# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1o
_database_code_depnum_ccdc_archive 'CCDC 1504114'
_audit_update_record             
;
2016-09-13 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H42 Cl0 N0 Ni O0 P2 S4'
_chemical_formula_weight         891.73

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'
P P 0.1023 0.0942 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   14.513(6)
_cell_length_b                   24.868(11)
_cell_length_c                   12.425(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.208(9)
_cell_angle_gamma                90.00
_cell_volume                     4483(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11966
_cell_measurement_theta_min      2.1356
_cell_measurement_theta_max      27.7198

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6075
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_process_details   
; 
RIGAKU/MSC(2004), CrystalClear Version 1.3.6, 
  Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34681
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         27.49
_reflns_number_total             10185
_reflns_number_gt                6498
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0967P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10185
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1952
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25230(3) -0.003238(17) 0.54886(3) 0.04215(16) Uani 1 1 d . . .
S1 S 0.20422(7) -0.05783(4) 0.42645(7) 0.0478(2) Uani 1 1 d . . .
S4 S 0.37647(8) 0.08924(4) 0.04126(8) 0.0573(3) Uani 1 1 d . . .
P2 P 0.27862(7) 0.05402(4) 0.67789(8) 0.0480(3) Uani 1 1 d . . .
S2 S 0.29797(7) 0.05291(4) 0.43036(7) 0.0482(2) Uani 1 1 d . . .
P1 P 0.22907(7) -0.06287(4) 0.67337(8) 0.0480(3) Uani 1 1 d . . .
S3 S 0.11620(8) -0.08767(4) 0.03454(8) 0.0577(3) Uani 1 1 d . . .
C17 C 0.2842(4) 0.18779(16) 0.0622(3) 0.0632(12) Uani 1 1 d . . .
C2 C 0.2705(3) 0.02242(14) 0.3046(3) 0.0419(8) Uani 1 1 d . . .
C1 C 0.2297(2) -0.02571(13) 0.3040(3) 0.0407(8) Uani 1 1 d . . .
C14 C 0.2972(3) 0.05469(14) 0.2100(3) 0.0432(8) Uani 1 1 d . . .
C15 C 0.2674(3) 0.10902(14) 0.1928(3) 0.0510(9) Uani 1 1 d . . .
H15A H 0.2275 0.1264 0.2390 0.061 Uiso 1 1 calc R . .
C6 C 0.2117(4) -0.18583(16) 0.0471(3) 0.0628(12) Uani 1 1 d . . .
C45 C 0.3782(3) 0.09851(16) 0.6738(3) 0.0525(9) Uani 1 1 d . . .
C4 C 0.2305(3) -0.11002(14) 0.1851(3) 0.0512(9) Uani 1 1 d . . .
H4A H 0.2726 -0.1280 0.2296 0.061 Uiso 1 1 calc R . .
C3 C 0.1995(3) -0.05698(14) 0.2065(3) 0.0443(8) Uani 1 1 d . . .
C25 C 0.2210(3) -0.02766(18) 0.8027(3) 0.0657(12) Uani 1 1 d . . .
H25A H 0.1604 -0.0117 0.8097 0.079 Uiso 1 1 calc R . .
H25B H 0.2314 -0.0525 0.8619 0.079 Uiso 1 1 calc R . .
C5 C 0.1933(3) -0.13230(15) 0.0941(3) 0.0506(9) Uani 1 1 d . . .
C12 C 0.1367(3) -0.03878(15) 0.1307(3) 0.0503(9) Uani 1 1 d . . .
C28 C 0.4048(3) -0.09978(16) 0.6334(4) 0.0583(10) Uani 1 1 d . . .
H28A H 0.4008 -0.0778 0.5730 0.070 Uiso 1 1 calc R . .
C16 C 0.3018(3) 0.13338(15) 0.1041(3) 0.0532(10) Uani 1 1 d . . .
C47 C 0.5406(3) 0.1076(3) 0.6473(4) 0.0787(15) Uani 1 1 d . . .
H47A H 0.5971 0.0920 0.6324 0.094 Uiso 1 1 calc R . .
C33 C 0.1269(3) -0.10530(17) 0.6667(3) 0.0522(9) Uani 1 1 d . . .
C37 C -0.0371(3) -0.1096(3) 0.6443(4) 0.0848(16) Uani 1 1 d . . .
H37A H -0.0932 -0.0922 0.6327 0.102 Uiso 1 1 calc R . .
C23 C 0.3578(3) 0.03835(15) 0.1340(3) 0.0515(9) Uani 1 1 d . . .
C46 C 0.4612(3) 0.0767(2) 0.6472(3) 0.0665(12) Uani 1 1 d . . .
H46A H 0.4643 0.0405 0.6287 0.080 Uiso 1 1 calc R . .
C44 C 0.1017(3) 0.09346(17) 0.6360(4) 0.0594(10) Uani 1 1 d . . .
H44A H 0.1045 0.0740 0.5722 0.071 Uiso 1 1 calc R . .
C40 C 0.1716(4) 0.1241(2) 0.8026(4) 0.0835(16) Uani 1 1 d . . .
H40A H 0.2211 0.1255 0.8513 0.100 Uiso 1 1 calc R . .
C34 C 0.1287(3) -0.16060(19) 0.6763(4) 0.0764(14) Uani 1 1 d . . .
H34A H 0.1847 -0.1784 0.6850 0.092 Uiso 1 1 calc R . .
C42 C 0.0172(4) 0.1495(2) 0.7529(5) 0.0830(15) Uani 1 1 d . . .
H42A H -0.0368 0.1679 0.7685 0.100 Uiso 1 1 calc R . .
C27 C 0.3294(3) -0.10497(17) 0.6981(3) 0.0551(10) Uani 1 1 d . . .
C30 C 0.4919(4) -0.1600(2) 0.7448(5) 0.0827(15) Uani 1 1 d . . .
H30A H 0.5466 -0.1781 0.7609 0.099 Uiso 1 1 calc R . .
C26 C 0.2946(3) 0.01569(17) 0.8036(3) 0.0648(12) Uani 1 1 d . . .
H26A H 0.3555 -0.0004 0.8070 0.078 Uiso 1 1 calc R . .
H26B H 0.2878 0.0391 0.8654 0.078 Uiso 1 1 calc R . .
C29 C 0.4870(3) -0.12690(19) 0.6568(4) 0.0719(13) Uani 1 1 d . . .
H29A H 0.5378 -0.1225 0.6133 0.086 Uiso 1 1 calc R . .
C24 C 0.4067(3) -0.01406(18) 0.1222(4) 0.0715(13) Uani 1 1 d . . .
H24A H 0.3893 -0.0379 0.1791 0.107 Uiso 1 1 calc R . .
H24B H 0.4721 -0.0082 0.1260 0.107 Uiso 1 1 calc R . .
H24C H 0.3902 -0.0299 0.0540 0.107 Uiso 1 1 calc R . .
C39 C 0.1784(3) 0.09438(16) 0.7071(3) 0.0536(10) Uani 1 1 d . . .
C9 C 0.2468(6) -0.2872(2) -0.0395(6) 0.115(3) Uani 1 1 d . . .
H9A H 0.2587 -0.3210 -0.0684 0.138 Uiso 1 1 calc R . .
C41 C 0.0905(4) 0.1515(3) 0.8239(5) 0.0967(18) Uani 1 1 d . . .
H41A H 0.0861 0.1713 0.8871 0.116 Uiso 1 1 calc R . .
C31 C 0.4174(4) -0.1669(2) 0.8097(4) 0.0902(17) Uani 1 1 d . . .
H31A H 0.4212 -0.1903 0.8681 0.108 Uiso 1 1 calc R . .
C7 C 0.2899(4) -0.21437(19) 0.0755(4) 0.0832(15) Uani 1 1 d . . .
H7A H 0.3318 -0.1996 0.1247 0.100 Uiso 1 1 calc R . .
C38 C 0.0431(3) -0.0804(2) 0.6478(4) 0.0705(13) Uani 1 1 d . . .
H38A H 0.0411 -0.0434 0.6372 0.085 Uiso 1 1 calc R . .
C43 C 0.0225(3) 0.1210(2) 0.6597(5) 0.0768(14) Uani 1 1 d . . .
H43A H -0.0276 0.1201 0.6119 0.092 Uiso 1 1 calc R . .
C11 C 0.1493(4) -0.2089(2) -0.0272(4) 0.0881(17) Uani 1 1 d . . .
H11A H 0.0961 -0.1905 -0.0483 0.106 Uiso 1 1 calc R . .
C10 C 0.1676(6) -0.2600(3) -0.0692(5) 0.113(2) Uani 1 1 d . . .
H10A H 0.1260 -0.2756 -0.1177 0.136 Uiso 1 1 calc R . .
C21 C 0.3257(6) 0.2632(2) -0.0483(5) 0.111(2) Uani 1 1 d . . .
H21A H 0.3661 0.2791 -0.0959 0.133 Uiso 1 1 calc R . .
C36 C -0.0351(4) -0.1641(3) 0.6579(5) 0.0932(19) Uani 1 1 d . . .
H36A H -0.0897 -0.1836 0.6569 0.112 Uiso 1 1 calc R . .
C20 C 0.2497(6) 0.2910(2) -0.0162(6) 0.107(2) Uani 1 1 d . . .
H20A H 0.2383 0.3256 -0.0418 0.129 Uiso 1 1 calc R . .
C32 C 0.3365(4) -0.1391(2) 0.7878(4) 0.0802(15) Uani 1 1 d . . .
H32A H 0.2866 -0.1431 0.8328 0.096 Uiso 1 1 calc R . .
C48 C 0.5349(4) 0.1610(3) 0.6693(5) 0.0926(18) Uani 1 1 d . . .
H48A H 0.5877 0.1821 0.6668 0.111 Uiso 1 1 calc R . .
C50 C 0.3737(4) 0.15290(19) 0.6963(5) 0.0789(15) Uani 1 1 d . . .
H50A H 0.3177 0.1688 0.7123 0.095 Uiso 1 1 calc R . .
C13 C 0.0852(4) 0.01353(19) 0.1252(4) 0.0784(14) Uani 1 1 d . . .
H13A H 0.1043 0.0360 0.1844 0.118 Uiso 1 1 calc R . .
H13B H 0.0202 0.0067 0.1291 0.118 Uiso 1 1 calc R . .
H13C H 0.0980 0.0313 0.0587 0.118 Uiso 1 1 calc R . .
C22 C 0.3437(4) 0.2109(2) -0.0108(4) 0.0908(17) Uani 1 1 d . . .
H22A H 0.3948 0.1921 -0.0344 0.109 Uiso 1 1 calc R . .
C19 C 0.1912(5) 0.2676(2) 0.0532(5) 0.106(2) Uani 1 1 d . . .
H19A H 0.1389 0.2863 0.0740 0.127 Uiso 1 1 calc R . .
C35 C 0.0472(4) -0.1897(2) 0.6729(5) 0.0938(18) Uani 1 1 d . . .
H35A H 0.0487 -0.2268 0.6810 0.113 Uiso 1 1 calc R . .
C18 C 0.2075(4) 0.21676(19) 0.0939(5) 0.0843(16) Uani 1 1 d . . .
H18A H 0.1671 0.2018 0.1426 0.101 Uiso 1 1 calc R . .
C8 C 0.3075(5) -0.2648(2) 0.0323(5) 0.104(2) Uani 1 1 d . . .
H8A H 0.3608 -0.2832 0.0525 0.125 Uiso 1 1 calc R . .
C49 C 0.4543(4) 0.1837(2) 0.6948(6) 0.0996(19) Uani 1 1 d . . .
H49A H 0.4521 0.2201 0.7115 0.120 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.1443(11) . ?
Ni1 S1 2.1445(12) . ?
Ni1 P2 2.1721(12) . ?
Ni1 P1 2.1744(12) . ?
S1 C1 1.765(3) . ?
S4 C23 1.736(4) . ?
S4 C16 1.739(4) . ?
P2 C39 1.810(4) . ?
P2 C45 1.821(4) . ?
P2 C26 1.840(4) . ?
S2 C2 1.774(4) . ?
P1 C27 1.815(4) . ?
P1 C33 1.820(4) . ?
P1 C25 1.836(4) . ?
S3 C12 1.726(4) . ?
S3 C5 1.731(4) . ?
C17 C18 1.389(7) . ?
C17 C22 1.391(7) . ?
C17 C16 1.470(5) . ?
C2 C1 1.336(5) . ?
C2 C14 1.482(5) . ?
C1 C3 1.497(5) . ?
C14 C23 1.366(5) . ?
C14 C15 1.433(5) . ?
C15 C16 1.362(5) . ?
C6 C7 1.378(7) . ?
C6 C11 1.402(7) . ?
C6 C5 1.480(5) . ?
C45 C46 1.368(6) . ?
C45 C50 1.383(6) . ?
C4 C5 1.361(5) . ?
C4 C3 1.421(5) . ?
C3 C12 1.374(5) . ?
C25 C26 1.517(6) . ?
C12 C13 1.501(6) . ?
C28 C27 1.376(5) . ?
C28 C29 1.396(6) . ?
C47 C48 1.358(8) . ?
C47 C46 1.385(7) . ?
C33 C38 1.380(6) . ?
C33 C34 1.381(6) . ?
C37 C36 1.366(8) . ?
C37 C38 1.372(7) . ?
C23 C24 1.493(6) . ?
C44 C43 1.375(6) . ?
C44 C39 1.408(6) . ?
C40 C41 1.389(7) . ?
C40 C39 1.403(6) . ?
C34 C35 1.386(7) . ?
C42 C43 1.362(7) . ?
C42 C41 1.369(8) . ?
C27 C32 1.403(6) . ?
C30 C29 1.369(7) . ?
C30 C31 1.373(7) . ?
C9 C8 1.360(9) . ?
C9 C10 1.377(9) . ?
C31 C32 1.384(7) . ?
C7 C8 1.389(7) . ?
C11 C10 1.401(8) . ?
C21 C20 1.370(9) . ?
C21 C22 1.403(7) . ?
C36 C35 1.364(8) . ?
C20 C19 1.354(9) . ?
C48 C49 1.343(8) . ?
C50 C49 1.398(7) . ?
C19 C18 1.381(6) . ?

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
S2 Ni1 S1 91.48(5) . . ?
S2 Ni1 P2 91.60(5) . . ?
S1 Ni1 P2 171.14(5) . . ?
S2 Ni1 P1 170.91(5) . . ?
S1 Ni1 P1 91.14(5) . . ?
P2 Ni1 P1 87.10(5) . . ?
C1 S1 Ni1 104.73(12) . . ?
C23 S4 C16 93.15(19) . . ?
C39 P2 C45 108.06(19) . . ?
C39 P2 C26 101.8(2) . . ?
C45 P2 C26 104.6(2) . . ?
C39 P2 Ni1 112.47(13) . . ?
C45 P2 Ni1 120.31(14) . . ?
C26 P2 Ni1 107.69(14) . . ?
C2 S2 Ni1 105.03(12) . . ?
C27 P1 C33 108.87(19) . . ?
C27 P1 C25 101.1(2) . . ?
C33 P1 C25 104.44(19) . . ?
C27 P1 Ni1 112.20(13) . . ?
C33 P1 Ni1 120.09(13) . . ?
C25 P1 Ni1 108.12(15) . . ?
C12 S3 C5 93.18(18) . . ?
C18 C17 C22 118.8(5) . . ?
C18 C17 C16 120.8(4) . . ?
C22 C17 C16 120.4(5) . . ?
C1 C2 C14 127.1(3) . . ?
C1 C2 S2 118.7(3) . . ?
C14 C2 S2 114.2(2) . . ?
C2 C1 C3 126.4(3) . . ?
C2 C1 S1 120.1(3) . . ?
C3 C1 S1 113.5(2) . . ?
C23 C14 C15 112.0(3) . . ?
C23 C14 C2 124.8(3) . . ?
C15 C14 C2 123.1(3) . . ?
C16 C15 C14 115.1(4) . . ?
C7 C6 C11 118.3(5) . . ?
C7 C6 C5 121.1(4) . . ?
C11 C6 C5 120.6(5) . . ?
C46 C45 C50 118.8(4) . . ?
C46 C45 P2 118.0(3) . . ?
C50 C45 P2 123.2(3) . . ?
C5 C4 C3 114.4(4) . . ?
C12 C3 C4 112.7(3) . . ?
C12 C3 C1 124.2(3) . . ?
C4 C3 C1 123.1(3) . . ?
C26 C25 P1 106.7(3) . . ?
C4 C5 C6 128.5(4) . . ?
C4 C5 S3 109.6(3) . . ?
C6 C5 S3 121.9(3) . . ?
C3 C12 C13 129.7(4) . . ?
C3 C12 S3 110.2(3) . . ?
C13 C12 S3 120.0(3) . . ?
C27 C28 C29 121.3(4) . . ?
C15 C16 C17 129.2(4) . . ?
C15 C16 S4 109.0(3) . . ?
C17 C16 S4 121.9(3) . . ?
C48 C47 C46 119.2(5) . . ?
C38 C33 C34 118.4(4) . . ?
C38 C33 P1 117.5(3) . . ?
C34 C33 P1 124.0(3) . . ?
C36 C37 C38 120.3(5) . . ?
C14 C23 C24 129.9(4) . . ?
C14 C23 S4 110.7(3) . . ?
C24 C23 S4 119.3(3) . . ?
C45 C46 C47 121.1(5) . . ?
C43 C44 C39 120.8(4) . . ?
C41 C40 C39 119.7(5) . . ?
C33 C34 C35 120.2(5) . . ?
C43 C42 C41 120.6(5) . . ?
C28 C27 C32 118.3(4) . . ?
C28 C27 P1 119.5(3) . . ?
C32 C27 P1 121.9(3) . . ?
C29 C30 C31 121.1(5) . . ?
C25 C26 P2 106.6(3) . . ?
C30 C29 C28 119.1(5) . . ?
C40 C39 C44 118.0(4) . . ?
C40 C39 P2 122.3(3) . . ?
C44 C39 P2 119.6(3) . . ?
C8 C9 C10 119.9(6) . . ?
C42 C41 C40 120.7(5) . . ?
C30 C31 C32 119.8(5) . . ?
C6 C7 C8 121.5(6) . . ?
C37 C38 C33 120.9(5) . . ?
C42 C43 C44 120.3(5) . . ?
C10 C11 C6 119.4(6) . . ?
C9 C10 C11 120.7(6) . . ?
C20 C21 C22 121.2(6) . . ?
C35 C36 C37 119.8(5) . . ?
C19 C20 C21 119.2(6) . . ?
C31 C32 C27 120.4(5) . . ?
C49 C48 C47 121.0(5) . . ?
C45 C50 C49 119.3(5) . . ?
C17 C22 C21 119.1(6) . . ?
C20 C19 C18 121.4(7) . . ?
C36 C35 C34 120.4(5) . . ?
C19 C18 C17 120.3(6) . . ?
C9 C8 C7 120.1(7) . . ?
C48 C49 C50 120.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.103

####################################################################### 
# 
# 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_2o
_database_code_depnum_ccdc_archive 'CCDC 1504115'
_audit_update_record             
;
2016-09-13 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H42 Cl0 N0 O0 P2 Pd S4'
_chemical_formula_weight         939.42

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'
P P 0.1023 0.0942 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   25.348(6)
_cell_length_b                   12.843(2)
_cell_length_c                   14.647(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4768.4(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13767
_cell_measurement_theta_min      2.1090
_cell_measurement_theta_max      27.2249

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6045
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_process_details   
; 
RIGAKU/MSC(2004), CrystalClear Version 1.3.6, 
  Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23715
_diffrn_reflns_av_R_equivalents  0.1464
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3989
_reflns_number_gt                3815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+23.8268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3989
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.1684
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.0000 0.45230(4) 0.7500 0.0441(3) Uani 1 2 d S . .
S1 S 0.94122(6) 0.58181(11) 0.70589(12) 0.0490(4) Uani 1 1 d . . .
P1 P 0.93967(7) 0.31967(12) 0.72507(13) 0.0543(5) Uani 1 1 d . . .
S2 S 0.91189(7) 0.96317(12) 0.61993(14) 0.0602(5) Uani 1 1 d . . .
C1 C 0.9755(2) 0.7014(4) 0.7305(4) 0.0451(13) Uani 1 1 d . . .
C3 C 0.8912(2) 0.8154(5) 0.7330(5) 0.0537(15) Uani 1 1 d . . .
H3A H 0.8740 0.7722 0.7745 0.064 Uiso 1 1 calc R . .
C5 C 0.8137(3) 0.9456(5) 0.7135(6) 0.0652(19) Uani 1 1 d . . .
C4 C 0.8678(2) 0.9038(5) 0.6962(5) 0.0570(16) Uani 1 1 d . . .
C14 C 0.8960(3) 0.3254(5) 0.6239(5) 0.0562(16) Uani 1 1 d . . .
C20 C 0.8997(3) 0.2931(5) 0.8259(5) 0.0586(17) Uani 1 1 d . . .
C21 C 0.9011(2) 0.3600(5) 0.9014(5) 0.0570(16) Uani 1 1 d . . .
H21A H 0.9207 0.4212 0.8976 0.068 Uiso 1 1 calc R . .
C11 C 0.9618(2) 0.8695(4) 0.6394(5) 0.0510(15) Uani 1 1 d . . .
C2 C 0.9447(2) 0.7958(4) 0.7016(4) 0.0484(14) Uani 1 1 d . . .
C16 C 0.8897(4) 0.3554(6) 0.4603(6) 0.087(3) Uani 1 1 d . . .
H16A H 0.9058 0.3710 0.4049 0.104 Uiso 1 1 calc R . .
C12 C 1.0128(3) 0.8773(6) 0.5878(6) 0.074(2) Uani 1 1 d . . .
H12A H 1.0356 0.8213 0.6055 0.111 Uiso 1 1 calc R . .
H12B H 1.0295 0.9426 0.6013 0.111 Uiso 1 1 calc R . .
H12C H 1.0058 0.8730 0.5234 0.111 Uiso 1 1 calc R . .
C9 C 0.7389(5) 1.0566(9) 0.6698(11) 0.124(4) Uani 1 1 d . . .
H9A H 0.7238 1.1044 0.6298 0.149 Uiso 1 1 calc R . .
C22 C 0.8743(3) 0.3380(7) 0.9817(5) 0.076(2) Uani 1 1 d . . .
H22A H 0.8766 0.3835 1.0309 0.091 Uiso 1 1 calc R . .
C15 C 0.9196(3) 0.3519(6) 0.5398(5) 0.0696(19) Uani 1 1 d . . .
H15A H 0.9554 0.3672 0.5375 0.084 Uiso 1 1 calc R . .
C13 C 0.9784(3) 0.1957(5) 0.7130(6) 0.073(2) Uani 1 1 d . . .
H13A H 0.9554 0.1360 0.7208 0.087 Uiso 1 1 calc R . .
H13B H 0.9943 0.1919 0.6528 0.087 Uiso 1 1 calc R . .
C8 C 0.7112(4) 1.0241(10) 0.7467(12) 0.127(5) Uani 1 1 d . . .
H8A H 0.6770 1.0483 0.7564 0.152 Uiso 1 1 calc R . .
C24 C 0.8400(4) 0.1791(7) 0.9132(7) 0.107(3) Uani 1 1 d . . .
H24A H 0.8192 0.1196 0.9164 0.128 Uiso 1 1 calc R . .
C25 C 0.8675(4) 0.2013(7) 0.8341(6) 0.094(3) Uani 1 1 d . . .
H25A H 0.8651 0.1557 0.7849 0.113 Uiso 1 1 calc R . .
C19 C 0.8425(3) 0.3062(8) 0.6259(6) 0.092(3) Uani 1 1 d . . .
H19A H 0.8264 0.2889 0.6808 0.110 Uiso 1 1 calc R . .
C23 C 0.8433(4) 0.2461(8) 0.9890(6) 0.089(3) Uani 1 1 d . . .
H23A H 0.8256 0.2306 1.0428 0.107 Uiso 1 1 calc R . .
C17 C 0.8358(5) 0.3356(7) 0.4636(8) 0.100(3) Uani 1 1 d . . .
H17A H 0.8157 0.3382 0.4106 0.120 Uiso 1 1 calc R . .
C10 C 0.7900(3) 1.0168(7) 0.6525(8) 0.101(3) Uani 1 1 d . . .
H10A H 0.8082 1.0378 0.6005 0.121 Uiso 1 1 calc R . .
C6 C 0.7850(3) 0.9179(7) 0.7893(8) 0.090(3) Uani 1 1 d . . .
H6A H 0.7998 0.8712 0.8305 0.108 Uiso 1 1 calc R . .
C7 C 0.7332(4) 0.9578(9) 0.8077(10) 0.118(4) Uani 1 1 d . . .
H7A H 0.7152 0.9386 0.8603 0.142 Uiso 1 1 calc R . .
C18 C 0.8124(4) 0.3122(10) 0.5466(9) 0.116(4) Uani 1 1 d . . .
H18A H 0.7762 0.3003 0.5493 0.139 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 P1 2.3181(16) . ?
Pd1 P1 2.3181(16) 3_756 ?
Pd1 S1 2.3247(15) 3_756 ?
Pd1 S1 2.3247(15) . ?
S1 C1 1.801(6) . ?
P1 C20 1.823(7) . ?
P1 C14 1.850(7) . ?
P1 C13 1.879(7) . ?
S2 C4 1.754(8) . ?
S2 C11 1.769(6) . ?
C1 C1 1.366(11) 3_756 ?
C1 C2 1.503(8) . ?
C3 C4 1.390(8) . ?
C3 C2 1.455(8) . ?
C5 C6 1.373(12) . ?
C5 C10 1.413(11) . ?
C5 C4 1.496(9) . ?
C14 C19 1.379(10) . ?
C14 C15 1.411(10) . ?
C20 C21 1.401(9) . ?
C20 C25 1.439(9) . ?
C21 C22 1.387(10) . ?
C11 C2 1.383(8) . ?
C11 C12 1.500(9) . ?
C16 C15 1.389(11) . ?
C16 C17 1.390(13) . ?
C9 C8 1.391(17) . ?
C9 C10 1.416(14) . ?
C22 C23 1.422(12) . ?
C13 C13 1.540(14) 3_756 ?
C8 C7 1.355(17) . ?
C24 C25 1.381(13) . ?
C24 C23 1.407(13) . ?
C19 C18 1.392(13) . ?
C17 C18 1.386(15) . ?
C6 C7 1.433(12) . ?

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
P1 Pd1 P1 85.42(9) . 3_756 ?
P1 Pd1 S1 172.93(6) . 3_756 ?
P1 Pd1 S1 93.39(6) 3_756 3_756 ?
P1 Pd1 S1 93.39(6) . . ?
P1 Pd1 S1 172.93(6) 3_756 . ?
S1 Pd1 S1 88.63(7) 3_756 . ?
C1 S1 Pd1 104.18(18) . . ?
C20 P1 C14 108.9(3) . . ?
C20 P1 C13 102.0(3) . . ?
C14 P1 C13 105.7(3) . . ?
C20 P1 Pd1 112.1(2) . . ?
C14 P1 Pd1 119.4(2) . . ?
C13 P1 Pd1 107.0(2) . . ?
C4 S2 C11 93.3(3) . . ?
C1 C1 C2 126.1(3) 3_756 . ?
C1 C1 S1 121.47(18) 3_756 . ?
C2 C1 S1 112.4(4) . . ?
C4 C3 C2 114.6(6) . . ?
C6 C5 C10 117.0(8) . . ?
C6 C5 C4 122.1(7) . . ?
C10 C5 C4 120.9(8) . . ?
C3 C4 C5 128.2(7) . . ?
C3 C4 S2 109.3(5) . . ?
C5 C4 S2 122.5(5) . . ?
C19 C14 C15 118.5(7) . . ?
C19 C14 P1 124.4(6) . . ?
C15 C14 P1 117.2(5) . . ?
C21 C20 C25 116.8(7) . . ?
C21 C20 P1 120.7(5) . . ?
C25 C20 P1 122.4(6) . . ?
C22 C21 C20 122.1(7) . . ?
C2 C11 C12 130.3(6) . . ?
C2 C11 S2 110.3(4) . . ?
C12 C11 S2 119.3(5) . . ?
C11 C2 C3 112.5(5) . . ?
C11 C2 C1 125.1(6) . . ?
C3 C2 C1 122.3(5) . . ?
C15 C16 C17 120.0(9) . . ?
C8 C9 C10 119.9(11) . . ?
C21 C22 C23 120.2(7) . . ?
C16 C15 C14 120.6(8) . . ?
C13 C13 P1 107.8(4) 3_756 . ?
C7 C8 C9 120.9(10) . . ?
C25 C24 C23 120.4(8) . . ?
C24 C25 C20 121.6(8) . . ?
C14 C19 C18 120.8(9) . . ?
C24 C23 C22 118.8(8) . . ?
C18 C17 C16 119.4(9) . . ?
C5 C10 C9 120.6(11) . . ?
C5 C6 C7 123.0(10) . . ?
C8 C7 C6 118.6(12) . . ?
C17 C18 C19 120.6(9) . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.140

