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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex1
_audit_creation_date             09-03-16
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '3051723 ben0905'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-03-03- Report on C36 H28 P2 Pt S2 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-03-03- passes checkcif tests with minor warnings  
;

_cell_length_a                   9.6154(1)
_cell_length_b                   19.0693(2)
_cell_length_c                   17.4036(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.0430(6)
_cell_angle_gamma                90
_cell_volume                     3151.44(6)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103
11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C36 H28 P2 Pt1 S2 
# Dc =      1.65 Fooo =   1536.00 Mu =     47.11 M =    781.79
# Found Formula = C36 H28 P2 Pt1 S2 
# Dc =      1.65 FOOO =   1536.00 Mu =     47.11 M =    781.79

_chemical_formula_sum            'C36 H28 P2 Pt S2'
_chemical_formula_moiety         'C36 H28 P2 Pt S2'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         781.79


_cell_measurement_reflns_used    69310
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.09
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_max          0.36

_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    4.711

# Sheldrick geometric approximatio 0.49 0.65 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.160
-1 0 0 0.200
0 1 0 0.020
0 -1 0 0.070
0 0 1 0.080
0 0 -1 0.070
2 0 2 0.128
-1 0 -1 0.185
-1 0 1 0.190
0 3 -2 0.028


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.5 deg at rate 45 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 95 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            86124
_reflns_number_total             9227
_diffrn_reflns_av_R_equivalents  0.052
# Number of reflections with Friedels Law is 9227 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 9219 


_diffrn_reflns_theta_min         2.600
_diffrn_reflns_theta_max         30.032
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.032
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              26
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      23.66

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.49
_refine_diff_density_max         1.71


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9225
_refine_ls_number_restraints     0
_refine_ls_number_parameters     370
_oxford_refine_ls_R_factor_ref   0.0374
_refine_ls_wR_factor_ref         0.1335
_refine_ls_goodness_of_fit_ref   0.7760
_refine_ls_shift/su_max          0.001796


# The values computed from all data 
_oxford_reflns_number_all        9225
_refine_ls_R_factor_all          0.0374
_refine_ls_wR_factor_all         0.1335

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6853
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_gt          0.0790

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 56.3 88.2 44.8 11.7 
;
_refine_special_details          
;
Hydrogen atoms were included at idealized positions
and ride on the atoms to which they are attached.

;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pt1 Pt 0.318538(14) 0.424922(7) 0.743826(7) 0.0258 1.0000 Uani . . . . . . .
S1 S 0.49741(13) 0.47881(6) 0.68077(7) 0.0373 1.0000 Uani . . . . . . .
S2 S 0.19917(13) 0.53594(5) 0.73481(6) 0.0352 1.0000 Uani . . . . . . .
P1 P 0.52344(11) 0.38831(6) 0.62643(6) 0.0306 1.0000 Uani . . . . . . .
P2 P 0.12951(11) 0.51833(5) 0.83542(6) 0.0290 1.0000 Uani . . . . . . .
C1 C 0.5196(4) 0.3203(2) 0.6976(2) 0.0298 1.0000 Uani . . . . . . .
C2 C 0.4294(4) 0.3356(2) 0.7522(2) 0.0280 1.0000 Uani . . . . . . .
C3 C 0.4339(5) 0.2854(2) 0.8121(2) 0.0343 1.0000 Uani . . . . . . .
C4 C 0.5215(5) 0.2270(2) 0.8165(3) 0.0381 1.0000 Uani . . . . . . .
C5 C 0.6063(6) 0.2143(3) 0.7610(3) 0.0436 1.0000 Uani . . . . . . .
C6 C 0.6066(5) 0.2617(2) 0.6999(3) 0.0372 1.0000 Uani . . . . . . .
C11 C 0.3890(4) 0.3730(2) 0.5441(2) 0.0315 1.0000 Uani . . . . . . .
C12 C 0.3345(6) 0.4286(3) 0.4976(4) 0.0479 1.0000 Uani . . . . . . .
C13 C 0.2430(8) 0.4173(3) 0.4296(4) 0.0564 1.0000 Uani . . . . . . .
C14 C 0.1993(5) 0.3500(3) 0.4081(3) 0.0476 1.0000 Uani . . . . . . .
C15 C 0.2498(5) 0.2941(3) 0.4546(3) 0.0424 1.0000 Uani . . . . . . .
C16 C 0.3438(5) 0.3055(3) 0.5219(3) 0.0411 1.0000 Uani . . . . . . .
C21 C 0.6871(4) 0.3855(3) 0.5880(3) 0.0366 1.0000 Uani . . . . . . .
C22 C 0.8131(5) 0.3948(3) 0.6389(3) 0.0420 1.0000 Uani . . . . . . .
C23 C 0.9391(5) 0.3967(4) 0.6106(4) 0.0545 1.0000 Uani . . . . . . .
C24 C 0.9418(6) 0.3898(6) 0.5331(5) 0.0830 1.0000 Uani . . . . . . .
C25 C 0.8182(8) 0.3829(7) 0.4807(4) 0.0886 1.0000 Uani . . . . . . .
C26 C 0.6897(6) 0.3803(5) 0.5086(3) 0.0630 1.0000 Uani . . . . . . .
C31 C 0.0790(5) 0.4282(2) 0.8337(3) 0.0311 1.0000 Uani . . . . . . .
C32 C 0.1590(4) 0.3843(2) 0.7919(2) 0.0284 1.0000 Uani . . . . . . .
C33 C 0.1085(5) 0.3151(2) 0.7820(3) 0.0367 1.0000 Uani . . . . . . .
C34 C -0.0106(5) 0.2918(3) 0.8098(3) 0.0416 1.0000 Uani . . . . . . .
C35 C -0.0836(5) 0.3370(3) 0.8537(3) 0.0434 1.0000 Uani . . . . . . .
C36 C -0.0379(5) 0.4052(3) 0.8661(3) 0.0404 1.0000 Uani . . . . . . .
C41 C 0.2561(5) 0.5379(2) 0.9204(2) 0.0339 1.0000 Uani . . . . . . .
C42 C 0.3528(7) 0.5910(3) 0.9184(4) 0.0557 1.0000 Uani . . . . . . .
C43 C 0.4399(8) 0.6099(4) 0.9875(4) 0.0689 1.0000 Uani . . . . . . .
C44 C 0.4345(7) 0.5747(3) 1.0556(4) 0.0554 1.0000 Uani . . . . . . .
C45 C 0.3425(6) 0.5202(4) 1.0567(3) 0.0547 1.0000 Uani . . . . . . .
C46 C 0.2510(5) 0.5018(3) 0.9895(3) 0.0453 1.0000 Uani . . . . . . .
C51 C -0.0197(5) 0.57424(19) 0.8431(3) 0.0312 1.0000 Uani . . . . . . .
C52 C -0.1420(6) 0.5650(3) 0.7889(3) 0.0411 1.0000 Uani . . . . . . .
C53 C -0.2559(5) 0.6099(3) 0.7886(3) 0.0467 1.0000 Uani . . . . . . .
C54 C -0.2465(6) 0.6652(3) 0.8406(3) 0.0479 1.0000 Uani . . . . . . .
C55 C -0.1250(7) 0.6745(4) 0.8944(4) 0.0624 1.0000 Uani . . . . . . .
C56 C -0.0138(6) 0.6279(3) 0.8968(3) 0.0485 1.0000 Uani . . . . . . .
H31 H 0.3721 0.2921 0.8527 0.0413 1.0000 Uiso R . . . . . .
H41 H 0.5231 0.1935 0.8609 0.0447 1.0000 Uiso R . . . . . .
H51 H 0.6670 0.1715 0.7645 0.0519 1.0000 Uiso R . . . . . .
H61 H 0.6673 0.2538 0.6591 0.0452 1.0000 Uiso R . . . . . .
H121 H 0.3621 0.4777 0.5136 0.0565 1.0000 Uiso R . . . . . .
H131 H 0.2079 0.4578 0.3956 0.0659 1.0000 Uiso R . . . . . .
H141 H 0.1315 0.3420 0.3592 0.0571 1.0000 Uiso R . . . . . .
H151 H 0.2183 0.2453 0.4395 0.0512 1.0000 Uiso R . . . . . .
H161 H 0.3801 0.2647 0.5553 0.0488 1.0000 Uiso R . . . . . .
H221 H 0.8120 0.4000 0.6960 0.0503 1.0000 Uiso R . . . . . .
H231 H 1.0292 0.4032 0.6473 0.0652 1.0000 Uiso R . . . . . .
H241 H 1.0343 0.3896 0.5137 0.1016 1.0000 Uiso R . . . . . .
H251 H 0.8209 0.3798 0.4236 0.1081 1.0000 Uiso R . . . . . .
H261 H 0.5998 0.3748 0.4715 0.0767 1.0000 Uiso R . . . . . .
H331 H 0.1611 0.2811 0.7535 0.0438 1.0000 Uiso R . . . . . .
H341 H -0.0449 0.2428 0.7987 0.0497 1.0000 Uiso R . . . . . .
H351 H -0.1675 0.3198 0.8756 0.0534 1.0000 Uiso R . . . . . .
H361 H -0.0874 0.4379 0.8977 0.0496 1.0000 Uiso R . . . . . .
H421 H 0.3606 0.6157 0.8686 0.0645 1.0000 Uiso R . . . . . .
H431 H 0.5073 0.6497 0.9871 0.0787 1.0000 Uiso R . . . . . .
H441 H 0.4977 0.5888 1.1044 0.0644 1.0000 Uiso R . . . . . .
H451 H 0.3408 0.4935 1.1060 0.0660 1.0000 Uiso R . . . . . .
H461 H 0.1819 0.4628 0.9909 0.0546 1.0000 Uiso R . . . . . .
H521 H -0.1476 0.5258 0.7503 0.0479 1.0000 Uiso R . . . . . .
H531 H -0.3444 0.6023 0.7509 0.0548 1.0000 Uiso R . . . . . .
H541 H -0.3272 0.6985 0.8394 0.0570 1.0000 Uiso R . . . . . .
H551 H -0.1178 0.7149 0.9314 0.0734 1.0000 Uiso R . . . . . .
H561 H 0.0711 0.6331 0.9376 0.0569 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.21117(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 . S1 . 2.4107(10) yes
Pt1 . S2 . 2.4014(10) yes
Pt1 . C2 . 2.003(4) yes
Pt1 . C32 . 2.014(4) yes
S1 . P1 . 2.0025(15) yes
S2 . P2 . 1.9990(15) yes
P1 . C1 . 1.797(4) yes
P1 . C11 . 1.797(4) yes
P1 . C21 . 1.805(4) yes
P2 . C31 . 1.785(4) yes
P2 . C41 . 1.800(4) yes
P2 . C51 . 1.809(4) yes
C1 . C2 . 1.415(5) yes
C1 . C6 . 1.393(6) yes
C2 . C3 . 1.409(6) yes
C3 . C4 . 1.392(6) yes
C3 . H31 . 1.000 no
C4 . C5 . 1.380(7) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.394(7) yes
C5 . H51 . 1.000 no
C6 . H61 . 1.000 no
C11 . C12 . 1.387(7) yes
C11 . C16 . 1.394(6) yes
C12 . C13 . 1.376(8) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.382(9) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.380(8) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.380(7) yes
C15 . H151 . 1.000 no
C16 . H161 . 1.000 no
C21 . C22 . 1.395(6) yes
C21 . C26 . 1.389(7) yes
C22 . C23 . 1.379(7) yes
C22 . H221 . 1.000 no
C23 . C24 . 1.359(10) yes
C23 . H231 . 1.000 no
C24 . C25 . 1.386(10) yes
C24 . H241 . 1.000 no
C25 . C26 . 1.397(8) yes
C25 . H251 . 1.000 no
C26 . H261 . 1.000 no
C31 . C32 . 1.413(6) yes
C31 . C36 . 1.405(6) yes
C32 . C33 . 1.407(6) yes
C33 . C34 . 1.384(7) yes
C33 . H331 . 1.000 no
C34 . C35 . 1.410(7) yes
C34 . H341 . 1.000 no
C35 . C36 . 1.379(7) yes
C35 . H351 . 1.000 no
C36 . H361 . 1.000 no
C41 . C42 . 1.380(7) yes
C41 . C46 . 1.393(7) yes
C42 . C43 . 1.399(8) yes
C42 . H421 . 1.000 no
C43 . C44 . 1.371(10) yes
C43 . H431 . 1.000 no
C44 . C45 . 1.366(10) yes
C44 . H441 . 1.000 no
C45 . C46 . 1.394(7) yes
C45 . H451 . 1.000 no
C46 . H461 . 1.000 no
C51 . C52 . 1.398(6) yes
C51 . C56 . 1.380(6) yes
C52 . C53 . 1.390(7) yes
C52 . H521 . 1.000 no
C53 . C54 . 1.383(8) yes
C53 . H531 . 1.000 no
C54 . C55 . 1.389(8) yes
C54 . H541 . 1.000 no
C55 . C56 . 1.387(7) yes
C55 . H551 . 1.000 no
C56 . H561 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 . Pt1 . S2 . 87.84(4) yes
S1 . Pt1 . C2 . 89.22(11) yes
S2 . Pt1 . C2 . 176.46(11) yes
S1 . Pt1 . C32 . 175.94(12) yes
S2 . Pt1 . C32 . 88.79(12) yes
C2 . Pt1 . C32 . 94.22(16) yes
Pt1 . S1 . P1 . 89.93(5) yes
Pt1 . S2 . P2 . 90.99(5) yes
S1 . P1 . C1 . 106.19(14) yes
S1 . P1 . C11 . 112.90(15) yes
C1 . P1 . C11 . 110.00(19) yes
S1 . P1 . C21 . 112.44(17) yes
C1 . P1 . C21 . 110.3(2) yes
C11 . P1 . C21 . 105.05(19) yes
S2 . P2 . C31 . 105.95(16) yes
S2 . P2 . C41 . 114.10(16) yes
C31 . P2 . C41 . 111.1(2) yes
S2 . P2 . C51 . 110.14(16) yes
C31 . P2 . C51 . 110.6(2) yes
C41 . P2 . C51 . 105.0(2) yes
P1 . C1 . C2 . 113.3(3) yes
P1 . C1 . C6 . 121.5(3) yes
C2 . C1 . C6 . 125.0(4) yes
C1 . C2 . Pt1 . 120.1(3) yes
C1 . C2 . C3 . 114.0(4) yes
Pt1 . C2 . C3 . 125.8(3) yes
C2 . C3 . C4 . 122.2(4) yes
C2 . C3 . H31 . 118.9 no
C4 . C3 . H31 . 118.9 no
C3 . C4 . C5 . 121.4(4) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 119.5(4) yes
C4 . C5 . H51 . 120.3 no
C6 . C5 . H51 . 120.3 no
C5 . C6 . C1 . 118.0(4) yes
C5 . C6 . H61 . 121.0 no
C1 . C6 . H61 . 121.0 no
P1 . C11 . C12 . 120.0(4) yes
P1 . C11 . C16 . 121.6(3) yes
C12 . C11 . C16 . 118.2(4) yes
C11 . C12 . C13 . 120.9(5) yes
C11 . C12 . H121 . 119.6 no
C13 . C12 . H121 . 119.6 no
C12 . C13 . C14 . 120.3(5) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 119.9 no
C13 . C14 . C15 . 119.6(5) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C16 . 120.0(5) yes
C14 . C15 . H151 . 120.0 no
C16 . C15 . H151 . 120.0 no
C11 . C16 . C15 . 120.9(5) yes
C11 . C16 . H161 . 119.5 no
C15 . C16 . H161 . 119.5 no
P1 . C21 . C22 . 118.8(3) yes
P1 . C21 . C26 . 121.6(4) yes
C22 . C21 . C26 . 119.5(4) yes
C21 . C22 . C23 . 120.0(5) yes
C21 . C22 . H221 . 120.0 no
C23 . C22 . H221 . 120.0 no
C22 . C23 . C24 . 120.5(5) yes
C22 . C23 . H231 . 119.7 no
C24 . C23 . H231 . 119.8 no
C23 . C24 . C25 . 120.9(5) yes
C23 . C24 . H241 . 119.6 no
C25 . C24 . H241 . 119.6 no
C24 . C25 . C26 . 119.3(6) yes
C24 . C25 . H251 . 120.4 no
C26 . C25 . H251 . 120.4 no
C25 . C26 . C21 . 119.8(5) yes
C25 . C26 . H261 . 120.1 no
C21 . C26 . H261 . 120.1 no
P2 . C31 . C32 . 114.2(3) yes
P2 . C31 . C36 . 121.8(4) yes
C32 . C31 . C36 . 123.8(4) yes
C31 . C32 . Pt1 . 119.8(3) yes
C31 . C32 . C33 . 114.4(4) yes
Pt1 . C32 . C33 . 125.5(3) yes
C32 . C33 . C34 . 123.2(4) yes
C32 . C33 . H331 . 118.4 no
C34 . C33 . H331 . 118.4 no
C33 . C34 . C35 . 120.1(5) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 119.9 no
C34 . C35 . C36 . 119.2(4) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 120.4 no
C31 . C36 . C35 . 119.1(4) yes
C31 . C36 . H361 . 120.4 no
C35 . C36 . H361 . 120.4 no
P2 . C41 . C42 . 120.2(4) yes
P2 . C41 . C46 . 119.8(4) yes
C42 . C41 . C46 . 119.9(5) yes
C41 . C42 . C43 . 118.8(6) yes
C41 . C42 . H421 . 120.6 no
C43 . C42 . H421 . 120.6 no
C42 . C43 . C44 . 121.2(6) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 119.4 no
C43 . C44 . C45 . 119.8(6) yes
C43 . C44 . H441 . 120.1 no
C45 . C44 . H441 . 120.1 no
C44 . C45 . C46 . 120.3(6) yes
C44 . C45 . H451 . 119.9 no
C46 . C45 . H451 . 119.9 no
C45 . C46 . C41 . 119.8(5) yes
C45 . C46 . H461 . 120.1 no
C41 . C46 . H461 . 120.1 no
P2 . C51 . C52 . 118.0(3) yes
P2 . C51 . C56 . 122.5(4) yes
C52 . C51 . C56 . 119.4(4) yes
C51 . C52 . C53 . 120.2(5) yes
C51 . C52 . H521 . 119.9 no
C53 . C52 . H521 . 119.9 no
C52 . C53 . C54 . 119.8(5) yes
C52 . C53 . H531 . 120.1 no
C54 . C53 . H531 . 120.1 no
C53 . C54 . C55 . 120.0(5) yes
C53 . C54 . H541 . 120.0 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 120.0(5) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 120.0 no
C55 . C56 . C51 . 120.4(5) yes
C55 . C56 . H561 . 119.8 no
C51 . C56 . H561 . 119.8 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
C23 C32 3.519(7) . 1_655 no
C23 C33 3.528(8) . 1_655 no
C42 C45 3.587(9) . 2_667 no
C43 C45 3.41(1) . 2_667 no
C44 C46 3.555(9) . 2_667 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pt1 S1 P1 C1 . . . . -42.0(1) no
Pt1 S1 P1 C11 . . . . 78.7(1) no
Pt1 S1 P1 C21 . . . . -162.7(2) no
Pt1 S2 P2 C31 . . . . -40.9(2) no
Pt1 S2 P2 C41 . . . . 81.7(1) no
Pt1 S2 P2 C51 . . . . -160.6(1) no
Pt1 C2 C1 P1 . . . . 1.3(4) no
Pt1 C2 C1 C6 . . . . 176.7(3) no
Pt1 C2 C3 C4 . . . . -175.4(3) no
Pt1 C32 C31 P2 . . . . 2.0(4) no
Pt1 C32 C31 C36 . . . . 177.0(4) no
Pt1 C32 C33 C34 . . . . -173.2(4) no
S1 Pt1 S2 P2 . . . . -146.40(5) no
S1 Pt1 C2 C1 . . . . -27.4(3) no
S1 Pt1 C2 C3 . . . . 148.6(3) no
S1 P1 C1 C2 . . . . 32.9(3) no
S1 P1 C1 C6 . . . . -142.7(3) no
S1 P1 C11 C12 . . . . 36.4(5) no
S1 P1 C11 C16 . . . . -148.2(3) no
S1 P1 C21 C22 . . . . 57.7(5) no
S1 P1 C21 C26 . . . . -116.8(6) no
S2 Pt1 S1 P1 . . . . -145.42(5) no
S2 Pt1 C32 C31 . . . . -27.2(3) no
S2 Pt1 C32 C33 . . . . 146.5(3) no
S2 P2 C31 C32 . . . . 31.4(3) no
S2 P2 C31 C36 . . . . -143.7(4) no
S2 P2 C41 C42 . . . . 31.7(5) no
S2 P2 C41 C46 . . . . -151.8(4) no
S2 P2 C51 C52 . . . . 63.6(4) no
S2 P2 C51 C56 . . . . -112.2(4) no
P1 S1 Pt1 C2 . . . . 36.5(1) no
P1 C1 C2 C3 . . . . -175.1(3) no
P1 C1 C6 C5 . . . . 174.5(3) no
P1 C11 C12 C13 . . . . 172.8(5) no
P1 C11 C16 C15 . . . . -174.1(4) no
P1 C21 C22 C23 . . . . -176.5(5) no
P1 C21 C26 C25 . . . . 175.8(8) no
P2 S2 Pt1 C32 . . . . 35.9(1) no
P2 C31 C32 C33 . . . . -172.4(3) no
P2 C31 C36 C35 . . . . 171.1(4) no
P2 C41 C42 C43 . . . . 173.3(5) no
P2 C41 C46 C45 . . . . -175.5(4) no
P2 C51 C52 C53 . . . . -175.2(4) no
P2 C51 C56 C55 . . . . 172.3(5) no
C1 P1 C11 C12 . . . . 154.8(4) no
C1 P1 C11 C16 . . . . -29.7(4) no
C1 P1 C21 C22 . . . . -60.6(5) no
C1 P1 C21 C26 . . . . 124.9(6) no
C1 C2 Pt1 C32 . . . . 150.5(3) no
C1 C2 C3 C4 . . . . 0.9(6) no
C1 C6 C5 C4 . . . . -0.3(7) no
C2 Pt1 C32 C31 . . . . 150.9(3) no
C2 Pt1 C32 C33 . . . . -35.4(3) no
C2 C1 P1 C11 . . . . -89.6(3) no
C2 C1 P1 C21 . . . . 155.0(3) no
C2 C1 C6 C5 . . . . -0.5(6) no
C2 C3 C4 C5 . . . . -1.7(7) no
C3 C2 Pt1 C32 . . . . -33.5(3) no
C3 C2 C1 C6 . . . . 0.2(5) no
C3 C4 C5 C6 . . . . 1.3(7) no
C6 C1 P1 C11 . . . . 94.9(4) no
C6 C1 P1 C21 . . . . -20.6(4) no
C11 P1 C21 C22 . . . . -179.1(4) no
C11 P1 C21 C26 . . . . 6.4(7) no
C11 C12 C13 C14 . . . . 3(1) no
C11 C16 C15 C14 . . . . 0.1(8) no
C12 C11 P1 C21 . . . . -86.4(5) no
C12 C11 C16 C15 . . . . 1.4(7) no
C12 C13 C14 C15 . . . . -1(1) no
C13 C12 C11 C16 . . . . -2.8(9) no
C13 C14 C15 C16 . . . . -0.3(9) no
C16 C11 P1 C21 . . . . 89.0(4) no
C21 C22 C23 C24 . . . . 0(1) no
C21 C26 C25 C24 . . . . 1(2) no
C22 C21 C26 C25 . . . . 1(1) no
C22 C23 C24 C25 . . . . 2(2) no
C23 C22 C21 C26 . . . . -2(1) no
C23 C24 C25 C26 . . . . -3(2) no
C31 P2 C41 C42 . . . . 151.5(4) no
C31 P2 C41 C46 . . . . -32.1(5) no
C31 P2 C51 C52 . . . . -53.2(5) no
C31 P2 C51 C56 . . . . 131.0(4) no
C31 C32 C33 C34 . . . . 0.8(6) no
C31 C36 C35 C34 . . . . 0.9(7) no
C32 C31 P2 C41 . . . . -93.1(4) no
C32 C31 P2 C51 . . . . 150.7(3) no
C32 C31 C36 C35 . . . . -3.5(7) no
C32 C33 C34 C35 . . . . -3.3(7) no
C33 C32 C31 C36 . . . . 2.6(6) no
C33 C34 C35 C36 . . . . 2.3(7) no
C36 C31 P2 C41 . . . . 91.8(4) no
C36 C31 P2 C51 . . . . -24.4(5) no
C41 P2 C51 C52 . . . . -173.2(4) no
C41 P2 C51 C56 . . . . 11.1(5) no
C41 C42 C43 C44 . . . . 3(1) no
C41 C46 C45 C44 . . . . 1.8(9) no
C42 C41 P2 C51 . . . . -89.0(5) no
C42 C41 C46 C45 . . . . 0.9(8) no
C42 C43 C44 C45 . . . . -0(1) no
C43 C42 C41 C46 . . . . -3.1(9) no
C43 C44 C45 C46 . . . . -2(1) no
C46 C41 P2 C51 . . . . 87.5(4) no
C51 C52 C53 C54 . . . . 2.0(8) no
C51 C56 C55 C54 . . . . 4(1) no
C52 C51 C56 C55 . . . . -3.5(8) no
C52 C53 C54 C55 . . . . -1.9(9) no
C53 C52 C51 C56 . . . . 0.7(8) no
C53 C54 C55 C56 . . . . -1(1) no
_database_code_depnum_ccdc_archive 'CCDC 999160'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex2
_audit_creation_date             09-03-03
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '2261648 ben0903'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-03-03- Report on C40 H36 Cl4 P2 Pt1 Se2 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-03-03- passes checkcif tests with minor warnings  
;


_cell_length_a                   16.0935(4)
_cell_length_b                   11.4059(2)
_cell_length_c                   22.5098(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.2742(10)
_cell_angle_gamma                90
_cell_volume                     3945.55(14)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103
11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C38 H32 Cl4 P2 Pt1 Se2 
# Dc =      1.76 Fooo =   2080.00 Mu =     57.80 M =    522.72
# Found Formula = C40 H36.00 Cl4 P2 Pt1 Se2 
# Dc =      1.81 FOOO =   2080.00 Mu =     57.82 M =    536.75

_chemical_formula_sum            'C40 H36 Cl4 P2 Pt1 Se2'
_chemical_formula_moiety         'C36 H28 P2 Pt Se2, 2(C2 H4 Cl2)'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         1073.49


_cell_measurement_reflns_used    68764
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.04
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_max          0.35

_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    5.782

# Sheldrick geometric approximatio 0.22 0.79 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.160
1 0 0 0.190
1 -1 0 0.091
1 3 0 0.090
0 1 0 0.100
0 -1 0 0.160
0 0 1 0.030
0 0 -1 0.010


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.074
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.1 deg at rate 33 sec/frame,
crystal-detector distance 35mm,
multiple scan sets so over 95 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            38436
_reflns_number_total             4539
_diffrn_reflns_av_R_equivalents  0.093
# Number of reflections with Friedels Law is 4539 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 4543 


_diffrn_reflns_theta_min         2.567
_diffrn_reflns_theta_max         27.524
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.5 # 27.524 
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       29
_reflns_limit_h_min              -20
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   3.29
_oxford_diffrn_Wilson_scale      124.56

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.24
_refine_diff_density_max         2.70


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4525
_refine_ls_number_restraints     72
_refine_ls_number_parameters     260
_oxford_refine_ls_R_factor_ref   0.0622
_refine_ls_wR_factor_ref         0.1167
_refine_ls_goodness_of_fit_ref   0.9215
_refine_ls_shift/su_max          0.038249


# The values computed from all data 
_oxford_reflns_number_all        4525
_refine_ls_R_factor_all          0.0622
_refine_ls_wR_factor_all         0.1167

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3488
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_gt          0.1118

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;

The crystal is twinned.
The utility DIRAX within COLLECT identified the twin components
to be related by a 180° rotation about
the direct axis 1 0 0.
This relationship was also recognized by ROTAX within CRYSTALS
and enabled the application of a twinning correction
during refinement of the structure.
Twin elements refined to 0.732(2):0.268(2). 


The 1,2-dichloroethane molecule is disordered 
and this has been modelled by assuming there are 
two overlapping images of the molecule.
Restraints were applied to bond distances and angles and
to displacement parameters.
The relative populations of each image were refined.

Hydrogen atoms were included at idealized positions
and ride on the atoms to which they are attached.

The largest peak in the final difference electron density map
is located at (0.000, 0.269, 0.250) and appears to be a "ghost image"
of the Pt atom, presumably arising from a stacking fault.
The computer program can handle twins and multiple scales
but, apparently, not both together. 
The magnitude of any stacking fault appears to be moderately low
so omission of a correction has little effect on the structure.
;



# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pt1 Pt 0.5000 0.25907(4) 0.2500 0.0387 1.0000 Uani S T . . . . .
Se1 Se 0.48054(6) 0.10113(6) 0.32201(4) 0.0480 1.0000 Uani . . . . . . .
Cl31 Cl 0.2905(7) 0.6201(14) 0.4232(6) 0.1284 0.535(9) Uani D U P . . . .
Cl32 Cl 0.2763(7) 0.8836(8) 0.3610(5) 0.1308 0.535(9) Uani D U P . . . .
Cl41 Cl 0.3190(6) 0.6192(17) 0.4529(8) 0.1276 0.465(9) Uani D U P . . . .
Cl42 Cl 0.2867(9) 0.8972(11) 0.4095(7) 0.1609 0.465(9) Uani D U P . . . .
P1 P 0.40566(14) 0.22420(17) 0.35811(9) 0.0451 1.0000 Uani . . . . . . .
C1 C 0.4601(5) 0.3625(6) 0.3612(4) 0.0457 1.0000 Uani . . . . . . .
C2 C 0.5001(4) 0.3819(6) 0.3152(3) 0.0375 1.0000 Uani . . . . . . .
C3 C 0.5467(5) 0.4873(7) 0.3207(4) 0.0529 1.0000 Uani . . . . . . .
C4 C 0.5531(6) 0.5665(7) 0.3679(4) 0.0595 1.0000 Uani . . . . . . .
C5 C 0.5104(7) 0.5467(8) 0.4117(4) 0.0654 1.0000 Uani . . . . . . .
C6 C 0.4640(7) 0.4416(8) 0.4097(4) 0.0619 1.0000 Uani . . . . . . .
C11 C 0.2947(5) 0.2370(7) 0.3099(4) 0.0475 1.0000 Uani . . . . . . .
C12 C 0.2537(6) 0.1458(8) 0.2704(4) 0.0587 1.0000 Uani . . . . . . .
C13 C 0.1654(7) 0.1582(10) 0.2362(5) 0.0748 1.0000 Uani . . . . . . .
C14 C 0.1255(8) 0.2585(9) 0.2424(5) 0.0725 1.0000 Uani . . . . . . .
C15 C 0.1609(6) 0.3477(10) 0.2800(5) 0.0718 1.0000 Uani . . . . . . .
C16 C 0.2473(6) 0.3391(8) 0.3140(5) 0.0618 1.0000 Uani . . . . . . .
C21 C 0.4006(6) 0.1848(7) 0.4346(4) 0.0560 1.0000 Uani . . . . . . .
C22 C 0.4783(8) 0.1706(9) 0.4824(4) 0.0679 1.0000 Uani . . . . . . .
C23 C 0.4775(10) 0.1356(10) 0.5412(5) 0.0927 1.0000 Uani . . . . . . .
C24 C 0.4006(10) 0.1188(10) 0.5533(6) 0.0924 1.0000 Uani . . . . . . .
C25 C 0.3257(11) 0.1329(12) 0.5083(7) 0.1076 1.0000 Uani . . . . . . .
C26 C 0.3259(7) 0.1663(11) 0.4475(5) 0.0813 1.0000 Uani . . . . . . .
C31 C 0.2049(14) 0.719(2) 0.4045(16) 0.1176 0.535(9) Uani D U P . . . .
C32 C 0.2317(19) 0.842(2) 0.4204(12) 0.1234 0.535(9) Uani D U P . . . .
C41 C 0.2215(14) 0.658(2) 0.4015(16) 0.1223 0.465(9) Uani D U P . . . .
C42 C 0.221(2) 0.778(2) 0.3718(14) 0.1304 0.465(9) Uani D U P . . . .
H31 H 0.5766 0.5058 0.2887 0.0609 1.0000 Uiso R . . . . . .
H41 H 0.5890 0.6390 0.3704 0.0677 1.0000 Uiso R . . . . . .
H51 H 0.5126 0.6064 0.4447 0.0754 1.0000 Uiso R . . . . . .
H61 H 0.4344 0.4237 0.4419 0.0740 1.0000 Uiso R . . . . . .
H121 H 0.2865 0.0732 0.2665 0.0715 1.0000 Uiso R . . . . . .
H131 H 0.1334 0.0942 0.2082 0.0907 1.0000 Uiso R . . . . . .
H141 H 0.0635 0.2677 0.2164 0.0875 1.0000 Uiso R . . . . . .
H151 H 0.1258 0.4183 0.2834 0.0879 1.0000 Uiso R . . . . . .
H161 H 0.2765 0.4052 0.3415 0.0745 1.0000 Uiso R . . . . . .
H221 H 0.5351 0.1859 0.4742 0.0810 1.0000 Uiso R . . . . . .
H231 H 0.5336 0.1228 0.5748 0.1082 1.0000 Uiso R . . . . . .
H241 H 0.4000 0.0957 0.5960 0.1149 1.0000 Uiso R . . . . . .
H251 H 0.2692 0.1198 0.5173 0.1410 1.0000 Uiso R . . . . . .
H261 H 0.2694 0.1763 0.4141 0.1010 1.0000 Uiso R . . . . . .
H311 H 0.1627 0.6965 0.4273 0.1395 0.535 Uiso R . . . . . .
H312 H 0.1757 0.7147 0.3587 0.1395 0.535 Uiso R . . . . . .
H321 H 0.2761 0.8466 0.4621 0.1453 0.535 Uiso R . . . . . .
H322 H 0.1805 0.8917 0.4200 0.1453 0.535 Uiso R . . . . . .
H411 H 0.1766 0.6587 0.4241 0.1433 0.465 Uiso R . . . . . .
H412 H 0.2057 0.5983 0.3676 0.1433 0.465 Uiso R . . . . . .
H421 H 0.1596 0.8068 0.3610 0.1505 0.465 Uiso R . . . . . .
H422 H 0.2370 0.7641 0.3327 0.1505 0.465 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.12619(6)

loop_
_oxford_twin_element_scale_factors
0.7320(15)
0.2680(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 . C2 5_655 2.028(7) yes
Pt1 . Se1 5_655 2.5045(8) yes
Pt1 . P1 5_655 3.253(2) yes
Pt1 . Se1 . 2.5045(8) yes
Pt1 . P1 . 3.253(2) yes
Pt1 . C2 . 2.028(7) yes
Se1 . P1 . 2.160(2) yes
Cl31 . C31 . 1.736(17) yes
Cl31 . C41 . 1.16(2) yes
Cl31 . H412 . 1.575 no
Cl32 . C32 . 1.761(17) yes
Cl32 . C42 . 1.56(3) yes
Cl32 . H422 . 1.557 no
Cl41 . C31 . 2.16(3) yes
Cl41 . C41 . 1.710(17) yes
Cl42 . C32 . 1.17(2) yes
Cl42 . C42 . 1.773(18) yes
Cl42 . H321 . 1.373 no
P1 . C1 . 1.796(8) yes
P1 . C11 . 1.799(8) yes
P1 . C21 . 1.805(8) yes
C1 . C2 . 1.390(10) yes
C1 . C6 . 1.404(11) yes
C2 . C3 . 1.403(10) yes
C3 . C4 . 1.375(12) yes
C3 . H31 . 1.000 no
C4 . C5 . 1.378(12) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.407(13) yes
C5 . H51 . 1.000 no
C6 . H61 . 1.000 no
C11 . C12 . 1.400(11) yes
C11 . C16 . 1.409(11) yes
C12 . C13 . 1.408(13) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.339(14) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.339(14) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.377(13) yes
C15 . H151 . 1.000 no
C16 . H161 . 1.000 no
C21 . C22 . 1.395(14) yes
C21 . C26 . 1.335(13) yes
C22 . C23 . 1.387(14) yes
C22 . H221 . 1.000 no
C23 . C24 . 1.358(17) yes
C23 . H231 . 1.000 no
C24 . C25 . 1.334(19) yes
C24 . H241 . 1.000 no
C25 . C26 . 1.420(15) yes
C25 . H251 . 1.000 no
C26 . H261 . 1.000 no
C31 . C32 . 1.473(18) yes
C31 . H311 . 1.000 no
C31 . H312 . 1.000 no
C32 . H321 . 1.000 no
C32 . H322 . 1.000 no
C41 . C42 . 1.522(18) yes
C41 . H411 . 1.000 no
C41 . H412 . 1.000 no
C42 . H421 . 1.000 no
C42 . H422 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 5_655 Pt1 . Se1 5_655 90.1(2) yes
C2 5_655 Pt1 . P1 5_655 56.2(2) yes
Se1 5_655 Pt1 . P1 5_655 41.58(4) yes
C2 5_655 Pt1 . Se1 . 172.57(19) yes
Se1 5_655 Pt1 . Se1 . 88.01(4) yes
P1 5_655 Pt1 . Se1 . 124.90(4) yes
C2 5_655 Pt1 . P1 . 136.5(2) yes
Se1 5_655 Pt1 . P1 . 124.90(4) yes
P1 5_655 Pt1 . P1 . 165.95(7) yes
Se1 . Pt1 . P1 . 41.58(4) yes
C2 5_655 Pt1 . C2 . 92.6(4) yes
Se1 5_655 Pt1 . C2 . 172.57(19) yes
P1 5_655 Pt1 . C2 . 136.5(2) yes
Se1 . Pt1 . C2 . 90.1(2) yes
P1 . Pt1 . C2 . 56.2(2) yes
Pt1 . Se1 . P1 . 88.11(6) yes
Se1 . P1 . Pt1 . 50.31(5) yes
Se1 . P1 . C1 . 105.4(3) yes
Pt1 . P1 . C1 . 65.8(2) yes
Se1 . P1 . C11 . 113.0(3) yes
Pt1 . P1 . C11 . 98.0(2) yes
C1 . P1 . C11 . 109.7(4) yes
Se1 . P1 . C21 . 112.7(3) yes
Pt1 . P1 . C21 . 155.2(3) yes
C1 . P1 . C21 . 110.0(4) yes
C11 . P1 . C21 . 106.1(4) yes
P1 . C1 . C2 . 116.1(6) yes
P1 . C1 . C6 . 120.2(6) yes
C2 . C1 . C6 . 123.7(8) yes
C1 . C2 . Pt1 . 121.8(5) yes
C1 . C2 . C3 . 115.1(7) yes
Pt1 . C2 . C3 . 122.8(6) yes
C2 . C3 . C4 . 123.2(8) yes
C2 . C3 . H31 . 118.4 no
C4 . C3 . H31 . 118.4 no
C3 . C4 . C5 . 120.4(8) yes
C3 . C4 . H41 . 119.8 no
C5 . C4 . H41 . 119.8 no
C4 . C5 . C6 . 119.3(8) yes
C4 . C5 . H51 . 120.3 no
C6 . C5 . H51 . 120.3 no
C5 . C6 . C1 . 118.2(8) yes
C5 . C6 . H61 . 120.9 no
C1 . C6 . H61 . 120.9 no
P1 . C11 . C12 . 121.3(6) yes
P1 . C11 . C16 . 119.1(7) yes
C12 . C11 . C16 . 119.5(8) yes
C11 . C12 . C13 . 118.8(9) yes
C11 . C12 . H121 . 120.6 no
C13 . C12 . H121 . 120.6 no
C12 . C13 . C14 . 117.8(10) yes
C12 . C13 . H131 . 121.1 no
C14 . C13 . H131 . 121.1 no
C13 . C14 . C15 . 126.0(11) yes
C13 . C14 . H141 . 117.0 no
C15 . C14 . H141 . 117.0 no
C14 . C15 . C16 . 117.9(10) yes
C14 . C15 . H151 . 121.1 no
C16 . C15 . H151 . 121.1 no
C11 . C16 . C15 . 120.0(9) yes
C11 . C16 . H161 . 120.0 no
C15 . C16 . H161 . 120.0 no
P1 . C21 . C22 . 118.7(7) yes
P1 . C21 . C26 . 123.1(8) yes
C22 . C21 . C26 . 118.2(9) yes
C21 . C22 . C23 . 120.6(11) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . C24 . 119.9(12) yes
C22 . C23 . H231 . 120.1 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 120.2(11) yes
C23 . C24 . H241 . 120.0 no
C25 . C24 . H241 . 119.9 no
C24 . C25 . C26 . 120.3(12) yes
C24 . C25 . H251 . 119.9 no
C26 . C25 . H251 . 119.8 no
C25 . C26 . C21 . 120.8(12) yes
C25 . C26 . H261 . 119.6 no
C21 . C26 . H261 . 119.6 no
Cl31 . C31 . C32 . 113.9(16) yes
Cl31 . C31 . H311 . 108.5 no
C32 . C31 . H311 . 108.4 no
Cl31 . C31 . H312 . 108.2 no
C32 . C31 . H312 . 108.3 no
H311 . C31 . H312 . 109.5 no
C31 . C32 . Cl32 . 103.3(17) yes
C31 . C32 . H321 . 111.0 no
Cl32 . C32 . H321 . 111.0 no
C31 . C32 . H322 . 111.0 no
Cl32 . C32 . H322 . 111.1 no
H321 . C32 . H322 . 109.5 no
Cl41 . C41 . C42 . 114.6(17) yes
Cl41 . C41 . H411 . 108.2 no
Cl31 . C41 . H411 . 122.2 no
C42 . C41 . H411 . 108.1 no
Cl41 . C41 . H412 . 108.2 no
C42 . C41 . H412 . 108.3 no
H411 . C41 . H412 . 109.5 no
C41 . C42 . Cl42 . 123.6(18) yes
C41 . C42 . H421 . 105.9 no
Cl42 . C42 . H421 . 105.9 no
C41 . C42 . H422 . 105.7 no
Cl42 . C42 . H422 . 105.9 no
H421 . C42 . H422 . 109.5 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl31 C6 3.54(2) . . no
Cl32 C14 3.48(2) . 7 no
Cl32 C12 3.58(1) . 1_565 no
Cl41 C32 3.22(4) . 4_566 no
Cl41 C6 3.44(2) . . no
Cl41 C5 3.57(2) . . no
Cl42 C26 3.20(2) . 1_565 no
Cl42 C25 3.43(2) . 1_565 no
C3 C32 3.56(3) . 3_545 no
C25 C25 3.56(3) . 4_556 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pt1 Se1 P1 C1 . . . . -38.8(3) no
Pt1 Se1 P1 C11 . . . . 81.0(3) no
Pt1 Se1 P1 C21 . . . . -158.7(3) no
Pt1 Se1 P1 C1 . 5_655 5_655 5_655 -38.8(3) no
Pt1 Se1 P1 C11 . 5_655 5_655 5_655 81.0(3) no
Pt1 Se1 P1 C21 . 5_655 5_655 5_655 -158.7(3) no
Pt1 C2 C1 P1 . . . . -1.8(7) no
Pt1 C2 C1 C6 . . . . 175.3(6) no
Pt1 C2 C3 C4 . . . . -174.4(6) no
Pt1 C2 C1 P1 . 5_655 5_655 5_655 -1.8(7) no
Pt1 C2 C1 C6 . 5_655 5_655 5_655 175.3(6) no
Pt1 C2 C3 C4 . 5_655 5_655 5_655 -174.4(6) no
Se1 Pt1 Se1 P1 . . 5_655 5_655 -154.41(6) no
Se1 Pt1 C2 C1 . . . . -24.6(5) no
Se1 Pt1 C2 C3 . . . . 149.5(5) no
Se1 P1 C1 C2 . . . . 32.9(6) no
Se1 P1 C1 C6 . . . . -144.2(6) no
Se1 P1 C11 C12 . . . . 24.8(9) no
Se1 P1 C11 C16 . . . . -157.8(7) no
Se1 P1 C21 C22 . . . . 56.8(8) no
Se1 P1 C21 C26 . . . . -121.8(8) no
Cl31 C31 C32 Cl32 . . . . 77(2) no
Cl41 C41 C42 Cl42 . . . . -31(4) no
P1 Se1 Pt1 C2 . . . . 32.8(2) no
P1 C1 C2 C3 . . . . -176.3(5) no
P1 C1 C6 C5 . . . . 177.4(7) no
P1 C11 C12 C13 . . . . 176.7(8) no
P1 C11 C16 C15 . . . . -176.4(9) no
P1 C21 C22 C23 . . . . -177.3(8) no
P1 C21 C26 C25 . . . . 178.6(9) no
C1 P1 C11 C12 . . . . 142.1(8) no
C1 P1 C11 C16 . . . . -41(1) no
C1 P1 C21 C22 . . . . -60.4(8) no
C1 P1 C21 C26 . . . . 120.9(9) no
C1 C2 Pt1 C2 . . . 5_655 148.5(6) no
C1 C2 C3 C4 . . . . 0(1) no
C1 C6 C5 C4 . . . . -3(1) no
C2 Pt1 C2 C3 . . 5_655 5_655 -37.4(5) no
C2 C1 P1 C11 . . . . -89.0(6) no
C2 C1 P1 C21 . . . . 154.6(6) no
C2 C1 C6 C5 . . . . 0(1) no
C2 C3 C4 C5 . . . . -2(1) no
C3 C2 C1 C6 . . . . 1(1) no
C3 C4 C5 C6 . . . . 3(1) no
C6 C1 P1 C11 . . . . 93.8(7) no
C6 C1 P1 C21 . . . . -22.6(8) no
C11 P1 C21 C22 . . . . -179.0(7) no
C11 P1 C21 C26 . . . . 2(1) no
C11 C12 C13 C14 . . . . 1(2) no
C11 C16 C15 C14 . . . . -2(2) no
C12 C11 P1 C21 . . . . -99.1(9) no
C12 C11 C16 C15 . . . . 1(2) no
C12 C13 C14 C15 . . . . -2(2) no
C13 C12 C11 C16 . . . . -1(2) no
C13 C14 C15 C16 . . . . 3(2) no
C16 C11 P1 C21 . . . . 78.3(9) no
C21 C22 C23 C24 . . . . -2(2) no
C21 C26 C25 C24 . . . . -0(2) no
C22 C21 C26 C25 . . . . -0(2) no
C22 C23 C24 C25 . . . . 2(2) no
C23 C22 C21 C26 . . . . 1(2) no
C23 C24 C25 C26 . . . . -0(2) no
_database_code_depnum_ccdc_archive 'CCDC 999161'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex4
_audit_creation_date             09-02-24
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '2241358 ben0902'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-02-25- Report on C40 H36 Cl4 P2 Pd1 Se2 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-02-25- passes checkcif tests with minor warnings  
;

_cell_length_a                   16.0798(2)
_cell_length_b                   11.3798(2)
_cell_length_c                   22.5745(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.2684(8)
_cell_angle_gamma                90
_cell_volume                     3944.60(10)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C40 H36 Cl4 P2 Pd1 Se2 
# Dc =      1.66 Fooo =   1952.00 Mu =     26.97 M =    492.40
# Found Formula = C40 H36.00 Cl4 P2 Pd1 Se2 
# Dc =      1.66 FOOO =   1952.00 Mu =     26.97 M =    492.40

_chemical_formula_sum            'C40 H36 Cl4 P2 Pd1 Se2'
_chemical_formula_moiety         'C36 H28 P2 Pd Se2, 2(C2 H4 Cl2)'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         984.80


_cell_measurement_reflns_used    39222
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.23
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_max          0.43

_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    2.697

# Sheldrick geometric approximatio 0.46 0.54 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.170
-1 0 0 0.170
0 0 1 0.130
0 0 -1 0.160
0 1 0 0.230
0 -1 0 0.200
-1 0 1 0.100
1 0 -1 0.130
0 -4 -4 0.180
0 1 -1 0.208
1 -1 -1 0.150
-1 1 1 0.220
-2 -2 2 0.180
5 5 -5 0.215


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_diffrn_reflns_av_R_equivalents  0.065
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.3 deg at rate 104 sec/frame,
crystal-detector distance 40mm,
multiple scan sets so over 95 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            40812
_reflns_number_total             5748
#_diffrn_reflns_av_R_equivalents   0.102 
# Number of reflections with Friedels Law is 5748 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 5794 


_diffrn_reflns_theta_min         2.654
_diffrn_reflns_theta_max         30.078
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        29.477
_diffrn_measured_fraction_theta_full 0.994


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              -22
_reflns_limit_h_max              21
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   2.71
_oxford_diffrn_Wilson_scale      5.13

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.71
_refine_diff_density_max         0.87


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     75
_refine_ls_number_parameters     260
_oxford_refine_ls_R_factor_ref   0.0398
_refine_ls_wR_factor_ref         0.0937
_refine_ls_goodness_of_fit_ref   1.0021
_refine_ls_shift/su_max          0.019158


# The values computed from all data 
_oxford_reflns_number_all        5747
_refine_ls_R_factor_all          0.0398
_refine_ls_wR_factor_all         0.0937

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4719
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_gt          0.0916

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 1.21P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The 1,2-dichloroethane molecule is disordered 
and this has been modelled by assuming there are 
two overlapping images of the molecule.
Restraints were applied to bond distances and angles and
to displacement parameters.
The relative populations of each image were refined.

Hydrogen atoms were included at idealized positions
and ride on the atoms to which they are attached.

The largest peaks in the final difference electron density map
are located within the disordered solvate molecule.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.5 0.259348(19) 0.25 0.0331 1.0000 Uani S T . . . . .
Se1 Se 0.479614(16) 0.09994(2) 0.321652(11) 0.0405 1.0000 Uani . . . . . . .
Cl31 Cl 0.31348(18) 0.6171(5) 0.4478(4) 0.1367 0.506(6) Uani D U P s 1 . .
Cl32 Cl 0.2743(2) 0.8873(2) 0.35923(15) 0.0964 0.506(6) Uani D U P s 1 . .
Cl41 Cl 0.2918(4) 0.6216(4) 0.4243(3) 0.1300 0.494(6) Uani D U P s 2 . .
Cl42 Cl 0.2844(4) 0.8969(4) 0.4076(3) 0.1801 0.494(6) Uani D U P s 2 . .
P1 P 0.40667(4) 0.22444(5) 0.35784(3) 0.0371 1.0000 Uani . . . . . . .
C1 C 0.46126(16) 0.3631(2) 0.36149(10) 0.0396 1.0000 Uani . . . . . . .
C2 C 0.50016(15) 0.38357(19) 0.31457(10) 0.0367 1.0000 Uani . . . . . . .
C3 C 0.54792(16) 0.4893(2) 0.32009(12) 0.0441 1.0000 Uani . . . . . . .
C4 C 0.55328(19) 0.5679(2) 0.36818(12) 0.0507 1.0000 Uani . . . . . . .
C5 C 0.5118(2) 0.5466(2) 0.41212(13) 0.0580 1.0000 Uani . . . . . . .
C6 C 0.4653(2) 0.4427(2) 0.40941(12) 0.0505 1.0000 Uani . . . . . . .
C11 C 0.29483(17) 0.2402(2) 0.31003(12) 0.0419 1.0000 Uani . . . . . . .
C12 C 0.25309(18) 0.1495(3) 0.27044(13) 0.0509 1.0000 Uani . . . . . . .
C13 C 0.1664(2) 0.1612(3) 0.23575(15) 0.0627 1.0000 Uani . . . . . . .
C14 C 0.1214(2) 0.2619(3) 0.24112(17) 0.0652 1.0000 Uani . . . . . . .
C15 C 0.1617(2) 0.3507(3) 0.28055(16) 0.0623 1.0000 Uani . . . . . . .
C16 C 0.24866(19) 0.3409(2) 0.31486(14) 0.0531 1.0000 Uani . . . . . . .
C21 C 0.40190(19) 0.1850(2) 0.43425(11) 0.0465 1.0000 Uani . . . . . . .
C22 C 0.4807(2) 0.1701(3) 0.48163(12) 0.0599 1.0000 Uani . . . . . . .
C23 C 0.4784(3) 0.1372(3) 0.54057(14) 0.0760 1.0000 Uani . . . . . . .
C24 C 0.4025(3) 0.1196(3) 0.55236(15) 0.0803 1.0000 Uani . . . . . . .
C25 C 0.3252(3) 0.1333(4) 0.50655(19) 0.0926 1.0000 Uani . . . . . . .
C26 C 0.3252(2) 0.1660(4) 0.44693(15) 0.0730 1.0000 Uani . . . . . . .
C31 C 0.2191(9) 0.6883(14) 0.3998(9) 0.1413 0.506(6) Uani D U P s 1 . .
C32 C 0.2255(7) 0.8329(10) 0.4154(5) 0.1090 0.506(6) Uani D U P s 1 . .
C41 C 0.2029(7) 0.7161(15) 0.4110(9) 0.1267 0.494(6) Uani D U P s 2 . .
C42 C 0.2250(8) 0.7895(12) 0.3650(6) 0.1410 0.494(6) Uani D U P s 2 . .
H31 H 0.5786 0.5080 0.2886 0.0517 1.0000 Uiso R . . . . . .
H41 H 0.5881 0.6416 0.3708 0.0575 1.0000 Uiso R . . . . . .
H51 H 0.5149 0.6051 0.4457 0.0669 1.0000 Uiso R . . . . . .
H61 H 0.4351 0.4253 0.4413 0.0608 1.0000 Uiso R . . . . . .
H121 H 0.2857 0.0763 0.2671 0.0615 1.0000 Uiso R . . . . . .
H131 H 0.1366 0.0969 0.2070 0.0747 1.0000 Uiso R . . . . . .
H141 H 0.0589 0.2704 0.2161 0.0775 1.0000 Uiso R . . . . . .
H151 H 0.1281 0.4228 0.2845 0.0759 1.0000 Uiso R . . . . . .
H161 H 0.2780 0.4062 0.3430 0.0638 1.0000 Uiso R . . . . . .
H221 H 0.5376 0.1830 0.4732 0.0706 1.0000 Uiso R . . . . . .
H231 H 0.5343 0.1265 0.5745 0.0890 1.0000 Uiso R . . . . . .
H241 H 0.4022 0.0963 0.5950 0.1010 1.0000 Uiso R . . . . . .
H251 H 0.2688 0.1200 0.5158 0.1204 1.0000 Uiso R . . . . . .
H261 H 0.2688 0.1754 0.4134 0.0922 1.0000 Uiso R . . . . . .
H311 H 0.1661 0.6552 0.4083 0.1675 0.506 Uiso R . . s 1 . .
H312 H 0.2150 0.6756 0.3552 0.1675 0.506 Uiso R . . s 1 . .
H321 H 0.2631 0.8489 0.4586 0.1352 0.506 Uiso R . . s 1 . .
H322 H 0.1666 0.8679 0.4095 0.1352 0.506 Uiso R . . s 1 . .
H411 H 0.2022 0.7610 0.4489 0.1529 0.494 Uiso R . . s 2 . .
H412 H 0.1460 0.6745 0.3937 0.1529 0.494 Uiso R . . s 2 . .
H421 H 0.1715 0.8216 0.3343 0.1610 0.494 Uiso R . . s 2 . .
H422 H 0.2597 0.7443 0.3425 0.1610 0.494 Uiso R . . s 2 . .


_refine_ls_extinction_coef       610(40)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.5178(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . C2 5_655 2.030(2) yes
Pd1 . Se1 5_655 2.5158(3) yes
Pd1 . Se1 . 2.5158(3) yes
Pd1 . C2 . 2.030(2) yes
Se1 . P1 . 2.1493(6) yes
Cl31 . C31 . 1.777(13) yes
Cl32 . C32 . 1.788(9) yes
Cl41 . C41 . 1.742(12) yes
Cl42 . C42 . 1.669(13) yes
P1 . C1 . 1.795(2) yes
P1 . C11 . 1.811(3) yes
P1 . C21 . 1.806(2) yes
C1 . C2 . 1.400(3) yes
C1 . C6 . 1.398(3) yes
C2 . C3 . 1.413(3) yes
C3 . C4 . 1.390(3) yes
C3 . H31 . 1.000 no
C4 . C5 . 1.372(4) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.390(4) yes
C5 . H51 . 1.000 no
C6 . H61 . 1.000 no
C11 . C12 . 1.399(4) yes
C11 . C16 . 1.387(4) yes
C12 . C13 . 1.388(4) yes
C12 . H121 . 1.000 no
C13 . C14 . 1.379(5) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.375(5) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.388(4) yes
C15 . H151 . 1.000 no
C16 . H161 . 1.000 no
C21 . C22 . 1.405(4) yes
C21 . C26 . 1.363(4) yes
C22 . C23 . 1.393(4) yes
C22 . H221 . 1.000 no
C23 . C24 . 1.340(6) yes
C23 . H231 . 1.000 no
C24 . C25 . 1.370(6) yes
C24 . H241 . 1.000 no
C25 . C26 . 1.396(4) yes
C25 . H251 . 1.000 no
C26 . H261 . 1.000 no
C31 . C32 . 1.678(16) yes
C31 . H311 . 1.000 no
C31 . H312 . 1.000 no
C32 . H321 . 1.000 no
C32 . H322 . 1.000 no
C41 . C42 . 1.457(16) yes
C41 . H411 . 1.000 no
C41 . H412 . 1.000 no
C42 . H421 . 1.000 no
C42 . H422 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 5_655 Pd1 . Se1 5_655 90.75(6) yes
C2 5_655 Pd1 . Se1 . 172.37(6) yes
Se1 5_655 Pd1 . Se1 . 87.716(13) yes
C2 5_655 Pd1 . C2 . 91.72(13) yes
Se1 5_655 Pd1 . C2 . 172.37(6) yes
Se1 . Pd1 . C2 . 90.75(6) yes
Pd1 . Se1 . P1 . 87.652(17) yes
Se1 . P1 . C1 . 106.38(8) yes
Se1 . P1 . C11 . 113.33(9) yes
C1 . P1 . C11 . 109.03(11) yes
Se1 . P1 . C21 . 112.45(8) yes
C1 . P1 . C21 . 109.48(11) yes
C11 . P1 . C21 . 106.12(12) yes
P1 . C1 . C2 . 115.71(16) yes
P1 . C1 . C6 . 121.00(19) yes
C2 . C1 . C6 . 123.3(2) yes
C1 . C2 . Pd1 . 121.43(16) yes
C1 . C2 . C3 . 115.4(2) yes
Pd1 . C2 . C3 . 122.77(18) yes
C2 . C3 . C4 . 121.6(2) yes
C2 . C3 . H31 . 119.2 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 121.3(2) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 119.3(2) yes
C4 . C5 . H51 . 120.3 no
C6 . C5 . H51 . 120.3 no
C1 . C6 . C5 . 119.1(3) yes
C1 . C6 . H61 . 120.5 no
C5 . C6 . H61 . 120.4 no
P1 . C11 . C12 . 120.8(2) yes
P1 . C11 . C16 . 119.7(2) yes
C12 . C11 . C16 . 119.5(3) yes
C11 . C12 . C13 . 120.1(3) yes
C11 . C12 . H121 . 120.0 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C14 . 119.7(3) yes
C12 . C13 . H131 . 120.2 no
C14 . C13 . H131 . 120.2 no
C13 . C14 . C15 . 120.6(3) yes
C13 . C14 . H141 . 119.7 no
C15 . C14 . H141 . 119.7 no
C14 . C15 . C16 . 120.3(3) yes
C14 . C15 . H151 . 119.8 no
C16 . C15 . H151 . 119.8 no
C15 . C16 . C11 . 119.8(3) yes
C15 . C16 . H161 . 120.1 no
C11 . C16 . H161 . 120.1 no
P1 . C21 . C22 . 118.2(2) yes
P1 . C21 . C26 . 122.5(2) yes
C22 . C21 . C26 . 119.2(3) yes
C21 . C22 . C23 . 119.1(3) yes
C21 . C22 . H221 . 120.4 no
C23 . C22 . H221 . 120.4 no
C22 . C23 . C24 . 120.9(3) yes
C22 . C23 . H231 . 119.6 no
C24 . C23 . H231 . 119.5 no
C23 . C24 . C25 . 120.6(3) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 119.7 no
C24 . C25 . C26 . 119.9(4) yes
C24 . C25 . H251 . 120.1 no
C26 . C25 . H251 . 120.1 no
C25 . C26 . C21 . 120.3(3) yes
C25 . C26 . H261 . 119.9 no
C21 . C26 . H261 . 119.9 no
Cl31 . C31 . C32 . 109.3(9) yes
Cl31 . C31 . H311 . 109.5 no
C32 . C31 . H311 . 109.4 no
Cl31 . C31 . H312 . 109.6 no
C32 . C31 . H312 . 109.5 no
H311 . C31 . H312 . 109.5 no
Cl32 . C32 . C31 . 101.7(9) yes
Cl32 . C32 . H321 . 111.3 no
C31 . C32 . H321 . 111.4 no
Cl32 . C32 . H322 . 111.4 no
C31 . C32 . H322 . 111.4 no
H321 . C32 . H322 . 109.5 no
Cl41 . C41 . C42 . 96.6(9) yes
Cl41 . C41 . H411 . 112.6 no
C42 . C41 . H411 . 112.6 no
Cl41 . C41 . H412 . 112.6 no
C42 . C41 . H412 . 112.5 no
H411 . C41 . H412 . 109.5 no
C41 . C42 . Cl42 . 103.2(10) yes
C41 . C42 . H421 . 111.1 no
Cl42 . C42 . H421 . 111.0 no
C41 . C42 . H422 . 110.9 no
Cl42 . C42 . H422 . 111.0 no
H421 . C42 . H422 . 109.5 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl31 C32 3.38(2) . 4_566 no
Cl31 C6 3.450(7) . . no
Cl32 C14 3.498(5) . 7 no
Cl32 C12 3.554(4) . 1_565 no
Cl41 C6 3.549(7) . . no
Cl42 C26 3.202(6) . 1_565 no
Cl42 C25 3.433(7) . 1_565 no
C3 C32 3.51(1) . 3_545 no
C3 C42 3.55(1) . 3_545 no
C12 C42 3.56(1) . 7_545 no
C13 C42 3.57(2) . 7_545 no
C25 C25 3.545(9) . 4_556 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 P1 C1 . . . . -38.73(7) no
Pd1 Se1 P1 C11 . . . . 81.1(1) no
Pd1 Se1 P1 C21 . . . . -158.57(9) no
Pd1 Se1 P1 C1 . 5_655 5_655 5_655 -38.73(7) no
Pd1 Se1 P1 C11 . 5_655 5_655 5_655 81.1(1) no
Pd1 Se1 P1 C21 . 5_655 5_655 5_655 -158.57(9) no
Pd1 C2 C1 P1 . . . . -3.4(2) no
Pd1 C2 C1 C6 . . . . 175.2(2) no
Pd1 C2 C3 C4 . . . . -174.0(2) no
Pd1 C2 C1 P1 . 5_655 5_655 5_655 -3.4(2) no
Pd1 C2 C1 C6 . 5_655 5_655 5_655 175.2(2) no
Pd1 C2 C3 C4 . 5_655 5_655 5_655 -174.0(2) no
Se1 Pd1 Se1 P1 . . 5_655 5_655 -155.44(2) no
Se1 Pd1 C2 C1 . . . . -22.9(2) no
Se1 Pd1 C2 C3 . . . . 149.1(2) no
Se1 P1 C1 C2 . . . . 34.0(2) no
Se1 P1 C1 C6 . . . . -144.7(2) no
Se1 P1 C11 C12 . . . . 24.4(3) no
Se1 P1 C11 C16 . . . . -158.7(2) no
Se1 P1 C21 C22 . . . . 57.2(2) no
Se1 P1 C21 C26 . . . . -120.9(3) no
Cl31 C31 C32 Cl32 . . . . 93(1) no
Cl41 C41 C42 Cl42 . . . . -91.6(9) no
P1 Se1 Pd1 C2 . . . . 32.04(7) no
P1 C1 C2 C3 . . . . -175.9(2) no
P1 C1 C6 C5 . . . . 176.9(2) no
P1 C11 C12 C13 . . . . 177.7(3) no
P1 C11 C16 C15 . . . . -176.8(3) no
P1 C21 C22 C23 . . . . -178.6(2) no
P1 C21 C26 C25 . . . . 178.7(3) no
C1 P1 C11 C12 . . . . 142.7(2) no
C1 P1 C11 C16 . . . . -40.5(3) no
C1 P1 C21 C22 . . . . -60.9(2) no
C1 P1 C21 C26 . . . . 121.1(3) no
C1 C2 Pd1 C2 . . . 5_655 149.9(2) no
C1 C2 C3 C4 . . . . -1.6(3) no
C1 C6 C5 C4 . . . . -0.7(4) no
C2 Pd1 C2 C3 . . 5_655 5_655 -38.1(1) no
C2 C1 P1 C11 . . . . -88.6(2) no
C2 C1 P1 C21 . . . . 155.7(2) no
C2 C1 C6 C5 . . . . -1.6(4) no
C2 C3 C4 C5 . . . . -0.5(4) no
C3 C2 C1 C6 . . . . 2.7(3) no
C3 C4 C5 C6 . . . . 1.7(4) no
C6 C1 P1 C11 . . . . 92.8(2) no
C6 C1 P1 C21 . . . . -22.9(2) no
C11 P1 C21 C22 . . . . -178.4(2) no
C11 P1 C21 C26 . . . . 3.6(3) no
C11 C12 C13 C14 . . . . -0.8(5) no
C11 C16 C15 C14 . . . . -1.0(5) no
C12 C11 P1 C21 . . . . -99.5(3) no
C12 C11 C16 C15 . . . . 0.1(5) no
C12 C13 C14 C15 . . . . -0.0(6) no
C13 C12 C11 C16 . . . . 0.8(5) no
C13 C14 C15 C16 . . . . 0.9(6) no
C16 C11 P1 C21 . . . . 77.4(3) no
C21 C22 C23 C24 . . . . 0.1(5) no
C21 C26 C25 C24 . . . . -0.4(6) no
C22 C21 C26 C25 . . . . 0.7(6) no
C22 C23 C24 C25 . . . . 0.2(6) no
C23 C22 C21 C26 . . . . -0.5(5) no
C23 C24 C25 C26 . . . . -0.0(6) no
_database_code_depnum_ccdc_archive 'CCDC 999162'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex8
_audit_creation_date             10-01-15
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2010-01-15 - Report on C40 H34 O4 P2 Pd2 S2 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2010-01-15 - passes checkcif tests with minor warnings  
;

_oxford_structure_analysis_title '1150939 ben0917'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   10.9570(1)
_cell_length_b                   12.5765(2)
_cell_length_c                   15.0107(2)
_cell_angle_alpha                102.7197(7)
_cell_angle_beta                 103.9060(9)
_cell_angle_gamma                103.1252(8)
_cell_volume                     1871.00(5)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C40 H34 O4 P2 Pd2 S2 
# Dc =      1.63 Fooo =    920.00 Mu =     11.99 M =    917.59
# Found Formula = C40 H34 O4 P2 Pd2 S2 
# Dc =      1.63 FOOO =    920.00 Mu =     11.99 M =    917.59

_chemical_formula_sum            'C40 H34 O4 P2 Pd2 S2'
_chemical_formula_moiety         'C40 H34 O4 P2 Pd2 S2'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         917.59


_cell_measurement_reflns_used    36428
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.310

_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    1.199

# Sheldrick geometric approximatio 0.85 0.85 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.140
-1 0 0 0.170
0 1 0 0.040
0 -1 0 0.100
0 0 1 0.070
0 0 -1 0.070
-1 0 1 0.170
1 0 -1 0.120
0 -1 1 0.086
-1 -5 5 0.070
1 0 -6 0.049


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.031

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 2.0 deg at rate 240 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 90 percent of data collected with 2-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            50303
_reflns_number_total             10937
_diffrn_reflns_av_R_equivalents  0.032
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10937 
# Theoretical number of reflections is about 21948 


_diffrn_reflns_theta_min         2.575
_diffrn_reflns_theta_max         30.060
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        30.060
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -15
_reflns_limit_h_max              14
_reflns_limit_k_min              -17
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   2.46
_oxford_diffrn_Wilson_scale      3.27

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.99
_refine_diff_density_max         0.49


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         10935
_refine_ls_number_restraints     71
_refine_ls_number_parameters     515
_oxford_refine_ls_R_factor_ref   0.0344
_refine_ls_wR_factor_ref         0.0691
_refine_ls_goodness_of_fit_ref   1.0064
_refine_ls_shift/su_max          0.0195925
_refine_ls_shift/su_mean         .003 # 0.3163903 


# The values computed from all data 
_oxford_reflns_number_all        10935
_refine_ls_R_factor_all          0.0344
_refine_ls_wR_factor_all         0.0691

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9564
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_gt          0.0656

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.34P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
One phenyl ring is disordered over two orientations related to 
each other by a rotation about the P2---C51 vector.
The relative occupancies of the two images were refined.
Restraints were imposed upon bonded distances, angles, planarity
and displacement parameters in this part of the structure. 


Hydrogen atoms were included at idealized positions.
The positional parameters of the methyl H atoms were refined
while restraints were imposed on distances and angles involving them.
The other H atoms ride on the atoms to which they are bonded.


;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.270944(13) 0.858860(12) 0.685551(10) 0.0309 1.0000 Uani . . . . . . .
Pd2 Pd 0.128545(14) 0.704400(12) 0.771767(10) 0.0310 1.0000 Uani . . . . . . .
S1 S 0.48682(5) 0.93348(5) 0.77997(4) 0.0437 1.0000 Uani . . . . . . .
S2 S 0.13069(6) 0.53507(5) 0.67712(3) 0.0390 1.0000 Uani . . . . . . .
P1 P 0.57202(4) 0.83862(4) 0.70338(4) 0.0294 1.0000 Uani . . . . . . .
P2 P 0.17856(5) 0.46732(4) 0.78465(3) 0.0312 1.0000 Uani . . . . . . .
O11 O 0.08522(14) 0.82500(15) 0.59043(11) 0.0437 1.0000 Uani . . . . . . .
O12 O -0.02593(14) 0.70780(14) 0.65527(11) 0.0409 1.0000 Uani . . . . . . .
O21 O 0.22342(17) 0.97304(14) 0.79172(13) 0.0483 1.0000 Uani . . . . . . .
O22 O 0.11617(17) 0.85252(14) 0.85681(11) 0.0453 1.0000 Uani . . . . . . .
C1 C 0.44338(17) 0.74134(15) 0.60169(13) 0.0294 1.0000 Uani . . . . . . .
C2 C 0.31461(17) 0.74831(16) 0.59140(13) 0.0291 1.0000 Uani . . . . . . .
C3 C 0.21575(19) 0.66433(19) 0.51428(14) 0.0382 1.0000 Uani . . . . . . .
C4 C 0.2426(2) 0.57924(19) 0.45303(15) 0.0397 1.0000 Uani . . . . . . .
C5 C 0.3707(2) 0.57589(17) 0.46371(15) 0.0381 1.0000 Uani . . . . . . .
C6 C 0.47139(19) 0.65746(17) 0.53800(15) 0.0369 1.0000 Uani . . . . . . .
C11 C 0.65122(17) 0.75656(16) 0.77018(13) 0.0301 1.0000 Uani . . . . . . .
C12 C 0.6121(2) 0.7334(2) 0.84691(16) 0.0454 1.0000 Uani . . . . . . .
C13 C 0.6628(3) 0.6610(3) 0.8919(2) 0.0634 1.0000 Uani . . . . . . .
C14 C 0.7499(2) 0.6098(2) 0.86083(18) 0.0517 1.0000 Uani . . . . . . .
C15 C 0.7907(2) 0.63372(19) 0.78604(16) 0.0409 1.0000 Uani . . . . . . .
C16 C 0.7409(2) 0.70625(18) 0.74006(15) 0.0366 1.0000 Uani . . . . . . .
C21 C 0.69150(18) 0.91987(16) 0.65992(15) 0.0343 1.0000 Uani . . . . . . .
C22 C 0.6451(2) 0.94846(19) 0.57574(17) 0.0438 1.0000 Uani . . . . . . .
C23 C 0.7327(3) 1.0106(2) 0.5396(2) 0.0544 1.0000 Uani . . . . . . .
C24 C 0.8666(3) 1.0421(2) 0.5854(2) 0.0608 1.0000 Uani . . . . . . .
C25 C 0.9136(2) 1.0141(2) 0.6684(2) 0.0562 1.0000 Uani . . . . . . .
C26 C 0.8266(2) 0.95433(19) 0.70701(18) 0.0447 1.0000 Uani . . . . . . .
C31 C 0.27714(18) 0.58465(16) 0.88655(12) 0.0304 1.0000 Uani . . . . . . .
C32 C 0.26137(18) 0.69161(16) 0.88158(13) 0.0300 1.0000 Uani . . . . . . .
C33 C 0.3438(2) 0.78619(17) 0.95787(14) 0.0365 1.0000 Uani . . . . . . .
C34 C 0.4342(2) 0.77410(19) 1.03479(14) 0.0398 1.0000 Uani . . . . . . .
C35 C 0.4447(2) 0.66722(19) 1.03941(14) 0.0392 1.0000 Uani . . . . . . .
C36 C 0.3671(2) 0.57224(18) 0.96456(14) 0.0363 1.0000 Uani . . . . . . .
C41 C 0.27309(19) 0.37235(16) 0.75502(13) 0.0322 1.0000 Uani . . . . . . .
C42 C 0.3873(2) 0.41696(19) 0.73275(16) 0.0435 1.0000 Uani . . . . . . .
C43 C 0.4609(3) 0.3467(2) 0.70544(18) 0.0516 1.0000 Uani . . . . . . .
C44 C 0.4196(3) 0.2321(2) 0.69795(18) 0.0530 1.0000 Uani . . . . . . .
C45 C 0.3079(3) 0.1879(2) 0.7191(2) 0.0552 1.0000 Uani . . . . . . .
C46 C 0.2347(2) 0.25756(18) 0.74838(17) 0.0447 1.0000 Uani . . . . . . .
C51 C 0.0387(2) 0.38830(18) 0.81076(16) 0.0420 1.0000 Uani D U . . . . .
C52 C -0.0693(8) 0.3149(6) 0.7353(5) 0.0401 0.533(7) Uani D U P . . . .
C53 C -0.1786(9) 0.2539(7) 0.7532(7) 0.0576 0.533(7) Uani D U P . . . .
C54 C -0.1888(10) 0.2721(8) 0.8436(8) 0.0732 0.533(7) Uani D U P . . . .
C55 C -0.0866(7) 0.3475(6) 0.9172(5) 0.0791 0.533(7) Uani D U P . . . .
C56 C 0.0250(6) 0.4095(5) 0.9018(4) 0.0604 0.533(7) Uani D U P . . . .
C61 C -0.01766(19) 0.75848(19) 0.59345(14) 0.0356 1.0000 Uani D . . . . . .
C62 C -0.1419(2) 0.7363(2) 0.51237(16) 0.0460 1.0000 Uani D . . . . . .
C71 C 0.1638(2) 0.9497(2) 0.84980(16) 0.0421 1.0000 Uani D . . . . . .
C72 C 0.1502(4) 1.0491(3) 0.9207(2) 0.0658 1.0000 Uani D . . . . . .
C521 C -0.0815(10) 0.3449(8) 0.7437(7) 0.0581 0.467(7) Uani D U P . . . .
C531 C -0.1865(12) 0.2804(9) 0.7653(9) 0.0872 0.467(7) Uani D U P . . . .
C541 C -0.1617(12) 0.2541(9) 0.8533(10) 0.0790 0.467(7) Uani D U P . . . .
C551 C -0.0400(8) 0.2934(5) 0.9207(6) 0.0753 0.467(7) Uani D U P . . . .
C561 C 0.0641(7) 0.3570(5) 0.8991(4) 0.0625 0.467(7) Uani D U P . . . .
H31 H 0.1272 0.6659 0.5037 0.0458 1.0000 Uiso R . . . . . .
H41 H 0.1723 0.5225 0.4030 0.0476 1.0000 Uiso R . . . . . .
H51 H 0.3889 0.5184 0.4206 0.0457 1.0000 Uiso R . . . . . .
H61 H 0.5599 0.6568 0.5460 0.0443 1.0000 Uiso R . . . . . .
H121 H 0.5511 0.7671 0.8684 0.0545 1.0000 Uiso R . . . . . .
H131 H 0.6371 0.6462 0.9452 0.0761 1.0000 Uiso R . . . . . .
H141 H 0.7815 0.5583 0.8911 0.0620 1.0000 Uiso R . . . . . .
H151 H 0.8529 0.6007 0.7657 0.0490 1.0000 Uiso R . . . . . .
H161 H 0.7683 0.7217 0.6876 0.0439 1.0000 Uiso R . . . . . .
H221 H 0.5533 0.9253 0.5433 0.0525 1.0000 Uiso R . . . . . .
H231 H 0.7008 1.0315 0.4833 0.0653 1.0000 Uiso R . . . . . .
H241 H 0.9265 1.0833 0.5597 0.0730 1.0000 Uiso R . . . . . .
H251 H 1.0057 1.0358 0.6994 0.0675 1.0000 Uiso R . . . . . .
H261 H 0.8591 0.9371 0.7651 0.0536 1.0000 Uiso R . . . . . .
H331 H 0.3380 0.8602 0.9571 0.0438 1.0000 Uiso R . . . . . .
H341 H 0.4897 0.8400 1.0851 0.0477 1.0000 Uiso R . . . . . .
H351 H 0.5045 0.6597 1.0934 0.0470 1.0000 Uiso R . . . . . .
H361 H 0.3746 0.4988 0.9659 0.0435 1.0000 Uiso R . . . . . .
H421 H 0.4145 0.4955 0.7364 0.0522 1.0000 Uiso R . . . . . .
H431 H 0.5396 0.3774 0.6919 0.0619 1.0000 Uiso R . . . . . .
H441 H 0.4692 0.1838 0.6780 0.0635 1.0000 Uiso R . . . . . .
H451 H 0.2801 0.1089 0.7137 0.0662 1.0000 Uiso R . . . . . .
H461 H 0.1578 0.2263 0.7639 0.0535 1.0000 Uiso R . . . . . .
H521 H -0.0682 0.3065 0.6710 0.0480 0.533 Uiso R . . . . . .
H531 H -0.2477 0.1984 0.7014 0.0690 0.533 Uiso R . . . . . .
H541 H -0.2659 0.2328 0.8548 0.0879 0.533 Uiso R . . . . . .
H551 H -0.0912 0.3583 0.9808 0.0949 0.533 Uiso R . . . . . .
H561 H 0.0920 0.4665 0.9539 0.0724 0.533 Uiso R . . . . . .
H621 H -0.1207(19) 0.7591(18) 0.4617(13) 0.0552 1.0000 Uiso D . . . . . .
H622 H -0.1962(19) 0.7781(17) 0.5332(14) 0.0552 1.0000 Uiso D . . . . . .
H623 H -0.1912(19) 0.6565(15) 0.4896(15) 0.0552 1.0000 Uiso D . . . . . .
H721 H 0.186(2) 1.1187(16) 0.9108(17) 0.0789 1.0000 Uiso D . . . . . .
H722 H 0.198(2) 1.051(2) 0.9830(13) 0.0789 1.0000 Uiso D . . . . . .
H723 H 0.0623(18) 1.0389(19) 0.9178(17) 0.0789 1.0000 Uiso D . . . . . .
H5211 H -0.0943 0.3581 0.6826 0.0698 0.467 Uiso R . . . . . .
H5311 H -0.2729 0.2548 0.7214 0.1046 0.467 Uiso R . . . . . .
H5411 H -0.2323 0.2071 0.8663 0.0950 0.467 Uiso R . . . . . .
H5511 H -0.0274 0.2776 0.9807 0.0903 0.467 Uiso R . . . . . .
H5611 H 0.1511 0.3797 0.9418 0.0749 0.467 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.6217(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Pd2 . 2.92983(19) yes
Pd1 . S1 . 2.2977(6) yes
Pd1 . O11 . 2.0745(15) yes
Pd1 . O21 . 2.1456(15) yes
Pd1 . C2 . 1.9801(18) yes
Pd2 . S2 . 2.2936(5) yes
Pd2 . O12 . 2.1372(13) yes
Pd2 . O22 . 2.0661(15) yes
Pd2 . C32 . 1.9827(17) yes
S1 . P1 . 2.0084(7) yes
S2 . P2 . 2.0020(7) yes
P1 . C1 . 1.7815(18) yes
P1 . C11 . 1.8077(19) yes
P1 . C21 . 1.8111(19) yes
P2 . C31 . 1.7810(19) yes
P2 . C41 . 1.802(2) yes
P2 . C51 . 1.805(2) yes
O11 . C61 . 1.259(3) yes
O12 . C61 . 1.245(2) yes
O21 . C71 . 1.254(3) yes
O22 . C71 . 1.253(3) yes
C1 . C2 . 1.407(2) yes
C1 . C6 . 1.402(3) yes
C2 . C3 . 1.403(3) yes
C3 . C4 . 1.385(3) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.385(3) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.380(3) yes
C5 . H51 . 0.950 no
C6 . H61 . 0.950 no
C11 . C12 . 1.387(3) yes
C11 . C16 . 1.393(3) yes
C12 . C13 . 1.384(3) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.380(4) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.371(3) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.389(3) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.400(3) yes
C21 . C26 . 1.396(3) yes
C22 . C23 . 1.387(3) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.382(4) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.382(4) yes
C24 . H241 . 0.950 no
C25 . C26 . 1.393(3) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . C32 . 1.410(3) yes
C31 . C36 . 1.401(2) yes
C32 . C33 . 1.399(3) yes
C33 . C34 . 1.390(3) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.390(3) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.379(3) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.950 no
C41 . C42 . 1.399(3) yes
C41 . C46 . 1.383(3) yes
C42 . C43 . 1.387(3) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.378(4) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.365(4) yes
C44 . H441 . 0.950 no
C45 . C46 . 1.388(4) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.950 no
C51 . C52 . 1.391(8) yes
C51 . C56 . 1.384(6) yes
C51 . C521 . 1.357(10) yes
C51 . C561 . 1.447(6) yes
C52 . C53 . 1.387(11) yes
C52 . H521 . 0.950 no
C53 . C54 . 1.361(12) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.354(11) yes
C54 . H541 . 0.950 no
C55 . C56 . 1.393(8) yes
C55 . H551 . 0.950 no
C56 . H561 . 0.950 no
C61 . C62 . 1.514(3) yes
C62 . H621 . 0.931(16) no
C62 . H622 . 0.942(16) no
C62 . H623 . 0.965(16) no
C71 . C72 . 1.514(3) yes
C72 . H721 . 0.932(17) no
C72 . H722 . 0.947(17) no
C72 . H723 . 0.932(17) no
C521 . C531 . 1.399(14) yes
C521 . H5211 . 0.950 no
C531 . C541 . 1.410(14) yes
C531 . H5311 . 0.950 no
C541 . C551 . 1.370(13) yes
C541 . H5411 . 0.950 no
C551 . C561 . 1.387(8) yes
C551 . H5511 . 0.950 no
C561 . H5611 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pd2 . Pd1 . S1 . 108.796(17) yes
Pd2 . Pd1 . O11 . 83.25(4) yes
S1 . Pd1 . O11 . 166.87(5) yes
Pd2 . Pd1 . O21 . 77.16(4) yes
S1 . Pd1 . O21 . 87.58(5) yes
O11 . Pd1 . O21 . 90.16(7) yes
Pd2 . Pd1 . C2 . 100.36(5) yes
S1 . Pd1 . C2 . 92.08(5) yes
O11 . Pd1 . C2 . 90.79(7) yes
O21 . Pd1 . C2 . 177.22(7) yes
Pd1 . Pd2 . S2 . 98.354(15) yes
Pd1 . Pd2 . O12 . 77.77(4) yes
S2 . Pd2 . O12 . 88.13(5) yes
Pd1 . Pd2 . O22 . 84.13(4) yes
S2 . Pd2 . O22 . 176.83(5) yes
O12 . Pd2 . O22 . 90.50(6) yes
Pd1 . Pd2 . C32 . 106.77(5) yes
S2 . Pd2 . C32 . 90.63(6) yes
O12 . Pd2 . C32 . 175.42(7) yes
O22 . Pd2 . C32 . 90.52(7) yes
Pd1 . S1 . P1 . 100.57(3) yes
Pd2 . S2 . P2 . 95.65(2) yes
S1 . P1 . C1 . 106.54(6) yes
S1 . P1 . C11 . 111.99(7) yes
C1 . P1 . C11 . 108.07(8) yes
S1 . P1 . C21 . 114.12(7) yes
C1 . P1 . C21 . 107.71(9) yes
C11 . P1 . C21 . 108.16(8) yes
S2 . P2 . C31 . 105.66(6) yes
S2 . P2 . C41 . 109.11(6) yes
C31 . P2 . C41 . 109.98(9) yes
S2 . P2 . C51 . 113.99(8) yes
C31 . P2 . C51 . 109.93(9) yes
C41 . P2 . C51 . 108.13(10) yes
Pd1 . O11 . C61 . 124.15(13) yes
Pd2 . O12 . C61 . 128.47(13) yes
Pd1 . O21 . C71 . 128.45(15) yes
Pd2 . O22 . C71 . 123.38(14) yes
P1 . C1 . C2 . 117.85(14) yes
P1 . C1 . C6 . 119.82(14) yes
C2 . C1 . C6 . 122.24(17) yes
C1 . C2 . Pd1 . 122.94(14) yes
C1 . C2 . C3 . 115.55(17) yes
Pd1 . C2 . C3 . 121.25(13) yes
C2 . C3 . C4 . 122.34(18) yes
C2 . C3 . H31 . 118.8 no
C4 . C3 . H31 . 118.8 no
C3 . C4 . C5 . 120.83(19) yes
C3 . C4 . H41 . 119.6 no
C5 . C4 . H41 . 119.6 no
C4 . C5 . C6 . 118.87(19) yes
C4 . C5 . H51 . 120.6 no
C6 . C5 . H51 . 120.6 no
C1 . C6 . C5 . 120.13(18) yes
C1 . C6 . H61 . 119.9 no
C5 . C6 . H61 . 119.9 no
P1 . C11 . C12 . 119.36(15) yes
P1 . C11 . C16 . 121.13(14) yes
C12 . C11 . C16 . 119.17(18) yes
C11 . C12 . C13 . 119.4(2) yes
C11 . C12 . H121 . 120.3 no
C13 . C12 . H121 . 120.3 no
C12 . C13 . C14 . 121.2(2) yes
C12 . C13 . H131 . 119.4 no
C14 . C13 . H131 . 119.4 no
C13 . C14 . C15 . 119.7(2) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C16 . 119.9(2) yes
C14 . C15 . H151 . 120.1 no
C16 . C15 . H151 . 120.1 no
C11 . C16 . C15 . 120.59(18) yes
C11 . C16 . H161 . 119.7 no
C15 . C16 . H161 . 119.7 no
P1 . C21 . C22 . 118.03(15) yes
P1 . C21 . C26 . 122.54(16) yes
C22 . C21 . C26 . 119.43(19) yes
C21 . C22 . C23 . 120.2(2) yes
C21 . C22 . H221 . 119.9 no
C23 . C22 . H221 . 119.9 no
C22 . C23 . C24 . 120.1(2) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 120.3(2) yes
C23 . C24 . H241 . 119.9 no
C25 . C24 . H241 . 119.9 no
C24 . C25 . C26 . 120.3(2) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 119.8 no
C21 . C26 . C25 . 119.7(2) yes
C21 . C26 . H261 . 120.2 no
C25 . C26 . H261 . 120.2 no
P2 . C31 . C32 . 115.12(13) yes
P2 . C31 . C36 . 122.47(15) yes
C32 . C31 . C36 . 122.38(17) yes
C31 . C32 . Pd2 . 120.95(13) yes
C31 . C32 . C33 . 116.27(17) yes
Pd2 . C32 . C33 . 122.78(14) yes
C32 . C33 . C34 . 121.37(19) yes
C32 . C33 . H331 . 119.3 no
C34 . C33 . H331 . 119.3 no
C33 . C34 . C35 . 121.17(19) yes
C33 . C34 . H341 . 119.4 no
C35 . C34 . H341 . 119.4 no
C34 . C35 . C36 . 119.13(18) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 120.4 no
C31 . C36 . C35 . 119.64(18) yes
C31 . C36 . H361 . 120.2 no
C35 . C36 . H361 . 120.2 no
P2 . C41 . C42 . 117.55(15) yes
P2 . C41 . C46 . 123.36(17) yes
C42 . C41 . C46 . 119.0(2) yes
C41 . C42 . C43 . 120.1(2) yes
C41 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 119.9(2) yes
C42 . C43 . H431 . 120.0 no
C44 . C43 . H431 . 120.0 no
C43 . C44 . C45 . 120.3(2) yes
C43 . C44 . H441 . 119.8 no
C45 . C44 . H441 . 119.8 no
C44 . C45 . C46 . 120.5(2) yes
C44 . C45 . H451 . 119.8 no
C46 . C45 . H451 . 119.8 no
C45 . C46 . C41 . 120.2(2) yes
C45 . C46 . H461 . 119.9 no
C41 . C46 . H461 . 119.9 no
P2 . C51 . C52 . 119.2(4) yes
P2 . C51 . C56 . 122.8(3) yes
C52 . C51 . C56 . 117.3(5) yes
P2 . C51 . C521 . 120.9(5) yes
P2 . C51 . C561 . 117.3(3) yes
C521 . C51 . C561 . 121.0(6) yes
C51 . C52 . C53 . 120.4(6) yes
C51 . C52 . H521 . 119.8 no
C53 . C52 . H521 . 119.8 no
C52 . C53 . C54 . 121.2(8) yes
C52 . C53 . H531 . 119.4 no
C54 . C53 . H531 . 119.4 no
C53 . C54 . C55 . 118.6(8) yes
C53 . C54 . H541 . 120.7 no
C55 . C54 . H541 . 120.7 no
C54 . C55 . C56 . 121.6(7) yes
C54 . C55 . H551 . 119.2 no
C56 . C55 . H551 . 119.2 no
C55 . C56 . C51 . 120.2(5) yes
C55 . C56 . H561 . 119.9 no
C51 . C56 . H561 . 119.9 no
O11 . C61 . O12 . 126.23(18) yes
O11 . C61 . C62 . 116.34(18) yes
O12 . C61 . C62 . 117.41(19) yes
C61 . C62 . H621 . 110.0(12) no
C61 . C62 . H622 . 110.4(12) no
H621 . C62 . H622 . 108.0(14) no
C61 . C62 . H623 . 111.2(12) no
H621 . C62 . H623 . 108.9(14) no
H622 . C62 . H623 . 108.2(14) no
O21 . C71 . O22 . 126.9(2) yes
O21 . C71 . C72 . 116.9(2) yes
O22 . C71 . C72 . 116.2(2) yes
C71 . C72 . H721 . 111.9(14) no
C71 . C72 . H722 . 107.8(14) no
H721 . C72 . H722 . 107.5(16) no
C71 . C72 . H723 . 110.4(14) no
H721 . C72 . H723 . 110.7(15) no
H722 . C72 . H723 . 108.4(16) no
C51 . C521 . C531 . 119.3(9) yes
C51 . C521 . H5211 . 120.3 no
C531 . C521 . H5211 . 120.4 no
C521 . C531 . C541 . 118.9(9) yes
C521 . C531 . H5311 . 120.6 no
C541 . C531 . H5311 . 120.6 no
C531 . C541 . C551 . 122.7(9) yes
C531 . C541 . H5411 . 118.6 no
C551 . C541 . H5411 . 118.7 no
C541 . C551 . C561 . 118.4(8) yes
C541 . C551 . H5511 . 120.8 no
C561 . C551 . H5511 . 120.8 no
C51 . C561 . C551 . 119.1(6) yes
C51 . C561 . H5611 . 120.4 no
C551 . C561 . H5611 . 120.4 no



#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O11 C24 3.500(4) . 2_676 no
O11 C25 3.525(3) . 1_455 no
O12 C16 3.114(3) . 1_455 no
O12 C15 3.257(3) . 1_455 no
O21 C45 3.161(4) . 1_565 no
C4 C521 3.50(1) . 2_566 no
C14 C561 3.569(6) . 2_667 no
C24 C53 3.45(1) . 1_665 no
C24 C52 3.475(7) . 1_665 no
C25 C53 3.47(1) . 1_665 no
C25 C61 3.476(4) . 1_655 no
C25 C62 3.579(3) . 1_655 no
C55 C56 3.421(9) . 2_567 no
C56 C56 3.54(1) . 2_567 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Pd2 S2 P2 . . . . 135.89(2) no
Pd1 Pd2 O12 C61 . . . . 2.4(2) no
Pd1 Pd2 O22 C71 . . . . 0.0(2) no
Pd1 Pd2 C32 C31 . . . . -122.4(2) no
Pd1 Pd2 C32 C33 . . . . 57.8(2) no
Pd1 S1 P1 C1 . . . . -1.09(8) no
Pd1 S1 P1 C11 . . . . -119.06(6) no
Pd1 S1 P1 C21 . . . . 117.64(7) no
Pd1 O11 C61 O12 . . . . 3.8(3) no
Pd1 O11 C61 C62 . . . . -174.5(2) no
Pd1 O21 C71 O22 . . . . -1.6(3) no
Pd1 O21 C71 C72 . . . . 176.9(2) no
Pd1 C2 C1 P1 . . . . -1.1(3) no
Pd1 C2 C1 C6 . . . . 175.5(2) no
Pd1 C2 C3 C4 . . . . -173.5(2) no
Pd2 Pd1 S1 P1 . . . . 102.26(3) no
Pd2 Pd1 O11 C61 . . . . -1.4(2) no
Pd2 Pd1 O21 C71 . . . . 1.1(2) no
Pd2 Pd1 C2 C1 . . . . -109.3(2) no
Pd2 Pd1 C2 C3 . . . . 64.6(2) no
Pd2 S2 P2 C31 . . . . -31.28(8) no
Pd2 S2 P2 C41 . . . . -149.49(6) no
Pd2 S2 P2 C51 . . . . 89.54(8) no
Pd2 O12 C61 O11 . . . . -4.6(4) no
Pd2 O12 C61 C62 . . . . 173.8(2) no
Pd2 O22 C71 O21 . . . . 0.9(3) no
Pd2 O22 C71 C72 . . . . -177.6(2) no
Pd2 C32 C31 P2 . . . . 4.2(2) no
Pd2 C32 C31 C36 . . . . -177.9(2) no
Pd2 C32 C33 C34 . . . . 178.7(2) no
S1 Pd1 Pd2 S2 . . . . -99.48(2) no
S1 Pd1 Pd2 O12 . . . . 174.28(5) no
S1 Pd1 Pd2 O22 . . . . 82.49(5) no
S1 Pd1 Pd2 C32 . . . . -6.28(6) no
S1 Pd1 O11 C61 . . . . -158.4(2) no
S1 Pd1 O21 C71 . . . . -108.8(2) no
S1 Pd1 C2 C1 . . . . 0.2(2) no
S1 Pd1 C2 C3 . . . . 174.1(2) no
S1 P1 C1 C2 . . . . 1.4(2) no
S1 P1 C1 C6 . . . . -175.2(2) no
S1 P1 C11 C12 . . . . 21.8(1) no
S1 P1 C11 C16 . . . . -165.0(1) no
S1 P1 C21 C22 . . . . -82.3(2) no
S1 P1 C21 C26 . . . . 97.7(2) no
S2 Pd2 Pd1 O11 . . . . 85.89(5) no
S2 Pd2 Pd1 O21 . . . . 177.60(5) no
S2 Pd2 Pd1 C2 . . . . -3.68(5) no
S2 Pd2 O12 C61 . . . . -96.5(2) no
S2 Pd2 C32 C31 . . . . -23.4(2) no
S2 Pd2 C32 C33 . . . . 156.7(2) no
S2 P2 C31 C32 . . . . 21.5(2) no
S2 P2 C31 C36 . . . . -156.4(2) no
S2 P2 C41 C42 . . . . 55.9(2) no
S2 P2 C41 C46 . . . . -120.6(2) no
S2 P2 C51 C52 . . . . 43.3(5) no
S2 P2 C51 C56 . . . . -126.8(4) no
S2 P2 C51 C521 . . . . 22.6(6) no
S2 P2 C51 C561 . . . . -167.5(3) no
P1 S1 Pd1 O11 . . . . -101.9(2) no
P1 S1 Pd1 O21 . . . . 177.83(6) no
P1 S1 Pd1 C2 . . . . 0.59(7) no
P1 C1 C2 C3 . . . . -175.3(2) no
P1 C1 C6 C5 . . . . 174.5(2) no
P1 C11 C12 C13 . . . . 173.4(2) no
P1 C11 C16 C15 . . . . -173.2(1) no
P1 C21 C22 C23 . . . . 180.0(2) no
P1 C21 C26 C25 . . . . 178.3(2) no
P2 S2 Pd2 O12 . . . . -146.76(5) no
P2 S2 Pd2 C32 . . . . 28.83(6) no
P2 C31 C32 C33 . . . . -176.0(2) no
P2 C31 C36 C35 . . . . 177.1(2) no
P2 C41 C42 C43 . . . . -177.3(2) no
P2 C41 C46 C45 . . . . 175.7(2) no
P2 C51 C52 C53 . . . . -179.4(7) no
P2 C51 C56 C55 . . . . 178.5(5) no
P2 C51 C521 C52 . . . . 90(2) no
P2 C51 C521 C531 . . . . 177.6(8) no
P2 C51 C561 C551 . . . . -178.2(5) no
O11 Pd1 Pd2 O12 . . . . -0.35(7) no
O11 Pd1 Pd2 O22 . . . . -92.14(7) no
O11 Pd1 Pd2 C32 . . . . 179.10(8) no
O11 Pd1 O21 C71 . . . . 84.2(2) no
O11 Pd1 C2 C1 . . . . 167.4(2) no
O11 Pd1 C2 C3 . . . . -18.7(2) no
O12 Pd2 Pd1 O21 . . . . 91.36(7) no
O12 Pd2 Pd1 C2 . . . . -89.91(7) no
O12 Pd2 O22 C71 . . . . -77.6(2) no
O21 Pd1 Pd2 O22 . . . . -0.42(7) no
O21 Pd1 Pd2 C32 . . . . -89.19(8) no
O21 Pd1 O11 C61 . . . . -78.5(2) no
O22 Pd2 Pd1 C2 . . . . 178.30(7) no
O22 Pd2 O12 C61 . . . . 86.3(2) no
O22 Pd2 C32 C31 . . . . 153.6(2) no
O22 Pd2 C32 C33 . . . . -26.2(2) no
C1 P1 C11 C12 . . . . -95.3(2) no
C1 P1 C11 C16 . . . . 78.0(2) no
C1 P1 C21 C22 . . . . 35.7(2) no
C1 P1 C21 C26 . . . . -144.2(2) no
C1 C2 C3 C4 . . . . 0.8(3) no
C1 C6 C5 C4 . . . . 0.5(4) no
C2 Pd1 Pd2 C32 . . . . 89.53(8) no
C2 Pd1 O11 C61 . . . . 98.9(2) no
C2 C1 P1 C11 . . . . 121.9(2) no
C2 C1 P1 C21 . . . . -121.4(2) no
C2 C1 C6 C5 . . . . -1.9(4) no
C2 C3 C4 C5 . . . . -2.2(4) no
C3 C2 C1 C6 . . . . 1.2(3) no
C3 C4 C5 C6 . . . . 1.5(4) no
C6 C1 P1 C11 . . . . -54.7(2) no
C6 C1 P1 C21 . . . . 62.0(2) no
C11 P1 C21 C22 . . . . 152.3(2) no
C11 P1 C21 C26 . . . . -27.6(2) no
C11 C12 C13 C14 . . . . -1.1(3) no
C11 C16 C15 C14 . . . . 1.0(3) no
C12 C11 P1 C21 . . . . 148.4(1) no
C12 C11 C16 C15 . . . . 0.0(2) no
C12 C13 C14 C15 . . . . 2.2(3) no
C13 C12 C11 C16 . . . . 0.0(3) no
C13 C14 C15 C16 . . . . -2.1(3) no
C16 C11 P1 C21 . . . . -38.4(2) no
C21 C22 C23 C24 . . . . 1.6(4) no
C21 C26 C25 C24 . . . . 1.8(4) no
C22 C21 C26 C25 . . . . -1.6(3) no
C22 C23 C24 C25 . . . . -1.4(4) no
C23 C22 C21 C26 . . . . -0.1(3) no
C23 C24 C25 C26 . . . . -0.3(4) no
C31 P2 C41 C42 . . . . -59.6(2) no
C31 P2 C41 C46 . . . . 124.0(2) no
C31 P2 C51 C52 . . . . 161.7(4) no
C31 P2 C51 C56 . . . . -8.4(4) no
C31 P2 C51 C521 . . . . 140.9(6) no
C31 P2 C51 C561 . . . . -49.1(3) no
C31 C32 C33 C34 . . . . -1.1(3) no
C31 C36 C35 C34 . . . . -1.5(4) no
C32 Pd2 O22 C71 . . . . 106.8(2) no
C32 C31 P2 C41 . . . . 139.1(2) no
C32 C31 P2 C51 . . . . -101.9(2) no
C32 C31 C36 C35 . . . . -0.6(3) no
C32 C33 C34 C35 . . . . -0.9(4) no
C33 C32 C31 C36 . . . . 1.9(3) no
C33 C34 C35 C36 . . . . 2.3(4) no
C36 C31 P2 C41 . . . . -38.8(2) no
C36 C31 P2 C51 . . . . 80.2(2) no
C41 P2 C51 C52 . . . . -78.2(4) no
C41 P2 C51 C56 . . . . 111.7(4) no
C41 P2 C51 C521 . . . . -99.0(6) no
C41 P2 C51 C561 . . . . 71.0(3) no
C41 C42 C43 C44 . . . . 1.6(3) no
C41 C46 C45 C44 . . . . 1.0(4) no
C42 C41 P2 C51 . . . . -179.6(2) no
C42 C41 C46 C45 . . . . -0.7(3) no
C42 C43 C44 C45 . . . . -1.3(4) no
C43 C42 C41 C46 . . . . -0.6(3) no
C43 C44 C45 C46 . . . . -0.0(4) no
C46 C41 P2 C51 . . . . 3.9(2) no
C51 C52 C53 C54 . . . . 6(1) no
C51 C56 C55 C54 . . . . -5(1) no
C51 C521 C531 C541 . . . . -5(2) no
C51 C561 C551 C541 . . . . 6(1) no
C52 C51 C56 C55 . . . . 8.2(9) no
C52 C53 C54 C55 . . . . -3(2) no
C53 C52 C51 C56 . . . . -9(1) no
C53 C54 C55 C56 . . . . 3(2) no
C521 C51 C561 C551 . . . . -8.2(9) no
C521 C531 C541 C551 . . . . 3(2) no
C531 C521 C51 C561 . . . . 8(1) no
C531 C541 C551 C561 . . . . -3(2) no
_database_code_depnum_ccdc_archive 'CCDC 999163'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex9
_audit_creation_date             09-12-22
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title '12221126 ben0916'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-12-22- Report on C23 H21 O2 P Pd S 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-11-25- passes checkcif tests with minor warnings  
;

_cell_length_a                   9.1580(2)
_cell_length_b                   16.9618(3)
_cell_length_c                   27.7043(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.7247(12)
_cell_angle_gamma                90
_cell_volume                     4303.14(15)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C23 H21 O2 P1 Pd1 S1 
# Dc =      1.54 Fooo =   2016.00 Mu =     10.49 M =    997.72
# Found Formula = C23 H21 O2 P1 Pd1 S1 
# Dc =      1.54 FOOO =   2016.00 Mu =     10.49 M =    997.72

_chemical_formula_sum            'C23 H21 O2 P Pd S'
_chemical_formula_moiety         'C23 H21 O2 P Pd S'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         498.86


_cell_measurement_reflns_used    98955
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.09
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.27

_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2016
_exptl_absorpt_coefficient_mu    1.049

# Sheldrick geometric approximatio 1.00 1.00 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.150
-1 0 0 0.120
0 1 -1 0.030
0 -1 1 0.060
0 1 1 0.029
0 -7 -7 0.073
0 0 1 0.062
0 0 -1 0.060


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.2 deg at rate 24 sec/frame,
crystal-detector distance 40mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            67914
_reflns_number_total             7579
_diffrn_reflns_av_R_equivalents  0.079
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7579 
# Theoretical number of reflections is about 15213 


_diffrn_reflns_theta_min         2.625
_diffrn_reflns_theta_max         25.032
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        25.032
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              32

_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      128.16

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.18
_refine_diff_density_max         1.28


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7579
_refine_ls_number_restraints     0
_refine_ls_number_parameters     505
_oxford_refine_ls_R_factor_ref   0.0707
_refine_ls_wR_factor_ref         0.0857
_refine_ls_goodness_of_fit_ref   0.9847
_refine_ls_shift/su_max          0.0244203
_refine_ls_shift/su_mean         0.0019693


# The values computed from all data 
_oxford_reflns_number_all        7579
_refine_ls_R_factor_all          0.0707
_refine_ls_wR_factor_all         0.0857

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5327
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_gt          0.0772

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 7.60P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;

Hydrogen atoms were included at idealized positions
They were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.


;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.90664(3) 0.73072(2) 0.286331(12) 0.0329 1.0000 Uani . . . . . . .
Pd2 Pd 0.48477(3) 0.22569(2) 0.461446(11) 0.0353 1.0000 Uani . . . . . . .
S1 S 1.14390(11) 0.68850(7) 0.29824(4) 0.0375 1.0000 Uani . . . . . . .
S2 S 0.66890(13) 0.31632(7) 0.45736(4) 0.0428 1.0000 Uani . . . . . . .
P1 P 1.10833(12) 0.58754(7) 0.26199(4) 0.0323 1.0000 Uani . . . . . . .
P2 P 0.73617(12) 0.30885(7) 0.52656(4) 0.0322 1.0000 Uani . . . . . . .
O11 O 0.6970(3) 0.76488(18) 0.27572(10) 0.0424 1.0000 Uani . . . . . . .
O12 O 0.9170(3) 0.78864(17) 0.35262(10) 0.0403 1.0000 Uani . . . . . . .
O21 O 0.3139(3) 0.14828(18) 0.46465(11) 0.0448 1.0000 Uani . . . . . . .
O22 O 0.3979(3) 0.27859(18) 0.39976(11) 0.0477 1.0000 Uani . . . . . . .
C1 C 0.9924(4) 0.6133(2) 0.21244(15) 0.0339 1.0000 Uani . . . . . . .
C2 C 0.9009(4) 0.6776(2) 0.22211(15) 0.0317 1.0000 Uani . . . . . . .
C3 C 0.8061(5) 0.7018(3) 0.18519(15) 0.0386 1.0000 Uani . . . . . . .
C4 C 0.8056(5) 0.6642(3) 0.14096(16) 0.0418 1.0000 Uani . . . . . . .
C5 C 0.8937(5) 0.5999(3) 0.13243(16) 0.0443 1.0000 Uani . . . . . . .
C6 C 0.9891(5) 0.5745(3) 0.16800(15) 0.0410 1.0000 Uani . . . . . . .
C11 C 1.0159(4) 0.5145(2) 0.29805(15) 0.0342 1.0000 Uani . . . . . . .
C12 C 1.0752(5) 0.4936(3) 0.34211(17) 0.0500 1.0000 Uani . . . . . . .
C13 C 1.0039(7) 0.4394(3) 0.37072(19) 0.0634 1.0000 Uani . . . . . . .
C14 C 0.8755(7) 0.4053(3) 0.3542(2) 0.0642 1.0000 Uani . . . . . . .
C15 C 0.8174(6) 0.4255(3) 0.3105(2) 0.0584 1.0000 Uani . . . . . . .
C16 C 0.8866(5) 0.4810(3) 0.28215(17) 0.0449 1.0000 Uani . . . . . . .
C21 C 1.2775(4) 0.5434(3) 0.24258(15) 0.0335 1.0000 Uani . . . . . . .
C22 C 1.3900(6) 0.5905(3) 0.2271(2) 0.0634 1.0000 Uani . . . . . . .
C23 C 1.5175(6) 0.5565(4) 0.2100(2) 0.0720 1.0000 Uani . . . . . . .
C24 C 1.5325(5) 0.4768(3) 0.20914(18) 0.0545 1.0000 Uani . . . . . . .
C25 C 1.4232(5) 0.4299(3) 0.2256(2) 0.0624 1.0000 Uani . . . . . . .
C26 C 1.2963(5) 0.4632(3) 0.24268(18) 0.0505 1.0000 Uani . . . . . . .
C31 C 0.4683(5) 0.8168(3) 0.29173(18) 0.0539 1.0000 Uani . . . . . . .
C32 C 0.6227(5) 0.8021(3) 0.30694(17) 0.0389 1.0000 Uani . . . . . . .
C33 C 0.6700(5) 0.8290(3) 0.35168(17) 0.0445 1.0000 Uani . . . . . . .
C34 C 0.8105(5) 0.8227(3) 0.37205(16) 0.0409 1.0000 Uani . . . . . . .
C35 C 0.8382(5) 0.8587(3) 0.42078(17) 0.0586 1.0000 Uani . . . . . . .
C41 C 0.6934(4) 0.2109(2) 0.54513(15) 0.0308 1.0000 Uani . . . . . . .
C42 C 0.5829(4) 0.1739(2) 0.51753(15) 0.0342 1.0000 Uani . . . . . . .
C43 C 0.5499(5) 0.0963(3) 0.52980(16) 0.0383 1.0000 Uani . . . . . . .
C44 C 0.6241(5) 0.0580(3) 0.56686(16) 0.0417 1.0000 Uani . . . . . . .
C45 C 0.7305(5) 0.0963(3) 0.59453(16) 0.0407 1.0000 Uani . . . . . . .
C46 C 0.7658(4) 0.1736(3) 0.58365(15) 0.0360 1.0000 Uani . . . . . . .
C51 C 0.6458(4) 0.3786(3) 0.56536(15) 0.0343 1.0000 Uani . . . . . . .
C52 C 0.6467(5) 0.4581(3) 0.55269(18) 0.0485 1.0000 Uani . . . . . . .
C53 C 0.5786(6) 0.5127(3) 0.5814(2) 0.0649 1.0000 Uani . . . . . . .
C54 C 0.5091(6) 0.4886(4) 0.6226(2) 0.0677 1.0000 Uani . . . . . . .
C55 C 0.5064(5) 0.4110(4) 0.63530(19) 0.0606 1.0000 Uani . . . . . . .
C56 C 0.5746(5) 0.3553(3) 0.60638(16) 0.0450 1.0000 Uani . . . . . . .
C61 C 0.9288(4) 0.3304(2) 0.53145(15) 0.0339 1.0000 Uani . . . . . . .
C62 C 1.0181(5) 0.3215(3) 0.49177(16) 0.0413 1.0000 Uani . . . . . . .
C63 C 1.1648(5) 0.3393(3) 0.49549(18) 0.0497 1.0000 Uani . . . . . . .
C64 C 1.2238(5) 0.3651(3) 0.53857(19) 0.0505 1.0000 Uani . . . . . . .
C65 C 1.1370(5) 0.3734(3) 0.57861(18) 0.0519 1.0000 Uani . . . . . . .
C66 C 0.9894(5) 0.3561(3) 0.57495(16) 0.0450 1.0000 Uani . . . . . . .
C71 C 0.0840(5) 0.0931(3) 0.4482(2) 0.0692 1.0000 Uani . . . . . . .
C72 C 0.2053(5) 0.1490(3) 0.43539(19) 0.0502 1.0000 Uani . . . . . . .
C73 C 0.1912(6) 0.1953(3) 0.39416(18) 0.0546 1.0000 Uani . . . . . . .
C74 C 0.2835(6) 0.2532(3) 0.37782(17) 0.0494 1.0000 Uani . . . . . . .
C75 C 0.2558(6) 0.2926(3) 0.32963(18) 0.0655 1.0000 Uani . . . . . . .
H31 H 0.7429 0.7433 0.1901 0.0452 1.0000 Uiso R . . . . . .
H41 H 0.7424 0.6820 0.1165 0.0489 1.0000 Uiso R . . . . . .
H51 H 0.8898 0.5738 0.1033 0.0530 1.0000 Uiso R . . . . . .
H61 H 1.0493 0.5320 0.1628 0.0488 1.0000 Uiso R . . . . . .
H121 H 1.1615 0.5164 0.3529 0.0598 1.0000 Uiso R . . . . . .
H131 H 1.0441 0.4264 0.4006 0.0762 1.0000 Uiso R . . . . . .
H141 H 0.8299 0.3680 0.3735 0.0768 1.0000 Uiso R . . . . . .
H151 H 0.7334 0.4013 0.2995 0.0698 1.0000 Uiso R . . . . . .
H161 H 0.8451 0.4957 0.2530 0.0539 1.0000 Uiso R . . . . . .
H221 H 1.3807 0.6449 0.2278 0.0759 1.0000 Uiso R . . . . . .
H231 H 1.5925 0.5884 0.1996 0.0862 1.0000 Uiso R . . . . . .
H241 H 1.6170 0.4539 0.1977 0.0645 1.0000 Uiso R . . . . . .
H251 H 1.4333 0.3754 0.2256 0.0753 1.0000 Uiso R . . . . . .
H261 H 1.2233 0.4313 0.2544 0.0612 1.0000 Uiso R . . . . . .
H311 H 0.4207 0.8499 0.3143 0.0807 1.0000 Uiso R . . . . . .
H312 H 0.4642 0.8405 0.2606 0.0809 1.0000 Uiso R . . . . . .
H313 H 0.4191 0.7680 0.2898 0.0812 1.0000 Uiso R . . . . . .
H331 H 0.6008 0.8536 0.3703 0.0526 1.0000 Uiso R . . . . . .
H351 H 0.7500 0.8671 0.4373 0.0882 1.0000 Uiso R . . . . . .
H352 H 0.8864 0.9078 0.4165 0.0883 1.0000 Uiso R . . . . . .
H353 H 0.8994 0.8257 0.4396 0.0884 1.0000 Uiso R . . . . . .
H431 H 0.4762 0.0702 0.5125 0.0456 1.0000 Uiso R . . . . . .
H441 H 0.6031 0.0059 0.5733 0.0494 1.0000 Uiso R . . . . . .
H451 H 0.7775 0.0699 0.6195 0.0488 1.0000 Uiso R . . . . . .
H461 H 0.8376 0.2004 0.6008 0.0425 1.0000 Uiso R . . . . . .
H521 H 0.6931 0.4738 0.5246 0.0578 1.0000 Uiso R . . . . . .
H531 H 0.5815 0.5656 0.5731 0.0777 1.0000 Uiso R . . . . . .
H541 H 0.4628 0.5252 0.6419 0.0808 1.0000 Uiso R . . . . . .
H551 H 0.4586 0.3944 0.6628 0.0725 1.0000 Uiso R . . . . . .
H561 H 0.5724 0.3026 0.6149 0.0541 1.0000 Uiso R . . . . . .
H621 H 0.9788 0.3037 0.4629 0.0493 1.0000 Uiso R . . . . . .
H631 H 1.2235 0.3331 0.4689 0.0600 1.0000 Uiso R . . . . . .
H641 H 1.3225 0.3772 0.5410 0.0610 1.0000 Uiso R . . . . . .
H651 H 1.1771 0.3899 0.6080 0.0620 1.0000 Uiso R . . . . . .
H661 H 0.9301 0.3614 0.6016 0.0539 1.0000 Uiso R . . . . . .
H711 H 0.0341 0.0768 0.4195 0.1040 1.0000 Uiso R . . . . . .
H712 H 0.0157 0.1192 0.4682 0.1042 1.0000 Uiso R . . . . . .
H713 H 0.1210 0.0477 0.4646 0.1039 1.0000 Uiso R . . . . . .
H731 H 0.1096 0.1858 0.3751 0.0645 1.0000 Uiso R . . . . . .
H751 H 0.1554 0.2860 0.3204 0.0979 1.0000 Uiso R . . . . . .
H752 H 0.2780 0.3479 0.3316 0.0980 1.0000 Uiso R . . . . . .
H753 H 0.3167 0.2688 0.3059 0.0980 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.097684(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . S1 . 2.3075(11) yes
Pd1 . O11 . 2.023(3) yes
Pd1 . O12 . 2.084(3) yes
Pd1 . C2 . 1.994(4) yes
Pd2 . S2 . 2.2857(12) yes
Pd2 . O21 . 2.045(3) yes
Pd2 . O22 . 2.080(3) yes
Pd2 . C42 . 1.989(4) yes
S1 . P1 . 2.0096(16) yes
S2 . P2 . 2.0102(16) yes
P1 . C1 . 1.779(4) yes
P1 . C11 . 1.808(4) yes
P1 . C21 . 1.809(4) yes
P2 . C41 . 1.784(4) yes
P2 . C51 . 1.806(4) yes
P2 . C61 . 1.805(4) yes
O11 . C32 . 1.275(5) yes
O12 . C34 . 1.260(5) yes
O21 . C72 . 1.275(5) yes
O22 . C74 . 1.279(6) yes
C1 . C2 . 1.403(6) yes
C1 . C6 . 1.396(6) yes
C2 . C3 . 1.395(6) yes
C3 . C4 . 1.382(6) yes
C3 . H31 . 0.922 no
C4 . C5 . 1.379(6) yes
C4 . H41 . 0.935 no
C5 . C6 . 1.378(6) yes
C5 . H51 . 0.922 no
C6 . H61 . 0.920 no
C11 . C12 . 1.376(6) yes
C11 . C16 . 1.381(6) yes
C12 . C13 . 1.383(7) yes
C12 . H121 . 0.926 no
C13 . C14 . 1.382(8) yes
C13 . H131 . 0.927 no
C14 . C15 . 1.360(7) yes
C14 . H141 . 0.930 no
C15 . C16 . 1.384(6) yes
C15 . H151 . 0.922 no
C16 . H161 . 0.923 no
C21 . C22 . 1.377(6) yes
C21 . C26 . 1.370(6) yes
C22 . C23 . 1.391(7) yes
C22 . H221 . 0.927 no
C23 . C24 . 1.359(7) yes
C23 . H231 . 0.923 no
C24 . C25 . 1.362(7) yes
C24 . H241 . 0.925 no
C25 . C26 . 1.381(6) yes
C25 . H251 . 0.929 no
C26 . H261 . 0.922 no
C31 . C32 . 1.491(6) yes
C31 . H311 . 0.950 no
C31 . H312 . 0.951 no
C31 . H313 . 0.943 no
C32 . C33 . 1.385(6) yes
C33 . C34 . 1.403(6) yes
C33 . H331 . 0.922 no
C34 . C35 . 1.500(6) yes
C35 . H351 . 0.945 no
C35 . H352 . 0.950 no
C35 . H353 . 0.944 no
C41 . C42 . 1.408(6) yes
C41 . C46 . 1.400(6) yes
C42 . C43 . 1.394(6) yes
C43 . C44 . 1.386(6) yes
C43 . H431 . 0.934 no
C44 . C45 . 1.393(6) yes
C44 . H441 . 0.922 no
C45 . C46 . 1.385(6) yes
C45 . H451 . 0.925 no
C46 . H461 . 0.926 no
C51 . C52 . 1.394(6) yes
C51 . C56 . 1.375(6) yes
C52 . C53 . 1.375(7) yes
C52 . H521 . 0.930 no
C53 . C54 . 1.377(8) yes
C53 . H531 . 0.927 no
C54 . C55 . 1.362(8) yes
C54 . H541 . 0.926 no
C55 . C56 . 1.392(7) yes
C55 . H551 . 0.928 no
C56 . H561 . 0.925 no
C61 . C62 . 1.387(6) yes
C61 . C66 . 1.391(6) yes
C62 . C63 . 1.379(6) yes
C62 . H621 . 0.924 no
C63 . C64 . 1.376(7) yes
C63 . H631 . 0.925 no
C64 . C65 . 1.380(6) yes
C64 . H641 . 0.928 no
C65 . C66 . 1.385(6) yes
C65 . H651 . 0.933 no
C66 . H661 . 0.926 no
C71 . C72 . 1.507(7) yes
C71 . H711 . 0.954 no
C71 . H712 . 0.950 no
C71 . H713 . 0.955 no
C72 . C73 . 1.390(7) yes
C73 . C74 . 1.376(7) yes
C73 . H731 . 0.925 no
C74 . C75 . 1.511(7) yes
C75 . H751 . 0.958 no
C75 . H752 . 0.961 no
C75 . H753 . 0.957 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 . Pd1 . O11 . 178.56(9) yes
S1 . Pd1 . O12 . 89.31(8) yes
O11 . Pd1 . O12 . 91.47(11) yes
S1 . Pd1 . C2 . 90.08(12) yes
O11 . Pd1 . C2 . 89.18(14) yes
O12 . Pd1 . C2 . 178.28(14) yes
S2 . Pd2 . O21 . 177.62(9) yes
S2 . Pd2 . O22 . 86.79(9) yes
O21 . Pd2 . O22 . 91.58(13) yes
S2 . Pd2 . C42 . 90.52(12) yes
O21 . Pd2 . C42 . 91.22(15) yes
O22 . Pd2 . C42 . 175.34(14) yes
Pd1 . S1 . P1 . 92.67(5) yes
Pd2 . S2 . P2 . 97.34(6) yes
S1 . P1 . C1 . 105.52(15) yes
S1 . P1 . C11 . 112.44(15) yes
C1 . P1 . C11 . 108.4(2) yes
S1 . P1 . C21 . 111.57(15) yes
C1 . P1 . C21 . 112.17(19) yes
C11 . P1 . C21 . 106.79(19) yes
S2 . P2 . C41 . 105.55(15) yes
S2 . P2 . C51 . 112.90(15) yes
C41 . P2 . C51 . 109.5(2) yes
S2 . P2 . C61 . 110.25(15) yes
C41 . P2 . C61 . 112.62(19) yes
C51 . P2 . C61 . 106.12(19) yes
Pd1 . O11 . C32 . 123.8(3) yes
Pd1 . O12 . C34 . 124.4(3) yes
Pd2 . O21 . C72 . 123.8(3) yes
Pd2 . O22 . C74 . 123.2(3) yes
P1 . C1 . C2 . 113.3(3) yes
P1 . C1 . C6 . 124.8(3) yes
C2 . C1 . C6 . 121.9(4) yes
C1 . C2 . Pd1 . 120.8(3) yes
C1 . C2 . C3 . 117.2(4) yes
Pd1 . C2 . C3 . 122.0(3) yes
C2 . C3 . C4 . 120.6(4) yes
C2 . C3 . H31 . 120.2 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 121.5(4) yes
C3 . C4 . H41 . 119.2 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 119.5(4) yes
C4 . C5 . H51 . 120.9 no
C6 . C5 . H51 . 119.6 no
C1 . C6 . C5 . 119.3(4) yes
C1 . C6 . H61 . 120.1 no
C5 . C6 . H61 . 120.5 no
P1 . C11 . C12 . 119.0(3) yes
P1 . C11 . C16 . 120.8(3) yes
C12 . C11 . C16 . 120.3(4) yes
C11 . C12 . C13 . 119.7(5) yes
C11 . C12 . H121 . 120.3 no
C13 . C12 . H121 . 120.0 no
C12 . C13 . C14 . 119.6(5) yes
C12 . C13 . H131 . 118.9 no
C14 . C13 . H131 . 121.5 no
C13 . C14 . C15 . 120.7(5) yes
C13 . C14 . H141 . 118.8 no
C15 . C14 . H141 . 120.6 no
C14 . C15 . C16 . 120.0(5) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 120.0 no
C15 . C16 . C11 . 119.7(5) yes
C15 . C16 . H161 . 119.6 no
C11 . C16 . H161 . 120.7 no
P1 . C21 . C22 . 119.9(3) yes
P1 . C21 . C26 . 121.2(3) yes
C22 . C21 . C26 . 118.8(4) yes
C21 . C22 . C23 . 120.0(5) yes
C21 . C22 . H221 . 120.2 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 120.3(5) yes
C22 . C23 . H231 . 119.7 no
C24 . C23 . H231 . 120.1 no
C23 . C24 . C25 . 120.0(5) yes
C23 . C24 . H241 . 120.6 no
C25 . C24 . H241 . 119.4 no
C24 . C25 . C26 . 120.1(5) yes
C24 . C25 . H251 . 120.5 no
C26 . C25 . H251 . 119.4 no
C25 . C26 . C21 . 120.7(4) yes
C25 . C26 . H261 . 119.8 no
C21 . C26 . H261 . 119.4 no
C32 . C31 . H311 . 110.8 no
C32 . C31 . H312 . 110.7 no
H311 . C31 . H312 . 109.3 no
C32 . C31 . H313 . 108.7 no
H311 . C31 . H313 . 109.5 no
H312 . C31 . H313 . 107.8 no
C31 . C32 . O11 . 113.8(4) yes
C31 . C32 . C33 . 118.9(4) yes
O11 . C32 . C33 . 127.4(4) yes
C32 . C33 . C34 . 127.6(4) yes
C32 . C33 . H331 . 116.1 no
C34 . C33 . H331 . 116.4 no
C33 . C34 . O12 . 125.1(4) yes
C33 . C34 . C35 . 118.3(4) yes
O12 . C34 . C35 . 116.6(4) yes
C34 . C35 . H351 . 111.3 no
C34 . C35 . H352 . 108.5 no
H351 . C35 . H352 . 109.3 no
C34 . C35 . H353 . 110.4 no
H351 . C35 . H353 . 109.0 no
H352 . C35 . H353 . 108.4 no
P2 . C41 . C42 . 114.6(3) yes
P2 . C41 . C46 . 122.5(3) yes
C42 . C41 . C46 . 122.9(4) yes
C41 . C42 . Pd2 . 122.8(3) yes
C41 . C42 . C43 . 116.4(4) yes
Pd2 . C42 . C43 . 120.6(3) yes
C42 . C43 . C44 . 121.2(4) yes
C42 . C43 . H431 . 118.8 no
C44 . C43 . H431 . 120.1 no
C43 . C44 . C45 . 121.4(4) yes
C43 . C44 . H441 . 119.5 no
C45 . C44 . H441 . 119.1 no
C44 . C45 . C46 . 119.1(4) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 120.8 no
C41 . C46 . C45 . 119.0(4) yes
C41 . C46 . H461 . 119.7 no
C45 . C46 . H461 . 121.3 no
P2 . C51 . C52 . 118.7(3) yes
P2 . C51 . C56 . 122.0(3) yes
C52 . C51 . C56 . 119.3(4) yes
C51 . C52 . C53 . 120.2(5) yes
C51 . C52 . H521 . 119.5 no
C53 . C52 . H521 . 120.4 no
C52 . C53 . C54 . 119.8(5) yes
C52 . C53 . H531 . 119.6 no
C54 . C53 . H531 . 120.5 no
C53 . C54 . C55 . 120.7(5) yes
C53 . C54 . H541 . 120.0 no
C55 . C54 . H541 . 119.2 no
C54 . C55 . C56 . 119.8(5) yes
C54 . C55 . H551 . 121.1 no
C56 . C55 . H551 . 119.0 no
C55 . C56 . C51 . 120.1(5) yes
C55 . C56 . H561 . 119.8 no
C51 . C56 . H561 . 120.0 no
P2 . C61 . C62 . 120.3(3) yes
P2 . C61 . C66 . 120.5(3) yes
C62 . C61 . C66 . 119.2(4) yes
C61 . C62 . C63 . 120.1(4) yes
C61 . C62 . H621 . 119.7 no
C63 . C62 . H621 . 120.3 no
C62 . C63 . C64 . 120.4(4) yes
C62 . C63 . H631 . 119.4 no
C64 . C63 . H631 . 120.1 no
C63 . C64 . C65 . 120.4(4) yes
C63 . C64 . H641 . 120.3 no
C65 . C64 . H641 . 119.3 no
C64 . C65 . C66 . 119.4(4) yes
C64 . C65 . H651 . 120.6 no
C66 . C65 . H651 . 120.0 no
C61 . C66 . C65 . 120.5(4) yes
C61 . C66 . H661 . 119.3 no
C65 . C66 . H661 . 120.2 no
C72 . C71 . H711 . 109.5 no
C72 . C71 . H712 . 109.7 no
H711 . C71 . H712 . 108.1 no
C72 . C71 . H713 . 111.2 no
H711 . C71 . H713 . 109.0 no
H712 . C71 . H713 . 109.4 no
C71 . C72 . O21 . 114.5(5) yes
C71 . C72 . C73 . 119.2(5) yes
O21 . C72 . C73 . 126.3(5) yes
C72 . C73 . C74 . 128.5(5) yes
C72 . C73 . H731 . 115.9 no
C74 . C73 . H731 . 115.6 no
C73 . C74 . O22 . 125.9(5) yes
C73 . C74 . C75 . 120.6(5) yes
O22 . C74 . C75 . 113.5(5) yes
C74 . C75 . H751 . 109.5 no
C74 . C75 . H752 . 110.4 no
H751 . C75 . H752 . 109.3 no
C74 . C75 . H753 . 109.2 no
H751 . C75 . H753 . 109.5 no
H752 . C75 . H753 . 109.0 no

#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O12 C66 3.278(6) . 2_766 no
O12 C65 3.384(6) . 2_766 no
O12 C46 3.440(5) . 2_766 no
O12 C25 3.558(6) . 3_755 no
O21 C35 3.484(6) . 2_666 no
O22 C4 3.534(5) . 3_645 no
O22 C63 3.577(6) . 1_455 no
O22 C53 3.584(6) . 2_666 no
C12 C66 3.488(7) . 2_766 no
C13 C75 3.589(8) . 1_655 no
C26 C31 3.590(7) . 3_645 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 S1 P1 C1 . . . . 38.8(1) no
Pd1 S1 P1 C11 . . . . -79.2(1) no
Pd1 S1 P1 C21 . . . . 160.8(2) no
Pd1 O11 C32 C31 . . . . -176.8(3) no
Pd1 O11 C32 C33 . . . . 3.2(7) no
Pd1 O12 C34 C33 . . . . -1.9(7) no
Pd1 O12 C34 C35 . . . . 177.9(3) no
Pd1 C2 C1 P1 . . . . -0.5(4) no
Pd1 C2 C1 C6 . . . . 179.2(3) no
Pd1 C2 C3 C4 . . . . 179.5(3) no
Pd2 S2 P2 C41 . . . . 28.5(1) no
Pd2 S2 P2 C51 . . . . -91.1(2) no
Pd2 S2 P2 C61 . . . . 150.4(1) no
Pd2 O21 C72 C71 . . . . -172.9(3) no
Pd2 O21 C72 C73 . . . . 7.3(7) no
Pd2 O22 C74 C73 . . . . 8.8(7) no
Pd2 O22 C74 C75 . . . . -170.4(3) no
Pd2 C42 C41 P2 . . . . 1.2(4) no
Pd2 C42 C41 C46 . . . . -177.9(3) no
Pd2 C42 C43 C44 . . . . 175.9(3) no
S1 Pd1 O12 C34 . . . . -174.3(3) no
S1 Pd1 C2 C1 . . . . 25.0(3) no
S1 Pd1 C2 C3 . . . . -155.5(3) no
S1 P1 C1 C2 . . . . -29.5(3) no
S1 P1 C1 C6 . . . . 150.9(3) no
S1 P1 C11 C12 . . . . -54.6(4) no
S1 P1 C11 C16 . . . . 124.3(3) no
S1 P1 C21 C22 . . . . -37.4(4) no
S1 P1 C21 C26 . . . . 142.9(3) no
S2 Pd2 O22 C74 . . . . 176.6(4) no
S2 Pd2 C42 C41 . . . . 17.1(3) no
S2 Pd2 C42 C43 . . . . -159.4(3) no
S2 P2 C41 C42 . . . . -22.1(3) no
S2 P2 C41 C46 . . . . 156.9(3) no
S2 P2 C51 C52 . . . . -53.1(4) no
S2 P2 C51 C56 . . . . 125.8(3) no
S2 P2 C61 C62 . . . . -22.8(4) no
S2 P2 C61 C66 . . . . 157.2(3) no
P1 S1 Pd1 O12 . . . . 148.10(9) no
P1 S1 Pd1 C2 . . . . -33.5(1) no
P1 C1 C2 C3 . . . . -179.9(3) no
P1 C1 C6 C5 . . . . 179.7(3) no
P1 C11 C12 C13 . . . . 178.3(4) no
P1 C11 C16 C15 . . . . -179.7(4) no
P1 C21 C22 C23 . . . . -176.9(4) no
P1 C21 C26 C25 . . . . 176.8(4) no
P2 S2 Pd2 O22 . . . . 159.5(1) no
P2 S2 Pd2 C42 . . . . -24.3(1) no
P2 C41 C42 C43 . . . . 177.8(3) no
P2 C41 C46 C45 . . . . -177.3(3) no
P2 C51 C52 C53 . . . . 179.9(4) no
P2 C51 C56 C55 . . . . 180.0(3) no
P2 C61 C62 C63 . . . . 178.9(4) no
P2 C61 C66 C65 . . . . -179.4(4) no
O11 Pd1 O12 C34 . . . . 4.5(4) no
O11 Pd1 C2 C1 . . . . -153.7(3) no
O11 Pd1 C2 C3 . . . . 25.7(3) no
O11 C32 C33 C34 . . . . 1.4(9) no
O12 Pd1 O11 C32 . . . . -5.0(4) no
O12 C34 C33 C32 . . . . -2.1(9) no
O21 Pd2 O22 C74 . . . . -5.1(4) no
O21 Pd2 C42 C41 . . . . -161.3(3) no
O21 Pd2 C42 C43 . . . . 22.2(3) no
O21 C72 C73 C74 . . . . -5.0(9) no
O22 Pd2 O21 C72 . . . . -2.6(4) no
O22 C74 C73 C72 . . . . -4.4(9) no
C1 P1 C11 C12 . . . . -170.9(3) no
C1 P1 C11 C16 . . . . 8.1(4) no
C1 P1 C21 C22 . . . . 80.7(4) no
C1 P1 C21 C26 . . . . -99.0(4) no
C1 C2 C3 C4 . . . . -1.1(6) no
C1 C6 C5 C4 . . . . 1.4(7) no
C2 Pd1 O11 C32 . . . . 176.5(4) no
C2 C1 P1 C11 . . . . 91.1(3) no
C2 C1 P1 C21 . . . . -151.2(3) no
C2 C1 C6 C5 . . . . 0.1(6) no
C2 C3 C4 C5 . . . . 2.7(7) no
C3 C2 C1 C6 . . . . -0.3(6) no
C3 C4 C5 C6 . . . . -2.9(7) no
C6 C1 P1 C11 . . . . -88.5(4) no
C6 C1 P1 C21 . . . . 29.2(4) no
C11 P1 C21 C22 . . . . -160.7(4) no
C11 P1 C21 C26 . . . . 19.7(4) no
C11 C12 C13 C14 . . . . 1.6(8) no
C11 C16 C15 C14 . . . . 1.2(8) no
C12 C11 P1 C21 . . . . 68.1(4) no
C12 C11 C16 C15 . . . . -0.7(7) no
C12 C13 C14 C15 . . . . -1.1(8) no
C13 C12 C11 C16 . . . . -0.7(7) no
C13 C14 C15 C16 . . . . -0.3(8) no
C16 C11 P1 C21 . . . . -113.0(4) no
C21 C22 C23 C24 . . . . -1.0(8) no
C21 C26 C25 C24 . . . . 1.1(8) no
C22 C21 C26 C25 . . . . -2.8(7) no
C22 C23 C24 C25 . . . . -0.8(8) no
C23 C22 C21 C26 . . . . 2.7(7) no
C23 C24 C25 C26 . . . . 0.7(8) no
C31 C32 C33 C34 . . . . -178.5(5) no
C32 C33 C34 C35 . . . . 178.1(5) no
C41 P2 C51 C52 . . . . -170.4(3) no
C41 P2 C51 C56 . . . . 8.5(4) no
C41 P2 C61 C62 . . . . 94.8(4) no
C41 P2 C61 C66 . . . . -85.2(4) no
C41 C42 C43 C44 . . . . -0.8(6) no
C41 C46 C45 C44 . . . . -0.0(6) no
C42 Pd2 O21 C72 . . . . -178.8(4) no
C42 C41 P2 C51 . . . . 99.7(3) no
C42 C41 P2 C61 . . . . -142.5(3) no
C42 C41 C46 C45 . . . . 1.7(6) no
C42 C43 C44 C45 . . . . 2.5(7) no
C43 C42 C41 C46 . . . . -1.3(6) no
C43 C44 C45 C46 . . . . -2.1(7) no
C46 C41 P2 C51 . . . . -81.2(4) no
C46 C41 P2 C61 . . . . 36.6(4) no
C51 P2 C61 C62 . . . . -145.3(3) no
C51 P2 C61 C66 . . . . 34.6(4) no
C51 C52 C53 C54 . . . . -0.2(8) no
C51 C56 C55 C54 . . . . 0.7(7) no
C52 C51 P2 C61 . . . . 67.8(4) no
C52 C51 C56 C55 . . . . -1.1(6) no
C52 C53 C54 C55 . . . . -0.2(8) no
C53 C52 C51 C56 . . . . 0.9(7) no
C53 C54 C55 C56 . . . . 0.0(8) no
C56 C51 P2 C61 . . . . -113.3(4) no
C61 C62 C63 C64 . . . . 0.7(7) no
C61 C66 C65 C64 . . . . 0.2(7) no
C62 C61 C66 C65 . . . . 0.6(7) no
C62 C63 C64 C65 . . . . 0.1(8) no
C63 C62 C61 C66 . . . . -1.1(7) no
C63 C64 C65 C66 . . . . -0.5(8) no
C71 C72 C73 C74 . . . . 175.3(5) no
C72 C73 C74 C75 . . . . 174.8(5) no
_database_code_depnum_ccdc_archive 'CCDC 999164'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex11
_audit_creation_date             09-11-25
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title '11251436 ben0914'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-11-25- Report on C36 H29 Cl P2 Pd S 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-11-25- passes checkcif tests with minor warnings  
;

_cell_length_a                   9.1347(1)
_cell_length_b                   10.9341(2)
_cell_length_c                   15.6582(3)
_cell_angle_alpha                86.9669(9)
_cell_angle_beta                 84.7318(11)
_cell_angle_gamma                76.1404(11)
_cell_volume                     1511.22(4)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C36 H29 Cl1 P2 Pd1 S1 
# Dc =      1.53 Fooo =    708.00 Mu =      9.03 M =    697.49
# Found Formula = C36 H29 Cl1 P2 Pd1 S1 
# Dc =      1.53 FOOO =    708.00 Mu =      9.03 M =    697.49

_chemical_formula_sum            'C36 H29 Cl P2 Pd S'
_chemical_formula_moiety         'C36 H29 Cl P2 Pd S'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         697.49


_cell_measurement_reflns_used    51491
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.270

_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             708
_exptl_absorpt_coefficient_mu    0.903

# Sheldrick geometric approximatio 0.90 0.96 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.100
-1 0 0 0.170
0 1 0 0.040
0 -1 0 0.080
0 0 1 0.010
0 0 -1 0.040
1 -3 0 0.048


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.042

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.7 deg at rate 170 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 90 percent of data collected with 2-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            42023
_reflns_number_total             8844
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8844 
# Theoretical number of reflections is about 17726 


_diffrn_reflns_theta_min         2.555
_diffrn_reflns_theta_max         30.059
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        30.059
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   1.82
_oxford_diffrn_Wilson_scale      3.65

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.83
_refine_diff_density_max         0.70


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_number_parameters     370
_oxford_refine_ls_R_factor_ref   0.0342
_refine_ls_wR_factor_ref         0.0698
_refine_ls_goodness_of_fit_ref   1.0043
_refine_ls_shift/su_max          0.0013812
_refine_ls_shift/su_mean         7.1192336 # power of ten out?  obviously less


# The values computed from all data 
_oxford_reflns_number_all        8840
_refine_ls_R_factor_all          0.0342
_refine_ls_wR_factor_all         0.0698

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7938
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_gt          0.0673

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.20P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;

Hydrogen atoms were included at idealized positions
They were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.


;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.406627(14) 0.644689(11) 0.258832(8) 0.0212 1.0000 Uani . . . . . . .
Cl1 Cl 0.33182(6) 0.50629(4) 0.36660(3) 0.0340 1.0000 Uani . . . . . . .
S1 S 0.30463(5) 0.52908(4) 0.16359(3) 0.0283 1.0000 Uani . . . . . . .
P1 P 0.25352(5) 0.68456(4) 0.08909(3) 0.0230 1.0000 Uani . . . . . . .
P2 P 0.45986(5) 0.77431(4) 0.35529(3) 0.0211 1.0000 Uani . . . . . . .
C1 C 0.41729(19) 0.74822(16) 0.07801(11) 0.0250 1.0000 Uani . . . . . . .
C2 C 0.48679(19) 0.73912(16) 0.15614(11) 0.0244 1.0000 Uani . . . . . . .
C3 C 0.6148(2) 0.78863(18) 0.15342(12) 0.0289 1.0000 Uani . . . . . . .
C4 C 0.6701(2) 0.84236(19) 0.07849(13) 0.0337 1.0000 Uani . . . . . . .
C5 C 0.5990(2) 0.8505(2) 0.00305(13) 0.0357 1.0000 Uani . . . . . . .
C6 C 0.4702(2) 0.80381(19) 0.00299(12) 0.0321 1.0000 Uani . . . . . . .
C11 C 0.10387(19) 0.80696(16) 0.13776(11) 0.0242 1.0000 Uani . . . . . . .
C12 C 0.0263(2) 0.78499(19) 0.21562(12) 0.0306 1.0000 Uani . . . . . . .
C13 C -0.0838(2) 0.8831(2) 0.25332(14) 0.0369 1.0000 Uani . . . . . . .
C14 C -0.1165(2) 1.0006(2) 0.21361(14) 0.0369 1.0000 Uani . . . . . . .
C15 C -0.0384(2) 1.02298(18) 0.13626(13) 0.0338 1.0000 Uani . . . . . . .
C16 C 0.0720(2) 0.92655(18) 0.09849(12) 0.0292 1.0000 Uani . . . . . . .
C21 C 0.1899(2) 0.65403(17) -0.01156(11) 0.0267 1.0000 Uani . . . . . . .
C22 C 0.2927(2) 0.6094(2) -0.08052(14) 0.0411 1.0000 Uani . . . . . . .
C23 C 0.2399(3) 0.5809(3) -0.15553(16) 0.0528 1.0000 Uani . . . . . . .
C24 C 0.0867(3) 0.5939(2) -0.16177(15) 0.0491 1.0000 Uani . . . . . . .
C25 C -0.0152(3) 0.6344(2) -0.09248(14) 0.0383 1.0000 Uani . . . . . . .
C26 C 0.0357(2) 0.66540(18) -0.01740(13) 0.0305 1.0000 Uani . . . . . . .
C31 C 0.34184(19) 0.78372(16) 0.45694(11) 0.0238 1.0000 Uani . . . . . . .
C32 C 0.2275(2) 0.88946(19) 0.47857(13) 0.0324 1.0000 Uani . . . . . . .
C33 C 0.1399(2) 0.8906(2) 0.55647(14) 0.0415 1.0000 Uani . . . . . . .
C34 C 0.1642(2) 0.7867(2) 0.61189(13) 0.0391 1.0000 Uani . . . . . . .
C35 C 0.2804(3) 0.6827(2) 0.59172(13) 0.0379 1.0000 Uani . . . . . . .
C36 C 0.3695(2) 0.68121(18) 0.51514(12) 0.0311 1.0000 Uani . . . . . . .
C41 C 0.42535(19) 0.93906(15) 0.31799(11) 0.0233 1.0000 Uani . . . . . . .
C42 C 0.3009(2) 0.98508(17) 0.27031(13) 0.0308 1.0000 Uani . . . . . . .
C43 C 0.2594(3) 1.11173(19) 0.24604(14) 0.0373 1.0000 Uani . . . . . . .
C44 C 0.3428(3) 1.19396(19) 0.26834(15) 0.0406 1.0000 Uani . . . . . . .
C45 C 0.4677(3) 1.14887(19) 0.31444(15) 0.0387 1.0000 Uani . . . . . . .
C46 C 0.5096(2) 1.02237(18) 0.33948(13) 0.0303 1.0000 Uani . . . . . . .
C51 C 0.64947(18) 0.72874(16) 0.39228(11) 0.0240 1.0000 Uani . . . . . . .
C52 C 0.7607(2) 0.63635(17) 0.35066(12) 0.0275 1.0000 Uani . . . . . . .
C53 C 0.9049(2) 0.59940(18) 0.38002(13) 0.0323 1.0000 Uani . . . . . . .
C54 C 0.9383(2) 0.6551(2) 0.45068(14) 0.0355 1.0000 Uani . . . . . . .
C55 C 0.8279(2) 0.7454(2) 0.49364(13) 0.0363 1.0000 Uani . . . . . . .
C56 C 0.6837(2) 0.78235(19) 0.46521(12) 0.0307 1.0000 Uani . . . . . . .
H31 H 0.6665 0.7862 0.2032 0.0346 1.0000 Uiso R . . . . . .
H41 H 0.7549 0.8744 0.0795 0.0411 1.0000 Uiso R . . . . . .
H51 H 0.6355 0.8878 -0.0467 0.0434 1.0000 Uiso R . . . . . .
H61 H 0.4182 0.8097 -0.0461 0.0387 1.0000 Uiso R . . . . . .
H121 H 0.0490 0.7048 0.2419 0.0366 1.0000 Uiso R . . . . . .
H131 H -0.1339 0.8690 0.3056 0.0445 1.0000 Uiso R . . . . . .
H141 H -0.1953 1.0658 0.2378 0.0427 1.0000 Uiso R . . . . . .
H151 H -0.0603 1.1036 0.1113 0.0412 1.0000 Uiso R . . . . . .
H161 H 0.1230 0.9406 0.0477 0.0363 1.0000 Uiso R . . . . . .
H221 H 0.3959 0.5979 -0.0767 0.0490 1.0000 Uiso R . . . . . .
H231 H 0.3078 0.5554 -0.2018 0.0634 1.0000 Uiso R . . . . . .
H241 H 0.0530 0.5730 -0.2123 0.0589 1.0000 Uiso R . . . . . .
H251 H -0.1185 0.6406 -0.0953 0.0457 1.0000 Uiso R . . . . . .
H261 H -0.0340 0.6925 0.0294 0.0369 1.0000 Uiso R . . . . . .
H321 H 0.2101 0.9605 0.4411 0.0391 1.0000 Uiso R . . . . . .
H331 H 0.0651 0.9650 0.5718 0.0503 1.0000 Uiso R . . . . . .
H341 H 0.1047 0.7879 0.6642 0.0471 1.0000 Uiso R . . . . . .
H351 H 0.3004 0.6124 0.6308 0.0449 1.0000 Uiso R . . . . . .
H361 H 0.4483 0.6124 0.5017 0.0378 1.0000 Uiso R . . . . . .
H421 H 0.2457 0.9298 0.2546 0.0374 1.0000 Uiso R . . . . . .
H431 H 0.1744 1.1417 0.2152 0.0446 1.0000 Uiso R . . . . . .
H441 H 0.3140 1.2796 0.2535 0.0493 1.0000 Uiso R . . . . . .
H451 H 0.5233 1.2037 0.3292 0.0467 1.0000 Uiso R . . . . . .
H461 H 0.5915 0.9935 0.3714 0.0350 1.0000 Uiso R . . . . . .
H521 H 0.7370 0.5985 0.3025 0.0325 1.0000 Uiso R . . . . . .
H531 H 0.9791 0.5376 0.3510 0.0387 1.0000 Uiso R . . . . . .
H541 H 1.0366 0.6308 0.4695 0.0429 1.0000 Uiso R . . . . . .
H551 H 0.8497 0.7837 0.5420 0.0448 1.0000 Uiso R . . . . . .
H561 H 0.6075 0.8445 0.4952 0.0375 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.5557(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3703(5) yes
Pd1 . S1 . 2.3894(4) yes
Pd1 . P2 . 2.2842(4) yes
Pd1 . C2 . 2.0391(18) yes
S1 . P1 . 1.9947(6) yes
P1 . C1 . 1.7863(17) yes
P1 . C11 . 1.8113(18) yes
P1 . C21 . 1.8027(17) yes
P2 . C31 . 1.8318(18) yes
P2 . C41 . 1.8264(17) yes
P2 . C51 . 1.8232(17) yes
C1 . C2 . 1.417(2) yes
C1 . C6 . 1.394(3) yes
C2 . C3 . 1.398(2) yes
C3 . C4 . 1.392(3) yes
C3 . H31 . 0.944 no
C4 . C5 . 1.388(3) yes
C4 . H41 . 0.925 no
C5 . C6 . 1.390(3) yes
C5 . H51 . 0.931 no
C6 . H61 . 0.931 no
C11 . C12 . 1.392(3) yes
C11 . C16 . 1.392(3) yes
C12 . C13 . 1.397(3) yes
C12 . H121 . 0.933 no
C13 . C14 . 1.376(3) yes
C13 . H131 . 0.925 no
C14 . C15 . 1.389(3) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.388(3) yes
C15 . H151 . 0.929 no
C16 . H161 . 0.909 no
C21 . C22 . 1.392(3) yes
C21 . C26 . 1.395(3) yes
C22 . C23 . 1.387(3) yes
C22 . H221 . 0.928 no
C23 . C24 . 1.385(4) yes
C23 . H231 . 0.918 no
C24 . C25 . 1.381(3) yes
C24 . H241 . 0.933 no
C25 . C26 . 1.389(3) yes
C25 . H251 . 0.935 no
C26 . H261 . 0.937 no
C31 . C32 . 1.393(3) yes
C31 . C36 . 1.396(3) yes
C32 . C33 . 1.395(3) yes
C32 . H321 . 0.939 no
C33 . C34 . 1.380(3) yes
C33 . H331 . 0.954 no
C34 . C35 . 1.385(3) yes
C34 . H341 . 0.939 no
C35 . C36 . 1.384(3) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.926 no
C41 . C42 . 1.395(2) yes
C41 . C46 . 1.396(2) yes
C42 . C43 . 1.387(3) yes
C42 . H421 . 0.930 no
C43 . C44 . 1.386(3) yes
C43 . H431 . 0.935 no
C44 . C45 . 1.382(3) yes
C44 . H441 . 0.933 no
C45 . C46 . 1.389(3) yes
C45 . H451 . 0.924 no
C46 . H461 . 0.922 no
C51 . C52 . 1.390(2) yes
C51 . C56 . 1.403(2) yes
C52 . C53 . 1.395(2) yes
C52 . H521 . 0.944 no
C53 . C54 . 1.383(3) yes
C53 . H531 . 0.938 no
C54 . C55 . 1.383(3) yes
C54 . H541 . 0.944 no
C55 . C56 . 1.389(3) yes
C55 . H551 . 0.943 no
C56 . H561 . 0.956 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . S1 . 84.596(16) yes
Cl1 . Pd1 . P2 . 93.713(16) yes
S1 . Pd1 . P2 . 169.659(16) yes
Cl1 . Pd1 . C2 . 171.13(5) yes
S1 . Pd1 . C2 . 89.74(5) yes
P2 . Pd1 . C2 . 93.06(5) yes
Pd1 . S1 . P1 . 88.74(2) yes
S1 . P1 . C1 . 106.42(6) yes
S1 . P1 . C11 . 113.10(6) yes
C1 . P1 . C11 . 105.27(8) yes
S1 . P1 . C21 . 112.08(6) yes
C1 . P1 . C21 . 113.95(9) yes
C11 . P1 . C21 . 105.97(8) yes
Pd1 . P2 . C31 . 114.28(5) yes
Pd1 . P2 . C41 . 113.31(6) yes
C31 . P2 . C41 . 102.38(8) yes
Pd1 . P2 . C51 . 115.77(6) yes
C31 . P2 . C51 . 101.54(8) yes
C41 . P2 . C51 . 108.13(8) yes
P1 . C1 . C2 . 111.85(13) yes
P1 . C1 . C6 . 125.06(14) yes
C2 . C1 . C6 . 123.07(16) yes
C1 . C2 . Pd1 . 119.01(12) yes
C1 . C2 . C3 . 115.56(16) yes
Pd1 . C2 . C3 . 125.22(13) yes
C2 . C3 . C4 . 121.81(17) yes
C2 . C3 . H31 . 120.1 no
C4 . C3 . H31 . 118.0 no
C3 . C4 . C5 . 121.28(17) yes
C3 . C4 . H41 . 119.1 no
C5 . C4 . H41 . 119.6 no
C4 . C5 . C6 . 118.92(18) yes
C4 . C5 . H51 . 120.9 no
C6 . C5 . H51 . 120.1 no
C1 . C6 . C5 . 119.35(18) yes
C1 . C6 . H61 . 119.5 no
C5 . C6 . H61 . 121.2 no
P1 . C11 . C12 . 121.09(14) yes
P1 . C11 . C16 . 119.03(13) yes
C12 . C11 . C16 . 119.80(17) yes
C11 . C12 . C13 . 119.63(18) yes
C11 . C12 . H121 . 119.4 no
C13 . C12 . H121 . 121.0 no
C12 . C13 . C14 . 120.36(19) yes
C12 . C13 . H131 . 119.7 no
C14 . C13 . H131 . 119.9 no
C13 . C14 . C15 . 120.11(18) yes
C13 . C14 . H141 . 120.2 no
C15 . C14 . H141 . 119.7 no
C14 . C15 . C16 . 120.07(19) yes
C14 . C15 . H151 . 118.8 no
C16 . C15 . H151 . 121.2 no
C11 . C16 . C15 . 120.03(18) yes
C11 . C16 . H161 . 119.6 no
C15 . C16 . H161 . 120.4 no
P1 . C21 . C22 . 121.03(14) yes
P1 . C21 . C26 . 118.94(14) yes
C22 . C21 . C26 . 119.81(17) yes
C21 . C22 . C23 . 119.4(2) yes
C21 . C22 . H221 . 120.8 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 120.7(2) yes
C22 . C23 . H231 . 119.1 no
C24 . C23 . H231 . 120.2 no
C23 . C24 . C25 . 119.9(2) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 120.3 no
C24 . C25 . C26 . 120.0(2) yes
C24 . C25 . H251 . 120.7 no
C26 . C25 . H251 . 119.3 no
C21 . C26 . C25 . 120.05(19) yes
C21 . C26 . H261 . 120.4 no
C25 . C26 . H261 . 119.6 no
P2 . C31 . C32 . 122.55(14) yes
P2 . C31 . C36 . 118.39(13) yes
C32 . C31 . C36 . 119.06(17) yes
C31 . C32 . C33 . 120.01(19) yes
C31 . C32 . H321 . 120.1 no
C33 . C32 . H321 . 119.9 no
C32 . C33 . C34 . 120.4(2) yes
C32 . C33 . H331 . 119.3 no
C34 . C33 . H331 . 120.3 no
C33 . C34 . C35 . 119.81(19) yes
C33 . C34 . H341 . 120.0 no
C35 . C34 . H341 . 120.1 no
C34 . C35 . C36 . 120.3(2) yes
C34 . C35 . H351 . 120.1 no
C36 . C35 . H351 . 119.6 no
C31 . C36 . C35 . 120.40(18) yes
C31 . C36 . H361 . 118.9 no
C35 . C36 . H361 . 120.7 no
P2 . C41 . C42 . 117.30(13) yes
P2 . C41 . C46 . 123.78(14) yes
C42 . C41 . C46 . 118.77(16) yes
C41 . C42 . C43 . 120.76(17) yes
C41 . C42 . H421 . 119.3 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 120.07(19) yes
C42 . C43 . H431 . 119.9 no
C44 . C43 . H431 . 120.0 no
C43 . C44 . C45 . 119.60(19) yes
C43 . C44 . H441 . 120.6 no
C45 . C44 . H441 . 119.8 no
C44 . C45 . C46 . 120.72(18) yes
C44 . C45 . H451 . 119.6 no
C46 . C45 . H451 . 119.7 no
C41 . C46 . C45 . 120.06(18) yes
C41 . C46 . H461 . 119.7 no
C45 . C46 . H461 . 120.2 no
P2 . C51 . C52 . 120.36(13) yes
P2 . C51 . C56 . 120.61(13) yes
C52 . C51 . C56 . 118.98(16) yes
C51 . C52 . C53 . 120.45(17) yes
C51 . C52 . H521 . 119.1 no
C53 . C52 . H521 . 120.5 no
C52 . C53 . C54 . 120.02(18) yes
C52 . C53 . H531 . 119.5 no
C54 . C53 . H531 . 120.4 no
C53 . C54 . C55 . 120.11(17) yes
C53 . C54 . H541 . 119.6 no
C55 . C54 . H541 . 120.3 no
C54 . C55 . C56 . 120.30(18) yes
C54 . C55 . H551 . 120.6 no
C56 . C55 . H551 . 119.1 no
C51 . C56 . C55 . 120.12(18) yes
C51 . C56 . H561 . 119.8 no
C55 . C56 . H561 . 120.1 no



#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 C36 3.595(2) . 2_666 no
C5 C5 3.337(4) . 2_675 no
C12 C53 3.461(3) . 1_455 no
C13 C52 3.553(3) . 1_455 no
C33 C33 3.583(4) . 2_576 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 S1 P1 C1 . . . . 46.26(6) no
Pd1 S1 P1 C11 . . . . -68.84(7) no
Pd1 S1 P1 C21 . . . . 171.44(6) no
Pd1 P2 C31 C32 . . . . -106.8(2) no
Pd1 P2 C31 C36 . . . . 74.0(2) no
Pd1 P2 C41 C42 . . . . 36.9(1) no
Pd1 P2 C41 C46 . . . . -147.7(1) no
Pd1 P2 C51 C52 . . . . 12.4(2) no
Pd1 P2 C51 C56 . . . . -164.9(1) no
Pd1 C2 C1 P1 . . . . 5.9(2) no
Pd1 C2 C1 C6 . . . . -175.8(1) no
Pd1 C2 C3 C4 . . . . 174.3(1) no
Cl1 Pd1 S1 P1 . . . . 150.00(2) no
Cl1 Pd1 P2 C31 . . . . -31.39(6) no
Cl1 Pd1 P2 C41 . . . . -148.16(6) no
Cl1 Pd1 P2 C51 . . . . 86.10(7) no
S1 Pd1 P2 C31 . . . . 48.8(1) no
S1 Pd1 P2 C41 . . . . -68.0(1) no
S1 Pd1 P2 C51 . . . . 166.3(1) no
S1 Pd1 C2 C1 . . . . 23.4(1) no
S1 Pd1 C2 C3 . . . . -151.2(1) no
S1 P1 C1 C2 . . . . -40.1(1) no
S1 P1 C1 C6 . . . . 141.6(1) no
S1 P1 C11 C12 . . . . -5.9(2) no
S1 P1 C11 C16 . . . . 170.7(1) no
S1 P1 C21 C22 . . . . -84.0(2) no
S1 P1 C21 C26 . . . . 90.5(1) no
P1 S1 Pd1 P2 . . . . 69.0(1) no
P1 S1 Pd1 C2 . . . . -36.84(5) no
P1 C1 C2 C3 . . . . -179.1(1) no
P1 C1 C6 C5 . . . . 179.6(1) no
P1 C11 C12 C13 . . . . 177.1(2) no
P1 C11 C16 C15 . . . . -177.7(2) no
P1 C21 C22 C23 . . . . 176.7(2) no
P1 C21 C26 C25 . . . . -175.8(2) no
P2 Pd1 C2 C1 . . . . -146.7(1) no
P2 Pd1 C2 C3 . . . . 38.8(1) no
P2 C31 C32 C33 . . . . 179.2(2) no
P2 C31 C36 C35 . . . . -178.2(2) no
P2 C41 C42 C43 . . . . 174.4(2) no
P2 C41 C46 C45 . . . . -174.5(2) no
P2 C51 C52 C53 . . . . -178.6(1) no
P2 C51 C56 C55 . . . . 178.9(2) no
C1 P1 C11 C12 . . . . -121.7(2) no
C1 P1 C11 C16 . . . . 54.9(2) no
C1 P1 C21 C22 . . . . 36.9(2) no
C1 P1 C21 C26 . . . . -148.5(1) no
C1 C2 C3 C4 . . . . -0.4(2) no
C1 C6 C5 C4 . . . . -1.1(3) no
C2 Pd1 P2 C31 . . . . 154.35(7) no
C2 Pd1 P2 C41 . . . . 37.58(7) no
C2 Pd1 P2 C51 . . . . -88.17(8) no
C2 C1 P1 C11 . . . . 80.2(1) no
C2 C1 P1 C21 . . . . -164.2(1) no
C2 C1 C6 C5 . . . . 1.5(3) no
C2 C3 C4 C5 . . . . 0.8(3) no
C3 C2 C1 C6 . . . . -0.7(2) no
C3 C4 C5 C6 . . . . -0.0(3) no
C6 C1 P1 C11 . . . . -98.1(2) no
C6 C1 P1 C21 . . . . 17.5(2) no
C11 P1 C21 C22 . . . . 152.2(2) no
C11 P1 C21 C26 . . . . -33.3(2) no
C11 C12 C13 C14 . . . . 0.5(3) no
C11 C16 C15 C14 . . . . 0.5(3) no
C12 C11 P1 C21 . . . . 117.3(2) no
C12 C11 C16 C15 . . . . -1.0(3) no
C12 C13 C14 C15 . . . . -1.0(3) no
C13 C12 C11 C16 . . . . 0.5(3) no
C13 C14 C15 C16 . . . . 0.5(3) no
C16 C11 P1 C21 . . . . -66.1(2) no
C21 C22 C23 C24 . . . . -1.4(4) no
C21 C26 C25 C24 . . . . -0.9(3) no
C22 C21 C26 C25 . . . . -1.2(3) no
C22 C23 C24 C25 . . . . -0.7(4) no
C23 C22 C21 C26 . . . . 2.3(3) no
C23 C24 C25 C26 . . . . 1.8(3) no
C31 P2 C41 C42 . . . . -86.7(1) no
C31 P2 C41 C46 . . . . 88.7(2) no
C31 P2 C51 C52 . . . . 136.8(2) no
C31 P2 C51 C56 . . . . -40.5(2) no
C31 C32 C33 C34 . . . . -1.0(3) no
C31 C36 C35 C34 . . . . -0.9(4) no
C32 C31 P2 C41 . . . . 16.1(2) no
C32 C31 P2 C51 . . . . 127.8(2) no
C32 C31 C36 C35 . . . . 2.6(3) no
C32 C33 C34 C35 . . . . 2.7(3) no
C33 C32 C31 C36 . . . . -1.7(3) no
C33 C34 C35 C36 . . . . -1.8(4) no
C36 C31 P2 C41 . . . . -163.0(2) no
C36 C31 P2 C51 . . . . -51.3(2) no
C41 P2 C51 C52 . . . . -116.0(2) no
C41 P2 C51 C56 . . . . 66.7(2) no
C41 C42 C43 C44 . . . . 0.7(3) no
C41 C46 C45 C44 . . . . 0.1(3) no
C42 C41 P2 C51 . . . . 166.6(1) no
C42 C41 C46 C45 . . . . 0.9(3) no
C42 C43 C44 C45 . . . . 0.3(3) no
C43 C42 C41 C46 . . . . -1.3(3) no
C43 C44 C45 C46 . . . . -0.7(3) no
C46 C41 P2 C51 . . . . -18.0(2) no
C51 C52 C53 C54 . . . . -0.3(3) no
C51 C56 C55 C54 . . . . -0.4(3) no
C52 C51 C56 C55 . . . . 1.6(3) no
C52 C53 C54 C55 . . . . 1.5(3) no
C53 C52 C51 C56 . . . . -1.2(3) no
C53 C54 C55 C56 . . . . -1.2(3) no
_database_code_depnum_ccdc_archive 'CCDC 999165'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex12
_audit_creation_date             09-12-09
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2009-12-14 - Report on C55 H42 Cl3 O P3 Pd3 S3 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-12-14 - passes checkcif tests with minor warnings  
;


_oxford_structure_analysis_title '12080836 ben0913'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   19.7141(2)
_cell_length_b                   11.2461(1)
_cell_length_c                   24.1286(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.3879(4)
_cell_angle_gamma                90
_cell_volume                     5292.25(8)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C54 H42 Cl3 O1 P3 Pd3 S3 
# Dc =      1.66 Fooo =   2648.00 Mu =     14.07 M =   1321.60
# Found Formula = C55.00 H42 Cl3 O1.00 P3 Pd3 S3 
# Dc =      1.67 FOOO =   2648.00 Mu =     14.08 M =   1333.62

_chemical_formula_sum            'C55 H46 Cl3 O P3 Pd3 S3'
_chemical_formula_moiety         'C54 H42 Cl3  P3 Pd3 S3, C H4 O'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         1335.59 # 1333.62


_cell_measurement_reflns_used    183720
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.110
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.270

_exptl_crystal_density_diffrn    1.679 # 1.674 
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2664 # 2648 
_exptl_absorpt_coefficient_mu    1.408

# Sheldrick geometric approximatio 0.84 0.86 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.010
-1 0 0 0.100
0 1 0 0.130
0 -1 0 0.140
0 0 1 0.050
0 0 -1 0.070
6 -5 0 0.077
-1 1 2 0.112


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.041

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.0 deg at rate 90 sec/frame,
crystal-detector distance 35mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            122273
_reflns_number_total             15457
_diffrn_reflns_av_R_equivalents  0.061
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 15457 
# Theoretical number of reflections is about 31002 


_diffrn_reflns_theta_min         2.601
_diffrn_reflns_theta_max         30.046
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        30.046
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_reflns_limit_h_min              -27
_reflns_limit_h_max              27
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              33

_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      26.54

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.81
_refine_diff_density_max         1.50


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         15457
_refine_ls_number_restraints     16
_refine_ls_number_parameters     632
_oxford_refine_ls_R_factor_ref   0.0416
_refine_ls_wR_factor_ref         0.0767
_refine_ls_goodness_of_fit_ref   1.0064
_refine_ls_shift/su_max          0.0481808
_refine_ls_shift/su_mean         0.8881751


# The values computed from all data 
_oxford_reflns_number_all        15457
_refine_ls_R_factor_all          0.0416
_refine_ls_wR_factor_all         0.0767

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                13010
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_gt          0.0720

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 8.39P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
Besides the organometallic species, there is also some solvate
of crystallization within the structure.   
There are two sites, about 1.5Å apart, which have been interpreted
as being a methanol molecule.  
Best agreement with the observed electron density is obtained
if each atom is assumed to be disordered over two sites,
corresponding to two orientations of the molecule.
Restraints were imposed on the bond lengths 
and displacement parameters while the
 relative occupancies were refined.

Hydrogen atoms were included at idealized positions
and ride on the atom to which they are bonded.
The hydrogen atoms of the disordered methanol molecule 
have not been included.


;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.677454(9) 0.742314(16) 0.695359(7) 0.0242 1.0000 Uani . . . . . . .
Pd2 Pd 0.799264(9) 0.572088(16) 0.621021(7) 0.0250 1.0000 Uani . . . . . . .
Pd3 Pd 0.777797(10) 0.527224(16) 0.770247(7) 0.0266 1.0000 Uani . . . . . . .
Cl1 Cl 0.62402(3) 0.73284(7) 0.77489(3) 0.0390 1.0000 Uani . . . . . . .
Cl2 Cl 0.87141(4) 0.66787(6) 0.56665(3) 0.0412 1.0000 Uani . . . . . . .
Cl3 Cl 0.76963(5) 0.33490(6) 0.80449(3) 0.0481 1.0000 Uani . . . . . . .
S1 S 0.73063(3) 0.74958(5) 0.61757(2) 0.0266 1.0000 Uani . . . . . . .
S2 S 0.73043(3) 0.47436(5) 0.67463(2) 0.0267 1.0000 Uani . . . . . . .
S3 S 0.79029(3) 0.72180(5) 0.74498(2) 0.0261 1.0000 Uani . . . . . . .
P1 P 0.57900(3) 0.75450(6) 0.63676(3) 0.0281 1.0000 Uani . . . . . . .
P2 P 0.85982(3) 0.40369(6) 0.62318(3) 0.0297 1.0000 Uani . . . . . . .
P3 P 0.81801(3) 0.58611(6) 0.85717(3) 0.0287 1.0000 Uani . . . . . . .
O91 O 0.6482(8) 0.3708(10) 0.5351(5) 0.1156 0.507(10) Uani D U P . . . .
O92 O 0.6001(3) 0.3856(7) 0.5610(3) 0.0842 0.493(10) Uani D U P . . . .
C1 C 0.59722(14) 0.7084(2) 0.56854(10) 0.0316 1.0000 Uani . . . . . . .
C2 C 0.66571(14) 0.7123(2) 0.56041(10) 0.0311 1.0000 Uani . . . . . . .
C3 C 0.68385(17) 0.6885(3) 0.50798(11) 0.0427 1.0000 Uani . . . . . . .
C4 C 0.63345(19) 0.6540(3) 0.46484(12) 0.0533 1.0000 Uani . . . . . . .
C5 C 0.56590(18) 0.6437(3) 0.47320(13) 0.0501 1.0000 Uani . . . . . . .
C6 C 0.54725(16) 0.6726(3) 0.52459(12) 0.0425 1.0000 Uani . . . . . . .
C11 C 0.50618(13) 0.6688(3) 0.65122(11) 0.0338 1.0000 Uani . . . . . . .
C12 C 0.51646(15) 0.5487(3) 0.66451(12) 0.0384 1.0000 Uani . . . . . . .
C13 C 0.46220(17) 0.4788(3) 0.67454(13) 0.0451 1.0000 Uani . . . . . . .
C14 C 0.39758(18) 0.5266(3) 0.67219(15) 0.0543 1.0000 Uani . . . . . . .
C15 C 0.38679(18) 0.6446(4) 0.6595(2) 0.0702 1.0000 Uani . . . . . . .
C16 C 0.44106(16) 0.7164(3) 0.64893(18) 0.0573 1.0000 Uani . . . . . . .
C21 C 0.55149(13) 0.9082(2) 0.62996(11) 0.0319 1.0000 Uani . . . . . . .
C22 C 0.53662(17) 0.9654(3) 0.67765(13) 0.0448 1.0000 Uani . . . . . . .
C23 C 0.5187(2) 1.0848(3) 0.67571(15) 0.0556 1.0000 Uani . . . . . . .
C24 C 0.5173(2) 1.1470(3) 0.62692(16) 0.0592 1.0000 Uani . . . . . . .
C25 C 0.5332(2) 1.0914(3) 0.57928(15) 0.0564 1.0000 Uani . . . . . . .
C26 C 0.54965(16) 0.9710(3) 0.58037(12) 0.0410 1.0000 Uani . . . . . . .
C31 C 0.80726(14) 0.2855(2) 0.64512(10) 0.0305 1.0000 Uani . . . . . . .
C32 C 0.74921(13) 0.3204(2) 0.66758(10) 0.0300 1.0000 Uani . . . . . . .
C33 C 0.70429(16) 0.2355(3) 0.68326(12) 0.0384 1.0000 Uani . . . . . . .
C34 C 0.71785(17) 0.1159(3) 0.67659(12) 0.0424 1.0000 Uani . . . . . . .
C35 C 0.77596(18) 0.0802(2) 0.65556(12) 0.0430 1.0000 Uani . . . . . . .
C36 C 0.82079(16) 0.1639(2) 0.63934(12) 0.0382 1.0000 Uani . . . . . . .
C41 C 0.88331(17) 0.3570(2) 0.55640(12) 0.0406 1.0000 Uani . . . . . . .
C42 C 0.8346(2) 0.3035(3) 0.51707(13) 0.0504 1.0000 Uani . . . . . . .
C43 C 0.8505(3) 0.2758(3) 0.46386(15) 0.0694 1.0000 Uani . . . . . . .
C44 C 0.9145(3) 0.3016(4) 0.45134(18) 0.0843 1.0000 Uani . . . . . . .
C45 C 0.9631(3) 0.3530(4) 0.4903(2) 0.0773 1.0000 Uani . . . . . . .
C46 C 0.9482(2) 0.3824(3) 0.54324(17) 0.0565 1.0000 Uani . . . . . . .
C51 C 0.93848(14) 0.4101(3) 0.67206(12) 0.0383 1.0000 Uani . . . . . . .
C52 C 0.9657(2) 0.5169(4) 0.6900(2) 0.0778 1.0000 Uani . . . . . . .
C53 C 1.0274(2) 0.5224(5) 0.7264(2) 0.0961 1.0000 Uani . . . . . . .
C54 C 1.05990(19) 0.4198(4) 0.74549(18) 0.0698 1.0000 Uani . . . . . . .
C55 C 1.03415(19) 0.3126(4) 0.7261(2) 0.0737 1.0000 Uani . . . . . . .
C56 C 0.97367(18) 0.3077(4) 0.6897(2) 0.0695 1.0000 Uani . . . . . . .
C61 C 0.81212(13) 0.7467(2) 0.85968(10) 0.0292 1.0000 Uani . . . . . . .
C62 C 0.79687(12) 0.8049(2) 0.80849(10) 0.0278 1.0000 Uani . . . . . . .
C63 C 0.79001(15) 0.9281(2) 0.80679(12) 0.0367 1.0000 Uani . . . . . . .
C64 C 0.79848(16) 0.9928(3) 0.85627(13) 0.0410 1.0000 Uani . . . . . . .
C65 C 0.81328(17) 0.9351(3) 0.90739(13) 0.0422 1.0000 Uani . . . . . . .
C66 C 0.81985(15) 0.8128(3) 0.90938(11) 0.0367 1.0000 Uani . . . . . . .
C71 C 0.76931(14) 0.5382(2) 0.91137(11) 0.0330 1.0000 Uani . . . . . . .
C72 C 0.69883(17) 0.5296(3) 0.89859(15) 0.0527 1.0000 Uani . . . . . . .
C73 C 0.6603(2) 0.4997(4) 0.94024(19) 0.0678 1.0000 Uani . . . . . . .
C74 C 0.6920(2) 0.4805(3) 0.99432(17) 0.0635 1.0000 Uani . . . . . . .
C75 C 0.7615(2) 0.4921(4) 1.00697(15) 0.0679 1.0000 Uani . . . . . . .
C76 C 0.80048(18) 0.5192(4) 0.96563(13) 0.0534 1.0000 Uani . . . . . . .
C81 C 0.90708(14) 0.5444(2) 0.87869(11) 0.0337 1.0000 Uani . . . . . . .
C82 C 0.93260(17) 0.4438(3) 0.85539(14) 0.0480 1.0000 Uani . . . . . . .
C83 C 0.99931(18) 0.4057(3) 0.87338(16) 0.0543 1.0000 Uani . . . . . . .
C84 C 1.04087(16) 0.4676(3) 0.91413(15) 0.0476 1.0000 Uani . . . . . . .
C85 C 1.01738(17) 0.5685(3) 0.93619(16) 0.0517 1.0000 Uani . . . . . . .
C86 C 0.95084(16) 0.6077(3) 0.91819(14) 0.0466 1.0000 Uani . . . . . . .
C91 C 0.6356(8) 0.3311(14) 0.4790(6) 0.1506 0.507(10) Uani D U P . . . .
C92 C 0.6441(12) 0.319(2) 0.5309(12) 0.1709 0.493(10) Uani D U P . . . .
H31 H 0.7302 0.6958 0.5018 0.0513 1.0000 Uiso R . . . . . .
H41 H 0.6456 0.6373 0.4289 0.0640 1.0000 Uiso R . . . . . .
H51 H 0.5323 0.6166 0.4437 0.0601 1.0000 Uiso R . . . . . .
H61 H 0.5005 0.6681 0.5300 0.0510 1.0000 Uiso R . . . . . .
H121 H 0.5610 0.5151 0.6666 0.0461 1.0000 Uiso R . . . . . .
H131 H 0.4694 0.3969 0.6831 0.0541 1.0000 Uiso R . . . . . .
H141 H 0.3605 0.4779 0.6794 0.0652 1.0000 Uiso R . . . . . .
H151 H 0.3422 0.6775 0.6579 0.0843 1.0000 Uiso R . . . . . .
H161 H 0.4334 0.7980 0.6401 0.0688 1.0000 Uiso R . . . . . .
H221 H 0.5387 0.9226 0.7118 0.0537 1.0000 Uiso R . . . . . .
H231 H 0.5075 1.1232 0.7083 0.0668 1.0000 Uiso R . . . . . .
H241 H 0.5052 1.2288 0.6257 0.0710 1.0000 Uiso R . . . . . .
H251 H 0.5329 1.1356 0.5457 0.0677 1.0000 Uiso R . . . . . .
H261 H 0.5595 0.9322 0.5475 0.0492 1.0000 Uiso R . . . . . .
H331 H 0.6646 0.2594 0.6984 0.0461 1.0000 Uiso R . . . . . .
H341 H 0.6868 0.0578 0.6866 0.0509 1.0000 Uiso R . . . . . .
H351 H 0.7853 -0.0021 0.6522 0.0516 1.0000 Uiso R . . . . . .
H361 H 0.8605 0.1392 0.6244 0.0459 1.0000 Uiso R . . . . . .
H421 H 0.7904 0.2856 0.5262 0.0605 1.0000 Uiso R . . . . . .
H431 H 0.8172 0.2395 0.4367 0.0833 1.0000 Uiso R . . . . . .
H441 H 0.9252 0.2836 0.4152 0.1011 1.0000 Uiso R . . . . . .
H451 H 1.0074 0.3687 0.4811 0.0928 1.0000 Uiso R . . . . . .
H461 H 0.9818 0.4193 0.5700 0.0678 1.0000 Uiso R . . . . . .
H521 H 0.9424 0.5882 0.6777 0.0933 1.0000 Uiso R . . . . . .
H531 H 1.0469 0.5973 0.7378 0.1153 1.0000 Uiso R . . . . . .
H541 H 1.1003 0.4232 0.7722 0.0838 1.0000 Uiso R . . . . . .
H551 H 1.0580 0.2414 0.7378 0.0885 1.0000 Uiso R . . . . . .
H561 H 0.9559 0.2327 0.6765 0.0834 1.0000 Uiso R . . . . . .
H631 H 0.7796 0.9678 0.7718 0.0440 1.0000 Uiso R . . . . . .
H641 H 0.7941 1.0769 0.8551 0.0492 1.0000 Uiso R . . . . . .
H651 H 0.8189 0.9798 0.9412 0.0507 1.0000 Uiso R . . . . . .
H661 H 0.8296 0.7736 0.9445 0.0440 1.0000 Uiso R . . . . . .
H721 H 0.6769 0.5442 0.8615 0.0632 1.0000 Uiso R . . . . . .
H731 H 0.6119 0.4923 0.9315 0.0814 1.0000 Uiso R . . . . . .
H741 H 0.6656 0.4593 1.0227 0.0762 1.0000 Uiso R . . . . . .
H751 H 0.7831 0.4813 1.0445 0.0815 1.0000 Uiso R . . . . . .
H761 H 0.8489 0.5249 0.9745 0.0641 1.0000 Uiso R . . . . . .
H821 H 0.9043 0.4008 0.8270 0.0575 1.0000 Uiso R . . . . . .
H831 H 1.0162 0.3365 0.8574 0.0652 1.0000 Uiso R . . . . . .
H841 H 1.0860 0.4400 0.9269 0.0571 1.0000 Uiso R . . . . . .
H851 H 1.0464 0.6121 0.9639 0.0620 1.0000 Uiso R . . . . . .
H861 H 0.9352 0.6790 0.9332 0.0559 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.20131(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3223(6) yes
Pd1 . S1 . 2.2809(6) yes
Pd1 . S3 . 2.3786(6) yes
Pd1 . P1 . 2.2327(7) yes
Pd2 . Cl2 . 2.3342(7) yes
Pd2 . S1 . 2.4060(6) yes
Pd2 . S2 . 2.2880(6) yes
Pd2 . P2 . 2.2353(7) yes
Pd3 . Cl3 . 2.3293(7) yes
Pd3 . S2 . 2.4330(6) yes
Pd3 . S3 . 2.2945(6) yes
Pd3 . P3 . 2.2317(7) yes
S1 . C2 . 1.789(3) yes
S2 . C32 . 1.784(3) yes
S3 . C62 . 1.784(2) yes
P1 . C1 . 1.811(3) yes
P1 . C11 . 1.805(3) yes
P1 . C21 . 1.812(3) yes
P2 . C31 . 1.812(3) yes
P2 . C41 . 1.818(3) yes
P2 . C51 . 1.808(3) yes
P3 . C61 . 1.811(3) yes
P3 . C71 . 1.814(3) yes
P3 . C81 . 1.819(3) yes
O91 . C91 . 1.413(13) yes
O92 . C92 . 1.426(16) yes
C1 . C2 . 1.393(4) yes
C1 . C6 . 1.397(4) yes
C2 . C3 . 1.390(4) yes
C3 . C4 . 1.385(4) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.380(5) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.383(4) yes
C5 . H51 . 0.950 no
C6 . H61 . 0.950 no
C11 . C12 . 1.397(4) yes
C11 . C16 . 1.384(4) yes
C12 . C13 . 1.377(4) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.376(5) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.371(6) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.393(5) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.386(4) yes
C21 . C26 . 1.385(4) yes
C22 . C23 . 1.388(4) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.366(5) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.384(5) yes
C24 . H241 . 0.950 no
C25 . C26 . 1.392(4) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . C32 . 1.392(4) yes
C31 . C36 . 1.403(4) yes
C32 . C33 . 1.392(4) yes
C33 . C34 . 1.386(4) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.378(5) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.386(4) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.950 no
C41 . C42 . 1.386(5) yes
C41 . C46 . 1.391(5) yes
C42 . C43 . 1.400(5) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.370(7) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.368(7) yes
C44 . H441 . 0.950 no
C45 . C46 . 1.392(5) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.950 no
C51 . C52 . 1.359(5) yes
C51 . C56 . 1.380(5) yes
C52 . C53 . 1.395(6) yes
C52 . H521 . 0.950 no
C53 . C54 . 1.366(6) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.364(6) yes
C54 . H541 . 0.950 no
C55 . C56 . 1.375(5) yes
C55 . H551 . 0.950 no
C56 . H561 . 0.950 no
C61 . C62 . 1.392(3) yes
C61 . C66 . 1.401(4) yes
C62 . C63 . 1.392(4) yes
C63 . C64 . 1.387(4) yes
C63 . H631 . 0.950 no
C64 . C65 . 1.387(4) yes
C64 . H641 . 0.950 no
C65 . C66 . 1.381(4) yes
C65 . H651 . 0.950 no
C66 . H661 . 0.950 no
C71 . C72 . 1.382(4) yes
C71 . C76 . 1.379(4) yes
C72 . C73 . 1.387(5) yes
C72 . H721 . 0.950 no
C73 . C74 . 1.380(6) yes
C73 . H731 . 0.950 no
C74 . C75 . 1.365(6) yes
C74 . H741 . 0.950 no
C75 . C76 . 1.379(5) yes
C75 . H751 . 0.950 no
C76 . H761 . 0.950 no
C81 . C82 . 1.389(4) yes
C81 . C86 . 1.386(4) yes
C82 . C83 . 1.391(5) yes
C82 . H821 . 0.950 no
C83 . C84 . 1.374(5) yes
C83 . H831 . 0.950 no
C84 . C85 . 1.363(5) yes
C84 . H841 . 0.950 no
C85 . C86 . 1.392(4) yes
C85 . H851 . 0.950 no
C86 . H861 . 0.950 no
C91 . C92 . 1.25(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . S1 . 179.31(2) yes
Cl1 . Pd1 . S3 . 94.78(2) yes
S1 . Pd1 . S3 . 84.79(2) yes
Cl1 . Pd1 . P1 . 93.95(2) yes
S1 . Pd1 . P1 . 86.46(2) yes
S3 . Pd1 . P1 . 170.93(2) yes
Cl2 . Pd2 . S1 . 89.05(2) yes
Cl2 . Pd2 . S2 . 178.58(2) yes
S1 . Pd2 . S2 . 92.36(2) yes
Cl2 . Pd2 . P2 . 92.12(3) yes
S1 . Pd2 . P2 . 178.06(2) yes
S2 . Pd2 . P2 . 86.48(2) yes
Cl3 . Pd3 . S2 . 94.17(2) yes
Cl3 . Pd3 . S3 . 174.56(2) yes
S2 . Pd3 . S3 . 91.28(2) yes
Cl3 . Pd3 . P3 . 88.60(3) yes
S2 . Pd3 . P3 . 176.58(2) yes
S3 . Pd3 . P3 . 85.96(2) yes
Pd2 . S1 . Pd1 . 105.40(2) yes
Pd2 . S1 . C2 . 99.64(8) yes
Pd1 . S1 . C2 . 105.25(9) yes
Pd3 . S2 . Pd2 . 103.97(2) yes
Pd3 . S2 . C32 . 105.75(8) yes
Pd2 . S2 . C32 . 105.30(9) yes
Pd1 . S3 . Pd3 . 95.59(2) yes
Pd1 . S3 . C62 . 109.09(8) yes
Pd3 . S3 . C62 . 105.59(8) yes
Pd1 . P1 . C1 . 106.77(9) yes
Pd1 . P1 . C11 . 119.16(9) yes
C1 . P1 . C11 . 106.95(13) yes
Pd1 . P1 . C21 . 109.69(9) yes
C1 . P1 . C21 . 106.71(12) yes
C11 . P1 . C21 . 106.92(12) yes
Pd2 . P2 . C31 . 107.60(9) yes
Pd2 . P2 . C41 . 115.36(9) yes
C31 . P2 . C41 . 106.12(13) yes
Pd2 . P2 . C51 . 112.68(10) yes
C31 . P2 . C51 . 108.16(13) yes
C41 . P2 . C51 . 106.55(14) yes
Pd3 . P3 . C61 . 108.16(8) yes
Pd3 . P3 . C71 . 115.89(9) yes
C61 . P3 . C71 . 103.24(12) yes
Pd3 . P3 . C81 . 112.80(9) yes
C61 . P3 . C81 . 108.17(12) yes
C71 . P3 . C81 . 107.93(12) yes
P1 . C1 . C2 . 116.34(19) yes
P1 . C1 . C6 . 124.1(2) yes
C2 . C1 . C6 . 119.5(2) yes
S1 . C2 . C1 . 119.86(19) yes
S1 . C2 . C3 . 119.8(2) yes
C1 . C2 . C3 . 120.4(3) yes
C2 . C3 . C4 . 119.1(3) yes
C2 . C3 . H31 . 120.5 no
C4 . C3 . H31 . 120.5 no
C3 . C4 . C5 . 121.0(3) yes
C3 . C4 . H41 . 119.5 no
C5 . C4 . H41 . 119.5 no
C4 . C5 . C6 . 120.0(3) yes
C4 . C5 . H51 . 120.0 no
C6 . C5 . H51 . 120.0 no
C1 . C6 . C5 . 119.9(3) yes
C1 . C6 . H61 . 120.1 no
C5 . C6 . H61 . 120.1 no
P1 . C11 . C12 . 117.9(2) yes
P1 . C11 . C16 . 123.0(2) yes
C12 . C11 . C16 . 119.0(3) yes
C11 . C12 . C13 . 120.2(3) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C14 . 120.5(3) yes
C12 . C13 . H131 . 119.7 no
C14 . C13 . H131 . 119.7 no
C13 . C14 . C15 . 120.0(3) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 120.2(3) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 119.9 no
C15 . C16 . C11 . 120.1(3) yes
C15 . C16 . H161 . 120.0 no
C11 . C16 . H161 . 120.0 no
P1 . C21 . C22 . 117.6(2) yes
P1 . C21 . C26 . 122.3(2) yes
C22 . C21 . C26 . 119.9(3) yes
C21 . C22 . C23 . 120.3(3) yes
C21 . C22 . H221 . 119.9 no
C23 . C22 . H221 . 119.9 no
C22 . C23 . C24 . 119.8(3) yes
C22 . C23 . H231 . 120.1 no
C24 . C23 . H231 . 120.1 no
C23 . C24 . C25 . 120.4(3) yes
C23 . C24 . H241 . 119.8 no
C25 . C24 . H241 . 119.8 no
C24 . C25 . C26 . 120.3(3) yes
C24 . C25 . H251 . 119.9 no
C26 . C25 . H251 . 119.9 no
C25 . C26 . C21 . 119.2(3) yes
C25 . C26 . H261 . 120.4 no
C21 . C26 . H261 . 120.4 no
P2 . C31 . C32 . 116.37(19) yes
P2 . C31 . C36 . 124.1(2) yes
C32 . C31 . C36 . 119.5(2) yes
S2 . C32 . C31 . 120.33(19) yes
S2 . C32 . C33 . 119.4(2) yes
C31 . C32 . C33 . 120.2(2) yes
C32 . C33 . C34 . 119.6(3) yes
C32 . C33 . H331 . 120.2 no
C34 . C33 . H331 . 120.2 no
C33 . C34 . C35 . 120.6(3) yes
C33 . C34 . H341 . 119.7 no
C35 . C34 . H341 . 119.7 no
C34 . C35 . C36 . 120.3(3) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 119.8 no
C31 . C36 . C35 . 119.7(3) yes
C31 . C36 . H361 . 120.2 no
C35 . C36 . H361 . 120.2 no
P2 . C41 . C42 . 119.4(2) yes
P2 . C41 . C46 . 120.3(3) yes
C42 . C41 . C46 . 120.1(3) yes
C41 . C42 . C43 . 119.9(4) yes
C41 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 119.4(4) yes
C42 . C43 . H431 . 120.3 no
C44 . C43 . H431 . 120.3 no
C43 . C44 . C45 . 120.9(4) yes
C43 . C44 . H441 . 119.6 no
C45 . C44 . H441 . 119.6 no
C44 . C45 . C46 . 120.7(4) yes
C44 . C45 . H451 . 119.7 no
C46 . C45 . H451 . 119.7 no
C45 . C46 . C41 . 119.0(4) yes
C45 . C46 . H461 . 120.5 no
C41 . C46 . H461 . 120.5 no
P2 . C51 . C52 . 120.3(2) yes
P2 . C51 . C56 . 120.8(3) yes
C52 . C51 . C56 . 118.8(3) yes
C51 . C52 . C53 . 120.5(4) yes
C51 . C52 . H521 . 119.7 no
C53 . C52 . H521 . 119.7 no
C52 . C53 . C54 . 119.8(4) yes
C52 . C53 . H531 . 120.1 no
C54 . C53 . H531 . 120.1 no
C53 . C54 . C55 . 119.9(4) yes
C53 . C54 . H541 . 120.1 no
C55 . C54 . H541 . 120.1 no
C54 . C55 . C56 . 120.0(4) yes
C54 . C55 . H551 . 120.0 no
C56 . C55 . H551 . 120.0 no
C51 . C56 . C55 . 120.9(4) yes
C51 . C56 . H561 . 119.6 no
C55 . C56 . H561 . 119.6 no
P3 . C61 . C62 . 116.52(19) yes
P3 . C61 . C66 . 124.0(2) yes
C62 . C61 . C66 . 119.5(2) yes
S3 . C62 . C61 . 119.65(19) yes
S3 . C62 . C63 . 120.1(2) yes
C61 . C62 . C63 . 120.2(2) yes
C62 . C63 . C64 . 119.8(3) yes
C62 . C63 . H631 . 120.1 no
C64 . C63 . H631 . 120.1 no
C63 . C64 . C65 . 120.2(3) yes
C63 . C64 . H641 . 119.9 no
C65 . C64 . H641 . 119.9 no
C64 . C65 . C66 . 120.2(3) yes
C64 . C65 . H651 . 119.9 no
C66 . C65 . H651 . 119.9 no
C61 . C66 . C65 . 120.1(3) yes
C61 . C66 . H661 . 120.0 no
C65 . C66 . H661 . 120.0 no
P3 . C71 . C72 . 118.7(2) yes
P3 . C71 . C76 . 121.4(2) yes
C72 . C71 . C76 . 119.7(3) yes
C71 . C72 . C73 . 119.7(3) yes
C71 . C72 . H721 . 120.2 no
C73 . C72 . H721 . 120.2 no
C72 . C73 . C74 . 120.1(4) yes
C72 . C73 . H731 . 119.9 no
C74 . C73 . H731 . 119.9 no
C73 . C74 . C75 . 119.9(3) yes
C73 . C74 . H741 . 120.0 no
C75 . C74 . H741 . 120.0 no
C74 . C75 . C76 . 120.4(3) yes
C74 . C75 . H751 . 119.8 no
C76 . C75 . H751 . 119.8 no
C75 . C76 . C71 . 120.2(3) yes
C75 . C76 . H761 . 119.9 no
C71 . C76 . H761 . 119.9 no
P3 . C81 . C82 . 119.1(2) yes
P3 . C81 . C86 . 122.8(2) yes
C82 . C81 . C86 . 118.1(3) yes
C81 . C82 . C83 . 120.4(3) yes
C81 . C82 . H821 . 119.8 no
C83 . C82 . H821 . 119.8 no
C82 . C83 . C84 . 120.3(3) yes
C82 . C83 . H831 . 119.8 no
C84 . C83 . H831 . 119.8 no
C83 . C84 . C85 . 120.0(3) yes
C83 . C84 . H841 . 120.0 no
C85 . C84 . H841 . 120.0 no
C84 . C85 . C86 . 120.0(3) yes
C84 . C85 . H851 . 120.0 no
C86 . C85 . H851 . 120.0 no
C85 . C86 . C81 . 121.0(3) yes
C85 . C86 . H861 . 119.5 no
C81 . C86 . H861 . 119.5 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 C13 3.555(4) . 3_656 no
Cl1 C14 3.589(4) . 3_656 no
S3 C55 3.578(4) . 3_756 no
O91 C32 3.56(1) . . no
O91 C4 3.60(1) . . no
O92 C5 3.273(7) . 2_666 no
O92 C6 3.374(7) . 2_666 no
O92 C6 3.465(8) . . no
O92 C5 3.599(8) . . no
C5 C24 3.593(5) . 2_676 no
C6 C91 3.59(2) . 2_666 no
C13 C22 3.566(4) . 3_646 no
C15 C91 3.32(2) . 2_666 no
C16 C91 3.28(1) . 2_666 no
C43 C76 3.463(6) . 4_554 no
C43 C65 3.560(5) . 4_564 no
C44 C83 3.562(6) . 4_554 no
C54 C63 3.383(5) . 3_746 no
C54 C62 3.523(5) . 3_746 no
C55 C62 3.551(5) . 3_746 no
C85 C85 3.597(8) . 2_767 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 S1 Pd2 Cl2 . . . . -155.09(3) no
Pd1 S1 Pd2 S2 . . . . 24.72(2) no
Pd1 S1 C2 C1 . . . . 11.8(2) no
Pd1 S1 C2 C3 . . . . -168.9(2) no
Pd1 S3 Pd3 S2 . . . . 48.66(2) no
Pd1 S3 Pd3 P3 . . . . -129.32(2) no
Pd1 S3 C62 C61 . . . . 118.8(2) no
Pd1 S3 C62 C63 . . . . -64.2(2) no
Pd1 P1 C1 C2 . . . . -19.7(2) no
Pd1 P1 C1 C6 . . . . 161.7(2) no
Pd1 P1 C11 C12 . . . . -48.0(3) no
Pd1 P1 C11 C16 . . . . 132.9(3) no
Pd1 P1 C21 C22 . . . . -62.6(2) no
Pd1 P1 C21 C26 . . . . 112.8(2) no
Pd2 S1 Pd1 S3 . . . . 54.78(2) no
Pd2 S1 Pd1 P1 . . . . -122.84(3) no
Pd2 S1 C2 C1 . . . . 120.8(2) no
Pd2 S1 C2 C3 . . . . -59.9(2) no
Pd2 S2 Pd3 Cl3 . . . . -136.88(3) no
Pd2 S2 Pd3 S3 . . . . 43.02(2) no
Pd2 S2 C32 C31 . . . . 14.4(2) no
Pd2 S2 C32 C33 . . . . -163.8(2) no
Pd2 P2 C31 C32 . . . . -13.4(2) no
Pd2 P2 C31 C36 . . . . 164.9(2) no
Pd2 P2 C41 C42 . . . . -77.3(2) no
Pd2 P2 C41 C46 . . . . 98.1(2) no
Pd2 P2 C51 C52 . . . . -19.6(3) no
Pd2 P2 C51 C56 . . . . 163.6(3) no
Pd3 S2 Pd2 S1 . . . . -87.41(2) no
Pd3 S2 Pd2 P2 . . . . 94.14(2) no
Pd3 S2 C32 C31 . . . . -95.4(2) no
Pd3 S2 C32 C33 . . . . 86.5(2) no
Pd3 S3 Pd1 Cl1 . . . . 69.30(3) no
Pd3 S3 Pd1 S1 . . . . -110.17(2) no
Pd3 S3 C62 C61 . . . . 17.1(2) no
Pd3 S3 C62 C63 . . . . -166.0(2) no
Pd3 P3 C61 C62 . . . . -11.1(2) no
Pd3 P3 C61 C66 . . . . 166.9(2) no
Pd3 P3 C71 C72 . . . . -34.8(2) no
Pd3 P3 C71 C76 . . . . 150.2(3) no
Pd3 P3 C81 C82 . . . . -28.2(3) no
Pd3 P3 C81 C86 . . . . 152.8(2) no
Cl1 Pd1 S3 C62 . . . . -39.34(9) no
Cl1 Pd1 P1 C1 . . . . -159.05(8) no
Cl1 Pd1 P1 C11 . . . . -37.9(1) no
Cl1 Pd1 P1 C21 . . . . 85.7(1) no
Cl2 Pd2 S1 C2 . . . . 96.04(9) no
Cl2 Pd2 P2 C31 . . . . -163.47(8) no
Cl2 Pd2 P2 C41 . . . . -45.3(1) no
Cl2 Pd2 P2 C51 . . . . 77.4(1) no
Cl3 Pd3 S2 C32 . . . . -26.23(9) no
Cl3 Pd3 P3 C61 . . . . -164.1(1) no
Cl3 Pd3 P3 C71 . . . . -48.81(9) no
Cl3 Pd3 P3 C81 . . . . 76.35(9) no
S1 Pd1 S3 C62 . . . . 141.20(9) no
S1 Pd1 P1 C1 . . . . 20.39(8) no
S1 Pd1 P1 C11 . . . . 141.5(1) no
S1 Pd1 P1 C21 . . . . -94.9(1) no
S1 Pd2 S2 C32 . . . . 161.61(8) no
S1 C2 C1 P1 . . . . 5.0(3) no
S1 C2 C1 C6 . . . . -176.3(2) no
S1 C2 C3 C4 . . . . 176.8(2) no
S2 Pd2 S1 C2 . . . . -84.16(9) no
S2 Pd2 P2 C31 . . . . 16.77(8) no
S2 Pd2 P2 C41 . . . . 135.0(1) no
S2 Pd2 P2 C51 . . . . -102.4(1) no
S2 Pd3 S3 C62 . . . . 160.29(8) no
S2 C32 C31 P2 . . . . -1.0(3) no
S2 C32 C31 C36 . . . . -179.3(2) no
S2 C32 C33 C34 . . . . 178.5(2) no
S3 Pd1 S1 C2 . . . . 159.58(8) no
S3 Pd3 S2 C32 . . . . 153.67(9) no
S3 Pd3 P3 C61 . . . . 16.21(9) no
S3 Pd3 P3 C71 . . . . 131.48(9) no
S3 Pd3 P3 C81 . . . . -103.37(9) no
S3 C62 C61 P3 . . . . -4.4(3) no
S3 C62 C61 C66 . . . . 177.6(2) no
S3 C62 C63 C64 . . . . -176.9(2) no
P1 Pd1 S1 C2 . . . . -18.04(8) no
P1 C1 C2 C3 . . . . -174.4(2) no
P1 C1 C6 C5 . . . . 177.3(2) no
P1 C11 C12 C13 . . . . -178.4(2) no
P1 C11 C16 C15 . . . . 178.7(3) no
P1 C21 C22 C23 . . . . 176.7(3) no
P1 C21 C26 C25 . . . . -175.0(2) no
P2 Pd2 S2 C32 . . . . -16.83(8) no
P2 C31 C32 C33 . . . . 177.2(2) no
P2 C31 C36 C35 . . . . -177.6(2) no
P2 C41 C42 C43 . . . . 174.9(3) no
P2 C41 C46 C45 . . . . -175.5(3) no
P2 C51 C52 C53 . . . . -178.1(3) no
P2 C51 C56 C55 . . . . 178.8(3) no
P3 Pd3 S3 C62 . . . . -17.69(8) no
P3 C61 C62 C63 . . . . 178.7(2) no
P3 C61 C66 C65 . . . . -178.8(2) no
P3 C71 C72 C73 . . . . -176.3(3) no
P3 C71 C76 C75 . . . . 174.8(3) no
P3 C81 C82 C83 . . . . -176.2(3) no
P3 C81 C86 C85 . . . . 175.8(3) no
C1 P1 C11 C12 . . . . 73.1(2) no
C1 P1 C11 C16 . . . . -106.0(3) no
C1 P1 C21 C22 . . . . -177.9(2) no
C1 P1 C21 C26 . . . . -2.5(3) no
C1 C2 C3 C4 . . . . -3.8(4) no
C1 C6 C5 C4 . . . . -2.1(5) no
C2 C1 P1 C11 . . . . -148.3(2) no
C2 C1 P1 C21 . . . . 97.6(2) no
C2 C1 C6 C5 . . . . -1.3(4) no
C2 C3 C4 C5 . . . . 0.3(5) no
C3 C2 C1 C6 . . . . 4.3(4) no
C3 C4 C5 C6 . . . . 2.6(5) no
C6 C1 P1 C11 . . . . 33.1(3) no
C6 C1 P1 C21 . . . . -81.0(2) no
C11 P1 C21 C22 . . . . 67.9(2) no
C11 P1 C21 C26 . . . . -116.6(2) no
C11 C12 C13 C14 . . . . -0.7(5) no
C11 C16 C15 C14 . . . . -0.0(6) no
C12 C11 P1 C21 . . . . -172.9(2) no
C12 C11 C16 C15 . . . . -0.4(5) no
C12 C13 C14 C15 . . . . 0.3(5) no
C13 C12 C11 C16 . . . . 0.7(4) no
C13 C14 C15 C16 . . . . 0.0(6) no
C16 C11 P1 C21 . . . . 8.0(3) no
C21 C22 C23 C24 . . . . -1.6(5) no
C21 C26 C25 C24 . . . . -1.5(5) no
C22 C21 C26 C25 . . . . 0.4(4) no
C22 C23 C24 C25 . . . . 0.4(6) no
C23 C22 C21 C26 . . . . 1.2(5) no
C23 C24 C25 C26 . . . . 1.1(6) no
C31 P2 C41 C42 . . . . 41.7(3) no
C31 P2 C41 C46 . . . . -142.9(2) no
C31 P2 C51 C52 . . . . -138.4(3) no
C31 P2 C51 C56 . . . . 44.8(3) no
C31 C32 C33 C34 . . . . 0.3(4) no
C31 C36 C35 C34 . . . . 0.9(4) no
C32 C31 P2 C41 . . . . -137.4(2) no
C32 C31 P2 C51 . . . . 108.6(2) no
C32 C31 C36 C35 . . . . 0.6(4) no
C32 C33 C34 C35 . . . . 1.2(4) no
C33 C32 C31 C36 . . . . -1.1(4) no
C33 C34 C35 C36 . . . . -1.8(4) no
C36 C31 P2 C41 . . . . 40.9(2) no
C36 C31 P2 C51 . . . . -73.1(2) no
C41 P2 C51 C52 . . . . 107.9(3) no
C41 P2 C51 C56 . . . . -69.0(3) no
C41 C42 C43 C44 . . . . 0.3(5) no
C41 C46 C45 C44 . . . . 1.0(6) no
C42 C41 P2 C51 . . . . 156.8(2) no
C42 C41 C46 C45 . . . . -0.1(5) no
C42 C43 C44 C45 . . . . 0.6(6) no
C43 C42 C41 C46 . . . . -0.5(5) no
C43 C44 C45 C46 . . . . -1.3(7) no
C46 C41 P2 C51 . . . . -27.8(3) no
C51 C52 C53 C54 . . . . -1.8(7) no
C51 C56 C55 C54 . . . . 0.4(7) no
C52 C51 C56 C55 . . . . 2.0(6) no
C52 C53 C54 C55 . . . . 4.2(7) no
C53 C52 C51 C56 . . . . -1.2(6) no
C53 C54 C55 C56 . . . . -3.4(7) no
C61 P3 C71 C72 . . . . 83.3(2) no
C61 P3 C71 C76 . . . . -91.7(3) no
C61 P3 C81 C82 . . . . -147.8(2) no
C61 P3 C81 C86 . . . . 33.2(3) no
C61 C62 C63 C64 . . . . 0.1(4) no
C61 C66 C65 C64 . . . . 0.5(5) no
C62 C61 P3 C71 . . . . -134.4(2) no
C62 C61 P3 C81 . . . . 111.4(2) no
C62 C61 C66 C65 . . . . -0.9(4) no
C62 C63 C64 C65 . . . . -0.4(5) no
C63 C62 C61 C66 . . . . 0.6(4) no
C63 C64 C65 C66 . . . . 0.2(5) no
C66 C61 P3 C71 . . . . 43.6(3) no
C66 C61 P3 C81 . . . . -70.6(3) no
C71 P3 C81 C82 . . . . 101.2(3) no
C71 P3 C81 C86 . . . . -77.8(3) no
C71 C72 C73 C74 . . . . 1.0(6) no
C71 C76 C75 C74 . . . . 1.9(6) no
C72 C71 P3 C81 . . . . -162.4(2) no
C72 C71 C76 C75 . . . . -0.2(5) no
C72 C73 C74 C75 . . . . 0.6(6) no
C73 C72 C71 C76 . . . . -1.2(5) no
C73 C74 C75 C76 . . . . -2.1(6) no
C76 C71 P3 C81 . . . . 22.6(3) no
C81 C82 C83 C84 . . . . -0.4(5) no
C81 C86 C85 C84 . . . . 1.3(5) no
C82 C81 C86 C85 . . . . -3.2(5) no
C82 C83 C84 C85 . . . . -1.6(6) no
C83 C82 C81 C86 . . . . 2.8(5) no
C83 C84 C85 C86 . . . . 1.2(6) no
_database_code_depnum_ccdc_archive 'CCDC 999166'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex13
_audit_creation_date             09-09-09
_audit_creation_method           CRYSTALS_ver_12.85

_oxford_structure_analysis_title '9091019 ben0911'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_audit_update_record             
;
2009-09-09- Report on C36 H29 Cl P2 Pd Se 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-09-09- passes checkcif tests with minor warnings  
;

_cell_length_a                   9.0444(2)
_cell_length_b                   32.6774(6)
_cell_length_c                   10.7989(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.9592(8)
_cell_angle_gamma                90
_cell_volume                     3179.64(11)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C36 H29 Cl1 P2 Pd1 Se1 
# Dc =      1.55 Fooo =   1488.00 Mu =     19.37 M =    744.39
# Found Formula = C36 H29 Cl1 P2 Pd1 Se1 
# Dc =      1.55 FOOO =   1488.00 Mu =     19.37 M =    744.39

_chemical_formula_sum            'C36 H29 Cl P2 Pd Se'
_chemical_formula_moiety         'C36 H29 Cl P2 Pd Se'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         744.39


_cell_measurement_reflns_used    70489
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.11
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_max          0.36

_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    1.937

# Sheldrick geometric approximatio 0.71 0.81 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.170
-1 0 0 0.190
0 1 0 0.030
0 -1 0 0.080
0 0 1 0.030
0 0 -1 0.150
-1 10 0 0.020


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.048

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 0.7 deg at rate 49 sec/frame,
crystal-detector distance 55mm,
multiple scan sets so over 95 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            48290
_reflns_number_total             7249
_diffrn_reflns_av_R_equivalents  0.072
# Number of reflections with Friedels Law is 7249 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 7293 


_diffrn_reflns_theta_min         2.661
_diffrn_reflns_theta_max         27.484
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        26.934
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              42
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   2.42
_oxford_diffrn_Wilson_scale      13.96

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.66
_refine_diff_density_max         0.55


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7249
_refine_ls_number_restraints     0
_refine_ls_number_parameters     370
_oxford_refine_ls_R_factor_ref   0.0365
_refine_ls_wR_factor_ref         0.0927
_refine_ls_goodness_of_fit_ref   0.7946
_refine_ls_shift/su_max          0.001516


# The values computed from all data 
_oxford_reflns_number_all        7249
_refine_ls_R_factor_all          0.0365
_refine_ls_wR_factor_all         0.0927

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5460
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_gt          0.0680

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 26.6 40.7 21.0 5.91 
;
_refine_special_details          
;

Hydrogen atoms were included at idealized positions
They were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.


;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.32712(2) 0.374721(6) 0.769442(17) 0.0272 1.0000 Uani . . . . . . .
Se1 Se 0.39181(4) 0.304124(9) 0.84227(3) 0.0372 1.0000 Uani . . . . . . .
Cl1 Cl 0.30071(9) 0.39297(2) 0.98117(6) 0.0425 1.0000 Uani . . . . . . .
P1 P 0.28821(7) 0.28516(2) 0.66398(6) 0.0294 1.0000 Uani . . . . . . .
P2 P 0.20208(7) 0.43205(2) 0.69579(6) 0.0281 1.0000 Uani . . . . . . .
C1 C 0.3617(3) 0.31901(8) 0.5547(2) 0.0311 1.0000 Uani . . . . . . .
C2 C 0.3855(3) 0.35907(8) 0.6001(2) 0.0299 1.0000 Uani . . . . . . .
C3 C 0.4583(3) 0.38588(9) 0.5237(3) 0.0376 1.0000 Uani . . . . . . .
C4 C 0.4989(4) 0.37345(11) 0.4087(3) 0.0516 1.0000 Uani . . . . . . .
C5 C 0.4673(5) 0.33439(12) 0.3637(3) 0.0545 1.0000 Uani . . . . . . .
C6 C 0.3988(4) 0.30680(10) 0.4370(3) 0.0415 1.0000 Uani . . . . . . .
C11 C 0.0882(3) 0.29077(8) 0.6474(3) 0.0340 1.0000 Uani . . . . . . .
C12 C 0.0080(4) 0.29512(11) 0.7504(4) 0.0493 1.0000 Uani . . . . . . .
C13 C -0.1455(4) 0.30183(13) 0.7336(4) 0.0606 1.0000 Uani . . . . . . .
C14 C -0.2162(4) 0.30449(11) 0.6154(5) 0.0590 1.0000 Uani . . . . . . .
C15 C -0.1368(4) 0.29987(11) 0.5120(4) 0.0541 1.0000 Uani . . . . . . .
C16 C 0.0150(4) 0.29296(10) 0.5283(3) 0.0446 1.0000 Uani . . . . . . .
C21 C 0.3322(3) 0.23291(8) 0.6257(3) 0.0341 1.0000 Uani . . . . . . .
C22 C 0.4814(4) 0.22217(9) 0.6270(3) 0.0428 1.0000 Uani . . . . . . .
C23 C 0.5209(4) 0.18293(10) 0.5922(3) 0.0507 1.0000 Uani . . . . . . .
C24 C 0.4120(5) 0.15469(10) 0.5592(3) 0.0546 1.0000 Uani . . . . . . .
C25 C 0.2637(5) 0.16466(10) 0.5604(4) 0.0535 1.0000 Uani . . . . . . .
C26 C 0.2220(4) 0.20408(9) 0.5930(3) 0.0419 1.0000 Uani . . . . . . .
C31 C 0.0215(3) 0.43305(8) 0.7608(3) 0.0319 1.0000 Uani . . . . . . .
C32 C -0.1031(3) 0.41294(11) 0.7055(3) 0.0437 1.0000 Uani . . . . . . .
C33 C -0.2326(4) 0.41092(12) 0.7656(4) 0.0523 1.0000 Uani . . . . . . .
C34 C -0.2405(3) 0.42926(10) 0.8799(3) 0.0441 1.0000 Uani . . . . . . .
C35 C -0.1182(4) 0.44984(9) 0.9351(3) 0.0418 1.0000 Uani . . . . . . .
C36 C 0.0125(3) 0.45149(9) 0.8766(3) 0.0368 1.0000 Uani . . . . . . .
C41 C 0.1662(3) 0.43553(9) 0.5269(3) 0.0345 1.0000 Uani . . . . . . .
C42 C 0.1091(4) 0.40109(11) 0.4628(3) 0.0439 1.0000 Uani . . . . . . .
C43 C 0.0996(4) 0.40052(13) 0.3333(3) 0.0576 1.0000 Uani . . . . . . .
C44 C 0.1474(4) 0.43375(15) 0.2674(3) 0.0607 1.0000 Uani . . . . . . .
C45 C 0.2027(4) 0.46755(13) 0.3301(3) 0.0540 1.0000 Uani . . . . . . .
C46 C 0.2123(3) 0.46901(10) 0.4592(3) 0.0418 1.0000 Uani . . . . . . .
C51 C 0.2825(3) 0.48096(8) 0.7441(2) 0.0300 1.0000 Uani . . . . . . .
C52 C 0.4237(3) 0.48191(9) 0.8077(3) 0.0362 1.0000 Uani . . . . . . .
C53 C 0.4860(3) 0.51890(10) 0.8491(3) 0.0401 1.0000 Uani . . . . . . .
C54 C 0.4090(4) 0.55499(10) 0.8275(3) 0.0404 1.0000 Uani . . . . . . .
C55 C 0.2688(4) 0.55443(9) 0.7647(3) 0.0402 1.0000 Uani . . . . . . .
C56 C 0.2053(3) 0.51772(9) 0.7233(3) 0.0353 1.0000 Uani . . . . . . .
H31 H 0.4790 0.4128 0.5499 0.0456 1.0000 Uiso R . . . . . .
H41 H 0.5485 0.3915 0.3608 0.0631 1.0000 Uiso R . . . . . .
H51 H 0.4929 0.3265 0.2858 0.0672 1.0000 Uiso R . . . . . .
H61 H 0.3776 0.2807 0.4084 0.0495 1.0000 Uiso R . . . . . .
H121 H 0.0568 0.2935 0.8295 0.0598 1.0000 Uiso R . . . . . .
H131 H -0.2002 0.3043 0.8025 0.0741 1.0000 Uiso R . . . . . .
H141 H -0.3169 0.3094 0.6054 0.0704 1.0000 Uiso R . . . . . .
H151 H -0.1851 0.3019 0.4324 0.0639 1.0000 Uiso R . . . . . .
H161 H 0.0690 0.2903 0.4606 0.0529 1.0000 Uiso R . . . . . .
H221 H 0.5540 0.2409 0.6510 0.0512 1.0000 Uiso R . . . . . .
H231 H 0.6200 0.1759 0.5915 0.0610 1.0000 Uiso R . . . . . .
H241 H 0.4392 0.1285 0.5362 0.0648 1.0000 Uiso R . . . . . .
H251 H 0.1904 0.1455 0.5393 0.0635 1.0000 Uiso R . . . . . .
H261 H 0.1231 0.2113 0.5934 0.0497 1.0000 Uiso R . . . . . .
H321 H -0.0998 0.4009 0.6276 0.0527 1.0000 Uiso R . . . . . .
H331 H -0.3147 0.3971 0.7287 0.0631 1.0000 Uiso R . . . . . .
H341 H -0.3280 0.4274 0.9207 0.0531 1.0000 Uiso R . . . . . .
H351 H -0.1232 0.4619 1.0124 0.0508 1.0000 Uiso R . . . . . .
H361 H 0.0937 0.4648 0.9155 0.0450 1.0000 Uiso R . . . . . .
H421 H 0.0788 0.3783 0.5052 0.0514 1.0000 Uiso R . . . . . .
H431 H 0.0618 0.3771 0.2925 0.0677 1.0000 Uiso R . . . . . .
H441 H 0.1435 0.4333 0.1820 0.0731 1.0000 Uiso R . . . . . .
H451 H 0.2337 0.4902 0.2864 0.0651 1.0000 Uiso R . . . . . .
H461 H 0.2509 0.4924 0.5016 0.0511 1.0000 Uiso R . . . . . .
H521 H 0.4750 0.4572 0.8231 0.0429 1.0000 Uiso R . . . . . .
H531 H 0.5805 0.5190 0.8916 0.0484 1.0000 Uiso R . . . . . .
H541 H 0.4507 0.5798 0.8544 0.0486 1.0000 Uiso R . . . . . .
H551 H 0.2152 0.5782 0.7515 0.0488 1.0000 Uiso R . . . . . .
H561 H 0.1110 0.5170 0.6821 0.0431 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.27699(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Se1 . 2.4906(3) yes
Pd1 . Cl1 . 2.3947(7) yes
Pd1 . P2 . 2.2947(7) yes
Pd1 . C2 . 2.013(3) yes
Se1 . P1 . 2.1579(7) yes
P1 . C1 . 1.787(3) yes
P1 . C11 . 1.812(3) yes
P1 . C21 . 1.809(3) yes
P2 . C31 . 1.833(3) yes
P2 . C41 . 1.828(3) yes
P2 . C51 . 1.814(3) yes
C1 . C2 . 1.408(4) yes
C1 . C6 . 1.400(4) yes
C2 . C3 . 1.406(4) yes
C3 . C4 . 1.386(5) yes
C3 . H31 . 0.939 no
C4 . C5 . 1.386(5) yes
C4 . H41 . 0.925 no
C5 . C6 . 1.381(5) yes
C5 . H51 . 0.929 no
C6 . H61 . 0.921 no
C11 . C12 . 1.386(4) yes
C11 . C16 . 1.396(4) yes
C12 . C13 . 1.401(5) yes
C12 . H121 . 0.928 no
C13 . C14 . 1.380(6) yes
C13 . H131 . 0.932 no
C14 . C15 . 1.387(6) yes
C14 . H141 . 0.922 no
C15 . C16 . 1.387(5) yes
C15 . H151 . 0.933 no
C16 . H161 . 0.919 no
C21 . C22 . 1.393(4) yes
C21 . C26 . 1.395(4) yes
C22 . C23 . 1.392(4) yes
C22 . H221 . 0.920 no
C23 . C24 . 1.374(5) yes
C23 . H231 . 0.927 no
C24 . C25 . 1.382(6) yes
C24 . H241 . 0.931 no
C25 . C26 . 1.396(4) yes
C25 . H251 . 0.925 no
C26 . H261 . 0.925 no
C31 . C32 . 1.393(4) yes
C31 . C36 . 1.397(4) yes
C32 . C33 . 1.389(5) yes
C32 . H321 . 0.931 no
C33 . C34 . 1.380(5) yes
C33 . H331 . 0.929 no
C34 . C35 . 1.385(5) yes
C34 . H341 . 0.940 no
C35 . C36 . 1.389(4) yes
C35 . H351 . 0.927 no
C36 . H361 . 0.923 no
C41 . C42 . 1.397(4) yes
C41 . C46 . 1.399(4) yes
C42 . C43 . 1.394(5) yes
C42 . H421 . 0.927 no
C43 . C44 . 1.388(6) yes
C43 . H431 . 0.933 no
C44 . C45 . 1.367(6) yes
C44 . H441 . 0.920 no
C45 . C46 . 1.390(4) yes
C45 . H451 . 0.934 no
C46 . H461 . 0.942 no
C51 . C52 . 1.397(4) yes
C51 . C56 . 1.397(4) yes
C52 . C53 . 1.391(4) yes
C52 . H521 . 0.940 no
C53 . C54 . 1.380(5) yes
C53 . H531 . 0.934 no
C54 . C55 . 1.385(5) yes
C54 . H541 . 0.930 no
C55 . C56 . 1.387(4) yes
C55 . H551 . 0.921 no
C56 . H561 . 0.928 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se1 . Pd1 . Cl1 . 88.24(2) yes
Se1 . Pd1 . P2 . 163.93(2) yes
Cl1 . Pd1 . P2 . 92.34(3) yes
Se1 . Pd1 . C2 . 88.77(7) yes
Cl1 . Pd1 . C2 . 170.53(7) yes
P2 . Pd1 . C2 . 93.02(7) yes
Pd1 . Se1 . P1 . 84.97(2) yes
Se1 . P1 . C1 . 104.71(9) yes
Se1 . P1 . C11 . 114.32(10) yes
C1 . P1 . C11 . 107.30(13) yes
Se1 . P1 . C21 . 112.83(10) yes
C1 . P1 . C21 . 109.35(13) yes
C11 . P1 . C21 . 108.08(13) yes
Pd1 . P2 . C31 . 108.10(9) yes
Pd1 . P2 . C41 . 115.87(9) yes
C31 . P2 . C41 . 107.08(13) yes
Pd1 . P2 . C51 . 116.51(9) yes
C31 . P2 . C51 . 102.85(12) yes
C41 . P2 . C51 . 105.32(13) yes
P1 . C1 . C2 . 113.55(19) yes
P1 . C1 . C6 . 123.7(2) yes
C2 . C1 . C6 . 122.7(3) yes
C1 . C2 . Pd1 . 120.59(19) yes
C1 . C2 . C3 . 116.1(2) yes
Pd1 . C2 . C3 . 123.2(2) yes
C2 . C3 . C4 . 121.1(3) yes
C2 . C3 . H31 . 119.9 no
C4 . C3 . H31 . 118.9 no
C3 . C4 . C5 . 121.4(3) yes
C3 . C4 . H41 . 119.5 no
C5 . C4 . H41 . 119.1 no
C4 . C5 . C6 . 119.3(3) yes
C4 . C5 . H51 . 120.9 no
C6 . C5 . H51 . 119.8 no
C1 . C6 . C5 . 119.2(3) yes
C1 . C6 . H61 . 120.6 no
C5 . C6 . H61 . 120.2 no
P1 . C11 . C12 . 121.2(3) yes
P1 . C11 . C16 . 119.1(2) yes
C12 . C11 . C16 . 119.6(3) yes
C11 . C12 . C13 . 119.6(4) yes
C11 . C12 . H121 . 119.5 no
C13 . C12 . H121 . 121.0 no
C12 . C13 . C14 . 120.3(3) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 119.8 no
C13 . C14 . C15 . 120.5(3) yes
C13 . C14 . H141 . 119.5 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 119.4(4) yes
C14 . C15 . H151 . 120.0 no
C16 . C15 . H151 . 120.6 no
C11 . C16 . C15 . 120.7(3) yes
C11 . C16 . H161 . 119.1 no
C15 . C16 . H161 . 120.2 no
P1 . C21 . C22 . 117.9(2) yes
P1 . C21 . C26 . 121.9(2) yes
C22 . C21 . C26 . 120.2(3) yes
C21 . C22 . C23 . 120.1(3) yes
C21 . C22 . H221 . 120.2 no
C23 . C22 . H221 . 119.8 no
C22 . C23 . C24 . 119.6(3) yes
C22 . C23 . H231 . 120.2 no
C24 . C23 . H231 . 120.2 no
C23 . C24 . C25 . 120.9(3) yes
C23 . C24 . H241 . 119.1 no
C25 . C24 . H241 . 119.9 no
C24 . C25 . C26 . 120.2(3) yes
C24 . C25 . H251 . 120.9 no
C26 . C25 . H251 . 118.9 no
C25 . C26 . C21 . 119.0(3) yes
C25 . C26 . H261 . 121.3 no
C21 . C26 . H261 . 119.7 no
P2 . C31 . C32 . 122.8(2) yes
P2 . C31 . C36 . 118.2(2) yes
C32 . C31 . C36 . 118.7(3) yes
C31 . C32 . C33 . 120.4(3) yes
C31 . C32 . H321 . 119.8 no
C33 . C32 . H321 . 119.8 no
C32 . C33 . C34 . 120.6(3) yes
C32 . C33 . H331 . 119.8 no
C34 . C33 . H331 . 119.6 no
C33 . C34 . C35 . 119.6(3) yes
C33 . C34 . H341 . 120.1 no
C35 . C34 . H341 . 120.2 no
C34 . C35 . C36 . 120.2(3) yes
C34 . C35 . H351 . 119.6 no
C36 . C35 . H351 . 120.2 no
C31 . C36 . C35 . 120.5(3) yes
C31 . C36 . H361 . 120.4 no
C35 . C36 . H361 . 119.1 no
P2 . C41 . C42 . 118.1(2) yes
P2 . C41 . C46 . 122.3(2) yes
C42 . C41 . C46 . 119.0(3) yes
C41 . C42 . C43 . 119.7(4) yes
C41 . C42 . H421 . 120.9 no
C43 . C42 . H421 . 119.3 no
C42 . C43 . C44 . 120.6(4) yes
C42 . C43 . H431 . 118.2 no
C44 . C43 . H431 . 121.2 no
C43 . C44 . C45 . 119.7(3) yes
C43 . C44 . H441 . 121.0 no
C45 . C44 . H441 . 119.4 no
C44 . C45 . C46 . 120.9(4) yes
C44 . C45 . H451 . 120.2 no
C46 . C45 . H451 . 118.9 no
C41 . C46 . C45 . 120.1(3) yes
C41 . C46 . H461 . 119.6 no
C45 . C46 . H461 . 120.3 no
P2 . C51 . C52 . 119.2(2) yes
P2 . C51 . C56 . 121.9(2) yes
C52 . C51 . C56 . 118.8(2) yes
C51 . C52 . C53 . 120.3(3) yes
C51 . C52 . H521 . 119.0 no
C53 . C52 . H521 . 120.7 no
C52 . C53 . C54 . 120.2(3) yes
C52 . C53 . H531 . 119.4 no
C54 . C53 . H531 . 120.4 no
C53 . C54 . C55 . 120.0(3) yes
C53 . C54 . H541 . 120.5 no
C55 . C54 . H541 . 119.6 no
C54 . C55 . C56 . 120.3(3) yes
C54 . C55 . H551 . 120.8 no
C56 . C55 . H551 . 118.8 no
C51 . C56 . C55 . 120.3(3) yes
C51 . C56 . H561 . 118.8 no
C55 . C56 . H561 . 120.9 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
C24 C34 3.566(5) . 4_554 no
C34 C52 3.519(4) . 1_455 no
C44 C56 3.572(5) . 2_566 no
C45 C53 3.579(5) . 2_666 no
C53 C53 3.474(7) . 2_667 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 P1 C1 . . . . 46.03(9) no
Pd1 Se1 P1 C11 . . . . -71.1(1) no
Pd1 Se1 P1 C21 . . . . 164.9(1) no
Pd1 P2 C31 C32 . . . . -86.5(3) no
Pd1 P2 C31 C36 . . . . 87.3(2) no
Pd1 P2 C41 C42 . . . . 47.0(3) no
Pd1 P2 C41 C46 . . . . -124.1(2) no
Pd1 P2 C51 C52 . . . . 8.8(2) no
Pd1 P2 C51 C56 . . . . -169.0(2) no
Pd1 C2 C1 P1 . . . . -3.5(3) no
Pd1 C2 C1 C6 . . . . 179.2(2) no
Pd1 C2 C3 C4 . . . . 178.7(2) no
Se1 Pd1 P2 C31 . . . . 37.0(1) no
Se1 Pd1 P2 C41 . . . . -83.1(1) no
Se1 Pd1 P2 C51 . . . . 152.2(1) no
Se1 Pd1 C2 C1 . . . . 33.8(2) no
Se1 Pd1 C2 C3 . . . . -142.7(2) no
Se1 P1 C1 C2 . . . . -35.6(2) no
Se1 P1 C1 C6 . . . . 141.7(2) no
Se1 P1 C11 C12 . . . . -17.9(3) no
Se1 P1 C11 C16 . . . . 158.6(2) no
Se1 P1 C21 C22 . . . . -55.3(3) no
Se1 P1 C21 C26 . . . . 126.1(3) no
Cl1 Pd1 Se1 P1 . . . . 148.53(3) no
Cl1 Pd1 P2 C31 . . . . -54.7(1) no
Cl1 Pd1 P2 C41 . . . . -174.8(1) no
Cl1 Pd1 P2 C51 . . . . 60.40(9) no
P1 Se1 Pd1 P2 . . . . 56.19(8) no
P1 Se1 Pd1 C2 . . . . -40.47(8) no
P1 C1 C2 C3 . . . . 173.2(2) no
P1 C1 C6 C5 . . . . -174.2(3) no
P1 C11 C12 C13 . . . . 176.2(3) no
P1 C11 C16 C15 . . . . -175.9(3) no
P1 C21 C22 C23 . . . . -176.8(2) no
P1 C21 C26 C25 . . . . 177.8(3) no
P2 Pd1 C2 C1 . . . . -130.3(2) no
P2 Pd1 C2 C3 . . . . 53.3(2) no
P2 C31 C32 C33 . . . . 172.9(3) no
P2 C31 C36 C35 . . . . -174.2(2) no
P2 C41 C42 C43 . . . . -171.1(3) no
P2 C41 C46 C45 . . . . 170.2(2) no
P2 C51 C52 C53 . . . . -178.0(2) no
P2 C51 C56 C55 . . . . 178.2(2) no
C1 P1 C11 C12 . . . . -133.5(3) no
C1 P1 C11 C16 . . . . 43.0(3) no
C1 P1 C21 C22 . . . . 60.7(3) no
C1 P1 C21 C26 . . . . -117.8(3) no
C1 C2 C3 C4 . . . . 2.1(4) no
C1 C6 C5 C4 . . . . 0.5(5) no
C2 Pd1 P2 C31 . . . . 133.1(1) no
C2 Pd1 P2 C41 . . . . 13.0(1) no
C2 Pd1 P2 C51 . . . . -111.8(1) no
C2 C1 P1 C11 . . . . 86.2(2) no
C2 C1 P1 C21 . . . . -156.8(2) no
C2 C1 C6 C5 . . . . 2.8(5) no
C2 C3 C4 C5 . . . . 1.0(5) no
C3 C2 C1 C6 . . . . -4.1(4) no
C3 C4 C5 C6 . . . . -2.4(6) no
C6 C1 P1 C11 . . . . -96.5(3) no
C6 C1 P1 C21 . . . . 20.5(3) no
C11 P1 C21 C22 . . . . 177.2(3) no
C11 P1 C21 C26 . . . . -1.3(3) no
C11 C12 C13 C14 . . . . -0.6(6) no
C11 C16 C15 C14 . . . . -0.2(5) no
C12 C11 P1 C21 . . . . 108.6(3) no
C12 C11 C16 C15 . . . . 0.7(5) no
C12 C13 C14 C15 . . . . 1.1(6) no
C13 C12 C11 C16 . . . . -0.3(5) no
C13 C14 C15 C16 . . . . -0.7(5) no
C16 C11 P1 C21 . . . . -74.9(3) no
C21 C22 C23 C24 . . . . -1.4(5) no
C21 C26 C25 C24 . . . . -0.8(5) no
C22 C21 C26 C25 . . . . -0.7(5) no
C22 C23 C24 C25 . . . . -0.2(5) no
C23 C22 C21 C26 . . . . 1.8(5) no
C23 C24 C25 C26 . . . . 1.3(6) no
C31 P2 C41 C42 . . . . -73.6(3) no
C31 P2 C41 C46 . . . . 115.3(2) no
C31 P2 C51 C52 . . . . 126.8(2) no
C31 P2 C51 C56 . . . . -51.0(3) no
C31 C32 C33 C34 . . . . 0.9(5) no
C31 C36 C35 C34 . . . . 1.0(5) no
C32 C31 P2 C41 . . . . 39.0(3) no
C32 C31 P2 C51 . . . . 149.7(3) no
C32 C31 C36 C35 . . . . -0.1(4) no
C32 C33 C34 C35 . . . . -0.0(5) no
C33 C32 C31 C36 . . . . -0.9(5) no
C33 C34 C35 C36 . . . . -1.0(5) no
C36 C31 P2 C41 . . . . -147.3(2) no
C36 C31 P2 C51 . . . . -36.5(2) no
C41 P2 C51 C52 . . . . -121.2(2) no
C41 P2 C51 C56 . . . . 61.0(3) no
C41 C42 C43 C44 . . . . 0.5(5) no
C41 C46 C45 C44 . . . . 0.5(5) no
C42 C41 P2 C51 . . . . 177.4(2) no
C42 C41 C46 C45 . . . . -0.8(4) no
C42 C43 C44 C45 . . . . -0.8(6) no
C43 C42 C41 C46 . . . . 0.3(5) no
C43 C44 C45 C46 . . . . 0.3(6) no
C46 C41 P2 C51 . . . . 6.3(3) no
C51 C52 C53 C54 . . . . -0.1(5) no
C51 C56 C55 C54 . . . . -0.3(5) no
C52 C51 C56 C55 . . . . 0.4(4) no
C52 C53 C54 C55 . . . . 0.2(5) no
C53 C52 C51 C56 . . . . -0.2(4) no
C53 C54 C55 C56 . . . . -0.0(5) no
_database_code_depnum_ccdc_archive 'CCDC 999167'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex14
_audit_creation_date             09-11-17
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2009-11-17 - Report on C54.38 H44.50 Cl2 O0.38 P3 Pd2 Se1 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2009-11-17 - passes checkcif tests with minor warnings  
;

_oxford_structure_analysis_title '11171143 ben0912'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   19.3124(2)
_cell_length_b                   12.3355(1)
_cell_length_c                   22.5574(2)
_cell_angle_alpha                90
_cell_angle_beta                 114.9619(4)
_cell_angle_gamma                90
_cell_volume                     4871.83(8)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C55 H47 Cl2 O1 P3 Pd2 Se1 
# Dc =      1.61 Fooo =   2315.05 Mu =     17.33 M =   1179.56
# Found Formula = C54.38 H44.50 Cl2 O0.38 P3 Pd2 Se1 
# Dc =      1.58 FOOO =   2315.05 Mu =     17.31 M =   1159.56

_chemical_formula_sum            'C54.376 H44.504 Cl2 O0.376 P3 Pd2 Se'
_chemical_formula_moiety         'C54 H43 Cl2 P3 Pd2 Se, 0.376(C H4 O)'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         1159.56


_cell_measurement_reflns_used    93888
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30
_cell_measurement_temperature    200

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.140
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.420

_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2315.047
_exptl_absorpt_coefficient_mu    1.731

# Sheldrick geometric approximatio 0.71 0.78 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.080
0 1 0 0.220
0 -1 0 0.200
0 0 1 0.035
0 0 -1 0.100
-3 0 -3 0.060
3 0 3 0.060
-2 0 2 0.090
2 0 -2 0.110


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.4 deg at rate 28 sec/frame,
crystal-detector distance 35mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            116293
_reflns_number_total             14243
_diffrn_reflns_av_R_equivalents  0.043
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 14243 
# Theoretical number of reflections is about 28508 


_diffrn_reflns_theta_min         2.587
_diffrn_reflns_theta_max         30.034
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.034
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_reflns_limit_h_min              -27
_reflns_limit_h_max              24
_reflns_limit_k_min              0
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      27.94

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.73
_refine_diff_density_max         0.85


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         14243
_refine_ls_number_restraints     0
_refine_ls_number_parameters     578
_oxford_refine_ls_R_factor_ref   0.0399
_refine_ls_wR_factor_ref         0.0612
_refine_ls_goodness_of_fit_ref   0.9874
_refine_ls_shift/su_max          0.0095027
_refine_ls_shift/su_mean         0.7582021


# The values computed from all data 
_oxford_reflns_number_all        14243
_refine_ls_R_factor_all          0.0399
_refine_ls_wR_factor_all         0.0612

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                11684
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_gt          0.0571

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 4.02P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
Besides the organometallic species, there is also some solvate
of crystallization within the structure.   
There are two sites, about 1.5Å apart, which have been interpreted
as being a methanol molecule.  If included with full-occupancy their
 displacement parameters refine to very large values.  Consequently their
occupancies (constrained to be equal to each other)
have been allowed to refine and give a final value of 0.376(7).
An alternative interpretation, not used here,
would be for them to be two mutually exclusive water molecule sites.

Hydrogen atoms were included at idealized positions
and ride on the atom to which they are bonded.
The hydrogen on the methanol O atom is assumed to lie directly on the 
O....Cl vector and the Hs on the methanol C atom are assumed to be staggered
relative to that H.


;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.776408(8) 0.323282(11) 0.511388(7) 0.0221 1.0000 Uani . . . . . . .
Pd2 Pd 0.725970(8) 0.549347(11) 0.558557(7) 0.0234 1.0000 Uani . . . . . . .
Se1 Se 0.678862(10) 0.359454(15) 0.547388(9) 0.0225 1.0000 Uani . . . . . . .
Cl1 Cl 0.87014(3) 0.27458(5) 0.47661(3) 0.0373 1.0000 Uani . . . . . . .
Cl2 Cl 0.64316(3) 0.60313(4) 0.44952(3) 0.0426 1.0000 Uani . . . . . . .
P1 P 0.68061(3) 0.27805(4) 0.41190(2) 0.0251 1.0000 Uani . . . . . . .
P2 P 0.86973(3) 0.36002(4) 0.61593(2) 0.0218 1.0000 Uani . . . . . . .
P3 P 0.78262(3) 0.71671(4) 0.57977(2) 0.0232 1.0000 Uani . . . . . . .
O91 O 0.8728(5) 0.1147(8) 0.3591(5) 0.1549 0.376(7) Uani . . P . . . .
C1 C 0.59080(11) 0.33024(16) 0.40735(9) 0.0259 1.0000 Uani . . . . . . .
C2 C 0.58783(10) 0.35584(15) 0.46636(9) 0.0250 1.0000 Uani . . . . . . .
C3 C 0.51931(11) 0.38659(17) 0.46777(10) 0.0310 1.0000 Uani . . . . . . .
C4 C 0.45482(12) 0.39878(19) 0.40933(11) 0.0359 1.0000 Uani . . . . . . .
C5 C 0.45794(12) 0.3764(2) 0.35044(11) 0.0384 1.0000 Uani . . . . . . .
C6 C 0.52512(12) 0.34109(18) 0.34918(10) 0.0339 1.0000 Uani . . . . . . .
C11 C 0.69105(11) 0.33105(19) 0.34103(10) 0.0329 1.0000 Uani . . . . . . .
C12 C 0.69797(16) 0.4422(2) 0.33712(12) 0.0502 1.0000 Uani . . . . . . .
C13 C 0.70901(18) 0.4872(3) 0.28545(14) 0.0674 1.0000 Uani . . . . . . .
C14 C 0.71378(16) 0.4219(3) 0.23817(14) 0.0680 1.0000 Uani . . . . . . .
C15 C 0.70703(18) 0.3121(3) 0.24155(13) 0.0693 1.0000 Uani . . . . . . .
C16 C 0.69603(16) 0.2655(3) 0.29328(12) 0.0529 1.0000 Uani . . . . . . .
C21 C 0.66638(12) 0.13201(17) 0.40008(10) 0.0316 1.0000 Uani . . . . . . .
C22 C 0.72918(13) 0.06587(18) 0.41207(11) 0.0381 1.0000 Uani . . . . . . .
C23 C 0.72097(16) -0.04601(19) 0.40641(12) 0.0462 1.0000 Uani . . . . . . .
C24 C 0.65035(17) -0.0925(2) 0.38992(12) 0.0507 1.0000 Uani . . . . . . .
C25 C 0.58744(16) -0.0274(2) 0.37786(13) 0.0504 1.0000 Uani . . . . . . .
C26 C 0.59525(14) 0.0844(2) 0.38280(11) 0.0410 1.0000 Uani . . . . . . .
C31 C 0.83815(10) 0.42069(15) 0.67383(9) 0.0231 1.0000 Uani . . . . . . .
C32 C 0.78278(10) 0.50289(15) 0.65242(8) 0.0227 1.0000 Uani . . . . . . .
C33 C 0.76219(11) 0.55050(16) 0.69915(10) 0.0282 1.0000 Uani . . . . . . .
C34 C 0.79539(13) 0.51900(18) 0.76412(10) 0.0345 1.0000 Uani . . . . . . .
C35 C 0.85036(13) 0.43801(19) 0.78462(10) 0.0374 1.0000 Uani . . . . . . .
C36 C 0.87131(12) 0.38901(17) 0.73968(9) 0.0303 1.0000 Uani . . . . . . .
C41 C 0.95221(10) 0.44105(15) 0.62499(9) 0.0252 1.0000 Uani . . . . . . .
C42 C 0.95472(11) 0.49471(16) 0.57170(10) 0.0291 1.0000 Uani . . . . . . .
C43 C 1.01800(13) 0.55780(19) 0.57998(12) 0.0385 1.0000 Uani . . . . . . .
C44 C 1.07857(13) 0.5659(2) 0.64080(13) 0.0456 1.0000 Uani . . . . . . .
C45 C 1.07640(13) 0.5133(2) 0.69392(12) 0.0447 1.0000 Uani . . . . . . .
C46 C 1.01328(12) 0.45176(19) 0.68661(11) 0.0361 1.0000 Uani . . . . . . .
C51 C 0.90822(11) 0.22831(16) 0.65003(9) 0.0269 1.0000 Uani . . . . . . .
C52 C 0.86133(13) 0.15810(17) 0.66548(11) 0.0349 1.0000 Uani . . . . . . .
C53 C 0.88625(15) 0.05487(18) 0.68822(11) 0.0436 1.0000 Uani . . . . . . .
C54 C 0.95704(16) 0.01986(19) 0.69487(12) 0.0496 1.0000 Uani . . . . . . .
C55 C 1.00276(15) 0.0874(2) 0.67829(12) 0.0475 1.0000 Uani . . . . . . .
C56 C 0.97881(13) 0.19230(18) 0.65631(11) 0.0361 1.0000 Uani . . . . . . .
C61 C 0.83895(12) 0.74548(16) 0.53399(10) 0.0292 1.0000 Uani . . . . . . .
C62 C 0.82702(14) 0.6856(2) 0.47817(11) 0.0386 1.0000 Uani . . . . . . .
C63 C 0.86921(16) 0.7086(3) 0.44258(13) 0.0534 1.0000 Uani . . . . . . .
C64 C 0.92270(17) 0.7898(3) 0.46227(15) 0.0638 1.0000 Uani . . . . . . .
C65 C 0.93519(16) 0.8492(3) 0.51737(15) 0.0598 1.0000 Uani . . . . . . .
C66 C 0.89405(13) 0.8272(2) 0.55335(12) 0.0414 1.0000 Uani . . . . . . .
C71 C 0.84811(11) 0.74445(15) 0.66473(9) 0.0270 1.0000 Uani . . . . . . .
C72 C 0.92279(13) 0.70578(18) 0.68963(11) 0.0362 1.0000 Uani . . . . . . .
C73 C 0.97148(15) 0.7212(2) 0.75477(12) 0.0500 1.0000 Uani . . . . . . .
C74 C 0.94687(17) 0.7740(2) 0.79601(12) 0.0550 1.0000 Uani . . . . . . .
C75 C 0.87212(16) 0.81031(19) 0.77245(11) 0.0464 1.0000 Uani . . . . . . .
C76 C 0.82283(13) 0.79602(16) 0.70674(10) 0.0330 1.0000 Uani . . . . . . .
C81 C 0.71446(11) 0.82774(16) 0.56110(9) 0.0269 1.0000 Uani . . . . . . .
C82 C 0.63933(12) 0.8057(2) 0.54995(11) 0.0382 1.0000 Uani . . . . . . .
C83 C 0.58828(15) 0.8892(3) 0.54182(12) 0.0530 1.0000 Uani . . . . . . .
C84 C 0.61118(16) 0.9952(2) 0.54423(12) 0.0558 1.0000 Uani . . . . . . .
C85 C 0.68503(16) 1.0186(2) 0.55374(11) 0.0471 1.0000 Uani . . . . . . .
C86 C 0.73687(13) 0.93576(17) 0.56229(10) 0.0359 1.0000 Uani . . . . . . .
C92 C 0.9005(6) 0.1749(8) 0.3205(8) 0.1207 0.376(7) Uani . . P . . . .
H31 H 0.5166 0.3991 0.5083 0.0371 1.0000 Uiso R . . . . . .
H41 H 0.4083 0.4226 0.4098 0.0431 1.0000 Uiso R . . . . . .
H51 H 0.4136 0.3854 0.3106 0.0460 1.0000 Uiso R . . . . . .
H61 H 0.5266 0.3242 0.3086 0.0407 1.0000 Uiso R . . . . . .
H121 H 0.6952 0.4878 0.3700 0.0602 1.0000 Uiso R . . . . . .
H131 H 0.7133 0.5636 0.2828 0.0809 1.0000 Uiso R . . . . . .
H141 H 0.7218 0.4530 0.2030 0.0816 1.0000 Uiso R . . . . . .
H151 H 0.7099 0.2672 0.2084 0.0832 1.0000 Uiso R . . . . . .
H161 H 0.6920 0.1890 0.2957 0.0634 1.0000 Uiso R . . . . . .
H221 H 0.7781 0.0975 0.4242 0.0457 1.0000 Uiso R . . . . . .
H231 H 0.7640 -0.0905 0.4139 0.0554 1.0000 Uiso R . . . . . .
H241 H 0.6448 -0.1691 0.3868 0.0608 1.0000 Uiso R . . . . . .
H251 H 0.5387 -0.0594 0.3662 0.0605 1.0000 Uiso R . . . . . .
H261 H 0.5518 0.1286 0.3743 0.0492 1.0000 Uiso R . . . . . .
H331 H 0.7245 0.6058 0.6859 0.0339 1.0000 Uiso R . . . . . .
H341 H 0.7805 0.5529 0.7947 0.0414 1.0000 Uiso R . . . . . .
H351 H 0.8734 0.4165 0.8292 0.0448 1.0000 Uiso R . . . . . .
H361 H 0.9086 0.3331 0.7535 0.0364 1.0000 Uiso R . . . . . .
H421 H 0.9133 0.4884 0.5297 0.0349 1.0000 Uiso R . . . . . .
H431 H 1.0195 0.5953 0.5437 0.0462 1.0000 Uiso R . . . . . .
H441 H 1.1220 0.6079 0.6461 0.0547 1.0000 Uiso R . . . . . .
H451 H 1.1183 0.5193 0.7356 0.0536 1.0000 Uiso R . . . . . .
H461 H 1.0115 0.4168 0.7235 0.0433 1.0000 Uiso R . . . . . .
H521 H 0.8122 0.1815 0.6603 0.0419 1.0000 Uiso R . . . . . .
H531 H 0.8546 0.0078 0.6993 0.0523 1.0000 Uiso R . . . . . .
H541 H 0.9742 -0.0509 0.7109 0.0595 1.0000 Uiso R . . . . . .
H551 H 1.0509 0.0623 0.6818 0.0570 1.0000 Uiso R . . . . . .
H561 H 1.0109 0.2391 0.6456 0.0433 1.0000 Uiso R . . . . . .
H621 H 0.7901 0.6292 0.4644 0.0463 1.0000 Uiso R . . . . . .
H631 H 0.8609 0.6678 0.4045 0.0641 1.0000 Uiso R . . . . . .
H641 H 0.9512 0.8051 0.4377 0.0765 1.0000 Uiso R . . . . . .
H651 H 0.9722 0.9054 0.5308 0.0718 1.0000 Uiso R . . . . . .
H661 H 0.9034 0.8681 0.5917 0.0497 1.0000 Uiso R . . . . . .
H721 H 0.9404 0.6686 0.6617 0.0435 1.0000 Uiso R . . . . . .
H731 H 1.0225 0.6951 0.7712 0.0600 1.0000 Uiso R . . . . . .
H741 H 0.9810 0.7855 0.8405 0.0660 1.0000 Uiso R . . . . . .
H751 H 0.8545 0.8450 0.8011 0.0557 1.0000 Uiso R . . . . . .
H761 H 0.7717 0.8216 0.6906 0.0396 1.0000 Uiso R . . . . . .
H821 H 0.6229 0.7327 0.5479 0.0459 1.0000 Uiso R . . . . . .
H831 H 0.5372 0.8732 0.5346 0.0636 1.0000 Uiso R . . . . . .
H841 H 0.5762 1.0524 0.5394 0.0670 1.0000 Uiso R . . . . . .
H851 H 0.7004 1.0919 0.5544 0.0565 1.0000 Uiso R . . . . . .
H861 H 0.7877 0.9524 0.5690 0.0430 1.0000 Uiso R . . . . . .
H911 H 0.8721 0.1604 0.3927 0.1862 0.376 Uiso R . . . . . .
H921 H 0.9016 0.1301 0.2866 0.1442 0.376 Uiso R . . . . . .
H922 H 0.9506 0.2000 0.3470 0.1442 0.376 Uiso R . . . . . .
H923 H 0.8679 0.2351 0.3018 0.1442 0.376 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.19543(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Pd2 . 3.2760(2) yes
Pd1 . Se1 . 2.3872(2) yes
Pd1 . Cl1 . 2.3350(5) yes
Pd1 . P1 . 2.2949(5) yes
Pd1 . P2 . 2.3296(5) yes
Pd2 . Se1 . 2.4869(2) yes
Pd2 . Cl2 . 2.3933(5) yes
Pd2 . P3 . 2.2905(5) yes
Pd2 . C32 . 2.0137(17) yes
Se1 . C2 . 1.9291(18) yes
P1 . C1 . 1.812(2) yes
P1 . C11 . 1.815(2) yes
P1 . C21 . 1.825(2) yes
P2 . C31 . 1.8193(19) yes
P2 . C41 . 1.8176(19) yes
P2 . C51 . 1.817(2) yes
P3 . C61 . 1.823(2) yes
P3 . C71 . 1.8286(19) yes
P3 . C81 . 1.822(2) yes
O91 . C92 . 1.411(16) yes
O91 . H911 . 0.950 no
C1 . C2 . 1.393(3) yes
C1 . C6 . 1.394(3) yes
C2 . C3 . 1.390(3) yes
C3 . C4 . 1.388(3) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.383(3) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.380(3) yes
C5 . H51 . 0.950 no
C6 . H61 . 0.950 no
C11 . C12 . 1.384(3) yes
C11 . C16 . 1.382(3) yes
C12 . C13 . 1.386(3) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.370(5) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.365(5) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.396(4) yes
C15 . H151 . 0.950 no
C16 . H161 . 0.950 no
C21 . C22 . 1.390(3) yes
C21 . C26 . 1.390(3) yes
C22 . C23 . 1.389(3) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.378(4) yes
C23 . H231 . 0.950 no
C24 . C25 . 1.385(4) yes
C24 . H241 . 0.950 no
C25 . C26 . 1.386(3) yes
C25 . H251 . 0.950 no
C26 . H261 . 0.950 no
C31 . C32 . 1.403(3) yes
C31 . C36 . 1.402(3) yes
C32 . C33 . 1.403(3) yes
C33 . C34 . 1.384(3) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.387(3) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.380(3) yes
C35 . H351 . 0.950 no
C36 . H361 . 0.950 no
C41 . C42 . 1.391(3) yes
C41 . C46 . 1.399(3) yes
C42 . C43 . 1.393(3) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.381(3) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.379(3) yes
C44 . H441 . 0.950 no
C45 . C46 . 1.386(3) yes
C45 . H451 . 0.950 no
C46 . H461 . 0.950 no
C51 . C52 . 1.399(3) yes
C51 . C56 . 1.383(3) yes
C52 . C53 . 1.381(3) yes
C52 . H521 . 0.950 no
C53 . C54 . 1.380(4) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.375(4) yes
C54 . H541 . 0.950 no
C55 . C56 . 1.394(3) yes
C55 . H551 . 0.950 no
C56 . H561 . 0.950 no
C61 . C62 . 1.392(3) yes
C61 . C66 . 1.395(3) yes
C62 . C63 . 1.393(3) yes
C62 . H621 . 0.950 no
C63 . C64 . 1.372(4) yes
C63 . H631 . 0.950 no
C64 . C65 . 1.373(4) yes
C64 . H641 . 0.950 no
C65 . C66 . 1.381(3) yes
C65 . H651 . 0.950 no
C66 . H661 . 0.950 no
C71 . C72 . 1.393(3) yes
C71 . C76 . 1.390(3) yes
C72 . C73 . 1.383(3) yes
C72 . H721 . 0.950 no
C73 . C74 . 1.374(4) yes
C73 . H731 . 0.950 no
C74 . C75 . 1.385(4) yes
C74 . H741 . 0.950 no
C75 . C76 . 1.394(3) yes
C75 . H751 . 0.950 no
C76 . H761 . 0.950 no
C81 . C82 . 1.391(3) yes
C81 . C86 . 1.398(3) yes
C82 . C83 . 1.383(3) yes
C82 . H821 . 0.950 no
C83 . C84 . 1.374(4) yes
C83 . H831 . 0.950 no
C84 . C85 . 1.380(4) yes
C84 . H841 . 0.950 no
C85 . C86 . 1.386(3) yes
C85 . H851 . 0.950 no
C86 . H861 . 0.950 no
C92 . H921 . 0.950 no
C92 . H922 . 0.950 no
C92 . H923 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pd2 . Pd1 . Se1 . 49.074(6) yes
Pd2 . Pd1 . Cl1 . 134.998(15) yes
Se1 . Pd1 . Cl1 . 175.863(16) yes
Pd2 . Pd1 . P1 . 107.283(14) yes
Se1 . Pd1 . P1 . 87.241(14) yes
Cl1 . Pd1 . P1 . 91.617(19) yes
Pd2 . Pd1 . P2 . 73.424(13) yes
Se1 . Pd1 . P2 . 90.214(13) yes
Cl1 . Pd1 . P2 . 90.682(18) yes
P1 . Pd1 . P2 . 175.731(18) yes
Pd1 . Pd2 . Se1 . 46.490(5) yes
Pd1 . Pd2 . Cl2 . 93.641(15) yes
Se1 . Pd2 . Cl2 . 95.726(14) yes
Pd1 . Pd2 . P3 . 130.830(14) yes
Se1 . Pd2 . P3 . 172.845(14) yes
Cl2 . Pd2 . P3 . 91.029(18) yes
Pd1 . Pd2 . C32 . 89.69(5) yes
Se1 . Pd2 . C32 . 81.50(5) yes
Cl2 . Pd2 . C32 . 172.24(5) yes
P3 . Pd2 . C32 . 92.10(5) yes
Pd2 . Se1 . Pd1 . 84.436(7) yes
Pd2 . Se1 . C2 . 105.42(6) yes
Pd1 . Se1 . C2 . 101.99(6) yes
Pd1 . P1 . C1 . 109.05(6) yes
Pd1 . P1 . C11 . 115.48(7) yes
C1 . P1 . C11 . 106.35(9) yes
Pd1 . P1 . C21 . 113.10(7) yes
C1 . P1 . C21 . 105.13(10) yes
C11 . P1 . C21 . 107.02(10) yes
Pd1 . P2 . C31 . 117.14(6) yes
Pd1 . P2 . C41 . 119.19(6) yes
C31 . P2 . C41 . 103.67(9) yes
Pd1 . P2 . C51 . 104.96(6) yes
C31 . P2 . C51 . 105.37(9) yes
C41 . P2 . C51 . 105.17(9) yes
Pd2 . P3 . C61 . 113.81(7) yes
Pd2 . P3 . C71 . 116.47(6) yes
C61 . P3 . C71 . 104.07(9) yes
Pd2 . P3 . C81 . 113.24(7) yes
C61 . P3 . C81 . 105.57(9) yes
C71 . P3 . C81 . 102.37(9) yes
C92 . O91 . H911 . 108.6 no
P1 . C1 . C2 . 116.81(14) yes
P1 . C1 . C6 . 123.80(16) yes
C2 . C1 . C6 . 119.32(18) yes
C1 . C2 . Se1 . 121.49(14) yes
C1 . C2 . C3 . 120.49(17) yes
Se1 . C2 . C3 . 117.89(14) yes
C2 . C3 . C4 . 119.30(19) yes
C2 . C3 . H31 . 120.4 no
C4 . C3 . H31 . 120.4 no
C3 . C4 . C5 . 120.4(2) yes
C3 . C4 . H41 . 119.8 no
C5 . C4 . H41 . 119.8 no
C4 . C5 . C6 . 120.35(19) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 119.8 no
C1 . C6 . C5 . 120.0(2) yes
C1 . C6 . H61 . 120.0 no
C5 . C6 . H61 . 120.0 no
P1 . C11 . C12 . 117.56(17) yes
P1 . C11 . C16 . 123.1(2) yes
C12 . C11 . C16 . 119.3(2) yes
C11 . C12 . C13 . 120.2(3) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C14 . 120.2(3) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 119.9 no
C13 . C14 . C15 . 120.0(3) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 120.5(3) yes
C14 . C15 . H151 . 119.8 no
C16 . C15 . H151 . 119.8 no
C15 . C16 . C11 . 119.7(3) yes
C15 . C16 . H161 . 120.2 no
C11 . C16 . H161 . 120.2 no
P1 . C21 . C22 . 119.06(16) yes
P1 . C21 . C26 . 121.90(18) yes
C22 . C21 . C26 . 118.9(2) yes
C21 . C22 . C23 . 120.6(2) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 119.7 no
C22 . C23 . C24 . 120.0(2) yes
C22 . C23 . H231 . 120.0 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 119.8(2) yes
C23 . C24 . H241 . 120.1 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 120.3(2) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 119.8 no
C21 . C26 . C25 . 120.3(2) yes
C21 . C26 . H261 . 119.9 no
C25 . C26 . H261 . 119.9 no
P2 . C31 . C32 . 119.20(13) yes
P2 . C31 . C36 . 120.28(15) yes
C32 . C31 . C36 . 120.45(17) yes
C31 . C32 . Pd2 . 124.43(13) yes
C31 . C32 . C33 . 117.42(16) yes
Pd2 . C32 . C33 . 118.00(14) yes
C32 . C33 . C34 . 121.76(19) yes
C32 . C33 . H331 . 119.1 no
C34 . C33 . H331 . 119.1 no
C33 . C34 . C35 . 120.16(19) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 119.9 no
C34 . C35 . C36 . 119.41(19) yes
C34 . C35 . H351 . 120.3 no
C36 . C35 . H351 . 120.3 no
C31 . C36 . C35 . 120.80(19) yes
C31 . C36 . H361 . 119.6 no
C35 . C36 . H361 . 119.6 no
P2 . C41 . C42 . 120.86(14) yes
P2 . C41 . C46 . 119.68(15) yes
C42 . C41 . C46 . 119.44(18) yes
C41 . C42 . C43 . 119.90(19) yes
C41 . C42 . H421 . 120.0 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 120.1(2) yes
C42 . C43 . H431 . 120.0 no
C44 . C43 . H431 . 120.0 no
C43 . C44 . C45 . 120.4(2) yes
C43 . C44 . H441 . 119.8 no
C45 . C44 . H441 . 119.8 no
C44 . C45 . C46 . 120.2(2) yes
C44 . C45 . H451 . 119.9 no
C46 . C45 . H451 . 119.9 no
C41 . C46 . C45 . 120.0(2) yes
C41 . C46 . H461 . 120.0 no
C45 . C46 . H461 . 120.0 no
P2 . C51 . C52 . 117.83(16) yes
P2 . C51 . C56 . 122.68(16) yes
C52 . C51 . C56 . 119.29(19) yes
C51 . C52 . C53 . 120.2(2) yes
C51 . C52 . H521 . 119.9 no
C53 . C52 . H521 . 119.9 no
C52 . C53 . C54 . 120.2(2) yes
C52 . C53 . H531 . 119.9 no
C54 . C53 . H531 . 119.9 no
C53 . C54 . C55 . 120.1(2) yes
C53 . C54 . H541 . 120.0 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 120.3(2) yes
C54 . C55 . H551 . 119.9 no
C56 . C55 . H551 . 119.9 no
C55 . C56 . C51 . 120.0(2) yes
C55 . C56 . H561 . 120.0 no
C51 . C56 . H561 . 120.0 no
P3 . C61 . C62 . 119.90(17) yes
P3 . C61 . C66 . 121.46(16) yes
C62 . C61 . C66 . 118.6(2) yes
C61 . C62 . C63 . 120.0(2) yes
C61 . C62 . H621 . 120.0 no
C63 . C62 . H621 . 120.0 no
C62 . C63 . C64 . 120.4(3) yes
C62 . C63 . H631 . 119.8 no
C64 . C63 . H631 . 119.8 no
C63 . C64 . C65 . 120.2(2) yes
C63 . C64 . H641 . 119.9 no
C65 . C64 . H641 . 119.9 no
C64 . C65 . C66 . 120.2(3) yes
C64 . C65 . H651 . 119.9 no
C66 . C65 . H651 . 119.9 no
C61 . C66 . C65 . 120.6(2) yes
C61 . C66 . H661 . 119.7 no
C65 . C66 . H661 . 119.7 no
P3 . C71 . C72 . 119.94(16) yes
P3 . C71 . C76 . 120.91(16) yes
C72 . C71 . C76 . 118.93(19) yes
C71 . C72 . C73 . 120.4(2) yes
C71 . C72 . H721 . 119.8 no
C73 . C72 . H721 . 119.8 no
C72 . C73 . C74 . 120.7(2) yes
C72 . C73 . H731 . 119.7 no
C74 . C73 . H731 . 119.7 no
C73 . C74 . C75 . 119.7(2) yes
C73 . C74 . H741 . 120.1 no
C75 . C74 . H741 . 120.1 no
C74 . C75 . C76 . 120.0(2) yes
C74 . C75 . H751 . 120.0 no
C76 . C75 . H751 . 120.0 no
C75 . C76 . C71 . 120.3(2) yes
C75 . C76 . H761 . 119.9 no
C71 . C76 . H761 . 119.9 no
P3 . C81 . C82 . 119.48(16) yes
P3 . C81 . C86 . 121.65(16) yes
C82 . C81 . C86 . 118.7(2) yes
C81 . C82 . C83 . 120.6(2) yes
C81 . C82 . H821 . 119.7 no
C83 . C82 . H821 . 119.7 no
C82 . C83 . C84 . 120.2(3) yes
C82 . C83 . H831 . 119.9 no
C84 . C83 . H831 . 119.9 no
C83 . C84 . C85 . 119.9(2) yes
C83 . C84 . H841 . 120.0 no
C85 . C84 . H841 . 120.0 no
C84 . C85 . C86 . 120.4(2) yes
C84 . C85 . H851 . 119.8 no
C86 . C85 . H851 . 119.8 no
C81 . C86 . C85 . 120.0(2) yes
C81 . C86 . H861 . 120.0 no
C85 . C86 . H861 . 120.0 no
O91 . C92 . H921 . 109.5 no
O91 . C92 . H922 . 109.5 no
H921 . C92 . H922 . 109.5 no
O91 . C92 . H923 . 109.5 no
H921 . C92 . H923 . 109.5 no
H922 . C92 . H923 . 109.5 no



#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 O91 3.32(1) . . no
Cl1 C43 3.592(3) . 2_766 no
O91 C14 3.19(1) . 3_645 no
O91 C13 3.35(1) . 3_645 no
O91 C22 3.50(1) . . no
C3 C3 3.378(4) . 2_666 no
C4 C82 3.453(4) . 2_666 no
C5 C53 3.428(3) . 4_454 no
C6 C54 3.595(3) . 4_454 no
C13 C92 3.36(1) . 3_655 no
C23 C86 3.405(4) . 1_545 no
C24 C86 3.542(3) . 1_545 no
C25 C84 3.594(4) . 1_545 no
C26 C85 3.590(3) . 1_545 no
C44 C92 3.29(1) . 2_766 no
C53 C86 3.411(3) . 1_545 no
C53 C76 3.507(3) . 1_545 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 Pd2 Cl2 . . . . 89.59(2) no
Pd1 Se1 Pd2 C32 . . . . -97.72(6) no
Pd1 Se1 C2 C1 . . . . 3.3(2) no
Pd1 Se1 C2 C3 . . . . -172.6(1) no
Pd1 P1 C1 C2 . . . . -19.4(2) no
Pd1 P1 C1 C6 . . . . 163.5(2) no
Pd1 P1 C11 C12 . . . . -56.9(2) no
Pd1 P1 C11 C16 . . . . 119.9(2) no
Pd1 P1 C21 C22 . . . . -50.1(2) no
Pd1 P1 C21 C26 . . . . 126.4(2) no
Pd1 P2 C31 C32 . . . . -41.5(2) no
Pd1 P2 C31 C36 . . . . 141.4(1) no
Pd1 P2 C41 C42 . . . . 9.9(2) no
Pd1 P2 C41 C46 . . . . -171.6(2) no
Pd1 P2 C51 C52 . . . . -69.9(2) no
Pd1 P2 C51 C56 . . . . 105.0(2) no
Pd2 Se1 Pd1 P1 . . . . -115.81(1) no
Pd2 Se1 Pd1 P2 . . . . 67.61(1) no
Pd2 Se1 C2 C1 . . . . 90.7(2) no
Pd2 Se1 C2 C3 . . . . -85.1(2) no
Pd2 P3 C61 C62 . . . . 18.9(2) no
Pd2 P3 C61 C66 . . . . -161.4(1) no
Pd2 P3 C71 C72 . . . . 80.7(2) no
Pd2 P3 C71 C76 . . . . -93.9(2) no
Pd2 P3 C81 C82 . . . . 13.5(2) no
Pd2 P3 C81 C86 . . . . -171.2(2) no
Pd2 C32 C31 P2 . . . . 7.0(2) no
Pd2 C32 C31 C36 . . . . -175.9(2) no
Pd2 C32 C33 C34 . . . . 176.4(2) no
Se1 Pd1 P1 C1 . . . . 16.47(7) no
Se1 Pd1 P1 C11 . . . . 136.11(9) no
Se1 Pd1 P1 C21 . . . . -100.1(1) no
Se1 Pd1 P2 C31 . . . . -10.66(7) no
Se1 Pd1 P2 C41 . . . . -136.87(8) no
Se1 Pd1 P2 C51 . . . . 105.78(8) no
Se1 Pd2 C32 C31 . . . . 63.1(2) no
Se1 Pd2 C32 C33 . . . . -112.4(2) no
Se1 C2 C1 P1 . . . . 10.3(2) no
Se1 C2 C1 C6 . . . . -172.5(2) no
Se1 C2 C3 C4 . . . . 171.5(2) no
Cl1 Pd1 P1 C1 . . . . -167.51(8) no
Cl1 Pd1 P1 C11 . . . . -47.87(9) no
Cl1 Pd1 P1 C21 . . . . 75.9(1) no
Cl1 Pd1 P2 C31 . . . . 173.38(7) no
Cl1 Pd1 P2 C41 . . . . 47.17(8) no
Cl1 Pd1 P2 C51 . . . . -70.18(9) no
Cl2 Pd2 Se1 C2 . . . . -11.35(7) no
Cl2 Pd2 P3 C61 . . . . -67.93(7) no
Cl2 Pd2 P3 C71 . . . . 170.97(9) no
Cl2 Pd2 P3 C81 . . . . 52.65(8) no
P1 Pd1 Se1 C2 . . . . -11.19(6) no
P1 C1 C2 C3 . . . . -173.9(2) no
P1 C1 C6 C5 . . . . 176.7(2) no
P1 C11 C12 C13 . . . . 177.5(2) no
P1 C11 C16 C15 . . . . -177.5(2) no
P1 C21 C22 C23 . . . . 177.1(2) no
P1 C21 C26 C25 . . . . -176.3(2) no
P2 Pd1 Se1 C2 . . . . 172.23(6) no
P2 C31 C32 C33 . . . . -177.5(1) no
P2 C31 C36 C35 . . . . 177.0(2) no
P2 C41 C42 C43 . . . . 179.0(2) no
P2 C41 C46 C45 . . . . 179.9(2) no
P2 C51 C52 C53 . . . . 176.5(2) no
P2 C51 C56 C55 . . . . -175.2(2) no
P3 Pd2 C32 C31 . . . . -113.7(2) no
P3 Pd2 C32 C33 . . . . 70.8(2) no
P3 C61 C62 C63 . . . . 179.0(2) no
P3 C61 C66 C65 . . . . -178.8(2) no
P3 C71 C72 C73 . . . . -176.4(2) no
P3 C71 C76 C75 . . . . 175.8(2) no
P3 C81 C82 C83 . . . . 173.8(2) no
P3 C81 C86 C85 . . . . -174.1(2) no
C1 P1 C11 C12 . . . . 64.2(2) no
C1 P1 C11 C16 . . . . -119.0(2) no
C1 P1 C21 C22 . . . . -169.0(2) no
C1 P1 C21 C26 . . . . 7.5(2) no
C1 C2 C3 C4 . . . . -4.4(3) no
C1 C6 C5 C4 . . . . -1.5(4) no
C2 Se1 Pd2 C32 . . . . 161.3(1) no
C2 C1 P1 C11 . . . . -144.6(2) no
C2 C1 P1 C21 . . . . 102.2(2) no
C2 C1 C6 C5 . . . . -0.3(3) no
C2 C3 C4 C5 . . . . 2.6(3) no
C3 C2 C1 C6 . . . . 3.3(3) no
C3 C4 C5 C6 . . . . 0.4(4) no
C6 C1 P1 C11 . . . . 38.4(2) no
C6 C1 P1 C21 . . . . -74.9(2) no
C11 P1 C21 C22 . . . . 78.2(2) no
C11 P1 C21 C26 . . . . -105.3(2) no
C11 C12 C13 C14 . . . . -0.5(4) no
C11 C16 C15 C14 . . . . 0.8(4) no
C12 C11 P1 C21 . . . . 176.2(2) no
C12 C11 C16 C15 . . . . -0.7(4) no
C12 C13 C14 C15 . . . . 0.5(4) no
C13 C12 C11 C16 . . . . 0.6(4) no
C13 C14 C15 C16 . . . . -0.6(4) no
C16 C11 P1 C21 . . . . -7.0(2) no
C21 C22 C23 C24 . . . . -1.2(4) no
C21 C26 C25 C24 . . . . -0.2(4) no
C22 C21 C26 C25 . . . . 0.2(4) no
C22 C23 C24 C25 . . . . 1.2(4) no
C23 C22 C21 C26 . . . . 0.5(4) no
C23 C24 C25 C26 . . . . -0.5(4) no
C31 P2 C41 C42 . . . . -122.5(2) no
C31 P2 C41 C46 . . . . 56.0(2) no
C31 P2 C51 C52 . . . . 54.4(2) no
C31 P2 C51 C56 . . . . -130.8(2) no
C31 C32 C33 C34 . . . . 0.6(3) no
C31 C36 C35 C34 . . . . 0.5(3) no
C32 Pd2 P3 C61 . . . . 119.17(9) no
C32 Pd2 P3 C71 . . . . -1.9(1) no
C32 Pd2 P3 C81 . . . . -120.2(1) no
C32 C31 P2 C41 . . . . 92.1(2) no
C32 C31 P2 C51 . . . . -157.7(1) no
C32 C31 C36 C35 . . . . -0.1(3) no
C32 C33 C34 C35 . . . . -0.3(3) no
C33 C32 C31 C36 . . . . -0.4(3) no
C33 C34 C35 C36 . . . . -0.3(3) no
C36 C31 P2 C41 . . . . -85.1(2) no
C36 C31 P2 C51 . . . . 25.2(2) no
C41 P2 C51 C52 . . . . 163.6(2) no
C41 P2 C51 C56 . . . . -21.6(2) no
C41 C42 C43 C44 . . . . 0.9(4) no
C41 C46 C45 C44 . . . . 1.3(4) no
C42 C41 P2 C51 . . . . 127.1(2) no
C42 C41 C46 C45 . . . . -1.5(3) no
C42 C43 C44 C45 . . . . -1.1(4) no
C43 C42 C41 C46 . . . . 0.5(3) no
C43 C44 C45 C46 . . . . 0.0(4) no
C46 C41 P2 C51 . . . . -54.4(2) no
C51 C52 C53 C54 . . . . -1.0(3) no
C51 C56 C55 C54 . . . . -1.1(3) no
C52 C51 C56 C55 . . . . -0.5(3) no
C52 C53 C54 C55 . . . . -0.6(4) no
C53 C52 C51 C56 . . . . 1.5(3) no
C53 C54 C55 C56 . . . . 1.6(4) no
C61 P3 C71 C72 . . . . -45.4(2) no
C61 P3 C71 C76 . . . . 140.0(2) no
C61 P3 C81 C82 . . . . 138.7(2) no
C61 P3 C81 C86 . . . . -46.0(2) no
C61 C62 C63 C64 . . . . 0.2(4) no
C61 C66 C65 C64 . . . . -0.6(4) no
C62 C61 P3 C71 . . . . 146.7(2) no
C62 C61 P3 C81 . . . . -105.9(2) no
C62 C61 C66 C65 . . . . 0.9(3) no
C62 C63 C64 C65 . . . . 0.0(5) no
C63 C62 C61 C66 . . . . -0.6(3) no
C63 C64 C65 C66 . . . . 0.2(5) no
C66 C61 P3 C71 . . . . -33.6(2) no
C66 C61 P3 C81 . . . . 73.8(2) no
C71 P3 C81 C82 . . . . -112.7(2) no
C71 P3 C81 C86 . . . . 62.6(2) no
C71 C72 C73 C74 . . . . 0.5(4) no
C71 C76 C75 C74 . . . . 0.6(4) no
C72 C71 P3 C81 . . . . -155.2(2) no
C72 C71 C76 C75 . . . . 1.1(3) no
C72 C73 C74 C75 . . . . 1.3(4) no
C73 C72 C71 C76 . . . . -1.7(3) no
C73 C74 C75 C76 . . . . -1.8(4) no
C76 C71 P3 C81 . . . . 30.2(2) no
C81 C82 C83 C84 . . . . 0.5(4) no
C81 C86 C85 C84 . . . . 0.2(4) no
C82 C81 C86 C85 . . . . 1.3(3) no
C82 C83 C84 C85 . . . . 1.0(4) no
C83 C82 C81 C86 . . . . -1.6(3) no
C83 C84 C85 C86 . . . . -1.4(4) no
#------------------------------------------------------------------------------
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O91 H911 Cl1 0.95 2.37 3.32(1) 179.9 . no
_database_code_depnum_ccdc_archive 'CCDC 999168'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex16
_audit_creation_date             10-03-16
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2010-05-21 - Report on C59 H55 Cl4 O P3 Pd2 Se 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2010-05-21 - passes checkcif tests with minor warnings  
;



_oxford_structure_analysis_title '3161117 ben1002'
_chemical_name_systematic        ?
_chemical_melting_point          ?

#end of refcif 
_cell_length_a                   12.3871(2)
_cell_length_b                   12.4707(2)
_cell_length_c                   19.1951(4)
_cell_angle_alpha                74.7759(8)
_cell_angle_beta                 86.7437(11)
_cell_angle_gamma                76.0615(11)
_cell_volume                     2776.81(9)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C59 H55 Cl4 O1 P3 Pd2 Se1 
# Dc =      1.56 Fooo =   1312.00 Mu =     16.22 M =   1306.58
# Found Formula = C59 H55 Cl4 O1 P3 Pd2 Se1 
# Dc =      1.56 FOOO =   1312.00 Mu =     16.22 M =   1306.58

_chemical_formula_sum            'C59 H55 Cl4 O P3 Pd2 Se'
_chemical_formula_moiety         'C57 H49 Cl2 P3 Pd2 Se, C H2 Cl2, C H4 O'
_chemical_compound_source        ' from RMIT University'
_chemical_formula_weight         1306.58


_cell_measurement_reflns_used    50247
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.090
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_max          0.350

_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    1.622

# Sheldrick geometric approximatio 0.73 0.86 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.160
-1 0 0 0.190
0 1 0 0.001
0 -1 0 0.090
0 0 1 0.080
0 0 -1 0.110
-2 0 -3 0.152
-2 -3 0 0.147


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.042

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.6 deg at rate 64 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            54754
_reflns_number_total             12702
_diffrn_reflns_av_R_equivalents  0.051
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 12702 
# Theoretical number of reflections is about 25502 


_diffrn_reflns_theta_min         2.586
_diffrn_reflns_theta_max         27.494
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        27.494
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              -15
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      15.07

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -1.02
_refine_diff_density_max         1.07


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     6
_refine_ls_number_parameters     642
_oxford_refine_ls_R_factor_ref   0.0510
_refine_ls_wR_factor_ref         0.0995
_refine_ls_goodness_of_fit_ref   0.9964
_refine_ls_shift/su_max          0.0064696
_refine_ls_shift/su_mean         0.0006 # 0.0570270 


# The values computed from all data 
_oxford_reflns_number_all        12702
_refine_ls_R_factor_all          0.0510
_refine_ls_wR_factor_all         0.0995

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10343
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_gt          0.0921

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 3.91P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
#_publ_section_exptl_refinement 
# see also _refine_ls_hydrogen for refinement keywords.                         

;

Hydrogen atoms of the organometallic species
 were included at idealized positions,
with methyl groups oriented to best-match peaks in 
difference electron density maps.
These H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.
H atoms of the dichloromethane were included at idealized positions
and ride on the atom to which they are bonded.
H atoms of the methanol molecule were included 
at positions to best-match peaks in a difference map and to minimise close 
contacts with adjacent H atoms, 
and then ride on the atoms to which they are bonded.


The largest peaks in the final difference electron density map
were located near disorder or appear to be weak images of the heavy atoms
generated by non-crystallographic symmetry.

;



# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.28089(2) 0.61068(2) 0.727284(13) 0.0288 1.0000 Uani . . . . . . .
Pd2 Pd 0.484486(18) 0.57187(2) 0.832599(13) 0.0262 1.0000 Uani . . . . . . .
Se1 Se 0.28107(2) 0.61264(3) 0.852086(16) 0.0273 1.0000 Uani . . . . . . .
Cl1 Cl 0.26931(9) 0.61994(9) 0.60456(5) 0.0529 1.0000 Uani . . . . . . .
Cl2 Cl 0.49726(7) 0.76789(7) 0.79237(5) 0.0395 1.0000 Uani . . . . . . .
Cl3 Cl 0.00794(13) 0.69276(18) 0.48281(8) 0.0969 1.0000 Uani . . . . . . .
Cl41 Cl 0.0957(4) 0.8598(9) 0.3740(4) 0.0954 0.63(3) Uani . U P . . . .
Cl42 Cl 0.1220(15) 0.807(2) 0.3604(6) 0.1053 0.37(3) Uani . U P . . . .
P1 P 0.18694(7) 0.79779(7) 0.70555(5) 0.0316 1.0000 Uani . . . . . . .
P2 P 0.35487(6) 0.41280(7) 0.75747(4) 0.0269 1.0000 Uani . . . . . . .
P3 P 0.66738(6) 0.51261(7) 0.80689(4) 0.0261 1.0000 Uani . . . . . . .
O91 O 0.4725(3) 0.9803(3) 0.8590(2) 0.0696 0.60(2) Uani . . P . . . .
O92 O 0.5870(4) 0.9658(4) 0.8579(3) 0.0891 0.40(2) Uani . . P . . . .
C1 C 0.2061(3) 0.8545(3) 0.78068(18) 0.0331 1.0000 Uani . . . . . . .
C2 C 0.2394(3) 0.7743(3) 0.84582(18) 0.0308 1.0000 Uani . . . . . . .
C3 C 0.2504(3) 0.8102(3) 0.90707(19) 0.0352 1.0000 Uani . . . . . . .
C4 C 0.2322(3) 0.9259(3) 0.9023(2) 0.0411 1.0000 Uani . . . . . . .
C5 C 0.2016(3) 1.0058(3) 0.8371(2) 0.0414 1.0000 Uani . . . . . . .
C6 C 0.1873(3) 0.9705(3) 0.7765(2) 0.0410 1.0000 Uani . . . . . . .
C11 C 0.2258(3) 0.8952(3) 0.62538(19) 0.0371 1.0000 Uani . . . . . . .
C12 C 0.3296(4) 0.9190(4) 0.6242(2) 0.0616 1.0000 Uani . . . . . . .
C13 C 0.3636(4) 0.9900(5) 0.5626(3) 0.0748 1.0000 Uani . . . . . . .
C14 C 0.2952(4) 1.0368(4) 0.5032(3) 0.0668 1.0000 Uani . . . . . . .
C15 C 0.1920(4) 1.0129(4) 0.5044(2) 0.0656 1.0000 Uani . . . . . . .
C16 C 0.1575(4) 0.9426(4) 0.5655(2) 0.0518 1.0000 Uani . . . . . . .
C21 C 0.0374(3) 0.8120(3) 0.69966(19) 0.0358 1.0000 Uani . . . . . . .
C22 C -0.0029(3) 0.7486(3) 0.6623(2) 0.0421 1.0000 Uani . . . . . . .
C23 C -0.1162(3) 0.7567(3) 0.6590(2) 0.0479 1.0000 Uani . . . . . . .
C24 C -0.1896(3) 0.8254(4) 0.6932(2) 0.0523 1.0000 Uani . . . . . . .
C25 C -0.1502(4) 0.8876(5) 0.7309(3) 0.0689 1.0000 Uani . . . . . . .
C26 C -0.0382(3) 0.8816(4) 0.7345(3) 0.0594 1.0000 Uani . . . . . . .
C31 C 0.4178(3) 0.3487(3) 0.84690(17) 0.0283 1.0000 Uani . . . . . . .
C32 C 0.4730(2) 0.4106(3) 0.87787(17) 0.0273 1.0000 Uani . . . . . . .
C33 C 0.5158(3) 0.3595(3) 0.94799(18) 0.0324 1.0000 Uani . . . . . . .
C34 C 0.5053(3) 0.2519(3) 0.98544(19) 0.0388 1.0000 Uani . . . . . . .
C35 C 0.4535(3) 0.1901(3) 0.9528(2) 0.0420 1.0000 Uani . . . . . . .
C36 C 0.4099(3) 0.2381(3) 0.88402(19) 0.0350 1.0000 Uani . . . . . . .
C41 C 0.4483(3) 0.3475(3) 0.69527(18) 0.0335 1.0000 Uani . . . . . . .
C42 C 0.4965(3) 0.4128(4) 0.6377(2) 0.0410 1.0000 Uani . . . . . . .
C43 C 0.5648(3) 0.3624(4) 0.5899(2) 0.0546 1.0000 Uani . . . . . . .
C44 C 0.5875(4) 0.2461(5) 0.5993(3) 0.0617 1.0000 Uani . . . . . . .
C45 C 0.5434(4) 0.1792(4) 0.6574(3) 0.0622 1.0000 Uani . . . . . . .
C46 C 0.4734(3) 0.2284(3) 0.7055(2) 0.0477 1.0000 Uani . . . . . . .
C51 C 0.2318(3) 0.3556(3) 0.76118(18) 0.0319 1.0000 Uani . . . . . . .
C52 C 0.1613(3) 0.3568(3) 0.8198(2) 0.0429 1.0000 Uani . . . . . . .
C53 C 0.0636(3) 0.3196(4) 0.8223(3) 0.0501 1.0000 Uani . . . . . . .
C54 C 0.0354(3) 0.2836(3) 0.7655(2) 0.0476 1.0000 Uani . . . . . . .
C55 C 0.1035(4) 0.2832(4) 0.7065(2) 0.0534 1.0000 Uani . . . . . . .
C56 C 0.2018(3) 0.3196(4) 0.7043(2) 0.0442 1.0000 Uani . . . . . . .
C61 C 0.6913(3) 0.5500(3) 0.70988(17) 0.0311 1.0000 Uani . . . . . . .
C62 C 0.6107(3) 0.6326(3) 0.66388(19) 0.0369 1.0000 Uani . . . . . . .
C63 C 0.6253(3) 0.6598(3) 0.5902(2) 0.0448 1.0000 Uani . . . . . . .
C64 C 0.7203(3) 0.6082(3) 0.55914(19) 0.0437 1.0000 Uani . . . . . . .
C65 C 0.8007(3) 0.5267(3) 0.6048(2) 0.0451 1.0000 Uani . . . . . . .
C66 C 0.7868(3) 0.4978(3) 0.67862(19) 0.0370 1.0000 Uani . . . . . . .
C67 C 0.7341(4) 0.6372(4) 0.4787(2) 0.0623 1.0000 Uani . . . . . . .
C71 C 0.7322(2) 0.3601(3) 0.83456(17) 0.0284 1.0000 Uani . . . . . . .
C72 C 0.7134(3) 0.2862(3) 0.79601(19) 0.0356 1.0000 Uani . . . . . . .
C73 C 0.7607(3) 0.1702(3) 0.8179(2) 0.0394 1.0000 Uani . . . . . . .
C74 C 0.8269(3) 0.1232(3) 0.8797(2) 0.0385 1.0000 Uani . . . . . . .
C75 C 0.8449(3) 0.1967(3) 0.91885(19) 0.0364 1.0000 Uani . . . . . . .
C76 C 0.7981(3) 0.3129(3) 0.89702(17) 0.0307 1.0000 Uani . . . . . . .
C77 C 0.8793(4) -0.0029(3) 0.9048(3) 0.0560 1.0000 Uani . . . . . . .
C81 C 0.7574(3) 0.5726(3) 0.84970(17) 0.0284 1.0000 Uani . . . . . . .
C82 C 0.7215(3) 0.6091(3) 0.9110(2) 0.0406 1.0000 Uani . . . . . . .
C83 C 0.7931(3) 0.6434(4) 0.9496(2) 0.0466 1.0000 Uani . . . . . . .
C84 C 0.9014(3) 0.6430(3) 0.9270(2) 0.0396 1.0000 Uani . . . . . . .
C85 C 0.9360(3) 0.6084(3) 0.8653(2) 0.0385 1.0000 Uani . . . . . . .
C86 C 0.8661(3) 0.5732(3) 0.82675(18) 0.0344 1.0000 Uani . . . . . . .
C87 C 0.9799(4) 0.6785(4) 0.9693(3) 0.0567 1.0000 Uani . . . . . . .
C91 C 0.5870(4) 0.9658(4) 0.8579(3) 0.0891 0.60(2) Uani . . P . . . .
C92 C 0.4725(3) 0.9803(3) 0.8590(2) 0.0696 0.40(2) Uani . . P . . . .
C93 C 0.1238(5) 0.7444(6) 0.4482(3) 0.0872 1.0000 Uani . . . . . . .
H31 H 0.2712 0.7559 0.9516 0.0409 1.0000 Uiso R . . . . . .
H41 H 0.2410 0.9497 0.9433 0.0480 1.0000 Uiso R . . . . . .
H51 H 0.1912 1.0835 0.8343 0.0493 1.0000 Uiso R . . . . . .
H61 H 0.1658 1.0233 0.7331 0.0490 1.0000 Uiso R . . . . . .
H121 H 0.3761 0.8882 0.6643 0.0740 1.0000 Uiso R . . . . . .
H131 H 0.4342 1.0052 0.5616 0.0901 1.0000 Uiso R . . . . . .
H141 H 0.3180 1.0854 0.4623 0.0791 1.0000 Uiso R . . . . . .
H151 H 0.1460 1.0429 0.4637 0.0781 1.0000 Uiso R . . . . . .
H161 H 0.0859 0.9285 0.5668 0.0625 1.0000 Uiso R . . . . . .
H221 H 0.0463 0.7006 0.6397 0.0503 1.0000 Uiso R . . . . . .
H231 H -0.1415 0.7148 0.6323 0.0563 1.0000 Uiso R . . . . . .
H241 H -0.2657 0.8302 0.6916 0.0620 1.0000 Uiso R . . . . . .
H251 H -0.1999 0.9346 0.7548 0.0811 1.0000 Uiso R . . . . . .
H261 H -0.0120 0.9241 0.7607 0.0699 1.0000 Uiso R . . . . . .
H331 H 0.5520 0.3985 0.9706 0.0379 1.0000 Uiso R . . . . . .
H341 H 0.5324 0.2211 1.0323 0.0449 1.0000 Uiso R . . . . . .
H351 H 0.4492 0.1153 0.9773 0.0490 1.0000 Uiso R . . . . . .
H361 H 0.3753 0.1960 0.8620 0.0417 1.0000 Uiso R . . . . . .
H421 H 0.4825 0.4920 0.6316 0.0478 1.0000 Uiso R . . . . . .
H431 H 0.5958 0.4082 0.5511 0.0652 1.0000 Uiso R . . . . . .
H441 H 0.6328 0.2123 0.5667 0.0740 1.0000 Uiso R . . . . . .
H451 H 0.5597 0.1003 0.6646 0.0742 1.0000 Uiso R . . . . . .
H461 H 0.4426 0.1830 0.7444 0.0571 1.0000 Uiso R . . . . . .
H521 H 0.1790 0.3827 0.8583 0.0510 1.0000 Uiso R . . . . . .
H531 H 0.0165 0.3195 0.8622 0.0580 1.0000 Uiso R . . . . . .
H541 H -0.0300 0.2595 0.7672 0.0557 1.0000 Uiso R . . . . . .
H551 H 0.0841 0.2587 0.6680 0.0631 1.0000 Uiso R . . . . . .
H561 H 0.2482 0.3186 0.6645 0.0518 1.0000 Uiso R . . . . . .
H621 H 0.5459 0.6703 0.6829 0.0441 1.0000 Uiso R . . . . . .
H631 H 0.5700 0.7141 0.5603 0.0529 1.0000 Uiso R . . . . . .
H651 H 0.8653 0.4905 0.5856 0.0521 1.0000 Uiso R . . . . . .
H661 H 0.8428 0.4430 0.7079 0.0442 1.0000 Uiso R . . . . . .
H671 H 0.7421 0.7144 0.4620 0.0952 1.0000 Uiso R . . . . . .
H672 H 0.7997 0.5871 0.4667 0.0951 1.0000 Uiso R . . . . . .
H673 H 0.6712 0.6290 0.4555 0.0955 1.0000 Uiso R . . . . . .
H721 H 0.6703 0.3149 0.7545 0.0419 1.0000 Uiso R . . . . . .
H731 H 0.7483 0.1225 0.7904 0.0471 1.0000 Uiso R . . . . . .
H751 H 0.8892 0.1678 0.9602 0.0431 1.0000 Uiso R . . . . . .
H761 H 0.8099 0.3617 0.9242 0.0349 1.0000 Uiso R . . . . . .
H771 H 0.8854 -0.0264 0.9567 0.0833 1.0000 Uiso R . . . . . .
H772 H 0.9531 -0.0184 0.8842 0.0834 1.0000 Uiso R . . . . . .
H773 H 0.8350 -0.0465 0.8888 0.0830 1.0000 Uiso R . . . . . .
H821 H 0.6499 0.6102 0.9269 0.0481 1.0000 Uiso R . . . . . .
H831 H 0.7670 0.6659 0.9913 0.0551 1.0000 Uiso R . . . . . .
H851 H 1.0081 0.6084 0.8488 0.0452 1.0000 Uiso R . . . . . .
H861 H 0.8922 0.5502 0.7850 0.0409 1.0000 Uiso R . . . . . .
H871 H 1.0246 0.7229 0.9373 0.0843 1.0000 Uiso R . . . . . .
H872 H 0.9384 0.7232 1.0003 0.0838 1.0000 Uiso R . . . . . .
H873 H 1.0273 0.6125 0.9992 0.0841 1.0000 Uiso R . . . . . .
H910 H 0.4598 0.9219 0.8479 0.1324 0.60 Uiso R . . . . . .
H911 H 0.6056 1.0284 0.8698 0.1065 0.60 Uiso R . . . . . .
H912 H 0.6202 0.8968 0.8920 0.1065 0.60 Uiso R . . . . . .
H913 H 0.6138 0.9621 0.8110 0.1065 0.60 Uiso R . . . . . .
H920 H 0.6098 0.9692 0.8149 0.1020 0.40 Uiso R . . . . . .
H921 H 0.4466 0.9765 0.9069 0.0838 0.40 Uiso R . . . . . .
H922 H 0.4389 1.0527 0.8283 0.0838 0.40 Uiso R . . . . . .
H923 H 0.4536 0.9217 0.8425 0.0838 0.40 Uiso R . . . . . .
H931 H 0.1543 0.7666 0.4850 0.1046 0.63 Uiso R . . . . . .
H932 H 0.1769 0.6845 0.4348 0.1046 0.63 Uiso R . . . . . .
H933 H 0.1314 0.7987 0.4731 0.1046 0.37 Uiso R . . . . . .
H934 H 0.1869 0.6818 0.4577 0.1046 0.37 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.26418(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Pd2 . 3.1872(3) yes
Pd1 . Se1 . 2.4023(4) yes
Pd1 . Cl1 . 2.3390(9) yes
Pd1 . P1 . 2.2823(9) yes
Pd1 . P2 . 2.3420(8) yes
Pd2 . Se1 . 2.4744(4) yes
Pd2 . Cl2 . 2.4037(9) yes
Pd2 . P3 . 2.2760(8) yes
Pd2 . C32 . 2.007(3) yes
Se1 . C2 . 1.930(3) yes
Cl3 . C93 . 1.740(6) yes
Cl41 . C93 . 1.720(8) yes
Cl42 . C93 . 1.659(10) yes
P1 . C1 . 1.814(3) yes
P1 . C11 . 1.814(4) yes
P1 . C21 . 1.825(4) yes
P2 . C31 . 1.824(3) yes
P2 . C41 . 1.824(3) yes
P2 . C51 . 1.823(3) yes
P3 . C61 . 1.822(3) yes
P3 . C71 . 1.824(3) yes
P3 . C81 . 1.819(3) yes
O91 . C91 . 1.385(6) yes
O91 . H910 . 0.861 no
O92 . C92 . 1.385(6) yes
O92 . H920 . 0.850 no
C1 . C2 . 1.392(5) yes
C1 . C6 . 1.391(5) yes
C2 . C3 . 1.387(5) yes
C3 . C4 . 1.385(5) yes
C3 . H31 . 0.944 no
C4 . C5 . 1.386(5) yes
C4 . H41 . 0.931 no
C5 . C6 . 1.380(5) yes
C5 . H51 . 0.933 no
C6 . H61 . 0.923 no
C11 . C12 . 1.385(6) yes
C11 . C16 . 1.379(5) yes
C12 . C13 . 1.390(6) yes
C12 . H121 . 0.928 no
C13 . C14 . 1.371(7) yes
C13 . H131 . 0.937 no
C14 . C15 . 1.379(7) yes
C14 . H141 . 0.933 no
C15 . C16 . 1.381(6) yes
C15 . H151 . 0.932 no
C16 . H161 . 0.942 no
C21 . C22 . 1.385(5) yes
C21 . C26 . 1.386(5) yes
C22 . C23 . 1.386(5) yes
C22 . H221 . 0.921 no
C23 . C24 . 1.358(6) yes
C23 . H231 . 0.934 no
C24 . C25 . 1.372(6) yes
C24 . H241 . 0.932 no
C25 . C26 . 1.376(6) yes
C25 . H251 . 0.932 no
C26 . H261 . 0.939 no
C31 . C32 . 1.399(4) yes
C31 . C36 . 1.400(5) yes
C32 . C33 . 1.403(4) yes
C33 . C34 . 1.380(5) yes
C33 . H331 . 0.928 no
C34 . C35 . 1.390(5) yes
C34 . H341 . 0.928 no
C35 . C36 . 1.380(5) yes
C35 . H351 . 0.941 no
C36 . H361 . 0.940 no
C41 . C42 . 1.388(5) yes
C41 . C46 . 1.405(5) yes
C42 . C43 . 1.382(5) yes
C42 . H421 . 0.938 no
C43 . C44 . 1.373(7) yes
C43 . H431 . 0.937 no
C44 . C45 . 1.379(7) yes
C44 . H441 . 0.932 no
C45 . C46 . 1.388(6) yes
C45 . H451 . 0.930 no
C46 . H461 . 0.936 no
C51 . C52 . 1.385(5) yes
C51 . C56 . 1.384(5) yes
C52 . C53 . 1.392(5) yes
C52 . H521 . 0.935 no
C53 . C54 . 1.372(6) yes
C53 . H531 . 0.936 no
C54 . C55 . 1.374(6) yes
C54 . H541 . 0.926 no
C55 . C56 . 1.393(5) yes
C55 . H551 . 0.934 no
C56 . H561 . 0.930 no
C61 . C62 . 1.402(5) yes
C61 . C66 . 1.392(5) yes
C62 . C63 . 1.378(5) yes
C62 . H621 . 0.935 no
C63 . C64 . 1.382(6) yes
C63 . H631 . 0.935 no
C64 . C65 . 1.391(6) yes
C64 . C67 . 1.501(5) yes
C65 . C66 . 1.380(5) yes
C65 . H651 . 0.927 no
C66 . H661 . 0.937 no
C67 . H671 . 0.960 no
C67 . H672 . 0.955 no
C67 . H673 . 0.957 no
C71 . C72 . 1.390(5) yes
C71 . C76 . 1.400(4) yes
C72 . C73 . 1.384(5) yes
C72 . H721 . 0.924 no
C73 . C74 . 1.392(5) yes
C73 . H731 . 0.936 no
C74 . C75 . 1.389(5) yes
C74 . C77 . 1.508(5) yes
C75 . C76 . 1.384(5) yes
C75 . H751 . 0.929 no
C76 . H761 . 0.939 no
C77 . H771 . 0.964 no
C77 . H772 . 0.970 no
C77 . H773 . 0.970 no
C81 . C82 . 1.384(5) yes
C81 . C86 . 1.394(4) yes
C82 . C83 . 1.393(5) yes
C82 . H821 . 0.919 no
C83 . C84 . 1.385(5) yes
C83 . H831 . 0.933 no
C84 . C85 . 1.377(5) yes
C84 . C87 . 1.512(5) yes
C85 . C86 . 1.385(5) yes
C85 . H851 . 0.931 no
C86 . H861 . 0.936 no
C87 . H871 . 0.961 no
C87 . H872 . 0.964 no
C87 . H873 . 0.953 no
C91 . H911 . 0.950 no
C91 . H912 . 0.950 no
C91 . H913 . 0.950 no
C92 . H921 . 0.950 no
C92 . H922 . 0.950 no
C92 . H923 . 0.950 no
C93 . H931 . 0.950 no
C93 . H932 . 0.950 no
C93 . H933 . 0.950 no
C93 . H934 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pd2 . Pd1 . Se1 . 50.179(9) yes
Pd2 . Pd1 . Cl1 . 133.02(3) yes
Se1 . Pd1 . Cl1 . 175.82(3) yes
Pd2 . Pd1 . P1 . 108.07(2) yes
Se1 . Pd1 . P1 . 86.27(2) yes
Cl1 . Pd1 . P1 . 89.90(3) yes
Pd2 . Pd1 . P2 . 75.45(2) yes
Se1 . Pd1 . P2 . 90.92(2) yes
Cl1 . Pd1 . P2 . 92.66(3) yes
P1 . Pd1 . P2 . 172.08(3) yes
Pd1 . Pd2 . Se1 . 48.214(9) yes
Pd1 . Pd2 . Cl2 . 93.18(2) yes
Se1 . Pd2 . Cl2 . 96.35(2) yes
Pd1 . Pd2 . P3 . 125.58(2) yes
Se1 . Pd2 . P3 . 170.99(2) yes
Cl2 . Pd2 . P3 . 90.33(3) yes
Pd1 . Pd2 . C32 . 90.85(9) yes
Se1 . Pd2 . C32 . 82.41(8) yes
Cl2 . Pd2 . C32 . 173.34(9) yes
P3 . Pd2 . C32 . 91.63(8) yes
Pd2 . Se1 . Pd1 . 81.606(12) yes
Pd2 . Se1 . C2 . 104.34(9) yes
Pd1 . Se1 . C2 . 101.89(10) yes
Pd1 . P1 . C1 . 109.94(11) yes
Pd1 . P1 . C11 . 116.69(12) yes
C1 . P1 . C11 . 105.91(16) yes
Pd1 . P1 . C21 . 110.92(11) yes
C1 . P1 . C21 . 105.59(16) yes
C11 . P1 . C21 . 107.11(16) yes
Pd1 . P2 . C31 . 116.77(11) yes
Pd1 . P2 . C41 . 120.00(12) yes
C31 . P2 . C41 . 106.20(15) yes
Pd1 . P2 . C51 . 102.90(11) yes
C31 . P2 . C51 . 104.25(15) yes
C41 . P2 . C51 . 104.85(15) yes
Pd2 . P3 . C61 . 111.20(11) yes
Pd2 . P3 . C71 . 118.36(10) yes
C61 . P3 . C71 . 103.28(15) yes
Pd2 . P3 . C81 . 112.66(11) yes
C61 . P3 . C81 . 108.34(14) yes
C71 . P3 . C81 . 102.05(14) yes
C91 . O91 . H910 . 106.2 no
C92 . O92 . H920 . 109.1 no
P1 . C1 . C2 . 116.1(2) yes
P1 . C1 . C6 . 124.0(3) yes
C2 . C1 . C6 . 119.9(3) yes
C1 . C2 . Se1 . 121.4(2) yes
C1 . C2 . C3 . 120.0(3) yes
Se1 . C2 . C3 . 118.4(2) yes
C2 . C3 . C4 . 119.6(3) yes
C2 . C3 . H31 . 120.1 no
C4 . C3 . H31 . 120.3 no
C3 . C4 . C5 . 120.4(3) yes
C3 . C4 . H41 . 119.4 no
C5 . C4 . H41 . 120.1 no
C4 . C5 . C6 . 120.1(3) yes
C4 . C5 . H51 . 119.7 no
C6 . C5 . H51 . 120.2 no
C1 . C6 . C5 . 119.9(3) yes
C1 . C6 . H61 . 119.5 no
C5 . C6 . H61 . 120.6 no
P1 . C11 . C12 . 118.1(3) yes
P1 . C11 . C16 . 122.3(3) yes
C12 . C11 . C16 . 119.5(4) yes
C11 . C12 . C13 . 119.6(4) yes
C11 . C12 . H121 . 120.3 no
C13 . C12 . H121 . 120.1 no
C12 . C13 . C14 . 120.6(5) yes
C12 . C13 . H131 . 119.6 no
C14 . C13 . H131 . 119.8 no
C13 . C14 . C15 . 119.7(4) yes
C13 . C14 . H141 . 120.3 no
C15 . C14 . H141 . 120.1 no
C14 . C15 . C16 . 120.1(4) yes
C14 . C15 . H151 . 120.1 no
C16 . C15 . H151 . 119.9 no
C15 . C16 . C11 . 120.5(4) yes
C15 . C16 . H161 . 119.9 no
C11 . C16 . H161 . 119.5 no
P1 . C21 . C22 . 120.1(3) yes
P1 . C21 . C26 . 121.6(3) yes
C22 . C21 . C26 . 118.2(3) yes
C21 . C22 . C23 . 120.5(4) yes
C21 . C22 . H221 . 119.4 no
C23 . C22 . H221 . 120.1 no
C22 . C23 . C24 . 120.8(4) yes
C22 . C23 . H231 . 118.9 no
C24 . C23 . H231 . 120.3 no
C23 . C24 . C25 . 119.0(4) yes
C23 . C24 . H241 . 121.0 no
C25 . C24 . H241 . 119.9 no
C24 . C25 . C26 . 121.2(4) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 119.1 no
C21 . C26 . C25 . 120.2(4) yes
C21 . C26 . H261 . 119.2 no
C25 . C26 . H261 . 120.6 no
P2 . C31 . C32 . 119.7(2) yes
P2 . C31 . C36 . 119.6(2) yes
C32 . C31 . C36 . 120.7(3) yes
C31 . C32 . Pd2 . 124.8(2) yes
C31 . C32 . C33 . 117.6(3) yes
Pd2 . C32 . C33 . 117.5(2) yes
C32 . C33 . C34 . 121.8(3) yes
C32 . C33 . H331 . 120.0 no
C34 . C33 . H331 . 118.2 no
C33 . C34 . C35 . 119.8(3) yes
C33 . C34 . H341 . 120.0 no
C35 . C34 . H341 . 120.2 no
C34 . C35 . C36 . 119.9(3) yes
C34 . C35 . H351 . 120.1 no
C36 . C35 . H351 . 120.0 no
C31 . C36 . C35 . 120.2(3) yes
C31 . C36 . H361 . 120.1 no
C35 . C36 . H361 . 119.7 no
P2 . C41 . C42 . 121.6(3) yes
P2 . C41 . C46 . 119.9(3) yes
C42 . C41 . C46 . 118.5(3) yes
C41 . C42 . C43 . 120.9(4) yes
C41 . C42 . H421 . 119.1 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 120.3(4) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 120.2 no
C43 . C44 . C45 . 119.8(4) yes
C43 . C44 . H441 . 120.3 no
C45 . C44 . H441 . 120.0 no
C44 . C45 . C46 . 120.7(4) yes
C44 . C45 . H451 . 120.1 no
C46 . C45 . H451 . 119.1 no
C41 . C46 . C45 . 119.7(4) yes
C41 . C46 . H461 . 119.7 no
C45 . C46 . H461 . 120.7 no
P2 . C51 . C52 . 119.2(3) yes
P2 . C51 . C56 . 121.7(3) yes
C52 . C51 . C56 . 118.9(3) yes
C51 . C52 . C53 . 120.5(4) yes
C51 . C52 . H521 . 120.3 no
C53 . C52 . H521 . 119.2 no
C52 . C53 . C54 . 119.8(4) yes
C52 . C53 . H531 . 120.4 no
C54 . C53 . H531 . 119.8 no
C53 . C54 . C55 . 120.5(4) yes
C53 . C54 . H541 . 119.6 no
C55 . C54 . H541 . 120.0 no
C54 . C55 . C56 . 119.7(4) yes
C54 . C55 . H551 . 120.2 no
C56 . C55 . H551 . 120.1 no
C55 . C56 . C51 . 120.6(4) yes
C55 . C56 . H561 . 119.6 no
C51 . C56 . H561 . 119.8 no
P3 . C61 . C62 . 119.8(3) yes
P3 . C61 . C66 . 122.4(3) yes
C62 . C61 . C66 . 117.8(3) yes
C61 . C62 . C63 . 120.9(3) yes
C61 . C62 . H621 . 120.3 no
C63 . C62 . H621 . 118.8 no
C62 . C63 . C64 . 121.4(4) yes
C62 . C63 . H631 . 119.6 no
C64 . C63 . H631 . 119.0 no
C63 . C64 . C65 . 117.8(3) yes
C63 . C64 . C67 . 120.7(4) yes
C65 . C64 . C67 . 121.4(4) yes
C64 . C65 . C66 . 121.5(4) yes
C64 . C65 . H651 . 119.9 no
C66 . C65 . H651 . 118.5 no
C61 . C66 . C65 . 120.6(3) yes
C61 . C66 . H661 . 119.9 no
C65 . C66 . H661 . 119.5 no
C64 . C67 . H671 . 109.2 no
C64 . C67 . H672 . 109.2 no
H671 . C67 . H672 . 108.7 no
C64 . C67 . H673 . 110.7 no
H671 . C67 . H673 . 109.7 no
H672 . C67 . H673 . 109.2 no
P3 . C71 . C72 . 120.9(2) yes
P3 . C71 . C76 . 121.2(2) yes
C72 . C71 . C76 . 117.9(3) yes
C71 . C72 . C73 . 120.8(3) yes
C71 . C72 . H721 . 119.8 no
C73 . C72 . H721 . 119.3 no
C72 . C73 . C74 . 121.3(3) yes
C72 . C73 . H731 . 119.2 no
C74 . C73 . H731 . 119.4 no
C73 . C74 . C75 . 118.0(3) yes
C73 . C74 . C77 . 122.3(4) yes
C75 . C74 . C77 . 119.7(3) yes
C74 . C75 . C76 . 121.0(3) yes
C74 . C75 . H751 . 119.9 no
C76 . C75 . H751 . 119.2 no
C71 . C76 . C75 . 121.0(3) yes
C71 . C76 . H761 . 118.7 no
C75 . C76 . H761 . 120.3 no
C74 . C77 . H771 . 110.3 no
C74 . C77 . H772 . 109.1 no
H771 . C77 . H772 . 109.1 no
C74 . C77 . H773 . 110.3 no
H771 . C77 . H773 . 109.3 no
H772 . C77 . H773 . 108.8 no
P3 . C81 . C82 . 119.4(2) yes
P3 . C81 . C86 . 121.9(3) yes
C82 . C81 . C86 . 118.4(3) yes
C81 . C82 . C83 . 120.6(3) yes
C81 . C82 . H821 . 119.9 no
C83 . C82 . H821 . 119.5 no
C82 . C83 . C84 . 120.9(4) yes
C82 . C83 . H831 . 118.7 no
C84 . C83 . H831 . 120.4 no
C83 . C84 . C85 . 118.2(3) yes
C83 . C84 . C87 . 121.0(4) yes
C85 . C84 . C87 . 120.8(4) yes
C84 . C85 . C86 . 121.6(3) yes
C84 . C85 . H851 . 119.7 no
C86 . C85 . H851 . 118.7 no
C81 . C86 . C85 . 120.3(3) yes
C81 . C86 . H861 . 120.2 no
C85 . C86 . H861 . 119.5 no
C84 . C87 . H871 . 110.6 no
C84 . C87 . H872 . 110.1 no
H871 . C87 . H872 . 109.0 no
C84 . C87 . H873 . 110.0 no
H871 . C87 . H873 . 109.2 no
H872 . C87 . H873 . 107.8 no
O91 . C91 . H911 . 109.5 no
O91 . C91 . H912 . 109.5 no
H911 . C91 . H912 . 109.5 no
O91 . C91 . H913 . 109.4 no
C92 . C91 . H913 . 109.4 no
H911 . C91 . H913 . 109.5 no
H912 . C91 . H913 . 109.5 no
O92 . C92 . H921 . 109.4 no
O92 . C92 . H922 . 109.5 no
H921 . C92 . H922 . 109.5 no
O92 . C92 . H923 . 109.5 no
C91 . C92 . H923 . 109.5 no
H921 . C92 . H923 . 109.5 no
H922 . C92 . H923 . 109.5 no
Cl3 . C93 . Cl41 . 114.1(4) yes
Cl3 . C93 . Cl42 . 116.7(4) yes
Cl3 . C93 . H931 . 108.3 no
Cl41 . C93 . H931 . 108.3 no
Cl3 . C93 . H932 . 108.3 no
Cl41 . C93 . H932 . 108.3 no
H931 . C93 . H932 . 109.5 no
Cl3 . C93 . H933 . 107.6 no
Cl42 . C93 . H933 . 107.7 no
Cl3 . C93 . H934 . 107.6 no
Cl42 . C93 . H934 . 107.6 no
H933 . C93 . H934 . 109.5 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 C93 3.389(6) . . no
Cl2 O91 3.176(4) . . no
Cl2 O92 3.467(6) . . no
Cl41 C26 3.28(1) . 2_576 no
Cl41 C25 3.46(1) . 2_576 no
Cl42 C44 3.59(2) . 2_666 no
O91 C4 3.226(5) . . no
O91 C36 3.276(5) . 1_565 no
O91 C5 3.334(5) . . no
O91 C35 3.503(6) . 1_565 no
O91 C34 3.542(4) . 2_667 no
C3 C75 3.467(5) . 2_667 no
C3 C34 3.572(5) . 2_667 no
C4 C92 3.226(5) . . no
C4 C75 3.551(5) . 2_667 no
C5 C92 3.334(5) . . no
C5 C54 3.537(4) . 1_565 no
C23 C86 3.456(5) . 1_455 no
C24 C86 3.444(5) . 1_455 no
C34 C92 3.542(4) . 2_667 no
C35 C92 3.503(6) . 1_545 no
C36 C92 3.276(5) . 1_545 no
C53 C86 3.519(5) . 1_455 no
C53 C76 3.523(5) . 1_455 no
C56 C67 3.486(5) . 2_666 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 Pd2 Cl2 . . . . 88.59(3) no
Pd1 Se1 Pd2 C32 . . . . -98.0(1) no
Pd1 Se1 C2 C1 . . . . 7.3(3) no
Pd1 Se1 C2 C3 . . . . -168.4(3) no
Pd1 P1 C1 C2 . . . . -20.2(3) no
Pd1 P1 C1 C6 . . . . 161.2(3) no
Pd1 P1 C11 C12 . . . . -68.8(4) no
Pd1 P1 C11 C16 . . . . 109.0(3) no
Pd1 P1 C21 C22 . . . . -42.5(3) no
Pd1 P1 C21 C26 . . . . 134.6(3) no
Pd1 P2 C31 C32 . . . . -33.6(3) no
Pd1 P2 C31 C36 . . . . 146.1(2) no
Pd1 P2 C41 C42 . . . . 14.2(4) no
Pd1 P2 C41 C46 . . . . -166.2(3) no
Pd1 P2 C51 C52 . . . . -75.0(3) no
Pd1 P2 C51 C56 . . . . 99.6(3) no
Pd2 Se1 Pd1 P1 . . . . -117.32(3) no
Pd2 Se1 Pd1 P2 . . . . 70.09(2) no
Pd2 Se1 C2 C1 . . . . 91.6(3) no
Pd2 Se1 C2 C3 . . . . -84.1(3) no
Pd2 P3 C61 C62 . . . . 17.0(4) no
Pd2 P3 C61 C66 . . . . -161.8(3) no
Pd2 P3 C71 C72 . . . . 76.9(3) no
Pd2 P3 C71 C76 . . . . -100.0(3) no
Pd2 P3 C81 C82 . . . . 23.7(3) no
Pd2 P3 C81 C86 . . . . -162.5(2) no
Pd2 C32 C31 P2 . . . . 2.6(4) no
Pd2 C32 C31 C36 . . . . -177.1(2) no
Pd2 C32 C33 C34 . . . . 175.7(3) no
Se1 Pd1 P1 C1 . . . . 19.0(1) no
Se1 Pd1 P1 C11 . . . . 139.6(2) no
Se1 Pd1 P1 C21 . . . . -97.4(1) no
Se1 Pd1 P2 C31 . . . . -16.7(1) no
Se1 Pd1 P2 C41 . . . . -147.5(2) no
Se1 Pd1 P2 C51 . . . . 96.7(1) no
Se1 Pd2 C32 C31 . . . . 66.0(2) no
Se1 Pd2 C32 C33 . . . . -108.7(2) no
Se1 C2 C1 P1 . . . . 7.7(4) no
Se1 C2 C1 C6 . . . . -173.6(3) no
Se1 C2 C3 C4 . . . . 173.3(3) no
Cl1 Pd1 P1 C1 . . . . -162.6(1) no
Cl1 Pd1 P1 C11 . . . . -42.1(2) no
Cl1 Pd1 P1 C21 . . . . 80.9(1) no
Cl1 Pd1 P2 C31 . . . . 165.4(1) no
Cl1 Pd1 P2 C41 . . . . 34.7(2) no
Cl1 Pd1 P2 C51 . . . . -81.1(1) no
Cl2 Pd2 Se1 C2 . . . . -11.6(1) no
Cl2 Pd2 P3 C61 . . . . -68.4(1) no
Cl2 Pd2 P3 C71 . . . . 172.3(1) no
Cl2 Pd2 P3 C81 . . . . 53.5(1) no
Cl3 C93 Cl41 Cl42 . . . . -102(2) no
Cl3 C93 Cl42 Cl41 . . . . 91(2) no
P1 Pd1 Se1 C2 . . . . -14.3(1) no
P1 C1 C2 C3 . . . . -176.6(3) no
P1 C1 C6 C5 . . . . 178.5(3) no
P1 C11 C12 C13 . . . . 177.7(4) no
P1 C11 C16 C15 . . . . -177.4(4) no
P1 C21 C22 C23 . . . . 178.4(3) no
P1 C21 C26 C25 . . . . -177.9(4) no
P2 Pd1 Se1 C2 . . . . 173.1(1) no
P2 C31 C32 C33 . . . . 177.3(2) no
P2 C31 C36 C35 . . . . -177.6(3) no
P2 C41 C42 C43 . . . . -178.3(3) no
P2 C41 C46 C45 . . . . 179.1(4) no
P2 C51 C52 C53 . . . . 176.4(3) no
P2 C51 C56 C55 . . . . -175.8(3) no
P3 Pd2 C32 C31 . . . . -107.2(3) no
P3 Pd2 C32 C33 . . . . 78.0(2) no
P3 C61 C62 C63 . . . . -178.0(3) no
P3 C61 C66 C65 . . . . 178.6(3) no
P3 C71 C72 C73 . . . . -178.6(3) no
P3 C71 C76 C75 . . . . 178.4(3) no
P3 C81 C82 C83 . . . . 172.7(3) no
P3 C81 C86 C85 . . . . -173.1(2) no
C1 P1 C11 C12 . . . . 53.9(4) no
C1 P1 C11 C16 . . . . -128.3(4) no
C1 P1 C21 C22 . . . . -161.6(3) no
C1 P1 C21 C26 . . . . 15.6(4) no
C1 C2 C3 C4 . . . . -2.5(6) no
C1 C6 C5 C4 . . . . -1.4(6) no
C2 Se1 Pd2 C32 . . . . 161.8(1) no
C2 C1 P1 C11 . . . . -147.1(3) no
C2 C1 P1 C21 . . . . 99.6(3) no
C2 C1 C6 C5 . . . . -0.1(6) no
C2 C3 C4 C5 . . . . 0.9(6) no
C3 C2 C1 C6 . . . . 2.0(6) no
C3 C4 C5 C6 . . . . 1.0(6) no
C6 C1 P1 C11 . . . . 34.3(4) no
C6 C1 P1 C21 . . . . -79.0(3) no
C11 P1 C21 C22 . . . . 85.9(3) no
C11 P1 C21 C26 . . . . -97.0(3) no
C11 C12 C13 C14 . . . . 0.2(8) no
C11 C16 C15 C14 . . . . -0.5(7) no
C12 C11 P1 C21 . . . . 166.2(3) no
C12 C11 C16 C15 . . . . 0.4(7) no
C12 C13 C14 C15 . . . . -0.3(9) no
C13 C12 C11 C16 . . . . -0.2(7) no
C13 C14 C15 C16 . . . . 0.4(8) no
C16 C11 P1 C21 . . . . -16.0(4) no
C21 C22 C23 C24 . . . . -1.0(5) no
C21 C26 C25 C24 . . . . 0.1(7) no
C22 C21 C26 C25 . . . . -0.7(6) no
C22 C23 C24 C25 . . . . 0.4(6) no
C23 C22 C21 C26 . . . . 1.2(5) no
C23 C24 C25 C26 . . . . 0.1(7) no
C31 P2 C41 C42 . . . . -121.0(3) no
C31 P2 C41 C46 . . . . 58.6(4) no
C31 P2 C51 C52 . . . . 47.3(3) no
C31 P2 C51 C56 . . . . -138.1(3) no
C31 C32 C33 C34 . . . . 0.5(5) no
C31 C36 C35 C34 . . . . 0.1(5) no
C32 Pd2 P3 C61 . . . . 118.0(2) no
C32 Pd2 P3 C71 . . . . -1.3(2) no
C32 Pd2 P3 C81 . . . . -120.1(1) no
C32 C31 P2 C41 . . . . 103.3(3) no
C32 C31 P2 C51 . . . . -146.3(3) no
C32 C31 C36 C35 . . . . 2.1(5) no
C32 C33 C34 C35 . . . . 1.7(5) no
C33 C32 C31 C36 . . . . -2.4(5) no
C33 C34 C35 C36 . . . . -2.0(5) no
C36 C31 P2 C41 . . . . -77.0(3) no
C36 C31 P2 C51 . . . . 33.4(3) no
C41 P2 C51 C52 . . . . 158.7(3) no
C41 P2 C51 C56 . . . . -26.7(3) no
C41 C42 C43 C44 . . . . -1.0(6) no
C41 C46 C45 C44 . . . . -0.7(7) no
C42 C41 P2 C51 . . . . 129.0(3) no
C42 C41 C46 C45 . . . . -1.3(6) no
C42 C43 C44 C45 . . . . -1.1(7) no
C43 C42 C41 C46 . . . . 2.2(6) no
C43 C44 C45 C46 . . . . 1.9(8) no
C46 C41 P2 C51 . . . . -51.4(3) no
C51 C52 C53 C54 . . . . -1.4(5) no
C51 C56 C55 C54 . . . . 0.3(6) no
C52 C51 C56 C55 . . . . -1.2(5) no
C52 C53 C54 C55 . . . . 0.5(6) no
C53 C52 C51 C56 . . . . 1.7(5) no
C53 C54 C55 C56 . . . . -0.0(6) no
C61 P3 C71 C72 . . . . -46.4(3) no
C61 P3 C71 C76 . . . . 136.6(3) no
C61 P3 C81 C82 . . . . 147.1(3) no
C61 P3 C81 C86 . . . . -39.1(3) no
C61 C62 C63 C64 . . . . -1.0(7) no
C61 C66 C65 C64 . . . . -0.2(7) no
C62 C61 P3 C71 . . . . 144.9(3) no
C62 C61 P3 C81 . . . . -107.4(4) no
C62 C61 C66 C65 . . . . -0.2(6) no
C62 C63 C64 C65 . . . . 0.6(6) no
C62 C63 C64 C67 . . . . 178.9(4) no
C63 C62 C61 C66 . . . . 0.8(6) no
C63 C64 C65 C66 . . . . 0.0(6) no
C66 C61 P3 C71 . . . . -33.8(4) no
C66 C61 P3 C81 . . . . 73.9(4) no
C66 C65 C64 C67 . . . . -178.3(4) no
C71 P3 C81 C82 . . . . -104.3(3) no
C71 P3 C81 C86 . . . . 69.5(3) no
C71 C72 C73 C74 . . . . 1.1(6) no
C71 C76 C75 C74 . . . . -0.6(5) no
C72 C71 P3 C81 . . . . -158.8(3) no
C72 C71 C76 C75 . . . . 1.3(5) no
C72 C73 C74 C75 . . . . -0.4(6) no
C72 C73 C74 C77 . . . . 179.9(4) no
C73 C72 C71 C76 . . . . -1.5(5) no
C73 C74 C75 C76 . . . . 0.2(5) no
C76 C71 P3 C81 . . . . 24.2(3) no
C76 C75 C74 C77 . . . . 179.8(4) no
C81 C82 C83 C84 . . . . 0.8(5) no
C81 C86 C85 C84 . . . . 0.3(5) no
C82 C81 C86 C85 . . . . 0.7(5) no
C82 C83 C84 C85 . . . . 0.3(5) no
C82 C83 C84 C87 . . . . -179.1(3) no
C83 C82 C81 C86 . . . . -1.3(5) no
C83 C84 C85 C86 . . . . -0.9(5) no
C86 C85 C84 C87 . . . . 178.6(3) no
#------------------------------------------------------------------------------
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O91 H910 Cl2 0.86 2.37 3.176(4) 155.6 . no
_database_code_depnum_ccdc_archive 'CCDC 999169'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex17
_audit_creation_date             11-01-17
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record             
;
2011-01-18 - Report on C32 H26 N O2 P Pd S  
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2011-01-19 - passes checkcif tests with minor warnings  
;

_oxford_structure_analysis_title '1171522 ben1101a'
_chemical_name_systematic        ?
_chemical_melting_point          ?


_cell_length_a                   10.2542(2)
_cell_length_b                   11.4908(2)
_cell_length_c                   12.9393(3)
_cell_angle_alpha                106.1144(9)
_cell_angle_beta                 109.7145(12)
_cell_angle_gamma                96.5437(12)
_cell_volume                     1342.05(5)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C32 H26 N1 O2 P1 Pd1 S1 
# Dc =      1.55 Fooo =    636.00 Mu =      8.60 M =    626.00
# Found Formula = C32 H26 N1 O2 P1 Pd1 S1 
# Dc =      1.55 FOOO =    636.00 Mu =      8.60 M =    626.00

_chemical_formula_sum            'C32 H26 N O2 P Pd S'
_chemical_formula_moiety         'C32 H26 N O2 P Pd S'
_chemical_compound_source        'from RMITU'
_chemical_formula_weight         626.00


_cell_measurement_reflns_used    19680
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.340

_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.860

# Sheldrick geometric approximatio 0.89 0.93 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.040
0 -1 0 0.040
0 0 1 0.070
0 0 -1 0.070
6 -4 -3 0.152
-2 2 1 0.100
-2 -2 -1 0.106
-4 -3 6 0.134


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.047

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 2.0 deg at rate 40 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 95 percent of data collected with 2-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            30412
_reflns_number_total             6148
_diffrn_reflns_av_R_equivalents  0.038
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6148 
# Theoretical number of reflections is about 12332 


_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         27.500
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -13
_reflns_limit_h_max              12
_reflns_limit_k_min              -14
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      6.93

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.72
_refine_diff_density_max         0.45


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6148
_refine_ls_number_restraints     0
_refine_ls_number_parameters     421
_oxford_refine_ls_R_factor_ref   0.0333
_refine_ls_wR_factor_ref         0.0672
_refine_ls_goodness_of_fit_ref   0.9964
_refine_ls_shift/su_max          0.0008094
_refine_ls_shift/su_mean         0.0000622


# The values computed from all data 
_oxford_reflns_number_all        6148
_refine_ls_R_factor_all          0.0333
_refine_ls_wR_factor_all         0.0672

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5466
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_gt          0.0651

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.18P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;                                                                               


;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.399952(16) 0.557241(14) 0.321075(14) 0.0227 1.0000 Uani . . . . . .
S1 S 0.39053(6) 0.35075(5) 0.30587(5) 0.0293 1.0000 Uani . . . . . .
P1 P 0.55840(5) 0.34408(5) 0.26075(5) 0.0224 1.0000 Uani . . . . . .
O1 O 0.42040(16) 0.74098(14) 0.34076(15) 0.0334 1.0000 Uani . . . . . .
O2 O -0.15005(19) 0.04338(15) 0.06965(15) 0.0391 1.0000 Uani . . . . . .
N1 N 0.17682(18) 0.53012(16) 0.25229(15) 0.0252 1.0000 Uani . . . . . .
C1 C 0.6814(2) 0.49015(19) 0.34768(17) 0.0233 1.0000 Uani . . . . . .
C2 C 0.6137(2) 0.58772(19) 0.37565(17) 0.0234 1.0000 Uani . . . . . .
C3 C 0.7017(2) 0.7074(2) 0.43381(19) 0.0289 1.0000 Uani . . . . . .
C4 C 0.8472(2) 0.7280(2) 0.46028(19) 0.0324 1.0000 Uani . . . . . .
C5 C 0.9110(2) 0.6300(2) 0.4314(2) 0.0333 1.0000 Uani . . . . . .
C6 C 0.8280(2) 0.5100(2) 0.37503(19) 0.0295 1.0000 Uani . . . . . .
C11 C 0.6310(2) 0.21293(19) 0.28286(18) 0.0244 1.0000 Uani . . . . . .
C12 C 0.6963(2) 0.2132(2) 0.3961(2) 0.0297 1.0000 Uani . . . . . .
C13 C 0.7459(3) 0.1106(2) 0.4156(2) 0.0351 1.0000 Uani . . . . . .
C14 C 0.7277(3) 0.0067(2) 0.3218(2) 0.0368 1.0000 Uani . . . . . .
C15 C 0.6607(3) 0.0055(2) 0.2091(2) 0.0369 1.0000 Uani . . . . . .
C16 C 0.6134(3) 0.1084(2) 0.1893(2) 0.0307 1.0000 Uani . . . . . .
C21 C 0.5200(2) 0.33246(19) 0.11064(18) 0.0250 1.0000 Uani . . . . . .
C22 C 0.3867(2) 0.3385(2) 0.0395(2) 0.0318 1.0000 Uani . . . . . .
C23 C 0.3624(3) 0.3375(2) -0.0731(2) 0.0408 1.0000 Uani . . . . . .
C24 C 0.4698(3) 0.3300(2) -0.1147(2) 0.0412 1.0000 Uani . . . . . .
C25 C 0.6022(3) 0.3241(2) -0.0446(2) 0.0397 1.0000 Uani . . . . . .
C26 C 0.6287(3) 0.3265(2) 0.0682(2) 0.0330 1.0000 Uani . . . . . .
C31 C 0.3203(2) 0.80115(19) 0.32131(19) 0.0278 1.0000 Uani . . . . . .
C32 C 0.3626(3) 0.9316(2) 0.3454(2) 0.0344 1.0000 Uani . . . . . .
C33 C 0.2648(3) 1.0039(2) 0.3303(2) 0.0402 1.0000 Uani . . . . . .
C34 C 0.1198(3) 0.9523(2) 0.2901(2) 0.0440 1.0000 Uani . . . . . .
C35 C 0.0750(3) 0.8272(2) 0.2633(2) 0.0381 1.0000 Uani . . . . . .
C36 C 0.1724(2) 0.7487(2) 0.27718(19) 0.0285 1.0000 Uani . . . . . .
C37 C 0.1107(2) 0.6182(2) 0.24201(19) 0.0277 1.0000 Uani . . . . . .
C41 C 0.0876(2) 0.40654(19) 0.20209(19) 0.0247 1.0000 Uani . . . . . .
C42 C 0.0663(2) 0.3435(2) 0.27492(19) 0.0265 1.0000 Uani . . . . . .
C43 C -0.0169(2) 0.2241(2) 0.2276(2) 0.0283 1.0000 Uani . . . . . .
C44 C -0.0756(2) 0.1639(2) 0.1070(2) 0.0290 1.0000 Uani . . . . . .
C45 C -0.0547(2) 0.2261(2) 0.0346(2) 0.0321 1.0000 Uani . . . . . .
C46 C 0.0263(2) 0.3480(2) 0.0829(2) 0.0304 1.0000 Uani . . . . . .
C47 C -0.2141(3) -0.0207(3) -0.0534(3) 0.0480 1.0000 Uani . . . . . .
H31 H 0.661(3) 0.779(2) 0.456(2) 0.0349 1.0000 Uiso . . . . . .
H41 H 0.902(3) 0.813(3) 0.499(2) 0.0388 1.0000 Uiso . . . . . .
H51 H 1.007(3) 0.645(2) 0.448(2) 0.0403 1.0000 Uiso . . . . . .
H61 H 0.868(3) 0.441(2) 0.353(2) 0.0361 1.0000 Uiso . . . . . .
H121 H 0.706(3) 0.281(3) 0.461(2) 0.0364 1.0000 Uiso . . . . . .
H131 H 0.790(3) 0.111(3) 0.491(2) 0.0419 1.0000 Uiso . . . . . .
H141 H 0.757(3) -0.065(3) 0.333(2) 0.0442 1.0000 Uiso . . . . . .
H151 H 0.649(3) -0.065(3) 0.145(2) 0.0444 1.0000 Uiso . . . . . .
H161 H 0.575(3) 0.113(2) 0.119(2) 0.0370 1.0000 Uiso . . . . . .
H221 H 0.317(3) 0.346(2) 0.065(2) 0.0374 1.0000 Uiso . . . . . .
H231 H 0.282(3) 0.345(3) -0.116(3) 0.0487 1.0000 Uiso . . . . . .
H241 H 0.450(3) 0.327(3) -0.189(3) 0.0494 1.0000 Uiso . . . . . .
H251 H 0.683(3) 0.323(3) -0.071(2) 0.0480 1.0000 Uiso . . . . . .
H261 H 0.721(3) 0.327(2) 0.117(2) 0.0392 1.0000 Uiso . . . . . .
H321 H 0.458(3) 0.965(3) 0.375(2) 0.0408 1.0000 Uiso . . . . . .
H331 H 0.295(3) 1.088(3) 0.344(2) 0.0474 1.0000 Uiso . . . . . .
H341 H 0.054(3) 1.003(3) 0.278(3) 0.0530 1.0000 Uiso . . . . . .
H351 H -0.028(3) 0.791(3) 0.232(2) 0.0458 1.0000 Uiso . . . . . .
H371 H 0.003(3) 0.587(2) 0.208(2) 0.0334 1.0000 Uiso . . . . . .
H421 H 0.110(3) 0.384(2) 0.358(2) 0.0319 1.0000 Uiso . . . . . .
H431 H -0.034(3) 0.181(2) 0.273(2) 0.0345 1.0000 Uiso . . . . . .
H451 H -0.090(3) 0.189(3) -0.042(2) 0.0385 1.0000 Uiso . . . . . .
H461 H 0.038(3) 0.392(2) 0.033(2) 0.0356 1.0000 Uiso . . . . . .
H471 H -0.262(4) -0.103(4) -0.065(3) 0.0715 1.0000 Uiso . . . . . .
H472 H -0.281(4) 0.021(3) -0.090(3) 0.0712 1.0000 Uiso . . . . . .
H473 H -0.147(4) -0.025(3) -0.090(3) 0.0718 1.0000 Uiso . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4003(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . S1 . 2.3138(5) yes
Pd1 . O1 . 2.0325(15) yes
Pd1 . N1 . 2.1057(17) yes
Pd1 . C2 . 2.017(2) yes
S1 . P1 . 1.9983(7) yes
P1 . C1 . 1.785(2) yes
P1 . C11 . 1.805(2) yes
P1 . C21 . 1.809(2) yes
O1 . C31 . 1.296(3) yes
O2 . C44 . 1.369(3) yes
O2 . C47 . 1.429(3) yes
N1 . C37 . 1.293(3) yes
N1 . C41 . 1.438(3) yes
C1 . C2 . 1.411(3) yes
C1 . C6 . 1.399(3) yes
C2 . C3 . 1.399(3) yes
C3 . C4 . 1.388(3) yes
C3 . H31 . 0.98(3) no
C4 . C5 . 1.392(3) yes
C4 . H41 . 0.96(3) no
C5 . C6 . 1.383(3) yes
C5 . H51 . 0.92(3) no
C6 . H61 . 0.95(3) no
C11 . C12 . 1.390(3) yes
C11 . C16 . 1.392(3) yes
C12 . C13 . 1.388(3) yes
C12 . H121 . 0.94(3) no
C13 . C14 . 1.387(4) yes
C13 . H131 . 0.93(3) no
C14 . C15 . 1.382(4) yes
C14 . H141 . 0.94(3) no
C15 . C16 . 1.384(3) yes
C15 . H151 . 0.94(3) no
C16 . H161 . 0.88(3) no
C21 . C22 . 1.389(3) yes
C21 . C26 . 1.399(3) yes
C22 . C23 . 1.390(4) yes
C22 . H221 . 0.89(3) no
C23 . C24 . 1.380(4) yes
C23 . H231 . 0.86(3) no
C24 . C25 . 1.377(4) yes
C24 . H241 . 0.91(3) no
C25 . C26 . 1.383(3) yes
C25 . H251 . 1.00(3) no
C26 . H261 . 0.94(3) no
C31 . C32 . 1.426(3) yes
C31 . C36 . 1.416(3) yes
C32 . C33 . 1.371(3) yes
C32 . H321 . 0.91(3) no
C33 . C34 . 1.393(4) yes
C33 . H331 . 0.92(3) no
C34 . C35 . 1.365(4) yes
C34 . H341 . 0.94(3) no
C35 . C36 . 1.421(3) yes
C35 . H351 . 0.99(3) no
C36 . C37 . 1.437(3) yes
C37 . H371 . 1.02(3) no
C41 . C42 . 1.394(3) yes
C41 . C46 . 1.379(3) yes
C42 . C43 . 1.377(3) yes
C42 . H421 . 0.96(3) no
C43 . C44 . 1.396(3) yes
C43 . H431 . 0.91(3) no
C44 . C45 . 1.381(3) yes
C45 . C46 . 1.392(3) yes
C45 . H451 . 0.89(3) no
C46 . H461 . 0.95(3) no
C47 . H471 . 0.97(4) no
C47 . H472 . 0.95(4) no
C47 . H473 . 0.96(4) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 . Pd1 . O1 . 176.65(5) yes
S1 . Pd1 . N1 . 93.18(5) yes
O1 . Pd1 . N1 . 90.04(6) yes
S1 . Pd1 . C2 . 89.17(6) yes
O1 . Pd1 . C2 . 87.68(7) yes
N1 . Pd1 . C2 . 175.22(7) yes
Pd1 . S1 . P1 . 93.74(3) yes
S1 . P1 . C1 . 105.59(7) yes
S1 . P1 . C11 . 110.69(7) yes
C1 . P1 . C11 . 113.05(10) yes
S1 . P1 . C21 . 114.10(7) yes
C1 . P1 . C21 . 105.98(9) yes
C11 . P1 . C21 . 107.46(10) yes
Pd1 . O1 . C31 . 127.84(14) yes
C44 . O2 . C47 . 117.2(2) yes
Pd1 . N1 . C37 . 124.09(15) yes
Pd1 . N1 . C41 . 120.32(13) yes
C37 . N1 . C41 . 115.31(18) yes
P1 . C1 . C2 . 112.79(15) yes
P1 . C1 . C6 . 124.10(16) yes
C2 . C1 . C6 . 122.76(19) yes
C1 . C2 . Pd1 . 121.40(15) yes
C1 . C2 . C3 . 116.27(19) yes
Pd1 . C2 . C3 . 122.09(15) yes
C2 . C3 . C4 . 121.3(2) yes
C2 . C3 . H31 . 120.3(15) no
C4 . C3 . H31 . 118.4(15) no
C3 . C4 . C5 . 121.1(2) yes
C3 . C4 . H41 . 117.7(16) no
C5 . C4 . H41 . 121.2(16) no
C4 . C5 . C6 . 119.4(2) yes
C4 . C5 . H51 . 120.5(17) no
C6 . C5 . H51 . 120.1(17) no
C1 . C6 . C5 . 119.1(2) yes
C1 . C6 . H61 . 119.2(16) no
C5 . C6 . H61 . 121.7(16) no
P1 . C11 . C12 . 118.79(16) yes
P1 . C11 . C16 . 121.47(17) yes
C12 . C11 . C16 . 119.6(2) yes
C11 . C12 . C13 . 120.1(2) yes
C11 . C12 . H121 . 122.0(16) no
C13 . C12 . H121 . 117.9(16) no
C12 . C13 . C14 . 119.9(2) yes
C12 . C13 . H131 . 120.0(17) no
C14 . C13 . H131 . 120.0(17) no
C13 . C14 . C15 . 120.1(2) yes
C13 . C14 . H141 . 121.3(17) no
C15 . C14 . H141 . 118.6(17) no
C14 . C15 . C16 . 120.2(2) yes
C14 . C15 . H151 . 120.2(17) no
C16 . C15 . H151 . 119.6(17) no
C11 . C16 . C15 . 120.1(2) yes
C11 . C16 . H161 . 117.0(18) no
C15 . C16 . H161 . 122.8(18) no
P1 . C21 . C22 . 120.76(17) yes
P1 . C21 . C26 . 119.58(16) yes
C22 . C21 . C26 . 119.5(2) yes
C21 . C22 . C23 . 119.7(2) yes
C21 . C22 . H221 . 121.6(17) no
C23 . C22 . H221 . 118.6(17) no
C22 . C23 . C24 . 120.4(2) yes
C22 . C23 . H231 . 120(2) no
C24 . C23 . H231 . 119(2) no
C23 . C24 . C25 . 120.2(2) yes
C23 . C24 . H241 . 118.6(19) no
C25 . C24 . H241 . 121.2(19) no
C24 . C25 . C26 . 120.2(2) yes
C24 . C25 . H251 . 122.1(17) no
C26 . C25 . H251 . 117.6(17) no
C21 . C26 . C25 . 120.0(2) yes
C21 . C26 . H261 . 120.4(17) no
C25 . C26 . H261 . 119.5(17) no
O1 . C31 . C32 . 117.2(2) yes
O1 . C31 . C36 . 125.78(19) yes
C32 . C31 . C36 . 117.0(2) yes
C31 . C32 . C33 . 121.6(2) yes
C31 . C32 . H321 . 116.9(18) no
C33 . C32 . H321 . 121.5(18) no
C32 . C33 . C34 . 121.1(2) yes
C32 . C33 . H331 . 119.8(18) no
C34 . C33 . H331 . 119.0(18) no
C33 . C34 . C35 . 119.0(2) yes
C33 . C34 . H341 . 119.7(19) no
C35 . C34 . H341 . 121.2(19) no
C34 . C35 . C36 . 121.8(2) yes
C34 . C35 . H351 . 118.7(17) no
C36 . C35 . H351 . 119.5(17) no
C35 . C36 . C31 . 119.4(2) yes
C35 . C36 . C37 . 116.1(2) yes
C31 . C36 . C37 . 124.50(19) yes
C36 . C37 . N1 . 127.5(2) yes
C36 . C37 . H371 . 120.0(15) no
N1 . C37 . H371 . 112.5(15) no
N1 . C41 . C42 . 119.60(19) yes
N1 . C41 . C46 . 120.90(19) yes
C42 . C41 . C46 . 119.5(2) yes
C41 . C42 . C43 . 120.0(2) yes
C41 . C42 . H421 . 119.5(15) no
C43 . C42 . H421 . 120.6(15) no
C42 . C43 . C44 . 120.4(2) yes
C42 . C43 . H431 . 122.1(16) no
C44 . C43 . H431 . 117.5(16) no
C43 . C44 . O2 . 115.5(2) yes
C43 . C44 . C45 . 119.7(2) yes
O2 . C44 . C45 . 124.7(2) yes
C44 . C45 . C46 . 119.6(2) yes
C44 . C45 . H451 . 120.9(18) no
C46 . C45 . H451 . 119.5(18) no
C45 . C46 . C41 . 120.8(2) yes
C45 . C46 . H461 . 119.7(16) no
C41 . C46 . H461 . 119.5(16) no
O2 . C47 . H471 . 107(2) no
O2 . C47 . H472 . 111(2) no
H471 . C47 . H472 . 110(3) no
O2 . C47 . H473 . 113(2) no
H471 . C47 . H473 . 110(3) no
H472 . C47 . H473 . 106(3) no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 C24 3.405(4) . 2_665 no
O2 C15 3.133(4) . 1_455 no
O2 C16 3.338(4) . 1_455 no
C4 C42 3.589(4) . 2_666 no
C13 C31 3.589(4) . 2_666 no
C33 C47 3.506(5) . 2_565 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 S1 P1 C1 . . . . 38.97(8) no
Pd1 S1 P1 C11 . . . . 161.65(6) no
Pd1 S1 P1 C21 . . . . -76.99(8) no
Pd1 O1 C31 C32 . . . . 178.1(2) no
Pd1 O1 C31 C36 . . . . -2.6(4) no
Pd1 N1 C37 C36 . . . . -2.1(4) no
Pd1 N1 C41 C42 . . . . 77.5(3) no
Pd1 N1 C41 C46 . . . . -100.5(2) no
Pd1 C2 C1 P1 . . . . 0.6(3) no
Pd1 C2 C1 C6 . . . . 174.0(2) no
Pd1 C2 C3 C4 . . . . -173.4(2) no
S1 Pd1 N1 C37 . . . . 177.1(2) no
S1 Pd1 N1 C41 . . . . -9.3(2) no
S1 Pd1 C2 C1 . . . . 23.8(2) no
S1 Pd1 C2 C3 . . . . -162.0(2) no
S1 P1 C1 C2 . . . . -30.0(2) no
S1 P1 C1 C6 . . . . 156.7(2) no
S1 P1 C11 C12 . . . . -67.9(2) no
S1 P1 C11 C16 . . . . 107.2(2) no
S1 P1 C21 C22 . . . . 5.0(2) no
S1 P1 C21 C26 . . . . -179.7(2) no
P1 S1 Pd1 N1 . . . . 142.86(6) no
P1 S1 Pd1 C2 . . . . -32.98(7) no
P1 C1 C2 C3 . . . . -173.9(2) no
P1 C1 C6 C5 . . . . 172.5(2) no
P1 C11 C12 C13 . . . . 176.3(2) no
P1 C11 C16 C15 . . . . -175.0(2) no
P1 C21 C22 C23 . . . . 175.8(2) no
P1 C21 C26 C25 . . . . -176.7(2) no
O1 Pd1 N1 C37 . . . . -2.0(2) no
O1 Pd1 N1 C41 . . . . 171.6(2) no
O1 Pd1 C2 C1 . . . . -157.3(2) no
O1 Pd1 C2 C3 . . . . 16.8(2) no
O1 C31 C32 C33 . . . . -178.4(2) no
O1 C31 C36 C35 . . . . 178.3(2) no
O1 C31 C36 C37 . . . . -3.0(4) no
O2 C44 C43 C42 . . . . 176.7(2) no
O2 C44 C45 C46 . . . . -178.3(2) no
N1 Pd1 O1 C31 . . . . 4.3(2) no
N1 C37 C36 C31 . . . . 5.6(4) no
N1 C37 C36 C35 . . . . -175.7(3) no
N1 C41 C42 C43 . . . . -178.8(2) no
N1 C41 C46 C45 . . . . 177.0(2) no
C1 P1 C11 C12 . . . . 50.4(2) no
C1 P1 C11 C16 . . . . -134.6(2) no
C1 P1 C21 C22 . . . . -110.7(2) no
C1 P1 C21 C26 . . . . 64.5(2) no
C1 C2 C3 C4 . . . . 1.0(4) no
C1 C6 C5 C4 . . . . 0.4(4) no
C2 Pd1 O1 C31 . . . . -179.9(2) no
C2 C1 P1 C11 . . . . -151.1(2) no
C2 C1 P1 C21 . . . . 91.4(2) no
C2 C1 C6 C5 . . . . -0.3(4) no
C2 C3 C4 C5 . . . . -1.0(4) no
C3 C2 C1 C6 . . . . -0.4(4) no
C3 C4 C5 C6 . . . . 0.2(4) no
C6 C1 P1 C11 . . . . 35.5(3) no
C6 C1 P1 C21 . . . . -82.0(2) no
C11 P1 C21 C22 . . . . 128.1(2) no
C11 P1 C21 C26 . . . . -56.6(2) no
C11 C12 C13 C14 . . . . -1.3(4) no
C11 C16 C15 C14 . . . . -1.1(5) no
C12 C11 P1 C21 . . . . 166.9(2) no
C12 C11 C16 C15 . . . . -0.0(4) no
C12 C13 C14 C15 . . . . 0.2(5) no
C13 C12 C11 C16 . . . . 1.2(4) no
C13 C14 C15 C16 . . . . 0.9(5) no
C16 C11 P1 C21 . . . . -18.0(2) no
C21 C22 C23 C24 . . . . 0.3(3) no
C21 C26 C25 C24 . . . . 1.3(3) no
C22 C21 C26 C25 . . . . -1.3(3) no
C22 C23 C24 C25 . . . . -0.3(3) no
C23 C22 C21 C26 . . . . 0.5(3) no
C23 C24 C25 C26 . . . . -0.4(3) no
C31 C32 C33 C34 . . . . -0.3(4) no
C31 C36 C35 C34 . . . . 0.8(4) no
C32 C31 C36 C35 . . . . -2.3(4) no
C32 C31 C36 C37 . . . . 176.3(2) no
C32 C33 C34 C35 . . . . -1.3(4) no
C33 C32 C31 C36 . . . . 2.2(4) no
C33 C34 C35 C36 . . . . 1.1(4) no
C34 C35 C36 C37 . . . . -178.0(3) no
C36 C37 N1 C41 . . . . -175.9(2) no
C37 N1 C41 C42 . . . . -108.4(3) no
C37 N1 C41 C46 . . . . 73.6(3) no
C41 C42 C43 C44 . . . . 2.5(3) no
C41 C46 C45 C44 . . . . 1.0(3) no
C42 C41 C46 C45 . . . . -1.0(3) no
C42 C43 C44 C45 . . . . -2.5(3) no
C43 C42 C41 C46 . . . . -0.8(3) no
C43 C44 O2 C47 . . . . 178.8(2) no
C43 C44 C45 C46 . . . . 0.7(3) no
C45 C44 O2 C47 . . . . -2.0(3) no
_database_code_depnum_ccdc_archive 'CCDC 999170'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex20a
_audit_creation_date             10-12-15
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2010-12-16- Report on C31 H23 N2 O3 P Pd Se 
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2010-12-16- passes checkcif tests with minor warnings  
;

_oxford_structure_analysis_title '12151646 ben1008'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   8.2026(2)
_cell_length_b                   11.3200(3)
_cell_length_c                   15.5766(4)
_cell_angle_alpha                81.6051(12)
_cell_angle_beta                 84.9680(17)
_cell_angle_gamma                71.6954(16)
_cell_volume                     1357.09(6)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C32 H23 N2 O3 P1 Pd1 Se1 
# Dc =      1.71 Fooo =    684.00 Mu =     21.22 M =    699.88
# Found Formula = C31 H23 N2 O3 P1 Pd1 Se1 
# Dc =      1.68 FOOO =    684.00 Mu =     21.20 M =    687.87

_chemical_formula_sum            'C31 H23 N2 O3 P Pd Se'
_chemical_formula_moiety         'C31 H23 N2 O3 P Pd Se'
_chemical_compound_source        'from RMITU'
_chemical_formula_weight         687.87


_cell_measurement_reflns_used    24684
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    2.120

# Sheldrick geometric approximatio 0.79 0.88 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.100
-1 0 0 0.100
0 1 0 0.050
0 -1 0 0.055
0 0 1 0.050
0 0 -1 0.055
0 1 1 0.030
0 -1 -1 0.035
1 0 1 0.086
-1 0 1 0.090


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.046

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 2.0 deg at rate 160 sec/frame,
crystal-detector distance 30mm,
multiple scan sets so over 95 percent of data collected with 2-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            30921
_reflns_number_total             6216
_diffrn_reflns_av_R_equivalents  0.060
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6216 
# Theoretical number of reflections is about 12445 


_diffrn_reflns_theta_min         2.618
_diffrn_reflns_theta_max         27.480
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.480
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              -14
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   2.13
_oxford_diffrn_Wilson_scale      13.68

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.81
_refine_diff_density_max         0.64


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     0
_refine_ls_number_parameters     421
_oxford_refine_ls_R_factor_ref   0.0440
_refine_ls_wR_factor_ref         0.0683
_refine_ls_goodness_of_fit_ref   0.9827
_refine_ls_shift/su_max          0.0020387
_refine_ls_shift/su_mean         0.1987706


# The values computed from all data 
_oxford_reflns_number_all        6215
_refine_ls_R_factor_all          0.0440
_refine_ls_wR_factor_all         0.0683

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5068
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_gt          0.0641

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    refxyz # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 1.40P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;                                                                               


;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.44699(3) 0.891210(18) 0.245131(12) 0.0235 1.0000 Uani . . . . . . .
Se1 Se 0.54545(4) 0.74256(3) 0.140538(17) 0.0307 1.0000 Uani . . . . . . .
P1 P 0.46624(9) 0.60036(6) 0.22671(4) 0.0250 1.0000 Uani . . . . . . .
O1 O 0.3470(2) 1.02070(19) 0.32833(13) 0.0344 1.0000 Uani . . . . . . .
O2 O 0.9721(3) 0.8616(2) -0.16348(14) 0.0502 1.0000 Uani . . . . . . .
O3 O 1.1845(3) 0.7508(3) -0.08545(16) 0.0584 1.0000 Uani . . . . . . .
N1 N 0.6428(3) 0.9759(2) 0.20832(13) 0.0252 1.0000 Uani . . . . . . .
N2 N 1.0394(3) 0.8241(2) -0.09360(16) 0.0364 1.0000 Uani . . . . . . .
C1 C 0.2798(3) 0.6847(2) 0.28566(16) 0.0259 1.0000 Uani . . . . . . .
C2 C 0.2663(3) 0.8099(2) 0.29287(16) 0.0251 1.0000 Uani . . . . . . .
C3 C 0.1196(4) 0.8772(3) 0.33796(18) 0.0297 1.0000 Uani . . . . . . .
C4 C -0.0052(4) 0.8233(3) 0.37246(18) 0.0319 1.0000 Uani . . . . . . .
C5 C 0.0092(4) 0.7006(3) 0.36329(19) 0.0341 1.0000 Uani . . . . . . .
C6 C 0.1530(4) 0.6301(3) 0.32009(19) 0.0320 1.0000 Uani . . . . . . .
C11 C 0.4110(3) 0.4911(2) 0.17050(18) 0.0280 1.0000 Uani . . . . . . .
C12 C 0.3570(4) 0.5272(3) 0.08608(19) 0.0318 1.0000 Uani . . . . . . .
C13 C 0.2952(4) 0.4502(3) 0.0457(2) 0.0392 1.0000 Uani . . . . . . .
C14 C 0.2872(4) 0.3366(3) 0.0894(2) 0.0408 1.0000 Uani . . . . . . .
C15 C 0.3418(4) 0.2985(3) 0.1730(2) 0.0385 1.0000 Uani . . . . . . .
C16 C 0.4046(4) 0.3750(3) 0.2140(2) 0.0330 1.0000 Uani . . . . . . .
C21 C 0.6332(3) 0.5123(3) 0.29953(18) 0.0289 1.0000 Uani . . . . . . .
C22 C 0.7814(4) 0.4276(3) 0.2683(2) 0.0377 1.0000 Uani . . . . . . .
C23 C 0.9161(4) 0.3672(3) 0.3217(2) 0.0420 1.0000 Uani . . . . . . .
C24 C 0.9050(4) 0.3906(3) 0.4066(2) 0.0421 1.0000 Uani . . . . . . .
C25 C 0.7581(4) 0.4737(3) 0.4393(2) 0.0393 1.0000 Uani . . . . . . .
C26 C 0.6220(4) 0.5344(3) 0.38561(19) 0.0333 1.0000 Uani . . . . . . .
C31 C 0.4344(4) 1.0752(2) 0.36602(17) 0.0277 1.0000 Uani . . . . . . .
C32 C 0.3567(4) 1.1326(3) 0.44028(19) 0.0354 1.0000 Uani . . . . . . .
C33 C 0.4409(4) 1.1879(3) 0.4861(2) 0.0401 1.0000 Uani . . . . . . .
C34 C 0.6070(4) 1.1928(3) 0.4601(2) 0.0402 1.0000 Uani . . . . . . .
C35 C 0.6814(4) 1.1432(3) 0.38581(19) 0.0320 1.0000 Uani . . . . . . .
C36 C 0.6000(4) 1.0838(2) 0.33694(17) 0.0272 1.0000 Uani . . . . . . .
C37 C 0.6884(4) 1.0405(2) 0.25885(17) 0.0271 1.0000 Uani . . . . . . .
C41 C 0.7498(3) 0.9444(2) 0.13205(16) 0.0257 1.0000 Uani . . . . . . .
C42 C 0.6867(4) 0.9953(3) 0.05091(19) 0.0342 1.0000 Uani . . . . . . .
C43 C 0.7818(4) 0.9575(3) -0.02355(19) 0.0351 1.0000 Uani . . . . . . .
C44 C 0.9407(4) 0.8692(3) -0.01498(17) 0.0288 1.0000 Uani . . . . . . .
C45 C 1.0088(4) 0.8223(3) 0.0644(2) 0.0430 1.0000 Uani . . . . . . .
C46 C 0.9122(4) 0.8603(3) 0.1381(2) 0.0418 1.0000 Uani . . . . . . .
H31 H 0.105(4) 0.959(3) 0.3450(19) 0.0354 1.0000 Uiso . . . . . . .
H41 H -0.099(4) 0.872(3) 0.402(2) 0.0382 1.0000 Uiso . . . . . . .
H51 H -0.073(4) 0.667(3) 0.385(2) 0.0407 1.0000 Uiso . . . . . . .
H61 H 0.168(4) 0.547(3) 0.313(2) 0.0379 1.0000 Uiso . . . . . . .
H121 H 0.365(4) 0.606(3) 0.057(2) 0.0371 1.0000 Uiso . . . . . . .
H131 H 0.263(4) 0.473(3) -0.009(2) 0.0469 1.0000 Uiso . . . . . . .
H141 H 0.247(4) 0.281(3) 0.057(2) 0.0490 1.0000 Uiso . . . . . . .
H151 H 0.335(4) 0.221(3) 0.202(2) 0.0461 1.0000 Uiso . . . . . . .
H161 H 0.440(4) 0.354(3) 0.272(2) 0.0395 1.0000 Uiso . . . . . . .
H221 H 0.786(4) 0.411(3) 0.217(2) 0.0455 1.0000 Uiso . . . . . . .
H231 H 1.014(5) 0.314(3) 0.301(2) 0.0496 1.0000 Uiso . . . . . . .
H241 H 0.992(5) 0.346(3) 0.443(2) 0.0500 1.0000 Uiso . . . . . . .
H251 H 0.753(4) 0.490(3) 0.495(2) 0.0467 1.0000 Uiso . . . . . . .
H261 H 0.530(4) 0.584(3) 0.406(2) 0.0395 1.0000 Uiso . . . . . . .
H321 H 0.246(4) 1.129(3) 0.457(2) 0.0415 1.0000 Uiso . . . . . . .
H331 H 0.391(4) 1.220(3) 0.534(2) 0.0478 1.0000 Uiso . . . . . . .
H341 H 0.661(4) 1.230(3) 0.493(2) 0.0478 1.0000 Uiso . . . . . . .
H351 H 0.785(4) 1.148(3) 0.368(2) 0.0378 1.0000 Uiso . . . . . . .
H371 H 0.792(4) 1.063(3) 0.2426(19) 0.0312 1.0000 Uiso . . . . . . .
H421 H 0.596(4) 1.049(3) 0.047(2) 0.0413 1.0000 Uiso . . . . . . .
H431 H 0.738(4) 0.987(3) -0.079(2) 0.0421 1.0000 Uiso . . . . . . .
H451 H 1.118(5) 0.769(3) 0.070(2) 0.0526 1.0000 Uiso . . . . . . .
H461 H 0.953(4) 0.829(3) 0.191(2) 0.0505 1.0000 Uiso . . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.29875(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Se1 . 2.4195(3) yes
Pd1 . O1 . 2.0283(18) yes
Pd1 . N1 . 2.115(2) yes
Pd1 . C2 . 2.015(3) yes
Se1 . P1 . 2.1652(7) yes
P1 . C1 . 1.785(3) yes
P1 . C11 . 1.799(3) yes
P1 . C21 . 1.800(3) yes
O1 . C31 . 1.303(3) yes
O2 . N2 . 1.222(3) yes
O3 . N2 . 1.224(3) yes
N1 . C37 . 1.298(3) yes
N1 . C41 . 1.433(3) yes
N2 . C44 . 1.472(3) yes
C1 . C2 . 1.407(4) yes
C1 . C6 . 1.400(4) yes
C2 . C3 . 1.398(4) yes
C3 . C4 . 1.381(4) yes
C3 . H31 . 0.92(3) no
C4 . C5 . 1.384(4) yes
C4 . H41 . 0.93(3) no
C5 . C6 . 1.381(4) yes
C5 . H51 . 0.90(3) no
C6 . H61 . 0.93(3) no
C11 . C12 . 1.387(4) yes
C11 . C16 . 1.403(4) yes
C12 . C13 . 1.381(4) yes
C12 . H121 . 0.96(3) no
C13 . C14 . 1.383(5) yes
C13 . H131 . 0.89(3) no
C14 . C15 . 1.378(5) yes
C14 . H141 . 1.01(3) no
C15 . C16 . 1.387(4) yes
C15 . H151 . 0.94(3) no
C16 . H161 . 0.95(3) no
C21 . C22 . 1.390(4) yes
C21 . C26 . 1.390(4) yes
C22 . C23 . 1.378(4) yes
C22 . H221 . 0.84(3) no
C23 . C24 . 1.377(5) yes
C23 . H231 . 0.91(4) no
C24 . C25 . 1.384(5) yes
C24 . H241 . 0.92(4) no
C25 . C26 . 1.390(4) yes
C25 . H251 . 0.91(3) no
C26 . H261 . 0.86(3) no
C31 . C32 . 1.413(4) yes
C31 . C36 . 1.422(4) yes
C32 . C33 . 1.366(4) yes
C32 . H321 . 0.93(3) no
C33 . C34 . 1.402(5) yes
C33 . H331 . 0.89(3) no
C34 . C35 . 1.371(4) yes
C34 . H341 . 0.93(3) no
C35 . C36 . 1.413(4) yes
C35 . H351 . 0.89(3) no
C36 . C37 . 1.429(4) yes
C37 . H371 . 0.97(3) no
C41 . C42 . 1.383(4) yes
C41 . C46 . 1.375(4) yes
C42 . C43 . 1.383(4) yes
C42 . H421 . 0.80(3) no
C43 . C44 . 1.374(4) yes
C43 . H431 . 0.94(3) no
C44 . C45 . 1.366(4) yes
C45 . C46 . 1.378(4) yes
C45 . H451 . 0.91(4) no
C46 . H461 . 0.90(3) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se1 . Pd1 . O1 . 175.62(6) yes
Se1 . Pd1 . N1 . 93.87(6) yes
O1 . Pd1 . N1 . 88.40(8) yes
Se1 . Pd1 . C2 . 90.11(7) yes
O1 . Pd1 . C2 . 87.92(9) yes
N1 . Pd1 . C2 . 174.14(9) yes
Pd1 . Se1 . P1 . 91.90(2) yes
Se1 . P1 . C1 . 105.09(9) yes
Se1 . P1 . C11 . 113.46(9) yes
C1 . P1 . C11 . 108.91(12) yes
Se1 . P1 . C21 . 110.77(9) yes
C1 . P1 . C21 . 110.64(13) yes
C11 . P1 . C21 . 107.96(12) yes
Pd1 . O1 . C31 . 125.38(17) yes
Pd1 . N1 . C37 . 122.46(18) yes
Pd1 . N1 . C41 . 119.38(16) yes
C37 . N1 . C41 . 117.3(2) yes
O3 . N2 . O2 . 123.5(3) yes
O3 . N2 . C44 . 118.2(2) yes
O2 . N2 . C44 . 118.3(3) yes
P1 . C1 . C2 . 115.81(19) yes
P1 . C1 . C6 . 121.7(2) yes
C2 . C1 . C6 . 122.5(2) yes
C1 . C2 . Pd1 . 123.57(19) yes
C1 . C2 . C3 . 116.2(2) yes
Pd1 . C2 . C3 . 120.2(2) yes
C2 . C3 . C4 . 121.5(3) yes
C2 . C3 . H31 . 119.7(19) no
C4 . C3 . H31 . 118.8(19) no
C3 . C4 . C5 . 121.4(3) yes
C3 . C4 . H41 . 117.6(20) no
C5 . C4 . H41 . 121.0(20) no
C4 . C5 . C6 . 119.2(3) yes
C4 . C5 . H51 . 121(2) no
C6 . C5 . H51 . 120(2) no
C1 . C6 . C5 . 119.3(3) yes
C1 . C6 . H61 . 119.0(19) no
C5 . C6 . H61 . 121.7(19) no
P1 . C11 . C12 . 119.6(2) yes
P1 . C11 . C16 . 120.6(2) yes
C12 . C11 . C16 . 119.4(3) yes
C11 . C12 . C13 . 120.2(3) yes
C11 . C12 . H121 . 118.4(18) no
C13 . C12 . H121 . 121.3(18) no
C12 . C13 . C14 . 120.0(3) yes
C12 . C13 . H131 . 120(2) no
C14 . C13 . H131 . 120(2) no
C13 . C14 . C15 . 120.7(3) yes
C13 . C14 . H141 . 117.9(20) no
C15 . C14 . H141 . 121.4(19) no
C14 . C15 . C16 . 119.8(3) yes
C14 . C15 . H151 . 120(2) no
C16 . C15 . H151 . 120(2) no
C11 . C16 . C15 . 119.9(3) yes
C11 . C16 . H161 . 117.3(19) no
C15 . C16 . H161 . 122.7(19) no
P1 . C21 . C22 . 120.0(2) yes
P1 . C21 . C26 . 120.8(2) yes
C22 . C21 . C26 . 119.1(3) yes
C21 . C22 . C23 . 120.6(3) yes
C21 . C22 . H221 . 119(2) no
C23 . C22 . H221 . 120(2) no
C22 . C23 . C24 . 120.1(3) yes
C22 . C23 . H231 . 121(2) no
C24 . C23 . H231 . 119(2) no
C23 . C24 . C25 . 120.3(3) yes
C23 . C24 . H241 . 120(2) no
C25 . C24 . H241 . 120(2) no
C24 . C25 . C26 . 119.6(3) yes
C24 . C25 . H251 . 120(2) no
C26 . C25 . H251 . 121(2) no
C25 . C26 . C21 . 120.3(3) yes
C25 . C26 . H261 . 120(2) no
C21 . C26 . H261 . 120(2) no
O1 . C31 . C32 . 117.3(2) yes
O1 . C31 . C36 . 125.0(2) yes
C32 . C31 . C36 . 117.7(2) yes
C31 . C32 . C33 . 121.6(3) yes
C31 . C32 . H321 . 116.0(20) no
C33 . C32 . H321 . 122.5(20) no
C32 . C33 . C34 . 121.3(3) yes
C32 . C33 . H331 . 119(2) no
C34 . C33 . H331 . 119(2) no
C33 . C34 . C35 . 118.0(3) yes
C33 . C34 . H341 . 119(2) no
C35 . C34 . H341 . 123(2) no
C34 . C35 . C36 . 122.6(3) yes
C34 . C35 . H351 . 119(2) no
C36 . C35 . H351 . 119(2) no
C31 . C36 . C35 . 118.7(2) yes
C31 . C36 . C37 . 124.2(2) yes
C35 . C36 . C37 . 117.1(3) yes
C36 . C37 . N1 . 126.8(3) yes
C36 . C37 . H371 . 115.2(17) no
N1 . C37 . H371 . 117.9(17) no
N1 . C41 . C42 . 119.7(2) yes
N1 . C41 . C46 . 121.0(2) yes
C42 . C41 . C46 . 119.3(3) yes
C41 . C42 . C43 . 120.6(3) yes
C41 . C42 . H421 . 120(2) no
C43 . C42 . H421 . 119(2) no
C42 . C43 . C44 . 118.5(3) yes
C42 . C43 . H431 . 122(2) no
C44 . C43 . H431 . 120(2) no
N2 . C44 . C43 . 118.9(3) yes
N2 . C44 . C45 . 119.3(3) yes
C43 . C44 . C45 . 121.8(3) yes
C44 . C45 . C46 . 119.0(3) yes
C44 . C45 . H451 . 122(2) no
C46 . C45 . H451 . 119(2) no
C45 . C46 . C41 . 120.7(3) yes
C45 . C46 . H461 . 120(2) no
C41 . C46 . H461 . 119(2) no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O2 C37 3.453(4) . 2_775 no
O2 C14 3.564(4) . 2_665 no
O3 C12 3.462(4) . 1_655 no
O3 C42 3.482(5) . 2_775 no
O3 C13 3.596(4) . 1_655 no
N2 C41 3.524(4) . 2_775 no
C4 C37 3.335(4) . 1_455 no
C12 C12 3.398(6) . 2_665 no
C12 C13 3.420(4) . 2_665 no
C15 C37 3.565(4) . 1_545 no
C15 C36 3.580(4) . 1_545 no
C16 C36 3.533(4) . 1_545 no
C31 C33 3.423(4) . 2_676 no
C32 C33 3.545(4) . 2_676 no
C32 C32 3.564(5) . 2_676 no
C42 C42 3.536(7) . 2_675 no
C43 C45 3.406(5) . 2_775 no
C43 C44 3.575(5) . 2_775 no
C44 C44 3.497(8) . 2_775 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 P1 C1 . . . . 33.0(1) no
Pd1 Se1 P1 C11 . . . . 151.91(8) no
Pd1 Se1 P1 C21 . . . . -86.5(1) no
Pd1 O1 C31 C32 . . . . -161.3(2) no
Pd1 O1 C31 C36 . . . . 20.2(3) no
Pd1 N1 C37 C36 . . . . -11.9(3) no
Pd1 N1 C41 C42 . . . . 76.8(3) no
Pd1 N1 C41 C46 . . . . -100.6(3) no
Pd1 C2 C1 P1 . . . . -2.4(3) no
Pd1 C2 C1 C6 . . . . 179.4(2) no
Pd1 C2 C3 C4 . . . . -179.1(2) no
Se1 Pd1 N1 C37 . . . . -159.3(2) no
Se1 Pd1 N1 C41 . . . . 9.7(2) no
Se1 Pd1 C2 C1 . . . . 24.4(2) no
Se1 Pd1 C2 C3 . . . . -157.3(2) no
Se1 P1 C1 C2 . . . . -24.7(2) no
Se1 P1 C1 C6 . . . . 153.4(2) no
Se1 P1 C11 C12 . . . . -24.9(2) no
Se1 P1 C11 C16 . . . . 161.8(2) no
Se1 P1 C21 C22 . . . . -72.0(3) no
Se1 P1 C21 C26 . . . . 103.2(3) no
P1 Se1 Pd1 N1 . . . . 146.54(6) no
P1 Se1 Pd1 C2 . . . . -29.16(7) no
P1 C1 C2 C3 . . . . 179.2(2) no
P1 C1 C6 C5 . . . . -178.4(2) no
P1 C11 C12 C13 . . . . -172.4(2) no
P1 C11 C16 C15 . . . . 172.2(2) no
P1 C21 C22 C23 . . . . 174.7(3) no
P1 C21 C26 C25 . . . . -174.5(3) no
O1 Pd1 N1 C37 . . . . 24.5(2) no
O1 Pd1 N1 C41 . . . . -166.5(2) no
O1 Pd1 C2 C1 . . . . -159.6(2) no
O1 Pd1 C2 C3 . . . . 18.7(2) no
O1 C31 C32 C33 . . . . 177.5(2) no
O1 C31 C36 C35 . . . . -178.4(2) no
O1 C31 C36 C37 . . . . 4.2(3) no
O2 N2 C44 C43 . . . . -4.1(5) no
O2 N2 C44 C45 . . . . 175.7(3) no
O3 N2 C44 C43 . . . . 176.0(3) no
O3 N2 C44 C45 . . . . -4.1(5) no
N1 Pd1 O1 C31 . . . . -28.9(2) no
N1 C37 C36 C31 . . . . -8.1(4) no
N1 C37 C36 C35 . . . . 174.5(2) no
N1 C41 C42 C43 . . . . -174.1(3) no
N1 C41 C46 C45 . . . . 174.4(3) no
N2 C44 C43 C42 . . . . 177.2(3) no
N2 C44 C45 C46 . . . . -176.8(3) no
C1 P1 C11 C12 . . . . 91.7(2) no
C1 P1 C11 C16 . . . . -81.5(2) no
C1 P1 C21 C22 . . . . 171.9(3) no
C1 P1 C21 C26 . . . . -12.9(3) no
C1 C2 C3 C4 . . . . -0.7(4) no
C1 C6 C5 C4 . . . . -0.8(4) no
C2 Pd1 O1 C31 . . . . 146.6(2) no
C2 C1 P1 C11 . . . . -146.6(2) no
C2 C1 P1 C21 . . . . 94.9(2) no
C2 C1 C6 C5 . . . . -0.4(4) no
C2 C3 C4 C5 . . . . -0.5(4) no
C3 C2 C1 C6 . . . . 1.1(4) no
C3 C4 C5 C6 . . . . 1.2(4) no
C6 C1 P1 C11 . . . . 31.6(3) no
C6 C1 P1 C21 . . . . -86.9(3) no
C11 P1 C21 C22 . . . . 52.8(3) no
C11 P1 C21 C26 . . . . -132.0(3) no
C11 C12 C13 C14 . . . . -0.1(4) no
C11 C16 C15 C14 . . . . 0.5(4) no
C12 C11 P1 C21 . . . . -148.1(2) no
C12 C11 C16 C15 . . . . -1.1(4) no
C12 C13 C14 C15 . . . . -0.6(4) no
C13 C12 C11 C16 . . . . 0.9(4) no
C13 C14 C15 C16 . . . . 0.3(4) no
C16 C11 P1 C21 . . . . 38.6(2) no
C21 C22 C23 C24 . . . . -0.2(6) no
C21 C26 C25 C24 . . . . -0.2(6) no
C22 C21 C26 C25 . . . . 0.8(5) no
C22 C23 C24 C25 . . . . 0.7(6) no
C23 C22 C21 C26 . . . . -0.6(5) no
C23 C24 C25 C26 . . . . -0.5(6) no
C31 C32 C33 C34 . . . . 1.6(4) no
C31 C36 C35 C34 . . . . 0.0(4) no
C32 C31 C36 C35 . . . . 3.1(3) no
C32 C31 C36 C37 . . . . -174.2(2) no
C32 C33 C34 C35 . . . . 1.6(4) no
C33 C32 C31 C36 . . . . -4.0(4) no
C33 C34 C35 C36 . . . . -2.4(4) no
C34 C35 C36 C37 . . . . 177.6(2) no
C36 C37 N1 C41 . . . . 178.9(2) no
C37 N1 C41 C42 . . . . -113.7(3) no
C37 N1 C41 C46 . . . . 69.0(3) no
C41 C42 C43 C44 . . . . -0.6(6) no
C41 C46 C45 C44 . . . . -0.2(6) no
C42 C41 C46 C45 . . . . -3.0(5) no
C42 C43 C44 C45 . . . . -2.7(6) no
C43 C42 C41 C46 . . . . 3.3(5) no
C43 C44 C45 C46 . . . . 3.0(6) no
_database_code_depnum_ccdc_archive 'CCDC 999171'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex20b
_audit_creation_date             10-12-17
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record             
;
2010-12-17- Report on C31 H23 N2 O3 P Pd Se 
            (red needle form)
             by   Anthony C. Willis
             for  Steven Priver and Martin Bennett

2010-12-17- passes checkcif tests with minor warnings  
;

_oxford_structure_analysis_title '12171123 ben1009'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   13.0481(2)
_cell_length_b                   9.1069(2)
_cell_length_c                   23.0277(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.5870(11)
_cell_angle_gamma                90
_cell_volume                     2735.28(8)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C31 H23 N2 O3 P1 Pd1 Se1 
# Dc =      1.67 Fooo =   1368.00 Mu =     21.04 M =    687.87
# Found Formula = C31 H23 N2 O3 P1 Pd1 Se1 
# Dc =      1.67 FOOO =   1368.00 Mu =     21.04 M =    687.87

_chemical_formula_sum            'C31 H23 N2 O3 P Pd Se'
_chemical_formula_moiety         'C31 H23 N2 O3 P Pd Se'
_chemical_compound_source        ?
_chemical_formula_weight         687.87


_cell_measurement_reflns_used    34222
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      26
_cell_measurement_temperature    200

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.020
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_max          0.370

_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    2.104

# Sheldrick geometric approximatio 0.92 0.96 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.001
-1 0 0 0.020
0 0 1 0.010
0 0 -1 0.030
0 1 0 0.190
0 -1 0 0.180


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.050

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ' φ and ω scans with CCD '
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.5 deg at rate 255 sec/frame,
crystal-detector distance 30mm,
multiple scan sets so over 95 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            45304
_reflns_number_total             5392
_diffrn_reflns_av_R_equivalents  0.079
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5392 
# Theoretical number of reflections is about 10810 


_diffrn_reflns_theta_min         2.728
_diffrn_reflns_theta_max         26.048
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        26.048
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      49.12

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.85
_refine_diff_density_max         0.82


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         5391
_refine_ls_number_restraints     0
_refine_ls_number_parameters     352
_oxford_refine_ls_R_factor_ref   0.0446
_refine_ls_wR_factor_ref         0.0666
_refine_ls_goodness_of_fit_ref   0.9854
_refine_ls_shift/su_max          0.0010416
_refine_ls_shift/su_mean         4.3865395


# The values computed from all data 
_oxford_reflns_number_all        5391
_refine_ls_R_factor_all          0.0446
_refine_ls_wR_factor_all         0.0666

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4351
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_gt          0.0622

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 2.40P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;                                                                               


;


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.522851(16) 0.10920(2) 0.367032(9) 0.0226 1.0000 Uani . . . . . . .
Se1 Se 0.39001(2) -0.05740(4) 0.334429(13) 0.0305 1.0000 Uani . . . . . . .
P1 P 0.46815(6) -0.12101(8) 0.25643(3) 0.0243 1.0000 Uani . . . . . . .
O1 O 0.63469(16) 0.2573(2) 0.38960(10) 0.0345 1.0000 Uani . . . . . . .
O2 O 0.1065(2) -0.1793(4) 0.54866(12) 0.0620 1.0000 Uani . . . . . . .
O3 O 0.0367(2) 0.0339(4) 0.56019(11) 0.0579 1.0000 Uani . . . . . . .
N1 N 0.42313(18) 0.2256(3) 0.42188(10) 0.0253 1.0000 Uani . . . . . . .
N2 N 0.1029(2) -0.0463(4) 0.54112(12) 0.0462 1.0000 Uani . . . . . . .
C1 C 0.6011(2) -0.0944(3) 0.27328(12) 0.0262 1.0000 Uani . . . . . . .
C2 C 0.6253(2) 0.0019(3) 0.31901(12) 0.0235 1.0000 Uani . . . . . . .
C3 C 0.7301(2) 0.0171(3) 0.33368(13) 0.0287 1.0000 Uani . . . . . . .
C4 C 0.8041(2) -0.0598(4) 0.30436(14) 0.0351 1.0000 Uani . . . . . . .
C5 C 0.7779(2) -0.1551(4) 0.25927(15) 0.0366 1.0000 Uani . . . . . . .
C6 C 0.6760(2) -0.1718(4) 0.24331(13) 0.0332 1.0000 Uani . . . . . . .
C11 C 0.4444(2) -0.3111(3) 0.23799(12) 0.0244 1.0000 Uani . . . . . . .
C12 C 0.4667(3) -0.4161(3) 0.28025(13) 0.0327 1.0000 Uani . . . . . . .
C13 C 0.4491(3) -0.5633(4) 0.26870(14) 0.0373 1.0000 Uani . . . . . . .
C14 C 0.4100(2) -0.6056(3) 0.21492(14) 0.0328 1.0000 Uani . . . . . . .
C15 C 0.3900(2) -0.5027(3) 0.17270(13) 0.0321 1.0000 Uani . . . . . . .
C16 C 0.4071(2) -0.3548(3) 0.18379(13) 0.0305 1.0000 Uani . . . . . . .
C21 C 0.4267(2) -0.0157(3) 0.19343(13) 0.0317 1.0000 Uani . . . . . . .
C22 C 0.3229(3) 0.0150(4) 0.18444(15) 0.0402 1.0000 Uani . . . . . . .
C23 C 0.2901(3) 0.0892(4) 0.13510(17) 0.0494 1.0000 Uani . . . . . . .
C24 C 0.3589(4) 0.1319(4) 0.09471(18) 0.0635 1.0000 Uani . . . . . . .
C25 C 0.4612(4) 0.1043(5) 0.10355(19) 0.0720 1.0000 Uani . . . . . . .
C26 C 0.4956(3) 0.0297(4) 0.15301(16) 0.0538 1.0000 Uani . . . . . . .
C31 C 0.6167(2) 0.3956(3) 0.40024(12) 0.0291 1.0000 Uani . . . . . . .
C32 C 0.6982(3) 0.4962(4) 0.39311(15) 0.0411 1.0000 Uani . . . . . . .
C33 C 0.6856(3) 0.6446(4) 0.40144(14) 0.0434 1.0000 Uani . . . . . . .
C34 C 0.5929(3) 0.7009(4) 0.41962(13) 0.0377 1.0000 Uani . . . . . . .
C35 C 0.5137(3) 0.6065(3) 0.42976(12) 0.0325 1.0000 Uani . . . . . . .
C36 C 0.5226(2) 0.4534(3) 0.41965(12) 0.0266 1.0000 Uani . . . . . . .
C37 C 0.4366(2) 0.3634(3) 0.43450(12) 0.0279 1.0000 Uani . . . . . . .
C41 C 0.3381(2) 0.1553(3) 0.44800(12) 0.0254 1.0000 Uani . . . . . . .
C42 C 0.3532(2) 0.0171(3) 0.47235(12) 0.0281 1.0000 Uani . . . . . . .
C43 C 0.2762(2) -0.0507(4) 0.50252(13) 0.0325 1.0000 Uani . . . . . . .
C44 C 0.1841(2) 0.0216(4) 0.50709(12) 0.0323 1.0000 Uani . . . . . . .
C45 C 0.1653(2) 0.1564(4) 0.48160(13) 0.0352 1.0000 Uani . . . . . . .
C46 C 0.2426(2) 0.2231(4) 0.45134(13) 0.0311 1.0000 Uani . . . . . . .
H31 H 0.7498 0.0796 0.3632 0.0340 1.0000 Uiso R . . . . . .
H41 H 0.8732 -0.0485 0.3148 0.0418 1.0000 Uiso R . . . . . .
H51 H 0.8279 -0.2081 0.2400 0.0436 1.0000 Uiso R . . . . . .
H61 H 0.6565 -0.2339 0.2124 0.0399 1.0000 Uiso R . . . . . .
H121 H 0.4943 -0.3878 0.3163 0.0380 1.0000 Uiso R . . . . . .
H131 H 0.4638 -0.6339 0.2970 0.0452 1.0000 Uiso R . . . . . .
H141 H 0.3991 -0.7046 0.2070 0.0390 1.0000 Uiso R . . . . . .
H151 H 0.3644 -0.5309 0.1366 0.0389 1.0000 Uiso R . . . . . .
H161 H 0.3946 -0.2851 0.1558 0.0368 1.0000 Uiso R . . . . . .
H221 H 0.2763 -0.0144 0.2122 0.0481 1.0000 Uiso R . . . . . .
H231 H 0.2200 0.1101 0.1302 0.0590 1.0000 Uiso R . . . . . .
H241 H 0.3365 0.1791 0.0606 0.0757 1.0000 Uiso R . . . . . .
H251 H 0.5076 0.1349 0.0770 0.0858 1.0000 Uiso R . . . . . .
H261 H 0.5646 0.0116 0.1587 0.0653 1.0000 Uiso R . . . . . .
H321 H 0.7618 0.4616 0.3819 0.0493 1.0000 Uiso R . . . . . .
H331 H 0.7413 0.7072 0.3947 0.0523 1.0000 Uiso R . . . . . .
H341 H 0.5851 0.8021 0.4253 0.0445 1.0000 Uiso R . . . . . .
H351 H 0.4514 0.6433 0.4436 0.0387 1.0000 Uiso R . . . . . .
H371 H 0.3849 0.4115 0.4565 0.0326 1.0000 Uiso R . . . . . .
H421 H 0.4158 -0.0292 0.4685 0.0339 1.0000 Uiso R . . . . . .
H431 H 0.2867 -0.1421 0.5198 0.0395 1.0000 Uiso R . . . . . .
H451 H 0.1023 0.1997 0.4847 0.0414 1.0000 Uiso R . . . . . .
H461 H 0.2307 0.3129 0.4340 0.0370 1.0000 Uiso R . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.15019(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Se1 . 2.4079(4) yes
Pd1 . O1 . 2.043(2) yes
Pd1 . N1 . 2.122(2) yes
Pd1 . C2 . 2.011(3) yes
Se1 . P1 . 2.1686(8) yes
P1 . C1 . 1.784(3) yes
P1 . C11 . 1.807(3) yes
P1 . C21 . 1.809(3) yes
O1 . C31 . 1.306(4) yes
O2 . N2 . 1.224(4) yes
O3 . N2 . 1.223(4) yes
N1 . C37 . 1.299(4) yes
N1 . C41 . 1.429(4) yes
N2 . C44 . 1.471(4) yes
C1 . C2 . 1.400(4) yes
C1 . C6 . 1.402(4) yes
C2 . C3 . 1.407(4) yes
C3 . C4 . 1.384(4) yes
C3 . H31 . 0.918 no
C4 . C5 . 1.389(5) yes
C4 . H41 . 0.933 no
C5 . C6 . 1.378(4) yes
C5 . H51 . 0.933 no
C6 . H61 . 0.939 no
C11 . C12 . 1.389(4) yes
C11 . C16 . 1.385(4) yes
C12 . C13 . 1.385(4) yes
C12 . H121 . 0.932 no
C13 . C14 . 1.381(4) yes
C13 . H131 . 0.932 no
C14 . C15 . 1.370(4) yes
C14 . H141 . 0.930 no
C15 . C16 . 1.388(4) yes
C15 . H151 . 0.923 no
C16 . H161 . 0.915 no
C21 . C22 . 1.393(5) yes
C21 . C26 . 1.376(5) yes
C22 . C23 . 1.380(5) yes
C22 . H221 . 0.935 no
C23 . C24 . 1.367(6) yes
C23 . H231 . 0.938 no
C24 . C25 . 1.369(6) yes
C24 . H241 . 0.935 no
C25 . C26 . 1.390(6) yes
C25 . H251 . 0.915 no
C26 . H261 . 0.920 no
C31 . C32 . 1.417(4) yes
C31 . C36 . 1.420(4) yes
C32 . C33 . 1.376(5) yes
C32 . H321 . 0.931 no
C33 . C34 . 1.389(5) yes
C33 . H331 . 0.940 no
C34 . C35 . 1.368(4) yes
C34 . H341 . 0.937 no
C35 . C36 . 1.419(4) yes
C35 . H351 . 0.943 no
C36 . C37 . 1.437(4) yes
C37 . H371 . 0.960 no
C41 . C42 . 1.390(4) yes
C41 . C46 . 1.394(4) yes
C42 . C43 . 1.383(4) yes
C42 . H421 . 0.925 no
C43 . C44 . 1.377(4) yes
C43 . H431 . 0.930 no
C44 . C45 . 1.380(5) yes
C45 . C46 . 1.382(4) yes
C45 . H451 . 0.917 no
C46 . H461 . 0.922 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Se1 . Pd1 . O1 . 176.28(6) yes
Se1 . Pd1 . N1 . 93.01(6) yes
O1 . Pd1 . N1 . 87.95(9) yes
Se1 . Pd1 . C2 . 90.34(8) yes
O1 . Pd1 . C2 . 88.84(10) yes
N1 . Pd1 . C2 . 176.05(10) yes
Pd1 . Se1 . P1 . 94.34(2) yes
Se1 . P1 . C1 . 105.09(10) yes
Se1 . P1 . C11 . 111.66(10) yes
C1 . P1 . C11 . 109.89(13) yes
Se1 . P1 . C21 . 112.68(10) yes
C1 . P1 . C21 . 111.70(14) yes
C11 . P1 . C21 . 105.90(13) yes
Pd1 . O1 . C31 . 123.60(19) yes
Pd1 . N1 . C37 . 122.3(2) yes
Pd1 . N1 . C41 . 121.51(18) yes
C37 . N1 . C41 . 116.2(2) yes
O2 . N2 . O3 . 124.4(3) yes
O2 . N2 . C44 . 117.8(3) yes
O3 . N2 . C44 . 117.8(3) yes
P1 . C1 . C2 . 116.5(2) yes
P1 . C1 . C6 . 120.8(2) yes
C2 . C1 . C6 . 122.7(3) yes
C1 . C2 . Pd1 . 125.4(2) yes
C1 . C2 . C3 . 116.1(3) yes
Pd1 . C2 . C3 . 118.5(2) yes
C2 . C3 . C4 . 121.3(3) yes
C2 . C3 . H31 . 119.3 no
C4 . C3 . H31 . 119.4 no
C3 . C4 . C5 . 121.4(3) yes
C3 . C4 . H41 . 120.1 no
C5 . C4 . H41 . 118.6 no
C4 . C5 . C6 . 119.0(3) yes
C4 . C5 . H51 . 121.1 no
C6 . C5 . H51 . 119.9 no
C1 . C6 . C5 . 119.6(3) yes
C1 . C6 . H61 . 119.9 no
C5 . C6 . H61 . 120.5 no
P1 . C11 . C12 . 117.6(2) yes
P1 . C11 . C16 . 122.7(2) yes
C12 . C11 . C16 . 119.7(3) yes
C11 . C12 . C13 . 120.1(3) yes
C11 . C12 . H121 . 120.1 no
C13 . C12 . H121 . 119.8 no
C12 . C13 . C14 . 119.8(3) yes
C12 . C13 . H131 . 120.2 no
C14 . C13 . H131 . 119.9 no
C13 . C14 . C15 . 120.3(3) yes
C13 . C14 . H141 . 119.8 no
C15 . C14 . H141 . 120.0 no
C14 . C15 . C16 . 120.5(3) yes
C14 . C15 . H151 . 120.3 no
C16 . C15 . H151 . 119.2 no
C15 . C16 . C11 . 119.6(3) yes
C15 . C16 . H161 . 121.2 no
C11 . C16 . H161 . 119.1 no
P1 . C21 . C22 . 119.6(3) yes
P1 . C21 . C26 . 121.0(3) yes
C22 . C21 . C26 . 119.4(3) yes
C21 . C22 . C23 . 120.0(4) yes
C21 . C22 . H221 . 119.3 no
C23 . C22 . H221 . 120.7 no
C22 . C23 . C24 . 120.3(4) yes
C22 . C23 . H231 . 118.6 no
C24 . C23 . H231 . 121.1 no
C23 . C24 . C25 . 120.2(4) yes
C23 . C24 . H241 . 120.5 no
C25 . C24 . H241 . 119.3 no
C24 . C25 . C26 . 120.2(4) yes
C24 . C25 . H251 . 120.4 no
C26 . C25 . H251 . 119.4 no
C25 . C26 . C21 . 119.9(4) yes
C25 . C26 . H261 . 119.8 no
C21 . C26 . H261 . 120.3 no
O1 . C31 . C32 . 117.6(3) yes
O1 . C31 . C36 . 125.3(3) yes
C32 . C31 . C36 . 117.1(3) yes
C31 . C32 . C33 . 121.8(3) yes
C31 . C32 . H321 . 119.4 no
C33 . C32 . H321 . 118.8 no
C32 . C33 . C34 . 120.9(3) yes
C32 . C33 . H331 . 118.5 no
C34 . C33 . H331 . 120.6 no
C33 . C34 . C35 . 119.2(3) yes
C33 . C34 . H341 . 120.2 no
C35 . C34 . H341 . 120.6 no
C34 . C35 . C36 . 121.6(3) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 118.6 no
C31 . C36 . C35 . 119.4(3) yes
C31 . C36 . C37 . 123.4(3) yes
C35 . C36 . C37 . 117.0(3) yes
C36 . C37 . N1 . 126.8(3) yes
C36 . C37 . H371 . 115.5 no
N1 . C37 . H371 . 117.7 no
N1 . C41 . C42 . 118.2(3) yes
N1 . C41 . C46 . 122.0(3) yes
C42 . C41 . C46 . 119.7(3) yes
C41 . C42 . C43 . 120.7(3) yes
C41 . C42 . H421 . 119.3 no
C43 . C42 . H421 . 120.0 no
C42 . C43 . C44 . 118.2(3) yes
C42 . C43 . H431 . 120.9 no
C44 . C43 . H431 . 120.9 no
N2 . C44 . C43 . 118.8(3) yes
N2 . C44 . C45 . 118.6(3) yes
C43 . C44 . C45 . 122.6(3) yes
C44 . C45 . C46 . 118.8(3) yes
C44 . C45 . H451 . 120.0 no
C46 . C45 . H451 . 121.2 no
C41 . C46 . C45 . 119.9(3) yes
C41 . C46 . H461 . 120.6 no
C45 . C46 . H461 . 119.5 no


#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 C43 3.302(4) . 2_656 no
O2 O3 3.357(4) . 2_556 no
O3 N2 2.922(4) . 2_556 no
O3 O3 2.973(5) . 2_556 no
O3 C44 3.272(4) . 2_556 no
O3 C15 3.276(4) . 4_445 no
O3 C45 3.277(4) . 2_556 no
O3 C25 3.589(6) . 4_455 no
N2 N2 3.351(5) . 2_556 no
N2 C3 3.575(4) . 2_656 no
C3 C6 3.576(4) . 3_655 no
C12 C36 3.481(4) . 1_545 no
C12 C35 3.486(4) . 1_545 no
C13 C36 3.583(4) . 1_545 no
C34 C41 3.416(4) . 2_666 no
C34 C37 3.442(4) . 2_666 no
C35 C37 3.187(4) . 2_666 no
C35 C36 3.555(4) . 2_666 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 Se1 P1 C1 . . . . 26.6(1) no
Pd1 Se1 P1 C11 . . . . 145.8(1) no
Pd1 Se1 P1 C21 . . . . -95.2(1) no
Pd1 O1 C31 C32 . . . . -156.0(2) no
Pd1 O1 C31 C36 . . . . 25.5(4) no
Pd1 N1 C37 C36 . . . . -6.8(4) no
Pd1 N1 C41 C42 . . . . 43.8(3) no
Pd1 N1 C41 C46 . . . . -138.4(2) no
Pd1 C2 C1 P1 . . . . 0.7(3) no
Pd1 C2 C1 C6 . . . . -176.7(2) no
Pd1 C2 C3 C4 . . . . 176.5(2) no
Se1 Pd1 N1 C37 . . . . -151.6(2) no
Se1 Pd1 N1 C41 . . . . 29.7(2) no
Se1 Pd1 C2 C1 . . . . 17.4(2) no
Se1 Pd1 C2 C3 . . . . -159.0(2) no
Se1 P1 C1 C2 . . . . -21.2(2) no
Se1 P1 C1 C6 . . . . 156.2(2) no
Se1 P1 C11 C12 . . . . -54.9(3) no
Se1 P1 C11 C16 . . . . 126.2(2) no
Se1 P1 C21 C22 . . . . -41.8(3) no
Se1 P1 C21 C26 . . . . 140.8(2) no
P1 Se1 Pd1 N1 . . . . 159.48(7) no
P1 Se1 Pd1 C2 . . . . -22.62(8) no
P1 C1 C2 C3 . . . . 177.2(2) no
P1 C1 C6 C5 . . . . -176.5(3) no
P1 C11 C12 C13 . . . . 179.4(3) no
P1 C11 C16 C15 . . . . -179.6(2) no
P1 C21 C22 C23 . . . . -176.9(3) no
P1 C21 C26 C25 . . . . 176.9(3) no
O1 Pd1 N1 C37 . . . . 24.8(2) no
O1 Pd1 N1 C41 . . . . -153.9(2) no
O1 Pd1 C2 C1 . . . . -159.0(2) no
O1 Pd1 C2 C3 . . . . 24.6(2) no
O1 C31 C32 C33 . . . . 177.8(3) no
O1 C31 C36 C35 . . . . 179.8(3) no
O1 C31 C36 C37 . . . . 5.1(4) no
O2 N2 C44 C43 . . . . -22.3(4) no
O2 N2 C44 C45 . . . . 158.6(3) no
O3 N2 C44 C43 . . . . 157.4(3) no
O3 N2 C44 C45 . . . . -21.8(4) no
N1 Pd1 O1 C31 . . . . -34.0(2) no
N1 C37 C36 C31 . . . . -15.0(4) no
N1 C37 C36 C35 . . . . 170.2(3) no
N1 C41 C42 C43 . . . . 174.5(3) no
N1 C41 C46 C45 . . . . -174.2(3) no
N2 C44 C43 C42 . . . . -177.5(3) no
N2 C44 C45 C46 . . . . 177.7(3) no
C1 P1 C11 C12 . . . . 61.3(3) no
C1 P1 C11 C16 . . . . -117.6(2) no
C1 P1 C21 C22 . . . . -159.8(2) no
C1 P1 C21 C26 . . . . 22.8(3) no
C1 C2 C3 C4 . . . . -0.2(4) no
C1 C6 C5 C4 . . . . -0.9(5) no
C2 Pd1 O1 C31 . . . . 148.3(2) no
C2 C1 P1 C11 . . . . -141.5(2) no
C2 C1 P1 C21 . . . . 101.3(2) no
C2 C1 C6 C5 . . . . 0.7(5) no
C2 C3 C4 C5 . . . . -0.0(5) no
C3 C2 C1 C6 . . . . -0.1(4) no
C3 C4 C5 C6 . . . . 0.6(5) no
C6 C1 P1 C11 . . . . 35.9(3) no
C6 C1 P1 C21 . . . . -81.3(3) no
C11 P1 C21 C22 . . . . 80.5(3) no
C11 P1 C21 C26 . . . . -96.9(3) no
C11 C12 C13 C14 . . . . 0.5(6) no
C11 C16 C15 C14 . . . . -0.2(4) no
C12 C11 P1 C21 . . . . -177.9(2) no
C12 C11 C16 C15 . . . . 1.6(4) no
C12 C13 C14 C15 . . . . 1.0(5) no
C13 C12 C11 C16 . . . . -1.7(5) no
C13 C14 C15 C16 . . . . -1.1(4) no
C16 C11 P1 C21 . . . . 3.2(3) no
C21 C22 C23 C24 . . . . 0.5(5) no
C21 C26 C25 C24 . . . . -0.4(6) no
C22 C21 C26 C25 . . . . -0.6(5) no
C22 C23 C24 C25 . . . . -1.5(6) no
C23 C22 C21 C26 . . . . 0.5(5) no
C23 C24 C25 C26 . . . . 1.5(6) no
C31 C32 C33 C34 . . . . 2.7(5) no
C31 C36 C35 C34 . . . . 1.9(4) no
C32 C31 C36 C35 . . . . 1.2(4) no
C32 C31 C36 C37 . . . . -173.5(3) no
C32 C33 C34 C35 . . . . 0.6(5) no
C33 C32 C31 C36 . . . . -3.5(5) no
C33 C34 C35 C36 . . . . -2.9(5) no
C34 C35 C36 C37 . . . . 177.0(3) no
C36 C37 N1 C41 . . . . 172.0(3) no
C37 N1 C41 C42 . . . . -135.0(3) no
C37 N1 C41 C46 . . . . 42.8(4) no
C41 C42 C43 C44 . . . . 0.8(4) no
C41 C46 C45 C44 . . . . -1.2(5) no
C42 C41 C46 C45 . . . . 3.6(4) no
C42 C43 C44 C45 . . . . 1.7(5) no
C43 C42 C41 C46 . . . . -3.4(4) no
C43 C44 C45 C46 . . . . -1.4(5) no
#------------------------------------------------------------------------------




#===END



# start Validation Reply Form
_vrf_PUBL020_GLOBAL              
;
PROBLEM: The number of authors is greater than 20.
RESPONSE: The same authors are mentioned for each structure, leading to an erroneous sum.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 999172'
