# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015


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#
#                 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
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# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_compound-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H37 N2, Cl'
_chemical_formula_sum            'C25 H37 Cl N2'

_chemical_formula_weight         401.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   11.682(7)
_cell_length_b                   17.097(10)
_cell_length_c                   12.553(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.143(11)
_cell_angle_gamma                90.00
_cell_volume                     2442(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1683
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.47

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12698
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1028
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4517
_reflns_number_gt                2986
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.1098P)²+0.8168P] 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         4517
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2263
_refine_ls_wR_factor_gt          0.1945
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
C1 C 0.2303(3) 0.21185(19) 0.2790(3) 0.0258(8) Uani 1 1 d . . .
H1 H 0.2602 0.2053 0.2152 0.031 Uiso 1 1 calc R . .
C2 C 0.3573(3) 0.1064(2) 0.3519(3) 0.0277(8) Uani 1 1 d . . .
C3 C 0.3281(3) 0.0298(2) 0.3167(3) 0.0280(8) Uani 1 1 d . . .
C4 C 0.4211(3) -0.0211(2) 0.3160(3) 0.0374(9) Uani 1 1 d . . .
H4 H 0.4045 -0.0735 0.2926 0.045 Uiso 1 1 calc R . .
C5 C 0.5360(4) 0.0025(3) 0.3480(3) 0.0428(10) Uani 1 1 d . . .
H5 H 0.5976 -0.0336 0.3477 0.051 Uiso 1 1 calc R . .
C6 C 0.5621(3) 0.0789(2) 0.3807(3) 0.0377(9) Uani 1 1 d . . .
H6 H 0.6420 0.0949 0.4008 0.045 Uiso 1 1 calc R . .
C7 C 0.4737(3) 0.1331(2) 0.3849(3) 0.0312(8) Uani 1 1 d . . .
C8 C 0.2011(3) 0.0025(2) 0.2852(3) 0.0330(9) Uani 1 1 d . . .
H8 H 0.1522 0.0477 0.2505 0.040 Uiso 1 1 calc R . .
C9 C 0.1584(4) -0.0207(3) 0.3865(3) 0.0441(10) Uani 1 1 d . . .
H9A H 0.2031 -0.0661 0.4211 0.066 Uiso 1 1 calc R . .
H9B H 0.0747 -0.0341 0.3655 0.066 Uiso 1 1 calc R . .
H9C H 0.1698 0.0231 0.4382 0.066 Uiso 1 1 calc R . .
C10 C 0.1802(4) -0.0648(2) 0.2036(3) 0.0473(11) Uani 1 1 d . . .
H10A H 0.2172 -0.1124 0.2392 0.071 Uiso 1 1 calc R . .
H10B H 0.2144 -0.0519 0.1414 0.071 Uiso 1 1 calc R . .
H10C H 0.0955 -0.0735 0.1776 0.071 Uiso 1 1 calc R . .
C11 C 0.5026(3) 0.2172(2) 0.4220(3) 0.0368(9) Uani 1 1 d . . .
H11 H 0.4307 0.2399 0.4407 0.044 Uiso 1 1 calc R . .
C12 C 0.6021(4) 0.2229(3) 0.5239(4) 0.0577(13) Uani 1 1 d . . .
H12A H 0.6757 0.2058 0.5063 0.087 Uiso 1 1 calc R . .
H12B H 0.5845 0.1893 0.5814 0.087 Uiso 1 1 calc R . .
H12C H 0.6101 0.2771 0.5496 0.087 Uiso 1 1 calc R . .
C13 C 0.5301(4) 0.2664(3) 0.3296(4) 0.0557(12) Uani 1 1 d . . .
H13A H 0.5952 0.2424 0.3040 0.084 Uiso 1 1 calc R . .
H13B H 0.5524 0.3193 0.3564 0.084 Uiso 1 1 calc R . .
H13C H 0.4605 0.2690 0.2691 0.084 Uiso 1 1 calc R . .
C14 C 0.1123(3) 0.29737(19) 0.3705(3) 0.0233(7) Uani 1 1 d . . .
C15 C 0.1668(3) 0.3620(2) 0.4297(3) 0.0262(8) Uani 1 1 d . . .
C16 C 0.1168(3) 0.3902(2) 0.5118(3) 0.0335(9) Uani 1 1 d . . .
H16 H 0.1500 0.4348 0.5524 0.040 Uiso 1 1 calc R . .
C17 C 0.0192(3) 0.3547(2) 0.5361(3) 0.0320(9) Uani 1 1 d . . .
H17 H -0.0138 0.3751 0.5929 0.038 Uiso 1 1 calc R . .
C18 C -0.0300(3) 0.2901(2) 0.4782(3) 0.0307(8) Uani 1 1 d . . .
H18 H -0.0964 0.2659 0.4962 0.037 Uiso 1 1 calc R . .
C19 C 0.0154(3) 0.25911(19) 0.3936(3) 0.0233(7) Uani 1 1 d . . .
C20 C 0.2744(3) 0.4023(2) 0.4059(3) 0.0339(9) Uani 1 1 d . . .
H20 H 0.3031 0.3697 0.3512 0.041 Uiso 1 1 calc R . .
C21 C 0.3737(3) 0.4077(3) 0.5082(4) 0.0482(11) Uani 1 1 d . . .
H21A H 0.3515 0.4443 0.5602 0.072 Uiso 1 1 calc R . .
H21B H 0.4453 0.4263 0.4882 0.072 Uiso 1 1 calc R . .
H21C H 0.3880 0.3559 0.5421 0.072 Uiso 1 1 calc R . .
C22 C 0.2421(4) 0.4833(3) 0.3546(4) 0.0577(13) Uani 1 1 d . . .
H22A H 0.1818 0.4775 0.2866 0.087 Uiso 1 1 calc R . .
H22B H 0.3122 0.5077 0.3386 0.087 Uiso 1 1 calc R . .
H22C H 0.2118 0.5162 0.4058 0.087 Uiso 1 1 calc R . .
C23 C -0.0409(3) 0.1885(2) 0.3292(3) 0.0285(8) Uani 1 1 d . . .
H23 H 0.0193 0.1636 0.2948 0.034 Uiso 1 1 calc R . .
C24 C -0.1432(3) 0.2149(2) 0.2373(3) 0.0355(9) Uani 1 1 d . . .
H24A H -0.2030 0.2404 0.2688 0.053 Uiso 1 1 calc R . .
H24B H -0.1777 0.1694 0.1944 0.053 Uiso 1 1 calc R . .
H24C H -0.1145 0.2519 0.1897 0.053 Uiso 1 1 calc R . .
C25 C -0.0823(3) 0.1270(2) 0.4006(3) 0.0405(10) Uani 1 1 d . . .
H25A H -0.0176 0.1140 0.4627 0.061 Uiso 1 1 calc R . .
H25B H -0.1072 0.0798 0.3571 0.061 Uiso 1 1 calc R . .
H25C H -0.1485 0.1478 0.4276 0.061 Uiso 1 1 calc R . .
Cl1 Cl 0.23071(9) 0.14970(6) 0.59110(7) 0.0422(3) Uani 1 1 d . . .
N1 N 0.2641(2) 0.16175(16) 0.3570(2) 0.0260(7) Uani 1 1 d . . .
H1A H 0.2307 0.1611 0.4131 0.031 Uiso 1 1 calc R . .
N2 N 0.1585(2) 0.27095(15) 0.2798(2) 0.0242(6) Uani 1 1 d . . .
H2 H 0.1364 0.2972 0.2182 0.029 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
C1 N1 1.293(4) . ?
C1 N2 1.314(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.400(5) . ?
C2 C7 1.404(5) . ?
C2 N1 1.455(4) . ?
C3 C4 1.394(5) . ?
C3 C8 1.519(5) . ?
C4 C5 1.371(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(5) . ?
C6 H6 0.9500 . ?
C7 C11 1.527(5) . ?
C8 C9 1.520(5) . ?
C8 C10 1.524(5) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(5) . ?
C11 C13 1.525(6) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.394(4) . ?
C14 C15 1.402(5) . ?
C14 N2 1.439(4) . ?
C15 C16 1.382(5) . ?
C15 C20 1.521(5) . ?
C16 C17 1.385(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(5) . ?
C18 H18 0.9500 . ?
C19 C23 1.517(5) . ?
C20 C21 1.525(5) . ?
C20 C22 1.537(6) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.529(5) . ?
C23 C25 1.529(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
N1 H1A 0.8800 . ?
N2 H2 0.8800 . ?

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
N1 C1 N2 126.1(3) . . ?
N1 C1 H1 117.0 . . ?
N2 C1 H1 117.0 . . ?
C3 C2 C7 123.2(3) . . ?
C3 C2 N1 119.4(3) . . ?
C7 C2 N1 117.4(3) . . ?
C4 C3 C2 116.8(3) . . ?
C4 C3 C8 121.6(3) . . ?
C2 C3 C8 121.5(3) . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 121.5(4) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C2 116.7(3) . . ?
C6 C7 C11 121.5(3) . . ?
C2 C7 C11 121.9(3) . . ?
C3 C8 C9 110.4(3) . . ?
C3 C8 C10 113.9(3) . . ?
C9 C8 C10 109.4(3) . . ?
C3 C8 H8 107.6 . . ?
C9 C8 H8 107.6 . . ?
C10 C8 H8 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C13 110.5(3) . . ?
C12 C11 C7 112.9(3) . . ?
C13 C11 C7 111.0(3) . . ?
C12 C11 H11 107.4 . . ?
C13 C11 H11 107.4 . . ?
C7 C11 H11 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 123.5(3) . . ?
C19 C14 N2 119.1(3) . . ?
C15 C14 N2 117.4(3) . . ?
C16 C15 C14 116.9(3) . . ?
C16 C15 C20 119.8(3) . . ?
C14 C15 C20 123.3(3) . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 121.5(3) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C14 C19 C18 116.6(3) . . ?
C14 C19 C23 122.4(3) . . ?
C18 C19 C23 121.0(3) . . ?
C15 C20 C21 111.5(3) . . ?
C15 C20 C22 110.8(3) . . ?
C21 C20 C22 111.5(3) . . ?
C15 C20 H20 107.6 . . ?
C21 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C24 109.6(3) . . ?
C19 C23 C25 113.0(3) . . ?
C24 C23 C25 110.4(3) . . ?
C19 C23 H23 107.9 . . ?
C24 C23 H23 107.9 . . ?
C25 C23 H23 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 N1 C2 120.0(3) . . ?
C1 N1 H1A 120.0 . . ?
C2 N1 H1A 120.0 . . ?
C1 N2 C14 127.0(3) . . ?
C1 N2 H2 116.5 . . ?
C14 N2 H2 116.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 0.4(5) . . . . ?
N1 C2 C3 C4 -178.6(3) . . . . ?
C7 C2 C3 C8 178.0(3) . . . . ?
N1 C2 C3 C8 -1.0(5) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C8 C3 C4 C5 -177.7(4) . . . . ?
C3 C4 C5 C6 -1.0(6) . . . . ?
C4 C5 C6 C7 1.7(6) . . . . ?
C5 C6 C7 C2 -1.3(5) . . . . ?
C5 C6 C7 C11 179.4(4) . . . . ?
C3 C2 C7 C6 0.3(5) . . . . ?
N1 C2 C7 C6 179.3(3) . . . . ?
C3 C2 C7 C11 179.5(3) . . . . ?
N1 C2 C7 C11 -1.5(5) . . . . ?
C4 C3 C8 C9 94.7(4) . . . . ?
C2 C3 C8 C9 -82.8(4) . . . . ?
C4 C3 C8 C10 -28.9(5) . . . . ?
C2 C3 C8 C10 153.6(3) . . . . ?
C6 C7 C11 C12 -44.6(5) . . . . ?
C2 C7 C11 C12 136.3(4) . . . . ?
C6 C7 C11 C13 80.2(4) . . . . ?
C2 C7 C11 C13 -99.0(4) . . . . ?
C19 C14 C15 C16 -2.9(5) . . . . ?
N2 C14 C15 C16 175.7(3) . . . . ?
C19 C14 C15 C20 178.5(3) . . . . ?
N2 C14 C15 C20 -2.9(5) . . . . ?
C14 C15 C16 C17 1.7(5) . . . . ?
C20 C15 C16 C17 -179.6(3) . . . . ?
C15 C16 C17 C18 0.0(6) . . . . ?
C16 C17 C18 C19 -0.7(5) . . . . ?
C15 C14 C19 C18 2.3(5) . . . . ?
N2 C14 C19 C18 -176.3(3) . . . . ?
C15 C14 C19 C23 -179.1(3) . . . . ?
N2 C14 C19 C23 2.3(4) . . . . ?
C17 C18 C19 C14 -0.4(5) . . . . ?
C17 C18 C19 C23 -179.1(3) . . . . ?
C16 C15 C20 C21 55.2(5) . . . . ?
C14 C15 C20 C21 -126.2(4) . . . . ?
C16 C15 C20 C22 -69.6(5) . . . . ?
C14 C15 C20 C22 108.9(4) . . . . ?
C14 C19 C23 C24 -94.1(4) . . . . ?
C18 C19 C23 C24 84.5(4) . . . . ?
C14 C19 C23 C25 142.3(3) . . . . ?
C18 C19 C23 C25 -39.1(4) . . . . ?
N2 C1 N1 C2 -170.8(3) . . . . ?
C3 C2 N1 C1 -99.5(4) . . . . ?
C7 C2 N1 C1 81.5(4) . . . . ?
N1 C1 N2 C14 7.0(5) . . . . ?
C19 C14 N2 C1 -81.6(4) . . . . ?
C15 C14 N2 C1 99.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.074
_database_code_depnum_ccdc_archive 'CCDC 1014314'
#######################################################################
#
#                 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_Compound-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H39 Cl2 N3 Pd'
_chemical_formula_sum            'C27 H39 Cl2 N3 Pd'
_chemical_formula_weight         582.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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'

_cell_length_a                   10.4915(7)
_cell_length_b                   12.1600(8)
_cell_length_c                   13.8790(9)
_cell_angle_alpha                68.8130(10)
_cell_angle_beta                 68.1580(10)
_cell_angle_gamma                75.069(2)
_cell_volume                     1516.83(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    5405
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.22

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10658
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5622
_reflns_number_gt                4707
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.0469P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5622
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0845
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 1.000 222 49 ' '
_platon_squeeze_details          
;
;


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
C1 C 0.8518(3) 0.4715(3) 0.2724(2) 0.0118(6) Uani 1 1 d . . .
H1 H 0.9145 0.4452 0.2145 0.014 Uiso 1 1 calc R . .
C2 C 0.8968(3) 0.2721(3) 0.3642(2) 0.0124(6) Uani 1 1 d . . .
C3 C 0.8216(3) 0.1906(3) 0.3673(2) 0.0124(6) Uani 1 1 d . . .
C4 C 0.8895(3) 0.0759(3) 0.3693(2) 0.0154(6) Uani 1 1 d . . .
H4 H 0.8421 0.0199 0.3711 0.018 Uiso 1 1 calc R . .
C5 C 1.0258(3) 0.0434(3) 0.3685(2) 0.0181(7) Uani 1 1 d . . .
H5 H 1.0695 -0.0339 0.3702 0.022 Uiso 1 1 calc R . .
C6 C 1.0970(3) 0.1260(3) 0.3652(2) 0.0177(7) Uani 1 1 d . . .
H6 H 1.1892 0.1036 0.3639 0.021 Uiso 1 1 calc R . .
C7 C 1.0347(3) 0.2423(3) 0.3636(2) 0.0145(6) Uani 1 1 d . . .
C8 C 0.6730(3) 0.2240(3) 0.3662(3) 0.0186(7) Uani 1 1 d . . .
H8 H 0.6382 0.3017 0.3799 0.022 Uiso 1 1 calc R . .
C9 C 0.5793(4) 0.1365(3) 0.4537(3) 0.0311(8) Uani 1 1 d . . .
H9A H 0.6047 0.0617 0.4381 0.047 Uiso 1 1 calc R . .
H9B H 0.4847 0.1672 0.4558 0.047 Uiso 1 1 calc R . .
H9C H 0.5892 0.1251 0.5229 0.047 Uiso 1 1 calc R . .
C10 C 0.6659(4) 0.2381(4) 0.2548(3) 0.0374(10) Uani 1 1 d . . .
H10A H 0.7280 0.2920 0.2001 0.056 Uiso 1 1 calc R . .
H10B H 0.5729 0.2694 0.2524 0.056 Uiso 1 1 calc R . .
H10C H 0.6923 0.1620 0.2416 0.056 Uiso 1 1 calc R . .
C11 C 1.1144(3) 0.3290(3) 0.3655(3) 0.0223(7) Uani 1 1 d . . .
H11 H 1.0714 0.4098 0.3351 0.027 Uiso 1 1 calc R . .
C12 C 1.2659(3) 0.3168(3) 0.2979(3) 0.0271(8) Uani 1 1 d . . .
H12A H 1.3134 0.2421 0.3312 0.041 Uiso 1 1 calc R . .
H12B H 1.3073 0.3809 0.2937 0.041 Uiso 1 1 calc R . .
H12C H 1.2730 0.3198 0.2261 0.041 Uiso 1 1 calc R . .
C13 C 1.1025(4) 0.3154(4) 0.4824(3) 0.0444(11) Uani 1 1 d . . .
H13A H 1.0064 0.3221 0.5250 0.067 Uiso 1 1 calc R . .
H13B H 1.1441 0.3768 0.4828 0.067 Uiso 1 1 calc R . .
H13C H 1.1494 0.2388 0.5126 0.067 Uiso 1 1 calc R . .
C14 C 0.8586(3) 0.6614(3) 0.1353(2) 0.0141(6) Uani 1 1 d . . .
C15 C 0.8116(3) 0.6578(3) 0.0542(2) 0.0149(6) Uani 1 1 d . . .
C16 C 0.8674(3) 0.7303(3) -0.0503(2) 0.0203(7) Uani 1 1 d . . .
H16 H 0.8385 0.7306 -0.1062 0.024 Uiso 1 1 calc R . .
C17 C 0.9640(3) 0.8016(3) -0.0733(3) 0.0230(7) Uani 1 1 d . . .
H17 H 0.9989 0.8500 -0.1438 0.028 Uiso 1 1 calc R . .
C18 C 1.0089(3) 0.8012(3) 0.0083(2) 0.0209(7) Uani 1 1 d . . .
H18 H 1.0756 0.8485 -0.0083 0.025 Uiso 1 1 calc R . .
C19 C 0.9571(3) 0.7317(3) 0.1148(2) 0.0152(6) Uani 1 1 d . . .
C20 C 0.7048(3) 0.5806(3) 0.0765(2) 0.0183(7) Uani 1 1 d . . .
H20 H 0.6797 0.5351 0.1537 0.022 Uiso 1 1 calc R . .
C21 C 0.7681(4) 0.4919(3) 0.0095(3) 0.0279(8) Uani 1 1 d . . .
H21A H 0.7930 0.5350 -0.0665 0.042 Uiso 1 1 calc R . .
H21B H 0.7015 0.4413 0.0260 0.042 Uiso 1 1 calc R . .
H21C H 0.8494 0.4443 0.0272 0.042 Uiso 1 1 calc R . .
C22 C 0.5733(3) 0.6555(3) 0.0518(3) 0.0274(8) Uani 1 1 d . . .
H22A H 0.5365 0.7119 0.0926 0.041 Uiso 1 1 calc R . .
H22B H 0.5058 0.6044 0.0717 0.041 Uiso 1 1 calc R . .
H22C H 0.5949 0.6973 -0.0244 0.041 Uiso 1 1 calc R . .
C23 C 1.0118(3) 0.7328(3) 0.2018(3) 0.0195(7) Uani 1 1 d . . .
H23 H 0.9568 0.6857 0.2722 0.023 Uiso 1 1 calc R . .
C24 C 1.1630(3) 0.6758(3) 0.1835(3) 0.0253(8) Uani 1 1 d . . .
H24A H 1.1716 0.5951 0.1840 0.038 Uiso 1 1 calc R . .
H24B H 1.1937 0.6764 0.2404 0.038 Uiso 1 1 calc R . .
H24C H 1.2190 0.7200 0.1146 0.038 Uiso 1 1 calc R . .
C25 C 0.9957(4) 0.8595(3) 0.2077(3) 0.0308(8) Uani 1 1 d . . .
H25A H 1.0508 0.9069 0.1403 0.046 Uiso 1 1 calc R . .
H25B H 1.0262 0.8564 0.2659 0.046 Uiso 1 1 calc R . .
H25C H 0.9000 0.8944 0.2206 0.046 Uiso 1 1 calc R . .
C26 C 0.6983(3) 0.6469(3) 0.3193(2) 0.0128(6) Uani 1 1 d . . .
C27 C 0.6343(3) 0.7696(3) 0.2729(2) 0.0192(7) Uani 1 1 d . . .
H27A H 0.5624 0.7968 0.3300 0.029 Uiso 1 1 calc R . .
H27B H 0.5954 0.7697 0.2203 0.029 Uiso 1 1 calc R . .
H27C H 0.7038 0.8218 0.2384 0.029 Uiso 1 1 calc R . .
Cl1 Cl 0.56288(8) 0.48175(7) 0.65770(6) 0.01710(17) Uani 1 1 d . . .
Cl2 Cl 0.73620(8) 0.23397(7) 0.61162(6) 0.02016(18) Uani 1 1 d . . .
N1 N 0.8257(2) 0.3915(2) 0.36542(18) 0.0091(5) Uani 1 1 d . . .
N2 N 0.7995(2) 0.5901(2) 0.24715(19) 0.0117(5) Uani 1 1 d . . .
N3 N 0.6615(2) 0.5933(2) 0.42083(19) 0.0137(5) Uani 1 1 d . . .
H3 H 0.6081 0.6385 0.4598 0.016 Uiso 1 1 calc R . .
Pd1 Pd 0.70323(2) 0.426698(19) 0.506036(18) 0.01120(8) Uani 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
C1 N1 1.286(4) . ?
C1 N2 1.369(4) . ?
C1 H1 0.9300 . ?
C2 C7 1.395(4) . ?
C2 C3 1.398(4) . ?
C2 N1 1.454(3) . ?
C3 C4 1.388(4) . ?
C3 C8 1.511(4) . ?
C4 C5 1.379(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(4) . ?
C6 H6 0.9300 . ?
C7 C11 1.517(4) . ?
C8 C9 1.513(4) . ?
C8 C10 1.521(4) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.516(4) . ?
C11 C13 1.530(5) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C19 1.392(4) . ?
C14 C15 1.405(4) . ?
C14 N2 1.461(4) . ?
C15 C16 1.391(4) . ?
C15 C20 1.518(4) . ?
C16 C17 1.376(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9300 . ?
C19 C23 1.524(4) . ?
C20 C22 1.526(4) . ?
C20 C21 1.538(4) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.525(4) . ?
C23 C25 1.534(4) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N3 1.273(4) . ?
C26 N2 1.392(4) . ?
C26 C27 1.484(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Cl1 Pd1 2.2916(7) . ?
Cl2 Pd1 2.2883(8) . ?
N1 Pd1 2.024(2) . ?
N3 Pd1 1.972(2) . ?
N3 H3 0.8600 . ?

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
N1 C1 N2 128.7(3) . . ?
N1 C1 H1 115.6 . . ?
N2 C1 H1 115.6 . . ?
C7 C2 C3 122.8(3) . . ?
C7 C2 N1 119.2(3) . . ?
C3 C2 N1 118.0(2) . . ?
C4 C3 C2 117.5(3) . . ?
C4 C3 C8 120.1(3) . . ?
C2 C3 C8 122.4(3) . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 116.9(3) . . ?
C6 C7 C11 120.2(3) . . ?
C2 C7 C11 122.8(3) . . ?
C3 C8 C9 112.9(3) . . ?
C3 C8 C10 110.4(3) . . ?
C9 C8 C10 110.6(3) . . ?
C3 C8 H8 107.6 . . ?
C9 C8 H8 107.6 . . ?
C10 C8 H8 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 113.4(3) . . ?
C12 C11 C13 109.8(3) . . ?
C7 C11 C13 110.5(3) . . ?
C12 C11 H11 107.6 . . ?
C7 C11 H11 107.6 . . ?
C13 C11 H11 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 123.2(3) . . ?
C19 C14 N2 118.2(2) . . ?
C15 C14 N2 118.6(3) . . ?
C16 C15 C14 116.5(3) . . ?
C16 C15 C20 120.3(3) . . ?
C14 C15 C20 123.2(3) . . ?
C17 C16 C15 121.8(3) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 121.6(3) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C14 117.1(3) . . ?
C18 C19 C23 119.6(3) . . ?
C14 C19 C23 123.3(3) . . ?
C15 C20 C22 111.7(3) . . ?
C15 C20 C21 109.7(3) . . ?
C22 C20 C21 110.5(3) . . ?
C15 C20 H20 108.3 . . ?
C22 C20 H20 108.3 . . ?
C21 C20 H20 108.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C24 111.5(2) . . ?
C19 C23 C25 111.7(3) . . ?
C24 C23 C25 109.8(3) . . ?
C19 C23 H23 107.9 . . ?
C24 C23 H23 107.9 . . ?
C25 C23 H23 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 120.3(3) . . ?
N3 C26 C27 122.1(3) . . ?
N2 C26 C27 117.5(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 N1 C2 115.0(2) . . ?
C1 N1 Pd1 123.7(2) . . ?
C2 N1 Pd1 121.23(17) . . ?
C1 N2 C26 125.4(2) . . ?
C1 N2 C14 116.1(2) . . ?
C26 N2 C14 118.5(2) . . ?
C26 N3 Pd1 132.5(2) . . ?
C26 N3 H3 113.8 . . ?
Pd1 N3 H3 113.8 . . ?
N3 Pd1 N1 88.51(9) . . ?
N3 Pd1 Cl2 176.15(7) . . ?
N1 Pd1 Cl2 94.34(7) . . ?
N3 Pd1 Cl1 87.12(7) . . ?
N1 Pd1 Cl1 175.59(7) . . ?
Cl2 Pd1 Cl1 90.05(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 -0.3(4) . . . . ?
N1 C2 C3 C4 -178.2(2) . . . . ?
C7 C2 C3 C8 -179.1(3) . . . . ?
N1 C2 C3 C8 3.1(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C8 C3 C4 C5 178.9(3) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C4 C5 C6 C7 0.7(4) . . . . ?
C5 C6 C7 C2 -0.8(4) . . . . ?
C5 C6 C7 C11 177.1(3) . . . . ?
C3 C2 C7 C6 0.6(4) . . . . ?
N1 C2 C7 C6 178.5(2) . . . . ?
C3 C2 C7 C11 -177.2(3) . . . . ?
N1 C2 C7 C11 0.7(4) . . . . ?
C4 C3 C8 C9 50.1(4) . . . . ?
C2 C3 C8 C9 -131.2(3) . . . . ?
C4 C3 C8 C10 -74.3(4) . . . . ?
C2 C3 C8 C10 104.4(3) . . . . ?
C6 C7 C11 C12 38.5(4) . . . . ?
C2 C7 C11 C12 -143.7(3) . . . . ?
C6 C7 C11 C13 -85.2(4) . . . . ?
C2 C7 C11 C13 92.5(4) . . . . ?
C19 C14 C15 C16 -0.8(4) . . . . ?
N2 C14 C15 C16 177.8(3) . . . . ?
C19 C14 C15 C20 179.7(3) . . . . ?
N2 C14 C15 C20 -1.7(4) . . . . ?
C14 C15 C16 C17 0.2(4) . . . . ?
C20 C15 C16 C17 179.8(3) . . . . ?
C15 C16 C17 C18 0.7(5) . . . . ?
C16 C17 C18 C19 -1.2(5) . . . . ?
C17 C18 C19 C14 0.7(4) . . . . ?
C17 C18 C19 C23 179.0(3) . . . . ?
C15 C14 C19 C18 0.4(4) . . . . ?
N2 C14 C19 C18 -178.3(3) . . . . ?
C15 C14 C19 C23 -177.9(3) . . . . ?
N2 C14 C19 C23 3.4(4) . . . . ?
C16 C15 C20 C22 -62.1(4) . . . . ?
C14 C15 C20 C22 117.4(3) . . . . ?
C16 C15 C20 C21 60.8(4) . . . . ?
C14 C15 C20 C21 -119.7(3) . . . . ?
C18 C19 C23 C24 -67.6(4) . . . . ?
C14 C19 C23 C24 110.7(3) . . . . ?
C18 C19 C23 C25 55.8(4) . . . . ?
C14 C19 C23 C25 -126.0(3) . . . . ?
N2 C1 N1 C2 178.7(3) . . . . ?
N2 C1 N1 Pd1 -4.2(4) . . . . ?
C7 C2 N1 C1 80.7(3) . . . . ?
C3 C2 N1 C1 -101.4(3) . . . . ?
C7 C2 N1 Pd1 -96.5(3) . . . . ?
C3 C2 N1 Pd1 81.4(3) . . . . ?
N1 C1 N2 C26 -4.1(5) . . . . ?
N1 C1 N2 C14 174.5(3) . . . . ?
N3 C26 N2 C1 10.8(4) . . . . ?
C27 C26 N2 C1 -167.9(3) . . . . ?
N3 C26 N2 C14 -167.8(3) . . . . ?
C27 C26 N2 C14 13.5(4) . . . . ?
C19 C14 N2 C1 -101.5(3) . . . . ?
C15 C14 N2 C1 79.8(3) . . . . ?
C19 C14 N2 C26 77.2(3) . . . . ?
C15 C14 N2 C26 -101.4(3) . . . . ?
N2 C26 N3 Pd1 -8.9(4) . . . . ?
C27 C26 N3 Pd1 169.7(2) . . . . ?
C26 N3 Pd1 N1 1.8(3) . . . . ?
C26 N3 Pd1 Cl2 -136.0(9) . . . . ?
C26 N3 Pd1 Cl1 -178.8(3) . . . . ?
C1 N1 Pd1 N3 4.7(2) . . . . ?
C2 N1 Pd1 N3 -178.4(2) . . . . ?
C1 N1 Pd1 Cl2 -177.9(2) . . . . ?
C2 N1 Pd1 Cl2 -1.0(2) . . . . ?
C1 N1 Pd1 Cl1 -2.9(10) . . . . ?
C2 N1 Pd1 Cl1 174.0(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.091
_database_code_depnum_ccdc_archive 'CCDC 1014315'
#######################################################################
#
#                 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_Compound-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H41 Cl2 N3 Pd, C H Cl3'
_chemical_formula_sum            'C29 H42 Cl5 N3 Pd'
_chemical_formula_weight         716.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '
_symmetry_space_group_name_HALL  '-P 2ac 2ab'

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                   12.857(5)
_cell_length_b                   21.354(5)
_cell_length_c                   23.497(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6451(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5725
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.30

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_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            34159
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6304
_reflns_number_gt                5375
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.0694P)²+2.4255P] 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         6304
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.169
_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
C1 C 0.6290(2) 0.12895(13) 0.93258(12) 0.0160(6) Uani 1 1 d . . .
H1 H 0.6233 0.0862 0.9395 0.019 Uiso 1 1 calc R . .
C2 C 0.5231(2) 0.13271(12) 1.01184(12) 0.0150(6) Uani 1 1 d . . .
C3 C 0.5767(2) 0.12625(14) 1.06346(13) 0.0171(6) Uani 1 1 d . . .
C4 C 0.5256(2) 0.09562(14) 1.10762(12) 0.0201(6) Uani 1 1 d . . .
H4 H 0.5593 0.0904 1.1423 0.024 Uiso 1 1 calc R . .
C5 C 0.4256(2) 0.07276(14) 1.10090(13) 0.0196(6) Uani 1 1 d . . .
H5 H 0.3931 0.0520 1.1308 0.024 Uiso 1 1 calc R . .
C6 C 0.3739(2) 0.08077(14) 1.04979(13) 0.0209(7) Uani 1 1 d . . .
H6 H 0.3060 0.0663 1.0460 0.025 Uiso 1 1 calc R . .
C7 C 0.4223(2) 0.11041(13) 1.00353(13) 0.0161(6) Uani 1 1 d . . .
C8 C 0.6843(2) 0.15458(15) 1.07281(13) 0.0213(6) Uani 1 1 d . . .
H8 H 0.7177 0.1592 1.0356 0.026 Uiso 1 1 calc R . .
C9 C 0.7550(2) 0.11445(15) 1.11012(13) 0.0242(7) Uani 1 1 d . . .
H9A H 0.7297 0.1149 1.1486 0.036 Uiso 1 1 calc R . .
H9B H 0.8244 0.1310 1.1091 0.036 Uiso 1 1 calc R . .
H9C H 0.7553 0.0722 1.0961 0.036 Uiso 1 1 calc R . .
C10 C 0.6727(3) 0.22006(15) 1.09894(15) 0.0295(7) Uani 1 1 d . . .
H10A H 0.6306 0.2456 1.0745 0.044 Uiso 1 1 calc R . .
H10B H 0.7402 0.2388 1.1031 0.044 Uiso 1 1 calc R . .
H10C H 0.6401 0.2167 1.1356 0.044 Uiso 1 1 calc R . .
C11 C 0.3674(2) 0.11675(14) 0.94657(13) 0.0200(6) Uani 1 1 d . . .
H11 H 0.4003 0.1510 0.9255 0.024 Uiso 1 1 calc R . .
C12 C 0.2522(2) 0.13113(16) 0.95220(14) 0.0249(7) Uani 1 1 d . . .
H12A H 0.2174 0.0961 0.9693 0.037 Uiso 1 1 calc R . .
H12B H 0.2234 0.1389 0.9152 0.037 Uiso 1 1 calc R . .
H12C H 0.2431 0.1675 0.9757 0.037 Uiso 1 1 calc R . .
C13 C 0.3815(3) 0.05630(16) 0.91229(14) 0.0289(7) Uani 1 1 d . . .
H13A H 0.4542 0.0496 0.9050 0.043 Uiso 1 1 calc R . .
H13B H 0.3450 0.0598 0.8768 0.043 Uiso 1 1 calc R . .
H13C H 0.3542 0.0216 0.9336 0.043 Uiso 1 1 calc R . .
C14 C 0.7344(2) 0.09424(13) 0.85453(12) 0.0154(6) Uani 1 1 d . . .
C15 C 0.6875(2) 0.08221(13) 0.80194(12) 0.0175(6) Uani 1 1 d . . .
C16 C 0.7204(2) 0.02937(14) 0.77256(12) 0.0205(6) Uani 1 1 d . . .
H16 H 0.6917 0.0206 0.7371 0.025 Uiso 1 1 calc R . .
C17 C 0.7948(3) -0.01049(14) 0.79487(13) 0.0234(7) Uani 1 1 d . . .
H17 H 0.8131 -0.0468 0.7754 0.028 Uiso 1 1 calc R . .
C18 C 0.8423(2) 0.00391(14) 0.84646(13) 0.0212(6) Uani 1 1 d . . .
H18 H 0.8934 -0.0225 0.8608 0.025 Uiso 1 1 calc R . .
C19 C 0.8144(2) 0.05733(13) 0.87708(12) 0.0163(6) Uani 1 1 d . . .
C20 C 0.6049(3) 0.12506(15) 0.77542(13) 0.0250(7) Uani 1 1 d . . .
H20 H 0.5910 0.1596 0.8018 0.030 Uiso 1 1 calc R . .
C21 C 0.5030(3) 0.08911(19) 0.76540(16) 0.0377(9) Uani 1 1 d . . .
H21A H 0.5146 0.0564 0.7381 0.057 Uiso 1 1 calc R . .
H21B H 0.4510 0.1173 0.7512 0.057 Uiso 1 1 calc R . .
H21C H 0.4797 0.0711 0.8006 0.057 Uiso 1 1 calc R . .
C22 C 0.6442(3) 0.15261(17) 0.71915(15) 0.0337(8) Uani 1 1 d . . .
H22A H 0.7069 0.1759 0.7259 0.051 Uiso 1 1 calc R . .
H22B H 0.5922 0.1799 0.7035 0.051 Uiso 1 1 calc R . .
H22C H 0.6581 0.1193 0.6928 0.051 Uiso 1 1 calc R . .
C23 C 0.8738(2) 0.07538(13) 0.93057(12) 0.0174(6) Uani 1 1 d . . .
H23 H 0.8507 0.1173 0.9420 0.021 Uiso 1 1 calc R . .
C24 C 0.9912(2) 0.07846(15) 0.91910(13) 0.0239(7) Uani 1 1 d . . .
H24A H 1.0171 0.0371 0.9117 0.036 Uiso 1 1 calc R . .
H24B H 1.0259 0.0955 0.9518 0.036 Uiso 1 1 calc R . .
H24C H 1.0040 0.1047 0.8867 0.036 Uiso 1 1 calc R . .
C25 C 0.8525(2) 0.03053(14) 0.98016(13) 0.0232(7) Uani 1 1 d . . .
H25A H 0.7794 0.0302 0.9884 0.035 Uiso 1 1 calc R . .
H25B H 0.8901 0.0443 1.0132 0.035 Uiso 1 1 calc R . .
H25C H 0.8747 -0.0109 0.9700 0.035 Uiso 1 1 calc R . .
C26 C 0.7353(2) 0.20690(13) 0.88234(12) 0.0161(6) Uani 1 1 d . . .
C27 C 0.8305(2) 0.21318(13) 0.84636(13) 0.0198(6) Uani 1 1 d . . .
H27A H 0.8126 0.2034 0.8073 0.024 Uiso 1 1 calc R . .
H27B H 0.8816 0.1828 0.8589 0.024 Uiso 1 1 calc R . .
C28 C 0.8790(2) 0.27806(14) 0.84830(13) 0.0223(7) Uani 1 1 d . . .
H28A H 0.8313 0.3080 0.8326 0.033 Uiso 1 1 calc R . .
H28B H 0.9422 0.2782 0.8265 0.033 Uiso 1 1 calc R . .
H28C H 0.8943 0.2890 0.8870 0.033 Uiso 1 1 calc R . .
C29 C 0.4959(3) 0.33216(15) 0.79916(13) 0.0280(7) Uani 1 1 d . . .
H29 H 0.5113 0.3453 0.8382 0.034 Uiso 1 1 calc R . .
Cl1 Cl 0.41148(6) 0.26751(3) 1.00387(3) 0.02122(18) Uani 1 1 d . . .
Cl2 Cl 0.56189(5) 0.36426(3) 0.93348(3) 0.01897(17) Uani 1 1 d . . .
Cl3 Cl 0.41659(8) 0.26454(4) 0.80200(4) 0.0343(2) Uani 1 1 d . . .
Cl4 Cl 0.61459(7) 0.31499(4) 0.76470(4) 0.0351(2) Uani 1 1 d . . .
Cl5 Cl 0.43239(7) 0.39443(4) 0.76415(4) 0.0327(2) Uani 1 1 d . . .
N1 N 0.57487(18) 0.16503(12) 0.96473(10) 0.0161(5) Uani 1 1 d . . .
N2 N 0.69502(18) 0.14642(11) 0.88880(10) 0.0146(5) Uani 1 1 d . . .
N3 N 0.6921(2) 0.25321(11) 0.90779(11) 0.0172(5) Uani 1 1 d . . .
H3 H 0.7252 0.2880 0.9047 0.021 Uiso 1 1 calc R . .
Pd1 Pd 0.562515(17) 0.258382(11) 0.952891(9) 0.01381(10) Uani 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
C1 N1 1.284(4) . ?
C1 N2 1.385(4) . ?
C1 H1 0.9300 . ?
C2 C7 1.395(4) . ?
C2 C3 1.402(4) . ?
C2 N1 1.465(4) . ?
C3 C4 1.392(4) . ?
C3 C8 1.526(4) . ?
C4 C5 1.384(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(4) . ?
C6 H6 0.9300 . ?
C7 C11 1.519(4) . ?
C8 C9 1.526(4) . ?
C8 C10 1.534(4) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.519(4) . ?
C11 C13 1.532(4) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.399(4) . ?
C14 C19 1.400(4) . ?
C14 N2 1.465(3) . ?
C15 C16 1.389(4) . ?
C15 C20 1.534(4) . ?
C16 C17 1.384(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(4) . ?
C18 H18 0.9300 . ?
C19 C23 1.520(4) . ?
C20 C22 1.533(5) . ?
C20 C21 1.537(5) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C25 1.533(4) . ?
C23 C24 1.535(4) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N3 1.282(4) . ?
C26 N2 1.400(4) . ?
C26 C27 1.494(4) . ?
C27 C28 1.520(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 Cl5 1.764(3) . ?
C29 Cl4 1.766(4) . ?
C29 Cl3 1.769(3) . ?
C29 H29 0.9800 . ?
Cl1 Pd1 2.2899(10) . ?
Cl2 Pd1 2.3065(9) . ?
N1 Pd1 2.019(3) . ?
N3 Pd1 1.978(3) . ?
N3 H3 0.8600 . ?

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
N1 C1 N2 127.4(3) . . ?
N1 C1 H1 116.3 . . ?
N2 C1 H1 116.3 . . ?
C7 C2 C3 123.0(3) . . ?
C7 C2 N1 118.5(2) . . ?
C3 C2 N1 118.5(2) . . ?
C4 C3 C2 117.4(3) . . ?
C4 C3 C8 120.5(3) . . ?
C2 C3 C8 122.1(3) . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 117.2(3) . . ?
C2 C7 C11 121.6(3) . . ?
C6 C7 C11 121.1(3) . . ?
C9 C8 C3 113.6(3) . . ?
C9 C8 C10 109.8(3) . . ?
C3 C8 C10 109.3(2) . . ?
C9 C8 H8 108.0 . . ?
C3 C8 H8 108.0 . . ?
C10 C8 H8 108.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C12 113.2(2) . . ?
C7 C11 C13 109.5(2) . . ?
C12 C11 C13 109.3(3) . . ?
C7 C11 H11 108.2 . . ?
C12 C11 H11 108.2 . . ?
C13 C11 H11 108.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 123.2(3) . . ?
C15 C14 N2 118.4(2) . . ?
C19 C14 N2 118.3(2) . . ?
C16 C15 C14 117.2(3) . . ?
C16 C15 C20 119.6(3) . . ?
C14 C15 C20 123.2(3) . . ?
C17 C16 C15 121.5(3) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 121.1(3) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C14 117.0(3) . . ?
C18 C19 C23 120.3(3) . . ?
C14 C19 C23 122.6(3) . . ?
C22 C20 C15 110.6(3) . . ?
C22 C20 C21 109.9(3) . . ?
C15 C20 C21 110.8(3) . . ?
C22 C20 H20 108.5 . . ?
C15 C20 H20 108.5 . . ?
C21 C20 H20 108.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C25 112.4(2) . . ?
C19 C23 C24 111.1(2) . . ?
C25 C23 C24 109.6(2) . . ?
C19 C23 H23 107.9 . . ?
C25 C23 H23 107.9 . . ?
C24 C23 H23 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 120.1(3) . . ?
N3 C26 C27 123.4(3) . . ?
N2 C26 C27 116.6(2) . . ?
C26 C27 C28 113.7(2) . . ?
C26 C27 H27A 108.8 . . ?
C28 C27 H27A 108.8 . . ?
C26 C27 H27B 108.8 . . ?
C28 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl5 C29 Cl4 110.04(18) . . ?
Cl5 C29 Cl3 111.47(19) . . ?
Cl4 C29 Cl3 110.24(18) . . ?
Cl5 C29 H29 108.3 . . ?
Cl4 C29 H29 108.3 . . ?
Cl3 C29 H29 108.3 . . ?
C1 N1 C2 114.1(2) . . ?
C1 N1 Pd1 123.6(2) . . ?
C2 N1 Pd1 122.25(18) . . ?
C1 N2 C26 123.8(2) . . ?
C1 N2 C14 114.5(2) . . ?
C26 N2 C14 120.9(2) . . ?
C26 N3 Pd1 131.1(2) . . ?
C26 N3 H3 114.4 . . ?
Pd1 N3 H3 114.4 . . ?
N3 Pd1 N1 87.27(9) . . ?
N3 Pd1 Cl1 178.14(7) . . ?
N1 Pd1 Cl1 94.51(7) . . ?
N3 Pd1 Cl2 87.23(7) . . ?
N1 Pd1 Cl2 174.47(7) . . ?
Cl1 Pd1 Cl2 90.98(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 0.5(4) . . . . ?
N1 C2 C3 C4 179.7(3) . . . . ?
C7 C2 C3 C8 -176.1(3) . . . . ?
N1 C2 C3 C8 3.1(4) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C8 C3 C4 C5 176.3(3) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C4 C5 C6 C7 1.8(5) . . . . ?
C3 C2 C7 C6 0.5(4) . . . . ?
N1 C2 C7 C6 -178.7(3) . . . . ?
C3 C2 C7 C11 -178.4(3) . . . . ?
N1 C2 C7 C11 2.3(4) . . . . ?
C5 C6 C7 C2 -1.6(4) . . . . ?
C5 C6 C7 C11 177.3(3) . . . . ?
C4 C3 C8 C9 39.0(4) . . . . ?
C2 C3 C8 C9 -144.6(3) . . . . ?
C4 C3 C8 C10 -84.1(3) . . . . ?
C2 C3 C8 C10 92.4(3) . . . . ?
C2 C7 C11 C12 -142.3(3) . . . . ?
C6 C7 C11 C12 38.9(4) . . . . ?
C2 C7 C11 C13 95.5(3) . . . . ?
C6 C7 C11 C13 -83.4(3) . . . . ?
C19 C14 C15 C16 2.6(4) . . . . ?
N2 C14 C15 C16 -174.7(2) . . . . ?
C19 C14 C15 C20 -175.8(3) . . . . ?
N2 C14 C15 C20 6.9(4) . . . . ?
C14 C15 C16 C17 1.4(4) . . . . ?
C20 C15 C16 C17 179.9(3) . . . . ?
C15 C16 C17 C18 -3.4(5) . . . . ?
C16 C17 C18 C19 1.5(5) . . . . ?
C17 C18 C19 C14 2.2(4) . . . . ?
C17 C18 C19 C23 -174.5(3) . . . . ?
C15 C14 C19 C18 -4.3(4) . . . . ?
N2 C14 C19 C18 173.0(2) . . . . ?
C15 C14 C19 C23 172.2(3) . . . . ?
N2 C14 C19 C23 -10.5(4) . . . . ?
C16 C15 C20 C22 -61.3(4) . . . . ?
C14 C15 C20 C22 117.1(3) . . . . ?
C16 C15 C20 C21 60.8(4) . . . . ?
C14 C15 C20 C21 -120.8(3) . . . . ?
C18 C19 C23 C25 -70.6(3) . . . . ?
C14 C19 C23 C25 112.9(3) . . . . ?
C18 C19 C23 C24 52.6(3) . . . . ?
C14 C19 C23 C24 -123.9(3) . . . . ?
N3 C26 C27 C28 6.9(4) . . . . ?
N2 C26 C27 C28 -171.4(2) . . . . ?
N2 C1 N1 C2 -172.6(3) . . . . ?
N2 C1 N1 Pd1 6.7(4) . . . . ?
C7 C2 N1 C1 -91.6(3) . . . . ?
C3 C2 N1 C1 89.2(3) . . . . ?
C7 C2 N1 Pd1 89.2(3) . . . . ?
C3 C2 N1 Pd1 -90.0(3) . . . . ?
N1 C1 N2 C26 18.2(4) . . . . ?
N1 C1 N2 C14 -171.6(3) . . . . ?
N3 C26 N2 C1 -18.4(4) . . . . ?
C27 C26 N2 C1 159.9(3) . . . . ?
N3 C26 N2 C14 172.0(3) . . . . ?
C27 C26 N2 C14 -9.6(4) . . . . ?
C15 C14 N2 C1 100.4(3) . . . . ?
C19 C14 N2 C1 -77.0(3) . . . . ?
C15 C14 N2 C26 -89.1(3) . . . . ?
C19 C14 N2 C26 93.4(3) . . . . ?
N2 C26 N3 Pd1 -6.4(4) . . . . ?
C27 C26 N3 Pd1 175.3(2) . . . . ?
C26 N3 Pd1 N1 21.5(3) . . . . ?
C26 N3 Pd1 Cl1 -142(2) . . . . ?
C26 N3 Pd1 Cl2 -157.9(3) . . . . ?
C1 N1 Pd1 N3 -20.5(2) . . . . ?
C2 N1 Pd1 N3 158.7(2) . . . . ?
C1 N1 Pd1 Cl1 159.0(2) . . . . ?
C2 N1 Pd1 Cl1 -21.8(2) . . . . ?
C1 N1 Pd1 Cl2 -14.3(9) . . . . ?
C2 N1 Pd1 Cl2 164.9(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.670
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.156
_database_code_depnum_ccdc_archive 'CCDC 1014316'
#######################################################################
#
#                 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_Compound-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H38 Cl2 N3 Pd, C25 H37 N2, C H2 Cl2'
_chemical_formula_sum            'C54 H77 Cl4 N5 Pd'
_chemical_formula_weight         1044.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   10.2658(18)
_cell_length_b                   14.678(3)
_cell_length_c                   36.568(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.918(3)
_cell_angle_gamma                90.00
_cell_volume                     5457.5(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5804
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.34

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29117
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.12
_diffrn_reflns_theta_max         25.50
_reflns_number_total             10110
_reflns_number_gt                7899
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.1042P)²+8.4436P] 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         10110
_refine_ls_number_parameters     593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1849
_refine_ls_wR_factor_gt          0.1376
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
C1 C 0.1007(4) 0.3495(3) 0.56422(12) 0.0171(9) Uani 1 1 d . . .
H1 H 0.0900 0.3673 0.5396 0.020 Uiso 1 1 calc R . .
C2 C 0.0707(4) 0.2077(3) 0.53710(12) 0.0182(9) Uani 1 1 d . . .
C3 C -0.0516(5) 0.1664(3) 0.52644(13) 0.0221(10) Uani 1 1 d . . .
C4 C -0.0669(5) 0.1154(3) 0.49419(13) 0.0238(10) Uani 1 1 d . . .
H4 H -0.1471 0.0872 0.4865 0.029 Uiso 1 1 calc R . .
C5 C 0.0348(5) 0.1055(3) 0.47318(13) 0.0257(11) Uani 1 1 d . . .
H5 H 0.0225 0.0713 0.4516 0.031 Uiso 1 1 calc R . .
C6 C 0.1525(5) 0.1460(3) 0.48436(13) 0.0250(10) Uani 1 1 d . . .
H6 H 0.2199 0.1389 0.4700 0.030 Uiso 1 1 calc R . .
C7 C 0.1762(5) 0.1982(3) 0.51674(13) 0.0209(10) Uani 1 1 d . . .
C8 C -0.1632(5) 0.1788(3) 0.54934(13) 0.0240(10) Uani 1 1 d . . .
H8 H -0.1247 0.1769 0.5754 0.029 Uiso 1 1 calc R . .
C9 C -0.2298(5) 0.2709(3) 0.54249(14) 0.0277(11) Uani 1 1 d . . .
H9A H -0.1642 0.3180 0.5443 0.042 Uiso 1 1 calc R . .
H9B H -0.2877 0.2812 0.5606 0.042 Uiso 1 1 calc R . .
H9C H -0.2794 0.2718 0.5182 0.042 Uiso 1 1 calc R . .
C10 C -0.2661(5) 0.1027(4) 0.54330(16) 0.0355(13) Uani 1 1 d . . .
H10A H -0.3284 0.1100 0.5604 0.053 Uiso 1 1 calc R . .
H10B H -0.2233 0.0447 0.5472 0.053 Uiso 1 1 calc R . .
H10C H -0.3109 0.1058 0.5185 0.053 Uiso 1 1 calc R . .
C11 C 0.3103(5) 0.2382(3) 0.52937(13) 0.0238(10) Uani 1 1 d . . .
H11 H 0.2965 0.2999 0.5384 0.029 Uiso 1 1 calc R . .
C12 C 0.3985(5) 0.2470(4) 0.49896(14) 0.0309(12) Uani 1 1 d . . .
H12A H 0.4226 0.1874 0.4914 0.046 Uiso 1 1 calc R . .
H12B H 0.4764 0.2805 0.5082 0.046 Uiso 1 1 calc R . .
H12C H 0.3517 0.2786 0.4782 0.046 Uiso 1 1 calc R . .
C13 C 0.3833(5) 0.1846(4) 0.56172(15) 0.0358(13) Uani 1 1 d . . .
H13A H 0.3311 0.1829 0.5816 0.054 Uiso 1 1 calc R . .
H13B H 0.4659 0.2136 0.5700 0.054 Uiso 1 1 calc R . .
H13C H 0.3987 0.1235 0.5539 0.054 Uiso 1 1 calc R . .
C14 C 0.1478(4) 0.5068(3) 0.57563(12) 0.0189(9) Uani 1 1 d . . .
C15 C 0.2761(4) 0.5363(3) 0.57455(12) 0.0201(10) Uani 1 1 d . . .
C16 C 0.2940(5) 0.6250(3) 0.56281(13) 0.0248(10) Uani 1 1 d . . .
H16 H 0.3789 0.6462 0.5619 0.030 Uiso 1 1 calc R . .
C17 C 0.1891(5) 0.6821(3) 0.55254(14) 0.0276(11) Uani 1 1 d . . .
H17 H 0.2035 0.7415 0.5452 0.033 Uiso 1 1 calc R . .
C18 C 0.0630(5) 0.6513(3) 0.55311(12) 0.0224(10) Uani 1 1 d . . .
H18 H -0.0073 0.6899 0.5455 0.027 Uiso 1 1 calc R . .
C19 C 0.0383(5) 0.5632(3) 0.56488(12) 0.0207(10) Uani 1 1 d . . .
C20 C 0.3959(4) 0.4756(3) 0.58508(12) 0.0208(10) Uani 1 1 d . . .
H20 H 0.3636 0.4142 0.5894 0.025 Uiso 1 1 calc R . .
C21 C 0.4759(5) 0.5071(3) 0.62076(14) 0.0296(11) Uani 1 1 d . . .
H21A H 0.5066 0.5681 0.6177 0.044 Uiso 1 1 calc R . .
H21B H 0.5498 0.4673 0.6269 0.044 Uiso 1 1 calc R . .
H21C H 0.4220 0.5060 0.6402 0.044 Uiso 1 1 calc R . .
C22 C 0.4804(5) 0.4689(4) 0.55372(14) 0.0282(11) Uani 1 1 d . . .
H22A H 0.5162 0.5278 0.5494 0.042 Uiso 1 1 calc R . .
H22B H 0.4271 0.4482 0.5317 0.042 Uiso 1 1 calc R . .
H22C H 0.5509 0.4266 0.5605 0.042 Uiso 1 1 calc R . .
C23 C -0.1013(4) 0.5314(3) 0.56553(12) 0.0204(10) Uani 1 1 d . . .
H23 H -0.0974 0.4696 0.5758 0.024 Uiso 1 1 calc R . .
C24 C -0.1732(5) 0.5917(4) 0.59048(14) 0.0311(12) Uani 1 1 d . . .
H24A H -0.1239 0.5938 0.6148 0.047 Uiso 1 1 calc R . .
H24B H -0.2589 0.5669 0.5919 0.047 Uiso 1 1 calc R . .
H24C H -0.1818 0.6522 0.5804 0.047 Uiso 1 1 calc R . .
C25 C -0.1765(4) 0.5266(3) 0.52646(12) 0.0224(10) Uani 1 1 d . . .
H25A H -0.1866 0.5869 0.5163 0.034 Uiso 1 1 calc R . .
H25B H -0.2616 0.5002 0.5273 0.034 Uiso 1 1 calc R . .
H25C H -0.1284 0.4897 0.5113 0.034 Uiso 1 1 calc R . .
C26 C 0.1517(5) 0.4016(3) 0.62931(11) 0.0197(9) Uani 1 1 d . . .
H26A H 0.1364 0.4584 0.6416 0.024 Uiso 1 1 calc R . .
H26B H 0.2435 0.3856 0.6361 0.024 Uiso 1 1 calc R . .
C27 C 0.0675(5) 0.3282(3) 0.64311(12) 0.0227(10) Uani 1 1 d . . .
H27 H 0.0913 0.3242 0.6699 0.027 Uiso 1 1 calc R . .
C28 C -0.0734(5) 0.3480(3) 0.63567(12) 0.0237(10) Uani 1 1 d . . .
C29 C 0.6448(5) 0.4635(3) 0.82226(14) 0.0283(11) Uani 1 1 d . . .
H29 H 0.5790 0.4358 0.8060 0.034 Uiso 1 1 calc R . .
C30 C 0.4755(5) 0.5298(3) 0.85332(13) 0.0216(10) Uani 1 1 d . . .
C31 C 0.4195(5) 0.6118(3) 0.84078(14) 0.0288(11) Uani 1 1 d . . .
C32 C 0.2864(5) 0.6263(4) 0.84442(17) 0.0383(13) Uani 1 1 d . . .
H32 H 0.2460 0.6808 0.8363 0.046 Uiso 1 1 calc R . .
C33 C 0.2146(5) 0.5599(4) 0.86000(16) 0.0383(13) Uani 1 1 d . . .
H33 H 0.1263 0.5696 0.8619 0.046 Uiso 1 1 calc R . .
C34 C 0.2750(5) 0.4791(4) 0.87264(14) 0.0327(12) Uani 1 1 d . . .
H34 H 0.2261 0.4354 0.8832 0.039 Uiso 1 1 calc R . .
C35 C 0.4060(4) 0.4614(3) 0.87002(13) 0.0243(10) Uani 1 1 d . . .
C36 C 0.4960(6) 0.6828(4) 0.82216(17) 0.0406(14) Uani 1 1 d . . .
H36 H 0.5894 0.6672 0.8280 0.049 Uiso 1 1 calc R . .
C37 C 0.4628(7) 0.6797(5) 0.78073(19) 0.0585(19) Uani 1 1 d . . .
H37A H 0.4797 0.6196 0.7721 0.088 Uiso 1 1 calc R . .
H37B H 0.5160 0.7230 0.7699 0.088 Uiso 1 1 calc R . .
H37C H 0.3716 0.6943 0.7739 0.088 Uiso 1 1 calc R . .
C38 C 0.4795(7) 0.7787(4) 0.83677(18) 0.0496(16) Uani 1 1 d . . .
H38A H 0.5288 0.8208 0.8240 0.074 Uiso 1 1 calc R . .
H38B H 0.5112 0.7805 0.8627 0.074 Uiso 1 1 calc R . .
H38C H 0.3882 0.7951 0.8328 0.074 Uiso 1 1 calc R . .
C39 C 0.4766(5) 0.3771(4) 0.88654(14) 0.0315(12) Uani 1 1 d . . .
H39 H 0.5392 0.3583 0.8701 0.038 Uiso 1 1 calc R . .
C40 C 0.3807(5) 0.2969(3) 0.88937(18) 0.0381(13) Uani 1 1 d . . .
H40A H 0.3233 0.3112 0.9072 0.057 Uiso 1 1 calc R . .
H40B H 0.4300 0.2429 0.8970 0.057 Uiso 1 1 calc R . .
H40C H 0.3295 0.2867 0.8657 0.057 Uiso 1 1 calc R . .
C41 C 0.5539(6) 0.3988(4) 0.92355(16) 0.0436(15) Uani 1 1 d . . .
H41A H 0.6212 0.4424 0.9204 0.065 Uiso 1 1 calc R . .
H41B H 0.5936 0.3441 0.9343 0.065 Uiso 1 1 calc R . .
H41C H 0.4961 0.4238 0.9395 0.065 Uiso 1 1 calc R . .
C42 C 0.8039(5) 0.3941(3) 0.78875(14) 0.0268(11) Uani 1 1 d . . .
C43 C 0.8516(5) 0.3070(3) 0.79912(14) 0.0289(11) Uani 1 1 d . . .
C44 C 0.8979(5) 0.2549(4) 0.77259(14) 0.0323(12) Uani 1 1 d . . .
H44 H 0.9299 0.1967 0.7786 0.039 Uiso 1 1 calc R . .
C45 C 0.8978(6) 0.2873(4) 0.73692(16) 0.0386(14) Uani 1 1 d . . .
H45 H 0.9328 0.2519 0.7196 0.046 Uiso 1 1 calc R . .
C46 C 0.8456(5) 0.3721(4) 0.72716(14) 0.0332(12) Uani 1 1 d . . .
H46 H 0.8418 0.3920 0.7029 0.040 Uiso 1 1 calc R . .
C47 C 0.7988(5) 0.4280(3) 0.75313(13) 0.0275(11) Uani 1 1 d . . .
C48 C 0.8568(6) 0.2737(4) 0.83926(15) 0.0364(13) Uani 1 1 d . . .
H48 H 0.7847 0.3027 0.8499 0.044 Uiso 1 1 calc R . .
C49 C 0.9859(7) 0.3038(4) 0.86157(18) 0.0507(17) Uani 1 1 d . . .
H49A H 0.9868 0.2867 0.8869 0.076 Uiso 1 1 calc R . .
H49B H 0.9944 0.3687 0.8599 0.076 Uiso 1 1 calc R . .
H49C H 1.0580 0.2749 0.8520 0.076 Uiso 1 1 calc R . .
C50 C 0.8397(7) 0.1717(4) 0.84140(16) 0.0459(15) Uani 1 1 d . . .
H50A H 0.9155 0.1418 0.8343 0.069 Uiso 1 1 calc R . .
H50B H 0.7628 0.1536 0.8250 0.069 Uiso 1 1 calc R . .
H50C H 0.8298 0.1547 0.8662 0.069 Uiso 1 1 calc R . .
C51 C 0.7417(6) 0.5211(4) 0.74100(14) 0.0346(13) Uani 1 1 d . . .
H51 H 0.7268 0.5545 0.7632 0.041 Uiso 1 1 calc R . .
C52 C 0.8337(8) 0.5772(5) 0.7212(2) 0.063(2) Uani 1 1 d . . .
H52A H 0.8424 0.5493 0.6979 0.095 Uiso 1 1 calc R . .
H52B H 0.9184 0.5804 0.7360 0.095 Uiso 1 1 calc R . .
H52C H 0.7988 0.6376 0.7171 0.095 Uiso 1 1 calc R . .
C53 C 0.6110(7) 0.5093(5) 0.71744(18) 0.0558(18) Uani 1 1 d . . .
H53A H 0.6222 0.4746 0.6958 0.084 Uiso 1 1 calc R . .
H53B H 0.5752 0.5680 0.7102 0.084 Uiso 1 1 calc R . .
H53C H 0.5519 0.4778 0.7312 0.084 Uiso 1 1 calc R . .
C54 C 0.1989(7) 0.4294(5) 0.77175(19) 0.0579(18) Uani 1 1 d . . .
H54A H 0.1115 0.4041 0.7714 0.070 Uiso 1 1 calc R . .
H54B H 0.2137 0.4728 0.7919 0.070 Uiso 1 1 calc R . .
Cl1 Cl 0.12791(12) 0.04999(8) 0.59951(3) 0.0259(3) Uani 1 1 d . . .
Cl2 Cl 0.10307(12) 0.14651(8) 0.68107(3) 0.0267(3) Uani 1 1 d . . .
Cl3 Cl 0.3163(2) 0.34096(13) 0.77933(6) 0.0691(5) Uani 1 1 d . . .
Cl4 Cl 0.2080(2) 0.48616(14) 0.72991(5) 0.0712(5) Uani 1 1 d . . .
N1 N 0.0893(3) 0.2624(2) 0.57038(10) 0.0175(8) Uani 1 1 d . . .
N2 N 0.1259(4) 0.4158(2) 0.58904(10) 0.0176(8) Uani 1 1 d . . .
N3 N -0.1822(4) 0.3639(3) 0.62981(12) 0.0325(10) Uani 1 1 d . . .
N4 N 0.7645(4) 0.4514(3) 0.81754(12) 0.0291(9) Uani 1 1 d . . .
H4A H 0.8249 0.4787 0.8322 0.035 Uiso 1 1 calc R . .
N5 N 0.6105(4) 0.5142(3) 0.84958(11) 0.0234(9) Uani 1 1 d . . .
H5A H 0.6708 0.5380 0.8653 0.028 Uiso 1 1 calc R . .
Pd1 Pd 0.09702(3) 0.20314(2) 0.621769(9) 0.01847(13) Uani 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
C1 N1 1.306(6) . ?
C1 N2 1.331(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.401(7) . ?
C2 C7 1.403(6) . ?
C2 N1 1.448(6) . ?
C3 C4 1.388(7) . ?
C3 C8 1.520(6) . ?
C4 C5 1.386(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.358(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(6) . ?
C6 H6 0.9300 . ?
C7 C11 1.510(7) . ?
C8 C9 1.521(7) . ?
C8 C10 1.531(7) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.529(7) . ?
C11 C12 1.533(7) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.392(6) . ?
C14 C19 1.408(6) . ?
C14 N2 1.451(6) . ?
C15 C16 1.392(7) . ?
C15 C20 1.525(6) . ?
C16 C17 1.375(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.398(6) . ?
C18 H18 0.9300 . ?
C19 C23 1.510(6) . ?
C20 C21 1.515(6) . ?
C20 C22 1.534(7) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C25 1.529(6) . ?
C23 C24 1.532(6) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N2 1.475(5) . ?
C26 C27 1.511(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.464(7) . ?
C27 Pd1 2.033(5) . ?
C27 H27 0.9800 . ?
C28 N3 1.133(6) . ?
C29 N4 1.277(6) . ?
C29 N5 1.331(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.385(7) . ?
C30 C35 1.417(7) . ?
C30 N5 1.430(6) . ?
C31 C32 1.407(7) . ?
C31 C36 1.521(7) . ?
C32 C33 1.390(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.388(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.386(7) . ?
C34 H34 0.9300 . ?
C35 C39 1.516(7) . ?
C36 C37 1.507(9) . ?
C36 C38 1.523(8) . ?
C36 H36 0.9800 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C41 1.506(8) . ?
C39 C40 1.547(7) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C47 1.388(7) . ?
C42 C43 1.403(7) . ?
C42 N4 1.448(6) . ?
C43 C44 1.371(7) . ?
C43 C48 1.541(7) . ?
C44 C45 1.388(8) . ?
C44 H44 0.9300 . ?
C45 C46 1.382(8) . ?
C45 H45 0.9300 . ?
C46 C47 1.390(7) . ?
C46 H46 0.9300 . ?
C47 C51 1.528(7) . ?
C48 C50 1.511(8) . ?
C48 C49 1.523(8) . ?
C48 H48 0.9800 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C53 1.502(8) . ?
C51 C52 1.512(8) . ?
C51 H51 0.9800 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 Cl4 1.756(7) . ?
C54 Cl3 1.767(7) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
Cl1 Pd1 2.4265(12) . ?
Cl2 Pd1 2.3152(12) . ?
N1 Pd1 2.062(4) . ?
N4 H4A 0.8600 . ?
N5 H5A 0.8600 . ?

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
N1 C1 N2 127.7(4) . . ?
N1 C1 H1 116.2 . . ?
N2 C1 H1 116.2 . . ?
C3 C2 C7 122.5(4) . . ?
C3 C2 N1 118.9(4) . . ?
C7 C2 N1 118.6(4) . . ?
C4 C3 C2 117.5(4) . . ?
C4 C3 C8 121.8(4) . . ?
C2 C3 C8 120.7(4) . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 122.4(5) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C2 C7 C6 116.5(4) . . ?
C2 C7 C11 122.5(4) . . ?
C6 C7 C11 121.0(4) . . ?
C3 C8 C9 111.8(4) . . ?
C3 C8 C10 113.0(4) . . ?
C9 C8 C10 109.8(4) . . ?
C3 C8 H8 107.3 . . ?
C9 C8 H8 107.3 . . ?
C10 C8 H8 107.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C13 111.4(4) . . ?
C7 C11 C12 114.6(4) . . ?
C13 C11 C12 109.2(4) . . ?
C7 C11 H11 107.1 . . ?
C13 C11 H11 107.1 . . ?
C12 C11 H11 107.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 122.1(4) . . ?
C15 C14 N2 119.2(4) . . ?
C19 C14 N2 118.7(4) . . ?
C16 C15 C14 117.8(4) . . ?
C16 C15 C20 119.2(4) . . ?
C14 C15 C20 123.0(4) . . ?
C17 C16 C15 121.5(4) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 121.4(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C18 C19 C14 117.3(4) . . ?
C18 C19 C23 120.3(4) . . ?
C14 C19 C23 122.4(4) . . ?
C21 C20 C15 111.2(4) . . ?
C21 C20 C22 111.6(4) . . ?
C15 C20 C22 111.6(4) . . ?
C21 C20 H20 107.4 . . ?
C15 C20 H20 107.4 . . ?
C22 C20 H20 107.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C25 110.9(4) . . ?
C19 C23 C24 111.5(4) . . ?
C25 C23 C24 111.1(4) . . ?
C19 C23 H23 107.7 . . ?
C25 C23 H23 107.7 . . ?
C24 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 C27 113.7(4) . . ?
N2 C26 H26A 108.8 . . ?
C27 C26 H26A 108.8 . . ?
N2 C26 H26B 108.8 . . ?
C27 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C26 113.1(4) . . ?
C28 C27 Pd1 107.7(3) . . ?
C26 C27 Pd1 113.2(3) . . ?
C28 C27 H27 107.5 . . ?
C26 C27 H27 107.5 . . ?
Pd1 C27 H27 107.5 . . ?
N3 C28 C27 179.6(6) . . ?
N4 C29 N5 122.5(5) . . ?
N4 C29 H29 118.7 . . ?
N5 C29 H29 118.7 . . ?
C31 C30 C35 123.2(4) . . ?
C31 C30 N5 118.1(4) . . ?
C35 C30 N5 118.7(4) . . ?
C30 C31 C32 117.6(5) . . ?
C30 C31 C36 121.8(5) . . ?
C32 C31 C36 120.5(5) . . ?
C33 C32 C31 120.6(5) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 119.9(5) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C35 C34 C33 122.0(5) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C34 C35 C30 116.6(4) . . ?
C34 C35 C39 122.7(5) . . ?
C30 C35 C39 120.6(4) . . ?
C37 C36 C31 111.7(5) . . ?
C37 C36 C38 111.1(5) . . ?
C31 C36 C38 112.7(5) . . ?
C37 C36 H36 107.0 . . ?
C31 C36 H36 107.0 . . ?
C38 C36 H36 107.0 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41 C39 C35 110.5(5) . . ?
C41 C39 C40 111.2(5) . . ?
C35 C39 C40 112.0(4) . . ?
C41 C39 H39 107.7 . . ?
C35 C39 H39 107.7 . . ?
C40 C39 H39 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 123.2(4) . . ?
C47 C42 N4 119.7(4) . . ?
C43 C42 N4 117.1(4) . . ?
C44 C43 C42 117.4(5) . . ?
C44 C43 C48 121.8(5) . . ?
C42 C43 C48 120.8(4) . . ?
C43 C44 C45 121.2(5) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C46 C45 C44 120.1(5) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C45 C46 C47 120.9(5) . . ?
C45 C46 H46 119.6 . . ?
C47 C46 H46 119.6 . . ?
C42 C47 C46 117.2(5) . . ?
C42 C47 C51 123.8(4) . . ?
C46 C47 C51 119.0(5) . . ?
C50 C48 C49 111.0(5) . . ?
C50 C48 C43 112.0(4) . . ?
C49 C48 C43 109.3(5) . . ?
C50 C48 H48 108.1 . . ?
C49 C48 H48 108.1 . . ?
C43 C48 H48 108.1 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C53 C51 C52 110.8(5) . . ?
C53 C51 C47 109.9(5) . . ?
C52 C51 C47 112.7(5) . . ?
C53 C51 H51 107.7 . . ?
C52 C51 H51 107.7 . . ?
C47 C51 H51 107.7 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Cl4 C54 Cl3 111.6(4) . . ?
Cl4 C54 H54A 109.3 . . ?
Cl3 C54 H54A 109.3 . . ?
Cl4 C54 H54B 109.3 . . ?
Cl3 C54 H54B 109.3 . . ?
H54A C54 H54B 108.0 . . ?
C1 N1 C2 113.7(4) . . ?
C1 N1 Pd1 125.2(3) . . ?
C2 N1 Pd1 121.1(3) . . ?
C1 N2 C14 117.8(4) . . ?
C1 N2 C26 124.7(4) . . ?
C14 N2 C26 116.9(3) . . ?
C29 N4 C42 123.3(4) . . ?
C29 N4 H4A 118.4 . . ?
C42 N4 H4A 118.4 . . ?
C29 N5 C30 121.4(4) . . ?
C29 N5 H5A 119.3 . . ?
C30 N5 H5A 119.3 . . ?
C27 Pd1 N1 88.87(16) . . ?
C27 Pd1 Cl2 87.18(13) . . ?
N1 Pd1 Cl2 176.05(11) . . ?
C27 Pd1 Cl1 176.62(13) . . ?
N1 Pd1 Cl1 94.31(11) . . ?
Cl2 Pd1 Cl1 89.64(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 -0.7(7) . . . . ?
N1 C2 C3 C4 179.2(4) . . . . ?
C7 C2 C3 C8 -179.9(4) . . . . ?
N1 C2 C3 C8 0.1(6) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C8 C3 C4 C5 179.1(4) . . . . ?
C3 C4 C5 C6 0.4(7) . . . . ?
C4 C5 C6 C7 0.0(7) . . . . ?
C3 C2 C7 C6 1.1(6) . . . . ?
N1 C2 C7 C6 -178.9(4) . . . . ?
C3 C2 C7 C11 -176.4(4) . . . . ?
N1 C2 C7 C11 3.7(6) . . . . ?
C5 C6 C7 C2 -0.8(7) . . . . ?
C5 C6 C7 C11 176.8(4) . . . . ?
C4 C3 C8 C9 -100.9(5) . . . . ?
C2 C3 C8 C9 78.2(5) . . . . ?
C4 C3 C8 C10 23.6(6) . . . . ?
C2 C3 C8 C10 -157.3(5) . . . . ?
C2 C7 C11 C13 73.4(6) . . . . ?
C6 C7 C11 C13 -104.0(5) . . . . ?
C2 C7 C11 C12 -162.0(4) . . . . ?
C6 C7 C11 C12 20.7(6) . . . . ?
C19 C14 C15 C16 0.8(7) . . . . ?
N2 C14 C15 C16 -177.7(4) . . . . ?
C19 C14 C15 C20 -178.3(4) . . . . ?
N2 C14 C15 C20 3.1(6) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C20 C15 C16 C17 179.1(4) . . . . ?
C15 C16 C17 C18 -1.2(7) . . . . ?
C16 C17 C18 C19 1.6(7) . . . . ?
C17 C18 C19 C14 -0.9(7) . . . . ?
C17 C18 C19 C23 179.5(4) . . . . ?
C15 C14 C19 C18 -0.3(6) . . . . ?
N2 C14 C19 C18 178.2(4) . . . . ?
C15 C14 C19 C23 179.3(4) . . . . ?
N2 C14 C19 C23 -2.2(6) . . . . ?
C16 C15 C20 C21 70.2(5) . . . . ?
C14 C15 C20 C21 -110.7(5) . . . . ?
C16 C15 C20 C22 -55.2(6) . . . . ?
C14 C15 C20 C22 123.9(5) . . . . ?
C18 C19 C23 C25 65.4(5) . . . . ?
C14 C19 C23 C25 -114.2(5) . . . . ?
C18 C19 C23 C24 -59.0(6) . . . . ?
C14 C19 C23 C24 121.4(5) . . . . ?
N2 C26 C27 C28 -61.1(5) . . . . ?
N2 C26 C27 Pd1 61.8(4) . . . . ?
C26 C27 C28 N3 3(91) . . . . ?
Pd1 C27 C28 N3 -123(100) . . . . ?
C35 C30 C31 C32 -1.2(7) . . . . ?
N5 C30 C31 C32 179.7(5) . . . . ?
C35 C30 C31 C36 -178.5(5) . . . . ?
N5 C30 C31 C36 2.3(7) . . . . ?
C30 C31 C32 C33 -0.2(8) . . . . ?
C36 C31 C32 C33 177.2(5) . . . . ?
C31 C32 C33 C34 1.0(9) . . . . ?
C32 C33 C34 C35 -0.5(8) . . . . ?
C33 C34 C35 C30 -0.7(7) . . . . ?
C33 C34 C35 C39 174.7(5) . . . . ?
C31 C30 C35 C34 1.6(7) . . . . ?
N5 C30 C35 C34 -179.2(4) . . . . ?
C31 C30 C35 C39 -173.9(5) . . . . ?
N5 C30 C35 C39 5.2(7) . . . . ?
C30 C31 C36 C37 100.0(6) . . . . ?
C32 C31 C36 C37 -77.3(7) . . . . ?
C30 C31 C36 C38 -134.0(5) . . . . ?
C32 C31 C36 C38 48.7(7) . . . . ?
C34 C35 C39 C41 -97.7(6) . . . . ?
C30 C35 C39 C41 77.5(6) . . . . ?
C34 C35 C39 C40 26.9(7) . . . . ?
C30 C35 C39 C40 -157.9(5) . . . . ?
C47 C42 C43 C44 1.6(8) . . . . ?
N4 C42 C43 C44 -175.4(5) . . . . ?
C47 C42 C43 C48 179.1(5) . . . . ?
N4 C42 C43 C48 2.0(7) . . . . ?
C42 C43 C44 C45 0.2(8) . . . . ?
C48 C43 C44 C45 -177.2(5) . . . . ?
C43 C44 C45 C46 -2.6(9) . . . . ?
C44 C45 C46 C47 3.3(9) . . . . ?
C43 C42 C47 C46 -1.0(8) . . . . ?
N4 C42 C47 C46 176.0(5) . . . . ?
C43 C42 C47 C51 177.3(5) . . . . ?
N4 C42 C47 C51 -5.8(8) . . . . ?
C45 C46 C47 C42 -1.5(8) . . . . ?
C45 C46 C47 C51 -179.8(5) . . . . ?
C44 C43 C48 C50 -33.1(8) . . . . ?
C42 C43 C48 C50 149.6(5) . . . . ?
C44 C43 C48 C49 90.4(6) . . . . ?
C42 C43 C48 C49 -86.9(6) . . . . ?
C42 C47 C51 C53 -106.5(6) . . . . ?
C46 C47 C51 C53 71.6(7) . . . . ?
C42 C47 C51 C52 129.3(6) . . . . ?
C46 C47 C51 C52 -52.6(7) . . . . ?
N2 C1 N1 C2 -175.9(4) . . . . ?
N2 C1 N1 Pd1 3.8(6) . . . . ?
C3 C2 N1 C1 -110.4(5) . . . . ?
C7 C2 N1 C1 69.5(5) . . . . ?
C3 C2 N1 Pd1 69.9(5) . . . . ?
C7 C2 N1 Pd1 -110.2(4) . . . . ?
N1 C1 N2 C14 173.7(4) . . . . ?
N1 C1 N2 C26 2.8(7) . . . . ?
C15 C14 N2 C1 -95.7(5) . . . . ?
C19 C14 N2 C1 85.8(5) . . . . ?
C15 C14 N2 C26 76.0(5) . . . . ?
C19 C14 N2 C26 -102.6(5) . . . . ?
C27 C26 N2 C1 -38.6(6) . . . . ?
C27 C26 N2 C14 150.4(4) . . . . ?
N5 C29 N4 C42 177.8(4) . . . . ?
C47 C42 N4 C29 81.5(6) . . . . ?
C43 C42 N4 C29 -101.4(6) . . . . ?
N4 C29 N5 C30 177.3(4) . . . . ?
C31 C30 N5 C29 -100.1(5) . . . . ?
C35 C30 N5 C29 80.7(6) . . . . ?
C28 C27 Pd1 N1 80.3(3) . . . . ?
C26 C27 Pd1 N1 -45.4(3) . . . . ?
C28 C27 Pd1 Cl2 -99.6(3) . . . . ?
C26 C27 Pd1 Cl2 134.7(3) . . . . ?
C28 C27 Pd1 Cl1 -80(2) . . . . ?
C26 C27 Pd1 Cl1 154(2) . . . . ?
C1 N1 Pd1 C27 16.2(4) . . . . ?
C2 N1 Pd1 C27 -164.1(3) . . . . ?
C1 N1 Pd1 Cl2 17.2(17) . . . . ?
C2 N1 Pd1 Cl2 -163.2(13) . . . . ?
C1 N1 Pd1 Cl1 -164.9(3) . . . . ?
C2 N1 Pd1 Cl1 14.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.145
_database_code_depnum_ccdc_archive 'CCDC 1014317'
#######################################################################
#
#                 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_Compound5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H72 Cl2 N4 Pd'
_chemical_formula_sum            'C50 H72 Cl2 N4 Pd'
_chemical_formula_weight         906.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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'

_cell_length_a                   10.132(5)
_cell_length_b                   12.087(5)
_cell_length_c                   12.675(5)
_cell_angle_alpha                98.951(5)
_cell_angle_beta                 102.976(5)
_cell_angle_gamma                102.750(5)
_cell_volume                     1440.5(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    5123
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      22.52

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8817
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13618
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5336
_reflns_number_gt                4332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.0768P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5336
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
C1 C 0.9411(3) 1.0014(3) 0.2178(3) 0.0383(7) Uani 1 1 d . . .
H1 H 0.9016 0.9663 0.2678 0.046 Uiso 1 1 calc R . .
C2 C 0.8467(3) 0.8173(3) 0.1067(3) 0.0403(8) Uani 1 1 d . . .
C3 C 0.9207(4) 0.7318(3) 0.1068(3) 0.0518(9) Uani 1 1 d . . .
C4 C 0.8448(5) 0.6189(3) 0.0976(4) 0.0686(12) Uani 1 1 d . . .
H4 H 0.8914 0.5607 0.0971 0.082 Uiso 1 1 calc R . .
C5 C 0.7043(6) 0.5893(4) 0.0894(4) 0.0803(14) Uani 1 1 d . . .
H5 H 0.6566 0.5127 0.0840 0.096 Uiso 1 1 calc R . .
C6 C 0.6346(5) 0.6740(4) 0.0890(4) 0.0682(12) Uani 1 1 d . . .
H6 H 0.5391 0.6539 0.0843 0.082 Uiso 1 1 calc R . .
C7 C 0.7018(4) 0.7896(3) 0.0955(3) 0.0486(9) Uani 1 1 d . . .
C8 C 1.0768(5) 0.7603(4) 0.1176(4) 0.0661(11) Uani 1 1 d . . .
H8 H 1.1142 0.8449 0.1381 0.079 Uiso 1 1 calc R . .
C9 C 1.1032(7) 0.7184(7) 0.0102(6) 0.137(3) Uani 1 1 d . . .
H9A H 1.0917 0.6361 -0.0016 0.206 Uiso 1 1 calc R . .
H9B H 1.1973 0.7567 0.0112 0.206 Uiso 1 1 calc R . .
H9C H 1.0378 0.7354 -0.0485 0.206 Uiso 1 1 calc R . .
C10 C 1.1527(6) 0.7095(7) 0.2067(7) 0.139(3) Uani 1 1 d . . .
H10A H 1.1395 0.6282 0.1787 0.208 Uiso 1 1 calc R . .
H10B H 1.1157 0.7195 0.2699 0.208 Uiso 1 1 calc R . .
H10C H 1.2512 0.7485 0.2281 0.208 Uiso 1 1 calc R . .
C11 C 0.6158(4) 0.8765(4) 0.0905(3) 0.0547(10) Uani 1 1 d . . .
H11 H 0.6757 0.9500 0.0852 0.066 Uiso 1 1 calc R . .
C12 C 0.5665(5) 0.8988(5) 0.1965(4) 0.0844(14) Uani 1 1 d . . .
H12A H 0.5117 0.8271 0.2056 0.127 Uiso 1 1 calc R . .
H12B H 0.5103 0.9531 0.1904 0.127 Uiso 1 1 calc R . .
H12C H 0.6469 0.9302 0.2595 0.127 Uiso 1 1 calc R . .
C13 C 0.4901(4) 0.8367(5) -0.0128(4) 0.0788(14) Uani 1 1 d . . .
H13A H 0.5217 0.8147 -0.0770 0.118 Uiso 1 1 calc R . .
H13B H 0.4472 0.8992 -0.0218 0.118 Uiso 1 1 calc R . .
H13C H 0.4228 0.7714 -0.0044 0.118 Uiso 1 1 calc R . .
C14 C 1.0391(4) 1.1742(3) 0.3649(3) 0.0444(8) Uani 1 1 d . . .
C15 C 0.9579(4) 1.2475(3) 0.3908(3) 0.0533(9) Uani 1 1 d . . .
C16 C 0.9931(5) 1.3079(4) 0.5006(4) 0.0703(12) Uani 1 1 d . . .
H16 H 0.9408 1.3579 0.5206 0.084 Uiso 1 1 calc R . .
C17 C 1.1007(5) 1.2960(4) 0.5784(3) 0.0730(13) Uani 1 1 d . . .
H17 H 1.1214 1.3380 0.6507 0.088 Uiso 1 1 calc R . .
C18 C 1.1804(5) 1.2227(4) 0.5525(3) 0.0657(11) Uani 1 1 d . . .
H18 H 1.2539 1.2152 0.6074 0.079 Uiso 1 1 calc R . .
C19 C 1.1512(4) 1.1595(3) 0.4440(3) 0.0536(9) Uani 1 1 d . . .
C20 C 0.8362(5) 1.2637(4) 0.3053(3) 0.0642(11) Uani 1 1 d . . .
H20 H 0.8233 1.2084 0.2361 0.077 Uiso 1 1 calc R . .
C21 C 0.7009(6) 1.2361(6) 0.3388(5) 0.110(2) Uani 1 1 d . . .
H21A H 0.7086 1.2909 0.4048 0.164 Uiso 1 1 calc R . .
H21B H 0.6829 1.1590 0.3527 0.164 Uiso 1 1 calc R . .
H21C H 0.6250 1.2406 0.2801 0.164 Uiso 1 1 calc R . .
C22 C 0.8669(8) 1.3842(6) 0.2818(6) 0.122(2) Uani 1 1 d . . .
H22A H 0.7919 1.3888 0.2223 0.182 Uiso 1 1 calc R . .
H22B H 0.9535 1.4002 0.2609 0.182 Uiso 1 1 calc R . .
H22C H 0.8748 1.4403 0.3470 0.182 Uiso 1 1 calc R . .
C23 C 1.2392(5) 1.0798(4) 0.4158(3) 0.0658(11) Uani 1 1 d . . .
H23 H 1.2116 1.0525 0.3351 0.079 Uiso 1 1 calc R . .
C24 C 1.3936(6) 1.1405(6) 0.4509(7) 0.132(3) Uani 1 1 d . . .
H24A H 1.4106 1.2049 0.4155 0.198 Uiso 1 1 calc R . .
H24B H 1.4453 1.0871 0.4298 0.198 Uiso 1 1 calc R . .
H24C H 1.4235 1.1683 0.5300 0.198 Uiso 1 1 calc R . .
C25 C 1.2128(6) 0.9757(5) 0.4659(5) 0.1047(18) Uani 1 1 d . . .
H25A H 1.2460 0.9995 0.5452 0.157 Uiso 1 1 calc R . .
H25B H 1.2616 0.9222 0.4397 0.157 Uiso 1 1 calc R . .
H25C H 1.1139 0.9386 0.4450 0.157 Uiso 1 1 calc R . .
Cl1 Cl 0.77594(9) 0.93767(10) -0.11438(7) 0.0601(3) Uani 1 1 d . . .
N1 N 0.9247(3) 0.9364(2) 0.1225(2) 0.0362(6) Uani 1 1 d . . .
N2 N 1.0077(3) 1.1122(2) 0.2515(2) 0.0439(7) Uani 1 1 d . . .
H2 H 1.0337 1.1494 0.2039 0.053 Uiso 1 1 calc R . .
Pd1 Pd 1.0000 1.0000 0.0000 0.03686(15) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.289(4) . ?
C1 N2 1.313(4) . ?
C1 H1 0.9300 . ?
C2 C7 1.401(5) . ?
C2 C3 1.405(5) . ?
C2 N1 1.440(4) . ?
C3 C4 1.384(5) . ?
C3 C8 1.512(6) . ?
C4 C5 1.364(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.366(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(5) . ?
C6 H6 0.9300 . ?
C7 C11 1.506(5) . ?
C8 C9 1.479(8) . ?
C8 C10 1.509(8) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.534(6) . ?
C11 C12 1.542(6) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.386(5) . ?
C14 C19 1.400(5) . ?
C14 N2 1.444(4) . ?
C15 C16 1.394(5) . ?
C15 C20 1.519(6) . ?
C16 C17 1.346(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.398(5) . ?
C18 H18 0.9300 . ?
C19 C23 1.505(6) . ?
C20 C21 1.508(7) . ?
C20 C22 1.512(7) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C25 1.494(7) . ?
C23 C24 1.504(7) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
Cl1 Pd1 2.2913(13) . ?
N1 Pd1 2.056(3) . ?
N2 H2 0.8600 . ?
Pd1 N1 2.056(3) 2_775 ?
Pd1 Cl1 2.2913(13) 2_775 ?

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
N1 C1 N2 126.7(3) . . ?
N1 C1 H1 116.7 . . ?
N2 C1 H1 116.7 . . ?
C7 C2 C3 121.7(3) . . ?
C7 C2 N1 120.2(3) . . ?
C3 C2 N1 118.1(3) . . ?
C4 C3 C2 117.1(4) . . ?
C4 C3 C8 120.7(4) . . ?
C2 C3 C8 122.3(3) . . ?
C5 C4 C3 122.8(4) . . ?
C5 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C7 122.2(4) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C2 117.2(4) . . ?
C6 C7 C11 118.7(3) . . ?
C2 C7 C11 124.1(3) . . ?
C9 C8 C10 110.2(5) . . ?
C9 C8 C3 110.4(4) . . ?
C10 C8 C3 111.7(4) . . ?
C9 C8 H8 108.1 . . ?
C10 C8 H8 108.1 . . ?
C3 C8 H8 108.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C13 111.0(3) . . ?
C7 C11 C12 111.2(3) . . ?
C13 C11 C12 110.8(4) . . ?
C7 C11 H11 107.9 . . ?
C13 C11 H11 107.9 . . ?
C12 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 122.6(3) . . ?
C15 C14 N2 118.4(3) . . ?
C19 C14 N2 118.9(3) . . ?
C14 C15 C16 116.9(4) . . ?
C14 C15 C20 122.8(3) . . ?
C16 C15 C20 120.3(4) . . ?
C17 C16 C15 121.9(4) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 121.0(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 117.3(4) . . ?
C18 C19 C23 120.1(4) . . ?
C14 C19 C23 122.6(3) . . ?
C21 C20 C22 110.8(5) . . ?
C21 C20 C15 111.8(4) . . ?
C22 C20 C15 111.9(4) . . ?
C21 C20 H20 107.4 . . ?
C22 C20 H20 107.4 . . ?
C15 C20 H20 107.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C24 109.8(5) . . ?
C25 C23 C19 111.2(4) . . ?
C24 C23 C19 112.4(4) . . ?
C25 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C19 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 N1 C2 115.4(3) . . ?
C1 N1 Pd1 122.1(2) . . ?
C2 N1 Pd1 122.5(2) . . ?
C1 N2 C14 122.9(3) . . ?
C1 N2 H2 118.5 . . ?
C14 N2 H2 118.5 . . ?
N1 Pd1 N1 180.00(13) 2_775 . ?
N1 Pd1 Cl1 88.79(8) 2_775 2_775 ?
N1 Pd1 Cl1 91.21(8) . 2_775 ?
N1 Pd1 Cl1 91.21(8) 2_775 . ?
N1 Pd1 Cl1 88.79(8) . . ?
Cl1 Pd1 Cl1 180.0 2_775 . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 362 83 ' '
_platon_squeeze_details          
;
;

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 -1.4(5) . . . . ?
N1 C2 C3 C4 176.5(3) . . . . ?
C7 C2 C3 C8 179.3(4) . . . . ?
N1 C2 C3 C8 -2.8(5) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C8 C3 C4 C5 179.0(4) . . . . ?
C3 C4 C5 C6 0.6(8) . . . . ?
C4 C5 C6 C7 0.8(7) . . . . ?
C5 C6 C7 C2 -2.4(6) . . . . ?
C5 C6 C7 C11 177.8(4) . . . . ?
C3 C2 C7 C6 2.7(5) . . . . ?
N1 C2 C7 C6 -175.2(3) . . . . ?
C3 C2 C7 C11 -177.5(3) . . . . ?
N1 C2 C7 C11 4.6(5) . . . . ?
C4 C3 C8 C9 73.3(6) . . . . ?
C2 C3 C8 C9 -107.4(5) . . . . ?
C4 C3 C8 C10 -49.7(6) . . . . ?
C2 C3 C8 C10 129.6(5) . . . . ?
C6 C7 C11 C13 -53.8(5) . . . . ?
C2 C7 C11 C13 126.4(4) . . . . ?
C6 C7 C11 C12 69.9(5) . . . . ?
C2 C7 C11 C12 -109.9(4) . . . . ?
C19 C14 C15 C16 0.4(6) . . . . ?
N2 C14 C15 C16 -178.6(3) . . . . ?
C19 C14 C15 C20 -179.9(4) . . . . ?
N2 C14 C15 C20 1.0(5) . . . . ?
C14 C15 C16 C17 -0.1(7) . . . . ?
C20 C15 C16 C17 -179.8(4) . . . . ?
C15 C16 C17 C18 -0.3(8) . . . . ?
C16 C17 C18 C19 0.4(7) . . . . ?
C17 C18 C19 C14 -0.1(6) . . . . ?
C17 C18 C19 C23 179.7(4) . . . . ?
C15 C14 C19 C18 -0.3(6) . . . . ?
N2 C14 C19 C18 178.7(3) . . . . ?
C15 C14 C19 C23 179.9(4) . . . . ?
N2 C14 C19 C23 -1.0(5) . . . . ?
C14 C15 C20 C21 123.3(5) . . . . ?
C16 C15 C20 C21 -57.0(6) . . . . ?
C14 C15 C20 C22 -111.8(5) . . . . ?
C16 C15 C20 C22 67.9(6) . . . . ?
C18 C19 C23 C25 70.1(5) . . . . ?
C14 C19 C23 C25 -110.1(5) . . . . ?
C18 C19 C23 C24 -53.4(6) . . . . ?
C14 C19 C23 C24 126.3(5) . . . . ?
N2 C1 N1 C2 -179.9(3) . . . . ?
N2 C1 N1 Pd1 -1.7(5) . . . . ?
C7 C2 N1 C1 70.9(4) . . . . ?
C3 C2 N1 C1 -107.1(4) . . . . ?
C7 C2 N1 Pd1 -107.3(3) . . . . ?
C3 C2 N1 Pd1 74.7(3) . . . . ?
N1 C1 N2 C14 -170.5(3) . . . . ?
C15 C14 N2 C1 -103.5(4) . . . . ?
C19 C14 N2 C1 77.4(4) . . . . ?
C1 N1 Pd1 N1 -39(42) . . . 2_775 ?
C2 N1 Pd1 N1 140(42) . . . 2_775 ?
C1 N1 Pd1 Cl1 57.5(2) . . . 2_775 ?
C2 N1 Pd1 Cl1 -124.4(2) . . . 2_775 ?
C1 N1 Pd1 Cl1 -122.5(2) . . . . ?
C2 N1 Pd1 Cl1 55.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.087
_database_code_depnum_ccdc_archive 'CCDC 1014318'
#######################################################################
#
#                 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_Compound-7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H78 N6 Pd, 2(B F4)'
_chemical_formula_sum            'C54 H78 B2 F8 N6 Pd'
_chemical_formula_weight         1091.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_HALL  '-P 2yn'

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                   11.3947(6)
_cell_length_b                   12.3625(6)
_cell_length_c                   19.4057(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3820(10)
_cell_angle_gamma                90.00
_cell_volume                     2704.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.33

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20061
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5301
_reflns_number_gt                4477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.0261P)²+2.4908P] 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         5301
_refine_ls_number_parameters     331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
B1 B 0.9803(2) 0.3462(2) 0.86212(14) 0.0282(6) Uani 1 1 d . . .
C1 C 0.78118(17) 0.12291(15) 0.00860(10) 0.0121(4) Uani 1 1 d . . .
H1 H 0.6989 0.1276 -0.0003 0.014 Uiso 1 1 calc R . .
C2 C 0.74548(17) -0.02852(15) -0.06153(10) 0.0131(4) Uani 1 1 d . . .
C3 C 0.68846(18) -0.11153(16) -0.03006(11) 0.0168(4) Uani 1 1 d . . .
C4 C 0.61839(19) -0.18240(17) -0.07416(12) 0.0227(5) Uani 1 1 d . . .
H4 H 0.5783 -0.2379 -0.0551 0.027 Uiso 1 1 calc R . .
C5 C 0.6074(2) -0.17193(19) -0.14541(12) 0.0274(5) Uani 1 1 d . . .
H5 H 0.5616 -0.2212 -0.1739 0.033 Uiso 1 1 calc R . .
C6 C 0.6637(2) -0.08907(19) -0.17469(12) 0.0258(5) Uani 1 1 d . . .
H6 H 0.6545 -0.0826 -0.2229 0.031 Uiso 1 1 calc R . .
C7 C 0.73412(18) -0.01485(16) -0.13394(10) 0.0178(4) Uani 1 1 d . . .
C8 C 0.6989(2) -0.12482(17) 0.04851(11) 0.0229(5) Uani 1 1 d . . .
H8 H 0.7642 -0.0789 0.0701 0.027 Uiso 1 1 calc R . .
C9 C 0.5858(3) -0.0879(2) 0.07441(14) 0.0402(7) Uani 1 1 d . . .
H9A H 0.5730 -0.0124 0.0641 0.060 Uiso 1 1 calc R . .
H9B H 0.5931 -0.0989 0.1238 0.060 Uiso 1 1 calc R . .
H9C H 0.5198 -0.1289 0.0516 0.060 Uiso 1 1 calc R . .
C10 C 0.7267(2) -0.2416(2) 0.07128(14) 0.0371(6) Uani 1 1 d . . .
H10A H 0.7431 -0.2449 0.1212 0.056 Uiso 1 1 calc R . .
H10B H 0.7947 -0.2664 0.0519 0.056 Uiso 1 1 calc R . .
H10C H 0.6598 -0.2867 0.0551 0.056 Uiso 1 1 calc R . .
C11 C 0.7967(2) 0.07485(18) -0.16809(11) 0.0231(5) Uani 1 1 d . . .
H11 H 0.8312 0.1251 -0.1317 0.028 Uiso 1 1 calc R . .
C12 C 0.7094(2) 0.1379(2) -0.22080(13) 0.0362(6) Uani 1 1 d . . .
H12A H 0.6794 0.0914 -0.2589 0.054 Uiso 1 1 calc R . .
H12B H 0.7493 0.1984 -0.2379 0.054 Uiso 1 1 calc R . .
H12C H 0.6447 0.1634 -0.1986 0.054 Uiso 1 1 calc R . .
C13 C 0.8970(2) 0.0289(2) -0.20360(14) 0.0340(6) Uani 1 1 d . . .
H13A H 0.9528 -0.0081 -0.1698 0.051 Uiso 1 1 calc R . .
H13B H 0.9364 0.0869 -0.2239 0.051 Uiso 1 1 calc R . .
H13C H 0.8649 -0.0209 -0.2394 0.051 Uiso 1 1 calc R . .
C14 C 0.75904(17) 0.27523(15) 0.08099(10) 0.0129(4) Uani 1 1 d . . .
C15 C 0.70541(18) 0.36231(16) 0.04254(11) 0.0159(4) Uani 1 1 d . . .
C16 C 0.62763(19) 0.42500(16) 0.07492(11) 0.0199(5) Uani 1 1 d . . .
H16 H 0.5896 0.4835 0.0512 0.024 Uiso 1 1 calc R . .
C17 C 0.60598(19) 0.40196(17) 0.14150(11) 0.0212(5) Uani 1 1 d . . .
H17 H 0.5533 0.4447 0.1619 0.025 Uiso 1 1 calc R . .
C18 C 0.66158(19) 0.31627(17) 0.17812(11) 0.0188(4) Uani 1 1 d . . .
H18 H 0.6470 0.3027 0.2233 0.023 Uiso 1 1 calc R . .
C19 C 0.73921(17) 0.24966(16) 0.14860(10) 0.0154(4) Uani 1 1 d . . .
C20 C 0.72863(19) 0.38832(17) -0.03068(11) 0.0186(4) Uani 1 1 d . . .
H20 H 0.8012 0.3504 -0.0383 0.022 Uiso 1 1 calc R . .
C21 C 0.6281(2) 0.34859(18) -0.08537(11) 0.0232(5) Uani 1 1 d . . .
H21A H 0.6197 0.2717 -0.0812 0.035 Uiso 1 1 calc R . .
H21B H 0.6458 0.3657 -0.1310 0.035 Uiso 1 1 calc R . .
H21C H 0.5554 0.3834 -0.0784 0.035 Uiso 1 1 calc R . .
C22 C 0.7484(2) 0.50905(18) -0.04056(12) 0.0304(5) Uani 1 1 d . . .
H22A H 0.6756 0.5473 -0.0387 0.046 Uiso 1 1 calc R . .
H22B H 0.7738 0.5210 -0.0850 0.046 Uiso 1 1 calc R . .
H22C H 0.8082 0.5347 -0.0042 0.046 Uiso 1 1 calc R . .
C23 C 0.79926(19) 0.15514(17) 0.18989(11) 0.0202(5) Uani 1 1 d . . .
H23 H 0.8340 0.1086 0.1574 0.024 Uiso 1 1 calc R . .
C24 C 0.8994(2) 0.1938(2) 0.24499(14) 0.0378(6) Uani 1 1 d . . .
H24A H 0.9582 0.2304 0.2228 0.057 Uiso 1 1 calc R . .
H24B H 0.9349 0.1328 0.2706 0.057 Uiso 1 1 calc R . .
H24C H 0.8683 0.2427 0.2763 0.057 Uiso 1 1 calc R . .
C25 C 0.7109(2) 0.0873(2) 0.22338(14) 0.0340(6) Uani 1 1 d . . .
H25A H 0.6848 0.1274 0.2607 0.051 Uiso 1 1 calc R . .
H25B H 0.7485 0.0216 0.2414 0.051 Uiso 1 1 calc R . .
H25C H 0.6439 0.0702 0.1891 0.051 Uiso 1 1 calc R . .
C26 C 0.95981(17) 0.21856(15) 0.06041(9) 0.0124(4) Uani 1 1 d . . .
C27 C 1.00441(18) 0.32517(16) 0.08936(11) 0.0174(4) Uani 1 1 d . . .
H27A H 1.0885 0.3211 0.1037 0.026 Uiso 1 1 calc R . .
H27B H 0.9660 0.3431 0.1287 0.026 Uiso 1 1 calc R . .
H27C H 0.9874 0.3799 0.0543 0.026 Uiso 1 1 calc R . .
F1 F 1.05671(19) 0.43057(13) 0.87525(11) 0.0658(5) Uani 1 1 d . . .
F2 F 0.86660(16) 0.3815(2) 0.83953(8) 0.0759(7) Uani 1 1 d . . .
F3 F 1.01744(14) 0.28041(12) 0.81232(7) 0.0411(4) Uani 1 1 d . . .
F4 F 0.97908(15) 0.28727(16) 0.92297(8) 0.0531(5) Uani 1 1 d . . .
N1 N 0.82751(14) 0.04139(13) -0.01787(8) 0.0111(3) Uani 1 1 d . . .
N2 N 0.83776(14) 0.20405(12) 0.04831(8) 0.0120(3) Uani 1 1 d . . .
N3 N 1.02947(14) 0.14407(12) 0.04518(8) 0.0125(3) Uani 1 1 d . . .
H3 H 1.1034 0.1591 0.0567 0.015 Uiso 1 1 calc R . .
Pd1 Pd 1.0000 0.0000 0.0000 0.00936(6) Uani 1 2 d S . .


_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
B1 F1 1.359(3) . ?
B1 F3 1.376(3) . ?
B1 F2 1.376(3) . ?
B1 F4 1.389(3) . ?
C1 N1 1.280(2) . ?
C1 N2 1.368(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.401(3) . ?
C2 C7 1.402(3) . ?
C2 N1 1.452(2) . ?
C3 C4 1.392(3) . ?
C3 C8 1.521(3) . ?
C4 C5 1.376(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(3) . ?
C6 H6 0.9300 . ?
C7 C11 1.521(3) . ?
C8 C9 1.521(3) . ?
C8 C10 1.529(3) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.528(3) . ?
C11 C12 1.532(3) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.399(3) . ?
C14 C19 1.400(3) . ?
C14 N2 1.465(2) . ?
C15 C16 1.394(3) . ?
C15 C20 1.517(3) . ?
C16 C17 1.380(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.392(3) . ?
C18 H18 0.9300 . ?
C19 C23 1.522(3) . ?
C20 C21 1.525(3) . ?
C20 C22 1.526(3) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.523(3) . ?
C23 C25 1.526(3) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N3 1.278(2) . ?
C26 N2 1.388(2) . ?
C26 C27 1.493(3) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N1 Pd1 2.0116(16) . ?
N3 Pd1 1.9920(15) . ?
N3 H3 0.8600 . ?
Pd1 N3 1.9920(15) 3_755 ?
Pd1 N1 2.0116(16) 3_755 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 B1 F3 109.3(2) . . ?
F1 B1 F2 111.4(2) . . ?
F3 B1 F2 109.6(2) . . ?
F1 B1 F4 109.2(2) . . ?
F3 B1 F4 109.2(2) . . ?
F2 B1 F4 108.1(2) . . ?
N1 C1 N2 127.99(18) . . ?
N1 C1 H1 116.0 . . ?
N2 C1 H1 116.0 . . ?
C3 C2 C7 122.95(18) . . ?
C3 C2 N1 118.80(17) . . ?
C7 C2 N1 118.06(17) . . ?
C4 C3 C2 116.99(19) . . ?
C4 C3 C8 120.16(19) . . ?
C2 C3 C8 122.84(18) . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 121.5(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C2 116.91(19) . . ?
C6 C7 C11 120.14(19) . . ?
C2 C7 C11 122.94(18) . . ?
C9 C8 C3 110.64(19) . . ?
C9 C8 C10 109.75(19) . . ?
C3 C8 C10 111.99(19) . . ?
C9 C8 H8 108.1 . . ?
C3 C8 H8 108.1 . . ?
C10 C8 H8 108.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C13 110.77(18) . . ?
C7 C11 C12 111.2(2) . . ?
C13 C11 C12 110.11(19) . . ?
C7 C11 H11 108.2 . . ?
C13 C11 H11 108.2 . . ?
C12 C11 H11 108.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 123.79(18) . . ?
C15 C14 N2 118.61(17) . . ?
C19 C14 N2 117.57(17) . . ?
C16 C15 C14 116.39(18) . . ?
C16 C15 C20 120.89(18) . . ?
C14 C15 C20 122.72(17) . . ?
C17 C16 C15 121.3(2) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C16 120.68(19) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.99(19) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C14 116.84(18) . . ?
C18 C19 C23 120.11(18) . . ?
C14 C19 C23 123.05(17) . . ?
C15 C20 C21 111.56(17) . . ?
C15 C20 C22 111.97(18) . . ?
C21 C20 C22 109.71(18) . . ?
C15 C20 H20 107.8 . . ?
C21 C20 H20 107.8 . . ?
C22 C20 H20 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C24 111.21(18) . . ?
C19 C23 C25 111.87(18) . . ?
C24 C23 C25 110.29(19) . . ?
C19 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 120.56(17) . . ?
N3 C26 C27 122.30(18) . . ?
N2 C26 C27 117.10(16) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 N1 C2 115.78(16) . . ?
C1 N1 Pd1 125.53(14) . . ?
C2 N1 Pd1 118.62(12) . . ?
C1 N2 C26 124.65(16) . . ?
C1 N2 C14 114.60(15) . . ?
C26 N2 C14 120.71(15) . . ?
C26 N3 Pd1 132.49(14) . . ?
C26 N3 H3 113.8 . . ?
Pd1 N3 H3 113.8 . . ?
N3 Pd1 N3 179.999(2) 3_755 . ?
N3 Pd1 N1 93.08(6) 3_755 . ?
N3 Pd1 N1 86.92(6) . . ?
N3 Pd1 N1 86.92(6) 3_755 3_755 ?
N3 Pd1 N1 93.09(6) . 3_755 ?
N1 Pd1 N1 180.0 . 3_755 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 0.2(3) . . . . ?
N1 C2 C3 C4 -174.68(18) . . . . ?
C7 C2 C3 C8 -178.74(19) . . . . ?
N1 C2 C3 C8 6.4(3) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C8 C3 C4 C5 179.9(2) . . . . ?
C3 C4 C5 C6 -1.5(3) . . . . ?
C4 C5 C6 C7 0.9(4) . . . . ?
C5 C6 C7 C2 0.2(3) . . . . ?
C5 C6 C7 C11 179.1(2) . . . . ?
C3 C2 C7 C6 -0.8(3) . . . . ?
N1 C2 C7 C6 174.15(18) . . . . ?
C3 C2 C7 C11 -179.60(19) . . . . ?
N1 C2 C7 C11 -4.7(3) . . . . ?
C4 C3 C8 C9 -74.0(3) . . . . ?
C2 C3 C8 C9 104.9(2) . . . . ?
C4 C3 C8 C10 48.8(3) . . . . ?
C2 C3 C8 C10 -132.3(2) . . . . ?
C6 C7 C11 C13 -70.3(3) . . . . ?
C2 C7 C11 C13 108.5(2) . . . . ?
C6 C7 C11 C12 52.5(3) . . . . ?
C2 C7 C11 C12 -128.7(2) . . . . ?
C19 C14 C15 C16 -0.5(3) . . . . ?
N2 C14 C15 C16 177.50(18) . . . . ?
C19 C14 C15 C20 179.91(19) . . . . ?
N2 C14 C15 C20 -2.1(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C20 C15 C16 C17 -179.99(19) . . . . ?
C15 C16 C17 C18 0.4(3) . . . . ?
C16 C17 C18 C19 -1.2(3) . . . . ?
C17 C18 C19 C14 1.0(3) . . . . ?
C17 C18 C19 C23 -179.73(19) . . . . ?
C15 C14 C19 C18 -0.2(3) . . . . ?
N2 C14 C19 C18 -178.21(17) . . . . ?
C15 C14 C19 C23 -179.44(19) . . . . ?
N2 C14 C19 C23 2.6(3) . . . . ?
C16 C15 C20 C21 -78.5(2) . . . . ?
C14 C15 C20 C21 101.1(2) . . . . ?
C16 C15 C20 C22 44.9(3) . . . . ?
C14 C15 C20 C22 -135.5(2) . . . . ?
C18 C19 C23 C24 -75.6(3) . . . . ?
C14 C19 C23 C24 103.6(2) . . . . ?
C18 C19 C23 C25 48.2(3) . . . . ?
C14 C19 C23 C25 -132.6(2) . . . . ?
N2 C1 N1 C2 -176.33(18) . . . . ?
N2 C1 N1 Pd1 6.9(3) . . . . ?
C3 C2 N1 C1 -86.2(2) . . . . ?
C7 C2 N1 C1 98.6(2) . . . . ?
C3 C2 N1 Pd1 90.85(18) . . . . ?
C7 C2 N1 Pd1 -84.31(19) . . . . ?
N1 C1 N2 C26 7.9(3) . . . . ?
N1 C1 N2 C14 -169.68(18) . . . . ?
N3 C26 N2 C1 -13.0(3) . . . . ?
C27 C26 N2 C1 164.98(17) . . . . ?
N3 C26 N2 C14 164.40(17) . . . . ?
C27 C26 N2 C14 -17.6(3) . . . . ?
C15 C14 N2 C1 -85.0(2) . . . . ?
C19 C14 N2 C1 93.0(2) . . . . ?
C15 C14 N2 C26 97.3(2) . . . . ?
C19 C14 N2 C26 -84.7(2) . . . . ?
N2 C26 N3 Pd1 3.3(3) . . . . ?
C27 C26 N3 Pd1 -174.67(14) . . . . ?
C26 N3 Pd1 N3 74(34) . . . 3_755 ?
C26 N3 Pd1 N1 6.82(18) . . . . ?
C26 N3 Pd1 N1 -173.18(18) . . . 3_755 ?
C1 N1 Pd1 N3 168.63(16) . . . 3_755 ?
C2 N1 Pd1 N3 -8.10(14) . . . 3_755 ?
C1 N1 Pd1 N3 -11.37(16) . . . . ?
C2 N1 Pd1 N3 171.90(14) . . . . ?
C1 N1 Pd1 N1 127.33(16) . . . 3_755 ?
C2 N1 Pd1 N1 -49.40(13) . . . 3_755 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 1020744'
#######################################################################
#
#                 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_Compound-8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H82 N6 Pd, 2(B F4)'
_chemical_formula_sum            'C56 H82 B2 F8 N6 Pd'
_chemical_formula_weight         1119.30

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_HALL  '-P 2yn'

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                   11.417(5)
_cell_length_b                   12.755(5)
_cell_length_c                   19.529(5)
_cell_angle_alpha                90.000(0)
_cell_angle_beta                 97.614(0)
_cell_angle_gamma                90.000(0)
_cell_volume                     2818.8(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    5698
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      28.30

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16405
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5525
_reflns_number_gt                3886
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.0416P)²+1.6438P] 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         5525
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
B1 B 0.9713(4) 0.3543(4) 0.8644(2) 0.0377(11) Uani 1 1 d . . .
C1 C 0.7800(3) 0.1140(2) 0.01470(14) 0.0171(7) Uani 1 1 d . . .
H1 H 0.6980 0.1175 0.0070 0.021 Uiso 1 1 calc R . .
C2 C 0.7454(3) -0.0283(2) -0.05849(16) 0.0187(8) Uani 1 1 d . . .
C3 C 0.6867(3) -0.1088(3) -0.02900(17) 0.0243(8) Uani 1 1 d . . .
C4 C 0.6127(3) -0.1714(3) -0.07438(19) 0.0313(9) Uani 1 1 d . . .
H4 H 0.5700 -0.2250 -0.0569 0.038 Uiso 1 1 calc R . .
C5 C 0.6016(3) -0.1554(3) -0.1445(2) 0.0367(10) Uani 1 1 d . . .
H5 H 0.5524 -0.1990 -0.1737 0.044 Uiso 1 1 calc R . .
C6 C 0.6612(3) -0.0770(3) -0.17167(18) 0.0330(9) Uani 1 1 d . . .
H6 H 0.6521 -0.0677 -0.2193 0.040 Uiso 1 1 calc R . .
C7 C 0.7356(3) -0.0105(3) -0.12976(16) 0.0248(8) Uani 1 1 d . . .
C8 C 0.6988(3) -0.1275(3) 0.04814(17) 0.0314(9) Uani 1 1 d . . .
H8 H 0.7634 -0.0831 0.0699 0.038 Uiso 1 1 calc R . .
C9 C 0.5855(4) -0.0937(3) 0.0763(2) 0.0570(13) Uani 1 1 d . . .
H9A H 0.5727 -0.0201 0.0683 0.086 Uiso 1 1 calc R . .
H9B H 0.5932 -0.1075 0.1250 0.086 Uiso 1 1 calc R . .
H9C H 0.5196 -0.1324 0.0532 0.086 Uiso 1 1 calc R . .
C10 C 0.7302(4) -0.2409(3) 0.0670(2) 0.0423(11) Uani 1 1 d . . .
H10A H 0.6675 -0.2861 0.0471 0.063 Uiso 1 1 calc R . .
H10B H 0.7408 -0.2485 0.1163 0.063 Uiso 1 1 calc R . .
H10C H 0.8021 -0.2595 0.0494 0.063 Uiso 1 1 calc R . .
C11 C 0.7984(3) 0.0785(3) -0.16095(16) 0.0320(9) Uani 1 1 d . . .
H11 H 0.8487 0.1142 -0.1235 0.038 Uiso 1 1 calc R . .
C12 C 0.7091(4) 0.1569(3) -0.1942(2) 0.0589(13) Uani 1 1 d . . .
H12A H 0.7495 0.2133 -0.2137 0.088 Uiso 1 1 calc R . .
H12B H 0.6641 0.1842 -0.1600 0.088 Uiso 1 1 calc R . .
H12C H 0.6569 0.1230 -0.2301 0.088 Uiso 1 1 calc R . .
C13 C 0.8761(4) 0.0403(4) -0.2125(2) 0.0565(13) Uani 1 1 d . . .
H13A H 0.9330 -0.0086 -0.1905 0.085 Uiso 1 1 calc R . .
H13B H 0.9164 0.0988 -0.2297 0.085 Uiso 1 1 calc R . .
H13C H 0.8283 0.0064 -0.2502 0.085 Uiso 1 1 calc R . .
C14 C 0.7567(3) 0.2570(3) 0.09035(16) 0.0209(8) Uani 1 1 d . . .
C15 C 0.7395(3) 0.2290(3) 0.15764(16) 0.0231(8) Uani 1 1 d . . .
C16 C 0.6638(3) 0.2913(3) 0.18996(18) 0.0314(9) Uani 1 1 d . . .
H16 H 0.6512 0.2762 0.2350 0.038 Uiso 1 1 calc R . .
C17 C 0.6074(3) 0.3748(3) 0.1561(2) 0.0396(10) Uani 1 1 d . . .
H17 H 0.5556 0.4149 0.1782 0.048 Uiso 1 1 calc R . .
C18 C 0.6258(3) 0.4002(3) 0.0903(2) 0.0369(10) Uani 1 1 d . . .
H18 H 0.5868 0.4577 0.0687 0.044 Uiso 1 1 calc R . .
C19 C 0.7016(3) 0.3420(3) 0.05514(18) 0.0273(8) Uani 1 1 d . . .
C20 C 0.7991(3) 0.1364(3) 0.19601(16) 0.0267(8) Uani 1 1 d . . .
H20 H 0.8344 0.0933 0.1626 0.032 Uiso 1 1 calc R . .
C21 C 0.8986(3) 0.1724(4) 0.25131(19) 0.0482(12) Uani 1 1 d . . .
H21A H 0.9586 0.2071 0.2296 0.072 Uiso 1 1 calc R . .
H21B H 0.9323 0.1127 0.2766 0.072 Uiso 1 1 calc R . .
H21C H 0.8674 0.2200 0.2824 0.072 Uiso 1 1 calc R . .
C22 C 0.7117(4) 0.0685(3) 0.2282(2) 0.0498(12) Uani 1 1 d . . .
H22A H 0.6871 0.1043 0.2671 0.075 Uiso 1 1 calc R . .
H22B H 0.7488 0.0033 0.2432 0.075 Uiso 1 1 calc R . .
H22C H 0.6442 0.0548 0.1946 0.075 Uiso 1 1 calc R . .
C23 C 0.7221(3) 0.3734(3) -0.01734(18) 0.0333(9) Uani 1 1 d . . .
H23 H 0.7857 0.3294 -0.0307 0.040 Uiso 1 1 calc R . .
C24 C 0.7615(5) 0.4872(3) -0.0194(2) 0.0608(14) Uani 1 1 d . . .
H24A H 0.6970 0.5324 -0.0121 0.091 Uiso 1 1 calc R . .
H24B H 0.7857 0.5021 -0.0637 0.091 Uiso 1 1 calc R . .
H24C H 0.8266 0.4990 0.0162 0.091 Uiso 1 1 calc R . .
C25 C 0.6121(4) 0.3548(4) -0.0692(2) 0.0550(13) Uani 1 1 d . . .
H25A H 0.5948 0.2811 -0.0717 0.082 Uiso 1 1 calc R . .
H25B H 0.6258 0.3795 -0.1139 0.082 Uiso 1 1 calc R . .
H25C H 0.5465 0.3919 -0.0547 0.082 Uiso 1 1 calc R . .
C26 C 0.9564(3) 0.2076(2) 0.06553(14) 0.0175(7) Uani 1 1 d . . .
C27 C 0.9983(3) 0.3100(2) 0.09632(16) 0.0223(8) Uani 1 1 d . . .
H27A H 0.9574 0.3240 0.1358 0.027 Uiso 1 1 calc R . .
H27B H 0.9769 0.3649 0.0626 0.027 Uiso 1 1 calc R . .
C28 C 1.1295(3) 0.3151(3) 0.11920(19) 0.0340(9) Uani 1 1 d . . .
H28A H 1.1522 0.2592 0.1511 0.051 Uiso 1 1 calc R . .
H28B H 1.1489 0.3812 0.1413 0.051 Uiso 1 1 calc R . .
H28C H 1.1708 0.3082 0.0797 0.051 Uiso 1 1 calc R . .
F1 F 1.0084(2) 0.28833(19) 0.81532(10) 0.0482(6) Uani 1 1 d . . .
F2 F 0.9708(2) 0.2991(2) 0.92579(10) 0.0533(7) Uani 1 1 d . . .
F3 F 0.8573(2) 0.3884(2) 0.84206(11) 0.0603(8) Uani 1 1 d . . .
F4 F 1.0448(3) 0.4377(2) 0.87499(14) 0.0724(8) Uani 1 1 d . . .
N1 N 0.8274(2) 0.0371(2) -0.01397(12) 0.0155(6) Uani 1 1 d . . .
N2 N 0.8352(2) 0.19098(19) 0.05500(12) 0.0165(6) Uani 1 1 d . . .
N3 N 1.0263(2) 0.13784(19) 0.04664(11) 0.0154(6) Uani 1 1 d . . .
H3 H 1.0998 0.1541 0.0561 0.018 Uiso 1 1 calc R . .
Pd1 Pd 1.0000 0.0000 0.0000 0.01309(10) Uani 1 2 d S . .


_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
B1 F4 1.354(5) . ?
B1 F1 1.383(5) . ?
B1 F3 1.386(5) . ?
B1 F2 1.391(5) . ?
C1 N1 1.284(4) . ?
C1 N2 1.360(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.392(4) . ?
C2 C7 1.400(4) . ?
C2 N1 1.454(4) . ?
C3 C4 1.392(5) . ?
C3 C8 1.513(4) . ?
C4 C5 1.373(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.358(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(5) . ?
C6 H6 0.9300 . ?
C7 C11 1.513(5) . ?
C8 C10 1.524(5) . ?
C8 C9 1.533(5) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.509(5) . ?
C11 C12 1.512(5) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C19 1.389(5) . ?
C14 C15 1.400(4) . ?
C14 N2 1.468(4) . ?
C15 C16 1.385(5) . ?
C15 C20 1.512(5) . ?
C16 C17 1.369(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.367(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(5) . ?
C18 H18 0.9300 . ?
C19 C23 1.519(5) . ?
C20 C22 1.518(5) . ?
C20 C21 1.531(5) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.522(5) . ?
C23 C25 1.524(5) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N3 1.282(4) . ?
C26 N2 1.388(4) . ?
C26 C27 1.490(4) . ?
C27 C28 1.507(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
N1 Pd1 2.009(3) . ?
N3 Pd1 1.985(2) . ?
N3 H3 0.8600 . ?
Pd1 N3 1.985(2) 3_755 ?
Pd1 N1 2.009(3) 3_755 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F4 B1 F1 110.0(4) . . ?
F4 B1 F3 109.7(4) . . ?
F1 B1 F3 109.5(3) . . ?
F4 B1 F2 109.9(4) . . ?
F1 B1 F2 109.0(4) . . ?
F3 B1 F2 108.6(4) . . ?
N1 C1 N2 127.9(3) . . ?
N1 C1 H1 116.0 . . ?
N2 C1 H1 116.0 . . ?
C3 C2 C7 123.5(3) . . ?
C3 C2 N1 118.9(3) . . ?
C7 C2 N1 117.5(3) . . ?
C2 C3 C4 116.4(3) . . ?
C2 C3 C8 122.9(3) . . ?
C4 C3 C8 120.7(3) . . ?
C5 C4 C3 121.2(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C2 116.7(3) . . ?
C6 C7 C11 120.4(3) . . ?
C2 C7 C11 122.9(3) . . ?
C3 C8 C10 112.2(3) . . ?
C3 C8 C9 110.0(3) . . ?
C10 C8 C9 111.3(3) . . ?
C3 C8 H8 107.7 . . ?
C10 C8 H8 107.7 . . ?
C9 C8 H8 107.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 110.4(3) . . ?
C13 C11 C7 112.2(3) . . ?
C12 C11 C7 109.9(3) . . ?
C13 C11 H11 108.0 . . ?
C12 C11 H11 108.0 . . ?
C7 C11 H11 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 123.6(3) . . ?
C19 C14 N2 118.7(3) . . ?
C15 C14 N2 117.8(3) . . ?
C16 C15 C14 117.1(3) . . ?
C16 C15 C20 119.3(3) . . ?
C14 C15 C20 123.6(3) . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 121.2(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 121.4(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C14 C19 C18 116.3(3) . . ?
C14 C19 C23 123.5(3) . . ?
C18 C19 C23 120.2(3) . . ?
C15 C20 C22 111.9(3) . . ?
C15 C20 C21 111.0(3) . . ?
C22 C20 C21 110.3(3) . . ?
C15 C20 H20 107.8 . . ?
C22 C20 H20 107.8 . . ?
C21 C20 H20 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C24 111.1(3) . . ?
C19 C23 C25 111.3(3) . . ?
C24 C23 C25 110.6(3) . . ?
C19 C23 H23 107.9 . . ?
C24 C23 H23 107.9 . . ?
C25 C23 H23 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 119.9(3) . . ?
N3 C26 C27 123.1(3) . . ?
N2 C26 C27 117.0(3) . . ?
C26 C27 C28 114.3(3) . . ?
C26 C27 H27A 108.7 . . ?
C28 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
C28 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C1 N1 C2 115.1(3) . . ?
C1 N1 Pd1 125.6(2) . . ?
C2 N1 Pd1 119.27(19) . . ?
C1 N2 C26 124.9(3) . . ?
C1 N2 C14 114.9(3) . . ?
C26 N2 C14 120.1(3) . . ?
C26 N3 Pd1 133.2(2) . . ?
C26 N3 H3 113.4 . . ?
Pd1 N3 H3 113.4 . . ?
N3 Pd1 N3 180.0 3_755 . ?
N3 Pd1 N1 86.57(10) 3_755 3_755 ?
N3 Pd1 N1 93.43(10) . 3_755 ?
N3 Pd1 N1 93.44(10) 3_755 . ?
N3 Pd1 N1 86.56(10) . . ?
N1 Pd1 N1 180.0 3_755 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 -1.8(5) . . . . ?
N1 C2 C3 C4 -177.6(3) . . . . ?
C7 C2 C3 C8 179.6(3) . . . . ?
N1 C2 C3 C8 3.8(5) . . . . ?
C2 C3 C4 C5 1.7(5) . . . . ?
C8 C3 C4 C5 -179.6(3) . . . . ?
C3 C4 C5 C6 -0.9(6) . . . . ?
C4 C5 C6 C7 0.2(6) . . . . ?
C5 C6 C7 C2 -0.2(5) . . . . ?
C5 C6 C7 C11 -178.1(4) . . . . ?
C3 C2 C7 C6 1.1(5) . . . . ?
N1 C2 C7 C6 176.9(3) . . . . ?
C3 C2 C7 C11 178.9(3) . . . . ?
N1 C2 C7 C11 -5.2(5) . . . . ?
C2 C3 C8 C10 -128.6(4) . . . . ?
C4 C3 C8 C10 52.9(5) . . . . ?
C2 C3 C8 C9 107.0(4) . . . . ?
C4 C3 C8 C9 -71.5(4) . . . . ?
C6 C7 C11 C13 -58.7(5) . . . . ?
C2 C7 C11 C13 123.6(4) . . . . ?
C6 C7 C11 C12 64.6(4) . . . . ?
C2 C7 C11 C12 -113.1(4) . . . . ?
C19 C14 C15 C16 -0.5(5) . . . . ?
N2 C14 C15 C16 -179.1(3) . . . . ?
C19 C14 C15 C20 179.9(3) . . . . ?
N2 C14 C15 C20 1.3(5) . . . . ?
C14 C15 C16 C17 1.3(5) . . . . ?
C20 C15 C16 C17 -179.1(3) . . . . ?
C15 C16 C17 C18 -1.3(6) . . . . ?
C16 C17 C18 C19 0.5(6) . . . . ?
C15 C14 C19 C18 -0.2(5) . . . . ?
N2 C14 C19 C18 178.4(3) . . . . ?
C15 C14 C19 C23 178.8(3) . . . . ?
N2 C14 C19 C23 -2.6(5) . . . . ?
C17 C18 C19 C14 0.2(5) . . . . ?
C17 C18 C19 C23 -178.8(4) . . . . ?
C16 C15 C20 C22 49.3(4) . . . . ?
C14 C15 C20 C22 -131.1(4) . . . . ?
C16 C15 C20 C21 -74.4(4) . . . . ?
C14 C15 C20 C21 105.2(4) . . . . ?
C14 C19 C23 C24 -124.8(4) . . . . ?
C18 C19 C23 C24 54.2(5) . . . . ?
C14 C19 C23 C25 111.5(4) . . . . ?
C18 C19 C23 C25 -69.5(4) . . . . ?
N3 C26 C27 C28 -13.9(4) . . . . ?
N2 C26 C27 C28 168.6(3) . . . . ?
N2 C1 N1 C2 -175.6(3) . . . . ?
N2 C1 N1 Pd1 6.1(4) . . . . ?
C3 C2 N1 C1 -84.6(4) . . . . ?
C7 C2 N1 C1 99.4(3) . . . . ?
C3 C2 N1 Pd1 93.8(3) . . . . ?
C7 C2 N1 Pd1 -82.2(3) . . . . ?
N1 C1 N2 C26 8.6(5) . . . . ?
N1 C1 N2 C14 -169.5(3) . . . . ?
N3 C26 N2 C1 -12.4(4) . . . . ?
C27 C26 N2 C1 165.1(3) . . . . ?
N3 C26 N2 C14 165.6(3) . . . . ?
C27 C26 N2 C14 -16.9(4) . . . . ?
C19 C14 N2 C1 -85.0(4) . . . . ?
C15 C14 N2 C1 93.7(3) . . . . ?
C19 C14 N2 C26 96.8(3) . . . . ?
C15 C14 N2 C26 -84.5(4) . . . . ?
N2 C26 N3 Pd1 1.5(4) . . . . ?
C27 C26 N3 Pd1 -175.9(2) . . . . ?
C26 N3 Pd1 N3 -88(36) . . . 3_755 ?
C26 N3 Pd1 N1 -171.8(3) . . . 3_755 ?
C26 N3 Pd1 N1 8.2(3) . . . . ?
C1 N1 Pd1 N3 168.6(2) . . . 3_755 ?
C2 N1 Pd1 N3 -9.7(2) . . . 3_755 ?
C1 N1 Pd1 N3 -11.4(2) . . . . ?
C2 N1 Pd1 N3 170.3(2) . . . . ?
C1 N1 Pd1 N1 18.9(4) . . . 3_755 ?
C2 N1 Pd1 N1 -159.4(4) . . . 3_755 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1020745'
#######################################################################
#
#                 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_Compound-9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H78 N6 Pd, 2(F6 P)'
_chemical_formula_sum            'C54 H78 F12 N6 P2 Pd'
_chemical_formula_weight         1207.56

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_HALL  '-P 2yn'
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                   10.4943(18)
_cell_length_b                   21.691(4)
_cell_length_c                   12.734(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.428(3)
_cell_angle_gamma                90.00
_cell_volume                     2898.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6385
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.75

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15376
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5342
_reflns_number_gt                4464
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.1231P)²+12.7350P] 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         5342
_refine_ls_number_parameters     349
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0725
_refine_ls_wR_factor_ref         0.2164
_refine_ls_wR_factor_gt          0.2024
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.175
_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
C1 C 0.9276(5) 0.1007(2) 0.6470(4) 0.0190(10) Uani 1 1 d . . .
H1 H 0.9121 0.1433 0.6589 0.023 Uiso 1 1 calc R . .
C2 C 0.9632(5) 0.1339(2) 0.4748(4) 0.0189(10) Uani 1 1 d . . .
C3 C 0.8529(5) 0.1447(2) 0.4138(4) 0.0207(11) Uani 1 1 d . . .
C4 C 0.8660(6) 0.1836(3) 0.3279(4) 0.0270(12) Uani 1 1 d . . .
H4 H 0.7937 0.1924 0.2851 0.032 Uiso 1 1 calc R . .
C5 C 0.9823(6) 0.2097(3) 0.3033(4) 0.0268(12) Uani 1 1 d . . .
H5 H 0.9895 0.2349 0.2426 0.032 Uiso 1 1 calc R . .
C6 C 1.0889(5) 0.1994(2) 0.3669(4) 0.0255(11) Uani 1 1 d . . .
H6 H 1.1675 0.2187 0.3503 0.031 Uiso 1 1 calc R . .
C7 C 1.0812(5) 0.1612(2) 0.4543(4) 0.0218(11) Uani 1 1 d . . .
C8 C 0.7247(5) 0.1158(3) 0.4381(5) 0.0322(13) Uani 1 1 d . . .
H8 H 0.7362 0.0893 0.5018 0.039 Uiso 1 1 calc R . .
C9 C 0.6766(7) 0.0742(4) 0.3488(7) 0.0500(18) Uani 1 1 d . . .
H9A H 0.6646 0.0989 0.2851 0.075 Uiso 1 1 calc R . .
H9B H 0.5953 0.0556 0.3687 0.075 Uiso 1 1 calc R . .
H9C H 0.7392 0.0417 0.3356 0.075 Uiso 1 1 calc R . .
C10 C 0.6267(6) 0.1662(3) 0.4655(6) 0.0426(16) Uani 1 1 d . . .
H10A H 0.6617 0.1929 0.5208 0.064 Uiso 1 1 calc R . .
H10B H 0.5480 0.1469 0.4902 0.064 Uiso 1 1 calc R . .
H10C H 0.6081 0.1910 0.4028 0.064 Uiso 1 1 calc R . .
C11 C 1.1980(5) 0.1492(3) 0.5244(5) 0.0286(12) Uani 1 1 d . . .
H11 H 1.1665 0.1350 0.5942 0.034 Uiso 1 1 calc R . .
C12 C 1.2757(6) 0.2078(3) 0.5425(5) 0.0369(14) Uani 1 1 d . . .
H12A H 1.3421 0.1998 0.5952 0.055 Uiso 1 1 calc R . .
H12B H 1.2195 0.2407 0.5673 0.055 Uiso 1 1 calc R . .
H12C H 1.3153 0.2204 0.4764 0.055 Uiso 1 1 calc R . .
C13 C 1.2830(6) 0.0978(3) 0.4797(6) 0.0420(17) Uani 1 1 d . . .
H13A H 1.2347 0.0591 0.4768 0.063 Uiso 1 1 calc R . .
H13B H 1.3580 0.0924 0.5251 0.063 Uiso 1 1 calc R . .
H13C H 1.3103 0.1091 0.4089 0.063 Uiso 1 1 calc R . .
C14 C 0.8962(5) 0.0916(2) 0.8333(4) 0.0218(11) Uani 1 1 d . . .
C15 C 1.0030(5) 0.1144(2) 0.8864(4) 0.0225(11) Uani 1 1 d . . .
C16 C 0.9826(6) 0.1416(3) 0.9851(4) 0.0292(13) Uani 1 1 d . . .
H16 H 1.0524 0.1581 1.0239 0.035 Uiso 1 1 calc R . .
C17 C 0.8616(6) 0.1442(3) 1.0256(5) 0.0339(14) Uani 1 1 d . . .
H17 H 0.8494 0.1620 1.0929 0.041 Uiso 1 1 calc R . .
C18 C 0.7566(6) 0.1215(3) 0.9705(5) 0.0319(13) Uani 1 1 d . . .
H18 H 0.6742 0.1242 1.0006 0.038 Uiso 1 1 calc R . .
C19 C 0.7711(5) 0.0948(3) 0.8716(4) 0.0261(12) Uani 1 1 d . . .
C20 C 1.1377(5) 0.1104(3) 0.8428(4) 0.0269(12) Uani 1 1 d . . .
H20 H 1.1319 0.0909 0.7718 0.032 Uiso 1 1 calc R . .
C21 C 1.1975(6) 0.1738(3) 0.8293(6) 0.0402(15) Uani 1 1 d . . .
H21A H 1.2019 0.1946 0.8975 0.060 Uiso 1 1 calc R . .
H21B H 1.1455 0.1983 0.7805 0.060 Uiso 1 1 calc R . .
H21C H 1.2836 0.1693 0.8011 0.060 Uiso 1 1 calc R . .
C22 C 1.2225(6) 0.0690(3) 0.9123(5) 0.0385(15) Uani 1 1 d . . .
H22A H 1.2333 0.0880 0.9816 0.058 Uiso 1 1 calc R . .
H22B H 1.3060 0.0640 0.8794 0.058 Uiso 1 1 calc R . .
H22C H 1.1822 0.0285 0.9202 0.058 Uiso 1 1 calc R . .
C23 C 0.6559(5) 0.0712(3) 0.8097(5) 0.0295(13) Uani 1 1 d . . .
H23 H 0.6872 0.0474 0.7478 0.035 Uiso 1 1 calc R . .
C24 C 0.5734(6) 0.0283(3) 0.8773(6) 0.0430(16) Uani 1 1 d . . .
H24A H 0.6243 -0.0073 0.9001 0.065 Uiso 1 1 calc R . .
H24B H 0.5001 0.0139 0.8359 0.065 Uiso 1 1 calc R . .
H24C H 0.5432 0.0508 0.9390 0.065 Uiso 1 1 calc R . .
C25 C 0.5769(6) 0.1261(3) 0.7695(6) 0.0419(16) Uani 1 1 d . . .
H25A H 0.5434 0.1493 0.8293 0.063 Uiso 1 1 calc R . .
H25B H 0.5059 0.1109 0.7262 0.063 Uiso 1 1 calc R . .
H25C H 0.6310 0.1531 0.7272 0.063 Uiso 1 1 calc R . .
C26 C 1.0627(5) 0.0011(2) 0.2703(4) 0.0190(11) Uani 1 1 d . . .
C27 C 1.0814(6) 0.0368(3) 0.1709(4) 0.0303(13) Uani 1 1 d . . .
H27A H 1.0565 0.0798 0.1821 0.045 Uiso 1 1 calc R . .
H27B H 1.0287 0.0189 0.1149 0.045 Uiso 1 1 calc R . .
H27C H 1.1713 0.0350 0.1509 0.045 Uiso 1 1 calc R . .
N1 N 0.9572(4) 0.08515(18) 0.5537(3) 0.0172(9) Uani 1 1 d . . .
N2 N 0.9160(4) 0.06209(19) 0.7319(3) 0.0179(9) Uani 1 1 d . . .
N3 N 1.0275(4) 0.0284(2) 0.3546(3) 0.0231(10) Uani 1 1 d . . .
H3 H 1.0126 0.0680 0.3458 0.028 Uiso 1 1 calc R . .
P1 P 0.40088(16) 0.19255(8) 0.15600(12) 0.0346(4) Uani 1 1 d . . .
Pd1 Pd 1.0000 0.0000 0.5000 0.0166(2) Uani 1 2 d S . .
F1 F 0.2568(5) 0.1800(4) 0.1406(5) 0.098(2) Uani 1 1 d U . .
F5 F 0.3943(5) 0.1973(4) 0.2742(4) 0.104(2) Uani 1 1 d U . .
F4 F 0.5516(6) 0.1913(4) 0.1749(5) 0.112(2) Uani 1 1 d U . .
F3 F 0.4208(17) 0.1276(6) 0.149(2) 0.364(15) Uani 1 1 d . . .
F2 F 0.4063(9) 0.1961(6) 0.0356(5) 0.152(3) Uani 1 1 d U . .
F6 F 0.4132(19) 0.2559(4) 0.1430(12) 0.260(7) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.275(7) . ?
C1 N2 1.374(6) . ?
C1 H1 0.9500 . ?
C2 C7 1.399(7) . ?
C2 C3 1.409(7) . ?
C2 N1 1.461(6) . ?
C3 C4 1.389(8) . ?
C3 C8 1.519(7) . ?
C4 C5 1.384(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(8) . ?
C6 H6 0.9500 . ?
C7 C11 1.533(8) . ?
C8 C9 1.533(9) . ?
C8 C10 1.544(9) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.526(8) . ?
C11 C13 1.538(9) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.394(8) . ?
C14 C19 1.406(8) . ?
C14 N2 1.458(6) . ?
C15 C16 1.407(8) . ?
C15 C20 1.525(8) . ?
C16 C17 1.375(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(8) . ?
C18 H18 0.9500 . ?
C19 C23 1.527(8) . ?
C20 C21 1.522(8) . ?
C20 C22 1.540(8) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.537(9) . ?
C23 C24 1.539(9) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N3 1.282(7) . ?
C26 N2 1.390(6) 3_756 ?
C26 C27 1.497(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N1 Pd1 2.021(4) . ?
N2 C26 1.390(6) 3_756 ?
N3 Pd1 1.975(4) . ?
N3 H3 0.8800 . ?
P1 F6 1.390(8) . ?
P1 F3 1.427(11) . ?
P1 F5 1.511(5) . ?
P1 F2 1.537(7) . ?
P1 F1 1.547(5) . ?
P1 F4 1.598(7) . ?
Pd1 N3 1.975(4) 3_756 ?
Pd1 N1 2.021(4) 3_756 ?

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
N1 C1 N2 126.5(5) . . ?
N1 C1 H1 116.8 . . ?
N2 C1 H1 116.8 . . ?
C7 C2 C3 123.5(5) . . ?
C7 C2 N1 118.5(5) . . ?
C3 C2 N1 117.4(4) . . ?
C4 C3 C2 116.7(5) . . ?
C4 C3 C8 120.3(5) . . ?
C2 C3 C8 123.0(5) . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 120.7(5) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 117.2(5) . . ?
C6 C7 C11 121.2(5) . . ?
C2 C7 C11 121.6(5) . . ?
C3 C8 C9 112.3(5) . . ?
C3 C8 C10 110.2(5) . . ?
C9 C8 C10 111.6(5) . . ?
C3 C8 H8 107.5 . . ?
C9 C8 H8 107.5 . . ?
C10 C8 H8 107.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 111.7(5) . . ?
C12 C11 C13 110.4(5) . . ?
C7 C11 C13 111.8(5) . . ?
C12 C11 H11 107.6 . . ?
C7 C11 H11 107.6 . . ?
C13 C11 H11 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 124.3(5) . . ?
C15 C14 N2 117.8(5) . . ?
C19 C14 N2 118.0(5) . . ?
C14 C15 C16 117.1(5) . . ?
C14 C15 C20 123.2(5) . . ?
C16 C15 C20 119.8(5) . . ?
C17 C16 C15 119.9(5) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 121.8(5) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C19 120.6(6) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 116.3(5) . . ?
C18 C19 C23 120.9(5) . . ?
C14 C19 C23 122.8(5) . . ?
C21 C20 C15 112.0(5) . . ?
C21 C20 C22 110.8(5) . . ?
C15 C20 C22 110.9(5) . . ?
C21 C20 H20 107.6 . . ?
C15 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 C25 109.6(5) . . ?
C19 C23 C24 111.2(5) . . ?
C25 C23 C24 110.6(5) . . ?
C19 C23 H23 108.5 . . ?
C25 C23 H23 108.5 . . ?
C24 C23 H23 108.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 121.3(5) . 3_756 ?
N3 C26 C27 120.6(4) . . ?
N2 C26 C27 118.1(5) 3_756 . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 N1 C2 117.4(4) . . ?
C1 N1 Pd1 127.9(3) . . ?
C2 N1 Pd1 114.7(3) . . ?
C1 N2 C26 124.8(4) . 3_756 ?
C1 N2 C14 116.3(4) . . ?
C26 N2 C14 118.4(4) 3_756 . ?
C26 N3 Pd1 133.3(4) . . ?
C26 N3 H3 113.4 . . ?
Pd1 N3 H3 113.4 . . ?
F6 P1 F3 162.8(15) . . ?
F6 P1 F5 93.2(7) . . ?
F3 P1 F5 97.6(12) . . ?
F6 P1 F2 80.1(8) . . ?
F3 P1 F2 89.2(12) . . ?
F5 P1 F2 173.2(6) . . ?
F6 P1 F1 104.5(8) . . ?
F3 P1 F1 87.9(7) . . ?
F5 P1 F1 94.9(3) . . ?
F2 P1 F1 85.8(4) . . ?
F6 P1 F4 86.6(8) . . ?
F3 P1 F4 81.2(7) . . ?
F5 P1 F4 84.5(3) . . ?
F2 P1 F4 96.1(4) . . ?
F1 P1 F4 168.8(5) . . ?
N3 Pd1 N3 180.0(3) . 3_756 ?
N3 Pd1 N1 93.82(17) . . ?
N3 Pd1 N1 86.18(17) 3_756 . ?
N3 Pd1 N1 86.18(17) . 3_756 ?
N3 Pd1 N1 93.82(17) 3_756 3_756 ?
N1 Pd1 N1 180.00(9) . 3_756 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 1.5(8) . . . . ?
N1 C2 C3 C4 -169.5(4) . . . . ?
C7 C2 C3 C8 -178.8(5) . . . . ?
N1 C2 C3 C8 10.2(7) . . . . ?
C2 C3 C4 C5 0.7(8) . . . . ?
C8 C3 C4 C5 -179.0(5) . . . . ?
C3 C4 C5 C6 -2.4(8) . . . . ?
C4 C5 C6 C7 1.9(8) . . . . ?
C5 C6 C7 C2 0.2(8) . . . . ?
C5 C6 C7 C11 179.6(5) . . . . ?
C3 C2 C7 C6 -2.0(8) . . . . ?
N1 C2 C7 C6 168.9(4) . . . . ?
C3 C2 C7 C11 178.7(5) . . . . ?
N1 C2 C7 C11 -10.4(7) . . . . ?
C4 C3 C8 C9 61.2(7) . . . . ?
C2 C3 C8 C9 -118.5(6) . . . . ?
C4 C3 C8 C10 -63.9(7) . . . . ?
C2 C3 C8 C10 116.5(6) . . . . ?
C6 C7 C11 C12 41.0(7) . . . . ?
C2 C7 C11 C12 -139.6(5) . . . . ?
C6 C7 C11 C13 -83.2(6) . . . . ?
C2 C7 C11 C13 96.1(6) . . . . ?
C19 C14 C15 C16 0.7(8) . . . . ?
N2 C14 C15 C16 -178.6(5) . . . . ?
C19 C14 C15 C20 -179.9(5) . . . . ?
N2 C14 C15 C20 0.8(7) . . . . ?
C14 C15 C16 C17 0.6(8) . . . . ?
C20 C15 C16 C17 -178.8(5) . . . . ?
C15 C16 C17 C18 -1.1(9) . . . . ?
C16 C17 C18 C19 0.3(9) . . . . ?
C17 C18 C19 C14 1.0(8) . . . . ?
C17 C18 C19 C23 -178.6(5) . . . . ?
C15 C14 C19 C18 -1.5(8) . . . . ?
N2 C14 C19 C18 177.8(5) . . . . ?
C15 C14 C19 C23 178.1(5) . . . . ?
N2 C14 C19 C23 -2.6(8) . . . . ?
C14 C15 C20 C21 120.2(6) . . . . ?
C16 C15 C20 C21 -60.4(7) . . . . ?
C14 C15 C20 C22 -115.4(6) . . . . ?
C16 C15 C20 C22 64.0(7) . . . . ?
C18 C19 C23 C25 71.7(7) . . . . ?
C14 C19 C23 C25 -107.9(6) . . . . ?
C18 C19 C23 C24 -50.9(7) . . . . ?
C14 C19 C23 C24 129.6(6) . . . . ?
N2 C1 N1 C2 179.5(5) . . . . ?
N2 C1 N1 Pd1 -1.4(7) . . . . ?
C7 C2 N1 C1 94.6(6) . . . . ?
C3 C2 N1 C1 -93.9(6) . . . . ?
C7 C2 N1 Pd1 -84.6(5) . . . . ?
C3 C2 N1 Pd1 86.9(5) . . . . ?
N1 C1 N2 C26 1.3(8) . . . 3_756 ?
N1 C1 N2 C14 172.9(5) . . . . ?
C15 C14 N2 C1 -81.6(6) . . . . ?
C19 C14 N2 C1 99.0(6) . . . . ?
C15 C14 N2 C26 90.6(6) . . . 3_756 ?
C19 C14 N2 C26 -88.8(6) . . . 3_756 ?
N2 C26 N3 Pd1 3.4(9) 3_756 . . . ?
C27 C26 N3 Pd1 -176.8(4) . . . . ?
C26 N3 Pd1 N3 169(20) . . . 3_756 ?
C26 N3 Pd1 N1 177.4(5) . . . . ?
C26 N3 Pd1 N1 -2.6(5) . . . 3_756 ?
C1 N1 Pd1 N3 179.8(4) . . . . ?
C2 N1 Pd1 N3 -1.1(4) . . . . ?
C1 N1 Pd1 N3 -0.2(4) . . . 3_756 ?
C2 N1 Pd1 N3 178.9(4) . . . 3_756 ?
C1 N1 Pd1 N1 -52(21) . . . 3_756 ?
C2 N1 Pd1 N1 127(21) . . . 3_756 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.402
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.154
_database_code_depnum_ccdc_archive 'CCDC 1020746'
#######################################################################
#
#                 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_Compound-10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H82 N6 Pd, 2(F6 P)'
_chemical_formula_sum            'C56 H82 F12 N6 P2 Pd'

_chemical_formula_weight         1235.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_HALL  '-P 2yn'

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                   11.370(2)
_cell_length_b                   13.036(3)
_cell_length_c                   19.856(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.279(3)
_cell_angle_gamma                90.00
_cell_volume                     2925.4(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4685
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      27.20

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15379
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5409
_reflns_number_gt                4240
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP 3'
_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)+(0.1056P)²+7.4029P] 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         5409
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1977
_refine_ls_wR_factor_gt          0.1783
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
C1 C 0.2162(4) 0.8813(4) 0.9838(2) 0.0285(10) Uani 1 1 d . . .
H1 H 0.2983 0.8765 0.9900 0.034 Uiso 1 1 calc R . .
C2 C 0.2563(4) 1.0214(4) 1.0547(3) 0.0321(11) Uani 1 1 d . . .
C3 C 0.3194(5) 1.0974(5) 1.0239(4) 0.0529(17) Uani 1 1 d . . .
C4 C 0.3948(6) 1.1583(5) 1.0689(6) 0.077(3) Uani 1 1 d . . .
H4 H 0.4391 1.2095 1.0509 0.093 Uiso 1 1 calc R . .
C5 C 0.4055(6) 1.1457(6) 1.1364(6) 0.081(3) Uani 1 1 d . . .
H5 H 0.4553 1.1882 1.1641 0.097 Uiso 1 1 calc R . .
C6 C 0.3431(6) 1.0703(6) 1.1642(4) 0.066(2) Uani 1 1 d . . .
H6 H 0.3514 1.0624 1.2110 0.079 Uiso 1 1 calc R . .
C7 C 0.2678(5) 1.0053(4) 1.1249(3) 0.0418(14) Uani 1 1 d . . .
C8 C 0.3091(6) 1.1127(6) 0.9488(4) 0.077(2) Uani 1 1 d . . .
H8 H 0.2487 1.0662 0.9270 0.092 Uiso 1 1 calc R . .
C9 C 0.4246(7) 1.0952(7) 0.9195(6) 0.099(3) Uani 1 1 d . . .
H9A H 0.4861 1.1343 0.9446 0.149 Uiso 1 1 calc R . .
H9B H 0.4167 1.1165 0.8729 0.149 Uiso 1 1 calc R . .
H9C H 0.4444 1.0236 0.9222 0.149 Uiso 1 1 calc R . .
C10 C 0.2716(10) 1.2274(8) 0.9321(6) 0.118(4) Uani 1 1 d . . .
H10A H 0.1923 1.2384 0.9429 0.177 Uiso 1 1 calc R . .
H10B H 0.2752 1.2405 0.8848 0.177 Uiso 1 1 calc R . .
H10C H 0.3245 1.2730 0.9586 0.177 Uiso 1 1 calc R . .
C11 C 0.2004(5) 0.9219(5) 1.1580(3) 0.0465(14) Uani 1 1 d . . .
H11 H 0.1551 0.8826 1.1219 0.056 Uiso 1 1 calc R . .
C12 C 0.1150(9) 0.9650(8) 1.2029(5) 0.094(3) Uani 1 1 d . . .
H12A H 0.1550 1.0135 1.2337 0.141 Uiso 1 1 calc R . .
H12B H 0.0837 0.9104 1.2281 0.141 Uiso 1 1 calc R . .
H12C H 0.0514 0.9986 1.1756 0.141 Uiso 1 1 calc R . .
C13 C 0.2874(7) 0.8489(6) 1.1975(4) 0.0675(19) Uani 1 1 d . . .
H13A H 0.3337 0.8860 1.2328 0.101 Uiso 1 1 calc R . .
H13B H 0.3387 0.8194 1.1674 0.101 Uiso 1 1 calc R . .
H13C H 0.2444 0.7952 1.2172 0.101 Uiso 1 1 calc R . .
C14 C 0.2369(4) 0.7424(4) 0.9077(3) 0.0311(11) Uani 1 1 d . . .
C15 C 0.2966(5) 0.6601(4) 0.9403(3) 0.0369(12) Uani 1 1 d . . .
C16 C 0.3741(5) 0.6066(4) 0.9022(3) 0.0477(15) Uani 1 1 d . . .
H16 H 0.4165 0.5511 0.9217 0.057 Uiso 1 1 calc R . .
C17 C 0.3886(5) 0.6340(5) 0.8373(3) 0.0489(15) Uani 1 1 d . . .
H17 H 0.4409 0.5973 0.8137 0.059 Uiso 1 1 calc R . .
C18 C 0.3270(5) 0.7151(4) 0.8063(3) 0.0422(13) Uani 1 1 d . . .
H18 H 0.3379 0.7322 0.7619 0.051 Uiso 1 1 calc R . .
C19 C 0.2485(4) 0.7720(4) 0.8407(3) 0.0353(12) Uani 1 1 d . . .
C20 C 0.2807(5) 0.6264(4) 1.0116(3) 0.0415(13) Uani 1 1 d . . .
H20 H 0.2106 0.6609 1.0255 0.050 Uiso 1 1 calc R . .
C21 C 0.3870(6) 0.6559(5) 1.0614(3) 0.0586(17) Uani 1 1 d . . .
H21A H 0.4578 0.6283 1.0462 0.088 Uiso 1 1 calc R . .
H21B H 0.3772 0.6287 1.1054 0.088 Uiso 1 1 calc R . .
H21C H 0.3930 0.7293 1.0641 0.088 Uiso 1 1 calc R . .
C22 C 0.2612(7) 0.5098(4) 1.0157(4) 0.0563(17) Uani 1 1 d . . .
H22A H 0.2000 0.4894 0.9811 0.085 Uiso 1 1 calc R . .
H22B H 0.2382 0.4926 1.0594 0.085 Uiso 1 1 calc R . .
H22C H 0.3333 0.4747 1.0091 0.085 Uiso 1 1 calc R . .
C23 C 0.1835(5) 0.8615(5) 0.8053(3) 0.0417(13) Uani 1 1 d . . .
H23 H 0.1405 0.8974 0.8384 0.050 Uiso 1 1 calc R . .
C24 C 0.0942(7) 0.8252(7) 0.7480(4) 0.073(2) Uani 1 1 d . . .
H24A H 0.1337 0.7852 0.7167 0.110 Uiso 1 1 calc R . .
H24B H 0.0572 0.8835 0.7250 0.110 Uiso 1 1 calc R . .
H24C H 0.0351 0.7840 0.7661 0.110 Uiso 1 1 calc R . .
C25 C 0.2692(7) 0.9361(7) 0.7793(5) 0.090(3) Uani 1 1 d . . .
H25A H 0.3275 0.9558 0.8157 0.134 Uiso 1 1 calc R . .
H25B H 0.2272 0.9959 0.7617 0.134 Uiso 1 1 calc R . .
H25C H 0.3077 0.9042 0.7440 0.134 Uiso 1 1 calc R . .
C26 C 0.0372(4) 0.7929(4) 0.9374(2) 0.0255(10) Uani 1 1 d . . .
C27 C -0.0074(4) 0.6929(4) 0.9081(3) 0.0314(11) Uani 1 1 d . . .
H27A H 0.0118 0.6396 0.9415 0.038 Uiso 1 1 calc R . .
H27B H 0.0343 0.6773 0.8692 0.038 Uiso 1 1 calc R . .
C28 C -0.1391(5) 0.6895(4) 0.8861(3) 0.0443(14) Uani 1 1 d . . .
H28A H -0.1816 0.6989 0.9248 0.066 Uiso 1 1 calc R . .
H28B H -0.1594 0.6243 0.8656 0.066 Uiso 1 1 calc R . .
H28C H -0.1597 0.7432 0.8538 0.066 Uiso 1 1 calc R . .
F1 F 0.0106(4) 0.6952(3) 0.1991(2) 0.0729(12) Uani 1 1 d . . .
F2 F 0.0117(5) 0.5207(4) 0.1841(3) 0.0898(15) Uani 1 1 d . . .
F3 F 0.0223(4) 0.5487(4) 0.0732(2) 0.0847(13) Uani 1 1 d . . .
F4 F 0.0287(4) 0.7149(3) 0.0871(2) 0.0709(11) Uani 1 1 d . . .
F5 F -0.1215(4) 0.6216(4) 0.1261(3) 0.0992(16) Uani 1 1 d . . .
F6 F 0.1564(3) 0.6147(3) 0.15320(19) 0.0637(10) Uani 1 1 d . . .
N1 N 0.1718(3) 0.9582(3) 1.01248(19) 0.0258(8) Uani 1 1 d . . .
N2 N 0.1593(3) 0.8061(3) 0.94572(19) 0.0267(8) Uani 1 1 d . . .
N3 N -0.0306(3) 0.8625(3) 0.95693(18) 0.0255(8) Uani 1 1 d . . .
H3 H -0.1045 0.8471 0.9502 0.031 Uiso 1 1 calc R . .
P1 P 0.01889(17) 0.62194(16) 0.13755(10) 0.0617(5) Uani 1 1 d . . .
Pd1 Pd 0.0000 1.0000 1.0000 0.02265(19) Uani 1 2 d S . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.282(6) . ?
C1 N2 1.359(6) . ?
C1 H1 0.9300 . ?
C2 C7 1.402(8) . ?
C2 C3 1.403(8) . ?
C2 N1 1.459(6) . ?
C3 C4 1.413(10) . ?
C3 C8 1.496(10) . ?
C4 C5 1.343(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.363(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.383(8) . ?
C6 H6 0.9300 . ?
C7 C11 1.520(9) . ?
C8 C9 1.511(10) . ?
C8 C10 1.580(12) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.498(10) . ?
C11 C13 1.526(9) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.391(7) . ?
C14 C19 1.405(7) . ?
C14 N2 1.478(6) . ?
C15 C16 1.409(8) . ?
C15 C20 1.513(8) . ?
C16 C17 1.364(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(7) . ?
C18 H18 0.9300 . ?
C19 C23 1.513(8) . ?
C20 C21 1.525(9) . ?
C20 C22 1.539(8) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C25 1.507(10) . ?
C23 C24 1.515(8) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N3 1.278(6) . ?
C26 N2 1.391(6) . ?
C26 C27 1.493(7) . ?
C27 C28 1.513(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
F1 P1 1.562(4) . ?
F2 P1 1.618(5) . ?
F3 P1 1.599(5) . ?
F4 P1 1.584(4) . ?
F5 P1 1.587(5) . ?
F6 P1 1.563(4) . ?
N1 Pd1 2.017(4) . ?
N3 Pd1 2.000(4) . ?
N3 H3 0.8600 . ?
Pd1 N3 2.000(4) 3_577 ?
Pd1 N1 2.017(4) 3_577 ?

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
N1 C1 N2 128.6(4) . . ?
N1 C1 H1 115.7 . . ?
N2 C1 H1 115.7 . . ?
C7 C2 C3 122.9(5) . . ?
C7 C2 N1 118.1(5) . . ?
C3 C2 N1 119.0(5) . . ?
C2 C3 C4 115.2(7) . . ?
C2 C3 C8 122.7(6) . . ?
C4 C3 C8 122.1(7) . . ?
C5 C4 C3 123.0(7) . . ?
C5 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
C4 C5 C6 119.9(7) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 122.1(8) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C2 117.0(6) . . ?
C6 C7 C11 120.3(6) . . ?
C2 C7 C11 122.7(5) . . ?
C3 C8 C9 112.8(7) . . ?
C3 C8 C10 108.9(8) . . ?
C9 C8 C10 106.7(6) . . ?
C3 C8 H8 109.4 . . ?
C9 C8 H8 109.4 . . ?
C10 C8 H8 109.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 112.3(6) . . ?
C12 C11 C13 110.7(6) . . ?
C7 C11 C13 109.9(5) . . ?
C12 C11 H11 107.9 . . ?
C7 C11 H11 107.9 . . ?
C13 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 124.2(5) . . ?
C15 C14 N2 118.9(4) . . ?
C19 C14 N2 116.9(4) . . ?
C14 C15 C16 115.7(5) . . ?
C14 C15 C20 124.0(5) . . ?
C16 C15 C20 120.3(5) . . ?
C17 C16 C15 121.7(6) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 121.1(5) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 120.6(5) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 116.7(5) . . ?
C18 C19 C23 119.3(5) . . ?
C14 C19 C23 124.0(4) . . ?
C15 C20 C21 111.4(5) . . ?
C15 C20 C22 111.7(5) . . ?
C21 C20 C22 108.9(5) . . ?
C15 C20 H20 108.2 . . ?
C21 C20 H20 108.2 . . ?
C22 C20 H20 108.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C19 110.8(5) . . ?
C25 C23 C24 110.5(6) . . ?
C19 C23 C24 111.1(5) . . ?
C25 C23 H23 108.1 . . ?
C19 C23 H23 108.1 . . ?
C24 C23 H23 108.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 N2 120.2(4) . . ?
N3 C26 C27 123.2(4) . . ?
N2 C26 C27 116.5(4) . . ?
C26 C27 C28 114.9(4) . . ?
C26 C27 H27A 108.5 . . ?
C28 C27 H27A 108.5 . . ?
C26 C27 H27B 108.5 . . ?
C28 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C1 N1 C2 115.4(4) . . ?
C1 N1 Pd1 125.4(3) . . ?
C2 N1 Pd1 119.1(3) . . ?
C1 N2 C26 124.3(4) . . ?
C1 N2 C14 114.6(4) . . ?
C26 N2 C14 120.9(4) . . ?
C26 N3 Pd1 133.1(3) . . ?
C26 N3 H3 113.4 . . ?
Pd1 N3 H3 113.4 . . ?
F1 P1 F6 91.5(2) . . ?
F1 P1 F4 92.4(3) . . ?
F6 P1 F4 91.9(2) . . ?
F1 P1 F5 88.2(3) . . ?
F6 P1 F5 175.2(3) . . ?
F4 P1 F5 92.9(3) . . ?
F1 P1 F3 177.7(3) . . ?
F6 P1 F3 90.7(2) . . ?
F4 P1 F3 86.7(3) . . ?
F5 P1 F3 89.7(3) . . ?
F1 P1 F2 92.3(3) . . ?
F6 P1 F2 87.1(3) . . ?
F4 P1 F2 175.2(3) . . ?
F5 P1 F2 88.1(3) . . ?
F3 P1 F2 88.7(3) . . ?
N3 Pd1 N3 180.000(2) 3_577 . ?
N3 Pd1 N1 86.04(16) 3_577 3_577 ?
N3 Pd1 N1 93.95(16) . 3_577 ?
N3 Pd1 N1 93.95(16) 3_577 . ?
N3 Pd1 N1 86.05(16) . . ?
N1 Pd1 N1 179.999(1) 3_577 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C2 C3 C4 -0.9(8) . . . . ?
N1 C2 C3 C4 176.9(5) . . . . ?
C7 C2 C3 C8 178.5(6) . . . . ?
N1 C2 C3 C8 -3.7(8) . . . . ?
C2 C3 C4 C5 -0.5(10) . . . . ?
C8 C3 C4 C5 -179.9(7) . . . . ?
C3 C4 C5 C6 0.9(11) . . . . ?
C4 C5 C6 C7 -0.1(10) . . . . ?
C5 C6 C7 C2 -1.2(9) . . . . ?
C5 C6 C7 C11 179.6(6) . . . . ?
C3 C2 C7 C6 1.7(8) . . . . ?
N1 C2 C7 C6 -176.2(5) . . . . ?
C3 C2 C7 C11 -179.1(5) . . . . ?
N1 C2 C7 C11 3.0(7) . . . . ?
C2 C3 C8 C9 -117.6(7) . . . . ?
C4 C3 C8 C9 61.7(9) . . . . ?
C2 C3 C8 C10 124.0(7) . . . . ?
C4 C3 C8 C10 -56.6(9) . . . . ?
C6 C7 C11 C12 63.7(8) . . . . ?
C2 C7 C11 C12 -115.5(7) . . . . ?
C6 C7 C11 C13 -60.1(7) . . . . ?
C2 C7 C11 C13 120.8(6) . . . . ?
C19 C14 C15 C16 1.1(8) . . . . ?
N2 C14 C15 C16 -176.5(5) . . . . ?
C19 C14 C15 C20 -177.8(5) . . . . ?
N2 C14 C15 C20 4.6(8) . . . . ?
C14 C15 C16 C17 -0.3(8) . . . . ?
C20 C15 C16 C17 178.7(5) . . . . ?
C15 C16 C17 C18 -0.5(9) . . . . ?
C16 C17 C18 C19 0.4(9) . . . . ?
C17 C18 C19 C14 0.3(8) . . . . ?
C17 C18 C19 C23 179.2(5) . . . . ?
C15 C14 C19 C18 -1.1(8) . . . . ?
N2 C14 C19 C18 176.5(4) . . . . ?
C15 C14 C19 C23 -180.0(5) . . . . ?
N2 C14 C19 C23 -2.4(7) . . . . ?
C14 C15 C20 C21 -106.2(6) . . . . ?
C16 C15 C20 C21 74.9(7) . . . . ?
C14 C15 C20 C22 131.8(6) . . . . ?
C16 C15 C20 C22 -47.1(7) . . . . ?
C18 C19 C23 C25 -54.8(8) . . . . ?
C14 C19 C23 C25 124.1(7) . . . . ?
C18 C19 C23 C24 68.5(7) . . . . ?
C14 C19 C23 C24 -112.7(6) . . . . ?
N3 C26 C27 C28 15.2(7) . . . . ?
N2 C26 C27 C28 -167.7(4) . . . . ?
N2 C1 N1 C2 175.3(5) . . . . ?
N2 C1 N1 Pd1 -7.7(7) . . . . ?
C7 C2 N1 C1 -99.0(5) . . . . ?
C3 C2 N1 C1 83.1(6) . . . . ?
C7 C2 N1 Pd1 83.8(5) . . . . ?
C3 C2 N1 Pd1 -94.1(5) . . . . ?
N1 C1 N2 C26 -8.0(8) . . . . ?
N1 C1 N2 C14 166.9(5) . . . . ?
N3 C26 N2 C1 11.5(7) . . . . ?
C27 C26 N2 C1 -165.7(4) . . . . ?
N3 C26 N2 C14 -163.0(4) . . . . ?
C27 C26 N2 C14 19.8(6) . . . . ?
C15 C14 N2 C1 84.0(6) . . . . ?
C19 C14 N2 C1 -93.7(5) . . . . ?
C15 C14 N2 C26 -100.9(5) . . . . ?
C19 C14 N2 C26 81.4(6) . . . . ?
N2 C26 N3 Pd1 0.8(7) . . . . ?
C27 C26 N3 Pd1 177.8(3) . . . . ?
C26 N3 Pd1 N3 157(100) . . . 3_577 ?
C26 N3 Pd1 N1 169.4(4) . . . 3_577 ?
C26 N3 Pd1 N1 -10.6(4) . . . . ?
C1 N1 Pd1 N3 -166.7(4) . . . 3_577 ?
C2 N1 Pd1 N3 10.2(4) . . . 3_577 ?
C1 N1 Pd1 N3 13.3(4) . . . . ?
C2 N1 Pd1 N3 -169.8(4) . . . . ?
C1 N1 Pd1 N1 -115.4(9) . . . 3_577 ?
C2 N1 Pd1 N1 61.5(10) . . . 3_577 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.130
_database_code_depnum_ccdc_archive 'CCDC 1020747'
