# Electronic Supplementary Material (ESI) for ChemComm.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1957895'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2019-11-13 deposited with the CCDC.	2019-11-25 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            'C36 H32 I14 N4'
_chemical_formula_weight         2297.25

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.3325(2)
_cell_length_b                   12.4358(3)
_cell_length_c                   21.5144(5)
_cell_angle_alpha                95.149(2)
_cell_angle_beta                 99.946(2)
_cell_angle_gamma                98.812(2)
_cell_volume                     2671.51(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    15189
_cell_measurement_theta_min      4.4000
_cell_measurement_theta_max      28.8780

_exptl_crystal_description       prismatic
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.856
_exptl_crystal_F_000             2036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    8.140
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.61201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.794
_oxdiff_exptl_absorpt_empirical_full_max 1.400
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_diffrn_ambient_temperature      100
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            42411
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         4.121
_diffrn_reflns_theta_max         29.495
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measured_fraction_theta_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_point_group_measured_fraction_full 0.943
_reflns_number_total             11976
_reflns_number_gt                9140
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
non-merohedral twinning
;
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7356 29546 17332 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2644 31103 17332 nmt 0.9260 0.2404 0.2378 -0.0007 -1.0006 0.0000 0.3254
0.0335 -0.9537
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 179.9864° 
 around [0.99 -0.00 0.17] (reciprocal) or [0.98 0.14 0.12] (direct)
;

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+136.8526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11976
_refine_ls_number_parameters     569
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0865
_refine_ls_wR_factor_ref         0.1772
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.006
_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
I1 I 0.06626(11) 0.57884(9) 0.08101(5) 0.0350(2) Uani 1 1 d . . . . .
I2 I 0.01136(8) 0.68757(7) 0.18983(4) 0.02216(19) Uani 1 1 d . . . . .
I3 I -0.02970(9) 0.80551(8) 0.31845(4) 0.0251(2) Uani 1 1 d . . . . .
I5 I -0.61308(11) 0.72810(12) 0.23945(6) 0.0513(4) Uani 1 1 d . . . . .
I4 I -0.33536(10) 0.77088(9) 0.27998(5) 0.0320(2) Uani 1 1 d . . . . .
C1 C 0.3287(19) 0.6838(15) 0.4783(8) 0.044(4) Uani 1 1 d . . . . .
H1A H 0.3010 0.6866 0.5192 0.053 Uiso 1 1 calc R U . . .
H1B H 0.4090 0.6516 0.4821 0.053 Uiso 1 1 calc R U . . .
N1 N 0.2204(14) 0.6146(11) 0.4288(5) 0.034(3) Uani 1 1 d . . . . .
C2 C 0.244(2) 0.5878(16) 0.3705(7) 0.048(5) Uani 1 1 d . . . . .
H2 H 0.3298 0.6060 0.3629 0.058 Uiso 1 1 calc R U . . .
C3 C 0.1465(18) 0.5354(15) 0.3224(8) 0.043(4) Uani 1 1 d . . . . .
H3 H 0.1650 0.5184 0.2822 0.051 Uiso 1 1 calc R U . . .
C4 C 0.0173(18) 0.5070(12) 0.3341(7) 0.034(4) Uani 1 1 d . . . . .
C5 C -0.0013(19) 0.5327(12) 0.3963(8) 0.039(4) Uani 1 1 d . . . . .
H5 H -0.0853 0.5143 0.4064 0.047 Uiso 1 1 calc R U . . .
C6 C 0.102(2) 0.5837(14) 0.4417(8) 0.044(5) Uani 1 1 d . . . . .
H6 H 0.0884 0.5974 0.4831 0.053 Uiso 1 1 calc R U . . .
C7 C -0.0945(18) 0.4643(12) 0.2808(7) 0.034(4) Uani 1 1 d . . . . .
C8 C -0.082(2) 0.4003(16) 0.2279(9) 0.055(5) Uani 1 1 d . . . . .
H8 H -0.0021 0.3749 0.2273 0.066 Uiso 1 1 calc R U . . .
C9 C -0.181(3) 0.3724(13) 0.1763(8) 0.055(6) Uani 1 1 d . . . . .
H9 H -0.1675 0.3301 0.1408 0.066 Uiso 1 1 calc R U . . .
N2 N -0.2999(16) 0.4065(11) 0.1766(7) 0.043(4) Uani 1 1 d . . . . .
C10 C -0.3181(18) 0.4667(16) 0.2281(8) 0.050(5) Uani 1 1 d . . . . .
H10 H -0.3996 0.4898 0.2280 0.060 Uiso 1 1 calc R U . . .
C11 C -0.2176(16) 0.4956(14) 0.2818(8) 0.040(4) Uani 1 1 d . . . . .
H11 H -0.2326 0.5353 0.3178 0.048 Uiso 1 1 calc R U . . .
C12 C -0.4049(19) 0.3867(16) 0.1176(8) 0.056(6) Uani 1 1 d . . . . .
H12A H -0.4915 0.3632 0.1282 0.067 Uiso 1 1 calc R U . . .
H12B H -0.3871 0.3291 0.0884 0.067 Uiso 1 1 calc R U . . .
C13 C -0.4054(16) 0.4914(14) 0.0863(7) 0.038(4) Uani 1 1 d . . . . .
C14 C -0.3081(15) 0.5183(14) 0.0495(8) 0.033(3) Uani 1 1 d . . . . .
H14 H -0.2523 0.4693 0.0408 0.040 Uiso 1 1 calc R U . . .
C15 C -0.2968(16) 0.6180(13) 0.0267(7) 0.034(3) Uani 1 1 d . . . . .
H15 H -0.2376 0.6343 -0.0005 0.040 Uiso 1 1 calc R U . . .
C16 C -0.3728(15) 0.6955(15) 0.0438(7) 0.037(4) Uani 1 1 d . . . . .
C17 C -0.4709(14) 0.6663(17) 0.0794(7) 0.043(5) Uani 1 1 d . . . . .
H17 H -0.5276 0.7149 0.0877 0.051 Uiso 1 1 calc R U . . .
C18 C -0.4842(17) 0.5652(18) 0.1024(7) 0.047(5) Uani 1 1 d . . . . .
H18 H -0.5456 0.5475 0.1284 0.057 Uiso 1 1 calc R U . . .
C19 C -0.3462(18) 0.8083(14) 0.0258(7) 0.042(4) Uani 1 1 d . . . . .
H19A H -0.4244 0.8427 0.0256 0.051 Uiso 1 1 calc R U . . .
H19B H -0.3247 0.8060 -0.0164 0.051 Uiso 1 1 calc R U . . .
N3 N -0.2279(15) 0.8740(10) 0.0749(6) 0.036(3) Uani 1 1 d . . . . .
C20 C -0.1039(19) 0.8916(12) 0.0628(7) 0.037(4) Uani 1 1 d . . . . .
H20 H -0.0906 0.8686 0.0224 0.044 Uiso 1 1 calc R U . . .
C21 C 0.0016(19) 0.9413(12) 0.1068(7) 0.037(4) Uani 1 1 d . . . . .
H21 H 0.0867 0.9517 0.0973 0.044 Uiso 1 1 calc R U . . .
C22 C -0.0185(17) 0.9773(11) 0.1678(7) 0.030(3) Uani 1 1 d . . . . .
C23 C -0.1497(18) 0.9615(13) 0.1786(7) 0.038(4) Uani 1 1 d . . . . .
H23 H -0.1665 0.9871 0.2179 0.046 Uiso 1 1 calc R U . . .
C24 C -0.2521(17) 0.9093(14) 0.1327(7) 0.035(4) Uani 1 1 d . . . . .
H24 H -0.3385 0.8976 0.1406 0.042 Uiso 1 1 calc R U . . .
C25 C 0.0972(15) 1.0229(11) 0.2204(6) 0.025(3) Uani 1 1 d . . . . .
C26 C 0.2137(16) 0.9832(14) 0.2239(7) 0.037(4) Uani 1 1 d . . . . .
H26 H 0.2265 0.9350 0.1908 0.044 Uiso 1 1 calc R U . . .
C27 C 0.3130(17) 1.0157(15) 0.2774(8) 0.043(4) Uani 1 1 d . . . . .
H27 H 0.3928 0.9890 0.2798 0.052 Uiso 1 1 calc R U . . .
N4 N 0.2964(19) 1.0849(12) 0.3260(7) 0.055(5) Uani 1 1 d . . . . .
C28 C 0.182(3) 1.1287(13) 0.3194(8) 0.053(6) Uani 1 1 d . . . . .
H28 H 0.1707 1.1803 0.3513 0.064 Uiso 1 1 calc R U . . .
C29 C 0.085(2) 1.0986(13) 0.2681(8) 0.046(5) Uani 1 1 d . . . . .
H29 H 0.0086 1.1299 0.2648 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4008(19) 1.1047(16) 0.3855(8) 0.052(5) Uani 1 1 d . . . . .
H30A H 0.4887 1.1239 0.3754 0.062 Uiso 1 1 calc R U . . .
H30B H 0.3855 1.1646 0.4140 0.062 Uiso 1 1 calc R U . . .
C31 C 0.3922(16) 1.0022(15) 0.4164(7) 0.041(4) Uani 1 1 d . . . . .
C32 C 0.4838(14) 0.9308(19) 0.4133(8) 0.055(6) Uani 1 1 d . . . . .
H32 H 0.5585 0.9527 0.3959 0.066 Uiso 1 1 calc R U . . .
C33 C 0.4690(17) 0.8326(14) 0.4343(8) 0.037(4) Uani 1 1 d . U . . .
H33 H 0.5327 0.7879 0.4316 0.044 Uiso 1 1 calc R U . . .
C34 C 0.3569(14) 0.7974(14) 0.4603(7) 0.033(4) Uani 1 1 d . . . . .
C35 C 0.2638(14) 0.8678(12) 0.4657(7) 0.026(3) Uani 1 1 d . . . . .
H35 H 0.1896 0.8449 0.4833 0.032 Uiso 1 1 calc R U . . .
C36 C 0.2809(13) 0.9688(12) 0.4455(6) 0.027(3) Uani 1 1 d . . . . .
H36 H 0.2205 1.0156 0.4506 0.032 Uiso 1 1 calc R U . . .
I11 I 0.4637(3) 0.3878(2) 0.34831(17) 0.0538(7) Uani 0.6260(16) 1 d . . P . .
I12 I 0.6532(2) 0.55443(19) 0.43793(10) 0.0581(7) Uani 0.6260(16) 1 d . . P . .
I13 I 0.8572(3) 0.7206(2) 0.51717(11) 0.0712(8) Uani 0.6260(16) 1 d . . P . .
I21 I 0.37110(18) 0.86027(13) 0.75704(9) 0.0393(5) Uani 0.6260(16) 1 d . . P .
.
I22 I 0.1846(2) 0.78654(17) 0.63436(10) 0.0401(4) Uani 0.6260(16) 1 d . . P . .
I23 I 0.5444(2) 0.94816(16) 0.87804(9) 0.0469(5) Uani 0.6260(16) 1 d . . P . .
I31 I -0.2367(3) 0.1474(2) 0.01075(18) 0.0537(8) Uani 0.6260(16) 1 d . . P . .
I32 I 0.0276(3) 0.23762(14) 0.09567(11) 0.0618(7) Uani 0.6260(16) 1 d . . P . .
I33 I 0.2658(3) 0.32859(16) 0.18865(13) 0.0630(7) Uani 0.6260(16) 1 d . . P . .
I41 I 1.6298(3) 1.0275(2) 0.92908(15) 0.0357(7) Uani 0.3740(16) 1 d . . P . .
I42 I 1.4526(3) 0.8825(2) 0.82612(18) 0.0427(8) Uani 0.3740(16) 1 d . . P . .
I43 I 1.8238(4) 1.1695(4) 1.02885(19) 0.0346(9) Uani 0.3740(16) 1 d . . P . .
I51 I 0.9995(4) 0.7539(2) 0.58115(18) 0.0493(9) Uani 0.3740(16) 1 d . . P . .
I52 I 1.2439(4) 0.8349(3) 0.6719(2) 0.0523(9) Uani 0.3740(16) 1 d . . P . .
I53 I 0.7451(3) 0.6592(3) 0.4942(2) 0.0549(10) Uani 0.3740(16) 1 d . . P . .
I61 I 0.3406(3) 0.3482(2) 0.25004(13) 0.0291(6) Uani 0.3740(16) 1 d . . P . .
I62 I 0.1682(3) 0.2611(2) 0.12788(13) 0.0334(7) Uani 0.3740(16) 1 d . . P . .
I63 I 0.5048(4) 0.4375(4) 0.37299(17) 0.0366(8) Uani 0.3740(16) 1 d . . P . .


_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
I1 I2 2.7850(14) . ?
I2 I3 3.1394(13) . ?
I3 I4 3.0760(13) . ?
I5 I4 2.8040(15) . ?
C1 C34 1.50(2) . ?
C1 N1 1.50(2) . ?
N1 C6 1.31(2) . ?
N1 C2 1.340(19) . ?
C2 C3 1.35(3) . ?
C3 C4 1.40(2) . ?
C4 C7 1.48(2) . ?
C4 C5 1.40(2) . ?
C5 C6 1.35(3) . ?
C7 C8 1.37(2) . ?
C7 C11 1.39(2) . ?
C8 C9 1.35(3) . ?
C9 N2 1.36(3) . ?
N2 C10 1.34(2) . ?
N2 C12 1.49(2) . ?
C10 C11 1.39(2) . ?
C12 C13 1.52(3) . ?
C13 C18 1.38(3) . ?
C13 C14 1.40(2) . ?
C14 C15 1.37(2) . ?
C15 C16 1.40(2) . ?
C16 C17 1.40(2) . ?
C16 C19 1.49(2) . ?
C17 C18 1.39(3) . ?
C19 N3 1.54(2) . ?
N3 C20 1.34(2) . ?
N3 C24 1.357(19) . ?
C20 C21 1.34(2) . ?
C21 C22 1.407(19) . ?
C22 C23 1.40(2) . ?
C22 C25 1.50(2) . ?
C23 C24 1.35(2) . ?
C25 C26 1.36(2) . ?
C25 C29 1.36(2) . ?
C26 C27 1.39(2) . ?
C27 N4 1.34(2) . ?
N4 C28 1.37(3) . ?
N4 C30 1.50(2) . ?
C28 C29 1.34(3) . ?
C30 C31 1.49(3) . ?
C31 C32 1.40(3) . ?
C31 C36 1.43(2) . ?
C32 C33 1.34(3) . ?
C33 C34 1.40(2) . ?
C34 C35 1.408(19) . ?
C35 C36 1.36(2) . ?
I11 I63 0.792(4) . ?
I11 I61 2.241(5) . ?
I11 I12 2.929(4) . ?
I12 I53 1.733(5) . ?
I12 I63 2.152(5) . ?
I12 I13 2.900(4) . ?
I13 I53 1.278(5) . ?
I13 I51 1.800(5) . ?
I21 I42 1.555(4) 1_455 ?
I21 I52 2.029(5) 1_455 ?
I21 I23 2.908(3) . ?
I21 I22 2.965(3) . ?
I22 I52 1.010(4) 1_455 ?
I22 I51 2.013(5) 1_455 ?
I23 I42 1.431(4) 1_455 ?
I23 I41 1.471(4) 1_455 ?
I31 I43 0.680(4) 1_344 ?
I31 I41 2.297(5) 1_344 ?
I31 I32 3.004(4) . ?
I32 I62 1.470(4) . ?
I32 I43 2.325(5) 1_344 ?
I32 I33 2.894(4) . ?
I33 I61 1.391(4) . ?
I33 I62 1.587(4) . ?
I41 I23 1.471(4) 1_655 ?
I41 I31 2.297(5) 1_766 ?
I41 I42 2.895(5) . ?
I41 I43 2.914(5) . ?
I42 I23 1.431(4) 1_655 ?
I42 I21 1.555(4) 1_655 ?
I43 I31 0.680(4) 1_766 ?
I43 I32 2.325(5) 1_766 ?
I51 I22 2.013(5) 1_655 ?
I51 I52 2.893(6) . ?
I51 I53 2.959(6) . ?
I52 I22 1.010(4) 1_655 ?
I52 I21 2.029(5) 1_655 ?
I61 I63 2.907(5) . ?
I61 I62 2.922(4) . ?

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 I2 I3 175.47(4) . . ?
I4 I3 I2 94.54(3) . . ?
I5 I4 I3 176.39(5) . . ?
C34 C1 N1 109.9(13) . . ?
C6 N1 C2 119.9(16) . . ?
C6 N1 C1 120.2(13) . . ?
C2 N1 C1 119.8(16) . . ?
N1 C2 C3 122.3(19) . . ?
C4 C3 C2 118.8(16) . . ?
C3 C4 C7 119.9(14) . . ?
C3 C4 C5 116.9(16) . . ?
C7 C4 C5 122.8(16) . . ?
C6 C5 C4 120.4(17) . . ?
N1 C6 C5 121.5(15) . . ?
C8 C7 C11 117.3(17) . . ?
C8 C7 C4 123.5(18) . . ?
C11 C7 C4 119.0(14) . . ?
C9 C8 C7 123(2) . . ?
C8 C9 N2 119.7(16) . . ?
C9 N2 C10 119.6(16) . . ?
C9 N2 C12 120.3(15) . . ?
C10 N2 C12 119.8(17) . . ?
C11 C10 N2 121.4(18) . . ?
C10 C11 C7 119.1(15) . . ?
N2 C12 C13 109.6(12) . . ?
C18 C13 C14 121.3(17) . . ?
C18 C13 C12 120.1(16) . . ?
C14 C13 C12 117.7(17) . . ?
C15 C14 C13 118.8(15) . . ?
C14 C15 C16 120.9(16) . . ?
C17 C16 C15 119.1(17) . . ?
C17 C16 C19 120.8(16) . . ?
C15 C16 C19 120.1(16) . . ?
C16 C17 C18 120.3(16) . . ?
C13 C18 C17 119.1(16) . . ?
C16 C19 N3 107.9(11) . . ?
C20 N3 C24 120.6(14) . . ?
C20 N3 C19 121.8(13) . . ?
C24 N3 C19 117.5(15) . . ?
N3 C20 C21 122.3(15) . . ?
C20 C21 C22 119.0(17) . . ?
C21 C22 C23 117.6(15) . . ?
C21 C22 C25 121.0(15) . . ?
C23 C22 C25 121.2(12) . . ?
C24 C23 C22 120.8(14) . . ?
C23 C24 N3 119.6(16) . . ?
C26 C25 C29 118.7(15) . . ?
C26 C25 C22 120.1(12) . . ?
C29 C25 C22 121.0(15) . . ?
C25 C26 C27 119.1(15) . . ?
N4 C27 C26 121.4(19) . . ?
C28 N4 C27 118.0(17) . . ?
C28 N4 C30 123.7(15) . . ?
C27 N4 C30 118.1(19) . . ?
C29 C28 N4 121.1(17) . . ?
C28 C29 C25 121.3(19) . . ?
C31 C30 N4 107.9(13) . . ?
C32 C31 C36 117.6(17) . . ?
C32 C31 C30 122.3(16) . . ?
C36 C31 C30 119.8(17) . . ?
C33 C32 C31 123.1(16) . . ?
C32 C33 C34 119.6(16) . . ?
C35 C34 C33 119.2(16) . . ?
C35 C34 C1 119.1(15) . . ?
C33 C34 C1 121.5(14) . . ?
C36 C35 C34 121.0(14) . . ?
C35 C36 C31 119.5(15) . . ?
I63 I11 I61 142.2(4) . . ?
I63 I11 I12 9.4(3) . . ?
I61 I11 I12 145.63(12) . . ?
I53 I12 I63 168.32(17) . . ?
I53 I12 I13 13.36(11) . . ?
I63 I12 I13 175.60(13) . . ?
I53 I12 I11 171.66(14) . . ?
I63 I12 I11 3.43(12) . . ?
I13 I12 I11 174.32(10) . . ?
I53 I13 I51 147.5(3) . . ?
I53 I13 I12 18.26(18) . . ?
I51 I13 I12 148.48(16) . . ?
I42 I21 I52 172.50(17) 1_455 1_455 ?
I42 I21 I23 12.52(11) 1_455 . ?
I52 I21 I23 166.91(13) 1_455 . ?
I42 I21 I22 169.58(14) 1_455 . ?
I52 I21 I22 8.89(11) 1_455 . ?
I23 I21 I22 175.44(8) . . ?
I52 I22 I51 144.2(3) 1_455 1_455 ?
I52 I22 I21 18.1(2) 1_455 . ?
I51 I22 I21 151.54(12) 1_455 . ?
I42 I23 I41 172.5(2) 1_455 1_455 ?
I42 I23 I21 13.62(13) 1_455 . ?
I41 I23 I21 160.23(15) 1_455 . ?
I43 I31 I41 151.9(6) 1_344 1_344 ?
I43 I31 I32 2.9(5) 1_344 . ?
I41 I31 I32 152.20(14) 1_344 . ?
I62 I32 I43 165.97(18) . 1_344 ?
I62 I32 I33 19.54(11) . . ?
I43 I32 I33 174.10(13) 1_344 . ?
I62 I32 I31 166.04(15) . . ?
I43 I32 I31 0.85(16) 1_344 . ?
I33 I32 I31 173.62(10) . . ?
I61 I33 I62 157.7(2) . . ?
I61 I33 I32 153.10(15) . . ?
I62 I33 I32 18.05(11) . . ?
I23 I41 I31 178.3(2) 1_655 1_766 ?
I23 I41 I42 3.69(10) 1_655 . ?
I31 I41 I42 177.44(14) 1_766 . ?
I23 I41 I43 173.24(18) 1_655 . ?
I31 I41 I43 6.30(12) 1_766 . ?
I42 I41 I43 176.00(13) . . ?
I23 I42 I21 153.9(2) 1_655 1_655 ?
I23 I42 I41 3.79(10) 1_655 . ?
I21 I42 I41 150.97(17) 1_655 . ?
I31 I43 I32 176.2(7) 1_766 1_766 ?
I31 I43 I41 21.8(5) 1_766 . ?
I32 I43 I41 158.45(19) 1_766 . ?
I13 I51 I22 165.24(19) . 1_655 ?
I13 I51 I52 170.63(19) . . ?
I22 I51 I52 11.79(9) 1_655 . ?
I13 I51 I53 13.41(12) . . ?
I22 I51 I53 167.26(16) 1_655 . ?
I52 I51 I53 175.95(15) . . ?
I22 I52 I21 153.0(3) 1_655 1_655 ?
I22 I52 I51 24.04(19) 1_655 . ?
I21 I52 I51 157.52(17) 1_655 . ?
I13 I53 I12 148.4(3) . . ?
I13 I53 I51 19.07(16) . . ?
I12 I53 I51 148.99(17) . . ?
I33 I61 I11 177.43(19) . . ?
I33 I61 I63 167.83(18) . . ?
I11 I61 I63 9.62(10) . . ?
I33 I61 I62 11.89(11) . . ?
I11 I61 I62 170.67(13) . . ?
I63 I61 I62 178.11(12) . . ?
I32 I62 I33 142.4(2) . . ?
I32 I62 I61 142.25(16) . . ?
I33 I62 I61 10.40(10) . . ?
I11 I63 I12 167.2(5) . . ?
I11 I63 I61 28.2(3) . . ?
I12 I63 I61 155.19(17) . . ?

_refine_diff_density_max         5.238
_refine_diff_density_min         -3.117
_refine_diff_density_rms         0.294

# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.943 Why?
RESPONSE: loss of some reflections during reduction procedure is mainly
due to the twinning issue affecting the crystals
;
_vrf_PLAT230_shelx               
;
PROBLEM: Hirshfeld Test Diff for C32 --C33 . 7.6 s.u.
RESPONSE: mainly due to poor quality of data and twinning issue affecting the crystals
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02412 Ang.
RESPONSE: mainly due to poor quality of data and twinning issue affecting the crystals
;
_vrf_PLAT780_shelx               
;
PROBLEM: Coordinates do not Form a Properly Connected Set Please Do !
RESPONSE: ...
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 46 Note
RESPONSE: due to beam stop mask during reduction procedure
;
# end Validation Reply Form
#===END

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1957896'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2019-10-10 deposited with the CCDC.	2019-11-25 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            'C36 H32 I16 N4'
_chemical_formula_weight         2551.05

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.1476(7)
_cell_length_b                   13.0508(10)
_cell_length_c                   21.8164(17)
_cell_angle_alpha                94.315(6)
_cell_angle_beta                 100.436(6)
_cell_angle_gamma                97.640(6)
_cell_volume                     2801.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    4118
_cell_measurement_theta_min      4.3770
_cell_measurement_theta_max      25.0400

_exptl_crystal_description       prismatic
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.024
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    8.866
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.74997
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            27093
_diffrn_reflns_av_unetI/netI     0.1644
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.130
_diffrn_reflns_theta_max         28.388
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             11421
_reflns_number_gt                6016
_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       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1056P)²+16.1309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11421
_refine_ls_number_parameters     435
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.0910
_refine_ls_wR_factor_ref         0.2618
_refine_ls_wR_factor_gt          0.2019
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_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
I1 I 0.58244(16) 0.57654(12) 0.07373(6) 0.0374(4) Uani 1 1 d . . . . .
I2 I 0.52697(14) 0.69216(11) 0.17810(6) 0.0307(4) Uani 1 1 d . . . . .
I3 I 0.48624(14) 0.80822(11) 0.29687(6) 0.0304(4) Uani 1 1 d . . . . .
I4 I 0.16780(16) 0.77611(14) 0.26499(7) 0.0493(5) Uani 1 1 d . . . . .
I5B I -0.1104(6) 0.7227(16) 0.2385(6) 0.031(3) Uani 0.50(4) 1 d . . P . .
I5A I -0.1153(5) 0.7631(16) 0.2232(6) 0.033(3) Uani 0.50(4) 1 d . . P . .
I11 I 0.9215(3) 1.0166(2) 0.09505(12) 0.0292(7) Uani 0.4993(11) 1 d . . P . .
I12 I 1.0856(3) 1.1343(2) 0.20521(12) 0.0303(7) Uani 0.4993(11) 1 d . . P . .
I13 I 1.2604(3) 1.2447(2) 0.32426(13) 0.0368(7) Uani 0.4993(11) 1 d . . P . .
I14 I 1.3389(3) 1.0389(3) 0.38743(15) 0.0314(8) Uani 0.4993(11) 1 d . . P . .
I15 I 1.3714(4) 0.8692(3) 0.45308(16) 0.0340(9) Uani 0.4993(11) 1 d . . P . .
I21 I -0.3879(3) 0.3180(2) -0.55706(12) 0.0316(7) Uani 0.4993(11) 1 d . . P . .
I22 I -0.1785(3) 0.4434(2) -0.45737(11) 0.0274(6) Uani 0.4993(11) 1 d . . P . .
I23 I 0.0070(3) 0.5766(2) -0.35946(12) 0.0315(7) Uani 0.4993(11) 1 d . . P . .
I31 I 0.2137(3) 0.6604(2) -0.20328(12) 0.0315(7) Uani 0.4993(11) 1 d . . P . .
I32 I 0.4552(3) 0.7442(2) -0.11130(11) 0.0247(6) Uani 0.4993(11) 1 d . . P . .
I33 I 0.7195(3) 0.8252(2) -0.03025(12) 0.0301(7) Uani 0.4993(11) 1 d . . P . .
I41 I -0.3724(3) -0.0042(3) -0.41182(14) 0.0311(8) Uani 0.5007(11) 1 d . . P .
.
I42 I -0.3304(4) 0.1860(3) -0.45720(15) 0.0323(8) Uani 0.5007(11) 1 d . . P . .
I43 I -0.2605(3) 0.3961(2) -0.51996(12) 0.0337(7) Uani 0.5007(11) 1 d . . P . .
I44 I -0.0700(3) 0.5144(2) -0.40621(12) 0.0292(7) Uani 0.5007(11) 1 d . . P . .
I45 I 0.1061(3) 0.6257(2) -0.29770(12) 0.0318(7) Uani 0.5007(11) 1 d . . P . .
I51 I 0.3098(3) 0.7224(2) -0.14037(11) 0.0316(7) Uani 0.5007(11) 1 d . . P . .
I52 I 0.5728(3) 0.8087(2) -0.05782(11) 0.0267(6) Uani 0.5007(11) 1 d . . P . .
I53 I 0.8099(3) 0.9116(2) 0.02990(12) 0.0326(7) Uani 0.5007(11) 1 d . . P . .
I61 I -0.9723(3) 0.1013(2) -0.85387(11) 0.0302(7) Uani 0.5007(11) 1 d . . P . .
I62 I -0.7957(3) 0.1844(2) -0.73602(11) 0.0272(7) Uani 0.5007(11) 1 d . . P . .
I63 I -0.5967(3) 0.2692(2) -0.62124(11) 0.0320(7) Uani 0.5007(11) 1 d . . P . .
C1 C 0.840(3) 0.722(3) 0.4706(14) 0.082(10) Uiso 1 1 d . . . . .
H1A H 0.8157 0.7259 0.5115 0.098 Uiso 1 1 calc R U . . .
H1B H 0.9255 0.6950 0.4744 0.098 Uiso 1 1 calc R U . . .
N1 N 0.733(2) 0.6492(17) 0.4256(9) 0.054(6) Uani 1 1 d . U . . .
C2 C 0.612(3) 0.626(2) 0.4380(12) 0.053(7) Uiso 1 1 d . . . . .
H2 H 0.5969 0.6476 0.4774 0.063 Uiso 1 1 calc R U . . .
C3 C 0.503(3) 0.569(2) 0.3926(11) 0.053(7) Uiso 1 1 d . . . . .
H3 H 0.4174 0.5498 0.4020 0.064 Uiso 1 1 calc R U . . .
C4 C 0.529(3) 0.5439(19) 0.3354(10) 0.044(6) Uiso 1 1 d . . . . .
C5 C 0.654(3) 0.560(2) 0.3240(12) 0.053(7) Uiso 1 1 d . . . . .
H5 H 0.6728 0.5361 0.2857 0.064 Uiso 1 1 calc R U . . .
C6 C 0.755(3) 0.614(2) 0.3699(11) 0.052(7) Uiso 1 1 d . . . . .
H6 H 0.8427 0.6273 0.3619 0.062 Uiso 1 1 calc R U . . .
C7 C 0.414(2) 0.4913(19) 0.2810(10) 0.041(6) Uiso 1 1 d . . . . .
C8 C 0.284(3) 0.514(2) 0.2811(11) 0.050(6) Uiso 1 1 d . . . . .
H8 H 0.2665 0.5495 0.3166 0.060 Uiso 1 1 calc R U . . .
C9 C 0.182(3) 0.485(2) 0.2305(12) 0.063(8) Uiso 1 1 d . . . . .
H9 H 0.0954 0.5018 0.2296 0.076 Uiso 1 1 calc R U . . .
N2 N 0.215(3) 0.4288(15) 0.1807(8) 0.061(7) Uani 1 1 d . . . . .
C10 C 0.325(3) 0.394(2) 0.1791(12) 0.054(7) Uiso 1 1 d . . . . .
H10 H 0.3329 0.3463 0.1469 0.064 Uiso 1 1 calc R U . . .
C11 C 0.436(3) 0.4327(19) 0.2293(10) 0.048(6) Uiso 1 1 d . . . . .
H11 H 0.5223 0.4184 0.2272 0.058 Uiso 1 1 calc R U . . .
C12 C 0.106(3) 0.402(2) 0.1223(12) 0.066(8) Uiso 1 1 d . . . . .
H12A H 0.0177 0.3824 0.1331 0.079 Uiso 1 1 calc R U . . .
H12B H 0.1251 0.3445 0.0960 0.079 Uiso 1 1 calc R U . . .
C13 C 0.109(2) 0.5002(19) 0.0890(10) 0.043(6) Uiso 1 1 d . . . . .
C14 C 0.012(3) 0.567(2) 0.0965(11) 0.057(7) Uiso 1 1 d . . . . .
H14 H -0.0590 0.5481 0.1170 0.068 Uiso 1 1 calc R U . . .
C15 C 0.028(3) 0.667(2) 0.0710(12) 0.065(8) Uiso 1 1 d . . . . .
H15 H -0.0308 0.7147 0.0765 0.078 Uiso 1 1 calc R U . . .
C16 C 0.133(3) 0.690(2) 0.0379(11) 0.048(6) Uiso 1 1 d . . . . .
C17 C 0.210(2) 0.6175(18) 0.0262(9) 0.038(5) Uiso 1 1 d . . . . .
H17 H 0.2741 0.6310 0.0009 0.046 Uiso 1 1 calc R U . . .
C18 C 0.197(2) 0.5264(18) 0.0502(9) 0.036(5) Uiso 1 1 d . . . . .
H18 H 0.2513 0.4780 0.0400 0.043 Uiso 1 1 calc R U . . .
C19 C 0.153(3) 0.793(2) 0.0172(14) 0.076(9) Uiso 1 1 d . . . . .
H19A H 0.1843 0.7899 -0.0222 0.091 Uiso 1 1 calc R U . . .
H19B H 0.0669 0.8201 0.0104 0.091 Uiso 1 1 calc R U . . .
N3 N 0.247(3) 0.8607(15) 0.0623(9) 0.063(7) Uani 1 1 d . . . . .
C20 C 0.227(3) 0.895(2) 0.1184(12) 0.059(7) Uiso 1 1 d . . . . .
H20 H 0.1418 0.8806 0.1282 0.070 Uiso 1 1 calc R U . . .
C21 C 0.332(3) 0.950(2) 0.1620(12) 0.053(7) Uiso 1 1 d . . . . .
H21 H 0.3138 0.9723 0.2006 0.063 Uiso 1 1 calc R U . . .
C22 C 0.463(3) 0.975(2) 0.1527(11) 0.049(6) Uiso 1 1 d . . . . .
C23 C 0.483(4) 0.936(3) 0.0939(16) 0.106(12) Uiso 1 1 d . . . . .
H23 H 0.5674 0.9434 0.0829 0.127 Uiso 1 1 calc R U . . .
C24 C 0.356(4) 0.882(3) 0.0496(18) 0.090(12) Uiso 1 1 d . . . . .
H24 H 0.3643 0.8641 0.0086 0.108 Uiso 1 1 calc R U . . .
C25 C 0.577(3) 1.021(2) 0.2024(11) 0.053(7) Uiso 1 1 d . . . . .
C26 C 0.553(3) 1.095(2) 0.2486(11) 0.054(7) Uiso 1 1 d . . . . .
H26 H 0.4733 1.1234 0.2434 0.065 Uiso 1 1 calc R U . . .
C27 C 0.653(3) 1.124(2) 0.3020(13) 0.063(8) Uiso 1 1 d . . . . .
H27 H 0.6345 1.1658 0.3349 0.075 Uiso 1 1 calc R U . . .
N4 N 0.771(3) 1.094(2) 0.3071(13) 0.087(9) Uani 1 1 d . . . . .
C28 C 0.788(3) 1.023(2) 0.2536(14) 0.074(9) Uiso 1 1 d . . . . .
H28 H 0.8697 0.9973 0.2561 0.089 Uiso 1 1 calc R U . . .
C29 C 0.699(4) 0.997(3) 0.2050(16) 0.089(10) Uiso 1 1 d . . . . .
H29 H 0.7191 0.9598 0.1707 0.107 Uiso 1 1 calc R U . . .
C30 C 0.879(4) 1.108(3) 0.3678(18) 0.110(13) Uiso 1 1 d . . . . .
H30A H 0.9681 1.1252 0.3578 0.133 Uiso 1 1 calc R U . . .
H30B H 0.8636 1.1653 0.3953 0.133 Uiso 1 1 calc R U . . .
C31 C 0.874(4) 1.011(3) 0.4011(15) 0.090(10) Uiso 1 1 d . . . . .
C32 C 0.769(3) 0.975(2) 0.4310(10) 0.048(6) Uiso 1 1 d . . . . .
H32 H 0.7031 1.0172 0.4351 0.058 Uiso 1 1 calc R U . . .
C33 C 0.759(3) 0.883(2) 0.4541(11) 0.058(7) Uiso 1 1 d . . . . .
H33 H 0.6840 0.8607 0.4716 0.070 Uiso 1 1 calc R U . . .
C34 C 0.858(3) 0.819(3) 0.4525(13) 0.073(9) Uiso 1 1 d . . . . .
C35 C 0.968(4) 0.859(3) 0.4244(15) 0.099(11) Uiso 1 1 d . . . . .
H35 H 1.0366 0.8185 0.4240 0.119 Uiso 1 1 calc R U . . .
C36 C 0.985(4) 0.952(3) 0.3980(16) 0.103(12) Uiso 1 1 d . . . . .
H36 H 1.0594 0.9735 0.3801 0.124 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
I1 I2 2.8198(19) . ?
I2 I3 3.0238(18) . ?
I3 I4 3.144(2) . ?
I4 I5B 2.760(5) . ?
I4 I5A 2.831(7) . ?
I5B I5A 0.648(4) . ?
I11 I61 1.639(4) 1_766 ?
I11 I53 1.973(4) . ?
I11 I12 2.868(4) . ?
I12 I61 1.329(4) 1_766 ?
I12 I62 1.621(4) 1_766 ?
I12 I13 3.010(4) . ?
I13 I62 1.459(4) 1_766 ?
I13 I63 1.677(4) 1_766 ?
I14 I41 0.784(3) 2_665 ?
I14 I15 2.750(5) . ?
I14 I63 3.017(5) 1_766 ?
I15 I42 0.803(4) 2_665 ?
I15 I41 2.037(5) 2_665 ?
I21 I43 1.584(4) . ?
I21 I63 2.299(4) . ?
I21 I42 2.903(4) . ?
I21 I22 2.964(4) . ?
I22 I43 1.504(4) . ?
I22 I44 1.564(4) . ?
I22 I23 2.871(4) . ?
I23 I44 1.314(4) . ?
I23 I45 1.564(4) . ?
I31 I51 1.622(4) . ?
I31 I45 2.134(4) . ?
I31 I32 2.899(4) . ?
I32 I51 1.477(4) . ?
I32 I52 1.605(4) . ?
I32 I33 2.947(4) . ?
I33 I52 1.482(4) . ?
I33 I53 1.703(4) . ?
I41 I14 0.785(3) 2_665 ?
I41 I15 2.037(5) 2_665 ?
I41 I42 2.750(5) . ?
I42 I15 0.803(4) 2_665 ?
I43 I44 3.029(4) . ?
I44 I45 2.858(4) . ?
I51 I52 2.964(4) . ?
I52 I53 2.888(4) . ?
I61 I12 1.329(4) 1_344 ?
I61 I11 1.639(4) 1_344 ?
I61 I62 2.897(4) . ?
I62 I13 1.459(4) 1_344 ?
I62 I12 1.621(4) 1_344 ?
I62 I63 2.955(4) . ?
I63 I13 1.677(4) 1_344 ?
I63 I14 3.017(5) 1_344 ?
C1 C34 1.35(4) . ?
C1 N1 1.50(3) . ?
N1 C2 1.30(3) . ?
N1 C6 1.33(3) . ?
C2 C3 1.43(3) . ?
C3 C4 1.35(3) . ?
C4 C5 1.33(3) . ?
C4 C7 1.55(3) . ?
C5 C6 1.37(3) . ?
C7 C11 1.38(3) . ?
C7 C8 1.39(3) . ?
C8 C9 1.36(3) . ?
C9 N2 1.38(3) . ?
N2 C10 1.26(3) . ?
N2 C12 1.51(3) . ?
C10 C11 1.43(3) . ?
C12 C13 1.52(3) . ?
C13 C18 1.37(3) . ?
C13 C14 1.42(3) . ?
C14 C15 1.45(4) . ?
C15 C16 1.41(3) . ?
C16 C17 1.34(3) . ?
C16 C19 1.46(4) . ?
C17 C18 1.34(3) . ?
C19 N3 1.40(3) . ?
N3 C24 1.19(4) . ?
N3 C20 1.33(3) . ?
C20 C21 1.37(3) . ?
C21 C22 1.38(3) . ?
C22 C23 1.40(4) . ?
C22 C25 1.46(3) . ?
C23 C24 1.51(5) . ?
C25 C29 1.31(4) . ?
C25 C26 1.42(3) . ?
C26 C27 1.39(3) . ?
C27 N4 1.30(4) . ?
N4 C28 1.48(4) . ?
N4 C30 1.54(4) . ?
C28 C29 1.26(4) . ?
C30 C31 1.50(5) . ?
C31 C32 1.40(4) . ?
C31 C36 1.46(5) . ?
C32 C33 1.34(3) . ?
C33 C34 1.39(4) . ?
C34 C35 1.43(4) . ?
C35 C36 1.38(4) . ?

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 I2 I3 175.11(6) . . ?
I2 I3 I4 96.96(5) . . ?
I5B I4 I5A 13.24(9) . . ?
I5B I4 I3 173.0(5) . . ?
I5A I4 I3 172.5(5) . . ?
I5A I5B I4 89.6(10) . . ?
I5B I5A I4 77.1(9) . . ?
I61 I11 I53 174.1(2) 1_766 . ?
I61 I11 I12 13.47(11) 1_766 . ?
I53 I11 I12 168.25(16) . . ?
I61 I12 I62 158.1(3) 1_766 1_766 ?
I61 I12 I11 16.69(15) 1_766 . ?
I62 I12 I11 166.66(18) 1_766 . ?
I61 I12 I13 166.0(2) 1_766 . ?
I62 I12 I13 11.61(11) 1_766 . ?
I11 I12 I13 176.28(13) . . ?
I62 I13 I63 140.7(2) 1_766 1_766 ?
I62 I13 I12 12.93(13) 1_766 . ?
I63 I13 I12 153.37(18) 1_766 . ?
I41 I14 I15 21.0(4) 2_665 . ?
I41 I14 I63 129.8(4) 2_665 1_766 ?
I15 I14 I63 149.69(16) . 1_766 ?
I42 I15 I41 147.9(5) 2_665 2_665 ?
I42 I15 I14 140.0(5) 2_665 . ?
I41 I15 I14 7.92(13) 2_665 . ?
I43 I21 I63 156.4(2) . . ?
I43 I21 I42 85.99(16) . . ?
I63 I21 I42 114.05(15) . . ?
I43 I21 I22 15.89(11) . . ?
I63 I21 I22 157.50(14) . . ?
I42 I21 I22 73.36(11) . . ?
I43 I22 I44 161.6(2) . . ?
I43 I22 I23 163.65(19) . . ?
I44 I22 I23 3.65(12) . . ?
I43 I22 I21 16.76(13) . . ?
I44 I22 I21 177.20(18) . . ?
I23 I22 I21 174.96(13) . . ?
I44 I23 I45 166.3(3) . . ?
I44 I23 I22 4.35(14) . . ?
I45 I23 I22 166.45(19) . . ?
I51 I31 I45 161.2(2) . . ?
I51 I31 I32 19.67(12) . . ?
I45 I31 I32 151.73(16) . . ?
I51 I32 I52 148.2(2) . . ?
I51 I32 I31 21.68(12) . . ?
I52 I32 I31 168.82(17) . . ?
I51 I32 I33 164.82(18) . . ?
I52 I32 I33 16.60(11) . . ?
I31 I32 I33 172.93(12) . . ?
I52 I33 I53 130.0(2) . . ?
I52 I33 I32 18.02(12) . . ?
I53 I33 I32 148.00(17) . . ?
I14 I41 I15 151.1(5) 2_665 2_665 ?
I14 I41 I42 142.2(4) 2_665 . ?
I15 I41 I42 8.93(15) 2_665 . ?
I15 I42 I41 23.2(4) 2_665 . ?
I15 I42 I21 128.1(5) 2_665 . ?
I41 I42 I21 149.48(17) . . ?
I22 I43 I21 147.4(2) . . ?
I22 I43 I44 9.38(13) . . ?
I21 I43 I44 156.62(17) . . ?
I23 I44 I22 172.0(3) . . ?
I23 I44 I45 7.44(15) . . ?
I22 I44 I45 170.16(18) . . ?
I23 I44 I43 172.6(2) . . ?
I22 I44 I43 9.02(11) . . ?
I45 I44 I43 179.03(12) . . ?
I23 I45 I31 165.0(2) . . ?
I23 I45 I44 6.24(13) . . ?
I31 I45 I44 159.87(17) . . ?
I32 I51 I31 138.6(2) . . ?
I32 I51 I52 16.56(12) . . ?
I31 I51 I52 154.75(18) . . ?
I33 I52 I32 145.4(2) . . ?
I33 I52 I53 26.86(13) . . ?
I32 I52 I53 172.14(17) . . ?
I33 I52 I51 160.57(18) . . ?
I32 I52 I51 15.21(11) . . ?
I53 I52 I51 172.56(12) . . ?
I33 I53 I11 175.8(2) . . ?
I33 I53 I52 23.14(11) . . ?
I11 I53 I52 158.21(16) . . ?
I12 I61 I11 149.8(3) 1_344 1_344 ?
I12 I61 I62 12.06(15) 1_344 . ?
I11 I61 I62 158.15(18) 1_344 . ?
I13 I62 I12 155.5(2) 1_344 1_344 ?
I13 I62 I61 162.7(2) 1_344 . ?
I12 I62 I61 9.87(12) 1_344 . ?
I13 I62 I63 21.05(14) 1_344 . ?
I12 I62 I63 174.68(18) 1_344 . ?
I61 I62 I63 175.30(12) . . ?
I13 I63 I21 171.3(2) 1_344 . ?
I13 I63 I62 18.20(12) 1_344 . ?
I21 I63 I62 157.94(14) . . ?
I13 I63 I14 81.82(16) 1_344 1_344 ?
I21 I63 I14 104.44(13) . 1_344 ?
I62 I63 I14 73.76(11) . 1_344 ?
C34 C1 N1 113(3) . . ?
C2 N1 C6 119(2) . . ?
C2 N1 C1 120(2) . . ?
C6 N1 C1 121(2) . . ?
N1 C2 C3 122(2) . . ?
C4 C3 C2 116(3) . . ?
C5 C4 C3 122(3) . . ?
C5 C4 C7 118(2) . . ?
C3 C4 C7 120(2) . . ?
C4 C5 C6 118(2) . . ?
N1 C6 C5 122(3) . . ?
C11 C7 C8 118(2) . . ?
C11 C7 C4 123(2) . . ?
C8 C7 C4 118(2) . . ?
C9 C8 C7 122(2) . . ?
C8 C9 N2 116(3) . . ?
C10 N2 C9 127(3) . . ?
C10 N2 C12 116(2) . . ?
C9 N2 C12 117(3) . . ?
N2 C10 C11 117(3) . . ?
C7 C11 C10 120(2) . . ?
N2 C12 C13 105(2) . . ?
C18 C13 C14 118(2) . . ?
C18 C13 C12 123(2) . . ?
C14 C13 C12 119(2) . . ?
C13 C14 C15 118(2) . . ?
C16 C15 C14 119(3) . . ?
C17 C16 C15 120(3) . . ?
C17 C16 C19 123(2) . . ?
C15 C16 C19 117(2) . . ?
C18 C17 C16 121(2) . . ?
C17 C18 C13 124(2) . . ?
N3 C19 C16 110(2) . . ?
C24 N3 C20 119(3) . . ?
C24 N3 C19 116(3) . . ?
C20 N3 C19 125(3) . . ?
N3 C20 C21 120(3) . . ?
C20 C21 C22 125(3) . . ?
C21 C22 C23 114(3) . . ?
C21 C22 C25 124(2) . . ?
C23 C22 C25 121(3) . . ?
C22 C23 C24 115(3) . . ?
N3 C24 C23 126(4) . . ?
C29 C25 C26 120(3) . . ?
C29 C25 C22 122(3) . . ?
C26 C25 C22 118(2) . . ?
C27 C26 C25 118(3) . . ?
N4 C27 C26 121(3) . . ?
C27 N4 C28 115(3) . . ?
C27 N4 C30 125(3) . . ?
C28 N4 C30 119(3) . . ?
C29 C28 N4 124(3) . . ?
C28 C29 C25 120(4) . . ?
C31 C30 N4 111(3) . . ?
C32 C31 C36 120(3) . . ?
C32 C31 C30 124(3) . . ?
C36 C31 C30 116(3) . . ?
C33 C32 C31 123(3) . . ?
C32 C33 C34 121(3) . . ?
C1 C34 C33 121(3) . . ?
C1 C34 C35 124(3) . . ?
C33 C34 C35 115(3) . . ?
C36 C35 C34 128(4) . . ?
C35 C36 C31 113(4) . . ?

_refine_diff_density_max         2.918
_refine_diff_density_min         -2.156
_refine_diff_density_rms         0.652

# start Validation Reply Form
_vrf_PLAT201_shelx               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 36 Report
RESPONSE: Crystals are a solid solution from to equally represented individuals,
each containing a very high number of iodine atoms.
Reflections were not enough to anisotropically refine all not hydrogen atoms, so
the decision was taken to isotropically refine all carbon atoms
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 0.05A From I2 4.20 eA-3
RESPONSE: Each of the two equally represented individuals contains a very high 
number of iodine atoms, while the ligand is constituted only by lighter atoms, nitrogen
being the second heaviest species. This could probably favoured occurrence of
series truncation errors and spurious peaks near the heaviest atoms 
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04176 Ang.
RESPONSE: Crystals are a solid solution from to equally represented individuals. 
This fact most likely lowered the overal data quality
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 47 Note
RESPONSE: due to beam stop mask during reduction procedure
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 4 Check
RESPONSE: Crystals are a solid solution from to equally represented individuals. 
This fact most likely lowered the overal data quality. Nevertheless the 4 outliers
are found at low theta value, no higher than 5, so they shouldn't affect too much 
the overall structure quality
;
# end Validation Reply Form
#===END
