# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_jd11
_database_code_depnum_ccdc_archive 'CCDC 965740'
_audit_update_record             
;
2013-10-10 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H28 N O2 P Pd'
_chemical_formula_weight         643.96

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

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P21/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                   15.6731(6)
_cell_length_b                   11.7347(4)
_cell_length_c                   17.4108(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.042(2)
_cell_angle_gamma                90.00
_cell_volume                     2877.07(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44600
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         27.02
_reflns_number_total             6244
_reflns_number_gt                5258
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0489P)²+0.3213P] 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         6244
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
Pd1 Pd 0.260374(11) 0.274261(14) 0.399606(10) 0.03198(7) Uani 1 1 d . . .
P1 P 0.16802(4) 0.36571(5) 0.45045(4) 0.03316(13) Uani 1 1 d . . .
O2 O 0.41347(17) -0.29382(16) 0.49139(15) 0.0676(6) Uani 1 1 d . . .
O1 O 0.24528(12) 0.12636(14) 0.45528(11) 0.0442(4) Uani 1 1 d . . .
N1 N 0.34200(13) 0.19173(16) 0.35237(12) 0.0343(4) Uani 1 1 d . . .
C131 C 0.07531(16) 0.45323(19) 0.37198(14) 0.0380(5) Uani 1 1 d . . .
C136 C 0.05119(19) 0.5603(2) 0.38986(17) 0.0492(6) Uani 1 1 d . . .
H136 H 0.0844 0.5919 0.4439 0.059 Uiso 1 1 calc R . .
C135 C -0.0226(2) 0.6199(3) 0.3268(2) 0.0658(8) Uani 1 1 d . . .
H135 H -0.0383 0.6921 0.3387 0.079 Uiso 1 1 calc R . .
C134 C -0.0725(2) 0.5743(3) 0.2477(2) 0.0739(10) Uani 1 1 d . . .
H134 H -0.1219 0.6153 0.2060 0.089 Uiso 1 1 calc R . .
C133 C -0.0501(2) 0.4684(3) 0.22917(19) 0.0694(9) Uani 1 1 d . . .
H133 H -0.0851 0.4368 0.1754 0.083 Uiso 1 1 calc R . .
C132 C 0.02442(19) 0.4086(3) 0.29058(16) 0.0552(7) Uani 1 1 d . . .
H132 H 0.0407 0.3376 0.2773 0.066 Uiso 1 1 calc R . .
C111 C 0.23190(16) 0.45662(19) 0.54300(14) 0.0362(5) Uani 1 1 d . . .
C112 C 0.32155(16) 0.4965(2) 0.55988(14) 0.0407(5) Uani 1 1 d . . .
H112 H 0.3487 0.4771 0.5237 0.049 Uiso 1 1 calc R . .
C113 C 0.37102(19) 0.5649(2) 0.63021(16) 0.0494(6) Uani 1 1 d . . .
H113 H 0.4313 0.5911 0.6412 0.059 Uiso 1 1 calc R . .
C114 C 0.3314(2) 0.5942(2) 0.68380(16) 0.0532(7) Uani 1 1 d . . .
H114 H 0.3647 0.6405 0.7310 0.064 Uiso 1 1 calc R . .
C115 C 0.2423(2) 0.5553(2) 0.66774(17) 0.0576(7) Uani 1 1 d . . .
H115 H 0.2155 0.5753 0.7041 0.069 Uiso 1 1 calc R . .
C116 C 0.19287(19) 0.4869(2) 0.59831(16) 0.0505(6) Uani 1 1 d . . .
H116 H 0.1328 0.4606 0.5880 0.061 Uiso 1 1 calc R . .
C121 C 0.10226(17) 0.26983(19) 0.48763(16) 0.0366(5) Uani 1 1 d . . .
C122 C 0.00454(19) 0.2582(2) 0.44553(19) 0.0511(6) Uani 1 1 d . . .
H122 H -0.0300 0.3012 0.3968 0.061 Uiso 1 1 calc R . .
C123 C -0.0422(2) 0.1834(3) 0.4752(2) 0.0661(8) Uani 1 1 d . . .
H123 H -0.1078 0.1760 0.4462 0.079 Uiso 1 1 calc R . .
C124 C 0.0077(2) 0.1199(3) 0.5473(2) 0.0616(8) Uani 1 1 d . . .
H124 H -0.0239 0.0696 0.5672 0.074 Uiso 1 1 calc R . .
C125 C 0.1048(2) 0.1311(2) 0.58995(18) 0.0529(6) Uani 1 1 d . . .
H125 H 0.1388 0.0884 0.6390 0.063 Uiso 1 1 calc R . .
C126 C 0.15207(19) 0.2049(2) 0.56077(17) 0.0453(6) Uani 1 1 d . . .
H126 H 0.2178 0.2115 0.5900 0.054 Uiso 1 1 calc R . .
C9 C 0.36439(17) 0.2601(2) 0.29638(15) 0.0371(5) Uani 1 1 d . . .
C17 C 0.33346(16) 0.3742(2) 0.29133(14) 0.0367(5) Uani 1 1 d . . .
C16 C 0.28127(16) 0.40792(19) 0.33799(14) 0.0372(5) Uani 1 1 d . . .
C15 C 0.25376(18) 0.5202(2) 0.33098(16) 0.0443(6) Uani 1 1 d . . .
H15 H 0.2211 0.5454 0.3613 0.053 Uiso 1 1 calc R . .
C14 C 0.2734(2) 0.5982(2) 0.27929(18) 0.0532(6) Uani 1 1 d . . .
H14 H 0.2536 0.6734 0.2764 0.064 Uiso 1 1 calc R . .
C13 C 0.32061(19) 0.5658(2) 0.23373(17) 0.0512(6) Uani 1 1 d . . .
H13 H 0.3323 0.6185 0.1995 0.061 Uiso 1 1 calc R . .
C18 C 0.35214(17) 0.4520(2) 0.23813(15) 0.0418(5) Uani 1 1 d . . .
C12 C 0.39926(18) 0.4112(2) 0.19012(16) 0.0494(6) Uani 1 1 d . . .
H12 H 0.4125 0.4611 0.1553 0.059 Uiso 1 1 calc R . .
C11 C 0.4251(2) 0.3006(2) 0.19441(18) 0.0515(7) Uani 1 1 d . . .
H11 H 0.4541 0.2753 0.1611 0.062 Uiso 1 1 calc R . .
C10 C 0.4088(2) 0.2228(2) 0.24841(18) 0.0472(6) Uani 1 1 d . . .
H10 H 0.4280 0.1473 0.2514 0.057 Uiso 1 1 calc R . .
C7 C 0.37391(16) 0.0889(2) 0.37259(15) 0.0382(5) Uani 1 1 d . . .
H7 H 0.4164 0.0645 0.3519 0.046 Uiso 1 1 calc R . .
C6 C 0.35196(16) 0.00875(19) 0.42258(14) 0.0372(5) Uani 1 1 d . . .
C5 C 0.39568(17) -0.1009(2) 0.43384(15) 0.0429(6) Uani 1 1 d . . .
H5 H 0.4393 -0.1143 0.4120 0.052 Uiso 1 1 calc R . .
C4 C 0.37478(19) -0.1859(2) 0.47590(17) 0.0466(6) Uani 1 1 d . . .
C8 C 0.4795(2) -0.3214(2) 0.4601(2) 0.0588(7) Uani 1 1 d . . .
H8A H 0.4492 -0.3182 0.3988 0.088 Uiso 1 1 calc R . .
H8B H 0.5034 -0.3969 0.4783 0.088 Uiso 1 1 calc R . .
H8C H 0.5311 -0.2680 0.4819 0.088 Uiso 1 1 calc R . .
C3 C 0.3072(2) -0.1670(2) 0.50690(18) 0.0526(6) Uani 1 1 d . . .
H3 H 0.2908 -0.2260 0.5336 0.063 Uiso 1 1 calc R . .
C2 C 0.26520(18) -0.0627(2) 0.49820(17) 0.0473(6) Uani 1 1 d . . .
H2 H 0.2209 -0.0521 0.5196 0.057 Uiso 1 1 calc R . .
C1 C 0.28696(16) 0.02961(19) 0.45767(14) 0.0363(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 C16 2.007(2) . ?
Pd1 N1 2.0433(17) . ?
Pd1 O1 2.0516(16) . ?
Pd1 P1 2.2705(6) . ?
P1 C131 1.814(2) . ?
P1 C111 1.822(2) . ?
P1 C121 1.826(2) . ?
O2 C4 1.379(3) . ?
O2 C8 1.402(3) . ?
O1 C1 1.301(3) . ?
N1 C7 1.294(3) . ?
N1 C9 1.421(3) . ?
C131 C136 1.386(3) . ?
C131 C132 1.388(3) . ?
C136 C135 1.385(4) . ?
C136 H136 0.9300 . ?
C135 C134 1.360(4) . ?
C135 H135 0.9300 . ?
C134 C133 1.368(5) . ?
C134 H134 0.9300 . ?
C133 C132 1.380(4) . ?
C133 H133 0.9300 . ?
C132 H132 0.9300 . ?
C111 C112 1.384(3) . ?
C111 C116 1.395(3) . ?
C112 C113 1.382(3) . ?
C112 H112 0.9300 . ?
C113 C114 1.373(4) . ?
C113 H113 0.9300 . ?
C114 C115 1.376(4) . ?
C114 H114 0.9300 . ?
C115 C116 1.372(4) . ?
C115 H115 0.9300 . ?
C116 H116 0.9300 . ?
C121 C122 1.384(4) . ?
C121 C126 1.393(4) . ?
C122 C123 1.381(4) . ?
C122 H122 0.9300 . ?
C123 C124 1.371(4) . ?
C123 H123 0.9300 . ?
C124 C125 1.376(4) . ?
C124 H124 0.9300 . ?
C125 C126 1.373(4) . ?
C125 H125 0.9300 . ?
C126 H126 0.9300 . ?
C9 C10 1.373(3) . ?
C9 C17 1.413(3) . ?
C17 C18 1.420(3) . ?
C17 C16 1.438(3) . ?
C16 C15 1.375(3) . ?
C15 C14 1.410(3) . ?
C15 H15 0.9300 . ?
C14 C13 1.354(4) . ?
C14 H14 0.9300 . ?
C13 C18 1.415(4) . ?
C13 H13 0.9300 . ?
C18 C12 1.420(3) . ?
C12 C11 1.351(4) . ?
C12 H12 0.9300 . ?
C11 C10 1.412(4) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?
C7 C6 1.423(3) . ?
C7 H7 0.9300 . ?
C6 C1 1.420(3) . ?
C6 C5 1.430(3) . ?
C5 C4 1.360(3) . ?
C5 H5 0.9300 . ?
C4 C3 1.402(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C3 C2 1.366(3) . ?
C3 H3 0.9300 . ?
C2 C1 1.414(3) . ?
C2 H2 0.9300 . ?

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
C16 Pd1 N1 82.95(8) . . ?
C16 Pd1 O1 173.49(8) . . ?
N1 Pd1 O1 90.67(7) . . ?
C16 Pd1 P1 96.93(7) . . ?
N1 Pd1 P1 179.26(5) . . ?
O1 Pd1 P1 89.43(4) . . ?
C131 P1 C111 106.38(10) . . ?
C131 P1 C121 103.04(11) . . ?
C111 P1 C121 102.93(11) . . ?
C131 P1 Pd1 114.27(7) . . ?
C111 P1 Pd1 115.13(7) . . ?
C121 P1 Pd1 113.75(7) . . ?
C4 O2 C8 118.2(2) . . ?
C1 O1 Pd1 126.35(14) . . ?
C7 N1 C9 122.08(19) . . ?
C7 N1 Pd1 124.59(15) . . ?
C9 N1 Pd1 113.29(15) . . ?
C136 C131 C132 118.7(2) . . ?
C136 C131 P1 123.46(19) . . ?
C132 C131 P1 117.83(18) . . ?
C135 C136 C131 119.7(3) . . ?
C135 C136 H136 120.2 . . ?
C131 C136 H136 120.2 . . ?
C134 C135 C136 120.8(3) . . ?
C134 C135 H135 119.6 . . ?
C136 C135 H135 119.6 . . ?
C135 C134 C133 120.2(3) . . ?
C135 C134 H134 119.9 . . ?
C133 C134 H134 119.9 . . ?
C134 C133 C132 119.8(3) . . ?
C134 C133 H133 120.1 . . ?
C132 C133 H133 120.1 . . ?
C133 C132 C131 120.7(3) . . ?
C133 C132 H132 119.6 . . ?
C131 C132 H132 119.6 . . ?
C112 C111 C116 118.6(2) . . ?
C112 C111 P1 119.86(17) . . ?
C116 C111 P1 121.52(18) . . ?
C113 C112 C111 120.4(2) . . ?
C113 C112 H112 119.8 . . ?
C111 C112 H112 119.8 . . ?
C114 C113 C112 120.2(2) . . ?
C114 C113 H113 119.9 . . ?
C112 C113 H113 119.9 . . ?
C113 C114 C115 120.0(2) . . ?
C113 C114 H114 120.0 . . ?
C115 C114 H114 120.0 . . ?
C116 C115 C114 120.2(3) . . ?
C116 C115 H115 119.9 . . ?
C114 C115 H115 119.9 . . ?
C115 C116 C111 120.5(2) . . ?
C115 C116 H116 119.7 . . ?
C111 C116 H116 119.7 . . ?
C122 C121 C126 118.4(2) . . ?
C122 C121 P1 122.6(2) . . ?
C126 C121 P1 118.97(19) . . ?
C123 C122 C121 120.6(3) . . ?
C123 C122 H122 119.7 . . ?
C121 C122 H122 119.7 . . ?
C124 C123 C122 120.4(3) . . ?
C124 C123 H123 119.8 . . ?
C122 C123 H123 119.8 . . ?
C123 C124 C125 119.5(3) . . ?
C123 C124 H124 120.2 . . ?
C125 C124 H124 120.2 . . ?
C126 C125 C124 120.6(3) . . ?
C126 C125 H125 119.7 . . ?
C124 C125 H125 119.7 . . ?
C125 C126 C121 120.4(3) . . ?
C125 C126 H126 119.8 . . ?
C121 C126 H126 119.8 . . ?
C10 C9 C17 121.1(2) . . ?
C10 C9 N1 125.5(2) . . ?
C17 C9 N1 113.4(2) . . ?
C9 C17 C18 119.1(2) . . ?
C9 C17 C16 119.4(2) . . ?
C18 C17 C16 121.5(2) . . ?
C15 C16 C17 116.6(2) . . ?
C15 C16 Pd1 132.69(18) . . ?
C17 C16 Pd1 110.70(16) . . ?
C16 C15 C14 122.1(2) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C13 C14 C15 121.4(2) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C14 C13 C18 120.0(2) . . ?
C14 C13 H13 120.0 . . ?
C18 C13 H13 120.0 . . ?
C13 C18 C17 118.4(2) . . ?
C13 C18 C12 123.1(2) . . ?
C17 C18 C12 118.5(2) . . ?
C11 C12 C18 120.8(2) . . ?
C11 C12 H12 119.6 . . ?
C18 C12 H12 119.6 . . ?
C12 C11 C10 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C9 C10 C11 119.1(2) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
N1 C7 C6 127.9(2) . . ?
N1 C7 H7 116.0 . . ?
C6 C7 H7 116.0 . . ?
C1 C6 C7 124.1(2) . . ?
C1 C6 C5 119.1(2) . . ?
C7 C6 C5 116.7(2) . . ?
C4 C5 C6 121.3(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C4 O2 126.1(2) . . ?
C5 C4 C3 119.5(2) . . ?
O2 C4 C3 114.3(2) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C3 C4 120.5(2) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C2 C1 122.1(2) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
O1 C1 C2 117.18(19) . . ?
O1 C1 C6 125.5(2) . . ?
C2 C1 C6 117.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_jd2
_database_code_depnum_ccdc_archive 'CCDC 965741'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-18 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 H25 N O P Pd'
_chemical_formula_weight         612.93

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'
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   P21/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                   14.3819(11)
_cell_length_b                   11.8875(9)
_cell_length_c                   17.6698(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.090(4)
_cell_angle_gamma                90.00
_cell_volume                     2799.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42175
_diffrn_reflns_av_R_equivalents  0.1401
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         28.16
_reflns_number_total             6506
_reflns_number_gt                3740
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0720P)²+5.1412P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6506
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0630
_refine_ls_wR_factor_ref         0.1772
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004

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 0.72586(3) 0.22767(4) 0.11688(3) 0.04176(17) Uani 1 1 d . . .
P1 P 0.81892(11) 0.12649(13) 0.06228(9) 0.0421(4) Uani 1 1 d . . .
C3 C 0.7174(6) 0.6627(7) 0.0203(5) 0.073(2) Uani 1 1 d . . .
H3 H 0.7342 0.7155 -0.0113 0.088 Uiso 1 1 calc R . .
C124 C 0.6400(6) -0.1102(6) -0.1461(5) 0.075(2) Uani 1 1 d . . .
H124 H 0.6033 -0.1590 -0.1878 0.089 Uiso 1 1 calc R . .
C12 C 0.6538(5) -0.0435(6) 0.2912(5) 0.0624(19) Uani 1 1 d . . .
H12 H 0.6403 -0.0925 0.3269 0.075 Uiso 1 1 calc R . .
C134 C 1.0689(6) -0.0773(7) 0.2530(5) 0.082(2) Uani 1 1 d . . .
H134 H 1.1212 -0.1164 0.2917 0.099 Uiso 1 1 calc R . .
N1 N 0.6547(3) 0.3218(4) 0.1748(3) 0.0436(11) Uani 1 1 d . . .
O1 O 0.7411(3) 0.3654(4) 0.0534(3) 0.0532(11) Uani 1 1 d . . .
C6 C 0.6682(5) 0.5027(5) 0.1132(5) 0.0563(17) Uani 1 1 d . . .
C2 C 0.7395(5) 0.5520(6) 0.0159(4) 0.0567(17) Uani 1 1 d . . .
H2 H 0.7714 0.5315 -0.0191 0.068 Uiso 1 1 calc R . .
C121 C 0.7485(4) 0.0335(5) -0.0220(4) 0.0468(14) Uani 1 1 d . . .
C131 C 0.9141(4) 0.0398(5) 0.1365(4) 0.0485(15) Uani 1 1 d . . .
C122 C 0.6523(5) 0.0032(6) -0.0325(4) 0.0592(18) Uani 1 1 d . . .
H122 H 0.6233 0.0324 0.0022 0.071 Uiso 1 1 calc R . .
C14 C 0.7194(5) -0.0094(6) 0.1867(4) 0.0567(17) Uani 1 1 d . . .
H14 H 0.7489 -0.0396 0.1526 0.068 Uiso 1 1 calc R . .
C9 C 0.5846(4) 0.3037(6) 0.2842(4) 0.0534(16) Uani 1 1 d . . .
H9 H 0.5681 0.3796 0.2818 0.064 Uiso 1 1 calc R . .
C111 C 0.8915(4) 0.2176(5) 0.0211(4) 0.0455(14) Uani 1 1 d . . .
C126 C 0.7890(5) -0.0066(6) -0.0765(4) 0.0582(17) Uani 1 1 d . . .
H126 H 0.8528 0.0160 -0.0717 0.070 Uiso 1 1 calc R . .
C13 C 0.6958(6) -0.0819(6) 0.2400(5) 0.069(2) Uani 1 1 d . . .
H13 H 0.7096 -0.1583 0.2397 0.083 Uiso 1 1 calc R . .
C136 C 0.9443(5) -0.0630(6) 0.1175(4) 0.0624(19) Uani 1 1 d . . .
H136 H 0.9140 -0.0927 0.0652 0.075 Uiso 1 1 calc R . .
C16 C 0.6533(4) 0.1435(5) 0.2357(4) 0.0453(14) Uani 1 1 d . . .
C113 C 1.0428(5) 0.3122(8) 0.0337(5) 0.081(2) Uani 1 1 d . . .
H113 H 1.1108 0.3249 0.0628 0.097 Uiso 1 1 calc R . .
C11 C 0.5852(5) 0.1211(6) 0.3426(4) 0.0581(17) Uani 1 1 d . . .
H11 H 0.5695 0.0754 0.3789 0.070 Uiso 1 1 calc R . .
C125 C 0.7350(6) -0.0802(6) -0.1381(4) 0.076(2) Uani 1 1 d . . .
H125 H 0.7630 -0.1089 -0.1737 0.091 Uiso 1 1 calc R . .
C17 C 0.6302(5) 0.0734(6) 0.2903(4) 0.0538(16) Uani 1 1 d . . .
C115 C 0.8942(6) 0.3514(6) -0.0797(5) 0.0652(19) Uani 1 1 d . . .
H115 H 0.8602 0.3914 -0.1273 0.078 Uiso 1 1 calc R . .
C112 C 0.9923(5) 0.2372(6) 0.0627(5) 0.0638(19) Uani 1 1 d . . .
H112 H 1.0264 0.1989 0.1111 0.077 Uiso 1 1 calc R . .
C114 C 0.9946(6) 0.3688(7) -0.0377(5) 0.070(2) Uani 1 1 d . . .
H114 H 1.0297 0.4187 -0.0575 0.084 Uiso 1 1 calc R . .
C1 C 0.7168(4) 0.4680(5) 0.0612(4) 0.0471(15) Uani 1 1 d . . .
C4 C 0.6699(7) 0.6969(6) 0.0717(6) 0.087(3) Uani 1 1 d . . .
H4 H 0.6536 0.7722 0.0743 0.104 Uiso 1 1 calc R . .
C15 C 0.7008(4) 0.1025(5) 0.1834(4) 0.0500(15) Uani 1 1 d . . .
C7 C 0.6401(4) 0.4296(5) 0.1663(4) 0.0523(16) Uani 1 1 d . . .
H7 H 0.6084 0.4632 0.1977 0.063 Uiso 1 1 calc R . .
C132 C 0.9630(5) 0.0833(6) 0.2125(4) 0.067(2) Uani 1 1 d . . .
H132 H 0.9445 0.1536 0.2252 0.080 Uiso 1 1 calc R . .
C5 C 0.6477(6) 0.6191(6) 0.1178(6) 0.081(2) Uani 1 1 d . . .
H5 H 0.6181 0.6423 0.1537 0.097 Uiso 1 1 calc R . .
C133 C 1.0397(6) 0.0250(8) 0.2712(5) 0.081(2) Uani 1 1 d . . .
H133 H 1.0713 0.0555 0.3231 0.097 Uiso 1 1 calc R . .
C8 C 0.6280(4) 0.2601(5) 0.2332(4) 0.0463(15) Uani 1 1 d . . .
C116 C 0.8433(5) 0.2739(6) -0.0510(4) 0.0549(16) Uani 1 1 d . . .
H116 H 0.7758 0.2598 -0.0809 0.066 Uiso 1 1 calc R . .
C10 C 0.5656(5) 0.2327(6) 0.3394(4) 0.0562(17) Uani 1 1 d . . .
H10 H 0.5385 0.2630 0.3751 0.067 Uiso 1 1 calc R . .
C123 C 0.5981(6) -0.0698(7) -0.0938(5) 0.074(2) Uani 1 1 d . . .
H123 H 0.5336 -0.0913 -0.0995 0.089 Uiso 1 1 calc R . .
C135 C 1.0197(6) -0.1214(7) 0.1765(5) 0.086(3) Uani 1 1 d . . .
H135 H 1.0378 -0.1922 0.1643 0.104 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 C15 2.011(6) . ?
Pd1 N1 2.034(5) . ?
Pd1 O1 2.043(4) . ?
Pd1 P1 2.2672(16) . ?
P1 C131 1.818(6) . ?
P1 C121 1.825(6) . ?
P1 C111 1.835(6) . ?
C3 C2 1.363(10) . ?
C3 C4 1.386(10) . ?
C124 C123 1.368(11) . ?
C124 C125 1.367(11) . ?
C12 C13 1.342(10) . ?
C12 C17 1.430(10) . ?
C134 C135 1.372(11) . ?
C134 C133 1.364(11) . ?
N1 C7 1.298(8) . ?
N1 C8 1.430(8) . ?
O1 C1 1.290(7) . ?
C6 C1 1.408(9) . ?
C6 C7 1.444(9) . ?
C6 C5 1.424(9) . ?
C2 C1 1.394(9) . ?
C121 C122 1.373(8) . ?
C121 C126 1.384(9) . ?
C131 C132 1.363(9) . ?
C131 C136 1.381(8) . ?
C122 C123 1.377(9) . ?
C14 C15 1.354(9) . ?
C14 C13 1.409(9) . ?
C9 C8 1.377(9) . ?
C9 C10 1.392(9) . ?
C111 C116 1.373(9) . ?
C111 C112 1.376(9) . ?
C126 C125 1.385(9) . ?
C136 C135 1.376(9) . ?
C16 C17 1.407(9) . ?
C16 C8 1.429(8) . ?
C16 C15 1.426(9) . ?
C113 C114 1.365(11) . ?
C113 C112 1.366(10) . ?
C11 C10 1.354(9) . ?
C11 C17 1.429(9) . ?
C115 C114 1.368(10) . ?
C115 C116 1.386(9) . ?
C4 C5 1.348(10) . ?
C132 C133 1.383(9) . ?

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
C15 Pd1 N1 83.0(2) . . ?
C15 Pd1 O1 173.7(2) . . ?
N1 Pd1 O1 90.78(18) . . ?
C15 Pd1 P1 96.91(19) . . ?
N1 Pd1 P1 174.60(13) . . ?
O1 Pd1 P1 89.38(12) . . ?
C131 P1 C121 106.4(3) . . ?
C131 P1 C111 103.6(3) . . ?
C121 P1 C111 104.9(3) . . ?
C131 P1 Pd1 113.5(2) . . ?
C121 P1 Pd1 115.7(2) . . ?
C111 P1 Pd1 111.76(18) . . ?
C2 C3 C4 120.3(7) . . ?
C123 C124 C125 121.1(7) . . ?
C13 C12 C17 119.2(7) . . ?
C135 C134 C133 118.9(7) . . ?
C7 N1 C8 121.0(5) . . ?
C7 N1 Pd1 125.1(4) . . ?
C8 N1 Pd1 113.7(4) . . ?
C1 O1 Pd1 127.5(4) . . ?
C1 C6 C7 125.2(6) . . ?
C1 C6 C5 119.0(6) . . ?
C7 C6 C5 115.7(6) . . ?
C3 C2 C1 123.3(6) . . ?
C122 C121 C126 118.7(6) . . ?
C122 C121 P1 119.4(5) . . ?
C126 C121 P1 121.8(5) . . ?
C132 C131 C136 118.8(6) . . ?
C132 C131 P1 117.8(5) . . ?
C136 C131 P1 123.2(5) . . ?
C121 C122 C123 121.1(7) . . ?
C15 C14 C13 122.4(7) . . ?
C8 C9 C10 119.2(6) . . ?
C116 C111 C112 118.5(6) . . ?
C116 C111 P1 119.4(5) . . ?
C112 C111 P1 122.0(5) . . ?
C121 C126 C125 120.5(7) . . ?
C12 C13 C14 121.7(7) . . ?
C135 C136 C131 119.5(7) . . ?
C17 C16 C8 118.2(6) . . ?
C17 C16 C15 122.5(6) . . ?
C8 C16 C15 119.3(6) . . ?
C114 C113 C112 120.7(7) . . ?
C10 C11 C17 120.0(6) . . ?
C124 C125 C126 119.3(7) . . ?
C16 C17 C11 119.3(6) . . ?
C16 C17 C12 117.8(6) . . ?
C11 C17 C12 122.8(6) . . ?
C114 C115 C116 119.8(7) . . ?
C111 C112 C113 120.7(7) . . ?
C113 C114 C115 119.5(7) . . ?
O1 C1 C2 118.9(6) . . ?
O1 C1 C6 124.6(6) . . ?
C2 C1 C6 116.5(6) . . ?
C5 C4 C3 118.8(7) . . ?
C14 C15 C16 116.3(6) . . ?
C14 C15 Pd1 132.6(5) . . ?
C16 C15 Pd1 111.1(4) . . ?
N1 C7 C6 126.6(6) . . ?
C131 C132 C133 121.3(7) . . ?
C4 C5 C6 122.1(7) . . ?
C134 C133 C132 119.9(7) . . ?
C9 C8 C16 121.1(6) . . ?
C9 C8 N1 126.1(6) . . ?
C16 C8 N1 112.7(5) . . ?
C111 C116 C115 120.7(6) . . ?
C11 C10 C9 122.1(7) . . ?
C124 C123 C122 119.3(7) . . ?
C134 C135 C136 121.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        28.16
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         1.276
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_jd22
_database_code_depnum_ccdc_archive 'CCDC 965742'
_audit_update_record             
;
2013-10-10 deposited with the CCDC.
2015-06-18 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 H27 Cl N O P Pd'
_chemical_formula_weight         650.40

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           ?
_symmetry_space_group_name_H-M   P21/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                   15.1395(5)
_cell_length_b                   11.7820(4)
_cell_length_c                   17.5381(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.068(2)
_cell_angle_gamma                90.00
_cell_volume                     2833.66(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.818
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42565
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.49
_reflns_number_total             5796
_reflns_number_gt                4580
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0425P)²+0.3432P] 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         5796
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
Pd1 Pd 0.265001(15) 0.269542(18) 0.395917(13) 0.03274(8) Uani 1 1 d . . .
Cl1 Cl 0.45959(6) -0.31059(7) 0.48321(6) 0.0576(2) Uani 1 1 d . . .
P1 P 0.17045(5) 0.36058(6) 0.44797(4) 0.03395(17) Uani 1 1 d . . .
O1 O 0.25111(14) 0.11896(15) 0.45096(12) 0.0431(5) Uani 1 1 d . . .
N1 N 0.34570(16) 0.18911(19) 0.34381(14) 0.0344(5) Uani 1 1 d . . .
C121 C 0.0758(2) 0.4489(2) 0.37107(17) 0.0375(6) Uani 1 1 d . . .
C122 C 0.0243(2) 0.4035(3) 0.29105(19) 0.0556(9) Uani 1 1 d . . .
H122 H 0.0403 0.3321 0.2782 0.067 Uiso 1 1 calc R . .
C123 C -0.0506(3) 0.4646(4) 0.2308(2) 0.0699(11) Uani 1 1 d . . .
H123 H -0.0863 0.4332 0.1779 0.084 Uiso 1 1 calc R . .
C124 C -0.0726(3) 0.5710(4) 0.2487(2) 0.0743(12) Uani 1 1 d . . .
H124 H -0.1225 0.6123 0.2076 0.089 Uiso 1 1 calc R . .
C125 C -0.0219(3) 0.6166(3) 0.3262(3) 0.0687(11) Uani 1 1 d . . .
H125 H -0.0372 0.6891 0.3377 0.082 Uiso 1 1 calc R . .
C126 C 0.0525(2) 0.5564(3) 0.3885(2) 0.0501(8) Uani 1 1 d . . .
H126 H 0.0865 0.5880 0.4416 0.060 Uiso 1 1 calc R . .
C111 C 0.2352(2) 0.4512(2) 0.53907(17) 0.0364(6) Uani 1 1 d . . .
C112 C 0.3292(2) 0.4868(2) 0.55748(17) 0.0417(7) Uani 1 1 d . . .
H112 H 0.3597 0.4639 0.5239 0.050 Uiso 1 1 calc R . .
C113 C 0.3777(2) 0.5568(3) 0.62639(19) 0.0514(8) Uani 1 1 d . . .
H113 H 0.4410 0.5805 0.6389 0.062 Uiso 1 1 calc R . .
C114 C 0.3333(3) 0.5913(3) 0.6760(2) 0.0557(9) Uani 1 1 d . . .
H114 H 0.3660 0.6394 0.7214 0.067 Uiso 1 1 calc R . .
C115 C 0.2406(3) 0.5551(3) 0.6590(2) 0.0578(9) Uani 1 1 d . . .
H115 H 0.2110 0.5775 0.6935 0.069 Uiso 1 1 calc R . .
C116 C 0.1915(2) 0.4856(3) 0.59074(19) 0.0506(8) Uani 1 1 d . . .
H116 H 0.1286 0.4615 0.5792 0.061 Uiso 1 1 calc R . .
C131 C 0.1014(2) 0.2663(2) 0.48535(19) 0.0362(7) Uani 1 1 d . . .
C136 C 0.0013(2) 0.2553(3) 0.4447(2) 0.0548(9) Uani 1 1 d . . .
H136 H -0.0333 0.2972 0.3962 0.066 Uiso 1 1 calc R . .
C135 C -0.0479(3) 0.1833(3) 0.4748(3) 0.0682(10) Uani 1 1 d . . .
H135 H -0.1154 0.1780 0.4470 0.082 Uiso 1 1 calc R . .
C134 C 0.0017(3) 0.1190(3) 0.5456(2) 0.0602(9) Uani 1 1 d . . .
H134 H -0.0317 0.0694 0.5654 0.072 Uiso 1 1 calc R . .
C133 C 0.1015(3) 0.1292(3) 0.5869(2) 0.0534(8) Uani 1 1 d . . .
H133 H 0.1358 0.0872 0.6355 0.064 Uiso 1 1 calc R . .
C132 C 0.1509(2) 0.2009(3) 0.55677(19) 0.0448(7) Uani 1 1 d . . .
H132 H 0.2184 0.2058 0.5846 0.054 Uiso 1 1 calc R . .
C1 C 0.2964(2) 0.0247(2) 0.45237(17) 0.0362(6) Uani 1 1 d . . .
C6 C 0.3614(2) 0.0072(2) 0.41455(17) 0.0365(6) Uani 1 1 d . . .
C5 C 0.4102(2) -0.0980(2) 0.42548(19) 0.0435(7) Uani 1 1 d . . .
H5 H 0.4543 -0.1084 0.4019 0.052 Uiso 1 1 calc R . .
C4 C 0.3945(2) -0.1838(2) 0.46933(18) 0.0421(7) Uani 1 1 d . . .
C3 C 0.3275(2) -0.1714(3) 0.5036(2) 0.0500(8) Uani 1 1 d . . .
H3 H 0.3151 -0.2313 0.5322 0.060 Uiso 1 1 calc R . .
C2 C 0.2798(2) -0.0698(2) 0.4949(2) 0.0473(8) Uani 1 1 d . . .
H2 H 0.2347 -0.0625 0.5177 0.057 Uiso 1 1 calc R . .
C7 C 0.3811(2) 0.0887(2) 0.36341(18) 0.0406(7) Uani 1 1 d . . .
H7 H 0.4249 0.0663 0.3418 0.049 Uiso 1 1 calc R . .
C8 C 0.3666(2) 0.2583(2) 0.28744(18) 0.0363(7) Uani 1 1 d . . .
C9 C 0.4099(2) 0.2219(3) 0.2365(2) 0.0445(7) Uani 1 1 d . . .
H9 H 0.4284 0.1465 0.2378 0.053 Uiso 1 1 calc R . .
C10 C 0.4256(2) 0.2994(3) 0.1829(2) 0.0498(8) Uani 1 1 d . . .
H10 H 0.4535 0.2747 0.1477 0.060 Uiso 1 1 calc R . .
C11 C 0.4004(2) 0.4101(3) 0.18167(19) 0.0483(8) Uani 1 1 d . . .
H11 H 0.4130 0.4604 0.1467 0.058 Uiso 1 1 calc R . .
C17 C 0.3554(2) 0.4506(2) 0.23240(18) 0.0423(7) Uani 1 1 d . . .
C12 C 0.3268(2) 0.5650(3) 0.2328(2) 0.0521(8) Uani 1 1 d . . .
H12 H 0.3386 0.6186 0.1993 0.062 Uiso 1 1 calc R . .
C13 C 0.2822(2) 0.5959(3) 0.2821(2) 0.0551(9) Uani 1 1 d . . .
H13 H 0.2645 0.6714 0.2825 0.066 Uiso 1 1 calc R . .
C14 C 0.2619(2) 0.5169(2) 0.33284(19) 0.0470(8) Uani 1 1 d . . .
H14 H 0.2310 0.5417 0.3657 0.056 Uiso 1 1 calc R . .
C15 C 0.2864(2) 0.4045(2) 0.33532(17) 0.0369(6) Uani 1 1 d . . .
C16 C 0.3362(2) 0.3717(2) 0.28501(17) 0.0355(6) 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 C15 2.013(3) . ?
Pd1 N1 2.042(2) . ?
Pd1 O1 2.0726(18) . ?
Pd1 P1 2.2672(7) . ?
Cl1 C4 1.749(3) . ?
P1 C121 1.821(3) . ?
P1 C111 1.824(3) . ?
P1 C131 1.826(3) . ?
O1 C1 1.300(3) . ?
N1 C7 1.285(3) . ?
N1 C8 1.417(3) . ?
C121 C126 1.383(4) . ?
C121 C122 1.391(4) . ?
C122 C123 1.380(4) . ?
C122 H122 0.9300 . ?
C123 C124 1.367(5) . ?
C123 H123 0.9300 . ?
C124 C125 1.357(5) . ?
C124 H124 0.9300 . ?
C125 C126 1.386(4) . ?
C125 H125 0.9300 . ?
C126 H126 0.9300 . ?
C111 C112 1.384(4) . ?
C111 C116 1.389(4) . ?
C112 C113 1.389(4) . ?
C112 H112 0.9300 . ?
C113 C114 1.368(5) . ?
C113 H113 0.9300 . ?
C114 C115 1.373(5) . ?
C114 H114 0.9300 . ?
C115 C116 1.380(4) . ?
C115 H115 0.9300 . ?
C116 H116 0.9300 . ?
C131 C136 1.381(4) . ?
C131 C132 1.389(4) . ?
C136 C135 1.373(5) . ?
C136 H136 0.9300 . ?
C135 C134 1.375(5) . ?
C135 H135 0.9300 . ?
C134 C133 1.377(5) . ?
C134 H134 0.9300 . ?
C133 C132 1.374(4) . ?
C133 H133 0.9300 . ?
C132 H132 0.9300 . ?
C1 C6 1.415(4) . ?
C1 C2 1.420(4) . ?
C6 C5 1.415(4) . ?
C6 C7 1.429(4) . ?
C5 C4 1.351(4) . ?
C5 H5 0.9300 . ?
C4 C3 1.389(4) . ?
C3 C2 1.374(4) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.381(4) . ?
C8 C16 1.407(4) . ?
C9 C10 1.402(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.356(4) . ?
C10 H10 0.9300 . ?
C11 C17 1.413(4) . ?
C11 H11 0.9300 . ?
C17 C12 1.416(4) . ?
C17 C16 1.424(4) . ?
C12 C13 1.353(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.409(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.371(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.436(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
C15 Pd1 N1 82.50(10) . . ?
C15 Pd1 O1 172.98(9) . . ?
N1 Pd1 O1 90.53(8) . . ?
C15 Pd1 P1 96.28(8) . . ?
N1 Pd1 P1 177.48(6) . . ?
O1 Pd1 P1 90.66(5) . . ?
C121 P1 C111 106.05(13) . . ?
C121 P1 C131 102.90(13) . . ?
C111 P1 C131 102.60(13) . . ?
C121 P1 Pd1 113.88(9) . . ?
C111 P1 Pd1 115.66(10) . . ?
C131 P1 Pd1 114.32(9) . . ?
C1 O1 Pd1 125.70(17) . . ?
C7 N1 C8 121.7(2) . . ?
C7 N1 Pd1 124.67(19) . . ?
C8 N1 Pd1 113.46(17) . . ?
C126 C121 C122 119.2(3) . . ?
C126 C121 P1 123.6(2) . . ?
C122 C121 P1 117.2(2) . . ?
C123 C122 C121 120.0(3) . . ?
C123 C122 H122 120.0 . . ?
C121 C122 H122 120.0 . . ?
C124 C123 C122 120.2(3) . . ?
C124 C123 H123 119.9 . . ?
C122 C123 H123 119.9 . . ?
C125 C124 C123 120.2(3) . . ?
C125 C124 H124 119.9 . . ?
C123 C124 H124 119.9 . . ?
C124 C125 C126 120.9(3) . . ?
C124 C125 H125 119.6 . . ?
C126 C125 H125 119.6 . . ?
C121 C126 C125 119.5(3) . . ?
C121 C126 H126 120.2 . . ?
C125 C126 H126 120.2 . . ?
C112 C111 C116 119.1(3) . . ?
C112 C111 P1 120.0(2) . . ?
C116 C111 P1 121.0(2) . . ?
C111 C112 C113 119.7(3) . . ?
C111 C112 H112 120.1 . . ?
C113 C112 H112 120.1 . . ?
C114 C113 C112 120.6(3) . . ?
C114 C113 H113 119.7 . . ?
C112 C113 H113 119.7 . . ?
C113 C114 C115 120.2(3) . . ?
C113 C114 H114 119.9 . . ?
C115 C114 H114 119.9 . . ?
C114 C115 C116 119.9(3) . . ?
C114 C115 H115 120.1 . . ?
C116 C115 H115 120.1 . . ?
C115 C116 C111 120.6(3) . . ?
C115 C116 H116 119.7 . . ?
C111 C116 H116 119.7 . . ?
C136 C131 C132 117.9(3) . . ?
C136 C131 P1 122.8(2) . . ?
C132 C131 P1 119.3(2) . . ?
C135 C136 C131 121.0(3) . . ?
C135 C136 H136 119.5 . . ?
C131 C136 H136 119.5 . . ?
C136 C135 C134 120.7(3) . . ?
C136 C135 H135 119.7 . . ?
C134 C135 H135 119.7 . . ?
C135 C134 C133 119.0(3) . . ?
C135 C134 H134 120.5 . . ?
C133 C134 H134 120.5 . . ?
C132 C133 C134 120.4(3) . . ?
C132 C133 H133 119.8 . . ?
C134 C133 H133 119.8 . . ?
C133 C132 C131 121.0(3) . . ?
C133 C132 H132 119.5 . . ?
C131 C132 H132 119.5 . . ?
O1 C1 C6 125.5(2) . . ?
O1 C1 C2 118.1(2) . . ?
C6 C1 C2 116.4(3) . . ?
C5 C6 C1 119.5(2) . . ?
C5 C6 C7 115.9(2) . . ?
C1 C6 C7 124.6(3) . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 Cl1 119.5(2) . . ?
C3 C4 Cl1 120.1(2) . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C2 C1 122.7(3) . . ?
C3 C2 H2 118.6 . . ?
C1 C2 H2 118.6 . . ?
N1 C7 C6 127.7(3) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C9 C8 C16 120.9(3) . . ?
C9 C8 N1 125.5(3) . . ?
C16 C8 N1 113.6(2) . . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C17 121.5(3) . . ?
C10 C11 H11 119.2 . . ?
C17 C11 H11 119.2 . . ?
C11 C17 C12 123.7(3) . . ?
C11 C17 C16 118.1(3) . . ?
C12 C17 C16 118.2(3) . . ?
C13 C12 C17 119.7(3) . . ?
C13 C12 H12 120.1 . . ?
C17 C12 H12 120.1 . . ?
C12 C13 C14 121.8(3) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 122.0(3) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C14 C15 C16 116.5(3) . . ?
C14 C15 Pd1 132.6(2) . . ?
C16 C15 Pd1 110.86(19) . . ?
C8 C16 C17 119.1(3) . . ?
C8 C16 C15 119.1(2) . . ?
C17 C16 C15 121.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.49
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_jd22
_database_code_depnum_ccdc_archive 'CCDC 965743'
_audit_update_record             
;
2013-10-10 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H28 N O P Pd'
_chemical_formula_weight         663.99

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   8.9539(3)
_cell_length_b                   14.4207(4)
_cell_length_c                   23.0345(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.811(2)
_cell_angle_gamma                90.00
_cell_volume                     2972.76(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_T_max  0.906
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24465
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         26.41
_reflns_number_total             6072
_reflns_number_gt                4013
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1050P)²+2.0717P] 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         6072
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1473
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_restrained_S_all      0.774
_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
Pd1 Pd 0.02051(4) 0.55698(2) 0.135115(13) 0.04171(14) Uani 1 1 d . . .
P1 P -0.09082(13) 0.54122(8) 0.22158(5) 0.0395(3) Uani 1 1 d . . .
O1 O 0.0240(4) 0.6983(2) 0.14543(14) 0.0583(9) Uani 1 1 d . . .
C1 C 0.0799(5) 0.7584(3) 0.1106(2) 0.0519(12) Uani 1 1 d . . .
C10 C 0.1705(5) 0.7389(3) 0.06299(19) 0.0452(10) Uani 1 1 d . . .
C8 C 0.2330(5) 0.8165(4) 0.0310(2) 0.0550(12) Uani 1 1 d . . .
C9 C 0.1880(6) 0.9074(4) 0.0440(3) 0.0683(15) Uani 1 1 d . . .
C3 C 0.0931(7) 0.9233(4) 0.0906(3) 0.0779(17) Uani 1 1 d . . .
H3 H 0.0647 0.9837 0.0991 0.094 Uiso 1 1 calc R . .
C2 C 0.0426(6) 0.8529(4) 0.1231(2) 0.0705(16) Uani 1 1 d . . .
H2 H -0.0176 0.8659 0.1542 0.085 Uiso 1 1 calc R . .
C6 C 0.3823(8) 0.8819(5) -0.0455(3) 0.094(2) Uani 1 1 d . . .
H6 H 0.4483 0.8731 -0.0754 0.113 Uiso 1 1 calc R . .
C7 C 0.3354(6) 0.8056(4) -0.0138(2) 0.0766(17) Uani 1 1 d . . .
H7 H 0.3719 0.7469 -0.0223 0.092 Uiso 1 1 calc R . .
C11 C 0.1960(5) 0.6479(3) 0.04327(19) 0.0492(11) Uani 1 1 d . . .
H11 H 0.2549 0.6430 0.0109 0.059 Uiso 1 1 calc R . .
N1 N 0.1484(4) 0.5695(2) 0.06419(14) 0.0426(9) Uani 1 1 d . . .
C12 C 0.1848(5) 0.4831(3) 0.03889(18) 0.0480(11) Uani 1 1 d . . .
C20 C 0.1073(5) 0.4073(3) 0.06409(18) 0.0464(11) Uani 1 1 d . . .
C21 C 0.1241(6) 0.3171(3) 0.04059(19) 0.0542(12) Uani 1 1 d . . .
C15 C 0.2265(7) 0.3044(4) -0.0038(2) 0.0728(16) Uani 1 1 d . . .
H15 H 0.2403 0.2455 -0.0191 0.087 Uiso 1 1 calc R . .
C14 C 0.3050(7) 0.3767(4) -0.0244(2) 0.0789(18) Uani 1 1 d . . .
H14 H 0.3747 0.3661 -0.0528 0.095 Uiso 1 1 calc R . .
C13 C 0.2840(6) 0.4669(4) -0.0041(2) 0.0636(14) Uani 1 1 d . . .
H13 H 0.3372 0.5158 -0.0197 0.076 Uiso 1 1 calc R . .
C16 C 0.0373(6) 0.2451(4) 0.0634(2) 0.0640(15) Uani 1 1 d . . .
H16 H 0.0453 0.1852 0.0489 0.077 Uiso 1 1 calc R . .
C17 C -0.0577(7) 0.2631(4) 0.1064(2) 0.0663(15) Uani 1 1 d . . .
H17 H -0.1165 0.2154 0.1203 0.080 Uiso 1 1 calc R . .
C18 C -0.0698(6) 0.3511(3) 0.1305(2) 0.0543(12) Uani 1 1 d . . .
H18 H -0.1357 0.3604 0.1604 0.065 Uiso 1 1 calc R . .
C19 C 0.0124(5) 0.4246(3) 0.11146(19) 0.0470(11) Uani 1 1 d . . .
C131 C -0.0508(5) 0.4380(3) 0.26505(19) 0.0433(10) Uani 1 1 d . . .
C132 C -0.1467(6) 0.4067(4) 0.3064(2) 0.0561(12) Uani 1 1 d . . .
H132 H -0.2387 0.4354 0.3105 0.067 Uiso 1 1 calc R . .
C133 C -0.1067(7) 0.3325(4) 0.3420(2) 0.0713(15) Uani 1 1 d . . .
H133 H -0.1712 0.3126 0.3703 0.086 Uiso 1 1 calc R . .
C134 C 0.0261(8) 0.2890(4) 0.3356(2) 0.0721(16) Uani 1 1 d . . .
H134 H 0.0524 0.2394 0.3596 0.087 Uiso 1 1 calc R . .
C135 C 0.1222(6) 0.3181(4) 0.2939(2) 0.0659(15) Uani 1 1 d . . .
H135 H 0.2129 0.2879 0.2895 0.079 Uiso 1 1 calc R . .
C136 C 0.0842(6) 0.3921(3) 0.2585(2) 0.0540(12) Uani 1 1 d . . .
H136 H 0.1490 0.4113 0.2301 0.065 Uiso 1 1 calc R . .
C111 C -0.0284(5) 0.6341(3) 0.26980(17) 0.0427(10) Uani 1 1 d . . .
C116 C -0.0873(6) 0.7229(3) 0.2623(2) 0.0595(13) Uani 1 1 d . . .
H116 H -0.1648 0.7333 0.2353 0.071 Uiso 1 1 calc R . .
C115 C -0.0298(7) 0.7957(4) 0.2953(2) 0.0688(15) Uani 1 1 d . . .
H115 H -0.0699 0.8548 0.2906 0.083 Uiso 1 1 calc R . .
C114 C 0.0865(7) 0.7812(4) 0.3352(2) 0.0730(16) Uani 1 1 d . . .
H114 H 0.1248 0.8305 0.3570 0.088 Uiso 1 1 calc R . .
C113 C 0.1444(6) 0.6951(4) 0.3423(2) 0.0677(15) Uani 1 1 d . . .
H113 H 0.2232 0.6855 0.3689 0.081 Uiso 1 1 calc R . .
C112 C 0.0872(5) 0.6211(4) 0.3102(2) 0.0529(12) Uani 1 1 d . . .
H112 H 0.1270 0.5621 0.3159 0.063 Uiso 1 1 calc R . .
C121 C -0.2931(5) 0.5521(3) 0.21807(19) 0.0427(10) Uani 1 1 d . . .
C126 C -0.3693(5) 0.5292(3) 0.1665(2) 0.0528(12) Uani 1 1 d . . .
H126 H -0.3159 0.5098 0.1347 0.063 Uiso 1 1 calc R . .
C125 C -0.5242(6) 0.5350(3) 0.1619(3) 0.0654(15) Uani 1 1 d . . .
H125 H -0.5744 0.5196 0.1273 0.078 Uiso 1 1 calc R . .
C124 C -0.6021(6) 0.5639(4) 0.2090(3) 0.0741(18) Uani 1 1 d . . .
H124 H -0.7057 0.5678 0.2062 0.089 Uiso 1 1 calc R . .
C123 C -0.5284(6) 0.5868(4) 0.2601(3) 0.0706(15) Uani 1 1 d . . .
H123 H -0.5821 0.6059 0.2918 0.085 Uiso 1 1 calc R . .
C122 C -0.3753(5) 0.5816(4) 0.2644(2) 0.0578(13) Uani 1 1 d . . .
H122 H -0.3262 0.5981 0.2991 0.069 Uiso 1 1 calc R . .
C4 C 0.2398(8) 0.9822(5) 0.0106(3) 0.094(2) Uiso 1 1 d . . .
H4 H 0.2088 1.0421 0.0192 0.113 Uiso 1 1 calc R . .
C5 C 0.3336(8) 0.9689(6) -0.0337(3) 0.101(2) Uiso 1 1 d . . .
H5 H 0.3644 1.0189 -0.0558 0.121 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 C19 1.986(5) . ?
Pd1 N1 2.033(4) . ?
Pd1 O1 2.051(3) . ?
Pd1 P1 2.2665(12) . ?
P1 C111 1.817(4) . ?
P1 C121 1.817(4) . ?
P1 C131 1.824(4) . ?
O1 C1 1.292(5) . ?
C1 C10 1.414(6) . ?
C1 C2 1.433(7) . ?
C10 C11 1.410(6) . ?
C10 C8 1.461(6) . ?
C8 C9 1.406(7) . ?
C8 C7 1.411(7) . ?
C9 C3 1.409(8) . ?
C9 C4 1.411(8) . ?
C3 C2 1.348(7) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C6 C5 1.360(9) . ?
C6 C7 1.392(8) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C11 N1 1.306(5) . ?
C11 H11 0.9300 . ?
N1 C12 1.417(5) . ?
C12 C13 1.371(6) . ?
C12 C20 1.428(7) . ?
C20 C21 1.419(6) . ?
C20 C19 1.426(6) . ?
C21 C15 1.407(7) . ?
C21 C16 1.409(7) . ?
C15 C14 1.352(8) . ?
C15 H15 0.9300 . ?
C14 C13 1.397(7) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C16 C17 1.350(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.369(6) . ?
C18 H18 0.9300 . ?
C131 C132 1.378(6) . ?
C131 C136 1.391(6) . ?
C132 C133 1.387(7) . ?
C132 H132 0.9300 . ?
C133 C134 1.357(8) . ?
C133 H133 0.9300 . ?
C134 C135 1.376(8) . ?
C134 H134 0.9300 . ?
C135 C136 1.378(7) . ?
C135 H135 0.9300 . ?
C136 H136 0.9300 . ?
C111 C112 1.382(6) . ?
C111 C116 1.394(6) . ?
C116 C115 1.385(7) . ?
C116 H116 0.9300 . ?
C115 C114 1.382(8) . ?
C115 H115 0.9300 . ?
C114 C113 1.354(8) . ?
C114 H114 0.9300 . ?
C113 C112 1.387(7) . ?
C113 H113 0.9300 . ?
C112 H112 0.9300 . ?
C121 C122 1.383(6) . ?
C121 C126 1.390(6) . ?
C126 C125 1.391(7) . ?
C126 H126 0.9300 . ?
C125 C124 1.373(8) . ?
C125 H125 0.9300 . ?
C124 C123 1.371(8) . ?
C124 H124 0.9300 . ?
C123 C122 1.373(7) . ?
C123 H123 0.9300 . ?
C122 H122 0.9300 . ?
C4 C5 1.355(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?

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
C19 Pd1 N1 83.18(17) . . ?
C19 Pd1 O1 170.68(15) . . ?
N1 Pd1 O1 89.90(13) . . ?
C19 Pd1 P1 97.55(14) . . ?
N1 Pd1 P1 171.79(10) . . ?
O1 Pd1 P1 90.20(9) . . ?
C111 P1 C121 104.5(2) . . ?
C111 P1 C131 102.4(2) . . ?
C121 P1 C131 105.8(2) . . ?
C111 P1 Pd1 109.16(14) . . ?
C121 P1 Pd1 114.69(15) . . ?
C131 P1 Pd1 118.70(15) . . ?
C1 O1 Pd1 126.9(3) . . ?
O1 C1 C10 126.2(4) . . ?
O1 C1 C2 114.6(4) . . ?
C10 C1 C2 119.2(4) . . ?
C11 C10 C1 122.6(4) . . ?
C11 C10 C8 118.8(4) . . ?
C1 C10 C8 118.5(4) . . ?
C9 C8 C7 117.2(5) . . ?
C9 C8 C10 119.3(5) . . ?
C7 C8 C10 123.5(5) . . ?
C8 C9 C3 119.8(5) . . ?
C8 C9 C4 119.7(6) . . ?
C3 C9 C4 120.5(6) . . ?
C2 C3 C9 121.4(5) . . ?
C2 C3 H3 119.3 . . ?
C9 C3 H3 119.3 . . ?
C3 C2 C1 121.4(5) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C5 C6 C7 121.3(6) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C8 120.6(6) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
N1 C11 C10 129.0(4) . . ?
N1 C11 H11 115.5 . . ?
C10 C11 H11 115.5 . . ?
C11 N1 C12 121.8(4) . . ?
C11 N1 Pd1 124.9(3) . . ?
C12 N1 Pd1 113.3(3) . . ?
C13 C12 N1 127.5(5) . . ?
C13 C12 C20 119.8(5) . . ?
N1 C12 C20 112.6(4) . . ?
C21 C20 C19 121.6(5) . . ?
C21 C20 C12 119.2(4) . . ?
C19 C20 C12 119.1(4) . . ?
C15 C21 C16 123.7(5) . . ?
C15 C21 C20 118.4(5) . . ?
C16 C21 C20 117.9(5) . . ?
C14 C15 C21 120.8(5) . . ?
C14 C15 H15 119.6 . . ?
C21 C15 H15 119.6 . . ?
C15 C14 C13 121.6(5) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C12 C13 C14 119.8(5) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C17 C16 C21 119.9(5) . . ?
C17 C16 H16 120.1 . . ?
C21 C16 H16 120.1 . . ?
C16 C17 C18 121.9(5) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C19 C18 C17 121.9(5) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 116.7(4) . . ?
C18 C19 Pd1 132.1(4) . . ?
C20 C19 Pd1 111.1(3) . . ?
C132 C131 C136 118.8(4) . . ?
C132 C131 P1 122.1(4) . . ?
C136 C131 P1 119.0(4) . . ?
C131 C132 C133 120.4(5) . . ?
C131 C132 H132 119.8 . . ?
C133 C132 H132 119.8 . . ?
C134 C133 C132 120.2(5) . . ?
C134 C133 H133 119.9 . . ?
C132 C133 H133 119.9 . . ?
C133 C134 C135 120.3(5) . . ?
C133 C134 H134 119.9 . . ?
C135 C134 H134 119.9 . . ?
C134 C135 C136 120.1(5) . . ?
C134 C135 H135 120.0 . . ?
C136 C135 H135 120.0 . . ?
C135 C136 C131 120.2(5) . . ?
C135 C136 H136 119.9 . . ?
C131 C136 H136 119.9 . . ?
C112 C111 C116 118.7(4) . . ?
C112 C111 P1 121.4(4) . . ?
C116 C111 P1 119.6(3) . . ?
C115 C116 C111 119.8(5) . . ?
C115 C116 H116 120.1 . . ?
C111 C116 H116 120.1 . . ?
C114 C115 C116 120.6(5) . . ?
C114 C115 H115 119.7 . . ?
C116 C115 H115 119.7 . . ?
C113 C114 C115 119.7(5) . . ?
C113 C114 H114 120.1 . . ?
C115 C114 H114 120.1 . . ?
C114 C113 C112 120.5(5) . . ?
C114 C113 H113 119.7 . . ?
C112 C113 H113 119.7 . . ?
C111 C112 C113 120.7(5) . . ?
C111 C112 H112 119.6 . . ?
C113 C112 H112 119.6 . . ?
C122 C121 C126 118.3(4) . . ?
C122 C121 P1 123.1(3) . . ?
C126 C121 P1 118.6(4) . . ?
C121 C126 C125 120.8(5) . . ?
C121 C126 H126 119.6 . . ?
C125 C126 H126 119.6 . . ?
C124 C125 C126 119.2(5) . . ?
C124 C125 H125 120.4 . . ?
C126 C125 H125 120.4 . . ?
C123 C124 C125 120.6(5) . . ?
C123 C124 H124 119.7 . . ?
C125 C124 H124 119.7 . . ?
C124 C123 C122 120.1(5) . . ?
C124 C123 H123 119.9 . . ?
C122 C123 H123 119.9 . . ?
C123 C122 C121 121.0(5) . . ?
C123 C122 H122 119.5 . . ?
C121 C122 H122 119.5 . . ?
C5 C4 C9 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C9 C4 H4 119.2 . . ?
C4 C5 C6 119.5(7) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.41
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.111
####################################################################### 
# 
# 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_jd11
_database_code_depnum_ccdc_archive 'CCDC 965744'
_audit_update_record             
;
2013-10-10 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H50 N2 O4 P2 Pd2'
_chemical_formula_weight         1161.78

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.6555(2)
_cell_length_b                   12.6136(3)
_cell_length_c                   13.6905(3)
_cell_angle_alpha                104.8440(10)
_cell_angle_beta                 107.3350(10)
_cell_angle_gamma                105.7500(10)
_cell_volume                     1277.47(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  0.885
_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21569
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.65
_reflns_number_total             5886
_reflns_number_gt                5321
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.4119P] 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         5886
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.091288(18) 0.197161(12) 0.441782(11) 0.02991(6) Uani 1 1 d . . .
P1 P -0.01606(6) 0.32678(4) 0.38823(4) 0.02992(11) Uani 1 1 d . . .
O1 O 0.1757(2) 0.30366(13) 0.60494(11) 0.0429(3) Uani 1 1 d . . .
O2 O 0.5322(3) 0.24848(16) 0.98362(13) 0.0644(5) Uani 1 1 d . . .
N1 N 0.1992(2) 0.08308(14) 0.48617(13) 0.0337(3) Uani 1 1 d . . .
C1 C 0.2569(3) 0.28164(17) 0.68936(16) 0.0356(4) Uani 1 1 d . . .
C2 C 0.2892(3) 0.35721(19) 0.79590(18) 0.0449(5) Uani 1 1 d . . .
H2 H 0.2477 0.4183 0.8022 0.054 Uiso 1 1 calc R . .
C3 C 0.3789(3) 0.3438(2) 0.88954(18) 0.0492(5) Uani 1 1 d . . .
H3 H 0.3971 0.3954 0.9577 0.059 Uiso 1 1 calc R . .
C4 C 0.4434(3) 0.2532(2) 0.88398(17) 0.0451(5) Uani 1 1 d . . .
C8 C 0.5779(4) 0.1486(2) 0.9796(2) 0.0640(7) Uani 1 1 d . . .
H8A H 0.4768 0.0778 0.9327 0.096 Uiso 1 1 calc R . .
H8B H 0.6208 0.1472 1.0523 0.096 Uiso 1 1 calc R . .
H8C H 0.6671 0.1527 0.9510 0.096 Uiso 1 1 calc R . .
C5 C 0.4140(3) 0.1776(2) 0.78423(18) 0.0442(5) Uani 1 1 d . . .
H5 H 0.4574 0.1175 0.7807 0.053 Uiso 1 1 calc R . .
C6 C 0.3181(3) 0.18740(18) 0.68419(16) 0.0360(4) Uani 1 1 d . . .
C7 C 0.2883(3) 0.09809(18) 0.58599(17) 0.0389(4) Uani 1 1 d . . .
H7 H 0.3396 0.0433 0.5946 0.047 Uiso 1 1 calc R . .
C9 C 0.1740(3) -0.01446(17) 0.39468(17) 0.0374(4) Uani 1 1 d . . .
C10 C 0.2355(4) -0.1029(2) 0.3999(2) 0.0536(6) Uani 1 1 d . . .
H10 H 0.3003 -0.1029 0.4677 0.064 Uiso 1 1 calc R . .
C11 C 0.1997(4) -0.1940(2) 0.3020(2) 0.0615(7) Uani 1 1 d . . .
H11 H 0.2412 -0.2542 0.3056 0.074 Uiso 1 1 calc R . .
C12 C 0.1057(3) -0.1952(2) 0.2024(2) 0.0537(6) Uani 1 1 d . . .
H12 H 0.0845 -0.2560 0.1388 0.064 Uiso 1 1 calc R . .
C18 C 0.0396(3) -0.10544(18) 0.19391(18) 0.0411(5) Uani 1 1 d . . .
C13 C -0.0583(3) -0.1021(2) 0.09244(18) 0.0477(5) Uani 1 1 d . . .
H13 H -0.0839 -0.1617 0.0268 0.057 Uiso 1 1 calc R . .
C14 C -0.1148(3) -0.0122(2) 0.09080(18) 0.0465(5) Uani 1 1 d . . .
H14 H -0.1789 -0.0107 0.0236 0.056 Uiso 1 1 calc R . .
C15 C -0.0789(3) 0.07868(19) 0.18834(17) 0.0399(5) Uani 1 1 d . . .
H15 H -0.1206 0.1387 0.1839 0.048 Uiso 1 1 calc R . .
C16 C 0.0162(2) 0.08198(17) 0.29043(16) 0.0322(4) Uani 1 1 d . . .
C17 C 0.0753(3) -0.01292(17) 0.29208(16) 0.0341(4) Uani 1 1 d . . .
C121 C 0.0906(3) 0.40104(17) 0.31444(18) 0.0404(5) Uani 1 1 d . . .
C122 C 0.2654(3) 0.4744(2) 0.3719(3) 0.0615(7) Uani 1 1 d . . .
H122 H 0.3221 0.4823 0.4443 0.074 Uiso 1 1 calc R . .
C123 C 0.3570(4) 0.5358(3) 0.3235(3) 0.0799(10) Uani 1 1 d . . .
H123 H 0.4737 0.5858 0.3637 0.096 Uiso 1 1 calc R . .
C124 C 0.2765(5) 0.5232(3) 0.2170(3) 0.0794(10) Uani 1 1 d . . .
H124 H 0.3380 0.5644 0.1844 0.095 Uiso 1 1 calc R . .
C125 C 0.1054(5) 0.4500(3) 0.1582(3) 0.0815(10) Uani 1 1 d . . .
H125 H 0.0512 0.4407 0.0852 0.098 Uiso 1 1 calc R . .
C126 C 0.0108(4) 0.3887(2) 0.2069(2) 0.0619(7) Uani 1 1 d . . .
H126 H -0.1061 0.3396 0.1664 0.074 Uiso 1 1 calc R . .
C111 C -0.2511(3) 0.27129(17) 0.31281(15) 0.0341(4) Uani 1 1 d . . .
C116 C -0.3397(3) 0.3334(2) 0.26398(19) 0.0490(6) Uani 1 1 d . . .
H116 H -0.2776 0.4052 0.2622 0.059 Uiso 1 1 calc R . .
C115 C -0.5213(3) 0.2876(3) 0.2178(2) 0.0622(7) Uani 1 1 d . . .
H115 H -0.5804 0.3286 0.1843 0.075 Uiso 1 1 calc R . .
C114 C -0.6138(3) 0.1827(3) 0.2212(2) 0.0649(7) Uani 1 1 d . . .
H114 H -0.7353 0.1539 0.1918 0.078 Uiso 1 1 calc R . .
C113 C -0.5284(3) 0.1201(3) 0.2675(3) 0.0665(7) Uani 1 1 d . . .
H113 H -0.5916 0.0482 0.2685 0.080 Uiso 1 1 calc R . .
C112 C -0.3484(3) 0.1639(2) 0.3127(2) 0.0485(5) Uani 1 1 d . . .
H112 H -0.2911 0.1206 0.3437 0.058 Uiso 1 1 calc R . .
C131 C 0.0264(3) 0.45014(17) 0.51092(16) 0.0371(4) Uani 1 1 d . . .
H13A H -0.0353 0.4192 0.5524 0.044 Uiso 1 1 calc R . .
H13B H 0.1503 0.4828 0.5568 0.044 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 C16 1.9923(19) . ?
Pd1 N1 2.0376(15) . ?
Pd1 O1 2.0700(14) . ?
Pd1 P1 2.2598(5) . ?
P1 C111 1.816(2) . ?
P1 C121 1.822(2) . ?
P1 C131 1.8331(19) . ?
O1 C1 1.301(2) . ?
O2 C4 1.378(3) . ?
O2 C8 1.413(3) . ?
N1 C7 1.288(3) . ?
N1 C9 1.426(2) . ?
C1 C2 1.419(3) . ?
C1 C6 1.421(3) . ?
C2 C3 1.365(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.396(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.354(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C5 C6 1.430(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.415(3) . ?
C7 H7 0.9300 . ?
C9 C10 1.369(3) . ?
C9 C17 1.418(3) . ?
C10 C11 1.408(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.358(4) . ?
C11 H11 0.9300 . ?
C12 C18 1.416(3) . ?
C12 H12 0.9300 . ?
C18 C13 1.413(3) . ?
C18 C17 1.420(3) . ?
C13 C14 1.354(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.403(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.426(3) . ?
C121 C126 1.374(3) . ?
C121 C122 1.386(3) . ?
C122 C123 1.383(4) . ?
C122 H122 0.9300 . ?
C123 C124 1.360(5) . ?
C123 H123 0.9300 . ?
C124 C125 1.364(5) . ?
C124 H124 0.9300 . ?
C125 C126 1.398(4) . ?
C125 H125 0.9300 . ?
C126 H126 0.9300 . ?
C111 C112 1.387(3) . ?
C111 C116 1.392(3) . ?
C116 C115 1.390(3) . ?
C116 H116 0.9300 . ?
C115 C114 1.369(4) . ?
C115 H115 0.9300 . ?
C114 C113 1.365(4) . ?
C114 H114 0.9300 . ?
C113 C112 1.378(3) . ?
C113 H113 0.9300 . ?
C112 H112 0.9300 . ?
C131 C131 1.518(4) 2_566 ?
C131 H13A 0.9700 . ?
C131 H13B 0.9700 . ?

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
C16 Pd1 N1 82.98(7) . . ?
C16 Pd1 O1 174.03(6) . . ?
N1 Pd1 O1 91.19(6) . . ?
C16 Pd1 P1 95.75(6) . . ?
N1 Pd1 P1 176.49(5) . . ?
O1 Pd1 P1 90.14(4) . . ?
C111 P1 C121 108.67(10) . . ?
C111 P1 C131 103.87(9) . . ?
C121 P1 C131 102.71(10) . . ?
C111 P1 Pd1 116.01(6) . . ?
C121 P1 Pd1 115.33(7) . . ?
C131 P1 Pd1 108.79(6) . . ?
C1 O1 Pd1 125.47(12) . . ?
C4 O2 C8 116.40(18) . . ?
C7 N1 C9 122.11(16) . . ?
C7 N1 Pd1 124.50(13) . . ?
C9 N1 Pd1 113.33(12) . . ?
O1 C1 C2 118.35(18) . . ?
O1 C1 C6 125.22(18) . . ?
C2 C1 C6 116.42(18) . . ?
C3 C2 C1 122.6(2) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
C2 C3 C4 120.7(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 O2 125.3(2) . . ?
C5 C4 C3 119.1(2) . . ?
O2 C4 C3 115.6(2) . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C5 C6 121.9(2) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C1 125.00(18) . . ?
C7 C6 C5 115.78(18) . . ?
C1 C6 C5 119.21(19) . . ?
N1 C7 C6 128.18(18) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
C10 C9 C17 121.00(19) . . ?
C10 C9 N1 126.0(2) . . ?
C17 C9 N1 113.03(16) . . ?
C9 C10 C11 119.5(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 121.1(2) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C18 120.9(2) . . ?
C11 C12 H12 119.5 . . ?
C18 C12 H12 119.5 . . ?
C13 C18 C12 123.3(2) . . ?
C13 C18 C17 118.18(19) . . ?
C12 C18 C17 118.5(2) . . ?
C14 C13 C18 119.9(2) . . ?
C14 C13 H13 120.0 . . ?
C18 C13 H13 120.0 . . ?
C13 C14 C15 121.4(2) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 122.14(19) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C17 116.41(18) . . ?
C15 C16 Pd1 132.04(15) . . ?
C17 C16 Pd1 111.55(14) . . ?
C9 C17 C18 118.98(18) . . ?
C9 C17 C16 119.08(17) . . ?
C18 C17 C16 121.93(18) . . ?
C126 C121 C122 118.3(2) . . ?
C126 C121 P1 124.82(19) . . ?
C122 C121 P1 116.86(18) . . ?
C123 C122 C121 121.2(3) . . ?
C123 C122 H122 119.4 . . ?
C121 C122 H122 119.4 . . ?
C124 C123 C122 120.0(3) . . ?
C124 C123 H123 120.0 . . ?
C122 C123 H123 120.0 . . ?
C123 C124 C125 119.9(3) . . ?
C123 C124 H124 120.0 . . ?
C125 C124 H124 120.0 . . ?
C124 C125 C126 120.6(3) . . ?
C124 C125 H125 119.7 . . ?
C126 C125 H125 119.7 . . ?
C121 C126 C125 120.0(3) . . ?
C121 C126 H126 120.0 . . ?
C125 C126 H126 120.0 . . ?
C112 C111 C116 118.37(19) . . ?
C112 C111 P1 116.80(15) . . ?
C116 C111 P1 124.59(16) . . ?
C115 C116 C111 119.8(2) . . ?
C115 C116 H116 120.1 . . ?
C111 C116 H116 120.1 . . ?
C114 C115 C116 120.6(2) . . ?
C114 C115 H115 119.7 . . ?
C116 C115 H115 119.7 . . ?
C113 C114 C115 120.2(2) . . ?
C113 C114 H114 119.9 . . ?
C115 C114 H114 119.9 . . ?
C114 C113 C112 119.9(3) . . ?
C114 C113 H113 120.1 . . ?
C112 C113 H113 120.1 . . ?
C113 C112 C111 121.2(2) . . ?
C113 C112 H112 119.4 . . ?
C111 C112 H112 119.4 . . ?
C131 C131 P1 115.42(18) 2_566 . ?
C131 C131 H13A 108.4 2_566 . ?
P1 C131 H13A 108.4 . . ?
C131 C131 H13B 108.4 2_566 . ?
P1 C131 H13B 108.4 . . ?
H13A C131 H13B 107.5 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.65
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_jd-pdpy
_database_code_depnum_ccdc_archive 'CCDC 965745'
_audit_update_record             
;
2013-10-10 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 N2 O2 Pd'
_chemical_formula_weight         478.85

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P21/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                   14.3458(4)
_cell_length_b                   15.7571(5)
_cell_length_c                   26.8926(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.016(2)
_cell_angle_gamma                90.00
_cell_volume                     6064.1(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            102218
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         27.64
_reflns_number_total             14085
_reflns_number_gt                10882
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0667P)²+7.6335P] 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         14085
_refine_ls_number_parameters     794
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1196
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_refine_ls_shift/su_max          0.412
_refine_ls_shift/su_mean         0.007

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 0.42992(2) 0.680330(18) 0.376825(10) 0.05139(9) Uani 1 1 d . . .
Pd2 Pd 0.078791(19) 0.639332(18) 0.134200(10) 0.04768(8) Uani 1 1 d . . .
Pd3 Pd 0.377187(16) 0.349172(16) 0.370750(9) 0.04124(7) Uani 1 1 d . . .
O1 O 0.4581(2) 0.59843(19) 0.32002(11) 0.0728(8) Uani 1 1 d . . .
O2 O 0.2150(9) 0.3906(4) 0.2118(3) 0.301(7) Uani 1 1 d . . .
O3 O 0.03855(17) 0.73812(18) 0.17827(10) 0.0593(7) Uani 1 1 d . . .
O4 O 0.2531(2) 0.9183(2) 0.31935(12) 0.0822(9) Uani 1 1 d . . .
O5 O 0.39857(16) 0.24550(16) 0.32484(10) 0.0540(6) Uani 1 1 d . . .
O6 O 0.1344(3) 0.0603(2) 0.21196(13) 0.0913(10) Uani 1 1 d . . .
O7 O 0.4654(2) 0.7520(3) 0.24709(16) 0.1111(14) Uani 1 1 d . . .
N1 N 0.2926(2) 0.6764(2) 0.35987(13) 0.0590(8) Uani 1 1 d . . .
N2 N 0.5700(2) 0.6808(2) 0.39809(12) 0.0557(7) Uani 1 1 d . . .
N3 N 0.2122(2) 0.64705(19) 0.15926(11) 0.0500(7) Uani 1 1 d . . .
N4 N -0.0573(2) 0.63075(19) 0.10672(11) 0.0497(7) Uani 1 1 d . . .
N5 N 0.23898(18) 0.34527(16) 0.35716(10) 0.0402(6) Uani 1 1 d . . .
N6 N 0.51859(19) 0.35804(18) 0.38433(11) 0.0458(6) Uani 1 1 d . . .
C1 C 0.3959(4) 0.5519(3) 0.29590(15) 0.0750(13) Uani 1 1 d . . .
C2 C 0.4245(5) 0.4850(3) 0.26616(18) 0.104(2) Uani 1 1 d . . .
H2 H 0.4881 0.4756 0.2638 0.124 Uiso 1 1 calc R . .
C3 C 0.3610(9) 0.4326(4) 0.2403(2) 0.144(4) Uani 1 1 d . . .
H3 H 0.3828 0.3865 0.2229 0.172 Uiso 1 1 calc R . .
C4 C 0.2698(9) 0.4463(5) 0.2396(3) 0.152(5) Uani 1 1 d . . .
C5 C 0.2355(5) 0.5099(3) 0.2681(2) 0.112(2) Uani 1 1 d . . .
H5 H 0.1713 0.5179 0.2682 0.134 Uiso 1 1 calc R . .
C6 C 0.2970(4) 0.5634(3) 0.29748(17) 0.0824(16) Uani 1 1 d . . .
C7 C 0.2535(4) 0.6239(3) 0.32702(19) 0.0780(14) Uani 1 1 d . . .
H7 H 0.1887 0.6268 0.3225 0.094 Uiso 1 1 calc R . .
C9 C 0.2398(3) 0.7311(3) 0.38869(18) 0.0672(11) Uani 1 1 d . . .
C10 C 0.1454(3) 0.7432(4) 0.3845(3) 0.0986(18) Uani 1 1 d . . .
H10 H 0.1081 0.7136 0.3607 0.118 Uiso 1 1 calc R . .
C11 C 0.1053(4) 0.8006(4) 0.4163(3) 0.117(2) Uani 1 1 d . . .
H11 H 0.0410 0.8087 0.4134 0.140 Uiso 1 1 calc R . .
C12 C 0.1569(4) 0.8441(4) 0.4509(3) 0.107(2) Uani 1 1 d . . .
H12 H 0.1277 0.8813 0.4717 0.129 Uiso 1 1 calc R . .
C13 C 0.3137(5) 0.8811(3) 0.4909(2) 0.0891(15) Uani 1 1 d . . .
H13 H 0.2885 0.9196 0.5125 0.107 Uiso 1 1 calc R . .
C14 C 0.4064(4) 0.8695(3) 0.49241(19) 0.0817(14) Uani 1 1 d . . .
H14 H 0.4445 0.9016 0.5146 0.098 Uiso 1 1 calc R . .
C15 C 0.4478(3) 0.8103(3) 0.46154(15) 0.0633(10) Uani 1 1 d . . .
H15 H 0.5123 0.8027 0.4645 0.076 Uiso 1 1 calc R . .
C16 C 0.3945(3) 0.7634(2) 0.42721(13) 0.0514(8) Uani 1 1 d . . .
C17 C 0.2959(3) 0.7768(2) 0.42471(16) 0.0598(10) Uani 1 1 d . . .
C18 C 0.2538(4) 0.8347(3) 0.4562(2) 0.0775(13) Uani 1 1 d . . .
C19 C 0.6027(3) 0.6536(3) 0.44304(17) 0.0655(11) Uani 1 1 d . . .
H19 H 0.5598 0.6401 0.4662 0.079 Uiso 1 1 calc R . .
C20 C 0.6956(3) 0.6444(3) 0.4570(2) 0.0749(13) Uani 1 1 d . . .
H20 H 0.7145 0.6253 0.4888 0.090 Uiso 1 1 calc R . .
C21 C 0.7605(3) 0.6633(3) 0.4239(3) 0.0851(16) Uani 1 1 d . . .
C22 C 0.7277(4) 0.6904(4) 0.3783(2) 0.105(2) Uani 1 1 d . . .
H22 H 0.7697 0.7033 0.3546 0.126 Uiso 1 1 calc R . .
C23 C 0.6333(4) 0.6992(4) 0.36623(18) 0.0853(15) Uani 1 1 d . . .
H23 H 0.6134 0.7187 0.3346 0.102 Uiso 1 1 calc R . .
C24 C 0.8645(4) 0.6536(5) 0.4383(3) 0.137(3) Uani 1 1 d . . .
H24A H 0.8858 0.7007 0.4587 0.206 Uiso 1 1 calc R . .
H24B H 0.8982 0.6521 0.4087 0.206 Uiso 1 1 calc R . .
H24C H 0.8752 0.6017 0.4565 0.206 Uiso 1 1 calc R . .
C69 C 0.1895(2) 0.4059(2) 0.38341(12) 0.0430(7) Uani 1 1 d . . .
C77 C 0.2491(2) 0.4579(2) 0.41479(12) 0.0427(7) Uani 1 1 d . . .
C76 C 0.3472(2) 0.4430(2) 0.41573(12) 0.0410(7) Uani 1 1 d . . .
C46 C 0.1239(3) 0.5432(2) 0.09562(13) 0.0535(8) Uani 1 1 d . . .
C47 C 0.2218(3) 0.5302(2) 0.10565(13) 0.0566(9) Uani 1 1 d . . .
C48 C 0.2693(3) 0.4625(3) 0.08387(15) 0.0697(12) Uani 1 1 d . . .
C42 C 0.3667(4) 0.4572(3) 0.09449(18) 0.0823(15) Uani 1 1 d . . .
H42 H 0.3998 0.4132 0.0809 0.099 Uiso 1 1 calc R . .
C41 C 0.4129(4) 0.5148(4) 0.12409(19) 0.0854(16) Uani 1 1 d . . .
H41 H 0.4775 0.5104 0.1296 0.102 Uiso 1 1 calc R . .
C40 C 0.3661(3) 0.5811(3) 0.14675(16) 0.0687(11) Uani 1 1 d . . .
H40 H 0.3989 0.6202 0.1671 0.082 Uiso 1 1 calc R . .
C39 C 0.2714(3) 0.5869(2) 0.13832(13) 0.0545(9) Uani 1 1 d . . .
C37 C 0.2434(2) 0.7011(3) 0.19302(13) 0.0528(8) Uani 1 1 d . . .
H37 H 0.3074 0.6995 0.2014 0.063 Uiso 1 1 calc R . .
C36 C 0.1922(2) 0.7624(2) 0.21877(13) 0.0513(8) Uani 1 1 d . . .
C35 C 0.2465(3) 0.8114(3) 0.25491(14) 0.0570(9) Uani 1 1 d . . .
H35 H 0.3107 0.8030 0.2589 0.068 Uiso 1 1 calc R . .
C34 C 0.2065(3) 0.8694(3) 0.28321(16) 0.0638(10) Uani 1 1 d . . .
C38 C 0.3517(3) 0.9098(3) 0.32452(19) 0.0807(13) Uani 1 1 d . . .
H38A H 0.3678 0.8514 0.3304 0.121 Uiso 1 1 calc R . .
H38B H 0.3762 0.9436 0.3521 0.121 Uiso 1 1 calc R . .
H38C H 0.3778 0.9288 0.2945 0.121 Uiso 1 1 calc R . .
C33 C 0.1110(3) 0.8822(3) 0.27742(18) 0.0760(13) Uani 1 1 d . . .
H33 H 0.0831 0.9215 0.2974 0.091 Uiso 1 1 calc R . .
C32 C 0.0568(3) 0.8372(3) 0.24230(17) 0.0721(12) Uani 1 1 d . . .
H32 H -0.0072 0.8472 0.2389 0.087 Uiso 1 1 calc R . .
C31 C 0.0956(3) 0.7765(3) 0.21130(14) 0.0547(9) Uani 1 1 d . . .
C43 C 0.2155(4) 0.4071(3) 0.05179(17) 0.0831(15) Uani 1 1 d . . .
H43 H 0.2441 0.3607 0.0379 0.100 Uiso 1 1 calc R . .
C44 C 0.1234(4) 0.4207(3) 0.04106(18) 0.0831(14) Uani 1 1 d . . .
H44 H 0.0902 0.3846 0.0189 0.100 Uiso 1 1 calc R . .
C45 C 0.0765(3) 0.4886(3) 0.06269(16) 0.0693(11) Uani 1 1 d . . .
H45 H 0.0130 0.4966 0.0546 0.083 Uiso 1 1 calc R . .
C49 C -0.1120(3) 0.5647(3) 0.11562(16) 0.0642(10) Uani 1 1 d . . .
H49 H -0.0853 0.5181 0.1324 0.077 Uiso 1 1 calc R . .
C50 C -0.2052(3) 0.5621(3) 0.10134(17) 0.0730(12) Uani 1 1 d . . .
H50 H -0.2403 0.5145 0.1083 0.088 Uiso 1 1 calc R . .
C51 C -0.2474(3) 0.6299(3) 0.07665(15) 0.0635(11) Uani 1 1 d . . .
C52 C -0.1904(3) 0.6965(3) 0.06626(14) 0.0615(10) Uani 1 1 d . . .
H52 H -0.2153 0.7429 0.0486 0.074 Uiso 1 1 calc R . .
C53 C -0.0973(3) 0.6955(2) 0.08167(14) 0.0543(9) Uani 1 1 d . . .
H53 H -0.0606 0.7420 0.0743 0.065 Uiso 1 1 calc R . .
C54 C -0.3499(3) 0.6297(4) 0.0619(2) 0.0959(18) Uani 1 1 d . . .
H54A H -0.3668 0.6820 0.0452 0.144 Uiso 1 1 calc R . .
H54B H -0.3842 0.6242 0.0911 0.144 Uiso 1 1 calc R . .
H54C H -0.3645 0.5829 0.0399 0.144 Uiso 1 1 calc R . .
C61 C 0.3306(3) 0.2037(2) 0.30051(13) 0.0498(8) Uani 1 1 d . . .
C66 C 0.2345(2) 0.2242(2) 0.30008(12) 0.0461(7) Uani 1 1 d . . .
C65 C 0.1672(3) 0.1756(2) 0.27087(13) 0.0550(9) Uani 1 1 d . . .
H65 H 0.1041 0.1894 0.2708 0.066 Uiso 1 1 calc R . .
C64 C 0.1943(3) 0.1091(3) 0.24301(15) 0.0643(10) Uani 1 1 d . . .
C68 C 0.0396(4) 0.0775(4) 0.2138(3) 0.119(2) Uani 1 1 d . . .
H68A H 0.0225 0.0728 0.2475 0.178 Uiso 1 1 calc R . .
H68B H 0.0041 0.0375 0.1932 0.178 Uiso 1 1 calc R . .
H68C H 0.0268 0.1340 0.2018 0.178 Uiso 1 1 calc R . .
C63 C 0.2871(3) 0.0865(3) 0.24426(17) 0.0721(12) Uani 1 1 d . . .
H63 H 0.3051 0.0403 0.2257 0.087 Uiso 1 1 calc R . .
C62 C 0.3540(3) 0.1316(3) 0.27274(16) 0.0641(10) Uani 1 1 d . . .
H62 H 0.4160 0.1141 0.2736 0.077 Uiso 1 1 calc R . .
C67 C 0.1955(2) 0.2911(2) 0.32716(12) 0.0444(7) Uani 1 1 d . . .
H67 H 0.1310 0.2971 0.3230 0.053 Uiso 1 1 calc R . .
C75 C 0.4031(2) 0.4931(2) 0.44713(13) 0.0496(8) Uani 1 1 d . . .
H75 H 0.4674 0.4845 0.4493 0.060 Uiso 1 1 calc R . .
C74 C 0.3650(3) 0.5572(2) 0.47620(14) 0.0572(9) Uani 1 1 d . . .
H74 H 0.4050 0.5903 0.4969 0.069 Uiso 1 1 calc R . .
C73 C 0.2721(3) 0.5719(2) 0.47480(14) 0.0567(9) Uani 1 1 d . . .
H73 H 0.2489 0.6150 0.4941 0.068 Uiso 1 1 calc R . .
C78 C 0.2103(2) 0.5218(2) 0.44403(13) 0.0498(8) Uani 1 1 d . . .
C72 C 0.1122(3) 0.5319(3) 0.44103(17) 0.0643(10) Uani 1 1 d . . .
H72 H 0.0852 0.5738 0.4597 0.077 Uiso 1 1 calc R . .
C71 C 0.0569(3) 0.4802(3) 0.41070(18) 0.0681(11) Uani 1 1 d . . .
H71 H -0.0076 0.4876 0.4092 0.082 Uiso 1 1 calc R . .
C70 C 0.0942(2) 0.4168(2) 0.38204(15) 0.0567(9) Uani 1 1 d . . .
H70 H 0.0550 0.3820 0.3621 0.068 Uiso 1 1 calc R . .
C83 C 0.5654(3) 0.4288(3) 0.37237(14) 0.0579(9) Uani 1 1 d . . .
H83 H 0.5317 0.4759 0.3606 0.069 Uiso 1 1 calc R . .
C82 C 0.6614(3) 0.4330(3) 0.37717(16) 0.0688(11) Uani 1 1 d . . .
H82 H 0.6913 0.4824 0.3680 0.083 Uiso 1 1 calc R . .
C81 C 0.7137(3) 0.3653(3) 0.39532(17) 0.0655(11) Uani 1 1 d . . .
C84 C 0.8189(3) 0.3697(4) 0.4014(2) 0.0991(19) Uani 1 1 d . . .
H84A H 0.8433 0.3153 0.4117 0.149 Uiso 1 1 calc R . .
H84B H 0.8374 0.4115 0.4261 0.149 Uiso 1 1 calc R . .
H84C H 0.8428 0.3851 0.3702 0.149 Uiso 1 1 calc R . .
C80 C 0.6660(3) 0.2949(3) 0.40842(17) 0.0669(11) Uani 1 1 d . . .
H80 H 0.6984 0.2480 0.4216 0.080 Uiso 1 1 calc R . .
C79 C 0.5700(3) 0.2929(3) 0.40220(15) 0.0561(9) Uani 1 1 d . . .
H79 H 0.5395 0.2436 0.4109 0.067 Uiso 1 1 calc R . .
C8 C 0.1509(8) 0.3886(8) 0.1972(4) 0.176(4) Uiso 1 1 d . . .
H8A H 0.1363 0.4409 0.1801 0.264 Uiso 1 1 calc R . .
H8B H 0.1090 0.3806 0.2231 0.264 Uiso 1 1 calc R . .
H8C H 0.1444 0.3423 0.1740 0.264 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 C16 1.976(4) . ?
Pd1 N1 1.992(3) . ?
Pd1 N2 2.050(3) . ?
Pd1 O1 2.061(3) . ?
Pd2 C46 1.971(4) . ?
Pd2 N3 1.987(3) . ?
Pd2 N4 2.043(3) . ?
Pd2 O3 2.063(2) . ?
Pd3 C76 1.977(3) . ?
Pd3 N5 1.992(3) . ?
Pd3 N6 2.041(3) . ?
Pd3 O5 2.083(2) . ?
O1 C1 1.295(6) . ?
O2 C8 0.975(13) . ?
O2 C4 1.365(8) . ?
O3 C31 1.313(4) . ?
O4 C34 1.376(5) . ?
O4 C38 1.417(5) . ?
O5 C61 1.313(4) . ?
O6 C64 1.389(5) . ?
O6 C68 1.391(7) . ?
N1 C7 1.307(6) . ?
N1 C9 1.414(6) . ?
N2 C23 1.324(5) . ?
N2 C19 1.337(5) . ?
N3 C37 1.302(5) . ?
N3 C39 1.415(5) . ?
N4 C53 1.331(5) . ?
N4 C49 1.336(5) . ?
N5 C67 1.303(4) . ?
N5 C69 1.409(4) . ?
N6 C79 1.334(5) . ?
N6 C83 1.351(5) . ?
C1 C2 1.402(7) . ?
C1 C6 1.433(8) . ?
C2 C3 1.380(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.325(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(13) . ?
C5 C6 1.419(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.415(8) . ?
C7 H7 0.9300 . ?
C9 C10 1.365(6) . ?
C9 C17 1.412(6) . ?
C10 C11 1.395(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.337(10) . ?
C11 H11 0.9300 . ?
C12 C18 1.395(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.339(8) . ?
C13 C18 1.424(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.408(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.427(5) . ?
C17 C18 1.410(6) . ?
C19 C20 1.366(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.364(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.352(8) . ?
C21 C24 1.523(7) . ?
C22 C23 1.377(8) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C69 C70 1.375(5) . ?
C69 C77 1.419(4) . ?
C77 C78 1.416(5) . ?
C77 C76 1.424(4) . ?
C76 C75 1.372(4) . ?
C46 C45 1.379(6) . ?
C46 C47 1.426(5) . ?
C47 C39 1.410(6) . ?
C47 C48 1.415(5) . ?
C48 C42 1.409(7) . ?
C48 C43 1.418(7) . ?
C42 C41 1.350(8) . ?
C42 H42 0.9300 . ?
C41 C40 1.405(6) . ?
C41 H41 0.9300 . ?
C40 C39 1.364(5) . ?
C40 H40 0.9300 . ?
C37 C36 1.422(5) . ?
C37 H37 0.9300 . ?
C36 C31 1.404(5) . ?
C36 C35 1.429(5) . ?
C35 C34 1.343(6) . ?
C35 H35 0.9300 . ?
C34 C33 1.383(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C33 C32 1.377(6) . ?
C33 H33 0.9300 . ?
C32 C31 1.409(5) . ?
C32 H32 0.9300 . ?
C43 C44 1.349(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.411(6) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C49 C50 1.366(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.375(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.371(6) . ?
C51 C54 1.496(6) . ?
C52 C53 1.371(5) . ?
C52 H52 0.9300 . ?
C53 H53 0.9300 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C61 C62 1.412(5) . ?
C61 C66 1.416(5) . ?
C66 C67 1.418(5) . ?
C66 C65 1.424(5) . ?
C65 C64 1.361(6) . ?
C65 H65 0.9300 . ?
C64 C63 1.376(6) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C63 C62 1.382(6) . ?
C63 H63 0.9300 . ?
C62 H62 0.9300 . ?
C67 H67 0.9300 . ?
C75 C74 1.411(5) . ?
C75 H75 0.9300 . ?
C74 C73 1.351(5) . ?
C74 H74 0.9300 . ?
C73 C78 1.411(5) . ?
C73 H73 0.9300 . ?
C78 C72 1.414(5) . ?
C72 C71 1.366(6) . ?
C72 H72 0.9300 . ?
C71 C70 1.392(6) . ?
C71 H71 0.9300 . ?
C70 H70 0.9300 . ?
C83 C82 1.377(6) . ?
C83 H83 0.9300 . ?
C82 C81 1.374(6) . ?
C82 H82 0.9300 . ?
C81 C80 1.363(6) . ?
C81 C84 1.507(6) . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
C80 C79 1.375(5) . ?
C80 H80 0.9300 . ?
C79 H79 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
C16 Pd1 N1 83.09(15) . . ?
C16 Pd1 N2 95.76(14) . . ?
N1 Pd1 N2 176.65(13) . . ?
C16 Pd1 O1 174.99(14) . . ?
N1 Pd1 O1 93.06(14) . . ?
N2 Pd1 O1 88.26(13) . . ?
C46 Pd2 N3 83.21(15) . . ?
C46 Pd2 N4 95.70(14) . . ?
N3 Pd2 N4 178.59(12) . . ?
C46 Pd2 O3 176.14(13) . . ?
N3 Pd2 O3 93.47(11) . . ?
N4 Pd2 O3 87.65(10) . . ?
C76 Pd3 N5 83.03(12) . . ?
C76 Pd3 N6 95.49(12) . . ?
N5 Pd3 N6 177.83(11) . . ?
C76 Pd3 O5 175.26(11) . . ?
N5 Pd3 O5 93.04(10) . . ?
N6 Pd3 O5 88.51(10) . . ?
C1 O1 Pd1 124.2(3) . . ?
C8 O2 C4 137.1(16) . . ?
C31 O3 Pd2 123.4(2) . . ?
C34 O4 C38 116.6(4) . . ?
C61 O5 Pd3 123.7(2) . . ?
C64 O6 C68 115.9(4) . . ?
C7 N1 C9 122.4(4) . . ?
C7 N1 Pd1 123.0(3) . . ?
C9 N1 Pd1 114.5(3) . . ?
C23 N2 C19 116.2(4) . . ?
C23 N2 Pd1 121.6(3) . . ?
C19 N2 Pd1 121.8(3) . . ?
C37 N3 C39 121.9(3) . . ?
C37 N3 Pd2 123.6(2) . . ?
C39 N3 Pd2 114.5(2) . . ?
C53 N4 C49 116.8(3) . . ?
C53 N4 Pd2 120.0(3) . . ?
C49 N4 Pd2 123.1(3) . . ?
C67 N5 C69 121.2(3) . . ?
C67 N5 Pd3 124.1(2) . . ?
C69 N5 Pd3 114.7(2) . . ?
C79 N6 C83 116.7(3) . . ?
C79 N6 Pd3 122.0(2) . . ?
C83 N6 Pd3 121.2(3) . . ?
O1 C1 C2 119.5(6) . . ?
O1 C1 C6 124.3(4) . . ?
C2 C1 C6 116.2(5) . . ?
C3 C2 C1 121.8(8) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 121.8(8) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 O2 115.7(11) . . ?
C3 C4 C5 120.2(7) . . ?
O2 C4 C5 124.0(12) . . ?
C4 C5 C6 120.7(8) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 115.5(6) . . ?
C7 C6 C1 125.4(4) . . ?
C5 C6 C1 119.1(6) . . ?
N1 C7 C6 128.3(5) . . ?
N1 C7 H7 115.8 . . ?
C6 C7 H7 115.8 . . ?
C10 C9 C17 120.0(5) . . ?
C10 C9 N1 127.3(5) . . ?
C17 C9 N1 112.7(3) . . ?
C9 C10 C11 119.3(6) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 121.8(5) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C18 121.0(6) . . ?
C11 C12 H12 119.5 . . ?
C18 C12 H12 119.5 . . ?
C14 C13 C18 120.2(5) . . ?
C14 C13 H13 119.9 . . ?
C18 C13 H13 119.9 . . ?
C13 C14 C15 122.1(5) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 117.2(4) . . ?
C15 C16 Pd1 131.2(3) . . ?
C17 C16 Pd1 111.5(3) . . ?
C18 C17 C9 119.7(4) . . ?
C18 C17 C16 122.1(4) . . ?
C9 C17 C16 118.2(4) . . ?
C12 C18 C17 118.2(6) . . ?
C12 C18 C13 124.3(5) . . ?
C17 C18 C13 117.4(5) . . ?
N2 C19 C20 123.8(4) . . ?
N2 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
C21 C20 C19 119.7(5) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 116.7(5) . . ?
C22 C21 C24 122.3(6) . . ?
C20 C21 C24 121.0(6) . . ?
C21 C22 C23 121.3(5) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
N2 C23 C22 122.2(5) . . ?
N2 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C70 C69 N5 127.3(3) . . ?
C70 C69 C77 120.1(3) . . ?
N5 C69 C77 112.6(3) . . ?
C78 C77 C69 119.8(3) . . ?
C78 C77 C76 122.2(3) . . ?
C69 C77 C76 118.0(3) . . ?
C75 C76 C77 116.7(3) . . ?
C75 C76 Pd3 131.6(3) . . ?
C77 C76 Pd3 111.7(2) . . ?
C45 C46 C47 117.8(4) . . ?
C45 C46 Pd2 130.7(3) . . ?
C47 C46 Pd2 111.4(3) . . ?
C39 C47 C48 119.9(4) . . ?
C39 C47 C46 118.4(3) . . ?
C48 C47 C46 121.8(4) . . ?
C42 C48 C47 117.5(5) . . ?
C42 C48 C43 125.2(4) . . ?
C47 C48 C43 117.2(4) . . ?
C41 C42 C48 121.2(4) . . ?
C41 C42 H42 119.4 . . ?
C48 C42 H42 119.4 . . ?
C42 C41 C40 121.7(5) . . ?
C42 C41 H41 119.2 . . ?
C40 C41 H41 119.1 . . ?
C39 C40 C41 118.7(5) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C40 C39 C47 120.9(4) . . ?
C40 C39 N3 126.7(4) . . ?
C47 C39 N3 112.4(3) . . ?
N3 C37 C36 128.3(3) . . ?
N3 C37 H37 115.9 . . ?
C36 C37 H37 115.9 . . ?
C31 C36 C37 125.2(3) . . ?
C31 C36 C35 119.8(3) . . ?
C37 C36 C35 115.0(3) . . ?
C34 C35 C36 121.3(4) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C34 O4 125.2(4) . . ?
C35 C34 C33 119.6(4) . . ?
O4 C34 C33 115.2(4) . . ?
O4 C38 H38A 109.5 . . ?
O4 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O4 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 C33 C34 120.6(4) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C33 C32 C31 121.9(4) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
O3 C31 C36 125.9(3) . . ?
O3 C31 C32 117.4(3) . . ?
C36 C31 C32 116.7(3) . . ?
C44 C43 C48 121.1(4) . . ?
C44 C43 H43 119.5 . . ?
C48 C43 H43 119.5 . . ?
C43 C44 C45 121.3(5) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C46 C45 C44 120.7(5) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
N4 C49 C50 123.3(4) . . ?
N4 C49 H49 118.4 . . ?
C50 C49 H49 118.4 . . ?
C49 C50 C51 120.1(4) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C52 C51 C50 116.5(4) . . ?
C52 C51 C54 122.4(5) . . ?
C50 C51 C54 121.1(5) . . ?
C51 C52 C53 120.8(4) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
N4 C53 C52 122.5(4) . . ?
N4 C53 H53 118.7 . . ?
C52 C53 H53 118.7 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O5 C61 C62 118.1(3) . . ?
O5 C61 C66 125.3(3) . . ?
C62 C61 C66 116.5(3) . . ?
C61 C66 C67 125.7(3) . . ?
C61 C66 C65 120.3(3) . . ?
C67 C66 C65 114.0(3) . . ?
C64 C65 C66 120.5(4) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 H65 119.7 . . ?
C65 C64 C63 120.0(4) . . ?
C65 C64 O6 124.6(4) . . ?
C63 C64 O6 115.4(4) . . ?
O6 C68 H68A 109.5 . . ?
O6 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
O6 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C64 C63 C62 120.9(4) . . ?
C64 C63 H63 119.5 . . ?
C62 C63 H63 119.5 . . ?
C63 C62 C61 121.7(4) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.2 . . ?
N5 C67 C66 128.1(3) . . ?
N5 C67 H67 116.0 . . ?
C66 C67 H67 116.0 . . ?
C76 C75 C74 121.4(3) . . ?
C76 C75 H75 119.3 . . ?
C74 C75 H75 119.3 . . ?
C73 C74 C75 121.8(3) . . ?
C73 C74 H74 119.1 . . ?
C75 C74 H74 119.1 . . ?
C74 C73 C78 119.9(3) . . ?
C74 C73 H73 120.1 . . ?
C78 C73 H73 120.1 . . ?
C73 C78 C72 123.5(3) . . ?
C73 C78 C77 118.0(3) . . ?
C72 C78 C77 118.5(3) . . ?
C71 C72 C78 120.0(4) . . ?
C71 C72 H72 120.0 . . ?
C78 C72 H72 120.0 . . ?
C72 C71 C70 121.9(3) . . ?
C72 C71 H71 119.0 . . ?
C70 C71 H71 119.0 . . ?
C69 C70 C71 119.6(3) . . ?
C69 C70 H70 120.2 . . ?
C71 C70 H70 120.2 . . ?
N6 C83 C82 121.9(4) . . ?
N6 C83 H83 119.0 . . ?
C82 C83 H83 119.0 . . ?
C81 C82 C83 120.9(4) . . ?
C81 C82 H82 119.6 . . ?
C83 C82 H82 119.6 . . ?
C80 C81 C82 116.9(4) . . ?
C80 C81 C84 121.8(5) . . ?
C82 C81 C84 121.4(5) . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C81 C80 C79 120.3(4) . . ?
C81 C80 H80 119.9 . . ?
C79 C80 H80 119.9 . . ?
N6 C79 C80 123.4(4) . . ?
N6 C79 H79 118.3 . . ?
C80 C79 H79 118.3 . . ?
O2 C8 H8A 109.7 . . ?
O2 C8 H8B 109.8 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 108.9 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.601
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.073
