# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2092836'
loop_
_audit_author_name
_audit_author_address
'Anirban Karmakar'
;Instituto Superior Tecnico
Portugal
;
_audit_update_record             
;
2021-06-28 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H23 Cd N3 O10'
_chemical_formula_weight         529.77

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   34.5866(14)
_cell_length_b                   10.3057(4)
_cell_length_c                   12.0934(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.5550(10)
_cell_angle_gamma                90
_cell_volume                     4109.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9593
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      26.39

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.122
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31972
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.070
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4194
_reflns_number_gt                3627
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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)+(0.0559P)²+10.4782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4194
_refine_ls_number_parameters     297
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001

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
O4 O 0.33061(9) 0.2184(2) 0.7306(2) 0.0531(7) Uani 1 1 d . . . . .
Cd1 Cd 0.31013(2) 1.06187(2) 0.59236(2) 0.03534(11) Uani 1 1 d . . . . .
O10 O 0.24602(9) 1.0500(3) 0.6234(3) 0.0540(7) Uani 1 1 d D . . . .
O12 O 0.23062(11) 0.2178(4) 0.1436(3) 0.0744(9) Uani 1 1 d D . . . .
O2 O 0.33047(8) 0.9092(2) 0.7372(2) 0.0450(6) Uani 1 1 d . . . . .
O1 O 0.31436(9) 0.8157(2) 0.5693(2) 0.0530(7) Uani 1 1 d . . . . .
N1 N 0.39334(10) 0.5674(3) 1.0272(3) 0.0448(7) Uani 1 1 d . . . . .
N2 N 0.40908(9) 0.4628(3) 1.0827(3) 0.0449(7) Uani 1 1 d . . . . .
O5 O 0.46617(14) 0.3309(4) 1.3454(3) 0.1049(14) Uani 1 1 d . . . . .
O3 O 0.30756(9) 0.3193(3) 0.5630(2) 0.0591(7) Uani 1 1 d . . . . .
C7 C 0.36980(10) 0.5622(3) 0.9088(3) 0.0365(7) Uani 1 1 d . . . . .
O6 O 0.43067(15) 0.6928(4) 1.2131(3) 0.1022(14) Uani 1 1 d . . . . .
O9 O 0.37342(9) 1.0674(3) 0.5601(3) 0.0524(7) Uani 1 1 d . . . . .
O11 O 0.27870(11) 1.0664(3) 0.3985(3) 0.0663(9) Uani 1 1 d D . . . .
C1 C 0.32662(10) 0.8093(3) 0.6755(3) 0.0376(7) Uani 1 1 d . . . . .
C2 C 0.33700(9) 0.6803(3) 0.7349(3) 0.0334(6) Uani 1 1 d . . . . .
C8 C 0.35826(10) 0.6786(3) 0.8521(3) 0.0365(7) Uani 1 1 d . . . . .
H8 H 0.3648 0.7562 0.8926 0.044 Uiso 1 1 calc R U . . .
C11 C 0.43184(12) 0.4663(4) 1.1923(3) 0.0503(9) Uani 1 1 d . . . . .
C12 C 0.44294(18) 0.5852(5) 1.2597(4) 0.0726(14) Uani 1 1 d . . . . .
C13 C 0.4735(2) 0.5916(8) 1.3810(5) 0.105(2) Uani 1 1 d . . . . .
H13A H 0.4831 0.6791 1.3973 0.158 Uiso 1 1 calc R U . . .
H13B H 0.4960 0.5354 1.3846 0.158 Uiso 1 1 calc R U . . .
H13C H 0.4606 0.5644 1.4372 0.158 Uiso 1 1 calc R U . . .
C10 C 0.44644(13) 0.3411(5) 1.2442(4) 0.0629(11) Uani 1 1 d . . . . .
C9 C 0.43696(18) 0.2243(5) 1.1695(5) 0.0885(17) Uani 1 1 d . . . . .
H9A H 0.4511 0.1509 1.2116 0.133 Uiso 1 1 calc R U . . .
H9B H 0.4453 0.2381 1.1015 0.133 Uiso 1 1 calc R U . . .
H9C H 0.4083 0.2082 1.1469 0.133 Uiso 1 1 calc R U . . .
C6 C 0.35863(10) 0.4453(3) 0.8507(3) 0.0359(7) Uani 1 1 d . . . . .
H6 H 0.3657 0.3669 0.8895 0.043 Uiso 1 1 calc R U . . .
C4 C 0.33662(10) 0.4471(3) 0.7332(3) 0.0340(7) Uani 1 1 d . . . . .
C3 C 0.32652(10) 0.5643(3) 0.6753(3) 0.0338(7) Uani 1 1 d . . . . .
H3 H 0.3127 0.5650 0.5963 0.041 Uiso 1 1 calc R U . . .
C5 C 0.32409(9) 0.3202(3) 0.6701(3) 0.0360(7) Uani 1 1 d . . . . .
C14 C 0.38125(13) 0.9997(4) 0.4858(4) 0.0565(10) Uani 1 1 d . . . . .
H14 H 0.3614 0.9426 0.4438 0.068 Uiso 1 1 calc R U . . .
N3 N 0.41639(12) 1.0035(4) 0.4620(4) 0.0650(9) Uani 1 1 d . . . . .
C16 C 0.4220(2) 0.9249(6) 0.3698(5) 0.0902(18) Uani 1 1 d . . . . .
H16A H 0.3971 0.8804 0.3315 0.135 Uiso 1 1 calc R U . . .
H16B H 0.4430 0.8625 0.4012 0.135 Uiso 1 1 calc R U . . .
H16C H 0.4294 0.9792 0.3150 0.135 Uiso 1 1 calc R U . . .
C15 C 0.44907(18) 1.0879(6) 0.5267(6) 0.0925(18) Uani 1 1 d . . . . .
H15A H 0.4403 1.1372 0.5821 0.139 Uiso 1 1 calc R U . . .
H15B H 0.4563 1.1460 0.4741 0.139 Uiso 1 1 calc R U . . .
H15C H 0.4722 1.0363 0.5665 0.139 Uiso 1 1 calc R U . . .
H1N H 0.4021(11) 0.637(4) 1.071(3) 0.043(10) Uiso 1 1 d . . . . .
H11B H 0.2926(14) 1.073(4) 0.345(3) 0.065 Uiso 1 1 d D U . . .
H11A H 0.2622(12) 1.136(3) 0.375(4) 0.065 Uiso 1 1 d D U . . .
H10A H 0.2285(12) 1.093(4) 0.568(3) 0.065 Uiso 1 1 d D U . . .
H10B H 0.2403(15) 0.968(2) 0.640(4) 0.065 Uiso 1 1 d D U . . .
H12A H 0.2146(12) 0.258(4) 0.178(4) 0.065 Uiso 1 1 d D U . . .
H12B H 0.2199(13) 0.253(4) 0.075(2) 0.065 Uiso 1 1 d D 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
O4 C5 1.260(4) . ?
O4 Cd1 2.277(2) 1_545 ?
Cd1 O11 2.268(3) . ?
Cd1 O4 2.277(2) 1_565 ?
Cd1 O2 2.301(2) . ?
Cd1 O9 2.337(3) . ?
Cd1 O10 2.361(3) . ?
Cd1 O1 2.561(3) . ?
O10 H10A 0.870(19) . ?
O10 H10B 0.903(19) . ?
O12 H12A 0.888(19) . ?
O12 H12B 0.884(19) . ?
O2 C1 1.255(4) . ?
O1 C1 1.227(4) . ?
N1 N2 1.299(4) . ?
N1 C7 1.419(4) . ?
N1 H1N 0.89(4) . ?
N2 C11 1.322(5) . ?
O5 C10 1.213(5) . ?
O3 C5 1.248(4) . ?
C7 C8 1.380(4) . ?
C7 C6 1.390(4) . ?
O6 C12 1.258(6) . ?
O9 C14 1.230(5) . ?
O11 H11B 0.922(19) . ?
O11 H11A 0.908(19) . ?
C1 C2 1.503(4) . ?
C2 C8 1.385(4) . ?
C2 C3 1.387(4) . ?
C8 H8 0.9300 . ?
C11 C10 1.456(6) . ?
C11 C12 1.458(7) . ?
C12 C13 1.529(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C10 C9 1.481(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C6 C4 1.394(5) . ?
C6 H6 0.9300 . ?
C4 C3 1.387(4) . ?
C4 C5 1.511(4) . ?
C3 H3 0.9300 . ?
C14 N3 1.332(6) . ?
C14 H14 0.9300 . ?
N3 C16 1.438(7) . ?
N3 C15 1.454(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?

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
C5 O4 Cd1 101.7(2) . 1_545 ?
O11 Cd1 O4 133.66(11) . 1_565 ?
O11 Cd1 O2 137.92(11) . . ?
O4 Cd1 O2 88.26(9) 1_565 . ?
O11 Cd1 O9 90.47(12) . . ?
O4 Cd1 O9 90.32(11) 1_565 . ?
O2 Cd1 O9 93.27(10) . . ?
O11 Cd1 O10 89.15(12) . . ?
O4 Cd1 O10 91.10(11) 1_565 . ?
O2 Cd1 O10 85.95(10) . . ?
O9 Cd1 O10 178.37(10) . . ?
O11 Cd1 O1 86.16(10) . . ?
O4 Cd1 O1 140.04(8) 1_565 . ?
O2 Cd1 O1 52.51(8) . . ?
O9 Cd1 O1 85.34(10) . . ?
O10 Cd1 O1 93.05(10) . . ?
Cd1 O10 H10A 109(3) . . ?
Cd1 O10 H10B 111(3) . . ?
H10A O10 H10B 119(5) . . ?
H12A O12 H12B 96(4) . . ?
C1 O2 Cd1 98.9(2) . . ?
C1 O1 Cd1 87.3(2) . . ?
N2 N1 C7 120.9(3) . . ?
N2 N1 H1N 110(3) . . ?
C7 N1 H1N 128(3) . . ?
N1 N2 C11 121.7(3) . . ?
C8 C7 C6 120.5(3) . . ?
C8 C7 N1 117.5(3) . . ?
C6 C7 N1 122.0(3) . . ?
C14 O9 Cd1 122.1(3) . . ?
Cd1 O11 H11B 123(3) . . ?
Cd1 O11 H11A 113(3) . . ?
H11B O11 H11A 98(4) . . ?
O1 C1 O2 121.3(3) . . ?
O1 C1 C2 120.4(3) . . ?
O2 C1 C2 118.3(3) . . ?
C8 C2 C3 119.7(3) . . ?
C8 C2 C1 118.5(3) . . ?
C3 C2 C1 121.8(3) . . ?
C7 C8 C2 120.3(3) . . ?
C7 C8 H8 119.9 . . ?
C2 C8 H8 119.9 . . ?
N2 C11 C10 115.6(4) . . ?
N2 C11 C12 124.1(4) . . ?
C10 C11 C12 120.3(4) . . ?
O6 C12 C11 119.6(4) . . ?
O6 C12 C13 115.7(5) . . ?
C11 C12 C13 124.2(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C10 C11 121.9(5) . . ?
O5 C10 C9 119.9(5) . . ?
C11 C10 C9 118.2(4) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C6 C4 119.1(3) . . ?
C7 C6 H6 120.4 . . ?
C4 C6 H6 120.4 . . ?
C3 C4 C6 120.2(3) . . ?
C3 C4 C5 120.5(3) . . ?
C6 C4 C5 119.2(3) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
O3 C5 O4 122.9(3) . . ?
O3 C5 C4 120.2(3) . . ?
O4 C5 C4 117.0(3) . . ?
O9 C14 N3 123.9(4) . . ?
O9 C14 H14 118.0 . . ?
N3 C14 H14 118.0 . . ?
C14 N3 C16 119.7(4) . . ?
C14 N3 C15 120.9(4) . . ?
C16 N3 C15 119.4(5) . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

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
C7 N1 N2 C11 178.5(3) . . . . ?
N2 N1 C7 C8 -172.3(3) . . . . ?
N2 N1 C7 C6 7.5(5) . . . . ?
Cd1 O1 C1 O2 0.7(3) . . . . ?
Cd1 O1 C1 C2 -180.0(3) . . . . ?
Cd1 O2 C1 O1 -0.8(4) . . . . ?
Cd1 O2 C1 C2 179.9(2) . . . . ?
O1 C1 C2 C8 167.1(3) . . . . ?
O2 C1 C2 C8 -13.6(5) . . . . ?
O1 C1 C2 C3 -11.7(5) . . . . ?
O2 C1 C2 C3 167.6(3) . . . . ?
C6 C7 C8 C2 -3.0(5) . . . . ?
N1 C7 C8 C2 176.7(3) . . . . ?
C3 C2 C8 C7 1.4(5) . . . . ?
C1 C2 C8 C7 -177.4(3) . . . . ?
N1 N2 C11 C10 178.2(4) . . . . ?
N1 N2 C11 C12 -2.7(6) . . . . ?
N2 C11 C12 O6 -0.3(9) . . . . ?
C10 C11 C12 O6 178.8(5) . . . . ?
N2 C11 C12 C13 -171.9(5) . . . . ?
C10 C11 C12 C13 7.2(8) . . . . ?
N2 C11 C10 O5 -176.9(5) . . . . ?
C12 C11 C10 O5 4.0(7) . . . . ?
N2 C11 C10 C9 3.7(6) . . . . ?
C12 C11 C10 C9 -175.4(5) . . . . ?
C8 C7 C6 C4 1.9(5) . . . . ?
N1 C7 C6 C4 -177.9(3) . . . . ?
C7 C6 C4 C3 0.8(5) . . . . ?
C7 C6 C4 C5 -179.4(3) . . . . ?
C6 C4 C3 C2 -2.4(5) . . . . ?
C5 C4 C3 C2 177.9(3) . . . . ?
C8 C2 C3 C4 1.2(5) . . . . ?
C1 C2 C3 C4 -180.0(3) . . . . ?
Cd1 O4 C5 O3 4.5(4) 1_545 . . . ?
Cd1 O4 C5 C4 -176.5(2) 1_545 . . . ?
C3 C4 C5 O3 6.1(5) . . . . ?
C6 C4 C5 O3 -173.7(3) . . . . ?
C3 C4 C5 O4 -172.9(3) . . . . ?
C6 C4 C5 O4 7.4(5) . . . . ?
Cd1 O9 C14 N3 177.5(3) . . . . ?
O9 C14 N3 C16 -177.1(5) . . . . ?
O9 C14 N3 C15 1.8(7) . . . . ?

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
C16 H16A O4 0.96 2.48 3.433(7) 175.8 6_565
C15 H15A O6 0.96 2.45 3.385(8) 164.2 6_575
C15 H15B O5 0.96 2.55 3.494(8) 168.8 1_564
N1 H1N O6 0.89(4) 1.79(4) 2.576(5) 145(4) .
O11 H11B O2 0.922(19) 2.11(2) 3.030(4) 173(5) 6_575
O10 H10A O3 0.870(19) 1.93(2) 2.795(4) 175(5) 7_566
O10 H10B O12 0.903(19) 1.95(2) 2.835(5) 168(5) 6_566
O12 H12A O4 0.888(19) 2.19(3) 3.030(4) 158(4) 7_556
O12 H12B O1 0.884(19) 1.90(2) 2.766(4) 167(4) 4_545

_refine_diff_density_max         1.039
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.115

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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 2092837'
loop_
_audit_author_name
_audit_author_address
'Anirban Karmakar'
;Instituto Superior Tecnico
Portugal
;
_audit_update_record             
;
2021-06-28 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H3 Cd I3 N4 O7'
_chemical_formula_weight         808.28

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'
Cd Cd -0.8075 1.2024 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.2124(9)
_cell_length_b                   29.969(3)
_cell_length_c                   11.2765(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.977(4)
_cell_angle_gamma                90
_cell_volume                     2887.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.992
_shelx_estimated_absorpt_T_min   0.460
_shelx_estimated_absorpt_T_max   0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40420
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.384
_diffrn_reflns_theta_max         28.409
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             7087
_reflns_number_gt                5852
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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)+56.8475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7087
_refine_ls_number_parameters     254
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.063
_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
Cd1 Cd 1.16126(6) 0.32509(2) 0.85250(6) 0.02673(14) Uani 1 1 d . . . . .
I2 I 0.70060(7) 0.38972(2) 0.90816(6) 0.04067(16) Uani 1 1 d . . . . .
I3 I 0.10622(6) 0.29503(2) 0.56851(6) 0.04291(17) Uani 1 1 d . . . . .
O7 O 0.1722(8) 0.39317(18) 0.9400(6) 0.0358(14) Uani 1 1 d . . . . .
O2 O 0.9329(8) 0.2983(2) 0.8597(8) 0.056(2) Uani 1 1 d . . . . .
N1 N 0.3243(8) 0.3633(2) 0.7747(7) 0.0295(14) Uani 1 1 d . . . . .
O3 O 0.3333(8) 0.2017(2) 0.5484(7) 0.0531(19) Uani 1 1 d . . . . .
O1 O 0.8975(7) 0.3480(3) 0.7110(7) 0.0486(17) Uani 1 1 d . . . . .
C8 C 0.5817(8) 0.3425(2) 0.7695(7) 0.0232(14) Uani 1 1 d . . . . .
O4 O 0.2996(9) 0.2454(2) 0.3867(7) 0.0522(18) Uani 1 1 d . . . . .
C6 C 0.3480(8) 0.3032(2) 0.6376(8) 0.0245(15) Uani 1 1 d . . . . .
N4 N 0.1220(9) 0.4659(2) 0.9252(8) 0.0415(19) Uani 1 1 d . . . . .
H4 H 0.0774 0.4618 0.9790 0.050 Uiso 1 1 calc R U . . .
N2 N 0.3327(9) 0.4049(2) 0.7553(8) 0.0374(17) Uani 1 1 d . . . . .
C2 C 0.6706(8) 0.3144(3) 0.7229(9) 0.0313(18) Uani 1 1 d . . . . .
C7 C 0.4166(8) 0.3380(2) 0.7238(7) 0.0223(14) Uani 1 1 d . . . . .
O6 O 0.0652(9) 0.5398(2) 0.9181(8) 0.0527(19) Uani 1 1 d . . . . .
C4 C 0.4355(8) 0.2746(3) 0.5925(9) 0.0326(19) Uani 1 1 d . . . . .
C3 C 0.5949(10) 0.2808(3) 0.6359(11) 0.045(2) Uani 1 1 d . . . . .
C9 C 0.2599(11) 0.4361(3) 0.8022(10) 0.042(2) Uani 1 1 d . . . . .
C10 C 0.1833(10) 0.4286(3) 0.8888(8) 0.0306(17) Uani 1 1 d . . . . .
C1 C 0.8457(8) 0.3213(3) 0.7687(9) 0.034(2) Uani 1 1 d . . . . .
C5 C 0.3537(9) 0.2377(3) 0.5009(10) 0.037(2) Uani 1 1 d . . . . .
N3 N 0.2004(14) 0.5140(3) 0.8044(11) 0.069(3) Uani 1 1 d . . . . .
H3 H 0.2066 0.5407 0.7789 0.083 Uiso 1 1 calc R U . . .
C11 C 0.1252(13) 0.5087(3) 0.8838(11) 0.047(3) Uani 1 1 d . . . . .
C12 C 0.2696(18) 0.4805(3) 0.7588(15) 0.074(4) Uani 1 1 d . . . . .
I1A I 0.7336(3) 0.23251(19) 0.5932(10) 0.0577(15) Uani 0.467(16) 1 d . . P A 1
I1B I 0.7165(4) 0.2479(3) 0.5284(10) 0.067(2) Uani 0.533(16) 1 d . . P A 2
O5 O 0.3385(14) 0.4918(4) 0.6854(11) 0.102(4) Uani 1 1 d . U . . .
H5O H 0.3843 0.4690 0.6707 0.152 Uiso 1 1 d 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
Cd1 O7 2.252(6) 1_655 ?
Cd1 O2 2.281(7) . ?
Cd1 N1 2.308(7) 1_655 ?
Cd1 O3 2.326(7) 4_666 ?
Cd1 O4 2.421(7) 4_666 ?
Cd1 O1 2.454(7) . ?
Cd1 C5 2.696(8) 4_666 ?
Cd1 C1 2.702(7) . ?
Cd1 I3 3.1794(9) 1_655 ?
I2 C8 2.090(7) . ?
I3 C6 2.081(7) . ?
I3 Cd1 3.1794(9) 1_455 ?
O7 C10 1.232(10) . ?
O7 Cd1 2.252(6) 1_455 ?
O2 C1 1.248(12) . ?
N1 N2 1.271(9) . ?
N1 C7 1.412(9) . ?
N1 Cd1 2.308(6) 1_455 ?
O3 C5 1.252(12) . ?
O3 Cd1 2.327(7) 4_465 ?
O1 C1 1.235(12) . ?
C8 C2 1.407(9) . ?
C8 C7 1.418(9) . ?
O4 C5 1.215(12) . ?
O4 Cd1 2.421(7) 4_465 ?
C6 C4 1.397(10) . ?
C6 C7 1.404(10) . ?
N4 C11 1.369(11) . ?
N4 C10 1.381(10) . ?
N4 H4 0.8600 . ?
N2 C9 1.369(10) . ?
C2 C3 1.396(11) . ?
C2 C1 1.512(10) . ?
O6 C11 1.219(10) . ?
C4 C3 1.376(10) . ?
C4 C5 1.508(11) . ?
C3 I1A 2.102(8) . ?
C3 I1B 2.171(9) . ?
C9 C10 1.420(11) . ?
C9 C12 1.431(13) . ?
C5 Cd1 2.696(8) 4_465 ?
N3 C11 1.331(12) . ?
N3 C12 1.386(12) . ?
N3 H3 0.8600 . ?
C12 O5 1.263(15) . ?
O5 H5O 0.8500 . ?

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
O7 Cd1 O2 101.2(2) 1_655 . ?
O7 Cd1 N1 77.8(2) 1_655 1_655 ?
O2 Cd1 N1 158.2(3) . 1_655 ?
O7 Cd1 O3 89.6(2) 1_655 4_666 ?
O2 Cd1 O3 98.9(3) . 4_666 ?
N1 Cd1 O3 102.9(3) 1_655 4_666 ?
O7 Cd1 O4 141.8(3) 1_655 4_666 ?
O2 Cd1 O4 97.1(3) . 4_666 ?
N1 Cd1 O4 96.6(2) 1_655 4_666 ?
O3 Cd1 O4 54.4(3) 4_666 4_666 ?
O7 Cd1 O1 84.4(2) 1_655 . ?
O2 Cd1 O1 54.5(3) . . ?
N1 Cd1 O1 103.9(2) 1_655 . ?
O3 Cd1 O1 150.5(3) 4_666 . ?
O4 Cd1 O1 133.0(3) 4_666 . ?
O7 Cd1 C5 116.7(3) 1_655 4_666 ?
O2 Cd1 C5 97.6(2) . 4_666 ?
N1 Cd1 C5 102.3(2) 1_655 4_666 ?
O3 Cd1 C5 27.6(3) 4_666 4_666 ?
O4 Cd1 C5 26.8(3) 4_666 4_666 ?
O1 Cd1 C5 149.3(3) . 4_666 ?
O7 Cd1 C1 93.3(2) 1_655 . ?
O2 Cd1 C1 27.4(3) . . ?
N1 Cd1 C1 131.0(3) 1_655 . ?
O3 Cd1 C1 125.4(3) 4_666 . ?
O4 Cd1 C1 116.9(3) 4_666 . ?
O1 Cd1 C1 27.2(3) . . ?
C5 Cd1 C1 124.0(3) 4_666 . ?
O7 Cd1 I3 131.46(15) 1_655 1_655 ?
O2 Cd1 I3 97.7(2) . 1_655 ?
N1 Cd1 I3 68.83(17) 1_655 1_655 ?
O3 Cd1 I3 130.8(2) 4_666 1_655 ?
O4 Cd1 I3 77.86(18) 4_666 1_655 ?
O1 Cd1 I3 71.25(16) . 1_655 ?
C5 Cd1 I3 104.3(2) 4_666 1_655 ?
C1 Cd1 I3 83.73(18) . 1_655 ?
C6 I3 Cd1 81.1(2) . 1_455 ?
C10 O7 Cd1 125.0(5) . 1_455 ?
C1 O2 Cd1 95.4(6) . . ?
N2 N1 C7 111.8(6) . . ?
N2 N1 Cd1 129.9(5) . 1_455 ?
C7 N1 Cd1 117.7(5) . 1_455 ?
C5 O3 Cd1 92.8(6) . 4_465 ?
C1 O1 Cd1 87.7(5) . . ?
C2 C8 C7 120.2(7) . . ?
C2 C8 I2 118.0(5) . . ?
C7 C8 I2 121.8(5) . . ?
C5 O4 Cd1 89.3(6) . 4_465 ?
C4 C6 C7 122.4(6) . . ?
C4 C6 I3 118.3(5) . . ?
C7 C6 I3 119.2(5) . . ?
C11 N4 C10 126.3(7) . . ?
C11 N4 H4 116.8 . . ?
C10 N4 H4 116.8 . . ?
N1 N2 C9 122.2(7) . . ?
C3 C2 C8 119.1(7) . . ?
C3 C2 C1 121.9(6) . . ?
C8 C2 C1 119.1(7) . . ?
C6 C7 N1 119.8(6) . . ?
C6 C7 C8 117.7(6) . . ?
N1 C7 C8 121.9(6) . . ?
C3 C4 C6 118.2(7) . . ?
C3 C4 C5 122.5(7) . . ?
C6 C4 C5 119.4(6) . . ?
C4 C3 C2 122.3(7) . . ?
C4 C3 I1A 119.0(6) . . ?
C2 C3 I1A 118.1(6) . . ?
C4 C3 I1B 116.4(7) . . ?
C2 C3 I1B 119.6(6) . . ?
N2 C9 C10 126.8(8) . . ?
N2 C9 C12 113.6(8) . . ?
C10 C9 C12 119.6(8) . . ?
O7 C10 N4 116.3(7) . . ?
O7 C10 C9 127.5(7) . . ?
N4 C10 C9 116.1(7) . . ?
O1 C1 O2 122.3(7) . . ?
O1 C1 C2 118.9(9) . . ?
O2 C1 C2 118.7(8) . . ?
O1 C1 Cd1 65.1(4) . . ?
O2 C1 Cd1 57.2(4) . . ?
C2 C1 Cd1 174.5(6) . . ?
O4 C5 O3 123.2(8) . . ?
O4 C5 C4 119.3(9) . . ?
O3 C5 C4 117.2(9) . . ?
O4 C5 Cd1 63.9(5) . 4_465 ?
O3 C5 Cd1 59.5(5) . 4_465 ?
C4 C5 Cd1 168.9(5) . 4_465 ?
C11 N3 C12 126.2(8) . . ?
C11 N3 H3 116.9 . . ?
C12 N3 H3 116.9 . . ?
O6 C11 N3 122.3(9) . . ?
O6 C11 N4 122.6(9) . . ?
N3 C11 N4 115.1(8) . . ?
O5 C12 N3 117.6(10) . . ?
O5 C12 C9 125.7(10) . . ?
N3 C12 C9 116.7(8) . . ?
C12 O5 H5O 108.8 . . ?

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
N4 H4 O6 0.86 2.05 2.899(10) 168.1 3_567
N4 H4 O6 0.86 2.05 2.899(10) 168.1 3_567
O5 H5O N2 0.85 2.27 2.727(14) 113.5 .

_refine_diff_density_max         2.030
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.202

_shelxl_version_number           2014/6




####################################################################### 
# 
# 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_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2092845'
loop_
_audit_author_name
_audit_author_address
'Atash Gurbanov'
;Instituto Superior Tecnico
Portugal
;
_audit_update_record             
;
2021-06-28 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H20 Cd I6 N4 O15'
_chemical_formula_weight         1502.26

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'
Cd Cd -0.8075 1.2024 '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'

_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                   8.3320(5)
_cell_length_b                   13.7864(8)
_cell_length_c                   17.0388(11)
_cell_angle_alpha                91.308(2)
_cell_angle_beta                 102.606(3)
_cell_angle_gamma                97.660(2)
_cell_volume                     1890.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      26.41

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.639
_exptl_crystal_F_000             1380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.548
_shelx_estimated_absorpt_T_min   0.362
_shelx_estimated_absorpt_T_max   0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7680
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_v_R_equivalents   ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.453
_diffrn_reflns_theta_max         26.437
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             7680
_reflns_number_gt                7078
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          
;
 Refined as a 2-component 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)+79.8309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7680
_refine_ls_number_parameters     477
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1362
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.065
_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
Cd1 Cd 0.0000 0.0000 0.5000 0.0155(2) Uani 1 2 d S . P . .
I1 I 0.23782(10) 0.33001(6) 0.59799(5) 0.02708(18) Uani 1 1 d . . . . .
I4 I 0.02016(12) 0.02019(5) 0.25195(5) 0.02965(19) Uani 1 1 d . . . . .
Cd2 Cd 0.5000 0.0000 0.5000 0.0189(2) Uani 1 2 d S . P . .
I5 I -0.03207(11) 0.41196(6) 0.40563(5) 0.02912(19) Uani 1 1 d . . . . .
I3 I 0.49649(13) -0.01093(6) 0.77363(6) 0.0380(2) Uani 1 1 d . . . . .
I2 I 0.56434(14) 0.37226(7) 0.95727(5) 0.0422(2) Uani 1 1 d . . . . .
I6 I 0.10813(15) 0.38128(7) 0.07010(6) 0.0453(3) Uani 1 1 d . . . . .
O1 O 0.4457(12) 0.0961(7) 0.5919(6) 0.037(2) Uani 1 1 d . . . . .
O10 O -0.0542(11) 0.1196(7) 0.0613(5) 0.032(2) Uani 1 1 d . . . . .
O2 O 0.1792(10) 0.0790(6) 0.6061(5) 0.0261(18) Uani 1 1 d . . . . .
O7 O 0.0758(10) 0.1306(6) 0.4300(5) 0.0232(17) Uani 1 1 d . . . . .
O13 O 0.2254(10) -0.0825(5) 0.4766(5) 0.0201(16) Uani 1 1 d . . . . .
O14 O 0.4026(12) 0.1182(8) 0.4186(7) 0.045(3) Uani 1 1 d . . . . .
O8 O -0.1766(11) 0.1783(7) 0.3970(6) 0.032(2) Uani 1 1 d . . . . .
N2 N 0.4555(13) 0.4964(7) 0.7337(6) 0.026(2) Uani 1 1 d . . . . .
C8 C 0.3670(13) 0.2756(8) 0.7034(6) 0.017(2) Uani 1 1 d . . . . .
O4 O 0.5541(13) 0.1089(8) 0.9683(6) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.4639(13) 0.1359(7) 0.7730(6) 0.016(2) Uani 1 1 d . U . . .
O5 O 0.3293(14) 0.5779(7) 0.8558(6) 0.043(3) Uani 1 1 d . . . . .
O12 O -0.0675(17) 0.6066(7) 0.1387(6) 0.052(3) Uani 1 1 d . . . . .
N4 N 0.1133(13) 0.5460(7) 0.2834(6) 0.027(2) Uani 1 1 d . . . . .
C1 C 0.3313(15) 0.1111(8) 0.6269(7) 0.020(2) Uani 1 1 d . . . . .
C23 C 0.1767(16) 0.7083(9) 0.3369(8) 0.030(3) Uani 1 1 d . . . . .
N3 N 0.0448(14) 0.4759(7) 0.2287(7) 0.029(2) Uani 1 1 d . . . . .
H3N H -0.0059 0.4912 0.1821 0.035 Uiso 1 1 calc R U . . .
O3 O 0.7751(12) 0.1733(10) 0.9241(6) 0.053(3) Uani 1 1 d . . . . .
C2 C 0.3873(13) 0.1763(7) 0.7029(6) 0.016(2) Uani 1 1 d . . . . .
C6 C 0.4951(15) 0.2925(8) 0.8458(6) 0.022(2) Uani 1 1 d . . . . .
O11 O 0.1573(15) 0.7932(7) 0.3371(7) 0.049(3) Uani 1 1 d . . . . .
O6 O 0.5432(15) 0.7398(8) 0.6941(8) 0.055(3) Uani 1 1 d . U . . .
C19 C 0.0706(15) 0.3185(8) 0.1780(7) 0.020(2) Uani 1 1 d . . . . .
N1 N 0.4005(14) 0.4342(7) 0.7815(6) 0.027(2) Uani 1 1 d . . . . .
H1 H 0.3498 0.4536 0.8166 0.032 Uiso 1 1 calc R U . . .
O9 O 0.2211(11) 0.1488(7) 0.1016(6) 0.037(2) Uani 1 1 d . . . . .
C14 C -0.0349(13) 0.1755(7) 0.3867(6) 0.015(2) Uani 1 1 d . . . . .
C22 C 0.0957(16) 0.6379(8) 0.2686(8) 0.025(3) Uani 1 1 d . . . . .
C4 C 0.5186(14) 0.1942(8) 0.8444(7) 0.021(2) Uani 1 1 d . . . . .
C15 C 0.0123(13) 0.2283(8) 0.3164(6) 0.017(2) Uani 1 1 d . . . . .
C10 C 0.3845(16) 0.6332(9) 0.8106(8) 0.028(3) Uani 1 1 d . . . . .
C21 C 0.0189(15) 0.3300(8) 0.3101(6) 0.022(2) Uani 1 1 d . . . . .
C9 C 0.4494(15) 0.5897(8) 0.7429(7) 0.024(2) Uani 1 1 d . . . . .
C12 C 0.5151(17) 0.6526(10) 0.6840(9) 0.036(3) Uani 1 1 d . . . . .
C18 C 0.0735(15) 0.1558(8) 0.1089(7) 0.023(2) Uani 1 1 d . . . . .
C25 C -0.0055(18) 0.6687(9) 0.1922(9) 0.035(3) Uani 1 1 d . . . . .
C16 C 0.0340(14) 0.1734(7) 0.2505(6) 0.018(2) Uani 1 1 d . U . . .
C20 C 0.0509(15) 0.3768(8) 0.2430(7) 0.023(2) Uani 1 1 d . . . . .
C17 C 0.0614(13) 0.2178(7) 0.1802(6) 0.016(2) Uani 1 1 d . . . . .
C13 C 0.543(2) 0.6012(12) 0.6101(9) 0.046(4) Uani 1 1 d . . . . .
H13A H 0.4423 0.5606 0.5834 0.070 Uiso 1 1 calc R U . . .
H13B H 0.6295 0.5613 0.6257 0.070 Uiso 1 1 calc R U . . .
H13C H 0.5750 0.6491 0.5743 0.070 Uiso 1 1 calc R U . . .
C7 C 0.4242(15) 0.3348(7) 0.7758(7) 0.021(2) Uani 1 1 d . . . . .
C24 C 0.280(2) 0.6706(11) 0.4113(10) 0.051(4) Uani 1 1 d . . . . .
H24A H 0.3453 0.7249 0.4449 0.077 Uiso 1 1 calc R U . . .
H24B H 0.3515 0.6285 0.3957 0.077 Uiso 1 1 calc R U . . .
H24C H 0.2074 0.6344 0.4406 0.077 Uiso 1 1 calc R U . . .
C26 C -0.040(2) 0.7733(10) 0.1827(10) 0.047(4) Uani 1 1 d . . . . .
H26A H -0.1104 0.7785 0.1308 0.070 Uiso 1 1 calc R U . . .
H26B H 0.0633 0.8159 0.1873 0.070 Uiso 1 1 calc R U . . .
H26C H -0.0935 0.7918 0.2240 0.070 Uiso 1 1 calc R U . . .
C5 C 0.6142(15) 0.1528(9) 0.9184(7) 0.025(2) Uani 1 1 d . . . . .
C11 C 0.3817(19) 0.7386(9) 0.8194(10) 0.041(3) Uani 1 1 d . . . . .
H11A H 0.3147 0.7511 0.8567 0.062 Uiso 1 1 calc R U . . .
H11B H 0.3357 0.7624 0.7680 0.062 Uiso 1 1 calc R U . . .
H11C H 0.4928 0.7714 0.8392 0.062 Uiso 1 1 calc R U . . .
O32 O 0.2278(13) 0.0721(8) -0.0309(7) 0.047(3) Uani 1 1 d . . . . .
H32A H 0.2203 0.0973 0.0140 0.070 Uiso 1 1 d R U . . .
H32B H 0.3294 0.0819 -0.0333 0.070 Uiso 1 1 d R U . . .
H10O H -0.0775 0.0595 0.0719 0.070 Uiso 1 1 d R U . . .
H3O H 0.8290 0.1551 0.9689 0.070 Uiso 1 1 d R U . . .
H13O H 0.2082 -0.1161 0.5163 0.070 Uiso 1 1 d R U . . .
H14O H 0.2035 -0.1226 0.4353 0.070 Uiso 1 1 d 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
Cd1 O2 2.233(8) 2_556 ?
Cd1 O2 2.233(8) . ?
Cd1 O7 2.278(7) . ?
Cd1 O7 2.278(7) 2_556 ?
Cd1 O13 2.420(7) . ?
Cd1 O13 2.420(7) 2_556 ?
I1 C8 2.093(10) . ?
I4 C16 2.101(10) . ?
Cd2 O1 2.188(8) 2_656 ?
Cd2 O1 2.188(9) . ?
Cd2 O14 2.281(10) 2_656 ?
Cd2 O14 2.281(10) . ?
Cd2 O13 2.361(8) . ?
Cd2 O13 2.361(8) 2_656 ?
I5 C21 2.110(11) . ?
I3 C3 2.078(10) . ?
I2 C6 2.099(10) . ?
I6 C19 2.116(10) . ?
O1 C1 1.265(14) . ?
O10 C18 1.225(15) . ?
O10 H10O 0.8574 . ?
O2 C1 1.255(14) . ?
O7 C14 1.287(13) . ?
O13 H13O 0.8560 . ?
O13 H14O 0.8562 . ?
O8 C14 1.236(14) . ?
N2 C9 1.301(15) . ?
N2 N1 1.303(14) . ?
C8 C2 1.402(14) . ?
C8 C7 1.417(15) . ?
O4 C5 1.212(15) . ?
C3 C2 1.391(14) . ?
C3 C4 1.396(15) . ?
O5 C10 1.214(16) . ?
O12 C25 1.213(17) . ?
N4 N3 1.307(14) . ?
N4 C22 1.318(15) . ?
C1 C2 1.508(14) . ?
C23 O11 1.202(16) . ?
C23 C22 1.477(18) . ?
C23 C24 1.51(2) . ?
N3 C20 1.398(14) . ?
N3 H3N 0.8600 . ?
O3 C5 1.315(15) . ?
O3 H3O 0.8593 . ?
C6 C7 1.389(16) . ?
C6 C4 1.396(15) . ?
O6 C12 1.195(17) . ?
C19 C17 1.382(14) . ?
C19 C20 1.404(15) . ?
N1 C7 1.414(14) . ?
N1 H1 0.8600 . ?
O9 C18 1.279(15) . ?
C14 C15 1.511(13) . ?
C22 C25 1.492(19) . ?
C4 C5 1.505(15) . ?
C15 C16 1.397(15) . ?
C15 C21 1.405(15) . ?
C10 C11 1.460(17) . ?
C10 C9 1.521(18) . ?
C21 C20 1.384(16) . ?
C9 C12 1.487(17) . ?
C12 C13 1.51(2) . ?
C18 C17 1.499(15) . ?
C25 C26 1.512(17) . ?
C16 C17 1.406(14) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
O32 H32A 0.8499 . ?
O32 H32B 0.8500 . ?

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
O2 Cd1 O2 180.0(3) 2_556 . ?
O2 Cd1 O7 94.4(3) 2_556 . ?
O2 Cd1 O7 85.6(3) . . ?
O2 Cd1 O7 85.6(3) 2_556 2_556 ?
O2 Cd1 O7 94.4(3) . 2_556 ?
O7 Cd1 O7 180.0 . 2_556 ?
O2 Cd1 O13 92.6(3) 2_556 . ?
O2 Cd1 O13 87.4(3) . . ?
O7 Cd1 O13 92.2(3) . . ?
O7 Cd1 O13 87.8(3) 2_556 . ?
O2 Cd1 O13 87.4(3) 2_556 2_556 ?
O2 Cd1 O13 92.6(3) . 2_556 ?
O7 Cd1 O13 87.8(3) . 2_556 ?
O7 Cd1 O13 92.2(3) 2_556 2_556 ?
O13 Cd1 O13 180.0 . 2_556 ?
O1 Cd2 O1 180.0 2_656 . ?
O1 Cd2 O14 81.7(4) 2_656 2_656 ?
O1 Cd2 O14 98.3(4) . 2_656 ?
O1 Cd2 O14 98.3(4) 2_656 . ?
O1 Cd2 O14 81.7(4) . . ?
O14 Cd2 O14 180.0 2_656 . ?
O1 Cd2 O13 90.4(3) 2_656 . ?
O1 Cd2 O13 89.6(3) . . ?
O14 Cd2 O13 91.6(3) 2_656 . ?
O14 Cd2 O13 88.4(3) . . ?
O1 Cd2 O13 89.6(3) 2_656 2_656 ?
O1 Cd2 O13 90.4(3) . 2_656 ?
O14 Cd2 O13 88.4(3) 2_656 2_656 ?
O14 Cd2 O13 91.6(3) . 2_656 ?
O13 Cd2 O13 180.0 . 2_656 ?
C1 O1 Cd2 141.9(8) . . ?
C18 O10 H10O 108.7 . . ?
C1 O2 Cd1 138.5(7) . . ?
C14 O7 Cd1 120.6(7) . . ?
Cd2 O13 Cd1 121.2(3) . . ?
Cd2 O13 H13O 112.1 . . ?
Cd1 O13 H13O 84.6 . . ?
Cd2 O13 H14O 111.5 . . ?
Cd1 O13 H14O 116.6 . . ?
H13O O13 H14O 106.6 . . ?
C9 N2 N1 121.1(11) . . ?
C2 C8 C7 119.7(9) . . ?
C2 C8 I1 118.5(7) . . ?
C7 C8 I1 121.7(8) . . ?
C2 C3 C4 119.9(9) . . ?
C2 C3 I3 121.0(7) . . ?
C4 C3 I3 119.1(8) . . ?
N3 N4 C22 120.3(11) . . ?
O2 C1 O1 128.3(10) . . ?
O2 C1 C2 116.8(10) . . ?
O1 C1 C2 114.9(10) . . ?
O11 C23 C22 122.6(13) . . ?
O11 C23 C24 118.8(13) . . ?
C22 C23 C24 118.5(11) . . ?
N4 N3 C20 122.6(10) . . ?
N4 N3 H3N 118.7 . . ?
C20 N3 H3N 118.7 . . ?
C5 O3 H3O 110.5 . . ?
C3 C2 C8 120.2(9) . . ?
C3 C2 C1 118.3(9) . . ?
C8 C2 C1 121.5(9) . . ?
C7 C6 C4 120.7(10) . . ?
C7 C6 I2 121.5(8) . . ?
C4 C6 I2 117.8(8) . . ?
C17 C19 C20 122.0(10) . . ?
C17 C19 I6 116.8(8) . . ?
C20 C19 I6 121.1(8) . . ?
N2 N1 C7 120.0(10) . . ?
N2 N1 H1 120.0 . . ?
C7 N1 H1 120.0 . . ?
O8 C14 O7 125.7(9) . . ?
O8 C14 C15 117.4(9) . . ?
O7 C14 C15 116.9(9) . . ?
N4 C22 C23 113.9(11) . . ?
N4 C22 C25 123.7(11) . . ?
C23 C22 C25 122.3(10) . . ?
C6 C4 C3 120.2(10) . . ?
C6 C4 C5 119.9(10) . . ?
C3 C4 C5 119.8(10) . . ?
C16 C15 C21 117.5(9) . . ?
C16 C15 C14 119.2(9) . . ?
C21 C15 C14 123.0(10) . . ?
O5 C10 C11 120.4(13) . . ?
O5 C10 C9 118.4(11) . . ?
C11 C10 C9 121.1(12) . . ?
C20 C21 C15 122.6(10) . . ?
C20 C21 I5 119.7(8) . . ?
C15 C21 I5 117.7(8) . . ?
N2 C9 C12 115.8(12) . . ?
N2 C9 C10 122.8(10) . . ?
C12 C9 C10 121.4(11) . . ?
O6 C12 C9 122.0(14) . . ?
O6 C12 C13 121.3(13) . . ?
C9 C12 C13 116.8(12) . . ?
O10 C18 O9 125.3(11) . . ?
O10 C18 C17 119.3(11) . . ?
O9 C18 C17 115.4(10) . . ?
O12 C25 C22 118.4(11) . . ?
O12 C25 C26 120.1(14) . . ?
C22 C25 C26 121.3(12) . . ?
C15 C16 C17 121.6(9) . . ?
C15 C16 I4 120.9(7) . . ?
C17 C16 I4 117.5(8) . . ?
C21 C20 N3 126.1(11) . . ?
C21 C20 C19 117.8(10) . . ?
N3 C20 C19 115.5(10) . . ?
C19 C17 C16 118.4(10) . . ?
C19 C17 C18 121.6(9) . . ?
C16 C17 C18 120.0(9) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C7 N1 117.9(10) . . ?
C6 C7 C8 119.2(9) . . ?
N1 C7 C8 122.7(10) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O4 C5 O3 123.3(12) . . ?
O4 C5 C4 125.7(11) . . ?
O3 C5 C4 111.0(10) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H32A O32 H32B 107.7 . . ?

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
N3 H3N O12 0.86 1.86 2.535(14) 134.6 .
N1 H1 O5 0.86 1.87 2.531(13) 132.7 .
C24 H24C I5 0.96 3.30 4.198(19) 156.0 2_566
C26 H26B O3 0.96 2.55 3.176(19) 122.8 2_666
C11 H11C O9 0.96 2.47 3.430(17) 176.4 2_666
O32 H32A O10 0.85 2.64 3.223(13) 127.2 .
O32 H32A O9 0.85 1.64 2.485(13) 175.6 .
O32 H32B O4 0.85 1.85 2.702(15) 175.8 1_554
O10 H10O I4 0.86 3.08 3.517(9) 114.2 .
O10 H10O O32 0.86 2.07 2.817(14) 144.5 2
O3 H3O O10 0.86 1.78 2.635(13) 178.3 1_656
O13 H13O O8 0.86 1.78 2.630(11) 176.1 2_556
O13 H14O O11 0.86 1.95 2.806(13) 176.2 1_545

_refine_diff_density_max         2.604
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.267

_shelxl_version_number           2014/6



