# Electronic Supplementary Material (ESI) for ChemComm.
# 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_3D-T4-SnOS
_database_code_depnum_ccdc_archive 'CCDC 1909342'
loop_
_audit_author_name
_audit_author_address
'Qipu Lin'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-08-09 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-18
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5775)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        3D-T4-SnOS
_chemical_formula_moiety         'O10 S32 Sn20, 4[C3H8N], 5[C4H9NO], 8[C2H7O]'
_chemical_formula_sum            'C48 H133 N9 O23 S32 Sn20'
_chemical_formula_weight         4604.35
_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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 '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      tetragonal
_space_group_IT_number           142
_space_group_name_H-M_alt        'I 41/a c d'
_space_group_name_Hall           '-I 4bd 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   23.5105(4)
_cell_length_b                   23.5105(4)
_cell_length_c                   40.205(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22223(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    99.99(16)
_cell_measurement_theta_max      74.1410
_cell_measurement_theta_min      4.3370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    41.182
_exptl_absorpt_correction_T_max  0.338
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             17440
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            20736
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.971
_diffrn_reflns_theta_min         3.450
_diffrn_ambient_temperature      99.99(16)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  41.00   1.00    6.08    --  -40.84  19.00 120.00  113
  2  ω    101.00 176.00   1.00   24.32    --  108.54  77.00-150.00   75
  3  ω     61.00 109.00   1.00   24.32    --  108.54 -95.00   0.00   48
  4  ω     81.00 177.00   1.00   24.32    --  108.54  44.00 -31.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4350
_reflns_number_total             5597
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         5597
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0776P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1173
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Sn1 Sn 0.63662(2) 0.93641(2) 0.28021(2) 0.02634(13) Uani 1 1 d . . . . .
Sn2 Sn 0.64977(2) 0.82631(2) 0.34407(2) 0.02113(12) Uani 1 1 d . . . . .
Sn3 Sn 0.56702(2) 0.70057(2) 0.34058(2) 0.01758(12) Uani 1 1 d . . . . .
Sn4 Sn 0.54435(2) 0.81081(2) 0.28145(2) 0.02265(12) Uani 1 1 d . . . . .
Sn5 Sn 0.52862(2) 0.91658(2) 0.34394(2) 0.02141(12) Uani 1 1 d . . . . .
S1 S 0.70985(8) 0.89078(8) 0.31179(5) 0.0303(4) Uani 1 1 d . . . . .
S2 S 0.59019(8) 0.87471(9) 0.24141(4) 0.0315(4) Uani 1 1 d . . . . .
S3 S 0.57267(9) 0.99349(8) 0.31204(5) 0.0323(4) Uani 1 1 d . . . . .
S4 S 0.72726(7) 0.78437(8) 0.37474(5) 0.0284(4) Uani 1 1 d . . . . .
S5 S 0.63065(7) 0.74971(8) 0.29968(4) 0.0223(3) Uani 1 1 d . . . . .
S6 S 0.500000 0.750000 0.24103(6) 0.0334(6) Uani 1 2 d S T P . .
S7 S 0.64721(7) 0.64193(7) 0.36337(4) 0.0231(3) Uani 1 1 d . . . . .
S8 S 0.53958(7) 0.62507(8) 0.29990(4) 0.0245(3) Uani 1 1 d . . . . .
S9 S 0.69741(11) 1.000000 0.250000 0.0341(6) Uani 1 2 d S T P . .
O1 O 0.5762(2) 0.8547(2) 0.32155(12) 0.0236(10) Uani 1 1 d . . . . .
O2 O 0.59215(18) 0.76411(19) 0.37480(10) 0.0159(9) Uani 1 1 d . . . . .
O3 O 0.500000 0.750000 0.32092(16) 0.0198(13) Uani 1 2 d S T 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
Sn1 S1 2.3933(19) . ?
Sn1 S2 2.393(2) . ?
Sn1 S3 2.387(2) . ?
Sn1 S9 2.3985(16) . ?
Sn2 S1 2.4446(18) . ?
Sn2 S4 2.4107(18) . ?
Sn2 S5 2.5750(18) . ?
Sn2 S7 2.5821(18) 28_656 ?
Sn2 O1 2.063(5) . ?
Sn2 O2 2.345(4) . ?
Sn3 S5 2.5055(17) . ?
Sn3 S7 2.5089(17) . ?
Sn3 S8 2.4984(17) . ?
Sn3 O2 2.120(4) 19_576 ?
Sn3 O2 2.115(4) . ?
Sn3 O3 2.111(2) . ?
Sn4 S2 2.4515(19) . ?
Sn4 S5 2.5918(17) . ?
Sn4 S6 2.4026(17) . ?
Sn4 S8 2.5916(18) 10_564 ?
Sn4 O1 2.056(5) . ?
Sn4 O3 2.377(4) . ?
Sn5 S3 2.4468(18) . ?
Sn5 S4 2.4113(18) 28_656 ?
Sn5 S7 2.5772(18) 28_656 ?
Sn5 S8 2.5816(19) 10_564 ?
Sn5 O1 2.044(5) . ?
Sn5 O2 2.377(4) 28_656 ?

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
S1 Sn1 S2 113.72(7) . . ?
S1 Sn1 S9 96.86(7) . . ?
S2 Sn1 S9 108.64(5) . . ?
S3 Sn1 S1 114.87(7) . . ?
S3 Sn1 S2 113.76(7) . . ?
S3 Sn1 S9 107.23(6) . . ?
S1 Sn2 S5 99.59(6) . . ?
S1 Sn2 S7 99.84(6) . 28_656 ?
S4 Sn2 S1 95.08(6) . . ?
S4 Sn2 S5 101.56(6) . . ?
S4 Sn2 S7 102.24(6) . 28_656 ?
S5 Sn2 S7 147.62(6) . 28_656 ?
O1 Sn2 S1 92.89(15) . . ?
O1 Sn2 S4 172.03(15) . . ?
O1 Sn2 S5 77.06(15) . . ?
O1 Sn2 S7 76.32(14) . 28_656 ?
O1 Sn2 O2 87.08(18) . . ?
O2 Sn2 S1 179.69(12) . . ?
O2 Sn2 S4 84.95(11) . . ?
O2 Sn2 S5 80.11(11) . . ?
O2 Sn2 S7 80.45(11) . 28_656 ?
S5 Sn3 S7 92.55(6) . . ?
S8 Sn3 S5 92.99(6) . . ?
S8 Sn3 S7 92.44(6) . . ?
O2 Sn3 S5 86.24(13) . . ?
O2 Sn3 S5 179.07(13) 19_576 . ?
O2 Sn3 S7 86.60(12) . . ?
O2 Sn3 S7 86.61(13) 19_576 . ?
O2 Sn3 S8 86.65(12) 19_576 . ?
O2 Sn3 S8 178.74(13) . . ?
O2 Sn3 O2 94.10(14) . 19_576 ?
O3 Sn3 S5 86.91(12) . . ?
O3 Sn3 S7 179.39(16) . . ?
O3 Sn3 S8 87.32(12) . . ?
O3 Sn3 O2 93.93(16) . 19_576 ?
O3 Sn3 O2 93.63(16) . . ?
S2 Sn4 S5 100.44(6) . . ?
S2 Sn4 S8 99.57(6) . 10_564 ?
S6 Sn4 S2 96.39(6) . . ?
S6 Sn4 S5 101.61(4) . . ?
S6 Sn4 S8 102.08(4) . 10_564 ?
S8 Sn4 S5 146.88(6) 10_564 . ?
O1 Sn4 S2 92.69(15) . . ?
O1 Sn4 S5 76.78(14) . . ?
O1 Sn4 S6 170.92(15) . . ?
O1 Sn4 S8 76.17(14) . 10_564 ?
O1 Sn4 O3 86.48(18) . . ?
O3 Sn4 S2 179.10(12) . . ?
O3 Sn4 S5 79.71(5) . . ?
O3 Sn4 S6 84.45(13) . . ?
O3 Sn4 S8 79.91(5) . 10_564 ?
S3 Sn5 S7 99.96(6) . 28_656 ?
S3 Sn5 S8 100.59(7) . 10_564 ?
S4 Sn5 S3 95.54(6) 28_656 . ?
S4 Sn5 S7 101.65(6) 28_656 28_656 ?
S4 Sn5 S8 101.60(6) 28_656 10_564 ?
S7 Sn5 S8 147.13(6) 28_656 10_564 ?
O1 Sn5 S3 93.62(15) . . ?
O1 Sn5 S4 170.84(15) . 28_656 ?
O1 Sn5 S7 76.74(14) . 28_656 ?
O1 Sn5 S8 76.60(14) . 10_564 ?
O1 Sn5 O2 86.59(18) . 28_656 ?
O2 Sn5 S3 179.69(12) 28_656 . ?
O2 Sn5 S4 84.25(11) 28_656 28_656 ?
O2 Sn5 S7 79.87(11) 28_656 28_656 ?
O2 Sn5 S8 79.68(11) 28_656 10_564 ?
Sn1 S1 Sn2 98.27(7) . . ?
Sn1 S2 Sn4 98.27(7) . . ?
Sn1 S3 Sn5 97.59(7) . . ?
Sn2 S4 Sn5 94.09(6) . 19_576 ?
Sn2 S5 Sn4 86.85(5) . . ?
Sn3 S5 Sn2 88.38(5) . . ?
Sn3 S5 Sn4 88.49(5) . . ?
Sn4 S6 Sn4 94.87(9) 10_564 . ?
Sn3 S7 Sn2 88.03(5) . 19_576 ?
Sn3 S7 Sn5 88.72(5) . 19_576 ?
Sn5 S7 Sn2 87.02(5) 19_576 19_576 ?
Sn3 S8 Sn4 88.32(6) . 10_564 ?
Sn3 S8 Sn5 88.91(5) . 10_564 ?
Sn5 S8 Sn4 86.80(5) 10_564 10_564 ?
Sn1 S9 Sn1 106.85(10) . 6_575 ?
Sn4 O1 Sn2 119.1(2) . . ?
Sn5 O1 Sn2 119.7(2) . . ?
Sn5 O1 Sn4 120.2(2) . . ?
Sn2 O2 Sn5 96.71(15) . 19_576 ?
Sn3 O2 Sn2 105.02(18) . . ?
Sn3 O2 Sn2 104.70(18) 28_656 . ?
Sn3 O2 Sn3 135.2(2) . 28_656 ?
Sn3 O2 Sn5 104.54(18) . 19_576 ?
Sn3 O2 Sn5 104.45(17) 28_656 19_576 ?
Sn3 O3 Sn3 136.0(3) 10_564 . ?
Sn3 O3 Sn4 104.25(7) 10_564 . ?
Sn3 O3 Sn4 104.69(7) . . ?
Sn3 O3 Sn4 104.69(7) 10_564 10_564 ?
Sn3 O3 Sn4 104.26(7) . 10_564 ?
Sn4 O3 Sn4 96.2(2) 10_564 . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 4692 electrons were 
found in a volume of 12255Å^3 in 1 void. 
This is consistent with the presence of 
4[C3H8N], 5[C4H9NO], 8[C2H7O] per formula unit 
which account for 4704 electrons.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.981 -0.619 -0.594 12254.6 4692.1 'C3H8N, 1.25 C4H9NO, 2 ethanol'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_preparation       Luminescent
