#------------------------------------------------------------------------------ #$Date: 2021-09-30 00:46:04 +0300 (Thu, 30 Sep 2021) $ #$Revision: 269372 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564768.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_1564768 loop_ _publ_author_name 'Prima, Darya O.' 'Madiyeva, Malena' 'Burykina, Julia V.' 'Minyaev, Mikhail E.' 'Boiko, Daniil A.' 'Ananikov, Valentine P.' _publ_section_title ; Evidence for “cocktail”-type catalysis in Buchwald--Hartwig reaction. A mechanistic study ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D1CY01601F _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C54 H72 I4 N4 Pd2, C H2 Cl2' _chemical_formula_sum 'C55 H74 Cl2 I4 N4 Pd2' _chemical_formula_weight 1582.48 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-04-25 deposited with the CCDC. 2021-09-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.0640(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.5373(3) _cell_length_b 15.0465(3) _cell_length_c 16.1547(3) _cell_measurement_reflns_used 9653 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 36.33 _cell_measurement_theta_min 2.79 _cell_volume 3000.57(11) _computing_cell_refinement 'SAINT (Bruker, 2019)' _computing_data_collection 'APEX3 (Bruker, 2019)' _computing_data_reduction 'SAINT (Bruker, 2019)' _computing_molecular_graphics 'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_publication_material 'SHELXTL (Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_structure_refinement 'SHELXL-2018 (Sheldrick, Acta Cryst., 2015, C71, 3-8)' _computing_structure_solution 'SHELXT, SHELXS-2013 (Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS D8 QUEST, Photon III detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 220125 _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 36.347 _diffrn_reflns_theta_min 2.258 _diffrn_source 'sealed X-Ray tube' _diffrn_source_current 30 _diffrn_source_power 50 _diffrn_source_size '0.6 mm, fine-focus' _exptl_absorpt_coefficient_mu 2.783 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.6088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2016/2 (Krause et al., J. Appl. Cryst. 2015, 48, 3-10)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.752 _exptl_crystal_description block _exptl_crystal_F_000 1540 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.42 _refine_diff_density_max 0.775 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.075 _refine_ls_abs_structure_details ; Flack x determined using 13267 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack, Wagner, Acta Cryst., 2013, B69, 249-259). ; _refine_ls_abs_structure_Flack 0.010(3) _refine_ls_extinction_coef 0.00128(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 631 _refine_ls_number_reflns 29074 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0185 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+1.0134P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0417 _reflns_Friedel_coverage 0.941 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 28350 _reflns_number_total 29074 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cy01601f2.cif _cod_data_source_block 2C _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1564768 _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 0.310 _shelx_estimated_absorpt_t_max 0.388 _shelx_res_file ; TITL MM2C_a.res in P2(1) MM2C.res created by SHELXL-2018/3 at 15:48:24 on 21-Dec-2020 CELL 0.71073 12.5373 15.0465 16.1547 90.000 100.064 90.000 ZERR 2.00 0.0003 0.0003 0.0003 0.000 0.001 0.000 LATT -1 SYMM -x, y+1/2, -z SFAC C H N CL PD I UNIT 110 148 8 4 4 8 TEMP -173.15 SIZE 0.42 0.47 0.55 LIST 4 L.S. 10 FMAP 2 PLAN 20 ACTA BOND $H CONF SADI 0.002 C55A Cl1A C55B Cl1B SADI 0.002 C55A Cl2A C55B Cl2B EADP C55A C55B EADP Cl1A Cl1B EADP Cl2A Cl2B WGHT 0.015900 1.013400 EXTI 0.001284 FVAR 0.28641 0.89314 I1 6 0.837228 0.594225 0.274158 11.00000 0.01854 0.01461 = 0.02171 0.00385 0.00042 -0.00056 I2 6 0.736399 0.378001 0.221781 11.00000 0.02910 0.01175 = 0.01652 0.00036 0.00317 0.00198 I3 6 0.902751 0.536822 0.500671 11.00000 0.01945 0.01595 = 0.02071 -0.00214 0.00303 -0.00197 I4 6 0.502956 0.468982 0.073701 11.00000 0.02944 0.02174 = 0.02152 -0.00133 -0.00345 -0.00810 PD1 5 0.812609 0.452796 0.366141 11.00000 0.01449 0.01056 = 0.01530 0.00059 0.00333 0.00125 PD2 5 0.667251 0.538644 0.170089 11.00000 0.01668 0.01104 = 0.01323 0.00012 0.00245 -0.00001 N1 3 0.740940 0.334697 0.499815 11.00000 0.01633 0.01223 = 0.01525 -0.00028 0.00468 0.00084 N2 3 0.865230 0.273132 0.441950 11.00000 0.01672 0.01270 = 0.01399 -0.00075 0.00338 0.00302 N3 3 0.527868 0.705559 0.149216 11.00000 0.01488 0.01583 = 0.01716 0.00174 0.00391 0.00289 N4 3 0.671861 0.721844 0.094854 11.00000 0.01610 0.01374 = 0.01794 0.00278 0.00477 0.00171 C1 1 0.800592 0.346481 0.437604 11.00000 0.01443 0.01313 = 0.01428 -0.00255 0.00282 0.00006 C2 1 0.849210 0.218120 0.508012 11.00000 0.02156 0.01515 = 0.01688 0.00225 0.00457 0.00381 AFIX 43 H2 2 0.886010 0.164112 0.524711 11.00000 -1.20000 AFIX 0 C3 1 0.771148 0.256589 0.543656 11.00000 0.02221 0.01500 = 0.01554 0.00158 0.00512 0.00119 AFIX 43 H3 2 0.742185 0.234386 0.590133 11.00000 -1.20000 AFIX 0 C4 1 0.651336 0.389473 0.515141 11.00000 0.01771 0.01192 = 0.02081 -0.00104 0.00843 0.00073 C5 1 0.555185 0.388080 0.454650 11.00000 0.01785 0.01526 = 0.02326 0.00268 0.00705 0.00123 C6 1 0.469193 0.439740 0.471276 11.00000 0.02124 0.02196 = 0.03270 0.00797 0.01112 0.00563 AFIX 43 H6 2 0.403257 0.440349 0.432014 11.00000 -1.20000 AFIX 0 C7 1 0.477707 0.490061 0.543555 11.00000 0.02838 0.02000 = 0.03947 0.00452 0.01953 0.00781 AFIX 43 H7 2 0.418989 0.526714 0.552313 11.00000 -1.20000 AFIX 0 C8 1 0.571246 0.487435 0.603326 11.00000 0.03331 0.01774 = 0.03345 -0.00342 0.02006 0.00192 AFIX 43 H8 2 0.574918 0.521055 0.653521 11.00000 -1.20000 AFIX 0 C9 1 0.660568 0.436320 0.591434 11.00000 0.02442 0.01492 = 0.02384 -0.00364 0.01133 -0.00272 C10 1 0.540551 0.329255 0.377157 11.00000 0.01776 0.02127 = 0.02114 0.00264 0.00274 -0.00112 AFIX 13 H10 2 0.613130 0.322156 0.360313 11.00000 -1.20000 AFIX 0 C11 1 0.463647 0.368605 0.301969 11.00000 0.03036 0.03581 = 0.02494 0.00604 -0.00446 0.00172 AFIX 137 H11A 2 0.469226 0.334453 0.251247 11.00000 -1.50000 H11B 2 0.483430 0.430642 0.294030 11.00000 -1.50000 H11C 2 0.389082 0.365896 0.312526 11.00000 -1.50000 AFIX 0 C12 1 0.502149 0.236644 0.398922 11.00000 0.03663 0.02187 = 0.03299 -0.00139 0.00768 -0.00799 AFIX 137 H12A 2 0.495488 0.198229 0.349296 11.00000 -1.50000 H12B 2 0.431583 0.241624 0.416756 11.00000 -1.50000 H12C 2 0.554859 0.210956 0.444610 11.00000 -1.50000 AFIX 0 C13 1 0.756889 0.429142 0.662503 11.00000 0.02668 0.02591 = 0.02256 -0.01087 0.01027 -0.00857 AFIX 13 H13 2 0.818195 0.400627 0.640291 11.00000 -1.20000 AFIX 0 C14 1 0.794755 0.519789 0.699978 11.00000 0.04696 0.03485 = 0.03588 -0.01906 0.01958 -0.01964 AFIX 137 H14A 2 0.862295 0.512405 0.740270 11.00000 -1.50000 H14B 2 0.739049 0.544920 0.728757 11.00000 -1.50000 H14C 2 0.807121 0.559968 0.654854 11.00000 -1.50000 AFIX 0 C15 1 0.726114 0.369617 0.732030 11.00000 0.02774 0.03274 = 0.02048 -0.00443 0.00681 -0.00264 AFIX 137 H15A 2 0.786552 0.367375 0.779506 11.00000 -1.50000 H15B 2 0.710186 0.309492 0.709973 11.00000 -1.50000 H15C 2 0.661988 0.394043 0.750926 11.00000 -1.50000 AFIX 0 C16 1 0.924229 0.245556 0.376939 11.00000 0.01773 0.01449 = 0.01404 0.00129 0.00344 0.00525 C17 1 0.876028 0.179978 0.320190 11.00000 0.02206 0.01487 = 0.01697 -0.00159 0.00260 0.00465 C18 1 0.931645 0.155619 0.256025 11.00000 0.03350 0.01881 = 0.01924 -0.00335 0.00788 0.00589 AFIX 43 H18 2 0.901172 0.112140 0.216171 11.00000 -1.20000 AFIX 0 C19 1 1.030350 0.193580 0.249324 11.00000 0.03554 0.02236 = 0.02437 -0.00072 0.01563 0.00730 AFIX 43 H19 2 1.066391 0.176497 0.204749 11.00000 -1.20000 AFIX 0 C20 1 1.076818 0.256380 0.307334 11.00000 0.02612 0.02129 = 0.02839 0.00127 0.01436 0.00535 AFIX 43 H20 2 1.145362 0.280895 0.302719 11.00000 -1.20000 AFIX 0 C21 1 1.024784 0.284264 0.372389 11.00000 0.01731 0.01592 = 0.02028 0.00169 0.00489 0.00537 C22 1 0.770526 0.132799 0.328129 11.00000 0.02081 0.02016 = 0.02250 -0.00416 0.00222 0.00231 AFIX 13 H22 2 0.733822 0.167852 0.367640 11.00000 -1.20000 AFIX 0 C23 1 0.691845 0.123938 0.244657 11.00000 0.03206 0.02337 = 0.03135 -0.00143 -0.00809 -0.00122 AFIX 137 H23A 2 0.680099 0.182449 0.217972 11.00000 -1.50000 H23B 2 0.622619 0.100236 0.255131 11.00000 -1.50000 H23C 2 0.722456 0.083457 0.207440 11.00000 -1.50000 AFIX 0 C24 1 0.795343 0.040040 0.365847 11.00000 0.02721 0.02499 = 0.02678 0.00323 0.00479 -0.00139 AFIX 137 H24A 2 0.841095 0.045487 0.421367 11.00000 -1.50000 H24B 2 0.833370 0.005061 0.328882 11.00000 -1.50000 H24C 2 0.727429 0.010270 0.371405 11.00000 -1.50000 AFIX 0 C25 1 1.079440 0.351589 0.436118 11.00000 0.01702 0.01910 = 0.02506 0.00008 0.00310 0.00156 AFIX 13 H25 2 1.023812 0.374456 0.468213 11.00000 -1.20000 AFIX 0 C26 1 1.124360 0.431012 0.393636 11.00000 0.02912 0.02281 = 0.04150 -0.00115 0.01427 -0.00440 AFIX 137 H26A 2 1.159247 0.472606 0.436689 11.00000 -1.50000 H26B 2 1.064955 0.461164 0.356756 11.00000 -1.50000 H26C 2 1.177588 0.410025 0.360312 11.00000 -1.50000 AFIX 0 C27 1 1.169289 0.307237 0.498633 11.00000 0.03172 0.03016 = 0.04385 -0.00181 -0.01089 0.00573 AFIX 137 H27A 2 1.200030 0.350351 0.541734 11.00000 -1.50000 H27B 2 1.226192 0.286112 0.468903 11.00000 -1.50000 H27C 2 1.139251 0.256814 0.525342 11.00000 -1.50000 AFIX 0 C28 1 0.618222 0.661637 0.135533 11.00000 0.01468 0.01406 = 0.01264 -0.00006 0.00122 0.00015 C29 1 0.615447 0.801251 0.082621 11.00000 0.02330 0.01613 = 0.02850 0.00733 0.00711 0.00419 AFIX 43 H29 2 0.635800 0.852758 0.055134 11.00000 -1.20000 AFIX 0 C30 1 0.525787 0.791065 0.117457 11.00000 0.02177 0.01801 = 0.02831 0.00647 0.00666 0.00711 AFIX 43 H30 2 0.471413 0.834529 0.119728 11.00000 -1.20000 AFIX 0 C31 1 0.442403 0.670911 0.189109 11.00000 0.01496 0.01852 = 0.01805 -0.00171 0.00403 0.00039 C32 1 0.340519 0.654955 0.139345 11.00000 0.01704 0.02764 = 0.02147 -0.00511 0.00341 0.00040 C33 1 0.258876 0.622821 0.180577 11.00000 0.01817 0.02980 = 0.03357 -0.00759 0.00564 -0.00439 AFIX 43 H33 2 0.188595 0.612082 0.149274 11.00000 -1.20000 AFIX 0 C34 1 0.278991 0.606528 0.265983 11.00000 0.02192 0.02403 = 0.03551 -0.00163 0.01231 -0.00571 AFIX 43 H34 2 0.223161 0.582949 0.292410 11.00000 -1.20000 AFIX 0 C35 1 0.379757 0.624221 0.313501 11.00000 0.02447 0.01847 = 0.02338 0.00011 0.00908 -0.00025 AFIX 43 H35 2 0.392097 0.612909 0.372255 11.00000 -1.20000 AFIX 0 C36 1 0.463553 0.658482 0.276250 11.00000 0.01749 0.01412 = 0.01850 -0.00057 0.00459 0.00161 C37 1 0.316037 0.672487 0.045321 11.00000 0.01869 0.05719 = 0.01961 -0.00340 0.00082 0.00291 AFIX 13 H37 2 0.386487 0.675472 0.024445 11.00000 -1.20000 AFIX 0 C38 1 0.247846 0.598529 -0.002860 11.00000 0.02816 0.07762 = 0.03546 -0.02511 -0.00672 0.00535 AFIX 137 H38A 2 0.241192 0.609001 -0.063421 11.00000 -1.50000 H38B 2 0.175639 0.598182 0.012558 11.00000 -1.50000 H38C 2 0.283042 0.541050 0.011431 11.00000 -1.50000 AFIX 0 C39 1 0.258053 0.763230 0.027120 11.00000 0.02559 0.06083 = 0.03408 0.01501 0.00137 0.00414 AFIX 137 H39A 2 0.245579 0.774782 -0.033507 11.00000 -1.50000 H39B 2 0.303467 0.810470 0.056513 11.00000 -1.50000 H39C 2 0.188466 0.761787 0.046851 11.00000 -1.50000 AFIX 0 C40 1 0.569443 0.688485 0.329103 11.00000 0.01830 0.01741 = 0.01788 -0.00166 0.00244 0.00243 AFIX 13 H40 2 0.626755 0.685015 0.293247 11.00000 -1.20000 AFIX 0 C41 1 0.606009 0.631543 0.406906 11.00000 0.02817 0.02529 = 0.01902 0.00219 0.00174 0.00509 AFIX 137 H41A 2 0.678583 0.650094 0.434244 11.00000 -1.50000 H41B 2 0.607748 0.568963 0.390382 11.00000 -1.50000 H41C 2 0.555211 0.638955 0.446121 11.00000 -1.50000 AFIX 0 C42 1 0.558702 0.786042 0.353786 11.00000 0.02574 0.01865 = 0.03455 -0.00542 -0.00644 0.00214 AFIX 137 H42A 2 0.628365 0.807295 0.384554 11.00000 -1.50000 H42B 2 0.503483 0.791247 0.389612 11.00000 -1.50000 H42C 2 0.537392 0.821941 0.302971 11.00000 -1.50000 AFIX 0 C43 1 0.770428 0.707208 0.062427 11.00000 0.01641 0.01635 = 0.02054 0.00338 0.00566 0.00148 C44 1 0.765238 0.656049 -0.010361 11.00000 0.02769 0.01974 = 0.02144 0.00188 0.01074 0.00080 C45 1 0.861427 0.645924 -0.042144 11.00000 0.03877 0.03084 = 0.03482 0.00216 0.02057 0.00736 AFIX 43 H45 2 0.861521 0.610505 -0.090813 11.00000 -1.20000 AFIX 0 C46 1 0.956085 0.686386 -0.004156 11.00000 0.02686 0.04496 = 0.05537 0.00449 0.02259 0.00636 AFIX 43 H46 2 1.020381 0.678398 -0.026884 11.00000 -1.20000 AFIX 0 C47 1 0.958440 0.738372 0.066538 11.00000 0.01919 0.04220 = 0.04957 0.00678 0.00975 -0.00186 AFIX 43 H47 2 1.024373 0.765946 0.091615 11.00000 -1.20000 AFIX 0 C48 1 0.865125 0.751181 0.101985 11.00000 0.02014 0.02332 = 0.03026 0.00600 0.00430 -0.00142 C49 1 0.659693 0.619926 -0.058560 11.00000 0.04085 0.02772 = 0.01887 -0.00263 0.00784 -0.01039 AFIX 13 H49 2 0.605406 0.619206 -0.019982 11.00000 -1.20000 AFIX 0 C50 1 0.672056 0.525291 -0.089356 11.00000 0.08205 0.03853 = 0.04462 -0.02079 0.03419 -0.02404 AFIX 137 H50A 2 0.601436 0.503151 -0.117447 11.00000 -1.50000 H50B 2 0.699788 0.486976 -0.041352 11.00000 -1.50000 H50C 2 0.722889 0.524938 -0.129058 11.00000 -1.50000 AFIX 0 C51 1 0.618079 0.682587 -0.132010 11.00000 0.05483 0.05818 = 0.03042 0.01408 -0.00986 -0.01916 AFIX 137 H51A 2 0.546491 0.662725 -0.160303 11.00000 -1.50000 H51B 2 0.668499 0.681998 -0.172027 11.00000 -1.50000 H51C 2 0.612661 0.743072 -0.110629 11.00000 -1.50000 AFIX 0 C52 1 0.868429 0.814938 0.175249 11.00000 0.03341 0.03050 = 0.03191 -0.00004 0.00135 -0.01145 AFIX 13 H52 2 0.803866 0.803104 0.202219 11.00000 -1.20000 AFIX 0 C53 1 0.970511 0.806376 0.242779 11.00000 0.04533 0.05624 = 0.04340 0.00790 -0.01096 -0.02948 AFIX 137 H53A 2 0.960759 0.840204 0.292758 11.00000 -1.50000 H53B 2 1.033023 0.829797 0.220886 11.00000 -1.50000 H53C 2 0.982917 0.743659 0.257804 11.00000 -1.50000 AFIX 0 C54 1 0.860840 0.910861 0.142170 11.00000 0.06400 0.02505 = 0.05302 -0.00428 0.00725 -0.00998 AFIX 137 H54A 2 0.848354 0.951259 0.187095 11.00000 -1.50000 H54B 2 0.800651 0.915625 0.094700 11.00000 -1.50000 H54C 2 0.928673 0.926891 0.123614 11.00000 -1.50000 AFIX 0 PART 1 21 CL1A 4 0.167633 0.384905 0.138296 21.00000 0.05243 0.04795 = 0.06457 0.01023 0.01048 0.00047 CL2A 4 -0.033640 0.468824 0.059217 21.00000 0.08611 0.07252 = 0.08304 0.04672 0.03620 0.03544 C55A 1 0.024018 0.390387 0.131105 21.00000 0.05631 0.04852 = 0.05994 0.02275 0.00812 0.00479 AFIX 23 H55A 2 -0.007715 0.331435 0.114442 21.00000 -1.20000 H55B 2 0.006810 0.405116 0.187033 21.00000 -1.20000 AFIX 0 PART 2 -21 CL1B 4 0.134069 0.413233 0.132314 -21.00000 0.05243 0.04795 = 0.06457 0.01023 0.01048 0.00047 CL2B 4 -0.073672 0.419145 0.039098 -21.00000 0.08611 0.07252 = 0.08304 0.04672 0.03620 0.03544 C55B 1 -0.002927 0.440523 0.138493 -21.00000 0.05631 0.04852 = 0.05994 0.02275 0.00812 0.00479 AFIX 23 H55C 2 -0.029896 0.403189 0.180897 -21.00000 -1.20000 H55D 2 -0.009450 0.503850 0.153476 -21.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM MM2C_a.res in P2(1) REM wR2 = 0.041657, GooF = S = 1.08578, Restrained GooF = 1.08572 for all data REM R1 = 0.018511 for 28350 Fo > 4sig(Fo) and 0.019690 for all 29074 data REM 631 parameters refined using 3 restraints END WGHT 0.0159 1.0135 REM Highest difference peak 0.775, deepest hole -0.640, 1-sigma level 0.075 Q1 1 0.8739 0.5396 0.4587 11.00000 0.05 0.77 Q2 1 0.7056 0.3895 0.2382 11.00000 0.05 0.59 Q3 1 0.7952 0.4587 0.3377 11.00000 0.05 0.57 Q4 1 0.0607 0.4735 0.0078 11.00000 0.05 0.57 Q5 1 0.0784 0.4344 0.0773 11.00000 0.05 0.56 Q6 1 0.7834 0.5911 0.2852 11.00000 0.05 0.53 Q7 1 0.6392 0.5377 0.1803 11.00000 0.05 0.49 Q8 1 0.6791 0.5373 0.1988 11.00000 0.05 0.49 Q9 1 0.6847 0.3826 0.1958 11.00000 0.05 0.45 Q10 1 0.8990 0.6048 0.3092 11.00000 0.05 0.44 Q11 1 0.8087 0.3997 0.4107 11.00000 0.05 0.44 Q12 1 0.9302 0.6560 -0.0304 11.00000 0.05 0.43 Q13 1 0.7011 0.3576 0.2004 11.00000 0.05 0.43 Q14 1 0.7956 0.5653 0.2503 11.00000 0.05 0.42 Q15 1 0.8360 0.4527 0.3535 11.00000 0.05 0.41 Q16 1 0.5666 0.4673 0.1134 11.00000 0.05 0.41 Q17 1 0.6482 0.5512 0.1511 11.00000 0.05 0.41 Q18 1 0.8223 0.4726 0.3756 11.00000 0.05 0.41 Q19 1 0.7741 0.5970 0.2371 11.00000 0.05 0.40 Q20 1 0.8136 0.2350 0.5277 11.00000 0.05 0.39 ; _shelx_res_checksum 7615 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.83723(2) 0.59422(2) 0.27416(2) 0.01866(3) Uani 1 1 d . . . . . I2 I 0.73640(2) 0.37800(2) 0.22178(2) 0.01922(3) Uani 1 1 d . . . . . I3 I 0.90275(2) 0.53682(2) 0.50067(2) 0.01876(3) Uani 1 1 d . . . . . I4 I 0.50296(2) 0.46898(2) 0.07370(2) 0.02518(3) Uani 1 1 d . . . . . Pd1 Pd 0.81261(2) 0.45280(2) 0.36614(2) 0.01336(3) Uani 1 1 d . . . . . Pd2 Pd 0.66725(2) 0.53864(2) 0.17009(2) 0.01367(3) Uani 1 1 d . . . . . N1 N 0.74094(14) 0.33470(11) 0.49981(11) 0.0144(3) Uani 1 1 d . . . . . N2 N 0.86523(14) 0.27313(11) 0.44195(11) 0.0144(3) Uani 1 1 d . . . . . N3 N 0.52787(15) 0.70556(12) 0.14922(12) 0.0158(3) Uani 1 1 d . . . . . N4 N 0.67186(14) 0.72184(12) 0.09485(12) 0.0157(3) Uani 1 1 d . . . . . C1 C 0.80059(16) 0.34648(13) 0.43760(12) 0.0139(3) Uani 1 1 d . . . . . C2 C 0.84921(18) 0.21812(14) 0.50801(14) 0.0177(4) Uani 1 1 d . . . . . H2 H 0.886010 0.164112 0.524711 0.021 Uiso 1 1 calc R U . . . C3 C 0.77115(18) 0.25659(14) 0.54366(13) 0.0174(3) Uani 1 1 d . . . . . H3 H 0.742185 0.234386 0.590133 0.021 Uiso 1 1 calc R U . . . C4 C 0.65134(17) 0.38947(13) 0.51514(14) 0.0162(3) Uani 1 1 d . . . . . C5 C 0.55519(17) 0.38808(14) 0.45465(14) 0.0184(4) Uani 1 1 d . . . . . C6 C 0.4692(2) 0.43974(16) 0.47128(17) 0.0245(4) Uani 1 1 d . . . . . H6 H 0.403257 0.440349 0.432014 0.029 Uiso 1 1 calc R U . . . C7 C 0.4777(2) 0.49006(17) 0.54356(19) 0.0276(5) Uani 1 1 d . . . . . H7 H 0.418989 0.526714 0.552313 0.033 Uiso 1 1 calc R U . . . C8 C 0.5712(2) 0.48744(16) 0.60333(18) 0.0265(5) Uani 1 1 d . . . . . H8 H 0.574918 0.521055 0.653521 0.032 Uiso 1 1 calc R U . . . C9 C 0.66057(19) 0.43632(14) 0.59143(15) 0.0202(4) Uani 1 1 d . . . . . C10 C 0.54055(18) 0.32925(16) 0.37716(15) 0.0201(4) Uani 1 1 d . . . . . H10 H 0.613130 0.322156 0.360313 0.024 Uiso 1 1 calc R U . . . C11 C 0.4636(2) 0.3686(2) 0.30197(17) 0.0315(5) Uani 1 1 d . . . . . H11A H 0.469226 0.334453 0.251247 0.047 Uiso 1 1 calc R U . . . H11B H 0.483430 0.430642 0.294030 0.047 Uiso 1 1 calc R U . . . H11C H 0.389082 0.365896 0.312526 0.047 Uiso 1 1 calc R U . . . C12 C 0.5021(2) 0.23664(18) 0.39892(19) 0.0303(5) Uani 1 1 d . . . . . H12A H 0.495488 0.198229 0.349296 0.045 Uiso 1 1 calc R U . . . H12B H 0.431583 0.241624 0.416756 0.045 Uiso 1 1 calc R U . . . H12C H 0.554859 0.210956 0.444610 0.045 Uiso 1 1 calc R U . . . C13 C 0.7569(2) 0.42914(17) 0.66250(16) 0.0243(5) Uani 1 1 d . . . . . H13 H 0.818195 0.400627 0.640291 0.029 Uiso 1 1 calc R U . . . C14 C 0.7948(3) 0.5198(2) 0.7000(2) 0.0377(7) Uani 1 1 d . . . . . H14A H 0.862295 0.512405 0.740270 0.057 Uiso 1 1 calc R U . . . H14B H 0.739049 0.544920 0.728757 0.057 Uiso 1 1 calc R U . . . H14C H 0.807121 0.559968 0.654854 0.057 Uiso 1 1 calc R U . . . C15 C 0.7261(2) 0.3696(2) 0.73203(16) 0.0267(5) Uani 1 1 d . . . . . H15A H 0.786552 0.367375 0.779506 0.040 Uiso 1 1 calc R U . . . H15B H 0.710186 0.309492 0.709973 0.040 Uiso 1 1 calc R U . . . H15C H 0.661988 0.394043 0.750926 0.040 Uiso 1 1 calc R U . . . C16 C 0.92423(17) 0.24556(14) 0.37694(13) 0.0153(3) Uani 1 1 d . . . . . C17 C 0.87603(18) 0.17998(14) 0.32019(14) 0.0181(4) Uani 1 1 d . . . . . C18 C 0.9316(2) 0.15562(16) 0.25603(15) 0.0235(4) Uani 1 1 d . . . . . H18 H 0.901172 0.112140 0.216171 0.028 Uiso 1 1 calc R U . . . C19 C 1.0303(2) 0.19358(17) 0.24932(16) 0.0262(5) Uani 1 1 d . . . . . H19 H 1.066391 0.176497 0.204749 0.031 Uiso 1 1 calc R U . . . C20 C 1.0768(2) 0.25638(17) 0.30733(17) 0.0241(4) Uani 1 1 d . . . . . H20 H 1.145362 0.280895 0.302719 0.029 Uiso 1 1 calc R U . . . C21 C 1.02478(17) 0.28426(14) 0.37239(14) 0.0176(3) Uani 1 1 d . . . . . C22 C 0.77053(19) 0.13280(16) 0.32813(15) 0.0213(4) Uani 1 1 d . . . . . H22 H 0.733822 0.167852 0.367640 0.026 Uiso 1 1 calc R U . . . C23 C 0.6918(2) 0.12394(19) 0.24466(19) 0.0306(5) Uani 1 1 d . . . . . H23A H 0.680099 0.182449 0.217972 0.046 Uiso 1 1 calc R U . . . H23B H 0.622619 0.100236 0.255131 0.046 Uiso 1 1 calc R U . . . H23C H 0.722456 0.083457 0.207440 0.046 Uiso 1 1 calc R U . . . C24 C 0.7953(2) 0.04004(19) 0.36585(16) 0.0263(4) Uani 1 1 d . . . . . H24A H 0.841095 0.045487 0.421367 0.039 Uiso 1 1 calc R U . . . H24B H 0.833370 0.005061 0.328882 0.039 Uiso 1 1 calc R U . . . H24C H 0.727429 0.010270 0.371405 0.039 Uiso 1 1 calc R U . . . C25 C 1.07944(18) 0.35159(15) 0.43612(15) 0.0205(4) Uani 1 1 d . . . . . H25 H 1.023812 0.374456 0.468213 0.025 Uiso 1 1 calc R U . . . C26 C 1.1244(2) 0.43101(18) 0.3936(2) 0.0302(5) Uani 1 1 d . . . . . H26A H 1.159247 0.472606 0.436689 0.045 Uiso 1 1 calc R U . . . H26B H 1.064955 0.461164 0.356756 0.045 Uiso 1 1 calc R U . . . H26C H 1.177588 0.410025 0.360312 0.045 Uiso 1 1 calc R U . . . C27 C 1.1693(3) 0.3072(2) 0.4986(2) 0.0373(7) Uani 1 1 d . . . . . H27A H 1.200030 0.350351 0.541734 0.056 Uiso 1 1 calc R U . . . H27B H 1.226192 0.286112 0.468903 0.056 Uiso 1 1 calc R U . . . H27C H 1.139251 0.256814 0.525342 0.056 Uiso 1 1 calc R U . . . C28 C 0.61822(16) 0.66164(13) 0.13553(12) 0.0139(3) Uani 1 1 d . . . . . C29 C 0.61545(19) 0.80125(15) 0.08262(16) 0.0223(4) Uani 1 1 d . . . . . H29 H 0.635800 0.852758 0.055134 0.027 Uiso 1 1 calc R U . . . C30 C 0.52579(19) 0.79106(16) 0.11746(16) 0.0224(4) Uani 1 1 d . . . . . H30 H 0.471413 0.834529 0.119728 0.027 Uiso 1 1 calc R U . . . C31 C 0.44240(17) 0.67091(15) 0.18911(14) 0.0170(3) Uani 1 1 d . . . . . C32 C 0.34052(19) 0.65495(17) 0.13934(15) 0.0220(4) Uani 1 1 d . . . . . C33 C 0.2589(2) 0.62282(19) 0.18058(18) 0.0270(5) Uani 1 1 d . . . . . H33 H 0.188595 0.612082 0.149274 0.032 Uiso 1 1 calc R U . . . C34 C 0.2790(2) 0.60653(18) 0.26598(18) 0.0263(5) Uani 1 1 d . . . . . H34 H 0.223161 0.582949 0.292410 0.032 Uiso 1 1 calc R U . . . C35 C 0.3798(2) 0.62422(16) 0.31350(16) 0.0215(4) Uani 1 1 d . . . . . H35 H 0.392097 0.612909 0.372255 0.026 Uiso 1 1 calc R U . . . C36 C 0.46355(17) 0.65848(14) 0.27625(14) 0.0165(3) Uani 1 1 d . . . . . C37 C 0.3160(2) 0.6725(2) 0.04532(17) 0.0321(6) Uani 1 1 d . . . . . H37 H 0.386487 0.675472 0.024445 0.039 Uiso 1 1 calc R U . . . C38 C 0.2478(3) 0.5985(3) -0.0029(2) 0.0486(10) Uani 1 1 d . . . . . H38A H 0.241192 0.609001 -0.063421 0.073 Uiso 1 1 calc R U . . . H38B H 0.175639 0.598182 0.012558 0.073 Uiso 1 1 calc R U . . . H38C H 0.283042 0.541050 0.011431 0.073 Uiso 1 1 calc R U . . . C39 C 0.2581(3) 0.7632(3) 0.0271(2) 0.0406(8) Uani 1 1 d . . . . . H39A H 0.245579 0.774782 -0.033507 0.061 Uiso 1 1 calc R U . . . H39B H 0.303467 0.810470 0.056513 0.061 Uiso 1 1 calc R U . . . H39C H 0.188466 0.761787 0.046851 0.061 Uiso 1 1 calc R U . . . C40 C 0.56944(18) 0.68849(14) 0.32910(14) 0.0180(4) Uani 1 1 d . . . . . H40 H 0.626755 0.685015 0.293247 0.022 Uiso 1 1 calc R U . . . C41 C 0.6060(2) 0.63154(18) 0.40691(15) 0.0245(4) Uani 1 1 d . . . . . H41A H 0.678583 0.650094 0.434244 0.037 Uiso 1 1 calc R U . . . H41B H 0.607748 0.568963 0.390382 0.037 Uiso 1 1 calc R U . . . H41C H 0.555211 0.638955 0.446121 0.037 Uiso 1 1 calc R U . . . C42 C 0.5587(2) 0.78604(17) 0.35379(18) 0.0277(5) Uani 1 1 d . . . . . H42A H 0.628365 0.807295 0.384554 0.042 Uiso 1 1 calc R U . . . H42B H 0.503483 0.791247 0.389612 0.042 Uiso 1 1 calc R U . . . H42C H 0.537392 0.821941 0.302971 0.042 Uiso 1 1 calc R U . . . C43 C 0.77043(17) 0.70721(14) 0.06243(14) 0.0175(3) Uani 1 1 d . . . . . C44 C 0.7652(2) 0.65605(16) -0.01036(15) 0.0222(4) Uani 1 1 d . . . . . C45 C 0.8614(3) 0.6459(2) -0.0421(2) 0.0331(6) Uani 1 1 d . . . . . H45 H 0.861521 0.610505 -0.090813 0.040 Uiso 1 1 calc R U . . . C46 C 0.9561(3) 0.6864(2) -0.0042(2) 0.0405(7) Uani 1 1 d . . . . . H46 H 1.020381 0.678398 -0.026884 0.049 Uiso 1 1 calc R U . . . C47 C 0.9584(2) 0.7384(2) 0.0665(2) 0.0365(6) Uani 1 1 d . . . . . H47 H 1.024373 0.765946 0.091615 0.044 Uiso 1 1 calc R U . . . C48 C 0.8651(2) 0.75118(17) 0.10198(17) 0.0246(4) Uani 1 1 d . . . . . C49 C 0.6597(2) 0.61993(19) -0.05856(16) 0.0288(5) Uani 1 1 d . . . . . H49 H 0.605406 0.619206 -0.019982 0.035 Uiso 1 1 calc R U . . . C50 C 0.6721(4) 0.5253(2) -0.0894(2) 0.0523(10) Uani 1 1 d . . . . . H50A H 0.601436 0.503151 -0.117447 0.078 Uiso 1 1 calc R U . . . H50B H 0.699788 0.486976 -0.041352 0.078 Uiso 1 1 calc R U . . . H50C H 0.722889 0.524938 -0.129058 0.078 Uiso 1 1 calc R U . . . C51 C 0.6181(3) 0.6826(3) -0.1320(2) 0.0499(10) Uani 1 1 d . . . . . H51A H 0.546491 0.662725 -0.160303 0.075 Uiso 1 1 calc R U . . . H51B H 0.668499 0.681998 -0.172027 0.075 Uiso 1 1 calc R U . . . H51C H 0.612661 0.743072 -0.110629 0.075 Uiso 1 1 calc R U . . . C52 C 0.8684(2) 0.8149(2) 0.17525(19) 0.0325(6) Uani 1 1 d . . . . . H52 H 0.803866 0.803104 0.202219 0.039 Uiso 1 1 calc R U . . . C53 C 0.9705(3) 0.8064(3) 0.2428(2) 0.0506(10) Uani 1 1 d . . . . . H53A H 0.960759 0.840204 0.292758 0.076 Uiso 1 1 calc R U . . . H53B H 1.033023 0.829797 0.220886 0.076 Uiso 1 1 calc R U . . . H53C H 0.982917 0.743659 0.257804 0.076 Uiso 1 1 calc R U . . . C54 C 0.8608(4) 0.9109(2) 0.1422(3) 0.0477(9) Uani 1 1 d . . . . . H54A H 0.848354 0.951259 0.187095 0.072 Uiso 1 1 calc R U . . . H54B H 0.800651 0.915625 0.094700 0.072 Uiso 1 1 calc R U . . . H54C H 0.928673 0.926891 0.123614 0.072 Uiso 1 1 calc R U . . . Cl1A Cl 0.16763(12) 0.38491(10) 0.13830(9) 0.0550(3) Uani 0.893(3) 1 d D . P A 1 Cl2A Cl -0.03364(15) 0.46882(13) 0.05922(11) 0.0780(6) Uani 0.893(3) 1 d D . P A 1 C55A C 0.0240(4) 0.3904(4) 0.1311(3) 0.0552(12) Uani 0.893(3) 1 d D . P A 1 H55A H -0.007715 0.331435 0.114442 0.066 Uiso 0.893(3) 1 calc R U P A 1 H55B H 0.006810 0.405116 0.187033 0.066 Uiso 0.893(3) 1 calc R U P A 1 Cl1B Cl 0.1341(10) 0.4132(9) 0.1323(9) 0.0550(3) Uani 0.107(3) 1 d D . P A 2 Cl2B Cl -0.0737(13) 0.4191(11) 0.0391(9) 0.0780(6) Uani 0.107(3) 1 d D . P A 2 C55B C -0.0029(12) 0.441(3) 0.1385(13) 0.0552(12) Uani 0.107(3) 1 d D . P A 2 H55C H -0.029896 0.403189 0.180897 0.066 Uiso 0.107(3) 1 calc R U P A 2 H55D H -0.009450 0.503850 0.153476 0.066 Uiso 0.107(3) 1 calc R U P A 2 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 I1 0.01854(6) 0.01461(5) 0.02171(6) 0.00385(4) 0.00042(5) -0.00056(4) I2 0.02910(7) 0.01175(5) 0.01652(6) 0.00036(4) 0.00317(5) 0.00198(5) I3 0.01945(5) 0.01595(5) 0.02071(6) -0.00214(5) 0.00303(4) -0.00197(5) I4 0.02944(7) 0.02174(7) 0.02152(7) -0.00133(5) -0.00345(5) -0.00810(5) Pd1 0.01449(6) 0.01056(5) 0.01530(6) 0.00059(4) 0.00333(4) 0.00125(4) Pd2 0.01668(6) 0.01104(5) 0.01323(6) 0.00012(5) 0.00245(4) -0.00001(5) N1 0.0163(7) 0.0122(7) 0.0152(7) -0.0003(5) 0.0047(6) 0.0008(5) N2 0.0167(7) 0.0127(7) 0.0140(7) -0.0008(5) 0.0034(6) 0.0030(5) N3 0.0149(7) 0.0158(7) 0.0172(8) 0.0017(6) 0.0039(6) 0.0029(6) N4 0.0161(7) 0.0137(7) 0.0179(8) 0.0028(6) 0.0048(6) 0.0017(6) C1 0.0144(7) 0.0131(7) 0.0143(8) -0.0025(6) 0.0028(6) 0.0001(6) C2 0.0216(9) 0.0151(8) 0.0169(9) 0.0023(6) 0.0046(7) 0.0038(7) C3 0.0222(9) 0.0150(8) 0.0155(8) 0.0016(6) 0.0051(7) 0.0012(7) C4 0.0177(8) 0.0119(7) 0.0208(9) -0.0010(6) 0.0084(7) 0.0007(6) C5 0.0179(8) 0.0153(8) 0.0233(9) 0.0027(7) 0.0070(7) 0.0012(7) C6 0.0212(9) 0.0220(10) 0.0327(12) 0.0080(9) 0.0111(9) 0.0056(8) C7 0.0284(11) 0.0200(10) 0.0395(14) 0.0045(9) 0.0195(10) 0.0078(8) C8 0.0333(12) 0.0177(9) 0.0335(13) -0.0034(8) 0.0201(10) 0.0019(8) C9 0.0244(10) 0.0149(8) 0.0238(10) -0.0036(7) 0.0113(8) -0.0027(7) C10 0.0178(9) 0.0213(9) 0.0211(10) 0.0026(7) 0.0027(7) -0.0011(7) C11 0.0304(12) 0.0358(14) 0.0249(12) 0.0060(10) -0.0045(9) 0.0017(11) C12 0.0366(14) 0.0219(11) 0.0330(13) -0.0014(9) 0.0077(11) -0.0080(10) C13 0.0267(11) 0.0259(11) 0.0226(10) -0.0109(8) 0.0103(8) -0.0086(9) C14 0.0470(16) 0.0348(15) 0.0359(14) -0.0191(12) 0.0196(13) -0.0196(13) C15 0.0277(11) 0.0327(13) 0.0205(10) -0.0044(9) 0.0068(8) -0.0026(10) C16 0.0177(8) 0.0145(8) 0.0140(8) 0.0013(6) 0.0034(6) 0.0052(6) C17 0.0221(9) 0.0149(8) 0.0170(9) -0.0016(7) 0.0026(7) 0.0047(7) C18 0.0335(12) 0.0188(9) 0.0192(10) -0.0034(7) 0.0079(9) 0.0059(8) C19 0.0355(13) 0.0224(10) 0.0244(11) -0.0007(8) 0.0156(10) 0.0073(9) C20 0.0261(11) 0.0213(10) 0.0284(11) 0.0013(8) 0.0144(9) 0.0054(8) C21 0.0173(8) 0.0159(8) 0.0203(9) 0.0017(7) 0.0049(7) 0.0054(7) C22 0.0208(9) 0.0202(9) 0.0225(10) -0.0042(8) 0.0022(8) 0.0023(7) C23 0.0321(13) 0.0234(11) 0.0314(13) -0.0014(9) -0.0081(10) -0.0012(10) C24 0.0272(10) 0.0250(10) 0.0268(11) 0.0032(10) 0.0048(8) -0.0014(9) C25 0.0170(9) 0.0191(9) 0.0251(10) 0.0001(7) 0.0031(7) 0.0016(7) C26 0.0291(12) 0.0228(11) 0.0415(15) -0.0012(10) 0.0143(11) -0.0044(9) C27 0.0317(13) 0.0302(14) 0.0439(17) -0.0018(12) -0.0109(12) 0.0057(11) C28 0.0147(8) 0.0141(7) 0.0126(8) -0.0001(6) 0.0012(6) 0.0001(6) C29 0.0233(10) 0.0161(9) 0.0285(11) 0.0073(8) 0.0071(8) 0.0042(7) C30 0.0218(10) 0.0180(9) 0.0283(11) 0.0065(8) 0.0067(8) 0.0071(8) C31 0.0150(8) 0.0185(9) 0.0181(9) -0.0017(7) 0.0040(7) 0.0004(7) C32 0.0170(9) 0.0276(11) 0.0215(10) -0.0051(8) 0.0034(7) 0.0004(8) C33 0.0182(10) 0.0298(12) 0.0336(13) -0.0076(10) 0.0056(9) -0.0044(8) C34 0.0219(10) 0.0240(11) 0.0355(13) -0.0016(9) 0.0123(9) -0.0057(8) C35 0.0245(10) 0.0185(9) 0.0234(10) 0.0001(7) 0.0091(8) -0.0002(8) C36 0.0175(8) 0.0141(8) 0.0185(9) -0.0006(6) 0.0046(7) 0.0016(6) C37 0.0187(10) 0.0572(19) 0.0196(11) -0.0034(11) 0.0008(8) 0.0029(11) C38 0.0282(13) 0.078(3) 0.0355(16) -0.0251(18) -0.0067(12) 0.0053(16) C39 0.0256(13) 0.061(2) 0.0341(15) 0.0150(14) 0.0014(11) 0.0041(13) C40 0.0183(9) 0.0174(8) 0.0179(9) -0.0017(7) 0.0024(7) 0.0024(7) C41 0.0282(11) 0.0253(11) 0.0190(10) 0.0022(8) 0.0017(8) 0.0051(9) C42 0.0257(11) 0.0186(10) 0.0346(13) -0.0054(9) -0.0064(9) 0.0021(8) C43 0.0164(8) 0.0163(8) 0.0205(9) 0.0034(7) 0.0057(7) 0.0015(7) C44 0.0277(11) 0.0197(9) 0.0214(10) 0.0019(7) 0.0107(8) 0.0008(8) C45 0.0388(15) 0.0308(13) 0.0348(14) 0.0022(11) 0.0206(12) 0.0074(11) C46 0.0269(13) 0.0450(17) 0.055(2) 0.0045(15) 0.0226(13) 0.0064(12) C47 0.0192(11) 0.0422(16) 0.0496(18) 0.0068(14) 0.0097(11) -0.0019(11) C48 0.0201(10) 0.0233(10) 0.0303(12) 0.0060(9) 0.0043(8) -0.0014(8) C49 0.0408(14) 0.0277(12) 0.0189(10) -0.0026(8) 0.0078(10) -0.0104(10) C50 0.082(3) 0.0385(19) 0.0446(18) -0.0208(15) 0.0342(19) -0.0240(18) C51 0.055(2) 0.058(2) 0.0304(15) 0.0141(15) -0.0099(14) -0.0192(18) C52 0.0334(13) 0.0305(13) 0.0319(13) 0.0000(10) 0.0013(10) -0.0115(11) C53 0.0453(18) 0.056(2) 0.0434(18) 0.0079(16) -0.0110(15) -0.0295(17) C54 0.064(2) 0.0250(14) 0.053(2) -0.0043(13) 0.0072(18) -0.0100(15) Cl1A 0.0524(7) 0.0480(7) 0.0646(7) 0.0102(6) 0.0105(5) 0.0005(5) Cl2A 0.0861(11) 0.0725(11) 0.0830(10) 0.0467(9) 0.0362(8) 0.0354(9) C55A 0.056(3) 0.049(3) 0.060(3) 0.023(2) 0.008(2) 0.005(2) Cl1B 0.0524(7) 0.0480(7) 0.0646(7) 0.0102(6) 0.0105(5) 0.0005(5) Cl2B 0.0861(11) 0.0725(11) 0.0830(10) 0.0467(9) 0.0362(8) 0.0354(9) C55B 0.056(3) 0.049(3) 0.060(3) 0.023(2) 0.008(2) 0.005(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' I I -0.4742 1.8119 '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 Pd2 I1 Pd1 86.662(6) . . ? Pd1 I2 Pd2 86.388(6) . . ? C1 Pd1 I3 88.39(6) . . ? C1 Pd1 I2 96.79(6) . . ? I3 Pd1 I2 173.611(8) . . ? C1 Pd1 I1 177.61(6) . . ? I3 Pd1 I1 90.116(7) . . ? I2 Pd1 I1 84.579(6) . . ? C28 Pd2 I4 91.92(6) . . ? C28 Pd2 I1 93.43(6) . . ? I4 Pd2 I1 174.534(8) . . ? C28 Pd2 I2 177.70(6) . . ? I4 Pd2 I2 90.134(7) . . ? I1 Pd2 I2 84.496(6) . . ? C1 N1 C3 110.45(17) . . ? C1 N1 C4 126.35(17) . . ? C3 N1 C4 122.96(17) . . ? C1 N2 C2 110.88(17) . . ? C1 N2 C16 124.70(17) . . ? C2 N2 C16 123.11(17) . . ? C28 N3 C30 110.68(18) . . ? C28 N3 C31 126.97(18) . . ? C30 N3 C31 122.34(18) . . ? C28 N4 C29 111.06(18) . . ? C28 N4 C43 126.89(18) . . ? C29 N4 C43 121.94(18) . . ? N2 C1 N1 104.72(17) . . ? N2 C1 Pd1 125.08(14) . . ? N1 C1 Pd1 129.57(14) . . ? C3 C2 N2 106.53(18) . . ? C3 C2 H2 126.7 . . ? N2 C2 H2 126.7 . . ? C2 C3 N1 107.37(18) . . ? C2 C3 H3 126.3 . . ? N1 C3 H3 126.3 . . ? C9 C4 C5 122.88(19) . . ? C9 C4 N1 119.1(2) . . ? C5 C4 N1 117.81(18) . . ? C6 C5 C4 117.0(2) . . ? C6 C5 C10 119.9(2) . . ? C4 C5 C10 122.99(19) . . ? C7 C6 C5 121.4(2) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 120.4(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.4(2) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 116.8(2) . . ? C8 C9 C13 119.0(2) . . ? C4 C9 C13 124.0(2) . . ? C5 C10 C11 113.4(2) . . ? C5 C10 C12 109.8(2) . . ? C11 C10 C12 110.7(2) . . ? C5 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 112.7(2) . . ? C9 C13 C15 109.0(2) . . ? C14 C13 C15 109.2(2) . . ? C9 C13 H13 108.6 . . ? C14 C13 H13 108.6 . . ? C15 C13 H13 108.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 122.96(19) . . ? C21 C16 N2 119.82(19) . . ? C17 C16 N2 117.23(19) . . ? C18 C17 C16 117.0(2) . . ? C18 C17 C22 119.5(2) . . ? C16 C17 C22 123.40(19) . . ? C19 C18 C17 121.3(2) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.3(2) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 121.2(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 117.2(2) . . ? C20 C21 C25 119.7(2) . . ? C16 C21 C25 122.99(19) . . ? C17 C22 C23 113.6(2) . . ? C17 C22 C24 109.77(19) . . ? C23 C22 C24 109.0(2) . . ? C17 C22 H22 108.1 . . ? C23 C22 H22 108.1 . . ? C24 C22 H22 108.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 110.5(2) . . ? C21 C25 C26 111.9(2) . . ? C27 C25 C26 110.5(2) . . ? C21 C25 H25 107.9 . . ? C27 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? 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 . . ? N3 C28 N4 104.48(17) . . ? N3 C28 Pd2 128.88(15) . . ? N4 C28 Pd2 126.60(15) . . ? C30 C29 N4 106.50(19) . . ? C30 C29 H29 126.7 . . ? N4 C29 H29 126.7 . . ? C29 C30 N3 107.27(19) . . ? C29 C30 H30 126.4 . . ? N3 C30 H30 126.4 . . ? C36 C31 C32 123.1(2) . . ? C36 C31 N3 118.26(19) . . ? C32 C31 N3 118.6(2) . . ? C33 C32 C31 117.0(2) . . ? C33 C32 C37 119.9(2) . . ? C31 C32 C37 123.1(2) . . ? C34 C33 C32 121.0(2) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 120.6(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 120.9(2) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 117.3(2) . . ? C35 C36 C40 121.2(2) . . ? C31 C36 C40 121.35(19) . . ? C32 C37 C38 112.3(3) . . ? C32 C37 C39 110.4(2) . . ? C38 C37 C39 110.0(3) . . ? C32 C37 H37 108.0 . . ? C38 C37 H37 108.0 . . ? C39 C37 H37 108.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 C41 113.87(19) . . ? C36 C40 C42 108.87(18) . . ? C41 C40 C42 110.6(2) . . ? C36 C40 H40 107.8 . . ? C41 C40 H40 107.8 . . ? C42 C40 H40 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 123.5(2) . . ? C44 C43 N4 118.2(2) . . ? C48 C43 N4 118.1(2) . . ? C43 C44 C45 116.9(2) . . ? C43 C44 C49 122.6(2) . . ? C45 C44 C49 120.3(2) . . ? C46 C45 C44 121.2(3) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C45 C46 C47 120.7(3) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C46 C47 C48 121.1(3) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 116.5(3) . . ? C47 C48 C52 119.6(3) . . ? C43 C48 C52 123.7(2) . . ? C44 C49 C50 111.9(3) . . ? C44 C49 C51 109.0(2) . . ? C50 C49 C51 111.2(3) . . ? C44 C49 H49 108.2 . . ? C50 C49 H49 108.2 . . ? C51 C49 H49 108.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 C53 114.0(3) . . ? C48 C52 C54 109.3(3) . . ? C53 C52 C54 108.6(3) . . ? C48 C52 H52 108.3 . . ? C53 C52 H52 108.3 . . ? C54 C52 H52 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl2A C55A Cl1A 112.0(3) . . ? Cl2A C55A H55A 109.2 . . ? Cl1A C55A H55A 109.2 . . ? Cl2A C55A H55B 109.2 . . ? Cl1A C55A H55B 109.2 . . ? H55A C55A H55B 107.9 . . ? Cl2B C55B Cl1B 104.4(11) . . ? Cl2B C55B H55C 110.9 . . ? Cl1B C55B H55C 110.9 . . ? Cl2B C55B H55D 110.9 . . ? Cl1B C55B H55D 110.9 . . ? H55C C55B H55D 108.9 . . ? 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 I1 Pd2 2.6106(2) . ? I1 Pd1 2.6442(2) . ? I2 Pd1 2.6152(2) . ? I2 Pd2 2.6530(2) . ? I3 Pd1 2.5962(2) . ? I4 Pd2 2.5778(2) . ? Pd1 C1 1.994(2) . ? Pd2 C28 1.999(2) . ? N1 C1 1.365(3) . ? N1 C3 1.390(3) . ? N1 C4 1.449(3) . ? N2 C1 1.364(3) . ? N2 C2 1.393(3) . ? N2 C16 1.447(3) . ? N3 C28 1.362(3) . ? N3 C30 1.384(3) . ? N3 C31 1.441(3) . ? N4 C28 1.364(3) . ? N4 C29 1.385(3) . ? N4 C43 1.441(3) . ? C2 C3 1.350(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.407(3) . ? C4 C5 1.413(3) . ? C5 C6 1.393(3) . ? C5 C10 1.518(3) . ? C6 C7 1.380(4) . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 H7 0.9500 . ? C8 C9 1.399(3) . ? C8 H8 0.9500 . ? C9 C13 1.518(4) . ? C10 C11 1.532(3) . ? C10 C12 1.535(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.534(4) . ? C13 C15 1.538(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.402(3) . ? C16 C17 1.409(3) . ? C17 C18 1.396(3) . ? C17 C22 1.526(3) . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C25 1.520(3) . ? C22 C23 1.531(4) . ? C22 C24 1.533(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.529(4) . ? C25 C26 1.533(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.351(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.399(3) . ? C31 C32 1.406(3) . ? C32 C33 1.401(4) . ? C32 C37 1.519(4) . ? C33 C34 1.380(4) . ? C33 H33 0.9500 . ? C34 C35 1.385(4) . ? C34 H34 0.9500 . ? C35 C36 1.397(3) . ? C35 H35 0.9500 . ? C36 C40 1.516(3) . ? C37 C38 1.531(5) . ? C37 C39 1.551(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.524(3) . ? C40 C42 1.533(3) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.397(3) . ? C43 C48 1.411(3) . ? C44 C45 1.399(4) . ? C44 C49 1.514(4) . ? C45 C46 1.379(5) . ? C45 H45 0.9500 . ? C46 C47 1.380(5) . ? C46 H46 0.9500 . ? C47 C48 1.403(4) . ? C47 H47 0.9500 . ? C48 C52 1.518(4) . ? C49 C50 1.525(4) . ? C49 C51 1.534(4) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.535(5) . ? C52 C54 1.536(5) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Cl1A C55A 1.786(5) . ? Cl2A C55A 1.724(4) . ? C55A H55A 0.9900 . ? C55A H55B 0.9900 . ? Cl1B C55B 1.786(6) . ? Cl2B C55B 1.724(5) . ? C55B H55C 0.9900 . ? C55B H55D 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 -2.3(2) . . . . ? C16 N2 C1 N1 164.91(19) . . . . ? C2 N2 C1 Pd1 169.33(15) . . . . ? C16 N2 C1 Pd1 -23.4(3) . . . . ? C3 N1 C1 N2 2.0(2) . . . . ? C4 N1 C1 N2 -172.53(19) . . . . ? C3 N1 C1 Pd1 -169.14(16) . . . . ? C4 N1 C1 Pd1 16.3(3) . . . . ? C1 N2 C2 C3 1.8(2) . . . . ? C16 N2 C2 C3 -165.7(2) . . . . ? N2 C2 C3 N1 -0.5(2) . . . . ? C1 N1 C3 C2 -1.0(2) . . . . ? C4 N1 C3 C2 173.79(19) . . . . ? C1 N1 C4 C9 -117.0(2) . . . . ? C3 N1 C4 C9 69.1(3) . . . . ? C1 N1 C4 C5 67.5(3) . . . . ? C3 N1 C4 C5 -106.4(2) . . . . ? C9 C4 C5 C6 3.4(3) . . . . ? N1 C4 C5 C6 178.73(19) . . . . ? C9 C4 C5 C10 -172.7(2) . . . . ? N1 C4 C5 C10 2.7(3) . . . . ? C4 C5 C6 C7 0.1(3) . . . . ? C10 C5 C6 C7 176.3(2) . . . . ? C5 C6 C7 C8 -2.7(4) . . . . ? C6 C7 C8 C9 1.9(4) . . . . ? C7 C8 C9 C4 1.3(3) . . . . ? C7 C8 C9 C13 -174.3(2) . . . . ? C5 C4 C9 C8 -4.1(3) . . . . ? N1 C4 C9 C8 -179.35(19) . . . . ? C5 C4 C9 C13 171.4(2) . . . . ? N1 C4 C9 C13 -3.9(3) . . . . ? C6 C5 C10 C11 33.7(3) . . . . ? C4 C5 C10 C11 -150.4(2) . . . . ? C6 C5 C10 C12 -90.7(3) . . . . ? C4 C5 C10 C12 85.3(3) . . . . ? C8 C9 C13 C14 -48.9(3) . . . . ? C4 C9 C13 C14 135.8(2) . . . . ? C8 C9 C13 C15 72.6(3) . . . . ? C4 C9 C13 C15 -102.7(2) . . . . ? C1 N2 C16 C21 82.7(3) . . . . ? C2 N2 C16 C21 -111.5(2) . . . . ? C1 N2 C16 C17 -97.0(2) . . . . ? C2 N2 C16 C17 68.7(3) . . . . ? C21 C16 C17 C18 -1.7(3) . . . . ? N2 C16 C17 C18 178.05(19) . . . . ? C21 C16 C17 C22 175.6(2) . . . . ? N2 C16 C17 C22 -4.6(3) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C22 C17 C18 C19 -176.6(2) . . . . ? C17 C18 C19 C20 0.7(4) . . . . ? C18 C19 C20 C21 -1.4(4) . . . . ? C19 C20 C21 C16 0.5(3) . . . . ? C19 C20 C21 C25 178.5(2) . . . . ? C17 C16 C21 C20 1.0(3) . . . . ? N2 C16 C21 C20 -178.68(19) . . . . ? C17 C16 C21 C25 -176.8(2) . . . . ? N2 C16 C21 C25 3.4(3) . . . . ? C18 C17 C22 C23 -46.7(3) . . . . ? C16 C17 C22 C23 136.0(2) . . . . ? C18 C17 C22 C24 75.6(3) . . . . ? C16 C17 C22 C24 -101.6(2) . . . . ? C20 C21 C25 C27 -76.2(3) . . . . ? C16 C21 C25 C27 101.7(3) . . . . ? C20 C21 C25 C26 47.4(3) . . . . ? C16 C21 C25 C26 -134.7(2) . . . . ? C30 N3 C28 N4 0.1(2) . . . . ? C31 N3 C28 N4 178.84(19) . . . . ? C30 N3 C28 Pd2 177.92(17) . . . . ? C31 N3 C28 Pd2 -3.4(3) . . . . ? C29 N4 C28 N3 -0.7(2) . . . . ? C43 N4 C28 N3 -176.8(2) . . . . ? C29 N4 C28 Pd2 -178.55(16) . . . . ? C43 N4 C28 Pd2 5.3(3) . . . . ? C28 N4 C29 C30 1.0(3) . . . . ? C43 N4 C29 C30 177.3(2) . . . . ? N4 C29 C30 N3 -0.9(3) . . . . ? C28 N3 C30 C29 0.5(3) . . . . ? C31 N3 C30 C29 -178.3(2) . . . . ? C28 N3 C31 C36 73.2(3) . . . . ? C30 N3 C31 C36 -108.2(3) . . . . ? C28 N3 C31 C32 -109.6(3) . . . . ? C30 N3 C31 C32 69.0(3) . . . . ? C36 C31 C32 C33 -1.8(4) . . . . ? N3 C31 C32 C33 -178.9(2) . . . . ? C36 C31 C32 C37 177.1(2) . . . . ? N3 C31 C32 C37 0.0(4) . . . . ? C31 C32 C33 C34 -1.0(4) . . . . ? C37 C32 C33 C34 -179.9(3) . . . . ? C32 C33 C34 C35 2.0(4) . . . . ? C33 C34 C35 C36 -0.3(4) . . . . ? C34 C35 C36 C31 -2.3(3) . . . . ? C34 C35 C36 C40 172.5(2) . . . . ? C32 C31 C36 C35 3.4(3) . . . . ? N3 C31 C36 C35 -179.55(19) . . . . ? C32 C31 C36 C40 -171.4(2) . . . . ? N3 C31 C36 C40 5.7(3) . . . . ? C33 C32 C37 C38 -42.9(4) . . . . ? C31 C32 C37 C38 138.3(3) . . . . ? C33 C32 C37 C39 80.3(3) . . . . ? C31 C32 C37 C39 -98.5(3) . . . . ? C35 C36 C40 C41 36.2(3) . . . . ? C31 C36 C40 C41 -149.3(2) . . . . ? C35 C36 C40 C42 -87.7(3) . . . . ? C31 C36 C40 C42 86.9(3) . . . . ? C28 N4 C43 C44 73.6(3) . . . . ? C29 N4 C43 C44 -102.1(3) . . . . ? C28 N4 C43 C48 -111.4(3) . . . . ? C29 N4 C43 C48 72.9(3) . . . . ? C48 C43 C44 C45 2.9(4) . . . . ? N4 C43 C44 C45 177.6(2) . . . . ? C48 C43 C44 C49 -171.4(2) . . . . ? N4 C43 C44 C49 3.4(3) . . . . ? C43 C44 C45 C46 -1.4(4) . . . . ? C49 C44 C45 C46 172.9(3) . . . . ? C44 C45 C46 C47 -0.1(5) . . . . ? C45 C46 C47 C48 0.3(5) . . . . ? C46 C47 C48 C43 1.0(4) . . . . ? C46 C47 C48 C52 -174.9(3) . . . . ? C44 C43 C48 C47 -2.7(4) . . . . ? N4 C43 C48 C47 -177.4(2) . . . . ? C44 C43 C48 C52 173.0(2) . . . . ? N4 C43 C48 C52 -1.7(3) . . . . ? C43 C44 C49 C50 -139.6(3) . . . . ? C45 C44 C49 C50 46.4(3) . . . . ? C43 C44 C49 C51 97.0(3) . . . . ? C45 C44 C49 C51 -77.1(4) . . . . ? C47 C48 C52 C53 -43.8(4) . . . . ? C43 C48 C52 C53 140.7(3) . . . . ? C47 C48 C52 C54 78.0(4) . . . . ? C43 C48 C52 C54 -97.6(3) . . . . ?