# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_AniMeCl
_database_code_depnum_ccdc_archive 'CCDC 1408864'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H39 Cl O3 P2 Pd'
_chemical_formula_sum            'C29 H39 Cl O3 P2 Pd'
_chemical_formula_weight         639.39

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.278(2)
_cell_length_b                   15.524(4)
_cell_length_c                   18.474(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2947.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    11420
_cell_measurement_theta_min      1.7135
_cell_measurement_theta_max      30.8953

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.857
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8790
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'RIGAKU/MSC Mercury CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            20838
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5787
_reflns_number_gt                5651
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXLT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²+3.8349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2426 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.114(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5787
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.01153(4) 0.89820(2) 0.27685(2) 0.01929(13) Uani 1 1 d . . . . .
C1 C -0.1580(5) 0.9690(3) 0.2621(3) 0.0203(11) Uani 1 1 d . . . . .
H1 H -0.2181 0.9366 0.2312 0.030 Uiso 1 1 calc R U . . .
H2 H -0.1370 1.0241 0.2390 0.030 Uiso 1 1 calc R U . . .
H3 H -0.1990 0.9797 0.3091 0.030 Uiso 1 1 calc R U . . .
Cl1 Cl -0.03467(11) 0.88081(7) 0.40437(6) 0.0136(2) Uani 1 1 d . . . . .
P1 P 0.05989(13) 0.90237(9) 0.15957(7) 0.0187(3) Uani 1 1 d . . . . .
C2 C 0.2340(5) 0.9273(3) 0.1420(3) 0.0195(11) Uani 1 1 d . . . . .
C3 C 0.2621(6) 0.9784(4) 0.0811(3) 0.0239(12) Uani 1 1 d . . . . .
H4 H 0.1927 0.9959 0.0504 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3867(6) 1.0039(4) 0.0645(3) 0.0278(13) Uani 1 1 d . . . . .
H5 H 0.4028 1.0391 0.0234 0.033 Uiso 1 1 calc R U . . .
C5 C 0.4885(6) 0.9777(4) 0.1084(3) 0.0304(13) Uani 1 1 d . . . . .
H6 H 0.5750 0.9950 0.0975 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4646(6) 0.9260(4) 0.1684(3) 0.0268(12) Uani 1 1 d . . . . .
H7 H 0.5354 0.9071 0.1974 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3373(5) 0.9011(4) 0.1869(3) 0.0209(11) Uani 1 1 d . . . . .
P2 P 0.31929(13) 0.83307(9) 0.26665(8) 0.0203(3) Uani 1 1 d . . . . .
O1 O 0.1792(4) 0.8127(2) 0.2816(2) 0.0219(8) Uani 1 1 d . . . . .
C8 C 0.0359(5) 0.7947(3) 0.1231(3) 0.0206(11) Uani 1 1 d . . . . .
C9 C 0.0805(6) 0.7673(4) 0.0545(3) 0.0248(12) Uani 1 1 d . . . . .
C10 C 0.0744(7) 0.6810(4) 0.0353(4) 0.0297(13) Uani 1 1 d . . . . .
H8 H 0.1046 0.6628 -0.0108 0.036 Uiso 1 1 calc R U . . .
C11 C 0.0235(6) 0.6207(4) 0.0842(3) 0.0290(13) Uani 1 1 d . . . . .
H9 H 0.0215 0.5615 0.0714 0.035 Uiso 1 1 calc R U . . .
C12 C -0.0228(6) 0.6458(4) 0.1493(3) 0.0290(13) Uani 1 1 d . . . . .
H10 H -0.0584 0.6045 0.1817 0.035 Uiso 1 1 calc R U . . .
C13 C -0.0181(6) 0.7325(4) 0.1686(3) 0.0260(12) Uani 1 1 d . . . . .
H11 H -0.0526 0.7497 0.2141 0.031 Uiso 1 1 calc R U . . .
O2 O 0.1289(4) 0.8298(3) 0.0109(2) 0.0275(9) Uani 1 1 d . . . . .
C14 C 0.2039(8) 0.8043(5) -0.0489(4) 0.0414(17) Uani 1 1 d . . . . .
H12 H 0.2781 0.7700 -0.0323 0.062 Uiso 1 1 calc R U . . .
H13 H 0.2355 0.8555 -0.0745 0.062 Uiso 1 1 calc R U . . .
H14 H 0.1503 0.7697 -0.0818 0.062 Uiso 1 1 calc R U . . .
C15 C -0.0299(5) 0.9749(4) 0.1012(3) 0.0220(11) Uani 1 1 d . . . . .
C16 C -0.0169(6) 1.0652(4) 0.1117(3) 0.0251(12) Uani 1 1 d . . . . .
C17 C -0.0908(6) 1.1229(4) 0.0728(3) 0.0308(14) Uani 1 1 d . . . . .
H15 H -0.0805 1.1831 0.0801 0.037 Uiso 1 1 calc R U . . .
C18 C -0.1810(6) 1.0922(5) 0.0226(3) 0.0332(14) Uani 1 1 d . . . . .
H16 H -0.2323 1.1317 -0.0044 0.040 Uiso 1 1 calc R U . . .
C19 C -0.1959(6) 1.0037(5) 0.0119(3) 0.0313(14) Uani 1 1 d . . . . .
H17 H -0.2570 0.9831 -0.0226 0.038 Uiso 1 1 calc R U . . .
C20 C -0.1217(6) 0.9460(4) 0.0515(3) 0.0279(13) Uani 1 1 d . . . . .
H18 H -0.1336 0.8858 0.0447 0.033 Uiso 1 1 calc R U . . .
O3 O 0.0733(4) 1.0884(3) 0.1621(2) 0.0292(9) Uani 1 1 d . . . . .
C21 C 0.1272(9) 1.1725(5) 0.1546(4) 0.0451(19) Uani 1 1 d . . . . .
H19 H 0.1749 1.1764 0.1088 0.068 Uiso 1 1 calc R U . . .
H20 H 0.1868 1.1838 0.1950 0.068 Uiso 1 1 calc R U . . .
H21 H 0.0571 1.2153 0.1550 0.068 Uiso 1 1 calc R U . . .
C22 C 0.4004(6) 0.7291(4) 0.2457(4) 0.0290(14) Uani 1 1 d . . . . .
C23 C 0.3561(8) 0.7023(5) 0.1704(4) 0.0426(17) Uani 1 1 d . . . . .
H22 H 0.3713 0.7496 0.1363 0.064 Uiso 1 1 calc R U . . .
H23 H 0.2630 0.6885 0.1715 0.064 Uiso 1 1 calc R U . . .
H24 H 0.4052 0.6514 0.1548 0.064 Uiso 1 1 calc R U . . .
C24 C 0.3511(10) 0.6619(5) 0.2996(5) 0.056(2) Uani 1 1 d . . . . .
H25 H 0.3876 0.6054 0.2875 0.084 Uiso 1 1 calc R U . . .
H26 H 0.2559 0.6591 0.2974 0.084 Uiso 1 1 calc R U . . .
H27 H 0.3781 0.6781 0.3487 0.084 Uiso 1 1 calc R U . . .
C25 C 0.5489(7) 0.7299(5) 0.2499(6) 0.058(3) Uani 1 1 d . . . . .
H28 H 0.5827 0.6732 0.2362 0.088 Uiso 1 1 calc R U . . .
H29 H 0.5760 0.7433 0.2995 0.088 Uiso 1 1 calc R U . . .
H30 H 0.5833 0.7737 0.2168 0.088 Uiso 1 1 calc R U . . .
C26 C 0.3862(6) 0.8927(4) 0.3458(3) 0.0299(13) Uani 1 1 d . . . . .
C27 C 0.3063(8) 0.9767(5) 0.3510(4) 0.0451(19) Uani 1 1 d . . . . .
H31 H 0.2134 0.9627 0.3534 0.068 Uiso 1 1 calc R U . . .
H32 H 0.3232 1.0124 0.3083 0.068 Uiso 1 1 calc R U . . .
H33 H 0.3316 1.0083 0.3948 0.068 Uiso 1 1 calc R U . . .
C28 C 0.5296(7) 0.9192(6) 0.3425(4) 0.053(2) Uani 1 1 d . . . . .
H34 H 0.5540 0.9477 0.3878 0.079 Uiso 1 1 calc R U . . .
H35 H 0.5427 0.9590 0.3019 0.079 Uiso 1 1 calc R U . . .
H36 H 0.5837 0.8679 0.3355 0.079 Uiso 1 1 calc R U . . .
C29 C 0.3584(9) 0.8411(5) 0.4128(4) 0.050(2) Uani 1 1 d . . . . .
H37 H 0.3678 0.8779 0.4555 0.075 Uiso 1 1 calc R U . . .
H38 H 0.4198 0.7929 0.4159 0.075 Uiso 1 1 calc R U . . .
H39 H 0.2693 0.8187 0.4106 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.079(5) . ?
Pd1 O1 2.177(4) . ?
Pd1 P1 2.2239(15) . ?
Pd1 Cl1 2.4182(12) . ?
C1 H1 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
P1 C15 1.812(6) . ?
P1 C8 1.819(6) . ?
P1 C2 1.859(6) . ?
C2 C3 1.407(8) . ?
C2 C7 1.408(8) . ?
C3 C4 1.375(9) . ?
C3 H4 0.9500 . ?
C4 C5 1.386(9) . ?
C4 H5 0.9500 . ?
C5 C6 1.390(9) . ?
C5 H6 0.9500 . ?
C6 C7 1.406(8) . ?
C6 H7 0.9500 . ?
C7 P2 1.822(6) . ?
P2 O1 1.500(4) . ?
P2 C22 1.858(6) . ?
P2 C26 1.862(6) . ?
C8 C13 1.396(8) . ?
C8 C9 1.414(8) . ?
C9 O2 1.355(7) . ?
C9 C10 1.387(8) . ?
C10 C11 1.402(9) . ?
C10 H8 0.9500 . ?
C11 C12 1.350(8) . ?
C11 H9 0.9500 . ?
C12 C13 1.394(8) . ?
C12 H10 0.9500 . ?
C13 H11 0.9500 . ?
O2 C14 1.405(8) . ?
C14 H12 0.9800 . ?
C14 H13 0.9800 . ?
C14 H14 0.9800 . ?
C15 C20 1.391(8) . ?
C15 C16 1.420(8) . ?
C16 O3 1.362(7) . ?
C16 C17 1.377(9) . ?
C17 C18 1.395(10) . ?
C17 H15 0.9500 . ?
C18 C19 1.397(10) . ?
C18 H16 0.9500 . ?
C19 C20 1.387(9) . ?
C19 H17 0.9500 . ?
C20 H18 0.9500 . ?
O3 C21 1.425(8) . ?
C21 H19 0.9800 . ?
C21 H20 0.9800 . ?
C21 H21 0.9800 . ?
C22 C23 1.522(9) . ?
C22 C25 1.528(10) . ?
C22 C24 1.529(10) . ?
C23 H22 0.9800 . ?
C23 H23 0.9800 . ?
C23 H24 0.9800 . ?
C24 H25 0.9800 . ?
C24 H26 0.9800 . ?
C24 H27 0.9800 . ?
C25 H28 0.9800 . ?
C25 H29 0.9800 . ?
C25 H30 0.9800 . ?
C26 C29 1.501(10) . ?
C26 C28 1.532(9) . ?
C26 C27 1.545(9) . ?
C27 H31 0.9800 . ?
C27 H32 0.9800 . ?
C27 H33 0.9800 . ?
C28 H34 0.9800 . ?
C28 H35 0.9800 . ?
C28 H36 0.9800 . ?
C29 H37 0.9800 . ?
C29 H38 0.9800 . ?
C29 H39 0.9800 . ?

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
C1 Pd1 O1 172.52(19) . . ?
C1 Pd1 P1 92.53(15) . . ?
O1 Pd1 P1 83.11(11) . . ?
C1 Pd1 Cl1 91.28(15) . . ?
O1 Pd1 Cl1 92.76(11) . . ?
P1 Pd1 Cl1 175.02(5) . . ?
Pd1 C1 H1 109.5 . . ?
Pd1 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
Pd1 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
C15 P1 C8 106.4(3) . . ?
C15 P1 C2 104.9(3) . . ?
C8 P1 C2 104.9(2) . . ?
C15 P1 Pd1 118.93(18) . . ?
C8 P1 Pd1 107.69(18) . . ?
C2 P1 Pd1 113.04(18) . . ?
C3 C2 C7 118.7(5) . . ?
C3 C2 P1 117.1(4) . . ?
C7 C2 P1 124.3(4) . . ?
C4 C3 C2 122.1(6) . . ?
C4 C3 H4 118.9 . . ?
C2 C3 H4 118.9 . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 H5 120.4 . . ?
C5 C4 H5 120.4 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H6 119.9 . . ?
C6 C5 H6 119.9 . . ?
C5 C6 C7 121.1(6) . . ?
C5 C6 H7 119.4 . . ?
C7 C6 H7 119.4 . . ?
C6 C7 C2 118.7(5) . . ?
C6 C7 P2 116.7(4) . . ?
C2 C7 P2 124.6(4) . . ?
O1 P2 C7 111.6(2) . . ?
O1 P2 C22 106.6(3) . . ?
C7 P2 C22 106.8(3) . . ?
O1 P2 C26 108.3(3) . . ?
C7 P2 C26 108.1(3) . . ?
C22 P2 C26 115.4(3) . . ?
P2 O1 Pd1 128.6(2) . . ?
C13 C8 C9 117.4(5) . . ?
C13 C8 P1 117.8(4) . . ?
C9 C8 P1 124.4(4) . . ?
O2 C9 C10 123.8(6) . . ?
O2 C9 C8 115.8(5) . . ?
C10 C9 C8 120.4(6) . . ?
C9 C10 C11 119.7(6) . . ?
C9 C10 H8 120.1 . . ?
C11 C10 H8 120.1 . . ?
C12 C11 C10 120.9(5) . . ?
C12 C11 H9 119.5 . . ?
C10 C11 H9 119.5 . . ?
C11 C12 C13 119.6(6) . . ?
C11 C12 H10 120.2 . . ?
C13 C12 H10 120.2 . . ?
C12 C13 C8 121.9(6) . . ?
C12 C13 H11 119.1 . . ?
C8 C13 H11 119.1 . . ?
C9 O2 C14 117.8(5) . . ?
O2 C14 H12 109.5 . . ?
O2 C14 H13 109.5 . . ?
H12 C14 H13 109.5 . . ?
O2 C14 H14 109.5 . . ?
H12 C14 H14 109.5 . . ?
H13 C14 H14 109.5 . . ?
C20 C15 C16 118.2(5) . . ?
C20 C15 P1 122.5(5) . . ?
C16 C15 P1 118.9(4) . . ?
O3 C16 C17 124.0(5) . . ?
O3 C16 C15 114.8(5) . . ?
C17 C16 C15 121.2(6) . . ?
C16 C17 C18 119.4(6) . . ?
C16 C17 H15 120.3 . . ?
C18 C17 H15 120.3 . . ?
C17 C18 C19 120.2(6) . . ?
C17 C18 H16 119.9 . . ?
C19 C18 H16 119.9 . . ?
C20 C19 C18 120.0(6) . . ?
C20 C19 H17 120.0 . . ?
C18 C19 H17 120.0 . . ?
C19 C20 C15 120.8(6) . . ?
C19 C20 H18 119.6 . . ?
C15 C20 H18 119.6 . . ?
C16 O3 C21 116.2(5) . . ?
O3 C21 H19 109.5 . . ?
O3 C21 H20 109.5 . . ?
H19 C21 H20 109.5 . . ?
O3 C21 H21 109.5 . . ?
H19 C21 H21 109.5 . . ?
H20 C21 H21 109.5 . . ?
C23 C22 C25 110.4(6) . . ?
C23 C22 C24 108.1(6) . . ?
C25 C22 C24 107.7(7) . . ?
C23 C22 P2 107.1(4) . . ?
C25 C22 P2 115.5(5) . . ?
C24 C22 P2 107.9(5) . . ?
C22 C23 H22 109.5 . . ?
C22 C23 H23 109.5 . . ?
H22 C23 H23 109.5 . . ?
C22 C23 H24 109.5 . . ?
H22 C23 H24 109.5 . . ?
H23 C23 H24 109.5 . . ?
C22 C24 H25 109.5 . . ?
C22 C24 H26 109.5 . . ?
H25 C24 H26 109.5 . . ?
C22 C24 H27 109.5 . . ?
H25 C24 H27 109.5 . . ?
H26 C24 H27 109.5 . . ?
C22 C25 H28 109.5 . . ?
C22 C25 H29 109.5 . . ?
H28 C25 H29 109.5 . . ?
C22 C25 H30 109.5 . . ?
H28 C25 H30 109.5 . . ?
H29 C25 H30 109.5 . . ?
C29 C26 C28 111.1(6) . . ?
C29 C26 C27 107.3(6) . . ?
C28 C26 C27 106.7(6) . . ?
C29 C26 P2 108.2(5) . . ?
C28 C26 P2 117.2(5) . . ?
C27 C26 P2 105.8(4) . . ?
C26 C27 H31 109.5 . . ?
C26 C27 H32 109.5 . . ?
H31 C27 H32 109.5 . . ?
C26 C27 H33 109.5 . . ?
H31 C27 H33 109.5 . . ?
H32 C27 H33 109.5 . . ?
C26 C28 H34 109.5 . . ?
C26 C28 H35 109.5 . . ?
H34 C28 H35 109.5 . . ?
C26 C28 H36 109.5 . . ?
H34 C28 H36 109.5 . . ?
H35 C28 H36 109.5 . . ?
C26 C29 H37 109.5 . . ?
C26 C29 H38 109.5 . . ?
H37 C29 H38 109.5 . . ?
C26 C29 H39 109.5 . . ?
H37 C29 H39 109.5 . . ?
H38 C29 H39 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 P1 C2 C3 -13.0(5) . . . . ?
C8 P1 C2 C3 98.9(4) . . . . ?
Pd1 P1 C2 C3 -144.1(4) . . . . ?
C15 P1 C2 C7 164.6(5) . . . . ?
C8 P1 C2 C7 -83.5(5) . . . . ?
Pd1 P1 C2 C7 33.5(5) . . . . ?
C7 C2 C3 C4 -0.5(8) . . . . ?
P1 C2 C3 C4 177.2(5) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C3 C4 C5 C6 0.2(9) . . . . ?
C4 C5 C6 C7 -1.6(9) . . . . ?
C5 C6 C7 C2 2.0(9) . . . . ?
C5 C6 C7 P2 179.9(5) . . . . ?
C3 C2 C7 C6 -0.9(8) . . . . ?
P1 C2 C7 C6 -178.5(4) . . . . ?
C3 C2 C7 P2 -178.6(4) . . . . ?
P1 C2 C7 P2 3.8(7) . . . . ?
C6 C7 P2 O1 178.7(4) . . . . ?
C2 C7 P2 O1 -3.6(6) . . . . ?
C6 C7 P2 C22 -65.1(5) . . . . ?
C2 C7 P2 C22 112.6(5) . . . . ?
C6 C7 P2 C26 59.7(5) . . . . ?
C2 C7 P2 C26 -122.6(5) . . . . ?
C7 P2 O1 Pd1 -42.5(4) . . . . ?
C22 P2 O1 Pd1 -158.8(3) . . . . ?
C26 P2 O1 Pd1 76.3(4) . . . . ?
C15 P1 C8 C13 -122.4(5) . . . . ?
C2 P1 C8 C13 126.8(5) . . . . ?
Pd1 P1 C8 C13 6.1(5) . . . . ?
C15 P1 C8 C9 64.6(5) . . . . ?
C2 P1 C8 C9 -46.2(5) . . . . ?
Pd1 P1 C8 C9 -166.9(4) . . . . ?
C13 C8 C9 O2 178.2(5) . . . . ?
P1 C8 C9 O2 -8.8(8) . . . . ?
C13 C8 C9 C10 -2.3(9) . . . . ?
P1 C8 C9 C10 170.7(5) . . . . ?
O2 C9 C10 C11 179.6(6) . . . . ?
C8 C9 C10 C11 0.1(9) . . . . ?
C9 C10 C11 C12 1.7(10) . . . . ?
C10 C11 C12 C13 -1.0(10) . . . . ?
C11 C12 C13 C8 -1.4(10) . . . . ?
C9 C8 C13 C12 3.0(9) . . . . ?
P1 C8 C13 C12 -170.5(5) . . . . ?
C10 C9 O2 C14 -15.5(9) . . . . ?
C8 C9 O2 C14 164.0(6) . . . . ?
C8 P1 C15 C20 14.1(5) . . . . ?
C2 P1 C15 C20 124.9(5) . . . . ?
Pd1 P1 C15 C20 -107.5(5) . . . . ?
C8 P1 C15 C16 -172.8(4) . . . . ?
C2 P1 C15 C16 -62.0(5) . . . . ?
Pd1 P1 C15 C16 65.6(5) . . . . ?
C20 C15 C16 O3 178.9(5) . . . . ?
P1 C15 C16 O3 5.5(7) . . . . ?
C20 C15 C16 C17 -1.3(8) . . . . ?
P1 C15 C16 C17 -174.7(5) . . . . ?
O3 C16 C17 C18 -179.7(5) . . . . ?
C15 C16 C17 C18 0.5(9) . . . . ?
C16 C17 C18 C19 0.0(9) . . . . ?
C17 C18 C19 C20 0.4(9) . . . . ?
C18 C19 C20 C15 -1.3(9) . . . . ?
C16 C15 C20 C19 1.7(9) . . . . ?
P1 C15 C20 C19 174.8(5) . . . . ?
C17 C16 O3 C21 -24.2(8) . . . . ?
C15 C16 O3 C21 155.7(6) . . . . ?
O1 P2 C22 C23 73.4(5) . . . . ?
C7 P2 C22 C23 -46.0(5) . . . . ?
C26 P2 C22 C23 -166.2(5) . . . . ?
O1 P2 C22 C25 -163.2(6) . . . . ?
C7 P2 C22 C25 77.4(6) . . . . ?
C26 P2 C22 C25 -42.8(7) . . . . ?
O1 P2 C22 C24 -42.7(6) . . . . ?
C7 P2 C22 C24 -162.2(5) . . . . ?
C26 P2 C22 C24 77.7(6) . . . . ?
O1 P2 C26 C29 52.8(6) . . . . ?
C7 P2 C26 C29 173.9(5) . . . . ?
C22 P2 C26 C29 -66.6(6) . . . . ?
O1 P2 C26 C28 179.3(6) . . . . ?
C7 P2 C26 C28 -59.6(6) . . . . ?
C22 P2 C26 C28 59.9(7) . . . . ?
O1 P2 C26 C27 -62.0(5) . . . . ?
C7 P2 C26 C27 59.1(5) . . . . ?
C22 P2 C26 C27 178.6(5) . . . . ?

_refine_diff_density_max         1.827
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.102

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_iPMA12
_database_code_depnum_ccdc_archive 'CCDC 1408865'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H45 O3 P2 Pd, F6 P'
_chemical_formula_sum            'C25 H45 F6 O3 P3 Pd'
_chemical_formula_weight         706.92

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.338(4)
_cell_length_b                   13.576(6)
_cell_length_c                   14.319(7)
_cell_angle_alpha                81.992(15)
_cell_angle_beta                 83.829(16)
_cell_angle_gamma                75.466(16)
_cell_volume                     1549.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    93
_cell_measurement_reflns_used    5660
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      31.6

_exptl_crystal_description       Chip
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.815
_shelx_estimated_absorpt_T_min   0.953
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            22424
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.636
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             5971
_reflns_number_gt                5369
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+12.0662P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5971
_refine_ls_number_parameters     430
_refine_ls_number_restraints     342
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0879
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1410
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.214
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.49206(7) 0.37106(4) 0.23156(4) 0.01164(14) Uani 1 1 d . . . . .
P1 P 0.3850(2) 0.32557(14) 0.37458(12) 0.0153(4) Uani 1 1 d . . . . .
P2 P 0.3440(2) 0.18377(14) 0.18514(13) 0.0185(4) Uani 1 1 d . . . . .
P3 P 0.0531(4) 0.7922(2) 0.24948(19) 0.0548(8) Uani 1 1 d . . . . .
O3 O 0.3558(6) 0.2943(4) 0.1643(3) 0.0225(12) Uani 1 1 d . . . . .
O1 O 0.6096(6) 0.4143(4) 0.0972(3) 0.0253(12) Uani 1 1 d . . . . .
O2 O 0.7939(7) 0.5046(4) 0.0348(3) 0.0326(14) Uani 1 1 d . . . . .
C14 C 0.2566(9) 0.5189(6) 0.4367(6) 0.0265(18) Uani 1 1 d . . . . .
H18 H 0.1589 0.5684 0.4605 0.040 Uiso 1 1 calc R U . . .
H19 H 0.3043 0.5496 0.3777 0.040 Uiso 1 1 calc R U . . .
H20 H 0.3394 0.4999 0.4838 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2939(9) 0.1501(5) 0.3107(5) 0.0199(16) Uani 1 1 d . . . . .
C10 C 0.2383(10) 0.0611(6) 0.3345(6) 0.0286(19) Uani 1 1 d . . . . .
H13 H 0.2387 0.0195 0.2863 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5408(9) 0.2988(5) 0.4645(5) 0.0207(16) Uani 1 1 d . . . . .
H21 H 0.5817 0.3627 0.4591 0.025 Uiso 1 1 calc R U . . .
C6 C 0.2988(9) 0.2113(5) 0.3840(5) 0.0196(16) Uani 1 1 d . . . . .
C12 C 0.2050(9) 0.4232(6) 0.4183(5) 0.0213(16) Uani 1 1 d . . . . .
H14 H 0.1569 0.3928 0.4792 0.026 Uiso 1 1 calc R U . . .
C24 C 0.6629(10) 0.1000(7) 0.2286(6) 0.034(2) Uani 1 1 d . U . . .
H40 H 0.7750 0.0595 0.2125 0.051 Uiso 1 1 calc R U . . .
H41 H 0.6204 0.0713 0.2902 0.051 Uiso 1 1 calc R U . . .
H42 H 0.6665 0.1711 0.2315 0.051 Uiso 1 1 calc R U . . .
C4 C 0.6895(10) 0.4770(6) 0.1029(5) 0.0251(17) Uani 1 1 d . . . . .
C5 C 0.8095(10) 0.4581(7) -0.0524(5) 0.0287(19) Uani 1 1 d . . . . .
H7 H 0.7112 0.4891 -0.0876 0.043 Uiso 1 1 calc R U . . .
H8 H 0.8188 0.3843 -0.0373 0.043 Uiso 1 1 calc R U . . .
H9 H 0.9091 0.4695 -0.0909 0.043 Uiso 1 1 calc R U . . .
C1 C 0.6338(10) 0.4538(6) 0.2756(5) 0.0256(18) Uani 1 1 d . . . . .
H1 H 0.5693 0.4957 0.3246 0.031 Uiso 1 1 calc R U . A 1
H2 H 0.7323 0.4071 0.3040 0.031 Uiso 1 1 calc R U . A 1
F6 F -0.0052(12) 0.8521(7) 0.1522(6) 0.057(2) Uani 0.727(6) 1 d . U P B 1
C20 C 0.0122(9) 0.2503(6) 0.1662(5) 0.0290(18) Uani 1 1 d . . . . .
H31 H -0.0086 0.2207 0.2315 0.044 Uiso 1 1 calc R U . . .
H32 H -0.0853 0.2571 0.1311 0.044 Uiso 1 1 calc R U . . .
H33 H 0.0338 0.3180 0.1663 0.044 Uiso 1 1 calc R U . . .
C18 C 0.1652(9) 0.1794(5) 0.1185(5) 0.0204(16) Uani 1 1 d . . . . .
C7 C 0.2352(9) 0.1799(6) 0.4752(5) 0.0240(17) Uani 1 1 d . . . . .
H10 H 0.2314 0.2208 0.5244 0.029 Uiso 1 1 calc R U . . .
C17 C 0.4826(10) 0.2797(6) 0.5691(5) 0.0317(19) Uani 1 1 d . . . . .
H25 H 0.5698 0.2833 0.6083 0.047 Uiso 1 1 calc R U . . .
H26 H 0.4592 0.2117 0.5822 0.047 Uiso 1 1 calc R U . . .
H27 H 0.3815 0.3320 0.5837 0.047 Uiso 1 1 calc R U . . .
C16 C 0.6933(10) 0.2159(6) 0.4368(6) 0.0298(19) Uani 1 1 d . . . . .
H22 H 0.6637 0.1497 0.4437 0.045 Uiso 1 1 calc R U . . .
H23 H 0.7818 0.2119 0.4780 0.045 Uiso 1 1 calc R U . . .
H24 H 0.7321 0.2331 0.3709 0.045 Uiso 1 1 calc R U . . .
C26 C 0.629(4) 0.544(3) 0.187(2) 0.017(5) Uani 0.327(16) 1 d . U P C 2
H46 H 0.5124 0.5863 0.1796 0.021 Uiso 0.327(16) 1 calc R U P C 2
C19 C 0.1962(10) 0.2304(6) 0.0169(5) 0.0294(19) Uani 1 1 d . . . . .
H28 H 0.0976 0.2393 -0.0179 0.044 Uiso 1 1 calc R U . . .
H29 H 0.2919 0.1867 -0.0153 0.044 Uiso 1 1 calc R U . . .
H30 H 0.2187 0.2974 0.0196 0.044 Uiso 1 1 calc R U . . .
C22 C 0.5473(10) 0.0969(7) 0.1522(6) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.1779(10) 0.0915(6) 0.4958(6) 0.033(2) Uani 1 1 d . . . . .
H11 H 0.1353 0.0726 0.5581 0.040 Uiso 1 1 calc R U . . .
C9 C 0.1830(11) 0.0307(7) 0.4249(6) 0.038(2) Uani 1 1 d . . . . .
H12 H 0.1483 -0.0316 0.4389 0.046 Uiso 1 1 calc R U . . .
C13 C 0.0721(9) 0.4501(6) 0.3464(5) 0.0279(18) Uani 1 1 d . . . . .
H15 H 0.1147 0.4838 0.2873 0.042 Uiso 1 1 calc R U . . .
H16 H -0.0279 0.4964 0.3721 0.042 Uiso 1 1 calc R U . . .
H17 H 0.0446 0.3873 0.3340 0.042 Uiso 1 1 calc R U . . .
C21 C 0.1286(11) 0.0756(6) 0.1125(7) 0.035(2) Uani 1 1 d . . . . .
H34 H 0.2270 0.0304 0.0840 0.053 Uiso 1 1 calc R U . . .
H35 H 0.0351 0.0853 0.0734 0.053 Uiso 1 1 calc R U . . .
H36 H 0.1005 0.0446 0.1761 0.053 Uiso 1 1 calc R U . . .
F4 F 0.0030(12) 0.9091(6) 0.2837(6) 0.059(2) Uani 0.727(6) 1 d . U P B 1
F3 F -0.1215(14) 0.7833(8) 0.2803(7) 0.081(2) Uani 0.727(6) 1 d . U P B 1
C23 C 0.6163(12) 0.1419(9) 0.0555(7) 0.055(3) Uani 1 1 d . U . . .
H37 H 0.5442 0.1397 0.0065 0.082 Uiso 1 1 calc R U . . .
H38 H 0.7288 0.1014 0.0403 0.082 Uiso 1 1 calc R U . . .
H39 H 0.6194 0.2130 0.0585 0.082 Uiso 1 1 calc R U . . .
F2 F 0.1079(15) 0.6859(7) 0.2145(7) 0.073(3) Uani 0.727(6) 1 d . U P B 1
F1 F 0.1042(14) 0.7509(7) 0.3538(6) 0.077(3) Uani 0.727(6) 1 d . U P B 1
F5 F 0.2379(10) 0.8134(8) 0.2233(8) 0.085(3) Uani 0.727(6) 1 d . . P B 1
C25 C 0.5438(12) -0.0127(7) 0.1495(8) 0.054(3) Uani 1 1 d . U . . .
H43 H 0.6539 -0.0512 0.1273 0.080 Uiso 1 1 calc R U . . .
H44 H 0.4620 -0.0155 0.1063 0.080 Uiso 1 1 calc R U . . .
H45 H 0.5132 -0.0428 0.2131 0.080 Uiso 1 1 calc R U . . .
C3 C 0.5542(15) 0.6246(9) 0.1795(8) 0.031(3) Uani 0.673(16) 1 d . U P C 1
H4 H 0.4456 0.6091 0.1794 0.046 Uiso 0.673(16) 1 calc R U P C 1
H5 H 0.5788 0.6639 0.1192 0.046 Uiso 0.673(16) 1 calc R U P C 1
H6 H 0.5525 0.6648 0.2314 0.046 Uiso 0.673(16) 1 calc R U P C 1
F7 F -0.007(3) 0.7202(17) 0.3553(16) 0.062(4) Uani 0.273(6) 1 d . U P B 2
F12 F 0.081(4) 0.818(2) 0.138(2) 0.069(4) Uani 0.273(6) 1 d . U P B 2
F11 F 0.206(4) 0.688(2) 0.2371(19) 0.075(4) Uani 0.273(6) 1 d . U P B 2
F9 F -0.152(4) 0.855(2) 0.2788(18) 0.077(4) Uani 0.273(6) 1 d . U P B 2
F8 F -0.069(3) 0.7107(17) 0.2165(16) 0.067(4) Uani 0.273(6) 1 d . U P B 2
F10 F 0.125(4) 0.851(2) 0.2944(17) 0.070(4) Uani 0.273(6) 1 d . U P B 2
C27 C 0.742(3) 0.6109(17) 0.1992(16) 0.023(6) Uani 0.327(16) 1 d . U P C 2
H47 H 0.7360 0.6655 0.1461 0.034 Uiso 0.327(16) 1 calc R U P C 2
H48 H 0.8567 0.5693 0.2011 0.034 Uiso 0.327(16) 1 calc R U P C 2
H49 H 0.7084 0.6414 0.2585 0.034 Uiso 0.327(16) 1 calc R U P C 2
C2 C 0.6896(18) 0.5234(12) 0.1926(11) 0.021(3) Uani 0.673(16) 1 d . U P C 1
H3 H 0.8005 0.5357 0.2004 0.025 Uiso 0.673(16) 1 calc R U P C 1


_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 C1 2.020(8) . ?
Pd1 O3 2.101(5) . ?
Pd1 O1 2.139(5) . ?
Pd1 P1 2.214(2) . ?
P1 C6 1.850(7) . ?
P1 C12 1.852(7) . ?
P1 C15 1.863(7) . ?
P2 O3 1.515(5) . ?
P2 C11 1.823(7) . ?
P2 C22 1.862(8) . ?
P2 C18 1.871(7) . ?
P3 F10 1.37(2) . ?
P3 F3 1.505(11) . ?
P3 F2 1.537(9) . ?
P3 F6 1.572(9) . ?
P3 F1 1.584(9) . ?
P3 F12 1.59(3) . ?
P3 F5 1.633(9) . ?
P3 F11 1.66(3) . ?
P3 F4 1.666(8) . ?
P3 F9 1.75(3) . ?
P3 F7 1.78(2) . ?
P3 F8 1.81(2) . ?
O1 C4 1.221(9) . ?
O2 C4 1.315(9) . ?
O2 C5 1.455(9) . ?
C14 C12 1.531(10) . ?
C14 H18 0.9800 . ?
C14 H19 0.9800 . ?
C14 H20 0.9800 . ?
C11 C10 1.386(10) . ?
C11 C6 1.436(10) . ?
C10 C9 1.370(11) . ?
C10 H13 0.9500 . ?
C15 C16 1.530(10) . ?
C15 C17 1.530(10) . ?
C15 H21 1.0000 . ?
C6 C7 1.406(10) . ?
C12 C13 1.535(10) . ?
C12 H14 1.0000 . ?
C24 C22 1.545(11) . ?
C24 H40 0.9800 . ?
C24 H41 0.9800 . ?
C24 H42 0.9800 . ?
C4 C2 1.507(17) . ?
C4 C26 1.57(3) . ?
C5 H7 0.9800 . ?
C5 H8 0.9800 . ?
C5 H9 0.9800 . ?
C1 C2 1.520(16) . ?
C1 C26 1.64(3) . ?
C1 H1 0.9900 . ?
C1 H2 0.9900 . ?
C20 C18 1.549(10) . ?
C20 H31 0.9800 . ?
C20 H32 0.9800 . ?
C20 H33 0.9800 . ?
C18 C21 1.530(10) . ?
C18 C19 1.546(10) . ?
C7 C8 1.383(10) . ?
C7 H10 0.9500 . ?
C17 H25 0.9800 . ?
C17 H26 0.9800 . ?
C17 H27 0.9800 . ?
C16 H22 0.9800 . ?
C16 H23 0.9800 . ?
C16 H24 0.9800 . ?
C26 C27 1.50(4) . ?
C26 H46 1.0000 . ?
C19 H28 0.9800 . ?
C19 H29 0.9800 . ?
C19 H30 0.9800 . ?
C22 C25 1.501(12) . ?
C22 C23 1.546(13) . ?
C8 C9 1.385(12) . ?
C8 H11 0.9500 . ?
C9 H12 0.9500 . ?
C13 H15 0.9800 . ?
C13 H16 0.9800 . ?
C13 H17 0.9800 . ?
C21 H34 0.9800 . ?
C21 H35 0.9800 . ?
C21 H36 0.9800 . ?
C23 H37 0.9800 . ?
C23 H38 0.9800 . ?
C23 H39 0.9800 . ?
C25 H43 0.9800 . ?
C25 H44 0.9800 . ?
C25 H45 0.9800 . ?
C3 C2 1.546(19) . ?
C3 H4 0.9800 . ?
C3 H5 0.9800 . ?
C3 H6 0.9800 . ?
C27 H47 0.9800 . ?
C27 H48 0.9800 . ?
C27 H49 0.9800 . ?
C2 H3 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 O3 171.0(2) . . ?
C1 Pd1 O1 81.6(2) . . ?
O3 Pd1 O1 89.5(2) . . ?
C1 Pd1 P1 95.5(2) . . ?
O3 Pd1 P1 93.41(14) . . ?
O1 Pd1 P1 176.45(16) . . ?
C6 P1 C12 102.3(3) . . ?
C6 P1 C15 106.9(3) . . ?
C12 P1 C15 106.3(3) . . ?
C6 P1 Pd1 114.7(2) . . ?
C12 P1 Pd1 114.1(2) . . ?
C15 P1 Pd1 111.8(2) . . ?
O3 P2 C11 111.3(3) . . ?
O3 P2 C22 109.9(4) . . ?
C11 P2 C22 107.2(4) . . ?
O3 P2 C18 103.7(3) . . ?
C11 P2 C18 108.6(3) . . ?
C22 P2 C18 116.0(3) . . ?
F3 P3 F2 94.5(6) . . ?
F3 P3 F6 90.5(6) . . ?
F2 P3 F6 95.9(5) . . ?
F3 P3 F1 89.4(6) . . ?
F2 P3 F1 94.1(5) . . ?
F6 P3 F1 170.0(5) . . ?
F10 P3 F12 109.6(16) . . ?
F3 P3 F5 173.2(6) . . ?
F2 P3 F5 92.2(6) . . ?
F6 P3 F5 90.5(6) . . ?
F1 P3 F5 88.5(6) . . ?
F10 P3 F11 102.5(17) . . ?
F12 P3 F11 85.8(14) . . ?
F3 P3 F4 88.6(5) . . ?
F2 P3 F4 176.7(6) . . ?
F6 P3 F4 83.0(5) . . ?
F1 P3 F4 87.0(5) . . ?
F5 P3 F4 84.8(5) . . ?
F10 P3 F9 96.4(16) . . ?
F12 P3 F9 105.4(14) . . ?
F11 P3 F9 153.3(15) . . ?
F10 P3 F7 94.9(13) . . ?
F12 P3 F7 155.1(14) . . ?
F11 P3 F7 84.6(12) . . ?
F9 P3 F7 75.2(12) . . ?
F10 P3 F8 166.7(14) . . ?
F12 P3 F8 83.1(13) . . ?
F11 P3 F8 81.8(13) . . ?
F9 P3 F8 75.8(13) . . ?
F7 P3 F8 72.8(11) . . ?
P2 O3 Pd1 128.3(3) . . ?
C4 O1 Pd1 111.4(5) . . ?
C4 O2 C5 116.7(6) . . ?
C12 C14 H18 109.5 . . ?
C12 C14 H19 109.5 . . ?
H18 C14 H19 109.5 . . ?
C12 C14 H20 109.5 . . ?
H18 C14 H20 109.5 . . ?
H19 C14 H20 109.5 . . ?
C10 C11 C6 118.9(7) . . ?
C10 C11 P2 116.0(6) . . ?
C6 C11 P2 125.0(5) . . ?
C9 C10 C11 122.5(8) . . ?
C9 C10 H13 118.7 . . ?
C11 C10 H13 118.7 . . ?
C16 C15 C17 111.6(6) . . ?
C16 C15 P1 110.6(5) . . ?
C17 C15 P1 118.8(5) . . ?
C16 C15 H21 104.8 . . ?
C17 C15 H21 104.8 . . ?
P1 C15 H21 104.8 . . ?
C7 C6 C11 116.9(7) . . ?
C7 C6 P1 115.1(5) . . ?
C11 C6 P1 128.0(5) . . ?
C14 C12 C13 111.1(6) . . ?
C14 C12 P1 111.6(5) . . ?
C13 C12 P1 109.1(5) . . ?
C14 C12 H14 108.3 . . ?
C13 C12 H14 108.3 . . ?
P1 C12 H14 108.3 . . ?
C22 C24 H40 109.5 . . ?
C22 C24 H41 109.5 . . ?
H40 C24 H41 109.5 . . ?
C22 C24 H42 109.5 . . ?
H40 C24 H42 109.5 . . ?
H41 C24 H42 109.5 . . ?
O1 C4 O2 123.8(7) . . ?
O1 C4 C2 122.9(8) . . ?
O2 C4 C2 113.1(8) . . ?
O1 C4 C26 115.2(13) . . ?
O2 C4 C26 119.4(13) . . ?
O2 C5 H7 109.5 . . ?
O2 C5 H8 109.5 . . ?
H7 C5 H8 109.5 . . ?
O2 C5 H9 109.5 . . ?
H7 C5 H9 109.5 . . ?
H8 C5 H9 109.5 . . ?
C2 C1 Pd1 110.0(7) . . ?
C26 C1 Pd1 100.9(12) . . ?
C2 C1 H1 109.7 . . ?
Pd1 C1 H1 109.7 . . ?
C2 C1 H2 109.7 . . ?
Pd1 C1 H2 109.7 . . ?
H1 C1 H2 108.2 . . ?
C18 C20 H31 109.5 . . ?
C18 C20 H32 109.5 . . ?
H31 C20 H32 109.5 . . ?
C18 C20 H33 109.5 . . ?
H31 C20 H33 109.5 . . ?
H32 C20 H33 109.5 . . ?
C21 C18 C19 108.5(6) . . ?
C21 C18 C20 109.9(6) . . ?
C19 C18 C20 107.7(6) . . ?
C21 C18 P2 118.9(5) . . ?
C19 C18 P2 106.6(5) . . ?
C20 C18 P2 104.8(5) . . ?
C8 C7 C6 122.4(7) . . ?
C8 C7 H10 118.8 . . ?
C6 C7 H10 118.8 . . ?
C15 C17 H25 109.5 . . ?
C15 C17 H26 109.5 . . ?
H25 C17 H26 109.5 . . ?
C15 C17 H27 109.5 . . ?
H25 C17 H27 109.5 . . ?
H26 C17 H27 109.5 . . ?
C15 C16 H22 109.5 . . ?
C15 C16 H23 109.5 . . ?
H22 C16 H23 109.5 . . ?
C15 C16 H24 109.5 . . ?
H22 C16 H24 109.5 . . ?
H23 C16 H24 109.5 . . ?
C27 C26 C4 114(2) . . ?
C27 C26 C1 111(2) . . ?
C4 C26 C1 99.8(19) . . ?
C27 C26 H46 110.8 . . ?
C4 C26 H46 110.8 . . ?
C1 C26 H46 110.8 . . ?
C18 C19 H28 109.5 . . ?
C18 C19 H29 109.5 . . ?
H28 C19 H29 109.5 . . ?
C18 C19 H30 109.5 . . ?
H28 C19 H30 109.5 . . ?
H29 C19 H30 109.5 . . ?
C25 C22 C24 108.3(8) . . ?
C25 C22 C23 110.3(8) . . ?
C24 C22 C23 108.9(7) . . ?
C25 C22 P2 115.4(6) . . ?
C24 C22 P2 105.5(5) . . ?
C23 C22 P2 108.3(6) . . ?
C7 C8 C9 119.6(8) . . ?
C7 C8 H11 120.2 . . ?
C9 C8 H11 120.2 . . ?
C10 C9 C8 119.6(8) . . ?
C10 C9 H12 120.2 . . ?
C8 C9 H12 120.2 . . ?
C12 C13 H15 109.5 . . ?
C12 C13 H16 109.5 . . ?
H15 C13 H16 109.5 . . ?
C12 C13 H17 109.5 . . ?
H15 C13 H17 109.5 . . ?
H16 C13 H17 109.5 . . ?
C18 C21 H34 109.5 . . ?
C18 C21 H35 109.5 . . ?
H34 C21 H35 109.5 . . ?
C18 C21 H36 109.5 . . ?
H34 C21 H36 109.5 . . ?
H35 C21 H36 109.5 . . ?
C22 C23 H37 109.5 . . ?
C22 C23 H38 109.5 . . ?
H37 C23 H38 109.5 . . ?
C22 C23 H39 109.5 . . ?
H37 C23 H39 109.5 . . ?
H38 C23 H39 109.5 . . ?
C22 C25 H43 109.5 . . ?
C22 C25 H44 109.5 . . ?
H43 C25 H44 109.5 . . ?
C22 C25 H45 109.5 . . ?
H43 C25 H45 109.5 . . ?
H44 C25 H45 109.5 . . ?
C2 C3 H4 109.5 . . ?
C2 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
C2 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?
C26 C27 H47 109.5 . . ?
C26 C27 H48 109.5 . . ?
H47 C27 H48 109.5 . . ?
C26 C27 H49 109.5 . . ?
H47 C27 H49 109.5 . . ?
H48 C27 H49 109.5 . . ?
C4 C2 C1 108.5(10) . . ?
C4 C2 C3 102.8(10) . . ?
C1 C2 C3 109.2(10) . . ?
C4 C2 H3 112.0 . . ?
C1 C2 H3 112.0 . . ?
C3 C2 H3 112.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 P2 O3 Pd1 50.5(5) . . . . ?
C22 P2 O3 Pd1 -68.2(5) . . . . ?
C18 P2 O3 Pd1 167.1(4) . . . . ?
O3 P2 C11 C10 164.0(6) . . . . ?
C22 P2 C11 C10 -75.7(6) . . . . ?
C18 P2 C11 C10 50.4(7) . . . . ?
O3 P2 C11 C6 -12.3(7) . . . . ?
C22 P2 C11 C6 108.0(7) . . . . ?
C18 P2 C11 C6 -125.9(6) . . . . ?
C6 C11 C10 C9 2.1(12) . . . . ?
P2 C11 C10 C9 -174.4(6) . . . . ?
C6 P1 C15 C16 69.4(6) . . . . ?
C12 P1 C15 C16 178.1(5) . . . . ?
Pd1 P1 C15 C16 -56.8(6) . . . . ?
C6 P1 C15 C17 -61.5(6) . . . . ?
C12 P1 C15 C17 47.2(7) . . . . ?
Pd1 P1 C15 C17 172.3(5) . . . . ?
C10 C11 C6 C7 -4.3(10) . . . . ?
P2 C11 C6 C7 171.8(5) . . . . ?
C10 C11 C6 P1 173.7(6) . . . . ?
P2 C11 C6 P1 -10.2(10) . . . . ?
C12 P1 C6 C7 -57.9(6) . . . . ?
C15 P1 C6 C7 53.6(6) . . . . ?
Pd1 P1 C6 C7 178.1(5) . . . . ?
C12 P1 C6 C11 124.1(7) . . . . ?
C15 P1 C6 C11 -124.4(7) . . . . ?
Pd1 P1 C6 C11 0.1(7) . . . . ?
C6 P1 C12 C14 168.0(5) . . . . ?
C15 P1 C12 C14 56.0(6) . . . . ?
Pd1 P1 C12 C14 -67.6(5) . . . . ?
C6 P1 C12 C13 -68.8(6) . . . . ?
C15 P1 C12 C13 179.2(5) . . . . ?
Pd1 P1 C12 C13 55.5(6) . . . . ?
Pd1 O1 C4 O2 169.1(6) . . . . ?
Pd1 O1 C4 C2 -5.1(11) . . . . ?
Pd1 O1 C4 C26 -25.7(14) . . . . ?
C5 O2 C4 O1 1.5(12) . . . . ?
C5 O2 C4 C2 176.2(8) . . . . ?
C5 O2 C4 C26 -163.1(14) . . . . ?
O3 P2 C18 C21 172.4(6) . . . . ?
C11 P2 C18 C21 -69.0(7) . . . . ?
C22 P2 C18 C21 51.7(8) . . . . ?
O3 P2 C18 C19 49.6(5) . . . . ?
C11 P2 C18 C19 168.1(5) . . . . ?
C22 P2 C18 C19 -71.1(6) . . . . ?
O3 P2 C18 C20 -64.4(5) . . . . ?
C11 P2 C18 C20 54.1(6) . . . . ?
C22 P2 C18 C20 174.9(5) . . . . ?
C11 C6 C7 C8 3.3(11) . . . . ?
P1 C6 C7 C8 -175.0(6) . . . . ?
O1 C4 C26 C27 172.5(17) . . . . ?
O2 C4 C26 C27 -22(3) . . . . ?
O1 C4 C26 C1 54.9(18) . . . . ?
O2 C4 C26 C1 -139.2(11) . . . . ?
Pd1 C1 C26 C27 -174.1(18) . . . . ?
Pd1 C1 C26 C4 -54.2(15) . . . . ?
O3 P2 C22 C25 -167.4(7) . . . . ?
C11 P2 C22 C25 71.4(8) . . . . ?
C18 P2 C22 C25 -50.2(8) . . . . ?
O3 P2 C22 C24 73.1(6) . . . . ?
C11 P2 C22 C24 -48.1(7) . . . . ?
C18 P2 C22 C24 -169.6(5) . . . . ?
O3 P2 C22 C23 -43.4(7) . . . . ?
C11 P2 C22 C23 -164.5(6) . . . . ?
C18 P2 C22 C23 73.9(7) . . . . ?
C6 C7 C8 C9 0.2(12) . . . . ?
C11 C10 C9 C8 1.5(13) . . . . ?
C7 C8 C9 C10 -2.7(13) . . . . ?
O1 C4 C2 C1 20.6(14) . . . . ?
O2 C4 C2 C1 -154.1(8) . . . . ?
O1 C4 C2 C3 -94.9(11) . . . . ?
O2 C4 C2 C3 90.3(11) . . . . ?
Pd1 C1 C2 C4 -25.1(11) . . . . ?
Pd1 C1 C2 C3 86.3(11) . . . . ?

_refine_diff_density_max         1.083
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.145

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_iPMA21Py
_database_code_depnum_ccdc_archive 'CCDC 1408866'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H49 N O3 P2 Pd, F6 P, C H2 Cl2'
_chemical_formula_sum            'C31 H51 Cl2 F6 N O3 P3 Pd'
_chemical_formula_weight         869.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.2128(13)
_cell_length_b                   22.725(4)
_cell_length_c                   20.504(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.2994(19)
_cell_angle_gamma                90
_cell_volume                     3765.1(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    93
_cell_measurement_reflns_used    7644
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      31.6

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             1788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.824
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            13465
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.069
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.955
_reflns_number_total             7013
_reflns_number_gt                6801
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.900
_reflns_Friedel_fraction_full    0.912

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0270P)²+1.9380P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7013
_refine_ls_number_parameters     436
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.27707(2) 0.77139(2) 0.73172(2) 0.00991(7) Uani 1 1 d . . . . .
P1 P 0.18030(13) 0.72596(5) 0.81508(5) 0.0104(2) Uani 1 1 d . . . . .
P3 P -0.09969(13) 0.95986(5) 0.51224(5) 0.0137(2) Uani 1 1 d . . . . .
P2 P 0.24914(13) 0.88262(4) 0.83342(5) 0.0103(2) Uani 1 1 d . . . . .
O2 O -0.0282(4) 0.72704(14) 0.62416(15) 0.0210(7) Uani 1 1 d . . . . .
F1 F -0.0854(3) 0.89281(12) 0.53749(14) 0.0270(6) Uani 1 1 d . . . . .
C6 C 0.1216(5) 0.77544(18) 0.8787(2) 0.0127(8) Uani 1 1 d . . . . .
F3 F 0.0187(3) 0.94480(13) 0.46019(13) 0.0249(6) Uani 1 1 d . . . . .
F6 F -0.1156(4) 1.02627(12) 0.48630(15) 0.0286(6) Uani 1 1 d . . . . .
O3 O 0.3445(3) 0.84495(12) 0.79257(14) 0.0124(6) Uani 1 1 d . . . . .
F2 F -0.2581(3) 0.94202(12) 0.45805(13) 0.0237(6) Uani 1 1 d . . . . .
F5 F -0.2183(3) 0.97448(13) 0.56381(14) 0.0277(6) Uani 1 1 d . . . . .
O1 O 0.1519(4) 0.71740(15) 0.55463(16) 0.0236(7) Uani 1 1 d . . . . .
C16 C -0.1553(6) 0.7251(2) 0.7631(2) 0.0257(11) Uani 1 1 d . . . . .
H21 H -0.1853 0.7446 0.8019 0.039 Uiso 1 1 calc R U . . .
H22 H -0.2507 0.7031 0.7397 0.039 Uiso 1 1 calc R U . . .
H23 H -0.1220 0.7547 0.7334 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4109(5) 0.92437(18) 0.89072(19) 0.0131(8) Uani 1 1 d . . . . .
C8 C -0.0323(6) 0.77659(19) 0.9699(2) 0.0191(9) Uani 1 1 d . . . . .
H10 H -0.0880 0.7556 0.9995 0.023 Uiso 1 1 calc R U . . .
C15 C -0.0113(5) 0.68270(19) 0.7856(2) 0.0185(9) Uani 1 1 d . . . . .
H20 H 0.0080 0.6627 0.7442 0.022 Uiso 1 1 calc R U . . .
C1 C 0.2426(5) 0.69775(19) 0.6712(2) 0.0150(9) Uani 1 1 d . . . . .
C20 C 0.3538(6) 0.9804(2) 0.9220(3) 0.0278(11) Uani 1 1 d . . . . .
H30 H 0.4497 1.0000 0.9484 0.042 Uiso 1 1 calc R U . . .
H31 H 0.2746 0.9699 0.9506 0.042 Uiso 1 1 calc R U . . .
H32 H 0.3006 1.0069 0.8869 0.042 Uiso 1 1 calc R U . . .
C4 C 0.1230(6) 0.71421(19) 0.6103(2) 0.0175(9) Uani 1 1 d . . . . .
C9 C -0.0272(6) 0.83763(19) 0.9719(2) 0.0181(9) Uani 1 1 d . . . . .
H11 H -0.0819 0.8589 1.0015 0.022 Uiso 1 1 calc R U . . .
C17 C -0.0625(7) 0.6333(2) 0.8292(3) 0.0303(12) Uani 1 1 d . . . . .
H24 H -0.1442 0.6078 0.8022 0.045 Uiso 1 1 calc R U . . .
H25 H -0.1109 0.6507 0.8651 0.045 Uiso 1 1 calc R U . . .
H26 H 0.0351 0.6101 0.8480 0.045 Uiso 1 1 calc R U . . .
C5 C -0.1555(6) 0.7395(2) 0.5676(2) 0.0255(11) Uani 1 1 d . . . . .
H6 H -0.1645 0.7064 0.5364 0.038 Uiso 1 1 calc R U . . .
H7 H -0.1268 0.7753 0.5456 0.038 Uiso 1 1 calc R U . . .
H8 H -0.2615 0.7451 0.5823 0.038 Uiso 1 1 calc R U . . .
C7 C 0.0431(5) 0.7465(2) 0.9254(2) 0.0163(9) Uani 1 1 d . . . . .
H9 H 0.0423 0.7047 0.9261 0.020 Uiso 1 1 calc R U . . .
F4 F 0.0588(3) 0.97721(13) 0.56591(13) 0.0289(7) Uani 1 1 d . . . . .
C21 C 0.5440(6) 0.9429(2) 0.8505(2) 0.0274(11) Uani 1 1 d . . . . .
H33 H 0.5836 0.9081 0.8298 0.041 Uiso 1 1 calc R U . . .
H34 H 0.6368 0.9614 0.8801 0.041 Uiso 1 1 calc R U . . .
H35 H 0.4963 0.9709 0.8160 0.041 Uiso 1 1 calc R U . . .
C10 C 0.0598(5) 0.8668(2) 0.9294(2) 0.0164(9) Uani 1 1 d . . . . .
H12 H 0.0692 0.9085 0.9323 0.020 Uiso 1 1 calc R U . . .
N1 N 0.3673(4) 0.81746(15) 0.65573(17) 0.0122(7) Uani 1 1 d . . . . .
C26 C 0.5306(5) 0.82547(19) 0.6606(2) 0.0156(9) Uani 1 1 d . . . . .
H45 H 0.6023 0.8104 0.6985 0.019 Uiso 1 1 calc R U . . .
C30 C 0.2678(5) 0.83990(19) 0.6027(2) 0.0158(9) Uani 1 1 d . . . . .
H49 H 0.1516 0.8349 0.5989 0.019 Uiso 1 1 calc R U . . .
C29 C 0.3274(6) 0.87016(19) 0.5529(2) 0.0187(9) Uani 1 1 d . . . . .
H48 H 0.2533 0.8860 0.5162 0.022 Uiso 1 1 calc R U . . .
C23 C -0.0195(6) 0.8861(2) 0.7335(2) 0.0242(10) Uani 1 1 d . . . . .
H36 H -0.0952 0.9085 0.7001 0.036 Uiso 1 1 calc R U . . .
H37 H -0.0835 0.8632 0.7605 0.036 Uiso 1 1 calc R U . . .
H38 H 0.0468 0.8595 0.7112 0.036 Uiso 1 1 calc R U . . .
C11 C 0.1341(5) 0.83738(18) 0.8825(2) 0.0128(8) Uani 1 1 d . . . . .
C28 C 0.4952(6) 0.8768(2) 0.5578(2) 0.0187(10) Uani 1 1 d . . . . .
H47 H 0.5395 0.8962 0.5239 0.022 Uiso 1 1 calc R U . . .
C22 C 0.0959(5) 0.92892(18) 0.7782(2) 0.0152(9) Uani 1 1 d . . . . .
C13 C 0.4861(6) 0.7101(2) 0.8950(2) 0.0229(10) Uani 1 1 d . . . . .
H14 H 0.5357 0.7283 0.8598 0.034 Uiso 1 1 calc R U . . .
H15 H 0.5660 0.6832 0.9208 0.034 Uiso 1 1 calc R U . . .
H16 H 0.4560 0.7409 0.9242 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3317(5) 0.67605(18) 0.8642(2) 0.0157(9) Uani 1 1 d . . . . .
H13 H 0.2806 0.6593 0.9009 0.019 Uiso 1 1 calc R U . . .
C19 C 0.4884(6) 0.8823(2) 0.9453(2) 0.0271(11) Uani 1 1 d . . . . .
H27 H 0.5843 0.9011 0.9727 0.041 Uiso 1 1 calc R U . . .
H28 H 0.5240 0.8464 0.9254 0.041 Uiso 1 1 calc R U . . .
H29 H 0.4067 0.8722 0.9730 0.041 Uiso 1 1 calc R U . . .
C27 C 0.5990(5) 0.8546(2) 0.6132(2) 0.0188(10) Uani 1 1 d . . . . .
H46 H 0.7154 0.8595 0.6183 0.023 Uiso 1 1 calc R U . . .
C3 C 0.3940(6) 0.61087(19) 0.6327(2) 0.0227(10) Uani 1 1 d . . . . .
H3 H 0.3122 0.6071 0.5918 0.034 Uiso 1 1 calc R U . . .
H4 H 0.3601 0.5866 0.6675 0.034 Uiso 1 1 calc R U . . .
H5 H 0.5022 0.5976 0.6247 0.034 Uiso 1 1 calc R U . . .
C2 C 0.4057(6) 0.67538(19) 0.6549(2) 0.0188(9) Uani 1 1 d . . . . .
H1 H 0.4936 0.6794 0.6945 0.023 Uiso 1 1 calc R U . . .
H2 H 0.4370 0.6999 0.6192 0.023 Uiso 1 1 calc R U . . .
C24 C -0.0116(6) 0.9682(2) 0.8138(2) 0.0270(11) Uani 1 1 d . . . . .
H39 H -0.0826 0.9928 0.7812 0.041 Uiso 1 1 calc R U . . .
H40 H 0.0595 0.9933 0.8458 0.041 Uiso 1 1 calc R U . . .
H41 H -0.0806 0.9436 0.8371 0.041 Uiso 1 1 calc R U . . .
Cl1 Cl 0.86720(17) 0.59212(6) 0.62161(7) 0.0349(3) Uani 1 1 d . . . . .
Cl2 Cl 1.08670(15) 0.50345(6) 0.69214(6) 0.0356(3) Uani 1 1 d . . . . .
C14 C 0.3751(7) 0.6252(2) 0.8218(2) 0.0298(12) Uani 1 1 d . . . . .
H17 H 0.4504 0.5981 0.8495 0.045 Uiso 1 1 calc R U . . .
H18 H 0.4289 0.6406 0.7864 0.045 Uiso 1 1 calc R U . . .
H19 H 0.2738 0.6042 0.8023 0.045 Uiso 1 1 calc R U . . .
C31 C 0.9571(6) 0.5227(2) 0.6165(2) 0.0242(10) Uani 1 1 d . . . . .
H50 H 1.0228 0.5229 0.5805 0.029 Uiso 1 1 calc R U . . .
H51 H 0.8687 0.4928 0.6055 0.029 Uiso 1 1 calc R U . . .
C25 C 0.1904(6) 0.9663(2) 0.7349(2) 0.0262(11) Uani 1 1 d . . . . .
H42 H 0.2521 0.9973 0.7620 0.039 Uiso 1 1 calc R U . . .
H43 H 0.1117 0.9843 0.6988 0.039 Uiso 1 1 calc R U . . .
H44 H 0.2677 0.9413 0.7162 0.039 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.072(4) . ?
Pd1 O3 2.100(3) . ?
Pd1 N1 2.118(3) . ?
Pd1 P1 2.2594(10) . ?
P1 C12 1.843(4) . ?
P1 C6 1.851(4) . ?
P1 C15 1.862(4) . ?
P3 F5 1.596(3) . ?
P3 F4 1.596(3) . ?
P3 F6 1.598(3) . ?
P3 F3 1.604(3) . ?
P3 F2 1.605(3) . ?
P3 F1 1.607(3) . ?
P2 O3 1.511(3) . ?
P2 C11 1.817(4) . ?
P2 C22 1.861(4) . ?
P2 C18 1.868(4) . ?
O2 C4 1.354(5) . ?
O2 C5 1.444(5) . ?
C6 C7 1.409(6) . ?
C6 C11 1.412(6) . ?
O1 C4 1.209(5) . ?
C16 C15 1.531(7) . ?
C18 C19 1.523(6) . ?
C18 C20 1.535(6) . ?
C18 C21 1.540(6) . ?
C8 C7 1.374(6) . ?
C8 C9 1.388(6) . ?
C15 C17 1.539(6) . ?
C1 C4 1.492(6) . ?
C1 C2 1.524(6) . ?
C9 C10 1.390(6) . ?
C10 C11 1.398(6) . ?
N1 C30 1.339(5) . ?
N1 C26 1.339(5) . ?
C26 C27 1.377(6) . ?
C30 C29 1.390(6) . ?
C29 C28 1.372(7) . ?
C23 C22 1.541(6) . ?
C28 C27 1.387(6) . ?
C22 C24 1.529(6) . ?
C22 C25 1.536(6) . ?
C13 C12 1.524(7) . ?
C12 C14 1.526(6) . ?
C3 C2 1.533(6) . ?
Cl1 C31 1.752(5) . ?
Cl2 C31 1.772(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
C1 Pd1 O3 172.63(15) . . ?
C1 Pd1 N1 89.25(15) . . ?
O3 Pd1 N1 87.35(12) . . ?
C1 Pd1 P1 93.16(12) . . ?
O3 Pd1 P1 90.31(8) . . ?
N1 Pd1 P1 177.54(10) . . ?
C12 P1 C6 102.95(18) . . ?
C12 P1 C15 107.5(2) . . ?
C6 P1 C15 103.8(2) . . ?
C12 P1 Pd1 113.60(14) . . ?
C6 P1 Pd1 115.28(14) . . ?
C15 P1 Pd1 112.76(14) . . ?
F5 P3 F4 90.63(15) . . ?
F5 P3 F6 90.05(16) . . ?
F4 P3 F6 90.23(16) . . ?
F5 P3 F3 179.59(18) . . ?
F4 P3 F3 89.71(15) . . ?
F6 P3 F3 90.18(15) . . ?
F5 P3 F2 89.76(15) . . ?
F4 P3 F2 179.54(18) . . ?
F6 P3 F2 90.02(15) . . ?
F3 P3 F2 89.91(15) . . ?
F5 P3 F1 90.12(16) . . ?
F4 P3 F1 90.48(16) . . ?
F6 P3 F1 179.27(18) . . ?
F3 P3 F1 89.65(15) . . ?
F2 P3 F1 89.27(15) . . ?
O3 P2 C11 111.02(17) . . ?
O3 P2 C22 110.13(18) . . ?
C11 P2 C22 107.1(2) . . ?
O3 P2 C18 104.81(18) . . ?
C11 P2 C18 108.74(19) . . ?
C22 P2 C18 115.03(19) . . ?
C4 O2 C5 115.6(4) . . ?
C7 C6 C11 117.8(4) . . ?
C7 C6 P1 113.8(3) . . ?
C11 C6 P1 128.2(3) . . ?
P2 O3 Pd1 132.28(17) . . ?
C19 C18 C20 109.4(4) . . ?
C19 C18 C21 108.8(4) . . ?
C20 C18 C21 107.2(4) . . ?
C19 C18 P2 107.4(3) . . ?
C20 C18 P2 116.6(3) . . ?
C21 C18 P2 107.2(3) . . ?
C7 C8 C9 120.1(4) . . ?
C16 C15 C17 110.9(4) . . ?
C16 C15 P1 109.1(3) . . ?
C17 C15 P1 119.9(3) . . ?
C4 C1 C2 111.9(4) . . ?
C4 C1 Pd1 107.3(3) . . ?
C2 C1 Pd1 111.7(3) . . ?
O1 C4 O2 121.8(4) . . ?
O1 C4 C1 126.4(4) . . ?
O2 C4 C1 111.7(4) . . ?
C8 C9 C10 118.4(4) . . ?
C8 C7 C6 122.3(4) . . ?
C9 C10 C11 122.6(4) . . ?
C30 N1 C26 117.8(4) . . ?
C30 N1 Pd1 122.9(3) . . ?
C26 N1 Pd1 119.3(3) . . ?
N1 C26 C27 122.8(4) . . ?
N1 C30 C29 122.7(4) . . ?
C28 C29 C30 118.8(4) . . ?
C10 C11 C6 118.6(4) . . ?
C10 C11 P2 116.3(3) . . ?
C6 C11 P2 125.0(3) . . ?
C29 C28 C27 118.8(4) . . ?
C24 C22 C25 110.3(4) . . ?
C24 C22 C23 107.8(4) . . ?
C25 C22 C23 109.0(4) . . ?
C24 C22 P2 115.1(3) . . ?
C25 C22 P2 108.0(3) . . ?
C23 C22 P2 106.4(3) . . ?
C13 C12 C14 111.0(4) . . ?
C13 C12 P1 110.1(3) . . ?
C14 C12 P1 111.0(3) . . ?
C26 C27 C28 119.0(4) . . ?
C1 C2 C3 111.9(4) . . ?
Cl1 C31 Cl2 111.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 P1 C6 C7 -63.1(4) . . . . ?
C15 P1 C6 C7 48.9(4) . . . . ?
Pd1 P1 C6 C7 172.6(3) . . . . ?
C12 P1 C6 C11 122.3(4) . . . . ?
C15 P1 C6 C11 -125.7(4) . . . . ?
Pd1 P1 C6 C11 -1.9(4) . . . . ?
C11 P2 O3 Pd1 47.0(3) . . . . ?
C22 P2 O3 Pd1 -71.5(3) . . . . ?
C18 P2 O3 Pd1 164.3(2) . . . . ?
O3 P2 C18 C19 -76.5(3) . . . . ?
C11 P2 C18 C19 42.3(4) . . . . ?
C22 P2 C18 C19 162.4(3) . . . . ?
O3 P2 C18 C20 160.3(3) . . . . ?
C11 P2 C18 C20 -80.9(4) . . . . ?
C22 P2 C18 C20 39.2(4) . . . . ?
O3 P2 C18 C21 40.2(3) . . . . ?
C11 P2 C18 C21 159.0(3) . . . . ?
C22 P2 C18 C21 -80.9(4) . . . . ?
C12 P1 C15 C16 163.1(3) . . . . ?
C6 P1 C15 C16 54.5(3) . . . . ?
Pd1 P1 C15 C16 -70.9(3) . . . . ?
C12 P1 C15 C17 33.6(4) . . . . ?
C6 P1 C15 C17 -75.0(4) . . . . ?
Pd1 P1 C15 C17 159.6(3) . . . . ?
C5 O2 C4 O1 5.4(6) . . . . ?
C5 O2 C4 C1 -175.8(4) . . . . ?
C2 C1 C4 O1 -8.9(6) . . . . ?
Pd1 C1 C4 O1 113.9(4) . . . . ?
C2 C1 C4 O2 172.3(4) . . . . ?
Pd1 C1 C4 O2 -64.8(4) . . . . ?
C7 C8 C9 C10 -2.0(7) . . . . ?
C9 C8 C7 C6 -2.6(7) . . . . ?
C11 C6 C7 C8 5.5(7) . . . . ?
P1 C6 C7 C8 -169.6(4) . . . . ?
C8 C9 C10 C11 3.7(7) . . . . ?
C30 N1 C26 C27 -1.1(6) . . . . ?
Pd1 N1 C26 C27 179.6(3) . . . . ?
C26 N1 C30 C29 0.7(6) . . . . ?
Pd1 N1 C30 C29 179.9(3) . . . . ?
N1 C30 C29 C28 0.8(7) . . . . ?
C9 C10 C11 C6 -0.7(7) . . . . ?
C9 C10 C11 P2 -177.8(3) . . . . ?
C7 C6 C11 C10 -3.8(6) . . . . ?
P1 C6 C11 C10 170.6(3) . . . . ?
C7 C6 C11 P2 173.0(3) . . . . ?
P1 C6 C11 P2 -12.6(6) . . . . ?
O3 P2 C11 C10 171.2(3) . . . . ?
C22 P2 C11 C10 -68.5(4) . . . . ?
C18 P2 C11 C10 56.4(4) . . . . ?
O3 P2 C11 C6 -5.6(4) . . . . ?
C22 P2 C11 C6 114.6(4) . . . . ?
C18 P2 C11 C6 -120.4(4) . . . . ?
C30 C29 C28 C27 -1.9(7) . . . . ?
O3 P2 C22 C24 178.7(3) . . . . ?
C11 P2 C22 C24 57.8(4) . . . . ?
C18 P2 C22 C24 -63.2(4) . . . . ?
O3 P2 C22 C25 -57.6(3) . . . . ?
C11 P2 C22 C25 -178.5(3) . . . . ?
C18 P2 C22 C25 60.5(4) . . . . ?
O3 P2 C22 C23 59.3(3) . . . . ?
C11 P2 C22 C23 -61.6(3) . . . . ?
C18 P2 C22 C23 177.4(3) . . . . ?
C6 P1 C12 C13 -65.8(3) . . . . ?
C15 P1 C12 C13 -175.0(3) . . . . ?
Pd1 P1 C12 C13 59.6(3) . . . . ?
C6 P1 C12 C14 170.9(3) . . . . ?
C15 P1 C12 C14 61.7(4) . . . . ?
Pd1 P1 C12 C14 -63.8(4) . . . . ?
N1 C26 C27 C28 0.0(7) . . . . ?
C29 C28 C27 C26 1.6(7) . . . . ?
C4 C1 C2 C3 -80.3(5) . . . . ?
Pd1 C1 C2 C3 159.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C16 H23 O2 0.98 2.57 3.205(6) 122.3 .
C21 H35 Cl2 0.98 2.87 3.601(5) 132.3 3_455
C10 H12 F6 0.95 2.52 3.153(5) 124.5 2_575
C30 H49 F1 0.95 2.50 3.203(5) 131.3 .
C29 H48 F3 0.95 2.46 3.346(5) 156.2 .
C12 H13 F2 1.00 2.63 3.458(5) 140.3 4_565
C27 H46 F1 0.95 2.64 3.365(5) 133.6 1_655
C14 H17 F3 0.98 2.44 3.283(6) 143.8 4_565
C31 H50 F5 0.99 2.47 3.241(6) 134.3 3_645
C31 H51 F4 0.99 2.55 3.410(6) 144.7 3_545

_refine_diff_density_max         0.543
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.059

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_AniMA21
_database_code_depnum_ccdc_archive 'CCDC 1408867'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H45 O5 P2 Pd, F6 P, C H Cl3, C H Cl2'
_chemical_formula_sum            'C35 H47 Cl5 F6 O5 P3 Pd'
_chemical_formula_weight         1038.28

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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.521(3)
_cell_length_b                   16.475(4)
_cell_length_c                   22.564(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.836(4)
_cell_angle_gamma                90
_cell_volume                     4219.9(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    93
_cell_measurement_reflns_used    14363
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      31.6

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_F_000             2108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.937
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            44666
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.473
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8269
_reflns_number_gt                7736
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0687P)²+24.4956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8269
_refine_ls_number_parameters     516
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.45065(3) 0.62408(2) 0.52925(2) 0.01145(11) Uani 1 1 d . . . . .
P1 P 0.41686(10) 0.74837(7) 0.49311(5) 0.0116(2) Uani 1 1 d . . . . .
P2 P 0.28024(10) 0.70154(7) 0.61723(5) 0.0136(2) Uani 1 1 d . . . . .
P3 P 0.15267(11) 0.42660(7) 0.24899(5) 0.0163(3) Uani 1 1 d . . . . .
Cl2 Cl 0.11933(12) 0.09106(9) 0.25484(6) 0.0339(3) Uani 1 1 d . . . . .
Cl3 Cl 0.37262(13) 0.11127(9) 0.28311(9) 0.0415(4) Uani 1 1 d . . . . .
Cl1 Cl 0.2484(2) 0.13182(11) 0.16052(9) 0.0575(5) Uani 1 1 d . . . . .
O1 O 0.5189(3) 0.48707(19) 0.42332(14) 0.0168(7) Uani 1 1 d . . . . .
F3 F 0.0159(3) 0.4192(2) 0.25319(14) 0.0293(7) Uani 1 1 d . . . . .
F4 F 0.2900(3) 0.4333(2) 0.24416(14) 0.0289(7) Uani 1 1 d . . . . .
O3 O 0.3022(3) 0.64025(19) 0.57019(14) 0.0153(6) Uani 1 1 d . . . . .
F5 F 0.1436(3) 0.52272(19) 0.24720(17) 0.0359(8) Uani 1 1 d . . . . .
O2 O 0.4817(3) 0.61074(19) 0.38634(14) 0.0176(7) Uani 1 1 d . . . . .
O5 O 0.6409(3) 0.7860(2) 0.56314(15) 0.0193(7) Uani 1 1 d . . . . .
F6 F 0.1858(3) 0.4283(2) 0.32051(14) 0.0402(9) Uani 1 1 d . . . . .
F1 F 0.1200(3) 0.4229(2) 0.17729(14) 0.0366(8) Uani 1 1 d . . . . .
F2 F 0.1632(3) 0.3295(2) 0.25109(19) 0.0460(10) Uani 1 1 d . . . . .
O4 O 0.3085(4) 0.8897(2) 0.41786(17) 0.0288(9) Uani 1 1 d . . . . .
C4 C 0.5300(4) 0.5612(3) 0.4303(2) 0.0138(9) Uani 1 1 d . . . . .
C1 C 0.5905(4) 0.6043(3) 0.4844(2) 0.0151(9) Uani 1 1 d . . . . .
H1 H 0.6206 0.6577 0.4722 0.018 Uiso 1 1 calc R U . . .
C6 C 0.3824(4) 0.8214(3) 0.5498(2) 0.0145(9) Uani 1 1 d . . . . .
C11 C 0.3207(4) 0.8036(3) 0.5972(2) 0.0151(9) Uani 1 1 d . . . . .
C19 C 0.5395(4) 0.7936(3) 0.4642(2) 0.0145(9) Uani 1 1 d . . . . .
C7 C 0.4180(4) 0.9017(3) 0.5434(2) 0.0176(9) Uani 1 1 d . . . . .
H10 H 0.4617 0.9141 0.5124 0.021 Uiso 1 1 calc R U . . .
C12 C 0.2887(4) 0.7498(3) 0.4336(2) 0.0173(9) Uani 1 1 d . . . . .
C20 C 0.6461(4) 0.8030(3) 0.5041(2) 0.0151(9) Uani 1 1 d . . . . .
C24 C 0.5378(4) 0.8056(3) 0.4028(2) 0.0169(9) Uani 1 1 d . . . . .
H24 H 0.4664 0.7986 0.3753 0.020 Uiso 1 1 calc R U . . .
C2 C 0.6907(4) 0.5580(3) 0.5227(2) 0.0198(10) Uani 1 1 d . . . . .
H2 H 0.6641 0.5022 0.5297 0.024 Uiso 1 1 calc R U . . .
H3 H 0.7116 0.5850 0.5623 0.024 Uiso 1 1 calc R U . . .
C10 C 0.2936(5) 0.8680(3) 0.6338(2) 0.0217(10) Uani 1 1 d . . . . .
H13 H 0.2502 0.8566 0.6651 0.026 Uiso 1 1 calc R U . . .
C30 C 0.3765(4) 0.6786(3) 0.6895(2) 0.0191(10) Uani 1 1 d . . . . .
C13 C 0.2462(4) 0.8207(3) 0.4025(2) 0.0225(11) Uani 1 1 d . . . . .
C17 C 0.2279(4) 0.6774(3) 0.4196(2) 0.0223(10) Uani 1 1 d . . . . .
H17 H 0.2549 0.6293 0.4408 0.027 Uiso 1 1 calc R U . . .
C32 C 0.5039(4) 0.6791(3) 0.6767(2) 0.0225(10) Uani 1 1 d . . . . .
H40 H 0.5148 0.6334 0.6504 0.034 Uiso 1 1 calc R U . . .
H41 H 0.5592 0.6741 0.7147 0.034 Uiso 1 1 calc R U . . .
H42 H 0.5186 0.7302 0.6569 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4079(5) 0.5724(3) 0.3351(2) 0.0228(11) Uani 1 1 d . . . . .
H7 H 0.3523 0.5352 0.3494 0.034 Uiso 1 1 calc R U . . .
H8 H 0.4576 0.5420 0.3117 0.034 Uiso 1 1 calc R U . . .
H9 H 0.3640 0.6142 0.3096 0.034 Uiso 1 1 calc R U . . .
C14 C 0.1445(5) 0.8174(4) 0.3584(3) 0.0316(13) Uani 1 1 d . . . . .
H14 H 0.1150 0.8653 0.3378 0.038 Uiso 1 1 calc R U . . .
C21 C 0.7480(4) 0.8253(3) 0.4832(2) 0.0218(10) Uani 1 1 d . . . . .
H21 H 0.8198 0.8323 0.5105 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6399(5) 0.8276(3) 0.3818(2) 0.0226(11) Uani 1 1 d . . . . .
H23 H 0.6380 0.8360 0.3400 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3921(5) 0.9639(3) 0.5803(2) 0.0251(11) Uani 1 1 d . . . . .
H11 H 0.4177 1.0177 0.5748 0.030 Uiso 1 1 calc R U . . .
C26 C 0.1187(4) 0.6962(3) 0.6169(2) 0.0232(11) Uani 1 1 d . . . . .
C29 C 0.0762(5) 0.7361(4) 0.6710(3) 0.0280(12) Uani 1 1 d . . . . .
H34 H -0.0091 0.7290 0.6674 0.042 Uiso 1 1 calc R U . . .
H35 H 0.0949 0.7942 0.6718 0.042 Uiso 1 1 calc R U . . .
H36 H 0.1158 0.7107 0.7083 0.042 Uiso 1 1 calc R U . . .
C22 C 0.7441(5) 0.8374(3) 0.4216(2) 0.0232(11) Uani 1 1 d . . . . .
H22 H 0.8137 0.8524 0.4070 0.028 Uiso 1 1 calc R U . . .
C15 C 0.0874(5) 0.7445(4) 0.3450(3) 0.0356(14) Uani 1 1 d . . . . .
H15 H 0.0192 0.7427 0.3147 0.043 Uiso 1 1 calc R U . . .
C25 C 0.7495(4) 0.7711(3) 0.6029(2) 0.0243(11) Uani 1 1 d . . . . .
H25 H 0.7933 0.8221 0.6106 0.036 Uiso 1 1 calc R U . . .
H26 H 0.7966 0.7320 0.5844 0.036 Uiso 1 1 calc R U . . .
H27 H 0.7331 0.7490 0.6410 0.036 Uiso 1 1 calc R U . . .
C9 C 0.3277(5) 0.9460(3) 0.6259(2) 0.0274(12) Uani 1 1 d . . . . .
H12 H 0.3078 0.9880 0.6512 0.033 Uiso 1 1 calc R U . . .
C16 C 0.1271(5) 0.6744(4) 0.3746(3) 0.0313(13) Uani 1 1 d . . . . .
H16 H 0.0870 0.6245 0.3649 0.038 Uiso 1 1 calc R U . . .
C3 C 0.8006(4) 0.5539(3) 0.4922(2) 0.0268(11) Uani 1 1 d . . . . .
H4 H 0.8278 0.6090 0.4858 0.040 Uiso 1 1 calc R U . . .
H5 H 0.7807 0.5260 0.4534 0.040 Uiso 1 1 calc R U . . .
H6 H 0.8633 0.5240 0.5181 0.040 Uiso 1 1 calc R U . . .
C31 C 0.3490(6) 0.5931(4) 0.7101(3) 0.0339(13) Uani 1 1 d . . . . .
H37 H 0.4101 0.5765 0.7437 0.051 Uiso 1 1 calc R U . . .
H38 H 0.3473 0.5550 0.6766 0.051 Uiso 1 1 calc R U . . .
H39 H 0.2722 0.5933 0.7232 0.051 Uiso 1 1 calc R U . . .
C33 C 0.3705(5) 0.7400(4) 0.7406(2) 0.0279(12) Uani 1 1 d . . . . .
H43 H 0.4232 0.7224 0.7771 0.042 Uiso 1 1 calc R U . . .
H44 H 0.2896 0.7429 0.7486 0.042 Uiso 1 1 calc R U . . .
H45 H 0.3949 0.7937 0.7286 0.042 Uiso 1 1 calc R U . . .
C34 C 0.2408(5) 0.1450(3) 0.2373(3) 0.0320(13) Uani 1 1 d . . . . .
H46 H 0.2299 0.2040 0.2451 0.038 Uiso 1 1 calc R U . . .
C28 C 0.0634(5) 0.7361(5) 0.5575(3) 0.0388(15) Uani 1 1 d . . . . .
H31 H 0.0798 0.7945 0.5595 0.058 Uiso 1 1 calc R U . . .
H32 H -0.0220 0.7273 0.5506 0.058 Uiso 1 1 calc R U . . .
H33 H 0.0969 0.7121 0.5245 0.058 Uiso 1 1 calc R U . . .
C27 C 0.0835(5) 0.6063(4) 0.6145(3) 0.0358(14) Uani 1 1 d . . . . .
H28 H -0.0020 0.6017 0.6118 0.054 Uiso 1 1 calc R U . . .
H29 H 0.1229 0.5789 0.6511 0.054 Uiso 1 1 calc R U . . .
H30 H 0.1073 0.5808 0.5792 0.054 Uiso 1 1 calc R U . . .
C18 C 0.2788(7) 0.9612(4) 0.3821(3) 0.0439(16) Uani 1 1 d . . . . .
H18 H 0.2000 0.9798 0.3868 0.066 Uiso 1 1 calc R U . . .
H19 H 0.2796 0.9487 0.3398 0.066 Uiso 1 1 calc R U . . .
H20 H 0.3364 1.0040 0.3955 0.066 Uiso 1 1 calc R U . . .
Cl5 Cl 0.0646(4) -0.0683(2) 0.48301(18) 0.0505(11) Uani 0.775(13) 1 d . U P A 2
Cl4 Cl -0.0138(3) -0.06631(18) 0.60264(13) 0.0847(7) Uani 1 1 d . . . . .
C35 C 0.0336(14) -0.0007(10) 0.5456(6) 0.132(6) Uani 1 1 d . . . . .
H47 H 0.0751 0.0472 0.5666 0.158 Uiso 0.225(13) 1 calc R U P A 1
H48 H 0.1081 0.0275 0.5638 0.158 Uiso 0.775(13) 1 calc R U P A 2
Cl6 Cl 0.1146(14) -0.0363(10) 0.4993(6) 0.054(3) Uani 0.225(13) 1 d . U P A 1


_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 C1 2.070(5) . ?
Pd1 O3 2.095(3) . ?
Pd1 O1 2.120(3) 3_666 ?
Pd1 P1 2.2138(12) . ?
P1 C19 1.814(5) . ?
P1 C12 1.818(5) . ?
P1 C6 1.848(5) . ?
P2 O3 1.517(3) . ?
P2 C11 1.823(5) . ?
P2 C30 1.848(5) . ?
P2 C26 1.862(5) . ?
P3 F5 1.587(3) . ?
P3 F6 1.594(3) . ?
P3 F1 1.598(3) . ?
P3 F3 1.599(3) . ?
P3 F2 1.605(4) . ?
P3 F4 1.608(3) . ?
Cl2 C34 1.760(6) . ?
Cl3 C34 1.775(7) . ?
Cl1 C34 1.762(6) . ?
O1 C4 1.235(6) . ?
O1 Pd1 2.120(3) 3_666 ?
O2 C4 1.330(6) . ?
O2 C5 1.458(6) . ?
O5 C20 1.373(5) . ?
O5 C25 1.431(6) . ?
O4 C13 1.358(7) . ?
O4 C18 1.435(6) . ?
C4 C1 1.481(6) . ?
C1 C2 1.524(6) . ?
C1 H1 1.0000 . ?
C6 C7 1.400(7) . ?
C6 C11 1.412(6) . ?
C11 C10 1.413(7) . ?
C19 C24 1.394(6) . ?
C19 C20 1.402(7) . ?
C7 C8 1.384(7) . ?
C7 H10 0.9500 . ?
C12 C17 1.393(7) . ?
C12 C13 1.407(7) . ?
C20 C21 1.388(7) . ?
C24 C23 1.390(7) . ?
C24 H24 0.9500 . ?
C2 C3 1.542(7) . ?
C2 H2 0.9900 . ?
C2 H3 0.9900 . ?
C10 C9 1.364(7) . ?
C10 H13 0.9500 . ?
C30 C31 1.533(7) . ?
C30 C32 1.543(7) . ?
C30 C33 1.544(7) . ?
C13 C14 1.403(7) . ?
C17 C16 1.407(7) . ?
C17 H17 0.9500 . ?
C32 H40 0.9800 . ?
C32 H41 0.9800 . ?
C32 H42 0.9800 . ?
C5 H7 0.9800 . ?
C5 H8 0.9800 . ?
C5 H9 0.9800 . ?
C14 C15 1.378(9) . ?
C14 H14 0.9500 . ?
C21 C22 1.396(7) . ?
C21 H21 0.9500 . ?
C23 C22 1.381(8) . ?
C23 H23 0.9500 . ?
C8 C9 1.399(8) . ?
C8 H11 0.9500 . ?
C26 C28 1.530(8) . ?
C26 C27 1.534(8) . ?
C26 C29 1.538(7) . ?
C29 H34 0.9800 . ?
C29 H35 0.9800 . ?
C29 H36 0.9800 . ?
C22 H22 0.9500 . ?
C15 C16 1.372(9) . ?
C15 H15 0.9500 . ?
C25 H25 0.9800 . ?
C25 H26 0.9800 . ?
C25 H27 0.9800 . ?
C9 H12 0.9500 . ?
C16 H16 0.9500 . ?
C3 H4 0.9800 . ?
C3 H5 0.9800 . ?
C3 H6 0.9800 . ?
C31 H37 0.9800 . ?
C31 H38 0.9800 . ?
C31 H39 0.9800 . ?
C33 H43 0.9800 . ?
C33 H44 0.9800 . ?
C33 H45 0.9800 . ?
C34 H46 1.0000 . ?
C28 H31 0.9800 . ?
C28 H32 0.9800 . ?
C28 H33 0.9800 . ?
C27 H28 0.9800 . ?
C27 H29 0.9800 . ?
C27 H30 0.9800 . ?
C18 H18 0.9800 . ?
C18 H19 0.9800 . ?
C18 H20 0.9800 . ?
Cl5 C35 1.655(18) 3_556 ?
Cl5 C35 1.880(17) . ?
Cl4 C35 1.834(13) . ?
C35 Cl6 1.625(19) . ?
C35 Cl5 1.655(18) 3_556 ?
C35 Cl6 1.93(2) 3_556 ?
C35 H47 1.0000 . ?
C35 H48 1.0000 . ?
Cl6 C35 1.93(2) 3_556 ?

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
C1 Pd1 O3 176.36(15) . . ?
C1 Pd1 O1 92.02(16) . 3_666 ?
O3 Pd1 O1 87.97(13) . 3_666 ?
C1 Pd1 P1 93.90(13) . . ?
O3 Pd1 P1 86.53(9) . . ?
O1 Pd1 P1 171.32(9) 3_666 . ?
C19 P1 C12 108.2(2) . . ?
C19 P1 C6 104.7(2) . . ?
C12 P1 C6 105.0(2) . . ?
C19 P1 Pd1 114.43(15) . . ?
C12 P1 Pd1 110.72(17) . . ?
C6 P1 Pd1 113.12(15) . . ?
O3 P2 C11 111.1(2) . . ?
O3 P2 C30 109.6(2) . . ?
C11 P2 C30 105.5(2) . . ?
O3 P2 C26 104.6(2) . . ?
C11 P2 C26 109.9(2) . . ?
C30 P2 C26 116.3(2) . . ?
F5 P3 F6 90.7(2) . . ?
F5 P3 F1 90.5(2) . . ?
F6 P3 F1 178.8(2) . . ?
F5 P3 F3 90.93(18) . . ?
F6 P3 F3 90.54(18) . . ?
F1 P3 F3 89.62(17) . . ?
F5 P3 F2 179.4(2) . . ?
F6 P3 F2 89.1(2) . . ?
F1 P3 F2 89.8(2) . . ?
F3 P3 F2 89.57(19) . . ?
F5 P3 F4 89.48(18) . . ?
F6 P3 F4 89.94(18) . . ?
F1 P3 F4 89.88(17) . . ?
F3 P3 F4 179.4(2) . . ?
F2 P3 F4 90.02(19) . . ?
C4 O1 Pd1 141.8(3) . 3_666 ?
P2 O3 Pd1 129.72(19) . . ?
C4 O2 C5 116.0(4) . . ?
C20 O5 C25 117.7(4) . . ?
C13 O4 C18 118.6(4) . . ?
O1 C4 O2 119.4(4) . . ?
O1 C4 C1 127.1(4) . . ?
O2 C4 C1 113.5(4) . . ?
C4 C1 C2 115.6(4) . . ?
C4 C1 Pd1 100.5(3) . . ?
C2 C1 Pd1 112.3(3) . . ?
C4 C1 H1 109.4 . . ?
C2 C1 H1 109.4 . . ?
Pd1 C1 H1 109.4 . . ?
C7 C6 C11 118.0(4) . . ?
C7 C6 P1 116.3(3) . . ?
C11 C6 P1 125.7(4) . . ?
C6 C11 C10 118.6(4) . . ?
C6 C11 P2 124.3(3) . . ?
C10 C11 P2 117.1(4) . . ?
C24 C19 C20 118.9(4) . . ?
C24 C19 P1 122.4(4) . . ?
C20 C19 P1 117.7(3) . . ?
C8 C7 C6 122.7(5) . . ?
C8 C7 H10 118.7 . . ?
C6 C7 H10 118.7 . . ?
C17 C12 C13 118.6(4) . . ?
C17 C12 P1 118.0(4) . . ?
C13 C12 P1 123.3(4) . . ?
O5 C20 C21 124.3(4) . . ?
O5 C20 C19 115.0(4) . . ?
C21 C20 C19 120.7(4) . . ?
C23 C24 C19 120.4(5) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
C1 C2 C3 111.7(4) . . ?
C1 C2 H2 109.3 . . ?
C3 C2 H2 109.3 . . ?
C1 C2 H3 109.3 . . ?
C3 C2 H3 109.3 . . ?
H2 C2 H3 107.9 . . ?
C9 C10 C11 122.2(5) . . ?
C9 C10 H13 118.9 . . ?
C11 C10 H13 118.9 . . ?
C31 C30 C32 108.3(4) . . ?
C31 C30 C33 109.7(4) . . ?
C32 C30 C33 107.6(4) . . ?
C31 C30 P2 109.3(4) . . ?
C32 C30 P2 106.3(3) . . ?
C33 C30 P2 115.4(4) . . ?
O4 C13 C14 123.7(5) . . ?
O4 C13 C12 116.3(4) . . ?
C14 C13 C12 119.9(5) . . ?
C12 C17 C16 121.0(5) . . ?
C12 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C30 C32 H40 109.5 . . ?
C30 C32 H41 109.5 . . ?
H40 C32 H41 109.5 . . ?
C30 C32 H42 109.5 . . ?
H40 C32 H42 109.5 . . ?
H41 C32 H42 109.5 . . ?
O2 C5 H7 109.5 . . ?
O2 C5 H8 109.5 . . ?
H7 C5 H8 109.5 . . ?
O2 C5 H9 109.5 . . ?
H7 C5 H9 109.5 . . ?
H8 C5 H9 109.5 . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C20 C21 C22 119.3(5) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C22 C23 C24 120.1(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C7 C8 C9 118.9(5) . . ?
C7 C8 H11 120.6 . . ?
C9 C8 H11 120.6 . . ?
C28 C26 C27 108.5(5) . . ?
C28 C26 C29 111.7(5) . . ?
C27 C26 C29 108.8(4) . . ?
C28 C26 P2 104.5(4) . . ?
C27 C26 P2 107.7(4) . . ?
C29 C26 P2 115.5(4) . . ?
C26 C29 H34 109.5 . . ?
C26 C29 H35 109.5 . . ?
H34 C29 H35 109.5 . . ?
C26 C29 H36 109.5 . . ?
H34 C29 H36 109.5 . . ?
H35 C29 H36 109.5 . . ?
C23 C22 C21 120.5(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C16 C15 C14 121.3(5) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
O5 C25 H25 109.5 . . ?
O5 C25 H26 109.5 . . ?
H25 C25 H26 109.5 . . ?
O5 C25 H27 109.5 . . ?
H25 C25 H27 109.5 . . ?
H26 C25 H27 109.5 . . ?
C10 C9 C8 119.7(5) . . ?
C10 C9 H12 120.1 . . ?
C8 C9 H12 120.1 . . ?
C15 C16 C17 119.1(5) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C2 C3 H4 109.5 . . ?
C2 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
C2 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?
C30 C31 H37 109.5 . . ?
C30 C31 H38 109.5 . . ?
H37 C31 H38 109.5 . . ?
C30 C31 H39 109.5 . . ?
H37 C31 H39 109.5 . . ?
H38 C31 H39 109.5 . . ?
C30 C33 H43 109.5 . . ?
C30 C33 H44 109.5 . . ?
H43 C33 H44 109.5 . . ?
C30 C33 H45 109.5 . . ?
H43 C33 H45 109.5 . . ?
H44 C33 H45 109.5 . . ?
Cl2 C34 Cl1 109.5(3) . . ?
Cl2 C34 Cl3 110.1(3) . . ?
Cl1 C34 Cl3 110.7(3) . . ?
Cl2 C34 H46 108.8 . . ?
Cl1 C34 H46 108.8 . . ?
Cl3 C34 H46 108.8 . . ?
C26 C28 H31 109.5 . . ?
C26 C28 H32 109.5 . . ?
H31 C28 H32 109.5 . . ?
C26 C28 H33 109.5 . . ?
H31 C28 H33 109.5 . . ?
H32 C28 H33 109.5 . . ?
C26 C27 H28 109.5 . . ?
C26 C27 H29 109.5 . . ?
H28 C27 H29 109.5 . . ?
C26 C27 H30 109.5 . . ?
H28 C27 H30 109.5 . . ?
H29 C27 H30 109.5 . . ?
O4 C18 H18 109.5 . . ?
O4 C18 H19 109.5 . . ?
H18 C18 H19 109.5 . . ?
O4 C18 H20 109.5 . . ?
H18 C18 H20 109.5 . . ?
H19 C18 H20 109.5 . . ?
C35 Cl5 C35 71.4(8) 3_556 . ?
Cl6 C35 Cl4 120.7(11) . . ?
Cl5 C35 Cl4 114.4(9) 3_556 . ?
Cl5 C35 Cl5 108.6(8) 3_556 . ?
Cl4 C35 Cl5 107.2(8) . . ?
Cl6 C35 Cl6 109.3(9) . 3_556 ?
Cl4 C35 Cl6 102.3(8) . 3_556 ?
Cl6 C35 H47 108.0 . . ?
Cl4 C35 H47 108.0 . . ?
Cl6 C35 H47 108.0 3_556 . ?
Cl5 C35 H48 108.8 3_556 . ?
Cl4 C35 H48 108.8 . . ?
Cl5 C35 H48 108.8 . . ?
C35 Cl6 C35 70.7(8) . 3_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 P2 O3 Pd1 47.5(3) . . . . ?
C30 P2 O3 Pd1 -68.7(3) . . . . ?
C26 P2 O3 Pd1 166.0(3) . . . . ?
Pd1 O1 C4 O2 -171.1(3) 3_666 . . . ?
Pd1 O1 C4 C1 7.1(8) 3_666 . . . ?
C5 O2 C4 O1 6.2(6) . . . . ?
C5 O2 C4 C1 -172.2(4) . . . . ?
O1 C4 C1 C2 28.6(7) . . . . ?
O2 C4 C1 C2 -153.1(4) . . . . ?
O1 C4 C1 Pd1 -92.5(5) . . . . ?
O2 C4 C1 Pd1 85.8(4) . . . . ?
C19 P1 C6 C7 23.1(4) . . . . ?
C12 P1 C6 C7 -90.8(4) . . . . ?
Pd1 P1 C6 C7 148.4(3) . . . . ?
C19 P1 C6 C11 -159.0(4) . . . . ?
C12 P1 C6 C11 87.1(4) . . . . ?
Pd1 P1 C6 C11 -33.8(4) . . . . ?
C7 C6 C11 C10 2.7(7) . . . . ?
P1 C6 C11 C10 -175.1(4) . . . . ?
C7 C6 C11 P2 -173.6(4) . . . . ?
P1 C6 C11 P2 8.6(6) . . . . ?
O3 P2 C11 C6 -9.9(5) . . . . ?
C30 P2 C11 C6 108.8(4) . . . . ?
C26 P2 C11 C6 -125.2(4) . . . . ?
O3 P2 C11 C10 173.7(4) . . . . ?
C30 P2 C11 C10 -67.7(4) . . . . ?
C26 P2 C11 C10 58.4(4) . . . . ?
C12 P1 C19 C24 -15.2(4) . . . . ?
C6 P1 C19 C24 -126.9(4) . . . . ?
Pd1 P1 C19 C24 108.7(4) . . . . ?
C12 P1 C19 C20 176.3(3) . . . . ?
C6 P1 C19 C20 64.7(4) . . . . ?
Pd1 P1 C19 C20 -59.8(4) . . . . ?
C11 C6 C7 C8 -1.9(7) . . . . ?
P1 C6 C7 C8 176.1(4) . . . . ?
C19 P1 C12 C17 127.9(4) . . . . ?
C6 P1 C12 C17 -120.6(4) . . . . ?
Pd1 P1 C12 C17 1.8(4) . . . . ?
C19 P1 C12 C13 -54.1(5) . . . . ?
C6 P1 C12 C13 57.4(5) . . . . ?
Pd1 P1 C12 C13 179.8(4) . . . . ?
C25 O5 C20 C21 -15.7(7) . . . . ?
C25 O5 C20 C19 162.2(4) . . . . ?
C24 C19 C20 O5 -176.8(4) . . . . ?
P1 C19 C20 O5 -7.9(5) . . . . ?
C24 C19 C20 C21 1.2(7) . . . . ?
P1 C19 C20 C21 170.1(4) . . . . ?
C20 C19 C24 C23 -0.9(7) . . . . ?
P1 C19 C24 C23 -169.3(4) . . . . ?
C4 C1 C2 C3 73.2(5) . . . . ?
Pd1 C1 C2 C3 -172.2(3) . . . . ?
C6 C11 C10 C9 -1.7(8) . . . . ?
P2 C11 C10 C9 174.9(4) . . . . ?
O3 P2 C30 C31 -60.1(4) . . . . ?
C11 P2 C30 C31 -179.8(4) . . . . ?
C26 P2 C30 C31 58.1(4) . . . . ?
O3 P2 C30 C32 56.5(4) . . . . ?
C11 P2 C30 C32 -63.1(4) . . . . ?
C26 P2 C30 C32 174.8(3) . . . . ?
O3 P2 C30 C33 175.7(4) . . . . ?
C11 P2 C30 C33 56.0(4) . . . . ?
C26 P2 C30 C33 -66.1(4) . . . . ?
C18 O4 C13 C14 -8.4(8) . . . . ?
C18 O4 C13 C12 171.6(5) . . . . ?
C17 C12 C13 O4 180.0(4) . . . . ?
P1 C12 C13 O4 2.0(6) . . . . ?
C17 C12 C13 C14 0.0(7) . . . . ?
P1 C12 C13 C14 -178.0(4) . . . . ?
C13 C12 C17 C16 1.1(7) . . . . ?
P1 C12 C17 C16 179.2(4) . . . . ?
O4 C13 C14 C15 179.1(5) . . . . ?
C12 C13 C14 C15 -0.9(8) . . . . ?
O5 C20 C21 C22 176.9(4) . . . . ?
C19 C20 C21 C22 -0.9(7) . . . . ?
C19 C24 C23 C22 0.4(7) . . . . ?
C6 C7 C8 C9 -0.1(8) . . . . ?
O3 P2 C26 C28 -71.7(4) . . . . ?
C11 P2 C26 C28 47.7(4) . . . . ?
C30 P2 C26 C28 167.4(4) . . . . ?
O3 P2 C26 C27 43.5(4) . . . . ?
C11 P2 C26 C27 162.9(4) . . . . ?
C30 P2 C26 C27 -77.4(4) . . . . ?
O3 P2 C26 C29 165.3(4) . . . . ?
C11 P2 C26 C29 -75.4(4) . . . . ?
C30 P2 C26 C29 44.3(5) . . . . ?
C24 C23 C22 C21 -0.1(7) . . . . ?
C20 C21 C22 C23 0.3(7) . . . . ?
C13 C14 C15 C16 0.8(9) . . . . ?
C11 C10 C9 C8 -0.3(8) . . . . ?
C7 C8 C9 C10 1.2(8) . . . . ?
C14 C15 C16 C17 0.2(9) . . . . ?
C12 C17 C16 C15 -1.2(8) . . . . ?
C35 Cl5 C35 Cl5 0.001(1) 3_556 . . 3_556 ?
C35 Cl5 C35 Cl4 124.1(12) 3_556 . . . ?
Cl4 C35 Cl6 C35 118.0(13) . . . 3_556 ?
Cl6 C35 Cl6 C35 -0.002(1) 3_556 . . 3_556 ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -2.736
_refine_diff_density_rms         0.143

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_CF3MA21
_database_code_depnum_ccdc_archive 'CCDC 1408868'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H44 F6 N O3 P2 Pd, F6 P'
_chemical_formula_sum            'C38 H44 F12 N O3 P3 Pd'
_chemical_formula_weight         990.05

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'
F F 0.0171 0.0103 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.361(3)
_cell_length_b                   22.678(5)
_cell_length_c                   25.532(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8315(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    93
_cell_measurement_reflns_used    23304
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      31.7

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.653
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            57538
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.135
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8117
_reflns_number_gt                7574
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RIGAKU CrystalClear'
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²+42.7860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8117
_refine_ls_number_parameters     590
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.1770
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_restrained_S_all      1.332
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.36500(3) 0.37285(2) 0.57707(2) 0.01725(14) Uani 1 1 d . . . . .
P1 P 0.21670(10) 0.39965(7) 0.56022(6) 0.0145(3) Uani 1 1 d . . . . .
P2 P 0.30464(10) 0.46457(7) 0.67428(6) 0.0177(3) Uani 1 1 d . . . . .
P3 P 0.16088(13) 0.69223(8) 0.76025(7) 0.0282(4) Uani 1 1 d . . . . .
F4 F -0.0041(2) 0.41696(17) 0.54756(14) 0.0274(8) Uani 1 1 d . . . . .
F5 F -0.0135(3) 0.44920(18) 0.62713(15) 0.0354(10) Uani 1 1 d . . . . .
F2 F 0.3238(3) 0.48294(17) 0.50103(15) 0.0317(9) Uani 1 1 d . . . . .
F6 F -0.1067(3) 0.3811(2) 0.60022(18) 0.0428(11) Uani 1 1 d . . . . .
F3 F 0.2347(3) 0.52982(18) 0.44751(18) 0.0440(11) Uani 1 1 d . . . . .
O3 O 0.3406(3) 0.40709(18) 0.65239(15) 0.0191(9) Uani 1 1 d . . . . .
F1 F 0.3483(3) 0.4789(2) 0.41834(16) 0.0452(12) Uani 1 1 d . . . . .
N1 N 0.4946(3) 0.3446(2) 0.60629(19) 0.0187(11) Uani 1 1 d . . . . .
F8 F 0.1785(3) 0.6736(2) 0.70061(17) 0.0489(12) Uani 1 1 d . U . . .
F11 F 0.1449(3) 0.7120(2) 0.81894(18) 0.0544(13) Uani 1 1 d . U . . .
F12 F 0.2678(4) 0.7042(3) 0.7667(2) 0.0748(17) Uani 1 1 d . U . . .
F10 F 0.1433(5) 0.7566(2) 0.7425(2) 0.0808(18) Uani 1 1 d . U . . .
C6 C 0.1845(4) 0.4734(3) 0.5842(2) 0.0172(12) Uani 1 1 d . . . . .
C12 C 0.1796(4) 0.3938(2) 0.4917(2) 0.0155(12) Uani 1 1 d . . . . .
C1 C 0.3853(5) 0.3324(3) 0.5047(3) 0.0307(16) Uani 1 1 d . . . . .
H36 H 0.3336 0.3444 0.4807 0.07(4) Uiso 0.727(8) 1 calc R . P A 1
H37 H 0.3604 0.3573 0.4756 0.11(18) Uiso 0.273(8) 1 calc R . P A 2
C13 C 0.2174(4) 0.4260(3) 0.4495(2) 0.0208(13) Uani 1 1 d . . . . .
F9 F 0.0535(4) 0.6785(3) 0.7522(3) 0.0871(19) Uani 1 1 d . U . . .
C20 C 0.0486(4) 0.3531(3) 0.6156(2) 0.0212(13) Uani 1 1 d . . . . .
C30 C 0.2603(4) 0.4454(3) 0.7407(2) 0.0218(13) Uani 1 1 d . . . . .
C38 C 0.4928(4) 0.3039(3) 0.6443(2) 0.0218(13) Uani 1 1 d . . . . .
H35 H 0.4344 0.2883 0.6548 0.026 Uiso 1 1 calc R U . . .
C19 C 0.1430(4) 0.3486(3) 0.5997(2) 0.0182(12) Uani 1 1 d . . . . .
C37 C 0.5721(5) 0.2838(3) 0.6688(2) 0.0248(14) Uani 1 1 d . . . . .
H34 H 0.5683 0.2550 0.6957 0.030 Uiso 1 1 calc R U . . .
C34 C 0.5775(4) 0.3675(3) 0.5934(3) 0.0277(15) Uani 1 1 d . . . . .
H31 H 0.5800 0.3976 0.5676 0.033 Uiso 1 1 calc R U . . .
C36 C 0.6565(5) 0.3060(3) 0.6536(3) 0.0307(16) Uani 1 1 d . . . . .
H33 H 0.7124 0.2917 0.6688 0.037 Uiso 1 1 calc R U . . .
C25 C -0.0176(4) 0.4000(3) 0.5977(3) 0.0281(15) Uani 1 1 d . . . . .
C7 C 0.1254(4) 0.5078(3) 0.5535(3) 0.0244(14) Uani 1 1 d . . . . .
H1 H 0.1094 0.4944 0.5194 0.029 Uiso 1 1 calc R U . . .
C17 C 0.1222(4) 0.3462(3) 0.4791(2) 0.0186(12) Uani 1 1 d . . . . .
H8 H 0.0955 0.3236 0.5066 0.022 Uiso 1 1 calc R U . . .
C24 C 0.1940(4) 0.3010(3) 0.6195(2) 0.0223(13) Uani 1 1 d . . . . .
H12 H 0.2567 0.2960 0.6086 0.027 Uiso 1 1 calc R U . . .
C11 C 0.2112(4) 0.4953(3) 0.6344(2) 0.0193(12) Uani 1 1 d . . . . .
C14 C 0.1980(5) 0.4099(3) 0.3981(2) 0.0285(15) Uani 1 1 d . . . . .
H5 H 0.2242 0.4321 0.3702 0.034 Uiso 1 1 calc R U . . .
C32 C 0.2503(5) 0.4963(3) 0.7792(3) 0.0365(18) Uani 1 1 d . . . . .
H25 H 0.2129 0.5277 0.7632 0.055 Uiso 1 1 calc R U . . .
H26 H 0.3121 0.5117 0.7880 0.055 Uiso 1 1 calc R U . . .
H27 H 0.2195 0.4824 0.8111 0.055 Uiso 1 1 calc R U . . .
C35 C 0.6591(4) 0.3491(3) 0.6161(3) 0.0362(18) Uani 1 1 d . . . . .
H32 H 0.7168 0.3661 0.6060 0.043 Uiso 1 1 calc R U . . .
C21 C 0.0125(5) 0.3132(3) 0.6511(2) 0.0293(16) Uani 1 1 d . . . . .
H9 H -0.0504 0.3171 0.6620 0.035 Uiso 1 1 calc R U . . .
C16 C 0.1030(4) 0.3309(3) 0.4275(2) 0.0241(14) Uani 1 1 d . . . . .
H7 H 0.0631 0.2984 0.4204 0.029 Uiso 1 1 calc R U . . .
C26 C 0.3989(4) 0.5204(3) 0.6717(3) 0.0257(14) Uani 1 1 d . . . . .
C23 C 0.1561(5) 0.2610(3) 0.6544(3) 0.0312(16) Uani 1 1 d . . . . .
H11 H 0.1924 0.2290 0.6669 0.037 Uiso 1 1 calc R U . . .
C15 C 0.1413(5) 0.3622(3) 0.3868(3) 0.0320(16) Uani 1 1 d . . . . .
H6 H 0.1291 0.3514 0.3515 0.038 Uiso 1 1 calc R U . . .
C33 C 0.1660(4) 0.4150(3) 0.7321(2) 0.0264(14) Uani 1 1 d . . . . .
H28 H 0.1416 0.4012 0.7658 0.040 Uiso 1 1 calc R U . . .
H29 H 0.1741 0.3814 0.7085 0.040 Uiso 1 1 calc R U . . .
H30 H 0.1221 0.4431 0.7165 0.040 Uiso 1 1 calc R U . . .
C10 C 0.1710(5) 0.5469(3) 0.6522(3) 0.0288(15) Uani 1 1 d . . . . .
H4 H 0.1861 0.5608 0.6862 0.035 Uiso 1 1 calc R U . . .
C29 C 0.3755(5) 0.5827(3) 0.6905(3) 0.0346(17) Uani 1 1 d . . . . .
H19 H 0.4325 0.6064 0.6918 0.052 Uiso 1 1 calc R U . . .
H20 H 0.3479 0.5807 0.7256 0.052 Uiso 1 1 calc R U . . .
H21 H 0.3311 0.6010 0.6663 0.052 Uiso 1 1 calc R U . . .
C18 C 0.2811(5) 0.4788(3) 0.4543(3) 0.0309(16) Uani 1 1 d . . . . .
O2 O 0.2830(5) 0.2514(3) 0.5118(3) 0.042(2) Uani 0.727(8) 1 d . . P A 1
C31 C 0.3275(5) 0.3999(3) 0.7643(3) 0.0341(16) Uani 1 1 d . . . . .
H22 H 0.3896 0.4173 0.7676 0.051 Uiso 1 1 calc R U . . .
H23 H 0.3306 0.3652 0.7414 0.051 Uiso 1 1 calc R U . . .
H24 H 0.3050 0.3880 0.7990 0.051 Uiso 1 1 calc R U . . .
F7 F 0.1754(6) 0.6263(3) 0.7769(3) 0.097(2) Uani 1 1 d . U . . .
C27 C 0.4284(5) 0.5233(3) 0.6137(3) 0.0343(16) Uani 1 1 d . . . . .
H13 H 0.3755 0.5362 0.5924 0.051 Uiso 1 1 calc R U . . .
H14 H 0.4487 0.4841 0.6021 0.051 Uiso 1 1 calc R U . . .
H15 H 0.4798 0.5513 0.6098 0.051 Uiso 1 1 calc R U . . .
C8 C 0.0892(5) 0.5608(3) 0.5709(3) 0.0301(16) Uani 1 1 d . . . . .
H2 H 0.0513 0.5843 0.5487 0.036 Uiso 1 1 calc R U . . .
C9 C 0.1094(5) 0.5790(3) 0.6216(3) 0.0344(17) Uani 1 1 d . . . . .
H3 H 0.0809 0.6135 0.6353 0.041 Uiso 1 1 calc R U . . .
O1 O 0.4335(6) 0.2336(3) 0.5276(3) 0.051(2) Uani 0.727(8) 1 d . . P A 1
C22 C 0.0656(5) 0.2679(3) 0.6711(3) 0.0374(18) Uani 1 1 d . . . . .
H10 H 0.0399 0.2416 0.6962 0.045 Uiso 1 1 calc R U . . .
C28 C 0.4816(5) 0.4966(3) 0.7038(3) 0.0392(18) Uani 1 1 d . . . . .
H16 H 0.5356 0.5225 0.6990 0.059 Uiso 1 1 calc R U . . .
H17 H 0.4972 0.4567 0.6919 0.059 Uiso 1 1 calc R U . . .
H18 H 0.4647 0.4955 0.7410 0.059 Uiso 1 1 calc R U . . .
C4 C 0.3744(10) 0.2678(7) 0.5174(5) 0.044(4) Uani 0.727(8) 1 d . U P A 1
C2 C 0.4755(10) 0.3471(7) 0.4791(6) 0.046(3) Uani 0.727(8) 1 d . U P A 1
H38 H 0.5269 0.3294 0.4996 0.055 Uiso 0.727(8) 1 calc R U P A 1
H39 H 0.4840 0.3904 0.4794 0.055 Uiso 0.727(8) 1 calc R U P A 1
C3 C 0.4812(9) 0.3252(5) 0.4234(4) 0.047(3) Uani 0.727(8) 1 d . . P A 1
H40 H 0.4777 0.2820 0.4231 0.071 Uiso 0.727(8) 1 calc R U P A 1
H41 H 0.5403 0.3378 0.4078 0.071 Uiso 0.727(8) 1 calc R U P A 1
H42 H 0.4293 0.3415 0.4031 0.071 Uiso 0.727(8) 1 calc R U P A 1
C5 C 0.2655(10) 0.1903(5) 0.5252(6) 0.060(4) Uani 0.727(8) 1 d . . P A 1
H46 H 0.2966 0.1646 0.4998 0.091 Uiso 0.727(8) 1 calc R U P A 1
H47 H 0.1984 0.1827 0.5246 0.091 Uiso 0.727(8) 1 calc R U P A 1
H48 H 0.2899 0.1823 0.5604 0.091 Uiso 0.727(8) 1 calc R U P A 1
O4 O 0.5171(17) 0.2686(9) 0.5056(9) 0.057(7) Uani 0.273(8) 1 d . . P A 2
O5 O 0.528(2) 0.3662(11) 0.4801(9) 0.056(7) Uani 0.273(8) 1 d . . P A 2
C40 C 0.332(3) 0.2464(18) 0.4495(14) 0.075(12) Uani 0.273(8) 1 d D U P A 2
H49 H 0.3059 0.2763 0.4258 0.112 Uiso 0.273(8) 1 calc R U P A 2
H50 H 0.2903 0.2121 0.4503 0.112 Uiso 0.273(8) 1 calc R U P A 2
H51 H 0.3934 0.2344 0.4371 0.112 Uiso 0.273(8) 1 calc R U P A 2
C42 C 0.633(3) 0.354(2) 0.4668(17) 0.080(13) Uani 0.273(8) 1 d . . P A 2
H43 H 0.6634 0.3355 0.4972 0.121 Uiso 0.273(8) 1 calc R U P A 2
H44 H 0.6643 0.3908 0.4582 0.121 Uiso 0.273(8) 1 calc R U P A 2
H45 H 0.6367 0.3268 0.4368 0.121 Uiso 0.273(8) 1 calc R U P A 2
C41 C 0.485(3) 0.3161(19) 0.4951(14) 0.048(9) Uani 0.273(8) 1 d . U P A 2
C39 C 0.340(3) 0.2725(18) 0.5051(13) 0.039(8) Uani 0.273(8) 1 d D U P A 2
H52 H 0.2771 0.2758 0.5207 0.047 Uiso 0.273(8) 1 calc R U P A 2
H53 H 0.3771 0.2454 0.5272 0.047 Uiso 0.273(8) 1 calc R U P A 2


_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 C1 2.085(7) . ?
Pd1 O3 2.103(4) . ?
Pd1 N1 2.105(5) . ?
Pd1 P1 2.2561(15) . ?
P1 C12 1.834(6) . ?
P1 C6 1.840(6) . ?
P1 C19 1.864(6) . ?
P2 O3 1.510(4) . ?
P2 C11 1.822(6) . ?
P2 C26 1.855(7) . ?
P2 C30 1.863(6) . ?
P3 F10 1.549(5) . ?
P3 F12 1.568(5) . ?
P3 F7 1.568(6) . ?
P3 F11 1.581(5) . ?
P3 F9 1.587(6) . ?
P3 F8 1.600(5) . ?
F4 C25 1.351(7) . ?
F5 C25 1.347(8) . ?
F2 C18 1.345(8) . ?
F6 C25 1.352(7) . ?
F3 C18 1.346(8) . ?
F1 C18 1.332(8) . ?
N1 C38 1.340(8) . ?
N1 C34 1.340(8) . ?
C6 C7 1.395(8) . ?
C6 C11 1.427(8) . ?
C12 C17 1.396(8) . ?
C12 C13 1.410(8) . ?
C1 C2 1.488(15) . ?
C1 C41 1.50(4) . ?
C1 C39 1.51(4) . ?
C1 C4 1.508(18) . ?
C1 H36 1.0000 . ?
C1 H37 1.0000 . ?
C13 C14 1.390(8) . ?
C13 C18 1.511(9) . ?
C20 C21 1.381(9) . ?
C20 C19 1.419(8) . ?
C20 C25 1.498(9) . ?
C30 C32 1.522(9) . ?
C30 C33 1.536(9) . ?
C30 C31 1.537(9) . ?
C38 C37 1.376(9) . ?
C38 H35 0.9500 . ?
C19 C24 1.399(8) . ?
C37 C36 1.369(10) . ?
C37 H34 0.9500 . ?
C34 C35 1.373(9) . ?
C34 H31 0.9500 . ?
C36 C35 1.367(10) . ?
C36 H33 0.9500 . ?
C7 C8 1.383(9) . ?
C7 H1 0.9500 . ?
C17 C16 1.389(8) . ?
C17 H8 0.9500 . ?
C24 C23 1.383(9) . ?
C24 H12 0.9500 . ?
C11 C10 1.383(9) . ?
C14 C15 1.384(10) . ?
C14 H5 0.9500 . ?
C32 H25 0.9800 . ?
C32 H26 0.9800 . ?
C32 H27 0.9800 . ?
C35 H32 0.9500 . ?
C21 C22 1.376(10) . ?
C21 H9 0.9500 . ?
C16 C15 1.375(9) . ?
C16 H7 0.9500 . ?
C26 C29 1.531(9) . ?
C26 C27 1.540(10) . ?
C26 C28 1.541(9) . ?
C23 C22 1.377(10) . ?
C23 H11 0.9500 . ?
C15 H6 0.9500 . ?
C33 H28 0.9800 . ?
C33 H29 0.9800 . ?
C33 H30 0.9800 . ?
C10 C9 1.387(9) . ?
C10 H4 0.9500 . ?
C29 H19 0.9800 . ?
C29 H20 0.9800 . ?
C29 H21 0.9800 . ?
O2 C4 1.373(17) . ?
O2 C5 1.449(13) . ?
C31 H22 0.9800 . ?
C31 H23 0.9800 . ?
C31 H24 0.9800 . ?
C27 H13 0.9800 . ?
C27 H14 0.9800 . ?
C27 H15 0.9800 . ?
C8 C9 1.388(9) . ?
C8 H2 0.9500 . ?
C9 H3 0.9500 . ?
O1 C4 1.178(14) . ?
C22 H10 0.9500 . ?
C28 H16 0.9800 . ?
C28 H17 0.9800 . ?
C28 H18 0.9800 . ?
C2 C3 1.508(16) . ?
C2 H38 0.9900 . ?
C2 H39 0.9900 . ?
C3 H40 0.9800 . ?
C3 H41 0.9800 . ?
C3 H42 0.9800 . ?
C5 H46 0.9800 . ?
C5 H47 0.9800 . ?
C5 H48 0.9800 . ?
O4 C41 1.20(5) . ?
O5 C41 1.35(4) . ?
O5 C42 1.57(5) . ?
C40 C39 1.54(4) . ?
C40 H49 0.9800 . ?
C40 H50 0.9800 . ?
C40 H51 0.9800 . ?
C42 H43 0.9800 . ?
C42 H44 0.9800 . ?
C42 H45 0.9800 . ?
C39 H52 0.9900 . ?
C39 H53 0.9900 . ?

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
C1 Pd1 O3 175.4(2) . . ?
C1 Pd1 N1 93.2(2) . . ?
O3 Pd1 N1 86.31(17) . . ?
C1 Pd1 P1 94.7(2) . . ?
O3 Pd1 P1 85.28(11) . . ?
N1 Pd1 P1 169.81(14) . . ?
C12 P1 C6 108.0(3) . . ?
C12 P1 C19 107.9(3) . . ?
C6 P1 C19 104.0(3) . . ?
C12 P1 Pd1 115.89(18) . . ?
C6 P1 Pd1 114.8(2) . . ?
C19 P1 Pd1 105.40(19) . . ?
O3 P2 C11 112.0(3) . . ?
O3 P2 C26 109.0(3) . . ?
C11 P2 C26 104.9(3) . . ?
O3 P2 C30 104.6(3) . . ?
C11 P2 C30 110.2(3) . . ?
C26 P2 C30 116.2(3) . . ?
F10 P3 F12 91.5(4) . . ?
F10 P3 F7 177.8(4) . . ?
F12 P3 F7 90.4(4) . . ?
F10 P3 F11 89.2(3) . . ?
F12 P3 F11 89.6(3) . . ?
F7 P3 F11 91.9(3) . . ?
F10 P3 F9 89.4(4) . . ?
F12 P3 F9 178.0(3) . . ?
F7 P3 F9 88.7(4) . . ?
F11 P3 F9 92.1(3) . . ?
F10 P3 F8 89.8(3) . . ?
F12 P3 F8 89.5(3) . . ?
F7 P3 F8 89.1(3) . . ?
F11 P3 F8 178.6(3) . . ?
F9 P3 F8 88.8(3) . . ?
P2 O3 Pd1 135.6(2) . . ?
C38 N1 C34 117.5(5) . . ?
C38 N1 Pd1 116.7(4) . . ?
C34 N1 Pd1 125.5(4) . . ?
C7 C6 C11 118.4(5) . . ?
C7 C6 P1 118.3(4) . . ?
C11 C6 P1 123.1(4) . . ?
C17 C12 C13 116.8(5) . . ?
C17 C12 P1 116.6(4) . . ?
C13 C12 P1 125.5(4) . . ?
C41 C1 C39 101(2) . . ?
C2 C1 C4 113.7(9) . . ?
C2 C1 Pd1 114.4(7) . . ?
C41 C1 Pd1 112.7(14) . . ?
C39 C1 Pd1 109.3(13) . . ?
C4 C1 Pd1 102.8(6) . . ?
C2 C1 H36 108.6 . . ?
C4 C1 H36 108.6 . . ?
Pd1 C1 H36 108.6 . . ?
C41 C1 H37 111.1 . . ?
C39 C1 H37 111.1 . . ?
Pd1 C1 H37 111.1 . . ?
C14 C13 C12 120.6(6) . . ?
C14 C13 C18 113.9(6) . . ?
C12 C13 C18 125.5(6) . . ?
C21 C20 C19 120.0(6) . . ?
C21 C20 C25 115.3(6) . . ?
C19 C20 C25 124.7(6) . . ?
C32 C30 C33 110.5(5) . . ?
C32 C30 C31 108.4(5) . . ?
C33 C30 C31 107.9(5) . . ?
C32 C30 P2 116.3(5) . . ?
C33 C30 P2 106.0(4) . . ?
C31 C30 P2 107.4(4) . . ?
N1 C38 C37 122.8(6) . . ?
N1 C38 H35 118.6 . . ?
C37 C38 H35 118.6 . . ?
C24 C19 C20 116.8(6) . . ?
C24 C19 P1 112.2(4) . . ?
C20 C19 P1 130.8(5) . . ?
C36 C37 C38 118.8(6) . . ?
C36 C37 H34 120.6 . . ?
C38 C37 H34 120.6 . . ?
N1 C34 C35 122.4(6) . . ?
N1 C34 H31 118.8 . . ?
C35 C34 H31 118.8 . . ?
C35 C36 C37 119.1(6) . . ?
C35 C36 H33 120.5 . . ?
C37 C36 H33 120.5 . . ?
F5 C25 F4 106.6(6) . . ?
F5 C25 F6 106.1(5) . . ?
F4 C25 F6 105.7(5) . . ?
F5 C25 C20 113.0(5) . . ?
F4 C25 C20 113.6(5) . . ?
F6 C25 C20 111.2(6) . . ?
C8 C7 C6 122.2(6) . . ?
C8 C7 H1 118.9 . . ?
C6 C7 H1 118.9 . . ?
C16 C17 C12 122.0(6) . . ?
C16 C17 H8 119.0 . . ?
C12 C17 H8 119.0 . . ?
C23 C24 C19 122.2(6) . . ?
C23 C24 H12 118.9 . . ?
C19 C24 H12 118.9 . . ?
C10 C11 C6 118.4(5) . . ?
C10 C11 P2 116.6(5) . . ?
C6 C11 P2 124.6(4) . . ?
C15 C14 C13 121.3(6) . . ?
C15 C14 H5 119.3 . . ?
C13 C14 H5 119.3 . . ?
C30 C32 H25 109.5 . . ?
C30 C32 H26 109.5 . . ?
H25 C32 H26 109.5 . . ?
C30 C32 H27 109.5 . . ?
H25 C32 H27 109.5 . . ?
H26 C32 H27 109.5 . . ?
C36 C35 C34 119.3(6) . . ?
C36 C35 H32 120.3 . . ?
C34 C35 H32 120.3 . . ?
C22 C21 C20 121.6(6) . . ?
C22 C21 H9 119.2 . . ?
C20 C21 H9 119.2 . . ?
C15 C16 C17 120.5(6) . . ?
C15 C16 H7 119.8 . . ?
C17 C16 H7 119.8 . . ?
C29 C26 C27 108.9(6) . . ?
C29 C26 C28 109.0(6) . . ?
C27 C26 C28 108.3(6) . . ?
C29 C26 P2 117.3(5) . . ?
C27 C26 P2 105.3(4) . . ?
C28 C26 P2 107.7(5) . . ?
C22 C23 C24 119.7(7) . . ?
C22 C23 H11 120.1 . . ?
C24 C23 H11 120.1 . . ?
C16 C15 C14 118.8(6) . . ?
C16 C15 H6 120.6 . . ?
C14 C15 H6 120.6 . . ?
C30 C33 H28 109.5 . . ?
C30 C33 H29 109.5 . . ?
H28 C33 H29 109.5 . . ?
C30 C33 H30 109.5 . . ?
H28 C33 H30 109.5 . . ?
H29 C33 H30 109.5 . . ?
C11 C10 C9 121.8(6) . . ?
C11 C10 H4 119.1 . . ?
C9 C10 H4 119.1 . . ?
C26 C29 H19 109.5 . . ?
C26 C29 H20 109.5 . . ?
H19 C29 H20 109.5 . . ?
C26 C29 H21 109.5 . . ?
H19 C29 H21 109.5 . . ?
H20 C29 H21 109.5 . . ?
F1 C18 F2 106.3(6) . . ?
F1 C18 F3 105.5(5) . . ?
F2 C18 F3 106.3(6) . . ?
F1 C18 C13 112.6(6) . . ?
F2 C18 C13 113.8(5) . . ?
F3 C18 C13 111.8(5) . . ?
C4 O2 C5 113.6(10) . . ?
C30 C31 H22 109.5 . . ?
C30 C31 H23 109.5 . . ?
H22 C31 H23 109.5 . . ?
C30 C31 H24 109.5 . . ?
H22 C31 H24 109.5 . . ?
H23 C31 H24 109.5 . . ?
C26 C27 H13 109.5 . . ?
C26 C27 H14 109.5 . . ?
H13 C27 H14 109.5 . . ?
C26 C27 H15 109.5 . . ?
H13 C27 H15 109.5 . . ?
H14 C27 H15 109.5 . . ?
C7 C8 C9 118.7(6) . . ?
C7 C8 H2 120.6 . . ?
C9 C8 H2 120.6 . . ?
C10 C9 C8 120.1(6) . . ?
C10 C9 H3 119.9 . . ?
C8 C9 H3 119.9 . . ?
C21 C22 C23 119.5(7) . . ?
C21 C22 H10 120.2 . . ?
C23 C22 H10 120.2 . . ?
C26 C28 H16 109.5 . . ?
C26 C28 H17 109.5 . . ?
H16 C28 H17 109.5 . . ?
C26 C28 H18 109.5 . . ?
H16 C28 H18 109.5 . . ?
H17 C28 H18 109.5 . . ?
O1 C4 O2 122.2(14) . . ?
O1 C4 C1 127.7(14) . . ?
O2 C4 C1 109.9(9) . . ?
C1 C2 C3 112.8(10) . . ?
C1 C2 H38 109.0 . . ?
C3 C2 H38 109.0 . . ?
C1 C2 H39 109.0 . . ?
C3 C2 H39 109.0 . . ?
H38 C2 H39 107.8 . . ?
C2 C3 H40 109.5 . . ?
C2 C3 H41 109.5 . . ?
H40 C3 H41 109.5 . . ?
C2 C3 H42 109.5 . . ?
H40 C3 H42 109.5 . . ?
H41 C3 H42 109.5 . . ?
O2 C5 H46 109.5 . . ?
O2 C5 H47 109.5 . . ?
H46 C5 H47 109.5 . . ?
O2 C5 H48 109.5 . . ?
H46 C5 H48 109.5 . . ?
H47 C5 H48 109.5 . . ?
C41 O5 C42 110(3) . . ?
C39 C40 H49 109.5 . . ?
C39 C40 H50 109.5 . . ?
H49 C40 H50 109.5 . . ?
C39 C40 H51 109.5 . . ?
H49 C40 H51 109.5 . . ?
H50 C40 H51 109.5 . . ?
O5 C42 H43 109.5 . . ?
O5 C42 H44 109.5 . . ?
H43 C42 H44 109.5 . . ?
O5 C42 H45 109.5 . . ?
H43 C42 H45 109.5 . . ?
H44 C42 H45 109.5 . . ?
O4 C41 O5 130(4) . . ?
O4 C41 C1 123(3) . . ?
O5 C41 C1 106(3) . . ?
C1 C39 C40 112(3) . . ?
C1 C39 H52 109.2 . . ?
C40 C39 H52 109.2 . . ?
C1 C39 H53 109.2 . . ?
C40 C39 H53 109.2 . . ?
H52 C39 H53 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 P2 O3 Pd1 37.5(4) . . . . ?
C26 P2 O3 Pd1 -78.2(4) . . . . ?
C30 P2 O3 Pd1 156.9(3) . . . . ?
C12 P1 C6 C7 11.5(6) . . . . ?
C19 P1 C6 C7 -103.0(5) . . . . ?
Pd1 P1 C6 C7 142.4(4) . . . . ?
C12 P1 C6 C11 -173.4(5) . . . . ?
C19 P1 C6 C11 72.1(5) . . . . ?
Pd1 P1 C6 C11 -42.5(5) . . . . ?
C6 P1 C12 C17 -125.4(4) . . . . ?
C19 P1 C12 C17 -13.6(5) . . . . ?
Pd1 P1 C12 C17 104.2(4) . . . . ?
C6 P1 C12 C13 67.2(5) . . . . ?
C19 P1 C12 C13 179.1(5) . . . . ?
Pd1 P1 C12 C13 -63.1(5) . . . . ?
C17 C12 C13 C14 -0.5(9) . . . . ?
P1 C12 C13 C14 166.8(5) . . . . ?
C17 C12 C13 C18 -179.8(6) . . . . ?
P1 C12 C13 C18 -12.5(9) . . . . ?
O3 P2 C30 C32 159.8(5) . . . . ?
C11 P2 C30 C32 -79.6(5) . . . . ?
C26 P2 C30 C32 39.5(6) . . . . ?
O3 P2 C30 C33 -77.0(4) . . . . ?
C11 P2 C30 C33 43.6(5) . . . . ?
C26 P2 C30 C33 162.7(4) . . . . ?
O3 P2 C30 C31 38.1(5) . . . . ?
C11 P2 C30 C31 158.8(4) . . . . ?
C26 P2 C30 C31 -82.1(5) . . . . ?
C34 N1 C38 C37 -2.3(9) . . . . ?
Pd1 N1 C38 C37 -176.6(5) . . . . ?
C21 C20 C19 C24 3.2(9) . . . . ?
C25 C20 C19 C24 -178.5(6) . . . . ?
C21 C20 C19 P1 -171.0(5) . . . . ?
C25 C20 C19 P1 7.3(9) . . . . ?
C12 P1 C19 C24 111.7(5) . . . . ?
C6 P1 C19 C24 -133.8(4) . . . . ?
Pd1 P1 C19 C24 -12.7(5) . . . . ?
C12 P1 C19 C20 -73.9(6) . . . . ?
C6 P1 C19 C20 40.6(6) . . . . ?
Pd1 P1 C19 C20 161.7(5) . . . . ?
N1 C38 C37 C36 -0.3(9) . . . . ?
C38 N1 C34 C35 2.6(10) . . . . ?
Pd1 N1 C34 C35 176.3(5) . . . . ?
C38 C37 C36 C35 2.6(10) . . . . ?
C21 C20 C25 F5 91.8(7) . . . . ?
C19 C20 C25 F5 -86.6(7) . . . . ?
C21 C20 C25 F4 -146.5(6) . . . . ?
C19 C20 C25 F4 35.1(9) . . . . ?
C21 C20 C25 F6 -27.4(8) . . . . ?
C19 C20 C25 F6 154.3(6) . . . . ?
C11 C6 C7 C8 -2.8(10) . . . . ?
P1 C6 C7 C8 172.6(5) . . . . ?
C13 C12 C17 C16 0.1(8) . . . . ?
P1 C12 C17 C16 -168.3(5) . . . . ?
C20 C19 C24 C23 -2.3(9) . . . . ?
P1 C19 C24 C23 172.9(5) . . . . ?
C7 C6 C11 C10 5.6(9) . . . . ?
P1 C6 C11 C10 -169.5(5) . . . . ?
C7 C6 C11 P2 -167.2(5) . . . . ?
P1 C6 C11 P2 17.7(8) . . . . ?
O3 P2 C11 C10 177.7(5) . . . . ?
C26 P2 C11 C10 -64.2(6) . . . . ?
C30 P2 C11 C10 61.6(6) . . . . ?
O3 P2 C11 C6 -9.4(6) . . . . ?
C26 P2 C11 C6 108.7(5) . . . . ?
C30 P2 C11 C6 -125.5(5) . . . . ?
C12 C13 C14 C15 0.2(10) . . . . ?
C18 C13 C14 C15 179.5(6) . . . . ?
C37 C36 C35 C34 -2.3(11) . . . . ?
N1 C34 C35 C36 -0.3(11) . . . . ?
C19 C20 C21 C22 -1.3(10) . . . . ?
C25 C20 C21 C22 -179.7(6) . . . . ?
C12 C17 C16 C15 0.7(10) . . . . ?
O3 P2 C26 C29 178.1(5) . . . . ?
C11 P2 C26 C29 57.9(6) . . . . ?
C30 P2 C26 C29 -64.0(6) . . . . ?
O3 P2 C26 C27 56.8(5) . . . . ?
C11 P2 C26 C27 -63.3(5) . . . . ?
C30 P2 C26 C27 174.7(4) . . . . ?
O3 P2 C26 C28 -58.7(5) . . . . ?
C11 P2 C26 C28 -178.8(5) . . . . ?
C30 P2 C26 C28 59.2(6) . . . . ?
C19 C24 C23 C22 -0.6(10) . . . . ?
C17 C16 C15 C14 -1.1(10) . . . . ?
C13 C14 C15 C16 0.7(11) . . . . ?
C6 C11 C10 C9 -3.1(10) . . . . ?
P2 C11 C10 C9 170.3(6) . . . . ?
C14 C13 C18 F1 -38.4(8) . . . . ?
C12 C13 C18 F1 140.9(6) . . . . ?
C14 C13 C18 F2 -159.5(6) . . . . ?
C12 C13 C18 F2 19.9(9) . . . . ?
C14 C13 C18 F3 80.1(7) . . . . ?
C12 C13 C18 F3 -100.5(7) . . . . ?
C6 C7 C8 C9 -2.8(11) . . . . ?
C11 C10 C9 C8 -2.5(12) . . . . ?
C7 C8 C9 C10 5.4(11) . . . . ?
C20 C21 C22 C23 -1.7(11) . . . . ?
C24 C23 C22 C21 2.6(11) . . . . ?
C5 O2 C4 O1 6.5(18) . . . . ?
C5 O2 C4 C1 -177.8(9) . . . . ?
C2 C1 C4 O1 29.8(18) . . . . ?
Pd1 C1 C4 O1 -94.4(14) . . . . ?
C2 C1 C4 O2 -145.6(10) . . . . ?
Pd1 C1 C4 O2 90.2(9) . . . . ?
C4 C1 C2 C3 71.6(14) . . . . ?
Pd1 C1 C2 C3 -170.7(9) . . . . ?
C42 O5 C41 O4 11(5) . . . . ?
C42 O5 C41 C1 -178(2) . . . . ?
C39 C1 C41 O4 -24(4) . . . . ?
Pd1 C1 C41 O4 93(3) . . . . ?
C39 C1 C41 O5 164(2) . . . . ?
Pd1 C1 C41 O5 -80(3) . . . . ?
C41 C1 C39 C40 -75(3) . . . . ?
Pd1 C1 C39 C40 166(2) . . . . ?

_refine_diff_density_max         1.281
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.134

_shelxl_version_number           2014/6

