data_ds6y2_0m _audit_creation_date 2016-09-07 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _shelxl_version_number 2013-4 _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. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H16 N2 O5 Pd, H2 O' _chemical_formula_sum 'C15 H18 N2 O6 Pd' _chemical_formula_weight 428.71 _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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.425(5) _cell_length_b 6.913(2) _cell_length_c 15.918(5) _cell_angle_alpha 90 _cell_angle_beta 102.100(6) _cell_angle_gamma 90 _cell_volume 1552.1(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2826 _cell_measurement_temperature 293 _cell_measurement_theta_max 23.490 _cell_measurement_theta_min 2.889 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.8 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour 'clear yellowish' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.012 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_unetI/netI 0.0875 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.939 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 23580 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.939 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.143 _diffrn_reflns_theta_min 1.733 _diffrn_ambient_temperature 293.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.939 _diffrn_measurement_device_type 'SMART APEX2' _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2645 _reflns_number_total 5123 _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 ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.685 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.119 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 5123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0548 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1338 _refine_ls_wR_factor_ref 0.1746 _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, All O(H,H) groups 2.a Free rotating group: O6(H6A,H6B) 2.b Aromatic/amide H refined with riding coordinates: C12(H12) 2.c Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _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 0.88565(3) 0.29173(6) 0.11524(3) 0.04089(16) Uani 1 1 d . . . . . N1 N 0.7557(3) 0.2746(6) 0.0463(3) 0.0395(9) Uani 1 1 d . . . . . O5 O 0.5766(3) 0.3063(6) 0.2714(3) 0.0519(10) Uani 1 1 d . . . . . C5 C 0.6756(3) 0.2828(7) 0.1651(3) 0.0374(10) Uani 1 1 d . . . . . C7 C 0.6538(4) 0.2862(7) 0.3380(4) 0.0417(11) Uani 1 1 d . . . . . C8 C 0.7447(4) 0.2754(7) 0.3207(3) 0.0373(11) Uani 1 1 d . . . . . C3 C 0.6773(4) 0.2648(7) 0.0725(3) 0.0378(11) Uani 1 1 d . . . . . C13 C 0.6371(5) 0.2770(8) 0.4201(4) 0.0480(13) Uani 1 1 d . . . . . C9 C 0.7560(3) 0.2748(7) 0.2319(3) 0.0356(10) Uani 1 1 d . . . . . C4 C 0.5872(4) 0.2317(9) 0.0064(4) 0.0514(14) Uani 1 1 d . . . . . H4A H 0.5620 0.3538 -0.0164 0.077 Uiso 1 1 calc GR . . . . H4B H 0.5416 0.1676 0.0329 0.077 Uiso 1 1 calc GR . . . . H4C H 0.6006 0.1527 -0.0392 0.077 Uiso 1 1 calc GR . . . . C1 C 0.8564(5) 0.3130(8) -0.0617(4) 0.0532(15) Uani 1 1 d . . . . . C6 C 0.5837(4) 0.3178(8) 0.1864(4) 0.0476(13) Uani 1 1 d . . . . . C2 C 0.7576(5) 0.2668(9) -0.0454(4) 0.0471(13) Uani 1 1 d . . . . . C11 C 0.8056(4) 0.2550(8) 0.4733(4) 0.0462(13) Uani 1 1 d . . . . . C12 C 0.7156(5) 0.2619(8) 0.4884(4) 0.0497(14) Uani 1 1 d . . . . . H12 H 0.7065 0.2566 0.5445 0.060 Uiso 1 1 calc R . . . . C10 C 0.8210(4) 0.2620(8) 0.3916(4) 0.0442(13) Uani 1 1 d . . . . . O4 O 0.5106(3) 0.3660(8) 0.1385(3) 0.0707(12) Uani 1 1 d . . . . . O2 O 0.9251(3) 0.3154(6) 0.0031(3) 0.0585(11) Uani 1 1 d . . . . . O3 O 0.8441(2) 0.2667(6) 0.2247(2) 0.0450(9) Uani 1 1 d . . . . . O1 O 0.8651(4) 0.3429(8) -0.1357(3) 0.0756(14) Uani 1 1 d . . . . . N2 N 1.0256(4) 0.3132(9) 0.1764(4) 0.0588(14) Uani 1 1 d . . . . . C14 C 1.0461(5) 0.3399(14) 0.2684(5) 0.091(3) Uani 1 1 d . . . . . H14A H 1.0038 0.4349 0.2833 0.136 Uiso 1 1 calc GR . . . . H14B H 1.1104 0.3829 0.2871 0.136 Uiso 1 1 calc GR . . . . H14C H 1.0377 0.2194 0.2959 0.136 Uiso 1 1 calc GR . . . . C15 C 1.0802(6) 0.1373(14) 0.1574(6) 0.100(3) Uani 1 1 d . . . . . H15A H 1.0565 0.0243 0.1811 0.150 Uiso 1 1 calc GR . . . . H15B H 1.1462 0.1536 0.1828 0.150 Uiso 1 1 calc GR . . . . H15C H 1.0724 0.1223 0.0964 0.150 Uiso 1 1 calc GR . . . . O6 O 0.8273(7) 0.2396(18) -0.3125(6) 0.169(4) Uani 1 1 d . . . . . H6A H 0.8291 0.2158 -0.2598 0.253 Uiso 1 1 d G . . . . H6B H 0.8776 0.1980 -0.3261 0.253 Uiso 1 1 d G . . . . H11 H 0.869(4) 0.249(6) 0.526(3) 0.027(12) Uiso 1 1 d . . . . . H13 H 0.571(5) 0.286(8) 0.429(4) 0.062(19) Uiso 1 1 d . . . . . H10 H 0.873(4) 0.252(7) 0.379(4) 0.036(15) Uiso 1 1 d . . . . . H2A H 0.734(4) 0.146(8) -0.067(3) 0.042(14) Uiso 1 1 d . . . . . H2 H 1.046(4) 0.408(8) 0.151(3) 0.043(16) Uiso 1 1 d . . . . . H2B H 0.714(4) 0.349(8) -0.067(3) 0.043(16) Uiso 1 1 d . . . . . 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 0.0342(2) 0.0505(3) 0.0414(2) 0.00362(18) 0.01562(16) 0.00023(17) N1 0.046(2) 0.038(2) 0.036(2) 0.0059(18) 0.0110(19) -0.0014(18) O5 0.033(2) 0.071(3) 0.055(2) 0.0015(19) 0.0195(17) 0.0000(17) C5 0.033(2) 0.040(2) 0.042(3) 0.006(2) 0.014(2) 0.000(2) C7 0.038(3) 0.042(3) 0.048(3) 0.001(2) 0.015(2) -0.001(2) C8 0.036(3) 0.036(2) 0.042(3) 0.005(2) 0.014(2) -0.001(2) C3 0.038(3) 0.034(2) 0.040(3) 0.003(2) 0.006(2) 0.0018(19) C13 0.049(3) 0.052(3) 0.051(3) 0.003(3) 0.026(3) -0.002(3) C9 0.032(2) 0.033(2) 0.043(3) 0.002(2) 0.012(2) 0.0018(19) C4 0.042(3) 0.066(4) 0.045(3) -0.003(3) 0.008(2) 0.000(3) C1 0.067(4) 0.058(4) 0.042(3) 0.004(3) 0.027(3) 0.004(3) C6 0.035(3) 0.063(4) 0.047(3) 0.003(3) 0.015(2) -0.001(2) C2 0.053(3) 0.046(3) 0.044(3) 0.001(3) 0.016(3) 0.002(3) C11 0.050(3) 0.048(3) 0.041(3) -0.001(2) 0.011(3) 0.000(2) C12 0.064(4) 0.047(3) 0.043(3) -0.002(2) 0.021(3) 0.001(3) C10 0.039(3) 0.044(3) 0.052(3) 0.002(2) 0.016(3) -0.001(2) O4 0.038(2) 0.116(4) 0.059(3) 0.007(3) 0.0124(19) 0.017(2) O2 0.050(2) 0.083(3) 0.049(2) 0.003(2) 0.0251(19) -0.005(2) O3 0.0263(17) 0.069(2) 0.042(2) 0.0049(17) 0.0132(15) 0.0002(15) O1 0.083(3) 0.107(4) 0.045(2) 0.006(2) 0.033(2) -0.007(3) N2 0.037(3) 0.087(4) 0.054(3) 0.018(3) 0.011(2) -0.002(3) C14 0.054(4) 0.147(8) 0.070(5) 0.002(5) 0.010(4) -0.004(4) C15 0.063(5) 0.125(7) 0.120(7) 0.003(6) 0.037(5) 0.018(5) O6 0.119(7) 0.293(12) 0.090(6) -0.017(6) 0.012(5) 0.010(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 1.968(5) . ? Pd1 O2 1.990(4) . ? Pd1 O3 1.966(4) . ? Pd1 N2 2.055(5) . ? N1 C3 1.287(7) . ? N1 C2 1.467(7) . ? O5 C7 1.374(7) . ? O5 C6 1.380(7) . ? C5 C3 1.485(8) . ? C5 C9 1.400(7) . ? C5 C6 1.455(7) . ? C7 C8 1.397(7) . ? C7 C13 1.379(8) . ? C8 C9 1.457(7) . ? C8 C10 1.405(8) . ? C3 C4 1.508(7) . ? C13 C12 1.399(9) . ? C13 H13 0.99(7) . ? C9 O3 1.301(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C1 C2 1.534(9) . ? C1 O2 1.272(8) . ? C1 O1 1.229(7) . ? C6 O4 1.212(7) . ? C2 H2A 0.94(5) . ? C2 H2B 0.86(5) . ? C11 C12 1.369(9) . ? C11 C10 1.366(8) . ? C11 H11 1.10(5) . ? C12 H12 0.9300 . ? C10 H10 0.82(6) . ? N2 C14 1.444(9) . ? N2 C15 1.513(10) . ? N2 H2 0.86(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O6 H6A 0.8500 . ? O6 H6B 0.8501 . ? 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 O2 85.57(18) . . ? N1 Pd1 N2 174.49(19) . . ? O2 Pd1 N2 88.9(2) . . ? O3 Pd1 N1 93.31(17) . . ? O3 Pd1 O2 178.85(15) . . ? O3 Pd1 N2 92.20(19) . . ? C3 N1 Pd1 128.4(4) . . ? C3 N1 C2 121.5(5) . . ? C2 N1 Pd1 110.0(4) . . ? C7 O5 C6 123.2(4) . . ? C9 C5 C3 124.5(5) . . ? C9 C5 C6 118.7(5) . . ? C6 C5 C3 116.8(5) . . ? O5 C7 C8 119.7(5) . . ? O5 C7 C13 117.5(5) . . ? C13 C7 C8 122.8(5) . . ? C7 C8 C9 119.5(5) . . ? C7 C8 C10 117.1(5) . . ? C10 C8 C9 123.4(5) . . ? N1 C3 C5 121.1(5) . . ? N1 C3 C4 117.9(5) . . ? C5 C3 C4 120.9(5) . . ? C7 C13 C12 117.8(5) . . ? C7 C13 H13 120(4) . . ? C12 C13 H13 122(4) . . ? C5 C9 C8 119.5(4) . . ? O3 C9 C5 127.2(5) . . ? O3 C9 C8 113.3(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C1 C2 117.4(5) . . ? O1 C1 C2 118.7(6) . . ? O1 C1 O2 123.9(6) . . ? O5 C6 C5 118.5(5) . . ? O4 C6 O5 113.5(5) . . ? O4 C6 C5 127.9(5) . . ? N1 C2 C1 111.9(5) . . ? N1 C2 H2A 108(3) . . ? N1 C2 H2B 102(4) . . ? C1 C2 H2A 113(3) . . ? C1 C2 H2B 115(4) . . ? H2A C2 H2B 105(5) . . ? C12 C11 H11 122(3) . . ? C10 C11 C12 121.0(6) . . ? C10 C11 H11 117(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12 119.7 . . ? C8 C10 H10 114(4) . . ? C11 C10 C8 120.7(6) . . ? C11 C10 H10 125(4) . . ? C1 O2 Pd1 113.9(4) . . ? C9 O3 Pd1 124.0(3) . . ? Pd1 N2 H2 103(3) . . ? C14 N2 Pd1 117.5(4) . . ? C14 N2 C15 107.5(6) . . ? C14 N2 H2 112(4) . . ? C15 N2 Pd1 110.4(5) . . ? C15 N2 H2 106(4) . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H6A O6 H6B 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 C3 C5 5.5(7) . . . . ? Pd1 N1 C3 C4 -173.7(3) . . . . ? Pd1 N1 C2 C1 -10.9(6) . . . . ? O5 C7 C8 C9 -3.4(7) . . . . ? O5 C7 C8 C10 177.8(5) . . . . ? O5 C7 C13 C12 -178.3(5) . . . . ? C5 C9 O3 Pd1 6.8(7) . . . . ? C7 O5 C6 C5 8.0(7) . . . . ? C7 O5 C6 O4 -168.8(5) . . . . ? C7 C8 C9 C5 -0.7(7) . . . . ? C7 C8 C9 O3 179.2(5) . . . . ? C7 C8 C10 C11 1.6(8) . . . . ? C7 C13 C12 C11 -0.5(8) . . . . ? C8 C7 C13 C12 1.9(8) . . . . ? C8 C9 O3 Pd1 -173.1(3) . . . . ? C3 N1 C2 C1 171.0(5) . . . . ? C3 C5 C9 C8 -174.0(5) . . . . ? C3 C5 C9 O3 6.0(8) . . . . ? C3 C5 C6 O5 170.3(4) . . . . ? C3 C5 C6 O4 -13.4(9) . . . . ? C13 C7 C8 C9 176.4(5) . . . . ? C13 C7 C8 C10 -2.4(8) . . . . ? C9 C5 C3 N1 -12.6(7) . . . . ? C9 C5 C3 C4 166.6(5) . . . . ? C9 C5 C6 O5 -11.8(7) . . . . ? C9 C5 C6 O4 164.5(6) . . . . ? C9 C8 C10 C11 -177.2(5) . . . . ? C6 O5 C7 C8 -0.4(7) . . . . ? C6 O5 C7 C13 179.8(5) . . . . ? C6 C5 C3 N1 165.2(5) . . . . ? C6 C5 C3 C4 -15.6(7) . . . . ? C6 C5 C9 C8 8.2(7) . . . . ? C6 C5 C9 O3 -171.7(5) . . . . ? C2 N1 C3 C5 -176.9(4) . . . . ? C2 N1 C3 C4 3.9(7) . . . . ? C2 C1 O2 Pd1 -7.6(6) . . . . ? C12 C11 C10 C8 -0.4(8) . . . . ? C10 C8 C9 C5 178.0(5) . . . . ? C10 C8 C9 O3 -2.0(7) . . . . ? C10 C11 C12 C13 -0.2(9) . . . . ? O2 C1 C2 N1 12.6(7) . . . . ? O1 C1 C2 N1 -168.2(5) . . . . ? O1 C1 O2 Pd1 173.3(5) . . . . ? _shelx_res_file ; TITL ds6y2_0m in P21/n #14 REM reset to P21/n #14 CELL 0.71073 14.4247 6.9133 15.918 90 102.1 90 ZERR 4 0.0049 0.0024 0.0053 0 0.006 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Pd UNIT 60 72 8 24 4 L.S. 40 PLAN 5 TEMP 20 BOND fmap 2 53 acta MORE -1 BOND $H CONF REM REM REM WGHT 0.100000 FVAR 0.20501 PD1 5 0.885653 0.291728 0.115241 11.00000 0.03420 0.05049 = 0.04137 0.00362 0.01562 0.00023 N1 3 0.755666 0.274627 0.046258 11.00000 0.04590 0.03757 = 0.03622 0.00587 0.01101 -0.00139 O5 4 0.576626 0.306263 0.271406 11.00000 0.03326 0.07145 = 0.05538 0.00146 0.01951 -0.00004 C5 1 0.675579 0.282812 0.165142 11.00000 0.03317 0.04019 = 0.04153 0.00560 0.01376 0.00009 C7 1 0.653810 0.286203 0.338011 11.00000 0.03805 0.04193 = 0.04792 0.00119 0.01539 -0.00051 C8 1 0.744675 0.275395 0.320728 11.00000 0.03608 0.03628 = 0.04201 0.00537 0.01384 -0.00131 C3 1 0.677298 0.264794 0.072531 11.00000 0.03829 0.03392 = 0.04036 0.00315 0.00620 0.00181 C13 1 0.637108 0.277034 0.420077 11.00000 0.04870 0.05174 = 0.05062 0.00290 0.02625 -0.00162 C9 1 0.755971 0.274820 0.231894 11.00000 0.03224 0.03283 = 0.04339 0.00221 0.01192 0.00182 C4 1 0.587201 0.231713 0.006450 11.00000 0.04236 0.06557 = 0.04549 -0.00327 0.00778 -0.00028 AFIX 137 H4A 2 0.562043 0.353814 -0.016445 11.00000 -1.50000 H4B 2 0.541634 0.167596 0.032889 11.00000 -1.50000 H4C 2 0.600578 0.152671 -0.039158 11.00000 -1.50000 AFIX 0 C1 1 0.856441 0.312959 -0.061652 11.00000 0.06700 0.05761 = 0.04175 0.00353 0.02714 0.00431 C6 1 0.583747 0.317819 0.186432 11.00000 0.03520 0.06313 = 0.04709 0.00257 0.01479 -0.00062 C2 1 0.757643 0.266827 -0.045447 11.00000 0.05291 0.04647 = 0.04439 0.00059 0.01594 0.00211 C11 1 0.805553 0.254959 0.473346 11.00000 0.05034 0.04795 = 0.04087 -0.00142 0.01069 -0.00006 C12 1 0.715579 0.261932 0.488357 11.00000 0.06388 0.04661 = 0.04314 -0.00225 0.02134 0.00084 AFIX 43 H12 2 0.706525 0.256581 0.544462 11.00000 -1.20000 AFIX 0 C10 1 0.821012 0.261983 0.391625 11.00000 0.03933 0.04391 = 0.05235 0.00163 0.01641 -0.00084 O4 4 0.510615 0.366024 0.138501 11.00000 0.03758 0.11630 = 0.05926 0.00689 0.01242 0.01673 O2 4 0.925114 0.315425 0.003140 11.00000 0.04979 0.08344 = 0.04883 0.00321 0.02515 -0.00501 O3 4 0.844128 0.266689 0.224741 11.00000 0.02631 0.06910 = 0.04210 0.00489 0.01321 0.00016 O1 4 0.865057 0.342934 -0.135719 11.00000 0.08283 0.10747 = 0.04523 0.00626 0.03305 -0.00679 N2 3 1.025637 0.313217 0.176362 11.00000 0.03710 0.08656 = 0.05351 0.01831 0.01096 -0.00244 C14 1 1.046110 0.339862 0.268388 11.00000 0.05379 0.14663 = 0.06993 0.00222 0.00963 -0.00430 AFIX 137 H14A 2 1.003823 0.434938 0.283339 11.00000 -1.50000 H14B 2 1.110400 0.382926 0.287114 11.00000 -1.50000 H14C 2 1.037716 0.219435 0.295885 11.00000 -1.50000 AFIX 0 C15 1 1.080168 0.137276 0.157411 11.00000 0.06332 0.12471 = 0.11964 0.00268 0.03747 0.01783 AFIX 137 H15A 2 1.056533 0.024343 0.181080 11.00000 -1.50000 H15B 2 1.146201 0.153587 0.182752 11.00000 -1.50000 H15C 2 1.072376 0.122252 0.096374 11.00000 -1.50000 AFIX 6 O6 4 0.827257 0.239566 -0.312523 11.00000 0.11912 0.29349 = 0.08974 -0.01691 0.01226 0.01002 H6A 2 0.829108 0.215805 -0.259803 11.00000 -1.50000 H6B 2 0.877617 0.197970 -0.326084 11.00000 -1.50000 AFIX 0 H11 2 0.868643 0.248738 0.525857 11.00000 0.02691 H13 2 0.571192 0.286059 0.429215 11.00000 0.06239 H10 2 0.872669 0.251902 0.378670 11.00000 0.03625 H2A 2 0.734269 0.145592 -0.067084 11.00000 0.04200 H2 2 1.045975 0.408083 0.150687 11.00000 0.04296 H2B 2 0.714457 0.348714 -0.067221 11.00000 0.04303 HKLF 4 REM ds6y2_0m in P21/n #14 REM R1 = 0.0548 for 2645 Fo > 4sig(Fo) and 0.1347 for all 5123 data REM 247 parameters refined using 0 restraints END WGHT 0.0674 0.0000 REM Highest difference peak 0.685, deepest hole -0.774, 1-sigma level 0.119 Q1 1 0.9143 0.2810 0.1639 11.00000 0.05 0.69 Q2 1 0.8326 0.3764 0.0582 11.00000 0.05 0.60 Q3 1 0.8023 0.2050 0.0979 11.00000 0.05 0.59 Q4 1 1.1784 0.1045 0.2081 11.00000 0.05 0.58 Q5 1 0.7230 0.2913 0.0526 11.00000 0.05 0.53 ; _shelx_res_checksum 92052 _shelx_hkl_file ; 1 0 0 -0.0958 0.1628 3 -1 0 0 -0.3163 0.1329 6 1 0 0 -0.3916 0.1330 2 -1 0 0 0.14168 0.16194 4 -2 0 0 93.9308 3.2208 4 2 0 0 96.6036 3.1171 2 2 0 0 95.4432 3.8135 3 -2 0 0 92.0163 3.4695 6 -3 0 0 0.97456 0.91241 6 3 0 0 1.21503 0.99171 3 -3 0 0 0.58438 0.74344 4 3 0 0 0.48849 0.68813 2 4 0 0 1096.50 31.52 3 4 0 0 1093.52 27.35 2 -4 0 0 1056.42 28.30 4 -4 0 0 999.902 29.152 6 5 0 0 -0.3977 1.7254 3 -5 0 0 -1.2947 0.9874 4 5 0 0 0.52411 0.95919 2 -5 0 0 0.17575 1.17661 6 6 0 0 99.2162 4.5816 2 -6 0 0 107.335 5.507 6 6 0 0 106.301 6.489 3 -6 0 0 110.379 4.841 4 -7 0 0 1.23781 1.55302 6 -7 0 0 -0.1784 1.3001 4 7 0 0 -0.9246 1.0881 2 7 0 0 -0.3733 1.8095 3 8 0 0 271.280 9.710 2 -8 0 0 279.234 9.999 4 8 0 0 259.825 12.485 3 -8 0 0 272.987 11.174 6 9 0 0 1.79267 2.47412 3 -9 0 0 0.45832 1.98064 6 9 0 0 0.41510 1.44256 2 10 0 0 15.6488 4.5394 3 10 0 0 18.7463 3.1635 2 -10 0 0 18.5760 3.7640 6 -11 0 0 3.06640 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39.7572 2.4749 3 3 1 0 39.3850 3.5127 3 -3 1 0 36.1103 2.3944 6 -3 1 0 34.7137 2.7959 4 3 1 0 33.4806 2.6303 2 4 -1 0 109.277 4.845 3 -4 -1 0 104.389 4.793 6 -4 1 0 97.6456 4.5279 6 4 1 0 107.253 5.991 3 4 1 0 95.8416 4.6112 2 -4 1 0 102.272 4.877 4 5 -1 0 60.8596 3.7204 3 -5 -1 0 58.6297 2.3918 5 -5 -1 0 55.1572 3.6813 6 5 -1 0 57.9213 2.6707 2 -5 1 0 58.3000 3.8794 4 -5 1 0 52.5352 3.5007 6 5 1 0 55.1369 4.7710 3 5 1 0 64.5365 3.7749 2 6 -1 0 886.300 26.629 3 -6 -1 0 850.436 25.635 6 -6 -1 0 860.899 22.109 5 6 -1 0 880.514 22.665 2 6 1 0 846.321 28.073 3 -6 1 0 849.878 25.178 6 6 1 0 864.549 24.318 2 -6 1 0 845.206 25.095 4 -7 -1 0 9.86319 2.57081 6 -7 -1 0 13.4813 1.6344 5 7 -1 0 10.9526 1.8167 2 7 -1 0 14.1269 2.6471 3 7 1 0 10.7064 3.6118 3 -7 1 0 11.3002 2.5238 6 -7 1 0 12.7674 2.6285 4 7 1 0 8.64986 2.23851 2 8 -1 0 61.2160 3.5104 2 -8 -1 0 54.2190 3.0626 5 -8 -1 0 65.3461 5.0245 6 8 -1 0 61.9845 4.8642 3 -8 1 0 57.6738 4.5938 4 8 1 0 60.4885 7.4033 3 -8 1 0 49.0642 4.3624 6 8 1 0 55.4511 4.2528 2 9 -1 0 11.4610 3.2283 3 -9 -1 0 17.8001 2.2770 5 9 -1 0 21.5394 2.6536 2 -9 -1 0 20.3064 3.8158 6 9 1 0 12.9581 2.9598 2 -9 1 0 16.7184 3.3662 6 -9 1 0 20.7811 3.4234 4 9 1 0 10.7849 4.6137 3 10 -1 0 163.250 9.958 3 -10 -1 0 152.309 6.187 5 10 -1 0 151.139 6.559 2 -10 -1 0 152.620 8.769 6 -10 1 0 155.356 8.192 4 10 1 0 167.746 8.215 2 10 1 0 148.478 11.013 3 -10 1 0 140.630 8.274 6 -11 -1 0 3.99044 3.10705 6 11 -1 0 6.35881 3.43909 3 11 1 0 7.55083 2.79627 2 -11 1 0 7.12469 3.04244 4 11 1 0 9.59602 5.24361 3 -11 1 0 9.11988 3.15652 6 12 -1 0 46.1290 7.5314 3 -12 -1 0 37.8674 6.1597 6 12 1 0 39.5758 7.7617 3 12 1 0 38.2943 4.9901 2 -12 1 0 32.3835 5.5672 6 -13 -1 0 18.5438 4.4017 6 13 -1 0 7.59248 4.69142 3 -13 1 0 21.4854 4.8181 6 13 1 0 19.5337 6.0165 3 14 -1 0 33.1074 7.2849 3 -14 -1 0 44.9572 6.9542 6 14 1 0 48.5892 9.2218 3 -14 1 0 48.2974 7.0788 6 15 -1 0 3.34911 4.82471 3 -15 -1 0 8.78069 4.31684 6 15 1 0 -5.8217 4.6951 3 -15 1 0 4.04804 3.92893 6 -16 -1 0 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321.361 10.122 6 3 2 0 325.377 12.153 3 3 2 0 323.593 11.150 2 4 -2 0 521.844 17.699 3 4 -2 0 564.642 15.831 1 -4 -2 0 555.554 16.789 6 -4 2 0 544.204 16.280 6 -4 2 0 541.458 17.339 4 4 2 0 558.301 17.121 2 4 2 0 536.559 18.660 3 5 -2 0 46.6040 2.5864 1 5 -2 0 45.0463 3.4898 3 -5 -2 0 47.4418 3.4817 6 -5 2 0 45.1505 3.2568 6 5 2 0 43.9709 5.1348 3 -5 2 0 47.6227 3.9466 4 5 2 0 44.9390 3.8272 2 6 -2 0 57.6459 4.2657 3 -6 -2 0 58.1241 4.1768 6 6 2 0 54.6415 5.9859 3 -6 2 0 58.2901 4.5591 4 6 2 0 64.5006 4.6606 2 -6 2 0 61.0247 4.0322 6 -7 -2 0 155.079 7.764 6 7 -2 0 146.567 7.602 3 -7 2 0 155.822 8.017 4 -7 2 0 155.521 7.245 6 7 2 0 151.480 7.725 2 7 2 0 170.824 9.498 3 8 -2 0 151.409 5.687 2 -8 -2 0 157.880 8.194 6 8 -2 0 141.008 7.768 3 8 2 0 139.894 9.532 3 8 2 0 153.978 8.099 2 -8 2 0 144.703 7.455 6 -8 2 0 153.029 8.055 4 9 -2 0 0.14433 1.25050 2 -9 -2 0 -2.2422 1.8544 6 9 -2 0 -0.1635 1.4991 3 -9 2 0 2.18338 2.13023 6 9 2 0 0.35411 2.02815 2 9 2 0 -2.2745 3.1895 3 -9 2 0 -1.4138 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6.5122 3 -17 2 0 4.83766 4.67885 6 18 -2 0 8.06848 8.26971 3 -18 -2 0 3.37634 5.23089 6 18 2 0 8.62336 7.84746 3 -18 2 0 1.21970 4.46239 6 19 -2 0 2.50205 8.39556 3 -19 -2 0 2.93151 6.07033 6 -19 2 0 3.55145 5.79277 6 19 2 0 9.17938 8.11194 3 -20 2 0 -0.7754 6.1309 6 0 -3 0 0.92616 0.54811 1 0 -3 0 0.15716 0.54225 6 0 3 0 -1.1630 1.1872 4 0 3 0 0.21543 1.35083 3 -1 -3 0 166.820 7.565 1 1 -3 0 173.461 7.263 1 -1 -3 0 182.242 6.251 6 1 3 0 175.092 6.879 4 -1 3 0 163.134 7.417 4 -1 3 0 175.943 8.267 3 -1 3 0 181.264 6.933 6 -2 -3 0 243.244 9.615 1 -2 -3 0 228.124 8.016 6 2 -3 0 231.589 8.815 1 -2 3 0 233.861 9.978 3 2 3 0 230.584 8.078 4 2 3 0 233.790 10.236 3 -2 3 0 231.437 8.221 6 -2 3 0 236.019 9.423 4 3 -3 0 75.7688 4.1495 1 -3 -3 0 72.0579 4.0133 6 3 3 0 78.8613 5.7283 3 3 3 0 83.8668 5.4403 2 -3 3 0 75.1844 5.1091 4 -3 3 0 72.8248 5.2473 3 -3 3 0 77.7455 3.9563 6 3 3 0 81.2747 3.6794 4 -4 -3 0 3.04225 1.51851 6 4 -3 0 5.03877 1.40304 1 4 3 0 2.05825 2.11131 3 -4 3 0 2.42649 1.49289 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