#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:40:53 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705301.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_7705301 loop_ _publ_author_name 'Exp\'osito, J. Emilio' 'Aull\'on, Gabriel' 'Bardaji, Manuel' 'Miguel, Jesus Angel' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02494E _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C28 H19 N O Pd S2' _chemical_formula_sum 'C28 H19 N O Pd S2' _chemical_formula_weight 555.96 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2020-07-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-10 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.8850(4) _cell_length_b 15.3326(3) _cell_length_c 7.25084(18) _cell_measurement_reflns_used 3715 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.2776 _cell_measurement_theta_min 2.4366 _cell_volume 2210.70(8) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.4757 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.863 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -15.00 58.00 1.0000 5.0900 omega____ theta____ kappa____ phi______ frames - 12.4346 0.0000 -60.0000 73 #__ type_ start__ end____ width___ exp.time_ 2 omega 9.00 36.00 1.0000 5.0900 omega____ theta____ kappa____ phi______ frames - 12.4346 -123.0000 20.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega -71.00 -25.00 1.0000 5.0900 omega____ theta____ kappa____ phi______ frames - 12.4346 0.0000 -60.0000 46 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0172633000 _diffrn_orient_matrix_UB_12 -0.0285468000 _diffrn_orient_matrix_UB_13 -0.0606680000 _diffrn_orient_matrix_UB_21 0.0310395000 _diffrn_orient_matrix_UB_22 0.0122425000 _diffrn_orient_matrix_UB_23 0.0407112000 _diffrn_orient_matrix_UB_31 -0.0032749000 _diffrn_orient_matrix_UB_32 -0.0342552000 _diffrn_orient_matrix_UB_33 0.0651209000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0379 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.863 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 8215 _diffrn_reflns_point_group_measured_fraction_full 0.757 _diffrn_reflns_point_group_measured_fraction_max 0.624 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.342 _diffrn_reflns_theta_min 2.441 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_density_diffrn 1.670 _exptl_crystal_description block _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.2969 _exptl_crystal_size_mid 0.2528 _exptl_crystal_size_min 0.1921 _refine_diff_density_max 0.274 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.079 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.23(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 3776 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0308 _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^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0675 _reflns_Friedel_coverage 0.345 _reflns_Friedel_fraction_full 0.470 _reflns_Friedel_fraction_max 0.346 _reflns_number_gt 3205 _reflns_number_total 3776 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 8 _cod_database_code 7705301 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C28 H19 N O S2 Pd' _chemical_oxdiff_usercomment THF/hexano _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.77(4) 0.23(4) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C7(H7), C8(H8), C9(H9), C20(H20), C19(H19), C18(H18), C16(H16), C15(H15), C14(H14), C22(H22), C24(H24), C25(H25) 3.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C28(H28A,H28B,H28C) ; _shelx_res_file ; TITL je265 in Pna2(1) je265.res created by SHELXL-2018/3 at 17:25:13 on 08-Jul-2020 CELL 0.71073 19.885012 15.332625 7.250842 90 90 90 ZERR 4 0.000414 0.000252 0.000178 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H N O Pd S UNIT 112 76 4 4 4 8 L.S. 4 PLAN 5 BOND MORE -1 BOND $H CONF fmap 2 acta 52 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.028300 BASF 0.23126 FVAR 2.22478 PD1 5 0.537224 0.766396 0.511630 11.00000 0.02730 0.03074 = 0.04615 -0.00102 -0.00018 0.00073 N1 3 0.622252 0.837604 0.475148 11.00000 0.02421 0.03692 = 0.04218 -0.00138 -0.00133 0.00096 C2 1 0.497210 0.883392 0.471489 11.00000 0.02749 0.03326 = 0.03608 -0.00270 0.00071 -0.00068 S2 6 0.574762 0.617215 0.570109 11.00000 0.03533 0.04026 = 0.07966 0.00478 -0.00007 0.00570 S1 6 0.440311 0.683811 0.533379 11.00000 0.03036 0.03657 = 0.07894 -0.00017 0.00469 -0.00042 C3 1 0.428471 0.900563 0.459236 11.00000 0.03374 0.02796 = 0.04848 0.00165 0.00381 -0.00254 AFIX 43 H3 2 0.398552 0.854196 0.469479 11.00000 -1.20000 AFIX 0 C1 1 0.543285 0.951768 0.459084 11.00000 0.02442 0.03760 = 0.03402 0.00073 -0.00134 -0.00134 C6 1 0.519062 1.040275 0.465423 11.00000 0.02823 0.03294 = 0.03690 -0.00098 0.00301 -0.00266 C7 1 0.561110 1.112779 0.498356 11.00000 0.03224 0.03994 = 0.04431 0.00082 -0.00350 -0.00781 AFIX 43 H7 2 0.607105 1.104372 0.513317 11.00000 -1.20000 AFIX 0 C8 1 0.535161 1.195161 0.508558 11.00000 0.04301 0.03299 = 0.06146 0.00120 0.00026 -0.01108 AFIX 43 H8 2 0.563656 1.242006 0.531612 11.00000 -1.20000 AFIX 0 C9 1 0.467336 1.209712 0.485134 11.00000 0.04721 0.03060 = 0.05971 0.00024 0.00308 -0.00203 AFIX 43 H9 2 0.451399 1.266734 0.486397 11.00000 -1.20000 AFIX 0 C10 1 0.422343 1.142312 0.459867 11.00000 0.03849 0.03273 = 0.03923 0.00373 0.00495 0.00138 C5 1 0.448368 1.055464 0.451039 11.00000 0.03387 0.03212 = 0.03058 0.00254 0.00249 -0.00351 C4 1 0.402942 0.983013 0.432679 11.00000 0.02570 0.03359 = 0.03517 -0.00284 0.00148 -0.00013 C13 1 0.331926 0.998887 0.390834 11.00000 0.02826 0.04065 = 0.03470 0.00260 0.00519 -0.00333 C12 1 0.306621 1.086161 0.398283 11.00000 0.03096 0.04235 = 0.03370 0.00351 0.00424 0.00415 C11 1 0.349938 1.157400 0.440822 11.00000 0.04067 0.03704 = 0.03595 0.00172 0.00354 0.00425 C20 1 0.321261 1.239753 0.455364 11.00000 0.05153 0.03931 = 0.06559 -0.00635 0.00273 0.00666 AFIX 43 H20 2 0.348475 1.287090 0.484708 11.00000 -1.20000 AFIX 0 C19 1 0.252837 1.253127 0.427101 11.00000 0.05444 0.04692 = 0.08480 -0.00327 0.00153 0.02417 AFIX 43 H19 2 0.235259 1.308959 0.440810 11.00000 -1.20000 AFIX 0 C18 1 0.211324 1.187089 0.380280 11.00000 0.03774 0.06123 = 0.07013 0.00533 0.00339 0.01662 AFIX 43 H18 2 0.165976 1.197957 0.358922 11.00000 -1.20000 AFIX 0 C17 1 0.236958 1.101000 0.363663 11.00000 0.03194 0.05487 = 0.03847 0.00470 0.00385 0.00726 C16 1 0.195354 1.030043 0.312051 11.00000 0.02480 0.06493 = 0.05060 0.00149 0.00426 0.00118 AFIX 43 H16 2 0.150081 1.039479 0.286801 11.00000 -1.20000 AFIX 0 C15 1 0.221107 0.948896 0.299378 11.00000 0.02910 0.06087 = 0.05091 0.00386 -0.00441 -0.00595 AFIX 43 H15 2 0.193515 0.903015 0.263156 11.00000 -1.20000 AFIX 0 C14 1 0.288778 0.932775 0.339980 11.00000 0.02682 0.04347 = 0.05084 0.00507 0.00025 -0.00270 AFIX 43 H14 2 0.305045 0.876018 0.332458 11.00000 -1.20000 AFIX 0 C21 1 0.613142 0.924148 0.439605 11.00000 0.03088 0.03981 = 0.03158 -0.00234 0.00034 -0.00202 C22 1 0.668380 0.972817 0.378598 11.00000 0.03027 0.04688 = 0.03887 -0.00385 0.00007 -0.00981 AFIX 43 H22 2 0.662137 1.030725 0.344494 11.00000 -1.20000 AFIX 0 C23 1 0.732107 0.936765 0.367830 11.00000 0.02857 0.06000 = 0.03684 -0.00743 -0.00015 -0.00603 C24 1 0.739647 0.849601 0.412316 11.00000 0.02761 0.05794 = 0.05343 -0.00263 -0.00436 0.00753 AFIX 43 H24 2 0.781853 0.823510 0.409238 11.00000 -1.20000 AFIX 0 C25 1 0.683813 0.802177 0.461118 11.00000 0.02911 0.04451 = 0.05388 -0.00315 -0.00043 0.00372 AFIX 43 H25 2 0.688852 0.742987 0.485495 11.00000 -1.20000 AFIX 0 C26 1 0.790802 0.991618 0.306086 11.00000 0.03045 0.07725 = 0.05518 0.00351 0.00937 -0.00559 AFIX 137 H26A 2 0.815889 0.960639 0.213866 11.00000 -1.50000 H26B 2 0.819361 1.003697 0.409734 11.00000 -1.50000 H26C 2 0.774555 1.045468 0.255319 11.00000 -1.50000 AFIX 0 C27 1 0.492091 0.597280 0.565814 11.00000 0.03841 0.03664 = 0.04540 0.00352 0.00093 -0.00109 O1 4 0.463959 0.519300 0.580734 11.00000 0.05562 0.03544 = 0.07106 0.00248 0.00577 -0.00368 C28 1 0.507176 0.443419 0.595065 11.00000 0.08806 0.03744 = 0.08078 0.00955 0.00817 0.00284 AFIX 137 H28A 2 0.541676 0.454244 0.684807 11.00000 -1.50000 H28B 2 0.527486 0.431893 0.477450 11.00000 -1.50000 H28C 2 0.480977 0.393886 0.632424 11.00000 -1.50000 AFIX 0 HKLF 4 REM je265 in Pna2(1) REM wR2 = 0.0675, GooF = S = 1.068, Restrained GooF = 1.068 for all data REM R1 = 0.0308 for 3205 Fo > 4sig(Fo) and 0.0416 for all 3776 data REM 301 parameters refined using 1 restraints END WGHT 0.0283 0.0000 REM Highest difference peak 0.274, deepest hole -0.602, 1-sigma level 0.079 Q1 1 0.4463 0.9786 0.2205 11.00000 0.05 0.27 Q2 1 0.5406 0.6989 0.5133 11.00000 0.05 0.27 Q3 1 0.6812 0.7337 0.5845 11.00000 0.05 0.27 Q4 1 0.3902 0.7670 0.5143 11.00000 0.05 0.27 Q5 1 0.1107 0.8846 0.2262 11.00000 0.05 0.26 ; _shelx_res_checksum 57436 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 0.53722(2) 0.76640(2) 0.51163(10) 0.03473(11) Uani 1 1 d . . . . . N1 N 0.62225(16) 0.8376(2) 0.4751(6) 0.0344(11) Uani 1 1 d . . . . . C2 C 0.4972(2) 0.8834(2) 0.4715(7) 0.0323(13) Uani 1 1 d . . . . . S2 S 0.57476(6) 0.61721(8) 0.5701(2) 0.0518(5) Uani 1 1 d . . . . . S1 S 0.44031(6) 0.68381(7) 0.5334(3) 0.0486(4) Uani 1 1 d . . . . . C3 C 0.4285(2) 0.9006(2) 0.4592(7) 0.0367(13) Uani 1 1 d . . . . . H3 H 0.398552 0.854196 0.469479 0.044 Uiso 1 1 calc R . . . . C1 C 0.5433(2) 0.9518(3) 0.4591(6) 0.0320(12) Uani 1 1 d . . . . . C6 C 0.5191(2) 1.0403(3) 0.4654(7) 0.0327(12) Uani 1 1 d . . . . . C7 C 0.5611(2) 1.1128(2) 0.4984(10) 0.0388(11) Uani 1 1 d . . . . . H7 H 0.607105 1.104372 0.513317 0.047 Uiso 1 1 calc R . . . . C8 C 0.5352(2) 1.1952(2) 0.5086(16) 0.0458(11) Uani 1 1 d . . . . . H8 H 0.563656 1.242006 0.531612 0.055 Uiso 1 1 calc R . . . . C9 C 0.4673(2) 1.2097(3) 0.4851(13) 0.0458(18) Uani 1 1 d . . . . . H9 H 0.451399 1.266734 0.486397 0.055 Uiso 1 1 calc R . . . . C10 C 0.4223(2) 1.1423(3) 0.4599(7) 0.0368(12) Uani 1 1 d . . . . . C5 C 0.4484(2) 1.0555(3) 0.4510(6) 0.0322(11) Uani 1 1 d . . . . . C4 C 0.4029(2) 0.9830(3) 0.4327(7) 0.0315(10) Uani 1 1 d . . . . . C13 C 0.3319(2) 0.9989(3) 0.3908(7) 0.0345(11) Uani 1 1 d . . . . . C12 C 0.3066(2) 1.0862(3) 0.3983(7) 0.0357(12) Uani 1 1 d . . . . . C11 C 0.3499(2) 1.1574(3) 0.4408(7) 0.0379(12) Uani 1 1 d . . . . . C20 C 0.3213(3) 1.2398(3) 0.4554(9) 0.0521(17) Uani 1 1 d . . . . . H20 H 0.348475 1.287090 0.484708 0.063 Uiso 1 1 calc R . . . . C19 C 0.2528(3) 1.2531(3) 0.4271(10) 0.0621(19) Uani 1 1 d . . . . . H19 H 0.235259 1.308959 0.440810 0.074 Uiso 1 1 calc R . . . . C18 C 0.2113(3) 1.1871(4) 0.3803(9) 0.0564(16) Uani 1 1 d . . . . . H18 H 0.165976 1.197957 0.358922 0.068 Uiso 1 1 calc R . . . . C17 C 0.2370(3) 1.1010(3) 0.3637(7) 0.0418(13) Uani 1 1 d . . . . . C16 C 0.1954(3) 1.0300(4) 0.3121(9) 0.0468(14) Uani 1 1 d . . . . . H16 H 0.150081 1.039479 0.286801 0.056 Uiso 1 1 calc R . . . . C15 C 0.2211(2) 0.9489(4) 0.2994(9) 0.0470(14) Uani 1 1 d . . . . . H15 H 0.193515 0.903015 0.263156 0.056 Uiso 1 1 calc R . . . . C14 C 0.2888(2) 0.9328(3) 0.3400(8) 0.0404(12) Uani 1 1 d . . . . . H14 H 0.305045 0.876018 0.332458 0.048 Uiso 1 1 calc R . . . . C21 C 0.6131(2) 0.9241(3) 0.4396(7) 0.0341(11) Uani 1 1 d . . . . . C22 C 0.6684(2) 0.9728(3) 0.3786(7) 0.0387(12) Uani 1 1 d . . . . . H22 H 0.662137 1.030725 0.344494 0.046 Uiso 1 1 calc R . . . . C23 C 0.7321(2) 0.9368(3) 0.3678(7) 0.0418(13) Uani 1 1 d . . . . . C24 C 0.7396(3) 0.8496(3) 0.4123(7) 0.0463(14) Uani 1 1 d . . . . . H24 H 0.781853 0.823510 0.409238 0.056 Uiso 1 1 calc R . . . . C25 C 0.6838(2) 0.8022(3) 0.4611(7) 0.0425(14) Uani 1 1 d . . . . . H25 H 0.688852 0.742987 0.485495 0.051 Uiso 1 1 calc R . . . . C26 C 0.7908(3) 0.9916(4) 0.3061(9) 0.0543(16) Uani 1 1 d . . . . . H26A H 0.815889 0.960639 0.213866 0.081 Uiso 1 1 calc GR . . . . H26B H 0.819361 1.003697 0.409734 0.081 Uiso 1 1 calc GR . . . . H26C H 0.774555 1.045468 0.255319 0.081 Uiso 1 1 calc GR . . . . C27 C 0.4921(2) 0.5973(3) 0.5658(7) 0.0401(13) Uani 1 1 d . . . . . O1 O 0.46396(17) 0.5193(2) 0.5807(6) 0.0540(12) Uani 1 1 d . . . . . C28 C 0.5072(3) 0.4434(3) 0.5951(10) 0.069(2) Uani 1 1 d . . . . . H28A H 0.541676 0.454244 0.684807 0.103 Uiso 1 1 calc GR . . . . H28B H 0.527486 0.431893 0.477450 0.103 Uiso 1 1 calc GR . . . . H28C H 0.480977 0.393886 0.632424 0.103 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 0.02730(17) 0.03074(15) 0.0462(2) -0.0010(3) -0.0002(3) 0.00073(11) N1 0.0242(18) 0.0369(16) 0.042(3) -0.001(2) -0.0013(19) 0.0010(13) C2 0.027(2) 0.0333(19) 0.036(4) -0.003(2) 0.001(2) -0.0007(16) S2 0.0353(7) 0.0403(6) 0.0797(13) 0.0048(7) -0.0001(7) 0.0057(5) S1 0.0304(6) 0.0366(5) 0.0789(12) -0.0002(9) 0.0047(9) -0.0004(4) C3 0.034(3) 0.0280(19) 0.048(4) 0.002(2) 0.004(2) -0.0025(17) C1 0.024(2) 0.038(2) 0.034(3) 0.001(2) -0.001(2) -0.0013(16) C6 0.028(2) 0.033(2) 0.037(3) -0.001(2) 0.003(2) -0.0027(16) C7 0.032(2) 0.040(2) 0.044(3) 0.001(4) -0.003(3) -0.0078(16) C8 0.043(3) 0.0330(19) 0.061(3) 0.001(5) 0.000(4) -0.0111(17) C9 0.047(3) 0.0306(19) 0.060(6) 0.000(4) 0.003(3) -0.0020(17) C10 0.038(3) 0.033(2) 0.039(3) 0.004(2) 0.005(2) 0.0014(18) C5 0.034(3) 0.032(2) 0.031(3) 0.003(2) 0.002(2) -0.0035(17) C4 0.026(2) 0.034(2) 0.035(3) -0.003(2) 0.001(2) -0.0001(18) C13 0.028(3) 0.041(2) 0.035(3) 0.003(2) 0.005(2) -0.003(2) C12 0.031(3) 0.042(2) 0.034(3) 0.004(2) 0.004(2) 0.004(2) C11 0.041(3) 0.037(2) 0.036(3) 0.002(2) 0.004(2) 0.004(2) C20 0.052(3) 0.039(2) 0.066(5) -0.006(3) 0.003(3) 0.007(2) C19 0.054(4) 0.047(3) 0.085(5) -0.003(3) 0.002(4) 0.024(3) C18 0.038(3) 0.061(3) 0.070(5) 0.005(3) 0.003(3) 0.017(3) C17 0.032(3) 0.055(3) 0.038(3) 0.005(3) 0.004(2) 0.007(2) C16 0.025(3) 0.065(3) 0.051(4) 0.001(3) 0.004(3) 0.001(2) C15 0.029(3) 0.061(3) 0.051(4) 0.004(3) -0.004(3) -0.006(2) C14 0.027(3) 0.043(3) 0.051(3) 0.005(3) 0.000(2) -0.003(2) C21 0.031(3) 0.040(2) 0.032(3) -0.002(2) 0.000(2) -0.0020(19) C22 0.030(3) 0.047(3) 0.039(3) -0.004(2) 0.000(2) -0.010(2) C23 0.029(3) 0.060(3) 0.037(3) -0.007(3) 0.000(2) -0.006(2) C24 0.028(3) 0.058(3) 0.053(4) -0.003(3) -0.004(2) 0.008(2) C25 0.029(2) 0.045(2) 0.054(4) -0.003(3) 0.000(2) 0.0037(19) C26 0.030(3) 0.077(4) 0.055(4) 0.004(4) 0.009(3) -0.006(3) C27 0.038(3) 0.037(2) 0.045(4) 0.004(2) 0.001(2) -0.0011(19) O1 0.056(2) 0.0354(17) 0.071(3) 0.0025(18) 0.006(2) -0.0037(14) C28 0.088(5) 0.037(3) 0.081(5) 0.010(3) 0.008(4) 0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -15 18 0 0.0753 -15.0000 18.0000 0.0000 -0.7739 -0.2436 -0.5657 17 17 1 0.1072 17.0000 17.0000 1.0000 -0.2526 0.7761 -0.5730 -17 -17 0 0.0728 -17.0000 -17.0000 0.0000 0.1920 -0.7354 0.6382 -3 2 10 0.1318 -3.0000 2.0000 10.0000 -0.7145 0.3388 0.5935 3 0 -10 0.1221 3.0000 0.0000 -10.0000 0.6573 -0.3143 -0.6619 13 -19 -1 0.1046 13.0000 -19.0000 -1.0000 0.8284 0.1286 0.5414 24 -11 0 0.1506 24.0000 -11.0000 0.0000 0.7294 0.6083 0.2962 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 S2 105.76(10) . . ? N1 Pd1 S1 176.40(15) . . ? C2 Pd1 N1 80.13(15) . . ? C2 Pd1 S2 174.02(13) . . ? C2 Pd1 S1 99.85(12) . . ? S1 Pd1 S2 74.33(4) . . ? C21 N1 Pd1 115.9(3) . . ? C25 N1 Pd1 123.5(3) . . ? C25 N1 C21 120.0(4) . . ? C3 C2 Pd1 125.0(3) . . ? C3 C2 C1 119.8(4) . . ? C1 C2 Pd1 115.2(3) . . ? C27 S2 Pd1 82.39(15) . . ? C27 S1 Pd1 86.09(16) . . ? C2 C3 H3 118.5 . . ? C4 C3 C2 123.0(4) . . ? C4 C3 H3 118.5 . . ? C2 C1 C6 119.1(4) . . ? C2 C1 C21 114.4(4) . . ? C6 C1 C21 126.5(4) . . ? C7 C6 C1 123.3(4) . . ? C7 C6 C5 117.8(4) . . ? C5 C6 C1 118.7(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 120.9(4) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.8(4) . . ? C9 C8 H8 119.6 . . ? C8 C9 H9 119.0 . . ? C8 C9 C10 122.0(4) . . ? C10 C9 H9 119.0 . . ? C9 C10 C5 118.0(4) . . ? C9 C10 C11 122.1(4) . . ? C5 C10 C11 119.9(4) . . ? C6 C5 C10 120.3(4) . . ? C6 C5 C4 119.9(4) . . ? C10 C5 C4 119.7(4) . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C13 122.5(4) . . ? C5 C4 C13 119.8(4) . . ? C12 C13 C4 119.1(4) . . ? C14 C13 C4 122.2(4) . . ? C14 C13 C12 118.6(4) . . ? C11 C12 C13 120.8(4) . . ? C11 C12 C17 120.2(4) . . ? C17 C12 C13 119.0(4) . . ? C12 C11 C10 119.6(4) . . ? C20 C11 C10 122.7(4) . . ? C20 C11 C12 117.7(5) . . ? C11 C20 H20 119.2 . . ? C11 C20 C19 121.6(5) . . ? C19 C20 H20 119.2 . . ? C20 C19 H19 119.2 . . ? C18 C19 C20 121.6(5) . . ? C18 C19 H19 119.2 . . ? C19 C18 H18 120.0 . . ? C19 C18 C17 119.9(5) . . ? C17 C18 H18 120.0 . . ? C18 C17 C12 118.8(5) . . ? C16 C17 C12 119.4(5) . . ? C16 C17 C18 121.8(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C16 C15 H15 119.5 . . ? C16 C15 C14 120.9(5) . . ? C14 C15 H15 119.5 . . ? C13 C14 C15 121.7(5) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? N1 C21 C1 113.0(4) . . ? N1 C21 C22 118.3(4) . . ? C22 C21 C1 128.5(4) . . ? C21 C22 H22 119.2 . . ? C23 C22 C21 121.5(5) . . ? C23 C22 H22 119.2 . . ? C22 C23 C26 120.2(5) . . ? C24 C23 C22 118.2(5) . . ? C24 C23 C26 121.7(5) . . ? C23 C24 H24 120.5 . . ? C25 C24 C23 118.9(5) . . ? C25 C24 H24 120.5 . . ? N1 C25 C24 122.8(4) . . ? N1 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S2 C27 S1 117.2(3) . . ? O1 C27 S2 125.4(4) . . ? O1 C27 S1 117.5(4) . . ? C27 O1 C28 118.7(4) . . ? O1 C28 H28A 109.5 . . ? O1 C28 H28B 109.5 . . ? O1 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 N1 2.030(3) . ? Pd1 C2 1.984(4) . ? Pd1 S2 2.4431(12) . ? Pd1 S1 2.3113(11) . ? N1 C21 1.364(5) . ? N1 C25 1.343(5) . ? C2 C3 1.395(6) . ? C2 C1 1.395(6) . ? S2 C27 1.672(5) . ? S1 C27 1.696(4) . ? C3 H3 0.9300 . ? C3 C4 1.376(5) . ? C1 C6 1.441(6) . ? C1 C21 1.459(6) . ? C6 C7 1.411(6) . ? C6 C5 1.429(6) . ? C7 H7 0.9300 . ? C7 C8 1.366(5) . ? C8 H8 0.9300 . ? C8 C9 1.378(6) . ? C9 H9 0.9300 . ? C9 C10 1.379(6) . ? C10 C5 1.430(6) . ? C10 C11 1.465(6) . ? C5 C4 1.438(6) . ? C4 C13 1.465(6) . ? C13 C12 1.431(6) . ? C13 C14 1.378(6) . ? C12 C11 1.425(7) . ? C12 C17 1.426(7) . ? C11 C20 1.389(6) . ? C20 H20 0.9300 . ? C20 C19 1.391(9) . ? C19 H19 0.9300 . ? C19 C18 1.350(8) . ? C18 H18 0.9300 . ? C18 C17 1.420(7) . ? C17 C16 1.417(8) . ? C16 H16 0.9300 . ? C16 C15 1.349(8) . ? C15 H15 0.9300 . ? C15 C14 1.399(6) . ? C14 H14 0.9300 . ? C21 C22 1.400(6) . ? C22 H22 0.9300 . ? C22 C23 1.385(7) . ? C23 C24 1.383(7) . ? C23 C26 1.507(7) . ? C24 H24 0.9300 . ? C24 C25 1.374(7) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O1 1.324(5) . ? O1 C28 1.450(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 C21 C1 7.8(5) . . . . ? Pd1 N1 C21 C22 -167.9(4) . . . . ? Pd1 N1 C25 C24 171.1(4) . . . . ? Pd1 C2 C3 C4 179.5(4) . . . . ? Pd1 C2 C1 C6 -168.3(3) . . . . ? Pd1 C2 C1 C21 12.0(6) . . . . ? Pd1 S2 C27 S1 -1.5(3) . . . . ? Pd1 S2 C27 O1 176.6(5) . . . . ? Pd1 S1 C27 S2 1.6(3) . . . . ? Pd1 S1 C27 O1 -176.6(4) . . . . ? N1 C21 C22 C23 -5.1(7) . . . . ? C2 C3 C4 C5 -11.2(7) . . . . ? C2 C3 C4 C13 170.1(5) . . . . ? C2 C1 C6 C7 164.3(6) . . . . ? C2 C1 C6 C5 -11.0(7) . . . . ? C2 C1 C21 N1 -12.8(6) . . . . ? C2 C1 C21 C22 162.4(5) . . . . ? S2 C27 O1 C28 -2.5(7) . . . . ? S1 C27 O1 C28 175.6(4) . . . . ? C3 C2 C1 C6 10.5(7) . . . . ? C3 C2 C1 C21 -169.2(4) . . . . ? C3 C4 C13 C12 168.7(5) . . . . ? C3 C4 C13 C14 -12.9(8) . . . . ? C1 C2 C3 C4 0.8(8) . . . . ? C1 C6 C7 C8 -178.0(8) . . . . ? C1 C6 C5 C10 179.0(4) . . . . ? C1 C6 C5 C4 0.7(7) . . . . ? C1 C21 C22 C23 -180.0(5) . . . . ? C6 C1 C21 N1 167.5(4) . . . . ? C6 C1 C21 C22 -17.3(8) . . . . ? C6 C7 C8 C9 -0.7(16) . . . . ? C6 C5 C4 C3 10.2(7) . . . . ? C6 C5 C4 C13 -171.0(4) . . . . ? C7 C6 C5 C10 3.4(7) . . . . ? C7 C6 C5 C4 -174.9(5) . . . . ? C7 C8 C9 C10 3.3(17) . . . . ? C8 C9 C10 C5 -2.5(13) . . . . ? C8 C9 C10 C11 178.0(9) . . . . ? C9 C10 C5 C6 -0.9(8) . . . . ? C9 C10 C5 C4 177.4(6) . . . . ? C9 C10 C11 C12 174.3(6) . . . . ? C9 C10 C11 C20 -3.1(9) . . . . ? C10 C5 C4 C3 -168.1(4) . . . . ? C10 C5 C4 C13 10.7(7) . . . . ? C10 C11 C20 C19 176.5(6) . . . . ? C5 C6 C7 C8 -2.6(11) . . . . ? C5 C10 C11 C12 -5.2(7) . . . . ? C5 C10 C11 C20 177.4(5) . . . . ? C5 C4 C13 C12 -10.0(7) . . . . ? C5 C4 C13 C14 168.4(5) . . . . ? C4 C13 C12 C11 1.7(7) . . . . ? C4 C13 C12 C17 -177.9(4) . . . . ? C4 C13 C14 C15 -179.6(5) . . . . ? C13 C12 C11 C10 5.9(7) . . . . ? C13 C12 C11 C20 -176.6(5) . . . . ? C13 C12 C17 C18 176.9(5) . . . . ? C13 C12 C17 C16 -3.7(7) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C12 C11 C20 C19 -0.9(8) . . . . ? C12 C17 C16 C15 1.3(9) . . . . ? C11 C10 C5 C6 178.6(4) . . . . ? C11 C10 C5 C4 -3.1(7) . . . . ? C11 C12 C17 C18 -2.7(7) . . . . ? C11 C12 C17 C16 176.7(5) . . . . ? C11 C20 C19 C18 -1.5(10) . . . . ? C20 C19 C18 C17 1.7(10) . . . . ? C19 C18 C17 C12 0.4(8) . . . . ? C19 C18 C17 C16 -179.0(6) . . . . ? C18 C17 C16 C15 -179.3(6) . . . . ? C17 C12 C11 C10 -174.6(5) . . . . ? C17 C12 C11 C20 2.9(7) . . . . ? C17 C16 C15 C14 1.2(10) . . . . ? C16 C15 C14 C13 -1.2(9) . . . . ? C14 C13 C12 C11 -176.8(5) . . . . ? C14 C13 C12 C17 3.7(7) . . . . ? C21 N1 C25 C24 0.3(8) . . . . ? C21 C1 C6 C7 -16.0(8) . . . . ? C21 C1 C6 C5 168.7(4) . . . . ? C21 C22 C23 C24 2.5(8) . . . . ? C21 C22 C23 C26 -178.5(5) . . . . ? C22 C23 C24 C25 1.4(8) . . . . ? C23 C24 C25 N1 -2.9(8) . . . . ? C25 N1 C21 C1 179.3(4) . . . . ? C25 N1 C21 C22 3.6(7) . . . . ? C26 C23 C24 C25 -177.6(5) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.77(4) 2 0.23(4)