# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 891104' #TrackingRef 'PCPPdPF6_ccdc_deposit.cif' _audit_creation_date 2012-03-19T17:46:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H45 F6 O1 P3 Pd1' _chemical_formula_sum 'C24 H45 F6 O P3 Pd' _chemical_formula_weight 662.91 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.501(2) _cell_length_b 16.505(3) _cell_length_c 11.134(3) _cell_angle_alpha 90 _cell_angle_beta 106.599(3) _cell_angle_gamma 90 _cell_volume 1497.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9623 _cell_measurement_theta_min 4.3197 _cell_measurement_theta_max 30.8468 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.91233 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.0854318 _diffrn_orient_matrix_ub_12 -0.000678 _diffrn_orient_matrix_ub_13 -0.0308081 _diffrn_orient_matrix_ub_21 -0.0167096 _diffrn_orient_matrix_ub_22 0.0021904 _diffrn_orient_matrix_ub_23 0.0587841 _diffrn_orient_matrix_ub_31 -0.0004777 _diffrn_orient_matrix_ub_32 0.0429261 _diffrn_orient_matrix_ub_33 -0.0034933 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_number 15074 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 30.91 _diffrn_reflns_theta_full 30.91 _diffrn_measured_fraction_theta_full 0.886 _diffrn_measured_fraction_theta_max 0.886 _reflns_number_total 7046 _reflns_number_gt 6498 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET) (compiled Sep 13 2010,14:28:38) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.6040P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7046 _refine_ls_number_parameters 334 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.093(18) _refine_diff_density_max 0.969 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1898(4) 0.64021(18) 0.3970(3) 0.0142(6) Uani 1 1 d . . . C2 C 0.2648(4) 0.6710(2) 0.5184(3) 0.0188(6) Uani 1 1 d . . . C3 C 0.3932(4) 0.62794(19) 0.5999(3) 0.0221(7) Uani 1 1 d . . . H3 H 0.4416 0.6481 0.6821 0.026 Uiso 1 1 calc R . . C4 C 0.4512(4) 0.5567(2) 0.5631(3) 0.0254(7) Uani 1 1 d . . . H4 H 0.5394 0.5285 0.6194 0.03 Uiso 1 1 calc R . . C5 C 0.3798(4) 0.5261(2) 0.4431(3) 0.0236(7) Uani 1 1 d . . . H5 H 0.4207 0.4776 0.4171 0.028 Uiso 1 1 calc R . . C6 C 0.2485(4) 0.56674(18) 0.3611(3) 0.0179(6) Uani 1 1 d . . . C7 C 0.1668(4) 0.53137(19) 0.2341(3) 0.0199(6) Uani 1 1 d . . . H7A H 0.0897 0.488 0.2416 0.024 Uiso 1 1 calc R . . H7B H 0.2505 0.5074 0.1984 0.024 Uiso 1 1 calc R . . C8 C 0.2127(4) 0.7505(2) 0.5585(3) 0.0244(7) Uani 1 1 d . . . H8A H 0.2977 0.7919 0.5608 0.029 Uiso 1 1 calc R . . H8B H 0.1998 0.7455 0.6438 0.029 Uiso 1 1 calc R . . C9 C -0.1430(5) 0.7576(2) 0.5274(3) 0.0250(8) Uani 1 1 d . . . C10 C -0.1345(5) 0.8097(3) 0.6434(4) 0.0383(10) Uani 1 1 d . . . H10A H -0.1651 0.8656 0.6172 0.058 Uiso 1 1 calc R . . H10B H -0.0225 0.8087 0.6999 0.058 Uiso 1 1 calc R . . H10C H -0.2106 0.7881 0.687 0.058 Uiso 1 1 calc R . . C11 C -0.3135(5) 0.7639(3) 0.4338(4) 0.0428(10) Uani 1 1 d . . . H11A H -0.3967 0.7492 0.4752 0.064 Uiso 1 1 calc R . . H11B H -0.3207 0.7271 0.3634 0.064 Uiso 1 1 calc R . . H11C H -0.3323 0.8197 0.4026 0.064 Uiso 1 1 calc R . . C12 C -0.1147(6) 0.6685(2) 0.5691(4) 0.0382(10) Uani 1 1 d . . . H12A H -0.2022 0.6509 0.6045 0.057 Uiso 1 1 calc R . . H12B H -0.0083 0.6634 0.6328 0.057 Uiso 1 1 calc R . . H12C H -0.1154 0.6346 0.4967 0.057 Uiso 1 1 calc R . . C13 C 0.0467(5) 0.89345(19) 0.4286(3) 0.0264(7) Uani 1 1 d . . . C14 C 0.1215(5) 0.9379(2) 0.5527(4) 0.0358(9) Uani 1 1 d . . . H14A H 0.2252 0.9119 0.5978 0.054 Uiso 1 1 calc R . . H14B H 0.0451 0.9356 0.6039 0.054 Uiso 1 1 calc R . . H14C H 0.142 0.9945 0.5356 0.054 Uiso 1 1 calc R . . C15 C 0.1656(6) 0.8993(3) 0.3486(4) 0.0420(10) Uani 1 1 d . . . H15A H 0.1899 0.9564 0.3374 0.063 Uiso 1 1 calc R . . H15B H 0.1156 0.8746 0.2666 0.063 Uiso 1 1 calc R . . H15C H 0.2676 0.8708 0.3906 0.063 Uiso 1 1 calc R . . C16 C -0.1158(6) 0.9352(2) 0.3592(4) 0.0419(10) Uani 1 1 d . . . H16A H -0.0952 0.9925 0.3464 0.063 Uiso 1 1 calc R . . H16B H -0.1933 0.9307 0.4093 0.063 Uiso 1 1 calc R . . H16C H -0.1622 0.9089 0.2778 0.063 Uiso 1 1 calc R . . C17 C -0.1221(4) 0.55723(19) 0.0217(3) 0.0223(7) Uani 1 1 d . . . C18 C -0.2488(4) 0.5459(2) 0.0952(4) 0.0313(8) Uani 1 1 d . . . H18A H -0.2895 0.599 0.1122 0.047 Uiso 1 1 calc R . . H18B H -0.1969 0.5183 0.1746 0.047 Uiso 1 1 calc R . . H18C H -0.3406 0.5131 0.0456 0.047 Uiso 1 1 calc R . . C19 C -0.0759(5) 0.4740(2) -0.0175(4) 0.0337(9) Uani 1 1 d . . . H19A H -0.1712 0.4499 -0.0784 0.051 Uiso 1 1 calc R . . H19B H -0.0409 0.4389 0.0563 0.051 Uiso 1 1 calc R . . H19C H 0.0141 0.4797 -0.0556 0.051 Uiso 1 1 calc R . . C20 C -0.2030(4) 0.6070(2) -0.0958(3) 0.0288(7) Uani 1 1 d . . . H20A H -0.3067 0.5814 -0.1419 0.043 Uiso 1 1 calc R . . H20B H -0.1295 0.6094 -0.1494 0.043 Uiso 1 1 calc R . . H20C H -0.2246 0.662 -0.0714 0.043 Uiso 1 1 calc R . . C21 C 0.2001(4) 0.6549(2) 0.0492(3) 0.0251(7) Uani 1 1 d . . . C22 C 0.1292(5) 0.7358(2) -0.0094(4) 0.0346(9) Uani 1 1 d . . . H22A H 0.2055 0.761 -0.0496 0.052 Uiso 1 1 calc R . . H22B H 0.1131 0.7718 0.056 0.052 Uiso 1 1 calc R . . H22C H 0.0236 0.7263 -0.0722 0.052 Uiso 1 1 calc R . . C23 C 0.3624(4) 0.6734(2) 0.1497(4) 0.0309(8) Uani 1 1 d . . . H23A H 0.4375 0.701 0.1108 0.046 Uiso 1 1 calc R . . H23B H 0.4124 0.6227 0.1879 0.046 Uiso 1 1 calc R . . H23C H 0.3407 0.7084 0.2143 0.046 Uiso 1 1 calc R . . C24 C 0.2360(5) 0.5984(3) -0.0488(3) 0.0344(9) Uani 1 1 d . . . H24A H 0.1348 0.5892 -0.1165 0.052 Uiso 1 1 calc R . . H24B H 0.2776 0.5466 -0.0095 0.052 Uiso 1 1 calc R . . H24C H 0.3184 0.6233 -0.0832 0.052 Uiso 1 1 calc R . . F1 F -0.6712(2) 0.85381(12) -0.17353(19) 0.0262(4) Uani 1 1 d . . . F2 F -0.4728(3) 0.87480(14) 0.0084(2) 0.0346(5) Uani 1 1 d . . . F3 F -0.4720(3) 0.76013(12) -0.1030(2) 0.0355(5) Uani 1 1 d . . . F4 F -0.2773(2) 0.85607(13) -0.09181(19) 0.0303(5) Uani 1 1 d . . . F5 F -0.4759(3) 0.83630(16) -0.27369(19) 0.0377(6) Uani 1 1 d . . . F6 F -0.4778(3) 0.94973(13) -0.1629(2) 0.0373(5) Uani 1 1 d . . . P1 P 0.01799(10) 0.78162(5) 0.44871(7) 0.01698(15) Uani 1 1 d . . . P2 P 0.05582(9) 0.61138(5) 0.13141(7) 0.01520(15) Uani 1 1 d . . . P3 P -0.47550(10) 0.85508(5) -0.13306(8) 0.01922(16) Uani 1 1 d . . . Pd1 Pd 0.00603(2) 0.701973(13) 0.275313(18) 0.01503(5) Uani 1 1 d . . . O1 O -0.1930(4) 0.76570(19) 0.1459(3) 0.0442(8) Uani 1 1 d . . . H1A H -0.265(7) 0.737(3) 0.071(5) 0.066 Uiso 1 1 d . . . H1B H -0.282(6) 0.795(3) 0.182(5) 0.066 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0144(14) 0.0177(14) 0.0102(13) -0.0001(11) 0.0029(11) 0.0007(10) C2 0.0153(15) 0.0229(14) 0.0172(15) 0.0002(12) 0.0032(12) 0.0015(11) C3 0.0200(16) 0.0242(17) 0.0180(15) 0.0021(13) -0.0011(13) 0.0016(12) C4 0.0221(17) 0.0261(17) 0.0237(17) 0.0015(14) -0.0001(14) 0.0088(13) C5 0.0242(17) 0.0219(16) 0.0236(16) 0.0043(13) 0.0052(14) 0.0102(12) C6 0.0189(15) 0.0192(15) 0.0170(14) 0.0025(12) 0.0075(12) 0.0022(11) C7 0.0243(16) 0.0178(15) 0.0179(14) -0.0009(12) 0.0068(13) 0.0023(11) C8 0.0220(17) 0.0243(17) 0.0218(16) -0.0003(13) -0.0022(14) 0.0059(13) C9 0.0273(19) 0.0281(19) 0.0228(17) 0.0033(14) 0.0125(15) 0.0023(14) C10 0.045(2) 0.045(2) 0.030(2) -0.0034(17) 0.0188(19) 0.0163(18) C11 0.026(2) 0.070(3) 0.034(2) 0.002(2) 0.0125(18) -0.0040(18) C12 0.051(3) 0.031(2) 0.040(2) 0.0045(18) 0.026(2) -0.0037(18) C13 0.038(2) 0.0149(15) 0.0241(17) -0.0003(13) 0.0055(15) -0.0003(13) C14 0.056(3) 0.0175(17) 0.0275(19) -0.0032(14) 0.0011(18) 0.0025(16) C15 0.054(3) 0.036(2) 0.036(2) 0.0034(18) 0.012(2) -0.0174(19) C16 0.056(3) 0.0217(18) 0.035(2) 0.0019(16) -0.0083(19) 0.0070(17) C17 0.0235(16) 0.0205(16) 0.0220(16) -0.0027(13) 0.0053(13) -0.0006(12) C18 0.0244(18) 0.0327(19) 0.036(2) -0.0013(16) 0.0063(16) -0.0097(14) C19 0.041(2) 0.0267(19) 0.0257(19) -0.0083(14) -0.0035(17) 0.0025(15) C20 0.0297(19) 0.0322(19) 0.0206(16) -0.0028(14) 0.0008(14) 0.0011(15) C21 0.0225(17) 0.0328(19) 0.0224(17) 0.0018(14) 0.0103(15) -0.0021(13) C22 0.033(2) 0.038(2) 0.038(2) 0.0167(17) 0.0185(19) -0.0028(16) C23 0.0224(18) 0.044(2) 0.0283(18) 0.0028(15) 0.0102(15) -0.0058(14) C24 0.033(2) 0.051(2) 0.0245(18) -0.0004(17) 0.0162(16) 0.0041(17) F1 0.0162(9) 0.0325(11) 0.0293(10) 0.0060(9) 0.0052(8) -0.0009(7) F2 0.0306(12) 0.0515(14) 0.0213(10) -0.0053(10) 0.0066(9) 0.0056(10) F3 0.0314(12) 0.0227(11) 0.0520(14) 0.0059(10) 0.0114(11) 0.0012(8) F4 0.0150(10) 0.0458(13) 0.0282(11) 0.0013(10) 0.0030(8) 0.0006(8) F5 0.0264(12) 0.0682(17) 0.0200(10) -0.0054(10) 0.0093(9) -0.0009(10) F6 0.0267(11) 0.0273(11) 0.0591(15) 0.0101(10) 0.0141(11) -0.0025(8) P1 0.0201(4) 0.0159(4) 0.0140(3) -0.0005(3) 0.0034(3) 0.0026(3) P2 0.0169(4) 0.0160(4) 0.0132(3) 0.0003(3) 0.0052(3) 0.0004(3) P3 0.0156(4) 0.0222(4) 0.0194(4) 0.0017(3) 0.0040(3) 0.0001(3) Pd1 0.01549(9) 0.01592(9) 0.01263(9) -0.00041(10) 0.00233(7) 0.00244(10) O1 0.0443(19) 0.0469(18) 0.0329(16) -0.0045(13) -0.0026(14) 0.0187(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C6 1.412(4) . ? C1 C2 1.414(4) . ? C1 Pd1 2.026(3) . ? C2 C3 1.397(4) . ? C2 C8 1.494(4) . ? C3 C4 1.382(5) . ? C3 H3 0.95 . ? C4 C5 1.394(5) . ? C4 H4 0.95 . ? C5 C6 1.395(4) . ? C5 H5 0.95 . ? C6 C7 1.504(4) . ? C7 P2 1.823(3) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 P1 1.828(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C11 1.528(5) . ? C9 C10 1.536(5) . ? C9 C12 1.540(5) . ? C9 P1 1.867(4) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C15 1.530(5) . ? C13 C14 1.532(5) . ? C13 C16 1.539(5) . ? C13 P1 1.884(3) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C19 1.527(5) . ? C17 C20 1.532(5) . ? C17 C18 1.539(5) . ? C17 P2 1.877(3) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C24 1.531(5) . ? C21 C22 1.532(5) . ? C21 C23 1.538(5) . ? C21 P2 1.871(3) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? F1 P3 1.595(2) . ? F2 P3 1.602(2) . ? F3 P3 1.601(2) . ? F4 P3 1.615(2) . ? F5 P3 1.595(2) . ? F6 P3 1.596(2) . ? P1 Pd1 2.3138(11) . ? P2 Pd1 2.3172(10) . ? Pd1 O1 2.157(3) . ? O1 H1A 1.00(5) . ? O1 H1B 1.07(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 C6 C1 C2 118.7(3) . . ? C6 C1 Pd1 120.7(2) . . ? C2 C1 Pd1 120.6(2) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C8 119.7(3) . . ? C1 C2 C8 120.7(3) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 120.6(3) . . ? C5 C6 C7 119.8(3) . . ? C1 C6 C7 119.6(3) . . ? C6 C7 P2 109.0(2) . . ? C6 C7 H7A 109.9 . . ? P2 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? P2 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C2 C8 P1 109.7(2) . . ? C2 C8 H8A 109.7 . . ? P1 C8 H8A 109.7 . . ? C2 C8 H8B 109.7 . . ? P1 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C11 C9 C10 110.0(3) . . ? C11 C9 C12 107.9(4) . . ? C10 C9 C12 108.4(3) . . ? C11 C9 P1 110.2(3) . . ? C10 C9 P1 114.2(3) . . ? C12 C9 P1 105.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 108.7(3) . . ? C15 C13 C16 109.1(3) . . ? C14 C13 C16 108.7(3) . . ? C15 C13 P1 105.1(2) . . ? C14 C13 P1 113.3(2) . . ? C16 C13 P1 111.7(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C20 109.1(3) . . ? C19 C17 C18 108.6(3) . . ? C20 C17 C18 107.9(3) . . ? C19 C17 P2 112.9(2) . . ? C20 C17 P2 112.5(2) . . ? C18 C17 P2 105.6(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 111.2(3) . . ? C24 C21 C23 108.7(3) . . ? C22 C21 C23 107.4(3) . . ? C24 C21 P2 114.0(3) . . ? C22 C21 P2 108.0(2) . . ? C23 C21 P2 107.3(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 P1 C9 105.76(17) . . ? C8 P1 C13 103.41(16) . . ? C9 P1 C13 113.67(16) . . ? C8 P1 Pd1 102.34(11) . . ? C9 P1 Pd1 114.04(12) . . ? C13 P1 Pd1 115.72(11) . . ? C7 P2 C21 106.88(16) . . ? C7 P2 C17 103.86(15) . . ? C21 P2 C17 112.55(16) . . ? C7 P2 Pd1 101.42(10) . . ? C21 P2 Pd1 111.45(12) . . ? C17 P2 Pd1 119.00(11) . . ? F1 P3 F5 90.60(11) . . ? F1 P3 F6 90.25(11) . . ? F5 P3 F6 89.39(14) . . ? F1 P3 F3 90.10(11) . . ? F5 P3 F3 90.57(14) . . ? F6 P3 F3 179.65(12) . . ? F1 P3 F2 90.06(12) . . ? F5 P3 F2 179.17(14) . . ? F6 P3 F2 90.11(13) . . ? F3 P3 F2 89.93(13) . . ? F1 P3 F4 179.79(13) . . ? F5 P3 F4 89.47(11) . . ? F6 P3 F4 89.94(12) . . ? F3 P3 F4 89.71(11) . . ? F2 P3 F4 89.88(12) . . ? C1 Pd1 O1 178.82(13) . . ? C1 Pd1 P1 83.48(9) . . ? O1 Pd1 P1 96.86(9) . . ? C1 Pd1 P2 83.07(9) . . ? O1 Pd1 P2 96.67(9) . . ? P1 Pd1 P2 166.02(3) . . ? Pd1 O1 H1A 121(3) . . ? Pd1 O1 H1B 118(3) . . ? H1A O1 H1B 101(4) . . ? 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 O1 H1A F3 1.00(5) 2.24(5) 3.091(4) 142(4) . O1 H1B F2 1.07(5) 2.51(5) 3.027(4) 109(3) . # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF