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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1450245'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;

_audit_creation_date             2015-01-28T11:51:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C24 H32 Cl4 K2 Ni1 O5 S4'
_chemical_formula_sum            'C24 H32 Cl4 K2 Ni1 O5 S4'
_chemical_formula_weight         807.44
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.064(3)
_cell_length_b                   14.446(5)
_cell_length_c                   26.473(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.273(14)
_cell_angle_gamma                90
_cell_volume                     3438.5(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    152
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            reddish
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 3 -7 0.203
-7 6 -6 0.187
5 -2 1 0.15
1 -6 10 0.127
0 0 -1 0.12
0 0 1 0.044


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_T_max  0.819


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_number            26810
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.103
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_Friedel_coverage         0
_reflns_number_total             3952
_reflns_number_gt                2567
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond (Branderburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0865P)²+32.0534P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3952
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.124
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2278
_refine_ls_wR_factor_gt          0.2123
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.331
_refine_diff_density_min         -1
_refine_diff_density_rms         0.124

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5593(7) 0.9372(5) 0.3661(2) 0.0383(15) Uani 1 1 d . . . . .
C2 C 0.5840(9) 0.9827(6) 0.4122(3) 0.0483(18) Uani 1 1 d . . . . .
C3 C 0.6120(9) 0.9372(6) 0.4586(3) 0.055(2) Uani 1 1 d . . . . .
H3 H 0.6278 0.971 0.4896 0.066 Uiso 1 1 calc R U . . .
C4 C 0.6164(10) 0.8420(7) 0.4587(3) 0.058(2) Uani 1 1 d . . . . .
H4 H 0.6339 0.8093 0.49 0.069 Uiso 1 1 calc R U . . .
C5 C 0.5955(8) 0.7938(5) 0.4132(3) 0.0441(17) Uani 1 1 d . . . . .
C6 C 0.5635(7) 0.8410(5) 0.3658(2) 0.0358(15) Uani 1 1 d . . . . .
C51 C -0.0258(16) 0.9394(11) 0.4134(6) 0.124(3) Uani 1 1 d . . . . .
H51A H -0.1155 0.9276 0.3888 0.148 Uiso 1 1 calc R U . . .
H51B H -0.0416 0.9962 0.4329 0.148 Uiso 1 1 calc R U . . .
C52 C 0.0066(16) 0.8623(11) 0.4465(6) 0.124(3) Uani 1 1 d . . . . .
H52A H -0.0325 0.8745 0.4791 0.148 Uiso 1 1 calc R U . . .
H52B H -0.0443 0.8067 0.4309 0.148 Uiso 1 1 calc R U . . .
C53 C 0.1515(16) 0.8460(11) 0.4555(6) 0.124(3) Uani 1 1 d . . . . .
H53A H 0.1714 0.7789 0.4601 0.148 Uiso 1 1 calc R U . . .
H53B H 0.1965 0.8793 0.4864 0.148 Uiso 1 1 calc R U . . .
C54 C 0.2094(17) 0.8805(11) 0.4104(6) 0.124(3) Uani 1 1 d . . . . .
H54A H 0.3077 0.9099 0.4197 0.148 Uiso 1 1 calc R U . . .
H54B H 0.22 0.8295 0.3862 0.148 Uiso 1 1 calc R U . . .
C61 C 0.0965(12) 0.8522(8) 0.2249(5) 0.094(4) Uani 1 1 d . . . . .
H61A H 0.082 0.8642 0.1877 0.113 Uiso 1 1 calc R U . . .
H61B H 0.2017 0.8649 0.238 0.113 Uiso 1 1 calc R U . . .
C62 C 0.0611(17) 0.7598(8) 0.2346(8) 0.151(8) Uani 1 1 d . . . . .
H62A H 0.1487 0.728 0.2529 0.181 Uiso 1 1 calc R U . . .
H62B H 0.0313 0.7267 0.2021 0.181 Uiso 1 1 calc R U . . .
O1 O -0.1510(6) 1.0875(4) 0.2948(2) 0.0601(16) Uani 1 1 d . . . . .
H1A H -0.2101 1.043 0.3124 0.072 Uiso 1 1 calc R U . . .
H1B H -0.1767 1.1521 0.3025 0.072 Uiso 1 1 calc R U . . .
O5 O 0.1021(8) 0.9474(5) 0.3883(3) 0.087(2) Uani 1 1 d . . . . .
O6 O 0 0.9113(6) 0.25 0.068(3) Uani 1 2 d S T P . .
S1 S 0.51873(18) 0.99596(12) 0.30775(6) 0.0345(4) Uani 1 1 d . . . . .
S2 S 0.53309(19) 0.78063(12) 0.30788(6) 0.0369(4) Uani 1 1 d . . . . .
Cl1 Cl 0.5759(4) 1.10337(16) 0.41364(9) 0.0785(8) Uani 1 1 d . . . . .
Cl2 Cl 0.6027(3) 0.67318(15) 0.41423(8) 0.0697(7) Uani 1 1 d . . . . .
K1 K 0.15292(19) 1.05159(13) 0.30830(7) 0.0546(5) Uani 1 1 d . . . . .
Ni1 Ni 0.5 0.88815(8) 0.25 0.0294(3) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.382(10) . ?
C1 C6 1.390(10) . ?
C1 S1 1.759(7) . ?
C2 C3 1.387(11) . ?
C2 Cl1 1.745(8) . ?
C3 C4 1.376(12) . ?
C3 H3 0.95 . ?
C4 C5 1.384(11) . ?
C4 H4 0.95 . ?
C5 C6 1.424(9) . ?
C5 Cl2 1.744(8) . ?
C6 S2 1.756(7) . ?
C51 O5 1.413(15) . ?
C51 C52 1.424(19) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
C52 C53 1.326(18) . ?
C52 H52A 0.99 . ?
C52 H52B 0.99 . ?
C53 C54 1.452(18) . ?
C53 H53A 0.99 . ?
C53 H53B 0.99 . ?
C54 O5 1.442(15) . ?
C54 H54A 0.99 . ?
C54 H54B 0.99 . ?
C61 C62 1.404(15) . ?
C61 O6 1.443(11) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C62 C62 1.46(3) 2 ?
C62 H62A 0.99 . ?
C62 H62B 0.99 . ?
O1 K1 2.776(6) 2 ?
O1 K1 2.781(6) . ?
O1 H1A 0.99 . ?
O1 H1B 0.99 . ?
O5 K1 2.684(6) . ?
O6 C61 1.443(11) 2 ?
O6 K1 2.805(6) . ?
O6 K1 2.805(6) 2 ?
S1 Ni1 2.1739(19) . ?
S1 K1 3.414(3) . ?
S2 Ni1 2.1758(19) . ?
S2 K1 3.482(3) 3_545 ?
Cl2 K1 3.388(3) 3_545 ?
K1 O1 2.776(6) 2 ?
K1 Cl2 3.388(3) 3_455 ?
K1 S2 3.482(3) 3_455 ?
K1 K1 3.879(4) 2 ?
Ni1 S1 2.1738(19) 2_655 ?
Ni1 S2 2.1758(19) 2_655 ?

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
C2 C1 C6 118.6(7) . . ?
C2 C1 S1 122.6(6) . . ?
C6 C1 S1 118.8(5) . . ?
C1 C2 C3 123.2(8) . . ?
C1 C2 Cl1 119.5(6) . . ?
C3 C2 Cl1 117.3(6) . . ?
C4 C3 C2 118.5(7) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 120.1(7) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C4 C5 C6 121.1(7) . . ?
C4 C5 Cl2 119.2(6) . . ?
C6 C5 Cl2 119.7(5) . . ?
C1 C6 C5 118.5(6) . . ?
C1 C6 S2 120.0(5) . . ?
C5 C6 S2 121.5(6) . . ?
O5 C51 C52 103.7(11) . . ?
O5 C51 H51A 111 . . ?
C52 C51 H51A 111 . . ?
O5 C51 H51B 111 . . ?
C52 C51 H51B 111 . . ?
H51A C51 H51B 109 . . ?
C53 C52 C51 111.9(14) . . ?
C53 C52 H52A 109.2 . . ?
C51 C52 H52A 109.2 . . ?
C53 C52 H52B 109.2 . . ?
C51 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
C52 C53 C54 104.0(14) . . ?
C52 C53 H53A 110.9 . . ?
C54 C53 H53A 110.9 . . ?
C52 C53 H53B 110.9 . . ?
C54 C53 H53B 110.9 . . ?
H53A C53 H53B 109 . . ?
O5 C54 C53 105.7(11) . . ?
O5 C54 H54A 110.6 . . ?
C53 C54 H54A 110.6 . . ?
O5 C54 H54B 110.6 . . ?
C53 C54 H54B 110.6 . . ?
H54A C54 H54B 108.7 . . ?
C62 C61 O6 108.2(10) . . ?
C62 C61 H61A 110.1 . . ?
O6 C61 H61A 110.1 . . ?
C62 C61 H61B 110.1 . . ?
O6 C61 H61B 110.1 . . ?
H61A C61 H61B 108.4 . . ?
C61 C62 C62 108.1(7) . 2 ?
C61 C62 H62A 110.1 . . ?
C62 C62 H62A 110.1 2 . ?
C61 C62 H62B 110.1 . . ?
C62 C62 H62B 110.1 2 . ?
H62A C62 H62B 108.4 . . ?
K1 O1 K1 88.54(16) 2 . ?
K1 O1 H1A 113.9 2 . ?
K1 O1 H1A 113.9 . . ?
K1 O1 H1B 113.9 2 . ?
K1 O1 H1B 113.9 . . ?
H1A O1 H1B 111.1 . . ?
C51 O5 C54 107.7(9) . . ?
C51 O5 K1 130.6(7) . . ?
C54 O5 K1 121.5(7) . . ?
C61 O6 C61 107.5(11) 2 . ?
C61 O6 K1 117.3(6) 2 . ?
C61 O6 K1 113.3(5) . . ?
C61 O6 K1 113.3(5) 2 2 ?
C61 O6 K1 117.3(6) . 2 ?
K1 O6 K1 87.5(2) . 2 ?
C1 S1 Ni1 105.1(2) . . ?
C1 S1 K1 101.8(2) . . ?
Ni1 S1 K1 100.50(6) . . ?
C6 S2 Ni1 104.7(2) . . ?
C6 S2 K1 117.1(2) . 3_545 ?
Ni1 S2 K1 134.09(7) . 3_545 ?
C5 Cl2 K1 120.9(2) . 3_545 ?
O5 K1 O1 154.1(2) . 2 ?
O5 K1 O1 86.5(2) . . ?
O1 K1 O1 87.48(17) 2 . ?
O5 K1 O6 84.7(2) . . ?
O1 K1 O6 69.68(16) 2 . ?
O1 K1 O6 69.61(14) . . ?
O5 K1 Cl2 65.37(19) . 3_455 ?
O1 K1 Cl2 137.08(14) 2 3_455 ?
O1 K1 Cl2 77.00(13) . 3_455 ?
O6 K1 Cl2 136.15(8) . 3_455 ?
O5 K1 S1 97.76(16) . . ?
O1 K1 S1 85.70(12) 2 . ?
O1 K1 S1 171.94(14) . . ?
O6 K1 S1 103.90(10) . . ?
Cl2 K1 S1 110.97(8) 3_455 . ?
O5 K1 S2 116.78(18) . 3_455 ?
O1 K1 S2 81.74(12) 2 3_455 ?
O1 K1 S2 61.26(12) . 3_455 ?
O6 K1 S2 123.55(13) . 3_455 ?
Cl2 K1 S2 55.63(5) 3_455 3_455 ?
S1 K1 S2 121.77(7) . 3_455 ?
O5 K1 K1 116.81(19) . 2 ?
O1 K1 K1 45.78(13) 2 2 ?
O1 K1 K1 45.68(12) . 2 ?
O6 K1 K1 46.26(12) . 2 ?
Cl2 K1 K1 120.09(8) 3_455 2 ?
S1 K1 K1 126.40(8) . 2 ?
S2 K1 K1 78.83(4) 3_455 2 ?
S1 Ni1 S1 88.48(10) 2_655 . ?
S1 Ni1 S2 91.42(6) 2_655 2_655 ?
S1 Ni1 S2 176.58(6) . 2_655 ?
S1 Ni1 S2 176.58(6) 2_655 . ?
S1 Ni1 S2 91.41(6) . . ?
S2 Ni1 S2 88.89(10) 2_655 . ?

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
C6 C1 C2 C3 -0.4(11) . . . . ?
S1 C1 C2 C3 178.2(6) . . . . ?
C6 C1 C2 Cl1 -178.8(5) . . . . ?
S1 C1 C2 Cl1 -0.3(9) . . . . ?
C1 C2 C3 C4 0.4(13) . . . . ?
Cl1 C2 C3 C4 178.9(7) . . . . ?
C2 C3 C4 C5 1.0(13) . . . . ?
C3 C4 C5 C6 -2.4(13) . . . . ?
C3 C4 C5 Cl2 179.6(7) . . . . ?
C2 C1 C6 C5 -1.0(10) . . . . ?
S1 C1 C6 C5 -179.6(5) . . . . ?
C2 C1 C6 S2 -179.9(5) . . . . ?
S1 C1 C6 S2 1.5(8) . . . . ?
C4 C5 C6 C1 2.4(11) . . . . ?
Cl2 C5 C6 C1 -179.6(5) . . . . ?
C4 C5 C6 S2 -178.7(6) . . . . ?
Cl2 C5 C6 S2 -0.8(9) . . . . ?
O5 C51 C52 C53 21(2) . . . . ?
C51 C52 C53 C54 -28(2) . . . . ?
C52 C53 C54 O5 23.0(19) . . . . ?
O6 C61 C62 C62 1(3) . . . 2 ?
C52 C51 O5 C54 -4.8(17) . . . . ?
C52 C51 O5 K1 170.1(10) . . . . ?
C53 C54 O5 C51 -10.8(18) . . . . ?
C53 C54 O5 K1 173.8(10) . . . . ?
C62 C61 O6 C61 -0.4(10) . . . 2 ?
C62 C61 O6 K1 130.9(12) . . . . ?
C62 C61 O6 K1 -129.4(12) . . . 2 ?
C2 C1 S1 Ni1 178.0(5) . . . . ?
C6 C1 S1 Ni1 -3.4(6) . . . . ?
C2 C1 S1 K1 -77.5(6) . . . . ?
C6 C1 S1 K1 101.0(5) . . . . ?
C1 C6 S2 Ni1 1.2(6) . . . . ?
C5 C6 S2 Ni1 -177.6(5) . . . . ?
C1 C6 S2 K1 161.4(5) . . . 3_545 ?
C5 C6 S2 K1 -17.4(6) . . . 3_545 ?
C4 C5 Cl2 K1 -162.2(5) . . . 3_545 ?
C6 C5 Cl2 K1 19.8(7) . . . 3_545 ?



# END of CIF
####################################################################### 
# 
# 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_DH72_3_KPd
_database_code_depnum_ccdc_archive 'CCDC 1450246'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;

_audit_creation_date             2014-07-10T12:31:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H32 Cl4 K2 O5 Pd S4'
_chemical_formula_sum            'C24 H32 Cl4 K2 O5 Pd S4'
_chemical_formula_weight         855.13

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.064(3)
_cell_length_b                   14.446(5)
_cell_length_c                   26.473(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.273(14)
_cell_angle_gamma                90
_cell_volume                     3438.5(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    1356
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  1.186

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_number            35756
_diffrn_reflns_av_unetI/netI     0.1408
_diffrn_reflns_av_R_equivalents  0.1442
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.103
_diffrn_reflns_theta_max         27.744
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_reflns_number_total             3939
_reflns_number_gt                2121
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1149P)²+30.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3939
_refine_ls_number_parameters     178
_refine_ls_number_restraints     40
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1728
_refine_ls_R_factor_gt           0.0952
_refine_ls_wR_factor_ref         0.2691
_refine_ls_wR_factor_gt          0.2412
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.173

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5603(10) 0.9367(8) 0.3686(4) 0.039(2) Uani 1 d . .
C2 C 0.5875(13) 0.9819(8) 0.4146(4) 0.052(3) Uani 1 d . .
C3 C 0.6126(14) 0.9355(9) 0.4603(4) 0.060(3) Uani 1 d . .
H3 H 0.6252 0.9681 0.4917 0.072 Uiso 1 calc . .
C4 C 0.6190(13) 0.8396(9) 0.4590(4) 0.056(3) Uani 1 d . .
H4 H 0.6425 0.806 0.4899 0.067 Uiso 1 calc . .
C5 C 0.5921(12) 0.7935(8) 0.4145(4) 0.046(3) Uani 1 d . .
C6 C 0.5640(11) 0.8382(8) 0.3672(4) 0.045(3) Uani 1 d . .
C51 C -0.0271(19) 0.9400(14) 0.4121(7) 0.115(6) Uani 1 d . .
H51A H -0.1156 0.9236 0.388 0.138 Uiso 1 calc . .
H51B H -0.0467 0.9985 0.4297 0.138 Uiso 1 calc . .
C52 C 0.013(3) 0.8657(18) 0.4485(9) 0.167(8) Uani 1 d . .
H52A H -0.0145 0.884 0.4822 0.201 Uiso 1 calc . .
H52B H -0.0451 0.8096 0.4373 0.201 Uiso 1 calc . .
C53 C 0.160(3) 0.8452(15) 0.4533(8) 0.127(6) Uani 1 d . .
H53A H 0.1759 0.7774 0.4538 0.152 Uiso 1 calc . .
H53B H 0.2124 0.872 0.4851 0.152 Uiso 1 calc . .
C54 C 0.2134(19) 0.8860(15) 0.4094(8) 0.117(6) Uani 1 d . .
H54A H 0.307 0.9203 0.4195 0.141 Uiso 1 calc . .
H54B H 0.2325 0.8374 0.3846 0.141 Uiso 1 calc . .
O1 O -0.1467(10) 1.0847(6) 0.2954(3) 0.074(3) Uani 1 d . .
H1A H -0.2048 1.0404 0.3136 0.088 Uiso 1 calc . .
H1B H -0.1717 1.1494 0.3032 0.088 Uiso 1 calc . .
O5 O 0.0997(12) 0.9473(7) 0.3874(4) 0.090(3) Uani 1 d . .
S1 S 0.5232(3) 1.00063(17) 0.31196(9) 0.0349(6) Uani 1 d . .
S2 S 0.5333(3) 0.77770(18) 0.31123(9) 0.0398(6) Uani 1 d . .
Cl1 Cl 0.5809(5) 1.1035(2) 0.41637(12) 0.0769(11) Uani 1 d . .
Cl2 Cl 0.6017(5) 0.6723(2) 0.41518(12) 0.0742(11) Uani 1 d . .
K1 K 0.1556(3) 1.0485(2) 0.30722(11) 0.0621(8) Uani 1 d . .
Pd1 Pd 0.5 0.88933(8) 0.25 0.0328(4) Uani 1 d . .
O6 O 0 0.9057(8) 0.25 0.063(3) Uani 1 d . .
C61 C 0.089(2) 0.8465(13) 0.2262(8) 0.111(6) Uiso 1 d . .
H61A H 0.076 0.8594 0.1892 0.134 Uiso 1 calc . .
H61B H 0.1948 0.8584 0.2394 0.134 Uiso 1 calc . .
C62 C 0.058(3) 0.7562(12) 0.2339(14) 0.204(15) Uani 1 d . .
H62A H 0.1468 0.7234 0.2505 0.245 Uiso 1 calc . .
H62B H 0.0235 0.7254 0.2011 0.245 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.377(14) . ?
C1 C6 1.424(15) . ?
C1 S1 1.757(10) . ?
C2 C3 1.375(16) . ?
C2 Cl1 1.759(12) . ?
C3 C4 1.387(17) . ?
C3 H3 0.95 . ?
C4 C5 1.348(15) . ?
C4 H4 0.95 . ?
C5 C6 1.404(14) . ?
C5 Cl2 1.754(12) . ?
C6 S2 1.712(11) . ?
C51 O5 1.397(17) . ?
C51 C52 1.46(3) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
C52 C53 1.36(3) . ?
C52 H52A 0.99 . ?
C52 H52B 0.99 . ?
C53 C54 1.44(3) . ?
C53 H53A 0.99 . ?
C53 H53B 0.99 . ?
C54 O5 1.426(19) . ?
C54 H54A 0.99 . ?
C54 H54B 0.99 . ?
O1 K1 2.759(8) 2 ?
O1 K1 2.768(9) . ?
O1 H1A 0.99 . ?
O1 H1B 0.99 . ?
O5 K1 2.679(9) . ?
S1 Pd1 2.287(2) . ?
S1 K1 3.390(4) . ?
S2 Pd1 2.279(3) . ?
S2 K1 3.497(4) 3_545 ?
Cl2 K1 3.457(4) 3_545 ?
K1 O1 2.759(8) 2 ?
K1 O6 2.828(9) . ?
K1 Cl2 3.457(4) 3_455 ?
K1 S2 3.497(4) 3_455 ?
K1 K1 3.870(6) 2 ?
Pd1 S2 2.279(3) 2_655 ?
Pd1 S1 2.287(2) 2_655 ?
O6 C61 1.384(19) . ?
O6 C61 1.384(19) 2 ?
O6 K1 2.828(9) 2 ?
C61 C62 1.36(2) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C62 C62 1.43(4) 2 ?
C62 H62A 0.99 . ?
C62 H62B 0.99 . ?

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
C2 C1 C6 119.7(10) . . ?
C2 C1 S1 120.0(9) . . ?
C6 C1 S1 120.3(7) . . ?
C3 C2 C1 122.5(11) . . ?
C3 C2 Cl1 117.8(9) . . ?
C1 C2 Cl1 119.6(9) . . ?
C2 C3 C4 118.0(11) . . ?
C2 C3 H3 121 . . ?
C4 C3 H3 121 . . ?
C5 C4 C3 120.7(11) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 123.1(11) . . ?
C4 C5 Cl2 118.8(9) . . ?
C6 C5 Cl2 118.1(8) . . ?
C5 C6 C1 116.0(10) . . ?
C5 C6 S2 121.9(9) . . ?
C1 C6 S2 122.1(8) . . ?
O5 C51 C52 102.4(14) . . ?
O5 C51 H51A 111.3 . . ?
C52 C51 H51A 111.3 . . ?
O5 C51 H51B 111.3 . . ?
C52 C51 H51B 111.3 . . ?
H51A C51 H51B 109.2 . . ?
C53 C52 C51 112.3(18) . . ?
C53 C52 H52A 109.1 . . ?
C51 C52 H52A 109.1 . . ?
C53 C52 H52B 109.1 . . ?
C51 C52 H52B 109.1 . . ?
H52A C52 H52B 107.9 . . ?
C52 C53 C54 105.2(16) . . ?
C52 C53 H53A 110.7 . . ?
C54 C53 H53A 110.7 . . ?
C52 C53 H53B 110.7 . . ?
C54 C53 H53B 110.7 . . ?
H53A C53 H53B 108.8 . . ?
O5 C54 C53 106.5(15) . . ?
O5 C54 H54A 110.4 . . ?
C53 C54 H54A 110.4 . . ?
O5 C54 H54B 110.4 . . ?
C53 C54 H54B 110.4 . . ?
H54A C54 H54B 108.6 . . ?
K1 O1 K1 88.9(2) 2 . ?
K1 O1 H1A 113.8 2 . ?
K1 O1 H1A 113.8 . . ?
K1 O1 H1B 113.8 2 . ?
K1 O1 H1B 113.8 . . ?
H1A O1 H1B 111.1 . . ?
C51 O5 C54 111.0(13) . . ?
C51 O5 K1 131.4(10) . . ?
C54 O5 K1 117.5(10) . . ?
C1 S1 Pd1 103.5(3) . . ?
C1 S1 K1 102.7(3) . . ?
Pd1 S1 K1 96.68(9) . . ?
C6 S2 Pd1 104.3(4) . . ?
C6 S2 K1 119.5(4) . 3_545 ?
Pd1 S2 K1 131.47(11) . 3_545 ?
C5 Cl2 K1 121.4(4) . 3_545 ?
O5 K1 O1 154.1(3) . 2 ?
O5 K1 O1 84.7(3) . . ?
O1 K1 O1 87.0(2) 2 . ?
O5 K1 O6 84.0(3) . . ?
O1 K1 O6 70.1(2) 2 . ?
O1 K1 O6 70.0(2) . . ?
O5 K1 S1 98.2(2) . . ?
O1 K1 S1 88.93(19) 2 . ?
O1 K1 S1 175.6(2) . . ?
O6 K1 S1 106.99(14) . . ?
O5 K1 Cl2 64.3(2) . 3_455 ?
O1 K1 Cl2 136.6(2) 2 3_455 ?
O1 K1 Cl2 75.77(19) . 3_455 ?
O6 K1 Cl2 134.97(12) . 3_455 ?
S1 K1 Cl2 108.43(11) . 3_455 ?
O5 K1 S2 113.6(2) . 3_455 ?
O1 K1 S2 83.16(19) 2 3_455 ?
O1 K1 S2 60.78(19) . 3_455 ?
O6 K1 S2 124.63(18) . 3_455 ?
S1 K1 S2 120.40(10) . 3_455 ?
Cl2 K1 S2 53.63(8) 3_455 3_455 ?
O5 K1 K1 115.4(3) . 2 ?
O1 K1 K1 45.7(2) 2 2 ?
O1 K1 K1 45.46(18) . 2 ?
O6 K1 K1 46.83(17) . 2 ?
S1 K1 K1 130.14(12) . 2 ?
Cl2 K1 K1 118.81(12) 3_455 2 ?
S2 K1 K1 79.71(6) 3_455 2 ?
S2 Pd1 S2 89.94(13) . 2_655 ?
S2 Pd1 S1 89.74(9) . . ?
S2 Pd1 S1 177.59(9) 2_655 . ?
S2 Pd1 S1 177.59(9) . 2_655 ?
S2 Pd1 S1 89.74(9) 2_655 2_655 ?
S1 Pd1 S1 90.68(13) . 2_655 ?
C61 O6 C61 103.5(18) . 2 ?
C61 O6 K1 119.3(8) . 2 ?
C61 O6 K1 114.5(9) 2 2 ?
C61 O6 K1 114.5(9) . . ?
C61 O6 K1 119.3(8) 2 . ?
K1 O6 K1 86.3(3) 2 . ?
C62 C61 O6 112.4(17) . . ?
C62 C61 H61A 109.1 . . ?
O6 C61 H61A 109.1 . . ?
C62 C61 H61B 109.1 . . ?
O6 C61 H61B 109.1 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 C62 105.8(12) . 2 ?
C61 C62 H62A 110.6 . . ?
C62 C62 H62A 110.6 2 . ?
C61 C62 H62B 110.6 . . ?
C62 C62 H62B 110.6 2 . ?
H62A C62 H62B 108.7 . . ?



# END of CIF



####################################################################### 
# 
# 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_DH67PtK
_database_code_depnum_ccdc_archive 'CCDC 1450247'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;

_audit_creation_date             2014-01-20T14:42:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H56 Cl4 K2 O8 Pt1 S4'
_chemical_formula_sum            'C36 H56 Cl4 K2 O8 Pt1 S4'
_chemical_formula_weight         1160.13
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   13.933(5)
_cell_length_b                   9.234(3)
_cell_length_c                   18.4983(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.239(15)
_cell_angle_gamma                90
_cell_volume                     2349.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    783
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.29
_exptl_crystal_density_diffrn    1.64
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -10 -1 0.166
-1 3 -7 0.28
-1 12 3 0.27
1 3 14 0.249
1 -4 6 0.288
18 7 -8 0.267
3 -1 5 0.274
-1 -3 6 0.238
1 1 -2 0.297
-3 0 -2 0.269
-5 -2 3 0.209

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_T_max  0.196


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_number            44170
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.138
_diffrn_reflns_theta_max         27.616
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_number_total             5405
_reflns_number_gt                3409
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0033P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5405
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.393
_refine_diff_density_min         -2.331
_refine_diff_density_rms         0.133

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.7768(3) 0.0734(5) -0.0731(2) 0.0344(11) Uani 1 d . .
C12 C 0.6951(4) 0.1172(5) -0.1203(3) 0.0424(12) Uani 1 d . .
C13 C 0.6031(4) 0.1369(5) -0.0995(3) 0.0518(14) Uani 1 d . .
H13 H 0.5479 0.1653 -0.1335 0.062 Uiso 1 calc . .
C14 C 0.5983(4) 0.1120(6) -0.0257(3) 0.0510(14) Uani 1 d . .
H14 H 0.5381 0.1253 -0.0086 0.061 Uiso 1 calc . .
C15 C 0.6777(4) 0.0693(6) 0.0225(3) 0.0453(13) Uani 1 d . .
C16 C 0.7703(3) 0.0468(5) 0.0013(3) 0.0360(11) Uani 1 d . .
C201 C 1.0410(5) -0.3377(7) -0.1561(4) 0.084(2) Uani 1 d . .
H20A H 1.0839 -0.4238 -0.152 0.101 Uiso 1 calc . .
H20B H 1.0585 -0.2778 -0.1116 0.101 Uiso 1 calc . .
C202 C 1.0517(6) -0.2535(12) -0.2218(4) 0.123(4) Uani 1 d . .
H20C H 1.0853 -0.161 -0.2076 0.147 Uiso 1 calc . .
H20D H 1.0907 -0.3085 -0.2527 0.147 Uiso 1 calc . .
C203 C 0.9578(6) -0.2262(9) -0.2613(4) 0.112(3) Uani 1 d . .
H20E H 0.9561 -0.2469 -0.314 0.134 Uiso 1 calc . .
H20F H 0.9398 -0.1235 -0.2559 0.134 Uiso 1 calc . .
C204 C 0.8898(4) -0.3217(7) -0.2308(3) 0.0706(18) Uani 1 d . .
H20G H 0.8326 -0.2663 -0.2207 0.085 Uiso 1 calc . .
H20H H 0.867 -0.4005 -0.2657 0.085 Uiso 1 calc . .
C301 C 0.7249(4) -0.5686(7) 0.0547(4) 0.0754(19) Uani 1 d . .
H30A H 0.7552 -0.6454 0.0882 0.091 Uiso 1 calc . .
H30B H 0.7275 -0.599 0.0038 0.091 Uiso 1 calc . .
C302 C 0.6244(5) -0.5471(9) 0.0647(5) 0.105(3) Uani 1 d . .
H30C H 0.603 -0.625 0.0952 0.126 Uiso 1 calc . .
H30D H 0.5806 -0.5452 0.0169 0.126 Uiso 1 calc . .
C303 C 0.6250(5) -0.4057(8) 0.1018(4) 0.101(3) Uani 1 d . .
H30E H 0.5849 -0.3349 0.0701 0.121 Uiso 1 calc . .
H30F H 0.5985 -0.4154 0.1481 0.121 Uiso 1 calc . .
C304 C 0.7251(5) -0.3581(8) 0.1166(4) 0.110(3) Uani 1 d . .
H30G H 0.7295 -0.2532 0.1066 0.132 Uiso 1 calc . .
H30H H 0.7531 -0.3764 0.1684 0.132 Uiso 1 calc . .
C401 C 0.6724(6) -0.4764(7) -0.1597(4) 0.087(2) Uani 1 d . .
H40A H 0.6464 -0.5562 -0.1328 0.104 Uiso 1 calc . .
H40B H 0.7249 -0.5151 -0.1845 0.104 Uiso 1 calc . .
C402 C 0.5933(6) -0.4110(12) -0.2144(4) 0.120(3) Uani 1 d . .
H40C H 0.6135 -0.4063 -0.2632 0.144 Uiso 1 calc . .
H40D H 0.5334 -0.4701 -0.2182 0.144 Uiso 1 calc . .
C403 C 0.5759(6) -0.2678(10) -0.1889(5) 0.113(3) Uani 1 d . .
H40E H 0.5065 -0.2544 -0.1849 0.136 Uiso 1 calc . .
H40F H 0.595 -0.1934 -0.2224 0.136 Uiso 1 calc . .
C404 C 0.6359(6) -0.2595(9) -0.1182(5) 0.131(3) Uani 1 d . .
H40G H 0.6659 -0.1622 -0.1116 0.157 Uiso 1 calc . .
H40H H 0.5952 -0.2738 -0.0795 0.157 Uiso 1 calc . .
Cl1 Cl 0.66647(10) 0.04112(17) 0.11395(8) 0.0607(4) Uani 1 d . .
Cl2 Cl 0.70053(10) 0.14762(17) -0.21285(7) 0.0625(4) Uani 1 d . .
K3 K 0.88691(8) -0.33103(12) -0.02412(6) 0.0488(3) Uani 1 d . .
O2 O 1.0645(2) -0.3922(4) 0.06962(17) 0.0540(9) Uani 1 d . .
H2A H 1.1152 -0.3205 0.0631 0.065 Uiso 1 calc . .
H2B H 1.0555 -0.3928 0.1216 0.065 Uiso 1 calc . .
O21 O 0.9428(3) -0.3802(4) -0.16412(19) 0.0620(10) Uani 1 d . .
O31 O 0.7751(3) -0.4380(5) 0.0700(2) 0.0722(12) Uani 1 d . .
O41 O 0.7079(3) -0.3631(5) -0.1113(2) 0.0767(12) Uani 1 d . .
Pt1 Pt 1 0 0 0.03259(10) Uani 1 d . .
S1 S 0.88935(9) 0.04803(15) -0.10419(6) 0.0388(3) Uani 1 d . .
S2 S 0.87180(9) -0.01010(12) 0.06429(7) 0.0378(3) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C11 C12 1.380(6) . ?
C11 C16 1.415(6) . ?
C11 S1 1.770(4) . ?
C12 C13 1.407(6) . ?
C12 Cl2 1.749(5) . ?
C13 C14 1.397(6) . ?
C14 C15 1.363(7) . ?
C15 C16 1.423(6) . ?
C15 Cl1 1.744(5) . ?
C16 S2 1.761(5) . ?
C201 O21 1.408(7) . ?
C201 C202 1.470(9) . ?
C202 C203 1.415(10) . ?
C203 C204 1.471(8) . ?
C204 O21 1.437(6) . ?
C301 O31 1.400(7) . ?
C301 C302 1.455(8) . ?
C302 C303 1.475(10) . ?
C303 C304 1.446(8) . ?
C304 O31 1.402(7) . ?
C401 O41 1.414(7) . ?
C401 C402 1.499(10) . ?
C402 C403 1.436(11) . ?
C403 C404 1.437(9) . ?
C404 O41 1.377(8) . ?
K3 O31 2.702(4) . ?
K3 O41 2.760(4) . ?
K3 O2 2.808(4) 3_745 ?
K3 O2 2.841(3) . ?
K3 O21 2.858(4) . ?
K3 S2 3.4076(18) . ?
K3 Pt1 3.4351(14) . ?
K3 K3 4.423(2) 3_745 ?
O2 K3 2.808(4) 3_745 ?
Pt1 S2 2.3013(13) . ?
Pt1 S2 2.3013(13) 3_755 ?
Pt1 S1 2.3095(13) 3_755 ?
Pt1 S1 2.3096(13) . ?
Pt1 K3 3.4350(14) 3_755 ?

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 C11 C16 119.4(4) . . ?
C12 C11 S1 121.2(3) . . ?
C16 C11 S1 119.5(4) . . ?
C11 C12 C13 124.1(4) . . ?
C11 C12 Cl2 120.3(3) . . ?
C13 C12 Cl2 115.6(4) . . ?
C14 C13 C12 115.8(5) . . ?
C15 C14 C13 121.6(4) . . ?
C14 C15 C16 122.7(5) . . ?
C14 C15 Cl1 119.2(4) . . ?
C16 C15 Cl1 118.1(4) . . ?
C11 C16 C15 116.4(4) . . ?
C11 C16 S2 121.7(3) . . ?
C15 C16 S2 121.9(4) . . ?
O21 C201 C202 106.6(6) . . ?
C203 C202 C201 108.3(6) . . ?
C202 C203 C204 107.1(7) . . ?
O21 C204 C203 106.3(5) . . ?
O31 C301 C302 108.5(6) . . ?
C301 C302 C303 104.2(6) . . ?
C304 C303 C302 106.9(6) . . ?
O31 C304 C303 106.5(6) . . ?
O41 C401 C402 105.9(6) . . ?
C403 C402 C401 107.1(6) . . ?
C402 C403 C404 104.1(7) . . ?
O41 C404 C403 110.9(7) . . ?
O31 K3 O41 77.09(14) . . ?
O31 K3 O2 92.99(12) . 3_745 ?
O41 K3 O2 88.06(12) . 3_745 ?
O31 K3 O2 93.99(12) . . ?
O41 K3 O2 162.19(12) . . ?
O2 K3 O2 76.91(11) 3_745 . ?
O31 K3 O21 142.63(12) . . ?
O41 K3 O21 78.81(12) . . ?
O2 K3 O21 57.97(10) 3_745 . ?
O2 K3 O21 100.62(10) . . ?
O31 K3 S2 85.55(10) . . ?
O41 K3 S2 104.71(10) . . ?
O2 K3 S2 166.41(8) 3_745 . ?
O2 K3 S2 89.70(8) . . ?
O21 K3 S2 128.31(8) . . ?
O31 K3 Pt1 122.79(10) . . ?
O41 K3 Pt1 121.61(10) . . ?
O2 K3 Pt1 136.15(8) 3_745 . ?
O2 K3 Pt1 76.19(8) . . ?
O21 K3 Pt1 94.18(8) . . ?
S2 K3 Pt1 39.30(3) . . ?
O31 K3 K3 94.46(11) . 3_745 ?
O41 K3 K3 126.16(10) . 3_745 ?
O2 K3 K3 38.72(7) 3_745 3_745 ?
O2 K3 K3 38.19(7) . 3_745 ?
O21 K3 K3 77.39(8) . 3_745 ?
S2 K3 K3 127.86(5) . 3_745 ?
Pt1 K3 K3 107.73(5) . 3_745 ?
K3 O2 K3 103.09(11) 3_745 . ?
C201 O21 C204 110.0(4) . . ?
C201 O21 K3 105.2(4) . . ?
C204 O21 K3 122.7(3) . . ?
C301 O31 C304 107.1(4) . . ?
C301 O31 K3 120.5(3) . . ?
C304 O31 K3 126.8(4) . . ?
C404 O41 C401 106.2(5) . . ?
C404 O41 K3 123.8(4) . . ?
C401 O41 K3 129.9(4) . . ?
S2 Pt1 S2 180 . 3_755 ?
S2 Pt1 S1 91.75(5) . 3_755 ?
S2 Pt1 S1 88.25(5) 3_755 3_755 ?
S2 Pt1 S1 88.25(5) . . ?
S2 Pt1 S1 91.75(5) 3_755 . ?
S1 Pt1 S1 180 3_755 . ?
S2 Pt1 K3 110.30(3) . 3_755 ?
S2 Pt1 K3 69.70(3) 3_755 3_755 ?
S1 Pt1 K3 80.31(4) 3_755 3_755 ?
S1 Pt1 K3 99.69(4) . 3_755 ?
S2 Pt1 K3 69.70(3) . . ?
S2 Pt1 K3 110.29(3) 3_755 . ?
S1 Pt1 K3 99.69(4) 3_755 . ?
S1 Pt1 K3 80.31(4) . . ?
K3 Pt1 K3 180 3_755 . ?
C11 S1 Pt1 105.15(16) . . ?
C16 S2 Pt1 104.68(16) . . ?
C16 S2 K3 92.69(16) . . ?
Pt1 S2 K3 70.99(3) . . ?

# END of CIF


####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1450248'
_audit_update_record             
;
2016-01-27 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;

_audit_creation_date             2015-01-29T11:03:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C20 H22 Cl4 K2 O3 Pt S4'
_chemical_formula_sum            'C20 H22 Cl4 K2 O3 Pt S4'
_chemical_formula_weight         853.7

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2056(7)
_cell_length_b                   12.7042(11)
_cell_length_c                   14.4749(8)
_cell_angle_alpha                82.782(5)
_cell_angle_beta                 74.848(5)
_cell_angle_gamma                76.633(7)
_cell_volume                     1413.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    120
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 12 0 0.037
-1 -10 1 0.117
-1 -4 -17 0.275
1 2 13 0.145
-5 -1 -2 0.115
5 1 6 0.142
7 1 -4 0.16
-4 -1 -8 0.184


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    5.954
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_T_max  0.343

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_number            30685
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.256
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             6479
_reflns_number_gt                4584
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0428P)²+17.9314P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6479
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.099
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1585
_refine_ls_wR_factor_gt          0.1441
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.9
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.229

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0087(14) 0.7540(9) -0.0529(7) 0.029(2) Uani 1 1 d . . . . .
C2 C -0.0521(13) 0.8612(9) -0.0901(8) 0.034(2) Uani 1 1 d . . . . .
C3 C 0.0549(14) 0.9330(10) -0.0994(9) 0.037(3) Uani 1 1 d . . . . .
H3 H 0.0269 1.0029 -0.1269 0.045 Uiso 1 1 calc R U . . .
C4 C 0.7957(14) 0.1005(10) 0.0673(9) 0.039(3) Uani 1 1 d . . . . .
H4 H 0.724 0.0524 0.0709 0.047 Uiso 1 1 calc R U . . .
C5 C 0.7534(14) 0.2062(9) 0.0295(7) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.1426(13) 0.7194(8) -0.0221(7) 0.027(2) Uani 1 1 d . . . . .
C7 C -0.0990(15) 0.7603(9) -0.5083(8) 0.033(2) Uani 1 1 d . . . . .
C8 C -0.1759(15) 0.8675(9) -0.4884(8) 0.038(3) Uani 1 1 d . . . . .
C9 C 1.1322(18) 0.0461(9) -0.4508(9) 0.049(3) Uani 1 1 d . . . . .
H9 H 1.1823 -0.0247 -0.4671 0.058 Uiso 1 1 calc R U . . .
C10 C 1.0113(16) 0.0664(10) -0.3638(9) 0.042(3) Uani 1 1 d . . . . .
H10 H 0.9802 0.0092 -0.3211 0.05 Uiso 1 1 calc R U . . .
C11 C 0.9383(15) 0.1719(9) -0.3418(8) 0.036(3) Uani 1 1 d . . . . .
C12 C -0.0222(14) 0.2596(8) -0.4047(8) 0.029(2) Uani 1 1 d . . . . .
C21 C 0.274(2) 0.6828(12) -0.2624(9) 0.056(4) Uani 1 1 d . . . . .
H21A H 0.3722 0.7044 -0.2501 0.067 Uiso 1 1 calc R U . . .
H21B H 0.1854 0.6827 -0.2032 0.067 Uiso 1 1 calc R U . . .
C22 C 0.208(2) 0.7563(12) -0.3373(11) 0.063(4) Uani 1 1 d . . . . .
H22A H 0.2127 0.8306 -0.3312 0.075 Uiso 1 1 calc R U . . .
H22B H 0.09 0.7526 -0.3343 0.075 Uiso 1 1 calc R U . . .
C23 C 0.3282(18) 0.7143(12) -0.4290(10) 0.056(4) Uani 1 1 d . . . . .
H23A H 0.2703 0.7279 -0.4811 0.067 Uiso 1 1 calc R U . . .
H23B H 0.429 0.7468 -0.4473 0.067 Uiso 1 1 calc R U . . .
C24 C 0.3760(16) 0.5951(11) -0.4026(8) 0.046(3) Uani 1 1 d . . . . .
H24A H 0.3178 0.5553 -0.4322 0.055 Uiso 1 1 calc R U . . .
H24B H 0.4996 0.5693 -0.425 0.055 Uiso 1 1 calc R U . . .
C31 C 0.3964(17) 0.2982(10) -0.3390(8) 0.044(3) Uani 1 1 d . . . . .
H31A H 0.4982 0.3293 -0.3622 0.053 Uiso 1 1 calc R U . . .
H31B H 0.315 0.3301 -0.3779 0.053 Uiso 1 1 calc R U . . .
C32 C 0.4442(18) 0.1757(10) -0.3436(9) 0.048(3) Uani 1 1 d . . . . .
H32A H 0.3973 0.1535 -0.3913 0.058 Uiso 1 1 calc R U . . .
H32B H 0.5686 0.1508 -0.3601 0.058 Uiso 1 1 calc R U . . .
C33 C 0.367(2) 0.1304(12) -0.2456(11) 0.066(4) Uani 1 1 d . . . . .
H33A H 0.3012 0.0775 -0.2492 0.079 Uiso 1 1 calc R U . . .
H33B H 0.4567 0.096 -0.2125 0.079 Uiso 1 1 calc R U . . .
C34 C 0.254(2) 0.2257(14) -0.1958(11) 0.069(5) Uani 1 1 d . . . . .
H34A H 0.1364 0.2334 -0.2015 0.083 Uiso 1 1 calc R U . . .
H34B H 0.2536 0.2172 -0.1282 0.083 Uiso 1 1 calc R U . . .
Cl1 Cl -0.2391(4) 0.9051(3) -0.1307(3) 0.0551(9) Uani 1 1 d . . . . .
Cl2 Cl 0.5597(3) 0.2448(2) -0.0040(2) 0.0403(7) Uani 1 1 d . . . . .
Cl3 Cl -0.3279(5) 0.8940(3) -0.3811(3) 0.0645(11) Uani 1 1 d . . . . .
Cl4 Cl 0.7932(4) 0.1939(2) -0.2306(2) 0.0431(7) Uani 1 1 d . . . . .
K1 K 0.0319(3) 0.4917(2) -0.24083(19) 0.0450(7) Uani 1 1 d . . . . .
K2 K 0.5041(4) 0.4435(2) -0.1720(2) 0.0430(6) Uani 1 1 d . . . . .
O1 O 0.3250(11) 0.5782(7) -0.3000(6) 0.043(2) Uani 1 1 d . . . . .
O2 O 0.3199(11) 0.3178(7) -0.2400(6) 0.043(2) Uani 1 1 d . . . . .
O3 O -0.3219(12) 0.6079(7) -0.2087(6) 0.047(2) Uani 1 1 d . . . . .
H3A H -0.3528 0.6523 -0.1544 0.056 Uiso 1 1 calc R U . . .
H3B H -0.3435 0.6534 -0.2651 0.056 Uiso 1 1 calc R U . . .
Pt1 Pt 0 0.5 0 0.02664(16) Uani 1 2 d S . P . .
Pt2 Pt 0 0.5 -0.5 0.02815(17) Uani 1 2 d S . P . .
S1 S -0.1445(3) 0.6639(2) -0.0496(2) 0.0328(6) Uani 1 1 d . . . . .
S2 S 0.2085(3) 0.5839(2) 0.01848(19) 0.0301(6) Uani 1 1 d . . . . .
S3 S -0.1644(4) 0.6524(2) -0.4300(2) 0.0385(7) Uani 1 1 d . . . . .
S4 S -0.1321(3) 0.3932(2) -0.37691(19) 0.0308(6) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.386(14) . ?
C1 C2 1.401(15) . ?
C1 S1 1.761(11) . ?
C2 C3 1.378(16) . ?
C2 Cl1 1.733(11) . ?
C3 C4 1.381(16) 2_665 ?
C3 H3 0.93 . ?
C4 C3 1.381(16) 2_665 ?
C4 C5 1.387(16) . ?
C4 H4 0.93 . ?
C5 C6 1.390(15) 2_665 ?
C5 Cl2 1.727(11) . ?
C6 C5 1.390(15) 2_665 ?
C6 S2 1.755(10) . ?
C7 C12 1.395(16) 2_564 ?
C7 C8 1.394(15) . ?
C7 S3 1.756(11) . ?
C8 C9 1.373(17) 2_664 ?
C8 Cl3 1.734(12) . ?
C9 C8 1.373(17) 2_664 ?
C9 C10 1.395(18) . ?
C9 H9 0.93 . ?
C10 C11 1.375(16) . ?
C10 H10 0.93 . ?
C11 C12 1.391(15) 1_655 ?
C11 Cl4 1.744(12) . ?
C12 C7 1.395(16) 2_564 ?
C12 C11 1.391(15) 1_455 ?
C12 S4 1.770(11) . ?
C21 O1 1.429(16) . ?
C21 C22 1.470(19) . ?
C21 K1 3.415(17) . ?
C21 K2 3.486(14) . ?
C21 H21A 0.97 . ?
C21 H21B 0.97 . ?
C22 C23 1.51(2) . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C23 C24 1.501(19) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C24 O1 1.435(14) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C31 O2 1.434(14) . ?
C31 C32 1.520(17) . ?
C31 K1 3.502(13) . ?
C31 H31A 0.97 . ?
C31 H31B 0.97 . ?
C32 C33 1.496(18) . ?
C32 H32A 0.97 . ?
C32 H32B 0.97 . ?
C33 C34 1.48(2) . ?
C33 H33A 0.97 . ?
C33 H33B 0.97 . ?
C34 O2 1.412(17) . ?
C34 K1 3.519(19) . ?
C34 H34A 0.97 . ?
C34 H34B 0.97 . ?
Cl2 K2 3.317(4) . ?
Cl4 K2 3.543(4) . ?
K1 O1 2.763(9) . ?
K1 O2 2.839(9) . ?
K1 O3 2.883(9) . ?
K1 S4 3.169(4) . ?
K1 Pt1 3.440(3) . ?
K1 S2 3.457(4) 2_565 ?
K1 S1 3.537(4) . ?
K1 S3 3.694(4) . ?
K1 Pt2 3.815(3) . ?
K2 O3 2.717(9) 1_655 ?
K2 O1 2.825(8) . ?
K2 O2 2.844(9) . ?
K2 S2 3.523(4) . ?
K2 S2 3.576(4) 2_665 ?
K2 S4 3.617(4) 1_655 ?
K2 K1 4.353(4) 1_655 ?
O3 K2 2.717(9) 1_455 ?
O3 H3A 0.97 . ?
O3 H3B 0.97 . ?
Pt1 S1 2.277(3) 2_565 ?
Pt1 S1 2.277(3) . ?
Pt1 S2 2.300(3) . ?
Pt1 S2 2.300(3) 2_565 ?
Pt1 K1 3.440(3) 2_565 ?
Pt2 S3 2.273(3) . ?
Pt2 S3 2.273(3) 2_564 ?
Pt2 S4 2.292(3) 2_564 ?
Pt2 S4 2.292(3) . ?
Pt2 K1 3.815(3) 2_564 ?
S2 K1 3.457(4) 2_565 ?
S2 K2 3.577(4) 2_665 ?
S4 K2 3.617(4) 1_455 ?

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
C6 C1 C2 119.8(10) . . ?
C6 C1 S1 120.9(8) . . ?
C2 C1 S1 119.2(8) . . ?
C3 C2 C1 121.4(10) . . ?
C3 C2 Cl1 118.2(9) . . ?
C1 C2 Cl1 120.3(9) . . ?
C4 C3 C2 119.0(11) 2_665 . ?
C4 C3 H3 120.5 2_665 . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.6(11) 2_665 . ?
C3 C4 H4 120.2 2_665 . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 122.1(10) . 2_665 ?
C4 C5 Cl2 117.3(8) . . ?
C6 C5 Cl2 120.6(8) 2_665 . ?
C1 C6 C5 118.0(10) . 2_665 ?
C1 C6 S2 121.4(8) . . ?
C5 C6 S2 120.5(8) 2_665 . ?
C12 C7 C8 118.5(10) 2_564 . ?
C12 C7 S3 120.5(8) 2_564 . ?
C8 C7 S3 120.8(9) . . ?
C9 C8 C7 122.5(11) 2_664 . ?
C9 C8 Cl3 118.2(9) 2_664 . ?
C7 C8 Cl3 119.2(9) . . ?
C8 C9 C10 118.7(11) 2_664 . ?
C8 C9 H9 120.6 2_664 . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 119.4(11) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 122.1(11) . 1_655 ?
C10 C11 Cl4 117.9(9) . . ?
C12 C11 Cl4 120.0(9) 1_655 . ?
C7 C12 C11 118.8(10) 2_564 1_455 ?
C7 C12 S4 121.0(8) 2_564 . ?
C11 C12 S4 120.2(9) 1_455 . ?
O1 C21 C22 105.0(11) . . ?
O1 C21 K1 51.5(7) . . ?
C22 C21 K1 98.7(10) . . ?
O1 C21 K2 51.5(5) . . ?
C22 C21 K2 155.0(9) . . ?
K1 C21 K2 73.7(3) . . ?
O1 C21 H21A 110.7 . . ?
C22 C21 H21A 110.7 . . ?
K1 C21 H21A 149.5 . . ?
K2 C21 H21A 76.2 . . ?
O1 C21 H21B 110.7 . . ?
C22 C21 H21B 110.7 . . ?
K1 C21 H21B 65.7 . . ?
K2 C21 H21B 88.2 . . ?
H21A C21 H21B 108.8 . . ?
C21 C22 C23 103.3(11) . . ?
C21 C22 H22A 111.1 . . ?
C23 C22 H22A 111.1 . . ?
C21 C22 H22B 111.1 . . ?
C23 C22 H22B 111.1 . . ?
H22A C22 H22B 109.1 . . ?
C24 C23 C22 102.3(10) . . ?
C24 C23 H23A 111.3 . . ?
C22 C23 H23A 111.3 . . ?
C24 C23 H23B 111.3 . . ?
C22 C23 H23B 111.3 . . ?
H23A C23 H23B 109.2 . . ?
O1 C24 C23 108.2(10) . . ?
O1 C24 H24A 110.1 . . ?
C23 C24 H24A 110.1 . . ?
O1 C24 H24B 110.1 . . ?
C23 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
O2 C31 C32 106.1(10) . . ?
O2 C31 K1 51.5(5) . . ?
C32 C31 K1 137.1(8) . . ?
O2 C31 H31A 110.5 . . ?
C32 C31 H31A 110.5 . . ?
K1 C31 H31A 111.8 . . ?
O2 C31 H31B 110.5 . . ?
C32 C31 H31B 110.5 . . ?
K1 C31 H31B 61.5 . . ?
H31A C31 H31B 108.7 . . ?
C33 C32 C31 105.6(11) . . ?
C33 C32 H32A 110.6 . . ?
C31 C32 H32A 110.6 . . ?
C33 C32 H32B 110.6 . . ?
C31 C32 H32B 110.6 . . ?
H32A C32 H32B 108.7 . . ?
C34 C33 C32 104.6(12) . . ?
C34 C33 H33A 110.8 . . ?
C32 C33 H33A 110.8 . . ?
C34 C33 H33B 110.8 . . ?
C32 C33 H33B 110.8 . . ?
H33A C33 H33B 108.9 . . ?
O2 C34 C33 107.1(11) . . ?
O2 C34 K1 50.6(7) . . ?
C33 C34 K1 141.8(11) . . ?
O2 C34 H34A 110.3 . . ?
C33 C34 H34A 110.3 . . ?
K1 C34 H34A 63.9 . . ?
O2 C34 H34B 110.3 . . ?
C33 C34 H34B 110.3 . . ?
K1 C34 H34B 107 . . ?
H34A C34 H34B 108.5 . . ?
C5 Cl2 K2 120.7(4) . . ?
C11 Cl4 K2 124.1(4) . . ?
O1 K1 O2 72.7(2) . . ?
O1 K1 O3 127.3(3) . . ?
O2 K1 O3 159.7(3) . . ?
O1 K1 S4 125.1(2) . . ?
O2 K1 S4 97.10(19) . . ?
O3 K1 S4 74.63(18) . . ?
O1 K1 C21 23.9(3) . . ?
O2 K1 C21 92.7(3) . . ?
O3 K1 C21 106.1(3) . . ?
S4 K1 C21 136.9(2) . . ?
O1 K1 Pt1 94.77(18) . . ?
O2 K1 Pt1 86.66(18) . . ?
O3 K1 Pt1 87.97(17) . . ?
S4 K1 Pt1 139.32(10) . . ?
C21 K1 Pt1 83.0(2) . . ?
O1 K1 S2 133.55(19) . 2_565 ?
O2 K1 S2 95.42(19) . 2_565 ?
O3 K1 S2 68.60(18) . 2_565 ?
S4 K1 S2 100.50(10) . 2_565 ?
C21 K1 S2 120.3(2) . 2_565 ?
Pt1 K1 S2 38.95(5) . 2_565 ?
O1 K1 C31 68.1(3) . . ?
O2 K1 C31 23.3(3) . . ?
O3 K1 C31 156.6(3) . . ?
S4 K1 C31 82.0(2) . . ?
C21 K1 C31 91.7(3) . . ?
Pt1 K1 C31 109.6(2) . . ?
S2 K1 C31 115.6(2) 2_565 . ?
O1 K1 C34 95.0(3) . . ?
O2 K1 C34 22.6(3) . . ?
O3 K1 C34 137.1(3) . . ?
S4 K1 C34 87.0(3) . . ?
C21 K1 C34 113.5(3) . . ?
Pt1 K1 C34 81.3(3) . . ?
S2 K1 C34 77.5(2) 2_565 . ?
C31 K1 C34 38.1(3) . . ?
O1 K1 S1 92.3(2) . . ?
O2 K1 S1 122.17(18) . . ?
O3 K1 S1 59.85(18) . . ?
S4 K1 S1 133.46(10) . . ?
C21 K1 S1 70.3(2) . . ?
Pt1 K1 S1 38.07(5) . . ?
S2 K1 S1 55.69(8) 2_565 . ?
C31 K1 S1 142.7(2) . . ?
C34 K1 S1 119.3(3) . . ?
O1 K1 S3 92.92(19) . . ?
O2 K1 S3 134.48(19) . . ?
O3 K1 S3 55.76(17) . . ?
S4 K1 S3 55.92(8) . . ?
C21 K1 S3 88.0(2) . . ?
Pt1 K1 S3 138.36(9) . . ?
S2 K1 S3 123.01(9) 2_565 . ?
C31 K1 S3 111.2(2) . . ?
C34 K1 S3 138.6(3) . . ?
S1 K1 S3 100.83(9) . . ?
O1 K1 Pt2 90.74(18) . . ?
O2 K1 Pt2 100.55(18) . . ?
O3 K1 Pt2 84.06(17) . . ?
S4 K1 Pt2 36.87(6) . . ?
C21 K1 Pt2 100.0(2) . . ?
Pt1 K1 Pt2 171.98(7) . . ?
S2 K1 Pt2 135.68(8) 2_565 . ?
C31 K1 Pt2 77.8(2) . . ?
C34 K1 Pt2 104.0(3) . . ?
S1 K1 Pt2 136.01(9) . . ?
S3 K1 Pt2 35.19(5) . . ?
O3 K2 O1 80.8(3) 1_655 . ?
O3 K2 O2 147.7(3) 1_655 . ?
O1 K2 O2 71.7(3) . . ?
O3 K2 Cl2 122.7(2) 1_655 . ?
O1 K2 Cl2 155.1(2) . . ?
O2 K2 Cl2 87.5(2) . . ?
O3 K2 C21 67.2(3) 1_655 . ?
O1 K2 C21 23.3(3) . . ?
O2 K2 C21 91.1(3) . . ?
Cl2 K2 C21 153.1(3) . . ?
O3 K2 S2 88.9(2) 1_655 . ?
O1 K2 S2 88.65(18) . . ?
O2 K2 S2 106.60(18) . . ?
Cl2 K2 S2 84.32(9) . . ?
C21 K2 S2 70.3(2) . . ?
O3 K2 Cl4 110.3(2) 1_655 . ?
O1 K2 Cl4 124.0(2) . . ?
O2 K2 Cl4 73.67(19) . . ?
Cl2 K2 Cl4 59.21(8) . . ?
C21 K2 Cl4 145.3(2) . . ?
S2 K2 Cl4 143.53(10) . . ?
O3 K2 S2 68.30(19) 1_655 2_665 ?
O1 K2 S2 147.9(2) . 2_665 ?
O2 K2 S2 140.3(2) . 2_665 ?
Cl2 K2 S2 54.43(8) . 2_665 ?
C21 K2 S2 127.6(3) . 2_665 ?
S2 K2 S2 82.60(9) . 2_665 ?
Cl4 K2 S2 76.76(9) . 2_665 ?
O3 K2 S4 69.3(2) 1_655 1_655 ?
O1 K2 S4 86.53(18) . 1_655 ?
O2 K2 S4 92.09(18) . 1_655 ?
Cl2 K2 S4 108.24(10) . 1_655 ?
C21 K2 S4 98.7(2) . 1_655 ?
S2 K2 S4 158.13(11) . 1_655 ?
Cl4 K2 S4 52.30(7) . 1_655 ?
S2 K2 S4 90.26(9) 2_665 1_655 ?
O3 K2 K1 119.4(2) 1_655 . ?
O1 K2 K1 41.62(18) . . ?
O2 K2 K1 43.20(18) . . ?
Cl2 K2 K1 113.56(10) . . ?
C21 K2 K1 52.4(3) . . ?
S2 K2 K1 75.59(8) . . ?
Cl4 K2 K1 116.48(10) . . ?
S2 K2 K1 156.40(10) 2_665 . ?
S4 K2 K1 113.33(9) 1_655 . ?
O3 K2 K1 40.4(2) 1_655 1_655 ?
O1 K2 K1 109.16(19) . 1_655 ?
O2 K2 K1 136.32(19) . 1_655 ?
Cl2 K2 K1 95.23(8) . 1_655 ?
C21 K2 K1 104.1(3) . 1_655 ?
S2 K2 K1 117.06(9) . 1_655 ?
Cl4 K2 K1 70.71(8) . 1_655 ?
S2 K2 K1 50.55(7) 2_665 1_655 ?
S4 K2 K1 45.71(6) 1_655 1_655 ?
K1 K2 K1 150.09(10) . 1_655 ?
C21 O1 C24 107.1(9) . . ?
C21 O1 K1 104.6(8) . . ?
C24 O1 K1 112.0(7) . . ?
C21 O1 K2 105.2(7) . . ?
C24 O1 K2 129.7(7) . . ?
K1 O1 K2 95.6(3) . . ?
C34 O2 C31 107.4(10) . . ?
C34 O2 K1 106.8(9) . . ?
C31 O2 K1 105.3(7) . . ?
C34 O2 K2 129.8(9) . . ?
C31 O2 K2 110.6(7) . . ?
K1 O2 K2 93.5(3) . . ?
K2 O3 K1 102.0(3) 1_455 . ?
K2 O3 H3A 111.4 1_455 . ?
K1 O3 H3A 111.4 . . ?
K2 O3 H3B 111.4 1_455 . ?
K1 O3 H3B 111.4 . . ?
H3A O3 H3B 109.2 . . ?
S1 Pt1 S1 180 2_565 . ?
S1 Pt1 S2 91.10(9) 2_565 . ?
S1 Pt1 S2 88.90(9) . . ?
S1 Pt1 S2 88.90(9) 2_565 2_565 ?
S1 Pt1 S2 91.10(9) . 2_565 ?
S2 Pt1 S2 180 . 2_565 ?
S1 Pt1 K1 73.26(9) 2_565 2_565 ?
S1 Pt1 K1 106.74(9) . 2_565 ?
S2 Pt1 K1 70.94(8) . 2_565 ?
S2 Pt1 K1 109.07(8) 2_565 2_565 ?
S1 Pt1 K1 106.74(9) 2_565 . ?
S1 Pt1 K1 73.26(9) . . ?
S2 Pt1 K1 109.07(8) . . ?
S2 Pt1 K1 70.93(8) 2_565 . ?
K1 Pt1 K1 180 2_565 . ?
S3 Pt2 S3 180.00(14) . 2_564 ?
S3 Pt2 S4 89.17(10) . 2_564 ?
S3 Pt2 S4 90.83(10) 2_564 2_564 ?
S3 Pt2 S4 90.83(10) . . ?
S3 Pt2 S4 89.17(10) 2_564 . ?
S4 Pt2 S4 180 2_564 . ?
S3 Pt2 K1 69.49(9) . . ?
S3 Pt2 K1 110.51(9) 2_564 . ?
S4 Pt2 K1 123.94(8) 2_564 . ?
S4 Pt2 K1 56.06(8) . . ?
S3 Pt2 K1 110.51(9) . 2_564 ?
S3 Pt2 K1 69.49(9) 2_564 2_564 ?
S4 Pt2 K1 56.06(8) 2_564 2_564 ?
S4 Pt2 K1 123.94(8) . 2_564 ?
K1 Pt2 K1 180 . 2_564 ?
C1 S1 Pt1 104.6(4) . . ?
C1 S1 K1 110.1(4) . . ?
Pt1 S1 K1 68.67(8) . . ?
C6 S2 Pt1 104.0(4) . . ?
C6 S2 K1 114.6(3) . 2_565 ?
Pt1 S2 K1 70.11(8) . 2_565 ?
C6 S2 K2 109.1(3) . . ?
Pt1 S2 K2 89.36(9) . . ?
K1 S2 K2 134.90(10) 2_565 . ?
C6 S2 K2 112.2(4) . 2_665 ?
Pt1 S2 K2 138.36(11) . 2_665 ?
K1 S2 K2 76.44(8) 2_565 2_665 ?
K2 S2 K2 97.40(9) . 2_665 ?
C7 S3 Pt2 105.0(4) . . ?
C7 S3 K1 129.3(4) . . ?
Pt2 S3 K1 75.33(9) . . ?
C12 S4 Pt2 103.9(4) . . ?
C12 S4 K1 112.3(3) . . ?
Pt2 S4 K1 87.08(10) . . ?
C12 S4 K2 121.2(4) . 1_455 ?
Pt2 S4 K2 134.75(11) . 1_455 ?
K1 S4 K2 79.50(9) . 1_455 ?

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
C6 C1 C2 C3 1.8(17) . . . . ?
S1 C1 C2 C3 -176.2(9) . . . . ?
C6 C1 C2 Cl1 179.0(8) . . . . ?
S1 C1 C2 Cl1 1.0(13) . . . . ?
C1 C2 C3 C4 -2.9(18) . . . 2_665 ?
Cl1 C2 C3 C4 179.8(9) . . . 2_665 ?
C3 C4 C5 C6 0.4(17) 2_665 . . 2_665 ?
C3 C4 C5 Cl2 -176.9(9) 2_665 . . . ?
C2 C1 C6 C5 0.1(15) . . . 2_665 ?
S1 C1 C6 C5 178.0(8) . . . 2_665 ?
C2 C1 C6 S2 -176.3(8) . . . . ?
S1 C1 C6 S2 1.7(13) . . . . ?
C12 C7 C8 C9 -2.5(18) 2_564 . . 2_664 ?
S3 C7 C8 C9 -177.8(10) . . . 2_664 ?
C12 C7 C8 Cl3 179.5(8) 2_564 . . . ?
S3 C7 C8 Cl3 4.2(14) . . . . ?
C8 C9 C10 C11 1(2) 2_664 . . . ?
C9 C10 C11 C12 1.7(19) . . . 1_655 ?
C9 C10 C11 Cl4 -177.8(10) . . . . ?
O1 C21 C22 C23 -38.2(16) . . . . ?
K1 C21 C22 C23 -90.6(11) . . . . ?
K2 C21 C22 C23 -21(3) . . . . ?
C21 C22 C23 C24 31.4(16) . . . . ?
C22 C23 C24 O1 -14.1(15) . . . . ?
O2 C31 C32 C33 8.0(15) . . . . ?
K1 C31 C32 C33 -42.1(17) . . . . ?
C31 C32 C33 C34 10.3(16) . . . . ?
C32 C33 C34 O2 -25.7(18) . . . . ?
C32 C33 C34 K1 21(2) . . . . ?
C4 C5 Cl2 K2 -154.1(8) . . . . ?
C6 C5 Cl2 K2 28.6(10) 2_665 . . . ?
C10 C11 Cl4 K2 -163.9(8) . . . . ?
C12 C11 Cl4 K2 16.5(12) 1_655 . . . ?
C22 C21 O1 C24 29.7(14) . . . . ?
K1 C21 O1 C24 119.0(9) . . . . ?
K2 C21 O1 C24 -140.9(9) . . . . ?
C22 C21 O1 K1 -89.3(11) . . . . ?
K2 C21 O1 K1 100.1(5) . . . . ?
C22 C21 O1 K2 170.6(10) . . . . ?
K1 C21 O1 K2 -100.1(5) . . . . ?
C23 C24 O1 C21 -9.2(14) . . . . ?
C23 C24 O1 K1 104.9(10) . . . . ?
C23 C24 O1 K2 -137.0(9) . . . . ?
C33 C34 O2 C31 31.8(16) . . . . ?
K1 C34 O2 C31 -112.5(9) . . . . ?
C33 C34 O2 K1 144.3(11) . . . . ?
C33 C34 O2 K2 -106.1(13) . . . . ?
K1 C34 O2 K2 109.6(9) . . . . ?
C32 C31 O2 C34 -24.5(14) . . . . ?
K1 C31 O2 C34 113.6(11) . . . . ?
C32 C31 O2 K1 -138.1(8) . . . . ?
C32 C31 O2 K2 122.1(9) . . . . ?
K1 C31 O2 K2 -99.8(5) . . . . ?
C6 C1 S1 Pt1 -4.3(9) . . . . ?
C2 C1 S1 Pt1 173.7(8) . . . . ?
C6 C1 S1 K1 -76.5(9) . . . . ?
C2 C1 S1 K1 101.4(9) . . . . ?
C1 C6 S2 Pt1 1.8(9) . . . . ?
C5 C6 S2 Pt1 -174.4(8) 2_665 . . . ?
C1 C6 S2 K1 -72.4(9) . . . 2_565 ?
C5 C6 S2 K1 111.3(8) 2_665 . . 2_565 ?
C1 C6 S2 K2 96.1(8) . . . . ?
C5 C6 S2 K2 -80.2(9) 2_665 . . . ?
C1 C6 S2 K2 -157.2(8) . . . 2_665 ?
C5 C6 S2 K2 26.6(9) 2_665 . . 2_665 ?
C12 C7 S3 Pt2 3.8(10) 2_564 . . . ?
C8 C7 S3 Pt2 179.0(9) . . . . ?
C12 C7 S3 K1 87.0(9) 2_564 . . . ?
C8 C7 S3 K1 -97.8(10) . . . . ?
C7 C12 S4 Pt2 -6.9(9) 2_564 . . . ?
C11 C12 S4 Pt2 176.3(8) 1_455 . . . ?
C7 C12 S4 K1 -99.5(8) 2_564 . . . ?
C11 C12 S4 K1 83.7(9) 1_455 . . . ?
C7 C12 S4 K2 169.5(7) 2_564 . . 1_455 ?
C11 C12 S4 K2 -7.4(10) 1_455 . . 1_455 ?



# END of CIF

