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     15.698
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.3867
_exptl_absorpt_correction_T_max   0.7454
_exptl_absorpt_process_details    
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'micro focus'
_diffrn_measurement_device_type   'Bruker D8 Venture Photon II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             10191
_diffrn_reflns_av_unetI/netI      0.0310
_diffrn_reflns_av_R_equivalents   0.0384
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.505
_diffrn_reflns_theta_max          26.389
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.950
_diffrn_measured_fraction_theta_full  0.945
_diffrn_reflns_Laue_measured_fraction_max    0.950
_diffrn_reflns_Laue_measured_fraction_full   0.945
_diffrn_reflns_point_group_measured_fraction_max   0.950
_diffrn_reflns_point_group_measured_fraction_full  0.945
_reflns_number_total              2203
_reflns_number_gt                 2095
_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 Apex3'
_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     ?
_computing_publication_material   ?
_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)+(0.0188P)²+0.4486P] 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          2203
_refine_ls_number_parameters      87
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0248
_refine_ls_R_factor_gt            0.0229
_refine_ls_wR_factor_ref          0.0488
_refine_ls_wR_factor_gt           0.0482
_refine_ls_goodness_of_fit_ref    1.151
_refine_ls_restrained_S_all       1.151
_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
Pb1 Pb 0.750000 0.28294(2) 0.750000 0.01415(8) Uani 1 2 d S T P . .
I1 I 0.74767(3) 0.25104(3) 0.49329(2) 0.01847(9) Uani 1 1 d . . . . .
I2 I 0.48867(3) 0.06107(3) 0.73236(2) 0.01579(9) Uani 1 1 d . . . . .
I3 I 0.96750(3) 0.54001(3) 0.72947(2) 0.01552(9) Uani 1 1 d . . . . .
N1 N 0.3802(4) 0.1997(4) 0.4713(3) 0.0172(8) Uani 1 1 d . . . . .
H1A H 0.401557 0.135883 0.525478 0.021 Uiso 1 1 calc R U . . .
H1B H 0.449862 0.199898 0.426241 0.021 Uiso 1 1 calc R U . . .
N2 N 0.1202(4) 0.3021(4) 0.5303(3) 0.0181(8) Uani 1 1 d . . . . .
H2A H 0.099365 0.366316 0.476359 0.022 Uiso 1 1 calc R U . . .
H2B H 0.050226 0.301957 0.575103 0.022 Uiso 1 1 calc R U . . .
C1 C 0.2522(4) 0.1526(5) 0.4107(4) 0.0166(10) Uani 1 1 d . . . . .
H1C H 0.263962 0.053612 0.382831 0.020 Uiso 1 1 calc R U . . .
H1D H 0.232496 0.217542 0.348370 0.020 Uiso 1 1 calc R U . . .
C2 C 0.1340(5) 0.1556(5) 0.4833(4) 0.0240(11) Uani 1 1 d . . . . .
H2C H 0.048610 0.129350 0.441188 0.029 Uiso 1 1 calc R U . . .
H2D H 0.149712 0.083975 0.541902 0.029 Uiso 1 1 calc R U . . .
C3 C 0.2473(4) 0.3490(5) 0.5915(4) 0.0163(10) Uani 1 1 d . . . . .
H3A H 0.267290 0.283496 0.653517 0.020 Uiso 1 1 calc R U . . .
H3B H 0.235430 0.447755 0.619814 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3652(5) 0.3465(5) 0.5176(4) 0.0204(10) Uani 1 1 d . . . . .
H4A H 0.347991 0.417250 0.458637 0.024 Uiso 1 1 calc R U . . .
H4B H 0.450738 0.374178 0.558915 0.024 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb1 I1 3.2005(3) 2_656 ?
Pb1 I1 3.2005(3) . ?
Pb1 I3 3.2190(3) . ?
Pb1 I3 3.2191(3) 2_656 ?
Pb1 I2 3.2833(3) 2_656 ?
Pb1 I2 3.2833(3) . ?
N1 C4 1.488(6) . ?
N1 C1 1.489(6) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C3 1.484(6) . ?
N2 C2 1.488(6) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C1 C2 1.512(6) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.521(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
I1 Pb1 I1 169.400(13) 2_656 . ?
I1 Pb1 I3 100.575(8) 2_656 . ?
I1 Pb1 I3 87.317(8) . . ?
I1 Pb1 I3 87.318(8) 2_656 2_656 ?
I1 Pb1 I3 100.575(8) . 2_656 ?
I3 Pb1 I3 84.524(12) . 2_656 ?
I1 Pb1 I2 85.322(8) 2_656 2_656 ?
I1 Pb1 I2 88.044(8) . 2_656 ?
I3 Pb1 I2 87.129(7) . 2_656 ?
I3 Pb1 I2 167.680(9) 2_656 2_656 ?
I1 Pb1 I2 88.044(8) 2_656 . ?
I1 Pb1 I2 85.323(8) . . ?
I3 Pb1 I2 167.681(9) . . ?
I3 Pb1 I2 87.129(7) 2_656 . ?
I2 Pb1 I2 102.458(12) 2_656 . ?
C4 N1 C1 111.2(3) . . ?
C4 N1 H1A 109.4 . . ?
C1 N1 H1A 109.4 . . ?
C4 N1 H1B 109.4 . . ?
C1 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
C3 N2 C2 112.0(4) . . ?
C3 N2 H2A 109.2 . . ?
C2 N2 H2A 109.2 . . ?
C3 N2 H2B 109.2 . . ?
C2 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
N1 C1 C2 110.3(4) . . ?
N1 C1 H1C 109.6 . . ?
C2 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
C2 C1 H1D 109.6 . . ?
H1C C1 H1D 108.1 . . ?
N2 C2 C1 110.0(4) . . ?
N2 C2 H2C 109.7 . . ?
C1 C2 H2C 109.7 . . ?
N2 C2 H2D 109.7 . . ?
C1 C2 H2D 109.7 . . ?
H2C C2 H2D 108.2 . . ?
N2 C3 C4 109.4(4) . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N1 C4 C3 110.2(4) . . ?
N1 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
 
_refine_diff_density_max    0.848
_refine_diff_density_min   -1.044
_refine_diff_density_rms    0.155



