#------------------------------------------------------------------------------ #$Date: 2026-05-27 23:11:25 +0100 (Wed, 27 May 2026) $ #$Revision: 306105 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/72/1577298.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_1577298 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 H41 N5 Pd, 2(B F4), C2 H3 N' _chemical_formula_sum 'C30 H44 B2 F8 N6 Pd' _chemical_formula_weight 768.73 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-04-18 _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 85.0080(10) _cell_angle_beta 84.3020(10) _cell_angle_gamma 86.3840(10) _cell_formula_units_Z 2 _cell_length_a 7.7290(3) _cell_length_b 9.6870(4) _cell_length_c 22.8572(9) _cell_measurement_reflns_used 30350 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 26.412 _cell_measurement_theta_min 2.363 _cell_volume 1693.86(12) _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_detector 'Bruker Photon II area detector' _diffrn_detector_type 'CPAD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture/Photon II' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 72887 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.440 _diffrn_reflns_theta_min 2.114 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.7002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0689 before and 0.0600 after correction. The Ratio of minimum to maximum transmission is 0.9394. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.507 _exptl_crystal_description plate _exptl_crystal_F_000 788 _exptl_crystal_size_max 0.115 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.023 _refine_diff_density_max 0.658 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 464 _refine_ls_number_reflns 6961 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.101 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0273 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+1.7988P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.0641 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6481 _reflns_number_total 6961 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc03081e2.cif _cod_data_source_block p1 _cod_database_code 1577298 _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. ; _olex2_refinement_description ; 1. Restrained distances F8A-B2 \\sim F8B-B2 with sigma of 0.02 F7A-B2 \\sim F7B-B2 with sigma of 0.02 F7A-F8B \\sim F7B-F8B with sigma of 0.02 F6A-B2 \\sim F6B-B2 with sigma of 0.02 2. Others Sof(F8B)=1-FVAR(1) Sof(F8A)=FVAR(1) Sof(F7B)=1-FVAR(2) Sof(F7A)=FVAR(2) Sof(F6B)=1-FVAR(3) Sof(F6A)=FVAR(3) 3.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C10(H10A,H10B), C16(H16A,H16B), C8(H8A,H8B) 3.b Aromatic/amide H refined with riding coordinates: C14(H14), C1(H1), C13(H13), C4(H4), C12(H12), C6(H6) 3.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C18(H18A,H18B, H18C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C19(H19A, H19B,H19C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C) ; _shelx_res_file ; TITL p1_a.res in P-1 p1.res created by SHELXL-2016/4 at 14:26:01 on 06-Apr-2023 REM Old TITL P1 in P1 REM SHELXT solution in P-1 REM R1 0.096, Rweak 0.010, Alpha 0.051, Orientation as input REM Formula found by SHELXT: C32 N6 F8 Pd CELL 0.71073 7.729 9.687 22.8572 85.008 84.302 86.384 ZERR 2 0.0003 0.0004 0.0009 0.001 0.001 0.001 LATT 1 SFAC C H B F N Pd UNIT 60 88 4 16 12 2 SADI F8A B2 F8B B2 SADI F7A B2 F7B B2 SADI F7A F8B F7B F8B SADI F6A B2 F6B B2 L.S. 20 PLAN 4 TEMP -173.15 CONF BOND $H list 4 MORE -1 fmap 2 ACTA REM REM REM WGHT 0.021700 1.798800 FVAR 0.40335 0.61955 0.65638 0.47311 PD1 6 0.457432 0.607034 0.718125 11.00000 0.01736 0.01351 = 0.01509 0.00154 -0.00046 0.00198 F1 4 0.760763 0.802024 0.770001 11.00000 0.04762 0.01653 = 0.02929 0.00151 0.00100 0.00315 F4 4 0.620337 0.995975 0.730266 11.00000 0.07344 0.02318 = 0.03708 0.00198 -0.01201 0.01056 F3 4 0.787589 1.011624 0.804256 11.00000 0.05325 0.03401 = 0.06096 -0.02126 -0.00908 0.00178 N2 5 0.321305 0.477055 0.776278 11.00000 0.01742 0.01622 = 0.01430 -0.00064 -0.00372 -0.00102 N1 5 0.641389 0.441373 0.718708 11.00000 0.02006 0.01634 = 0.01913 0.00167 0.00109 0.00281 N3 5 0.166096 0.647566 0.906168 11.00000 0.01787 0.01634 = 0.01519 -0.00208 -0.00211 -0.00100 F2 4 0.530700 0.907154 0.822460 11.00000 0.05392 0.03905 = 0.06512 0.01043 0.02698 0.00747 N4 5 0.260091 0.752051 0.713610 11.00000 0.02504 0.01896 = 0.01801 0.00075 0.00189 0.00071 N5 5 0.579876 0.741687 0.658365 11.00000 0.02576 0.02105 = 0.01975 0.00151 0.00009 0.00243 C2 1 0.655838 0.430259 0.830481 11.00000 0.01263 0.02164 = 0.02097 0.00149 -0.00470 -0.00218 C15 1 0.197383 0.508700 0.820000 11.00000 0.01495 0.01788 = 0.01413 -0.00053 -0.00492 0.00064 C14 1 0.097232 0.404542 0.848052 11.00000 0.01605 0.02060 = 0.01897 -0.00092 -0.00419 -0.00202 AFIX 43 H14 2 0.006295 0.426409 0.877446 11.00000 -1.20000 AFIX 0 C1 1 0.569699 0.545376 0.854666 11.00000 0.01656 0.01684 = 0.01993 0.00182 -0.00637 -0.00308 AFIX 43 H1 2 0.587228 0.635407 0.835818 11.00000 -1.20000 AFIX 0 C3 1 0.753325 0.446130 0.770026 11.00000 0.01751 0.02186 = 0.02251 0.00284 -0.00202 0.00139 AFIX 23 H3A 2 0.846486 0.371373 0.767242 11.00000 -1.20000 H3B 2 0.810105 0.535727 0.765652 11.00000 -1.20000 AFIX 0 C7 1 0.458353 0.530198 0.906057 11.00000 0.01721 0.01981 = 0.01963 -0.00277 -0.00792 -0.00353 C13 1 0.128487 0.268715 0.833627 11.00000 0.02117 0.01957 = 0.02377 0.00259 -0.00680 -0.00625 AFIX 43 H13 2 0.053668 0.198793 0.850575 11.00000 -1.20000 AFIX 0 C5 1 0.537222 0.282674 0.914154 11.00000 0.01914 0.01970 = 0.02086 0.00243 -0.00915 -0.00416 C4 1 0.641703 0.299909 0.861134 11.00000 0.01698 0.01980 = 0.02440 0.00043 -0.00758 0.00170 AFIX 43 H4 2 0.704403 0.221654 0.845566 11.00000 -1.20000 AFIX 0 C10 1 0.528978 0.317893 0.727448 11.00000 0.02440 0.01451 = 0.02205 -0.00084 -0.00046 0.00170 AFIX 23 H10A 2 0.497516 0.295171 0.688590 11.00000 -1.20000 H10B 2 0.596803 0.236813 0.744566 11.00000 -1.20000 AFIX 0 C12 1 0.269758 0.235938 0.794291 11.00000 0.02341 0.01451 = 0.02398 -0.00164 -0.00674 -0.00062 AFIX 43 H12 2 0.299825 0.142410 0.786256 11.00000 -1.20000 AFIX 0 C16 1 0.177854 0.654525 0.841002 11.00000 0.01857 0.01588 = 0.01629 -0.00044 -0.00243 -0.00094 AFIX 23 H16A 2 0.279225 0.707530 0.824333 11.00000 -1.20000 H16B 2 0.071548 0.703426 0.826912 11.00000 -1.20000 AFIX 0 C11 1 0.366103 0.343058 0.766961 11.00000 0.02039 0.01793 = 0.01527 -0.00143 -0.00556 0.00141 C8 1 0.342252 0.651367 0.926517 11.00000 0.02064 0.01942 = 0.01835 -0.00249 -0.00488 -0.00326 AFIX 23 H8A 2 0.332614 0.648016 0.970126 11.00000 -1.20000 H8B 2 0.394524 0.739323 0.910754 11.00000 -1.20000 AFIX 0 C21 1 0.036679 0.752445 0.932358 11.00000 0.01982 0.01895 = 0.01898 -0.00415 0.00020 -0.00087 C25 1 0.167106 0.841471 0.700692 11.00000 0.02467 0.02084 = 0.02634 0.00293 0.00465 0.00189 C6 1 0.444559 0.398543 0.935455 11.00000 0.01885 0.02495 = 0.01587 0.00050 -0.00521 -0.00476 AFIX 43 H6 2 0.369919 0.387684 0.970966 11.00000 -1.20000 AFIX 0 C27 1 0.615336 0.833404 0.625957 11.00000 0.02424 0.02331 = 0.02317 0.00054 -0.00110 0.00142 C9 1 0.518556 0.139858 0.945643 11.00000 0.03101 0.02044 = 0.02667 0.00443 -0.00411 -0.00418 AFIX 137 H9A 2 0.401023 0.109988 0.942911 11.00000 -1.50000 H9B 2 0.538128 0.142807 0.987214 11.00000 -1.50000 H9C 2 0.604413 0.074172 0.927222 11.00000 -1.50000 AFIX 0 F5 4 0.284613 0.650933 0.566835 11.00000 0.06293 0.06748 = 0.15252 -0.00161 0.00170 0.01727 C17 1 0.766505 0.428053 0.660829 11.00000 0.02867 0.02314 = 0.02201 0.00166 0.00761 0.00650 PART 1 F6A 4 0.035498 0.786794 0.566657 41.00000 0.02936 0.05018 = 0.06393 -0.00462 0.01141 -0.00953 PART 0 C22 1 -0.144397 0.721433 0.917233 11.00000 0.02021 0.02763 = 0.02156 -0.00368 0.00054 -0.00060 AFIX 137 H22A 2 -0.148599 0.733360 0.874371 11.00000 -1.50000 H22B 2 -0.231599 0.785365 0.936127 11.00000 -1.50000 H22C 2 -0.169106 0.625689 0.931503 11.00000 -1.50000 AFIX 0 C28 1 0.662806 0.950155 0.584300 11.00000 0.05123 0.03057 = 0.03316 0.01393 -0.00026 -0.00296 AFIX 137 H28A 2 0.592788 0.953356 0.550687 11.00000 -1.50000 H28B 2 0.786564 0.939161 0.570355 11.00000 -1.50000 H28C 2 0.641047 1.036605 0.603793 11.00000 -1.50000 AFIX 0 C18 1 0.909235 0.531416 0.657105 11.00000 0.02660 0.03046 = 0.03018 0.00850 0.00895 0.00345 AFIX 137 H18A 2 0.857708 0.621998 0.667657 11.00000 -1.50000 H18B 2 0.966098 0.540426 0.616789 11.00000 -1.50000 H18C 2 0.995483 0.498147 0.684481 11.00000 -1.50000 AFIX 0 C24 1 0.034015 0.733790 0.999921 11.00000 0.02752 0.03344 = 0.01949 -0.00841 -0.00151 -0.00147 AFIX 137 H24A 2 0.027851 0.635104 1.013175 11.00000 -1.50000 H24B 2 -0.067829 0.785702 1.017738 11.00000 -1.50000 H24C 2 0.140325 0.768671 1.011918 11.00000 -1.50000 AFIX 0 C26 1 0.048707 0.957905 0.684603 11.00000 0.03570 0.02946 = 0.06786 0.01727 0.01097 0.01508 AFIX 137 H26A 2 0.103463 1.014661 0.651072 11.00000 -1.50000 H26B 2 0.021808 1.014417 0.718219 11.00000 -1.50000 H26C 2 -0.059044 0.923203 0.673662 11.00000 -1.50000 AFIX 0 C20 1 0.659877 0.451649 0.607388 11.00000 0.04147 0.03017 = 0.02022 -0.00077 0.00576 0.00285 AFIX 137 H20A 2 0.569166 0.384332 0.611000 11.00000 -1.50000 H20B 2 0.736685 0.439753 0.571198 11.00000 -1.50000 H20C 2 0.605630 0.545943 0.605808 11.00000 -1.50000 AFIX 0 C19 1 0.853987 0.281001 0.660735 11.00000 0.03801 0.02542 = 0.03519 0.00090 0.01192 0.01129 AFIX 137 H19A 2 0.918188 0.261679 0.695685 11.00000 -1.50000 H19B 2 0.934760 0.274396 0.625098 11.00000 -1.50000 H19C 2 0.764761 0.213222 0.661361 11.00000 -1.50000 AFIX 0 C23 1 0.077158 0.902711 0.910379 11.00000 0.02762 0.01717 = 0.03681 -0.00471 0.00109 0.00004 AFIX 137 H23A 2 0.194498 0.920908 0.919448 11.00000 -1.50000 H23B 2 -0.007929 0.966958 0.930052 11.00000 -1.50000 H23C 2 0.070686 0.915960 0.867639 11.00000 -1.50000 AFIX 0 N6 5 0.311594 1.197202 0.626190 11.00000 0.04518 0.06938 = 0.05138 0.00989 -0.01214 -0.02194 PART 1 F8A 4 0.292376 0.890754 0.550438 21.00000 0.06430 0.07030 = 0.05813 -0.00317 -0.00850 -0.03932 PART 0 C29 1 0.297369 1.252451 0.581133 11.00000 0.03553 0.05665 = 0.04086 -0.00178 -0.00168 -0.01062 PART 1 F7A 4 0.177129 0.783151 0.480824 31.00000 0.13465 0.06101 = 0.03352 -0.01126 -0.00128 -0.03356 PART 0 B1 3 0.673292 0.929365 0.782172 11.00000 0.03988 0.01806 = 0.03024 0.00148 0.00247 0.00087 C30 1 0.280960 1.327139 0.524210 11.00000 0.07432 0.07447 = 0.03501 0.00225 -0.00386 -0.00280 AFIX 137 H30A 2 0.387855 1.310951 0.498308 11.00000 -1.50000 H30B 2 0.261951 1.426632 0.529077 11.00000 -1.50000 H30C 2 0.181949 1.294468 0.506655 11.00000 -1.50000 AFIX 0 B2 3 0.203482 0.769934 0.540815 11.00000 0.03378 0.05710 = 0.03639 -0.00975 0.00347 -0.00487 PART 2 F8B 4 0.336356 0.812244 0.509453 -21.00000 0.05122 0.08524 = 0.12561 0.04966 0.02704 -0.00816 F7B 4 0.099257 0.687979 0.511137 -31.00000 0.04929 0.11772 = 0.05726 -0.03434 -0.01194 -0.01278 F6B 4 0.089835 0.820897 0.581173 -41.00000 0.14295 0.08258 = 0.04723 -0.00722 0.00853 0.05819 HKLF 4 REM p1_a.res in P-1 REM R1 = 0.0273 for 6481 Fo > 4sig(Fo) and 0.0309 for all 6961 data REM 464 parameters refined using 3 restraints END WGHT 0.0217 1.7983 REM Highest difference peak 0.658, deepest hole -0.549, 1-sigma level 0.062 Q1 1 0.2131 0.6271 0.5383 11.00000 0.05 0.66 Q2 1 0.3507 0.7159 0.5373 11.00000 0.05 0.47 Q3 1 0.0341 0.7438 0.9637 11.00000 0.05 0.36 Q4 1 0.1962 0.5777 0.8310 11.00000 0.05 0.35 ; _shelx_res_checksum 41893 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.45743(2) 0.60703(2) 0.71813(2) 0.01567(5) Uani 1 1 d . . . . . F1 F 0.76076(19) 0.80202(13) 0.77000(6) 0.0319(3) Uani 1 1 d . . . . . F4 F 0.6203(2) 0.99598(15) 0.73027(7) 0.0449(4) Uani 1 1 d . . . . . F3 F 0.7876(2) 1.01162(16) 0.80426(8) 0.0483(4) Uani 1 1 d . . . . . N2 N 0.3213(2) 0.47705(17) 0.77628(7) 0.0159(3) Uani 1 1 d . . . . . N1 N 0.6414(2) 0.44137(17) 0.71871(7) 0.0191(4) Uani 1 1 d . . . . . N3 N 0.1661(2) 0.64757(17) 0.90617(7) 0.0164(3) Uani 1 1 d . . . . . F2 F 0.5307(2) 0.90715(17) 0.82246(8) 0.0562(5) Uani 1 1 d . . . . . N4 N 0.2601(2) 0.75205(18) 0.71361(8) 0.0211(4) Uani 1 1 d . . . . . N5 N 0.5799(2) 0.74169(19) 0.65836(8) 0.0227(4) Uani 1 1 d . . . . . C2 C 0.6558(3) 0.4303(2) 0.83048(9) 0.0183(4) Uani 1 1 d . . . . . C15 C 0.1974(2) 0.5087(2) 0.82000(8) 0.0155(4) Uani 1 1 d . . . . . C14 C 0.0972(3) 0.4045(2) 0.84805(9) 0.0184(4) Uani 1 1 d . . . . . H14 H 0.006295 0.426409 0.877446 0.022 Uiso 1 1 calc R U . . . C1 C 0.5697(3) 0.5454(2) 0.85467(9) 0.0176(4) Uani 1 1 d . . . . . H1 H 0.587228 0.635407 0.835818 0.021 Uiso 1 1 calc R U . . . C3 C 0.7533(3) 0.4461(2) 0.77003(9) 0.0210(4) Uani 1 1 d . . . . . H3A H 0.846486 0.371373 0.767242 0.025 Uiso 1 1 calc R U . . . H3B H 0.810105 0.535727 0.765652 0.025 Uiso 1 1 calc R U . . . C7 C 0.4584(3) 0.5302(2) 0.90606(9) 0.0183(4) Uani 1 1 d . . . . . C13 C 0.1285(3) 0.2687(2) 0.83363(9) 0.0212(4) Uani 1 1 d . . . . . H13 H 0.053668 0.198793 0.850575 0.025 Uiso 1 1 calc R U . . . C5 C 0.5372(3) 0.2827(2) 0.91415(9) 0.0195(4) Uani 1 1 d . . . . . C4 C 0.6417(3) 0.2999(2) 0.86113(9) 0.0203(4) Uani 1 1 d . . . . . H4 H 0.704403 0.221654 0.845566 0.024 Uiso 1 1 calc R U . . . C10 C 0.5290(3) 0.3179(2) 0.72745(9) 0.0206(4) Uani 1 1 d . . . . . H10A H 0.497516 0.295171 0.688590 0.025 Uiso 1 1 calc R U . . . H10B H 0.596803 0.236813 0.744566 0.025 Uiso 1 1 calc R U . . . C12 C 0.2698(3) 0.2359(2) 0.79429(9) 0.0203(4) Uani 1 1 d . . . . . H12 H 0.299825 0.142410 0.786256 0.024 Uiso 1 1 calc R U . . . C16 C 0.1779(3) 0.6545(2) 0.84100(8) 0.0169(4) Uani 1 1 d . . . . . H16A H 0.279225 0.707530 0.824333 0.020 Uiso 1 1 calc R U . . . H16B H 0.071548 0.703426 0.826912 0.020 Uiso 1 1 calc R U . . . C11 C 0.3661(3) 0.3431(2) 0.76696(8) 0.0177(4) Uani 1 1 d . . . . . C8 C 0.3423(3) 0.6514(2) 0.92652(9) 0.0191(4) Uani 1 1 d . . . . . H8A H 0.332614 0.648016 0.970126 0.023 Uiso 1 1 calc R U . . . H8B H 0.394524 0.739323 0.910754 0.023 Uiso 1 1 calc R U . . . C21 C 0.0367(3) 0.7524(2) 0.93236(9) 0.0192(4) Uani 1 1 d . . . . . C25 C 0.1671(3) 0.8415(2) 0.70069(10) 0.0248(5) Uani 1 1 d . . . . . C6 C 0.4446(3) 0.3985(2) 0.93546(9) 0.0196(4) Uani 1 1 d . . . . . H6 H 0.369919 0.387684 0.970966 0.024 Uiso 1 1 calc R U . . . C27 C 0.6153(3) 0.8334(2) 0.62596(10) 0.0239(5) Uani 1 1 d . . . . . C9 C 0.5186(3) 0.1399(2) 0.94564(10) 0.0262(5) Uani 1 1 d . . . . . H9A H 0.401023 0.109988 0.942911 0.039 Uiso 1 1 calc R U . . . H9B H 0.538128 0.142807 0.987214 0.039 Uiso 1 1 calc R U . . . H9C H 0.604413 0.074172 0.927222 0.039 Uiso 1 1 calc R U . . . F5 F 0.2846(3) 0.6509(2) 0.56683(14) 0.0964(8) Uani 1 1 d . . . . . C17 C 0.7665(3) 0.4281(2) 0.66083(10) 0.0258(5) Uani 1 1 d . . . . . F6A F 0.0355(7) 0.7868(8) 0.5667(6) 0.049(2) Uani 0.47(3) 1 d D . P A 1 C22 C -0.1444(3) 0.7214(2) 0.91723(9) 0.0232(4) Uani 1 1 d . . . . . H22A H -0.148599 0.733360 0.874371 0.035 Uiso 1 1 calc R U . . . H22B H -0.231599 0.785365 0.936127 0.035 Uiso 1 1 calc R U . . . H22C H -0.169106 0.625689 0.931503 0.035 Uiso 1 1 calc R U . . . C28 C 0.6628(4) 0.9502(3) 0.58430(12) 0.0395(6) Uani 1 1 d . . . . . H28A H 0.592788 0.953356 0.550687 0.059 Uiso 1 1 calc R U . . . H28B H 0.786564 0.939161 0.570355 0.059 Uiso 1 1 calc R U . . . H28C H 0.641047 1.036605 0.603793 0.059 Uiso 1 1 calc R U . . . C18 C 0.9092(3) 0.5314(2) 0.65711(11) 0.0307(5) Uani 1 1 d . . . . . H18A H 0.857708 0.621998 0.667657 0.046 Uiso 1 1 calc R U . . . H18B H 0.966098 0.540426 0.616789 0.046 Uiso 1 1 calc R U . . . H18C H 0.995483 0.498147 0.684481 0.046 Uiso 1 1 calc R U . . . C24 C 0.0340(3) 0.7338(2) 0.99992(9) 0.0265(5) Uani 1 1 d . . . . . H24A H 0.027851 0.635104 1.013175 0.040 Uiso 1 1 calc R U . . . H24B H -0.067829 0.785702 1.017738 0.040 Uiso 1 1 calc R U . . . H24C H 0.140325 0.768671 1.011918 0.040 Uiso 1 1 calc R U . . . C26 C 0.0487(4) 0.9579(3) 0.68460(14) 0.0474(8) Uani 1 1 d . . . . . H26A H 0.103463 1.014661 0.651072 0.071 Uiso 1 1 calc R U . . . H26B H 0.021808 1.014417 0.718219 0.071 Uiso 1 1 calc R U . . . H26C H -0.059044 0.923203 0.673662 0.071 Uiso 1 1 calc R U . . . C20 C 0.6599(3) 0.4516(3) 0.60739(10) 0.0315(5) Uani 1 1 d . . . . . H20A H 0.569166 0.384332 0.611000 0.047 Uiso 1 1 calc R U . . . H20B H 0.736685 0.439753 0.571198 0.047 Uiso 1 1 calc R U . . . H20C H 0.605630 0.545943 0.605808 0.047 Uiso 1 1 calc R U . . . C19 C 0.8540(3) 0.2810(2) 0.66073(11) 0.0347(6) Uani 1 1 d . . . . . H19A H 0.918188 0.261679 0.695685 0.052 Uiso 1 1 calc R U . . . H19B H 0.934760 0.274396 0.625098 0.052 Uiso 1 1 calc R U . . . H19C H 0.764761 0.213222 0.661361 0.052 Uiso 1 1 calc R U . . . C23 C 0.0772(3) 0.9027(2) 0.91038(11) 0.0274(5) Uani 1 1 d . . . . . H23A H 0.194498 0.920908 0.919448 0.041 Uiso 1 1 calc R U . . . H23B H -0.007929 0.966958 0.930052 0.041 Uiso 1 1 calc R U . . . H23C H 0.070686 0.915960 0.867639 0.041 Uiso 1 1 calc R U . . . N6 N 0.3116(3) 1.1972(3) 0.62619(12) 0.0549(7) Uani 1 1 d . . . . . F8A F 0.2924(5) 0.8908(4) 0.55044(16) 0.0627(15) Uani 0.620(8) 1 d D . P A 1 C29 C 0.2974(4) 1.2525(3) 0.58113(13) 0.0443(7) Uani 1 1 d . . . . . F7A F 0.1771(6) 0.7832(3) 0.48082(12) 0.0752(14) Uani 0.656(6) 1 d D . P A 1 B1 B 0.6733(4) 0.9294(3) 0.78217(12) 0.0301(6) Uani 1 1 d . . . . . C30 C 0.2810(5) 1.3271(4) 0.52421(14) 0.0618(9) Uani 1 1 d . . . . . H30A H 0.387855 1.310951 0.498308 0.093 Uiso 1 1 calc R U . . . H30B H 0.261951 1.426632 0.529077 0.093 Uiso 1 1 calc R U . . . H30C H 0.181949 1.294468 0.506655 0.093 Uiso 1 1 calc R U . . . B2 B 0.2035(4) 0.7699(4) 0.54081(14) 0.0424(7) Uani 1 1 d D . . . . F8B F 0.3364(7) 0.8122(8) 0.5095(4) 0.093(4) Uani 0.380(8) 1 d D . P A 2 F7B F 0.0993(7) 0.6880(8) 0.5111(3) 0.072(3) Uani 0.344(6) 1 d D . P A 2 F6B F 0.090(3) 0.8209(18) 0.5812(4) 0.095(5) Uani 0.53(3) 1 d D . P A 2 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 0.01736(8) 0.01351(8) 0.01509(8) 0.00154(5) -0.00046(5) 0.00198(5) F1 0.0476(9) 0.0165(6) 0.0293(7) 0.0015(5) 0.0010(6) 0.0031(6) F4 0.0734(12) 0.0232(7) 0.0371(8) 0.0020(6) -0.0120(8) 0.0106(7) F3 0.0532(10) 0.0340(8) 0.0610(11) -0.0213(8) -0.0091(8) 0.0018(7) N2 0.0174(8) 0.0162(8) 0.0143(8) -0.0006(6) -0.0037(6) -0.0010(7) N1 0.0201(9) 0.0163(8) 0.0191(8) 0.0017(7) 0.0011(7) 0.0028(7) N3 0.0179(8) 0.0163(8) 0.0152(8) -0.0021(6) -0.0021(6) -0.0010(7) F2 0.0539(11) 0.0391(9) 0.0651(11) 0.0104(8) 0.0270(9) 0.0075(8) N4 0.0250(9) 0.0190(9) 0.0180(9) 0.0008(7) 0.0019(7) 0.0007(8) N5 0.0258(10) 0.0210(9) 0.0198(9) 0.0015(7) 0.0001(7) 0.0024(8) C2 0.0126(9) 0.0216(10) 0.0210(10) 0.0015(8) -0.0047(8) -0.0022(8) C15 0.0149(9) 0.0179(10) 0.0141(9) -0.0005(7) -0.0049(7) 0.0006(8) C14 0.0160(10) 0.0206(10) 0.0190(10) -0.0009(8) -0.0042(8) -0.0020(8) C1 0.0166(10) 0.0168(10) 0.0199(10) 0.0018(8) -0.0064(8) -0.0031(8) C3 0.0175(10) 0.0219(10) 0.0225(10) 0.0028(8) -0.0020(8) 0.0014(8) C7 0.0172(10) 0.0198(10) 0.0196(10) -0.0028(8) -0.0079(8) -0.0035(8) C13 0.0212(10) 0.0196(10) 0.0238(10) 0.0026(8) -0.0068(8) -0.0062(8) C5 0.0191(10) 0.0197(10) 0.0209(10) 0.0024(8) -0.0092(8) -0.0042(8) C4 0.0170(10) 0.0198(10) 0.0244(10) 0.0004(8) -0.0076(8) 0.0017(8) C10 0.0244(11) 0.0145(10) 0.0220(10) -0.0008(8) -0.0005(8) 0.0017(8) C12 0.0234(11) 0.0145(9) 0.0240(10) -0.0016(8) -0.0067(8) -0.0006(8) C16 0.0186(10) 0.0159(9) 0.0163(9) -0.0004(7) -0.0024(7) -0.0009(8) C11 0.0204(10) 0.0179(10) 0.0153(9) -0.0014(7) -0.0056(8) 0.0014(8) C8 0.0206(10) 0.0194(10) 0.0184(10) -0.0025(8) -0.0049(8) -0.0033(8) C21 0.0198(10) 0.0190(10) 0.0190(10) -0.0041(8) 0.0002(8) -0.0009(8) C25 0.0247(11) 0.0208(11) 0.0263(11) 0.0029(9) 0.0046(9) 0.0019(9) C6 0.0189(10) 0.0250(11) 0.0159(9) 0.0005(8) -0.0052(8) -0.0048(8) C27 0.0242(11) 0.0233(11) 0.0232(11) 0.0005(9) -0.0011(9) 0.0014(9) C9 0.0310(12) 0.0204(11) 0.0267(11) 0.0044(9) -0.0041(9) -0.0042(9) F5 0.0629(14) 0.0675(15) 0.153(3) -0.0016(15) 0.0017(15) 0.0173(12) C17 0.0287(12) 0.0231(11) 0.0220(11) 0.0017(9) 0.0076(9) 0.0065(9) F6A 0.029(3) 0.050(3) 0.064(5) -0.005(2) 0.011(2) -0.010(2) C22 0.0202(11) 0.0276(11) 0.0216(10) -0.0037(9) 0.0005(8) -0.0006(9) C28 0.0512(17) 0.0306(13) 0.0332(13) 0.0139(11) -0.0003(12) -0.0030(12) C18 0.0266(12) 0.0305(12) 0.0302(12) 0.0085(10) 0.0089(9) 0.0035(10) C24 0.0275(12) 0.0334(12) 0.0195(11) -0.0084(9) -0.0015(9) -0.0015(10) C26 0.0357(15) 0.0295(14) 0.068(2) 0.0173(13) 0.0110(13) 0.0151(12) C20 0.0415(14) 0.0302(12) 0.0202(11) -0.0008(9) 0.0058(10) 0.0029(11) C19 0.0380(14) 0.0254(12) 0.0352(13) 0.0009(10) 0.0119(11) 0.0113(10) C23 0.0276(12) 0.0172(10) 0.0368(13) -0.0047(9) 0.0011(10) 0.0000(9) N6 0.0452(15) 0.0694(18) 0.0514(16) 0.0099(14) -0.0121(12) -0.0219(13) F8A 0.064(2) 0.070(2) 0.058(2) -0.0032(18) -0.0085(17) -0.0393(19) C29 0.0355(15) 0.0567(18) 0.0409(16) -0.0018(14) -0.0017(12) -0.0106(13) F7A 0.135(4) 0.061(2) 0.0335(16) -0.0113(14) -0.0013(18) -0.034(2) B1 0.0399(16) 0.0181(12) 0.0302(14) 0.0015(10) 0.0025(11) 0.0009(11) C30 0.074(2) 0.074(2) 0.0350(16) 0.0022(15) -0.0039(15) -0.0028(19) B2 0.0338(16) 0.057(2) 0.0364(16) -0.0097(14) 0.0035(13) -0.0049(15) F8B 0.051(3) 0.085(5) 0.126(8) 0.050(5) 0.027(4) -0.008(3) F7B 0.049(4) 0.118(7) 0.057(4) -0.034(4) -0.012(3) -0.013(4) F6B 0.143(10) 0.083(6) 0.047(3) -0.007(3) 0.009(5) 0.058(7) 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0110 0.00 0.00 -1.00 0.0090 0.00 -1.00 0.00 0.0530 -1.00 0.00 0.00 0.0530 -1.00 1.00 0.00 0.0230 1.00 0.00 0.00 0.0230 0.00 1.00 0.00 0.0440 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 N2 Pd1 N1 82.65(7) . . ? N4 Pd1 N2 94.10(7) . . ? F6Aa B2 F5 109.5(4) . . ? F8Bb B2 F5 96.7(4) . . ? F6Bb B2 F5 107.5(4) . . ? F6Aa B2 F8A 107.2(5) . . ? F7Aa B2 F8A 105.5(3) . . ? F6Aa B2 F7A 101.5(6) . . ? F6Bb B2 F7B 102.3(14) . . ? F8Bb B2 F7B 113.8(6) . . ? F8Bb B2 F6B 136.0(13) . . ? N4 Pd1 N1 173.00(7) . . ? N4 Pd1 N5 82.81(7) . . ? N5 Pd1 N2 176.58(7) . . ? N5 Pd1 N1 100.26(7) . . ? C15 N2 Pd1 128.55(13) . . ? C11 N2 Pd1 111.25(13) . . ? C11 N2 C15 120.20(17) . . ? C3 N1 Pd1 110.09(12) . . ? C3 N1 C17 108.07(16) . . ? C10 N1 Pd1 102.25(12) . . ? C10 N1 C3 111.46(15) . . ? C10 N1 C17 108.38(16) . . ? C17 N1 Pd1 116.51(12) . . ? C16 N3 C8 110.23(15) . . ? C16 N3 C21 113.57(15) . . ? C8 N3 C21 113.36(15) . . ? C25 N4 Pd1 166.26(17) . . ? C27 N5 Pd1 165.17(18) . . ? C1 C2 C3 119.80(18) . . ? C1 C2 C4 119.26(19) . . ? C4 C2 C3 120.82(19) . . ? N2 C15 C14 119.04(18) . . ? N2 C15 C16 120.35(17) . . ? C14 C15 C16 120.46(18) . . ? C15 C14 H14 119.7 . . ? C15 C14 C13 120.55(19) . . ? C13 C14 H14 119.7 . . ? C2 C1 H1 119.6 . . ? C7 C1 C2 120.72(19) . . ? C7 C1 H1 119.6 . . ? N1 C3 H3A 108.5 . . ? N1 C3 H3B 108.5 . . ? C2 C3 N1 114.92(16) . . ? C2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C1 C7 C8 120.47(18) . . ? C1 C7 C6 118.72(19) . . ? C6 C7 C8 120.57(19) . . ? C14 C13 H13 120.3 . . ? C12 C13 C14 119.30(19) . . ? C12 C13 H13 120.3 . . ? C4 C5 C9 120.3(2) . . ? C6 C5 C4 118.30(19) . . ? C6 C5 C9 121.34(19) . . ? C2 C4 H4 119.5 . . ? C5 C4 C2 121.0(2) . . ? C5 C4 H4 119.5 . . ? N1 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C11 C10 N1 112.71(16) . . ? C11 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? C13 C12 H12 120.9 . . ? C13 C12 C11 118.19(19) . . ? C11 C12 H12 120.9 . . ? N3 C16 C15 110.22(15) . . ? N3 C16 H16A 109.6 . . ? N3 C16 H16B 109.6 . . ? C15 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N2 C11 C10 115.99(17) . . ? N2 C11 C12 121.62(19) . . ? C12 C11 C10 122.35(18) . . ? N3 C8 C7 110.66(16) . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N3 C21 C22 108.36(16) . . ? N3 C21 C24 108.82(17) . . ? N3 C21 C23 112.77(17) . . ? C22 C21 C24 106.91(17) . . ? C22 C21 C23 110.08(18) . . ? C24 C21 C23 109.72(18) . . ? N4 C25 C26 179.1(3) . . ? C7 C6 H6 119.1 . . ? C5 C6 C7 121.72(19) . . ? C5 C6 H6 119.1 . . ? N5 C27 C28 179.3(3) . . ? 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 . . ? C18 C17 N1 110.39(18) . . ? C18 C17 C20 111.21(19) . . ? C18 C17 C19 108.16(19) . . ? C20 C17 N1 109.13(18) . . ? C20 C17 C19 108.0(2) . . ? C19 C17 N1 109.95(17) . . ? 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 . . ? 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 . . ? 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 . . ? 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 . . ? 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 . . ? 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 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C29 C30 178.1(4) . . ? F4 B1 F1 109.2(2) . . ? F3 B1 F1 108.7(2) . . ? F3 B1 F4 108.5(2) . . ? F2 B1 F1 109.9(2) . . ? F2 B1 F4 110.0(2) . . ? F2 B1 F3 110.5(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 . . ? F5 B2 F8A 110.4(3) . . ? F5 B2 F7A 121.7(3) . . ? F5 B2 F7B 90.8(4) . . ? 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 N2 2.0143(16) . ? Pd1 N1 2.0759(17) . ? Pd1 N4 2.0115(18) . ? Pd1 N5 2.0129(18) . ? F7Aa B2 1.400(4) . ? F6Aa B2 1.378(7) . ? F8Aa B2 1.438(4) . ? F1 B1 1.405(3) . ? F4 B1 1.386(3) . ? F3 B1 1.385(3) . ? N2 C15 1.355(3) . ? N2 C11 1.352(3) . ? N1 C3 1.531(3) . ? N1 C10 1.510(3) . ? N1 C17 1.569(3) . ? N3 C16 1.479(2) . ? N3 C8 1.485(3) . ? N3 C21 1.500(3) . ? F2 B1 1.379(3) . ? N4 C25 1.128(3) . ? N5 C27 1.135(3) . ? C2 C1 1.390(3) . ? C2 C3 1.507(3) . ? C2 C4 1.395(3) . ? C15 C14 1.384(3) . ? C15 C16 1.525(3) . ? C14 H14 0.9500 . ? C14 C13 1.385(3) . ? C1 H1 0.9500 . ? C1 C7 1.388(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C7 C8 1.510(3) . ? C7 C6 1.394(3) . ? C13 H13 0.9500 . ? C13 C12 1.383(3) . ? C5 C4 1.391(3) . ? C5 C6 1.391(3) . ? C5 C9 1.511(3) . ? C4 H4 0.9500 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.495(3) . ? C12 H12 0.9500 . ? C12 C11 1.383(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C21 C22 1.528(3) . ? C21 C24 1.537(3) . ? C21 C23 1.539(3) . ? C25 C26 1.452(3) . ? C6 H6 0.9500 . ? C27 C28 1.455(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? F5 B2 1.393(4) . ? C17 C18 1.527(3) . ? C17 C20 1.533(3) . ? C17 C19 1.538(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N6 C29 1.131(4) . ? C29 C30 1.446(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? B2 F8B 1.262(6) . ? B2 F7B 1.422(6) . ? B2 F6B 1.315(7) . ? 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 N2 C15 C14 168.22(14) . . . . ? Pd1 N2 C15 C16 -16.3(3) . . . . ? Pd1 N2 C11 C10 13.9(2) . . . . ? Pd1 N2 C11 C12 -168.46(15) . . . . ? Pd1 N1 C3 C2 63.34(19) . . . . ? Pd1 N1 C10 C11 -35.60(18) . . . . ? Pd1 N1 C17 C18 78.02(19) . . . . ? Pd1 N1 C17 C20 -44.5(2) . . . . ? Pd1 N1 C17 C19 -162.73(16) . . . . ? N2 C15 C14 C13 3.0(3) . . . . ? N2 C15 C16 N3 -132.21(18) . . . . ? N1 C10 C11 N2 16.3(2) . . . . ? N1 C10 C11 C12 -161.36(18) . . . . ? C2 C1 C7 C8 -169.59(18) . . . . ? C2 C1 C7 C6 4.8(3) . . . . ? C15 N2 C11 C10 -166.84(17) . . . . ? C15 N2 C11 C12 10.8(3) . . . . ? C15 C14 C13 C12 5.2(3) . . . . ? C14 C15 C16 N3 43.2(2) . . . . ? C14 C13 C12 C11 -5.4(3) . . . . ? C1 C2 C3 N1 -83.9(2) . . . . ? C1 C2 C4 C5 2.7(3) . . . . ? C1 C7 C8 N3 95.5(2) . . . . ? C1 C7 C6 C5 -0.9(3) . . . . ? C3 N1 C10 C11 82.0(2) . . . . ? C3 N1 C17 C18 -46.5(2) . . . . ? C3 N1 C17 C20 -169.01(17) . . . . ? C3 N1 C17 C19 72.8(2) . . . . ? C3 C2 C1 C7 170.39(18) . . . . ? C3 C2 C4 C5 -173.34(18) . . . . ? C13 C12 C11 N2 -2.4(3) . . . . ? C13 C12 C11 C10 175.09(19) . . . . ? C4 C2 C1 C7 -5.7(3) . . . . ? C4 C2 C3 N1 92.1(2) . . . . ? C4 C5 C6 C7 -2.0(3) . . . . ? C10 N1 C3 C2 -49.4(2) . . . . ? C10 N1 C17 C18 -167.41(17) . . . . ? C10 N1 C17 C20 70.1(2) . . . . ? C10 N1 C17 C19 -48.2(2) . . . . ? C16 N3 C8 C7 -60.0(2) . . . . ? C16 N3 C21 C22 63.2(2) . . . . ? C16 N3 C21 C24 179.14(16) . . . . ? C16 N3 C21 C23 -58.9(2) . . . . ? C16 C15 C14 C13 -172.49(18) . . . . ? C11 N2 C15 C14 -11.0(3) . . . . ? C11 N2 C15 C16 164.55(17) . . . . ? C8 N3 C16 C15 91.05(19) . . . . ? C8 N3 C21 C22 -169.93(16) . . . . ? C8 N3 C21 C24 -54.0(2) . . . . ? C8 N3 C21 C23 68.0(2) . . . . ? C8 C7 C6 C5 173.46(18) . . . . ? C21 N3 C16 C15 -140.50(16) . . . . ? C21 N3 C8 C7 171.45(16) . . . . ? C6 C7 C8 N3 -78.8(2) . . . . ? C6 C5 C4 C2 1.1(3) . . . . ? C9 C5 C4 C2 177.84(19) . . . . ? C9 C5 C6 C7 -178.70(19) . . . . ? C17 N1 C3 C2 -168.39(17) . . . . ? C17 N1 C10 C11 -159.21(17) . . . . ?