# 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_diwu_sq
_database_code_depnum_ccdc_archive 'CCDC 1961426'
loop_
_audit_author_name
_audit_author_address
'Xia Wang'
;soochow university
China
;
_audit_update_record             
;
2019-11-11 deposited with the CCDC.	2019-11-15 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         '3(C14 H6 In N2 O8), C4 H9 N, 3(H) [+ solvent]'
_chemical_formula_sum            'C46 H30 In3 N7 O24'
_chemical_formula_weight         1409.23

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'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                   15.7163(18)
_cell_length_b                   15.7163(18)
_cell_length_c                   52.205(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11167(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3986
_cell_measurement_theta_min      2.332
_cell_measurement_theta_max      24.995

_exptl_crystal_description       BULK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_meas      1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_F_000             4164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.986
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            92993
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.1554
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_theta_min         2.162
_diffrn_reflns_theta_max         27.758
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2942
_reflns_number_gt                1964
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0792P)²+30.9202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2942
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1368
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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
In1 In 0.19993(3) 0.86659(3) 0.083333 0.0382(2) Uani 1 2 d S T P . .
N1 N 0.3389(3) 0.9061(3) 0.10573(8) 0.0430(10) Uani 1 1 d . . . . .
C3 C 0.3478(4) 0.9508(4) 0.12810(10) 0.0459(13) Uani 1 1 d . . . . .
C4 C 0.4061(3) 0.8806(4) 0.09955(10) 0.0453(12) Uani 1 1 d . . . . .
H4 H 0.400721 0.850535 0.083826 0.054 Uiso 1 1 calc R U . . .
C6 C 0.4213(5) 0.9698(5) 0.14526(12) 0.0641(16) Uani 1 1 d . . . . .
H6 H 0.425458 1.000357 0.160841 0.077 Uiso 1 1 calc R U . . .
C7 C 0.4902(5) 0.9414(5) 0.13843(13) 0.0673(17) Uani 1 1 d . . . . .
H7 H 0.540954 0.952805 0.149593 0.081 Uiso 1 1 calc R U . . .
C2 C 0.4823(4) 0.8971(4) 0.11545(10) 0.0467(13) Uani 1 1 d . . . . .
C5 C 0.2689(4) 0.9776(4) 0.13341(11) 0.0499(13) Uani 1 1 d . . . . .
O1 O 0.2064(3) 0.9584(3) 0.11608(7) 0.0491(9) Uani 1 1 d . . . . .
O2 O 0.2717(4) 1.0159(4) 0.15419(8) 0.0825(15) Uani 1 1 d . . . . .
C8 C 0.5547(4) 0.8663(4) 0.10804(12) 0.0491(13) Uani 1 1 d . . . . .
O3 O 0.5482(3) 0.8332(3) 0.08567(8) 0.0582(10) Uani 1 1 d . . . . .
O4 O 0.6179(3) 0.8740(4) 0.12280(10) 0.0763(13) Uani 1 1 d . . . . .
C102 C 0.333333 0.666667 0.0460(5) 0.087(7) Uiso 0.5 3 d S . P . .
H10A H 0.280047 0.605571 0.052113 0.130 Uiso 0.1667 1 calc R U P . .
H10B H 0.394429 0.674476 0.052113 0.130 Uiso 0.1667 1 calc R U P . .
H10C H 0.325524 0.719953 0.052113 0.130 Uiso 0.1667 1 calc R U P . .
N2 N 0.333333 0.666667 0.0177(7) 0.167(13) Uiso 0.5 3 d S . P . .
C101 C 0.429(3) 0.776(3) 0.0083(7) 0.267(18) Uiso 0.5 1 d . . P . .
H10D H 0.431707 0.779456 -0.010021 0.401 Uiso 0.5 1 calc R U P . .
H10E H 0.420170 0.828469 0.014893 0.401 Uiso 0.5 1 calc R U P . .
H10F H 0.489075 0.782992 0.014893 0.401 Uiso 0.5 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
In1 O3 2.173(4) 17_564 ?
In1 O3 2.173(4) 2_665 ?
In1 O1 2.207(4) . ?
In1 O1 2.207(4) 16_454 ?
In1 N1 2.273(4) 16_454 ?
In1 N1 2.273(4) . ?
N1 C3 1.334(7) . ?
N1 C4 1.343(6) . ?
C3 C6 1.372(8) . ?
C3 C5 1.520(7) . ?
C4 C2 1.372(7) . ?
C6 C7 1.409(8) . ?
C7 C2 1.361(8) . ?
C2 C8 1.491(7) . ?
C5 O2 1.231(6) . ?
C5 O1 1.257(6) . ?
C8 O4 1.215(7) . ?
C8 O3 1.262(7) . ?
C102 N2 1.48(4) . ?
N2 C101 1.69(4) . ?
N2 C101 1.70(4) 2_665 ?
N2 C101 1.70(4) 3_565 ?

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
O3 In1 O3 96.2(2) 17_564 2_665 ?
O3 In1 O1 83.49(15) 17_564 . ?
O3 In1 O1 125.53(15) 2_665 . ?
O3 In1 O1 125.52(15) 17_564 16_454 ?
O3 In1 O1 83.48(15) 2_665 16_454 ?
O1 In1 O1 139.0(2) . 16_454 ?
O3 In1 N1 86.65(15) 17_564 16_454 ?
O3 In1 N1 152.01(16) 2_665 16_454 ?
O1 In1 N1 82.46(14) . 16_454 ?
O1 In1 N1 72.50(13) 16_454 16_454 ?
O3 In1 N1 152.01(16) 17_564 . ?
O3 In1 N1 86.65(15) 2_665 . ?
O1 In1 N1 72.50(13) . . ?
O1 In1 N1 82.46(14) 16_454 . ?
N1 In1 N1 103.8(2) 16_454 . ?
C3 N1 C4 118.5(4) . . ?
C3 N1 In1 115.3(3) . . ?
C4 N1 In1 125.9(3) . . ?
N1 C3 C6 122.7(5) . . ?
N1 C3 C5 114.9(5) . . ?
C6 C3 C5 122.4(5) . . ?
N1 C4 C2 122.8(5) . . ?
C3 C6 C7 117.6(6) . . ?
C2 C7 C6 119.9(5) . . ?
C7 C2 C4 118.5(5) . . ?
C7 C2 C8 120.3(5) . . ?
C4 C2 C8 121.2(5) . . ?
O2 C5 O1 125.7(5) . . ?
O2 C5 C3 117.5(5) . . ?
O1 C5 C3 116.8(5) . . ?
C5 O1 In1 119.2(3) . . ?
O4 C8 O3 121.4(5) . . ?
O4 C8 C2 121.4(6) . . ?
O3 C8 C2 117.2(5) . . ?
C8 O3 In1 104.4(3) . 3_565 ?
C102 N2 C101 106.7(19) . . ?
C102 N2 C101 106.7(19) . 2_665 ?
C101 N2 C101 112.1(17) . 2_665 ?
C102 N2 C101 106.7(19) . 3_565 ?
C101 N2 C101 112.1(17) . 3_565 ?
C101 N2 C101 112.1(17) 2_665 3_565 ?

_refine_diff_density_max         0.738
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.098



# SQUEEZE RESULTS (Version =  91117)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 115 24 ' '
2 -0.333 0.333 0.083 521 173 ' '
3 0.000 0.000 0.250 520 173 ' '
4 0.000 0.000 0.500 115 24 ' '
5 0.333 0.667 0.417 521 173 ' '
6 -0.333 0.333 0.583 521 173 ' '
7 0.000 1.000 0.750 519 173 ' '
8 0.333 0.667 0.917 521 173 ' '
9 0.333 0.667 0.167 111 23 ' '
10 0.333 0.667 0.667 111 23 ' '
11 0.667 0.333 0.333 111 23 ' '
12 0.667 0.333 0.833 111 23 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          As
