data_global _audit_creation_date 'Sep 2010' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Assistant Prof. Masato Ohashi' _publ_contact_author_email 'ohashi@chem.eng.osaka-u.ac.jp' _publ_contact_author_fax '+81 6 6879 7394' _publ_contact_author_phone '+81 6 6879 7393' _publ_contact_author_address ; Department of Applied Chemistry, Faculty of Engineering, Suita, Osaka-565-0871, Japan ; _publ_requested_journal ' JACS ' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Palladium-Catalyzed Coupling Reactions of Tetrafluoroethylene with Arylzinc Compounds ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name ' Masato Ohashi ' ' Tadashi Kambara ' ' Tsubasa Hatanaka ' ' Sensuke Ogoshi ' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; #============================================================================== data_TFE-Pd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H30 F4 P2 Pd), C7' _chemical_formula_sum 'C83 H60 F8 P4 Pd2' _chemical_formula_weight 1545.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-p 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 18.0191(9) _cell_length_b 9.5138(5) _cell_length_c 20.8353(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.3190(18) _cell_angle_gamma 90.00 _cell_volume 3570.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 32512 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 30.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ; Higashi, T. (1999). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'imaging plate' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31619 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6235 _reflns_number_gt 5247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1999)' _computing_structure_solution 'PATTY (Bueskens, et al., 1994)' _computing_publication_material 'SHELXL-97 and modified' _computing_molecular_graphics 'Ortep-3 (Louis J. Farrugia, 1999)' # Carroll K. Johnson and M. N. Burnett, ORNL-6895, ORTEP-III(version 1.0.2), # A FORTRAN Thermal-Ellipsoid Plot Program, Oak Ridge National Labratory, # Oak Ridge, Tennessee. # Ortep-3 for Windows, Version 1.05 Louis J. Farrugia, _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^)+(0.0370P)^2^+3.5412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6235 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.271968(10) 0.50357(2) 0.193354(9) 0.01600(8) Uani 1 1 d . . . P1 P 0.17740(4) 0.37220(7) 0.13996(3) 0.01847(16) Uani 1 1 d . . . P2 P 0.36370(4) 0.52129(7) 0.11567(3) 0.01789(16) Uani 1 1 d . . . F1 F 0.23458(10) 0.41920(18) 0.32540(7) 0.0338(4) Uani 1 1 d . . . F2 F 0.18196(9) 0.62081(18) 0.29887(7) 0.0335(4) Uani 1 1 d . . . F3 F 0.36952(9) 0.53518(18) 0.30879(8) 0.0307(4) Uani 1 1 d . . . F4 F 0.31675(9) 0.73509(16) 0.28208(7) 0.0302(4) Uani 1 1 d . . . C1 C 0.23902(16) 0.5320(3) 0.28489(13) 0.0236(6) Uani 1 1 d . . . C2 C 0.31033(15) 0.5931(3) 0.27645(12) 0.0229(6) Uani 1 1 d . . . C101 C 0.08552(14) 0.4284(3) 0.16462(12) 0.0199(6) Uani 1 1 d . . . C102 C 0.02726(15) 0.3367(3) 0.17541(13) 0.0270(6) Uani 1 1 d . . . H102 H 0.0333 0.2387 0.1683 0.032 Uiso 1 1 calc R . . C103 C -0.04024(16) 0.3888(4) 0.19677(14) 0.0343(7) Uani 1 1 d . . . H103 H -0.0798 0.3258 0.2051 0.041 Uiso 1 1 calc R . . C104 C -0.04999(17) 0.5308(4) 0.20585(14) 0.0335(7) Uani 1 1 d . . . H104 H -0.0957 0.5653 0.2212 0.040 Uiso 1 1 calc R . . C105 C 0.00664(17) 0.6229(3) 0.19260(14) 0.0344(7) Uani 1 1 d . . . H105 H -0.0007 0.7213 0.1968 0.041 Uiso 1 1 calc R . . C106 C 0.07433(16) 0.5714(3) 0.17309(13) 0.0274(6) Uani 1 1 d . . . H106 H 0.1138 0.6351 0.1654 0.033 Uiso 1 1 calc R . . C111 C 0.18376(14) 0.1857(3) 0.15943(12) 0.0203(6) Uani 1 1 d . . . C112 C 0.22914(15) 0.1449(3) 0.21125(13) 0.0235(6) Uani 1 1 d . . . H112 H 0.2537 0.2144 0.2366 0.028 Uiso 1 1 calc R . . C113 C 0.23868(16) 0.0046(3) 0.22598(15) 0.0275(7) Uani 1 1 d . . . H113 H 0.2699 -0.0221 0.2613 0.033 Uiso 1 1 calc R . . C114 C 0.20291(16) -0.0969(3) 0.18950(14) 0.0300(7) Uani 1 1 d . . . H114 H 0.2099 -0.1936 0.1994 0.036 Uiso 1 1 calc R . . C115 C 0.15664(16) -0.0578(3) 0.13838(14) 0.0298(7) Uani 1 1 d . . . H115 H 0.1313 -0.1277 0.1138 0.036 Uiso 1 1 calc R . . C116 C 0.14736(15) 0.0826(3) 0.12319(13) 0.0255(6) Uani 1 1 d . . . H116 H 0.1160 0.1089 0.0879 0.031 Uiso 1 1 calc R . . C121 C 0.16943(15) 0.3719(3) 0.05238(12) 0.0232(6) Uani 1 1 d . . . C122 C 0.12129(18) 0.4614(3) 0.01921(14) 0.0329(7) Uani 1 1 d . . . H122 H 0.0872 0.5174 0.0421 0.040 Uiso 1 1 calc R . . C123 C 0.1227(2) 0.4692(4) -0.04707(16) 0.0464(9) Uani 1 1 d . . . H123 H 0.0893 0.5300 -0.0695 0.056 Uiso 1 1 calc R . . C124 C 0.17227(19) 0.3892(4) -0.08059(15) 0.0484(9) Uani 1 1 d . . . H124 H 0.1738 0.3965 -0.1260 0.058 Uiso 1 1 calc R . . C125 C 0.21974(17) 0.2985(4) -0.04821(14) 0.0408(8) Uani 1 1 d . . . H125 H 0.2534 0.2421 -0.0714 0.049 Uiso 1 1 calc R . . C126 C 0.21841(15) 0.2894(3) 0.01801(13) 0.0289(7) Uani 1 1 d . . . H126 H 0.2511 0.2266 0.0401 0.035 Uiso 1 1 calc R . . C201 C 0.38822(14) 0.3498(3) 0.08431(12) 0.0219(6) Uani 1 1 d . . . C202 C 0.39421(17) 0.2414(3) 0.12915(14) 0.0314(7) Uani 1 1 d . . . H202 H 0.3867 0.2608 0.1732 0.038 Uiso 1 1 calc R . . C203 C 0.41095(19) 0.1061(3) 0.11029(17) 0.0420(8) Uani 1 1 d . . . H203 H 0.4153 0.0334 0.1414 0.050 Uiso 1 1 calc R . . C204 C 0.42135(19) 0.0765(3) 0.04640(18) 0.0441(9) Uani 1 1 d . . . H204 H 0.4325 -0.0167 0.0334 0.053 Uiso 1 1 calc R . . C205 C 0.41557(17) 0.1825(3) 0.00132(16) 0.0376(8) Uani 1 1 d . . . H205 H 0.4227 0.1617 -0.0427 0.045 Uiso 1 1 calc R . . C206 C 0.39944(15) 0.3186(3) 0.01968(14) 0.0274(6) Uani 1 1 d . . . H206 H 0.3960 0.3910 -0.0117 0.033 Uiso 1 1 calc R . . C211 C 0.45313(15) 0.5918(3) 0.14382(12) 0.0216(6) Uani 1 1 d . . . C212 C 0.52004(16) 0.5225(3) 0.13452(14) 0.0269(6) Uani 1 1 d . . . H212 H 0.5203 0.4330 0.1142 0.032 Uiso 1 1 calc R . . C213 C 0.58676(17) 0.5840(4) 0.15491(14) 0.0349(7) Uani 1 1 d . . . H213 H 0.6323 0.5364 0.1485 0.042 Uiso 1 1 calc R . . C214 C 0.58673(17) 0.7133(4) 0.18424(15) 0.0370(8) Uani 1 1 d . . . H214 H 0.6324 0.7559 0.1972 0.044 Uiso 1 1 calc R . . C215 C 0.52030(17) 0.7818(3) 0.19493(15) 0.0368(8) Uani 1 1 d . . . H215 H 0.5203 0.8705 0.2158 0.044 Uiso 1 1 calc R . . C216 C 0.45402(16) 0.7207(3) 0.17508(14) 0.0284(7) Uani 1 1 d . . . H216 H 0.4085 0.7675 0.1829 0.034 Uiso 1 1 calc R . . C221 C 0.34167(14) 0.6358(3) 0.04789(12) 0.0205(6) Uani 1 1 d . . . C222 C 0.27106(16) 0.6930(3) 0.04291(14) 0.0295(7) Uani 1 1 d . . . H222 H 0.2351 0.6689 0.0737 0.035 Uiso 1 1 calc R . . C223 C 0.25225(18) 0.7850(4) -0.00643(15) 0.0400(8) Uani 1 1 d . . . H223 H 0.2038 0.8242 -0.0090 0.048 Uiso 1 1 calc R . . C224 C 0.30369(18) 0.8196(3) -0.05173(14) 0.0378(8) Uani 1 1 d . . . H224 H 0.2906 0.8818 -0.0858 0.045 Uiso 1 1 calc R . . C225 C 0.37436(18) 0.7634(3) -0.04732(14) 0.0336(7) Uani 1 1 d . . . H225 H 0.4099 0.7870 -0.0786 0.040 Uiso 1 1 calc R . . C226 C 0.39367(16) 0.6733(3) 0.00231(13) 0.0262(6) Uani 1 1 d . . . H226 H 0.4427 0.6366 0.0054 0.031 Uiso 1 1 calc R . . C41 C 0.0686(4) 0.0019(10) -0.0858(5) 0.132(3) Uani 1 1 d . A -1 C42 C 0.0293(6) 0.1285(16) -0.0471(5) 0.079(4) Uani 0.50 1 d P A -1 C43 C -0.0092(3) 0.1230(5) -0.0027(4) 0.0773(19) Uani 1 1 d . A -1 C44 C -0.0288(4) -0.0011(10) 0.0388(4) 0.0447(19) Uani 0.50 1 d P A -1 C45 C 0.0469(6) -0.125(2) -0.0418(7) 0.126(8) Uani 0.50 1 d P A -1 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 Pd 0.01762(13) 0.01639(13) 0.01393(12) 0.00003(7) -0.00131(8) -0.00054(8) P1 0.0197(4) 0.0167(4) 0.0188(3) 0.0011(3) -0.0027(3) -0.0015(3) P2 0.0174(4) 0.0196(4) 0.0166(3) -0.0002(3) -0.0008(3) -0.0007(3) F1 0.0470(11) 0.0326(10) 0.0219(8) 0.0086(7) 0.0035(7) -0.0010(8) F2 0.0311(10) 0.0396(10) 0.0298(9) -0.0033(8) 0.0040(7) 0.0099(8) F3 0.0296(9) 0.0341(9) 0.0276(9) -0.0019(7) -0.0133(7) 0.0107(7) F4 0.0386(10) 0.0193(8) 0.0322(9) -0.0055(7) -0.0094(7) 0.0016(7) C1 0.0300(16) 0.0236(15) 0.0171(13) 0.0003(12) 0.0015(11) 0.0092(12) C2 0.0282(16) 0.0212(15) 0.0189(13) -0.0016(11) -0.0085(11) 0.0050(12) C101 0.0187(14) 0.0233(15) 0.0174(13) 0.0012(11) -0.0042(10) 0.0005(11) C102 0.0232(16) 0.0267(16) 0.0307(15) 0.0062(13) -0.0052(12) 0.0003(12) C103 0.0230(16) 0.047(2) 0.0323(16) 0.0111(15) -0.0014(12) -0.0009(14) C104 0.0270(17) 0.052(2) 0.0210(15) -0.0010(14) -0.0026(12) 0.0135(15) C105 0.0368(18) 0.0334(18) 0.0323(16) -0.0089(14) -0.0117(13) 0.0111(14) C106 0.0256(16) 0.0246(16) 0.0315(16) -0.0024(13) -0.0066(12) 0.0002(12) C111 0.0188(14) 0.0170(14) 0.0250(14) 0.0020(11) 0.0001(11) 0.0009(11) C112 0.0233(15) 0.0226(15) 0.0244(14) -0.0016(12) -0.0044(11) -0.0028(12) C113 0.0253(16) 0.0256(16) 0.0311(16) 0.0030(12) -0.0093(12) 0.0023(12) C114 0.0323(17) 0.0185(15) 0.0390(17) 0.0025(13) -0.0067(13) 0.0025(12) C115 0.0326(17) 0.0203(15) 0.0361(17) -0.0015(13) -0.0085(13) -0.0034(13) C116 0.0244(15) 0.0210(15) 0.0306(15) -0.0009(12) -0.0079(12) 0.0012(12) C121 0.0254(15) 0.0244(15) 0.0197(13) -0.0016(12) -0.0033(11) -0.0070(12) C122 0.0394(19) 0.0337(17) 0.0253(15) -0.0004(14) -0.0082(13) 0.0043(14) C123 0.055(2) 0.056(2) 0.0274(18) 0.0064(16) -0.0128(16) 0.0064(18) C124 0.048(2) 0.078(3) 0.0188(15) 0.0010(17) -0.0035(14) -0.005(2) C125 0.0301(18) 0.065(2) 0.0269(16) -0.0121(16) -0.0021(13) -0.0025(16) C126 0.0225(15) 0.0379(18) 0.0261(15) -0.0056(13) -0.0047(12) -0.0022(13) C201 0.0154(14) 0.0245(15) 0.0256(14) -0.0026(12) -0.0010(11) -0.0002(11) C202 0.0368(18) 0.0242(16) 0.0334(16) 0.0029(13) 0.0036(13) 0.0043(13) C203 0.047(2) 0.0257(17) 0.053(2) 0.0056(16) 0.0082(16) 0.0052(15) C204 0.043(2) 0.0248(18) 0.064(2) -0.0141(17) 0.0074(17) 0.0042(15) C205 0.0338(18) 0.0369(19) 0.0422(18) -0.0163(16) 0.0050(14) -0.0008(14) C206 0.0209(15) 0.0300(16) 0.0313(15) -0.0037(13) 0.0015(12) -0.0037(12) C211 0.0214(15) 0.0258(15) 0.0176(13) 0.0038(11) -0.0020(11) -0.0031(11) C212 0.0228(15) 0.0322(17) 0.0256(15) -0.0006(12) -0.0027(12) -0.0029(12) C213 0.0236(16) 0.044(2) 0.0372(17) -0.0009(15) -0.0070(13) 0.0029(14) C214 0.0264(17) 0.046(2) 0.0383(17) 0.0050(16) -0.0125(13) -0.0121(15) C215 0.0380(19) 0.0303(17) 0.0417(18) -0.0050(15) -0.0088(14) -0.0088(14) C216 0.0235(16) 0.0254(16) 0.0361(16) -0.0025(13) -0.0022(12) -0.0027(12) C221 0.0228(14) 0.0209(14) 0.0178(13) -0.0010(11) -0.0027(11) -0.0023(11) C222 0.0237(16) 0.0351(18) 0.0298(16) 0.0098(13) 0.0006(12) 0.0000(13) C223 0.0303(18) 0.051(2) 0.0390(18) 0.0156(16) -0.0010(14) 0.0071(15) C224 0.048(2) 0.0383(19) 0.0269(16) 0.0132(14) -0.0058(14) 0.0039(15) C225 0.0434(19) 0.0337(18) 0.0241(15) 0.0058(13) 0.0077(13) -0.0021(14) C226 0.0243(16) 0.0264(16) 0.0281(15) 0.0018(12) 0.0029(12) -0.0003(12) C41 0.070(5) 0.176(9) 0.146(7) -0.001(6) -0.044(5) -0.033(5) C42 0.043(6) 0.132(12) 0.061(6) 0.024(7) -0.028(5) -0.045(6) C43 0.062(4) 0.036(3) 0.130(5) -0.003(3) -0.068(4) -0.001(2) C44 0.036(4) 0.053(6) 0.044(5) -0.004(4) -0.021(3) -0.011(4) C45 0.040(6) 0.218(19) 0.119(11) -0.132(12) -0.042(6) 0.058(9) _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 Pd C1 2.029(3) . ? Pd C2 2.036(3) . ? Pd P2 2.3460(7) . ? Pd P1 2.3699(7) . ? P1 C111 1.823(3) . ? P1 C101 1.825(3) . ? P1 C121 1.827(3) . ? P2 C201 1.816(3) . ? P2 C221 1.820(3) . ? P2 C211 1.830(3) . ? F1 C1 1.369(3) . ? F2 C1 1.367(3) . ? F3 C2 1.365(3) . ? F4 C2 1.360(3) . ? C1 C2 1.425(4) . ? C101 C106 1.388(4) . ? C101 C102 1.387(4) . ? C102 C103 1.396(4) . ? C102 H102 0.9500 . ? C103 C104 1.376(4) . ? C103 H103 0.9500 . ? C104 C105 1.378(4) . ? C104 H104 0.9500 . ? C105 C106 1.384(4) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C111 C116 1.393(4) . ? C111 C112 1.394(4) . ? C112 C113 1.380(4) . ? C112 H112 0.9500 . ? C113 C114 1.380(4) . ? C113 H113 0.9500 . ? C114 C115 1.388(4) . ? C114 H114 0.9500 . ? C115 C116 1.382(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.388(4) . ? C121 C126 1.392(4) . ? C122 C123 1.384(4) . ? C122 H122 0.9500 . ? C123 C124 1.376(5) . ? C123 H123 0.9500 . ? C124 C125 1.380(5) . ? C124 H124 0.9500 . ? C125 C126 1.383(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C201 C202 1.394(4) . ? C201 C206 1.398(4) . ? C202 C203 1.381(4) . ? C202 H202 0.9500 . ? C203 C204 1.378(5) . ? C203 H203 0.9500 . ? C204 C205 1.380(5) . ? C204 H204 0.9500 . ? C205 C206 1.384(4) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C211 C212 1.392(4) . ? C211 C216 1.389(4) . ? C212 C213 1.395(4) . ? C212 H212 0.9500 . ? C213 C214 1.373(5) . ? C213 H213 0.9500 . ? C214 C215 1.385(4) . ? C214 H214 0.9500 . ? C215 C216 1.383(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.386(4) . ? C221 C226 1.396(4) . ? C222 C223 1.386(4) . ? C222 H222 0.9500 . ? C223 C224 1.378(4) . ? C223 H223 0.9500 . ? C224 C225 1.382(4) . ? C224 H224 0.9500 . ? C225 C226 1.382(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C41 C45 1.57(2) . ? C41 C42 1.621(17) . ? C42 C43 1.170(11) . ? C43 C44 1.511(10) . ? 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 Pd C2 41.04(11) . . ? C1 Pd P2 149.90(9) . . ? C2 Pd P2 109.01(8) . . ? C1 Pd P1 106.79(9) . . ? C2 Pd P1 147.80(8) . . ? P2 Pd P1 102.98(2) . . ? C111 P1 C101 105.97(12) . . ? C111 P1 C121 102.94(12) . . ? C101 P1 C121 103.33(12) . . ? C111 P1 Pd 111.59(9) . . ? C101 P1 Pd 111.15(9) . . ? C121 P1 Pd 120.57(9) . . ? C201 P2 C221 108.01(12) . . ? C201 P2 C211 103.01(12) . . ? C221 P2 C211 101.77(12) . . ? C201 P2 Pd 111.40(9) . . ? C221 P2 Pd 115.70(9) . . ? C211 P2 Pd 115.76(9) . . ? F2 C1 F1 107.3(2) . . ? F2 C1 C2 117.3(2) . . ? F1 C1 C2 117.5(2) . . ? F2 C1 Pd 121.36(18) . . ? F1 C1 Pd 119.84(18) . . ? C2 C1 Pd 69.77(15) . . ? F4 C2 F3 107.1(2) . . ? F4 C2 C1 118.0(2) . . ? F3 C2 C1 118.1(2) . . ? F4 C2 Pd 121.02(17) . . ? F3 C2 Pd 119.78(18) . . ? C1 C2 Pd 69.19(15) . . ? C106 C101 C102 118.9(3) . . ? C106 C101 P1 117.3(2) . . ? C102 C101 P1 123.8(2) . . ? C101 C102 C103 119.8(3) . . ? C101 C102 H102 120.1 . . ? C103 C102 H102 120.1 . . ? C104 C103 C102 120.5(3) . . ? C104 C103 H103 119.7 . . ? C102 C103 H103 119.7 . . ? C103 C104 C105 120.0(3) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 C106 119.7(3) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C105 C106 C101 121.1(3) . . ? C105 C106 H106 119.5 . . ? C101 C106 H106 119.5 . . ? C116 C111 C112 119.0(2) . . ? C116 C111 P1 122.6(2) . . ? C112 C111 P1 118.4(2) . . ? C113 C112 C111 120.6(3) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C112 C113 C114 120.0(3) . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C113 C114 C115 120.0(3) . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C116 C115 C114 120.1(3) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 120.2(2) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C122 C121 C126 119.1(3) . . ? C122 C121 P1 122.0(2) . . ? C126 C121 P1 118.6(2) . . ? C123 C122 C121 120.3(3) . . ? C123 C122 H122 119.9 . . ? C121 C122 H122 119.9 . . ? C124 C123 C122 120.2(3) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 120.0(3) . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C124 C125 C126 120.1(3) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C126 C121 120.3(3) . . ? C125 C126 H126 119.9 . . ? C121 C126 H126 119.9 . . ? C202 C201 C206 118.5(3) . . ? C202 C201 P2 116.1(2) . . ? C206 C201 P2 125.4(2) . . ? C203 C202 C201 120.8(3) . . ? C203 C202 H202 119.6 . . ? C201 C202 H202 119.6 . . ? C204 C203 C202 120.1(3) . . ? C204 C203 H203 120.0 . . ? C202 C203 H203 120.0 . . ? C203 C204 C205 119.9(3) . . ? C203 C204 H204 120.1 . . ? C205 C204 H204 120.1 . . ? C204 C205 C206 120.6(3) . . ? C204 C205 H205 119.7 . . ? C206 C205 H205 119.7 . . ? C205 C206 C201 120.0(3) . . ? C205 C206 H206 120.0 . . ? C201 C206 H206 120.0 . . ? C212 C211 C216 118.9(3) . . ? C212 C211 P2 122.7(2) . . ? C216 C211 P2 118.3(2) . . ? C211 C212 C213 120.1(3) . . ? C211 C212 H212 119.9 . . ? C213 C212 H212 119.9 . . ? C214 C213 C212 120.2(3) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C215 120.1(3) . . ? C213 C214 H214 119.9 . . ? C215 C214 H214 119.9 . . ? C216 C215 C214 119.9(3) . . ? C216 C215 H215 120.1 . . ? C214 C215 H215 120.1 . . ? C215 C216 C211 120.8(3) . . ? C215 C216 H216 119.6 . . ? C211 C216 H216 119.6 . . ? C222 C221 C226 118.6(2) . . ? C222 C221 P2 118.5(2) . . ? C226 C221 P2 122.9(2) . . ? C221 C222 C223 120.8(3) . . ? C221 C222 H222 119.6 . . ? C223 C222 H222 119.6 . . ? C224 C223 C222 120.1(3) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 119.7(3) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C224 C225 C226 120.4(3) . . ? C224 C225 H225 119.8 . . ? C226 C225 H225 119.8 . . ? C225 C226 C221 120.4(3) . . ? C225 C226 H226 119.8 . . ? C221 C226 H226 119.8 . . ? C45 C41 C42 99.4(8) . . ? C43 C42 C41 129.3(12) . . ? C42 C43 C44 129.7(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 C1 Pd P1 C111 -79.17(12) . . . . ? C2 Pd P1 C111 -76.99(17) . . . . ? P2 Pd P1 C111 96.28(9) . . . . ? C1 Pd P1 C101 38.89(12) . . . . ? C2 Pd P1 C101 41.07(17) . . . . ? P2 Pd P1 C101 -145.66(9) . . . . ? C1 Pd P1 C121 159.94(14) . . . . ? C2 Pd P1 C121 162.12(17) . . . . ? P2 Pd P1 C121 -24.62(11) . . . . ? C1 Pd P2 C201 118.31(18) . . . . ? C2 Pd P2 C201 123.24(12) . . . . ? P1 Pd P2 C201 -52.97(9) . . . . ? C1 Pd P2 C221 -117.84(18) . . . . ? C2 Pd P2 C221 -112.91(12) . . . . ? P1 Pd P2 C221 70.88(10) . . . . ? C1 Pd P2 C211 1.09(19) . . . . ? C2 Pd P2 C211 6.02(13) . . . . ? P1 Pd P2 C211 -170.19(10) . . . . ? C2 Pd C1 F2 110.4(3) . . . . ? P2 Pd C1 F2 117.5(2) . . . . ? P1 Pd C1 F2 -71.4(2) . . . . ? C2 Pd C1 F1 -110.9(3) . . . . ? P2 Pd C1 F1 -103.7(2) . . . . ? P1 Pd C1 F1 67.4(2) . . . . ? P2 Pd C1 C2 7.1(2) . . . . ? P1 Pd C1 C2 178.23(13) . . . . ? F2 C1 C2 F4 -0.7(3) . . . . ? F1 C1 C2 F4 -131.1(2) . . . . ? Pd C1 C2 F4 115.0(2) . . . . ? F2 C1 C2 F3 130.7(2) . . . . ? F1 C1 C2 F3 0.4(4) . . . . ? Pd C1 C2 F3 -113.5(2) . . . . ? F2 C1 C2 Pd -115.7(2) . . . . ? F1 C1 C2 Pd 114.0(2) . . . . ? C1 Pd C2 F4 -111.0(3) . . . . ? P2 Pd C2 F4 72.8(2) . . . . ? P1 Pd C2 F4 -114.1(2) . . . . ? C1 Pd C2 F3 111.3(3) . . . . ? P2 Pd C2 F3 -65.0(2) . . . . ? P1 Pd C2 F3 108.1(2) . . . . ? P2 Pd C2 C1 -176.24(13) . . . . ? P1 Pd C2 C1 -3.2(2) . . . . ? C111 P1 C101 C106 161.2(2) . . . . ? C121 P1 C101 C106 -91.0(2) . . . . ? Pd P1 C101 C106 39.7(2) . . . . ? C111 P1 C101 C102 -18.6(3) . . . . ? C121 P1 C101 C102 89.3(2) . . . . ? Pd P1 C101 C102 -140.0(2) . . . . ? C106 C101 C102 C103 -2.4(4) . . . . ? P1 C101 C102 C103 177.3(2) . . . . ? C101 C102 C103 C104 1.4(4) . . . . ? C102 C103 C104 C105 1.3(4) . . . . ? C103 C104 C105 C106 -3.0(4) . . . . ? C104 C105 C106 C101 2.1(4) . . . . ? C102 C101 C106 C105 0.6(4) . . . . ? P1 C101 C106 C105 -179.1(2) . . . . ? C101 P1 C111 C116 75.1(2) . . . . ? C121 P1 C111 C116 -33.1(3) . . . . ? Pd P1 C111 C116 -163.8(2) . . . . ? C101 P1 C111 C112 -107.4(2) . . . . ? C121 P1 C111 C112 144.5(2) . . . . ? Pd P1 C111 C112 13.8(2) . . . . ? C116 C111 C112 C113 0.8(4) . . . . ? P1 C111 C112 C113 -176.8(2) . . . . ? C111 C112 C113 C114 -0.3(5) . . . . ? C112 C113 C114 C115 -0.7(5) . . . . ? C113 C114 C115 C116 1.2(5) . . . . ? C114 C115 C116 C111 -0.6(4) . . . . ? C112 C111 C116 C115 -0.4(4) . . . . ? P1 C111 C116 C115 177.2(2) . . . . ? C111 P1 C121 C122 139.0(2) . . . . ? C101 P1 C121 C122 28.9(3) . . . . ? Pd P1 C121 C122 -95.9(2) . . . . ? C111 P1 C121 C126 -47.4(2) . . . . ? C101 P1 C121 C126 -157.6(2) . . . . ? Pd P1 C121 C126 77.6(2) . . . . ? C126 C121 C122 C123 -0.7(5) . . . . ? P1 C121 C122 C123 172.8(3) . . . . ? C121 C122 C123 C124 -0.6(5) . . . . ? C122 C123 C124 C125 1.4(6) . . . . ? C123 C124 C125 C126 -1.1(5) . . . . ? C124 C125 C126 C121 -0.2(5) . . . . ? C122 C121 C126 C125 1.1(4) . . . . ? P1 C121 C126 C125 -172.7(2) . . . . ? C221 P2 C201 C202 -169.1(2) . . . . ? C211 P2 C201 C202 83.7(2) . . . . ? Pd P2 C201 C202 -41.0(2) . . . . ? C221 P2 C201 C206 9.2(3) . . . . ? C211 P2 C201 C206 -98.0(2) . . . . ? Pd P2 C201 C206 137.3(2) . . . . ? C206 C201 C202 C203 0.1(4) . . . . ? P2 C201 C202 C203 178.5(2) . . . . ? C201 C202 C203 C204 -0.6(5) . . . . ? C202 C203 C204 C205 0.5(5) . . . . ? C203 C204 C205 C206 0.1(5) . . . . ? C204 C205 C206 C201 -0.5(5) . . . . ? C202 C201 C206 C205 0.4(4) . . . . ? P2 C201 C206 C205 -177.8(2) . . . . ? C201 P2 C211 C212 4.9(3) . . . . ? C221 P2 C211 C212 -106.9(2) . . . . ? Pd P2 C211 C212 126.8(2) . . . . ? C201 P2 C211 C216 -175.8(2) . . . . ? C221 P2 C211 C216 72.3(2) . . . . ? Pd P2 C211 C216 -54.0(2) . . . . ? C216 C211 C212 C213 -1.7(4) . . . . ? P2 C211 C212 C213 177.5(2) . . . . ? C211 C212 C213 C214 0.0(4) . . . . ? C212 C213 C214 C215 1.4(5) . . . . ? C213 C214 C215 C216 -1.0(5) . . . . ? C214 C215 C216 C211 -0.7(5) . . . . ? C212 C211 C216 C215 2.0(4) . . . . ? P2 C211 C216 C215 -177.2(2) . . . . ? C201 P2 C221 C222 119.3(2) . . . . ? C211 P2 C221 C222 -132.7(2) . . . . ? Pd P2 C221 C222 -6.3(3) . . . . ? C201 P2 C221 C226 -63.5(2) . . . . ? C211 P2 C221 C226 44.5(3) . . . . ? Pd P2 C221 C226 170.9(2) . . . . ? C226 C221 C222 C223 0.3(4) . . . . ? P2 C221 C222 C223 177.6(2) . . . . ? C221 C222 C223 C224 0.7(5) . . . . ? C222 C223 C224 C225 -0.7(5) . . . . ? C223 C224 C225 C226 -0.2(5) . . . . ? C224 C225 C226 C221 1.2(5) . . . . ? C222 C221 C226 C225 -1.2(4) . . . . ? P2 C221 C226 C225 -178.4(2) . . . . ? C45 C41 C42 C43 -5.9(11) . . . . ? C41 C42 C43 C44 7.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.554 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.078 #===End of TFE-Pd data_CF2CFPd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H30 F3 I P2 Pd' _chemical_formula_sum 'C38 H30 F3 I P2 Pd' _chemical_formula_weight 838.86 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-p 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 12.0400(12) _cell_length_b 22.7606(18) _cell_length_c 13.3116(13) _cell_angle_alpha 90.00 _cell_angle_beta 110.433(2) _cell_angle_gamma 90.00 _cell_volume 3418.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6927 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 25.29 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.582 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; Higashi, T. (1999). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'imaging plate' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17905 _diffrn_reflns_av_R_equivalents 0.1560 _diffrn_reflns_av_sigmaI/netI 0.1737 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6170 _reflns_number_gt 3059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1999)' _computing_structure_solution 'PATTY (Bueskens, et al., 1994)' _computing_publication_material 'SHELXL-97 and modified' _computing_molecular_graphics 'Ortep-3 (Louis J. Farrugia, 1999)' # Carroll K. Johnson and M. N. Burnett, ORNL-6895, ORTEP-III(version 1.0.2), # A FORTRAN Thermal-Ellipsoid Plot Program, Oak Ridge National Labratory, # Oak Ridge, Tennessee. # Ortep-3 for Windows, Version 1.05 Louis J. Farrugia, _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^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6170 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1727 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.00781(6) 0.14508(3) 0.19035(7) 0.0387(3) Uani 1 1 d . . . I I 0.06323(6) 0.03189(3) 0.21952(7) 0.0510(3) Uani 1 1 d . . . P1 P 0.1975(2) 0.16819(11) 0.1948(2) 0.0371(7) Uani 1 1 d . . . P2 P -0.1863(2) 0.12483(11) 0.1804(2) 0.0406(7) Uani 1 1 d . . . F1 F -0.0675(6) 0.2553(3) 0.0690(5) 0.077(2) Uani 1 1 d . . . F2 F -0.0495(6) 0.3261(3) 0.2322(6) 0.088(2) Uani 1 1 d . . . F3 F 0.0137(7) 0.2535(3) 0.3470(6) 0.091(2) Uani 1 1 d . . . C1 C -0.0284(9) 0.2308(5) 0.1735(11) 0.060(3) Uani 1 1 d . . . C2 C -0.0231(11) 0.2684(5) 0.2406(12) 0.064(4) Uani 1 1 d . . . C101 C 0.3141(9) 0.1298(4) 0.2994(9) 0.040(3) Uani 1 1 d . . . C102 C 0.3071(10) 0.1261(5) 0.4011(10) 0.061(3) Uani 1 1 d . . . H102 H 0.2393 0.1419 0.4123 0.073 Uiso 1 1 calc R . . C103 C 0.3938(11) 0.1007(5) 0.4863(10) 0.065(4) Uani 1 1 d . . . H103 H 0.3881 0.1000 0.5556 0.078 Uiso 1 1 calc R . . C104 C 0.4901(13) 0.0760(5) 0.4676(12) 0.076(5) Uani 1 1 d . . . H104 H 0.5493 0.0565 0.5245 0.092 Uiso 1 1 calc R . . C105 C 0.5015(10) 0.0789(5) 0.3707(12) 0.063(4) Uani 1 1 d . . . H105 H 0.5691 0.0625 0.3602 0.076 Uiso 1 1 calc R . . C106 C 0.4139(9) 0.1062(4) 0.2857(9) 0.050(3) Uani 1 1 d . . . H106 H 0.4228 0.1086 0.2177 0.060 Uiso 1 1 calc R . . C111 C 0.2199(8) 0.1519(4) 0.0710(8) 0.036(3) Uani 1 1 d . . . C112 C 0.3122(9) 0.1771(4) 0.0438(9) 0.043(3) Uani 1 1 d . . . H112 H 0.3670 0.2020 0.0946 0.051 Uiso 1 1 calc R . . C113 C 0.3268(9) 0.1676(5) -0.0511(9) 0.051(3) Uani 1 1 d . . . H113 H 0.3879 0.1870 -0.0680 0.061 Uiso 1 1 calc R . . C114 C 0.2518(10) 0.1296(5) -0.1223(9) 0.056(3) Uani 1 1 d . . . H114 H 0.2629 0.1217 -0.1882 0.067 Uiso 1 1 calc R . . C115 C 0.1620(10) 0.1028(4) -0.1012(9) 0.047(3) Uani 1 1 d . . . H115 H 0.1105 0.0770 -0.1526 0.057 Uiso 1 1 calc R . . C116 C 0.1449(8) 0.1127(4) -0.0060(9) 0.043(3) Uani 1 1 d . . . H116 H 0.0823 0.0933 0.0085 0.051 Uiso 1 1 calc R . . C121 C 0.2432(8) 0.2453(4) 0.2167(9) 0.041(3) Uani 1 1 d . . . C122 C 0.3131(9) 0.2647(4) 0.3180(9) 0.048(3) Uani 1 1 d . . . H122 H 0.3399 0.2382 0.3767 0.058 Uiso 1 1 calc R . . C123 C 0.3430(11) 0.3245(6) 0.3313(11) 0.070(4) Uani 1 1 d . . . H123 H 0.3895 0.3388 0.4002 0.085 Uiso 1 1 calc R . . C124 C 0.3068(11) 0.3623(5) 0.2473(14) 0.070(4) Uani 1 1 d . . . H124 H 0.3277 0.4027 0.2579 0.084 Uiso 1 1 calc R . . C125 C 0.2399(11) 0.3423(6) 0.1471(12) 0.074(4) Uani 1 1 d . . . H125 H 0.2171 0.3685 0.0878 0.089 Uiso 1 1 calc R . . C126 C 0.2064(9) 0.2852(5) 0.1330(10) 0.055(3) Uani 1 1 d . . . H126 H 0.1566 0.2723 0.0642 0.066 Uiso 1 1 calc R . . C201 C -0.2763(9) 0.0881(4) 0.0593(8) 0.037(3) Uani 1 1 d . . . C202 C -0.3990(9) 0.0874(5) 0.0288(10) 0.058(3) Uani 1 1 d . . . H202 H -0.4349 0.1077 0.0718 0.070 Uiso 1 1 calc R . . C203 C -0.4706(11) 0.0586(6) -0.0613(11) 0.078(4) Uani 1 1 d . . . H203 H -0.5540 0.0576 -0.0781 0.093 Uiso 1 1 calc R . . C204 C -0.4195(10) 0.0308(5) -0.1277(10) 0.062(4) Uani 1 1 d . . . H204 H -0.4675 0.0123 -0.1922 0.074 Uiso 1 1 calc R . . C205 C -0.3005(10) 0.0306(4) -0.0986(9) 0.051(3) Uani 1 1 d . . . H205 H -0.2647 0.0100 -0.1414 0.061 Uiso 1 1 calc R . . C206 C -0.2290(10) 0.0598(4) -0.0074(9) 0.048(3) Uani 1 1 d . . . H206 H -0.1456 0.0603 0.0091 0.058 Uiso 1 1 calc R . . C211 C -0.1873(9) 0.0774(4) 0.2901(9) 0.045(3) Uani 1 1 d . . . C212 C -0.2426(9) 0.0227(5) 0.2719(9) 0.051(3) Uani 1 1 d . . . H212 H -0.2851 0.0099 0.2008 0.061 Uiso 1 1 calc R . . C213 C -0.2348(9) -0.0124(5) 0.3572(10) 0.059(3) Uani 1 1 d . . . H213 H -0.2712 -0.0500 0.3433 0.071 Uiso 1 1 calc R . . C214 C -0.1763(10) 0.0039(6) 0.4638(10) 0.065(4) Uani 1 1 d . . . H214 H -0.1761 -0.0203 0.5220 0.078 Uiso 1 1 calc R . . C215 C -0.1180(9) 0.0581(6) 0.4794(10) 0.066(4) Uani 1 1 d . . . H215 H -0.0744 0.0709 0.5502 0.079 Uiso 1 1 calc R . . C216 C -0.1229(10) 0.0931(5) 0.3935(10) 0.059(3) Uani 1 1 d . . . H216 H -0.0805 0.1292 0.4063 0.070 Uiso 1 1 calc R . . C221 C -0.2800(8) 0.1864(4) 0.1880(10) 0.044(3) Uani 1 1 d . . . C222 C -0.3149(9) 0.2263(5) 0.1023(10) 0.064(4) Uani 1 1 d . . . H222 H -0.2881 0.2214 0.0436 0.077 Uiso 1 1 calc R . . C223 C -0.3898(10) 0.2737(5) 0.1038(12) 0.070(4) Uani 1 1 d . . . H223 H -0.4106 0.3021 0.0481 0.084 Uiso 1 1 calc R . . C224 C -0.4320(10) 0.2782(6) 0.1860(13) 0.072(4) Uani 1 1 d . . . H224 H -0.4855 0.3092 0.1848 0.087 Uiso 1 1 calc R . . C225 C -0.3998(10) 0.2394(6) 0.2710(11) 0.067(4) Uani 1 1 d . . . H225 H -0.4287 0.2439 0.3285 0.080 Uiso 1 1 calc R . . C226 C -0.3250(9) 0.1941(5) 0.2704(10) 0.056(3) Uani 1 1 d . . . H226 H -0.3031 0.1670 0.3283 0.067 Uiso 1 1 calc R . . 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 Pd 0.0330(4) 0.0366(5) 0.0466(5) 0.0005(4) 0.0140(4) -0.0001(4) I 0.0436(4) 0.0388(4) 0.0750(6) 0.0062(4) 0.0264(4) 0.0029(3) P1 0.0361(15) 0.0347(14) 0.0382(17) 0.0000(13) 0.0101(13) -0.0030(12) P2 0.0349(15) 0.0427(16) 0.0424(19) -0.0032(14) 0.0111(13) 0.0006(12) F1 0.096(5) 0.082(5) 0.047(5) 0.013(4) 0.018(4) 0.005(4) F2 0.122(6) 0.045(4) 0.116(6) -0.011(4) 0.066(5) 0.010(4) F3 0.132(7) 0.090(6) 0.053(5) -0.015(4) 0.034(5) 0.013(5) C1 0.045(7) 0.066(8) 0.076(10) -0.014(8) 0.031(7) -0.006(6) C2 0.078(9) 0.056(8) 0.074(10) -0.003(8) 0.049(8) 0.017(7) C101 0.041(6) 0.033(6) 0.040(7) 0.002(5) 0.008(5) -0.007(5) C102 0.046(7) 0.076(9) 0.052(9) 0.013(7) 0.006(7) 0.002(6) C103 0.058(8) 0.092(10) 0.037(8) 0.013(7) 0.006(7) -0.018(7) C104 0.074(10) 0.049(8) 0.084(12) 0.034(8) -0.001(9) 0.002(7) C105 0.045(7) 0.060(8) 0.074(10) 0.002(8) 0.006(8) 0.006(6) C106 0.049(7) 0.050(7) 0.049(8) 0.009(6) 0.015(6) -0.001(6) C111 0.025(5) 0.048(6) 0.031(6) 0.009(5) 0.006(5) 0.009(5) C112 0.046(7) 0.039(6) 0.042(7) -0.008(5) 0.015(6) -0.006(5) C113 0.045(7) 0.060(7) 0.056(9) -0.001(6) 0.027(6) 0.001(6) C114 0.049(7) 0.081(9) 0.046(8) 0.006(7) 0.026(6) 0.003(6) C115 0.049(7) 0.052(7) 0.041(8) -0.016(6) 0.017(6) 0.006(6) C116 0.034(6) 0.039(6) 0.048(7) -0.002(6) 0.005(6) 0.003(5) C121 0.032(6) 0.043(6) 0.045(7) -0.005(6) 0.011(5) -0.004(5) C122 0.056(7) 0.028(6) 0.062(8) -0.005(6) 0.022(6) -0.013(5) C123 0.070(9) 0.072(9) 0.073(10) -0.036(8) 0.030(8) -0.027(7) C124 0.071(9) 0.035(7) 0.125(14) 0.006(9) 0.059(10) 0.002(7) C125 0.062(9) 0.078(10) 0.083(11) 0.015(9) 0.024(8) -0.009(7) C126 0.050(7) 0.041(7) 0.067(9) 0.011(7) 0.012(6) -0.009(6) C201 0.033(6) 0.051(6) 0.025(6) 0.002(5) 0.006(5) -0.001(5) C202 0.038(7) 0.073(8) 0.064(9) -0.027(7) 0.019(6) 0.003(6) C203 0.048(8) 0.093(10) 0.079(11) -0.013(9) 0.005(8) 0.006(7) C204 0.050(8) 0.064(8) 0.052(8) -0.016(7) -0.007(7) 0.013(6) C205 0.063(8) 0.050(7) 0.043(7) -0.009(6) 0.023(6) 0.002(6) C206 0.050(7) 0.052(7) 0.051(8) 0.003(6) 0.029(6) -0.011(6) C211 0.047(7) 0.046(7) 0.044(8) 0.001(6) 0.019(6) 0.009(5) C212 0.049(7) 0.055(7) 0.045(8) 0.005(6) 0.012(6) -0.002(6) C213 0.053(7) 0.060(8) 0.066(10) 0.012(7) 0.025(7) 0.001(6) C214 0.055(8) 0.081(9) 0.060(10) 0.024(8) 0.020(7) 0.019(7) C215 0.038(7) 0.102(10) 0.055(9) -0.009(8) 0.014(6) -0.004(7) C216 0.055(8) 0.082(9) 0.045(8) 0.010(7) 0.024(7) 0.003(6) C221 0.029(6) 0.037(6) 0.060(8) 0.000(6) 0.008(6) 0.001(5) C222 0.057(8) 0.068(8) 0.058(9) -0.014(7) 0.008(7) 0.010(6) C223 0.043(7) 0.047(7) 0.097(12) 0.003(7) -0.003(8) 0.019(6) C224 0.036(7) 0.074(9) 0.104(13) -0.038(9) 0.020(8) 0.012(6) C225 0.049(8) 0.074(9) 0.068(10) -0.024(8) 0.008(7) 0.000(7) C226 0.043(7) 0.062(8) 0.070(9) -0.012(7) 0.029(7) 0.000(6) _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 Pd C1 1.994(12) . ? Pd P1 2.325(3) . ? Pd P2 2.339(3) . ? Pd I 2.6557(10) . ? P1 C111 1.799(10) . ? P1 C101 1.819(10) . ? P1 C121 1.831(10) . ? P2 C201 1.803(10) . ? P2 C211 1.821(11) . ? P2 C221 1.825(10) . ? F1 C1 1.418(13) . ? F2 C2 1.345(12) . ? F3 C2 1.371(14) . ? C1 C2 1.223(15) . ? C101 C106 1.385(14) . ? C101 C102 1.388(15) . ? C102 C103 1.372(14) . ? C102 H102 0.9500 . ? C103 C104 1.386(17) . ? C103 H103 0.9500 . ? C104 C105 1.346(17) . ? C104 H104 0.9500 . ? C105 C106 1.394(14) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C111 C112 1.406(13) . ? C111 C116 1.419(12) . ? C112 C113 1.353(14) . ? C112 H112 0.9500 . ? C113 C114 1.365(14) . ? C113 H113 0.9500 . ? C114 C115 1.353(14) . ? C114 H114 0.9500 . ? C115 C116 1.372(14) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.385(13) . ? C121 C122 1.389(13) . ? C122 C123 1.404(14) . ? C122 H122 0.9500 . ? C123 C124 1.355(16) . ? C123 H123 0.9500 . ? C124 C125 1.372(17) . ? C124 H124 0.9500 . ? C125 C126 1.354(14) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C201 C206 1.371(14) . ? C201 C202 1.388(13) . ? C202 C203 1.375(14) . ? C202 H202 0.9500 . ? C203 C204 1.393(16) . ? C203 H203 0.9500 . ? C204 C205 1.347(14) . ? C204 H204 0.9500 . ? C205 C206 1.389(13) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C211 C216 1.371(14) . ? C211 C212 1.392(13) . ? C212 C213 1.364(14) . ? C212 H212 0.9500 . ? C213 C214 1.396(15) . ? C213 H213 0.9500 . ? C214 C215 1.399(16) . ? C214 H214 0.9500 . ? C215 C216 1.377(15) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.394(15) . ? C221 C222 1.402(15) . ? C222 C223 1.412(14) . ? C222 H222 0.9500 . ? C223 C224 1.361(18) . ? C223 H223 0.9500 . ? C224 C225 1.381(17) . ? C224 H224 0.9500 . ? C225 C226 1.369(14) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? 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 Pd P1 87.5(3) . . ? C1 Pd P2 90.6(3) . . ? P1 Pd P2 177.60(10) . . ? C1 Pd I 177.8(4) . . ? P1 Pd I 91.22(7) . . ? P2 Pd I 90.70(7) . . ? C111 P1 C101 106.2(5) . . ? C111 P1 C121 102.2(5) . . ? C101 P1 C121 103.3(4) . . ? C111 P1 Pd 112.9(3) . . ? C101 P1 Pd 113.6(4) . . ? C121 P1 Pd 117.3(3) . . ? C201 P2 C211 105.8(5) . . ? C201 P2 C221 102.4(5) . . ? C211 P2 C221 103.5(5) . . ? C201 P2 Pd 114.8(4) . . ? C211 P2 Pd 111.0(3) . . ? C221 P2 Pd 118.1(3) . . ? C2 C1 F1 110.8(12) . . ? C2 C1 Pd 130.5(12) . . ? F1 C1 Pd 118.7(8) . . ? C1 C2 F2 132.2(14) . . ? C1 C2 F3 119.8(12) . . ? F2 C2 F3 108.0(11) . . ? C106 C101 C102 117.1(10) . . ? C106 C101 P1 124.0(9) . . ? C102 C101 P1 118.8(9) . . ? C103 C102 C101 122.9(12) . . ? C103 C102 H102 118.5 . . ? C101 C102 H102 118.5 . . ? C102 C103 C104 117.7(13) . . ? C102 C103 H103 121.1 . . ? C104 C103 H103 121.1 . . ? C105 C104 C103 121.5(12) . . ? C105 C104 H104 119.2 . . ? C103 C104 H104 119.2 . . ? C104 C105 C106 119.9(13) . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C101 C106 C105 120.8(12) . . ? C101 C106 H106 119.6 . . ? C105 C106 H106 119.6 . . ? C112 C111 C116 115.5(10) . . ? C112 C111 P1 122.4(8) . . ? C116 C111 P1 122.0(8) . . ? C113 C112 C111 123.2(10) . . ? C113 C112 H112 118.4 . . ? C111 C112 H112 118.4 . . ? C112 C113 C114 118.6(11) . . ? C112 C113 H113 120.7 . . ? C114 C113 H113 120.7 . . ? C115 C114 C113 121.6(12) . . ? C115 C114 H114 119.2 . . ? C113 C114 H114 119.2 . . ? C114 C115 C116 120.4(11) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.5(10) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C126 C121 C122 119.1(9) . . ? C126 C121 P1 120.5(8) . . ? C122 C121 P1 120.4(8) . . ? C121 C122 C123 118.2(10) . . ? C121 C122 H122 120.9 . . ? C123 C122 H122 120.9 . . ? C124 C123 C122 121.1(12) . . ? C124 C123 H123 119.4 . . ? C122 C123 H123 119.4 . . ? C123 C124 C125 120.1(11) . . ? C123 C124 H124 119.9 . . ? C125 C124 H124 119.9 . . ? C126 C125 C124 119.8(12) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? C125 C126 C121 121.5(11) . . ? C125 C126 H126 119.3 . . ? C121 C126 H126 119.3 . . ? C206 C201 C202 116.5(10) . . ? C206 C201 P2 122.7(8) . . ? C202 C201 P2 120.9(9) . . ? C203 C202 C201 122.7(11) . . ? C203 C202 H202 118.7 . . ? C201 C202 H202 118.7 . . ? C202 C203 C204 119.2(11) . . ? C202 C203 H203 120.4 . . ? C204 C203 H203 120.4 . . ? C205 C204 C203 118.7(11) . . ? C205 C204 H204 120.6 . . ? C203 C204 H204 120.6 . . ? C204 C205 C206 121.5(11) . . ? C204 C205 H205 119.2 . . ? C206 C205 H205 119.2 . . ? C201 C206 C205 121.3(10) . . ? C201 C206 H206 119.4 . . ? C205 C206 H206 119.4 . . ? C216 C211 C212 118.5(10) . . ? C216 C211 P2 119.4(9) . . ? C212 C211 P2 121.8(9) . . ? C213 C212 C211 119.2(11) . . ? C213 C212 H212 120.4 . . ? C211 C212 H212 120.4 . . ? C212 C213 C214 123.7(11) . . ? C212 C213 H213 118.1 . . ? C214 C213 H213 118.1 . . ? C213 C214 C215 115.7(12) . . ? C213 C214 H214 122.1 . . ? C215 C214 H214 122.1 . . ? C216 C215 C214 120.9(12) . . ? C216 C215 H215 119.6 . . ? C214 C215 H215 119.6 . . ? C211 C216 C215 121.8(12) . . ? C211 C216 H216 119.1 . . ? C215 C216 H216 119.1 . . ? C226 C221 C222 118.1(10) . . ? C226 C221 P2 124.0(9) . . ? C222 C221 P2 117.8(10) . . ? C221 C222 C223 119.6(13) . . ? C221 C222 H222 120.2 . . ? C223 C222 H222 120.2 . . ? C224 C223 C222 119.3(13) . . ? C224 C223 H223 120.4 . . ? C222 C223 H223 120.4 . . ? C223 C224 C225 122.2(12) . . ? C223 C224 H224 118.9 . . ? C225 C224 H224 118.9 . . ? C226 C225 C224 118.3(13) . . ? C226 C225 H225 120.8 . . ? C224 C225 H225 120.8 . . ? C225 C226 C221 122.4(12) . . ? C225 C226 H226 118.8 . . ? C221 C226 H226 118.8 . . ? 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 C1 Pd P1 C111 -103.4(5) . . . . ? I Pd P1 C111 78.4(3) . . . . ? C1 Pd P1 C101 135.5(5) . . . . ? I Pd P1 C101 -42.7(4) . . . . ? C1 Pd P1 C121 15.1(6) . . . . ? I Pd P1 C121 -163.1(4) . . . . ? C1 Pd P2 C201 109.9(5) . . . . ? I Pd P2 C201 -71.9(3) . . . . ? C1 Pd P2 C211 -130.3(6) . . . . ? I Pd P2 C211 47.9(4) . . . . ? C1 Pd P2 C221 -11.1(6) . . . . ? I Pd P2 C221 167.1(4) . . . . ? P1 Pd C1 C2 -93.9(12) . . . . ? P2 Pd C1 C2 87.6(12) . . . . ? P1 Pd C1 F1 86.3(7) . . . . ? P2 Pd C1 F1 -92.2(7) . . . . ? F1 C1 C2 F2 2(2) . . . . ? Pd C1 C2 F2 -178.1(9) . . . . ? F1 C1 C2 F3 -179.6(9) . . . . ? Pd C1 C2 F3 0.6(19) . . . . ? C111 P1 C101 C106 14.4(9) . . . . ? C121 P1 C101 C106 -92.7(9) . . . . ? Pd P1 C101 C106 139.2(8) . . . . ? C111 P1 C101 C102 -169.0(8) . . . . ? C121 P1 C101 C102 83.9(9) . . . . ? Pd P1 C101 C102 -44.2(9) . . . . ? C106 C101 C102 C103 0.2(16) . . . . ? P1 C101 C102 C103 -176.6(9) . . . . ? C101 C102 C103 C104 -2.3(18) . . . . ? C102 C103 C104 C105 2.9(19) . . . . ? C103 C104 C105 C106 -1.4(19) . . . . ? C102 C101 C106 C105 1.4(15) . . . . ? P1 C101 C106 C105 178.0(8) . . . . ? C104 C105 C106 C101 -0.8(17) . . . . ? C101 P1 C111 C112 -73.9(9) . . . . ? C121 P1 C111 C112 34.0(9) . . . . ? Pd P1 C111 C112 161.0(7) . . . . ? C101 P1 C111 C116 106.4(8) . . . . ? C121 P1 C111 C116 -145.7(7) . . . . ? Pd P1 C111 C116 -18.7(8) . . . . ? C116 C111 C112 C113 3.2(14) . . . . ? P1 C111 C112 C113 -176.6(8) . . . . ? C111 C112 C113 C114 -3.2(16) . . . . ? C112 C113 C114 C115 1.9(16) . . . . ? C113 C114 C115 C116 -0.8(16) . . . . ? C114 C115 C116 C111 0.9(15) . . . . ? C112 C111 C116 C115 -2.0(13) . . . . ? P1 C111 C116 C115 177.8(7) . . . . ? C111 P1 C121 C126 44.6(9) . . . . ? C101 P1 C121 C126 154.8(9) . . . . ? Pd P1 C121 C126 -79.5(9) . . . . ? C111 P1 C121 C122 -136.8(8) . . . . ? C101 P1 C121 C122 -26.6(10) . . . . ? Pd P1 C121 C122 99.1(8) . . . . ? C126 C121 C122 C123 0.3(16) . . . . ? P1 C121 C122 C123 -178.3(8) . . . . ? C121 C122 C123 C124 -1.2(18) . . . . ? C122 C123 C124 C125 -0.2(19) . . . . ? C123 C124 C125 C126 2(2) . . . . ? C124 C125 C126 C121 -3.3(19) . . . . ? C122 C121 C126 C125 1.9(17) . . . . ? P1 C121 C126 C125 -179.5(9) . . . . ? C211 P2 C201 C206 -105.5(9) . . . . ? C221 P2 C201 C206 146.5(9) . . . . ? Pd P2 C201 C206 17.2(10) . . . . ? C211 P2 C201 C202 74.9(9) . . . . ? C221 P2 C201 C202 -33.2(10) . . . . ? Pd P2 C201 C202 -162.5(8) . . . . ? C206 C201 C202 C203 2.1(17) . . . . ? P2 C201 C202 C203 -178.2(10) . . . . ? C201 C202 C203 C204 -2.8(19) . . . . ? C202 C203 C204 C205 3.2(19) . . . . ? C203 C204 C205 C206 -3.3(18) . . . . ? C202 C201 C206 C205 -2.1(15) . . . . ? P2 C201 C206 C205 178.2(8) . . . . ? C204 C205 C206 C201 2.8(17) . . . . ? C201 P2 C211 C216 178.2(8) . . . . ? C221 P2 C211 C216 -74.5(9) . . . . ? Pd P2 C211 C216 53.1(9) . . . . ? C201 P2 C211 C212 4.5(10) . . . . ? C221 P2 C211 C212 111.8(9) . . . . ? Pd P2 C211 C212 -120.6(8) . . . . ? C216 C211 C212 C213 2.5(16) . . . . ? P2 C211 C212 C213 176.3(8) . . . . ? C211 C212 C213 C214 1.6(17) . . . . ? C212 C213 C214 C215 -3.9(17) . . . . ? C213 C214 C215 C216 2.1(17) . . . . ? C212 C211 C216 C215 -4.3(17) . . . . ? P2 C211 C216 C215 -178.2(9) . . . . ? C214 C215 C216 C211 1.9(18) . . . . ? C201 P2 C221 C226 116.7(9) . . . . ? C211 P2 C221 C226 6.9(10) . . . . ? Pd P2 C221 C226 -116.1(8) . . . . ? C201 P2 C221 C222 -59.1(9) . . . . ? C211 P2 C221 C222 -168.9(8) . . . . ? Pd P2 C221 C222 68.1(8) . . . . ? C226 C221 C222 C223 2.4(15) . . . . ? P2 C221 C222 C223 178.4(8) . . . . ? C221 C222 C223 C224 -3.3(17) . . . . ? C222 C223 C224 C225 3.0(19) . . . . ? C223 C224 C225 C226 -1.6(18) . . . . ? C224 C225 C226 C221 0.6(17) . . . . ? C222 C221 C226 C225 -1.0(16) . . . . ? P2 C221 C226 C225 -176.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.974 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.145 #===End of CF2CFPd