#------------------------------------------------------------------------------ #$Date: 2019-11-24 22:36:01 +0200 (Sun, 24 Nov 2019) $ #$Revision: 239622 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/68/4516899.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_4516899 loop_ _publ_author_name 'Kumar, Anuj' 'Naaz, Afsana' 'Prakasham, A. P.' 'Gangwar, Manoj Kumar' 'Butcher, Raymond J.' 'Panda, Dulal' 'Ghosh, Prasenjit' _publ_section_title ; Potent Anticancer Activity with High Selectivity of a Chiral Palladium N-Heterocyclic Carbene Complex. ; _journal_issue 8 _journal_name_full 'ACS omega' _journal_page_first 4632 _journal_page_last 4646 _journal_paper_doi 10.1021/acsomega.7b00688 _journal_volume 2 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C32 H50 F6 N6 O4 Pd' _chemical_formula_sum 'C32 H50 F6 N6 O4 Pd' _chemical_formula_weight 803.18 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-07-09 _audit_creation_method ; Olex2 1.2-alpha (compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128) ; _cell_angle_alpha 90 _cell_angle_beta 92.303(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.561(2) _cell_length_b 11.169(2) _cell_length_c 16.133(3) _cell_measurement_reflns_used 6953 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.20 _cell_measurement_theta_min 4.80 _cell_volume 1901.4(6) _computing_cell_refinement 'Rigaku CrystalClear' _computing_data_collection 'Rigaku CrystalClear' _computing_data_reduction 'Rigaku CrystalClear' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'Rigaku SHELXTL (Sheldrick, 2008)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Rigaku CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0680 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26732 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.241 _diffrn_reflns_theta_max 29.203 _diffrn_reflns_theta_min 4.802 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_T_max 0.9462 _exptl_absorpt_correction_T_min 0.9109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details CrystalClear _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.999 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.078 _refine_ls_abs_structure_details ; Flack x determined using 3574 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.035(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 450 _refine_ls_number_reflns 10091 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0397 _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^)+(0.0331P)^2^+0.1791P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.0829 _reflns_Friedel_coverage 0.898 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.978 _reflns_number_gt 9292 _reflns_number_total 10091 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao7b00688_si_002.cif _cod_data_source_block 1S2S5R-1c_PG-AK-9-97 _cod_database_code 4516899 _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 0.946 _shelx_estimated_absorpt_t_min 0.911 _exptl_absorpt_special_details ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _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 Ternary CH refined with riding coordinates: C5(H5), C7(H7), C11(H11), C12(H12), C19(H19), C21(H21), C25(H25), C26(H26) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C16(H16) 2.d Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C28(H28A,H28B, H28C) ; _shelx_res_file ; pg_97.res created by SHELXL-2014/7 TITL PG-AK-9-97 CELL 0.7107 10.561 11.169 16.133 90 92.303 90 ZERR 2 0.002 0.002 0.003 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H F N O Pd UNIT 64 100 12 12 8 2 L.S. 20 PLAN -25 SIZE 0.1 0.16 0.17 TEMP -173 HTAB BOND $H LIST 4 MORE -1 CONF fmap 2 acta SHEL 99999 0 OMIT -1 6 11 OMIT 9 1 0 OMIT 9 1 1 OMIT -7 2 9 OMIT 3 -7 -8 OMIT -3 -7 8 OMIT -2 4 1 OMIT -1 0 8 OMIT -2 -4 1 OMIT -2 0 7 OMIT -2 0 4 OMIT -4 0 1 OMIT 0 -3 1 OMIT -4 -2 5 OMIT 0 3 1 OMIT -4 2 5 OMIT -1 0 7 OMIT -1 -4 5 OMIT -5 0 5 OMIT 0 -5 6 OMIT 1 -2 3 OMIT -3 3 11 OMIT 0 -5 7 OMIT -9 -10 6 OMIT 4 -8 6 OMIT -5 -7 6 REM REM REM WGHT 0.033100 0.179100 FVAR 1.03563 PD1 6 -0.976887 -0.611840 -0.257082 11.00000 0.01612 0.01284 = 0.01277 -0.00039 -0.00175 0.00029 F1 3 -1.385670 -0.713986 -0.176497 11.00000 0.02410 0.04752 = 0.12496 0.02777 -0.00797 -0.00740 F2 3 -1.315246 -0.812964 -0.072575 11.00000 0.04813 0.19257 = 0.04442 0.04423 0.00690 -0.04152 F3 3 -1.301287 -0.879645 -0.192318 11.00000 0.07027 0.05320 = 0.13433 -0.04359 0.04170 -0.03662 F4 3 -0.653975 -0.346698 -0.276163 11.00000 0.04946 0.04294 = 0.02921 -0.00893 0.00203 -0.02650 F5 3 -0.661098 -0.330033 -0.407598 11.00000 0.04889 0.05145 = 0.03283 0.01894 -0.00197 -0.02017 F6 3 -0.570228 -0.481966 -0.350265 11.00000 0.02012 0.03742 = 0.09178 -0.00473 0.00252 0.00199 O1 5 -1.146623 -0.681680 -0.227704 11.00000 0.01617 0.01907 = 0.01748 0.00272 -0.00163 -0.00583 O2 5 -0.867875 -0.464589 -0.410079 11.00000 0.03110 0.05659 = 0.02281 0.01435 -0.01141 -0.00971 O3 5 -1.088395 -0.723769 -0.095228 11.00000 0.03327 0.05764 = 0.02236 0.01624 -0.00863 -0.00998 O4 5 -0.807409 -0.540105 -0.285247 11.00000 0.01761 0.02014 = 0.01679 0.00327 -0.00108 -0.00139 N1 4 -0.909739 -0.435030 -0.118828 11.00000 0.01677 0.01969 = 0.01299 -0.00163 -0.00442 0.00002 N2 4 -1.067645 -0.307607 -0.112358 11.00000 0.02486 0.01861 = 0.01732 -0.00690 -0.00178 0.00023 N3 4 -1.090114 -0.394157 -0.172682 11.00000 0.01682 0.01538 = 0.01464 -0.00432 -0.00560 -0.00196 N4 4 -1.040644 -0.798654 -0.392066 11.00000 0.01951 0.01615 = 0.01485 -0.00058 -0.00579 -0.00080 N5 4 -0.876366 -0.920824 -0.393309 11.00000 0.02746 0.02176 = 0.02108 -0.00665 -0.00566 0.00424 N6 4 -0.857752 -0.830139 -0.336404 11.00000 0.02170 0.01619 = 0.01606 -0.00187 -0.00352 0.00134 C1 1 -0.996107 -0.472649 -0.178166 11.00000 0.01894 0.01575 = 0.01116 0.00007 -0.00001 -0.00225 C2 1 -0.957386 -0.335898 -0.080807 11.00000 0.02055 0.02160 = 0.01532 -0.00166 -0.00211 -0.00202 AFIX 43 H2 2 -0.914775 -0.293504 -0.036916 11.00000 -1.20000 AFIX 0 C3 1 -0.790243 -0.494263 -0.092796 11.00000 0.01504 0.02609 = 0.01916 0.00144 -0.00469 0.00096 AFIX 23 H3A 2 -0.727184 -0.432788 -0.075231 11.00000 -1.20000 H3B 2 -0.756712 -0.538013 -0.140568 11.00000 -1.20000 AFIX 0 C4 1 -0.807742 -0.580842 -0.022198 11.00000 0.03211 0.03658 = 0.03502 0.01333 -0.00951 0.00298 AFIX 137 H4A 2 -0.871754 -0.640624 -0.038848 11.00000 -1.50000 H4B 2 -0.835663 -0.537003 0.026416 11.00000 -1.50000 H4C 2 -0.727159 -0.621048 -0.008378 11.00000 -1.50000 AFIX 0 C5 1 -1.209766 -0.394618 -0.223212 11.00000 0.01911 0.01598 = 0.01887 -0.00375 -0.00209 0.00110 AFIX 13 H5 2 -1.208113 -0.467322 -0.259327 11.00000 -1.20000 AFIX 0 C6 1 -1.322954 -0.409052 -0.167151 11.00000 0.02631 0.02185 = 0.02758 0.00188 0.00050 -0.00736 AFIX 23 H6A 2 -1.302471 -0.471808 -0.125398 11.00000 -1.20000 H6B 2 -1.397060 -0.436967 -0.201390 11.00000 -1.20000 AFIX 0 C7 1 -1.359520 -0.293931 -0.121827 11.00000 0.02022 0.03484 = 0.02538 -0.00628 0.00278 -0.00413 AFIX 13 H7 2 -1.289302 -0.273730 -0.080775 11.00000 -1.20000 AFIX 0 C8 1 -1.480631 -0.312075 -0.074273 11.00000 0.02940 0.05396 = 0.04560 -0.00859 0.00956 -0.00153 AFIX 137 H8A 2 -1.551523 -0.329072 -0.113572 11.00000 -1.50000 H8B 2 -1.498831 -0.239288 -0.042988 11.00000 -1.50000 H8C 2 -1.469054 -0.379480 -0.035824 11.00000 -1.50000 AFIX 0 C9 1 -1.374557 -0.189946 -0.182760 11.00000 0.02655 0.02923 = 0.03169 -0.00884 -0.00054 0.00793 AFIX 23 H9A 2 -1.448879 -0.205184 -0.220647 11.00000 -1.20000 H9B 2 -1.391160 -0.115644 -0.151548 11.00000 -1.20000 AFIX 0 C10 1 -1.258156 -0.171615 -0.233873 11.00000 0.02694 0.01837 = 0.02456 -0.00078 -0.00435 0.00541 AFIX 23 H10A 2 -1.185086 -0.148954 -0.196805 11.00000 -1.20000 H10B 2 -1.274021 -0.105542 -0.273858 11.00000 -1.20000 AFIX 0 C11 1 -1.226705 -0.286411 -0.281034 11.00000 0.01968 0.01815 = 0.01911 -0.00143 -0.00464 0.00211 AFIX 13 H11 2 -1.304802 -0.304433 -0.315906 11.00000 -1.20000 AFIX 0 C12 1 -1.120497 -0.273838 -0.343274 11.00000 0.02829 0.02274 = 0.02181 -0.00363 0.00013 0.00157 AFIX 13 H12 2 -1.093017 -0.356548 -0.358050 11.00000 -1.20000 AFIX 0 C13 1 -1.003139 -0.206804 -0.310410 11.00000 0.02699 0.04103 = 0.02878 0.00234 0.00080 -0.00680 AFIX 137 H13A 2 -1.025163 -0.123078 -0.299921 11.00000 -1.50000 H13B 2 -0.937430 -0.210204 -0.351543 11.00000 -1.50000 H13C 2 -0.971397 -0.244049 -0.258643 11.00000 -1.50000 AFIX 0 C14 1 -1.171260 -0.213860 -0.423542 11.00000 0.03294 0.05122 = 0.02479 0.00353 -0.00200 -0.00058 AFIX 137 H14A 2 -1.239773 -0.262594 -0.448655 11.00000 -1.50000 H14B 2 -1.102688 -0.206673 -0.462402 11.00000 -1.50000 H14C 2 -1.203720 -0.134030 -0.410805 11.00000 -1.50000 AFIX 0 C15 1 -0.955477 -0.753561 -0.334013 11.00000 0.02018 0.01590 = 0.01312 0.00120 -0.00196 -0.00245 C16 1 -0.988533 -0.897577 -0.425707 11.00000 0.02910 0.01734 = 0.02082 -0.00769 -0.00440 0.00202 AFIX 43 H16 2 -1.029263 -0.944479 -0.468051 11.00000 -1.20000 AFIX 0 C17 1 -1.168620 -0.752891 -0.413281 11.00000 0.01728 0.02544 = 0.01977 0.00162 -0.00446 -0.00165 AFIX 23 H17A 2 -1.217063 -0.747599 -0.362132 11.00000 -1.20000 H17B 2 -1.213016 -0.810098 -0.451243 11.00000 -1.20000 AFIX 0 C18 1 -1.166234 -0.630912 -0.454127 11.00000 0.02894 0.02441 = 0.03353 0.00209 -0.00772 0.00421 AFIX 137 H18A 2 -1.126369 -0.637367 -0.507760 11.00000 -1.50000 H18B 2 -1.117668 -0.575126 -0.418364 11.00000 -1.50000 H18C 2 -1.253121 -0.601288 -0.462696 11.00000 -1.50000 AFIX 0 C19 1 -0.740905 -0.824343 -0.281253 11.00000 0.02071 0.01949 = 0.02169 -0.00116 -0.00895 -0.00004 AFIX 13 H19 2 -0.705159 -0.741845 -0.286099 11.00000 -1.20000 AFIX 0 C20 1 -0.776277 -0.841885 -0.190572 11.00000 0.02471 0.02088 = 0.02178 -0.00423 -0.00761 0.00979 AFIX 23 H20A 2 -0.702341 -0.820839 -0.153777 11.00000 -1.20000 H20B 2 -0.846025 -0.786310 -0.178123 11.00000 -1.20000 AFIX 0 C21 1 -0.817335 -0.969268 -0.171433 11.00000 0.02932 0.02556 = 0.02108 -0.00021 -0.00228 0.00660 AFIX 13 H21 2 -0.894450 -0.988442 -0.206953 11.00000 -1.20000 AFIX 0 C22 1 -0.851213 -0.979946 -0.080782 11.00000 0.05097 0.03685 = 0.02803 0.00577 0.00932 0.00831 AFIX 137 H22A 2 -0.776474 -0.961635 -0.045061 11.00000 -1.50000 H22B 2 -0.879715 -1.061692 -0.069718 11.00000 -1.50000 H22C 2 -0.919234 -0.923376 -0.069282 11.00000 -1.50000 AFIX 0 C23 1 -0.711650 -1.056580 -0.193229 11.00000 0.03642 0.02204 = 0.02844 0.00223 0.00223 0.00564 AFIX 23 H23A 2 -0.740825 -1.139647 -0.184285 11.00000 -1.20000 H23B 2 -0.636703 -1.042332 -0.155688 11.00000 -1.20000 AFIX 0 C24 1 -0.673283 -1.042654 -0.283435 11.00000 0.02800 0.01883 = 0.02720 -0.00153 -0.00185 0.00597 AFIX 23 H24A 2 -0.744770 -1.068086 -0.320943 11.00000 -1.20000 H24B 2 -0.600622 -1.096099 -0.293261 11.00000 -1.20000 AFIX 0 C25 1 -0.636542 -0.913305 -0.304618 11.00000 0.01766 0.02322 = 0.02284 0.00172 -0.00309 0.00383 AFIX 13 H25 2 -0.562436 -0.894228 -0.266363 11.00000 -1.20000 AFIX 0 C26 1 -0.587170 -0.898989 -0.392623 11.00000 0.02748 0.02657 = 0.02171 0.00088 -0.00240 0.00278 AFIX 13 H26 2 -0.654538 -0.926793 -0.433508 11.00000 -1.20000 AFIX 0 C27 1 -0.468240 -0.975021 -0.403449 11.00000 0.03642 0.03916 = 0.03844 0.00092 0.01210 0.00983 AFIX 137 H27A 2 -0.403677 -0.953337 -0.360748 11.00000 -1.50000 H27B 2 -0.435309 -0.960401 -0.458471 11.00000 -1.50000 H27C 2 -0.489654 -1.059965 -0.398053 11.00000 -1.50000 AFIX 0 C28 1 -0.555220 -0.768667 -0.412026 11.00000 0.03755 0.03718 = 0.02586 0.00493 0.00253 -0.00004 AFIX 137 H28A 2 -0.633095 -0.720862 -0.413977 11.00000 -1.50000 H28B 2 -0.515526 -0.764395 -0.465819 11.00000 -1.50000 H28C 2 -0.496566 -0.737235 -0.368715 11.00000 -1.50000 AFIX 0 C29 1 -0.796322 -0.477998 -0.350080 11.00000 0.01910 0.01979 = 0.01608 -0.00138 0.00153 0.00150 C30 1 -0.668735 -0.409038 -0.346680 11.00000 0.02570 0.02549 = 0.01875 0.00188 0.00306 -0.00438 C31 1 -1.160652 -0.722891 -0.155469 11.00000 0.02285 0.01829 = 0.01773 0.00032 -0.00064 -0.00040 C32 1 -1.293774 -0.780221 -0.147424 11.00000 0.03408 0.02688 = 0.02513 0.00588 0.00492 -0.00150 HKLF 4 REM PG-AK-9-97 REM R1 = 0.0397 for 9292 Fo > 4sig(Fo) and 0.0443 for all 10091 data REM 450 parameters refined using 1 restraints END WGHT 0.0331 0.1791 REM Instructions for potential hydrogen bonds EQIV $1 -x-2, y+1/2, -z HTAB C2 O3_$1 HTAB C3 O4 HTAB C4 O3 HTAB C5 O1 EQIV $2 -x-2, y-1/2, -z-1 HTAB C16 O2_$2 HTAB C17 O1 HTAB C17 F5_$2 HTAB C19 O4 REM Highest difference peak 0.999, deepest hole -0.790, 1-sigma level 0.078 Q1 1 -1.0778 -0.6070 -0.2254 11.00000 0.05 1.00 Q2 1 -1.3519 -0.7160 -0.0934 11.00000 0.05 0.46 Q3 1 -0.9468 -0.6105 -0.2509 11.00000 0.05 0.45 Q4 1 -0.8004 -0.6134 -0.2999 11.00000 0.05 0.43 Q5 1 -0.9963 -0.6142 -0.1815 11.00000 0.05 0.42 Q6 1 -1.2227 -0.7538 -0.1524 11.00000 0.05 0.40 Q7 1 -0.9717 -0.7063 -0.2747 11.00000 0.05 0.38 Q8 1 -0.9325 -0.5215 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104.35 -4 -6 9 2060.19 159.25 -4 -6 9 2425.87 136.09 4 6 -9 2205.41 147.79 4 6 -9 2145.08 207.42 -9 0 1 2456.34 139.86 -9 0 1 2274.92 164.31 -9 0 1 2624.83 153.35 9 0 -1 2750.15 159.66 -9 0 0 329.78 114.95 9 0 0 416.77 52.60 -9 0 0 419.67 60.13 -9 0 0 491.86 120.01 -4 1 -12 427.16 49.99 -4 1 -12 462.14 102.05 4 1 12 363.49 35.28 -4 -1 -12 479.60 52.50 -4 -1 -12 486.80 84.12 4 -1 12 424.03 45.30 -4 -1 -12 498.95 73.67 7 -6 0 768.34 104.84 -7 -6 0 721.98 71.34 -7 -6 0 625.92 79.76 -7 6 0 711.29 66.90 7 6 0 798.18 68.46 7 6 0 638.51 57.31 7 6 -1 998.49 89.68 -7 6 1 1046.42 92.85 7 6 -1 1088.60 86.46 7 -6 -1 1084.51 83.56 7 -6 -1 1069.96 105.08 -7 -6 1 1168.04 112.83 -7 -6 1 1037.84 86.15 2 4 12 2012.77 100.36 -2 4 -12 2211.11 137.04 -2 4 -12 2106.98 120.48 -2 4 -12 2111.75 117.47 2 -4 12 2227.24 129.14 -2 -4 -12 2014.68 195.23 -2 -4 -12 2316.77 125.92 2 -4 12 2070.59 116.88 -7 1 9 369.64 150.38 -3 9 0 53.80 45.46 3 9 0 22.71 43.93 -3 -9 0 45.37 28.22 3 -9 0 46.83 18.95 -3 -9 0 33.16 8.53 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56.52 -7 -6 2 440.33 107.75 7 -6 -2 322.96 41.78 -7 -6 2 213.13 65.43 7 -6 -2 340.56 87.06 -5 -8 0 2825.35 149.71 -5 -8 0 2236.02 130.10 -5 8 0 2721.72 150.53 5 8 0 2934.36 163.89 1 -3 13 206.15 67.72 -1 -3 -13 117.20 45.17 1 -3 13 192.45 55.61 -1 3 -13 40.17 35.24 -1 3 -13 65.20 33.93 1 3 13 41.39 13.64 -1 3 -13 22.45 28.70 -6 4 9 112.20 63.74 6 4 -9 190.72 44.83 6 4 -9 195.93 61.63 -6 -4 9 135.15 30.21 -6 -4 9 97.19 37.61 -4 7 -7 1952.04 118.64 -4 7 -7 1880.87 110.19 4 7 7 1890.18 108.25 4 -7 7 1887.03 116.92 -4 -7 -7 1715.97 147.07 -5 -8 1 1449.23 124.37 -5 -8 1 1447.23 125.15 5 8 -1 1327.03 153.00 5 8 -1 1257.84 104.81 -5 8 1 1360.82 102.28 -3 -6 10 970.46 79.97 -3 -6 10 987.64 81.59 3 6 -10 1156.09 119.90 3 6 -10 1066.19 91.96 5 6 -8 528.29 56.73 5 6 -8 600.44 73.47 -5 -6 8 651.60 67.78 -5 -6 8 568.61 60.80 -3 8 -6 2649.39 148.75 3 8 6 2545.25 137.39 -3 -8 -6 2454.87 157.08 5 -7 -6 306.37 9.20 -5 -7 6 344.35 61.16 -5 -7 6 331.11 42.97 -5 7 6 316.44 15.75 5 7 -6 490.15 103.53 6 7 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515.78 116.52 -5 -8 2 1008.61 132.29 -5 -8 2 848.00 82.59 5 8 -2 958.68 79.91 -5 8 2 940.40 78.77 5 8 -2 1064.70 89.35 -3 -9 -2 450.91 49.43 -3 -9 -2 349.14 45.42 3 9 2 398.63 40.54 -3 9 -2 470.22 71.59 -2 -7 -9 395.66 44.38 -2 7 -9 385.95 72.29 -2 7 -9 435.41 43.80 2 7 9 440.12 70.15 -8 4 -3 502.22 53.65 8 4 3 512.00 126.15 -8 -4 -3 465.34 94.82 -8 -4 -3 395.78 56.70 9 0 -3 3024.47 172.07 -9 0 3 2684.76 159.77 9 0 -3 2626.27 152.38 -9 0 3 2719.97 184.27 -8 4 4 295.31 45.62 -8 4 4 310.97 36.17 8 4 -4 272.22 29.17 8 4 -4 226.37 89.45 8 -4 -4 262.31 23.79 -8 -4 4 324.92 62.37 -8 -4 4 286.15 115.72 8 -4 -4 242.50 31.67 3 0 13 232.08 42.37 -3 0 -13 262.64 73.53 -3 0 -13 276.27 89.64 5 0 -12 8.35 14.59 -5 0 12 1.63 18.30 -5 0 12 -2.52 22.22 5 0 -12 12.13 7.81 5 0 -12 19.00 16.76 -2 9 -4 0.13 3.47 2 9 4 161.26 44.65 -2 9 -4 148.16 31.59 -2 -9 -4 98.48 26.67 -2 -9 -4 183.16 45.82 7 6 2 633.84 41.79 -7 6 -2 678.31 74.39 -7 -6 -2 720.04 82.05 -7 -6 -2 736.57 75.11 7 -6 2 742.21 78.76 -9 0 -2 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64.77 4 8 -11 958.86 94.66 4 8 -11 875.92 121.70 -4 -8 11 762.92 167.50 -4 -8 11 823.68 76.02 9 2 -10 80.59 43.70 -9 2 10 129.33 50.62 9 2 -10 100.11 39.45 -9 -2 10 87.37 28.85 9 -2 -10 71.31 34.50 -9 -2 10 65.74 26.13 -11 -1 -1 12.22 26.47 -11 -1 -1 9.96 37.68 -11 1 -1 11.30 13.28 -11 1 -1 8.36 19.32 3 6 -14 204.26 49.05 -3 6 14 142.23 44.51 3 6 -14 266.62 117.10 -3 -6 14 284.02 78.45 -3 -6 14 153.83 96.23 10 -5 -2 725.99 56.54 -10 -5 2 740.10 69.73 -10 -5 2 611.62 58.07 -10 5 2 771.20 38.37 10 5 -2 889.00 74.82 10 5 -2 786.25 107.77 -6 8 -8 1063.81 89.28 6 8 8 986.69 84.55 6 -8 8 1113.40 138.84 -6 -8 -8 1161.60 140.36 3 7 -13 433.97 48.03 3 7 -13 479.44 53.77 -3 -7 13 425.33 39.29 -3 -7 13 344.12 129.41 7 -7 8 46.19 29.79 -7 -7 -8 28.16 22.71 7 7 8 43.25 22.74 -7 7 -8 23.23 18.94 -11 0 3 253.29 104.56 -11 0 3 201.83 61.48 11 0 -3 246.31 75.71 -11 0 3 295.84 29.57 5 -5 13 2090.10 142.94 -5 -5 -13 1857.74 153.62 -5 -5 -13 1957.37 151.17 -5 5 -13 2002.27 241.06 -5 5 -13 2180.83 151.73 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2 -8 131.30 60.54 -2 11 6 212.19 60.61 2 11 -6 213.43 53.57 -2 -11 6 413.53 82.91 -2 -11 6 244.49 74.39 -6 4 -13 46.66 12.84 -6 4 -13 33.55 37.85 -6 -4 -13 45.21 26.29 -6 -4 -13 36.81 20.95 6 -4 13 23.62 24.11 -5 -9 -8 356.00 94.63 5 9 8 305.82 81.61 -5 9 -8 291.76 111.06 -8 6 -8 843.37 138.04 8 6 8 824.80 85.98 -8 -6 -8 915.05 100.09 8 -6 8 1021.44 161.96 3 11 -5 869.89 80.79 -3 11 5 728.74 39.22 -3 -11 5 1089.61 133.65 -3 -11 5 981.23 96.68 2 1 -17 783.85 103.18 -2 1 17 749.25 49.01 2 1 -17 762.81 133.13 2 1 -17 803.39 172.17 -2 -1 17 601.12 61.91 2 -1 -17 540.32 80.17 2 -1 -17 598.56 50.22 -3 -10 -8 1122.50 87.10 -3 10 -8 1193.96 120.24 3 10 8 1127.06 87.75 9 -5 -8 608.05 61.05 -9 -5 8 613.69 81.37 -9 -5 8 740.38 86.40 9 5 -8 850.05 202.79 -9 5 8 704.15 65.35 9 5 -8 743.92 66.20 -5 4 -14 542.95 97.63 -5 4 -14 628.99 41.45 -5 -4 -14 627.50 85.56 5 -4 14 533.30 79.43 5 -4 14 572.93 86.23 -5 -4 -14 593.43 134.80 2 9 -11 1237.05 95.68 2 9 -11 1115.58 95.05 -2 -9 11 1071.46 142.24 -2 -9 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-16 216.24 109.91 -9 -3 -16 165.88 40.94 -9 -3 -16 190.64 41.46 9 -3 16 179.59 61.60 -9 -3 -16 220.95 104.27 2 -12 13 91.52 50.80 2 -12 13 83.64 34.33 -2 12 -13 141.58 54.07 -2 -15 2 3.23 24.05 2 15 -2 51.16 34.97 -12 -2 -11 647.99 185.60 10 10 -7 499.51 128.80 -10 -10 7 225.08 102.69 -10 -10 7 358.54 134.88 -14 -2 5 70.52 37.04 -14 -2 5 52.05 23.65 -14 -2 5 131.51 48.21 14 -2 -5 198.01 88.58 14 2 -5 114.70 49.21 9 11 -7 88.98 52.75 -9 -11 7 52.22 27.09 -9 -11 7 35.49 29.43 -14 -1 -4 346.56 135.43 -14 -1 -4 412.71 199.58 -14 1 -4 378.51 134.11 -14 1 -4 375.35 128.44 12 -5 9 7.74 11.33 -12 -5 -9 14.44 26.28 -12 5 -9 51.62 17.75 5 10 -15 507.26 85.74 5 10 -15 208.44 130.18 -5 -10 15 414.61 164.10 -5 -10 15 538.66 60.67 2 15 2 67.71 22.05 -2 15 -2 76.62 19.40 -2 -15 -2 26.69 18.37 2 -15 2 29.92 18.71 2 -15 2 36.26 20.05 -4 6 -19 19.70 17.37 4 -6 19 12.39 21.01 5 6 -19 436.45 75.96 5 6 -19 465.70 134.34 -5 -6 19 249.60 73.10 -5 -6 19 374.79 95.93 -9 -5 -15 292.57 127.26 -9 -5 -15 434.99 138.25 -9 -5 -15 487.56 115.16 -2 -11 15 48.58 31.02 -2 -11 15 117.69 42.92 2 11 -15 167.58 74.67 2 11 -15 158.63 72.39 -11 9 -5 92.86 47.79 11 9 5 14.98 25.32 11 -9 5 24.48 25.94 -11 -9 -5 24.32 43.94 -12 7 -6 294.37 110.98 12 -7 6 187.76 115.74 -14 0 6 145.93 79.28 -5 5 -19 1100.67 208.12 5 -5 19 887.11 208.25 6 -5 -19 8.73 25.73 -6 -5 19 10.42 22.57 6 5 -19 21.82 25.01 -13 -6 -3 324.94 112.11 13 -6 3 389.31 136.75 -13 6 -3 416.21 103.14 13 6 3 318.54 142.86 -14 -3 -2 261.70 77.46 -14 -3 -2 332.22 107.93 -14 3 -2 245.92 135.43 -14 3 -2 266.13 100.72 2 -14 8 377.11 125.90 2 -14 8 502.00 122.87 -2 14 -8 144.52 125.13 1 0 -22 111.27 76.22 1 0 -22 83.59 52.86 9 11 6 216.62 51.24 -9 11 -6 197.32 77.27 -9 -11 -6 222.59 94.09 0 0 -22 128.13 37.70 0 0 -22 96.51 61.88 -12 4 -10 73.80 52.59 12 -4 10 20.65 16.95 13 -5 -7 102.70 37.38 -13 -5 7 110.14 27.44 -13 -5 7 126.60 46.54 13 5 -7 119.03 57.22 13 5 -7 193.52 85.53 -4 -13 10 598.20 87.33 11 8 -9 789.40 188.42 11 8 -9 825.66 52.46 -11 -8 9 959.16 111.19 -11 -8 9 678.06 81.77 4 14 6 331.61 102.61 -4 -14 -6 318.02 115.48 4 -14 6 508.51 94.97 0 -15 4 100.96 77.95 0 -15 4 130.07 28.10 0 15 -4 128.86 49.68 -3 8 -18 213.94 71.98 3 -8 18 265.87 115.00 3 -9 17 744.30 144.58 -10 10 -6 199.25 84.28 10 10 6 174.51 74.79 -10 -10 -6 229.73 61.96 10 -10 6 188.74 54.15 -2 13 -11 533.51 176.59 2 -13 11 583.69 175.33 5 -14 4 324.44 84.07 -5 -14 -4 346.21 120.57 -5 14 -4 291.72 64.60 5 14 4 288.24 96.89 -10 -2 -15 104.73 42.43 -10 -2 -15 22.16 37.02 -10 -2 -15 102.34 64.49 -6 -8 -16 772.70 132.86 -6 -8 -16 899.82 54.65 6 -8 16 780.47 232.56 11 6 -12 176.02 73.29 11 -6 -12 184.58 67.80 -11 -6 12 276.33 77.78 -11 -6 12 152.03 70.48 -14 1 6 117.59 58.10 14 1 -6 98.70 34.44 -14 -1 6 100.03 85.23 14 -1 -6 186.51 43.52 -3 -12 13 234.88 67.58 10 11 -1 17.78 16.25 -10 -11 1 27.14 20.73 7 12 8 727.29 140.72 -7 12 -8 797.70 168.97 -7 -12 -8 586.18 165.48 -14 -3 4 201.53 75.30 14 -3 -4 181.40 79.13 -14 -3 4 154.11 69.94 14 3 -4 191.86 87.20 14 3 -4 210.85 74.58 -7 -8 -15 234.22 71.71 -7 -8 -15 180.64 61.12 1 -1 -22 286.35 99.86 1 1 -22 434.17 99.92 4 8 -18 27.44 13.92 4 8 -18 8.65 40.61 -7 -13 -4 263.51 69.78 7 -13 4 141.34 113.05 7 13 4 189.96 81.42 -7 13 -4 252.62 55.21 -5 -13 9 87.14 33.85 -5 -13 9 82.03 41.60 -11 5 13 33.15 30.29 11 5 -13 139.12 77.41 -11 -5 13 127.12 36.48 5 -12 11 30.69 21.17 5 12 11 15.35 7.86 -5 12 -11 12.56 13.34 0 1 -22 429.22 105.32 0 1 -22 287.81 115.86 0 -1 -22 334.75 116.26 0 -1 -22 342.49 73.67 -7 -7 -16 69.04 36.96 -7 -7 -16 3.28 17.39 7 -7 16 124.97 58.01 9 10 -10 36.61 28.70 -9 -10 10 18.97 17.85 -9 -10 10 -1.32 25.12 2 15 -3 569.13 196.95 -2 -15 3 582.02 163.49 -13 -6 5 206.63 78.36 -13 -6 5 339.41 96.04 13 -6 -5 215.18 88.76 13 6 -5 204.25 78.22 13 6 -5 282.19 122.06 5 0 -21 219.05 72.90 -5 0 21 164.54 54.59 -1 -15 4 16.61 15.90 -1 -15 4 10.83 20.47 1 15 -4 37.52 27.98 4 9 -17 35.61 22.49 -4 -9 17 9.07 11.17 13 -2 -10 337.48 81.14 -4 -3 21 40.32 43.36 4 -3 -21 27.25 29.40 4 -3 -21 72.57 36.52 12 -6 8 4.10 18.19 -12 6 -8 17.32 23.38 12 8 -5 64.00 62.95 12 8 -5 44.41 57.61 -12 -8 5 93.64 40.94 12 -8 -5 44.76 26.86 -12 -8 5 197.13 67.28 11 0 -15 19.93 16.55 -11 0 15 69.95 35.27 7 -4 18 479.56 115.73 -7 -4 -18 448.13 86.32 -7 -4 -18 420.78 104.72 7 -4 18 404.79 164.62 -7 -4 -18 391.38 86.27 -10 -6 14 166.66 32.54 10 6 -14 116.54 61.47 -10 6 14 77.37 51.10 10 6 -14 131.67 61.39 -1 15 -4 19.88 17.89 1 -15 4 40.42 20.12 1 -15 4 7.30 23.73 -7 -12 9 165.62 50.78 -3 -4 21 666.35 221.87 6 -7 17 1485.08 84.53 -6 -7 -17 1202.36 178.89 -6 -7 -17 1157.98 115.13 -11 -3 -13 141.72 81.26 2 -15 3 545.71 118.62 -2 -15 -3 534.20 96.79 2 -15 3 550.51 154.11 2 15 3 274.45 144.61 -2 15 -3 545.97 88.17 -13 4 -7 1282.69 299.29 12 1 -13 73.56 31.23 6 -3 -20 517.79 121.70 -6 -3 20 358.37 132.71 -6 3 20 360.35 106.16 -9 10 -9 451.08 119.10 9 10 9 475.22 75.67 9 -10 9 338.77 113.89 -9 -10 -9 415.74 148.77 -8 4 -17 168.91 34.83 -8 -4 -17 71.72 44.62 -8 -4 -17 83.15 30.87 8 -4 17 16.18 18.25 -8 -4 -17 71.19 65.02 -10 3 16 581.90 203.96 10 3 -16 664.53 226.88 10 -3 -16 604.11 180.92 10 7 -13 121.83 78.56 10 7 -13 84.20 35.41 -10 -7 13 76.25 39.33 -10 -7 13 113.89 34.66 3 -3 21 168.04 55.10 3 -3 21 139.24 59.84 -3 3 -21 152.87 65.60 -3 3 -21 148.71 66.63 -3 3 -21 174.68 60.74 9 9 -12 368.34 156.08 -9 -9 12 304.79 93.66 -9 -9 12 401.88 142.42 -5 -1 21 -5.51 27.18 5 -1 -21 56.48 39.69 -5 1 21 21.19 28.67 -14 -2 -4 120.47 38.50 -14 -2 -4 90.65 24.73 -14 2 -4 167.69 49.63 -14 2 -4 70.25 49.80 -3 -6 20 0.05 18.29 -3 -6 20 26.56 22.76 3 6 -20 25.10 14.58 3 6 -20 59.91 37.94 -4 0 -21 46.94 56.68 4 0 21 46.90 30.41 -4 0 -21 49.75 19.51 -6 -9 -15 656.03 110.50 -6 -9 -15 466.70 91.74 2 -4 21 162.93 38.12 -2 4 -21 167.54 39.72 -2 4 -21 178.80 77.98 -6 11 -12 49.42 25.30 -6 -11 -12 54.09 25.49 -6 -11 -12 5.01 19.44 8 4 -18 115.60 52.00 -8 4 18 109.81 34.99 8 -4 -18 114.37 39.12 -8 -4 18 82.29 29.88 -1 0 -22 325.76 98.51 -11 1 15 344.83 170.27 11 1 -15 322.14 140.17 11 -1 -15 330.84 105.28 2 -6 20 370.34 114.69 -2 6 -20 575.23 126.82 -2 6 -20 257.10 80.97 0 14 -9 73.74 22.09 0 -14 9 181.35 42.26 0 -14 9 139.78 36.45 -5 3 -20 22.75 20.85 5 3 20 8.90 18.52 -5 3 -20 30.40 23.39 -5 3 -20 54.48 54.89 5 -3 20 52.51 32.01 -5 -3 -20 24.22 18.29 -8 -10 -11 185.59 100.22 -8 -10 -11 186.17 107.61 -8 10 -11 268.24 97.30 -13 3 -8 458.64 158.49 ; _shelx_hkl_checksum 41739 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Pd1 Pd -0.97689(2) -0.61184(4) -0.25708(2) 0.01397(7) Uani 1 1 d . F1 F -1.3857(3) -0.7140(3) -0.1765(3) 0.0658(12) Uani 1 1 d . F2 F -1.3152(4) -0.8130(5) -0.0726(2) 0.0949(19) Uani 1 1 d . F3 F -1.3013(4) -0.8796(4) -0.1923(3) 0.0849(16) Uani 1 1 d . F4 F -0.6540(3) -0.3467(3) -0.27616(19) 0.0405(8) Uani 1 1 d . F5 F -0.6611(3) -0.3300(3) -0.40760(18) 0.0445(8) Uani 1 1 d . F6 F -0.5702(3) -0.4820(3) -0.3503(2) 0.0498(9) Uani 1 1 d . O1 O -1.1466(3) -0.6817(3) -0.22770(17) 0.0176(6) Uani 1 1 d . O2 O -0.8679(3) -0.4646(4) -0.4101(2) 0.0372(9) Uani 1 1 d . O3 O -1.0884(3) -0.7238(4) -0.0952(2) 0.0380(9) Uani 1 1 d . O4 O -0.8074(3) -0.5401(3) -0.28525(17) 0.0182(6) Uani 1 1 d . N1 N -0.9097(3) -0.4350(3) -0.1188(2) 0.0166(7) Uani 1 1 d . N2 N -1.0676(3) -0.3076(3) -0.1124(2) 0.0203(7) Uani 1 1 d . N3 N -1.0901(3) -0.3942(3) -0.1727(2) 0.0158(7) Uani 1 1 d . N4 N -1.0406(3) -0.7987(3) -0.3921(2) 0.0170(7) Uani 1 1 d . N5 N -0.8764(4) -0.9208(3) -0.3933(2) 0.0236(8) Uani 1 1 d . N6 N -0.8578(3) -0.8301(3) -0.3364(2) 0.0181(7) Uani 1 1 d . C1 C -0.9961(4) -0.4726(4) -0.1782(2) 0.0153(8) Uani 1 1 d . C2 C -0.9574(4) -0.3359(4) -0.0808(2) 0.0192(8) Uani 1 1 d . H2 H -0.9148 -0.2935 -0.0369 0.023 Uiso 1 1 calc R C3 C -0.7902(4) -0.4943(4) -0.0928(3) 0.0202(9) Uani 1 1 d . H3A H -0.7272 -0.4328 -0.0752 0.024 Uiso 1 1 calc R H3B H -0.7567 -0.5380 -0.1406 0.024 Uiso 1 1 calc R C4 C -0.8077(5) -0.5808(4) -0.0222(3) 0.0349(13) Uani 1 1 d . H4A H -0.8718 -0.6406 -0.0388 0.052 Uiso 1 1 calc GR H4B H -0.8357 -0.5370 0.0264 0.052 Uiso 1 1 calc GR H4C H -0.7272 -0.6210 -0.0084 0.052 Uiso 1 1 calc GR C5 C -1.2098(4) -0.3946(4) -0.2232(3) 0.0181(8) Uani 1 1 d . H5 H -1.2081 -0.4673 -0.2593 0.022 Uiso 1 1 calc R C6 C -1.3230(5) -0.4091(5) -0.1672(3) 0.0253(10) Uani 1 1 d . H6A H -1.3025 -0.4718 -0.1254 0.030 Uiso 1 1 calc R H6B H -1.3971 -0.4370 -0.2014 0.030 Uiso 1 1 calc R C7 C -1.3595(4) -0.2939(5) -0.1218(3) 0.0268(10) Uani 1 1 d . H7 H -1.2893 -0.2737 -0.0808 0.032 Uiso 1 1 calc R C8 C -1.4806(5) -0.3121(6) -0.0743(4) 0.0428(14) Uani 1 1 d . H8A H -1.5515 -0.3291 -0.1136 0.064 Uiso 1 1 calc GR H8B H -1.4988 -0.2393 -0.0430 0.064 Uiso 1 1 calc GR H8C H -1.4691 -0.3795 -0.0358 0.064 Uiso 1 1 calc GR C9 C -1.3746(4) -0.1899(5) -0.1828(3) 0.0292(10) Uani 1 1 d . H9A H -1.4489 -0.2052 -0.2206 0.035 Uiso 1 1 calc R H9B H -1.3912 -0.1156 -0.1515 0.035 Uiso 1 1 calc R C10 C -1.2582(4) -0.1716(4) -0.2339(3) 0.0234(9) Uani 1 1 d . H10A H -1.1851 -0.1490 -0.1968 0.028 Uiso 1 1 calc R H10B H -1.2740 -0.1055 -0.2739 0.028 Uiso 1 1 calc R C11 C -1.2267(4) -0.2864(4) -0.2810(3) 0.0191(8) Uani 1 1 d . H11 H -1.3048 -0.3044 -0.3159 0.023 Uiso 1 1 calc R C12 C -1.1205(4) -0.2738(4) -0.3433(3) 0.0243(9) Uani 1 1 d . H12 H -1.0930 -0.3565 -0.3581 0.029 Uiso 1 1 calc R C13 C -1.0031(4) -0.2068(5) -0.3104(3) 0.0323(11) Uani 1 1 d . H13A H -1.0252 -0.1231 -0.2999 0.048 Uiso 1 1 calc GR H13B H -0.9374 -0.2102 -0.3515 0.048 Uiso 1 1 calc GR H13C H -0.9714 -0.2440 -0.2586 0.048 Uiso 1 1 calc GR C14 C -1.1713(5) -0.2139(6) -0.4235(3) 0.0364(12) Uani 1 1 d . H14A H -1.2398 -0.2626 -0.4487 0.055 Uiso 1 1 calc GR H14B H -1.1027 -0.2067 -0.4624 0.055 Uiso 1 1 calc GR H14C H -1.2037 -0.1340 -0.4108 0.055 Uiso 1 1 calc GR C15 C -0.9555(4) -0.7536(4) -0.3340(2) 0.0165(8) Uani 1 1 d . C16 C -0.9885(4) -0.8976(4) -0.4257(3) 0.0226(9) Uani 1 1 d . H16 H -1.0293 -0.9445 -0.4681 0.027 Uiso 1 1 calc R C17 C -1.1686(4) -0.7529(4) -0.4133(3) 0.0210(9) Uani 1 1 d . H17A H -1.2171 -0.7476 -0.3621 0.025 Uiso 1 1 calc R H17B H -1.2130 -0.8101 -0.4512 0.025 Uiso 1 1 calc R C18 C -1.1662(4) -0.6309(4) -0.4541(3) 0.0292(11) Uani 1 1 d . H18A H -1.1264 -0.6374 -0.5078 0.044 Uiso 1 1 calc GR H18B H -1.1177 -0.5751 -0.4184 0.044 Uiso 1 1 calc GR H18C H -1.2531 -0.6013 -0.4627 0.044 Uiso 1 1 calc GR C19 C -0.7409(4) -0.8243(4) -0.2813(3) 0.0209(9) Uani 1 1 d . H19 H -0.7052 -0.7418 -0.2861 0.025 Uiso 1 1 calc R C20 C -0.7763(4) -0.8419(4) -0.1906(3) 0.0227(9) Uani 1 1 d . H20A H -0.7023 -0.8208 -0.1538 0.027 Uiso 1 1 calc R H20B H -0.8460 -0.7863 -0.1781 0.027 Uiso 1 1 calc R C21 C -0.8173(5) -0.9693(4) -0.1714(3) 0.0254(10) Uani 1 1 d . H21 H -0.8945 -0.9884 -0.2070 0.030 Uiso 1 1 calc R C22 C -0.8512(5) -0.9799(5) -0.0808(3) 0.0384(13) Uani 1 1 d . H22A H -0.7765 -0.9616 -0.0451 0.058 Uiso 1 1 calc GR H22B H -0.8797 -1.0617 -0.0697 0.058 Uiso 1 1 calc GR H22C H -0.9192 -0.9234 -0.0693 0.058 Uiso 1 1 calc GR C23 C -0.7117(5) -1.0566(4) -0.1932(3) 0.0289(10) Uani 1 1 d . H23A H -0.7408 -1.1396 -0.1843 0.035 Uiso 1 1 calc R H23B H -0.6367 -1.0423 -0.1557 0.035 Uiso 1 1 calc R C24 C -0.6733(4) -1.0427(4) -0.2834(3) 0.0248(10) Uani 1 1 d . H24A H -0.7448 -1.0681 -0.3209 0.030 Uiso 1 1 calc R H24B H -0.6006 -1.0961 -0.2933 0.030 Uiso 1 1 calc R C25 C -0.6365(4) -0.9133(4) -0.3046(3) 0.0213(9) Uani 1 1 d . H25 H -0.5624 -0.8942 -0.2664 0.026 Uiso 1 1 calc R C26 C -0.5872(5) -0.8990(4) -0.3926(3) 0.0253(10) Uani 1 1 d . H26 H -0.6545 -0.9268 -0.4335 0.030 Uiso 1 1 calc R C27 C -0.4682(5) -0.9750(5) -0.4034(3) 0.0377(12) Uani 1 1 d . H27A H -0.4037 -0.9533 -0.3607 0.057 Uiso 1 1 calc GR H27B H -0.4353 -0.9604 -0.4585 0.057 Uiso 1 1 calc GR H27C H -0.4897 -1.0600 -0.3981 0.057 Uiso 1 1 calc GR C28 C -0.5552(5) -0.7687(5) -0.4120(3) 0.0335(11) Uani 1 1 d . H28A H -0.6331 -0.7209 -0.4140 0.050 Uiso 1 1 calc GR H28B H -0.5155 -0.7644 -0.4658 0.050 Uiso 1 1 calc GR H28C H -0.4966 -0.7372 -0.3687 0.050 Uiso 1 1 calc GR C29 C -0.7963(4) -0.4780(4) -0.3501(3) 0.0183(8) Uani 1 1 d . C30 C -0.6687(4) -0.4090(4) -0.3467(3) 0.0233(9) Uani 1 1 d . C31 C -1.1607(4) -0.7229(4) -0.1555(3) 0.0197(8) Uani 1 1 d . C32 C -1.2938(5) -0.7802(5) -0.1474(3) 0.0286(11) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01612(12) 0.01284(12) 0.01277(11) -0.00039(14) -0.00175(8) 0.00029(15) F1 0.0241(17) 0.048(2) 0.125(4) 0.028(2) -0.0080(19) -0.0074(15) F2 0.048(2) 0.193(6) 0.044(2) 0.044(3) 0.0069(18) -0.042(3) F3 0.070(3) 0.053(3) 0.134(4) -0.044(3) 0.042(3) -0.037(2) F4 0.0495(19) 0.0429(19) 0.0292(15) -0.0089(14) 0.0020(14) -0.0265(16) F5 0.049(2) 0.051(2) 0.0328(16) 0.0189(15) -0.0020(15) -0.0202(16) F6 0.0201(15) 0.0374(18) 0.092(3) -0.0047(19) 0.0025(16) 0.0020(13) O1 0.0162(14) 0.0191(15) 0.0175(13) 0.0027(12) -0.0016(11) -0.0058(12) O2 0.0311(18) 0.057(3) 0.0228(16) 0.0144(17) -0.0114(14) -0.0097(17) O3 0.0333(19) 0.058(2) 0.0224(16) 0.0162(16) -0.0086(14) -0.0100(18) O4 0.0176(14) 0.0201(15) 0.0168(13) 0.0033(12) -0.0011(11) -0.0014(12) N1 0.0168(16) 0.0197(18) 0.0130(15) -0.0016(14) -0.0044(13) 0.0000(14) N2 0.0249(19) 0.0186(18) 0.0173(16) -0.0069(15) -0.0018(14) 0.0002(15) N3 0.0168(16) 0.0154(17) 0.0146(15) -0.0043(13) -0.0056(13) -0.0020(13) N4 0.0195(17) 0.0161(17) 0.0148(15) -0.0006(13) -0.0058(13) -0.0008(14) N5 0.027(2) 0.0218(19) 0.0211(17) -0.0066(15) -0.0057(15) 0.0042(16) N6 0.0217(18) 0.0162(17) 0.0161(16) -0.0019(14) -0.0035(14) 0.0013(14) C1 0.019(2) 0.0158(19) 0.0112(17) 0.0001(15) 0.0000(15) -0.0022(16) C2 0.021(2) 0.022(2) 0.0153(18) -0.0017(17) -0.0021(16) -0.0020(17) C3 0.0150(19) 0.026(2) 0.0192(19) 0.0014(18) -0.0047(15) 0.0010(17) C4 0.032(3) 0.037(3) 0.035(2) 0.013(2) -0.010(2) 0.003(2) C5 0.019(2) 0.016(2) 0.0189(18) -0.0037(16) -0.0021(16) 0.0011(16) C6 0.026(2) 0.022(2) 0.028(2) 0.002(2) 0.000(2) -0.007(2) C7 0.020(2) 0.035(3) 0.025(2) -0.006(2) 0.0028(18) -0.0041(19) C8 0.029(3) 0.054(4) 0.046(3) -0.009(3) 0.010(2) -0.002(3) C9 0.027(2) 0.029(2) 0.032(2) -0.009(2) -0.0005(19) 0.008(2) C10 0.027(2) 0.018(2) 0.025(2) -0.0008(18) -0.0044(18) 0.0054(18) C11 0.020(2) 0.018(2) 0.0191(19) -0.0014(16) -0.0046(16) 0.0021(16) C12 0.028(2) 0.023(2) 0.022(2) -0.0036(18) 0.0001(18) 0.0016(18) C13 0.027(2) 0.041(3) 0.029(2) 0.002(2) 0.0008(19) -0.007(2) C14 0.033(3) 0.051(3) 0.025(2) 0.004(2) -0.002(2) -0.001(2) C15 0.020(2) 0.0159(19) 0.0131(17) 0.0012(16) -0.0020(15) -0.0024(16) C16 0.029(2) 0.017(2) 0.021(2) -0.0077(17) -0.0044(17) 0.0020(18) C17 0.017(2) 0.025(2) 0.0198(19) 0.0016(18) -0.0045(16) -0.0017(17) C18 0.029(2) 0.024(3) 0.034(2) 0.002(2) -0.0077(17) 0.004(2) C19 0.021(2) 0.019(2) 0.022(2) -0.0012(17) -0.0090(17) 0.0000(17) C20 0.025(2) 0.021(2) 0.022(2) -0.0042(17) -0.0076(17) 0.0098(18) C21 0.029(2) 0.026(2) 0.021(2) -0.0002(19) -0.0023(18) 0.0066(19) C22 0.051(3) 0.037(3) 0.028(3) 0.006(2) 0.009(2) 0.008(3) C23 0.036(3) 0.022(2) 0.028(2) 0.0022(19) 0.002(2) 0.006(2) C24 0.028(2) 0.019(2) 0.027(2) -0.0015(19) -0.0019(18) 0.0060(19) C25 0.018(2) 0.023(2) 0.023(2) 0.0017(18) -0.0031(17) 0.0038(18) C26 0.027(2) 0.027(2) 0.022(2) 0.0009(19) -0.0024(18) 0.003(2) C27 0.036(3) 0.039(3) 0.038(3) 0.001(2) 0.012(2) 0.010(2) C28 0.038(3) 0.037(3) 0.026(2) 0.005(2) 0.003(2) 0.000(2) C29 0.019(2) 0.020(2) 0.0161(18) -0.0014(16) 0.0015(15) 0.0015(17) C30 0.026(2) 0.025(2) 0.019(2) 0.0019(18) 0.0031(17) -0.0044(19) C31 0.023(2) 0.018(2) 0.0177(19) 0.0003(16) -0.0006(16) -0.0004(17) C32 0.034(3) 0.027(3) 0.025(2) 0.006(2) 0.005(2) -0.001(2) 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' O O 0.0106 0.0060 '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 O1 Pd1 O4 179.18(13) O1 Pd1 C15 87.95(14) O4 Pd1 C15 92.87(14) C1 Pd1 O1 92.09(14) C1 Pd1 O4 87.09(14) C1 Pd1 C15 178.65(17) C31 O1 Pd1 119.4(3) C29 O4 Pd1 120.9(3) C1 N1 C2 108.4(3) C1 N1 C3 127.2(4) C2 N1 C3 124.2(3) C2 N2 N3 103.4(3) N2 N3 C5 120.6(3) C1 N3 N2 113.5(3) C1 N3 C5 125.9(3) C15 N4 C17 127.1(4) C16 N4 C15 107.9(3) C16 N4 C17 124.9(4) C16 N5 N6 103.0(3) N5 N6 C19 121.5(3) C15 N6 N5 113.5(3) C15 N6 C19 125.0(3) N1 C1 Pd1 126.7(3) N3 C1 Pd1 129.9(3) N3 C1 N1 103.3(3) N1 C2 H2 124.4 N2 C2 N1 111.3(4) N2 C2 H2 124.4 N1 C3 H3A 109.2 N1 C3 H3B 109.2 N1 C3 C4 111.9(3) H3A C3 H3B 107.9 C4 C3 H3A 109.2 C4 C3 H3B 109.2 C3 C4 H4A 109.5 C3 C4 H4B 109.5 C3 C4 H4C 109.5 H4A C4 H4B 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 N3 C5 H5 106.9 N3 C5 C6 110.1(3) N3 C5 C11 114.2(3) C6 C5 H5 106.9 C11 C5 H5 106.9 C11 C5 C6 111.5(4) C5 C6 H6A 108.7 C5 C6 H6B 108.7 C5 C6 C7 114.1(4) H6A C6 H6B 107.6 C7 C6 H6A 108.7 C7 C6 H6B 108.7 C6 C7 H7 108.1 C8 C7 C6 111.0(4) C8 C7 H7 108.1 C9 C7 C6 110.6(4) C9 C7 H7 108.1 C9 C7 C8 110.9(4) C7 C8 H8A 109.5 C7 C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C7 C9 H9A 109.0 C7 C9 H9B 109.0 H9A C9 H9B 107.8 C10 C9 C7 112.7(4) C10 C9 H9A 109.0 C10 C9 H9B 109.0 C9 C10 H10A 109.5 C9 C10 H10B 109.5 C9 C10 C11 110.6(4) H10A C10 H10B 108.1 C11 C10 H10A 109.5 C11 C10 H10B 109.5 C5 C11 C10 112.3(3) C5 C11 H11 104.9 C5 C11 C12 113.5(3) C10 C11 H11 104.9 C10 C11 C12 115.1(4) C12 C11 H11 104.9 C11 C12 H12 107.3 C13 C12 C11 114.9(4) C13 C12 H12 107.3 C13 C12 C14 109.3(4) C14 C12 C11 110.5(4) C14 C12 H12 107.3 C12 C13 H13A 109.5 C12 C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C12 C14 H14A 109.5 C12 C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N4 C15 Pd1 128.3(3) N6 C15 Pd1 128.3(3) N6 C15 N4 103.3(3) N4 C16 H16 123.9 N5 C16 N4 112.3(4) N5 C16 H16 123.9 N4 C17 H17A 109.1 N4 C17 H17B 109.1 N4 C17 C18 112.5(3) H17A C17 H17B 107.8 C18 C17 H17A 109.1 C18 C17 H17B 109.1 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 N6 C19 H19 107.4 N6 C19 C20 109.6(3) N6 C19 C25 114.1(3) C20 C19 H19 107.4 C20 C19 C25 110.7(3) C25 C19 H19 107.4 C19 C20 H20A 108.9 C19 C20 H20B 108.9 H20A C20 H20B 107.7 C21 C20 C19 113.2(4) C21 C20 H20A 108.9 C21 C20 H20B 108.9 C20 C21 H21 108.4 C20 C21 C22 110.3(4) C20 C21 C23 109.4(4) C22 C21 H21 108.4 C22 C21 C23 111.8(4) C23 C21 H21 108.4 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 C21 C23 H23A 109.2 C21 C23 H23B 109.2 C21 C23 C24 112.1(4) H23A C23 H23B 107.9 C24 C23 H23A 109.2 C24 C23 H23B 109.2 C23 C24 H24A 109.1 C23 C24 H24B 109.1 C23 C24 C25 112.6(4) H24A C24 H24B 107.8 C25 C24 H24A 109.1 C25 C24 H24B 109.1 C19 C25 H25 105.1 C24 C25 C19 111.2(4) C24 C25 H25 105.1 C24 C25 C26 113.6(4) C26 C25 C19 115.5(4) C26 C25 H25 105.1 C25 C26 H26 108.5 C27 C26 C25 110.9(4) C27 C26 H26 108.5 C28 C26 C25 111.9(4) C28 C26 H26 108.5 C28 C26 C27 108.4(4) C26 C27 H27A 109.5 C26 C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28B 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 O2 C29 O4 130.7(4) O2 C29 C30 118.6(4) O4 C29 C30 110.6(3) F4 C30 C29 111.1(3) F5 C30 F4 106.0(4) F5 C30 C29 112.5(4) F6 C30 F4 107.0(4) F6 C30 F5 107.8(4) F6 C30 C29 112.1(4) O1 C31 C32 111.5(4) O3 C31 O1 130.4(4) O3 C31 C32 118.2(4) F1 C32 F3 104.7(5) F1 C32 C31 113.7(4) F2 C32 F1 110.1(5) F2 C32 F3 105.4(5) F2 C32 C31 112.8(4) F3 C32 C31 109.5(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 O1 2.028(3) Pd1 O4 2.029(3) Pd1 C1 2.025(4) Pd1 C15 2.030(4) F1 C32 1.293(6) F2 C32 1.290(6) F3 C32 1.326(6) F4 C30 1.338(5) F5 C30 1.326(5) F6 C30 1.324(5) O1 C31 1.267(5) O2 C29 1.213(5) O3 C31 1.211(5) O4 C29 1.264(5) N1 C1 1.362(5) N1 C2 1.371(5) N1 C3 1.471(5) N2 N3 1.385(5) N2 C2 1.291(5) N3 C1 1.330(5) N3 C5 1.476(5) N4 C15 1.368(5) N4 C16 1.357(5) N4 C17 1.472(5) N5 N6 1.376(5) N5 C16 1.302(5) N6 C15 1.342(5) N6 C19 1.493(5) C2 H2 0.9500 C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.511(6) C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 H5 1.0000 C5 C6 1.536(6) C5 C11 1.533(6) C6 H6A 0.9900 C6 H6B 0.9900 C6 C7 1.536(7) C7 H7 1.0000 C7 C8 1.531(6) C7 C9 1.526(7) C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.521(6) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.534(6) C11 H11 1.0000 C11 C12 1.542(6) C12 H12 1.0000 C12 C13 1.525(6) C12 C14 1.535(6) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C16 H16 0.9500 C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.514(6) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19 1.0000 C19 C20 1.537(6) C19 C25 1.542(6) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.523(6) C21 H21 1.0000 C21 C22 1.524(6) C21 C23 1.534(6) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.534(6) C24 H24A 0.9900 C24 H24B 0.9900 C24 C25 1.538(6) C25 H25 1.0000 C25 C26 1.540(6) C26 H26 1.0000 C26 C27 1.532(7) C26 C28 1.529(7) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 C30 1.551(6) C31 C32 1.555(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 Pd1 O1 C31 O3 4.0(7) Pd1 O1 C31 C32 -175.9(3) Pd1 O4 C29 O2 -12.6(7) Pd1 O4 C29 C30 166.3(3) O1 C31 C32 F1 -47.6(6) O1 C31 C32 F2 -173.9(5) O1 C31 C32 F3 69.1(6) O2 C29 C30 F4 126.7(5) O2 C29 C30 F5 8.0(6) O2 C29 C30 F6 -113.6(5) O3 C31 C32 F1 132.5(5) O3 C31 C32 F2 6.1(7) O3 C31 C32 F3 -110.8(6) O4 C29 C30 F4 -52.4(5) O4 C29 C30 F5 -171.0(4) O4 C29 C30 F6 67.3(5) N2 N3 C1 Pd1 -177.6(3) N2 N3 C1 N1 0.1(4) N2 N3 C5 C6 -60.3(5) N2 N3 C5 C11 66.0(5) N3 N2 C2 N1 0.5(4) N3 C5 C6 C7 77.8(5) N3 C5 C11 C10 -73.9(4) N3 C5 C11 C12 58.9(5) N5 N6 C15 Pd1 176.5(3) N5 N6 C15 N4 0.4(4) N5 N6 C19 C20 -114.5(4) N5 N6 C19 C25 10.3(5) N6 N5 C16 N4 -0.3(5) N6 C19 C20 C21 70.6(5) N6 C19 C25 C24 -71.8(5) N6 C19 C25 C26 59.5(5) C1 N1 C2 N2 -0.4(5) C1 N1 C3 C4 -90.6(5) C1 N3 C5 C6 119.0(4) C1 N3 C5 C11 -114.7(4) C2 N1 C1 Pd1 178.0(3) C2 N1 C1 N3 0.2(4) C2 N1 C3 C4 83.4(5) C2 N2 N3 C1 -0.3(4) C2 N2 N3 C5 179.0(3) C3 N1 C1 Pd1 -7.2(6) C3 N1 C1 N3 175.0(4) C3 N1 C2 N2 -175.4(4) C5 N3 C1 Pd1 3.0(6) C5 N3 C1 N1 -179.3(3) C5 C6 C7 C8 174.3(4) C5 C6 C7 C9 50.8(5) C5 C11 C12 C13 -85.5(5) C5 C11 C12 C14 150.3(4) C6 C5 C11 C10 51.8(5) C6 C5 C11 C12 -175.5(3) C6 C7 C9 C10 -54.2(5) C7 C9 C10 C11 56.9(5) C8 C7 C9 C10 -177.8(4) C9 C10 C11 C5 -55.3(5) C9 C10 C11 C12 172.8(4) C10 C11 C12 C13 45.8(5) C10 C11 C12 C14 -78.4(5) C11 C5 C6 C7 -50.0(5) C15 N4 C16 N5 0.6(5) C15 N4 C17 C18 67.2(5) C15 N6 C19 C20 62.7(5) C15 N6 C19 C25 -172.6(4) C16 N4 C15 Pd1 -176.7(3) C16 N4 C15 N6 -0.6(4) C16 N4 C17 C18 -115.4(5) C16 N5 N6 C15 0.0(5) C16 N5 N6 C19 177.4(4) C17 N4 C15 Pd1 1.0(6) C17 N4 C15 N6 177.2(4) C17 N4 C16 N5 -177.2(4) C19 N6 C15 Pd1 -0.8(6) C19 N6 C15 N4 -176.9(3) C19 C20 C21 C22 -179.8(4) C19 C20 C21 C23 56.8(5) C19 C25 C26 C27 169.4(4) C19 C25 C26 C28 48.2(6) C20 C19 C25 C24 52.4(5) C20 C19 C25 C26 -176.3(4) C20 C21 C23 C24 -55.1(5) C21 C23 C24 C25 54.4(5) C22 C21 C23 C24 -177.6(4) C23 C24 C25 C19 -52.5(5) C23 C24 C25 C26 175.2(4) C24 C25 C26 C27 -60.4(5) C24 C25 C26 C28 178.4(4) C25 C19 C20 C21 -56.1(5)