#------------------------------------------------------------------------------ #$Date: 2026-05-27 23:11:25 +0100 (Wed, 27 May 2026) $ #$Revision: 306105 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/72/1577296.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1577296 loop_ _publ_author_name 'Bae, Dae Young' 'Ruhs, Nicholas P.' 'Mirica, Liviu M.' _publ_section_title ; Aerobic Base-free C-H Bond Activation at a Pd Center in Aqueous Conditions ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC03081E _journal_year 2026 _chemical_formula_moiety 'C28 H40 N5 Pd, 2(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C32 H46 F12 N7 P2 Pd' _chemical_formula_weight 925.10 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2023-08-09 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-02-06 deposited with the CCDC. 2026-05-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.9980(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.4894(4) _cell_length_b 10.4350(2) _cell_length_c 20.2727(4) _cell_measurement_reflns_used 68727 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 30.535 _cell_measurement_theta_min 2.245 _cell_volume 3882.21(14) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/4 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture/Photon II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0185 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 153495 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.566 _diffrn_reflns_theta_min 2.199 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0922 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.9268. The \l/2 correction factor is Not present. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.583 _exptl_crystal_description plate _exptl_crystal_F_000 1884 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.151 _exptl_crystal_size_min 0.081 _refine_diff_density_max 0.800 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 11891 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+2.9813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.0617 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10821 _reflns_number_total 11891 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc03081e2.cif _cod_data_source_block p21n_a _cod_database_code 1577296 _shelx_shelxl_version_number 2016/4 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.949 _shelx_estimated_absorpt_t_min 0.838 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C15(H15A,H15B), C8(H8A,H8B), C16(H16A,H16B) 2.b Aromatic/amide H refined with riding coordinates: C11(H11), C4(H4), C6(H6), C13(H13), C12(H12) 2.c Idealised Me refined as rotating group: C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C18(H18A,H18B, H18C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C24(H24A, H24B,H24C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C) ; _shelx_res_file ; TITL P21n_a.res in P2(1)/n p21n_a.res created by SHELXL-2016/4 at 11:02:29 on 09-Aug-2023 REM Old TITL P21n in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.079, Rweak 0.003, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C32 N7 F12 P2 Pd CELL 0.71073 18.4894 10.435 20.2727 90 96.998 90 ZERR 4 0.0004 0.0002 0.0004 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N P Pd UNIT 128 184 48 28 8 4 L.S. 10 PLAN 4 SIZE 0.081 0.151 0.28 TEMP -173.15 CONF BOND $H LIST 6 MORE -1 fmap 2 acta OMIT 2 0 0 REM REM REM WGHT 0.024100 2.981300 FVAR 0.18939 PD1 6 0.752307 0.290970 0.507607 11.00000 0.00953 0.01211 = 0.01265 -0.00135 0.00179 -0.00107 P2 5 0.450381 0.193232 0.388408 11.00000 0.01703 0.02229 = 0.01721 -0.00253 0.00129 -0.00050 P1 5 0.614454 0.360521 0.153713 11.00000 0.02745 0.02085 = 0.02151 -0.00329 0.00024 -0.00272 F7 3 0.529545 0.148203 0.421342 11.00000 0.01783 0.03670 = 0.02401 -0.00041 -0.00040 0.00242 F9 3 0.444063 0.068669 0.341976 11.00000 0.04166 0.02426 = 0.02283 -0.00632 -0.00670 0.00388 F12 3 0.456154 0.318711 0.434798 11.00000 0.02883 0.02928 = 0.02963 -0.01131 0.00535 -0.00283 F11 3 0.414405 0.116057 0.444432 11.00000 0.02597 0.03987 = 0.02709 0.00230 0.00621 -0.00931 F8 3 0.486236 0.269985 0.332422 11.00000 0.03799 0.03025 = 0.02704 0.00633 0.01251 0.00283 F10 3 0.370759 0.238632 0.355795 11.00000 0.02275 0.03818 = 0.03379 -0.00416 -0.00579 0.00647 F4 3 0.549128 0.264658 0.161963 11.00000 0.02563 0.03695 = 0.04730 -0.00261 0.00572 -0.00642 F3 3 0.609344 0.324414 0.076245 11.00000 0.07652 0.03072 = 0.02443 -0.00256 0.00629 -0.00277 F2 3 0.670440 0.242786 0.168867 11.00000 0.03190 0.04383 = 0.05205 0.01167 0.00080 0.00897 N1 4 0.791677 0.379219 0.593199 11.00000 0.01271 0.01376 = 0.01306 -0.00056 0.00139 -0.00188 F1 3 0.680924 0.454835 0.144048 11.00000 0.05680 0.04728 = 0.05587 0.00264 0.00302 -0.02938 N5 4 0.713335 0.198689 0.418629 11.00000 0.01501 0.01664 = 0.01836 -0.00222 0.00333 -0.00157 N4 4 0.650795 0.244634 0.544973 11.00000 0.01442 0.01962 = 0.01750 -0.00168 0.00206 -0.00061 F5 3 0.559610 0.475420 0.135513 11.00000 0.06609 0.03161 = 0.08514 0.00330 0.01535 0.02389 F6 3 0.622107 0.393330 0.229884 11.00000 0.10619 0.06281 = 0.02577 -0.02116 0.01066 -0.02722 N2 4 0.730179 0.513838 0.485100 11.00000 0.01086 0.01427 = 0.01427 -0.00114 0.00033 0.00066 N3 4 0.835073 0.132613 0.556139 11.00000 0.01336 0.01283 = 0.01753 0.00112 0.00373 -0.00091 C1 1 0.844022 0.337323 0.474510 11.00000 0.01067 0.01460 = 0.01466 0.00033 0.00317 -0.00079 C5 1 0.968157 0.394591 0.418451 11.00000 0.01261 0.01872 = 0.01946 0.00140 0.00370 -0.00161 C2 1 0.855155 0.463678 0.457114 11.00000 0.01274 0.01370 = 0.01383 0.00012 0.00113 -0.00040 C11 1 0.860038 0.370098 0.699498 11.00000 0.01870 0.02256 = 0.01464 0.00190 0.00013 -0.00278 AFIX 43 H11 2 0.893279 0.326550 0.731264 11.00000 -1.20000 AFIX 0 C3 1 0.804080 0.566271 0.475580 11.00000 0.01189 0.01321 = 0.01683 0.00011 0.00116 -0.00019 AFIX 23 H3A 2 0.798423 0.632146 0.440183 11.00000 -1.20000 H3B 2 0.825578 0.608234 0.517205 11.00000 -1.20000 AFIX 0 C10 1 0.840710 0.318559 0.636669 11.00000 0.01404 0.01422 = 0.01561 0.00220 0.00149 -0.00226 C7 1 0.894761 0.241050 0.470804 11.00000 0.01376 0.01459 = 0.01705 0.00100 0.00326 0.00045 C4 1 0.917926 0.490967 0.427764 11.00000 0.01402 0.01572 = 0.01871 0.00266 0.00203 -0.00224 AFIX 43 H4 2 0.926571 0.576030 0.413972 11.00000 -1.20000 AFIX 0 C15 1 0.710976 0.552686 0.551525 11.00000 0.01540 0.01585 = 0.01621 -0.00211 0.00223 0.00211 AFIX 23 H15A 2 0.660538 0.525197 0.555913 11.00000 -1.20000 H15B 2 0.713102 0.647206 0.555502 11.00000 -1.20000 AFIX 0 C8 1 0.880552 0.112501 0.500472 11.00000 0.01565 0.01405 = 0.02147 0.00165 0.00721 0.00140 AFIX 23 H8A 2 0.854510 0.056134 0.466158 11.00000 -1.20000 H8B 2 0.927249 0.071026 0.517579 11.00000 -1.20000 AFIX 0 C23 1 0.660217 0.698073 0.427018 11.00000 0.01750 0.01674 = 0.02241 0.00071 -0.00195 0.00336 AFIX 137 H23A 2 0.641805 0.724311 0.468292 11.00000 -1.50000 H23B 2 0.624432 0.720292 0.389031 11.00000 -1.50000 H23C 2 0.706211 0.742413 0.423051 11.00000 -1.50000 AFIX 0 C14 1 0.762679 0.493322 0.606536 11.00000 0.01362 0.01551 = 0.01463 -0.00121 0.00316 -0.00162 C6 1 0.957319 0.270886 0.441803 11.00000 0.01363 0.01711 = 0.02138 0.00103 0.00489 0.00144 AFIX 43 H6 2 0.992885 0.206526 0.437888 11.00000 -1.20000 AFIX 0 C25 1 0.595599 0.218435 0.560733 11.00000 0.01582 0.01639 = 0.01434 -0.00041 0.00055 0.00143 N7 4 0.328875 0.717985 0.276227 11.00000 0.04808 0.02795 = 0.03268 0.00171 0.00181 0.00002 C13 1 0.781596 0.550142 0.668147 11.00000 0.01842 0.01907 = 0.01632 -0.00389 0.00431 -0.00223 AFIX 43 H13 2 0.761943 0.630990 0.678113 11.00000 -1.20000 AFIX 0 C19 1 0.747580 -0.044785 0.525380 11.00000 0.02104 0.01624 = 0.02628 -0.00168 0.00680 -0.00530 AFIX 137 H19A 2 0.727582 -0.125120 0.540456 11.00000 -1.50000 H19B 2 0.770959 -0.060863 0.485311 11.00000 -1.50000 H19C 2 0.708139 0.017563 0.515319 11.00000 -1.50000 AFIX 0 C16 1 0.878670 0.203957 0.611220 11.00000 0.01392 0.01568 = 0.01816 0.00178 -0.00083 -0.00010 AFIX 23 H16A 2 0.924552 0.233184 0.595500 11.00000 -1.20000 H16B 2 0.891796 0.144124 0.648665 11.00000 -1.20000 AFIX 0 C17 1 0.803776 0.008307 0.580009 11.00000 0.01669 0.01216 = 0.02220 0.00256 0.00599 -0.00074 C12 1 0.829881 0.486412 0.715003 11.00000 0.02060 0.02348 = 0.01401 -0.00245 0.00237 -0.00409 AFIX 43 H12 2 0.842281 0.522724 0.757861 11.00000 -1.20000 AFIX 0 C21 1 0.673104 0.552270 0.428085 11.00000 0.01297 0.01569 = 0.01701 -0.00013 -0.00290 0.00170 C22 1 0.601533 0.482772 0.434703 11.00000 0.01365 0.02173 = 0.02538 -0.00017 -0.00350 -0.00078 AFIX 137 H22A 2 0.582338 0.511611 0.475168 11.00000 -1.50000 H22B 2 0.610267 0.390170 0.437223 11.00000 -1.50000 H22C 2 0.566126 0.501994 0.395961 11.00000 -1.50000 AFIX 0 C27 1 0.682979 0.149281 0.373500 11.00000 0.01913 0.01731 = 0.02016 -0.00211 0.00475 -0.00194 C18 1 0.765481 0.036319 0.641376 11.00000 0.02114 0.01796 = 0.02113 0.00370 0.00755 0.00043 AFIX 137 H18A 2 0.732137 0.108869 0.632085 11.00000 -1.50000 H18B 2 0.801938 0.057389 0.679043 11.00000 -1.50000 H18C 2 0.737882 -0.039389 0.652238 11.00000 -1.50000 AFIX 0 C9 1 1.033936 0.426467 0.384551 11.00000 0.01595 0.02501 = 0.02906 0.00406 0.00780 -0.00145 AFIX 137 H9A 2 1.018139 0.461141 0.340207 11.00000 -1.50000 H9B 2 1.062773 0.348689 0.380503 11.00000 -1.50000 H9C 2 1.063720 0.490323 0.410872 11.00000 -1.50000 AFIX 0 C20 1 0.864173 -0.092073 0.596698 11.00000 0.02312 0.01508 = 0.03130 0.00598 0.00840 0.00406 AFIX 137 H20A 2 0.844465 -0.165663 0.618668 11.00000 -1.50000 H20B 2 0.904238 -0.054017 0.626403 11.00000 -1.50000 H20C 2 0.882292 -0.120484 0.555653 11.00000 -1.50000 AFIX 0 C26 1 0.524766 0.188109 0.580645 11.00000 0.01489 0.02722 = 0.02364 0.00272 0.00550 -0.00169 AFIX 137 H26A 2 0.507787 0.105974 0.561061 11.00000 -1.50000 H26B 2 0.489960 0.255638 0.565119 11.00000 -1.50000 H26C 2 0.528730 0.182241 0.629198 11.00000 -1.50000 AFIX 0 N6 4 0.547621 0.770759 0.266778 11.00000 0.04553 0.06994 = 0.03076 0.00389 0.01088 0.01278 C24 1 0.699972 0.511565 0.362683 11.00000 0.02226 0.02043 = 0.01601 -0.00052 -0.00123 0.00119 AFIX 137 H24A 2 0.661455 0.526616 0.325829 11.00000 -1.50000 H24B 2 0.712474 0.420268 0.364694 11.00000 -1.50000 H24C 2 0.743179 0.561763 0.355677 11.00000 -1.50000 AFIX 0 C29 1 0.599389 0.763302 0.241762 11.00000 0.03851 0.03639 = 0.01970 0.00288 0.00159 0.00450 C30 1 0.666282 0.754260 0.210924 11.00000 0.03143 0.03982 = 0.02633 0.00093 0.00430 -0.00111 AFIX 137 H30A 2 0.665695 0.818813 0.175752 11.00000 -1.50000 H30B 2 0.669973 0.668637 0.191757 11.00000 -1.50000 H30C 2 0.708224 0.769240 0.244496 11.00000 -1.50000 AFIX 0 C31 1 0.370222 0.637189 0.283692 11.00000 0.04099 0.02463 = 0.02665 0.00162 -0.00658 -0.00591 C28 1 0.643792 0.087685 0.315260 11.00000 0.03330 0.03722 = 0.02227 -0.01144 0.00110 -0.01029 AFIX 137 H28A 2 0.618781 0.152970 0.286118 11.00000 -1.50000 H28B 2 0.607899 0.027664 0.329344 11.00000 -1.50000 H28C 2 0.678345 0.041000 0.291152 11.00000 -1.50000 AFIX 0 C32 1 0.422330 0.532464 0.294488 11.00000 0.05410 0.03343 = 0.05576 0.00102 -0.02097 0.00820 AFIX 137 H32A 2 0.461743 0.545663 0.266966 11.00000 -1.50000 H32B 2 0.397705 0.451167 0.282327 11.00000 -1.50000 H32C 2 0.442624 0.530059 0.341441 11.00000 -1.50000 AFIX 0 HKLF 4 REM P21n_a.res in P2(1)/n REM R1 = 0.0250 for 10821 Fo > 4sig(Fo) and 0.0291 for all 11891 data REM 498 parameters refined using 0 restraints END WGHT 0.0241 2.9813 REM Highest difference peak 0.800, deepest hole -0.588, 1-sigma level 0.063 Q1 1 0.6696 0.2956 0.2004 11.00000 0.05 0.80 Q2 1 0.5780 0.4549 0.2193 11.00000 0.05 0.59 Q3 1 0.6435 0.3228 0.1036 11.00000 0.05 0.54 Q4 1 0.5760 0.3537 0.0900 11.00000 0.05 0.50 ; _shelx_res_checksum 70468 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.75231(2) 0.29097(2) 0.50761(2) 0.01139(3) Uani 1 1 d . . . . . P2 P 0.45038(2) 0.19323(4) 0.38841(2) 0.01891(7) Uani 1 1 d . . . . . P1 P 0.61445(2) 0.36052(4) 0.15371(2) 0.02350(8) Uani 1 1 d . . . . . F7 F 0.52955(5) 0.14820(10) 0.42134(5) 0.02642(19) Uani 1 1 d . . . . . F9 F 0.44406(6) 0.06867(9) 0.34198(5) 0.0305(2) Uani 1 1 d . . . . . F12 F 0.45615(5) 0.31871(10) 0.43480(5) 0.0291(2) Uani 1 1 d . . . . . F11 F 0.41441(5) 0.11606(10) 0.44443(5) 0.0307(2) Uani 1 1 d . . . . . F8 F 0.48624(6) 0.26998(10) 0.33242(5) 0.0311(2) Uani 1 1 d . . . . . F10 F 0.37076(5) 0.23863(11) 0.35580(5) 0.0323(2) Uani 1 1 d . . . . . F4 F 0.54913(6) 0.26466(11) 0.16196(6) 0.0365(2) Uani 1 1 d . . . . . F3 F 0.60934(8) 0.32441(11) 0.07624(5) 0.0439(3) Uani 1 1 d . . . . . F2 F 0.67044(6) 0.24279(12) 0.16887(6) 0.0429(3) Uani 1 1 d . . . . . N1 N 0.79168(6) 0.37922(10) 0.59320(5) 0.01319(19) Uani 1 1 d . . . . . F1 F 0.68092(8) 0.45483(13) 0.14405(7) 0.0536(3) Uani 1 1 d . . . . . N5 N 0.71333(6) 0.19869(11) 0.41863(6) 0.0166(2) Uani 1 1 d . . . . . N4 N 0.65079(6) 0.24463(12) 0.54497(6) 0.0172(2) Uani 1 1 d . . . . . F5 F 0.55961(8) 0.47542(12) 0.13551(8) 0.0604(4) Uani 1 1 d . . . . . F6 F 0.62211(10) 0.39333(15) 0.22988(6) 0.0647(4) Uani 1 1 d . . . . . N2 N 0.73018(6) 0.51384(11) 0.48510(5) 0.01323(19) Uani 1 1 d . . . . . N3 N 0.83507(6) 0.13261(11) 0.55614(6) 0.0144(2) Uani 1 1 d . . . . . C1 C 0.84402(7) 0.33732(12) 0.47451(6) 0.0132(2) Uani 1 1 d . . . . . C5 C 0.96816(7) 0.39459(13) 0.41845(7) 0.0168(2) Uani 1 1 d . . . . . C2 C 0.85515(7) 0.46368(12) 0.45711(6) 0.0135(2) Uani 1 1 d . . . . . C11 C 0.86004(8) 0.37010(14) 0.69950(7) 0.0188(3) Uani 1 1 d . . . . . H11 H 0.893279 0.326550 0.731264 0.023 Uiso 1 1 calc R U . . . C3 C 0.80408(7) 0.56627(12) 0.47558(6) 0.0140(2) Uani 1 1 d . . . . . H3A H 0.798423 0.632146 0.440183 0.017 Uiso 1 1 calc R U . . . H3B H 0.825578 0.608234 0.517205 0.017 Uiso 1 1 calc R U . . . C10 C 0.84071(7) 0.31856(12) 0.63667(6) 0.0146(2) Uani 1 1 d . . . . . C7 C 0.89476(7) 0.24105(13) 0.47080(7) 0.0150(2) Uani 1 1 d . . . . . C4 C 0.91793(7) 0.49097(13) 0.42776(7) 0.0161(2) Uani 1 1 d . . . . . H4 H 0.926571 0.576030 0.413972 0.019 Uiso 1 1 calc R U . . . C15 C 0.71098(7) 0.55269(13) 0.55152(6) 0.0158(2) Uani 1 1 d . . . . . H15A H 0.660538 0.525197 0.555913 0.019 Uiso 1 1 calc R U . . . H15B H 0.713102 0.647206 0.555502 0.019 Uiso 1 1 calc R U . . . C8 C 0.88055(7) 0.11250(13) 0.50047(7) 0.0166(2) Uani 1 1 d . . . . . H8A H 0.854510 0.056134 0.466158 0.020 Uiso 1 1 calc R U . . . H8B H 0.927249 0.071026 0.517579 0.020 Uiso 1 1 calc R U . . . C23 C 0.66022(8) 0.69807(13) 0.42702(7) 0.0192(3) Uani 1 1 d . . . . . H23A H 0.641805 0.724311 0.468292 0.029 Uiso 1 1 calc R U . . . H23B H 0.624432 0.720292 0.389031 0.029 Uiso 1 1 calc R U . . . H23C H 0.706211 0.742413 0.423051 0.029 Uiso 1 1 calc R U . . . C14 C 0.76268(7) 0.49332(12) 0.60654(6) 0.0145(2) Uani 1 1 d . . . . . C6 C 0.95732(7) 0.27089(13) 0.44180(7) 0.0171(2) Uani 1 1 d . . . . . H6 H 0.992885 0.206526 0.437888 0.021 Uiso 1 1 calc R U . . . C25 C 0.59560(7) 0.21844(13) 0.56073(6) 0.0156(2) Uani 1 1 d . . . . . N7 N 0.32887(10) 0.71799(15) 0.27623(8) 0.0365(3) Uani 1 1 d . . . . . C13 C 0.78160(7) 0.55014(13) 0.66815(7) 0.0178(2) Uani 1 1 d . . . . . H13 H 0.761943 0.630990 0.678113 0.021 Uiso 1 1 calc R U . . . C19 C 0.74758(8) -0.04478(14) 0.52538(7) 0.0209(3) Uani 1 1 d . . . . . H19A H 0.727582 -0.125120 0.540456 0.031 Uiso 1 1 calc R U . . . H19B H 0.770959 -0.060863 0.485311 0.031 Uiso 1 1 calc R U . . . H19C H 0.708139 0.017563 0.515319 0.031 Uiso 1 1 calc R U . . . C16 C 0.87867(7) 0.20396(13) 0.61122(7) 0.0161(2) Uani 1 1 d . . . . . H16A H 0.924552 0.233184 0.595500 0.019 Uiso 1 1 calc R U . . . H16B H 0.891796 0.144124 0.648665 0.019 Uiso 1 1 calc R U . . . C17 C 0.80378(7) 0.00831(12) 0.58001(7) 0.0167(2) Uani 1 1 d . . . . . C12 C 0.82988(8) 0.48641(14) 0.71500(7) 0.0193(3) Uani 1 1 d . . . . . H12 H 0.842281 0.522724 0.757861 0.023 Uiso 1 1 calc R U . . . C21 C 0.67310(7) 0.55227(13) 0.42808(7) 0.0156(2) Uani 1 1 d . . . . . C22 C 0.60153(7) 0.48277(14) 0.43470(7) 0.0207(3) Uani 1 1 d . . . . . H22A H 0.582338 0.511611 0.475168 0.031 Uiso 1 1 calc R U . . . H22B H 0.610267 0.390170 0.437223 0.031 Uiso 1 1 calc R U . . . H22C H 0.566126 0.501994 0.395961 0.031 Uiso 1 1 calc R U . . . C27 C 0.68298(8) 0.14928(13) 0.37350(7) 0.0187(3) Uani 1 1 d . . . . . C18 C 0.76548(8) 0.03632(14) 0.64138(7) 0.0197(3) Uani 1 1 d . . . . . H18A H 0.732137 0.108869 0.632085 0.030 Uiso 1 1 calc R U . . . H18B H 0.801938 0.057389 0.679043 0.030 Uiso 1 1 calc R U . . . H18C H 0.737882 -0.039389 0.652238 0.030 Uiso 1 1 calc R U . . . C9 C 1.03394(8) 0.42647(15) 0.38455(8) 0.0229(3) Uani 1 1 d . . . . . H9A H 1.018139 0.461141 0.340207 0.034 Uiso 1 1 calc R U . . . H9B H 1.062773 0.348689 0.380503 0.034 Uiso 1 1 calc R U . . . H9C H 1.063720 0.490323 0.410872 0.034 Uiso 1 1 calc R U . . . C20 C 0.86417(8) -0.09207(14) 0.59670(8) 0.0227(3) Uani 1 1 d . . . . . H20A H 0.844465 -0.165663 0.618668 0.034 Uiso 1 1 calc R U . . . H20B H 0.904238 -0.054017 0.626403 0.034 Uiso 1 1 calc R U . . . H20C H 0.882292 -0.120484 0.555653 0.034 Uiso 1 1 calc R U . . . C26 C 0.52477(8) 0.18811(15) 0.58065(7) 0.0217(3) Uani 1 1 d . . . . . H26A H 0.507787 0.105974 0.561061 0.032 Uiso 1 1 calc R U . . . H26B H 0.489960 0.255638 0.565119 0.032 Uiso 1 1 calc R U . . . H26C H 0.528730 0.182241 0.629198 0.032 Uiso 1 1 calc R U . . . N6 N 0.54762(10) 0.7708(2) 0.26678(9) 0.0482(5) Uani 1 1 d . . . . . C24 C 0.69997(8) 0.51156(14) 0.36268(7) 0.0199(3) Uani 1 1 d . . . . . H24A H 0.661455 0.526616 0.325829 0.030 Uiso 1 1 calc R U . . . H24B H 0.712474 0.420268 0.364694 0.030 Uiso 1 1 calc R U . . . H24C H 0.743179 0.561763 0.355677 0.030 Uiso 1 1 calc R U . . . C29 C 0.59939(10) 0.76330(18) 0.24176(8) 0.0317(4) Uani 1 1 d . . . . . C30 C 0.66628(10) 0.75426(19) 0.21092(9) 0.0325(4) Uani 1 1 d . . . . . H30A H 0.665695 0.818813 0.175752 0.049 Uiso 1 1 calc R U . . . H30B H 0.669973 0.668637 0.191757 0.049 Uiso 1 1 calc R U . . . H30C H 0.708224 0.769240 0.244496 0.049 Uiso 1 1 calc R U . . . C31 C 0.37022(10) 0.63719(16) 0.28369(9) 0.0316(4) Uani 1 1 d . . . . . C28 C 0.64379(10) 0.08769(18) 0.31526(8) 0.0311(4) Uani 1 1 d . . . . . H28A H 0.618781 0.152970 0.286118 0.047 Uiso 1 1 calc R U . . . H28B H 0.607899 0.027664 0.329344 0.047 Uiso 1 1 calc R U . . . H28C H 0.678345 0.041000 0.291152 0.047 Uiso 1 1 calc R U . . . C32 C 0.42233(13) 0.5325(2) 0.29449(12) 0.0500(6) Uani 1 1 d . . . . . H32A H 0.461743 0.545663 0.266966 0.075 Uiso 1 1 calc R U . . . H32B H 0.397705 0.451167 0.282327 0.075 Uiso 1 1 calc R U . . . H32C H 0.442624 0.530059 0.341441 0.075 Uiso 1 1 calc R U . . . 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 Pd1 0.00953(4) 0.01211(4) 0.01265(5) -0.00135(3) 0.00179(3) -0.00107(3) P2 0.01703(16) 0.02229(17) 0.01721(16) -0.00253(13) 0.00129(12) -0.00050(13) P1 0.02745(19) 0.02085(18) 0.02151(18) -0.00329(14) 0.00024(14) -0.00272(15) F7 0.0178(4) 0.0367(5) 0.0240(4) -0.0004(4) -0.0004(3) 0.0024(4) F9 0.0417(6) 0.0243(5) 0.0228(4) -0.0063(4) -0.0067(4) 0.0039(4) F12 0.0288(5) 0.0293(5) 0.0296(5) -0.0113(4) 0.0054(4) -0.0028(4) F11 0.0260(5) 0.0399(6) 0.0271(5) 0.0023(4) 0.0062(4) -0.0093(4) F8 0.0380(6) 0.0303(5) 0.0270(5) 0.0063(4) 0.0125(4) 0.0028(4) F10 0.0228(5) 0.0382(5) 0.0338(5) -0.0042(4) -0.0058(4) 0.0065(4) F4 0.0256(5) 0.0369(6) 0.0473(6) -0.0026(5) 0.0057(4) -0.0064(4) F3 0.0765(9) 0.0307(5) 0.0244(5) -0.0026(4) 0.0063(5) -0.0028(6) F2 0.0319(6) 0.0438(6) 0.0520(7) 0.0117(5) 0.0008(5) 0.0090(5) N1 0.0127(5) 0.0138(5) 0.0131(5) -0.0006(4) 0.0014(4) -0.0019(4) F1 0.0568(8) 0.0473(7) 0.0559(8) 0.0026(6) 0.0030(6) -0.0294(6) N5 0.0150(5) 0.0166(5) 0.0184(5) -0.0022(4) 0.0033(4) -0.0016(4) N4 0.0144(5) 0.0196(5) 0.0175(5) -0.0017(4) 0.0021(4) -0.0006(4) F5 0.0661(9) 0.0316(6) 0.0851(11) 0.0033(6) 0.0153(8) 0.0239(6) F6 0.1062(12) 0.0628(9) 0.0258(6) -0.0212(6) 0.0107(7) -0.0272(9) N2 0.0109(5) 0.0143(5) 0.0143(5) -0.0011(4) 0.0003(4) 0.0007(4) N3 0.0134(5) 0.0128(5) 0.0175(5) 0.0011(4) 0.0037(4) -0.0009(4) C1 0.0107(5) 0.0146(5) 0.0147(5) 0.0003(4) 0.0032(4) -0.0008(4) C5 0.0126(5) 0.0187(6) 0.0195(6) 0.0014(5) 0.0037(5) -0.0016(5) C2 0.0127(5) 0.0137(5) 0.0138(5) 0.0001(4) 0.0011(4) -0.0004(4) C11 0.0187(6) 0.0226(6) 0.0146(6) 0.0019(5) 0.0001(5) -0.0028(5) C3 0.0119(5) 0.0132(5) 0.0168(6) 0.0001(4) 0.0012(4) -0.0002(4) C10 0.0140(6) 0.0142(5) 0.0156(6) 0.0022(4) 0.0015(4) -0.0023(4) C7 0.0138(6) 0.0146(5) 0.0171(6) 0.0010(4) 0.0033(4) 0.0004(4) C4 0.0140(6) 0.0157(6) 0.0187(6) 0.0027(5) 0.0020(5) -0.0022(5) C15 0.0154(6) 0.0159(6) 0.0162(6) -0.0021(4) 0.0022(4) 0.0021(5) C8 0.0156(6) 0.0140(6) 0.0215(6) 0.0017(5) 0.0072(5) 0.0014(5) C23 0.0175(6) 0.0167(6) 0.0224(6) 0.0007(5) -0.0020(5) 0.0034(5) C14 0.0136(5) 0.0155(6) 0.0146(5) -0.0012(4) 0.0032(4) -0.0016(4) C6 0.0136(6) 0.0171(6) 0.0214(6) 0.0010(5) 0.0049(5) 0.0014(5) C25 0.0158(6) 0.0164(6) 0.0143(5) -0.0004(4) 0.0005(4) 0.0014(5) N7 0.0481(9) 0.0279(7) 0.0327(8) 0.0017(6) 0.0018(7) 0.0000(7) C13 0.0184(6) 0.0191(6) 0.0163(6) -0.0039(5) 0.0043(5) -0.0022(5) C19 0.0210(7) 0.0162(6) 0.0263(7) -0.0017(5) 0.0068(5) -0.0053(5) C16 0.0139(6) 0.0157(6) 0.0182(6) 0.0018(5) -0.0008(4) -0.0001(5) C17 0.0167(6) 0.0122(5) 0.0222(6) 0.0026(5) 0.0060(5) -0.0007(5) C12 0.0206(6) 0.0235(7) 0.0140(6) -0.0025(5) 0.0024(5) -0.0041(5) C21 0.0130(6) 0.0157(6) 0.0170(6) -0.0001(4) -0.0029(4) 0.0017(4) C22 0.0137(6) 0.0217(7) 0.0254(7) -0.0002(5) -0.0035(5) -0.0008(5) C27 0.0191(6) 0.0173(6) 0.0202(6) -0.0021(5) 0.0048(5) -0.0019(5) C18 0.0211(6) 0.0180(6) 0.0211(6) 0.0037(5) 0.0075(5) 0.0004(5) C9 0.0160(6) 0.0250(7) 0.0291(7) 0.0041(6) 0.0078(5) -0.0015(5) C20 0.0231(7) 0.0151(6) 0.0313(7) 0.0060(5) 0.0084(6) 0.0041(5) C26 0.0149(6) 0.0272(7) 0.0236(7) 0.0027(5) 0.0055(5) -0.0017(5) N6 0.0455(10) 0.0699(13) 0.0308(8) 0.0039(8) 0.0109(7) 0.0128(9) C24 0.0223(7) 0.0204(6) 0.0160(6) -0.0005(5) -0.0012(5) 0.0012(5) C29 0.0385(9) 0.0364(9) 0.0197(7) 0.0029(6) 0.0016(6) 0.0045(7) C30 0.0314(9) 0.0398(9) 0.0263(8) 0.0009(7) 0.0043(6) -0.0011(7) C31 0.0410(9) 0.0246(8) 0.0266(8) 0.0016(6) -0.0066(7) -0.0059(7) C28 0.0333(9) 0.0372(9) 0.0223(7) -0.0114(6) 0.0011(6) -0.0103(7) C32 0.0541(13) 0.0334(10) 0.0558(13) 0.0010(9) -0.0210(10) 0.0082(9) 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' N N 0.0061 0.0033 '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' 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 N1 Pd1 N5 179.02(4) . . ? N1 Pd1 N4 92.20(4) . . ? N1 Pd1 N2 75.90(4) . . ? N1 Pd1 N3 79.36(4) . . ? N5 Pd1 N4 88.66(4) . . ? N5 Pd1 N2 104.45(4) . . ? N5 Pd1 N3 99.97(4) . . ? N4 Pd1 N2 98.53(4) . . ? N4 Pd1 N3 103.98(4) . . ? N3 Pd1 N2 146.97(4) . . ? C1 Pd1 N1 86.86(5) . . ? C1 Pd1 N5 92.29(5) . . ? C1 Pd1 N4 178.58(5) . . ? C1 Pd1 N2 80.21(5) . . ? C1 Pd1 N3 76.90(5) . . ? F7 P2 F12 90.17(5) . . ? F7 P2 F10 179.64(6) . . ? F9 P2 F7 90.25(5) . . ? F9 P2 F12 179.58(6) . . ? F9 P2 F11 90.11(6) . . ? F9 P2 F10 89.99(6) . . ? F12 P2 F10 89.59(6) . . ? F11 P2 F7 89.67(5) . . ? F11 P2 F12 89.91(6) . . ? F11 P2 F10 90.07(6) . . ? F8 P2 F7 90.34(5) . . ? F8 P2 F9 89.78(6) . . ? F8 P2 F12 90.20(6) . . ? F8 P2 F11 179.89(7) . . ? F8 P2 F10 89.92(6) . . ? F4 P1 F3 90.02(7) . . ? F4 P1 F2 88.79(6) . . ? F4 P1 F1 178.60(8) . . ? F3 P1 F2 88.14(7) . . ? F1 P1 F3 88.81(7) . . ? F1 P1 F2 90.41(7) . . ? F5 P1 F4 91.59(7) . . ? F5 P1 F3 89.43(8) . . ? F5 P1 F2 177.54(8) . . ? F5 P1 F1 89.16(8) . . ? F6 P1 F4 90.70(7) . . ? F6 P1 F3 177.98(9) . . ? F6 P1 F2 90.00(8) . . ? F6 P1 F1 90.44(8) . . ? F6 P1 F5 92.43(9) . . ? C10 N1 Pd1 119.50(9) . . ? C10 N1 C14 122.57(11) . . ? C14 N1 Pd1 117.70(9) . . ? C27 N5 Pd1 170.45(11) . . ? C25 N4 Pd1 175.77(11) . . ? C3 N2 Pd1 103.92(7) . . ? C3 N2 C21 111.29(10) . . ? C15 N2 Pd1 98.39(7) . . ? C15 N2 C3 109.68(10) . . ? C15 N2 C21 113.29(10) . . ? C21 N2 Pd1 119.16(8) . . ? C8 N3 Pd1 100.19(7) . . ? C8 N3 C17 112.88(10) . . ? C16 N3 Pd1 102.95(7) . . ? C16 N3 C8 109.32(10) . . ? C16 N3 C17 112.22(10) . . ? C17 N3 Pd1 118.18(8) . . ? C2 C1 Pd1 118.91(9) . . ? C7 C1 Pd1 117.42(9) . . ? C7 C1 C2 123.66(12) . . ? C4 C5 C6 119.60(12) . . ? C4 C5 C9 119.34(12) . . ? C6 C5 C9 121.05(12) . . ? C1 C2 C3 119.74(11) . . ? C1 C2 C4 117.33(12) . . ? C4 C2 C3 122.70(12) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C12 C11 C10 118.74(13) . . ? N2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C2 C3 N2 112.34(10) . . ? C2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N1 C10 C11 119.80(12) . . ? N1 C10 C16 117.00(11) . . ? C11 C10 C16 122.82(12) . . ? C1 C7 C8 118.22(11) . . ? C1 C7 C6 117.62(12) . . ? C6 C7 C8 124.12(12) . . ? C5 C4 H4 119.6 . . ? C2 C4 C5 120.76(12) . . ? C2 C4 H4 119.6 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 C14 110.89(10) . . ? H15A C15 H15B 108.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? N3 C8 C7 108.45(10) . . ? N3 C8 H8A 110.0 . . ? N3 C8 H8B 110.0 . . ? C7 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? N1 C14 C15 116.49(11) . . ? N1 C14 C13 119.70(12) . . ? C13 C14 C15 123.81(12) . . ? C5 C6 H6 119.7 . . ? C7 C6 C5 120.62(12) . . ? C7 C6 H6 119.7 . . ? N4 C25 C26 178.69(15) . . ? C14 C13 H13 120.6 . . ? C14 C13 C12 118.72(13) . . ? C12 C13 H13 120.6 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? N3 C16 C10 114.80(11) . . ? N3 C16 H16A 108.6 . . ? N3 C16 H16B 108.6 . . ? C10 C16 H16A 108.6 . . ? C10 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? N3 C17 C19 109.25(11) . . ? N3 C17 C18 109.05(11) . . ? N3 C17 C20 110.86(11) . . ? C19 C17 C18 108.48(11) . . ? C19 C17 C20 108.90(12) . . ? C18 C17 C20 110.25(12) . . ? C11 C12 C13 120.37(13) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N2 C21 C23 111.29(10) . . ? N2 C21 C22 109.63(11) . . ? N2 C21 C24 108.46(10) . . ? C22 C21 C23 109.62(11) . . ? C22 C21 C24 108.65(11) . . ? C24 C21 C23 109.14(11) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C27 C28 179.21(17) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C29 C30 179.0(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 C32 178.7(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0201(11) . ? Pd1 N5 2.0937(11) . ? Pd1 N4 2.1626(12) . ? Pd1 N2 2.3955(11) . ? Pd1 N3 2.3819(11) . ? Pd1 C1 1.9588(12) . ? P2 F7 1.6034(10) . ? P2 F9 1.6008(10) . ? P2 F12 1.6081(10) . ? P2 F11 1.6016(10) . ? P2 F8 1.5977(10) . ? P2 F10 1.6099(10) . ? P1 F4 1.5927(11) . ? P1 F3 1.6066(11) . ? P1 F2 1.6118(12) . ? P1 F1 1.6050(12) . ? P1 F5 1.5845(13) . ? P1 F6 1.5711(12) . ? N1 C10 1.3433(16) . ? N1 C14 1.3467(17) . ? N5 C27 1.1370(18) . ? N4 C25 1.1392(18) . ? N2 C3 1.5060(16) . ? N2 C15 1.4900(16) . ? N2 C21 1.5209(16) . ? N3 C8 1.5020(17) . ? N3 C16 1.4938(17) . ? N3 C17 1.5231(17) . ? C1 C2 1.3867(18) . ? C1 C7 1.3828(18) . ? C5 C4 1.3973(19) . ? C5 C6 1.3977(19) . ? C5 C9 1.5052(19) . ? C2 C3 1.5047(18) . ? C2 C4 1.3966(18) . ? C11 H11 0.9500 . ? C11 C10 1.3887(18) . ? C11 C12 1.388(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C10 C16 1.5090(19) . ? C7 C8 1.5062(18) . ? C7 C6 1.3951(18) . ? C4 H4 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C14 1.5105(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 C21 1.5397(19) . ? C14 C13 1.3883(18) . ? C6 H6 0.9500 . ? C25 C26 1.4516(19) . ? N7 C31 1.136(2) . ? C13 H13 0.9500 . ? C13 C12 1.391(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 C17 1.527(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.5327(19) . ? C17 C20 1.5384(19) . ? C12 H12 0.9500 . ? C21 C22 1.5292(19) . ? C21 C24 1.5315(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C27 C28 1.457(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N6 C29 1.139(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C29 C30 1.455(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.456(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 Pd1 N1 C10 C11 -170.63(10) . . . . ? Pd1 N1 C10 C16 16.24(15) . . . . ? Pd1 N1 C14 C15 -8.39(15) . . . . ? Pd1 N1 C14 C13 172.24(10) . . . . ? Pd1 N2 C3 C2 21.97(11) . . . . ? Pd1 N2 C15 C14 43.64(11) . . . . ? Pd1 N2 C21 C23 173.00(8) . . . . ? Pd1 N2 C21 C22 51.56(13) . . . . ? Pd1 N2 C21 C24 -66.93(12) . . . . ? Pd1 N3 C8 C7 41.04(11) . . . . ? Pd1 N3 C16 C10 24.56(12) . . . . ? Pd1 N3 C17 C19 48.66(13) . . . . ? Pd1 N3 C17 C18 -69.76(12) . . . . ? Pd1 N3 C17 C20 168.68(9) . . . . ? Pd1 C1 C2 C3 11.38(16) . . . . ? Pd1 C1 C2 C4 -173.99(9) . . . . ? Pd1 C1 C7 C8 -7.82(16) . . . . ? Pd1 C1 C7 C6 174.44(10) . . . . ? N1 C10 C16 N3 -29.28(16) . . . . ? N1 C14 C13 C12 -0.61(19) . . . . ? N2 C15 C14 N1 -29.81(16) . . . . ? N2 C15 C14 C13 149.54(12) . . . . ? C1 C2 C3 N2 -24.33(16) . . . . ? C1 C2 C4 C5 -1.90(19) . . . . ? C1 C7 C8 N3 -28.07(16) . . . . ? C1 C7 C6 C5 1.0(2) . . . . ? C2 C1 C7 C8 171.21(12) . . . . ? C2 C1 C7 C6 -6.5(2) . . . . ? C11 C10 C16 N3 157.82(12) . . . . ? C3 N2 C15 C14 -64.48(13) . . . . ? C3 N2 C21 C23 -66.12(14) . . . . ? C3 N2 C21 C22 172.44(11) . . . . ? C3 N2 C21 C24 53.94(13) . . . . ? C3 C2 C4 C5 172.56(12) . . . . ? C10 N1 C14 C15 177.15(12) . . . . ? C10 N1 C14 C13 -2.23(19) . . . . ? C10 C11 C12 C13 -0.4(2) . . . . ? C7 C1 C2 C3 -167.63(12) . . . . ? C7 C1 C2 C4 7.0(2) . . . . ? C4 C5 C6 C7 3.7(2) . . . . ? C4 C2 C3 N2 161.34(12) . . . . ? C15 N2 C3 C2 126.35(11) . . . . ? C15 N2 C21 C23 58.03(14) . . . . ? C15 N2 C21 C22 -63.41(14) . . . . ? C15 N2 C21 C24 178.09(11) . . . . ? C15 C14 C13 C12 -179.94(12) . . . . ? C8 N3 C16 C10 130.40(11) . . . . ? C8 N3 C17 C19 -67.70(14) . . . . ? C8 N3 C17 C18 173.88(11) . . . . ? C8 N3 C17 C20 52.32(15) . . . . ? C8 C7 C6 C5 -176.65(13) . . . . ? C14 N1 C10 C11 3.73(19) . . . . ? C14 N1 C10 C16 -169.39(11) . . . . ? C14 C13 C12 C11 1.9(2) . . . . ? C6 C5 C4 C2 -3.3(2) . . . . ? C6 C7 C8 N3 149.52(13) . . . . ? C16 N3 C8 C7 -66.67(13) . . . . ? C16 N3 C17 C19 168.23(11) . . . . ? C16 N3 C17 C18 49.81(14) . . . . ? C16 N3 C17 C20 -71.75(14) . . . . ? C17 N3 C8 C7 167.67(11) . . . . ? C17 N3 C16 C10 -103.57(12) . . . . ? C12 C11 C10 N1 -2.3(2) . . . . ? C12 C11 C10 C16 170.37(12) . . . . ? C21 N2 C3 C2 -107.48(12) . . . . ? C21 N2 C15 C14 170.50(10) . . . . ? C9 C5 C4 C2 177.94(13) . . . . ? C9 C5 C6 C7 -177.46(13) . . . . ?