# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 Ni O4 S4'
_chemical_formula_weight         513.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   4.7556(2)
_cell_length_b                   5.8030(4)
_cell_length_c                   39.1558(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.537(4)
_cell_angle_gamma                90.00
_cell_volume                     1080.53(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7232
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      30.00

_exptl_crystal_description       needle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.914
_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            7232
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         30.00
_reflns_number_total             3156
_reflns_number_gt                2500
_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)+(0.0282P)²+0.8011P] 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         3156
_refine_ls_number_parameters     134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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 0.0000 0.0000 0.0000 0.01953(15) Uani 1 2 d S . .
S11 S -0.29201(17) -0.27679(13) 0.01507(2) 0.02302(18) Uani 1 1 d . . .
S13 S -0.08357(17) 0.09902(13) 0.05361(2) 0.02151(18) Uani 1 1 d . . .
C12 C -0.2950(6) -0.1363(5) 0.05296(8) 0.0176(6) Uani 1 1 d . . .
O14 O -0.4405(4) -0.1954(3) 0.07967(5) 0.0200(5) Uani 1 1 d . . .
C15 C -0.6237(6) -0.3983(5) 0.07668(8) 0.0198(6) Uani 1 1 d . . .
H15A H -0.5130 -0.5345 0.0718 0.024 Uiso 1 1 calc R . .
H15B H -0.7597 -0.3766 0.0583 0.024 Uiso 1 1 calc R . .
C16 C -0.7723(6) -0.4259(6) 0.11040(8) 0.0227(7) Uani 1 1 d . . .
H16A H -0.8724 -0.2845 0.1155 0.027 Uiso 1 1 calc R . .
H16B H -0.9103 -0.5483 0.1083 0.027 Uiso 1 1 calc R . .
C21 C -0.5763(6) -0.4810(5) 0.13985(8) 0.0196(6) Uani 1 1 d . . .
C22 C -0.4282(6) -0.6861(5) 0.14096(8) 0.0216(6) Uani 1 1 d . . .
H22 H -0.4524 -0.7920 0.1233 0.026 Uiso 1 1 calc R . .
C23 C -0.2430(6) -0.7390(5) 0.16787(8) 0.0226(7) Uani 1 1 d . . .
H23 H -0.1439 -0.8771 0.1680 0.027 Uiso 1 1 calc R . .
C24 C -0.2096(6) -0.5813(5) 0.19440(8) 0.0205(6) Uani 1 1 d . . .
C25 C -0.3559(6) -0.3750(6) 0.19348(8) 0.0246(7) Uani 1 1 d . . .
H25 H -0.3324 -0.2686 0.2110 0.029 Uiso 1 1 calc R . .
C26 C -0.5370(6) -0.3264(5) 0.16650(8) 0.0233(7) Uani 1 1 d . . .
H26 H -0.6342 -0.1873 0.1663 0.028 Uiso 1 1 calc R . .
O27 O -0.0401(5) -0.6161(4) 0.22243(6) 0.0281(5) Uani 1 1 d . . .
C28 C 0.1302(7) -0.8184(6) 0.22270(9) 0.0305(8) Uani 1 1 d . . .
H28A H 0.0117 -0.9523 0.2230 0.046 Uiso 1 1 calc R . .
H28B H 0.2490 -0.8178 0.2427 0.046 Uiso 1 1 calc R . .
H28C H 0.2444 -0.8212 0.2026 0.046 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0291(3) 0.0146(3) 0.0148(3) -0.0016(2) -0.0017(2) -0.0053(2)
S11 0.0332(4) 0.0186(4) 0.0172(4) -0.0038(3) -0.0023(3) -0.0086(3)
S13 0.0308(4) 0.0162(4) 0.0175(4) -0.0035(3) -0.0007(3) -0.0060(3)
C12 0.0204(14) 0.0159(14) 0.0165(15) 0.0010(11) -0.0050(12) 0.0028(11)
O14 0.0221(10) 0.0181(10) 0.0197(11) -0.0011(9) -0.0048(9) -0.0033(8)
C15 0.0186(14) 0.0176(14) 0.0231(16) 0.0010(12) -0.0030(12) -0.0021(12)
C16 0.0187(14) 0.0248(16) 0.0247(17) -0.0007(13) -0.0001(13) -0.0022(12)
C21 0.0182(13) 0.0200(15) 0.0207(15) 0.0011(12) 0.0030(12) -0.0050(12)
C22 0.0256(15) 0.0211(15) 0.0180(16) -0.0027(12) 0.0008(13) -0.0053(12)
C23 0.0238(15) 0.0221(16) 0.0221(17) 0.0007(13) 0.0038(13) -0.0009(12)
C24 0.0182(14) 0.0261(16) 0.0173(15) 0.0029(12) 0.0014(12) -0.0063(12)
C25 0.0277(16) 0.0238(16) 0.0223(17) -0.0057(13) 0.0024(14) -0.0061(13)
C26 0.0235(15) 0.0200(15) 0.0264(18) -0.0044(13) 0.0034(14) -0.0025(12)
O27 0.0299(12) 0.0332(13) 0.0212(12) -0.0005(10) -0.0048(10) -0.0008(10)
C28 0.0288(17) 0.035(2) 0.0278(19) 0.0035(15) -0.0044(15) -0.0042(15)

_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 S11 2.2072(8) . ?
Ni1 S11 2.2072(8) 3 ?
Ni1 S13 2.2161(8) 3 ?
Ni1 S13 2.2161(8) . ?
S11 C12 1.693(3) . ?
S13 C12 1.696(3) . ?
C12 O14 1.305(3) . ?
O14 C15 1.468(3) . ?
C15 C16 1.512(4) . ?
C16 C21 1.510(4) . ?
C21 C22 1.384(4) . ?
C21 C26 1.388(4) . ?
C22 C23 1.401(4) . ?
C23 C24 1.392(4) . ?
C24 O27 1.371(4) . ?
C24 C25 1.385(4) . ?
C25 C26 1.386(4) . ?
O27 C28 1.426(4) . ?

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
S11 Ni1 S11 180 . 3 ?
S11 Ni1 S13 100.57(3) . 3 ?
S11 Ni1 S13 79.43(3) 3 3 ?
S11 Ni1 S13 79.43(3) . . ?
S11 Ni1 S13 100.57(3) 3 . ?
S13 Ni1 S13 180 3 . ?
C12 S11 Ni1 83.94(10) . . ?
C12 S13 Ni1 83.60(11) . . ?
O14 C12 S11 125.8(2) . . ?
O14 C12 S13 121.2(2) . . ?
S11 C12 S13 113.02(17) . . ?
C12 O14 C15 117.7(2) . . ?
O14 C15 C16 107.3(2) . . ?
C21 C16 C15 113.5(2) . . ?
C22 C21 C26 117.9(3) . . ?
C22 C21 C16 121.1(3) . . ?
C26 C21 C16 121.0(3) . . ?
C21 C22 C23 121.9(3) . . ?
C24 C23 C22 118.9(3) . . ?
O27 C24 C25 116.1(3) . . ?
O27 C24 C23 124.3(3) . . ?
C25 C24 C23 119.7(3) . . ?
C24 C25 C26 120.3(3) . . ?
C25 C26 C21 121.3(3) . . ?
C24 O27 C28 117.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 997873'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H28 N2 Ni O4 S4'
_chemical_formula_weight         523.37

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.2640(13)
_cell_length_b                   6.4556(14)
_cell_length_c                   14.969(3)
_cell_angle_alpha                78.985(17)
_cell_angle_beta                 86.378(16)
_cell_angle_gamma                86.602(17)
_cell_volume                     592.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4224
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             274
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.894
_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_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            4224
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2600
_reflns_number_gt                1576
_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)+(0.0744P)²+0.0633P] 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         2600
_refine_ls_number_parameters     134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_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 0.0000 0.0000 0.0000 0.0553(3) Uani 1 2 d S . .
S11 S 0.22088(18) -0.06640(17) -0.11302(8) 0.0631(4) Uani 1 1 d . . .
C12 C 0.3381(7) 0.1631(6) -0.1031(3) 0.0533(10) Uani 1 1 d . . .
S13 S 0.19337(19) 0.27874(18) -0.02269(8) 0.0653(4) Uani 1 1 d . . .
N14 N 0.5094(6) 0.2359(5) -0.1486(3) 0.0588(9) Uani 1 1 d . . .
C15 C 0.6369(8) 0.1183(7) -0.2107(3) 0.0734(14) Uani 1 1 d . . .
H15A H 0.5472 0.0188 -0.2297 0.088 Uiso 1 1 calc R . .
H15B H 0.7538 0.0383 -0.1784 0.088 Uiso 1 1 calc R . .
C16 C 0.7253(9) 0.2616(8) -0.2926(4) 0.0827(15) Uani 1 1 d . . .
H16A H 0.6084 0.3290 -0.3287 0.099 Uiso 1 1 calc R . .
H16B H 0.8149 0.1794 -0.3295 0.099 Uiso 1 1 calc R . .
C17 C 0.8562(9) 0.4300(8) -0.2672(4) 0.0781(14) Uani 1 1 d . . .
H17 H 0.9759 0.3604 -0.2320 0.094 Uiso 1 1 calc R . .
C18 C 0.7149(8) 0.5502(7) -0.2075(3) 0.0731(13) Uani 1 1 d . . .
H18A H 0.7987 0.6538 -0.1881 0.088 Uiso 1 1 calc R . .
H18B H 0.6008 0.6260 -0.2430 0.088 Uiso 1 1 calc R . .
C19 C 0.6193(7) 0.4133(6) -0.1257(3) 0.0698(13) Uani 1 1 d . . .
H19A H 0.7312 0.3577 -0.0845 0.084 Uiso 1 1 calc R . .
H19B H 0.5175 0.4975 -0.0943 0.084 Uiso 1 1 calc R . .
C20 C 0.9433(12) 0.5757(12) -0.3478(5) 0.106(2) Uani 1 1 d . . .
O21 O 0.8364(11) 0.6728(12) -0.4060(5) 0.223(4) Uani 1 1 d . . .
O22 O 1.1393(9) 0.5907(11) -0.3531(4) 0.162(2) Uani 1 1 d . . .
C23 C 1.251(2) 0.732(2) -0.4307(9) 0.215(6) Uani 1 1 d . . .
H23A H 1.3958 0.6765 -0.4413 0.258 Uiso 1 1 calc R . .
H23B H 1.1749 0.7427 -0.4859 0.258 Uiso 1 1 calc R . .
C24 C 1.255(3) 0.923(2) -0.4074(10) 0.300(10) Uani 1 1 d . . .
H24A H 1.1210 1.0000 -0.4203 0.450 Uiso 1 1 calc R . .
H24B H 1.3692 1.0003 -0.4418 0.450 Uiso 1 1 calc R . .
H24C H 1.2775 0.9059 -0.3435 0.450 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0532(5) 0.0511(4) 0.0647(6) -0.0171(4) -0.0086(4) -0.0033(3)
S11 0.0633(7) 0.0520(6) 0.0788(8) -0.0243(6) -0.0011(6) -0.0074(5)
C12 0.057(2) 0.046(2) 0.058(3) -0.0132(19) -0.011(2) 0.0062(19)
S13 0.0650(7) 0.0603(6) 0.0775(8) -0.0311(6) 0.0038(6) -0.0095(5)
N14 0.068(2) 0.0412(17) 0.071(2) -0.0206(17) -0.001(2) -0.0008(16)
C15 0.079(3) 0.054(3) 0.091(4) -0.028(3) 0.012(3) -0.003(2)
C16 0.088(4) 0.082(3) 0.081(4) -0.024(3) 0.013(3) -0.011(3)
C17 0.077(3) 0.066(3) 0.084(4) 0.001(3) 0.001(3) -0.006(3)
C18 0.081(3) 0.054(2) 0.081(3) -0.003(2) -0.003(3) -0.010(2)
C19 0.075(3) 0.053(2) 0.085(4) -0.022(3) 0.001(3) -0.012(2)
C20 0.094(5) 0.125(5) 0.086(5) 0.011(4) -0.002(4) -0.008(4)
O21 0.140(5) 0.277(8) 0.187(6) 0.125(6) -0.004(5) -0.032(5)
O22 0.113(4) 0.243(7) 0.104(4) 0.041(4) 0.016(3) -0.060(4)
C23 0.169(10) 0.243(14) 0.180(11) 0.065(11) 0.046(8) 0.018(11)
C24 0.36(2) 0.287(18) 0.182(12) 0.064(13) 0.089(13) 0.131(18)

_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 S11 2.2071(12) 2 ?
Ni1 S11 2.2071(12) . ?
Ni1 S13 2.1893(12) . ?
Ni1 S13 2.1893(12) 2 ?
S11 C12 1.727(4) . ?
S13 C12 1.718(4) . ?
N14 C12 1.297(6) . ?
N14 C15 1.477(5) . ?
N14 C19 1.475(5) . ?
C15 C16 1.485(7) . ?
C16 C17 1.518(7) . ?
C17 C18 1.505(7) . ?
C17 C20 1.477(9) . ?
C18 C19 1.482(6) . ?
C20 O21 1.190(8) . ?
C20 O22 1.233(8) . ?
O22 C23 1.497(12) . ?
C23 C24 1.347(17) . ?

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
S13 Ni1 S13 180 . 2 ?
S13 Ni1 S11 100.53(4) . 2 ?
S13 Ni1 S11 79.47(4) 2 2 ?
S13 Ni1 S11 79.47(4) . . ?
S13 Ni1 S11 100.53(4) 2 . ?
S11 Ni1 S11 180 2 . ?
C12 S11 Ni1 85.11(15) . . ?
N14 C12 S13 125.3(3) . . ?
N14 C12 S11 125.3(3) . . ?
S13 C12 S11 109.3(3) . . ?
C12 S13 Ni1 85.88(15) . . ?
C12 N14 C19 121.9(3) . . ?
C12 N14 C15 122.4(3) . . ?
C19 N14 C15 114.2(4) . . ?
N14 C15 C16 111.9(3) . . ?
C15 C16 C17 111.8(4) . . ?
C20 C17 C18 110.4(4) . . ?
C20 C17 C16 112.6(5) . . ?
C18 C17 C16 108.0(4) . . ?
C19 C18 C17 113.4(4) . . ?
N14 C19 C18 112.4(4) . . ?
O21 C20 O22 120.3(8) . . ?
O21 C20 C17 123.8(7) . . ?
O22 C20 C17 115.9(7) . . ?
C20 O22 C23 122.2(8) . . ?
O22 C23 C24 107.1(13) . . ?

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.072
_database_code_depnum_ccdc_archive 'CCDC 997874'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H20 N2 Ni O4 S4'
_chemical_formula_weight         563.35

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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   5.6942(9)
_cell_length_b                   18.8463(14)
_cell_length_c                   10.8100(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.696(9)
_cell_angle_gamma                90.00
_cell_volume                     1160.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5412
_cell_measurement_theta_min      3.58
_cell_measurement_theta_max      30.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.877
_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            5412
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         30.00
_reflns_number_total             3292
_reflns_number_gt                2213
_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)+(0.0285P)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         3292
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_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 0.0000 0.0000 0.0000 0.01617(16) Uani 1 2 d S . .
S11 S 0.15548(16) 0.01173(5) -0.18436(8) 0.0185(2) Uani 1 1 d . . .
S13 S 0.27912(15) -0.08018(5) 0.01070(8) 0.0180(2) Uani 1 1 d . . .
C12 C 0.3466(6) -0.05413(17) -0.1378(3) 0.0156(7) Uani 1 1 d . . .
N14 N 0.5163(5) -0.08047(14) -0.2050(2) 0.0154(6) Uani 1 1 d . . .
C21 C 0.6827(6) -0.13249(18) -0.1500(3) 0.0190(7) Uani 1 1 d . . .
H21A H 0.6105 -0.1538 -0.0782 0.023 Uiso 1 1 calc R . .
H21B H 0.8220 -0.1074 -0.1217 0.023 Uiso 1 1 calc R . .
C22 C 0.7552(6) -0.18999(18) -0.2354(3) 0.0186(7) Uani 1 1 d . . .
C23 C 0.9526(6) -0.2029(2) -0.2974(3) 0.0251(8) Uani 1 1 d . . .
H23 H 1.0851 -0.1742 -0.3007 0.030 Uiso 1 1 calc R . .
C24 C 0.9189(8) -0.2694(2) -0.3573(4) 0.0345(10) Uani 1 1 d . . .
H24 H 1.0251 -0.2923 -0.4084 0.041 Uiso 1 1 calc R . .
C25 C 0.7078(8) -0.2924(2) -0.3266(4) 0.0324(10) Uani 1 1 d . . .
H25 H 0.6428 -0.3352 -0.3525 0.039 Uiso 1 1 calc R . .
O26 O 0.5984(4) -0.24452(13) -0.2516(2) 0.0257(6) Uani 1 1 d . . .
C31 C 0.5680(6) -0.05134(18) -0.3294(3) 0.0186(7) Uani 1 1 d . . .
H31A H 0.5322 -0.0010 -0.3299 0.022 Uiso 1 1 calc R . .
H31B H 0.7347 -0.0565 -0.3447 0.022 Uiso 1 1 calc R . .
C32 C 0.4347(6) -0.08610(18) -0.4313(3) 0.0176(7) Uani 1 1 d . . .
C33 C 0.4736(6) -0.14283(19) -0.5054(3) 0.0233(8) Uani 1 1 d . . .
H33 H 0.6057 -0.1719 -0.5049 0.028 Uiso 1 1 calc R . .
C34 C 0.2714(7) -0.1492(2) -0.5846(3) 0.0257(8) Uani 1 1 d . . .
H34 H 0.2468 -0.1831 -0.6459 0.031 Uiso 1 1 calc R . .
C35 C 0.1251(6) -0.09718(19) -0.5535(3) 0.0231(8) Uani 1 1 d . . .
H35 H -0.0207 -0.0893 -0.5907 0.028 Uiso 1 1 calc R . .
O261 O 0.2178(4) -0.05692(13) -0.4597(2) 0.0219(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0191(3) 0.0178(3) 0.0117(3) 0.0000(3) 0.0002(2) 0.0007(3)
S11 0.0226(5) 0.0191(4) 0.0139(4) 0.0014(3) 0.0007(4) 0.0035(4)
S13 0.0209(4) 0.0200(4) 0.0130(4) 0.0024(3) 0.0000(3) 0.0022(4)
C12 0.0201(17) 0.0133(15) 0.0134(15) -0.0024(13) -0.0034(14) -0.0048(14)
N14 0.0192(15) 0.0142(13) 0.0128(13) -0.0002(11) 0.0003(12) -0.0006(12)
C21 0.0202(18) 0.0210(17) 0.0157(17) -0.0034(14) -0.0036(14) 0.0043(15)
C22 0.0217(19) 0.0175(17) 0.0164(17) 0.0020(14) -0.0022(15) -0.0032(14)
C23 0.023(2) 0.027(2) 0.025(2) 0.0034(16) 0.0016(16) 0.0036(17)
C24 0.045(3) 0.036(2) 0.023(2) -0.0053(18) 0.002(2) 0.020(2)
C25 0.054(3) 0.0173(18) 0.026(2) -0.0064(16) -0.007(2) 0.0027(19)
O26 0.0304(15) 0.0202(13) 0.0264(14) -0.0032(11) -0.0016(12) -0.0072(12)
C31 0.0220(18) 0.0193(17) 0.0147(16) 0.0035(14) 0.0025(14) -0.0035(15)
C32 0.0167(17) 0.0208(17) 0.0155(16) 0.0013(14) 0.0040(14) 0.0016(14)
C33 0.027(2) 0.0236(18) 0.0194(17) -0.0019(15) 0.0001(16) 0.0058(16)
C34 0.031(2) 0.029(2) 0.0174(18) -0.0033(16) -0.0034(16) -0.0013(17)
C35 0.0226(19) 0.029(2) 0.0175(17) 0.0010(15) -0.0019(15) -0.0019(16)
O261 0.0220(13) 0.0265(13) 0.0173(12) 0.0012(11) -0.0024(11) 0.0046(11)

_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 S13 2.1951(9) 3 ?
Ni1 S13 2.1951(9) . ?
Ni1 S11 2.2016(9) 3 ?
Ni1 S11 2.2017(9) . ?
S11 C12 1.722(3) . ?
S13 C12 1.727(3) . ?
C12 N14 1.313(4) . ?
N14 C21 1.483(4) . ?
N14 C31 1.486(4) . ?
C21 C22 1.485(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.338(5) . ?
C22 O26 1.371(4) . ?
C23 C24 1.422(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.324(5) . ?
C24 H24 0.9300 . ?
C25 O26 1.368(4) . ?
C25 H25 0.9300 . ?
C31 C32 1.483(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.356(5) . ?
C32 O261 1.383(4) . ?
C33 C34 1.432(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.332(5) . ?
C34 H34 0.9300 . ?
C35 O261 1.368(4) . ?
C35 H35 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
S13 Ni1 S13 180 3 . ?
S13 Ni1 S11 79.51(3) 3 3 ?
S13 Ni1 S11 100.49(3) . 3 ?
S13 Ni1 S11 100.49(3) 3 . ?
S13 Ni1 S11 79.51(3) . . ?
S11 Ni1 S11 180 3 . ?
C12 S11 Ni1 85.57(12) . . ?
C12 S13 Ni1 85.66(12) . . ?
N14 C12 S11 125.3(3) . . ?
N14 C12 S13 125.5(3) . . ?
S11 C12 S13 109.25(19) . . ?
C12 N14 C21 119.9(3) . . ?
C12 N14 C31 121.1(3) . . ?
C21 N14 C31 118.3(3) . . ?
N14 C21 C22 114.5(3) . . ?
N14 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
N14 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C23 C22 O26 110.4(3) . . ?
C23 C22 C21 133.3(3) . . ?
O26 C22 C21 116.2(3) . . ?
C22 C23 C24 106.2(4) . . ?
C22 C23 H23 126.9 . . ?
C24 C23 H23 126.9 . . ?
C25 C24 C23 107.0(4) . . ?
C25 C24 H24 126.5 . . ?
C23 C24 H24 126.5 . . ?
C24 C25 O26 110.7(3) . . ?
C24 C25 H25 124.6 . . ?
O26 C25 H25 124.6 . . ?
C25 O26 C22 105.6(3) . . ?
C32 C31 N14 113.8(3) . . ?
C32 C31 H31A 108.8 . . ?
N14 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
N14 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C33 C32 O261 109.6(3) . . ?
C33 C32 C31 134.5(3) . . ?
O261 C32 C31 115.9(3) . . ?
C32 C33 C34 106.4(3) . . ?
C32 C33 H33 126.8 . . ?
C34 C33 H33 126.8 . . ?
C35 C34 C33 106.8(3) . . ?
C35 C34 H34 126.6 . . ?
C33 C34 H34 126.6 . . ?
C34 C35 O261 111.0(3) . . ?
C34 C35 H35 124.5 . . ?
O261 C35 H35 124.5 . . ?
C35 O261 C32 106.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.116
_database_code_depnum_ccdc_archive 'CCDC 997875'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H26 N4 Pd S4'
_chemical_formula_weight         653.17

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'
Pd Pd -0.9988 1.0072 '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                   6.503(6)
_cell_length_b                   10.171(9)
_cell_length_c                   11.709(10)
_cell_angle_alpha                75.41(8)
_cell_angle_beta                 80.37(8)
_cell_angle_gamma                72.19(8)
_cell_volume                     710.2(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5245
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             332
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.924
_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_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            5245
_diffrn_reflns_av_R_equivalents  0.1473
_diffrn_reflns_av_sigmaI/netI    0.1823
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3100
_reflns_number_gt                1479
_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)+(0.0686P)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         3100
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2144
_refine_ls_wR_factor_gt          0.1631
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      0.930
_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
S11 S -0.1576(3) 0.0289(2) -0.17339(18) 0.0561(6) Uani 1 1 d . . .
S13 S -0.1844(3) -0.1735(2) 0.04480(17) 0.0553(6) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.0000 0.0000 0.0510(3) Uani 1 2 d S . .
C12 C -0.2685(11) -0.1054(8) -0.0978(6) 0.0463(17) Uani 1 1 d . . .
N14 N -0.3997(10) -0.1533(7) -0.1401(5) 0.0508(15) Uani 1 1 d . . .
C21 C -0.4881(13) -0.0753(9) -0.2567(7) 0.059(2) Uani 1 1 d . . .
H21A H -0.4674 0.0186 -0.2762 0.071 Uiso 1 1 calc R . .
H21B H -0.6429 -0.0648 -0.2485 0.071 Uiso 1 1 calc R . .
C22 C -0.3799(12) -0.1503(9) -0.3590(6) 0.0533(19) Uani 1 1 d . B .
C23 C -0.5033(15) -0.1752(11) -0.4305(7) 0.074(3) Uani 1 1 d . . .
H23 H -0.6533 -0.1490 -0.4132 0.088 Uiso 1 1 calc R A 1
C24 C -0.4206(18) -0.2362(12) -0.5258(8) 0.099(4) Uani 0.28(7) 1 d P B 1
H24 H -0.5112 -0.2544 -0.5699 0.119 Uiso 0.28(7) 1 calc PR B 1
N24 N -0.4206(18) -0.2362(12) -0.5258(8) 0.099(4) Uani 0.72(7) 1 d P B 2
C25 C -0.206(2) -0.2689(16) -0.5539(10) 0.120(5) Uani 1 1 d . . .
H25 H -0.1463 -0.3106 -0.6185 0.145 Uiso 1 1 calc R B 1
C26 C -0.0715(18) -0.2412(16) -0.4871(10) 0.115(5) Uani 1 1 d . B .
H26 H 0.0777 -0.2635 -0.5078 0.138 Uiso 1 1 calc R . .
C27 C -0.1581(16) -0.1817(13) -0.3921(8) 0.089(3) Uani 1 1 d . . .
H27 H -0.0680 -0.1618 -0.3488 0.107 Uiso 1 1 calc R B .
C31 C -0.4947(13) -0.2670(9) -0.0683(7) 0.058(2) Uani 1 1 d . . .
H31B H -0.6439 -0.2254 -0.0403 0.069 Uiso 1 1 calc R . .
H31A H -0.4150 -0.3141 0.0006 0.069 Uiso 1 1 calc R . .
C32 C -0.4889(12) -0.3739(8) -0.1371(6) 0.0490(18) Uani 1 1 d . B .
C37 C -0.2946(14) -0.4746(9) -0.1637(8) 0.070(2) Uani 1 1 d . . .
H37 H -0.1670 -0.4755 -0.1372 0.084 Uiso 1 1 calc R . .
C36 C -0.2898(18) -0.5696(11) -0.2268(9) 0.086(3) Uani 1 1 d . B .
H36 H -0.1576 -0.6328 -0.2444 0.103 Uiso 1 1 calc R . .
C35 C -0.471(2) -0.5766(12) -0.2655(9) 0.093(3) Uani 1 1 d . . .
H35 H -0.4636 -0.6419 -0.3102 0.112 Uiso 1 1 calc R B 1
C34 C -0.6688(16) -0.4826(11) -0.2362(8) 0.083(3) Uani 0.72(7) 1 d P B 1
H34 H -0.7962 -0.4851 -0.2607 0.100 Uiso 0.72(7) 1 calc PR B 1
N34 N -0.6688(16) -0.4826(11) -0.2362(8) 0.083(3) Uani 0.28(7) 1 d P B 2
C33 C -0.6743(13) -0.3863(9) -0.1707(7) 0.064(2) Uani 1 1 d . . .
H33 H -0.8078 -0.3275 -0.1483 0.076 Uiso 1 1 calc R B 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S11 0.0681(14) 0.0515(13) 0.0582(12) -0.0091(10) -0.0184(10) -0.0259(11)
S13 0.0666(13) 0.0539(13) 0.0539(11) -0.0094(10) -0.0182(9) -0.0242(11)
Pd1 0.0527(6) 0.0523(6) 0.0560(6) -0.0166(4) -0.0121(4) -0.0184(4)
C12 0.051(5) 0.041(4) 0.050(4) -0.023(3) -0.007(3) -0.004(3)
N14 0.062(4) 0.043(4) 0.051(4) -0.016(3) -0.014(3) -0.010(3)
C21 0.069(5) 0.055(5) 0.066(5) -0.017(4) -0.021(4) -0.024(4)
C22 0.057(5) 0.055(5) 0.050(4) -0.004(4) -0.016(3) -0.018(4)
C23 0.079(6) 0.104(8) 0.057(5) -0.020(5) -0.009(4) -0.049(6)
C24 0.127(9) 0.118(9) 0.077(6) -0.034(6) -0.016(5) -0.054(7)
N24 0.127(9) 0.118(9) 0.077(6) -0.034(6) -0.016(5) -0.054(7)
C25 0.138(11) 0.179(16) 0.073(7) -0.065(8) 0.008(7) -0.064(11)
C26 0.081(8) 0.189(16) 0.089(8) -0.059(9) 0.010(6) -0.042(9)
C27 0.078(7) 0.141(11) 0.067(6) -0.045(7) -0.010(5) -0.038(7)
C31 0.065(5) 0.060(6) 0.060(5) -0.022(4) 0.001(4) -0.030(4)
C32 0.059(5) 0.042(4) 0.053(4) -0.002(3) -0.013(3) -0.027(4)
C37 0.063(6) 0.048(5) 0.095(7) -0.010(5) -0.027(5) -0.003(5)
C36 0.093(8) 0.062(7) 0.093(8) -0.029(6) 0.010(6) -0.006(6)
C35 0.132(10) 0.063(7) 0.097(8) -0.023(6) -0.012(7) -0.041(7)
C34 0.087(8) 0.072(7) 0.110(8) -0.022(6) -0.030(6) -0.038(6)
N34 0.087(8) 0.072(7) 0.110(8) -0.022(6) -0.030(6) -0.038(6)
C33 0.065(6) 0.055(5) 0.076(6) -0.015(4) -0.014(4) -0.021(4)

_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
S11 C12 1.717(8) . ?
S11 Pd1 2.339(3) . ?
S13 C12 1.749(7) . ?
S13 Pd1 2.333(3) . ?
Pd1 S13 2.333(3) 2 ?
Pd1 S11 2.339(3) 2 ?
C12 N14 1.315(8) . ?
N14 C31 1.483(9) . ?
N14 C21 1.504(9) . ?
C21 C22 1.537(11) . ?
C22 C23 1.367(10) . ?
C22 C27 1.388(11) . ?
C23 C24 1.364(12) . ?
C24 C25 1.334(14) . ?
C25 C26 1.398(14) . ?
C26 C27 1.357(13) . ?
C31 C32 1.496(10) . ?
C32 C33 1.379(9) . ?
C32 C37 1.407(11) . ?
C37 C36 1.347(12) . ?
C36 C35 1.358(13) . ?
C35 C34 1.397(14) . ?
C34 C33 1.377(11) . ?

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
C12 S11 Pd1 86.6(2) . . ?
C12 S13 Pd1 86.1(3) . . ?
S13 Pd1 S13 180 . 2 ?
S13 Pd1 S11 75.69(10) . . ?
S13 Pd1 S11 104.31(10) 2 . ?
S13 Pd1 S11 104.31(10) . 2 ?
S13 Pd1 S11 75.69(10) 2 2 ?
S11 Pd1 S11 180 . 2 ?
N14 C12 S11 125.3(6) . . ?
N14 C12 S13 123.2(6) . . ?
S11 C12 S13 111.6(4) . . ?
C12 N14 C31 122.3(6) . . ?
C12 N14 C21 119.4(7) . . ?
C31 N14 C21 117.5(6) . . ?
N14 C21 C22 113.1(6) . . ?
C23 C22 C27 116.4(8) . . ?
C23 C22 C21 120.4(7) . . ?
C27 C22 C21 122.8(7) . . ?
C24 C23 C22 124.2(9) . . ?
C25 C24 C23 118.2(9) . . ?
C24 C25 C26 120.5(11) . . ?
C27 C26 C25 120.0(10) . . ?
C26 C27 C22 120.6(9) . . ?
N14 C31 C32 112.3(6) . . ?
C33 C32 C37 116.1(8) . . ?
C33 C32 C31 122.3(8) . . ?
C37 C32 C31 121.5(7) . . ?
C36 C37 C32 121.3(8) . . ?
C37 C36 C35 122.4(10) . . ?
C36 C35 C34 118.0(10) . . ?
C33 C34 C35 119.7(8) . . ?
C34 C33 C32 122.3(9) . . ?

_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.949
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.159
_database_code_depnum_ccdc_archive 'CCDC 997876'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H20 N2 O4 Pt S4'
_chemical_formula_weight         699.73

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                   5.7453(3)
_cell_length_b                   19.0518(10)
_cell_length_c                   11.0760(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.441(4)
_cell_angle_gamma                90.00
_cell_volume                     1211.98(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4254
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    6.166
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.812
_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_device_type  'CCD diffractometer'
_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            4254
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2128
_reflns_number_gt                1440
_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)
_computing_publication_material  'SHELXL-97, PLATON'



_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)+(0.0175P)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         2128
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0590
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_restrained_S_all      0.927
_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 0.0000 0.0000 0.0000 0.03640(14) Uani 1 2 d S . .
S11 S 0.1660(3) 0.00773(9) -0.18821(15) 0.0415(4) Uani 1 1 d . . .
S13 S 0.2897(3) -0.08482(10) 0.00093(16) 0.0440(5) Uani 1 1 d . . .
C12 C 0.3529(10) -0.0591(3) -0.1420(6) 0.0374(17) Uani 1 1 d . . .
C21 C 0.6789(11) -0.1396(4) -0.1582(6) 0.051(2) Uani 1 1 d . . .
H21A H 0.8163 -0.1157 -0.1264 0.061 Uiso 1 1 calc R . .
H21B H 0.6040 -0.1619 -0.0906 0.061 Uiso 1 1 calc R . .
C22 C 0.7531(11) -0.1938(4) -0.2395(6) 0.0385(17) Uani 1 1 d . . .
C23 C 0.9517(11) -0.2050(4) -0.2969(7) 0.057(2) Uani 1 1 d . . .
H23 H 1.0818 -0.1759 -0.2955 0.069 Uiso 1 1 calc R . .
C24 C 0.9277(16) -0.2685(5) -0.3593(8) 0.081(3) Uani 1 1 d . . .
H24 H 1.0354 -0.2890 -0.4097 0.097 Uiso 1 1 calc R . .
C25 C 0.7208(18) -0.2935(4) -0.3321(9) 0.083(3) Uani 1 1 d . . .
H25 H 0.6622 -0.3364 -0.3589 0.099 Uiso 1 1 calc R . .
C31 C 0.5683(10) -0.0566(4) -0.3290(6) 0.0430(18) Uani 1 1 d . . .
H31A H 0.7335 -0.0618 -0.3427 0.052 Uiso 1 1 calc R . .
H31B H 0.5344 -0.0067 -0.3278 0.052 Uiso 1 1 calc R . .
C32 C 0.4374(11) -0.0887(4) -0.4318(6) 0.0425(18) Uani 1 1 d . . .
C33 C 0.4733(12) -0.1423(4) -0.5062(7) 0.059(2) Uani 1 1 d . . .
H33 H 0.6039 -0.1711 -0.5058 0.071 Uiso 1 1 calc R . .
C34 C 0.2767(14) -0.1475(4) -0.5863(7) 0.068(2) Uani 1 1 d . . .
H34 H 0.2541 -0.1800 -0.6481 0.081 Uiso 1 1 calc R . .
C35 C 0.1331(13) -0.0972(5) -0.5552(7) 0.060(2) Uani 1 1 d . . .
H35 H -0.0106 -0.0886 -0.5930 0.073 Uiso 1 1 calc R . .
N14 N 0.5174(8) -0.0861(3) -0.2097(5) 0.0366(13) Uani 1 1 d . . .
O26 O 0.6052(9) -0.2487(3) -0.2603(5) 0.0658(16) Uani 1 1 d . . .
O36 O 0.2234(8) -0.0591(3) -0.4599(4) 0.0569(14) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0408(2) 0.0372(2) 0.0311(2) -0.0015(2) -0.00165(16) 0.00021(19)
S11 0.0483(10) 0.0424(12) 0.0339(10) 0.0036(11) 0.0007(8) 0.0083(9)
S13 0.0503(10) 0.0473(12) 0.0345(10) 0.0057(11) 0.0030(8) 0.0084(9)
C12 0.044(4) 0.032(4) 0.035(4) -0.006(4) -0.012(3) -0.005(3)
C21 0.059(5) 0.047(5) 0.047(5) -0.003(5) -0.013(4) 0.011(4)
C22 0.039(4) 0.035(4) 0.041(5) -0.002(4) -0.009(3) 0.003(3)
C23 0.043(4) 0.060(6) 0.069(6) 0.001(5) 0.002(4) 0.011(4)
C24 0.101(7) 0.082(8) 0.061(7) -0.005(7) 0.011(6) 0.045(6)
C25 0.143(9) 0.037(5) 0.068(7) -0.024(6) -0.012(7) 0.001(6)
C31 0.049(4) 0.033(4) 0.048(5) 0.002(4) 0.008(4) -0.001(3)
C32 0.045(4) 0.048(5) 0.035(4) 0.002(4) 0.005(3) 0.001(4)
C33 0.060(5) 0.071(6) 0.046(5) -0.023(5) -0.005(4) 0.021(4)
C34 0.090(6) 0.067(7) 0.045(5) -0.014(5) -0.005(5) 0.005(5)
C35 0.063(5) 0.090(7) 0.028(4) 0.006(5) -0.003(4) 0.000(5)
N14 0.045(3) 0.032(3) 0.033(3) 0.002(3) 0.004(3) 0.006(3)
O26 0.075(3) 0.057(4) 0.065(4) -0.012(4) 0.000(3) -0.022(3)
O36 0.058(3) 0.062(4) 0.051(3) 0.002(3) -0.002(3) 0.015(3)

_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 S11 2.3188(17) . ?
Pt1 S11 2.3188(17) 3 ?
Pt1 S13 2.3195(17) . ?
Pt1 S13 2.3195(17) 3 ?
S11 C12 1.734(6) . ?
S13 C12 1.706(7) . ?
C12 N14 1.326(7) . ?
C21 C22 1.441(8) . ?
C21 N14 1.483(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.337(8) . ?
C22 O26 1.364(7) . ?
C23 C24 1.400(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.323(10) . ?
C24 H24 0.9300 . ?
C25 O26 1.353(9) . ?
C25 H25 0.9300 . ?
C31 N14 1.472(8) . ?
C31 C32 1.480(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.332(9) . ?
C32 O36 1.381(7) . ?
C33 C34 1.422(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.316(9) . ?
C34 H34 0.9300 . ?
C35 O36 1.373(8) . ?
C35 H35 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
S11 Pt1 S11 180 . 3 ?
S11 Pt1 S13 74.75(6) . . ?
S11 Pt1 S13 105.25(6) 3 . ?
S11 Pt1 S13 105.25(6) . 3 ?
S11 Pt1 S13 74.75(6) 3 3 ?
S13 Pt1 S13 180 . 3 ?
C12 S11 Pt1 87.4(2) . . ?
C12 S13 Pt1 88.0(2) . . ?
N14 C12 S13 125.8(5) . . ?
N14 C12 S11 124.3(5) . . ?
S13 C12 S11 109.9(4) . . ?
C22 C21 N14 116.3(6) . . ?
C22 C21 H21A 108.2 . . ?
N14 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
N14 C21 H21B 108.2 . . ?
H21A C21 H21B 107.4 . . ?
C23 C22 O26 109.5(7) . . ?
C23 C22 C21 132.9(7) . . ?
O26 C22 C21 117.5(6) . . ?
C22 C23 C24 107.3(7) . . ?
C22 C23 H23 126.3 . . ?
C24 C23 H23 126.3 . . ?
C25 C24 C23 106.1(8) . . ?
C25 C24 H24 127.0 . . ?
C23 C24 H24 127.0 . . ?
C24 C25 O26 111.4(8) . . ?
C24 C25 H25 124.3 . . ?
O26 C25 H25 124.3 . . ?
N14 C31 C32 115.0(5) . . ?
N14 C31 H31A 108.5 . . ?
C32 C31 H31A 108.5 . . ?
N14 C31 H31B 108.5 . . ?
C32 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C33 C32 O36 108.9(6) . . ?
C33 C32 C31 135.1(7) . . ?
O36 C32 C31 115.9(7) . . ?
C32 C33 C34 107.9(7) . . ?
C32 C33 H33 126.1 . . ?
C34 C33 H33 126.1 . . ?
C35 C34 C33 106.2(8) . . ?
C35 C34 H34 126.9 . . ?
C33 C34 H34 126.9 . . ?
C34 C35 O36 111.0(7) . . ?
C34 C35 H35 124.5 . . ?
O36 C35 H35 124.5 . . ?
C12 N14 C31 121.3(5) . . ?
C12 N14 C21 119.8(5) . . ?
C31 N14 C21 118.2(5) . . ?
C25 O26 C22 105.7(6) . . ?
C35 O36 C32 106.0(6) . . ?


_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.134
_database_code_depnum_ccdc_archive 'CCDC 997877'
