#------------------------------------------------------------------------------ #$Date: 2019-12-20 12:49:53 +0200 (Fri, 20 Dec 2019) $ #$Revision: 245433 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/66/1556697.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_1556697 loop_ _publ_author_name 'Messelberger, J.' 'Grunwald, A.' 'Stegner, P.' 'Senft, L.' 'Heinemann, F.W.' 'Munz, D.' _publ_section_title ; Transmetalation from Magnesium-NHCs-Convenient Synthesis of Chelating pi-Acidic NHC Complexes ; _journal_name_full Inorganics _journal_page_first 65 _journal_paper_doi 10.3390/inorganics7050065 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C43 H45 Br N5 Pd, Br' _chemical_formula_sum 'C43 H45 Br2 N5 Pd' _chemical_formula_weight 898.06 _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 _cell_angle_alpha 90 _cell_angle_beta 106.623(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.957(5) _cell_length_b 8.1726(17) _cell_length_c 22.929(5) _cell_measurement_reflns_used 6940 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.11 _cell_measurement_theta_min 2.32 _cell_volume 3763.0(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 83.33 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator 'Quazar focussing montel optics' _diffrn_radiation_source 'ImuS high brilliance micro-focus tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1164 _diffrn_reflns_av_unetI/netI 0.0882 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 46711 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 1.162 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.655 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1133 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.6130. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 1816 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.567 _refine_diff_density_min -1.487 _refine_diff_density_rms 0.164 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 468 _refine_ls_number_reflns 7389 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0694 _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^)+(0.0491P)^2^+34.1566P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1525 _refine_ls_wR_factor_ref 0.1683 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5351 _reflns_number_total 7389 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Inorganics-2019-7-65.cif _cod_data_source_block dm1603 _cod_original_cell_volume 3763.1(14) _cod_database_code 1556697 _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 0.676 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C26(H26), C29(H29), C38(H38), C41(H41) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C34(H34), C35(H35), C36(H36) 2.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B, H31C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A, H43B,H43C) ; _shelx_res_file ; TITL DM1603 in P2(1)/n, D.MUNZ, MD50 CELL 0.71073 20.9574 8.1726 22.9293 90 106.623 90 ZERR 4 0.0045 0.0017 0.0049 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Br Pd UNIT 172 180 20 8 4 L.S. 10 PLAN 20 SIZE 0.16 0.08 0.02 TEMP -173 BOND .5 $H HTAB CONF WPDB -1 LIST 4 fmap 2 acta MORE -1 OMIT -3 52 REM REM REM WGHT 0.049100 34.156590 FVAR 0.17652 PD1 5 0.455144 0.398459 0.688061 11.00000 0.01536 0.01343 = 0.01703 0.00267 0.00051 -0.00008 BR1 4 0.397989 0.271310 0.752688 11.00000 0.02568 0.03407 = 0.02928 0.00777 0.00588 -0.00095 BR2 4 0.550549 0.143594 0.608003 11.00000 0.05492 0.03170 = 0.03511 0.00527 0.01302 0.00327 N1 3 0.586217 0.352975 0.798127 11.00000 0.01475 0.01513 = 0.01762 0.00066 0.00100 0.00162 N2 3 0.590569 0.495240 0.719642 11.00000 0.01817 0.01461 = 0.01567 -0.00163 0.00058 -0.00041 N3 3 0.500132 0.523900 0.637516 11.00000 0.01732 0.00834 = 0.01826 -0.00054 -0.00153 0.00246 N4 3 0.398573 0.518398 0.568064 11.00000 0.01878 0.00960 = 0.01947 -0.00218 0.00369 -0.00281 N5 3 0.314716 0.394738 0.586704 11.00000 0.01675 0.01392 = 0.01386 -0.00086 0.00060 -0.00315 C1 1 0.548976 0.407439 0.745070 11.00000 0.02358 0.00867 = 0.02604 -0.00551 0.01077 0.00072 C2 1 0.653123 0.403475 0.808623 11.00000 0.01728 0.01600 = 0.01949 -0.00379 0.00143 0.00081 C3 1 0.708081 0.379184 0.858433 11.00000 0.02804 0.02321 = 0.01892 -0.01104 -0.00183 0.00321 AFIX 43 H3 2 0.706033 0.314509 0.892277 11.00000 -1.20000 AFIX 0 C4 1 0.766115 0.455114 0.855734 11.00000 0.01641 0.02513 = 0.02776 -0.00739 -0.00318 0.00581 AFIX 43 H4 2 0.804945 0.442831 0.889145 11.00000 -1.20000 AFIX 0 C5 1 0.770132 0.548421 0.806394 11.00000 0.01461 0.03059 = 0.02496 -0.00725 0.00428 0.00024 AFIX 43 H5 2 0.811119 0.598735 0.806792 11.00000 -1.20000 AFIX 0 C6 1 0.715238 0.568725 0.756864 11.00000 0.02303 0.01998 = 0.02141 -0.00233 0.00651 -0.00030 AFIX 43 H6 2 0.717995 0.631419 0.722779 11.00000 -1.20000 AFIX 0 C7 1 0.655537 0.495371 0.757779 11.00000 0.01747 0.01170 = 0.02310 -0.00149 0.00340 0.00169 C8 1 0.564816 0.559328 0.660286 11.00000 0.02302 0.01433 = 0.01490 -0.00236 -0.00043 0.00161 C9 1 0.596850 0.651845 0.627206 11.00000 0.01349 0.02933 = 0.02310 -0.00143 0.00241 -0.00880 AFIX 43 H9 2 0.642691 0.678398 0.643088 11.00000 -1.20000 AFIX 0 C10 1 0.560514 0.705103 0.570233 11.00000 0.02680 0.02209 = 0.02415 0.00036 0.01092 -0.00327 AFIX 43 H10 2 0.581514 0.770974 0.546965 11.00000 -1.20000 AFIX 0 C11 1 0.493999 0.664176 0.546421 11.00000 0.02354 0.02183 = 0.01713 0.00400 0.00376 -0.00189 AFIX 43 H11 2 0.469238 0.698786 0.506869 11.00000 -1.20000 AFIX 0 C12 1 0.465415 0.572753 0.581643 11.00000 0.01697 0.01152 = 0.01964 -0.00393 -0.00077 -0.00056 C13 1 0.345559 0.539600 0.515616 11.00000 0.01789 0.00902 = 0.01681 -0.00086 0.00080 0.00692 C14 1 0.337629 0.619380 0.460079 11.00000 0.03025 0.01331 = 0.01981 -0.00132 0.00451 -0.00358 AFIX 43 H14 2 0.373516 0.674572 0.450977 11.00000 -1.20000 AFIX 0 C15 1 0.275374 0.613786 0.419464 11.00000 0.04013 0.02363 = 0.01662 0.00506 0.00193 0.00186 AFIX 43 H15 2 0.268348 0.664639 0.380882 11.00000 -1.20000 AFIX 0 C16 1 0.221799 0.535889 0.432775 11.00000 0.02544 0.02817 = 0.02026 0.00085 -0.00200 -0.00302 AFIX 43 H16 2 0.179235 0.538059 0.403581 11.00000 -1.20000 AFIX 0 C17 1 0.229263 0.456647 0.486852 11.00000 0.02125 0.02356 = 0.02131 -0.00134 -0.00180 -0.00455 AFIX 43 H17 2 0.193229 0.401601 0.495752 11.00000 -1.20000 AFIX 0 C18 1 0.291733 0.460988 0.527619 11.00000 0.02139 0.01514 = 0.01353 -0.00316 0.00047 0.00508 C19 1 0.379147 0.430083 0.612139 11.00000 0.01871 0.01080 = 0.01402 0.00288 0.00229 0.00042 C20 1 0.566366 0.249547 0.840944 11.00000 0.01531 0.01902 = 0.02150 0.00557 -0.00057 0.00131 C21 1 0.555485 0.084518 0.827694 11.00000 0.02283 0.02519 = 0.02204 0.00290 -0.00287 0.00181 C22 1 0.541360 -0.013411 0.872075 11.00000 0.02885 0.01542 = 0.03155 0.00532 0.00006 -0.00083 AFIX 43 H22 2 0.533204 -0.126904 0.864535 11.00000 -1.20000 AFIX 0 C23 1 0.539062 0.051491 0.926362 11.00000 0.02451 0.02701 = 0.03946 0.01623 0.01361 0.00870 AFIX 43 H23 2 0.530769 -0.018311 0.956518 11.00000 -1.20000 AFIX 0 C24 1 0.548468 0.214689 0.937994 11.00000 0.02338 0.03397 = 0.01959 0.00458 0.00013 0.00417 AFIX 43 H24 2 0.546432 0.256716 0.976049 11.00000 -1.20000 AFIX 0 C25 1 0.560990 0.320695 0.895105 11.00000 0.01640 0.02968 = 0.02021 0.00514 0.00288 -0.00211 C26 1 0.559060 0.007908 0.768307 11.00000 0.04210 0.01923 = 0.02498 0.00143 -0.00170 0.00175 AFIX 13 H26 2 0.554042 0.096870 0.737376 11.00000 -1.20000 AFIX 0 C27 1 0.503903 -0.117410 0.743975 11.00000 0.03572 0.05644 = 0.07093 -0.03893 0.00427 -0.00143 AFIX 137 H27A 2 0.464040 -0.084520 0.755242 11.00000 -1.50000 H27B 2 0.518791 -0.225003 0.761508 11.00000 -1.50000 H27C 2 0.493447 -0.123208 0.699545 11.00000 -1.50000 AFIX 0 C28 1 0.626150 -0.074622 0.776318 11.00000 0.04041 0.04971 = 0.02922 -0.01061 0.01178 -0.00876 AFIX 137 H28A 2 0.661869 0.005804 0.790792 11.00000 -1.50000 H28B 2 0.628063 -0.119447 0.737212 11.00000 -1.50000 H28C 2 0.631703 -0.163347 0.806107 11.00000 -1.50000 AFIX 0 C29 1 0.563932 0.503109 0.906085 11.00000 0.02941 0.01773 = 0.02851 -0.00304 0.00750 0.00233 AFIX 13 H29 2 0.577938 0.556340 0.872443 11.00000 -1.20000 AFIX 0 C30 1 0.614726 0.548917 0.966303 11.00000 0.05994 0.05143 = 0.04019 -0.01801 0.01421 -0.01438 AFIX 137 H30A 2 0.658937 0.510020 0.966232 11.00000 -1.50000 H30B 2 0.602062 0.497987 1.000062 11.00000 -1.50000 H30C 2 0.615727 0.668096 0.971202 11.00000 -1.50000 AFIX 0 C31 1 0.494908 0.563387 0.902777 11.00000 0.05063 0.02100 = 0.06166 0.00265 0.02693 0.00468 AFIX 137 H31A 2 0.465179 0.544214 0.861806 11.00000 -1.50000 H31B 2 0.496566 0.680783 0.911800 11.00000 -1.50000 H31C 2 0.478164 0.504302 0.932577 11.00000 -1.50000 AFIX 0 C32 1 0.272227 0.289810 0.610156 11.00000 0.01829 0.01410 = 0.01536 0.00077 -0.00223 -0.00603 C33 1 0.282662 0.122415 0.608840 11.00000 0.02546 0.01957 = 0.01849 0.00109 -0.00297 -0.00632 C34 1 0.237855 0.022863 0.627050 11.00000 0.02767 0.02431 = 0.02583 -0.00121 -0.00078 -0.00138 AFIX 43 H34 2 0.242674 -0.092702 0.626846 11.00000 -1.20000 AFIX 0 C35 1 0.186514 0.091248 0.645382 11.00000 0.02253 0.03170 = 0.03527 0.00962 0.00303 -0.00755 AFIX 43 H35 2 0.155924 0.021302 0.656808 11.00000 -1.20000 AFIX 0 C36 1 0.178561 0.255898 0.647520 11.00000 0.02121 0.02700 = 0.03317 0.00410 0.00638 -0.00092 AFIX 43 H36 2 0.143440 0.299337 0.661375 11.00000 -1.20000 AFIX 0 C37 1 0.222010 0.362426 0.629345 11.00000 0.01558 0.02252 = 0.01996 0.00148 -0.00613 -0.00350 C38 1 0.340105 0.048201 0.589294 11.00000 0.03632 0.01971 = 0.03488 -0.00200 0.00950 -0.00133 AFIX 13 H38 2 0.379279 0.121761 0.605663 11.00000 -1.20000 AFIX 0 C39 1 0.327966 0.042955 0.521277 11.00000 0.04983 0.02461 = 0.04154 -0.00025 0.01163 0.00256 AFIX 137 H39A 2 0.369333 0.013399 0.512014 11.00000 -1.50000 H39B 2 0.313047 0.150752 0.503968 11.00000 -1.50000 H39C 2 0.293625 -0.038695 0.503625 11.00000 -1.50000 AFIX 0 C40 1 0.360422 -0.118841 0.616850 11.00000 0.02976 0.02857 = 0.04221 0.00217 0.00264 0.00629 AFIX 137 H40A 2 0.401853 -0.152729 0.608600 11.00000 -1.50000 H40B 2 0.325236 -0.198195 0.598867 11.00000 -1.50000 H40C 2 0.367332 -0.113768 0.660928 11.00000 -1.50000 AFIX 0 C41 1 0.214800 0.545090 0.633859 11.00000 0.01604 0.02973 = 0.02251 0.00084 0.00302 -0.00009 AFIX 13 H41 2 0.242121 0.598008 0.609797 11.00000 -1.20000 AFIX 0 C42 1 0.142608 0.602610 0.607503 11.00000 0.02515 0.03376 = 0.02636 0.00387 0.00059 0.00059 AFIX 137 H42A 2 0.124107 0.556071 0.566762 11.00000 -1.50000 H42B 2 0.141509 0.722316 0.604897 11.00000 -1.50000 H42C 2 0.116077 0.566200 0.634008 11.00000 -1.50000 AFIX 0 C43 1 0.243490 0.595683 0.699812 11.00000 0.02721 0.03470 = 0.02998 0.00069 0.00135 0.00072 AFIX 137 H43A 2 0.290473 0.563721 0.714041 11.00000 -1.50000 H43B 2 0.218789 0.541436 0.724736 11.00000 -1.50000 H43C 2 0.239751 0.714589 0.703286 11.00000 -1.50000 AFIX 0 HKLF 4 REM DM1603 in P2(1)/n, D.MUNZ, MD50 REM R1 = 0.0694 for 5351 Fo > 4sig(Fo) and 0.1029 for all 7389 data REM 468 parameters refined using 0 restraints END WGHT 0.0495 34.1313 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C11 Br2_$1 HTAB C14 Br2_$1 REM Highest difference peak 1.567, deepest hole -1.487, 1-sigma level 0.164 Q1 1 0.4970 0.2179 0.5787 11.00000 0.05 1.57 Q2 1 0.5832 0.2200 0.6473 11.00000 0.05 1.39 Q3 1 0.4431 0.2974 0.6791 11.00000 0.05 1.37 Q4 1 0.4424 0.4913 0.6777 11.00000 0.05 1.35 Q5 1 0.5778 0.0695 0.5690 11.00000 0.05 1.33 Q6 1 0.4768 0.3940 0.6711 11.00000 0.05 1.25 Q7 1 0.4366 0.3989 0.7059 11.00000 0.05 1.19 Q8 1 0.4278 0.0066 0.5056 11.00000 0.05 1.12 Q9 1 0.5223 -0.0088 0.6287 11.00000 0.05 1.10 Q10 1 0.5000 1.0000 0.5000 10.50000 0.05 0.97 Q11 1 0.4206 0.1524 0.7618 11.00000 0.05 0.90 Q12 1 0.4743 0.3908 0.7150 11.00000 0.05 0.81 Q13 1 0.5418 0.0033 0.6018 11.00000 0.05 0.81 Q14 1 0.2808 -0.0370 0.5222 11.00000 0.05 0.75 Q15 1 0.5005 0.0626 0.5925 11.00000 0.05 0.72 Q16 1 0.3647 0.3793 0.7382 11.00000 0.05 0.69 Q17 1 0.4579 0.5978 0.6703 11.00000 0.05 0.69 Q18 1 0.5143 0.0770 0.5676 11.00000 0.05 0.68 Q19 1 0.5204 0.4180 0.6500 11.00000 0.05 0.67 Q20 1 0.3770 0.1514 0.7383 11.00000 0.05 0.67 ; _shelx_res_checksum 91411 _shelx_hkl_file ; -1 0 0 -0.30 0.90 2 0 0 1912.41 196.68 -2 0 0 1773.12 196.78 2 0 0 1795.92 196.88 -2 0 0 1811.52 196.78 -2 0 0 1973.00 196.68 3 0 0 -1.20 2.40 -3 0 0 2.00 1.80 3 0 0 -5.60 2.30 -3 0 0 0.30 2.60 -3 0 0 1.60 1.90 -3 0 0 -1.00 3.20 3 0 0 -0.20 2.10 4 0 0 476.55 52.49 4 0 0 470.05 52.69 -4 0 0 503.55 52.39 -4 0 0 471.55 52.89 4 0 0 505.25 52.39 -4 0 0 515.75 52.39 5 0 0 1.50 3.70 -5 0 0 4.60 5.20 -5 0 0 3.50 2.70 -5 0 0 6.90 3.10 5 0 0 -0.70 3.70 6 0 0 1105.79 122.99 -6 0 0 1177.08 122.79 -6 0 0 1119.69 123.29 -6 0 0 1202.88 122.59 6 0 0 1156.08 122.89 -7 0 0 0.10 3.10 -7 0 0 5.50 6.50 7 0 0 14.00 4.90 7 0 0 3.20 4.50 -7 0 0 10.00 3.80 8 0 0 661.43 71.19 8 0 0 657.33 70.99 -8 0 0 652.83 71.89 -8 0 0 666.23 70.49 -8 0 0 663.83 70.79 -9 0 0 3.00 4.70 -9 0 0 0.20 3.60 9 0 0 1.50 5.90 9 0 0 1.20 5.50 -9 0 0 2.60 7.70 10 0 0 629.24 69.99 -10 0 0 624.04 71.19 -10 0 0 648.44 69.69 10 0 0 639.74 70.29 -10 0 0 687.33 69.29 11 0 0 0.20 6.90 -11 0 0 -4.60 8.70 11 0 0 3.30 6.30 -11 0 0 1.20 5.40 -11 0 0 -0.90 3.90 12 0 0 639.44 68.39 -12 0 0 649.64 67.39 12 0 0 633.24 68.79 -12 0 0 606.84 69.89 -12 0 0 615.14 68.09 13 0 0 7.00 7.30 -13 0 0 -6.60 9.60 13 0 0 4.90 7.90 -13 0 0 -6.40 6.00 14 0 0 202.88 25.10 -14 0 0 199.68 24.40 14 0 0 206.08 25.40 -15 0 0 -4.30 7.60 15 0 0 -3.50 8.40 15 0 0 -17.70 8.80 16 0 0 104.29 16.80 -16 0 0 113.49 15.70 16 0 0 113.09 17.40 17 0 0 -9.30 10.90 17 0 0 -3.60 10.80 -17 0 0 15.60 9.50 -18 0 0 662.33 77.69 18 0 0 766.02 80.29 -19 0 0 29.80 11.40 19 0 0 14.20 15.30 19 0 0 -5.80 12.50 20 0 0 575.84 67.59 20 0 0 623.94 69.19 21 0 0 -2.60 15.10 -21 0 0 0.60 12.10 21 0 0 0.70 14.60 22 0 0 334.37 43.20 -22 0 0 322.27 40.30 22 0 0 339.47 42.40 23 0 0 5.10 16.70 -23 0 0 1.40 13.80 -24 0 0 -11.30 14.50 24 0 0 -4.10 17.10 25 0 0 -11.60 20.00 -25 0 0 28.80 16.40 0 -1 0 2.50 1.90 0 -1 0 -1.80 2.40 0 1 0 -5.10 2.10 0 1 0 3.10 2.10 -1 -1 0 1202.88 121.89 -1 -1 0 1166.58 121.89 -1 -1 0 1101.59 121.89 -1 -1 0 1248.78 121.89 1 -1 0 1150.18 121.99 1 -1 0 1132.29 122.09 1 -1 0 1162.98 122.09 1 1 0 1131.29 121.89 1 1 0 1201.08 121.89 -1 1 0 1164.88 121.99 -1 1 0 1128.39 122.09 1 1 0 1069.59 121.89 1 1 0 1129.29 121.89 -1 1 0 1168.48 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13 1 -27 -3.80 21.30 13 1 -27 2.20 28.40 12 -1 -27 7.50 28.30 -12 -1 27 -4.90 17.50 12 -1 -27 5.40 22.00 12 -1 -27 -35.10 28.00 -12 1 27 -11.10 16.80 12 1 -27 -10.10 28.70 12 1 -27 -3.40 23.50 12 1 -27 -5.70 28.30 11 -1 -27 -0.50 26.90 -11 -1 27 1.40 17.40 11 -1 -27 51.39 32.90 11 1 -27 -15.90 22.90 11 1 -27 -18.30 26.00 11 1 -27 -0.70 27.10 -11 1 27 8.10 16.90 10 -1 -27 4.20 26.10 10 -1 -27 21.40 28.50 -10 -1 27 -50.39 15.80 10 1 -27 33.70 29.10 -10 1 27 -22.10 16.10 10 1 -27 9.10 27.60 10 1 -27 5.10 22.60 9 -1 -27 51.99 30.80 9 -1 -27 14.30 26.20 -9 -1 27 1.50 16.60 9 1 -27 -8.10 27.20 9 1 -27 2.50 29.30 -9 1 27 -15.90 16.00 9 1 -27 18.60 22.20 8 -1 -27 15.50 26.20 8 -1 -27 21.20 34.60 -8 -1 27 -7.20 16.10 8 1 -27 4.30 22.50 8 1 -27 7.10 25.30 -8 1 27 -10.30 15.20 8 1 -27 -15.20 24.70 -7 -1 27 -22.70 15.80 7 -1 -27 -14.40 28.80 7 -1 -27 0.70 24.90 7 1 -27 -16.70 26.50 -7 1 27 -20.90 15.00 7 1 -27 4.50 22.60 7 1 -27 1.00 24.90 6 -1 -27 42.10 24.90 6 -1 -27 9.10 29.40 -6 -1 27 -4.10 16.30 6 1 -27 18.70 22.50 -6 1 27 20.30 15.30 6 1 -27 -9.40 28.80 6 1 -27 30.40 25.90 5 -1 -27 82.69 35.00 5 -1 -27 63.09 23.30 -5 -1 27 11.80 16.00 5 1 -27 26.50 24.70 -5 1 27 8.10 15.30 5 1 -27 52.09 27.10 4 -1 -27 -7.60 29.50 -4 -1 27 0.30 15.20 4 1 -27 28.40 26.10 -4 1 27 1.00 22.80 4 1 -27 9.80 24.30 -3 -1 27 -19.50 14.30 3 -1 -27 -13.30 35.00 -3 -1 27 1.50 21.50 3 1 -27 21.60 30.40 3 1 -27 20.20 23.60 2 -1 -27 24.80 30.10 -2 -1 27 -18.00 13.80 -2 -1 27 -5.40 22.10 2 1 -27 3.10 22.90 2 1 -27 22.40 25.80 -1 -1 27 -5.50 22.20 1 -1 -27 1.10 35.30 1 1 -27 -14.40 25.50 1 1 -27 30.00 27.40 0 -1 -27 -19.70 28.90 0 -1 27 25.10 22.80 0 1 -27 20.60 30.40 0 1 -27 6.50 27.40 -1 -1 -27 44.90 34.70 1 -1 27 14.50 23.10 -1 1 -27 29.80 22.20 -1 1 -27 44.10 27.10 -2 -1 -27 -4.40 28.50 2 -1 27 30.10 22.10 2 1 27 17.20 23.90 -2 1 -27 -26.70 24.50 -16 -2 27 62.39 21.20 -16 2 27 53.89 23.20 16 2 -27 67.59 23.90 -15 -2 27 10.50 19.50 15 -2 -27 30.60 36.80 15 -2 -27 50.19 30.30 -15 2 27 -31.90 19.70 15 2 -27 9.10 30.60 15 2 -27 24.60 24.90 -14 -2 27 97.89 25.00 14 -2 -27 195.28 37.20 14 -2 -27 166.78 35.60 -14 2 27 88.69 25.60 14 2 -27 161.48 35.00 14 2 -27 118.49 27.90 13 -2 -27 48.10 30.20 -13 -2 27 16.20 18.70 13 -2 -27 40.80 30.40 -13 2 27 12.70 19.10 13 2 -27 12.60 24.20 13 2 -27 15.80 30.80 12 -2 -27 105.49 35.70 12 -2 -27 138.69 32.60 -12 -2 27 42.20 21.00 -12 2 27 54.79 20.80 12 2 -27 84.19 32.90 12 2 -27 83.89 24.00 11 -2 -27 50.49 33.80 11 -2 -27 9.60 27.10 -11 -2 27 1.70 18.50 11 2 -27 14.10 27.60 11 2 -27 24.40 20.70 -11 2 27 3.50 17.90 10 -2 -27 -20.80 26.10 10 -2 -27 24.50 29.50 -10 -2 27 -35.00 17.80 -10 2 27 -14.20 16.60 10 2 -27 -23.50 22.00 10 2 -27 3.30 26.80 -9 -2 27 -4.80 17.30 9 -2 -27 2.90 29.60 9 -2 -27 -18.70 26.00 -9 2 27 -16.30 16.90 9 2 -27 22.40 22.90 9 2 -27 -5.20 26.50 8 -2 -27 37.00 25.70 8 -2 -27 42.60 34.30 -8 -2 27 -15.80 17.00 -8 2 27 -11.80 16.10 8 2 -27 1.50 25.90 8 2 -27 17.20 19.90 8 2 -27 -17.50 27.30 -7 -2 27 -24.20 16.30 7 -2 -27 17.60 30.60 -7 -2 27 10.00 20.90 7 2 -27 17.10 19.60 -7 2 27 5.40 16.10 7 2 -27 2.50 28.90 7 2 -27 -4.70 22.90 6 -2 -27 109.29 34.90 -6 -2 27 142.19 27.50 -6 -2 27 60.79 21.00 -6 2 27 74.79 20.70 6 2 -27 139.59 28.40 6 2 -27 154.68 31.00 -5 -2 27 -11.50 15.20 5 -2 -27 36.00 32.20 -5 -2 27 -21.20 20.40 5 2 -27 11.30 26.00 5 2 -27 37.00 27.40 -4 -2 27 46.20 18.30 -4 -2 27 111.09 26.90 4 -2 -27 119.59 33.90 4 2 -27 102.49 31.50 4 2 -27 108.09 29.50 3 -2 -27 34.50 31.00 -3 -2 27 -12.30 14.20 -3 -2 27 35.90 21.70 3 2 -27 8.70 23.40 3 2 -27 39.30 25.80 -2 -2 27 54.59 19.40 -2 -2 27 131.09 27.20 2 -2 -27 134.19 35.30 2 2 -27 165.48 30.20 2 2 -27 156.68 30.40 1 -2 -27 30.50 30.60 -1 -2 27 -7.60 13.50 -1 -2 27 7.20 21.50 1 2 -27 5.70 25.20 1 2 -27 1.80 23.90 0 -2 27 6.10 22.00 0 -2 -27 41.70 38.40 0 2 -27 26.80 29.00 0 2 -27 7.70 24.30 -1 -2 -27 31.20 30.30 1 -2 27 9.10 22.40 -1 2 -27 14.40 23.90 -1 2 -27 -7.30 23.00 14 -3 -27 68.59 32.00 -14 -3 27 -3.30 19.80 14 -3 -27 -31.00 30.00 14 3 -27 11.80 28.60 -14 3 27 16.10 21.00 14 3 -27 16.90 19.90 13 -3 -27 34.30 31.40 -13 -3 27 6.70 19.90 13 -3 -27 64.39 36.00 13 3 -27 45.00 21.00 13 3 -27 43.70 30.40 -13 3 27 42.30 20.40 -12 -3 27 -19.70 19.10 12 -3 -27 49.50 31.20 12 -3 -27 -11.60 32.10 12 3 -27 19.40 20.30 12 3 -27 14.60 30.30 -12 3 27 -54.29 17.30 11 -3 -27 10.70 36.00 11 -3 -27 44.90 30.60 -11 -3 27 -9.70 20.00 -11 3 27 -34.00 17.50 11 3 -27 -6.70 27.90 11 3 -27 19.20 19.90 -10 -3 27 -16.30 18.90 10 -3 -27 41.20 30.20 10 3 -27 -3.30 18.90 10 3 -27 19.20 29.00 -10 3 27 3.40 17.80 9 -3 -27 91.19 32.90 -9 -3 27 22.20 19.50 -9 3 27 42.30 19.50 9 3 -27 78.69 31.00 9 3 -27 52.49 21.10 8 -3 -27 19.70 31.60 -8 -3 27 -49.90 16.60 8 3 -27 26.70 25.50 -8 3 27 -19.00 16.80 8 3 -27 4.80 20.90 -7 -3 27 46.80 26.00 -7 -3 27 2.50 17.50 7 -3 -27 9.50 30.80 -7 3 27 9.20 17.40 7 3 -27 20.30 27.60 7 3 -27 33.70 20.00 -6 -3 27 -13.40 19.30 6 -3 -27 16.90 32.10 -6 -3 27 -19.50 15.90 6 3 -27 6.40 27.30 -5 -3 27 -10.20 15.70 -5 -3 27 13.40 20.20 5 -3 -27 -6.90 41.50 5 3 -27 14.90 26.80 5 3 -27 14.40 24.70 -4 -3 27 -2.10 14.50 4 -3 -27 -3.00 31.70 -4 -3 27 -12.10 20.60 4 3 -27 30.50 26.50 4 3 -27 16.00 25.70 -3 -3 27 -25.90 14.00 3 -3 -27 6.50 40.90 -3 -3 27 -5.70 20.70 3 3 -27 0.30 26.40 3 3 -27 15.00 26.40 2 -3 -27 4.50 30.70 -2 -3 27 -13.10 13.90 -2 -3 27 5.20 21.10 2 3 -27 11.80 26.50 2 3 -27 8.30 26.20 1 -3 -27 28.00 32.30 -1 -3 27 2.30 13.90 -1 -3 27 26.70 21.70 1 3 -27 35.30 25.90 1 3 -27 -0.90 27.20 0 -3 27 3.60 13.50 -10 -4 27 -8.90 19.90 -10 4 27 -3.00 19.00 9 -4 -27 85.89 34.20 -9 -4 27 0.40 19.60 -9 4 27 2.80 19.50 9 4 -27 42.80 19.50 9 4 -27 49.30 30.50 -8 -4 27 -8.70 18.30 8 -4 -27 59.19 38.20 -8 4 27 -11.10 18.20 8 4 -27 -6.30 26.40 8 4 -27 38.40 19.10 7 -4 -27 49.00 34.70 -7 -4 27 -17.00 18.40 7 4 -27 22.00 29.60 6 -4 -27 40.10 34.00 -6 -4 27 -7.80 16.80 6 4 -27 23.10 26.30 -5 -4 27 -26.90 15.50 5 -4 -27 37.60 35.10 5 4 -27 -3.80 27.40 15 0 -28 17.60 32.90 -15 0 28 -29.20 18.00 15 0 -28 -10.50 22.60 14 0 -28 1.20 31.70 14 0 -28 32.90 29.30 -14 0 28 -3.80 18.70 14 0 -28 16.10 23.30 -13 0 28 -8.60 17.80 13 0 -28 -24.20 27.10 13 0 -28 -18.30 25.80 13 0 -28 -10.90 29.20 -12 0 28 -7.20 17.50 12 0 -28 19.40 24.20 12 0 -28 26.60 30.20 12 0 -28 46.20 29.30 -11 0 28 -7.20 16.80 11 0 -28 24.30 32.80 11 0 -28 -1.70 27.90 11 0 -28 23.20 24.90 10 0 -28 10.80 27.70 -10 0 28 -23.20 16.10 10 0 -28 17.10 23.80 10 0 -28 20.60 32.40 9 0 -28 7.50 28.30 9 0 -28 10.30 24.10 9 0 -28 22.20 29.00 -9 0 28 -7.00 16.10 8 0 -28 66.09 27.60 -8 0 28 8.50 17.10 8 0 -28 44.00 30.00 8 0 -28 48.70 24.60 7 0 -28 24.10 26.10 -7 0 28 -19.40 15.40 7 0 -28 30.10 28.90 7 0 -28 26.00 24.30 6 0 -28 84.39 28.70 6 0 -28 78.59 36.30 -6 0 28 44.90 17.80 5 0 -28 31.80 24.50 -5 0 28 -56.89 14.60 5 0 -28 9.00 29.10 -4 0 28 49.70 18.20 4 0 -28 111.59 31.60 4 0 -28 85.29 28.80 3 0 -28 25.20 27.00 3 0 -28 11.70 28.80 2 0 -28 21.60 28.80 -1 0 28 9.30 23.70 1 0 -28 22.10 35.40 0 0 28 64.39 28.00 0 0 -28 101.59 32.10 14 -1 -28 49.60 34.50 -14 -1 28 -20.60 19.60 14 -1 -28 -15.20 34.50 -14 1 28 -35.60 18.40 14 1 -28 -11.70 23.00 14 1 -28 11.80 31.90 13 -1 -28 33.50 34.30 -13 -1 28 -26.50 18.70 13 -1 -28 -2.30 30.60 13 1 -28 9.70 26.70 13 1 -28 7.90 30.70 -13 1 28 -27.70 17.80 12 -1 -28 -43.70 32.50 -12 -1 28 -3.60 18.10 12 -1 -28 -6.70 34.10 12 1 -28 -20.60 28.50 -12 1 28 -26.50 17.20 12 1 -28 19.70 22.10 11 -1 -28 -26.20 28.60 11 -1 -28 32.10 29.20 -11 -1 28 1.20 18.20 11 1 -28 16.80 30.90 11 1 -28 17.60 29.40 11 1 -28 21.00 20.90 -11 1 28 1.80 17.60 -10 -1 28 -4.60 17.30 10 -1 -28 -4.70 29.40 10 -1 -28 -13.70 30.20 10 1 -28 -24.50 26.80 -10 1 28 -6.90 16.40 10 1 -28 21.50 20.30 10 1 -28 14.70 30.80 9 -1 -28 -27.30 28.90 -9 -1 28 -2.50 17.30 9 -1 -28 31.40 35.70 9 1 -28 17.20 27.00 9 1 -28 33.50 21.10 9 1 -28 20.90 28.60 -9 1 28 -22.90 16.00 8 -1 -28 119.29 29.50 -8 -1 28 83.69 21.30 8 -1 -28 134.69 34.60 8 1 -28 117.09 25.00 8 1 -28 102.69 31.20 -8 1 28 47.50 20.00 8 1 -28 129.29 34.20 7 -1 -28 52.29 25.50 -7 -1 28 18.20 17.30 7 -1 -28 -11.70 30.60 7 1 -28 36.40 27.20 -7 1 28 22.50 16.80 7 1 -28 43.40 20.80 7 1 -28 58.09 27.70 6 -1 -28 156.58 40.10 6 -1 -28 168.38 31.90 -6 -1 28 21.60 19.50 6 1 -28 100.19 34.10 -6 1 28 78.59 19.40 6 1 -28 126.49 32.20 -5 -1 28 13.40 17.30 5 -1 -28 36.90 31.40 -5 1 28 31.60 16.30 5 1 -28 58.69 27.30 5 1 -28 40.90 26.90 -4 -1 28 19.30 22.40 4 -1 -28 43.60 31.90 -4 -1 28 -28.80 15.40 4 1 -28 -12.00 24.70 4 1 -28 -5.70 26.40 3 -1 -28 86.29 39.40 -3 -1 28 22.10 17.20 -3 -1 28 86.89 26.20 3 1 -28 83.69 27.90 3 1 -28 65.69 28.80 -2 -1 28 69.79 26.30 2 -1 -28 58.49 32.20 2 1 -28 56.59 25.10 2 1 -28 34.40 33.30 -1 -1 28 -13.40 22.30 1 -1 -28 32.30 35.80 1 1 -28 -4.60 26.10 1 1 -28 27.90 29.00 0 -1 -28 95.69 33.20 0 1 -28 51.19 29.20 0 1 -28 76.19 30.80 -13 -2 28 16.40 20.60 13 -2 -28 43.80 31.00 13 -2 -28 31.00 30.70 -13 2 28 15.20 20.20 13 2 -28 23.30 21.90 13 2 -28 11.20 32.30 -12 -2 28 -6.90 19.00 12 -2 -28 18.60 34.10 12 -2 -28 34.50 30.80 12 2 -28 8.60 30.60 12 2 -28 -1.30 25.00 -12 2 28 -25.30 18.20 11 -2 -28 37.50 31.90 11 -2 -28 64.19 30.00 -11 -2 28 14.20 18.90 11 2 -28 23.90 20.50 11 2 -28 41.80 28.40 -11 2 28 -6.40 18.50 10 -2 -28 -11.20 28.70 -10 -2 28 -35.70 18.40 10 -2 -28 42.80 31.50 10 2 -28 8.60 20.40 -10 2 28 -30.70 17.60 10 2 -28 14.70 29.40 -9 -2 28 -25.10 17.90 9 -2 -28 22.10 29.20 9 -2 -28 -30.90 35.10 9 2 -28 -4.90 20.80 -9 2 28 -28.10 17.50 9 2 -28 16.40 27.80 8 -2 -28 0.20 30.90 -8 -2 28 3.90 20.60 -8 -2 28 -17.90 17.50 8 2 -28 34.70 32.60 8 2 -28 7.70 30.10 -8 2 28 -1.80 16.80 8 2 -28 23.40 24.30 7 -2 -28 -30.90 31.30 -7 -2 28 -26.60 17.10 -7 -2 28 -22.10 21.30 7 2 -28 -1.90 29.20 -7 2 28 -3.70 16.60 7 2 -28 20.50 25.60 7 2 -28 -19.30 27.30 6 -2 -28 0.30 31.90 -6 -2 28 -2.40 22.40 -6 -2 28 1.00 16.90 6 2 -28 18.20 26.60 6 2 -28 11.00 24.60 -5 -2 28 -23.20 15.90 5 -2 -28 -41.90 31.40 -5 -2 28 3.20 22.10 5 2 -28 24.40 27.80 5 2 -28 -15.70 24.30 -4 -2 28 29.30 22.70 4 -2 -28 33.70 38.70 -4 -2 28 -10.30 15.80 4 2 -28 -1.70 24.20 4 2 -28 7.70 26.50 -3 -2 28 2.80 15.30 -3 -2 28 52.89 24.30 3 -2 -28 66.29 34.60 3 2 -28 69.79 28.10 3 2 -28 61.39 31.10 2 -2 -28 -7.90 40.90 -2 -2 28 -2.70 22.30 -2 -2 28 -12.80 14.70 2 2 -28 28.40 26.50 2 2 -28 -8.60 28.80 -10 -3 28 10.70 19.50 -10 3 28 -8.20 18.10 10 3 -28 10.60 20.10 -9 -3 28 -55.99 18.50 9 -3 -28 15.10 35.90 9 3 -28 -15.00 19.30 -9 3 28 -19.60 17.30 9 3 -28 4.40 29.40 8 -3 -28 1.30 31.30 -8 -3 28 -27.00 17.80 -8 3 28 -4.40 18.10 8 3 -28 25.50 20.50 8 3 -28 13.10 26.10 7 -3 -28 35.10 33.60 -7 -3 28 -26.90 17.20 7 3 -28 -4.20 28.30 -6 -3 28 -28.80 16.50 -6 -3 28 -44.10 20.90 6 -3 -28 58.19 43.00 6 3 -28 -1.10 27.50 -5 -3 28 -20.50 15.90 5 3 -28 19.80 26.60 -12 0 29 -25.40 17.60 -11 0 29 -12.70 17.60 11 0 -29 -20.40 31.60 11 0 -29 -34.50 33.10 11 0 -29 21.50 22.30 -10 0 29 -27.10 16.70 10 0 -29 10.00 29.20 10 0 -29 -26.70 28.20 10 0 -29 -9.60 21.70 9 0 -29 29.70 30.40 -9 0 29 -6.30 16.80 9 0 -29 13.30 28.00 8 0 -29 -0.30 30.90 -8 0 29 -42.70 16.00 8 0 -29 29.20 30.50 7 0 -29 23.90 36.00 -7 0 29 -6.70 16.40 7 0 -29 51.49 31.20 6 0 -29 39.60 30.80 6 0 -29 -14.00 29.70 -6 0 29 -2.00 16.40 5 0 -29 -53.89 28.70 -5 0 29 -15.00 16.30 5 0 -29 -5.00 28.70 4 0 -29 14.50 29.10 4 0 -29 5.00 35.00 -11 -1 29 -3.10 18.60 -11 1 29 -8.70 17.20 11 1 -29 14.70 26.90 -10 -1 29 -31.80 17.30 10 -1 -29 1.10 36.50 10 -1 -29 19.50 29.00 10 1 -29 26.40 32.50 10 1 -29 29.80 31.80 10 1 -29 15.60 26.10 -10 1 29 9.40 16.60 -9 -1 29 -25.10 17.60 9 -1 -29 -3.50 27.60 9 -1 -29 6.10 30.90 9 1 -29 16.90 29.80 9 1 -29 8.80 26.60 -9 1 29 -11.90 16.10 9 1 -29 -6.30 27.70 -8 -1 29 -42.40 17.00 8 -1 -29 28.60 29.70 8 -1 -29 7.70 32.40 -8 1 29 0.50 16.20 8 1 -29 6.00 32.10 8 1 -29 2.70 26.20 8 1 -29 12.90 27.80 7 -1 -29 64.99 32.30 7 -1 -29 41.10 32.80 -7 -1 29 -7.60 17.40 -7 1 29 8.50 16.40 7 1 -29 28.10 31.80 7 1 -29 61.19 33.10 6 -1 -29 5.70 36.90 -6 -1 29 -50.59 16.10 6 1 -29 -5.20 26.80 -6 1 29 -27.30 15.60 6 1 -29 7.90 32.70 -5 -1 29 9.00 18.70 -5 -1 29 120.49 27.50 5 -1 -29 72.59 35.60 5 1 -29 85.69 34.80 5 1 -29 97.09 29.70 -4 -1 29 4.30 16.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 25773 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 0.45514(3) 0.39846(7) 0.68806(2) 0.01613(16) Uani 1 1 d . . . . . Br1 Br 0.39799(4) 0.27131(11) 0.75269(4) 0.0301(2) Uani 1 1 d . . . . . Br2 Br 0.55055(5) 0.14359(12) 0.60800(4) 0.0405(3) Uani 1 1 d . . . . . N1 N 0.5862(3) 0.3530(7) 0.7981(3) 0.0166(13) Uani 1 1 d . . . . . N2 N 0.5906(3) 0.4952(7) 0.7196(3) 0.0170(13) Uani 1 1 d . . . . . N3 N 0.5001(3) 0.5239(7) 0.6375(3) 0.0160(13) Uani 1 1 d . . . . . N4 N 0.3986(3) 0.5184(7) 0.5681(3) 0.0163(13) Uani 1 1 d . . . . . N5 N 0.3147(3) 0.3947(7) 0.5867(2) 0.0156(12) Uani 1 1 d . . . . . C1 C 0.5490(4) 0.4074(9) 0.7451(3) 0.0187(15) Uani 1 1 d . . . . . C2 C 0.6531(3) 0.4035(9) 0.8086(3) 0.0184(15) Uani 1 1 d . . . . . C3 C 0.7081(4) 0.3792(10) 0.8584(3) 0.0252(18) Uani 1 1 d . . . . . H3 H 0.7060 0.3145 0.8923 0.030 Uiso 1 1 calc R . . . . C4 C 0.7661(4) 0.4551(10) 0.8557(4) 0.0251(18) Uani 1 1 d . . . . . H4 H 0.8049 0.4428 0.8891 0.030 Uiso 1 1 calc R . . . . C5 C 0.7701(4) 0.5484(10) 0.8064(3) 0.0237(17) Uani 1 1 d . . . . . H5 H 0.8111 0.5987 0.8068 0.028 Uiso 1 1 calc R . . . . C6 C 0.7152(4) 0.5687(9) 0.7569(3) 0.0214(16) Uani 1 1 d . . . . . H6 H 0.7180 0.6314 0.7228 0.026 Uiso 1 1 calc R . . . . C7 C 0.6555(3) 0.4954(9) 0.7578(3) 0.0179(15) Uani 1 1 d . . . . . C8 C 0.5648(4) 0.5593(9) 0.6603(3) 0.0186(16) Uani 1 1 d . . . . . C9 C 0.5969(4) 0.6518(10) 0.6272(3) 0.0226(17) Uani 1 1 d . . . . . H9 H 0.6427 0.6784 0.6431 0.027 Uiso 1 1 calc R . . . . C10 C 0.5605(4) 0.7051(10) 0.5702(3) 0.0236(17) Uani 1 1 d . . . . . H10 H 0.5815 0.7710 0.5470 0.028 Uiso 1 1 calc R . . . . C11 C 0.4940(4) 0.6642(9) 0.5464(3) 0.0213(16) Uani 1 1 d . . . . . H11 H 0.4692 0.6988 0.5069 0.026 Uiso 1 1 calc R . . . . C12 C 0.4654(3) 0.5728(8) 0.5816(3) 0.0173(15) Uani 1 1 d . . . . . C13 C 0.3456(3) 0.5396(8) 0.5156(3) 0.0154(15) Uani 1 1 d . . . . . C14 C 0.3376(4) 0.6194(9) 0.4601(3) 0.0217(16) Uani 1 1 d . . . . . H14 H 0.3735 0.6746 0.4510 0.026 Uiso 1 1 calc R . . . . C15 C 0.2754(4) 0.6138(10) 0.4195(3) 0.0281(18) Uani 1 1 d . . . . . H15 H 0.2683 0.6646 0.3809 0.034 Uiso 1 1 calc R . . . . C16 C 0.2218(4) 0.5359(10) 0.4328(3) 0.0264(18) Uani 1 1 d . . . . . H16 H 0.1792 0.5381 0.4036 0.032 Uiso 1 1 calc R . . . . C17 C 0.2293(4) 0.4566(10) 0.4869(3) 0.0237(17) Uani 1 1 d . . . . . H17 H 0.1932 0.4016 0.4958 0.028 Uiso 1 1 calc R . . . . C18 C 0.2917(4) 0.4610(9) 0.5276(3) 0.0176(15) Uani 1 1 d . . . . . C19 C 0.3791(3) 0.4301(8) 0.6121(3) 0.0150(15) Uani 1 1 d . . . . . C20 C 0.5664(3) 0.2495(9) 0.8409(3) 0.0198(16) Uani 1 1 d . . . . . C21 C 0.5555(4) 0.0845(10) 0.8277(3) 0.0253(18) Uani 1 1 d . . . . . C22 C 0.5414(4) -0.0134(10) 0.8721(4) 0.0271(18) Uani 1 1 d . . . . . H22 H 0.5332 -0.1269 0.8645 0.032 Uiso 1 1 calc R . . . . C23 C 0.5391(4) 0.0515(10) 0.9264(4) 0.0294(19) Uani 1 1 d . . . . . H23 H 0.5308 -0.0183 0.9565 0.035 Uiso 1 1 calc R . . . . C24 C 0.5485(4) 0.2147(10) 0.9380(3) 0.0269(18) Uani 1 1 d . . . . . H24 H 0.5464 0.2567 0.9760 0.032 Uiso 1 1 calc R . . . . C25 C 0.5610(4) 0.3207(10) 0.8951(3) 0.0226(17) Uani 1 1 d . . . . . C26 C 0.5591(4) 0.0079(10) 0.7683(4) 0.031(2) Uani 1 1 d . . . . . H26 H 0.5540 0.0969 0.7374 0.037 Uiso 1 1 calc R . . . . C27 C 0.5039(5) -0.1174(13) 0.7440(5) 0.057(3) Uani 1 1 d . . . . . H27A H 0.4640 -0.0845 0.7552 0.085 Uiso 1 1 calc GR . . . . H27B H 0.5188 -0.2250 0.7615 0.085 Uiso 1 1 calc GR . . . . H27C H 0.4934 -0.1232 0.6995 0.085 Uiso 1 1 calc GR . . . . C28 C 0.6261(4) -0.0746(12) 0.7763(4) 0.039(2) Uani 1 1 d . . . . . H28A H 0.6619 0.0058 0.7908 0.059 Uiso 1 1 calc GR . . . . H28B H 0.6281 -0.1194 0.7372 0.059 Uiso 1 1 calc GR . . . . H28C H 0.6317 -0.1633 0.8061 0.059 Uiso 1 1 calc GR . . . . C29 C 0.5639(4) 0.5031(9) 0.9061(4) 0.0254(18) Uani 1 1 d . . . . . H29 H 0.5779 0.5563 0.8724 0.030 Uiso 1 1 calc R . . . . C30 C 0.6147(5) 0.5489(13) 0.9663(4) 0.051(3) Uani 1 1 d . . . . . H30A H 0.6589 0.5100 0.9662 0.076 Uiso 1 1 calc GR . . . . H30B H 0.6021 0.4980 1.0001 0.076 Uiso 1 1 calc GR . . . . H30C H 0.6157 0.6681 0.9712 0.076 Uiso 1 1 calc GR . . . . C31 C 0.4949(5) 0.5634(11) 0.9028(5) 0.042(2) Uani 1 1 d . . . . . H31A H 0.4652 0.5442 0.8618 0.063 Uiso 1 1 calc GR . . . . H31B H 0.4966 0.6808 0.9118 0.063 Uiso 1 1 calc GR . . . . H31C H 0.4782 0.5043 0.9326 0.063 Uiso 1 1 calc GR . . . . C32 C 0.2722(3) 0.2898(9) 0.6102(3) 0.0174(15) Uani 1 1 d . . . . . C33 C 0.2827(4) 0.1224(9) 0.6088(3) 0.0231(17) Uani 1 1 d . . . . . C34 C 0.2379(4) 0.0229(11) 0.6271(3) 0.0277(18) Uani 1 1 d . . . . . H34 H 0.2427 -0.0927 0.6268 0.033 Uiso 1 1 calc R . . . . C35 C 0.1865(4) 0.0912(11) 0.6454(4) 0.0309(19) Uani 1 1 d . . . . . H35 H 0.1559 0.0213 0.6568 0.037 Uiso 1 1 calc R . . . . C36 C 0.1786(4) 0.2559(10) 0.6475(4) 0.0274(18) Uani 1 1 d . . . . . H36 H 0.1434 0.2993 0.6614 0.033 Uiso 1 1 calc R . . . . C37 C 0.2220(3) 0.3624(9) 0.6293(3) 0.0217(17) Uani 1 1 d . . . . . C38 C 0.3401(4) 0.0482(10) 0.5893(4) 0.0304(19) Uani 1 1 d . . . . . H38 H 0.3793 0.1218 0.6057 0.037 Uiso 1 1 calc R . . . . C39 C 0.3280(5) 0.0430(11) 0.5213(4) 0.039(2) Uani 1 1 d . . . . . H39A H 0.3693 0.0134 0.5120 0.058 Uiso 1 1 calc GR . . . . H39B H 0.3130 0.1508 0.5040 0.058 Uiso 1 1 calc GR . . . . H39C H 0.2936 -0.0387 0.5036 0.058 Uiso 1 1 calc GR . . . . C40 C 0.3604(4) -0.1188(11) 0.6169(4) 0.035(2) Uani 1 1 d . . . . . H40A H 0.4019 -0.1527 0.6086 0.053 Uiso 1 1 calc GR . . . . H40B H 0.3252 -0.1982 0.5989 0.053 Uiso 1 1 calc GR . . . . H40C H 0.3673 -0.1138 0.6609 0.053 Uiso 1 1 calc GR . . . . C41 C 0.2148(4) 0.5451(10) 0.6339(3) 0.0233(17) Uani 1 1 d . . . . . H41 H 0.2421 0.5980 0.6098 0.028 Uiso 1 1 calc R . . . . C42 C 0.1426(4) 0.6026(11) 0.6075(4) 0.0298(19) Uani 1 1 d . . . . . H42A H 0.1241 0.5561 0.5668 0.045 Uiso 1 1 calc GR . . . . H42B H 0.1415 0.7223 0.6049 0.045 Uiso 1 1 calc GR . . . . H42C H 0.1161 0.5662 0.6340 0.045 Uiso 1 1 calc GR . . . . C43 C 0.2435(4) 0.5957(11) 0.6998(4) 0.0320(19) Uani 1 1 d . . . . . H43A H 0.2905 0.5637 0.7140 0.048 Uiso 1 1 calc GR . . . . H43B H 0.2188 0.5414 0.7247 0.048 Uiso 1 1 calc GR . . . . H43C H 0.2398 0.7146 0.7033 0.048 Uiso 1 1 calc GR . . . . 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 0.0154(3) 0.0134(3) 0.0170(3) 0.0027(2) 0.0005(2) -0.0001(2) Br1 0.0257(4) 0.0341(5) 0.0293(4) 0.0078(4) 0.0059(3) -0.0010(4) Br2 0.0549(6) 0.0317(5) 0.0351(5) 0.0053(4) 0.0130(4) 0.0033(4) N1 0.015(3) 0.015(3) 0.018(3) 0.001(2) 0.001(2) 0.002(2) N2 0.018(3) 0.015(3) 0.016(3) -0.002(2) 0.001(2) 0.000(3) N3 0.017(3) 0.008(3) 0.018(3) -0.001(2) -0.002(2) 0.002(2) N4 0.019(3) 0.010(3) 0.019(3) -0.002(2) 0.004(2) -0.003(3) N5 0.017(3) 0.014(3) 0.014(3) -0.001(2) 0.001(2) -0.003(3) C1 0.024(4) 0.009(4) 0.026(4) -0.006(3) 0.011(3) 0.001(3) C2 0.017(3) 0.016(4) 0.019(4) -0.004(3) 0.001(3) 0.001(3) C3 0.028(4) 0.023(4) 0.019(4) -0.011(3) -0.002(3) 0.003(4) C4 0.016(4) 0.025(4) 0.028(4) -0.007(3) -0.003(3) 0.006(3) C5 0.015(4) 0.031(5) 0.025(4) -0.007(3) 0.004(3) 0.000(3) C6 0.023(4) 0.020(4) 0.021(4) -0.002(3) 0.007(3) 0.000(3) C7 0.017(4) 0.012(4) 0.023(4) -0.001(3) 0.003(3) 0.002(3) C8 0.023(4) 0.014(4) 0.015(4) -0.002(3) 0.000(3) 0.002(3) C9 0.013(3) 0.029(4) 0.023(4) -0.001(3) 0.002(3) -0.009(3) C10 0.027(4) 0.022(4) 0.024(4) 0.000(3) 0.011(3) -0.003(3) C11 0.024(4) 0.022(4) 0.017(4) 0.004(3) 0.004(3) -0.002(3) C12 0.017(3) 0.012(4) 0.020(4) -0.004(3) -0.001(3) -0.001(3) C13 0.018(3) 0.009(3) 0.017(4) -0.001(3) 0.001(3) 0.007(3) C14 0.030(4) 0.013(4) 0.020(4) -0.001(3) 0.005(3) -0.004(3) C15 0.040(5) 0.024(4) 0.017(4) 0.005(3) 0.002(3) 0.002(4) C16 0.025(4) 0.028(5) 0.020(4) 0.001(3) -0.002(3) -0.003(4) C17 0.021(4) 0.024(4) 0.021(4) -0.001(3) -0.002(3) -0.005(3) C18 0.021(4) 0.015(4) 0.014(3) -0.003(3) 0.000(3) 0.005(3) C19 0.019(3) 0.011(4) 0.014(3) 0.003(3) 0.002(3) 0.000(3) C20 0.015(4) 0.019(4) 0.021(4) 0.006(3) -0.001(3) 0.001(3) C21 0.023(4) 0.025(5) 0.022(4) 0.003(3) -0.003(3) 0.002(3) C22 0.029(4) 0.015(4) 0.032(4) 0.005(3) 0.000(4) -0.001(3) C23 0.025(4) 0.027(5) 0.039(5) 0.016(4) 0.014(4) 0.009(4) C24 0.023(4) 0.034(5) 0.020(4) 0.005(3) 0.000(3) 0.004(4) C25 0.016(4) 0.030(5) 0.020(4) 0.005(3) 0.003(3) -0.002(3) C26 0.042(5) 0.019(4) 0.025(4) 0.001(3) -0.002(4) 0.002(4) C27 0.036(5) 0.056(7) 0.071(7) -0.039(6) 0.004(5) -0.001(5) C28 0.040(5) 0.050(6) 0.029(5) -0.011(4) 0.012(4) -0.009(5) C29 0.029(4) 0.018(4) 0.029(4) -0.003(3) 0.008(3) 0.002(3) C30 0.060(7) 0.051(7) 0.040(6) -0.018(5) 0.014(5) -0.014(5) C31 0.051(6) 0.021(5) 0.062(6) 0.003(4) 0.027(5) 0.005(4) C32 0.018(4) 0.014(4) 0.015(4) 0.001(3) -0.002(3) -0.006(3) C33 0.025(4) 0.020(4) 0.018(4) 0.001(3) -0.003(3) -0.006(3) C34 0.028(4) 0.024(5) 0.026(4) -0.001(3) -0.001(3) -0.001(4) C35 0.023(4) 0.032(5) 0.035(5) 0.010(4) 0.003(3) -0.008(4) C36 0.021(4) 0.027(5) 0.033(5) 0.004(4) 0.006(3) -0.001(4) C37 0.016(4) 0.023(4) 0.020(4) 0.001(3) -0.006(3) -0.004(3) C38 0.036(5) 0.020(4) 0.035(5) -0.002(4) 0.009(4) -0.001(4) C39 0.050(6) 0.025(5) 0.042(5) 0.000(4) 0.012(4) 0.003(4) C40 0.030(4) 0.029(5) 0.042(5) 0.002(4) 0.003(4) 0.006(4) C41 0.016(4) 0.030(5) 0.023(4) 0.001(3) 0.003(3) 0.000(3) C42 0.025(4) 0.034(5) 0.026(4) 0.004(4) 0.001(3) 0.001(4) C43 0.027(4) 0.035(5) 0.030(4) 0.001(4) 0.001(4) 0.001(4) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 N3 Pd1 Br1 174.50(17) . . N3 Pd1 C1 79.7(3) . . N3 Pd1 C19 79.5(3) . . C1 Pd1 Br1 100.5(2) . . C19 Pd1 Br1 100.3(2) . . C19 Pd1 C1 159.2(3) . . C1 N1 C2 110.7(6) . . C1 N1 C20 127.9(6) . . C2 N1 C20 121.3(6) . . C1 N2 C7 110.9(6) . . C1 N2 C8 119.1(6) . . C7 N2 C8 129.8(6) . . C8 N3 Pd1 118.9(5) . . C8 N3 C12 121.4(6) . . C12 N3 Pd1 119.7(5) . . C13 N4 C12 130.1(6) . . C19 N4 C12 118.6(6) . . C19 N4 C13 111.3(6) . . C18 N5 C32 120.5(6) . . C19 N5 C18 111.1(6) . . C19 N5 C32 128.1(6) . . N1 C1 Pd1 142.2(6) . . N1 C1 N2 106.6(6) . . N2 C1 Pd1 111.1(5) . . C3 C2 N1 130.4(7) . . C3 C2 C7 123.0(7) . . C7 C2 N1 106.6(6) . . C2 C3 H3 122.2 . . C4 C3 C2 115.7(8) . . C4 C3 H3 122.2 . . C3 C4 H4 118.6 . . C3 C4 C5 122.9(7) . . C5 C4 H4 118.6 . . C4 C5 H5 119.7 . . C6 C5 C4 120.5(7) . . C6 C5 H5 119.7 . . C5 C6 H6 120.7 . . C5 C6 C7 118.6(7) . . C7 C6 H6 120.7 . . N2 C7 C2 105.1(6) . . N2 C7 C6 135.4(7) . . C6 C7 C2 119.3(6) . . N3 C8 N2 111.2(6) . . N3 C8 C9 120.3(6) . . C9 C8 N2 128.5(7) . . C8 C9 H9 120.9 . . C8 C9 C10 118.1(7) . . C10 C9 H9 120.9 . . C9 C10 H10 119.4 . . C9 C10 C11 121.2(7) . . C11 C10 H10 119.4 . . C10 C11 H11 121.2 . . C12 C11 C10 117.6(7) . . C12 C11 H11 121.2 . . N3 C12 N4 110.4(6) . . N3 C12 C11 121.4(6) . . C11 C12 N4 128.2(6) . . N4 C13 C14 134.5(7) . . C18 C13 N4 105.2(6) . . C18 C13 C14 120.2(6) . . C13 C14 H14 121.8 . . C15 C14 C13 116.5(7) . . C15 C14 H14 121.8 . . C14 C15 H15 118.8 . . C14 C15 C16 122.3(7) . . C16 C15 H15 118.8 . . C15 C16 H16 119.2 . . C17 C16 C15 121.5(7) . . C17 C16 H16 119.2 . . C16 C17 H17 121.8 . . C16 C17 C18 116.4(7) . . C18 C17 H17 121.8 . . C13 C18 N5 107.1(6) . . C17 C18 N5 129.9(7) . . C17 C18 C13 123.1(7) . . N4 C19 Pd1 111.8(5) . . N5 C19 Pd1 143.0(5) . . N5 C19 N4 105.2(5) . . C21 C20 N1 118.8(7) . . C21 C20 C25 123.1(7) . . C25 C20 N1 118.1(7) . . C20 C21 C22 117.1(7) . . C20 C21 C26 123.3(7) . . C22 C21 C26 119.6(7) . . C21 C22 H22 119.6 . . C23 C22 C21 120.9(8) . . C23 C22 H22 119.6 . . C22 C23 H23 119.4 . . C24 C23 C22 121.1(8) . . C24 C23 H23 119.4 . . C23 C24 H24 119.4 . . C23 C24 C25 121.1(8) . . C25 C24 H24 119.4 . . C20 C25 C29 123.1(7) . . C24 C25 C20 116.5(7) . . C24 C25 C29 120.3(7) . . C21 C26 H26 108.3 . . C21 C26 C27 112.2(8) . . C21 C26 C28 110.8(7) . . C27 C26 H26 108.3 . . C28 C26 H26 108.3 . . C28 C26 C27 108.9(7) . . 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 . . C25 C29 H29 107.9 . . C25 C29 C30 112.1(7) . . C30 C29 H29 107.9 . . C31 C29 C25 108.7(7) . . C31 C29 H29 107.9 . . C31 C29 C30 112.0(8) . . 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 . . C29 C31 H31A 109.5 . . C29 C31 H31B 109.5 . . C29 C31 H31C 109.5 . . H31A C31 H31B 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C33 C32 N5 117.3(7) . . C37 C32 N5 117.9(6) . . C37 C32 C33 124.6(7) . . C32 C33 C34 116.4(7) . . C32 C33 C38 122.8(7) . . C34 C33 C38 120.8(7) . . C33 C34 H34 119.8 . . C35 C34 C33 120.4(8) . . C35 C34 H34 119.8 . . C34 C35 H35 119.1 . . C36 C35 C34 121.8(8) . . C36 C35 H35 119.1 . . C35 C36 H36 119.8 . . C35 C36 C37 120.4(8) . . C37 C36 H36 119.8 . . C32 C37 C36 116.4(7) . . C32 C37 C41 123.1(7) . . C36 C37 C41 120.4(7) . . C33 C38 H38 106.4 . . C39 C38 C33 113.7(7) . . C39 C38 H38 106.4 . . C39 C38 C40 110.5(7) . . C40 C38 C33 112.8(7) . . C40 C38 H38 106.4 . . C38 C39 H39A 109.5 . . C38 C39 H39B 109.5 . . C38 C39 H39C 109.5 . . H39A C39 H39B 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . C38 C40 H40A 109.5 . . C38 C40 H40B 109.5 . . C38 C40 H40C 109.5 . . H40A C40 H40B 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C37 C41 H41 107.8 . . C37 C41 C42 112.6(6) . . C37 C41 C43 108.6(6) . . C42 C41 H41 107.8 . . C43 C41 H41 107.8 . . C43 C41 C42 112.0(7) . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42B 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C41 C43 H43A 109.5 . . C41 C43 H43B 109.5 . . C41 C43 H43C 109.5 . . H43A C43 H43B 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 Br1 2.3929(10) . Pd1 N3 1.977(6) . Pd1 C1 2.027(7) . Pd1 C19 2.012(7) . N1 C1 1.321(9) . N1 C2 1.415(9) . N1 C20 1.444(9) . N2 C1 1.380(9) . N2 C7 1.392(9) . N2 C8 1.413(9) . N3 C8 1.338(9) . N3 C12 1.340(9) . N4 C12 1.417(9) . N4 C13 1.395(9) . N4 C19 1.394(9) . N5 C18 1.410(9) . N5 C19 1.340(9) . N5 C32 1.446(9) . C2 C3 1.385(10) . C2 C7 1.400(10) . C3 H3 0.9500 . C3 C4 1.382(11) . C4 H4 0.9500 . C4 C5 1.387(11) . C5 H5 0.9500 . C5 C6 1.376(10) . C6 H6 0.9500 . C6 C7 1.393(10) . C8 C9 1.374(10) . C9 H9 0.9500 . C9 C10 1.381(10) . C10 H10 0.9500 . C10 C11 1.385(10) . C11 H11 0.9500 . C11 C12 1.359(10) . C13 C14 1.398(10) . C13 C18 1.392(10) . C14 H14 0.9500 . C14 C15 1.370(11) . C15 H15 0.9500 . C15 C16 1.398(11) . C16 H16 0.9500 . C16 C17 1.368(11) . C17 H17 0.9500 . C17 C18 1.374(10) . C20 C21 1.387(11) . C20 C25 1.405(11) . C21 C22 1.391(11) . C21 C26 1.520(11) . C22 H22 0.9500 . C22 C23 1.367(12) . C23 H23 0.9500 . C23 C24 1.363(12) . C24 H24 0.9500 . C24 C25 1.391(11) . C25 C29 1.510(11) . C26 H26 1.0000 . C26 C27 1.526(12) . C26 C28 1.522(12) . 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 H29 1.0000 . C29 C30 1.529(12) . C29 C31 1.509(12) . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C32 C33 1.387(11) . C32 C37 1.385(11) . C33 C34 1.394(11) . C33 C38 1.525(11) . C34 H34 0.9500 . C34 C35 1.380(12) . C35 H35 0.9500 . C35 C36 1.359(12) . C36 H36 0.9500 . C36 C37 1.406(11) . C37 C41 1.507(11) . C38 H38 1.0000 . C38 C39 1.507(12) . C38 C40 1.513(12) . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 H41 1.0000 . C41 C42 1.534(10) . C41 C43 1.516(11) . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 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 Pd1 N3 C8 N2 0.6(8) . . . . Pd1 N3 C8 C9 -177.4(6) . . . . Pd1 N3 C12 N4 -1.2(8) . . . . Pd1 N3 C12 C11 177.6(6) . . . . N1 C2 C3 C4 -175.7(7) . . . . N1 C2 C7 N2 -0.1(7) . . . . N1 C2 C7 C6 176.7(6) . . . . N1 C20 C21 C22 175.3(6) . . . . N1 C20 C21 C26 -4.0(11) . . . . N1 C20 C25 C24 -173.6(6) . . . . N1 C20 C25 C29 10.3(10) . . . . N2 C8 C9 C10 -178.1(7) . . . . N3 C8 C9 C10 -0.5(11) . . . . N4 C13 C14 C15 -179.0(8) . . . . N4 C13 C18 N5 -0.4(7) . . . . N4 C13 C18 C17 179.0(7) . . . . N5 C32 C33 C34 -175.0(6) . . . . N5 C32 C33 C38 5.6(10) . . . . N5 C32 C37 C36 175.3(6) . . . . N5 C32 C37 C41 -7.5(10) . . . . C1 N1 C2 C3 177.7(8) . . . . C1 N1 C2 C7 0.1(8) . . . . C1 N1 C20 C21 74.3(10) . . . . C1 N1 C20 C25 -107.6(8) . . . . C1 N2 C7 C2 0.0(8) . . . . C1 N2 C7 C6 -176.0(8) . . . . C1 N2 C8 N3 0.9(9) . . . . C1 N2 C8 C9 178.7(7) . . . . C2 N1 C1 Pd1 176.2(7) . . . . C2 N1 C1 N2 -0.2(8) . . . . C2 N1 C20 C21 -102.6(8) . . . . C2 N1 C20 C25 75.5(9) . . . . C2 C3 C4 C5 -0.7(11) . . . . C3 C2 C7 N2 -177.8(7) . . . . C3 C2 C7 C6 -1.0(11) . . . . C3 C4 C5 C6 -0.4(12) . . . . C4 C5 C6 C7 0.8(11) . . . . C5 C6 C7 N2 175.5(8) . . . . C5 C6 C7 C2 -0.1(11) . . . . C7 N2 C1 Pd1 -177.5(5) . . . . C7 N2 C1 N1 0.1(8) . . . . C7 N2 C8 N3 175.6(7) . . . . C7 N2 C8 C9 -6.6(13) . . . . C7 C2 C3 C4 1.4(11) . . . . C8 N2 C1 Pd1 -1.8(8) . . . . C8 N2 C1 N1 175.8(6) . . . . C8 N2 C7 C2 -175.1(7) . . . . C8 N2 C7 C6 8.9(13) . . . . C8 N3 C12 N4 179.3(6) . . . . C8 N3 C12 C11 -1.8(11) . . . . C8 C9 C10 C11 -1.2(12) . . . . C9 C10 C11 C12 1.4(12) . . . . C10 C11 C12 N3 0.1(11) . . . . C10 C11 C12 N4 178.7(7) . . . . C12 N3 C8 N2 180.0(6) . . . . C12 N3 C8 C9 2.0(11) . . . . C12 N4 C13 C14 -1.2(13) . . . . C12 N4 C13 C18 -179.8(7) . . . . C12 N4 C19 Pd1 -0.4(8) . . . . C12 N4 C19 N5 -179.5(6) . . . . C13 N4 C12 N3 -179.4(6) . . . . C13 N4 C12 C11 1.8(12) . . . . C13 N4 C19 Pd1 180.0(4) . . . . C13 N4 C19 N5 0.9(8) . . . . C13 C14 C15 C16 1.4(12) . . . . C14 C13 C18 N5 -179.3(6) . . . . C14 C13 C18 C17 0.1(11) . . . . C14 C15 C16 C17 -1.9(13) . . . . C15 C16 C17 C18 1.3(12) . . . . C16 C17 C18 N5 178.7(7) . . . . C16 C17 C18 C13 -0.5(11) . . . . C18 N5 C19 Pd1 -179.7(7) . . . . C18 N5 C19 N4 -1.2(8) . . . . C18 N5 C32 C33 100.3(8) . . . . C18 N5 C32 C37 -76.4(8) . . . . C18 C13 C14 C15 -0.5(10) . . . . C19 N4 C12 N3 1.1(9) . . . . C19 N4 C12 C11 -177.7(7) . . . . C19 N4 C13 C14 178.3(8) . . . . C19 N4 C13 C18 -0.3(8) . . . . C19 N5 C18 C13 1.0(8) . . . . C19 N5 C18 C17 -178.3(8) . . . . C19 N5 C32 C33 -72.8(9) . . . . C19 N5 C32 C37 110.4(8) . . . . C20 N1 C1 Pd1 -1.0(13) . . . . C20 N1 C1 N2 -177.4(6) . . . . C20 N1 C2 C3 -4.9(12) . . . . C20 N1 C2 C7 177.6(6) . . . . C20 C21 C22 C23 -0.6(11) . . . . C20 C21 C26 C27 -139.2(8) . . . . C20 C21 C26 C28 98.9(9) . . . . C20 C25 C29 C30 -128.5(8) . . . . C20 C25 C29 C31 107.1(9) . . . . C21 C20 C25 C24 4.4(11) . . . . C21 C20 C25 C29 -171.7(7) . . . . C21 C22 C23 C24 2.1(12) . . . . C22 C21 C26 C27 41.5(10) . . . . C22 C21 C26 C28 -80.4(9) . . . . C22 C23 C24 C25 -0.3(12) . . . . C23 C24 C25 C20 -2.8(11) . . . . C23 C24 C25 C29 173.4(7) . . . . C24 C25 C29 C30 55.6(10) . . . . C24 C25 C29 C31 -68.9(9) . . . . C25 C20 C21 C22 -2.7(11) . . . . C25 C20 C21 C26 178.0(7) . . . . C26 C21 C22 C23 178.8(7) . . . . C32 N5 C18 C13 -173.2(6) . . . . C32 N5 C18 C17 7.5(11) . . . . C32 N5 C19 Pd1 -6.0(13) . . . . C32 N5 C19 N4 172.5(6) . . . . C32 C33 C34 C35 -0.2(11) . . . . C32 C33 C38 C39 -78.9(10) . . . . C32 C33 C38 C40 154.2(7) . . . . C32 C37 C41 C42 135.3(7) . . . . C32 C37 C41 C43 -100.0(8) . . . . C33 C32 C37 C36 -1.2(11) . . . . C33 C32 C37 C41 176.0(7) . . . . C33 C34 C35 C36 -1.3(12) . . . . C34 C33 C38 C39 101.7(9) . . . . C34 C33 C38 C40 -25.2(10) . . . . C34 C35 C36 C37 1.7(13) . . . . C35 C36 C37 C32 -0.5(11) . . . . C35 C36 C37 C41 -177.8(7) . . . . C36 C37 C41 C42 -47.6(10) . . . . C36 C37 C41 C43 77.0(8) . . . . C37 C32 C33 C34 1.5(11) . . . . C37 C32 C33 C38 -177.9(7) . . . . C38 C33 C34 C35 179.2(7) . . . .