# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 2059597'
loop_
_audit_author_name
_audit_author_address
'fengqin wang'
;tian kong university
China
;
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_audit_creation_date             2019-05-30
_chemical_formula_sum            'C52 H36 Cd4 N4 O24 S4'
_chemical_formula_weight         1678.690
_refine_ls_R_factor_all          0.077
_cell_length_a                   14.862(4)
_cell_length_b                   6.2811(13)
_cell_length_c                   28.213(6)
_cell_angle_alpha                90.000
_cell_angle_beta                 95.88(4)
_cell_angle_gamma                90.000
_cell_volume                     2619.8(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    3757
_cell_measurement_theta_min      2.5773
_cell_measurement_theta_max      27.8864
_symmetry_int_tables_number      15
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  -C_2yc

_exptl_crystal_description       block
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_reflns_number            12693
_diffrn_reflns_av_R_equivalents  0.0434

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_radius_bond
Cd ? 1.200
S ? 1.200
O ? 1.200
N ? 1.200
C ? 1.200
H ? 1.200


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_thermal_displace_type
_atom_site_u_iso_or_equiv
Cd1 Cd 0.375() 0.6928(1) -0.0064(0) 1.000 8 f ? d Uani 0.01459(18)
S1 S 0.1955(2) 0.5516(4) 0.1445(1) 0.750 8 f ? d Uani 0.0197(6)
O3 O 0.1332(4) 0.5382(10) 0.2398(2) 0.750 8 f ? d Uani 0.0320(15)
N1 N 0.1306(5) 0.1769(11) 0.2491(3) 0.750 8 f ? d Uani 0.0222(15)
C1 C 0.2759(13) 0.521(3) 0.0610(7) 0.750 8 f ? d Uani 0.012(3)
C2 C 0.2444(9) 0.4078(17) 0.1010(4) 0.750 8 f ? d Uani 0.017(2)
C3 C 0.2510(9) 0.1879(17) 0.1131(4) 0.750 8 f ? d Uani 0.020(2)
C4 C 0.2154(10) 0.1486(16) 0.1576(4) 0.750 8 f ? d Uani 0.021(2)
C5 C 0.1835(7) 0.3310(14) 0.1798(3) 0.750 8 f ? d Uani 0.0221(18)
C6 C 0.1467(6) 0.3586(13) 0.2253(3) 0.750 8 f ? d Uani 0.0209(16)
C7 C 0.0925(5) 0.1537(10) 0.2924(2) 0.750 8 f ? d Uani 0.019(2)
C8 C 0.0660(6) -0.0519(8) 0.3028(2) 0.750 8 f ? d Uani 0.015(2)
C9 C 0.0295(5) -0.0932(7) 0.3453(2) 0.750 8 f ? d Uani 0.0126(19)
C10 C 0.0195(5) 0.0711(9) 0.3774(2) 0.750 8 f ? d Uani 0.013(2)
C11 C 0.0460(5) 0.2766(8) 0.3669(2) 0.750 8 f ? d Uani 0.018(2)
C12 C 0.0825(4) 0.3179(7) 0.3244(2) 0.750 8 f ? d Uani 0.0177(16)
C13 C -0.0219(7) 0.0218(17) 0.4226(3) 0.750 8 f ? d Uani 0.009(2)
S1' S 0.0579(5) 0.2679(10) 0.3544(2) 0.250 8 f ? d Uani 0.0123(12)
O3' O 0.1191(14) 0.475(3) 0.2727(7) 0.250 8 f ? d Uani 0.033(4)
N1' N 0.1504(17) 0.175(3) 0.2288(8) 0.250 8 f ? d Uani 0.024(4)
C1' C -0.009(3) 0.049(7) 0.4271(10) 0.250 8 f ? d Uani 0.026(7)
C2' C 0.018(2) 0.024(5) 0.3767(9) 0.250 8 f ? d Uani 0.021(5)
C3' C 0.019(2) -0.149(5) 0.3438(11) 0.250 8 f ? d Uani 0.023(5)
C4' C 0.062(2) -0.087(5) 0.3039(10) 0.250 8 f ? d Uani 0.019(5)
C5' C 0.085(2) 0.155(4) 0.3024(11) 0.250 8 f ? d Uani 0.016(4)
C6' C 0.1187(19) 0.285(4) 0.2672(9) 0.250 8 f ? d Uani 0.019(4)
C7' C 0.1822(17) 0.275(3) 0.1888(7) 0.250 8 f ? d Uani 0.019(4)
C8' C 0.223(2) 0.140(3) 0.1583(9) 0.250 8 f ? d Uani 0.017(5)
C9' C 0.252(2) 0.219(4) 0.1164(8) 0.250 8 f ? d Uani 0.011(5)
C10' C 0.240(2) 0.433(4) 0.1049(7) 0.250 8 f ? d Uani 0.008(5)
C11' C 0.199(2) 0.568(3) 0.1354(7) 0.250 8 f ? d Uani 0.012(5)
C12' C 0.1701(13) 0.489(3) 0.1773(6) 0.250 8 f ? d Uani 0.010(3)
C13' C 0.284(4) 0.506(9) 0.060(2) 0.250 8 f ? d Uani 0.008(7)
O1 O 0.2640(3) 0.7162(6) 0.0536(1) 1.000 8 f ? d Uani 0.0165(9)
O2 O 0.3247(3) 0.4095(6) 0.0342(1) 1.000 8 f ? d Uani 0.0168(9)
O4 O -0.0082(3) 0.1645(6) 0.4560(2) 1.000 8 f ? d Uani 0.0181(10)
O5 O -0.0647(3) -0.1448(7) 0.4275(1) 1.000 8 f ? d Uani 0.0224(10)
O11 O 0.3951(3) 1.0463(6) 0.0009(1) 1.000 8 f ? d Uani 0.021(1)
H11A H 0.4236 1.1227 -0.0224 1.000 8 f ? calc Uiso 0.02500
H11B H 0.3751 1.1193 0.0274 1.000 8 f ? calc Uiso 0.02500



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cd1 O5 . 8_554 2.171(4) no
Cd1 O11 . . 2.247(4) no
Cd1 O2 . . 2.284(4) no
Cd1 O4 . 6 2.324(4) no
Cd1 O1 . 7_565 2.409(4) no
Cd1 O1 . . 2.488(4) no
Cd1 C13' . . 2.70(6) no
Cd1 C1 . . 2.74(2) no
S1 C5 . . 1.726(9) no
S1 C2 . . 1.742(9) no
O3 C6 . . 1.223(10) no
N1 C6 . . 1.357(11) no
N1 C7 . . 1.406(8) no
C1 O1 . . 1.255(19) no
C1 O2 . . 1.301(18) no
C1 C2 . . 1.45(2) no
C2 C3 . . 1.424(12) no
C3 C4 . . 1.434(11) no
C4 C5 . . 1.410(12) no
C5 C6 . . 1.457(12) no
C7 C8 . . 1.3900 no
C7 C12 . . 1.3900 no
C8 C9 . . 1.3900 no
C9 C10 . . 1.3900 no
C10 C11 . . 1.3900 no
C10 C13 . . 1.504(8) no
C11 C12 . . 1.3900 no
C13 O5 . . 1.240(11) no
C13 O4 . . 1.301(10) no
S1' C5' . . 1.71(3) no
S1' C2' . . 1.78(3) no
O3' C6' . . 1.20(3) no
N1' C6' . . 1.40(4) no
N1' C7' . . 1.41(3) no
C1' O4 . . 1.09(3) no
C1' O5 . . 1.47(4) no
C1' C2' . . 1.525(10) no
C2' C3' . . 1.43(4) no
C3' C4' . . 1.41(4) no
C4' C5' . . 1.56(4) no
C5' C6' . . 1.42(4) no
C7' C8' . . 1.3900 no
C7' C12' . . 1.3900 no
C8' C9' . . 1.3900 no
C9' C10' . . 1.3900 no
C10' C11' . . 1.3900 no
C10' C13' . . 1.54(6) no
C11' C12' . . 1.3900 no
C13' O2 . . 1.17(5) no
C13' O1 . . 1.36(5) no
O11 H11A . . 0.9500 no
O11 H11B . . 0.9500 no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Cd1 O11 8_554 . . 98.84(15) no
O5 Cd1 O2 8_554 . . 120.54(15) no
O11 Cd1 O2 . . . 140.43(14) no
O5 Cd1 O4 8_554 . 6 96.59(17) no
O11 Cd1 O4 . . 6 85.54(15) no
O2 Cd1 O4 . . 6 86.28(15) no
O5 Cd1 O1 8_554 . 7_565 87.90(16) no
O11 Cd1 O1 . . 7_565 85.12(14) no
O2 Cd1 O1 . . 7_565 99.01(14) no
O4 Cd1 O1 6 . 7_565 170.16(13) no
O5 Cd1 O1 8_554 . . 162.56(17) no
O11 Cd1 O1 . . . 88.29(13) no
O2 Cd1 O1 . . . 55.24(12) no
O4 Cd1 O1 6 . . 99.83(15) no
O1 Cd1 O1 7_565 . . 76.81(15) no
O5 Cd1 C13' 8_554 . . 145.1(12) no
O11 Cd1 C13' . . . 115.9(11) no
O2 Cd1 C13' . . . 25.5(11) no
O4 Cd1 C13' 6 . . 89.8(12) no
O1 Cd1 C13' 7_565 . . 91.5(12) no
O1 Cd1 C13' . . . 30.1(11) no
O5 Cd1 C1 8_554 . . 147.0(4) no
O11 Cd1 C1 . . . 113.7(4) no
O2 Cd1 C1 . . . 28.2(4) no
O4 Cd1 C1 6 . . 91.7(4) no
O1 Cd1 C1 7_565 . . 89.2(4) no
O1 Cd1 C1 . . . 27.2(4) no
C5 S1 C2 . . . 93.8(4) no
C6 N1 C7 . . . 128.5(7) no
O1 C1 O2 . . . 120.5(16) no
O1 C1 C2 . . . 123.7(15) no
O2 C1 C2 . . . 115.6(14) no
O1 C1 Cd1 . . . 65.0(8) no
O2 C1 Cd1 . . . 55.9(7) no
C2 C1 Cd1 . . . 166.1(13) no
C3 C2 C1 . . . 129.9(11) no
C3 C2 S1 . . . 110.9(6) no
C1 C2 S1 . . . 119.1(10) no
C2 C3 C4 . . . 110.8(8) no
C5 C4 C3 . . . 114.8(8) no
C4 C5 C6 . . . 131.3(9) no
C4 C5 S1 . . . 109.7(7) no
C6 C5 S1 . . . 118.9(6) no
O3 C6 N1 . . . 124.6(8) no
O3 C6 C5 . . . 119.5(8) no
N1 C6 C5 . . . 115.9(7) no
C8 C7 C12 . . . 120.00 no
C8 C7 N1 . . . 115.4(5) no
C12 C7 N1 . . . 124.6(5) no
C9 C8 C7 . . . 120.00 no
C8 C9 C10 . . . 120.00 no
C9 C10 C11 . . . 120.00 no
C9 C10 C13 . . . 118.7(6) no
C11 C10 C13 . . . 121.3(6) no
C12 C11 C10 . . . 120.00 no
C11 C12 C7 . . . 120.00 no
O5 C13 O4 . . . 122.9(7) no
O5 C13 C10 . . . 121.8(7) no
O4 C13 C10 . . . 115.2(8) no
C5' S1' C2' . . . 93.5(12) no
C6' N1' C7' . . . 124.(2) no
O4 C1' O5 . . . 121.(2) no
O4 C1' C2' . . . 141.(4) no
O5 C1' C2' . . . 97.(2) no
C3' C2' C1' . . . 135.(3) no
C3' C2' S1' . . . 113.4(19) no
C1' C2' S1' . . . 112.(3) no
C4' C3' C2' . . . 110.(3) no
C3' C4' C5' . . . 114.(3) no
C6' C5' C4' . . . 132.(3) no
C6' C5' S1' . . . 120.(2) no
C4' C5' S1' . . . 108.1(19) no
O3' C6' N1' . . . 126.(3) no
O3' C6' C5' . . . 119.(3) no
N1' C6' C5' . . . 115.(2) no
C8' C7' C12' . . . 120.00 no
C8' C7' N1' . . . 115.2(15) no
C12' C7' N1' . . . 124.7(15) no
C9' C8' C7' . . . 120.00 no
C8' C9' C10' . . . 120.00 no
C11' C10' C9' . . . 120.00 no
C11' C10' C13' . . . 125.(3) no
C9' C10' C13' . . . 115.(3) no
C10' C11' C12' . . . 120.00 no
C11' C12' C7' . . . 120.00 no
O2 C13' O1 . . . 122.(4) no
O2 C13' C10' . . . 131.(4) no
O1 C13' C10' . . . 107.(4) no
O2 C13' Cd1 . . . 57.(2) no
O1 C13' Cd1 . . . 66.(2) no
C10' C13' Cd1 . . . 169.(3) no
C1 O1 Cd1 . . 7_565 115.(1) no
C1 O1 Cd1 . . . 87.8(9) no
C13' O1 Cd1 . . . 84.(2) no
Cd1 O1 Cd1 7_565 . . 103.19(15) no
C13' O2 Cd1 . . . 98.(3) no
C1 O2 Cd1 . . . 95.9(9) no
C13 O4 Cd1 . . 6_545 123.8(6) no
C13 O5 Cd1 . . 8_455 118.4(5) no
Cd1 O11 H11A . . . 120.00 no
Cd1 O11 H11B . . . 120.00 no
H11A O11 H11B . . . 120.00 no

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 . . . . 178.4(13) no
O2 C1 C2 C3 . . . . -7.(2) no
Cd1 C1 C2 C3 . . . . -56.(6) no
O1 C1 C2 S1 . . . . -6.(2) no
O2 C1 C2 S1 . . . . 169.1(11) no
Cd1 C1 C2 S1 . . . . 120.(5) no
C5 S1 C2 C3 . . . . 0.6(8) no
C5 S1 C2 C1 . . . . -176.2(13) no
C1 C2 C3 C4 . . . . 176.4(16) no
S1 C2 C3 C4 . . . . 0.1(10) no
C2 C3 C4 C5 . . . . -0.9(12) no
C3 C4 C5 C6 . . . . -177.0(11) no
C3 C4 C5 S1 . . . . 1.3(11) no
C2 S1 C5 C4 . . . . -1.1(8) no
C2 S1 C5 C6 . . . . 177.5(9) no
C7 N1 C6 O3 . . . . 3.4(16) no
C7 N1 C6 C5 . . . . -177.3(9) no
C4 C5 C6 O3 . . . . 171.2(11) no
S1 C5 C6 O3 . . . . -7.0(14) no
C4 C5 C6 N1 . . . . -8.1(16) no
S1 C5 C6 N1 . . . . 173.7(7) no
C6 N1 C7 C8 . . . . 166.3(8) no
C6 N1 C7 C12 . . . . -15.3(13) no
C12 C7 C8 C9 . . . . 0.00 no
N1 C7 C8 C9 . . . . 178.4(8) no
C7 C8 C9 C10 . . . . 0.00 no
C8 C9 C10 C11 . . . . 0.00 no
C8 C9 C10 C13 . . . . 178.8(8) no
C9 C10 C11 C12 . . . . 0.00 no
C13 C10 C11 C12 . . . . -178.8(8) no
C10 C11 C12 C7 . . . . 0.00 no
C8 C7 C12 C11 . . . . 0.00 no
N1 C7 C12 C11 . . . . -178.3(8) no
C9 C10 C13 O5 . . . . -16.1(13) no
C11 C10 C13 O5 . . . . 162.7(8) no
C9 C10 C13 O4 . . . . 163.0(7) no
C11 C10 C13 O4 . . . . -18.2(12) no
O4 C1' C2' C3' . . . . 173.(5) no
O5 C1' C2' C3' . . . . -18.(5) no
O4 C1' C2' S1' . . . . -6.(7) no
O5 C1' C2' S1' . . . . 162.(2) no
C5' S1' C2' C3' . . . . -3.(2) no
C5' S1' C2' C1' . . . . 176.(3) no
C1' C2' C3' C4' . . . . -172.(4) no
S1' C2' C3' C4' . . . . 7.(3) no
C2' C3' C4' C5' . . . . -8.(4) no
C3' C4' C5' C6' . . . . -172.(3) no
C3' C4' C5' S1' . . . . 5.(3) no
C2' S1' C5' C6' . . . . 177.(3) no
C2' S1' C5' C4' . . . . -1.(2) no
C7' N1' C6' O3' . . . . -5.(5) no
C7' N1' C6' C5' . . . . 176.(3) no
C4' C5' C6' O3' . . . . 170.(3) no
S1' C5' C6' O3' . . . . -7.(4) no
C4' C5' C6' N1' . . . . -11.(5) no
S1' C5' C6' N1' . . . . 172.(2) no
C6' N1' C7' C8' . . . . 171.(2) no
C6' N1' C7' C12' . . . . -13.(4) no
C12' C7' C8' C9' . . . . 0.00 no
N1' C7' C8' C9' . . . . 176.(2) no
C7' C8' C9' C10' . . . . 0.00 no
C8' C9' C10' C11' . . . . 0.00 no
C8' C9' C10' C13' . . . . 174.(3) no
C9' C10' C11' C12' . . . . 0.00 no
C13' C10' C11' C12' . . . . -173.(4) no
C10' C11' C12' C7' . . . . 0.00 no
C8' C7' C12' C11' . . . . 0.00 no
N1' C7' C12' C11' . . . . -176.(3) no
C11' C10' C13' O2 . . . . 174.(4) no
C9' C10' C13' O2 . . . . 1.(7) no
C11' C10' C13' O1 . . . . -8.(5) no
C9' C10' C13' O1 . . . . 179.(3) no
C11' C10' C13' Cd1 . . . . 45.(19) no
C9' C10' C13' Cd1 . . . . -128.(17) no
O2 C1 O1 Cd1 . . . 7_565 96.6(16) no
C2 C1 O1 Cd1 . . . 7_565 -88.9(18) no
Cd1 C1 O1 Cd1 . . . 7_565 103.5(5) no
O2 C1 O1 Cd1 . . . . -6.9(16) no
C2 C1 O1 Cd1 . . . . 167.6(18) no
O2 C13' O1 Cd1 . . . 7_565 90.(5) no
C10' C13' O1 Cd1 . . . 7_565 -88.(4) no
Cd1 C13' O1 Cd1 . . . 7_565 101.6(12) no
O2 C13' O1 Cd1 . . . . -12.(5) no
C10' C13' O1 Cd1 . . . . 170.(3) no
O1 C13' O2 Cd1 . . . . 13.(5) no
C10' C13' O2 Cd1 . . . . -170.(5) no
O1 C1 O2 Cd1 . . . . 7.6(18) no
C2 C1 O2 Cd1 . . . . -167.3(14) no
O5 C1' O4 Cd1 . . . 6_545 110.(3) no
C2' C1' O4 Cd1 . . . 6_545 -83.(6) no
O5 C13 O4 Cd1 . . . 6_545 99.(1) no
C10 C13 O4 Cd1 . . . 6_545 -80.1(9) no
O4 C13 O5 Cd1 . . . 8_455 3.0(13) no
C10 C13 O5 Cd1 . . . 8_455 -178.0(7) no
O4 C1' O5 Cd1 . . . 8_455 -8.(5) no
C2' C1' O5 Cd1 . . . 8_455 -179.5(17) no
_diffrn_measured_fraction_theta_full 0.990
####################################################################### 
# 
# 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_r20171026c1
_database_code_depnum_ccdc_archive 'CCDC 2059614'
loop_
_audit_author_name
_audit_author_address
'fengqin wang'
;tian kong university
China
;
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H22 N2 O14 S2 Zn2'
_chemical_formula_weight         781.32

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.878(3)
_cell_length_b                   7.6402(15)
_cell_length_c                   11.509(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.45(3)
_cell_angle_gamma                90.00
_cell_volume                     1389.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    3757
_cell_measurement_theta_min      2.5773
_cell_measurement_theta_max      27.8864

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_T_max  0.7992
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(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 saturn'
_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            12693
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2418
_reflns_number_gt                2216
_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)+(0.0590P)²+4.3235P] 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         2418
_refine_ls_number_parameters     223
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1116
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.016
_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
Zn1 Zn 0.44571(3) 0.07781(6) 0.85875(4) 0.01413(17) Uani 1 1 d . . .
S1 S 0.17738(6) 0.17259(15) 0.65484(9) 0.0223(3) Uani 1 1 d . . .
O1 O 0.34459(18) 0.0850(4) 0.7486(3) 0.0233(7) Uani 1 1 d . . .
O2 O 0.40213(17) 0.0322(4) 0.5826(3) 0.0222(7) Uani 1 1 d . . .
O3 O -0.0008(2) 0.2613(5) 0.6482(3) 0.0381(9) Uani 1 1 d . . .
O4 O -0.40151(17) 0.5715(3) 0.4844(2) 0.0159(6) Uani 1 1 d . . .
O5 O -0.43054(16) 0.3924(4) 0.3349(2) 0.0156(6) Uani 1 1 d . . .
O6 O 0.44744(17) -0.1974(4) 0.8612(2) 0.0191(6) Uani 1 1 d D . .
H6A H 0.4970(13) -0.231(5) 0.887(3) 0.023 Uiso 1 1 d D . .
H6B H 0.428(2) -0.244(5) 0.797(2) 0.023 Uiso 1 1 d D . .
O7 O 0.44706(17) 0.3492(4) 0.8765(2) 0.0194(6) Uani 1 1 d D . .
H7A H 0.4986(10) 0.383(6) 0.881(4) 0.023 Uiso 1 1 d D . .
H7B H 0.4166(19) 0.395(5) 0.926(3) 0.023 Uiso 1 1 d D . .
N1 N -0.0298(2) 0.2693(5) 0.4502(3) 0.0273(9) Uani 1 1 d . . .
H1 H -0.001(4) 0.236(7) 0.392(5) 0.041 Uiso 1 1 d . . .
C1 C 0.3409(2) 0.0688(5) 0.6382(3) 0.0144(8) Uani 1 1 d . . .
C2 C 0.2557(2) 0.1000(5) 0.5769(3) 0.0163(8) Uani 1 1 d . . .
C3 C 0.2279(3) 0.0744(5) 0.4616(4) 0.0189(9) Uani 1 1 d . . .
H3 H 0.2633 0.0330 0.4054 0.023 Uiso 1 1 calc R . .
C4 C 0.1421(3) 0.1152(5) 0.4347(4) 0.0190(9) Uani 1 1 d . . .
H4 H 0.1132 0.1042 0.3589 0.023 Uiso 1 1 calc R . .
C5 C 0.1045(3) 0.1730(6) 0.5304(4) 0.0228(9) Uani 1 1 d . . .
C6 C 0.0200(3) 0.2381(6) 0.5493(4) 0.0267(10) Uani 1 1 d . . .
C7 C -0.1185(3) 0.3251(5) 0.4418(3) 0.0178(8) Uani 1 1 d . . .
C8 C -0.1665(2) 0.2935(5) 0.3365(4) 0.0172(8) Uani 1 1 d . . .
H8 H -0.1409 0.2429 0.2732 0.021 Uiso 1 1 calc R . .
C9 C -0.2519(2) 0.3359(5) 0.3239(4) 0.0173(8) Uani 1 1 d . . .
H9 H -0.2854 0.3115 0.2529 0.021 Uiso 1 1 calc R . .
C10 C -0.2878(2) 0.4149(5) 0.4168(4) 0.0158(8) Uani 1 1 d . . .
C11 C -0.2306(2) 0.4442(4) 0.5199(3) 0.0070(7) Uani 1 1 d U . .
H11 H -0.2541 0.4960 0.5845 0.008 Uiso 1 1 calc R . .
C12 C -0.1514(3) 0.4078(6) 0.5339(4) 0.0255(10) Uani 1 1 d U . .
H12 H -0.1173 0.4362 0.6037 0.031 Uiso 1 1 calc R . .
C13 C -0.3785(2) 0.4617(5) 0.4117(3) 0.0128(8) Uani 1 1 d . . .


_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
Zn1 O1 1.950(3) . ?
Zn1 O4 1.999(3) 2_546 ?
Zn1 O5 2.023(3) 4_666 ?
Zn1 O7 2.084(3) . ?
Zn1 O6 2.103(3) . ?
S1 C2 1.694(4) . ?
S1 C5 1.754(5) . ?
O1 C1 1.272(5) . ?
O2 C1 1.246(5) . ?
O3 C6 1.228(6) . ?
O4 C13 1.262(5) . ?
O4 Zn1 1.999(3) 2_556 ?
O5 C13 1.267(5) . ?
O5 Zn1 2.023(3) 4_465 ?
O6 H6A 0.853(10) . ?
O6 H6B 0.856(10) . ?
O7 H7A 0.855(10) . ?
O7 H7B 0.853(10) . ?
N1 C6 1.346(6) . ?
N1 C7 1.467(6) . ?
N1 H1 0.88(6) . ?
C1 C2 1.483(5) . ?
C2 C3 1.373(6) . ?
C3 C4 1.403(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.466(6) . ?
C7 C12 1.378(6) . ?
C7 C8 1.390(6) . ?
C8 C9 1.387(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.442(5) . ?
C10 C13 1.480(5) . ?
C11 C12 1.283(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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
O1 Zn1 O4 104.47(12) . 2_546 ?
O1 Zn1 O5 131.24(12) . 4_666 ?
O4 Zn1 O5 123.67(11) 2_546 4_666 ?
O1 Zn1 O7 92.04(12) . . ?
O4 Zn1 O7 86.38(11) 2_546 . ?
O5 Zn1 O7 84.28(11) 4_666 . ?
O1 Zn1 O6 92.63(12) . . ?
O4 Zn1 O6 88.22(11) 2_546 . ?
O5 Zn1 O6 95.88(11) 4_666 . ?
O7 Zn1 O6 173.60(11) . . ?
C2 S1 C5 91.68(19) . . ?
C1 O1 Zn1 127.1(3) . . ?
C13 O4 Zn1 139.7(2) . 2_556 ?
C13 O5 Zn1 115.8(2) . 4_465 ?
Zn1 O6 H6A 108(3) . . ?
Zn1 O6 H6B 113(3) . . ?
H6A O6 H6B 115.4(19) . . ?
Zn1 O7 H7A 108(3) . . ?
Zn1 O7 H7B 118(3) . . ?
H7A O7 H7B 115.7(19) . . ?
C6 N1 C7 126.2(4) . . ?
C6 N1 H1 107(4) . . ?
C7 N1 H1 127(4) . . ?
O2 C1 O1 124.8(4) . . ?
O2 C1 C2 120.9(4) . . ?
O1 C1 C2 114.4(3) . . ?
C3 C2 C1 129.2(4) . . ?
C3 C2 S1 111.9(3) . . ?
C1 C2 S1 118.9(3) . . ?
C2 C3 C4 113.4(4) . . ?
C2 C3 H3 123.3 . . ?
C4 C3 H3 123.3 . . ?
C5 C4 C3 112.4(4) . . ?
C5 C4 H4 123.8 . . ?
C3 C4 H4 123.8 . . ?
C4 C5 C6 134.6(4) . . ?
C4 C5 S1 110.5(3) . . ?
C6 C5 S1 114.9(3) . . ?
O3 C6 N1 124.9(4) . . ?
O3 C6 C5 121.2(4) . . ?
N1 C6 C5 113.9(4) . . ?
C12 C7 C8 122.3(4) . . ?
C12 C7 N1 120.9(4) . . ?
C8 C7 N1 116.8(4) . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.1(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C10 C11 115.2(3) . . ?
C9 C10 C13 122.8(4) . . ?
C11 C10 C13 122.0(3) . . ?
C12 C11 C10 127.1(4) . . ?
C12 C11 H11 116.5 . . ?
C10 C11 H11 116.5 . . ?
C11 C12 C7 116.1(4) . . ?
C11 C12 H12 121.9 . . ?
C7 C12 H12 121.9 . . ?
O4 C13 O5 122.0(3) . . ?
O4 C13 C10 118.4(3) . . ?
O5 C13 C10 119.6(3) . . ?

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
O4 Zn1 O1 C1 -170.7(3) 2_546 . . . ?
O5 Zn1 O1 C1 18.3(4) 4_666 . . . ?
O7 Zn1 O1 C1 102.5(3) . . . . ?
O6 Zn1 O1 C1 -81.9(3) . . . . ?
Zn1 O1 C1 O2 5.7(6) . . . . ?
Zn1 O1 C1 C2 -173.5(2) . . . . ?
O2 C1 C2 C3 8.9(6) . . . . ?
O1 C1 C2 C3 -171.9(4) . . . . ?
O2 C1 C2 S1 -172.9(3) . . . . ?
O1 C1 C2 S1 6.3(5) . . . . ?
C5 S1 C2 C3 -0.9(3) . . . . ?
C5 S1 C2 C1 -179.4(3) . . . . ?
C1 C2 C3 C4 178.8(4) . . . . ?
S1 C2 C3 C4 0.6(5) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C3 C4 C5 C6 176.9(5) . . . . ?
C3 C4 C5 S1 -0.9(5) . . . . ?
C2 S1 C5 C4 1.0(3) . . . . ?
C2 S1 C5 C6 -177.2(3) . . . . ?
C7 N1 C6 O3 -4.2(8) . . . . ?
C7 N1 C6 C5 176.3(4) . . . . ?
C4 C5 C6 O3 170.7(5) . . . . ?
S1 C5 C6 O3 -11.7(6) . . . . ?
C4 C5 C6 N1 -9.8(8) . . . . ?
S1 C5 C6 N1 167.9(3) . . . . ?
C6 N1 C7 C12 22.5(7) . . . . ?
C6 N1 C7 C8 -158.7(4) . . . . ?
C12 C7 C8 C9 -4.0(6) . . . . ?
N1 C7 C8 C9 177.2(4) . . . . ?
C7 C8 C9 C10 1.9(6) . . . . ?
C8 C9 C10 C11 -0.4(5) . . . . ?
C8 C9 C10 C13 -178.9(4) . . . . ?
C9 C10 C11 C12 1.0(6) . . . . ?
C13 C10 C11 C12 179.5(4) . . . . ?
C10 C11 C12 C7 -2.9(6) . . . . ?
C8 C7 C12 C11 4.4(6) . . . . ?
N1 C7 C12 C11 -176.9(4) . . . . ?
Zn1 O4 C13 O5 87.4(5) 2_556 . . . ?
Zn1 O4 C13 C10 -93.2(4) 2_556 . . . ?
Zn1 O5 C13 O4 -14.0(5) 4_465 . . . ?
Zn1 O5 C13 C10 166.6(3) 4_465 . . . ?
C9 C10 C13 O4 -161.6(4) . . . . ?
C11 C10 C13 O4 20.0(5) . . . . ?
C9 C10 C13 O5 17.8(6) . . . . ?
C11 C10 C13 O5 -160.6(3) . . . . ?

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
O6 H6A O4 0.853(10) 2.24(3) 2.836(4) 127(3) 4_666
O6 H6A O2 0.853(10) 2.42(2) 3.178(4) 148(4) 2_646
O6 H6B O5 0.856(10) 1.90(2) 2.696(4) 155(3) 3_556
O7 H7A O2 0.855(10) 1.957(18) 2.774(4) 160(4) 2_656
O7 H7B O2 0.853(10) 1.93(2) 2.698(4) 150(4) 4_566

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.102
