data_stahl217 _audit_creation_date 2015-06-30 _audit_creation_method ; Olex2 1.2 (compiled 2015.02.20 svn.r3157 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C18 H25 N3 O2 Pd' _chemical_formula_sum 'C18 H25 N3 O2 Pd' _chemical_formula_weight 421.81 _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.600(3) _cell_length_b 10.020(3) _cell_length_c 11.759(4) _cell_angle_alpha 109.470(18) _cell_angle_beta 104.215(11) _cell_angle_gamma 99.016(16) _cell_volume 998.0(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9898 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.631 _cell_measurement_theta_min 2.267 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 432 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 24590 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 30.742 _diffrn_reflns_theta_min 1.939 _diffrn_ambient_temperature 100.05 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5631 _reflns_number_total 6186 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.625 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.081 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 224 _refine_ls_number_reflns 6186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0244 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+0.5195P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.0536 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5) 2.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B, H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.21259(2) 0.01017(2) 0.50005(2) 0.01114(4) Uani 1 1 d . . . . . O1 O 0.17637(15) -0.14647(14) 0.12001(11) 0.0238(3) Uani 1 1 d . . . . . O2 O 0.32416(12) 0.11380(13) 0.31505(11) 0.0176(2) Uani 1 1 d . . . . . N1 N 0.22658(14) 0.00385(15) 0.33078(13) 0.0145(3) Uani 1 1 d . . . . . N2 N 0.45671(15) 0.31651(15) 0.66178(13) 0.0173(3) Uani 1 1 d . . . . . N3 N 0.18275(15) -0.03518(15) 0.74139(13) 0.0155(3) Uani 1 1 d . . . . . C1 C 0.07524(16) -0.19009(17) 0.38557(15) 0.0136(3) Uani 1 1 d . . . . . C2 C -0.00676(17) -0.29366(19) 0.41579(16) 0.0184(3) Uani 1 1 d . . . . . H2 H -0.0052 -0.2714 0.5013 0.022 Uiso 1 1 calc R . . . . C3 C -0.09091(19) -0.4294(2) 0.32147(18) 0.0237(4) Uani 1 1 d . . . . . H3 H -0.1455 -0.4990 0.3437 0.028 Uiso 1 1 calc R . . . . C4 C -0.09622(19) -0.4647(2) 0.19567(17) 0.0239(4) Uani 1 1 d . . . . . H4 H -0.1543 -0.5573 0.1319 0.029 Uiso 1 1 calc R . . . . C5 C -0.01548(18) -0.36271(19) 0.16439(16) 0.0198(3) Uani 1 1 d . . . . . H5 H -0.0181 -0.3852 0.0786 0.024 Uiso 1 1 calc R . . . . C6 C 0.06901(17) -0.22796(17) 0.25816(15) 0.0146(3) Uani 1 1 d . . . . . C7 C 0.16228(17) -0.12031(18) 0.22658(15) 0.0159(3) Uani 1 1 d . . . . . C8 C 0.46674(18) 0.0841(2) 0.33249(18) 0.0227(4) Uani 1 1 d . . . . . H8A H 0.4583 -0.0108 0.2672 0.034 Uiso 1 1 calc GR . . . . H8B H 0.5036 0.0816 0.4170 0.034 Uiso 1 1 calc GR . . . . H8C H 0.5363 0.1613 0.3253 0.034 Uiso 1 1 calc GR . . . . C9 C 0.36440(18) 0.20938(18) 0.60381(15) 0.0169(3) Uani 1 1 d . . . . . C10 C 0.57477(18) 0.45268(19) 0.73334(17) 0.0218(3) Uani 1 1 d . . . . . C11 C 0.6791(2) 0.4576(2) 0.6557(2) 0.0336(5) Uani 1 1 d . . . . . H11A H 0.7200 0.3720 0.6423 0.050 Uiso 1 1 calc GR . . . . H11B H 0.7605 0.5474 0.7015 0.050 Uiso 1 1 calc GR . . . . H11C H 0.6241 0.4566 0.5732 0.050 Uiso 1 1 calc GR . . . . C12 C 0.6525(2) 0.4498(2) 0.86191(18) 0.0328(5) Uani 1 1 d . . . . . H12A H 0.5806 0.4434 0.9076 0.049 Uiso 1 1 calc GR . . . . H12B H 0.7331 0.5397 0.9121 0.049 Uiso 1 1 calc GR . . . . H12C H 0.6939 0.3646 0.8487 0.049 Uiso 1 1 calc GR . . . . C13 C 0.5007(2) 0.5786(2) 0.7497(2) 0.0320(5) Uani 1 1 d . . . . . H13A H 0.4418 0.5713 0.6660 0.048 Uiso 1 1 calc GR . . . . H13B H 0.5773 0.6722 0.7925 0.048 Uiso 1 1 calc GR . . . . H13C H 0.4354 0.5734 0.8013 0.048 Uiso 1 1 calc GR . . . . C14 C 0.18862(17) -0.01604(17) 0.65182(15) 0.0148(3) Uani 1 1 d . . . . . C15 C 0.18074(17) -0.06397(17) 0.85520(14) 0.0143(3) Uani 1 1 d . . . . . C16 C 0.30498(17) -0.13829(19) 0.88264(16) 0.0176(3) Uani 1 1 d . . . . . H16A H 0.2844 -0.2319 0.8112 0.026 Uiso 1 1 calc GR . . . . H16B H 0.3101 -0.1560 0.9605 0.026 Uiso 1 1 calc GR . . . . H16C H 0.4002 -0.0747 0.8939 0.026 Uiso 1 1 calc GR . . . . C17 C 0.2100(2) 0.0832(2) 0.96343(16) 0.0238(4) Uani 1 1 d . . . . . H17A H 0.3045 0.1473 0.9741 0.036 Uiso 1 1 calc GR . . . . H17B H 0.2152 0.0682 1.0424 0.036 Uiso 1 1 calc GR . . . . H17C H 0.1291 0.1288 0.9435 0.036 Uiso 1 1 calc GR . . . . C18 C 0.02904(17) -0.1651(2) 0.82532(17) 0.0201(3) Uani 1 1 d . . . . . H18A H -0.0490 -0.1167 0.8041 0.030 Uiso 1 1 calc GR . . . . H18B H 0.0249 -0.1872 0.8997 0.030 Uiso 1 1 calc GR . . . . H18C H 0.0136 -0.2564 0.7529 0.030 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 0.01315(5) 0.01159(6) 0.00975(6) 0.00509(4) 0.00427(4) 0.00313(4) O1 0.0347(7) 0.0268(7) 0.0128(6) 0.0099(5) 0.0094(5) 0.0078(5) O2 0.0189(5) 0.0185(6) 0.0227(6) 0.0144(5) 0.0099(5) 0.0053(5) N1 0.0168(6) 0.0164(7) 0.0136(6) 0.0097(5) 0.0059(5) 0.0030(5) N2 0.0190(6) 0.0156(7) 0.0156(7) 0.0047(5) 0.0044(5) 0.0050(5) N3 0.0184(6) 0.0156(7) 0.0130(6) 0.0053(5) 0.0062(5) 0.0045(5) C1 0.0129(6) 0.0143(7) 0.0137(7) 0.0053(6) 0.0042(5) 0.0044(5) C2 0.0172(7) 0.0209(8) 0.0175(8) 0.0085(7) 0.0060(6) 0.0029(6) C3 0.0209(8) 0.0184(8) 0.0290(10) 0.0102(7) 0.0062(7) -0.0019(6) C4 0.0231(8) 0.0169(8) 0.0217(9) 0.0034(7) -0.0001(7) -0.0011(6) C5 0.0222(8) 0.0190(8) 0.0149(8) 0.0050(6) 0.0022(6) 0.0059(6) C6 0.0159(7) 0.0157(7) 0.0136(7) 0.0071(6) 0.0041(5) 0.0058(6) C7 0.0181(7) 0.0187(8) 0.0133(7) 0.0087(6) 0.0041(6) 0.0072(6) C8 0.0192(8) 0.0254(9) 0.0301(10) 0.0154(8) 0.0122(7) 0.0069(7) C9 0.0204(7) 0.0188(8) 0.0140(7) 0.0073(6) 0.0073(6) 0.0068(6) C10 0.0169(7) 0.0143(8) 0.0241(9) 0.0020(7) -0.0013(6) 0.0009(6) C11 0.0225(9) 0.0319(11) 0.0461(13) 0.0174(10) 0.0105(8) 0.0024(8) C12 0.0306(10) 0.0311(11) 0.0233(10) 0.0020(8) -0.0043(8) 0.0112(8) C13 0.0275(9) 0.0157(9) 0.0395(12) 0.0032(8) -0.0019(8) 0.0063(7) C14 0.0149(6) 0.0134(7) 0.0149(7) 0.0040(6) 0.0046(5) 0.0036(6) C15 0.0193(7) 0.0166(7) 0.0102(7) 0.0070(6) 0.0067(5) 0.0056(6) C16 0.0161(7) 0.0228(8) 0.0170(8) 0.0098(7) 0.0065(6) 0.0069(6) C17 0.0388(10) 0.0205(9) 0.0151(8) 0.0065(7) 0.0129(7) 0.0102(8) C18 0.0171(7) 0.0284(9) 0.0217(8) 0.0160(7) 0.0090(6) 0.0065(7) _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 2.0085(14) . ? Pd1 C1 2.0188(17) . ? Pd1 C9 2.0466(19) . ? Pd1 C14 1.9498(17) . ? O1 C7 1.238(2) . ? O2 N1 1.4223(17) . ? O2 C8 1.4262(19) . ? N1 C7 1.342(2) . ? N2 C9 1.149(2) . ? N2 C10 1.462(2) . ? N3 C14 1.144(2) . ? N3 C15 1.464(2) . ? C1 C2 1.396(2) . ? C1 C6 1.401(2) . ? C2 H2 0.9500 . ? C2 C3 1.394(2) . ? C3 H3 0.9500 . ? C3 C4 1.387(3) . ? C4 H4 0.9500 . ? C4 C5 1.387(3) . ? C5 H5 0.9500 . ? C5 C6 1.386(2) . ? C6 C7 1.494(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.517(3) . ? C10 C12 1.525(3) . ? C10 C13 1.524(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 C16 1.527(2) . ? C15 C17 1.522(2) . ? C15 C18 1.523(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C1 80.08(6) . . ? N1 Pd1 C9 95.09(6) . . ? C1 Pd1 C9 174.17(6) . . ? C14 Pd1 N1 171.30(6) . . ? C14 Pd1 C1 91.76(7) . . ? C14 Pd1 C9 92.88(7) . . ? N1 O2 C8 108.55(11) . . ? O2 N1 Pd1 124.09(10) . . ? C7 N1 Pd1 119.86(11) . . ? C7 N1 O2 114.97(13) . . ? C9 N2 C10 178.92(17) . . ? C14 N3 C15 177.12(15) . . ? C2 C1 Pd1 129.86(12) . . ? C2 C1 C6 117.58(15) . . ? C6 C1 Pd1 112.51(12) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.51(16) . . ? C3 C2 H2 119.7 . . ? C2 C3 H3 119.5 . . ? C4 C3 C2 121.07(17) . . ? C4 C3 H3 119.5 . . ? C3 C4 H4 120.5 . . ? C5 C4 C3 118.97(17) . . ? C5 C4 H4 120.5 . . ? C4 C5 H5 120.0 . . ? C6 C5 C4 120.05(16) . . ? C6 C5 H5 120.0 . . ? C1 C6 C7 117.70(14) . . ? C5 C6 C1 121.81(16) . . ? C5 C6 C7 120.44(15) . . ? O1 C7 N1 127.14(16) . . ? O1 C7 C6 123.61(15) . . ? N1 C7 C6 109.25(14) . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 Pd1 175.58(14) . . ? N2 C10 C11 107.31(15) . . ? N2 C10 C12 107.50(16) . . ? N2 C10 C13 107.18(14) . . ? C11 C10 C12 112.17(16) . . ? C11 C10 C13 111.43(17) . . ? C13 C10 C12 110.97(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 Pd1 175.38(13) . . ? N3 C15 C16 106.85(12) . . ? N3 C15 C17 107.45(13) . . ? N3 C15 C18 107.66(13) . . ? C17 C15 C16 111.02(14) . . ? C17 C15 C18 112.50(14) . . ? C18 C15 C16 111.08(14) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 C7 O1 -170.51(13) . . . . ? Pd1 N1 C7 C6 8.74(16) . . . . ? Pd1 C1 C2 C3 -177.27(12) . . . . ? Pd1 C1 C6 C5 178.11(12) . . . . ? Pd1 C1 C6 C7 0.72(17) . . . . ? O2 N1 C7 O1 -1.9(2) . . . . ? O2 N1 C7 C6 177.37(11) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C1 C6 C7 O1 173.36(14) . . . . ? C1 C6 C7 N1 -5.92(19) . . . . ? C2 C1 C6 C5 0.3(2) . . . . ? C2 C1 C6 C7 -177.13(13) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C5 C6 C1 -0.4(2) . . . . ? C4 C5 C6 C7 176.95(14) . . . . ? C5 C6 C7 O1 -4.1(2) . . . . ? C5 C6 C7 N1 176.65(14) . . . . ? C6 C1 C2 C3 0.1(2) . . . . ? C8 O2 N1 Pd1 84.21(14) . . . . ? C8 O2 N1 C7 -83.88(16) . . . . ? _shelx_res_file ; stahl217.res created by SHELXL-2014/7 TITL Stahl217b in P-1 #2 REM reset to P-1 #2 CELL 0.71073 9.59977 10.02039 11.75891 109.4696 104.2149 99.0163 ZERR 2 0.00314 0.00282 0.0037 0.0177 0.011 0.0162 LATT 1 SFAC C H N O Pd UNIT 36 50 6 4 2 L.S. 12 PLAN 2 TEMP -173.1 BOND MORE -1 BOND $H CONF fmap 2 53 acta 50 OMIT -6 6 0 OMIT 6 -6 3 REM REM REM WGHT 0.017000 0.519500 FVAR 0.17274 PD1 5 0.212587 0.010167 0.500053 11.00000 0.01315 0.01159 = 0.00975 0.00509 0.00427 0.00313 O1 4 0.176366 -0.146471 0.120013 11.00000 0.03471 0.02680 = 0.01280 0.00994 0.00943 0.00785 O2 4 0.324161 0.113800 0.315054 11.00000 0.01887 0.01850 = 0.02266 0.01439 0.00990 0.00528 N1 3 0.226585 0.003850 0.330782 11.00000 0.01680 0.01638 = 0.01358 0.00974 0.00591 0.00304 N2 3 0.456706 0.316506 0.661782 11.00000 0.01900 0.01560 = 0.01563 0.00474 0.00445 0.00502 N3 3 0.182753 -0.035182 0.741387 11.00000 0.01835 0.01563 = 0.01304 0.00531 0.00618 0.00450 C1 1 0.075236 -0.190088 0.385572 11.00000 0.01288 0.01429 = 0.01373 0.00533 0.00423 0.00436 C2 1 -0.006758 -0.293656 0.415792 11.00000 0.01722 0.02086 = 0.01752 0.00846 0.00599 0.00290 AFIX 43 H2 2 -0.005183 -0.271410 0.501278 11.00000 -1.20000 AFIX 0 C3 1 -0.090910 -0.429448 0.321475 11.00000 0.02089 0.01844 = 0.02902 0.01016 0.00625 -0.00191 AFIX 43 H3 2 -0.145506 -0.498957 0.343712 11.00000 -1.20000 AFIX 0 C4 1 -0.096222 -0.464722 0.195665 11.00000 0.02313 0.01686 = 0.02168 0.00336 -0.00006 -0.00114 AFIX 43 H4 2 -0.154271 -0.557326 0.131929 11.00000 -1.20000 AFIX 0 C5 1 -0.015485 -0.362714 0.164390 11.00000 0.02224 0.01902 = 0.01488 0.00502 0.00218 0.00589 AFIX 43 H5 2 -0.018077 -0.385191 0.078645 11.00000 -1.20000 AFIX 0 C6 1 0.069009 -0.227961 0.258156 11.00000 0.01588 0.01571 = 0.01356 0.00708 0.00408 0.00584 C7 1 0.162281 -0.120306 0.226575 11.00000 0.01806 0.01867 = 0.01325 0.00874 0.00408 0.00720 C8 1 0.466738 0.084140 0.332489 11.00000 0.01922 0.02545 = 0.03014 0.01542 0.01219 0.00691 AFIX 137 H8A 2 0.458282 -0.010850 0.267164 11.00000 -1.50000 H8B 2 0.503598 0.081604 0.417002 11.00000 -1.50000 H8C 2 0.536306 0.161284 0.325282 11.00000 -1.50000 AFIX 0 C9 1 0.364402 0.209376 0.603811 11.00000 0.02038 0.01878 = 0.01401 0.00731 0.00734 0.00679 C10 1 0.574774 0.452681 0.733342 11.00000 0.01692 0.01426 = 0.02407 0.00205 -0.00135 0.00086 C11 1 0.679115 0.457597 0.655714 11.00000 0.02252 0.03193 = 0.04607 0.01740 0.01046 0.00242 AFIX 137 H11A 2 0.720047 0.372025 0.642285 11.00000 -1.50000 H11B 2 0.760540 0.547387 0.701540 11.00000 -1.50000 H11C 2 0.624146 0.456554 0.573182 11.00000 -1.50000 AFIX 0 C12 1 0.652538 0.449846 0.861914 11.00000 0.03056 0.03112 = 0.02328 0.00196 -0.00433 0.01122 AFIX 137 H12A 2 0.580609 0.443400 0.907570 11.00000 -1.50000 H12B 2 0.733051 0.539737 0.912091 11.00000 -1.50000 H12C 2 0.693937 0.364577 0.848718 11.00000 -1.50000 AFIX 0 C13 1 0.500700 0.578637 0.749738 11.00000 0.02755 0.01567 = 0.03951 0.00321 -0.00193 0.00635 AFIX 137 H13A 2 0.441754 0.571339 0.666006 11.00000 -1.50000 H13B 2 0.577279 0.672199 0.792459 11.00000 -1.50000 H13C 2 0.435432 0.573374 0.801294 11.00000 -1.50000 AFIX 0 C14 1 0.188617 -0.016038 0.651818 11.00000 0.01493 0.01338 = 0.01486 0.00399 0.00462 0.00355 C15 1 0.180743 -0.063966 0.855200 11.00000 0.01928 0.01656 = 0.01019 0.00704 0.00673 0.00564 C16 1 0.304984 -0.138288 0.882635 11.00000 0.01613 0.02278 = 0.01697 0.00984 0.00650 0.00687 AFIX 137 H16A 2 0.284444 -0.231912 0.811160 11.00000 -1.50000 H16B 2 0.310091 -0.155955 0.960483 11.00000 -1.50000 H16C 2 0.400167 -0.074707 0.893874 11.00000 -1.50000 AFIX 0 C17 1 0.209983 0.083197 0.963430 11.00000 0.03879 0.02052 = 0.01509 0.00651 0.01293 0.01024 AFIX 137 H17A 2 0.304529 0.147337 0.974055 11.00000 -1.50000 H17B 2 0.215182 0.068203 1.042419 11.00000 -1.50000 H17C 2 0.129065 0.128800 0.943498 11.00000 -1.50000 AFIX 0 C18 1 0.029043 -0.165074 0.825325 11.00000 0.01710 0.02837 = 0.02169 0.01597 0.00897 0.00649 AFIX 137 H18A 2 -0.048960 -0.116710 0.804110 11.00000 -1.50000 H18B 2 0.024879 -0.187199 0.899750 11.00000 -1.50000 H18C 2 0.013600 -0.256370 0.752891 11.00000 -1.50000 AFIX 0 HKLF 4 REM Stahl217b in P-1 #2 REM R1 = 0.0244 for 5631 Fo > 4sig(Fo) and 0.0289 for all 6186 data REM 224 parameters refined using 0 restraints END WGHT 0.0170 0.5196 REM Highest difference peak 0.625, deepest hole -0.517, 1-sigma level 0.081 Q1 1 0.2809 -0.0361 0.5053 11.00000 0.05 0.63 Q2 1 0.2451 -0.0889 0.8757 11.00000 0.05 0.52 ; _shelx_res_checksum 34008 _shelx_hkl_file ; -1 0 0 65.05 2.23 -1 0 0 60.71 2.19 -1 0 0 70.32 2.21 -1 0 0 69.16 2.23 1 0 0 71.33 2.23 1 0 0 67.95 2.21 1 0 0 72.38 2.29 1 0 0 67.20 2.26 -2 0 0 132.88 4.46 -2 0 0 133.20 4.45 -2 0 0 128.91 4.38 -2 0 0 137.72 4.42 2 0 0 136.38 4.45 2 0 0 136.32 4.56 2 0 0 145.10 4.42 -3 0 0 97.88 3.35 -3 0 0 87.70 3.24 -3 0 0 100.56 3.35 -3 0 0 102.31 3.30 3 0 0 98.83 3.46 3 0 0 99.17 3.29 3 0 0 103.24 3.52 -4 0 0 72.48 2.45 -4 0 0 70.60 2.56 -4 0 0 71.17 2.49 -4 0 0 74.43 2.58 4 0 0 66.95 2.73 4 0 0 70.74 2.69 -5 0 0 114.37 4.04 -5 0 0 114.22 3.95 -5 0 0 110.58 3.89 -5 0 0 118.22 4.04 5 0 0 116.57 4.22 5 0 0 117.64 4.31 -6 0 0 12.33 0.71 -6 0 0 12.47 0.77 -6 0 0 10.61 0.64 -6 0 0 12.74 0.77 6 0 0 12.70 0.95 6 0 0 13.11 0.98 -7 0 0 81.40 3.25 -7 0 0 86.41 3.09 -7 0 0 91.68 3.28 7 0 0 82.99 3.50 7 0 0 89.41 3.65 -8 0 0 28.88 1.30 -8 0 0 26.84 1.42 8 0 0 27.09 1.72 8 0 0 30.04 1.70 -9 0 0 37.37 1.69 9 0 0 40.51 2.25 9 0 0 39.44 2.17 -10 0 0 24.93 1.29 10 0 0 23.74 1.76 10 0 0 24.71 1.74 -11 0 0 1.57 0.39 11 0 0 1.53 0.62 11 0 0 1.02 0.54 -12 0 0 7.56 0.81 12 0 0 6.89 1.21 12 0 0 5.50 1.13 13 -1 0 0.85 0.60 13 -1 0 0.61 0.63 -13 1 0 0.41 0.30 12 -1 0 16.69 1.76 12 -1 0 16.19 1.75 -12 1 0 17.15 1.03 11 -1 0 1.44 0.57 11 -1 0 0.76 0.61 -11 1 0 1.03 0.31 10 -1 0 23.32 1.69 10 -1 0 25.46 1.70 -10 1 0 22.88 1.16 9 -1 0 30.88 1.85 9 -1 0 32.79 1.92 -9 1 0 28.95 1.34 -9 1 0 32.58 1.66 8 -1 0 47.90 2.37 8 -1 0 45.15 2.37 -8 1 0 51.33 2.17 -8 1 0 49.80 2.20 -8 1 0 51.93 1.91 7 -1 0 101.42 3.98 7 -1 0 111.12 4.10 -7 1 0 100.25 3.56 -7 1 0 98.61 3.49 -7 1 0 98.07 3.79 -7 1 0 103.68 3.79 6 -1 0 1.27 0.30 6 -1 0 1.71 0.30 6 -1 0 1.95 0.42 6 -1 0 1.68 0.43 -6 1 0 1.66 0.35 -6 1 0 1.77 0.25 -6 1 0 1.62 0.22 -6 1 0 1.59 0.33 5 -1 0 208.29 6.96 5 -1 0 217.68 7.21 5 -1 0 190.33 7.20 5 -1 0 210.89 7.06 -5 1 0 217.07 7.11 -5 1 0 222.81 6.87 -5 1 0 204.53 6.81 -5 1 0 210.97 7.10 4 -1 0 51.70 2.06 4 -1 0 54.87 2.12 4 -1 0 51.87 1.99 4 -1 0 54.26 1.93 -4 1 0 54.43 1.80 -4 1 0 51.62 2.00 -4 1 0 50.61 1.77 -4 1 0 52.66 2.00 3 -1 0 257.15 8.22 3 -1 0 221.17 8.20 3 -1 0 259.27 8.11 3 -1 0 254.88 8.18 -3 1 0 253.43 8.18 -3 1 0 245.57 7.94 -3 1 0 256.30 7.95 2 -1 0 891.89 26.79 2 -1 0 767.79 26.81 2 -1 0 783.51 26.82 2 -1 0 923.95 26.84 1 -1 0 24.65 0.89 1 -1 0 27.00 0.97 1 -1 0 27.21 0.95 1 -1 0 25.83 0.92 -1 1 0 26.86 0.86 -1 1 0 25.14 0.86 -1 1 0 24.87 0.91 0 -1 0 430.70 14.02 0 -1 0 472.47 14.02 0 1 0 428.92 14.01 0 1 0 451.81 14.01 0 1 0 414.17 13.99 -1 -1 0 117.79 3.77 -1 -1 0 119.62 3.79 -1 -1 0 108.32 3.77 1 1 0 116.16 3.82 1 1 0 113.63 3.86 -2 -1 0 311.89 9.96 -2 -1 0 313.68 9.94 -2 -1 0 292.46 9.94 2 1 0 316.40 10.12 2 1 0 308.35 10.04 -3 -1 0 199.93 6.46 -3 -1 0 194.48 6.50 -3 -1 0 201.04 6.44 -3 -1 0 206.15 6.45 3 1 0 179.57 6.64 3 1 0 192.99 6.60 -4 -1 0 83.85 2.96 -4 -1 0 87.85 3.01 -4 -1 0 90.45 2.97 -4 -1 0 79.84 2.97 4 1 0 81.11 3.14 4 1 0 79.27 3.21 -5 -1 0 144.56 4.94 -5 -1 0 143.85 4.91 -5 -1 0 150.96 4.89 -5 -1 0 143.26 4.93 5 1 0 144.75 5.16 5 1 0 129.46 5.19 -6 -1 0 5.02 0.53 -6 -1 0 4.36 0.49 -6 -1 0 3.40 0.44 6 1 0 3.21 0.56 6 1 0 3.95 0.66 -7 -1 0 61.07 2.43 -7 -1 0 62.80 2.38 -7 -1 0 58.07 2.40 7 1 0 63.13 2.86 7 1 0 56.47 2.69 -8 -1 0 5.75 0.63 8 1 0 3.14 0.70 8 1 0 5.44 0.88 -9 -1 0 4.75 0.62 9 1 0 4.74 0.87 9 1 0 5.47 0.96 -10 -1 0 5.90 0.72 10 1 0 5.72 0.99 10 1 0 6.44 1.05 -11 -1 0 11.70 0.95 11 1 0 9.05 1.32 11 1 0 10.48 1.40 -12 -1 0 23.11 1.44 12 1 0 23.54 2.00 12 1 0 24.29 2.06 13 -2 0 4.78 1.07 13 -2 0 4.82 1.08 -13 2 0 3.80 0.49 12 -2 0 20.53 1.67 12 -2 0 19.59 1.68 -12 2 0 18.86 1.01 11 -2 0 8.92 1.16 11 -2 0 5.48 0.94 -11 2 0 8.19 0.57 10 -2 0 47.73 2.51 10 -2 0 45.80 2.47 -10 2 0 46.84 1.82 9 -2 0 39.64 2.10 9 -2 0 40.24 2.14 -9 2 0 37.97 1.51 -9 2 0 38.95 1.95 8 -2 0 42.09 2.08 8 -2 0 42.81 1.79 8 -2 0 40.18 1.90 8 -2 0 38.88 2.05 -8 2 0 42.71 1.54 -8 2 0 41.92 1.96 -8 2 0 36.68 1.89 -8 2 0 42.63 1.61 7 -2 0 114.58 4.07 7 -2 0 109.81 4.34 7 -2 0 115.57 4.36 7 -2 0 118.31 4.24 -7 2 0 112.01 3.80 -7 2 0 116.65 3.87 -7 2 0 114.19 4.27 -7 2 0 115.05 4.26 6 -2 0 0.07 0.23 6 -2 0 0.05 0.17 6 -2 0 0.08 0.19 6 -2 0 0.18 0.23 -6 2 0 0.11 0.11 -6 2 0 0.12 0.17 -6 2 0 0.39 0.10 -6 2 0 0.67 0.26 5 -2 0 87.06 3.22 5 -2 0 85.53 3.07 5 -2 0 88.34 3.24 5 -2 0 83.89 3.18 -5 2 0 86.24 2.81 -5 2 0 86.23 3.20 4 -2 0 32.96 1.45 4 -2 0 37.26 1.47 4 -2 0 34.53 1.40 4 -2 0 33.66 1.47 3 -2 0 410.48 13.02 3 -2 0 399.19 13.03 3 -2 0 407.52 13.05 3 -2 0 387.53 13.10 -3 2 0 411.36 13.01 2 -2 0 942.95 30.33 2 -2 0 880.00 30.20 2 -2 0 942.04 30.25 2 -2 0 962.34 30.15 -2 2 0 1000.00 30.09 -2 2 0 910.15 30.05 -2 2 0 949.02 30.10 -2 2 0 978.34 30.09 1 -2 0 3.47 0.34 1 -2 0 3.35 0.33 -1 2 0 3.48 0.27 -1 2 0 3.37 0.25 -1 2 0 3.44 0.28 0 -2 0 522.52 16.70 0 -2 0 523.52 16.66 0 -2 0 514.90 16.69 0 2 0 522.01 16.66 0 2 0 517.48 16.69 0 2 0 524.56 16.67 -1 -2 0 0.26 0.15 -1 -2 0 0.08 0.15 -1 -2 0 0.03 0.14 1 2 0 0.06 0.18 1 2 0 -0.31 0.15 1 2 0 0.19 0.17 -2 -2 0 94.99 3.23 -2 -2 0 91.35 3.24 -2 -2 0 95.01 3.21 2 2 0 93.46 3.30 2 2 0 93.49 3.30 2 2 0 91.69 3.38 -3 -2 0 103.17 3.65 -3 -2 0 111.87 3.66 -3 -2 0 100.47 3.67 3 2 0 105.42 3.80 3 2 0 108.64 3.91 -4 -2 0 23.61 1.05 -4 -2 0 23.43 1.09 -4 -2 0 22.27 1.06 4 2 0 22.51 1.21 4 2 0 23.06 1.31 -5 -2 0 91.88 3.36 -5 -2 0 97.25 3.35 -5 -2 0 94.70 3.33 5 2 0 88.83 3.57 5 2 0 86.30 3.65 -6 -2 0 1.43 0.33 -6 -2 0 1.91 0.35 -6 -2 0 1.45 0.33 6 2 0 2.06 0.47 6 2 0 1.55 0.49 -7 -2 0 50.08 2.11 -7 -2 0 49.11 2.08 -7 -2 0 51.44 2.11 7 2 0 49.43 2.53 7 2 0 47.07 2.40 -8 -2 0 0.64 0.30 8 2 0 0.08 0.39 8 2 0 0.19 0.36 -9 -2 0 28.51 1.53 9 2 0 26.73 1.86 9 2 0 30.12 2.04 -10 -2 0 6.88 0.82 10 2 0 5.62 1.10 10 2 0 8.01 1.22 -11 -2 0 7.95 0.93 11 2 0 5.49 1.09 11 2 0 5.32 1.07 -12 -2 0 5.25 0.84 12 2 0 5.55 1.17 12 2 0 5.40 1.14 13 -3 0 0.00 0.49 13 -3 0 0.04 0.53 -13 3 0 -0.15 0.46 -13 3 0 0.29 0.20 12 -3 0 33.26 2.19 12 -3 0 33.64 2.24 -12 3 0 36.79 1.43 11 -3 0 0.78 0.50 11 -3 0 -0.24 0.41 -11 3 0 0.02 0.15 10 -3 0 27.71 1.75 10 -3 0 29.82 1.78 -10 3 0 26.14 1.62 -10 3 0 26.17 1.09 9 -3 0 31.73 1.70 9 -3 0 31.68 1.78 9 -3 0 30.24 1.77 9 -3 0 30.97 1.54 -9 3 0 31.29 1.24 -9 3 0 32.78 1.76 -9 3 0 32.75 1.76 -9 3 0 30.58 1.18 8 -3 0 20.23 1.11 8 -3 0 20.41 1.27 8 -3 0 20.09 1.28 8 -3 0 19.90 1.22 -8 3 0 19.01 0.76 -8 3 0 19.59 1.25 -8 3 0 18.06 1.22 -8 3 0 19.77 0.82 7 -3 0 79.52 2.90 7 -3 0 72.32 3.02 7 -3 0 77.00 3.03 7 -3 0 76.59 3.02 -7 3 0 71.93 3.02 -7 3 0 75.23 3.05 -7 3 0 74.77 2.51 -7 3 0 73.04 2.47 5 -3 0 344.99 11.48 5 -3 0 342.34 11.53 5 -3 0 363.32 11.64 5 -3 0 347.06 11.50 -5 3 0 349.76 11.48 4 -3 0 239.11 8.24 4 -3 0 232.63 8.39 4 -3 0 252.83 8.32 4 -3 0 248.25 8.29 -4 3 0 255.03 8.02 -4 3 0 266.24 8.02 -4 3 0 256.91 8.27 3 -3 0 168.20 5.70 3 -3 0 175.31 5.47 3 -3 0 163.89 5.53 3 -3 0 160.85 5.59 -3 3 0 165.11 5.52 -3 3 0 167.62 5.51 -3 3 0 159.13 5.40 -3 3 0 167.71 5.39 2 -3 0 27.08 1.24 2 -3 0 26.48 1.20 -2 3 0 29.97 1.10 -2 3 0 29.11 1.14 -2 3 0 30.63 1.12 -2 3 0 28.02 1.11 1 -3 0 6.07 0.49 1 -3 0 6.38 0.48 -1 3 0 5.42 0.38 -1 3 0 6.70 0.42 -1 3 0 6.63 0.45 0 -3 0 55.68 2.01 0 -3 0 55.31 2.06 0 3 0 54.03 2.06 0 3 0 57.22 2.02 0 3 0 51.84 1.99 -1 -3 0 6.76 0.49 -1 -3 0 6.82 0.49 -1 -3 0 6.72 0.50 1 3 0 6.45 0.50 1 3 0 7.13 0.56 1 3 0 6.35 0.51 -2 -3 0 192.92 6.21 -2 -3 0 179.09 6.20 -2 -3 0 180.48 6.18 2 3 0 184.87 6.36 2 3 0 181.82 6.25 2 3 0 187.15 6.29 -3 -3 0 103.67 3.65 -3 -3 0 102.15 3.69 -3 -3 0 100.39 3.65 3 3 0 103.83 3.89 3 3 0 103.56 3.81 3 3 0 106.77 3.79 -4 -3 0 47.94 2.01 -4 -3 0 51.46 2.00 -4 -3 0 48.89 1.96 4 3 0 48.32 2.14 4 3 0 49.55 2.25 -5 -3 0 55.74 2.28 -5 -3 0 57.18 2.35 -5 -3 0 58.65 2.28 5 3 0 60.39 2.67 5 3 0 56.44 2.53 -7 -3 0 23.00 1.30 7 3 0 23.14 1.54 7 3 0 21.92 1.60 -8 -3 0 5.33 0.73 8 3 0 4.11 0.80 8 3 0 5.75 0.98 -9 -3 0 31.77 1.74 9 3 0 32.46 2.19 9 3 0 29.90 2.05 -10 -3 0 9.26 1.02 10 3 0 6.12 1.14 10 3 0 6.12 1.12 -11 -3 0 6.07 0.90 11 3 0 5.55 1.11 11 3 0 4.45 1.03 13 -4 0 0.83 0.62 13 -4 0 0.29 0.55 -13 4 0 0.14 0.49 -13 4 0 1.74 0.67 12 -4 0 28.97 1.93 12 -4 0 28.34 1.95 -12 4 0 27.67 1.86 11 -4 0 1.36 0.54 11 -4 0 1.17 0.54 -11 4 0 1.58 0.55 -11 4 0 1.91 0.80 10 -4 0 37.51 2.01 10 -4 0 35.03 2.03 10 -4 0 36.29 2.03 -10 4 0 38.07 2.08 -10 4 0 39.04 2.01 9 -4 0 30.65 1.71 9 -4 0 28.84 1.52 9 -4 0 31.35 1.70 9 -4 0 27.80 1.66 -9 4 0 28.27 1.70 -9 4 0 30.10 1.73 -9 4 0 28.67 1.61 8 -4 0 15.09 1.01 8 -4 0 15.99 1.07 8 -4 0 16.02 1.14 8 -4 0 14.48 1.07 -8 4 0 15.65 1.13 -8 4 0 16.34 1.05 7 -4 0 45.17 2.11 7 -4 0 45.71 2.00 7 -4 0 43.49 1.94 7 -4 0 47.06 2.05 -7 4 0 45.93 2.13 -7 4 0 44.05 1.97 -7 4 0 42.45 1.51 -7 4 0 44.30 1.52 6 -4 0 11.53 0.89 6 -4 0 13.79 0.85 6 -4 0 11.82 0.83 6 -4 0 11.07 0.75 -6 4 0 12.45 0.80 -6 4 0 12.42 0.51 -6 4 0 11.39 0.77 -6 4 0 11.59 0.50 5 -4 0 215.56 7.25 5 -4 0 218.75 7.12 5 -4 0 212.57 7.38 5 -4 0 213.06 7.20 -5 4 0 216.24 6.90 -5 4 0 213.42 7.19 -5 4 0 215.10 6.91 -5 4 0 198.51 7.15 4 -4 0 12.42 0.73 4 -4 0 13.57 0.81 4 -4 0 14.95 0.90 4 -4 0 12.57 0.65 -4 4 0 14.22 0.75 -4 4 0 13.85 0.63 -4 4 0 12.75 0.72 -4 4 0 13.65 0.61 3 -4 0 48.03 2.02 3 -4 0 49.46 1.97 -3 4 0 49.25 1.82 -3 4 0 49.97 1.78 -3 4 0 49.28 1.84 -3 4 0 45.25 1.78 2 -4 0 179.30 6.02 2 -4 0 172.99 6.08 -2 4 0 184.13 5.89 -2 4 0 173.71 5.91 -2 4 0 175.46 5.89 -2 4 0 173.85 5.85 1 -4 0 79.09 3.05 1 -4 0 82.02 3.03 -1 4 0 76.81 2.97 -1 4 0 83.79 2.90 -1 4 0 89.69 2.95 0 -4 0 89.48 3.28 0 -4 0 86.40 3.28 0 -4 0 95.92 3.23 0 4 0 90.98 3.22 0 4 0 87.20 3.28 0 4 0 90.89 3.21 -1 -4 0 1.55 0.30 -1 -4 0 1.18 0.28 -1 -4 0 1.62 0.32 1 4 0 1.59 0.33 1 4 0 2.01 0.36 1 4 0 1.89 0.35 -2 -4 0 46.47 1.94 -2 -4 0 47.08 1.97 -2 -4 0 50.32 1.98 2 4 0 46.69 1.99 2 4 0 48.31 2.06 2 4 0 50.66 2.11 -3 -4 0 49.04 1.98 -3 -4 0 48.05 1.99 -3 -4 0 47.86 2.02 3 4 0 46.65 2.16 3 4 0 47.89 2.11 3 4 0 49.77 2.13 -4 -4 0 32.51 1.50 -4 -4 0 31.97 1.54 -4 -4 0 31.62 1.46 4 4 0 33.42 1.65 4 4 0 30.46 1.69 -5 -4 0 22.76 1.27 -5 -4 0 23.00 1.22 -5 -4 0 22.79 1.20 5 4 0 22.84 1.39 5 4 0 22.88 1.49 -6 -4 0 21.75 1.27 -6 -4 0 21.05 1.18 6 4 0 18.13 1.36 6 4 0 21.29 1.48 -7 -4 0 87.94 3.69 7 4 0 98.39 4.21 -8 -4 0 0.77 0.40 8 4 0 1.09 0.53 8 4 0 0.04 0.37 -9 -4 0 18.36 1.36 9 4 0 21.65 1.78 9 4 0 20.61 1.70 -10 -4 0 0.45 0.41 10 4 0 0.33 0.44 10 4 0 0.87 0.66 -11 -4 0 4.60 0.85 11 4 0 4.91 1.11 11 4 0 3.10 0.92 13 -5 0 3.40 0.84 -13 5 0 2.25 0.67 12 -5 0 23.60 1.71 -12 5 0 21.03 1.61 11 -5 0 -0.10 0.33 11 -5 0 -0.07 0.37 11 -5 0 -0.10 0.34 -11 5 0 -0.36 0.30 -11 5 0 0.14 0.37 -11 5 0 0.01 0.32 10 -5 0 22.40 1.42 10 -5 0 21.07 1.61 10 -5 0 20.36 1.44 10 -5 0 22.38 1.54 -10 5 0 20.64 1.53 -10 5 0 22.58 1.75 -10 5 0 21.51 1.43 -10 5 0 22.63 1.51 9 -5 0 10.34 0.88 9 -5 0 8.34 1.02 9 -5 0 8.93 0.81 9 -5 0 8.46 0.95 -9 5 0 8.13 0.92 -9 5 0 9.85 1.10 -9 5 0 10.44 1.09 8 -5 0 10.48 1.08 8 -5 0 10.38 0.86 8 -5 0 11.38 0.91 8 -5 0 9.82 0.80 -8 5 0 9.27 0.94 -8 5 0 10.20 0.47 -8 5 0 11.04 0.50 -8 5 0 10.12 0.88 -8 5 0 10.82 1.13 7 -5 0 119.87 4.48 7 -5 0 124.88 4.38 7 -5 0 116.18 4.64 7 -5 0 123.01 4.46 -7 5 0 127.10 4.49 -7 5 0 117.25 4.41 -7 5 0 116.81 4.01 -7 5 0 120.34 4.01 6 -5 0 3.19 0.54 6 -5 0 2.93 0.38 6 -5 0 3.43 0.49 6 -5 0 2.28 0.44 -6 5 0 2.29 0.40 -6 5 0 2.50 0.28 -6 5 0 2.57 0.42 -6 5 0 2.65 0.28 5 -5 0 97.02 3.70 5 -5 0 98.67 3.83 5 -5 0 98.16 3.45 -5 5 0 105.58 3.41 -5 5 0 94.49 3.40 -5 5 0 99.55 3.58 -5 5 0 98.42 3.58 4 -5 0 15.85 1.03 4 -5 0 15.87 0.96 -4 5 0 16.72 0.86 -4 5 0 16.81 0.79 -4 5 0 16.63 0.86 -4 5 0 15.14 0.80 3 -5 0 93.14 3.39 3 -5 0 84.38 3.42 -3 5 0 90.19 3.17 -3 5 0 86.18 3.19 -3 5 0 92.35 3.23 -3 5 0 90.70 3.17 2 -5 0 10.62 0.77 2 -5 0 12.69 0.86 -2 5 0 13.07 0.67 -2 5 0 11.63 0.75 -2 5 0 11.92 0.71 1 -5 0 52.61 2.21 1 -5 0 56.15 2.08 1 -5 0 50.10 2.16 -1 5 0 55.36 2.18 -1 5 0 51.47 2.06 -1 5 0 52.49 2.03 0 -5 0 93.76 3.38 0 -5 0 90.41 3.47 0 -5 0 94.22 3.45 0 5 0 96.96 3.40 0 5 0 91.25 3.38 0 5 0 88.93 3.45 -1 -5 0 3.61 0.49 -1 -5 0 3.44 0.49 -1 -5 0 3.24 0.47 1 5 0 3.47 0.48 1 5 0 4.96 0.59 1 5 0 3.81 0.56 -2 -5 0 140.18 4.98 -2 -5 0 140.46 4.98 -2 -5 0 137.75 4.97 2 5 0 141.02 5.11 2 5 0 138.23 5.01 2 5 0 139.45 5.11 -3 -5 0 8.60 0.71 -3 -5 0 7.63 0.66 -3 -5 0 9.06 0.85 3 5 0 9.52 0.92 3 5 0 8.06 0.88 3 5 0 10.30 0.83 -4 -5 0 29.38 1.46 -4 -5 0 29.06 1.43 -4 -5 0 26.99 1.48 4 5 0 28.89 1.59 4 5 0 27.88 1.66 -5 -5 0 29.21 1.44 -5 -5 0 28.33 1.46 -5 -5 0 26.39 1.50 5 5 0 27.17 1.71 5 5 0 26.76 1.63 -6 -5 0 15.58 1.04 -6 -5 0 13.86 1.11 6 5 0 15.36 1.29 6 5 0 14.48 1.25 -7 -5 0 44.52 2.21 7 5 0 41.46 2.39 7 5 0 43.67 2.53 -8 -5 0 -0.19 0.30 8 5 0 0.22 0.51 8 5 0 0.76 0.50 -9 -5 0 8.93 1.07 9 5 0 8.78 1.35 9 5 0 5.93 1.07 -10 -5 0 5.21 0.93 10 5 0 5.04 1.13 10 5 0 6.17 1.20 13 -6 0 0.78 0.61 -13 6 0 1.71 0.66 12 -6 0 26.01 1.83 12 -6 0 24.47 1.83 -12 6 0 26.37 2.86 -12 6 0 24.81 1.72 11 -6 0 0.27 0.44 11 -6 0 -0.06 0.39 -11 6 0 0.30 0.38 -11 6 0 0.44 0.47 10 -6 0 36.12 2.09 10 -6 0 34.61 1.88 10 -6 0 34.72 1.94 -10 6 0 35.77 1.91 -10 6 0 33.55 2.06 9 -6 0 32.28 1.73 9 -6 0 28.98 1.82 9 -6 0 30.53 1.69 -9 6 0 30.19 1.68 -9 6 0 31.11 1.18 -9 6 0 34.38 1.96 -9 6 0 29.61 1.17 8 -6 0 9.07 0.78 8 -6 0 8.80 1.06 8 -6 0 9.15 0.92 8 -6 0 7.92 0.90 -8 6 0 9.22 0.53 -8 6 0 9.70 0.53 -8 6 0 11.36 1.18 -8 6 0 8.45 1.04 -8 6 0 8.14 0.85 7 -6 0 29.98 1.70 7 -6 0 26.53 1.50 7 -6 0 26.71 1.29 7 -6 0 28.10 1.43 -7 6 0 27.94 1.15 -7 6 0 27.42 1.17 -7 6 0 28.88 1.47 -7 6 0 26.34 1.40 6 -6 0 11.19 0.97 -6 6 0 10.22 0.61 -6 6 0 11.26 0.66 -6 6 0 9.68 0.73 5 -6 0 67.97 2.87 5 -6 0 62.23 2.70 -5 6 0 67.11 2.53 -5 6 0 61.92 2.53 -5 6 0 66.14 2.43 -5 6 0 65.81 2.47 4 -6 0 4.42 0.62 4 -6 0 4.16 0.63 -4 6 0 3.83 0.47 -4 6 0 4.25 0.47 -4 6 0 3.89 0.45 -4 6 0 4.15 0.49 3 -6 0 72.85 2.88 3 -6 0 71.98 2.96 -3 6 0 74.34 2.63 -3 6 0 69.48 2.68 -3 6 0 71.24 2.80 -3 6 0 66.63 2.73 2 -6 0 110.50 4.18 2 -6 0 110.41 4.10 -2 6 0 105.68 4.02 -2 6 0 105.65 3.92 -2 6 0 115.03 3.86 1 -6 0 47.86 2.22 1 -6 0 54.83 2.11 1 -6 0 49.65 2.21 -1 6 0 49.41 2.18 -1 6 0 49.69 2.02 -1 6 0 53.69 2.10 0 -6 0 80.42 3.16 0 -6 0 81.53 3.09 0 -6 0 82.68 3.20 0 6 0 82.07 3.21 0 6 0 77.20 3.06 0 6 0 79.86 3.06 -1 -6 0 0.46 0.27 -1 -6 0 0.31 0.24 -1 -6 0 0.30 0.27 1 6 0 0.23 0.21 1 6 0 0.37 0.26 1 6 0 0.12 0.28 -2 -6 0 38.95 1.80 -2 -6 0 34.82 1.76 -2 -6 0 37.97 1.81 2 6 0 36.78 1.86 2 6 0 39.56 1.83 2 6 0 39.49 1.95 -3 -6 0 2.08 0.43 -3 -6 0 3.08 0.52 -3 -6 0 2.67 0.52 3 6 0 1.73 0.48 3 6 0 2.65 0.55 -4 -6 0 50.00 2.27 -4 -6 0 51.95 2.26 -4 -6 0 53.17 2.36 4 6 0 48.94 2.49 4 6 0 48.90 2.41 -5 -6 0 52.68 2.37 -5 -6 0 54.37 2.50 5 6 0 49.22 2.63 5 6 0 52.77 2.57 -6 -6 0 9.89 1.10 6 6 0 9.22 1.22 6 6 0 10.05 1.26 -7 -6 0 16.89 1.33 7 6 0 21.33 1.63 7 6 0 17.51 1.57 -8 -6 0 2.36 0.64 8 6 0 0.73 0.61 8 6 0 1.31 0.59 -9 -6 0 11.25 1.32 9 6 0 13.95 1.76 9 6 0 10.82 1.54 -10 -6 0 -0.21 0.43 10 6 0 0.23 0.52 10 6 0 -0.42 0.43 12 -7 0 15.67 1.67 -12 7 0 14.13 1.67 11 -7 0 0.96 0.59 11 -7 0 2.25 0.61 -11 7 0 0.74 0.46 -11 7 0 1.96 0.68 10 -7 0 26.41 1.79 10 -7 0 24.77 1.52 10 -7 0 22.76 1.53 -10 7 0 22.56 1.73 -10 7 0 22.63 0.97 -10 7 0 22.52 1.48 9 -7 0 21.09 1.59 9 -7 0 20.14 1.39 -9 7 0 20.81 1.31 -9 7 0 22.32 1.60 -9 7 0 20.35 0.98 8 -7 0 18.77 1.44 8 -7 0 18.42 1.30 -8 7 0 19.69 0.98 -8 7 0 19.27 1.21 7 -7 0 52.25 2.40 7 -7 0 47.85 2.49 -7 7 0 53.39 2.04 -7 7 0 46.80 2.18 6 -7 0 3.22 0.61 6 -7 0 2.93 0.65 -6 7 0 2.99 0.44 -6 7 0 3.61 0.53 5 -7 0 65.07 3.00 5 -7 0 72.23 2.94 -5 7 0 66.53 2.67 -5 7 0 67.97 2.69 4 -7 0 3.10 0.59 4 -7 0 3.04 0.55 -4 7 0 2.73 0.44 -4 7 0 3.82 0.56 3 -7 0 59.60 2.64 3 -7 0 57.32 2.52 -3 7 0 53.83 2.31 -3 7 0 59.49 2.45 -3 7 0 58.24 2.21 2 -7 0 29.13 1.52 2 -7 0 25.34 1.51 -2 7 0 25.80 1.33 -2 7 0 25.97 1.44 -2 7 0 28.15 1.26 1 -7 0 6.19 0.81 1 -7 0 7.23 0.83 -1 7 0 8.20 0.87 -1 7 0 7.56 0.75 -1 7 0 6.80 0.60 0 -7 0 98.42 3.91 0 -7 0 99.46 3.93 0 7 0 102.52 3.78 0 7 0 100.42 3.81 0 7 0 99.68 3.97 -1 -7 0 0.11 0.26 -1 -7 0 0.16 0.24 -1 -7 0 -0.30 0.23 1 7 0 -0.07 0.28 1 7 0 -0.17 0.23 1 7 0 0.00 0.25 -2 -7 0 77.95 3.21 -2 -7 0 76.82 3.19 -2 -7 0 79.13 3.20 2 7 0 74.08 3.22 2 7 0 74.46 3.34 2 7 0 79.95 3.22 -3 -7 0 7.06 0.86 -3 -7 0 8.24 0.93 -3 -7 0 6.99 0.81 3 7 0 6.41 0.88 3 7 0 6.19 0.85 -4 -7 0 36.79 1.94 -4 -7 0 41.56 2.09 4 7 0 38.81 2.11 4 7 0 37.15 2.14 -5 -7 0 12.85 1.29 -5 -7 0 8.63 1.02 5 7 0 9.68 1.21 5 7 0 9.16 1.15 -6 -7 0 0.93 0.52 6 7 0 1.03 0.54 6 7 0 3.08 0.78 -7 -7 0 6.27 0.96 7 7 0 5.80 1.05 7 7 0 5.90 1.14 -8 -7 0 0.04 0.43 8 7 0 0.17 0.47 8 7 0 0.13 0.48 -9 -7 0 10.24 1.33 9 7 0 11.61 1.63 9 7 0 10.70 1.60 12 -8 0 24.01 1.94 -12 8 0 22.69 1.95 11 -8 0 8.27 1.23 -11 8 0 8.92 1.32 10 -8 0 28.89 1.99 10 -8 0 25.46 1.72 -10 8 0 27.10 1.24 -10 8 0 29.20 1.99 9 -8 0 5.86 0.91 9 -8 0 3.83 0.85 -9 8 0 4.34 0.74 -9 8 0 3.83 0.88 -9 8 0 4.16 0.51 8 -8 0 19.95 1.52 8 -8 0 17.54 1.32 -8 8 0 17.76 1.18 -8 8 0 17.03 1.02 7 -8 0 33.21 1.91 7 -8 0 35.19 2.06 -7 8 0 35.69 1.73 -7 8 0 33.07 1.61 6 -8 0 6.78 0.90 -6 8 0 6.90 0.75 -6 8 0 9.28 0.77 5 -8 0 59.76 2.88 5 -8 0 60.65 2.76 -5 8 0 61.30 2.53 -5 8 0 61.19 2.58 4 -8 0 8.18 0.99 4 -8 0 7.83 0.93 -4 8 0 7.44 0.85 -4 8 0 7.28 0.76 3 -8 0 29.91 1.78 3 -8 0 33.14 1.76 -3 8 0 31.33 1.67 -3 8 0 30.49 1.54 2 -8 0 54.76 2.58 2 -8 0 65.34 2.78 -2 8 0 56.06 2.59 -2 8 0 56.42 2.44 1 -8 0 17.65 1.26 1 -8 0 18.99 1.25 -1 8 0 17.73 1.29 -1 8 0 17.49 1.12 0 -8 0 25.69 1.57 0 -8 0 24.45 1.50 0 8 0 25.62 1.63 0 8 0 25.64 1.44 0 8 0 26.26 1.41 -1 -8 0 0.31 0.31 -1 -8 0 1.12 0.42 1 8 0 0.88 0.45 1 8 0 0.97 0.41 1 8 0 1.04 0.41 -2 -8 0 61.32 2.81 -2 -8 0 67.28 2.87 2 8 0 62.25 2.82 2 8 0 62.11 2.86 -3 -8 0 0.69 0.39 -3 -8 0 1.17 0.41 3 8 0 0.79 0.42 3 8 0 1.78 0.55 -4 -8 0 19.27 1.36 4 8 0 21.83 1.54 4 8 0 19.06 1.48 5 8 0 11.05 1.32 5 8 0 10.84 1.35 6 8 0 2.55 0.78 6 8 0 2.68 0.79 7 8 0 4.98 1.05 7 8 0 5.18 0.99 8 8 0 -0.05 0.53 8 8 0 0.87 0.70 11 -9 0 0.75 0.52 11 -9 0 -0.26 0.57 -11 9 0 0.86 0.26 -11 9 0 0.55 0.60 10 -9 0 18.65 1.93 10 -9 0 19.93 1.53 -10 9 0 21.05 1.72 -10 9 0 16.85 1.04 9 -9 0 12.20 1.32 9 -9 0 12.30 1.52 -9 9 0 11.94 0.89 8 -9 0 21.44 1.65 8 -9 0 16.24 1.39 -8 9 0 20.90 1.22 7 -9 0 56.33 2.95 7 -9 0 55.24 2.78 -7 9 0 59.88 2.52 6 -9 0 2.99 0.70 6 -9 0 3.06 0.65 -6 9 0 4.23 0.63 5 -9 0 29.08 1.76 5 -9 0 27.47 1.84 -5 9 0 29.18 1.63 -5 9 0 28.60 1.53 4 -9 0 0.79 0.42 4 -9 0 1.63 0.54 -4 9 0 1.37 0.47 -4 9 0 1.26 0.41 3 -9 0 32.27 1.84 3 -9 0 31.90 1.92 -3 9 0 31.63 1.65 -3 9 0 30.45 1.77 2 -9 0 10.82 1.16 2 -9 0 10.37 1.18 -2 9 0 11.45 1.21 -2 9 0 12.27 0.95 1 -9 0 0.47 0.40 1 -9 0 0.10 0.33 -1 9 0 0.35 0.33 -1 9 0 0.34 0.41 0 -9 0 68.47 3.08 0 -9 0 64.42 2.98 0 9 0 62.96 3.10 0 9 0 66.68 2.91 -1 -9 0 1.82 0.53 -1 -9 0 1.10 0.45 1 9 0 2.01 0.53 -2 -9 0 45.72 2.35 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_olex2_submission_special_instructions 'No special instructions were received'