#------------------------------------------------------------------------------ #$Date: 2025-03-08 01:14:20 +0200 (Sat, 08 Mar 2025) $ #$Revision: 298338 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/40/1574093.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_1574093 loop_ _publ_author_name 'Yu, Hao' 'Guo, Ziteng' 'Tang, Jie' 'Han, Ningxu' 'Shi, Junjuan' 'Li, Meng' 'Zhang, Houyu' 'Wang, Ming' _publ_section_title ; Configurational Control of Low-Symmetry Heteroleptic Metal-Organic Cages with Asymmetric Ligands ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC08647C _journal_year 2025 _chemical_formula_moiety 'C282 H204 N24 Pd6' _chemical_formula_sum 'C282 H204 N24 Pd6' _chemical_formula_weight 4567.08 _space_group_crystal_system trigonal _space_group_IT_number 163 _space_group_name_Hall '-P 3 2c' _space_group_name_H-M_alt 'P -3 1 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2025-02-09 _audit_creation_method ; Olex2 1.5-ac6-020 (compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966) ; _audit_update_record ; 2025-02-10 deposited with the CCDC. 2025-03-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 26.2350(17) _cell_length_b 26.2350(17) _cell_length_c 46.357(4) _cell_measurement_reflns_used 9909 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 16.229 _cell_measurement_theta_min 2.272 _cell_volume 27632(3) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'Synchrotron radiation X-ray' _diffrn_measurement_method '\f scans' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.6887 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_unetI/netI 0.1003 _diffrn_reflns_Laue_measured_fraction_full 0.964 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 99021 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 16.499 _diffrn_reflns_theta_max 16.499 _diffrn_reflns_theta_min 0.868 _diffrn_source_current 0.0 _diffrn_source_power 0.0 _diffrn_source_voltage 0.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_T_max 0.7440 _exptl_absorpt_correction_T_min 0.4068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1973 before and 0.0759 after correction. The Ratio of minimum to maximum transmission is 0.5468. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 0.549 _exptl_crystal_description block _exptl_crystal_F_000 4680 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.187 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.397 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 374 _refine_ls_number_reflns 5238 _refine_ls_number_restraints 1204 _refine_ls_restrained_S_all 1.315 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.1258 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3361 _refine_ls_wR_factor_ref 0.3594 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3969 _reflns_number_total 5238 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08647c2.cif _cod_data_source_block 1_CCDC1 _cod_original_cell_volume 27632(4) _cod_database_code 1574093 _shelx_shelxl_version_number 2019/2 _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_max 0.980 _shelx_estimated_absorpt_t_min 0.970 _olex2_refinement_description ; 1. Restrained distances C45-C47 1.5 with sigma of 0.01 C11-C23 1.5 with sigma of 0.01 C23-C45 1.2 with sigma of 0.01 H15-H32 2.2 with sigma of 0.01 C31-C40 1.5 with sigma of 0.01 C40-C31 1.45 with sigma of 0.01 C7-C17 1.5 with sigma of 0.01 2. Rigid bond restraints N4, Pd1, N2 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002 3. Uiso/Uaniso restraints and constraints C1 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C7 \\sim C29 \\sim C15 \\sim C31 \\sim C2 \\sim C33 \\sim C17 \\sim C13 \\sim C35 \\sim C9 \\sim C19 \\sim C37 \\sim C12 \\sim C14 \\sim C16 \\sim C18 \\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C23 \\sim C27 \\sim C32 \\sim C34 \\sim C36 \\sim C38 \\sim C40 \\sim C39 \\sim C5 \\sim C41 \\sim C21 \\sim C43 \\sim C11 \\sim C42 \\sim C44 \\sim C46 \\sim C47 \\sim C3 \\sim C25 \\sim C45 \\sim N1 \\sim N4 \\sim N2 \\sim N3: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A 4.a Aromatic/amide H refined with riding coordinates: C1(H1), C4(H4), C6(H6), C10(H10), C29(H29), C15(H15), C2(H2), C33(H33), C13(H13), C9(H9), C19(H19), C37(H37), C12(H12), C14(H14), C18(H18), C20(H20), C24(H24), C26(H26), C28(H28), C30(H30), C32(H32), C36(H36), C38(H38), C39(H39), C5(H5), C21(H21), C43(H43), C44(H44), C46(H46), C3(H3), C25(H25) 4.b Fitted hexagon refined as free rotating group: N1(C1,C4,C6,C8,C10), C7(C29,C15,C31,C2,C33), C17(C13,C35,C9,C19,C37), C12(N4, C14,C16,C18,C20), C22(C24,C26,N2,C28,C30), C32(C34,N3,C36,C38,C40), C39(C5,C41, C21,C43,C11), C42(C44,C46,C47,C3,C25) 4.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 1_a.res in P-31c 1.res created by SHELXL-2019/2 at 09:03:16 on 19-Sep-2022 REM Old TITL 1 in P-31c #163 REM SHELXT solution in P-31c: R1 0.392, Rweak 0.046, Alpha 0.074 REM 1.045 for 328 systematic absences, Orientation as input REM Formula found by SHELXT: C145 N98 Pd3 CELL 0.6887 26.235 26.235 46.3575 90 90 120 ZERR 2 0.0017 0.0017 0.0043 0 0 0 LATT 1 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -Y,-X,0.5-Z SYMM +Y-X,+Y,0.5-Z SYMM +X,+X-Y,0.5-Z SFAC C H N Pd DISP C 0.0019 0.0015 10.8362 DISP H 0 0 0.6228 DISP N 0.0037 0.0031 18.3135 DISP Pd -1.2476 0.9534 4024.8143 UNIT 564 408 48 12 SIMU 0.01 0.02 3.8 $c $n DFIX 1.5 0.01 C45 C47 DFIX 1.5 0.01 C11 C23 DFIX 1.2 0.01 C23 C45 DFIX 2.2 0.01 H15 H32 DFIX 1.5 0.01 C31 C40 DFIX 1.45 0.01 C40 C31 DELU 0.001 0.002 N4 Pd1 N2 DFIX 1.5 0.01 C7 C17 L.S. 20 0 0 PLAN 100 SIZE 0.15 0.12 0.1 TEMP 0 CONF BOND list 4 MORE -1 BOND $H ABIN fmap 2 53 acta OMIT -3 33 OMIT 0 0 4 OMIT 0 0 10 OMIT 0 0 18 OMIT 0 0 6 OMIT 3 3 6 OMIT 4 0 7 OMIT 1 1 -4 OMIT 0 0 2 OMIT 3 1 1 OMIT 0 0 14 OMIT 3 0 12 OMIT 2 1 3 OMIT 1 1 10 OMIT 3 2 2 OMIT 3 1 8 OMIT 4 1 -6 OMIT 4 1 -8 OMIT 1 1 12 OMIT 2 2 6 OMIT 2 1 -5 OMIT 3 1 -4 OMIT 4 2 -3 OMIT 3 1 7 OMIT 4 0 12 OMIT 4 2 7 OMIT 3 2 0 OMIT 1 1 6 OMIT 1 2 5 OMIT 0 5 6 OMIT -2 6 3 OMIT -1 4 4 OMIT -1 3 5 OMIT 1 3 7 OMIT -5 11 3 OMIT -1 5 8 OMIT -1 5 6 OMIT -3 7 17 OMIT 0 11 7 OMIT 0 9 11 OMIT -4 12 5 OMIT 2 3 18 OMIT -1 9 8 OMIT 0 10 7 OMIT 0 4 12 OMIT -3 12 11 OMIT 1 10 13 OMIT 5 8 4 OMIT 1 5 14 OMIT 1 3 6 OMIT 0 9 3 OMIT -1 5 16 OMIT -4 10 12 OMIT 0 2 7 OMIT 1 2 8 OMIT -2 8 8 OMIT -3 8 12 OMIT 2 4 7 OMIT -1 4 9 OMIT -1 8 7 OMIT -2 10 14 OMIT 0 2 15 OMIT 0 1 13 OMIT 1 4 11 OMIT 1 3 8 OMIT 4 7 7 OMIT -4 10 17 OMIT 0 9 1 OMIT -1 5 5 OMIT 0 4 8 OMIT 3 7 9 OMIT 1 2 23 OMIT 1 5 8 OMIT -1 10 3 OMIT -2 10 22 OMIT 1 2 11 OMIT 2 3 16 OMIT 7 8 7 OMIT -2 5 0 OMIT 0 10 12 OMIT -1 2 2 OMIT -3 9 10 OMIT -3 12 8 OMIT 1 1 2 OMIT -4 9 10 OMIT -2 11 12 OMIT -2 7 16 OMIT -6 12 6 OMIT -2 5 11 OMIT 1 8 15 OMIT 2 6 3 OMIT 0 4 7 OMIT -1 9 0 OMIT 3 8 7 OMIT 1 6 15 OMIT 0 12 11 OMIT 0 2 3 OMIT 1 1 8 OMIT 3 6 4 OMIT 0 6 22 OMIT -3 6 8 OMIT 1 8 6 OMIT 1 11 5 OMIT -2 12 3 OMIT 3 7 2 OMIT 0 5 9 OMIT 2 3 13 OMIT -1 6 18 OMIT -3 12 13 OMIT -2 5 17 OMIT 0 4 16 OMIT 0 1 17 OMIT 2 5 2 OMIT 2 5 20 OMIT 2 10 10 OMIT -3 10 19 OMIT 2 3 8 OMIT -1 9 3 OMIT 1 6 22 OMIT -3 7 16 OMIT -1 3 1 OMIT -2 4 8 OMIT -4 9 9 OMIT -4 8 8 OMIT 1 2 1 OMIT 2 3 15 OMIT -2 5 25 OMIT 1 7 12 OMIT 2 6 13 OMIT 3 5 2 OMIT 0 5 13 OMIT 3 5 12 OMIT 1 11 11 OMIT -4 9 22 OMIT 4 7 18 OMIT -4 10 16 OMIT -4 9 2 OMIT 2 8 3 OMIT 4 6 17 OMIT 1 2 12 OMIT 1 2 3 OMIT 0 0 26 OMIT 4 5 10 OMIT -4 10 4 OMIT 1 5 9 OMIT 0 13 11 OMIT 3 4 22 OMIT -1 3 3 OMIT 1 1 18 OMIT 0 5 7 OMIT 4 8 10 OMIT -6 17 1 OMIT -1 4 18 OMIT -2 12 12 OMIT -2 11 19 OMIT -2 11 4 OMIT 1 5 4 OMIT -2 5 3 OMIT -2 7 4 OMIT -1 3 18 OMIT 2 6 16 OMIT 0 4 15 OMIT -2 8 20 OMIT -2 9 12 OMIT 2 9 9 OMIT -1 3 7 OMIT 1 10 11 OMIT 2 3 20 OMIT 1 7 6 OMIT 1 1 14 OMIT -2 6 4 OMIT 0 8 5 OMIT 0 11 2 OMIT -1 10 12 OMIT -2 6 21 OMIT -4 8 22 OMIT -1 6 3 OMIT 1 8 4 OMIT 3 9 2 OMIT 0 15 6 OMIT 3 4 12 OMIT 1 6 13 OMIT -1 6 4 OMIT 0 4 26 OMIT 3 7 12 OMIT -1 2 20 OMIT -6 12 4 OMIT 0 5 8 OMIT -2 12 11 OMIT -1 7 3 OMIT -1 11 2 OMIT 0 9 5 OMIT 2 3 24 OMIT 0 4 22 OMIT -3 6 2 OMIT 2 5 15 OMIT -3 15 9 OMIT 1 9 11 OMIT -1 6 26 OMIT 5 6 17 OMIT -2 7 15 OMIT -4 10 22 OMIT 2 8 16 OMIT -1 5 0 OMIT 0 6 17 OMIT 4 4 8 OMIT -2 11 2 OMIT 3 5 4 OMIT 1 4 7 OMIT -4 9 18 OMIT -1 13 10 OMIT 3 14 3 OMIT 6 6 4 OMIT -2 6 22 REM REM REM WGHT 0.200000 FVAR 0.14127 PD1 4 1.232087 0.759871 0.646098 11.00000 0.16574 0.14761 = 0.12340 0.00703 -0.00136 0.10236 AFIX 66 N1 3 0.532270 0.706172 0.669905 11.00000 0.11497 0.18518 = 0.18345 -0.00712 0.01661 0.08210 C1 1 0.483411 0.661270 0.683740 11.00000 0.11395 0.18592 = 0.18654 -0.00328 0.01211 0.08113 AFIX 43 H1 2 0.447137 0.659388 0.682411 11.00000 -1.20000 AFIX 65 C4 1 0.488769 0.619182 0.699561 11.00000 0.11551 0.18717 = 0.19009 -0.00213 0.01232 0.08224 AFIX 43 H4 2 0.456079 0.589139 0.708817 11.00000 -1.20000 AFIX 65 C6 1 0.542985 0.621995 0.701547 11.00000 0.12199 0.18977 = 0.19430 0.00437 0.00614 0.08414 AFIX 43 H6 2 0.546570 0.593835 0.712132 11.00000 -1.20000 AFIX 65 C8 1 0.591845 0.666897 0.687712 11.00000 0.12475 0.19691 = 0.19987 0.00441 0.00842 0.08074 C10 1 0.586488 0.708986 0.671891 11.00000 0.11853 0.19041 = 0.19343 0.00339 0.00769 0.08579 AFIX 43 H10 2 0.619178 0.739028 0.662635 11.00000 -1.20000 AFIX 66 C7 1 1.442306 0.944179 0.477554 11.00000 0.26722 0.23101 = 0.18342 0.05771 0.05930 0.12776 C29 1 1.470462 0.950006 0.451346 11.00000 0.26924 0.23156 = 0.18538 0.05832 0.05707 0.12919 AFIX 43 H29 2 1.486131 0.925951 0.447130 11.00000 -1.20000 AFIX 65 C15 1 1.475198 0.991785 0.431442 11.00000 0.26607 0.23548 = 0.18704 0.05730 0.05599 0.12498 AFIX 43 H15 2 1.494036 0.995684 0.413907 11.00000 -1.20000 AFIX 65 C31 1 1.451778 1.027738 0.437744 11.00000 0.26394 0.23334 = 0.18403 0.06335 0.05553 0.12550 C2 1 1.423622 1.021912 0.463951 11.00000 0.26526 0.23320 = 0.18772 0.06234 0.05687 0.12798 AFIX 43 H2 2 1.407952 1.045967 0.468168 11.00000 -1.20000 AFIX 65 C33 1 1.418885 0.980133 0.483856 11.00000 0.26568 0.23660 = 0.18766 0.06017 0.05681 0.12757 AFIX 43 H33 2 1.400047 0.976235 0.501391 11.00000 -1.20000 AFIX 66 C17 1 1.443471 0.898497 0.498017 11.00000 0.26446 0.23205 = 0.18616 0.05324 0.05809 0.13352 C13 1 1.403160 0.878290 0.520573 11.00000 0.26718 0.22894 = 0.18009 0.05588 0.05636 0.12978 AFIX 43 H13 2 1.375955 0.891008 0.522247 11.00000 -1.20000 AFIX 65 C35 1 1.403511 0.839075 0.540625 11.00000 0.26533 0.23059 = 0.18168 0.04746 0.06042 0.12996 C9 1 1.444172 0.820067 0.538122 11.00000 0.26803 0.23523 = 0.18511 0.05040 0.05679 0.12793 AFIX 43 H9 2 1.444407 0.793830 0.551539 11.00000 -1.20000 AFIX 65 C19 1 1.484484 0.840273 0.515567 11.00000 0.26826 0.23211 = 0.18713 0.05776 0.05825 0.12910 AFIX 43 H19 2 1.511689 0.827555 0.513893 11.00000 -1.20000 AFIX 65 C37 1 1.484133 0.879488 0.495515 11.00000 0.27115 0.23639 = 0.18569 0.05472 0.05657 0.12546 AFIX 43 H37 2 1.511104 0.893008 0.480424 11.00000 -1.20000 AFIX 66 C12 1 1.195109 0.703047 0.703934 11.00000 0.14208 0.19505 = 0.19336 0.05334 0.01739 0.11622 AFIX 43 H12 2 1.231594 0.705222 0.703751 11.00000 -1.20000 AFIX 65 N4 3 1.180027 0.729048 0.681932 11.00000 0.13763 0.19376 = 0.18213 0.05710 0.02864 0.10814 C14 1 1.125497 0.725798 0.682205 11.00000 0.14249 0.19755 = 0.20068 0.05117 0.01918 0.11326 AFIX 43 H14 2 1.115406 0.743195 0.667485 11.00000 -1.20000 AFIX 65 C16 1 1.086048 0.696548 0.704480 11.00000 0.13981 0.20131 = 0.20261 0.04909 0.01672 0.11189 C18 1 1.101130 0.670546 0.726483 11.00000 0.14410 0.20249 = 0.19872 0.05304 0.01868 0.10924 AFIX 43 H18 2 1.074736 0.650976 0.741386 11.00000 -1.20000 AFIX 65 C20 1 1.155660 0.673796 0.726210 11.00000 0.14651 0.19825 = 0.19834 0.05245 0.01978 0.10786 AFIX 43 H20 2 1.165750 0.656399 0.740930 11.00000 -1.20000 AFIX 66 C22 1 1.361493 0.820609 0.566051 11.00000 0.26204 0.22883 = 0.17502 0.04867 0.05773 0.12975 C24 1 1.344621 0.858936 0.577466 11.00000 0.26230 0.22980 = 0.17889 0.04559 0.06066 0.12930 AFIX 43 H24 2 1.358769 0.896066 0.569401 11.00000 -1.20000 AFIX 65 C26 1 1.306604 0.841767 0.600935 11.00000 0.26508 0.23230 = 0.17077 0.04626 0.05830 0.12333 AFIX 43 H26 2 1.295316 0.867411 0.608572 11.00000 -1.20000 AFIX 65 N2 3 1.285459 0.786272 0.612989 11.00000 0.25503 0.22264 = 0.16776 0.04322 0.06099 0.13163 C28 1 1.302330 0.747944 0.601575 11.00000 0.25945 0.23002 = 0.17119 0.04369 0.06064 0.12643 AFIX 43 H28 2 1.288182 0.710813 0.609640 11.00000 -1.20000 AFIX 65 C30 1 1.340348 0.765112 0.578106 11.00000 0.26538 0.23130 = 0.17879 0.04357 0.05769 0.12527 AFIX 43 H30 2 1.351636 0.739468 0.570469 11.00000 -1.20000 AFIX 0 C23 1 0.866852 0.693835 0.701056 11.00000 0.14305 0.21872 = 0.22094 0.03106 0.00825 0.09118 C27 1 1.547110 1.167277 0.354899 11.00000 0.23986 0.22069 = 0.17511 0.06123 0.04285 0.11483 AFIX 137 H27A 2 1.582355 1.166064 0.359001 11.00000 -1.50000 H27B 2 1.556530 1.207462 0.352779 11.00000 -1.50000 H27C 2 1.529877 1.146237 0.337347 11.00000 -1.50000 AFIX 66 C32 1 1.500155 1.096180 0.396153 11.00000 0.25369 0.22551 = 0.18027 0.06556 0.05267 0.13227 AFIX 43 H32 2 1.525444 1.081070 0.394689 11.00000 -1.20000 AFIX 65 C34 1 1.506839 1.140955 0.377755 11.00000 0.25704 0.23036 = 0.18120 0.06262 0.04857 0.12240 N3 3 1.469042 1.163538 0.379943 11.00000 0.24270 0.21603 = 0.17768 0.06571 0.04371 0.14083 C36 1 1.424560 1.141345 0.400529 11.00000 0.25303 0.22932 = 0.17949 0.06758 0.04781 0.12554 AFIX 43 H36 2 1.399271 1.156455 0.401992 11.00000 -1.20000 AFIX 65 C38 1 1.417875 1.096569 0.418927 11.00000 0.25784 0.23044 = 0.18564 0.06504 0.05056 0.12845 AFIX 43 H38 2 1.388114 1.081721 0.432700 11.00000 -1.20000 AFIX 65 C40 1 1.455672 1.073986 0.416739 11.00000 0.25912 0.22965 = 0.18558 0.06307 0.05160 0.12861 AFIX 66 C39 1 0.924945 0.643240 0.715236 11.00000 0.14711 0.21881 = 0.21795 0.04264 0.01071 0.09417 AFIX 43 H39 2 0.891316 0.610980 0.722612 11.00000 -1.20000 AFIX 65 C5 1 0.978270 0.643933 0.715444 11.00000 0.14559 0.21328 = 0.21433 0.04980 0.01345 0.10390 AFIX 43 H5 2 0.980318 0.612137 0.722959 11.00000 -1.20000 AFIX 65 C41 1 1.028533 0.692149 0.704420 11.00000 0.14818 0.20734 = 0.20665 0.04881 0.01586 0.10171 C21 1 1.025473 0.739672 0.693188 11.00000 0.14379 0.21123 = 0.20993 0.04893 0.01164 0.10555 AFIX 43 H21 2 1.059103 0.771931 0.685812 11.00000 -1.20000 AFIX 65 C43 1 0.972149 0.738979 0.692980 11.00000 0.14631 0.21363 = 0.21739 0.04278 0.01343 0.10093 AFIX 43 H43 2 0.970102 0.770775 0.685465 11.00000 -1.20000 AFIX 65 C11 1 0.921885 0.690764 0.704004 11.00000 0.14151 0.21412 = 0.21784 0.03651 0.01404 0.10333 AFIX 66 C42 1 0.649859 0.671638 0.693425 11.00000 0.12608 0.19823 = 0.20341 0.00725 0.01403 0.08393 C44 1 0.652701 0.622212 0.701737 11.00000 0.13113 0.20850 = 0.21171 0.01360 0.00750 0.08057 AFIX 43 H44 2 0.618256 0.586861 0.705233 11.00000 -1.20000 AFIX 65 C46 1 0.707024 0.625621 0.704823 11.00000 0.13612 0.21371 = 0.21791 0.01868 0.00622 0.08212 AFIX 43 H46 2 0.708924 0.592551 0.710384 11.00000 -1.20000 AFIX 65 C47 1 0.758505 0.678456 0.699598 11.00000 0.13654 0.21274 = 0.21850 0.01950 0.00545 0.08176 C3 1 0.755665 0.727882 0.691286 11.00000 0.13464 0.21169 = 0.21810 0.01704 0.00602 0.08341 AFIX 43 H3 2 0.790110 0.763233 0.687790 11.00000 -1.20000 AFIX 65 C25 1 0.701342 0.724474 0.688200 11.00000 0.13341 0.20804 = 0.21445 0.01448 0.00332 0.08124 AFIX 43 H25 2 0.699442 0.757544 0.682639 11.00000 -1.20000 AFIX 0 C45 1 0.818443 0.685827 0.702224 11.00000 0.13995 0.21543 = 0.21988 0.02551 0.00611 0.08997 HKLF 4 REM 1_a.res in P-31c REM wR2 = 0.3594, GooF = S = 1.397, Restrained GooF = 1.315 for all data REM R1 = 0.1258 for 3969 Fo > 4sig(Fo) and 0.1399 for all 5238 data REM 374 parameters refined using 1204 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.187, deepest hole -0.343, 1-sigma level 0.079 Q1 1 1.1605 0.7227 0.6828 11.00000 0.05 0.41 Q2 1 0.6868 0.6926 0.6634 11.00000 0.05 0.37 Q3 1 1.3147 0.7477 0.5945 11.00000 0.05 0.35 Q4 1 0.5035 0.6771 0.6764 11.00000 0.05 0.34 Q5 1 0.5742 0.6890 0.6793 11.00000 0.05 0.34 Q6 1 0.5612 0.7004 0.6765 11.00000 0.05 0.34 Q7 1 0.3333 0.6667 0.6791 10.33333 0.05 0.33 Q8 1 0.9642 0.7128 0.7188 11.00000 0.05 0.32 Q9 1 1.4710 1.0950 0.3997 11.00000 0.05 0.32 Q10 1 1.1381 0.6813 0.7228 11.00000 0.05 0.32 Q11 1 0.9741 0.6995 0.7180 11.00000 0.05 0.32 Q12 1 0.7417 0.6878 0.7187 11.00000 0.05 0.32 Q13 1 1.3598 0.8077 0.5578 11.00000 0.05 0.29 Q14 1 1.2947 0.7979 0.5998 11.00000 0.05 0.29 Q15 1 1.4384 0.8750 0.5180 11.00000 0.05 0.28 Q16 1 1.1148 0.7126 0.6909 11.00000 0.05 0.27 Q17 1 1.2206 0.6197 0.7534 11.00000 0.05 0.27 Q18 1 1.2848 0.8188 0.6024 11.00000 0.05 0.26 Q19 1 1.4387 1.0971 0.3942 11.00000 0.05 0.26 Q20 1 0.6638 0.6621 0.6715 11.00000 0.05 0.25 Q21 1 1.0886 0.7140 0.6997 11.00000 0.05 0.25 Q22 1 0.9995 0.7010 0.7213 11.00000 0.05 0.24 Q23 1 0.9398 0.7004 0.6857 11.00000 0.05 0.24 Q24 1 0.6836 0.7442 0.7016 11.00000 0.05 0.24 Q25 1 0.7872 0.6944 0.6781 11.00000 0.05 0.23 Q26 1 1.0208 0.7035 0.7377 11.00000 0.05 0.23 Q27 1 0.6771 0.7092 0.6973 11.00000 0.05 0.23 Q28 1 1.2943 0.8702 0.5931 11.00000 0.05 0.22 Q29 1 1.4556 0.9910 0.4368 11.00000 0.05 0.22 Q30 1 1.4865 1.0145 0.4393 11.00000 0.05 0.22 Q31 1 1.4439 0.9659 0.4402 11.00000 0.05 0.22 Q32 1 0.7706 0.6823 0.6777 11.00000 0.05 0.21 Q33 1 0.5588 0.5332 0.7420 11.00000 0.05 0.21 Q34 1 0.3935 0.6955 0.6613 11.00000 0.05 0.21 Q35 1 0.6834 0.6414 0.6767 11.00000 0.05 0.21 Q36 1 0.9995 0.7163 0.6601 11.00000 0.05 0.20 Q37 1 1.4369 0.9389 0.4411 11.00000 0.05 0.20 Q38 1 1.5441 1.1535 0.3616 11.00000 0.05 0.20 Q39 1 1.3830 0.9234 0.4849 11.00000 0.05 0.20 Q40 1 1.3873 0.7883 0.5369 11.00000 0.05 0.20 Q41 1 1.5477 0.8461 0.5172 11.00000 0.05 0.19 Q42 1 1.5145 0.9975 0.4571 11.00000 0.05 0.19 Q43 1 1.5684 1.1338 0.3282 11.00000 0.05 0.19 Q44 1 1.1102 0.7691 0.6563 11.00000 0.05 0.19 Q45 1 1.3893 0.9088 0.5317 11.00000 0.05 0.19 Q46 1 1.5875 1.1431 0.3370 11.00000 0.05 0.19 Q47 1 1.5156 0.9806 0.4583 11.00000 0.05 0.18 Q48 1 1.5544 1.1204 0.3756 11.00000 0.05 0.18 Q49 1 1.3612 0.9162 0.4972 11.00000 0.05 0.18 Q50 1 0.9511 0.7557 0.7040 11.00000 0.05 0.17 Q51 1 1.3463 0.8635 0.5600 11.00000 0.05 0.17 Q52 1 0.7181 0.6362 0.6787 11.00000 0.05 0.17 Q53 1 0.9061 0.5515 0.6826 11.00000 0.05 0.17 Q54 1 1.5028 0.8161 0.4979 11.00000 0.05 0.17 Q55 1 1.0114 0.7074 0.6635 11.00000 0.05 0.16 Q56 1 0.9024 0.8088 0.7289 11.00000 0.05 0.16 Q57 1 0.6731 0.8090 0.6366 11.00000 0.05 0.16 Q58 1 1.5043 0.7644 0.4407 11.00000 0.05 0.16 Q59 1 1.3150 0.8924 0.5825 11.00000 0.05 0.16 Q60 1 1.3178 1.0027 0.5802 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0.7600 0.7500 10.50000 0.05 0.13 Q83 1 1.3214 0.9818 0.3856 11.00000 0.05 0.13 Q84 1 0.6836 0.8273 0.7206 11.00000 0.05 0.13 Q85 1 1.0841 0.7789 0.6568 11.00000 0.05 0.13 Q86 1 0.9075 0.7869 0.7448 11.00000 0.05 0.12 Q87 1 0.4710 0.5290 0.7500 10.50000 0.05 0.12 Q88 1 1.3653 0.7241 0.5848 11.00000 0.05 0.12 Q89 1 1.3333 0.6667 0.5152 10.33333 0.05 0.12 Q90 1 1.3053 0.9827 0.4087 11.00000 0.05 0.12 Q91 1 1.3953 0.8580 0.4877 11.00000 0.05 0.12 Q92 1 1.3299 1.0720 0.5014 11.00000 0.05 0.12 Q93 1 0.4336 0.5566 0.7185 11.00000 0.05 0.11 Q94 1 1.3060 0.7870 0.4546 11.00000 0.05 0.11 Q95 1 1.5317 0.8595 0.4044 11.00000 0.05 0.11 Q96 1 1.3333 0.6667 0.4267 10.33333 0.05 0.11 Q97 1 0.8676 0.7368 0.7292 11.00000 0.05 0.11 Q98 1 1.2103 1.0355 0.4364 11.00000 0.05 0.11 Q99 1 1.3374 0.9504 0.5416 11.00000 0.05 0.11 Q100 1 1.3446 0.8024 0.4595 11.00000 0.05 0.11 ; _shelx_res_checksum 72723 _shelx_fab_file ; 0 0 2 341.8278 3.0687 0 0 4 -318.7200 6.2278 0 0 6 -287.9969 -5.5160 0 0 8 674.2179 -3.6174 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2.5064 0.0798 15 5 -3 -2.1922 -0.1278 15 5 -2 8.6417 -0.0244 15 5 -1 -7.9918 -0.1626 15 5 0 -0.5973 -0.0511 15 5 1 12.6464 0.2712 15 5 2 5.3376 0.0475 15 5 3 -2.6367 -0.0469 15 5 4 -1.7754 -0.0153 15 5 5 -6.5372 -0.3779 15 5 6 -4.8632 -0.0702 15 5 7 12.3340 0.2552 15 5 8 3.2022 0.0043 15 5 9 -3.3876 0.2972 15 5 10 8.1803 0.2243 15 6 0 17.4957 0.2424 16 0 0 -5.8405 0.1603 16 0 1 17.7663 -0.1269 16 0 2 11.4625 0.0085 16 0 3 -1.1250 -0.0867 16 0 4 3.6767 -0.1270 16 0 5 -9.6929 0.1624 16 0 6 -6.0096 0.0750 16 0 7 -2.0904 0.0195 16 0 8 -4.5568 0.1119 16 0 9 0.6970 -0.2190 16 0 10 -2.1975 -0.1810 16 0 11 1.4142 0.0794 16 0 12 -4.3573 0.0937 16 0 13 8.1072 0.2128 16 0 14 4.3448 0.1523 16 0 15 -9.5466 -0.2143 16 0 16 -0.2475 -0.2596 16 0 17 -5.4329 -0.0442 16 0 18 -4.4012 -0.0888 16 0 19 4.0258 -0.1784 16 1 -18 2.2518 -0.0730 16 1 -17 1.5600 0.1247 16 1 -16 3.0942 -0.0138 16 1 -15 -0.2206 0.3199 16 1 -14 4.7627 -0.1302 16 1 -13 1.1628 -0.2439 16 1 -12 11.1689 -0.0079 16 1 -11 -5.2945 -0.1332 16 1 -10 3.3840 0.1996 16 1 -9 -0.9462 0.3292 16 1 -8 -4.7724 -0.0374 16 1 -7 -1.7089 -0.0611 16 1 -6 8.9717 -0.1388 16 1 -5 0.2912 -0.3274 16 1 -4 7.3185 0.1166 16 1 -3 1.9920 0.2563 16 1 -2 -1.3815 0.0965 16 1 -1 -1.6395 0.1780 16 1 0 5.8560 -0.1578 16 1 1 -2.5818 -0.3764 16 1 2 -12.8452 -0.0059 16 1 3 4.6392 0.0450 16 1 4 2.0243 0.1074 16 1 5 5.2568 0.3861 16 1 6 8.7935 -0.0662 16 1 7 -3.7060 -0.2163 16 1 8 -9.9159 -0.0651 16 1 9 0.5392 -0.2341 16 1 10 -2.3020 0.0682 16 1 11 -0.9098 0.3664 16 1 12 9.3766 0.0871 16 1 13 2.8034 0.0023 16 1 14 7.2302 -0.0678 16 1 15 -4.5826 -0.4371 16 1 16 4.4312 0.0651 16 1 17 1.6820 0.1500 16 1 18 6.2298 -0.1781 16 2 -15 -2.4030 0.0145 16 2 -14 3.1789 -0.3741 16 2 -13 9.3898 0.2225 16 2 -12 -2.3996 -0.0126 16 2 -11 -6.8840 0.1236 16 2 -10 2.8603 0.3179 16 2 -9 -7.5341 -0.3444 16 2 -8 6.9210 -0.3398 16 2 -7 8.1709 0.0273 16 2 -6 -3.4697 -0.2027 16 2 -5 0.7949 0.3116 16 2 -4 6.0783 0.4570 16 2 -3 -5.6073 -0.1489 16 2 -2 4.8274 0.0106 16 2 -1 6.2588 -0.2361 16 2 0 -8.0398 -0.4605 16 2 1 -2.3190 0.2303 16 2 2 4.0467 0.2742 16 2 3 -2.2010 0.1679 16 2 4 -1.8690 0.3877 16 2 5 -4.3894 -0.3146 16 2 6 -10.7908 -0.4599 16 2 7 -10.0822 -0.0419 16 2 8 5.4608 -0.1438 16 2 9 11.3876 0.3565 16 2 10 -2.9208 0.4933 16 2 11 1.8585 -0.1695 16 2 12 -7.6221 -0.1824 16 2 13 -3.1221 -0.1911 16 2 14 2.2361 -0.3655 16 2 15 8.9735 0.1457 16 3 -12 -9.0613 0.1237 16 3 -11 -2.3517 0.2136 16 3 -10 0.0684 0.1365 16 3 -9 1.9460 -0.1544 16 3 -8 -1.4991 -0.0901 16 3 -7 -10.7578 -0.0908 16 3 -6 -3.5956 0.1957 16 3 -5 12.6063 0.2131 16 3 -4 -5.2237 -0.1257 16 3 -3 3.0976 -0.1093 16 3 -2 1.8869 -0.1677 16 3 -1 -1.4891 -0.1789 16 3 0 3.1081 0.1808 16 3 1 6.2865 0.2246 16 3 2 3.3577 0.0904 16 3 3 -3.3435 0.0468 16 3 4 -2.2748 -0.2600 16 3 5 -6.0498 -0.2587 16 3 6 -5.1417 0.0081 16 3 7 5.8360 0.1451 16 3 8 -9.2734 0.2093 16 3 9 0.5464 0.1475 16 3 10 -3.8101 0.0828 16 3 11 -6.5314 -0.1890 16 3 12 -15.7029 -0.1094 16 4 -7 -3.9421 0.0059 16 4 -6 2.4715 0.2367 16 4 -5 -2.0141 0.2950 16 4 -4 -6.3081 -0.4847 16 4 -3 4.8724 -0.1522 16 4 -2 -6.6274 0.0637 16 4 -1 -1.1594 -0.1885 16 4 0 18.8028 0.4249 16 4 1 -0.1608 0.2302 16 4 2 -9.1638 -0.2976 16 4 3 4.4279 0.0919 16 4 4 -3.4576 -0.3093 16 4 5 -0.6093 -0.2418 16 4 6 11.9232 0.4411 16 4 7 4.0584 0.0234 17 0 0 -7.3298 -0.2288 17 0 1 -1.2487 0.1274 17 0 2 -4.4858 0.0452 17 0 3 -5.2596 -0.0022 17 0 4 1.2590 0.1983 17 0 5 -7.1227 -0.0929 17 0 6 -7.8670 -0.2057 17 0 7 2.7791 0.0829 17 0 8 5.2166 -0.0509 17 0 9 0.8312 0.0682 17 0 10 -6.1134 0.1485 17 0 11 1.5578 -0.0933 17 0 12 -1.5864 -0.0206 17 0 13 -9.7674 -0.0286 17 0 14 2.6916 -0.3609 17 0 15 12.6258 0.0280 17 0 16 -2.8066 0.3321 17 1 -13 -5.3918 0.1290 17 1 -12 -9.4278 -0.2313 17 1 -11 0.1853 0.2306 17 1 -10 -3.7672 -0.1332 17 1 -9 0.5309 -0.1595 17 1 -8 6.4337 0.2151 17 1 -7 -9.2061 0.0257 17 1 -6 -3.3110 0.0237 17 1 -5 5.5532 0.1814 17 1 -4 -3.8160 -0.2637 17 1 -3 5.6590 -0.0699 17 1 -2 0.5001 0.0820 17 1 -1 -9.0000 -0.1584 17 1 0 -3.5650 0.2149 17 1 1 11.0810 0.1717 17 1 2 8.5060 -0.2120 17 1 3 -6.3834 0.0239 17 1 4 -0.7925 -0.1016 17 1 5 -8.9076 -0.2593 17 1 6 -7.9868 0.1981 17 1 7 5.2839 -0.0215 17 1 8 -4.6727 0.0084 17 1 9 -6.2999 0.2185 17 1 10 5.4072 -0.1622 17 1 11 1.2423 -0.0925 17 1 12 -8.6270 0.0453 17 1 13 1.0800 -0.2602 17 2 -10 -3.6796 -0.2479 17 2 -9 -6.1747 -0.0591 17 2 -8 -3.6762 -0.0833 17 2 -7 2.4827 -0.0027 17 2 -6 6.6188 0.1624 17 2 -5 -2.3417 -0.1010 17 2 -4 -5.5672 -0.0163 17 2 -3 -6.9796 0.0487 17 2 -2 -10.9795 -0.1247 17 2 -1 -1.6851 0.0921 17 2 0 18.4942 0.0626 17 2 1 3.5762 -0.0579 17 2 2 -11.5417 0.0390 17 2 3 3.7436 -0.0930 17 2 4 -2.2601 -0.0765 17 2 5 1.7060 0.1282 17 2 6 5.3294 0.0568 17 2 7 -0.0085 0.1466 17 2 8 -1.8054 0.0980 17 2 9 4.8412 -0.0345 17 2 10 -1.5207 -0.0876 17 3 -2 -10.0044 0.0451 17 3 -1 16.5766 0.2435 17 3 0 -5.2564 0.2674 17 3 1 -7.9176 -0.3635 17 3 2 5.0137 -0.1424 18 0 0 14.2420 0.1444 18 0 1 -1.0467 -0.0448 18 0 2 -8.4278 -0.0020 18 0 3 -2.8997 -0.0001 18 0 4 2.9208 -0.1115 18 0 5 4.5606 0.0351 18 0 6 3.0434 0.0888 18 0 7 -3.1796 0.0948 18 0 8 -11.7909 0.0999 18 0 9 6.1227 -0.1566 18 0 10 0.5244 -0.0974 18 1 -5 -9.3903 -0.0696 18 1 -4 1.7225 -0.1361 18 1 -3 -3.5386 -0.1380 18 1 -2 3.8129 0.1388 18 1 -1 5.6502 0.1218 18 1 0 -0.6446 0.1295 18 1 1 -10.0864 0.0883 18 1 2 0.9972 -0.1840 18 1 3 1.0864 -0.1296 18 1 4 3.0178 -0.0421 18 1 5 3.0288 0.0441 0 0 0 0.0 0.0 ; _shelx_fab_checksum 75601 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, 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 1.23209(4) 0.75987(4) 0.64610(2) 0.1349(7) Uani 1 1 d . U . . . N1 N 0.5323(4) 0.7062(4) 0.66991(18) 0.158(3) Uani 1 1 d G U . . . C1 C 0.4834(3) 0.6613(4) 0.6837(2) 0.159(3) Uani 1 1 d G U . . . H1 H 0.447137 0.659388 0.682411 0.191 Uiso 1 1 calc R U . . . C4 C 0.4888(3) 0.6192(4) 0.69956(19) 0.161(3) Uani 1 1 d G U . . . H4 H 0.456079 0.589139 0.708817 0.194 Uiso 1 1 calc R U . . . C6 C 0.5430(4) 0.6220(4) 0.7015(2) 0.166(3) Uani 1 1 d G U . . . H6 H 0.546570 0.593835 0.712132 0.199 Uiso 1 1 calc R U . . . C8 C 0.5918(3) 0.6669(4) 0.6877(2) 0.174(3) Uani 1 1 d G U . . . C10 C 0.5865(3) 0.7090(4) 0.6719(2) 0.164(3) Uani 1 1 d G U . . . H10 H 0.619178 0.739028 0.662635 0.196 Uiso 1 1 calc R U . . . C7 C 1.4423(6) 0.9442(5) 0.4776(2) 0.226(3) Uani 1 1 d DG U . . . C29 C 1.4705(5) 0.9500(4) 0.4513(3) 0.227(3) Uani 1 1 d G U . . . H29 H 1.486131 0.925951 0.447130 0.272 Uiso 1 1 calc R U . . . C15 C 1.4752(5) 0.9918(4) 0.4314(2) 0.230(3) Uani 1 1 d G U . . . H15 H 1.494036 0.995684 0.413907 0.276 Uiso 1 1 calc DR U . . . C31 C 1.4518(6) 1.0277(5) 0.4377(2) 0.227(3) Uani 1 1 d DG U . . . C2 C 1.4236(6) 1.0219(5) 0.4640(3) 0.227(3) Uani 1 1 d G U . . . H2 H 1.407952 1.045967 0.468168 0.273 Uiso 1 1 calc R U . . . C33 C 1.4189(5) 0.9801(5) 0.4839(2) 0.229(3) Uani 1 1 d G U . . . H33 H 1.400047 0.976235 0.501391 0.275 Uiso 1 1 calc R U . . . C17 C 1.4435(6) 0.8985(5) 0.4980(2) 0.223(3) Uani 1 1 d DG U . . . C13 C 1.4032(5) 0.8783(6) 0.5206(3) 0.223(3) Uani 1 1 d G U . . . H13 H 1.375955 0.891008 0.522247 0.267 Uiso 1 1 calc R U . . . C35 C 1.4035(5) 0.8391(6) 0.5406(2) 0.223(3) Uani 1 1 d G U . . . C9 C 1.4442(6) 0.8201(5) 0.5381(2) 0.229(3) Uani 1 1 d G U . . . H9 H 1.444407 0.793830 0.551539 0.274 Uiso 1 1 calc R U . . . C19 C 1.4845(5) 0.8403(6) 0.5156(3) 0.227(4) Uani 1 1 d G U . . . H19 H 1.511689 0.827555 0.513893 0.273 Uiso 1 1 calc R U . . . C37 C 1.4841(5) 0.8795(5) 0.4955(2) 0.232(4) Uani 1 1 d G U . . . H37 H 1.511104 0.893008 0.480424 0.278 Uiso 1 1 calc R U . . . C12 C 1.1951(3) 0.7030(4) 0.7039(2) 0.163(3) Uani 1 1 d G U . . . H12 H 1.231594 0.705222 0.703751 0.195 Uiso 1 1 calc R U . . . N4 N 1.1800(3) 0.7290(4) 0.68193(17) 0.160(2) Uani 1 1 d G U . . . C14 C 1.1255(4) 0.7258(4) 0.68221(18) 0.168(3) Uani 1 1 d G U . . . H14 H 1.115406 0.743195 0.667485 0.201 Uiso 1 1 calc R U . . . C16 C 1.0860(3) 0.6965(5) 0.7045(2) 0.169(3) Uani 1 1 d G U . . . C18 C 1.1011(4) 0.6705(4) 0.72648(19) 0.172(3) Uani 1 1 d G U . . . H18 H 1.074736 0.650976 0.741386 0.206 Uiso 1 1 calc R U . . . C20 C 1.1557(4) 0.6738(4) 0.72621(18) 0.171(3) Uani 1 1 d G U . . . H20 H 1.165750 0.656399 0.740930 0.206 Uiso 1 1 calc R U . . . C22 C 1.3615(5) 0.8206(6) 0.5661(2) 0.219(3) Uani 1 1 d G U . . . C24 C 1.3446(5) 0.8589(5) 0.5775(3) 0.221(3) Uani 1 1 d G U . . . H24 H 1.358769 0.896066 0.569401 0.265 Uiso 1 1 calc R U . . . C26 C 1.3066(5) 0.8418(5) 0.6009(2) 0.223(4) Uani 1 1 d G U . . . H26 H 1.295316 0.867411 0.608572 0.268 Uiso 1 1 calc R U . . . N2 N 1.2855(5) 0.7863(6) 0.61299(19) 0.210(3) Uani 1 1 d G U . . . C28 C 1.3023(5) 0.7479(4) 0.6016(2) 0.218(4) Uani 1 1 d G U . . . H28 H 1.288182 0.710813 0.609640 0.262 Uiso 1 1 calc R U . . . C30 C 1.3403(6) 0.7651(5) 0.5781(3) 0.225(3) Uani 1 1 d G U . . . H30 H 1.351636 0.739468 0.570469 0.270 Uiso 1 1 calc R U . . . C23 C 0.8669(5) 0.6938(7) 0.7011(4) 0.194(3) Uani 1 1 d D U . . . C27 C 1.5471(8) 1.1673(7) 0.3549(3) 0.212(5) Uani 1 1 d . U . . . H27A H 1.582355 1.166064 0.359001 0.318 Uiso 1 1 calc R U . . . H27B H 1.556530 1.207462 0.352779 0.318 Uiso 1 1 calc R U . . . H27C H 1.529877 1.146237 0.337347 0.318 Uiso 1 1 calc R U . . . C32 C 1.5002(5) 1.0962(5) 0.3962(3) 0.214(3) Uani 1 1 d G U . . . H32 H 1.525444 1.081070 0.394689 0.257 Uiso 1 1 calc DR U . . . C34 C 1.5068(5) 1.1410(5) 0.3778(2) 0.223(4) Uani 1 1 d G U . . . N3 N 1.4690(5) 1.1635(4) 0.3799(2) 0.201(3) Uani 1 1 d G U . . . C36 C 1.4246(5) 1.1413(5) 0.4005(3) 0.218(4) Uani 1 1 d G U . . . H36 H 1.399271 1.156455 0.401992 0.262 Uiso 1 1 calc R U . . . C38 C 1.4179(5) 1.0966(5) 0.4189(2) 0.222(3) Uani 1 1 d G U . . . H38 H 1.388114 1.081721 0.432700 0.266 Uiso 1 1 calc R U . . . C40 C 1.4557(6) 1.0740(4) 0.4167(2) 0.222(3) Uani 1 1 d DG U . . . C39 C 0.9249(4) 0.6432(4) 0.7152(2) 0.193(3) Uani 1 1 d G U . . . H39 H 0.891316 0.610980 0.722612 0.232 Uiso 1 1 calc R U . . . C5 C 0.9783(5) 0.6439(4) 0.7154(2) 0.185(3) Uani 1 1 d G U . . . H5 H 0.980318 0.612137 0.722959 0.222 Uiso 1 1 calc R U . . . C41 C 1.0285(4) 0.6921(5) 0.7044(3) 0.182(3) Uani 1 1 d G U . . . C21 C 1.0255(4) 0.7397(4) 0.6932(3) 0.181(3) Uani 1 1 d G U . . . H21 H 1.059103 0.771931 0.685812 0.217 Uiso 1 1 calc R U . . . C43 C 0.9721(5) 0.7390(4) 0.6930(3) 0.188(3) Uani 1 1 d G U . . . H43 H 0.970102 0.770775 0.685465 0.225 Uiso 1 1 calc R U . . . C11 C 0.9219(4) 0.6908(5) 0.7040(3) 0.185(3) Uani 1 1 d DG U . . . C42 C 0.6499(3) 0.6716(5) 0.6934(2) 0.175(3) Uani 1 1 d G U . . . C44 C 0.6527(4) 0.6222(4) 0.7017(2) 0.186(3) Uani 1 1 d G U . . . H44 H 0.618256 0.586861 0.705233 0.223 Uiso 1 1 calc R U . . . C46 C 0.7070(5) 0.6256(4) 0.7048(2) 0.192(3) Uani 1 1 d G U . . . H46 H 0.708924 0.592551 0.710384 0.230 Uiso 1 1 calc R U . . . C47 C 0.7585(3) 0.6785(5) 0.6996(3) 0.192(3) Uani 1 1 d DG U . . . C3 C 0.7557(4) 0.7279(4) 0.6913(3) 0.190(3) Uani 1 1 d G U . . . H3 H 0.790110 0.763233 0.687790 0.227 Uiso 1 1 calc R U . . . C25 C 0.7013(5) 0.7245(4) 0.6882(2) 0.187(3) Uani 1 1 d G U . . . H25 H 0.699442 0.757544 0.682639 0.225 Uiso 1 1 calc R U . . . C45 C 0.8184(5) 0.6858(7) 0.7022(4) 0.191(3) Uani 1 1 d D 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 0.1657(11) 0.1476(10) 0.1234(11) 0.0070(6) -0.0014(6) 0.1024(8) N1 0.115(4) 0.185(5) 0.183(5) -0.007(4) 0.017(4) 0.082(4) C1 0.114(5) 0.186(6) 0.187(6) -0.003(5) 0.012(5) 0.081(5) C4 0.116(4) 0.187(5) 0.190(5) -0.002(5) 0.012(4) 0.082(4) C6 0.122(4) 0.190(5) 0.194(5) 0.004(4) 0.006(4) 0.084(4) C8 0.125(4) 0.197(5) 0.200(5) 0.004(4) 0.008(4) 0.081(4) C10 0.119(4) 0.190(5) 0.193(5) 0.003(4) 0.008(4) 0.086(4) C7 0.267(6) 0.231(5) 0.183(5) 0.058(4) 0.059(4) 0.128(5) C29 0.269(6) 0.232(6) 0.185(5) 0.058(4) 0.057(5) 0.129(5) C15 0.266(6) 0.235(5) 0.187(5) 0.057(4) 0.056(5) 0.125(5) C31 0.264(6) 0.233(5) 0.184(5) 0.063(4) 0.056(5) 0.126(5) C2 0.265(6) 0.233(6) 0.188(5) 0.062(5) 0.057(5) 0.128(5) C33 0.266(6) 0.237(6) 0.188(5) 0.060(4) 0.057(5) 0.128(5) C17 0.264(5) 0.232(5) 0.186(5) 0.053(4) 0.058(4) 0.134(5) C13 0.267(5) 0.229(5) 0.180(5) 0.056(4) 0.056(4) 0.130(5) C35 0.265(6) 0.231(5) 0.182(5) 0.047(4) 0.060(4) 0.130(5) C9 0.268(6) 0.235(6) 0.185(5) 0.050(5) 0.057(5) 0.128(5) C19 0.268(6) 0.232(6) 0.187(6) 0.058(5) 0.058(5) 0.129(6) C37 0.271(6) 0.236(6) 0.186(5) 0.055(5) 0.057(5) 0.125(5) C12 0.142(5) 0.195(5) 0.193(6) 0.053(5) 0.017(5) 0.116(4) N4 0.138(4) 0.194(5) 0.182(4) 0.057(4) 0.029(3) 0.108(4) C14 0.142(4) 0.198(5) 0.201(5) 0.051(4) 0.019(4) 0.113(4) C16 0.140(4) 0.201(5) 0.203(5) 0.049(4) 0.017(4) 0.112(4) C18 0.144(4) 0.202(5) 0.199(5) 0.053(4) 0.019(4) 0.109(4) C20 0.147(5) 0.198(5) 0.198(5) 0.052(5) 0.020(4) 0.108(4) C22 0.262(6) 0.229(6) 0.175(5) 0.049(5) 0.058(4) 0.130(5) C24 0.262(6) 0.230(6) 0.179(5) 0.046(5) 0.061(4) 0.129(5) C26 0.265(7) 0.232(6) 0.171(6) 0.046(5) 0.058(5) 0.123(6) N2 0.255(6) 0.223(6) 0.168(5) 0.043(5) 0.061(3) 0.132(5) C28 0.259(6) 0.230(6) 0.171(6) 0.044(5) 0.061(5) 0.126(5) C30 0.265(6) 0.231(6) 0.179(5) 0.044(5) 0.058(4) 0.125(5) C23 0.143(4) 0.219(5) 0.221(5) 0.031(4) 0.008(4) 0.091(4) C27 0.240(9) 0.221(8) 0.175(8) 0.061(7) 0.043(7) 0.115(8) C32 0.254(6) 0.226(6) 0.180(5) 0.066(5) 0.053(5) 0.132(5) C34 0.257(6) 0.230(6) 0.181(6) 0.063(5) 0.049(5) 0.122(5) N3 0.243(6) 0.216(6) 0.178(6) 0.066(5) 0.044(5) 0.141(5) C36 0.253(6) 0.229(6) 0.179(6) 0.068(5) 0.048(5) 0.126(6) C38 0.258(6) 0.230(6) 0.186(5) 0.065(5) 0.051(5) 0.128(5) C40 0.259(6) 0.230(6) 0.186(5) 0.063(4) 0.052(5) 0.129(5) C39 0.147(4) 0.219(5) 0.218(5) 0.043(4) 0.011(4) 0.094(4) C5 0.146(4) 0.213(5) 0.214(5) 0.050(4) 0.013(4) 0.104(4) C41 0.148(4) 0.207(5) 0.207(5) 0.049(4) 0.016(4) 0.102(4) C21 0.144(4) 0.211(5) 0.210(5) 0.049(4) 0.012(4) 0.106(4) C43 0.146(4) 0.214(5) 0.217(5) 0.043(4) 0.013(4) 0.101(4) C11 0.142(5) 0.214(5) 0.218(5) 0.037(5) 0.014(4) 0.103(4) C42 0.126(4) 0.198(5) 0.203(5) 0.007(4) 0.014(4) 0.084(4) C44 0.131(4) 0.209(5) 0.212(5) 0.014(4) 0.008(4) 0.081(4) C46 0.136(4) 0.214(5) 0.218(5) 0.019(4) 0.006(4) 0.082(4) C47 0.137(4) 0.213(5) 0.218(5) 0.020(5) 0.005(4) 0.082(4) C3 0.135(4) 0.212(5) 0.218(5) 0.017(4) 0.006(4) 0.083(4) C25 0.133(4) 0.208(5) 0.214(5) 0.014(4) 0.003(4) 0.081(4) C45 0.140(4) 0.215(5) 0.220(5) 0.026(4) 0.006(4) 0.090(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0019 0.0015 '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 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -1.2476 0.9534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N4 89.2(4) 2_765 . ? N1 Pd1 N3 175(2) 2_765 8_566 ? N4 Pd1 N3 91(3) . 8_566 ? N2 Pd1 N1 90.0(4) . 2_765 ? N2 Pd1 N4 175.3(4) . . ? N2 Pd1 N3 90(3) . 8_566 ? C1 N1 Pd1 122.4(5) . 3_675 ? C1 N1 C10 120.0 . . ? C10 N1 Pd1 117.6(5) . 3_675 ? N1 C1 H1 120.0 . . ? C4 C1 N1 120.0 . . ? C4 C1 H1 120.0 . . ? C1 C4 H4 120.0 . . ? C1 C4 C6 120.0 . . ? C6 C4 H4 120.0 . . ? C4 C6 H6 120.0 . . ? C8 C6 C4 120.0 . . ? C8 C6 H6 120.0 . . ? C6 C8 C42 117.4(8) . . ? C10 C8 C6 120.0 . . ? C10 C8 C42 122.2(8) . . ? N1 C10 H10 120.0 . . ? C8 C10 N1 120.0 . . ? C8 C10 H10 120.0 . . ? C29 C7 C33 120.0 . . ? C29 C7 C17 114.1(9) . . ? C33 C7 C17 125.9(9) . . ? C7 C29 H29 120.0 . . ? C15 C29 C7 120.0 . . ? C15 C29 H29 120.0 . . ? C29 C15 H15 120.0 . . ? C29 C15 C31 120.0 . . ? C31 C15 H15 120.0 . . ? C15 C31 C2 120.0 . . ? C15 C31 C40 122.1(10) . . ? C2 C31 C40 117.9(10) . . ? C31 C2 H2 120.0 . . ? C33 C2 C31 120.0 . . ? C33 C2 H2 120.0 . . ? C7 C33 H33 120.0 . . ? C2 C33 C7 120.0 . . ? C2 C33 H33 120.0 . . ? C13 C17 C7 116.9(10) . . ? C13 C17 C37 120.0 . . ? C37 C17 C7 123.0(10) . . ? C17 C13 H13 120.0 . . ? C35 C13 C17 120.0 . . ? C35 C13 H13 120.0 . . ? C13 C35 C9 120.0 . . ? C13 C35 C22 118.9(11) . . ? C9 C35 C22 121.0(11) . . ? C35 C9 H9 120.0 . . ? C19 C9 C35 120.0 . . ? C19 C9 H9 120.0 . . ? C9 C19 H19 120.0 . . ? C9 C19 C37 120.0 . . ? C37 C19 H19 120.0 . . ? C17 C37 H37 120.0 . . ? C19 C37 C17 120.0 . . ? C19 C37 H37 120.0 . . ? N4 C12 H12 120.0 . . ? N4 C12 C20 120.0 . . ? C20 C12 H12 120.0 . . ? C12 N4 Pd1 119.5(5) . . ? C14 N4 Pd1 119.7(5) . . ? C14 N4 C12 120.0 . . ? N4 C14 H14 120.0 . . ? N4 C14 C16 120.0 . . ? C16 C14 H14 120.0 . . ? C14 C16 C41 119.9(7) . . ? C18 C16 C14 120.0 . . ? C18 C16 C41 120.1(7) . . ? C16 C18 H18 120.0 . . ? C20 C18 C16 120.0 . . ? C20 C18 H18 120.0 . . ? C12 C20 H20 120.0 . . ? C18 C20 C12 120.0 . . ? C18 C20 H20 120.0 . . ? C24 C22 C35 120.5(10) . . ? C24 C22 C30 120.0 . . ? C30 C22 C35 119.5(10) . . ? C22 C24 H24 120.0 . . ? C26 C24 C22 120.0 . . ? C26 C24 H24 120.0 . . ? C24 C26 H26 120.0 . . ? C24 C26 N2 120.0 . . ? N2 C26 H26 120.0 . . ? C26 N2 Pd1 121.8(7) . . ? C28 N2 Pd1 118.2(7) . . ? C28 N2 C26 120.0 . . ? N2 C28 H28 120.0 . . ? N2 C28 C30 120.0 . . ? C30 C28 H28 120.0 . . ? C22 C30 H30 120.0 . . ? C28 C30 C22 120.0 . . ? C28 C30 H30 120.0 . . ? C45 C23 C11 166.0(17) . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C34 C27 H27A 109.5 . . ? C34 C27 H27B 109.5 . . ? C34 C27 H27C 109.5 . . ? C34 C32 H32 120.0 . . ? C34 C32 C40 120.0 . . ? C40 C32 H32 120.0 . . ? C32 C34 C27 128.5(11) . . ? C32 C34 N3 120.0 . . ? N3 C34 C27 111.5(11) . . ? C34 N3 Pd1 125.6(6) . 9_656 ? C36 N3 Pd1 114.4(7) . 9_656 ? C36 N3 C34 120.0 . . ? N3 C36 H36 120.0 . . ? N3 C36 C38 120.0 . . ? C38 C36 H36 120.0 . . ? C36 C38 H38 120.0 . . ? C40 C38 C36 120.0 . . ? C40 C38 H38 120.0 . . ? C32 C40 C31 118.8(10) . . ? C38 C40 C31 121.1(10) . . ? C38 C40 C32 120.0 . . ? C5 C39 H39 120.0 . . ? C5 C39 C11 120.0 . . ? C11 C39 H39 120.0 . . ? C39 C5 H5 120.0 . . ? C41 C5 C39 120.0 . . ? C41 C5 H5 120.0 . . ? C5 C41 C16 123.1(8) . . ? C5 C41 C21 120.0 . . ? C21 C41 C16 116.9(8) . . ? C41 C21 H21 120.0 . . ? C43 C21 C41 120.0 . . ? C43 C21 H21 120.0 . . ? C21 C43 H43 120.0 . . ? C21 C43 C11 120.0 . . ? C11 C43 H43 120.0 . . ? C39 C11 C23 125.0(10) . . ? C43 C11 C23 114.9(9) . . ? C43 C11 C39 120.0 . . ? C44 C42 C8 120.1(8) . . ? C44 C42 C25 120.0 . . ? C25 C42 C8 119.7(8) . . ? C42 C44 H44 120.0 . . ? C46 C44 C42 120.0 . . ? C46 C44 H44 120.0 . . ? C44 C46 H46 120.0 . . ? C47 C46 C44 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C3 120.0 . . ? C46 C47 C45 123.5(10) . . ? C3 C47 C45 116.5(10) . . ? C47 C3 H3 120.0 . . ? C25 C3 C47 120.0 . . ? C25 C3 H3 120.0 . . ? C42 C25 H25 120.0 . . ? C3 C25 C42 120.0 . . ? C3 C25 H25 120.0 . . ? C23 C45 C47 172.3(18) . . ? 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 2.011(7) 2_765 ? Pd1 N4 2.043(7) . ? Pd1 N2 1.956(8) . ? Pd1 N3 2.13(5) 8_566 ? N1 C1 1.3900 . ? N1 C10 1.3900 . ? C1 H1 0.9300 . ? C1 C4 1.3900 . ? C4 H4 0.9300 . ? C4 C6 1.3900 . ? C6 H6 0.9300 . ? C6 C8 1.3900 . ? C8 C10 1.3900 . ? C8 C42 1.488(9) . ? C10 H10 0.9300 . ? C7 C29 1.3900 . ? C7 C33 1.3900 . ? C7 C17 1.541(8) . ? C29 H29 0.9300 . ? C29 C15 1.3900 . ? C15 H15 0.9300 . ? C15 C31 1.3900 . ? C31 C2 1.3900 . ? C31 C40 1.519(6) . ? C2 H2 0.9300 . ? C2 C33 1.3900 . ? C33 H33 0.9300 . ? C17 C13 1.3900 . ? C17 C37 1.3900 . ? C13 H13 0.9300 . ? C13 C35 1.3900 . ? C35 C9 1.3900 . ? C35 C22 1.518(11) . ? C9 H9 0.9300 . ? C9 C19 1.3900 . ? C19 H19 0.9300 . ? C19 C37 1.3900 . ? C37 H37 0.9300 . ? C12 H12 0.9300 . ? C12 N4 1.3900 . ? C12 C20 1.3900 . ? N4 C14 1.3900 . ? C14 H14 0.9300 . ? C14 C16 1.3900 . ? C16 C18 1.3900 . ? C16 C41 1.455(8) . ? C18 H18 0.9300 . ? C18 C20 1.3900 . ? C20 H20 0.9300 . ? C22 C24 1.3900 . ? C22 C30 1.3900 . ? C24 H24 0.9300 . ? C24 C26 1.3900 . ? C26 H26 0.9300 . ? C26 N2 1.3900 . ? N2 C28 1.3900 . ? C28 H28 0.9300 . ? C28 C30 1.3900 . ? C30 H30 0.9300 . ? C23 C11 1.492(8) . ? C23 C45 1.180(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 C34 1.409(16) . ? C32 H32 0.9300 . ? C32 C34 1.3900 . ? C32 C40 1.3900 . ? C34 N3 1.3900 . ? N3 C36 1.3900 . ? C36 H36 0.9300 . ? C36 C38 1.3900 . ? C38 H38 0.9300 . ? C38 C40 1.3900 . ? C39 H39 0.9300 . ? C39 C5 1.3900 . ? C39 C11 1.3900 . ? C5 H5 0.9300 . ? C5 C41 1.3900 . ? C41 C21 1.3900 . ? C21 H21 0.9300 . ? C21 C43 1.3900 . ? C43 H43 0.9300 . ? C43 C11 1.3900 . ? C42 C44 1.3900 . ? C42 C25 1.3900 . ? C44 H44 0.9300 . ? C44 C46 1.3900 . ? C46 H46 0.9300 . ? C46 C47 1.3900 . ? C47 C3 1.3900 . ? C47 C45 1.490(8) . ? C3 H3 0.9300 . ? C3 C25 1.3900 . ? C25 H25 0.9300 . ? 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 C4 179.0(6) 3_675 . . . ? Pd1 N1 C10 C8 -179.0(6) 3_675 . . . ? Pd1 N4 C14 C16 169.9(6) . . . . ? Pd1 N2 C28 C30 -179.8(8) . . . . ? Pd1 N3 C36 C38 -179.9(8) 9_656 . . . ? N1 C1 C4 C6 0.0 . . . . ? C1 N1 C10 C8 0.0 . . . . ? C1 C4 C6 C8 0.0 . . . . ? C4 C6 C8 C10 0.0 . . . . ? C4 C6 C8 C42 173.0(9) . . . . ? C6 C8 C10 N1 0.0 . . . . ? C6 C8 C42 C44 25.7(10) . . . . ? C6 C8 C42 C25 -159.4(6) . . . . ? C8 C42 C44 C46 174.8(10) . . . . ? C8 C42 C25 C3 -174.9(10) . . . . ? C10 N1 C1 C4 0.0 . . . . ? C10 C8 C42 C44 -161.4(6) . . . . ? C10 C8 C42 C25 13.4(10) . . . . ? C7 C29 C15 C31 0.0 . . . . ? C7 C17 C13 C35 -177.1(11) . . . . ? C7 C17 C37 C19 176.9(12) . . . . ? C29 C7 C33 C2 0.0 . . . . ? C29 C7 C17 C13 -162.4(7) . . . . ? C29 C7 C17 C37 20.6(12) . . . . ? C29 C15 C31 C2 0.0 . . . . ? C29 C15 C31 C40 -179.9(13) . . . . ? C15 C31 C2 C33 0.0 . . . . ? C15 C31 C40 C32 -23.8(13) . . . . ? C15 C31 C40 C38 160.0(8) . . . . ? C31 C2 C33 C7 0.0 . . . . ? C2 C31 C40 C32 156.3(7) . . . . ? C2 C31 C40 C38 -19.9(12) . . . . ? C33 C7 C29 C15 0.0 . . . . ? C33 C7 C17 C13 21.0(14) . . . . ? C33 C7 C17 C37 -156.0(8) . . . . ? C17 C7 C29 C15 -176.8(12) . . . . ? C17 C7 C33 C2 176.4(13) . . . . ? C17 C13 C35 C9 0.0 . . . . ? C17 C13 C35 C22 176.3(12) . . . . ? C13 C17 C37 C19 0.0 . . . . ? C13 C35 C9 C19 0.0 . . . . ? C13 C35 C22 C24 -30.7(13) . . . . ? C13 C35 C22 C30 149.9(7) . . . . ? C35 C9 C19 C37 0.0 . . . . ? C35 C22 C24 C26 -179.3(12) . . . . ? C35 C22 C30 C28 179.3(12) . . . . ? C9 C35 C22 C24 145.5(8) . . . . ? C9 C35 C22 C30 -33.8(12) . . . . ? C9 C19 C37 C17 0.0 . . . . ? C37 C17 C13 C35 0.0 . . . . ? C12 N4 C14 C16 0.0 . . . . ? N4 C12 C20 C18 0.0 . . . . ? N4 C14 C16 C18 0.0 . . . . ? N4 C14 C16 C41 -178.7(10) . . . . ? C14 C16 C18 C20 0.0 . . . . ? C14 C16 C41 C5 147.0(7) . . . . ? C14 C16 C41 C21 -34.3(10) . . . . ? C16 C18 C20 C12 0.0 . . . . ? C16 C41 C21 C43 -178.7(11) . . . . ? C18 C16 C41 C5 -31.8(12) . . . . ? C18 C16 C41 C21 146.9(6) . . . . ? C20 C12 N4 Pd1 -169.9(6) . . . . ? C20 C12 N4 C14 0.0 . . . . ? C22 C35 C9 C19 -176.2(12) . . . . ? C22 C24 C26 N2 0.0 . . . . ? C24 C22 C30 C28 0.0 . . . . ? C24 C26 N2 Pd1 179.8(8) . . . . ? C24 C26 N2 C28 0.0 . . . . ? C26 N2 C28 C30 0.0 . . . . ? N2 C28 C30 C22 0.0 . . . . ? C30 C22 C24 C26 0.0 . . . . ? C27 C34 N3 Pd1 -2.7(13) . . . 9_656 ? C27 C34 N3 C36 177.4(13) . . . . ? C32 C34 N3 Pd1 179.8(8) . . . 9_656 ? C32 C34 N3 C36 0.0 . . . . ? C34 C32 C40 C31 -176.3(11) . . . . ? C34 C32 C40 C38 0.0 . . . . ? C34 N3 C36 C38 0.0 . . . . ? N3 C36 C38 C40 0.0 . . . . ? C36 C38 C40 C31 176.2(11) . . . . ? C36 C38 C40 C32 0.0 . . . . ? C40 C31 C2 C33 179.9(12) . . . . ? C40 C32 C34 C27 -177.0(15) . . . . ? C40 C32 C34 N3 0.0 . . . . ? C39 C5 C41 C16 178.6(11) . . . . ? C39 C5 C41 C21 0.0 . . . . ? C5 C39 C11 C23 176.4(14) . . . . ? C5 C39 C11 C43 0.0 . . . . ? C5 C41 C21 C43 0.0 . . . . ? C41 C16 C18 C20 178.7(10) . . . . ? C41 C21 C43 C11 0.0 . . . . ? C21 C43 C11 C23 -176.7(12) . . . . ? C21 C43 C11 C39 0.0 . . . . ? C11 C39 C5 C41 0.0 . . . . ? C42 C8 C10 N1 -172.7(9) . . . . ? C42 C44 C46 C47 0.0 . . . . ? C44 C42 C25 C3 0.0 . . . . ? C44 C46 C47 C3 0.0 . . . . ? C44 C46 C47 C45 -179.6(13) . . . . ? C46 C47 C3 C25 0.0 . . . . ? C47 C3 C25 C42 0.0 . . . . ? C25 C42 C44 C46 0.0 . . . . ? C45 C23 C11 C39 11(9) . . . . ? C45 C23 C11 C43 -173(8) . . . . ? C45 C47 C3 C25 179.6(12) . . . . ? 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 -0.044 -0.341 -0.355 18342.3 5206.5 ? 2 0.333 0.667 0.750 240.7 254.8 ? 3 0.667 0.333 0.250 240.7 254.8 ?