# CIF-file generated for C63H57BF24N2Pd CP848 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date '2003-11-12 09:59:23' _audit_creation_method ; PLATON option SHELXL97-2 & Manual Editing ; _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Drs. A. Meetsma ; _publ_contact_author_address # Address of author for correspondence ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; _publ_contact_author_email A.Meetsma@fwn.rug.nl _publ_contact_author_fax '+31 50 3634441' _publ_contact_author_phone '+31 50 3634368' _publ_requested_journal 'JACS' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission : 2004-06-24 08:18:23 Consider this CIF submission for deposition of the third X-ray structure of a manuscript to be submitted to : JACS (Our Compound_Identification_Code : CP848) ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Meetsma, Auke' ; ? # author related footnote ; ; Crystal Structure Center, Inorganic Solid State Chemistry Laboratory Chemical Physics, Materials Science Center, Groningen University, Nijenborgh 4, NL-9747 AG Groningen, The Netherlands. ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; Refinement was frustrated by a configurational-disorder problem: from the solution it was clear that C19 an C130 positions were disordered. A disorder model with two alternative positions was used in the refinement. Some atoms showed unrealistic displacement parameters when allowed to vary anisotropically, suggesting dynamic disorder (dynamic means that the smeared electron density is due to fluctuations of the atomic positions within each unit cell) as a consequence of the rotational-disorder of some CF~3~ ligands. >From the solution it was clear that a pentane solvent molecule was highly disordered over an inversion center. The electron density appeared to be spread out, indicating transformational disorder. No satisfactory discrete model could be fitted in this density. The BYPASS (Sluis, 1990) procedure was used to take into account the electron density in the potential solvent area, which resulted in an electron count of 18 within a volume of 100.3 \%A^3^ in the unit cell (probably the cavities are partly occupied). ; # Insert blank lines between references _publ_section_references ; Beurskens, P.T., Beurskens, G., Gelder, R. de Garc\'ia-Granda, S. Gould, R.O. Isra\"el, & Smits, J.M.M. (1999). The DIRDIF99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bondi, A. (1964). J. Phys. Chem. 68, 441-451. Bruker, (2000). SMART, SAINT, SADABS, XPREP and SHELXTL/NT. Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA. International Tables for Crystallography (1983). Vol. A. Space-group symmetry, edited by T. Hahn. Dordrecht: Reidel. (Present distributor Kluwer Academic Publishers, Dordrecht). International Tables for Crystallography (1992). Vol. C. Edited by A.J.C Wilson, Kluwer Academic Publishers, Dordrecht, The Netherlands. Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269. Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984. Meetsma, A. (2003). Extended version of the program PLUTO. Groningen University, The Netherlands. (unpublished). Sheldrick, G.M. SHELXL97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany, 1997. Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction Program. University of G\"ottingen, Germany, 2001 Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1987). Acta Cryst. C43, 1233-1235. Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579. Spek, A.L. (1990). Acta Cryst. A46, C-34. Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66. ; _publ_section_figure_captions ; Fig. 1. Chemical structural diagram (scheme 1) of the title compound Fig. 2. Perspective PLUTO drawing of the molecule illustrating the configuration and the adopted numbering scheme. Fig. 3. Molecular packing viewed down unit cell axes. Fig. 4. Perspective ORTEP drawing of the title compound. Displacement ellipsoids for non-H are represented at the 50% probability level. The H-atoms have been omitted to improve clarity. ; #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H45 N2 Pd, C32 H12 B F24, 0.5(C5 H12)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C65.5 H63 B F24 N2 Pd' _chemical_formula_iupac ? _chemical_formula_weight 1451.43 _chemical_compound_source 'see text' 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' N N 0.0061 0.0033 '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' B B 0.0013 0.0007 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.6191(5) _cell_length_b 14.6417(6) _cell_length_c 18.3813(8) _cell_angle_alpha 108.590(1) _cell_angle_beta 95.619(1) _cell_angle_gamma 94.228(1) _cell_volume 3183.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9490 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.30 _cell_special_details ; The final unit cell was obtained from the xyz centroids of 9490 reflections after integration using the SAINT software package (Bruker, 2000). ; _exptl_crystal_description 'platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1474 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type 'Multi-Scan' _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000))' _exptl_absorpt_correction_T_min 0.8814 _exptl_absorpt_correction_T_max 0.9571 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube ' _diffrn_radiation_monochromator 'parallel mounted graphite' _diffrn_radiation_detector ; CCD area-detector ; _diffrn_measurement_device_type ; Bruker Smart Apex ; _diffrn_measurement_method 'phi and omega scans' _diffrn_special_details ; Crystal into the cold nitrogen stream of the low-temparature unit (KRYOFLEX, (Bruker, 2000)). ; _diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 29404 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_reduction_process ; Intensity data were corrected for Lorentz and polarization effects, decay and absorption and reduced to F~o~^2^ using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001) ; # number of unique reflections _reflns_number_total 15198 _reflns_number_gt 11959 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART, Bruker Version 5.624, 2001' _computing_cell_refinement 'SAINT, Bruker Version 6.02A, 2000' _computing_data_reduction 'XPREP, Bruker Version 5.1/NT, 2000' _computing_structure_solution ; DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; PLUTO (Meetsma, 2003) PLATON (Spek, 1994) ; _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.1015P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _chemical_absolute_configuration ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 15198 _refine_ls_number_parameters 851 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.773 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.098 _vrn_publ_code_squeezed_elec 18 _vrn_publ_code_void_volume 100.3 _vrn_publ_code_frame_time_sec 10.0 _vrn_publ_code_meas_time_hour 8.0 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd11 Pd Uani 0.04459(2) 0.28205(2) 0.31278(1) 1.000 0.0297(1) . . N11 N Uani 0.03673(19) 0.38764(16) 0.25853(13) 1.000 0.0286(7) . . N12 N Uani 0.08520(19) 0.21088(16) 0.20244(13) 1.000 0.0283(7) . . C11 C Uani -0.0097(2) 0.4763(2) 0.29314(16) 1.000 0.0291(8) . . C12 C Uani -0.1211(3) 0.4719(2) 0.2816(2) 1.000 0.0454(10) . . C13 C Uani -0.1680(3) 0.5537(2) 0.3214(2) 1.000 0.0407(10) . . C14 C Uani -0.1065(3) 0.6360(2) 0.37012(17) 1.000 0.0361(9) . . C15 C Uani 0.0038(3) 0.6391(2) 0.38005(17) 1.000 0.0360(9) . . C16 C Uani 0.0549(2) 0.5588(2) 0.34130(17) 1.000 0.0322(8) . . C17 C Uani -0.1917(3) 0.3829(3) 0.2292(4) 1.000 0.097(2) . . C18 C Uani -0.2618(5) 0.3380(4) 0.2708(4) 1.000 0.118(3) . . C110 C Uani 0.1766(3) 0.5640(2) 0.3538(2) 1.000 0.0417(10) . . C111 C Uani 0.2296(3) 0.6454(3) 0.3322(2) 1.000 0.0564(13) . . C112 C Uani 0.2162(3) 0.5766(5) 0.4386(3) 1.000 0.087(2) . . C113 C Uani 0.0696(2) 0.3644(2) 0.19187(15) 1.000 0.0293(8) . . C114 C Uani 0.0725(3) 0.4302(2) 0.14301(17) 1.000 0.0342(9) . . C115 C Uani 0.0974(2) 0.2638(2) 0.15952(16) 1.000 0.0292(8) . . C116 C Uani 0.1304(3) 0.2297(2) 0.07975(16) 1.000 0.0369(9) . . C117 C Uani 0.0944(3) 0.1072(2) 0.17577(16) 1.000 0.0316(8) . . C118 C Uani 0.1945(3) 0.0728(2) 0.17643(16) 1.000 0.0338(9) . . C119 C Uani 0.1952(3) -0.0275(2) 0.1546(2) 1.000 0.0484(11) . . C120 C Uani 0.1021(4) -0.0893(3) 0.1339(3) 1.000 0.0605(15) . . C121 C Uani 0.0032(3) -0.0536(3) 0.1336(2) 1.000 0.0512(11) . . C122 C Uani -0.0028(3) 0.0466(2) 0.15617(18) 1.000 0.0395(10) . . C123 C Uani 0.2982(2) 0.1407(2) 0.20169(16) 1.000 0.0335(9) . . C124 C Uani 0.3978(3) 0.0932(3) 0.1723(2) 1.000 0.0491(12) . . C125 C Uani 0.3179(3) 0.1852(3) 0.29052(18) 1.000 0.0452(11) . . C126 C Uani -0.1106(3) 0.0857(3) 0.1552(2) 1.000 0.0484(11) . . C127 C Uani -0.1975(4) 0.0271(4) 0.1801(3) 1.000 0.0762(19) . . C128 C Uani -0.1499(4) 0.0917(4) 0.0763(3) 1.000 0.081(2) . . C129 C Uani 0.0076(4) 0.3460(3) 0.4259(2) 1.000 0.0621(14) . . C131 C Uani 0.0555(4) 0.1848(3) 0.3765(2) 1.000 0.0673(16) . . C191 C Uani -0.2721(4) 0.4140(4) 0.1658(3) 0.666(11) 0.0519(19) . . C192 C Uani -0.2009(16) 0.3428(15) 0.1632(10) 0.334(11) 0.103(8) . . C1301 C Uani 0.0571(19) 0.2727(9) 0.4233(6) 0.49(2) 0.066(5) . . C1302 C Uani -0.0082(12) 0.2505(7) 0.4092(5) 0.51(2) 0.041(3) . . H13 H Uiso -0.24377 0.55255 0.31468 1.000 0.0488 . . H14 H Uiso -0.13994 0.69067 0.39700 1.000 0.0433 . . H15 H Uiso 0.04572 0.69630 0.41354 1.000 0.0432 . . H18 H Uiso -0.31134 0.38363 0.29489 1.000 0.1769 . . H18' H Uiso -0.21806 0.32148 0.31090 1.000 0.1769 . . H18" H Uiso -0.30275 0.27896 0.23429 1.000 0.1769 . . H110 H Uiso 0.19816 0.50158 0.32033 1.000 0.0500 . . H111 H Uiso 0.20614 0.63625 0.27770 1.000 0.0845 . . H111' H Uiso 0.30756 0.64556 0.34014 1.000 0.0845 . . H111" H Uiso 0.20967 0.70732 0.36471 1.000 0.0845 . . H112 H Uiso 0.29098 0.56285 0.44293 1.000 0.1301 . . H112' H Uiso 0.17187 0.53170 0.45583 1.000 0.1301 . . H112" H Uiso 0.21116 0.64341 0.47102 1.000 0.1301 . . H114 H Uiso 0.05500 0.49439 0.17298 1.000 0.0513 . . H114' H Uiso 0.02012 0.40266 0.09653 1.000 0.0513 . . H114" H Uiso 0.14439 0.43615 0.12787 1.000 0.0513 . . H116 H Uiso 0.13689 0.16001 0.06449 1.000 0.0554 . . H116' H Uiso 0.19961 0.26476 0.07969 1.000 0.0554 . . H116" H Uiso 0.07631 0.24205 0.04303 1.000 0.0554 . . H119 H Uiso 0.26193 -0.05365 0.15400 1.000 0.0580 . . H120 H Uiso 0.10527 -0.15727 0.11950 1.000 0.0727 . . H121 H Uiso -0.06073 -0.09729 0.11813 1.000 0.0613 . . H123 H Uiso 0.28950 0.19495 0.18036 1.000 0.0402 . . H124 H Uiso 0.41141 0.04258 0.19525 1.000 0.0733 . . H124' H Uiso 0.45999 0.14243 0.18711 1.000 0.0733 . . H124" H Uiso 0.38522 0.06428 0.11577 1.000 0.0733 . . H125 H Uiso 0.25774 0.22093 0.30896 1.000 0.0679 . . H125' H Uiso 0.38427 0.22952 0.30589 1.000 0.0679 . . H125" H Uiso 0.32410 0.13336 0.31324 1.000 0.0679 . . H126 H Uiso -0.10106 0.15313 0.19297 1.000 0.0578 . . H127 H Uiso -0.21495 -0.03716 0.14082 1.000 0.1140 . . H127' H Uiso -0.26184 0.06105 0.18556 1.000 0.1140 . . H127" H Uiso -0.17111 0.02004 0.22974 1.000 0.1140 . . H128 H Uiso -0.15915 0.02664 0.03777 1.000 0.1217 . . H128' H Uiso -0.09720 0.13341 0.06200 1.000 0.1217 . . H128" H Uiso -0.21857 0.11899 0.07823 1.000 0.1217 . . H171 H Uiso -0.14580 0.33416 0.20070 1.000 0.1157 . . H191 H Uiso -0.32445 0.45386 0.19272 0.666(11) 0.0780 . . H191' H Uiso -0.30972 0.35534 0.12652 0.666(11) 0.0780 . . H191" H Uiso -0.22942 0.45095 0.14069 0.666(11) 0.0780 . . H192 H Uiso -0.14422 0.36967 0.14065 0.334(11) 0.1544 . . H192' H Uiso -0.27102 0.35103 0.13956 0.334(11) 0.1544 . . H192" H Uiso -0.19536 0.27360 0.15360 0.334(11) 0.1544 . . H1291 H Uiso 0.04661 0.41031 0.45584 1.000 0.0742 . . H1291' H Uiso -0.06908 0.34033 0.43307 1.000 0.0742 . . H1301 H Uiso 0.10902 0.28575 0.46742 0.49(2) 0.0787 . . H1302 H Uiso -0.07298 0.22604 0.42217 0.51(2) 0.0492 . . H1311 H Uiso -0.00936 0.13981 0.37156 1.000 0.0807 . . H1311' H Uiso 0.12304 0.15454 0.37749 1.000 0.0807 . . F21 F Uani 0.77714(15) 0.62352(16) 0.03813(11) 1.000 0.0514(7) . . F22 F Uani 0.93532(16) 0.69655(16) 0.07092(12) 1.000 0.0531(7) . . F23 F Uani 0.8965(2) 0.57013(16) 0.10104(13) 1.000 0.0715(9) . . F24 F Uani 1.06050(18) 0.8550(2) 0.35327(16) 1.000 0.0798(10) . . F25 F Uani 0.9656(3) 0.97617(18) 0.37214(18) 1.000 0.0952(11) . . F26 F Uani 0.94468(18) 0.87513(16) 0.43177(12) 1.000 0.0613(8) . . F27 F Uani 0.6159(3) 1.1780(3) 0.3207(3) 1.000 0.1456(19) . . F28 F Uani 0.73891(18) 1.14374(17) 0.38926(19) 1.000 0.0791(12) . . F29 F Uani 0.6223(3) 1.22486(18) 0.4397(3) 1.000 0.1266(16) . . F210 F Uani 0.32241(16) 1.05808(14) 0.50761(11) 1.000 0.0510(6) . . F211 F Uani 0.27813(15) 0.90559(14) 0.45104(11) 1.000 0.0449(6) . . F212 F Uani 0.23486(15) 1.00608(16) 0.39373(12) 1.000 0.0515(7) . . F213 F Uani 0.6714(2) 0.57392(19) 0.48749(14) 1.000 0.0759(10) . . F214 F Uani 0.6484(2) 0.72295(15) 0.52203(11) 1.000 0.0604(8) . . F215 F Uani 0.5228(2) 0.6185(2) 0.52364(13) 1.000 0.0709(9) . . F216 F Uani 0.47555(19) 0.35255(16) 0.21581(18) 1.000 0.0856(9) . . F217 F Uani 0.3303(2) 0.39731(17) 0.2493(2) 1.000 0.1008(12) . . F218 F Uani 0.3808(4) 0.4219(2) 0.1563(2) 1.000 0.1589(19) . . F219 F Uani 0.15153(13) 0.68634(14) 0.14104(10) 1.000 0.0391(6) . . F220 F Uani 0.14522(13) 0.67543(15) 0.02116(10) 1.000 0.0450(6) . . F221 F Uani 0.21302(15) 0.56738(14) 0.06232(14) 1.000 0.0569(7) . . F222 F Uani 0.43247(17) 0.84934(18) -0.05248(12) 1.000 0.0618(8) . . F223 F Uani 0.5773(2) 0.78992(17) -0.03247(13) 1.000 0.0627(8) . . F224 F Uani 0.55717(16) 0.93253(14) 0.03664(11) 1.000 0.0495(6) . . C21 C Uani 0.6883(2) 0.77720(19) 0.25017(15) 1.000 0.0256(7) . . C22 C Uani 0.7205(2) 0.71806(19) 0.18142(16) 1.000 0.0264(8) . . C23 C Uani 0.8285(2) 0.7131(2) 0.17094(17) 1.000 0.0305(8) . . C24 C Uani 0.9079(2) 0.7660(2) 0.22898(18) 1.000 0.0360(9) . . C25 C Uani 0.8787(2) 0.8230(2) 0.29795(18) 1.000 0.0355(9) . . C26 C Uani 0.7713(2) 0.8288(2) 0.30882(16) 1.000 0.0301(8) . . C27 C Uani 0.8579(2) 0.6509(2) 0.09595(19) 1.000 0.0374(10) . . C28 C Uani 0.9623(3) 0.8833(3) 0.3635(2) 1.000 0.0516(11) . . C29 C Uani 0.5357(2) 0.88320(19) 0.32109(14) 1.000 0.0243(7) . . C210 C Uani 0.5940(2) 0.9709(2) 0.32783(16) 1.000 0.0302(8) . . C211 C Uani 0.5682(2) 1.0595(2) 0.37439(17) 1.000 0.0340(9) . . C212 C Uani 0.4798(2) 1.0654(2) 0.41253(16) 1.000 0.0335(8) . . C213 C Uani 0.4166(2) 0.9800(2) 0.40450(15) 1.000 0.0283(8) . . C214 C Uani 0.4449(2) 0.89075(19) 0.36063(14) 1.000 0.0252(7) . . C215 C Uani 0.6370(3) 1.1511(2) 0.3802(2) 1.000 0.0487(11) . . C216 C Uani 0.3137(2) 0.9859(2) 0.43906(16) 1.000 0.0347(9) . . C217 C Uani 0.5347(2) 0.68876(18) 0.29455(14) 1.000 0.0237(7) . . C218 C Uani 0.5680(2) 0.69914(19) 0.37254(15) 1.000 0.0258(7) . . C219 C Uani 0.5568(2) 0.6222(2) 0.40102(16) 1.000 0.0288(8) . . C220 C Uani 0.5087(2) 0.5319(2) 0.35417(18) 1.000 0.0347(9) . . C221 C Uani 0.4748(2) 0.5200(2) 0.27739(17) 1.000 0.0332(8) . . C222 C Uani 0.4896(2) 0.59552(19) 0.24824(15) 1.000 0.0281(8) . . C223 C Uani 0.5994(3) 0.6346(2) 0.48294(17) 1.000 0.0380(10) . . C224 C Uani 0.4192(3) 0.4225(2) 0.2262(2) 1.000 0.0482(11) . . C225 C Uani 0.4862(2) 0.76816(18) 0.18107(14) 1.000 0.0235(7) . . C226 C Uani 0.3797(2) 0.72538(19) 0.16445(14) 1.000 0.0259(7) . . C227 C Uani 0.3153(2) 0.71955(19) 0.09685(15) 1.000 0.0262(7) . . C228 C Uani 0.3534(2) 0.7588(2) 0.04330(15) 1.000 0.0275(8) . . C229 C Uani 0.4580(2) 0.80400(18) 0.05979(15) 1.000 0.0256(7) . . C230 C Uani 0.5221(2) 0.80847(18) 0.12701(14) 1.000 0.0241(7) . . C231 C Uani 0.2067(2) 0.6626(2) 0.07990(17) 1.000 0.0333(8) . . C232 C Uani 0.5048(2) 0.8441(2) 0.00327(16) 1.000 0.0322(9) . . B2 B Uani 0.5604(2) 0.7790(2) 0.26228(16) 1.000 0.0242(8) . . H22 H Uiso 0.66719 0.68018 0.14064 1.000 0.0317 . . H24 H Uiso 0.98130 0.76331 0.22170 1.000 0.0432 . . H26 H Uiso 0.75381 0.86857 0.35707 1.000 0.0361 . . H210 H Uiso 0.65334 0.96998 0.29961 1.000 0.0362 . . H212 H Uiso 0.46210 1.12625 0.44372 1.000 0.0401 . . H214 H Uiso 0.40164 0.83326 0.35726 1.000 0.0302 . . H218 H Uiso 0.59921 0.76080 0.40675 1.000 0.0309 . . H220 H Uiso 0.49912 0.47977 0.37399 1.000 0.0417 . . H222 H Uiso 0.46831 0.58372 0.19473 1.000 0.0338 . . H226 H Uiso 0.35065 0.69953 0.20044 1.000 0.0310 . . H228 H Uiso 0.30942 0.75489 -0.00286 1.000 0.0329 . . H230 H Uiso 0.59308 0.84007 0.13671 1.000 0.0289 . . 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 Pd11 0.0381(1) 0.0239(1) 0.0307(1) 0.0123(1) 0.0122(1) 0.0016(1) N11 0.0324(12) 0.0214(11) 0.0348(12) 0.0117(9) 0.0087(9) 0.0033(10) N12 0.0339(12) 0.0196(11) 0.0316(11) 0.0080(9) 0.0076(9) 0.0021(9) C1302 0.047(6) 0.054(5) 0.027(3) 0.021(3) 0.011(3) -0.011(4) C11 0.0310(14) 0.0246(14) 0.0358(14) 0.0131(11) 0.0117(11) 0.0053(11) C12 0.0327(16) 0.0284(16) 0.070(2) 0.0065(15) 0.0192(15) -0.0011(13) C13 0.0301(15) 0.0345(17) 0.0588(19) 0.0127(14) 0.0173(14) 0.0086(13) C14 0.0431(17) 0.0317(16) 0.0389(15) 0.0146(12) 0.0142(13) 0.0132(13) C15 0.0416(17) 0.0254(15) 0.0396(15) 0.0085(12) 0.0046(13) 0.0066(13) C16 0.0345(15) 0.0246(14) 0.0382(14) 0.0111(12) 0.0047(12) 0.0050(12) C17 0.033(2) 0.043(2) 0.169(6) -0.031(3) 0.032(3) -0.0082(18) C18 0.107(4) 0.089(4) 0.166(6) 0.084(5) -0.037(4) -0.057(4) C110 0.0321(16) 0.0295(16) 0.0552(19) 0.0033(14) 0.0018(14) 0.0047(13) C111 0.0348(18) 0.077(3) 0.071(2) 0.041(2) 0.0148(17) 0.0055(18) C112 0.040(2) 0.146(5) 0.107(4) 0.092(4) -0.006(2) 0.002(3) C113 0.0217(13) 0.0369(16) 0.0289(13) 0.0109(11) 0.0049(10) -0.0015(11) C114 0.0439(17) 0.0266(15) 0.0386(15) 0.0176(12) 0.0099(12) 0.0070(13) C115 0.0285(14) 0.0299(15) 0.0318(13) 0.0158(11) 0.0019(11) -0.0039(11) C116 0.0541(19) 0.0280(15) 0.0308(14) 0.0107(12) 0.0113(13) 0.0055(14) C117 0.0463(17) 0.0187(13) 0.0301(13) 0.0087(11) 0.0081(12) -0.0011(12) C118 0.0518(18) 0.0205(13) 0.0321(14) 0.0099(11) 0.0141(12) 0.0064(13) C119 0.065(2) 0.0246(16) 0.062(2) 0.0177(15) 0.0199(18) 0.0133(16) C120 0.084(3) 0.0209(16) 0.076(3) 0.0114(16) 0.024(2) 0.0046(18) C121 0.062(2) 0.0286(17) 0.060(2) 0.0114(15) 0.0119(18) -0.0053(16) C122 0.0510(19) 0.0263(15) 0.0418(16) 0.0127(13) 0.0082(14) -0.0026(14) C123 0.0418(16) 0.0287(15) 0.0346(14) 0.0142(12) 0.0089(12) 0.0097(13) C124 0.052(2) 0.045(2) 0.058(2) 0.0213(16) 0.0236(17) 0.0116(16) C125 0.0462(19) 0.054(2) 0.0359(16) 0.0156(15) 0.0045(14) 0.0067(16) C126 0.0453(19) 0.0341(18) 0.063(2) 0.0149(16) 0.0045(16) -0.0043(15) C127 0.057(3) 0.075(3) 0.110(4) 0.045(3) 0.029(3) 0.001(2) C128 0.058(3) 0.102(4) 0.094(4) 0.051(3) 0.000(2) 0.006(3) C129 0.099(3) 0.055(2) 0.0440(19) 0.0206(18) 0.040(2) 0.022(2) C131 0.110(4) 0.054(2) 0.064(2) 0.042(2) 0.044(2) 0.027(2) C191 0.043(3) 0.047(4) 0.050(3) -0.004(2) 0.014(2) -0.015(3) C192 0.130(16) 0.106(16) 0.075(11) 0.061(11) -0.046(10) -0.036(13) C1301 0.097(14) 0.070(7) 0.036(4) 0.028(4) 0.011(5) -0.004(7) F21 0.0381(10) 0.0617(14) 0.0451(10) 0.0027(9) 0.0096(8) 0.0096(9) F22 0.0426(11) 0.0680(14) 0.0526(11) 0.0224(10) 0.0197(9) 0.0018(10) F23 0.116(2) 0.0518(13) 0.0626(13) 0.0276(11) 0.0252(13) 0.0509(14) F24 0.0362(12) 0.095(2) 0.0918(19) 0.0199(15) -0.0145(12) -0.0164(12) F25 0.109(2) 0.0438(14) 0.117(2) 0.0379(15) -0.0616(18) -0.0422(14) F26 0.0651(14) 0.0509(13) 0.0521(12) 0.0089(10) -0.0253(10) -0.0124(11) F27 0.148(3) 0.117(3) 0.189(4) 0.124(3) -0.072(3) -0.088(2) F28 0.0453(13) 0.0402(13) 0.150(3) 0.0309(15) 0.0164(14) -0.0106(10) F29 0.111(2) 0.0248(13) 0.209(4) -0.0199(17) 0.078(3) -0.0247(14) F210 0.0496(11) 0.0456(12) 0.0412(10) -0.0094(8) 0.0106(8) 0.0015(9) F211 0.0448(11) 0.0384(10) 0.0517(11) 0.0119(9) 0.0185(9) 0.0019(8) F212 0.0319(10) 0.0659(14) 0.0578(12) 0.0236(10) -0.0029(8) 0.0089(9) F213 0.1042(19) 0.0733(17) 0.0576(13) 0.0254(12) -0.0011(13) 0.0536(15) F214 0.0985(17) 0.0448(12) 0.0356(10) 0.0191(9) -0.0131(10) -0.0052(12) F215 0.0734(16) 0.103(2) 0.0509(12) 0.0438(13) 0.0196(11) 0.0020(14) F216 0.0529(14) 0.0316(12) 0.135(2) -0.0245(13) 0.0175(14) -0.0017(10) F217 0.0595(15) 0.0379(13) 0.164(3) -0.0270(16) 0.0439(17) -0.0195(11) F218 0.284(5) 0.0570(19) 0.099(2) 0.0313(17) -0.085(3) -0.093(3) F219 0.0275(9) 0.0524(11) 0.0395(9) 0.0188(8) 0.0059(7) -0.0020(8) F220 0.0278(9) 0.0696(14) 0.0319(9) 0.0134(9) -0.0036(7) -0.0066(9) F221 0.0393(11) 0.0306(10) 0.0878(15) 0.0048(10) 0.0069(10) -0.0089(8) F222 0.0504(12) 0.0928(18) 0.0557(12) 0.0540(12) -0.0114(10) -0.0166(12) F223 0.0881(16) 0.0607(14) 0.0646(13) 0.0393(11) 0.0485(12) 0.0317(12) F224 0.0614(12) 0.0394(11) 0.0486(10) 0.0216(9) 0.0036(9) -0.0165(9) C21 0.0284(13) 0.0204(12) 0.0296(12) 0.0123(10) 0.0025(10) -0.0033(10) C22 0.0263(13) 0.0209(13) 0.0333(13) 0.0115(10) 0.0032(10) -0.0005(10) C23 0.0297(14) 0.0270(14) 0.0416(15) 0.0203(12) 0.0070(11) 0.0026(11) C24 0.0245(14) 0.0397(17) 0.0519(17) 0.0271(14) 0.0043(12) -0.0001(12) C25 0.0325(15) 0.0307(16) 0.0429(16) 0.0168(13) -0.0047(12) -0.0086(12) C26 0.0321(14) 0.0254(14) 0.0327(13) 0.0125(11) -0.0007(11) -0.0051(11) C27 0.0307(15) 0.0416(18) 0.0485(17) 0.0238(14) 0.0095(13) 0.0122(13) C28 0.0374(19) 0.044(2) 0.066(2) 0.0172(18) -0.0111(16) -0.0141(16) C29 0.0280(13) 0.0213(13) 0.0224(11) 0.0082(9) -0.0018(10) -0.0030(10) C210 0.0305(14) 0.0243(14) 0.0355(14) 0.0108(11) 0.0029(11) -0.0012(11) C211 0.0365(16) 0.0202(14) 0.0422(15) 0.0102(12) -0.0029(12) -0.0047(12) C212 0.0373(16) 0.0203(14) 0.0361(14) 0.0024(11) -0.0043(12) 0.0038(12) C213 0.0270(14) 0.0276(14) 0.0257(12) 0.0053(10) -0.0057(10) 0.0010(11) C214 0.0296(13) 0.0203(13) 0.0229(11) 0.0061(10) -0.0022(10) -0.0030(10) C215 0.050(2) 0.0227(16) 0.071(2) 0.0147(16) 0.0059(17) -0.0055(14) C216 0.0367(16) 0.0301(15) 0.0314(14) 0.0027(12) 0.0014(12) 0.0037(13) C217 0.0247(13) 0.0185(12) 0.0268(12) 0.0058(10) 0.0055(10) 0.0001(10) C218 0.0290(14) 0.0191(12) 0.0296(12) 0.0082(10) 0.0059(10) 0.0013(10) C219 0.0311(14) 0.0255(14) 0.0342(13) 0.0138(11) 0.0092(11) 0.0057(11) C220 0.0398(16) 0.0227(14) 0.0486(16) 0.0179(12) 0.0169(13) 0.0047(12) C221 0.0338(15) 0.0182(13) 0.0442(16) 0.0057(12) 0.0100(12) -0.0040(11) C222 0.0299(14) 0.0225(13) 0.0293(13) 0.0046(10) 0.0070(10) -0.0005(11) C223 0.0521(19) 0.0313(16) 0.0380(15) 0.0193(13) 0.0095(13) 0.0113(14) C224 0.065(2) 0.0225(16) 0.0511(19) 0.0072(14) 0.0073(17) -0.0111(16) C225 0.0257(13) 0.0176(12) 0.0245(11) 0.0042(9) 0.0026(9) -0.0013(10) C226 0.0270(13) 0.0237(13) 0.0250(12) 0.0052(10) 0.0057(10) 0.0008(10) C227 0.0246(13) 0.0237(13) 0.0270(12) 0.0044(10) 0.0034(10) 0.0004(11) C228 0.0270(13) 0.0267(14) 0.0259(12) 0.0053(10) 0.0012(10) 0.0036(11) C229 0.0280(13) 0.0196(13) 0.0295(12) 0.0081(10) 0.0043(10) 0.0035(10) C230 0.0238(12) 0.0200(12) 0.0266(12) 0.0061(10) 0.0028(10) -0.0019(10) C231 0.0273(14) 0.0331(16) 0.0361(14) 0.0070(12) 0.0051(11) 0.0002(12) C232 0.0363(16) 0.0294(15) 0.0333(14) 0.0147(12) 0.0021(11) 0.0023(12) B2 0.0267(14) 0.0193(14) 0.0243(13) 0.0055(11) 0.0029(11) -0.0029(11) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd11 N11 2.093(2) . . yes Pd11 N12 2.097(2) . . yes Pd11 C1302 2.123(10) . . yes Pd11 C129 2.105(4) . . yes Pd11 C131 2.116(4) . . yes Pd11 C1301 2.071(11) . . yes F21 C27 1.336(4) . . yes F22 C27 1.342(4) . . yes F23 C27 1.338(4) . . yes F24 C28 1.347(5) . . yes F25 C28 1.315(5) . . yes F26 C28 1.336(4) . . yes F27 C215 1.287(6) . . yes F28 C215 1.297(4) . . yes F29 C215 1.309(6) . . yes F210 C216 1.350(3) . . yes F211 C216 1.319(4) . . yes F212 C216 1.345(3) . . yes F213 C223 1.332(4) . . yes F214 C223 1.332(4) . . yes F215 C223 1.330(4) . . yes F216 C224 1.265(4) . . yes F217 C224 1.307(5) . . yes F218 C224 1.325(5) . . yes F219 C231 1.345(3) . . yes F220 C231 1.338(3) . . yes F221 C231 1.337(4) . . yes F222 C232 1.329(3) . . yes F223 C232 1.338(4) . . yes F224 C232 1.333(4) . . yes N11 C113 1.282(3) . . yes N11 C11 1.446(4) . . yes N12 C115 1.282(4) . . yes N12 C117 1.456(4) . . yes C1301 C131 1.298(13) . . no C1301 C129 1.271(18) . . no C1302 C131 1.332(14) . . no C1302 C129 1.328(11) . . no C11 C16 1.393(4) . . no C11 C12 1.395(5) . . no C12 C13 1.397(5) . . no C12 C17 1.510(7) . . no C13 C14 1.376(5) . . no C14 C15 1.381(5) . . no C15 C16 1.405(4) . . no C16 C110 1.523(5) . . no C17 C192 1.157(19) . . no C17 C18 1.472(8) . . no C17 C191 1.664(8) . . no C1301 H1301 0.9498 . . no C1302 H1302 0.9501 . . no C110 C112 1.538(6) . . no C110 C111 1.504(5) . . no C113 C115 1.485(4) . . no C13 H13 0.9502 . . no C113 C114 1.513(4) . . no C14 H14 0.9494 . . no C15 H15 0.9499 . . no C115 C116 1.502(4) . . no C117 C118 1.394(5) . . no C17 H171 1.0006 . . no C117 C122 1.404(5) . . no C18 H18 0.9800 . . no C18 H18" 0.9803 . . no C118 C119 1.395(4) . . no C18 H18' 0.9799 . . no C118 C123 1.520(4) . . no C119 C120 1.371(6) . . no C120 C121 1.388(6) . . no C121 C122 1.402(5) . . no C122 C126 1.515(5) . . no C123 C124 1.542(5) . . no C123 C125 1.540(4) . . no C126 C127 1.536(7) . . no C126 C128 1.518(6) . . no C110 H110 0.9994 . . no C111 H111" 0.9798 . . no C111 H111' 0.9800 . . no C111 H111 0.9796 . . no C112 H112 0.9802 . . no C112 H112" 0.9803 . . no C112 H112' 0.9791 . . no C114 H114" 0.9804 . . no C114 H114 0.9797 . . no C114 H114' 0.9797 . . no C116 H116' 0.9802 . . no C116 H116" 0.9798 . . no C116 H116 0.9803 . . no C119 H119 0.9500 . . no C120 H120 0.9498 . . no C121 H121 0.9507 . . no C21 C26 1.405(4) . . no C21 C22 1.402(4) . . no C21 B2 1.652(4) . . yes C22 C23 1.399(4) . . no C123 H123 0.9998 . . no C23 C27 1.489(4) . . no C23 C24 1.375(4) . . no C124 H124' 0.9794 . . no C124 H124" 0.9805 . . no C24 C25 1.379(4) . . no C124 H124 0.9802 . . no C125 H125' 0.9793 . . no C125 H125" 0.9804 . . no C125 H125 0.9802 . . no C25 C26 1.394(4) . . no C25 C28 1.510(5) . . no C126 H126 1.0002 . . no C127 H127 0.9799 . . no C127 H127" 0.9797 . . no C127 H127' 0.9798 . . no C128 H128 0.9797 . . no C128 H128' 0.9803 . . no C128 H128" 0.9797 . . no C129 H1291' 0.9903 . . no C129 H1291 0.9900 . . no C29 C210 1.395(4) . . no C29 C214 1.409(4) . . no C29 B2 1.636(4) . . yes C131 H1311' 0.9904 . . no C131 H1311 0.9899 . . no C191 H191' 0.9807 . . no C191 H191 0.9791 . . no C191 H191" 0.9802 . . no C192 H192" 0.9805 . . no C192 H192 0.9791 . . no C192 H192' 0.9799 . . no C192 H171 0.9743 . . no C22 H22 0.9504 . . no C24 H24 0.9506 . . no C26 H26 0.9499 . . no C210 C211 1.389(4) . . no C211 C212 1.368(4) . . no C211 C215 1.511(4) . . no C212 C213 1.391(4) . . no C213 C214 1.392(4) . . no C213 C216 1.497(4) . . no C217 C218 1.410(4) . . no C217 C222 1.401(4) . . no C217 B2 1.636(4) . . yes C218 C219 1.389(4) . . no C219 C223 1.497(4) . . no C219 C220 1.383(4) . . no C220 C221 1.385(4) . . no C221 C222 1.383(4) . . no C221 C224 1.511(4) . . no C225 C226 1.402(4) . . no C225 C230 1.401(4) . . no C225 B2 1.638(4) . . yes C226 C227 1.391(4) . . no C227 C231 1.501(4) . . no C227 C228 1.394(4) . . no C228 C229 1.392(4) . . no C229 C230 1.389(4) . . no C229 C232 1.494(4) . . no C210 H210 0.9503 . . no C212 H212 0.9493 . . no C214 H214 0.9501 . . no C218 H218 0.9501 . . no C220 H220 0.9499 . . no C222 H222 0.9500 . . no C226 H226 0.9497 . . no C228 H228 0.9504 . . no C230 H230 0.9504 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pd11 N12 76.92(9) . . . yes N11 Pd11 C1302 140.2(3) . . . yes N11 Pd11 C129 106.78(14) . . . yes N11 Pd11 C131 175.24(12) . . . yes N11 Pd11 C1301 139.2(4) . . . yes N12 Pd11 C1302 140.2(3) . . . yes N12 Pd11 C129 176.19(14) . . . yes N12 Pd11 C131 107.30(13) . . . yes N12 Pd11 C1301 140.8(5) . . . yes C1302 Pd11 C129 36.6(3) . . . yes C1302 Pd11 C131 36.6(4) . . . yes C129 Pd11 C131 68.97(16) . . . yes C1301 Pd11 C129 35.4(5) . . . yes C1301 Pd11 C131 36.1(4) . . . yes Pd11 N11 C11 120.91(18) . . . yes Pd11 N11 C113 114.9(2) . . . yes C11 N11 C113 124.1(3) . . . yes Pd11 N12 C115 115.7(2) . . . yes Pd11 N12 C117 121.71(18) . . . yes C115 N12 C117 122.6(2) . . . yes C129 C1301 C131 137.0(14) . . . no Pd11 C1301 C129 73.8(6) . . . yes Pd11 C1301 C131 73.9(5) . . . yes Pd11 C1302 C131 71.4(5) . . . yes Pd11 C1302 C129 71.0(5) . . . yes C129 C1302 C131 128.0(11) . . . no N11 C11 C12 116.9(3) . . . yes N11 C11 C16 120.3(2) . . . yes C12 C11 C16 122.5(3) . . . no C13 C12 C17 119.4(3) . . . no C11 C12 C17 122.9(3) . . . no C11 C12 C13 117.7(3) . . . no C12 C13 C14 121.2(3) . . . no C13 C14 C15 120.1(3) . . . no C14 C15 C16 120.9(3) . . . no C11 C16 C15 117.6(3) . . . no C11 C16 C110 122.7(3) . . . no C15 C16 C110 119.8(3) . . . no C12 C17 C191 109.1(4) . . . no C18 C17 C192 113.9(12) . . . no C12 C17 C192 132.8(12) . . . no C18 C17 C191 106.4(4) . . . no C12 C17 C18 113.3(5) . . . no C129 C1301 H1301 111.49 . . . no C131 C1301 H1301 111.54 . . . no Pd11 C1301 H1301 139.60 . . . no C131 C1302 H1302 116.02 . . . no Pd11 C1302 H1302 137.29 . . . no C129 C1302 H1302 115.97 . . . no C111 C110 C112 109.4(4) . . . no C16 C110 C111 111.9(3) . . . no C16 C110 C112 110.5(3) . . . no C12 C13 H13 119.40 . . . no C14 C13 H13 119.38 . . . no C114 C113 C115 119.3(2) . . . no N11 C113 C114 123.8(3) . . . yes N11 C113 C115 116.7(3) . . . yes C13 C14 H14 119.95 . . . no C15 C14 H14 119.96 . . . no N12 C115 C113 115.2(2) . . . yes N12 C115 C116 125.1(3) . . . yes C113 C115 C116 119.6(3) . . . no C16 C15 H15 119.50 . . . no C14 C15 H15 119.59 . . . no C191 C17 H171 109.28 . . . no C192 C17 H171 53.10 . . . no C18 C17 H171 109.30 . . . no C118 C117 C122 123.4(3) . . . no C12 C17 H171 109.30 . . . no N12 C117 C122 115.6(3) . . . yes N12 C117 C118 120.8(3) . . . yes C17 C18 H18 109.47 . . . no C17 C18 H18' 109.49 . . . no C119 C118 C123 121.2(3) . . . no H18 C18 H18' 109.48 . . . no H18 C18 H18" 109.44 . . . no C17 C18 H18" 109.49 . . . no C117 C118 C123 122.1(3) . . . no C117 C118 C119 116.7(3) . . . no H18' C18 H18" 109.45 . . . no C118 C119 C120 121.7(4) . . . no C119 C120 C121 120.7(4) . . . no C120 C121 C122 120.3(4) . . . no C117 C122 C121 117.1(3) . . . no C121 C122 C126 120.4(3) . . . no C117 C122 C126 122.4(3) . . . no C124 C123 C125 109.3(3) . . . no C118 C123 C124 114.3(3) . . . no C118 C123 C125 110.4(2) . . . no C122 C126 C127 113.4(4) . . . no C122 C126 C128 111.7(3) . . . no C127 C126 C128 109.1(4) . . . no Pd11 C129 C1302 72.4(5) . . . yes Pd11 C129 C1301 70.8(5) . . . yes Pd11 C131 C1301 70.1(6) . . . yes Pd11 C131 C1302 72.0(5) . . . yes C111 C110 H110 108.34 . . . no C16 C110 H110 108.27 . . . no C112 C110 H110 108.31 . . . no C110 C111 H111' 109.41 . . . no C110 C111 H111" 109.48 . . . no H111" C111 H111 109.52 . . . no H111' C111 H111 109.49 . . . no C110 C111 H111 109.45 . . . no H111' C111 H111" 109.49 . . . no C110 C112 H112' 109.50 . . . no C110 C112 H112" 109.45 . . . no C110 C112 H112 109.40 . . . no H112' C112 H112" 109.52 . . . no H112' C112 H112 109.53 . . . no H112" C112 H112 109.43 . . . no C113 C114 H114" 109.44 . . . no H114' C114 H114 109.50 . . . no C113 C114 H114 109.48 . . . no H114' C114 H114" 109.46 . . . no C113 C114 H114' 109.49 . . . no H114" C114 H114 109.46 . . . no H116' C116 H116" 109.48 . . . no H116' C116 H116 109.44 . . . no H116" C116 H116 109.48 . . . no C115 C116 H116 109.47 . . . no C115 C116 H116' 109.47 . . . no C115 C116 H116" 109.49 . . . no C118 C119 H119 119.11 . . . no C120 C119 H119 119.18 . . . no C119 C120 H120 119.67 . . . no C121 C120 H120 119.62 . . . no C22 C21 C26 115.8(2) . . . no C26 C21 B2 122.8(2) . . . yes C122 C121 H121 119.86 . . . no C22 C21 B2 121.2(2) . . . yes C120 C121 H121 119.87 . . . no C21 C22 C23 122.1(3) . . . no C24 C23 C27 119.6(2) . . . no C124 C123 H123 107.58 . . . no C22 C23 C24 120.6(3) . . . no C118 C123 H123 107.51 . . . no C125 C123 H123 107.55 . . . no C22 C23 C27 119.8(2) . . . no C23 C24 C25 118.6(2) . . . no H124" C124 H124 109.42 . . . no C123 C124 H124 109.48 . . . no H124' C124 H124" 109.47 . . . no H124' C124 H124 109.50 . . . no C123 C124 H124' 109.49 . . . no C123 C124 H124" 109.46 . . . no C123 C125 H125" 109.45 . . . no C123 C125 H125 109.46 . . . no H125' C125 H125" 109.49 . . . no C24 C25 C28 120.9(3) . . . no C123 C125 H125' 109.49 . . . no C24 C25 C26 121.3(3) . . . no H125' C125 H125 109.51 . . . no H125" C125 H125 109.43 . . . no C26 C25 C28 117.8(3) . . . no C127 C126 H126 107.39 . . . no C122 C126 H126 107.46 . . . no C128 C126 H126 107.51 . . . no C21 C26 C25 121.6(3) . . . no F21 C27 F23 107.1(3) . . . yes C126 C127 H127' 109.44 . . . no F21 C27 C23 114.1(2) . . . yes F21 C27 F22 105.3(3) . . . yes H127' C127 H127 109.49 . . . no H127" C127 H127 109.49 . . . no F23 C27 C23 112.5(3) . . . yes F22 C27 F23 105.4(2) . . . yes F22 C27 C23 111.9(3) . . . yes H127' C127 H127" 109.51 . . . no C126 C127 H127" 109.47 . . . no C126 C127 H127 109.42 . . . no C126 C128 H128' 109.41 . . . no F25 C28 F26 106.2(3) . . . yes C126 C128 H128" 109.49 . . . no C126 C128 H128 109.47 . . . no H128' C128 H128" 109.47 . . . no H128' C128 H128 109.47 . . . no H128" C128 H128 109.52 . . . no F24 C28 F25 109.1(4) . . . yes F24 C28 F26 104.7(3) . . . yes F25 C28 C25 111.9(3) . . . yes F26 C28 C25 112.9(3) . . . yes F24 C28 C25 111.7(3) . . . yes C210 C29 C214 115.6(2) . . . no C210 C29 B2 122.7(2) . . . yes Pd11 C129 H1291 116.54 . . . no Pd11 C129 H1291' 116.51 . . . no C214 C29 B2 121.2(2) . . . yes H1291 C129 H1291' 113.51 . . . no C1302 C129 H1291 151.61 . . . no C1302 C129 H1291' 81.62 . . . no C1301 C129 H1291' 116.57 . . . no C1301 C129 H1291 116.55 . . . no C1301 C131 H1311' 116.60 . . . no Pd11 C131 H1311' 116.62 . . . no Pd11 C131 H1311 116.65 . . . no C1302 C131 H1311 81.99 . . . no C1302 C131 H1311' 151.29 . . . no H1311 C131 H1311' 113.61 . . . no C1301 C131 H1311 116.68 . . . no C17 C191 H191' 109.45 . . . no C17 C191 H191" 109.47 . . . no C17 C191 H191 109.50 . . . no H191" C191 H191 109.52 . . . no H191' C191 H191" 109.40 . . . no H191' C191 H191 109.48 . . . no H192" C192 H192 109.51 . . . no H171 C192 H192 88.49 . . . no H192' C192 H192" 109.45 . . . no H192' C192 H192 109.55 . . . no C17 C192 H171 55.21 . . . no C17 C192 H192' 109.43 . . . no C17 C192 H192" 109.39 . . . no C17 C192 H192 109.49 . . . no H192' C192 H171 160.36 . . . no H192" C192 H171 69.76 . . . no C23 C22 H22 118.98 . . . no C21 C22 H22 118.90 . . . no C23 C24 H24 120.71 . . . no C25 C24 H24 120.74 . . . no C21 C26 H26 119.19 . . . no C25 C26 H26 119.21 . . . no C29 C210 C211 122.2(2) . . . no C212 C211 C215 119.7(3) . . . no C210 C211 C215 119.0(3) . . . no C210 C211 C212 121.3(3) . . . no C211 C212 C213 118.3(3) . . . no C214 C213 C216 120.4(3) . . . no C212 C213 C214 120.5(2) . . . no C212 C213 C216 119.0(3) . . . no C29 C214 C213 122.0(3) . . . no F27 C215 C211 112.1(3) . . . yes F27 C215 F28 108.3(3) . . . yes F27 C215 F29 105.4(4) . . . yes F29 C215 C211 112.5(3) . . . yes F28 C215 F29 104.7(3) . . . yes F28 C215 C211 113.3(3) . . . yes F211 C216 F212 106.7(2) . . . yes F211 C216 C213 113.9(2) . . . yes F212 C216 C213 111.6(2) . . . yes F210 C216 C213 111.9(2) . . . yes F210 C216 F211 106.9(2) . . . yes F210 C216 F212 105.3(2) . . . yes C218 C217 C222 115.1(2) . . . no C218 C217 B2 120.0(2) . . . yes C222 C217 B2 124.6(2) . . . yes C217 C218 C219 122.2(3) . . . no C220 C219 C223 118.4(3) . . . no C218 C219 C220 121.1(3) . . . no C218 C219 C223 120.6(3) . . . no C219 C220 C221 117.8(3) . . . no C220 C221 C224 118.3(3) . . . no C222 C221 C224 120.5(3) . . . no C220 C221 C222 121.2(3) . . . no C217 C222 C221 122.6(2) . . . no F213 C223 C219 112.4(3) . . . yes F214 C223 F215 106.2(3) . . . yes F213 C223 F214 105.5(3) . . . yes F213 C223 F215 106.2(3) . . . yes F214 C223 C219 113.6(3) . . . yes F215 C223 C219 112.4(3) . . . yes F217 C224 C221 113.5(3) . . . yes F216 C224 F217 107.6(3) . . . yes F216 C224 F218 106.1(3) . . . yes F216 C224 C221 115.5(3) . . . yes F217 C224 F218 99.4(4) . . . yes F218 C224 C221 113.2(3) . . . yes C226 C225 C230 115.8(2) . . . no C226 C225 B2 122.0(2) . . . yes C230 C225 B2 122.0(2) . . . yes C225 C226 C227 122.1(2) . . . no C228 C227 C231 120.6(2) . . . no C226 C227 C228 121.1(2) . . . no C226 C227 C231 118.1(2) . . . no C227 C228 C229 117.7(2) . . . no C230 C229 C232 118.9(2) . . . no C228 C229 C230 120.8(2) . . . no C228 C229 C232 120.2(2) . . . no C225 C230 C229 122.6(2) . . . no F219 C231 C227 112.4(2) . . . yes F219 C231 F220 106.6(2) . . . yes F219 C231 F221 105.2(2) . . . yes F220 C231 C227 112.8(2) . . . yes F221 C231 C227 112.0(2) . . . yes F220 C231 F221 107.3(2) . . . yes F223 C232 F224 105.0(2) . . . yes F223 C232 C229 111.8(3) . . . yes F222 C232 F223 106.0(2) . . . yes F222 C232 F224 107.1(3) . . . yes F222 C232 C229 113.5(2) . . . yes F224 C232 C229 112.9(2) . . . yes C29 C210 H210 118.88 . . . no C211 C210 H210 118.91 . . . no C211 C212 H212 120.84 . . . no C213 C212 H212 120.84 . . . no C213 C214 H214 119.00 . . . no C29 C214 H214 119.05 . . . no C217 C218 H218 118.90 . . . no C219 C218 H218 118.89 . . . no C219 C220 H220 121.10 . . . no C221 C220 H220 121.10 . . . no C221 C222 H222 118.72 . . . no C217 C222 H222 118.73 . . . no C225 C226 H226 118.95 . . . no C227 C226 H226 119.00 . . . no C227 C228 H228 121.13 . . . no C229 C228 H228 121.15 . . . no C229 C230 H230 118.73 . . . no C225 C230 H230 118.70 . . . no C21 B2 C217 104.0(2) . . . yes C21 B2 C225 110.9(2) . . . yes C29 B2 C225 103.6(2) . . . yes C217 B2 C225 113.3(2) . . . yes C29 B2 C217 113.1(2) . . . yes C21 B2 C29 112.3(2) . . . yes 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 N12 Pd11 N11 C11 169.0(2) . . . . no N12 Pd11 N11 C113 -7.0(2) . . . . no C1302 Pd11 N11 C11 6.7(6) . . . . no C1302 Pd11 N11 C113 -169.3(6) . . . . no C129 Pd11 N11 C11 -12.0(3) . . . . no C129 Pd11 N11 C113 172.1(2) . . . . no N11 Pd11 N12 C115 7.1(2) . . . . no N11 Pd11 N12 C117 -170.5(2) . . . . no C1302 Pd11 N12 C115 169.4(6) . . . . no C1302 Pd11 N12 C117 -8.2(7) . . . . no C131 Pd11 N12 C115 -170.6(2) . . . . no C131 Pd11 N12 C117 11.8(3) . . . . no N11 Pd11 C1302 C129 -30.9(10) . . . . no N11 Pd11 C1302 C131 -174.4(2) . . . . no N12 Pd11 C1302 C129 176.7(3) . . . . no N12 Pd11 C1302 C131 33.3(9) . . . . no C129 Pd11 C1302 C131 -143.4(10) . . . . no C131 Pd11 C1302 C129 143.4(10) . . . . no N11 Pd11 C129 C1302 159.9(7) . . . . no C131 Pd11 C129 C1302 -22.4(7) . . . . no N12 Pd11 C131 C1302 -158.4(6) . . . . no C129 Pd11 C131 C1302 22.4(6) . . . . no Pd11 N11 C11 C16 92.7(3) . . . . no C113 N11 C11 C12 93.9(4) . . . . no Pd11 N11 C11 C12 -81.7(3) . . . . no Pd11 N11 C113 C115 6.1(3) . . . . no C113 N11 C11 C16 -91.8(4) . . . . no Pd11 N11 C113 C114 -179.1(2) . . . . no C11 N11 C113 C114 5.1(4) . . . . no C11 N11 C113 C115 -169.7(2) . . . . no Pd11 N12 C115 C116 177.6(2) . . . . no Pd11 N12 C115 C113 -6.2(3) . . . . no Pd11 N12 C117 C118 -101.0(3) . . . . no C117 N12 C115 C113 171.4(3) . . . . no C117 N12 C115 C116 -4.9(4) . . . . no C115 N12 C117 C122 -103.4(3) . . . . no Pd11 N12 C117 C122 74.0(3) . . . . no C115 N12 C117 C118 81.6(4) . . . . no C129 C1302 C131 Pd11 -45.7(8) . . . . no C131 C1302 C129 Pd11 45.8(8) . . . . no N11 C11 C12 C17 -6.1(5) . . . . no C16 C11 C12 C13 -1.0(5) . . . . no C16 C11 C12 C17 179.7(4) . . . . no N11 C11 C16 C15 -172.9(3) . . . . no N11 C11 C16 C110 6.2(4) . . . . no C12 C11 C16 C15 1.1(4) . . . . no C12 C11 C16 C110 -179.8(3) . . . . no N11 C11 C12 C13 173.2(3) . . . . no C11 C12 C13 C14 0.2(5) . . . . no C17 C12 C13 C14 179.5(4) . . . . no C11 C12 C17 C191 -126.6(4) . . . . no C13 C12 C17 C18 -64.3(5) . . . . no C13 C12 C17 C191 54.1(5) . . . . no C11 C12 C17 C18 115.0(4) . . . . no C12 C13 C14 C15 0.4(5) . . . . no C13 C14 C15 C16 -0.4(5) . . . . no C14 C15 C16 C11 -0.4(4) . . . . no C14 C15 C16 C110 -179.6(3) . . . . no C11 C16 C110 C111 122.2(3) . . . . no C15 C16 C110 C111 -58.7(4) . . . . no C11 C16 C110 C112 -115.6(4) . . . . no C15 C16 C110 C112 63.5(5) . . . . no C16 C110 C111 H111' -178.97 . . . . no C16 C110 C111 H111" 61.04 . . . . no C16 C110 C111 H111 -59.00 . . . . no C112 C110 C111 H111' 58.23 . . . . no C112 C110 C111 H111" -61.76 . . . . no C112 C110 C111 H111 178.20 . . . . no H110 C110 C111 H111' -59.67 . . . . no H110 C110 C111 H111" -179.66 . . . . no H110 C110 C111 H111 60.29 . . . . no C16 C110 C112 H112' 45.22 . . . . no C16 C110 C112 H112" -74.84 . . . . no C16 C110 C112 H112 165.27 . . . . no C111 C110 C112 H112' 168.88 . . . . no C111 C110 C112 H112" 48.81 . . . . no C111 C110 C112 H112 -71.08 . . . . no H110 C110 C112 H112' -73.20 . . . . no H110 C110 C112 H112" 166.73 . . . . no H110 C110 C112 H112 46.84 . . . . no N11 C113 C114 H114' -112.57 . . . . no N11 C113 C114 H114" 127.46 . . . . no N11 C113 C114 H114 7.48 . . . . no C115 C113 C114 H114' 62.11 . . . . no C115 C113 C114 H114" -57.86 . . . . no C115 C113 C114 H114 -177.84 . . . . no N12 C115 C116 H116' -116.58 . . . . no N12 C115 C116 H116" 123.41 . . . . no N12 C115 C116 H116 3.38 . . . . no C113 C115 C116 H116' 67.33 . . . . no C113 C115 C116 H116" -52.69 . . . . no C113 C115 C116 H116 -172.71 . . . . no C117 C118 C119 H119 179.57 . . . . no C123 C118 C119 H119 -2.03 . . . . no C117 C118 C123 H123 -40.11 . . . . no C119 C118 C123 H123 141.58 . . . . no C118 C119 C120 H120 -179.77 . . . . no H119 C119 C120 C121 -179.54 . . . . no H119 C119 C120 H120 0.32 . . . . no C119 C120 C121 H121 178.74 . . . . no H120 C120 C121 C122 178.74 . . . . no H120 C120 C121 H121 -1.12 . . . . no H121 C121 C122 C117 -177.83 . . . . no H121 C121 C122 C126 -0.69 . . . . no C26 C21 B2 C217 -89.8(3) . . . . no C26 C21 B2 C225 148.2(3) . . . . no C22 C21 C26 C25 1.6(4) . . . . no B2 C21 C26 C25 177.5(3) . . . . no C22 C21 B2 C29 -151.6(3) . . . . no C22 C21 B2 C217 85.9(3) . . . . no C22 C21 B2 C225 -36.2(4) . . . . no C26 C21 C22 C23 -2.0(4) . . . . no B2 C21 C22 C23 -177.9(3) . . . . no C26 C21 B2 C29 32.8(4) . . . . no C21 C22 C23 C24 0.8(5) . . . . no C21 C22 C23 C27 -178.5(3) . . . . no C117 C122 C126 H126 -27.25 . . . . no C121 C122 C126 H126 155.77 . . . . no C118 C123 C124 H124 -64.69 . . . . no C125 C123 C124 H124' -60.50 . . . . no C125 C123 C124 H124" 179.49 . . . . no C118 C123 C124 H124' 175.25 . . . . no C118 C123 C124 H124" 55.25 . . . . no H123 C123 C125 H125 57.98 . . . . no C27 C23 C24 C25 -179.9(3) . . . . no C22 C23 C27 F21 15.9(4) . . . . no C22 C23 C27 F22 135.2(3) . . . . no C22 C23 C27 F23 -106.4(3) . . . . no C24 C23 C27 F21 -163.4(3) . . . . no C24 C23 C27 F22 -44.1(4) . . . . no C24 C23 C27 F23 74.3(4) . . . . no C118 C123 C125 H125' -179.09 . . . . no C118 C123 C125 H125" 60.89 . . . . no C118 C123 C125 H125 -59.04 . . . . no C124 C123 C125 H125' 54.42 . . . . no C124 C123 C125 H125" -65.60 . . . . no C124 C123 C125 H125 174.47 . . . . no H123 C123 C125 H125' -62.08 . . . . no H123 C123 C125 H125" 177.90 . . . . no C22 C23 C24 C25 0.8(5) . . . . no H123 C123 C124 H124' 55.97 . . . . no H123 C123 C124 H124" -64.03 . . . . no C125 C123 C124 H124 59.55 . . . . no H123 C123 C124 H124 176.03 . . . . no C23 C24 C25 C28 -179.5(3) . . . . no C23 C24 C25 C26 -1.1(5) . . . . no C24 C25 C26 C21 -0.1(5) . . . . no C26 C25 C28 F26 48.1(5) . . . . no C24 C25 C28 F25 106.8(4) . . . . no C28 C25 C26 C21 178.3(3) . . . . no C24 C25 C28 F24 -15.9(5) . . . . no C26 C25 C28 F25 -71.6(4) . . . . no C24 C25 C28 F26 -133.5(3) . . . . no C26 C25 C28 F24 165.7(3) . . . . no H126 C126 C128 H128 179.26 . . . . no C122 C126 C127 H127' 171.83 . . . . no C122 C126 C127 H127" 51.80 . . . . no C122 C126 C127 H127 -68.19 . . . . no C128 C126 C127 H127' -62.95 . . . . no C128 C126 C127 H127" 177.02 . . . . no C128 C126 C127 H127 57.02 . . . . no H126 C126 C127 H127' 53.28 . . . . no H126 C126 C127 H127" -66.74 . . . . no H126 C126 C127 H127 173.26 . . . . no C122 C126 C128 H128' -58.37 . . . . no C122 C126 C128 H128" -178.34 . . . . no C122 C126 C128 H128 61.59 . . . . no C127 C126 C128 H128' 175.46 . . . . no C127 C126 C128 H128" 55.49 . . . . no C127 C126 C128 H128 -64.58 . . . . no H126 C126 C128 H128' 59.31 . . . . no H126 C126 C128 H128" -60.67 . . . . no C210 C29 B2 C21 31.1(3) . . . . no C210 C29 B2 C217 148.4(2) . . . . no C210 C29 B2 C225 -88.6(3) . . . . no C214 C29 B2 C21 -157.3(2) . . . . no C214 C29 B2 C217 -40.0(3) . . . . no C214 C29 B2 C225 83.0(3) . . . . no C214 C29 C210 C211 3.9(4) . . . . no B2 C29 C210 C211 176.0(2) . . . . no B2 C29 C214 C213 -173.2(2) . . . . no C210 C29 C214 C213 -1.0(4) . . . . no C29 C210 C211 C212 -4.0(4) . . . . no C29 C210 C211 C215 178.5(3) . . . . no C210 C211 C212 C213 0.9(4) . . . . no C210 C211 C215 F29 -163.3(3) . . . . no C215 C211 C212 C213 178.4(3) . . . . no C210 C211 C215 F28 -44.7(4) . . . . no C212 C211 C215 F29 19.2(5) . . . . no C212 C211 C215 F28 137.7(3) . . . . no C210 C211 C215 F27 78.2(4) . . . . no C212 C211 C215 F27 -99.5(4) . . . . no C211 C212 C213 C214 2.0(4) . . . . no C211 C212 C213 C216 -173.8(3) . . . . no C212 C213 C216 F210 -37.5(4) . . . . no C214 C213 C216 F211 25.4(4) . . . . no C214 C213 C216 F210 146.8(3) . . . . no C214 C213 C216 F212 -95.5(3) . . . . no C216 C213 C214 C29 173.8(2) . . . . no C212 C213 C214 C29 -1.9(4) . . . . no C212 C213 C216 F211 -158.9(2) . . . . no C212 C213 C216 F212 80.2(3) . . . . no C222 C217 B2 C225 24.4(3) . . . . no C222 C217 C218 C219 0.1(4) . . . . no B2 C217 C218 C219 -174.1(2) . . . . no C218 C217 B2 C29 -44.6(3) . . . . no C218 C217 C222 C221 2.5(4) . . . . no C218 C217 B2 C21 77.5(3) . . . . no C222 C217 B2 C29 141.8(2) . . . . no C218 C217 B2 C225 -162.0(2) . . . . no C222 C217 B2 C21 -96.1(3) . . . . no B2 C217 C222 C221 176.3(2) . . . . no C217 C218 C219 C223 176.1(3) . . . . no C217 C218 C219 C220 -2.2(4) . . . . no C223 C219 C220 C221 -176.6(3) . . . . no C218 C219 C223 F213 -120.9(3) . . . . no C218 C219 C223 F214 -1.3(4) . . . . no C218 C219 C223 F215 119.3(3) . . . . no C220 C219 C223 F213 57.5(4) . . . . no C220 C219 C223 F214 177.1(3) . . . . no C218 C219 C220 C221 1.8(4) . . . . no C220 C219 C223 F215 -62.3(4) . . . . no C219 C220 C221 C224 -178.2(3) . . . . no C219 C220 C221 C222 0.7(4) . . . . no C222 C221 C224 F217 -117.7(3) . . . . no C220 C221 C224 F216 -63.7(4) . . . . no C220 C221 C224 F217 61.3(4) . . . . no C224 C221 C222 C217 176.0(3) . . . . no C222 C221 C224 F216 117.4(3) . . . . no C220 C221 C222 C217 -3.0(4) . . . . no C220 C221 C224 F218 173.7(3) . . . . no C222 C221 C224 F218 -5.3(5) . . . . no C226 C225 B2 C21 150.9(3) . . . . no B2 C225 C226 C227 177.4(3) . . . . no C226 C225 C230 C229 -2.0(4) . . . . no C230 C225 C226 C227 2.7(4) . . . . no C230 C225 B2 C21 -34.8(3) . . . . no C230 C225 B2 C29 85.9(3) . . . . no B2 C225 C230 C229 -176.7(2) . . . . no C226 C225 B2 C29 -88.4(3) . . . . no C226 C225 B2 C217 34.4(3) . . . . no C230 C225 B2 C217 -151.3(2) . . . . no C225 C226 C227 C231 173.2(3) . . . . no C225 C226 C227 C228 -1.8(4) . . . . no C226 C227 C231 F219 48.7(4) . . . . no C226 C227 C228 C229 0.0(4) . . . . no C231 C227 C228 C229 -174.9(3) . . . . no C226 C227 C231 F221 -69.5(3) . . . . no C228 C227 C231 F219 -136.2(3) . . . . no C228 C227 C231 F220 -15.7(4) . . . . no C228 C227 C231 F221 105.5(3) . . . . no C226 C227 C231 F220 169.3(2) . . . . no C227 C228 C229 C230 0.8(4) . . . . no C227 C228 C229 C232 177.7(3) . . . . no C230 C229 C232 F224 -48.3(3) . . . . no C228 C229 C232 F222 12.7(4) . . . . no C228 C229 C232 F223 -107.2(3) . . . . no C228 C229 C232 F224 134.8(3) . . . . no C230 C229 C232 F222 -170.3(3) . . . . no C230 C229 C232 F223 69.8(3) . . . . no C232 C229 C230 C225 -176.7(3) . . . . no C228 C229 C230 C225 0.3(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd11 C17 3.825(5) . . no Pd11 C18 4.062(6) . . no Pd11 C110 4.140(3) . . no Pd11 C125 3.834(4) . . no Pd11 C126 3.639(4) . . no Pd11 H18' 3.4047 . . no Pd11 H110 3.5848 . . no Pd11 H125 2.8970 . . no Pd11 H126 2.7994 . . no Pd11 H171 3.3018 . . no F21 F221 2.836(3) . 2_665 no F22 C116 3.334(4) . 2_665 no F22 F219 2.936(3) . 1_655 no F22 F220 2.892(3) . 1_655 no F23 C114 3.327(4) . 1_655 no F24 F211 3.034(3) . 1_655 no F24 F212 2.864(3) . 1_655 no F25 C131 3.153(5) . 1_665 no F26 C14 3.310(4) . 1_655 no F27 C18 3.135(8) . 1_665 no F29 F215 2.990(5) . 2_676 no F21 H22 2.4184 . . no F22 H116" 2.5252 . 2_665 no F22 H24 2.6168 . . no F22 H121 2.8577 . 1_665 no F22 H120 2.7762 . 1_665 no F23 H191" 2.5942 . 1_655 no F23 H114 2.7790 . 1_655 no F24 H24 2.4308 . . no F25 H1311 2.3971 . 1_665 no F26 H14 2.6802 . 1_655 no F26 H26 2.6325 . . no F27 H18" 2.7119 . 1_665 no F28 H210 2.6320 . . no F28 H1302 2.5070 . 1_665 no F29 H112" 2.7457 . 2_676 no F29 H212 2.4174 . . no F210 C29 3.287(3) . 2_676 no F210 C210 3.271(3) . 2_676 no F211 F24 3.034(3) . 1_455 no F212 F24 2.864(3) . 1_455 no F213 C112 3.272(7) . 2_666 no F214 C125 3.246(4) . 2_666 no F215 F29 2.990(5) . 2_676 no F217 C115 3.366(4) . . no F217 C113 3.306(4) . . no F219 F22 2.936(3) . 1_455 no F220 F22 2.892(3) . 1_455 no F221 F21 2.836(3) . 2_665 no F221 C114 3.357(4) . . no F222 F224 3.105(3) . 2_675 no F224 F224 3.088(3) . 2_675 no F224 F222 3.105(3) . 2_675 no F210 H218 2.6713 . 2_676 no F210 H212 2.5251 . . no F210 H26 2.6801 . 2_676 no F211 H214 2.4754 . . no F211 H111" 2.8489 . . no F212 H1311' 2.7548 . 1_565 no F213 H220 2.7956 . . no F213 H112 2.7433 . 2_666 no F214 H218 2.3926 . . no F214 H212 2.6373 . 2_676 no F215 H220 2.8229 . . no F215 H220 2.7308 . 2_666 no F216 H18 2.8608 . 1_655 no F217 H220 2.8547 . . no F217 H123 2.8112 . . no F217 H110 2.5193 . . no F218 H222 2.3930 . . no F219 H111 2.8693 . . no F219 H120 2.5438 . 1_565 no F219 H24 2.8281 . 1_455 no F219 H226 2.6077 . . no F220 H114' 2.7437 . 2_565 no F220 H228 2.4481 . . no F220 H120 2.6569 . 1_565 no F220 H192 2.8323 . 2_565 no F221 H114" 2.7072 . . no F222 H228 2.4332 . . no F222 H128" 2.7927 . 2_565 no F224 H230 2.6337 . . no N11 N12 2.606(3) . . no N11 C115 2.358(4) . . no N11 C129 3.370(4) . . no N11 C192 3.23(2) . . no N12 C113 2.338(4) . . no N12 C131 3.393(4) . . no N12 N11 2.606(3) . . no N12 C125 3.317(4) . . no N11 H110 2.4619 . . no N11 H171 2.4026 . . no N11 H192 2.9253 . . no N12 H123 2.6644 . . no N12 H125 2.7441 . . no N12 H126 2.4089 . . no C1301 C14 3.574(11) . 2_566 no C14 F26 3.310(4) . 1_455 no C14 C25 3.411(4) . 1_455 no C14 C1301 3.574(11) . 2_566 no C15 C129 3.521(5) . 2_566 no C16 C114 3.567(4) . . no C17 Pd11 3.825(5) . . no C17 C113 3.446(5) . . no C18 F27 3.135(8) . 1_445 no C18 Pd11 4.062(6) . . no C22 C230 3.141(4) . . no C25 C14 3.411(4) . 1_655 no C26 C218 3.584(4) . . no C26 C210 3.136(4) . . no C29 F210 3.287(3) . 2_676 no C1301 H1311 1.9537 . . no C1301 H1311' 1.9533 . . no C1301 H1291 1.9291 . . no C1301 H1291' 1.9296 . . no C1302 H1311 1.5444 . . no C1302 H1291 2.2483 . . no C1302 H1291' 1.5361 . . no C1302 H1311' 2.2509 . . no C110 C113 3.508(4) . . no C110 Pd11 4.140(3) . . no C11 H192 3.0105 . . no C11 H114 2.5118 . . no C112 F213 3.272(7) . 2_666 no C13 H191 2.8434 . . no C13 H18 2.8460 . . no C113 C110 3.508(4) . . no C113 F217 3.306(4) . . no C113 C192 3.38(2) . . no C113 C17 3.446(5) . . no C114 C16 3.567(4) . . no C114 F23 3.327(4) . 1_455 no C114 F221 3.357(4) . . no C14 H1301 2.8414 . 2_566 no C115 C123 3.384(4) . . no C15 H111" 2.7869 . . no C115 F217 3.366(4) . . no C115 C126 3.538(5) . . no C15 H112" 2.9494 . . no C116 C118 3.418(4) . . no C16 H114 2.9330 . . no C116 C123 3.542(4) . . no C116 F22 3.334(4) . 2_665 no C118 C116 3.418(4) . . no C18 H13 2.9688 . . no C21 H210 2.7594 . . no C21 H230 2.7454 . . no C22 H230 2.7483 . . no C123 C116 3.542(4) . . no C123 C115 3.384(4) . . no C125 F214 3.246(4) . 2_666 no C125 N12 3.317(4) . . no C25 H14 3.0643 . 1_655 no C125 Pd11 3.834(4) . . no C26 H210 2.6730 . . no C126 Pd11 3.639(4) . . no C126 C115 3.538(5) . . no C129 C131 2.390(6) . . no C129 C11 3.545(5) . . no C29 H218 2.8455 . . no C129 N11 3.370(4) . . no C29 H26 2.8070 . . no C129 C15 3.521(5) . 2_566 no C131 N12 3.393(4) . . no C131 F25 3.153(5) . 1_445 no C131 C117 3.593(5) . . no C131 C129 2.390(6) . . no C192 N11 3.23(2) . . no C192 C113 3.38(2) . . no C210 C26 3.136(4) . . no C210 F210 3.271(3) . 2_676 no C111 H15 2.8981 . . no C112 H15 2.9646 . . no C113 H192 2.7843 . . no C113 H171 2.7505 . . no C113 H110 2.8262 . . no C214 C218 3.362(4) . . no C114 H116' 2.9893 . . no C114 H116" 2.7889 . . no C114 H192 2.8038 . . no C115 H123 2.7320 . . no C115 H128' 3.0254 . . no C116 H114' 2.9242 . . no C116 H128' 3.0445 . . no C116 H114" 2.8525 . . no C116 H123 2.7809 . . no C117 H125 2.9869 . . no C117 H116 2.4963 . . no C218 C214 3.362(4) . . no C118 H116 2.8128 . . no C218 C26 3.584(4) . . no C119 H124" 2.9218 . . no C119 H124 2.7847 . . no C121 H127 2.7933 . . no C121 H127" 3.0033 . . no C222 C226 3.122(4) . . no C124 H119 2.5609 . . no C226 C222 3.122(4) . . no C126 H192" 3.0320 . . no C127 H121 2.6682 . . no C128 H192" 2.7228 . . no C129 H1302 1.9416 . . no C129 H1301 1.8447 . . no C129 H1311 2.8457 . . no C230 C22 3.141(4) . . no C131 H125 3.0289 . . no C131 H1301 1.8683 . . no C131 H1302 1.9457 . . no C131 H1291' 2.8420 . . no C191 H13 2.8096 . . no C192 H228 2.9733 . 2_565 no C210 H26 2.7106 . . no C212 H125" 2.9875 . 1_565 no C214 H218 3.0630 . . no C217 H226 2.8023 . . no C217 H214 2.8235 . . no C218 H214 3.0309 . . no C221 H111' 2.9767 . . no C222 H111' 2.9810 . . no C222 H226 2.6666 . . no C225 H222 2.7857 . . no C225 H22 2.7539 . . no C226 H222 2.6112 . . no C228 H191' 3.0069 . 2_565 no C230 H22 2.7678 . . no C231 H120 2.9292 . 1_565 no H111' C222 2.9810 . . no H111' C221 2.9767 . . no H111' H112 2.5650 . . no H111" F211 2.8489 . . no H111" C15 2.7869 . . no H111" H15 2.3492 . . no H111" H112" 2.4199 . . no H112' H1291 2.2899 . . no H112" C15 2.9494 . . no H112" F29 2.7457 . 2_676 no H112" H15 2.5303 . . no H112" H111" 2.4199 . . no H114' C116 2.9242 . . no H114' H116" 2.4306 . . no H114' H192 2.3713 . . no H114' F220 2.7437 . 2_565 no H114" C116 2.8525 . . no H114" F221 2.7072 . . no H114" H116' 2.5552 . . no H116' C114 2.9893 . . no H116' H114" 2.5552 . . no H116' H123 2.5926 . . no H116" H114' 2.4306 . . no H116" F22 2.5252 . 2_665 no H116" C114 2.7889 . . no H124' H125' 2.4737 . . no H124" H119 2.5470 . . no H124" C119 2.9218 . . no H125' H124' 2.4737 . . no H125" H124 2.5554 . . no H125" C212 2.9875 . 1_545 no H13 H191 2.3283 . . no H13 C191 2.8096 . . no H13 H18 2.4558 . . no H13 C18 2.9688 . . no H127' H128" 2.4738 . . no H14 C25 3.0643 . 1_455 no H14 F26 2.6802 . 1_455 no H14 H1301 2.3923 . 2_566 no H127" C121 3.0033 . . no H15 C112 2.9646 . . no H15 C111 2.8981 . . no H15 H111" 2.3492 . . no H15 H112" 2.5303 . . no H128' C115 3.0254 . . no H128' C116 3.0445 . . no H128" F222 2.7927 . 2_565 no H128" H127' 2.4738 . . no H128" H192" 2.2255 . . no H191' H18" 2.5643 . . no H191' C228 3.0069 . 2_565 no H191' H228 2.3313 . 2_565 no H18 H191 2.4098 . . no H18 H13 2.4558 . . no H18 C13 2.8460 . . no H18 F216 2.8608 . 1_455 no H18' Pd11 3.4047 . . no H18" H192" 2.0923 . . no H18" H192' 2.3562 . . no H18" H191' 2.5643 . . no H18" F27 2.7119 . 1_445 no H191" F23 2.5942 . 1_455 no H192' H18" 2.3562 . . no H192' H228 2.4738 . 2_565 no H192" H128" 2.2255 . . no H192" C128 2.7228 . . no H192" H18" 2.0923 . . no H192" H126 2.4507 . . no H192" C126 3.0320 . . no H1291 H112' 2.2899 . . no H22 C230 2.7678 . . no H22 C225 2.7539 . . no H22 F21 2.4184 . . no H1301 H14 2.3923 . 2_566 no H1301 C14 2.8414 . 2_566 no H24 F219 2.8281 . 1_655 no H24 F22 2.6168 . . no H24 F24 2.4308 . . no H1302 F28 2.5070 . 1_445 no H1311 F25 2.3971 . 1_445 no H26 H210 2.4378 . . no H26 C210 2.7106 . . no H26 C29 2.8070 . . no H26 F26 2.6325 . . no H26 F210 2.6801 . 2_676 no H1311' F212 2.7548 . 1_545 no H1311' H125 2.5253 . . no H110 Pd11 3.5848 . . no H110 C113 2.8262 . . no H110 N11 2.4619 . . no H110 F217 2.5193 . . no H111 F219 2.8693 . . no H112 H111' 2.5650 . . no H112 F213 2.7433 . 2_666 no H114 F23 2.7790 . 1_455 no H114 C11 2.5118 . . no H114 C16 2.9330 . . no H116 C117 2.4963 . . no H116 C118 2.8128 . . no H119 C124 2.5609 . . no H119 H124" 2.5470 . . no H119 H124 2.1829 . . no H120 F22 2.7762 . 1_445 no H120 F220 2.6569 . 1_545 no H120 C231 2.9292 . 1_545 no H120 F219 2.5438 . 1_545 no H121 F22 2.8577 . 1_445 no H121 H127 2.2167 . . no H121 C127 2.6682 . . no H123 F217 2.8112 . . no H123 C116 2.7809 . . no H123 N12 2.6644 . . no H123 C115 2.7320 . . no H123 H116' 2.5926 . . no H124 H119 2.1829 . . no H124 C119 2.7847 . . no H124 H125" 2.5554 . . no H125 C131 3.0289 . . no H125 Pd11 2.8970 . . no H125 H1311' 2.5253 . . no H125 C117 2.9869 . . no H125 N12 2.7441 . . no H126 H192" 2.4507 . . no H126 Pd11 2.7994 . . no H126 N12 2.4089 . . no H127 C121 2.7933 . . no H127 H121 2.2167 . . no H127 H128 2.4998 . . no H128 H127 2.4998 . . no H171 Pd11 3.3018 . . no H171 N11 2.4026 . . no H171 C113 2.7505 . . no H191 H18 2.4098 . . no H191 H13 2.3283 . . no H191 C13 2.8434 . . no H192 C11 3.0105 . . no H192 C113 2.7843 . . no H192 H114' 2.3713 . . no H192 F220 2.8323 . 2_565 no H192 C114 2.8038 . . no H192 N11 2.9253 . . no H210 F28 2.6320 . . no H210 C21 2.7594 . . no H210 C26 2.6730 . . no H210 H26 2.4378 . . no H212 F29 2.4174 . . no H212 F210 2.5251 . . no H212 F214 2.6373 . 2_676 no H214 F211 2.4754 . . no H214 C217 2.8235 . . no H214 C218 3.0309 . . no H218 F214 2.3926 . . no H218 C29 2.8455 . . no H218 C214 3.0630 . . no H218 F210 2.6713 . 2_676 no H220 F213 2.7956 . . no H220 F215 2.8229 . . no H220 F217 2.8547 . . no H220 F215 2.7308 . 2_666 no H222 F218 2.3930 . . no H222 C225 2.7857 . . no H222 C226 2.6112 . . no H222 H226 2.3193 . . no H226 F219 2.6077 . . no H226 C217 2.8023 . . no H226 C222 2.6666 . . no H226 H222 2.3193 . . no H228 F220 2.4481 . . no H228 F222 2.4332 . . no H228 H191' 2.3313 . 2_565 no H228 C192 2.9733 . 2_565 no H228 H192' 2.4738 . 2_565 no H230 F224 2.6337 . . no H230 C21 2.7454 . . no H230 C22 2.7483 . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C116 H116" F22 0.9800 2.5300 3.334(4) 140.00 2_665 yes C22 H22 F21 0.9500 2.4200 2.749(3) 100.00 . yes C1302 H1302 F28 0.9500 2.5100 3.381(15) 153.00 1_445 yes C131 H1311 F25 0.9900 2.4000 3.153(5) 133.00 1_445 yes C110 H110 F217 1.0000 2.5200 3.442(5) 153.00 . yes C110 H110 N11 1.0000 2.4600 2.948(4) 109.00 . yes C120 H120 F219 0.9500 2.5400 3.429(5) 155.00 1_545 yes C126 H126 N12 1.0000 2.4100 2.849(5) 106.00 . yes C17 H171 N11 1.0000 2.4000 2.872(5) 108.00 . yes C218 H218 F214 0.9500 2.3900 2.737(3) 101.00 . yes C222 H222 F218 0.9500 2.3900 2.738(5) 101.00 . yes #===END of Crystallographic Information File