#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:40:53 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705297.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_7705297 loop_ _publ_author_name 'Exp\'osito, J. Emilio' 'Aull\'on, Gabriel' 'Bardaji, Manuel' 'Miguel, Jesus Angel' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02494E _journal_year 2020 _chemical_formula_moiety 'C56 H38 N2 O4 Pd2' _chemical_formula_sum 'C56 H38 N2 O4 Pd2' _chemical_formula_weight 1015.68 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-08-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-08 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 116.206(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.6782(8) _cell_length_b 17.1192(5) _cell_length_c 16.1066(7) _cell_measurement_reflns_used 5219 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.3959 _cell_measurement_theta_min 2.2020 _cell_volume 4620.8(4) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.4757 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.840 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -57.00 36.00 1.0000 11.6900 omega____ theta____ kappa____ phi______ frames - 12.4346 -37.0000 -120.0000 93 #__ type_ start__ end____ width___ exp.time_ 2 omega 19.00 76.00 1.0000 11.6900 omega____ theta____ kappa____ phi______ frames - 12.4346 37.0000 -150.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega 45.00 99.00 1.0000 11.6900 omega____ theta____ kappa____ phi______ frames - 12.4346 179.0000 -150.0000 54 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0055243000 _diffrn_orient_matrix_UB_12 -0.0173874000 _diffrn_orient_matrix_UB_13 -0.0367101000 _diffrn_orient_matrix_UB_21 0.0270475000 _diffrn_orient_matrix_UB_22 -0.0271901000 _diffrn_orient_matrix_UB_23 0.0314971000 _diffrn_orient_matrix_UB_31 -0.0321188000 _diffrn_orient_matrix_UB_32 -0.0259586000 _diffrn_orient_matrix_UB_33 -0.0084751000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.840 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 12093 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.840 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.461 _diffrn_reflns_theta_min 2.379 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.460 _exptl_crystal_description block _exptl_crystal_F_000 2048 _exptl_crystal_size_max 0.4132 _exptl_crystal_size_mid 0.3198 _exptl_crystal_size_min 0.1502 _refine_diff_density_max 0.518 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 5402 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0329 _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^)+(0.0389P)^2^+0.5378P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.0841 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4012 _reflns_number_total 5402 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 4 _cod_database_code 7705297 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C56 H38 N2 O4 Pd2' _chemical_oxdiff_usercomment THF/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 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C25(H25), C22(H22), C14(H14), C7(H7), C24(H24), C9(H9), C15(H15), C20(H20), C8(H8), C16(H16), C18(H18), C19(H19) 2.b Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL je244.3b_a.res in C2/c je244.3b.res created by SHELXL-2018/3 at 12:18:46 on 06-Aug-2020 REM Old TITL JE 244 in C2/c REM SHELXT solution in C2/c REM R1 0.127, Rweak 0.023, Alpha 0.046, Orientation as input REM Formula found by SHELXT: C15 N2 O3 Pd CELL 0.71073 18.6782 17.1192 16.1066 90 116.206 90 ZERR 4 0.0008 0.0005 0.0007 0 0.006 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Pd UNIT 224 152 8 16 8 L.S. 20 PLAN 10 TEMP 20(2) BOND $H LIST 6 ABIN fmap 2 acta REM REM REM WGHT 0.038900 0.537800 FVAR 0.11589 PD1 5 0.415202 0.387861 0.716859 11.00000 0.04582 0.03211 = 0.03714 -0.00352 0.01256 -0.00288 O1 4 0.415475 0.480442 0.637481 11.00000 0.06018 0.03503 = 0.04721 0.00405 0.01394 -0.00101 O2 4 0.543624 0.469612 0.666930 11.00000 0.06548 0.04567 = 0.04979 0.01296 0.02257 0.00254 N1 3 0.413429 0.292777 0.786617 11.00000 0.04681 0.03864 = 0.03938 -0.00240 0.01754 -0.00430 C2 1 0.379560 0.310884 0.616581 11.00000 0.03763 0.03666 = 0.03867 -0.00254 0.01225 0.00006 C21 1 0.402232 0.223173 0.741242 11.00000 0.03530 0.03633 = 0.04385 -0.00077 0.01402 -0.00206 C4 1 0.338922 0.273475 0.456162 11.00000 0.03535 0.04100 = 0.03642 -0.00196 0.00989 -0.00088 C6 1 0.347755 0.174122 0.571770 11.00000 0.04223 0.03583 = 0.04347 -0.00220 0.01401 -0.00344 C5 1 0.331615 0.194198 0.478836 11.00000 0.03284 0.03982 = 0.04314 -0.00718 0.01059 -0.00255 C1 1 0.375822 0.233675 0.641365 11.00000 0.04033 0.03451 = 0.03992 -0.00151 0.01307 -0.00299 C3 1 0.360227 0.329255 0.524358 11.00000 0.04458 0.03382 = 0.04213 0.00155 0.01135 -0.00286 AFIX 43 H3 2 0.361866 0.381268 0.508620 11.00000 -1.20000 AFIX 0 C27 1 0.476456 0.501267 0.629776 11.00000 0.06405 0.03351 = 0.03531 0.00130 0.01204 -0.00120 C13 1 0.321557 0.294333 0.360200 11.00000 0.03948 0.05089 = 0.04009 -0.00395 0.01141 -0.00024 C12 1 0.296046 0.234893 0.290932 11.00000 0.04142 0.06296 = 0.04357 -0.01021 0.01412 0.00115 C11 1 0.288431 0.156227 0.313259 11.00000 0.04558 0.05754 = 0.04707 -0.01369 0.01836 -0.00376 C25 1 0.436765 0.293486 0.878316 11.00000 0.06419 0.04912 = 0.04553 -0.00734 0.02453 -0.00760 AFIX 43 H25 2 0.443457 0.341466 0.907912 11.00000 -1.20000 AFIX 0 C10 1 0.305924 0.135367 0.409247 11.00000 0.04091 0.04588 = 0.05231 -0.01158 0.01573 -0.00293 C22 1 0.421150 0.155321 0.793520 11.00000 0.06256 0.04137 = 0.04544 0.00014 0.01612 -0.00340 AFIX 43 H22 2 0.417454 0.107685 0.764138 11.00000 -1.20000 AFIX 0 C14 1 0.330090 0.368932 0.334401 11.00000 0.06388 0.05480 = 0.04064 0.00281 0.01307 -0.00030 AFIX 43 H14 2 0.346018 0.408232 0.378814 11.00000 -1.20000 AFIX 0 C7 1 0.331729 0.096701 0.588678 11.00000 0.07069 0.04660 = 0.04972 -0.00550 0.01984 -0.01358 AFIX 43 H7 2 0.338296 0.082860 0.647456 11.00000 -1.20000 AFIX 0 C24 1 0.451076 0.227295 0.929949 11.00000 0.07244 0.06308 = 0.04323 0.00303 0.02321 -0.00744 AFIX 43 H24 2 0.464552 0.230123 0.992782 11.00000 -1.20000 AFIX 0 C9 1 0.295537 0.060245 0.432312 11.00000 0.07012 0.04269 = 0.06259 -0.01803 0.02243 -0.01464 AFIX 43 H9 2 0.280650 0.021220 0.387626 11.00000 -1.20000 AFIX 0 C17 1 0.278490 0.254941 0.197399 11.00000 0.05976 0.08217 = 0.03993 -0.00832 0.01802 -0.00125 C23 1 0.445317 0.156191 0.887856 11.00000 0.06282 0.05357 = 0.05208 0.01029 0.02059 -0.00657 C15 1 0.315722 0.388174 0.243681 11.00000 0.07923 0.06519 = 0.05132 0.01300 0.02173 0.00333 AFIX 43 H15 2 0.324136 0.438934 0.229371 11.00000 -1.20000 AFIX 0 C20 1 0.262910 0.100850 0.242285 11.00000 0.08394 0.06725 = 0.06687 -0.02160 0.03546 -0.00974 AFIX 43 H20 2 0.258359 0.048916 0.256220 11.00000 -1.20000 AFIX 0 C8 1 0.306818 0.041960 0.520364 11.00000 0.09001 0.03910 = 0.06998 -0.00691 0.02765 -0.01938 AFIX 43 H8 2 0.297248 -0.008784 0.533516 11.00000 -1.20000 AFIX 0 C16 1 0.289553 0.332544 0.177031 11.00000 0.08559 0.08480 = 0.04398 0.00646 0.02608 0.00051 AFIX 43 H16 2 0.278706 0.345953 0.116672 11.00000 -1.20000 AFIX 0 C18 1 0.251723 0.196389 0.129340 11.00000 0.09919 0.10182 = 0.04462 -0.01513 0.03430 -0.00939 AFIX 43 H18 2 0.239011 0.209221 0.068304 11.00000 -1.20000 AFIX 0 C19 1 0.244138 0.121151 0.151484 11.00000 0.09693 0.09609 = 0.05538 -0.03449 0.03523 -0.01398 AFIX 43 H19 2 0.226281 0.083091 0.105567 11.00000 -1.20000 AFIX 0 C28 1 0.464894 0.570944 0.568294 11.00000 0.08639 0.06245 = 0.07148 0.03291 0.02574 0.00674 AFIX 137 H28A 2 0.453447 0.553579 0.507025 11.00000 -1.50000 H28B 2 0.512652 0.601910 0.592479 11.00000 -1.50000 H28C 2 0.421201 0.601826 0.566129 11.00000 -1.50000 AFIX 0 C26 1 0.466216 0.080970 0.942085 11.00000 0.12655 0.06741 = 0.05994 0.02198 0.02667 -0.00391 AFIX 137 H26A 2 0.456661 0.037762 0.900523 11.00000 -1.50000 H26B 2 0.433798 0.075448 0.974273 11.00000 -1.50000 H26C 2 0.521498 0.081797 0.985995 11.00000 -1.50000 AFIX 0 HKLF 4 REM je244.3b_a.res in C2/c REM wR2 = 0.0841, GooF = S = 1.011, Restrained GooF = 1.011 for all data REM R1 = 0.0329 for 4012 Fo > 4sig(Fo) and 0.0506 for all 5402 data REM 291 parameters refined using 0 restraints END WGHT 0.0389 0.5545 REM Highest difference peak 0.518, deepest hole -0.437, 1-sigma level 0.061 Q1 1 0.2523 0.1109 0.3430 11.00000 0.05 0.52 Q2 1 0.4730 0.3819 0.7230 11.00000 0.05 0.38 Q3 1 0.4104 0.3874 0.6647 11.00000 0.05 0.38 Q4 1 0.3774 0.2304 0.6836 11.00000 0.05 0.31 Q5 1 0.4782 0.5973 0.6189 11.00000 0.05 0.30 Q6 1 0.3375 0.1864 0.5228 11.00000 0.05 0.29 Q7 1 0.3432 0.2814 0.4187 11.00000 0.05 0.29 Q8 1 0.5833 0.4882 0.7016 11.00000 0.05 0.26 Q9 1 0.3009 0.0928 0.6466 11.00000 0.05 0.26 Q10 1 0.3000 0.2358 0.2561 11.00000 0.05 0.26 ; _shelx_res_checksum 56555 _shelx_fab_file ; -25 1 13 -3.6628 0.1181 -25 3 6 -0.2581 -0.2149 -25 3 7 0.6115 -0.1107 -25 5 7 -3.6414 0.0293 -25 5 8 2.3707 0.1211 -25 5 9 2.9503 0.0270 -25 5 10 -2.9520 -0.0433 -24 0 2 -0.8463 0.2748 -24 0 4 -1.0267 -0.3808 -24 0 12 -4.3031 0.4797 -24 0 14 5.6896 -0.5435 -24 2 3 1.8239 -0.1809 -24 2 4 3.0048 -0.0731 -24 2 5 -3.4252 0.0425 -24 2 6 0.5363 -0.0559 -24 2 7 0.5030 0.0698 -24 2 8 -1.1365 0.1355 -24 2 11 -0.1605 -0.1318 -24 2 12 1.0934 0.1206 -24 2 13 3.8984 0.0634 -24 2 14 -1.1753 -0.1063 -24 4 4 -1.2515 0.1205 -24 4 5 -1.5608 0.1911 -24 4 6 -0.7138 0.0214 -24 4 7 3.5668 -0.0989 -24 4 8 2.6646 -0.1586 -24 4 9 -3.9221 0.0932 -24 4 10 -0.9378 0.0519 -24 4 11 2.8853 -0.0857 -24 4 13 -2.9932 0.0652 -24 4 14 -0.4324 0.1007 -24 4 15 -0.1888 -0.0253 -24 6 6 1.1403 0.0151 -24 6 7 1.4347 -0.0520 -24 6 8 -2.5118 -0.0903 -24 6 9 -1.4624 0.0456 -24 6 10 2.9817 0.1665 -24 6 11 0.8745 -0.0225 -24 6 12 0.3647 -0.0667 -24 6 13 0.2428 0.0161 -23 1 1 1.6983 0.0471 -23 1 2 1.2506 -0.1004 -23 1 3 2.4590 0.2064 -23 1 4 -2.2448 0.1702 -23 1 5 1.2557 -0.0712 -23 1 6 1.7392 -0.0760 -23 1 7 -1.2380 -0.0043 -23 1 8 0.8190 0.0632 -23 1 9 0.0822 0.2239 -23 1 10 0.5930 -0.0441 -23 1 11 1.5980 -0.2489 -23 1 12 2.0924 0.0848 -23 1 13 -5.3499 0.3212 -23 1 14 -2.4137 0.0268 -23 1 15 0.0629 -0.2503 -23 3 2 0.3916 -0.0687 -23 3 3 -2.9632 0.1171 -23 3 4 0.0683 0.0306 -23 3 5 2.3739 -0.0744 -23 3 6 -0.2003 -0.0201 -23 3 7 1.3829 -0.1734 -23 3 8 -1.9731 0.0221 -23 3 9 -0.2722 0.1834 -23 3 10 0.7818 0.0919 -23 3 11 1.3109 -0.1380 -23 3 12 -4.1947 -0.1439 -23 3 13 -0.1741 0.1971 -23 3 14 0.3397 0.1386 -23 3 15 1.7905 -0.0889 -23 5 3 -1.4704 -0.0337 -23 5 4 0.4211 -0.0727 -23 5 5 1.0591 0.0396 -23 5 6 -1.2270 0.0897 -23 5 7 -4.0580 0.0319 -23 5 8 2.0667 -0.0817 -23 5 9 4.9054 0.0021 -23 5 10 -1.5593 0.1186 -23 5 11 -3.4619 0.0107 -23 5 12 1.0886 -0.1217 -23 5 13 1.2105 -0.0817 -23 5 14 -1.1265 0.1495 -23 5 15 0.9843 0.0400 -23 7 5 -0.0505 -0.0069 -23 7 6 -0.4330 0.0204 -23 7 7 -1.5734 0.0214 -23 7 8 2.8151 -0.0367 -23 7 9 0.1409 -0.1020 -23 7 10 -3.4633 0.0361 -23 7 11 -1.6003 0.1274 -23 7 12 0.4219 -0.0913 -23 7 13 0.6391 -0.0975 -23 7 14 0.4288 -0.0407 -23 7 15 -0.8845 -0.0111 -22 0 2 1.3934 0.1252 -22 0 4 -0.6933 0.2691 -22 0 6 -1.7412 -0.4317 -22 0 8 -1.4261 0.7564 -22 0 10 0.7941 -0.8852 -22 0 12 -5.6666 0.7606 -22 0 14 5.0316 -0.5785 -22 0 16 -1.5458 0.2427 -22 2 1 -1.4134 -0.1253 -22 2 2 -1.7843 -0.0538 -22 2 3 0.4655 -0.1098 -22 2 4 2.5526 0.0532 -22 2 5 -3.3153 0.1481 -22 2 6 1.5110 -0.2073 -22 2 7 -0.8778 -0.2057 -22 2 8 -0.8716 0.1806 -22 2 9 -0.6818 0.1168 -22 2 10 0.7501 -0.1369 -22 2 11 -2.1642 -0.1893 -22 2 12 2.1164 0.0962 -22 2 13 1.8794 0.0593 -22 2 14 1.2615 -0.0429 -22 2 15 -1.6213 -0.0814 -22 2 16 -5.4902 -0.0378 -22 4 1 -1.1774 0.0372 -22 4 2 -0.6348 -0.0066 -22 4 3 2.2521 -0.1000 -22 4 4 -0.6180 0.1207 -22 4 5 -1.4429 0.1406 -22 4 6 -1.2925 -0.0030 -22 4 7 3.1583 -0.1248 -22 4 8 2.3050 -0.1063 -22 4 9 -2.3249 0.1068 -22 4 10 -3.3228 0.0436 -22 4 11 2.6498 -0.0196 -22 4 12 2.1746 -0.0876 -22 4 13 -1.3982 -0.0381 -22 4 14 0.2826 0.0205 -22 4 15 -0.3223 0.0371 -22 4 16 -1.3803 0.0864 -22 6 2 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-0.3714 0.0878 13 1 6 -0.9474 0.1200 13 1 7 0.3738 -0.3738 13 1 8 0.2173 -0.1284 13 1 9 -1.0827 0.4218 13 1 10 -0.3439 0.0284 13 3 0 1.6458 0.0517 13 3 1 -1.2728 -0.1856 13 3 2 -0.0513 -0.1644 13 3 3 0.1214 0.1227 13 3 4 0.8940 -0.0317 13 3 5 -0.5921 -0.0627 13 3 6 0.5582 0.1297 13 3 7 0.1644 0.0076 13 3 8 -1.9795 -0.2488 13 3 9 -0.2193 0.1213 13 3 10 2.1601 0.2859 13 5 0 -0.4009 0.1176 13 5 1 1.1744 -0.0364 13 5 2 0.1214 -0.1563 13 5 3 1.6320 -0.0048 13 5 4 0.9321 0.0625 13 5 5 -0.4311 -0.0792 13 5 6 0.1338 -0.0126 13 5 7 -1.9509 0.1233 13 5 8 2.1846 -0.0956 13 5 9 2.2305 -0.0679 13 5 10 1.4085 0.1657 13 7 0 1.1642 0.1266 13 7 1 -1.0393 0.0682 13 7 2 -0.4827 -0.0441 13 7 3 0.7973 -0.0992 13 7 4 -0.6465 0.0455 13 7 5 -1.0268 0.0459 13 7 6 -1.1748 -0.0447 13 7 7 1.0576 0.0951 13 7 8 -1.5058 0.0517 13 9 0 -0.9768 -0.0215 13 9 1 0.0684 0.1216 13 9 2 -0.9222 0.0134 13 9 3 -0.1888 -0.0595 13 9 4 -1.1077 -0.0480 13 9 5 -0.6289 0.0462 13 9 6 -1.9618 0.0458 13 9 7 -2.3887 0.0181 13 9 8 1.9214 0.0236 13 11 0 -0.1421 -0.0848 13 11 1 -1.0439 0.0242 13 11 2 0.0710 0.0696 13 11 3 -0.2205 -0.0420 13 11 4 0.9745 -0.0351 13 11 5 0.1869 -0.0527 13 11 6 0.4936 0.0314 13 13 0 1.1049 -0.0587 13 13 1 -0.6752 -0.0454 13 13 2 0.6499 0.0350 13 13 3 -0.7108 -0.0136 13 13 4 0.5907 -0.0946 13 13 5 3.1349 -0.0687 13 15 0 -0.5257 0.0340 13 15 1 -0.6344 -0.0366 13 15 2 -3.0861 0.0262 13 15 3 -0.5332 0.0449 13 17 0 0.6132 0.0265 14 0 0 1.7202 -0.6209 14 0 2 -0.7649 0.0221 14 0 4 0.6965 0.5521 14 0 6 0.3666 -1.0014 14 0 8 -1.7550 1.1035 14 2 0 -1.4424 -0.1576 14 2 1 0.2661 -0.0916 14 2 2 -0.2266 0.1703 14 2 3 -0.0983 0.0519 14 2 4 0.3694 -0.0171 14 2 5 0.7031 0.0838 14 2 6 0.0914 -0.0132 14 2 7 -0.7899 -0.1039 14 2 8 0.8219 0.1544 14 2 9 3.1643 0.1533 14 4 0 0.5649 -0.0302 14 4 1 -0.1216 -0.1095 14 4 2 -0.6380 0.0052 14 4 3 0.6905 0.1569 14 4 4 -0.5161 0.0482 14 4 5 0.3525 -0.0671 14 4 6 -0.4949 0.0425 14 4 7 2.6405 0.0216 14 4 8 1.8080 -0.0343 14 4 9 -1.6491 -0.0348 14 6 0 -1.8892 0.0734 14 6 1 -0.9400 -0.0284 14 6 2 0.6816 -0.0837 14 6 3 -1.5548 0.0550 14 6 4 -0.9122 0.1622 14 6 5 -0.4121 -0.0332 14 6 6 2.0037 -0.0606 14 6 7 -0.8116 0.0632 14 6 8 -2.0882 0.0591 14 6 9 -1.5803 -0.1677 14 8 0 1.3266 0.0671 14 8 1 0.8547 0.0054 14 8 2 1.0343 -0.0776 14 8 3 -1.8394 -0.0251 14 8 4 0.1850 0.0803 14 8 5 0.8198 0.1040 14 8 6 0.6509 -0.1087 14 8 7 2.2216 -0.0726 14 10 0 -0.9893 -0.0316 14 10 1 1.2943 0.0420 14 10 2 -0.5370 -0.0580 14 10 3 1.9859 -0.0545 14 10 4 0.6174 0.0106 14 10 5 1.0447 0.0918 14 10 6 2.7398 -0.0072 14 12 0 0.1084 -0.0439 14 12 1 0.9885 0.0202 14 12 2 1.2009 0.0234 14 12 3 -0.5958 -0.0594 14 12 4 0.2300 -0.0082 14 12 5 -2.7687 0.0347 14 14 0 0.4261 -0.0142 14 14 1 -0.6492 0.0002 14 14 2 -0.6107 0.0456 14 14 3 3.6616 0.0283 14 16 0 0.6399 0.0243 15 1 0 -0.6711 -0.0114 15 1 1 0.1017 0.3395 15 1 2 0.4585 0.1834 15 1 3 0.1151 -0.4976 15 1 4 -0.0331 -0.0841 15 1 5 -0.1633 0.5279 15 1 6 -0.0323 0.0430 15 1 7 0.8680 -0.4602 15 1 8 2.7113 -0.0027 15 3 0 0.3630 -0.0448 15 3 1 -0.7111 0.0320 15 3 2 2.3616 0.1950 15 3 3 -0.3114 -0.0661 15 3 4 -0.7990 -0.3288 15 3 5 -0.2224 0.1084 15 3 6 0.2879 0.2458 15 3 7 -0.4927 -0.1905 15 3 8 -3.8794 -0.2363 15 5 0 -0.0691 0.0028 15 5 1 1.4742 -0.0438 15 5 2 -1.4361 0.0387 15 5 3 -0.2510 0.0493 15 5 4 0.7143 -0.1812 15 5 5 0.4643 -0.1299 15 5 6 -2.3684 0.1747 15 5 7 -2.2822 0.0784 15 5 8 0.9374 -0.2311 15 7 0 0.9847 0.0524 15 7 1 0.1141 -0.0324 15 7 2 -1.5382 0.0410 15 7 3 1.7194 0.0118 15 7 4 1.4821 -0.0316 15 7 5 -0.5523 -0.1550 15 7 6 0.4296 -0.0262 15 7 7 -0.7656 0.1274 15 7 8 1.1876 -0.0548 15 9 0 0.4100 0.0471 15 9 1 -1.7264 0.0079 15 9 2 1.8987 0.0118 15 9 3 1.1736 0.0288 15 9 4 -0.8131 -0.0246 15 9 5 0.4524 -0.0871 15 11 0 -0.2225 0.0082 15 11 1 0.6326 0.0540 15 11 2 -2.3656 0.0219 15 11 3 -1.7215 0.0259 15 11 4 -0.9184 -0.0114 15 13 0 -0.6779 -0.0420 15 13 1 -2.9456 -0.0073 15 13 2 2.5646 0.0421 16 0 0 1.3376 0.4989 16 0 2 -1.0889 -1.3494 16 0 4 -0.4227 1.2906 16 0 6 0.1016 -1.0895 16 2 0 -0.3488 -0.0291 16 2 1 1.1037 -0.0279 16 2 2 -1.0869 -0.0748 16 2 3 -1.2412 -0.1541 16 2 4 0.1757 0.1670 16 2 5 -0.5319 0.2017 16 2 6 -0.1672 -0.1913 16 2 7 -2.8950 -0.1557 16 4 0 1.4101 -0.0832 16 4 1 -1.9593 -0.0947 16 4 2 -0.9798 -0.0476 16 4 3 1.7231 0.0391 16 4 4 0.2079 0.0025 16 4 5 -0.4757 0.0787 16 4 6 1.6456 0.0622 16 4 7 3.5090 -0.1149 16 6 0 -0.6319 -0.0072 16 6 1 -0.4975 -0.0349 16 6 2 1.5636 -0.0714 16 6 3 -0.7928 0.0572 16 6 4 -1.1229 0.0496 16 6 5 1.7629 -0.0256 16 6 6 0.3756 0.0372 16 6 7 0.0289 0.0704 16 8 0 -0.4206 0.0549 16 8 1 1.8474 -0.0245 16 8 2 0.6497 -0.0750 16 8 3 -2.8448 -0.0015 16 8 4 0.0627 0.0995 16 8 5 -1.3446 0.0325 16 10 0 0.1472 0.0490 16 10 1 -1.2380 0.0409 16 10 2 -2.0427 -0.0699 16 10 3 1.1665 -0.0372 16 10 4 -0.6153 0.0809 16 12 0 -2.1286 -0.0427 16 12 1 3.4871 0.0720 16 12 2 2.1089 -0.0096 17 1 0 -0.5732 0.1164 17 1 1 0.5512 0.5940 17 1 2 0.4226 0.0733 17 1 3 0.4565 -0.4763 17 1 4 0.1263 0.0657 17 1 5 0.2394 0.2937 17 1 6 -1.0220 -0.0834 17 3 0 -1.4116 -0.0848 17 3 1 -0.5493 0.1695 17 3 2 2.5729 0.2699 17 3 3 0.9247 -0.1663 17 3 4 0.2129 -0.2091 17 3 5 1.5192 0.1659 17 3 6 1.1227 0.0804 17 5 0 -0.3858 -0.0895 17 5 1 1.2315 0.0468 17 5 2 -2.0468 0.1908 17 5 3 -0.6556 0.0288 17 5 4 1.3531 -0.1790 17 5 5 -2.7869 -0.0394 17 5 6 -3.1223 0.1859 17 7 0 0.8323 -0.0295 17 7 1 0.0174 -0.0532 17 7 2 -1.1688 0.1008 17 7 3 1.7526 0.1258 17 7 4 -0.8015 -0.0664 17 7 5 0.4859 -0.0956 17 7 6 2.0278 0.0431 17 9 0 -0.0726 0.0450 17 9 1 -1.8569 -0.0812 17 9 2 2.2142 0.0076 17 9 3 0.6642 0.0685 17 11 0 2.0776 0.0540 17 11 1 2.2641 -0.0254 18 0 0 1.2029 0.8153 18 0 2 -1.4633 -1.0518 18 0 4 -0.5788 0.6184 18 2 0 -0.1685 0.1133 18 2 1 0.3149 0.0730 18 2 2 0.7399 -0.1871 18 2 3 -0.8830 -0.1655 18 2 4 0.1661 0.2011 18 2 5 -0.3557 0.1602 18 4 0 1.8143 -0.0188 18 4 1 -1.9232 0.0313 18 4 2 -1.3725 -0.0278 18 4 3 0.2403 -0.1032 18 4 4 -2.6326 -0.0615 18 4 5 -0.7767 0.1645 18 6 0 0.3403 -0.0794 18 6 1 1.0055 -0.0368 18 6 2 1.4213 0.0242 18 6 3 -1.5728 -0.0355 18 6 4 1.7326 -0.0837 18 6 5 4.1862 -0.0071 18 8 0 -1.2678 -0.0332 18 8 1 1.1377 -0.0666 18 8 2 -0.3161 -0.0573 18 8 3 -1.1410 0.0224 18 8 4 0.6312 -0.0598 18 8 5 -2.9436 -0.1263 18 10 0 0.7384 0.0611 18 10 1 -1.3091 -0.0194 19 1 0 -0.8212 0.1469 19 1 1 2.8493 0.2259 19 1 2 0.0568 -0.0839 19 1 3 0.4677 0.0002 19 1 4 -0.1083 0.1901 19 3 0 -0.9745 -0.0181 19 3 1 -1.6844 0.1257 19 3 2 0.4885 0.0214 19 3 3 0.1922 -0.1465 19 3 4 1.0294 0.0339 19 5 0 0.5256 -0.1056 19 5 1 0.5817 0.0670 19 5 2 -1.0909 0.1113 19 5 3 2.0169 -0.0124 19 5 4 2.3804 -0.0441 19 7 0 -0.0630 -0.0888 19 7 1 -0.7008 -0.0334 19 7 2 -0.0169 0.1020 19 7 3 0.6436 0.0877 19 7 4 -3.7707 -0.0702 19 9 0 0.5144 0.0119 20 0 0 3.6966 0.3143 20 0 2 -0.7384 -0.0150 20 2 0 -2.1106 0.1249 20 2 1 -0.8682 0.0238 20 2 2 1.1216 -0.1716 20 2 3 0.4952 -0.0963 20 4 0 1.0815 0.0215 20 4 1 -0.2196 0.1593 20 4 2 -0.3657 0.0496 20 4 3 -0.1951 -0.1116 20 4 4 -2.6329 -0.0498 20 6 0 0.0666 -0.0324 20 6 1 1.2432 0.0509 20 6 2 0.1076 0.0931 20 6 3 -3.0576 -0.0912 20 6 4 2.7936 -0.0820 21 1 0 -1.3206 0.0077 21 1 1 2.3782 -0.1996 21 1 2 0.5907 -0.1039 21 3 0 0.7448 0.1412 21 3 1 -1.8327 0.0505 21 3 2 -0.5415 -0.1292 21 5 0 0.8980 -0.0286 21 5 1 0.5193 -0.0018 21 5 2 -0.9542 -0.0470 22 0 0 2.9204 -0.1692 22 2 0 -2.1938 0.0775 22 2 1 -0.8344 -0.0602 22 4 0 1.2556 -0.0341 22 4 1 0.0220 0.1222 23 1 0 -0.4951 -0.1766 0 0 0 0.0 0.0 ; _shelx_fab_checksum 47841 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.41520(2) 0.38786(2) 0.71686(2) 0.04046(8) Uani 1 1 d . . . . . O1 O 0.41548(11) 0.48044(10) 0.63748(12) 0.0510(5) Uani 1 1 d . . . . . O2 O 0.54362(12) 0.46961(11) 0.66693(13) 0.0547(5) Uani 1 1 d . . . . . N1 N 0.41343(12) 0.29278(12) 0.78662(14) 0.0422(5) Uani 1 1 d . . . . . C2 C 0.37956(14) 0.31088(15) 0.61658(17) 0.0393(6) Uani 1 1 d . . . . . C21 C 0.40223(14) 0.22317(15) 0.74124(17) 0.0398(6) Uani 1 1 d . . . . . C4 C 0.33892(14) 0.27347(15) 0.45616(17) 0.0398(6) Uani 1 1 d . . . . . C6 C 0.34776(14) 0.17412(15) 0.57177(17) 0.0423(6) Uani 1 1 d . . . . . C5 C 0.33161(14) 0.19420(15) 0.47884(18) 0.0409(6) Uani 1 1 d . . . . . C1 C 0.37582(14) 0.23368(14) 0.64136(17) 0.0400(6) Uani 1 1 d . . . . . C3 C 0.36023(14) 0.32925(15) 0.52436(17) 0.0430(6) Uani 1 1 d . . . . . H3 H 0.361866 0.381268 0.508620 0.052 Uiso 1 1 calc R . . . . C27 C 0.47646(18) 0.50127(15) 0.62978(18) 0.0479(7) Uani 1 1 d . . . . . C13 C 0.32156(15) 0.29433(16) 0.36020(18) 0.0457(6) Uani 1 1 d . . . . . C12 C 0.29605(15) 0.23489(18) 0.29093(19) 0.0510(7) Uani 1 1 d . . . . . C11 C 0.28843(15) 0.15623(18) 0.31326(19) 0.0508(7) Uani 1 1 d . . . . . C25 C 0.43677(17) 0.29349(17) 0.87832(19) 0.0528(7) Uani 1 1 d . . . . . H25 H 0.443457 0.341466 0.907912 0.063 Uiso 1 1 calc R . . . . C10 C 0.30592(15) 0.13537(17) 0.4092(2) 0.0481(7) Uani 1 1 d . . . . . C22 C 0.42115(16) 0.15532(16) 0.79352(19) 0.0526(7) Uani 1 1 d . . . . . H22 H 0.417454 0.107685 0.764138 0.063 Uiso 1 1 calc R . . . . C14 C 0.33009(18) 0.36893(18) 0.3344(2) 0.0568(7) Uani 1 1 d . . . . . H14 H 0.346018 0.408232 0.378814 0.068 Uiso 1 1 calc R . . . . C7 C 0.33173(18) 0.09670(17) 0.5887(2) 0.0581(8) Uani 1 1 d . . . . . H7 H 0.338296 0.082860 0.647456 0.070 Uiso 1 1 calc R . . . . C24 C 0.45108(18) 0.22730(19) 0.9299(2) 0.0604(8) Uani 1 1 d . . . . . H24 H 0.464552 0.230123 0.992782 0.073 Uiso 1 1 calc R . . . . C9 C 0.29554(18) 0.06024(17) 0.4323(2) 0.0610(8) Uani 1 1 d . . . . . H9 H 0.280650 0.021220 0.387626 0.073 Uiso 1 1 calc R . . . . C17 C 0.27849(17) 0.2549(2) 0.1974(2) 0.0621(8) Uani 1 1 d . . . . . C23 C 0.44532(18) 0.15619(18) 0.8879(2) 0.0579(7) Uani 1 1 d . . . . . C15 C 0.3157(2) 0.38817(19) 0.2437(2) 0.0678(9) Uani 1 1 d . . . . . H15 H 0.324136 0.438934 0.229371 0.081 Uiso 1 1 calc R . . . . C20 C 0.2629(2) 0.1008(2) 0.2423(2) 0.0719(9) Uani 1 1 d . . . . . H20 H 0.258359 0.048916 0.256220 0.086 Uiso 1 1 calc R . . . . C8 C 0.3068(2) 0.04196(18) 0.5204(2) 0.0692(9) Uani 1 1 d . . . . . H8 H 0.297248 -0.008784 0.533516 0.083 Uiso 1 1 calc R . . . . C16 C 0.2896(2) 0.3325(2) 0.1770(2) 0.0724(9) Uani 1 1 d . . . . . H16 H 0.278706 0.345953 0.116672 0.087 Uiso 1 1 calc R . . . . C18 C 0.2517(2) 0.1964(2) 0.1293(2) 0.0809(11) Uani 1 1 d . . . . . H18 H 0.239011 0.209221 0.068304 0.097 Uiso 1 1 calc R . . . . C19 C 0.2441(2) 0.1212(2) 0.1515(3) 0.0822(11) Uani 1 1 d . . . . . H19 H 0.226281 0.083091 0.105567 0.099 Uiso 1 1 calc R . . . . C28 C 0.4649(2) 0.5709(2) 0.5683(2) 0.0768(10) Uani 1 1 d . . . . . H28A H 0.453447 0.553579 0.507025 0.115 Uiso 1 1 calc GR . . . . H28B H 0.512652 0.601910 0.592479 0.115 Uiso 1 1 calc GR . . . . H28C H 0.421201 0.601826 0.566129 0.115 Uiso 1 1 calc GR . . . . C26 C 0.4662(3) 0.0810(2) 0.9421(2) 0.0899(12) Uani 1 1 d . . . . . H26A H 0.456661 0.037762 0.900523 0.135 Uiso 1 1 calc GR . . . . H26B H 0.433798 0.075448 0.974273 0.135 Uiso 1 1 calc GR . . . . H26C H 0.521498 0.081797 0.985995 0.135 Uiso 1 1 calc GR . . . . 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 0.04582(13) 0.03211(12) 0.03714(13) -0.00352(8) 0.01256(10) -0.00288(9) O1 0.0602(12) 0.0350(10) 0.0472(11) 0.0041(8) 0.0139(9) -0.0010(9) O2 0.0655(13) 0.0457(11) 0.0498(12) 0.0130(9) 0.0226(10) 0.0025(10) N1 0.0468(12) 0.0386(12) 0.0394(12) -0.0024(10) 0.0175(10) -0.0043(10) C2 0.0376(13) 0.0367(14) 0.0387(14) -0.0025(11) 0.0123(11) 0.0001(11) C21 0.0353(12) 0.0363(14) 0.0439(14) -0.0008(12) 0.0140(11) -0.0021(11) C4 0.0353(12) 0.0410(15) 0.0364(13) -0.0020(11) 0.0099(11) -0.0009(11) C6 0.0422(13) 0.0358(14) 0.0435(15) -0.0022(12) 0.0140(12) -0.0034(12) C5 0.0328(12) 0.0398(15) 0.0431(14) -0.0072(12) 0.0106(11) -0.0026(11) C1 0.0403(13) 0.0345(14) 0.0399(14) -0.0015(11) 0.0131(11) -0.0030(11) C3 0.0446(14) 0.0338(14) 0.0421(14) 0.0016(12) 0.0114(12) -0.0029(12) C27 0.0641(18) 0.0335(14) 0.0353(14) 0.0013(11) 0.0120(14) -0.0012(14) C13 0.0395(14) 0.0509(17) 0.0401(15) -0.0039(13) 0.0114(12) -0.0002(12) C12 0.0414(14) 0.0630(19) 0.0436(15) -0.0102(14) 0.0141(12) 0.0011(14) C11 0.0456(15) 0.0575(19) 0.0471(16) -0.0137(14) 0.0184(13) -0.0038(14) C25 0.0642(18) 0.0491(17) 0.0455(16) -0.0073(13) 0.0245(14) -0.0076(14) C10 0.0409(14) 0.0459(16) 0.0523(17) -0.0116(13) 0.0157(13) -0.0029(13) C22 0.0626(17) 0.0414(16) 0.0454(16) 0.0001(13) 0.0161(14) -0.0034(14) C14 0.0639(18) 0.0548(18) 0.0406(16) 0.0028(14) 0.0131(14) -0.0003(15) C7 0.071(2) 0.0466(18) 0.0497(17) -0.0055(14) 0.0198(16) -0.0136(15) C24 0.0724(19) 0.063(2) 0.0432(16) 0.0030(15) 0.0232(15) -0.0074(17) C9 0.070(2) 0.0427(17) 0.063(2) -0.0180(15) 0.0224(16) -0.0146(15) C17 0.0598(18) 0.082(2) 0.0399(16) -0.0083(16) 0.0180(14) -0.0012(17) C23 0.0628(18) 0.0536(19) 0.0521(18) 0.0103(15) 0.0206(15) -0.0066(15) C15 0.079(2) 0.065(2) 0.0513(19) 0.0130(16) 0.0217(17) 0.0033(17) C20 0.084(2) 0.067(2) 0.067(2) -0.0216(17) 0.0355(19) -0.0097(18) C8 0.090(2) 0.0391(17) 0.070(2) -0.0069(16) 0.0276(19) -0.0194(17) C16 0.086(2) 0.085(3) 0.0440(18) 0.0065(18) 0.0261(17) 0.001(2) C18 0.099(3) 0.102(3) 0.0446(19) -0.015(2) 0.0343(19) -0.009(2) C19 0.097(3) 0.096(3) 0.055(2) -0.034(2) 0.035(2) -0.014(2) C28 0.086(2) 0.062(2) 0.071(2) 0.0329(18) 0.0257(19) 0.0067(18) C26 0.127(3) 0.067(2) 0.060(2) 0.0220(19) 0.027(2) -0.004(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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _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 23 -2 0 0.0374 23.0000 -2.0000 0.0000 0.1640 0.6797 -0.6860 24 -6 -15 0.0796 24.0000 -6.0000 -15.0000 0.7894 0.3412 -0.4862 18 -1 7 0.0328 18.0000 -1.0000 7.0000 -0.1383 0.7379 -0.6112 -4 5 21 0.1232 -4.0000 5.0000 21.0000 -0.8798 0.4194 -0.1807 0 24 -2 0.2213 -0.0000 24.0000 -2.0000 -0.3439 -0.7151 -0.6087 -3 -24 2 0.1750 -3.0000 -24.0000 2.0000 0.3271 0.6335 0.7050 -24 -1 1 0.0885 -24.0000 -1.0000 1.0000 -0.1541 -0.5938 0.7878 14 -7 -22 0.1368 14.0000 -7.0000 -22.0000 1.0075 -0.1248 -0.0796 -22 -6 19 0.1231 -22.0000 -6.0000 19.0000 -0.7163 0.1655 0.7008 7 23 -4 0.1752 7.0000 23.0000 -4.0000 -0.2138 -0.5608 -0.7903 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 O1 Pd1 Pd1 85.70(5) . 2_656 ? O1 Pd1 O2 86.67(7) . 2_656 ? O2 Pd1 Pd1 76.57(5) 2_656 2_656 ? N1 Pd1 Pd1 94.66(6) . 2_656 ? N1 Pd1 O1 175.95(8) . . ? N1 Pd1 O2 97.34(8) . 2_656 ? C2 Pd1 Pd1 102.99(7) . 2_656 ? C2 Pd1 O1 95.74(9) . . ? C2 Pd1 O2 177.52(9) . 2_656 ? C2 Pd1 N1 80.25(9) . . ? C27 O1 Pd1 122.59(17) . . ? C27 O2 Pd1 125.90(17) . 2_656 ? C21 N1 Pd1 116.71(16) . . ? C25 N1 Pd1 122.44(18) . . ? C25 N1 C21 119.7(2) . . ? C1 C2 Pd1 116.38(18) . . ? C1 C2 C3 119.7(2) . . ? C3 C2 Pd1 123.90(19) . . ? N1 C21 C1 112.2(2) . . ? N1 C21 C22 118.0(2) . . ? C22 C21 C1 129.8(2) . . ? C5 C4 C13 119.8(2) . . ? C3 C4 C5 118.8(2) . . ? C3 C4 C13 121.4(2) . . ? C5 C6 C1 118.8(2) . . ? C7 C6 C5 117.5(2) . . ? C7 C6 C1 123.6(2) . . ? C4 C5 C6 119.7(2) . . ? C10 C5 C4 120.6(2) . . ? C10 C5 C6 119.7(2) . . ? C2 C1 C21 113.3(2) . . ? C2 C1 C6 119.9(2) . . ? C6 C1 C21 126.8(2) . . ? C2 C3 H3 118.7 . . ? C4 C3 C2 122.6(2) . . ? C4 C3 H3 118.7 . . ? O1 C27 C28 114.8(3) . . ? O2 C27 O1 126.5(2) . . ? O2 C27 C28 118.8(3) . . ? C12 C13 C4 119.3(2) . . ? C14 C13 C4 122.7(2) . . ? C14 C13 C12 118.0(3) . . ? C13 C12 C17 119.5(3) . . ? C11 C12 C13 121.0(3) . . ? C11 C12 C17 119.5(3) . . ? C12 C11 C10 119.7(2) . . ? C20 C11 C12 118.3(3) . . ? C20 C11 C10 122.1(3) . . ? N1 C25 H25 118.5 . . ? N1 C25 C24 123.1(3) . . ? C24 C25 H25 118.5 . . ? C5 C10 C11 119.7(3) . . ? C9 C10 C5 119.2(3) . . ? C9 C10 C11 121.1(3) . . ? C21 C22 H22 119.0 . . ? C23 C22 C21 122.1(3) . . ? C23 C22 H22 119.0 . . ? C13 C14 H14 118.7 . . ? C13 C14 C15 122.6(3) . . ? C15 C14 H14 118.7 . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7 119.5 . . ? C25 C24 H24 120.5 . . ? C25 C24 C23 119.0(3) . . ? C23 C24 H24 120.5 . . ? C10 C9 H9 119.5 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C16 C17 C12 118.8(3) . . ? C18 C17 C12 119.1(3) . . ? C18 C17 C16 122.1(3) . . ? C22 C23 C26 120.2(3) . . ? C24 C23 C22 118.0(3) . . ? C24 C23 C26 121.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C11 C20 H20 119.1 . . ? C19 C20 C11 121.9(3) . . ? C19 C20 H20 119.1 . . ? C7 C8 C9 121.3(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C17 C16 H16 119.4 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.6 . . ? C20 C19 H19 119.8 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 Pd1 2.8614(4) 2_656 ? Pd1 O1 2.0377(18) . ? Pd1 O2 2.1868(18) 2_656 ? Pd1 N1 1.986(2) . ? Pd1 C2 1.959(2) . ? O1 C27 1.251(3) . ? O2 C27 1.250(3) . ? N1 C21 1.365(3) . ? N1 C25 1.343(3) . ? C2 C1 1.391(3) . ? C2 C3 1.401(3) . ? C21 C1 1.471(3) . ? C21 C22 1.386(4) . ? C4 C5 1.428(3) . ? C4 C3 1.375(3) . ? C4 C13 1.476(3) . ? C6 C5 1.432(3) . ? C6 C1 1.432(3) . ? C6 C7 1.412(4) . ? C5 C10 1.423(4) . ? C3 H3 0.9300 . ? C27 C28 1.504(4) . ? C13 C12 1.427(4) . ? C13 C14 1.374(4) . ? C12 C11 1.417(4) . ? C12 C17 1.435(4) . ? C11 C10 1.476(4) . ? C11 C20 1.397(4) . ? C25 H25 0.9300 . ? C25 C24 1.360(4) . ? C10 C9 1.376(4) . ? C22 H22 0.9300 . ? C22 C23 1.381(4) . ? C14 H14 0.9300 . ? C14 C15 1.403(4) . ? C7 H7 0.9300 . ? C7 C8 1.361(4) . ? C24 H24 0.9300 . ? C24 C23 1.374(4) . ? C9 H9 0.9300 . ? C9 C8 1.375(4) . ? C17 C16 1.405(5) . ? C17 C18 1.404(5) . ? C23 C26 1.507(4) . ? C15 H15 0.9300 . ? C15 C16 1.355(5) . ? C20 H20 0.9300 . ? C20 C19 1.389(5) . ? C8 H8 0.9300 . ? C16 H16 0.9300 . ? C18 H18 0.9300 . ? C18 C19 1.360(5) . ? C19 H19 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.336 0.750 202.3 40.0 ? 2 0.000 0.664 0.250 202.3 40.6 ? 3 0.500 0.164 0.250 202.3 40.6 ? 4 0.500 0.836 0.750 202.3 40.0 ?