# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_Phase_I
_database_code_depnum_ccdc_archive 'CCDC 1966627'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2019-11-19 deposited with the CCDC.	2020-03-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H15 I9 N6 Sb2'
_chemical_formula_weight         1520.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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      hexagonal
_space_group_IT_number           186
_space_group_name_H-M_alt        'P 63 m c'
_space_group_name_Hall           'P 6c -2c'

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

_cell_length_a                   8.6995(2)
_cell_length_b                   8.6995(2)
_cell_length_c                   21.6776(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1420.79(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    194.9(3)
_cell_measurement_reflns_used    3051
_cell_measurement_theta_min      2.9080
_cell_measurement_theta_max      22.4150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.555
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    11.680
_exptl_absorpt_correction_T_min  0.36204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.673
_oxdiff_exptl_absorpt_empirical_full_max 1.928
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      194.9(3)
_diffrn_ambient_environment      N~2~
_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, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            10329
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.293
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.681
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1097
_reflns_number_gt                897
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.993

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0300P)²+4.0000P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.6(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1097
_refine_ls_number_parameters     43
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.654
_refine_ls_restrained_S_all      1.648
_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
Sb1 Sb 0.333333 0.666667 0.1408(3) 0.0622(15) Uani 1 6 d S T P . .
Sb2 Sb 0.333333 0.666667 0.3301(3) 0.0572(13) Uani 1 6 d S T P . .
I1 I 0.6525(8) 0.8262(4) 0.0676(3) 0.1352(19) Uani 1 2 d S T P . .
I2 I 0.49786(10) 0.50214(10) 0.2351(4) 0.0869(7) Uani 1 2 d S T P . .
I3 I 0.1726(3) 0.3451(7) 0.4002(3) 0.1149(15) Uani 1 2 d S T P . .
C1 C 0.000000 0.000000 0.220(4) 0.16(3) Uiso 1 6 d DS . P . .
H1 H -0.013735 0.079009 0.194837 0.194 Uiso 0.1667 1 calc R U P . .
N2 N 0.105(8) 0.053(4) 0.267(5) 0.16(3) Uiso 0.3333 2 d DS . P . .
H2A H 0.115352 -0.023495 0.289768 0.194 Uiso 0.1667 1 calc R U P . .
H2B H 0.165110 0.163726 0.276423 0.194 Uiso 0.1667 1 calc R U P . .
N3 N -0.0849(7) -0.1697(14) 0.210(4) 0.16(3) Uiso 0.3333 2 d DS . P . .
H3A H -0.069457 -0.239559 0.233767 0.194 Uiso 0.1667 1 calc R U P . .
H3B H -0.156494 -0.212342 0.178987 0.194 Uiso 0.1667 1 calc R U P . .
C6 C 0.666667 0.333333 0.0683(17) 0.090(14) Uiso 1 6 d DS . P . .
H6 H 0.670851 0.335425 0.111129 0.109 Uiso 0.3333 6 calc R U P . .
N7 N 0.664(4) 0.4642(18) 0.0403(17) 0.090(14) Uiso 0.3333 1 d D . P . .
H7A H 0.660069 0.465963 0.000642 0.109 Uiso 0.3333 1 calc R U P . .
H7B H 0.665995 0.548864 0.061373 0.109 Uiso 0.3333 1 calc R U P . .
C4 C 0.666667 0.333333 0.366(3) 0.17(3) Uiso 1 6 d DS . P . .
H4 H 0.603138 0.301569 0.328955 0.203 Uiso 0.3333 2 calc R U P . .
N5 N 0.692(9) 0.202(4) 0.380(2) 0.17(3) Uiso 0.3333 1 d D . P . .
H5A H 0.749112 0.208002 0.413475 0.203 Uiso 0.3333 1 calc R U P . .
H5B H 0.651565 0.110511 0.356994 0.203 Uiso 0.3333 1 calc R U 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
Sb1 I1 2.881(6) 2_665 ?
Sb1 I1 2.881(6) 3_565 ?
Sb1 I1 2.881(6) . ?
Sb1 I2 3.213(5) 2_665 ?
Sb1 I2 3.213(5) 3_565 ?
Sb1 I2 3.213(5) . ?
Sb2 I3 2.859(5) 3_565 ?
Sb2 I3 2.859(5) 2_665 ?
Sb2 I3 2.859(5) . ?
Sb2 I2 3.224(5) . ?
Sb2 I2 3.224(5) 3_565 ?
Sb2 I2 3.224(5) 2_665 ?
C1 N3 1.297(7) . ?
C1 N2 1.299(7) . ?
C1 H1 0.9300 . ?
C1 H1 0.9300 2 ?
C1 H1 0.9300 3 ?
C1 H1 0.9300 7 ?
C1 H1 0.9300 8 ?
C1 H1 0.9300 9 ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 H3A 0.8600 8 ?
C6 N7 1.300(7) 9 ?
C6 N7 1.300(7) . ?
C6 H6 0.9300 . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
C4 N5 1.302(7) . ?
C4 N5 1.302(7) 9 ?
C4 H4 0.9300 . ?
N5 H5A 0.8600 . ?
N5 H5B 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
I1 Sb1 I1 92.6(2) 2_665 3_565 ?
I1 Sb1 I1 92.6(2) 2_665 . ?
I1 Sb1 I1 92.6(2) 3_565 . ?
I1 Sb1 I2 91.63(10) 2_665 2_665 ?
I1 Sb1 I2 173.9(2) 3_565 2_665 ?
I1 Sb1 I2 91.63(10) . 2_665 ?
I1 Sb1 I2 91.63(10) 2_665 3_565 ?
I1 Sb1 I2 91.63(10) 3_565 3_565 ?
I1 Sb1 I2 173.9(2) . 3_565 ?
I2 Sb1 I2 83.87(17) 2_665 3_565 ?
I1 Sb1 I2 173.9(2) 2_665 . ?
I1 Sb1 I2 91.63(10) 3_565 . ?
I1 Sb1 I2 91.63(10) . . ?
I2 Sb1 I2 83.87(17) 2_665 . ?
I2 Sb1 I2 83.87(17) 3_565 . ?
I3 Sb2 I3 94.40(19) 3_565 2_665 ?
I3 Sb2 I3 94.40(19) 3_565 . ?
I3 Sb2 I3 94.40(19) 2_665 . ?
I3 Sb2 I2 172.4(2) 3_565 . ?
I3 Sb2 I2 90.79(10) 2_665 . ?
I3 Sb2 I2 90.79(10) . . ?
I3 Sb2 I2 90.79(10) 3_565 3_565 ?
I3 Sb2 I2 172.4(2) 2_665 3_565 ?
I3 Sb2 I2 90.79(10) . 3_565 ?
I2 Sb2 I2 83.52(16) . 3_565 ?
I3 Sb2 I2 90.79(10) 3_565 2_665 ?
I3 Sb2 I2 90.79(10) 2_665 2_665 ?
I3 Sb2 I2 172.4(2) . 2_665 ?
I2 Sb2 I2 83.52(16) . 2_665 ?
I2 Sb2 I2 83.52(16) 3_565 2_665 ?
Sb1 I2 Sb2 79.23(6) . . ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag

N2 H2A I3 0.86 2.88 3.69(9) 157.2 3 yes
N3 H3B I1 0.86 3.04 3.83(7) 152.3 1_445 yes
N7 H7B I1 0.86 2.48 3.255(7) 150.8 . yes
N7 H7A I3 0.86 2.68 3.41(3) 144.0 4_664 yes
N5 H5B I2 0.86 2.90 3.60(5) 139.5 2_655 yes

_refine_diff_density_max         0.836
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.140



