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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pdohnth
_database_code_depnum_ccdc_archive 'CCDC 852732'
_audit_update_record             
;
2011-11-04 deposited with the CCDC.
2015-07-03 downloaded from the CCDC.
;
#TrackingRef 'PdOHNTH.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H25 N2 O2 P Pd S'
_chemical_formula_weight         662.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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

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                   15.531(5)
_cell_length_b                   10.833(3)
_cell_length_c                   17.549(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.774(3)
_cell_angle_gamma                90.00
_cell_volume                     2890.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9811
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7391
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(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  'APEX II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31660
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_reflns_number_total             6583
_reflns_number_gt                6146
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2003)'
_computing_cell_refinement       
;
APEX-II(BRUKER-NONIUS, 2003)
;
_computing_data_reduction        APEX-II
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0251P)²+1.5057P] 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         6583
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0531
_refine_ls_wR_factor_gt          0.0518
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.420566(7) 1.012291(10) 0.104749(6) 0.01746(4) Uani 1 1 d . . .
P1 P 0.35090(2) 0.86912(3) 0.16525(2) 0.01694(8) Uani 1 1 d . . .
S1 S 0.27047(3) 1.35188(4) -0.11302(2) 0.03256(10) Uani 1 1 d . . .
C24 C 0.30535(10) 0.62304(14) 0.12030(9) 0.0234(3) Uani 1 1 d . . .
H24A H 0.2471 0.6418 0.1256 0.028 Uiso 1 1 calc R . .
O2 O 0.31069(7) 1.07850(9) 0.03859(6) 0.0211(2) Uani 1 1 d . . .
N1 N 0.47166(8) 1.14145(11) 0.04912(7) 0.0194(2) Uani 1 1 d . . .
O1 O 0.53629(7) 0.95832(10) 0.16399(6) 0.0226(2) Uani 1 1 d . . .
N2 N 0.41059(8) 1.20714(11) -0.00552(7) 0.0212(2) Uani 1 1 d . . .
C12 C 0.33137(10) 1.16684(13) -0.00527(8) 0.0197(3) Uani 1 1 d . . .
C17 C 0.23250(9) 0.88948(13) 0.14598(8) 0.0200(3) Uani 1 1 d . . .
C2 C 0.62354(9) 1.11428(14) 0.11358(8) 0.0210(3) Uani 1 1 d . . .
C18 C 0.18847(10) 0.91978(15) 0.20512(9) 0.0251(3) Uani 1 1 d . . .
H18A H 0.2200 0.9242 0.2575 0.030 Uiso 1 1 calc R . .
C1 C 0.55347(10) 1.17311(14) 0.06035(8) 0.0218(3) Uani 1 1 d . . .
H1A H 0.5683 1.2407 0.0310 0.026 Uiso 1 1 calc R . .
C13 C 0.25725(10) 1.22485(13) -0.05791(8) 0.0209(3) Uani 1 1 d . . .
C16 C 0.17125(10) 1.18584(14) -0.07182(8) 0.0232(3) Uani 1 1 d . . .
H16A H 0.1511 1.1163 -0.0475 0.028 Uiso 1 1 calc R . .
C28 C 0.45675(10) 0.68368(14) 0.12990(9) 0.0240(3) Uani 1 1 d . . .
H28A H 0.5018 0.7442 0.1415 0.029 Uiso 1 1 calc R . .
C23 C 0.37116(9) 0.71233(13) 0.13706(8) 0.0191(3) Uani 1 1 d . . .
C22 C 0.18511(10) 0.88161(15) 0.06941(9) 0.0261(3) Uani 1 1 d . . .
H22A H 0.2144 0.8615 0.0285 0.031 Uiso 1 1 calc R . .
C3 C 0.61156(10) 1.00924(13) 0.15762(9) 0.0207(3) Uani 1 1 d . . .
C7 C 0.71214(10) 1.16494(15) 0.12120(9) 0.0234(3) Uani 1 1 d . . .
C21 C 0.09506(11) 0.90320(16) 0.05320(10) 0.0322(4) Uani 1 1 d . . .
H21A H 0.0625 0.8954 0.0014 0.039 Uiso 1 1 calc R . .
C19 C 0.09853(11) 0.94361(17) 0.18786(11) 0.0320(4) Uani 1 1 d . . .
H19A H 0.0689 0.9651 0.2283 0.038 Uiso 1 1 calc R . .
C29 C 0.38115(9) 0.87260(14) 0.27059(8) 0.0204(3) Uani 1 1 d . . .
C6 C 0.78438(10) 1.10236(15) 0.16755(9) 0.0256(3) Uani 1 1 d . . .
C5 C 0.76934(11) 0.99227(15) 0.20717(10) 0.0267(3) Uani 1 1 d . . .
H5A H 0.8179 0.9493 0.2373 0.032 Uiso 1 1 calc R . .
C27 C 0.47594(11) 0.56680(15) 0.10577(10) 0.0309(4) Uani 1 1 d . . .
H27A H 0.5342 0.5472 0.1010 0.037 Uiso 1 1 calc R . .
C15 C 0.11610(11) 1.26231(16) -0.12704(9) 0.0294(3) Uani 1 1 d . . .
H15A H 0.0546 1.2497 -0.1435 0.035 Uiso 1 1 calc R . .
C26 C 0.41004(12) 0.47827(15) 0.08847(11) 0.0321(4) Uani 1 1 d . . .
H26A H 0.4232 0.3984 0.0716 0.039 Uiso 1 1 calc R . .
C25 C 0.32539(12) 0.50660(14) 0.09589(10) 0.0292(3) Uani 1 1 d . . .
H25A H 0.2805 0.4458 0.0842 0.035 Uiso 1 1 calc R . .
C4 C 0.68688(10) 0.94787(15) 0.20259(9) 0.0244(3) Uani 1 1 d . . .
H4A H 0.6788 0.8744 0.2298 0.029 Uiso 1 1 calc R . .
C10 C 0.81493(11) 1.31999(17) 0.09337(10) 0.0333(4) Uani 1 1 d . . .
H10A H 0.8253 1.3943 0.0679 0.040 Uiso 1 1 calc R . .
C8 C 0.87079(11) 1.15009(17) 0.17480(10) 0.0314(4) Uani 1 1 d . . .
H8A H 0.9190 1.1072 0.2055 0.038 Uiso 1 1 calc R . .
C11 C 0.73014(11) 1.27632(16) 0.08532(9) 0.0285(3) Uani 1 1 d . . .
H11A H 0.6830 1.3219 0.0551 0.034 Uiso 1 1 calc R . .
C20 C 0.05252(10) 0.93602(16) 0.11210(11) 0.0326(4) Uani 1 1 d . . .
H20A H -0.0087 0.9534 0.1003 0.039 Uiso 1 1 calc R . .
C9 C 0.88562(11) 1.25695(18) 0.13817(11) 0.0353(4) Uani 1 1 d . . .
H9A H 0.9437 1.2880 0.1432 0.042 Uiso 1 1 calc R . .
C14 C 0.16052(11) 1.35512(17) -0.15366(10) 0.0337(4) Uani 1 1 d . . .
H14A H 0.1338 1.4150 -0.1906 0.040 Uiso 1 1 calc R . .
C34 C 0.41266(10) 0.98118(16) 0.30801(10) 0.0280(3) Uani 1 1 d . . .
H34A H 0.4255 1.0501 0.2787 0.034 Uiso 1 1 calc R . .
C30 C 0.36413(10) 0.77157(15) 0.31408(9) 0.0268(3) Uani 1 1 d . . .
H30A H 0.3435 0.6967 0.2886 0.032 Uiso 1 1 calc R . .
C33 C 0.42535(12) 0.98869(19) 0.38908(11) 0.0373(4) Uani 1 1 d . . .
H33A H 0.4466 1.0630 0.4150 0.045 Uiso 1 1 calc R . .
C31 C 0.37720(12) 0.77972(18) 0.39457(10) 0.0350(4) Uani 1 1 d . . .
H31A H 0.3655 0.7105 0.4242 0.042 Uiso 1 1 calc R . .
C32 C 0.40710(11) 0.8883(2) 0.43138(10) 0.0383(4) Uani 1 1 d . . .
H32A H 0.4152 0.8941 0.4864 0.046 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 1.9638(12) . ?
Pd1 O1 1.9724(11) . ?
Pd1 O2 1.9914(11) . ?
Pd1 P1 2.2743(5) . ?
P1 C29 1.8126(16) . ?
P1 C17 1.8141(15) . ?
P1 C23 1.8144(15) . ?
S1 C14 1.7114(18) . ?
S1 C13 1.7183(15) . ?
C24 C25 1.388(2) . ?
C24 C23 1.394(2) . ?
C24 H24A 0.9500 . ?
O2 C12 1.3085(17) . ?
N1 C1 1.2919(19) . ?
N1 N2 1.3980(17) . ?
O1 C3 1.3179(18) . ?
N2 C12 1.3063(19) . ?
C12 C13 1.463(2) . ?
C17 C18 1.394(2) . ?
C17 C22 1.397(2) . ?
C2 C3 1.409(2) . ?
C2 C1 1.431(2) . ?
C2 C7 1.462(2) . ?
C18 C19 1.392(2) . ?
C18 H18A 0.9500 . ?
C1 H1A 0.9500 . ?
C13 C16 1.374(2) . ?
C16 C15 1.421(2) . ?
C16 H16A 0.9500 . ?
C28 C27 1.387(2) . ?
C28 C23 1.396(2) . ?
C28 H28A 0.9500 . ?
C22 C21 1.389(2) . ?
C22 H22A 0.9500 . ?
C3 C4 1.434(2) . ?
C7 C11 1.415(2) . ?
C7 C6 1.417(2) . ?
C21 C20 1.382(3) . ?
C21 H21A 0.9500 . ?
C19 C20 1.377(3) . ?
C19 H19A 0.9500 . ?
C29 C34 1.387(2) . ?
C29 C30 1.390(2) . ?
C6 C8 1.420(2) . ?
C6 C5 1.424(2) . ?
C5 C4 1.355(2) . ?
C5 H5A 0.9500 . ?
C27 C26 1.390(2) . ?
C27 H27A 0.9500 . ?
C15 C14 1.355(2) . ?
C15 H15A 0.9500 . ?
C26 C25 1.382(3) . ?
C26 H26A 0.9500 . ?
C25 H25A 0.9500 . ?
C4 H4A 0.9500 . ?
C10 C11 1.379(2) . ?
C10 C9 1.392(3) . ?
C10 H10A 0.9500 . ?
C8 C9 1.366(3) . ?
C8 H8A 0.9500 . ?
C11 H11A 0.9500 . ?
C20 H20A 0.9500 . ?
C9 H9A 0.9500 . ?
C14 H14A 0.9500 . ?
C34 C33 1.398(3) . ?
C34 H34A 0.9500 . ?
C30 C31 1.388(2) . ?
C30 H30A 0.9500 . ?
C33 C32 1.378(3) . ?
C33 H33A 0.9500 . ?
C31 C32 1.376(3) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?

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 Pd1 O1 93.21(5) . . ?
N1 Pd1 O2 80.72(5) . . ?
O1 Pd1 O2 173.89(4) . . ?
N1 Pd1 P1 175.52(4) . . ?
O1 Pd1 P1 91.20(4) . . ?
O2 Pd1 P1 94.88(4) . . ?
C29 P1 C17 103.27(7) . . ?
C29 P1 C23 105.92(7) . . ?
C17 P1 C23 106.78(7) . . ?
C29 P1 Pd1 114.39(5) . . ?
C17 P1 Pd1 113.00(5) . . ?
C23 P1 Pd1 112.68(5) . . ?
C14 S1 C13 91.56(8) . . ?
C25 C24 C23 119.65(15) . . ?
C25 C24 H24A 120.2 . . ?
C23 C24 H24A 120.2 . . ?
C12 O2 Pd1 108.80(9) . . ?
C1 N1 N2 118.56(12) . . ?
C1 N1 Pd1 126.72(11) . . ?
N2 N1 Pd1 114.66(9) . . ?
C3 O1 Pd1 124.05(10) . . ?
C12 N2 N1 109.59(12) . . ?
N2 C12 O2 126.21(14) . . ?
N2 C12 C13 118.34(13) . . ?
O2 C12 C13 115.44(13) . . ?
C18 C17 C22 119.25(14) . . ?
C18 C17 P1 121.50(11) . . ?
C22 C17 P1 119.14(11) . . ?
C3 C2 C1 123.34(13) . . ?
C3 C2 C7 118.69(14) . . ?
C1 C2 C7 117.95(13) . . ?
C19 C18 C17 120.32(15) . . ?
C19 C18 H18A 119.8 . . ?
C17 C18 H18A 119.8 . . ?
N1 C1 C2 125.08(14) . . ?
N1 C1 H1A 117.5 . . ?
C2 C1 H1A 117.5 . . ?
C16 C13 C12 126.24(13) . . ?
C16 C13 S1 111.70(11) . . ?
C12 C13 S1 122.04(11) . . ?
C13 C16 C15 111.75(14) . . ?
C13 C16 H16A 124.1 . . ?
C15 C16 H16A 124.1 . . ?
C27 C28 C23 119.91(14) . . ?
C27 C28 H28A 120.0 . . ?
C23 C28 H28A 120.0 . . ?
C24 C23 C28 119.83(14) . . ?
C24 C23 P1 123.13(11) . . ?
C28 C23 P1 117.01(11) . . ?
C21 C22 C17 119.84(15) . . ?
C21 C22 H22A 120.1 . . ?
C17 C22 H22A 120.1 . . ?
O1 C3 C2 127.10(14) . . ?
O1 C3 C4 113.42(13) . . ?
C2 C3 C4 119.47(14) . . ?
C11 C7 C6 117.27(14) . . ?
C11 C7 C2 123.17(15) . . ?
C6 C7 C2 119.55(14) . . ?
C20 C21 C22 120.34(15) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C20 C19 C18 119.93(16) . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C34 C29 C30 119.74(14) . . ?
C34 C29 P1 119.58(12) . . ?
C30 C29 P1 120.32(12) . . ?
C7 C6 C8 120.04(16) . . ?
C7 C6 C5 119.45(14) . . ?
C8 C6 C5 120.51(16) . . ?
C4 C5 C6 121.05(15) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
C28 C27 C26 120.14(15) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C14 C15 C16 112.90(15) . . ?
C14 C15 H15A 123.6 . . ?
C16 C15 H15A 123.6 . . ?
C25 C26 C27 119.90(15) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C26 C25 C24 120.57(15) . . ?
C26 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
C5 C4 C3 121.54(15) . . ?
C5 C4 H4A 119.2 . . ?
C3 C4 H4A 119.2 . . ?
C11 C10 C9 121.08(17) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C9 C8 C6 120.89(17) . . ?
C9 C8 H8A 119.6 . . ?
C6 C8 H8A 119.6 . . ?
C10 C11 C7 121.21(16) . . ?
C10 C11 H11A 119.4 . . ?
C7 C11 H11A 119.4 . . ?
C19 C20 C21 120.28(15) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C8 C9 C10 119.48(15) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
C15 C14 S1 112.08(13) . . ?
C15 C14 H14A 124.0 . . ?
S1 C14 H14A 124.0 . . ?
C29 C34 C33 119.61(16) . . ?
C29 C34 H34A 120.2 . . ?
C33 C34 H34A 120.2 . . ?
C31 C30 C29 120.25(16) . . ?
C31 C30 H30A 119.9 . . ?
C29 C30 H30A 119.9 . . ?
C32 C33 C34 120.02(17) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C32 C31 C30 119.81(17) . . ?
C32 C31 H31A 120.1 . . ?
C30 C31 H31A 120.1 . . ?
C31 C32 C33 120.56(16) . . ?
C31 C32 H32A 119.7 . . ?
C33 C32 H32A 119.7 . . ?

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
N1 Pd1 P1 C29 -118.2(5) . . . . ?
O1 Pd1 P1 C29 52.15(6) . . . . ?
O2 Pd1 P1 C29 -128.50(6) . . . . ?
N1 Pd1 P1 C17 -0.4(5) . . . . ?
O1 Pd1 P1 C17 169.94(6) . . . . ?
O2 Pd1 P1 C17 -10.71(6) . . . . ?
N1 Pd1 P1 C23 120.7(5) . . . . ?
O1 Pd1 P1 C23 -68.91(6) . . . . ?
O2 Pd1 P1 C23 110.44(6) . . . . ?
N1 Pd1 O2 C12 1.13(9) . . . . ?
O1 Pd1 O2 C12 -5.8(4) . . . . ?
P1 Pd1 O2 C12 -179.68(8) . . . . ?
O1 Pd1 N1 C1 -4.89(13) . . . . ?
O2 Pd1 N1 C1 175.85(13) . . . . ?
P1 Pd1 N1 C1 165.4(4) . . . . ?
O1 Pd1 N1 N2 177.92(9) . . . . ?
O2 Pd1 N1 N2 -1.34(9) . . . . ?
P1 Pd1 N1 N2 -11.8(5) . . . . ?
N1 Pd1 O1 C3 0.75(12) . . . . ?
O2 Pd1 O1 C3 7.6(5) . . . . ?
P1 Pd1 O1 C3 -178.50(11) . . . . ?
C1 N1 N2 C12 -176.20(13) . . . . ?
Pd1 N1 N2 C12 1.24(14) . . . . ?
N1 N2 C12 O2 -0.2(2) . . . . ?
N1 N2 C12 C13 179.22(12) . . . . ?
Pd1 O2 C12 N2 -0.86(17) . . . . ?
Pd1 O2 C12 C13 179.69(9) . . . . ?
C29 P1 C17 C18 8.83(14) . . . . ?
C23 P1 C17 C18 120.26(13) . . . . ?
Pd1 P1 C17 C18 -115.30(12) . . . . ?
C29 P1 C17 C22 -174.92(12) . . . . ?
C23 P1 C17 C22 -63.49(13) . . . . ?
Pd1 P1 C17 C22 60.96(13) . . . . ?
C22 C17 C18 C19 -0.9(2) . . . . ?
P1 C17 C18 C19 175.34(13) . . . . ?
N2 N1 C1 C2 -179.42(13) . . . . ?
Pd1 N1 C1 C2 3.5(2) . . . . ?
C3 C2 C1 N1 3.4(2) . . . . ?
C7 C2 C1 N1 -177.76(14) . . . . ?
N2 C12 C13 C16 172.18(14) . . . . ?
O2 C12 C13 C16 -8.3(2) . . . . ?
N2 C12 C13 S1 -5.85(19) . . . . ?
O2 C12 C13 S1 173.64(10) . . . . ?
C14 S1 C13 C16 1.04(13) . . . . ?
C14 S1 C13 C12 179.33(13) . . . . ?
C12 C13 C16 C15 -179.22(14) . . . . ?
S1 C13 C16 C15 -1.01(17) . . . . ?
C25 C24 C23 C28 -0.6(2) . . . . ?
C25 C24 C23 P1 177.22(12) . . . . ?
C27 C28 C23 C24 0.3(2) . . . . ?
C27 C28 C23 P1 -177.63(13) . . . . ?
C29 P1 C23 C24 97.56(13) . . . . ?
C17 P1 C23 C24 -12.02(14) . . . . ?
Pd1 P1 C23 C24 -136.66(11) . . . . ?
C29 P1 C23 C28 -84.55(12) . . . . ?
C17 P1 C23 C28 165.87(11) . . . . ?
Pd1 P1 C23 C28 41.23(13) . . . . ?
C18 C17 C22 C21 -0.4(2) . . . . ?
P1 C17 C22 C21 -176.73(12) . . . . ?
Pd1 O1 C3 C2 5.2(2) . . . . ?
Pd1 O1 C3 C4 -175.76(9) . . . . ?
C1 C2 C3 O1 -8.2(2) . . . . ?
C7 C2 C3 O1 172.99(14) . . . . ?
C1 C2 C3 C4 172.75(13) . . . . ?
C7 C2 C3 C4 -6.0(2) . . . . ?
C3 C2 C7 C11 -173.94(14) . . . . ?
C1 C2 C7 C11 7.2(2) . . . . ?
C3 C2 C7 C6 4.9(2) . . . . ?
C1 C2 C7 C6 -173.97(13) . . . . ?
C17 C22 C21 C20 1.9(2) . . . . ?
C17 C18 C19 C20 0.7(3) . . . . ?
C17 P1 C29 C34 -98.03(13) . . . . ?
C23 P1 C29 C34 149.91(12) . . . . ?
Pd1 P1 C29 C34 25.19(13) . . . . ?
C17 P1 C29 C30 75.05(13) . . . . ?
C23 P1 C29 C30 -37.02(14) . . . . ?
Pd1 P1 C29 C30 -161.74(10) . . . . ?
C11 C7 C6 C8 -1.7(2) . . . . ?
C2 C7 C6 C8 179.43(14) . . . . ?
C11 C7 C6 C5 177.74(14) . . . . ?
C2 C7 C6 C5 -1.2(2) . . . . ?
C7 C6 C5 C4 -1.4(2) . . . . ?
C8 C6 C5 C4 177.98(15) . . . . ?
C23 C28 C27 C26 0.2(3) . . . . ?
C13 C16 C15 C14 0.4(2) . . . . ?
C28 C27 C26 C25 -0.5(3) . . . . ?
C27 C26 C25 C24 0.2(3) . . . . ?
C23 C24 C25 C26 0.4(2) . . . . ?
C6 C5 C4 C3 0.2(2) . . . . ?
O1 C3 C4 C5 -175.56(14) . . . . ?
C2 C3 C4 C5 3.6(2) . . . . ?
C7 C6 C8 C9 0.7(2) . . . . ?
C5 C6 C8 C9 -178.74(15) . . . . ?
C9 C10 C11 C7 -1.1(3) . . . . ?
C6 C7 C11 C10 1.9(2) . . . . ?
C2 C7 C11 C10 -179.26(15) . . . . ?
C18 C19 C20 C21 0.9(3) . . . . ?
C22 C21 C20 C19 -2.2(3) . . . . ?
C6 C8 C9 C10 0.2(3) . . . . ?
C11 C10 C9 C8 0.0(3) . . . . ?
C16 C15 C14 S1 0.4(2) . . . . ?
C13 S1 C14 C15 -0.80(15) . . . . ?
C30 C29 C34 C33 -1.3(2) . . . . ?
P1 C29 C34 C33 171.85(13) . . . . ?
C34 C29 C30 C31 1.1(2) . . . . ?
P1 C29 C30 C31 -172.01(12) . . . . ?
C29 C34 C33 C32 0.4(3) . . . . ?
C29 C30 C31 C32 0.0(2) . . . . ?
C30 C31 C32 C33 -0.9(3) . . . . ?
C34 C33 C32 C31 0.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.050


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pdohfh_0ma
_database_code_depnum_ccdc_archive 'CCDC 1005675'
_audit_update_record             
;
2014-05-28 deposited with the CCDC.
2015-07-03 downloaded from the CCDC.
;

_audit_creation_date             2014-04-23T13:06:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 pdohfhb
;
_chemical_name_common            pdohfhb
_chemical_formula_moiety         'C34 H25 N2 O3 P Pd'
_chemical_formula_sum            'C34 H25 N2 O3 P Pd'
_chemical_formula_weight         646.93

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
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                   15.5191(14)
_cell_length_b                   9.0388(8)
_cell_length_c                   19.9113(17)
_cell_angle_alpha                90
_cell_angle_beta                 97.858(3)
_cell_angle_gamma                90
_cell_volume                     2766.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    440
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_special_details           
;
 10 seconds. 0.5 degrees, 40 mm
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.8805
_exptl_absorpt_correction_T_max  0.9482

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.023
_diffrn_reflns_number            88216
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             6860
_reflns_number_gt                5829
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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 > 2σ(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)+(0.0422P)²+1.8259P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6860
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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 0.42828(13) 0.2744(2) 0.92111(10) 0.0171(4) Uani 1 1 d . . .
C2 C 0.34461(14) 0.2090(2) 0.90028(10) 0.0210(4) Uani 1 1 d . . .
H2 H 0.3137 0.2337 0.8572 0.025 Uiso 1 1 calc R . .
C3 C 0.30892(14) 0.1129(2) 0.94063(11) 0.0222(4) Uani 1 1 d . . .
H3 H 0.2529 0.0733 0.9257 0.027 Uiso 1 1 calc R . .
C4 C 0.35333(14) 0.0697(2) 1.00485(10) 0.0196(4) Uani 1 1 d . . .
C5 C 0.31602(15) -0.0353(2) 1.04535(11) 0.0222(4) Uani 1 1 d . . .
H5 H 0.2596 -0.0733 1.0304 0.027 Uiso 1 1 calc R . .
C6 C 0.36034(14) -0.0826(2) 1.10577(11) 0.0227(4) Uani 1 1 d . . .
H6 H 0.3351 -0.1535 1.1324 0.027 Uiso 1 1 calc R . .
C7 C 0.44309(15) -0.0256(2) 1.12791(11) 0.0215(4) Uani 1 1 d . . .
H7 H 0.4742 -0.059 1.1696 0.026 Uiso 1 1 calc R . .
C8 C 0.48020(14) 0.0787(2) 1.09010(10) 0.0194(4) Uani 1 1 d . . .
H8 H 0.5364 0.1159 1.1064 0.023 Uiso 1 1 calc R . .
C9 C 0.43647(13) 0.1314(2) 1.02762(10) 0.0172(4) Uani 1 1 d . . .
C10 C 0.47397(13) 0.2397(2) 0.98544(10) 0.0167(4) Uani 1 1 d . . .
C11 C 0.55630(13) 0.3033(2) 1.01115(10) 0.0176(4) Uani 1 1 d . . .
H11 H 0.582 0.2734 1.0551 0.021 Uiso 1 1 calc R . .
C12 C 0.71199(13) 0.5420(2) 0.97154(10) 0.0179(4) Uani 1 1 d . . .
C13 C 0.79442(14) 0.6161(2) 0.99352(10) 0.0207(4) Uani 1 1 d . . .
C14 C 0.83924(15) 0.7149(3) 0.96050(12) 0.0268(5) Uani 1 1 d . . .
H14 H 0.8241 0.7494 0.9153 0.032 Uiso 1 1 calc R . .
C15 C 0.91335(16) 0.7569(3) 1.00676(12) 0.0317(5) Uani 1 1 d . . .
H15 H 0.9575 0.8248 0.9986 0.038 Uiso 1 1 calc R . .
C16 C 0.90842(15) 0.6814(3) 1.06406(13) 0.0314(5) Uani 1 1 d . . .
H16 H 0.9497 0.6882 1.1038 0.038 Uiso 1 1 calc R . .
C17 C 0.60438(13) 0.6810(2) 0.74326(10) 0.0179(4) Uani 1 1 d . . .
C18 C 0.65733(13) 0.7782(2) 0.78511(11) 0.0204(4) Uani 1 1 d . . .
H18 H 0.6562 0.7771 0.8327 0.025 Uiso 1 1 calc R . .
C19 C 0.71167(14) 0.8765(3) 0.75723(12) 0.0251(5) Uani 1 1 d . . .
H19 H 0.7474 0.9424 0.7859 0.03 Uiso 1 1 calc R . .
C20 C 0.71400(14) 0.8791(3) 0.68782(12) 0.0269(5) Uani 1 1 d . . .
H20 H 0.7504 0.9477 0.6689 0.032 Uiso 1 1 calc R . .
C21 C 0.66272(15) 0.7807(3) 0.64611(11) 0.0266(5) Uani 1 1 d . . .
H21 H 0.6649 0.781 0.5986 0.032 Uiso 1 1 calc R . .
C22 C 0.60824(14) 0.6815(2) 0.67353(11) 0.0220(4) Uani 1 1 d . . .
H22 H 0.5736 0.6142 0.6448 0.026 Uiso 1 1 calc R . .
C23 C 0.43052(13) 0.6921(2) 0.77684(9) 0.0168(4) Uani 1 1 d . . .
C24 C 0.42751(14) 0.8303(2) 0.74560(10) 0.0214(4) Uani 1 1 d . . .
H24 H 0.475 0.8622 0.7238 0.026 Uiso 1 1 calc R . .
C25 C 0.35573(15) 0.9218(3) 0.74610(11) 0.0273(5) Uani 1 1 d . . .
H25 H 0.3539 1.0152 0.7241 0.033 Uiso 1 1 calc R . .
C26 C 0.28680(14) 0.8771(3) 0.77862(11) 0.0257(5) Uani 1 1 d . . .
H26 H 0.2376 0.9396 0.7789 0.031 Uiso 1 1 calc R . .
C28 C 0.28982(14) 0.7405(2) 0.81088(11) 0.0229(4) Uani 1 1 d . . .
H28 H 0.2428 0.7106 0.8337 0.027 Uiso 1 1 calc R . .
C29 C 0.36067(13) 0.6474(2) 0.81007(10) 0.0193(4) Uani 1 1 d . . .
H29 H 0.362 0.5539 0.8319 0.023 Uiso 1 1 calc R . .
C30 C 0.49365(13) 0.4265(2) 0.71832(10) 0.0175(4) Uani 1 1 d . . .
C31 C 0.42649(14) 0.4445(3) 0.66504(11) 0.0227(4) Uani 1 1 d . . .
H31 H 0.393 0.5328 0.6616 0.027 Uiso 1 1 calc R . .
C32 C 0.40827(15) 0.3337(3) 0.61685(11) 0.0272(5) Uani 1 1 d . . .
H32 H 0.3623 0.3464 0.5806 0.033 Uiso 1 1 calc R . .
C33 C 0.45706(16) 0.2047(3) 0.62153(12) 0.0295(5) Uani 1 1 d . . .
H33 H 0.4443 0.129 0.5886 0.035 Uiso 1 1 calc R . .
C34 C 0.52469(16) 0.1859(2) 0.67440(12) 0.0282(5) Uani 1 1 d . . .
H34 H 0.5587 0.0981 0.6773 0.034 Uiso 1 1 calc R . .
C35 C 0.54216(14) 0.2959(2) 0.72279(11) 0.0224(4) Uani 1 1 d . . .
H35 H 0.5876 0.2823 0.7594 0.027 Uiso 1 1 calc R . .
N1 N 0.59888(11) 0.39850(18) 0.97939(8) 0.0161(3) Uani 1 1 d . . .
N2 N 0.67941(11) 0.44892(19) 1.01157(8) 0.0191(4) Uani 1 1 d . . .
O1 O 0.45400(9) 0.36261(16) 0.87492(7) 0.0197(3) Uani 1 1 d . . .
O2 O 0.67689(9) 0.57989(16) 0.91012(7) 0.0180(3) Uani 1 1 d . . .
O3 O 0.83592(10) 0.59326(18) 1.05774(8) 0.0267(3) Uani 1 1 d . . .
P1 P 0.52496(3) 0.57081(6) 0.78059(2) 0.01532(10) Uani 1 1 d . . .
Pd1 Pd 0.563411(9) 0.476051(17) 0.887448(7) 0.01471(6) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.320(2) . ?
C1 C10 1.412(3) . ?
C1 C2 1.435(3) . ?
C2 C3 1.352(3) . ?
C2 H2 0.95 . ?
C3 C4 1.422(3) . ?
C3 H3 0.95 . ?
C4 C5 1.419(3) . ?
C4 C9 1.422(3) . ?
C5 C6 1.370(3) . ?
C5 H5 0.95 . ?
C6 C7 1.398(3) . ?
C6 H6 0.95 . ?
C7 C8 1.380(3) . ?
C7 H7 0.95 . ?
C8 C9 1.416(3) . ?
C8 H8 0.95 . ?
C9 C10 1.462(3) . ?
C10 C11 1.430(3) . ?
C11 N1 1.301(3) . ?
C11 H11 0.95 . ?
C12 N2 1.307(3) . ?
C12 O2 1.314(2) . ?
C12 C13 1.457(3) . ?
C13 C14 1.356(3) . ?
C13 O3 1.366(2) . ?
C14 C15 1.423(3) . ?
C14 H14 0.95 . ?
C15 C16 1.340(3) . ?
C15 H15 0.95 . ?
C16 O3 1.371(3) . ?
C16 H16 0.95 . ?
C17 C22 1.398(3) . ?
C17 C18 1.398(3) . ?
C17 P1 1.820(2) . ?
C18 C19 1.392(3) . ?
C18 H18 0.95 . ?
C19 C20 1.388(3) . ?
C19 H19 0.95 . ?
C20 C21 1.391(3) . ?
C20 H20 0.95 . ?
C21 C22 1.394(3) . ?
C21 H21 0.95 . ?
C22 H22 0.95 . ?
C23 C24 1.393(3) . ?
C23 C29 1.404(3) . ?
C23 P1 1.824(2) . ?
C24 C25 1.388(3) . ?
C24 H24 0.95 . ?
C25 C26 1.384(3) . ?
C25 H25 0.95 . ?
C26 C28 1.390(3) . ?
C26 H26 0.95 . ?
C28 C29 1.386(3) . ?
C28 H28 0.95 . ?
C29 H29 0.95 . ?
C30 C31 1.391(3) . ?
C30 C35 1.397(3) . ?
C30 P1 1.819(2) . ?
C31 C32 1.389(3) . ?
C31 H31 0.95 . ?
C32 C33 1.386(4) . ?
C32 H32 0.95 . ?
C33 C34 1.392(3) . ?
C33 H33 0.95 . ?
C34 C35 1.386(3) . ?
C34 H34 0.95 . ?
C35 H35 0.95 . ?
N1 N2 1.400(2) . ?
N1 Pd1 1.9674(16) . ?
O1 Pd1 1.9700(14) . ?
O2 Pd1 1.9922(14) . ?
P1 Pd1 2.2956(5) . ?

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 C10 127.17(18) . . ?
O1 C1 C2 113.30(17) . . ?
C10 C1 C2 119.53(18) . . ?
C3 C2 C1 121.39(19) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 121.5(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C9 120.26(19) . . ?
C5 C4 C3 120.61(19) . . ?
C9 C4 C3 119.12(18) . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 119.4(2) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C8 C7 C6 120.9(2) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 121.6(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C4 116.97(18) . . ?
C8 C9 C10 123.34(19) . . ?
C4 C9 C10 119.64(18) . . ?
C1 C10 C11 123.28(18) . . ?
C1 C10 C9 118.68(18) . . ?
C11 C10 C9 118.02(18) . . ?
N1 C11 C10 125.47(18) . . ?
N1 C11 H11 117.3 . . ?
C10 C11 H11 117.3 . . ?
N2 C12 O2 126.11(19) . . ?
N2 C12 C13 120.62(18) . . ?
O2 C12 C13 113.27(17) . . ?
C14 C13 O3 110.22(19) . . ?
C14 C13 C12 130.1(2) . . ?
O3 C13 C12 119.60(18) . . ?
C13 C14 C15 106.5(2) . . ?
C13 C14 H14 126.7 . . ?
C15 C14 H14 126.7 . . ?
C16 C15 C14 106.3(2) . . ?
C16 C15 H15 126.9 . . ?
C14 C15 H15 126.9 . . ?
C15 C16 O3 111.1(2) . . ?
C15 C16 H16 124.5 . . ?
O3 C16 H16 124.5 . . ?
C22 C17 C18 119.23(19) . . ?
C22 C17 P1 122.06(16) . . ?
C18 C17 P1 118.42(15) . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 120.5(2) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 119.6(2) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C20 C21 C22 120.4(2) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.1(2) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C24 C23 C29 119.16(19) . . ?
C24 C23 P1 122.34(15) . . ?
C29 C23 P1 118.40(15) . . ?
C25 C24 C23 120.58(19) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C28 119.7(2) . . ?
C25 C26 H26 120.1 . . ?
C28 C26 H26 120.1 . . ?
C29 C28 C26 120.7(2) . . ?
C29 C28 H28 119.6 . . ?
C26 C28 H28 119.6 . . ?
C28 C29 C23 119.7(2) . . ?
C28 C29 H29 120.1 . . ?
C23 C29 H29 120.1 . . ?
C31 C30 C35 119.2(2) . . ?
C31 C30 P1 122.57(16) . . ?
C35 C30 P1 118.11(16) . . ?
C32 C31 C30 120.2(2) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C32 C33 C34 120.2(2) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 119.6(2) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C34 C35 C30 120.7(2) . . ?
C34 C35 H35 119.7 . . ?
C30 C35 H35 119.7 . . ?
C11 N1 N2 118.29(16) . . ?
C11 N1 Pd1 126.31(14) . . ?
N2 N1 Pd1 115.37(12) . . ?
C12 N2 N1 109.02(16) . . ?
C1 O1 Pd1 124.33(13) . . ?
C12 O2 Pd1 109.22(12) . . ?
C13 O3 C16 105.92(17) . . ?
C30 P1 C17 104.27(9) . . ?
C30 P1 C23 105.36(9) . . ?
C17 P1 C23 103.87(9) . . ?
C30 P1 Pd1 112.06(7) . . ?
C17 P1 Pd1 118.55(7) . . ?
C23 P1 Pd1 111.59(6) . . ?
N1 Pd1 O1 93.38(6) . . ?
N1 Pd1 O2 80.26(6) . . ?
O1 Pd1 O2 173.64(6) . . ?
N1 Pd1 P1 178.52(5) . . ?
O1 Pd1 P1 88.08(4) . . ?
O2 Pd1 P1 98.28(4) . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ndb
_database_code_depnum_ccdc_archive 'CCDC 1017037'
_audit_update_record             
;
2014-07-30 deposited with the CCDC.
2015-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H26 N3 O2 P Pd'
_chemical_formula_weight         657.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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

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                   15.3735(13)
_cell_length_b                   8.9176(8)
_cell_length_c                   20.6686(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.251(5)
_cell_angle_gamma                90.00
_cell_volume                     2810.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3753
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      62.80

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    6.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4579
_exptl_absorpt_correction_T_max  0.8365
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21167
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.31
_diffrn_reflns_theta_max         59.99
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_reflns_number_total             3994
_reflns_number_gt                3256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_cell_refinement       
; 
  CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) 
;
_computing_data_reduction        'Bruker APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; calc 
 [0.00000+1.00000exp(1.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0472P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00109(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3994
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.566549(15) 0.51703(3) 0.885751(11) 0.01739(11) Uani 1 1 d . . .
P1 P 0.52696(5) 0.42798(9) 0.78179(4) 0.0176(2) Uani 1 1 d . . .
C1 C 0.5574(2) 0.6853(4) 1.00629(17) 0.0205(8) Uani 1 1 d . . .
H1A H 0.5821 0.7118 1.0492 0.025 Uiso 1 1 calc R . .
C2 C 0.4763(2) 0.7552(4) 0.98146(17) 0.0192(7) Uani 1 1 d . . .
C3 C 0.4333(2) 0.7286(4) 0.91839(17) 0.0204(8) Uani 1 1 d . . .
C4 C 0.3519(2) 0.8027(4) 0.89693(18) 0.0231(8) Uani 1 1 d . . .
H4A H 0.3228 0.7828 0.8545 0.028 Uiso 1 1 calc R . .
C5 C 0.3156(2) 0.9001(4) 0.93584(17) 0.0252(8) Uani 1 1 d . . .
H5A H 0.2615 0.9467 0.9203 0.030 Uiso 1 1 calc R . .
C6 C 0.3568(2) 0.9343(4) 0.99962(17) 0.0218(8) Uani 1 1 d . . .
C7 C 0.4381(2) 0.8637(4) 1.02294(16) 0.0190(7) Uani 1 1 d . . .
C8 C 0.3193(2) 1.0386(4) 1.03934(18) 0.0249(8) Uani 1 1 d . . .
H8A H 0.2649 1.0842 1.0233 0.030 Uiso 1 1 calc R . .
C9 C 0.3588(2) 1.0759(4) 1.10010(18) 0.0268(8) Uani 1 1 d . . .
H9A H 0.3322 1.1451 1.1265 0.032 Uiso 1 1 calc R . .
C10 C 0.4402(2) 1.0093(4) 1.12268(17) 0.0245(8) Uani 1 1 d . . .
H10A H 0.4694 1.0359 1.1644 0.029 Uiso 1 1 calc R . .
C11 C 0.4778(2) 0.9067(4) 1.08533(16) 0.0209(8) Uani 1 1 d . . .
H11A H 0.5325 0.8632 1.1021 0.025 Uiso 1 1 calc R . .
C12 C 0.7124(2) 0.4385(4) 0.96783(16) 0.0183(7) Uani 1 1 d . . .
C13 C 0.7955(2) 0.3602(4) 0.99170(17) 0.0216(8) Uani 1 1 d . . .
C14 C 0.8410(2) 0.3867(4) 1.05286(19) 0.0305(9) Uani 1 1 d . . .
H14A H 0.8202 0.4590 1.0810 0.037 Uiso 1 1 calc R . .
C15 C 0.9164(3) 0.3076(5) 1.0725(2) 0.0377(10) Uani 1 1 d . . .
H15A H 0.9478 0.3316 1.1138 0.045 Uiso 1 1 calc R . .
C16 C 0.9045(2) 0.1722(4) 0.97940(19) 0.0301(9) Uani 1 1 d . . .
H16A H 0.9254 0.0958 0.9533 0.036 Uiso 1 1 calc R . .
C17 C 0.8296(2) 0.2492(4) 0.95478(18) 0.0267(8) Uani 1 1 d . . .
H17A H 0.8011 0.2262 0.9124 0.032 Uiso 1 1 calc R . .
C18 C 0.6056(2) 0.3153(4) 0.74358(17) 0.0193(7) Uani 1 1 d . . .
C19 C 0.6605(2) 0.2196(4) 0.78297(18) 0.0229(8) Uani 1 1 d . . .
H19A H 0.6607 0.2216 0.8289 0.027 Uiso 1 1 calc R . .
C20 C 0.7153(2) 0.1208(4) 0.7553(2) 0.0306(9) Uani 1 1 d . . .
H20A H 0.7523 0.0548 0.7823 0.037 Uiso 1 1 calc R . .
C21 C 0.7160(2) 0.1185(4) 0.6881(2) 0.0318(9) Uani 1 1 d . . .
H21A H 0.7532 0.0509 0.6691 0.038 Uiso 1 1 calc R . .
C22 C 0.6619(2) 0.2157(4) 0.64897(19) 0.0296(9) Uani 1 1 d . . .
H22A H 0.6624 0.2143 0.6031 0.035 Uiso 1 1 calc R . .
C23 C 0.6069(2) 0.3151(4) 0.67619(17) 0.0224(8) Uani 1 1 d . . .
H23A H 0.5705 0.3821 0.6492 0.027 Uiso 1 1 calc R . .
C24 C 0.4304(2) 0.3068(4) 0.77834(16) 0.0186(7) Uani 1 1 d . . .
C25 C 0.4271(2) 0.1674(4) 0.74933(17) 0.0250(8) Uani 1 1 d . . .
H25A H 0.4751 0.1342 0.7282 0.030 Uiso 1 1 calc R . .
C26 C 0.3548(2) 0.0749(4) 0.75057(19) 0.0322(9) Uani 1 1 d . . .
H26A H 0.3532 -0.0209 0.7303 0.039 Uiso 1 1 calc R . .
C27 C 0.2851(2) 0.1225(4) 0.78143(19) 0.0302(9) Uani 1 1 d . . .
H27A H 0.2351 0.0602 0.7818 0.036 Uiso 1 1 calc R . .
C28 C 0.2881(2) 0.2603(4) 0.81169(18) 0.0272(8) Uani 1 1 d . . .
H28A H 0.2405 0.2918 0.8335 0.033 Uiso 1 1 calc R . .
C29 C 0.3601(2) 0.3536(4) 0.81066(17) 0.0236(8) Uani 1 1 d . . .
H29A H 0.3618 0.4485 0.8317 0.028 Uiso 1 1 calc R . .
C30 C 0.4968(2) 0.5772(4) 0.72358(16) 0.0204(8) Uani 1 1 d . . .
C31 C 0.4332(2) 0.5586(4) 0.66962(18) 0.0258(8) Uani 1 1 d . . .
H31A H 0.3995 0.4690 0.6650 0.031 Uiso 1 1 calc R . .
C32 C 0.4191(2) 0.6699(5) 0.62308(19) 0.0317(9) Uani 1 1 d . . .
H32A H 0.3755 0.6567 0.5866 0.038 Uiso 1 1 calc R . .
C33 C 0.4680(3) 0.8005(5) 0.6293(2) 0.0353(10) Uani 1 1 d . . .
H33A H 0.4584 0.8763 0.5969 0.042 Uiso 1 1 calc R . .
C34 C 0.5314(3) 0.8207(4) 0.6831(2) 0.0323(9) Uani 1 1 d . . .
H34A H 0.5650 0.9104 0.6875 0.039 Uiso 1 1 calc R . .
C35 C 0.5450(2) 0.7110(4) 0.72955(18) 0.0269(8) Uani 1 1 d . . .
H35A H 0.5877 0.7257 0.7664 0.032 Uiso 1 1 calc R . .
N1 N 0.60010(18) 0.5893(3) 0.97559(13) 0.0195(6) Uani 1 1 d . . .
N2 N 0.67946(18) 0.5328(3) 1.00643(14) 0.0216(6) Uani 1 1 d . . .
N3 N 0.9489(2) 0.1993(4) 1.03764(16) 0.0332(8) Uani 1 1 d . . .
O1 O 0.45911(14) 0.6390(3) 0.87342(11) 0.0225(5) Uani 1 1 d . . .
O2 O 0.67868(14) 0.4041(3) 0.90822(11) 0.0203(5) 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
Pd1 O1 1.967(2) . ?
Pd1 N1 1.972(3) . ?
Pd1 O2 2.000(2) . ?
Pd1 P1 2.2996(9) . ?
P1 C30 1.814(3) . ?
P1 C18 1.826(3) . ?
P1 C24 1.831(3) . ?
C1 N1 1.294(4) . ?
C1 C2 1.429(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.406(5) . ?
C2 C7 1.464(5) . ?
C3 O1 1.324(4) . ?
C3 C4 1.436(5) . ?
C4 C5 1.351(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.422(5) . ?
C5 H5A 0.9500 . ?
C6 C8 1.412(5) . ?
C6 C7 1.428(5) . ?
C7 C11 1.408(5) . ?
C8 C9 1.366(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.410(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.372(5) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 N2 1.304(4) . ?
C12 O2 1.311(4) . ?
C12 C13 1.485(5) . ?
C13 C14 1.386(5) . ?
C13 C17 1.392(5) . ?
C14 C15 1.374(5) . ?
C14 H14A 0.9500 . ?
C15 N3 1.339(5) . ?
C15 H15A 0.9500 . ?
C16 N3 1.329(5) . ?
C16 C17 1.382(5) . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
C18 C19 1.390(5) . ?
C18 C23 1.395(5) . ?
C19 C20 1.390(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.390(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.389(5) . ?
C21 H21A 0.9500 . ?
C22 C23 1.392(5) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.379(5) . ?
C24 C29 1.404(5) . ?
C25 C26 1.388(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.381(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.377(5) . ?
C27 H27A 0.9500 . ?
C28 C29 1.386(5) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 C31 1.397(5) . ?
C30 C35 1.402(5) . ?
C31 C32 1.380(5) . ?
C31 H31A 0.9500 . ?
C32 C33 1.384(6) . ?
C32 H32A 0.9500 . ?
C33 C34 1.396(6) . ?
C33 H33A 0.9500 . ?
C34 C35 1.368(5) . ?
C34 H34A 0.9500 . ?
C35 H35A 0.9500 . ?
N1 N2 1.397(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 N1 93.27(10) . . ?
O1 Pd1 O2 173.50(9) . . ?
N1 Pd1 O2 80.24(10) . . ?
O1 Pd1 P1 87.19(7) . . ?
N1 Pd1 P1 178.83(8) . . ?
O2 Pd1 P1 99.31(7) . . ?
C30 P1 C18 104.16(16) . . ?
C30 P1 C24 105.59(15) . . ?
C18 P1 C24 103.67(15) . . ?
C30 P1 Pd1 112.44(12) . . ?
C18 P1 Pd1 118.85(11) . . ?
C24 P1 Pd1 110.97(11) . . ?
N1 C1 C2 125.9(3) . . ?
N1 C1 H1A 117.1 . . ?
C2 C1 H1A 117.1 . . ?
C3 C2 C1 123.1(3) . . ?
C3 C2 C7 118.6(3) . . ?
C1 C2 C7 118.3(3) . . ?
O1 C3 C2 127.3(3) . . ?
O1 C3 C4 112.8(3) . . ?
C2 C3 C4 119.9(3) . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5A 119.3 . . ?
C6 C5 H5A 119.3 . . ?
C8 C6 C5 120.9(3) . . ?
C8 C6 C7 120.0(3) . . ?
C5 C6 C7 119.1(3) . . ?
C11 C7 C6 116.7(3) . . ?
C11 C7 C2 123.8(3) . . ?
C6 C7 C2 119.5(3) . . ?
C9 C8 C6 121.9(3) . . ?
C9 C8 H8A 119.1 . . ?
C6 C8 H8A 119.1 . . ?
C8 C9 C10 118.4(3) . . ?
C8 C9 H9A 120.8 . . ?
C10 C9 H9A 120.8 . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C10 C11 C7 122.1(3) . . ?
C10 C11 H11A 118.9 . . ?
C7 C11 H11A 118.9 . . ?
N2 C12 O2 126.0(3) . . ?
N2 C12 C13 118.9(3) . . ?
O2 C12 C13 115.1(3) . . ?
C14 C13 C17 116.1(3) . . ?
C14 C13 C12 122.5(3) . . ?
C17 C13 C12 121.3(3) . . ?
C15 C14 C13 119.5(4) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
N3 C15 C14 124.7(4) . . ?
N3 C15 H15A 117.6 . . ?
C14 C15 H15A 117.6 . . ?
N3 C16 C17 123.5(3) . . ?
N3 C16 H16A 118.2 . . ?
C17 C16 H16A 118.2 . . ?
C16 C17 C13 120.4(3) . . ?
C16 C17 H17A 119.8 . . ?
C13 C17 H17A 119.8 . . ?
C19 C18 C23 120.0(3) . . ?
C19 C18 P1 118.1(3) . . ?
C23 C18 P1 121.7(3) . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19A 119.9 . . ?
C18 C19 H19A 119.9 . . ?
C19 C20 C21 120.1(4) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C23 120.8(3) . . ?
C21 C22 H22A 119.6 . . ?
C23 C22 H22A 119.6 . . ?
C22 C23 C18 119.3(3) . . ?
C22 C23 H23A 120.3 . . ?
C18 C23 H23A 120.3 . . ?
C25 C24 C29 119.2(3) . . ?
C25 C24 P1 122.3(3) . . ?
C29 C24 P1 118.4(3) . . ?
C24 C25 C26 120.9(3) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C27 C26 C25 119.7(4) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27A 120.0 . . ?
C26 C27 H27A 120.0 . . ?
C27 C28 C29 120.7(3) . . ?
C27 C28 H28A 119.7 . . ?
C29 C28 H28A 119.7 . . ?
C28 C29 C24 119.5(3) . . ?
C28 C29 H29A 120.2 . . ?
C24 C29 H29A 120.2 . . ?
C31 C30 C35 118.7(3) . . ?
C31 C30 P1 122.5(3) . . ?
C35 C30 P1 118.6(3) . . ?
C32 C31 C30 120.2(3) . . ?
C32 C31 H31A 119.9 . . ?
C30 C31 H31A 119.9 . . ?
C31 C32 C33 120.4(4) . . ?
C31 C32 H32A 119.8 . . ?
C33 C32 H32A 119.8 . . ?
C32 C33 C34 119.9(4) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C35 C34 C33 119.7(4) . . ?
C35 C34 H34A 120.1 . . ?
C33 C34 H34A 120.1 . . ?
C34 C35 C30 121.0(4) . . ?
C34 C35 H35A 119.5 . . ?
C30 C35 H35A 119.5 . . ?
C1 N1 N2 118.9(3) . . ?
C1 N1 Pd1 126.1(2) . . ?
N2 N1 Pd1 114.9(2) . . ?
C12 N2 N1 109.7(3) . . ?
C16 N3 C15 115.8(3) . . ?
C3 O1 Pd1 124.3(2) . . ?
C12 O2 Pd1 109.1(2) . . ?

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
O1 Pd1 P1 C30 48.40(13) . . . . ?
N1 Pd1 P1 C30 162(4) . . . . ?
O2 Pd1 P1 C30 -131.33(13) . . . . ?
O1 Pd1 P1 C18 170.39(14) . . . . ?
N1 Pd1 P1 C18 -76(4) . . . . ?
O2 Pd1 P1 C18 -9.34(14) . . . . ?
O1 Pd1 P1 C24 -69.60(14) . . . . ?
N1 Pd1 P1 C24 44(4) . . . . ?
O2 Pd1 P1 C24 110.67(13) . . . . ?
N1 C1 C2 C3 -1.2(5) . . . . ?
N1 C1 C2 C7 -178.9(3) . . . . ?
C1 C2 C3 O1 0.0(5) . . . . ?
C7 C2 C3 O1 177.7(3) . . . . ?
C1 C2 C3 C4 179.8(3) . . . . ?
C7 C2 C3 C4 -2.5(5) . . . . ?
O1 C3 C4 C5 -179.2(3) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
C3 C4 C5 C6 0.4(5) . . . . ?
C4 C5 C6 C8 178.6(3) . . . . ?
C4 C5 C6 C7 -0.1(5) . . . . ?
C8 C6 C7 C11 -1.5(5) . . . . ?
C5 C6 C7 C11 177.3(3) . . . . ?
C8 C6 C7 C2 179.8(3) . . . . ?
C5 C6 C7 C2 -1.4(5) . . . . ?
C3 C2 C7 C11 -175.9(3) . . . . ?
C1 C2 C7 C11 1.9(5) . . . . ?
C3 C2 C7 C6 2.7(5) . . . . ?
C1 C2 C7 C6 -179.5(3) . . . . ?
C5 C6 C8 C9 -178.3(3) . . . . ?
C7 C6 C8 C9 0.4(5) . . . . ?
C6 C8 C9 C10 1.1(5) . . . . ?
C8 C9 C10 C11 -1.6(5) . . . . ?
C9 C10 C11 C7 0.5(5) . . . . ?
C6 C7 C11 C10 1.0(5) . . . . ?
C2 C7 C11 C10 179.7(3) . . . . ?
N2 C12 C13 C14 -1.9(5) . . . . ?
O2 C12 C13 C14 178.1(3) . . . . ?
N2 C12 C13 C17 174.4(3) . . . . ?
O2 C12 C13 C17 -5.5(5) . . . . ?
C17 C13 C14 C15 1.9(5) . . . . ?
C12 C13 C14 C15 178.4(4) . . . . ?
C13 C14 C15 N3 -3.0(7) . . . . ?
N3 C16 C17 C13 -1.2(6) . . . . ?
C14 C13 C17 C16 0.1(5) . . . . ?
C12 C13 C17 C16 -176.5(3) . . . . ?
C30 P1 C18 C19 161.1(3) . . . . ?
C24 P1 C18 C19 -88.6(3) . . . . ?
Pd1 P1 C18 C19 35.1(3) . . . . ?
C30 P1 C18 C23 -23.8(3) . . . . ?
C24 P1 C18 C23 86.5(3) . . . . ?
Pd1 P1 C18 C23 -149.8(2) . . . . ?
C23 C18 C19 C20 -1.6(5) . . . . ?
P1 C18 C19 C20 173.6(3) . . . . ?
C18 C19 C20 C21 0.7(6) . . . . ?
C19 C20 C21 C22 0.2(6) . . . . ?
C20 C21 C22 C23 -0.1(6) . . . . ?
C21 C22 C23 C18 -0.8(5) . . . . ?
C19 C18 C23 C22 1.6(5) . . . . ?
P1 C18 C23 C22 -173.4(3) . . . . ?
C30 P1 C24 C25 107.0(3) . . . . ?
C18 P1 C24 C25 -2.3(3) . . . . ?
Pd1 P1 C24 C25 -131.0(3) . . . . ?
C30 P1 C24 C29 -77.9(3) . . . . ?
C18 P1 C24 C29 172.9(3) . . . . ?
Pd1 P1 C24 C29 44.2(3) . . . . ?
C29 C24 C25 C26 1.4(5) . . . . ?
P1 C24 C25 C26 176.5(3) . . . . ?
C24 C25 C26 C27 -0.2(6) . . . . ?
C25 C26 C27 C28 -1.0(6) . . . . ?
C26 C27 C28 C29 1.1(6) . . . . ?
C27 C28 C29 C24 0.1(5) . . . . ?
C25 C24 C29 C28 -1.3(5) . . . . ?
P1 C24 C29 C28 -176.6(3) . . . . ?
C18 P1 C30 C31 82.5(3) . . . . ?
C24 P1 C30 C31 -26.4(3) . . . . ?
Pd1 P1 C30 C31 -147.5(2) . . . . ?
C18 P1 C30 C35 -91.2(3) . . . . ?
C24 P1 C30 C35 159.9(3) . . . . ?
Pd1 P1 C30 C35 38.7(3) . . . . ?
C35 C30 C31 C32 0.6(5) . . . . ?
P1 C30 C31 C32 -173.1(3) . . . . ?
C30 C31 C32 C33 0.3(6) . . . . ?
C31 C32 C33 C34 -0.6(6) . . . . ?
C32 C33 C34 C35 0.1(6) . . . . ?
C33 C34 C35 C30 0.8(5) . . . . ?
C31 C30 C35 C34 -1.1(5) . . . . ?
P1 C30 C35 C34 172.9(3) . . . . ?
C2 C1 N1 N2 179.0(3) . . . . ?
C2 C1 N1 Pd1 1.5(5) . . . . ?
O1 Pd1 N1 C1 -0.7(3) . . . . ?
O2 Pd1 N1 C1 178.9(3) . . . . ?
P1 Pd1 N1 C1 -114(4) . . . . ?
O1 Pd1 N1 N2 -178.3(2) . . . . ?
O2 Pd1 N1 N2 1.3(2) . . . . ?
P1 Pd1 N1 N2 69(4) . . . . ?
O2 C12 N2 N1 2.1(5) . . . . ?
C13 C12 N2 N1 -177.8(3) . . . . ?
C1 N1 N2 C12 -179.9(3) . . . . ?
Pd1 N1 N2 C12 -2.1(3) . . . . ?
C17 C16 N3 C15 0.2(6) . . . . ?
C14 C15 N3 C16 1.9(6) . . . . ?
C2 C3 O1 Pd1 0.7(5) . . . . ?
C4 C3 O1 Pd1 -179.1(2) . . . . ?
N1 Pd1 O1 C3 -0.4(3) . . . . ?
O2 Pd1 O1 C3 -3.8(10) . . . . ?
P1 Pd1 O1 C3 178.5(2) . . . . ?
N2 C12 O2 Pd1 -1.0(4) . . . . ?
C13 C12 O2 Pd1 178.9(2) . . . . ?
O1 Pd1 O2 C12 3.2(9) . . . . ?
N1 Pd1 O2 C12 -0.3(2) . . . . ?
P1 Pd1 O2 C12 -179.17(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        59.99
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.079
