# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_BB_1_105
_database_code_depnum_ccdc_archive 'CCDC 1940830'
loop_
_audit_author_name
_audit_author_address
'Naveen R. Venkatesan'
;University of California, Santa Barbara
United States of America
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_BB_1_105            
;
PROBLEM: Check Calcd Resid. Dens.  0.78A   From I2              4.05 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105            
;
PROBLEM: Check Calcd Resid. Dens.  1.69A   From C10            -5.47 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105_2          
;
PROBLEM: Check Calcd Resid. Dens.  0.35A   From I3             -5.47 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT315_BB_1_105            
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).        C15 Check
RESPONSE: Disorder model for methylammonium has fractional occupancy Ns
;
_vrf_PLAT342_BB_1_105            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.
RESPONSE: Due to disorder model
;
_vrf_PLAT971_BB_1_105_2          
;
PROBLEM: Check Calcd Resid. Dens.  0.54A   From I1              3.31 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_3          
;
PROBLEM: Check Calcd Resid. Dens.  0.12A   From I4              3.24 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_4          
;
PROBLEM: Check Calcd Resid. Dens.  0.91A   From Pb1             3.24 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_5          
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From I3              3.08 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_6          
;
PROBLEM: Check Calcd Resid. Dens.  0.64A   From I1              3.03 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_7          
;
PROBLEM: Check Calcd Resid. Dens.  0.82A   From Pb1             2.94 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_8          
;
PROBLEM: Check Calcd Resid. Dens.  0.89A   From I3              2.92 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_9          
;
PROBLEM: Check Calcd Resid. Dens.  0.43A   From I2              2.80 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_BB_1_105_10         
;
PROBLEM: Check Calcd Resid. Dens.  0.60A   From C3              2.75 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105_3          
;
PROBLEM: Check Calcd Resid. Dens.  0.61A   From I1             -3.45 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105_4          
;
PROBLEM: Check Calcd Resid. Dens.  1.39A   From C13            -3.22 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105_5          
;
PROBLEM: Check Calcd Resid. Dens.  0.73A   From I2             -2.93 eA-3
RESPONSE: Due to structure factor validation
;
_vrf_PLAT972_BB_1_105_6          
;
PROBLEM: Check Calcd Resid. Dens.  0.66A   From I2             -2.64 eA-3
RESPONSE: Due to structure factor validation
;
# Added during the CSD deposition process: Tuesday 16 July 2019 05:05 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         ?
_chemical_formula_sum            'C29 H38 I7 N3 Pb2'
_chemical_formula_weight         1731.30

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -2ac'

_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, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   8.7633(8)
_cell_length_b                   55.030(5)
_cell_length_c                   8.7081(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4199.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1830
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      26.05

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.738
_exptl_crystal_F_000             3072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    13.176
_shelx_estimated_absorpt_T_min   0.178
_shelx_estimated_absorpt_T_max   0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4908
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9269
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.480
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3551
_reflns_number_gt                2783
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+560.4957P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.62(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3551
_refine_ls_number_parameters     116
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.1471
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.083
_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 0.458(4) 0.3866(5) 0.641(4) 0.025(4) Uani 1 1 d D . . A 1
H1A H 0.4521 0.3978 0.5518 0.030 Uiso 1 1 calc R U . A 1
H1B H 0.3573 0.3866 0.6921 0.030 Uiso 1 1 calc R U . A 1
C2 C 0.495(4) 0.3609(4) 0.584(3) 0.025(4) Uani 1 1 d D . . A 1
H2A H 0.4137 0.3551 0.5137 0.030 Uiso 1 1 calc R U . A 1
H2B H 0.5931 0.3608 0.5280 0.030 Uiso 1 1 calc R U . A 1
C3 C 0.504(3) 0.3446(5) 0.726(3) 0.025(4) Uani 1 1 d D . . A 1
C4 C 0.381(4) 0.3400(7) 0.826(3) 0.034(5) Uani 1 1 d D . . A 1
H4 H 0.2887 0.3485 0.8094 0.040 Uiso 1 1 calc R U . A 1
C5 C 0.387(3) 0.3236(6) 0.949(4) 0.034(5) Uani 1 1 d D . . A 1
H5 H 0.2965 0.3195 1.0035 0.040 Uiso 1 1 calc R U . A 1
C6 C 0.527(3) 0.3130(6) 0.993(3) 0.027(6) Uani 1 1 d D . . A 1
C7 C 0.654(4) 0.3183(7) 0.900(4) 0.034(5) Uani 1 1 d D . . A 1
H7 H 0.7501 0.3113 0.9248 0.040 Uiso 1 1 calc R U . A 1
C8 C 0.642(3) 0.3336(6) 0.771(4) 0.034(5) Uani 1 1 d D . . A 1
H8 H 0.7312 0.3367 0.7123 0.040 Uiso 1 1 calc R U . A 1
C9 C 0.541(5) 0.2965(6) 1.115(3) 0.027(6) Uani 1 1 d D . . A 1
C10 C 0.446(5) 0.2980(8) 1.245(4) 0.048(6) Uani 1 1 d D . . A 1
H10 H 0.3717 0.3105 1.2453 0.058 Uiso 1 1 calc R U . A 1
C11 C 0.451(5) 0.2829(6) 1.376(5) 0.048(6) Uani 1 1 d D . . A 1
H11 H 0.3926 0.2862 1.4652 0.058 Uiso 1 1 calc R U . A 1
C12 C 0.548(4) 0.2627(6) 1.364(5) 0.049(12) Uani 1 1 d D . . A 1
H12 H 0.5493 0.2511 1.4454 0.058 Uiso 1 1 calc R U . A 1
C13 C 0.643(5) 0.2591(8) 1.236(4) 0.048(6) Uani 1 1 d D . . A 1
H13 H 0.7120 0.2457 1.2325 0.058 Uiso 1 1 calc R U . A 1
C14 C 0.633(5) 0.2757(6) 1.115(4) 0.048(6) Uani 1 1 d D . . A 1
H14 H 0.6933 0.2726 1.0259 0.058 Uiso 1 1 calc R U . A 1
C15 C 0.5000 0.5000 0.700(8) 0.060(19) Uiso 1 2 d DS . P B 1
I1 I 0.6957(3) 0.44284(5) 0.4805(3) 0.0170(3) Uani 1 1 d . . . C 1
I2 I 0.1927(2) 0.44233(5) 0.3678(3) 0.0170(3) Uani 1 1 d . . . C 1
I3 I 0.5174(2) 0.38396(3) 0.1586(4) 0.0173(3) Uani 1 1 d . . . C 1
I4 I 0.5000 0.5000 0.1749(6) 0.0173(3) Uani 1 2 d S T P C 1
N1 N 0.571(3) 0.3954(5) 0.746(3) 0.025(4) Uani 1 1 d D . . A 1
H1C H 0.5401 0.3924 0.8439 0.037 Uiso 1 1 calc R U . A 1
H1D H 0.5836 0.4117 0.7325 0.037 Uiso 1 1 calc R U . A 1
H1E H 0.6611 0.3876 0.7281 0.037 Uiso 1 1 calc R U . A 1
N2 N 0.596(7) 0.5080(11) 0.579(7) 0.031(15) Uiso 0.5 1 d D . P B 1
H2C H 0.5739 0.4996 0.4914 0.047 Uiso 0.5 1 calc R U P B 1
H2D H 0.6957 0.5054 0.6044 0.047 Uiso 0.5 1 calc R U P B 1
H2E H 0.5814 0.5242 0.5620 0.047 Uiso 0.5 1 calc R U P B 1
Pb1 Pb 0.49893(15) 0.44073(2) 0.1724(3) 0.0107(2) Uani 1 1 d . . . C 1


_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 1.43(4) . ?
C1 C2 1.53(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.53(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.405(13) . ?
C3 C8 1.411(13) . ?
C4 C5 1.404(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(12) . ?
C5 H5 0.9500 . ?
C6 C9 1.404(12) . ?
C6 C7 1.405(12) . ?
C7 C8 1.408(13) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.404(13) . ?
C9 C10 1.405(13) . ?
C10 C11 1.405(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.406(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.406(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(13) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 N2 1.42(4) . ?
C15 N2 1.42(4) 2_665 ?
I1 Pb1 3.158(3) 8_645 ?
I1 Pb1 3.191(4) . ?
I2 Pb1 3.141(4) 8_545 ?
I2 Pb1 3.178(3) . ?
I3 Pb1 3.1306(19) . ?
I4 Pb1 3.2618(9) . ?
I4 Pb1 3.2619(9) 2_665 ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
N2 H2E 0.9100 . ?
Pb1 I2 3.141(4) 8_544 ?
Pb1 I1 3.158(3) 8_644 ?

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 111.9(19) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C1 107(2) . . ?
C3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
C3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C4 C3 C8 114(3) . . ?
C4 C3 C2 125(2) . . ?
C8 C3 C2 121(2) . . ?
C5 C4 C3 124(3) . . ?
C5 C4 H4 117.8 . . ?
C3 C4 H4 117.8 . . ?
C4 C5 C6 120(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C9 C6 C7 120(3) . . ?
C9 C6 C5 123(3) . . ?
C7 C6 C5 117(3) . . ?
C6 C7 C8 121(3) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 123(3) . . ?
C7 C8 H8 118.5 . . ?
C3 C8 H8 118.5 . . ?
C6 C9 C14 125(3) . . ?
C6 C9 C10 122(3) . . ?
C14 C9 C10 113(3) . . ?
C9 C10 C11 127(4) . . ?
C9 C10 H10 116.5 . . ?
C11 C10 H10 116.5 . . ?
C10 C11 C12 115(4) . . ?
C10 C11 H11 122.3 . . ?
C12 C11 H11 122.3 . . ?
C11 C12 C13 122(4) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C14 C13 C12 118(4) . . ?
C14 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
C13 C14 C9 124(4) . . ?
C13 C14 H14 117.8 . . ?
C9 C14 H14 117.8 . . ?
N2 C15 N2 84(6) . 2_665 ?
Pb1 I1 Pb1 154.38(12) 8_645 . ?
Pb1 I2 Pb1 154.50(12) 8_545 . ?
Pb1 I4 Pb1 179.25(17) . 2_665 ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C15 N2 H2C 109.5 . . ?
C15 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C15 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
I3 Pb1 I2 91.32(8) . 8_544 ?
I3 Pb1 I1 88.42(7) . 8_644 ?
I2 Pb1 I1 90.28(12) 8_544 8_644 ?
I3 Pb1 I2 95.27(7) . . ?
I2 Pb1 I2 89.99(4) 8_544 . ?
I1 Pb1 I2 176.29(6) 8_644 . ?
I3 Pb1 I1 92.33(7) . . ?
I2 Pb1 I1 176.29(5) 8_544 . ?
I1 Pb1 I1 89.18(4) 8_644 . ?
I2 Pb1 I1 90.31(12) . . ?
I3 Pb1 I4 176.38(8) . . ?
I2 Pb1 I4 88.80(9) 8_544 . ?
I1 Pb1 I4 87.96(7) 8_644 . ?
I2 Pb1 I4 88.35(7) . . ?
I1 Pb1 I4 87.51(9) . . ?

_refine_diff_density_max         4.473
_refine_diff_density_min         -5.449
_refine_diff_density_rms         0.423

####################################################################### 
# 
# 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_check
_database_code_depnum_ccdc_archive 'CCDC 1940831'
loop_
_audit_author_name
_audit_author_address
'Naveen R. Venkatesan'
;University of California, Santa Barbara
United States of America
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_check               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03067 Ang.
RESPONSE: Due to disorder model
;
_vrf_PLAT915_check               
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         43 %
RESPONSE: Due to structure factor validation
;
_vrf_PLAT934_check               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check
RESPONSE: Due to structure factor validation
;
_vrf_PLAT971_check               
;
PROBLEM: Check Calcd Resid. Dens.  0.31A   From Pb1             3.04 eA-3
RESPONSE: Due to structure factor validation
;
# Added during the CSD deposition process: Tuesday 16 July 2019 05:05 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         ?
_chemical_formula_sum            'C28 H28 I4 N2 Pb'
_chemical_formula_weight         1107.31

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

_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, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   42.920(6)
_cell_length_b                   8.7431(11)
_cell_length_c                   8.6629(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3250.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    873
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      28.6

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    9.007
_shelx_estimated_absorpt_T_min   0.345
_shelx_estimated_absorpt_T_max   0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker kappa Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10433
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.898
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2500
_reflns_number_gt                1780
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.4397P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2500
_refine_ls_number_parameters     123
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.436
_refine_ls_restrained_S_all      1.427
_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
C4 C 0.3670(5) 0.134(3) 0.594(2) 0.032(4) Uani 1 1 d D . . . .
H4 H 0.3767 0.0411 0.5720 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3464(5) 0.140(2) 0.720(2) 0.025(4) Uani 1 1 d . . . . .
H5 H 0.3423 0.0514 0.7754 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3324(6) 0.272(3) 0.761(3) 0.034(5) Uani 1 1 d . . . . .
C7 C 0.3379(5) 0.406(2) 0.669(2) 0.025(4) Uani 1 1 d . . . . .
H7 H 0.3279 0.4977 0.6926 0.030 Uiso 1 1 calc R U . . .
C8 C 0.3587(5) 0.400(3) 0.541(3) 0.032(4) Uani 1 1 d D . . . .
H8 H 0.3627 0.4872 0.4823 0.038 Uiso 1 1 calc R U . . .
C9 C 0.3095(4) 0.285(3) 0.887(2) 0.021(4) Uani 1 1 d D . . . .
C10 C 0.3152(5) 0.197(3) 1.022(2) 0.042(6) Uani 1 1 d D . . . .
H10 H 0.3326 0.1337 1.0272 0.051 Uiso 1 1 calc R U . . .
C11 C 0.2943(5) 0.206(3) 1.148(2) 0.065(7) Uani 1 1 d D . . . .
H11 H 0.2985 0.1522 1.2388 0.078 Uiso 1 1 calc R U . . .
C12 C 0.2669(4) 0.296(2) 1.137(2) 0.034(5) Uani 1 1 d D . . . .
H12 H 0.2522 0.2937 1.2161 0.041 Uiso 1 1 calc R U . . .
C13 C 0.2620(5) 0.390(3) 1.006(2) 0.065(7) Uani 1 1 d D . . . .
H13 H 0.2448 0.4546 1.0012 0.078 Uiso 1 1 calc R U . . .
C14 C 0.2834(5) 0.384(2) 0.881(2) 0.042(6) Uani 1 1 d D . . . .
H14 H 0.2803 0.4451 0.7946 0.051 Uiso 1 1 calc R U . . .
I1 I 0.5000 0.9414(3) 0.1268(3) 0.0152(10) Uani 1 2 d S T P . .
I2 I 0.42531(3) 0.7545(5) 0.4347(6) 0.0278(4) Uani 1 1 d . . . . .
I3 I 0.5000 0.4399(4) 0.2479(3) 0.0162(10) Uani 1 2 d S T P . .
Pb1 Pb 0.5000 0.7453(3) 0.4417(5) 0.0116(2) Uani 1 2 d S T P . .
N1 N 0.4376(6) 0.334(2) 0.515(2) 0.034(7) Uani 1 1 d . . . . .
H1A H 0.4338 0.4271 0.4780 0.051 Uiso 1 1 calc R U . . .
H1B H 0.4579 0.3246 0.5352 0.051 Uiso 1 1 calc R U . . .
H1C H 0.4267 0.3192 0.6007 0.051 Uiso 1 1 calc R U . . .
C1 C 0.4285(5) 0.219(3) 0.399(3) 0.036(5) Uani 1 1 d D . . . .
H1D H 0.4311 0.1162 0.4391 0.044 Uiso 1 1 calc R U . . .
H1E H 0.4410 0.2292 0.3059 0.044 Uiso 1 1 calc R U . . .
C3 C 0.3735(5) 0.258(3) 0.503(2) 0.021(4) Uani 1 1 d . . . . .
C2 C 0.3947(5) 0.251(3) 0.365(3) 0.036(5) Uani 1 1 d D . . . .
H2A H 0.3934 0.3482 0.3110 0.044 Uiso 1 1 calc R U . . .
H2B H 0.3870 0.1728 0.2958 0.044 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
C4 C3 1.38(3) . ?
C4 C5 1.40(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.35(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.44(3) . ?
C6 C9 1.48(3) . ?
C7 C8 1.43(3) . ?
C7 H7 0.9300 . ?
C8 C3 1.43(3) . ?
C8 H8 0.9300 . ?
C9 C14 1.416(12) . ?
C9 C10 1.418(12) . ?
C10 C11 1.419(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.418(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.420(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.420(12) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
I1 Pb1 3.174(5) 2_674 ?
I1 Pb1 3.222(5) . ?
I2 Pb1 3.2071(13) . ?
I3 Pb1 3.107(5) 2_664 ?
I3 Pb1 3.154(5) . ?
Pb1 I3 3.107(5) 2_665 ?
Pb1 I1 3.174(5) 2_675 ?
Pb1 I2 3.2070(13) 4_655 ?
N1 C1 1.47(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C2 1.509(11) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C3 C2 1.50(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
C3 C4 C5 123(2) . . ?
C3 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C6 C5 C4 121(2) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 119(2) . . ?
C5 C6 C9 124(2) . . ?
C7 C6 C9 117(2) . . ?
C8 C7 C6 120(2) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C3 119(2) . . ?
C7 C8 H8 120.3 . . ?
C3 C8 H8 120.3 . . ?
C14 C9 C10 120.0(6) . . ?
C14 C9 C6 122.9(16) . . ?
C10 C9 C6 117.0(16) . . ?
C9 C10 C11 119.7(6) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 120.1(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.9(6) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.6(6) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C9 C14 C13 120.3(6) . . ?
C9 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
Pb1 I1 Pb1 152.48(16) 2_674 . ?
Pb1 I3 Pb1 153.57(17) 2_664 . ?
I3 Pb1 I3 90.78(8) 2_665 . ?
I3 Pb1 I1 91.06(17) 2_665 2_675 ?
I3 Pb1 I1 178.2(2) . 2_675 ?
I3 Pb1 I2 91.68(7) 2_665 4_655 ?
I3 Pb1 I2 90.65(7) . 4_655 ?
I1 Pb1 I2 89.30(7) 2_675 4_655 ?
I3 Pb1 I2 91.68(7) 2_665 . ?
I3 Pb1 I2 90.65(7) . . ?
I1 Pb1 I2 89.30(7) 2_675 . ?
I2 Pb1 I2 176.38(13) 4_655 . ?
I3 Pb1 I1 179.25(17) 2_665 . ?
I3 Pb1 I1 89.98(16) . . ?
I1 Pb1 I1 88.19(8) 2_675 . ?
I2 Pb1 I1 88.31(7) 4_655 . ?
I2 Pb1 I1 88.31(7) . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 104.9(19) . . ?
N1 C1 H1D 110.8 . . ?
C2 C1 H1D 110.8 . . ?
N1 C1 H1E 110.8 . . ?
C2 C1 H1E 110.8 . . ?
H1D C1 H1E 108.8 . . ?
C4 C3 C8 118(2) . . ?
C4 C3 C2 123.3(19) . . ?
C8 C3 C2 119.0(18) . . ?
C3 C2 C1 116.1(18) . . ?
C3 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
C3 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?

_refine_diff_density_max         2.612
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.315

