# Electronic Supplementary Material (ESI) for ChemComm.
# 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_complex_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H27 F3 N P Pd'
_chemical_formula_sum            'C37 H27 F3 N P Pd'
_chemical_formula_weight         679.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   18.5049(9)
_cell_length_b                   8.9306(4)
_cell_length_c                   19.6878(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.881(2)
_cell_angle_gamma                90.00
_cell_volume                     3019.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8418
_exptl_absorpt_correction_T_max  0.9193
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77364
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         30.58
_reflns_number_total             9264
_reflns_number_gt                7991
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0265P)²+2.0493P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9264
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0593
_refine_ls_wR_factor_gt          0.0562
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.863480(6) 0.793420(11) 0.588864(5) 0.01196(3) Uani 1 1 d . . .
N1 N 0.96317(7) 0.64946(13) 0.61201(6) 0.0147(2) Uani 1 1 d . . .
F1 F 0.71033(6) 0.74224(12) 0.62112(6) 0.0325(2) Uani 1 1 d . . .
F2 F 0.79851(6) 1.06193(11) 0.47831(6) 0.0297(2) Uani 1 1 d . . .
F3 F 0.55139(6) 1.13154(12) 0.48678(7) 0.0407(3) Uani 1 1 d . . .
P1 P 0.91275(2) 0.98896(4) 0.675735(19) 0.01267(7) Uani 1 1 d . . .
C1 C 0.81812(8) 0.63959(15) 0.50757(7) 0.0141(2) Uani 1 1 d . . .
C2 C 0.74360(8) 0.62467(16) 0.45393(8) 0.0175(3) Uani 1 1 d . . .
H2 H 0.7044 0.6950 0.4520 0.021 Uiso 1 1 calc R . .
C3 C 0.72569(9) 0.50824(18) 0.40305(8) 0.0215(3) Uani 1 1 d . . .
H3 H 0.6744 0.5005 0.3674 0.026 Uiso 1 1 calc R . .
C4 C 0.78117(9) 0.40367(18) 0.40339(8) 0.0229(3) Uani 1 1 d . . .
H4 H 0.7684 0.3263 0.3677 0.027 Uiso 1 1 calc R . .
C5 C 0.85563(9) 0.41353(17) 0.45655(8) 0.0196(3) Uani 1 1 d . . .
H5 H 0.8942 0.3420 0.4582 0.024 Uiso 1 1 calc R . .
C6 C 0.87317(8) 0.52987(15) 0.50762(7) 0.0148(2) Uani 1 1 d . . .
C7 C 0.94893(8) 0.53989(16) 0.56628(7) 0.0156(3) Uani 1 1 d . . .
H7 H 0.9877 0.4665 0.5710 0.019 Uiso 1 1 calc R . .
C8 C 1.03547(8) 0.64387(16) 0.67386(8) 0.0170(3) Uani 1 1 d . . .
C9 C 1.08975(8) 0.75821(17) 0.68607(9) 0.0198(3) Uani 1 1 d . . .
H9 H 1.0801 0.8396 0.6528 0.024 Uiso 1 1 calc R . .
C10 C 1.15842(9) 0.7521(2) 0.74760(10) 0.0274(4) Uani 1 1 d . . .
H10 H 1.1959 0.8297 0.7563 0.033 Uiso 1 1 calc R . .
C11 C 1.17244(10) 0.6336(2) 0.79629(10) 0.0320(4) Uani 1 1 d . . .
H11 H 1.2193 0.6304 0.8383 0.038 Uiso 1 1 calc R . .
C12 C 1.11830(10) 0.5201(2) 0.78361(9) 0.0319(4) Uani 1 1 d . . .
H12 H 1.1280 0.4389 0.8170 0.038 Uiso 1 1 calc R . .
C13 C 1.04956(9) 0.52437(18) 0.72199(9) 0.0240(3) Uani 1 1 d . . .
H13 H 1.0125 0.4458 0.7130 0.029 Uiso 1 1 calc R . .
C14 C 0.76072(8) 0.89751(16) 0.55247(8) 0.0160(3) Uani 1 1 d . . .
C15 C 0.70003(9) 0.85965(17) 0.57438(9) 0.0205(3) Uani 1 1 d . . .
C16 C 0.62926(9) 0.93321(19) 0.55380(9) 0.0259(3) Uani 1 1 d . . .
H16 H 0.5897 0.9024 0.5707 0.031 Uiso 1 1 calc R . .
C17 C 0.61947(9) 1.05348(18) 0.50751(10) 0.0262(3) Uani 1 1 d . . .
C18 C 0.67505(9) 1.09943(18) 0.48167(9) 0.0252(3) Uani 1 1 d . . .
H18 H 0.6671 1.1828 0.4497 0.030 Uiso 1 1 calc R . .
C19 C 0.74356(8) 1.01721(17) 0.50483(8) 0.0201(3) Uani 1 1 d . . .
C20 C 0.84516(8) 1.14021(15) 0.67164(7) 0.0148(2) Uani 1 1 d . . .
C21 C 0.78516(9) 1.11034(18) 0.69668(8) 0.0210(3) Uani 1 1 d . . .
H21 H 0.7826 1.0155 0.7176 0.025 Uiso 1 1 calc R . .
C22 C 0.72937(10) 1.21790(19) 0.69128(9) 0.0257(3) Uani 1 1 d . . .
H22 H 0.6890 1.1966 0.7086 0.031 Uiso 1 1 calc R . .
C23 C 0.73222(10) 1.35617(19) 0.66075(9) 0.0259(3) Uani 1 1 d . . .
H23 H 0.6934 1.4291 0.6564 0.031 Uiso 1 1 calc R . .
C24 C 0.79172(10) 1.38801(18) 0.63652(9) 0.0257(3) Uani 1 1 d . . .
H24 H 0.7942 1.4835 0.6163 0.031 Uiso 1 1 calc R . .
C25 C 0.84805(9) 1.28014(16) 0.64177(8) 0.0196(3) Uani 1 1 d . . .
H25 H 0.8887 1.3024 0.6248 0.024 Uiso 1 1 calc R . .
C26 C 0.99247(8) 1.08090(15) 0.65862(7) 0.0135(2) Uani 1 1 d . . .
C27 C 0.98415(8) 1.10031(16) 0.58544(8) 0.0166(3) Uani 1 1 d . . .
H27 H 0.9371 1.0715 0.5472 0.020 Uiso 1 1 calc R . .
C28 C 1.04441(9) 1.16147(17) 0.56846(8) 0.0196(3) Uani 1 1 d . . .
H28 H 1.0382 1.1751 0.5187 0.023 Uiso 1 1 calc R . .
C29 C 1.11360(9) 1.20266(18) 0.62390(9) 0.0216(3) Uani 1 1 d . . .
H29 H 1.1547 1.2444 0.6122 0.026 Uiso 1 1 calc R . .
C30 C 1.12259(9) 1.18278(18) 0.69630(9) 0.0224(3) Uani 1 1 d . . .
H30 H 1.1702 1.2100 0.7343 0.027 Uiso 1 1 calc R . .
C31 C 1.06219(8) 1.12312(17) 0.71371(8) 0.0176(3) Uani 1 1 d . . .
H31 H 1.0685 1.1111 0.7636 0.021 Uiso 1 1 calc R . .
C32 C 0.95231(8) 0.94439(16) 0.77310(7) 0.0156(3) Uani 1 1 d . . .
C33 C 0.97139(9) 1.05641(18) 0.82663(8) 0.0213(3) Uani 1 1 d . . .
H33 H 0.9600 1.1581 0.8126 0.026 Uiso 1 1 calc R . .
C34 C 1.00699(10) 1.0195(2) 0.90031(9) 0.0279(3) Uani 1 1 d . . .
H34 H 1.0206 1.0960 0.9364 0.034 Uiso 1 1 calc R . .
C35 C 1.02263(10) 0.8706(2) 0.92101(9) 0.0305(4) Uani 1 1 d . . .
H35 H 1.0477 0.8456 0.9713 0.037 Uiso 1 1 calc R . .
C36 C 1.00183(11) 0.7592(2) 0.86879(10) 0.0301(4) Uani 1 1 d . . .
H36 H 1.0116 0.6574 0.8832 0.036 Uiso 1 1 calc R . .
C37 C 0.96649(9) 0.79567(18) 0.79484(9) 0.0213(3) Uani 1 1 d . . .
H37 H 0.9520 0.7184 0.7591 0.026 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C14 1.9945(13) . ?
Pd1 C1 2.0377(14) . ?
Pd1 N1 2.1534(11) . ?
Pd1 P1 2.3756(4) . ?
N1 C7 1.2887(18) . ?
N1 C8 1.4357(17) . ?
F1 C15 1.3608(18) . ?
F2 C19 1.3644(18) . ?
F3 C17 1.3625(17) . ?
P1 C20 1.8220(14) . ?
P1 C32 1.8228(14) . ?
P1 C26 1.8262(14) . ?
C1 C2 1.3962(19) . ?
C1 C6 1.4131(19) . ?
C2 C3 1.395(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.388(2) . ?
C5 C6 1.397(2) . ?
C6 C7 1.4493(19) . ?
C8 C13 1.386(2) . ?
C8 C9 1.389(2) . ?
C9 C10 1.392(2) . ?
C10 C11 1.386(3) . ?
C11 C12 1.381(3) . ?
C12 C13 1.393(2) . ?
C14 C19 1.379(2) . ?
C14 C15 1.386(2) . ?
C15 C16 1.384(2) . ?
C16 C17 1.376(3) . ?
C17 C18 1.369(2) . ?
C18 C19 1.387(2) . ?
C20 C25 1.391(2) . ?
C20 C21 1.398(2) . ?
C21 C22 1.385(2) . ?
C22 C23 1.383(2) . ?
C23 C24 1.383(2) . ?
C24 C25 1.394(2) . ?
C26 C31 1.3928(19) . ?
C26 C27 1.4014(19) . ?
C27 C28 1.390(2) . ?
C28 C29 1.387(2) . ?
C29 C30 1.383(2) . ?
C30 C31 1.391(2) . ?
C32 C37 1.390(2) . ?
C32 C33 1.400(2) . ?
C33 C34 1.391(2) . ?
C34 C35 1.389(3) . ?
C35 C36 1.378(3) . ?
C36 C37 1.394(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 Pd1 C1 88.49(6) . . ?
C14 Pd1 N1 168.86(5) . . ?
C1 Pd1 N1 80.40(5) . . ?
C14 Pd1 P1 88.55(4) . . ?
C1 Pd1 P1 175.06(4) . . ?
N1 Pd1 P1 102.58(3) . . ?
C7 N1 C8 116.71(12) . . ?
C7 N1 Pd1 111.69(9) . . ?
C8 N1 Pd1 130.87(9) . . ?
C20 P1 C32 102.03(6) . . ?
C20 P1 C26 104.30(6) . . ?
C32 P1 C26 104.88(6) . . ?
C20 P1 Pd1 116.11(5) . . ?
C32 P1 Pd1 119.51(5) . . ?
C26 P1 Pd1 108.50(4) . . ?
C2 C1 C6 116.29(12) . . ?
C2 C1 Pd1 131.30(11) . . ?
C6 C1 Pd1 112.40(9) . . ?
C3 C2 C1 121.16(14) . . ?
C4 C3 C2 121.42(14) . . ?
C3 C4 C5 119.09(14) . . ?
C4 C5 C6 119.26(14) . . ?
C5 C6 C1 122.75(13) . . ?
C5 C6 C7 121.03(13) . . ?
C1 C6 C7 116.15(12) . . ?
N1 C7 C6 119.26(12) . . ?
C13 C8 C9 120.54(14) . . ?
C13 C8 N1 119.02(13) . . ?
C9 C8 N1 120.42(13) . . ?
C8 C9 C10 119.23(15) . . ?
C11 C10 C9 120.45(16) . . ?
C12 C11 C10 119.95(15) . . ?
C11 C12 C13 120.18(17) . . ?
C8 C13 C12 119.64(16) . . ?
C19 C14 C15 113.13(13) . . ?
C19 C14 Pd1 123.55(11) . . ?
C15 C14 Pd1 123.29(11) . . ?
F1 C15 C16 116.26(14) . . ?
F1 C15 C14 118.21(13) . . ?
C16 C15 C14 125.52(15) . . ?
C17 C16 C15 116.16(15) . . ?
F3 C17 C18 118.29(15) . . ?
F3 C17 C16 118.46(15) . . ?
C18 C17 C16 123.24(14) . . ?
C17 C18 C19 116.12(15) . . ?
F2 C19 C14 118.14(13) . . ?
F2 C19 C18 116.07(14) . . ?
C14 C19 C18 125.78(15) . . ?
C25 C20 C21 118.76(13) . . ?
C25 C20 P1 123.44(11) . . ?
C21 C20 P1 117.72(11) . . ?
C22 C21 C20 120.52(14) . . ?
C23 C22 C21 120.31(14) . . ?
C24 C23 C22 119.85(14) . . ?
C23 C24 C25 120.11(15) . . ?
C20 C25 C24 120.45(14) . . ?
C31 C26 C27 118.83(13) . . ?
C31 C26 P1 123.74(10) . . ?
C27 C26 P1 117.29(10) . . ?
C28 C27 C26 120.34(13) . . ?
C29 C28 C27 120.20(13) . . ?
C30 C29 C28 119.86(14) . . ?
C29 C30 C31 120.25(14) . . ?
C30 C31 C26 120.51(13) . . ?
C37 C32 C33 119.03(14) . . ?
C37 C32 P1 119.22(11) . . ?
C33 C32 P1 121.70(11) . . ?
C34 C33 C32 120.28(15) . . ?
C35 C34 C33 119.93(16) . . ?
C36 C35 C34 120.15(15) . . ?
C35 C36 C37 120.15(16) . . ?
C32 C37 C36 120.39(15) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 1005721'
#######################################################################
#
#                 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_complex_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 F3 N2 P Pd'
_chemical_formula_sum            'C36 H26 F3 N2 P Pd'
_chemical_formula_weight         680.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.9041(6)
_cell_length_b                   12.3289(7)
_cell_length_c                   13.1446(8)
_cell_angle_alpha                92.202(2)
_cell_angle_beta                 110.621(2)
_cell_angle_gamma                102.448(2)
_cell_volume                     1455.37(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8364
_exptl_absorpt_correction_T_max  0.9229
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48365
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         30.63
_reflns_number_total             8958
_reflns_number_gt                8190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0546P)²+2.5792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8958
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.857346(16) 0.683963(12) 0.740279(12) 0.01216(5) Uani 1 1 d . . .
P1 P 1.09076(6) 0.80218(4) 0.75958(4) 0.01314(10) Uani 1 1 d . . .
N1 N 0.9028(2) 0.52424(15) 0.77450(14) 0.0139(3) Uani 1 1 d . . .
N2 N 0.7902(2) 0.44340(15) 0.75699(15) 0.0155(3) Uani 1 1 d . . .
F2 F 0.77455(19) 0.82427(13) 0.53782(12) 0.0264(3) Uani 1 1 d . . .
F3 F 0.5927(2) 1.09738(13) 0.66939(14) 0.0310(3) Uani 1 1 d . . .
F1 F 0.7609(2) 0.82888(14) 0.89179(13) 0.0335(4) Uani 1 1 d . . .
C1 C 0.6506(2) 0.58381(18) 0.69736(17) 0.0158(4) Uani 1 1 d . . .
C2 C 0.5104(3) 0.6042(2) 0.6478(2) 0.0222(4) Uani 1 1 d . . .
H2 H 0.5022 0.6787 0.6377 0.027 Uiso 1 1 calc R . .
C3 C 0.3815(3) 0.5168(2) 0.6127(2) 0.0250(5) Uani 1 1 d . . .
H3 H 0.2873 0.5331 0.5795 0.030 Uiso 1 1 calc R . .
C4 C 0.3888(3) 0.4064(2) 0.6255(2) 0.0227(4) Uani 1 1 d . . .
H4 H 0.3005 0.3477 0.6009 0.027 Uiso 1 1 calc R . .
C5 C 0.5263(3) 0.38303(19) 0.67477(19) 0.0195(4) Uani 1 1 d . . .
H5 H 0.5336 0.3083 0.6849 0.023 Uiso 1 1 calc R . .
C6 C 0.6540(2) 0.47122(17) 0.70927(17) 0.0151(4) Uani 1 1 d . . .
C7 C 1.0398(2) 0.49361(17) 0.83163(17) 0.0141(3) Uani 1 1 d . . .
C8 C 1.1623(2) 0.53059(18) 0.80236(18) 0.0169(4) Uani 1 1 d . . .
H8 H 1.1565 0.5765 0.7453 0.020 Uiso 1 1 calc R . .
C9 C 1.2936(3) 0.4994(2) 0.8579(2) 0.0210(4) Uani 1 1 d . . .
H9 H 1.3770 0.5222 0.8369 0.025 Uiso 1 1 calc R . .
C10 C 1.3035(3) 0.4354(2) 0.9433(2) 0.0229(4) Uani 1 1 d . . .
H10 H 1.3939 0.4151 0.9811 0.027 Uiso 1 1 calc R . .
C11 C 1.1815(3) 0.40064(18) 0.97404(18) 0.0203(4) Uani 1 1 d . . .
H11 H 1.1892 0.3583 1.0339 0.024 Uiso 1 1 calc R . .
C12 C 1.0486(2) 0.42797(17) 0.91705(17) 0.0165(4) Uani 1 1 d . . .
H12 H 0.9640 0.4022 0.9359 0.020 Uiso 1 1 calc R . .
C13 C 0.7694(2) 0.81720(17) 0.71519(17) 0.0147(4) Uani 1 1 d . . .
C14 C 0.7339(3) 0.86968(19) 0.79374(18) 0.0180(4) Uani 1 1 d . . .
C15 C 0.6754(3) 0.96302(19) 0.78308(19) 0.0199(4) Uani 1 1 d . . .
H15 H 0.6535 0.9955 0.8403 0.024 Uiso 1 1 calc R . .
C16 C 0.6506(3) 1.00603(18) 0.6846(2) 0.0196(4) Uani 1 1 d . . .
C17 C 0.6816(3) 0.96017(19) 0.60045(19) 0.0207(4) Uani 1 1 d . . .
H17 H 0.6637 0.9906 0.5330 0.025 Uiso 1 1 calc R . .
C18 C 0.7402(2) 0.86741(18) 0.61988(17) 0.0163(4) Uani 1 1 d . . .
C19 C 1.0978(2) 0.95140(17) 0.75628(17) 0.0148(4) Uani 1 1 d . . .
C20 C 1.0966(2) 1.00560(18) 0.66482(18) 0.0176(4) Uani 1 1 d . . .
H20 H 1.1001 0.9660 0.6027 0.021 Uiso 1 1 calc R . .
C21 C 1.0903(3) 1.11752(19) 0.66402(19) 0.0211(4) Uani 1 1 d . . .
H21 H 1.0904 1.1539 0.6016 0.025 Uiso 1 1 calc R . .
C22 C 1.0840(3) 1.17587(19) 0.7538(2) 0.0220(4) Uani 1 1 d . . .
H22 H 1.0796 1.2521 0.7532 0.026 Uiso 1 1 calc R . .
C23 C 1.0841(3) 1.1221(2) 0.84499(19) 0.0239(5) Uani 1 1 d . . .
H23 H 1.0796 1.1617 0.9067 0.029 Uiso 1 1 calc R . .
C24 C 1.0909(3) 1.01076(19) 0.84639(18) 0.0195(4) Uani 1 1 d . . .
H24 H 1.0908 0.9747 0.9090 0.023 Uiso 1 1 calc R . .
C25 C 1.1381(2) 0.76492(17) 0.64342(16) 0.0138(3) Uani 1 1 d . . .
C26 C 1.0329(2) 0.68139(18) 0.56180(17) 0.0172(4) Uani 1 1 d . . .
H26 H 0.9451 0.6432 0.5717 0.021 Uiso 1 1 calc R . .
C27 C 1.0555(3) 0.6537(2) 0.46640(18) 0.0211(4) Uani 1 1 d . . .
H27 H 0.9831 0.5971 0.4115 0.025 Uiso 1 1 calc R . .
C28 C 1.1838(3) 0.7087(2) 0.45150(19) 0.0220(4) Uani 1 1 d . . .
H28 H 1.1989 0.6904 0.3861 0.026 Uiso 1 1 calc R . .
C29 C 1.2900(3) 0.7904(2) 0.5322(2) 0.0205(4) Uani 1 1 d . . .
H29 H 1.3789 0.8267 0.5227 0.025 Uiso 1 1 calc R . .
C30 C 1.2669(2) 0.81938(18) 0.62679(19) 0.0177(4) Uani 1 1 d . . .
H30 H 1.3391 0.8768 0.6808 0.021 Uiso 1 1 calc R . .
C31 C 1.2440(2) 0.8001(2) 0.88610(18) 0.0200(4) Uani 1 1 d . . .
C32 C 1.3914(4) 0.8176(4) 0.8987(3) 0.0575(12) Uani 1 1 d . . .
H32 H 1.4197 0.8316 0.8376 0.069 Uiso 1 1 calc R . .
C33 C 1.4994(4) 0.8148(5) 1.0004(3) 0.0663(14) Uani 1 1 d . . .
H33 H 1.6008 0.8281 1.0080 0.080 Uiso 1 1 calc R . .
C34 C 1.4618(3) 0.7934(3) 1.0882(2) 0.0395(7) Uani 1 1 d . . .
H34 H 1.5368 0.7977 1.1584 0.047 Uiso 1 1 calc R . .
C35 C 1.3160(4) 0.7657(3) 1.0753(2) 0.0373(7) Uani 1 1 d . . .
H35 H 1.2881 0.7450 1.1354 0.045 Uiso 1 1 calc R . .
C36 C 1.2073(3) 0.7677(2) 0.9740(2) 0.0304(6) Uani 1 1 d . . .
H36 H 1.1054 0.7462 0.9653 0.036 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C13 2.005(2) . ?
Pd1 C1 2.020(2) . ?
Pd1 N1 2.1427(17) . ?
Pd1 P1 2.3746(6) . ?
P1 C25 1.818(2) . ?
P1 C31 1.820(2) . ?
P1 C19 1.829(2) . ?
N1 N2 1.270(3) . ?
N1 C7 1.440(3) . ?
N2 C6 1.397(3) . ?
F2 C18 1.362(2) . ?
F3 C16 1.361(2) . ?
F1 C14 1.360(2) . ?
C1 C2 1.393(3) . ?
C1 C6 1.409(3) . ?
C2 C3 1.399(3) . ?
C3 C4 1.392(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.397(3) . ?
C7 C8 1.389(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.393(3) . ?
C9 C10 1.385(3) . ?
C10 C11 1.394(4) . ?
C11 C12 1.386(3) . ?
C13 C14 1.382(3) . ?
C13 C18 1.385(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.380(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.383(3) . ?
C19 C20 1.395(3) . ?
C19 C24 1.398(3) . ?
C20 C21 1.395(3) . ?
C21 C22 1.386(3) . ?
C22 C23 1.391(3) . ?
C23 C24 1.389(3) . ?
C25 C30 1.401(3) . ?
C25 C26 1.401(3) . ?
C26 C27 1.392(3) . ?
C27 C28 1.389(3) . ?
C28 C29 1.386(4) . ?
C29 C30 1.389(3) . ?
C31 C36 1.377(3) . ?
C31 C32 1.377(4) . ?
C32 C33 1.394(5) . ?
C33 C34 1.351(5) . ?
C34 C35 1.357(5) . ?
C35 C36 1.392(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Pd1 C1 89.38(8) . . ?
C13 Pd1 N1 165.92(8) . . ?
C1 Pd1 N1 78.02(8) . . ?
C13 Pd1 P1 88.78(6) . . ?
C1 Pd1 P1 170.65(6) . . ?
N1 Pd1 P1 104.66(5) . . ?
C25 P1 C31 109.31(10) . . ?
C25 P1 C19 103.45(9) . . ?
C31 P1 C19 103.03(10) . . ?
C25 P1 Pd1 108.92(7) . . ?
C31 P1 Pd1 115.30(8) . . ?
C19 P1 Pd1 116.04(7) . . ?
N2 N1 C7 111.81(17) . . ?
N2 N1 Pd1 115.99(13) . . ?
C7 N1 Pd1 131.26(14) . . ?
N1 N2 C6 114.07(17) . . ?
C2 C1 C6 116.2(2) . . ?
C2 C1 Pd1 131.69(17) . . ?
C6 C1 Pd1 111.66(15) . . ?
C1 C2 C3 121.1(2) . . ?
C4 C3 C2 121.2(2) . . ?
C5 C4 C3 119.2(2) . . ?
C4 C5 C6 118.9(2) . . ?
N2 C6 C5 116.79(19) . . ?
N2 C6 C1 119.84(19) . . ?
C5 C6 C1 123.37(19) . . ?
C8 C7 C12 120.70(19) . . ?
C8 C7 N1 119.80(18) . . ?
C12 C7 N1 119.49(19) . . ?
C7 C8 C9 119.1(2) . . ?
C10 C9 C8 120.5(2) . . ?
C9 C10 C11 120.2(2) . . ?
C12 C11 C10 119.8(2) . . ?
C11 C12 C7 119.7(2) . . ?
C14 C13 C18 112.98(19) . . ?
C14 C13 Pd1 122.60(15) . . ?
C18 C13 Pd1 124.41(16) . . ?
F1 C14 C13 118.11(18) . . ?
F1 C14 C15 116.00(19) . . ?
C13 C14 C15 125.9(2) . . ?
C16 C15 C14 116.2(2) . . ?
F3 C16 C17 118.5(2) . . ?
F3 C16 C15 118.7(2) . . ?
C17 C16 C15 122.8(2) . . ?
C16 C17 C18 116.3(2) . . ?
F2 C18 C17 116.08(19) . . ?
F2 C18 C13 118.00(18) . . ?
C17 C18 C13 125.9(2) . . ?
C20 C19 C24 118.91(19) . . ?
C20 C19 P1 123.02(16) . . ?
C24 C19 P1 117.82(16) . . ?
C21 C20 C19 120.4(2) . . ?
C22 C21 C20 120.3(2) . . ?
C21 C22 C23 119.5(2) . . ?
C24 C23 C22 120.4(2) . . ?
C23 C24 C19 120.4(2) . . ?
C30 C25 C26 118.31(19) . . ?
C30 C25 P1 124.39(16) . . ?
C26 C25 P1 117.14(16) . . ?
C27 C26 C25 120.8(2) . . ?
C28 C27 C26 120.0(2) . . ?
C29 C28 C27 119.9(2) . . ?
C28 C29 C30 120.2(2) . . ?
C29 C30 C25 120.7(2) . . ?
C36 C31 C32 117.1(2) . . ?
C36 C31 P1 116.83(18) . . ?
C32 C31 P1 125.8(2) . . ?
C31 C32 C33 120.6(3) . . ?
C34 C33 C32 120.9(3) . . ?
C33 C34 C35 119.5(3) . . ?
C34 C35 C36 119.9(3) . . ?
C31 C36 C35 121.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         3.451
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 1005722'
#######################################################################
#
#                 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_complex_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H38 F6 O3 P2 Pd2'
_chemical_formula_sum            'C50 H38 F6 O3 P2 Pd2'
_chemical_formula_weight         1075.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.9714(5)
_cell_length_b                   12.3041(5)
_cell_length_c                   16.0441(7)
_cell_angle_alpha                67.9750(10)
_cell_angle_beta                 88.8630(10)
_cell_angle_gamma                86.9690(10)
_cell_volume                     2187.72(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1076
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25529
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         28.23
_reflns_number_total             9820
_reflns_number_gt                8393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0572P)²+0.7517P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9820
_refine_ls_number_parameters     572
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1137
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd2 Pd 0.85816(2) 0.06286(2) 0.198706(18) 0.01900(8) Uani 1 1 d . . .
Pd1 Pd 0.83295(2) -0.17364(2) 0.383006(19) 0.01993(8) Uani 1 1 d . . .
O1 O 0.9392(2) -0.0425(3) 0.31640(19) 0.0270(6) Uani 1 1 d . . .
O2 O 0.8692(2) -0.2465(2) 0.28665(18) 0.0259(6) Uani 1 1 d . . .
C39 C 0.8092(3) 0.1745(3) -0.0299(2) 0.0218(8) Uani 1 1 d . . .
C45 C 0.6159(3) 0.1373(3) 0.0903(3) 0.0218(8) Uani 1 1 d . . .
P2 P 0.76087(8) 0.17919(8) 0.07724(6) 0.0192(2) Uani 1 1 d . . .
P1 P 0.71611(8) -0.31740(8) 0.44628(6) 0.0193(2) Uani 1 1 d . . .
F3 F 0.96789(19) -0.1586(2) 0.54725(17) 0.0379(6) Uani 1 1 d . . .
F1 F 0.61739(19) -0.0314(2) 0.40662(16) 0.0327(5) Uani 1 1 d . . .
C12 C 0.5150(3) -0.2884(3) 0.5318(3) 0.0258(8) Uani 1 1 d . . .
H12 H 0.4773 -0.2829 0.4787 0.031 Uiso 1 1 calc R . .
C2 C 0.6937(3) -0.0397(3) 0.4710(3) 0.0246(8) Uani 1 1 d . . .
C33 C 0.7470(3) 0.3364(3) 0.0549(2) 0.0214(8) Uani 1 1 d . . .
C7 C 0.6306(3) -0.3095(3) 0.5385(2) 0.0208(7) Uani 1 1 d . . .
C8 C 0.6840(3) -0.3190(3) 0.6179(2) 0.0246(8) Uani 1 1 d . . .
H8 H 0.7625 -0.3352 0.6239 0.030 Uiso 1 1 calc R . .
C1 C 0.7946(3) -0.0999(3) 0.4722(2) 0.0217(8) Uani 1 1 d . . .
C19 C 0.6205(3) -0.3184(3) 0.3591(2) 0.0226(8) Uani 1 1 d . . .
C34 C 0.8415(3) 0.4029(3) 0.0277(3) 0.0273(8) Uani 1 1 d . . .
H34 H 0.9109 0.3661 0.0206 0.033 Uiso 1 1 calc R . .
C24 C 0.5973(4) -0.4211(4) 0.3483(3) 0.0348(10) Uani 1 1 d . . .
H24 H 0.6296 -0.4939 0.3879 0.042 Uiso 1 1 calc R . .
C14 C 0.7216(3) -0.5558(3) 0.5570(3) 0.0260(8) Uani 1 1 d . . .
H14 H 0.6558 -0.5369 0.5839 0.031 Uiso 1 1 calc R . .
C6 C 0.8656(3) -0.1025(3) 0.5403(3) 0.0257(8) Uani 1 1 d . . .
C44 C 0.8584(3) 0.0704(4) -0.0317(3) 0.0282(9) Uani 1 1 d . . .
H44 H 0.8687 0.0042 0.0228 0.034 Uiso 1 1 calc R . .
C13 C 0.7768(3) -0.4673(3) 0.4904(2) 0.0213(8) Uani 1 1 d . . .
C18 C 0.8738(3) -0.4958(3) 0.4518(3) 0.0241(8) Uani 1 1 d . . .
H18 H 0.9119 -0.4364 0.4059 0.029 Uiso 1 1 calc R . .
C38 C 0.6466(3) 0.3917(4) 0.0653(3) 0.0310(9) Uani 1 1 d . . .
H38 H 0.5816 0.3477 0.0843 0.037 Uiso 1 1 calc R . .
F4 F 1.0880(2) 0.1876(2) 0.15353(19) 0.0415(6) Uani 1 1 d . . .
F6 F 0.7416(2) 0.2328(2) 0.28229(18) 0.0424(7) Uani 1 1 d . . .
O3 O 0.8088(2) -0.0837(2) 0.17134(18) 0.0264(6) Uani 1 1 d . . .
F5 F 1.0283(2) 0.4834(2) 0.26807(19) 0.0472(7) Uani 1 1 d . . .
C27 C 0.9119(3) 0.2015(3) 0.2179(2) 0.0206(7) Uani 1 1 d . . .
C46 C 0.5672(3) 0.1130(3) 0.1742(3) 0.0287(9) Uani 1 1 d . . .
H46 H 0.6115 0.1084 0.2240 0.034 Uiso 1 1 calc R . .
C3 C 0.6611(4) 0.0113(3) 0.5314(3) 0.0295(9) Uani 1 1 d . . .
H3 H 0.5896 0.0499 0.5283 0.035 Uiso 1 1 calc R . .
C16 C 0.8587(3) -0.6989(3) 0.5466(3) 0.0277(9) Uani 1 1 d . . .
H16 H 0.8867 -0.7782 0.5659 0.033 Uiso 1 1 calc R . .
C5 C 0.8399(4) -0.0525(4) 0.6031(3) 0.0298(9) Uani 1 1 d . . .
H5 H 0.8915 -0.0570 0.6486 0.036 Uiso 1 1 calc R . .
C15 C 0.7621(3) -0.6707(3) 0.5841(3) 0.0282(9) Uani 1 1 d . . .
H15 H 0.7233 -0.7309 0.6288 0.034 Uiso 1 1 calc R . .
C29 C 1.0598(4) 0.3349(4) 0.2111(3) 0.0319(9) Uani 1 1 d . . .
H29 H 1.1342 0.3579 0.1949 0.038 Uiso 1 1 calc R . .
C28 C 1.0178(3) 0.2420(3) 0.1954(3) 0.0256(8) Uani 1 1 d . . .
C17 C 0.9142(3) -0.6122(3) 0.4812(3) 0.0285(9) Uani 1 1 d . . .
H17 H 0.9809 -0.6319 0.4558 0.034 Uiso 1 1 calc R . .
C4 C 0.7379(4) 0.0031(3) 0.5966(3) 0.0296(9) Uani 1 1 d . . .
C31 C 0.8822(4) 0.3601(4) 0.2753(3) 0.0335(10) Uani 1 1 d . . .
H31 H 0.8338 0.4014 0.3021 0.040 Uiso 1 1 calc R . .
C50 C 0.5517(3) 0.1387(3) 0.0191(3) 0.0275(8) Uani 1 1 d . . .
H50 H 0.5856 0.1529 -0.0379 0.033 Uiso 1 1 calc R . .
C43 C 0.8927(4) 0.0625(4) -0.1124(3) 0.0344(10) Uani 1 1 d . . .
H43 H 0.9244 -0.0096 -0.1130 0.041 Uiso 1 1 calc R . .
C35 C 0.8350(4) 0.5219(4) 0.0109(3) 0.0341(10) Uani 1 1 d . . .
H35 H 0.8999 0.5662 -0.0070 0.041 Uiso 1 1 calc R . .
C42 C 0.8810(3) 0.1575(4) -0.1910(3) 0.0339(10) Uani 1 1 d . . .
H42 H 0.9044 0.1515 -0.2461 0.041 Uiso 1 1 calc R . .
C22 C 0.4800(4) -0.3141(4) 0.2229(3) 0.0397(11) Uani 1 1 d . . .
H22 H 0.4313 -0.3123 0.1763 0.048 Uiso 1 1 calc R . .
C49 C 0.4380(4) 0.1194(4) 0.0302(3) 0.0341(10) Uani 1 1 d . . .
H49 H 0.3944 0.1199 -0.0187 0.041 Uiso 1 1 calc R . .
C10 C 0.5086(4) -0.2818(4) 0.6792(3) 0.0328(10) Uani 1 1 d . . .
H10 H 0.4671 -0.2703 0.7265 0.039 Uiso 1 1 calc R . .
C30 C 0.9903(4) 0.3921(3) 0.2508(3) 0.0300(9) Uani 1 1 d . . .
C36 C 0.7351(4) 0.5758(4) 0.0201(3) 0.0396(11) Uani 1 1 d . . .
H36 H 0.7307 0.6578 0.0071 0.048 Uiso 1 1 calc R . .
C41 C 0.8352(4) 0.2627(4) -0.1903(3) 0.0369(10) Uani 1 1 d . . .
H41 H 0.8290 0.3294 -0.2448 0.044 Uiso 1 1 calc R . .
C40 C 0.7981(4) 0.2714(4) -0.1103(3) 0.0309(9) Uani 1 1 d . . .
H40 H 0.7653 0.3435 -0.1105 0.037 Uiso 1 1 calc R . .
C25 C 0.8411(3) -0.1913(3) 0.2063(3) 0.0253(8) Uani 1 1 d . . .
C37 C 0.6408(4) 0.5118(4) 0.0480(3) 0.0407(11) Uani 1 1 d . . .
H37 H 0.5720 0.5495 0.0554 0.049 Uiso 1 1 calc R . .
C32 C 0.8485(3) 0.2648(4) 0.2587(3) 0.0274(8) Uani 1 1 d . . .
C26 C 0.8434(4) -0.2607(4) 0.1458(3) 0.0408(11) Uani 1 1 d . . .
H26A H 0.8202 -0.2090 0.0850 0.061 Uiso 1 1 calc R . .
H26B H 0.7920 -0.3247 0.1694 0.061 Uiso 1 1 calc R . .
H26C H 0.9194 -0.2933 0.1439 0.061 Uiso 1 1 calc R . .
C9 C 0.6234(4) -0.3050(4) 0.6876(3) 0.0317(9) Uani 1 1 d . . .
H9 H 0.6602 -0.3113 0.7413 0.038 Uiso 1 1 calc R . .
C47 C 0.4531(4) 0.0955(4) 0.1851(3) 0.0342(10) Uani 1 1 d . . .
H47 H 0.4192 0.0807 0.2421 0.041 Uiso 1 1 calc R . .
C23 C 0.5268(4) -0.4184(4) 0.2793(3) 0.0434(12) Uani 1 1 d . . .
H23 H 0.5115 -0.4891 0.2717 0.052 Uiso 1 1 calc R . .
C20 C 0.5727(4) -0.2134(4) 0.3000(3) 0.0385(11) Uani 1 1 d . . .
H20 H 0.5885 -0.1418 0.3061 0.046 Uiso 1 1 calc R . .
C11 C 0.4548(3) -0.2755(3) 0.6027(3) 0.0293(9) Uani 1 1 d . . .
H11 H 0.3759 -0.2623 0.5982 0.035 Uiso 1 1 calc R . .
C48 C 0.3887(4) 0.0995(4) 0.1131(4) 0.0391(11) Uani 1 1 d . . .
H48 H 0.3107 0.0886 0.1207 0.047 Uiso 1 1 calc R . .
C21 C 0.5028(5) -0.2118(4) 0.2329(3) 0.0483(13) Uani 1 1 d . . .
H21 H 0.4700 -0.1394 0.1931 0.058 Uiso 1 1 calc R . .
F2 F 0.7103(2) 0.0532(2) 0.65752(17) 0.0434(7) Uani 1 1 d . . .
H1 H 0.937(4) -0.001(4) 0.339(3) 0.034(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd2 C27 1.984(4) . ?
Pd2 O1 2.072(3) . ?
Pd2 O3 2.124(3) . ?
Pd2 P2 2.2417(10) . ?
Pd1 C1 1.996(4) . ?
Pd1 O1 2.058(3) . ?
Pd1 O2 2.087(3) . ?
Pd1 P1 2.2303(10) . ?
O2 C25 1.254(5) . ?
C39 C44 1.392(5) . ?
C39 C40 1.393(5) . ?
C39 P2 1.823(4) . ?
C45 C50 1.385(5) . ?
C45 C46 1.388(5) . ?
C45 P2 1.822(4) . ?
P2 C33 1.829(4) . ?
P1 C7 1.812(4) . ?
P1 C13 1.825(4) . ?
P1 C19 1.829(4) . ?
F3 C6 1.359(4) . ?
F1 C2 1.364(4) . ?
C12 C11 1.389(5) . ?
C12 C7 1.393(5) . ?
C2 C3 1.379(5) . ?
C2 C1 1.380(5) . ?
C33 C38 1.388(5) . ?
C33 C34 1.396(5) . ?
C7 C8 1.399(5) . ?
C8 C9 1.380(5) . ?
C1 C6 1.387(5) . ?
C19 C24 1.381(6) . ?
C19 C20 1.387(5) . ?
C34 C35 1.384(5) . ?
C24 C23 1.395(6) . ?
C14 C15 1.378(5) . ?
C14 C13 1.393(5) . ?
C6 C5 1.385(6) . ?
C44 C43 1.388(6) . ?
C13 C18 1.395(5) . ?
C18 C17 1.391(5) . ?
C38 C37 1.396(6) . ?
F4 C28 1.364(4) . ?
F6 C32 1.364(4) . ?
O3 C25 1.271(4) . ?
F5 C30 1.356(4) . ?
C27 C28 1.378(5) . ?
C27 C32 1.382(5) . ?
C46 C47 1.391(5) . ?
C3 C4 1.377(6) . ?
C16 C17 1.374(6) . ?
C16 C15 1.381(6) . ?
C5 C4 1.353(6) . ?
C29 C30 1.359(6) . ?
C29 C28 1.381(6) . ?
C4 F2 1.366(4) . ?
C31 C32 1.377(6) . ?
C31 C30 1.379(6) . ?
C50 C49 1.391(6) . ?
C43 C42 1.363(6) . ?
C35 C36 1.369(6) . ?
C42 C41 1.382(6) . ?
C22 C23 1.361(6) . ?
C22 C21 1.369(6) . ?
C49 C48 1.384(7) . ?
C10 C11 1.371(6) . ?
C10 C9 1.387(6) . ?
C36 C37 1.381(7) . ?
C41 C40 1.389(6) . ?
C25 C26 1.513(6) . ?
C47 C48 1.385(6) . ?
C20 C21 1.370(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 Pd2 O1 88.24(13) . . ?
C27 Pd2 O3 176.18(13) . . ?
O1 Pd2 O3 92.76(11) . . ?
C27 Pd2 P2 90.99(10) . . ?
O1 Pd2 P2 176.02(9) . . ?
O3 Pd2 P2 88.25(7) . . ?
C1 Pd1 O1 91.10(14) . . ?
C1 Pd1 O2 178.02(13) . . ?
O1 Pd1 O2 88.55(12) . . ?
C1 Pd1 P1 92.40(10) . . ?
O1 Pd1 P1 176.06(9) . . ?
O2 Pd1 P1 87.88(8) . . ?
Pd1 O1 Pd2 106.22(13) . . ?
C25 O2 Pd1 120.0(2) . . ?
C44 C39 C40 118.7(4) . . ?
C44 C39 P2 118.9(3) . . ?
C40 C39 P2 122.4(3) . . ?
C50 C45 C46 119.8(4) . . ?
C50 C45 P2 122.7(3) . . ?
C46 C45 P2 117.3(3) . . ?
C45 P2 C39 106.73(17) . . ?
C45 P2 C33 102.55(17) . . ?
C39 P2 C33 103.31(17) . . ?
C45 P2 Pd2 108.94(13) . . ?
C39 P2 Pd2 115.80(12) . . ?
C33 P2 Pd2 118.20(12) . . ?
C7 P1 C13 103.31(17) . . ?
C7 P1 C19 106.96(17) . . ?
C13 P1 C19 103.17(17) . . ?
C7 P1 Pd1 117.16(12) . . ?
C13 P1 Pd1 117.13(13) . . ?
C19 P1 Pd1 107.87(12) . . ?
C11 C12 C7 120.1(4) . . ?
F1 C2 C3 116.1(3) . . ?
F1 C2 C1 118.4(3) . . ?
C3 C2 C1 125.4(4) . . ?
C38 C33 C34 118.8(4) . . ?
C38 C33 P2 122.5(3) . . ?
C34 C33 P2 118.7(3) . . ?
C12 C7 C8 118.9(3) . . ?
C12 C7 P1 122.7(3) . . ?
C8 C7 P1 118.4(3) . . ?
C9 C8 C7 120.5(4) . . ?
C2 C1 C6 113.3(3) . . ?
C2 C1 Pd1 122.5(3) . . ?
C6 C1 Pd1 124.2(3) . . ?
C24 C19 C20 118.6(4) . . ?
C24 C19 P1 121.8(3) . . ?
C20 C19 P1 119.6(3) . . ?
C35 C34 C33 120.6(4) . . ?
C19 C24 C23 120.3(4) . . ?
C15 C14 C13 120.2(4) . . ?
F3 C6 C5 116.8(3) . . ?
F3 C6 C1 118.3(3) . . ?
C5 C6 C1 124.8(4) . . ?
C43 C44 C39 120.5(4) . . ?
C14 C13 C18 119.5(3) . . ?
C14 C13 P1 120.4(3) . . ?
C18 C13 P1 119.9(3) . . ?
C17 C18 C13 119.3(4) . . ?
C33 C38 C37 120.2(4) . . ?
C25 O3 Pd2 130.3(2) . . ?
C28 C27 C32 112.8(3) . . ?
C28 C27 Pd2 123.7(3) . . ?
C32 C27 Pd2 123.4(3) . . ?
C45 C46 C47 119.8(4) . . ?
C4 C3 C2 116.3(4) . . ?
C17 C16 C15 119.9(4) . . ?
C4 C5 C6 117.0(4) . . ?
C14 C15 C16 120.3(4) . . ?
C30 C29 C28 117.2(4) . . ?
F4 C28 C27 118.4(3) . . ?
F4 C28 C29 116.2(3) . . ?
C27 C28 C29 125.4(4) . . ?
C16 C17 C18 120.7(4) . . ?
C5 C4 F2 118.3(4) . . ?
C5 C4 C3 123.0(4) . . ?
F2 C4 C3 118.7(4) . . ?
C32 C31 C30 116.2(4) . . ?
C45 C50 C49 120.5(4) . . ?
C42 C43 C44 120.5(4) . . ?
C36 C35 C34 120.1(4) . . ?
C43 C42 C41 119.9(4) . . ?
C23 C22 C21 120.3(4) . . ?
C48 C49 C50 119.6(4) . . ?
C11 C10 C9 120.2(4) . . ?
F5 C30 C29 119.2(4) . . ?
F5 C30 C31 118.3(4) . . ?
C29 C30 C31 122.5(4) . . ?
C35 C36 C37 120.5(4) . . ?
C42 C41 C40 120.4(4) . . ?
C41 C40 C39 120.0(4) . . ?
O2 C25 O3 126.4(4) . . ?
O2 C25 C26 116.6(3) . . ?
O3 C25 C26 117.0(4) . . ?
C36 C37 C38 119.8(4) . . ?
F6 C32 C31 116.6(4) . . ?
F6 C32 C27 117.4(3) . . ?
C31 C32 C27 125.9(4) . . ?
C8 C9 C10 119.9(4) . . ?
C48 C47 C46 120.2(4) . . ?
C22 C23 C24 119.8(4) . . ?
C21 C20 C19 120.6(4) . . ?
C10 C11 C12 120.4(4) . . ?
C49 C48 C47 120.1(4) . . ?
C22 C21 C20 120.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.128
_database_code_depnum_ccdc_archive 'CCDC 1005723'
#######################################################################
#
#                 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_complex_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H32 Cl F3 P2 Pd'
_chemical_formula_sum            'C42 H32 Cl F3 P2 Pd'
_chemical_formula_weight         797.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   12.1168(9)
_cell_length_b                   23.2879(19)
_cell_length_c                   24.9924(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7052.2(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8437
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            121306
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         30.59
_reflns_number_total             10820
_reflns_number_gt                8037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0374P)²+52.0968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10820
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1533
_refine_ls_wR_factor_gt          0.1406
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.40303(2) 0.169201(12) 0.140077(11) 0.01419(8) Uani 1 1 d . . .
F1 F 0.2191(2) 0.21321(11) 0.22119(10) 0.0227(5) Uani 1 1 d . . .
F2 F 0.3777(3) 0.16546(17) 0.38642(11) 0.0487(9) Uani 1 1 d . . .
F3 F 0.5687(2) 0.12580(11) 0.22732(10) 0.0229(5) Uani 1 1 d . . .
Cl1 Cl 0.41342(9) 0.16854(5) 0.04537(4) 0.02121(19) Uani 1 1 d . . .
P1 P 0.37006(8) 0.07102(4) 0.13819(4) 0.01480(19) Uani 1 1 d . . .
P2 P 0.43100(8) 0.26725(4) 0.13967(4) 0.01529(19) Uani 1 1 d . . .
C1 C 0.3952(3) 0.16984(16) 0.22015(15) 0.0139(7) Uani 1 1 d . . .
C2 C 0.3052(3) 0.19090(17) 0.24898(17) 0.0186(8) Uani 1 1 d . . .
C3 C 0.2965(4) 0.1905(2) 0.30446(19) 0.0262(9) Uani 1 1 d . . .
H3 H 0.2334 0.2053 0.3223 0.031 Uiso 1 1 calc R . .
C4 C 0.3836(4) 0.1676(2) 0.33189(17) 0.0291(10) Uani 1 1 d . . .
C5 C 0.4765(4) 0.1458(2) 0.30740(18) 0.0256(9) Uani 1 1 d . . .
H5 H 0.5363 0.1304 0.3273 0.031 Uiso 1 1 calc R . .
C6 C 0.4773(3) 0.14776(17) 0.25202(17) 0.0181(8) Uani 1 1 d . . .
C7 C 0.2376(3) 0.0523(2) 0.10759(17) 0.0213(8) Uani 1 1 d . . .
C8 C 0.1896(4) -0.0012(2) 0.1163(2) 0.0304(10) Uani 1 1 d . . .
H8 H 0.2266 -0.0290 0.1376 0.036 Uiso 1 1 calc R . .
C9 C 0.0858(5) -0.0142(3) 0.0935(2) 0.0419(14) Uani 1 1 d . . .
H9 H 0.0533 -0.0509 0.0987 0.050 Uiso 1 1 calc R . .
C10 C 0.0323(4) 0.0272(3) 0.0637(2) 0.0405(14) Uani 1 1 d . . .
H10 H -0.0380 0.0189 0.0487 0.049 Uiso 1 1 calc R . .
C11 C 0.0787(4) 0.0799(3) 0.0553(2) 0.0391(13) Uani 1 1 d . . .
H11 H 0.0408 0.1077 0.0344 0.047 Uiso 1 1 calc R . .
C12 C 0.1823(4) 0.0932(2) 0.07737(19) 0.0282(10) Uani 1 1 d . . .
H12 H 0.2142 0.1300 0.0717 0.034 Uiso 1 1 calc R . .
C13 C 0.4787(3) 0.03402(17) 0.10111(16) 0.0176(8) Uani 1 1 d . . .
C14 C 0.5827(3) 0.05911(18) 0.10047(17) 0.0202(8) Uani 1 1 d . . .
H14 H 0.5945 0.0948 0.1180 0.024 Uiso 1 1 calc R . .
C15 C 0.6698(4) 0.0321(2) 0.07419(18) 0.0250(9) Uani 1 1 d . . .
H15 H 0.7413 0.0489 0.0744 0.030 Uiso 1 1 calc R . .
C16 C 0.6520(4) -0.0192(2) 0.04781(19) 0.0284(10) Uani 1 1 d . . .
H16 H 0.7108 -0.0370 0.0290 0.034 Uiso 1 1 calc R . .
C17 C 0.5488(4) -0.0446(2) 0.0488(2) 0.0298(10) Uani 1 1 d . . .
H17 H 0.5374 -0.0802 0.0309 0.036 Uiso 1 1 calc R . .
C18 C 0.4622(4) -0.01869(19) 0.07551(19) 0.0243(9) Uani 1 1 d . . .
H18 H 0.3918 -0.0366 0.0765 0.029 Uiso 1 1 calc R . .
C19 C 0.3660(3) 0.03475(17) 0.20238(16) 0.0164(7) Uani 1 1 d . . .
C20 C 0.2772(3) 0.04619(18) 0.23632(17) 0.0201(8) Uani 1 1 d . . .
H20 H 0.2161 0.0677 0.2235 0.024 Uiso 1 1 calc R . .
C21 C 0.2776(4) 0.02629(19) 0.28875(18) 0.0227(9) Uani 1 1 d . . .
H21 H 0.2172 0.0344 0.3118 0.027 Uiso 1 1 calc R . .
C22 C 0.3664(4) -0.0054(2) 0.30720(18) 0.0253(9) Uani 1 1 d . . .
H22 H 0.3676 -0.0183 0.3433 0.030 Uiso 1 1 calc R . .
C23 C 0.4527(4) -0.0183(2) 0.27370(19) 0.0260(9) Uani 1 1 d . . .
H23 H 0.5125 -0.0408 0.2865 0.031 Uiso 1 1 calc R . .
C24 C 0.4533(4) 0.00143(18) 0.22095(18) 0.0210(8) Uani 1 1 d . . .
H24 H 0.5130 -0.0078 0.1979 0.025 Uiso 1 1 calc R . .
C25 C 0.3317(4) 0.29980(18) 0.09420(18) 0.0207(8) Uani 1 1 d . . .
C26 C 0.2213(4) 0.2831(2) 0.0978(2) 0.0290(10) Uani 1 1 d . . .
H26 H 0.1993 0.2555 0.1236 0.035 Uiso 1 1 calc R . .
C27 C 0.1433(4) 0.3073(2) 0.0633(2) 0.0332(11) Uani 1 1 d . . .
H27 H 0.0679 0.2964 0.0659 0.040 Uiso 1 1 calc R . .
C28 C 0.1761(5) 0.3472(2) 0.0252(2) 0.0331(11) Uani 1 1 d . . .
H28 H 0.1230 0.3643 0.0022 0.040 Uiso 1 1 calc R . .
C29 C 0.2855(5) 0.3619(2) 0.0207(2) 0.0360(12) Uani 1 1 d . . .
H29 H 0.3080 0.3880 -0.0063 0.043 Uiso 1 1 calc R . .
C30 C 0.3632(4) 0.3389(2) 0.0553(2) 0.0300(10) Uani 1 1 d . . .
H30 H 0.4384 0.3500 0.0523 0.036 Uiso 1 1 calc R . .
C31 C 0.5647(3) 0.29098(17) 0.11504(16) 0.0172(8) Uani 1 1 d . . .
C32 C 0.6277(4) 0.25604(19) 0.08143(19) 0.0235(9) Uani 1 1 d . . .
H32 H 0.6032 0.2183 0.0732 0.028 Uiso 1 1 calc R . .
C33 C 0.7258(4) 0.2764(2) 0.0601(2) 0.0296(10) Uani 1 1 d . . .
H33 H 0.7684 0.2525 0.0373 0.036 Uiso 1 1 calc R . .
C34 C 0.7621(4) 0.3315(2) 0.0720(2) 0.0306(10) Uani 1 1 d . . .
H34 H 0.8286 0.3456 0.0567 0.037 Uiso 1 1 calc R . .
C35 C 0.7013(4) 0.3656(2) 0.10596(19) 0.0272(10) Uani 1 1 d . . .
H35 H 0.7271 0.4030 0.1147 0.033 Uiso 1 1 calc R . .
C36 C 0.6031(4) 0.34620(18) 0.12761(18) 0.0218(8) Uani 1 1 d . . .
H36 H 0.5617 0.3702 0.1509 0.026 Uiso 1 1 calc R . .
C37 C 0.4177(3) 0.30674(17) 0.20210(16) 0.0184(8) Uani 1 1 d . . .
C38 C 0.3314(4) 0.34441(19) 0.2125(2) 0.0244(9) Uani 1 1 d . . .
H38 H 0.2760 0.3508 0.1863 0.029 Uiso 1 1 calc R . .
C39 C 0.3264(4) 0.3728(2) 0.2615(2) 0.0335(11) Uani 1 1 d . . .
H39 H 0.2668 0.3982 0.2688 0.040 Uiso 1 1 calc R . .
C40 C 0.4072(5) 0.3644(2) 0.2996(2) 0.0338(11) Uani 1 1 d . . .
H40 H 0.4040 0.3845 0.3326 0.041 Uiso 1 1 calc R . .
C41 C 0.4934(4) 0.3265(2) 0.28951(19) 0.0320(11) Uani 1 1 d . . .
H41 H 0.5488 0.3205 0.3159 0.038 Uiso 1 1 calc R . .
C42 C 0.4989(4) 0.29752(19) 0.24123(18) 0.0236(9) Uani 1 1 d . . .
H42 H 0.5575 0.2714 0.2346 0.028 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.003(4) . ?
Pd1 P2 2.3083(10) . ?
Pd1 P1 2.3215(10) . ?
Pd1 Cl1 2.3702(10) . ?
F1 C2 1.357(5) . ?
F2 C4 1.366(5) . ?
F3 C6 1.366(5) . ?
P1 C19 1.814(4) . ?
P1 C13 1.826(4) . ?
P1 C7 1.830(4) . ?
P2 C37 1.818(4) . ?
P2 C25 1.821(4) . ?
P2 C31 1.819(4) . ?
C1 C6 1.374(5) . ?
C1 C2 1.396(5) . ?
C2 C3 1.391(6) . ?
C3 C4 1.366(7) . ?
C4 C5 1.379(7) . ?
C5 C6 1.385(6) . ?
C7 C12 1.389(7) . ?
C7 C8 1.393(7) . ?
C8 C9 1.412(7) . ?
C9 C10 1.381(9) . ?
C10 C11 1.365(9) . ?
C11 C12 1.405(7) . ?
C13 C14 1.390(6) . ?
C13 C18 1.398(6) . ?
C14 C15 1.393(6) . ?
C15 C16 1.381(7) . ?
C16 C17 1.384(7) . ?
C17 C18 1.384(6) . ?
C19 C24 1.392(6) . ?
C19 C20 1.395(6) . ?
C20 C21 1.390(6) . ?
C21 C22 1.383(7) . ?
C22 C23 1.374(7) . ?
C23 C24 1.396(6) . ?
C25 C30 1.387(7) . ?
C25 C26 1.395(7) . ?
C26 C27 1.398(7) . ?
C27 C28 1.389(8) . ?
C28 C29 1.373(8) . ?
C29 C30 1.384(7) . ?
C31 C32 1.396(6) . ?
C31 C36 1.403(6) . ?
C32 C33 1.386(6) . ?
C33 C34 1.389(7) . ?
C34 C35 1.377(7) . ?
C35 C36 1.383(6) . ?
C37 C38 1.389(6) . ?
C37 C42 1.404(6) . ?
C38 C39 1.394(7) . ?
C39 C40 1.379(8) . ?
C40 C41 1.390(8) . ?
C41 C42 1.384(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 P2 90.23(11) . . ?
C1 Pd1 P1 91.12(11) . . ?
P2 Pd1 P1 177.96(4) . . ?
C1 Pd1 Cl1 179.66(12) . . ?
P2 Pd1 Cl1 89.67(4) . . ?
P1 Pd1 Cl1 88.99(4) . . ?
C19 P1 C13 104.40(18) . . ?
C19 P1 C7 103.6(2) . . ?
C13 P1 C7 107.90(19) . . ?
C19 P1 Pd1 116.44(13) . . ?
C13 P1 Pd1 110.56(14) . . ?
C7 P1 Pd1 113.20(15) . . ?
C37 P2 C25 105.44(19) . . ?
C37 P2 C31 102.47(19) . . ?
C25 P2 C31 104.6(2) . . ?
C37 P2 Pd1 118.91(14) . . ?
C25 P2 Pd1 108.51(14) . . ?
C31 P2 Pd1 115.64(14) . . ?
C6 C1 C2 113.5(4) . . ?
C6 C1 Pd1 122.8(3) . . ?
C2 C1 Pd1 123.7(3) . . ?
F1 C2 C3 117.1(4) . . ?
F1 C2 C1 118.1(4) . . ?
C3 C2 C1 124.8(4) . . ?
C4 C3 C2 116.4(4) . . ?
C3 C4 F2 118.4(4) . . ?
C3 C4 C5 123.5(4) . . ?
F2 C4 C5 118.1(4) . . ?
C4 C5 C6 116.0(4) . . ?
F3 C6 C1 117.7(4) . . ?
F3 C6 C5 116.4(4) . . ?
C1 C6 C5 125.9(4) . . ?
C12 C7 C8 119.8(4) . . ?
C12 C7 P1 119.2(4) . . ?
C8 C7 P1 121.0(4) . . ?
C7 C8 C9 120.0(5) . . ?
C10 C9 C8 119.1(5) . . ?
C11 C10 C9 121.0(5) . . ?
C10 C11 C12 120.5(6) . . ?
C7 C12 C11 119.5(5) . . ?
C14 C13 C18 119.6(4) . . ?
C14 C13 P1 117.5(3) . . ?
C18 C13 P1 122.9(3) . . ?
C13 C14 C15 120.2(4) . . ?
C16 C15 C14 119.8(4) . . ?
C17 C16 C15 120.3(4) . . ?
C16 C17 C18 120.4(4) . . ?
C17 C18 C13 119.7(4) . . ?
C24 C19 C20 119.3(4) . . ?
C24 C19 P1 122.3(3) . . ?
C20 C19 P1 118.0(3) . . ?
C21 C20 C19 120.5(4) . . ?
C22 C21 C20 119.6(4) . . ?
C23 C22 C21 120.4(4) . . ?
C22 C23 C24 120.5(4) . . ?
C19 C24 C23 119.6(4) . . ?
C30 C25 C26 119.5(4) . . ?
C30 C25 P2 121.9(4) . . ?
C26 C25 P2 118.6(4) . . ?
C25 C26 C27 119.8(5) . . ?
C28 C27 C26 119.9(5) . . ?
C29 C28 C27 119.9(5) . . ?
C28 C29 C30 120.7(5) . . ?
C29 C30 C25 120.2(5) . . ?
C32 C31 C36 119.2(4) . . ?
C32 C31 P2 120.9(3) . . ?
C36 C31 P2 119.8(3) . . ?
C33 C32 C31 120.0(4) . . ?
C32 C33 C34 120.4(4) . . ?
C35 C34 C33 119.7(4) . . ?
C34 C35 C36 120.9(4) . . ?
C35 C36 C31 119.8(4) . . ?
C38 C37 C42 119.6(4) . . ?
C38 C37 P2 123.2(3) . . ?
C42 C37 P2 117.3(3) . . ?
C37 C38 C39 119.8(5) . . ?
C40 C39 C38 120.5(5) . . ?
C39 C40 C41 120.0(4) . . ?
C42 C41 C40 120.2(5) . . ?
C41 C42 C37 120.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        0.50
_diffrn_measured_fraction_theta_full 0.000
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.137


_database_code_depnum_ccdc_archive 'CCDC 1005724'
