#------------------------------------------------------------------------------ #$Date: 2019-11-08 04:16:03 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225341 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/07/1550751.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_1550751 loop_ _publ_author_name 'Du, Cheng' 'Zhong, Liu' 'Gao, Jie' 'Zhong, Shuhuang' 'Liao, Heng' 'Gao, Haiyang' 'Wu, Qing' _publ_section_title ; Living (co)polymerization of ethylene and bio-based furfuryl acrylate using dibenzobarrelene derived \a-diimine palladium catalysts ; _journal_issue 16 _journal_name_full 'Polymer Chemistry' _journal_page_first 2029 _journal_paper_doi 10.1039/C9PY00126C _journal_volume 10 _journal_year 2019 _chemical_formula_moiety 'C49 H63 Cl N2 Pd' _chemical_formula_sum 'C49 H63 Cl N2 Pd' _chemical_formula_weight 821.86 _chemical_properties_physical Oxygen-sensitive _space_group_crystal_system tetragonal _space_group_IT_number 110 _space_group_name_Hall 'I 4bw -2c' _space_group_name_H-M_alt 'I 41 c d' _symmetry_space_group_name_Hall 'I 4bw -2c' _symmetry_space_group_name_H-M 'I 41 c d' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2017-06-21 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _audit_update_record ; 2019-01-22 deposited with the CCDC. 2019-03-15 downloaded from the CCDC. ; _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 16 _cell_length_a 24.7912(3) _cell_length_b 24.7912(3) _cell_length_c 31.0121(6) _cell_measurement_reflns_used 9808 _cell_measurement_temperature 149.97(10) _cell_measurement_theta_max 73.6290 _cell_measurement_theta_min 4.5520 _cell_volume 19060.1(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (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 149.97(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2913 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.975 _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 -35.00 -8.00 1.00 3.60 -- -40.84 -77.00 -30.00 27 2 \w -111.00 -72.00 1.00 3.60 -- -40.84 -77.00 -30.00 39 3 \w -113.00 -67.00 1.00 3.60 -- -40.84-140.00-121.00 46 4 \w -124.00 -82.00 1.00 3.60 -- -40.84 -86.00 -61.00 42 5 \w 60.00 153.00 1.00 14.41 -- 108.22 15.00-120.00 93 6 \w 107.00 156.00 1.00 14.41 -- 108.22 125.00-180.00 49 7 \w 108.00 170.00 1.00 14.41 -- 108.22 125.00 150.00 62 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'four-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0551454000 _diffrn_orient_matrix_UB_12 0.0003677000 _diffrn_orient_matrix_UB_13 0.0228285000 _diffrn_orient_matrix_UB_21 -0.0009203000 _diffrn_orient_matrix_UB_22 0.0621394000 _diffrn_orient_matrix_UB_23 0.0008880000 _diffrn_orient_matrix_UB_31 -0.0285417000 _diffrn_orient_matrix_UB_32 -0.0014670000 _diffrn_orient_matrix_UB_33 0.0441380000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 18906 _diffrn_reflns_point_group_measured_fraction_full 0.697 _diffrn_reflns_point_group_measured_fraction_max 0.664 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.820 _diffrn_reflns_theta_min 3.566 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.881 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.42480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.146 _exptl_crystal_description block _exptl_crystal_F_000 6944 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.339 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details ; Flack x determined using 1453 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.011(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 626 _refine_ls_number_reflns 6411 _refine_ls_number_restraints 378 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0410 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+28.0002P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.1063 _reflns_Friedel_coverage 0.336 _reflns_Friedel_fraction_full 0.382 _reflns_Friedel_fraction_max 0.341 _reflns_number_gt 5985 _reflns_number_total 6411 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL w_a.res in I4(1)cd w_sq.res created by SHELXL-2016/6 at 14:01:38 on 21-Jun-2017 CELL 1.54178 24.7912 24.7912 31.0121 90 90 90 ZERR 16 0.0002 0.0002 0.0006 0 0 0 LATT -2 SYMM -X,-Y,+Z SYMM -Y,0.5+X,0.25+Z SYMM +Y,0.5-X,0.25+Z SYMM +X,-Y,0.5+Z SYMM -X,+Y,0.5+Z SYMM +Y,0.5+X,0.75+Z SYMM -Y,0.5-X,0.75+Z SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.018 0.009 = 89.9 0.68 12.01 SFAC H SFAC Cl 11.460 0.01 7.196 1.166 6.256 18.519 1.646 47.778 -9.557 0.364 = 0.702 6240 0.99 35.45 SFAC N 12.213 0.006 3.132 9.893 2.013 28.998 1.166 0.583 -11.529 0.031 = 0.018 173 0.68 14.01 SFAC Pd 19.332 0.699 15.502 7.989 5.295 25.205 0.606 76.899 5.266 0.122 = 3.934 35200 1.5 106.4 UNIT 784 1008 16 32 16 DFIX 1.5 C12 C14 DFIX 1.5 C13 C12 C12 C14 DFIX 1.5 C12 C11 DFIX 1.5 C12A C11A DFIX 1.5 C48 C46 C46 C48A DFIX 2.4 C11A C14A RIGU N2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 RIGU Pd1 Cl1 Cl1A C49 C49A RIGU N2 C3 C4 C4A C5 C5A C6 C6A C7 C7A C8 C8A C9 C9A C10 C10A C11 C11A C12 = C12A C13 C13A C14 RIGU C45 C46 C47 C48 RIGU C45 C46 C47 C48 C48A ISOR 0.001 0.002 C49A ISOR 0.01 0.02 C48 ISOR 0.01 0.02 C9 C6 C10 C7 C3 C4 C5 C8 C11 C6A C5A C7A C8A C9A C10A C4A = C11A C12 C13 C14 C12A C13A C14A L.S. 10 0 19 PLAN -20 TEMP -123.18(10) BOND CONF ABIN fmap 2 acta OMIT 8 16 -14 OMIT 2 5 7 OMIT 11 12 -11 OMIT 10 12 -10 OMIT 11 12 -13 OMIT 11 12 -15 OMIT 12 14 -12 OMIT 4 14 -18 OMIT 11 11 -10 OMIT 12 12 -12 OMIT 3 14 -17 OMIT 10 14 -10 REM REM REM WGHT 0.058600 28.000200 FVAR 0.08159 0.74479 0.62284 0.44655 PD1 5 0.382613 0.230398 0.177935 11.00000 0.04028 0.02927 = 0.07081 0.00762 0.01418 0.01084 PART 1 CL1 3 0.418855 0.264241 0.116262 21.00000 0.07853 0.06631 = 0.09847 0.03633 0.04909 0.03162 PART 0 PART 2 CL1A 3 0.334207 0.306471 0.171632 -21.00000 0.04876 0.04329 = 0.08800 0.02616 0.01794 0.03319 PART 0 N1 4 0.352421 0.196245 0.235368 11.00000 0.02617 0.02994 = 0.05533 -0.00403 0.00256 0.00789 N2 4 0.431635 0.159351 0.184097 11.00000 0.03718 0.02995 = 0.07412 0.00253 0.01704 0.00562 C1 1 0.373891 0.150418 0.244594 11.00000 0.02337 0.02685 = 0.06275 -0.00570 -0.00286 0.00152 C2 1 0.418833 0.131231 0.217298 11.00000 0.02730 0.03145 = 0.06141 -0.00465 0.00519 0.00308 C3 1 0.476061 0.143137 0.157202 11.00000 0.05700 0.04690 = 0.09286 0.01469 0.03289 0.02209 PART 1 C4 1 0.529791 0.165080 0.171910 31.00000 0.04719 0.06324 = 0.07828 0.02623 0.01566 0.01963 PART 0 PART 2 C4A 1 0.521215 0.158404 0.153541 -31.00000 0.05459 0.05204 = 0.06520 0.02535 0.02732 0.01492 PART 0 PART 1 C5 1 0.535655 0.207419 0.206309 31.00000 0.06230 0.09862 = 0.11565 -0.00419 0.01345 -0.01401 AFIX 13 H5 2 0.500811 0.208037 0.222545 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C5A 1 0.537111 0.194419 0.187475 -31.00000 0.04462 0.07680 = 0.07863 0.00441 0.01740 0.01425 AFIX 13 H5A 2 0.507769 0.202266 0.208694 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C6 1 0.541405 0.258728 0.187274 31.00000 0.10616 0.08393 = 0.15778 0.01115 -0.01094 0.04061 AFIX 137 H6A 2 0.528596 0.286426 0.207360 31.00000 -1.50000 H6B 2 0.520125 0.260270 0.160671 31.00000 -1.50000 H6C 2 0.579492 0.265161 0.180555 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C6A 1 0.563065 0.250404 0.163531 -31.00000 0.15982 0.08458 = 0.16401 0.03414 0.03148 -0.02032 AFIX 137 H6AA 2 0.540735 0.260265 0.138675 -31.00000 -1.50000 H6AB 2 0.599957 0.242973 0.153859 -31.00000 -1.50000 H6AC 2 0.563460 0.280238 0.184260 -31.00000 -1.50000 AFIX 0 PART 0 PART 1 C7 1 0.577836 0.192992 0.237689 31.00000 0.14369 0.09672 = 0.12094 0.03629 -0.02711 -0.04962 AFIX 137 H7A 2 0.613181 0.193992 0.223560 31.00000 -1.50000 H7B 2 0.571054 0.156594 0.248760 31.00000 -1.50000 H7C 2 0.577345 0.218790 0.261629 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C7A 1 0.589415 0.177170 0.207970 -31.00000 0.06585 0.09290 = 0.15441 0.02110 -0.01268 0.00567 AFIX 137 H7AA 2 0.601333 0.143062 0.195148 -31.00000 -1.50000 H7AB 2 0.584063 0.172296 0.239036 -31.00000 -1.50000 H7AC 2 0.616883 0.204927 0.203062 -31.00000 -1.50000 AFIX 0 PART 0 PART 1 C8 1 0.573474 0.147406 0.146419 31.00000 0.05167 0.07440 = 0.09361 0.02389 0.02102 0.01411 AFIX 43 H8 2 0.609154 0.159006 0.152654 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C8A 1 0.560135 0.136883 0.124819 -31.00000 0.07112 0.07096 = 0.08125 -0.00380 0.03067 0.00164 AFIX 43 H8A 2 0.597689 0.142260 0.129141 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C9 1 0.563715 0.113145 0.112406 31.00000 0.08706 0.10195 = 0.10385 -0.00156 0.02953 0.02251 AFIX 43 H9 2 0.592898 0.105186 0.093600 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C9A 1 0.539711 0.106266 0.088533 -31.00000 0.09804 0.08145 = 0.08885 -0.00045 0.01740 0.00312 AFIX 43 H9A 2 0.565576 0.095634 0.067589 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C10 1 0.514986 0.089761 0.103780 31.00000 0.11107 0.10244 = 0.10891 -0.02884 0.02354 0.02159 AFIX 43 H10 2 0.513067 0.063782 0.081313 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C10A 1 0.490079 0.091574 0.081206 -31.00000 0.09566 0.08084 = 0.09912 -0.01305 0.00579 0.01512 AFIX 43 H10A 2 0.477755 0.068999 0.058498 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C11 1 0.465021 0.102930 0.127735 31.00000 0.11882 0.08871 = 0.09825 -0.02200 0.03839 0.02670 PART 0 PART 2 C11A 1 0.459488 0.114776 0.112289 -31.00000 0.10283 0.08262 = 0.09643 -0.00505 0.02021 0.02238 PART 0 PART 1 C12 1 0.408167 0.099563 0.105747 31.00000 0.15069 0.12991 = 0.12684 -0.04939 0.00588 0.01383 AFIX 13 H12 2 0.383156 0.117500 0.126590 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C12A 1 0.412523 0.077672 0.122798 -31.00000 0.10843 0.07845 = 0.06626 0.00327 -0.00066 0.01011 AFIX 13 H12A 2 0.404607 0.076232 0.154395 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C13 1 0.387258 0.041222 0.102393 31.00000 0.16833 0.13803 = 0.13979 0.01137 -0.01529 0.00092 AFIX 137 H13A 2 0.394850 0.022047 0.129352 31.00000 -1.50000 H13B 2 0.405361 0.022859 0.078442 31.00000 -1.50000 H13C 2 0.348257 0.041633 0.097252 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C13A 1 0.418619 0.022818 0.103372 -31.00000 0.13699 0.10164 = 0.09118 -0.03608 0.00577 -0.00962 AFIX 137 H13D 2 0.437894 0.025709 0.075880 -31.00000 -1.50000 H13E 2 0.382879 0.007109 0.098412 -31.00000 -1.50000 H13F 2 0.439081 -0.000321 0.123092 -31.00000 -1.50000 AFIX 0 PART 0 PART 1 C14 1 0.395465 0.125206 0.062942 31.00000 0.21690 0.13891 = 0.19580 0.00481 -0.02196 0.03052 AFIX 137 H14A 2 0.361914 0.109949 0.051520 31.00000 -1.50000 H14B 2 0.424985 0.118145 0.042697 31.00000 -1.50000 H14C 2 0.391227 0.164220 0.066738 31.00000 -1.50000 AFIX 0 PART 0 PART 2 C14A 1 0.365918 0.116961 0.094501 -31.00000 0.14550 0.12410 = 0.09135 0.02713 -0.00464 -0.00391 AFIX 3 H14D 2 0.376649 0.154151 0.095641 -31.00000 -1.50000 H14E 2 0.330918 0.113001 0.107341 -31.00000 -1.50000 H14F 2 0.364629 0.105311 0.065001 -31.00000 -1.50000 AFIX 0 PART 0 C15 1 0.443199 0.079198 0.234195 11.00000 0.03088 0.02790 = 0.06579 -0.00264 0.00436 0.00766 AFIX 13 H15 2 0.474081 0.065895 0.216385 11.00000 -1.20000 AFIX 0 C16 1 0.458793 0.091068 0.281157 11.00000 0.03019 0.02684 = 0.07181 -0.00513 -0.00266 0.00343 C17 1 0.415264 0.108544 0.306318 11.00000 0.03022 0.02505 = 0.06279 -0.00582 -0.00402 0.00210 C18 1 0.362251 0.113028 0.281699 11.00000 0.02569 0.02607 = 0.05990 0.00060 0.00166 0.00130 AFIX 13 H18 2 0.331388 0.125160 0.300056 11.00000 -1.20000 AFIX 0 C19 1 0.353002 0.057788 0.260619 11.00000 0.03365 0.02573 = 0.05672 0.00211 -0.00707 -0.00107 C20 1 0.396296 0.040378 0.235514 11.00000 0.04101 0.02317 = 0.06075 -0.00113 -0.00468 0.00354 C21 1 0.393542 -0.009774 0.215224 11.00000 0.06894 0.02875 = 0.05579 -0.00394 -0.00559 0.00611 AFIX 43 H21 2 0.422686 -0.021947 0.197877 11.00000 -1.20000 AFIX 0 C22 1 0.348522 -0.041550 0.220398 11.00000 0.08743 0.03259 = 0.06153 -0.00596 0.00021 -0.01024 AFIX 43 H22 2 0.347096 -0.075689 0.206530 11.00000 -1.20000 AFIX 0 C23 1 0.305179 -0.024993 0.245349 11.00000 0.05972 0.03935 = 0.05899 -0.00004 -0.01305 -0.01421 C24 1 0.307743 0.025983 0.265899 11.00000 0.04414 0.03408 = 0.05628 0.00434 -0.01057 -0.00761 AFIX 43 H24 2 0.278552 0.038194 0.283179 11.00000 -1.20000 AFIX 0 C25 1 0.255608 -0.060558 0.252707 11.00000 0.06963 0.04711 = 0.08592 0.00222 -0.00679 -0.02598 C26 1 0.209850 -0.037264 0.227852 11.00000 0.06919 0.09729 = 0.25688 0.06005 -0.06448 -0.03684 AFIX 137 H26A 2 0.201376 -0.001277 0.239038 11.00000 -1.50000 H26B 2 0.178174 -0.060626 0.230791 11.00000 -1.50000 H26C 2 0.219865 -0.034548 0.197360 11.00000 -1.50000 AFIX 0 C27 1 0.244830 -0.065749 0.301064 11.00000 0.09579 0.07838 = 0.10409 -0.00838 0.01770 -0.04798 AFIX 137 H27A 2 0.232340 -0.031030 0.312404 11.00000 -1.50000 H27B 2 0.278151 -0.076308 0.315824 11.00000 -1.50000 H27C 2 0.217090 -0.093236 0.305965 11.00000 -1.50000 AFIX 0 C28 1 0.265736 -0.118714 0.236587 11.00000 0.10809 0.05898 = 0.12508 -0.01231 -0.01016 -0.04178 AFIX 137 H28A 2 0.233222 -0.140473 0.241110 11.00000 -1.50000 H28B 2 0.295862 -0.134569 0.252650 11.00000 -1.50000 H28C 2 0.274544 -0.117955 0.205787 11.00000 -1.50000 AFIX 0 C29 1 0.422705 0.119631 0.349531 11.00000 0.03352 0.03144 = 0.07174 -0.00471 -0.00261 0.00253 AFIX 43 H29 2 0.393592 0.132042 0.366803 11.00000 -1.20000 AFIX 0 C30 1 0.474134 0.112193 0.367410 11.00000 0.04038 0.04348 = 0.06995 -0.01595 -0.01216 0.00975 AFIX 43 H30 2 0.479425 0.119572 0.397171 11.00000 -1.20000 AFIX 0 C31 1 0.517663 0.094342 0.342922 11.00000 0.03743 0.04203 = 0.09091 -0.01838 -0.01372 0.00730 C32 1 0.509143 0.083746 0.299037 11.00000 0.02901 0.04231 = 0.07971 -0.01414 -0.00560 0.00904 AFIX 43 H32 2 0.538156 0.071488 0.281587 11.00000 -1.20000 AFIX 0 C33 1 0.574239 0.086266 0.361720 11.00000 0.03811 0.06613 = 0.12019 -0.04057 -0.02553 0.00904 C34 1 0.595190 0.030846 0.350199 11.00000 0.05208 0.06573 = 0.10827 -0.02083 -0.03372 0.02574 AFIX 137 H34A 2 0.631599 0.026289 0.361954 11.00000 -1.50000 H34B 2 0.596283 0.026989 0.318761 11.00000 -1.50000 H34C 2 0.571269 0.003333 0.362413 11.00000 -1.50000 AFIX 0 C35 1 0.574416 0.093890 0.410227 11.00000 0.07649 0.18226 = 0.14297 -0.08026 -0.06049 0.05726 AFIX 137 H35A 2 0.554957 0.064024 0.423888 11.00000 -1.50000 H35B 2 0.556695 0.128049 0.417453 11.00000 -1.50000 H35C 2 0.611709 0.094524 0.420693 11.00000 -1.50000 AFIX 0 C36 1 0.612514 0.128270 0.344201 11.00000 0.05497 0.08365 = 0.29999 -0.00993 -0.05734 -0.01592 AFIX 137 H36A 2 0.649021 0.121073 0.354870 11.00000 -1.50000 H36B 2 0.600954 0.164138 0.353742 11.00000 -1.50000 H36C 2 0.612411 0.126859 0.312620 11.00000 -1.50000 AFIX 0 C37 1 0.311016 0.218273 0.262624 11.00000 0.04018 0.02928 = 0.06237 0.00578 0.01714 0.01368 C38 1 0.326219 0.247241 0.298669 11.00000 0.06768 0.03839 = 0.06732 0.00500 0.01324 0.01703 C39 1 0.384879 0.257967 0.309243 11.00000 0.08741 0.04430 = 0.08397 -0.01657 -0.00045 -0.00529 AFIX 13 H39 2 0.405968 0.225673 0.299805 11.00000 -1.20000 AFIX 0 C40 1 0.395357 0.265737 0.356723 11.00000 0.13509 0.04998 = 0.10064 0.00004 -0.02837 -0.01529 AFIX 137 H40A 2 0.376116 0.297854 0.366863 11.00000 -1.50000 H40B 2 0.434147 0.270372 0.361553 11.00000 -1.50000 H40C 2 0.382620 0.234035 0.372620 11.00000 -1.50000 AFIX 0 C41 1 0.405810 0.306132 0.283807 11.00000 0.12812 0.09491 = 0.09572 0.00170 -0.01299 -0.03763 AFIX 137 H41A 2 0.402865 0.298643 0.252868 11.00000 -1.50000 H41B 2 0.443671 0.312635 0.291257 11.00000 -1.50000 H41C 2 0.384367 0.338127 0.290920 11.00000 -1.50000 AFIX 0 C42 1 0.283510 0.268756 0.323663 11.00000 0.11146 0.07298 = 0.07236 -0.00824 0.02863 0.03807 AFIX 43 H42 2 0.291435 0.289471 0.348644 11.00000 -1.20000 AFIX 0 C43 1 0.230792 0.259963 0.312136 11.00000 0.08396 0.10936 = 0.08249 0.01268 0.02521 0.05830 AFIX 43 H43 2 0.202864 0.273508 0.330101 11.00000 -1.20000 AFIX 0 C44 1 0.217285 0.232319 0.275607 11.00000 0.04916 0.09401 = 0.11526 0.02425 0.02865 0.03514 AFIX 43 H44 2 0.180458 0.227601 0.268027 11.00000 -1.20000 AFIX 0 C45 1 0.257318 0.211329 0.249830 11.00000 0.03556 0.07117 = 0.09865 0.01672 0.01659 0.01802 C46 1 0.241798 0.185034 0.205857 11.00000 0.03657 0.09588 = 0.18217 -0.03209 -0.00196 0.00680 PART 1 AFIX 13 H46 2 0.273403 0.175038 0.187484 41.00000 -1.20000 AFIX 13 PART 0 PART 2 H46A 2 0.274434 0.191054 0.187528 -41.00000 -1.20000 AFIX 0 PART 0 C47 1 0.197170 0.214930 0.181716 11.00000 0.08928 0.11213 = 0.12172 0.02312 -0.01444 0.00870 AFIX 137 H47A 2 0.163001 0.210704 0.197244 11.00000 -1.50000 H47B 2 0.193573 0.199949 0.152615 11.00000 -1.50000 H47C 2 0.206308 0.253315 0.179805 11.00000 -1.50000 AFIX 0 PART 1 C48 1 0.211365 0.134255 0.227307 41.00000 0.14183 0.10724 = 0.13760 0.01694 -0.06215 -0.00004 AFIX 3 H48A 2 0.236525 0.114035 0.244397 41.00000 -1.50000 H48B 2 0.196725 0.111475 0.205177 41.00000 -1.50000 H48C 2 0.182685 0.147155 0.245367 41.00000 -1.50000 AFIX 0 PART 0 PART 2 C48A 1 0.235066 0.125424 0.205514 -41.00000 0.07490 0.08576 = 0.09636 0.00592 -0.00119 0.01798 AFIX 137 H48D 2 0.269569 0.108204 0.212467 -41.00000 -1.50000 H48E 2 0.223188 0.113763 0.176851 -41.00000 -1.50000 H48F 2 0.208005 0.115026 0.226997 -41.00000 -1.50000 AFIX 0 PART 0 PART 1 C49 1 0.333782 0.294739 0.180074 21.00000 0.09606 0.06552 = 0.04814 0.02362 0.01012 0.04487 AFIX 137 H49A 2 0.355231 0.327727 0.177040 21.00000 -1.50000 H49B 2 0.314677 0.295352 0.207735 21.00000 -1.50000 H49C 2 0.307553 0.292610 0.156494 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C49A 1 0.409996 0.253358 0.121184 -21.00000 0.05312 0.05365 = 0.05368 -0.00040 -0.00027 0.00037 AFIX 137 H49D 2 0.384866 0.241722 0.098634 -21.00000 -1.50000 H49E 2 0.445429 0.237030 0.116095 -21.00000 -1.50000 H49F 2 0.413312 0.292742 0.120596 -21.00000 -1.50000 AFIX 0 HKLF 4 REM w_a.res in I4(1)cd REM R1 = 0.0410 for 5985 Fo > 4sig(Fo) and 0.0470 for all 6411 data REM 626 parameters refined using 378 restraints END WGHT 0.0586 28.0006 REM Highest difference peak 0.339, deepest hole -0.490, 1-sigma level 0.053 Q1 1 0.3787 0.2514 0.1359 11.00000 0.05 0.34 Q2 1 0.3979 0.2908 0.1783 11.00000 0.05 0.32 Q3 1 0.4442 0.2119 0.1788 11.00000 0.05 0.31 Q4 1 0.3352 0.1999 0.1786 11.00000 0.05 0.31 Q5 1 0.3821 0.2128 0.2232 11.00000 0.05 0.29 Q6 1 0.3806 0.2513 0.2179 11.00000 0.05 0.29 Q7 1 0.2458 0.1577 0.2257 11.00000 0.05 0.27 Q8 1 0.3394 0.2409 0.3796 11.00000 0.05 0.26 Q9 1 0.3397 0.2629 0.1786 11.00000 0.05 0.26 Q10 1 0.3779 0.0876 0.1159 11.00000 0.05 0.26 Q11 1 0.2824 0.1006 0.1450 11.00000 0.05 0.26 Q12 1 0.3816 0.2110 0.1312 11.00000 0.05 0.25 Q13 1 0.3179 0.2168 0.1705 11.00000 0.05 0.25 Q14 1 0.2350 0.1709 0.1707 11.00000 0.05 0.25 Q15 1 0.1909 0.1225 0.2391 11.00000 0.05 0.24 Q16 1 0.3569 0.1781 0.1779 11.00000 0.05 0.24 Q17 1 0.3783 0.2067 0.1436 11.00000 0.05 0.24 Q18 1 0.4606 0.2300 0.1911 11.00000 0.05 0.24 Q19 1 0.4222 0.0629 0.2279 11.00000 0.05 0.22 Q20 1 0.3959 0.1126 0.0902 11.00000 0.05 0.21 REM The information below was added by Olex2. REM REM R1 = 0.0410 for 5985 Fo > 4sig(Fo) and 0.0470 for all 18906 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.49 REM Mean Shift 0, Max Shift -0.018. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0470 REM R1_gt = 0.0410 REM wR_ref = n/a REM GOOF = n/a REM Shift_max = -0.018 REM Shift_mean = 0 REM Reflections_all = 18906 REM Reflections_gt = 5985 REM Parameters = n/a REM Hole = -0.49 REM Peak = 0.34 REM Flack = -0.011(6) ; _cod_data_source_file c9py00126c2.cif _cod_data_source_block w_sq _cod_depositor_comments 'Adding full bibliography for 1550751--1550752.cif.' _cod_original_cell_volume 19060.2(5) _cod_database_code 1550751 _chemical_oxdiff_formula CHNClPd _chemical_oxdiff_usercomment C2a _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. ; _symmetry_space_group_name_h-m_alt 'I 41 c d' _cell_oxdiff_angle_alpha 89.980(2) _cell_oxdiff_angle_beta 89.964(2) _cell_oxdiff_angle_gamma 90.073(2) _cell_oxdiff_length_a 24.8077(7) _cell_oxdiff_length_b 24.7848(5) _cell_oxdiff_length_c 30.9996(10) _cell_oxdiff_measurement_reflns_used 9807 _cell_oxdiff_volume 19060.2(9) _reflns_odcompleteness_completeness 99.83 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 C12-C14 1.5 with sigma of 0.02 C13-C12 = C12-C14 1.5 with sigma of 0.02 C12-C11 1.5 with sigma of 0.02 C12A-C11A 1.5 with sigma of 0.02 C48-C46 = C46-C48A 1.5 with sigma of 0.02 C11A-C14A 2.4 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C49A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains N2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 Pd1, Cl1, Cl1A, C49, C49A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N2, C3, C4, C4A, C5, C5A, C6, C6A, C7, C7A, C8, C8A, C9, C9A, C10, C10A, C11, C11A, C12, C12A, C13, C13A, C14 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C45, C46, C47, C48 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C45, C46, C47, C48, C48A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(Cl1A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(1) Sof(Cl1)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(1) Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)= Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)= Sof(H10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)= Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2) Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)= Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)= Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)= Sof(H14B)=Sof(H14C)=FVAR(2) Sof(H46A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(3) Sof(H46)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(3) 6.a Riding coordinates: C14A(H14D,H14E,H14F), C48(H48A,H48B,H48C) 6.b Ternary CH refined with riding coordinates: C5(H5), C5A(H5A), C12(H12), C12A(H12A), C15(H15), C18(H18), C39(H39), C46(H46), C46(H46A) 6.c Aromatic/amide H refined with riding coordinates: C8(H8), C8A(H8A), C9(H9), C9A(H9A), C10(H10), C10A(H10A), C21(H21), C22(H22), C24(H24), C29(H29), C30(H30), C32(H32), C42(H42), C43(H43), C44(H44) 6.d Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C26(H26A,H26B, H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C35(H35A, H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C48A(H48D,H48E,H48F), C49(H49A,H49B,H49C), C49A(H49D,H49E, H49F) ; _shelx_fab_checksum 42750 _shelx_fab_file ; 1 1 26 2.74 4.48 0 2 26 -1.56 -3.22 1 3 26 1.15 1.19 3 3 26 0.58 -0.69 0 4 26 -2.51 -2.97 2 4 26 -0.84 -1.19 1 2 25 -0.27 1.10 2 3 25 1.23 -1.65 1 4 25 0.91 1.61 3 4 25 0.45 -2.30 2 5 25 0.79 -0.91 4 5 25 1.86 0.83 1 6 25 0.95 1.33 3 6 25 0.81 -2.67 2 7 25 0.32 -1.01 0 0 24 -7.08 -8.38 0 2 24 -2.37 -4.20 2 2 24 0.06 -1.41 1 3 24 1.88 3.65 0 4 24 -0.99 -1.17 2 4 24 -0.83 -0.53 4 4 24 -0.59 -0.77 1 5 24 1.44 2.54 3 5 24 0.89 0.74 0 6 24 3.34 0.22 2 6 24 1.05 -0.89 4 6 24 0.52 -1.28 6 6 24 -2.68 -1.83 1 7 24 2.38 0.07 3 7 24 0.83 0.01 5 7 24 -0.82 -0.06 2 8 24 0.74 0.62 4 8 24 1.77 0.07 1 2 23 1.26 0.39 2 3 23 -0.28 1.10 1 4 23 1.39 1.20 3 4 23 -3.07 0.46 2 5 23 -1.65 -0.69 4 5 23 -1.30 1.72 1 6 23 0.89 1.11 3 6 23 -2.90 -0.32 5 6 23 -3.17 -0.66 2 7 23 -1.50 0.28 4 7 23 -1.84 3.81 6 7 23 0.06 6.15 1 8 23 0.73 1.64 3 8 23 0.73 0.08 5 8 23 -0.45 -0.10 4 9 23 -1.80 -0.03 1 1 22 2.55 6.03 0 2 22 -3.10 -0.62 1 3 22 1.64 2.74 3 3 22 2.16 1.41 0 4 22 0.07 -5.84 2 4 22 0.06 -2.84 1 5 22 -0.06 -0.10 3 5 22 0.63 1.14 5 5 22 -0.99 4.62 0 6 22 -1.82 -1.33 2 6 22 -3.18 1.58 4 6 22 0.20 -0.49 1 7 22 -1.16 1.41 3 7 22 -0.16 1.18 5 7 22 0.20 3.48 7 7 22 3.34 1.48 0 8 22 -0.52 -2.81 2 8 22 -1.86 0.23 4 8 22 2.56 -2.27 6 8 22 0.41 -1.11 3 9 22 -1.85 -3.63 5 9 22 -1.14 -0.02 7 9 22 1.91 0.85 6 10 22 -1.23 0.78 1 2 21 0.20 -0.89 2 3 21 -1.23 -0.82 1 4 21 0.62 -0.43 3 4 21 -0.01 2.38 2 5 21 2.44 -1.23 4 5 21 3.60 1.31 1 6 21 2.00 -0.02 3 6 21 2.63 -0.48 5 6 21 4.11 -7.43 2 7 21 0.41 -3.80 4 7 21 0.59 -1.15 6 7 21 4.63 -0.02 1 8 21 1.00 2.26 3 8 21 -0.02 -0.05 5 8 21 1.35 -4.93 7 8 21 -2.06 -4.11 2 9 21 -0.10 -1.75 4 9 21 -0.41 2.73 6 9 21 2.18 3.01 8 9 21 2.33 1.25 5 10 21 1.83 0.84 7 10 21 -1.43 0.24 6 11 21 -0.05 2.46 0 0 20 -0.25 -2.88 0 2 20 -2.45 -5.36 2 2 20 -2.99 -6.43 1 3 20 -0.62 3.08 0 4 20 -2.04 0.19 2 4 20 -0.88 -0.79 4 4 20 0.54 -2.69 1 5 20 3.52 1.84 3 5 20 1.60 -0.74 0 6 20 -2.26 -5.66 2 6 20 0.45 -3.17 4 6 20 0.87 -5.28 6 6 20 -0.19 -3.31 1 7 20 1.69 -1.17 3 7 20 -1.35 -1.76 5 7 20 -1.89 0.66 0 8 20 -1.12 1.07 2 8 20 2.00 4.29 4 8 20 1.60 -0.27 6 8 20 -1.02 -0.44 8 8 20 -2.71 -2.74 1 9 20 2.92 5.93 3 9 20 -0.91 2.76 5 9 20 -1.74 1.40 7 9 20 0.19 0.16 4 10 20 1.83 3.05 6 10 20 -1.09 1.26 7 11 20 1.01 -2.08 1 2 19 -0.45 0.81 2 3 19 3.26 -4.08 1 4 19 -2.61 0.46 3 4 19 0.29 1.93 2 5 19 -1.05 -2.81 4 5 19 -6.06 3.31 1 6 19 -3.44 2.50 3 6 19 -3.53 5.28 5 6 19 -6.62 -3.19 2 7 19 0.67 -3.12 4 7 19 -3.02 3.53 6 7 19 -1.78 7.75 1 8 19 -1.13 1.58 3 8 19 -2.09 2.21 5 8 19 -1.81 -4.14 7 8 19 -3.93 -1.92 2 9 19 0.24 -4.30 4 9 19 -1.83 0.04 6 9 19 -1.11 3.57 8 9 19 1.22 0.69 3 10 19 -2.03 -0.09 5 10 19 0.81 -4.89 7 10 19 -1.72 -3.88 1 1 18 2.16 7.37 0 2 18 4.03 -2.29 1 3 18 3.20 2.54 3 3 18 1.20 0.08 0 4 18 -5.25 -3.00 2 4 18 -5.20 -1.43 1 5 18 -0.76 6.40 3 5 18 -3.24 4.01 5 5 18 -4.72 4.27 0 6 18 -3.61 1.55 2 6 18 -1.08 1.47 4 6 18 0.58 1.39 1 7 18 1.64 1.99 3 7 18 -0.51 0.72 5 7 18 -0.10 1.07 7 7 18 4.31 1.94 0 8 18 -4.45 -2.92 2 8 18 0.20 -1.89 4 8 18 1.72 1.27 6 8 18 3.40 2.73 1 9 18 -0.21 -6.57 3 9 18 -1.55 -6.60 5 9 18 -0.02 -3.54 7 9 18 3.66 2.19 4 10 18 0.72 -1.96 6 10 18 -0.40 0.92 8 10 18 -3.66 -0.72 5 11 18 -0.53 -2.68 0 14 18 -2.71 -2.07 4 14 18 1.43 1.81 6 14 18 -0.58 2.46 1 15 18 1.34 5.30 3 15 18 -1.77 0.66 1 2 17 -3.97 1.87 2 3 17 0.63 -4.35 1 4 17 -3.60 3.78 3 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0.40 0.33 3 4 29 0.79 -1.83 2 5 29 0.59 0.06 4 5 29 1.42 0.18 1 6 29 -0.09 0.43 3 6 29 1.20 -1.53 5 6 29 -0.01 -1.34 2 7 29 0.72 -0.63 4 7 29 0.92 -1.11 6 7 29 0.87 -1.31 1 8 29 -0.61 -0.21 3 8 29 1.23 -2.99 5 8 29 -0.06 -3.67 7 8 29 -1.18 -2.24 2 9 29 0.50 -0.73 4 9 29 0.17 -1.20 6 9 29 1.09 -1.50 8 9 29 1.89 -1.18 1 10 29 -0.38 0.97 3 10 29 1.66 -0.41 5 10 29 1.20 -0.85 7 10 29 0.42 1.19 9 10 29 1.29 1.23 2 11 29 1.53 0.33 4 11 29 0.92 1.43 6 11 29 1.20 1.41 8 11 29 0.57 0.56 10 11 29 -1.66 1.44 1 12 29 -0.29 1.76 3 12 29 0.49 1.17 5 12 29 0.53 -0.06 7 12 29 -0.01 0.86 9 12 29 1.72 0.24 11 12 29 1.53 -0.01 2 13 29 -0.24 -0.31 4 13 29 -1.75 0.90 6 13 29 -1.73 0.61 8 13 29 -1.32 -0.69 10 13 29 -1.23 -0.28 12 13 29 0.49 0.70 1 14 29 -0.94 1.54 3 14 29 -2.61 1.13 5 14 29 -2.57 -0.08 7 14 29 -2.04 0.98 9 14 29 -0.01 1.14 11 14 29 0.16 0.79 13 14 29 -0.11 0.49 2 15 29 -0.19 -0.92 4 15 29 -0.85 0.46 6 15 29 -1.61 1.19 8 15 29 -1.03 0.80 10 15 29 -0.25 0.60 12 15 29 0.88 1.00 1 16 29 0.40 1.25 3 16 29 -0.03 1.89 5 16 29 0.17 0.59 7 16 29 0.66 0.88 9 16 29 0.61 0.81 11 16 29 0.80 0.28 2 17 29 0.33 -0.80 4 17 29 1.08 0.11 6 17 29 -0.26 0.73 8 17 29 -0.17 0.63 10 17 29 0.07 0.37 1 18 29 0.41 -0.04 3 18 29 -0.39 0.23 5 18 29 -0.72 -0.86 7 18 29 0.36 -0.19 9 18 29 -0.42 0.33 2 19 29 -0.23 -1.23 4 19 29 1.13 -0.94 6 19 29 0.22 0.02 1 20 29 0.63 -0.33 3 20 29 0.45 0.02 1 1 30 2.20 3.68 0 2 30 -0.51 -3.22 1 3 30 -0.35 1.16 3 3 30 -1.53 0.63 0 4 30 -0.86 -0.87 2 4 30 -1.01 0.53 1 5 30 -0.80 -1.42 3 5 30 -0.98 -0.16 5 5 30 -0.83 -0.11 0 6 30 0.29 -1.95 2 6 30 -0.30 -1.40 4 6 30 -0.13 -0.87 1 7 30 -2.00 -3.32 3 7 30 -1.21 -0.70 5 7 30 -1.35 0.00 7 7 30 -1.93 0.71 0 8 30 1.12 0.98 2 8 30 0.78 0.43 4 8 30 0.38 -0.81 6 8 30 1.52 -0.49 1 9 30 -1.15 -1.62 3 9 30 -0.15 0.41 5 9 30 -0.48 0.24 7 9 30 -1.14 0.43 9 9 30 -1.15 0.20 0 10 30 -0.44 0.50 2 10 30 0.10 0.36 4 10 30 -0.19 -0.67 6 10 30 1.91 0.62 8 10 30 0.78 0.80 1 11 30 -2.59 -3.73 3 11 30 -1.68 -1.25 5 11 30 -1.14 0.03 7 11 30 -0.64 0.72 9 11 30 -0.48 0.79 11 11 30 -0.07 0.67 0 12 30 -1.70 -0.47 2 12 30 -0.72 -0.28 4 12 30 -0.85 -0.72 6 12 30 1.77 1.01 8 12 30 2.22 1.48 10 12 30 2.30 0.63 1 13 30 -1.08 -2.27 3 13 30 -0.72 -0.35 5 13 30 -0.09 1.15 7 13 30 0.11 1.14 9 13 30 -0.14 0.93 11 13 30 -0.32 0.30 13 13 30 -0.57 -0.47 0 14 30 0.89 0.51 2 14 30 1.31 0.34 4 14 30 0.30 0.25 6 14 30 1.22 0.91 8 14 30 1.73 1.30 10 14 30 1.82 0.22 12 14 30 0.61 0.50 1 15 30 1.41 -0.06 3 15 30 0.94 0.48 5 15 30 0.56 0.73 7 15 30 -0.32 -0.07 9 15 30 -0.40 0.03 11 15 30 -0.22 0.47 0 16 30 1.31 1.36 2 16 30 1.00 0.37 4 16 30 -0.07 -0.14 6 16 30 0.37 -0.73 8 16 30 1.65 -0.22 10 16 30 1.81 -0.94 1 17 30 -0.90 0.72 3 17 30 -0.22 1.00 5 17 30 0.33 0.56 7 17 30 -0.28 -0.46 9 17 30 -0.34 -0.70 0 18 30 -0.16 0.34 2 18 30 -0.76 -0.40 4 18 30 -0.95 0.07 6 18 30 -0.41 -0.13 1 19 30 0.22 0.02 3 19 30 0.69 0.75 1 2 31 -0.67 0.88 2 3 31 -1.16 0.14 1 4 31 -2.04 1.24 3 4 31 -2.32 -1.19 2 5 31 -0.48 0.46 4 5 31 -0.43 3.23 1 6 31 -1.20 0.99 3 6 31 0.13 -0.48 5 6 31 -0.58 -0.44 2 7 31 0.03 0.03 4 7 31 0.65 2.39 6 7 31 0.88 0.79 1 8 31 -0.91 0.89 3 8 31 0.43 1.10 5 8 31 -0.45 0.85 7 8 31 -0.96 1.93 2 9 31 0.01 0.33 4 9 31 0.51 2.48 6 9 31 -0.09 1.81 8 9 31 -0.24 1.15 1 10 31 -0.54 0.94 3 10 31 0.80 1.27 5 10 31 0.33 0.59 7 10 31 0.17 0.83 9 10 31 0.43 -1.07 2 11 31 -0.79 -0.86 4 11 31 -0.05 0.49 6 11 31 0.01 0.60 8 11 31 -0.51 0.13 10 11 31 -1.34 -0.30 1 12 31 -0.46 0.75 3 12 31 0.17 -0.57 5 12 31 -0.19 -1.47 7 12 31 -0.09 -1.36 9 12 31 0.31 -1.53 11 12 31 -0.39 -1.89 2 13 31 0.02 -1.73 4 13 31 1.05 -0.65 6 13 31 0.77 -0.26 8 13 31 -0.46 -0.46 10 13 31 -0.67 -0.29 12 13 31 -1.04 0.20 1 14 31 0.20 1.26 3 14 31 0.87 -0.08 5 14 31 0.99 -0.60 7 14 31 1.14 -0.58 9 14 31 1.08 0.06 11 14 31 -0.05 -0.40 2 15 31 -0.21 -1.69 4 15 31 0.97 -0.60 6 15 31 1.20 -0.57 8 15 31 0.32 -0.53 10 15 31 0.28 -0.23 1 16 31 0.35 0.81 3 16 31 0.06 -0.65 5 16 31 0.01 -1.37 7 16 31 0.08 -1.31 2 17 31 -0.76 -1.07 4 17 31 0.12 -0.08 6 17 31 0.23 -0.53 3 18 31 -0.60 1.02 0 0 32 1.56 -6.19 0 2 32 -1.52 -2.85 2 2 32 -3.67 -0.85 1 3 32 -0.55 1.03 0 4 32 3.14 -0.89 2 4 32 1.05 -0.39 4 4 32 1.17 -0.59 1 5 32 1.29 0.82 3 5 32 1.12 0.22 0 6 32 3.10 3.73 2 6 32 2.01 2.58 4 6 32 0.71 0.19 6 6 32 1.40 -1.64 1 7 32 -1.82 2.60 3 7 32 -0.74 1.93 5 7 32 0.32 0.79 0 8 32 1.51 2.71 2 8 32 0.70 2.37 4 8 32 -0.95 0.54 6 8 32 0.51 -1.00 8 8 32 0.88 -1.35 1 9 32 -1.46 -0.22 3 9 32 -0.36 0.40 5 9 32 0.30 0.75 7 9 32 -0.97 1.54 0 10 32 2.00 0.93 2 10 32 1.23 1.52 4 10 32 -0.01 -0.05 6 10 32 0.88 -0.13 8 10 32 1.02 -0.46 10 10 32 1.05 0.83 1 11 32 -0.69 -0.17 3 11 32 0.09 -0.20 5 11 32 -0.27 -0.33 7 11 32 -1.93 0.23 9 11 32 -1.30 -0.62 0 12 32 2.25 0.55 2 12 32 1.40 1.43 4 12 32 -0.11 -0.28 6 12 32 -0.07 -0.31 8 12 32 -0.22 -1.06 10 12 32 0.51 -0.20 12 12 32 0.40 -0.54 1 13 32 0.16 0.62 3 13 32 0.77 -0.14 5 13 32 -0.15 -0.54 7 13 32 -1.84 -0.36 9 13 32 -2.07 -0.30 11 13 32 -1.82 0.24 0 14 32 0.28 0.46 2 14 32 0.19 1.08 4 14 32 -0.58 0.18 6 14 32 0.17 0.17 8 14 32 -0.28 0.04 10 14 32 0.35 0.18 1 15 32 -1.50 -1.16 3 15 32 -0.35 -1.12 5 15 32 -0.33 -0.30 7 15 32 -1.17 0.22 2 16 32 -0.18 -0.52 4 16 32 -1.08 0.21 1 2 33 -0.93 -0.57 2 3 33 1.64 0.27 1 4 33 -0.76 -0.51 3 4 33 1.62 -1.40 2 5 33 2.03 -1.61 4 5 33 2.31 -0.41 1 6 33 -0.57 -0.55 3 6 33 0.85 -1.35 5 6 33 -0.73 -3.00 2 7 33 0.27 -0.51 4 7 33 0.22 0.91 6 7 33 1.07 -0.20 1 8 33 -0.45 0.49 3 8 33 -0.51 1.21 5 8 33 -1.42 -0.58 7 8 33 -1.19 -0.05 2 9 33 -1.47 -1.16 4 9 33 -1.56 0.24 6 9 33 -0.69 0.08 8 9 33 -0.17 0.42 1 10 33 0.09 -0.04 3 10 33 -0.09 -0.56 5 10 33 -0.97 -2.25 7 10 33 -0.71 -1.61 9 10 33 1.21 -0.98 2 11 33 -0.82 -1.31 4 11 33 -0.29 -0.03 6 11 33 -0.15 0.02 8 11 33 0.21 0.57 10 11 33 0.81 1.79 1 12 33 0.16 0.63 3 12 33 0.45 0.57 5 12 33 -1.02 -0.15 7 12 33 -0.75 0.08 9 12 33 0.02 0.38 2 13 33 -1.05 -0.48 4 13 33 -0.56 1.25 6 13 33 -0.41 1.55 8 13 33 -0.23 1.17 1 14 33 0.00 0.89 3 14 33 0.63 0.68 5 14 33 -0.87 0.28 1 1 34 1.66 3.45 0 2 34 3.19 0.58 1 3 34 1.14 1.79 3 3 34 1.46 0.69 0 4 34 -0.04 -1.69 2 4 34 -1.13 -0.73 1 5 34 -3.57 -1.28 3 5 34 -1.27 -0.97 5 5 34 0.03 0.46 0 6 34 0.05 -3.07 2 6 34 -0.49 -1.16 4 6 34 -1.30 -1.18 1 7 34 -2.56 -1.52 3 7 34 -0.81 -1.45 5 7 34 0.73 0.80 7 7 34 -0.19 1.55 0 8 34 1.41 -3.09 2 8 34 0.75 -0.94 4 8 34 -0.44 -1.10 6 8 34 -0.04 -0.20 1 9 34 -1.14 -2.39 3 9 34 -0.23 -2.60 5 9 34 0.97 -0.67 7 9 34 -0.31 0.50 9 9 34 -0.21 0.34 0 10 34 2.76 -2.57 2 10 34 1.38 -0.85 4 10 34 0.15 -0.99 6 10 34 -0.36 -0.66 8 10 34 0.45 -1.02 1 11 34 -0.26 0.64 3 11 34 -0.05 0.01 5 11 34 0.48 0.20 7 11 34 -0.69 0.46 9 11 34 -0.73 0.09 0 12 34 0.02 -0.13 2 12 34 -0.51 1.05 4 12 34 0.22 1.04 6 12 34 0.53 0.80 1 13 34 -0.71 -0.43 3 13 34 -0.44 -0.71 1 2 35 -0.38 -0.63 2 3 35 0.58 1.03 1 4 35 -0.35 -0.27 3 4 35 -1.28 1.97 2 5 35 -0.99 1.41 4 5 35 -0.05 2.16 1 6 35 -0.30 -0.17 3 6 35 -1.62 1.48 5 6 35 -2.65 0.42 2 7 35 -0.38 -0.91 4 7 35 0.37 -0.40 6 7 35 0.96 0.90 1 8 35 0.84 -0.38 3 8 35 1.19 -0.53 5 8 35 0.45 -0.90 7 8 35 -0.04 -0.53 2 9 35 -0.25 -0.54 4 9 35 0.61 0.23 6 9 35 1.94 0.54 8 9 35 0.86 0.34 1 10 35 0.59 0.13 3 10 35 1.14 -0.03 5 10 35 0.16 -0.51 7 10 35 -0.85 -1.26 2 11 35 -0.40 -0.42 4 11 35 0.08 0.39 6 11 35 1.08 0.07 1 12 35 0.51 0.02 0 2 36 -1.68 -2.95 2 2 36 -2.41 -1.70 1 3 36 -0.46 1.44 0 4 36 1.47 -0.47 2 4 36 -0.14 0.65 4 4 36 0.48 0.25 1 5 36 0.26 1.88 3 5 36 0.44 0.26 0 6 36 3.52 -0.97 2 6 36 1.15 0.78 4 6 36 0.21 0.23 6 6 36 -1.79 0.72 1 7 36 1.16 1.45 3 7 36 1.24 0.04 5 7 36 0.91 0.21 0 8 36 2.85 0.97 2 8 36 1.01 1.97 4 8 36 0.85 0.58 6 8 36 -0.91 -0.03 1 9 36 -1.56 3.64 3 9 36 -0.76 1.58 5 9 36 0.23 0.73 2 10 36 -1.64 1.17 4 10 36 -0.28 1.06 2 3 37 0.13 -0.64 1 4 37 0.71 -0.96 3 4 37 -0.89 -1.01 2 5 37 0.33 -0.54 4 5 37 1.31 -1.22 1 6 37 0.79 -0.33 3 6 37 0.21 -0.12 5 6 37 -0.83 -0.60 2 7 37 -0.29 0.18 4 7 37 0.23 -0.22 3 8 37 0.88 0.23 0 14 0 5.13 0.27 22 22 0 -0.63 -0.04 17 25 0 -0.36 -0.02 14 26 0 -0.71 -0.02 16 26 0 -0.36 -0.03 15 27 0 0.49 0.01 12 28 0 -1.10 0.05 9 29 0 0.37 -0.10 11 29 0 -0.01 0.00 0 30 0 -0.79 0.13 2 30 0 0.18 -0.17 4 30 0 2.33 0.01 6 30 0 1.81 -0.01 8 30 0 -0.63 0.04 21 22 1 -0.54 -0.43 20 23 1 0.12 0.27 19 24 1 0.02 0.16 18 25 1 0.08 0.01 15 26 1 -0.31 -0.09 17 26 1 -0.37 0.70 13 28 1 1.00 0.30 10 29 1 0.06 0.37 1 30 1 -0.49 -0.60 3 30 1 -0.46 -0.67 5 30 1 -0.56 -0.68 7 30 1 -0.22 -0.52 16 26 2 -0.09 0.00 15 27 2 -0.06 0.05 12 28 2 -1.04 0.90 9 29 2 0.26 0.10 11 29 2 0.98 -0.20 4 30 2 0.51 -0.16 6 30 2 -0.06 0.19 8 30 2 -0.27 -0.16 21 22 3 0.46 0.07 20 23 3 -0.04 0.69 19 24 3 -0.93 0.21 18 25 3 0.25 -0.73 13 28 3 -0.25 -0.12 10 29 3 0.14 -0.08 5 30 3 0.64 0.27 7 30 3 0.54 0.12 16 26 4 0.18 0.08 15 27 4 0.93 0.92 6 30 4 0.90 -0.99 21 22 5 -0.02 0.50 20 23 5 1.27 -0.60 19 24 5 0.37 -0.38 18 25 5 -0.66 0.35 13 28 5 -0.37 0.63 10 29 5 -0.33 0.19 5 30 5 -0.60 0.09 7 30 5 -0.17 0.83 16 26 6 -0.16 0.04 12 28 6 0.85 1.05 6 30 6 -0.42 -0.58 21 22 7 -0.15 0.90 20 23 7 -0.21 0.63 19 24 7 -0.40 -0.23 14 27 7 0.37 -0.79 5 30 7 0.54 -0.91 17 25 8 0.77 -0.81 12 28 8 0.75 0.46 9 29 8 0.79 0.03 4 30 8 0.06 -0.68 11 28 9 -0.23 0.29 8 29 9 0.16 0.87 1 30 9 -0.06 -0.45 3 30 9 -0.39 0.32 19 23 10 0.13 -0.41 18 24 10 0.43 0.47 13 27 10 0.23 -0.10 0 30 10 -0.98 1.08 2 30 10 -1.44 1.28 16 25 11 -0.74 0.30 6 29 11 -0.43 -0.74 14 26 12 -0.56 0.19 5 29 12 1.50 0.73 19 22 13 -0.06 0.26 18 23 13 -1.05 -0.56 13 26 13 -0.77 0.12 2 29 13 0.41 0.23 4 29 13 -0.24 0.71 16 24 14 0.42 0.34 1 29 14 0.12 -0.50 14 25 15 -0.05 -0.89 5 28 15 -0.16 -0.45 20 20 16 1.53 -0.31 19 21 16 0.18 -0.02 13 25 16 -1.28 -0.12 7 27 16 0.05 1.12 0 28 16 0.10 0.60 2 28 16 0.18 1.09 4 28 16 1.42 1.04 19 20 17 -0.01 -0.02 18 21 17 -0.03 1.20 17 22 17 0.04 -1.30 12 25 17 -0.42 -0.17 6 27 17 0.96 -0.02 19 19 18 -0.63 0.52 18 20 18 -1.11 -0.59 17 21 18 -1.01 -0.13 16 22 18 0.37 -0.47 15 23 18 0.03 -0.86 11 25 18 0.59 -0.21 8 26 18 0.00 -0.77 1 27 18 -0.11 -1.21 3 27 18 -0.31 -0.84 5 27 18 -0.18 -0.58 18 19 19 -0.76 0.35 14 23 19 -0.86 -0.01 10 25 19 0.42 0.90 3 26 19 -0.22 0.26 5 26 19 0.28 0.60 7 26 19 0.43 0.81 2 27 19 -0.77 0.05 18 18 20 -0.35 -1.67 13 23 20 -0.30 -0.23 9 25 20 0.11 0.74 0 26 20 -0.24 1.68 2 26 20 0.26 0.35 4 26 20 -0.20 1.07 6 26 20 0.25 0.23 18 19 21 0.45 0.12 12 23 21 -0.31 -0.89 2 25 21 -0.54 0.62 4 25 21 -0.49 -0.26 6 25 21 -0.75 -0.75 1 26 21 0.93 0.56 3 26 21 0.15 -1.09 17 19 22 0.71 0.30 16 20 22 -0.86 -0.38 11 23 22 -1.53 0.34 8 24 22 -0.74 -0.44 1 25 22 -0.43 -0.77 3 25 22 0.36 -0.78 5 25 22 0.42 -0.02 17 18 23 0.51 -1.14 16 19 23 -1.37 -0.20 15 20 23 0.80 0.23 10 23 23 0.58 -0.47 1 24 23 -0.64 0.02 5 24 23 0.70 0.53 7 24 23 1.18 0.26 2 25 23 -0.17 0.72 16 18 24 -0.93 0.84 15 19 24 0.19 0.22 14 20 24 -0.77 1.03 10 22 24 0.99 -0.46 0 24 24 1.01 -0.01 2 24 24 0.06 0.00 4 24 24 -0.56 0.35 16 17 25 -0.01 1.62 15 18 25 0.97 0.63 14 19 25 0.05 1.06 13 20 25 0.49 -0.07 9 22 25 0.85 0.24 4 23 25 0.30 0.68 6 23 25 -0.48 0.64 15 17 26 0.09 -0.87 14 18 26 0.10 -0.62 13 19 26 0.07 -1.50 9 21 26 -0.60 0.33 6 22 26 -0.23 0.15 1 23 26 -0.65 -0.42 15 16 27 -0.60 -0.67 14 17 27 -1.58 -0.94 13 18 27 -0.38 -0.08 9 20 27 0.07 -0.11 1 22 27 -0.11 -0.40 3 22 27 -0.22 -0.18 14 16 28 0.16 0.25 13 17 28 -0.21 0.26 12 18 28 0.75 0.60 8 20 28 -0.07 0.60 1 21 28 0.20 0.66 3 21 28 0.41 0.63 5 21 28 0.32 0.76 14 15 29 0.12 -0.48 13 16 29 1.04 0.34 8 19 29 0.26 0.57 5 20 29 0.16 -0.74 13 15 30 -0.14 0.08 8 18 30 0.62 -0.29 5 19 30 0.40 0.45 9 16 31 -0.05 -0.78 8 17 31 -0.24 -0.34 1 18 31 0.36 0.84 5 18 31 -0.73 0.51 9 15 32 -1.27 0.51 0 16 32 -0.42 -0.85 6 16 32 0.18 0.26 1 17 32 -0.39 0.27 3 17 32 0.31 -0.05 5 17 32 0.26 -0.09 11 12 33 0.65 -0.29 10 13 33 0.21 1.43 7 14 33 -0.18 -0.18 2 15 33 -0.38 -0.15 4 15 33 0.00 0.90 6 15 33 0.32 0.85 1 16 33 0.03 0.42 3 16 33 0.54 0.05 8 12 34 1.49 -0.65 5 13 34 0.36 -0.87 7 13 34 0.15 -0.16 0 14 34 0.62 -0.61 2 14 34 0.51 0.16 4 14 34 0.36 0.29 1 15 34 0.01 -0.04 9 10 35 -1.02 -0.99 8 11 35 0.28 0.14 3 12 35 1.65 -0.27 5 12 35 0.59 -0.92 2 13 35 -0.26 -0.15 4 13 35 0.40 0.68 0 0 36 -1.49 -3.66 8 8 36 -0.05 -0.96 7 9 36 0.42 -0.09 0 10 36 -0.89 0.44 6 10 36 -0.59 0.58 1 11 36 -0.19 0.58 3 11 36 -0.34 -0.45 1 2 37 0.52 -0.48 6 7 37 0.75 -0.32 1 8 37 0.58 -0.09 5 8 37 -0.64 0.05 2 9 37 -0.16 0.62 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 21116) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.028 173 27 ' ' 2 0.000 0.000 0.222 173 27 ' ' 3 0.026 0.253 0.355 42 4 ' ' 4 -0.027 0.747 0.355 43 4 ' ' 5 0.000 0.500 0.472 173 27 ' ' 6 0.000 0.000 0.722 172 27 ' ' 7 -0.027 0.253 0.855 43 4 ' ' 8 0.026 0.747 0.855 42 4 ' ' 9 0.247 0.026 0.105 42 4 ' ' 10 0.253 0.527 0.105 42 4 ' ' 11 0.247 -0.027 0.605 43 4 ' ' 12 0.253 0.473 0.605 43 4 ' ' 13 0.500 0.000 0.472 173 27 ' ' 14 0.500 1.000 0.972 173 27 ' ' 15 0.500 0.500 0.222 172 27 ' ' 16 0.500 0.500 0.722 173 27 ' ' 17 0.473 0.753 0.355 43 4 ' ' 18 0.473 0.247 0.855 43 4 ' ' 19 0.526 0.247 0.355 42 4 ' ' 20 0.526 0.753 0.855 42 4 ' ' 21 0.747 0.473 0.105 43 4 ' ' 22 0.753 0.973 0.105 43 4 ' ' 23 0.747 0.526 0.605 42 4 ' ' 24 0.753 0.027 0.605 42 4 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL w I 41 c d R = 0.05 CELL 24.7912 24.7912 31.0121 90.00 90.00 90.00 SPGR I41cd # Solvent Accessible Volume = 2062 # Electrons Found in S.A.V. = 272 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.595 0.953 0.460 ! 1.59 eA-3 C102 0.561 0.956 0.482 ! 1.42 eA-3 Q103 0.156 0.475 0.492 ! 1.16 eA-3 Q104 0.847 0.498 0.479 ! 0.95 eA-3 Q105 0.796 0.440 0.148 ! 0.69 eA-3 C106 0.983 0.485 0.496 ! 0.59 eA-3 Q107 0.720 0.963 0.116 ! 0.57 eA-3 C108 0.514 0.518 0.218 ! 0.57 eA-3 Q109 0.912 0.449 0.398 ! 0.54 eA-3 C110 0.040 0.236 0.314 ! 0.53 eA-3 Q111 0.227 0.567 0.064 ! 0.51 eA-3 ) ; _shelx_shelxl_version_number 2016/6 _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 2.192 _oxdiff_exptl_absorpt_empirical_full_min 0.619 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x+1/2, z+1/4' 'y, -x+1/2, z+1/4' 'x, -y, z+1/2' '-x, y, z+1/2' 'y, x+1/2, z+3/4' '-y, -x+1/2, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' 'y+1/2, -x+1, z+3/4' 'x+1/2, -y+1/2, z+1' '-x+1/2, y+1/2, z+1' 'y+1/2, x+1, z+5/4' '-y+1/2, -x+1, z+5/4' 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 0.38261(2) 0.23040(2) 0.17794(2) 0.04679(13) Uani 1 1 d . U . . . Cl1 Cl 0.41885(16) 0.26424(15) 0.11626(13) 0.0811(13) Uani 0.745(8) 1 d . U P A 1 Cl1A Cl 0.3342(5) 0.3065(6) 0.1716(6) 0.060(4) Uani 0.255(8) 1 d . U P A 2 N1 N 0.35242(15) 0.19624(16) 0.23537(15) 0.0371(9) Uani 1 1 d . . . . . N2 N 0.43163(16) 0.15935(16) 0.18410(18) 0.0471(11) Uani 1 1 d . U . . . C1 C 0.37389(18) 0.15042(19) 0.24459(19) 0.0377(11) Uani 1 1 d . . . . . C2 C 0.41883(19) 0.1312(2) 0.21730(19) 0.0401(12) Uani 1 1 d . . . . . C3 C 0.4761(3) 0.1431(3) 0.1572(3) 0.0656(16) Uani 1 1 d . U . . . C4 C 0.5298(6) 0.1651(7) 0.1719(6) 0.063(3) Uani 0.623(16) 1 d . U P B 1 C4A C 0.5212(10) 0.1584(10) 0.1535(8) 0.057(4) Uani 0.377(16) 1 d . U P B 2 C5 C 0.5357(7) 0.2074(8) 0.2063(7) 0.092(4) Uani 0.623(16) 1 d . U P B 1 H5 H 0.500811 0.208037 0.222545 0.111 Uiso 0.623(16) 1 calc R . P B 1 C5A C 0.5371(10) 0.1944(12) 0.1875(9) 0.067(5) Uani 0.377(16) 1 d . U P B 2 H5A H 0.507769 0.202266 0.208694 0.080 Uiso 0.377(16) 1 calc R . P B 2 C6 C 0.5414(8) 0.2587(7) 0.1873(8) 0.116(7) Uani 0.623(16) 1 d . U P B 1 H6A H 0.528596 0.286426 0.207360 0.174 Uiso 0.623(16) 1 calc GR . P B 1 H6B H 0.520125 0.260270 0.160671 0.174 Uiso 0.623(16) 1 calc GR . P B 1 H6C H 0.579492 0.265161 0.180555 0.174 Uiso 0.623(16) 1 calc GR . P B 1 C6A C 0.563(2) 0.2504(15) 0.1635(14) 0.136(12) Uani 0.377(16) 1 d . U P B 2 H6AA H 0.540735 0.260265 0.138675 0.204 Uiso 0.377(16) 1 calc GR . P B 2 H6AB H 0.599957 0.242973 0.153859 0.204 Uiso 0.377(16) 1 calc GR . P B 2 H6AC H 0.563460 0.280238 0.184260 0.204 Uiso 0.377(16) 1 calc GR . P B 2 C7 C 0.5778(10) 0.1930(9) 0.2377(7) 0.120(7) Uani 0.623(16) 1 d . U P B 1 H7A H 0.613181 0.193992 0.223560 0.181 Uiso 0.623(16) 1 calc GR . P B 1 H7B H 0.571054 0.156594 0.248760 0.181 Uiso 0.623(16) 1 calc GR . P B 1 H7C H 0.577345 0.218790 0.261629 0.181 Uiso 0.623(16) 1 calc GR . P B 1 C7A C 0.5894(11) 0.1772(13) 0.2080(13) 0.104(9) Uani 0.377(16) 1 d . U P B 2 H7AA H 0.601333 0.143062 0.195148 0.157 Uiso 0.377(16) 1 calc GR . P B 2 H7AB H 0.584063 0.172296 0.239036 0.157 Uiso 0.377(16) 1 calc GR . P B 2 H7AC H 0.616883 0.204927 0.203062 0.157 Uiso 0.377(16) 1 calc GR . P B 2 C8 C 0.5735(6) 0.1474(7) 0.1464(6) 0.073(4) Uani 0.623(16) 1 d . U P B 1 H8 H 0.609154 0.159006 0.152654 0.088 Uiso 0.623(16) 1 calc R . P B 1 C8A C 0.5601(12) 0.1369(12) 0.1248(10) 0.074(6) Uani 0.377(16) 1 d . U P B 2 H8A H 0.597689 0.142260 0.129141 0.089 Uiso 0.377(16) 1 calc R . P B 2 C9 C 0.5637(8) 0.1131(9) 0.1124(7) 0.098(5) Uani 0.623(16) 1 d . U P B 1 H9 H 0.592898 0.105186 0.093600 0.117 Uiso 0.623(16) 1 calc R . P B 1 C9A C 0.5397(15) 0.1063(12) 0.0885(11) 0.089(7) Uani 0.377(16) 1 d . U P B 2 H9A H 0.565576 0.095634 0.067589 0.107 Uiso 0.377(16) 1 calc R . P B 2 C10 C 0.5150(9) 0.0898(9) 0.1038(7) 0.107(5) Uani 0.623(16) 1 d . U P B 1 H10 H 0.513067 0.063782 0.081313 0.129 Uiso 0.623(16) 1 calc R . P B 1 C10A C 0.4901(13) 0.0916(11) 0.0812(11) 0.092(6) Uani 0.377(16) 1 d . U P B 2 H10A H 0.477755 0.068999 0.058498 0.110 Uiso 0.377(16) 1 calc R . P B 2 C11 C 0.4650(8) 0.1029(9) 0.1277(6) 0.102(5) Uani 0.623(16) 1 d D U P B 1 C11A C 0.4595(11) 0.1148(13) 0.1123(12) 0.094(6) Uani 0.377(16) 1 d D U P B 2 C12 C 0.4082(10) 0.0996(10) 0.1057(8) 0.136(6) Uani 0.623(16) 1 d D U P B 1 H12 H 0.383156 0.117500 0.126590 0.163 Uiso 0.623(16) 1 calc R . P B 1 C12A C 0.4125(11) 0.0777(11) 0.1228(9) 0.084(6) Uani 0.377(16) 1 d D U P B 2 H12A H 0.404607 0.076232 0.154395 0.101 Uiso 0.377(16) 1 calc R . P B 2 C13 C 0.3873(12) 0.0412(10) 0.1024(10) 0.149(9) Uani 0.623(16) 1 d D U P B 1 H13A H 0.394850 0.022047 0.129352 0.223 Uiso 0.623(16) 1 calc GR . P B 1 H13B H 0.405361 0.022859 0.078442 0.223 Uiso 0.623(16) 1 calc GR . P B 1 H13C H 0.348257 0.041633 0.097252 0.223 Uiso 0.623(16) 1 calc GR . P B 1 C13A C 0.4186(16) 0.0228(13) 0.1034(12) 0.110(10) Uani 0.377(16) 1 d . U P B 2 H13D H 0.437894 0.025709 0.075880 0.165 Uiso 0.377(16) 1 calc GR . P B 2 H13E H 0.382879 0.007109 0.098412 0.165 Uiso 0.377(16) 1 calc GR . P B 2 H13F H 0.439081 -0.000321 0.123092 0.165 Uiso 0.377(16) 1 calc GR . P B 2 C14 C 0.3955(14) 0.1252(11) 0.0629(9) 0.184(11) Uani 0.623(16) 1 d D U P B 1 H14A H 0.361914 0.109949 0.051520 0.276 Uiso 0.623(16) 1 calc GR . P B 1 H14B H 0.424985 0.118145 0.042697 0.276 Uiso 0.623(16) 1 calc GR . P B 1 H14C H 0.391227 0.164220 0.066738 0.276 Uiso 0.623(16) 1 calc GR . P B 1 C14A C 0.3659(12) 0.1170(14) 0.0945(10) 0.120(11) Uani 0.377(16) 1 d D U P B 2 H14D H 0.376649 0.154151 0.095641 0.180 Uiso 0.377(16) 1 d R . P B 2 H14E H 0.330918 0.113001 0.107341 0.180 Uiso 0.377(16) 1 d R . P B 2 H14F H 0.364629 0.105311 0.065001 0.180 Uiso 0.377(16) 1 d R . P B 2 C15 C 0.4432(2) 0.0792(2) 0.2342(2) 0.0415(12) Uani 1 1 d . . . . . H15 H 0.474081 0.065895 0.216385 0.050 Uiso 1 1 calc R . . . . C16 C 0.4588(2) 0.0911(2) 0.2812(2) 0.0429(12) Uani 1 1 d . . . . . C17 C 0.4153(2) 0.10854(19) 0.30632(19) 0.0394(12) Uani 1 1 d . . . . . C18 C 0.36225(19) 0.11303(19) 0.28170(19) 0.0372(11) Uani 1 1 d . . . . . H18 H 0.331388 0.125160 0.300056 0.045 Uiso 1 1 calc R . . . . C19 C 0.3530(2) 0.05779(19) 0.26062(19) 0.0387(11) Uani 1 1 d . . . . . C20 C 0.3963(2) 0.0404(2) 0.2355(2) 0.0416(12) Uani 1 1 d . . . . . C21 C 0.3935(3) -0.0098(2) 0.2152(2) 0.0512(14) Uani 1 1 d . . . . . H21 H 0.422686 -0.021947 0.197877 0.061 Uiso 1 1 calc R . . . . C22 C 0.3485(3) -0.0416(2) 0.2204(2) 0.0605(17) Uani 1 1 d . . . . . H22 H 0.347096 -0.075689 0.206530 0.073 Uiso 1 1 calc R . . . . C23 C 0.3052(3) -0.0250(2) 0.2453(2) 0.0527(14) Uani 1 1 d . . . . . C24 C 0.3077(2) 0.0260(2) 0.26590(19) 0.0448(12) Uani 1 1 d . . . . . H24 H 0.278552 0.038194 0.283179 0.054 Uiso 1 1 calc R . . . . C25 C 0.2556(3) -0.0606(3) 0.2527(3) 0.0676(19) Uani 1 1 d . . . . . C26 C 0.2098(4) -0.0373(4) 0.2279(5) 0.141(6) Uani 1 1 d . . . . . H26A H 0.201376 -0.001277 0.239038 0.212 Uiso 1 1 calc GR . . . . H26B H 0.178174 -0.060626 0.230791 0.212 Uiso 1 1 calc GR . . . . H26C H 0.219865 -0.034548 0.197360 0.212 Uiso 1 1 calc GR . . . . C27 C 0.2448(4) -0.0657(4) 0.3011(3) 0.093(3) Uani 1 1 d . . . . . H27A H 0.232340 -0.031030 0.312404 0.139 Uiso 1 1 calc GR . . . . H27B H 0.278151 -0.076308 0.315824 0.139 Uiso 1 1 calc GR . . . . H27C H 0.217090 -0.093236 0.305965 0.139 Uiso 1 1 calc GR . . . . C28 C 0.2657(4) -0.1187(3) 0.2366(4) 0.097(4) Uani 1 1 d . . . . . H28A H 0.233222 -0.140473 0.241110 0.146 Uiso 1 1 calc GR . . . . H28B H 0.295862 -0.134569 0.252650 0.146 Uiso 1 1 calc GR . . . . H28C H 0.274544 -0.117955 0.205787 0.146 Uiso 1 1 calc GR . . . . C29 C 0.4227(2) 0.1196(2) 0.3495(2) 0.0456(13) Uani 1 1 d . . . . . H29 H 0.393592 0.132042 0.366803 0.055 Uiso 1 1 calc R . . . . C30 C 0.4741(2) 0.1122(2) 0.3674(2) 0.0513(15) Uani 1 1 d . . . . . H30 H 0.479425 0.119572 0.397171 0.062 Uiso 1 1 calc R . . . . C31 C 0.5177(2) 0.0943(2) 0.3429(3) 0.0568(16) Uani 1 1 d . . . . . C32 C 0.5091(2) 0.0837(2) 0.2990(2) 0.0503(14) Uani 1 1 d . . . . . H32 H 0.538156 0.071488 0.281587 0.060 Uiso 1 1 calc R . . . . C33 C 0.5742(3) 0.0863(3) 0.3617(3) 0.075(2) Uani 1 1 d . . . . . C34 C 0.5952(3) 0.0308(3) 0.3502(3) 0.075(2) Uani 1 1 d . . . . . H34A H 0.631599 0.026289 0.361954 0.113 Uiso 1 1 calc GR . . . . H34B H 0.596283 0.026989 0.318761 0.113 Uiso 1 1 calc GR . . . . H34C H 0.571269 0.003333 0.362413 0.113 Uiso 1 1 calc GR . . . . C35 C 0.5744(4) 0.0939(6) 0.4102(4) 0.134(5) Uani 1 1 d . . . . . H35A H 0.554957 0.064024 0.423888 0.201 Uiso 1 1 calc GR . . . . H35B H 0.556695 0.128049 0.417453 0.201 Uiso 1 1 calc GR . . . . H35C H 0.611709 0.094524 0.420693 0.201 Uiso 1 1 calc GR . . . . C36 C 0.6125(4) 0.1283(4) 0.3442(6) 0.146(7) Uani 1 1 d . . . . . H36A H 0.649021 0.121073 0.354870 0.219 Uiso 1 1 calc GR . . . . H36B H 0.600954 0.164138 0.353742 0.219 Uiso 1 1 calc GR . . . . H36C H 0.612411 0.126859 0.312620 0.219 Uiso 1 1 calc GR . . . . C37 C 0.3110(2) 0.2183(2) 0.26262(19) 0.0439(13) Uani 1 1 d . . . . . C38 C 0.3262(3) 0.2472(3) 0.2987(2) 0.0578(16) Uani 1 1 d . . . . . C39 C 0.3849(3) 0.2580(3) 0.3092(3) 0.072(2) Uani 1 1 d . . . . . H39 H 0.405968 0.225673 0.299805 0.086 Uiso 1 1 calc R . . . . C40 C 0.3954(5) 0.2657(3) 0.3567(4) 0.095(3) Uani 1 1 d . . . . . H40A H 0.376116 0.297854 0.366863 0.143 Uiso 1 1 calc GR . . . . H40B H 0.434147 0.270372 0.361553 0.143 Uiso 1 1 calc GR . . . . H40C H 0.382620 0.234035 0.372620 0.143 Uiso 1 1 calc GR . . . . C41 C 0.4058(5) 0.3061(4) 0.2838(3) 0.106(3) Uani 1 1 d . . . . . H41A H 0.402865 0.298643 0.252868 0.159 Uiso 1 1 calc GR . . . . H41B H 0.443671 0.312635 0.291257 0.159 Uiso 1 1 calc GR . . . . H41C H 0.384367 0.338127 0.290920 0.159 Uiso 1 1 calc GR . . . . C42 C 0.2835(4) 0.2688(3) 0.3237(3) 0.086(3) Uani 1 1 d . . . . . H42 H 0.291435 0.289471 0.348644 0.103 Uiso 1 1 calc R . . . . C43 C 0.2308(4) 0.2600(5) 0.3121(3) 0.092(3) Uani 1 1 d . . . . . H43 H 0.202864 0.273508 0.330101 0.110 Uiso 1 1 calc R . . . . C44 C 0.2173(3) 0.2323(4) 0.2756(4) 0.086(3) Uani 1 1 d . . . . . H44 H 0.180458 0.227601 0.268027 0.103 Uiso 1 1 calc R . . . . C45 C 0.2573(3) 0.2113(3) 0.2498(3) 0.0685(19) Uani 1 1 d . U . . . C46 C 0.2418(3) 0.1850(4) 0.2059(4) 0.105(3) Uani 1 1 d D U . . . H46 H 0.273403 0.175038 0.187484 0.126 Uiso 0.45(5) 1 calc R . P C 1 H46A H 0.274434 0.191054 0.187528 0.126 Uiso 0.55(5) 1 calc R . P C 2 C47 C 0.1972(4) 0.2149(4) 0.1817(4) 0.108(3) Uani 1 1 d . U . . . H47A H 0.163001 0.210704 0.197244 0.162 Uiso 1 1 calc GR . . . . H47B H 0.193573 0.199949 0.152615 0.162 Uiso 1 1 calc GR . . . . H47C H 0.206308 0.253315 0.179805 0.162 Uiso 1 1 calc GR . . . . C48 C 0.2114(19) 0.1343(15) 0.2273(15) 0.129(12) Uani 0.45(5) 1 d D U P C 1 H48A H 0.236525 0.114035 0.244397 0.193 Uiso 0.45(5) 1 d R . P C 1 H48B H 0.196725 0.111475 0.205177 0.193 Uiso 0.45(5) 1 d R . P C 1 H48C H 0.182685 0.147155 0.245367 0.193 Uiso 0.45(5) 1 d R . P C 1 C48A C 0.2351(9) 0.1254(6) 0.2055(9) 0.086(6) Uani 0.55(5) 1 d D U P C 2 H48D H 0.269569 0.108204 0.212467 0.129 Uiso 0.55(5) 1 calc GR . P C 2 H48E H 0.223188 0.113763 0.176851 0.129 Uiso 0.55(5) 1 calc GR . P C 2 H48F H 0.208005 0.115026 0.226997 0.129 Uiso 0.55(5) 1 calc GR . P C 2 C49 C 0.3338(9) 0.2947(8) 0.1801(8) 0.070(7) Uani 0.745(8) 1 d . U P A 1 H49A H 0.355231 0.327727 0.177040 0.105 Uiso 0.745(8) 1 calc GR . P A 1 H49B H 0.314677 0.295352 0.207735 0.105 Uiso 0.745(8) 1 calc GR . P A 1 H49C H 0.307553 0.292610 0.156494 0.105 Uiso 0.745(8) 1 calc GR . P A 1 C49A C 0.4100(19) 0.2534(18) 0.1212(13) 0.053(7) Uani 0.255(8) 1 d . U P A 2 H49D H 0.384866 0.241722 0.098634 0.080 Uiso 0.255(8) 1 calc GR . P A 2 H49E H 0.445429 0.237030 0.116095 0.080 Uiso 0.255(8) 1 calc GR . P A 2 H49F H 0.413312 0.292742 0.120596 0.080 Uiso 0.255(8) 1 calc GR . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04028(19) 0.02927(17) 0.0708(2) 0.0076(2) 0.0142(2) 0.01084(13) Cl1 0.079(2) 0.066(2) 0.098(2) 0.0363(15) 0.0491(17) 0.0316(15) Cl1A 0.049(4) 0.043(5) 0.088(10) 0.026(5) 0.018(4) 0.033(3) N1 0.0262(18) 0.0299(19) 0.055(3) -0.0040(19) 0.0026(18) 0.0079(15) N2 0.037(2) 0.0300(18) 0.074(3) 0.003(2) 0.017(2) 0.0056(16) C1 0.023(2) 0.027(2) 0.063(3) -0.006(2) -0.003(2) 0.0015(18) C2 0.027(2) 0.031(2) 0.061(3) -0.005(2) 0.005(2) 0.0031(19) C3 0.057(3) 0.047(3) 0.093(4) 0.015(3) 0.033(3) 0.022(2) C4 0.047(5) 0.063(6) 0.078(8) 0.026(6) 0.016(5) 0.020(4) C4A 0.055(6) 0.052(8) 0.065(8) 0.025(6) 0.027(6) 0.015(5) C5 0.062(7) 0.099(8) 0.116(9) -0.004(6) 0.013(7) -0.014(6) C5A 0.045(7) 0.077(9) 0.079(10) 0.004(7) 0.017(7) 0.014(7) C6 0.106(11) 0.084(8) 0.158(16) 0.011(9) -0.011(11) 0.041(8) C6A 0.16(2) 0.085(14) 0.16(2) 0.034(14) 0.031(17) -0.020(14) C7 0.144(14) 0.097(12) 0.121(12) 0.036(10) -0.027(11) -0.050(10) C7A 0.066(11) 0.093(15) 0.154(19) 0.021(14) -0.013(12) 0.006(11) C8 0.052(6) 0.074(7) 0.094(8) 0.024(6) 0.021(5) 0.014(5) C8A 0.071(9) 0.071(10) 0.081(10) -0.004(8) 0.031(7) 0.002(8) C9 0.087(7) 0.102(9) 0.104(9) -0.002(7) 0.030(7) 0.023(7) C9A 0.098(9) 0.081(11) 0.089(10) 0.000(8) 0.017(8) 0.003(8) C10 0.111(8) 0.102(9) 0.109(10) -0.029(8) 0.024(7) 0.022(7) C10A 0.096(9) 0.081(11) 0.099(10) -0.013(9) 0.006(8) 0.015(8) C11 0.119(8) 0.089(9) 0.098(9) -0.022(7) 0.038(6) 0.027(7) C11A 0.103(10) 0.083(10) 0.096(10) -0.005(8) 0.020(8) 0.022(7) C12 0.151(10) 0.130(10) 0.127(10) -0.049(9) 0.006(8) 0.014(9) C12A 0.108(10) 0.078(9) 0.066(10) 0.003(8) -0.001(8) 0.010(8) C13 0.168(18) 0.138(13) 0.140(16) 0.011(14) -0.015(16) 0.001(12) C13A 0.14(2) 0.102(13) 0.091(15) -0.036(13) 0.006(16) -0.010(13) C14 0.22(2) 0.139(16) 0.196(17) 0.005(14) -0.022(15) 0.031(16) C14A 0.15(2) 0.124(19) 0.091(17) 0.027(15) -0.005(16) -0.004(17) C15 0.031(2) 0.028(2) 0.066(3) -0.003(2) 0.004(2) 0.0077(19) C16 0.030(2) 0.027(2) 0.072(4) -0.005(2) -0.003(3) 0.0034(19) C17 0.030(2) 0.025(2) 0.063(3) -0.006(2) -0.004(2) 0.0021(18) C18 0.026(2) 0.026(2) 0.060(3) 0.001(2) 0.002(2) 0.0013(17) C19 0.034(2) 0.026(2) 0.057(3) 0.002(2) -0.007(2) -0.0011(18) C20 0.041(3) 0.023(2) 0.061(3) -0.001(2) -0.005(3) 0.004(2) C21 0.069(4) 0.029(3) 0.056(3) -0.004(3) -0.006(3) 0.006(2) C22 0.087(5) 0.033(3) 0.062(4) -0.006(3) 0.000(4) -0.010(3) C23 0.060(4) 0.039(3) 0.059(3) 0.000(3) -0.013(3) -0.014(3) C24 0.044(3) 0.034(3) 0.056(3) 0.004(2) -0.011(3) -0.008(2) C25 0.070(4) 0.047(4) 0.086(5) 0.002(4) -0.007(4) -0.026(3) C26 0.069(6) 0.097(7) 0.257(16) 0.060(9) -0.064(8) -0.037(5) C27 0.096(6) 0.078(6) 0.104(6) -0.008(5) 0.018(6) -0.048(5) C28 0.108(7) 0.059(5) 0.125(9) -0.012(5) -0.010(6) -0.042(5) C29 0.034(3) 0.031(2) 0.072(4) -0.005(3) -0.003(3) 0.0025(19) C30 0.040(3) 0.043(3) 0.070(4) -0.016(3) -0.012(3) 0.010(2) C31 0.037(3) 0.042(3) 0.091(5) -0.018(3) -0.014(3) 0.007(2) C32 0.029(2) 0.042(3) 0.080(4) -0.014(3) -0.006(3) 0.009(2) C33 0.038(3) 0.066(4) 0.120(7) -0.041(4) -0.026(4) 0.009(3) C34 0.052(4) 0.066(4) 0.108(6) -0.021(4) -0.034(4) 0.026(3) C35 0.076(6) 0.182(12) 0.143(10) -0.080(9) -0.060(6) 0.057(7) C36 0.055(5) 0.084(7) 0.30(2) -0.010(10) -0.057(8) -0.016(4) C37 0.040(3) 0.029(2) 0.062(3) 0.006(2) 0.017(3) 0.014(2) C38 0.068(4) 0.038(3) 0.067(4) 0.005(3) 0.013(3) 0.017(3) C39 0.087(5) 0.044(4) 0.084(5) -0.017(4) 0.000(4) -0.005(3) C40 0.135(9) 0.050(4) 0.101(7) 0.000(4) -0.028(7) -0.015(5) C41 0.128(9) 0.095(7) 0.096(7) 0.002(6) -0.013(6) -0.038(7) C42 0.111(7) 0.073(5) 0.072(5) -0.008(4) 0.029(5) 0.038(5) C43 0.084(6) 0.109(7) 0.082(6) 0.013(6) 0.025(5) 0.058(5) C44 0.049(4) 0.094(6) 0.115(7) 0.024(6) 0.029(5) 0.035(4) C45 0.036(3) 0.071(4) 0.099(5) 0.017(4) 0.017(3) 0.018(3) C46 0.037(3) 0.096(5) 0.182(9) -0.032(6) -0.002(5) 0.007(4) C47 0.089(6) 0.112(7) 0.122(7) 0.023(8) -0.014(7) 0.009(5) C48 0.14(2) 0.107(14) 0.14(2) 0.017(13) -0.062(16) 0.000(13) C48A 0.075(11) 0.086(7) 0.096(15) 0.006(8) -0.001(11) 0.018(7) C49 0.096(11) 0.066(13) 0.048(7) 0.024(9) 0.010(6) 0.045(8) C49A 0.053(8) 0.054(8) 0.054(7) 0.000(2) 0.000(2) 0.000(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0180 0.0090 '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 0.3640 0.7020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0310 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1220 3.9340 '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 N1 Pd1 Cl1 177.03(13) N1 Pd1 Cl1A 102.8(4) N1 Pd1 N2 78.26(17) N2 Pd1 Cl1 98.85(16) N2 Pd1 Cl1A 177.9(4) C49 Pd1 Cl1 88.4(6) C49 Pd1 N1 94.4(6) C49 Pd1 N2 172.5(7) C49A Pd1 Cl1A 82.2(15) C49A Pd1 N1 172.9(13) C49A Pd1 N2 97.0(14) C1 N1 Pd1 113.3(4) C1 N1 C37 120.0(5) C37 N1 Pd1 126.7(3) C2 N2 Pd1 112.1(3) C2 N2 C3 120.2(4) C3 N2 Pd1 127.6(4) N1 C1 C2 117.9(5) N1 C1 C18 129.4(5) C2 C1 C18 112.6(4) N2 C2 C1 118.1(5) N2 C2 C15 129.8(5) C1 C2 C15 112.1(5) N2 C3 C4 113.6(9) N2 C3 C11A 115.3(11) C4A C3 N2 133.5(14) C4A C3 C11A 107.2(17) C11 C3 N2 115.7(10) C11 C3 C4 129.5(12) C5 C4 C3 123.5(12) C8 C4 C3 113.3(16) C8 C4 C5 122.7(15) C3 C4A C5A 112.8(19) C3 C4A C8A 126(2) C8A C4A C5A 121(2) C6 C5 C4 110.0(17) C6 C5 C7 115.1(16) C7 C5 C4 111.6(17) C4A C5A C6A 107(2) C4A C5A C7A 112(2) C7A C5A C6A 95(3) C9 C8 C4 119.1(16) C4A C8A C9A 117(3) C10 C9 C8 124.6(17) C10A C9A C8A 128(3) C9 C10 C11 123.2(19) C9A C10A C11A 107(3) C3 C11 C10 109.0(17) C3 C11 C12 120.3(15) C10 C11 C12 121.5(18) C10A C11A C3 131(2) C10A C11A C12A 109(3) C12A C11A C3 106(2) C13 C12 C11 112(2) C14 C12 C11 123(2) C14 C12 C13 105(2) C11A C12A C14A 93.5(17) C13A C12A C11A 113(3) C13A C12A C14A 112(2) C2 C15 C16 105.4(4) C20 C15 C2 104.2(4) C20 C15 C16 106.9(5) C17 C16 C15 113.2(5) C32 C16 C15 125.8(5) C32 C16 C17 121.0(6) C16 C17 C18 114.1(5) C29 C17 C16 120.0(5) C29 C17 C18 126.0(5) C1 C18 C17 105.2(4) C1 C18 C19 104.6(5) C17 C18 C19 106.1(4) C20 C19 C18 113.5(4) C24 C19 C18 125.5(5) C24 C19 C20 121.0(5) C19 C20 C15 114.2(5) C19 C20 C21 119.3(5) C21 C20 C15 126.4(5) C22 C21 C20 119.8(6) C21 C22 C23 121.6(6) C22 C23 C24 118.7(6) C22 C23 C25 122.4(6) C24 C23 C25 118.9(6) C19 C24 C23 119.5(6) C23 C25 C28 111.0(7) C26 C25 C23 108.1(6) C26 C25 C27 114.1(10) C26 C25 C28 108.5(8) C27 C25 C23 109.6(6) C27 C25 C28 105.5(8) C17 C29 C30 118.6(6) C31 C30 C29 122.1(6) C30 C31 C32 118.2(5) C30 C31 C33 122.9(7) C32 C31 C33 118.9(6) C16 C32 C31 120.2(6) C34 C33 C31 110.1(5) C34 C33 C35 110.3(8) C35 C33 C31 111.3(7) C36 C33 C31 110.4(8) C36 C33 C34 109.0(8) C36 C33 C35 105.6(9) C38 C37 N1 118.6(5) C38 C37 C45 123.6(6) C45 C37 N1 117.8(6) C37 C38 C39 121.9(6) C37 C38 C42 115.8(7) C42 C38 C39 122.2(7) C38 C39 C41 110.7(7) C40 C39 C38 113.5(8) C40 C39 C41 110.3(7) C43 C42 C38 120.6(8) C44 C43 C42 122.0(7) C43 C44 C45 119.6(9) C37 C45 C46 122.3(6) C44 C45 C37 118.3(9) C44 C45 C46 119.2(8) C45 C46 C48 94.7(18) C47 C46 C45 113.9(8) C47 C46 C48 104.0(15) C48A C46 C45 116.7(13) C48A C46 C47 113.4(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 Cl1 2.274(3) Pd1 Cl1A 2.244(12) Pd1 N1 2.109(5) Pd1 N2 2.148(4) Pd1 C49 2.004(18) Pd1 C49A 1.97(4) N1 C1 1.287(6) N1 C37 1.437(6) N2 C2 1.283(7) N2 C3 1.439(7) C1 C2 1.478(7) C1 C18 1.506(8) C2 C15 1.518(7) C3 C4 1.509(19) C3 C4A 1.19(3) C3 C11 1.38(2) C3 C11A 1.61(4) C4 C5 1.50(2) C4 C8 1.41(2) C4A C5A 1.44(4) C4A C8A 1.42(3) C5 C6 1.41(3) C5 C7 1.47(3) C5A C6A 1.70(4) C5A C7A 1.51(4) C8 C9 1.38(3) C8A C9A 1.45(4) C9 C10 1.37(3) C9A C10A 1.30(5) C10 C11 1.48(3) C10A C11A 1.35(4) C11 C12 1.57(2) C11A C12A 1.52(2) C12 C13 1.54(2) C12 C14 1.505(16) C12A C13A 1.50(4) C12A C14A 1.75(4) C15 C16 1.535(8) C15 C20 1.510(7) C16 C17 1.400(8) C16 C32 1.378(8) C17 C18 1.524(7) C17 C29 1.380(9) C18 C19 1.535(7) C19 C20 1.394(8) C19 C24 1.381(7) C20 C21 1.395(7) C21 C22 1.375(10) C22 C23 1.386(10) C23 C24 1.417(8) C23 C25 1.530(9) C25 C26 1.488(13) C25 C27 1.529(12) C25 C28 1.546(12) C29 C30 1.403(8) C30 C31 1.392(9) C31 C32 1.402(10) C31 C33 1.532(8) C33 C34 1.512(9) C33 C35 1.516(13) C33 C36 1.510(14) C37 C38 1.381(9) C37 C45 1.400(9) C38 C39 1.514(11) C38 C42 1.416(10) C39 C40 1.508(13) C39 C41 1.522(13) C42 C43 1.372(14) C43 C44 1.366(15) C44 C45 1.377(10) C45 C46 1.560(14) C46 C47 1.528(13) C46 C48 1.61(2) C46 C48A 1.487(16) 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 Pd1 N1 C1 C2 5.8(6) Pd1 N1 C1 C18 -178.1(4) Pd1 N1 C37 C38 -97.5(6) Pd1 N1 C37 C45 79.4(6) Pd1 N2 C2 C1 1.0(6) Pd1 N2 C2 C15 -178.9(5) Pd1 N2 C3 C4 88.9(9) Pd1 N2 C3 C4A 74(2) Pd1 N2 C3 C11 -102.7(12) Pd1 N2 C3 C11A -80.0(14) N1 C1 C2 N2 -4.8(8) N1 C1 C2 C15 175.1(5) N1 C1 C18 C17 -119.4(6) N1 C1 C18 C19 129.0(5) N1 C37 C38 C39 2.2(9) N1 C37 C38 C42 178.8(6) N1 C37 C45 C44 -179.9(6) N1 C37 C45 C46 -5.0(10) N2 C2 C15 C16 125.0(6) N2 C2 C15 C20 -122.7(6) N2 C3 C4 C5 -10.2(17) N2 C3 C4 C8 177.7(10) N2 C3 C4A C5A 12(3) N2 C3 C4A C8A 179.7(18) N2 C3 C11 C10 -178.2(13) N2 C3 C11 C12 35(2) N2 C3 C11A C10A -175(3) N2 C3 C11A C12A -41(2) C1 N1 C37 C38 84.5(6) C1 N1 C37 C45 -98.6(7) C1 C2 C15 C16 -54.8(5) C1 C2 C15 C20 57.5(6) C1 C18 C19 C20 56.9(6) C1 C18 C19 C24 -124.9(6) C2 N2 C3 C4 -87.9(9) C2 N2 C3 C4A -102.6(19) C2 N2 C3 C11 80.5(13) C2 N2 C3 C11A 103.2(14) C2 C1 C18 C17 56.8(5) C2 C1 C18 C19 -54.8(5) C2 C15 C16 C17 57.1(6) C2 C15 C16 C32 -125.7(6) C2 C15 C20 C19 -57.3(6) C2 C15 C20 C21 124.1(6) C3 N2 C2 C1 178.3(6) C3 N2 C2 C15 -1.6(9) C3 C4 C5 C6 -97.3(17) C3 C4 C5 C7 133.7(15) C3 C4 C8 C9 -1(2) C3 C4A C5A C6A -128(3) C3 C4A C5A C7A 129(2) C3 C4A C8A C9A 20(4) C3 C11 C12 C13 -138(2) C3 C11 C12 C14 93(3) C3 C11A C12A C13A -134(2) C3 C11A C12A C14A 111(2) C4 C3 C11 C10 -12(2) C4 C3 C11 C12 -159.2(17) C4 C8 C9 C10 -7(3) C4A C3 C11A C10A 25(4) C4A C3 C11A C12A 159(2) C4A C8A C9A C10A -7(5) C5 C4 C8 C9 -172.6(16) C5A C4A C8A C9A -173(2) C8 C4 C5 C6 74(2) C8 C4 C5 C7 -55(2) C8 C9 C10 C11 6(4) C8A C4A C5A C6A 63(3) C8A C4A C5A C7A -40(3) C8A C9A C10A C11A 6(5) C9 C10 C11 C3 3(3) C9 C10 C11 C12 150(2) C9A C10A C11A C3 -14(5) C9A C10A C11A C12A -147(3) C10 C11 C12 C13 78(3) C10 C11 C12 C14 -50(3) C10A C11A C12A C13A 11(4) C10A C11A C12A C14A -104(3) C11 C3 C4 C5 -176.7(17) C11 C3 C4 C8 11(2) C11A C3 C4A C5A 167(2) C11A C3 C4A C8A -25(3) C15 C16 C17 C18 -1.1(6) C15 C16 C17 C29 178.5(5) C15 C16 C32 C31 -177.7(6) C15 C20 C21 C22 178.1(6) C16 C15 C20 C19 53.9(6) C16 C15 C20 C21 -124.7(6) C16 C17 C18 C1 -56.2(5) C16 C17 C18 C19 54.3(6) C16 C17 C29 C30 -1.0(8) C17 C16 C32 C31 -0.7(9) C17 C18 C19 C20 -54.0(6) C17 C18 C19 C24 124.1(6) C17 C29 C30 C31 0.3(9) C18 C1 C2 N2 178.6(5) C18 C1 C2 C15 -1.6(6) C18 C17 C29 C30 178.6(5) C18 C19 C20 C15 0.0(7) C18 C19 C20 C21 178.7(5) C18 C19 C24 C23 -178.3(5) C19 C20 C21 C22 -0.4(9) C20 C15 C16 C17 -53.3(6) C20 C15 C16 C32 123.9(6) C20 C19 C24 C23 -0.3(8) C20 C21 C22 C23 0.2(10) C21 C22 C23 C24 0.0(10) C21 C22 C23 C25 -177.9(7) C22 C23 C24 C19 0.0(9) C22 C23 C25 C26 -108.1(10) C22 C23 C25 C27 127.0(8) C22 C23 C25 C28 10.8(11) C24 C19 C20 C15 -178.2(5) C24 C19 C20 C21 0.5(8) C24 C23 C25 C26 74.0(10) C24 C23 C25 C27 -50.9(10) C24 C23 C25 C28 -167.0(7) C25 C23 C24 C19 178.0(6) C29 C17 C18 C1 124.3(6) C29 C17 C18 C19 -125.2(6) C29 C30 C31 C32 0.1(10) C29 C30 C31 C33 179.6(6) C30 C31 C32 C16 0.1(9) C30 C31 C33 C34 129.2(8) C30 C31 C33 C35 6.5(11) C30 C31 C33 C36 -110.5(10) C32 C16 C17 C18 -178.4(5) C32 C16 C17 C29 1.2(8) C32 C31 C33 C34 -51.3(10) C32 C31 C33 C35 -174.0(8) C32 C31 C33 C36 69.0(9) C33 C31 C32 C16 -179.5(6) C37 N1 C1 C2 -175.9(5) C37 N1 C1 C18 0.1(8) C37 C38 C39 C40 -152.9(7) C37 C38 C39 C41 82.4(9) C37 C38 C42 C43 0.8(11) C37 C45 C46 C47 -135.6(8) C37 C45 C46 C48 117(2) C37 C45 C46 C48A 89.3(13) C38 C37 C45 C44 -3.2(10) C38 C37 C45 C46 171.7(7) C38 C42 C43 C44 -2.7(14) C39 C38 C42 C43 177.4(8) C42 C38 C39 C40 30.7(10) C42 C38 C39 C41 -94.0(9) C42 C43 C44 C45 1.6(14) C43 C44 C45 C37 1.3(12) C43 C44 C45 C46 -173.8(9) C44 C45 C46 C47 39.3(12) C44 C45 C46 C48 -68(2) C44 C45 C46 C48A -95.9(13) C45 C37 C38 C39 -174.5(7) C45 C37 C38 C42 2.1(9)