#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:38:48 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132568.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_4132568 loop_ _publ_author_name 'Yuan, Shuai' 'Zhang, Peng' 'Zhang, Liangliang' 'Garcia-Esparza, Angel T' 'Sokaras, Dimosthenis' 'Qin, Jun-Sheng' 'Feng, Liang' 'Day, Gregory S.' 'Chen, Wenmiao' 'Drake, Hannah F.' 'Elumalai, Palani' 'Madrahimov, Sherzod T.' 'Sun, Daofeng' 'Zhou, Hong-Cai' _publ_section_title ; Exposed Equatorial Positions of Metal Centers via Sequential Ligand Elimination and Installation in MOFs. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10814 _journal_page_last 10819 _journal_paper_doi 10.1021/jacs.8b04886 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C12 H10 Cl2 N2 O4 Pd, 2(C2 H6 O S)' _chemical_formula_sum 'C16 H22 Cl2 N2 O6 Pd S2' _chemical_formula_weight 579.77 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2018-05-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _cell_angle_alpha 99.2697(18) _cell_angle_beta 101.0558(19) _cell_angle_gamma 98.754(2) _cell_formula_units_Z 1 _cell_length_a 5.5954(4) _cell_length_b 8.3386(6) _cell_length_c 12.7456(8) _cell_measurement_reflns_used 6736 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 27.569 _cell_measurement_theta_min 2.521 _cell_volume 565.64(7) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 110.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_unetI/netI 0.0219 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7643 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.569 _diffrn_reflns_theta_min 2.520 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6323 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.702 _exptl_crystal_description needle _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.385 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2590 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.244 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0228 _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^)+(0.0266P)^2^+0.2841P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.0605 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2451 _reflns_number_total 2590 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04886_si_002.cif _cod_data_source_block PdINA _cod_database_code 4132568 _shelx_shelxl_version_number 2014/7 _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 0.951 _shelx_estimated_absorpt_t_min 0.862 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C4(H4), C3(H3), C6(H6) 2.b Idealised Me refined as rotating group: C15(H15a,H15b,H15c), C25(H25a,H25b,H25c) 2.c Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; PdINA.res created by SHELXL-2014/7 TITL PdINA in P-1 CELL 0.71073 5.5954 8.3386 12.7456 99.2697 101.0558 98.7538 ZERR 1 0.0004 0.0006 0.0008 0.0018 0.0019 0.002 LATT 1 SFAC C H Cl N O Pd S UNIT 16 22 2 2 6 1 2 L.S. 99 PLAN 5 SIZE 0.04 0.05 0.12 TEMP -163.15 fmap 2 acta REM REM REM WGHT 0.026600 0.284100 FVAR 0.89527 PD1 6 0.000000 0.000000 0.000000 10.50000 0.01101 0.01571 = 0.01150 0.00437 -0.00012 -0.00060 CL1 3 -0.005254 0.276565 0.007166 11.00000 0.01799 0.01668 = 0.02043 0.00567 0.00052 0.00023 S4 7 0.706164 0.608922 0.287326 11.00000 0.01721 0.01932 = 0.02111 0.00355 -0.00165 0.00046 O3 5 0.843075 0.787306 0.324953 11.00000 0.02417 0.02128 = 0.01654 0.00421 -0.00308 -0.00502 O1 5 1.069806 0.275424 0.414064 11.00000 0.01574 0.03695 = 0.02019 0.00829 -0.00127 -0.00607 O2 5 0.817839 0.138323 0.500854 11.00000 0.01613 0.03170 = 0.01333 0.00600 -0.00175 -0.00352 AFIX 147 H2 2 0.940561 0.167878 0.553859 11.00000 -1.50000 AFIX 0 N1 4 0.280275 0.056600 0.132858 11.00000 0.01281 0.01618 = 0.01415 0.00506 0.00072 0.00029 C5 1 0.246833 0.012618 0.227065 11.00000 0.01306 0.01917 = 0.01765 0.00653 0.00310 0.00024 AFIX 43 H5 2 0.091012 -0.048950 0.229294 11.00000 -1.20000 AFIX 0 C4 1 0.501753 0.141994 0.129415 11.00000 0.01537 0.01886 = 0.01451 0.00464 0.00264 0.00083 AFIX 43 H4 2 0.524579 0.173178 0.063011 11.00000 -1.20000 AFIX 0 C15 1 0.544350 0.600368 0.151955 11.00000 0.02876 0.04183 = 0.01726 0.00192 -0.00394 -0.01054 AFIX 137 H15A 2 0.456789 0.693463 0.150140 11.00000 -1.50000 H15B 2 0.424316 0.496077 0.126483 11.00000 -1.50000 H15C 2 0.662503 0.606835 0.104417 11.00000 -1.50000 AFIX 0 C3 1 0.696801 0.185716 0.219279 11.00000 0.01341 0.01819 = 0.01647 0.00395 0.00298 0.00067 AFIX 43 H3 2 0.852484 0.244564 0.214590 11.00000 -1.20000 AFIX 0 C1 1 0.874040 0.193427 0.415617 11.00000 0.01664 0.01966 = 0.01438 0.00221 0.00036 0.00334 C2 1 0.661936 0.142245 0.316980 11.00000 0.01351 0.01672 = 0.01441 0.00289 0.00071 0.00359 C6 1 0.433299 0.054838 0.320229 11.00000 0.01666 0.02073 = 0.01454 0.00536 0.00272 0.00155 AFIX 43 H6 2 0.405098 0.024198 0.386092 11.00000 -1.20000 AFIX 0 C25 1 0.450136 0.592621 0.350759 11.00000 0.03483 0.04343 = 0.03432 0.00789 0.01470 -0.00829 AFIX 137 H25A 2 0.510384 0.618694 0.430132 11.00000 -1.50000 H25B 2 0.353615 0.479605 0.328585 11.00000 -1.50000 H25C 2 0.344920 0.670556 0.328614 11.00000 -1.50000 AFIX 0 HKLF 4 REM PdINA in P-1 REM R1 = 0.0228 for 2451 Fo > 4sig(Fo) and 0.0250 for all 2590 data REM 136 parameters refined using 0 restraints END WGHT 0.0266 0.2841 REM Highest difference peak 0.385, deepest hole -0.865, 1-sigma level 0.140 Q1 1 0.4673 0.5744 0.5352 11.00000 0.05 0.39 Q2 1 0.6903 0.5430 0.1189 11.00000 0.05 0.34 Q3 1 0.8573 0.4650 0.1841 11.00000 0.05 0.32 Q4 1 0.9909 0.4301 0.2473 11.00000 0.05 0.32 Q5 1 0.3605 0.2654 0.0122 11.00000 0.05 0.31 ; _shelx_res_checksum 66371 _shelx_hkl_file ; -1 0 0 1203.33 30.1769 1 -1 0 0 1461.60 31.3186 2 1 0 0 1444.51 30.3326 1 -2 0 0 1220.23 29.9756 2 2 0 0 1253.80 28.1818 1 2 0 0 1181.55 29.9150 2 -3 0 0 1549.09 36.6310 1 -3 0 0 1521.25 39.0286 2 3 0 0 1580.61 38.8397 2 -4 0 0 1693.63 40.9731 1 -4 0 0 1691.27 44.3495 2 4 0 0 1695.78 40.2741 1 -5 0 0 119.440 6.52564 1 -5 0 0 118.943 8.47217 2 5 0 0 111.644 6.22796 1 -6 0 0 589.427 18.9001 1 -6 0 0 600.393 23.4270 2 -7 1 0 28.5100 5.11350 1 -6 1 0 70.7711 8.95201 2 -6 1 0 69.8795 6.65521 1 5 -1 0 732.310 21.5037 1 -5 1 0 757.528 22.2402 1 -5 1 0 765.470 25.1446 2 4 -1 0 589.232 17.0703 1 4 -1 0 567.845 19.3346 2 -4 1 0 580.643 19.4122 2 -4 1 0 610.734 17.6557 1 3 -1 0 176.102 7.99726 2 3 -1 0 168.384 6.70747 1 -3 1 0 172.538 6.86413 1 -3 1 0 172.282 7.82870 2 2 -1 0 406.775 12.5055 2 2 -1 0 414.339 11.3277 1 -2 1 0 389.356 12.0107 2 -2 1 0 405.895 11.4033 1 1 -1 0 2081.35 46.1285 1 1 -1 0 2024.94 46.2752 2 1 -1 0 2133.49 46.5843 2 0 -1 0 1186.58 28.6323 1 0 -1 0 1424.95 28.5740 2 -1 -1 0 1214.17 26.3665 1 1 1 0 1185.69 27.4686 2 1 1 0 1201.18 26.3026 1 -2 -1 0 258.423 9.03147 2 -2 -1 0 264.900 7.33177 1 2 1 0 261.076 7.08285 1 2 1 0 259.018 8.68308 2 -3 -1 0 240.502 7.60777 1 -3 -1 0 229.873 9.65112 2 3 1 0 236.930 7.29188 1 3 1 0 224.611 9.14480 2 -4 -1 0 154.104 6.28927 1 -4 -1 0 142.594 8.42141 2 4 1 0 153.081 5.97258 1 4 1 0 134.511 7.67537 2 -5 -1 0 227.450 8.95966 1 -5 -1 0 225.339 12.0408 2 5 1 0 225.785 8.62868 1 -6 -1 0 314.674 16.3483 2 -6 -1 0 293.289 11.3447 1 7 -2 0 17.5771 6.17780 2 -7 2 0 19.2187 5.05109 1 -6 2 0 65.9670 6.95821 1 5 -2 0 201.488 9.27057 1 -5 2 0 209.391 10.8950 2 -5 2 0 212.003 9.86068 1 4 -2 0 61.3130 5.92736 2 4 -2 0 59.8555 4.82244 1 -4 2 0 61.5253 4.75690 1 -4 2 0 58.0730 5.29629 2 3 -2 0 734.666 20.0227 1 3 -2 0 726.794 21.5428 2 -3 2 0 728.594 20.1414 1 2 -2 0 61.3950 3.61232 2 2 -2 0 64.5210 4.02978 2 2 -2 0 62.2883 3.60049 1 -2 2 0 65.6705 3.70267 1 1 -2 0 2968.96 63.7545 1 1 -2 0 2895.94 63.1378 2 1 -2 0 2749.93 61.7925 3 -1 2 0 2822.34 63.3931 2 -1 2 0 2877.88 63.6151 1 0 -2 0 19.6158 1.41891 2 0 -2 0 21.4022 1.16521 3 0 -2 0 22.0078 1.55857 1 0 2 0 18.3636 1.44639 1 0 2 0 21.4242 1.04177 3 0 2 0 20.5946 1.42611 2 -1 -2 0 232.835 6.17546 1 -1 -2 0 237.471 7.41181 2 1 2 0 245.957 6.39396 1 1 2 0 241.960 7.00010 2 1 2 0 242.915 7.12289 3 -2 -2 0 1.80863 0.59224 1 -2 -2 0 2.69638 0.95658 2 2 2 0 2.24005 0.64343 1 2 2 0 2.90759 1.06976 2 -3 -2 0 97.8153 6.06799 2 -3 -2 0 105.791 4.19503 1 3 2 0 99.7568 3.89289 1 3 2 0 97.5600 5.41339 2 -4 -2 0 1008.86 25.1003 1 -4 -2 0 1018.49 30.1981 2 4 2 0 1003.42 24.4933 1 -5 -2 0 28.4031 4.99489 2 -5 -2 0 27.1596 3.76870 1 5 2 0 31.0251 3.87866 1 -6 -2 0 26.9448 5.73221 2 7 -3 0 328.928 17.7244 2 -7 3 0 331.897 15.6381 1 6 -3 0 37.6511 7.30384 2 -6 3 0 32.0365 6.27112 1 5 -3 0 772.013 25.0076 2 -5 3 0 757.473 23.6548 1 4 -3 0 2099.35 51.9843 2 4 -3 0 2049.79 53.0707 2 4 -3 0 2052.69 50.7759 1 -4 3 0 2087.96 51.1786 1 3 -3 0 986.006 26.5298 2 3 -3 0 999.129 27.6142 2 3 -3 0 968.054 26.1869 1 -3 3 0 983.573 26.3498 1 2 -3 0 148.361 6.11214 2 2 -3 0 155.048 6.63281 1 -2 3 0 144.582 6.36403 1 -2 3 0 147.880 6.63150 2 1 -3 0 2631.60 57.1685 3 1 -3 0 2587.54 58.7983 2 1 -3 0 2685.22 60.1955 1 -1 3 0 2698.38 60.0002 1 0 -3 0 1142.56 25.7550 3 0 -3 0 1147.96 26.6482 2 0 -3 0 1161.40 27.0968 1 0 3 0 1130.03 25.3929 3 0 3 0 1216.44 27.1586 1 0 3 0 1091.30 27.3458 2 -1 -3 0 370.995 9.59765 1 -1 -3 0 353.164 9.39993 1 -1 -3 0 361.783 10.6849 2 1 3 0 354.246 9.92752 2 1 3 0 351.112 9.90539 3 -2 -3 0 2972.60 68.3797 2 -2 -3 0 2931.43 64.5716 1 2 3 0 2970.16 67.0418 3 2 3 0 2936.90 66.5481 2 2 3 0 2939.31 64.7844 1 -3 -3 0 2758.83 65.9687 2 -3 -3 0 2702.36 61.0409 1 3 3 0 2711.31 63.3693 2 3 3 0 2676.58 63.9157 3 3 3 0 2780.52 60.3028 1 -4 -3 0 520.878 14.0992 1 4 3 0 526.502 13.8547 1 -5 -3 0 135.717 9.95349 2 -5 -3 0 141.083 5.98395 1 -6 -3 0 241.402 15.0422 2 -7 4 0 114.500 10.7603 1 6 -4 0 77.9278 8.19281 2 -6 4 0 57.9518 6.90649 1 5 -4 0 1173.46 33.9455 2 -5 4 0 1166.09 33.4547 1 4 -4 0 523.888 17.5350 2 4 -4 0 510.890 19.4445 1 -4 4 0 528.889 17.7874 1 3 -4 0 993.790 28.1083 2 3 -4 0 995.616 24.2345 3 3 -4 0 1013.10 26.8513 2 -3 4 0 984.040 27.3068 1 2 -4 0 1704.30 41.5709 1 2 -4 0 1721.42 40.2765 2 2 -4 0 1684.20 37.7970 3 -2 4 0 1659.90 41.3891 2 -2 4 0 1713.68 41.4779 1 1 -4 0 5319.95 116.428 1 1 -4 0 5152.67 112.732 3 1 -4 0 5189.72 114.713 2 -1 4 0 5261.48 115.873 2 -1 4 0 5361.00 116.280 1 0 -4 0 529.038 14.1685 2 0 -4 0 550.799 15.9047 1 0 -4 0 524.594 13.1281 3 0 4 0 545.737 14.3604 2 0 4 0 528.901 12.5716 3 0 4 0 542.356 14.6521 1 -1 -4 0 2358.97 55.5504 2 -1 -4 0 2477.34 54.0926 1 -1 -4 0 2435.33 54.1952 1 1 4 0 2421.58 54.0502 3 1 4 0 2354.39 54.4005 2 -2 -4 0 1853.34 45.7021 2 -2 -4 0 1866.88 41.9330 1 -2 -4 0 1831.82 42.4157 1 2 4 0 1882.29 43.9129 3 2 4 0 1836.93 43.4256 2 -3 -4 0 557.787 18.9400 2 -3 -4 0 551.662 14.5137 1 3 4 0 528.618 16.8143 3 -4 -4 0 356.549 15.6072 2 -5 -4 0 675.380 25.5919 2 6 -5 0 49.8399 6.51002 3 6 -5 0 54.7675 7.95846 2 -6 5 0 63.0689 8.24315 1 5 -5 0 6.43498 2.58130 3 -5 5 0 0.65500 3.19872 1 4 -5 0 125.547 7.48063 2 4 -5 0 125.100 5.63943 3 -4 5 0 133.248 8.17673 1 3 -5 0 207.591 9.64236 1 3 -5 0 238.885 9.32944 2 3 -5 0 219.782 6.99087 3 -3 5 0 241.594 10.1485 1 -3 5 0 203.486 9.88261 2 2 -5 0 9.28875 2.14703 1 2 -5 0 6.21208 0.99160 3 2 -5 0 7.01110 1.35209 2 -2 5 0 5.76817 1.82462 1 -2 5 0 4.88107 2.02036 2 1 -5 0 585.376 15.9856 2 1 -5 0 599.151 17.5716 1 -1 5 0 585.903 17.1457 2 -1 5 0 621.551 17.4613 1 0 -5 0 1621.34 38.5243 2 0 -5 0 1634.71 39.2313 1 0 5 0 1668.12 39.1404 1 0 5 0 1602.07 38.6935 2 0 5 0 1645.97 36.1497 3 -1 -5 0 125.567 5.34735 1 -1 -5 0 124.738 6.06218 2 -1 -5 0 122.119 5.06207 1 1 5 0 113.642 5.37823 3 1 5 0 126.455 5.40737 2 -2 -5 0 9.64671 1.57590 1 -2 -5 0 9.53018 1.66909 1 2 5 0 5.54393 1.42406 2 2 5 0 8.66360 2.00344 3 -3 -5 0 109.197 4.51264 1 -3 -5 0 116.634 8.08806 2 -3 -5 0 109.699 4.37496 1 3 5 0 102.261 6.52500 3 -4 -5 0 219.106 12.8368 2 -5 -5 0 -4.7665 4.86251 2 6 -6 0 47.1660 6.70812 3 6 -6 0 40.0294 5.63197 2 -6 6 0 53.4546 9.24143 1 5 -6 0 199.359 8.34541 3 5 -6 0 195.745 10.6081 2 -5 6 0 205.718 11.6450 1 4 -6 0 101.892 6.94558 2 4 -6 0 105.098 5.04965 3 -4 6 0 114.219 7.79480 1 3 -6 0 -1.9299 1.58932 2 3 -6 0 1.20759 1.13192 3 -3 6 0 6.06764 2.34944 1 2 -6 0 10.4480 2.59031 1 2 -6 0 12.7143 2.39554 2 2 -6 0 16.0599 1.53266 3 -2 6 0 16.6550 3.03054 1 -2 6 0 11.5558 2.99182 2 1 -6 0 1298.35 33.7262 1 1 -6 0 1314.09 31.7663 2 -1 6 0 1230.65 33.1049 2 -1 6 0 1329.92 33.5244 1 0 -6 0 92.2190 5.39012 1 0 -6 0 94.6837 4.94388 2 0 6 0 96.8835 3.26758 3 0 6 0 90.5338 5.14722 2 0 6 0 92.7445 5.13355 1 -1 -6 0 7.09153 1.50310 1 -1 -6 0 7.27824 1.87746 2 -1 -6 0 10.5328 1.97440 1 1 6 0 6.45024 1.42989 3 -2 -6 0 275.500 8.65603 1 -2 -6 0 283.816 9.20026 1 2 6 0 269.188 9.57126 3 -3 -6 0 232.739 7.56617 1 -3 -6 0 225.827 7.36116 1 -3 -6 0 252.793 12.5801 2 -4 -6 0 65.5086 8.80906 2 6 -7 0 641.064 19.0706 3 6 -7 0 580.115 22.0905 2 -6 7 0 623.077 23.4941 1 5 -7 0 430.531 13.3827 3 5 -7 0 452.115 16.8630 2 -5 7 0 433.487 18.4962 1 4 -7 0 204.044 9.83548 2 4 -7 0 214.577 7.31818 3 -4 7 0 211.580 11.2857 1 3 -7 0 786.853 22.1469 2 3 -7 0 758.621 18.4286 3 -3 7 0 752.672 24.0641 1 2 -7 0 1080.10 28.7612 2 -2 7 0 1112.37 30.7236 1 1 -7 0 255.811 10.8563 1 1 -7 0 260.060 9.51046 2 -1 7 0 272.065 10.9674 1 0 -7 0 1022.43 26.7667 2 0 -7 0 980.162 27.1348 1 0 -7 0 1003.99 27.3942 1 -1 -7 0 1169.72 29.6021 1 -1 -7 0 1135.15 29.8947 1 -1 -7 0 1192.74 31.9245 2 1 7 0 1162.14 27.5172 3 -2 -7 0 636.323 17.4480 1 -2 -7 0 626.932 21.5329 2 -2 -7 0 607.595 16.7394 1 2 7 0 640.119 17.6760 3 -3 -7 0 328.172 15.9934 2 -4 -7 0 964.989 33.6586 2 5 -8 0 228.433 11.2692 2 -5 8 0 216.767 13.4837 1 4 -8 0 497.833 13.7066 3 4 -8 0 516.681 17.5352 2 -4 8 0 534.735 20.2086 1 3 -8 0 195.156 8.78493 2 -3 8 0 187.367 10.5908 1 2 -8 0 74.0105 5.05990 2 -2 8 0 56.1962 6.10901 1 1 -8 0 405.506 13.3735 2 -1 8 0 383.913 14.6444 1 0 -8 0 419.792 15.1932 1 0 -8 0 465.256 15.2088 2 0 -8 0 447.487 15.3492 1 -1 -8 0 116.196 6.15213 1 -1 -8 0 112.824 6.92181 1 -1 -8 0 122.690 7.60903 2 -2 -8 0 254.339 13.0111 2 -2 -8 0 261.414 8.92698 1 -3 -8 0 352.733 17.6333 2 4 -9 0 2.07634 3.08051 2 -4 9 0 5.53677 4.75702 1 3 -9 0 4.46783 2.57906 2 -3 9 0 2.37375 4.17967 1 2 -9 0 87.2313 5.77740 2 -2 9 0 72.0111 7.46842 1 1 -9 0 82.6247 5.84553 2 0 -9 0 65.2012 5.69845 2 0 -9 0 65.7870 6.15640 1 -1 -9 0 127.751 8.69268 2 -1 -9 0 118.527 6.62018 1 -2 -9 0 48.1754 7.89024 2 3 -10 0 186.200 9.41164 2 -3 10 0 201.511 12.4829 1 2 -10 0 78.3193 6.30016 2 -2 10 0 81.2128 9.20738 1 1 -10 0 118.428 7.48353 2 1 -10 0 124.368 8.90621 1 0 -10 0 253.695 11.5074 1 0 -10 0 265.333 12.1149 2 -1 -10 0 245.531 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6.37643 2 0 -6 -1 682.796 19.9598 1 0 -6 -1 701.049 20.1160 1 0 -6 -1 732.252 19.4567 2 0 6 1 671.891 19.4366 2 -1 -6 -1 96.9907 5.90836 2 -1 -6 -1 87.9001 5.24216 1 -1 -6 -1 88.9718 4.86831 1 1 6 1 96.7245 4.23875 3 -2 -6 -1 133.209 7.90468 2 -2 -6 -1 128.260 5.55905 1 -2 -6 -1 131.309 6.16759 1 2 6 1 129.520 6.12090 3 -3 -6 -1 217.430 8.66042 1 -3 -6 -1 226.420 7.89451 1 -3 -6 -1 241.126 12.4527 2 -4 -6 -1 46.7079 8.56671 2 6 -7 -1 235.774 10.2184 3 6 -7 -1 218.848 12.2434 2 -6 7 1 227.655 13.5664 1 5 -7 -1 665.478 18.3311 3 5 -7 -1 658.970 21.8858 2 -5 7 1 678.653 23.9661 1 4 -7 -1 404.987 11.1402 3 4 -7 -1 395.695 14.4691 2 -4 7 1 395.454 16.2821 1 3 -7 -1 133.485 6.91623 2 3 -7 -1 128.037 4.31342 3 -3 7 1 130.462 8.02551 1 -2 7 1 2439.62 59.9731 1 1 -7 -1 1479.31 35.9428 2 1 -7 -1 1346.56 37.6461 1 -1 7 1 1517.34 37.9837 1 0 -7 -1 36.9790 4.04674 1 0 -7 -1 36.9654 5.22266 2 0 -7 -1 38.8753 4.84996 1 -1 -7 -1 644.712 20.1065 2 -1 -7 -1 625.187 18.2088 1 -1 -7 -1 611.964 18.5792 1 1 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794.727 21.2804 2 -3 7 -2 243.637 11.7221 1 3 -7 2 228.838 7.54020 3 3 -7 2 235.093 9.52989 2 -4 7 -2 969.363 30.2946 1 4 -7 2 967.534 24.3901 3 4 -7 2 963.242 27.5701 2 -5 7 -2 501.957 20.5631 1 5 -7 2 513.190 15.6133 3 5 -7 2 500.378 18.1703 2 -6 7 -2 111.616 18.9521 1 6 -7 2 96.6569 7.97069 3 6 -7 2 73.7065 9.47954 2 -5 -6 2 37.4572 6.44806 2 -4 -6 2 95.5136 9.21769 2 -3 -6 2 482.253 18.7149 2 2 6 -2 13.9441 2.18640 3 -2 -6 2 10.1169 2.50077 2 -2 -6 2 9.54928 1.41896 1 1 6 -2 650.982 16.6180 3 1 6 -2 627.713 17.7217 2 -1 -6 2 624.875 18.8766 2 -1 -6 2 642.516 17.0708 1 0 6 -2 832.588 22.2263 1 0 6 -2 851.061 19.9347 3 0 6 -2 816.241 22.2150 2 0 -6 2 842.461 22.0727 2 0 -6 2 816.214 22.2622 1 0 -6 2 848.975 21.1953 3 -1 6 -2 47.6790 2.81434 3 -1 6 -2 56.9043 4.80051 2 -1 6 -2 48.8204 4.18920 1 1 -6 2 52.2437 3.44934 2 1 -6 2 45.7579 4.03681 1 1 -6 2 47.2558 2.86564 3 -2 6 -2 11.9275 2.67157 1 -2 6 -2 5.24346 2.67406 2 2 -6 2 11.3293 1.71855 3 2 -6 2 11.4081 2.25357 2 2 -6 2 12.2695 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2 -5 2 183.751 7.05574 2 2 -5 2 175.203 5.71596 3 -3 5 -2 69.0871 5.64560 1 3 -5 2 75.8039 5.52097 1 3 -5 2 75.0075 5.09818 2 3 -5 2 76.6990 3.81290 3 4 -5 2 13.2965 2.63617 2 4 -5 2 18.5264 3.06302 3 -5 5 -2 309.198 14.1768 1 5 -5 2 306.234 13.6968 2 5 -5 2 326.559 11.6556 3 -6 5 -2 113.333 9.79135 1 6 -5 2 107.643 9.17367 2 6 -5 2 79.2179 7.52770 3 -6 -4 2 380.075 18.6807 2 -5 -4 2 246.419 13.6573 2 -4 -4 2 357.183 15.4845 2 3 4 -2 2429.83 59.4407 2 3 4 -2 2580.16 60.5558 3 -3 -4 2 2661.38 63.1863 2 2 4 -2 447.885 13.4064 3 2 4 -2 431.937 12.9022 2 -2 -4 2 475.176 14.8948 2 1 4 -2 703.470 16.7991 1 1 4 -2 711.923 17.6516 3 1 4 -2 691.395 17.6227 2 -1 -4 2 691.560 18.2194 3 -1 -4 2 673.268 18.5203 2 -1 -4 2 695.635 16.8076 1 0 4 -2 1607.21 35.5108 3 0 4 -2 1577.40 36.5894 2 0 4 -2 1575.57 36.8358 1 0 -4 2 1567.43 36.4761 2 0 -4 2 1587.15 36.9387 1 0 -4 2 1580.91 36.0929 3 -1 4 -2 2062.63 46.7278 2 -1 4 -2 1965.85 44.7493 3 -1 4 -2 2047.15 47.1688 1 1 -4 2 1967.96 45.5058 2 1 -4 2 2017.94 47.0542 1 1 -4 2 1990.05 44.4618 3 -2 4 -2 1283.87 32.8821 2 -2 4 -2 1287.51 33.0356 1 2 -4 2 1282.49 32.8722 1 2 -4 2 1298.26 29.9173 3 2 -4 2 1344.28 31.8352 2 -3 4 -2 2655.63 63.6414 1 3 -4 2 2682.53 62.7039 2 3 -4 2 2628.89 63.2343 1 3 -4 2 2673.53 60.0685 3 3 -4 2 2667.83 64.2975 2 -4 4 -2 1566.53 41.6188 1 4 -4 2 1612.93 38.4880 3 4 -4 2 1561.10 41.1465 2 -5 4 -2 62.1822 6.67360 1 5 -4 2 61.6544 5.24748 3 5 -4 2 65.1294 6.35618 2 -6 4 -2 310.505 14.8558 1 6 -4 2 311.728 12.7677 3 6 -4 2 314.617 15.0199 2 -6 -3 2 65.4862 9.58304 2 -5 -3 2 288.008 14.2283 2 -4 -3 2 1271.05 36.2871 2 3 3 -2 404.214 12.9889 2 3 3 -2 394.140 13.2546 3 -3 -3 2 400.094 14.4701 2 2 3 -2 523.268 14.4689 2 2 3 -2 530.147 14.9060 3 -2 -3 2 514.260 15.6468 2 1 3 -2 3031.48 64.9531 1 1 3 -2 3031.74 66.4718 3 -1 -3 2 2974.86 66.9383 2 -1 -3 2 2948.32 66.8276 3 -1 -3 2 2986.35 64.9130 1 0 3 -2 1618.02 36.3274 2 0 3 -2 1599.83 35.7715 3 0 -3 2 1599.99 36.6471 1 0 -3 2 1614.70 36.2919 2 0 -3 2 1612.90 36.0837 3 -1 3 -2 695.805 16.5231 3 -1 3 -2 679.857 18.0767 1 -1 3 -2 696.803 17.6908 2 1 -3 2 682.104 16.9755 2 1 -3 2 693.378 16.2027 3 -2 3 -2 2843.93 65.4977 1 2 -3 2 2857.20 64.7790 2 2 -3 2 2920.69 65.4262 1 2 -3 2 2770.22 62.9303 3 -3 3 -2 3991.66 90.2450 1 3 -3 2 4036.30 91.1714 2 3 -3 2 3871.42 89.8195 2 3 -3 2 3893.00 87.5369 3 3 -3 2 3892.72 89.6016 1 -4 3 -2 246.608 10.7101 1 4 -3 2 243.052 11.5988 2 4 -3 2 262.532 11.2268 2 4 -3 2 234.715 10.1536 1 5 -3 2 12.8108 3.36246 2 -6 3 -2 614.964 22.2938 1 6 -3 2 658.304 24.1240 2 -6 -2 2 435.105 19.7420 2 5 2 -2 136.949 5.81381 1 -5 -2 2 131.376 9.26473 2 -5 -2 2 141.679 5.47263 1 4 2 -2 14.8655 1.84893 1 -4 -2 2 18.8245 3.83138 2 3 2 -2 18.7941 2.83853 2 3 2 -2 19.4790 2.89625 3 -3 -2 2 20.6063 3.09436 2 2 2 -2 1416.86 34.1592 2 2 2 -2 1458.19 34.4586 3 -2 -2 2 1444.95 35.1668 2 1 2 -2 37.3044 2.02563 2 1 2 -2 35.4635 2.13460 3 -1 -2 2 38.6054 2.38300 3 -1 -2 2 34.5877 2.16227 2 0 2 -2 13.4286 1.33917 1 0 2 -2 16.0350 1.13895 3 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-2 14 94.3308 9.08328 3 3 2 -14 43.8124 5.98363 1 -3 -2 14 52.6442 7.23556 3 2 2 -14 8.86006 3.45636 1 -2 -2 14 3.81031 3.39307 3 1 2 -14 318.571 13.6466 1 -1 -2 14 318.683 13.4845 3 0 2 -14 69.1236 7.53227 1 0 -2 14 83.5887 6.73999 3 -1 2 -14 -1.4911 3.55416 1 1 -2 14 5.42869 2.79999 3 -2 2 -14 7.81530 4.23871 1 2 -2 14 2.42344 3.12050 3 4 1 -14 43.8985 6.61253 1 -4 -1 14 29.3387 5.31898 3 3 1 -14 373.950 14.6389 1 -3 -1 14 386.872 16.1370 3 2 1 -14 396.152 15.3864 1 -2 -1 14 372.328 15.3984 3 1 1 -14 547.956 19.3140 1 -1 -1 14 541.066 18.8413 3 0 1 -14 51.2536 6.57073 1 0 -1 14 49.5396 5.79695 3 -1 1 -14 412.364 17.4201 1 1 -1 14 409.332 14.7634 3 -2 1 -14 7.14980 4.67257 1 2 -1 14 15.3210 3.56574 3 5 0 -14 25.0145 5.38795 1 4 0 -14 387.869 15.3740 1 -4 0 14 367.329 16.1291 3 3 0 -14 391.465 15.5284 1 -3 0 14 391.507 15.8573 3 2 0 -14 244.059 11.8220 1 -2 0 14 263.252 11.8536 3 1 0 -14 255.422 12.3203 1 -1 0 14 255.058 11.3941 3 0 0 -14 1041.36 31.2059 1 0 0 14 985.767 28.4104 3 -1 0 -14 371.594 16.7136 1 1 0 14 382.434 13.8540 3 -2 0 -14 44.1653 8.13750 1 2 0 14 29.3356 5.37170 3 4 -1 -14 139.429 9.83681 1 -4 1 14 134.311 9.76756 3 3 -1 -14 2.72174 3.46217 1 -3 1 14 -1.7591 3.65289 3 2 -1 -14 25.2763 4.32019 1 -2 1 14 38.5601 5.69701 3 1 -1 -14 228.331 11.9195 1 -1 1 14 248.054 10.8863 3 0 -1 -14 62.2064 7.34057 1 0 1 14 43.8267 5.26305 3 -1 -1 -14 136.902 10.2085 1 1 1 14 150.167 7.99342 3 4 -2 -14 108.927 9.62058 1 3 -2 -14 88.4289 7.99754 1 -3 2 14 64.8191 7.05535 3 2 -2 -14 55.6722 6.96582 1 -2 2 14 73.7402 6.27720 3 1 -2 -14 1.73403 3.39054 1 -1 2 14 -0.7999 2.95823 3 0 -2 -14 86.2722 8.83243 1 0 2 14 88.8403 6.53335 3 -1 -2 -14 258.581 14.0791 1 1 2 14 259.724 10.6454 3 4 -3 -14 551.678 20.8969 1 3 -3 -14 144.695 10.1427 1 2 -3 -14 68.8758 7.85004 1 -2 3 14 77.4443 6.77383 3 1 -3 -14 420.866 17.4526 1 -1 3 14 407.545 16.0571 3 0 -3 -14 370.405 16.6113 1 0 3 14 403.693 14.0806 3 2 -4 -14 210.558 14.1186 1 1 6 -15 95.0769 10.5478 1 0 6 -15 2.69688 5.27040 1 2 5 -15 247.178 13.1686 1 -2 -5 15 280.178 14.0566 3 -1 -5 15 38.8425 7.43662 3 0 5 -15 119.435 10.9877 1 0 -5 15 142.787 9.16369 3 -1 5 -15 476.438 20.0730 1 -3 -4 15 333.298 16.2319 3 2 4 -15 414.875 16.5664 1 -2 -4 15 436.581 17.9009 3 1 4 -15 637.545 22.0833 1 -1 -4 15 635.117 22.5538 3 0 4 -15 511.872 20.0987 1 0 -4 15 520.534 18.8855 3 -1 4 -15 244.133 13.7658 1 1 -4 15 228.788 11.2517 3 3 3 -15 133.355 9.51048 1 -3 -3 15 120.647 10.2689 3 2 3 -15 228.415 12.0208 1 -2 -3 15 234.434 12.8979 3 1 3 -15 260.324 13.0701 1 -1 -3 15 249.614 12.6660 3 0 3 -15 17.7157 4.76017 1 0 -3 15 13.3642 3.82310 3 -1 3 -15 300.658 15.1345 1 1 -3 15 285.929 12.6984 3 4 2 -15 65.9297 8.52346 1 -4 -2 15 80.8620 10.0774 3 3 2 -15 108.414 8.12430 1 -3 -2 15 79.4427 9.02431 3 2 2 -15 0.21929 3.90196 1 -2 -2 15 9.23911 4.44407 3 1 2 -15 7.99879 4.14653 1 -1 -2 15 -2.7075 3.57666 3 0 2 -15 132.545 9.80916 1 0 -2 15 147.507 8.82286 3 -1 2 -15 112.866 9.87563 1 1 -2 15 124.741 8.06576 3 4 1 -15 334.528 14.5284 1 -4 -1 15 333.523 16.2946 3 3 1 -15 95.7004 8.12608 1 -3 -1 15 100.084 9.16401 3 2 1 -15 169.190 10.3525 1 -2 -1 15 169.133 10.4062 3 1 1 -15 549.115 20.0421 1 -1 -1 15 516.543 19.0901 3 0 1 -15 328.947 15.3102 1 0 -1 15 318.137 13.5516 3 -1 1 -15 282.722 14.6055 1 1 -1 15 297.373 12.3567 3 4 0 -15 135.026 10.3828 1 -4 0 15 139.633 10.5891 3 3 0 -15 299.397 13.9492 1 -3 0 15 312.750 14.4731 3 2 0 -15 685.455 23.4499 1 -2 0 15 705.960 23.1286 3 1 0 -15 147.638 9.92982 1 -1 0 15 141.135 9.14373 3 0 0 -15 297.123 14.8654 1 0 0 15 310.669 12.9302 3 -1 0 -15 389.087 18.0197 1 1 0 15 423.952 15.0150 3 4 -1 -15 163.792 10.8701 1 -4 1 15 150.324 10.7503 3 3 -1 -15 28.9197 5.46583 1 -3 1 15 46.8463 7.74187 3 2 -1 -15 53.4125 7.60291 1 -2 1 15 67.3327 7.17829 3 1 -1 -15 13.8879 4.32478 1 -1 1 15 16.7524 3.77852 3 0 -1 -15 147.303 10.3673 1 0 1 15 141.603 8.54245 3 3 -2 -15 18.0119 4.84597 1 -3 2 15 8.36573 4.52423 3 2 -2 -15 169.314 11.1521 1 -2 2 15 180.223 9.88861 3 1 -2 -15 174.350 10.8454 1 -1 2 15 154.802 9.37381 3 0 2 15 2.54736 3.49090 3 2 4 -16 323.824 15.8769 1 1 4 -16 141.341 11.0656 1 -1 -4 16 119.341 10.5400 3 0 4 -16 419.313 18.5760 1 2 3 -16 38.1358 6.15595 1 -2 -3 16 51.9332 8.60526 3 1 3 -16 318.475 15.5830 1 -1 -3 16 327.775 14.9374 3 0 3 -16 175.400 12.3888 1 0 -3 16 203.225 10.9543 3 3 2 -16 105.174 9.61975 1 -3 -2 16 125.470 10.9151 3 2 2 -16 159.984 10.6345 1 -2 -2 16 202.430 12.1240 3 1 2 -16 18.9941 4.92318 1 -1 -2 16 17.7472 4.65575 3 0 2 -16 28.2855 5.63779 1 3 1 -16 454.618 18.0329 1 -3 -1 16 434.850 18.6132 3 2 1 -16 156.810 10.8203 1 -2 -1 16 163.365 10.9778 3 1 1 -16 31.8365 5.28050 1 0 1 -16 566.189 21.9458 1 0 -1 16 551.051 19.6134 3 3 0 -16 66.4784 8.44179 1 -3 0 16 52.1957 9.32954 3 2 0 -16 214.596 12.5622 1 -2 0 16 223.654 12.1947 3 1 0 -16 286.746 14.2229 1 -1 0 16 262.637 13.0350 3 2 -1 -16 56.1962 8.15576 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6323 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71124 5.611 8.358 12.780 99.240 101.071 98.723 ) ; _shelx_hkl_checksum 32707 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Pd1 Pd 0.0000 0.0000 0.0000 0.01324(7) Uani 1 2 d S T P Cl1 Cl -0.00525(9) 0.27657(6) 0.00717(4) 0.01898(11) Uani 1 1 d . . . S4 S 0.70616(9) 0.60892(6) 0.28733(4) 0.02040(12) Uani 1 1 d . . . O3 O 0.8431(3) 0.78731(18) 0.32495(11) 0.0227(3) Uani 1 1 d . . . O1 O 1.0698(3) 0.2754(2) 0.41406(12) 0.0259(3) Uani 1 1 d . . . O2 O 0.8178(3) 0.13832(19) 0.50085(11) 0.0218(3) Uani 1 1 d . . . H2 H 0.9406 0.1679 0.5539 0.033 Uiso 1 1 calc GR . . N1 N 0.2803(3) 0.0566(2) 0.13286(13) 0.0147(3) Uani 1 1 d . . . C5 C 0.2468(4) 0.0126(2) 0.22707(15) 0.0166(4) Uani 1 1 d . . . H5 H 0.0910 -0.0489 0.2293 0.020 Uiso 1 1 calc R . . C4 C 0.5018(4) 0.1420(2) 0.12941(15) 0.0164(4) Uani 1 1 d . . . H4 H 0.5246 0.1732 0.0630 0.020 Uiso 1 1 calc R . . C15 C 0.5444(5) 0.6004(3) 0.15196(18) 0.0328(6) Uani 1 1 d . . . H15A H 0.4568 0.6935 0.1501 0.049 Uiso 1 1 calc GR . . H15B H 0.4243 0.4961 0.1265 0.049 Uiso 1 1 calc GR . . H15C H 0.6625 0.6068 0.1044 0.049 Uiso 1 1 calc GR . . C3 C 0.6968(4) 0.1857(2) 0.21928(15) 0.0163(4) Uani 1 1 d . . . H3 H 0.8525 0.2446 0.2146 0.020 Uiso 1 1 calc R . . C1 C 0.8740(4) 0.1934(2) 0.41562(15) 0.0175(4) Uani 1 1 d . . . C2 C 0.6619(4) 0.1422(2) 0.31698(15) 0.0151(4) Uani 1 1 d . . . C6 C 0.4333(4) 0.0548(2) 0.32023(15) 0.0174(4) Uani 1 1 d . . . H6 H 0.4051 0.0242 0.3861 0.021 Uiso 1 1 calc R . . C25 C 0.4501(5) 0.5926(4) 0.3508(2) 0.0382(6) Uani 1 1 d . . . H25A H 0.5104 0.6187 0.4301 0.057 Uiso 1 1 calc GR . . H25B H 0.3536 0.4796 0.3286 0.057 Uiso 1 1 calc GR . . H25C H 0.3449 0.6706 0.3286 0.057 Uiso 1 1 calc GR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01101(11) 0.01571(12) 0.01150(11) 0.00437(7) -0.00012(7) -0.00060(8) Cl1 0.0180(2) 0.0167(2) 0.0204(2) 0.00567(17) 0.00052(18) 0.00023(18) S4 0.0172(3) 0.0193(3) 0.0211(3) 0.00355(19) -0.00165(19) 0.0005(2) O3 0.0242(8) 0.0213(7) 0.0165(7) 0.0042(6) -0.0031(6) -0.0050(6) O1 0.0157(8) 0.0370(9) 0.0202(7) 0.0083(6) -0.0013(6) -0.0061(7) O2 0.0161(7) 0.0317(8) 0.0133(7) 0.0060(6) -0.0018(5) -0.0035(6) N1 0.0128(8) 0.0162(8) 0.0142(7) 0.0051(6) 0.0007(6) 0.0003(6) C5 0.0131(9) 0.0192(9) 0.0177(9) 0.0065(7) 0.0031(7) 0.0002(8) C4 0.0154(9) 0.0189(10) 0.0145(9) 0.0046(7) 0.0026(7) 0.0008(8) C15 0.0288(13) 0.0418(14) 0.0173(11) 0.0019(9) -0.0039(9) -0.0105(11) C3 0.0134(9) 0.0182(9) 0.0165(9) 0.0039(7) 0.0030(7) 0.0007(7) C1 0.0166(10) 0.0197(10) 0.0144(9) 0.0022(7) 0.0004(7) 0.0033(8) C2 0.0135(9) 0.0167(9) 0.0144(9) 0.0029(7) 0.0007(7) 0.0036(7) C6 0.0167(10) 0.0207(10) 0.0145(9) 0.0054(7) 0.0027(7) 0.0015(8) C25 0.0348(14) 0.0434(15) 0.0343(13) 0.0079(11) 0.0147(11) -0.0083(12) 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 Cl1 Pd1 Cl1 180.00(2) . 2 N1 Pd1 Cl1 90.06(5) . . N1 Pd1 Cl1 90.06(5) 2 2 N1 Pd1 Cl1 89.94(5) 2 . N1 Pd1 Cl1 89.94(5) . 2 N1 Pd1 N1 180.0 2 . O3 S4 C15 104.13(10) . . O3 S4 C25 105.97(11) . . C15 S4 C25 98.87(13) . . C5 N1 Pd1 120.48(13) . . C4 N1 Pd1 120.34(13) . . C4 N1 C5 119.17(16) . . N1 C5 C6 121.60(18) . . N1 C4 C3 122.03(18) . . C4 C3 C2 118.93(18) . . O1 C1 O2 125.44(18) . . O1 C1 C2 122.48(18) . . O2 C1 C2 112.08(17) . . C3 C2 C1 118.74(18) . . C6 C2 C3 118.82(17) . . C6 C2 C1 122.43(17) . . C5 C6 C2 119.44(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pd1 Cl1 2.2981(5) . Pd1 Cl1 2.2982(5) 2 Pd1 N1 2.0120(15) 2 Pd1 N1 2.0120(15) . S4 O3 1.5205(15) . S4 C15 1.773(2) . S4 C25 1.773(3) . O1 C1 1.205(3) . O2 C1 1.318(2) . N1 C5 1.348(2) . N1 C4 1.344(3) . C5 C6 1.379(3) . C4 C3 1.379(3) . C3 C2 1.392(3) . C1 C2 1.507(3) . C2 C6 1.384(3) .