#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305997.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4305997
loop_
_publ_author_name
'Roberto Pattacini'
'Günter Margraf'
'Abdelatif Messaoudi'
'Nicola Oberbeckmann-Winter'
'Pierre Braunstein'
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
CNRS-Université Louis Pasteur
Institut Le Bel - 4 rue Blaise Pascal
67070 Strasbourg Cedex - France
;
_publ_contact_author_email       braunst@chimie.u-strasbg.fr
_publ_contact_author_fax         +33(0)390241322
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       +33(0)390241308
_publ_section_title
;
Formation of P-C Bonds under Unexpectedly Mild Conditions. Phosphoryl
Migration and Metal Coordination of Diphenylphosphinomethyl-oxazolines and
-thiazolines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9886
_journal_page_last               9897
_journal_paper_doi               10.1021/ic800934h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'4(C25 H28 N2 P Pd S), 4(C F3 O3 S), C4 H10 O '
_chemical_formula_sum            'C54 H61 F6 N4 O6.5 P2 Pd2 S4'
_chemical_formula_weight         1387.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.3772(4)
_cell_angle_beta                 92.9540(4)
_cell_angle_gamma                107.7705(7)
_cell_formula_units_Z            2
_cell_length_a                   9.6076(1)
_cell_length_b                   12.7675(1)
_cell_length_c                   25.3804(4)
_cell_measurement_reflns_used    27216
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2934.37(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31900
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12127
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/
   [σ²(Fo²)+0.0000+0.1311*P+(0.0796P)²+1.0000sinθ/λ]
 where P = 0.33333Fo² + 0.66667Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                9078
_reflns_number_total             12127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800934h_si_001_6.cif
_cod_data_source_block           Compound8
_cod_original_cell_volume        2934.367(61)
_cod_original_formula_sum        'C54 H61 F6 N4 O6.50 P2 Pd2 S4'
_cod_database_code               4305997
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1A Pd 0.69979(3) 0.86237(2) 0.821476(11) 0.02803(10) Uani 1 1 d . . .
P1A P 0.81164(10) 0.87354(8) 0.90155(4) 0.0256(2) Uani 1 1 d . . .
N1A N 0.9220(3) 0.9396(3) 0.80281(13) 0.0323(8) Uani 1 1 d . . .
N2A N 0.5708(4) 0.8499(3) 0.74681(14) 0.0393(9) Uani 1 1 d . . .
S1A S 1.19879(11) 1.04917(10) 0.82576(5) 0.0444(3) Uani 1 1 d . . .
C1A C 0.9766(5) 0.9638(4) 0.75124(17) 0.0480(12) Uani 1 1 d . . .
H1A1 H 0.9232 1.0093 0.7351 0.058 Uiso 1 1 calc R . .
H1A2 H 0.9566 0.8934 0.7272 0.058 Uiso 1 1 calc R . .
C2A C 1.1361(5) 1.0240(5) 0.7563(2) 0.0650(16) Uani 1 1 d . . .
H2A1 H 1.1548 1.0951 0.7415 0.078 Uiso 1 1 calc R . .
H2A2 H 1.1886 0.9788 0.7364 0.078 Uiso 1 1 calc R . .
C3A C 1.0220(4) 0.9792(3) 0.84110(15) 0.0289(8) Uani 1 1 d . . .
C4A C 0.9940(4) 0.9720(3) 0.89749(15) 0.0311(9) Uani 1 1 d . . .
H4A1 H 0.9995 1.0460 0.9156 0.037 Uiso 1 1 calc R . .
H4A2 H 1.0696 0.9470 0.9156 0.037 Uiso 1 1 calc R . .
C5A C 0.5013(4) 0.7921(3) 0.84455(16) 0.0319(9) Uani 1 1 d . . .
C6A C 0.4580(4) 0.7294(3) 0.88584(17) 0.0360(10) Uani 1 1 d . . .
H6A H 0.5307 0.7167 0.9088 0.043 Uiso 1 1 calc R . .
C7A C 0.3104(4) 0.6847(4) 0.89424(19) 0.0455(11) Uani 1 1 d . . .
H7A H 0.2839 0.6415 0.9224 0.055 Uiso 1 1 calc R . .
C8A C 0.2022(5) 0.7030(4) 0.8617(2) 0.0562(14) Uani 1 1 d . . .
H8A H 0.1019 0.6738 0.8679 0.067 Uiso 1 1 calc R . .
C9A C 0.2418(5) 0.7638(4) 0.8207(2) 0.0507(13) Uani 1 1 d . . .
H9A H 0.1679 0.7765 0.7983 0.061 Uiso 1 1 calc R . .
C10A C 0.3884(4) 0.8073(4) 0.81116(18) 0.0413(10) Uani 1 1 d . . .
C11A C 0.4353(5) 0.8699(4) 0.7662(2) 0.0497(12) Uani 1 1 d . . .
H11A H 0.4553 0.9502 0.7778 0.060 Uiso 1 1 calc R . .
H11B H 0.3557 0.8463 0.7369 0.060 Uiso 1 1 calc R . .
C12A C 0.5313(6) 0.7360(4) 0.71848(18) 0.0504(12) Uani 1 1 d . . .
H12A H 0.4869 0.6828 0.7426 0.076 Uiso 1 1 calc R . .
H12B H 0.6197 0.7217 0.7063 0.076 Uiso 1 1 calc R . .
H12C H 0.4610 0.7279 0.6877 0.076 Uiso 1 1 calc R . .
C13A C 0.6302(6) 0.9281(4) 0.7083(2) 0.0597(15) Uani 1 1 d . . .
H13A H 0.7073 0.9067 0.6905 0.090 Uiso 1 1 calc R . .
H13B H 0.6713 1.0035 0.7273 0.090 Uiso 1 1 calc R . .
H13C H 0.5512 0.9257 0.6818 0.090 Uiso 1 1 calc R . .
C14A C 0.8439(4) 0.7468(3) 0.91585(16) 0.0320(9) Uani 1 1 d . . .
C15A C 0.9247(5) 0.7420(4) 0.96150(18) 0.0420(11) Uani 1 1 d . . .
H15A H 0.9617 0.8060 0.9873 0.050 Uiso 1 1 calc R . .
C16A C 0.9523(5) 0.6449(5) 0.9700(2) 0.0601(15) Uani 1 1 d . . .
H16A H 1.0087 0.6422 1.0014 0.072 Uiso 1 1 calc R . .
C17A C 0.8979(6) 0.5522(4) 0.9328(2) 0.0622(15) Uani 1 1 d . . .
H17A H 0.9177 0.4857 0.9387 0.075 Uiso 1 1 calc R . .
C18A C 0.8156(5) 0.5538(4) 0.8873(2) 0.0524(13) Uani 1 1 d . . .
H18A H 0.7773 0.4887 0.8622 0.063 Uiso 1 1 calc R . .
C19A C 0.7886(4) 0.6508(3) 0.87808(18) 0.0374(10) Uani 1 1 d . . .
H19A H 0.7330 0.6529 0.8464 0.045 Uiso 1 1 calc R . .
C20A C 0.7476(4) 0.9295(3) 0.96114(15) 0.0292(9) Uani 1 1 d . . .
C21A C 0.7535(4) 1.0411(3) 0.96646(16) 0.0337(9) Uani 1 1 d . . .
H21A H 0.7927 1.0862 0.9400 0.040 Uiso 1 1 calc R . .
C22A C 0.7011(4) 1.0851(4) 1.01105(17) 0.0390(10) Uani 1 1 d . . .
H22A H 0.7061 1.1611 1.0153 0.047 Uiso 1 1 calc R . .
C23A C 0.6420(4) 1.0194(4) 1.04931(17) 0.0392(10) Uani 1 1 d . . .
H23A H 0.6067 1.0504 1.0796 0.047 Uiso 1 1 calc R . .
C24A C 0.6343(4) 0.9098(4) 1.04363(16) 0.0398(10) Uani 1 1 d . . .
H24A H 0.5929 0.8649 1.0699 0.048 Uiso 1 1 calc R . .
C25A C 0.6865(4) 0.8641(4) 0.99993(16) 0.0347(9) Uani 1 1 d . . .
H25A H 0.6807 0.7880 0.9963 0.042 Uiso 1 1 calc R . .
Pd1B Pd 0.48247(3) 0.30108(2) 0.580003(11) 0.02811(10) Uani 1 1 d . . .
P1B P 0.55569(11) 0.34613(8) 0.66637(4) 0.0281(2) Uani 1 1 d . . .
N1B N 0.6467(4) 0.2188(3) 0.58626(13) 0.0331(8) Uani 1 1 d . . .
N2B N 0.3969(4) 0.2468(3) 0.49813(13) 0.0370(8) Uani 1 1 d . . .
S1B S 0.82940(14) 0.14659(12) 0.63909(5) 0.0521(3) Uani 1 1 d . . .
C1B C 0.7363(6) 0.1901(5) 0.54601(19) 0.0612(15) Uani 1 1 d . . .
H1B1 H 0.7677 0.2510 0.5239 0.073 Uiso 1 1 calc R . .
H1B2 H 0.6776 0.1221 0.5224 0.073 Uiso 1 1 calc R . .
C2B C 0.8688(6) 0.1710(5) 0.5718(2) 0.0594(14) Uani 1 1 d . . .
H2B1 H 0.9563 0.2368 0.5721 0.071 Uiso 1 1 calc R . .
H2B2 H 0.8877 0.1060 0.5522 0.071 Uiso 1 1 calc R . .
C3B C 0.6809(4) 0.1971(3) 0.63252(17) 0.0351(9) Uani 1 1 d . . .
C4B C 0.6020(5) 0.2208(3) 0.67932(16) 0.0364(10) Uani 1 1 d . . .
H4B1 H 0.6660 0.2349 0.7129 0.044 Uiso 1 1 calc R . .
H4B2 H 0.5123 0.1581 0.6815 0.044 Uiso 1 1 calc R . .
C5B C 0.3405(4) 0.3875(3) 0.57739(16) 0.0332(9) Uani 1 1 d . . .
C6B C 0.3355(4) 0.4788(3) 0.61183(17) 0.0343(9) Uani 1 1 d . . .
H6B H 0.4046 0.5060 0.6422 0.041 Uiso 1 1 calc R . .
C7B C 0.2299(5) 0.5306(4) 0.60216(19) 0.0469(11) Uani 1 1 d . . .
H7B H 0.2269 0.5920 0.6264 0.056 Uiso 1 1 calc R . .
C8B C 0.1319(6) 0.4944(5) 0.5588(2) 0.0607(15) Uani 1 1 d . . .
H8B H 0.0609 0.5307 0.5526 0.073 Uiso 1 1 calc R . .
C9B C 0.1350(5) 0.4044(5) 0.5233(2) 0.0610(15) Uani 1 1 d . . .
H9B H 0.0666 0.3794 0.4927 0.073 Uiso 1 1 calc R . .
C10B C 0.2382(5) 0.3510(4) 0.53264(18) 0.0420(11) Uani 1 1 d . . .
C11B C 0.2432(5) 0.2511(4) 0.49673(19) 0.0465(11) Uani 1 1 d . . .
H11C H 0.1782 0.1830 0.5085 0.056 Uiso 1 1 calc R . .
H11D H 0.2078 0.2549 0.4599 0.056 Uiso 1 1 calc R . .
C12B C 0.4835(6) 0.3262(4) 0.46442(19) 0.0585(14) Uani 1 1 d . . .
H12D H 0.4426 0.3036 0.4272 0.088 Uiso 1 1 calc R . .
H12E H 0.5858 0.3266 0.4674 0.088 Uiso 1 1 calc R . .
H12F H 0.4793 0.4008 0.4763 0.088 Uiso 1 1 calc R . .
C13B C 0.3945(6) 0.1337(4) 0.47761(19) 0.0537(13) Uani 1 1 d . . .
H13D H 0.3373 0.1105 0.4428 0.081 Uiso 1 1 calc R . .
H13E H 0.3493 0.0825 0.5025 0.081 Uiso 1 1 calc R . .
H13F H 0.4951 0.1327 0.4738 0.081 Uiso 1 1 calc R . .
C14B C 0.4361(4) 0.3695(3) 0.71554(16) 0.0322(9) Uani 1 1 d . . .
C15B C 0.4844(5) 0.4500(4) 0.75970(18) 0.0427(11) Uani 1 1 d . . .
H15B H 0.5852 0.4926 0.7656 0.051 Uiso 1 1 calc R . .
C16B C 0.3886(6) 0.4686(4) 0.7947(2) 0.0622(15) Uani 1 1 d . . .
H16B H 0.4235 0.5232 0.8251 0.075 Uiso 1 1 calc R . .
C17B C 0.2420(6) 0.4089(5) 0.7863(2) 0.0634(15) Uani 1 1 d . . .
H17B H 0.1760 0.4220 0.8109 0.076 Uiso 1 1 calc R . .
C18B C 0.1915(5) 0.3311(4) 0.7428(2) 0.0561(13) Uani 1 1 d . . .
H18B H 0.0900 0.2904 0.7367 0.067 Uiso 1 1 calc R . .
C19B C 0.2884(5) 0.3113(4) 0.70722(19) 0.0469(11) Uani 1 1 d . . .
H19B H 0.2526 0.2570 0.6768 0.056 Uiso 1 1 calc R . .
C20B C 0.7275(4) 0.4583(3) 0.67960(16) 0.0335(9) Uani 1 1 d . . .
C21B C 0.8292(5) 0.4647(4) 0.72206(18) 0.0460(11) Uani 1 1 d . . .
H21B H 0.8089 0.4102 0.7457 0.055 Uiso 1 1 calc R . .
C22B C 0.9597(5) 0.5510(5) 0.7294(2) 0.0609(14) Uani 1 1 d . . .
H22B H 1.0301 0.5555 0.7580 0.073 Uiso 1 1 calc R . .
C23B C 0.9878(5) 0.6304(4) 0.6954(2) 0.0612(15) Uani 1 1 d . . .
H23B H 1.0772 0.6901 0.7012 0.073 Uiso 1 1 calc R . .
C24B C 0.8907(5) 0.6252(4) 0.6539(2) 0.0537(13) Uani 1 1 d . . .
H24B H 0.9122 0.6805 0.6307 0.064 Uiso 1 1 calc R . .
C25B C 0.7584(4) 0.5380(3) 0.64535(18) 0.0402(10) Uani 1 1 d . . .
H25B H 0.6900 0.5334 0.6161 0.048 Uiso 1 1 calc R . .
O1 O 0.9179(4) 0.1883(3) 0.87140(15) 0.0643(10) Uani 1 1 d . . .
O2 O 0.9083(4) 0.3510(3) 0.83298(18) 0.0758(12) Uani 1 1 d . . .
O3 O 0.8259(4) 0.1719(4) 0.77950(15) 0.0728(11) Uani 1 1 d . . .
S2 S 0.85076(12) 0.23322(10) 0.83179(5) 0.0431(3) Uani 1 1 d . . .
C26 C 0.6684(6) 0.2136(5) 0.8520(2) 0.0563(13) Uani 1 1 d . . .
F1 F 0.5962(3) 0.1060(2) 0.85416(13) 0.0668(8) Uani 1 1 d . . .
F2 F 0.6715(4) 0.2659(3) 0.90084(15) 0.0851(11) Uani 1 1 d . . .
F3 F 0.5885(4) 0.2520(4) 0.81999(17) 0.1103(15) Uani 1 1 d . . .
O4 O 0.2249(5) 0.8721(4) 0.65816(15) 0.1001(16) Uani 1 1 d . . .
O5 O 0.3494(4) 0.9523(4) 0.58403(19) 0.0879(14) Uani 1 1 d . . .
O6 O 0.1385(5) 0.7836(3) 0.56898(16) 0.0786(12) Uani 1 1 d . . .
S3 S 0.21909(16) 0.88649(14) 0.60353(5) 0.0630(4) Uani 1 1 d . . .
C27 C 0.1011(4) 0.9673(3) 0.59780(15) 0.0324(9) Uani 1 1 d . . .
F4 F 0.1497(4) 1.0673(3) 0.62551(16) 0.0943(12) Uani 1 1 d . . .
F5 F 0.0673(4) 0.9794(3) 0.54819(12) 0.0768(10) Uani 1 1 d . . .
F6 F -0.0300(3) 0.9195(3) 0.61725(13) 0.0765(9) Uani 1 1 d . . .
O7 O 0.4531(15) 0.5766(10) 0.0097(5) 0.192(7) Uani 0.50 1 d PDU A -1
C28 C 0.401(3) 0.4211(17) -0.0711(5) 0.108(7) Uani 0.50 1 d PDU A -1
C29 C 0.4211(10) 0.4597(8) -0.0126(4) 0.042(2) Uani 0.50 1 d PDU A -1
C30 C 0.5770(19) 0.5862(18) 0.0531(8) 0.134(9) Uani 0.50 1 d PDU A -1
C31 C 0.7323(14) 0.6376(14) 0.0807(6) 0.106(5) Uani 0.50 1 d PDU A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C5A Pd1A N1A 175.52(14) . . ?
C5A Pd1A N2A 81.55(15) . . ?
N1A Pd1A N2A 102.91(13) . . ?
C5A Pd1A P1A 93.23(12) . . ?
N1A Pd1A P1A 82.29(9) . . ?
N2A Pd1A P1A 174.45(10) . . ?
C14A P1A C20A 106.62(18) . . ?
C14A P1A C4A 105.42(18) . . ?
C20A P1A C4A 104.33(18) . . ?
C14A P1A Pd1A 114.50(14) . . ?
C20A P1A Pd1A 121.42(12) . . ?
C4A P1A Pd1A 102.85(13) . . ?
C3A N1A C1A 112.2(3) . . ?
C3A N1A Pd1A 118.4(3) . . ?
C1A N1A Pd1A 129.2(3) . . ?
C12A N2A C13A 107.9(4) . . ?
C12A N2A C11A 108.9(3) . . ?
C13A N2A C11A 109.0(4) . . ?
C12A N2A Pd1A 109.9(3) . . ?
C13A N2A Pd1A 119.3(3) . . ?
C11A N2A Pd1A 101.3(3) . . ?
C3A S1A C2A 90.2(2) . . ?
N1A C1A C2A 112.0(4) . . ?
N1A C1A H1A1 109.2 . . ?
C2A C1A H1A1 109.2 . . ?
N1A C1A H1A2 109.2 . . ?
C2A C1A H1A2 109.2 . . ?
H1A1 C1A H1A2 107.9 . . ?
C1A C2A S1A 107.7(3) . . ?
C1A C2A H2A1 110.2 . . ?
S1A C2A H2A1 110.2 . . ?
C1A C2A H2A2 110.2 . . ?
S1A C2A H2A2 110.2 . . ?
H2A1 C2A H2A2 108.5 . . ?
N1A C3A C4A 123.0(3) . . ?
N1A C3A S1A 117.9(3) . . ?
C4A C3A S1A 119.0(3) . . ?
C3A C4A P1A 109.7(3) . . ?
C3A C4A H4A1 109.7 . . ?
P1A C4A H4A1 109.7 . . ?
C3A C4A H4A2 109.7 . . ?
P1A C4A H4A2 109.7 . . ?
H4A1 C4A H4A2 108.2 . . ?
C6A C5A C10A 116.8(4) . . ?
C6A C5A Pd1A 130.9(3) . . ?
C10A C5A Pd1A 112.2(3) . . ?
C5A C6A C7A 121.5(4) . . ?
C5A C6A H6A 119.2 . . ?
C7A C6A H6A 119.2 . . ?
C8A C7A C6A 120.4(5) . . ?
C8A C7A H7A 119.8 . . ?
C6A C7A H7A 119.8 . . ?
C9A C8A C7A 119.2(4) . . ?
C9A C8A H8A 120.4 . . ?
C7A C8A H8A 120.4 . . ?
C8A C9A C10A 121.2(4) . . ?
C8A C9A H9A 119.4 . . ?
C10A C9A H9A 119.4 . . ?
C9A C10A C5A 120.8(4) . . ?
C9A C10A C11A 122.8(4) . . ?
C5A C10A C11A 116.3(4) . . ?
C10A C11A N2A 110.1(4) . . ?
C10A C11A H11A 109.6 . . ?
N2A C11A H11A 109.6 . . ?
C10A C11A H11B 109.6 . . ?
N2A C11A H11B 109.6 . . ?
H11A C11A H11B 108.2 . . ?
N2A C12A H12A 109.5 . . ?
N2A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
N2A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N2A C13A H13A 109.5 . . ?
N2A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
N2A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C15A C14A C19A 119.1(4) . . ?
C15A C14A P1A 122.1(3) . . ?
C19A C14A P1A 118.7(3) . . ?
C14A C15A C16A 120.5(5) . . ?
C14A C15A H15A 119.8 . . ?
C16A C15A H15A 119.8 . . ?
C17A C16A C15A 119.7(5) . . ?
C17A C16A H16A 120.2 . . ?
C15A C16A H16A 120.2 . . ?
C18A C17A C16A 121.3(5) . . ?
C18A C17A H17A 119.4 . . ?
C16A C17A H17A 119.4 . . ?
C17A C18A C19A 119.6(5) . . ?
C17A C18A H18A 120.2 . . ?
C19A C18A H18A 120.2 . . ?
C18A C19A C14A 119.9(4) . . ?
C18A C19A H19A 120.0 . . ?
C14A C19A H19A 120.0 . . ?
C25A C20A C21A 119.5(4) . . ?
C25A C20A P1A 122.4(3) . . ?
C21A C20A P1A 118.0(3) . . ?
C22A C21A C20A 119.1(4) . . ?
C22A C21A H21A 120.5 . . ?
C20A C21A H21A 120.5 . . ?
C23A C22A C21A 120.7(4) . . ?
C23A C22A H22A 119.6 . . ?
C21A C22A H22A 119.6 . . ?
C24A C23A C22A 120.1(4) . . ?
C24A C23A H23A 119.9 . . ?
C22A C23A H23A 119.9 . . ?
C23A C24A C25A 120.4(4) . . ?
C23A C24A H24A 119.8 . . ?
C25A C24A H24A 119.8 . . ?
C24A C25A C20A 120.2(4) . . ?
C24A C25A H25A 119.9 . . ?
C20A C25A H25A 119.9 . . ?
C5B Pd1B N2B 82.21(15) . . ?
C5B Pd1B N1B 175.74(14) . . ?
N2B Pd1B N1B 101.00(13) . . ?
C5B Pd1B P1B 97.43(12) . . ?
N2B Pd1B P1B 175.34(9) . . ?
N1B Pd1B P1B 79.61(9) . . ?
C14B P1B C20B 107.74(19) . . ?
C14B P1B C4B 107.15(18) . . ?
C20B P1B C4B 104.97(19) . . ?
C14B P1B Pd1B 122.80(13) . . ?
C20B P1B Pd1B 112.70(14) . . ?
C4B P1B Pd1B 99.62(14) . . ?
C3B N1B C1B 112.8(3) . . ?
C3B N1B Pd1B 117.5(3) . . ?
C1B N1B Pd1B 129.6(3) . . ?
C13B N2B C12B 109.3(4) . . ?
C13B N2B C11B 109.1(3) . . ?
C12B N2B C11B 109.9(4) . . ?
C13B N2B Pd1B 114.9(3) . . ?
C12B N2B Pd1B 109.1(3) . . ?
C11B N2B Pd1B 104.5(3) . . ?
C3B S1B C2B 89.8(2) . . ?
N1B C1B C2B 110.4(4) . . ?
N1B C1B H1B1 109.6 . . ?
C2B C1B H1B1 109.6 . . ?
N1B C1B H1B2 109.6 . . ?
C2B C1B H1B2 109.6 . . ?
H1B1 C1B H1B2 108.1 . . ?
C1B C2B S1B 106.6(3) . . ?
C1B C2B H2B1 110.4 . . ?
S1B C2B H2B1 110.4 . . ?
C1B C2B H2B2 110.4 . . ?
S1B C2B H2B2 110.4 . . ?
H2B1 C2B H2B2 108.6 . . ?
N1B C3B C4B 121.1(4) . . ?
N1B C3B S1B 117.3(3) . . ?
C4B C3B S1B 121.5(3) . . ?
C3B C4B P1B 103.8(3) . . ?
C3B C4B H4B1 111.0 . . ?
P1B C4B H4B1 111.0 . . ?
C3B C4B H4B2 111.0 . . ?
P1B C4B H4B2 111.0 . . ?
H4B1 C4B H4B2 109.0 . . ?
C6B C5B C10B 117.9(4) . . ?
C6B C5B Pd1B 129.1(3) . . ?
C10B C5B Pd1B 112.9(3) . . ?
C5B C6B C7B 120.6(4) . . ?
C5B C6B H6B 119.7 . . ?
C7B C6B H6B 119.7 . . ?
C8B C7B C6B 120.8(4) . . ?
C8B C7B H7B 119.6 . . ?
C6B C7B H7B 119.6 . . ?
C7B C8B C9B 120.0(4) . . ?
C7B C8B H8B 120.0 . . ?
C9B C8B H8B 120.0 . . ?
C8B C9B C10B 119.9(4) . . ?
C8B C9B H9B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C9B C10B C5B 120.7(4) . . ?
C9B C10B C11B 122.2(4) . . ?
C5B C10B C11B 117.1(4) . . ?
N2B C11B C10B 109.7(3) . . ?
N2B C11B H11C 109.7 . . ?
C10B C11B H11C 109.7 . . ?
N2B C11B H11D 109.7 . . ?
C10B C11B H11D 109.7 . . ?
H11C C11B H11D 108.2 . . ?
N2B C12B H12D 109.5 . . ?
N2B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
N2B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
N2B C13B H13D 109.5 . . ?
N2B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
N2B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C19B C14B C15B 118.2(4) . . ?
C19B C14B P1B 119.0(3) . . ?
C15B C14B P1B 122.7(3) . . ?
C16B C15B C14B 120.8(4) . . ?
C16B C15B H15B 119.6 . . ?
C14B C15B H15B 119.6 . . ?
C15B C16B C17B 120.3(5) . . ?
C15B C16B H16B 119.8 . . ?
C17B C16B H16B 119.8 . . ?
C18B C17B C16B 120.0(5) . . ?
C18B C17B H17B 120.0 . . ?
C16B C17B H17B 120.0 . . ?
C17B C18B C19B 119.9(5) . . ?
C17B C18B H18B 120.0 . . ?
C19B C18B H18B 120.0 . . ?
C14B C19B C18B 120.7(4) . . ?
C14B C19B H19B 119.7 . . ?
C18B C19B H19B 119.7 . . ?
C25B C20B C21B 119.9(4) . . ?
C25B C20B P1B 118.1(3) . . ?
C21B C20B P1B 122.0(3) . . ?
C22B C21B C20B 119.3(5) . . ?
C22B C21B H21B 120.4 . . ?
C20B C21B H21B 120.4 . . ?
C23B C22B C21B 120.1(5) . . ?
C23B C22B H22B 120.0 . . ?
C21B C22B H22B 120.0 . . ?
C24B C23B C22B 121.3(4) . . ?
C24B C23B H23B 119.3 . . ?
C22B C23B H23B 119.3 . . ?
C23B C24B C25B 119.6(5) . . ?
C23B C24B H24B 120.2 . . ?
C25B C24B H24B 120.2 . . ?
C20B C25B C24B 119.8(4) . . ?
C20B C25B H25B 120.1 . . ?
C24B C25B H25B 120.1 . . ?
O1 S2 O2 115.2(3) . . ?
O1 S2 O3 115.0(3) . . ?
O2 S2 O3 114.3(3) . . ?
O1 S2 C26 103.3(2) . . ?
O2 S2 C26 103.0(2) . . ?
O3 S2 C26 103.7(2) . . ?
F3 C26 F2 106.7(5) . . ?
F3 C26 F1 108.3(5) . . ?
F2 C26 F1 105.8(4) . . ?
F3 C26 S2 112.3(3) . . ?
F2 C26 S2 111.6(4) . . ?
F1 C26 S2 111.8(4) . . ?
O4 S3 O5 117.8(3) . . ?
O4 S3 O6 112.5(3) . . ?
O5 S3 O6 115.3(3) . . ?
O4 S3 C27 104.3(2) . . ?
O5 S3 C27 102.2(2) . . ?
O6 S3 C27 102.0(2) . . ?
F5 C27 F4 107.6(4) . . ?
F5 C27 F6 105.3(3) . . ?
F4 C27 F6 103.8(4) . . ?
F5 C27 S3 113.7(3) . . ?
F4 C27 S3 114.5(3) . . ?
F6 C27 S3 111.1(3) . . ?
C29 O7 C30 99.5(11) . . ?
O7 C29 C28 123.0(12) . . ?
C31 C30 O7 153.4(15) . . ?
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
Pd1A C5A 1.993(4) . ?
Pd1A N1A 2.163(3) . ?
Pd1A N2A 2.173(3) . ?
Pd1A P1A 2.2186(10) . ?
P1A C14A 1.808(4) . ?
P1A C20A 1.817(4) . ?
P1A C4A 1.834(4) . ?
N1A C3A 1.273(5) . ?
N1A C1A 1.465(5) . ?
N2A C12A 1.476(5) . ?
N2A C13A 1.484(6) . ?
N2A C11A 1.498(6) . ?
S1A C3A 1.747(4) . ?
S1A C2A 1.795(5) . ?
C1A C2A 1.481(7) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C3A C4A 1.478(5) . ?
C4A H4A1 0.9900 . ?
C4A H4A2 0.9900 . ?
C5A C6A 1.393(6) . ?
C5A C10A 1.415(5) . ?
C6A C7A 1.396(6) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.384(7) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.368(7) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.392(6) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.477(7) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C14A C15A 1.379(6) . ?
C14A C19A 1.411(6) . ?
C15A C16A 1.382(6) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.374(8) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.372(7) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.381(6) . ?
C18A H18A 0.9500 . ?
C19A H19A 0.9500 . ?
C20A C25A 1.398(5) . ?
C20A C21A 1.399(5) . ?
C21A C22A 1.393(6) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.384(6) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.369(6) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.384(6) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
Pd1B C5B 2.002(4) . ?
Pd1B N2B 2.152(3) . ?
Pd1B N1B 2.154(3) . ?
Pd1B P1B 2.2237(10) . ?
P1B C14B 1.800(4) . ?
P1B C20B 1.812(4) . ?
P1B C4B 1.845(4) . ?
N1B C3B 1.285(5) . ?
N1B C1B 1.456(5) . ?
N2B C13B 1.473(6) . ?
N2B C12B 1.484(5) . ?
N2B C11B 1.493(6) . ?
S1B C3B 1.744(4) . ?
S1B C2B 1.808(5) . ?
C1B C2B 1.499(7) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B C4B 1.493(6) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B C6B 1.392(6) . ?
C5B C10B 1.400(6) . ?
C6B C7B 1.395(6) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.352(6) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.387(7) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.389(6) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.498(6) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B C19B 1.379(6) . ?
C14B C15B 1.388(6) . ?
C15B C16B 1.366(6) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.374(7) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.360(7) . ?
C17B H17B 0.9500 . ?
C18B C19B 1.388(6) . ?
C18B H18B 0.9500 . ?
C19B H19B 0.9500 . ?
C20B C25B 1.384(6) . ?
C20B C21B 1.395(6) . ?
C21B C22B 1.381(6) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.378(8) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.352(7) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.399(6) . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
O1 S2 1.430(3) . ?
O2 S2 1.431(4) . ?
O3 S2 1.433(4) . ?
S2 C26 1.803(5) . ?
C26 F3 1.321(6) . ?
C26 F2 1.335(6) . ?
C26 F1 1.345(6) . ?
O4 S3 1.419(4) . ?
O5 S3 1.426(4) . ?
O6 S3 1.466(4) . ?
S3 C27 1.761(4) . ?
C27 F5 1.321(5) . ?
C27 F4 1.321(5) . ?
C27 F6 1.365(5) . ?
O7 C29 1.470(9) . ?
O7 C30 1.547(9) . ?
C28 C29 1.494(10) . ?
C30 C31 1.530(10) . ?
