#------------------------------------------------------------------------------ #$Date: 2019-12-13 11:04:13 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245052 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556555.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_1556555 loop_ _publ_author_name 'Sunada, Y.' 'Taniyama, N.' 'Shimamoto, K.' 'Kyushin, S.' 'Nagashima, H.' _publ_section_title ; Construction of a Planar Tetrapalladium Cluster by the Reaction of Palladium(0) Bis(isocyanide) with Cyclic Tetrasilane ; _journal_name_full Inorganics _journal_page_first 84 _journal_paper_doi 10.3390/inorganics5040084 _journal_volume 5 _journal_year 2017 _chemical_formula_moiety 'C51 H100 N6 Pd4 Si3' _chemical_formula_sum 'C51 H100 N6 Pd4 Si3' _chemical_formula_weight 1307.25 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 89.593(12) _cell_angle_beta 63.724(6) _cell_angle_gamma 81.301(11) _cell_formula_units_Z 2 _cell_length_a 14.505(3) _cell_length_b 15.339(4) _cell_length_c 15.655(4) _cell_measurement_reflns_used 9427 _cell_measurement_temperature 193 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.12 _cell_volume 3080.2(13) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.2.5' _computing_publication_material 'CrystalStructure 4.2.5 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 193 _diffrn_detector_area_resol_mean 7.111 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 38434 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.495 _diffrn_reflns_theta_min 3.080 _diffrn_standards_interval_count . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1348.00 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.05 _refine_diff_density_min -0.67 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 577 _refine_ls_number_reflns 14053 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0453P)^2^+1.3612P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.1016 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11359 _reflns_number_total 14053 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file Inorganics-2017-5-84.cif _cod_data_source_block Pd4Si3(NHCiPr)3 _cod_database_code 1556555 _shelxl_version_number 2014-1 _shelx_res_file ; TITL Pd4Si3NHC CELL 0.71075 14.50450 15.33920 15.65520 89.59320 63.72410 81.30140 ZERR 2 0.00310 0.00400 0.00390 0.01150 0.00640 0.01100 LATT 1 SFAC C H N PD SI UNIT 102 26 12 8 6 L.S. 50 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -79.8 ACTA SIZE 0.050 0.050 0.010 WGHT 0.045300 1.361200 FVAR 0.87433 PD1 4 0.380847 0.888102 0.277409 11.00000 0.02255 0.02815 = 0.02228 0.00373 -0.00871 -0.00810 PD2 4 0.237357 0.754869 0.566770 11.00000 0.02381 0.02657 = 0.02012 0.00252 -0.00955 -0.00437 PD3 4 0.151840 0.689544 0.321535 11.00000 0.02231 0.02508 = 0.02494 -0.00119 -0.01116 -0.00496 PD4 4 0.249080 0.783444 0.392195 11.00000 0.02209 0.02603 = 0.01997 0.00278 -0.00957 -0.00775 SI1 5 0.343687 0.860128 0.437324 11.00000 0.02001 0.02197 = 0.02479 -0.00173 -0.00997 -0.00233 SI2 5 0.142458 0.697972 0.495293 11.00000 0.01989 0.02605 = 0.02680 0.00502 -0.00960 -0.00460 SI3 5 0.260364 0.794911 0.243970 11.00000 0.02899 0.02919 = 0.02284 0.00241 -0.01224 -0.00676 N1 3 0.601157 0.927064 0.154220 11.00000 0.02455 0.03837 = 0.02406 0.00592 -0.00846 -0.01036 N2 3 0.502073 1.047857 0.230064 11.00000 0.02942 0.03279 = 0.02619 0.00819 -0.01145 -0.01191 N3 3 0.276275 0.648704 0.720518 11.00000 0.03257 0.02722 = 0.02723 0.00210 -0.01467 -0.00103 N4 3 0.141237 0.749629 0.786964 11.00000 0.03472 0.02998 = 0.02349 0.00511 -0.01025 -0.00525 N5 3 0.005710 0.649827 0.234981 11.00000 0.02852 0.03442 = 0.02512 0.00013 -0.01295 -0.00914 N6 3 0.137325 0.545562 0.191851 11.00000 0.03229 0.02221 = 0.02951 -0.00232 -0.01308 -0.00420 C1 1 0.500891 0.960923 0.215721 11.00000 0.02635 0.03154 = 0.02133 0.00472 -0.00993 -0.00715 C2 1 0.664601 0.993090 0.130410 11.00000 0.03270 0.05619 = 0.02263 0.00934 -0.01162 -0.02488 C3 1 0.602384 1.068307 0.178526 11.00000 0.03511 0.04566 = 0.02671 0.00697 -0.01105 -0.01854 C4 1 0.627912 0.835695 0.113894 11.00000 0.02780 0.03612 = 0.03653 -0.00083 -0.01211 -0.00463 AFIX 13 H4 2 0.565829 0.807087 0.152080 11.00000 -1.20000 AFIX 0 C5 1 0.719030 0.781812 0.125258 11.00000 0.03745 0.05336 = 0.05407 0.00226 -0.01419 0.00150 AFIX 33 H5A 2 0.701758 0.780413 0.193216 11.00000 -1.20000 H5B 2 0.781456 0.809121 0.092066 11.00000 -1.20000 H5C 2 0.732285 0.721360 0.097778 11.00000 -1.20000 AFIX 0 C6 1 0.642111 0.831228 0.011679 11.00000 0.04447 0.05784 = 0.03165 -0.00370 -0.01320 -0.01675 AFIX 33 H6A 2 0.583592 0.869368 0.007868 11.00000 -1.20000 H6B 2 0.644439 0.770154 -0.008146 11.00000 -1.20000 H6C 2 0.707449 0.851286 -0.030545 11.00000 -1.20000 AFIX 0 C7 1 0.404076 1.108209 0.286624 11.00000 0.03896 0.03496 = 0.03439 0.00469 -0.01389 -0.01288 AFIX 13 H7 2 0.350057 1.070145 0.320112 11.00000 -1.20000 AFIX 0 C8 1 0.407219 1.164960 0.363686 11.00000 0.05818 0.04779 = 0.03989 -0.00182 -0.01536 -0.01762 AFIX 33 H8A 2 0.461508 1.201772 0.334361 11.00000 -1.20000 H8B 2 0.422722 1.126913 0.407809 11.00000 -1.20000 H8C 2 0.339463 1.202939 0.398784 11.00000 -1.20000 AFIX 0 C9 1 0.368922 1.162279 0.221471 11.00000 0.05473 0.04777 = 0.05350 0.00884 -0.02602 -0.00191 AFIX 33 H9A 2 0.358801 1.122484 0.178790 11.00000 -1.20000 H9B 2 0.422175 1.197654 0.183458 11.00000 -1.20000 H9C 2 0.303117 1.201574 0.260145 11.00000 -1.20000 AFIX 0 C10 1 0.779388 0.976373 0.067264 11.00000 0.03801 0.06769 = 0.04205 0.00255 -0.01188 -0.02377 AFIX 33 H10A 2 0.816226 0.990031 0.103709 11.00000 -1.20000 H10B 2 0.795672 1.013988 0.013284 11.00000 -1.20000 H10C 2 0.801560 0.914135 0.043378 11.00000 -1.20000 AFIX 0 C11 1 0.632334 1.156592 0.180473 11.00000 0.05287 0.05411 = 0.04603 0.00642 -0.01637 -0.02686 AFIX 33 H11A 2 0.663303 1.176300 0.115483 11.00000 -1.20000 H11B 2 0.683154 1.152504 0.206305 11.00000 -1.20000 H11C 2 0.570271 1.199122 0.220914 11.00000 -1.20000 AFIX 0 C12 1 0.215323 0.715252 0.700422 11.00000 0.02885 0.02968 = 0.01499 0.00289 -0.00575 -0.00678 C13 1 0.239171 0.645103 0.819584 11.00000 0.04503 0.03945 = 0.02532 0.01217 -0.01982 -0.01136 C14 1 0.154302 0.706666 0.860550 11.00000 0.04662 0.04485 = 0.02136 0.00821 -0.01306 -0.00956 C15 1 0.370727 0.598435 0.642428 11.00000 0.03805 0.02786 = 0.03375 -0.00271 -0.01928 0.00257 AFIX 13 H15 2 0.368146 0.615494 0.581658 11.00000 -1.20000 AFIX 0 C16 1 0.373360 0.499604 0.644475 11.00000 0.07800 0.02856 = 0.05613 0.00027 -0.03297 0.00264 AFIX 33 H16A 2 0.312609 0.484882 0.639115 11.00000 -1.20000 H16B 2 0.371889 0.480009 0.704719 11.00000 -1.20000 H16C 2 0.437289 0.469827 0.590918 11.00000 -1.20000 AFIX 0 C17 1 0.467972 0.626781 0.638666 11.00000 0.03754 0.06525 = 0.05851 -0.00729 -0.02030 -0.00400 AFIX 33 H17A 2 0.471289 0.615480 0.699017 11.00000 -1.20000 H17B 2 0.465876 0.690037 0.628595 11.00000 -1.20000 H17C 2 0.529677 0.593168 0.585953 11.00000 -1.20000 AFIX 0 C18 1 0.059109 0.822682 0.794409 11.00000 0.03247 0.03496 = 0.02834 -0.00164 -0.00794 -0.00201 AFIX 13 H18 2 0.077142 0.839238 0.727632 11.00000 -1.20000 AFIX 0 C19 1 -0.046785 0.794645 0.831922 11.00000 0.03416 0.05797 = 0.03944 0.00163 -0.00912 -0.00842 AFIX 33 H19A 2 -0.066157 0.773544 0.895892 11.00000 -1.20000 H19B 2 -0.044171 0.747040 0.789088 11.00000 -1.20000 H19C 2 -0.098656 0.845179 0.835099 11.00000 -1.20000 AFIX 0 C20 1 0.058962 0.904954 0.848237 11.00000 0.04745 0.03633 = 0.04148 -0.00347 -0.01278 -0.00174 AFIX 33 H20A 2 0.126686 0.924614 0.815421 11.00000 -1.20000 H20B 2 0.046221 0.891237 0.913383 11.00000 -1.20000 H20C 2 0.003882 0.951997 0.850576 11.00000 -1.20000 AFIX 0 C21 1 0.288696 0.580140 0.865632 11.00000 0.07397 0.05459 = 0.04587 0.01407 -0.03816 -0.00298 AFIX 33 H21A 2 0.238975 0.541922 0.903591 11.00000 -1.20000 H21B 2 0.308411 0.612231 0.907238 11.00000 -1.20000 H21C 2 0.350983 0.543922 0.816081 11.00000 -1.20000 AFIX 0 C22 1 0.086414 0.729756 0.965381 11.00000 0.07108 0.08166 = 0.02228 0.00859 -0.01699 -0.00457 AFIX 33 H22A 2 0.127973 0.749405 0.994421 11.00000 -1.20000 H22B 2 0.057928 0.677596 0.996064 11.00000 -1.20000 H22C 2 0.029091 0.777316 0.973991 11.00000 -1.20000 AFIX 0 C23 1 0.095953 0.625322 0.242638 11.00000 0.02345 0.02757 = 0.02287 -0.00220 -0.00872 -0.00593 C24 1 -0.009008 0.585925 0.181186 11.00000 0.04011 0.04133 = 0.03166 0.00423 -0.02029 -0.02076 C25 1 0.073411 0.521222 0.154081 11.00000 0.04720 0.03119 = 0.03285 -0.00295 -0.02153 -0.01505 C26 1 -0.061476 0.735610 0.280926 11.00000 0.02837 0.03738 = 0.02833 -0.00005 -0.01329 -0.00306 AFIX 13 H26 2 -0.029274 0.760948 0.317829 11.00000 -1.20000 AFIX 0 C27 1 -0.170678 0.725387 0.352954 11.00000 0.02929 0.06632 = 0.04336 0.00388 -0.01363 -0.00157 AFIX 33 H27A 2 -0.167034 0.688489 0.403084 11.00000 -1.20000 H27B 2 -0.204365 0.697336 0.320858 11.00000 -1.20000 H27C 2 -0.211258 0.783724 0.381502 11.00000 -1.20000 AFIX 0 C28 1 -0.060703 0.801208 0.208129 11.00000 0.04464 0.04514 = 0.04244 0.00135 -0.02558 -0.00397 AFIX 33 H28A 2 -0.087072 0.777438 0.166881 11.00000 -1.20000 H28B 2 0.010724 0.811684 0.169223 11.00000 -1.20000 H28C 2 -0.105260 0.857008 0.241112 11.00000 -1.20000 AFIX 0 C29 1 0.233772 0.494692 0.188506 11.00000 0.03414 0.02826 = 0.03713 -0.00459 -0.01217 -0.00197 AFIX 13 H29 2 0.263178 0.535735 0.215425 11.00000 -1.20000 AFIX 0 C30 1 0.210525 0.418513 0.253512 11.00000 0.05539 0.04391 = 0.06178 0.01020 -0.03005 -0.00428 AFIX 33 H30A 2 0.176932 0.378300 0.232582 11.00000 -1.20000 H30B 2 0.163900 0.441732 0.319291 11.00000 -1.20000 H30C 2 0.275762 0.386424 0.250550 11.00000 -1.20000 AFIX 0 C31 1 0.317449 0.464869 0.087848 11.00000 0.04674 0.04864 = 0.05119 -0.01364 -0.00945 0.00198 AFIX 33 H31A 2 0.335506 0.516676 0.050662 11.00000 -1.20000 H31B 2 0.291162 0.426161 0.057308 11.00000 -1.20000 H31C 2 0.379579 0.432560 0.090732 11.00000 -1.20000 AFIX 0 C32 1 -0.101470 0.592483 0.161246 11.00000 0.04677 0.06342 = 0.05694 0.00266 -0.03366 -0.02066 AFIX 33 H32A 2 -0.138091 0.542610 0.187298 11.00000 -1.20000 H32B 2 -0.078238 0.591090 0.092120 11.00000 -1.20000 H32C 2 -0.148683 0.648049 0.191251 11.00000 -1.20000 AFIX 0 C33 1 0.094721 0.435875 0.096225 11.00000 0.09513 0.03577 = 0.06673 -0.00639 -0.04929 -0.01163 AFIX 33 H33A 2 0.097281 0.448993 0.033930 11.00000 -1.20000 H33B 2 0.039040 0.401348 0.130144 11.00000 -1.20000 H33C 2 0.161685 0.401847 0.087023 11.00000 -1.20000 AFIX 0 C34 1 0.470335 0.812645 0.443522 11.00000 0.02473 0.02873 = 0.02962 0.00577 -0.01260 -0.00506 AFIX 13 H34 2 0.451404 0.801185 0.511769 11.00000 -1.20000 AFIX 0 C35 1 0.519633 0.724256 0.385947 11.00000 0.02776 0.02897 = 0.06478 -0.00039 -0.01931 0.00317 AFIX 33 H35A 2 0.580031 0.698690 0.395829 11.00000 -1.20000 H35B 2 0.542162 0.733167 0.318009 11.00000 -1.20000 H35C 2 0.468455 0.683987 0.406923 11.00000 -1.20000 AFIX 0 C36 1 0.549751 0.876212 0.413656 11.00000 0.01993 0.04086 = 0.04383 -0.00136 -0.01570 -0.00454 AFIX 33 H36A 2 0.568732 0.890513 0.347456 11.00000 -1.20000 H36B 2 0.612232 0.848168 0.418891 11.00000 -1.20000 H36C 2 0.519028 0.930569 0.455540 11.00000 -1.20000 AFIX 0 C37 1 0.294796 0.970502 0.512016 11.00000 0.02726 0.02487 = 0.02838 -0.00207 -0.00941 -0.00611 AFIX 13 H37 2 0.347604 1.009916 0.479854 11.00000 -1.20000 AFIX 0 C38 1 0.283860 0.960852 0.613279 11.00000 0.05835 0.03871 = 0.03014 -0.00595 -0.01254 -0.01297 AFIX 33 H38A 2 0.350076 0.930984 0.610157 11.00000 -1.20000 H38B 2 0.228969 0.925876 0.648222 11.00000 -1.20000 H38C 2 0.265530 1.019517 0.646312 11.00000 -1.20000 AFIX 0 C39 1 0.191547 1.015615 0.514931 11.00000 0.03484 0.03722 = 0.06015 -0.01772 -0.01791 0.00944 AFIX 33 H39A 2 0.171215 1.074180 0.548570 11.00000 -1.20000 H39B 2 0.137327 0.979635 0.548482 11.00000 -1.20000 H39C 2 0.200096 1.021869 0.449605 11.00000 -1.20000 AFIX 0 C40 1 0.160633 0.572155 0.495331 11.00000 0.04205 0.02454 = 0.05292 0.00391 -0.02971 -0.00800 AFIX 13 H40 2 0.122179 0.551838 0.461713 11.00000 -1.20000 AFIX 0 C41 1 0.274411 0.529942 0.438905 11.00000 0.05148 0.02936 = 0.06467 -0.00528 -0.03200 0.01041 AFIX 33 H41A 2 0.279556 0.465546 0.434307 11.00000 -1.20000 H41B 2 0.314458 0.545609 0.471436 11.00000 -1.20000 H41C 2 0.302466 0.551493 0.374647 11.00000 -1.20000 AFIX 0 C42 1 0.113447 0.538375 0.596188 11.00000 0.06329 0.03702 = 0.06330 0.02271 -0.02715 -0.01606 AFIX 33 H42A 2 0.151558 0.554135 0.630610 11.00000 -1.20000 H42B 2 0.118772 0.473971 0.591400 11.00000 -1.20000 H42C 2 0.039968 0.565510 0.630775 11.00000 -1.20000 AFIX 0 C43 1 -0.004229 0.736624 0.573543 11.00000 0.02330 0.03917 = 0.02583 0.00643 -0.00852 -0.00401 AFIX 13 H43 2 -0.022135 0.714119 0.638178 11.00000 -1.20000 AFIX 0 C44 1 -0.069844 0.698239 0.533859 11.00000 0.02623 0.08306 = 0.03731 0.01165 -0.01348 -0.01896 AFIX 33 H44A 2 -0.055900 0.721042 0.471415 11.00000 -1.20000 H44B 2 -0.143947 0.715435 0.577826 11.00000 -1.20000 H44C 2 -0.051753 0.633633 0.526896 11.00000 -1.20000 AFIX 0 C45 1 -0.031327 0.837469 0.585968 11.00000 0.03255 0.05227 = 0.05552 0.00457 -0.01115 0.00729 AFIX 33 H45A 2 -0.104042 0.854943 0.633501 11.00000 -1.20000 H45B 2 -0.021847 0.861100 0.524816 11.00000 -1.20000 H45C 2 0.014539 0.861000 0.607551 11.00000 -1.20000 AFIX 0 C46 1 0.375186 0.742226 0.127346 11.00000 0.04219 0.05455 = 0.02536 -0.00351 -0.00820 -0.01213 C47 1 0.343512 0.716083 0.051779 11.00000 0.07475 0.09166 = 0.02844 -0.01011 -0.01779 -0.03280 AFIX 33 H47A 2 0.301923 0.668534 0.073936 11.00000 -1.20000 H47B 2 0.406127 0.695526 -0.007718 11.00000 -1.20000 H47C 2 0.302085 0.767349 0.040447 11.00000 -1.20000 AFIX 0 C48 1 0.441061 0.663589 0.147036 11.00000 0.03103 0.06300 = 0.04831 -0.02260 0.00118 -0.00676 AFIX 33 H48A 2 0.504449 0.643100 0.088139 11.00000 -1.20000 H48B 2 0.400536 0.615396 0.169507 11.00000 -1.20000 H48C 2 0.460134 0.682212 0.195997 11.00000 -1.20000 AFIX 0 C49 1 0.183301 0.887409 0.206496 11.00000 0.04588 0.03999 = 0.04235 0.01810 -0.02795 -0.01613 C50 1 0.252715 0.954128 0.150047 11.00000 0.08242 0.06040 = 0.08109 0.04089 -0.05778 -0.03436 AFIX 33 H50A 2 0.277609 0.981723 0.190392 11.00000 -1.20000 H50B 2 0.212405 0.999749 0.130295 11.00000 -1.20000 H50C 2 0.312477 0.923538 0.093392 11.00000 -1.20000 AFIX 0 C51 1 0.089639 0.933522 0.294078 11.00000 0.06086 0.03727 = 0.07078 0.00223 -0.04307 0.00700 AFIX 33 H51A 2 0.049088 0.978893 0.274308 11.00000 -1.20000 H51B 2 0.113381 0.961286 0.335259 11.00000 -1.20000 H51C 2 0.045922 0.890188 0.329265 11.00000 -1.20000 AFIX 0 HKLF 4 REM Pd4Si3NHC REM R1 = 0.0439 for 11359 Fo > 4sig(Fo) and 0.0585 for all 14053 data REM 577 parameters refined using 0 restraints END WGHT 0.0453 1.3611 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.047, deepest hole -0.669, 1-sigma level 0.110 Q1 1 0.6380 1.2281 0.2784 11.00000 0.05 1.05 Q2 1 0.4605 0.9528 0.5255 11.00000 0.05 1.02 Q3 1 0.1321 0.5732 0.7591 11.00000 0.05 0.96 Q4 1 0.0214 0.5876 0.4378 11.00000 0.05 0.95 Q5 1 0.2177 0.6396 1.0053 11.00000 0.05 0.91 Q6 1 0.3951 0.9164 0.1021 11.00000 0.05 0.87 Q7 1 0.0051 0.5546 0.6159 11.00000 0.05 0.85 Q8 1 0.4794 0.9777 0.3432 11.00000 0.05 0.84 Q9 1 0.1606 0.8632 0.1618 11.00000 0.05 0.82 Q10 1 0.1623 0.7151 0.1504 11.00000 0.05 0.80 Q11 1 0.2972 0.8222 0.0267 11.00000 0.05 0.79 Q12 1 0.4171 0.7932 0.1054 11.00000 0.05 0.77 Q13 1 0.1122 0.6543 0.6756 11.00000 0.05 0.75 Q14 1 0.3361 0.8461 0.6285 11.00000 0.05 0.74 Q15 1 0.1242 0.6635 0.5059 11.00000 0.05 0.69 Q16 1 0.3618 0.8726 0.4547 11.00000 0.05 0.67 Q17 1 0.2452 0.7833 0.4195 11.00000 0.05 0.63 Q18 1 0.2811 0.7954 0.2027 11.00000 0.05 0.61 Q19 1 0.1039 0.6566 0.2795 11.00000 0.05 0.58 Q20 1 0.2253 0.7585 0.5594 11.00000 0.05 0.57 Q21 1 0.2591 0.8039 0.3834 11.00000 0.05 0.56 Q22 1 0.0640 0.6283 1.0804 11.00000 0.05 0.56 Q23 1 0.5817 1.2127 0.1582 11.00000 0.05 0.55 Q24 1 0.0380 0.4321 0.0832 11.00000 0.05 0.53 Q25 1 0.3768 0.8027 0.5484 11.00000 0.05 0.53 ; _shelx_res_checksum 71703 _shelx_hkl_file ; 0 0 3 2202.94 88.22 0 0 3 2359.84 77.72 0 0 3 2400.22 86.40 0 0 -3 2337.39 93.42 0 0 -3 2318.27 88.21 0 0 -3 2354.60 95.36 0 0 4 2296.66 85.39 0 0 4 2249.95 67.60 0 0 4 2241.04 86.56 0 0 -4 2417.32 133.96 0 0 -4 2275.60 68.96 0 0 -4 2234.65 92.50 0 0 5 2287.40 137.97 0 0 5 2330.12 71.86 0 0 5 2504.97 100.15 0 0 -5 2508.74 118.60 0 0 -5 2406.16 74.84 0 0 -5 2469.52 90.50 0 0 6 1444.54 84.64 0 0 6 1502.28 86.50 0 0 6 1375.92 120.67 0 0 -6 1459.35 102.02 0 0 -6 1310.48 71.24 0 0 -6 1404.02 98.62 0 0 7 9516.56 308.53 0 0 -7 9340.76 311.22 0 0 -7 9391.01 297.35 0 0 -7 9632.06 324.68 0 0 8 1061.79 56.42 0 0 -8 1066.36 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613.52 152.53 -9 -12 7 487.96 128.78 9 12 -6 801.69 186.28 -9 -12 6 481.73 219.63 9 12 -5 65.20 102.28 -9 -12 5 12.86 23.82 9 12 -4 2931.04 178.41 -9 -12 4 2646.85 257.80 9 12 -3 3346.94 199.95 -9 -12 3 3196.01 170.84 9 12 -2 206.33 106.03 -9 -12 2 145.45 78.36 9 12 -1 128.24 65.80 -9 -12 1 165.44 77.45 9 12 0 82.83 69.29 -9 -12 0 82.06 85.02 9 12 1 3479.84 248.18 9 12 1 3177.36 131.23 -9 -12 -1 3482.67 223.98 9 12 2 5897.28 297.93 9 12 2 5596.07 191.07 -9 -12 -2 6479.72 331.45 9 12 3 496.13 122.78 9 12 3 398.61 99.98 -9 -12 -3 464.97 192.15 9 12 4 965.22 89.46 -9 -12 -4 902.24 108.41 -9 -12 -4 794.41 262.65 9 12 5 606.35 100.22 -9 -12 -5 341.22 103.33 -9 -12 -5 477.43 127.44 9 12 6 474.82 137.14 -9 -12 -6 430.21 116.39 -9 -12 -6 453.36 130.26 9 12 7 1662.79 136.87 -9 -12 -7 1519.60 82.40 -9 -12 -7 1575.63 188.35 9 12 8 54.99 55.47 -9 -12 -8 60.72 34.22 -9 -12 -8 83.39 79.31 9 12 9 1021.75 222.11 -9 -12 -9 683.22 114.62 -9 -12 -9 787.61 228.38 9 12 10 290.63 102.25 -9 -12 -10 167.79 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1024.66 267.36 -9 -14 4 1117.02 171.23 9 14 -3 5137.52 430.89 -9 -14 3 5779.21 318.66 9 14 -2 3928.88 456.18 -9 -14 2 3812.83 218.89 9 14 -1 272.25 103.98 -9 -14 1 110.00 72.86 9 14 0 2691.63 352.08 -9 -14 0 2775.28 163.89 9 14 1 1223.99 134.95 -9 -14 -1 1215.06 191.99 9 14 2 188.13 94.49 -9 -14 -2 146.57 56.68 9 14 3 985.52 273.33 -9 -14 -3 730.26 182.29 9 14 4 2260.25 139.32 -9 -14 -4 2409.82 209.82 9 14 5 735.83 229.84 -9 -14 -5 968.29 105.25 9 14 6 44.98 44.98 -9 -14 -6 15.37 20.15 -9 -14 -6 -32.26 72.38 9 14 7 -0.36 67.42 -9 -14 -7 106.75 55.03 -9 -14 -7 198.22 77.40 9 14 8 516.98 145.67 -9 -14 -8 543.20 85.53 -9 -14 -8 444.87 216.98 9 14 9 54.97 36.93 -9 -14 -9 91.48 54.50 -9 -14 -9 173.51 69.69 9 14 10 86.20 59.71 -9 -14 -10 22.44 39.33 -9 -14 -10 32.25 57.96 9 14 11 57.82 37.78 -9 -14 -11 78.97 55.99 -9 -14 -11 61.99 41.09 9 14 12 -3.26 55.73 -9 -14 -12 119.53 55.01 -9 -14 -12 43.67 53.52 9 14 13 12.49 60.44 -9 -14 -13 5.24 51.70 -9 -14 -13 47.68 83.07 9 14 14 1265.64 164.40 -9 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3 2382.26 157.31 10 11 -2 86.09 96.56 -10 -11 2 178.97 89.53 10 11 -1 80.01 66.94 10 11 -1 19.30 26.64 -10 -11 1 38.08 83.21 10 11 0 7.21 44.83 10 11 0 12.88 26.88 -10 -11 0 85.56 78.15 10 11 1 4292.65 250.08 10 11 1 3505.16 192.11 -10 -11 -1 3932.63 370.00 10 11 2 5708.81 393.19 10 11 2 5379.18 196.46 -10 -11 -2 5388.06 237.33 10 11 3 61.93 37.86 10 11 3 39.64 43.65 -10 -11 -3 99.67 71.17 10 11 4 758.05 223.18 -10 -11 -4 394.60 113.18 -10 -11 -4 472.36 164.51 10 11 5 79.35 52.27 -10 -11 -5 17.78 22.89 -10 -11 -5 95.84 70.08 10 11 6 165.34 67.43 -10 -11 -6 346.03 86.25 -10 -11 -6 258.91 127.03 10 11 7 955.18 192.22 -10 -11 -7 981.70 89.90 -10 -11 -7 917.89 357.76 10 11 8 15.48 51.41 -10 -11 -8 35.25 49.23 -10 -11 -8 41.17 45.95 10 11 9 785.43 232.19 -10 -11 -9 798.84 89.97 -10 -11 -9 1024.14 101.12 10 11 10 13.39 39.85 -10 -11 -10 34.12 46.66 -10 -11 -10 13.00 55.56 10 11 11 1791.30 135.51 -10 -11 -11 1803.31 219.32 -10 -11 -11 1879.95 223.97 10 11 12 1760.99 397.12 -10 -11 -12 2008.19 254.91 -10 -11 -12 1813.11 201.64 10 11 13 114.06 73.29 -10 -11 -13 216.15 74.73 -10 -11 -13 256.23 80.74 10 11 14 3389.64 172.57 -10 -11 -14 3664.62 152.82 -10 -11 -14 3232.92 346.50 10 11 15 895.94 220.82 -10 -11 -15 1001.79 211.03 -10 -11 -15 678.17 266.87 10 11 16 93.28 99.90 -10 -11 -16 -33.33 62.70 -10 -11 -16 99.43 74.72 10 12 -7 1633.09 195.21 -10 -12 7 1487.01 100.19 10 12 -6 437.29 164.06 -10 -12 6 246.91 104.07 10 12 -5 1086.01 334.11 -10 -12 5 1104.73 228.11 10 12 -4 884.22 214.29 -10 -12 4 863.17 108.48 10 12 -3 554.12 165.01 -10 -12 3 337.94 169.29 10 12 -2 2002.80 161.61 -10 -12 2 1695.89 282.32 10 12 -1 476.54 110.80 -10 -12 1 388.86 126.71 10 12 0 114.89 89.63 -10 -12 0 142.71 163.64 10 12 1 761.06 164.72 10 12 1 525.33 101.68 -10 -12 -1 784.72 122.40 10 12 2 1572.00 359.04 10 12 2 1250.04 84.95 -10 -12 -2 1289.96 247.22 10 12 3 1629.73 328.17 10 12 3 1498.11 64.71 -10 -12 -3 1474.24 171.61 10 12 4 2895.98 195.75 -10 -12 -4 2889.17 128.67 -10 -12 -4 3471.53 387.65 10 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126.27 11 14 11 52.15 42.04 -11 -14 -11 57.43 51.67 -11 -14 -11 15.53 49.82 11 14 12 1056.03 307.57 -11 -14 -12 1247.55 209.56 -11 -14 -12 1222.78 221.66 11 14 13 624.58 266.61 -11 -14 -13 699.18 278.90 -11 -14 -13 947.42 219.73 11 15 -3 106.21 83.05 -11 -15 3 91.17 61.82 11 15 -2 -64.43 66.64 -11 -15 2 219.64 75.39 11 15 -1 150.97 62.11 -11 -15 1 205.13 96.29 11 15 0 124.95 74.79 -11 -15 0 -12.90 63.09 11 15 1 49.98 27.51 -11 -15 -1 129.29 87.96 11 15 2 371.55 139.66 -11 -15 -2 445.01 120.19 11 15 3 201.84 82.20 -11 -15 -3 79.57 71.96 11 15 4 40.61 33.35 -11 -15 -4 76.67 63.77 11 15 5 606.58 140.08 -11 -15 -5 362.54 255.63 11 15 6 1112.57 305.33 -11 -15 -6 1225.94 449.10 11 15 7 88.02 106.10 -11 -15 -7 52.66 68.96 11 15 8 2150.61 350.72 -11 -15 -8 1722.61 233.07 11 15 9 4990.95 435.46 -11 -15 -9 5508.53 360.79 11 15 10 421.86 169.52 -11 -15 -10 551.63 112.67 11 15 11 1626.68 307.36 -11 -15 -11 1246.48 350.50 11 15 12 359.86 206.52 -11 -15 -12 430.23 142.66 -11 -15 -12 605.40 201.68 11 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242.97 159.24 -11 -17 -8 226.17 48.05 12 -13 5 51.41 18.96 -12 13 -5 217.43 77.02 12 -13 6 150.73 93.11 -12 13 -6 4.85 63.92 12 -13 7 1065.72 179.71 12 -13 8 190.86 99.55 12 -13 8 85.49 83.16 12 -13 9 89.61 52.32 12 -13 9 27.21 44.19 12 -12 2 32.54 72.12 -12 12 -2 39.30 62.04 12 -12 3 660.66 335.93 -12 12 -3 543.40 213.49 12 -12 4 726.31 404.57 -12 12 -4 1075.40 353.88 12 -12 5 168.22 132.03 -12 12 -5 158.44 78.75 12 -12 6 36.11 59.15 -12 12 -6 151.56 78.48 -12 12 -7 260.71 107.13 12 -12 8 28.78 41.50 -12 12 -8 28.91 64.52 12 -12 9 45.34 64.45 -12 12 -9 272.56 93.20 12 -12 10 813.41 267.12 12 -12 10 778.69 134.97 12 -12 11 2629.66 268.79 12 -12 11 2423.13 168.25 12 -12 12 242.73 74.24 12 -11 0 167.36 139.03 -12 11 0 430.07 189.31 12 -11 1 218.89 98.96 -12 11 -1 208.77 150.67 12 -11 2 177.65 100.34 -12 11 -2 204.54 131.84 12 -11 3 111.89 91.98 -12 11 -3 181.84 103.56 12 -11 4 184.56 101.62 -12 11 -4 276.28 109.60 12 -11 5 29.56 34.85 -12 11 -5 168.86 102.15 12 -11 6 137.01 67.21 -12 11 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12 -10 13 -6.61 40.81 12 -10 14 1598.05 137.12 12 -10 14 2053.74 147.86 12 -10 15 1314.38 202.18 12 -10 15 1503.62 180.79 12 -9 -3 194.28 80.24 -12 9 3 41.03 91.28 12 -9 -2 2605.32 259.55 -12 9 2 2436.03 224.07 12 -9 -1 1644.80 362.66 -12 9 1 2054.60 264.77 12 -9 0 53.09 82.14 -12 9 0 87.27 77.15 -12 9 -1 305.08 138.24 12 -9 2 23.53 70.79 -12 9 -2 248.49 143.61 12 -9 3 243.06 93.71 -12 9 -3 124.01 93.27 12 -9 4 117.34 77.20 -12 9 -4 206.58 125.15 12 -9 5 2874.24 218.12 -12 9 -5 3109.59 313.56 12 -9 6 2391.96 149.89 -12 9 -6 2034.90 929.45 12 -9 7 140.51 88.41 -12 9 -7 82.82 51.91 12 -9 8 963.61 180.91 -12 9 -8 845.55 300.04 12 -9 9 74.56 44.02 -12 9 -9 22.97 29.33 12 -9 10 94.47 51.22 -12 9 -10 96.35 56.15 12 -9 11 94.99 66.76 12 -9 11 27.02 64.14 -12 9 -11 37.47 46.30 12 -9 12 10.83 53.76 12 -9 12 49.83 25.60 -12 9 -12 78.94 67.24 12 -9 13 216.90 130.17 12 -9 13 283.76 165.62 12 -9 14 95.63 61.54 12 -9 14 167.51 92.04 12 -9 15 392.71 118.66 12 -9 15 179.45 146.71 12 -9 16 430.80 124.12 -12 9 -16 417.33 119.95 12 -8 -4 46.87 58.75 -12 8 4 52.18 48.98 12 -8 -3 410.75 110.88 -12 8 3 331.41 178.13 12 -8 -2 71.68 77.23 -12 8 2 55.47 52.75 12 -8 -1 414.06 86.04 -12 8 1 289.94 117.42 12 -8 0 104.61 81.36 -12 8 0 104.64 95.26 12 -8 1 519.16 199.35 -12 8 -1 276.82 149.06 12 -8 2 2621.30 164.62 -12 8 -2 2573.97 153.06 12 -8 3 1229.03 127.20 -12 8 -3 1505.43 146.25 12 -8 4 -5.91 77.26 -12 8 -4 305.36 108.91 12 -8 5 106.66 64.47 -12 8 -5 -5.08 65.89 12 -8 6 1852.96 304.79 -12 8 -6 2022.42 146.50 12 -8 7 3915.83 344.76 -12 8 -7 4098.59 358.80 12 -8 8 119.20 41.27 12 -8 8 129.50 90.46 -12 8 -8 225.47 85.56 12 -8 9 2656.63 158.13 12 -8 9 2512.11 254.61 -12 8 -9 2837.74 196.07 12 -8 10 2244.14 137.32 12 -8 10 2239.48 116.27 -12 8 -10 2425.01 198.12 12 -8 11 331.49 159.19 12 -8 11 703.71 203.71 -12 8 -11 436.27 143.50 12 -8 12 482.55 211.38 12 -8 12 516.13 139.22 -12 8 -12 495.26 72.97 12 -8 13 314.58 154.19 12 -8 13 416.19 128.35 -12 8 -13 490.65 82.68 12 -8 14 50.69 40.06 12 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-12 6 -9 695.10 156.76 12 -6 10 3366.06 131.04 12 -6 10 3281.56 149.61 -12 6 -10 3026.93 161.80 12 -6 11 403.64 194.79 12 -6 11 701.89 146.80 -12 6 -11 497.18 137.44 12 -6 12 70.67 60.90 -12 6 -12 12.22 44.94 -12 6 -12 163.51 68.84 12 -6 13 30.55 36.30 -12 6 -13 70.04 39.47 -12 6 -13 80.36 48.22 12 -6 14 444.97 185.45 -12 6 -14 555.96 172.39 12 -6 15 58.75 42.39 -12 6 -15 111.44 68.53 12 -6 16 430.25 114.27 -12 6 -16 702.06 125.16 12 -6 17 2751.59 217.23 -12 6 -17 2371.47 849.72 12 -6 18 1595.61 154.38 -12 6 -18 1789.15 178.17 12 -5 -6 846.40 315.52 -12 5 6 1265.66 117.18 12 -5 -5 157.97 90.03 -12 5 5 86.12 76.12 12 -5 -4 1489.21 366.51 -12 5 4 1515.21 112.83 12 -5 -3 1305.15 121.92 -12 5 3 1315.38 346.34 12 -5 -2 120.00 69.82 -12 5 2 236.74 92.60 12 -5 -1 -9.18 51.40 -12 5 1 -27.48 75.83 12 -5 0 1609.97 138.01 -12 5 0 1888.60 149.18 12 -5 1 4218.99 400.73 -12 5 -1 5120.68 213.94 12 -5 2 623.05 56.24 12 -5 2 796.35 216.08 -12 5 -2 607.90 290.15 12 -5 3 253.23 92.31 12 -5 3 300.00 93.68 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68.14 12 -4 -4 90.55 82.53 -12 4 4 42.30 56.16 12 -4 -3 580.45 115.75 -12 4 3 567.58 370.93 12 -4 -2 926.93 248.12 -12 4 2 819.85 285.93 12 -4 -1 1527.73 129.30 -12 4 1 972.79 274.97 12 -4 0 5608.12 173.90 12 -4 0 5982.19 261.02 -12 4 0 5763.76 226.84 12 -4 1 1905.74 75.99 12 -4 1 2047.34 128.58 -12 4 -1 2168.77 154.45 12 -4 2 299.36 81.36 12 -4 2 146.53 119.99 -12 4 -2 336.23 98.95 12 -4 3 1678.98 64.40 12 -4 3 1790.52 123.67 -12 4 -3 1816.19 136.75 12 -4 4 242.78 88.15 12 -4 4 245.82 90.60 -12 4 -4 189.16 151.05 12 -4 5 1443.94 71.83 12 -4 5 1266.25 127.92 -12 4 -5 1243.96 282.38 12 -4 6 976.55 73.88 12 -4 6 926.24 311.11 -12 4 -6 878.93 184.64 12 -4 7 90.52 60.12 12 -4 7 131.05 60.55 -12 4 -7 105.00 74.87 12 -4 8 50.91 47.46 12 -4 8 36.70 33.40 -12 4 -8 104.60 113.76 12 -4 9 119.84 62.56 12 -4 9 110.76 62.26 -12 4 -9 225.16 78.55 12 -4 10 242.94 58.90 -12 4 -10 362.36 66.89 12 -4 11 131.72 62.07 -12 4 -11 97.93 38.99 -12 4 -11 146.27 53.39 12 -4 12 362.68 155.22 -12 4 -12 411.53 107.28 -12 4 -12 323.70 95.46 12 -4 13 135.06 63.65 -12 4 -13 319.97 152.19 -12 4 -13 159.78 53.46 12 -4 14 228.13 94.25 -12 4 -14 109.87 78.50 -12 4 -14 79.81 29.04 12 -4 15 22.90 68.05 -12 4 -15 70.50 50.87 -12 4 -16 178.10 120.58 12 -4 17 2168.19 287.85 -12 4 -17 2135.77 142.32 12 -4 18 2404.86 230.79 -12 4 -18 2882.72 232.81 12 -4 19 285.71 111.78 -12 4 -19 226.66 77.86 12 -3 -7 40.84 77.37 -12 3 7 43.56 76.55 12 -3 -6 79.33 68.79 -12 3 6 105.41 101.27 12 -3 -5 186.96 61.70 -12 3 5 234.57 86.82 12 -3 -4 42.10 75.37 -12 3 4 -28.74 69.82 12 -3 -3 895.37 162.24 -12 3 3 614.97 259.49 12 -3 -2 62.89 41.34 12 -3 -2 285.07 102.88 -12 3 2 48.28 81.48 12 -3 -1 23.95 23.80 12 -3 -1 0.99 57.16 -12 3 1 84.06 78.88 12 -3 0 397.86 52.91 12 -3 0 516.81 135.49 -12 3 0 185.67 147.72 12 -3 1 6671.84 280.35 12 -3 1 7782.46 390.96 -12 3 -1 6798.26 381.49 12 -3 210880.04 399.01 12 -3 2 9045.78 406.36 -12 3 -210647.58 434.25 12 -3 3 169.91 93.41 12 -3 3 291.60 83.35 -12 3 -3 179.38 76.01 12 -3 4 5141.74 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979.22 244.28 -12 -10 -12 775.35 197.72 12 10 13 3450.55 463.88 -12 -10 -13 3500.97 149.36 -12 -10 -13 3481.60 167.14 12 10 14 597.11 98.11 -12 -10 -14 755.51 188.26 -12 -10 -14 828.31 107.93 12 10 15 121.10 63.24 -12 -10 -15 143.18 85.45 -12 -10 -15 61.11 49.91 12 10 16 347.37 159.80 -12 -10 -16 276.73 156.95 -12 -10 -16 412.40 199.55 12 10 17 108.10 96.40 -12 -10 -17 322.09 165.66 12 11 -6 520.18 264.76 -12 -11 6 496.02 224.94 12 11 -5 149.02 103.45 -12 -11 5 10.65 64.00 12 11 -4 2138.54 178.96 -12 -11 4 1797.47 301.09 12 11 -3 4838.68 365.23 -12 -11 3 5092.41 220.61 12 11 -2 710.84 117.40 -12 -11 2 890.82 345.17 12 11 -1 1489.92 151.60 -12 -11 1 1055.48 341.52 12 11 0 1393.01 418.27 -12 -11 0 1637.59 394.69 12 11 1 29.83 65.39 12 11 1 38.38 45.34 -12 -11 -1 87.43 66.56 12 11 2 67.41 59.97 12 11 2 53.61 43.36 -12 -11 -2 118.65 61.98 12 11 3 957.79 103.38 12 11 3 778.45 137.60 -12 -11 -3 804.01 169.27 12 11 4 1416.13 140.89 12 11 4 1237.38 119.89 -12 -11 -4 1348.08 193.22 12 11 5 1209.92 143.82 12 11 5 927.78 222.94 -12 -11 -5 779.68 342.74 12 11 6 -43.98 80.87 -12 -11 -6 51.19 34.28 -12 -11 -6 23.05 85.14 12 11 7 1620.21 356.56 -12 -11 -7 1210.15 174.48 -12 -11 -7 1425.70 147.82 12 11 8 -11.81 80.41 -12 -11 -8 47.48 36.07 -12 -11 -8 120.00 74.06 12 11 9 1063.07 159.80 -12 -11 -9 931.28 103.46 -12 -11 -9 780.97 105.62 12 11 10 -7.77 73.74 -12 -11 -10 22.27 55.42 -12 -11 -10 90.93 72.69 12 11 11 50.54 95.33 -12 -11 -11 122.14 83.87 -12 -11 -11 112.94 72.92 12 11 12 -51.11 67.54 -12 -11 -12 51.08 46.58 -12 -11 -12 -23.50 55.91 12 11 13 658.64 186.04 -12 -11 -13 496.35 154.76 -12 -11 -13 544.56 151.40 12 11 14 1981.53 241.22 -12 -11 -14 1927.43 128.46 -12 -11 -14 1529.36 428.88 12 11 15 1648.43 189.74 -12 -11 -15 1549.92 128.20 -12 -11 -15 1755.47 256.15 12 11 16 75.08 60.85 -12 -11 -16 -17.49 66.19 -12 -11 -16 11.30 40.90 12 12 -5 356.29 114.47 -12 -12 5 261.33 80.29 12 12 -4 102.44 49.25 -12 -12 4 130.83 95.62 12 12 -3 332.49 92.44 -12 -12 3 262.10 146.41 12 12 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12 13 11 200.33 110.17 -12 -13 -11 61.26 74.87 -12 -13 -11 26.12 52.71 12 13 12 2028.28 226.50 -12 -13 -12 2049.96 113.14 -12 -13 -12 1950.23 381.75 12 13 13 1042.16 322.27 -12 -13 -13 990.08 237.03 -12 -13 -13 695.59 266.08 12 13 14 237.05 171.16 -12 -13 -14 73.99 60.87 12 14 -3 33.95 56.85 -12 -14 3 101.16 70.28 12 14 -2 73.82 51.06 -12 -14 2 38.55 68.15 12 14 -1 115.98 80.24 -12 -14 1 22.66 64.28 12 14 0 102.01 75.22 -12 -14 0 36.73 53.06 12 14 1 -6.69 60.56 -12 -14 -1 75.66 96.46 12 14 2 301.61 91.81 -12 -14 -2 159.22 77.44 12 14 3 281.23 106.24 -12 -14 -3 163.20 93.38 12 14 4 329.82 144.81 -12 -14 -4 272.35 134.19 12 14 5 683.16 184.53 -12 -14 -5 926.44 154.62 12 14 6 741.05 223.78 -12 -14 -6 636.26 358.11 12 14 7 -12.81 47.78 -12 -14 -7 -7.39 81.42 12 14 8 2325.17 307.74 -12 -14 -8 2346.35 247.86 12 14 9 5023.36 435.50 -12 -14 -9 5518.14 270.82 12 14 10 339.99 76.45 -12 -14 -10 174.11 117.25 -12 -14 -10 245.96 128.17 12 14 11 808.02 315.69 -12 -14 -11 1016.69 207.70 -12 -14 -11 1025.69 230.41 12 14 12 417.99 181.39 -12 -14 -12 404.94 177.99 -12 -14 -12 443.87 162.70 12 14 13 98.31 85.80 -12 -14 -13 41.57 19.81 -12 -14 -13 127.23 71.40 12 15 -2 35.92 70.65 -12 -15 2 80.31 61.43 12 15 -1 1055.32 262.83 -12 -15 1 1053.00 303.48 12 15 0 1445.39 179.68 -12 -15 0 1632.96 350.96 12 15 1 124.79 121.96 -12 -15 -1 20.20 81.77 12 15 2 699.45 280.27 -12 -15 -2 560.58 198.62 12 15 3 1139.04 369.87 -12 -15 -3 944.11 339.18 12 15 4 339.41 153.03 -12 -15 -4 515.44 114.01 12 15 5 172.51 69.68 -12 -15 -5 108.42 72.74 12 15 6 84.67 62.56 -12 -15 -6 89.49 81.33 12 15 7 248.61 116.11 -12 -15 -7 119.50 83.12 12 15 8 324.48 96.41 -12 -15 -8 190.72 80.00 12 15 9 23.16 72.72 -12 -15 -9 70.92 64.99 12 15 10 634.10 138.11 -12 -15 -10 437.29 173.88 12 15 11 115.98 73.43 -12 -15 -11 85.74 62.98 12 15 12 307.00 187.73 12 16 0 389.45 132.78 -12 -16 0 223.72 135.01 12 16 1 251.34 78.15 -12 -16 -1 366.88 141.18 12 16 2 456.45 135.29 -12 -16 -2 464.21 141.40 12 16 3 412.89 163.48 -12 -16 -3 683.62 235.78 12 16 4 2397.37 321.02 -12 -16 -4 2652.55 467.78 12 16 5 462.28 174.67 -12 -16 -5 517.97 291.52 12 16 6 206.69 82.92 -12 -16 -6 104.20 32.60 12 16 7 203.97 114.59 -12 -16 -7 361.83 90.99 12 16 8 337.77 157.88 -12 -16 -8 326.23 81.89 12 16 9 857.72 225.19 -12 -16 -9 883.81 305.73 12 16 10 431.64 65.44 -12 -16 -10 160.96 177.49 12 17 4 768.26 159.05 -12 -17 -4 911.62 155.75 12 17 5 364.27 101.80 -12 -17 -5 218.31 143.09 12 17 6 605.16 248.39 -12 -17 -6 469.09 205.83 13 -12 6 136.76 102.84 -13 12 -6 87.58 57.63 13 -12 7 211.87 114.81 -13 12 -7 413.07 142.50 13 -12 8 193.53 109.90 -13 12 -8 276.42 88.33 13 -12 9 50.31 95.90 -13 12 -9 36.06 36.47 13 -11 2 238.77 91.04 -13 11 -2 444.15 122.83 13 -11 3 -16.25 65.54 -13 11 -3 43.07 41.16 13 -11 4 200.56 139.85 -13 11 -4 201.07 99.63 13 -11 5 660.19 369.56 -13 11 -5 966.40 202.22 13 -11 6 466.33 224.94 -13 11 -6 544.20 118.72 13 -11 7 79.68 61.40 -13 11 -7 49.71 63.17 13 -11 8 59.28 44.64 -13 11 -8 32.68 64.97 13 -11 9 490.03 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888.54 231.66 17 9 5 82.35 96.74 17 9 5 120.88 61.67 -17 -9 -5 209.40 151.60 17 9 6 18.81 42.28 17 9 6 -23.77 50.12 -17 -9 -6 79.23 63.51 17 9 7 790.19 118.18 17 9 7 440.94 131.75 -17 -9 -7 757.18 247.75 17 9 8 2099.45 294.40 17 9 8 1945.81 219.47 -17 -9 -8 2225.72 190.36 17 9 9 633.80 273.41 17 9 9 737.66 266.48 -17 -9 -9 1078.95 126.92 17 9 10 43.72 68.99 17 9 10 74.65 91.65 -17 -9 -10 177.97 145.34 17 9 11 1222.33 142.98 -17 -9 -11 1006.04 378.32 -17 -9 -11 1196.74 250.17 17 9 12 72.91 68.59 -17 -9 -12 -41.45 60.39 -17 -9 -12 65.98 63.00 17 10 4 407.45 133.90 17 10 4 289.83 90.99 -17 -10 -4 344.31 128.00 17 10 5 359.78 95.02 17 10 5 299.34 87.13 -17 -10 -5 261.89 161.41 17 10 6 38.28 66.10 17 10 6 52.13 33.33 -17 -10 -6 7.52 85.66 17 10 7 172.09 139.24 17 10 7 62.29 35.46 -17 -10 -7 214.60 118.94 17 10 8 81.62 44.83 17 10 8 84.72 83.66 -17 -10 -8 305.99 104.32 17 10 9 471.41 127.71 17 10 9 510.14 225.47 -17 -10 -9 533.24 136.21 17 10 10 743.02 190.53 17 10 10 429.10 137.76 -17 -10 -10 418.38 149.49 17 10 11 27.06 70.49 -17 -10 -11 102.82 74.79 -17 -10 -11 85.71 36.61 17 11 6 585.22 311.69 -17 -11 -6 885.87 245.23 17 11 7 528.24 320.60 17 11 7 909.57 221.33 -17 -11 -7 751.67 375.76 17 11 8 268.01 80.46 17 11 8 308.59 129.12 -17 -11 -8 115.51 85.81 17 11 9 427.66 173.06 17 11 9 95.17 71.70 -17 -11 -9 177.70 91.26 18 -2 7 174.46 97.50 -18 2 -7 182.83 102.63 18 -2 8 643.35 193.40 -18 2 -8 714.33 111.05 18 -2 9 418.10 122.10 -18 2 -9 207.33 96.07 18 -2 10 73.03 66.11 18 -2 10 33.33 49.96 -18 2 -10 60.82 66.08 18 -2 11 1075.71 127.87 18 -2 11 1093.78 300.77 -18 2 -11 849.94 385.41 18 -1 5 1625.52 267.77 -18 1 -5 1367.44 282.43 18 -1 6 1316.13 270.99 -18 1 -6 830.86 370.89 18 -1 7 234.42 183.86 18 -1 7 453.66 212.26 -18 1 -7 715.56 180.95 18 -1 8 540.30 160.59 18 -1 8 901.63 228.81 -18 1 -8 541.16 302.67 18 -1 9 23.38 46.72 18 -1 9 83.19 102.30 -18 1 -9 249.07 86.26 18 -1 10 80.95 57.38 18 -1 10 175.67 88.95 -18 1 -10 344.29 112.25 18 -1 11 246.85 114.57 18 -1 11 195.91 101.09 -18 1 -11 166.02 99.78 18 -1 12 160.86 76.64 18 -1 12 250.83 90.84 -18 1 -12 160.08 110.29 18 0 5 78.78 44.84 18 0 5 169.59 89.12 -18 0 -5 52.68 43.10 18 0 6 762.73 94.68 18 0 6 733.36 181.23 -18 0 -6 722.19 255.41 18 0 7 493.95 249.86 18 0 7 967.07 194.73 -18 0 -7 674.42 225.41 18 0 8 12.77 41.17 18 0 8 160.21 106.41 -18 0 -8 94.43 96.80 18 0 9 63.16 56.15 18 0 9 79.38 74.98 -18 0 -9 52.17 84.58 18 0 10 4.08 62.55 18 0 10 57.41 106.47 -18 0 -10 66.27 53.83 18 0 11 92.28 48.32 18 0 11 103.77 88.23 -18 0 -11 1.34 67.67 18 0 12 6.54 53.77 18 0 12 16.33 66.76 -18 0 -12 22.52 71.78 18 0 13 35.34 64.16 18 0 13 35.52 40.66 -18 0 -13 79.48 59.27 18 1 4 39.63 34.03 18 1 4 110.12 75.53 -18 -1 -4 44.18 64.18 18 1 5 1557.21 119.94 18 1 5 1472.87 341.54 -18 -1 -5 1607.87 344.89 18 1 6 2245.08 180.58 18 1 6 1832.39 395.44 -18 -1 -6 1808.23 236.05 18 1 7 229.68 140.08 18 1 7 330.72 142.18 -18 -1 -7 282.43 121.29 18 1 8 22.59 37.72 18 1 8 43.15 68.13 -18 -1 -8 21.17 59.27 18 1 9 166.24 145.08 18 1 9 328.73 125.45 -18 -1 -9 316.61 108.22 18 1 10 566.71 215.68 18 1 10 602.29 150.41 -18 -1 -10 739.38 180.84 18 1 11 22.29 60.61 18 1 11 53.12 63.07 -18 -1 -11 47.25 62.71 18 1 12 582.62 147.35 18 1 12 639.44 290.53 -18 -1 -12 643.84 131.89 18 1 13 2062.71 192.69 18 1 13 2386.50 159.48 -18 -1 -13 2438.71 225.09 18 2 4 78.83 54.04 18 2 4 54.13 46.02 -18 -2 -4 75.97 95.87 18 2 5 367.13 158.55 -18 -2 -5 341.99 141.73 18 2 6 14.21 54.35 18 2 6 89.20 109.05 -18 -2 -6 -72.65 72.71 18 2 7 415.68 159.99 18 2 7 682.57 269.81 -18 -2 -7 535.12 150.07 18 2 8 75.00 82.55 18 2 8 17.08 35.61 -18 -2 -8 148.93 101.48 18 2 9 436.03 203.88 18 2 9 478.51 188.78 -18 -2 -9 453.74 186.69 18 2 10 179.17 119.36 18 2 10 338.26 80.31 -18 -2 -10 185.82 62.98 18 2 11 88.11 74.44 18 2 11 142.59 130.91 -18 -2 -11 2.63 92.66 18 2 12 302.21 171.35 18 2 12 370.11 104.95 -18 -2 -12 227.19 138.00 18 2 13 38.47 56.05 18 2 13 80.27 68.53 -18 -2 -13 61.27 51.33 18 3 4 141.54 106.92 18 3 4 55.86 99.72 -18 -3 -4 134.32 70.81 18 3 5 63.44 56.37 18 3 5 68.39 50.28 -18 -3 -5 13.16 87.81 18 3 6 101.55 45.11 18 3 6 184.21 92.50 -18 -3 -6 157.71 89.34 18 3 7 380.09 250.95 18 3 7 546.02 155.92 -18 -3 -7 201.36 96.70 18 3 8 158.56 137.88 18 3 8 255.45 109.77 -18 -3 -8 377.07 187.53 18 3 9 66.74 74.40 18 3 9 23.85 66.22 -18 -3 -9 102.65 82.82 18 3 10 59.43 43.53 18 3 10 14.59 32.74 -18 -3 -10 114.27 63.34 18 3 11 103.76 72.63 18 3 11 187.30 62.74 -18 -3 -11 232.02 137.52 18 3 12 496.21 198.37 18 3 12 512.22 139.23 -18 -3 -12 329.37 158.93 18 3 13 3050.81 396.70 18 3 13 3682.85 195.36 -18 -3 -13 3662.91 217.47 18 4 4 288.22 128.50 18 4 4 396.54 142.79 -18 -4 -4 732.56 242.16 18 4 5 450.89 182.27 18 4 5 551.58 120.25 -18 -4 -5 231.66 140.90 18 4 6 -26.07 48.03 18 4 6 97.81 53.61 -18 -4 -6 16.11 85.74 18 4 7 1130.08 156.15 18 4 7 938.19 169.05 -18 -4 -7 1221.23 116.62 18 4 8 11.28 46.22 18 4 8 87.88 79.71 -18 -4 -8 198.46 124.53 18 4 9 101.96 77.80 18 4 9 33.93 58.01 -18 -4 -9 55.71 59.50 18 4 10 -6.10 92.00 18 4 10 117.02 47.46 -18 -4 -10 347.14 94.35 18 4 11 42.94 27.17 18 4 11 48.46 77.78 -18 -4 -11 130.82 84.14 18 4 12 60.51 61.93 18 4 12 129.70 80.96 -18 -4 -12 -2.05 48.73 18 4 13 33.80 66.38 -18 -4 -13 53.99 85.80 -18 -4 -13 184.52 108.66 18 5 4 140.31 100.17 18 5 4 105.88 78.57 -18 -5 -4 32.02 59.39 18 5 5 48.29 93.62 18 5 5 44.22 50.71 -18 -5 -5 6.14 49.81 18 5 6 394.53 196.90 18 5 6 464.96 158.88 -18 -5 -6 521.27 162.66 18 5 7 62.90 74.38 18 5 7 78.71 77.89 -18 -5 -7 92.97 74.99 18 5 8 1837.78 179.22 18 5 8 2190.87 268.26 -18 -5 -8 2220.28 205.14 18 5 9 1768.97 177.61 18 5 9 1546.83 185.74 -18 -5 -9 1292.66 543.05 18 5 10 130.09 79.78 18 5 10 66.73 37.63 -18 -5 -10 98.19 66.84 18 5 11 504.21 133.01 -18 -5 -11 512.96 193.62 18 5 12 746.75 262.71 18 5 12 690.66 307.29 -18 -5 -12 1188.96 274.29 18 5 13 571.15 368.84 -18 -5 -13 811.77 166.32 -18 -5 -13 833.50 290.58 18 6 4 135.10 130.45 -18 -6 -4 329.66 157.60 18 6 5 1462.40 159.96 18 6 5 1110.73 298.71 -18 -6 -5 1483.03 258.42 18 6 6 255.99 119.96 18 6 6 300.97 72.14 -18 -6 -6 236.07 147.85 18 6 7 2127.98 179.89 18 6 7 1569.35 657.68 -18 -6 -7 1284.55 294.63 18 6 8 3324.84 249.34 18 6 8 2859.70 412.29 -18 -6 -8 2774.44 481.80 18 6 9 137.13 87.12 18 6 9 216.51 155.85 -18 -6 -9 48.29 54.03 18 6 10 1119.28 460.33 18 6 10 1195.23 160.43 -18 -6 -10 765.73 275.20 18 6 11 55.22 69.83 18 6 11 62.84 41.73 -18 -6 -11 23.52 69.68 18 6 12 735.14 361.81 18 6 12 783.42 259.99 -18 -6 -12 963.29 360.55 18 7 5 113.64 91.71 18 7 5 107.54 60.97 -18 -7 -5 69.06 49.41 18 7 6 279.57 156.73 18 7 6 215.98 113.78 -18 -7 -6 338.22 144.11 18 7 7 102.16 52.37 18 7 7 61.69 57.39 -18 -7 -7 11.87 71.35 18 7 8 666.46 188.41 18 7 8 903.75 194.16 -18 -7 -8 856.94 130.59 18 7 9 3666.90 202.25 18 7 9 3655.41 205.15 -18 -7 -9 3745.85 410.64 18 7 10 408.42 174.10 -18 -7 -10 416.68 167.29 18 7 11 697.85 345.39 18 7 11 778.47 283.59 -18 -7 -11 926.49 178.97 18 7 12 2101.96 475.48 -18 -7 -12 2320.55 240.83 18 8 6 52.11 49.27 18 8 6 17.81 45.93 -18 -8 -6 27.44 83.90 18 8 7 228.87 133.28 18 8 7 325.75 63.33 18 8 8 1418.24 128.59 18 8 8 1162.97 287.87 -18 -8 -8 1045.74 418.21 18 8 9 183.35 207.13 18 8 9 552.33 146.14 -18 -8 -9 441.72 132.97 18 8 10 326.81 127.66 18 8 10 216.44 111.13 -18 -8 -10 425.55 166.11 ; _shelx_hkl_checksum 73163 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z 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 0.38085(2) 0.88810(2) 0.27741(2) 0.02438(8) Uani 1 1 d . . . . . Pd2 Pd 0.23736(2) 0.75487(2) 0.56677(2) 0.02358(7) Uani 1 1 d . . . . . Pd3 Pd 0.15184(2) 0.68954(2) 0.32153(2) 0.02375(8) Uani 1 1 d . . . . . Pd4 Pd 0.24908(2) 0.78344(2) 0.39219(2) 0.02220(7) Uani 1 1 d . . . . . Si1 Si 0.34369(8) 0.86013(7) 0.43732(7) 0.0224(2) Uani 1 1 d . . . . . Si2 Si 0.14246(8) 0.69797(7) 0.49529(7) 0.0245(2) Uani 1 1 d . . . . . Si3 Si 0.26036(8) 0.79491(7) 0.24397(7) 0.0265(2) Uani 1 1 d . . . . . N1 N 0.6012(2) 0.9271(2) 0.1542(2) 0.0293(7) Uani 1 1 d . . . . . N2 N 0.5021(3) 1.0479(2) 0.2301(2) 0.0291(7) Uani 1 1 d . . . . . N3 N 0.2763(3) 0.6487(2) 0.7205(2) 0.0290(7) Uani 1 1 d . . . . . N4 N 0.1412(3) 0.7496(2) 0.7870(2) 0.0305(7) Uani 1 1 d . . . . . N5 N 0.0057(2) 0.6498(2) 0.2350(2) 0.0285(7) Uani 1 1 d . . . . . N6 N 0.1373(3) 0.5456(2) 0.1919(2) 0.0283(7) Uani 1 1 d . . . . . C1 C 0.5009(3) 0.9609(3) 0.2157(3) 0.0264(8) Uani 1 1 d . . . . . C2 C 0.6646(3) 0.9931(3) 0.1304(3) 0.0355(10) Uani 1 1 d . . . . . C3 C 0.6024(3) 1.0683(3) 0.1785(3) 0.0355(10) Uani 1 1 d . . . . . C4 C 0.6279(3) 0.8357(3) 0.1139(3) 0.0344(9) Uani 1 1 d . . . . . H4 H 0.5658 0.8071 0.1521 0.041 Uiso 1 1 calc R U . . . C5 C 0.7190(4) 0.7818(3) 0.1253(4) 0.0517(13) Uani 1 1 d . . . . . H5A H 0.7018 0.7804 0.1932 0.062 Uiso 1 1 calc R U . . . H5B H 0.7815 0.8091 0.0921 0.062 Uiso 1 1 calc R U . . . H5C H 0.7323 0.7214 0.0978 0.062 Uiso 1 1 calc R U . . . C6 C 0.6421(4) 0.8312(3) 0.0117(3) 0.0451(11) Uani 1 1 d . . . . . H6A H 0.5836 0.8694 0.0079 0.054 Uiso 1 1 calc R U . . . H6B H 0.6444 0.7702 -0.0081 0.054 Uiso 1 1 calc R U . . . H6C H 0.7074 0.8513 -0.0305 0.054 Uiso 1 1 calc R U . . . C7 C 0.4041(3) 1.1082(3) 0.2866(3) 0.0363(10) Uani 1 1 d . . . . . H7 H 0.3501 1.0701 0.3201 0.044 Uiso 1 1 calc R U . . . C8 C 0.4072(4) 1.1650(3) 0.3637(3) 0.0500(12) Uani 1 1 d . . . . . H8A H 0.4615 1.2018 0.3344 0.060 Uiso 1 1 calc R U . . . H8B H 0.4227 1.1269 0.4078 0.060 Uiso 1 1 calc R U . . . H8C H 0.3395 1.2029 0.3988 0.060 Uiso 1 1 calc R U . . . C9 C 0.3689(4) 1.1623(3) 0.2215(4) 0.0521(13) Uani 1 1 d . . . . . H9A H 0.3588 1.1225 0.1788 0.063 Uiso 1 1 calc R U . . . H9B H 0.4222 1.1977 0.1835 0.063 Uiso 1 1 calc R U . . . H9C H 0.3031 1.2016 0.2601 0.063 Uiso 1 1 calc R U . . . C10 C 0.7794(3) 0.9764(3) 0.0673(3) 0.0497(12) Uani 1 1 d . . . . . H10A H 0.8162 0.9900 0.1037 0.060 Uiso 1 1 calc R U . . . H10B H 0.7957 1.0140 0.0133 0.060 Uiso 1 1 calc R U . . . H10C H 0.8016 0.9141 0.0434 0.060 Uiso 1 1 calc R U . . . C11 C 0.6323(4) 1.1566(3) 0.1805(3) 0.0511(13) Uani 1 1 d . . . . . H11A H 0.6633 1.1763 0.1155 0.061 Uiso 1 1 calc R U . . . H11B H 0.6832 1.1525 0.2063 0.061 Uiso 1 1 calc R U . . . H11C H 0.5703 1.1991 0.2209 0.061 Uiso 1 1 calc R U . . . C12 C 0.2153(3) 0.7153(2) 0.7004(2) 0.0258(8) Uani 1 1 d . . . . . C13 C 0.2392(3) 0.6451(3) 0.8196(3) 0.0346(10) Uani 1 1 d . . . . . C14 C 0.1543(4) 0.7067(3) 0.8606(3) 0.0382(10) Uani 1 1 d . . . . . C15 C 0.3707(3) 0.5984(3) 0.6424(3) 0.0329(9) Uani 1 1 d . . . . . H15 H 0.3681 0.6155 0.5817 0.039 Uiso 1 1 calc R U . . . C16 C 0.3734(4) 0.4996(3) 0.6445(4) 0.0544(14) Uani 1 1 d . . . . . H16A H 0.3126 0.4849 0.6391 0.065 Uiso 1 1 calc R U . . . H16B H 0.3719 0.4800 0.7047 0.065 Uiso 1 1 calc R U . . . H16C H 0.4373 0.4698 0.5909 0.065 Uiso 1 1 calc R U . . . C17 C 0.4680(4) 0.6268(4) 0.6387(4) 0.0547(13) Uani 1 1 d . . . . . H17A H 0.4713 0.6155 0.6990 0.066 Uiso 1 1 calc R U . . . H17B H 0.4659 0.6900 0.6286 0.066 Uiso 1 1 calc R U . . . H17C H 0.5297 0.5932 0.5860 0.066 Uiso 1 1 calc R U . . . C18 C 0.0591(3) 0.8227(3) 0.7944(3) 0.0344(9) Uani 1 1 d . . . . . H18 H 0.0771 0.8392 0.7276 0.041 Uiso 1 1 calc R U . . . C19 C -0.0468(3) 0.7946(3) 0.8319(3) 0.0465(12) Uani 1 1 d . . . . . H19A H -0.0662 0.7735 0.8959 0.056 Uiso 1 1 calc R U . . . H19B H -0.0442 0.7470 0.7891 0.056 Uiso 1 1 calc R U . . . H19C H -0.0987 0.8452 0.8351 0.056 Uiso 1 1 calc R U . . . C20 C 0.0590(4) 0.9050(3) 0.8482(3) 0.0450(11) Uani 1 1 d . . . . . H20A H 0.1267 0.9246 0.8154 0.054 Uiso 1 1 calc R U . . . H20B H 0.0462 0.8912 0.9134 0.054 Uiso 1 1 calc R U . . . H20C H 0.0039 0.9520 0.8506 0.054 Uiso 1 1 calc R U . . . C21 C 0.2887(4) 0.5801(3) 0.8656(4) 0.0548(14) Uani 1 1 d . . . . . H21A H 0.2390 0.5419 0.9036 0.066 Uiso 1 1 calc R U . . . H21B H 0.3084 0.6122 0.9072 0.066 Uiso 1 1 calc R U . . . H21C H 0.3510 0.5439 0.8161 0.066 Uiso 1 1 calc R U . . . C22 C 0.0864(4) 0.7298(4) 0.9654(3) 0.0607(15) Uani 1 1 d . . . . . H22A H 0.1280 0.7494 0.9944 0.073 Uiso 1 1 calc R U . . . H22B H 0.0579 0.6776 0.9961 0.073 Uiso 1 1 calc R U . . . H22C H 0.0291 0.7773 0.9740 0.073 Uiso 1 1 calc R U . . . C23 C 0.0960(3) 0.6253(2) 0.2426(3) 0.0250(8) Uani 1 1 d . . . . . C24 C -0.0090(3) 0.5859(3) 0.1812(3) 0.0345(10) Uani 1 1 d . . . . . C25 C 0.0734(4) 0.5212(3) 0.1541(3) 0.0347(10) Uani 1 1 d . . . . . C26 C -0.0615(3) 0.7356(3) 0.2809(3) 0.0314(9) Uani 1 1 d . . . . . H26 H -0.0293 0.7609 0.3178 0.038 Uiso 1 1 calc R U . . . C27 C -0.1707(3) 0.7254(3) 0.3530(3) 0.0480(12) Uani 1 1 d . . . . . H27A H -0.1670 0.6885 0.4031 0.058 Uiso 1 1 calc R U . . . H27B H -0.2044 0.6973 0.3209 0.058 Uiso 1 1 calc R U . . . H27C H -0.2113 0.7837 0.3815 0.058 Uiso 1 1 calc R U . . . C28 C -0.0607(4) 0.8012(3) 0.2081(3) 0.0422(11) Uani 1 1 d . . . . . H28A H -0.0871 0.7774 0.1669 0.051 Uiso 1 1 calc R U . . . H28B H 0.0107 0.8117 0.1692 0.051 Uiso 1 1 calc R U . . . H28C H -0.1053 0.8570 0.2411 0.051 Uiso 1 1 calc R U . . . C29 C 0.2338(3) 0.4947(3) 0.1885(3) 0.0349(9) Uani 1 1 d . . . . . H29 H 0.2632 0.5357 0.2154 0.042 Uiso 1 1 calc R U . . . C30 C 0.2105(4) 0.4185(3) 0.2535(4) 0.0527(13) Uani 1 1 d . . . . . H30A H 0.1769 0.3783 0.2326 0.063 Uiso 1 1 calc R U . . . H30B H 0.1639 0.4417 0.3193 0.063 Uiso 1 1 calc R U . . . H30C H 0.2758 0.3864 0.2505 0.063 Uiso 1 1 calc R U . . . C31 C 0.3174(4) 0.4649(3) 0.0878(3) 0.0545(13) Uani 1 1 d . . . . . H31A H 0.3355 0.5167 0.0507 0.065 Uiso 1 1 calc R U . . . H31B H 0.2912 0.4262 0.0573 0.065 Uiso 1 1 calc R U . . . H31C H 0.3796 0.4326 0.0907 0.065 Uiso 1 1 calc R U . . . C32 C -0.1015(4) 0.5925(3) 0.1612(4) 0.0504(12) Uani 1 1 d . . . . . H32A H -0.1381 0.5426 0.1873 0.061 Uiso 1 1 calc R U . . . H32B H -0.0782 0.5911 0.0921 0.061 Uiso 1 1 calc R U . . . H32C H -0.1487 0.6480 0.1913 0.061 Uiso 1 1 calc R U . . . C33 C 0.0947(5) 0.4359(3) 0.0962(4) 0.0608(15) Uani 1 1 d . . . . . H33A H 0.0973 0.4490 0.0339 0.073 Uiso 1 1 calc R U . . . H33B H 0.0390 0.4013 0.1301 0.073 Uiso 1 1 calc R U . . . H33C H 0.1617 0.4018 0.0870 0.073 Uiso 1 1 calc R U . . . C34 C 0.4703(3) 0.8126(2) 0.4435(3) 0.0275(8) Uani 1 1 d . . . . . H34 H 0.4514 0.8012 0.5118 0.033 Uiso 1 1 calc R U . . . C35 C 0.5196(3) 0.7243(3) 0.3859(3) 0.0419(11) Uani 1 1 d . . . . . H35A H 0.5800 0.6987 0.3958 0.050 Uiso 1 1 calc R U . . . H35B H 0.5422 0.7332 0.3180 0.050 Uiso 1 1 calc R U . . . H35C H 0.4685 0.6840 0.4069 0.050 Uiso 1 1 calc R U . . . C36 C 0.5498(3) 0.8762(3) 0.4137(3) 0.0344(9) Uani 1 1 d . . . . . H36A H 0.5687 0.8905 0.3475 0.041 Uiso 1 1 calc R U . . . H36B H 0.6122 0.8482 0.4189 0.041 Uiso 1 1 calc R U . . . H36C H 0.5190 0.9306 0.4555 0.041 Uiso 1 1 calc R U . . . C37 C 0.2948(3) 0.9705(2) 0.5120(3) 0.0277(8) Uani 1 1 d . . . . . H37 H 0.3476 1.0099 0.4799 0.033 Uiso 1 1 calc R U . . . C38 C 0.2839(4) 0.9609(3) 0.6133(3) 0.0445(11) Uani 1 1 d . . . . . H38A H 0.3501 0.9310 0.6102 0.053 Uiso 1 1 calc R U . . . H38B H 0.2290 0.9259 0.6482 0.053 Uiso 1 1 calc R U . . . H38C H 0.2655 1.0195 0.6463 0.053 Uiso 1 1 calc R U . . . C39 C 0.1915(3) 1.0156(3) 0.5149(4) 0.0470(12) Uani 1 1 d . . . . . H39A H 0.1712 1.0742 0.5486 0.056 Uiso 1 1 calc R U . . . H39B H 0.1373 0.9796 0.5485 0.056 Uiso 1 1 calc R U . . . H39C H 0.2001 1.0219 0.4496 0.056 Uiso 1 1 calc R U . . . C40 C 0.1606(3) 0.5722(3) 0.4953(3) 0.0364(10) Uani 1 1 d . . . . . H40 H 0.1222 0.5518 0.4617 0.044 Uiso 1 1 calc R U . . . C41 C 0.2744(4) 0.5299(3) 0.4389(4) 0.0482(12) Uani 1 1 d . . . . . H41A H 0.2796 0.4655 0.4343 0.058 Uiso 1 1 calc R U . . . H41B H 0.3145 0.5456 0.4714 0.058 Uiso 1 1 calc R U . . . H41C H 0.3025 0.5515 0.3746 0.058 Uiso 1 1 calc R U . . . C42 C 0.1134(4) 0.5384(3) 0.5962(4) 0.0542(13) Uani 1 1 d . . . . . H42A H 0.1516 0.5541 0.6306 0.065 Uiso 1 1 calc R U . . . H42B H 0.1188 0.4740 0.5914 0.065 Uiso 1 1 calc R U . . . H42C H 0.0400 0.5655 0.6308 0.065 Uiso 1 1 calc R U . . . C43 C -0.0042(3) 0.7366(3) 0.5735(3) 0.0305(9) Uani 1 1 d . . . . . H43 H -0.0221 0.7141 0.6382 0.037 Uiso 1 1 calc R U . . . C44 C -0.0698(3) 0.6982(4) 0.5339(3) 0.0480(12) Uani 1 1 d . . . . . H44A H -0.0559 0.7210 0.4714 0.058 Uiso 1 1 calc R U . . . H44B H -0.1439 0.7154 0.5778 0.058 Uiso 1 1 calc R U . . . H44C H -0.0518 0.6336 0.5269 0.058 Uiso 1 1 calc R U . . . C45 C -0.0313(4) 0.8375(3) 0.5860(4) 0.0516(13) Uani 1 1 d . . . . . H45A H -0.1040 0.8549 0.6335 0.062 Uiso 1 1 calc R U . . . H45B H -0.0218 0.8611 0.5248 0.062 Uiso 1 1 calc R U . . . H45C H 0.0145 0.8610 0.6076 0.062 Uiso 1 1 calc R U . . . C46 C 0.3752(4) 0.7422(3) 0.1273(3) 0.0428(11) Uani 1 1 d . . . . . C47 C 0.3435(5) 0.7161(4) 0.0518(3) 0.0646(16) Uani 1 1 d . . . . . H47A H 0.3019 0.6685 0.0739 0.078 Uiso 1 1 calc R U . . . H47B H 0.4061 0.6955 -0.0077 0.078 Uiso 1 1 calc R U . . . H47C H 0.3021 0.7673 0.0404 0.078 Uiso 1 1 calc R U . . . C48 C 0.4411(4) 0.6636(3) 0.1470(3) 0.0545(14) Uani 1 1 d . . . . . H48A H 0.5044 0.6431 0.0881 0.065 Uiso 1 1 calc R U . . . H48B H 0.4005 0.6154 0.1695 0.065 Uiso 1 1 calc R U . . . H48C H 0.4601 0.6822 0.1960 0.065 Uiso 1 1 calc R U . . . C49 C 0.1833(4) 0.8874(3) 0.2065(3) 0.0387(10) Uani 1 1 d . . . . . C50 C 0.2527(5) 0.9541(4) 0.1500(4) 0.0643(16) Uani 1 1 d . . . . . H50A H 0.2776 0.9817 0.1904 0.077 Uiso 1 1 calc R U . . . H50B H 0.2124 0.9997 0.1303 0.077 Uiso 1 1 calc R U . . . H50C H 0.3125 0.9235 0.0934 0.077 Uiso 1 1 calc R U . . . C51 C 0.0896(4) 0.9335(3) 0.2941(4) 0.0529(13) Uani 1 1 d . . . . . H51A H 0.0491 0.9789 0.2743 0.064 Uiso 1 1 calc R U . . . H51B H 0.1134 0.9613 0.3353 0.064 Uiso 1 1 calc R U . . . H51C H 0.0459 0.8902 0.3293 0.064 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02255(15) 0.02815(16) 0.02228(15) 0.00373(11) -0.00871(12) -0.00810(12) Pd2 0.02381(15) 0.02657(16) 0.02012(15) 0.00252(11) -0.00955(12) -0.00437(12) Pd3 0.02231(15) 0.02508(16) 0.02494(15) -0.00119(11) -0.01116(12) -0.00496(12) Pd4 0.02209(14) 0.02603(15) 0.01997(14) 0.00278(11) -0.00957(11) -0.00775(12) Si1 0.0200(5) 0.0220(5) 0.0248(5) -0.0017(4) -0.0100(4) -0.0023(4) Si2 0.0199(5) 0.0260(5) 0.0268(5) 0.0050(4) -0.0096(4) -0.0046(4) Si3 0.0290(6) 0.0292(6) 0.0228(5) 0.0024(4) -0.0122(4) -0.0068(5) N1 0.0245(17) 0.0384(19) 0.0241(17) 0.0059(14) -0.0085(14) -0.0104(15) N2 0.0294(18) 0.0328(18) 0.0262(17) 0.0082(14) -0.0114(14) -0.0119(15) N3 0.0326(18) 0.0272(17) 0.0272(17) 0.0021(13) -0.0147(15) -0.0010(14) N4 0.0347(19) 0.0300(18) 0.0235(17) 0.0051(14) -0.0102(15) -0.0052(15) N5 0.0285(17) 0.0344(19) 0.0251(17) 0.0001(14) -0.0130(14) -0.0091(15) N6 0.0323(18) 0.0222(16) 0.0295(18) -0.0023(13) -0.0131(15) -0.0042(14) C1 0.0263(19) 0.032(2) 0.0213(19) 0.0047(15) -0.0099(16) -0.0072(16) C2 0.033(2) 0.056(3) 0.023(2) 0.0093(19) -0.0116(17) -0.025(2) C3 0.035(2) 0.046(3) 0.027(2) 0.0070(19) -0.0111(18) -0.019(2) C4 0.028(2) 0.036(2) 0.037(2) -0.0008(18) -0.0121(18) -0.0046(18) C5 0.037(3) 0.053(3) 0.054(3) 0.002(2) -0.014(2) 0.002(2) C6 0.044(3) 0.058(3) 0.032(2) -0.004(2) -0.013(2) -0.017(2) C7 0.039(2) 0.035(2) 0.034(2) 0.0047(18) -0.0139(19) -0.0129(19) C8 0.058(3) 0.048(3) 0.040(3) -0.002(2) -0.015(2) -0.018(2) C9 0.055(3) 0.048(3) 0.054(3) 0.009(2) -0.026(3) -0.002(2) C10 0.038(3) 0.068(3) 0.042(3) 0.003(2) -0.012(2) -0.024(2) C11 0.053(3) 0.054(3) 0.046(3) 0.006(2) -0.016(2) -0.027(3) C12 0.029(2) 0.030(2) 0.0150(17) 0.0029(15) -0.0057(15) -0.0068(16) C13 0.045(3) 0.039(2) 0.025(2) 0.0122(18) -0.0198(19) -0.011(2) C14 0.047(3) 0.045(3) 0.021(2) 0.0082(18) -0.0131(19) -0.010(2) C15 0.038(2) 0.028(2) 0.034(2) -0.0027(17) -0.0193(19) 0.0026(18) C16 0.078(4) 0.029(2) 0.056(3) 0.000(2) -0.033(3) 0.003(2) C17 0.038(3) 0.065(3) 0.059(3) -0.007(3) -0.020(2) -0.004(2) C18 0.032(2) 0.035(2) 0.028(2) -0.0016(17) -0.0079(18) -0.0020(18) C19 0.034(2) 0.058(3) 0.039(3) 0.002(2) -0.009(2) -0.008(2) C20 0.047(3) 0.036(3) 0.041(3) -0.003(2) -0.013(2) -0.002(2) C21 0.074(4) 0.055(3) 0.046(3) 0.014(2) -0.038(3) -0.003(3) C22 0.071(4) 0.082(4) 0.022(2) 0.009(2) -0.017(2) -0.005(3) C23 0.0235(18) 0.028(2) 0.0229(19) -0.0022(15) -0.0087(15) -0.0059(16) C24 0.040(2) 0.041(2) 0.032(2) 0.0042(18) -0.0203(19) -0.021(2) C25 0.047(3) 0.031(2) 0.033(2) -0.0030(18) -0.022(2) -0.015(2) C26 0.028(2) 0.037(2) 0.028(2) -0.0001(17) -0.0133(17) -0.0031(18) C27 0.029(2) 0.066(3) 0.043(3) 0.004(2) -0.014(2) -0.002(2) C28 0.045(3) 0.045(3) 0.042(3) 0.001(2) -0.026(2) -0.004(2) C29 0.034(2) 0.028(2) 0.037(2) -0.0046(18) -0.0122(19) -0.0020(18) C30 0.055(3) 0.044(3) 0.062(3) 0.010(2) -0.030(3) -0.004(2) C31 0.047(3) 0.049(3) 0.051(3) -0.014(2) -0.009(2) 0.002(2) C32 0.047(3) 0.063(3) 0.057(3) 0.003(3) -0.034(3) -0.021(2) C33 0.095(5) 0.036(3) 0.067(4) -0.006(2) -0.049(3) -0.012(3) C34 0.0247(19) 0.029(2) 0.030(2) 0.0058(16) -0.0126(16) -0.0051(16) C35 0.028(2) 0.029(2) 0.065(3) 0.000(2) -0.019(2) 0.0032(18) C36 0.0199(19) 0.041(2) 0.044(2) -0.0014(19) -0.0157(18) -0.0045(17) C37 0.027(2) 0.025(2) 0.028(2) -0.0021(16) -0.0094(16) -0.0061(16) C38 0.058(3) 0.039(3) 0.030(2) -0.0060(19) -0.013(2) -0.013(2) C39 0.035(2) 0.037(3) 0.060(3) -0.018(2) -0.018(2) 0.009(2) C40 0.042(2) 0.025(2) 0.053(3) 0.0039(19) -0.030(2) -0.0080(19) C41 0.051(3) 0.029(2) 0.065(3) -0.005(2) -0.032(3) 0.010(2) C42 0.063(3) 0.037(3) 0.063(3) 0.023(2) -0.027(3) -0.016(2) C43 0.0233(19) 0.039(2) 0.026(2) 0.0064(17) -0.0085(16) -0.0040(17) C44 0.026(2) 0.083(4) 0.037(3) 0.012(2) -0.0135(19) -0.019(2) C45 0.033(2) 0.052(3) 0.056(3) 0.005(2) -0.011(2) 0.007(2) C46 0.042(3) 0.055(3) 0.025(2) -0.004(2) -0.0082(19) -0.012(2) C47 0.075(4) 0.092(4) 0.028(3) -0.010(3) -0.018(3) -0.033(3) C48 0.031(2) 0.063(3) 0.048(3) -0.023(2) 0.001(2) -0.007(2) C49 0.046(3) 0.040(2) 0.042(3) 0.018(2) -0.028(2) -0.016(2) C50 0.082(4) 0.060(3) 0.081(4) 0.041(3) -0.058(4) -0.034(3) C51 0.061(3) 0.037(3) 0.071(4) 0.002(2) -0.043(3) 0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.9988 1.0072 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Si Si 0.0817 0.0704 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 Pd1 Si1 112.24(10) . . C1 Pd1 Si3 144.65(11) . . Si1 Pd1 Si3 102.60(4) . . C1 Pd1 Pd4 163.61(10) . . Si1 Pd1 Pd4 52.53(3) . . Si3 Pd1 Pd4 50.08(3) . . C12 Pd2 Si2 118.18(11) . . C12 Pd2 Si1 139.59(11) . . Si2 Pd2 Si1 102.21(4) . . C12 Pd2 Pd4 170.18(10) . . Si2 Pd2 Pd4 52.31(3) . . Si1 Pd2 Pd4 50.05(2) . . C23 Pd3 Si3 117.02(10) . . C23 Pd3 Si2 140.99(10) . . Si3 Pd3 Si2 101.99(4) . . C23 Pd3 Pd4 169.15(10) . . Si3 Pd3 Pd4 52.42(3) . . Si2 Pd3 Pd4 49.69(2) . . Si2 Pd4 Si3 120.31(4) . . Si2 Pd4 Si1 120.18(4) . . Si3 Pd4 Si1 119.50(4) . . Si2 Pd4 Pd2 56.48(3) . . Si3 Pd4 Pd2 175.17(3) . . Si1 Pd4 Pd2 63.89(3) . . Si2 Pd4 Pd1 176.26(3) . . Si3 Pd4 Pd1 63.42(3) . . Si1 Pd4 Pd1 56.09(3) . . Pd2 Pd4 Pd1 119.783(17) . . Si2 Pd4 Pd3 64.30(3) . . Si3 Pd4 Pd3 56.18(3) . . Si1 Pd4 Pd3 174.52(3) . . Pd2 Pd4 Pd3 120.196(18) . . Pd1 Pd4 Pd3 119.41(2) . . C34 Si1 C37 105.15(17) . . C34 Si1 Pd4 125.85(12) . . C37 Si1 Pd4 126.47(13) . . C34 Si1 Pd1 109.39(13) . . C37 Si1 Pd1 108.69(13) . . Pd4 Si1 Pd1 71.38(3) . . C34 Si1 Pd2 91.91(12) . . C37 Si1 Pd2 100.39(12) . . Pd4 Si1 Pd2 66.06(3) . . Pd1 Si1 Pd2 137.15(4) . . C40 Si2 C43 104.75(19) . . C40 Si2 Pd4 128.66(15) . . C43 Si2 Pd4 123.74(13) . . C40 Si2 Pd2 110.28(13) . . C43 Si2 Pd2 109.06(13) . . Pd4 Si2 Pd2 71.21(4) . . C40 Si2 Pd3 90.46(14) . . C43 Si2 Pd3 101.49(13) . . Pd4 Si2 Pd3 66.01(3) . . Pd2 Si2 Pd3 136.37(4) . . C46 Si3 C49 105.5(2) . . C46 Si3 Pd4 126.16(16) . . C49 Si3 Pd4 125.36(15) . . C46 Si3 Pd3 110.14(15) . . C49 Si3 Pd3 109.01(14) . . Pd4 Si3 Pd3 71.40(3) . . C46 Si3 Pd1 91.16(14) . . C49 Si3 Pd1 99.23(14) . . Pd4 Si3 Pd1 66.50(3) . . Pd3 Si3 Pd1 137.60(5) . . C1 N1 C2 110.9(3) . . C1 N1 C4 120.2(3) . . C2 N1 C4 128.5(3) . . C1 N2 C3 111.2(3) . . C1 N2 C7 120.1(3) . . C3 N2 C7 128.5(3) . . C12 N3 C13 110.2(3) . . C12 N3 C15 120.1(3) . . C13 N3 C15 129.5(3) . . C12 N4 C14 111.7(3) . . C12 N4 C18 120.0(3) . . C14 N4 C18 128.2(3) . . C23 N5 C24 111.3(3) . . C23 N5 C26 119.7(3) . . C24 N5 C26 129.0(3) . . C23 N6 C25 111.1(3) . . C23 N6 C29 120.0(3) . . C25 N6 C29 128.7(3) . . N2 C1 N1 104.6(3) . . N2 C1 Pd1 130.2(3) . . N1 C1 Pd1 125.1(3) . . C3 C2 N1 106.5(4) . . C3 C2 C10 129.5(4) . . N1 C2 C10 124.0(4) . . C2 C3 N2 106.8(4) . . C2 C3 C11 127.7(4) . . N2 C3 C11 125.4(4) . . N1 C4 C6 111.7(3) . . N1 C4 C5 113.5(4) . . C6 C4 C5 112.9(4) . . N1 C4 H4 106.0 . . C6 C4 H4 106.0 . . C5 C4 H4 106.0 . . C4 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . H5A C5 H5B 109.5 . . C4 C5 H5C 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . C4 C6 H6A 109.5 . . C4 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C4 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . N2 C7 C8 113.9(4) . . N2 C7 C9 110.4(4) . . C8 C7 C9 112.6(4) . . N2 C7 H7 106.4 . . C8 C7 H7 106.4 . . C9 C7 H7 106.4 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C7 C9 H9A 109.5 . . C7 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C7 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C2 C10 H10A 109.5 . . C2 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C2 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C3 C11 H11A 109.5 . . C3 C11 H11B 109.5 . . H11A C11 H11B 109.5 . . C3 C11 H11C 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . N4 C12 N3 104.2(3) . . N4 C12 Pd2 128.7(3) . . N3 C12 Pd2 127.2(3) . . C14 C13 N3 107.1(3) . . C14 C13 C21 129.1(4) . . N3 C13 C21 123.8(4) . . C13 C14 N4 106.8(4) . . C13 C14 C22 127.9(4) . . N4 C14 C22 125.3(4) . . N3 C15 C16 113.1(4) . . N3 C15 C17 110.8(3) . . C16 C15 C17 113.4(4) . . N3 C15 H15 106.3 . . C16 C15 H15 106.3 . . C17 C15 H15 106.3 . . C15 C16 H16A 109.5 . . C15 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . C15 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C15 C17 H17A 109.5 . . C15 C17 H17B 109.5 . . H17A C17 H17B 109.5 . . C15 C17 H17C 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . N4 C18 C19 112.4(4) . . N4 C18 C20 112.3(4) . . C19 C18 C20 113.3(4) . . N4 C18 H18 106.0 . . C19 C18 H18 106.0 . . C20 C18 H18 106.0 . . C18 C19 H19A 109.5 . . C18 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C18 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C18 C20 H20A 109.5 . . C18 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . C18 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . C13 C21 H21A 109.5 . . C13 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C13 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C14 C22 H22A 109.5 . . C14 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C14 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . N5 C23 N6 103.9(3) . . N5 C23 Pd3 128.1(3) . . N6 C23 Pd3 127.9(3) . . C25 C24 N5 106.6(3) . . C25 C24 C32 129.1(4) . . N5 C24 C32 124.3(4) . . C24 C25 N6 107.1(3) . . C24 C25 C33 128.0(4) . . N6 C25 C33 124.9(4) . . N5 C26 C28 111.9(3) . . N5 C26 C27 112.9(4) . . C28 C26 C27 112.8(4) . . N5 C26 H26 106.2 . . C28 C26 H26 106.2 . . C27 C26 H26 106.2 . . C26 C27 H27A 109.5 . . C26 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . C26 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C26 C28 H28A 109.5 . . C26 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C26 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . N6 C29 C30 111.2(4) . . N6 C29 C31 113.7(4) . . C30 C29 C31 112.3(4) . . N6 C29 H29 106.3 . . C30 C29 H29 106.3 . . C31 C29 H29 106.3 . . C29 C30 H30A 109.5 . . C29 C30 H30B 109.5 . . H30A C30 H30B 109.5 . . C29 C30 H30C 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C29 C31 H31A 109.5 . . C29 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C29 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C24 C32 H32A 109.5 . . C24 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C24 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C25 C33 H33A 109.5 . . C25 C33 H33B 109.5 . . H33A C33 H33B 109.5 . . C25 C33 H33C 109.5 . . H33A C33 H33C 109.5 . . H33B C33 H33C 109.5 . . C35 C34 C36 110.5(3) . . C35 C34 Si1 111.3(3) . . C36 C34 Si1 113.6(3) . . C35 C34 H34 107.0 . . C36 C34 H34 107.0 . . Si1 C34 H34 107.0 . . C34 C35 H35A 109.5 . . C34 C35 H35B 109.5 . . H35A C35 H35B 109.5 . . C34 C35 H35C 109.5 . . H35A C35 H35C 109.5 . . H35B C35 H35C 109.5 . . C34 C36 H36A 109.5 . . C34 C36 H36B 109.5 . . H36A C36 H36B 109.5 . . C34 C36 H36C 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . C38 C37 C39 110.5(4) . . C38 C37 Si1 112.7(3) . . C39 C37 Si1 110.9(3) . . C38 C37 H37 107.5 . . C39 C37 H37 107.5 . . Si1 C37 H37 107.5 . . C37 C38 H38A 109.5 . . C37 C38 H38B 109.5 . . H38A C38 H38B 109.5 . . C37 C38 H38C 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . C37 C39 H39A 109.5 . . C37 C39 H39B 109.5 . . H39A C39 H39B 109.5 . . C37 C39 H39C 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . C41 C40 C42 110.8(4) . . C41 C40 Si2 112.0(3) . . C42 C40 Si2 113.3(3) . . C41 C40 H40 106.8 . . C42 C40 H40 106.8 . . Si2 C40 H40 106.8 . . C40 C41 H41A 109.5 . . C40 C41 H41B 109.5 . . H41A C41 H41B 109.5 . . C40 C41 H41C 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . C40 C42 H42A 109.5 . . C40 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C40 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C44 C43 C45 110.7(4) . . C44 C43 Si2 111.6(3) . . C45 C43 Si2 111.5(3) . . C44 C43 H43 107.6 . . C45 C43 H43 107.6 . . Si2 C43 H43 107.6 . . C43 C44 H44A 109.5 . . C43 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . C43 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . C43 C45 H45A 109.5 . . C43 C45 H45B 109.5 . . H45A C45 H45B 109.5 . . C43 C45 H45C 109.5 . . H45A C45 H45C 109.5 . . H45B C45 H45C 109.5 . . C47 C46 C48 111.2(4) . . C47 C46 Si3 113.9(3) . . C48 C46 Si3 110.9(3) . . C46 C47 H47A 109.5 . . C46 C47 H47B 109.5 . . H47A C47 H47B 109.5 . . C46 C47 H47C 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . C46 C48 H48A 109.5 . . C46 C48 H48B 109.5 . . H48A C48 H48B 109.5 . . C46 C48 H48C 109.5 . . H48A C48 H48C 109.5 . . H48B C48 H48C 109.5 . . C51 C49 C50 110.4(4) . . C51 C49 Si3 109.9(3) . . C50 C49 Si3 110.9(3) . . C49 C50 H50A 109.5 . . C49 C50 H50B 109.5 . . H50A C50 H50B 109.5 . . C49 C50 H50C 109.5 . . H50A C50 H50C 109.5 . . H50B C50 H50C 109.5 . . C49 C51 H51A 109.5 . . C49 C51 H51B 109.5 . . H51A C51 H51B 109.5 . . C49 C51 H51C 109.5 . . H51A C51 H51C 109.5 . . H51B C51 H51C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 C1 2.073(4) . Pd1 Si1 2.3669(12) . Pd1 Si3 2.6358(12) . Pd1 Pd4 2.7028(6) . Pd2 C12 2.073(4) . Pd2 Si2 2.3768(11) . Pd2 Si1 2.6517(12) . Pd2 Pd4 2.6990(8) . Pd3 C23 2.073(4) . Pd3 Si3 2.3693(12) . Pd3 Si2 2.6659(13) . Pd3 Pd4 2.7030(6) . Pd4 Si2 2.2559(11) . Pd4 Si3 2.2603(12) . Pd4 Si1 2.2636(11) . Si1 C34 1.915(4) . Si1 C37 1.915(4) . Si2 C40 1.908(4) . Si2 C43 1.924(4) . Si3 C46 1.919(4) . Si3 C49 1.922(4) . N1 C1 1.360(5) . N1 C2 1.409(5) . N1 C4 1.464(5) . N2 C1 1.358(5) . N2 C3 1.400(5) . N2 C7 1.470(5) . N3 C12 1.375(5) . N3 C13 1.402(5) . N3 C15 1.475(5) . N4 C12 1.348(5) . N4 C14 1.394(5) . N4 C18 1.471(5) . N5 C23 1.363(5) . N5 C24 1.396(5) . N5 C26 1.484(5) . N6 C23 1.363(5) . N6 C25 1.393(5) . N6 C29 1.475(5) . C2 C3 1.345(6) . C2 C10 1.494(6) . C3 C11 1.488(6) . C4 C6 1.521(6) . C4 C5 1.529(6) . C4 H4 1.0000 . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . C7 C8 1.514(6) . C7 C9 1.519(6) . C7 H7 1.0000 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C13 C14 1.333(6) . C13 C21 1.503(6) . C14 C22 1.503(6) . C15 C16 1.511(6) . C15 C17 1.514(6) . C15 H15 1.0000 . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 C19 1.512(6) . C18 C20 1.522(6) . C18 H18 1.0000 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 H20A 0.9800 . C20 H20B 0.9800 . C20 H20C 0.9800 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C24 C25 1.339(6) . C24 C32 1.495(6) . C25 C33 1.509(6) . C26 C28 1.512(5) . C26 C27 1.515(6) . C26 H26 1.0000 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 C30 1.521(6) . C29 C31 1.521(6) . C29 H29 1.0000 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C33 H33A 0.9800 . C33 H33B 0.9800 . C33 H33C 0.9800 . C34 C35 1.522(5) . C34 C36 1.534(5) . C34 H34 1.0000 . C35 H35A 0.9800 . C35 H35B 0.9800 . C35 H35C 0.9800 . C36 H36A 0.9800 . C36 H36B 0.9800 . C36 H36C 0.9800 . C37 C38 1.530(6) . C37 C39 1.533(6) . C37 H37 1.0000 . C38 H38A 0.9800 . C38 H38B 0.9800 . C38 H38C 0.9800 . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 C41 1.522(6) . C40 C42 1.539(6) . C40 H40 1.0000 . C41 H41A 0.9800 . C41 H41B 0.9800 . C41 H41C 0.9800 . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 C44 1.529(6) . C43 C45 1.529(6) . C43 H43 1.0000 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . C46 C47 1.522(6) . C46 C48 1.539(7) . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . C48 H48A 0.9800 . C48 H48B 0.9800 . C48 H48C 0.9800 . C49 C51 1.517(7) . C49 C50 1.534(6) . C50 H50A 0.9800 . C50 H50B 0.9800 . C50 H50C 0.9800 . C51 H51A 0.9800 . C51 H51B 0.9800 . C51 H51C 0.9800 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C3 N2 C1 N1 -0.4(4) . . . . C7 N2 C1 N1 174.4(3) . . . . C3 N2 C1 Pd1 175.4(3) . . . . C7 N2 C1 Pd1 -9.8(5) . . . . C2 N1 C1 N2 0.0(4) . . . . C4 N1 C1 N2 -173.4(3) . . . . C2 N1 C1 Pd1 -176.1(3) . . . . C4 N1 C1 Pd1 10.5(5) . . . . C1 N1 C2 C3 0.4(5) . . . . C4 N1 C2 C3 173.1(4) . . . . C1 N1 C2 C10 177.6(4) . . . . C4 N1 C2 C10 -9.7(6) . . . . N1 C2 C3 N2 -0.6(4) . . . . C10 C2 C3 N2 -177.6(4) . . . . N1 C2 C3 C11 177.7(4) . . . . C10 C2 C3 C11 0.8(8) . . . . C1 N2 C3 C2 0.7(5) . . . . C7 N2 C3 C2 -173.6(4) . . . . C1 N2 C3 C11 -177.7(4) . . . . C7 N2 C3 C11 8.0(7) . . . . C1 N1 C4 C6 102.1(4) . . . . C2 N1 C4 C6 -70.0(5) . . . . C1 N1 C4 C5 -128.8(4) . . . . C2 N1 C4 C5 59.1(5) . . . . C1 N2 C7 C8 130.4(4) . . . . C3 N2 C7 C8 -55.8(5) . . . . C1 N2 C7 C9 -101.7(4) . . . . C3 N2 C7 C9 72.1(5) . . . . C14 N4 C12 N3 0.2(4) . . . . C18 N4 C12 N3 -178.9(3) . . . . C14 N4 C12 Pd2 -177.9(3) . . . . C18 N4 C12 Pd2 3.0(5) . . . . C13 N3 C12 N4 -1.3(4) . . . . C15 N3 C12 N4 -176.3(3) . . . . C13 N3 C12 Pd2 176.9(3) . . . . C15 N3 C12 Pd2 1.8(5) . . . . C12 N3 C13 C14 2.0(5) . . . . C15 N3 C13 C14 176.4(4) . . . . C12 N3 C13 C21 -179.5(4) . . . . C15 N3 C13 C21 -5.1(7) . . . . N3 C13 C14 N4 -1.8(5) . . . . C21 C13 C14 N4 179.8(4) . . . . N3 C13 C14 C22 -179.5(5) . . . . C21 C13 C14 C22 2.1(8) . . . . C12 N4 C14 C13 1.0(5) . . . . C18 N4 C14 C13 180.0(4) . . . . C12 N4 C14 C22 178.8(4) . . . . C18 N4 C14 C22 -2.2(7) . . . . C12 N3 C15 C16 -126.7(4) . . . . C13 N3 C15 C16 59.4(6) . . . . C12 N3 C15 C17 104.8(4) . . . . C13 N3 C15 C17 -69.2(5) . . . . C12 N4 C18 C19 110.6(4) . . . . C14 N4 C18 C19 -68.3(5) . . . . C12 N4 C18 C20 -120.2(4) . . . . C14 N4 C18 C20 60.9(5) . . . . C24 N5 C23 N6 0.6(4) . . . . C26 N5 C23 N6 -179.1(3) . . . . C24 N5 C23 Pd3 -175.2(3) . . . . C26 N5 C23 Pd3 5.0(5) . . . . C25 N6 C23 N5 -0.3(4) . . . . C29 N6 C23 N5 -176.2(3) . . . . C25 N6 C23 Pd3 175.5(3) . . . . C29 N6 C23 Pd3 -0.4(5) . . . . C23 N5 C24 C25 -0.6(5) . . . . C26 N5 C24 C25 179.0(4) . . . . C23 N5 C24 C32 178.9(4) . . . . C26 N5 C24 C32 -1.4(7) . . . . N5 C24 C25 N6 0.4(5) . . . . C32 C24 C25 N6 -179.1(4) . . . . N5 C24 C25 C33 178.7(4) . . . . C32 C24 C25 C33 -0.8(8) . . . . C23 N6 C25 C24 -0.1(5) . . . . C29 N6 C25 C24 175.4(4) . . . . C23 N6 C25 C33 -178.4(4) . . . . C29 N6 C25 C33 -3.0(7) . . . . C23 N5 C26 C28 110.3(4) . . . . C24 N5 C26 C28 -69.4(5) . . . . C23 N5 C26 C27 -121.2(4) . . . . C24 N5 C26 C27 59.2(5) . . . . C23 N6 C29 C30 103.3(4) . . . . C25 N6 C29 C30 -71.7(5) . . . . C23 N6 C29 C31 -128.7(4) . . . . C25 N6 C29 C31 56.2(5) . . . .