# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_ig_918_0m
_database_code_depnum_ccdc_archive 'CCDC 2120270'
loop_
_audit_author_name
_audit_author_address
'Ilya Guralskiy'
;Taras Shevchenko National University of Kyiv
Ukraine
;
_audit_update_record             
;
2022-01-13 deposited with the CCDC.	2022-01-13 downloaded from the CCDC.
;
_audit_creation_date             2021-01-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1.5(Hg2 I8), C18 H47.999 Fe3 N35.999 O6'
_chemical_formula_sum            'C18 H48 Fe3 Hg3 I12 N36 O6'
_chemical_formula_weight         3156.98
_chemical_melting_point          ?
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   19.2123(15)
_cell_length_b                   19.2123(15)
_cell_length_c                   31.531(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10079.3(18)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    3424
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.974
_cell_measurement_theta_min      2.768
_shelx_estimated_absorpt_T_max   0.562
_shelx_estimated_absorpt_T_min   0.387
_exptl_absorpt_coefficient_mu    13.035
_exptl_absorpt_correction_T_max  0.5991
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'c.f. r.h. blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8460
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.441
_diffrn_reflns_theta_min         1.779
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1799
_reflns_number_total             2313
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0666
_refine_ls_restrained_S_all      1.218
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+1091.0433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1579
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H,H,H) groups
2. Others
 Fixed Sof: I2A(0.5) Fe2(0.16667) H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5)
 I1A(0.5) I2B(0.5) I1B(0.5)
3.a Riding coordinates:
 N7(H7), O1(H1AA,H1AB), O1(H1BC), O1(H1BD), N4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Hg1 Hg 0.29329(5) 0.333333 0.583333 0.0395(3) Uani 1 2 d S T P . .
I2A I 0.2000(8) 0.2857(8) 0.5094(4) 0.047(2) Uani 0.5 1 d . . P A 1
Fe1 Fe 0.333333 0.666667 0.47523(11) 0.0212(7) Uani 1 3 d S T P . .
Fe2 Fe 0.333333 0.666667 0.5946(2) 0.0255(16) Uani 0.5 3 d S T P B 1
N5 N 0.3383(7) 0.5832(7) 0.4387(3) 0.022(2) Uani 1 1 d . . . . .
N2 N 0.4312(10) 0.6825(10) 0.5533(5) 0.051(4) Uani 1 1 d . . . . .
N6 N 0.333333 0.4745(9) 0.416667 0.030(4) Uani 1 2 d S T P . .
N3 N 0.5408(10) 0.6887(10) 0.5306(6) 0.050(4) Uani 1 1 d . . . . .
N1 N 0.4265(8) 0.6757(8) 0.5107(4) 0.033(3) Uani 1 1 d . . . . .
N7 N 0.333333 0.4010(11) 0.416667 0.060(7) Uani 1 2 d S T P . .
H7 H 0.310870 0.366087 0.398570 0.071 Uiso 1 1 d R U . . .
C3 C 0.3411(9) 0.5195(10) 0.4508(5) 0.029(3) Uani 1 1 d . . . . .
H3 H 0.347710 0.507181 0.479142 0.035 Uiso 1 1 calc R U . . .
C1 C 0.4913(10) 0.6783(10) 0.4974(6) 0.037(4) Uani 1 1 d . . . . .
H1 H 0.502783 0.673650 0.468551 0.044 Uiso 1 1 calc R U . . .
O1 O 0.2341(12) 0.6456(12) 0.6318(5) 0.094(6) Uani 1 1 d . . . . .
H1AA H 0.231416 0.671165 0.652796 0.141 Uiso 0.5 1 d R U P B 1
H1AB H 0.187536 0.624765 0.621316 0.141 Uiso 0.5 1 d R U P B 1
H1BC H 0.248166 0.674845 0.609526 0.141 Uiso 0.5 1 d R U P B 2
H1BD H 0.257286 0.617155 0.634146 0.141 Uiso 0.5 1 d R U P B 2
C2 C 0.5016(14) 0.6887(14) 0.5636(6) 0.055(6) Uani 1 1 d . . . . .
H2 H 0.520392 0.692756 0.591827 0.066 Uiso 1 1 calc R U . . .
N4 N 0.6142(11) 0.6938(14) 0.5302(7) 0.079(6) Uani 1 1 d . . . . .
H4A H 0.643674 0.683409 0.514774 0.095 Uiso 1 1 d R U . . .
H4B H 0.644834 0.742779 0.534914 0.095 Uiso 1 1 d R U . . .
I1A I 0.4346(6) 0.4710(6) 0.5607(3) 0.0453(15) Uani 0.5 1 d . . P A 2
I2B I 0.1956(8) 0.3019(7) 0.5139(4) 0.048(2) Uani 0.5 1 d . . P A 2
I1B I 0.4484(6) 0.4578(7) 0.5600(4) 0.0495(19) Uani 0.5 1 d . . P A 2


_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
Hg1 I2A 2.801(14) 17 ?
Hg1 I2A 2.802(15) . ?
Hg1 I1A 2.774(10) 17 ?
Hg1 I1A 2.774(11) . ?
Hg1 I2B 2.747(14) . ?
Hg1 I2B 2.746(14) 17 ?
Hg1 I1B 2.831(12) . ?
Hg1 I1B 2.831(11) 17 ?
Fe1 N5 2.015(12) 3_565 ?
Fe1 N5 2.015(12) 2_665 ?
Fe1 N5 2.015(11) . ?
Fe1 N1 2.043(14) 2_665 ?
Fe1 N1 2.043(14) 3_565 ?
Fe1 N1 2.043(14) . ?
Fe2 N2 2.178(19) 3_565 ?
Fe2 N2 2.178(18) 2_665 ?
Fe2 N2 2.178(18) . ?
Fe2 O1 2.100(18) 2_665 ?
Fe2 O1 2.100(18) . ?
Fe2 O1 2.100(18) 3_565 ?
N5 N5 1.40(2) 12 ?
N5 C3 1.310(19) . ?
N2 N1 1.35(2) . ?
N2 C2 1.34(3) . ?
N6 N7 1.41(3) . ?
N6 C3 1.340(19) 12 ?
N6 C3 1.340(19) . ?
N3 C1 1.36(2) . ?
N3 C2 1.29(3) . ?
N3 N4 1.36(2) . ?
N1 C1 1.29(2) . ?
N7 H7 0.8202 12 ?
N7 H7 0.8201 . ?
C3 H3 0.9500 . ?
C1 H1 0.9500 . ?
O1 H1AA 0.8406 . ?
O1 H1AB 0.8434 . ?
O1 H1BC 0.8554 . ?
O1 H1BD 0.8638 . ?
C2 H2 0.9500 . ?
N4 H4A 0.8427 . ?
N4 H4B 0.8368 . ?

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
I2A Hg1 I2A 123.1(4) . 17 ?
I2A Hg1 I1B 106.9(4) 17 17 ?
I2A Hg1 I1B 108.1(3) . 17 ?
I1A Hg1 I1A 119.8(3) 17 . ?
I1A Hg1 I1B 9.2(2) 17 17 ?
I1A Hg1 I1B 110.78(14) 17 . ?
I1A Hg1 I1B 9.2(2) . . ?
I1A Hg1 I1B 110.78(14) . 17 ?
I2B Hg1 I1A 103.9(3) . . ?
I2B Hg1 I1A 109.6(3) 17 . ?
I2B Hg1 I2B 110.0(4) 17 . ?
I2B Hg1 I1B 115.4(3) . 17 ?
I2B Hg1 I1B 107.1(3) . . ?
I2B Hg1 I1B 115.4(3) 17 . ?
I2B Hg1 I1B 107.1(3) 17 17 ?
I1B Hg1 I1B 101.9(3) . 17 ?
N5 Fe1 N5 90.5(5) 3_565 2_665 ?
N5 Fe1 N5 90.5(5) 3_565 . ?
N5 Fe1 N5 90.5(5) 2_665 . ?
N5 Fe1 N1 87.0(5) 3_565 2_665 ?
N5 Fe1 N1 177.5(5) 2_665 3_565 ?
N5 Fe1 N1 89.6(5) . . ?
N5 Fe1 N1 87.0(5) 2_665 . ?
N5 Fe1 N1 89.6(5) 2_665 2_665 ?
N5 Fe1 N1 89.6(5) 3_565 3_565 ?
N5 Fe1 N1 87.0(5) . 3_565 ?
N5 Fe1 N1 177.5(5) 3_565 . ?
N5 Fe1 N1 177.5(5) . 2_665 ?
N1 Fe1 N1 92.9(5) 2_665 . ?
N1 Fe1 N1 92.9(5) 3_565 . ?
N1 Fe1 N1 92.9(5) 2_665 3_565 ?
N2 Fe2 N2 88.0(6) 2_665 . ?
N2 Fe2 N2 88.0(6) 3_565 . ?
N2 Fe2 N2 88.0(6) 2_665 3_565 ?
O1 Fe2 N2 88.4(7) 3_565 2_665 ?
O1 Fe2 N2 91.8(6) . 2_665 ?
O1 Fe2 N2 176.4(7) 3_565 3_565 ?
O1 Fe2 N2 88.4(7) 2_665 . ?
O1 Fe2 N2 91.8(6) 2_665 3_565 ?
O1 Fe2 N2 176.4(7) . . ?
O1 Fe2 N2 176.4(7) 2_665 2_665 ?
O1 Fe2 N2 88.4(7) . 3_565 ?
O1 Fe2 N2 91.8(6) 3_565 . ?
O1 Fe2 O1 91.7(7) 3_565 2_665 ?
O1 Fe2 O1 91.7(7) . 2_665 ?
O1 Fe2 O1 91.7(7) . 3_565 ?
N5 N5 Fe1 124.3(4) 12 . ?
C3 N5 Fe1 128.1(10) . . ?
C3 N5 N5 107.1(9) . 12 ?
N1 N2 Fe2 124.8(12) . . ?
C2 N2 Fe2 129.2(14) . . ?
C2 N2 N1 105.3(16) . . ?
C3 N6 N7 126.1(9) 12 . ?
C3 N6 N7 126.1(9) . . ?
C3 N6 C3 107.8(19) . 12 ?
C1 N3 N4 128.8(18) . . ?
C2 N3 C1 104.8(16) . . ?
C2 N3 N4 126.2(18) . . ?
N2 N1 Fe1 124.5(11) . . ?
C1 N1 Fe1 127.8(12) . . ?
C1 N1 N2 107.7(15) . . ?
N6 N7 H7 123.712(8) . 12 ?
N6 N7 H7 123.7 . . ?
H7 N7 H7 112.6 . 12 ?
N5 C3 N6 109.0(14) . . ?
N5 C3 H3 125.5 . . ?
N6 C3 H3 125.5 . . ?
N3 C1 H1 124.9 . . ?
N1 C1 N3 110.2(16) . . ?
N1 C1 H1 124.9 . . ?
Fe2 O1 H1AA 129.9 . . ?
Fe2 O1 H1AB 121.1 . . ?
H1AA O1 H1AB 103.1 . . ?
H1BC O1 H1BD 113.0 . . ?
N2 C2 H2 124.1 . . ?
N3 C2 N2 111.8(18) . . ?
N3 C2 H2 124.1 . . ?
N3 N4 H4A 141.2 . . ?
N3 N4 H4B 101.5 . . ?
H4A N4 H4B 101.0 . . ?

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
N7 H7 N4 0.82 2.23 3.00(2) 155.9 30_455 yes
O1 H1AA I2A 0.84 2.99 3.55(2) 125.5 18 yes
O1 H1BC N2 0.86 2.24 3.07(2) 163.2 2_665 yes
O1 H1BD O1 0.86 2.20 3.01(3) 158.2 2_665 yes
O1 H1BD O1 0.86 2.32 2.80(3) 115.4 27_556 yes
N4 H4A I2A 0.84 2.86 3.61(2) 149.9 19_666 yes
N4 H4B I2B 0.84 2.63 3.38(3) 149.6 2_665 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N5 C3 N6 172.1(8) . . . . ?
Fe1 N1 C1 N3 176.8(11) . . . . ?
Fe2 N2 N1 Fe1 10(2) . . . . ?
Fe2 N2 N1 C1 -171.7(12) . . . . ?
Fe2 N2 C2 N3 172.8(13) . . . . ?
N5 N5 C3 N6 -0.2(18) 12 . . . ?
N2 N1 C1 N3 -1.4(19) . . . . ?
N1 N2 C2 N3 2(2) . . . . ?
N7 N6 C3 N5 -179.9(7) . . . . ?
C3 N6 C3 N5 0.1(7) 12 . . . ?
C1 N3 C2 N2 -3(2) . . . . ?
C2 N2 N1 Fe1 -178.5(13) . . . . ?
C2 N2 N1 C1 0(2) . . . . ?
C2 N3 C1 N1 2(2) . . . . ?
N4 N3 C1 N1 179.4(19) . . . . ?
N4 N3 C2 N2 -179.7(19) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
