# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_mo_2017943-zwo-74_0ma
_audit_block_doi                 10.5517/ccdc.csd.cc25f7tp
_database_code_depnum_ccdc_archive 'CCDC 2008732'
loop_
_audit_author_name
_audit_author_address
'Yuteng Cao'
;CAEP
China
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_audit_creation_date             2020-01-08
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C8 H40 N100 Na20 O16 S4), C2 H6 O S'
_chemical_formula_sum            'C4 H16 N25 Na5 O5 S2'
_chemical_formula_weight         673.49
_chemical_absolute_configuration ad
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, -z+1/2'
4 'x, -y, -z'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 '-x+1/2, y+1/2, -z+1/2'
8 'x+1/2, -y+1/2, -z'

_cell_length_a                   9.3283(9)
_cell_length_b                   30.151(3)
_cell_length_c                   9.6156(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2704.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1401
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.51
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0642 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.9044. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6989
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.35
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                2271
_reflns_number_total             2605
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(14)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0317P)²+1.5052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0940
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: S2(0.5)
3.a Riding coordinates:
 O1(H1A,H1B), C4(H4A,H4B,H4C)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
S1 S -0.32565(13) -0.5000 -0.5000 0.0178(2) Uani 1 d . . 2 S T P
Na1 Na -0.65942(13) -0.53373(4) -0.64087(13) 0.0195(3) Uani 1 d . . 1 . . .
Na2 Na -0.5000 -0.75351(5) -0.7500 0.0144(4) Uani 1 d . . 2 S T P
Na3 Na 0.16216(13) -0.67201(3) -0.59428(13) 0.0192(3) Uani 1 d . . 1 . . .
O1 O -0.7058(3) -0.54332(7) -0.4002(3) 0.0303(6) Uani 1 d . . 1 . . .
H1A H -0.7819 -0.5585 -0.3738 0.047(13) Uiso 1 d . . 1 R . .
H1B H -0.6447 -0.5616 -0.3672 0.14(3) Uiso 1 d . . 1 R . .
O2 O -0.4086(3) -0.51386(7) -0.6197(2) 0.0258(5) Uani 1 d . . 1 . . .
C3 C -0.2138(4) -0.45696(12) -0.5521(4) 0.0348(10) Uani 1 d . . 1 . . .
H3A H -0.2701 -0.4338 -0.5932 0.052 Uiso 1 calc . . 1 GR . .
H3B H -0.1460 -0.4678 -0.6191 0.052 Uiso 1 calc . . 1 GR . .
H3C H -0.1634 -0.4455 -0.4728 0.052 Uiso 1 calc . . 1 GR . .
N1 N -1.0000 -0.53534(12) -0.7500 0.0243(9) Uani 1 d . . 2 S T P
N2 N -0.9017(3) -0.56131(8) -0.6944(3) 0.0251(6) Uani 1 d . . 1 . . .
N3 N -0.9397(3) -0.60296(9) -0.7159(3) 0.0262(7) Uani 1 d . . 1 . . .
N4 N -0.5568(3) -0.60478(8) -0.7100(3) 0.0298(8) Uani 1 d . . 1 . . .
N5 N -0.5924(3) -0.64635(8) -0.6844(3) 0.0234(6) Uani 1 d . . 1 . . .
N6 N -0.5000 -0.67179(11) -0.7500 0.0238(9) Uani 1 d . . 2 S T P
N7 N -0.5000 -0.83506(12) -0.7500 0.0281(10) Uani 1 d . . 2 S T P
N8 N -0.5665(3) -0.86067(8) -0.8414(3) 0.0260(7) Uani 1 d . . 1 . . .
N9 N -0.5407(3) -0.90195(8) -0.8059(3) 0.0286(7) Uani 1 d . . 1 . . .
N10 N -0.2597(3) -0.74660(9) -0.6473(3) 0.0226(6) Uani 1 d . . 1 . . .
N11 N -0.2216(3) -0.76393(8) -0.5255(3) 0.0197(6) Uani 1 d . . 1 . . .
N12 N -0.1048(3) -0.74242(8) -0.4834(3) 0.0232(6) Uani 1 d . . 1 . . .
N13 N -0.0721(3) -0.71203(8) -0.5769(3) 0.0215(6) Uani 1 d . . 1 . . .
N14 N -0.1703(3) -0.71474(8) -0.6778(3) 0.0232(6) Uani 1 d . . 1 . . .
S2 S -0.5477(2) -0.64273(6) -0.3070(2) 0.0394(5) Uani 0.50 d . . 1 . . .
C4 C -0.4025(7) -0.66990(16) -0.3573(6) 0.0714(17) Uani 1 d . . 1 . . .
H4A H -0.3092 -0.6654 -0.3126 0.33(7) Uiso 1 d . . 1 R . .
H4B H -0.4240 -0.7017 -0.3615 0.20(4) Uiso 1 d . . 1 R . .
H4C H -0.3999 -0.6577 -0.4518 0.41(9) Uiso 1 d . . 1 R . .
O0AA O -0.5000 -0.59607(12) -0.2500 0.0651(15) Uani 1 d . . 2 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
S1 O2 1.449(2) . ?
S1 O2 1.449(2) 4_544 ?
S1 C3 1.739(3) 4_544 ?
S1 C3 1.739(3) . ?
Na1 Na1 3.640(2) 3_453 ?
Na1 Na1 3.388(2) 4_544 ?
Na1 O1 2.372(3) . ?
Na1 O1 2.396(2) 4_544 ?
Na1 O2 2.423(3) . ?
Na1 O2 2.462(3) 3_453 ?
Na1 N2 2.463(3) . ?
Na1 N4 2.439(3) . ?
Na2 N6 2.464(4) . ?
Na2 N7 2.459(4) . ?
Na2 N10 2.458(3) . ?
Na2 N10 2.458(3) 3_453 ?
Na2 N12 2.451(3) 8_434 ?
Na2 N12 2.451(3) 6_434 ?
Na3 N3 2.570(3) 1_655 ?
Na3 N5 2.567(3) 1_655 ?
Na3 N8 2.771(3) 6_435 ?
Na3 N11 2.497(3) 8_534 ?
Na3 N13 2.502(3) . ?
Na3 N14 2.543(3) 3_553 ?
O1 Na1 2.396(2) 4_544 ?
O2 Na1 2.462(3) 3_453 ?
N1 N2 1.319(3) 3_353 ?
N1 N2 1.319(3) . ?
N2 N3 1.321(4) . ?
N3 Na3 2.570(3) 1_455 ?
N3 N3 1.302(5) 3_353 ?
N4 N4 1.309(6) 3_453 ?
N4 N5 1.320(3) . ?
N5 Na3 2.567(3) 1_455 ?
N5 N6 1.315(3) . ?
N6 N5 1.315(3) 3_453 ?
N7 N8 1.324(3) 3_453 ?
N7 N8 1.324(3) . ?
N8 Na3 2.771(3) 6_434 ?
N8 N9 1.313(4) . ?
N9 N9 1.316(6) 3_453 ?
N10 N11 1.331(4) . ?
N10 N14 1.305(4) . ?
N11 Na3 2.497(3) 8_434 ?
N11 N12 1.331(4) . ?
N12 Na2 2.451(3) 6_435 ?
N12 N13 1.319(4) . ?
N13 N14 1.337(4) . ?
N14 Na3 2.543(3) 3_553 ?
S2 S2 1.412(4) 3_454 ?
S2 C4 1.839(6) 3_454 ?
S2 C4 1.656(6) . ?
S2 O0AA 1.574(4) . ?
C4 S2 1.839(6) 3_454 ?
O0AA S2 1.574(4) 3_454 ?

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 S1 O2 115.4(2) . 4_544 ?
O2 S1 C3 107.88(16) . . ?
O2 S1 C3 109.53(16) . 4_544 ?
O2 S1 C3 107.88(16) 4_544 4_544 ?
O2 S1 C3 109.53(16) 4_544 . ?
C3 S1 C3 106.2(3) 4_544 . ?
Na1 Na1 Na1 117.45(2) 4_544 3_453 ?
O1 Na1 Na1 104.04(7) 4_544 3_453 ?
O1 Na1 Na1 44.43(7) 4_544 4_544 ?
O1 Na1 Na1 45.01(6) . 4_544 ?
O1 Na1 Na1 135.36(9) . 3_453 ?
O1 Na1 O1 85.66(10) . 4_544 ?
O1 Na1 O2 87.98(9) 4_544 3_453 ?
O1 Na1 O2 85.45(9) 4_544 . ?
O1 Na1 O2 97.13(9) . . ?
O1 Na1 O2 171.47(9) . 3_453 ?
O1 Na1 N2 89.73(10) . . ?
O1 Na1 N2 101.31(10) 4_544 . ?
O1 Na1 N4 165.37(10) 4_544 . ?
O1 Na1 N4 103.33(10) . . ?
O2 Na1 Na1 77.55(6) . 4_544 ?
O2 Na1 Na1 42.24(6) . 3_453 ?
O2 Na1 Na1 126.99(8) 3_453 4_544 ?
O2 Na1 Na1 41.43(6) 3_453 3_453 ?
O2 Na1 O2 76.67(9) . 3_453 ?
O2 Na1 N2 170.74(10) . . ?
O2 Na1 N2 97.09(10) 3_453 . ?
O2 Na1 N4 82.01(9) . . ?
N2 Na1 Na1 111.70(7) . 4_544 ?
N2 Na1 Na1 129.01(9) . 3_453 ?
N4 Na1 Na1 138.19(9) . 4_544 ?
N4 Na1 Na1 61.45(7) . 3_453 ?
N4 Na1 O2 81.82(9) . 3_453 ?
N4 Na1 N2 90.39(10) . . ?
N7 Na2 N6 180.000(1) . . ?
N10 Na2 N6 85.14(7) . . ?
N10 Na2 N6 85.14(7) 3_453 . ?
N10 Na2 N7 94.86(7) . . ?
N10 Na2 N7 94.86(7) 3_453 . ?
N10 Na2 N10 170.28(14) 3_453 . ?
N12 Na2 N6 92.87(7) 8_434 . ?
N12 Na2 N6 92.87(7) 6_434 . ?
N12 Na2 N7 87.13(7) 8_434 . ?
N12 Na2 N7 87.13(7) 6_434 . ?
N12 Na2 N10 90.00(9) 6_434 3_453 ?
N12 Na2 N10 90.00(9) 8_434 . ?
N12 Na2 N10 90.48(10) 8_434 3_453 ?
N12 Na2 N10 90.48(10) 6_434 . ?
N12 Na2 N12 174.26(14) 6_434 8_434 ?
N3 Na3 N8 89.55(9) 1_655 6_435 ?
N5 Na3 N3 86.10(9) 1_655 1_655 ?
N5 Na3 N8 118.45(10) 1_655 6_435 ?
N11 Na3 N3 175.73(10) 8_534 1_655 ?
N11 Na3 N5 90.08(9) 8_534 1_655 ?
N11 Na3 N8 90.59(9) 8_534 6_435 ?
N11 Na3 N13 88.60(9) 8_534 . ?
N11 Na3 N14 89.57(9) 8_534 3_553 ?
N13 Na3 N3 95.63(10) . 1_655 ?
N13 Na3 N5 161.23(10) . 1_655 ?
N13 Na3 N8 80.29(9) . 6_435 ?
N13 Na3 N14 80.76(10) . 3_553 ?
N14 Na3 N3 91.67(10) 3_553 1_655 ?
N14 Na3 N5 80.51(10) 3_553 1_655 ?
N14 Na3 N8 161.04(10) 3_553 6_435 ?
Na1 O1 Na1 90.56(9) . 4_544 ?
S1 O2 Na1 130.83(14) . . ?
S1 O2 Na1 132.48(14) . 3_453 ?
Na1 O2 Na1 96.33(9) . 3_453 ?
N2 N1 N2 107.2(3) 3_353 . ?
N1 N2 Na1 121.48(19) . . ?
N1 N2 N3 108.3(3) . . ?
N3 N2 Na1 126.9(2) . . ?
N2 N3 Na3 126.8(2) . 1_455 ?
N3 N3 Na3 123.27(10) 3_353 1_455 ?
N3 N3 N2 108.11(18) 3_353 . ?
N4 N4 Na1 118.54(7) 3_453 . ?
N4 N4 N5 108.26(17) 3_453 . ?
N5 N4 Na1 133.2(2) . . ?
N4 N5 Na3 125.0(2) . 1_455 ?
N6 N5 Na3 124.80(18) . 1_455 ?
N6 N5 N4 107.4(3) . . ?
N5 N6 Na2 125.68(16) . . ?
N5 N6 Na2 125.68(16) 3_453 . ?
N5 N6 N5 108.6(3) . 3_453 ?
N8 N7 Na2 125.66(18) . . ?
N8 N7 Na2 125.66(18) 3_453 . ?
N8 N7 N8 108.7(4) 3_453 . ?
N7 N8 Na3 121.74(19) . 6_434 ?
N9 N8 Na3 128.6(2) . 6_434 ?
N9 N8 N7 107.1(3) . . ?
N8 N9 N9 108.55(18) . 3_453 ?
N11 N10 Na2 124.3(2) . . ?
N14 N10 Na2 123.7(2) . . ?
N14 N10 N11 108.4(3) . . ?
N10 N11 Na3 126.40(19) . 8_434 ?
N12 N11 Na3 126.33(19) . 8_434 ?
N12 N11 N10 107.2(2) . . ?
N11 N12 Na2 125.5(2) . 6_435 ?
N13 N12 Na2 124.5(2) . 6_435 ?
N13 N12 N11 108.7(3) . . ?
N12 N13 Na3 125.6(2) . . ?
N12 N13 N14 107.1(2) . . ?
N14 N13 Na3 125.4(2) . . ?
N10 N14 Na3 125.8(2) . 3_553 ?
N10 N14 N13 108.6(2) . . ?
N13 N14 Na3 125.03(19) . 3_553 ?
S2 S2 C4 59.5(2) 3_454 3_454 ?
S2 S2 C4 73.2(2) 3_454 . ?
S2 S2 O0AA 63.35(10) 3_454 . ?
C4 S2 C4 103.7(4) . 3_454 ?
O0AA S2 C4 99.8(2) . 3_454 ?
O0AA S2 C4 108.2(2) . . ?
S2 C4 S2 47.30(19) . 3_454 ?
S2 O0AA S2 53.30(19) 3_454 . ?

_olex2_submission_special_instructions 'No special instructions were received'
