#------------------------------------------------------------------------------ #$Date: 2019-07-13 03:19:52 +0300 (Sat, 13 Jul 2019) $ #$Revision: 216988 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552096.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_1552096 loop_ _publ_author_name 'Scott, Neil W. J.' 'Ford, Mark J.' 'Schotes, Christoph' 'Parker, Rachel R.' 'Whitwood, Adrian C.' 'Fairlamb, Ian J. S.' _publ_section_title ; The ubiquitous cross-coupling catalyst system ‘Pd(OAc)2’/2PPh3 forms a unique dinuclear PdI complex: an important entry point into catalytically competent cyclic Pd3 clusters ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC01847F _journal_year 2019 _chemical_formula_moiety 'C40 H36 O4 P2 Pd' _chemical_formula_sum 'C40 H36 O4 P2 Pd' _chemical_formula_weight 749.03 _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 _atom_sites_solution_primary dual _audit_creation_date 2018-03-23 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-01-31 deposited with the CCDC. 2019-07-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.765(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.6975(2) _cell_length_b 15.0053(3) _cell_length_c 19.3767(3) _cell_measurement_reflns_used 5912 _cell_measurement_temperature 110.05(10) _cell_measurement_theta_max 70.5410 _cell_measurement_theta_min 4.7970 _cell_volume 3389.33(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 110.05(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -28.00 21.00 1.00 1.50 -- 0.00 -57.00 -30.00 49 2 \w 32.00 107.00 1.00 4.50 -- 54.00-125.00 60.00 75 3 \w 49.00 77.00 1.00 4.50 -- 108.00-111.00 60.00 28 4 \w 37.00 114.00 1.00 4.50 -- 108.00-111.00 120.00 77 5 \w 46.00 136.00 1.00 4.50 -- 108.00 -77.00 150.00 90 6 \w 130.00 156.00 1.00 4.50 -- 108.00 25.00 0.00 26 7 \w 108.00 172.00 1.00 4.50 -- 108.00 62.00 -61.00 64 8 \w 99.00 140.00 1.00 4.50 -- 108.00 -25.00-150.00 41 9 \w 48.00 97.00 1.00 4.50 -- 108.00 -50.00 -90.00 49 10 \w 35.00 84.00 1.00 4.50 -- 108.00 -25.00-150.00 49 11 \w 23.00 78.00 1.00 4.50 -- 54.00-125.00 -60.00 55 12 \w 9.00 69.00 1.00 4.50 -- 54.00 -57.00 120.00 60 13 \w 90.00 148.00 1.00 4.50 -- 108.00 50.00 60.00 58 14 \w 68.00 96.00 1.00 4.50 -- 108.00 178.00 -30.00 28 15 \w 31.00 123.00 1.00 4.50 -- 54.00 77.00 90.00 92 16 \w -26.00 15.00 1.00 1.50 -- 0.00 91.00 171.00 41 17 \w -61.00 -34.00 1.00 1.50 -- 0.00 -57.00 -30.00 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1005092000 _diffrn_orient_matrix_UB_12 -0.0483546000 _diffrn_orient_matrix_UB_13 0.0304178000 _diffrn_orient_matrix_UB_21 -0.0184754000 _diffrn_orient_matrix_UB_22 -0.0565909000 _diffrn_orient_matrix_UB_23 -0.0663276000 _diffrn_orient_matrix_UB_31 0.0836956000 _diffrn_orient_matrix_UB_32 -0.0707040000 _diffrn_orient_matrix_UB_33 0.0323649000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 12675 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.065 _diffrn_reflns_theta_max 67.065 _diffrn_reflns_theta_min 3.731 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.641 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.468 _exptl_crystal_description block _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.193 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.094 _refine_diff_density_max 0.711 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 426 _refine_ls_number_reflns 6044 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0289 _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^)+(0.0334P)^2^+1.5655P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.0743 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5295 _reflns_number_total 6044 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; ijsf1807a.res created by SHELXL-2014/7 TITL ijsf1807a_a.res in P2(1)/c REM Old TITL ijsf1807a_a.res in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.065, Rweak 0.011, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C40 O4 P2 Pd CELL 1.54184 11.6975 15.0053 19.3767 90 94.765 90 ZERR 4 0.0002 0.0003 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O P Pd UNIT 160 144 16 8 4 L.S. 10 PLAN 20 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.033400 1.565500 FVAR 0.27725 PD1 5 0.656964 0.733668 0.380593 11.00000 0.01835 0.01952 = 0.02064 -0.00039 0.00140 0.00199 P2 4 0.463441 0.765639 0.391717 11.00000 0.01862 0.02174 = 0.02110 -0.00226 0.00251 0.00177 P1 4 0.840373 0.711549 0.346320 11.00000 0.01797 0.02352 = 0.02111 0.00064 0.00179 0.00248 O1 3 0.686676 0.863925 0.361436 11.00000 0.02311 0.02122 = 0.02475 -0.00045 0.00011 0.00155 O3 3 0.628787 0.602131 0.396058 11.00000 0.02839 0.02213 = 0.03086 0.00139 -0.00089 0.00039 O2 3 0.699324 0.885314 0.476105 11.00000 0.04702 0.03177 = 0.02388 0.00135 0.00371 -0.00021 O4 3 0.725812 0.616524 0.498860 11.00000 0.06879 0.03257 = 0.03117 -0.00133 -0.00975 0.00799 C36 1 0.405888 0.946802 0.405180 11.00000 0.02344 0.02794 = 0.03033 0.00047 0.00404 0.00118 AFIX 43 H36 2 0.400368 0.935610 0.451993 11.00000 -1.20000 AFIX 0 C31 1 0.432447 0.878124 0.361616 11.00000 0.01393 0.02669 = 0.02767 -0.00076 0.00251 0.00091 C14 1 0.883483 0.661033 0.210117 11.00000 0.02052 0.02375 = 0.03182 -0.00195 0.00196 -0.00062 AFIX 43 H14 2 0.929305 0.615611 0.229920 11.00000 -1.20000 AFIX 0 C13 1 0.829120 0.720392 0.252096 11.00000 0.01849 0.02480 = 0.02213 -0.00181 0.00097 -0.00408 C37 1 0.701740 0.912849 0.416907 11.00000 0.02185 0.02643 = 0.02684 -0.00077 -0.00006 0.00369 C30 1 0.359725 0.697649 0.338909 11.00000 0.02373 0.03189 = 0.02335 -0.00610 0.00441 -0.00253 C9 1 1.033480 0.881508 0.471506 11.00000 0.02647 0.04556 = 0.02643 -0.00781 -0.00091 0.00098 AFIX 43 H9 2 1.044415 0.891965 0.518902 11.00000 -1.20000 AFIX 0 C16 1 0.801990 0.737586 0.108696 11.00000 0.03259 0.03317 = 0.02120 0.00032 0.00252 -0.00913 AFIX 43 H16 2 0.791298 0.742341 0.060740 11.00000 -1.20000 AFIX 0 C12 1 0.999046 0.850816 0.330864 11.00000 0.02981 0.02910 = 0.02659 -0.00215 0.00233 -0.00236 AFIX 43 H12 2 0.986943 0.841530 0.283365 11.00000 -1.20000 AFIX 0 C17 1 0.751211 0.797836 0.150156 11.00000 0.03133 0.03097 = 0.02857 0.00408 0.00043 0.00050 AFIX 43 H17 2 0.708552 0.844738 0.129968 11.00000 -1.20000 AFIX 0 C1 1 0.908804 0.604445 0.365169 11.00000 0.02786 0.03365 = 0.02618 0.00683 0.00882 0.00985 C19 1 0.414287 0.758462 0.478160 11.00000 0.02644 0.01820 = 0.02551 -0.00108 0.00584 -0.00028 C15 1 0.868906 0.670056 0.138869 11.00000 0.03298 0.03059 = 0.02764 -0.00893 0.00816 -0.00494 AFIX 43 H15 2 0.904662 0.630098 0.110940 11.00000 -1.20000 AFIX 0 C32 1 0.442405 0.896266 0.291498 11.00000 0.02516 0.03793 = 0.02674 0.00139 0.00280 0.00629 AFIX 43 H32 2 0.461517 0.850773 0.261957 11.00000 -1.20000 AFIX 0 C35 1 0.387410 1.032502 0.379261 11.00000 0.02888 0.02633 = 0.04665 -0.00336 0.00225 0.00529 AFIX 43 H35 2 0.368951 1.078415 0.408603 11.00000 -1.20000 AFIX 0 C10 1 1.091568 0.932534 0.426688 11.00000 0.02431 0.02866 = 0.04072 -0.00568 -0.00456 0.00077 AFIX 43 H10 2 1.142190 0.976688 0.443612 11.00000 -1.20000 AFIX 0 C18 1 0.762866 0.789460 0.221446 11.00000 0.02711 0.02485 = 0.02589 -0.00133 0.00392 0.00141 AFIX 43 H18 2 0.726685 0.829712 0.248926 11.00000 -1.20000 AFIX 0 C2 1 0.851634 0.528149 0.339689 11.00000 0.03753 0.02815 = 0.04508 0.00463 0.01290 0.00966 AFIX 43 H2 2 0.781449 0.533550 0.313735 11.00000 -1.20000 AFIX 0 C7 1 0.942042 0.797814 0.376304 11.00000 0.01741 0.02569 = 0.02827 -0.00213 0.00267 0.00217 C38 1 0.724515 1.009321 0.401767 11.00000 0.04432 0.02533 = 0.03310 -0.00161 -0.00154 -0.00537 AFIX 137 H38A 2 0.802846 1.016309 0.391391 11.00000 -1.50000 H38B 2 0.710782 1.044816 0.441461 11.00000 -1.50000 H38C 2 0.674442 1.028367 0.362792 11.00000 -1.50000 AFIX 0 C24 1 0.297819 0.756520 0.488552 11.00000 0.02904 0.02839 = 0.02858 0.00164 0.00489 0.00406 AFIX 43 H24 2 0.243540 0.757931 0.450672 11.00000 -1.20000 AFIX 0 C8 1 0.959110 0.814929 0.446845 11.00000 0.02307 0.04290 = 0.02617 -0.00158 0.00316 -0.00034 AFIX 43 H8 2 0.920224 0.781355 0.477763 11.00000 -1.20000 AFIX 0 C20 1 0.494580 0.755630 0.535061 11.00000 0.02672 0.03867 = 0.02958 0.00200 0.00428 -0.00367 AFIX 43 H20 2 0.572567 0.755886 0.528856 11.00000 -1.20000 AFIX 0 C34 1 0.396555 1.049286 0.309726 11.00000 0.03537 0.03123 = 0.04812 0.01384 -0.00137 0.00805 AFIX 43 H34 2 0.384186 1.106545 0.292310 11.00000 -1.20000 AFIX 0 C11 1 1.073605 0.917225 0.356179 11.00000 0.03132 0.02976 = 0.03515 0.00254 0.00319 -0.00365 AFIX 43 H11 2 1.111836 0.951745 0.325540 11.00000 -1.20000 AFIX 0 C6 1 1.012601 0.595772 0.404888 11.00000 0.03095 0.05508 = 0.03601 0.01131 0.00500 0.01716 AFIX 43 H6 2 1.051691 0.645788 0.422670 11.00000 -1.20000 AFIX 0 C29 1 0.261007 0.733943 0.305701 11.00000 0.02425 0.04098 = 0.04079 -0.00375 0.00036 -0.00131 AFIX 43 H29 2 0.248029 0.794963 0.308173 11.00000 -1.20000 AFIX 0 C22 1 0.342543 0.751047 0.611145 11.00000 0.04693 0.03096 = 0.02836 0.00181 0.01717 -0.00001 AFIX 43 H22 2 0.318748 0.749144 0.655740 11.00000 -1.20000 AFIX 0 C39 1 0.670297 0.572738 0.455860 11.00000 0.03340 0.02739 = 0.03250 -0.00073 0.00648 0.00488 C28 1 0.181505 0.680003 0.268847 11.00000 0.02348 0.05539 = 0.04056 -0.00761 -0.00309 -0.00229 AFIX 43 H28 2 0.115657 0.705121 0.246680 11.00000 -1.20000 AFIX 0 C33 1 0.424023 0.981143 0.266144 11.00000 0.03305 0.04443 = 0.03285 0.01245 -0.00013 0.00583 AFIX 43 H33 2 0.430121 0.992690 0.219437 11.00000 -1.20000 AFIX 0 C25 1 0.377263 0.606329 0.333916 11.00000 0.03248 0.03491 = 0.05515 -0.01523 -0.00904 0.00138 AFIX 43 H25 2 0.443065 0.580674 0.355704 11.00000 -1.20000 AFIX 0 C27 1 0.199121 0.589951 0.264800 11.00000 0.02665 0.05690 = 0.04209 -0.01950 0.00400 -0.00950 AFIX 43 H27 2 0.144877 0.553940 0.240610 11.00000 -1.20000 AFIX 0 C23 1 0.262467 0.752504 0.554875 11.00000 0.03177 0.03112 = 0.03696 0.00494 0.01288 0.00374 AFIX 43 H23 2 0.184645 0.750789 0.561458 11.00000 -1.20000 AFIX 0 C21 1 0.457586 0.752405 0.601439 11.00000 0.04317 0.04391 = 0.02273 0.00053 0.00100 -0.00523 AFIX 43 H21 2 0.511262 0.751155 0.639625 11.00000 -1.20000 AFIX 0 C5 1 1.057533 0.509616 0.417715 11.00000 0.04557 0.07568 = 0.05125 0.02067 0.00573 0.03423 AFIX 43 H5 2 1.127064 0.502954 0.444164 11.00000 -1.20000 AFIX 0 C3 1 0.898316 0.444704 0.352658 11.00000 0.06189 0.02936 = 0.05884 0.00685 0.02722 0.01225 AFIX 43 H3 2 0.860370 0.394259 0.334740 11.00000 -1.20000 AFIX 0 C40 1 0.644077 0.475304 0.467257 11.00000 0.06592 0.02906 = 0.05950 0.01202 0.01111 0.00337 AFIX 137 H40A 2 0.568206 0.462002 0.447170 11.00000 -1.50000 H40B 2 0.648650 0.463042 0.516034 11.00000 -1.50000 H40C 2 0.698749 0.439078 0.445794 11.00000 -1.50000 AFIX 0 C4 1 1.001024 0.436314 0.392118 11.00000 0.06948 0.04157 = 0.06651 0.02558 0.03231 0.03415 AFIX 43 H4 2 1.031904 0.380023 0.401300 11.00000 -1.20000 AFIX 0 C26 1 0.296934 0.553228 0.296528 11.00000 0.04550 0.03643 = 0.07337 -0.01993 -0.00489 -0.00389 AFIX 43 H26 2 0.309699 0.492283 0.293026 11.00000 -1.20000 AFIX 0 HKLF 4 REM ijsf1807a_a.res in P2(1)/c REM R1 = 0.0289 for 5295 Fo > 4sig(Fo) and 0.0354 for all 6044 data REM 426 parameters refined using 0 restraints END WGHT 0.0334 1.5655 REM Highest difference peak 0.711, deepest hole -0.513, 1-sigma level 0.066 Q1 1 0.6214 0.7177 0.4230 11.00000 0.05 0.71 Q2 1 0.7573 0.7657 0.3687 11.00000 0.05 0.51 Q3 1 0.4396 0.7663 0.4350 11.00000 0.05 0.49 Q4 1 0.7615 0.6958 0.3685 11.00000 0.05 0.47 Q5 1 0.6987 0.7665 0.4164 11.00000 0.05 0.39 Q6 1 0.7605 0.7349 0.2994 11.00000 0.05 0.38 Q7 1 0.5559 0.7762 0.3943 11.00000 0.05 0.38 Q8 1 0.8395 0.7238 0.2892 11.00000 0.05 0.37 Q9 1 0.8166 0.6616 0.4185 11.00000 0.05 0.34 Q10 1 0.7028 0.6980 0.4231 11.00000 0.05 0.32 Q11 1 0.6857 0.7444 0.3331 11.00000 0.05 0.32 Q12 1 0.4063 0.7333 0.3542 11.00000 0.05 0.30 Q13 1 0.5944 0.6953 0.3368 11.00000 0.05 0.30 Q14 1 0.4529 0.7428 0.5002 11.00000 0.05 0.30 Q15 1 0.6007 0.7717 0.3327 11.00000 0.05 0.29 Q16 1 0.8654 0.6530 0.3686 11.00000 0.05 0.28 Q17 1 0.8133 0.7623 0.2345 11.00000 0.05 0.28 Q18 1 0.5352 0.7371 0.4317 11.00000 0.05 0.26 Q19 1 0.8277 0.6820 0.2313 11.00000 0.05 0.25 Q20 1 0.6223 0.5196 0.5048 11.00000 0.05 0.25 REM The information below was added by Olex2. REM REM R1 = 0.0289 for 5295 Fo > 4sig(Fo) and 0.0354 for all 13034 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.71, deepest hole -0.51 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0354 REM R1_gt = 0.0289 REM wR_ref = 0.0743 REM GOOF = 1.043 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 13034 REM Reflections_gt = 5295 REM Parameters = n/a REM Hole = -0.51 REM Peak = 0.71 REM Flack = n/a ; _cod_data_source_file c9sc01847f2.cif _cod_data_source_block ijsf1807a _cod_database_code 1552096 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C86 H73 O2 P5 Pd3' _chemical_oxdiff_usercomment 'Neil Scott nwjs-3-204-recryst' _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. ; _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C36(H36), C14(H14), C9(H9), C16(H16), C12(H12), C17(H17), C15(H15), C32(H32), C35(H35), C10(H10), C18(H18), C2(H2), C24(H24), C8(H8), C20(H20), C34(H34), C11(H11), C6(H6), C29(H29), C22(H22), C28(H28), C33(H33), C25(H25), C27(H27), C23(H23), C21(H21), C5(H5), C3(H3), C4(H4), C26(H26) 2.b Idealised Me refined as rotating group: C38(H38A,H38B,H38C), C40(H40A,H40B,H40C) ; _olex2_date_sample_data_collection 2018-03-16 _olex2_date_sample_submission 2018-03-12 _olex2_exptl_crystal_mounting_method 'oil on micromount ' _olex2_submission_original_sample_id 'Neil Scott -3-204-recrys' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.765 _oxdiff_exptl_absorpt_empirical_full_min 0.814 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 Pd1 Pd 0.65696(2) 0.73367(2) 0.38059(2) 0.01951(7) Uani 1 1 d . P2 P 0.46344(5) 0.76564(4) 0.39172(3) 0.02044(14) Uani 1 1 d . P1 P 0.84037(5) 0.71155(4) 0.34632(3) 0.02086(14) Uani 1 1 d . O1 O 0.68668(14) 0.86392(12) 0.36144(9) 0.0231(4) Uani 1 1 d . O3 O 0.62879(15) 0.60213(12) 0.39606(10) 0.0273(4) Uani 1 1 d . O2 O 0.69932(18) 0.88531(14) 0.47610(10) 0.0342(5) Uani 1 1 d . O4 O 0.7258(2) 0.61652(15) 0.49886(11) 0.0449(6) Uani 1 1 d . C36 C 0.4059(2) 0.94680(19) 0.40518(15) 0.0271(6) Uani 1 1 d . H36 H 0.4004 0.9356 0.4520 0.033 Uiso 1 1 calc R C31 C 0.4324(2) 0.87812(18) 0.36162(13) 0.0227(5) Uani 1 1 d . C14 C 0.8835(2) 0.66103(18) 0.21012(14) 0.0254(6) Uani 1 1 d . H14 H 0.9293 0.6156 0.2299 0.030 Uiso 1 1 calc R C13 C 0.8291(2) 0.72039(17) 0.25210(13) 0.0218(5) Uani 1 1 d . C37 C 0.7017(2) 0.91285(18) 0.41691(14) 0.0252(6) Uani 1 1 d . C30 C 0.3597(2) 0.69765(19) 0.33891(14) 0.0262(6) Uani 1 1 d . C9 C 1.0335(2) 0.8815(2) 0.47151(15) 0.0330(7) Uani 1 1 d . H9 H 1.0444 0.8920 0.5189 0.040 Uiso 1 1 calc R C16 C 0.8020(2) 0.73759(19) 0.10870(15) 0.0290(6) Uani 1 1 d . H16 H 0.7913 0.7423 0.0607 0.035 Uiso 1 1 calc R C12 C 0.9990(2) 0.85082(19) 0.33086(15) 0.0285(6) Uani 1 1 d . H12 H 0.9869 0.8415 0.2834 0.034 Uiso 1 1 calc R C17 C 0.7512(2) 0.7978(2) 0.15016(15) 0.0304(6) Uani 1 1 d . H17 H 0.7086 0.8447 0.1300 0.036 Uiso 1 1 calc R C1 C 0.9088(2) 0.6044(2) 0.36517(14) 0.0289(6) Uani 1 1 d . C19 C 0.4143(2) 0.75846(17) 0.47816(14) 0.0232(6) Uani 1 1 d . C15 C 0.8689(2) 0.6701(2) 0.13887(14) 0.0301(6) Uani 1 1 d . H15 H 0.9047 0.6301 0.1109 0.036 Uiso 1 1 calc R C32 C 0.4424(2) 0.8963(2) 0.29150(14) 0.0299(6) Uani 1 1 d . H32 H 0.4615 0.8508 0.2620 0.036 Uiso 1 1 calc R C35 C 0.3874(2) 1.0325(2) 0.37926(16) 0.0340(7) Uani 1 1 d . H35 H 0.3690 1.0784 0.4086 0.041 Uiso 1 1 calc R C10 C 1.0916(2) 0.93253(19) 0.42669(15) 0.0316(7) Uani 1 1 d . H10 H 1.1422 0.9767 0.4436 0.038 Uiso 1 1 calc R C18 C 0.7629(2) 0.78946(18) 0.22145(14) 0.0259(6) Uani 1 1 d . H18 H 0.7267 0.8297 0.2489 0.031 Uiso 1 1 calc R C2 C 0.8516(3) 0.5281(2) 0.33969(17) 0.0364(7) Uani 1 1 d . H2 H 0.7814 0.5335 0.3137 0.044 Uiso 1 1 calc R C7 C 0.9420(2) 0.79781(18) 0.37630(14) 0.0237(6) Uani 1 1 d . C38 C 0.7245(3) 1.00932(19) 0.40177(16) 0.0345(7) Uani 1 1 d . H38A H 0.8028 1.0163 0.3914 0.052 Uiso 1 1 calc GR H38B H 0.7108 1.0448 0.4415 0.052 Uiso 1 1 calc GR H38C H 0.6744 1.0284 0.3628 0.052 Uiso 1 1 calc GR C24 C 0.2978(2) 0.75652(18) 0.48855(15) 0.0285(6) Uani 1 1 d . H24 H 0.2435 0.7579 0.4507 0.034 Uiso 1 1 calc R C8 C 0.9591(2) 0.8149(2) 0.44684(14) 0.0307(6) Uani 1 1 d . H8 H 0.9202 0.7814 0.4778 0.037 Uiso 1 1 calc R C20 C 0.4946(2) 0.7556(2) 0.53506(15) 0.0315(6) Uani 1 1 d . H20 H 0.5726 0.7559 0.5289 0.038 Uiso 1 1 calc R C34 C 0.3966(3) 1.0493(2) 0.30973(17) 0.0385(7) Uani 1 1 d . H34 H 0.3842 1.1065 0.2923 0.046 Uiso 1 1 calc R C11 C 1.0736(2) 0.9172(2) 0.35618(16) 0.0321(6) Uani 1 1 d . H11 H 1.1118 0.9517 0.3255 0.038 Uiso 1 1 calc R C6 C 1.0126(3) 0.5958(2) 0.40489(16) 0.0406(8) Uani 1 1 d . H6 H 1.0517 0.6458 0.4227 0.049 Uiso 1 1 calc R C29 C 0.2610(2) 0.7339(2) 0.30570(17) 0.0355(7) Uani 1 1 d . H29 H 0.2480 0.7950 0.3082 0.043 Uiso 1 1 calc R C22 C 0.3425(3) 0.7510(2) 0.61115(16) 0.0346(7) Uani 1 1 d . H22 H 0.3187 0.7491 0.6557 0.042 Uiso 1 1 calc R C39 C 0.6703(2) 0.57274(19) 0.45586(15) 0.0309(6) Uani 1 1 d . C28 C 0.1815(2) 0.6800(2) 0.26885(16) 0.0401(8) Uani 1 1 d . H28 H 0.1157 0.7051 0.2467 0.048 Uiso 1 1 calc R C33 C 0.4240(2) 0.9811(2) 0.26614(16) 0.0369(7) Uani 1 1 d . H33 H 0.4301 0.9927 0.2194 0.044 Uiso 1 1 calc R C25 C 0.3773(3) 0.6063(2) 0.33392(18) 0.0416(8) Uani 1 1 d . H25 H 0.4431 0.5807 0.3557 0.050 Uiso 1 1 calc R C27 C 0.1991(3) 0.5900(2) 0.26480(17) 0.0418(8) Uani 1 1 d . H27 H 0.1449 0.5539 0.2406 0.050 Uiso 1 1 calc R C23 C 0.2625(3) 0.75250(19) 0.55488(16) 0.0327(7) Uani 1 1 d . H23 H 0.1846 0.7508 0.5615 0.039 Uiso 1 1 calc R C21 C 0.4576(3) 0.7524(2) 0.60144(16) 0.0367(7) Uani 1 1 d . H21 H 0.5113 0.7512 0.6396 0.044 Uiso 1 1 calc R C5 C 1.0575(3) 0.5096(3) 0.4177(2) 0.0574(11) Uani 1 1 d . H5 H 1.1271 0.5030 0.4442 0.069 Uiso 1 1 calc R C3 C 0.8983(3) 0.4447(2) 0.35266(19) 0.0488(9) Uani 1 1 d . H3 H 0.8604 0.3943 0.3347 0.059 Uiso 1 1 calc R C40 C 0.6441(3) 0.4753(2) 0.4673(2) 0.0512(9) Uani 1 1 d . H40A H 0.5682 0.4620 0.4472 0.077 Uiso 1 1 calc GR H40B H 0.6487 0.4630 0.5160 0.077 Uiso 1 1 calc GR H40C H 0.6987 0.4391 0.4458 0.077 Uiso 1 1 calc GR C4 C 1.0010(3) 0.4363(3) 0.3921(2) 0.0577(11) Uani 1 1 d . H4 H 1.0319 0.3800 0.4013 0.069 Uiso 1 1 calc R C26 C 0.2969(3) 0.5532(2) 0.2965(2) 0.0523(9) Uani 1 1 d . H26 H 0.3097 0.4923 0.2930 0.063 Uiso 1 1 calc R 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 0.01835(10) 0.01952(11) 0.02064(11) -0.00039(7) 0.00140(7) 0.00199(7) P2 0.0186(3) 0.0217(3) 0.0211(3) -0.0023(3) 0.0025(2) 0.0018(2) P1 0.0180(3) 0.0235(3) 0.0211(3) 0.0006(3) 0.0018(2) 0.0025(3) O1 0.0231(9) 0.0212(9) 0.0247(9) -0.0005(8) 0.0001(7) 0.0016(7) O3 0.0284(10) 0.0221(10) 0.0309(10) 0.0014(8) -0.0009(8) 0.0004(8) O2 0.0470(12) 0.0318(11) 0.0239(10) 0.0014(9) 0.0037(9) -0.0002(9) O4 0.0688(15) 0.0326(12) 0.0312(12) -0.0013(10) -0.0097(11) 0.0080(11) C36 0.0234(13) 0.0279(15) 0.0303(15) 0.0005(12) 0.0040(11) 0.0012(11) C31 0.0139(11) 0.0267(14) 0.0277(14) -0.0008(11) 0.0025(10) 0.0009(10) C14 0.0205(12) 0.0238(14) 0.0318(15) -0.0020(12) 0.0020(11) -0.0006(11) C13 0.0185(12) 0.0248(14) 0.0221(13) -0.0018(11) 0.0010(10) -0.0041(10) C37 0.0218(13) 0.0264(14) 0.0268(15) -0.0008(12) -0.0001(11) 0.0037(11) C30 0.0237(13) 0.0319(15) 0.0234(14) -0.0061(12) 0.0044(11) -0.0025(11) C9 0.0265(14) 0.0456(18) 0.0264(15) -0.0078(13) -0.0009(11) 0.0010(13) C16 0.0326(15) 0.0332(16) 0.0212(14) 0.0003(12) 0.0025(11) -0.0091(12) C12 0.0298(14) 0.0291(15) 0.0266(14) -0.0022(12) 0.0023(11) -0.0024(12) C17 0.0313(15) 0.0310(15) 0.0286(15) 0.0041(12) 0.0004(12) 0.0005(12) C1 0.0279(14) 0.0337(16) 0.0262(14) 0.0068(12) 0.0088(11) 0.0098(12) C19 0.0264(13) 0.0182(13) 0.0255(14) -0.0011(11) 0.0058(11) -0.0003(10) C15 0.0330(14) 0.0306(15) 0.0276(15) -0.0089(12) 0.0082(12) -0.0049(12) C32 0.0252(14) 0.0379(17) 0.0267(15) 0.0014(12) 0.0028(11) 0.0063(12) C35 0.0289(15) 0.0263(15) 0.0467(19) -0.0034(13) 0.0022(13) 0.0053(12) C10 0.0243(14) 0.0287(15) 0.0407(17) -0.0057(13) -0.0046(12) 0.0008(12) C18 0.0271(13) 0.0248(14) 0.0259(14) -0.0013(11) 0.0039(11) 0.0014(11) C2 0.0375(16) 0.0281(16) 0.0451(18) 0.0046(14) 0.0129(14) 0.0097(13) C7 0.0174(12) 0.0257(14) 0.0283(14) -0.0021(11) 0.0027(10) 0.0022(10) C38 0.0443(17) 0.0253(15) 0.0331(16) -0.0016(13) -0.0015(13) -0.0054(13) C24 0.0290(14) 0.0284(15) 0.0286(15) 0.0016(12) 0.0049(12) 0.0041(11) C8 0.0231(13) 0.0429(18) 0.0262(14) -0.0016(13) 0.0032(11) -0.0003(12) C20 0.0267(14) 0.0387(17) 0.0296(15) 0.0020(13) 0.0043(12) -0.0037(12) C34 0.0354(16) 0.0312(16) 0.0481(19) 0.0138(14) -0.0014(14) 0.0080(13) C11 0.0313(15) 0.0298(15) 0.0352(16) 0.0025(13) 0.0032(12) -0.0036(12) C6 0.0310(16) 0.055(2) 0.0360(17) 0.0113(15) 0.0050(13) 0.0172(15) C29 0.0243(14) 0.0410(18) 0.0408(18) -0.0037(14) 0.0004(12) -0.0013(13) C22 0.0469(18) 0.0310(16) 0.0284(15) 0.0018(12) 0.0172(14) 0.0000(13) C39 0.0334(15) 0.0274(15) 0.0325(16) -0.0007(13) 0.0065(12) 0.0049(12) C28 0.0235(14) 0.055(2) 0.0406(18) -0.0076(16) -0.0031(13) -0.0023(14) C33 0.0330(15) 0.0444(18) 0.0329(16) 0.0124(14) -0.0001(13) 0.0058(14) C25 0.0325(16) 0.0349(18) 0.055(2) -0.0152(15) -0.0090(14) 0.0014(13) C27 0.0266(15) 0.057(2) 0.0421(18) -0.0195(16) 0.0040(13) -0.0095(15) C23 0.0318(15) 0.0311(16) 0.0370(17) 0.0049(13) 0.0129(13) 0.0037(12) C21 0.0432(18) 0.0439(19) 0.0227(15) 0.0005(13) 0.0010(13) -0.0052(14) C5 0.046(2) 0.076(3) 0.051(2) 0.021(2) 0.0057(17) 0.034(2) C3 0.062(2) 0.0294(17) 0.059(2) 0.0068(16) 0.0272(18) 0.0122(16) C40 0.066(2) 0.0291(18) 0.059(2) 0.0120(16) 0.0111(19) 0.0034(16) C4 0.069(3) 0.042(2) 0.067(3) 0.0256(19) 0.032(2) 0.034(2) C26 0.046(2) 0.0364(19) 0.073(3) -0.0199(18) -0.0049(18) -0.0039(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 3 -5 1 0.0563 -3 5 2 0.0667 0 1 5 0.0641 0 0 -1 0.0613 -3 4 -5 0.0700 -5 2 -2 0.0436 -4 -5 2 0.0384 5 3 -1 0.0558 5 -2 2 0.0504 -1 -1 5 0.0591 3 2 -5 0.0553 1 0 -1 0.0470 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle P1 Pd1 P2 168.25(2) O1 Pd1 P2 90.06(5) O1 Pd1 P1 84.77(5) O1 Pd1 O3 177.81(7) O3 Pd1 P2 90.89(5) O3 Pd1 P1 93.93(6) C31 P2 Pd1 109.28(8) C31 P2 C30 103.50(12) C31 P2 C19 106.34(12) C30 P2 Pd1 115.79(9) C19 P2 Pd1 117.04(9) C19 P2 C30 103.66(12) C13 P1 Pd1 106.52(8) C1 P1 Pd1 118.07(9) C1 P1 C13 105.02(12) C1 P1 C7 107.42(13) C7 P1 Pd1 113.69(9) C7 P1 C13 104.99(12) C37 O1 Pd1 113.99(17) C39 O3 Pd1 114.21(18) C31 C36 H36 119.9 C31 C36 C35 120.3(3) C35 C36 H36 119.9 C36 C31 P2 123.1(2) C36 C31 C32 119.2(3) C32 C31 P2 117.6(2) C13 C14 H14 120.2 C15 C14 H14 120.2 C15 C14 C13 119.7(3) C14 C13 P1 122.6(2) C14 C13 C18 119.3(2) C18 C13 P1 118.1(2) O1 C37 C38 113.3(2) O2 C37 O1 124.9(3) O2 C37 C38 121.8(3) C29 C30 P2 121.9(2) C29 C30 C25 118.5(3) C25 C30 P2 119.6(2) C10 C9 H9 119.6 C10 C9 C8 120.8(3) C8 C9 H9 119.6 C17 C16 H16 120.3 C17 C16 C15 119.5(3) C15 C16 H16 120.3 C7 C12 H12 119.8 C11 C12 H12 119.8 C11 C12 C7 120.4(3) C16 C17 H17 119.6 C16 C17 C18 120.8(3) C18 C17 H17 119.6 C2 C1 P1 117.6(2) C6 C1 P1 123.0(3) C6 C1 C2 119.4(3) C24 C19 P2 121.5(2) C20 C19 P2 119.2(2) C20 C19 C24 119.3(3) C14 C15 H15 119.6 C16 C15 C14 120.9(3) C16 C15 H15 119.6 C31 C32 H32 119.9 C33 C32 C31 120.2(3) C33 C32 H32 119.9 C36 C35 H35 120.1 C34 C35 C36 119.8(3) C34 C35 H35 120.1 C9 C10 H10 120.4 C9 C10 C11 119.2(3) C11 C10 H10 120.4 C13 C18 H18 120.1 C17 C18 C13 119.8(3) C17 C18 H18 120.1 C1 C2 H2 119.7 C3 C2 C1 120.6(3) C3 C2 H2 119.7 C12 C7 P1 122.5(2) C8 C7 P1 118.8(2) C8 C7 C12 118.6(3) C37 C38 H38A 109.5 C37 C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38B 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C19 C24 H24 119.8 C23 C24 C19 120.4(3) C23 C24 H24 119.8 C9 C8 C7 120.6(3) C9 C8 H8 119.7 C7 C8 H8 119.7 C19 C20 H20 120.2 C19 C20 C21 119.6(3) C21 C20 H20 120.2 C35 C34 H34 120.0 C33 C34 C35 120.1(3) C33 C34 H34 120.0 C12 C11 H11 119.7 C10 C11 C12 120.5(3) C10 C11 H11 119.7 C1 C6 H6 120.7 C1 C6 C5 118.7(4) C5 C6 H6 120.7 C30 C29 H29 119.8 C28 C29 C30 120.5(3) C28 C29 H29 119.8 C23 C22 H22 120.0 C21 C22 H22 120.0 C21 C22 C23 120.0(3) O3 C39 C40 113.2(3) O4 C39 O3 124.9(3) O4 C39 C40 121.9(3) C29 C28 H28 119.7 C27 C28 C29 120.5(3) C27 C28 H28 119.7 C32 C33 C34 120.3(3) C32 C33 H33 119.8 C34 C33 H33 119.8 C30 C25 H25 119.9 C26 C25 C30 120.3(3) C26 C25 H25 119.9 C28 C27 H27 120.2 C26 C27 C28 119.7(3) C26 C27 H27 120.2 C24 C23 H23 120.0 C22 C23 C24 120.0(3) C22 C23 H23 120.0 C20 C21 H21 119.7 C22 C21 C20 120.7(3) C22 C21 H21 119.7 C6 C5 H5 119.5 C4 C5 C6 121.1(3) C4 C5 H5 119.5 C2 C3 H3 120.1 C4 C3 C2 119.9(4) C4 C3 H3 120.1 C39 C40 H40A 109.5 C39 C40 H40B 109.5 C39 C40 H40C 109.5 H40A C40 H40B 109.5 H40A C40 H40C 109.5 H40B C40 H40C 109.5 C5 C4 C3 120.4(3) C5 C4 H4 119.8 C3 C4 H4 119.8 C25 C26 H26 119.8 C27 C26 C25 120.5(3) C27 C26 H26 119.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 P2 2.3414(6) Pd1 P1 2.3218(6) Pd1 O1 2.0249(18) Pd1 O3 2.0274(19) P2 C31 1.813(3) P2 C30 1.831(3) P2 C19 1.819(3) P1 C13 1.824(3) P1 C1 1.819(3) P1 C7 1.820(3) O1 C37 1.301(3) O3 C39 1.296(3) O2 C37 1.222(3) O4 C39 1.207(4) C36 H36 0.9300 C36 C31 1.384(4) C36 C35 1.391(4) C31 C32 1.400(4) C14 H14 0.9300 C14 C13 1.395(4) C14 C15 1.384(4) C13 C18 1.397(4) C37 C38 1.505(4) C30 C29 1.386(4) C30 C25 1.390(4) C9 H9 0.9300 C9 C10 1.378(4) C9 C8 1.384(4) C16 H16 0.9300 C16 C17 1.377(4) C16 C15 1.380(4) C12 H12 0.9300 C12 C7 1.396(4) C12 C11 1.387(4) C17 H17 0.9300 C17 C18 1.382(4) C1 C2 1.395(4) C1 C6 1.389(4) C19 C24 1.394(4) C19 C20 1.388(4) C15 H15 0.9300 C32 H32 0.9300 C32 C33 1.376(4) C35 H35 0.9300 C35 C34 1.384(4) C10 H10 0.9300 C10 C11 1.384(4) C18 H18 0.9300 C2 H2 0.9300 C2 C3 1.381(4) C7 C8 1.389(4) C38 H38A 0.9600 C38 H38B 0.9600 C38 H38C 0.9600 C24 H24 0.9300 C24 C23 1.384(4) C8 H8 0.9300 C20 H20 0.9300 C20 C21 1.392(4) C34 H34 0.9300 C34 C33 1.381(5) C11 H11 0.9300 C6 H6 0.9300 C6 C5 1.410(5) C29 H29 0.9300 C29 C28 1.385(4) C22 H22 0.9300 C22 C23 1.377(4) C22 C21 1.374(4) C39 C40 1.514(4) C28 H28 0.9300 C28 C27 1.370(5) C33 H33 0.9300 C25 H25 0.9300 C25 C26 1.389(4) C27 H27 0.9300 C27 C26 1.369(5) C23 H23 0.9300 C21 H21 0.9300 C5 H5 0.9300 C5 C4 1.356(6) C3 H3 0.9300 C3 C4 1.375(5) C40 H40A 0.9600 C40 H40B 0.9600 C40 H40C 0.9600 C4 H4 0.9300 C26 H26 0.9300 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3.0010 -5.0006 1.0068 -0.0292 0.1608 0.6373 -3.0041 5.0022 1.9905 0.1206 -0.3596 -0.5407 -0.0050 1.0025 4.9950 0.1040 -0.3879 0.0904 0.0011 -0.0005 -0.9991 -0.0305 0.0663 -0.0322 -2.9970 3.9986 -5.0027 -0.0443 0.1609 -0.6955 -5.0031 2.0020 -2.0077 0.3450 0.1123 -0.6253 -4.0083 -4.9952 1.9941 0.7051 0.2245 0.0822 5.0078 2.9954 -0.9922 -0.6784 -0.1962 0.1752 5.0031 -2.0020 2.0077 -0.3450 -0.1123 0.6253 -1.0067 -0.9964 4.9944 0.3013 -0.2563 0.1478 3.0094 1.9948 -4.9915 -0.5508 0.1626 -0.0507 1.0022 -0.0012 -0.9974 -0.1310 0.0477 0.0517