#------------------------------------------------------------------------------ #$Date: 2025-05-14 02:59:23 +0100 (Wed, 14 May 2025) $ #$Revision: 299652 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023503.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_2023503 loop_ _publ_author_name 'Bosch, Eric' _publ_section_title ; Phenyl palladium(II) iodide complexes isolated after Sonogashira coupling of iodobenzenes with terminal alkynes ; _journal_coeditor_code JY2058 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025004025 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac '[Pd (C6 H2 F3) I (C18 H15 P)2], 2C H2 Cl2' _chemical_formula_moiety 'C42 H30 F3 I3 P2 Pd, 2(C H2 Cl2)' _chemical_formula_sum 'C44 H34 Cl4 F3 I3 P2 Pd' _chemical_formula_weight 1310.642 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_primary iterative _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 76.4260(10) _cell_angle_beta 77.7220(10) _cell_angle_gamma 81.3440(10) _cell_formula_units_Z 2 _cell_length_a 11.5608(5) _cell_length_b 11.6437(5) _cell_length_c 18.1311(8) _cell_measurement_reflns_used 9954 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.15 _cell_measurement_theta_min 2.35 _cell_volume 2305.16(17) _computing_molecular_graphics ; X-SEED 4 (Barbour, 2020) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement ; olex2.refine 1.5 (Bourhis et al., 2015) ; _computing_structure_solution ; olex2.solve 1.5 (Bourhis et al., 2015) ; _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.9989 _diffrn_measured_fraction_theta_max 0.9896 _diffrn_measurement_device_type 'Bruker APEXI CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 28953 _diffrn_reflns_theta_full 25.2417 _diffrn_reflns_theta_max 27.16 _diffrn_reflns_theta_min 1.18 _exptl_absorpt_coefficient_mu 2.756 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'clear orange' _exptl_crystal_density_diffrn 1.888 _exptl_crystal_description block _exptl_crystal_F_000 1253.792 _exptl_crystal_size_max 0.234 _exptl_crystal_size_mid 0.114 _exptl_crystal_size_min 0.098 _refine_diff_density_max 1.0601 _refine_diff_density_min -1.0272 _refine_ls_goodness_of_fit_ref 1.0564 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 70 _refine_ls_number_parameters 542 _refine_ls_number_reflns 10132 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.0563 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0299 _refine_ls_shift/su_max -0.0002 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+4.2389P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.0618 _reflns_number_gt 8450 _reflns_number_total 10132 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL eb321_a.res in P-1 CELL 0.71073 11.5608 11.6437 18.1311 76.426 77.722 81.344 ZERR 2 0.0005 0.0005 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H Cl F I P Pd UNIT 88 68 8 6 6 4 2 EQIV $1 -1+X,+Y,+Z EQIV $2 1-X,1-Y,1-Z EQIV $3 +X,-1+Y,+Z DFIX 1.79 C44A Cl3A DFIX 1.79 C44A Cl4A L.S. 16 PLAN 20 0 0 TEMP -173 MPLA 6 C1 C2 C3 C4 C5 C6 Pd1 I1 HTAB C24 I1 HTAB C36 I1 HTAB C26 I2_$1 HTAB C42 I3_$2 HTAB C18 I2_$3 CONF BOND $H ACTA FMAP 2 1 53 HTAB 2.0 LIST 4 1 MORE -1 OMIT 0 1 0 WGHT 0.018997 4.238944 FVAR 0.183898 0.630867 REM REM REM I1 5 0.23962 -0.04364 0.79661 11.00000 0.01382 0.01547 0.01843 = -0.00247 0.00093 -0.00637 Pd1 7 0.39999 0.11224 0.75875 11.00000 0.00817 0.00891 0.00759 = -0.00098 -0.00059 -0.00203 Cl1 3 0.01465 0.81829 0.58804 11.00000 0.03925 0.07032 0.09062 = -0.04087 -0.01686 -0.00802 P1 6 0.25283 0.26815 0.77555 11.00000 0.00996 0.01078 0.01058 = -0.00196 -0.00071 -0.00079 F1 4 0.50264 0.22392 0.58875 11.00000 0.02414 0.02554 0.00921 = -0.00382 -0.00388 -0.01158 C1 1 0.51967 0.23113 0.71437 11.00000 0.00919 0.01020 0.01129 = -0.00079 -0.00187 0.00027 I2 5 0.73642 0.43117 0.79899 11.00000 0.01897 0.02511 0.02632 = -0.01266 -0.00724 -0.00558 Cl2 3 0.20648 0.97093 0.54543 11.00000 0.03975 0.03795 0.04571 = -0.01155 -0.01105 0.00246 P2 6 0.55621 -0.03829 0.75689 11.00000 0.01020 0.01004 0.00812 = -0.00171 -0.00168 -0.00175 F2 4 0.76543 0.47459 0.61696 11.00000 0.01619 0.01685 0.02724 = -0.00113 0.00112 -0.01084 C2 1 0.55273 0.26997 0.63565 11.00000 0.01247 0.01539 0.01116 = -0.00460 -0.00425 -0.00211 I3 5 0.68119 0.40425 0.48172 11.00000 0.03102 0.02993 0.01275 = 0.00125 0.00400 -0.00971 F3 4 0.54666 0.24532 0.83631 11.00000 0.02162 0.02326 0.00717 = -0.00242 -0.00371 -0.00541 C3 1 0.63391 0.35121 0.60091 11.00000 0.01505 0.01479 0.00872 = 0.00144 0.00080 -0.00292 PART 1 Cl4A 3 -0.04404 0.69475 0.78242 21.00000 0.05076 0.04950 0.10035 = -0.03215 -0.01553 -0.00577 PART 0 C4 1 0.68534 0.39554 0.64918 11.00000 0.00993 0.01062 0.01872 = 0.00060 0.00048 -0.00353 C5 1 0.65781 0.36114 0.72854 11.00000 0.01250 0.01121 0.01728 = -0.00699 -0.00312 -0.00086 C6 1 0.57554 0.27915 0.75843 11.00000 0.01267 0.01145 0.00778 = -0.00153 -0.00223 0.00165 C7 1 0.70322 0.00882 0.74620 11.00000 0.00974 0.01048 0.01628 = -0.00246 -0.00423 0.00025 C8 1 0.75308 0.00832 0.80977 11.00000 0.02213 0.01878 0.01744 = 0.00557 -0.00944 -0.00923 AFIX 43 H8 2 0.71231 -0.02174 0.86041 11.00000 -1.20000 AFIX 0 C9 1 0.86214 0.05159 0.79935 11.00000 0.02822 0.03711 0.02834 = 0.00395 -0.01710 -0.01463 AFIX 43 H9 2 0.89643 0.05026 0.84277 11.00000 -1.20000 AFIX 0 C10 1 0.92029 0.09621 0.72648 11.00000 0.01375 0.03236 0.03889 = -0.00019 -0.00962 -0.00723 AFIX 43 H10 2 0.99462 0.12627 0.71991 11.00000 -1.20000 AFIX 0 C11 1 0.87347 0.09833 0.66302 11.00000 0.01649 0.02138 0.02607 = -0.00151 0.00386 -0.00601 AFIX 43 H11 2 0.91490 0.12970 0.61282 11.00000 -1.20000 AFIX 0 C12 1 0.76445 0.05415 0.67236 11.00000 0.01788 0.01694 0.01484 = -0.00386 -0.00413 -0.00268 AFIX 43 H12 2 0.73178 0.05489 0.62838 11.00000 -1.20000 AFIX 0 C13 1 0.53957 -0.14377 0.84997 11.00000 0.01570 0.01548 0.01183 = -0.00350 -0.00452 -0.00384 C14 1 0.48375 -0.09902 0.91522 11.00000 0.03016 0.01919 0.01223 = -0.00283 -0.00359 0.00309 AFIX 43 H14 2 0.45416 -0.01740 0.90980 11.00000 -1.20000 AFIX 0 C15 1 0.47139 -0.17259 0.98736 11.00000 0.04473 0.02779 0.01060 = -0.00565 -0.00494 0.00505 AFIX 43 H15 2 0.43393 -0.14119 1.03145 11.00000 -1.20000 AFIX 0 C16 1 0.51307 -0.29175 0.99611 11.00000 0.05933 0.02077 0.00932 = 0.00374 -0.00319 -0.00845 AFIX 43 H16 2 0.50487 -0.34237 1.04592 11.00000 -1.20000 AFIX 0 C17 1 0.56667 -0.33612 0.93158 11.00000 0.07822 0.01201 0.01781 = -0.00029 -0.00482 -0.00035 AFIX 43 H17 2 0.59476 -0.41811 0.93715 11.00000 -1.20000 AFIX 0 C18 1 0.58023 -0.26293 0.85864 11.00000 0.04417 0.01549 0.01164 = -0.00424 -0.00084 0.00131 AFIX 43 H18 2 0.61747 -0.29479 0.81469 11.00000 -1.20000 AFIX 0 C19 1 0.57834 -0.11949 0.68008 11.00000 0.01535 0.01221 0.00761 = 0.00008 0.00218 -0.00651 C20 1 0.68132 -0.19692 0.66570 11.00000 0.01628 0.01211 0.01312 = -0.00161 -0.00273 -0.00014 AFIX 43 H20 2 0.73917 -0.20988 0.69779 11.00000 -1.20000 AFIX 0 C21 1 0.69959 -0.25476 0.60514 11.00000 0.01815 0.01294 0.01824 = -0.00301 0.00023 0.00051 AFIX 43 H21 2 0.76874 -0.30897 0.59665 11.00000 -1.20000 AFIX 0 C22 1 0.61717 -0.23380 0.55675 11.00000 0.02395 0.02102 0.01262 = -0.00701 -0.00024 -0.00845 AFIX 43 H22 2 0.63013 -0.27371 0.51516 11.00000 -1.20000 AFIX 0 C23 1 0.51604 -0.15502 0.56870 11.00000 0.01725 0.02183 0.01372 = -0.00561 -0.00387 -0.00480 AFIX 43 H23 2 0.46036 -0.13990 0.53496 11.00000 -1.20000 AFIX 0 C24 1 0.49641 -0.09806 0.63045 11.00000 0.01305 0.01513 0.01299 = -0.00256 -0.00150 -0.00335 AFIX 43 H24 2 0.42690 -0.04429 0.63891 11.00000 -1.20000 AFIX 0 C25 1 0.14740 0.22645 0.86487 11.00000 0.01726 0.01376 0.01172 = -0.00211 0.00275 -0.00198 C26 1 0.02489 0.24144 0.86950 11.00000 0.01787 0.02943 0.01684 = -0.00318 0.00031 -0.00362 AFIX 43 H26 2 -0.00839 0.27671 0.82479 11.00000 -1.20000 AFIX 0 C27 1 -0.04900 0.20446 0.94008 11.00000 0.01989 0.04610 0.02774 = -0.00716 0.00794 -0.01029 AFIX 43 H27 2 -0.13287 0.21481 0.94321 11.00000 -1.20000 AFIX 0 C28 1 -0.00229 0.15329 1.00514 11.00000 0.04520 0.04767 0.01628 = -0.00101 0.01096 -0.01364 AFIX 43 H28 2 -0.05339 0.12770 1.05293 11.00000 -1.20000 AFIX 0 C29 1 0.11993 0.13926 1.00059 11.00000 0.03857 0.05924 0.01363 = 0.00452 -0.00226 -0.00056 AFIX 43 H29 2 0.15268 0.10476 1.04561 11.00000 -1.20000 AFIX 0 C30 1 0.19421 0.17494 0.93132 11.00000 0.02391 0.03788 0.01548 = 0.00259 0.00045 0.00210 AFIX 43 H30 2 0.27797 0.16443 0.92873 11.00000 -1.20000 AFIX 0 C31 1 0.17017 0.31446 0.69683 11.00000 0.00900 0.01743 0.01055 = 0.00303 -0.00188 -0.00353 C32 1 0.09126 0.41800 0.69092 11.00000 0.01446 0.01716 0.01807 = -0.00268 0.00002 -0.00266 AFIX 43 H32 2 0.08203 0.46661 0.72761 11.00000 -1.20000 AFIX 0 C33 1 0.02621 0.45037 0.63183 11.00000 0.01222 0.01823 0.02446 = 0.00227 -0.00344 0.00086 AFIX 43 H33 2 -0.02687 0.52132 0.62777 11.00000 -1.20000 AFIX 0 C34 1 0.03894 0.37873 0.57861 11.00000 0.01777 0.02780 0.01443 = 0.00849 -0.00622 -0.00740 AFIX 43 H34 2 -0.00760 0.39917 0.53918 11.00000 -1.20000 AFIX 0 C35 1 0.11936 0.27758 0.58297 11.00000 0.01382 0.02448 0.01221 = -0.00329 0.00018 -0.00682 AFIX 43 H35 2 0.12958 0.23010 0.54554 11.00000 -1.20000 AFIX 0 C36 1 0.18526 0.24510 0.64186 11.00000 0.01333 0.01647 0.00966 = 0.00151 0.00093 -0.00394 AFIX 43 H36 2 0.24049 0.17569 0.64457 11.00000 -1.20000 AFIX 0 C37 1 0.29617 0.40874 0.78393 11.00000 0.01346 0.00955 0.02316 = -0.00381 -0.00696 0.00202 C38 1 0.27156 0.44740 0.85325 11.00000 0.04456 0.02526 0.02818 = -0.01178 -0.00315 -0.00793 AFIX 43 H38 2 0.23041 0.40074 0.89875 11.00000 -1.20000 AFIX 0 C39 1 0.30802 0.55551 0.85517 11.00000 0.07349 0.03836 0.04780 = -0.02526 -0.01688 -0.00948 AFIX 43 H39 2 0.29301 0.58155 0.90254 11.00000 -1.20000 AFIX 0 C40 1 0.36550 0.62472 0.78911 11.00000 0.04648 0.01685 0.06323 = -0.01189 -0.01840 -0.00871 AFIX 43 H40 2 0.38801 0.69913 0.79076 11.00000 -1.20000 AFIX 0 C41 1 0.38982 0.58697 0.72214 11.00000 0.01578 0.00816 0.04781 = 0.00409 -0.00535 -0.00210 AFIX 43 H41 2 0.43083 0.63456 0.67701 11.00000 -1.20000 AFIX 0 C42 1 0.35569 0.47908 0.71809 11.00000 0.01799 0.01288 0.02720 = 0.00031 -0.00406 0.00142 AFIX 43 H42 2 0.37309 0.45372 0.67042 11.00000 -1.20000 AFIX 0 C43 1 0.13182 0.86608 0.61888 11.00000 0.03459 0.04012 0.04575 = -0.01557 -0.01120 -0.00129 AFIX 23 H43a 2 0.09879 0.90157 0.66453 11.00000 -1.20000 H43b 2 0.18899 0.79669 0.63435 11.00000 -1.20000 AFIX 0 PART 1 C44A 1 -0.06087 0.65923 0.88439 21.00000 0.14674 0.09067 0.10689 = -0.07098 -0.06447 0.00688 AFIX 23 H44a 2 0.01204 0.67363 0.89973 21.00000 -1.20000 H44b 2 -0.12853 0.71094 0.90700 21.00000 -1.20000 AFIX 0 Cl3A 3 -0.08643 0.51083 0.91955 21.00000 0.07995 0.09051 0.06526 = -0.02899 -0.03916 0.00650 PART 2 Cl3B 3 -0.15176 0.54469 0.94105 -21.00000 0.06665 0.10390 0.06381 = -0.04218 -0.00375 -0.01330 C44B 1 -0.01590 0.58785 0.89095 -21.00000 0.06205 0.04432 0.08735 = -0.04110 -0.02261 -0.00318 AFIX 23 H44c 2 0.02185 0.62210 0.92385 -21.00000 -1.20000 H44d 2 0.03697 0.51778 0.87737 -21.00000 -1.20000 AFIX 0 Cl4B 3 -0.03380 0.69333 0.80682 -21.00000 0.17097 0.13015 0.08790 = -0.01847 -0.02022 -0.06227 HKLF 4 END Q1 1 0.55 0.75 0.703125 11 0.05 1.06 Q2 1 0.175 0.95 0.59375 11 0.05 0.87 Q3 1 0.875 0.05 0.75 11 0.05 0.85 Q4 1 0.5 -0.15 0.890625 11 0.05 0.71 Q5 1 0.1 0.75 0.578125 11 0.05 0.71 Q6 1 0.675 0.5 0.46875 11 0.05 0.68 Q7 1 0.75 0.425 0.5 11 0.05 0.67 Q8 1 0.325 -0.05 0.828125 11 0.05 0.64 Q9 1 0.625 0.55 0.703125 11 0.05 0.62 Q10 1 0.65 0.35 0.578125 11 0.05 0.61 Q11 1 0.4 -0.2 0.546875 11 0.05 0.61 Q12 1 0.2 0.25 0.59375 11 0.05 0.61 Q13 1 0.7 0.35 0.6875 11 0.05 0.61 REM The information below was added by Olex2. REM REM R1 = 0.0299 for 8450 Fo > 4sig(Fo) and 0.0417 for all 10132 data REM 542 parameters refined using 2 restraints REM Highest difference peak 1.0601, deepest hole -1.0272 REM Mean Shift 0.0000, Max Shift -0.0002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0417 REM R1_gt = 0.0299 REM wR_ref = 0.0618 REM GOOF = 1.0564 REM Shift_max = -0.0002 REM Shift_mean = 0.0000 REM Reflections_all = 10132 REM Reflections_gt = 8450 REM Parameters = 542 REM Hole = -1.0272 REM Peak = 1.0601 REM Flack = n/a ; _cod_data_source_file jy2058.cif _cod_data_source_block 4 _cod_database_code 2023503 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-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_occupancy _atom_site_disorder_group I I1 0.23962(2) -0.04364(2) 0.796612(13) 0.01617(6) Uani 1.000000 . Pd Pd1 0.39999(2) 0.11224(2) 0.758753(14) 0.00837(6) Uani 1.000000 . Cl Cl1 0.01465(12) 0.81829(14) 0.58804(10) 0.0617(4) Uani 1.000000 . P P1 0.25283(8) 0.26815(8) 0.77555(5) 0.01070(17) Uani 1.000000 . F F1 0.50264(18) 0.22392(18) 0.58875(11) 0.0185(4) Uani 1.000000 . C C1 0.5197(3) 0.2311(3) 0.71437(19) 0.0106(7) Uani 1.000000 . I I2 0.73642(2) 0.43117(2) 0.798995(15) 0.02142(6) Uani 1.000000 . Cl Cl2 0.20648(11) 0.97093(10) 0.54543(7) 0.0409(3) Uani 1.000000 . P P2 0.55621(8) -0.03829(7) 0.75689(5) 0.00942(17) Uani 1.000000 . F F2 0.76543(18) 0.47459(18) 0.61696(12) 0.0205(5) Uani 1.000000 . C C2 0.5527(3) 0.2700(3) 0.63565(19) 0.0123(7) Uani 1.000000 . I I3 0.68119(2) 0.40425(2) 0.481715(14) 0.02607(7) Uani 1.000000 . F F3 0.54666(18) 0.24532(18) 0.83631(11) 0.0170(4) Uani 1.000000 . C C3 0.6339(3) 0.3512(3) 0.60091(19) 0.0138(7) Uani 1.000000 . Cl Cl4A -0.0440(4) 0.6948(4) 0.7824(4) 0.0638(14) Uani 0.631(13) 1 C C4 0.6853(3) 0.3955(3) 0.6492(2) 0.0139(7) Uani 1.000000 . C C5 0.6578(3) 0.3611(3) 0.7285(2) 0.0130(7) Uani 1.000000 . C C6 0.5755(3) 0.2792(3) 0.75843(18) 0.0110(7) Uani 1.000000 . C C7 0.7032(3) 0.0088(3) 0.74620(19) 0.0121(7) Uani 1.000000 . C C8 0.7531(3) 0.0083(3) 0.8098(2) 0.0194(8) Uani 1.000000 . H H8 0.7123(3) -0.0217(3) 0.8604(2) 0.0233(10) Uiso 1.000000 . C C9 0.8621(4) 0.0516(4) 0.7993(2) 0.0300(10) Uani 1.000000 . H H9 0.8964(4) 0.0503(4) 0.8428(2) 0.0361(12) Uiso 1.000000 . C C10 0.9203(3) 0.0962(4) 0.7265(2) 0.0283(9) Uani 1.000000 . H H10 0.9946(3) 0.1263(4) 0.7199(2) 0.0340(11) Uiso 1.000000 . C C11 0.8735(3) 0.0983(3) 0.6630(2) 0.0227(8) Uani 1.000000 . H H11 0.9149(3) 0.1297(3) 0.6128(2) 0.0272(10) Uiso 1.000000 . C C12 0.7645(3) 0.0541(3) 0.6724(2) 0.0162(7) Uani 1.000000 . H H12 0.7318(3) 0.0549(3) 0.6284(2) 0.0194(9) Uiso 1.000000 . C C13 0.5396(3) -0.1438(3) 0.84997(19) 0.0137(7) Uani 1.000000 . C C14 0.4838(3) -0.0990(3) 0.9152(2) 0.0213(8) Uani 1.000000 . H H14 0.4542(3) -0.0174(3) 0.9098(2) 0.0255(10) Uiso 1.000000 . C C15 0.4714(4) -0.1726(4) 0.9874(2) 0.0284(9) Uani 1.000000 . H H15 0.4339(4) -0.1412(4) 1.0314(2) 0.0341(11) Uiso 1.000000 . C C16 0.5131(4) -0.2918(4) 0.9961(2) 0.0310(10) Uani 1.000000 . H H16 0.5049(4) -0.3424(4) 1.0459(2) 0.0372(12) Uiso 1.000000 . C C17 0.5667(5) -0.3361(4) 0.9316(2) 0.0376(12) Uani 1.000000 . H H17 0.5948(5) -0.4181(4) 0.9371(2) 0.0451(14) Uiso 1.000000 . C C18 0.5802(4) -0.2629(3) 0.8586(2) 0.0247(9) Uani 1.000000 . H H18 0.6175(4) -0.2948(3) 0.8147(2) 0.0296(11) Uiso 1.000000 . C C19 0.5783(3) -0.1195(3) 0.68008(18) 0.0122(7) Uani 1.000000 . C C20 0.6813(3) -0.1969(3) 0.66570(19) 0.0142(7) Uani 1.000000 . H H20 0.7392(3) -0.2099(3) 0.69779(19) 0.0170(9) Uiso 1.000000 . C C21 0.6996(3) -0.2548(3) 0.6051(2) 0.0173(8) Uani 1.000000 . H H21 0.7687(3) -0.3090(3) 0.5966(2) 0.0207(9) Uiso 1.000000 . C C22 0.6172(3) -0.2338(3) 0.5567(2) 0.0184(8) Uani 1.000000 . H H22 0.6301(3) -0.2737(3) 0.5152(2) 0.0221(9) Uiso 1.000000 . C C23 0.5160(3) -0.1550(3) 0.5687(2) 0.0168(8) Uani 1.000000 . H H23 0.4604(3) -0.1399(3) 0.5350(2) 0.0202(9) Uiso 1.000000 . C C24 0.4964(3) -0.0981(3) 0.63045(19) 0.0137(7) Uani 1.000000 . H H24 0.4269(3) -0.0443(3) 0.63891(19) 0.0165(8) Uiso 1.000000 . C C25 0.1474(3) 0.2264(3) 0.86487(19) 0.0151(7) Uani 1.000000 . C C26 0.0249(3) 0.2414(3) 0.8695(2) 0.0221(8) Uani 1.000000 . H H26 -0.0084(3) 0.2767(3) 0.8248(2) 0.0265(10) Uiso 1.000000 . C C27 -0.0490(4) 0.2045(4) 0.9401(2) 0.0325(10) Uani 1.000000 . H H27 -0.1329(4) 0.2148(4) 0.9432(2) 0.0390(12) Uiso 1.000000 . C C28 -0.0023(4) 0.1533(4) 1.0051(2) 0.0390(11) Uani 1.000000 . H H28 -0.0534(4) 0.1277(4) 1.0529(2) 0.0467(14) Uiso 1.000000 . C C29 0.1199(4) 0.1393(5) 1.0006(2) 0.0401(12) Uani 1.000000 . H H29 0.1527(4) 0.1048(5) 1.0456(2) 0.0481(14) Uiso 1.000000 . C C30 0.1942(4) 0.1749(4) 0.9313(2) 0.0283(9) Uani 1.000000 . H H30 0.2780(4) 0.1644(4) 0.9287(2) 0.0340(11) Uiso 1.000000 . C C31 0.1702(3) 0.3145(3) 0.69683(19) 0.0131(7) Uani 1.000000 . C C32 0.0913(3) 0.4180(3) 0.6909(2) 0.0171(8) Uani 1.000000 . H H32 0.0820(3) 0.4666(3) 0.7276(2) 0.0205(9) Uiso 1.000000 . C C33 0.0262(3) 0.4504(3) 0.6318(2) 0.0197(8) Uani 1.000000 . H H33 -0.0269(3) 0.5213(3) 0.6278(2) 0.0236(10) Uiso 1.000000 . C C34 0.0389(3) 0.3787(3) 0.5786(2) 0.0212(8) Uani 1.000000 . H H34 -0.0076(3) 0.3992(3) 0.5392(2) 0.0254(10) Uiso 1.000000 . C C35 0.1194(3) 0.2776(3) 0.5830(2) 0.0168(8) Uani 1.000000 . H H35 0.1296(3) 0.2301(3) 0.5455(2) 0.0202(9) Uiso 1.000000 . C C36 0.1853(3) 0.2451(3) 0.64186(19) 0.0141(7) Uani 1.000000 . H H36 0.2405(3) 0.1757(3) 0.64457(19) 0.0169(9) Uiso 1.000000 . C C37 0.2962(3) 0.4087(3) 0.7839(2) 0.0151(7) Uani 1.000000 . C C38 0.2716(4) 0.4474(4) 0.8533(3) 0.0317(10) Uani 1.000000 . H H38 0.2304(4) 0.4007(4) 0.8987(3) 0.0381(12) Uiso 1.000000 . C C39 0.3080(5) 0.5555(4) 0.8552(3) 0.0492(14) Uani 1.000000 . H H39 0.2930(5) 0.5815(4) 0.9025(3) 0.0591(16) Uiso 1.000000 . C C40 0.3655(4) 0.6247(4) 0.7891(3) 0.0398(12) Uani 1.000000 . H H40 0.3880(4) 0.6991(4) 0.7908(3) 0.0477(14) Uiso 1.000000 . C C41 0.3898(3) 0.5870(3) 0.7221(3) 0.0256(9) Uani 1.000000 . H H41 0.4308(3) 0.6346(3) 0.6770(3) 0.0307(11) Uiso 1.000000 . C C42 0.3557(3) 0.4791(3) 0.7181(2) 0.0205(8) Uani 1.000000 . H H42 0.3731(3) 0.4537(3) 0.6704(2) 0.0246(10) Uiso 1.000000 . C C43 0.1318(4) 0.8661(4) 0.6189(3) 0.0387(11) Uani 1.000000 . H H43a 0.0988(4) 0.9016(4) 0.6645(3) 0.0465(13) Uiso 1.000000 . H H43b 0.1890(4) 0.7967(4) 0.6343(3) 0.0465(13) Uiso 1.000000 . C C44A -0.0609(15) 0.6592(12) 0.8844(7) 0.102(6) Uani 0.631(13) 1 H H44a 0.0120(15) 0.6736(12) 0.8997(7) 0.122(7) Uiso 0.631(13) 1 H H44b -0.1285(15) 0.7109(12) 0.9070(7) 0.122(7) Uiso 0.631(13) 1 Cl Cl3A -0.0864(6) 0.5108(4) 0.9195(3) 0.0742(17) Uani 0.631(13) 1 Cl Cl3B -0.1518(10) 0.5447(9) 0.9410(3) 0.075(3) Uani 0.369(13) 2 C C44B -0.0159(17) 0.5878(18) 0.8910(11) 0.059(5) Uani 0.369(13) 2 H H44c 0.0218(17) 0.6221(18) 0.9239(11) 0.071(6) Uiso 0.369(13) 2 H H44d 0.0370(17) 0.5178(18) 0.8774(11) 0.071(6) Uiso 0.369(13) 2 Cl Cl4B -0.0338(13) 0.6933(13) 0.8068(9) 0.126(5) Uani 0.369(13) 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.01382(11) 0.01547(12) 0.01843(12) -0.00637(9) 0.00093(9) -0.00247(9) Pd1 0.00817(12) 0.00891(12) 0.00759(12) -0.00203(9) -0.00059(9) -0.00098(9) Cl1 0.0393(7) 0.0703(10) 0.0906(11) -0.0080(7) -0.0169(7) -0.0409(9) P1 0.0100(4) 0.0108(4) 0.0106(4) -0.0008(3) -0.0007(3) -0.0020(3) F1 0.0241(11) 0.0255(11) 0.0092(10) -0.0116(9) -0.0039(8) -0.0038(9) C1 0.0092(16) 0.0102(16) 0.0113(16) 0.0003(13) -0.0019(13) -0.0008(13) I2 0.01897(13) 0.02511(13) 0.02632(14) -0.00558(10) -0.00724(10) -0.01266(11) Cl2 0.0398(7) 0.0379(6) 0.0457(7) 0.0025(5) -0.0111(5) -0.0115(5) P2 0.0102(4) 0.0100(4) 0.0081(4) -0.0017(3) -0.0017(3) -0.0017(3) F2 0.0162(11) 0.0169(11) 0.0272(12) -0.0108(9) 0.0011(9) -0.0011(9) C2 0.0125(17) 0.0154(17) 0.0112(17) -0.0021(14) -0.0042(13) -0.0046(14) I3 0.03102(15) 0.02993(15) 0.01275(12) -0.00971(12) 0.00400(10) 0.00125(10) F3 0.0216(11) 0.0233(11) 0.0072(10) -0.0054(9) -0.0037(8) -0.0024(8) C3 0.0151(18) 0.0148(17) 0.0087(16) -0.0029(14) 0.0008(13) 0.0014(14) Cl4A 0.0508(19) 0.0495(19) 0.100(4) -0.0058(13) -0.0155(19) -0.032(2) C4 0.0099(17) 0.0106(17) 0.0187(18) -0.0035(13) 0.0005(14) 0.0006(14) C5 0.0125(17) 0.0112(16) 0.0173(18) -0.0009(13) -0.0031(14) -0.0070(14) C6 0.0127(17) 0.0114(16) 0.0078(16) 0.0016(13) -0.0022(13) -0.0015(13) C7 0.0097(16) 0.0105(16) 0.0163(17) 0.0003(13) -0.0042(13) -0.0025(14) C8 0.022(2) 0.0188(19) 0.0174(19) -0.0092(16) -0.0094(15) 0.0056(15) C9 0.028(2) 0.037(2) 0.028(2) -0.0146(19) -0.0171(18) 0.0039(19) C10 0.014(2) 0.032(2) 0.039(2) -0.0072(17) -0.0096(18) -0.0002(19) C11 0.0165(19) 0.021(2) 0.026(2) -0.0060(16) 0.0039(16) -0.0015(17) C12 0.0179(19) 0.0169(18) 0.0148(18) -0.0027(15) -0.0041(14) -0.0039(14) C13 0.0157(18) 0.0155(17) 0.0118(17) -0.0038(14) -0.0045(14) -0.0035(14) C14 0.030(2) 0.0192(19) 0.0122(18) 0.0031(17) -0.0036(16) -0.0028(15) C15 0.045(3) 0.028(2) 0.0106(19) 0.0050(19) -0.0049(17) -0.0056(16) C16 0.059(3) 0.021(2) 0.0093(19) -0.008(2) -0.0032(19) 0.0037(16) C17 0.078(4) 0.0120(19) 0.018(2) 0.000(2) -0.005(2) -0.0003(16) C18 0.044(3) 0.0155(19) 0.0116(18) 0.0013(18) -0.0008(17) -0.0042(15) C19 0.0153(17) 0.0122(17) 0.0076(16) -0.0065(14) 0.0022(13) 0.0001(13) C20 0.0163(18) 0.0121(17) 0.0131(17) -0.0001(14) -0.0027(14) -0.0016(14) C21 0.0181(19) 0.0129(17) 0.0182(19) 0.0005(15) 0.0002(15) -0.0030(15) C22 0.024(2) 0.0210(19) 0.0126(18) -0.0084(16) -0.0002(15) -0.0070(15) C23 0.0173(19) 0.0218(19) 0.0137(18) -0.0048(15) -0.0039(14) -0.0056(15) C24 0.0130(17) 0.0151(17) 0.0130(17) -0.0033(14) -0.0015(13) -0.0026(14) C25 0.0173(18) 0.0138(17) 0.0117(17) -0.0020(14) 0.0027(14) -0.0021(14) C26 0.018(2) 0.029(2) 0.0168(19) -0.0036(16) 0.0003(15) -0.0032(16) C27 0.020(2) 0.046(3) 0.028(2) -0.010(2) 0.0079(17) -0.007(2) C28 0.045(3) 0.048(3) 0.016(2) -0.014(2) 0.0110(19) -0.001(2) C29 0.039(3) 0.059(3) 0.014(2) -0.001(2) -0.0023(19) 0.005(2) C30 0.024(2) 0.038(2) 0.015(2) 0.0021(19) 0.0004(16) 0.0026(17) C31 0.0090(16) 0.0174(18) 0.0106(17) -0.0035(14) -0.0019(13) 0.0030(14) C32 0.0145(18) 0.0172(18) 0.0181(19) -0.0027(15) 0.0000(14) -0.0027(15) C33 0.0122(18) 0.0182(19) 0.024(2) 0.0009(15) -0.0034(15) 0.0023(16) C34 0.0178(19) 0.028(2) 0.0144(18) -0.0074(16) -0.0062(15) 0.0085(16) C35 0.0138(18) 0.024(2) 0.0122(17) -0.0068(15) 0.0002(14) -0.0033(15) C36 0.0133(17) 0.0165(18) 0.0097(16) -0.0039(14) 0.0009(13) 0.0015(14) C37 0.0135(17) 0.0095(16) 0.0232(19) 0.0020(14) -0.0070(15) -0.0038(14) C38 0.045(3) 0.025(2) 0.028(2) -0.008(2) -0.003(2) -0.0118(18) C39 0.073(4) 0.038(3) 0.048(3) -0.009(3) -0.017(3) -0.025(3) C40 0.046(3) 0.017(2) 0.063(3) -0.009(2) -0.018(3) -0.012(2) C41 0.0158(19) 0.0082(17) 0.048(3) -0.0021(15) -0.0053(18) 0.0041(17) C42 0.0180(19) 0.0129(18) 0.027(2) 0.0014(15) -0.0041(16) 0.0003(16) C43 0.035(3) 0.040(3) 0.046(3) -0.001(2) -0.011(2) -0.016(2) C44A 0.147(15) 0.091(11) 0.107(12) 0.007(10) -0.064(10) -0.071(10) Cl3A 0.080(4) 0.091(2) 0.065(3) 0.006(2) -0.039(3) -0.0290(18) Cl3B 0.067(5) 0.104(5) 0.064(3) -0.013(4) -0.004(3) -0.042(3) C44B 0.062(12) 0.044(11) 0.087(13) -0.003(9) -0.023(10) -0.041(10) Cl4B 0.171(10) 0.130(8) 0.088(8) -0.062(7) -0.020(6) -0.018(5) loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.21560 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' Cl 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940 47.77840 -9.55740 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.14873 0.16029 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' F 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150 26.14760 0.27760 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.01794 0.01033 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' H 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.00304 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' I 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600 66.87760 4.07120 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' -0.41187 1.83264 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' P 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600 68.16450 1.11490 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' 0.10434 0.09671 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' Pd 19.33190 15.50170 5.29537 0.60584 0.69866 7.98929 25.20520 76.89860 5.26593 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' -0.98845 1.01473 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l -1 0 0 -1 0 0 1 0 0 1 0 0 -2 0 0 -2 0 0 2 0 0 2 0 0 -3 0 0 -3 0 0 3 0 0 3 0 0 -4 0 0 -4 0 0 4 0 0 4 0 0 -5 0 0 -5 0 0 5 0 0 5 0 0 -6 0 0 -6 0 0 6 0 0 6 0 0 -7 0 0 -7 0 0 7 0 0 7 0 0 -8 0 0 -8 0 0 8 0 0 8 0 0 -9 0 0 9 0 0 9 0 0 -10 0 0 10 0 0 10 0 0 -11 0 0 11 0 0 -12 0 0 12 0 0 -13 0 0 13 0 0 -14 0 0 14 0 0 14 -1 0 -14 1 0 13 -1 0 -13 1 0 12 -1 0 -12 1 0 11 -1 0 -11 1 0 10 -1 0 10 -1 0 -10 1 0 9 -1 0 9 -1 0 -9 1 0 8 -1 0 8 -1 0 8 -1 0 -8 1 0 7 -1 0 7 -1 0 7 -1 0 -7 1 0 6 -1 0 6 -1 0 -6 1 0 5 -1 0 5 -1 0 -5 1 0 4 -1 0 4 -1 0 -4 1 0 -4 1 0 3 -1 0 3 -1 0 -3 1 0 2 -1 0 2 -1 0 -2 1 0 1 -1 0 1 -1 0 -1 1 0 0 -1 0 0 -1 0 0 -1 0 0 -1 0 -1 -1 0 -1 -1 0 1 1 0 -2 -1 0 -2 -1 0 2 1 0 -3 -1 0 -3 -1 0 3 1 0 3 1 0 -4 -1 0 -4 -1 0 4 1 0 4 1 0 -5 -1 0 -5 -1 0 5 1 0 5 1 0 -6 -1 0 -6 -1 0 6 1 0 6 1 0 -7 -1 0 -7 -1 0 7 1 0 7 1 0 -8 -1 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6 21 -5 -6 -21 -6 -6 -21 6 6 21 -7 -6 -21 7 6 21 -8 -6 -21 8 6 21 -1 7 21 -1 7 21 0 -7 -21 0 7 21 0 7 21 -1 -7 -21 1 7 21 1 7 21 -2 -7 -21 2 7 21 2 7 21 -3 -7 -21 -3 -7 -21 3 7 21 -4 -7 -21 -4 -7 -21 4 7 21 -5 -7 -21 -5 -7 -21 -6 -7 -21 -6 -7 -21 -7 -7 -21 -7 -7 -21 7 7 21 -8 -7 -21 -8 -7 -21 8 7 21 0 -8 -21 0 8 21 0 8 21 -1 -8 -21 1 8 21 1 8 21 -2 -8 -21 2 8 21 2 8 21 -3 -8 -21 -3 -8 -21 3 8 21 -4 -8 -21 -4 -8 -21 4 8 21 -5 -8 -21 -5 -8 -21 -6 -8 -21 -6 -8 -21 -7 -8 -21 -7 -8 -21 -2 -9 -21 2 9 21 2 9 21 -3 -9 -21 -3 -9 -21 -4 -9 -21 -4 -9 -21 -5 -9 -21 -5 -9 -21 2 -1 22 3 -1 22 4 -1 22 2 0 22 3 0 22 4 0 22 -5 0 -22 5 0 22 -1 -1 -22 -4 -1 -22 4 1 22 -5 -1 -22 5 1 22 -6 -1 -22 6 1 22 0 2 22 1 2 22 -4 -2 -22 4 2 22 -5 -2 -22 5 2 22 -6 -2 -22 6 2 22 -7 -2 -22 7 2 22 -1 3 22 0 3 22 1 3 22 2 3 22 -3 -3 -22 -4 -3 -22 4 3 22 -5 -3 -22 5 3 22 -6 -3 -22 6 3 22 -7 -3 -22 7 3 22 0 4 22 1 4 22 -2 -4 -22 2 4 22 -3 -4 -22 -4 -4 -22 -5 -4 -22 5 4 22 -6 -4 -22 6 4 22 -7 -4 -22 7 4 22 -1 5 22 -2 -5 -22 2 5 22 -3 -5 -22 3 5 22 -4 -5 -22 -5 -5 -22 -6 -5 -22 6 5 22 -7 -5 -22 7 5 22 0 6 22 -1 -6 -22 1 6 22 -2 -6 -22 2 6 22 -3 -6 -22 3 6 22 -4 -6 -22 -5 -6 -22 -6 -6 -22 -7 -6 -22 7 6 22 -1 -7 -22 1 7 22 -2 -7 -22 2 7 22 2 7 22 -3 -7 -22 3 7 22 3 7 22 -4 -7 -22 -5 -7 -22 -6 -7 -22 -3 -8 -22 -4 -2 -23 4 2 23 -4 -3 -23 -5 -3 -23 5 3 23 -3 -4 -23 -4 -4 -23 -2 -5 -23 -4 -5 -23 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 P1 Pd1 I1 . . 91.66(2) ? C1 Pd1 I1 . . 171.82(9) ? C1 Pd1 P1 . . 89.09(9) ? P2 Pd1 I1 . . 91.72(2) ? P2 Pd1 P1 . . 171.80(3) ? P2 Pd1 C1 . . 88.63(9) ? C25 P1 Pd1 . . 110.31(12) ? C31 P1 Pd1 . . 113.10(12) ? C31 P1 C25 . . 108.12(16) ? C37 P1 Pd1 . . 118.72(11) ? C37 P1 C25 . . 103.15(16) ? C37 P1 C31 . . 102.49(16) ? C2 C1 Pd1 . . 121.3(2) ? C6 C1 Pd1 . . 124.0(2) ? C6 C1 C2 . . 114.8(3) ? C7 P2 Pd1 . . 115.27(11) ? C13 P2 Pd1 . . 109.67(12) ? C13 P2 C7 . . 103.29(15) ? C19 P2 Pd1 . . 116.61(12) ? C19 P2 C7 . . 101.96(15) ? C19 P2 C13 . . 109.01(15) ? C1 C2 F1 . . 117.7(3) ? C3 C2 F1 . . 117.7(3) ? C3 C2 C1 . . 124.6(3) ? I3 C3 C2 . . 122.6(2) ? C4 C3 C2 . . 117.0(3) ? C4 C3 I3 . . 120.4(2) ? C3 C4 F2 . . 118.3(3) ? C5 C4 F2 . . 119.4(3) ? C5 C4 C3 . . 122.2(3) ? C4 C5 I2 . . 120.9(2) ? C6 C5 I2 . . 122.1(2) ? C6 C5 C4 . . 116.9(3) ? F3 C6 C1 . . 117.8(3) ? C5 C6 C1 . . 124.5(3) ? C5 C6 F3 . . 117.7(3) ? C8 C7 P2 . . 121.9(3) ? C12 C7 P2 . . 119.1(3) ? C12 C7 C8 . . 118.9(3) ? H8 C8 C7 . . 119.9(2) ? C9 C8 C7 . . 120.2(3) ? C9 C8 H8 . . 119.9(2) ? H9 C9 C8 . . 120.0(2) ? C10 C9 C8 . . 120.0(4) ? C10 C9 H9 . . 120.0(2) ? H10 C10 C9 . . 119.4(2) ? C11 C10 C9 . . 121.2(4) ? C11 C10 H10 . . 119.4(2) ? H11 C11 C10 . . 120.2(2) ? C12 C11 C10 . . 119.6(4) ? C12 C11 H11 . . 120.2(2) ? C11 C12 C7 . . 120.2(3) ? H12 C12 C7 . . 119.9(2) ? H12 C12 C11 . . 119.9(2) ? C14 C13 P2 . . 117.2(3) ? C18 C13 P2 . . 123.6(3) ? C18 C13 C14 . . 119.1(3) ? H14 C14 C13 . . 119.8(2) ? C15 C14 C13 . . 120.4(3) ? C15 C14 H14 . . 119.8(2) ? H15 C15 C14 . . 119.7(2) ? C16 C15 C14 . . 120.5(4) ? C16 C15 H15 . . 119.7(2) ? H16 C16 C15 . . 120.5(2) ? C17 C16 C15 . . 119.1(4) ? C17 C16 H16 . . 120.5(2) ? H17 C17 C16 . . 119.5(2) ? C18 C17 C16 . . 121.0(4) ? C18 C17 H17 . . 119.5(2) ? C17 C18 C13 . . 119.9(3) ? H18 C18 C13 . . 120.0(2) ? H18 C18 C17 . . 120.0(2) ? C20 C19 P2 . . 120.9(3) ? C24 C19 P2 . . 120.0(3) ? C24 C19 C20 . . 118.9(3) ? H20 C20 C19 . . 119.8(2) ? C21 C20 C19 . . 120.5(3) ? C21 C20 H20 . . 119.8(2) ? H21 C21 C20 . . 119.9(2) ? C22 C21 C20 . . 120.1(3) ? C22 C21 H21 . . 119.9(2) ? H22 C22 C21 . . 119.8(2) ? C23 C22 C21 . . 120.4(3) ? C23 C22 H22 . . 119.8(2) ? H23 C23 C22 . . 120.2(2) ? C24 C23 C22 . . 119.7(3) ? C24 C23 H23 . . 120.2(2) ? C23 C24 C19 . . 120.4(3) ? H24 C24 C19 . . 119.8(2) ? H24 C24 C23 . . 119.8(2) ? C26 C25 P1 . . 123.6(3) ? C30 C25 P1 . . 117.2(3) ? C30 C25 C26 . . 119.2(3) ? H26 C26 C25 . . 120.2(2) ? C27 C26 C25 . . 119.6(4) ? C27 C26 H26 . . 120.2(2) ? H27 C27 C26 . . 119.6(2) ? C28 C27 C26 . . 120.9(4) ? C28 C27 H27 . . 119.6(3) ? H28 C28 C27 . . 120.3(3) ? C29 C28 C27 . . 119.5(4) ? C29 C28 H28 . . 120.3(2) ? H29 C29 C28 . . 119.8(2) ? C30 C29 C28 . . 120.4(4) ? C30 C29 H29 . . 119.8(3) ? C29 C30 C25 . . 120.4(4) ? H30 C30 C25 . . 119.8(2) ? H30 C30 C29 . . 119.8(3) ? C32 C31 P1 . . 121.1(3) ? C36 C31 P1 . . 119.5(3) ? C36 C31 C32 . . 119.5(3) ? H32 C32 C31 . . 119.8(2) ? C33 C32 C31 . . 120.4(3) ? C33 C32 H32 . . 119.8(2) ? H33 C33 C32 . . 120.1(2) ? C34 C33 C32 . . 119.8(3) ? C34 C33 H33 . . 120.1(2) ? H34 C34 C33 . . 120.0(2) ? C35 C34 C33 . . 120.1(3) ? C35 C34 H34 . . 120.0(2) ? H35 C35 C34 . . 119.8(2) ? C36 C35 C34 . . 120.3(3) ? C36 C35 H35 . . 119.8(2) ? C35 C36 C31 . . 119.9(3) ? H36 C36 C31 . . 120.1(2) ? H36 C36 C35 . . 120.1(2) ? C38 C37 P1 . . 122.6(3) ? C42 C37 P1 . . 118.2(3) ? C42 C37 C38 . . 119.2(3) ? H38 C38 C37 . . 120.4(2) ? C39 C38 C37 . . 119.3(4) ? C39 C38 H38 . . 120.4(3) ? H39 C39 C38 . . 119.7(3) ? C40 C39 C38 . . 120.7(4) ? C40 C39 H39 . . 119.7(3) ? H40 C40 C39 . . 120.0(3) ? C41 C40 C39 . . 120.0(4) ? C41 C40 H40 . . 120.0(2) ? H41 C41 C40 . . 119.5(2) ? C42 C41 C40 . . 121.0(4) ? C42 C41 H41 . . 119.5(2) ? C41 C42 C37 . . 119.8(4) ? H42 C42 C37 . . 120.1(2) ? H42 C42 C41 . . 120.1(2) ? Cl2 C43 Cl1 . . 111.3(3) ? H43a C43 Cl1 . . 109.37(16) ? H43a C43 Cl2 . . 109.37(16) ? H43b C43 Cl1 . . 109.37(16) ? H43b C43 Cl2 . . 109.37(16) ? H43b C43 H43a . . 108.0 ? H44a C44A Cl4A . . 109.6(5) ? H44b C44A Cl4A . . 109.6(6) ? H44b C44A H44a . . 108.1 ? Cl3A C44A Cl4A . . 110.2(6) ? Cl3A C44A H44a . . 109.6(6) ? Cl3A C44A H44b . . 109.6(7) ? H44c C44B Cl3B . . 109.6(6) ? H44d C44B Cl3B . . 109.6(8) ? H44d C44B H44c . . 108.134034658(15) ? Cl4B C44B Cl3B . . 110.2(12) ? Cl4B C44B H44c . . 109.6(8) ? Cl4B C44B H44d . . 109.6(8) ? 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 I1 Pd1 . 2.6626(3) ? Pd1 P1 . 2.3221(9) ? Pd1 C1 . 2.014(3) ? Pd1 P2 . 2.3203(9) ? Cl1 C43 . 1.775(5) ? P1 C25 . 1.820(3) ? P1 C31 . 1.818(3) ? P1 C37 . 1.830(3) ? F1 C2 . 1.365(4) ? C1 C2 . 1.380(5) ? C1 C6 . 1.381(4) ? I2 C5 . 2.080(3) ? Cl2 C43 . 1.753(5) ? P2 C7 . 1.821(3) ? P2 C13 . 1.831(3) ? P2 C19 . 1.815(3) ? F2 C4 . 1.349(4) ? C2 C3 . 1.382(5) ? I3 C3 . 2.079(3) ? F3 C6 . 1.356(4) ? C3 C4 . 1.383(5) ? Cl4A C44A . 1.772(12) ? C4 C5 . 1.380(5) ? C5 C6 . 1.386(5) ? C7 C8 . 1.393(5) ? C7 C12 . 1.396(5) ? C8 H8 . 0.9500 ? C8 C9 . 1.387(5) ? C9 H9 . 0.9500 ? C9 C10 . 1.368(6) ? C10 H10 . 0.9500 ? C10 C11 . 1.366(6) ? C11 H11 . 0.9500 ? C11 C12 . 1.395(5) ? C12 H12 . 0.9500 ? C13 C14 . 1.397(5) ? C13 C18 . 1.380(5) ? C14 H14 . 0.9500 ? C14 C15 . 1.377(5) ? C15 H15 . 0.9500 ? C15 C16 . 1.382(6) ? C16 H16 . 0.9500 ? C16 C17 . 1.378(6) ? C17 H17 . 0.9500 ? C17 C18 . 1.387(5) ? C18 H18 . 0.9500 ? C19 C20 . 1.398(5) ? C19 C24 . 1.398(5) ? C20 H20 . 0.9500 ? C20 C21 . 1.382(5) ? C21 H21 . 0.9500 ? C21 C22 . 1.387(5) ? C22 H22 . 0.9500 ? C22 C23 . 1.385(5) ? C23 H23 . 0.9500 ? C23 C24 . 1.393(5) ? C24 H24 . 0.9500 ? C25 C26 . 1.387(5) ? C25 C30 . 1.395(5) ? C26 H26 . 0.9500 ? C26 C27 . 1.393(5) ? C27 H27 . 0.9500 ? C27 C28 . 1.372(6) ? C28 H28 . 0.9500 ? C28 C29 . 1.385(6) ? C29 H29 . 0.9500 ? C29 C30 . 1.375(6) ? C30 H30 . 0.9500 ? C31 C32 . 1.395(5) ? C31 C36 . 1.392(5) ? C32 H32 . 0.9500 ? C32 C33 . 1.387(5) ? C33 H33 . 0.9500 ? C33 C34 . 1.389(5) ? C34 H34 . 0.9500 ? C34 C35 . 1.384(5) ? C35 H35 . 0.9500 ? C35 C36 . 1.390(5) ? C36 H36 . 0.9500 ? C37 C38 . 1.392(5) ? C37 C42 . 1.390(5) ? C38 H38 . 0.9500 ? C38 C39 . 1.396(6) ? C39 H39 . 0.9500 ? C39 C40 . 1.377(7) ? C40 H40 . 0.9500 ? C40 C41 . 1.347(6) ? C41 H41 . 0.9500 ? C41 C42 . 1.394(5) ? C42 H42 . 0.9500 ? C43 H43a . 0.9900 ? C43 H43b . 0.9900 ? C44A H44a . 0.9900 ? C44A H44b . 0.9900 ? C44A Cl3A . 1.742(12) ? Cl3B C44B . 1.72(2) ? C44B H44c . 0.9900 ? C44B H44d . 0.9900 ? C44B Cl4B . 1.75(2) ? 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 C1 C2 F1 . . . . -0.8(3) ? Pd1 C1 C2 C3 . . . . 179.9(3) ? Pd1 C1 C6 F3 . . . . -1.0(3) ? Pd1 C1 C6 C5 . . . . -179.9(3) ? P1 C25 C26 C27 . . . . 178.6(3) ? P1 C25 C30 C29 . . . . -178.8(3) ? P1 C31 C32 C33 . . . . -178.1(3) ? P1 C31 C36 C35 . . . . 177.8(3) ? P1 C37 C38 C39 . . . . 179.7(4) ? P1 C37 C42 C41 . . . . 179.8(3) ? F1 C2 C1 C6 . . . . 178.6(3) ? F1 C2 C3 I3 . . . . 0.0(3) ? F1 C2 C3 C4 . . . . -179.0(3) ? C1 C2 C3 I3 . . . . 179.2(3) ? C1 C2 C3 C4 . . . . 0.3(4) ? C1 C6 C5 I2 . . . . 179.1(3) ? C1 C6 C5 C4 . . . . -0.5(4) ? I2 C5 C4 F2 . . . . 0.8(3) ? I2 C5 C4 C3 . . . . -179.5(3) ? I2 C5 C6 F3 . . . . 0.2(3) ? P2 C7 C8 C9 . . . . -176.1(3) ? P2 C7 C12 C11 . . . . 175.6(3) ? P2 C13 C14 C15 . . . . -178.1(3) ? P2 C13 C18 C17 . . . . 178.3(4) ? P2 C19 C20 C21 . . . . -177.4(3) ? P2 C19 C24 C23 . . . . 176.4(3) ? F2 C4 C3 C2 . . . . 179.7(3) ? F2 C4 C3 I3 . . . . 0.7(3) ? F2 C4 C5 C6 . . . . -179.6(3) ? C2 C3 C4 C5 . . . . 0.0(4) ? I3 C3 C4 C5 . . . . -178.9(3) ? F3 C6 C5 C4 . . . . -179.4(3) ? C3 C4 C5 C6 . . . . 0.1(4) ? C7 C8 C9 C10 . . . . 0.8(4) ? C7 C12 C11 C10 . . . . 0.5(4) ? C8 C9 C10 C11 . . . . -0.5(5) ? C9 C10 C11 C12 . . . . -0.1(5) ? C13 C14 C15 C16 . . . . -0.6(5) ? C13 C18 C17 C16 . . . . -0.1(5) ? C14 C15 C16 C17 . . . . -0.3(5) ? C15 C16 C17 C18 . . . . 0.6(5) ? C19 C20 C21 C22 . . . . 1.8(4) ? C19 C24 C23 C22 . . . . 0.3(4) ? C20 C21 C22 C23 . . . . -0.1(4) ? C21 C22 C23 C24 . . . . -1.0(4) ? C25 C26 C27 C28 . . . . -0.1(5) ? C25 C30 C29 C28 . . . . 0.4(5) ? C26 C27 C28 C29 . . . . 0.6(5) ? C27 C28 C29 C30 . . . . -0.8(6) ? C31 C32 C33 C34 . . . . 0.6(4) ? C31 C36 C35 C34 . . . . 0.1(4) ? C32 C33 C34 C35 . . . . -2.3(4) ? C33 C34 C35 C36 . . . . 1.9(4) ? C37 C38 C39 C40 . . . . 1.4(5) ? C37 C42 C41 C40 . . . . -0.3(4) ? C38 C39 C40 C41 . . . . -1.7(6) ? C39 C40 C41 C42 . . . . 1.2(6) ? loop_ _restr_distance_atom_site_label_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param C44A Cl4A 1 1.7900 0.0200 C44A Cl3A 1 1.7900 0.0200