# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# 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_C4
_database_code_depnum_ccdc_archive 'CCDC 925921'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 Ni O4 S4'
_chemical_formula_weight         537.35

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'
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   P21

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

_cell_length_a                   12.1110(4)
_cell_length_b                   7.1701(3)
_cell_length_c                   13.5948(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.151(3)
_cell_angle_gamma                90.00
_cell_volume                     1168.61(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5096
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  1.000


_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       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            5096
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3660
_reflns_number_gt                3139
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)



_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.

 the structure was refined twinned hkl/-h-k-l and BASF was 0.57(1). The structure
 was also refined in P21/m with the majority of y coordinates 0.25 but the R value 
 was much higher at 0.09. So P21 is the correct spacegroup

;

_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)+(0.0320P)²+0.6054P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(14)
_refine_ls_number_reflns         3660
_refine_ls_number_parameters     285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_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
Ni1 Ni 0.23595(3) 0.00166(10) 0.18209(3) 0.03926(13) Uani 1 1 d . . .
S11 S 0.07376(6) 0.0067(3) 0.09641(5) 0.0422(2) Uani 1 1 d . . .
S13 S -0.16520(7) 0.0274(3) 0.11839(6) 0.0544(4) Uani 1 1 d . . .
S31 S 0.30210(6) -0.0066(3) 0.04427(6) 0.0481(3) Uani 1 1 d . . .
S33 S 0.51563(8) -0.0228(2) -0.03581(8) 0.0567(3) Uani 1 1 d . . .
C12 C -0.0260(2) 0.0216(7) 0.1731(2) 0.0329(8) Uani 1 1 d . . .
C14 C -0.0096(2) 0.0291(7) 0.2753(2) 0.0377(10) Uani 1 1 d . . .
H14 H -0.0725 0.0464 0.3063 0.045 Uiso 1 1 calc R . .
C15 C 0.0929(2) 0.0133(8) 0.3367(2) 0.0367(8) Uani 1 1 d . . .
C16 C -0.1641(3) 0.0052(12) -0.0120(2) 0.0521(10) Uani 1 1 d . . .
H16A H -0.1212 0.1050 -0.0346 0.078 Uiso 1 1 calc R . .
H16C H -0.2391 0.0107 -0.0459 0.078 Uiso 1 1 calc R . .
H16B H -0.1312 -0.1121 -0.0257 0.078 Uiso 1 1 calc R . .
C21 C 0.1016(2) 0.0041(9) 0.4463(2) 0.0343(7) Uani 1 1 d . . .
C22 C 0.1987(3) -0.0653(6) 0.5005(3) 0.0418(10) Uani 1 1 d . . .
H22 H 0.2567 -0.1038 0.4672 0.050 Uiso 1 1 calc R . .
C23 C 0.2111(3) -0.0783(6) 0.6022(3) 0.0466(11) Uani 1 1 d . . .
H23 H 0.2767 -0.1256 0.6371 0.056 Uiso 1 1 calc R . .
C24 C 0.1255(3) -0.0205(8) 0.6527(2) 0.0403(9) Uani 1 1 d . . .
C25 C 0.0283(3) 0.0520(6) 0.6005(3) 0.0417(10) Uani 1 1 d . . .
H25 H -0.0286 0.0940 0.6342 0.050 Uiso 1 1 calc R . .
C26 C 0.0170(3) 0.0614(5) 0.4980(2) 0.0378(10) Uani 1 1 d . . .
H26 H -0.0490 0.1073 0.4630 0.045 Uiso 1 1 calc R . .
C28 C 0.0575(4) 0.0065(11) 0.8087(3) 0.0699(13) Uani 1 1 d . . .
H28A H 0.0364 0.1348 0.7983 0.105 Uiso 1 1 calc R . .
H28B H 0.0822 -0.0144 0.8781 0.105 Uiso 1 1 calc R . .
H28C H -0.0054 -0.0720 0.7870 0.105 Uiso 1 1 calc R . .
C32 C 0.4434(3) -0.0174(8) 0.0663(3) 0.0399(9) Uani 1 1 d . . .
C34 C 0.5108(3) -0.0199(9) 0.1571(3) 0.0452(10) Uani 1 1 d . . .
H34 H 0.5874 -0.0271 0.1563 0.054 Uiso 1 1 calc R . .
C35 C 0.4747(2) -0.0128(9) 0.2497(3) 0.0416(9) Uani 1 1 d . . .
C41 C 0.5525(2) -0.0138(9) 0.3439(3) 0.0417(9) Uani 1 1 d . . .
C42 C 0.6610(3) -0.0882(6) 0.3521(3) 0.0481(11) Uani 1 1 d . . .
H42 H 0.6885 -0.1325 0.2961 0.058 Uiso 1 1 calc R . .
C43 C 0.7261(3) -0.0950(6) 0.4439(3) 0.0516(11) Uani 1 1 d . . .
H43 H 0.7978 -0.1439 0.4491 0.062 Uiso 1 1 calc R . .
C44 C 0.6874(3) -0.0312(8) 0.5276(3) 0.0517(13) Uani 1 1 d . . .
C45 C 0.5814(3) 0.0469(7) 0.5205(3) 0.0522(13) Uani 1 1 d . . .
H45 H 0.5558 0.0961 0.5764 0.063 Uiso 1 1 calc R . .
C46 C 0.5148(3) 0.0505(7) 0.4293(3) 0.0533(13) Uani 1 1 d . . .
H46 H 0.4426 0.0973 0.4251 0.064 Uiso 1 1 calc R . .
C48 C 0.7186(4) 0.0007(16) 0.7050(3) 0.0915(17) Uani 1 1 d . . .
H48B H 0.6963 0.1292 0.7041 0.137 Uiso 1 1 calc R . .
H48C H 0.7768 -0.0201 0.7595 0.137 Uiso 1 1 calc R . .
H48A H 0.6558 -0.0770 0.7126 0.137 Uiso 1 1 calc R . .
C36 C 0.4113(3) -0.0221(13) -0.1432(3) 0.0716(16) Uani 1 1 d . . .
H36C H 0.3619 -0.1259 -0.1400 0.107 Uiso 1 1 calc R . .
H36A H 0.4465 -0.0320 -0.2020 0.107 Uiso 1 1 calc R . .
H36B H 0.3696 0.0921 -0.1452 0.107 Uiso 1 1 calc R . .
O15 O 0.18596(16) 0.0021(8) 0.30445(15) 0.0500(7) Uani 1 1 d . . .
O27 O 0.1458(2) -0.0364(6) 0.75333(18) 0.0623(11) Uani 1 1 d . . .
O37 O 0.7581(2) -0.0437(7) 0.6147(2) 0.0776(14) Uani 1 1 d . . .
O35 O 0.37273(16) -0.0022(8) 0.26194(16) 0.0586(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
Ni1 O35 1.848(2) . ?
Ni1 O15 1.849(2) . ?
Ni1 S11 2.1371(8) . ?
Ni1 S31 2.1405(9) . ?
S11 C12 1.707(3) . ?
S13 C12 1.744(3) . ?
S13 C16 1.781(3) . ?
S31 C32 1.697(3) . ?
S33 C32 1.743(3) . ?
S33 C36 1.790(4) . ?
C12 C14 1.376(4) . ?
C14 C15 1.399(4) . ?
C14 H14 0.9300 . ?
C15 O15 1.269(3) . ?
C15 C21 1.480(4) . ?
C16 H16A 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16B 0.9600 . ?
C21 C26 1.385(5) . ?
C21 C22 1.389(5) . ?
C22 C23 1.373(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(5) . ?
C23 H23 0.9300 . ?
C24 O27 1.360(4) . ?
C24 C25 1.386(5) . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C28 O27 1.425(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C32 C34 1.380(5) . ?
C34 C35 1.391(5) . ?
C34 H34 0.9300 . ?
C35 O35 1.271(3) . ?
C35 C41 1.479(4) . ?
C41 C46 1.385(5) . ?
C41 C42 1.408(5) . ?
C42 C43 1.379(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.369(6) . ?
C43 H43 0.9300 . ?
C44 O37 1.363(4) . ?
C44 C45 1.391(5) . ?
C45 C46 1.380(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C48 O37 1.415(5) . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C48 H48A 0.9600 . ?
C36 H36C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?

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
O35 Ni1 O15 81.49(9) . . ?
O35 Ni1 S11 177.08(7) . . ?
O15 Ni1 S11 95.59(6) . . ?
O35 Ni1 S31 95.64(7) . . ?
O15 Ni1 S31 176.79(11) . . ?
S11 Ni1 S31 87.28(3) . . ?
C12 S11 Ni1 110.10(10) . . ?
C12 S13 C16 106.17(15) . . ?
C32 S31 Ni1 109.86(12) . . ?
C32 S33 C36 105.88(17) . . ?
C14 C12 S11 127.3(2) . . ?
C14 C12 S13 114.9(2) . . ?
S11 C12 S13 117.80(17) . . ?
C12 C14 C15 126.0(3) . . ?
C12 C14 H14 117.0 . . ?
C15 C14 H14 117.0 . . ?
O15 C15 C14 123.7(3) . . ?
O15 C15 C21 113.9(3) . . ?
C14 C15 C21 122.4(3) . . ?
S13 C16 H16A 109.5 . . ?
S13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
S13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16C C16 H16B 109.5 . . ?
C26 C21 C22 117.9(3) . . ?
C26 C21 C15 123.1(3) . . ?
C22 C21 C15 119.0(3) . . ?
C23 C22 C21 121.5(3) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C24 119.7(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
O27 C24 C25 124.4(3) . . ?
O27 C24 C23 115.6(3) . . ?
C25 C24 C23 120.0(3) . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C21 121.5(3) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
O27 C28 H28A 109.5 . . ?
O27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C32 S31 127.8(3) . . ?
C34 C32 S33 114.3(2) . . ?
S31 C32 S33 117.9(2) . . ?
C32 C34 C35 125.9(3) . . ?
C32 C34 H34 117.0 . . ?
C35 C34 H34 117.0 . . ?
O35 C35 C34 123.8(3) . . ?
O35 C35 C41 113.5(3) . . ?
C34 C35 C41 122.7(3) . . ?
C46 C41 C42 118.4(3) . . ?
C46 C41 C35 118.6(3) . . ?
C42 C41 C35 122.9(4) . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C44 C43 C42 121.4(4) . . ?
C44 C43 H43 119.3 . . ?
C42 C43 H43 119.3 . . ?
O37 C44 C43 116.9(4) . . ?
O37 C44 C45 123.2(4) . . ?
C43 C44 C45 119.9(4) . . ?
C46 C45 C44 119.1(4) . . ?
C46 C45 H45 120.5 . . ?
C44 C45 H45 120.5 . . ?
C45 C46 C41 121.7(4) . . ?
C45 C46 H46 119.1 . . ?
C41 C46 H46 119.1 . . ?
O37 C48 H48B 109.5 . . ?
O37 C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O37 C48 H48A 109.5 . . ?
H48B C48 H48A 109.5 . . ?
H48C C48 H48A 109.5 . . ?
S33 C36 H36C 109.5 . . ?
S33 C36 H36A 109.5 . . ?
H36C C36 H36A 109.5 . . ?
S33 C36 H36B 109.5 . . ?
H36C C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C15 O15 Ni1 137.0(2) . . ?
C24 O27 C28 118.1(3) . . ?
C44 O37 C48 119.4(4) . . ?
C35 O35 Ni1 136.9(2) . . ?

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
O35 Ni1 S11 C12 1(4) . . . . ?
O15 Ni1 S11 C12 3.3(3) . . . . ?
S31 Ni1 S11 C12 -178.2(2) . . . . ?
O35 Ni1 S31 C32 1.2(3) . . . . ?
O15 Ni1 S31 C32 -25(3) . . . . ?
S11 Ni1 S31 C32 -178.8(2) . . . . ?
Ni1 S11 C12 C14 -0.2(6) . . . . ?
Ni1 S11 C12 S13 -180.0(2) . . . . ?
C16 S13 C12 C14 -177.4(5) . . . . ?
C16 S13 C12 S11 2.4(5) . . . . ?
S11 C12 C14 C15 -4.6(9) . . . . ?
S13 C12 C14 C15 175.2(5) . . . . ?
C12 C14 C15 O15 5.0(10) . . . . ?
C12 C14 C15 C21 -173.7(5) . . . . ?
O15 C15 C21 C26 162.6(5) . . . . ?
C14 C15 C21 C26 -18.6(9) . . . . ?
O15 C15 C21 C22 -17.6(8) . . . . ?
C14 C15 C21 C22 161.2(5) . . . . ?
C26 C21 C22 C23 0.4(7) . . . . ?
C15 C21 C22 C23 -179.5(4) . . . . ?
C21 C22 C23 C24 -0.3(7) . . . . ?
C22 C23 C24 O27 -179.2(4) . . . . ?
C22 C23 C24 C25 -0.7(7) . . . . ?
O27 C24 C25 C26 180.0(5) . . . . ?
C23 C24 C25 C26 1.7(7) . . . . ?
C24 C25 C26 C21 -1.6(7) . . . . ?
C22 C21 C26 C25 0.6(7) . . . . ?
C15 C21 C26 C25 -179.6(5) . . . . ?
Ni1 S31 C32 C34 -0.3(7) . . . . ?
Ni1 S31 C32 S33 -179.3(3) . . . . ?
C36 S33 C32 C34 179.1(5) . . . . ?
C36 S33 C32 S31 -1.7(5) . . . . ?
S31 C32 C34 C35 -0.4(10) . . . . ?
S33 C32 C34 C35 178.6(5) . . . . ?
C32 C34 C35 O35 -0.3(11) . . . . ?
C32 C34 C35 C41 -179.2(6) . . . . ?
O35 C35 C41 C46 -18.8(9) . . . . ?
C34 C35 C41 C46 160.2(6) . . . . ?
O35 C35 C41 C42 157.0(5) . . . . ?
C34 C35 C41 C42 -24.0(10) . . . . ?
C46 C41 C42 C43 0.0(8) . . . . ?
C35 C41 C42 C43 -175.8(5) . . . . ?
C41 C42 C43 C44 0.2(7) . . . . ?
C42 C43 C44 O37 -179.9(5) . . . . ?
C42 C43 C44 C45 -1.8(8) . . . . ?
O37 C44 C45 C46 -178.8(5) . . . . ?
C43 C44 C45 C46 3.1(8) . . . . ?
C44 C45 C46 C41 -3.0(8) . . . . ?
C42 C41 C46 C45 1.5(8) . . . . ?
C35 C41 C46 C45 177.5(5) . . . . ?
C14 C15 O15 Ni1 0.5(11) . . . . ?
C21 C15 O15 Ni1 179.3(5) . . . . ?
O35 Ni1 O15 C15 175.7(7) . . . . ?
S11 Ni1 O15 C15 -4.2(7) . . . . ?
S31 Ni1 O15 C15 -158(3) . . . . ?
C25 C24 O27 C28 6.6(9) . . . . ?
C23 C24 O27 C28 -175.0(5) . . . . ?
C43 C44 O37 C48 -173.1(7) . . . . ?
C45 C44 O37 C48 8.9(9) . . . . ?
C34 C35 O35 Ni1 2.2(11) . . . . ?
C41 C35 O35 Ni1 -178.7(5) . . . . ?
O15 Ni1 O35 C35 176.1(8) . . . . ?
S11 Ni1 O35 C35 178(4) . . . . ?
S31 Ni1 O35 C35 -2.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_C2
_database_code_depnum_ccdc_archive 'CCDC 1055639'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 F2 Ni O2 S4'
_chemical_formula_weight         513.28

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'
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'
F F 0.0171 0.0103 '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

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

_cell_length_a                   12.2291(9)
_cell_length_b                   4.0160(4)
_cell_length_c                   23.0003(15)
_cell_angle_alpha                75.300(7)
_cell_angle_beta                 84.316(6)
_cell_angle_gamma                69.691(8)
_cell_volume                     1024.62(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8853
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.49

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  1.000


_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       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            8853
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4468
_reflns_number_gt                2966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)



_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)+(0.0330P)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         4468
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1191
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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
Ni1 Ni 0.03626(4) 0.27180(14) 0.31174(2) 0.03420(17) Uani 1 1 d . . .
S11 S -0.03721(9) -0.0175(3) 0.38806(5) 0.0397(3) Uani 1 1 d . . .
S13 S -0.26298(10) -0.1017(3) 0.43476(5) 0.0468(3) Uani 1 1 d . . .
S31 S 0.19798(9) 0.0396(3) 0.35921(5) 0.0379(3) Uani 1 1 d . . .
S33 S 0.44473(9) 0.0067(3) 0.34414(5) 0.0468(3) Uani 1 1 d . . .
C12 C -0.1813(3) 0.0785(10) 0.37566(18) 0.0309(9) Uani 1 1 d . . .
C14 C -0.2433(3) 0.2762(11) 0.32551(18) 0.0394(11) Uani 1 1 d . . .
H14 H -0.3214 0.2951 0.3263 0.047 Uiso 1 1 calc R . .
C15 C -0.2006(3) 0.4564(11) 0.27208(17) 0.0317(9) Uani 1 1 d . . .
O15 O -0.0972(2) 0.4640(8) 0.26612(12) 0.0415(7) Uani 1 1 d . . .
C16 C -0.1631(4) -0.3784(12) 0.49357(18) 0.0466(11) Uani 1 1 d . . .
H16A H -0.1025 -0.5651 0.4787 0.070 Uiso 1 1 calc R . .
H16B H -0.2036 -0.4898 0.5263 0.070 Uiso 1 1 calc R . .
H16C H -0.1294 -0.2293 0.5073 0.070 Uiso 1 1 calc R . .
C21 C -0.2738(3) 0.6534(11) 0.21880(18) 0.0333(10) Uani 1 1 d . . .
C22 C -0.2256(4) 0.8312(12) 0.16792(19) 0.0427(11) Uani 1 1 d . . .
H22 H -0.1490 0.8239 0.1691 0.051 Uiso 1 1 calc R . .
C23 C -0.2882(4) 1.0160(13) 0.1164(2) 0.0508(12) Uani 1 1 d . . .
H23 H -0.2549 1.1343 0.0831 0.061 Uiso 1 1 calc R . .
C24 C -0.3997(4) 1.0229(14) 0.1149(2) 0.0524(13) Uani 1 1 d . . .
C25 C -0.4514(4) 0.8556(12) 0.1636(2) 0.0484(12) Uani 1 1 d . . .
H25 H -0.5285 0.8687 0.1620 0.058 Uiso 1 1 calc R . .
C26 C -0.3874(4) 0.6670(12) 0.2152(2) 0.0451(12) Uani 1 1 d . . .
H26 H -0.4214 0.5475 0.2480 0.054 Uiso 1 1 calc R . .
F27 F -0.4639(3) 1.2047(9) 0.06441(13) 0.0810(10) Uani 1 1 d . . .
C32 C 0.3038(3) 0.1648(11) 0.31418(18) 0.0328(9) Uani 1 1 d . . .
C34 C 0.2936(4) 0.3812(11) 0.25735(19) 0.0390(10) Uani 1 1 d . . .
H34 H 0.3613 0.4133 0.2385 0.047 Uiso 1 1 calc R . .
C35 C 0.1908(3) 0.5579(11) 0.22527(18) 0.0352(10) Uani 1 1 d . . .
O35 O 0.0909(2) 0.5410(8) 0.24442(12) 0.0418(7) Uani 1 1 d . . .
C36 C 0.4387(4) -0.2607(12) 0.41903(19) 0.0500(12) Uani 1 1 d . . .
H36A H 0.3868 -0.1083 0.4433 0.075 Uiso 1 1 calc R . .
H36B H 0.5153 -0.3622 0.4360 0.075 Uiso 1 1 calc R . .
H36C H 0.4108 -0.4548 0.4179 0.075 Uiso 1 1 calc R . .
C41 C 0.1870(3) 0.8016(11) 0.16450(18) 0.0337(10) Uani 1 1 d . . .
C42 C 0.2829(4) 0.7389(12) 0.12487(18) 0.0436(11) Uani 1 1 d . . .
H42 H 0.3520 0.5497 0.1373 0.052 Uiso 1 1 calc R . .
C43 C 0.2743(4) 0.9608(15) 0.0669(2) 0.0558(14) Uani 1 1 d . . .
H43 H 0.3362 0.9157 0.0397 0.067 Uiso 1 1 calc R . .
C44 C 0.1741(5) 1.2436(14) 0.0509(2) 0.0539(13) Uani 1 1 d . . .
C45 C 0.0780(4) 1.3130(13) 0.0878(2) 0.0508(12) Uani 1 1 d . . .
H45 H 0.0095 1.5037 0.0750 0.061 Uiso 1 1 calc R . .
C46 C 0.0870(4) 1.0872(12) 0.14508(19) 0.0436(11) Uani 1 1 d . . .
H46 H 0.0233 1.1308 0.1712 0.052 Uiso 1 1 calc R . .
F47 F 0.1666(3) 1.4609(9) -0.00576(12) 0.0827(10) 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
Ni1 O15 1.847(3) . ?
Ni1 O35 1.860(2) . ?
Ni1 S31 2.1457(12) . ?
Ni1 S11 2.1484(10) . ?
S11 C12 1.705(4) . ?
S13 C12 1.762(3) . ?
S13 C16 1.783(4) . ?
S31 C32 1.709(3) . ?
S33 C32 1.761(4) . ?
S33 C36 1.794(4) . ?
C12 C14 1.352(5) . ?
C14 C15 1.411(5) . ?
C14 H14 0.9300 . ?
C15 O15 1.269(4) . ?
C15 C21 1.471(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 C26 1.380(5) . ?
C21 C22 1.400(5) . ?
C22 C23 1.372(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.358(6) . ?
C23 H23 0.9300 . ?
C24 F27 1.360(5) . ?
C24 C25 1.370(6) . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C32 C34 1.364(5) . ?
C34 C35 1.389(6) . ?
C34 H34 0.9300 . ?
C35 O35 1.275(4) . ?
C35 C41 1.483(5) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C41 C46 1.373(6) . ?
C41 C42 1.403(5) . ?
C42 C43 1.394(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.356(7) . ?
C43 H43 0.9300 . ?
C44 F47 1.363(5) . ?
C44 C45 1.369(6) . ?
C45 C46 1.386(6) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?

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
O15 Ni1 O35 81.21(11) . . ?
O15 Ni1 S31 176.01(8) . . ?
O35 Ni1 S31 95.99(9) . . ?
O15 Ni1 S11 95.68(8) . . ?
O35 Ni1 S11 176.58(9) . . ?
S31 Ni1 S11 87.19(4) . . ?
C12 S11 Ni1 109.12(15) . . ?
C12 S13 C16 106.64(19) . . ?
C32 S31 Ni1 109.21(15) . . ?
C32 S33 C36 107.30(19) . . ?
C14 C12 S11 128.6(3) . . ?
C14 C12 S13 114.1(3) . . ?
S11 C12 S13 117.3(2) . . ?
C12 C14 C15 126.0(4) . . ?
C12 C14 H14 117.0 . . ?
C15 C14 H14 117.0 . . ?
O15 C15 C14 123.1(4) . . ?
O15 C15 C21 114.7(3) . . ?
C14 C15 C21 122.1(3) . . ?
C15 O15 Ni1 137.2(3) . . ?
S13 C16 H16A 109.5 . . ?
S13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C26 C21 C22 117.5(4) . . ?
C26 C21 C15 123.9(4) . . ?
C22 C21 C15 118.6(3) . . ?
C23 C22 C21 121.8(4) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C24 C23 C22 118.7(4) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C23 C24 F27 119.9(4) . . ?
C23 C24 C25 121.8(4) . . ?
F27 C24 C25 118.3(4) . . ?
C24 C25 C26 119.2(4) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C21 C26 C25 121.0(4) . . ?
C21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C34 C32 S31 128.4(3) . . ?
C34 C32 S33 114.3(3) . . ?
S31 C32 S33 117.3(2) . . ?
C32 C34 C35 125.6(4) . . ?
C32 C34 H34 117.2 . . ?
C35 C34 H34 117.2 . . ?
O35 C35 C34 125.1(4) . . ?
O35 C35 C41 113.0(4) . . ?
C34 C35 C41 121.9(3) . . ?
C35 O35 Ni1 135.1(3) . . ?
S33 C36 H36A 109.5 . . ?
S33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
S33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C46 C41 C42 118.5(4) . . ?
C46 C41 C35 120.2(4) . . ?
C42 C41 C35 121.3(4) . . ?
C43 C42 C41 119.9(5) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C44 C43 C42 118.7(4) . . ?
C44 C43 H43 120.7 . . ?
C42 C43 H43 120.7 . . ?
C43 C44 F47 118.4(4) . . ?
C43 C44 C45 123.4(5) . . ?
F47 C44 C45 118.2(5) . . ?
C44 C45 C46 117.3(5) . . ?
C44 C45 H45 121.4 . . ?
C46 C45 H45 121.4 . . ?
C41 C46 C45 122.2(4) . . ?
C41 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_C3
_database_code_depnum_ccdc_archive 'CCDC 1055640'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 Ni O2 S4'
_chemical_formula_weight         577.41

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   24.946(4)
_cell_length_b                   5.8062(10)
_cell_length_c                   17.003(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.800(13)
_cell_angle_gamma                90.00
_cell_volume                     2461.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18304
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1.000


_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       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a

_diffrn_reflns_number            18304
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5584
_reflns_number_gt                3643
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)


_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)+(0.0868P)²+0.3227P] 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         5584
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.1780
_refine_ls_wR_factor_gt          0.1555
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
Ni1 Ni 0.33666(2) 0.82352(9) 0.11672(3) 0.0366(2) Uani 1 1 d . . .
S11 S 0.37936(4) 1.1055(2) 0.16897(7) 0.0460(3) Uani 1 1 d . . .
S13 S 0.36727(5) 1.4843(2) 0.28184(8) 0.0488(3) Uani 1 1 d . . .
S31 S 0.40373(4) 0.7969(2) 0.04316(8) 0.0480(3) Uani 1 1 d . . .
S33 S 0.44067(5) 0.5465(2) -0.09491(7) 0.0516(3) Uani 1 1 d . . .
C12 C 0.34067(16) 1.2421(7) 0.2335(3) 0.0360(9) Uani 1 1 d . . .
C14 C 0.28957(17) 1.1854(8) 0.2533(3) 0.0440(11) Uani 1 1 d . . .
H14 H 0.2733 1.2791 0.2899 0.053 Uiso 1 1 calc R . .
C15 C 0.25983(15) 1.0020(7) 0.2238(2) 0.0348(9) Uani 1 1 d . . .
C16 C 0.43344(18) 1.5128(8) 0.2461(3) 0.0574(14) Uani 1 1 d . . .
H16A H 0.4506 1.6439 0.2703 0.086 Uiso 1 1 calc R . .
H16B H 0.4316 1.5334 0.1901 0.086 Uiso 1 1 calc R . .
H16C H 0.4537 1.3764 0.2587 0.086 Uiso 1 1 calc R . .
C21 C 0.20386(15) 0.9613(7) 0.2497(3) 0.0357(9) Uani 1 1 d . . .
C22 C 0.17816(17) 0.7556(8) 0.2256(3) 0.0439(11) Uani 1 1 d . . .
H22 H 0.1968 0.6490 0.1960 0.053 Uiso 1 1 calc R . .
C23 C 0.12705(18) 0.7103(8) 0.2445(3) 0.0453(11) Uani 1 1 d . . .
H23 H 0.1110 0.5736 0.2276 0.054 Uiso 1 1 calc R . .
C25 C 0.04454(17) 0.8247(8) 0.3108(3) 0.0467(11) Uani 1 1 d . . .
H25 H 0.0271 0.6915 0.2937 0.056 Uiso 1 1 calc R . .
C26 C 0.01863(17) 0.9781(9) 0.3564(3) 0.0528(13) Uani 1 1 d . . .
H26 H -0.0163 0.9477 0.3711 0.063 Uiso 1 1 calc R . .
C27 C 0.04373(18) 1.1799(8) 0.3815(3) 0.0526(13) Uani 1 1 d . . .
H27 H 0.0254 1.2842 0.4122 0.063 Uiso 1 1 calc R . .
C28 C 0.09478(17) 1.2261(8) 0.3614(3) 0.0458(11) Uani 1 1 d . . .
H28 H 0.1111 1.3618 0.3786 0.055 Uiso 1 1 calc R . .
C30 C 0.17634(15) 1.1147(7) 0.2934(3) 0.0362(9) Uani 1 1 d . . .
H30 H 0.1929 1.2512 0.3093 0.043 Uiso 1 1 calc R . .
C24 C 0.09769(16) 0.8664(7) 0.2893(3) 0.0391(10) Uani 1 1 d . . .
C29 C 0.12336(16) 1.0717(7) 0.3150(3) 0.0360(9) Uani 1 1 d . . .
C32 C 0.39256(16) 0.5853(7) -0.0249(2) 0.0376(10) Uani 1 1 d . . .
C34 C 0.35016(16) 0.4371(7) -0.0300(3) 0.0403(10) Uani 1 1 d . . .
H34 H 0.3498 0.3307 -0.0709 0.048 Uiso 1 1 calc R . .
C35 C 0.30781(16) 0.4306(7) 0.0200(3) 0.0358(9) Uani 1 1 d . . .
C36 C 0.48995(19) 0.7650(10) -0.0748(3) 0.0608(14) Uani 1 1 d . . .
H36A H 0.5180 0.7529 -0.1120 0.091 Uiso 1 1 calc R . .
H36B H 0.5048 0.7451 -0.0225 0.091 Uiso 1 1 calc R . .
H36C H 0.4735 0.9140 -0.0793 0.091 Uiso 1 1 calc R . .
C41 C 0.26433(16) 0.2550(7) 0.0098(3) 0.0348(9) Uani 1 1 d . . .
C42 C 0.26975(17) 0.0569(7) -0.0380(3) 0.0403(10) Uani 1 1 d . . .
H42 H 0.3011 0.0337 -0.0650 0.048 Uiso 1 1 calc R . .
C43 C 0.22929(18) -0.0993(7) -0.0446(3) 0.0426(10) Uani 1 1 d . . .
H43 H 0.2334 -0.2283 -0.0763 0.051 Uiso 1 1 calc R . .
C44 C 0.18115(17) -0.0702(7) -0.0045(3) 0.0396(10) Uani 1 1 d . . .
C45 C 0.1381(2) -0.2273(8) -0.0101(3) 0.0493(12) Uani 1 1 d . . .
H45 H 0.1415 -0.3599 -0.0402 0.059 Uiso 1 1 calc R . .
C46 C 0.0925(2) -0.1890(9) 0.0271(3) 0.0560(14) Uani 1 1 d . . .
H46 H 0.0645 -0.2943 0.0222 0.067 Uiso 1 1 calc R . .
C47 C 0.08657(19) 0.0075(9) 0.0731(3) 0.0563(13) Uani 1 1 d . . .
H47 H 0.0548 0.0317 0.0991 0.068 Uiso 1 1 calc R . .
C48 C 0.12671(18) 0.1631(8) 0.0803(3) 0.0484(12) Uani 1 1 d . . .
H48 H 0.1221 0.2946 0.1106 0.058 Uiso 1 1 calc R . .
C49 C 0.17524(16) 0.1282(7) 0.0423(3) 0.0371(10) Uani 1 1 d . . .
C50 C 0.21833(17) 0.2863(7) 0.0481(3) 0.0399(10) Uani 1 1 d . . .
H50 H 0.2148 0.4165 0.0794 0.048 Uiso 1 1 calc R . .
O15 O 0.27543(11) 0.8568(5) 0.17497(18) 0.0391(7) Uani 1 1 d . . .
O35 O 0.30074(10) 0.5678(5) 0.07662(18) 0.0380(7) 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
Ni1 O35 1.853(3) . ?
Ni1 O15 1.856(3) . ?
Ni1 S31 2.1258(12) . ?
Ni1 S11 2.1318(12) . ?
S11 C12 1.683(4) . ?
S13 C12 1.749(4) . ?
S13 C16 1.785(5) . ?
S31 C32 1.705(5) . ?
S33 C32 1.731(4) . ?
S33 C36 1.792(5) . ?
C12 C14 1.368(5) . ?
C14 C15 1.383(6) . ?
C14 H14 0.9300 . ?
C15 O15 1.254(5) . ?
C15 C21 1.496(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 C30 1.360(6) . ?
C21 C22 1.410(6) . ?
C22 C23 1.351(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(6) . ?
C23 H23 0.9300 . ?
C25 C26 1.358(6) . ?
C25 C24 1.407(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.389(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.355(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.404(6) . ?
C28 H28 0.9300 . ?
C30 C29 1.405(5) . ?
C30 H30 0.9300 . ?
C24 C29 1.415(6) . ?
C32 C34 1.364(6) . ?
C34 C35 1.377(6) . ?
C34 H34 0.9300 . ?
C35 O35 1.267(5) . ?
C35 C41 1.495(5) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C41 C50 1.350(6) . ?
C41 C42 1.417(6) . ?
C42 C43 1.359(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.410(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.410(6) . ?
C44 C49 1.411(6) . ?
C45 C46 1.338(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.394(7) . ?
C46 H46 0.9300 . ?
C47 C48 1.351(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.404(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.414(5) . ?
C50 H50 0.9300 . ?

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
O35 Ni1 O15 83.29(12) . . ?
O35 Ni1 S31 96.07(9) . . ?
O15 Ni1 S31 175.88(10) . . ?
O35 Ni1 S11 176.52(10) . . ?
O15 Ni1 S11 96.11(9) . . ?
S31 Ni1 S11 84.77(4) . . ?
C12 S11 Ni1 110.15(15) . . ?
C12 S13 C16 104.8(2) . . ?
C32 S31 Ni1 109.70(15) . . ?
C32 S33 C36 105.3(2) . . ?
C14 C12 S11 127.2(3) . . ?
C14 C12 S13 114.9(3) . . ?
S11 C12 S13 117.9(2) . . ?
C12 C14 C15 126.1(4) . . ?
C12 C14 H14 116.9 . . ?
C15 C14 H14 116.9 . . ?
O15 C15 C14 125.7(4) . . ?
O15 C15 C21 113.6(3) . . ?
C14 C15 C21 120.7(4) . . ?
S13 C16 H16A 109.5 . . ?
S13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C30 C21 C22 118.8(4) . . ?
C30 C21 C15 123.3(4) . . ?
C22 C21 C15 117.9(4) . . ?
C23 C22 C21 121.3(4) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 121.1(4) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 120.7(4) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C28 C27 C26 120.5(4) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 120.9(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C21 C30 C29 121.4(4) . . ?
C21 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C23 C24 C25 122.8(4) . . ?
C23 C24 C29 118.1(4) . . ?
C25 C24 C29 119.1(4) . . ?
C28 C29 C30 122.1(4) . . ?
C28 C29 C24 118.6(4) . . ?
C30 C29 C24 119.3(4) . . ?
C34 C32 S31 127.4(4) . . ?
C34 C32 S33 115.3(3) . . ?
S31 C32 S33 117.3(2) . . ?
C32 C34 C35 125.9(4) . . ?
C32 C34 H34 117.0 . . ?
C35 C34 H34 117.0 . . ?
O35 C35 C34 125.4(4) . . ?
O35 C35 C41 113.5(4) . . ?
C34 C35 C41 121.0(4) . . ?
S33 C36 H36A 109.5 . . ?
S33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
S33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C50 C41 C42 119.0(4) . . ?
C50 C41 C35 118.5(4) . . ?
C42 C41 C35 122.6(4) . . ?
C43 C42 C41 120.3(4) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 121.4(4) . . ?
C42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
C45 C44 C43 123.2(4) . . ?
C45 C44 C49 118.3(4) . . ?
C43 C44 C49 118.5(4) . . ?
C46 C45 C44 121.2(5) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C45 C46 C47 120.5(4) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C48 C47 C46 120.4(5) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C47 C48 C49 120.6(5) . . ?
C47 C48 H48 119.7 . . ?
C49 C48 H48 119.7 . . ?
C48 C49 C44 118.9(4) . . ?
C48 C49 C50 122.6(4) . . ?
C44 C49 C50 118.4(4) . . ?
C41 C50 C49 122.4(4) . . ?
C41 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C15 O15 Ni1 134.5(3) . . ?
C35 O35 Ni1 135.0(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
O35 Ni1 S11 C12 -83.2(15) . . . . ?
O15 Ni1 S11 C12 -3.16(19) . . . . ?
S31 Ni1 S11 C12 172.80(17) . . . . ?
O35 Ni1 S31 C32 6.80(18) . . . . ?
O15 Ni1 S31 C32 -74.1(13) . . . . ?
S11 Ni1 S31 C32 -176.59(16) . . . . ?
Ni1 S11 C12 C14 1.4(5) . . . . ?
Ni1 S11 C12 S13 -178.54(19) . . . . ?
C16 S13 C12 C14 179.1(4) . . . . ?
C16 S13 C12 S11 -1.0(3) . . . . ?
S11 C12 C14 C15 0.4(7) . . . . ?
S13 C12 C14 C15 -179.7(4) . . . . ?
C12 C14 C15 O15 1.0(8) . . . . ?
C12 C14 C15 C21 -179.1(4) . . . . ?
O15 C15 C21 C30 -170.4(4) . . . . ?
C14 C15 C21 C30 9.8(6) . . . . ?
O15 C15 C21 C22 7.9(6) . . . . ?
C14 C15 C21 C22 -171.9(4) . . . . ?
C30 C21 C22 C23 0.5(7) . . . . ?
C15 C21 C22 C23 -177.9(4) . . . . ?
C21 C22 C23 C24 -0.3(7) . . . . ?
C24 C25 C26 C27 1.1(8) . . . . ?
C25 C26 C27 C28 -0.7(8) . . . . ?
C26 C27 C28 C29 0.1(8) . . . . ?
C22 C21 C30 C29 0.3(6) . . . . ?
C15 C21 C30 C29 178.6(4) . . . . ?
C22 C23 C24 C25 -179.5(4) . . . . ?
C22 C23 C24 C29 -0.7(7) . . . . ?
C26 C25 C24 C23 177.8(5) . . . . ?
C26 C25 C24 C29 -1.0(7) . . . . ?
C27 C28 C29 C30 -179.9(4) . . . . ?
C27 C28 C29 C24 0.1(7) . . . . ?
C21 C30 C29 C28 178.6(4) . . . . ?
C21 C30 C29 C24 -1.3(6) . . . . ?
C23 C24 C29 C28 -178.5(4) . . . . ?
C25 C24 C29 C28 0.4(6) . . . . ?
C23 C24 C29 C30 1.5(6) . . . . ?
C25 C24 C29 C30 -179.7(4) . . . . ?
Ni1 S31 C32 C34 -5.4(4) . . . . ?
Ni1 S31 C32 S33 176.17(18) . . . . ?
C36 S33 C32 C34 179.1(3) . . . . ?
C36 S33 C32 S31 -2.3(3) . . . . ?
S31 C32 C34 C35 -0.1(7) . . . . ?
S33 C32 C34 C35 178.3(4) . . . . ?
C32 C34 C35 O35 2.9(7) . . . . ?
C32 C34 C35 C41 -178.2(4) . . . . ?
O35 C35 C41 C50 13.6(6) . . . . ?
C34 C35 C41 C50 -165.4(4) . . . . ?
O35 C35 C41 C42 -166.0(4) . . . . ?
C34 C35 C41 C42 15.0(6) . . . . ?
C50 C41 C42 C43 -0.4(6) . . . . ?
C35 C41 C42 C43 179.2(4) . . . . ?
C41 C42 C43 C44 -0.1(7) . . . . ?
C42 C43 C44 C45 179.6(4) . . . . ?
C42 C43 C44 C49 1.0(6) . . . . ?
C43 C44 C45 C46 -177.9(5) . . . . ?
C49 C44 C45 C46 0.7(7) . . . . ?
C44 C45 C46 C47 -0.5(8) . . . . ?
C45 C46 C47 C48 0.6(8) . . . . ?
C46 C47 C48 C49 -0.8(8) . . . . ?
C47 C48 C49 C44 1.0(7) . . . . ?
C47 C48 C49 C50 180.0(4) . . . . ?
C45 C44 C49 C48 -1.0(6) . . . . ?
C43 C44 C49 C48 177.7(4) . . . . ?
C45 C44 C49 C50 -179.9(4) . . . . ?
C43 C44 C49 C50 -1.3(6) . . . . ?
C42 C41 C50 C49 0.1(6) . . . . ?
C35 C41 C50 C49 -179.5(4) . . . . ?
C48 C49 C50 C41 -178.1(4) . . . . ?
C44 C49 C50 C41 0.8(6) . . . . ?
C14 C15 O15 Ni1 -5.2(7) . . . . ?
C21 C15 O15 Ni1 175.0(3) . . . . ?
O35 Ni1 O15 C15 -177.7(4) . . . . ?
S31 Ni1 O15 C15 -96.4(13) . . . . ?
S11 Ni1 O15 C15 5.7(4) . . . . ?
C34 C35 O35 Ni1 2.2(7) . . . . ?
C41 C35 O35 Ni1 -176.8(3) . . . . ?
O15 Ni1 O35 C35 169.1(4) . . . . ?
S31 Ni1 O35 C35 -6.8(4) . . . . ?
S11 Ni1 O35 C35 -110.5(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_C8
_database_code_depnum_ccdc_archive 'CCDC 1055641'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 O4 Pd S4'
_chemical_formula_weight         585.03

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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-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'

_cell_length_a                   17.4781(5)
_cell_length_b                   17.4781(5)
_cell_length_c                   15.3714(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4695.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9818
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      27.46

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2368
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_T_max  1.000


_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       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            9818
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         27.46
_reflns_number_total             2626
_reflns_number_gt                1980
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)

_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)+(0.0374P)²+0.3445P] 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         2626
_refine_ls_number_parameters     143
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
Pd1 Pd 0.0000 0.7500 0.078457(17) 0.04940(13) Uani 1 2 d S . .
S11 S 0.07482(4) 0.79757(5) -0.02599(4) 0.0614(2) Uani 1 1 d . . .
S13 S 0.21734(5) 0.88307(5) -0.04974(5) 0.0623(2) Uani 1 1 d . . .
O15 O 0.06861(11) 0.78405(12) 0.17709(10) 0.0603(6) Uani 1 1 d . . .
C15 C 0.13429(15) 0.81453(15) 0.17982(15) 0.0424(6) Uani 1 1 d . . .
C14 C 0.17395(15) 0.84106(15) 0.10708(15) 0.0468(6) Uani 1 1 d . . .
H14 H 0.2210 0.8638 0.1183 0.056 Uiso 1 1 calc R . .
C12 C 0.15269(14) 0.83805(14) 0.02120(15) 0.0434(6) Uani 1 1 d . . .
C21 C 0.16580(15) 0.82097(15) 0.26871(15) 0.0435(6) Uani 1 1 d . . .
C22 C 0.13298(17) 0.77853(17) 0.33445(17) 0.0552(7) Uani 1 1 d . . .
H22 H 0.0943 0.7442 0.3202 0.066 Uiso 1 1 calc R . .
C23 C 0.15475(17) 0.78459(17) 0.41995(17) 0.0570(7) Uani 1 1 d . . .
H23 H 0.1318 0.7542 0.4622 0.068 Uiso 1 1 calc R . .
C25 C 0.24531(18) 0.8787(2) 0.37796(18) 0.0661(9) Uani 1 1 d . . .
H25 H 0.2837 0.9132 0.3928 0.079 Uiso 1 1 calc R . .
C26 C 0.22411(15) 0.87131(17) 0.29238(17) 0.0559(7) Uani 1 1 d . . .
H26 H 0.2488 0.9000 0.2499 0.067 Uiso 1 1 calc R . .
C24 C 0.21073(16) 0.83595(18) 0.44234(17) 0.0548(7) Uani 1 1 d . . .
C28 C 0.1963(2) 0.8106(2) 0.59320(18) 0.0847(12) Uani 1 1 d . . .
H28A H 0.1983 0.7564 0.5830 0.127 Uiso 1 1 calc R . .
H28B H 0.1439 0.8269 0.5954 0.127 Uiso 1 1 calc R . .
H28C H 0.2208 0.8221 0.6475 0.127 Uiso 1 1 calc R . .
C16 C 0.18680(19) 0.8597(2) -0.15777(19) 0.0706(10) Uani 1 1 d . . .
H16A H 0.1831 0.8051 -0.1636 0.106 Uiso 1 1 calc R . .
H16B H 0.2233 0.8790 -0.1990 0.106 Uiso 1 1 calc R . .
H16C H 0.1377 0.8824 -0.1686 0.106 Uiso 1 1 calc R . .
O27 O 0.23446(12) 0.84924(14) 0.52517(12) 0.0766(7) 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
Pd1 O15 2.0226(17) . ?
Pd1 O15 2.0226(17) 6_464 ?
Pd1 S11 2.2314(7) 6_464 ?
Pd1 S11 2.2314(7) . ?
S11 C12 1.697(3) . ?
S13 C12 1.757(3) . ?
S13 C16 1.792(3) . ?
O15 C15 1.266(3) . ?
C15 C14 1.395(3) . ?
C15 C21 1.477(3) . ?
C14 C12 1.372(3) . ?
C14 H14 0.9300 . ?
C21 C22 1.379(4) . ?
C21 C26 1.395(4) . ?
C22 C23 1.372(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.372(4) . ?
C23 H23 0.9300 . ?
C25 C26 1.373(4) . ?
C25 C24 1.380(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C24 O27 1.359(3) . ?
C28 O27 1.412(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
O15 Pd1 O15 82.88(10) . 6_464 ?
O15 Pd1 S11 175.17(6) . 6_464 ?
O15 Pd1 S11 94.72(5) 6_464 6_464 ?
O15 Pd1 S11 94.72(5) . . ?
O15 Pd1 S11 175.17(6) 6_464 . ?
S11 Pd1 S11 87.97(4) 6_464 . ?
C12 S11 Pd1 108.53(9) . . ?
C12 S13 C16 106.34(14) . . ?
C15 O15 Pd1 133.32(16) . . ?
O15 C15 C14 124.3(2) . . ?
O15 C15 C21 113.6(2) . . ?
C14 C15 C21 122.1(2) . . ?
C12 C14 C15 128.6(2) . . ?
C12 C14 H14 115.7 . . ?
C15 C14 H14 115.7 . . ?
C14 C12 S11 130.1(2) . . ?
C14 C12 S13 113.9(2) . . ?
S11 C12 S13 115.94(14) . . ?
C22 C21 C26 116.9(2) . . ?
C22 C21 C15 118.8(2) . . ?
C26 C21 C15 124.2(2) . . ?
C23 C22 C21 123.0(3) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C24 C23 C22 119.2(3) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C26 C25 C24 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C21 120.5(3) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
O27 C24 C23 124.4(3) . . ?
O27 C24 C25 116.5(3) . . ?
C23 C24 C25 119.2(2) . . ?
O27 C28 H28A 109.5 . . ?
O27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
S13 C16 H16A 109.5 . . ?
S13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 O27 C28 117.9(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
O15 Pd1 S11 C12 0.73(12) . . . . ?
O15 Pd1 S11 C12 60.8(7) 6_464 . . . ?
S11 Pd1 S11 C12 -175.25(11) 6_464 . . . ?
O15 Pd1 O15 C15 177.9(3) 6_464 . . . ?
S11 Pd1 O15 C15 117.5(6) 6_464 . . . ?
S11 Pd1 O15 C15 -6.3(3) . . . . ?
Pd1 O15 C15 C14 7.8(4) . . . . ?
Pd1 O15 C15 C21 -173.14(18) . . . . ?
O15 C15 C14 C12 -2.1(5) . . . . ?
C21 C15 C14 C12 178.9(3) . . . . ?
C15 C14 C12 S11 -3.7(5) . . . . ?
C15 C14 C12 S13 176.6(2) . . . . ?
Pd1 S11 C12 C14 3.2(3) . . . . ?
Pd1 S11 C12 S13 -177.21(11) . . . . ?
C16 S13 C12 C14 171.2(2) . . . . ?
C16 S13 C12 S11 -8.5(2) . . . . ?
O15 C15 C21 C22 15.8(4) . . . . ?
C14 C15 C21 C22 -165.1(3) . . . . ?
O15 C15 C21 C26 -159.8(3) . . . . ?
C14 C15 C21 C26 19.3(4) . . . . ?
C26 C21 C22 C23 0.6(4) . . . . ?
C15 C21 C22 C23 -175.4(3) . . . . ?
C21 C22 C23 C24 1.2(5) . . . . ?
C24 C25 C26 C21 1.1(5) . . . . ?
C22 C21 C26 C25 -1.7(4) . . . . ?
C15 C21 C26 C25 174.0(3) . . . . ?
C22 C23 C24 O27 177.0(3) . . . . ?
C22 C23 C24 C25 -1.8(5) . . . . ?
C26 C25 C24 O27 -178.2(3) . . . . ?
C26 C25 C24 C23 0.7(5) . . . . ?
C23 C24 O27 C28 -3.4(5) . . . . ?
C25 C24 O27 C28 175.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_C11
_database_code_depnum_ccdc_archive 'CCDC 1055642'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 O2 Pt S4'
_chemical_formula_weight         713.78

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   13.3438(5)
_cell_length_b                   16.6915(7)
_cell_length_c                   11.6650(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.870(4)
_cell_angle_gamma                90.00
_cell_volume                     2486.31(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15140
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      30.00


_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    6.005
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  1.000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         n/a
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a


_diffrn_reflns_number            15140
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7087
_reflns_number_gt                5020
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)



_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)+(0.0252P)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         7087
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_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
Pt1 Pt 0.657175(17) 0.967424(14) 0.21056(2) 0.01458(7) Uani 1 1 d . . .
O15 O 0.6980(3) 1.0715(2) 0.2985(3) 0.0183(10) Uani 1 1 d . . .
C15 C 0.6431(4) 1.1292(4) 0.3214(5) 0.0153(12) Uani 1 1 d . . .
C14 C 0.5329(4) 1.1347(4) 0.2802(5) 0.0169(13) Uani 1 1 d . . .
H14 H 0.5038 1.1810 0.3014 0.020 Uiso 1 1 calc R . .
C12 C 0.4622(4) 1.0792(4) 0.2114(5) 0.0187(14) Uani 1 1 d . . .
S11 S 0.48492(11) 0.98933(10) 0.15565(13) 0.0183(3) Uani 1 1 d . . .
S13 S 0.33252(12) 1.11029(10) 0.18146(14) 0.0223(4) Uani 1 1 d . . .
C16 C 0.2559(4) 1.0333(4) 0.0913(5) 0.0234(14) Uani 1 1 d . . .
H16A H 0.2796 1.0246 0.0221 0.035 Uiso 1 1 calc R . .
H16B H 0.1837 1.0492 0.0663 0.035 Uiso 1 1 calc R . .
H16C H 0.2632 0.9847 0.1370 0.035 Uiso 1 1 calc R . .
C21 C 0.7064(5) 1.1924(4) 0.3989(5) 0.0165(13) Uani 1 1 d . . .
C22 C 0.8139(5) 1.1879(4) 0.4273(5) 0.0174(13) Uani 1 1 d . . .
H22 H 0.8438 1.1458 0.3966 0.021 Uiso 1 1 calc R . .
C23 C 0.8800(5) 1.2449(4) 0.5010(5) 0.0181(13) Uani 1 1 d . . .
C24 C 0.9904(5) 1.2404(4) 0.5265(5) 0.0207(14) Uani 1 1 d . . .
H24 H 1.0205 1.1994 0.4938 0.025 Uiso 1 1 calc R . .
C25 C 1.0528(5) 1.2963(4) 0.5992(5) 0.0265(16) Uani 1 1 d . . .
H25 H 1.1251 1.2933 0.6156 0.032 Uiso 1 1 calc R . .
C26 C 1.0083(5) 1.3578(5) 0.6487(6) 0.0308(17) Uani 1 1 d . . .
H26 H 1.0520 1.3945 0.6995 0.037 Uiso 1 1 calc R . .
C27 C 0.9020(5) 1.3657(4) 0.6248(6) 0.0289(17) Uani 1 1 d . . .
H27 H 0.8738 1.4076 0.6578 0.035 Uiso 1 1 calc R . .
C28 C 0.8354(5) 1.3085(4) 0.5483(5) 0.0194(14) Uani 1 1 d . . .
C29 C 0.7236(5) 1.3123(4) 0.5201(5) 0.0194(14) Uani 1 1 d . . .
H29 H 0.6927 1.3533 0.5519 0.023 Uiso 1 1 calc R . .
C30 C 0.6617(5) 1.2566(4) 0.4474(5) 0.0197(14) Uani 1 1 d . . .
H30 H 0.5893 1.2606 0.4293 0.024 Uiso 1 1 calc R . .
O35 O 0.8150(3) 0.9571(3) 0.2614(4) 0.0193(10) Uani 1 1 d . . .
C35 C 0.8749(4) 0.9051(4) 0.2352(5) 0.0144(12) Uani 1 1 d . . .
C34 C 0.8414(4) 0.8365(4) 0.1660(5) 0.0165(13) Uani 1 1 d . . .
H34 H 0.8942 0.8059 0.1504 0.020 Uiso 1 1 calc R . .
C32 C 0.7401(4) 0.8075(4) 0.1172(5) 0.0172(13) Uani 1 1 d . . .
S31 S 0.62435(11) 0.84800(10) 0.11901(14) 0.0186(3) Uani 1 1 d . . .
S33 S 0.73916(12) 0.71622(10) 0.04237(15) 0.0222(4) Uani 1 1 d . . .
C36 C 0.6046(4) 0.6989(4) -0.0363(5) 0.0214(14) Uani 1 1 d . . .
H36A H 0.5746 0.7469 -0.0777 0.032 Uiso 1 1 calc R . .
H36B H 0.5674 0.6842 0.0197 0.032 Uiso 1 1 calc R . .
H36C H 0.5995 0.6564 -0.0931 0.032 Uiso 1 1 calc R . .
C41 C 0.9886(4) 0.9228(4) 0.2842(5) 0.0155(13) Uani 1 1 d . . .
C42 C 1.0186(4) 0.9879(4) 0.3654(5) 0.0151(13) Uani 1 1 d . . .
H42 H 0.9672 1.0175 0.3855 0.018 Uiso 1 1 calc R . .
C43 C 1.1217(5) 1.0079(4) 0.4147(5) 0.0210(14) Uani 1 1 d . . .
H43 H 1.1394 1.0505 0.4680 0.025 Uiso 1 1 calc R . .
C44 C 1.2013(5) 0.9642(4) 0.3850(5) 0.0160(12) Uani 1 1 d . . .
C45 C 1.3085(4) 0.9833(4) 0.4335(5) 0.0165(13) Uani 1 1 d . . .
H45 H 1.3287 1.0264 0.4856 0.020 Uiso 1 1 calc R . .
C46 C 1.3830(5) 0.9377(4) 0.4030(5) 0.0178(13) Uani 1 1 d . . .
H46 H 1.4535 0.9506 0.4346 0.021 Uiso 1 1 calc R . .
C47 C 1.3543(4) 0.8720(4) 0.3249(5) 0.0178(13) Uani 1 1 d . . .
H47 H 1.4059 0.8413 0.3066 0.021 Uiso 1 1 calc R . .
C48 C 1.2516(5) 0.8529(4) 0.2760(5) 0.0191(14) Uani 1 1 d . . .
H48 H 1.2331 0.8096 0.2240 0.023 Uiso 1 1 calc R . .
C49 C 1.1728(4) 0.8990(4) 0.3044(5) 0.0159(13) Uani 1 1 d . . .
C50 C 1.0649(4) 0.8808(4) 0.2546(5) 0.0167(13) Uani 1 1 d . . .
H50 H 1.0458 0.8389 0.2000 0.020 Uiso 1 1 calc 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
Pt1 O15 2.011(4) . ?
Pt1 O35 2.022(4) . ?
Pt1 S11 2.2299(15) . ?
Pt1 S31 2.2437(16) . ?
O15 C15 1.285(7) . ?
C15 C14 1.411(8) . ?
C15 C21 1.484(8) . ?
C14 C12 1.397(8) . ?
C12 S11 1.697(7) . ?
C12 S13 1.742(6) . ?
S13 C16 1.783(6) . ?
C21 C22 1.377(8) . ?
C21 C30 1.420(8) . ?
C22 C23 1.407(8) . ?
C23 C28 1.406(9) . ?
C23 C24 1.418(8) . ?
C24 C25 1.369(8) . ?
C25 C26 1.391(10) . ?
C26 C27 1.370(9) . ?
C27 C28 1.427(8) . ?
C28 C29 1.433(8) . ?
C29 C30 1.364(8) . ?
O35 C35 1.275(7) . ?
C35 C34 1.398(8) . ?
C35 C41 1.487(8) . ?
C34 C32 1.392(7) . ?
C32 S31 1.692(6) . ?
C32 S33 1.754(6) . ?
S33 C36 1.787(6) . ?
C41 C50 1.361(8) . ?
C41 C42 1.420(8) . ?
C42 C43 1.370(8) . ?
C43 C44 1.412(9) . ?
C44 C45 1.414(8) . ?
C44 C49 1.417(8) . ?
C45 C46 1.378(9) . ?
C46 C47 1.407(8) . ?
C47 C48 1.361(8) . ?
C48 C49 1.417(8) . ?
C49 C50 1.420(8) . ?

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
O15 Pt1 O35 79.58(16) . . ?
O15 Pt1 S11 96.26(12) . . ?
O35 Pt1 S11 175.46(13) . . ?
O15 Pt1 S31 175.55(12) . . ?
O35 Pt1 S31 96.11(12) . . ?
S11 Pt1 S31 88.07(6) . . ?
C15 O15 Pt1 131.9(4) . . ?
O15 C15 C14 125.4(5) . . ?
O15 C15 C21 113.7(5) . . ?
C14 C15 C21 121.0(5) . . ?
C12 C14 C15 128.0(6) . . ?
C14 C12 S11 129.8(5) . . ?
C14 C12 S13 112.6(5) . . ?
S11 C12 S13 117.6(3) . . ?
C12 S11 Pt1 108.6(2) . . ?
C12 S13 C16 105.7(3) . . ?
C22 C21 C30 118.3(5) . . ?
C22 C21 C15 118.5(5) . . ?
C30 C21 C15 123.2(5) . . ?
C21 C22 C23 122.3(6) . . ?
C28 C23 C22 119.2(6) . . ?
C28 C23 C24 119.3(6) . . ?
C22 C23 C24 121.4(6) . . ?
C25 C24 C23 120.2(6) . . ?
C24 C25 C26 120.3(7) . . ?
C27 C26 C25 121.8(6) . . ?
C26 C27 C28 118.9(6) . . ?
C23 C28 C27 119.5(6) . . ?
C23 C28 C29 118.3(6) . . ?
C27 C28 C29 122.2(6) . . ?
C30 C29 C28 121.0(6) . . ?
C29 C30 C21 120.9(6) . . ?
C35 O35 Pt1 131.3(4) . . ?
O35 C35 C34 125.3(5) . . ?
O35 C35 C41 114.5(5) . . ?
C34 C35 C41 120.2(5) . . ?
C32 C34 C35 129.1(6) . . ?
C34 C32 S31 129.6(5) . . ?
C34 C32 S33 111.8(5) . . ?
S31 C32 S33 118.6(3) . . ?
C32 S31 Pt1 107.9(2) . . ?
C32 S33 C36 104.9(3) . . ?
C50 C41 C42 118.4(5) . . ?
C50 C41 C35 123.8(5) . . ?
C42 C41 C35 117.8(5) . . ?
C43 C42 C41 121.4(6) . . ?
C42 C43 C44 120.4(6) . . ?
C43 C44 C45 122.1(6) . . ?
C43 C44 C49 118.9(5) . . ?
C45 C44 C49 119.0(6) . . ?
C46 C45 C44 119.6(6) . . ?
C45 C46 C47 121.1(5) . . ?
C48 C47 C46 120.4(6) . . ?
C47 C48 C49 120.1(6) . . ?
C48 C49 C44 119.8(5) . . ?
C48 C49 C50 121.5(5) . . ?
C44 C49 C50 118.7(6) . . ?
C41 C50 C49 122.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         2.157
_refine_diff_density_min         -2.435
_refine_diff_density_rms         0.249
