#------------------------------------------------------------------------------ #$Date: 2021-08-11 01:17:46 +0300 (Wed, 11 Aug 2021) $ #$Revision: 268012 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564339.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_1564339 loop_ _publ_author_name 'Chen, Qiu-Cheng' 'Fridman, Natalia' 'Tumanskii, Boris L.' 'Gross, Zeev' _publ_section_title ; Chromophore-Supported Structural and Functional Model of Dinuclear Copper Enzymes, for Facilitating Mechanism of Action Studies ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02593G _journal_year 2021 _chemical_formula_moiety 'C57 H21 F20 N5 Pd, 3(C4 H8 O)' _chemical_formula_sum 'C69 H45 F20 N5 O3 Pd' _chemical_formula_weight 1478.50 _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 _audit_block_doi 10.5517/ccdc.csd.cc24wl7w _audit_creation_date 2020-02-16 _audit_creation_method ; Olex2 1.3 (compiled 2019.11.21 svn.r41b79517 for OlexSys, GUI svn.r6003) ; _audit_update_record ; 2020-03-25 deposited with the CCDC. 2021-08-09 downloaded from the CCDC. ; _cell_angle_alpha 89.120(2) _cell_angle_beta 86.471(2) _cell_angle_gamma 86.785(2) _cell_formula_units_Z 2 _cell_length_a 7.8433(2) _cell_length_b 18.5899(5) _cell_length_c 21.0630(5) _cell_measurement_reflns_used 17859 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 79.0950 _cell_measurement_theta_min 4.7640 _cell_volume 3060.25(13) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _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 -37.00 89.00 0.50 11.28 -- 0.00 82.00 -90.00 252 2 \w -89.00 56.00 0.50 11.28 -- 0.00 -19.00 -60.00 290 3 \w -35.00 89.00 0.50 11.28 -- 0.00 77.00 150.00 248 4 \w -35.00 89.00 0.50 11.28 -- 0.00 77.00 150.00 248 5 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00 -30.00 254 6 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00-180.00 254 7 \w 18.00 143.00 0.50 45.13 -- 107.20 -77.00 150.00 250 8 \w 18.00 197.00 0.50 45.13 -- 107.20 15.00 120.00 358 9 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00 90.00 254 10 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00-150.00 254 11 \w 77.00 197.00 0.50 45.13 -- 107.20 45.00-120.00 240 12 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00 -90.00 254 13 \w 70.00 197.00 0.50 45.13 -- 107.20 82.00 120.00 254 14 \w 18.00 145.00 0.50 45.13 -- 107.20 -82.00 30.00 254 15 \w 77.00 197.00 0.50 45.13 -- 107.20 61.00 -30.00 240 16 \w 18.00 138.00 0.50 45.13 -- 107.20 -61.00 30.00 240 17 \w 77.00 179.00 0.50 45.13 -- 107.20 45.00 -90.00 204 18 \w 20.00 111.00 0.50 45.13 -- 107.20 -30.00 -60.00 182 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1599148000 _diffrn_orient_matrix_UB_12 -0.0008929000 _diffrn_orient_matrix_UB_13 -0.0463327000 _diffrn_orient_matrix_UB_21 -0.0374765000 _diffrn_orient_matrix_UB_22 0.0803880000 _diffrn_orient_matrix_UB_23 -0.0154646000 _diffrn_orient_matrix_UB_31 0.1089397000 _diffrn_orient_matrix_UB_32 0.0206682000 _diffrn_orient_matrix_UB_33 0.0546332000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 47309 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.067 _diffrn_reflns_theta_min 4.206 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.475 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.605 _exptl_crystal_description needle _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.075 _exptl_crystal_size_mid 0.029 _exptl_crystal_size_min 0.023 _refine_diff_density_max 1.428 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 929 _refine_ls_number_reflns 11605 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.131 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0706 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+6.0371P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1806 _refine_ls_wR_factor_ref 0.1841 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10505 _reflns_number_total 11605 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02593g2.cif _cod_data_source_block zg11 _cod_database_code 1564339 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C55H18F20N5Pd1 _chemical_oxdiff_usercomment 'vial 2 perfluorinated ether' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.69 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 69.95 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2. Others Sof(Pd1A)=Sof(H1)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)=Sof(H50A)=Sof(C51A)= Sof(H51A)=Sof(C52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)= Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=1-FVAR(1) Sof(Pd1)=Sof(H5)=Sof(C51)=Sof(H51)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)= Sof(H50)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)= Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=FVAR(1) 3.a Secondary CH2 refined with riding coordinates: C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A, H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B) 3.b Aromatic/amide H refined with riding coordinates: N1(H1), N3(H3), N5(H5), C2(H2), C51(H51), C3(H3A), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18), C22(H22), C23(H23), C50(H50), C50A(H50A), C51A(H51A), C53(H53), C53A(H53A), C54(H54), C54A(H54A), C55(H55), C55A(H55A), C56(H56), C56A(H56A), C57(H57), C57A(H57A) 3.c X=CH2 refined with riding coordinates: C49(H49A,H49B), C49A(H49C,H49D) ; _shelx_res_file ; zg11.res created by SHELXL-2014/7 TITL zg11_a.res in P-1 REM Old TITL zg11_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.156, Rweak 0.021, Alpha 0.078, Orientation as input REM Formula found by SHELXT: C69 N6 F20 Pd O2 K CELL 1.54184 7.8433 18.5899 21.063 89.12 86.471 86.785 ZERR 2 0.0002 0.0005 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H F N O Pd UNIT 138 90 40 10 6 2 L.S. 4 0 0 PLAN 2 TEMP -173 CONF BOND $H list 4 WPDB -2 MORE -1 fmap 2 53 acta OMIT 0 -1 3 REM REM REM WGHT 0.085800 6.037100 FVAR 0.40196 0.71190 PART 1 PD1 6 0.397102 0.279925 0.641128 21.00000 0.03221 0.03179 = 0.02341 0.00144 -0.00355 -0.00205 PART 0 PART 2 PD1A 6 0.371623 0.350499 0.744454 -21.00000 0.03446 0.03448 = 0.02781 -0.00069 -0.00313 -0.00131 PART 0 F26 3 0.576234 0.266793 0.392983 11.00000 0.04414 0.05569 = 0.03182 0.00208 -0.00325 -0.00408 F27 3 0.532921 0.262113 0.267428 11.00000 0.06861 0.04761 = 0.02719 0.00110 0.00553 -0.00380 F28 3 0.213282 0.274677 0.224373 11.00000 0.09071 0.05985 = 0.02562 -0.00550 -0.01761 0.00244 F29 3 -0.062538 0.292748 0.307780 11.00000 0.06287 0.07859 = 0.05094 -0.01133 -0.02834 0.00803 F30 3 -0.021792 0.296199 0.433180 11.00000 0.04467 0.06798 = 0.04049 -0.00670 -0.00474 0.00069 F32 3 0.436944 0.025666 0.653379 11.00000 0.05878 0.04672 = 0.05854 0.00933 0.00332 0.00742 F33 3 0.426784 -0.112595 0.687928 11.00000 0.11131 0.04215 = 0.06834 0.00158 -0.00666 0.01968 F34 3 0.130957 -0.163476 0.742175 11.00000 0.16974 0.03561 = 0.10766 0.01366 0.00897 -0.01625 F35 3 -0.152852 -0.073784 0.758439 11.00000 0.11186 0.07073 = 0.12549 0.01956 0.01912 -0.04447 F36 3 -0.143300 0.065508 0.724066 11.00000 0.05412 0.06485 = 0.06780 0.00733 0.00434 -0.01678 F38 3 0.378933 0.241939 0.942797 11.00000 0.05804 0.05395 = 0.05853 0.00304 -0.02269 -0.00622 F39 3 0.360176 0.148129 1.040289 11.00000 0.10108 0.06186 = 0.05936 0.00616 -0.04246 0.00738 F40 3 0.076959 0.070863 1.061858 11.00000 0.11332 0.05284 = 0.04505 0.01411 -0.00985 0.00143 F41 3 -0.185323 0.088551 0.983926 11.00000 0.07372 0.05356 = 0.05029 0.00696 0.01067 -0.01179 F42 3 -0.170209 0.183520 0.887432 11.00000 0.04308 0.05695 = 0.04452 0.00649 -0.00404 -0.00749 F44 3 0.545283 0.593992 0.824999 11.00000 0.04854 0.05437 = 0.05467 -0.01933 0.00215 -0.00803 F45 3 0.529365 0.723824 0.880770 11.00000 0.07430 0.06370 = 0.05851 -0.02672 0.01007 -0.02959 F46 3 0.224595 0.787201 0.920881 11.00000 0.09829 0.04627 = 0.05569 -0.02494 0.01619 -0.01178 F47 3 -0.067363 0.717964 0.908902 11.00000 0.06960 0.05600 = 0.05834 -0.01714 0.01148 0.00935 F48 3 -0.054621 0.588292 0.853942 11.00000 0.04639 0.05438 = 0.05204 -0.00647 0.00395 -0.00253 N1 4 0.319734 0.363102 0.578229 11.00000 0.03771 0.03187 = 0.02613 0.00216 -0.00504 -0.00115 PART 2 AFIX 43 H1 2 0.321096 0.331507 0.609761 -21.00000 -1.20000 AFIX 0 PART 0 N2 4 0.256653 0.212449 0.586426 11.00000 0.04472 0.03601 = 0.02574 0.00071 -0.00234 -0.00640 N3 4 0.106847 0.181023 0.773718 11.00000 0.03676 0.03179 = 0.02800 0.00443 -0.00155 -0.00523 AFIX 43 H3 2 0.126089 0.141795 0.796685 11.00000 -1.20000 AFIX 0 N4 4 0.200293 0.387299 0.819432 11.00000 0.03804 0.04063 = 0.03651 -0.00377 0.00476 -0.00692 N5 4 0.288944 0.456000 0.701623 11.00000 0.04024 0.03311 = 0.03088 -0.00320 0.00080 -0.00565 PART 1 AFIX 43 H5 2 0.274776 0.411356 0.714497 21.00000 -1.20000 AFIX 0 PART 0 C1 1 0.323245 0.434651 0.583447 11.00000 0.02985 0.03968 = 0.02825 0.00137 -0.00225 -0.00485 C2 1 0.322557 0.468008 0.522529 11.00000 0.04295 0.03272 = 0.03326 0.00118 -0.00073 -0.00853 AFIX 43 H2 2 0.326150 0.518138 0.513463 11.00000 -1.20000 AFIX 0 PART 1 C51 1 0.576128 0.330780 0.699756 21.00000 0.03539 0.03874 = 0.03511 -0.00829 -0.01856 -0.00696 AFIX 43 H51 2 0.473283 0.344629 0.723730 21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.315753 0.414443 0.479372 11.00000 0.04232 0.03853 = 0.02838 0.00323 -0.00036 -0.00695 AFIX 43 H3A 2 0.312979 0.420278 0.434554 11.00000 -1.20000 AFIX 0 C4 1 0.313573 0.347687 0.514325 11.00000 0.03356 0.03801 = 0.02568 0.00455 -0.00600 -0.00254 C5 1 0.295353 0.279904 0.488036 11.00000 0.03759 0.03922 = 0.02757 0.00067 -0.00188 -0.00276 C6 1 0.269113 0.215463 0.521137 11.00000 0.04654 0.03554 = 0.02618 -0.00163 -0.00522 0.00003 C7 1 0.235556 0.146777 0.497482 11.00000 0.05997 0.04104 = 0.02611 -0.00115 -0.00316 -0.00517 AFIX 43 H7 2 0.237442 0.134052 0.453924 11.00000 -1.20000 AFIX 0 C8 1 0.200524 0.102726 0.547642 11.00000 0.05895 0.03424 = 0.03454 -0.00170 -0.00957 -0.00540 AFIX 43 H8 2 0.176116 0.053314 0.546251 11.00000 -1.20000 AFIX 0 C9 1 0.207560 0.145463 0.603362 11.00000 0.04106 0.03316 = 0.03355 0.00035 -0.00739 -0.00433 C10 1 0.151408 0.127409 0.666778 11.00000 0.03663 0.03666 = 0.03152 0.00270 -0.00822 -0.00356 C11 1 0.099712 0.183410 0.708374 11.00000 0.03276 0.03861 = 0.02804 0.00210 -0.00485 -0.00466 C12 1 0.044107 0.255243 0.691947 11.00000 0.03018 0.03773 = 0.03148 0.00628 -0.00336 -0.00342 AFIX 43 H12 2 0.021222 0.272282 0.650408 11.00000 -1.20000 AFIX 0 C13 1 0.029376 0.295101 0.745437 11.00000 0.03121 0.03461 = 0.03595 0.00227 -0.00716 -0.00236 AFIX 43 H13 2 -0.007614 0.344574 0.747960 11.00000 -1.20000 AFIX 0 C14 1 0.078972 0.250045 0.797459 11.00000 0.03328 0.03305 = 0.03547 0.00238 -0.00011 -0.00374 C15 1 0.111326 0.271041 0.858665 11.00000 0.03574 0.03759 = 0.03193 0.00063 0.00003 0.00210 C16 1 0.152691 0.343137 0.868676 11.00000 0.03954 0.03834 = 0.03151 -0.00222 -0.00212 0.00186 C17 1 0.140870 0.382238 0.927698 11.00000 0.05362 0.04272 = 0.02619 -0.00147 -0.00274 0.00197 AFIX 43 H17 2 0.114465 0.363302 0.969064 11.00000 -1.20000 AFIX 0 C18 1 0.174909 0.451288 0.912371 11.00000 0.05313 0.03901 = 0.02817 -0.00568 -0.00480 0.00398 AFIX 43 H18 2 0.174149 0.490426 0.940881 11.00000 -1.20000 AFIX 0 C19 1 0.212637 0.453968 0.844247 11.00000 0.03850 0.03802 = 0.03168 -0.00558 -0.00371 -0.00414 C20 1 0.250345 0.514346 0.807201 11.00000 0.03827 0.03593 = 0.03600 -0.00459 -0.00227 -0.00481 C21 1 0.284269 0.514786 0.740416 11.00000 0.03951 0.03278 = 0.03428 -0.00297 0.00035 -0.00226 C22 1 0.312543 0.575966 0.700972 11.00000 0.04423 0.03155 = 0.03327 -0.00151 -0.00249 -0.00241 AFIX 43 H22 2 0.315895 0.624249 0.714777 11.00000 -1.20000 AFIX 0 C23 1 0.334190 0.552942 0.639307 11.00000 0.04700 0.03938 = 0.03310 0.00189 -0.00611 -0.00245 AFIX 43 H23 2 0.355568 0.582234 0.602639 11.00000 -1.20000 AFIX 0 C24 1 0.318768 0.477456 0.640443 11.00000 0.03396 0.03590 = 0.02814 -0.00226 -0.00080 -0.00139 C25 1 0.277930 0.278881 0.417350 11.00000 0.04566 0.03181 = 0.02680 -0.00063 -0.00357 -0.00254 C26 1 0.416815 0.271990 0.373699 11.00000 0.04521 0.03531 = 0.02742 0.00250 -0.00418 -0.00373 C27 1 0.395382 0.269761 0.308098 11.00000 0.05901 0.03204 = 0.02477 -0.00101 0.00139 -0.00277 C28 1 0.235644 0.276289 0.286509 11.00000 0.07227 0.03555 = 0.02835 -0.00092 -0.01145 0.00000 C29 1 0.095163 0.285268 0.328680 11.00000 0.05715 0.04222 = 0.03742 -0.00338 -0.01564 0.00228 C30 1 0.118399 0.286343 0.393454 11.00000 0.04622 0.04075 = 0.03521 -0.00251 -0.00406 -0.00198 C31 1 0.147079 0.050861 0.686951 11.00000 0.05469 0.03484 = 0.02724 0.00017 -0.00878 -0.00906 C32 1 0.289194 0.003015 0.678209 11.00000 0.05864 0.03876 = 0.03670 -0.00019 -0.00858 -0.00143 C33 1 0.284586 -0.068613 0.695766 11.00000 0.09814 0.03437 = 0.04400 -0.00476 -0.00861 0.00409 C34 1 0.135669 -0.094968 0.723867 11.00000 0.12051 0.03057 = 0.06079 0.00125 -0.00139 -0.01768 C35 1 -0.006438 -0.049589 0.732222 11.00000 0.09461 0.05110 = 0.05610 0.00603 0.00211 -0.03081 C36 1 0.000263 0.022902 0.715110 11.00000 0.06169 0.04932 = 0.04422 -0.00055 -0.00657 -0.01462 C37 1 0.102742 0.217877 0.911980 11.00000 0.04531 0.03422 = 0.02839 -0.00421 -0.00241 0.00215 C38 1 0.236497 0.206498 0.952636 11.00000 0.05298 0.04101 = 0.03540 -0.00462 -0.00977 0.00186 C39 1 0.227877 0.157584 1.002406 11.00000 0.07363 0.04357 = 0.03671 -0.00170 -0.01793 0.01061 C40 1 0.087346 0.117409 1.013044 11.00000 0.08215 0.04207 = 0.02984 0.00351 -0.00471 0.00444 C41 1 -0.046382 0.126574 0.973908 11.00000 0.06608 0.03833 = 0.03606 -0.00170 0.00625 -0.00207 C42 1 -0.036079 0.176219 0.924104 11.00000 0.04775 0.04226 = 0.03050 -0.00146 -0.00035 0.00585 C43 1 0.246047 0.586570 0.838375 11.00000 0.04743 0.03885 = 0.02705 -0.00251 0.00146 -0.00518 C44 1 0.391401 0.622847 0.845713 11.00000 0.04951 0.04255 = 0.03630 -0.00677 0.00361 -0.00586 C45 1 0.386911 0.690363 0.873763 11.00000 0.06058 0.04895 = 0.03190 -0.00877 0.00320 -0.01352 C46 1 0.230319 0.721877 0.894359 11.00000 0.07477 0.04146 = 0.03111 -0.01021 0.00836 -0.00624 C47 1 0.083036 0.686987 0.888246 11.00000 0.06294 0.04310 = 0.03656 -0.00576 0.00586 0.00373 C48 1 0.092787 0.620082 0.860076 11.00000 0.04817 0.04097 = 0.03226 -0.00237 0.00132 -0.00406 PART 1 C49 1 0.495636 0.206784 0.711094 21.00000 0.03802 0.03495 = 0.03516 0.00964 -0.01217 0.00441 AFIX 93 H49A 2 0.387180 0.223519 0.729387 21.00000 -1.20000 H49B 2 0.521405 0.156585 0.705989 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C49A 1 0.477266 0.245359 0.772421 -21.00000 0.03605 AFIX 93 H49C 2 0.378849 0.236399 0.750266 -21.00000 -1.20000 H49D 2 0.489760 0.225695 0.813879 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C50 1 0.618378 0.256458 0.691517 21.00000 0.02852 0.04200 = 0.02800 0.00562 -0.00970 0.00245 AFIX 43 H50 2 0.727218 0.240300 0.673170 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C50A 1 0.607794 0.288842 0.743095 -21.00000 0.03483 AFIX 43 H50A 2 0.708478 0.299385 0.763203 -21.00000 -1.20000 AFIX 0 C51A 1 0.571129 0.314271 0.681397 -21.00000 0.03210 AFIX 43 H51A 2 0.479342 0.298512 0.658721 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C52 1 0.682292 0.387457 0.673343 21.00000 0.03592 0.02644 = 0.03736 -0.00110 -0.01384 0.00239 PART 0 PART 2 C52A 1 0.695201 0.369940 0.655020 -21.00000 0.03650 PART 0 PART 1 C53 1 0.778027 0.381383 0.615853 21.00000 0.03823 0.03574 = 0.05016 0.00418 -0.01663 -0.00282 AFIX 43 H53 2 0.766217 0.340119 0.590774 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C53A 1 0.767219 0.367465 0.596776 -21.00000 0.04209 AFIX 43 H53A 2 0.738500 0.328021 0.572131 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C54 1 0.889752 0.432110 0.593031 21.00000 0.02975 0.03637 = 0.07411 0.01467 -0.01038 0.00196 AFIX 43 H54 2 0.953058 0.426368 0.553341 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C54A 1 0.872761 0.411466 0.567810 -21.00000 0.07307 AFIX 43 H54A 2 0.917218 0.404561 0.525228 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C55 1 0.905597 0.493058 0.631504 21.00000 0.03367 0.03663 = 0.09218 0.00968 -0.01101 -0.00612 AFIX 43 H55 2 0.982468 0.528824 0.618204 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C55A 1 0.916425 0.471726 0.606052 -21.00000 0.05900 AFIX 43 H55A 2 0.998086 0.503475 0.588447 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C56 1 0.807845 0.500355 0.689016 21.00000 0.04137 0.03499 = 0.08303 -0.00104 -0.02645 -0.00218 AFIX 43 H56 2 0.818514 0.541282 0.714642 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C56A 1 0.845709 0.484794 0.665955 -21.00000 0.05255 AFIX 43 H56A 2 0.869844 0.525785 0.689533 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C57 1 0.697121 0.449257 0.708772 21.00000 0.04605 0.03630 = 0.05454 -0.00565 -0.01803 0.00497 AFIX 43 H57 2 0.629040 0.455958 0.747330 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C57A 1 0.729015 0.430290 0.691129 -21.00000 0.04137 AFIX 43 H57A 2 0.675392 0.435913 0.732573 -21.00000 -1.20000 AFIX 0 PART 0 O1 5 0.312191 0.072912 0.835974 11.00000 0.05925 0.04786 = 0.05528 0.01729 -0.01206 0.00287 C58 1 0.492828 0.073654 0.838127 11.00000 0.05731 0.08780 = 0.09996 0.04020 -0.00872 -0.00018 AFIX 23 H58A 2 0.525008 0.119195 0.856720 11.00000 -1.20000 H58B 2 0.548384 0.069308 0.794759 11.00000 -1.20000 AFIX 0 C59 1 0.547248 0.010895 0.878602 11.00000 0.07939 0.09766 = 0.11651 0.04453 -0.03486 0.00146 AFIX 23 H59A 2 0.660725 -0.010270 0.863304 11.00000 -1.20000 H59B 2 0.551534 0.024919 0.923605 11.00000 -1.20000 AFIX 0 C60 1 0.411058 -0.039925 0.870825 11.00000 0.09366 0.06905 = 0.09627 0.02327 -0.00883 0.01576 AFIX 23 H60A 2 0.434048 -0.068466 0.831626 11.00000 -1.20000 H60B 2 0.399713 -0.073126 0.907857 11.00000 -1.20000 AFIX 0 C61 1 0.256912 0.008717 0.866570 11.00000 0.06928 0.04477 = 0.05395 0.00465 -0.00107 -0.00025 AFIX 23 H61A 2 0.171651 -0.013623 0.841491 11.00000 -1.20000 H61B 2 0.204242 0.019406 0.909554 11.00000 -1.20000 AFIX 0 O2 5 0.717339 0.417825 0.988164 11.00000 0.08658 0.07187 = 0.03208 -0.00426 -0.00747 -0.02265 C62 1 0.698082 0.474605 0.942249 11.00000 0.09143 0.06319 = 0.03955 -0.00139 0.00613 -0.00487 AFIX 23 H62A 2 0.789397 0.508927 0.944822 11.00000 -1.20000 H62B 2 0.585666 0.501118 0.949372 11.00000 -1.20000 AFIX 0 C63 1 0.711120 0.438350 0.878471 11.00000 0.06923 0.07661 = 0.03170 -0.00322 -0.00916 0.01190 AFIX 23 H63A 2 0.640337 0.465266 0.847762 11.00000 -1.20000 H63B 2 0.831171 0.434130 0.860850 11.00000 -1.20000 AFIX 0 C64 1 0.644069 0.365238 0.893306 11.00000 0.05121 0.07796 = 0.04564 -0.01978 -0.00935 0.00174 AFIX 23 H64A 2 0.524165 0.363449 0.881486 11.00000 -1.20000 H64B 2 0.714732 0.327167 0.870107 11.00000 -1.20000 AFIX 0 C65 1 0.655654 0.355827 0.963911 11.00000 0.11673 0.06897 = 0.05128 0.00180 -0.03122 -0.02099 AFIX 23 H65A 2 0.541257 0.347316 0.984248 11.00000 -1.20000 H65B 2 0.733540 0.313678 0.973025 11.00000 -1.20000 AFIX 0 O3 5 0.828892 0.068669 0.476331 11.00000 0.08435 0.04716 = 0.05584 -0.01180 0.00536 -0.00669 C66 1 0.767548 0.137382 0.459257 11.00000 0.08917 0.05088 = 0.04570 -0.01001 -0.01221 -0.00033 AFIX 23 H66A 2 0.652852 0.135797 0.442326 11.00000 -1.20000 H66B 2 0.845816 0.158651 0.426347 11.00000 -1.20000 AFIX 0 C67 1 0.758291 0.181477 0.520084 11.00000 0.06228 0.04521 = 0.04121 -0.00857 -0.00628 -0.00061 AFIX 23 H67A 2 0.869299 0.202075 0.526939 11.00000 -1.20000 H67B 2 0.668110 0.220875 0.519223 11.00000 -1.20000 AFIX 0 C68 1 0.714166 0.124971 0.570729 11.00000 0.06082 0.05761 = 0.04688 -0.00262 -0.00436 -0.00249 AFIX 23 H68A 2 0.784769 0.129034 0.607751 11.00000 -1.20000 H68B 2 0.591860 0.130539 0.585429 11.00000 -1.20000 AFIX 0 C69 1 0.753315 0.053192 0.538048 11.00000 0.08719 0.05060 = 0.06121 -0.00335 -0.00178 -0.01174 AFIX 23 H69A 2 0.833354 0.022383 0.562600 11.00000 -1.20000 H69B 2 0.646936 0.027651 0.534551 11.00000 -1.20000 AFIX 0 HKLF 4 REM zg11_a.res in P-1 REM R1 = 0.0706 for 10505 Fo > 4sig(Fo) and 0.0759 for all 11605 data REM 929 parameters refined using 0 restraints END WGHT 0.0858 6.0375 REM Highest difference peak 1.428, deepest hole -1.110, 1-sigma level 0.092 Q1 1 0.5075 0.3019 0.6349 11.00000 0.05 1.43 Q2 1 0.3320 0.3262 0.6399 11.00000 0.05 1.19 ; _shelx_res_checksum 65684 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.560 _oxdiff_exptl_absorpt_empirical_full_min 0.716 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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 0.39710(5) 0.27992(2) 0.64113(2) 0.02907(14) Uani 0.7119(12) 1 d . . P A 1 Pd1A Pd 0.37162(13) 0.35050(6) 0.74445(5) 0.0322(4) Uani 0.2881(12) 1 d . . P A 2 F26 F 0.5762(3) 0.26679(15) 0.39298(11) 0.0438(6) Uani 1 1 d . . . . . F27 F 0.5329(4) 0.26211(15) 0.26743(11) 0.0481(6) Uani 1 1 d . . . . . F28 F 0.2133(4) 0.27468(16) 0.22437(12) 0.0583(8) Uani 1 1 d . . . . . F29 F -0.0625(4) 0.29275(19) 0.30778(15) 0.0634(8) Uani 1 1 d . . . . . F30 F -0.0218(3) 0.29620(16) 0.43318(13) 0.0510(7) Uani 1 1 d . . . . . F32 F 0.4369(4) 0.02567(15) 0.65338(15) 0.0555(7) Uani 1 1 d . . . . . F33 F 0.4268(5) -0.11259(17) 0.68793(17) 0.0748(10) Uani 1 1 d . . . . . F34 F 0.1310(7) -0.16348(19) 0.7422(2) 0.1048(16) Uani 1 1 d . . . . . F35 F -0.1529(6) -0.0738(2) 0.7584(2) 0.1025(15) Uani 1 1 d . . . . . F36 F -0.1433(4) 0.06551(18) 0.72407(16) 0.0622(8) Uani 1 1 d . . . . . F38 F 0.3789(4) 0.24194(16) 0.94280(15) 0.0560(7) Uani 1 1 d . . . . . F39 F 0.3602(5) 0.14813(18) 1.04029(16) 0.0731(10) Uani 1 1 d . . . . . F40 F 0.0770(5) 0.07086(17) 1.06186(15) 0.0706(9) Uani 1 1 d . . . . . F41 F -0.1853(4) 0.08855(16) 0.98393(14) 0.0596(8) Uani 1 1 d . . . . . F42 F -0.1702(3) 0.18352(15) 0.88743(13) 0.0480(6) Uani 1 1 d . . . . . F44 F 0.5453(4) 0.59399(16) 0.82500(14) 0.0524(7) Uani 1 1 d . . . . . F45 F 0.5294(4) 0.72382(18) 0.88077(15) 0.0648(9) Uani 1 1 d . . . . . F46 F 0.2246(5) 0.78720(16) 0.92088(15) 0.0671(9) Uani 1 1 d . . . . . F47 F -0.0674(4) 0.71796(17) 0.90890(15) 0.0623(8) Uani 1 1 d . . . . . F48 F -0.0546(4) 0.58829(16) 0.85394(14) 0.0512(7) Uani 1 1 d . . . . . N1 N 0.3197(4) 0.36310(18) 0.57823(15) 0.0318(7) Uani 1 1 d . . . . . H1 H 0.3211 0.3315 0.6098 0.038 Uiso 0.2881(12) 1 calc R U P A 2 N2 N 0.2567(5) 0.21245(19) 0.58643(16) 0.0353(7) Uani 1 1 d . . . . . N3 N 0.1068(4) 0.18102(18) 0.77372(15) 0.0321(7) Uani 1 1 d . . . . . H3 H 0.1261 0.1418 0.7967 0.039 Uiso 1 1 calc R U . . . N4 N 0.2003(5) 0.3873(2) 0.81943(17) 0.0385(8) Uani 1 1 d . . . . . N5 N 0.2889(4) 0.45600(19) 0.70162(16) 0.0347(7) Uani 1 1 d . . . . . H5 H 0.2748 0.4114 0.7145 0.042 Uiso 0.7119(12) 1 calc R U P A 1 C1 C 0.3232(5) 0.4347(2) 0.58345(19) 0.0325(8) Uani 1 1 d . . . . . C2 C 0.3226(6) 0.4680(2) 0.5225(2) 0.0362(9) Uani 1 1 d . . . . . H2 H 0.3261 0.5181 0.5135 0.043 Uiso 1 1 calc R U . . . C51 C 0.5761(9) 0.3308(4) 0.6998(4) 0.0355(16) Uani 0.7119(12) 1 d . . P A 1 H51 H 0.4733 0.3446 0.7237 0.043 Uiso 0.7119(12) 1 calc R U P A 1 C3 C 0.3158(6) 0.4144(2) 0.4794(2) 0.0363(9) Uani 1 1 d . . . . . H3A H 0.3130 0.4203 0.4346 0.044 Uiso 1 1 calc R U . . . C4 C 0.3136(5) 0.3477(2) 0.51433(18) 0.0323(8) Uani 1 1 d . . . . . C5 C 0.2954(5) 0.2799(2) 0.48804(19) 0.0348(9) Uani 1 1 d . . . . . C6 C 0.2691(6) 0.2155(2) 0.52114(19) 0.0360(9) Uani 1 1 d . . . . . C7 C 0.2356(6) 0.1468(2) 0.4975(2) 0.0423(10) Uani 1 1 d . . . . . H7 H 0.2374 0.1341 0.4539 0.051 Uiso 1 1 calc R U . . . C8 C 0.2005(6) 0.1027(2) 0.5476(2) 0.0422(10) Uani 1 1 d . . . . . H8 H 0.1761 0.0533 0.5463 0.051 Uiso 1 1 calc R U . . . C9 C 0.2076(6) 0.1455(2) 0.6034(2) 0.0356(9) Uani 1 1 d . . . . . C10 C 0.1514(5) 0.1274(2) 0.6668(2) 0.0347(9) Uani 1 1 d . . . . . C11 C 0.0997(5) 0.1834(2) 0.70837(19) 0.0329(8) Uani 1 1 d . . . . . C12 C 0.0441(5) 0.2552(2) 0.69195(19) 0.0331(8) Uani 1 1 d . . . . . H12 H 0.0212 0.2723 0.6504 0.040 Uiso 1 1 calc R U . . . C13 C 0.0294(5) 0.2951(2) 0.7454(2) 0.0337(8) Uani 1 1 d . . . . . H13 H -0.0076 0.3446 0.7480 0.040 Uiso 1 1 calc R U . . . C14 C 0.0790(5) 0.2500(2) 0.7975(2) 0.0340(8) Uani 1 1 d . . . . . C15 C 0.1113(5) 0.2710(2) 0.8587(2) 0.0353(9) Uani 1 1 d . . . . . C16 C 0.1527(6) 0.3431(2) 0.8687(2) 0.0366(9) Uani 1 1 d . . . . . C17 C 0.1409(6) 0.3822(2) 0.9277(2) 0.0410(10) Uani 1 1 d . . . . . H17 H 0.1145 0.3633 0.9691 0.049 Uiso 1 1 calc R U . . . C18 C 0.1749(6) 0.4513(2) 0.9124(2) 0.0402(10) Uani 1 1 d . . . . . H18 H 0.1741 0.4904 0.9409 0.048 Uiso 1 1 calc R U . . . C19 C 0.2126(5) 0.4540(2) 0.8442(2) 0.0359(9) Uani 1 1 d . . . . . C20 C 0.2503(5) 0.5143(2) 0.8072(2) 0.0366(9) Uani 1 1 d . . . . . C21 C 0.2843(5) 0.5148(2) 0.7404(2) 0.0356(9) Uani 1 1 d . . . . . C22 C 0.3125(6) 0.5760(2) 0.7010(2) 0.0363(9) Uani 1 1 d . . . . . H22 H 0.3159 0.6242 0.7148 0.044 Uiso 1 1 calc R U . . . C23 C 0.3342(6) 0.5529(2) 0.6393(2) 0.0397(9) Uani 1 1 d . . . . . H23 H 0.3556 0.5822 0.6026 0.048 Uiso 1 1 calc R U . . . C24 C 0.3188(5) 0.4775(2) 0.64044(19) 0.0327(8) Uani 1 1 d . . . . . C25 C 0.2779(6) 0.2789(2) 0.41735(19) 0.0347(9) Uani 1 1 d . . . . . C26 C 0.4168(6) 0.2720(2) 0.37370(19) 0.0359(9) Uani 1 1 d . . . . . C27 C 0.3954(6) 0.2698(2) 0.30810(19) 0.0388(10) Uani 1 1 d . . . . . C28 C 0.2356(7) 0.2763(2) 0.2865(2) 0.0451(11) Uani 1 1 d . . . . . C29 C 0.0952(7) 0.2853(3) 0.3287(2) 0.0452(11) Uani 1 1 d . . . . . C30 C 0.1184(6) 0.2863(2) 0.3935(2) 0.0407(10) Uani 1 1 d . . . . . C31 C 0.1471(6) 0.0509(2) 0.6870(2) 0.0384(9) Uani 1 1 d . . . . . C32 C 0.2892(7) 0.0030(3) 0.6782(2) 0.0445(10) Uani 1 1 d . . . . . C33 C 0.2846(9) -0.0686(3) 0.6958(3) 0.0589(14) Uani 1 1 d . . . . . C34 C 0.1357(10) -0.0950(3) 0.7239(3) 0.0703(18) Uani 1 1 d . . . . . C35 C -0.0064(9) -0.0496(3) 0.7322(3) 0.0666(16) Uani 1 1 d . . . . . C36 C 0.0003(7) 0.0229(3) 0.7151(2) 0.0512(12) Uani 1 1 d . . . . . C37 C 0.1027(6) 0.2179(2) 0.91198(19) 0.0361(9) Uani 1 1 d . . . . . C38 C 0.2365(6) 0.2065(2) 0.9526(2) 0.0430(10) Uani 1 1 d . . . . . C39 C 0.2279(7) 0.1576(3) 1.0024(2) 0.0512(12) Uani 1 1 d . . . . . C40 C 0.0873(8) 0.1174(3) 1.0130(2) 0.0516(12) Uani 1 1 d . . . . . C41 C -0.0464(7) 0.1266(3) 0.9739(2) 0.0472(11) Uani 1 1 d . . . . . C42 C -0.0361(6) 0.1762(2) 0.9241(2) 0.0406(10) Uani 1 1 d . . . . . C43 C 0.2460(6) 0.5866(2) 0.83837(19) 0.0378(9) Uani 1 1 d . . . . . C44 C 0.3914(6) 0.6228(3) 0.8457(2) 0.0429(10) Uani 1 1 d . . . . . C45 C 0.3869(7) 0.6904(3) 0.8738(2) 0.0469(11) Uani 1 1 d . . . . . C46 C 0.2303(7) 0.7219(3) 0.8944(2) 0.0494(12) Uani 1 1 d . . . . . C47 C 0.0830(7) 0.6870(3) 0.8882(2) 0.0481(11) Uani 1 1 d . . . . . C48 C 0.0928(6) 0.6201(2) 0.8601(2) 0.0405(10) Uani 1 1 d . . . . . C49 C 0.4956(8) 0.2068(3) 0.7111(3) 0.0360(12) Uani 0.7119(12) 1 d . . P A 1 H49A H 0.3872 0.2235 0.7294 0.043 Uiso 0.7119(12) 1 calc R U P A 1 H49B H 0.5214 0.1566 0.7060 0.043 Uiso 0.7119(12) 1 calc R U P A 1 C49A C 0.4773(19) 0.2454(8) 0.7724(7) 0.036(3) Uiso 0.2881(12) 1 d . . P A 2 H49C H 0.3788 0.2364 0.7503 0.043 Uiso 0.2881(12) 1 calc R U P A 2 H49D H 0.4898 0.2257 0.8139 0.043 Uiso 0.2881(12) 1 calc R U P A 2 C50 C 0.6184(7) 0.2565(3) 0.6915(3) 0.0327(12) Uani 0.7119(12) 1 d . . P A 1 H50 H 0.7272 0.2403 0.6732 0.039 Uiso 0.7119(12) 1 calc R U P A 1 C50A C 0.6078(19) 0.2888(8) 0.7431(7) 0.035(3) Uiso 0.2881(12) 1 d . . P A 2 H50A H 0.7085 0.2994 0.7632 0.042 Uiso 0.2881(12) 1 calc R U P A 2 C51A C 0.571(3) 0.3143(10) 0.6814(9) 0.032(5) Uiso 0.2881(12) 1 d . . P A 2 H51A H 0.4793 0.2985 0.6587 0.039 Uiso 0.2881(12) 1 calc R U P A 2 C52 C 0.6823(9) 0.3875(4) 0.6733(4) 0.0329(15) Uani 0.7119(12) 1 d . . P A 1 C52A C 0.695(3) 0.3699(12) 0.6550(11) 0.037(6) Uiso 0.2881(12) 1 d . . P A 2 C53 C 0.7780(10) 0.3814(5) 0.6159(5) 0.0408(19) Uani 0.7119(12) 1 d . . P A 1 H53 H 0.7662 0.3401 0.5908 0.049 Uiso 0.7119(12) 1 calc R U P A 1 C53A C 0.767(3) 0.3675(13) 0.5968(11) 0.042(7) Uiso 0.2881(12) 1 d . . P A 2 H53A H 0.7385 0.3280 0.5721 0.051 Uiso 0.2881(12) 1 calc R U P A 2 C54 C 0.8898(9) 0.4321(5) 0.5930(5) 0.0467(18) Uani 0.7119(12) 1 d . . P A 1 H54 H 0.9531 0.4264 0.5533 0.056 Uiso 0.7119(12) 1 calc R U P A 1 C54A C 0.873(4) 0.4115(17) 0.5678(15) 0.073(9) Uiso 0.2881(12) 1 d . . P A 2 H54A H 0.9172 0.4046 0.5252 0.088 Uiso 0.2881(12) 1 calc R U P A 2 C55 C 0.9056(10) 0.4931(4) 0.6315(7) 0.054(2) Uani 0.7119(12) 1 d . . P A 1 H55 H 0.9825 0.5288 0.6182 0.065 Uiso 0.7119(12) 1 calc R U P A 1 C55A C 0.916(4) 0.472(2) 0.6061(14) 0.059(8) Uiso 0.2881(12) 1 d . . P A 2 H55A H 0.9981 0.5035 0.5884 0.071 Uiso 0.2881(12) 1 calc R U P A 2 C56 C 0.8078(11) 0.5004(4) 0.6890(6) 0.052(2) Uani 0.7119(12) 1 d . . P A 1 H56 H 0.8185 0.5413 0.7146 0.063 Uiso 0.7119(12) 1 calc R U P A 1 C56A C 0.846(4) 0.4848(15) 0.6660(14) 0.053(7) Uiso 0.2881(12) 1 d . . P A 2 H56A H 0.8698 0.5258 0.6895 0.063 Uiso 0.2881(12) 1 calc R U P A 2 C57 C 0.6971(12) 0.4493(4) 0.7088(5) 0.0452(18) Uani 0.7119(12) 1 d . . P A 1 H57 H 0.6290 0.4560 0.7473 0.054 Uiso 0.7119(12) 1 calc R U P A 1 C57A C 0.729(3) 0.4303(15) 0.6911(11) 0.041(6) Uiso 0.2881(12) 1 d . . P A 2 H57A H 0.6754 0.4359 0.7326 0.050 Uiso 0.2881(12) 1 calc R U P A 2 O1 O 0.3122(5) 0.07291(19) 0.83597(17) 0.0542(9) Uani 1 1 d . . . . . C58 C 0.4928(8) 0.0737(4) 0.8381(4) 0.082(2) Uani 1 1 d . . . . . H58A H 0.5250 0.1192 0.8567 0.099 Uiso 1 1 calc R U . . . H58B H 0.5484 0.0693 0.7948 0.099 Uiso 1 1 calc R U . . . C59 C 0.5472(10) 0.0109(5) 0.8786(5) 0.097(3) Uani 1 1 d . . . . . H59A H 0.6607 -0.0103 0.8633 0.117 Uiso 1 1 calc R U . . . H59B H 0.5515 0.0249 0.9236 0.117 Uiso 1 1 calc R U . . . C60 C 0.4111(10) -0.0399(4) 0.8708(4) 0.087(2) Uani 1 1 d . . . . . H60A H 0.4340 -0.0685 0.8316 0.105 Uiso 1 1 calc R U . . . H60B H 0.3997 -0.0731 0.9079 0.105 Uiso 1 1 calc R U . . . C61 C 0.2569(8) 0.0087(3) 0.8666(3) 0.0563(13) Uani 1 1 d . . . . . H61A H 0.1717 -0.0136 0.8415 0.068 Uiso 1 1 calc R U . . . H61B H 0.2042 0.0194 0.9096 0.068 Uiso 1 1 calc R U . . . O2 O 0.7173(6) 0.4178(2) 0.98816(16) 0.0626(10) Uani 1 1 d . . . . . C62 C 0.6981(9) 0.4746(3) 0.9422(3) 0.0651(15) Uani 1 1 d . . . . . H62A H 0.7894 0.5089 0.9448 0.078 Uiso 1 1 calc R U . . . H62B H 0.5857 0.5011 0.9494 0.078 Uiso 1 1 calc R U . . . C63 C 0.7111(8) 0.4384(3) 0.8785(2) 0.0595(14) Uani 1 1 d . . . . . H63A H 0.6403 0.4653 0.8478 0.071 Uiso 1 1 calc R U . . . H63B H 0.8312 0.4341 0.8609 0.071 Uiso 1 1 calc R U . . . C64 C 0.6441(7) 0.3652(3) 0.8933(3) 0.0580(14) Uani 1 1 d . . . . . H64A H 0.5242 0.3634 0.8815 0.070 Uiso 1 1 calc R U . . . H64B H 0.7147 0.3272 0.8701 0.070 Uiso 1 1 calc R U . . . C65 C 0.6557(11) 0.3558(4) 0.9639(3) 0.077(2) Uani 1 1 d . . . . . H65A H 0.5413 0.3473 0.9842 0.093 Uiso 1 1 calc R U . . . H65B H 0.7335 0.3137 0.9730 0.093 Uiso 1 1 calc R U . . . O3 O 0.8289(6) 0.0687(2) 0.47633(19) 0.0626(10) Uani 1 1 d . . . . . C66 C 0.7675(9) 0.1374(3) 0.4593(3) 0.0616(14) Uani 1 1 d . . . . . H66A H 0.6529 0.1358 0.4423 0.074 Uiso 1 1 calc R U . . . H66B H 0.8458 0.1587 0.4263 0.074 Uiso 1 1 calc R U . . . C67 C 0.7583(7) 0.1815(3) 0.5201(2) 0.0494(11) Uani 1 1 d . . . . . H67A H 0.8693 0.2021 0.5269 0.059 Uiso 1 1 calc R U . . . H67B H 0.6681 0.2209 0.5192 0.059 Uiso 1 1 calc R U . . . C68 C 0.7142(8) 0.1250(3) 0.5707(3) 0.0551(12) Uani 1 1 d . . . . . H68A H 0.7848 0.1290 0.6078 0.066 Uiso 1 1 calc R U . . . H68B H 0.5919 0.1305 0.5854 0.066 Uiso 1 1 calc R U . . . C69 C 0.7533(9) 0.0532(3) 0.5380(3) 0.0661(15) Uani 1 1 d . . . . . H69A H 0.8334 0.0224 0.5626 0.079 Uiso 1 1 calc R U . . . H69B H 0.6469 0.0277 0.5346 0.079 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 0.0322(2) 0.0318(2) 0.0234(2) 0.00144(14) -0.00355(15) -0.00205(15) Pd1A 0.0345(6) 0.0345(6) 0.0278(5) -0.0007(4) -0.0031(4) -0.0013(4) F26 0.0441(14) 0.0557(16) 0.0318(13) 0.0021(11) -0.0033(10) -0.0041(12) F27 0.0686(18) 0.0476(15) 0.0272(12) 0.0011(10) 0.0055(12) -0.0038(13) F28 0.091(2) 0.0599(18) 0.0256(13) -0.0055(12) -0.0176(13) 0.0024(16) F29 0.0629(19) 0.079(2) 0.0509(17) -0.0113(15) -0.0283(15) 0.0080(16) F30 0.0447(15) 0.0680(18) 0.0405(14) -0.0067(13) -0.0047(11) 0.0007(13) F32 0.0588(17) 0.0467(16) 0.0585(18) 0.0093(13) 0.0033(14) 0.0074(13) F33 0.111(3) 0.0421(17) 0.068(2) 0.0016(15) -0.0067(19) 0.0197(18) F34 0.170(5) 0.0356(18) 0.108(3) 0.0137(19) 0.009(3) -0.016(2) F35 0.112(3) 0.071(3) 0.125(4) 0.020(2) 0.019(3) -0.044(2) F36 0.0541(17) 0.065(2) 0.068(2) 0.0073(15) 0.0043(15) -0.0168(15) F38 0.0580(17) 0.0539(17) 0.0585(18) 0.0030(13) -0.0227(14) -0.0062(14) F39 0.101(3) 0.062(2) 0.059(2) 0.0062(15) -0.0425(19) 0.0074(18) F40 0.113(3) 0.0528(18) 0.0451(17) 0.0141(14) -0.0098(17) 0.0014(18) F41 0.074(2) 0.0536(17) 0.0503(17) 0.0070(13) 0.0107(15) -0.0118(15) F42 0.0431(14) 0.0570(16) 0.0445(15) 0.0065(12) -0.0040(11) -0.0075(12) F44 0.0485(15) 0.0544(17) 0.0547(17) -0.0193(13) 0.0022(13) -0.0080(13) F45 0.074(2) 0.0637(19) 0.0585(18) -0.0267(15) 0.0101(15) -0.0296(16) F46 0.098(2) 0.0463(17) 0.0557(18) -0.0249(14) 0.0162(17) -0.0118(16) F47 0.070(2) 0.0560(18) 0.0583(18) -0.0171(14) 0.0115(15) 0.0093(15) F48 0.0464(15) 0.0544(16) 0.0520(16) -0.0065(13) 0.0039(12) -0.0025(12) N1 0.0377(18) 0.0319(17) 0.0261(16) 0.0022(13) -0.0050(13) -0.0011(14) N2 0.0447(19) 0.0360(18) 0.0257(16) 0.0007(13) -0.0023(14) -0.0064(15) N3 0.0368(18) 0.0318(17) 0.0280(17) 0.0044(13) -0.0016(13) -0.0052(14) N4 0.0380(19) 0.041(2) 0.0365(19) -0.0038(15) 0.0048(15) -0.0069(15) N5 0.0402(19) 0.0331(18) 0.0309(17) -0.0032(14) 0.0008(14) -0.0057(14) C1 0.0299(19) 0.040(2) 0.0282(19) 0.0014(16) -0.0023(15) -0.0049(16) C2 0.043(2) 0.033(2) 0.033(2) 0.0012(16) -0.0007(17) -0.0085(17) C51 0.035(4) 0.039(4) 0.035(4) -0.008(3) -0.019(3) -0.007(3) C3 0.042(2) 0.039(2) 0.028(2) 0.0032(16) -0.0004(17) -0.0069(18) C4 0.034(2) 0.038(2) 0.0257(19) 0.0046(16) -0.0060(15) -0.0025(16) C5 0.038(2) 0.039(2) 0.028(2) 0.0007(16) -0.0019(16) -0.0028(17) C6 0.047(2) 0.036(2) 0.0262(19) -0.0016(16) -0.0052(17) 0.0000(18) C7 0.060(3) 0.041(2) 0.026(2) -0.0011(17) -0.0032(19) -0.005(2) C8 0.059(3) 0.034(2) 0.035(2) -0.0017(17) -0.010(2) -0.005(2) C9 0.041(2) 0.033(2) 0.034(2) 0.0003(16) -0.0074(17) -0.0043(17) C10 0.037(2) 0.037(2) 0.032(2) 0.0027(16) -0.0082(16) -0.0036(17) C11 0.033(2) 0.039(2) 0.0280(19) 0.0021(16) -0.0048(16) -0.0047(16) C12 0.0302(19) 0.038(2) 0.031(2) 0.0063(16) -0.0034(16) -0.0034(16) C13 0.031(2) 0.035(2) 0.036(2) 0.0023(16) -0.0072(16) -0.0024(16) C14 0.033(2) 0.033(2) 0.035(2) 0.0024(16) -0.0001(16) -0.0037(16) C15 0.036(2) 0.038(2) 0.032(2) 0.0006(16) 0.0000(16) 0.0021(17) C16 0.040(2) 0.038(2) 0.032(2) -0.0022(17) -0.0021(17) 0.0019(17) C17 0.054(3) 0.043(2) 0.026(2) -0.0015(17) -0.0027(18) 0.002(2) C18 0.053(3) 0.039(2) 0.028(2) -0.0057(17) -0.0048(18) 0.0040(19) C19 0.038(2) 0.038(2) 0.032(2) -0.0056(17) -0.0037(17) -0.0041(17) C20 0.038(2) 0.036(2) 0.036(2) -0.0046(17) -0.0023(17) -0.0048(17) C21 0.040(2) 0.033(2) 0.034(2) -0.0030(16) 0.0004(17) -0.0023(17) C22 0.044(2) 0.032(2) 0.033(2) -0.0015(16) -0.0025(17) -0.0024(17) C23 0.047(2) 0.039(2) 0.033(2) 0.0019(17) -0.0061(18) -0.0024(19) C24 0.034(2) 0.036(2) 0.0281(19) -0.0023(16) -0.0008(16) -0.0014(16) C25 0.046(2) 0.032(2) 0.0268(19) -0.0006(15) -0.0036(17) -0.0025(17) C26 0.045(2) 0.035(2) 0.027(2) 0.0025(16) -0.0042(17) -0.0037(18) C27 0.059(3) 0.032(2) 0.0248(19) -0.0010(15) 0.0014(18) -0.0028(19) C28 0.072(3) 0.036(2) 0.028(2) -0.0009(17) -0.011(2) 0.000(2) C29 0.057(3) 0.042(2) 0.037(2) -0.0034(19) -0.016(2) 0.002(2) C30 0.046(2) 0.041(2) 0.035(2) -0.0025(18) -0.0041(19) -0.0020(19) C31 0.055(3) 0.035(2) 0.027(2) 0.0002(16) -0.0088(18) -0.0091(19) C32 0.059(3) 0.039(2) 0.037(2) -0.0002(18) -0.009(2) -0.001(2) C33 0.098(4) 0.034(2) 0.044(3) -0.005(2) -0.009(3) 0.004(3) C34 0.121(6) 0.031(3) 0.061(3) 0.001(2) -0.001(4) -0.018(3) C35 0.095(5) 0.051(3) 0.056(3) 0.006(3) 0.002(3) -0.031(3) C36 0.062(3) 0.049(3) 0.044(3) -0.001(2) -0.007(2) -0.015(2) C37 0.045(2) 0.034(2) 0.028(2) -0.0042(16) -0.0024(17) 0.0022(18) C38 0.053(3) 0.041(2) 0.035(2) -0.0046(18) -0.010(2) 0.002(2) C39 0.074(3) 0.044(3) 0.037(2) -0.002(2) -0.018(2) 0.011(2) C40 0.082(4) 0.042(3) 0.030(2) 0.0035(19) -0.005(2) 0.004(2) C41 0.066(3) 0.038(2) 0.036(2) -0.0017(18) 0.006(2) -0.002(2) C42 0.048(2) 0.042(2) 0.030(2) -0.0015(17) -0.0004(18) 0.0058(19) C43 0.047(2) 0.039(2) 0.027(2) -0.0025(16) 0.0015(17) -0.0052(18) C44 0.050(3) 0.043(2) 0.036(2) -0.0068(18) 0.0036(19) -0.006(2) C45 0.061(3) 0.049(3) 0.032(2) -0.0088(19) 0.003(2) -0.014(2) C46 0.075(3) 0.041(3) 0.031(2) -0.0102(18) 0.008(2) -0.006(2) C47 0.063(3) 0.043(3) 0.037(2) -0.0058(19) 0.006(2) 0.004(2) C48 0.048(2) 0.041(2) 0.032(2) -0.0024(17) 0.0013(18) -0.0041(19) C49 0.038(3) 0.035(3) 0.035(3) 0.010(2) -0.012(2) 0.004(2) C50 0.029(3) 0.042(3) 0.028(3) 0.006(2) -0.010(2) 0.002(2) C52 0.036(4) 0.026(4) 0.037(4) -0.001(3) -0.014(3) 0.002(3) C53 0.038(4) 0.036(4) 0.050(5) 0.004(4) -0.017(4) -0.003(3) C54 0.030(3) 0.036(4) 0.074(6) 0.015(4) -0.010(3) 0.002(3) C55 0.034(4) 0.037(4) 0.092(8) 0.010(5) -0.011(5) -0.006(3) C56 0.041(4) 0.035(4) 0.083(7) -0.001(4) -0.026(5) -0.002(3) C57 0.046(4) 0.036(4) 0.055(5) -0.006(4) -0.018(4) 0.005(3) O1 0.059(2) 0.0479(19) 0.055(2) 0.0173(16) -0.0121(17) 0.0029(16) C58 0.057(4) 0.088(5) 0.100(5) 0.040(4) -0.009(3) 0.000(3) C59 0.079(5) 0.098(6) 0.117(7) 0.045(5) -0.035(5) 0.001(4) C60 0.094(5) 0.069(4) 0.096(5) 0.023(4) -0.009(4) 0.016(4) C61 0.069(3) 0.045(3) 0.054(3) 0.005(2) -0.001(3) 0.000(2) O2 0.087(3) 0.072(3) 0.0321(17) -0.0043(16) -0.0075(17) -0.023(2) C62 0.091(4) 0.063(4) 0.040(3) -0.001(2) 0.006(3) -0.005(3) C63 0.069(3) 0.077(4) 0.032(2) -0.003(2) -0.009(2) 0.012(3) C64 0.051(3) 0.078(4) 0.046(3) -0.020(3) -0.009(2) 0.002(3) C65 0.117(6) 0.069(4) 0.051(3) 0.002(3) -0.031(4) -0.021(4) O3 0.084(3) 0.047(2) 0.056(2) -0.0118(17) 0.0054(19) -0.0067(19) C66 0.089(4) 0.051(3) 0.046(3) -0.010(2) -0.012(3) 0.000(3) C67 0.062(3) 0.045(3) 0.041(3) -0.009(2) -0.006(2) -0.001(2) C68 0.061(3) 0.058(3) 0.047(3) -0.003(2) -0.004(2) -0.002(2) C69 0.087(4) 0.051(3) 0.061(3) -0.003(3) -0.002(3) -0.012(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _citation_id _citation_doi _citation_year 1 10.1002/chem.202002682 2020 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 8 8 0.0121 1 -12 3 0.0090 -3 -6 -10 0.0201 0 12 1 0.0097 5 2 -1 0.0210 0 3 13 0.0115 0 -3 -13 0.0115 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 85.71(13) . . ? N1 Pd1 C51 103.6(2) . . ? N1 Pd1 C49 171.86(19) . . ? N1 Pd1 C50 134.43(19) . . ? N2 Pd1 C51 168.7(2) . . ? N2 Pd1 C49 102.42(19) . . ? C49 Pd1 C51 68.2(2) . . ? C50 Pd1 N2 130.36(19) . . ? C50 Pd1 C51 38.3(3) . . ? C50 Pd1 C49 38.7(2) . . ? N4 Pd1A N5 81.84(14) . . ? N4 Pd1A C49A 107.2(4) . . ? N4 Pd1A C50A 132.3(4) . . ? C49A Pd1A N5 170.9(4) . . ? C50A Pd1A N5 133.7(4) . . ? C50A Pd1A C49A 39.3(5) . . ? C51A Pd1A N4 170.6(6) . . ? C51A Pd1A N5 102.5(5) . . ? C51A Pd1A C49A 68.5(7) . . ? C51A Pd1A C50A 39.4(7) . . ? C1 N1 Pd1 130.2(3) . . ? C1 N1 H1 126.1 . . ? C1 N1 C4 107.8(3) . . ? C4 N1 Pd1 118.7(3) . . ? C4 N1 H1 126.1 . . ? C6 N2 Pd1 121.3(3) . . ? C9 N2 Pd1 126.2(3) . . ? C9 N2 C6 107.0(3) . . ? C11 N3 H3 125.3 . . ? C11 N3 C14 109.3(3) . . ? C14 N3 H3 125.3 . . ? C16 N4 Pd1A 121.4(3) . . ? C16 N4 C19 106.8(4) . . ? C19 N4 Pd1A 120.5(3) . . ? C21 N5 Pd1A 116.5(3) . . ? C21 N5 H5 125.3 . . ? C24 N5 Pd1A 126.6(3) . . ? C24 N5 H5 125.3 . . ? C24 N5 C21 109.3(3) . . ? N1 C1 C2 110.3(4) . . ? N1 C1 C24 128.9(4) . . ? C2 C1 C24 120.8(4) . . ? C1 C2 H2 126.5 . . ? C3 C2 C1 106.9(4) . . ? C3 C2 H2 126.5 . . ? Pd1 C51 H51 81.9 . . ? C50 C51 Pd1 67.9(4) . . ? C50 C51 H51 118.3 . . ? C50 C51 C52 123.5(7) . . ? C52 C51 Pd1 120.7(5) . . ? C52 C51 H51 118.3 . . ? C2 C3 H3A 126.4 . . ? C2 C3 C4 107.2(4) . . ? C4 C3 H3A 126.4 . . ? N1 C4 C3 107.9(3) . . ? N1 C4 C5 126.7(4) . . ? C5 C4 C3 125.2(4) . . ? C4 C5 C25 116.0(4) . . ? C6 C5 C4 126.9(4) . . ? C6 C5 C25 116.5(4) . . ? N2 C6 C5 121.7(4) . . ? N2 C6 C7 108.7(4) . . ? C5 C6 C7 129.4(4) . . ? C6 C7 H7 125.9 . . ? C8 C7 C6 108.2(4) . . ? C8 C7 H7 125.9 . . ? C7 C8 H8 126.9 . . ? C7 C8 C9 106.2(4) . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 109.7(4) . . ? N2 C9 C10 122.3(4) . . ? C10 C9 C8 127.5(4) . . ? C9 C10 C31 119.9(4) . . ? C11 C10 C9 118.3(4) . . ? C11 C10 C31 121.8(4) . . ? N3 C11 C10 125.9(4) . . ? N3 C11 C12 106.7(3) . . ? C10 C11 C12 127.2(4) . . ? C11 C12 H12 125.7 . . ? C13 C12 C11 108.6(4) . . ? C13 C12 H12 125.7 . . ? C12 C13 H13 125.8 . . ? C12 C13 C14 108.3(4) . . ? C14 C13 H13 125.8 . . ? N3 C14 C13 106.5(4) . . ? N3 C14 C15 125.5(4) . . ? C15 C14 C13 127.7(4) . . ? C14 C15 C16 119.0(4) . . ? C14 C15 C37 119.8(4) . . ? C16 C15 C37 121.2(4) . . ? N4 C16 C15 121.6(4) . . ? N4 C16 C17 110.2(4) . . ? C15 C16 C17 128.1(4) . . ? C16 C17 H17 126.8 . . ? C18 C17 C16 106.4(4) . . ? C18 C17 H17 126.8 . . ? C17 C18 H18 126.6 . . ? C17 C18 C19 106.9(4) . . ? C19 C18 H18 126.6 . . ? N4 C19 C18 109.7(4) . . ? N4 C19 C20 123.1(4) . . ? C20 C19 C18 127.1(4) . . ? C19 C20 C21 125.3(4) . . ? C19 C20 C43 119.0(4) . . ? C21 C20 C43 115.6(4) . . ? N5 C21 C20 126.0(4) . . ? N5 C21 C22 107.4(4) . . ? C20 C21 C22 126.6(4) . . ? C21 C22 H22 126.1 . . ? C23 C22 C21 107.7(4) . . ? C23 C22 H22 126.1 . . ? C22 C23 H23 126.4 . . ? C22 C23 C24 107.3(4) . . ? C24 C23 H23 126.4 . . ? N5 C24 C1 128.4(4) . . ? N5 C24 C23 108.3(4) . . ? C23 C24 C1 123.2(4) . . ? C26 C25 C5 123.0(4) . . ? C30 C25 C5 120.0(4) . . ? C30 C25 C26 117.0(4) . . ? F26 C26 C25 120.7(4) . . ? F26 C26 C27 117.9(4) . . ? C25 C26 C27 121.4(4) . . ? F27 C27 C26 119.6(4) . . ? F27 C27 C28 120.7(4) . . ? C28 C27 C26 119.7(4) . . ? F28 C28 C27 120.4(4) . . ? F28 C28 C29 119.3(4) . . ? C27 C28 C29 120.2(4) . . ? F29 C29 C28 120.6(4) . . ? F29 C29 C30 120.0(4) . . ? C28 C29 C30 119.3(4) . . ? F30 C30 C25 120.1(4) . . ? F30 C30 C29 117.6(4) . . ? C25 C30 C29 122.3(4) . . ? C32 C31 C10 122.0(4) . . ? C36 C31 C10 121.6(4) . . ? C36 C31 C32 116.4(4) . . ? F32 C32 C31 120.5(4) . . ? F32 C32 C33 117.4(5) . . ? C33 C32 C31 122.1(5) . . ? F33 C33 C32 120.0(6) . . ? F33 C33 C34 119.8(5) . . ? C32 C33 C34 120.1(6) . . ? F34 C34 C33 120.6(6) . . ? F34 C34 C35 120.3(6) . . ? C35 C34 C33 119.1(5) . . ? F35 C35 C34 120.5(5) . . ? F35 C35 C36 119.2(6) . . ? C34 C35 C36 120.3(6) . . ? F36 C36 C31 119.9(4) . . ? F36 C36 C35 118.1(5) . . ? C31 C36 C35 121.9(5) . . ? C38 C37 C15 121.8(4) . . ? C42 C37 C15 122.3(4) . . ? C42 C37 C38 115.9(4) . . ? F38 C38 C37 120.1(4) . . ? F38 C38 C39 118.1(4) . . ? C39 C38 C37 121.8(5) . . ? F39 C39 C38 119.8(5) . . ? F39 C39 C40 119.7(5) . . ? C40 C39 C38 120.5(5) . . ? F40 C40 C39 120.8(5) . . ? F40 C40 C41 119.6(5) . . ? C39 C40 C41 119.5(4) . . ? F41 C41 C40 120.4(4) . . ? F41 C41 C42 120.3(5) . . ? C40 C41 C42 119.3(5) . . ? F42 C42 C37 120.0(4) . . ? F42 C42 C41 117.1(4) . . ? C37 C42 C41 123.0(4) . . ? C44 C43 C20 122.5(4) . . ? C44 C43 C48 116.9(4) . . ? C48 C43 C20 120.5(4) . . ? F44 C44 C43 120.4(4) . . ? F44 C44 C45 117.2(4) . . ? C43 C44 C45 122.4(4) . . ? F45 C45 C44 121.1(5) . . ? F45 C45 C46 120.4(4) . . ? C46 C45 C44 118.5(5) . . ? F46 C46 C45 118.9(5) . . ? F46 C46 C47 120.5(5) . . ? C47 C46 C45 120.7(4) . . ? F47 C47 C46 119.9(4) . . ? F47 C47 C48 120.9(5) . . ? C46 C47 C48 119.2(5) . . ? F48 C48 C43 120.3(4) . . ? F48 C48 C47 117.3(4) . . ? C43 C48 C47 122.4(4) . . ? Pd1 C49 H49A 75.9 . . ? Pd1 C49 H49B 126.4 . . ? H49A C49 H49B 120.0 . . ? C50 C49 Pd1 69.5(3) . . ? C50 C49 H49A 120.0 . . ? C50 C49 H49B 120.0 . . ? Pd1A C49A H49C 74.5 . . ? Pd1A C49A H49D 129.2 . . ? H49C C49A H49D 120.0 . . ? C50A C49A Pd1A 68.6(8) . . ? C50A C49A H49C 120.0 . . ? C50A C49A H49D 120.0 . . ? Pd1 C50 H50 125.5 . . ? C51 C50 Pd1 73.8(4) . . ? C51 C50 H50 120.7 . . ? C49 C50 Pd1 71.7(3) . . ? C49 C50 C51 118.6(6) . . ? C49 C50 H50 120.7 . . ? Pd1A C50A H50A 127.8 . . ? C49A C50A Pd1A 72.0(8) . . ? C49A C50A H50A 123.3 . . ? C51A C50A Pd1A 68.6(10) . . ? C51A C50A C49A 113.4(14) . . ? C51A C50A H50A 123.3 . . ? Pd1A C51A H51A 82.2 . . ? C50A C51A Pd1A 72.0(10) . . ? C50A C51A H51A 123.5 . . ? C50A C51A C52A 112.9(18) . . ? C52A C51A Pd1A 117.4(14) . . ? C52A C51A H51A 123.5 . . ? C53 C52 C51 123.3(8) . . ? C53 C52 C57 117.6(8) . . ? C57 C52 C51 119.1(8) . . ? C53A C52A C51A 123(2) . . ? C53A C52A C57A 116(2) . . ? C57A C52A C51A 121(2) . . ? C52 C53 H53 118.2 . . ? C54 C53 C52 123.6(10) . . ? C54 C53 H53 118.2 . . ? C52A C53A H53A 115.2 . . ? C54A C53A C52A 130(3) . . ? C54A C53A H53A 115.2 . . ? C53 C54 H54 121.5 . . ? C53 C54 C55 117.1(9) . . ? C55 C54 H54 121.5 . . ? C53A C54A H54A 122.6 . . ? C53A C54A C55A 115(3) . . ? C55A C54A H54A 122.6 . . ? C54 C55 H55 120.1 . . ? C56 C55 C54 119.8(8) . . ? C56 C55 H55 120.1 . . ? C54A C55A H55A 118.4 . . ? C56A C55A C54A 123(3) . . ? C56A C55A H55A 118.4 . . ? C55 C56 H56 119.7 . . ? C57 C56 C55 120.7(9) . . ? C57 C56 H56 119.7 . . ? C55A C56A H56A 122.6 . . ? C55A C56A C57A 115(3) . . ? C57A C56A H56A 122.6 . . ? C52 C57 H57 119.4 . . ? C56 C57 C52 121.1(10) . . ? C56 C57 H57 119.4 . . ? C52A C57A C56A 121(2) . . ? C52A C57A H57A 119.3 . . ? C56A C57A H57A 119.3 . . ? C58 O1 C61 108.5(4) . . ? O1 C58 H58A 110.4 . . ? O1 C58 H58B 110.4 . . ? O1 C58 C59 106.7(5) . . ? H58A C58 H58B 108.6 . . ? C59 C58 H58A 110.4 . . ? C59 C58 H58B 110.4 . . ? C58 C59 H59A 111.2 . . ? C58 C59 H59B 111.2 . . ? H59A C59 H59B 109.2 . . ? C60 C59 C58 102.6(6) . . ? C60 C59 H59A 111.2 . . ? C60 C59 H59B 111.2 . . ? C59 C60 H60A 111.2 . . ? C59 C60 H60B 111.2 . . ? H60A C60 H60B 109.2 . . ? C61 C60 C59 102.6(6) . . ? C61 C60 H60A 111.2 . . ? C61 C60 H60B 111.2 . . ? O1 C61 C60 106.3(5) . . ? O1 C61 H61A 110.5 . . ? O1 C61 H61B 110.5 . . ? C60 C61 H61A 110.5 . . ? C60 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? C65 O2 C62 108.4(4) . . ? O2 C62 H62A 110.6 . . ? O2 C62 H62B 110.6 . . ? O2 C62 C63 105.6(5) . . ? H62A C62 H62B 108.8 . . ? C63 C62 H62A 110.6 . . ? C63 C62 H62B 110.6 . . ? C62 C63 H63A 111.1 . . ? C62 C63 H63B 111.1 . . ? H63A C63 H63B 109.1 . . ? C64 C63 C62 103.4(5) . . ? C64 C63 H63A 111.1 . . ? C64 C63 H63B 111.1 . . ? C63 C64 H64A 110.8 . . ? C63 C64 H64B 110.8 . . ? H64A C64 H64B 108.9 . . ? C65 C64 C63 104.7(4) . . ? C65 C64 H64A 110.8 . . ? C65 C64 H64B 110.8 . . ? O2 C65 C64 108.9(5) . . ? O2 C65 H65A 109.9 . . ? O2 C65 H65B 109.9 . . ? C64 C65 H65A 109.9 . . ? C64 C65 H65B 109.9 . . ? H65A C65 H65B 108.3 . . ? C66 O3 C69 107.1(4) . . ? O3 C66 H66A 110.6 . . ? O3 C66 H66B 110.6 . . ? O3 C66 C67 105.8(4) . . ? H66A C66 H66B 108.7 . . ? C67 C66 H66A 110.6 . . ? C67 C66 H66B 110.6 . . ? C66 C67 H67A 111.4 . . ? C66 C67 H67B 111.4 . . ? H67A C67 H67B 109.3 . . ? C68 C67 C66 101.9(4) . . ? C68 C67 H67A 111.4 . . ? C68 C67 H67B 111.4 . . ? C67 C68 H68A 110.8 . . ? C67 C68 H68B 110.8 . . ? H68A C68 H68B 108.9 . . ? C69 C68 C67 104.9(4) . . ? C69 C68 H68A 110.8 . . ? C69 C68 H68B 110.8 . . ? O3 C69 C68 106.8(5) . . ? O3 C69 H69A 110.4 . . ? O3 C69 H69B 110.4 . . ? C68 C69 H69A 110.4 . . ? C68 C69 H69B 110.4 . . ? H69A C69 H69B 108.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.108(3) . ? Pd1 N2 2.114(3) . ? Pd1 C51 2.188(7) . ? Pd1 C49 2.140(5) . ? Pd1 C50 2.111(5) . ? Pd1A N4 2.106(4) . ? Pd1A N5 2.226(4) . ? Pd1A C49A 2.167(15) . ? Pd1A C50A 2.122(15) . ? Pd1A C51A 2.078(18) . ? F26 C26 1.336(5) . ? F27 C27 1.338(5) . ? F28 C28 1.332(5) . ? F29 C29 1.337(6) . ? F30 C30 1.346(5) . ? F32 C32 1.329(6) . ? F33 C33 1.349(7) . ? F34 C34 1.327(6) . ? F35 C35 1.341(7) . ? F36 C36 1.345(6) . ? F38 C38 1.332(6) . ? F39 C39 1.350(6) . ? F40 C40 1.335(6) . ? F41 C41 1.336(6) . ? F42 C42 1.343(5) . ? F44 C44 1.343(5) . ? F45 C45 1.326(6) . ? F46 C46 1.342(5) . ? F47 C47 1.334(6) . ? F48 C48 1.342(5) . ? N1 H1 0.8800 . ? N1 C1 1.338(5) . ? N1 C4 1.385(5) . ? N2 C6 1.373(5) . ? N2 C9 1.360(5) . ? N3 H3 0.8800 . ? N3 C11 1.381(5) . ? N3 C14 1.385(5) . ? N4 C16 1.360(6) . ? N4 C19 1.363(5) . ? N5 H5 0.8800 . ? N5 C21 1.372(5) . ? N5 C24 1.353(5) . ? C1 C2 1.417(6) . ? C1 C24 1.448(6) . ? C2 H2 0.9500 . ? C2 C3 1.364(6) . ? C51 H51 0.9500 . ? C51 C50 1.413(10) . ? C51 C52 1.462(10) . ? C3 H3A 0.9500 . ? C3 C4 1.434(6) . ? C4 C5 1.402(6) . ? C5 C6 1.396(6) . ? C5 C25 1.504(6) . ? C6 C7 1.422(6) . ? C7 H7 0.9500 . ? C7 C8 1.351(6) . ? C8 H8 0.9500 . ? C8 C9 1.433(6) . ? C9 C10 1.422(6) . ? C10 C11 1.397(6) . ? C10 C31 1.480(6) . ? C11 C12 1.426(6) . ? C12 H12 0.9500 . ? C12 C13 1.353(6) . ? C13 H13 0.9500 . ? C13 C14 1.429(6) . ? C14 C15 1.395(6) . ? C15 C16 1.418(6) . ? C15 C37 1.485(6) . ? C16 C17 1.445(6) . ? C17 H17 0.9500 . ? C17 C18 1.356(7) . ? C18 H18 0.9500 . ? C18 C19 1.448(6) . ? C19 C20 1.392(6) . ? C20 C21 1.415(6) . ? C20 C43 1.501(6) . ? C21 C22 1.418(6) . ? C22 H22 0.9500 . ? C22 C23 1.371(6) . ? C23 H23 0.9500 . ? C23 C24 1.415(6) . ? C25 C26 1.383(6) . ? C25 C30 1.376(6) . ? C26 C27 1.404(6) . ? C27 C28 1.357(7) . ? C28 C29 1.376(7) . ? C29 C30 1.388(6) . ? C31 C32 1.391(7) . ? C31 C36 1.386(7) . ? C32 C33 1.378(7) . ? C33 C34 1.387(9) . ? C34 C35 1.364(10) . ? C35 C36 1.393(8) . ? C37 C38 1.400(6) . ? C37 C42 1.380(7) . ? C38 C39 1.378(7) . ? C39 C40 1.371(8) . ? C40 C41 1.375(8) . ? C41 C42 1.388(6) . ? C43 C44 1.375(7) . ? C43 C48 1.378(6) . ? C44 C45 1.393(6) . ? C45 C46 1.379(7) . ? C46 C47 1.370(8) . ? C47 C48 1.382(6) . ? C49 H49A 0.9500 . ? C49 H49B 0.9500 . ? C49 C50 1.410(8) . ? C49A H49C 0.9500 . ? C49A H49D 0.9500 . ? C49A C50A 1.44(2) . ? C50 H50 0.9500 . ? C50A H50A 0.9500 . ? C50A C51A 1.42(2) . ? C51A H51A 0.9500 . ? C51A C52A 1.53(3) . ? C52 C53 1.388(14) . ? C52 C57 1.394(12) . ? C52A C53A 1.32(3) . ? C52A C57A 1.41(3) . ? C53 H53 0.9500 . ? C53 C54 1.384(12) . ? C53A H53A 0.9500 . ? C53A C54A 1.31(4) . ? C54 H54 0.9500 . ? C54 C55 1.419(15) . ? C54A H54A 0.9500 . ? C54A C55A 1.46(4) . ? C55 H55 0.9500 . ? C55 C56 1.397(17) . ? C55A H55A 0.9500 . ? C55A C56A 1.37(4) . ? C56 H56 0.9500 . ? C56 C57 1.366(12) . ? C56A H56A 0.9500 . ? C56A C57A 1.47(4) . ? C57 H57 0.9500 . ? C57A H57A 0.9500 . ? O1 C58 1.421(7) . ? O1 C61 1.424(6) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C58 C59 1.493(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C59 C60 1.483(11) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C60 C61 1.475(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? O2 C62 1.429(7) . ? O2 C65 1.391(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C62 C63 1.507(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 C64 1.506(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 C65 1.502(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O3 C66 1.390(7) . ? O3 C69 1.427(7) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C66 C67 1.527(7) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C67 C68 1.524(7) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C68 C69 1.518(8) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 N1 C1 C2 157.5(3) . . . . ? Pd1 N1 C1 C24 -25.9(6) . . . . ? Pd1 N1 C4 C3 -160.7(3) . . . . ? Pd1 N1 C4 C5 23.7(5) . . . . ? Pd1 N2 C6 C5 -33.3(6) . . . . ? Pd1 N2 C6 C7 151.9(3) . . . . ? Pd1 N2 C9 C8 -149.3(3) . . . . ? Pd1 N2 C9 C10 38.3(6) . . . . ? Pd1 C51 C50 C49 -58.0(5) . . . . ? Pd1 C51 C52 C53 -48.9(9) . . . . ? Pd1 C51 C52 C57 134.9(7) . . . . ? Pd1 C49 C50 C51 59.0(5) . . . . ? Pd1A N4 C16 C15 -42.9(5) . . . . ? Pd1A N4 C16 C17 141.1(3) . . . . ? Pd1A N4 C19 C18 -142.7(3) . . . . ? Pd1A N4 C19 C20 39.4(6) . . . . ? Pd1A N5 C21 C20 -30.4(6) . . . . ? Pd1A N5 C21 C22 152.0(3) . . . . ? Pd1A N5 C24 C1 36.0(6) . . . . ? Pd1A N5 C24 C23 -148.3(3) . . . . ? Pd1A C49A C50A C51A -56.1(12) . . . . ? Pd1A C50A C51A C52A 112.8(15) . . . . ? Pd1A C51A C52A C53A -145(2) . . . . ? Pd1A C51A C52A C57A 30(3) . . . . ? F26 C26 C27 F27 0.5(6) . . . . ? F26 C26 C27 C28 -178.7(4) . . . . ? F27 C27 C28 F28 0.5(7) . . . . ? F27 C27 C28 C29 -179.0(4) . . . . ? F28 C28 C29 F29 -0.4(7) . . . . ? F28 C28 C29 C30 179.5(4) . . . . ? F29 C29 C30 F30 -1.0(7) . . . . ? F29 C29 C30 C25 -180.0(4) . . . . ? F32 C32 C33 F33 0.5(7) . . . . ? F32 C32 C33 C34 177.9(5) . . . . ? F33 C33 C34 F34 -1.1(9) . . . . ? F33 C33 C34 C35 179.1(5) . . . . ? F34 C34 C35 F35 -0.6(10) . . . . ? F34 C34 C35 C36 177.7(6) . . . . ? F35 C35 C36 F36 -1.9(8) . . . . ? F35 C35 C36 C31 -179.0(5) . . . . ? F38 C38 C39 F39 1.5(7) . . . . ? F38 C38 C39 C40 -177.2(4) . . . . ? F39 C39 C40 F40 2.5(7) . . . . ? F39 C39 C40 C41 -179.2(5) . . . . ? F40 C40 C41 F41 -0.9(7) . . . . ? F40 C40 C41 C42 178.6(4) . . . . ? F41 C41 C42 F42 -0.1(6) . . . . ? F41 C41 C42 C37 178.9(4) . . . . ? F44 C44 C45 F45 -1.3(7) . . . . ? F44 C44 C45 C46 178.8(4) . . . . ? F45 C45 C46 F46 0.8(7) . . . . ? F45 C45 C46 C47 -178.8(5) . . . . ? F46 C46 C47 F47 -0.2(7) . . . . ? F46 C46 C47 C48 179.3(4) . . . . ? F47 C47 C48 F48 0.6(7) . . . . ? F47 C47 C48 C43 -179.9(4) . . . . ? N1 C1 C2 C3 0.9(5) . . . . ? N1 C1 C24 N5 -8.9(7) . . . . ? N1 C1 C24 C23 175.9(4) . . . . ? N1 C4 C5 C6 4.3(7) . . . . ? N1 C4 C5 C25 175.2(4) . . . . ? N2 C6 C7 C8 0.9(6) . . . . ? N2 C9 C10 C11 18.2(6) . . . . ? N2 C9 C10 C31 -162.5(4) . . . . ? N3 C11 C12 C13 3.7(5) . . . . ? N3 C14 C15 C16 151.5(4) . . . . ? N3 C14 C15 C37 -28.3(6) . . . . ? N4 C16 C17 C18 2.6(5) . . . . ? N4 C19 C20 C21 -1.5(7) . . . . ? N4 C19 C20 C43 174.7(4) . . . . ? N5 C21 C22 C23 -0.2(5) . . . . ? C1 N1 C4 C3 0.8(4) . . . . ? C1 N1 C4 C5 -174.8(4) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C1 C24 N5 167.3(4) . . . . ? C2 C1 C24 C23 -7.8(6) . . . . ? C2 C3 C4 N1 -0.2(5) . . . . ? C2 C3 C4 C5 175.5(4) . . . . ? C51 C52 C53 C54 -174.4(7) . . . . ? C51 C52 C57 C56 173.4(7) . . . . ? C3 C4 C5 C6 -170.5(4) . . . . ? C3 C4 C5 C25 0.3(6) . . . . ? C4 N1 C1 C2 -1.1(5) . . . . ? C4 N1 C1 C24 175.6(4) . . . . ? C4 C5 C6 N2 0.5(7) . . . . ? C4 C5 C6 C7 174.1(5) . . . . ? C4 C5 C25 C26 88.6(5) . . . . ? C4 C5 C25 C30 -90.1(5) . . . . ? C5 C6 C7 C8 -173.3(5) . . . . ? C5 C25 C26 F26 -0.9(6) . . . . ? C5 C25 C26 C27 178.7(4) . . . . ? C5 C25 C30 F30 1.5(6) . . . . ? C5 C25 C30 C29 -179.5(4) . . . . ? C6 N2 C9 C8 4.3(5) . . . . ? C6 N2 C9 C10 -168.1(4) . . . . ? C6 C5 C25 C26 -99.5(5) . . . . ? C6 C5 C25 C30 81.7(5) . . . . ? C6 C7 C8 C9 1.7(6) . . . . ? C7 C8 C9 N2 -3.8(5) . . . . ? C7 C8 C9 C10 168.1(4) . . . . ? C8 C9 C10 C11 -152.7(4) . . . . ? C8 C9 C10 C31 26.6(7) . . . . ? C9 N2 C6 C5 171.5(4) . . . . ? C9 N2 C6 C7 -3.2(5) . . . . ? C9 C10 C11 N3 -152.5(4) . . . . ? C9 C10 C11 C12 21.6(6) . . . . ? C9 C10 C31 C32 52.8(6) . . . . ? C9 C10 C31 C36 -126.7(5) . . . . ? C10 C11 C12 C13 -171.3(4) . . . . ? C10 C31 C32 F32 2.7(6) . . . . ? C10 C31 C32 C33 -178.7(4) . . . . ? C10 C31 C36 F36 0.7(7) . . . . ? C10 C31 C36 C35 177.8(5) . . . . ? C11 N3 C14 C13 8.2(4) . . . . ? C11 N3 C14 C15 -165.9(4) . . . . ? C11 C10 C31 C32 -127.9(5) . . . . ? C11 C10 C31 C36 52.6(6) . . . . ? C11 C12 C13 C14 1.3(5) . . . . ? C12 C13 C14 N3 -5.8(5) . . . . ? C12 C13 C14 C15 168.1(4) . . . . ? C13 C14 C15 C16 -21.3(7) . . . . ? C13 C14 C15 C37 159.0(4) . . . . ? C14 N3 C11 C10 167.7(4) . . . . ? C14 N3 C11 C12 -7.4(4) . . . . ? C14 C15 C16 N4 -15.5(6) . . . . ? C14 C15 C16 C17 159.8(4) . . . . ? C14 C15 C37 C38 128.4(5) . . . . ? C14 C15 C37 C42 -50.9(6) . . . . ? C15 C16 C17 C18 -173.0(4) . . . . ? C15 C37 C38 F38 -2.3(6) . . . . ? C15 C37 C38 C39 179.5(4) . . . . ? C15 C37 C42 F42 -0.6(6) . . . . ? C15 C37 C42 C41 -179.7(4) . . . . ? C16 N4 C19 C18 1.4(5) . . . . ? C16 N4 C19 C20 -176.6(4) . . . . ? C16 C15 C37 C38 -51.3(6) . . . . ? C16 C15 C37 C42 129.4(5) . . . . ? C16 C17 C18 C19 -1.7(5) . . . . ? C17 C18 C19 N4 0.3(5) . . . . ? C17 C18 C19 C20 178.1(4) . . . . ? C18 C19 C20 C21 -179.1(4) . . . . ? C18 C19 C20 C43 -2.8(7) . . . . ? C19 N4 C16 C15 173.6(4) . . . . ? C19 N4 C16 C17 -2.4(5) . . . . ? C19 C20 C21 N5 -1.4(7) . . . . ? C19 C20 C21 C22 175.8(4) . . . . ? C19 C20 C43 C44 110.8(5) . . . . ? C19 C20 C43 C48 -70.4(6) . . . . ? C20 C21 C22 C23 -177.8(4) . . . . ? C20 C43 C44 F44 -0.3(7) . . . . ? C20 C43 C44 C45 179.0(4) . . . . ? C20 C43 C48 F48 0.4(6) . . . . ? C20 C43 C48 C47 -179.1(4) . . . . ? C21 N5 C24 C1 -175.7(4) . . . . ? C21 N5 C24 C23 0.0(5) . . . . ? C21 C20 C43 C44 -72.6(6) . . . . ? C21 C20 C43 C48 106.2(5) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 N5 -0.1(5) . . . . ? C22 C23 C24 C1 175.9(4) . . . . ? C24 N5 C21 C20 177.7(4) . . . . ? C24 N5 C21 C22 0.1(5) . . . . ? C24 C1 C2 C3 -176.0(4) . . . . ? C25 C5 C6 N2 -170.3(4) . . . . ? C25 C5 C6 C7 3.3(7) . . . . ? C25 C26 C27 F27 -179.1(4) . . . . ? C25 C26 C27 C28 1.7(7) . . . . ? C26 C25 C30 F30 -177.3(4) . . . . ? C26 C25 C30 C29 1.6(7) . . . . ? C26 C27 C28 F28 179.6(4) . . . . ? C26 C27 C28 C29 0.2(7) . . . . ? C27 C28 C29 F29 179.1(4) . . . . ? C27 C28 C29 C30 -1.1(7) . . . . ? C28 C29 C30 F30 179.1(4) . . . . ? C28 C29 C30 C25 0.2(7) . . . . ? C30 C25 C26 F26 177.9(4) . . . . ? C30 C25 C26 C27 -2.5(6) . . . . ? C31 C10 C11 N3 28.1(6) . . . . ? C31 C10 C11 C12 -157.8(4) . . . . ? C31 C32 C33 F33 -178.2(4) . . . . ? C31 C32 C33 C34 -0.8(8) . . . . ? C32 C31 C36 F36 -178.8(4) . . . . ? C32 C31 C36 C35 -1.7(7) . . . . ? C32 C33 C34 F34 -178.6(5) . . . . ? C32 C33 C34 C35 1.7(9) . . . . ? C33 C34 C35 F35 179.1(6) . . . . ? C33 C34 C35 C36 -2.6(9) . . . . ? C34 C35 C36 F36 179.8(5) . . . . ? C34 C35 C36 C31 2.7(9) . . . . ? C36 C31 C32 F32 -177.9(4) . . . . ? C36 C31 C32 C33 0.8(7) . . . . ? C37 C15 C16 N4 164.3(4) . . . . ? C37 C15 C16 C17 -20.5(7) . . . . ? C37 C38 C39 F39 179.7(4) . . . . ? C37 C38 C39 C40 1.0(7) . . . . ? C38 C37 C42 F42 -180.0(4) . . . . ? C38 C37 C42 C41 1.0(6) . . . . ? C38 C39 C40 F40 -178.8(4) . . . . ? C38 C39 C40 C41 -0.5(7) . . . . ? C39 C40 C41 F41 -179.2(4) . . . . ? C39 C40 C41 C42 0.3(7) . . . . ? C40 C41 C42 F42 -179.6(4) . . . . ? C40 C41 C42 C37 -0.6(7) . . . . ? C42 C37 C38 F38 177.0(4) . . . . ? C42 C37 C38 C39 -1.2(6) . . . . ? C43 C20 C21 N5 -177.8(4) . . . . ? C43 C20 C21 C22 -0.6(7) . . . . ? C43 C44 C45 F45 179.4(4) . . . . ? C43 C44 C45 C46 -0.5(7) . . . . ? C44 C43 C48 F48 179.3(4) . . . . ? C44 C43 C48 C47 -0.2(7) . . . . ? C44 C45 C46 F46 -179.4(4) . . . . ? C44 C45 C46 C47 1.0(7) . . . . ? C45 C46 C47 F47 179.4(4) . . . . ? C45 C46 C47 C48 -1.1(8) . . . . ? C46 C47 C48 F48 -178.8(4) . . . . ? C46 C47 C48 C43 0.7(7) . . . . ? C48 C43 C44 F44 -179.2(4) . . . . ? C48 C43 C44 C45 0.1(7) . . . . ? C49A C50A C51A Pd1A 58.0(12) . . . . ? C49A C50A C51A C52A 170.8(15) . . . . ? C50 C51 C52 C53 33.4(10) . . . . ? C50 C51 C52 C57 -142.7(7) . . . . ? C50A C51A C52A C53A 134(2) . . . . ? C50A C51A C52A C57A -51(3) . . . . ? C51A C52A C53A C54A 179(3) . . . . ? C51A C52A C57A C56A -179(2) . . . . ? C52 C51 C50 Pd1 -113.1(7) . . . . ? C52 C51 C50 C49 -171.0(6) . . . . ? C52 C53 C54 C55 0.3(11) . . . . ? C52A C53A C54A C55A 0(5) . . . . ? C53 C52 C57 C56 -3.0(11) . . . . ? C53 C54 C55 C56 -1.3(10) . . . . ? C53A C52A C57A C56A -3(3) . . . . ? C53A C54A C55A C56A -4(5) . . . . ? C54 C55 C56 C57 0.1(11) . . . . ? C54A C55A C56A C57A 4(4) . . . . ? C55 C56 C57 C52 2.1(12) . . . . ? C55A C56A C57A C52A 0(4) . . . . ? C57 C52 C53 C54 1.8(11) . . . . ? C57A C52A C53A C54A 3(4) . . . . ? O1 C58 C59 C60 26.7(10) . . . . ? C58 O1 C61 C60 -16.4(7) . . . . ? C58 C59 C60 C61 -35.6(9) . . . . ? C59 C60 C61 O1 32.7(8) . . . . ? C61 O1 C58 C59 -6.7(8) . . . . ? O2 C62 C63 C64 29.4(6) . . . . ? C62 O2 C65 C64 17.3(8) . . . . ? C62 C63 C64 C65 -18.8(7) . . . . ? C63 C64 C65 O2 1.8(7) . . . . ? C65 O2 C62 C63 -29.5(7) . . . . ? O3 C66 C67 C68 -33.0(6) . . . . ? C66 O3 C69 C68 -27.1(6) . . . . ? C66 C67 C68 C69 16.0(6) . . . . ? C67 C68 C69 O3 5.2(6) . . . . ? C69 O3 C66 C67 38.0(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.4474 8.3100 8.3474 -0.0028 0.4472 0.8944 0.7693 -11.5365 2.8304 0.0022 -1.0000 0.0000 -2.9330 -5.5295 -10.0682 0.0024 -0.1789 -0.9839 0.4448 12.0196 1.3637 -0.0028 0.9285 0.3714 4.9902 2.1036 -1.3132 0.8570 0.0024 0.5154 -0.0248 2.5524 13.3652 -0.6255 -0.0006 0.7802 -0.0065 -2.9640 -13.0133 0.6046 -0.0368 -0.7729