# 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_exp_3669
_database_code_depnum_ccdc_archive 'CCDC 2112908'
loop_
_audit_author_name
_audit_author_address
'Guo ruixin'
;Technical Institute of Physics and Chemistry, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2022-05-12 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'I13 O39 Sm3'
_chemical_formula_weight         2724.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   21.8760(3)
_cell_length_b                   21.8760(3)
_cell_length_c                   13.2528(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5492.55(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21813
_cell_measurement_theta_min      3.193
_cell_measurement_theta_max      26.364

_exptl_crystal_description       Prism
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7122
_exptl_absorpt_coefficient_mu    15.835
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21719
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         26.36
_reflns_number_total             2467
_reflns_number_gt                2467
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0689P)²+335.6209P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000121(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_number_reflns         2467
_refine_ls_number_parameters     169
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.065
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.16732(4) 0.20401(3) 0.88482(5) 0.00986(18) Uani 1 1 d . . .
I1 I -0.03819(5) 0.13979(5) 0.93962(7) 0.0178(2) Uani 1 1 d . . .
I2 I 0.14349(4) 0.25781(5) 0.62680(6) 0.0120(2) Uani 1 1 d . . .
I3 I 0.30483(4) 0.30270(4) 1.09182(7) 0.0126(2) Uani 1 1 d . . .
I4 I 0.16395(5) 0.38140(4) 0.86500(6) 0.0117(2) Uani 1 1 d . . .
I5A I 0.3333 0.6667 0.95122(17) 0.0275(5) Uani 0.862(5) 3 d SP . .
I5B I 0.3333 0.6667 1.0181(12) 0.0275(5) Uani 0.138(5) 3 d SP . .
O1 O -0.0166(7) 0.1674(6) 1.0690(9) 0.028(3) Uani 1 1 d . . .
O2 O 0.1768(6) 0.4323(6) 0.9777(8) 0.020(2) Uani 1 1 d U . .
O3 O -0.0971(6) 0.0457(6) 0.9668(8) 0.022(2) Uani 1 1 d . . .
O4 O 0.2549(6) 0.4251(6) 0.8284(10) 0.025(2) Uani 1 1 d . . .
O5 O 0.3511(7) 0.3965(7) 1.0750(11) 0.034(3) Uani 1 1 d . . .
O6 O 0.0593(5) 0.2071(6) 0.5624(8) 0.017(2) Uani 1 1 d . . .
O7 O 0.1585(7) 0.3049(6) 0.9253(8) 0.022(2) Uani 1 1 d . . .
O8 O 0.2798(5) 0.2744(6) 0.9617(8) 0.019(2) Uani 1 1 d . . .
O9 O 0.3811(5) 0.2904(5) 1.0900(7) 0.0132(18) Uani 1 1 d U . .
O10 O 0.1086(6) 0.1987(7) 0.7333(9) 0.032(3) Uani 1 1 d . . .
O11 O 0.0389(6) 0.1348(7) 0.9045(10) 0.034(3) Uani 1 1 d . . .
O12 O 0.1327(6) 0.3308(7) 0.6694(10) 0.031(3) Uani 1 1 d . . .
O13 O 0.2861(9) 0.5832(9) 0.8857(15) 0.051(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sm1 0.0102(3) 0.0102(3) 0.0110(3) 0.0014(2) 0.0021(2) 0.0064(3)
I1 0.0133(4) 0.0124(4) 0.0207(4) 0.0031(3) -0.0046(3) 0.0013(3)
I2 0.0097(4) 0.0145(4) 0.0121(4) -0.0028(3) -0.0017(3) 0.0063(3)
I3 0.0096(4) 0.0113(4) 0.0176(4) -0.0002(3) 0.0010(3) 0.0058(3)
I4 0.0127(4) 0.0107(4) 0.0139(4) -0.0018(3) 0.0000(3) 0.0075(3)
I5A 0.0259(7) 0.0259(7) 0.0306(12) 0.000 0.000 0.0129(3)
I5B 0.0259(7) 0.0259(7) 0.0306(12) 0.000 0.000 0.0129(3)
O1 0.031(7) 0.026(6) 0.026(6) -0.010(5) -0.008(5) 0.014(5)
O2 0.021(4) 0.026(4) 0.015(4) -0.007(3) -0.005(3) 0.014(3)
O3 0.016(5) 0.018(5) 0.019(5) 0.000(4) -0.009(4) 0.000(4)
O4 0.015(5) 0.017(5) 0.043(7) 0.002(5) 0.003(5) 0.007(4)
O5 0.023(6) 0.020(6) 0.053(9) -0.006(6) 0.001(6) 0.007(5)
O6 0.013(5) 0.017(5) 0.017(5) -0.003(4) -0.005(4) 0.004(4)
O7 0.031(6) 0.023(5) 0.019(5) -0.001(4) 0.003(4) 0.018(5)
O8 0.011(5) 0.030(6) 0.014(5) -0.002(4) -0.003(4) 0.009(5)
O9 0.011(3) 0.017(4) 0.014(3) -0.002(3) 0.000(3) 0.009(3)
O10 0.014(5) 0.046(8) 0.019(5) 0.013(5) -0.001(4) 0.002(5)
O11 0.017(5) 0.044(8) 0.037(7) -0.003(6) 0.006(5) 0.012(5)
O12 0.022(6) 0.036(7) 0.041(7) -0.028(6) -0.016(5) 0.020(6)
O13 0.040(8) 0.042(8) 0.070(10) -0.022(8) -0.010(8) 0.020(7)

_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
Sm1 O10 2.355(11) . ?
Sm1 O7 2.370(11) . ?
Sm1 O8 2.383(10) . ?
Sm1 O3 2.384(10) 3 ?
Sm1 O2 2.390(11) 10_554 ?
Sm1 O6 2.399(10) 5 ?
Sm1 O9 2.417(10) 15_554 ?
Sm1 O11 2.449(12) . ?
I1 O1 1.800(12) . ?
I1 O11 1.805(12) . ?
I1 O3 1.837(11) . ?
I2 O10 1.805(11) . ?
I2 O12 1.817(12) . ?
I2 O6 1.819(10) . ?
I3 O5 1.792(13) . ?
I3 O9 1.818(10) . ?
I3 O8 1.821(10) . ?
I4 O4 1.790(11) . ?
I4 O2 1.799(11) . ?
I4 O7 1.805(11) . ?
I5A I5B 0.886(15) . ?
I5A O13 1.809(15) 3_565 ?
I5A O13 1.809(15) . ?
I5A O13 1.809(15) 2_665 ?
I5B O13 2.365(19) 3_565 ?
I5B O13 2.365(19) . ?
I5B O13 2.365(19) 2_665 ?
O2 Sm1 2.390(11) 16_554 ?
O3 Sm1 2.384(10) 2 ?
O6 Sm1 2.399(10) 5_554 ?
O9 Sm1 2.417(10) 8 ?

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
O10 Sm1 O7 86.7(5) . . ?
O10 Sm1 O8 139.3(4) . . ?
O7 Sm1 O8 80.8(4) . . ?
O10 Sm1 O3 119.4(4) . 3 ?
O7 Sm1 O3 136.6(4) . 3 ?
O8 Sm1 O3 95.3(4) . 3 ?
O10 Sm1 O2 93.9(5) . 10_554 ?
O7 Sm1 O2 148.3(4) . 10_554 ?
O8 Sm1 O2 78.2(4) . 10_554 ?
O3 Sm1 O2 69.3(4) 3 10_554 ?
O10 Sm1 O6 137.5(4) . 5 ?
O7 Sm1 O6 69.7(4) . 5 ?
O8 Sm1 O6 72.7(4) . 5 ?
O3 Sm1 O6 67.9(4) 3 5 ?
O2 Sm1 O6 124.8(4) 10_554 5 ?
O10 Sm1 O9 65.8(3) . 15_554 ?
O7 Sm1 O9 79.3(4) . 15_554 ?
O8 Sm1 O9 73.8(3) . 15_554 ?
O3 Sm1 O9 141.3(4) 3 15_554 ?
O2 Sm1 O9 72.2(3) 10_554 15_554 ?
O6 Sm1 O9 137.2(3) 5 15_554 ?
O10 Sm1 O11 68.4(4) . . ?
O7 Sm1 O11 87.1(4) . . ?
O8 Sm1 O11 148.1(4) . . ?
O3 Sm1 O11 73.7(4) 3 . ?
O2 Sm1 O11 122.6(4) 10_554 . ?
O6 Sm1 O11 75.4(4) 5 . ?
O9 Sm1 O11 132.7(4) 15_554 . ?
O1 I1 O11 99.8(6) . . ?
O1 I1 O3 96.2(5) . . ?
O11 I1 O3 97.8(6) . . ?
O10 I2 O12 101.1(7) . . ?
O10 I2 O6 89.6(5) . . ?
O12 I2 O6 98.4(5) . . ?
O5 I3 O9 97.6(5) . . ?
O5 I3 O8 100.0(6) . . ?
O9 I3 O8 94.5(5) . . ?
O4 I4 O2 96.1(5) . . ?
O4 I4 O7 99.0(6) . . ?
O2 I4 O7 97.1(5) . . ?
I5B I5A O13 118.7(7) . 3_565 ?
I5B I5A O13 118.7(7) . . ?
O13 I5A O13 98.9(8) 3_565 . ?
I5B I5A O13 118.7(7) . 2_665 ?
O13 I5A O13 98.9(8) 3_565 2_665 ?
O13 I5A O13 98.9(8) . 2_665 ?
I5A I5B O13 42.1(6) . 3_565 ?
I5A I5B O13 42.1(6) . . ?
O13 I5B O13 71.0(9) 3_565 . ?
I5A I5B O13 42.1(6) . 2_665 ?
O13 I5B O13 71.0(9) 3_565 2_665 ?
O13 I5B O13 71.0(9) . 2_665 ?
I4 O2 Sm1 137.6(6) . 16_554 ?
I1 O3 Sm1 129.2(5) . 2 ?
I2 O6 Sm1 127.5(5) . 5_554 ?
I4 O7 Sm1 139.9(6) . . ?
I3 O8 Sm1 131.5(5) . . ?
I3 O9 Sm1 133.5(5) . 8 ?
I2 O10 Sm1 127.4(6) . . ?
I1 O11 Sm1 143.9(7) . . ?
I5A O13 I5B 19.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.305
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.255
