#------------------------------------------------------------------------------ #$Date: 2024-07-17 04:57:21 +0300 (Wed, 17 Jul 2024) $ #$Revision: 293436 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572135.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1572135 loop_ _publ_author_name 'Anzaldo, Bertin' 'Guti\'errez P\'erez, Ren\'e' 'Hern\'andez T\'ellez, Guadalupe' 'Mendoza, \'Angel' 'Moreno Morales, Gloria E.' _publ_section_title ; Bis{(S)-(−)-N-[(2-biphenyl)methylidene]-1-(4-methoxyphenyl)ethylamine-\kN}dichloridopalladium(II) ; _journal_coeditor_code BX4025 _journal_issue 7 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624005558 _journal_volume 9 _journal_year 2024 _chemical_absolute_configuration syn _chemical_formula_iupac '[Pd Cl2 (C22 H21 N1 O1)2]' _chemical_formula_moiety 'C44 H42 Cl2 N2 O2 Pd' _chemical_formula_sum 'C44 H42 Cl2 N2 O2 Pd' _chemical_formula_weight 808.09 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 96.388(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.2505(4) _cell_length_b 18.6165(9) _cell_length_c 10.6345(5) _cell_measurement_reflns_used 5972 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.6430 _cell_measurement_theta_min 3.3860 _cell_volume 2016.77(16) _computing_cell_refinement ; CrysAlisPro (Agilent, 2013) ; _computing_data_collection ; CrysAlisPro (Agilent, 2013) ; _computing_data_reduction ; CrysAlisPro (Agilent, 2013) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015) ; _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.5564 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.912 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 25419 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.119 _diffrn_reflns_theta_min 2.916 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.938 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (CrysAlisPro; Agilent, 2013) ; _exptl_crystal_colour 'clear gold' _exptl_crystal_density_diffrn 1.331 _exptl_crystal_description prism _exptl_crystal_F_000 832 _exptl_crystal_size_max 0.2687 _exptl_crystal_size_mid 0.1447 _exptl_crystal_size_min 0.0883 _refine_diff_density_max 0.527 _refine_diff_density_min -0.302 _refine_ls_abs_structure_details ; Flack x determined using 2435 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 464 _refine_ls_number_reflns 10009 _refine_ls_number_restraints 108 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0405 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.0766 _reflns_number_gt 6673 _reflns_number_total 10009 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL IMDIBBPd_1_Mo in P21 #4 imdibbpd_1_mo.res created by SHELXL-2019/3 at 23:16:39 on 09-Jul-2024 REM reset to P21 #4 CELL 0.71073 10.250491 18.616525 10.634517 90 96.3884 90 ZERR 2 0.000421 0.000852 0.000498 0 0.0042 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O Pd UNIT 88 84 4 4 4 2 EQIV $1 1-X,-0.5+Y,1-Z EQIV $2 -X,0.5+Y,2-Z SIMU 0.04 0.08 1.7 C9 C4 C5 C6 C7 C8 C10 C15 C14 C13 C12 C11 DELU C6 C5 C4 C9 C8 C7 C10 C15 C14 C13 C12 C11 L.S. 50 PLAN 20 CONF HTAB C3 Cl1 HTAB C22 Cl1_$1 HTAB C25 Cl2 HTAB C44 Cl2_$2 LIST 4 BOND HTAB more -1 bond $H fmap 2 acta OMIT -10 -16 6 OMIT -9 4 3 REM REM REM WGHT 0.024600 FVAR 1.11813 PD1 6 0.248592 0.406479 0.751114 11.00000 0.03554 0.04656 = 0.03469 -0.00068 0.00435 -0.00173 CL1 3 0.437206 0.475381 0.768405 11.00000 0.04334 0.06678 = 0.07277 -0.01302 0.01392 -0.01159 CL2 3 0.058588 0.338391 0.724134 11.00000 0.04042 0.05807 = 0.06703 -0.01179 0.00807 -0.00821 O1 5 0.171856 0.048627 0.370233 11.00000 0.06539 0.08053 = 0.15548 -0.05020 0.01302 0.00047 O2 5 0.318356 0.764776 1.116858 11.00000 0.07125 0.06315 = 0.11219 -0.03419 0.01509 -0.00768 N1 4 0.349903 0.316566 0.720740 11.00000 0.03021 0.04828 = 0.03645 0.00312 -0.00028 -0.00414 N2 4 0.140382 0.495739 0.770823 11.00000 0.04131 0.04608 = 0.03152 -0.00151 0.00650 0.00098 C1 1 0.379539 0.269674 0.801407 11.00000 0.04788 0.06487 = 0.04503 -0.00882 0.01657 0.00186 AFIX 43 H1 2 0.416918 0.227848 0.773721 11.00000 -1.20000 AFIX 0 C2 1 0.384383 0.306205 0.588553 11.00000 0.05532 0.05249 = 0.03957 -0.00050 0.01612 -0.00319 AFIX 13 H2 2 0.336977 0.343456 0.536804 11.00000 -1.20000 AFIX 0 C3 1 0.528772 0.320809 0.584146 11.00000 0.07794 0.08479 = 0.08054 -0.02325 0.04360 -0.02919 AFIX 137 H3A 2 0.548930 0.368729 0.613494 11.00000 -1.50000 H3B 2 0.549528 0.315922 0.498733 11.00000 -1.50000 H3C 2 0.579616 0.287057 0.637410 11.00000 -1.50000 AFIX 0 C4 1 0.361647 0.273367 0.936701 11.00000 0.04851 0.08787 = 0.04465 0.01699 0.01291 0.02162 C5 1 0.399578 0.334487 1.004899 11.00000 0.07415 0.12323 = 0.04426 -0.00175 -0.00237 0.03087 AFIX 43 H5 2 0.431888 0.373415 0.963132 11.00000 -1.20000 AFIX 0 C6 1 0.390903 0.339465 1.133414 11.00000 0.09274 0.19444 = 0.05590 -0.00258 0.00001 0.04339 AFIX 43 H6 2 0.414431 0.381245 1.178252 11.00000 -1.20000 AFIX 0 C7 1 0.345414 0.279224 1.192872 11.00000 0.10386 0.27810 = 0.03956 0.02150 0.00197 0.02189 AFIX 43 H7 2 0.340691 0.280884 1.279651 11.00000 -1.20000 AFIX 0 C8 1 0.308559 0.219562 1.130474 11.00000 0.08027 0.23023 = 0.06175 0.07129 0.01092 0.00195 AFIX 43 H8 2 0.276143 0.181801 1.175099 11.00000 -1.20000 AFIX 0 C9 1 0.316148 0.210602 0.999649 11.00000 0.04693 0.14169 = 0.05906 0.04561 0.01257 0.01616 C10 1 0.278211 0.145343 0.935294 11.00000 0.05281 0.10169 = 0.11629 0.06173 0.03078 0.00616 C11 1 0.323809 0.076942 0.982595 11.00000 0.07543 0.12742 = 0.19859 0.11249 0.01758 0.00835 AFIX 43 H11 2 0.379967 0.074179 1.057397 11.00000 -1.20000 AFIX 0 C12 1 0.285830 0.016390 0.919332 11.00000 0.13641 0.09962 = 0.27300 0.11262 0.03194 0.02135 AFIX 43 H12 2 0.320193 -0.027287 0.949817 11.00000 -1.20000 AFIX 0 C13 1 0.199706 0.016614 0.813245 11.00000 0.12268 0.08866 = 0.24928 0.05672 0.04319 -0.00957 AFIX 43 H13 2 0.170297 -0.026383 0.775614 11.00000 -1.20000 AFIX 0 C14 1 0.156051 0.081461 0.761580 11.00000 0.09751 0.07585 = 0.13767 0.02732 0.03009 -0.00523 AFIX 43 H14 2 0.101062 0.082413 0.685895 11.00000 -1.20000 AFIX 0 C15 1 0.192853 0.143069 0.820412 11.00000 0.06581 0.08144 = 0.09641 0.02606 0.02786 -0.00288 AFIX 43 H15 2 0.161244 0.186121 0.784604 11.00000 -1.20000 AFIX 0 C16 1 0.337347 0.236400 0.534040 11.00000 0.04198 0.04770 = 0.04122 -0.00217 0.01312 0.00335 C17 1 0.205110 0.228101 0.493308 11.00000 0.04032 0.06190 = 0.08146 -0.02078 0.00652 0.00976 AFIX 43 H17 2 0.148723 0.266325 0.503160 11.00000 -1.20000 AFIX 0 C18 1 0.153502 0.165704 0.438853 11.00000 0.05282 0.08108 = 0.11534 -0.03913 0.00813 0.00326 AFIX 43 H18 2 0.064439 0.162442 0.410954 11.00000 -1.20000 AFIX 0 C19 1 0.234651 0.108839 0.426410 11.00000 0.05392 0.05277 = 0.08047 -0.01532 0.01382 -0.00584 C20 1 0.362844 0.112801 0.465795 11.00000 0.06024 0.06134 = 0.08699 -0.01170 0.01062 0.02324 AFIX 43 H20 2 0.416800 0.073219 0.458349 11.00000 -1.20000 AFIX 0 C21 1 0.415018 0.176368 0.517906 11.00000 0.04052 0.07245 = 0.07461 -0.00631 0.00494 0.00558 AFIX 43 H21 2 0.504769 0.178980 0.542875 11.00000 -1.20000 AFIX 0 C22 1 0.240705 -0.014452 0.369711 11.00000 0.09090 0.05888 = 0.18662 -0.03440 0.01610 0.01823 AFIX 137 H22A 2 0.304857 -0.010854 0.310764 11.00000 -1.50000 H22B 2 0.181398 -0.053147 0.345099 11.00000 -1.50000 H22C 2 0.284092 -0.023545 0.452904 11.00000 -1.50000 AFIX 0 C23 1 0.123747 0.545200 0.684359 11.00000 0.03429 0.04547 = 0.05135 0.01404 -0.00017 0.00127 AFIX 43 H23 2 0.085283 0.588047 0.706001 11.00000 -1.20000 AFIX 0 C24 1 0.084529 0.513066 0.893060 11.00000 0.04348 0.05910 = 0.03475 -0.00259 0.01088 -0.00594 AFIX 13 H24 2 -0.009558 0.521867 0.871482 11.00000 -1.20000 AFIX 0 C25 1 0.097101 0.451404 0.983884 11.00000 0.08660 0.06257 = 0.04637 -0.00380 0.02140 -0.01438 AFIX 137 H25A 2 0.052401 0.410297 0.945365 11.00000 -1.50000 H25B 2 0.058729 0.464220 1.059108 11.00000 -1.50000 H25C 2 0.188238 0.440139 1.005443 11.00000 -1.50000 AFIX 0 C26 1 0.160992 0.538991 0.554097 11.00000 0.04335 0.07976 = 0.02983 0.00834 -0.00194 -0.00624 C27 1 0.142633 0.473806 0.488488 11.00000 0.07532 0.07190 = 0.03838 0.00155 -0.00241 -0.00275 AFIX 43 H27 2 0.111914 0.433438 0.527477 11.00000 -1.20000 AFIX 0 C28 1 0.171225 0.470846 0.364431 11.00000 0.11466 0.10270 = 0.03745 -0.01694 0.00433 -0.00710 AFIX 43 H28 2 0.158934 0.428004 0.319704 11.00000 -1.20000 AFIX 0 C29 1 0.216575 0.528927 0.307198 11.00000 0.12078 0.16137 = 0.03225 -0.00729 0.01548 -0.02357 AFIX 43 H29 2 0.237239 0.525665 0.224424 11.00000 -1.20000 AFIX 0 C30 1 0.232427 0.593924 0.372435 11.00000 0.09272 0.11559 = 0.04210 0.00377 0.00598 -0.02946 AFIX 43 H30 2 0.262654 0.634092 0.332495 11.00000 -1.20000 AFIX 0 C31 1 0.203590 0.599016 0.495704 11.00000 0.05256 0.07640 = 0.04434 0.00884 -0.00004 -0.00325 C32 1 0.221577 0.670185 0.563897 11.00000 0.04259 0.07525 = 0.05207 0.02309 0.00803 -0.00498 C33 1 0.162727 0.729969 0.507904 11.00000 0.06364 0.08545 = 0.08757 0.03096 0.00452 -0.02126 AFIX 43 H33 2 0.113274 0.725890 0.429438 11.00000 -1.20000 AFIX 0 C34 1 0.175849 0.796153 0.566377 11.00000 0.07649 0.08040 = 0.13181 0.04962 0.00531 -0.00148 AFIX 43 H34 2 0.138444 0.837068 0.527241 11.00000 -1.20000 AFIX 0 C35 1 0.246514 0.799829 0.685297 11.00000 0.10122 0.05878 = 0.12394 -0.00236 0.03694 -0.01411 AFIX 43 H35 2 0.251564 0.843407 0.728319 11.00000 -1.20000 AFIX 0 C36 1 0.307840 0.742165 0.740001 11.00000 0.08647 0.08544 = 0.07750 0.00107 0.02069 -0.01538 AFIX 43 H36 2 0.358637 0.746573 0.817702 11.00000 -1.20000 AFIX 0 C37 1 0.294794 0.675234 0.679194 11.00000 0.06267 0.06911 = 0.05682 0.01699 0.00795 -0.00059 AFIX 43 H37 2 0.335477 0.634764 0.716872 11.00000 -1.20000 AFIX 0 C38 1 0.144266 0.582723 0.950785 11.00000 0.04353 0.05629 = 0.03618 -0.00069 0.01180 0.00157 C39 1 0.066410 0.638786 0.972256 11.00000 0.04717 0.05517 = 0.06249 -0.01020 0.01535 -0.00251 AFIX 43 H39 2 -0.023526 0.635579 0.948671 11.00000 -1.20000 AFIX 0 C40 1 0.119172 0.702116 1.029839 11.00000 0.05589 0.05102 = 0.08259 -0.01720 0.02302 0.00178 AFIX 43 H40 2 0.064808 0.740340 1.045416 11.00000 -1.20000 AFIX 0 C41 1 0.253858 0.706426 1.062921 11.00000 0.06032 0.06369 = 0.06097 -0.01752 0.02299 -0.00874 C42 1 0.330967 0.647409 1.045305 11.00000 0.04062 0.06967 = 0.05976 -0.02160 0.00949 -0.00923 AFIX 43 H42 2 0.420553 0.648662 1.071609 11.00000 -1.20000 AFIX 0 C43 1 0.275659 0.587241 0.989276 11.00000 0.05400 0.06005 = 0.04880 -0.01048 0.01255 0.00376 AFIX 43 H43 2 0.328990 0.548042 0.976853 11.00000 -1.20000 AFIX 0 C44 1 0.248486 0.830696 1.113571 11.00000 0.09483 0.06053 = 0.12163 -0.01762 0.03536 -0.00746 AFIX 137 H44A 2 0.210510 0.840209 1.028576 11.00000 -1.50000 H44B 2 0.307576 0.868873 1.141785 11.00000 -1.50000 H44C 2 0.180116 0.827590 1.168128 11.00000 -1.50000 AFIX 0 HKLF 4 REM IMDIBBPd_1_Mo in P21 #4 REM wR2 = 0.0766, GooF = S = 1.021, Restrained GooF = 1.019 for all data REM R1 = 0.0405 for 6673 Fo > 4sig(Fo) and 0.0810 for all 10009 data REM 464 parameters refined using 108 restraints END WGHT 0.0246 0.0000 REM Instructions for potential hydrogen bonds HTAB C3 Cl1 HTAB C22 Cl1_$1 HTAB C25 Cl2 HTAB C44 Cl2_$2 REM Highest difference peak 0.527, deepest hole -0.302, 1-sigma level 0.056 Q1 1 0.4414 0.3369 0.7745 11.00000 0.05 0.53 Q2 1 0.0600 0.4760 0.7290 11.00000 0.05 0.45 Q3 1 0.0662 0.3760 0.6766 11.00000 0.05 0.32 Q4 1 0.4321 0.4377 0.8263 11.00000 0.05 0.30 Q5 1 0.2598 0.4091 0.6464 11.00000 0.05 0.29 Q6 1 0.1625 0.4082 0.6887 11.00000 0.05 0.29 Q7 1 0.2368 0.4027 0.8486 11.00000 0.05 0.29 Q8 1 0.3225 0.3498 0.7590 11.00000 0.05 0.27 Q9 1 0.3403 0.4030 0.8137 11.00000 0.05 0.26 Q10 1 0.1819 0.4617 0.7374 11.00000 0.05 0.25 Q11 1 0.1184 0.6177 0.9400 11.00000 0.05 0.25 Q12 1 0.3840 0.4705 0.8417 11.00000 0.05 0.24 Q13 1 0.1029 0.3686 0.7726 11.00000 0.05 0.24 Q14 1 0.1874 0.1245 0.4798 11.00000 0.05 0.24 Q15 1 0.3634 0.5031 0.7326 11.00000 0.05 0.24 Q16 1 0.3116 0.6897 1.0213 11.00000 0.05 0.23 Q17 1 0.1210 0.3406 0.6644 11.00000 0.05 0.23 Q18 1 0.4219 0.3173 0.6706 11.00000 0.05 0.23 Q19 1 0.1417 0.5816 1.0043 11.00000 0.05 0.22 Q20 1 0.1416 -0.0421 0.2968 11.00000 0.05 0.22 REM The information below was added by Olex2. REM REM R1 = 0.0405 for 6673 Fo > 4sig(Fo) and 0.0810 for all 25456 data REM 464 parameters refined using n/a restraints REM Highest difference peak 0.53, deepest hole -0.30 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0810 REM R1_gt = 0.0405 REM wR_ref = 0.0766 REM GOOF = 1.021 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 25456 REM Reflections_gt = 6673 REM Parameters = 464 REM Hole = -0.30 REM Peak = 0.53 REM Flack = 0.00(3) ; _cod_data_source_file bx4025.cif _cod_data_source_block I _cod_database_code 1572135 _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd1 0.24859(6) 0.40648(10) 0.75111(6) 0.03890(9) Uani d 1 . . Cl Cl1 0.43721(19) 0.47538(12) 0.7684(2) 0.0604(6) Uani d 1 . . Cl Cl2 0.05859(18) 0.33839(10) 0.7241(2) 0.0550(6) Uani d 1 . . O O1 0.1719(6) 0.0486(4) 0.3702(8) 0.100(3) Uani d 1 . . O O2 0.3184(6) 0.7648(4) 1.1169(7) 0.082(2) Uani d 1 . . N N1 0.3499(5) 0.3166(3) 0.7207(6) 0.0386(16) Uani d 1 . . N N2 0.1404(6) 0.4957(3) 0.7708(6) 0.0395(16) Uani d 1 . . C C1 0.3795(7) 0.2697(5) 0.8014(7) 0.052(2) Uani d 1 . . H H1 0.416918 0.227848 0.773721 0.062 Uiso calc 1 . . C C2 0.3844(7) 0.3062(4) 0.5886(7) 0.0483(18) Uani d 1 . . H H2 0.336977 0.343456 0.536804 0.058 Uiso calc 1 . . C C3 0.5288(6) 0.3208(3) 0.5841(6) 0.0785(19) Uani d 1 . . H H3A 0.548930 0.368729 0.613494 0.118 Uiso calc 1 . . H H3B 0.549528 0.315922 0.498733 0.118 Uiso calc 1 . . H H3C 0.579616 0.287057 0.637410 0.118 Uiso calc 1 . . C C4 0.3616(7) 0.2734(6) 0.9367(8) 0.060(2) Uani d 1 . . C C5 0.3996(7) 0.3345(6) 1.0049(8) 0.081(2) Uani d 1 . . H H5 0.431888 0.373415 0.963132 0.097 Uiso calc 1 . . C C6 0.3909(8) 0.3395(7) 1.1334(9) 0.115(3) Uani d 1 . . H H6 0.414431 0.381245 1.178252 0.138 Uiso calc 1 . . C C7 0.3454(11) 0.2792(10) 1.1929(10) 0.141(5) Uani d 1 . . H H7 0.340691 0.280884 1.279651 0.169 Uiso calc 1 . . C C8 0.3086(10) 0.2196(9) 1.1305(11) 0.124(4) Uani d 1 . . H H8 0.276143 0.181801 1.175099 0.149 Uiso calc 1 . . C C9 0.3161(11) 0.2106(8) 0.9996(11) 0.082(3) Uani d 1 . . C C10 0.2782(10) 0.1453(7) 0.9353(13) 0.089(3) Uani d 1 . . C C11 0.3238(11) 0.0769(8) 0.9826(14) 0.134(5) Uani d 1 . . H H11 0.379967 0.074179 1.057397 0.160 Uiso calc 1 . . C C12 0.2858(15) 0.0164(8) 0.9193(18) 0.169(6) Uani d 1 . . H H12 0.320193 -0.027287 0.949817 0.203 Uiso calc 1 . . C C13 0.1997(12) 0.0166(8) 0.8132(17) 0.152(5) Uani d 1 . . H H13 0.170297 -0.026383 0.775614 0.182 Uiso calc 1 . . C C14 0.1561(10) 0.0815(6) 0.7616(12) 0.102(3) Uani d 1 . . H H14 0.101062 0.082413 0.685895 0.123 Uiso calc 1 . . C C15 0.1929(10) 0.1431(6) 0.8204(11) 0.080(3) Uani d 1 . . H H15 0.161244 0.186121 0.784604 0.096 Uiso calc 1 . . C C16 0.3373(7) 0.2364(4) 0.5340(7) 0.0430(18) Uani d 1 . . C C17 0.2051(9) 0.2281(6) 0.4933(10) 0.061(3) Uani d 1 . . H H17 0.148723 0.266325 0.503160 0.073 Uiso calc 1 . . C C18 0.1535(9) 0.1657(6) 0.4389(11) 0.083(3) Uani d 1 . . H H18 0.064439 0.162442 0.410954 0.100 Uiso calc 1 . . C C19 0.2347(9) 0.1088(5) 0.4264(10) 0.062(3) Uani d 1 . . C C20 0.3628(9) 0.1128(5) 0.4658(9) 0.069(3) Uani d 1 . . H H20 0.416800 0.073219 0.458349 0.083 Uiso calc 1 . . C C21 0.4150(8) 0.1764(5) 0.5179(9) 0.063(3) Uani d 1 . . H H21 0.504769 0.178980 0.542875 0.075 Uiso calc 1 . . C C22 0.2407(10) -0.0145(6) 0.3697(13) 0.112(4) Uani d 1 . . H H22A 0.304857 -0.010854 0.310764 0.168 Uiso calc 1 . . H H22B 0.181398 -0.053147 0.345099 0.168 Uiso calc 1 . . H H22C 0.284092 -0.023545 0.452904 0.168 Uiso calc 1 . . C C23 0.1237(6) 0.5452(4) 0.6844(7) 0.0441(19) Uani d 1 . . H H23 0.085283 0.588047 0.706001 0.053 Uiso calc 1 . . C C24 0.0845(7) 0.5131(4) 0.8931(6) 0.0453(17) Uani d 1 . . H H24 -0.009558 0.521867 0.871482 0.054 Uiso calc 1 . . C C25 0.0971(6) 0.4514(3) 0.9839(5) 0.0641(15) Uani d 1 . . H H25A 0.052401 0.410297 0.945365 0.096 Uiso calc 1 . . H H25B 0.058729 0.464220 1.059108 0.096 Uiso calc 1 . . H H25C 0.188238 0.440139 1.005443 0.096 Uiso calc 1 . . C C26 0.1610(7) 0.5390(5) 0.5541(7) 0.051(2) Uani d 1 . . C C27 0.1426(7) 0.4738(5) 0.4885(7) 0.0625(19) Uani d 1 . . H H27 0.111914 0.433438 0.527477 0.075 Uiso calc 1 . . C C28 0.1712(8) 0.4708(5) 0.3644(7) 0.085(2) Uani d 1 . . H H28 0.158934 0.428004 0.319704 0.102 Uiso calc 1 . . C C29 0.2166(8) 0.5289(7) 0.3072(8) 0.104(3) Uani d 1 . . H H29 0.237239 0.525665 0.224424 0.125 Uiso calc 1 . . C C30 0.2324(9) 0.5939(6) 0.3724(8) 0.084(3) Uani d 1 . . H H30 0.262654 0.634092 0.332495 0.100 Uiso calc 1 . . C C31 0.2036(9) 0.5990(6) 0.4957(9) 0.058(2) Uani d 1 . . C C32 0.2216(8) 0.6702(5) 0.5639(8) 0.056(2) Uani d 1 . . C C33 0.1627(9) 0.7300(6) 0.5079(9) 0.079(3) Uani d 1 . . H H33 0.113274 0.725890 0.429438 0.095 Uiso calc 1 . . C C34 0.1758(9) 0.7962(6) 0.5664(11) 0.097(3) Uani d 1 . . H H34 0.138444 0.837068 0.527241 0.116 Uiso calc 1 . . C C35 0.2465(9) 0.7998(6) 0.6853(12) 0.093(3) Uani d 1 . . H H35 0.251564 0.843407 0.728319 0.111 Uiso calc 1 . . C C36 0.3078(9) 0.7422(6) 0.7400(9) 0.082(3) Uani d 1 . . H H36 0.358637 0.746573 0.817702 0.099 Uiso calc 1 . . C C37 0.2948(8) 0.6752(6) 0.6792(9) 0.063(2) Uani d 1 . . H H37 0.335477 0.634764 0.716872 0.075 Uiso calc 1 . . C C38 0.1443(7) 0.5827(4) 0.9508(7) 0.0448(19) Uani d 1 . . C C39 0.0664(8) 0.6388(5) 0.9723(8) 0.054(2) Uani d 1 . . H H39 -0.023526 0.635579 0.948671 0.065 Uiso calc 1 . . C C40 0.1192(8) 0.7021(5) 1.0298(9) 0.062(2) Uani d 1 . . H H40 0.064808 0.740340 1.045416 0.074 Uiso calc 1 . . C C41 0.2539(9) 0.7064(5) 1.0629(9) 0.060(3) Uani d 1 . . C C42 0.3310(8) 0.6474(5) 1.0453(9) 0.056(2) Uani d 1 . . H H42 0.420553 0.648662 1.071609 0.068 Uiso calc 1 . . C C43 0.2757(8) 0.5872(5) 0.9893(9) 0.054(2) Uani d 1 . . H H43 0.328990 0.548042 0.976853 0.065 Uiso calc 1 . . C C44 0.2485(10) 0.8307(6) 1.1136(10) 0.091(3) Uani d 1 . . H H44A 0.210510 0.840209 1.028576 0.136 Uiso calc 1 . . H H44B 0.307576 0.868873 1.141785 0.136 Uiso calc 1 . . H H44C 0.180116 0.827590 1.168128 0.136 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.03554(14) 0.04656(15) 0.03469(15) -0.00173(13) 0.00435(10) -0.00068(14) Cl1 0.0433(11) 0.0668(16) 0.0728(15) -0.0116(11) 0.0139(10) -0.0130(13) Cl2 0.0404(10) 0.0581(14) 0.0670(14) -0.0082(10) 0.0081(9) -0.0118(12) O1 0.065(4) 0.081(5) 0.155(7) 0.000(4) 0.013(4) -0.050(5) O2 0.071(4) 0.063(5) 0.112(5) -0.008(4) 0.015(4) -0.034(4) N1 0.030(3) 0.048(4) 0.036(4) -0.004(3) 0.000(2) 0.003(3) N2 0.041(3) 0.046(4) 0.032(3) 0.001(3) 0.007(3) -0.002(3) C1 0.048(4) 0.065(6) 0.045(5) 0.002(4) 0.017(4) -0.009(4) C2 0.055(4) 0.052(4) 0.040(4) -0.003(3) 0.016(3) -0.001(3) C3 0.078(4) 0.085(4) 0.081(4) -0.029(3) 0.044(4) -0.023(4) C4 0.049(4) 0.088(5) 0.045(5) 0.022(4) 0.013(3) 0.017(4) C5 0.074(5) 0.123(6) 0.044(4) 0.031(4) -0.002(4) -0.002(4) C6 0.093(6) 0.194(9) 0.056(5) 0.043(7) 0.000(5) -0.003(5) C7 0.104(8) 0.278(14) 0.040(5) 0.022(9) 0.002(5) 0.021(6) C8 0.080(6) 0.230(12) 0.062(6) 0.002(7) 0.011(5) 0.071(6) C9 0.047(5) 0.142(7) 0.059(6) 0.016(5) 0.013(4) 0.046(5) C10 0.053(6) 0.102(7) 0.116(8) 0.006(6) 0.031(5) 0.062(6) C11 0.075(7) 0.127(8) 0.199(12) 0.008(7) 0.018(7) 0.112(9) C12 0.136(12) 0.100(7) 0.273(17) 0.021(8) 0.032(10) 0.113(10) C13 0.123(9) 0.089(6) 0.249(14) -0.010(6) 0.043(9) 0.057(8) C14 0.098(7) 0.076(6) 0.138(8) -0.005(5) 0.030(5) 0.027(5) C15 0.066(5) 0.081(6) 0.096(7) -0.003(5) 0.028(5) 0.026(5) C16 0.042(4) 0.048(4) 0.041(4) 0.003(3) 0.013(3) -0.002(3) C17 0.040(4) 0.062(6) 0.081(6) 0.010(4) 0.007(4) -0.021(5) C18 0.053(5) 0.081(7) 0.115(9) 0.003(5) 0.008(5) -0.039(6) C19 0.054(5) 0.053(6) 0.080(7) -0.006(4) 0.014(4) -0.015(5) C20 0.060(5) 0.061(6) 0.087(7) 0.023(4) 0.011(5) -0.012(5) C21 0.041(4) 0.072(7) 0.075(6) 0.006(4) 0.005(4) -0.006(5) C22 0.091(7) 0.059(7) 0.187(12) 0.018(6) 0.016(7) -0.034(7) C23 0.034(4) 0.045(5) 0.051(5) 0.001(3) 0.000(3) 0.014(4) C24 0.043(3) 0.059(4) 0.035(3) -0.006(3) 0.011(3) -0.003(3) C25 0.087(4) 0.063(4) 0.046(3) -0.014(3) 0.021(3) -0.004(3) C26 0.043(4) 0.080(5) 0.030(4) -0.006(3) -0.002(3) 0.008(4) C27 0.075(5) 0.072(5) 0.038(4) -0.003(4) -0.002(3) 0.002(3) C28 0.115(6) 0.103(6) 0.037(4) -0.007(6) 0.004(4) -0.017(4) C29 0.121(8) 0.161(9) 0.032(4) -0.024(7) 0.015(4) -0.007(5) C30 0.093(6) 0.116(6) 0.042(4) -0.029(5) 0.006(4) 0.004(4) C31 0.053(5) 0.076(5) 0.044(5) -0.003(4) 0.000(4) 0.009(4) C32 0.043(5) 0.075(6) 0.052(5) -0.005(4) 0.008(4) 0.023(4) C33 0.064(5) 0.085(6) 0.088(6) -0.021(5) 0.005(5) 0.031(5) C34 0.076(5) 0.080(7) 0.132(8) -0.001(5) 0.005(5) 0.050(6) C35 0.101(7) 0.059(5) 0.124(8) -0.014(5) 0.037(6) -0.002(5) C36 0.086(5) 0.085(7) 0.077(6) -0.015(5) 0.021(4) 0.001(5) C37 0.063(5) 0.069(6) 0.057(5) -0.001(4) 0.008(4) 0.017(4) C38 0.044(4) 0.056(5) 0.036(4) 0.002(3) 0.012(3) -0.001(3) C39 0.047(4) 0.055(5) 0.062(5) -0.003(4) 0.015(4) -0.010(4) C40 0.056(5) 0.051(5) 0.083(6) 0.002(4) 0.023(4) -0.017(5) C41 0.060(6) 0.064(6) 0.061(6) -0.009(5) 0.023(4) -0.018(5) C42 0.041(4) 0.070(6) 0.060(5) -0.009(4) 0.009(3) -0.022(4) C43 0.054(5) 0.060(6) 0.049(4) 0.004(4) 0.013(4) -0.010(4) C44 0.095(7) 0.061(7) 0.122(8) -0.007(6) 0.035(6) -0.018(6) 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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 -26 0 0 -26 1 0 -25 0 0 -25 -1 0 -25 1 0 -25 -2 0 -25 2 0 -25 3 0 -24 0 0 -24 -1 0 -24 1 0 -24 -2 0 -24 2 0 -24 -3 0 -24 -4 0 -24 4 0 -24 5 0 -23 0 0 -23 -1 0 -23 1 0 -23 -2 0 -23 2 0 -23 -3 0 -23 3 0 -23 4 0 -23 -4 0 -23 -5 0 -23 5 0 -23 6 0 -22 0 0 -22 0 0 -22 1 0 -22 1 0 -22 -1 0 -22 -2 0 -22 2 0 -22 3 0 -22 -3 0 -22 -4 0 -22 4 0 -22 5 0 -22 -5 0 -22 -6 0 -22 6 0 -22 7 0 -21 0 0 -21 0 0 -21 -1 0 -21 -1 0 -21 1 0 -21 1 0 -21 -2 0 -21 2 0 -21 3 0 -21 -3 0 -21 -4 0 -21 4 0 -21 -5 0 -21 5 0 -21 -6 0 -21 6 0 -21 7 0 -20 0 0 -20 0 0 -20 -1 0 -20 -1 0 -20 1 0 -20 -2 0 -20 2 0 -20 -2 0 -20 3 0 -20 -3 0 -20 -4 0 -20 4 0 -20 -5 0 -20 5 0 -20 -6 0 -20 6 0 -20 7 0 -20 8 0 -19 0 0 -19 0 0 -19 -1 0 -19 1 0 -19 -1 0 -19 -2 0 -19 -2 0 -19 2 0 -19 3 0 -19 -3 0 -19 -3 0 -19 -4 0 -19 4 0 -19 -5 0 -19 5 0 -19 -6 0 -19 6 0 -19 7 0 -19 8 0 -18 0 0 -18 0 0 -18 -1 0 -18 -1 0 -18 1 0 -18 2 0 -18 -2 0 -18 -2 0 -18 3 0 -18 -3 0 -18 -3 0 -18 -4 0 -18 -4 0 -18 4 0 -18 5 0 -18 -5 0 -18 -6 0 -18 6 0 -18 7 0 -18 8 0 -18 9 0 -17 0 0 -17 -1 0 -17 1 0 -17 -1 0 -17 1 0 -17 2 0 -17 -2 0 -17 2 0 -17 -2 0 -17 3 0 -17 3 0 -17 -3 0 -17 -3 0 -17 -4 0 -17 4 0 -17 -4 0 -17 4 0 -17 5 0 -17 -5 0 -17 6 0 -17 -6 0 -17 7 0 -17 8 0 -17 9 0 -16 0 0 -16 0 0 -16 1 0 -16 -1 0 -16 -1 0 -16 1 0 -16 2 0 -16 -2 0 -16 -2 0 -16 2 0 -16 3 0 -16 3 0 -16 -3 0 -16 -3 0 -16 4 0 -16 -4 0 -16 4 0 -16 -4 0 -16 5 0 -16 5 0 -16 -5 0 -16 -6 0 -16 6 0 -16 7 0 -16 8 0 -16 9 0 -16 -10 0 -16 10 0 -15 0 0 -15 0 0 -15 1 0 -15 -1 0 -15 -1 0 -15 -1 0 -15 1 0 -15 2 0 -15 -2 0 -15 2 0 -15 -2 0 -15 3 0 -15 -3 0 -15 3 0 -15 -3 0 -15 -4 0 -15 4 0 -15 4 0 -15 -4 0 -15 5 0 -15 -5 0 -15 -5 0 -15 5 0 -15 6 0 -15 6 0 -15 -6 0 -15 7 0 -15 8 0 -15 9 0 -15 -10 0 -15 10 0 -15 -11 0 -14 0 0 -14 0 0 -14 -1 0 -14 -1 0 -14 1 0 -14 -1 0 -14 1 0 -14 -2 0 -14 2 0 -14 2 0 -14 -2 0 -14 -3 0 -14 -3 0 -14 3 0 -14 3 0 -14 -4 0 -14 -4 0 -14 4 0 -14 -4 0 -14 -4 0 -14 4 0 -14 -5 0 -14 5 0 -14 5 0 -14 -5 0 -14 6 0 -14 6 0 -14 -6 0 -14 -6 0 -14 7 0 -14 8 0 -14 9 0 -14 -10 0 -14 10 0 -14 -11 0 -14 11 0 -14 -12 0 -13 0 0 -13 0 0 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5 12 4 6 -12 5 4 12 5 -2 12 5 -1 12 5 0 12 5 0 12 5 1 12 5 1 12 5 2 12 5 2 12 5 3 12 5 3 12 5 4 12 5 4 12 5 5 12 5 5 12 5 6 12 6 -2 12 6 -1 12 6 0 12 6 1 12 6 1 12 6 2 12 6 2 12 6 3 12 6 3 12 6 4 12 6 4 12 6 5 12 7 -2 12 7 -1 12 7 0 12 7 1 12 7 1 12 7 2 12 7 2 12 7 3 12 7 3 12 7 4 12 7 4 12 8 -2 12 8 -1 12 8 0 12 8 1 12 8 1 12 8 2 12 8 2 12 8 3 12 9 -2 12 9 -1 12 9 0 12 9 1 12 9 1 12 9 2 12 10 -2 12 10 -1 12 10 1 13 -9 -5 -13 -6 3 -13 -6 2 -13 -5 5 -13 -5 4 -13 -5 3 -13 -5 2 -13 -5 1 -13 -4 6 -13 -4 5 -13 -4 4 -13 -4 3 -13 -4 2 13 -4 -2 -13 -4 1 13 -4 -1 -13 -4 0 -13 -3 7 -13 -3 6 -13 -3 5 -13 -3 4 -13 -3 3 13 -3 -3 -13 -3 2 13 -3 -2 -13 -3 1 13 -3 -1 -13 -3 0 13 -3 0 -13 -3 -1 13 -3 1 -13 -2 7 -13 -2 6 -13 -2 5 -13 -2 4 -13 -2 3 13 -2 -3 -13 -2 2 13 -2 -2 -13 -2 1 13 -2 -1 -13 -2 0 13 -2 0 13 -2 1 -13 -1 7 -13 -1 6 -13 -1 5 -13 -1 4 -13 -1 3 13 -1 -3 -13 -1 2 13 -1 -2 -13 -1 1 13 -1 -1 -13 -1 0 13 -1 0 13 -1 1 13 -1 2 -13 0 6 -13 0 5 -13 0 4 -13 0 3 13 0 -3 -13 0 2 13 0 -2 -13 0 1 13 0 -1 13 0 0 13 0 0 13 0 1 13 0 1 13 0 2 13 0 2 13 0 3 13 0 4 -13 1 6 -13 1 5 -13 1 4 -13 1 3 13 1 -3 13 1 -2 13 1 -2 -13 1 1 13 1 -1 13 1 -1 13 1 0 13 1 0 13 1 1 13 1 1 13 1 2 13 1 2 13 1 3 13 1 3 13 1 4 13 1 5 -13 2 5 -13 2 4 -13 2 3 13 2 -3 -13 2 2 13 2 -2 13 2 -1 13 2 -1 13 2 0 13 2 0 13 2 1 13 2 1 13 2 2 13 2 2 13 2 3 13 2 3 13 2 4 -13 3 4 -13 3 3 13 3 -3 13 3 -2 13 3 -1 13 3 -1 13 3 0 13 3 0 13 3 1 13 3 1 13 3 2 13 3 2 13 3 3 13 3 3 13 3 4 13 3 4 -13 4 4 13 4 -3 13 4 -2 13 4 -1 13 4 -1 13 4 0 13 4 0 13 4 1 13 4 1 13 4 2 13 4 2 13 4 3 13 4 3 13 4 4 13 5 -3 13 5 -2 13 5 -1 13 5 0 13 5 0 13 5 1 13 5 1 13 5 2 13 5 2 13 5 3 13 5 3 13 5 4 13 6 -3 13 6 -2 13 6 -1 13 6 0 13 6 0 13 6 1 13 6 1 13 6 2 13 6 2 13 6 3 13 7 -3 13 7 -2 13 7 -1 13 7 0 13 7 0 13 7 1 13 7 1 13 7 2 13 8 -3 13 8 -2 13 8 -1 13 8 0 13 8 0 13 9 -3 13 9 -2 -14 -1 4 -14 -1 3 -14 0 5 -14 0 4 -14 0 3 -14 0 2 -14 1 4 -14 1 3 -14 1 2 -14 2 4 -14 2 3 14 3 0 14 3 1 14 4 -1 14 4 0 14 4 1 14 5 -1 14 5 0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Pd1 Cl2 . . 177.44(11) ? N1 Pd1 Cl1 . . 91.85(19) ? N1 Pd1 Cl2 . . 88.10(17) ? N1 Pd1 N2 . . 176.4(3) ? N2 Pd1 Cl1 . . 89.96(18) ? N2 Pd1 Cl2 . . 90.0(2) ? C22 O1 C19 . . 118.5(8) ? C41 O2 C44 . . 117.3(8) ? C1 N1 Pd1 . . 124.5(5) ? C1 N1 C2 . . 119.6(7) ? C2 N1 Pd1 . . 115.9(5) ? C23 N2 Pd1 . . 122.7(5) ? C23 N2 C24 . . 115.1(6) ? C24 N2 Pd1 . . 121.9(5) ? N1 C1 H1 . . 116.7 ? N1 C1 C4 . . 126.6(8) ? C4 C1 H1 . . 116.7 ? N1 C2 H2 . . 106.4 ? N1 C2 C3 . . 109.9(5) ? C3 C2 H2 . . 106.4 ? C16 C2 N1 . . 112.3(6) ? C16 C2 H2 . . 106.4 ? C16 C2 C3 . . 115.0(6) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3B . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C5 C4 C1 . . 119.5(9) ? C5 C4 C9 . . 120.5(9) ? C9 C4 C1 . . 119.7(10) ? C4 C5 H5 . . 119.0 ? C4 C5 C6 . . 121.9(11) ? C6 C5 H5 . . 119.0 ? C5 C6 H6 . . 121.4 ? C5 C6 C7 . . 117.2(12) ? C7 C6 H6 . . 121.4 ? C6 C7 H7 . . 118.7 ? C8 C7 C6 . . 122.5(11) ? C8 C7 H7 . . 118.7 ? C7 C8 H8 . . 118.4 ? C7 C8 C9 . . 123.2(13) ? C9 C8 H8 . . 118.4 ? C8 C9 C4 . . 114.6(13) ? C8 C9 C10 . . 122.1(13) ? C10 C9 C4 . . 123.3(11) ? C9 C10 C11 . . 121.9(14) ? C15 C10 C9 . . 123.1(12) ? C15 C10 C11 . . 115.0(14) ? C10 C11 H11 . . 119.8 ? C12 C11 C10 . . 120.3(14) ? C12 C11 H11 . . 119.8 ? C11 C12 H12 . . 118.7 ? C11 C12 C13 . . 122.6(15) ? C13 C12 H12 . . 118.7 ? C12 C13 H13 . . 120.4 ? C12 C13 C14 . . 119.2(15) ? C14 C13 H13 . . 120.4 ? C13 C14 H14 . . 120.0 ? C15 C14 C13 . . 120.0(13) ? C15 C14 H14 . . 120.0 ? C10 C15 H15 . . 118.6 ? C14 C15 C10 . . 122.7(12) ? C14 C15 H15 . . 118.6 ? C17 C16 C2 . . 119.0(8) ? C17 C16 C21 . . 115.1(8) ? C21 C16 C2 . . 125.9(7) ? C16 C17 H17 . . 118.6 ? C18 C17 C16 . . 122.8(9) ? C18 C17 H17 . . 118.6 ? C17 C18 H18 . . 120.4 ? C19 C18 C17 . . 119.1(9) ? C19 C18 H18 . . 120.4 ? C18 C19 O1 . . 114.1(8) ? C20 C19 O1 . . 124.8(9) ? C20 C19 C18 . . 121.1(9) ? C19 C20 H20 . . 120.2 ? C19 C20 C21 . . 119.6(9) ? C21 C20 H20 . . 120.2 ? C16 C21 H21 . . 118.9 ? C20 C21 C16 . . 122.2(8) ? C20 C21 H21 . . 118.9 ? O1 C22 H22A . . 109.5 ? O1 C22 H22B . . 109.5 ? O1 C22 H22C . . 109.5 ? H22A C22 H22B . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? N2 C23 H23 . . 117.3 ? N2 C23 C26 . . 125.4(8) ? C26 C23 H23 . . 117.3 ? N2 C24 H24 . . 106.9 ? N2 C24 C38 . . 110.6(6) ? C25 C24 N2 . . 112.2(6) ? C25 C24 H24 . . 106.9 ? C25 C24 C38 . . 112.9(6) ? C38 C24 H24 . . 106.9 ? C24 C25 H25A . . 109.5 ? C24 C25 H25B . . 109.5 ? C24 C25 H25C . . 109.5 ? H25A C25 H25B . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? C27 C26 C23 . . 119.9(8) ? C31 C26 C23 . . 119.2(8) ? C31 C26 C27 . . 120.7(7) ? C26 C27 H27 . . 120.7 ? C28 C27 C26 . . 118.5(8) ? C28 C27 H27 . . 120.7 ? C27 C28 H28 . . 119.4 ? C29 C28 C27 . . 121.2(8) ? C29 C28 H28 . . 119.4 ? C28 C29 H29 . . 120.1 ? C28 C29 C30 . . 119.9(8) ? C30 C29 H29 . . 120.1 ? C29 C30 H30 . . 119.8 ? C31 C30 C29 . . 120.5(9) ? C31 C30 H30 . . 119.8 ? C26 C31 C30 . . 119.1(10) ? C26 C31 C32 . . 121.6(9) ? C30 C31 C32 . . 119.3(10) ? C33 C32 C31 . . 118.6(9) ? C37 C32 C31 . . 121.0(9) ? C37 C32 C33 . . 120.3(10) ? C32 C33 H33 . . 119.6 ? C32 C33 C34 . . 120.9(9) ? C34 C33 H33 . . 119.6 ? C33 C34 H34 . . 121.0 ? C33 C34 C35 . . 118.0(10) ? C35 C34 H34 . . 121.0 ? C34 C35 H35 . . 119.1 ? C36 C35 C34 . . 121.8(10) ? C36 C35 H35 . . 119.1 ? C35 C36 H36 . . 120.2 ? C35 C36 C37 . . 119.6(10) ? C37 C36 H36 . . 120.2 ? C32 C37 C36 . . 119.3(9) ? C32 C37 H37 . . 120.4 ? C36 C37 H37 . . 120.4 ? C39 C38 C24 . . 120.3(7) ? C39 C38 C43 . . 118.9(8) ? C43 C38 C24 . . 120.6(8) ? C38 C39 H39 . . 119.5 ? C38 C39 C40 . . 121.0(8) ? C40 C39 H39 . . 119.5 ? C39 C40 H40 . . 120.6 ? C41 C40 C39 . . 118.8(8) ? C41 C40 H40 . . 120.6 ? O2 C41 C40 . . 125.0(9) ? O2 C41 C42 . . 115.7(8) ? C42 C41 C40 . . 119.2(9) ? C41 C42 H42 . . 120.1 ? C43 C42 C41 . . 119.9(8) ? C43 C42 H42 . . 120.1 ? C38 C43 H43 . . 119.0 ? C42 C43 C38 . . 122.0(9) ? C42 C43 H43 . . 119.0 ? O2 C44 H44A . . 109.5 ? O2 C44 H44B . . 109.5 ? O2 C44 H44C . . 109.5 ? H44A C44 H44B . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 Cl1 . 2.310(2) ? Pd1 Cl2 . 2.315(2) ? Pd1 N1 . 2.015(6) ? Pd1 N2 . 2.022(6) ? O1 C19 . 1.394(11) ? O1 C22 . 1.370(11) ? O2 C41 . 1.364(11) ? O2 C44 . 1.419(11) ? N1 C1 . 1.238(10) ? N1 C2 . 1.500(8) ? N2 C23 . 1.299(9) ? N2 C24 . 1.512(8) ? C1 H1 . 0.9300 ? C1 C4 . 1.472(11) ? C2 H2 . 0.9800 ? C2 C3 . 1.511(8) ? C2 C16 . 1.482(11) ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 C5 . 1.382(12) ? C4 C9 . 1.449(15) ? C5 H5 . 0.9300 ? C5 C6 . 1.383(12) ? C6 H6 . 0.9300 ? C6 C7 . 1.393(18) ? C7 H7 . 0.9300 ? C7 C8 . 1.327(19) ? C8 H8 . 0.9300 ? C8 C9 . 1.412(16) ? C9 C10 . 1.427(18) ? C10 C11 . 1.429(16) ? C10 C15 . 1.422(15) ? C11 H11 . 0.9300 ? C11 C12 . 1.35(2) ? C12 H12 . 0.9300 ? C12 C13 . 1.353(19) ? C13 H13 . 0.9300 ? C13 C14 . 1.380(15) ? C14 H14 . 0.9300 ? C14 C15 . 1.340(14) ? C15 H15 . 0.9300 ? C16 C17 . 1.385(11) ? C16 C21 . 1.394(11) ? C17 H17 . 0.9300 ? C17 C18 . 1.377(13) ? C18 H18 . 0.9300 ? C18 C19 . 1.362(12) ? C19 C20 . 1.336(12) ? C20 H20 . 0.9300 ? C20 C21 . 1.388(12) ? C21 H21 . 0.9300 ? C22 H22A . 0.9600 ? C22 H22B . 0.9600 ? C22 H22C . 0.9600 ? C23 H23 . 0.9300 ? C23 C26 . 1.482(10) ? C24 H24 . 0.9800 ? C24 C25 . 1.497(9) ? C24 C38 . 1.533(11) ? C25 H25A . 0.9600 ? C25 H25B . 0.9600 ? C25 H25C . 0.9600 ? C26 C27 . 1.402(11) ? C26 C31 . 1.373(12) ? C27 H27 . 0.9300 ? C27 C28 . 1.384(10) ? C28 H28 . 0.9300 ? C28 C29 . 1.349(12) ? C29 H29 . 0.9300 ? C29 C30 . 1.395(13) ? C30 H30 . 0.9300 ? C30 C31 . 1.379(12) ? C31 C32 . 1.512(14) ? C32 C33 . 1.370(12) ? C32 C37 . 1.368(12) ? C33 H33 . 0.9300 ? C33 C34 . 1.380(14) ? C34 H34 . 0.9300 ? C34 C35 . 1.387(13) ? C35 H35 . 0.9300 ? C35 C36 . 1.343(13) ? C36 H36 . 0.9300 ? C36 C37 . 1.403(12) ? C37 H37 . 0.9300 ? C38 C39 . 1.349(11) ? C38 C43 . 1.366(10) ? C39 H39 . 0.9300 ? C39 C40 . 1.408(11) ? C40 H40 . 0.9300 ? C40 C41 . 1.389(12) ? C41 C42 . 1.378(12) ? C42 H42 . 0.9300 ? C42 C43 . 1.362(12) ? C43 H43 . 0.9300 ? C44 H44A . 0.9600 ? C44 H44B . 0.9600 ? C44 H44C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C3 H3A Cl1 . 0.96 2.90 3.662(6) 137.5 yes C22 H22A Cl1 2_646 0.96 2.87 3.765(10) 154.7 yes C25 H25A Cl2 . 0.96 2.71 3.460(6) 135.0 yes C44 H44C Cl2 2_557 0.96 2.82 3.757(9) 164.9 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd1 N1 C1 C4 . . . . -7.7(12) ? Pd1 N1 C2 C3 . . . . 105.9(6) ? Pd1 N1 C2 C16 . . . . -124.8(6) ? Pd1 N2 C23 C26 . . . . 10.4(11) ? Pd1 N2 C24 C25 . . . . -10.7(8) ? Pd1 N2 C24 C38 . . . . 116.2(6) ? O1 C19 C20 C21 . . . . 178.5(10) ? O2 C41 C42 C43 . . . . -178.4(9) ? N1 C1 C4 C5 . . . . -46.8(12) ? N1 C1 C4 C9 . . . . 139.0(9) ? N1 C2 C16 C17 . . . . 75.6(10) ? N1 C2 C16 C21 . . . . -105.0(9) ? N2 C23 C26 C27 . . . . 38.9(11) ? N2 C23 C26 C31 . . . . -146.2(8) ? N2 C24 C38 C39 . . . . 121.4(8) ? N2 C24 C38 C43 . . . . -63.2(10) ? C1 N1 C2 C3 . . . . -76.9(9) ? C1 N1 C2 C16 . . . . 52.4(9) ? C1 C4 C5 C6 . . . . -176.8(8) ? C1 C4 C9 C8 . . . . 177.2(8) ? C1 C4 C9 C10 . . . . -4.5(15) ? C2 N1 C1 C4 . . . . 175.4(7) ? C2 C16 C17 C18 . . . . 178.5(10) ? C2 C16 C21 C20 . . . . -180.0(9) ? C3 C2 C16 C17 . . . . -157.7(8) ? C3 C2 C16 C21 . . . . 21.7(12) ? C4 C5 C6 C7 . . . . 1.7(13) ? C4 C9 C10 C11 . . . . 132.7(11) ? C4 C9 C10 C15 . . . . -47.4(16) ? C5 C4 C9 C8 . . . . 3.1(14) ? C5 C4 C9 C10 . . . . -178.6(9) ? C5 C6 C7 C8 . . . . -1.5(17) ? C6 C7 C8 C9 . . . . 2(2) ? C7 C8 C9 C4 . . . . -2.9(18) ? C7 C8 C9 C10 . . . . 178.8(13) ? C8 C9 C10 C11 . . . . -49.1(16) ? C8 C9 C10 C15 . . . . 130.8(12) ? C9 C4 C5 C6 . . . . -2.7(13) ? C9 C10 C11 C12 . . . . 179.9(13) ? C9 C10 C15 C14 . . . . -178.9(10) ? C10 C11 C12 C13 . . . . -3(2) ? C11 C10 C15 C14 . . . . 1.0(15) ? C11 C12 C13 C14 . . . . 5(3) ? C12 C13 C14 C15 . . . . -4(2) ? C13 C14 C15 C10 . . . . 0.9(16) ? C15 C10 C11 C12 . . . . 0.0(17) ? C16 C17 C18 C19 . . . . 1.4(18) ? C17 C16 C21 C20 . . . . -0.6(14) ? C17 C18 C19 O1 . . . . 179.9(10) ? C17 C18 C19 C20 . . . . -0.2(17) ? C18 C19 C20 C21 . . . . -1.4(16) ? C19 C20 C21 C16 . . . . 1.8(15) ? C21 C16 C17 C18 . . . . -1.0(15) ? C22 O1 C19 C18 . . . . -170.9(10) ? C22 O1 C19 C20 . . . . 9.2(16) ? C23 N2 C24 C25 . . . . 175.1(6) ? C23 N2 C24 C38 . . . . -57.9(8) ? C23 C26 C27 C28 . . . . 176.3(7) ? C23 C26 C31 C30 . . . . -177.0(8) ? C23 C26 C31 C32 . . . . 3.9(13) ? C24 N2 C23 C26 . . . . -175.5(7) ? C24 C38 C39 C40 . . . . 177.5(8) ? C24 C38 C43 C42 . . . . -177.5(8) ? C25 C24 C38 C39 . . . . -112.0(8) ? C25 C24 C38 C43 . . . . 63.4(9) ? C26 C27 C28 C29 . . . . 0.4(13) ? C26 C31 C32 C33 . . . . -128.0(9) ? C26 C31 C32 C37 . . . . 52.0(12) ? C27 C26 C31 C30 . . . . -2.1(14) ? C27 C26 C31 C32 . . . . 178.8(8) ? C27 C28 C29 C30 . . . . -1.5(14) ? C28 C29 C30 C31 . . . . 0.8(15) ? C29 C30 C31 C26 . . . . 1.0(15) ? C29 C30 C31 C32 . . . . -179.9(9) ? C30 C31 C32 C33 . . . . 53.0(12) ? C30 C31 C32 C37 . . . . -127.1(10) ? C31 C26 C27 C28 . . . . 1.4(12) ? C31 C32 C33 C34 . . . . 179.8(9) ? C31 C32 C37 C36 . . . . -179.3(8) ? C32 C33 C34 C35 . . . . -2.2(14) ? C33 C32 C37 C36 . . . . 0.6(13) ? C33 C34 C35 C36 . . . . 4.1(15) ? C34 C35 C36 C37 . . . . -3.6(14) ? C35 C36 C37 C32 . . . . 1.2(13) ? C37 C32 C33 C34 . . . . -0.1(13) ? C38 C39 C40 C41 . . . . 0.9(14) ? C39 C38 C43 C42 . . . . -2.0(14) ? C39 C40 C41 O2 . . . . 178.7(9) ? C39 C40 C41 C42 . . . . -3.7(14) ? C40 C41 C42 C43 . . . . 3.7(15) ? C41 C42 C43 C38 . . . . -0.9(15) ? C43 C38 C39 C40 . . . . 1.9(13) ? C44 O2 C41 C40 . . . . -14.6(14) ? C44 O2 C41 C42 . . . . 167.7(8) ?