#------------------------------------------------------------------------------ #$Date: 2024-10-05 15:36:14 +0300 (Sat, 05 Oct 2024) $ #$Revision: 295073 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160168.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_7160168 loop_ _publ_author_name 'Mandal, Subham' 'Sarkar, Piyali' 'Ghosh, Pradyut' _publ_section_title ; A macrocycle-based new organometallic nano-vessel towards sustainable C2-selective arylation of free indole in water. ; _journal_issue 36 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 7438 _journal_page_last 7447 _journal_paper_doi 10.1039/d4ob00886c _journal_volume 22 _journal_year 2024 _chemical_formula_moiety 'C28 H35 Cl N3 O4 Pd, Cl, C2 H6 O S' _chemical_formula_sum 'C30 H41 Cl2 N3 O5 Pd S' _chemical_formula_weight 733.02 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-06-25 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-06-25 deposited with the CCDC. 2024-08-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.747(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.576(3) _cell_length_b 38.304(13) _cell_length_c 10.469(4) _cell_measurement_reflns_used 9583 _cell_measurement_temperature 140.02 _cell_measurement_theta_max 25.44 _cell_measurement_theta_min 2.32 _cell_volume 3237(2) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 140.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_unetI/netI 0.0932 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 23410 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 2.324 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_T_max 0.7076 _exptl_absorpt_correction_T_min 0.4089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1692 before and 0.1269 after correction. The Ratio of minimum to maximum transmission is 0.5779. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.504 _exptl_crystal_description irregular _exptl_crystal_F_000 1512 _exptl_crystal_recrystallization_method 'Vapour deposition' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _refine_diff_density_max 1.273 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.200 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 381 _refine_ls_number_reflns 5684 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0933 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1458P)^2^+13.6780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2378 _refine_ls_wR_factor_ref 0.2494 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4705 _reflns_number_total 5684 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob00886c2.cif _cod_data_source_block mo_pg210623_0m_a _cod_original_cell_volume 3236.7(19) _cod_database_code 7160168 _shelx_shelxl_version_number 2016/6 _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 0.729 _shelx_estimated_absorpt_t_min 0.631 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C8, C7, C29, S2, C30 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints C29 \\sim S2 \\sim C30 \\sim C8 \\sim C7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4.a Ternary CH refined with riding coordinates: N3(H3), N2(H2), N1(H1) 4.b Secondary CH2 refined with riding coordinates: C28(H28A,H28B), C25(H25A,H25B), C27(H27A,H27B), C23(H23A,H23B), C26(H26A, H26B), C10(H10A,H10B), C24(H24A,H24B), C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B) 4.c Aromatic/amide H refined with riding coordinates: C19(H19), C5(H5), C15(H15), C18(H18), C16(H16), C4(H4), C22(H22), C21(H21), C2(H2A), C12(H12), C3(H3A), C13(H13) 4.d Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C29(H29A,H29B,H29C) ; _shelx_res_file ; TITL mo_PG210623_0m_a.res in P2(1)/n mo_pg210623_0m_a.res created by SHELXL-2016/6 at 18:01:38 on 25-Jun-2023 REM Old TITL mo_PG210623_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.139, Rweak 0.021, Alpha 0.059, Orientation as input REM Formula found by SHELXT: C30 Cl2 N2 O6 Pd S CELL 0.71073 8.5759 38.3038 10.4689 90 109.747 90 ZERR 4 0.0028 0.0125 0.0035 0 0.01 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N O Pd S UNIT 120 164 8 12 20 4 4 DELU C8 C7 C29 S2 C30 SIMU C29 S2 C30 C8 C7 L.S. 10 PLAN 2 SIZE 0.5 0.6 0.4 TEMP -133.13 CONF MORE -1 fmap 2 ACTA BOND $H REM REM REM WGHT 0.145800 13.678000 FVAR 0.40431 PD1 6 0.114981 0.440927 0.144965 11.00000 0.02378 0.02766 = 0.02493 -0.00256 0.00580 -0.00159 CL2 3 0.202550 0.476213 0.755165 11.00000 0.04583 0.04009 = 0.03560 0.01221 0.01667 0.00981 CL1 3 -0.121679 0.416564 -0.009937 11.00000 0.03704 0.05840 = 0.04188 -0.00715 -0.00186 -0.01212 S2 7 0.618657 0.406172 0.573723 11.00000 0.03192 0.04821 = 0.04782 0.00900 0.01409 0.00695 O5 5 0.573918 0.435637 0.473387 11.00000 0.04357 0.04021 = 0.05318 0.01425 0.00735 -0.00219 N3 4 0.254409 0.436241 0.021086 11.00000 0.03852 0.02178 = 0.02734 0.00079 0.00839 0.00020 AFIX 13 H3 2 0.203708 0.453068 -0.054637 11.00000 -1.20000 AFIX 0 N2 4 0.313537 0.466814 0.267931 11.00000 0.02928 0.02700 = 0.03069 0.00012 0.01103 -0.00271 AFIX 13 H2 2 0.388286 0.449781 0.332425 11.00000 -1.20000 AFIX 0 N1 4 0.004215 0.455324 0.283222 11.00000 0.02194 0.04765 = 0.03352 -0.00004 0.00842 -0.00012 AFIX 13 H1 2 -0.068038 0.475477 0.239064 11.00000 -1.20000 AFIX 0 O3 5 0.527568 0.285376 0.286995 11.00000 0.06730 0.02999 = 0.04739 0.00606 0.01250 0.00349 O1 5 0.633003 0.254141 0.551200 11.00000 0.08061 0.02933 = 0.04108 0.00006 0.01068 -0.00007 O2 5 0.422504 0.258628 0.699109 11.00000 0.05560 0.04032 = 0.07152 -0.00637 -0.00186 -0.01277 O4 5 0.153326 0.303728 0.570667 11.00000 0.08619 0.04742 = 0.05874 -0.00719 -0.00104 0.01875 C28 1 0.136042 0.471303 0.400737 11.00000 0.03305 0.04918 = 0.03702 -0.00951 0.01579 0.00526 AFIX 23 H28A 2 0.199335 0.452822 0.462851 11.00000 -1.20000 H28B 2 0.085557 0.486757 0.451808 11.00000 -1.20000 AFIX 0 C25 1 0.423676 0.451060 0.096274 11.00000 0.03460 0.04208 = 0.04159 -0.00061 0.01916 -0.00363 AFIX 23 H25A 2 0.477031 0.459059 0.031081 11.00000 -1.20000 H25B 2 0.494850 0.432972 0.155362 11.00000 -1.20000 AFIX 0 C19 1 0.509585 0.365656 0.090930 11.00000 0.05346 0.02843 = 0.04996 -0.00004 0.03269 0.00008 AFIX 43 H19 2 0.581042 0.381031 0.065599 11.00000 -1.20000 AFIX 0 C5 1 0.573582 0.306321 0.818598 11.00000 0.06538 0.03900 = 0.03455 0.00407 0.01788 -0.00983 AFIX 43 H5 2 0.493101 0.308581 0.862019 11.00000 -1.20000 AFIX 0 C27 1 0.249720 0.492071 0.346816 11.00000 0.03776 0.03579 = 0.04072 -0.00836 0.01154 0.00272 AFIX 23 H27A 2 0.188418 0.511260 0.287662 11.00000 -1.20000 H27B 2 0.342123 0.502196 0.422339 11.00000 -1.20000 AFIX 0 C15 1 0.023249 0.394090 0.530950 11.00000 0.04357 0.04116 = 0.04295 -0.00633 0.02614 -0.00259 AFIX 43 H15 2 0.016784 0.412915 0.588034 11.00000 -1.20000 AFIX 0 C18 1 0.576948 0.337476 0.171573 11.00000 0.03877 0.04420 = 0.03982 0.00113 0.01626 0.00617 AFIX 43 H18 2 0.693274 0.333721 0.202396 11.00000 -1.20000 AFIX 0 C17 1 0.473884 0.314492 0.207800 11.00000 0.04868 0.02892 = 0.02895 -0.00033 0.01335 0.00938 C20 1 0.336908 0.372653 0.044002 11.00000 0.04426 0.03395 = 0.02638 -0.00654 0.01822 0.00850 C1 1 0.668421 0.279150 0.651977 11.00000 0.07597 0.03024 = 0.03774 0.00344 0.01191 0.00422 C16 1 0.084700 0.362144 0.587479 11.00000 0.04579 0.05458 = 0.03607 -0.00292 0.00961 -0.00447 AFIX 43 H16 2 0.118313 0.359213 0.683084 11.00000 -1.20000 AFIX 0 C23 1 0.265461 0.402585 -0.047733 11.00000 0.06240 0.03268 = 0.02514 -0.00318 0.02119 0.00424 AFIX 23 H23A 2 0.152747 0.396065 -0.107590 11.00000 -1.20000 H23B 2 0.333501 0.406473 -0.106286 11.00000 -1.20000 AFIX 0 C4 1 0.712523 0.328032 0.857096 11.00000 0.10955 0.04047 = 0.04004 -0.01026 0.02490 -0.02544 AFIX 43 H4 2 0.728605 0.344630 0.927823 11.00000 -1.20000 AFIX 0 C26 1 0.401676 0.481652 0.181656 11.00000 0.03030 0.03863 = 0.05145 0.00326 0.01293 -0.00929 AFIX 23 H26A 2 0.510435 0.491258 0.237758 11.00000 -1.20000 H26B 2 0.335687 0.500465 0.123186 11.00000 -1.20000 AFIX 0 C6 1 0.551884 0.281554 0.717886 11.00000 0.06724 0.02533 = 0.03622 0.01173 -0.00655 -0.00238 C10 1 0.700079 0.284197 0.370760 11.00000 0.06188 0.05047 = 0.04075 0.00335 0.01543 0.01873 AFIX 23 H10A 2 0.730749 0.305829 0.425285 11.00000 -1.20000 H10B 2 0.770400 0.282303 0.313054 11.00000 -1.20000 AFIX 0 C22 1 0.302989 0.320269 0.161739 11.00000 0.05526 0.02206 = 0.04273 -0.00676 0.02242 -0.00896 AFIX 43 H22 2 0.231773 0.304540 0.185704 11.00000 -1.20000 AFIX 0 C21 1 0.238210 0.348766 0.081680 11.00000 0.03980 0.02912 = 0.04429 -0.00582 0.00929 0.00102 AFIX 43 H21 2 0.121719 0.352285 0.050927 11.00000 -1.20000 AFIX 0 C2 1 0.803997 0.300658 0.691327 11.00000 0.06734 0.06693 = 0.04614 -0.00121 0.01607 -0.00345 AFIX 43 H2A 2 0.884963 0.298614 0.648302 11.00000 -1.20000 AFIX 0 C24 1 -0.105499 0.432428 0.326978 11.00000 0.04526 0.04795 = 0.05629 0.00498 0.02939 0.00550 AFIX 23 H24A 2 -0.203937 0.426915 0.247050 11.00000 -1.20000 H24B 2 -0.144409 0.445395 0.392314 11.00000 -1.20000 AFIX 0 C14 1 -0.028859 0.398789 0.391748 11.00000 0.03150 0.04492 = 0.05876 0.00148 0.02891 0.00181 C9 1 0.726152 0.253389 0.461719 11.00000 0.08303 0.05101 = 0.03848 -0.00049 0.01817 0.02898 AFIX 23 H9A 2 0.696370 0.232054 0.405290 11.00000 -1.20000 H9B 2 0.845320 0.251830 0.516344 11.00000 -1.20000 AFIX 0 C12 1 0.049198 0.338894 0.368116 11.00000 0.05638 0.05656 = 0.04305 -0.01075 0.01738 -0.00326 AFIX 43 H12 2 0.056732 0.320169 0.310981 11.00000 -1.20000 AFIX 0 C11 1 0.098012 0.334473 0.507428 11.00000 0.04125 0.04071 = 0.05422 -0.00319 0.00300 0.00133 C3 1 0.825120 0.324990 0.791207 11.00000 0.06557 0.07457 = 0.02142 -0.00434 -0.00037 -0.02313 AFIX 43 H3A 2 0.918957 0.339951 0.815150 11.00000 -1.20000 AFIX 0 C13 1 -0.010953 0.371234 0.313651 11.00000 0.04117 0.06094 = 0.03941 0.00196 0.01395 0.00093 AFIX 43 H13 2 -0.041018 0.374466 0.218396 11.00000 -1.20000 AFIX 0 C8 1 0.234385 0.280817 0.491260 11.00000 0.10938 0.06561 = 0.04984 -0.00994 0.01808 0.00301 AFIX 23 H8A 2 0.150140 0.273291 0.404970 11.00000 -1.20000 H8B 2 0.320506 0.294327 0.469378 11.00000 -1.20000 AFIX 0 C30 1 0.518764 0.414193 0.692206 11.00000 0.06183 0.06073 = 0.04284 0.00172 0.02004 0.01792 AFIX 137 H30A 2 0.558822 0.436264 0.739177 11.00000 -1.50000 H30B 2 0.542823 0.395128 0.758474 11.00000 -1.50000 H30C 2 0.398910 0.415661 0.645075 11.00000 -1.50000 AFIX 0 C7 1 0.305145 0.251877 0.567847 11.00000 0.08623 0.09140 = 0.05232 -0.02183 -0.03000 0.01492 AFIX 23 H7A 2 0.360566 0.237928 0.516014 11.00000 -1.20000 H7B 2 0.215185 0.237331 0.578999 11.00000 -1.20000 AFIX 0 C29 1 0.490927 0.371034 0.489619 11.00000 0.17503 0.04789 = 0.06522 -0.01377 0.03974 -0.02887 AFIX 137 H29A 2 0.376371 0.379187 0.449420 11.00000 -1.50000 H29B 2 0.495946 0.352378 0.554950 11.00000 -1.50000 H29C 2 0.529765 0.362089 0.417936 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_PG210623_0m_a.res in P2(1)/n REM R1 = 0.0933 for 4705 Fo > 4sig(Fo) and 0.1076 for all 5684 data REM 381 parameters refined using 22 restraints END WGHT 0.1456 13.6542 REM Highest difference peak 1.273, deepest hole -1.136, 1-sigma level 0.200 Q1 1 0.1357 0.2676 0.5269 11.00000 0.05 1.27 Q2 1 0.7843 0.3310 0.9606 11.00000 0.05 0.89 ; _shelx_res_checksum 65660 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 0.11498(7) 0.44093(2) 0.14497(6) 0.0261(2) Uani 1 1 d . . . . . Cl2 Cl 0.2026(3) 0.47621(6) 0.7552(2) 0.0398(5) Uani 1 1 d . . . . . Cl1 Cl -0.1217(3) 0.41656(7) -0.0099(2) 0.0496(6) Uani 1 1 d . . . . . S2 S 0.6187(3) 0.40617(6) 0.5737(2) 0.0425(6) Uani 1 1 d . U . . . O5 O 0.5739(8) 0.43564(16) 0.4734(7) 0.0479(16) Uani 1 1 d . . . . . N3 N 0.2544(9) 0.43624(15) 0.0211(7) 0.0299(15) Uani 1 1 d . . . . . H3 H 0.203708 0.453068 -0.054637 0.036 Uiso 1 1 calc R U . . . N2 N 0.3135(8) 0.46681(16) 0.2679(7) 0.0288(14) Uani 1 1 d . . . . . H2 H 0.388286 0.449781 0.332425 0.035 Uiso 1 1 calc R U . . . N1 N 0.0042(8) 0.45532(19) 0.2832(7) 0.0346(15) Uani 1 1 d . . . . . H1 H -0.068038 0.475477 0.239064 0.042 Uiso 1 1 calc R U . . . O3 O 0.5276(9) 0.28538(15) 0.2870(7) 0.0500(17) Uani 1 1 d . . . . . O1 O 0.6330(10) 0.25414(15) 0.5512(7) 0.0529(18) Uani 1 1 d . . . . . O2 O 0.4225(9) 0.25863(17) 0.6991(8) 0.062(2) Uani 1 1 d . . . . . O4 O 0.1533(11) 0.30373(19) 0.5707(8) 0.071(2) Uani 1 1 d . . . . . C28 C 0.1360(10) 0.4713(2) 0.4007(9) 0.039(2) Uani 1 1 d . . . . . H28A H 0.199335 0.452822 0.462851 0.046 Uiso 1 1 calc R U . . . H28B H 0.085557 0.486757 0.451808 0.046 Uiso 1 1 calc R U . . . C25 C 0.4237(11) 0.4511(2) 0.0963(9) 0.0378(19) Uani 1 1 d . . . . . H25A H 0.477031 0.459059 0.031081 0.045 Uiso 1 1 calc R U . . . H25B H 0.494850 0.432972 0.155362 0.045 Uiso 1 1 calc R U . . . C19 C 0.5096(12) 0.3657(2) 0.0909(9) 0.040(2) Uani 1 1 d . . . . . H19 H 0.581042 0.381031 0.065599 0.048 Uiso 1 1 calc R U . . . C5 C 0.5736(13) 0.3063(2) 0.8186(9) 0.046(2) Uani 1 1 d . . . . . H5 H 0.493101 0.308581 0.862019 0.055 Uiso 1 1 calc R U . . . C27 C 0.2497(11) 0.4921(2) 0.3468(9) 0.039(2) Uani 1 1 d . . . . . H27A H 0.188418 0.511260 0.287662 0.046 Uiso 1 1 calc R U . . . H27B H 0.342123 0.502196 0.422339 0.046 Uiso 1 1 calc R U . . . C15 C 0.0232(11) 0.3941(2) 0.5310(9) 0.040(2) Uani 1 1 d . . . . . H15 H 0.016784 0.412915 0.588034 0.048 Uiso 1 1 calc R U . . . C18 C 0.5769(12) 0.3375(2) 0.1716(9) 0.040(2) Uani 1 1 d . . . . . H18 H 0.693274 0.333721 0.202396 0.048 Uiso 1 1 calc R U . . . C17 C 0.4739(11) 0.3145(2) 0.2078(8) 0.0355(19) Uani 1 1 d . . . . . C20 C 0.3369(11) 0.3727(2) 0.0440(8) 0.0333(18) Uani 1 1 d . . . . . C1 C 0.6684(14) 0.2792(2) 0.6520(10) 0.050(2) Uani 1 1 d . . . . . C16 C 0.0847(12) 0.3621(3) 0.5875(10) 0.047(2) Uani 1 1 d . . . . . H16 H 0.118313 0.359213 0.683084 0.056 Uiso 1 1 calc R U . . . C23 C 0.2655(12) 0.4026(2) -0.0477(8) 0.038(2) Uani 1 1 d . . . . . H23A H 0.152747 0.396065 -0.107590 0.046 Uiso 1 1 calc R U . . . H23B H 0.333501 0.406473 -0.106286 0.046 Uiso 1 1 calc R U . . . C4 C 0.7125(17) 0.3280(3) 0.8571(11) 0.063(3) Uani 1 1 d . . . . . H4 H 0.728605 0.344630 0.927823 0.076 Uiso 1 1 calc R U . . . C26 C 0.4017(11) 0.4817(2) 0.1817(9) 0.040(2) Uani 1 1 d . . . . . H26A H 0.510435 0.491258 0.237758 0.048 Uiso 1 1 calc R U . . . H26B H 0.335687 0.500465 0.123186 0.048 Uiso 1 1 calc R U . . . C6 C 0.5519(13) 0.2816(2) 0.7179(9) 0.049(3) Uani 1 1 d . . . . . C10 C 0.7001(13) 0.2842(3) 0.3708(10) 0.052(2) Uani 1 1 d . . . . . H10A H 0.730749 0.305829 0.425285 0.062 Uiso 1 1 calc R U . . . H10B H 0.770400 0.282303 0.313054 0.062 Uiso 1 1 calc R U . . . C22 C 0.3030(12) 0.3203(2) 0.1617(9) 0.039(2) Uani 1 1 d . . . . . H22 H 0.231773 0.304540 0.185704 0.046 Uiso 1 1 calc R U . . . C21 C 0.2382(11) 0.3488(2) 0.0817(9) 0.039(2) Uani 1 1 d . . . . . H21 H 0.121719 0.352285 0.050927 0.047 Uiso 1 1 calc R U . . . C2 C 0.8040(15) 0.3007(3) 0.6913(11) 0.061(3) Uani 1 1 d . . . . . H2A H 0.884963 0.298614 0.648302 0.073 Uiso 1 1 calc R U . . . C24 C -0.1055(12) 0.4324(3) 0.3270(11) 0.047(2) Uani 1 1 d . . . . . H24A H -0.203937 0.426915 0.247050 0.056 Uiso 1 1 calc R U . . . H24B H -0.144409 0.445395 0.392314 0.056 Uiso 1 1 calc R U . . . C14 C -0.0289(11) 0.3988(2) 0.3917(10) 0.042(2) Uani 1 1 d . . . . . C9 C 0.7262(15) 0.2534(3) 0.4617(10) 0.058(3) Uani 1 1 d . . . . . H9A H 0.696370 0.232054 0.405290 0.070 Uiso 1 1 calc R U . . . H9B H 0.845320 0.251830 0.516344 0.070 Uiso 1 1 calc R U . . . C12 C 0.0492(13) 0.3389(3) 0.3681(10) 0.052(2) Uani 1 1 d . . . . . H12 H 0.056732 0.320169 0.310981 0.062 Uiso 1 1 calc R U . . . C11 C 0.0980(12) 0.3345(2) 0.5074(11) 0.049(2) Uani 1 1 d . . . . . C3 C 0.8251(14) 0.3250(3) 0.7912(9) 0.058(3) Uani 1 1 d . . . . . H3A H 0.918957 0.339951 0.815150 0.069 Uiso 1 1 calc R U . . . C13 C -0.0110(12) 0.3712(3) 0.3137(10) 0.047(2) Uani 1 1 d . . . . . H13 H -0.041018 0.374466 0.218396 0.057 Uiso 1 1 calc R U . . . C8 C 0.2344(19) 0.2808(3) 0.4913(13) 0.077(4) Uani 1 1 d . U . . . H8A H 0.150140 0.273291 0.404970 0.093 Uiso 1 1 calc R U . . . H8B H 0.320506 0.294327 0.469378 0.093 Uiso 1 1 calc R U . . . C30 C 0.5188(14) 0.4142(3) 0.6922(10) 0.055(3) Uani 1 1 d . U . . . H30A H 0.558822 0.436264 0.739177 0.082 Uiso 1 1 calc R U . . . H30B H 0.542823 0.395128 0.758474 0.082 Uiso 1 1 calc R U . . . H30C H 0.398910 0.415661 0.645075 0.082 Uiso 1 1 calc R U . . . C7 C 0.3051(18) 0.2519(4) 0.5678(13) 0.090(5) Uani 1 1 d . U . . . H7A H 0.360566 0.237928 0.516014 0.108 Uiso 1 1 calc R U . . . H7B H 0.215185 0.237331 0.578999 0.108 Uiso 1 1 calc R U . . . C29 C 0.491(2) 0.3710(3) 0.4896(14) 0.096(5) Uani 1 1 d . U . . . H29A H 0.376371 0.379187 0.449420 0.144 Uiso 1 1 calc R U . . . H29B H 0.495946 0.352378 0.554950 0.144 Uiso 1 1 calc R U . . . H29C H 0.529765 0.362089 0.417936 0.144 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0238(4) 0.0277(4) 0.0249(4) -0.0026(2) 0.0058(3) -0.0016(2) Cl2 0.0458(12) 0.0401(11) 0.0356(11) 0.0122(8) 0.0167(9) 0.0098(9) Cl1 0.0370(12) 0.0584(14) 0.0419(13) -0.0071(10) -0.0019(10) -0.0121(10) S2 0.0319(11) 0.0482(13) 0.0478(14) 0.0090(10) 0.0141(10) 0.0070(9) O5 0.044(4) 0.040(4) 0.053(4) 0.014(3) 0.007(3) -0.002(3) N3 0.039(4) 0.022(3) 0.027(4) 0.001(2) 0.008(3) 0.000(3) N2 0.029(3) 0.027(3) 0.031(4) 0.000(3) 0.011(3) -0.003(3) N1 0.022(3) 0.048(4) 0.034(4) 0.000(3) 0.008(3) 0.000(3) O3 0.067(4) 0.030(3) 0.047(4) 0.006(3) 0.013(3) 0.003(3) O1 0.081(5) 0.029(3) 0.041(4) 0.000(3) 0.011(3) 0.000(3) O2 0.056(4) 0.040(4) 0.072(5) -0.006(3) -0.002(4) -0.013(3) O4 0.086(6) 0.047(4) 0.059(5) -0.007(3) -0.001(4) 0.019(4) C28 0.033(4) 0.049(5) 0.037(5) -0.010(4) 0.016(4) 0.005(4) C25 0.035(4) 0.042(5) 0.042(5) -0.001(4) 0.019(4) -0.004(4) C19 0.053(5) 0.028(4) 0.050(5) 0.000(4) 0.033(5) 0.000(4) C5 0.065(6) 0.039(5) 0.035(5) 0.004(4) 0.018(5) -0.010(4) C27 0.038(5) 0.036(5) 0.041(5) -0.008(4) 0.012(4) 0.003(4) C15 0.044(5) 0.041(5) 0.043(5) -0.006(4) 0.026(4) -0.003(4) C18 0.039(5) 0.044(5) 0.040(5) 0.001(4) 0.016(4) 0.006(4) C17 0.049(5) 0.029(4) 0.029(4) 0.000(3) 0.013(4) 0.009(4) C20 0.044(5) 0.034(4) 0.026(4) -0.007(3) 0.018(4) 0.009(4) C1 0.076(7) 0.030(5) 0.038(5) 0.003(4) 0.012(5) 0.004(5) C16 0.046(5) 0.055(6) 0.036(5) -0.003(4) 0.010(4) -0.004(4) C23 0.062(6) 0.033(4) 0.025(4) -0.003(3) 0.021(4) 0.004(4) C4 0.110(10) 0.040(6) 0.040(6) -0.010(4) 0.025(6) -0.025(6) C26 0.030(4) 0.039(5) 0.051(6) 0.003(4) 0.013(4) -0.009(4) C6 0.067(7) 0.025(4) 0.036(5) 0.012(4) -0.007(5) -0.002(4) C10 0.062(6) 0.050(6) 0.041(5) 0.003(4) 0.015(5) 0.019(5) C22 0.055(6) 0.022(4) 0.043(5) -0.007(3) 0.022(4) -0.009(4) C21 0.040(5) 0.029(4) 0.044(5) -0.006(4) 0.009(4) 0.001(4) C2 0.067(7) 0.067(7) 0.046(6) -0.001(5) 0.016(5) -0.003(6) C24 0.045(6) 0.048(5) 0.056(6) 0.005(4) 0.029(5) 0.006(4) C14 0.032(5) 0.045(5) 0.059(6) 0.001(4) 0.029(4) 0.002(4) C9 0.083(8) 0.051(6) 0.038(6) 0.000(4) 0.018(5) 0.029(5) C12 0.056(6) 0.057(6) 0.043(6) -0.011(5) 0.017(5) -0.003(5) C11 0.041(5) 0.041(5) 0.054(6) -0.003(4) 0.003(5) 0.001(4) C3 0.066(7) 0.075(7) 0.021(5) -0.004(4) 0.000(5) -0.023(6) C13 0.041(5) 0.061(6) 0.039(5) 0.002(4) 0.014(4) 0.001(4) C8 0.109(11) 0.066(7) 0.050(7) -0.010(5) 0.018(7) 0.003(7) C30 0.062(6) 0.061(6) 0.043(5) 0.002(4) 0.020(5) 0.018(5) C7 0.086(9) 0.091(9) 0.052(7) -0.022(6) -0.030(7) 0.015(7) C29 0.175(16) 0.048(7) 0.065(8) -0.014(5) 0.040(9) -0.029(8) 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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 '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 N3 Pd1 Cl1 94.7(2) . . ? N3 Pd1 N1 167.6(3) . . ? N2 Pd1 Cl1 173.89(19) . . ? N2 Pd1 N3 84.2(3) . . ? N2 Pd1 N1 84.8(3) . . ? N1 Pd1 Cl1 95.5(2) . . ? O5 S2 C30 107.0(5) . . ? O5 S2 C29 104.8(5) . . ? C30 S2 C29 96.7(7) . . ? Pd1 N3 H3 104.8 . . ? C25 N3 Pd1 107.5(5) . . ? C25 N3 H3 104.8 . . ? C23 N3 Pd1 121.8(5) . . ? C23 N3 H3 104.8 . . ? C23 N3 C25 111.7(7) . . ? Pd1 N2 H2 108.7 . . ? C27 N2 Pd1 106.5(5) . . ? C27 N2 H2 108.7 . . ? C26 N2 Pd1 107.2(5) . . ? C26 N2 H2 108.7 . . ? C26 N2 C27 116.7(6) . . ? Pd1 N1 H1 104.1 . . ? C28 N1 Pd1 106.8(5) . . ? C28 N1 H1 104.1 . . ? C24 N1 Pd1 123.8(6) . . ? C24 N1 H1 104.1 . . ? C24 N1 C28 112.0(7) . . ? C17 O3 C10 117.3(7) . . ? C1 O1 C9 119.3(9) . . ? C6 O2 C7 121.7(10) . . ? C11 O4 C8 112.4(9) . . ? N1 C28 H28A 110.0 . . ? N1 C28 H28B 110.0 . . ? N1 C28 C27 108.3(7) . . ? H28A C28 H28B 108.4 . . ? C27 C28 H28A 110.0 . . ? C27 C28 H28B 110.0 . . ? N3 C25 H25A 110.1 . . ? N3 C25 H25B 110.1 . . ? N3 C25 C26 107.9(7) . . ? H25A C25 H25B 108.4 . . ? C26 C25 H25A 110.1 . . ? C26 C25 H25B 110.1 . . ? C18 C19 H19 118.8 . . ? C18 C19 C20 122.3(8) . . ? C20 C19 H19 118.8 . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C6 C5 C4 120.7(10) . . ? N2 C27 C28 105.7(7) . . ? N2 C27 H27A 110.6 . . ? N2 C27 H27B 110.6 . . ? C28 C27 H27A 110.6 . . ? C28 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? C16 C15 H15 119.8 . . ? C16 C15 C14 120.4(8) . . ? C14 C15 H15 119.8 . . ? C19 C18 H18 120.2 . . ? C19 C18 C17 119.5(8) . . ? C17 C18 H18 120.2 . . ? O3 C17 C18 124.4(8) . . ? O3 C17 C22 115.8(8) . . ? C18 C17 C22 119.7(8) . . ? C19 C20 C23 121.5(8) . . ? C21 C20 C19 116.2(8) . . ? C21 C20 C23 122.2(8) . . ? O1 C1 C6 114.5(9) . . ? C2 C1 O1 126.3(10) . . ? C2 C1 C6 119.2(9) . . ? C15 C16 H16 119.4 . . ? C11 C16 C15 121.2(9) . . ? C11 C16 H16 119.4 . . ? N3 C23 H23A 108.4 . . ? N3 C23 H23B 108.4 . . ? C20 C23 N3 115.6(6) . . ? C20 C23 H23A 108.4 . . ? C20 C23 H23B 108.4 . . ? H23A C23 H23B 107.4 . . ? C5 C4 H4 120.6 . . ? C3 C4 C5 118.9(9) . . ? C3 C4 H4 120.6 . . ? N2 C26 C25 104.7(6) . . ? N2 C26 H26A 110.8 . . ? N2 C26 H26B 110.8 . . ? C25 C26 H26A 110.8 . . ? C25 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? O2 C6 C5 116.2(10) . . ? O2 C6 C1 124.4(9) . . ? C5 C6 C1 119.2(9) . . ? O3 C10 H10A 110.0 . . ? O3 C10 H10B 110.0 . . ? O3 C10 C9 108.4(9) . . ? H10A C10 H10B 108.4 . . ? C9 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C17 C22 H22 120.1 . . ? C21 C22 C17 119.8(8) . . ? C21 C22 H22 120.1 . . ? C20 C21 H21 118.8 . . ? C22 C21 C20 122.4(8) . . ? C22 C21 H21 118.8 . . ? C1 C2 H2A 119.3 . . ? C3 C2 C1 121.3(11) . . ? C3 C2 H2A 119.3 . . ? N1 C24 H24A 108.5 . . ? N1 C24 H24B 108.5 . . ? N1 C24 C14 115.1(7) . . ? H24A C24 H24B 107.5 . . ? C14 C24 H24A 108.5 . . ? C14 C24 H24B 108.5 . . ? C15 C14 C24 121.6(8) . . ? C13 C14 C15 117.7(9) . . ? C13 C14 C24 120.7(9) . . ? O1 C9 C10 114.2(8) . . ? O1 C9 H9A 108.7 . . ? O1 C9 H9B 108.7 . . ? C10 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C12 H12 120.7 . . ? C11 C12 C13 118.7(9) . . ? C13 C12 H12 120.7 . . ? O4 C11 C16 117.2(9) . . ? O4 C11 C12 123.5(9) . . ? C16 C11 C12 119.2(9) . . ? C4 C3 H3A 119.7 . . ? C2 C3 C4 120.7(10) . . ? C2 C3 H3A 119.7 . . ? C14 C13 C12 122.8(9) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? O4 C8 H8A 109.7 . . ? O4 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C7 C8 O4 109.6(11) . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? S2 C30 H30A 109.5 . . ? S2 C30 H30B 109.5 . . ? S2 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C7 H7A 108.2 . . ? O2 C7 H7B 108.2 . . ? C8 C7 O2 116.2(11) . . ? C8 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? S2 C29 H29A 109.5 . . ? S2 C29 H29B 109.5 . . ? S2 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 Cl1 2.323(2) . ? Pd1 N3 2.047(7) . ? Pd1 N2 2.015(6) . ? Pd1 N1 2.057(7) . ? S2 O5 1.501(6) . ? S2 C30 1.756(10) . ? S2 C29 1.771(13) . ? N3 H3 1.0000 . ? N3 C25 1.509(11) . ? N3 C23 1.495(10) . ? N2 H2 1.0000 . ? N2 C27 1.491(10) . ? N2 C26 1.474(10) . ? N1 H1 1.0000 . ? N1 C28 1.492(11) . ? N1 C24 1.468(11) . ? O3 C17 1.373(10) . ? O3 C10 1.443(12) . ? O1 C1 1.381(11) . ? O1 C9 1.422(13) . ? O2 C6 1.376(12) . ? O2 C7 1.426(13) . ? O4 C11 1.356(12) . ? O4 C8 1.528(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C27 1.508(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.524(12) . ? C19 H19 0.9500 . ? C19 C18 1.372(12) . ? C19 C20 1.419(12) . ? C5 H5 0.9500 . ? C5 C4 1.396(15) . ? C5 C6 1.383(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C15 H15 0.9500 . ? C15 C16 1.384(13) . ? C15 C14 1.384(13) . ? C18 H18 0.9500 . ? C18 C17 1.388(13) . ? C17 C22 1.397(13) . ? C20 C23 1.488(11) . ? C20 C21 1.391(12) . ? C1 C6 1.396(15) . ? C1 C2 1.370(15) . ? C16 H16 0.9500 . ? C16 C11 1.380(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C4 H4 0.9500 . ? C4 C3 1.368(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C9 1.485(14) . ? C22 H22 0.9500 . ? C22 C21 1.374(12) . ? C21 H21 0.9500 . ? C2 H2A 0.9500 . ? C2 C3 1.366(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C14 1.500(13) . ? C14 C13 1.375(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C12 H12 0.9500 . ? C12 C11 1.385(14) . ? C12 C13 1.388(14) . ? C3 H3A 0.9500 . ? C13 H13 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C7 1.382(18) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 N3 C25 C26 -34.7(7) . . . . ? Pd1 N3 C23 C20 -61.3(10) . . . . ? Pd1 N2 C27 C28 48.6(7) . . . . ? Pd1 N2 C26 C25 -50.9(7) . . . . ? Pd1 N1 C28 C27 37.3(8) . . . . ? Pd1 N1 C24 C14 59.2(10) . . . . ? N3 C25 C26 N2 56.7(8) . . . . ? N1 C28 C27 N2 -57.6(8) . . . . ? N1 C24 C14 C15 102.8(10) . . . . ? N1 C24 C14 C13 -78.4(12) . . . . ? O3 C17 C22 C21 -179.9(8) . . . . ? O3 C10 C9 O1 -61.1(11) . . . . ? O1 C1 C6 O2 7.9(13) . . . . ? O1 C1 C6 C5 -178.6(8) . . . . ? O1 C1 C2 C3 178.9(10) . . . . ? O4 C8 C7 O2 -55.8(18) . . . . ? C28 N1 C24 C14 -71.0(10) . . . . ? C25 N3 C23 C20 67.5(9) . . . . ? C19 C18 C17 O3 179.5(8) . . . . ? C19 C18 C17 C22 0.1(13) . . . . ? C19 C20 C23 N3 -89.9(10) . . . . ? C19 C20 C21 C22 1.1(12) . . . . ? C5 C4 C3 C2 -1.3(17) . . . . ? C27 N2 C26 C25 -170.1(7) . . . . ? C15 C16 C11 O4 -177.5(9) . . . . ? C15 C16 C11 C12 0.1(15) . . . . ? C15 C14 C13 C12 3.1(14) . . . . ? C18 C19 C20 C23 -177.6(8) . . . . ? C18 C19 C20 C21 -1.5(12) . . . . ? C18 C17 C22 C21 -0.4(12) . . . . ? C17 O3 C10 C9 171.9(7) . . . . ? C17 C22 C21 C20 -0.2(13) . . . . ? C20 C19 C18 C17 0.9(13) . . . . ? C1 O1 C9 C10 -66.6(12) . . . . ? C1 C2 C3 C4 1.4(17) . . . . ? C16 C15 C14 C24 176.2(8) . . . . ? C16 C15 C14 C13 -2.6(13) . . . . ? C23 N3 C25 C26 -170.7(7) . . . . ? C23 C20 C21 C22 177.2(8) . . . . ? C4 C5 C6 O2 172.2(9) . . . . ? C4 C5 C6 C1 -1.9(14) . . . . ? C26 N2 C27 C28 168.2(7) . . . . ? C6 O2 C7 C8 -50.4(19) . . . . ? C6 C5 C4 C3 1.6(16) . . . . ? C6 C1 C2 C3 -1.7(16) . . . . ? C10 O3 C17 C18 19.8(12) . . . . ? C10 O3 C17 C22 -160.8(8) . . . . ? C21 C20 C23 N3 94.2(10) . . . . ? C2 C1 C6 O2 -171.6(9) . . . . ? C2 C1 C6 C5 1.9(14) . . . . ? C24 N1 C28 C27 175.8(7) . . . . ? C24 C14 C13 C12 -175.7(9) . . . . ? C14 C15 C16 C11 1.0(14) . . . . ? C9 O1 C1 C6 169.1(8) . . . . ? C9 O1 C1 C2 -11.4(14) . . . . ? C11 O4 C8 C7 173.0(11) . . . . ? C11 C12 C13 C14 -2.0(16) . . . . ? C13 C12 C11 O4 177.8(10) . . . . ? C13 C12 C11 C16 0.3(15) . . . . ? C8 O4 C11 C16 -154.7(10) . . . . ? C8 O4 C11 C12 27.8(14) . . . . ? C7 O2 C6 C5 130.6(11) . . . . ? C7 O2 C6 C1 -55.8(14) . . . . ?