# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'John Spencer'
_publ_contact_author_email       J.SPENCER@GRE.AC.UK

_publ_section_title              
;
Synthesis of a 1,4-Benzodiazepine Containing
Palladacycle with in Vitro Anticancer and Cathepsin B Activity
;
loop_
_publ_author_name
'John Spencer'
'John A Hartley'
'Ali Hazrati'
'Mike Hursthouse'
'Arun K. Kotha'
'Louise Male'
;
M.Motukuri
;
'Rajendra P. Rathnam'
'Simon Richardson'

# Attachment 'Pdcycle.cif'

data_3
_database_code_depnum_ccdc_archive 'CCDC 706386'

# EPSRC National Crystallography Service Code: 2008src0444

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Pd2L2(m-dppe)Cl2]
where LH=1-methyl-5-phenyl-1H-1,4-benzodiazepin-2(3H)-one
;
_chemical_name_common            
;(Pd2L2(m-dppe)Cl2) where LH=1-methyl-5-phenyl-1H-1,4-
benzodiazepin-2(3H)-one
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H50 Cl2 N4 O2 P2 Pd2, 4(C1 H1 Cl3)'
_chemical_formula_sum            'C62 H54 Cl14 N4 O2 P2 Pd2'
_chemical_formula_weight         1658.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'P 2(1)/c'

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

_cell_length_a                   11.3456(5)
_cell_length_b                   10.9170(4)
_cell_length_c                   27.5717(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.760(2)
_cell_angle_gamma                90.00
_cell_volume                     3383.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    34010
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1660
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 19436 reflections reduced R(int) from 0.1123 to 0.671
Ratio of minimum to maximum apparent transmission: 0.818031
The given Tmin and Tmax were generated using the SHELX SIZE command.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21908
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5894
_reflns_number_gt                4287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    
;
Sir2004 (Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R.,
2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, (1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0000P)^2^+59.8772P] where P=(Fo^2^+2Fc^2^)/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         5894
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0856
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1567
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 0.4172(9) 0.3670(9) 0.1490(4) 0.032(2) Uani 1 1 d . . .
C2 C 0.6181(10) 0.4414(9) 0.1500(4) 0.038(3) Uani 1 1 d . . .
H2A H 0.5995 0.4486 0.1144 0.057 Uiso 1 1 calc R . .
H2B H 0.6999 0.4119 0.1585 0.057 Uiso 1 1 calc R . .
H2C H 0.6100 0.5217 0.1651 0.057 Uiso 1 1 calc R . .
C3 C 0.5753(8) 0.2801(9) 0.2100(3) 0.028(2) Uani 1 1 d . . .
C4 C 0.6552(8) 0.3315(10) 0.2465(4) 0.035(2) Uani 1 1 d . . .
H4 H 0.6835 0.4123 0.2426 0.042 Uiso 1 1 calc R . .
C5 C 0.6945(8) 0.2668(10) 0.2887(4) 0.034(2) Uani 1 1 d . . .
H5 H 0.7493 0.3033 0.3136 0.040 Uiso 1 1 calc R . .
C6 C 0.6541(9) 0.1488(10) 0.2947(4) 0.035(2) Uani 1 1 d . . .
H6 H 0.6786 0.1046 0.3240 0.042 Uiso 1 1 calc R . .
C7 C 0.5776(9) 0.0966(10) 0.2572(3) 0.034(2) Uani 1 1 d . . .
H7 H 0.5503 0.0154 0.2610 0.040 Uiso 1 1 calc R . .
C8 C 0.5394(8) 0.1589(9) 0.2142(3) 0.027(2) Uani 1 1 d . . .
C9 C 0.4568(8) 0.0988(9) 0.1744(3) 0.025(2) Uani 1 1 d . . .
C10 C 0.4798(8) -0.0222(9) 0.1545(3) 0.027(2) Uani 1 1 d . . .
C11 C 0.5866(8) -0.0866(9) 0.1685(4) 0.034(2) Uani 1 1 d . . .
H11 H 0.6455 -0.0523 0.1924 0.040 Uiso 1 1 calc R . .
C12 C 0.6069(9) -0.1984(10) 0.1481(4) 0.038(3) Uani 1 1 d . . .
H12 H 0.6778 -0.2427 0.1586 0.046 Uiso 1 1 calc R . .
C13 C 0.5212(9) -0.2455(9) 0.1118(4) 0.032(2) Uani 1 1 d . . .
H13 H 0.5344 -0.3216 0.0967 0.038 Uiso 1 1 calc R . .
C14 C 0.4158(9) -0.1806(9) 0.0976(4) 0.032(2) Uani 1 1 d . . .
H14 H 0.3580 -0.2146 0.0731 0.038 Uiso 1 1 calc R . .
C15 C 0.3928(8) -0.0687(8) 0.1179(3) 0.022(2) Uani 1 1 d . . .
C16 C 0.3340(8) 0.2767(9) 0.1698(4) 0.033(2) Uani 1 1 d . . .
H16A H 0.3454 0.2814 0.2059 0.039 Uiso 1 1 calc R . .
H16B H 0.2502 0.2976 0.1578 0.039 Uiso 1 1 calc R . .
C17 C 0.2190(8) -0.1339(8) -0.0009(3) 0.025(2) Uani 1 1 d . . .
C18 C 0.3084(8) -0.0568(9) -0.0136(3) 0.028(2) Uani 1 1 d . . .
H18 H 0.3398 0.0065 0.0080 0.033 Uiso 1 1 calc R . .
C19 C 0.3504(8) -0.0735(9) -0.0580(3) 0.029(2) Uani 1 1 d . . .
H19 H 0.4113 -0.0216 -0.0668 0.035 Uiso 1 1 calc R . .
C20 C 0.3044(9) -0.1655(10) -0.0897(4) 0.036(2) Uani 1 1 d . . .
H20 H 0.3325 -0.1750 -0.1204 0.043 Uiso 1 1 calc R . .
C21 C 0.2178(9) -0.2433(9) -0.0768(4) 0.035(3) Uani 1 1 d . . .
H21 H 0.1893 -0.3088 -0.0979 0.042 Uiso 1 1 calc R . .
C22 C 0.1723(8) -0.2256(9) -0.0328(4) 0.030(2) Uani 1 1 d . . .
H22 H 0.1097 -0.2760 -0.0246 0.036 Uiso 1 1 calc R . .
C23 C 0.1046(8) -0.2226(9) 0.0852(3) 0.024(2) Uani 1 1 d . . .
C24 C 0.1374(8) -0.3405(9) 0.0783(4) 0.029(2) Uani 1 1 d . . .
H24 H 0.1888 -0.3583 0.0548 0.035 Uiso 1 1 calc R . .
C25 C 0.0969(9) -0.4349(10) 0.1052(4) 0.040(3) Uani 1 1 d . . .
H25 H 0.1202 -0.5168 0.0998 0.048 Uiso 1 1 calc R . .
C26 C 0.0220(9) -0.4109(11) 0.1403(4) 0.043(3) Uani 1 1 d . . .
H26 H -0.0064 -0.4756 0.1587 0.052 Uiso 1 1 calc R . .
C27 C -0.0096(10) -0.2914(10) 0.1478(4) 0.040(3) Uani 1 1 d . . .
H27 H -0.0609 -0.2735 0.1714 0.048 Uiso 1 1 calc R . .
C28 C 0.0326(9) -0.1962(10) 0.1211(4) 0.034(2) Uani 1 1 d . . .
H28 H 0.0124 -0.1138 0.1274 0.041 Uiso 1 1 calc R . .
C29 C -0.0006(7) -0.0437(8) 0.0219(3) 0.0211(19) Uani 1 1 d . . .
H29A H -0.0453 -0.1186 0.0106 0.025 Uiso 1 1 calc R . .
H29B H -0.0437 -0.0036 0.0465 0.025 Uiso 1 1 calc R . .
N1 N 0.5352(7) 0.3539(7) 0.1683(3) 0.0281(18) Uani 1 1 d . . .
N2 N 0.3601(7) 0.1526(7) 0.1542(3) 0.0271(18) Uani 1 1 d . . .
O1 O 0.3822(7) 0.4417(7) 0.1188(3) 0.0420(18) Uani 1 1 d . . .
P1 P 0.1475(2) -0.0885(2) 0.05159(9) 0.0216(5) Uani 1 1 d . . .
Cl1 Cl 0.1077(2) 0.2032(2) 0.08697(9) 0.0278(5) Uani 1 1 d . . .
Pd1 Pd 0.25446(6) 0.04681(6) 0.10162(3) 0.0217(2) Uani 1 1 d . . .
C101 C 0.0044(11) 0.1521(10) 0.1981(5) 0.051(3) Uani 1 1 d . . .
H101 H 0.0154 0.1540 0.1627 0.061 Uiso 1 1 calc R . .
Cl11 Cl 0.1306(3) 0.0834(3) 0.23128(14) 0.0676(10) Uani 1 1 d . . .
Cl12 Cl -0.1202(3) 0.0657(4) 0.20402(16) 0.0846(13) Uani 1 1 d . . .
Cl13 Cl -0.0126(4) 0.3010(3) 0.21746(13) 0.0836(13) Uani 1 1 d . . .
C102 C 0.3022(9) 0.3544(10) 0.0103(4) 0.038(3) Uani 1 1 d . . .
H102 H 0.2585 0.3552 0.0394 0.046 Uiso 1 1 calc R . .
Cl21 Cl 0.4322(2) 0.2642(2) 0.02325(11) 0.0438(7) Uani 1 1 d . . .
Cl22 Cl 0.2097(3) 0.2933(3) -0.04026(12) 0.0606(9) Uani 1 1 d . . .
Cl23 Cl 0.3426(3) 0.5064(3) -0.00338(12) 0.0512(8) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.045(6) 0.023(5) 0.024(5) -0.010(5) -0.005(5) -0.003(5)
C2 0.052(7) 0.033(6) 0.033(6) 0.004(5) 0.015(5) -0.005(5)
C3 0.023(5) 0.035(6) 0.027(5) -0.005(4) 0.008(4) 0.000(4)
C4 0.026(5) 0.042(6) 0.038(6) -0.006(5) 0.005(5) -0.004(5)
C5 0.021(5) 0.052(7) 0.024(5) -0.015(5) -0.011(4) 0.000(5)
C6 0.034(6) 0.049(7) 0.021(5) 0.004(5) -0.002(4) 0.002(5)
C7 0.036(6) 0.038(6) 0.025(5) 0.006(5) -0.003(5) -0.005(5)
C8 0.033(5) 0.027(5) 0.020(5) 0.004(4) 0.002(4) 0.006(4)
C9 0.021(5) 0.033(5) 0.018(5) 0.001(4) -0.006(4) -0.007(4)
C10 0.029(5) 0.031(6) 0.021(5) 0.010(4) 0.006(4) -0.004(4)
C11 0.029(5) 0.026(5) 0.039(6) 0.017(5) -0.015(5) -0.008(4)
C12 0.025(5) 0.033(6) 0.054(7) 0.004(5) -0.007(5) 0.003(4)
C13 0.036(6) 0.033(6) 0.027(5) 0.001(4) 0.005(5) -0.002(5)
C14 0.034(6) 0.027(5) 0.033(6) 0.000(5) 0.000(5) -0.006(4)
C15 0.028(5) 0.023(5) 0.016(4) 0.006(4) 0.004(4) -0.002(4)
C16 0.022(5) 0.036(6) 0.037(6) 0.000(5) -0.006(4) 0.005(4)
C17 0.026(5) 0.025(5) 0.020(5) -0.005(4) -0.010(4) 0.010(4)
C18 0.024(5) 0.031(5) 0.029(5) 0.005(4) 0.006(4) 0.005(4)
C19 0.023(5) 0.040(6) 0.024(5) 0.004(4) 0.003(4) -0.008(4)
C20 0.038(6) 0.046(7) 0.025(5) -0.001(5) 0.005(5) 0.004(5)
C21 0.044(6) 0.035(6) 0.024(5) -0.019(5) -0.005(5) 0.007(5)
C22 0.024(5) 0.036(6) 0.028(5) -0.003(5) -0.003(4) 0.003(4)
C23 0.019(5) 0.039(6) 0.012(4) 0.000(4) -0.003(4) -0.004(4)
C24 0.024(5) 0.038(6) 0.024(5) 0.004(4) -0.005(4) 0.004(4)
C25 0.035(6) 0.031(6) 0.049(7) 0.009(5) -0.011(5) 0.001(5)
C26 0.034(6) 0.049(7) 0.043(7) 0.022(6) -0.006(5) -0.010(5)
C27 0.040(6) 0.050(7) 0.029(6) 0.017(5) -0.001(5) -0.006(5)
C28 0.033(6) 0.032(6) 0.034(6) -0.002(5) -0.002(5) 0.001(5)
C29 0.024(4) 0.020(4) 0.017(4) -0.002(4) -0.004(4) 0.001(4)
N1 0.038(5) 0.022(4) 0.025(4) -0.001(4) 0.003(4) 0.000(4)
N2 0.023(4) 0.031(4) 0.026(4) 0.002(4) -0.005(3) 0.001(3)
O1 0.054(5) 0.036(4) 0.032(4) -0.005(4) -0.008(4) 0.006(4)
P1 0.0231(12) 0.0215(12) 0.0188(12) -0.0003(10) -0.0019(10) -0.0011(9)
Cl1 0.0263(12) 0.0278(12) 0.0274(13) -0.0040(10) -0.0025(10) 0.0015(10)
Pd1 0.0231(4) 0.0227(4) 0.0180(3) -0.0010(3) -0.0026(3) -0.0009(3)
C101 0.068(8) 0.039(7) 0.050(8) 0.007(6) 0.022(7) 0.017(6)
Cl11 0.0492(19) 0.077(2) 0.079(2) 0.021(2) 0.0155(18) 0.0190(17)
Cl12 0.055(2) 0.109(3) 0.088(3) 0.028(3) 0.004(2) -0.014(2)
Cl13 0.156(4) 0.0420(19) 0.057(2) 0.0069(17) 0.030(2) 0.030(2)
C102 0.034(6) 0.038(6) 0.042(7) 0.007(5) -0.003(5) 0.002(5)
Cl21 0.0461(16) 0.0326(14) 0.0508(17) 0.0009(13) -0.0003(13) 0.0019(12)
Cl22 0.0442(17) 0.086(2) 0.0480(19) 0.0080(17) -0.0080(14) -0.0191(17)
Cl23 0.0631(19) 0.0318(15) 0.061(2) 0.0102(14) 0.0145(16) 0.0057(13)

_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 O1 1.195(12) . ?
C1 N1 1.380(12) . ?
C1 C16 1.529(14) . ?
C2 N1 1.476(12) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.379(13) . ?
C3 C8 1.394(13) . ?
C3 N1 1.428(12) . ?
C4 C5 1.383(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.494(12) . ?
C9 N2 1.302(11) . ?
C9 C10 1.467(13) . ?
C10 C15 1.408(13) . ?
C10 C11 1.409(13) . ?
C11 C12 1.376(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(13) . ?
C14 H14 0.9500 . ?
C15 Pd1 2.016(9) . ?
C16 N2 1.463(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.388(13) . ?
C17 C18 1.398(13) . ?
C17 P1 1.821(9) . ?
C18 C19 1.383(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(14) . ?
C20 H20 0.9500 . ?
C21 C22 1.396(13) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.361(13) . ?
C23 C28 1.397(13) . ?
C23 P1 1.833(9) . ?
C24 C25 1.384(14) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.376(16) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(14) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C29 1.543(17) 3 ?
C29 P1 1.833(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
N2 Pd1 2.099(8) . ?
P1 Pd1 2.259(2) . ?
Cl1 Pd1 2.381(2) . ?
C101 Cl12 1.726(13) . ?
C101 Cl13 1.731(12) . ?
C101 Cl11 1.760(12) . ?
C101 H101 1.0000 . ?
C102 Cl22 1.759(11) . ?
C102 Cl21 1.770(10) . ?
C102 Cl23 1.774(11) . ?
C102 H102 1.0000 . ?

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
O1 C1 N1 123.6(10) . . ?
O1 C1 C16 122.5(9) . . ?
N1 C1 C16 113.9(8) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.8(10) . . ?
C4 C3 N1 117.7(9) . . ?
C8 C3 N1 122.5(9) . . ?
C3 C4 C5 120.7(10) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 120.1(9) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 118.6(10) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C6 C7 C8 122.1(10) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C3 118.4(9) . . ?
C7 C8 C9 120.4(9) . . ?
C3 C8 C9 121.2(8) . . ?
N2 C9 C10 115.3(8) . . ?
N2 C9 C8 121.6(9) . . ?
C10 C9 C8 123.0(8) . . ?
C15 C10 C11 120.6(9) . . ?
C15 C10 C9 116.8(8) . . ?
C11 C10 C9 122.5(9) . . ?
C12 C11 C10 121.1(9) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 118.7(9) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C12 C13 C14 120.0(10) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 122.3(9) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C10 117.2(9) . . ?
C14 C15 Pd1 130.2(7) . . ?
C10 C15 Pd1 112.5(6) . . ?
N2 C16 C1 109.1(8) . . ?
N2 C16 H16A 109.9 . . ?
C1 C16 H16A 109.9 . . ?
N2 C16 H16B 109.9 . . ?
C1 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C22 C17 C18 120.2(9) . . ?
C22 C17 P1 121.7(8) . . ?
C18 C17 P1 116.8(7) . . ?
C19 C18 C17 119.4(9) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 120.5(9) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C21 C20 C19 120.3(9) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C22 119.8(9) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C21 119.7(9) . . ?
C17 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C28 119.4(9) . . ?
C24 C23 P1 126.1(7) . . ?
C28 C23 P1 114.5(7) . . ?
C23 C24 C25 120.8(10) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C26 120.6(10) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 118.5(10) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 120.9(10) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C23 119.7(10) . . ?
C27 C28 H28 120.1 . . ?
C23 C28 H28 120.1 . . ?
C29 C29 P1 114.2(8) 3 . ?
C29 C29 H29A 108.7 3 . ?
P1 C29 H29A 108.7 . . ?
C29 C29 H29B 108.7 3 . ?
P1 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C1 N1 C3 123.8(8) . . ?
C1 N1 C2 115.6(8) . . ?
C3 N1 C2 119.5(8) . . ?
C9 N2 C16 119.0(8) . . ?
C9 N2 Pd1 114.7(6) . . ?
C16 N2 Pd1 126.3(6) . . ?
C17 P1 C23 111.2(4) . . ?
C17 P1 C29 101.4(4) . . ?
C23 P1 C29 98.5(4) . . ?
C17 P1 Pd1 113.8(3) . . ?
C23 P1 Pd1 111.8(3) . . ?
C29 P1 Pd1 118.8(3) . . ?
C15 Pd1 N2 80.5(3) . . ?
C15 Pd1 P1 93.7(3) . . ?
N2 Pd1 P1 172.4(2) . . ?
C15 Pd1 Cl1 172.7(3) . . ?
N2 Pd1 Cl1 92.5(2) . . ?
P1 Pd1 Cl1 93.43(8) . . ?
Cl12 C101 Cl13 110.9(7) . . ?
Cl12 C101 Cl11 109.7(6) . . ?
Cl13 C101 Cl11 110.9(8) . . ?
Cl12 C101 H101 108.4 . . ?
Cl13 C101 H101 108.4 . . ?
Cl11 C101 H101 108.4 . . ?
Cl22 C102 Cl21 109.9(6) . . ?
Cl22 C102 Cl23 109.3(6) . . ?
Cl21 C102 Cl23 109.4(6) . . ?
Cl22 C102 H102 109.4 . . ?
Cl21 C102 H102 109.4 . . ?
Cl23 C102 H102 109.4 . . ?

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
C8 C3 C4 C5 -4.1(14) . . . . ?
N1 C3 C4 C5 177.7(9) . . . . ?
C3 C4 C5 C6 0.3(15) . . . . ?
C4 C5 C6 C7 2.1(15) . . . . ?
C5 C6 C7 C8 -0.6(15) . . . . ?
C6 C7 C8 C3 -3.2(15) . . . . ?
C6 C7 C8 C9 179.8(9) . . . . ?
C4 C3 C8 C7 5.5(14) . . . . ?
N1 C3 C8 C7 -176.5(9) . . . . ?
C4 C3 C8 C9 -177.5(9) . . . . ?
N1 C3 C8 C9 0.6(14) . . . . ?
C7 C8 C9 N2 130.0(10) . . . . ?
C3 C8 C9 N2 -47.0(13) . . . . ?
C7 C8 C9 C10 -51.7(13) . . . . ?
C3 C8 C9 C10 131.3(9) . . . . ?
N2 C9 C10 C15 -3.0(12) . . . . ?
C8 C9 C10 C15 178.6(8) . . . . ?
N2 C9 C10 C11 172.8(9) . . . . ?
C8 C9 C10 C11 -5.6(13) . . . . ?
C15 C10 C11 C12 -2.4(14) . . . . ?
C9 C10 C11 C12 -178.1(9) . . . . ?
C10 C11 C12 C13 2.3(15) . . . . ?
C11 C12 C13 C14 -1.6(15) . . . . ?
C12 C13 C14 C15 0.8(15) . . . . ?
C13 C14 C15 C10 -0.8(14) . . . . ?
C13 C14 C15 Pd1 176.1(7) . . . . ?
C11 C10 C15 C14 1.6(13) . . . . ?
C9 C10 C15 C14 177.5(8) . . . . ?
C11 C10 C15 Pd1 -175.8(7) . . . . ?
C9 C10 C15 Pd1 0.1(10) . . . . ?
O1 C1 C16 N2 113.1(10) . . . . ?
N1 C1 C16 N2 -66.8(10) . . . . ?
C22 C17 C18 C19 -0.7(13) . . . . ?
P1 C17 C18 C19 -168.1(7) . . . . ?
C17 C18 C19 C20 0.3(14) . . . . ?
C18 C19 C20 C21 -1.5(15) . . . . ?
C19 C20 C21 C22 3.2(15) . . . . ?
C18 C17 C22 C21 2.3(14) . . . . ?
P1 C17 C22 C21 169.1(7) . . . . ?
C20 C21 C22 C17 -3.5(15) . . . . ?
C28 C23 C24 C25 2.3(14) . . . . ?
P1 C23 C24 C25 -178.4(7) . . . . ?
C23 C24 C25 C26 -0.5(15) . . . . ?
C24 C25 C26 C27 -0.5(15) . . . . ?
C25 C26 C27 C28 -0.4(16) . . . . ?
C26 C27 C28 C23 2.2(15) . . . . ?
C24 C23 C28 C27 -3.2(14) . . . . ?
P1 C23 C28 C27 177.5(8) . . . . ?
O1 C1 N1 C3 168.8(9) . . . . ?
C16 C1 N1 C3 -11.3(13) . . . . ?
O1 C1 N1 C2 1.5(14) . . . . ?
C16 C1 N1 C2 -178.6(8) . . . . ?
C4 C3 N1 C1 -131.6(10) . . . . ?
C8 C3 N1 C1 50.3(13) . . . . ?
C4 C3 N1 C2 35.3(12) . . . . ?
C8 C3 N1 C2 -142.8(9) . . . . ?
C10 C9 N2 C16 -176.3(8) . . . . ?
C8 C9 N2 C16 2.1(13) . . . . ?
C10 C9 N2 Pd1 4.3(10) . . . . ?
C8 C9 N2 Pd1 -177.2(6) . . . . ?
C1 C16 N2 C9 73.5(11) . . . . ?
C1 C16 N2 Pd1 -107.3(8) . . . . ?
C22 C17 P1 C23 46.0(9) . . . . ?
C18 C17 P1 C23 -146.7(7) . . . . ?
C22 C17 P1 C29 -57.9(8) . . . . ?
C18 C17 P1 C29 109.4(7) . . . . ?
C22 C17 P1 Pd1 173.3(7) . . . . ?
C18 C17 P1 Pd1 -19.4(8) . . . . ?
C24 C23 P1 C17 10.5(10) . . . . ?
C28 C23 P1 C17 -170.2(7) . . . . ?
C24 C23 P1 C29 116.3(8) . . . . ?
C28 C23 P1 C29 -64.4(7) . . . . ?
C24 C23 P1 Pd1 -117.9(8) . . . . ?
C28 C23 P1 Pd1 61.4(7) . . . . ?
C29 C29 P1 C17 -48.9(9) 3 . . . ?
C29 C29 P1 C23 -162.7(9) 3 . . . ?
C29 C29 P1 Pd1 76.6(9) 3 . . . ?
C14 C15 Pd1 N2 -175.4(9) . . . . ?
C10 C15 Pd1 N2 1.6(6) . . . . ?
C14 C15 Pd1 P1 9.6(8) . . . . ?
C10 C15 Pd1 P1 -173.3(6) . . . . ?
C9 N2 Pd1 Cl1 178.9(6) . . . . ?
C16 N2 Pd1 Cl1 -0.4(7) . . . . ?
C17 P1 Pd1 C15 -61.5(4) . . . . ?
C23 P1 Pd1 C15 65.5(4) . . . . ?
C29 P1 Pd1 C15 179.2(4) . . . . ?
C17 P1 Pd1 Cl1 116.8(3) . . . . ?
C23 P1 Pd1 Cl1 -116.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.870
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.168