#------------------------------------------------------------------------------ #$Date: 2016-04-04 13:38:21 +0300 (Mon, 04 Apr 2016) $ #$Revision: 181374 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/64/4086447.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_4086447 loop_ _publ_author_name 'Magnuson, Kevin W.' 'Oshiro, Shelly M.' 'Gurr, Joshua R.' 'Yoshida, Wesley Y.' 'Gembicky, Milan' 'Rheingold, Arnold L.' 'Hughes, Russell P.' 'Cain, Matthew F.' _publ_contact_author_name ; ; _publ_section_title ; Streamlined Preparation and Coordination Chemistry of Hybrid Phosphine\^a€“Phosphaalkene Ligands ; _journal_issue 6 _journal_name_full Organometallics _journal_page_first 855 _journal_page_last 859 _journal_paper_doi 10.1021/acs.organomet.6b00101 _journal_volume 35 _journal_year 2016 _chemical_formula_moiety 'C32 H54 Cl2 P2 Pd, 1.33(C H Cl3)' _chemical_formula_sum 'C33.33 H55.33 Cl5.98 P2 Pd' _chemical_formula_weight 836.45 _chemical_name_common KM3-Pd _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2016-02-05 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _cell_angle_alpha 90 _cell_angle_beta 106.901(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.5058(6) _cell_length_b 15.1344(7) _cell_length_c 19.3313(11) _cell_measurement_reflns_used 5440 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.33 _cell_measurement_theta_min 2.26 _cell_volume 4060.6(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XM (Sheldrick, 2008)' _diffrn_ambient_temperature 100.15 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_unetI/netI 0.0937 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 33925 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.291 _diffrn_reflns_theta_min 2.202 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_T_max 0.2627 _exptl_absorpt_correction_T_min 0.2179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0617 before and 0.0565 after correction. The Ratio of minimum to maximum transmission is 0.8295. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description block _exptl_crystal_F_000 1732 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _refine_diff_density_max 2.681 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.151 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 10046 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0637 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+13.7539P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1498 _refine_ls_wR_factor_ref 0.1755 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6635 _reflns_number_total 10046 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om6b00101_si_002.cif _cod_data_source_block cain03 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4609 2016-04-01 06:22:49Z antanas ; _cod_database_code 4086447 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.911 _shelx_estimated_absorpt_t_min 0.744 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C33-Cl3 = C33-Cl4 = C33-Cl5 = C34-Cl6 = C34-Cl7 = C34-Cl8 1.73218 with sigma of 0.001 3. Others Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=Sof(C33)=Sof(H33)=FVAR(2) Sof(Cl6)=Sof(Cl7)=Sof(Cl8)=Sof(C34)=Sof(H34)=FVAR(3) 4.a Ternary CH refined with riding coordinates: C3(H3), C9(H9), C33(H33), C34(H34) 4.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B) 4.c Me refined with riding coordinates: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B, H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A, H30B,H30C), C31(H31A,H31B,H31C) 4.d Aromatic/amide H refined with riding coordinates: C2(H2), C17(H17), C19(H19) ; _shelx_res_file ; cain03.res created by SHELXL-2014/7 TITL CAIN02_a.res in P2(1)/c REM Old TITL CAIN02 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.160, Rweak 0.008, Alpha 0.050, Orientation as input REM Formula found by SHELXT: C38 Cl6 Pd CELL 0.71073 14.5058 15.1344 19.3313 90 106.901 90 ZERR 4 0.0006 0.0007 0.0011 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl P Pd UNIT 133.31 221.31 23.93 8 4 DFIX 21 0.001 C33 Cl3 C33 Cl4 C33 Cl5 C34 Cl6 C34 Cl7 C34 Cl8 L.S. 4 PLAN 10 SIZE 0.1 0.14 0.33 TEMP -173 BOND fmap 2 acta 50 OMIT -1 2 1 OMIT -1 2 3 REM REM REM WGHT 0.071600 13.753901 FVAR 0.26208 1.73218 0.57634 0.75075 PD1 5 0.866584 0.341987 0.741095 11.00000 0.01133 0.01672 = 0.01856 -0.00122 0.00493 -0.00031 P1 4 0.942201 0.217989 0.792895 11.00000 0.01356 0.01767 = 0.01966 -0.00173 0.00590 0.00090 P2 4 0.742561 0.285544 0.771474 11.00000 0.01154 0.02131 = 0.02459 0.00045 0.00571 -0.00050 CL1 3 1.009011 0.391537 0.719268 11.00000 0.01679 0.02304 = 0.03850 0.00028 0.01288 -0.00161 CL2 3 0.782113 0.472168 0.690640 11.00000 0.02143 0.02146 = 0.02867 0.00433 0.00548 0.00276 CL3 3 0.973775 0.468057 0.521789 31.00000 0.18581 0.06777 = 0.10797 -0.03378 0.10210 -0.02221 CL4 3 0.886658 0.301933 0.541534 31.00000 0.13681 0.03768 = 0.03305 0.00416 0.02626 0.02865 CL5 3 0.771628 0.450704 0.484123 31.00000 0.21131 0.06690 = 0.03301 -0.00675 -0.00486 0.08715 CL6 3 0.415253 0.364035 0.407146 41.00000 0.11360 0.12285 = 0.04285 0.01003 0.01782 -0.08568 CL7 3 0.495028 0.395735 0.291622 41.00000 0.07780 0.08561 = 0.06161 -0.02333 0.04347 -0.01524 CL8 3 0.556059 0.499153 0.421950 41.00000 0.09491 0.06143 = 0.07587 -0.01862 0.04088 -0.04027 C1 1 0.866946 0.158795 0.841440 11.00000 0.01860 0.01866 = 0.02795 0.00362 0.00990 0.00363 AFIX 23 H1A 2 0.864896 0.095078 0.829499 11.00000 -1.20000 H1B 2 0.896311 0.165154 0.894251 11.00000 -1.20000 AFIX 0 C2 1 0.766737 0.194940 0.820793 11.00000 0.01722 0.01989 = 0.02314 -0.00029 0.00952 -0.00190 AFIX 43 H2 2 0.717676 0.166112 0.835876 11.00000 -1.20000 AFIX 0 C3 1 0.962586 0.134871 0.729999 11.00000 0.01998 0.01616 = 0.02285 -0.00254 0.00913 0.00264 AFIX 13 H3 2 0.982181 0.079030 0.758080 11.00000 -1.20000 AFIX 0 C4 1 0.867553 0.115806 0.671126 11.00000 0.01879 0.02694 = 0.02367 -0.00658 0.00485 0.00015 AFIX 23 H4A 2 0.818596 0.095360 0.694075 11.00000 -1.20000 H4B 2 0.843574 0.170895 0.644302 11.00000 -1.20000 AFIX 0 C5 1 0.881516 0.045382 0.618384 11.00000 0.02382 0.02532 = 0.02555 -0.00758 0.00395 0.00177 AFIX 23 H5A 2 0.898171 -0.011551 0.644221 11.00000 -1.20000 H5B 2 0.820366 0.037233 0.579463 11.00000 -1.20000 AFIX 0 C6 1 0.960841 0.070913 0.585085 11.00000 0.03619 0.02949 = 0.01881 -0.00088 0.00770 0.00862 AFIX 23 H6A 2 0.969799 0.022988 0.552782 11.00000 -1.20000 H6B 2 0.941878 0.125109 0.555709 11.00000 -1.20000 AFIX 0 C7 1 1.055053 0.087069 0.643867 11.00000 0.02750 0.02735 = 0.02744 -0.00204 0.01023 0.00470 AFIX 23 H7A 2 1.105144 0.105540 0.621325 11.00000 -1.20000 H7B 2 1.076604 0.031398 0.670561 11.00000 -1.20000 AFIX 0 C8 1 1.043508 0.159043 0.697259 11.00000 0.01751 0.02662 = 0.02014 -0.00409 0.00983 0.00116 AFIX 23 H8A 2 1.104749 0.165616 0.736366 11.00000 -1.20000 H8B 2 1.028648 0.216302 0.671671 11.00000 -1.20000 AFIX 0 C9 1 1.056716 0.242648 0.860883 11.00000 0.01575 0.02503 = 0.02176 0.00103 0.00324 0.00258 AFIX 13 H9 2 1.100371 0.269952 0.835241 11.00000 -1.20000 AFIX 0 C10 1 1.107677 0.160035 0.900587 11.00000 0.02662 0.02957 = 0.02916 0.00296 0.00658 0.01209 AFIX 23 H10A 2 1.064501 0.129343 0.924098 11.00000 -1.20000 H10B 2 1.122089 0.118914 0.865271 11.00000 -1.20000 AFIX 0 C11 1 1.201515 0.185391 0.957808 11.00000 0.02409 0.05101 = 0.03969 0.00967 -0.00018 0.01627 AFIX 23 H11A 2 1.231709 0.131763 0.984144 11.00000 -1.20000 H11B 2 1.246932 0.211252 0.933812 11.00000 -1.20000 AFIX 0 C12 1 1.182338 0.252194 1.011482 11.00000 0.01957 0.05058 = 0.02817 0.00653 -0.00403 0.00411 AFIX 23 H12A 2 1.139664 0.225400 1.037443 11.00000 -1.20000 H12B 2 1.243822 0.268343 1.047570 11.00000 -1.20000 AFIX 0 C13 1 1.134976 0.334621 0.971504 11.00000 0.02368 0.03900 = 0.01828 -0.00152 0.00038 -0.00220 AFIX 23 H13A 2 1.179183 0.362982 0.947647 11.00000 -1.20000 H13B 2 1.122220 0.377260 1.006463 11.00000 -1.20000 AFIX 0 C14 1 1.040412 0.311231 0.914773 11.00000 0.01700 0.02671 = 0.01566 0.00070 0.00036 0.00112 AFIX 23 H14A 2 1.011862 0.365335 0.888337 11.00000 -1.20000 H14B 2 0.994408 0.287281 0.939091 11.00000 -1.20000 AFIX 0 C15 1 0.618910 0.321675 0.759594 11.00000 0.01324 0.02494 = 0.02160 0.00067 0.00581 -0.00081 C16 1 0.543260 0.293465 0.697010 11.00000 0.01873 0.02201 = 0.02262 -0.00443 0.00182 -0.00424 C17 1 0.449462 0.310444 0.697449 11.00000 0.01239 0.02978 = 0.02768 -0.00533 0.00249 -0.00283 AFIX 43 H17 2 0.398666 0.292627 0.656528 11.00000 -1.20000 AFIX 0 C18 1 0.424872 0.351849 0.753870 11.00000 0.01050 0.02478 = 0.03061 -0.00151 0.00444 0.00211 C19 1 0.499785 0.381124 0.811391 11.00000 0.02037 0.02971 = 0.02633 -0.00835 0.01074 0.00414 AFIX 43 H19 2 0.484338 0.411148 0.849729 11.00000 -1.20000 AFIX 0 C20 1 0.597174 0.368977 0.816281 11.00000 0.01441 0.02761 = 0.02161 0.00029 0.00714 -0.00094 C21 1 0.628959 0.297987 0.598890 11.00000 0.03453 0.05906 = 0.02883 -0.01685 0.01172 -0.00858 AFIX 33 H21A 2 0.690753 0.305272 0.636226 11.00000 -1.50000 H21B 2 0.639070 0.265807 0.557707 11.00000 -1.50000 H21C 2 0.601419 0.356218 0.582846 11.00000 -1.50000 AFIX 0 C22 1 0.595293 0.149504 0.648562 11.00000 0.03133 0.04190 = 0.04696 -0.02157 -0.00064 0.00320 AFIX 33 H22A 2 0.655993 0.150399 0.687693 11.00000 -1.50000 H22B 2 0.547114 0.115594 0.663910 11.00000 -1.50000 H22C 2 0.605817 0.121881 0.605634 11.00000 -1.50000 AFIX 0 C23 1 0.464245 0.236714 0.568914 11.00000 0.02717 0.04740 = 0.02949 -0.01419 0.00090 -0.00055 AFIX 33 H23A 2 0.417237 0.203649 0.586242 11.00000 -1.50000 H23B 2 0.438757 0.295705 0.553248 11.00000 -1.50000 H23C 2 0.476408 0.205294 0.528109 11.00000 -1.50000 AFIX 0 C24 1 0.558876 0.245330 0.630309 11.00000 0.01796 0.03721 = 0.03375 -0.01579 0.00569 -0.00707 C25 1 0.306001 0.401362 0.820032 11.00000 0.02276 0.06675 = 0.05846 -0.01735 0.01975 -0.00139 AFIX 33 H25A 2 0.237141 0.408671 0.814655 11.00000 -1.50000 H25B 2 0.333998 0.360000 0.859566 11.00000 -1.50000 H25C 2 0.338415 0.458678 0.830951 11.00000 -1.50000 AFIX 0 C26 1 0.272926 0.429510 0.688308 11.00000 0.01955 0.04911 = 0.07788 0.01472 0.01349 0.00506 AFIX 33 H26A 2 0.281076 0.406696 0.643004 11.00000 -1.50000 H26B 2 0.204091 0.435461 0.683577 11.00000 -1.50000 H26C 2 0.304118 0.487401 0.698898 11.00000 -1.50000 AFIX 0 C27 1 0.264893 0.277138 0.734412 11.00000 0.02035 0.03954 = 0.05977 0.00024 0.01076 -0.00582 AFIX 33 H27A 2 0.271910 0.251996 0.689497 11.00000 -1.50000 H27B 2 0.291640 0.236057 0.774405 11.00000 -1.50000 H27C 2 0.196470 0.287032 0.729318 11.00000 -1.50000 AFIX 0 C28 1 0.319112 0.365260 0.750079 11.00000 0.01245 0.03729 = 0.03743 -0.00281 0.00710 -0.00001 C29 1 0.632969 0.491127 0.908992 11.00000 0.05594 0.12746 = 0.16199 -0.12276 -0.04797 0.04165 AFIX 33 H29A 2 0.567243 0.481854 0.911697 11.00000 -1.50000 H29B 2 0.674612 0.508991 0.956553 11.00000 -1.50000 H29C 2 0.632693 0.537568 0.873605 11.00000 -1.50000 AFIX 0 C30 1 0.678484 0.338379 0.946819 11.00000 0.10537 0.13208 = 0.02979 0.01049 -0.00718 -0.07540 AFIX 33 H30A 2 0.613981 0.324188 0.950119 11.00000 -1.50000 H30B 2 0.709179 0.284532 0.935989 11.00000 -1.50000 H30C 2 0.717447 0.363041 0.992931 11.00000 -1.50000 AFIX 0 C31 1 0.770648 0.426066 0.883274 11.00000 0.03620 0.08491 = 0.03967 -0.03294 0.01583 -0.03547 AFIX 33 H31A 2 0.798390 0.372759 0.868552 11.00000 -1.50000 H31B 2 0.768555 0.473363 0.848226 11.00000 -1.50000 H31C 2 0.810475 0.444786 0.931174 11.00000 -1.50000 AFIX 0 C32 1 0.670381 0.406601 0.886139 11.00000 0.01761 0.04847 = 0.02468 -0.01358 0.00167 0.00314 C33 1 0.879513 0.416067 0.543581 31.00000 0.05501 0.04589 = 0.00916 0.00002 0.02038 0.01617 AFIX 13 H33 2 0.880699 0.434445 0.593521 31.00000 -1.20000 AFIX 0 C34 1 0.461569 0.443632 0.362102 41.00000 0.03572 0.03930 = 0.03822 -0.00265 0.00902 0.01376 AFIX 13 H34 2 0.409402 0.487481 0.340995 41.00000 -1.20000 AFIX 0 HKLF 4 REM CAIN02_a.res in P2(1)/c REM R1 = 0.0637 for 6635 Fo > 4sig(Fo) and 0.1092 for all 10046 data REM 409 parameters refined using 6 restraints END WGHT 0.0715 13.7729 REM Highest difference peak 2.681, deepest hole -1.041, 1-sigma level 0.151 Q1 1 0.4744 0.3104 0.3825 11.00000 0.05 2.68 Q2 1 0.5107 0.4858 0.3395 11.00000 0.05 2.17 Q3 1 0.4615 0.4578 0.4689 11.00000 0.05 2.03 Q4 1 0.9891 0.3594 0.5486 11.00000 0.05 1.78 Q5 1 0.8019 0.2936 0.5237 11.00000 0.05 1.60 Q6 1 0.3939 0.3715 0.3996 11.00000 0.05 1.27 Q7 1 0.8313 0.4057 0.5275 11.00000 0.05 1.07 Q8 1 0.8645 0.3728 0.5425 11.00000 0.05 0.94 Q9 1 0.8510 0.4172 0.5592 11.00000 0.05 0.89 Q10 1 0.8376 0.4745 0.4830 11.00000 0.05 0.86 ; _shelx_res_checksum 48599 _shelx_hkl_file ; 2 0 0 1686.53 59.79 2 0 0 1622.24 56.79 -2 0 0 1652.43 56.89 -2 0 0 1735.43 59.79 -2 0 0 1685.23 60.09 -3 0 0 1686.53 62.59 3 0 0 1729.53 62.39 3 0 0 1787.82 58.29 -3 0 0 1679.43 58.19 -3 0 0 1518.75 62.69 4 0 0 4.70 3.40 -4 0 0 -0.70 7.50 -4 0 0 -2.80 7.90 4 0 0 0.40 5.70 -4 0 0 6.10 3.20 -5 0 0 22.00 10.20 -5 0 0 7.00 6.60 -5 0 0 18.00 4.30 5 0 0 22.90 4.60 5 0 0 11.60 8.90 -6 0 0 51.89 6.10 6 0 0 61.79 6.30 6 0 0 59.69 12.30 -6 0 0 46.00 10.80 -7 0 0 1145.29 43.00 7 0 0 1057.99 42.20 7 0 0 1162.28 53.19 -7 0 0 1138.79 55.19 8 0 0 1256.37 59.29 8 0 0 1321.17 48.80 -8 0 0 1293.97 49.10 -8 0 0 1283.67 63.09 -9 0 0 342.57 17.80 9 0 0 342.07 27.30 -9 0 0 349.17 32.20 -10 0 0 507.35 36.90 10 0 0 470.25 36.20 -10 0 0 449.46 21.80 11 0 0 1538.15 73.99 -11 0 0 1412.86 54.39 -11 0 0 1446.16 76.19 -12 0 0 554.24 47.40 12 0 0 686.63 47.50 -13 0 0 35.50 10.80 13 0 0 3.50 11.70 -13 0 0 2.90 18.60 -14 0 0 104.29 23.70 -14 0 0 148.79 19.10 14 0 0 176.08 27.00 -15 0 0 676.03 55.09 15 0 0 858.11 59.19 16 0 0 509.25 49.99 -16 0 0 466.85 52.79 17 0 0 -2.00 16.90 -17 0 0 -2.10 21.40 -18 0 0 -12.00 23.80 18 0 0 -11.10 18.00 0 -1 0 -1.70 1.20 0 1 0 -2.20 1.40 -2 -1 0 1496.05 51.99 2 -1 0 1497.15 52.89 2 -1 0 1414.36 50.09 2 -1 0 1489.15 53.49 -2 -1 0 1439.96 50.99 -2 1 0 1468.65 52.99 2 1 0 1444.36 51.89 -2 1 0 1385.46 52.79 -3 -1 0 337.77 15.50 -3 -1 0 335.77 18.10 3 -1 0 346.67 14.40 3 -1 0 356.56 20.20 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506.15 45.30 8 -5 14 513.95 51.49 -8 5 -14 409.56 47.30 8 5 14 407.96 34.20 9 -5 14 413.36 48.10 -9 -5 -14 392.26 44.40 -9 5 -14 338.67 48.50 9 5 14 344.67 33.20 10 -5 14 9.50 21.70 -10 -5 -14 -17.30 11.40 -10 5 -14 -7.20 16.30 11 -5 14 68.59 23.90 -11 -5 -14 101.09 24.80 -11 5 -14 91.69 32.50 -17 -6 14 172.38 32.80 -16 -6 14 243.78 38.80 -15 -6 14 156.28 31.30 -14 -6 14 10.30 17.20 -14 6 14 15.40 14.70 -13 -6 14 87.89 26.30 -13 6 14 52.19 16.20 -13 6 14 75.99 16.80 -12 -6 14 64.19 24.80 -12 6 14 133.89 19.50 -12 6 14 99.79 18.10 -11 -6 14 182.68 33.00 -11 6 14 212.98 27.10 -11 6 14 191.38 21.60 -10 -6 14 53.39 18.50 -9 -6 14 221.68 34.20 -8 -6 14 628.24 48.70 -7 -6 14 14.10 16.20 -6 -6 14 101.79 22.80 -5 -6 14 176.08 27.00 -5 6 14 173.68 13.00 -4 -6 14 83.69 19.40 -4 6 14 92.49 9.90 -3 -6 14 5.30 11.60 -3 6 14 4.00 5.00 -2 -6 14 382.46 36.80 2 -6 -14 393.76 23.30 -2 6 14 358.36 21.60 2 6 -14 369.26 34.10 -1 -6 14 551.64 43.70 1 -6 -14 625.74 33.30 1 6 -14 709.63 48.60 0 -6 -14 696.23 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27.30 -11 3 22 20.20 23.50 -10 -3 22 9.20 19.30 -10 3 22 27.60 26.20 -9 -3 22 32.40 19.90 -9 3 22 16.30 23.10 -8 -3 22 -6.10 16.30 -8 3 22 1.10 20.50 -7 -3 22 7.00 24.20 -7 3 22 18.90 19.40 -6 -3 22 50.29 27.80 -6 3 22 12.20 24.00 -5 -3 22 -18.90 12.50 -5 3 22 -3.60 13.20 -4 -3 22 -3.80 18.50 -4 3 22 -12.00 19.00 -3 -3 22 -8.30 12.40 -2 -3 22 24.90 21.00 2 3 -22 25.10 21.30 -1 -3 22 49.20 22.20 1 3 -22 26.10 16.70 0 -3 -22 -11.80 18.00 0 -3 22 -3.10 11.50 0 3 -22 12.60 19.80 -1 -3 -22 52.19 22.00 1 -3 22 -2.80 17.10 -1 3 -22 7.80 19.40 2 -3 22 35.40 22.90 -2 -3 -22 36.50 18.90 -2 3 -22 31.60 22.70 2 3 22 41.40 18.00 -3 -3 -22 59.19 22.00 3 -3 22 69.29 26.20 -3 3 -22 67.79 28.00 3 3 22 39.20 17.70 4 -3 22 19.00 17.90 -4 -3 -22 18.40 16.50 -4 3 -22 71.29 22.80 -13 -4 22 -9.50 22.10 -13 4 22 -1.70 20.00 -12 -4 22 18.80 23.10 -12 4 22 -14.30 20.40 -11 -4 22 1.30 17.20 -11 4 22 -3.20 14.30 -10 -4 22 -10.20 17.00 -10 4 22 11.80 19.20 -9 -4 22 74.59 31.50 -9 4 22 69.79 30.20 -8 -4 22 191.98 39.00 -8 4 22 166.68 37.50 -7 -4 22 -1.10 18.40 -6 -4 22 121.39 30.00 -5 -4 22 258.77 41.40 -4 -4 22 25.10 22.30 -3 -4 22 -10.90 18.70 -2 -4 22 15.00 18.50 -1 -4 22 -13.80 11.90 1 4 -22 6.40 19.90 0 -4 22 14.00 17.90 0 4 -22 16.20 19.50 1 -4 22 -7.80 17.80 1 4 22 16.20 16.50 -1 4 -22 -8.60 19.80 2 -4 22 180.48 36.00 -2 4 -22 186.68 33.40 3 -4 22 77.99 27.90 -3 4 -22 16.50 24.80 4 -4 22 20.30 19.00 -4 4 -22 -5.60 20.20 -13 -5 22 4.10 23.80 -12 -5 22 153.78 32.70 -11 -5 22 156.28 39.10 -10 -5 22 170.28 37.60 -9 -5 22 -30.10 21.50 -8 -5 22 65.29 31.50 -7 -5 22 383.16 52.49 -6 -5 22 101.09 32.50 -5 -5 22 -21.00 13.70 -4 -5 22 23.20 24.40 -3 -5 22 47.60 20.80 -2 -5 22 -9.10 18.20 -1 -5 22 32.60 22.80 1 5 -22 56.69 24.50 0 -5 22 70.49 25.20 0 5 -22 56.89 21.80 1 -5 22 64.29 24.50 -1 5 -22 122.39 30.20 2 -5 22 22.00 22.70 -2 5 -22 -5.80 21.60 3 -5 22 43.40 25.30 -3 5 -22 54.79 25.00 -12 -6 22 80.69 27.70 -11 -6 22 -17.00 20.50 -10 -6 22 56.59 28.90 -9 -6 22 102.59 29.30 -8 -6 22 35.60 21.60 -7 -6 22 35.00 20.00 -6 -6 22 54.09 27.80 -5 -6 22 72.09 29.50 -4 -6 22 101.99 26.50 -3 -6 22 11.80 22.60 -2 -6 22 126.09 33.20 -1 -6 22 216.88 33.80 1 6 -22 196.38 33.90 0 -6 22 9.60 15.20 0 6 -22 27.40 22.70 1 -6 22 12.80 19.30 -1 6 -22 2.10 23.30 2 -6 22 91.09 30.80 -2 6 -22 53.89 21.30 3 -6 22 15.60 22.40 -3 6 -22 40.10 20.30 -10 -7 22 51.59 24.20 -9 -7 22 13.00 20.00 -8 -7 22 39.50 22.30 -7 -7 22 57.49 24.10 -6 -7 22 45.40 22.10 -5 -7 22 69.39 27.40 -4 -7 22 29.80 22.90 -3 -7 22 59.29 21.90 -1 -7 22 31.00 24.40 1 7 -22 39.00 26.50 0 -7 22 85.29 28.50 0 7 -22 199.78 38.60 1 -7 22 37.30 34.80 -1 7 -22 49.40 21.00 2 -7 22 26.20 18.60 -2 7 -22 -14.20 21.50 -11 -8 22 29.30 26.90 -10 -8 22 -9.10 14.80 -9 -8 22 36.20 20.40 -8 -8 22 -16.70 14.90 -7 -8 22 -30.30 13.90 -6 -8 22 -5.90 15.30 -5 -8 22 12.90 18.10 -4 -8 22 14.60 24.90 -3 -8 22 11.40 17.30 -1 -8 22 -13.30 21.80 0 -8 22 23.60 22.10 0 8 -22 -11.70 13.60 1 -8 22 37.80 28.00 -1 8 -22 5.90 24.40 -9 -9 22 3.90 17.60 -8 -9 22 31.90 19.70 -7 -9 22 64.49 26.50 -6 -9 22 54.59 23.90 -5 -9 22 -4.20 16.10 -4 -9 22 29.90 22.40 -3 -9 22 -19.70 21.80 -2 -9 22 41.90 25.60 -1 -9 22 33.90 18.00 0 -9 22 30.40 25.20 0 9 -22 14.80 27.20 -7 -10 22 -21.40 13.30 -6 -10 22 105.59 30.60 -5 -10 22 88.19 27.90 -4 -10 22 6.10 24.70 -3 -10 22 0.90 22.60 -2 -10 22 -6.80 22.40 -13 0 23 5.90 24.40 -12 0 23 -16.90 22.10 -11 0 23 5.40 25.30 -10 0 23 4.20 25.60 -9 0 23 0.20 23.10 -8 0 23 6.10 24.30 -7 0 23 -36.80 17.70 -6 0 23 -19.00 14.00 -5 0 23 -33.50 18.10 -4 0 23 -10.40 13.10 -3 0 23 -34.00 10.30 -2 0 23 -8.20 19.10 1 0 -23 -5.70 9.80 -1 0 23 -13.90 10.00 0 0 23 10.50 16.80 0 0 -23 -3.60 16.40 -1 0 -23 8.00 17.80 -2 0 -23 -11.50 17.70 2 0 23 14.60 14.40 -3 0 -23 20.20 21.40 3 0 23 1.20 12.60 -13 -1 23 63.99 27.50 -13 1 23 -2.30 13.40 -12 -1 23 126.19 32.00 -12 1 23 130.49 32.20 -11 -1 23 112.59 31.40 -11 1 23 114.29 31.20 -10 -1 23 42.20 26.60 -10 1 23 36.50 27.40 -9 -1 23 -20.50 22.30 -9 1 23 17.90 18.80 -8 -1 23 21.50 18.50 -8 1 23 2.60 17.50 -7 -1 23 -4.80 16.20 -7 1 23 11.60 24.20 -6 -1 23 4.30 22.30 -6 1 23 0.80 21.90 -5 -1 23 -10.20 13.40 -5 1 23 -27.90 17.50 -4 -1 23 41.30 24.40 -4 1 23 47.10 26.60 -3 -1 23 37.60 24.30 -3 1 23 -21.60 18.60 -2 -1 23 75.69 23.10 -2 1 23 11.70 20.60 1 -1 -23 40.80 16.00 -1 -1 23 44.50 22.60 -1 1 23 17.70 20.30 1 1 -23 -2.30 12.10 0 -1 -23 35.20 20.10 0 -1 23 41.20 19.40 0 1 -23 30.90 20.90 -1 -1 -23 48.80 19.90 1 -1 23 38.80 18.60 -1 1 -23 -32.70 16.90 2 -1 23 -0.50 13.70 -2 -1 -23 12.60 13.70 2 1 23 35.70 20.20 -2 1 -23 0.40 18.30 3 -1 23 92.29 23.30 -3 -1 -23 77.39 26.80 -3 1 -23 117.39 29.90 3 1 23 65.29 23.40 -13 -2 23 103.19 29.20 -13 2 23 56.19 29.00 -12 -2 23 96.99 33.60 -12 2 23 55.69 29.50 -11 -2 23 -4.60 22.90 -11 2 23 -1.90 22.80 -10 -2 23 116.29 36.50 -10 2 23 102.19 33.10 -9 -2 23 334.37 53.19 -9 2 23 320.97 50.89 -8 -2 23 40.90 28.50 -8 2 23 53.49 28.60 -7 -2 23 -11.40 24.00 -7 2 23 -31.30 12.00 -6 -2 23 84.89 26.40 -6 2 23 107.59 32.80 -5 -2 23 24.30 24.50 -5 2 23 55.59 20.20 -4 -2 23 112.09 27.60 -4 2 23 142.39 32.80 -3 -2 23 31.30 22.30 -3 2 23 7.10 21.00 -2 -2 23 100.99 28.30 1 -2 -23 74.59 27.20 -1 -2 23 69.79 25.90 1 2 -23 117.49 27.60 0 -2 -23 21.70 16.90 0 -2 23 12.00 17.70 0 2 -23 13.00 21.70 1 -2 23 44.70 19.40 -1 -2 -23 46.30 20.40 1 2 23 -3.40 17.80 -1 2 -23 60.09 20.60 -2 -2 -23 200.28 32.70 2 -2 23 160.48 30.60 2 2 23 135.89 28.10 -2 2 -23 171.18 33.30 3 -2 23 92.89 26.40 -3 -2 -23 15.60 20.50 -3 2 -23 69.29 26.80 3 2 23 59.49 20.20 -12 -3 23 99.89 33.40 -12 3 23 91.99 28.50 -11 -3 23 174.38 36.00 -11 3 23 129.29 31.90 -10 -3 23 227.08 42.20 -10 3 23 259.37 41.80 -9 -3 23 16.00 21.50 -9 3 23 30.60 23.20 -8 -3 23 88.29 26.10 -8 3 23 159.08 37.90 -7 -3 23 106.19 27.80 -7 3 23 93.59 29.20 -6 -3 23 33.90 26.80 -6 3 23 39.80 20.60 -5 -3 23 66.39 28.80 -5 3 23 98.39 29.70 -4 -3 23 66.49 29.60 -3 -3 23 104.49 27.20 -2 -3 23 64.09 24.80 -1 -3 23 39.00 23.90 1 3 -23 20.70 20.10 0 -3 23 4.30 13.40 0 3 -23 -11.10 14.40 1 -3 23 8.30 23.10 -1 3 -23 33.40 23.90 1 3 23 20.30 13.10 2 -3 23 13.30 21.00 -2 3 -23 -1.00 22.80 2 3 23 1.50 15.70 -12 -4 23 57.59 25.10 -12 4 23 -7.40 24.40 -11 -4 23 20.10 29.00 -11 4 23 9.30 23.60 -10 -4 23 106.59 37.10 -10 4 23 124.39 33.70 -9 -4 23 192.58 40.80 -9 4 23 168.28 39.30 -8 -4 23 49.80 31.70 -7 -4 23 10.60 27.50 -6 -4 23 49.00 24.30 -5 -4 23 135.69 34.80 -4 -4 23 74.29 24.00 -3 -4 23 11.00 22.70 -2 -4 23 76.89 29.00 -1 -4 23 -7.70 19.60 1 4 -23 3.50 20.00 0 -4 23 11.90 19.10 0 4 -23 43.20 22.10 -1 4 -23 -25.20 11.90 2 -4 23 1.30 14.60 -2 4 -23 56.39 26.50 -11 -5 23 0.40 24.40 -10 -5 23 53.89 28.80 -9 -5 23 72.79 32.60 -8 -5 23 9.00 26.40 -7 -5 23 24.10 29.60 -6 -5 23 29.00 29.80 -5 -5 23 91.79 27.50 -4 -5 23 109.49 30.80 -3 -5 23 12.80 17.40 -2 -5 23 2.70 23.90 -1 -5 23 11.80 23.60 1 5 -23 14.10 16.40 0 -5 23 3.60 20.00 0 5 -23 0.80 20.80 -1 5 -23 17.70 22.80 -11 -6 23 3.10 23.90 -10 -6 23 -8.00 25.20 -9 -6 23 -21.60 16.80 -8 -6 23 30.50 20.20 -7 -6 23 31.20 22.60 -6 -6 23 178.88 40.40 -5 -6 23 58.49 30.90 -4 -6 23 6.20 18.70 -3 -6 23 91.09 30.60 -2 -6 23 -9.20 22.30 -1 -6 23 80.79 29.30 1 6 -23 -9.00 22.40 0 -6 23 41.80 25.30 0 6 -23 37.00 25.20 1 -6 23 44.00 23.90 -1 6 -23 4.60 14.30 -10 -7 23 -4.80 15.60 -9 -7 23 -2.30 17.70 -8 -7 23 55.09 23.50 -7 -7 23 47.00 22.40 -6 -7 23 9.50 17.10 -4 -7 23 339.17 48.70 -3 -7 23 54.09 29.70 -2 -7 23 118.09 29.60 -1 -7 23 39.80 26.00 0 -7 23 23.70 24.80 0 7 -23 38.70 26.30 -8 -8 23 41.80 23.90 -7 -8 23 15.50 19.00 -6 -8 23 163.08 37.20 -5 -8 23 124.39 35.70 -4 -8 23 23.20 24.30 -3 -8 23 1.00 24.40 -2 -8 23 273.27 43.80 -6 -9 23 -22.40 13.10 -5 -9 23 71.19 30.70 -4 -9 23 37.20 24.50 -11 0 24 39.70 21.10 -10 0 24 130.29 32.90 -9 0 24 198.78 38.00 -8 0 24 -11.40 17.00 -7 0 24 14.80 24.50 -6 0 24 85.79 30.70 -5 0 24 352.56 49.10 -4 0 24 198.98 34.30 -3 0 24 27.90 23.40 -2 0 24 443.36 51.19 1 0 -24 185.68 33.10 -1 0 24 194.68 33.80 0 0 -24 -4.40 12.40 1 0 24 17.90 20.50 -1 0 -24 -31.60 15.90 -11 -1 24 99.59 33.70 -11 1 24 185.28 41.10 -10 -1 24 43.50 27.10 -10 1 24 55.49 31.10 -9 -1 24 8.00 24.90 -9 1 24 -1.00 23.10 -8 -1 24 44.40 28.00 -8 1 24 52.39 29.00 -7 -1 24 -1.00 18.70 -7 1 24 30.20 20.10 -6 -1 24 50.09 27.50 -6 1 24 59.19 26.20 -5 -1 24 64.79 29.40 -5 1 24 -1.20 15.70 -4 -1 24 134.79 34.00 -4 1 24 96.09 30.10 -3 -1 24 326.87 42.10 -3 1 24 330.17 44.80 -2 -1 24 139.89 28.70 -2 1 24 71.49 26.60 1 -1 -24 52.39 19.30 -1 -1 24 16.30 14.40 1 1 -24 8.60 20.80 0 -1 24 59.69 25.40 0 -1 -24 115.19 23.40 0 1 -24 70.59 22.10 -1 -1 -24 -34.80 16.50 1 -1 24 20.50 19.00 -1 1 -24 -23.10 15.90 1 1 24 1.20 16.30 -11 -2 24 -14.50 17.70 -11 2 24 33.70 20.20 -10 -2 24 35.50 23.30 -10 2 24 14.50 18.70 -9 -2 24 -0.70 19.60 -9 2 24 24.10 21.40 -8 -2 24 39.00 28.20 -8 2 24 1.90 17.10 -7 -2 24 47.10 28.30 -7 2 24 7.20 24.90 -6 -2 24 126.29 32.50 -6 2 24 40.10 20.80 -5 -2 24 7.80 22.60 -5 2 24 34.70 25.10 -4 -2 24 26.00 25.70 -4 2 24 9.90 16.00 -3 -2 24 10.80 23.40 -2 -2 24 19.70 22.80 -1 -2 24 25.80 20.50 1 2 -24 3.60 20.30 0 -2 24 44.60 22.80 0 2 -24 -14.10 19.70 1 -2 24 -7.10 19.20 -1 2 -24 -0.20 14.10 1 2 24 7.50 18.40 -11 -3 24 20.10 21.70 -11 3 24 3.80 25.90 -10 -3 24 8.50 27.20 -10 3 24 24.70 26.50 -9 -3 24 80.19 33.10 -9 3 24 69.49 32.20 -8 -3 24 16.40 20.10 -8 3 24 36.20 28.10 -7 -3 24 17.20 18.70 -7 3 24 -0.60 16.30 -6 -3 24 49.50 27.10 -6 3 24 -33.70 19.30 -5 -3 24 -31.70 21.50 -4 -3 24 46.20 28.60 -3 -3 24 33.80 19.60 -2 -3 24 27.20 23.70 -1 -3 24 -13.30 19.80 1 3 -24 18.80 17.30 0 -3 24 -9.40 12.10 0 3 -24 35.40 23.10 -10 -4 24 37.60 28.60 -9 -4 24 139.59 38.80 -8 -4 24 94.29 35.40 -7 -4 24 -13.30 23.60 -6 -4 24 42.80 22.90 -5 -4 24 29.40 24.90 -4 -4 24 -13.20 14.90 -3 -4 24 -3.30 22.60 -2 -4 24 -11.10 21.60 -1 -4 24 27.60 22.50 1 4 -24 1.80 23.40 0 -4 24 11.90 20.80 0 4 -24 -3.80 15.30 -10 -5 24 86.19 30.70 -9 -5 24 39.60 27.60 -8 -5 24 61.59 32.50 -7 -5 24 192.38 43.40 -6 -5 24 -2.30 27.10 -5 -5 24 19.80 17.60 -4 -5 24 22.50 26.50 -3 -5 24 -21.90 13.40 -2 -5 24 22.90 16.90 -1 -5 24 -17.40 21.10 -9 -6 24 60.29 24.10 -8 -6 24 -16.00 15.20 -7 -6 24 8.00 23.00 -4 -6 24 13.50 25.20 -3 -6 24 -36.30 19.90 -2 -6 24 84.39 29.70 -7 -7 24 132.29 31.20 -6 -7 24 82.39 31.00 -4 -7 24 2.20 18.70 -9 0 25 13.30 26.40 -8 0 25 10.60 25.60 -7 0 25 16.90 17.60 -6 0 25 46.40 28.00 -5 0 25 12.50 15.20 -4 0 25 17.00 21.40 -3 0 25 -9.90 20.50 -2 0 25 -47.90 16.70 -1 0 25 -5.20 18.50 1 0 -25 -10.30 19.00 -9 -1 25 43.30 26.70 -9 1 25 37.10 20.50 -8 -1 25 12.10 24.10 -8 1 25 12.60 22.80 -7 -1 25 65.89 31.40 -7 1 25 28.50 25.00 -6 -1 25 14.60 19.90 -6 1 25 12.40 18.80 -5 -1 25 29.50 22.50 -5 1 25 8.50 24.00 -4 -1 25 76.49 28.80 -4 1 25 101.19 29.20 -3 -1 25 197.68 34.50 -3 1 25 80.49 25.20 -2 -1 25 21.10 22.20 -9 -2 25 157.48 34.60 -9 2 25 187.18 42.00 -8 -2 25 33.10 20.30 -8 2 25 8.30 24.10 -7 2 25 17.30 16.90 -6 -2 25 87.99 34.10 -6 2 25 117.89 31.00 -5 -2 25 49.40 23.00 -5 2 25 61.59 22.50 -4 -2 25 49.30 26.80 -3 -2 25 157.78 35.90 -2 -2 25 130.09 32.60 -8 -3 25 137.99 36.20 -8 3 25 36.10 28.00 -7 -3 25 134.29 32.20 -7 3 25 136.19 37.00 -6 -3 25 34.30 27.80 -5 -3 25 20.30 25.90 -4 -3 25 54.19 28.40 -3 -3 25 144.59 31.00 -2 -3 25 39.00 26.30 -8 -4 25 45.00 29.00 -7 -4 25 33.20 25.40 -6 -4 25 27.30 19.80 -5 -4 25 7.90 24.70 -4 -4 25 -8.80 17.10 -3 -4 25 10.40 24.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 69407 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.86658(2) 0.34199(2) 0.74109(2) 0.01541(11) Uani 1 1 d . . . . . P1 P 0.94220(9) 0.21799(8) 0.79289(7) 0.0167(3) Uani 1 1 d . . . . . P2 P 0.74256(9) 0.28554(9) 0.77147(8) 0.0190(3) Uani 1 1 d . . . . . Cl1 Cl 1.00901(8) 0.39154(8) 0.71927(8) 0.0251(3) Uani 1 1 d . . . . . Cl2 Cl 0.78211(9) 0.47217(8) 0.69064(8) 0.0242(3) Uani 1 1 d . . . . . Cl3 Cl 0.9738(4) 0.4681(3) 0.5218(3) 0.108(2) Uani 0.576(5) 1 d D . P . . Cl4 Cl 0.8867(3) 0.3019(2) 0.54153(18) 0.0688(14) Uani 0.576(5) 1 d D . P . . Cl5 Cl 0.7716(4) 0.4507(3) 0.4841(2) 0.112(3) Uani 0.576(5) 1 d D . P . . Cl6 Cl 0.4153(3) 0.3640(3) 0.40715(16) 0.0941(15) Uani 0.751(5) 1 d D . P . . Cl7 Cl 0.4950(2) 0.3957(2) 0.29162(17) 0.0701(10) Uani 0.751(5) 1 d D . P . . Cl8 Cl 0.5561(2) 0.4992(2) 0.42195(18) 0.0740(11) Uani 0.751(5) 1 d D . P . . C1 C 0.8669(3) 0.1588(3) 0.8414(3) 0.0211(11) Uani 1 1 d . . . . . H1A H 0.8649 0.0951 0.8295 0.025 Uiso 1 1 calc R . . . . H1B H 0.8963 0.1652 0.8943 0.025 Uiso 1 1 calc R . . . . C2 C 0.7667(3) 0.1949(3) 0.8208(3) 0.0193(11) Uani 1 1 d . . . . . H2 H 0.7177 0.1661 0.8359 0.023 Uiso 1 1 calc R . . . . C3 C 0.9626(3) 0.1349(3) 0.7300(3) 0.0191(11) Uani 1 1 d . . . . . H3 H 0.9822 0.0790 0.7581 0.023 Uiso 1 1 calc R . . . . C4 C 0.8676(4) 0.1158(4) 0.6711(3) 0.0234(12) Uani 1 1 d . . . . . H4A H 0.8186 0.0954 0.6941 0.028 Uiso 1 1 calc R . . . . H4B H 0.8436 0.1709 0.6443 0.028 Uiso 1 1 calc R . . . . C5 C 0.8815(4) 0.0454(4) 0.6184(3) 0.0256(12) Uani 1 1 d . . . . . H5A H 0.8982 -0.0116 0.6442 0.031 Uiso 1 1 calc R . . . . H5B H 0.8204 0.0372 0.5795 0.031 Uiso 1 1 calc R . . . . C6 C 0.9608(4) 0.0709(4) 0.5851(3) 0.0282(13) Uani 1 1 d . . . . . H6A H 0.9698 0.0230 0.5528 0.034 Uiso 1 1 calc R . . . . H6B H 0.9419 0.1251 0.5557 0.034 Uiso 1 1 calc R . . . . C7 C 1.0551(4) 0.0871(4) 0.6439(3) 0.0270(12) Uani 1 1 d . . . . . H7A H 1.1051 0.1055 0.6213 0.032 Uiso 1 1 calc R . . . . H7B H 1.0766 0.0314 0.6706 0.032 Uiso 1 1 calc R . . . . C8 C 1.0435(3) 0.1590(4) 0.6973(3) 0.0205(11) Uani 1 1 d . . . . . H8A H 1.1047 0.1656 0.7364 0.025 Uiso 1 1 calc R . . . . H8B H 1.0286 0.2163 0.6717 0.025 Uiso 1 1 calc R . . . . C9 C 1.0567(3) 0.2426(3) 0.8609(3) 0.0213(11) Uani 1 1 d . . . . . H9 H 1.1004 0.2700 0.8352 0.026 Uiso 1 1 calc R . . . . C10 C 1.1077(4) 0.1600(4) 0.9006(3) 0.0288(13) Uani 1 1 d . . . . . H10A H 1.0645 0.1293 0.9241 0.035 Uiso 1 1 calc R . . . . H10B H 1.1221 0.1189 0.8653 0.035 Uiso 1 1 calc R . . . . C11 C 1.2015(4) 0.1854(5) 0.9578(4) 0.0403(16) Uani 1 1 d . . . . . H11A H 1.2317 0.1318 0.9841 0.048 Uiso 1 1 calc R . . . . H11B H 1.2469 0.2113 0.9338 0.048 Uiso 1 1 calc R . . . . C12 C 1.1823(4) 0.2522(4) 1.0115(3) 0.0351(15) Uani 1 1 d . . . . . H12A H 1.1397 0.2254 1.0374 0.042 Uiso 1 1 calc R . . . . H12B H 1.2438 0.2683 1.0476 0.042 Uiso 1 1 calc R . . . . C13 C 1.1350(4) 0.3346(4) 0.9715(3) 0.0282(13) Uani 1 1 d . . . . . H13A H 1.1792 0.3630 0.9476 0.034 Uiso 1 1 calc R . . . . H13B H 1.1222 0.3773 1.0065 0.034 Uiso 1 1 calc R . . . . C14 C 1.0404(3) 0.3112(3) 0.9148(3) 0.0207(11) Uani 1 1 d . . . . . H14A H 1.0119 0.3653 0.8883 0.025 Uiso 1 1 calc R . . . . H14B H 0.9944 0.2873 0.9391 0.025 Uiso 1 1 calc R . . . . C15 C 0.6189(3) 0.3217(3) 0.7596(3) 0.0198(11) Uani 1 1 d . . . . . C16 C 0.5433(4) 0.2935(3) 0.6970(3) 0.0220(11) Uani 1 1 d . . . . . C17 C 0.4495(3) 0.3104(4) 0.6974(3) 0.0240(12) Uani 1 1 d . . . . . H17 H 0.3987 0.2926 0.6565 0.029 Uiso 1 1 calc R . . . . C18 C 0.4249(3) 0.3518(3) 0.7539(3) 0.0223(11) Uani 1 1 d . . . . . C19 C 0.4998(4) 0.3811(4) 0.8114(3) 0.0246(12) Uani 1 1 d . . . . . H19 H 0.4843 0.4111 0.8497 0.030 Uiso 1 1 calc R . . . . C20 C 0.5972(3) 0.3690(4) 0.8163(3) 0.0208(11) Uani 1 1 d . . . . . C21 C 0.6290(4) 0.2980(5) 0.5989(3) 0.0403(16) Uani 1 1 d . . . . . H21A H 0.6908 0.3053 0.6362 0.060 Uiso 1 1 calc R . . . . H21B H 0.6391 0.2658 0.5577 0.060 Uiso 1 1 calc R . . . . H21C H 0.6014 0.3562 0.5828 0.060 Uiso 1 1 calc R . . . . C22 C 0.5953(4) 0.1495(4) 0.6486(4) 0.0426(17) Uani 1 1 d . . . . . H22A H 0.6560 0.1504 0.6877 0.064 Uiso 1 1 calc R . . . . H22B H 0.5471 0.1156 0.6639 0.064 Uiso 1 1 calc R . . . . H22C H 0.6058 0.1219 0.6056 0.064 Uiso 1 1 calc R . . . . C23 C 0.4642(4) 0.2367(4) 0.5689(3) 0.0362(15) Uani 1 1 d . . . . . H23A H 0.4172 0.2036 0.5862 0.054 Uiso 1 1 calc R . . . . H23B H 0.4388 0.2957 0.5532 0.054 Uiso 1 1 calc R . . . . H23C H 0.4764 0.2053 0.5281 0.054 Uiso 1 1 calc R . . . . C24 C 0.5589(4) 0.2453(4) 0.6303(3) 0.0300(14) Uani 1 1 d . . . . . C25 C 0.3060(4) 0.4014(5) 0.8200(4) 0.0476(19) Uani 1 1 d . . . . . H25A H 0.2371 0.4087 0.8147 0.071 Uiso 1 1 calc R . . . . H25B H 0.3340 0.3600 0.8596 0.071 Uiso 1 1 calc R . . . . H25C H 0.3384 0.4587 0.8310 0.071 Uiso 1 1 calc R . . . . C26 C 0.2729(4) 0.4295(5) 0.6883(4) 0.049(2) Uani 1 1 d . . . . . H26A H 0.2811 0.4067 0.6430 0.073 Uiso 1 1 calc R . . . . H26B H 0.2041 0.4355 0.6836 0.073 Uiso 1 1 calc R . . . . H26C H 0.3041 0.4874 0.6989 0.073 Uiso 1 1 calc R . . . . C27 C 0.2649(4) 0.2771(4) 0.7344(4) 0.0401(17) Uani 1 1 d . . . . . H27A H 0.2719 0.2520 0.6895 0.060 Uiso 1 1 calc R . . . . H27B H 0.2916 0.2361 0.7744 0.060 Uiso 1 1 calc R . . . . H27C H 0.1965 0.2870 0.7293 0.060 Uiso 1 1 calc R . . . . C28 C 0.3191(4) 0.3653(4) 0.7501(3) 0.0291(13) Uani 1 1 d . . . . . C29 C 0.6330(6) 0.4911(7) 0.9090(7) 0.132(6) Uani 1 1 d . . . . . H29A H 0.5672 0.4819 0.9117 0.198 Uiso 1 1 calc R . . . . H29B H 0.6746 0.5090 0.9566 0.198 Uiso 1 1 calc R . . . . H29C H 0.6327 0.5376 0.8736 0.198 Uiso 1 1 calc R . . . . C30 C 0.6785(8) 0.3384(7) 0.9468(4) 0.095(4) Uani 1 1 d . . . . . H30A H 0.6140 0.3242 0.9501 0.142 Uiso 1 1 calc R . . . . H30B H 0.7092 0.2845 0.9360 0.142 Uiso 1 1 calc R . . . . H30C H 0.7174 0.3630 0.9929 0.142 Uiso 1 1 calc R . . . . C31 C 0.7706(5) 0.4261(6) 0.8833(4) 0.053(2) Uani 1 1 d . . . . . H31A H 0.7984 0.3728 0.8686 0.079 Uiso 1 1 calc R . . . . H31B H 0.7686 0.4734 0.8482 0.079 Uiso 1 1 calc R . . . . H31C H 0.8105 0.4448 0.9312 0.079 Uiso 1 1 calc R . . . . C32 C 0.6704(4) 0.4066(4) 0.8861(3) 0.0312(14) Uani 1 1 d . . . . . C33 C 0.8795(3) 0.4161(2) 0.5436(4) 0.034(3) Uani 0.576(5) 1 d D . P . . H33 H 0.8807 0.4344 0.5935 0.041 Uiso 0.576(5) 1 calc R . P . . C34 C 0.4616(4) 0.4436(3) 0.36210(19) 0.038(2) Uani 0.751(5) 1 d D . P . . H34 H 0.4094 0.4875 0.3410 0.046 Uiso 0.751(5) 1 calc R . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01133(17) 0.01672(19) 0.0186(2) -0.00122(16) 0.00493(13) -0.00031(13) P1 0.0136(6) 0.0177(6) 0.0197(7) -0.0017(5) 0.0059(5) 0.0009(5) P2 0.0115(6) 0.0213(7) 0.0246(7) 0.0004(6) 0.0057(5) -0.0005(5) Cl1 0.0168(6) 0.0230(6) 0.0385(8) 0.0003(6) 0.0129(5) -0.0016(5) Cl2 0.0214(6) 0.0215(6) 0.0287(7) 0.0043(5) 0.0055(5) 0.0028(5) Cl3 0.186(6) 0.068(3) 0.108(4) -0.034(3) 0.102(4) -0.022(3) Cl4 0.137(4) 0.0377(18) 0.0330(18) 0.0042(14) 0.026(2) 0.029(2) Cl5 0.211(6) 0.067(3) 0.033(2) -0.0068(18) -0.005(3) 0.087(3) Cl6 0.114(3) 0.123(3) 0.0428(17) 0.0100(17) 0.0178(17) -0.086(2) Cl7 0.078(2) 0.086(2) 0.062(2) -0.0233(17) 0.0435(16) -0.0152(16) Cl8 0.095(2) 0.0614(18) 0.076(2) -0.0186(16) 0.0409(18) -0.0403(16) C1 0.019(2) 0.019(2) 0.028(3) 0.004(2) 0.010(2) 0.0036(19) C2 0.017(2) 0.020(2) 0.023(3) 0.000(2) 0.010(2) -0.0019(19) C3 0.020(2) 0.016(2) 0.023(3) -0.003(2) 0.009(2) 0.0026(18) C4 0.019(2) 0.027(3) 0.024(3) -0.007(2) 0.005(2) 0.000(2) C5 0.024(3) 0.025(3) 0.026(3) -0.008(2) 0.004(2) 0.002(2) C6 0.036(3) 0.029(3) 0.019(3) -0.001(2) 0.008(2) 0.009(2) C7 0.028(3) 0.027(3) 0.027(3) -0.002(2) 0.010(2) 0.005(2) C8 0.018(2) 0.027(3) 0.020(3) -0.004(2) 0.010(2) 0.001(2) C9 0.016(2) 0.025(3) 0.022(3) 0.001(2) 0.003(2) 0.0026(19) C10 0.027(3) 0.030(3) 0.029(3) 0.003(3) 0.007(2) 0.012(2) C11 0.024(3) 0.051(4) 0.040(4) 0.010(3) 0.000(3) 0.016(3) C12 0.020(3) 0.051(4) 0.028(3) 0.007(3) -0.004(2) 0.004(2) C13 0.024(3) 0.039(3) 0.018(3) -0.002(2) 0.000(2) -0.002(2) C14 0.017(2) 0.027(3) 0.016(3) 0.001(2) 0.000(2) 0.001(2) C15 0.013(2) 0.025(3) 0.022(3) 0.001(2) 0.006(2) -0.0008(18) C16 0.019(2) 0.022(3) 0.023(3) -0.004(2) 0.002(2) -0.0042(19) C17 0.012(2) 0.030(3) 0.028(3) -0.005(2) 0.002(2) -0.003(2) C18 0.011(2) 0.025(3) 0.031(3) -0.002(2) 0.004(2) 0.0021(19) C19 0.020(3) 0.030(3) 0.026(3) -0.008(2) 0.011(2) 0.004(2) C20 0.014(2) 0.028(3) 0.022(3) 0.000(2) 0.007(2) -0.0009(19) C21 0.035(3) 0.059(4) 0.029(4) -0.017(3) 0.012(3) -0.009(3) C22 0.031(3) 0.042(4) 0.047(4) -0.022(3) -0.001(3) 0.003(3) C23 0.027(3) 0.047(4) 0.029(3) -0.014(3) 0.001(3) -0.001(3) C24 0.018(3) 0.037(3) 0.034(3) -0.016(3) 0.006(2) -0.007(2) C25 0.023(3) 0.067(5) 0.058(5) -0.017(4) 0.020(3) -0.001(3) C26 0.020(3) 0.049(4) 0.078(6) 0.015(4) 0.013(3) 0.005(3) C27 0.020(3) 0.040(4) 0.060(5) 0.000(3) 0.011(3) -0.006(2) C28 0.012(2) 0.037(3) 0.037(4) -0.003(3) 0.007(2) 0.000(2) C29 0.056(5) 0.127(9) 0.162(12) -0.123(9) -0.048(6) 0.042(6) C30 0.105(8) 0.132(9) 0.030(4) 0.010(5) -0.007(5) -0.075(7) C31 0.036(4) 0.085(6) 0.040(4) -0.033(4) 0.016(3) -0.035(4) C32 0.018(3) 0.048(4) 0.025(3) -0.014(3) 0.002(2) 0.003(2) C33 0.055(7) 0.046(6) 0.009(5) 0.000(4) 0.020(5) 0.016(5) C34 0.036(4) 0.039(5) 0.038(5) -0.003(4) 0.009(4) 0.014(4) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 P1 Pd1 Cl1 90.33(5) . . P1 Pd1 Cl2 177.10(5) . . P2 Pd1 P1 83.64(5) . . P2 Pd1 Cl1 173.49(5) . . P2 Pd1 Cl2 93.83(5) . . Cl1 Pd1 Cl2 92.13(5) . . C1 P1 Pd1 110.07(16) . . C3 P1 Pd1 115.34(17) . . C3 P1 C1 103.6(2) . . C9 P1 Pd1 111.80(17) . . C9 P1 C1 106.2(3) . . C9 P1 C3 109.2(2) . . C2 P2 Pd1 114.88(18) . . C2 P2 C15 111.0(2) . . C15 P2 Pd1 133.96(18) . . Cl3 Cl3 C33 157.8(7) 3_766 . C2 C1 P1 110.9(4) . . C1 C2 P2 119.1(4) . . C4 C3 P1 109.7(3) . . C8 C3 P1 113.7(3) . . C8 C3 C4 111.6(4) . . C5 C4 C3 111.1(4) . . C6 C5 C4 111.6(5) . . C7 C6 C5 110.5(5) . . C6 C7 C8 111.4(4) . . C3 C8 C7 110.7(4) . . C10 C9 P1 113.3(4) . . C14 C9 P1 109.7(3) . . C14 C9 C10 110.9(4) . . C11 C10 C9 110.7(5) . . C12 C11 C10 110.9(5) . . C13 C12 C11 110.0(5) . . C12 C13 C14 110.7(5) . . C13 C14 C9 111.1(4) . . C16 C15 P2 119.8(4) . . C20 C15 P2 119.0(4) . . C20 C15 C16 120.8(4) . . C15 C16 C24 125.2(5) . . C17 C16 C15 116.7(5) . . C17 C16 C24 118.2(4) . . C16 C17 C18 124.3(5) . . C17 C18 C28 120.3(5) . . C19 C18 C17 117.0(5) . . C19 C18 C28 122.6(5) . . C18 C19 C20 123.6(5) . . C15 C20 C32 127.1(4) . . C19 C20 C15 117.4(5) . . C19 C20 C32 115.4(5) . . C21 C24 C16 110.8(5) . . C21 C24 C22 110.6(5) . . C22 C24 C16 111.9(5) . . C23 C24 C16 111.6(5) . . C23 C24 C21 106.4(5) . . C23 C24 C22 105.4(5) . . C18 C28 C26 109.1(5) . . C18 C28 C27 110.1(5) . . C25 C28 C18 112.9(5) . . C25 C28 C26 109.0(6) . . C25 C28 C27 107.4(5) . . C27 C28 C26 108.3(5) . . C29 C32 C20 110.5(5) . . C29 C32 C30 107.5(9) . . C30 C32 C20 107.2(5) . . C31 C32 C20 117.5(5) . . C31 C32 C29 106.3(7) . . C31 C32 C30 107.4(6) . . Cl4 C33 Cl3 113.0(4) . . Cl4 C33 Cl5 109.6(3) . . Cl5 C33 Cl3 109.0(5) . . Cl6 C34 Cl7 110.0(3) . . Cl6 C34 Cl8 110.4(3) . . Cl8 C34 Cl7 112.3(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 P1 2.2559(13) . Pd1 P2 2.2194(14) . Pd1 Cl1 2.3485(13) . Pd1 Cl2 2.3748(13) . P1 C1 1.863(5) . P1 C3 1.832(5) . P1 C9 1.832(5) . P2 C2 1.649(5) . P2 C15 1.825(5) . Cl3 Cl3 1.611(9) 3_766 Cl3 C33 1.732(3) . Cl4 C33 1.732(3) . Cl5 C33 1.732(3) . Cl6 C34 1.732(2) . Cl7 C34 1.733(2) . Cl8 C34 1.732(2) . C1 C2 1.495(6) . C3 C4 1.538(7) . C3 C8 1.531(7) . C4 C5 1.529(7) . C5 C6 1.523(8) . C6 C7 1.522(7) . C7 C8 1.543(7) . C9 C10 1.539(7) . C9 C14 1.537(7) . C10 C11 1.532(8) . C11 C12 1.531(9) . C12 C13 1.522(8) . C13 C14 1.528(7) . C15 C16 1.442(7) . C15 C20 1.419(8) . C16 C17 1.387(7) . C16 C24 1.554(8) . C17 C18 1.391(8) . C18 C19 1.382(7) . C18 C28 1.528(7) . C19 C20 1.400(7) . C20 C32 1.563(7) . C21 C24 1.548(9) . C22 C24 1.549(9) . C23 C24 1.537(7) . C25 C28 1.521(9) . C26 C28 1.535(9) . C27 C28 1.533(8) . C29 C32 1.505(10) . C30 C32 1.541(11) . C31 C32 1.501(8) .