# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1430418'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22 N2 Ni O6 S'
_chemical_formula_sum            'C30 H22 N2 Ni O6 S'
_chemical_formula_weight         597.27

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'
Ni Ni 0.3393 1.1124 '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
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   10.3795(7)
_cell_length_b                   14.1058(9)
_cell_length_c                   17.8623(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0360(10)
_cell_angle_gamma                90.00
_cell_volume                     2613.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4070
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'

_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 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14460
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4596
_reflns_number_gt                3544
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0689P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4596
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1252
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_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
C1 C 0.7985(3) 0.5981(2) 0.71183(18) 0.0380(8) Uani 1 1 d . . .
H1 H 0.8617 0.5518 0.7183 0.046 Uiso 1 1 calc R . .
C2 C 0.7226(3) 0.5966(2) 0.64661(17) 0.0365(8) Uani 1 1 d . . .
H2 H 0.7375 0.5512 0.6102 0.044 Uiso 1 1 calc R . .
C3 C 0.6247(3) 0.6621(2) 0.63516(17) 0.0353(8) Uani 1 1 d . . .
C4 C 0.6140(4) 0.7285(3) 0.6913(2) 0.0562(10) Uani 1 1 d . . .
H4 H 0.5518 0.7758 0.6864 0.067 Uiso 1 1 calc R . .
C5 C 0.6935(4) 0.7261(3) 0.7540(2) 0.0556(10) Uani 1 1 d . . .
H5 H 0.6821 0.7719 0.7907 0.067 Uiso 1 1 calc R . .
C6 C 0.5349(3) 0.6605(2) 0.56867(17) 0.0335(7) Uani 1 1 d . . .
C7 C 0.5725(3) 0.6227(2) 0.50089(16) 0.0314(7) Uani 1 1 d . . .
H7 H 0.6546 0.5972 0.4970 0.038 Uiso 1 1 calc R . .
C8 C 0.4872(3) 0.6230(2) 0.43891(16) 0.0313(7) Uani 1 1 d . . .
C9 C 0.3644(3) 0.6633(2) 0.44479(19) 0.0343(7) Uani 1 1 d . . .
C10 C 0.3246(3) 0.6995(2) 0.51359(19) 0.0388(8) Uani 1 1 d . . .
H10 H 0.2421 0.7239 0.5184 0.047 Uiso 1 1 calc R . .
C11 C 0.4102(3) 0.6975(2) 0.57268(18) 0.0373(8) Uani 1 1 d . . .
H11 H 0.3848 0.7221 0.6182 0.045 Uiso 1 1 calc R . .
C12 C 0.5066(3) 0.5885(2) 0.36325(16) 0.0304(7) Uani 1 1 d . . .
C13 C 0.6118(3) 0.5401(2) 0.33537(16) 0.0325(7) Uani 1 1 d . . .
H13 H 0.6830 0.5269 0.3667 0.039 Uiso 1 1 calc R . .
C14 C 0.6105(3) 0.5116(2) 0.26123(17) 0.0362(8) Uani 1 1 d . . .
C15 C 0.5006(3) 0.5307(2) 0.21478(18) 0.0425(8) Uani 1 1 d . . .
H15 H 0.4996 0.5111 0.1651 0.051 Uiso 1 1 calc R . .
C16 C 0.3961(3) 0.5770(2) 0.24073(18) 0.0422(8) Uani 1 1 d . . .
H16 H 0.3242 0.5887 0.2095 0.051 Uiso 1 1 calc R . .
C17 C 0.3992(3) 0.6066(2) 0.31544(18) 0.0360(7) Uani 1 1 d . . .
C18 C 0.7235(3) 0.4626(2) 0.23020(16) 0.0355(8) Uani 1 1 d . . .
C19 C 0.7920(3) 0.3940(2) 0.26943(17) 0.0376(8) Uani 1 1 d . . .
H19 H 0.7663 0.3757 0.3166 0.045 Uiso 1 1 calc R . .
C20 C 0.8985(3) 0.3522(2) 0.23909(18) 0.0394(8) Uani 1 1 d . . .
H20 H 0.9417 0.3052 0.2664 0.047 Uiso 1 1 calc R . .
C21 C 0.8737(4) 0.4415(3) 0.13291(18) 0.0481(9) Uani 1 1 d . . .
H21 H 0.9008 0.4583 0.0856 0.058 Uiso 1 1 calc R . .
C22 C 0.7656(4) 0.4845(3) 0.15911(19) 0.0497(9) Uani 1 1 d . . .
H22 H 0.7205 0.5283 0.1294 0.060 Uiso 1 1 calc R . .
C23 C 1.0418(3) 0.1826(2) 0.07011(17) 0.0324(7) Uani 1 1 d . . .
C24 C 1.2807(3) 0.4104(2) 0.06535(17) 0.0337(7) Uani 1 1 d . . .
C25 C 1.0312(3) 0.0056(2) 0.07576(16) 0.0354(7) Uani 1 1 d . . .
H25 H 1.0526 0.0091 0.1267 0.042 Uiso 1 1 calc R . .
C26 C 1.0186(3) 0.0885(2) 0.03369(16) 0.0289(7) Uani 1 1 d . . .
C27 C 0.9878(3) 0.0818(2) -0.04211(17) 0.0345(7) Uani 1 1 d . . .
H27 H 0.9799 0.1367 -0.0708 0.041 Uiso 1 1 calc R . .
C29 C 1.3919(3) 0.4579(2) 0.03042(15) 0.0306(7) Uani 1 1 d . . .
N1 N 0.9425(3) 0.37635(19) 0.17193(14) 0.0362(6) Uani 1 1 d . . .
N2 N 0.7861(3) 0.66220(17) 0.76574(14) 0.0359(6) Uani 1 1 d . . .
Ni1 Ni 1.11270(4) 0.32968(3) 0.13304(2) 0.03234(16) Uani 1 1 d . . .
O1 O 1.2860(2) 0.32279(14) 0.07785(13) 0.0402(6) Uani 1 1 d . . .
O2 O 1.1824(2) 0.45767(15) 0.08416(13) 0.0423(6) Uani 1 1 d . . .
O3 O 1.0194(2) 0.25859(14) 0.03487(12) 0.0406(6) Uani 1 1 d . . .
O4 O 1.0851(2) 0.18499(15) 0.13714(11) 0.0371(5) Uani 1 1 d . . .
S1 S 0.27390(8) 0.66358(6) 0.36115(5) 0.0439(2) Uani 1 1 d . . .
C28 C 1.5000(3) 0.4038(2) 0.01425(17) 0.0382(8) Uani 1 1 d . . .
H28 H 1.5000 0.3390 0.0237 0.046 Uiso 1 1 calc R . .
C30 C 1.3933(3) 0.5545(2) 0.01553(17) 0.0372(8) Uani 1 1 d . . .
H30 H 1.3218 0.5914 0.0258 0.045 Uiso 1 1 calc R . .
O1W O 0.0918(4) 0.8490(2) 0.59808(18) 0.0990(12) Uani 1 1 d . . .
H1WB H 0.0979 0.9048 0.5805 0.148 Uiso 1 1 d R . .
H1WC H 0.0166 0.8275 0.5882 0.148 Uiso 1 1 d R . .
O2W O 0.9622(4) 0.4047(3) 0.75737(19) 0.1166(14) Uani 1 1 d . . .
H2WA H 1.0050 0.4141 0.7981 0.175 Uiso 1 1 d R . .
H2WB H 0.9101 0.3589 0.7630 0.175 Uiso 1 1 d R . .


_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
C1 N2 1.330(4) . ?
C1 C2 1.383(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.383(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(4) . ?
C3 C6 1.483(5) . ?
C4 C5 1.368(5) . ?
C4 H4 0.9300 . ?
C5 N2 1.328(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(4) . ?
C6 C11 1.400(4) . ?
C7 C8 1.393(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.403(4) . ?
C8 C12 1.457(4) . ?
C9 C10 1.406(4) . ?
C9 S1 1.736(3) . ?
C10 C11 1.356(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.394(4) . ?
C12 C17 1.403(4) . ?
C13 C14 1.383(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.412(5) . ?
C14 C18 1.486(4) . ?
C15 C16 1.362(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(4) . ?
C16 H16 0.9300 . ?
C17 S1 1.755(3) . ?
C18 C19 1.378(5) . ?
C18 C22 1.392(4) . ?
C19 C20 1.380(4) . ?
C19 H19 0.9300 . ?
C20 N1 1.343(4) . ?
C20 H20 0.9300 . ?
C21 N1 1.343(4) . ?
C21 C22 1.373(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O3 1.260(4) . ?
C23 O4 1.264(4) . ?
C23 C26 1.494(4) . ?
C24 O1 1.256(4) . ?
C24 O2 1.274(4) . ?
C24 C29 1.490(4) . ?
C25 C27 1.383(4) 3_755 ?
C25 C26 1.394(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(4) . ?
C27 C25 1.383(4) 3_755 ?
C27 H27 0.9300 . ?
C29 C30 1.390(4) . ?
C29 C28 1.395(4) . ?
N1 Ni1 2.030(3) . ?
N2 Ni1 2.062(3) 3_766 ?
Ni1 N2 2.062(3) 3_766 ?
Ni1 O4 2.063(2) . ?
Ni1 O1 2.084(2) . ?
Ni1 O2 2.143(2) . ?
Ni1 O3 2.213(2) . ?
C28 C30 1.377(4) 3_865 ?
C28 H28 0.9300 . ?
C30 C28 1.377(4) 3_865 ?
C30 H30 0.9300 . ?
O1W H1WB 0.8500 . ?
O1W H1WC 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8501 . ?

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
N2 C1 C2 123.6(3) . . ?
N2 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 115.0(3) . . ?
C2 C3 C6 123.1(3) . . ?
C4 C3 C6 121.9(3) . . ?
C5 C4 C3 121.1(3) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
N2 C5 C4 123.9(3) . . ?
N2 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C7 C6 C11 118.4(3) . . ?
C7 C6 C3 121.0(3) . . ?
C11 C6 C3 120.6(3) . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 C12 129.2(3) . . ?
C9 C8 C12 111.1(3) . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 S1 113.7(2) . . ?
C10 C9 S1 125.8(3) . . ?
C11 C10 C9 117.9(3) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C10 C11 C6 123.3(3) . . ?
C10 C11 H11 118.3 . . ?
C6 C11 H11 118.3 . . ?
C13 C12 C17 119.1(3) . . ?
C13 C12 C8 129.1(3) . . ?
C17 C12 C8 111.8(3) . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.2(3) . . ?
C13 C14 C18 120.7(3) . . ?
C15 C14 C18 120.1(3) . . ?
C16 C15 C14 121.9(3) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 118.5(3) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C12 121.2(3) . . ?
C16 C17 S1 126.0(3) . . ?
C12 C17 S1 112.7(2) . . ?
C19 C18 C22 116.5(3) . . ?
C19 C18 C14 122.5(3) . . ?
C22 C18 C14 121.0(3) . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
N1 C20 C19 123.1(3) . . ?
N1 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N1 C21 C22 123.5(3) . . ?
N1 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C21 C22 C18 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C18 C22 H22 120.0 . . ?
O3 C23 O4 120.3(3) . . ?
O3 C23 C26 120.9(3) . . ?
O4 C23 C26 118.8(3) . . ?
O1 C24 O2 119.9(3) . . ?
O1 C24 C29 119.1(3) . . ?
O2 C24 C29 120.9(3) . . ?
C27 C25 C26 120.3(3) 3_755 . ?
C27 C25 H25 119.8 3_755 . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 119.0(3) . . ?
C27 C26 C23 121.0(3) . . ?
C25 C26 C23 120.0(3) . . ?
C25 C27 C26 120.7(3) 3_755 . ?
C25 C27 H27 119.7 3_755 . ?
C26 C27 H27 119.7 . . ?
C30 C29 C28 118.8(3) . . ?
C30 C29 C24 122.4(3) . . ?
C28 C29 C24 118.8(3) . . ?
C20 N1 C21 116.4(3) . . ?
C20 N1 Ni1 123.5(2) . . ?
C21 N1 Ni1 119.8(2) . . ?
C1 N2 C5 115.8(3) . . ?
C1 N2 Ni1 127.8(2) . 3_766 ?
C5 N2 Ni1 116.3(2) . 3_766 ?
N1 Ni1 N2 96.00(10) . 3_766 ?
N1 Ni1 O4 100.65(10) . . ?
N2 Ni1 O4 95.22(9) 3_766 . ?
N1 Ni1 O1 162.35(10) . . ?
N2 Ni1 O1 89.76(10) 3_766 . ?
O4 Ni1 O1 95.40(8) . . ?
N1 Ni1 O2 100.19(10) . . ?
N2 Ni1 O2 98.13(10) 3_766 . ?
O4 Ni1 O2 153.84(8) . . ?
O1 Ni1 O2 62.40(8) . . ?
N1 Ni1 O3 93.23(9) . . ?
N2 Ni1 O3 156.21(9) 3_766 . ?
O4 Ni1 O3 61.46(8) . . ?
O1 Ni1 O3 87.99(9) . . ?
O2 Ni1 O3 101.75(8) . . ?
C24 O1 Ni1 90.29(18) . . ?
C24 O2 Ni1 87.21(18) . . ?
C23 O3 Ni1 85.50(18) . . ?
C23 O4 Ni1 92.15(18) . . ?
C9 S1 C17 90.69(15) . . ?
C30 C28 C29 120.7(3) 3_865 . ?
C30 C28 H28 119.6 3_865 . ?
C29 C28 H28 119.6 . . ?
C28 C30 C29 120.5(3) 3_865 . ?
C28 C30 H30 119.8 3_865 . ?
C29 C30 H30 119.8 . . ?
H1WB O1W H1WC 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.066
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1430419'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H16 N2 O4 S Zn'
_chemical_formula_sum            'C26 H16 N2 O4 S Zn'
_chemical_formula_weight         517.84

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2321(10)
_cell_length_b                   10.6749(13)
_cell_length_c                   14.4681(17)
_cell_angle_alpha                68.662(2)
_cell_angle_beta                 87.955(2)
_cell_angle_gamma                72.429(2)
_cell_volume                     1125.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  0.764
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6336
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3923
_reflns_number_gt                3129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.1172P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3923
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0670
_refine_ls_wR_factor_ref         0.1819
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
C1 C 1.2354(6) 0.2508(5) 0.3511(3) 0.0469(12) Uani 1 1 d . . .
H1 H 1.3027 0.2379 0.3003 0.056 Uiso 1 1 calc R . .
C2 C 1.2363(6) 0.1340(5) 0.4328(4) 0.0475(12) Uani 1 1 d . . .
H2 H 1.3029 0.0449 0.4357 0.057 Uiso 1 1 calc R . .
C3 C 1.1390(6) 0.1467(5) 0.5115(4) 0.0450(11) Uani 1 1 d . . .
C4 C 1.0444(7) 0.2848(5) 0.5005(4) 0.0562(14) Uani 1 1 d . . .
H4 H 0.9774 0.3012 0.5506 0.067 Uiso 1 1 calc R . .
C5 C 1.0499(8) 0.3957(6) 0.4168(4) 0.0600(14) Uani 1 1 d . . .
H5 H 0.9854 0.4862 0.4120 0.072 Uiso 1 1 calc R . .
C6 C 1.1319(6) 0.0256(5) 0.6006(4) 0.0463(11) Uani 1 1 d . . .
C7 C 1.2604(7) -0.1063(5) 0.6309(4) 0.0583(14) Uani 1 1 d . . .
H7 H 1.3538 -0.1177 0.5932 0.070 Uiso 1 1 calc R . .
C8 C 1.2528(7) -0.2190(5) 0.7144(4) 0.0535(13) Uani 1 1 d . . .
H8 H 1.3416 -0.3040 0.7346 0.064 Uiso 1 1 calc R . .
C9 C 1.1085(6) -0.2028(5) 0.7679(4) 0.0454(11) Uani 1 1 d . . .
C10 C 0.9768(6) -0.0732(5) 0.7393(3) 0.0398(10) Uani 1 1 d . . .
C11 C 0.9892(6) 0.0397(5) 0.6566(4) 0.0438(11) Uani 1 1 d . . .
H11 H 0.9023 0.1257 0.6379 0.053 Uiso 1 1 calc R . .
C12 C 0.8364(6) -0.0808(4) 0.8026(3) 0.0397(10) Uani 1 1 d . . .
C13 C 0.8684(6) -0.2147(4) 0.8783(3) 0.0386(10) Uani 1 1 d . . .
C14 C 0.7478(6) -0.2452(5) 0.9451(3) 0.0443(11) Uani 1 1 d . . .
H14 H 0.7704 -0.3337 0.9959 0.053 Uiso 1 1 calc R . .
C15 C 0.5938(6) -0.1418(5) 0.9348(3) 0.0423(11) Uani 1 1 d . . .
H15 H 0.5124 -0.1615 0.9794 0.051 Uiso 1 1 calc R . .
C16 C 0.5565(6) -0.0070(4) 0.8586(3) 0.0389(10) Uani 1 1 d . . .
C17 C 0.6808(6) 0.0240(5) 0.7939(3) 0.0418(11) Uani 1 1 d . . .
H17 H 0.6602 0.1140 0.7453 0.050 Uiso 1 1 calc R . .
C18 C 0.3861(6) 0.1005(5) 0.8446(3) 0.0404(10) Uani 1 1 d . . .
C19 C 0.2406(7) 0.0612(5) 0.8689(4) 0.0507(12) Uani 1 1 d . . .
H19 H 0.2482 -0.0340 0.8967 0.061 Uiso 1 1 calc R . .
C20 C 0.0844(7) 0.1633(5) 0.8520(4) 0.0507(12) Uani 1 1 d . . .
H20 H -0.0117 0.1343 0.8704 0.061 Uiso 1 1 calc R . .
C21 C 0.2059(6) 0.3398(5) 0.7898(4) 0.0467(11) Uani 1 1 d . . .
H21 H 0.1951 0.4357 0.7636 0.056 Uiso 1 1 calc R . .
C22 C 0.3666(6) 0.2444(5) 0.8051(3) 0.0442(11) Uani 1 1 d . . .
H22 H 0.4617 0.2757 0.7893 0.053 Uiso 1 1 calc R . .
C23 C 1.3883(7) 0.5480(5) 0.3724(4) 0.0488(12) Uani 1 1 d . . .
C24 C 1.4393(7) 0.5530(5) 0.4681(4) 0.0520(12) Uani 1 1 d . . .
H24 H 1.3849 0.6321 0.4835 0.062 Uiso 1 1 calc R . .
C25 C 1.3428(6) 0.5886(5) 0.0766(3) 0.0415(11) Uani 1 1 d . . .
C26 C 1.4533(6) 0.5630(5) -0.0018(3) 0.0399(10) Uani 1 1 d . . .
H26 H 1.4570 0.6410 -0.0572 0.048 Uiso 1 1 calc R . .
N1 N 1.1429(5) 0.3822(4) 0.3408(3) 0.0465(10) Uani 1 1 d . . .
N2 N 0.0626(5) 0.3022(4) 0.8105(3) 0.0408(9) Uani 1 1 d . . .
O1 O 1.4750(5) 0.4609(4) 0.3394(3) 0.064 Uani 1 1 d . . .
O2 O 1.2450(5) 0.6377(4) 0.3291(2) 0.0528(9) Uani 1 1 d . . .
O3 O 1.2982(5) 0.7053(4) 0.0835(3) 0.0619(10) Uani 1 1 d . . .
O4 O 1.3024(4) 0.4833(4) 0.1374(2) 0.0499(8) Uani 1 1 d . . .
S1 S 1.06526(17) -0.33208(12) 0.87268(9) 0.0504(4) Uani 1 1 d . . .
Zn1 Zn 1.18131(6) 0.56132(5) 0.23272(3) 0.0394(2) 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
C1 N1 1.334(6) . ?
C1 C2 1.369(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.393(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.396(7) . ?
C3 C6 1.471(7) . ?
C4 C5 1.362(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.343(7) . ?
C5 H5 0.9300 . ?
C6 C11 1.405(7) . ?
C6 C7 1.407(7) . ?
C7 C8 1.376(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.396(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.404(6) . ?
C9 S1 1.751(5) . ?
C10 C11 1.382(6) . ?
C10 C12 1.452(6) . ?
C11 H11 0.9300 . ?
C12 C17 1.398(6) . ?
C12 C13 1.402(6) . ?
C13 C14 1.388(6) . ?
C13 S1 1.744(5) . ?
C14 C15 1.377(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.409(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(6) . ?
C16 C18 1.485(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.379(7) . ?
C18 C22 1.390(6) . ?
C19 C20 1.372(7) . ?
C19 H19 0.9300 . ?
C20 N2 1.338(6) . ?
C20 H20 0.9300 . ?
C21 N2 1.347(6) . ?
C21 C22 1.371(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O1 1.225(6) . ?
C23 O2 1.278(6) . ?
C23 C24 1.484(7) . ?
C24 C24 1.325(10) 2_866 ?
C24 H24 0.9300 . ?
C25 O3 1.228(6) . ?
C25 O4 1.279(6) . ?
C25 C26 1.480(6) . ?
C26 C26 1.315(9) 2_865 ?
C26 H26 0.9300 . ?
N1 Zn1 2.087(4) . ?
N2 Zn1 2.051(4) 2_666 ?
O2 Zn1 2.006(3) . ?
O4 Zn1 1.956(3) . ?
Zn1 N2 2.051(4) 2_666 ?

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
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 120.9(5) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C2 C3 C4 115.3(4) . . ?
C2 C3 C6 123.7(4) . . ?
C4 C3 C6 121.0(5) . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N1 C5 C4 124.0(5) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C11 C6 C7 118.1(4) . . ?
C11 C6 C3 119.2(4) . . ?
C7 C6 C3 122.7(5) . . ?
C8 C7 C6 122.3(5) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C7 C8 C9 118.4(5) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C8 C9 C10 120.9(4) . . ?
C8 C9 S1 126.9(4) . . ?
C10 C9 S1 112.2(4) . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 C12 128.3(4) . . ?
C9 C10 C12 111.9(4) . . ?
C10 C11 C6 120.6(4) . . ?
C10 C11 H11 119.7 . . ?
C6 C11 H11 119.7 . . ?
C17 C12 C13 119.7(4) . . ?
C17 C12 C10 128.2(4) . . ?
C13 C12 C10 112.0(4) . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 S1 126.4(3) . . ?
C12 C13 S1 112.5(3) . . ?
C15 C14 C13 118.6(4) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 121.7(4) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C17 C16 C15 119.1(4) . . ?
C17 C16 C18 119.7(4) . . ?
C15 C16 C18 121.1(4) . . ?
C16 C17 C12 119.6(4) . . ?
C16 C17 H17 120.2 . . ?
C12 C17 H17 120.2 . . ?
C19 C18 C22 117.4(4) . . ?
C19 C18 C16 121.1(4) . . ?
C22 C18 C16 121.4(4) . . ?
C20 C19 C18 119.7(4) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
N2 C20 C19 123.7(5) . . ?
N2 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N2 C21 C22 123.6(4) . . ?
N2 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C18 119.3(4) . . ?
C21 C22 H22 120.4 . . ?
C18 C22 H22 120.4 . . ?
O1 C23 O2 122.7(5) . . ?
O1 C23 C24 122.1(5) . . ?
O2 C23 C24 115.2(4) . . ?
C24 C24 C23 121.3(6) 2_866 . ?
C24 C24 H24 119.3 2_866 . ?
C23 C24 H24 119.3 . . ?
O3 C25 O4 122.6(5) . . ?
O3 C25 C26 120.5(4) . . ?
O4 C25 C26 116.9(4) . . ?
C26 C26 C25 124.3(5) 2_865 . ?
C26 C26 H26 117.9 2_865 . ?
C25 C26 H26 117.9 . . ?
C1 N1 C5 116.2(4) . . ?
C1 N1 Zn1 122.8(3) . . ?
C5 N1 Zn1 119.4(3) . . ?
C20 N2 C21 116.2(4) . . ?
C20 N2 Zn1 118.5(3) . 2_666 ?
C21 N2 Zn1 124.8(3) . 2_666 ?
C23 O2 Zn1 104.0(3) . . ?
C25 O4 Zn1 101.9(3) . . ?
C13 S1 C9 91.4(2) . . ?
O4 Zn1 O2 135.02(15) . . ?
O4 Zn1 N2 117.83(15) . 2_666 ?
O2 Zn1 N2 97.82(15) . 2_666 ?
O4 Zn1 N1 101.55(15) . . ?
O2 Zn1 N1 95.74(15) . . ?
N2 Zn1 N1 102.82(15) 2_666 . ?

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
N1 C1 C2 C3 -0.4(8) . . . . ?
C1 C2 C3 C4 -0.4(8) . . . . ?
C1 C2 C3 C6 179.0(5) . . . . ?
C2 C3 C4 C5 0.6(8) . . . . ?
C6 C3 C4 C5 -178.8(5) . . . . ?
C3 C4 C5 N1 0.0(10) . . . . ?
C2 C3 C6 C11 -156.4(5) . . . . ?
C4 C3 C6 C11 23.0(8) . . . . ?
C2 C3 C6 C7 21.7(8) . . . . ?
C4 C3 C6 C7 -159.0(5) . . . . ?
C11 C6 C7 C8 -1.9(8) . . . . ?
C3 C6 C7 C8 180.0(5) . . . . ?
C6 C7 C8 C9 2.8(9) . . . . ?
C7 C8 C9 C10 -2.1(8) . . . . ?
C7 C8 C9 S1 177.1(4) . . . . ?
C8 C9 C10 C11 0.5(8) . . . . ?
S1 C9 C10 C11 -178.8(4) . . . . ?
C8 C9 C10 C12 177.8(5) . . . . ?
S1 C9 C10 C12 -1.4(5) . . . . ?
C9 C10 C11 C6 0.4(7) . . . . ?
C12 C10 C11 C6 -176.5(5) . . . . ?
C7 C6 C11 C10 0.3(8) . . . . ?
C3 C6 C11 C10 178.4(4) . . . . ?
C11 C10 C12 C17 0.6(9) . . . . ?
C9 C10 C12 C17 -176.4(5) . . . . ?
C11 C10 C12 C13 178.5(5) . . . . ?
C9 C10 C12 C13 1.4(6) . . . . ?
C17 C12 C13 C14 -0.1(7) . . . . ?
C10 C12 C13 C14 -178.1(4) . . . . ?
C17 C12 C13 S1 177.3(4) . . . . ?
C10 C12 C13 S1 -0.8(5) . . . . ?
C12 C13 C14 C15 1.1(7) . . . . ?
S1 C13 C14 C15 -175.9(4) . . . . ?
C13 C14 C15 C16 0.0(7) . . . . ?
C14 C15 C16 C17 -2.2(7) . . . . ?
C14 C15 C16 C18 176.3(4) . . . . ?
C15 C16 C17 C12 3.2(7) . . . . ?
C18 C16 C17 C12 -175.3(4) . . . . ?
C13 C12 C17 C16 -2.1(7) . . . . ?
C10 C12 C17 C16 175.6(4) . . . . ?
C17 C16 C18 C19 148.1(5) . . . . ?
C15 C16 C18 C19 -30.3(7) . . . . ?
C17 C16 C18 C22 -30.9(7) . . . . ?
C15 C16 C18 C22 150.7(5) . . . . ?
C22 C18 C19 C20 1.2(8) . . . . ?
C16 C18 C19 C20 -177.8(5) . . . . ?
C18 C19 C20 N2 1.4(8) . . . . ?
N2 C21 C22 C18 -0.3(8) . . . . ?
C19 C18 C22 C21 -1.7(7) . . . . ?
C16 C18 C22 C21 177.3(4) . . . . ?
O1 C23 C24 C24 -14.1(10) . . . 2_866 ?
O2 C23 C24 C24 163.6(7) . . . 2_866 ?
O3 C25 C26 C26 159.3(6) . . . 2_865 ?
O4 C25 C26 C26 -18.4(8) . . . 2_865 ?
C2 C1 N1 C5 1.0(8) . . . . ?
C2 C1 N1 Zn1 166.3(4) . . . . ?
C4 C5 N1 C1 -0.9(9) . . . . ?
C4 C5 N1 Zn1 -166.7(5) . . . . ?
C19 C20 N2 C21 -3.3(7) . . . . ?
C19 C20 N2 Zn1 169.0(4) . . . 2_666 ?
C22 C21 N2 C20 2.7(7) . . . . ?
C22 C21 N2 Zn1 -169.0(4) . . . 2_666 ?
O1 C23 O2 Zn1 15.9(6) . . . . ?
C24 C23 O2 Zn1 -161.8(4) . . . . ?
O3 C25 O4 Zn1 -3.6(5) . . . . ?
C26 C25 O4 Zn1 174.0(3) . . . . ?
C14 C13 S1 C9 177.1(4) . . . . ?
C12 C13 S1 C9 -0.1(4) . . . . ?
C8 C9 S1 C13 -178.4(5) . . . . ?
C10 C9 S1 C13 0.9(4) . . . . ?
C25 O4 Zn1 O2 -62.8(4) . . . . ?
C25 O4 Zn1 N2 75.4(3) . . . 2_666 ?
C25 O4 Zn1 N1 -173.2(3) . . . . ?
C23 O2 Zn1 O4 -45.3(4) . . . . ?
C23 O2 Zn1 N2 171.2(3) . . . 2_666 ?
C23 O2 Zn1 N1 67.4(3) . . . . ?
C1 N1 Zn1 O4 20.2(4) . . . . ?
C5 N1 Zn1 O4 -174.9(4) . . . . ?
C1 N1 Zn1 O2 -118.0(4) . . . . ?
C5 N1 Zn1 O2 46.8(4) . . . . ?
C1 N1 Zn1 N2 142.6(4) . . . 2_666 ?
C5 N1 Zn1 N2 -52.6(4) . . . 2_666 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.106
