#------------------------------------------------------------------------------ #$Date: 2021-09-06 15:40:22 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268963 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564311.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_1564311 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_issue 32 _journal_name_full 'Polymer Chemistry' _journal_page_first 4736 _journal_page_last 4747 _journal_paper_doi 10.1039/D1PY00699A _journal_volume 12 _journal_year 2021 _chemical_formula_sum 'C32 H34 Cl N3 O Pd' _chemical_formula_weight 618.47 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-05 deposited with the CCDC. 2021-07-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.14(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.427(3) _cell_length_b 10.938(2) _cell_length_c 19.798(4) _cell_measurement_reflns_used 7981 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 27.8904 _cell_measurement_theta_min 1.6342 _cell_volume 2778.5(11) _computing_cell_refinement crystalclear _computing_data_collection crystalclear _computing_data_reduction crystalclear _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 113(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 32586 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.879 _diffrn_reflns_theta_min 1.634 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.8504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details crystalclear _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description prism _exptl_crystal_F_000 1272 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _refine_diff_density_max 1.204 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 349 _refine_ls_number_reflns 6620 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0375 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.9402P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.0908 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5738 _reflns_number_total 6620 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1py00699a2.cif _cod_data_source_block shelxl _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1564310--1564312.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564311 _shelx_shelxl_version_number 2018/3 _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_min 0.857 _shelx_estimated_absorpt_t_max 0.911 _shelx_res_file ; TITL shelxl in P2(1)/n shelxl.res created by SHELXL-2018/3 at 16:34:42 on 04-Jul-2019 CELL 0.71073 13.4273 10.9381 19.7977 90.000 107.142 90.000 ZERR 4.00 0.0027 0.0022 0.0040 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O Cl Pd UNIT 128 136 12 4 4 4 L.S. 5 ACTA CONF ISOR 0.005 PD1 HTAB SIZE 0.20 0.18 0.12 BOND $H TEMP -160 FMAP 2 PLAN 20 WGHT 0.046500 0.940200 FVAR 0.25902 MOLE 1 PD1 6 0.659938 1.053641 1.056995 11.00000 0.02417 0.01687 = 0.01566 -0.00039 0.00886 -0.00152 CL1 5 0.604736 0.991452 1.155722 11.00000 0.04401 0.02895 = 0.02934 0.00351 0.02301 -0.00432 O1 4 0.724535 0.890097 1.059933 11.00000 0.03221 0.01801 = 0.02570 0.00388 0.01407 0.00260 N1 3 0.765802 1.018292 0.946823 11.00000 0.02507 0.01715 = 0.01416 0.00112 0.00723 0.00282 N2 3 0.660100 1.171321 0.922924 11.00000 0.02732 0.02192 = 0.01570 0.00283 0.00915 0.00715 N3 3 0.595285 1.228560 1.057450 11.00000 0.02549 0.01943 = 0.01958 -0.00182 0.00910 -0.00046 C1 1 0.697593 1.084012 0.971676 11.00000 0.02384 0.01787 = 0.01816 0.00055 0.00688 0.00136 C2 1 0.704326 1.165136 0.868468 11.00000 0.03294 0.02277 = 0.01643 0.00372 0.01012 0.00690 AFIX 43 H2 2 0.690616 1.217609 0.828536 11.00000 -1.20000 AFIX 0 C3 1 0.771606 1.068882 0.883223 11.00000 0.02877 0.01923 = 0.01276 0.00260 0.00709 0.00254 C4 1 0.839671 1.016465 0.847524 11.00000 0.02699 0.02075 = 0.01540 -0.00121 0.00770 0.00171 C5 1 0.826170 1.062667 0.773950 11.00000 0.02690 0.02520 = 0.01672 0.00496 0.01116 0.00780 C6 1 0.860908 1.177923 0.762288 11.00000 0.03313 0.02933 = 0.02619 0.00255 0.01148 0.00263 AFIX 43 H6 2 0.896915 1.227243 0.801353 11.00000 -1.20000 AFIX 0 C7 1 0.843308 1.222197 0.693329 11.00000 0.04500 0.03520 = 0.03692 0.01447 0.02415 0.00636 AFIX 43 H7 2 0.867890 1.301017 0.685898 11.00000 -1.20000 AFIX 0 C8 1 0.790719 1.152177 0.636504 11.00000 0.04113 0.04967 = 0.02220 0.01456 0.01642 0.01715 AFIX 43 H8 2 0.778805 1.182346 0.589792 11.00000 -1.20000 AFIX 0 C9 1 0.755083 1.037244 0.647601 11.00000 0.04629 0.05017 = 0.01677 -0.00071 0.00910 0.00963 AFIX 43 H9 2 0.718543 0.988528 0.608401 11.00000 -1.20000 AFIX 0 C10 1 0.772727 0.992873 0.716207 11.00000 0.04301 0.02774 = 0.01920 0.00075 0.01076 0.00305 AFIX 43 H10 2 0.747876 0.914079 0.723408 11.00000 -1.20000 AFIX 0 C11 1 0.906166 0.926050 0.879332 11.00000 0.02356 0.01807 = 0.01762 -0.00241 0.00763 0.00003 C12 1 0.972928 0.873080 0.838135 11.00000 0.02350 0.02274 = 0.01404 -0.00035 0.00511 0.00523 C13 1 1.053756 0.941975 0.826864 11.00000 0.02681 0.02689 = 0.02372 -0.00487 0.00773 -0.00205 AFIX 43 H13 2 1.068491 1.020948 0.847349 11.00000 -1.20000 AFIX 0 C14 1 1.112981 0.895706 0.785771 11.00000 0.02592 0.03760 = 0.03134 -0.00395 0.01253 -0.00258 AFIX 43 H14 2 1.168462 0.942819 0.778636 11.00000 -1.20000 AFIX 0 C15 1 1.091322 0.780973 0.755156 11.00000 0.02410 0.04102 = 0.02136 -0.00608 0.00738 0.00782 AFIX 43 H15 2 1.131543 0.749508 0.726852 11.00000 -1.20000 AFIX 0 C16 1 1.011031 0.712851 0.766060 11.00000 0.02882 0.02571 = 0.01973 -0.00422 0.00421 0.00621 AFIX 43 H16 2 0.996280 0.634217 0.745117 11.00000 -1.20000 AFIX 0 C17 1 0.951587 0.757452 0.807115 11.00000 0.02444 0.02202 = 0.01992 -0.00015 0.00647 0.00158 AFIX 43 H17 2 0.896455 0.709609 0.814182 11.00000 -1.20000 AFIX 0 C18 1 0.904106 0.875787 0.947983 11.00000 0.02666 0.01818 = 0.01580 -0.00183 0.00523 0.00150 C19 1 0.971550 0.782051 0.984826 11.00000 0.03167 0.02156 = 0.01503 -0.00367 0.00367 0.00550 C20 1 0.946510 0.724927 1.040488 11.00000 0.03802 0.01878 = 0.01895 0.00012 0.00364 0.01010 AFIX 43 H20 2 0.990945 0.660619 1.063893 11.00000 -1.20000 AFIX 0 C21 1 0.862311 0.753517 1.064919 11.00000 0.03771 0.01673 = 0.01603 -0.00065 0.00580 0.00175 C22 1 0.801671 0.857154 1.034725 11.00000 0.02857 0.01625 = 0.01675 -0.00283 0.00483 -0.00096 C23 1 0.826001 0.916212 0.977940 11.00000 0.02605 0.01496 = 0.01433 -0.00224 0.00319 0.00024 C24 1 1.070800 0.741822 0.970276 11.00000 0.03358 0.03161 = 0.02505 0.00125 0.00496 0.01245 AFIX 137 H24A 2 1.118765 0.707922 1.013527 11.00000 -1.50000 H24B 2 1.103433 0.812202 0.954640 11.00000 -1.50000 H24C 2 1.054633 0.679224 0.933214 11.00000 -1.50000 AFIX 0 C25 1 0.834794 0.676514 1.122041 11.00000 0.04615 0.01819 = 0.02175 0.00646 0.00920 0.00373 C26 1 0.723007 0.626178 1.092106 11.00000 0.05587 0.02822 = 0.03406 0.00771 0.00426 -0.01417 AFIX 137 H26A 2 0.705892 0.575365 1.127916 11.00000 -1.50000 H26B 2 0.718429 0.576777 1.050002 11.00000 -1.50000 H26C 2 0.673732 0.694438 1.079395 11.00000 -1.50000 AFIX 0 C27 1 0.908101 0.566840 1.145564 11.00000 0.07490 0.02657 = 0.03648 0.01360 0.02158 0.01560 AFIX 137 H27A 2 0.887676 0.520515 1.181731 11.00000 -1.50000 H27B 2 0.979856 0.596028 1.165164 11.00000 -1.50000 H27C 2 0.903589 0.513934 1.104821 11.00000 -1.50000 AFIX 0 C28 1 0.840282 0.751805 1.188394 11.00000 0.04311 0.02926 = 0.02063 0.00562 0.00935 -0.00087 AFIX 137 H28A 2 0.790880 0.819964 1.175846 11.00000 -1.50000 H28B 2 0.911040 0.783864 1.208337 11.00000 -1.50000 H28C 2 0.822432 0.699699 1.223396 11.00000 -1.50000 AFIX 0 C29 1 0.647295 1.286371 1.126853 11.00000 0.06076 0.02382 = 0.01923 -0.00443 0.01090 -0.00127 AFIX 137 H29A 2 0.617194 1.367468 1.128724 11.00000 -1.50000 H29B 2 0.722055 1.294459 1.132698 11.00000 -1.50000 H29C 2 0.636923 1.235298 1.164891 11.00000 -1.50000 AFIX 0 C30 1 0.482412 1.216278 1.049737 11.00000 0.02931 0.03146 = 0.05304 0.00470 0.02173 0.00320 AFIX 137 H30A 2 0.472948 1.164960 1.087956 11.00000 -1.50000 H30B 2 0.447217 1.178424 1.004067 11.00000 -1.50000 H30C 2 0.452526 1.297338 1.052096 11.00000 -1.50000 AFIX 0 C31 1 0.610154 1.313426 1.002077 11.00000 0.03063 0.01611 = 0.02597 -0.00026 0.01297 0.00230 AFIX 23 H31A 2 0.684088 1.339196 1.015494 11.00000 -1.20000 H31B 2 0.567367 1.387483 1.001106 11.00000 -1.20000 AFIX 0 C32 1 0.581435 1.259133 0.928394 11.00000 0.03179 0.02611 = 0.02140 0.00370 0.00938 0.01363 AFIX 23 H32A 2 0.512874 1.218041 0.917972 11.00000 -1.20000 H32B 2 0.575832 1.325144 0.893254 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelxl in P2(1)/n REM wR2 = 0.0908, GooF = S = 1.081, Restrained GooF = 1.081 for all data REM R1 = 0.0375 for 5738 Fo > 4sig(Fo) and 0.0446 for all 6620 data REM 349 parameters refined using 6 restraints END WGHT 0.0448 0.8456 REM Instructions for potential hydrogen bonds HTAB C29 Cl1 HTAB C30 Cl1 EQIV $1 -x+1, -y+2, -z+2 HTAB C30 O1_$1 HTAB C32 Cl1_$1 REM Highest difference peak 1.204, deepest hole -0.963, 1-sigma level 0.091 Q1 1 0.6599 0.8394 1.0575 11.00000 0.05 1.20 Q2 1 1.0201 1.0541 0.8291 11.00000 0.05 0.92 Q3 1 1.0770 0.9934 0.7321 11.00000 0.05 0.57 Q4 1 0.5985 0.9053 1.1560 11.00000 0.05 0.54 Q5 1 0.7073 0.9866 0.9549 11.00000 0.05 0.40 Q6 1 0.4068 1.1105 0.9367 11.00000 0.05 0.37 Q7 1 0.5772 0.9765 1.0647 11.00000 0.05 0.34 Q8 1 0.6507 0.9035 0.9689 11.00000 0.05 0.34 Q9 1 0.6935 0.9672 1.0097 11.00000 0.05 0.34 Q10 1 0.6550 0.9739 1.1119 11.00000 0.05 0.33 Q11 1 0.5183 0.9527 1.1448 11.00000 0.05 0.33 Q12 1 0.7810 0.9412 0.6108 11.00000 0.05 0.32 Q13 1 0.7204 1.0797 1.0071 11.00000 0.05 0.30 Q14 1 0.6056 1.2774 0.9652 11.00000 0.05 0.30 Q15 1 0.9236 0.8088 0.9586 11.00000 0.05 0.29 Q16 1 0.9436 0.8997 0.8595 11.00000 0.05 0.29 Q17 1 0.8371 1.2076 0.5987 11.00000 0.05 0.29 Q18 1 0.8577 1.0446 0.8290 11.00000 0.05 0.28 Q19 1 0.6074 1.2642 1.0307 11.00000 0.05 0.28 Q20 1 0.8031 0.8812 0.9989 11.00000 0.05 0.28 ; _shelx_res_checksum 63562 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 0.65994(2) 1.05364(2) 1.05699(2) 0.01825(7) Uani 1 1 d . U . . . Cl1 Cl 0.60474(5) 0.99145(6) 1.15572(3) 0.03147(15) Uani 1 1 d . . . . . O1 O 0.72453(13) 0.89010(15) 1.05993(9) 0.0241(4) Uani 1 1 d . . . . . N1 N 0.76580(15) 1.01829(18) 0.94682(10) 0.0185(4) Uani 1 1 d . . . . . N2 N 0.66010(15) 1.17132(18) 0.92292(10) 0.0210(4) Uani 1 1 d . . . . . N3 N 0.59528(15) 1.22856(18) 1.05745(10) 0.0210(4) Uani 1 1 d . . . . . C1 C 0.69759(18) 1.0840(2) 0.97168(12) 0.0198(5) Uani 1 1 d . . . . . C2 C 0.70433(19) 1.1651(2) 0.86847(12) 0.0234(5) Uani 1 1 d . . . . . H2 H 0.690616 1.217609 0.828536 0.028 Uiso 1 1 calc R U . . . C3 C 0.77161(19) 1.0689(2) 0.88322(12) 0.0200(5) Uani 1 1 d . . . . . C4 C 0.83967(19) 1.0165(2) 0.84752(12) 0.0207(5) Uani 1 1 d . . . . . C5 C 0.82617(19) 1.0627(2) 0.77395(12) 0.0219(5) Uani 1 1 d . . . . . C6 C 0.8609(2) 1.1779(2) 0.76229(14) 0.0290(6) Uani 1 1 d . . . . . H6 H 0.896915 1.227243 0.801353 0.035 Uiso 1 1 calc R U . . . C7 C 0.8433(2) 1.2222(3) 0.69333(15) 0.0364(7) Uani 1 1 d . . . . . H7 H 0.867890 1.301017 0.685898 0.044 Uiso 1 1 calc R U . . . C8 C 0.7907(2) 1.1522(3) 0.63650(14) 0.0361(7) Uani 1 1 d . . . . . H8 H 0.778805 1.182346 0.589792 0.043 Uiso 1 1 calc R U . . . C9 C 0.7551(2) 1.0372(3) 0.64760(14) 0.0378(7) Uani 1 1 d . . . . . H9 H 0.718543 0.988528 0.608401 0.045 Uiso 1 1 calc R U . . . C10 C 0.7727(2) 0.9929(3) 0.71621(13) 0.0296(6) Uani 1 1 d . . . . . H10 H 0.747876 0.914079 0.723408 0.036 Uiso 1 1 calc R U . . . C11 C 0.90617(18) 0.9261(2) 0.87933(12) 0.0194(5) Uani 1 1 d . . . . . C12 C 0.97293(18) 0.8731(2) 0.83813(12) 0.0202(5) Uani 1 1 d . . . . . C13 C 1.0538(2) 0.9420(2) 0.82686(13) 0.0257(5) Uani 1 1 d . . . . . H13 H 1.068491 1.020948 0.847349 0.031 Uiso 1 1 calc R U . . . C14 C 1.1130(2) 0.8957(3) 0.78577(14) 0.0307(6) Uani 1 1 d . . . . . H14 H 1.168462 0.942819 0.778636 0.037 Uiso 1 1 calc R U . . . C15 C 1.09132(19) 0.7810(3) 0.75516(13) 0.0287(6) Uani 1 1 d . . . . . H15 H 1.131543 0.749508 0.726852 0.034 Uiso 1 1 calc R U . . . C16 C 1.01103(19) 0.7129(2) 0.76606(12) 0.0254(5) Uani 1 1 d . . . . . H16 H 0.996280 0.634217 0.745117 0.030 Uiso 1 1 calc R U . . . C17 C 0.95159(19) 0.7575(2) 0.80711(12) 0.0221(5) Uani 1 1 d . . . . . H17 H 0.896455 0.709609 0.814182 0.027 Uiso 1 1 calc R U . . . C18 C 0.90411(18) 0.8758(2) 0.94798(12) 0.0204(5) Uani 1 1 d . . . . . C19 C 0.97155(19) 0.7821(2) 0.98483(12) 0.0234(5) Uani 1 1 d . . . . . C20 C 0.9465(2) 0.7249(2) 1.04049(12) 0.0263(5) Uani 1 1 d . . . . . H20 H 0.990945 0.660619 1.063893 0.032 Uiso 1 1 calc R U . . . C21 C 0.8623(2) 0.7535(2) 1.06492(12) 0.0239(5) Uani 1 1 d . . . . . C22 C 0.80167(19) 0.8572(2) 1.03473(12) 0.0209(5) Uani 1 1 d . . . . . C23 C 0.82600(18) 0.9162(2) 0.97794(12) 0.0190(5) Uani 1 1 d . . . . . C24 C 1.0708(2) 0.7418(3) 0.97028(14) 0.0309(6) Uani 1 1 d . . . . . H24A H 1.118765 0.707922 1.013527 0.046 Uiso 1 1 calc R U . . . H24B H 1.103433 0.812202 0.954640 0.046 Uiso 1 1 calc R U . . . H24C H 1.054633 0.679224 0.933214 0.046 Uiso 1 1 calc R U . . . C25 C 0.8348(2) 0.6765(2) 1.12204(13) 0.0289(6) Uani 1 1 d . . . . . C26 C 0.7230(3) 0.6262(3) 1.09211(15) 0.0413(7) Uani 1 1 d . . . . . H26A H 0.705892 0.575365 1.127916 0.062 Uiso 1 1 calc R U . . . H26B H 0.718429 0.576777 1.050002 0.062 Uiso 1 1 calc R U . . . H26C H 0.673732 0.694438 1.079395 0.062 Uiso 1 1 calc R U . . . C27 C 0.9081(3) 0.5668(3) 1.14556(16) 0.0449(8) Uani 1 1 d . . . . . H27A H 0.887676 0.520515 1.181731 0.067 Uiso 1 1 calc R U . . . H27B H 0.979856 0.596028 1.165164 0.067 Uiso 1 1 calc R U . . . H27C H 0.903589 0.513934 1.104821 0.067 Uiso 1 1 calc R U . . . C28 C 0.8403(2) 0.7518(2) 1.18839(13) 0.0310(6) Uani 1 1 d . . . . . H28A H 0.790880 0.819964 1.175846 0.047 Uiso 1 1 calc R U . . . H28B H 0.911040 0.783864 1.208337 0.047 Uiso 1 1 calc R U . . . H28C H 0.822432 0.699699 1.223396 0.047 Uiso 1 1 calc R U . . . C29 C 0.6473(2) 1.2864(2) 1.12685(13) 0.0348(6) Uani 1 1 d . . . . . H29A H 0.617194 1.367468 1.128724 0.052 Uiso 1 1 calc R U . . . H29B H 0.722055 1.294459 1.132698 0.052 Uiso 1 1 calc R U . . . H29C H 0.636923 1.235298 1.164891 0.052 Uiso 1 1 calc R U . . . C30 C 0.4824(2) 1.2163(3) 1.04974(16) 0.0359(6) Uani 1 1 d . . . . . H30A H 0.472948 1.164960 1.087956 0.054 Uiso 1 1 calc R U . . . H30B H 0.447217 1.178424 1.004067 0.054 Uiso 1 1 calc R U . . . H30C H 0.452526 1.297338 1.052096 0.054 Uiso 1 1 calc R U . . . C31 C 0.6102(2) 1.3134(2) 1.00208(12) 0.0232(5) Uani 1 1 d . . . . . H31A H 0.684088 1.339196 1.015494 0.028 Uiso 1 1 calc R U . . . H31B H 0.567367 1.387483 1.001106 0.028 Uiso 1 1 calc R U . . . C32 C 0.5814(2) 1.2591(2) 0.92839(13) 0.0261(5) Uani 1 1 d . . . . . H32A H 0.512874 1.218041 0.917972 0.031 Uiso 1 1 calc R U . . . H32B H 0.575832 1.325144 0.893254 0.031 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02417(11) 0.01687(10) 0.01566(10) -0.00039(6) 0.00886(7) -0.00152(7) Cl1 0.0440(4) 0.0289(3) 0.0293(3) 0.0035(3) 0.0230(3) -0.0043(3) O1 0.0322(9) 0.0180(8) 0.0257(9) 0.0039(7) 0.0141(7) 0.0026(7) N1 0.0251(10) 0.0171(9) 0.0142(9) 0.0011(7) 0.0072(8) 0.0028(8) N2 0.0273(10) 0.0219(10) 0.0157(9) 0.0028(8) 0.0092(8) 0.0072(8) N3 0.0255(10) 0.0194(10) 0.0196(10) -0.0018(8) 0.0091(8) -0.0005(8) C1 0.0238(11) 0.0179(11) 0.0182(11) 0.0006(9) 0.0069(9) 0.0014(9) C2 0.0329(13) 0.0228(12) 0.0164(11) 0.0037(9) 0.0101(10) 0.0069(10) C3 0.0288(12) 0.0192(11) 0.0128(10) 0.0026(8) 0.0071(9) 0.0025(9) C4 0.0270(12) 0.0207(11) 0.0154(11) -0.0012(9) 0.0077(9) 0.0017(10) C5 0.0269(12) 0.0252(12) 0.0167(11) 0.0050(9) 0.0112(9) 0.0078(10) C6 0.0331(14) 0.0293(14) 0.0262(13) 0.0025(11) 0.0115(11) 0.0026(11) C7 0.0450(16) 0.0352(15) 0.0369(16) 0.0145(12) 0.0242(13) 0.0064(13) C8 0.0411(16) 0.0497(18) 0.0222(13) 0.0146(12) 0.0164(12) 0.0171(14) C9 0.0463(17) 0.0502(18) 0.0168(13) -0.0007(12) 0.0091(12) 0.0096(14) C10 0.0430(16) 0.0277(13) 0.0192(12) 0.0007(10) 0.0108(11) 0.0030(12) C11 0.0236(11) 0.0181(11) 0.0176(11) -0.0024(9) 0.0076(9) 0.0000(9) C12 0.0235(11) 0.0227(12) 0.0140(10) -0.0003(9) 0.0051(9) 0.0052(9) C13 0.0268(13) 0.0269(13) 0.0237(13) -0.0049(10) 0.0077(10) -0.0020(10) C14 0.0259(13) 0.0376(15) 0.0313(14) -0.0040(12) 0.0125(11) -0.0026(11) C15 0.0241(12) 0.0410(15) 0.0214(12) -0.0061(11) 0.0074(10) 0.0078(11) C16 0.0288(13) 0.0257(12) 0.0197(12) -0.0042(10) 0.0042(10) 0.0062(10) C17 0.0244(12) 0.0220(12) 0.0199(12) -0.0002(9) 0.0065(9) 0.0016(9) C18 0.0267(12) 0.0182(11) 0.0158(11) -0.0018(9) 0.0052(9) 0.0015(9) C19 0.0317(13) 0.0216(12) 0.0150(11) -0.0037(9) 0.0037(10) 0.0055(10) C20 0.0380(14) 0.0188(11) 0.0190(12) 0.0001(9) 0.0036(10) 0.0101(11) C21 0.0377(14) 0.0167(11) 0.0160(11) -0.0006(9) 0.0058(10) 0.0018(10) C22 0.0286(12) 0.0163(11) 0.0167(11) -0.0028(9) 0.0048(9) -0.0010(9) C23 0.0260(12) 0.0150(10) 0.0143(11) -0.0022(8) 0.0032(9) 0.0002(9) C24 0.0336(14) 0.0316(14) 0.0250(13) 0.0012(11) 0.0050(11) 0.0125(11) C25 0.0462(16) 0.0182(12) 0.0218(12) 0.0065(9) 0.0092(11) 0.0037(11) C26 0.0559(19) 0.0282(15) 0.0341(15) 0.0077(12) 0.0043(14) -0.0142(14) C27 0.075(2) 0.0266(15) 0.0365(17) 0.0136(12) 0.0216(16) 0.0156(14) C28 0.0431(16) 0.0293(14) 0.0206(12) 0.0056(10) 0.0094(11) -0.0009(12) C29 0.0608(19) 0.0238(13) 0.0192(12) -0.0044(10) 0.0109(12) -0.0013(13) C30 0.0293(14) 0.0315(14) 0.0530(18) 0.0047(13) 0.0217(13) 0.0032(11) C31 0.0306(13) 0.0161(11) 0.0260(12) -0.0003(9) 0.0130(10) 0.0023(9) C32 0.0318(13) 0.0261(13) 0.0214(12) 0.0037(10) 0.0094(10) 0.0136(11) 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' O O 0.0106 0.0060 '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' 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 C1 Pd1 O1 87.46(8) . . ? C1 Pd1 N3 93.56(9) . . ? O1 Pd1 N3 177.93(7) . . ? C1 Pd1 Cl1 172.60(7) . . ? O1 Pd1 Cl1 87.57(5) . . ? N3 Pd1 Cl1 91.58(6) . . ? C22 O1 Pd1 128.20(15) . . ? C1 N1 C3 109.73(19) . . ? C1 N1 C23 128.2(2) . . ? C3 N1 C23 122.01(19) . . ? C1 N2 C2 111.72(19) . . ? C1 N2 C32 122.78(19) . . ? C2 N2 C32 125.49(19) . . ? C30 N3 C29 108.7(2) . . ? C30 N3 C31 109.52(19) . . ? C29 N3 C31 106.62(19) . . ? C30 N3 Pd1 109.13(15) . . ? C29 N3 Pd1 108.00(15) . . ? C31 N3 Pd1 114.69(14) . . ? N2 C1 N1 105.32(19) . . ? N2 C1 Pd1 127.66(17) . . ? N1 C1 Pd1 126.99(17) . . ? C3 C2 N2 106.4(2) . . ? C3 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? C2 C3 N1 106.8(2) . . ? C2 C3 C4 133.2(2) . . ? N1 C3 C4 120.0(2) . . ? C11 C4 C3 119.5(2) . . ? C11 C4 C5 124.8(2) . . ? C3 C4 C5 115.6(2) . . ? C10 C5 C6 118.8(2) . . ? C10 C5 C4 120.0(2) . . ? C6 C5 C4 121.1(2) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C5 C10 C9 120.6(3) . . ? C5 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C4 C11 C18 120.8(2) . . ? C4 C11 C12 116.6(2) . . ? C18 C11 C12 122.4(2) . . ? C13 C12 C17 119.2(2) . . ? C13 C12 C11 119.9(2) . . ? C17 C12 C11 120.8(2) . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.6(2) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.9(2) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C12 119.8(2) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C23 C18 C19 116.7(2) . . ? C23 C18 C11 119.1(2) . . ? C19 C18 C11 124.1(2) . . ? C20 C19 C18 117.7(2) . . ? C20 C19 C24 116.9(2) . . ? C18 C19 C24 125.3(2) . . ? C21 C20 C19 125.9(2) . . ? C21 C20 H20 117.1 . . ? C19 C20 H20 117.1 . . ? C20 C21 C22 117.2(2) . . ? C20 C21 C25 121.9(2) . . ? C22 C21 C25 120.9(2) . . ? O1 C22 C23 124.3(2) . . ? O1 C22 C21 118.2(2) . . ? C23 C22 C21 117.4(2) . . ? N1 C23 C22 118.1(2) . . ? N1 C23 C18 117.6(2) . . ? C22 C23 C18 124.2(2) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C27 107.2(2) . . ? C28 C25 C21 112.0(2) . . ? C27 C25 C21 112.3(2) . . ? C28 C25 C26 108.4(2) . . ? C27 C25 C26 107.6(2) . . ? C21 C25 C26 109.3(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 H30A 109.5 . . ? N3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 114.3(2) . . ? N3 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N3 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N2 C32 C31 110.2(2) . . ? N2 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? N2 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? 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 C1 1.929(2) . ? Pd1 O1 1.9814(17) . ? Pd1 N3 2.102(2) . ? Pd1 Cl1 2.3846(8) . ? O1 C22 1.325(3) . ? N1 C1 1.365(3) . ? N1 C3 1.398(3) . ? N1 C23 1.409(3) . ? N2 C1 1.346(3) . ? N2 C2 1.377(3) . ? N2 C32 1.455(3) . ? N3 C30 1.484(3) . ? N3 C29 1.487(3) . ? N3 C31 1.494(3) . ? C2 C3 1.362(3) . ? C2 H2 0.9500 . ? C3 C4 1.430(3) . ? C4 C11 1.357(3) . ? C4 C5 1.501(3) . ? C5 C10 1.386(4) . ? C5 C6 1.387(3) . ? C6 C7 1.401(4) . ? C6 H6 0.9500 . ? C7 C8 1.372(4) . ? C7 H7 0.9500 . ? C8 C9 1.386(4) . ? C8 H8 0.9500 . ? C9 C10 1.395(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C18 1.474(3) . ? C11 C12 1.495(3) . ? C12 C13 1.392(3) . ? C12 C17 1.398(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.419(3) . ? C18 C19 1.419(3) . ? C19 C20 1.391(3) . ? C19 C24 1.510(3) . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C22 1.421(3) . ? C21 C25 1.540(3) . ? C22 C23 1.416(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.534(4) . ? C25 C27 1.534(4) . ? C25 C26 1.544(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.516(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 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 C2 N2 C1 N1 -1.5(3) . . . . ? C32 N2 C1 N1 177.8(2) . . . . ? C2 N2 C1 Pd1 -179.50(18) . . . . ? C32 N2 C1 Pd1 -0.2(3) . . . . ? C3 N1 C1 N2 1.7(3) . . . . ? C23 N1 C1 N2 -179.8(2) . . . . ? C3 N1 C1 Pd1 179.70(17) . . . . ? C23 N1 C1 Pd1 -1.8(4) . . . . ? C1 N2 C2 C3 0.7(3) . . . . ? C32 N2 C2 C3 -178.5(2) . . . . ? N2 C2 C3 N1 0.3(3) . . . . ? N2 C2 C3 C4 180.0(3) . . . . ? C1 N1 C3 C2 -1.3(3) . . . . ? C23 N1 C3 C2 -179.9(2) . . . . ? C1 N1 C3 C4 179.0(2) . . . . ? C23 N1 C3 C4 0.4(3) . . . . ? C2 C3 C4 C11 173.5(3) . . . . ? N1 C3 C4 C11 -6.9(4) . . . . ? C2 C3 C4 C5 -10.2(4) . . . . ? N1 C3 C4 C5 169.4(2) . . . . ? C11 C4 C5 C10 74.2(3) . . . . ? C3 C4 C5 C10 -101.9(3) . . . . ? C11 C4 C5 C6 -109.7(3) . . . . ? C3 C4 C5 C6 74.2(3) . . . . ? C10 C5 C6 C7 -0.8(4) . . . . ? C4 C5 C6 C7 -176.9(2) . . . . ? C5 C6 C7 C8 0.5(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 -0.1(4) . . . . ? C6 C5 C10 C9 0.6(4) . . . . ? C4 C5 C10 C9 176.8(2) . . . . ? C8 C9 C10 C5 -0.2(4) . . . . ? C3 C4 C11 C18 4.1(4) . . . . ? C5 C4 C11 C18 -171.9(2) . . . . ? C3 C4 C11 C12 178.3(2) . . . . ? C5 C4 C11 C12 2.4(4) . . . . ? C4 C11 C12 C13 70.8(3) . . . . ? C18 C11 C12 C13 -115.1(3) . . . . ? C4 C11 C12 C17 -105.5(3) . . . . ? C18 C11 C12 C17 68.7(3) . . . . ? C17 C12 C13 C14 -0.6(4) . . . . ? C11 C12 C13 C14 -176.9(2) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C12 0.0(4) . . . . ? C13 C12 C17 C16 0.3(3) . . . . ? C11 C12 C17 C16 176.6(2) . . . . ? C4 C11 C18 C23 5.0(3) . . . . ? C12 C11 C18 C23 -168.9(2) . . . . ? C4 C11 C18 C19 -179.5(2) . . . . ? C12 C11 C18 C19 6.6(4) . . . . ? C23 C18 C19 C20 9.5(3) . . . . ? C11 C18 C19 C20 -166.1(2) . . . . ? C23 C18 C19 C24 -168.2(2) . . . . ? C11 C18 C19 C24 16.1(4) . . . . ? C18 C19 C20 C21 -1.9(4) . . . . ? C24 C19 C20 C21 176.1(2) . . . . ? C19 C20 C21 C22 -6.0(4) . . . . ? C19 C20 C21 C25 173.7(2) . . . . ? Pd1 O1 C22 C23 -26.2(3) . . . . ? Pd1 O1 C22 C21 155.86(16) . . . . ? C20 C21 C22 O1 -176.4(2) . . . . ? C25 C21 C22 O1 3.9(3) . . . . ? C20 C21 C22 C23 5.5(3) . . . . ? C25 C21 C22 C23 -174.2(2) . . . . ? C1 N1 C23 C22 13.2(4) . . . . ? C3 N1 C23 C22 -168.5(2) . . . . ? C1 N1 C23 C18 -169.8(2) . . . . ? C3 N1 C23 C18 8.6(3) . . . . ? O1 C22 C23 N1 1.3(3) . . . . ? C21 C22 C23 N1 179.3(2) . . . . ? O1 C22 C23 C18 -175.6(2) . . . . ? C21 C22 C23 C18 2.4(3) . . . . ? C19 C18 C23 N1 173.0(2) . . . . ? C11 C18 C23 N1 -11.1(3) . . . . ? C19 C18 C23 C22 -10.1(3) . . . . ? C11 C18 C23 C22 165.8(2) . . . . ? C20 C21 C25 C28 119.1(3) . . . . ? C22 C21 C25 C28 -61.2(3) . . . . ? C20 C21 C25 C27 -1.5(4) . . . . ? C22 C21 C25 C27 178.2(2) . . . . ? C20 C21 C25 C26 -120.8(3) . . . . ? C22 C21 C25 C26 58.9(3) . . . . ? C30 N3 C31 C32 -74.2(3) . . . . ? C29 N3 C31 C32 168.4(2) . . . . ? Pd1 N3 C31 C32 48.9(2) . . . . ? C1 N2 C32 C31 47.3(3) . . . . ? C2 N2 C32 C31 -133.5(2) . . . . ? N3 C31 C32 N2 -73.6(3) . . . . ?