#------------------------------------------------------------------------------ #$Date: 2021-08-11 01:17:46 +0300 (Wed, 11 Aug 2021) $ #$Revision: 268012 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564338.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_1564338 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 'C54 H21 F20 N5 Pd2, C7 H16' _chemical_formula_sum 'C61 H37 F20 N5 Pd2' _chemical_formula_weight 1432.75 _chemical_name_common 'Gross222b (Chosen)' _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 mixed _audit_block_doi 10.5517/ccdc.csd.cc24wl6v _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-25 deposited with the CCDC. 2021-08-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.406(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.504(3) _cell_length_b 21.031(3) _cell_length_c 16.726(3) _cell_measurement_reflns_used 5355 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 25.108 _cell_measurement_theta_min 1.526 _cell_volume 6074.5(17) _computing_cell_refinement 'APEX2 v2010.7-0 (Bruker AXS)' _computing_data_collection 'Bruker Instrument Service v2010.7.0.0' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 95 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'APEX2 (Bruker AXS)' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_unetI/netI 0.0725 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23168 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.108 _diffrn_reflns_theta_max 25.108 _diffrn_reflns_theta_min 1.526 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_crystal_colour green-blue _exptl_crystal_density_diffrn 1.567 _exptl_crystal_description plate _exptl_crystal_F_000 2840 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.090 _refine_diff_density_max 1.526 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.109 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 393 _refine_ls_number_reflns 5355 _refine_ls_number_restraints 131 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0546 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1318 _refine_ls_wR_factor_ref 0.1511 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4626 _reflns_number_total 5355 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02593g2.cif _cod_data_source_block Gross222b _cod_original_cell_volume 6074.5(16) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1564338 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_min 0.885 _shelx_estimated_absorpt_t_max 0.940 _shelx_res_file ; TITL mo_Gross222b_0m_a.res in C2/c gross222b.res created by SHELXL-2018/3 at 12:24:30 on 11-Mar-2019 REM Old TITL mo_Gross222b_0m in C2/c REM SHELXT solution in C2/c REM R1 0.156, Rweak 0.012, Alpha 0.060, Orientation as input REM Formula found by SHELXT: C54 N5 F20 Pd2 CELL 0.71073 17.5036 21.0311 16.7264 90 99.406 90 ZERR 4 0.0026 0.0032 0.0025 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N Pd UNIT 244 148 80 20 8 DFIX 1.5 0.001 C28 C29 DFIX 1.5 0.001 C29 C30 DFIX 1.5 0.001 C30 C31 DELU EADP F8A C22 EADP F8 C22 L.S. 10 PLAN 20 SIZE 0.09 0.12 0.18 TEMP -73 LIST 6 fmap 2 acta OMIT 4 4 2 OMIT 1 1 2 OMIT -5 3 2 OMIT 3 1 8 OMIT -2 2 4 OMIT -2 0 4 OMIT 2 2 0 OMIT -4 2 8 OMIT -2 4 4 OMIT 0 6 0 OMIT 5 5 4 OMIT 3 3 2 OMIT -4 8 4 OMIT -1 1 1 OMIT -8 6 8 OMIT -1 5 2 OMIT -3 7 8 OMIT 8 6 3 OMIT -4 4 3 OMIT -4 2 4 OMIT 4 2 2 OMIT 0 2 2 OMIT 5 3 2 OMIT 2 4 0 OMIT -9 9 3 OMIT -1 3 2 OMIT -2 0 2 OMIT 1 1 1 OMIT -2 2 2 OMIT -1 1 2 OMIT 0 4 0 OMIT 0 2 0 OMIT 0 4 2 OMIT -3 1 2 OMIT 4 0 2 OMIT 1 1 3 OMIT -2 4 2 OMIT 0 4 1 OMIT 0 0 2 OMIT 1 7 2 OMIT 2 0 0 OMIT 1 3 3 OMIT 1 3 0 OMIT 7 3 12 OMIT 1 3 8 REM REM REM WGHT 0.085300 FVAR 0.17886 0.41804 PD1 5 0.497208 0.467489 0.348651 11.00000 0.03626 0.02731 = 0.03161 0.00047 0.01202 -0.00046 F1 3 0.487771 0.667776 0.502776 11.00000 0.06319 0.05323 = 0.04783 -0.00498 0.00299 0.01064 F2 3 0.445836 0.768161 0.585711 11.00000 0.11214 0.07984 = 0.06133 -0.03399 0.02631 -0.00121 F3 3 0.323277 0.839031 0.524155 11.00000 0.09587 0.07144 = 0.14577 -0.05713 0.05635 0.00893 F4 3 0.240266 0.810098 0.378314 11.00000 0.08746 0.08291 = 0.16784 -0.03704 -0.00462 0.05750 F5 3 0.281639 0.710171 0.293067 11.00000 0.08570 0.07296 = 0.09513 -0.02145 -0.02446 0.03742 F6 3 0.172051 0.404812 0.268400 11.00000 0.07621 0.10541 = 0.09176 0.01617 -0.01736 -0.02301 F7 3 0.048347 0.354274 0.321058 11.00000 0.04520 0.12137 = 0.27581 -0.02398 0.00296 -0.02823 PART 1 F8 3 0.058685 0.298983 0.454728 -21.00000 0.08948 0.08152 = 0.15541 -0.03734 0.08228 -0.05369 PART 0 PART 2 F8A 3 0.074368 0.301651 0.494825 21.00000 0.08948 0.08152 = 0.15541 -0.03734 0.08228 -0.05369 PART 0 F9 3 0.207439 0.296546 0.567173 11.00000 0.20604 0.10765 = 0.11405 0.02233 0.11059 -0.04181 F10 3 0.329230 0.346192 0.512538 11.00000 0.09549 0.07994 = 0.05841 0.01879 0.01278 -0.02763 N1 4 0.388934 0.510210 0.348190 11.00000 0.03705 0.02801 = 0.02848 -0.00122 0.01373 -0.00481 N2 4 0.439060 0.385022 0.302388 11.00000 0.04362 0.02579 = 0.03572 -0.00203 0.02127 -0.00252 N3 4 0.500000 0.607993 0.250000 10.50000 0.04439 0.01497 = 0.03953 0.00000 0.02071 0.00000 AFIX 43 H3 2 0.500001 0.566150 0.250001 10.50000 -1.20000 AFIX 0 C1 1 0.409526 0.629207 0.350174 11.00000 0.04134 0.02309 = 0.03769 -0.00146 0.01244 0.00197 C2 1 0.372429 0.572302 0.367142 11.00000 0.03672 0.03026 = 0.03425 -0.00030 0.01566 0.00320 C3 1 0.305019 0.572352 0.404686 11.00000 0.04544 0.03335 = 0.04966 -0.00700 0.02596 -0.00103 AFIX 43 H3A 2 0.282883 0.608575 0.425984 11.00000 -1.20000 AFIX 0 C4 1 0.278004 0.512591 0.404925 11.00000 0.03534 0.04385 = 0.04903 -0.00068 0.02390 -0.00021 AFIX 43 H4 2 0.232678 0.499026 0.424473 11.00000 -1.20000 AFIX 0 C5 1 0.330736 0.473213 0.370002 11.00000 0.03138 0.03945 = 0.03361 0.00004 0.01251 -0.00499 C6 1 0.322902 0.407151 0.362066 11.00000 0.04075 0.03128 = 0.03713 -0.00030 0.01837 -0.00630 C7 1 0.371274 0.366819 0.327696 11.00000 0.04739 0.03196 = 0.03266 -0.00236 0.01294 -0.00680 C8 1 0.359786 0.300052 0.311982 11.00000 0.05506 0.03422 = 0.04048 0.00133 0.02049 -0.01190 AFIX 43 H8 2 0.317904 0.275224 0.324353 11.00000 -1.20000 AFIX 0 C9 1 0.418847 0.278773 0.276598 11.00000 0.06595 0.02864 = 0.05462 -0.00476 0.02700 -0.00974 AFIX 43 H9 2 0.426891 0.236480 0.259834 11.00000 -1.20000 AFIX 0 C10 1 0.467057 0.332954 0.269409 11.00000 0.05703 0.02242 = 0.04218 0.00247 0.02329 -0.00029 C11 1 0.478034 0.709941 0.279357 11.00000 0.06190 0.02208 = 0.05109 -0.00025 0.02920 0.00372 AFIX 43 H11 2 0.461065 0.746731 0.304368 11.00000 -1.20000 AFIX 0 C12 1 0.460568 0.644635 0.298553 11.00000 0.04545 0.02073 = 0.03470 0.00125 0.01825 0.00181 C13 1 0.385410 0.685611 0.395633 11.00000 0.04095 0.02509 = 0.04378 0.00311 0.02129 0.00342 C14 1 0.426097 0.701953 0.470650 11.00000 0.05121 0.03332 = 0.04464 0.00216 0.02969 0.00144 C15 1 0.405599 0.753360 0.513334 11.00000 0.06653 0.04261 = 0.04826 -0.01328 0.03189 -0.00479 C16 1 0.342660 0.788680 0.481320 11.00000 0.06472 0.04467 = 0.08695 -0.02446 0.04327 0.00459 C17 1 0.301279 0.775377 0.407256 11.00000 0.04803 0.05206 = 0.09798 -0.01150 0.01966 0.02276 C18 1 0.322543 0.723304 0.365425 11.00000 0.05130 0.04485 = 0.06704 -0.00963 0.00907 0.01382 AFIX 66 C19 1 0.253884 0.377383 0.389517 11.00000 0.04985 0.03383 = 0.05290 -0.00869 0.02297 -0.01516 C20 1 0.181695 0.379120 0.340473 11.00000 0.05161 0.05688 = 0.08910 -0.01105 0.01164 -0.01923 C21 1 0.117650 0.353082 0.367758 11.00000 0.05351 0.06720 = 0.15269 -0.01640 0.03816 -0.02385 C22 1 0.125793 0.325306 0.444088 11.00000 0.08948 0.08152 = 0.15541 -0.03734 0.08228 -0.05369 C23 1 0.197982 0.323569 0.493133 11.00000 0.10424 0.05068 = 0.09921 -0.01672 0.07083 -0.02804 C24 1 0.262028 0.349607 0.465849 11.00000 0.07124 0.04342 = 0.05780 -0.00137 0.03227 -0.01588 AFIX 0 C25 1 0.613109 0.431848 0.378848 11.00000 0.04454 0.05026 = 0.04678 -0.00133 -0.00091 0.01045 H25A 2 0.616907 0.404802 0.436875 11.00000 0.06815 H25B 2 0.623800 0.402276 0.328062 11.00000 0.09205 C26 1 0.614700 0.497442 0.373661 11.00000 0.03992 0.05488 = 0.04830 0.00585 0.00576 -0.00176 AFIX 13 H26 2 0.638977 0.518364 0.330335 11.00000 -1.20000 AFIX 0 C27 1 0.570908 0.532889 0.418953 11.00000 0.04279 0.04757 = 0.04291 -0.00902 -0.00086 0.00117 AFIX 23 H27A 2 0.563417 0.578283 0.404048 11.00000 -1.20000 H27B 2 0.580581 0.525500 0.478202 11.00000 -1.20000 AFIX 0 C28 1 0.199304 0.560517 0.177796 11.00000 0.19040 0.33966 = 0.28406 0.13434 0.10378 0.13307 AFIX 137 H28A 2 0.179314 0.536622 0.128505 11.00000 -1.50000 H28B 2 0.222795 0.531018 0.220140 11.00000 -1.50000 H28C 2 0.238398 0.590994 0.166171 11.00000 -1.50000 AFIX 0 C29 1 0.134103 0.595593 0.206224 11.00000 0.17917 0.22693 = 0.25637 -0.03508 0.08507 -0.00487 AFIX 23 H29A 2 0.113230 0.626273 0.163274 11.00000 -1.20000 H29B 2 0.156518 0.620778 0.254385 11.00000 -1.20000 AFIX 0 C30 1 0.066924 0.558904 0.227954 11.00000 0.28502 0.25358 = 0.59689 0.15692 0.28500 0.07434 AFIX 23 H30A 2 0.086850 0.530808 0.274165 11.00000 -1.20000 H30B 2 0.046800 0.531102 0.181505 11.00000 -1.20000 AFIX 0 C31 1 0.000000 0.595763 0.250000 10.50000 0.19248 0.18526 = 0.28594 0.00000 0.10040 0.00000 AFIX 23 H31A 2 0.020124 0.623704 0.296305 10.50000 -1.20000 H31B 2 -0.020124 0.623706 0.203697 10.50000 -1.20000 AFIX 0 HKLF 4 REM mo_Gross222b_0m_a.res in C2/c REM wR2 = 0.1511, GooF = S = 1.012, Restrained GooF = 1.003 for all data REM R1 = 0.0546 for 3626 Fo > 4sig(Fo) and 0.0923 for all 5355 data REM 393 parameters refined using 131 restraints END WGHT 0.0853 0.0000 REM Highest difference peak 1.526, deepest hole -0.571, 1-sigma level 0.109 Q1 1 0.5655 0.5228 0.2926 11.00000 0.05 1.53 Q2 1 0.6045 0.4731 0.2899 11.00000 0.05 1.18 Q3 1 0.6019 0.4760 0.4555 11.00000 0.05 0.61 Q4 1 0.5678 0.4199 0.3129 11.00000 0.05 0.51 Q5 1 0.1252 0.3305 0.4049 11.00000 0.05 0.48 Q6 1 0.1376 0.3227 0.4774 11.00000 0.05 0.47 Q7 1 0.0672 0.4408 0.0549 11.00000 0.05 0.45 Q8 1 0.0664 0.4701 -0.0130 11.00000 0.05 0.44 Q9 1 0.1162 0.4685 0.0765 11.00000 0.05 0.43 Q10 1 0.1631 0.5003 0.1040 11.00000 0.05 0.40 Q11 1 0.0457 0.4007 0.3348 11.00000 0.05 0.40 Q12 1 0.0691 0.3214 0.3546 11.00000 0.05 0.39 Q13 1 0.5630 0.5204 0.4782 11.00000 0.05 0.38 Q14 1 0.1585 0.3695 0.3535 11.00000 0.05 0.37 Q15 1 0.3108 0.7379 0.2614 11.00000 0.05 0.35 Q16 1 0.3816 0.6023 0.3436 11.00000 0.05 0.35 Q17 1 0.0646 0.5632 0.3591 11.00000 0.05 0.33 Q18 1 0.1957 0.2928 0.5359 11.00000 0.05 0.32 Q19 1 0.3694 0.3431 0.3252 11.00000 0.05 0.32 Q20 1 -0.0158 0.5469 -0.0056 11.00000 0.05 0.32 ; _shelx_res_checksum 78930 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 0.49721(2) 0.46749(2) 0.34865(2) 0.03100(17) Uani 1 1 d . U . . . F1 F 0.4878(2) 0.66778(17) 0.5028(2) 0.0554(9) Uani 1 1 d . U . . . F2 F 0.4458(3) 0.7682(2) 0.5857(3) 0.0831(14) Uani 1 1 d . U . . . F3 F 0.3233(3) 0.8390(2) 0.5242(3) 0.1003(17) Uani 1 1 d . U . . . F4 F 0.2403(3) 0.8101(2) 0.3783(4) 0.116(2) Uani 1 1 d . U . . . F5 F 0.2816(3) 0.7102(2) 0.2931(3) 0.0890(15) Uani 1 1 d . U . . . F6 F 0.1721(3) 0.4048(2) 0.2684(3) 0.0946(15) Uani 1 1 d . U . . . F7 F 0.0483(3) 0.3543(3) 0.3211(5) 0.150(3) Uani 1 1 d . U . . . F8 F 0.0587(9) 0.2990(6) 0.4547(16) 0.102(2) Uani 0.58(3) 1 d . U P A 1 F8A F 0.0744(12) 0.3017(9) 0.495(2) 0.102(2) Uani 0.42(3) 1 d . U P A 2 F9 F 0.2074(4) 0.2965(3) 0.5672(3) 0.133(2) Uani 1 1 d . U . . . F10 F 0.3292(3) 0.3462(2) 0.5125(2) 0.0779(13) Uani 1 1 d . U . . . N1 N 0.3889(3) 0.5102(2) 0.3482(3) 0.0302(10) Uani 1 1 d . U . . . N2 N 0.4391(3) 0.3850(2) 0.3024(3) 0.0334(10) Uani 1 1 d . U . . . N3 N 0.500000 0.6080(3) 0.250000 0.0314(15) Uani 1 2 d S TU P . . H3 H 0.500001 0.566150 0.250001 0.038 Uiso 1 2 calc R U P . . C1 C 0.4095(3) 0.6292(2) 0.3502(3) 0.0334(12) Uani 1 1 d . U . . . C2 C 0.3724(3) 0.5723(3) 0.3671(3) 0.0326(12) Uani 1 1 d . U . . . C3 C 0.3050(3) 0.5724(3) 0.4047(4) 0.0408(14) Uani 1 1 d . U . . . H3A H 0.282883 0.608575 0.425984 0.049 Uiso 1 1 calc R U . . . C4 C 0.2780(3) 0.5126(3) 0.4049(4) 0.0408(14) Uani 1 1 d . U . . . H4 H 0.232678 0.499026 0.424473 0.049 Uiso 1 1 calc R U . . . C5 C 0.3307(3) 0.4732(3) 0.3700(3) 0.0340(12) Uani 1 1 d . U . . . C6 C 0.3229(3) 0.4072(3) 0.3621(3) 0.0350(13) Uani 1 1 d . U . . . C7 C 0.3713(3) 0.3668(3) 0.3277(3) 0.0366(13) Uani 1 1 d . U . . . C8 C 0.3598(4) 0.3001(3) 0.3120(3) 0.0418(14) Uani 1 1 d . U . . . H8 H 0.317904 0.275224 0.324353 0.050 Uiso 1 1 calc R U . . . C9 C 0.4188(4) 0.2788(3) 0.2766(4) 0.0478(16) Uani 1 1 d . U . . . H9 H 0.426891 0.236480 0.259834 0.057 Uiso 1 1 calc R U . . . C10 C 0.4671(3) 0.3330(3) 0.2694(4) 0.0388(14) Uani 1 1 d . U . . . C11 C 0.4780(3) 0.7099(3) 0.2794(4) 0.0428(15) Uani 1 1 d . U . . . H11 H 0.461065 0.746731 0.304368 0.051 Uiso 1 1 calc R U . . . C12 C 0.4606(3) 0.6446(2) 0.2986(3) 0.0323(12) Uani 1 1 d . U . . . C13 C 0.3854(3) 0.6856(2) 0.3956(4) 0.0350(12) Uani 1 1 d . U . . . C14 C 0.4261(4) 0.7020(3) 0.4706(4) 0.0406(13) Uani 1 1 d . U . . . C15 C 0.4056(4) 0.7534(3) 0.5133(4) 0.0499(15) Uani 1 1 d . U . . . C16 C 0.3427(4) 0.7887(3) 0.4813(5) 0.0620(18) Uani 1 1 d . U . . . C17 C 0.3013(4) 0.7754(3) 0.4073(5) 0.065(2) Uani 1 1 d . U . . . C18 C 0.3225(4) 0.7233(3) 0.3654(4) 0.0545(17) Uani 1 1 d . U . . . C19 C 0.2539(2) 0.3774(2) 0.3895(3) 0.0439(14) Uani 1 1 d G U . . . C20 C 0.1817(3) 0.3791(2) 0.3405(3) 0.0658(19) Uani 1 1 d G U . . . C21 C 0.1176(2) 0.3531(3) 0.3678(4) 0.089(2) Uani 1 1 d G U . . . C22 C 0.1258(3) 0.3253(2) 0.4441(4) 0.102(2) Uani 1 1 d G U . . . C23 C 0.1980(3) 0.3236(2) 0.4931(3) 0.079(2) Uani 1 1 d G U . . . C24 C 0.2620(2) 0.3496(2) 0.4658(2) 0.0551(17) Uani 1 1 d G U . . . C25 C 0.6131(4) 0.4318(3) 0.3788(4) 0.0481(16) Uani 1 1 d . U . . . H25A H 0.617(4) 0.405(3) 0.437(4) 0.07(2) Uiso 1 1 d . . . . . H25B H 0.624(4) 0.402(4) 0.328(5) 0.09(3) Uiso 1 1 d . . . . . C26 C 0.6147(3) 0.4974(3) 0.3737(4) 0.0479(15) Uani 1 1 d . U . . . H26 H 0.638977 0.518364 0.330335 0.057 Uiso 1 1 calc R U . . . C27 C 0.5709(3) 0.5329(3) 0.4190(4) 0.0453(15) Uani 1 1 d . U . . . H27A H 0.563417 0.578283 0.404048 0.054 Uiso 1 1 calc R U . . . H27B H 0.580581 0.525500 0.478202 0.054 Uiso 1 1 calc R U . . . C28 C 0.1993(10) 0.5605(10) 0.1778(12) 0.264(12) Uani 1 1 d D U . . . H28A H 0.179314 0.536622 0.128505 0.396 Uiso 1 1 calc R U . . . H28B H 0.222795 0.531018 0.220140 0.396 Uiso 1 1 calc R U . . . H28C H 0.238398 0.590994 0.166171 0.396 Uiso 1 1 calc R U . . . C29 C 0.1341(8) 0.5956(8) 0.2062(11) 0.215(8) Uani 1 1 d D U . . . H29A H 0.113230 0.626273 0.163274 0.258 Uiso 1 1 calc R U . . . H29B H 0.156518 0.620778 0.254385 0.258 Uiso 1 1 calc R U . . . C30 C 0.0669(10) 0.5589(7) 0.2280(18) 0.35(2) Uani 1 1 d D U . . . H30A H 0.086850 0.530808 0.274165 0.426 Uiso 1 1 calc R U . . . H30B H 0.046800 0.531102 0.181505 0.426 Uiso 1 1 calc R U . . . C31 C 0.000000 0.5958(10) 0.250000 0.214(11) Uani 1 2 d DS TU P . . H31A H 0.020124 0.623704 0.296305 0.257 Uiso 0.5 1 calc R U P . . H31B H -0.020124 0.623706 0.203697 0.257 Uiso 0.5 1 calc R U P . . 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 0.0363(3) 0.0273(3) 0.0316(3) 0.0005(2) 0.01202(18) -0.0005(2) F1 0.063(2) 0.053(2) 0.048(2) -0.0050(18) 0.0030(18) 0.0106(19) F2 0.112(4) 0.080(3) 0.061(3) -0.034(2) 0.026(2) -0.001(3) F3 0.096(3) 0.071(3) 0.146(5) -0.057(3) 0.056(3) 0.009(3) F4 0.087(3) 0.083(3) 0.168(5) -0.037(3) -0.005(3) 0.058(3) F5 0.086(3) 0.073(3) 0.095(3) -0.021(3) -0.024(3) 0.037(3) F6 0.076(3) 0.105(4) 0.092(3) 0.016(3) -0.017(3) -0.023(3) F7 0.045(3) 0.121(5) 0.276(8) -0.024(5) 0.003(4) -0.028(3) F8 0.089(3) 0.082(3) 0.155(6) -0.037(5) 0.082(4) -0.054(3) F8A 0.089(3) 0.082(3) 0.155(6) -0.037(5) 0.082(4) -0.054(3) F9 0.206(6) 0.108(4) 0.114(4) 0.022(3) 0.111(4) -0.042(4) F10 0.095(3) 0.080(3) 0.058(3) 0.019(2) 0.013(2) -0.028(3) N1 0.037(2) 0.028(2) 0.028(2) -0.0012(19) 0.014(2) -0.0048(19) N2 0.044(3) 0.026(2) 0.036(3) -0.0020(19) 0.021(2) -0.0025(19) N3 0.044(4) 0.015(3) 0.040(4) 0.000 0.021(3) 0.000 C1 0.041(3) 0.023(3) 0.038(3) -0.001(2) 0.012(3) 0.002(2) C2 0.037(3) 0.030(3) 0.034(3) 0.000(2) 0.016(2) 0.003(2) C3 0.045(3) 0.033(3) 0.050(4) -0.007(3) 0.026(3) -0.001(3) C4 0.035(3) 0.044(3) 0.049(4) -0.001(3) 0.024(3) 0.000(3) C5 0.031(3) 0.039(3) 0.034(3) 0.000(3) 0.013(2) -0.005(2) C6 0.041(3) 0.031(3) 0.037(3) 0.000(2) 0.018(3) -0.006(2) C7 0.047(3) 0.032(3) 0.033(3) -0.002(2) 0.013(3) -0.007(3) C8 0.055(4) 0.034(3) 0.040(3) 0.001(3) 0.020(3) -0.012(3) C9 0.066(4) 0.029(3) 0.055(4) -0.005(3) 0.027(3) -0.010(3) C10 0.057(4) 0.022(3) 0.042(3) 0.002(2) 0.023(3) 0.000(3) C11 0.062(4) 0.022(3) 0.051(4) 0.000(3) 0.029(3) 0.004(3) C12 0.045(3) 0.021(3) 0.035(3) 0.001(2) 0.018(3) 0.002(2) C13 0.041(3) 0.025(3) 0.044(3) 0.003(2) 0.021(2) 0.003(2) C14 0.051(3) 0.033(3) 0.045(3) 0.002(3) 0.030(3) 0.001(3) C15 0.067(4) 0.043(4) 0.048(4) -0.013(3) 0.032(3) -0.005(3) C16 0.065(4) 0.045(4) 0.087(5) -0.024(4) 0.043(3) 0.005(3) C17 0.048(4) 0.052(4) 0.098(5) -0.012(4) 0.020(4) 0.023(3) C18 0.051(4) 0.045(4) 0.067(4) -0.010(3) 0.009(3) 0.014(3) C19 0.050(3) 0.034(3) 0.053(3) -0.009(3) 0.023(3) -0.015(3) C20 0.052(4) 0.057(5) 0.089(5) -0.011(4) 0.012(4) -0.019(4) C21 0.054(4) 0.067(6) 0.153(7) -0.016(5) 0.038(4) -0.024(4) C22 0.089(3) 0.082(3) 0.155(6) -0.037(5) 0.082(4) -0.054(3) C23 0.104(5) 0.051(5) 0.099(5) -0.017(4) 0.071(4) -0.028(4) C24 0.071(4) 0.043(4) 0.058(4) -0.001(3) 0.032(3) -0.016(3) C25 0.045(3) 0.050(4) 0.047(4) -0.001(3) -0.001(3) 0.010(3) C26 0.040(3) 0.055(4) 0.048(4) 0.006(3) 0.006(3) -0.002(3) C27 0.043(3) 0.048(4) 0.043(4) -0.009(3) -0.001(3) 0.001(3) C28 0.190(16) 0.34(3) 0.28(2) 0.13(2) 0.104(16) 0.133(17) C29 0.179(15) 0.23(2) 0.26(2) -0.035(16) 0.085(14) -0.005(12) C30 0.29(3) 0.25(2) 0.60(6) 0.16(3) 0.28(3) 0.074(18) C31 0.19(2) 0.19(2) 0.29(3) 0.000 0.10(2) 0.000 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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 '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_ _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 N2 Pd1 N1 88.23(17) . . ? N2 Pd1 C27 164.3(2) . . ? N1 Pd1 C27 101.1(2) . . ? N2 Pd1 C26 135.6(2) . . ? N1 Pd1 C26 135.9(2) . . ? C27 Pd1 C26 38.1(2) . . ? N2 Pd1 C25 100.5(2) . . ? N1 Pd1 C25 166.1(2) . . ? C27 Pd1 C25 68.1(2) . . ? C26 Pd1 C25 37.8(2) . . ? C5 N1 C2 106.3(4) . . ? C5 N1 Pd1 117.7(4) . . ? C2 N1 Pd1 128.7(3) . . ? C10 N2 C7 106.7(4) . . ? C10 N2 Pd1 129.4(4) . . ? C7 N2 Pd1 120.5(3) . . ? C12 N3 C12 112.3(6) . 2_655 ? C12 C1 C2 133.7(5) . . ? C12 C1 C13 113.2(5) . . ? C2 C1 C13 113.0(5) . . ? N1 C2 C1 129.3(5) . . ? N1 C2 C3 108.7(5) . . ? C1 C2 C3 121.9(5) . . ? C4 C3 C2 108.5(5) . . ? C3 C4 C5 106.8(5) . . ? N1 C5 C6 126.9(5) . . ? N1 C5 C4 109.6(5) . . ? C6 C5 C4 123.5(5) . . ? C7 C6 C5 126.1(5) . . ? C7 C6 C19 116.7(5) . . ? C5 C6 C19 117.2(5) . . ? N2 C7 C6 124.9(5) . . ? N2 C7 C8 108.5(5) . . ? C6 C7 C8 126.6(5) . . ? C9 C8 C7 108.1(5) . . ? C8 C9 C10 106.1(5) . . ? N2 C10 C10 124.4(3) . 2_655 ? N2 C10 C9 110.6(5) . . ? C10 C10 C9 125.0(4) 2_655 . ? C11 C11 C12 109.1(3) 2_655 . ? C1 C12 N3 132.3(5) . . ? C1 C12 C11 122.8(5) . . ? N3 C12 C11 104.7(5) . . ? C14 C13 C18 116.8(5) . . ? C14 C13 C1 120.6(5) . . ? C18 C13 C1 122.6(6) . . ? F1 C14 C15 118.5(6) . . ? F1 C14 C13 119.7(5) . . ? C15 C14 C13 121.9(6) . . ? F2 C15 C16 120.1(6) . . ? F2 C15 C14 120.7(6) . . ? C16 C15 C14 119.1(6) . . ? F3 C16 C17 120.1(7) . . ? F3 C16 C15 118.4(7) . . ? C17 C16 C15 121.5(6) . . ? F4 C17 C16 120.0(6) . . ? F4 C17 C18 121.4(7) . . ? C16 C17 C18 118.5(6) . . ? F5 C18 C13 119.4(6) . . ? F5 C18 C17 118.4(6) . . ? C13 C18 C17 122.2(7) . . ? C20 C19 C24 120.0 . . ? C20 C19 C6 120.6(4) . . ? C24 C19 C6 119.4(4) . . ? F6 C20 C21 118.4(4) . . ? F6 C20 C19 121.6(4) . . ? C21 C20 C19 120.0 . . ? F7 C21 C20 120.4(5) . . ? F7 C21 C22 119.6(5) . . ? C20 C21 C22 120.0 . . ? F8 C22 C21 109.6(12) . . ? F8 C22 C23 130.1(11) . . ? C21 C22 C23 120.0 . . ? C21 C22 F8A 135.6(14) . . ? C23 C22 F8A 104.0(14) . . ? F9 C23 C24 118.9(5) . . ? F9 C23 C22 121.1(5) . . ? C24 C23 C22 120.0 . . ? F10 C24 C23 118.6(4) . . ? F10 C24 C19 121.4(4) . . ? C23 C24 C19 120.0 . . ? C26 C25 Pd1 70.4(4) . . ? C27 C26 C25 119.0(6) . . ? C27 C26 Pd1 70.3(4) . . ? C25 C26 Pd1 71.8(4) . . ? C26 C27 Pd1 71.7(4) . . ? C28 C29 C30 119.4(14) . . ? C29 C30 C31 117.9(9) . . ? C30 C31 C30 117.8(17) 2 . ? 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 N2 2.094(4) . ? Pd1 N1 2.096(4) . ? Pd1 C27 2.108(6) . ? Pd1 C26 2.126(6) . ? Pd1 C25 2.144(6) . ? F1 C14 1.335(7) . ? F2 C15 1.334(8) . ? F3 C16 1.352(7) . ? F4 C17 1.319(8) . ? F5 C18 1.331(8) . ? F6 C20 1.307(6) . ? F7 C21 1.331(7) . ? F8 C22 1.337(11) . ? F8A C22 1.424(19) . ? F9 C23 1.348(6) . ? F10 C24 1.303(6) . ? N1 C5 1.378(6) . ? N1 C2 1.385(7) . ? N2 C10 1.353(7) . ? N2 C7 1.378(7) . ? N3 C12 1.383(6) . ? N3 C12 1.383(6) 2_655 ? C1 C12 1.379(7) . ? C1 C2 1.412(7) . ? C1 C13 1.506(7) . ? C2 C3 1.424(7) . ? C3 C4 1.343(8) . ? C4 C5 1.434(7) . ? C5 C6 1.400(7) . ? C6 C7 1.388(8) . ? C6 C19 1.498(6) . ? C7 C8 1.437(8) . ? C8 C9 1.349(8) . ? C9 C10 1.435(8) . ? C10 C10 1.413(11) 2_655 ? C11 C11 1.343(11) 2_655 ? C11 C12 1.454(7) . ? C13 C14 1.381(8) . ? C13 C18 1.383(8) . ? C14 C15 1.375(8) . ? C15 C16 1.364(10) . ? C16 C17 1.358(10) . ? C17 C18 1.383(9) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.383(9) . ? C26 C27 1.381(9) . ? C28 C29 1.5000(11) . ? C29 C30 1.5000(11) . ? C30 C31 1.5001(11) . ?