# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common '[PdCl(PySMePy)](OTf)' _chemical_melting_point >465 _chemical_formula_moiety 'C17 H15 Cl N3 Pd S2, C F3 O3 S' _chemical_formula_sum 'C18 H15 Cl F3 N3 O3 Pd S3' _chemical_formula_weight 616.36 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.755(3) _cell_length_b 10.203(3) _cell_length_c 13.952(4) _cell_angle_alpha 65.946(17) _cell_angle_beta 74.499(18) _cell_angle_gamma 78.61(2) _cell_volume 1091.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7610 _cell_measurement_theta_min 3.106 _cell_measurement_theta_max 25.998 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.876 _exptl_crystal_F_000 612 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 1.313 _shelx_estimated_absorpt_T_min 0.937 _shelx_estimated_absorpt_T_max 0.937 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9373 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_measurement_device_type 'Rigaku Saturn724+ (4x4 bin mode)' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7610 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.106 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_Laue_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_point_group_measured_fraction_full 0.972 _reflns_number_total 4148 _reflns_number_gt 3333 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics Ortep-III _computing_publication_material Ortep-III _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+5.5464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4148 _refine_ls_number_parameters 282 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.81603(6) 0.45066(5) 0.45184(4) 0.03364(19) Uani 1 1 d . . . . . Cl1 Cl 0.7745(2) 0.65536(17) 0.48869(13) 0.0387(4) Uani 1 1 d . . . . . S1 S 1.0173(2) 0.53784(16) 0.30694(12) 0.0332(4) Uani 1 1 d . . . . . S2 S 0.6048(2) 0.34890(18) 0.58380(15) 0.0404(4) Uani 1 1 d . . . . . N1 N 0.8596(7) 0.2678(5) 0.4203(4) 0.0330(12) Uani 1 1 d . . . . . N2 N 0.9391(9) 0.5681(6) 0.1246(5) 0.0510(17) Uani 1 1 d . . . . . N3 N 0.7803(10) 0.1656(7) 0.7252(6) 0.062(2) Uani 1 1 d . . . . . C1 C 0.9895(9) 0.2510(7) 0.3476(5) 0.0357(14) Uani 1 1 d . . . . . C2 C 1.0251(10) 0.1253(7) 0.3279(6) 0.0443(17) Uani 1 1 d . . . . . H2A H 1.1163 0.1130 0.2760 0.053 Uiso 1 1 calc R U . . . C3 C 0.9247(11) 0.0174(8) 0.3854(7) 0.053(2) Uani 1 1 d . . . . . H3A H 0.9485 -0.0710 0.3743 0.064 Uiso 1 1 calc R U . . . C4 C 0.7898(10) 0.0370(8) 0.4590(6) 0.0483(18) Uani 1 1 d . . . . . H4A H 0.7191 -0.0360 0.4970 0.058 Uiso 1 1 calc R U . . . C5 C 0.7597(9) 0.1642(7) 0.4763(6) 0.0413(16) Uani 1 1 d . . . . . C6 C 1.0991(9) 0.3704(7) 0.2897(6) 0.0401(16) Uani 1 1 d . . . . . H6A H 1.1250 0.3885 0.2121 0.048 Uiso 1 1 calc R U . . . H6B H 1.1998 0.3370 0.3159 0.048 Uiso 1 1 calc R U . . . C7 C 0.6130(9) 0.1913(8) 0.5527(8) 0.056(2) Uani 1 1 d . . . . . H7A H 0.6037 0.1054 0.6205 0.067 Uiso 1 1 calc R U . . . H7B H 0.5194 0.2016 0.5221 0.067 Uiso 1 1 calc R U . . . C8 C 0.9080(9) 0.6249(7) 0.1994(5) 0.0378(16) Uani 1 1 d . . . . . C9 C 0.8117(9) 0.7477(7) 0.1969(6) 0.0399(16) Uani 1 1 d . . . . . H9A H 0.7982 0.7840 0.2518 0.048 Uiso 1 1 calc R U . . . C10 C 0.7338(9) 0.8186(8) 0.1127(6) 0.0446(17) Uani 1 1 d . . . . . H10A H 0.6631 0.9034 0.1087 0.054 Uiso 1 1 calc R U . . . C11 C 0.7625(11) 0.7613(9) 0.0339(6) 0.052(2) Uani 1 1 d . . . . . H11A H 0.7123 0.8074 -0.0258 0.062 Uiso 1 1 calc R U . . . C12 C 0.8619(13) 0.6399(9) 0.0429(7) 0.061(2) Uani 1 1 d . . . . . H12A H 0.8790 0.6023 -0.0116 0.073 Uiso 1 1 calc R U . . . C13 C 0.6705(9) 0.2785(8) 0.7074(6) 0.0456(18) Uani 1 1 d . . . . . C14 C 0.6036(10) 0.3468(12) 0.7761(7) 0.070(3) Uani 1 1 d . . . . . H14A H 0.5266 0.4280 0.7586 0.084 Uiso 1 1 calc R U . . . C15 C 0.6521(12) 0.2935(15) 0.8729(7) 0.090(4) Uani 1 1 d . . . . . H15A H 0.6085 0.3380 0.9237 0.108 Uiso 1 1 calc R U . . . C16 C 0.7618(12) 0.1777(13) 0.8947(7) 0.078(3) Uani 1 1 d . . . . . H16A H 0.7942 0.1387 0.9615 0.093 Uiso 1 1 calc R U . . . C17 C 0.8264(13) 0.1167(9) 0.8190(8) 0.068(3) Uani 1 1 d . . . . . H17A H 0.9061 0.0375 0.8338 0.081 Uiso 1 1 calc R U . . . S3 S 0.5434(4) 0.1469(3) 0.2252(3) 0.0509(9) Uiso 0.693(7) 1 d D . P A 2 O1 O 0.6667(11) 0.0324(10) 0.2506(8) 0.073(3) Uiso 0.693(7) 1 d D . P A 2 O2 O 0.4507(13) 0.1663(12) 0.3204(7) 0.076(3) Uiso 0.693(7) 1 d D . P A 2 O3 O 0.4641(16) 0.1479(16) 0.1494(10) 0.094(4) Uiso 0.693(7) 1 d D . P A 2 C18 C 0.6409(11) 0.3079(12) 0.1644(8) 0.052(3) Uiso 0.693(7) 1 d D . P A 2 S4 S 0.4716(9) 0.1971(7) 0.1911(6) 0.053(2) Uiso 0.307(7) 1 d D . P A 1 O4 O 0.413(2) 0.3375(14) 0.1274(15) 0.067(6) Uiso 0.307(7) 1 d D . P A 1 O5 O 0.501(2) 0.0994(19) 0.1372(15) 0.053(5) Uiso 0.307(7) 1 d D . P A 1 O6 O 0.3945(18) 0.1531(15) 0.3003(8) 0.033(3) Uiso 0.307(7) 1 d D . P A 1 C19 C 0.6717(19) 0.215(2) 0.1883(19) 0.096(12) Uiso 0.307(7) 1 d D . P A 1 F1 F 0.5466(11) 0.4216(9) 0.1188(7) 0.084(3) Uiso 0.693(7) 1 d D . P A 2 F2 F 0.7534(13) 0.3157(14) 0.0794(8) 0.094(3) Uiso 0.693(7) 1 d D . P A 2 F3 F 0.6866(13) 0.3402(13) 0.2338(8) 0.074(3) Uiso 0.693(7) 1 d D . P A 2 F4 F 0.762(3) 0.091(2) 0.2147(17) 0.082(6) Uiso 0.307(7) 1 d D . P A 1 F5 F 0.698(3) 0.295(3) 0.234(2) 0.090(9) Uiso 0.307(7) 1 d D . P A 1 F6 F 0.783(2) 0.252(3) 0.1006(16) 0.071(6) Uiso 0.307(7) 1 d D . P A 1 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 0.0430(3) 0.0275(3) 0.0306(3) -0.0056(2) -0.0127(2) -0.0088(2) Cl1 0.0518(10) 0.0304(8) 0.0382(9) -0.0134(7) -0.0153(7) -0.0046(7) S1 0.0452(9) 0.0269(7) 0.0264(8) -0.0048(6) -0.0109(7) -0.0082(6) S2 0.0367(9) 0.0339(9) 0.0462(10) -0.0072(7) -0.0108(8) -0.0080(7) N1 0.043(3) 0.027(3) 0.033(3) -0.004(2) -0.023(3) -0.005(2) N2 0.092(5) 0.033(3) 0.033(3) -0.008(3) -0.028(3) -0.006(3) N3 0.081(5) 0.030(3) 0.069(5) 0.004(3) -0.037(4) -0.014(3) C1 0.049(4) 0.027(3) 0.032(3) -0.007(3) -0.016(3) -0.005(3) C2 0.060(5) 0.034(4) 0.043(4) -0.014(3) -0.020(4) -0.002(3) C3 0.070(6) 0.029(4) 0.066(5) -0.014(4) -0.025(5) -0.008(3) C4 0.055(5) 0.038(4) 0.052(5) -0.007(3) -0.019(4) -0.016(3) C5 0.047(4) 0.035(3) 0.044(4) -0.006(3) -0.024(3) -0.010(3) C6 0.054(4) 0.035(3) 0.031(3) -0.010(3) -0.011(3) -0.009(3) C7 0.039(4) 0.038(4) 0.091(7) -0.018(4) -0.015(4) -0.014(3) C8 0.059(4) 0.026(3) 0.026(3) 0.001(3) -0.018(3) -0.011(3) C9 0.049(4) 0.037(4) 0.033(4) -0.010(3) -0.007(3) -0.013(3) C10 0.049(4) 0.041(4) 0.033(4) -0.001(3) -0.013(3) -0.003(3) C11 0.071(6) 0.049(4) 0.037(4) -0.005(3) -0.024(4) -0.015(4) C12 0.105(8) 0.048(5) 0.042(4) -0.017(4) -0.038(5) -0.004(5) C13 0.034(4) 0.044(4) 0.037(4) 0.009(3) -0.003(3) -0.014(3) C14 0.036(4) 0.106(8) 0.037(4) -0.012(5) 0.011(3) 0.003(5) C15 0.055(6) 0.147(11) 0.034(5) -0.012(6) 0.003(4) 0.002(7) C16 0.053(5) 0.102(8) 0.036(5) 0.020(5) -0.004(4) -0.021(5) C17 0.077(7) 0.037(4) 0.065(6) 0.016(4) -0.026(5) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.029(5) . ? Pd1 S1 2.2874(19) . ? Pd1 Cl1 2.2879(17) . ? Pd1 S2 2.295(2) . ? S1 C6 1.802(7) . ? S1 C8 1.817(7) . ? S2 C13 1.783(8) . ? S2 C7 1.814(8) . ? N1 C1 1.342(9) . ? N1 C5 1.349(9) . ? N2 C8 1.332(9) . ? N2 C12 1.352(10) . ? N3 C13 1.331(10) . ? N3 C17 1.339(11) . ? C1 C2 1.379(10) . ? C1 C6 1.517(9) . ? C2 C3 1.383(11) . ? C3 C4 1.384(12) . ? C4 C5 1.378(11) . ? C5 C7 1.493(12) . ? C8 C9 1.359(10) . ? C9 C10 1.382(10) . ? C10 C11 1.389(11) . ? C11 C12 1.347(12) . ? C13 C14 1.353(13) . ? C14 C15 1.384(13) . ? C15 C16 1.351(15) . ? C16 C17 1.378(15) . ? S3 O3 1.407(8) . ? S3 O1 1.423(7) . ? S3 O2 1.428(7) . ? S3 C18 1.783(12) . ? C18 F2 1.308(9) . ? C18 F3 1.314(9) . ? C18 F1 1.316(9) . ? S4 O6 1.411(8) . ? S4 O4 1.420(9) . ? S4 O5 1.425(9) . ? S4 C19 1.784(15) . ? C19 F6 1.311(10) . ? C19 F5 1.315(10) . ? C19 F4 1.316(10) . ? F4 F6 1.76(3) . ? 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 S1 86.48(17) . . ? N1 Pd1 Cl1 178.21(15) . . ? S1 Pd1 Cl1 92.79(7) . . ? N1 Pd1 S2 87.35(18) . . ? S1 Pd1 S2 172.18(6) . . ? Cl1 Pd1 S2 93.51(7) . . ? C6 S1 C8 101.6(3) . . ? C6 S1 Pd1 98.1(2) . . ? C8 S1 Pd1 101.3(2) . . ? C13 S2 C7 104.0(4) . . ? C13 S2 Pd1 106.5(2) . . ? C7 S2 Pd1 97.4(3) . . ? C1 N1 C5 121.9(6) . . ? C1 N1 Pd1 119.3(4) . . ? C5 N1 Pd1 118.7(5) . . ? C8 N2 C12 115.0(7) . . ? C13 N3 C17 116.6(9) . . ? N1 C1 C2 120.4(6) . . ? N1 C1 C6 119.1(6) . . ? C2 C1 C6 120.5(7) . . ? C1 C2 C3 118.4(8) . . ? C2 C3 C4 120.6(7) . . ? C5 C4 C3 118.8(7) . . ? N1 C5 C4 119.9(7) . . ? N1 C5 C7 119.6(6) . . ? C4 C5 C7 120.4(7) . . ? C1 C6 S1 114.3(5) . . ? C5 C7 S2 115.5(5) . . ? N2 C8 C9 125.4(6) . . ? N2 C8 S1 116.5(5) . . ? C9 C8 S1 117.9(5) . . ? C8 C9 C10 118.4(7) . . ? C9 C10 C11 117.6(7) . . ? C12 C11 C10 119.4(7) . . ? C11 C12 N2 124.2(7) . . ? N3 C13 C14 125.1(8) . . ? N3 C13 S2 118.7(7) . . ? C14 C13 S2 116.2(6) . . ? C13 C14 C15 117.2(9) . . ? C16 C15 C14 119.6(11) . . ? C15 C16 C17 119.4(9) . . ? N3 C17 C16 122.1(9) . . ? O3 S3 O1 114.8(8) . . ? O3 S3 O2 118.7(8) . . ? O1 S3 O2 110.3(6) . . ? O3 S3 C18 106.1(7) . . ? O1 S3 C18 105.2(6) . . ? O2 S3 C18 99.4(6) . . ? F2 C18 F3 112.5(10) . . ? F2 C18 F1 98.1(10) . . ? F3 C18 F1 104.6(10) . . ? F2 C18 S3 115.2(9) . . ? F3 C18 S3 112.9(8) . . ? F1 C18 S3 112.1(8) . . ? O6 S4 O4 113.4(11) . . ? O6 S4 O5 119.9(11) . . ? O4 S4 O5 111.9(13) . . ? O6 S4 C19 105.3(11) . . ? O4 S4 C19 104.2(12) . . ? O5 S4 C19 99.7(12) . . ? F6 C19 F5 99(2) . . ? F6 C19 F4 84.2(18) . . ? F5 C19 F4 110(2) . . ? F6 C19 S4 124.1(18) . . ? F5 C19 S4 119.4(18) . . ? F4 C19 S4 113.9(17) . . ? C19 F4 F6 47.8(9) . . ? C19 F6 F4 48.0(9) . . ? 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 C5 N1 C1 C2 -0.1(10) . . . . ? Pd1 N1 C1 C2 177.4(5) . . . . ? C5 N1 C1 C6 -178.4(6) . . . . ? Pd1 N1 C1 C6 -0.8(8) . . . . ? N1 C1 C2 C3 -0.5(10) . . . . ? C6 C1 C2 C3 177.7(7) . . . . ? C1 C2 C3 C4 1.6(11) . . . . ? C2 C3 C4 C5 -1.9(12) . . . . ? C1 N1 C5 C4 -0.2(10) . . . . ? Pd1 N1 C5 C4 -177.8(5) . . . . ? C1 N1 C5 C7 -177.2(6) . . . . ? Pd1 N1 C5 C7 5.2(8) . . . . ? C3 C4 C5 N1 1.2(11) . . . . ? C3 C4 C5 C7 178.2(7) . . . . ? N1 C1 C6 S1 -12.2(8) . . . . ? C2 C1 C6 S1 169.5(5) . . . . ? C8 S1 C6 C1 -86.9(5) . . . . ? Pd1 S1 C6 C1 16.4(5) . . . . ? N1 C5 C7 S2 -12.6(10) . . . . ? C4 C5 C7 S2 170.4(6) . . . . ? C13 S2 C7 C5 -97.2(7) . . . . ? Pd1 S2 C7 C5 12.0(7) . . . . ? C12 N2 C8 C9 -2.2(12) . . . . ? C12 N2 C8 S1 -176.7(6) . . . . ? C6 S1 C8 N2 -13.8(6) . . . . ? Pd1 S1 C8 N2 -114.6(6) . . . . ? C6 S1 C8 C9 171.2(6) . . . . ? Pd1 S1 C8 C9 70.4(6) . . . . ? N2 C8 C9 C10 2.5(11) . . . . ? S1 C8 C9 C10 177.0(5) . . . . ? C8 C9 C10 C11 -1.7(11) . . . . ? C9 C10 C11 C12 0.8(12) . . . . ? C10 C11 C12 N2 -0.6(15) . . . . ? C8 N2 C12 C11 1.2(14) . . . . ? C17 N3 C13 C14 0.3(12) . . . . ? C17 N3 C13 S2 179.8(6) . . . . ? C7 S2 C13 N3 33.7(7) . . . . ? Pd1 S2 C13 N3 -68.5(6) . . . . ? C7 S2 C13 C14 -146.8(7) . . . . ? Pd1 S2 C13 C14 110.9(6) . . . . ? N3 C13 C14 C15 -0.9(14) . . . . ? S2 C13 C14 C15 179.6(8) . . . . ? C13 C14 C15 C16 -0.1(17) . . . . ? C14 C15 C16 C17 1.5(17) . . . . ? C13 N3 C17 C16 1.2(13) . . . . ? C15 C16 C17 N3 -2.2(16) . . . . ? O3 S3 C18 F2 -64.7(11) . . . . ? O1 S3 C18 F2 57.3(10) . . . . ? O2 S3 C18 F2 171.5(9) . . . . ? O3 S3 C18 F3 164.1(10) . . . . ? O1 S3 C18 F3 -73.8(9) . . . . ? O2 S3 C18 F3 40.4(10) . . . . ? O3 S3 C18 F1 46.3(10) . . . . ? O1 S3 C18 F1 168.4(8) . . . . ? O2 S3 C18 F1 -77.4(9) . . . . ? O6 S4 C19 F6 179.2(19) . . . . ? O4 S4 C19 F6 -61(2) . . . . ? O5 S4 C19 F6 54(2) . . . . ? O6 S4 C19 F5 -53(2) . . . . ? O4 S4 C19 F5 66(2) . . . . ? O5 S4 C19 F5 -178(2) . . . . ? O6 S4 C19 F4 79.6(19) . . . . ? O4 S4 C19 F4 -160.8(19) . . . . ? O5 S4 C19 F4 -45(2) . . . . ? F5 C19 F4 F6 -98(2) . . . . ? S4 C19 F4 F6 125(2) . . . . ? F5 C19 F6 F4 109(2) . . . . ? S4 C19 F6 F4 -115(2) . . . . ? _refine_diff_density_max 2.168 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.147 _shelxl_version_number 2013-4 _shelx_res_file ; TITL complex2 REM Yadorkari-X generated CELL 0.71075 8.7555 10.2034 13.9516 65.9460 74.4990 78.6130 ZERR 2.0 0.0028 0.0031 0.0038 0.0170 0.0180 0.0200 LATT 1 REM SPGR P-1 triclinic SFAC C H Cl F N O Pd S UNIT 36.000000 30.000000 2.000000 6.000000 6.000000 6.000000 2.000000 6.000000 SIZE 0.05 0.05 0.05 TEMP -119.8 L.S. 10 FMAP 2 PLAN -200 ACTA CONF MERG 2 OMIT -10.000000 52.000000 OMIT -3 -2 8 OMIT -3 -1 12 OMIT 3 1 3 OMIT -3 -4 2 OMIT -3 -1 14 OMIT 0 2 5 OMIT 6 3 1 OMIT 3 13 8 OMIT 5 -8 6 OMIT -2 1 2 OMIT -7 -2 6 OMIT -6 0 9 OMIT -7 -1 7 EQIV $1 1-X, -Y, 1-Z EQIV $2 1+X, +Y, +Z EQIV $3 2-X, 1-Y, 1-Z EQIV $4 1-X, 1-Y, 1-Z EQIV $5 +X, 1+Y, +Z EQIV $6 1-X, 1-Y, -Z EQIV $7 +X, +Y, 1+Z SHEL 6.790236 0.769625 HTAB LIST 4 MPLA Pd1 > S2 N1 MPLA N1 C1 > C2 C3 C4 C5 SADI 0.01 S3 O1 S3 O2 S3 O3 S4 O4 S4 O5 S4 O6 SADI 0.01 C18 F1 C18 F2 C18 F3 C19 F4 C19 F5 C19 F6 SADI 0.01 S3 C18 S4 C19 WGHT 0.074700 5.546400 FVAR 0.47639 0.69327 PD1 7 0.816025 0.450662 0.451840 11.00000 0.04300 0.02748 = 0.03059 -0.00556 -0.01271 -0.00875 CL1 3 0.774541 0.655356 0.488688 11.00000 0.05185 0.03038 = 0.03818 -0.01342 -0.01525 -0.00460 S1 8 1.017289 0.537836 0.306936 11.00000 0.04516 0.02694 = 0.02637 -0.00476 -0.01092 -0.00822 S2 8 0.604818 0.348903 0.583798 11.00000 0.03670 0.03390 = 0.04616 -0.00722 -0.01081 -0.00799 N1 5 0.859633 0.267815 0.420321 11.00000 0.04282 0.02662 = 0.03292 -0.00440 -0.02278 -0.00512 N2 5 0.939135 0.568144 0.124633 11.00000 0.09208 0.03281 = 0.03320 -0.00830 -0.02807 -0.00592 N3 5 0.780329 0.165574 0.725233 11.00000 0.08105 0.03037 = 0.06883 0.00376 -0.03688 -0.01423 C1 1 0.989512 0.251028 0.347551 11.00000 0.04858 0.02720 = 0.03203 -0.00655 -0.01590 -0.00513 C2 1 1.025075 0.125277 0.327867 11.00000 0.05988 0.03377 = 0.04338 -0.01402 -0.01999 -0.00186 AFIX 43 H2A 2 1.116337 0.113048 0.276022 11.00000 -1.20000 AFIX 0 C3 1 0.924671 0.017390 0.385425 11.00000 0.06983 0.02859 = 0.06570 -0.01420 -0.02500 -0.00751 AFIX 43 H3A 2 0.948528 -0.070965 0.374327 11.00000 -1.20000 AFIX 0 C4 1 0.789751 0.037006 0.459045 11.00000 0.05493 0.03810 = 0.05153 -0.00658 -0.01890 -0.01606 AFIX 43 H4A 2 0.719128 -0.035966 0.497008 11.00000 -1.20000 AFIX 0 C5 1 0.759708 0.164214 0.476286 11.00000 0.04723 0.03464 = 0.04436 -0.00567 -0.02372 -0.01022 C6 1 1.099062 0.370404 0.289697 11.00000 0.05396 0.03546 = 0.03120 -0.00952 -0.01119 -0.00887 AFIX 23 H6A 2 1.125010 0.388465 0.212097 11.00000 -1.20000 H6B 2 1.199825 0.337044 0.315891 11.00000 -1.20000 AFIX 0 C7 1 0.612964 0.191253 0.552659 11.00000 0.03856 0.03812 = 0.09080 -0.01754 -0.01485 -0.01404 AFIX 23 H7A 2 0.603673 0.105448 0.620480 11.00000 -1.20000 H7B 2 0.519391 0.201565 0.522103 11.00000 -1.20000 AFIX 0 C8 1 0.907951 0.624891 0.199368 11.00000 0.05923 0.02631 = 0.02594 0.00055 -0.01768 -0.01109 C9 1 0.811674 0.747720 0.196918 11.00000 0.04944 0.03695 = 0.03292 -0.00952 -0.00698 -0.01348 AFIX 43 H9A 2 0.798220 0.784030 0.251771 11.00000 -1.20000 AFIX 0 C10 1 0.733766 0.818573 0.112658 11.00000 0.04897 0.04056 = 0.03323 -0.00082 -0.01272 -0.00310 AFIX 43 H10A 2 0.663144 0.903389 0.108749 11.00000 -1.20000 AFIX 0 C11 1 0.762454 0.761290 0.033899 11.00000 0.07086 0.04878 = 0.03689 -0.00465 -0.02366 -0.01490 AFIX 43 H11A 2 0.712330 0.807353 -0.025822 11.00000 -1.20000 AFIX 0 C12 1 0.861942 0.639886 0.042932 11.00000 0.10497 0.04763 = 0.04205 -0.01724 -0.03754 -0.00354 AFIX 43 H12A 2 0.878955 0.602276 -0.011574 11.00000 -1.20000 AFIX 0 C13 1 0.670475 0.278478 0.707423 11.00000 0.03380 0.04432 = 0.03663 0.00900 -0.00317 -0.01440 C14 1 0.603610 0.346814 0.776085 11.00000 0.03571 0.10573 = 0.03724 -0.01208 0.01144 0.00268 AFIX 43 H14A 2 0.526620 0.427980 0.758609 11.00000 -1.20000 AFIX 0 C15 1 0.652102 0.293484 0.872887 11.00000 0.05510 0.14696 = 0.03366 -0.01192 0.00258 0.00186 AFIX 43 H15A 2 0.608532 0.337976 0.923650 11.00000 -1.20000 AFIX 0 C16 1 0.761824 0.177719 0.894680 11.00000 0.05253 0.10168 = 0.03584 0.02006 -0.00367 -0.02134 AFIX 43 H16A 2 0.794159 0.138741 0.961531 11.00000 -1.20000 AFIX 0 C17 1 0.826374 0.116737 0.818993 11.00000 0.07749 0.03716 = 0.06547 0.01601 -0.02552 -0.01792 AFIX 43 H17A 2 0.906139 0.037467 0.833822 11.00000 -1.20000 PART 2 AFIX 0 S3 8 0.543350 0.146854 0.225177 21.00000 0.05090 O1 6 0.666725 0.032440 0.250561 21.00000 0.07347 O2 6 0.450665 0.166343 0.320436 21.00000 0.07553 O3 6 0.464109 0.147864 0.149360 21.00000 0.09437 C18 1 0.640925 0.307913 0.164362 21.00000 0.05159 PART 1 S4 8 0.471553 0.197102 0.191090 -21.00000 0.05307 O4 6 0.413365 0.337495 0.127366 -21.00000 0.06653 O5 6 0.500789 0.099382 0.137248 -21.00000 0.05281 O6 6 0.394521 0.153125 0.300282 -21.00000 0.03263 C19 1 0.671684 0.214511 0.188262 -21.00000 0.09557 PART 2 F1 4 0.546586 0.421587 0.118776 21.00000 0.08408 F2 4 0.753417 0.315672 0.079438 21.00000 0.09387 F3 4 0.686649 0.340207 0.233798 21.00000 0.07392 PART 1 F4 4 0.761918 0.091043 0.214706 -21.00000 0.08193 F5 4 0.698307 0.295399 0.234088 -21.00000 0.09012 F6 4 0.782828 0.252371 0.100632 -21.00000 0.07128 PART 0 HKLF 4 REM complex2 REM R1 = 0.0650 for 3333 Fo > 4sig(Fo) and 0.0792 for all 4148 data REM 282 parameters refined using 31 restraints END WGHT 0.0745 5.5584 REM Instructions for potential hydrogen bonds HTAB C4 O2_$1 HTAB C4 O6_$1 HTAB C6 N2 HTAB C6 O4_$2 HTAB C6 Cl1_$3 HTAB C6 O2_$2 HTAB C6 O6_$2 HTAB C7 S3_$1 HTAB C7 O2_$1 HTAB C7 O6_$1 HTAB C7 Cl1_$4 HTAB C9 Cl1 HTAB C9 O1_$5 HTAB C11 O3_$6 HTAB C11 O5_$6 HTAB C14 F1_$4 HTAB C16 F6_$7 REM Highest difference peak 2.168, deepest hole -1.237, 1-sigma level 0.147 Q1 1 0.4695 0.8971 0.7891 11.00000 0.05 2.17 Q2 1 0.5475 0.6392 0.6477 11.00000 0.05 1.24 Q3 1 0.4441 0.8269 0.7647 11.00000 0.05 1.14 Q4 1 0.3966 0.5966 0.9123 11.00000 0.05 0.96 Q5 1 0.3561 0.5630 0.7862 11.00000 0.05 0.94 Q6 1 0.3865 0.9954 0.7264 11.00000 0.05 0.87 Q7 1 0.5154 0.5617 0.8481 11.00000 0.05 0.86 Q8 1 0.5234 0.9449 0.8305 11.00000 0.05 0.81 Q9 1 0.2910 0.9387 0.7882 11.00000 0.05 0.77 Q10 1 0.8784 0.4403 0.4968 11.00000 0.05 0.73 Q11 1 0.3616 0.6963 0.7396 11.00000 0.05 0.73 Q12 1 0.3050 0.6272 0.9302 11.00000 0.05 0.69 Q13 1 0.2001 0.7192 0.8778 11.00000 0.05 0.69 Q14 1 0.2447 0.6525 0.7886 11.00000 0.05 0.69 Q15 1 0.5554 0.8170 0.8414 11.00000 0.05 0.67 Q16 1 0.5816 0.4516 0.6056 11.00000 0.05 0.67 Q17 1 0.7573 0.4473 0.4107 11.00000 0.05 0.66 Q18 1 0.2452 0.7620 0.9276 11.00000 0.05 0.65 Q19 1 0.7440 0.7455 0.5275 11.00000 0.05 0.65 Q20 1 0.4772 0.8629 0.9006 11.00000 0.05 0.64 Q21 1 0.8254 -0.0353 0.8682 11.00000 0.05 0.62 Q22 1 0.8485 0.5996 0.4376 11.00000 0.05 0.62 Q23 1 0.4845 0.8356 0.6631 11.00000 0.05 0.61 Q24 1 0.7773 0.5503 0.4941 11.00000 0.05 0.60 Q25 1 0.5419 0.5399 0.6360 11.00000 0.05 0.54 Q26 1 0.3291 0.7544 0.8310 11.00000 0.05 0.53 Q27 1 0.6864 0.5163 0.4247 11.00000 0.05 0.51 Q28 1 0.5899 0.9393 0.1904 11.00000 0.05 0.51 Q29 1 0.5594 0.8938 0.6994 11.00000 0.05 0.48 Q30 1 0.1898 0.8426 0.8192 11.00000 0.05 0.48 Q31 1 1.0487 0.3212 0.2860 11.00000 0.05 0.48 Q32 1 0.6594 0.1467 0.5334 11.00000 0.05 0.48 Q33 1 0.6311 -0.0584 0.6331 11.00000 0.05 0.45 Q34 1 1.0511 0.5630 0.3390 11.00000 0.05 0.45 Q35 1 0.7067 0.5960 0.4572 11.00000 0.05 0.45 Q36 1 0.9638 0.5377 0.3140 11.00000 0.05 0.45 Q37 1 0.8361 0.3187 0.4276 11.00000 0.05 0.45 Q38 1 0.9044 0.2413 0.3261 11.00000 0.05 0.44 Q39 1 0.5134 0.7830 0.7950 11.00000 0.05 0.44 Q40 1 0.8991 0.2602 0.4142 11.00000 0.05 0.44 Q41 1 0.7450 0.3398 0.4405 11.00000 0.05 0.44 Q42 1 0.7596 0.4746 0.2979 11.00000 0.05 0.43 Q43 1 0.9497 0.1179 0.3238 11.00000 0.05 0.42 Q44 1 0.5310 0.7771 0.6070 11.00000 0.05 0.40 Q45 1 0.9085 -0.0420 0.2978 11.00000 0.05 0.39 Q46 1 0.6253 0.7410 0.8652 11.00000 0.05 0.39 Q47 1 0.7766 0.1533 0.8807 11.00000 0.05 0.39 Q48 1 1.2064 0.4606 0.1841 11.00000 0.05 0.39 Q49 1 0.6020 0.3939 0.7709 11.00000 0.05 0.38 Q50 1 0.6548 -0.0305 0.6494 11.00000 0.05 0.38 Q51 1 0.6191 0.6070 0.3804 11.00000 0.05 0.38 Q52 1 0.3594 0.6431 0.8342 11.00000 0.05 0.38 Q53 1 1.0510 -0.0997 0.4059 11.00000 0.05 0.38 Q54 1 0.6802 0.0337 0.8770 11.00000 0.05 0.38 Q55 1 0.6367 0.0252 0.8678 11.00000 0.05 0.37 Q56 1 0.7614 0.7487 0.3017 11.00000 0.05 0.37 Q57 1 0.9738 0.7568 0.3508 11.00000 0.05 0.37 Q58 1 1.0180 0.5898 0.1420 11.00000 0.05 0.37 Q59 1 0.5210 0.0776 0.4846 11.00000 0.05 0.37 Q60 1 0.7234 -0.0759 0.5328 11.00000 0.05 0.36 Q61 1 0.6146 0.2537 0.8911 11.00000 0.05 0.36 Q62 1 0.7328 0.0031 0.3952 11.00000 0.05 0.36 Q63 1 0.4212 1.0624 0.6398 11.00000 0.05 0.36 Q64 1 1.1933 0.2446 0.1845 11.00000 0.05 0.36 Q65 1 0.8628 0.3749 0.5714 11.00000 0.05 0.35 Q66 1 1.0882 0.4236 0.4683 11.00000 0.05 0.35 Q67 1 0.7557 0.0872 0.8297 11.00000 0.05 0.35 Q68 1 1.0435 0.1815 0.3072 11.00000 0.05 0.35 Q69 1 0.5438 0.3491 0.5464 11.00000 0.05 0.35 Q70 1 0.6755 0.3148 0.6385 11.00000 0.05 0.35 Q71 1 0.5584 0.3132 0.8184 11.00000 0.05 0.34 Q72 1 0.6391 0.7961 0.7384 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-11 -2 -5 6.68 3.70 -11 -2 -6 34.35 6.95 -11 -2 -6 18.12 4.16 -11 -2 -7 40.29 7.42 -11 -2 -7 40.34 5.89 -11 -2 -8 10.68 3.47 -11 -3 -1 0.42 1.67 -11 -3 -1 5.65 3.32 -11 -3 -2 2.58 2.64 -11 -3 -2 -2.57 2.55 -11 -3 -3 4.25 2.09 -11 -3 -3 3.31 2.68 -11 -3 -4 29.20 7.39 -11 -3 -4 41.51 6.61 -11 -3 -5 40.00 11.96 -11 -3 -5 44.55 5.89 -11 -3 -6 10.31 4.06 -11 -3 -6 10.73 4.16 -11 -3 -7 1.86 2.37 -11 -3 -7 1.08 1.91 -11 -3 -8 -0.61 2.62 -11 -4 -2 1.40 1.78 -11 -4 -2 -0.08 2.48 -11 -4 -3 2.74 2.47 -11 -4 -3 3.72 3.82 -11 -4 -4 29.82 7.82 -11 -4 -4 50.13 7.19 -11 -4 -5 44.30 11.45 -11 -4 -5 52.28 7.10 -11 -4 -6 24.90 6.95 -11 -4 -6 23.17 4.03 -11 -4 -7 5.19 3.37 -11 -4 -7 2.78 3.23 -11 -4 -8 -2.54 2.68 -11 -5 -4 41.65 5.83 -11 -5 -4 30.51 5.10 -11 -5 -5 33.35 14.60 -11 -5 -5 71.71 8.65 -11 -5 -6 41.85 12.45 -11 -5 -7 33.61 5.89 -11 -5 -7 21.32 5.74 -11 -5 -8 9.87 3.48 ; _shelx_hkl_checksum 7669 _database_code_depnum_ccdc_archive 'CCDC 942653' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_complex4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common '[Pd(PSMePy)(PPh3)](OTf)2' _chemical_melting_point >478 _chemical_formula_moiety 'C33 H28 N5 P Pd S2, C2 F6 O6 S2' _chemical_formula_sum 'C35 H28 F6 N5 O6 P Pd S4' _chemical_formula_weight 994.23 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number ? _space_group_name_H-M_alt P21/a _space_group_name_Hall ? _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.7910(13) _cell_length_b 12.9731(6) _cell_length_c 18.4171(11) _cell_angle_alpha 90 _cell_angle_beta 110.727(2) _cell_angle_gamma 90 _cell_volume 3975.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30328 _cell_measurement_theta_min 3.073 _cell_measurement_theta_max 27.483 _exptl_crystal_description rhombic _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.661 _exptl_crystal_F_000 2000 _exptl_transmission_factor_min 0.7960 _exptl_transmission_factor_max 0.8569 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 0.797 _shelx_estimated_absorpt_T_min 0.796 _shelx_estimated_absorpt_T_max 0.857 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7960 _exptl_absorpt_correction_T_max 0.8569 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; Absorption correction was performed using REQAB (Rigaku, 1998) program. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_measurement_device_type 'Rigaku Saturn724+ (4x4 bin mode)' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30328 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.073 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_full 25.241 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 8934 _reflns_number_gt 7329 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics Ortep-III _computing_publication_material Ortep-III _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+4.1565P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8934 _refine_ls_number_parameters 540 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.81876(2) 0.86528(2) 0.77557(2) 0.02693(10) Uani 1 1 d . . . . . N1 N 0.90268(19) 0.8688(2) 0.88732(18) 0.0271(6) Uani 1 1 d . . . . . C1 C 0.8779(2) 0.8707(3) 0.9480(2) 0.0318(8) Uani 1 1 d . . . . . C2 C 0.9326(3) 0.8708(3) 1.0235(2) 0.0417(10) Uani 1 1 d . . . . . H1 H 0.9145 0.8716 1.0662 0.050 Uiso 1 1 calc R U . . . C3 C 1.0134(3) 0.8697(4) 1.0357(3) 0.0444(10) Uani 1 1 d . . . . . H2 H 1.0516 0.8707 1.0871 0.053 Uiso 1 1 calc R U . . . C4 C 1.0388(3) 0.8673(3) 0.9731(2) 0.0424(10) Uani 1 1 d . . . . . H3 H 1.0944 0.8651 0.9808 0.051 Uiso 1 1 calc R U . . . C5 C 0.9812(2) 0.8680(3) 0.8983(2) 0.0326(8) Uani 1 1 d . . . . . C6 C 0.7897(2) 0.8677(3) 0.9328(2) 0.0351(8) Uani 1 1 d . . . . . H4 H 0.7777 0.9167 0.9684 0.042 Uiso 1 1 calc R U . . . H5 H 0.7756 0.7978 0.9454 0.042 Uiso 1 1 calc R U . . . C7 C 1.0047(2) 0.8741(3) 0.8281(2) 0.0366(9) Uani 1 1 d . . . . . H6 H 1.0550 0.8347 0.8379 0.044 Uiso 1 1 calc R U . . . H7 H 1.0156 0.9469 0.8191 0.044 Uiso 1 1 calc R U . . . C8 C 0.7230(2) 1.0379(3) 0.8395(2) 0.0326(8) Uani 1 1 d . . . . . N2 N 0.6503(2) 1.0736(3) 0.8268(2) 0.0432(8) Uani 1 1 d . . . . . C9 C 0.6458(3) 1.1772(4) 0.8308(3) 0.0523(12) Uani 1 1 d . . . . . H8 H 0.5951 1.2081 0.8227 0.063 Uiso 1 1 calc R U . . . C10 C 0.7110(3) 1.2385(4) 0.8460(3) 0.0518(11) Uani 1 1 d . . . . . H9 H 0.7069 1.3114 0.8480 0.062 Uiso 1 1 calc R U . . . C11 C 0.7833(3) 1.1913(3) 0.8583(3) 0.0496(11) Uani 1 1 d . . . . . H10 H 0.8301 1.2328 0.8695 0.059 Uiso 1 1 calc R U . . . N3 N 0.7907(2) 1.0889(3) 0.8552(2) 0.0416(8) Uani 1 1 d . . . . . C12 C 0.9360(3) 0.6879(3) 0.7625(2) 0.0396(9) Uani 1 1 d . . . . . N4 N 0.8797(3) 0.6328(3) 0.7130(2) 0.0560(11) Uani 1 1 d . . . . . C13 C 0.8863(4) 0.5311(4) 0.7256(4) 0.0735(17) Uani 1 1 d . . . . . H11 H 0.8464 0.4871 0.6919 0.088 Uiso 1 1 calc R U . . . C14 C 0.9476(4) 0.4882(4) 0.7846(3) 0.0665(15) Uani 1 1 d . . . . . H12 H 0.9521 0.4157 0.7917 0.080 Uiso 1 1 calc R U . . . C15 C 1.0025(4) 0.5537(4) 0.8330(4) 0.0646(15) Uani 1 1 d . . . . . H13 H 1.0452 0.5255 0.8754 0.078 Uiso 1 1 calc R U . . . N5 N 0.9986(2) 0.6567(3) 0.8234(3) 0.0518(10) Uani 1 1 d . . . . . S1 S 0.72567(6) 0.89873(8) 0.83346(5) 0.0323(2) Uani 1 1 d . . . . . S2 S 0.92809(6) 0.82400(7) 0.74131(5) 0.0325(2) Uani 1 1 d . . . . . P1 P 0.72420(6) 0.86237(7) 0.65299(5) 0.0266(2) Uani 1 1 d . . . . . C16 C 0.6625(2) 0.7483(3) 0.6309(2) 0.0299(7) Uani 1 1 d . . . . . C17 C 0.6120(2) 0.7293(3) 0.5542(2) 0.0357(8) Uani 1 1 d . . . . . H14 H 0.6152 0.7718 0.5134 0.043 Uiso 1 1 calc R U . . . C18 C 0.5578(3) 0.6491(3) 0.5380(3) 0.0412(9) Uani 1 1 d . . . . . H15 H 0.5234 0.6366 0.4860 0.049 Uiso 1 1 calc R U . . . C19 C 0.5532(3) 0.5862(3) 0.5974(3) 0.0447(10) Uani 1 1 d . . . . . H16 H 0.5145 0.5324 0.5862 0.054 Uiso 1 1 calc R U . . . C20 C 0.6047(3) 0.6018(3) 0.6728(3) 0.0467(10) Uani 1 1 d . . . . . H17 H 0.6028 0.5574 0.7131 0.056 Uiso 1 1 calc R U . . . C21 C 0.6596(3) 0.6831(3) 0.6895(2) 0.0394(9) Uani 1 1 d . . . . . H18 H 0.6951 0.6938 0.7413 0.047 Uiso 1 1 calc R U . . . C22 C 0.7630(2) 0.8762(3) 0.5743(2) 0.0312(8) Uani 1 1 d . . . . . C23 C 0.7523(3) 0.9640(3) 0.5297(2) 0.0382(9) Uani 1 1 d . . . . . H19 H 0.7219 1.0199 0.5382 0.046 Uiso 1 1 calc R U . . . C24 C 0.7859(3) 0.9706(4) 0.4725(3) 0.0456(10) Uani 1 1 d . . . . . H20 H 0.7780 1.0310 0.4414 0.055 Uiso 1 1 calc R U . . . C25 C 0.8306(3) 0.8902(4) 0.4603(3) 0.0462(11) Uani 1 1 d . . . . . H21 H 0.8544 0.8957 0.4218 0.055 Uiso 1 1 calc R U . . . C26 C 0.8406(3) 0.8018(4) 0.5042(2) 0.0441(10) Uani 1 1 d . . . . . H22 H 0.8704 0.7458 0.4949 0.053 Uiso 1 1 calc R U . . . C27 C 0.8075(2) 0.7940(3) 0.5616(2) 0.0366(8) Uani 1 1 d . . . . . H23 H 0.8150 0.7333 0.5921 0.044 Uiso 1 1 calc R U . . . C28 C 0.6560(2) 0.9697(3) 0.6423(2) 0.0299(7) Uani 1 1 d . . . . . C29 C 0.6898(2) 1.0679(3) 0.6607(2) 0.0331(8) Uani 1 1 d . . . . . H24 H 0.7465 1.0758 0.6803 0.040 Uiso 1 1 calc R U . . . C30 C 0.6410(3) 1.1534(3) 0.6505(2) 0.0366(9) Uani 1 1 d . . . . . H25 H 0.6641 1.2201 0.6627 0.044 Uiso 1 1 calc R U . . . C31 C 0.5583(3) 1.1417(3) 0.6226(3) 0.0399(9) Uani 1 1 d . . . . . H26 H 0.5246 1.2006 0.6148 0.048 Uiso 1 1 calc R U . . . C32 C 0.5249(3) 1.0450(4) 0.6061(3) 0.0469(10) Uani 1 1 d . . . . . H27 H 0.4681 1.0375 0.5881 0.056 Uiso 1 1 calc R U . . . C33 C 0.5731(2) 0.9580(3) 0.6154(2) 0.0403(9) Uani 1 1 d . . . . . H28 H 0.5497 0.8915 0.6036 0.048 Uiso 1 1 calc R U . . . S3 S 0.94265(7) 1.14242(8) 0.71892(7) 0.0418(3) Uani 1 1 d . . . . . O1 O 0.9935(2) 1.1301(3) 0.6742(2) 0.0610(10) Uani 1 1 d . . . . . O2 O 0.8974(2) 1.0528(3) 0.7238(2) 0.0627(10) Uani 1 1 d . . . . . O3 O 0.9766(2) 1.1993(4) 0.7900(2) 0.0728(12) Uani 1 1 d . . . . . C34 C 0.8653(3) 1.2295(3) 0.6605(3) 0.0414(9) Uani 1 1 d . . . . . F1 F 0.82030(18) 1.1865(2) 0.59412(16) 0.0606(7) Uani 1 1 d . . . . . F2 F 0.81547(17) 1.2582(2) 0.69694(19) 0.0612(8) Uani 1 1 d . . . . . F3 F 0.89541(17) 1.31600(19) 0.64271(19) 0.0572(8) Uani 1 1 d . . . . . S4 S 0.75446(19) 0.5689(2) 0.91504(18) 0.0486(7) Uiso 0.55 1 d D . P A 1 C35 C 0.8494(7) 0.4943(8) 0.9469(5) 0.084(4) Uiso 0.55 1 d D . P A 1 F4 F 0.8464(4) 0.4279(5) 0.9987(4) 0.0996(19) Uiso 0.65 1 d D . P . . F5 F 0.9031(6) 0.5662(9) 0.9791(7) 0.131(4) Uiso 0.55 1 d D . P A 1 F6 F 0.8495(6) 0.4429(7) 0.8851(6) 0.107(3) Uiso 0.55 1 d D . P A 1 S5 S 0.7292(2) 0.5678(2) 0.91636(18) 0.0283(7) Uiso 0.35 1 d D . P A 2 C36 C 0.8186(9) 0.5330(12) 0.8905(10) 0.120(9) Uiso 0.35 1 d D . P A 2 F7 F 0.8642(11) 0.4578(15) 0.9330(11) 0.136(6) Uiso 0.35 1 d D . P A 2 F8 F 0.8712(8) 0.6094(10) 0.9036(8) 0.104(4) Uiso 0.35 1 d D . P A 2 F9 F 0.7885(10) 0.5018(13) 0.8169(9) 0.132(5) Uiso 0.35 1 d D . P A 2 O4 O 0.7660(5) 0.6456(5) 0.8645(4) 0.073(2) Uiso 0.55 1 d D . P A 1 O5 O 0.7602(6) 0.5900(8) 0.9927(4) 0.087(3) Uiso 0.55 1 d D . P A 1 O6 O 0.6942(5) 0.4944(7) 0.8747(5) 0.081(3) Uiso 0.55 1 d D . P A 1 S6 S 0.7364(9) 0.5540(7) 0.8856(9) 0.056(4) Uiso 0.1 1 d D . P A 3 C37 C 0.8351(12) 0.5187(15) 0.9619(17) 0.060(14) Uiso 0.1 1 d D . P A 3 F10 F 0.854(3) 0.603(3) 1.006(2) 0.098(12) Uiso 0.1 1 d D . P A 3 F11 F 0.9095(13) 0.527(2) 0.9615(15) 0.038(5) Uiso 0.1 1 d D . P A 3 O7 O 0.7074(5) 0.6583(5) 0.8717(4) 0.0542(18) Uiso 0.45 1 d D . P . . O8 O 0.7379(9) 0.6171(10) 0.9857(5) 0.062(3) Uiso 0.35 1 d D . P A 2 O9 O 0.6787(5) 0.4809(6) 0.8928(6) 0.039(2) Uiso 0.35 1 d D . P A 2 O10 O 0.6990(19) 0.493(2) 0.9272(19) 0.042(7) Uiso 0.1 1 d D . P A 3 O11 O 0.733(3) 0.500(3) 0.8174(18) 0.088(13) Uiso 0.1 1 d D . P A 3 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 0.02575(18) 0.02699(16) 0.02706(16) -0.00318(9) 0.00810(12) 0.00006(10) N1 0.0264(16) 0.0266(15) 0.0274(15) -0.0015(11) 0.0083(12) -0.0008(11) C1 0.032(2) 0.0309(18) 0.0293(18) -0.0020(14) 0.0071(16) -0.0007(14) C2 0.047(3) 0.045(2) 0.032(2) 0.0021(16) 0.0124(19) 0.0001(18) C3 0.036(2) 0.059(3) 0.032(2) -0.0012(18) 0.0042(18) 0.0020(19) C4 0.030(2) 0.054(3) 0.037(2) 0.0005(18) 0.0049(17) 0.0024(18) C5 0.030(2) 0.0345(19) 0.0317(19) -0.0020(14) 0.0082(16) -0.0006(14) C6 0.036(2) 0.039(2) 0.034(2) 0.0032(15) 0.0166(17) 0.0045(16) C7 0.028(2) 0.045(2) 0.035(2) -0.0002(16) 0.0097(16) -0.0001(16) C8 0.034(2) 0.037(2) 0.0257(17) 0.0007(14) 0.0092(15) 0.0034(16) N2 0.0348(19) 0.046(2) 0.052(2) 0.0034(16) 0.0194(16) 0.0093(15) C9 0.056(3) 0.048(3) 0.057(3) 0.004(2) 0.026(2) 0.022(2) C10 0.063(3) 0.037(2) 0.052(3) -0.002(2) 0.016(2) 0.006(2) C11 0.052(3) 0.035(2) 0.054(3) -0.0047(19) 0.010(2) -0.0046(19) N3 0.0372(19) 0.0349(18) 0.046(2) -0.0015(15) 0.0063(16) 0.0016(15) C12 0.042(2) 0.041(2) 0.041(2) -0.0015(17) 0.0217(19) 0.0091(18) N4 0.074(3) 0.036(2) 0.047(2) -0.0021(16) 0.007(2) -0.0003(18) C13 0.101(5) 0.037(3) 0.067(4) -0.005(2) 0.011(3) 0.000(3) C14 0.095(4) 0.037(2) 0.074(4) 0.002(2) 0.036(3) 0.017(3) C15 0.069(4) 0.052(3) 0.076(4) 0.017(3) 0.028(3) 0.029(3) N5 0.045(2) 0.049(2) 0.061(3) 0.0093(19) 0.018(2) 0.0166(18) S1 0.0287(5) 0.0345(5) 0.0338(5) -0.0042(4) 0.0113(4) 0.0001(4) S2 0.0315(5) 0.0344(5) 0.0333(5) -0.0021(4) 0.0134(4) 0.0017(4) P1 0.0260(5) 0.0262(4) 0.0262(4) -0.0029(3) 0.0076(4) -0.0017(3) C16 0.0286(18) 0.0292(17) 0.0336(18) -0.0054(14) 0.0129(15) -0.0030(14) C17 0.038(2) 0.0328(19) 0.0338(19) -0.0040(15) 0.0091(16) -0.0023(16) C18 0.039(2) 0.036(2) 0.043(2) -0.0109(17) 0.0078(19) -0.0073(17) C19 0.043(2) 0.035(2) 0.061(3) -0.0109(19) 0.024(2) -0.0132(18) C20 0.061(3) 0.037(2) 0.049(2) -0.0015(19) 0.028(2) -0.013(2) C21 0.044(2) 0.038(2) 0.037(2) -0.0027(16) 0.0143(18) -0.0076(18) C22 0.0286(19) 0.0349(18) 0.0275(17) -0.0054(14) 0.0068(15) -0.0051(15) C23 0.045(2) 0.0339(19) 0.038(2) -0.0025(16) 0.0174(18) -0.0070(17) C24 0.056(3) 0.042(2) 0.040(2) 0.0004(18) 0.020(2) -0.009(2) C25 0.050(3) 0.056(3) 0.042(2) -0.011(2) 0.027(2) -0.014(2) C26 0.044(2) 0.052(3) 0.040(2) -0.0129(19) 0.0197(19) -0.002(2) C27 0.038(2) 0.037(2) 0.0345(19) -0.0032(16) 0.0130(17) -0.0015(17) C28 0.0287(19) 0.0308(18) 0.0294(17) 0.0005(14) 0.0096(15) 0.0013(14) C29 0.034(2) 0.0338(19) 0.0328(18) 0.0007(15) 0.0134(16) -0.0017(15) C30 0.047(2) 0.0288(18) 0.039(2) 0.0029(15) 0.0208(18) 0.0008(16) C31 0.040(2) 0.039(2) 0.045(2) 0.0048(17) 0.0204(19) 0.0133(17) C32 0.034(2) 0.051(3) 0.055(3) -0.005(2) 0.014(2) 0.0060(19) C33 0.033(2) 0.040(2) 0.047(2) -0.0068(18) 0.0119(18) -0.0026(17) S3 0.0359(6) 0.0394(5) 0.0449(6) 0.0090(4) 0.0077(5) -0.0058(4) O1 0.060(2) 0.0455(19) 0.088(3) 0.0082(17) 0.039(2) 0.0134(16) O2 0.054(2) 0.0393(17) 0.085(3) 0.0251(17) 0.0134(19) -0.0078(15) O3 0.066(2) 0.097(3) 0.0427(19) -0.0024(19) 0.0035(17) -0.031(2) C34 0.047(2) 0.0288(19) 0.053(2) 0.0012(17) 0.023(2) -0.0065(17) F1 0.0599(18) 0.0611(18) 0.0469(15) 0.0055(13) 0.0017(13) -0.0042(14) F2 0.0573(17) 0.0530(17) 0.090(2) -0.0009(15) 0.0474(17) 0.0002(13) F3 0.0581(17) 0.0309(13) 0.095(2) 0.0133(13) 0.0428(17) -0.0006(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.072(3) . ? Pd1 P1 2.2890(10) . ? Pd1 S1 2.3061(10) . ? Pd1 S2 2.3102(10) . ? N1 C1 1.339(5) . ? N1 C5 1.340(5) . ? C1 C2 1.387(6) . ? C1 C6 1.494(6) . ? C2 C3 1.373(6) . ? C3 C4 1.379(6) . ? C4 C5 1.396(6) . ? C5 C7 1.495(6) . ? C6 S1 1.825(4) . ? C7 S2 1.814(4) . ? C8 N3 1.313(5) . ? C8 N2 1.314(5) . ? C8 S1 1.811(4) . ? N2 C9 1.350(6) . ? C9 C10 1.351(7) . ? C10 C11 1.370(7) . ? C11 N3 1.337(6) . ? C12 N4 1.304(6) . ? C12 N5 1.333(6) . ? C12 S2 1.803(4) . ? N4 C13 1.338(6) . ? C13 C14 1.356(8) . ? C14 C15 1.361(8) . ? C15 N5 1.347(6) . ? P1 C16 1.801(4) . ? P1 C28 1.811(4) . ? P1 C22 1.821(4) . ? C16 C21 1.386(5) . ? C16 C17 1.402(5) . ? C17 C18 1.378(5) . ? C18 C19 1.391(6) . ? C19 C20 1.381(7) . ? C20 C21 1.395(6) . ? C22 C23 1.377(5) . ? C22 C27 1.396(5) . ? C23 C24 1.387(6) . ? C24 C25 1.376(7) . ? C25 C26 1.378(7) . ? C26 C27 1.384(6) . ? C28 C33 1.387(5) . ? C28 C29 1.399(5) . ? C29 C30 1.379(5) . ? C30 C31 1.384(6) . ? C31 C32 1.376(6) . ? C32 C33 1.391(6) . ? S3 O1 1.433(4) . ? S3 O2 1.436(3) . ? S3 O3 1.437(4) . ? S3 C34 1.812(5) . ? C34 F1 1.324(5) . ? C34 F3 1.333(4) . ? C34 F2 1.339(5) . ? S4 O5 1.423(6) . ? S4 O4 1.426(6) . ? S4 O6 1.439(6) . ? S4 O7 1.487(7) . ? S4 C35 1.853(13) . ? C35 F4 1.301(8) . ? C35 F5 1.317(8) . ? C35 F6 1.320(8) . ? F4 C37 1.340(9) . ? F4 F7 1.410(19) . ? S5 O8 1.388(7) . ? S5 O7 1.408(6) . ? S5 O9 1.411(6) . ? S5 C36 1.869(14) . ? C36 F8 1.326(9) . ? C36 F7 1.331(9) . ? C36 F9 1.332(9) . ? O4 O7 1.110(10) . ? S6 O11 1.420(8) . ? S6 O10 1.423(8) . ? S6 O7 1.439(8) . ? S6 C37 1.876(14) . ? C37 F11 1.329(9) . ? C37 F10 1.334(10) . ? 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 P1 178.91(9) . . ? N1 Pd1 S1 85.38(9) . . ? P1 Pd1 S1 93.53(4) . . ? N1 Pd1 S2 84.04(9) . . ? P1 Pd1 S2 97.05(4) . . ? S1 Pd1 S2 169.05(4) . . ? C1 N1 C5 120.6(3) . . ? C1 N1 Pd1 119.7(3) . . ? C5 N1 Pd1 119.7(3) . . ? N1 C1 C2 121.0(4) . . ? N1 C1 C6 118.5(3) . . ? C2 C1 C6 120.4(4) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 119.8(4) . . ? C3 C4 C5 118.8(4) . . ? N1 C5 C4 120.7(4) . . ? N1 C5 C7 117.7(3) . . ? C4 C5 C7 121.5(4) . . ? C1 C6 S1 115.1(3) . . ? C5 C7 S2 113.0(3) . . ? N3 C8 N2 129.0(4) . . ? N3 C8 S1 118.3(3) . . ? N2 C8 S1 112.7(3) . . ? C8 N2 C9 114.5(4) . . ? N2 C9 C10 122.2(4) . . ? C9 C10 C11 117.3(4) . . ? N3 C11 C10 122.5(4) . . ? C8 N3 C11 114.5(4) . . ? N4 C12 N5 128.9(4) . . ? N4 C12 S2 113.8(3) . . ? N5 C12 S2 117.2(4) . . ? C12 N4 C13 114.9(5) . . ? N4 C13 C14 122.6(6) . . ? C13 C14 C15 117.2(5) . . ? N5 C15 C14 122.8(5) . . ? C12 N5 C15 113.6(5) . . ? C8 S1 C6 100.34(18) . . ? C8 S1 Pd1 104.74(13) . . ? C6 S1 Pd1 97.24(13) . . ? C12 S2 C7 100.5(2) . . ? C12 S2 Pd1 100.13(14) . . ? C7 S2 Pd1 96.85(14) . . ? C16 P1 C28 106.00(18) . . ? C16 P1 C22 105.88(17) . . ? C28 P1 C22 105.42(17) . . ? C16 P1 Pd1 114.36(13) . . ? C28 P1 Pd1 108.96(12) . . ? C22 P1 Pd1 115.47(13) . . ? C21 C16 C17 119.3(3) . . ? C21 C16 P1 120.9(3) . . ? C17 C16 P1 119.6(3) . . ? C18 C17 C16 120.0(4) . . ? C17 C18 C19 120.3(4) . . ? C20 C19 C18 120.1(4) . . ? C19 C20 C21 119.8(4) . . ? C16 C21 C20 120.4(4) . . ? C23 C22 C27 119.9(4) . . ? C23 C22 P1 123.0(3) . . ? C27 C22 P1 117.1(3) . . ? C22 C23 C24 119.9(4) . . ? C25 C24 C23 120.3(4) . . ? C24 C25 C26 119.9(4) . . ? C25 C26 C27 120.4(4) . . ? C26 C27 C22 119.5(4) . . ? C33 C28 C29 119.8(4) . . ? C33 C28 P1 122.8(3) . . ? C29 C28 P1 117.4(3) . . ? C30 C29 C28 120.3(4) . . ? C29 C30 C31 119.8(4) . . ? C32 C31 C30 120.1(4) . . ? C31 C32 C33 120.8(4) . . ? C28 C33 C32 119.1(4) . . ? O1 S3 O2 115.4(2) . . ? O1 S3 O3 115.7(2) . . ? O2 S3 O3 115.0(2) . . ? O1 S3 C34 103.3(2) . . ? O2 S3 C34 102.6(2) . . ? O3 S3 C34 101.9(2) . . ? F1 C34 F3 106.9(4) . . ? F1 C34 F2 106.8(4) . . ? F3 C34 F2 106.5(3) . . ? F1 C34 S3 111.7(3) . . ? F3 C34 S3 112.5(3) . . ? F2 C34 S3 112.0(3) . . ? O5 S4 O4 123.0(6) . . ? O5 S4 O6 115.1(6) . . ? O4 S4 O6 112.6(6) . . ? O5 S4 O7 102.5(6) . . ? O4 S4 O7 44.7(4) . . ? O6 S4 O7 94.1(5) . . ? O5 S4 C35 92.8(6) . . ? O4 S4 C35 104.2(5) . . ? O6 S4 C35 104.0(5) . . ? O7 S4 C35 148.7(5) . . ? F4 C35 F5 110.5(9) . . ? F4 C35 F6 108.1(10) . . ? F5 C35 F6 121.6(10) . . ? F4 C35 S4 108.0(8) . . ? F5 C35 S4 102.0(9) . . ? F6 C35 S4 105.7(7) . . ? O8 S5 O7 94.1(7) . . ? O8 S5 O9 120.2(8) . . ? O7 S5 O9 118.3(6) . . ? O8 S5 C36 121.1(8) . . ? O7 S5 C36 97.8(7) . . ? O9 S5 C36 103.6(6) . . ? F8 C36 F7 101.3(15) . . ? F8 C36 F9 114.6(16) . . ? F7 C36 F9 108.4(15) . . ? F8 C36 S5 112.6(11) . . ? F7 C36 S5 115.0(14) . . ? F9 C36 S5 105.1(12) . . ? C36 F7 F4 115.6(16) . . ? O7 O4 S4 70.6(5) . . ? O11 S6 O10 109(3) . . ? O11 S6 O7 114(2) . . ? O10 S6 O7 114.4(16) . . ? O11 S6 C37 106(3) . . ? O10 S6 C37 87.3(17) . . ? O7 S6 C37 123.0(11) . . ? F11 C37 F10 85(3) . . ? F11 C37 F4 95.8(17) . . ? F10 C37 F4 117(3) . . ? F11 C37 S6 130(2) . . ? F10 C37 S6 103(2) . . ? F4 C37 S6 121.8(12) . . ? O4 O7 S4 64.7(4) . . ? 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 C5 N1 C1 C2 -0.7(5) . . . . ? Pd1 N1 C1 C2 178.6(3) . . . . ? C5 N1 C1 C6 -177.8(3) . . . . ? Pd1 N1 C1 C6 1.4(4) . . . . ? N1 C1 C2 C3 0.5(6) . . . . ? C6 C1 C2 C3 177.6(4) . . . . ? C1 C2 C3 C4 -0.8(7) . . . . ? C2 C3 C4 C5 1.3(7) . . . . ? C1 N1 C5 C4 1.2(5) . . . . ? Pd1 N1 C5 C4 -178.1(3) . . . . ? C1 N1 C5 C7 -175.4(3) . . . . ? Pd1 N1 C5 C7 5.3(4) . . . . ? C3 C4 C5 N1 -1.5(6) . . . . ? C3 C4 C5 C7 175.0(4) . . . . ? N1 C1 C6 S1 -16.9(4) . . . . ? C2 C1 C6 S1 166.0(3) . . . . ? N1 C5 C7 S2 -26.4(4) . . . . ? C4 C5 C7 S2 157.1(3) . . . . ? N3 C8 N2 C9 -0.1(6) . . . . ? S1 C8 N2 C9 179.9(3) . . . . ? C8 N2 C9 C10 0.6(7) . . . . ? N2 C9 C10 C11 -0.8(8) . . . . ? C9 C10 C11 N3 0.5(8) . . . . ? N2 C8 N3 C11 -0.2(6) . . . . ? S1 C8 N3 C11 179.8(3) . . . . ? C10 C11 N3 C8 0.0(7) . . . . ? N5 C12 N4 C13 0.1(8) . . . . ? S2 C12 N4 C13 177.2(4) . . . . ? C12 N4 C13 C14 -1.2(9) . . . . ? N4 C13 C14 C15 1.8(10) . . . . ? C13 C14 C15 N5 -1.4(9) . . . . ? N4 C12 N5 C15 0.2(7) . . . . ? S2 C12 N5 C15 -176.8(4) . . . . ? C14 C15 N5 C12 0.5(8) . . . . ? N3 C8 S1 C6 63.0(3) . . . . ? N2 C8 S1 C6 -117.0(3) . . . . ? N3 C8 S1 Pd1 -37.4(3) . . . . ? N2 C8 S1 Pd1 142.6(3) . . . . ? C1 C6 S1 C8 -85.8(3) . . . . ? C1 C6 S1 Pd1 20.7(3) . . . . ? N4 C12 S2 C7 171.9(4) . . . . ? N5 C12 S2 C7 -10.7(4) . . . . ? N4 C12 S2 Pd1 72.9(4) . . . . ? N5 C12 S2 Pd1 -109.7(3) . . . . ? C5 C7 S2 C12 -71.6(3) . . . . ? C5 C7 S2 Pd1 30.1(3) . . . . ? C28 P1 C16 C21 -104.3(3) . . . . ? C22 P1 C16 C21 144.0(3) . . . . ? Pd1 P1 C16 C21 15.7(4) . . . . ? C28 P1 C16 C17 70.7(3) . . . . ? C22 P1 C16 C17 -40.9(4) . . . . ? Pd1 P1 C16 C17 -169.2(3) . . . . ? C21 C16 C17 C18 2.7(6) . . . . ? P1 C16 C17 C18 -172.4(3) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C17 C18 C19 C20 -2.1(7) . . . . ? C18 C19 C20 C21 2.2(7) . . . . ? C17 C16 C21 C20 -2.6(6) . . . . ? P1 C16 C21 C20 172.5(3) . . . . ? C19 C20 C21 C16 0.1(7) . . . . ? C16 P1 C22 C23 124.0(3) . . . . ? C28 P1 C22 C23 12.0(4) . . . . ? Pd1 P1 C22 C23 -108.3(3) . . . . ? C16 P1 C22 C27 -58.1(3) . . . . ? C28 P1 C22 C27 -170.1(3) . . . . ? Pd1 P1 C22 C27 69.6(3) . . . . ? C27 C22 C23 C24 -0.1(6) . . . . ? P1 C22 C23 C24 177.7(3) . . . . ? C22 C23 C24 C25 -0.6(6) . . . . ? C23 C24 C25 C26 1.4(7) . . . . ? C24 C25 C26 C27 -1.4(7) . . . . ? C25 C26 C27 C22 0.7(6) . . . . ? C23 C22 C27 C26 0.1(6) . . . . ? P1 C22 C27 C26 -177.9(3) . . . . ? C16 P1 C28 C33 -5.0(4) . . . . ? C22 P1 C28 C33 107.0(3) . . . . ? Pd1 P1 C28 C33 -128.5(3) . . . . ? C16 P1 C28 C29 176.4(3) . . . . ? C22 P1 C28 C29 -71.6(3) . . . . ? Pd1 P1 C28 C29 52.9(3) . . . . ? C33 C28 C29 C30 -1.5(6) . . . . ? P1 C28 C29 C30 177.1(3) . . . . ? C28 C29 C30 C31 0.5(6) . . . . ? C29 C30 C31 C32 0.9(6) . . . . ? C30 C31 C32 C33 -1.5(7) . . . . ? C29 C28 C33 C32 1.0(6) . . . . ? P1 C28 C33 C32 -177.6(3) . . . . ? C31 C32 C33 C28 0.5(7) . . . . ? O1 S3 C34 F1 66.2(3) . . . . ? O2 S3 C34 F1 -54.1(4) . . . . ? O3 S3 C34 F1 -173.4(3) . . . . ? O1 S3 C34 F3 -54.1(4) . . . . ? O2 S3 C34 F3 -174.4(3) . . . . ? O3 S3 C34 F3 66.3(4) . . . . ? O1 S3 C34 F2 -174.1(3) . . . . ? O2 S3 C34 F2 65.7(3) . . . . ? O3 S3 C34 F2 -53.7(3) . . . . ? O5 S4 C35 F4 49.4(8) . . . . ? O4 S4 C35 F4 174.6(7) . . . . ? O6 S4 C35 F4 -67.3(8) . . . . ? O7 S4 C35 F4 169.2(8) . . . . ? O5 S4 C35 F5 -67.0(8) . . . . ? O4 S4 C35 F5 58.1(8) . . . . ? O6 S4 C35 F5 176.3(8) . . . . ? O7 S4 C35 F5 52.8(12) . . . . ? O5 S4 C35 F6 165.0(8) . . . . ? O4 S4 C35 F6 -69.9(8) . . . . ? O6 S4 C35 F6 48.3(8) . . . . ? O7 S4 C35 F6 -75.2(12) . . . . ? F5 C35 F4 C37 71(3) . . . . ? F6 C35 F4 C37 -153(3) . . . . ? S4 C35 F4 C37 -39(2) . . . . ? F5 C35 F4 F7 -112(3) . . . . ? F6 C35 F4 F7 23.5(19) . . . . ? S4 C35 F4 F7 137(2) . . . . ? O8 S5 C36 F8 -45.6(16) . . . . ? O7 S5 C36 F8 53.9(13) . . . . ? O9 S5 C36 F8 175.6(12) . . . . ? O8 S5 C36 F7 69.8(16) . . . . ? O7 S5 C36 F7 169.3(14) . . . . ? O9 S5 C36 F7 -69.0(15) . . . . ? O8 S5 C36 F9 -171.0(12) . . . . ? O7 S5 C36 F9 -71.5(12) . . . . ? O9 S5 C36 F9 50.2(14) . . . . ? F8 C36 F7 F4 111.5(18) . . . . ? F9 C36 F7 F4 -127.6(16) . . . . ? S5 C36 F7 F4 -10(2) . . . . ? C35 F4 F7 C36 -28.8(14) . . . . ? C37 F4 F7 C36 -27.1(16) . . . . ? O5 S4 O4 O7 -73.1(9) . . . . ? O6 S4 O4 O7 71.9(7) . . . . ? C35 S4 O4 O7 -176.1(6) . . . . ? C35 F4 C37 F11 -49(2) . . . . ? F7 F4 C37 F11 -50.4(19) . . . . ? C35 F4 C37 F10 -135(4) . . . . ? F7 F4 C37 F10 -137(3) . . . . ? C35 F4 C37 S6 97(4) . . . . ? F7 F4 C37 S6 95(3) . . . . ? O11 S6 C37 F11 55(4) . . . . ? O10 S6 C37 F11 164(3) . . . . ? O7 S6 C37 F11 -78(4) . . . . ? O11 S6 C37 F10 149(3) . . . . ? O10 S6 C37 F10 -102(3) . . . . ? O7 S6 C37 F10 15(3) . . . . ? O11 S6 C37 F4 -77(4) . . . . ? O10 S6 C37 F4 31(3) . . . . ? O7 S6 C37 F4 149(2) . . . . ? S4 O4 O7 S5 -3.0(3) . . . . ? S4 O4 O7 S6 -24.1(7) . . . . ? O8 S5 O7 O4 112.8(8) . . . . ? O9 S5 O7 O4 -119.5(8) . . . . ? C36 S5 O7 O4 -9.4(8) . . . . ? O8 S5 O7 S6 160.6(17) . . . . ? O9 S5 O7 S6 -71.7(16) . . . . ? C36 S5 O7 S6 38.4(15) . . . . ? O8 S5 O7 S4 104.0(9) . . . . ? O9 S5 O7 S4 -128.3(10) . . . . ? C36 S5 O7 S4 -18.2(7) . . . . ? O11 S6 O7 O4 -71(3) . . . . ? O10 S6 O7 O4 163(2) . . . . ? C37 S6 O7 O4 59.0(15) . . . . ? O11 S6 O7 S5 162(3) . . . . ? O10 S6 O7 S5 36.3(18) . . . . ? C37 S6 O7 S5 -67.2(17) . . . . ? O11 S6 O7 S4 -154(3) . . . . ? O10 S6 O7 S4 80(2) . . . . ? C37 S6 O7 S4 -23.5(14) . . . . ? O5 S4 O7 O4 124.8(7) . . . . ? O6 S4 O7 O4 -118.4(7) . . . . ? C35 S4 O7 O4 7.4(12) . . . . ? O5 S4 O7 S5 -64.8(8) . . . . ? O4 S4 O7 S5 170.4(9) . . . . ? O6 S4 O7 S5 51.9(7) . . . . ? C35 S4 O7 S5 177.7(12) . . . . ? O5 S4 O7 S6 -148.0(19) . . . . ? O4 S4 O7 S6 87.2(18) . . . . ? O6 S4 O7 S6 -31.2(17) . . . . ? C35 S4 O7 S6 95(2) . . . . ? _refine_diff_density_max 0.861 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.100 _shelxl_version_number 2013-4 _shelx_res_file ; TITL complex4 REM Yadorkari-X generated CELL 0.71070 17.7910 12.9731 18.4171 90.0000 110.7268 90.0000 ZERR 4.0 0.0013 0.0006 0.0011 0.0000 0.0021 0.0000 LATT 1 SYMM 0.50000-X, 0.50000+Y,-Z REM SPGR P21/a monoclinic SFAC C H N O F P S Pd UNIT 140.000000 112.000000 20.000000 24.000000 24.000000 4.000000 16.000000 4.00 SIZE 0.30 0.20 0.20 TEMP -99.8 L.S. 10 FMAP 2 PLAN -100 ACTA CONF MERG 2 OMIT -10.000000 55.000000 OMIT 0 0 3 OMIT 4 0 1 SADI 0.01 S4 C35 S5 C36 S6 C37 SADI 0.01 S4 O4 S4 O5 S4 O6 S5 O7 S5 O8 S5 O9 S6 O7 S6 O10 S6 O11 SADI 0.01 C35 F4 C35 F5 C35 F6 C36 F7 C36 F8 C36 F9 C37 F10 C37 F11 C37 F4 MPLA Pd1 > N1 S1 > P1 MPLA N1 > C2 C3 C4 C5 RTAB ydkr C29 C8 MPLA C28 > C29 C30 C31 C32 C33 MPLA C8 > C9 C10 C11 N3 MPLA C28 > C29 C30 C31 C32 C33 MPLA C8 > C9 C10 C11 N3 WGHT 0.068400 4.156500 FVAR 1.33576 0.44367 PD1 8 0.818763 0.865282 0.775567 11.00000 0.02575 0.02699 = 0.02706 -0.00318 0.00810 0.00006 N1 3 0.902678 0.868819 0.887317 11.00000 0.02641 0.02657 = 0.02738 -0.00146 0.00834 -0.00080 C1 1 0.877898 0.870726 0.948002 11.00000 0.03230 0.03093 = 0.02925 -0.00198 0.00714 -0.00067 C2 1 0.932619 0.870816 1.023485 11.00000 0.04692 0.04481 = 0.03219 0.00210 0.01237 0.00010 AFIX 43 H1 2 0.914490 0.871621 1.066196 11.00000 -1.20000 AFIX 0 C3 1 1.013358 0.869726 1.035697 11.00000 0.03572 0.05932 = 0.03196 -0.00116 0.00422 0.00195 AFIX 43 H2 2 1.051587 0.870671 1.087073 11.00000 -1.20000 AFIX 0 C4 1 1.038767 0.867255 0.973128 11.00000 0.03013 0.05417 = 0.03723 0.00051 0.00487 0.00244 AFIX 43 H3 2 1.094438 0.865060 0.980824 11.00000 -1.20000 AFIX 0 C5 1 0.981235 0.868036 0.898266 11.00000 0.02955 0.03451 = 0.03168 -0.00200 0.00820 -0.00062 C6 1 0.789686 0.867671 0.932752 11.00000 0.03567 0.03879 = 0.03434 0.00319 0.01658 0.00451 AFIX 23 H4 2 0.777666 0.916737 0.968354 11.00000 -1.20000 H5 2 0.775561 0.797804 0.945375 11.00000 -1.20000 AFIX 0 C7 1 1.004713 0.874064 0.828079 11.00000 0.02792 0.04534 = 0.03537 -0.00024 0.00971 -0.00006 AFIX 23 H6 2 1.055015 0.834662 0.837946 11.00000 -1.20000 H7 2 1.015630 0.946885 0.819122 11.00000 -1.20000 AFIX 0 C8 1 0.723011 1.037938 0.839458 11.00000 0.03381 0.03727 = 0.02568 0.00072 0.00918 0.00340 N2 3 0.650343 1.073604 0.826769 11.00000 0.03479 0.04621 = 0.05190 0.00345 0.01939 0.00928 C9 1 0.645816 1.177239 0.830807 11.00000 0.05631 0.04768 = 0.05745 0.00373 0.02573 0.02227 AFIX 43 H8 2 0.595070 1.208116 0.822714 11.00000 -1.20000 AFIX 0 C10 1 0.711021 1.238513 0.845970 11.00000 0.06257 0.03738 = 0.05192 -0.00187 0.01587 0.00582 AFIX 43 H9 2 0.706868 1.311383 0.848000 11.00000 -1.20000 AFIX 0 C11 1 0.783340 1.191260 0.858292 11.00000 0.05163 0.03545 = 0.05429 -0.00466 0.00969 -0.00457 AFIX 43 H10 2 0.830073 1.232765 0.869450 11.00000 -1.20000 AFIX 0 N3 3 0.790654 1.088920 0.855209 11.00000 0.03724 0.03489 = 0.04598 -0.00148 0.00629 0.00160 C12 1 0.935951 0.687884 0.762547 11.00000 0.04230 0.04124 = 0.04084 -0.00147 0.02173 0.00907 N4 3 0.879676 0.632754 0.713000 11.00000 0.07368 0.03590 = 0.04687 -0.00209 0.00693 -0.00034 C13 1 0.886272 0.531055 0.725593 11.00000 0.10080 0.03676 = 0.06748 -0.00504 0.01068 -0.00015 AFIX 43 H11 2 0.846401 0.487051 0.691903 11.00000 -1.20000 AFIX 0 C14 1 0.947624 0.488245 0.784550 11.00000 0.09467 0.03664 = 0.07351 0.00218 0.03621 0.01662 AFIX 43 H12 2 0.952127 0.415683 0.791717 11.00000 -1.20000 AFIX 0 C15 1 1.002463 0.553685 0.833007 11.00000 0.06860 0.05213 = 0.07552 0.01728 0.02844 0.02861 AFIX 43 H13 2 1.045250 0.525495 0.875421 11.00000 -1.20000 AFIX 0 N5 3 0.998635 0.656701 0.823369 11.00000 0.04473 0.04928 = 0.06102 0.00926 0.01827 0.01660 S1 7 0.725666 0.898733 0.833457 11.00000 0.02874 0.03452 = 0.03380 -0.00422 0.01127 0.00012 S2 7 0.928091 0.823997 0.741308 11.00000 0.03151 0.03439 = 0.03326 -0.00208 0.01339 0.00166 P1 6 0.724203 0.862370 0.652992 11.00000 0.02604 0.02622 = 0.02618 -0.00286 0.00765 -0.00167 C16 1 0.662516 0.748301 0.630935 11.00000 0.02861 0.02917 = 0.03357 -0.00542 0.01286 -0.00296 C17 1 0.612047 0.729306 0.554192 11.00000 0.03756 0.03279 = 0.03378 -0.00395 0.00906 -0.00230 AFIX 43 H14 2 0.615239 0.771765 0.513355 11.00000 -1.20000 AFIX 0 C18 1 0.557804 0.649060 0.537970 11.00000 0.03881 0.03649 = 0.04285 -0.01092 0.00783 -0.00731 AFIX 43 H15 2 0.523441 0.636640 0.485969 11.00000 -1.20000 AFIX 0 C19 1 0.553176 0.586182 0.597447 11.00000 0.04304 0.03491 = 0.06064 -0.01087 0.02395 -0.01317 AFIX 43 H16 2 0.514487 0.532405 0.586202 11.00000 -1.20000 AFIX 0 C20 1 0.604711 0.601803 0.672780 11.00000 0.06141 0.03687 = 0.04886 -0.00151 0.02802 -0.01350 AFIX 43 H17 2 0.602817 0.557361 0.713093 11.00000 -1.20000 AFIX 0 C21 1 0.659589 0.683085 0.689506 11.00000 0.04410 0.03772 = 0.03651 -0.00266 0.01429 -0.00765 AFIX 43 H18 2 0.695137 0.693790 0.741312 11.00000 -1.20000 AFIX 0 C22 1 0.762981 0.876172 0.574304 11.00000 0.02859 0.03494 = 0.02746 -0.00537 0.00684 -0.00507 C23 1 0.752284 0.963965 0.529743 11.00000 0.04458 0.03386 = 0.03828 -0.00248 0.01740 -0.00695 AFIX 43 H19 2 0.721932 1.019912 0.538224 11.00000 -1.20000 AFIX 0 C24 1 0.785881 0.970607 0.472456 11.00000 0.05633 0.04239 = 0.04043 0.00035 0.02014 -0.00864 AFIX 43 H20 2 0.778016 1.030951 0.441422 11.00000 -1.20000 AFIX 0 C25 1 0.830552 0.890226 0.460346 11.00000 0.04986 0.05565 = 0.04172 -0.01129 0.02682 -0.01444 AFIX 43 H21 2 0.854433 0.895724 0.421818 11.00000 -1.20000 AFIX 0 C26 1 0.840587 0.801779 0.504177 11.00000 0.04442 0.05241 = 0.03955 -0.01294 0.01972 -0.00231 AFIX 43 H22 2 0.870405 0.745759 0.494932 11.00000 -1.20000 AFIX 0 C27 1 0.807487 0.794035 0.561604 11.00000 0.03831 0.03711 = 0.03450 -0.00318 0.01303 -0.00151 AFIX 43 H23 2 0.815009 0.733267 0.592145 11.00000 -1.20000 AFIX 0 C28 1 0.655990 0.969688 0.642295 11.00000 0.02870 0.03083 = 0.02945 0.00047 0.00958 0.00132 C29 1 0.689787 1.067942 0.660703 11.00000 0.03404 0.03382 = 0.03275 0.00074 0.01335 -0.00167 AFIX 43 H24 2 0.746547 1.075824 0.680289 11.00000 -1.20000 AFIX 0 C30 1 0.641045 1.153374 0.650535 11.00000 0.04655 0.02881 = 0.03909 0.00287 0.02080 0.00079 AFIX 43 H25 2 0.664146 1.220072 0.662658 11.00000 -1.20000 AFIX 0 C31 1 0.558346 1.141714 0.622610 11.00000 0.03959 0.03948 = 0.04512 0.00485 0.02040 0.01328 AFIX 43 H26 2 0.524641 1.200581 0.614825 11.00000 -1.20000 AFIX 0 C32 1 0.524895 1.044961 0.606112 11.00000 0.03372 0.05087 = 0.05502 -0.00486 0.01422 0.00603 AFIX 43 H27 2 0.468123 1.037468 0.588130 11.00000 -1.20000 AFIX 0 C33 1 0.573149 0.958001 0.615431 11.00000 0.03262 0.04010 = 0.04661 -0.00682 0.01194 -0.00255 AFIX 43 H28 2 0.549671 0.891475 0.603552 11.00000 -1.20000 AFIX 0 S3 7 0.942649 1.142424 0.718918 11.00000 0.03586 0.03939 = 0.04490 0.00896 0.00771 -0.00583 O1 4 0.993539 1.130119 0.674151 11.00000 0.05986 0.04550 = 0.08819 0.00816 0.03940 0.01342 O2 4 0.897372 1.052765 0.723820 11.00000 0.05439 0.03935 = 0.08526 0.02513 0.01344 -0.00777 O3 4 0.976607 1.199311 0.790027 11.00000 0.06609 0.09688 = 0.04266 -0.00242 0.00355 -0.03131 C34 1 0.865259 1.229542 0.660515 11.00000 0.04668 0.02877 = 0.05306 0.00121 0.02282 -0.00649 F1 5 0.820297 1.186549 0.594118 11.00000 0.05985 0.06113 = 0.04688 0.00552 0.00170 -0.00419 F2 5 0.815466 1.258208 0.696942 11.00000 0.05725 0.05302 = 0.09037 -0.00091 0.04738 0.00022 F3 5 0.895414 1.316003 0.642706 11.00000 0.05807 0.03092 = 0.09532 0.01329 0.04279 -0.00060 PART 1 S4 7 0.754455 0.568900 0.915038 10.55000 0.04856 C35 1 0.849408 0.494260 0.946899 10.55000 0.08374 PART 0 F4 5 0.846416 0.427863 0.998722 10.65000 0.09963 PART 1 F5 5 0.903136 0.566182 0.979082 10.55000 0.13106 F6 5 0.849548 0.442863 0.885085 10.55000 0.10688 PART 2 S5 7 0.729181 0.567752 0.916359 10.35000 0.02834 C36 1 0.818567 0.533034 0.890500 10.35000 0.11980 F7 5 0.864153 0.457842 0.932959 10.35000 0.13599 F8 5 0.871225 0.609384 0.903570 10.35000 0.10418 F9 5 0.788521 0.501763 0.816922 10.35000 0.13158 PART 1 O4 4 0.766036 0.645641 0.864524 10.55000 0.07321 O5 4 0.760217 0.590004 0.992673 10.55000 0.08658 O6 4 0.694180 0.494442 0.874675 10.55000 0.08082 PART 3 S6 7 0.736437 0.554033 0.885595 10.10000 0.05567 C37 1 0.835147 0.518742 0.961853 10.10000 0.06024 F10 5 0.853629 0.603412 1.005726 10.10000 0.09820 F11 5 0.909493 0.526733 0.961454 10.10000 0.03836 PART 0 O7 4 0.707366 0.658344 0.871691 10.45000 0.05422 PART 2 O8 4 0.737941 0.617112 0.985742 10.35000 0.06214 O9 4 0.678673 0.480879 0.892812 10.35000 0.03905 PART 3 O10 4 0.698982 0.492792 0.927196 10.10000 0.04185 O11 4 0.733115 0.500347 0.817355 10.10000 0.08762 PART 0 HKLF 4 REM complex4 REM R1 = 0.0535 for 7329 Fo > 4sig(Fo) and 0.0662 for all 8934 data REM 540 parameters refined using 75 restraints END WGHT 0.0684 4.1486 REM Highest difference peak 0.861, deepest hole -1.214, 1-sigma level 0.100 Q1 1 0.8348 0.3951 0.9679 11.00000 0.05 0.86 Q2 1 0.7315 0.6408 0.8592 11.00000 0.05 0.79 Q3 1 0.8461 0.6127 0.8694 11.00000 0.05 0.76 Q4 1 0.8189 0.4041 0.7767 11.00000 0.05 0.74 Q5 1 0.7174 0.5694 0.9897 11.00000 0.05 0.72 Q6 1 0.8195 0.4538 0.8473 11.00000 0.05 0.70 Q7 1 0.7632 0.6377 0.9797 11.00000 0.05 0.60 Q8 1 0.5428 0.8650 0.6734 11.00000 0.05 0.59 Q9 1 0.7684 0.8640 0.7058 11.00000 0.05 0.58 Q10 1 0.8363 0.8928 0.2819 11.00000 0.05 0.58 Q11 1 0.8926 0.4812 0.9170 11.00000 0.05 0.55 Q12 1 0.8293 0.5535 0.9421 11.00000 0.05 0.54 Q13 1 0.8805 0.6228 0.9449 11.00000 0.05 0.52 Q14 1 0.9197 0.9073 0.7284 11.00000 0.05 0.50 Q15 1 0.8754 0.8727 0.8484 11.00000 0.05 0.49 Q16 1 0.8882 0.5714 0.9336 11.00000 0.05 0.48 Q17 1 0.9019 0.6035 1.0183 11.00000 0.05 0.48 Q18 1 0.9250 1.3179 0.6988 11.00000 0.05 0.47 Q19 1 1.0028 1.1394 0.7893 11.00000 0.05 0.45 Q20 1 0.7978 0.5737 1.0088 11.00000 0.05 0.45 Q21 1 0.6394 0.8688 0.7969 11.00000 0.05 0.44 Q22 1 0.8736 0.6479 1.0031 11.00000 0.05 0.43 Q23 1 0.7396 0.8564 0.7777 11.00000 0.05 0.42 Q24 1 0.8578 1.2447 0.7475 11.00000 0.05 0.42 Q25 1 0.8094 0.9045 0.8424 11.00000 0.05 0.40 Q26 1 0.7276 0.4933 0.8586 11.00000 0.05 0.40 Q27 1 0.6810 0.9357 0.6530 11.00000 0.05 0.38 Q28 1 0.8670 0.7891 0.8193 11.00000 0.05 0.38 Q29 1 0.7790 0.7727 0.7514 11.00000 0.05 0.36 Q30 1 0.7749 0.9081 0.3460 11.00000 0.05 0.36 Q31 1 0.7819 0.9419 0.8082 11.00000 0.05 0.35 Q32 1 0.7173 0.8242 0.8211 11.00000 0.05 0.35 Q33 1 0.8893 0.8978 0.7711 11.00000 0.05 0.34 Q34 1 0.8327 0.7642 0.7786 11.00000 0.05 0.34 Q35 1 0.8398 1.0030 0.8691 11.00000 0.05 0.33 Q36 1 1.0463 0.9400 1.1116 11.00000 0.05 0.32 Q37 1 0.7466 0.6865 0.9198 11.00000 0.05 0.32 Q38 1 0.9590 1.2971 0.7330 11.00000 0.05 0.32 Q39 1 0.8491 0.8118 0.7275 11.00000 0.05 0.31 Q40 1 0.7883 0.5796 0.9108 11.00000 0.05 0.31 Q41 1 0.9177 0.3653 0.7256 11.00000 0.05 0.30 Q42 1 0.8978 0.8527 0.7882 11.00000 0.05 0.30 Q43 1 0.8393 0.9530 0.8191 11.00000 0.05 0.30 Q44 1 0.9294 0.4406 0.7480 11.00000 0.05 0.29 Q45 1 0.8327 0.6516 0.7077 11.00000 0.05 0.29 Q46 1 0.8577 1.0299 0.6607 11.00000 0.05 0.29 Q47 1 0.8372 1.2414 0.5990 11.00000 0.05 0.28 Q48 1 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0.24 Q70 1 0.7508 1.3273 0.9064 11.00000 0.05 0.24 Q71 1 0.8241 0.9689 0.6772 11.00000 0.05 0.24 Q72 1 0.9815 0.9682 0.7934 11.00000 0.05 0.24 Q73 1 0.9080 0.4942 0.7822 11.00000 0.05 0.24 Q74 1 1.0440 1.0912 0.6697 11.00000 0.05 0.24 Q75 1 0.9169 1.0420 0.6935 11.00000 0.05 0.24 Q76 1 0.8095 0.7719 0.8093 11.00000 0.05 0.24 Q77 1 0.6266 0.7875 0.8192 11.00000 0.05 0.24 Q78 1 0.6596 0.6135 0.6896 11.00000 0.05 0.24 Q79 1 0.7465 1.1622 0.9233 11.00000 0.05 0.24 Q80 1 0.9190 0.7645 0.8034 11.00000 0.05 0.23 Q81 1 0.7225 0.9369 0.5097 11.00000 0.05 0.23 Q82 1 0.5641 0.6206 0.5681 11.00000 0.05 0.23 Q83 1 0.7009 1.0006 0.8138 11.00000 0.05 0.23 Q84 1 0.7711 0.9497 0.7419 11.00000 0.05 0.23 Q85 1 0.6419 1.1188 0.5809 11.00000 0.05 0.23 Q86 1 0.6006 0.7865 0.7605 11.00000 0.05 0.23 Q87 1 0.8439 1.1033 0.7734 11.00000 0.05 0.23 Q88 1 0.6393 0.9218 0.7085 11.00000 0.05 0.23 Q89 1 0.7367 1.0704 0.8191 11.00000 0.05 0.23 Q90 1 0.8507 0.7426 0.8685 11.00000 0.05 0.23 Q91 1 0.6671 0.7999 0.9309 11.00000 0.05 0.23 Q92 1 0.7892 0.8533 0.8329 11.00000 0.05 0.23 Q93 1 0.8339 0.8391 0.6179 11.00000 0.05 0.23 Q94 1 0.6205 0.9879 0.8541 11.00000 0.05 0.22 Q95 1 0.7765 0.8965 0.8909 11.00000 0.05 0.22 Q96 1 0.9958 0.9880 0.9176 11.00000 0.05 0.22 Q97 1 0.8890 0.6461 0.4884 11.00000 0.05 0.22 Q98 1 0.8914 1.1929 0.6889 11.00000 0.05 0.22 Q99 1 0.9000 0.9884 0.8690 11.00000 0.05 0.22 Q100 1 0.7633 0.4370 0.8451 11.00000 0.05 0.22 ; _shelx_res_checksum 57273 _shelx_hkl_file ; 0 0 -3 904.17 116.79 0 0 3 1033.39 91.66 0 0 -3 1092.71 51.12 0 0 3 1263.15 109.91 0 0 -4 1320.51 121.20 0 0 4 1532.40 158.17 0 0 -4 1307.73 65.35 0 0 4 1905.75 562.21 0 0 -5 7700.75 377.54 0 0 5 7437.75 345.29 0 0 -5 7562.51 355.93 0 0 5 7416.99 328.59 0 0 -6 5664.11 275.36 0 0 6 7211.52 336.79 0 0 -6 5780.42 271.57 0 0 6 6927.13 316.47 0 0 -7 2001.55 130.21 0 0 7 1906.23 135.17 0 0 -7 2130.72 135.36 0 0 7 2304.21 353.25 0 0 8 3620.15 357.91 0 0 -8 3219.30 185.16 0 0 8 3593.41 466.93 0 0 9 3700.81 334.45 0 0 9 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