#------------------------------------------------------------------------------ #$Date: 2021-08-01 07:44:10 +0300 (Sun, 01 Aug 2021) $ #$Revision: 267883 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564312.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_1564312 loop_ _publ_author_name 'Dong, Jie' 'Wang, Baiquan' _publ_section_title ; Homo- and copolymerization of norbornene using tridentate IzQO palladium catalysts with dimethylaminoethyl as a side arm ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/D1PY00699A _journal_year 2021 _chemical_formula_moiety 'C34 H38 Cl N3 O3 Pd, 0.13(C H2 Cl2)' _chemical_formula_sum 'C34.12 H38.25 Cl1.25 N3 O3 Pd' _chemical_formula_weight 689.14 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-09-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-05-05 deposited with the CCDC. 2021-07-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.780(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.1028(7) _cell_length_b 14.4854(5) _cell_length_c 24.8028(9) _cell_measurement_reflns_used 14409 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 32.1260 _cell_measurement_theta_min 1.7530 _cell_volume 6367.0(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection CrystalClear(Rigaku,2008) _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 113.15 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -115.00 65.00 1.00 3.00 -- -25.00 45.00 0.00 180 2 \w -115.00 65.00 1.00 3.00 -- -25.00 45.00 90.00 180 3 \w -115.00 65.00 1.00 3.00 -- -25.00 45.00 180.00 180 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Rigaku Saturn 70 CCD' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0030482000 _diffrn_orient_matrix_UB_12 -0.0431365000 _diffrn_orient_matrix_UB_13 -0.0128859000 _diffrn_orient_matrix_UB_21 -0.0238950000 _diffrn_orient_matrix_UB_22 -0.0203370000 _diffrn_orient_matrix_UB_23 0.0160599000 _diffrn_orient_matrix_UB_31 -0.0319687000 _diffrn_orient_matrix_UB_32 0.0111421000 _diffrn_orient_matrix_UB_33 -0.0207166000 _diffrn_radiation_monochromator confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 33438 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.367 _diffrn_reflns_theta_min 1.677 _diffrn_source 'rotating anode' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _exptl_crystal_density_diffrn 1.438 _exptl_crystal_description block _exptl_crystal_F_000 2842 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.569 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 414 _refine_ls_number_reflns 6509 _refine_ls_number_restraints 21 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0402 _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^)+(0.0304P)^2^+13.3063P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.0900 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5311 _reflns_number_total 6509 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1py00699a2.cif _cod_data_source_block r20200914c _cod_database_code 1564312 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C11 H10 N O' _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 0.899 _shelx_estimated_absorpt_t_min 0.874 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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. Restrained distances Cl3-C35 = Cl2-C35 1.78 with sigma of 0.01 Cl2-Cl3 2.89 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(Cl3) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: Cl2(0.125) Cl3(0.125) C35(0.125) H35A(0.125) H35B(0.125) 5.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B) 5.b Aromatic/amide H refined with riding coordinates: C6(H6), C14(H14), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33) 5.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B, H34C) ; _shelx_res_file ; TITL r20200914c_a.res in I2/a r20200914c.res created by SHELXL-2018/3 at 11:02:37 on 16-Sep-2020 REM Old TITL r20200914c in I2/a REM SHELXT solution in I2/a: R1 0.166, Rweak 0.021, Alpha 0.034 REM 0.498 for 266 systematic absences, Orientation as input REM Formula found by SHELXT: C34 N4 O3 I CELL 0.71073 18.1028 14.4854 24.8028 90 101.78 90 ZERR 8 0.0007 0.0005 0.0009 0 0.004 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Cl N O Pd UNIT 273 306 10 24 24 8 DFIX 1.78 0.01 Cl3 C35 Cl2 C35 DFIX 2.89 0.01 Cl2 Cl3 ISOR 0.01 0.02 Cl3 Cl2 C35 L.S. 5 PLAN 20 SIZE 0.19 0.17 0.15 TEMP -160 list 4 conf htab bond $h fmap 2 acta OMIT 0 1 1 OMIT -2 0 2 REM REM REM WGHT 0.030400 13.306300 FVAR 0.19849 PD1 6 0.417394 0.527906 0.290177 11.00000 0.02199 0.01949 = 0.01851 0.00070 0.00695 -0.00053 CL1 3 0.382703 0.418391 0.217418 11.00000 0.04490 0.02775 = 0.02434 -0.00512 0.01267 -0.00519 O1 5 0.357963 0.451793 0.331986 11.00000 0.02613 0.02577 = 0.01865 -0.00240 0.00712 -0.00713 O2 5 0.345165 0.624751 0.729436 11.00000 0.03247 0.05113 = 0.02399 -0.01040 0.01227 -0.01102 O3 5 0.445266 1.045305 0.574340 11.00000 0.03490 0.02113 = 0.03953 -0.00588 0.00956 0.00261 N1 4 0.478073 0.607257 0.243507 11.00000 0.03139 0.02170 = 0.02584 0.00375 0.01404 -0.00025 N2 4 0.456013 0.702570 0.352250 11.00000 0.02696 0.02178 = 0.02114 0.00227 0.00469 -0.00341 N3 4 0.417051 0.599405 0.402485 11.00000 0.01892 0.01753 = 0.02034 -0.00172 0.00431 -0.00157 C1 1 0.533271 0.547798 0.222500 11.00000 0.05183 0.03249 = 0.05517 0.00434 0.03811 0.00262 AFIX 137 H1A 2 0.570681 0.523916 0.253612 11.00000 -1.50000 H1B 2 0.558795 0.584310 0.198484 11.00000 -1.50000 H1C 2 0.506607 0.496098 0.201599 11.00000 -1.50000 AFIX 0 C2 1 0.423511 0.644686 0.194904 11.00000 0.05335 0.02842 = 0.02253 0.00179 0.00719 -0.00446 AFIX 137 H2A 2 0.397557 0.593434 0.173111 11.00000 -1.50000 H2B 2 0.450840 0.681305 0.172097 11.00000 -1.50000 H2C 2 0.386381 0.683847 0.207657 11.00000 -1.50000 AFIX 0 C3 1 0.522032 0.683837 0.275026 11.00000 0.02848 0.03400 = 0.02607 0.00842 0.01013 -0.00551 AFIX 23 H3A 2 0.545100 0.720883 0.249249 11.00000 -1.20000 H3B 2 0.563658 0.656607 0.302576 11.00000 -1.20000 AFIX 0 C4 1 0.477766 0.747932 0.304516 11.00000 0.03746 0.02181 = 0.02310 0.00289 0.00750 -0.01124 AFIX 23 H4A 2 0.508652 0.803164 0.317224 11.00000 -1.20000 H4B 2 0.431747 0.768627 0.278528 11.00000 -1.20000 AFIX 0 C5 1 0.433237 0.613717 0.351363 11.00000 0.01718 0.02251 = 0.02488 0.00551 0.00608 -0.00073 C6 1 0.455562 0.744350 0.401992 11.00000 0.02971 0.01691 = 0.02464 -0.00147 0.00504 -0.00401 AFIX 43 H6 2 0.468965 0.806418 0.411822 11.00000 -1.20000 AFIX 0 C7 1 0.432196 0.679425 0.434254 11.00000 0.02073 0.01790 = 0.02350 -0.00134 0.00338 -0.00060 C8 1 0.420314 0.680162 0.489995 11.00000 0.01928 0.02234 = 0.01934 -0.00216 0.00295 -0.00232 C9 1 0.399637 0.600879 0.512503 11.00000 0.01671 0.02409 = 0.01846 -0.00396 0.00344 -0.00071 C10 1 0.387263 0.514828 0.480349 11.00000 0.01441 0.02128 = 0.01995 -0.00017 0.00357 -0.00009 C11 1 0.389761 0.517533 0.423315 11.00000 0.01411 0.01584 = 0.01943 0.00134 0.00467 -0.00097 C12 1 0.363204 0.445376 0.385795 11.00000 0.01387 0.02256 = 0.01942 -0.00073 0.00428 -0.00146 C13 1 0.337409 0.363245 0.407138 11.00000 0.01528 0.01856 = 0.02175 -0.00330 0.00447 -0.00080 C14 1 0.343921 0.358082 0.464149 11.00000 0.01916 0.01745 = 0.02448 0.00345 0.00751 -0.00023 AFIX 43 H14 2 0.330566 0.301349 0.478837 11.00000 -1.20000 AFIX 0 C15 1 0.368395 0.429312 0.501232 11.00000 0.01769 0.02299 = 0.01977 -0.00042 0.00705 -0.00041 C16 1 0.304231 0.283825 0.368423 11.00000 0.02078 0.02114 = 0.02479 -0.00437 0.00755 -0.00498 C17 1 0.362755 0.247590 0.335839 11.00000 0.02886 0.02348 = 0.02722 -0.00732 0.00983 -0.00158 AFIX 137 H17A 2 0.375781 0.297056 0.312482 11.00000 -1.50000 H17B 2 0.341210 0.195414 0.312737 11.00000 -1.50000 H17C 2 0.408289 0.227383 0.361687 11.00000 -1.50000 AFIX 0 C18 1 0.234347 0.317380 0.326601 11.00000 0.02481 0.03361 = 0.02878 -0.01110 0.00498 -0.00673 AFIX 137 H18A 2 0.249521 0.364773 0.302832 11.00000 -1.50000 H18B 2 0.197545 0.343479 0.346365 11.00000 -1.50000 H18C 2 0.211555 0.265220 0.304023 11.00000 -1.50000 AFIX 0 C19 1 0.279866 0.202034 0.399742 11.00000 0.04189 0.02571 = 0.02998 -0.00582 0.01266 -0.01382 AFIX 137 H19A 2 0.257719 0.154058 0.373513 11.00000 -1.50000 H19B 2 0.242382 0.222718 0.420575 11.00000 -1.50000 H19C 2 0.323893 0.176945 0.425194 11.00000 -1.50000 AFIX 0 C20 1 0.374352 0.405504 0.561807 11.00000 0.03495 0.02074 = 0.02213 0.00046 0.00601 -0.00436 AFIX 137 H20A 2 0.418301 0.436741 0.583922 11.00000 -1.50000 H20B 2 0.380048 0.338587 0.566817 11.00000 -1.50000 H20C 2 0.328539 0.425869 0.573641 11.00000 -1.50000 AFIX 0 C21 1 0.426919 0.773550 0.516690 11.00000 0.02589 0.01939 = 0.02127 -0.00076 0.00434 -0.00223 C22 1 0.495623 0.818756 0.530669 11.00000 0.02567 0.02473 = 0.03179 -0.00256 0.00319 0.00186 AFIX 43 H22 2 0.540348 0.787598 0.526620 11.00000 -1.20000 AFIX 0 C23 1 0.500433 0.908778 0.550498 11.00000 0.02782 0.02155 = 0.03434 -0.00352 0.00507 -0.00288 AFIX 43 H23 2 0.548240 0.938037 0.560506 11.00000 -1.20000 AFIX 0 C24 1 0.435549 0.956012 0.555710 11.00000 0.03146 0.02037 = 0.02033 -0.00023 0.00711 0.00099 C25 1 0.366810 0.911280 0.543072 11.00000 0.02671 0.03010 = 0.04871 -0.01164 0.00821 0.00501 AFIX 43 H25 2 0.322110 0.942276 0.547334 11.00000 -1.20000 AFIX 0 C26 1 0.363203 0.820261 0.523989 11.00000 0.02284 0.03222 = 0.05192 -0.00921 0.00563 -0.00344 AFIX 43 H26 2 0.315753 0.789800 0.515844 11.00000 -1.20000 AFIX 0 C27 1 0.378564 1.097795 0.573119 11.00000 0.04286 0.02327 = 0.04203 -0.00535 0.00943 0.00778 AFIX 137 H27A 2 0.347706 1.097247 0.535734 11.00000 -1.50000 H27B 2 0.392199 1.161541 0.584108 11.00000 -1.50000 H27C 2 0.349820 1.070771 0.598673 11.00000 -1.50000 AFIX 0 C28 1 0.383245 0.607240 0.569515 11.00000 0.02290 0.01723 = 0.02255 -0.00327 0.00513 -0.00204 C29 1 0.442340 0.618542 0.615261 11.00000 0.02026 0.01937 = 0.02484 -0.00058 0.00461 -0.00058 AFIX 43 H29 2 0.492825 0.623219 0.610196 11.00000 -1.20000 AFIX 0 C30 1 0.427577 0.622921 0.667711 11.00000 0.02732 0.02371 = 0.01811 -0.00426 0.00259 0.00007 AFIX 43 H30 2 0.468161 0.629154 0.698517 11.00000 -1.20000 AFIX 0 C31 1 0.353860 0.618293 0.675848 11.00000 0.03039 0.02537 = 0.02272 -0.00643 0.00931 -0.00369 C32 1 0.294880 0.606636 0.631047 11.00000 0.01899 0.03922 = 0.03113 -0.00637 0.01050 -0.00560 AFIX 43 H32 2 0.244410 0.602477 0.636205 11.00000 -1.20000 AFIX 0 C33 1 0.310279 0.601062 0.578315 11.00000 0.01849 0.04093 = 0.02328 -0.00678 0.00047 -0.00403 AFIX 43 H33 2 0.269741 0.592828 0.547678 11.00000 -1.20000 AFIX 0 C34 1 0.271420 0.608776 0.740027 11.00000 0.04189 0.08326 = 0.03715 -0.01881 0.02127 -0.02437 AFIX 137 H34A 2 0.236763 0.656381 0.721635 11.00000 -1.50000 H34B 2 0.273510 0.611149 0.779798 11.00000 -1.50000 H34C 2 0.253487 0.547856 0.725902 11.00000 -1.50000 AFIX 0 CL2 3 0.359847 0.958113 0.358521 10.12500 0.15172 0.12597 = 0.16344 0.00257 0.04504 -0.00885 CL3 3 0.259214 0.816743 0.382868 10.12500 0.14945 0.15283 = 0.14546 0.02095 0.02940 -0.00962 C35 1 0.277229 0.938214 0.385133 10.12500 0.08991 0.08459 = 0.08486 0.00300 0.02013 -0.00363 AFIX 23 H35A 2 0.233859 0.971542 0.362729 10.12500 -1.20000 H35B 2 0.284713 0.960794 0.423540 10.12500 -1.20000 AFIX 0 HKLF 4 REM r20200914c_a.res in I2/a REM wR2 = 0.0900, GooF = S = 1.043, Restrained GooF = 1.042 for all data REM R1 = 0.0402 for 5311 Fo > 4sig(Fo) and 0.0544 for all 6509 data REM 414 parameters refined using 21 restraints END WGHT 0.0304 13.3253 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C1 O2_$1 HTAB C1 Cl1 HTAB C2 Cl1 EQIV $2 -x+1, y+1/2, -z+1/2 HTAB C4 Cl1_$2 EQIV $3 x, -y+3/2, z-1/2 HTAB C4 O2_$3 EQIV $4 -x+1, -y+2, -z+1 HTAB C6 O3_$4 HTAB C23 Cl2_$4 EQIV $5 x, -y+3/2, z+1/2 HTAB C27 Cl1_$5 HTAB C34 Cl2_$5 HTAB C34 Cl3_$5 EQIV $6 -x+1/2, y, -z+1 HTAB C34 O1_$6 REM Highest difference peak 0.569, deepest hole -0.525, 1-sigma level 0.086 Q1 1 0.2516 1.0243 0.3707 11.00000 0.05 0.57 Q2 1 0.4181 0.4189 0.2898 11.00000 0.05 0.50 Q3 1 0.3433 0.4540 0.2150 11.00000 0.05 0.42 Q4 1 0.3281 0.3215 0.3906 11.00000 0.05 0.36 Q5 1 0.4245 0.6589 0.3457 11.00000 0.05 0.35 Q6 1 0.2764 0.5424 0.7895 11.00000 0.05 0.34 Q7 1 0.4113 0.3418 0.4077 11.00000 0.05 0.34 Q8 1 0.3649 0.4229 0.5283 11.00000 0.05 0.33 Q9 1 0.4013 0.5134 0.4516 11.00000 0.05 0.32 Q10 1 0.2848 0.4621 0.2039 11.00000 0.05 0.32 Q11 1 0.4533 0.6187 0.2165 11.00000 0.05 0.32 Q12 1 0.5657 0.6794 0.3317 11.00000 0.05 0.31 Q13 1 0.3775 0.4776 0.4072 11.00000 0.05 0.31 Q14 1 0.2177 0.5774 0.7995 11.00000 0.05 0.31 Q15 1 0.3573 0.3574 0.4294 11.00000 0.05 0.31 Q16 1 0.4704 0.8987 0.4144 11.00000 0.05 0.30 Q17 1 0.2500 0.5202 0.5000 10.50000 0.05 0.30 Q18 1 0.2623 0.6618 0.7698 11.00000 0.05 0.29 Q19 1 0.4893 1.0398 0.5893 11.00000 0.05 0.29 Q20 1 0.3906 0.5972 0.6666 11.00000 0.05 0.29 ; _shelx_res_checksum 1962 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.327 _oxdiff_exptl_absorpt_empirical_full_min 0.793 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -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 0.41739(2) 0.52791(2) 0.29018(2) 0.01960(8) Uani 1 1 d . . . . . Cl1 Cl 0.38270(5) 0.41839(6) 0.21742(3) 0.0315(2) Uani 1 1 d . . . . . O1 O 0.35796(12) 0.45179(15) 0.33199(8) 0.0232(5) Uani 1 1 d . . . . . O2 O 0.34517(13) 0.62475(18) 0.72944(9) 0.0349(6) Uani 1 1 d . . . . . O3 O 0.44527(13) 1.04530(15) 0.57434(10) 0.0316(6) Uani 1 1 d . . . . . N1 N 0.47807(15) 0.60726(18) 0.24351(11) 0.0251(6) Uani 1 1 d . . . . . N2 N 0.45601(14) 0.70257(18) 0.35225(10) 0.0233(6) Uani 1 1 d . . . . . N3 N 0.41705(14) 0.59940(17) 0.40248(10) 0.0189(5) Uani 1 1 d . . . . . C1 C 0.5333(2) 0.5478(3) 0.22250(17) 0.0426(10) Uani 1 1 d . . . . . H1A H 0.570681 0.523916 0.253612 0.064 Uiso 1 1 calc GR . . . . H1B H 0.558795 0.584310 0.198484 0.064 Uiso 1 1 calc GR . . . . H1C H 0.506607 0.496098 0.201599 0.064 Uiso 1 1 calc GR . . . . C2 C 0.4235(2) 0.6447(2) 0.19490(13) 0.0348(9) Uani 1 1 d . . . . . H2A H 0.397557 0.593434 0.173111 0.052 Uiso 1 1 calc GR . . . . H2B H 0.450840 0.681305 0.172097 0.052 Uiso 1 1 calc GR . . . . H2C H 0.386381 0.683847 0.207657 0.052 Uiso 1 1 calc GR . . . . C3 C 0.52203(19) 0.6838(2) 0.27503(13) 0.0289(8) Uani 1 1 d . . . . . H3A H 0.545100 0.720883 0.249249 0.035 Uiso 1 1 calc R . . . . H3B H 0.563658 0.656607 0.302576 0.035 Uiso 1 1 calc R . . . . C4 C 0.4778(2) 0.7479(2) 0.30452(13) 0.0273(8) Uani 1 1 d . . . . . H4A H 0.508652 0.803164 0.317224 0.033 Uiso 1 1 calc R . . . . H4B H 0.431747 0.768627 0.278528 0.033 Uiso 1 1 calc R . . . . C5 C 0.43324(17) 0.6137(2) 0.35136(13) 0.0213(7) Uani 1 1 d . . . . . C6 C 0.45556(18) 0.7444(2) 0.40199(13) 0.0238(7) Uani 1 1 d . . . . . H6 H 0.468965 0.806418 0.411822 0.029 Uiso 1 1 calc R . . . . C7 C 0.43220(17) 0.6794(2) 0.43425(12) 0.0209(7) Uani 1 1 d . . . . . C8 C 0.42031(17) 0.6802(2) 0.49000(12) 0.0205(7) Uani 1 1 d . . . . . C9 C 0.39964(16) 0.6009(2) 0.51250(12) 0.0198(7) Uani 1 1 d . . . . . C10 C 0.38726(16) 0.5148(2) 0.48035(12) 0.0185(6) Uani 1 1 d . . . . . C11 C 0.38976(16) 0.5175(2) 0.42331(12) 0.0163(6) Uani 1 1 d . . . . . C12 C 0.36320(16) 0.4454(2) 0.38580(12) 0.0185(6) Uani 1 1 d . . . . . C13 C 0.33741(16) 0.3632(2) 0.40714(12) 0.0184(6) Uani 1 1 d . . . . . C14 C 0.34392(16) 0.3581(2) 0.46415(12) 0.0199(7) Uani 1 1 d . . . . . H14 H 0.330566 0.301349 0.478837 0.024 Uiso 1 1 calc R . . . . C15 C 0.36840(17) 0.4293(2) 0.50123(12) 0.0197(6) Uani 1 1 d . . . . . C16 C 0.30423(17) 0.2838(2) 0.36842(13) 0.0218(7) Uani 1 1 d . . . . . C17 C 0.36275(18) 0.2476(2) 0.33584(13) 0.0259(7) Uani 1 1 d . . . . . H17A H 0.375781 0.297056 0.312482 0.039 Uiso 1 1 calc GR . . . . H17B H 0.341210 0.195414 0.312737 0.039 Uiso 1 1 calc GR . . . . H17C H 0.408289 0.227383 0.361687 0.039 Uiso 1 1 calc GR . . . . C18 C 0.23435(18) 0.3174(2) 0.32660(13) 0.0291(8) Uani 1 1 d . . . . . H18A H 0.249521 0.364773 0.302832 0.044 Uiso 1 1 calc GR . . . . H18B H 0.197545 0.343479 0.346365 0.044 Uiso 1 1 calc GR . . . . H18C H 0.211555 0.265220 0.304023 0.044 Uiso 1 1 calc GR . . . . C19 C 0.2799(2) 0.2020(2) 0.39974(14) 0.0318(8) Uani 1 1 d . . . . . H19A H 0.257719 0.154058 0.373513 0.048 Uiso 1 1 calc GR . . . . H19B H 0.242382 0.222718 0.420575 0.048 Uiso 1 1 calc GR . . . . H19C H 0.323893 0.176945 0.425194 0.048 Uiso 1 1 calc GR . . . . C20 C 0.37435(19) 0.4055(2) 0.56181(12) 0.0259(7) Uani 1 1 d . . . . . H20A H 0.418301 0.436741 0.583922 0.039 Uiso 1 1 calc GR . . . . H20B H 0.380048 0.338587 0.566817 0.039 Uiso 1 1 calc GR . . . . H20C H 0.328539 0.425869 0.573641 0.039 Uiso 1 1 calc GR . . . . C21 C 0.42692(18) 0.7736(2) 0.51669(12) 0.0223(7) Uani 1 1 d . . . . . C22 C 0.49562(19) 0.8188(2) 0.53067(13) 0.0278(7) Uani 1 1 d . . . . . H22 H 0.540348 0.787598 0.526620 0.033 Uiso 1 1 calc R . . . . C23 C 0.50043(19) 0.9088(2) 0.55050(14) 0.0281(7) Uani 1 1 d . . . . . H23 H 0.548240 0.938037 0.560506 0.034 Uiso 1 1 calc R . . . . C24 C 0.43555(19) 0.9560(2) 0.55571(13) 0.0238(7) Uani 1 1 d . . . . . C25 C 0.3668(2) 0.9113(2) 0.54307(15) 0.0351(9) Uani 1 1 d . . . . . H25 H 0.322110 0.942276 0.547334 0.042 Uiso 1 1 calc R . . . . C26 C 0.3632(2) 0.8203(3) 0.52399(16) 0.0359(9) Uani 1 1 d . . . . . H26 H 0.315753 0.789800 0.515844 0.043 Uiso 1 1 calc R . . . . C27 C 0.3786(2) 1.0978(2) 0.57312(15) 0.0359(9) Uani 1 1 d . . . . . H27A H 0.347706 1.097247 0.535734 0.054 Uiso 1 1 calc GR . . . . H27B H 0.392199 1.161541 0.584108 0.054 Uiso 1 1 calc GR . . . . H27C H 0.349820 1.070771 0.598673 0.054 Uiso 1 1 calc GR . . . . C28 C 0.38325(17) 0.6072(2) 0.56952(12) 0.0208(7) Uani 1 1 d . . . . . C29 C 0.44234(17) 0.6185(2) 0.61526(12) 0.0215(7) Uani 1 1 d . . . . . H29 H 0.492825 0.623219 0.610196 0.026 Uiso 1 1 calc R . . . . C30 C 0.42758(18) 0.6229(2) 0.66771(12) 0.0233(7) Uani 1 1 d . . . . . H30 H 0.468161 0.629154 0.698517 0.028 Uiso 1 1 calc R . . . . C31 C 0.35386(18) 0.6183(2) 0.67585(13) 0.0256(7) Uani 1 1 d . . . . . C32 C 0.29488(18) 0.6066(2) 0.63105(14) 0.0290(8) Uani 1 1 d . . . . . H32 H 0.244410 0.602477 0.636205 0.035 Uiso 1 1 calc R . . . . C33 C 0.31028(18) 0.6011(2) 0.57831(13) 0.0281(8) Uani 1 1 d . . . . . H33 H 0.269741 0.592828 0.547678 0.034 Uiso 1 1 calc R . . . . C34 C 0.2714(2) 0.6088(3) 0.74003(16) 0.0522(12) Uani 1 1 d . . . . . H34A H 0.236763 0.656381 0.721635 0.078 Uiso 1 1 calc GR . . . . H34B H 0.273510 0.611149 0.779798 0.078 Uiso 1 1 calc GR . . . . H34C H 0.253487 0.547856 0.725902 0.078 Uiso 1 1 calc GR . . . . Cl2 Cl 0.3598(10) 0.9581(11) 0.3585(9) 0.145(7) Uani 0.125 1 d D U P . . Cl3 Cl 0.2592(10) 0.8167(12) 0.3829(8) 0.149(7) Uani 0.125 1 d D U P . . C35 C 0.2772(18) 0.9382(14) 0.3851(19) 0.086(14) Uani 0.125 1 d D U P . . H35A H 0.233859 0.971542 0.362729 0.103 Uiso 0.125 1 calc R . P . . H35B H 0.284713 0.960794 0.423540 0.103 Uiso 0.125 1 calc R . P . . 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 0.02199(14) 0.01949(13) 0.01851(13) 0.00070(10) 0.00695(9) -0.00053(10) Cl1 0.0449(5) 0.0277(4) 0.0243(4) -0.0051(3) 0.0127(4) -0.0052(4) O1 0.0261(12) 0.0258(12) 0.0187(11) -0.0024(9) 0.0071(9) -0.0071(10) O2 0.0325(14) 0.0511(16) 0.0240(12) -0.0104(11) 0.0123(10) -0.0110(12) O3 0.0349(14) 0.0211(12) 0.0395(14) -0.0059(10) 0.0096(11) 0.0026(10) N1 0.0314(16) 0.0217(14) 0.0258(15) 0.0037(11) 0.0140(12) -0.0002(12) N2 0.0270(15) 0.0218(14) 0.0211(14) 0.0023(11) 0.0047(11) -0.0034(12) N3 0.0189(13) 0.0175(13) 0.0203(13) -0.0017(10) 0.0043(10) -0.0016(11) C1 0.052(3) 0.032(2) 0.055(3) 0.0043(18) 0.038(2) 0.0026(18) C2 0.053(2) 0.0284(19) 0.0225(18) 0.0018(15) 0.0072(16) -0.0045(17) C3 0.0285(19) 0.034(2) 0.0261(18) 0.0084(15) 0.0101(14) -0.0055(15) C4 0.037(2) 0.0218(17) 0.0231(17) 0.0029(13) 0.0075(14) -0.0112(15) C5 0.0172(16) 0.0225(17) 0.0249(17) 0.0055(13) 0.0061(13) -0.0007(13) C6 0.0297(18) 0.0169(16) 0.0246(17) -0.0015(13) 0.0050(14) -0.0040(14) C7 0.0207(16) 0.0179(16) 0.0235(16) -0.0013(13) 0.0034(13) -0.0006(13) C8 0.0193(16) 0.0223(17) 0.0193(16) -0.0022(13) 0.0029(12) -0.0023(13) C9 0.0167(15) 0.0241(17) 0.0185(16) -0.0040(13) 0.0034(12) -0.0007(13) C10 0.0144(15) 0.0213(16) 0.0200(16) -0.0002(12) 0.0036(12) -0.0001(12) C11 0.0141(15) 0.0158(15) 0.0194(15) 0.0013(12) 0.0047(11) -0.0010(12) C12 0.0139(15) 0.0226(16) 0.0194(16) -0.0007(12) 0.0043(12) -0.0015(12) C13 0.0153(15) 0.0186(16) 0.0218(16) -0.0033(12) 0.0045(12) -0.0008(12) C14 0.0192(16) 0.0174(16) 0.0245(16) 0.0035(13) 0.0075(13) -0.0002(13) C15 0.0177(15) 0.0230(16) 0.0198(16) -0.0004(13) 0.0071(12) -0.0004(13) C16 0.0208(16) 0.0211(17) 0.0248(17) -0.0044(13) 0.0075(13) -0.0050(13) C17 0.0289(18) 0.0235(17) 0.0272(18) -0.0073(14) 0.0098(14) -0.0016(14) C18 0.0248(18) 0.034(2) 0.0288(18) -0.0111(15) 0.0050(14) -0.0067(15) C19 0.042(2) 0.0257(19) 0.0300(19) -0.0058(15) 0.0127(16) -0.0138(16) C20 0.0349(19) 0.0207(17) 0.0221(17) 0.0005(13) 0.0060(14) -0.0044(14) C21 0.0259(18) 0.0194(16) 0.0213(16) -0.0008(13) 0.0043(13) -0.0022(13) C22 0.0257(18) 0.0247(18) 0.0318(19) -0.0026(15) 0.0032(14) 0.0019(14) C23 0.0278(18) 0.0215(17) 0.0343(19) -0.0035(14) 0.0051(15) -0.0029(14) C24 0.0315(18) 0.0204(17) 0.0203(16) -0.0002(13) 0.0071(13) 0.0010(14) C25 0.0267(19) 0.030(2) 0.049(2) -0.0116(17) 0.0082(16) 0.0050(16) C26 0.0228(19) 0.032(2) 0.052(2) -0.0092(17) 0.0056(16) -0.0034(16) C27 0.043(2) 0.0233(19) 0.042(2) -0.0054(16) 0.0094(17) 0.0078(16) C28 0.0229(17) 0.0172(16) 0.0225(16) -0.0033(13) 0.0051(13) -0.0020(13) C29 0.0203(16) 0.0194(16) 0.0248(17) -0.0006(13) 0.0046(13) -0.0006(13) C30 0.0273(18) 0.0237(17) 0.0181(16) -0.0043(13) 0.0026(13) 0.0001(14) C31 0.0304(19) 0.0254(18) 0.0227(17) -0.0064(14) 0.0093(14) -0.0037(14) C32 0.0190(17) 0.039(2) 0.0311(19) -0.0064(16) 0.0105(14) -0.0056(15) C33 0.0185(17) 0.041(2) 0.0233(17) -0.0068(15) 0.0005(13) -0.0040(15) C34 0.042(2) 0.083(3) 0.037(2) -0.019(2) 0.0213(19) -0.024(2) Cl2 0.152(13) 0.126(12) 0.163(13) 0.003(11) 0.045(11) -0.009(10) Cl3 0.149(13) 0.153(13) 0.145(13) 0.021(11) 0.029(11) -0.010(11) C35 0.090(16) 0.085(16) 0.085(16) 0.003(10) 0.020(10) -0.004(10) 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' Cl Cl 0.1484 0.1585 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd1 Cl1 86.48(6) . . ? O1 Pd1 N1 178.16(10) . . ? N1 Pd1 Cl1 91.92(8) . . ? C5 Pd1 Cl1 172.80(9) . . ? C5 Pd1 O1 87.50(11) . . ? C5 Pd1 N1 94.03(11) . . ? C12 O1 Pd1 129.39(19) . . ? C31 O2 C34 117.5(3) . . ? C24 O3 C27 116.5(3) . . ? C1 N1 Pd1 109.9(2) . . ? C1 N1 C2 107.9(3) . . ? C2 N1 Pd1 108.0(2) . . ? C3 N1 Pd1 113.75(19) . . ? C3 N1 C1 106.8(3) . . ? C3 N1 C2 110.3(3) . . ? C5 N2 C4 122.8(3) . . ? C5 N2 C6 112.1(3) . . ? C6 N2 C4 125.1(3) . . ? C5 N3 C7 109.9(2) . . ? C5 N3 C11 128.1(3) . . ? C7 N3 C11 122.0(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 108.4 . . ? N1 C3 H3B 108.4 . . ? N1 C3 C4 115.6(3) . . ? H3A C3 H3B 107.4 . . ? C4 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? N2 C4 C3 111.7(3) . . ? N2 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N2 C5 Pd1 128.3(2) . . ? N2 C5 N3 104.5(3) . . ? N3 C5 Pd1 126.9(2) . . ? N2 C6 H6 126.8 . . ? C7 C6 N2 106.5(3) . . ? C7 C6 H6 126.8 . . ? N3 C7 C8 119.8(3) . . ? C6 C7 N3 106.9(3) . . ? C6 C7 C8 133.3(3) . . ? C7 C8 C21 114.6(3) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 C21 125.7(3) . . ? C8 C9 C10 121.1(3) . . ? C8 C9 C28 117.2(3) . . ? C10 C9 C28 121.5(3) . . ? C11 C10 C9 118.8(3) . . ? C15 C10 C9 124.5(3) . . ? C15 C10 C11 116.6(3) . . ? N3 C11 C10 117.9(3) . . ? C12 C11 N3 118.2(3) . . ? C12 C11 C10 123.8(3) . . ? O1 C12 C11 123.8(3) . . ? O1 C12 C13 118.3(3) . . ? C11 C12 C13 117.8(3) . . ? C12 C13 C16 120.7(3) . . ? C14 C13 C12 117.1(3) . . ? C14 C13 C16 122.2(3) . . ? C13 C14 H14 117.3 . . ? C15 C14 C13 125.3(3) . . ? C15 C14 H14 117.3 . . ? C10 C15 C20 125.9(3) . . ? C14 C15 C10 118.4(3) . . ? C14 C15 C20 115.6(3) . . ? C13 C16 C17 110.9(2) . . ? C13 C16 C18 110.2(3) . . ? C18 C16 C17 108.1(3) . . ? C19 C16 C13 112.2(3) . . ? C19 C16 C17 107.5(3) . . ? C19 C16 C18 107.7(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C8 121.5(3) . . ? C26 C21 C8 120.4(3) . . ? C26 C21 C22 117.8(3) . . ? C21 C22 H22 119.3 . . ? C21 C22 C23 121.3(3) . . ? C23 C22 H22 119.3 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? O3 C24 C23 116.3(3) . . ? O3 C24 C25 124.5(3) . . ? C25 C24 C23 119.2(3) . . ? C24 C25 H25 120.1 . . ? C24 C25 C26 119.8(3) . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 121.6(3) . . ? C21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C9 120.2(3) . . ? C33 C28 C9 121.4(3) . . ? C33 C28 C29 118.4(3) . . ? C28 C29 H29 119.8 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29 119.8 . . ? C29 C30 H30 119.7 . . ? C29 C30 C31 120.7(3) . . ? C31 C30 H30 119.7 . . ? O2 C31 C30 116.1(3) . . ? O2 C31 C32 124.3(3) . . ? C32 C31 C30 119.6(3) . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.4(3) . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 121.6(3) . . ? C28 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Cl2 C35 Cl3 108.0(8) . . ? Cl2 C35 H35A 110.1 . . ? Cl2 C35 H35B 110.1 . . ? Cl3 C35 H35A 110.1 . . ? Cl3 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3885(8) . ? Pd1 O1 1.976(2) . ? Pd1 N1 2.095(3) . ? Pd1 C5 1.937(3) . ? O1 C12 1.322(3) . ? O2 C31 1.373(4) . ? O2 C34 1.431(4) . ? O3 C24 1.373(4) . ? O3 C27 1.422(4) . ? N1 C1 1.491(4) . ? N1 C2 1.496(4) . ? N1 C3 1.490(4) . ? N2 C4 1.476(4) . ? N2 C5 1.350(4) . ? N2 C6 1.376(4) . ? N3 C5 1.374(4) . ? N3 C7 1.397(4) . ? N3 C11 1.422(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.509(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C6 H6 0.9500 . ? C6 C7 1.357(4) . ? C7 C8 1.442(4) . ? C8 C9 1.362(4) . ? C8 C21 1.500(4) . ? C9 C10 1.472(4) . ? C9 C28 1.506(4) . ? C10 C11 1.425(4) . ? C10 C15 1.411(4) . ? C11 C12 1.417(4) . ? C12 C13 1.419(4) . ? C13 C14 1.397(4) . ? C13 C16 1.540(4) . ? C14 H14 0.9500 . ? C14 C15 1.393(4) . ? C15 C20 1.524(4) . ? C16 C17 1.549(4) . ? C16 C18 1.542(4) . ? C16 C19 1.530(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.386(4) . ? C21 C26 1.381(5) . ? C22 H22 0.9500 . ? C22 C23 1.390(4) . ? C23 H23 0.9500 . ? C23 C24 1.388(4) . ? C24 C25 1.381(5) . ? C25 H25 0.9500 . ? C25 C26 1.398(5) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.401(4) . ? C28 C33 1.385(4) . ? C29 H29 0.9500 . ? C29 C30 1.382(4) . ? C30 H30 0.9500 . ? C30 C31 1.391(4) . ? C31 C32 1.385(4) . ? C32 H32 0.9500 . ? C32 C33 1.394(4) . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Cl2 C35 1.777(10) . ? Cl3 C35 1.788(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 O1 C12 C11 27.8(4) . . . . ? Pd1 O1 C12 C13 -155.3(2) . . . . ? Pd1 N1 C3 C4 -53.2(3) . . . . ? O1 C12 C13 C14 179.7(3) . . . . ? O1 C12 C13 C16 0.0(4) . . . . ? O2 C31 C32 C33 179.9(3) . . . . ? O3 C24 C25 C26 179.5(3) . . . . ? N1 C3 C4 N2 71.1(4) . . . . ? N2 C6 C7 N3 -1.4(3) . . . . ? N2 C6 C7 C8 179.8(3) . . . . ? N3 C7 C8 C9 4.7(4) . . . . ? N3 C7 C8 C21 -170.9(3) . . . . ? N3 C11 C12 O1 -4.3(4) . . . . ? N3 C11 C12 C13 178.8(3) . . . . ? C1 N1 C3 C4 -174.6(3) . . . . ? C2 N1 C3 C4 68.4(3) . . . . ? C4 N2 C5 Pd1 -4.0(4) . . . . ? C4 N2 C5 N3 -178.8(3) . . . . ? C4 N2 C6 C7 179.9(3) . . . . ? C5 N2 C4 C3 -39.3(4) . . . . ? C5 N2 C6 C7 0.5(4) . . . . ? C5 N3 C7 C6 1.9(3) . . . . ? C5 N3 C7 C8 -179.2(3) . . . . ? C5 N3 C11 C10 171.2(3) . . . . ? C5 N3 C11 C12 -11.9(4) . . . . ? C6 N2 C4 C3 141.3(3) . . . . ? C6 N2 C5 Pd1 175.4(2) . . . . ? C6 N2 C5 N3 0.6(3) . . . . ? C6 C7 C8 C9 -176.7(3) . . . . ? C6 C7 C8 C21 7.7(5) . . . . ? C7 N3 C5 Pd1 -176.4(2) . . . . ? C7 N3 C5 N2 -1.5(3) . . . . ? C7 N3 C11 C10 -8.0(4) . . . . ? C7 N3 C11 C12 168.9(3) . . . . ? C7 C8 C9 C10 -1.6(4) . . . . ? C7 C8 C9 C28 -176.2(3) . . . . ? C7 C8 C21 C22 -69.1(4) . . . . ? C7 C8 C21 C26 105.6(4) . . . . ? C8 C9 C10 C11 -6.3(4) . . . . ? C8 C9 C10 C15 177.7(3) . . . . ? C8 C9 C28 C29 -73.0(4) . . . . ? C8 C9 C28 C33 107.8(4) . . . . ? C8 C21 C22 C23 173.8(3) . . . . ? C8 C21 C26 C25 -172.8(3) . . . . ? C9 C8 C21 C22 115.5(4) . . . . ? C9 C8 C21 C26 -69.7(4) . . . . ? C9 C10 C11 N3 10.8(4) . . . . ? C9 C10 C11 C12 -165.9(3) . . . . ? C9 C10 C15 C14 167.6(3) . . . . ? C9 C10 C15 C20 -14.3(5) . . . . ? C9 C28 C29 C30 -179.0(3) . . . . ? C9 C28 C33 C32 179.8(3) . . . . ? C10 C9 C28 C29 112.4(3) . . . . ? C10 C9 C28 C33 -66.8(4) . . . . ? C10 C11 C12 O1 172.4(3) . . . . ? C10 C11 C12 C13 -4.4(4) . . . . ? C11 N3 C5 Pd1 4.3(4) . . . . ? C11 N3 C5 N2 179.2(3) . . . . ? C11 N3 C7 C6 -178.7(3) . . . . ? C11 N3 C7 C8 0.2(4) . . . . ? C11 C10 C15 C14 -8.5(4) . . . . ? C11 C10 C15 C20 169.6(3) . . . . ? C11 C12 C13 C14 -3.3(4) . . . . ? C11 C12 C13 C16 177.0(3) . . . . ? C12 C13 C14 C15 5.0(5) . . . . ? C12 C13 C16 C17 59.8(4) . . . . ? C12 C13 C16 C18 -59.9(4) . . . . ? C12 C13 C16 C19 -180.0(3) . . . . ? C13 C14 C15 C10 1.1(5) . . . . ? C13 C14 C15 C20 -177.1(3) . . . . ? C14 C13 C16 C17 -119.9(3) . . . . ? C14 C13 C16 C18 120.4(3) . . . . ? C14 C13 C16 C19 0.4(4) . . . . ? C15 C10 C11 N3 -172.8(3) . . . . ? C15 C10 C11 C12 10.4(4) . . . . ? C16 C13 C14 C15 -175.3(3) . . . . ? C21 C8 C9 C10 173.5(3) . . . . ? C21 C8 C9 C28 -1.1(5) . . . . ? C21 C22 C23 C24 -1.2(5) . . . . ? C22 C21 C26 C25 2.1(5) . . . . ? C22 C23 C24 O3 -178.5(3) . . . . ? C22 C23 C24 C25 2.6(5) . . . . ? C23 C24 C25 C26 -1.6(5) . . . . ? C24 C25 C26 C21 -0.8(6) . . . . ? C26 C21 C22 C23 -1.1(5) . . . . ? C27 O3 C24 C23 172.2(3) . . . . ? C27 O3 C24 C25 -8.8(5) . . . . ? C28 C9 C10 C11 168.1(3) . . . . ? C28 C9 C10 C15 -8.0(5) . . . . ? C28 C29 C30 C31 -1.5(5) . . . . ? C29 C28 C33 C32 0.6(5) . . . . ? C29 C30 C31 O2 -179.0(3) . . . . ? C29 C30 C31 C32 1.8(5) . . . . ? C30 C31 C32 C33 -0.9(5) . . . . ? C31 C32 C33 C28 -0.2(5) . . . . ? C33 C28 C29 C30 0.3(5) . . . . ? C34 O2 C31 C30 -172.4(3) . . . . ? C34 O2 C31 C32 6.8(5) . . . . ?