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

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

data_pdsash
_database_code_depnum_ccdc_archive 'CCDC 1047924'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-08-25T14:20:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 pdsash
;
_chemical_name_common            pdsash
_chemical_formula_moiety         'C32 H25 N2 O3 P Pd'
_chemical_formula_sum            'C32 H25 N2 O3 P Pd'
_chemical_formula_weight         622.91

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'



_cell_length_a                   9.2348(5)
_cell_length_b                   10.1529(5)
_cell_length_c                   15.3801(10)
_cell_angle_alpha                97.685(4)
_cell_angle_beta                 90.359(4)
_cell_angle_gamma                110.319(4)
_cell_volume                     1338.00(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    870
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

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

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_special_details           
;
 30 mm, 2 degrees, 6 seconds per degree.
;

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

_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_T_max  0.9322

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

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_number            10984
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             6588
_reflns_number_gt                5302
_reflns_threshold_expression     >2σ(I)

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

_computing_data_collection       KappaCCD
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0393P)²+0.4772P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6588
_refine_ls_number_parameters     355
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.114

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0292(3) -0.1153(3) 0.65230(18) 0.0167(6) Uani 1 1 d . . .
C2 C -0.0109(4) -0.1465(3) 0.56069(19) 0.0218(6) Uani 1 1 d . . .
H2 H 0.046 -0.0821 0.5232 0.026 Uiso 1 1 calc R . .
C3 C -0.1298(4) -0.2672(3) 0.5247(2) 0.0253(7) Uani 1 1 d . . .
H3 H -0.1529 -0.2851 0.463 0.03 Uiso 1 1 calc R . .
C4 C -0.2162(4) -0.3630(3) 0.57728(19) 0.0272(7) Uani 1 1 d . . .
H4 H -0.299 -0.4458 0.5522 0.033 Uiso 1 1 calc R . .
C5 C -0.1808(4) -0.3366(3) 0.66610(19) 0.0240(6) Uani 1 1 d . . .
H5 H -0.2407 -0.4021 0.7021 0.029 Uiso 1 1 calc R . .
C6 C -0.0579(3) -0.2152(3) 0.70583(18) 0.0177(6) Uani 1 1 d . . .
C7 C -0.0291(3) -0.2055(3) 0.79886(18) 0.0187(6) Uani 1 1 d . . .
H7 H -0.0986 -0.2752 0.8289 0.022 Uiso 1 1 calc R . .
C8 C 0.2249(3) -0.0010(3) 0.96874(17) 0.0164(6) Uani 1 1 d . . .
C9 C 0.2620(3) 0.0123(3) 1.06388(18) 0.0186(6) Uani 1 1 d . . .
C10 C 0.1587(4) -0.0678(3) 1.11921(18) 0.0199(6) Uani 1 1 d . . .
C11 C 0.1970(4) -0.0481(3) 1.20918(19) 0.0252(7) Uani 1 1 d . . .
H11 H 0.1249 -0.0992 1.2473 0.03 Uiso 1 1 calc R . .
C12 C 0.3409(4) 0.0463(3) 1.2428(2) 0.0309(8) Uani 1 1 d . . .
H12 H 0.3675 0.0582 1.3038 0.037 Uiso 1 1 calc R . .
C13 C 0.4466(4) 0.1240(3) 1.1879(2) 0.0294(7) Uani 1 1 d . . .
H13 H 0.5452 0.188 1.2113 0.035 Uiso 1 1 calc R . .
C14 C 0.4076(4) 0.1074(3) 1.0995(2) 0.0250(7) Uani 1 1 d . . .
H14 H 0.4795 0.1607 1.0622 0.03 Uiso 1 1 calc R . .
C15 C 0.5520(3) 0.3644(3) 0.85224(17) 0.0156(5) Uani 1 1 d . . .
C16 C 0.6295(3) 0.2930(3) 0.89582(18) 0.0195(6) Uani 1 1 d . . .
H16 H 0.6062 0.194 0.879 0.023 Uiso 1 1 calc R . .
C17 C 0.7402(4) 0.3666(3) 0.96357(19) 0.0231(6) Uani 1 1 d . . .
H17 H 0.7948 0.3187 0.9917 0.028 Uiso 1 1 calc R . .
C18 C 0.7707(4) 0.5107(3) 0.98988(18) 0.0223(6) Uani 1 1 d . . .
H18 H 0.8467 0.5613 1.0358 0.027 Uiso 1 1 calc R . .
C19 C 0.6902(4) 0.5803(3) 0.94913(19) 0.0224(6) Uani 1 1 d . . .
H19 H 0.7089 0.6779 0.9687 0.027 Uiso 1 1 calc R . .
C20 C 0.5833(3) 0.5089(3) 0.88042(18) 0.0185(6) Uani 1 1 d . . .
H20 H 0.5305 0.5581 0.8521 0.022 Uiso 1 1 calc R . .
C21 C 0.3201(3) 0.3820(3) 0.73180(17) 0.0165(6) Uani 1 1 d . . .
C22 C 0.1827(3) 0.3813(3) 0.76822(19) 0.0221(6) Uani 1 1 d . . .
H22 H 0.136 0.3169 0.808 0.027 Uiso 1 1 calc R . .
C23 C 0.1133(4) 0.4754(3) 0.7462(2) 0.0299(7) Uani 1 1 d . . .
H23 H 0.0201 0.4759 0.7718 0.036 Uiso 1 1 calc R . .
C24 C 0.1795(4) 0.5678(3) 0.6874(2) 0.0295(7) Uani 1 1 d . . .
H24 H 0.1309 0.6306 0.6718 0.035 Uiso 1 1 calc R . .
C25 C 0.3161(4) 0.5689(3) 0.65125(19) 0.0232(6) Uani 1 1 d . . .
H25 H 0.3619 0.633 0.6111 0.028 Uiso 1 1 calc R . .
C26 C 0.3867(3) 0.4772(3) 0.67332(18) 0.0198(6) Uani 1 1 d . . .
H26 H 0.4811 0.4789 0.6485 0.024 Uiso 1 1 calc R . .
C27 C 0.5230(3) 0.2383(3) 0.66904(17) 0.0170(6) Uani 1 1 d . . .
C28 C 0.6830(3) 0.2760(3) 0.67457(19) 0.0211(6) Uani 1 1 d . . .
H28 H 0.7391 0.3134 0.7297 0.025 Uiso 1 1 calc R . .
C29 C 0.7608(4) 0.2589(4) 0.5990(2) 0.0278(7) Uani 1 1 d . . .
H29 H 0.8701 0.2847 0.6028 0.033 Uiso 1 1 calc R . .
C30 C 0.6805(4) 0.2048(3) 0.51886(19) 0.0250(7) Uani 1 1 d . . .
H30 H 0.7344 0.1941 0.4675 0.03 Uiso 1 1 calc R . .
C31 C 0.5211(4) 0.1662(3) 0.51320(19) 0.0262(7) Uani 1 1 d . . .
H31 H 0.4657 0.1287 0.4579 0.031 Uiso 1 1 calc R . .
C32 C 0.4420(4) 0.1820(3) 0.58795(18) 0.0233(6) Uani 1 1 d . . .
H32 H 0.3325 0.1544 0.5839 0.028 Uiso 1 1 calc R . .
N1 N 0.0843(3) -0.1089(2) 0.84338(14) 0.0157(5) Uani 1 1 d . . .
N2 N 0.1031(3) -0.1103(2) 0.93369(15) 0.0180(5) Uani 1 1 d . . .
O1 O 0.1456(2) 0.0041(2) 0.67813(12) 0.0209(4) Uani 1 1 d . . .
O2 O 0.3132(2) 0.09689(19) 0.92648(12) 0.0170(4) Uani 1 1 d . . .
P1 P 0.41218(8) 0.26215(7) 0.76346(4) 0.01453(15) Uani 1 1 d . . .
Pd1 Pd 0.23723(2) 0.05892(2) 0.800342(13) 0.01601(8) Uani 1 1 d . . .
O3 O 0.0186(3) -0.1654(2) 1.08972(14) 0.0237(5) Uani 1 1 d . . .
H3A H 0.005(4) -0.172(4) 1.040(2) 0.036 Uiso 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.320(3) . ?
C1 C2 1.420(4) . ?
C1 C6 1.420(4) . ?
C2 C3 1.375(4) . ?
C2 H2 0.95 . ?
C3 C4 1.384(4) . ?
C3 H3 0.95 . ?
C4 C5 1.371(4) . ?
C4 H4 0.95 . ?
C5 C6 1.414(4) . ?
C5 H5 0.95 . ?
C6 C7 1.438(4) . ?
C7 N1 1.274(4) . ?
C7 H7 0.95 . ?
C8 O2 1.301(3) . ?
C8 N2 1.324(4) . ?
C8 C9 1.478(4) . ?
C9 C10 1.397(4) . ?
C9 C14 1.410(4) . ?
C10 O3 1.358(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.387(5) . ?
C11 H11 0.95 . ?
C12 C13 1.393(5) . ?
C12 H12 0.95 . ?
C13 C14 1.377(4) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?
C15 C20 1.398(4) . ?
C15 C16 1.404(4) . ?
C15 P1 1.810(3) . ?
C16 C17 1.392(4) . ?
C16 H16 0.95 . ?
C17 C18 1.392(4) . ?
C17 H17 0.95 . ?
C18 C19 1.387(4) . ?
C18 H18 0.95 . ?
C19 C20 1.379(4) . ?
C19 H19 0.95 . ?
C20 H20 0.95 . ?
C21 C22 1.389(4) . ?
C21 C26 1.396(4) . ?
C21 P1 1.820(3) . ?
C22 C23 1.395(4) . ?
C22 H22 0.95 . ?
C23 C24 1.382(5) . ?
C23 H23 0.95 . ?
C24 C25 1.379(4) . ?
C24 H24 0.95 . ?
C25 C26 1.382(4) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C27 C28 1.391(4) . ?
C27 C32 1.394(4) . ?
C27 P1 1.820(3) . ?
C28 C29 1.393(4) . ?
C28 H28 0.95 . ?
C29 C30 1.377(4) . ?
C29 H29 0.95 . ?
C30 C31 1.384(5) . ?
C30 H30 0.95 . ?
C31 C32 1.387(4) . ?
C31 H31 0.95 . ?
C32 H32 0.95 . ?
N1 N2 1.401(3) . ?
N1 Pd1 1.995(2) . ?
O1 Pd1 1.9830(18) . ?
O2 Pd1 1.9998(18) . ?
P1 Pd1 2.2801(7) . ?
O3 H3A 0.76(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 115.7(3) . . ?
O1 C1 C6 127.1(2) . . ?
C2 C1 C6 117.2(2) . . ?
C3 C2 C1 121.9(3) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 122.2(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 115.9(3) . . ?
C1 C6 C7 125.1(3) . . ?
N1 C7 C6 123.9(3) . . ?
N1 C7 H7 118.1 . . ?
C6 C7 H7 118.1 . . ?
O2 C8 N2 125.3(2) . . ?
O2 C8 C9 117.3(2) . . ?
N2 C8 C9 117.4(2) . . ?
C10 C9 C14 119.0(3) . . ?
C10 C9 C8 122.2(3) . . ?
C14 C9 C8 118.8(3) . . ?
O3 C10 C11 117.1(3) . . ?
O3 C10 C9 122.8(3) . . ?
C11 C10 C9 120.1(3) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 119.6(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C9 120.7(3) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C20 C15 C16 119.0(3) . . ?
C20 C15 P1 123.3(2) . . ?
C16 C15 P1 117.7(2) . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 119.8(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 H18 120 . . ?
C17 C18 H18 120 . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 120.4(3) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
C22 C21 C26 119.2(3) . . ?
C22 C21 P1 119.4(2) . . ?
C26 C21 P1 121.4(2) . . ?
C21 C22 C23 119.8(3) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 120.0(3) . . ?
C25 C24 H24 120 . . ?
C23 C24 H24 120 . . ?
C24 C25 C26 120.2(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.5(3) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C28 C27 C32 119.5(3) . . ?
C28 C27 P1 122.9(2) . . ?
C32 C27 P1 117.6(2) . . ?
C27 C28 C29 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 120.5(3) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.9(3) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C32 120.3(3) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 120.0(3) . . ?
C31 C32 H32 120 . . ?
C27 C32 H32 120 . . ?
C7 N1 N2 119.3(2) . . ?
C7 N1 Pd1 126.86(19) . . ?
N2 N1 Pd1 113.67(17) . . ?
C8 N2 N1 110.6(2) . . ?
C1 O1 Pd1 122.80(17) . . ?
C8 O2 Pd1 109.97(16) . . ?
C15 P1 C27 106.29(13) . . ?
C15 P1 C21 105.52(12) . . ?
C27 P1 C21 103.01(13) . . ?
C15 P1 Pd1 113.40(9) . . ?
C27 P1 Pd1 115.42(9) . . ?
C21 P1 Pd1 112.20(10) . . ?
O1 Pd1 N1 93.85(8) . . ?
O1 Pd1 O2 174.29(8) . . ?
N1 Pd1 O2 80.44(8) . . ?
O1 Pd1 P1 90.50(6) . . ?
N1 Pd1 P1 174.77(7) . . ?
O2 Pd1 P1 95.20(6) . . ?
C10 O3 H3A 112(3) . . ?



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

data_pdsnah2
_database_code_depnum_ccdc_archive 'CCDC 1047925'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-10-23T13:30:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 pdsnah
;
_chemical_name_common            pdsnah
_chemical_formula_moiety         'C36 H27 N2 O3 P Pd'
_chemical_formula_sum            'C36 H27 N2 O3 P Pd'
_chemical_formula_weight         672.97

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'



_cell_length_a                   8.8683(4)
_cell_length_b                   21.5484(10)
_cell_length_c                   15.2026(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.079(3)
_cell_angle_gamma                90
_cell_volume                     2888.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    713
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

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

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_special_details           
;
 15 sec., 1 deg., 35 mm
;

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

_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_absorpt_correction_T_min  0.7564
_exptl_absorpt_correction_T_max  0.8663

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

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_number            12436
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_reflns_number_total             7108
_reflns_number_gt                4183
_reflns_threshold_expression     >2σ(I)

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

_computing_data_collection       KappaCCD
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0419P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7108
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.131
_refine_ls_wR_factor_gt          0.1137
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_restrained_S_all      0.935
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.35
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.153

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.2725(4) 0.4472(2) 0.6689(3) 0.0186(10) Uani 1 1 d . . .
C2 C 1.4049(5) 0.4609(2) 0.6276(3) 0.0273(11) Uani 1 1 d . . .
H2 H 1.4287 0.5028 0.6158 0.033 Uiso 1 1 calc R . .
C3 C 1.4992(5) 0.4144(3) 0.6046(3) 0.0292(12) Uani 1 1 d . . .
H3 H 1.5871 0.4249 0.577 0.035 Uiso 1 1 calc R . .
C4 C 1.4691(5) 0.3531(2) 0.6206(3) 0.0260(12) Uani 1 1 d . . .
H4 H 1.536 0.3216 0.6048 0.031 Uiso 1 1 calc R . .
C5 C 1.3403(4) 0.3380(2) 0.6599(3) 0.0244(11) Uani 1 1 d . . .
H5 H 1.3191 0.2955 0.6704 0.029 Uiso 1 1 calc R . .
C6 C 1.2395(4) 0.3840(2) 0.6848(3) 0.0195(10) Uani 1 1 d . . .
C7 C 1.1101(4) 0.3620(2) 0.7258(3) 0.0208(10) Uani 1 1 d . . .
H7 H 1.104 0.3189 0.7381 0.025 Uiso 1 1 calc R . .
C8 C 0.7816(4) 0.4152(2) 0.7998(3) 0.0189(10) Uani 1 1 d . . .
C9 C 0.6408(4) 0.3959(2) 0.8379(3) 0.0172(10) Uani 1 1 d . . .
C10 C 0.5953(4) 0.3326(2) 0.8435(3) 0.0186(10) Uani 1 1 d . . .
C11 C 0.4631(4) 0.3181(2) 0.8785(3) 0.0194(10) Uani 1 1 d . . .
H11 H 0.4338 0.2759 0.8823 0.023 Uiso 1 1 calc R . .
C12 C 0.3694(4) 0.3651(2) 0.9091(3) 0.0161(9) Uani 1 1 d . . .
C13 C 0.2276(4) 0.3522(2) 0.9435(3) 0.0189(10) Uani 1 1 d . . .
H13 H 0.1912 0.3108 0.9444 0.023 Uiso 1 1 calc R . .
C14 C 0.1461(5) 0.3987(2) 0.9745(3) 0.0229(11) Uani 1 1 d . . .
H14 H 0.0524 0.3892 0.9964 0.027 Uiso 1 1 calc R . .
C15 C 0.1958(5) 0.4611(2) 0.9754(3) 0.0250(11) Uani 1 1 d . . .
H15 H 0.1385 0.4929 0.9996 0.03 Uiso 1 1 calc R . .
C16 C 0.3283(4) 0.4747(2) 0.9405(3) 0.0186(10) Uani 1 1 d . . .
H16 H 0.3617 0.5165 0.9395 0.022 Uiso 1 1 calc R . .
C17 C 0.4157(4) 0.4277(2) 0.9062(3) 0.0176(10) Uani 1 1 d . . .
C18 C 0.5509(4) 0.4417(2) 0.8679(3) 0.0207(10) Uani 1 1 d . . .
H18 H 0.5803 0.4838 0.8629 0.025 Uiso 1 1 calc R . .
C19 C 1.0187(4) 0.6254(2) 0.6169(3) 0.0192(10) Uani 1 1 d . . .
C20 C 1.0447(4) 0.5845(2) 0.5484(3) 0.0216(10) Uani 1 1 d . . .
H20 H 1.0245 0.5415 0.554 0.026 Uiso 1 1 calc R . .
C21 C 1.1000(5) 0.6068(3) 0.4723(3) 0.0278(12) Uani 1 1 d . . .
H21 H 1.1178 0.579 0.426 0.033 Uiso 1 1 calc R . .
C22 C 1.1290(5) 0.6696(3) 0.4640(3) 0.0279(12) Uani 1 1 d . . .
H22 H 1.1655 0.685 0.4115 0.033 Uiso 1 1 calc R . .
C23 C 1.1054(5) 0.7097(2) 0.5312(3) 0.0282(11) Uani 1 1 d . . .
H23 H 1.1266 0.7527 0.5255 0.034 Uiso 1 1 calc R . .
C24 C 1.0505(5) 0.6877(2) 0.6074(3) 0.0234(11) Uani 1 1 d . . .
H24 H 1.0345 0.7158 0.6536 0.028 Uiso 1 1 calc R . .
C25 C 1.0338(4) 0.6388(2) 0.8073(3) 0.0149(9) Uani 1 1 d . . .
C26 C 1.1594(4) 0.6119(2) 0.8576(3) 0.0192(10) Uani 1 1 d . . .
H26 H 1.1971 0.5727 0.8415 0.023 Uiso 1 1 calc R . .
C27 C 1.2276(4) 0.6435(2) 0.9312(3) 0.0209(11) Uani 1 1 d . . .
H27 H 1.3122 0.6256 0.9657 0.025 Uiso 1 1 calc R . .
C28 C 1.1734(5) 0.7003(2) 0.9543(3) 0.0221(11) Uani 1 1 d . . .
H28 H 1.2204 0.7213 1.0049 0.026 Uiso 1 1 calc R . .
C29 C 1.0511(5) 0.7273(2) 0.9045(3) 0.0257(11) Uani 1 1 d . . .
H29 H 1.0153 0.7669 0.9204 0.031 Uiso 1 1 calc R . .
C30 C 0.9809(5) 0.6963(2) 0.8314(3) 0.0236(11) Uani 1 1 d . . .
H30 H 0.8962 0.7146 0.7975 0.028 Uiso 1 1 calc R . .
C31 C 0.7493(4) 0.6118(2) 0.7072(3) 0.0190(10) Uani 1 1 d . . .
C32 C 0.6642(5) 0.6261(2) 0.6281(3) 0.0244(11) Uani 1 1 d . . .
H32 H 0.7117 0.6274 0.575 0.029 Uiso 1 1 calc R . .
C33 C 0.5090(4) 0.6386(2) 0.6257(3) 0.0273(12) Uani 1 1 d . . .
H33 H 0.4515 0.6489 0.5713 0.033 Uiso 1 1 calc R . .
C34 C 0.4396(5) 0.6358(2) 0.7035(3) 0.0292(12) Uani 1 1 d . . .
H34 H 0.3342 0.6441 0.7024 0.035 Uiso 1 1 calc R . .
C35 C 0.5244(5) 0.6209(2) 0.7829(3) 0.0268(12) Uani 1 1 d . . .
H35 H 0.4766 0.6189 0.8359 0.032 Uiso 1 1 calc R . .
C36 C 0.6768(4) 0.6090(2) 0.7852(3) 0.0233(11) Uani 1 1 d . . .
H36 H 0.7339 0.5989 0.8398 0.028 Uiso 1 1 calc R . .
N1 N 1.0027(3) 0.39732(18) 0.7468(2) 0.0165(8) Uani 1 1 d . . .
N2 N 0.8769(3) 0.37126(18) 0.7820(2) 0.0185(8) Uani 1 1 d . . .
O1 O 1.1913(3) 0.49613(15) 0.68758(18) 0.0197(7) Uani 1 1 d . . .
O2 O 0.7986(3) 0.47407(15) 0.78571(18) 0.0202(7) Uani 1 1 d . . .
O3 O 0.6805(3) 0.28585(15) 0.8147(2) 0.0231(7) Uani 1 1 d . . .
H3O H 0.7564 0.3008 0.7936 0.035 Uiso 1 1 calc R . .
P1 P 0.94908(12) 0.59293(6) 0.71508(7) 0.0163(3) Uani 1 1 d . . .
Pd1 Pd 0.99202(3) 0.489152(18) 0.73396(2) 0.01591(11) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.325(5) . ?
C1 C6 1.418(6) . ?
C1 C2 1.421(6) . ?
C2 C3 1.373(6) . ?
C2 H2 0.95 . ?
C3 C4 1.374(7) . ?
C3 H3 0.95 . ?
C4 C5 1.384(6) . ?
C4 H4 0.95 . ?
C5 C6 1.414(6) . ?
C5 H5 0.95 . ?
C6 C7 1.442(6) . ?
C7 N1 1.285(5) . ?
C7 H7 0.95 . ?
C8 O2 1.299(5) . ?
C8 N2 1.316(5) . ?
C8 C9 1.490(5) . ?
C9 C18 1.376(6) . ?
C9 C10 1.427(6) . ?
C10 O3 1.359(5) . ?
C10 C11 1.374(5) . ?
C11 C12 1.418(6) . ?
C11 H11 0.95 . ?
C12 C17 1.412(6) . ?
C12 C13 1.440(5) . ?
C13 C14 1.349(6) . ?
C13 H13 0.95 . ?
C14 C15 1.414(7) . ?
C14 H14 0.95 . ?
C15 C16 1.370(6) . ?
C15 H15 0.95 . ?
C16 C17 1.408(6) . ?
C16 H16 0.95 . ?
C17 C18 1.420(5) . ?
C18 H18 0.95 . ?
C19 C24 1.381(6) . ?
C19 C20 1.403(6) . ?
C19 P1 1.815(4) . ?
C20 C21 1.389(6) . ?
C20 H20 0.95 . ?
C21 C22 1.388(7) . ?
C21 H21 0.95 . ?
C22 C23 1.371(7) . ?
C22 H22 0.95 . ?
C23 C24 1.387(6) . ?
C23 H23 0.95 . ?
C24 H24 0.95 . ?
C25 C30 1.389(6) . ?
C25 C26 1.407(6) . ?
C25 P1 1.812(4) . ?
C26 C27 1.393(6) . ?
C26 H26 0.95 . ?
C27 C28 1.374(6) . ?
C27 H27 0.95 . ?
C28 C29 1.383(6) . ?
C28 H28 0.95 . ?
C29 C30 1.386(6) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 C32 1.384(6) . ?
C31 C36 1.410(6) . ?
C31 P1 1.809(4) . ?
C32 C33 1.399(6) . ?
C32 H32 0.95 . ?
C33 C34 1.392(6) . ?
C33 H33 0.95 . ?
C34 C35 1.391(6) . ?
C34 H34 0.95 . ?
C35 C36 1.372(6) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
N1 N2 1.404(4) . ?
N1 Pd1 1.990(4) . ?
O1 Pd1 1.976(2) . ?
O2 Pd1 1.988(3) . ?
O3 H3O 0.84 . ?
P1 Pd1 2.2814(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 127.0(4) . . ?
O1 C1 C2 115.0(4) . . ?
C6 C1 C2 118.0(4) . . ?
C3 C2 C1 121.0(5) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 121.4(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 121.6(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 118.7(4) . . ?
C5 C6 C7 116.1(4) . . ?
C1 C6 C7 125.2(4) . . ?
N1 C7 C6 123.9(5) . . ?
N1 C7 H7 118.1 . . ?
C6 C7 H7 118.1 . . ?
O2 C8 N2 125.4(4) . . ?
O2 C8 C9 117.0(4) . . ?
N2 C8 C9 117.6(4) . . ?
C18 C9 C10 119.2(4) . . ?
C18 C9 C8 117.9(4) . . ?
C10 C9 C8 122.9(4) . . ?
O3 C10 C11 118.9(4) . . ?
O3 C10 C9 121.2(3) . . ?
C11 C10 C9 119.9(4) . . ?
C10 C11 C12 121.3(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C17 C12 C11 119.3(4) . . ?
C17 C12 C13 117.6(4) . . ?
C11 C12 C13 123.1(4) . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 122.1(4) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 118.5(4) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 121.2(4) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C12 120.2(4) . . ?
C16 C17 C18 121.4(4) . . ?
C12 C17 C18 118.4(4) . . ?
C9 C18 C17 121.9(4) . . ?
C9 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C24 C19 C20 118.8(4) . . ?
C24 C19 P1 123.5(3) . . ?
C20 C19 P1 117.7(4) . . ?
C21 C20 C19 120.1(5) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 120.2(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.1(5) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 120.9(4) . . ?
C19 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C30 C25 C26 119.7(4) . . ?
C30 C25 P1 124.5(3) . . ?
C26 C25 P1 115.8(3) . . ?
C27 C26 C25 119.1(4) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C26 120.5(4) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C30 119.8(4) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C25 120.3(4) . . ?
C29 C30 H30 119.8 . . ?
C25 C30 H30 119.8 . . ?
C32 C31 C36 119.0(4) . . ?
C32 C31 P1 123.2(3) . . ?
C36 C31 P1 117.7(3) . . ?
C31 C32 C33 120.7(4) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.4(4) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C35 C34 C33 120.0(4) . . ?
C35 C34 H34 120 . . ?
C33 C34 H34 120 . . ?
C36 C35 C34 120.4(4) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C31 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C7 N1 N2 119.8(4) . . ?
C7 N1 Pd1 126.4(3) . . ?
N2 N1 Pd1 113.8(2) . . ?
C8 N2 N1 110.2(4) . . ?
C1 O1 Pd1 122.9(3) . . ?
C8 O2 Pd1 110.2(3) . . ?
C10 O3 H3O 109.5 . . ?
C31 P1 C25 104.56(19) . . ?
C31 P1 C19 105.93(19) . . ?
C25 P1 C19 106.07(19) . . ?
C31 P1 Pd1 112.23(15) . . ?
C25 P1 Pd1 112.75(15) . . ?
C19 P1 Pd1 114.51(15) . . ?
O1 Pd1 O2 174.30(13) . . ?
O1 Pd1 N1 94.33(12) . . ?
O2 Pd1 N1 80.37(12) . . ?
O1 Pd1 P1 91.38(10) . . ?
O2 Pd1 P1 94.05(10) . . ?
N1 Pd1 P1 173.09(9) . . ?


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

data_pdmssh_0ma
_database_code_depnum_ccdc_archive 'CCDC 1047926'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-08-13T15:11:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 pdmssh
;
_chemical_name_common            pdmssh
_chemical_formula_moiety         'C33 H27 N2 O4 P Pd'
_chemical_formula_sum            'C33 H27 N2 O4 P Pd'
_chemical_formula_weight         652.94

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'



_cell_length_a                   11.0075(5)
_cell_length_b                   28.2609(12)
_cell_length_c                   8.8037(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.227(2)
_cell_angle_gamma                90
_cell_volume                     2736.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    720
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

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

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_special_details           
;
 10 seconds, 0.5 degrees, 40 mm
;

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

_exptl_absorpt_coefficient_mu    0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7997
_exptl_absorpt_correction_T_max  0.9261

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.01
_diffrn_reflns_number            127872
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             6828
_reflns_number_gt                6550
_reflns_threshold_expression     >2σ(I)

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

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

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0170P)²+4.4026P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6828
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.065
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.174
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.072

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.16287(18) -0.00291(7) 0.6533(2) 0.0172(4) Uani 1 1 d . . .
C2 C 0.20110(18) -0.03936(7) 0.5570(2) 0.0208(4) Uani 1 1 d . . .
H2 H 0.2789 -0.0373 0.5144 0.025 Uiso 1 1 calc R . .
C3 C 0.12827(19) -0.07793(7) 0.5229(2) 0.0207(4) Uani 1 1 d . . .
C4 C 0.01350(19) -0.08225(7) 0.5850(2) 0.0208(4) Uani 1 1 d . . .
H4 H -0.0362 -0.1091 0.5632 0.025 Uiso 1 1 calc R . .
C5 C -0.02523(19) -0.04715(8) 0.6771(3) 0.0220(4) Uani 1 1 d . . .
H5 H -0.1037 -0.0499 0.7175 0.026 Uiso 1 1 calc R . .
C6 C 0.04570(18) -0.00654(7) 0.7162(2) 0.0184(4) Uani 1 1 d . . .
C7 C 0.1033(2) -0.14995(8) 0.3826(3) 0.0294(5) Uani 1 1 d . . .
H7A H 0.0862 -0.1687 0.473 0.044 Uiso 1 1 calc R . .
H7B H 0.1471 -0.1695 0.3108 0.044 Uiso 1 1 calc R . .
H7C H 0.0267 -0.1391 0.3342 0.044 Uiso 1 1 calc R . .
C8 C -0.00645(18) 0.02744(8) 0.8130(2) 0.0206(4) Uani 1 1 d . . .
H8 H -0.0866 0.0217 0.8449 0.025 Uiso 1 1 calc R . .
C9 C 0.05576(17) 0.13285(7) 0.9930(2) 0.0167(4) Uani 1 1 d . . .
C10 C 0.00585(18) 0.16937(7) 1.0934(2) 0.0187(4) Uani 1 1 d . . .
C11 C -0.11315(19) 0.16617(8) 1.1482(2) 0.0200(4) Uani 1 1 d . . .
C12 C -0.1536(2) 0.20153(8) 1.2446(3) 0.0253(4) Uani 1 1 d . . .
H12 H -0.2337 0.2001 1.281 0.03 Uiso 1 1 calc R . .
C13 C -0.0782(2) 0.23852(8) 1.2876(3) 0.0268(5) Uani 1 1 d . . .
H13 H -0.1069 0.2619 1.3548 0.032 Uiso 1 1 calc R . .
C14 C 0.0381(2) 0.24235(8) 1.2353(3) 0.0261(5) Uani 1 1 d . . .
H14 H 0.0891 0.268 1.2659 0.031 Uiso 1 1 calc R . .
C15 C 0.07874(19) 0.20789(8) 1.1370(2) 0.0225(4) Uani 1 1 d . . .
H15 H 0.1579 0.2106 1.0986 0.027 Uiso 1 1 calc R . .
C16 C 0.51432(16) 0.06357(6) 0.8013(2) 0.0123(3) Uani 1 1 d . . .
C17 C 0.57377(17) 0.06183(7) 0.9441(2) 0.0161(4) Uani 1 1 d . . .
H17 H 0.5623 0.0866 1.0149 0.019 Uiso 1 1 calc R . .
C18 C 0.64952(18) 0.02418(7) 0.9836(2) 0.0185(4) Uani 1 1 d . . .
H18 H 0.6903 0.0234 1.0806 0.022 Uiso 1 1 calc R . .
C19 C 0.66553(18) -0.01242(7) 0.8808(2) 0.0185(4) Uani 1 1 d . . .
H19 H 0.7177 -0.0381 0.9075 0.022 Uiso 1 1 calc R . .
C20 C 0.60555(19) -0.01145(7) 0.7394(2) 0.0190(4) Uani 1 1 d . . .
H20 H 0.6163 -0.0366 0.6694 0.023 Uiso 1 1 calc R . .
C21 C 0.52980(18) 0.02619(7) 0.7001(2) 0.0163(4) Uani 1 1 d . . .
H21 H 0.4881 0.0266 0.6036 0.02 Uiso 1 1 calc R . .
C22 C 0.41574(17) 0.11838(6) 0.5483(2) 0.0136(3) Uani 1 1 d . . .
C23 C 0.30916(19) 0.12538(7) 0.4609(2) 0.0190(4) Uani 1 1 d . . .
H23 H 0.2326 0.1234 0.5068 0.023 Uiso 1 1 calc R . .
C24 C 0.3143(2) 0.13531(8) 0.3066(2) 0.0244(4) Uani 1 1 d . . .
H24 H 0.2415 0.1401 0.2471 0.029 Uiso 1 1 calc R . .
C25 C 0.4257(2) 0.13824(7) 0.2401(2) 0.0267(5) Uani 1 1 d . . .
H25 H 0.4292 0.1456 0.1351 0.032 Uiso 1 1 calc R . .
C26 C 0.5323(2) 0.13046(8) 0.3255(2) 0.0239(4) Uani 1 1 d . . .
H26 H 0.6084 0.1317 0.2783 0.029 Uiso 1 1 calc R . .
C27 C 0.52801(18) 0.12080(7) 0.4801(2) 0.0176(4) Uani 1 1 d . . .
H27 H 0.6011 0.1159 0.539 0.021 Uiso 1 1 calc R . .
C28 C 0.46195(18) 0.16432(7) 0.8341(2) 0.0147(3) Uani 1 1 d . . .
C29 C 0.3785(2) 0.20032(7) 0.8606(3) 0.0241(4) Uani 1 1 d . . .
H29 H 0.295 0.1959 0.8332 0.029 Uiso 1 1 calc R . .
C30 C 0.4173(3) 0.24264(8) 0.9270(3) 0.0332(5) Uani 1 1 d . . .
H30 H 0.3602 0.2671 0.9438 0.04 Uiso 1 1 calc R . .
C31 C 0.5376(3) 0.24911(8) 0.9681(3) 0.0347(6) Uani 1 1 d . . .
H31 H 0.5633 0.2776 1.0169 0.042 Uiso 1 1 calc R . .
C32 C 0.6214(2) 0.21428(8) 0.9387(3) 0.0303(5) Uani 1 1 d . . .
H32 H 0.7049 0.2192 0.9653 0.036 Uiso 1 1 calc R . .
C33 C 0.58441(19) 0.17206(7) 0.8702(2) 0.0214(4) Uani 1 1 d . . .
H33 H 0.6428 0.1485 0.8482 0.026 Uiso 1 1 calc R . .
N1 N 0.04673(14) 0.06516(6) 0.86045(19) 0.0166(3) Uani 1 1 d . . .
N2 N -0.01360(15) 0.09632(6) 0.9562(2) 0.0196(3) Uani 1 1 d . . .
O1 O 0.16599(12) 0.13915(5) 0.94686(16) 0.0174(3) Uani 1 1 d . . .
O2 O 0.24146(13) 0.03177(5) 0.67565(16) 0.0185(3) Uani 1 1 d . . .
O3 O -0.18983(14) 0.13057(6) 1.11070(19) 0.0256(3) Uani 1 1 d . . .
H3 H -0.145(3) 0.1132(11) 1.054(4) 0.038 Uiso 1 1 d . . .
O4 O 0.17596(15) -0.11018(6) 0.4258(2) 0.0317(4) Uani 1 1 d . . .
P1 P 0.40490(4) 0.109411(16) 0.75138(5) 0.01110(9) Uani 1 1 d . . .
Pd1 Pd 0.212356(12) 0.086148(5) 0.809164(16) 0.01305(4) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.317(2) . ?
C1 C2 1.409(3) . ?
C1 C6 1.427(3) . ?
C2 C3 1.379(3) . ?
C2 H2 0.95 . ?
C3 O4 1.369(3) . ?
C3 C4 1.401(3) . ?
C4 C5 1.361(3) . ?
C4 H4 0.95 . ?
C5 C6 1.423(3) . ?
C5 H5 0.95 . ?
C6 C8 1.420(3) . ?
C7 O4 1.422(3) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N1 1.278(3) . ?
C8 H8 0.95 . ?
C9 O1 1.307(2) . ?
C9 N2 1.317(3) . ?
C9 C10 1.479(3) . ?
C10 C15 1.397(3) . ?
C10 C11 1.416(3) . ?
C11 O3 1.346(3) . ?
C11 C12 1.395(3) . ?
C12 C13 1.379(3) . ?
C12 H12 0.95 . ?
C13 C14 1.381(3) . ?
C13 H13 0.95 . ?
C14 C15 1.388(3) . ?
C14 H14 0.95 . ?
C15 H15 0.95 . ?
C16 C17 1.395(3) . ?
C16 C21 1.397(3) . ?
C16 P1 1.8114(18) . ?
C17 C18 1.388(3) . ?
C17 H17 0.95 . ?
C18 C19 1.390(3) . ?
C18 H18 0.95 . ?
C19 C20 1.387(3) . ?
C19 H19 0.95 . ?
C20 C21 1.387(3) . ?
C20 H20 0.95 . ?
C21 H21 0.95 . ?
C22 C23 1.392(3) . ?
C22 C27 1.397(3) . ?
C22 P1 1.8139(19) . ?
C23 C24 1.390(3) . ?
C23 H23 0.95 . ?
C24 C25 1.382(3) . ?
C24 H24 0.95 . ?
C25 C26 1.386(3) . ?
C25 H25 0.95 . ?
C26 C27 1.391(3) . ?
C26 H26 0.95 . ?
C27 H27 0.95 . ?
C28 C33 1.390(3) . ?
C28 C29 1.396(3) . ?
C28 P1 1.8158(19) . ?
C29 C30 1.391(3) . ?
C29 H29 0.95 . ?
C30 C31 1.372(4) . ?
C30 H30 0.95 . ?
C31 C32 1.380(4) . ?
C31 H31 0.95 . ?
C32 C33 1.390(3) . ?
C32 H32 0.95 . ?
C33 H33 0.95 . ?
N1 N2 1.404(2) . ?
N1 Pd1 1.9858(16) . ?
O1 Pd1 2.0055(14) . ?
O2 Pd1 1.9686(14) . ?
O3 H3 0.87(3) . ?
P1 Pd1 2.2950(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 C2 115.11(18) . . ?
O2 C1 C6 126.42(18) . . ?
C2 C1 C6 118.47(18) . . ?
C3 C2 C1 121.60(19) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
O4 C3 C2 115.36(19) . . ?
O4 C3 C4 124.00(19) . . ?
C2 C3 C4 120.6(2) . . ?
C5 C4 C3 118.49(19) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 123.40(19) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C8 C6 C5 117.36(18) . . ?
C8 C6 C1 125.24(19) . . ?
C5 C6 C1 117.39(19) . . ?
O4 C7 H7A 109.5 . . ?
O4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 124.69(19) . . ?
N1 C8 H8 117.7 . . ?
C6 C8 H8 117.7 . . ?
O1 C9 N2 124.54(18) . . ?
O1 C9 C10 117.49(18) . . ?
N2 C9 C10 117.96(17) . . ?
C15 C10 C11 119.00(19) . . ?
C15 C10 C9 119.05(18) . . ?
C11 C10 C9 121.94(19) . . ?
O3 C11 C12 118.20(19) . . ?
O3 C11 C10 122.92(19) . . ?
C12 C11 C10 118.9(2) . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 121.6(2) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C13 C14 C15 118.6(2) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C14 C15 C10 121.5(2) . . ?
C14 C15 H15 119.3 . . ?
C10 C15 H15 119.3 . . ?
C17 C16 C21 118.91(17) . . ?
C17 C16 P1 121.88(14) . . ?
C21 C16 P1 118.85(14) . . ?
C18 C17 C16 120.61(18) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 119.83(18) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 120.12(18) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.96(18) . . ?
C19 C20 H20 120 . . ?
C21 C20 H20 120 . . ?
C20 C21 C16 120.55(18) . . ?
C20 C21 H21 119.7 . . ?
C16 C21 H21 119.7 . . ?
C23 C22 C27 119.72(18) . . ?
C23 C22 P1 118.59(15) . . ?
C27 C22 P1 121.60(15) . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.8(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.46(19) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 120.1(2) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C22 119.66(19) . . ?
C26 C27 H27 120.2 . . ?
C22 C27 H27 120.2 . . ?
C33 C28 C29 119.02(19) . . ?
C33 C28 P1 122.91(15) . . ?
C29 C28 P1 118.06(16) . . ?
C30 C29 C28 120.3(2) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 120.2(2) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 120.0(2) . . ?
C30 C31 H31 120 . . ?
C32 C31 H31 120 . . ?
C31 C32 C33 120.5(2) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C28 119.9(2) . . ?
C32 C33 H33 120 . . ?
C28 C33 H33 120 . . ?
C8 N1 N2 119.86(17) . . ?
C8 N1 Pd1 125.99(14) . . ?
N2 N1 Pd1 114.15(12) . . ?
C9 N2 N1 110.86(16) . . ?
C9 O1 Pd1 110.32(12) . . ?
C1 O2 Pd1 123.31(13) . . ?
C11 O3 H3 101(2) . . ?
C3 O4 C7 117.91(18) . . ?
C16 P1 C22 105.70(8) . . ?
C16 P1 C28 107.32(9) . . ?
C22 P1 C28 103.92(8) . . ?
C16 P1 Pd1 110.63(6) . . ?
C22 P1 Pd1 110.80(6) . . ?
C28 P1 Pd1 117.64(6) . . ?
O2 Pd1 N1 94.29(6) . . ?
O2 Pd1 O1 174.37(6) . . ?
N1 Pd1 O1 80.11(6) . . ?
O2 Pd1 P1 85.31(4) . . ?
N1 Pd1 P1 179.17(5) . . ?
O1 Pd1 P1 100.31(4) . . ?



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

data_pdmsna_0ma
_database_code_depnum_ccdc_archive 'CCDC 1047927'
_audit_update_record             
;
2015-02-06 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;

_audit_creation_date             2014-08-01T14:15:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 pdmsna
;
_chemical_name_common            pdmsna
_chemical_formula_moiety         'C37 H29 N2 O4 P Pd'
_chemical_formula_sum            'C37 H29 N2 O4 P Pd'
_chemical_formula_weight         702.99

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   15.087(2)
_cell_length_b                   21.144(3)
_cell_length_c                   9.3879(15)
_cell_angle_alpha                90
_cell_angle_beta                 94.528(8)
_cell_angle_gamma                90
_cell_volume                     2985.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2130
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

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

_exptl_crystal_description       piece
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_special_details           
;
 60 seconds, 1 degree, 40 mm
;

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

_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.7373
_exptl_absorpt_correction_T_max  0.9857

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

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_number            40321
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.898
_reflns_number_total             5156
_reflns_number_gt                3641
_reflns_threshold_expression     >2σ(I)

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

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

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0240P)²+11.1340P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5156
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.109

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2773(3) 1.1427(3) -0.0602(6) 0.0260(14) Uani 1 1 d . . .
H7 H 0.275 1.187 -0.0438 0.031 Uiso 1 1 calc R . .
C2 C 0.3142(3) 1.1218(3) -0.1878(6) 0.0254(14) Uani 1 1 d . . .
C3 C 0.3211(3) 1.0576(3) -0.2298(6) 0.0259(14) Uani 1 1 d . . .
C4 C 0.3544(3) 1.0445(3) -0.3608(7) 0.0287(14) Uani 1 1 d . . .
H6 H 0.3569 1.0019 -0.3921 0.034 Uiso 1 1 calc R . .
C5 C 0.3840(4) 1.0923(3) -0.4468(7) 0.0316(15) Uani 1 1 d . . .
C6 C 0.4092(4) 1.0183(3) -0.6308(7) 0.0417(16) Uani 1 1 d . . .
H1 H 0.4412 0.9893 -0.5637 0.063 Uiso 1 1 calc R . .
H2 H 0.4349 1.0164 -0.7233 0.063 Uiso 1 1 calc R . .
H3 H 0.3464 1.0062 -0.6429 0.063 Uiso 1 1 calc R . .
C7 C 0.3804(3) 1.1556(3) -0.4037(7) 0.0318(15) Uani 1 1 d . . .
H5 H 0.4014 1.1884 -0.4615 0.038 Uiso 1 1 calc R . .
C8 C 0.3463(3) 1.1692(3) -0.2782(7) 0.0303(15) Uani 1 1 d . . .
H4 H 0.3438 1.2121 -0.2491 0.036 Uiso 1 1 calc R . .
C9 C 0.1937(3) 1.0859(3) 0.2427(6) 0.0246(14) Uani 1 1 d . . .
C10 C 0.1595(3) 1.1042(2) 0.3804(6) 0.0228(13) Uani 1 1 d . . .
C11 C 0.1258(3) 1.0580(3) 0.4636(7) 0.0285(14) Uani 1 1 d . . .
H8 H 0.1244 1.0156 0.4303 0.034 Uiso 1 1 calc R . .
C12 C 0.0932(3) 1.0715(3) 0.5963(7) 0.0276(14) Uani 1 1 d . . .
C13 C 0.0572(4) 1.0239(3) 0.6788(7) 0.0336(15) Uani 1 1 d . . .
H13 H 0.0526 0.982 0.6427 0.04 Uiso 1 1 calc R . .
C14 C 0.0283(4) 1.0372(3) 0.8111(7) 0.0352(16) Uani 1 1 d . . .
H12 H 0.003 1.0049 0.8653 0.042 Uiso 1 1 calc R . .
C15 C 0.0370(3) 1.0992(3) 0.8651(7) 0.0304(15) Uani 1 1 d . . .
H11 H 0.0189 1.1083 0.9575 0.036 Uiso 1 1 calc R . .
C16 C 0.0704(3) 1.1456(3) 0.7872(7) 0.0317(15) Uani 1 1 d . . .
H10 H 0.0754 1.1871 0.8259 0.038 Uiso 1 1 calc R . .
C17 C 0.0984(3) 1.1342(3) 0.6489(6) 0.0245(13) Uani 1 1 d . . .
C18 C 0.1329(3) 1.1810(3) 0.5604(6) 0.0272(14) Uani 1 1 d . . .
H9 H 0.136 1.2235 0.5935 0.033 Uiso 1 1 calc R . .
C19 C 0.1615(3) 1.1678(3) 0.4317(6) 0.0248(14) Uani 1 1 d . . .
C20 C 0.2754(3) 0.8824(2) 0.2437(6) 0.0239(13) Uani 1 1 d . . .
C21 C 0.3560(4) 0.8663(3) 0.3170(7) 0.0307(14) Uani 1 1 d . . .
H18 H 0.4076 0.8618 0.266 0.037 Uiso 1 1 calc R . .
C22 C 0.3621(4) 0.8566(3) 0.4629(7) 0.0376(17) Uani 1 1 d . . .
H17 H 0.4176 0.8456 0.5115 0.045 Uiso 1 1 calc R . .
C23 C 0.2883(4) 0.8630(3) 0.5376(7) 0.0367(16) Uani 1 1 d . . .
H14 H 0.2923 0.8565 0.638 0.044 Uiso 1 1 calc R . .
C24 C 0.2072(4) 0.8789(3) 0.4653(7) 0.0344(15) Uani 1 1 d . . .
H15 H 0.1558 0.8829 0.5168 0.041 Uiso 1 1 calc R . .
C25 C 0.2009(4) 0.8886(3) 0.3220(6) 0.0260(14) Uani 1 1 d . . .
H16 H 0.1452 0.8997 0.2745 0.031 Uiso 1 1 calc R . .
C26 C 0.3663(3) 0.8758(2) -0.0171(6) 0.0204(12) Uani 1 1 d . . .
C27 C 0.3698(4) 0.8165(3) -0.0804(6) 0.0317(15) Uani 1 1 d . . .
H23 H 0.3201 0.7889 -0.0818 0.038 Uiso 1 1 calc R . .
C28 C 0.4469(4) 0.7978(3) -0.1418(7) 0.0400(17) Uani 1 1 d . . .
H22 H 0.4487 0.758 -0.1882 0.048 Uiso 1 1 calc R . .
C29 C 0.5198(4) 0.8364(3) -0.1356(7) 0.0348(15) Uani 1 1 d . . .
H21 H 0.5721 0.8233 -0.1775 0.042 Uiso 1 1 calc R . .
C30 C 0.5172(4) 0.8944(3) -0.0680(7) 0.0359(16) Uani 1 1 d . . .
H20 H 0.5685 0.9206 -0.0604 0.043 Uiso 1 1 calc R . .
C31 C 0.4401(3) 0.9144(3) -0.0116(6) 0.0276(14) Uani 1 1 d . . .
H19 H 0.4379 0.955 0.0312 0.033 Uiso 1 1 calc R . .
C32 C 0.1759(3) 0.8598(2) -0.0285(6) 0.0227(13) Uani 1 1 d . . .
C33 C 0.1467(3) 0.8021(2) 0.0232(6) 0.0287(14) Uani 1 1 d . . .
H28 H 0.1753 0.7845 0.1078 0.034 Uiso 1 1 calc R . .
C34 C 0.0764(3) 0.7706(3) -0.0479(7) 0.0320(15) Uani 1 1 d . . .
H27 H 0.0563 0.7315 -0.0123 0.038 Uiso 1 1 calc R . .
C35 C 0.0351(4) 0.7965(3) -0.1726(7) 0.0318(15) Uani 1 1 d . . .
H26 H -0.0132 0.7749 -0.2219 0.038 Uiso 1 1 calc R . .
C36 C 0.0631(3) 0.8522(3) -0.2243(6) 0.0296(14) Uani 1 1 d . . .
H25 H 0.0344 0.8694 -0.3093 0.036 Uiso 1 1 calc R . .
C37 C 0.1344(3) 0.8844(3) -0.1527(6) 0.0261(13) Uani 1 1 d . . .
H24 H 0.1543 0.9233 -0.1896 0.031 Uiso 1 1 calc R . .
N1 N 0.2472(3) 1.1065(2) 0.0336(5) 0.0233(11) Uani 1 1 d . . .
N2 N 0.2159(3) 1.1316(2) 0.1574(5) 0.0256(11) Uani 1 1 d . . .
O1 O 0.2981(2) 1.00763(17) -0.1586(4) 0.0293(9) Uani 1 1 d . . .
O2 O 0.4166(3) 1.0823(2) -0.5752(5) 0.0388(11) Uani 1 1 d . . .
O3 O 0.1994(2) 1.02598(16) 0.2171(4) 0.0296(10) Uani 1 1 d . . .
O4 O 0.1938(3) 1.21504(18) 0.3528(5) 0.0315(10) Uani 1 1 d . . .
H4O H 0.213(4) 1.197(3) 0.264(7) 0.047 Uiso 1 1 d . . .
P1 P 0.26693(9) 0.90506(6) 0.05690(16) 0.0215(4) Uani 1 1 d . . .
Pd1 Pd 0.25186(3) 1.01225(2) 0.03149(5) 0.02417(15) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.277(7) . ?
C1 C2 1.430(8) . ?
C1 H7 0.95 . ?
C2 C3 1.421(8) . ?
C2 C8 1.422(8) . ?
C3 O1 1.311(6) . ?
C3 C4 1.392(8) . ?
C4 C5 1.389(8) . ?
C4 H6 0.95 . ?
C5 O2 1.354(7) . ?
C5 C7 1.400(8) . ?
C6 O2 1.451(7) . ?
C6 H1 0.98 . ?
C6 H2 0.98 . ?
C6 H3 0.98 . ?
C7 C8 1.353(8) . ?
C7 H5 0.95 . ?
C8 H4 0.95 . ?
C9 O3 1.293(6) . ?
C9 N2 1.316(7) . ?
C9 C10 1.481(8) . ?
C10 C11 1.373(8) . ?
C10 C19 1.429(7) . ?
C11 C12 1.405(8) . ?
C11 H8 0.95 . ?
C12 C13 1.406(8) . ?
C12 C17 1.414(7) . ?
C13 C14 1.377(8) . ?
C13 H13 0.95 . ?
C14 C15 1.408(8) . ?
C14 H12 0.95 . ?
C15 C16 1.346(8) . ?
C15 H11 0.95 . ?
C16 C17 1.417(8) . ?
C16 H10 0.95 . ?
C17 C18 1.418(8) . ?
C18 C19 1.344(8) . ?
C18 H9 0.95 . ?
C19 O4 1.356(7) . ?
C20 C21 1.393(7) . ?
C20 C25 1.397(8) . ?
C20 P1 1.812(6) . ?
C21 C22 1.380(8) . ?
C21 H18 0.95 . ?
C22 C23 1.369(9) . ?
C22 H17 0.95 . ?
C23 C24 1.392(8) . ?
C23 H14 0.95 . ?
C24 C25 1.356(8) . ?
C24 H15 0.95 . ?
C25 H16 0.95 . ?
C26 C31 1.378(7) . ?
C26 C27 1.390(7) . ?
C26 P1 1.810(5) . ?
C27 C28 1.395(8) . ?
C27 H23 0.95 . ?
C28 C29 1.367(8) . ?
C28 H22 0.95 . ?
C29 C30 1.384(8) . ?
C29 H21 0.95 . ?
C30 C31 1.382(8) . ?
C30 H20 0.95 . ?
C31 H19 0.95 . ?
C32 C37 1.381(7) . ?
C32 C33 1.397(7) . ?
C32 P1 1.809(5) . ?
C33 C34 1.379(7) . ?
C33 H28 0.95 . ?
C34 C35 1.394(8) . ?
C34 H27 0.95 . ?
C35 C36 1.353(8) . ?
C35 H26 0.95 . ?
C36 C37 1.400(7) . ?
C36 H25 0.95 . ?
C37 H24 0.95 . ?
N1 N2 1.395(6) . ?
N1 Pd1 1.993(4) . ?
O1 Pd1 1.969(4) . ?
O3 Pd1 1.991(4) . ?
O4 H4O 0.98(6) . ?
P1 Pd1 2.2885(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 125.1(5) . . ?
N1 C1 H7 117.4 . . ?
C2 C1 H7 117.4 . . ?
C3 C2 C8 118.2(6) . . ?
C3 C2 C1 124.7(5) . . ?
C8 C2 C1 117.1(5) . . ?
O1 C3 C4 114.8(5) . . ?
O1 C3 C2 126.9(6) . . ?
C4 C3 C2 118.3(5) . . ?
C5 C4 C3 121.6(6) . . ?
C5 C4 H6 119.2 . . ?
C3 C4 H6 119.2 . . ?
O2 C5 C4 124.0(6) . . ?
O2 C5 C7 115.6(5) . . ?
C4 C5 C7 120.3(6) . . ?
O2 C6 H1 109.5 . . ?
O2 C6 H2 109.5 . . ?
H1 C6 H2 109.5 . . ?
O2 C6 H3 109.5 . . ?
H1 C6 H3 109.5 . . ?
H2 C6 H3 109.5 . . ?
C8 C7 C5 118.8(6) . . ?
C8 C7 H5 120.6 . . ?
C5 C7 H5 120.6 . . ?
C7 C8 C2 122.7(6) . . ?
C7 C8 H4 118.6 . . ?
C2 C8 H4 118.6 . . ?
O3 C9 N2 125.7(6) . . ?
O3 C9 C10 116.8(5) . . ?
N2 C9 C10 117.5(5) . . ?
C11 C10 C19 118.5(6) . . ?
C11 C10 C9 118.8(5) . . ?
C19 C10 C9 122.8(5) . . ?
C10 C11 C12 122.1(5) . . ?
C10 C11 H8 119 . . ?
C12 C11 H8 119 . . ?
C11 C12 C13 121.4(5) . . ?
C11 C12 C17 119.2(5) . . ?
C13 C12 C17 119.4(6) . . ?
C14 C13 C12 121.0(6) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.2(6) . . ?
C13 C14 H12 120.4 . . ?
C15 C14 H12 120.4 . . ?
C16 C15 C14 120.8(6) . . ?
C16 C15 H11 119.6 . . ?
C14 C15 H11 119.6 . . ?
C15 C16 C17 121.6(6) . . ?
C15 C16 H10 119.2 . . ?
C17 C16 H10 119.2 . . ?
C12 C17 C16 117.9(5) . . ?
C12 C17 C18 117.5(6) . . ?
C16 C17 C18 124.6(5) . . ?
C19 C18 C17 122.7(5) . . ?
C19 C18 H9 118.6 . . ?
C17 C18 H9 118.6 . . ?
C18 C19 O4 119.5(5) . . ?
C18 C19 C10 119.9(5) . . ?
O4 C19 C10 120.5(5) . . ?
C21 C20 C25 118.1(5) . . ?
C21 C20 P1 122.3(5) . . ?
C25 C20 P1 119.1(4) . . ?
C22 C21 C20 120.9(6) . . ?
C22 C21 H18 119.5 . . ?
C20 C21 H18 119.5 . . ?
C23 C22 C21 120.0(5) . . ?
C23 C22 H17 120 . . ?
C21 C22 H17 120 . . ?
C22 C23 C24 119.5(6) . . ?
C22 C23 H14 120.2 . . ?
C24 C23 H14 120.2 . . ?
C25 C24 C23 120.7(6) . . ?
C25 C24 H15 119.6 . . ?
C23 C24 H15 119.6 . . ?
C24 C25 C20 120.8(5) . . ?
C24 C25 H16 119.6 . . ?
C20 C25 H16 119.6 . . ?
C31 C26 C27 119.4(5) . . ?
C31 C26 P1 118.4(4) . . ?
C27 C26 P1 122.2(4) . . ?
C26 C27 C28 119.6(5) . . ?
C26 C27 H23 120.2 . . ?
C28 C27 H23 120.2 . . ?
C29 C28 C27 120.5(6) . . ?
C29 C28 H22 119.8 . . ?
C27 C28 H22 119.8 . . ?
C28 C29 C30 119.8(6) . . ?
C28 C29 H21 120.1 . . ?
C30 C29 H21 120.1 . . ?
C31 C30 C29 120.1(5) . . ?
C31 C30 H20 120 . . ?
C29 C30 H20 120 . . ?
C26 C31 C30 120.5(5) . . ?
C26 C31 H19 119.7 . . ?
C30 C31 H19 119.7 . . ?
C37 C32 C33 119.2(5) . . ?
C37 C32 P1 116.9(4) . . ?
C33 C32 P1 123.9(4) . . ?
C34 C33 C32 120.4(5) . . ?
C34 C33 H28 119.8 . . ?
C32 C33 H28 119.8 . . ?
C33 C34 C35 119.4(5) . . ?
C33 C34 H27 120.3 . . ?
C35 C34 H27 120.3 . . ?
C36 C35 C34 120.8(5) . . ?
C36 C35 H26 119.6 . . ?
C34 C35 H26 119.6 . . ?
C35 C36 C37 120.1(5) . . ?
C35 C36 H25 119.9 . . ?
C37 C36 H25 119.9 . . ?
C32 C37 C36 120.1(5) . . ?
C32 C37 H24 120 . . ?
C36 C37 H24 120 . . ?
C1 N1 N2 120.5(5) . . ?
C1 N1 Pd1 125.3(4) . . ?
N2 N1 Pd1 113.8(3) . . ?
C9 N2 N1 110.2(5) . . ?
C3 O1 Pd1 123.3(4) . . ?
C5 O2 C6 116.3(5) . . ?
C9 O3 Pd1 110.0(4) . . ?
C19 O4 H4O 109(4) . . ?
C32 P1 C26 105.8(2) . . ?
C32 P1 C20 106.4(3) . . ?
C26 P1 C20 106.5(2) . . ?
C32 P1 Pd1 114.35(17) . . ?
C26 P1 Pd1 112.15(18) . . ?
C20 P1 Pd1 111.17(17) . . ?
O1 Pd1 O3 173.74(15) . . ?
O1 Pd1 N1 94.23(19) . . ?
O3 Pd1 N1 80.15(18) . . ?
O1 Pd1 P1 90.35(11) . . ?
O3 Pd1 P1 95.53(11) . . ?
N1 Pd1 P1 172.74(13) . . ?



# END of CIF
