#------------------------------------------------------------------------------ #$Date: 2024-10-25 03:58:07 +0300 (Fri, 25 Oct 2024) $ #$Revision: 295619 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572945.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_1572945 loop_ _publ_author_name 'Li, Yongqing' 'Cao, Gui-Ping' 'Cao, Yucai' _publ_section_title ; Enhanced mechanical properties of acrylate and 5-vinyl-2-norbornene based ethylene terpolymers: rational design and synthesis using remotely modulated phosphine-sulfonate palladium complexes ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/D4PY00722K _journal_year 2024 _chemical_formula_sum 'C33 H32 N O5 P Pd S' _chemical_formula_weight 692.02 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-12-20 deposited with the CCDC. 2024-10-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.0896(6) _cell_length_b 12.0006(7) _cell_length_c 22.7952(13) _cell_measurement_reflns_used 9784 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 53.91 _cell_measurement_theta_min 3.62 _cell_volume 3033.6(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_Laue_measured_fraction_full 0.964 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 23824 _diffrn_reflns_point_group_measured_fraction_full 0.926 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_theta_full 52.094 _diffrn_reflns_theta_max 52.094 _diffrn_reflns_theta_min 3.621 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.324 _exptl_absorpt_correction_T_max 0.649 _exptl_absorpt_correction_T_min 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_meas 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1416 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_transmission_factor_max 0.649 _exptl_transmission_factor_min 0.458 _refine_diff_density_max 0.518 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.875(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 384 _refine_ls_number_reflns 4771 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0215 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+3.4327P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0568 _reflns_Friedel_coverage 0.694 _reflns_Friedel_fraction_full 0.876 _reflns_Friedel_fraction_max 0.876 _reflns_number_gt 4764 _reflns_number_total 4771 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4py00722k2.cif _cod_data_source_block 1 _cod_database_code 1572945 _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_res_file ; TITL 1 in P2(1)2(1)2(1) New: P212121 1.res created by SHELXL-2018/3 at 15:26:45 on 18-Dec-2023 CELL 1.34139 11.0896 12.0006 22.7952 90.000 90.000 90.000 ZERR 4 0.0006 0.0007 0.0013 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O P Pd S UNIT 132 128 4 20 4 4 4 L.S. 5 ACTA BOND $H FMAP 2 OMIT 6 8 0 OMIT 8 4 0 PLAN 1 CONF TWIN WGHT 0.000000 3.432700 BASF 0.87496 FVAR 0.17865 RESI 0 TEMP -80 PD1 6 0.039895 0.926897 0.579572 11.00000 0.02070 0.01706 = 0.01669 0.00164 -0.00065 -0.00134 S1 7 0.220248 1.052541 0.499145 11.00000 0.03110 0.02230 = 0.01587 0.00172 0.00179 -0.00335 P1 5 0.200470 0.946739 0.637857 11.00000 0.01997 0.01867 = 0.01512 0.00243 0.00034 0.00074 O1 4 -0.154425 0.918863 0.734909 11.00000 0.02979 0.04195 = 0.03842 0.00780 0.00111 -0.00699 O2 4 0.088895 1.205179 0.664230 11.00000 0.03284 0.02657 = 0.03504 0.01269 0.00007 0.00067 O3 4 0.260172 0.939743 0.488560 11.00000 0.04920 0.02671 = 0.03234 -0.00824 0.00498 0.00410 O4 4 0.237591 1.128850 0.451100 11.00000 0.04241 0.03876 = 0.02069 0.00980 0.00007 -0.01047 O5 4 0.094426 1.058288 0.520576 11.00000 0.02818 0.02693 = 0.02260 0.00710 -0.00135 -0.00541 N1 3 -0.119899 0.913925 0.528938 11.00000 0.03482 0.02262 = 0.02213 -0.00007 -0.00072 -0.00186 C1 1 0.299088 1.064159 0.616399 11.00000 0.02013 0.02095 = 0.02097 0.00058 0.00029 0.00289 C2 1 0.368796 1.115559 0.659297 11.00000 0.02150 0.02781 = 0.02436 -0.00016 -0.00061 0.00090 AFIX 43 H2 2 0.362836 1.089487 0.698540 11.00000 -1.20000 AFIX 0 C3 1 0.447044 1.203635 0.647315 11.00000 0.01950 0.02641 = 0.03686 -0.00606 -0.00074 -0.00172 C4 1 0.457223 1.239245 0.589638 11.00000 0.02553 0.02781 = 0.03951 -0.00053 0.00335 -0.00874 AFIX 43 H4 2 0.511699 1.297553 0.580035 11.00000 -1.20000 AFIX 0 C5 1 0.388401 1.190269 0.545945 11.00000 0.02427 0.02879 = 0.02776 0.00403 0.00575 -0.00240 AFIX 43 H5 2 0.395836 1.215769 0.506658 11.00000 -1.20000 AFIX 0 C6 1 0.308523 1.104219 0.558833 11.00000 0.02261 0.02048 = 0.02045 0.00071 0.00301 0.00084 C7 1 0.170292 0.971230 0.715822 11.00000 0.02075 0.01881 = 0.01643 0.00438 0.00099 -0.00132 C8 1 0.257370 0.940831 0.756920 11.00000 0.02314 0.02898 = 0.02259 0.00465 -0.00128 0.00539 AFIX 43 H8 2 0.328550 0.904404 0.743883 11.00000 -1.20000 AFIX 0 C9 1 0.064767 1.024473 0.735577 11.00000 0.02399 0.01573 = 0.01938 0.00421 -0.00055 0.00017 C10 1 0.052262 1.043790 0.795866 11.00000 0.03214 0.02490 = 0.02245 -0.00167 0.00189 0.00452 AFIX 43 H10 2 -0.019297 1.078238 0.809867 11.00000 -1.20000 AFIX 0 C11 1 0.140461 1.014406 0.835486 11.00000 0.04182 0.03021 = 0.01691 -0.00113 -0.00190 0.00380 AFIX 43 H11 2 0.130348 1.030188 0.876027 11.00000 -1.20000 AFIX 0 C12 1 -0.035233 1.062271 0.697134 11.00000 0.02315 0.02563 = 0.02101 -0.00183 0.00035 0.00727 C13 1 -0.022418 1.158250 0.662616 11.00000 0.03080 0.02668 = 0.02002 0.00125 0.00142 0.01118 C14 1 -0.118519 1.198697 0.629894 11.00000 0.03892 0.03941 = 0.02610 0.00592 0.00073 0.01816 AFIX 43 H14 2 -0.109236 1.263804 0.606621 11.00000 -1.20000 AFIX 0 C15 1 -0.147204 1.009517 0.698774 11.00000 0.02788 0.03138 = 0.02485 0.00125 0.00202 0.00467 C16 1 -0.243990 1.048829 0.665078 11.00000 0.01982 0.05647 = 0.03910 -0.00568 -0.00267 0.00478 AFIX 43 H16 2 -0.319337 1.011165 0.665327 11.00000 -1.20000 AFIX 0 C17 1 -0.258471 0.850383 0.731594 11.00000 0.03778 0.05732 = 0.06413 0.00707 0.00590 -0.01897 AFIX 137 H17A 2 -0.329220 0.892972 0.744279 11.00000 -1.50000 H17B 2 -0.248079 0.785446 0.757168 11.00000 -1.50000 H17C 2 -0.269991 0.825422 0.691046 11.00000 -1.50000 AFIX 0 C18 1 -0.014059 0.795642 0.630320 11.00000 0.02565 0.02424 = 0.02412 0.00513 0.00023 -0.00719 AFIX 137 H18A 2 -0.101479 0.785913 0.626669 11.00000 -1.50000 H18B 2 0.006546 0.810394 0.671399 11.00000 -1.50000 H18C 2 0.026885 0.727682 0.617226 11.00000 -1.50000 AFIX 0 C19 1 0.303661 0.827649 0.638363 11.00000 0.02695 0.02551 = 0.02073 -0.00149 -0.00431 0.00708 C20 1 0.412231 0.828966 0.607781 11.00000 0.03177 0.04215 = 0.03131 0.00263 0.00358 0.00983 AFIX 43 H20 2 0.437445 0.894697 0.588060 11.00000 -1.20000 AFIX 0 C21 1 0.483537 0.734106 0.606157 11.00000 0.04262 0.06196 = 0.04607 -0.00125 0.00649 0.02717 AFIX 43 H21 2 0.557783 0.735392 0.585379 11.00000 -1.20000 AFIX 0 C22 1 0.447813 0.637630 0.634441 11.00000 0.06104 0.04890 = 0.05432 -0.00105 -0.00340 0.03217 AFIX 43 H22 2 0.496434 0.572582 0.632280 11.00000 -1.20000 AFIX 0 C23 1 0.269354 0.730061 0.667851 11.00000 0.03821 0.02770 = 0.04148 0.00550 -0.00477 0.00553 AFIX 43 H23 2 0.196103 0.728254 0.689438 11.00000 -1.20000 AFIX 0 C24 1 0.243111 0.962155 0.816032 11.00000 0.02772 0.03718 = 0.01873 0.00666 -0.00589 -0.00031 AFIX 43 H24 2 0.303997 0.940792 0.843105 11.00000 -1.20000 AFIX 0 C25 1 0.111743 1.295689 0.625017 11.00000 0.05714 0.02726 = 0.04301 0.01732 0.00974 0.00623 AFIX 137 H25A 2 0.091263 1.273219 0.584904 11.00000 -1.50000 H25B 2 0.197249 1.316005 0.626890 11.00000 -1.50000 H25C 2 0.062383 1.359900 0.636372 11.00000 -1.50000 AFIX 0 C26 1 -0.169001 1.012012 0.512179 11.00000 0.04140 0.02124 = 0.03440 0.00074 -0.00773 -0.00041 AFIX 43 H26 2 -0.124395 1.078547 0.518426 11.00000 -1.20000 AFIX 0 C27 1 -0.280544 1.019356 0.486537 11.00000 0.05469 0.03236 = 0.05165 0.00298 -0.02140 0.00645 AFIX 43 H27 2 -0.313038 1.089973 0.476297 11.00000 -1.20000 AFIX 0 C28 1 -0.345223 0.923261 0.475728 11.00000 0.03950 0.05549 = 0.05368 -0.00044 -0.02564 0.00019 AFIX 43 H28 2 -0.423388 0.926571 0.458763 11.00000 -1.20000 AFIX 0 C29 1 -0.293900 0.822762 0.490079 11.00000 0.03697 0.03985 = 0.03983 -0.00440 -0.00953 -0.01212 AFIX 43 H29 2 -0.334391 0.755000 0.481349 11.00000 -1.20000 AFIX 0 C30 1 -0.183416 0.821386 0.517183 11.00000 0.03411 0.02471 = 0.02820 -0.00276 -0.00199 -0.00672 AFIX 43 H30 2 -0.150240 0.751450 0.528172 11.00000 -1.20000 AFIX 0 C31 1 0.342302 0.636079 0.665538 11.00000 0.06054 0.02952 = 0.05659 0.00696 -0.00941 0.01429 AFIX 43 H31 2 0.318775 0.570279 0.685685 11.00000 -1.20000 AFIX 0 C32 1 0.516518 1.258614 0.695910 11.00000 0.02494 0.04520 = 0.04210 -0.01362 0.00015 -0.00819 AFIX 137 H32A 2 0.602557 1.242037 0.691426 11.00000 -1.50000 H32B 2 0.488212 1.230273 0.733805 11.00000 -1.50000 H32C 2 0.504115 1.339403 0.694205 11.00000 -1.50000 AFIX 0 C33 1 -0.227589 1.143525 0.631472 11.00000 0.03112 0.05168 = 0.03113 -0.00058 -0.00582 0.02196 AFIX 43 H33 2 -0.293052 1.171282 0.608909 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)2(1)2(1) New: P212121 REM wR2 = 0.0568, GooF = S = 1.093, Restrained GooF = 1.093 for all data REM R1 = 0.0215 for 4764 Fo > 4sig(Fo) and 0.0215 for all 4771 data REM 384 parameters refined using 0 restraints END WGHT 0.0000 3.2614 REM Highest difference peak 0.518, deepest hole -0.507, 1-sigma level 0.056 Q1 1 0.0445 0.9254 0.5274 11.00000 0.05 0.52 ; _shelx_res_checksum 69739 _shelx_hkl_file ; -1 0 0 0.24 0.03 2 0 0 98.08 5.54 3 0 0 0.18 0.06 -3 0 0 0.26 0.06 -5 0 0 0.94 0.15 -5 0 0 1.19 0.14 -6 0 0 17.34 1.04 -6 0 0 18.01 1.03 6 0 0 17.25 1.03 -7 0 0 0.09 0.10 -7 0 0 0.15 0.11 -8 0 0 26.03 1.51 -8 0 0 26.25 1.53 -8 0 0 23.22 1.47 -9 0 0 4.96 0.43 -10 0 0 81.24 4.70 -10 0 0 83.14 4.73 -10 0 0 82.76 4.76 -11 0 0 0.24 0.19 -11 0 0 0.14 0.18 -12 0 0 150.46 8.77 -12 0 0 151.95 8.82 -12 0 0 162.08 8.76 -13 0 0 -0.05 0.19 -13 0 0 0.01 0.25 -13 0 0 0.06 0.22 0 -1 0 0.22 0.04 -2 1 0 4.21 0.26 -2 -1 0 4.12 0.27 -3 1 0 26.53 1.57 -3 -1 0 28.17 1.58 3 1 0 29.90 1.59 -3 -1 0 27.83 1.58 3 -1 0 26.54 1.58 -4 1 0 41.94 2.55 -4 -1 0 44.87 2.57 4 -1 0 48.43 2.57 -4 1 0 43.50 2.57 -4 1 0 49.43 2.57 -4 -1 0 48.63 2.56 4 1 0 41.82 2.58 -6 -1 0 102.56 5.53 -6 -1 0 100.83 5.54 -6 1 0 89.15 5.54 6 1 0 105.92 5.54 6 -1 0 99.39 5.51 -6 1 0 101.40 5.54 -6 1 0 97.18 5.52 -6 -1 0 91.14 5.54 -7 -1 0 134.86 7.34 -7 1 0 128.68 7.34 7 -1 0 126.44 7.27 -7 1 0 125.09 7.30 -7 -1 0 132.01 7.33 -7 1 0 136.39 7.33 7 1 0 123.53 7.30 -7 -1 0 135.42 7.31 -8 -1 0 96.34 5.50 -8 1 0 94.47 5.49 -8 1 0 94.89 5.52 -8 1 0 99.80 5.54 -8 -1 0 102.99 5.54 8 1 0 94.29 5.46 -8 -1 0 98.98 5.52 -9 1 0 5.66 0.49 -9 -1 0 5.43 0.44 -9 1 0 6.16 0.46 -9 1 0 5.94 0.51 -9 -1 0 6.18 0.51 -10 -1 0 18.97 1.17 -10 1 0 17.81 1.20 -10 1 0 18.77 1.24 -10 -1 0 18.26 1.20 -10 -1 0 18.96 1.23 -10 1 0 19.61 1.18 -11 -1 0 56.10 3.33 -11 1 0 55.80 3.27 -11 -1 0 56.74 3.26 -11 1 0 58.11 3.30 -11 -1 0 54.39 3.29 -11 1 0 56.20 3.34 -12 1 0 0.28 0.22 -12 -1 0 0.50 0.23 -12 1 0 0.46 0.23 -12 -1 0 0.41 0.21 -12 1 0 0.47 0.24 -12 -1 0 0.41 0.21 -13 -1 0 16.20 1.12 -13 -1 0 15.08 1.08 -13 -1 0 16.89 1.06 -13 1 0 15.95 1.07 -13 1 0 16.23 1.15 -3 -2 0 33.27 1.90 -3 -2 0 34.70 1.91 -3 2 0 32.23 1.89 -3 2 0 33.36 1.90 3 2 0 31.38 1.92 -3 2 0 35.73 1.90 -3 -2 0 34.15 1.91 -4 -2 0 75.73 4.28 4 -2 0 73.68 4.28 -4 2 0 70.61 4.27 -4 -2 0 74.91 4.29 -4 2 0 84.19 4.29 -4 -2 0 74.77 4.30 4 2 0 74.18 4.30 -4 2 0 82.36 4.29 -5 -2 0 34.19 1.87 5 -2 0 29.77 1.84 -5 -2 0 29.53 1.86 -5 -2 0 33.18 1.85 -5 2 0 34.01 1.86 -5 2 0 35.19 1.87 -5 2 0 31.87 1.84 5 2 0 31.23 1.87 6 2 0 0.55 0.12 -6 2 0 0.74 0.14 6 -2 0 0.77 0.11 -7 2 0 33.82 1.95 -7 2 0 34.13 1.98 7 2 0 33.64 1.96 -8 -2 0 54.75 3.19 -8 2 0 54.39 3.15 -8 2 0 57.73 3.20 -8 2 0 55.03 3.17 8 2 0 54.39 3.12 -8 -2 0 52.02 3.14 -8 -2 0 56.50 3.17 -9 2 0 159.24 8.69 -9 2 0 165.28 8.75 -9 -2 0 153.93 8.68 -9 2 0 152.05 8.71 -9 -2 0 144.29 8.71 -9 -2 0 151.07 8.70 -10 -2 0 102.60 5.58 -10 -2 0 95.76 5.62 -10 -2 0 91.91 5.59 -10 2 0 94.88 5.60 -10 2 0 101.35 5.65 -10 2 0 101.93 5.59 -11 2 0 34.18 2.00 -11 -2 0 34.54 1.99 -11 2 0 32.04 2.01 -11 2 0 32.99 2.07 -11 -2 0 34.42 2.05 -11 -2 0 30.42 2.00 -12 2 0 41.91 2.62 -12 -2 0 43.50 2.66 -12 2 0 43.98 2.62 -12 -2 0 46.42 2.61 -12 -2 0 45.66 2.63 -12 2 0 43.37 2.69 0 -3 0 0.58 0.11 0 -3 0 0.57 0.11 0 3 0 0.42 0.09 -2 -3 0 101.18 5.74 2 3 0 96.65 5.76 -2 3 0 100.58 5.74 -2 3 0 104.58 5.73 -2 -3 0 99.80 5.77 -2 -3 0 107.87 5.75 2 3 0 107.86 5.76 -3 3 0 38.99 2.33 3 3 0 42.53 2.35 -3 3 0 41.17 2.32 -3 3 0 41.42 2.34 -3 -3 0 42.30 2.34 3 3 0 40.56 2.36 4 3 0 117.44 6.81 -4 3 0 120.01 6.78 -4 -3 0 115.26 6.78 -4 -3 0 119.59 6.78 -4 3 0 117.42 6.77 -4 3 0 124.38 6.79 -4 -3 0 133.68 6.81 5 -3 0 121.64 6.64 -5 -3 0 108.66 6.65 -5 -3 0 118.54 6.65 -5 3 0 119.58 6.66 5 3 0 116.91 6.67 -5 3 0 126.14 6.66 -5 3 0 118.40 6.64 -7 3 0 30.71 1.87 -7 -3 0 32.57 1.89 -7 3 0 35.51 1.92 7 3 0 30.53 1.88 -7 3 0 31.50 1.88 -8 -3 0 265.43 14.64 8 3 0 275.36 14.64 -8 -3 0 262.86 14.68 -8 3 0 269.32 14.65 -8 -3 0 250.12 14.65 -8 3 0 243.93 14.65 -8 3 0 264.61 14.69 -9 3 0 10.95 0.78 -9 3 0 10.09 0.71 -9 -3 0 10.41 0.76 -9 3 0 10.74 0.73 -9 -3 0 9.24 0.70 -9 -3 0 9.65 0.69 -10 -3 0 53.05 3.23 -10 3 0 53.73 3.19 -10 3 0 56.53 3.21 -10 3 0 56.28 3.27 -11 -3 0 11.31 0.88 -11 -3 0 11.60 0.83 -11 -3 0 11.61 0.81 -11 3 0 12.64 0.86 -11 3 0 11.16 0.90 -11 3 0 11.83 0.83 -12 3 0 51.65 2.94 -12 -3 0 48.70 2.93 -12 -3 0 50.59 2.98 -12 -3 0 53.03 2.92 -12 3 0 46.06 2.93 -12 3 0 48.73 3.01 0 -4 0 32.08 1.91 0 -4 0 32.36 1.93 0 4 0 35.29 1.91 0 -4 0 33.47 1.91 0 4 0 34.72 1.92 0 4 0 33.24 1.91 1 4 0 241.06 13.67 -2 4 0 4.70 0.31 -2 4 0 4.91 0.31 -2 -4 0 4.16 0.32 -2 4 0 4.53 0.32 2 4 0 4.16 0.34 2 4 0 4.64 0.33 2 -4 0 5.19 0.32 -2 -4 0 4.09 0.34 -2 -4 0 4.52 0.28 2 -4 0 4.56 0.33 -2 -4 0 4.95 0.32 -2 -4 0 4.18 0.34 -3 -4 0 19.88 1.14 -3 -4 0 19.39 1.14 -3 -4 0 21.08 1.17 -3 4 0 18.42 1.12 -3 -4 0 18.36 1.11 -3 -4 0 18.75 1.17 -3 4 0 19.22 1.13 3 4 0 21.18 1.16 -3 -4 0 19.32 1.12 3 4 0 18.18 1.16 3 -4 0 19.63 1.15 -3 4 0 19.42 1.14 -4 4 0 0.58 0.12 -4 -4 0 0.70 0.14 4 4 0 0.48 0.13 -4 -4 0 0.48 0.11 -4 4 0 0.86 0.13 4 -4 0 0.77 0.13 -4 4 0 0.73 0.16 -5 4 0 124.17 7.20 -5 -4 0 124.87 7.23 -5 4 0 129.14 7.21 5 -4 0 137.91 7.21 -5 -4 0 132.61 7.22 5 4 0 122.17 7.23 -5 4 0 128.04 7.23 -6 4 0 0.16 0.13 -6 4 0 0.26 0.12 6 -4 0 0.24 0.09 -8 -4 0 14.14 0.93 -8 -4 0 14.90 0.98 -9 4 0 73.48 4.19 -9 -4 0 70.95 4.17 9 4 0 65.92 4.12 -9 4 0 75.70 4.18 -9 4 0 74.25 4.24 -9 -4 0 78.05 4.23 -9 -4 0 70.63 4.16 -10 -4 0 8.67 0.67 -10 -4 0 8.10 0.68 -10 -4 0 9.58 0.76 -10 4 0 9.99 0.72 -10 4 0 10.38 0.73 -10 4 0 10.45 0.79 -11 -4 0 15.52 1.02 -11 4 0 15.15 1.12 -11 4 0 16.31 1.06 -11 -4 0 16.03 1.05 -11 4 0 14.58 1.05 -11 -4 0 15.79 1.09 -12 4 0 7.48 0.72 -12 -4 0 8.87 0.73 -12 4 0 7.92 0.76 -12 -4 0 9.11 0.65 -12 -4 0 8.35 0.67 -12 4 0 9.29 0.69 0 -5 0 0.10 0.09 0 5 0 0.27 0.09 0 -5 0 0.16 0.10 0 -5 0 0.13 0.08 0 5 0 0.23 0.09 0 5 0 0.13 0.09 -1 -5 0 117.86 6.89 1 -5 0 134.79 6.91 1 5 0 121.42 6.90 1 5 0 120.48 6.88 -1 5 0 123.56 6.89 -1 -5 0 120.71 6.91 -1 -5 0 113.19 6.92 1 -5 0 118.64 6.91 -1 -5 0 114.77 6.89 1 -5 0 131.42 6.90 -1 5 0 135.57 6.91 2 5 0 68.04 4.05 -2 5 0 69.12 4.01 -2 -5 0 66.35 4.04 -2 -5 0 71.75 4.03 -2 5 0 73.17 4.02 2 5 0 69.21 4.03 2 5 0 75.02 4.01 -2 -5 0 68.97 4.05 2 -5 0 78.05 4.02 -2 5 0 72.74 4.03 -2 -5 0 73.60 4.02 -2 -5 0 69.90 3.99 2 -5 0 69.91 4.04 -3 -5 0 36.45 2.07 -3 -5 0 36.05 2.11 -3 -5 0 35.70 2.08 -3 -5 0 35.65 2.10 -3 5 0 35.92 2.09 -3 -5 0 39.06 2.14 3 5 0 38.06 2.13 3 -5 0 35.82 2.12 3 -5 0 38.50 2.09 -3 5 0 35.20 2.10 -3 5 0 35.84 2.11 -3 -5 0 35.73 2.14 3 5 0 38.11 2.14 4 5 0 55.56 3.36 -4 -5 0 54.15 3.34 -4 -5 0 63.03 3.38 -4 5 0 59.30 3.34 -4 5 0 59.16 3.36 4 -5 0 64.11 3.36 -4 -5 0 56.88 3.35 4 5 0 58.78 3.39 -4 5 0 59.17 3.35 5 -5 0 184.40 9.41 -5 5 0 157.67 9.39 -5 -5 0 160.75 9.41 5 5 0 154.50 9.44 -5 -5 0 174.33 9.44 -5 5 0 163.33 9.41 -5 5 0 169.96 9.43 -5 -5 0 177.31 9.41 -6 -5 0 242.19 14.10 -6 5 0 257.05 14.08 -6 -5 0 246.42 14.08 6 -5 0 258.08 14.05 -6 5 0 249.41 14.07 -6 5 0 248.36 14.11 -6 -5 0 259.49 14.08 -7 5 0 109.62 6.29 -7 5 0 110.07 6.34 -7 5 0 108.61 6.30 -7 -5 0 101.78 6.29 7 5 0 107.25 6.31 -7 -5 0 124.67 6.31 -7 -5 0 117.29 6.34 -8 5 0 222.20 12.09 -8 5 0 219.04 12.08 8 5 0 210.83 12.08 -8 -5 0 223.99 12.09 -8 5 0 215.11 12.13 -8 -5 0 211.11 12.07 -8 -5 0 203.38 12.11 -9 -5 0 41.36 2.67 -9 5 0 46.74 2.69 -9 5 0 48.28 2.69 9 5 0 45.52 2.64 -9 -5 0 43.93 2.67 -9 5 0 48.11 2.76 -9 -5 0 45.49 2.73 -11 5 0 32.71 2.11 -11 5 0 37.12 2.06 -11 5 0 33.84 2.05 -11 -5 0 30.87 2.02 -11 -5 0 31.86 2.07 -11 -5 0 34.92 2.02 -12 5 0 25.97 1.64 -12 -5 0 27.02 1.63 -12 -5 0 27.60 1.62 -12 -5 0 27.61 1.69 -12 5 0 23.01 1.68 1 6 0 7.83 0.58 1 -6 0 8.79 0.55 1 6 0 8.36 0.54 -1 -6 0 8.19 0.56 -1 6 0 9.26 0.58 1 6 0 8.34 0.56 -1 6 0 9.00 0.55 -1 -6 0 7.48 0.58 1 -6 0 8.61 0.58 -1 -6 0 8.23 0.58 1 -6 0 8.79 0.56 -1 6 0 9.00 0.55 -1 -6 0 7.44 0.54 2 -6 0 324.83 18.12 -3 -6 0 52.49 3.05 -3 6 0 53.57 3.09 -3 -6 0 50.40 3.11 3 6 0 54.38 3.10 -3 -6 0 57.73 3.11 -3 -6 0 53.75 3.08 -3 -6 0 58.21 3.08 -3 6 0 54.08 3.07 3 -6 0 57.81 3.06 -3 6 0 50.62 3.07 3 6 0 52.31 3.12 -3 -6 0 51.33 3.03 4 6 0 161.93 9.83 -4 -6 0 174.29 9.80 -4 6 0 182.86 9.82 4 -6 0 176.77 9.81 4 6 0 180.47 9.82 -4 6 0 172.48 9.79 -4 -6 0 171.46 9.83 -4 6 0 172.55 9.79 -4 -6 0 179.37 9.80 -5 6 0 115.58 6.66 -5 6 0 124.33 6.68 5 6 0 121.55 6.72 -5 -6 0 111.43 6.67 -5 6 0 126.70 6.71 -5 -6 0 116.65 6.68 -5 -6 0 112.13 6.70 -7 -6 0 6.08 0.50 -8 6 0 18.75 1.28 8 6 0 19.52 1.28 -8 6 0 20.40 1.34 -8 6 0 22.79 1.30 -9 6 0 12.19 0.91 -9 6 0 11.86 0.85 -9 -6 0 12.55 0.91 -9 -6 0 11.39 0.83 -10 6 0 56.79 3.22 -10 -6 0 55.24 3.21 -10 6 0 55.73 3.22 -10 -6 0 53.45 3.24 -10 -6 0 50.83 3.17 -10 6 0 55.95 3.28 -11 -6 0 0.96 0.24 -11 -6 0 1.08 0.28 -11 -6 0 1.26 0.28 0 -7 0 0.17 0.15 0 -7 0 0.15 0.12 0 7 0 0.40 0.14 0 7 0 0.13 0.14 0 -7 0 0.19 0.11 0 7 0 0.22 0.13 0 -7 0 0.10 0.11 1 -7 0 302.89 15.81 1 -7 0 295.69 15.80 -1 -7 0 259.09 15.81 -1 -7 0 273.13 15.79 -2 7 0 10.34 0.70 -2 7 0 11.05 0.67 -2 -7 0 10.27 0.62 -2 -7 0 9.63 0.70 2 7 0 9.85 0.65 -2 -7 0 10.66 0.64 -2 -7 0 9.90 0.68 2 7 0 10.34 0.70 -2 -7 0 9.17 0.66 2 -7 0 10.88 0.71 2 -7 0 10.83 0.67 -2 -7 0 10.30 0.72 -3 7 0 33.20 2.01 -3 -7 0 33.87 1.99 3 7 0 34.31 2.05 -3 -7 0 36.09 2.01 -3 -7 0 33.45 2.03 -3 7 0 33.54 1.98 3 -7 0 33.33 2.01 -3 7 0 36.17 2.00 3 7 0 32.90 2.02 3 -7 0 33.76 1.97 -4 7 0 24.07 1.44 4 7 0 23.12 1.50 -4 -7 0 21.75 1.48 -4 -7 0 23.71 1.46 -4 -7 0 24.29 1.45 4 -7 0 25.39 1.47 -4 7 0 24.81 1.45 -4 7 0 25.99 1.49 -6 7 0 8.36 0.64 -6 7 0 7.90 0.60 6 -7 0 7.57 0.48 -6 7 0 8.48 0.59 6 -7 0 8.03 0.54 -7 -7 0 223.01 13.42 7 7 0 243.51 13.42 -7 7 0 244.20 13.39 -7 -7 0 231.84 13.39 -7 7 0 259.25 13.45 -7 7 0 240.18 13.38 -7 -7 0 226.65 13.37 -8 -7 0 5.36 0.52 -8 -7 0 6.85 0.52 -8 7 0 6.23 0.59 -8 -7 0 6.66 0.60 -8 7 0 5.23 0.51 8 7 0 5.64 0.52 -9 7 0 16.29 1.08 -9 -7 0 15.37 1.06 -9 7 0 17.26 1.15 9 7 0 16.08 1.03 -9 -7 0 14.87 1.12 -9 -7 0 15.65 1.05 -9 7 0 16.21 1.08 -10 7 0 1.12 0.28 -10 7 0 1.32 0.30 -11 7 0 31.97 1.91 -11 -7 0 27.45 1.87 -11 7 0 31.57 1.98 -11 -7 0 30.89 1.88 -11 7 0 34.99 1.93 -11 -7 0 29.25 1.94 0 8 0 1000.00 56.25 1 -8 0 358.35 18.59 -1 -8 0 328.49 18.57 -1 -8 0 310.82 18.60 2 -8 0 34.62 1.89 2 8 0 30.91 1.88 2 8 0 29.42 1.92 2 -8 0 31.67 1.94 -2 8 0 34.23 1.94 -2 -8 0 30.78 1.86 2 8 0 32.57 1.96 -2 -8 0 30.64 1.95 -2 -8 0 31.07 1.84 -2 8 0 34.22 1.89 -2 -8 0 31.72 1.89 -2 -8 0 33.32 1.91 -2 -8 0 30.76 1.93 -2 8 0 34.38 1.91 3 8 0 32.36 2.02 -3 -8 0 31.65 2.00 3 -8 0 35.97 1.95 -3 8 0 33.62 2.00 -3 -8 0 33.01 1.97 -3 8 0 32.78 1.97 -3 -8 0 32.64 1.96 -3 8 0 33.33 1.96 3 -8 0 33.49 2.00 3 8 0 34.16 2.01 4 8 0 112.44 6.68 -4 8 0 120.42 6.67 -4 8 0 119.54 6.62 -4 -8 0 110.39 6.66 -4 -8 0 114.41 6.63 4 -8 0 122.11 6.65 -4 8 0 122.50 6.64 -4 -8 0 115.07 6.62 5 -8 0 9.90 0.69 -5 8 0 8.92 0.75 -5 8 0 9.71 0.70 5 -8 0 11.08 0.61 5 8 0 11.01 0.78 -5 8 0 9.40 0.71 -6 -8 0 58.80 3.43 -6 -8 0 57.79 3.38 -7 8 0 6.51 0.58 -7 8 0 5.94 0.62 -7 -8 0 7.76 0.66 7 8 0 6.77 0.61 -7 -8 0 7.97 0.60 -7 -8 0 8.00 0.59 -7 8 0 6.28 0.56 -8 8 0 44.64 2.72 -8 -8 0 47.01 2.78 -8 -8 0 45.75 2.71 -8 8 0 44.84 2.78 8 8 0 45.24 2.73 -8 8 0 48.99 2.74 -8 -8 0 45.42 2.73 -9 8 0 5.88 0.60 -9 8 0 5.88 0.55 -9 -8 0 6.02 0.53 -9 -8 0 5.46 0.51 -9 -8 0 5.44 0.59 -10 8 0 10.73 0.81 0 -9 0 0.38 0.17 0 9 0 0.30 0.18 0 -9 0 0.31 0.19 0 -9 0 0.14 0.20 0 -9 0 0.30 0.20 0 9 0 0.04 0.19 1 -9 0 205.71 12.03 -1 9 0 227.19 12.03 -1 -9 0 198.57 11.98 1 -9 0 226.13 11.99 -1 9 0 231.11 11.98 -1 9 0 204.94 12.05 -1 -9 0 204.65 12.04 1 9 0 210.85 11.97 1 9 0 210.04 12.06 -1 -9 0 212.13 11.94 1 9 0 217.58 12.02 2 9 0 30.57 1.96 -2 9 0 35.01 1.92 -2 -9 0 28.98 1.95 -2 9 0 29.84 1.98 2 9 0 33.43 2.00 2 -9 0 32.61 1.97 2 -9 0 33.40 1.91 -2 -9 0 32.35 1.93 -2 9 0 33.59 1.96 -2 -9 0 30.95 1.90 2 -9 0 34.18 1.85 -3 9 0 4.11 0.38 -3 9 0 3.65 0.36 -3 -9 0 3.46 0.38 3 9 0 3.68 0.44 -3 9 0 3.81 0.42 -3 -9 0 3.13 0.35 -3 -9 0 3.50 0.42 -4 9 0 176.02 9.63 -4 9 0 163.83 9.66 -4 9 0 170.06 9.61 4 9 0 161.41 9.68 4 -9 0 173.76 9.53 -4 -9 0 174.45 9.61 -4 -9 0 174.60 9.63 4 -9 0 170.36 9.63 -4 -9 0 170.76 9.66 5 -9 0 106.37 6.03 5 -9 0 103.47 5.94 -5 9 0 101.42 6.04 -5 -9 0 107.73 6.04 -5 -9 0 101.66 6.05 5 9 0 105.55 6.11 -5 -9 0 116.20 6.11 -5 9 0 105.63 6.05 5 -9 0 105.35 5.95 -5 9 0 108.01 6.10 -6 -9 0 167.62 9.97 -6 -9 0 171.96 10.02 -6 -9 0 171.82 9.96 6 9 0 180.83 10.03 -6 9 0 179.82 9.98 -6 9 0 180.68 9.97 -6 9 0 183.57 10.03 7 9 0 22.82 1.45 -7 9 0 21.06 1.40 -7 9 0 21.35 1.46 -7 -9 0 23.45 1.43 -8 9 0 62.72 3.61 -8 9 0 63.28 3.68 -8 9 0 59.05 3.60 -8 -9 0 61.13 3.59 8 9 0 66.40 3.62 -8 -9 0 60.00 3.66 -8 -9 0 59.45 3.60 -9 -9 0 0.95 0.30 -9 9 0 0.97 0.24 -9 9 0 0.91 0.27 -9 -9 0 1.13 0.28 9 9 0 0.63 0.19 -9 -9 0 0.75 0.22 -10 9 0 38.01 2.30 -10 -9 0 33.44 2.18 -10 9 0 38.68 2.22 -10 -9 0 33.64 2.19 -10 9 0 39.71 2.24 0 -10 0 139.47 7.86 0 -10 0 133.51 7.87 0 10 0 140.67 7.97 0 10 0 150.07 7.92 0 -10 0 133.86 7.98 0 10 0 137.29 8.01 0 -10 0 146.73 7.93 1 10 0 168.15 9.58 1 -10 0 173.70 9.56 1 -10 0 176.26 9.44 -1 10 0 183.63 9.49 -1 10 0 159.66 9.57 1 -10 0 171.46 9.42 -1 10 0 176.13 9.54 1 10 0 150.40 9.52 1 10 0 159.23 9.47 1 -10 0 168.35 9.48 -1 -10 0 165.36 9.50 2 -10 0 53.71 3.07 2 10 0 48.53 3.09 2 -10 0 54.07 2.96 2 10 0 47.69 3.06 -2 10 0 49.56 3.10 -2 10 0 55.27 3.07 -2 10 0 56.51 3.02 2 -10 0 51.37 2.94 -2 -10 0 48.78 3.02 3 -10 0 87.21 4.68 -3 10 0 84.83 4.80 -3 -10 0 73.36 4.72 3 -10 0 88.49 4.67 3 -10 0 88.89 4.80 3 10 0 75.57 4.82 -3 10 0 86.96 4.75 -3 -10 0 77.43 4.75 -4 -10 0 193.94 11.29 4 10 0 200.90 11.39 -4 10 0 206.61 11.31 -4 -10 0 193.18 11.35 -4 10 0 199.38 11.36 -4 -10 0 204.12 11.32 -4 10 0 207.03 11.41 -6 10 0 10.21 0.79 -6 -10 0 9.29 0.73 -6 -10 0 10.04 0.72 6 10 0 9.31 0.78 -6 10 0 8.03 0.71 -6 -10 0 9.99 0.81 -6 10 0 8.45 0.70 7 10 0 7.37 0.66 -8 10 0 6.50 0.60 -8 10 0 5.95 0.66 -8 10 0 7.68 0.63 -8 -10 0 7.30 0.73 8 10 0 6.43 0.58 -8 -10 0 6.83 0.59 -8 -10 0 7.71 0.60 -9 -10 0 51.75 3.12 -9 -10 0 54.12 3.44 9 10 0 47.89 3.07 -9 10 0 58.20 3.15 -9 -10 0 53.67 3.11 -9 10 0 51.53 3.20 -9 10 0 55.06 3.14 0 11 0 0.13 0.22 0 11 0 0.78 0.25 0 11 0 0.28 0.25 0 -11 0 0.37 0.22 -1 11 0 64.81 4.02 -1 11 0 70.36 3.98 -1 -11 0 66.24 3.92 1 11 0 67.28 3.99 1 11 0 69.05 4.03 -1 11 0 69.34 3.91 -2 11 0 25.93 1.57 2 11 0 22.22 1.58 -2 11 0 23.98 1.61 -2 -11 0 23.80 1.51 -3 11 0 57.38 3.48 -3 11 0 56.12 3.35 -3 -11 0 57.53 3.38 -3 11 0 59.44 3.43 3 11 0 57.89 3.46 -4 11 0 155.15 8.65 -4 11 0 158.46 8.58 -4 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15.79 1.00 0 4 -4 17.80 1.01 1 4 -4 354.19 18.62 -1 4 4 302.63 18.53 2 4 -4 2.17 0.23 -2 4 -4 2.11 0.17 2 -4 -4 2.61 0.24 -2 -4 4 2.27 0.22 2 4 4 2.64 0.21 -2 -4 4 2.02 0.20 2 -4 -4 2.61 0.20 -2 4 -4 2.04 0.19 -3 4 4 33.90 2.08 -3 4 4 32.58 2.06 3 4 4 39.01 2.08 3 -4 -4 38.21 2.09 -4 -4 -4 129.78 8.03 -4 4 4 149.34 8.01 -4 4 4 147.35 8.04 4 4 -4 142.63 8.05 -4 -4 -4 149.43 8.01 -4 -4 -4 147.22 8.02 4 4 -4 138.26 8.03 -4 4 4 148.95 8.02 4 4 4 131.49 8.02 -4 -4 4 137.99 8.04 -4 4 -4 141.82 7.99 4 -4 -4 147.64 8.03 -4 -4 4 138.89 8.02 -4 4 -4 145.05 7.98 -4 -4 4 144.14 8.01 -4 4 -4 145.00 7.97 -5 -4 -4 118.43 6.16 -5 4 4 116.45 6.17 5 4 -4 111.69 6.18 -5 -4 -4 108.23 6.17 5 4 -4 112.64 6.20 -5 4 4 116.29 6.18 -5 4 4 116.46 6.21 -5 -4 -4 109.08 6.14 5 4 4 113.57 6.17 -5 4 -4 96.49 6.12 5 -4 -4 103.58 6.17 -5 4 -4 109.11 6.12 -5 -4 4 96.09 6.18 -5 4 -4 107.18 6.14 -5 -4 4 105.08 6.17 -6 4 -4 317.45 16.91 -6 4 -4 289.08 16.91 -7 4 4 216.98 12.63 -7 4 4 197.11 12.56 -7 -4 -4 202.99 12.53 7 4 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1.65 -1 -1 -23 27.20 1.59 1 1 -23 27.03 1.59 1 -1 -23 21.39 1.56 1 -1 -23 21.83 1.62 -1 1 -23 22.02 1.54 2 1 -23 27.67 1.98 2 1 -23 28.00 1.92 -2 -1 -23 29.27 1.92 -2 1 -23 31.51 1.91 2 -1 -23 33.40 2.03 2 -1 -23 34.57 1.98 -3 -1 -23 7.09 0.63 3 1 -23 7.47 0.67 3 1 -23 7.32 0.78 4 1 -23 70.05 4.46 4 1 -23 73.60 4.51 -4 -1 -23 71.79 4.42 -4 1 -23 79.31 4.42 4 -1 -23 81.45 4.54 4 -1 -23 81.72 4.51 -5 -1 -23 77.46 4.09 5 1 -23 74.44 4.18 5 1 -23 73.69 4.16 5 -1 -23 62.79 4.15 5 -1 -23 67.35 4.05 -5 1 -23 65.26 4.04 6 1 -23 39.65 2.59 -6 -1 -23 37.08 2.48 -6 -1 -23 42.98 2.46 -6 1 -23 45.76 2.48 6 -1 -23 45.37 2.63 0 -2 -23 10.71 0.95 0 -2 -23 10.81 0.87 0 2 -23 10.95 0.84 1 2 -23 28.09 1.74 1 -2 -23 21.67 1.67 2 2 -23 117.31 6.74 2 2 -23 116.43 6.79 -2 -2 -23 110.38 6.73 2 -2 -23 117.03 6.77 2 -2 -23 121.54 6.83 -2 2 -23 121.11 6.72 3 2 -23 47.27 2.87 3 2 -23 47.35 2.92 -3 -2 -23 47.21 2.86 3 -2 -23 48.16 2.91 3 -2 -23 47.04 2.94 -3 2 -23 48.22 2.83 4 -2 -23 6.02 0.70 4 -2 -23 6.67 0.68 -4 2 -23 6.22 0.55 4 -2 -23 7.11 0.57 5 2 -23 1.26 0.38 -5 -2 -23 1.87 0.28 -5 -2 -23 1.59 0.33 5 2 -23 1.17 0.32 -6 -2 -23 40.46 2.35 6 2 -23 40.92 2.48 -6 2 -23 37.78 2.34 6 -2 -23 40.47 2.50 0 -3 -23 38.89 2.42 0 3 -23 39.40 2.38 0 -3 -23 38.45 2.47 -1 3 -23 0.72 0.24 1 -3 -23 0.80 0.32 1 -3 -23 0.85 0.30 2 3 -23 52.04 3.20 -2 -3 -23 50.91 3.21 2 3 -23 50.48 3.25 2 -3 -23 53.08 3.29 2 -3 -23 55.24 3.25 2 -3 -23 56.61 3.17 -2 3 -23 57.12 3.19 -3 -3 -23 53.63 3.46 -3 -3 -23 55.75 3.41 3 3 -23 55.28 3.51 3 3 -23 57.47 3.48 3 -3 -23 63.47 3.44 3 -3 -23 63.55 3.58 -3 3 -23 60.98 3.45 3 -3 -23 58.42 3.52 4 3 -23 16.34 1.06 4 -3 -23 12.96 0.96 4 -3 -23 12.66 1.07 5 3 -23 85.97 4.74 5 3 -23 83.70 4.72 -5 -3 -23 79.97 4.66 -5 -3 -23 79.21 4.61 -5 -3 -23 89.18 4.63 -5 3 -23 72.78 4.59 5 -3 -23 72.69 4.74 -6 -3 -23 1.82 0.34 6 3 -23 2.19 0.42 -6 -3 -23 2.08 0.29 6 -3 -23 2.67 0.45 0 4 -23 49.41 2.90 0 -4 -23 44.40 2.93 0 -4 -23 49.85 3.00 0 -4 -23 49.21 2.87 1 4 -23 7.57 0.69 -1 -4 -23 6.93 0.71 -1 4 -23 8.84 0.69 1 -4 -23 8.94 0.82 1 -4 -23 8.46 0.67 1 -4 -23 8.14 0.75 -2 -4 -23 116.52 6.57 2 4 -23 109.85 6.58 -2 -4 -23 117.00 6.50 2 4 -23 115.60 6.55 -2 4 -23 113.46 6.52 2 -4 -23 114.30 6.59 2 -4 -23 113.82 6.50 2 -4 -23 109.17 6.61 -3 -4 -23 37.93 2.40 3 4 -23 39.88 2.40 -3 -4 -23 40.46 2.35 3 4 -23 36.54 2.42 3 -4 -23 43.81 2.37 3 -4 -23 38.31 2.47 -3 4 -23 38.67 2.36 3 -4 -23 36.13 2.43 4 4 -23 19.56 1.34 4 4 -23 21.90 1.38 4 -4 -23 17.73 1.27 -5 -4 -23 17.17 1.11 5 4 -23 16.57 1.21 -5 -4 -23 17.81 1.12 0 -5 -23 36.38 2.31 0 -5 -23 34.92 2.16 0 5 -23 38.15 2.21 0 -5 -23 32.80 2.24 -1 -5 -23 9.22 0.74 -1 -5 -23 9.65 0.82 -1 5 -23 9.56 0.77 1 -5 -23 10.12 0.75 1 -5 -23 10.23 0.86 -2 5 -23 13.69 0.98 2 -5 -23 13.48 0.96 2 -5 -23 14.00 1.10 3 5 -23 25.18 1.57 -3 -5 -23 25.31 1.54 -3 -5 -23 25.22 1.47 3 5 -23 24.14 1.52 3 -5 -23 20.94 1.45 3 -5 -23 20.21 1.56 -3 5 -23 19.76 1.45 4 5 -23 41.66 2.36 -4 -5 -23 37.59 2.25 4 5 -23 36.76 2.31 -4 -5 -23 36.50 2.24 4 -5 -23 35.71 2.37 -4 5 -23 35.94 2.24 0 -6 -23 0.10 0.24 0 -6 -23 0.20 0.34 0 6 -23 0.28 0.20 0 -6 -23 0.33 0.27 1 6 -23 58.94 3.56 -1 -6 -23 57.26 3.60 -1 -6 -23 58.14 3.53 1 -6 -23 56.38 3.61 1 -6 -23 62.25 3.54 1 -6 -23 64.88 3.69 -1 6 -23 63.64 3.57 2 6 -23 36.77 2.40 -2 -6 -23 39.35 2.37 -2 6 -23 40.53 2.40 2 -6 -23 35.33 2.46 2 -6 -23 43.62 2.53 2 -6 -23 40.26 2.37 -3 -6 -23 52.70 3.41 3 6 -23 55.57 3.40 -3 -6 -23 60.58 3.38 3 6 -23 52.93 3.43 -3 -6 -23 58.81 3.36 3 -6 -23 63.04 3.43 3 -6 -23 56.43 3.48 -3 6 -23 58.27 3.38 0 7 -23 0.38 0.21 0 -7 -23 0.25 0.24 0 -7 -23 0.23 0.35 0 7 23 0.39 0.19 -1 -7 -23 27.00 1.80 -1 -7 -23 26.70 1.97 1 7 -23 26.39 1.84 1 -7 -23 33.19 1.98 -1 7 -23 33.06 1.87 1 -7 -23 29.78 1.82 0 0 -24 182.87 10.39 -1 0 -24 2.33 0.39 1 0 -24 2.30 0.44 1 0 -24 3.10 0.43 -2 0 -24 40.25 2.48 2 0 -24 41.94 2.58 2 0 -24 40.56 2.51 3 0 -24 15.38 1.17 -3 0 -24 15.16 1.08 3 0 -24 15.89 1.13 4 0 -24 44.04 2.80 -4 0 -24 48.60 2.73 4 0 -24 43.78 2.79 5 0 -24 39.27 2.34 -5 0 -24 34.66 2.21 0 1 -24 35.92 2.24 0 -1 -24 36.86 2.27 -1 -1 -24 23.77 1.62 1 1 -24 24.16 1.61 1 -1 -24 25.54 1.71 -1 1 -24 25.31 1.61 1 -1 -24 26.07 1.65 2 1 -24 48.91 3.02 -2 -1 -24 52.36 2.97 2 1 -24 50.42 2.96 2 -1 -24 48.94 2.98 2 -1 -24 44.12 3.00 -2 1 -24 49.80 2.93 -3 -1 -24 16.02 1.11 3 1 -24 16.51 1.15 3 1 -24 15.99 1.19 3 -1 -24 14.79 1.18 -3 1 -24 16.30 1.09 3 -1 -24 16.30 1.17 4 1 -24 24.77 1.63 4 1 -24 24.10 1.65 -4 -1 -24 25.02 1.57 4 -1 -24 25.06 1.66 4 -1 -24 24.10 1.65 -4 1 -24 24.62 1.55 -5 -1 -24 47.48 2.79 5 1 -24 42.17 2.85 5 -1 -24 49.26 2.90 -5 1 -24 48.79 2.77 0 -2 -24 32.85 2.18 0 2 -24 36.74 2.16 1 2 -24 43.40 2.88 -1 -2 -24 44.43 2.90 -1 2 -24 52.76 2.90 1 -2 -24 47.69 2.93 1 -2 -24 52.45 3.01 -2 -2 -24 8.82 0.72 -2 2 -24 7.59 0.67 3 2 -24 50.62 3.07 3 2 -24 52.89 3.13 -3 -2 -24 51.85 3.07 3 -2 -24 51.13 3.11 3 -2 -24 50.39 3.14 -3 2 -24 50.18 3.03 4 2 -24 57.64 3.43 4 2 -24 58.24 3.40 -4 -2 -24 58.26 3.31 -4 -2 -24 61.18 3.38 4 -2 -24 52.62 3.41 4 -2 -24 51.96 3.43 -4 2 -24 56.73 3.32 4 -2 -24 57.45 3.32 -5 -2 -24 27.65 1.63 5 2 -24 27.05 1.71 5 -2 -24 22.55 1.70 0 -3 -24 0.22 0.22 0 3 -24 0.39 0.21 1 3 -24 37.55 2.41 -1 -3 -24 34.97 2.42 -1 3 -24 40.58 2.41 1 -3 -24 41.19 2.38 1 -3 -24 44.12 2.54 1 -3 -24 38.16 2.45 -2 -3 -24 15.01 1.14 2 3 -24 15.86 1.22 2 3 -24 15.70 1.13 -2 -3 -24 15.66 1.07 2 -3 -24 16.32 1.19 2 -3 -24 16.38 1.23 2 -3 -24 17.51 1.10 -2 3 -24 16.41 1.11 3 3 -24 23.68 1.65 -3 -3 -24 24.50 1.55 -3 -3 -24 25.50 1.62 3 3 -24 24.72 1.62 3 -3 -24 24.69 1.69 3 -3 -24 25.73 1.56 3 -3 -24 24.32 1.67 -3 3 -24 24.96 1.57 -4 -3 -24 112.66 6.35 -4 -3 -24 119.80 6.42 4 3 -24 111.64 6.42 4 3 -24 112.64 6.46 4 -3 -24 114.59 6.36 -4 3 -24 103.77 6.34 4 -3 -24 104.75 6.47 -5 -3 -24 5.22 0.45 5 3 -24 4.93 0.56 -5 -3 -24 4.29 0.44 0 -4 -24 0.80 0.28 0 -4 -24 1.59 0.49 0 -4 -24 0.82 0.26 0 4 -24 0.81 0.25 -1 -4 -24 71.15 4.10 1 4 -24 68.09 4.13 -1 -4 -24 64.48 4.16 1 -4 -24 72.16 4.10 1 -4 -24 71.93 4.24 1 -4 -24 75.27 4.20 -2 -4 -24 7.73 0.69 2 -4 -24 10.01 0.84 -2 4 -24 9.89 0.75 -3 -4 -24 85.10 4.56 -3 -4 -24 81.95 4.62 3 4 -24 80.80 4.65 3 4 -24 84.94 4.62 3 -4 -24 71.97 4.64 3 -4 -24 76.37 4.54 -3 4 -24 77.18 4.56 3 -4 -24 71.80 4.65 4 4 -24 90.00 5.21 -4 -4 -24 90.25 5.11 -4 -4 -24 92.54 5.17 4 -4 -24 88.74 5.24 -4 4 -24 83.59 5.10 0 -5 -24 39.23 2.51 0 -5 -24 40.55 2.60 0 -5 -24 42.80 2.67 0 5 24 43.80 2.44 0 5 -24 43.35 2.56 -1 -5 -24 13.16 1.02 -1 -5 -24 13.69 0.93 1 5 -24 13.97 0.98 -1 5 -24 12.84 0.95 1 -5 -24 13.15 0.93 1 -5 -24 11.94 1.06 1 -5 -24 12.80 1.04 -2 -5 -24 14.78 1.02 2 -5 -24 12.18 0.91 2 -5 -24 11.76 1.05 -2 5 -24 13.12 0.94 2 -5 -24 13.25 1.06 3 5 -24 33.32 2.20 -3 -5 -24 38.13 2.12 3 5 -24 34.49 2.23 3 -5 -24 35.50 2.24 3 -5 -24 32.38 2.10 -3 5 -24 34.61 2.12 0 6 24 62.72 3.36 0 6 -24 55.46 3.36 0 -6 -24 51.48 3.45 0 -6 -24 57.08 3.34 1 6 -24 8.67 0.69 -1 -6 -24 7.24 0.63 1 -6 -24 7.81 0.80 -1 6 -24 8.17 0.68 1 -6 -24 7.03 0.63 0 0 -25 0.20 0.21 1 0 -25 2.38 0.42 -1 0 -25 2.26 0.40 2 0 -25 6.65 0.64 2 0 -25 6.40 0.72 -2 0 -25 6.58 0.62 3 0 -25 1.90 0.38 -3 0 -25 1.47 0.30 3 0 -25 1.31 0.37 4 0 -25 78.97 4.56 -4 0 -25 75.04 4.46 0 -1 -25 0.90 0.27 0 1 -25 1.05 0.26 1 1 -25 92.39 4.86 -1 -1 -25 85.84 4.86 -1 1 -25 78.63 4.82 1 -1 -25 75.11 4.84 2 1 -25 27.05 1.82 -2 -1 -25 26.50 1.81 2 1 -25 27.47 1.89 -2 1 -25 29.38 1.81 2 -1 -25 30.72 1.92 2 -1 -25 30.31 1.86 3 1 -25 77.18 4.58 3 1 -25 73.05 4.61 -3 -1 -25 77.93 4.56 3 -1 -25 83.07 4.66 -3 1 -25 80.93 4.55 3 -1 -25 77.22 4.60 4 1 -25 2.42 0.47 4 -1 -25 2.00 0.35 4 -1 -25 1.56 0.36 -4 1 -25 1.89 0.35 0 -2 -25 2.75 0.46 0 2 -25 2.96 0.42 -1 -2 -25 10.40 0.86 1 -2 -25 11.15 0.98 1 -2 -25 10.61 0.87 -1 2 -25 10.76 0.83 2 2 -25 3.04 0.61 2 2 -25 3.36 0.46 -2 -2 -25 2.85 0.46 -3 -2 -25 86.10 5.23 3 2 -25 89.85 5.25 3 2 -25 91.07 5.30 3 -2 -25 86.44 5.27 -3 2 -25 89.66 5.21 3 -2 -25 92.82 5.19 3 -2 -25 96.70 5.34 -4 -2 -25 33.68 2.24 4 2 -25 37.14 2.33 -4 -2 -25 36.05 2.20 -4 2 -25 36.91 2.22 4 -2 -25 38.67 2.35 4 -2 -25 38.97 2.22 0 3 -25 33.27 1.95 0 -3 -25 27.83 1.96 0 -3 -25 31.25 1.89 -1 3 -25 6.46 0.58 1 -3 -25 5.27 0.63 1 -3 -25 5.95 0.53 1 -3 -25 5.60 0.74 2 3 -25 192.71 11.10 -2 -3 -25 196.71 11.05 -2 -3 -25 189.69 11.11 -2 3 -25 203.73 11.09 2 -3 -25 186.23 11.13 2 -3 -25 204.34 11.06 2 -3 -25 197.27 11.19 3 3 -25 4.25 0.55 3 3 -25 4.78 0.63 -3 -3 -25 5.35 0.47 -3 -3 -25 5.33 0.55 -3 3 -25 4.04 0.47 3 -3 -25 4.45 0.47 3 -3 -25 3.78 0.59 0 -4 -25 1.62 0.30 0 -4 -25 1.56 0.35 0 4 -25 1.36 0.30 -1 -4 -25 10.79 0.88 1 4 -25 11.60 0.85 -1 -4 -25 11.70 0.81 1 -4 -25 10.34 0.96 -1 4 -25 10.95 0.84 1 -4 -25 9.65 0.78 -2 -4 -25 5.81 0.63 -2 -4 -25 6.07 0.55 2 4 -25 5.49 0.61 2 -4 -25 7.01 0.73 -2 4 -25 6.66 0.60 2 -4 -25 6.40 0.56 2 -4 -25 7.01 1.00 0 -5 -25 5.28 0.52 0 5 -25 6.48 0.58 0 0 -26 50.93 3.07 1 0 -26 13.49 1.02 -1 0 -26 13.75 1.01 -2 0 -26 87.10 5.16 2 0 -26 88.02 5.23 2 0 -26 91.53 5.19 -3 0 -26 26.42 1.67 3 0 -26 25.93 1.75 0 1 -26 2.88 0.42 0 -1 -26 2.45 0.44 -1 -1 -26 7.30 0.69 1 1 -26 7.50 0.68 -1 1 -26 7.80 0.67 1 -1 -26 8.13 0.72 2 1 -26 40.86 2.44 -2 -1 -26 39.81 2.43 -2 1 -26 38.59 2.40 2 -1 -26 39.53 2.51 2 -1 -26 38.66 2.45 3 1 -26 20.11 1.46 -3 -1 -26 20.57 1.38 3 -1 -26 22.84 1.50 -3 1 -26 20.23 1.37 0 2 -26 42.49 2.47 0 -2 -26 38.26 2.48 -1 -2 -26 54.99 3.01 -1 2 -26 43.86 2.93 -2 -2 -26 33.12 2.10 2 2 -26 37.29 2.11 -2 -2 -26 37.21 2.04 2 -2 -26 33.37 2.37 2 -2 -26 29.31 2.14 -2 2 -26 31.51 2.05 2 -2 -26 31.89 2.02 0 -3 -26 0.57 0.23 0 -3 -26 0.28 0.25 0 3 -26 0.06 0.19 1 3 -26 7.46 0.67 -1 -3 -26 7.05 0.70 -1 -3 -26 7.57 0.62 1 -3 -26 7.57 0.93 -1 3 -26 9.24 0.69 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 33887 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -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 0.03989(2) 0.92690(2) 0.57957(2) 0.01815(9) Uani 1 1 d . . . . . S1 S 0.22025(9) 1.05254(8) 0.49915(4) 0.0231(2) Uani 1 1 d . . . . . P1 P 0.20047(8) 0.94674(8) 0.63786(4) 0.0179(2) Uani 1 1 d . . . . . O1 O -0.1544(3) 0.9189(3) 0.73491(14) 0.0367(7) Uani 1 1 d . . . . . O2 O 0.0889(3) 1.2052(3) 0.66423(14) 0.0315(7) Uani 1 1 d . . . . . O3 O 0.2602(3) 0.9397(3) 0.48856(13) 0.0361(7) Uani 1 1 d . . . . . O4 O 0.2376(3) 1.1289(3) 0.45110(13) 0.0340(7) Uani 1 1 d . . . . . O5 O 0.0944(3) 1.0583(3) 0.52058(12) 0.0259(6) Uani 1 1 d . . . . . N1 N -0.1199(3) 0.9139(3) 0.52894(15) 0.0265(7) Uani 1 1 d . . . . . C1 C 0.2991(3) 1.0642(4) 0.61640(16) 0.0207(8) Uani 1 1 d . . . . . C2 C 0.3688(4) 1.1156(3) 0.65930(19) 0.0246(9) Uani 1 1 d . . . . . H2 H 0.362836 1.089487 0.698540 0.029 Uiso 1 1 calc R U . . . C3 C 0.4470(4) 1.2036(3) 0.6473(2) 0.0276(9) Uani 1 1 d . . . . . C4 C 0.4572(4) 1.2392(3) 0.58964(19) 0.0309(9) Uani 1 1 d . . . . . H4 H 0.511699 1.297553 0.580035 0.037 Uiso 1 1 calc R U . . . C5 C 0.3884(4) 1.1903(4) 0.5459(2) 0.0269(9) Uani 1 1 d . . . . . H5 H 0.395836 1.215769 0.506658 0.032 Uiso 1 1 calc R U . . . C6 C 0.3085(4) 1.1042(3) 0.55883(17) 0.0212(8) Uani 1 1 d . . . . . C7 C 0.1703(4) 0.9712(3) 0.71582(17) 0.0187(8) Uani 1 1 d . . . . . C8 C 0.2574(3) 0.9408(4) 0.75692(17) 0.0249(8) Uani 1 1 d . . . . . H8 H 0.328550 0.904404 0.743883 0.030 Uiso 1 1 calc R U . . . C9 C 0.0648(3) 1.0245(3) 0.73558(17) 0.0197(8) Uani 1 1 d . . . . . C10 C 0.0523(4) 1.0438(3) 0.79587(18) 0.0265(9) Uani 1 1 d . . . . . H10 H -0.019297 1.078238 0.809867 0.032 Uiso 1 1 calc R U . . . C11 C 0.1405(4) 1.0144(4) 0.83549(19) 0.0296(10) Uani 1 1 d . . . . . H11 H 0.130348 1.030188 0.876027 0.036 Uiso 1 1 calc R U . . . C12 C -0.0352(4) 1.0623(3) 0.69713(16) 0.0233(8) Uani 1 1 d . . . . . C13 C -0.0224(4) 1.1582(3) 0.66262(18) 0.0258(9) Uani 1 1 d . . . . . C14 C -0.1185(4) 1.1987(4) 0.6299(2) 0.0348(11) Uani 1 1 d . . . . . H14 H -0.109236 1.263804 0.606621 0.042 Uiso 1 1 calc R U . . . C15 C -0.1472(4) 1.0095(4) 0.69877(19) 0.0280(9) Uani 1 1 d . . . . . C16 C -0.2440(4) 1.0488(5) 0.6651(2) 0.0385(12) Uani 1 1 d . . . . . H16 H -0.319337 1.011165 0.665327 0.046 Uiso 1 1 calc R U . . . C17 C -0.2585(5) 0.8504(5) 0.7316(3) 0.0531(15) Uani 1 1 d . . . . . H17A H -0.329220 0.892972 0.744279 0.080 Uiso 1 1 calc R U . . . H17B H -0.248079 0.785446 0.757168 0.080 Uiso 1 1 calc R U . . . H17C H -0.269991 0.825422 0.691046 0.080 Uiso 1 1 calc R U . . . C18 C -0.0141(4) 0.7956(3) 0.63032(18) 0.0247(9) Uani 1 1 d . . . . . H18A H -0.101479 0.785913 0.626669 0.037 Uiso 1 1 calc R U . . . H18B H 0.006546 0.810394 0.671399 0.037 Uiso 1 1 calc R U . . . H18C H 0.026885 0.727682 0.617226 0.037 Uiso 1 1 calc R U . . . C19 C 0.3037(4) 0.8276(3) 0.63836(18) 0.0244(9) Uani 1 1 d . . . . . C20 C 0.4122(4) 0.8290(4) 0.6078(2) 0.0351(11) Uani 1 1 d . . . . . H20 H 0.437445 0.894697 0.588060 0.042 Uiso 1 1 calc R U . . . C21 C 0.4835(5) 0.7341(5) 0.6062(3) 0.0502(14) Uani 1 1 d . . . . . H21 H 0.557783 0.735392 0.585379 0.060 Uiso 1 1 calc R U . . . C22 C 0.4478(6) 0.6376(5) 0.6344(3) 0.0548(15) Uani 1 1 d . . . . . H22 H 0.496434 0.572582 0.632280 0.066 Uiso 1 1 calc R U . . . C23 C 0.2694(5) 0.7301(4) 0.6679(2) 0.0358(11) Uani 1 1 d . . . . . H23 H 0.196103 0.728254 0.689438 0.043 Uiso 1 1 calc R U . . . C24 C 0.2431(4) 0.9622(4) 0.81603(19) 0.0279(10) Uani 1 1 d . . . . . H24 H 0.303997 0.940792 0.843105 0.033 Uiso 1 1 calc R U . . . C25 C 0.1117(5) 1.2957(4) 0.6250(2) 0.0425(12) Uani 1 1 d . . . . . H25A H 0.091263 1.273219 0.584904 0.064 Uiso 1 1 calc R U . . . H25B H 0.197249 1.316005 0.626890 0.064 Uiso 1 1 calc R U . . . H25C H 0.062383 1.359900 0.636372 0.064 Uiso 1 1 calc R U . . . C26 C -0.1690(5) 1.0120(4) 0.5122(2) 0.0323(11) Uani 1 1 d . . . . . H26 H -0.124395 1.078547 0.518426 0.039 Uiso 1 1 calc R U . . . C27 C -0.2805(6) 1.0194(4) 0.4865(3) 0.0462(14) Uani 1 1 d . . . . . H27 H -0.313038 1.089973 0.476297 0.055 Uiso 1 1 calc R U . . . C28 C -0.3452(5) 0.9233(5) 0.4757(2) 0.0496(13) Uani 1 1 d . . . . . H28 H -0.423388 0.926571 0.458763 0.059 Uiso 1 1 calc R U . . . C29 C -0.2939(5) 0.8228(4) 0.4901(2) 0.0389(12) Uani 1 1 d . . . . . H29 H -0.334391 0.755000 0.481349 0.047 Uiso 1 1 calc R U . . . C30 C -0.1834(4) 0.8214(4) 0.5172(2) 0.0290(10) Uani 1 1 d . . . . . H30 H -0.150240 0.751450 0.528172 0.035 Uiso 1 1 calc R U . . . C31 C 0.3423(6) 0.6361(4) 0.6655(3) 0.0489(14) Uani 1 1 d . . . . . H31 H 0.318775 0.570279 0.685685 0.059 Uiso 1 1 calc R U . . . C32 C 0.5165(4) 1.2586(4) 0.6959(2) 0.0374(11) Uani 1 1 d . . . . . H32A H 0.602557 1.242037 0.691426 0.056 Uiso 1 1 calc R U . . . H32B H 0.488212 1.230273 0.733805 0.056 Uiso 1 1 calc R U . . . H32C H 0.504115 1.339403 0.694205 0.056 Uiso 1 1 calc R U . . . C33 C -0.2276(4) 1.1435(4) 0.6315(2) 0.0380(12) Uani 1 1 d . . . . . H33 H -0.293052 1.171282 0.608909 0.046 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02070(14) 0.01706(13) 0.01669(14) 0.00164(11) -0.00065(11) -0.00134(11) S1 0.0311(5) 0.0223(5) 0.0159(4) 0.0017(4) 0.0018(4) -0.0034(4) P1 0.0200(4) 0.0187(5) 0.0151(4) 0.0024(4) 0.0003(4) 0.0007(4) O1 0.0298(15) 0.0419(18) 0.0384(18) 0.0078(17) 0.0011(13) -0.0070(16) O2 0.0328(16) 0.0266(16) 0.0350(17) 0.0127(14) 0.0001(13) 0.0007(13) O3 0.0492(19) 0.0267(16) 0.0323(16) -0.0082(14) 0.0050(14) 0.0041(15) O4 0.0424(19) 0.0388(17) 0.0207(15) 0.0098(13) 0.0001(14) -0.0105(15) O5 0.0282(14) 0.0269(15) 0.0226(14) 0.0071(13) -0.0013(11) -0.0054(13) N1 0.0348(19) 0.0226(18) 0.0221(17) -0.0001(14) -0.0007(15) -0.0019(16) C1 0.0201(17) 0.0209(19) 0.0210(19) 0.0006(17) 0.0003(15) 0.0029(18) C2 0.022(2) 0.028(2) 0.024(2) -0.0002(17) -0.0006(17) 0.0009(17) C3 0.019(2) 0.026(2) 0.037(2) -0.0061(18) -0.0007(19) -0.0017(18) C4 0.026(2) 0.028(2) 0.040(3) -0.0005(17) 0.003(2) -0.0087(18) C5 0.024(2) 0.029(2) 0.028(2) 0.0040(17) 0.0058(18) -0.0024(17) C6 0.0226(19) 0.0205(19) 0.020(2) 0.0007(15) 0.0030(15) 0.0008(15) C7 0.0207(19) 0.0188(18) 0.0164(19) 0.0044(14) 0.0010(15) -0.0013(15) C8 0.0231(19) 0.029(2) 0.023(2) 0.0046(18) -0.0013(16) 0.0054(18) C9 0.024(2) 0.0157(17) 0.0194(19) 0.0042(15) -0.0006(16) 0.0002(15) C10 0.032(2) 0.025(2) 0.0224(19) -0.0017(15) 0.0019(18) 0.0045(18) C11 0.042(3) 0.030(2) 0.017(2) -0.0011(17) -0.0019(18) 0.004(2) C12 0.0231(18) 0.0256(19) 0.0210(18) -0.0018(16) 0.0003(16) 0.007(2) C13 0.031(2) 0.027(2) 0.020(2) 0.0012(16) 0.0014(18) 0.0112(19) C14 0.039(3) 0.039(3) 0.026(2) 0.006(2) 0.001(2) 0.018(2) C15 0.028(2) 0.031(2) 0.025(2) 0.0012(19) 0.0020(18) 0.0047(19) C16 0.020(2) 0.056(3) 0.039(3) -0.006(2) -0.0027(19) 0.005(2) C17 0.038(3) 0.057(3) 0.064(4) 0.007(3) 0.006(3) -0.019(3) C18 0.026(2) 0.024(2) 0.024(2) 0.0051(17) 0.0002(17) -0.0072(16) C19 0.027(2) 0.026(2) 0.021(2) -0.0015(16) -0.0043(17) 0.0071(17) C20 0.032(2) 0.042(3) 0.031(2) 0.003(2) 0.004(2) 0.010(2) C21 0.043(3) 0.062(3) 0.046(3) -0.001(3) 0.006(2) 0.027(3) C22 0.061(4) 0.049(3) 0.054(3) -0.001(3) -0.003(3) 0.032(3) C23 0.038(3) 0.028(2) 0.041(3) 0.006(2) -0.005(2) 0.006(2) C24 0.028(2) 0.037(2) 0.019(2) 0.0067(17) -0.0059(17) -0.0003(18) C25 0.057(3) 0.027(2) 0.043(3) 0.017(2) 0.010(3) 0.006(2) C26 0.041(3) 0.021(2) 0.034(3) 0.0007(19) -0.008(2) 0.000(2) C27 0.055(3) 0.032(3) 0.052(3) 0.003(2) -0.021(3) 0.006(3) C28 0.039(3) 0.055(3) 0.054(3) 0.000(3) -0.026(2) 0.000(3) C29 0.037(3) 0.040(3) 0.040(3) -0.004(2) -0.010(2) -0.012(2) C30 0.034(2) 0.025(2) 0.028(2) -0.0028(18) -0.0020(19) -0.0067(18) C31 0.061(4) 0.030(3) 0.057(4) 0.007(2) -0.009(3) 0.014(3) C32 0.025(2) 0.045(3) 0.042(3) -0.014(2) 0.000(2) -0.008(2) C33 0.031(3) 0.052(3) 0.031(3) -0.001(2) -0.006(2) 0.022(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.0375 3.1039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2925 0.4295 '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 C18 Pd1 N1 90.39(15) . . ? C18 Pd1 O5 175.94(15) . . ? N1 Pd1 O5 87.06(12) . . ? C18 Pd1 P1 88.79(12) . . ? N1 Pd1 P1 175.90(10) . . ? O5 Pd1 P1 93.98(8) . . ? O4 S1 O3 115.3(2) . . ? O4 S1 O5 110.32(19) . . ? O3 S1 O5 112.82(19) . . ? O4 S1 C6 106.56(19) . . ? O3 S1 C6 106.53(18) . . ? O5 S1 C6 104.42(17) . . ? C19 P1 C7 103.49(18) . . ? C19 P1 C1 103.11(19) . . ? C7 P1 C1 104.02(18) . . ? C19 P1 Pd1 114.75(14) . . ? C7 P1 Pd1 116.63(13) . . ? C1 P1 Pd1 113.28(12) . . ? C15 O1 C17 118.5(4) . . ? C13 O2 C25 117.4(4) . . ? S1 O5 Pd1 115.83(17) . . ? C30 N1 C26 116.9(4) . . ? C30 N1 Pd1 127.4(3) . . ? C26 N1 Pd1 115.2(3) . . ? C2 C1 C6 117.7(4) . . ? C2 C1 P1 118.7(3) . . ? C6 C1 P1 123.6(3) . . ? C1 C2 C3 123.0(4) . . ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C4 C3 C2 118.0(4) . . ? C4 C3 C32 121.5(4) . . ? C2 C3 C32 120.5(4) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 120.0(4) . . ? C5 C6 S1 116.4(3) . . ? C1 C6 S1 123.6(3) . . ? C8 C7 C9 118.7(4) . . ? C8 C7 P1 118.9(3) . . ? C9 C7 P1 122.4(3) . . ? C24 C8 C7 121.9(4) . . ? C24 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C7 118.1(4) . . ? C10 C9 C12 117.0(4) . . ? C7 C9 C12 124.8(3) . . ? C11 C10 C9 122.1(4) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C24 C11 C10 119.6(4) . . ? C24 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C15 C12 C13 118.6(4) . . ? C15 C12 C9 120.7(3) . . ? C13 C12 C9 120.4(4) . . ? O2 C13 C14 124.6(4) . . ? O2 C13 C12 114.7(4) . . ? C14 C13 C12 120.7(4) . . ? C33 C14 C13 119.4(4) . . ? C33 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? O1 C15 C12 115.4(4) . . ? O1 C15 C16 123.6(4) . . ? C12 C15 C16 121.0(4) . . ? C33 C16 C15 118.7(4) . . ? C33 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Pd1 C18 H18A 109.5 . . ? Pd1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Pd1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C23 119.0(4) . . ? C20 C19 P1 121.9(3) . . ? C23 C19 P1 119.0(3) . . ? C21 C20 C19 119.8(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.8(5) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C31 C22 C21 119.9(5) . . ? C31 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C31 C23 C19 120.1(5) . . ? C31 C23 H23 119.9 . . ? C19 C23 H23 119.9 . . ? C11 C24 C8 119.7(4) . . ? C11 C24 H24 120.2 . . ? C8 C24 H24 120.2 . . ? O2 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 122.7(4) . . ? N1 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C28 119.4(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 118.4(4) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 119.2(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N1 C30 C29 123.3(4) . . ? N1 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? C22 C31 C23 120.4(5) . . ? C22 C31 H31 119.8 . . ? C23 C31 H31 119.8 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C14 C33 C16 121.6(4) . . ? C14 C33 H33 119.2 . . ? C16 C33 H33 119.2 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C18 2.044(4) . ? Pd1 N1 2.121(4) . ? Pd1 O5 2.159(3) . ? Pd1 P1 2.2345(10) . ? S1 O4 1.441(3) . ? S1 O3 1.445(3) . ? S1 O5 1.480(3) . ? S1 C6 1.787(4) . ? P1 C19 1.831(4) . ? P1 C7 1.832(4) . ? P1 C1 1.850(4) . ? O1 C15 1.367(6) . ? O1 C17 1.419(6) . ? O2 C13 1.357(5) . ? O2 C25 1.429(5) . ? N1 C30 1.342(6) . ? N1 C26 1.352(6) . ? C1 C2 1.391(6) . ? C1 C6 1.401(6) . ? C2 C3 1.395(6) . ? C2 H2 0.9500 . ? C3 C4 1.387(6) . ? C3 C32 1.502(6) . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(6) . ? C5 H5 0.9500 . ? C7 C8 1.394(6) . ? C7 C9 1.407(6) . ? C8 C24 1.381(6) . ? C8 H8 0.9500 . ? C9 C10 1.401(6) . ? C9 C12 1.484(5) . ? C10 C11 1.377(6) . ? C10 H10 0.9500 . ? C11 C24 1.373(6) . ? C11 H11 0.9500 . ? C12 C15 1.394(6) . ? C12 C13 1.402(6) . ? C13 C14 1.388(6) . ? C14 C33 1.379(7) . ? C14 H14 0.9500 . ? C15 C16 1.402(6) . ? C16 C33 1.383(8) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.391(7) . ? C19 C23 1.403(6) . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 C22 1.383(9) . ? C21 H21 0.9500 . ? C22 C31 1.368(9) . ? C22 H22 0.9500 . ? C23 C31 1.389(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.371(8) . ? C26 H26 0.9500 . ? C27 C28 1.380(8) . ? C27 H27 0.9500 . ? C28 C29 1.373(8) . ? C28 H28 0.9500 . ? C29 C30 1.372(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33 0.9500 . ? 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 O4 S1 O5 Pd1 167.49(17) . . . . ? O3 S1 O5 Pd1 36.9(2) . . . . ? C6 S1 O5 Pd1 -78.4(2) . . . . ? C19 P1 C1 C2 -82.3(3) . . . . ? C7 P1 C1 C2 25.5(4) . . . . ? Pd1 P1 C1 C2 153.1(3) . . . . ? C19 P1 C1 C6 97.2(4) . . . . ? C7 P1 C1 C6 -155.1(3) . . . . ? Pd1 P1 C1 C6 -27.4(4) . . . . ? C6 C1 C2 C3 -0.4(6) . . . . ? P1 C1 C2 C3 179.1(3) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C1 C2 C3 C32 177.7(4) . . . . ? C2 C3 C4 C5 1.9(7) . . . . ? C32 C3 C4 C5 -177.3(4) . . . . ? C3 C4 C5 C6 -0.4(7) . . . . ? C4 C5 C6 C1 -1.6(6) . . . . ? C4 C5 C6 S1 177.3(3) . . . . ? C2 C1 C6 C5 1.9(6) . . . . ? P1 C1 C6 C5 -177.5(3) . . . . ? C2 C1 C6 S1 -176.8(3) . . . . ? P1 C1 C6 S1 3.7(5) . . . . ? O4 S1 C6 C5 -10.4(4) . . . . ? O3 S1 C6 C5 113.2(3) . . . . ? O5 S1 C6 C5 -127.2(3) . . . . ? O4 S1 C6 C1 168.4(3) . . . . ? O3 S1 C6 C1 -68.0(4) . . . . ? O5 S1 C6 C1 51.6(4) . . . . ? C19 P1 C7 C8 27.6(4) . . . . ? C1 P1 C7 C8 -79.9(3) . . . . ? Pd1 P1 C7 C8 154.6(3) . . . . ? C19 P1 C7 C9 -155.5(3) . . . . ? C1 P1 C7 C9 97.1(3) . . . . ? Pd1 P1 C7 C9 -28.5(4) . . . . ? C9 C7 C8 C24 -0.4(6) . . . . ? P1 C7 C8 C24 176.6(3) . . . . ? C8 C7 C9 C10 -0.3(5) . . . . ? P1 C7 C9 C10 -177.2(3) . . . . ? C8 C7 C9 C12 179.6(4) . . . . ? P1 C7 C9 C12 2.7(6) . . . . ? C7 C9 C10 C11 1.3(6) . . . . ? C12 C9 C10 C11 -178.6(4) . . . . ? C9 C10 C11 C24 -1.5(7) . . . . ? C10 C9 C12 C15 -69.2(5) . . . . ? C7 C9 C12 C15 110.9(5) . . . . ? C10 C9 C12 C13 104.7(4) . . . . ? C7 C9 C12 C13 -75.3(5) . . . . ? C25 O2 C13 C14 -6.6(6) . . . . ? C25 O2 C13 C12 173.2(4) . . . . ? C15 C12 C13 O2 179.1(4) . . . . ? C9 C12 C13 O2 5.0(5) . . . . ? C15 C12 C13 C14 -1.2(6) . . . . ? C9 C12 C13 C14 -175.2(4) . . . . ? O2 C13 C14 C33 179.7(4) . . . . ? C12 C13 C14 C33 0.0(7) . . . . ? C17 O1 C15 C12 -169.8(4) . . . . ? C17 O1 C15 C16 10.2(7) . . . . ? C13 C12 C15 O1 -177.7(4) . . . . ? C9 C12 C15 O1 -3.7(6) . . . . ? C13 C12 C15 C16 2.3(6) . . . . ? C9 C12 C15 C16 176.3(4) . . . . ? O1 C15 C16 C33 177.9(4) . . . . ? C12 C15 C16 C33 -2.1(7) . . . . ? C7 P1 C19 C20 -129.0(4) . . . . ? C1 P1 C19 C20 -20.8(4) . . . . ? Pd1 P1 C19 C20 102.9(4) . . . . ? C7 P1 C19 C23 54.5(4) . . . . ? C1 P1 C19 C23 162.7(3) . . . . ? Pd1 P1 C19 C23 -73.7(4) . . . . ? C23 C19 C20 C21 1.0(7) . . . . ? P1 C19 C20 C21 -175.6(4) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? C20 C21 C22 C31 -1.5(9) . . . . ? C20 C19 C23 C31 -1.0(7) . . . . ? P1 C19 C23 C31 175.6(4) . . . . ? C10 C11 C24 C8 0.7(7) . . . . ? C7 C8 C24 C11 0.2(7) . . . . ? C30 N1 C26 C27 2.7(7) . . . . ? Pd1 N1 C26 C27 -170.6(4) . . . . ? N1 C26 C27 C28 -1.7(9) . . . . ? C26 C27 C28 C29 -1.3(9) . . . . ? C27 C28 C29 C30 3.2(8) . . . . ? C26 N1 C30 C29 -0.7(7) . . . . ? Pd1 N1 C30 C29 171.6(4) . . . . ? C28 C29 C30 N1 -2.3(8) . . . . ? C21 C22 C31 C23 1.4(9) . . . . ? C19 C23 C31 C22 -0.2(8) . . . . ? C13 C14 C33 C16 0.2(7) . . . . ? C15 C16 C33 C14 0.8(7) . . . . ?