# 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_NTOU-2S
_database_code_depnum_ccdc_archive 'CCDC 1990629'
loop_
_audit_author_name
_audit_author_address
Wang
;National Taiwan Ocean University
Taiwan
;
_audit_update_record             
;
2020-03-16 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_NTOU-2S             
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: The organic molecules disordered in the crystalline structure of NTOU-2S and those atoms were flattened by the SQUEEZE option of PLATON. The TG and EA analyses confirmed the presence of organic amines in this compound.
;
# Added during the CSD deposition process: Monday 16 March 2020 09:33 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H4 N0 O10 P2 S Zn2'
_chemical_formula_weight         460.83

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pccn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   19.5786(9)
_cell_length_b                   29.0287(13)
_cell_length_c                   9.9053(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5629.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6504
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.62

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            103541
_diffrn_reflns_av_R_equivalents  0.1147
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         27.62
_reflns_number_total             6504
_reflns_number_gt                4879
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0625P)²+8.2703P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6504
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1338
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.03701(7) 0.48414(4) 0.30537(12) 0.0515(3) Uani 1 1 d . . .
Zn1 Zn 0.07183(3) 0.313179(14) 0.21638(4) 0.03511(14) Uani 1 1 d . . .
Zn2 Zn 0.15619(2) 0.144054(15) 0.37053(4) 0.03283(13) Uani 1 1 d . . .
P1 P 0.09507(6) 0.23871(3) 0.43276(10) 0.0363(2) Uani 1 1 d . . .
H1 H 0.1588 0.2490 0.4342 0.050 Uiso 1 1 d . . .
P2 P 0.22694(6) 0.33226(3) 0.16022(10) 0.0348(2) Uani 1 1 d . . .
H2 H 0.2370 0.2883 0.1631 0.050 Uiso 1 1 d . . .
O1 O 0.0777(2) 0.23334(11) 0.5783(3) 0.0697(12) Uani 1 1 d . . .
O2 O 0.09154(16) 0.19472(10) 0.3513(3) 0.0458(7) Uani 1 1 d . . .
O3 O 0.05084(16) 0.27698(10) 0.3742(3) 0.0452(7) Uani 1 1 d . . .
O4 O 0.16233(17) 0.34135(11) 0.2384(3) 0.0520(8) Uani 1 1 d . . .
O5 O 0.28553(17) 0.36112(11) 0.2111(3) 0.0493(8) Uani 1 1 d . . .
O6 O 0.21979(16) 0.33857(12) 0.0114(3) 0.0506(8) Uani 1 1 d . . .
O7 O 0.0222(2) 0.39195(12) 0.3772(4) 0.0642(10) Uani 1 1 d . . .
O8 O 0.0070(2) 0.36091(10) 0.1735(4) 0.0607(9) Uani 1 1 d . . .
O9 O -0.07693(19) 0.58386(12) 0.3009(4) 0.0616(9) Uani 1 1 d . . .
O10 O -0.12256(18) 0.58269(10) 0.0941(3) 0.0532(8) Uani 1 1 d . . .
C1 C 0.0017(2) 0.39347(15) 0.2586(5) 0.0500(11) Uani 1 1 d . . .
C2 C -0.0303(2) 0.43591(14) 0.2056(4) 0.0445(10) Uani 1 1 d . . .
C3 C -0.0553(3) 0.44372(15) 0.0796(5) 0.0539(12) Uani 1 1 d . . .
H3A H -0.0564 0.4216 0.0118 0.065 Uiso 1 1 calc R . .
C4 C -0.0793(3) 0.48893(16) 0.0633(5) 0.0558(13) Uani 1 1 d . . .
H4A H -0.0978 0.5000 -0.0169 0.067 Uiso 1 1 calc R . .
C5 C -0.0729(2) 0.51474(14) 0.1765(5) 0.0419(10) Uani 1 1 d . . .
C6 C -0.0910(2) 0.56423(15) 0.1950(5) 0.0463(10) 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
S1 0.0658(8) 0.0434(6) 0.0451(6) -0.0035(5) -0.0121(6) 0.0124(5)
Zn1 0.0532(3) 0.0254(2) 0.0268(2) 0.00003(17) -0.0004(2) 0.00136(19)
Zn2 0.0398(3) 0.0307(2) 0.0279(2) -0.00155(17) 0.00080(18) -0.00180(18)
P1 0.0518(6) 0.0280(5) 0.0291(5) 0.0048(4) 0.0000(5) 0.0023(4)
P2 0.0468(6) 0.0296(5) 0.0281(5) 0.0043(4) -0.0052(4) -0.0016(4)
O1 0.141(4) 0.0409(18) 0.0276(15) 0.0094(13) 0.0159(19) 0.020(2)
O2 0.0555(19) 0.0381(15) 0.0438(17) -0.0057(13) -0.0123(14) 0.0109(13)
O3 0.0621(19) 0.0394(16) 0.0340(15) 0.0091(12) 0.0098(14) 0.0137(14)
O4 0.060(2) 0.0548(19) 0.0414(17) -0.0106(14) 0.0054(14) -0.0130(16)
O5 0.0566(19) 0.0567(19) 0.0346(16) 0.0132(13) -0.0133(14) -0.0153(15)
O6 0.0508(18) 0.070(2) 0.0307(15) 0.0028(14) -0.0070(13) -0.0049(16)
O7 0.083(3) 0.053(2) 0.057(2) 0.0126(16) -0.0226(19) 0.0083(18)
O8 0.081(3) 0.0325(16) 0.068(2) -0.0005(15) -0.0229(19) 0.0144(16)
O9 0.073(2) 0.0485(19) 0.063(2) -0.0183(17) -0.0080(18) 0.0073(17)
O10 0.071(2) 0.0357(16) 0.0533(19) 0.0047(14) 0.0076(17) 0.0143(15)
C1 0.049(3) 0.038(2) 0.062(3) 0.005(2) -0.006(2) 0.008(2)
C2 0.050(3) 0.034(2) 0.049(3) 0.0017(18) -0.010(2) 0.0066(18)
C3 0.076(3) 0.035(2) 0.051(3) -0.005(2) -0.005(2) 0.016(2)
C4 0.081(4) 0.040(2) 0.046(3) 0.000(2) -0.015(2) 0.020(2)
C5 0.045(2) 0.034(2) 0.047(2) -0.0010(18) -0.0014(19) 0.0113(18)
C6 0.045(2) 0.038(2) 0.056(3) -0.003(2) 0.006(2) 0.0027(19)

_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 C5 1.706(4) . ?
S1 C2 1.719(4) . ?
Zn1 O1 1.926(3) 7_565 ?
Zn1 O8 1.927(3) . ?
Zn1 O3 1.928(3) . ?
Zn1 O4 1.964(3) . ?
Zn2 O10 1.931(3) 3_545 ?
Zn2 O6 1.937(3) 7_566 ?
Zn2 O2 1.950(3) . ?
Zn2 O5 1.954(3) 2 ?
P1 O1 1.490(3) . ?
P1 O2 1.512(3) . ?
P1 O3 1.523(3) . ?
P1 H1 1.2831 . ?
P2 O6 1.492(3) . ?
P2 O4 1.507(3) . ?
P2 O5 1.507(3) . ?
P2 H2 1.2916 . ?
O1 Zn1 1.926(3) 7_566 ?
O5 Zn2 1.954(3) 2 ?
O6 Zn2 1.937(3) 7_565 ?
O7 C1 1.243(6) . ?
O8 C1 1.271(6) . ?
O9 C6 1.225(5) . ?
O10 C6 1.291(6) . ?
O10 Zn2 1.931(3) 3 ?
C1 C2 1.478(6) . ?
C2 C3 1.360(6) . ?
C3 C4 1.403(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.354(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.491(6) . ?

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 S1 C2 91.5(2) . . ?
O1 Zn1 O8 112.75(16) 7_565 . ?
O1 Zn1 O3 101.91(13) 7_565 . ?
O8 Zn1 O3 115.48(15) . . ?
O1 Zn1 O4 108.52(16) 7_565 . ?
O8 Zn1 O4 108.63(15) . . ?
O3 Zn1 O4 109.23(14) . . ?
O10 Zn2 O6 109.19(15) 3_545 7_566 ?
O10 Zn2 O2 119.48(14) 3_545 . ?
O6 Zn2 O2 106.93(13) 7_566 . ?
O10 Zn2 O5 105.96(13) 3_545 2 ?
O6 Zn2 O5 103.12(13) 7_566 2 ?
O2 Zn2 O5 110.98(14) . 2 ?
O1 P1 O2 114.68(19) . . ?
O1 P1 O3 108.34(18) . . ?
O2 P1 O3 112.75(17) . . ?
O1 P1 H1 103.7 . . ?
O2 P1 H1 104.3 . . ?
O3 P1 H1 112.8 . . ?
O6 P2 O4 114.05(19) . . ?
O6 P2 O5 109.48(18) . . ?
O4 P2 O5 111.71(18) . . ?
O6 P2 H2 99.1 . . ?
O4 P2 H2 106.8 . . ?
O5 P2 H2 115.2 . . ?
P1 O1 Zn1 140.8(2) . 7_566 ?
P1 O2 Zn2 123.72(18) . . ?
P1 O3 Zn1 125.80(18) . . ?
P2 O4 Zn1 128.88(19) . . ?
P2 O5 Zn2 132.21(18) . 2 ?
P2 O6 Zn2 143.5(2) . 7_565 ?
C1 O8 Zn1 116.2(3) . . ?
C6 O10 Zn2 113.9(3) . 3 ?
O7 C1 O8 125.1(4) . . ?
O7 C1 C2 120.1(4) . . ?
O8 C1 C2 114.8(4) . . ?
C3 C2 C1 128.1(4) . . ?
C3 C2 S1 111.3(3) . . ?
C1 C2 S1 120.5(3) . . ?
C2 C3 C4 112.5(4) . . ?
C2 C3 H3A 123.8 . . ?
C4 C3 H3A 123.8 . . ?
C5 C4 C3 113.0(4) . . ?
C5 C4 H4A 123.5 . . ?
C3 C4 H4A 123.5 . . ?
C4 C5 C6 127.8(4) . . ?
C4 C5 S1 111.7(3) . . ?
C6 C5 S1 120.5(3) . . ?
O9 C6 O10 125.3(4) . . ?
O9 C6 C5 120.0(4) . . ?
O10 C6 C5 114.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.092
