data_amx-f13-et-100k _audit_creation_date 2017-07-22 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address 'Department of Chemical Science, IISER Mohali' _publ_contact_author_email angshurc@iisermohali.ac.in _publ_contact_author_id_orcid ? _publ_contact_author_name 'Angshuman Roy Choudhury' _publ_contact_author_phone 8054001404 _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '(C4 H3 O4)-, (C17 H17 Cl N3 O)+' _chemical_formula_sum 'C21 H20 Cl N3 O5' _chemical_formula_weight 429.85 _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.5724(6) _cell_length_b 9.8586(3) _cell_length_c 9.7866(3) _cell_angle_alpha 90 _cell_angle_beta 97.143(3) _cell_angle_gamma 90 _cell_volume 1969.46(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7223 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 28.0830 _cell_measurement_theta_min 2.8570 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 43349 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 32.839 _diffrn_reflns_theta_min 2.873 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -69.00 119.00 0.40 10.00 -- 29.89 54.00 90.00 470 2 \w -69.00 119.00 0.40 10.00 -- 29.89 54.00-120.00 470 3 \w -69.00 119.00 0.40 10.00 -- 29.89 54.00-150.00 470 4 \w -69.00 60.20 0.40 10.00 -- 29.89 54.00 -90.00 323 5 \w -69.00 119.00 0.40 10.00 -- 29.89 54.00 0.00 470 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (ROW)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0226990000 _diffrn_orient_matrix_UB_12 0.0477663000 _diffrn_orient_matrix_UB_13 0.0322958000 _diffrn_orient_matrix_UB_21 0.0256280000 _diffrn_orient_matrix_UB_22 -0.0478773000 _diffrn_orient_matrix_UB_23 -0.0012696000 _diffrn_orient_matrix_UB_31 0.0059086000 _diffrn_orient_matrix_UB_32 0.0244877000 _diffrn_orient_matrix_UB_33 -0.0655332000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4998 _reflns_number_total 7218 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.30 _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 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)' _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.478 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.098 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 7218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0677 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+1.0838P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1684 _refine_ls_wR_factor_ref 0.1989 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H) groups 2.a Secondary CH2 refined with riding coordinates: N3(H3A,H3B), C17(H17A,H17B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B) 2.b Aromatic/amide H refined with riding coordinates: C4(H4), C6(H6), C7(H7), C19(H19), C20(H20), C9(H9), C10(H10), C11(H11), C12(H12) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _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 O3 O 0.02156(6) 1.04820(14) 0.86226(13) 0.0261(3) Uani 1 1 d . . . . . O1 O 0.37354(6) 0.79450(14) 0.96805(13) 0.0251(3) Uani 1 1 d . . . . . O5 O 0.12280(7) 0.97394(15) 0.50639(15) 0.0307(3) Uani 1 1 d . . . . . O4 O 0.10029(8) 1.11341(17) 0.32887(15) 0.0346(3) Uani 1 1 d . . . . . O2 O 0.08989(7) 0.94987(15) 0.73477(15) 0.0319(3) Uani 1 1 d . . . . . N2 N 0.24084(7) 0.63216(15) 0.66639(16) 0.0220(3) Uani 1 1 d . . . . . N3 N 0.11352(7) 0.52028(16) 0.58218(16) 0.0238(3) Uani 1 1 d . . . . . H3A H 0.0798 0.5067 0.5174 0.029 Uiso 1 1 calc R . . . . H3B H 0.1046 0.4802 0.6592 0.029 Uiso 1 1 calc R . . . . N1 N 0.34555(7) 0.58247(16) 0.76700(16) 0.0233(3) Uani 1 1 d . . . . . C4 C 0.28580(8) 0.91107(18) 0.63898(18) 0.0228(3) Uani 1 1 d . . . . . H4 H 0.2643 0.8763 0.5573 0.027 Uiso 1 1 calc R . . . . C8 C 0.40957(8) 0.61707(19) 0.82288(18) 0.0236(3) Uani 1 1 d . . . . . C1 C 0.30180(8) 0.67315(18) 0.73236(17) 0.0209(3) Uani 1 1 d . . . . . C6 C 0.32442(9) 1.1058(2) 0.7785(2) 0.0264(4) Uani 1 1 d . . . . . H6 H 0.3276 1.1994 0.7897 0.032 Uiso 1 1 calc R . . . . C13 C 0.42461(9) 0.71952(19) 0.92153(18) 0.0240(3) Uani 1 1 d . . . . . C21 C 0.04786(9) 1.04055(18) 0.75488(19) 0.0236(3) Uani 1 1 d . . . . . C3 C 0.34478(8) 0.87913(19) 0.86438(18) 0.0228(3) Uani 1 1 d . . . . . C2 C 0.31073(8) 0.82348(18) 0.74561(18) 0.0222(3) Uani 1 1 d . . . . . C7 C 0.35043(9) 1.0186(2) 0.88312(19) 0.0252(4) Uani 1 1 d . . . . . H7 H 0.3715 1.0535 0.9652 0.030 Uiso 1 1 calc R . . . . C17 C 0.23260(8) 0.48516(18) 0.64372(19) 0.0234(3) Uani 1 1 d . . . . . H17A H 0.2263 0.4409 0.7296 0.028 Uiso 1 1 calc R . . . . H17B H 0.2717 0.4478 0.6118 0.028 Uiso 1 1 calc R . . . . C19 C 0.04847(9) 1.16224(19) 0.52209(19) 0.0256(4) Uani 1 1 d . . . . . H19 H 0.0310 1.2378 0.4738 0.031 Uiso 1 1 calc R . . . . C5 C 0.29349(9) 1.05015(18) 0.65644(19) 0.0236(3) Uani 1 1 d . . . . . C18 C 0.09337(9) 1.0786(2) 0.44717(19) 0.0251(3) Uani 1 1 d . . . . . C14 C 0.18193(8) 0.6925(2) 0.71335(19) 0.0242(3) Uani 1 1 d . . . . . H14A H 0.1885 0.7891 0.7277 0.029 Uiso 1 1 calc R . . . . H14B H 0.1743 0.6520 0.8003 0.029 Uiso 1 1 calc R . . . . C20 C 0.02921(9) 1.14687(19) 0.64639(19) 0.0251(4) Uani 1 1 d . . . . . H20 H -0.0003 1.2118 0.6697 0.030 Uiso 1 1 calc R . . . . C15 C 0.12282(9) 0.66873(19) 0.6068(2) 0.0251(3) Uani 1 1 d . . . . . H15A H 0.0840 0.7067 0.6392 0.030 Uiso 1 1 calc R . . . . H15B H 0.1293 0.7137 0.5213 0.030 Uiso 1 1 calc R . . . . C16 C 0.17387(9) 0.45918(19) 0.53761(19) 0.0245(3) Uani 1 1 d . . . . . H16A H 0.1817 0.4980 0.4500 0.029 Uiso 1 1 calc R . . . . H16B H 0.1677 0.3622 0.5251 0.029 Uiso 1 1 calc R . . . . C9 C 0.46141(9) 0.5384(2) 0.7876(2) 0.0263(4) Uani 1 1 d . . . . . H9 H 0.4529 0.4681 0.7244 0.032 Uiso 1 1 calc R . . . . C10 C 0.52539(9) 0.5629(2) 0.8449(2) 0.0302(4) Uani 1 1 d . . . . . H10 H 0.5593 0.5099 0.8193 0.036 Uiso 1 1 calc R . . . . C11 C 0.53911(9) 0.6666(2) 0.9405(2) 0.0307(4) Uani 1 1 d . . . . . H11 H 0.5821 0.6835 0.9781 0.037 Uiso 1 1 calc R . . . . C12 C 0.48814(9) 0.7452(2) 0.9799(2) 0.0283(4) Uani 1 1 d . . . . . H12 H 0.4968 0.8140 1.0447 0.034 Uiso 1 1 calc R . . . . Cl1 Cl 0.26573(2) 1.15751(5) 0.52086(5) 0.02984(13) Uani 1 1 d . . . . . H5 H 0.1094(18) 0.974(4) 0.609(4) 0.076(11) 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 O3 0.0246(6) 0.0308(7) 0.0229(6) 0.0008(5) 0.0033(5) 0.0015(5) O1 0.0246(6) 0.0290(7) 0.0217(6) 0.0010(5) 0.0025(5) 0.0024(5) O5 0.0342(7) 0.0296(7) 0.0298(7) 0.0017(6) 0.0099(6) 0.0055(6) O4 0.0400(8) 0.0381(8) 0.0262(7) 0.0011(6) 0.0064(6) 0.0029(6) O2 0.0365(7) 0.0326(8) 0.0271(7) 0.0041(6) 0.0063(6) 0.0125(6) N2 0.0185(6) 0.0208(7) 0.0263(7) -0.0023(5) 0.0015(5) 0.0011(5) N3 0.0200(6) 0.0250(8) 0.0262(7) -0.0012(6) 0.0023(5) -0.0012(5) N1 0.0210(6) 0.0246(7) 0.0242(7) 0.0016(6) 0.0021(5) 0.0005(5) C4 0.0208(7) 0.0238(8) 0.0237(8) -0.0011(6) 0.0025(6) 0.0017(6) C8 0.0205(7) 0.0258(9) 0.0246(8) 0.0047(7) 0.0025(6) 0.0016(6) C1 0.0202(7) 0.0222(8) 0.0207(7) -0.0013(6) 0.0041(6) -0.0009(6) C6 0.0275(8) 0.0220(9) 0.0300(9) -0.0026(7) 0.0050(7) -0.0010(7) C13 0.0228(8) 0.0265(9) 0.0224(7) 0.0022(6) 0.0023(6) 0.0004(6) C21 0.0236(8) 0.0230(8) 0.0241(8) -0.0014(6) 0.0023(6) 0.0008(6) C3 0.0214(7) 0.0253(8) 0.0220(7) -0.0005(6) 0.0042(6) -0.0001(6) C2 0.0188(7) 0.0227(8) 0.0254(8) -0.0021(6) 0.0036(6) -0.0010(6) C7 0.0238(8) 0.0261(9) 0.0260(8) -0.0064(7) 0.0043(6) -0.0006(6) C17 0.0209(7) 0.0204(8) 0.0286(8) -0.0010(6) 0.0016(6) 0.0006(6) C19 0.0255(8) 0.0245(9) 0.0262(8) 0.0010(7) 0.0004(6) 0.0012(6) C5 0.0218(7) 0.0217(8) 0.0274(8) 0.0011(6) 0.0041(6) 0.0019(6) C18 0.0253(8) 0.0254(9) 0.0246(8) -0.0028(7) 0.0029(6) -0.0016(6) C14 0.0199(7) 0.0252(9) 0.0280(8) -0.0044(7) 0.0043(6) 0.0002(6) C20 0.0238(8) 0.0250(9) 0.0263(8) -0.0007(7) 0.0018(6) 0.0037(6) C15 0.0199(7) 0.0245(9) 0.0305(9) 0.0002(7) 0.0011(6) 0.0009(6) C16 0.0231(8) 0.0245(9) 0.0259(8) -0.0036(6) 0.0036(6) 0.0003(6) C9 0.0239(8) 0.0288(9) 0.0261(8) 0.0034(7) 0.0031(6) 0.0034(7) C10 0.0217(8) 0.0366(11) 0.0325(9) 0.0062(8) 0.0047(7) 0.0039(7) C11 0.0212(8) 0.0387(11) 0.0309(9) 0.0053(8) -0.0014(7) -0.0014(7) C12 0.0242(8) 0.0322(10) 0.0271(8) 0.0019(7) -0.0016(7) -0.0013(7) Cl1 0.0340(2) 0.0224(2) 0.0321(2) 0.00297(16) 0.00029(18) 0.00302(16) _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 O3 C21 1.243(2) . ? O1 C13 1.406(2) . ? O1 C3 1.388(2) . ? O5 C18 1.296(2) . ? O5 H5 1.08(4) . ? O4 C18 1.233(2) . ? O2 C21 1.276(2) . ? O2 H5 1.36(4) . ? N2 C1 1.397(2) . ? N2 C17 1.473(2) . ? N2 C14 1.474(2) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 C15 1.492(2) . ? N3 C16 1.493(2) . ? N1 C8 1.404(2) . ? N1 C1 1.284(2) . ? C4 H4 0.9300 . ? C4 C2 1.402(2) . ? C4 C5 1.388(3) . ? C8 C13 1.405(3) . ? C8 C9 1.397(3) . ? C1 C2 1.497(2) . ? C6 H6 0.9300 . ? C6 C7 1.392(3) . ? C6 C5 1.394(3) . ? C13 C12 1.383(2) . ? C21 C20 1.507(3) . ? C3 C2 1.393(2) . ? C3 C7 1.390(3) . ? C7 H7 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C16 1.514(2) . ? C19 H19 0.9300 . ? C19 C18 1.496(3) . ? C19 C20 1.334(3) . ? C5 Cl1 1.7373(19) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.518(2) . ? C20 H20 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C9 H9 0.9300 . ? C9 C10 1.386(3) . ? C10 H10 0.9300 . ? C10 C11 1.391(3) . ? C11 H11 0.9300 . ? C11 C12 1.396(3) . ? C12 H12 0.9300 . ? 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 C3 O1 C13 110.31(13) . . ? C18 O5 H5 105(2) . . ? C21 O2 H5 107.5(16) . . ? C1 N2 C17 115.73(14) . . ? C1 N2 C14 117.71(14) . . ? C17 N2 C14 111.11(14) . . ? H3A N3 H3B 108.1 . . ? C15 N3 H3A 109.6 . . ? C15 N3 H3B 109.6 . . ? C15 N3 C16 110.39(14) . . ? C16 N3 H3A 109.6 . . ? C16 N3 H3B 109.6 . . ? C1 N1 C8 121.78(16) . . ? C2 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C5 C4 C2 119.43(16) . . ? N1 C8 C13 123.93(16) . . ? C9 C8 N1 118.48(17) . . ? C9 C8 C13 117.36(16) . . ? N2 C1 C2 114.83(15) . . ? N1 C1 N2 118.70(16) . . ? N1 C1 C2 126.29(16) . . ? C7 C6 H6 120.7 . . ? C7 C6 C5 118.66(17) . . ? C5 C6 H6 120.7 . . ? C8 C13 O1 119.40(15) . . ? C12 C13 O1 118.42(17) . . ? C12 C13 C8 122.11(17) . . ? O3 C21 O2 123.21(17) . . ? O3 C21 C20 117.00(16) . . ? O2 C21 C20 119.78(16) . . ? O1 C3 C2 119.85(16) . . ? O1 C3 C7 118.49(16) . . ? C7 C3 C2 121.66(17) . . ? C4 C2 C1 121.05(15) . . ? C3 C2 C4 118.56(16) . . ? C3 C2 C1 120.38(16) . . ? C6 C7 H7 120.1 . . ? C3 C7 C6 119.72(17) . . ? C3 C7 H7 120.1 . . ? N2 C17 H17A 109.7 . . ? N2 C17 H17B 109.7 . . ? N2 C17 C16 109.69(14) . . ? H17A C17 H17B 108.2 . . ? C16 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C18 C19 H19 114.5 . . ? C20 C19 H19 114.5 . . ? C20 C19 C18 130.97(17) . . ? C4 C5 C6 121.81(17) . . ? C4 C5 Cl1 119.09(14) . . ? C6 C5 Cl1 119.08(14) . . ? O5 C18 C19 120.13(16) . . ? O4 C18 O5 122.64(18) . . ? O4 C18 C19 117.23(17) . . ? N2 C14 H14A 109.6 . . ? N2 C14 H14B 109.6 . . ? N2 C14 C15 110.06(15) . . ? H14A C14 H14B 108.2 . . ? C15 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C21 C20 H20 115.0 . . ? C19 C20 C21 130.01(17) . . ? C19 C20 H20 115.0 . . ? N3 C15 C14 109.74(15) . . ? N3 C15 H15A 109.7 . . ? N3 C15 H15B 109.7 . . ? C14 C15 H15A 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N3 C16 C17 110.68(15) . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C8 C9 H9 119.4 . . ? C10 C9 C8 121.25(19) . . ? C10 C9 H9 119.4 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.24(18) . . ? C11 C10 H10 119.9 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.80(17) . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.22(18) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 3 0 0 976.48 17.7 3 0 0 1042.41 18.86 -3 0 0 817.63 17.1 -3 0 0 1039.66 18.48 -3 0 0 807.92 17.03 3 0 0 1057.01 17.89 3 0 0 1059.77 18.87 4 0 0 3.68 0.87 -4 0 0 4.5 0.88 -4 0 0 4.93 1.06 4 0 0 2.84 0.77 4 0 0 4.56 1.05 -5 0 0 6548.51 102.33 5 0 0 6334.53 104.09 5 0 0 6196.29 101.99 -5 0 0 6533.69 103.33 5 0 0 6396.13 103.91 6 0 0 123.12 6.57 -6 0 0 122.52 6.22 -6 0 0 127.97 5.92 6 0 0 130.2 6.61 6 0 0 139.65 6.12 7 0 0 23.27 2.67 -7 0 0 28.52 3.18 7 0 0 21.29 2.93 -7 0 0 21.79 2.61 7 0 0 22.04 3.03 -8 0 0 449.75 13.96 8 0 0 483 14.14 -8 0 0 461.97 14.96 8 0 0 456.81 15.52 8 0 0 449.82 15.41 9 0 0 267.25 12.3 -9 0 0 271.16 10.79 9 0 0 268.19 11.88 9 0 0 280.69 10.95 -9 0 0 266.38 11.42 -10 0 0 -0.75 0.9 10 0 0 1.09 1.19 10 0 0 2.15 1.2 10 0 0 0.92 1 -10 0 0 -0.8 1.47 11 0 0 537.68 17.46 11 0 0 486.26 18.71 11 0 0 500.94 19.18 -11 0 0 547.07 17.6 -11 0 0 562.95 18.94 12 0 0 5.09 2.09 12 0 0 12.64 3.08 -12 0 0 7.49 2.18 -12 0 0 8.13 2.11 12 0 0 8.64 2.32 -13 0 0 935.8 28.23 13 0 0 914.2 26.16 -13 0 0 964.17 26.62 13 0 0 949.1 29.52 13 0 0 917.68 29.24 14 0 0 800.06 27.7 -14 0 0 812.76 24.92 14 0 0 882.92 25.87 14 0 0 826.72 28.5 -14 0 0 832.23 27.1 15 0 0 159.99 11.87 15 0 0 178.37 12.46 -15 0 0 153.51 10.01 -15 0 0 151.55 11.15 15 0 0 153.68 10.26 16 0 0 101.35 10.24 16 0 0 102.99 8.63 16 0 0 115.8 10.81 -16 0 0 127.43 10.19 -16 0 0 113.68 8.95 17 0 0 238.04 13.64 17 0 0 206.21 14.8 17 0 0 256.09 16.51 -17 0 0 248.67 13.84 -17 0 0 207.57 14.04 -18 0 0 33.57 5.78 18 0 0 34.35 5.36 18 0 0 27.28 5.18 -18 0 0 26.21 4.19 18 0 0 22.38 5.01 19 0 0 0.07 1.45 -19 0 0 -0.97 1.35 19 0 0 0.34 1.1 19 0 0 2.29 1.81 -19 0 0 0.49 1.01 20 0 0 32.12 5.63 -20 0 0 39.59 6.86 20 0 0 33.43 6.75 20 0 0 40.18 7.04 -20 0 0 36.72 5.94 21 0 0 -0.69 2.39 21 0 0 2.3 1.88 21 0 0 5.39 2.27 -21 0 0 0.82 1.5 -21 0 0 2.84 1.61 -22 0 0 22.03 4.72 22 0 0 19.36 5.5 22 0 0 29.86 5.72 -22 0 0 29.92 6.51 22 0 0 35.24 7 23 0 0 34.34 6.27 23 0 0 33.14 7.48 -23 0 0 30.7 5.89 23 0 0 35.02 7.46 -23 0 0 31.58 6.6 -24 0 0 -1.42 1.98 24 0 0 -0.41 1.86 24 0 0 0.09 1.95 24 0 0 3.96 2.84 25 0 0 68.41 11.39 25 0 0 80.18 11.59 -25 0 0 88.08 11.58 25 0 0 86.58 10.53 -26 0 0 51.71 9.13 26 0 0 60.43 10.88 26 0 0 42.31 9.37 27 0 0 27.89 7.69 -27 0 0 13.34 5.67 27 0 0 20.18 6.69 28 0 0 84.35 13.62 28 0 0 81.9 12.78 -28 0 0 89.55 12.58 29 0 0 0.12 2.86 29 0 0 11.18 4.49 30 0 0 2.67 3.1 30 0 0 9.02 6.01 2 1 0 1212.39 12.53 2 -1 0 1221.56 11.55 -2 -1 0 872.34 10.36 2 1 0 1279.93 12.46 -2 -1 0 1261.9 13.58 2 -1 0 1218.53 13.44 2 -1 0 1238.93 12.92 -2 1 0 1195.29 13.57 -2 1 0 1187.59 10.66 2 1 0 1253.79 9.89 -3 -1 0 182.32 6.27 3 1 0 181.32 6.09 -3 1 0 168.55 6.2 3 1 0 168.51 5.7 3 -1 0 181.17 6.3 3 -1 0 176.46 5.61 3 -1 0 168.73 6.12 3 1 0 175.72 5.3 3 -1 0 155.62 5.11 -3 1 0 177.31 5.36 -3 -1 0 157.84 5.18 4 1 0 831.59 18.05 -4 -1 0 830.87 17.4 4 -1 0 794.64 17.91 -4 -1 0 845.22 17.87 -4 1 0 835.76 16.41 -4 -1 0 764.59 14.8 4 1 0 825.73 16.89 -4 1 0 789.6 17.94 4 -1 0 841.4 17.51 4 -1 0 726.78 17.75 4 1 0 805.47 14.84 -5 1 0 3203.38 52.32 5 1 0 3122.33 54.92 5 1 0 3173.29 50.8 -5 -1 0 3188.02 54.3 -5 1 0 3061.95 54.75 5 1 0 3114.44 53.37 5 -1 0 3256.41 55.59 -5 -1 0 3180.4 53.91 5 -1 0 3161.75 54.14 5 -1 0 3067.43 54.37 6 1 0 2.28 1.07 6 -1 0 -0.02 0.48 6 -1 0 1.62 1.43 6 1 0 -0.6 0.82 -6 -1 0 -0.64 0.75 6 -1 0 0.38 0.38 -6 1 0 2.22 1.16 6 1 0 3.55 0.93 -6 -1 0 -0.32 0.46 -6 1 0 -0.99 0.69 -7 1 0 82.35 4.78 -7 -1 0 80.8 5.34 7 1 0 83.98 4.46 7 1 0 90.5 6.06 -7 -1 0 80.25 5.35 7 1 0 80.45 5.3 7 -1 0 88.47 5.87 7 -1 0 77.49 5.75 -7 1 0 83.71 5.63 7 -1 0 87.16 5.79 -8 1 0 195.85 9.44 8 1 0 175.8 7.36 -8 1 0 202.03 8.29 8 1 0 195.22 9.73 -8 -1 0 198.79 9.07 8 -1 0 199.84 10.05 -8 -1 0 194.65 9.05 8 -1 0 185.95 9.38 8 1 0 202.08 9.28 8 -1 0 201.54 9.34 -9 -1 0 449.52 15.16 9 -1 0 466.82 15.61 -9 -1 0 436.4 15.19 -9 1 0 441.28 15.67 9 1 0 445.7 16.48 9 -1 0 462.5 16.66 -9 1 0 416.41 13.58 9 -1 0 449.12 16.04 9 1 0 456.22 15.72 9 1 0 446.74 13.27 10 1 0 66.92 5.84 10 -1 0 71.32 6.17 10 1 0 80.22 6.72 10 -1 0 80.95 6.4 -10 -1 0 72.64 6.06 10 1 0 76.23 5.22 -10 1 0 77.17 6.38 -10 1 0 79.33 5.55 -10 -1 0 67.57 5.74 10 -1 0 63.49 6.38 11 1 0 8.52 2.16 -11 1 0 12.37 2.88 11 -1 0 7.43 2.14 11 1 0 11.34 2.75 -11 -1 0 9.04 2.15 -11 1 0 9.69 2 11 -1 0 8.56 2.92 11 -1 0 5.94 1.74 11 1 0 11.74 2.27 -11 -1 0 7.67 1.83 -12 -1 0 218.52 11.76 -12 1 0 208.07 11.87 12 -1 0 227.74 12.56 -12 -1 0 226.13 11.74 12 -1 0 229.73 11.94 12 1 0 219.73 10.22 12 1 0 207.91 12.47 -12 1 0 223.73 10.63 12 1 0 219.49 12.28 12 -1 0 205.46 12.78 -13 1 0 96.19 7.22 13 1 0 105.9 7.18 13 1 0 102.19 9.11 13 1 0 103.79 8.7 -13 1 0 112.79 8.95 13 -1 0 93.72 8.86 -13 -1 0 96.73 8.02 -13 -1 0 101.93 8.03 13 -1 0 110.94 9.03 13 -1 0 96.01 7.91 -14 -1 0 27.65 4.5 14 1 0 39.44 5.36 14 -1 0 39.44 5.54 -14 1 0 36.8 4.47 14 1 0 40.72 4.58 -14 1 0 29.62 4.84 -14 -1 0 39.06 5.2 14 -1 0 39.75 5.93 14 -1 0 36.72 4.99 14 1 0 30.38 5.35 15 1 0 4.3 2.21 -15 -1 0 0.37 0.83 15 1 0 1.19 1.12 -15 1 0 0.63 0.94 15 -1 0 1.29 0.74 15 -1 0 -0.68 0.99 15 1 0 1.52 1.3 15 -1 0 -0.9 1.28 -15 1 0 -0.47 1.34 -15 -1 0 1.11 1.27 -16 1 0 489.02 21.71 -16 1 0 489.88 19.11 16 1 0 497.69 18.96 16 1 0 539.12 24.1 -16 -1 0 512.42 20.92 -16 -1 0 524.85 21.92 16 1 0 527.42 22.83 16 -1 0 514.54 21.31 16 -1 0 488.28 22.59 16 -1 0 525.96 23.92 -17 -1 0 439.21 19.83 17 1 0 469.76 18.95 17 1 0 454.89 22.7 -17 1 0 421.53 18.23 17 -1 0 433.88 22.18 17 1 0 501.62 22.87 17 -1 0 456.43 20.66 -17 -1 0 482.08 21.54 -17 1 0 495.96 22.44 17 -1 0 527.45 24.07 -18 -1 0 238.21 14.53 18 1 0 240.83 13.58 18 -1 0 256.64 15.49 -18 1 0 214.72 13.01 -18 -1 0 265.28 16.12 -18 1 0 249.11 16.23 18 1 0 238.39 16.14 18 -1 0 236.57 16.04 18 -1 0 210.1 15.73 18 1 0 247.4 16.95 19 -1 0 3.85 2.69 -19 1 0 3.59 3.12 19 1 0 -0.65 1.75 19 -1 0 5.37 2.86 -19 -1 0 1.1 1.84 19 1 0 3.28 2.32 -19 -1 0 7.54 3.18 19 -1 0 0.78 1.73 -19 1 0 1.15 1.49 19 1 0 2.69 2.12 20 1 0 73.55 9.69 20 1 0 76.63 7.92 -20 -1 0 86.07 9.95 -20 1 0 69.74 7.72 20 -1 0 78.64 9.96 20 -1 0 75.65 9.93 -20 1 0 84.91 9.9 20 -1 0 84.29 9.42 -20 -1 0 75.88 8.6 20 1 0 71.19 9.47 -21 -1 0 15.45 4.36 -21 -1 0 23.25 4.76 21 -1 0 18.63 4.44 21 1 0 19.75 4.98 21 1 0 17.39 4.11 -21 1 0 17 3.88 21 -1 0 22.97 5.52 21 1 0 15.29 5 -21 1 0 16.16 4.29 21 -1 0 17.58 4.59 22 -1 0 -0.27 2.21 -22 1 0 -4.11 2.04 22 1 0 1.43 1.59 22 1 0 2.7 3.11 22 -1 0 5.01 3.87 22 1 0 -1.44 2.53 -22 -1 0 -3.83 1.82 -22 -1 0 2.45 2.51 22 -1 0 -0.42 1.81 -22 1 0 -1.58 1.57 23 1 0 27.51 5.53 -23 -1 0 16.52 4.97 -23 1 0 27.37 5.66 -23 -1 0 31.04 6.71 23 -1 0 21.22 5.34 23 -1 0 22.44 5.67 23 1 0 24.83 6.47 23 1 0 24.19 6.72 23 -1 0 30.07 6.93 -23 1 0 0.17 1.91 24 -1 0 7.72 3.28 -24 -1 0 -1.43 1.51 24 -1 0 8.9 4.2 24 1 0 11.6 4.83 -24 1 0 5.72 2.2 24 1 0 6.01 4.71 24 -1 0 12.71 5.22 -24 -1 0 8.73 4.47 25 1 0 1.33 2.7 25 1 0 3.02 1.77 -25 1 0 7.59 4.13 25 -1 0 7.33 3.68 25 -1 0 5.94 3.71 25 -1 0 10.11 5.02 -25 -1 0 12.97 5.37 26 1 0 -0.53 2.03 26 -1 0 2.39 2.93 26 -1 0 1.97 2.48 26 -1 0 2.02 2.26 -26 -1 0 -0.73 2.24 -26 1 0 0.38 3.2 26 1 0 1.31 2.9 27 1 0 24.94 6.9 -27 -1 0 36.09 8.17 27 -1 0 31.15 8.61 27 1 0 27.28 7.83 -27 1 0 21.02 6.4 27 -1 0 22.91 7.4 28 1 0 4.14 3.5 28 1 0 5.26 4.63 28 -1 0 13.59 6.19 -28 -1 0 14.92 6.46 -28 1 0 13.66 5.69 28 -1 0 3.58 4 29 1 0 10.07 5.85 29 -1 0 11.33 6.08 29 1 0 8.97 5.77 29 -1 0 15.08 6.44 30 -1 0 27.85 8.88 30 1 0 7.83 5.25 30 -1 0 15.33 6.07 31 1 0 20.34 7.96 0 -2 0 2707.42 41.68 0 -2 0 2709.28 43.88 0 -2 0 2677.65 45.38 0 2 0 2706.72 45.56 0 2 0 2586.39 41.61 -1 2 0 2355.81 40.1 -1 2 0 2073.51 36.79 1 2 0 2215.24 36.72 1 -2 0 2406.67 37.3 -1 -2 0 2288.4 36.88 -1 -2 0 2181.17 36.55 1 2 0 2354.22 39.59 1 -2 0 2275.69 39.14 1 2 0 2314.84 36.7 -1 -2 0 2285.58 39.97 1 -2 0 2264.68 38.86 -2 -2 0 60.06 3.97 -2 2 0 58.53 2.56 -2 2 0 56.84 3.83 -2 -2 0 65.37 2.48 2 2 0 62.71 3.19 2 2 0 66.78 3.87 2 -2 0 70.43 4.1 2 -2 0 62.66 2.67 2 2 0 64.31 2.5 2 -2 0 53.64 3.49 2 -2 0 63.91 3.43 3 -2 0 19.72 2.12 3 -2 0 15.92 2.08 3 2 0 19.21 1.95 -3 -2 0 17.48 1.51 -3 2 0 24.74 2.34 -3 2 0 21.23 2.5 3 2 0 18.75 1.45 -3 -2 0 16.99 2.18 3 -2 0 21.41 1.82 3 2 0 16.03 2 4 -2 0 474.74 13.69 -4 2 0 509.29 12.79 4 -2 0 537.15 14.69 4 2 0 512.35 11.54 4 2 0 495.57 13.3 -4 2 0 496.75 14.51 4 2 0 498.3 13.55 4 -2 0 513.33 12.36 -4 -2 0 509.98 14.37 5 2 0 758.1 18.46 5 2 0 713.3 13.53 5 -2 0 715.57 18.77 5 -2 0 745.42 19.13 -5 2 0 718.68 18.99 5 2 0 753.19 16.35 -5 2 0 763.07 17.17 5 2 0 731.95 18.06 -5 -2 0 731.53 18.87 5 -2 0 729.1 17.08 -6 2 0 23.96 3.29 6 2 0 21.05 1.67 -6 2 0 20.91 2.41 -6 -2 0 20.32 2.79 6 2 0 23.6 3.05 6 -2 0 23.32 3.07 -6 -2 0 21.78 2.76 6 -2 0 20.76 3.05 6 -2 0 25.69 2.87 6 2 0 22.01 2.75 6 2 0 25.47 2.53 7 -2 0 91.93 6.36 -7 2 0 79.36 4.95 -7 -2 0 81.99 5.5 7 -2 0 76.64 6 7 2 0 80.18 5.86 7 2 0 87.21 3.89 -7 -2 0 86.51 5.98 7 -2 0 80.73 5.5 -7 2 0 72.41 5.72 7 2 0 84.97 5.27 8 -2 0 43.6 4.29 8 2 0 41.28 2.92 8 2 0 39.99 4.31 8 -2 0 38.61 4.36 -8 -2 0 41.77 4.28 8 2 0 37.89 3.81 -8 -2 0 43.05 4.15 -8 2 0 34.44 4.15 -8 2 0 33.84 3.36 8 -2 0 40 4.75 -9 2 0 1315.51 32.61 -9 -2 0 1282.97 31.07 9 -2 0 1383.95 33.01 -9 2 0 1340.09 29.18 9 -2 0 1342.68 31.66 9 2 0 1343.06 32.96 -9 -2 0 1344.36 32.22 9 2 0 1344.26 26.44 9 -2 0 1262.84 32.85 9 2 0 1396.51 31.09 10 2 0 1.02 1.04 -10 -2 0 0.62 1.02 -10 2 0 1.03 0.48 10 2 0 0.79 0.68 10 -2 0 -0.59 1.04 10 2 0 2.8 1.14 10 -2 0 1.51 0.87 10 -2 0 3.91 2.13 -10 2 0 -1.02 1.13 -10 -2 0 2.19 1.08 -11 -2 0 63.93 6.14 11 2 0 63.55 6 -11 -2 0 65.22 5.97 -11 2 0 70.79 6.75 11 -2 0 65.62 6.33 11 2 0 64.69 6.4 11 2 0 69.46 4.86 11 -2 0 67.37 6.71 -11 2 0 62.41 5.14 11 -2 0 66.1 6.33 -12 -2 0 17.89 3.21 12 2 0 15.91 3.52 12 -2 0 19.61 3.56 -12 -2 0 22.19 3.85 12 -2 0 28.68 4.81 -12 2 0 29.16 4.7 -12 2 0 17.29 2.85 12 2 0 18.16 2.56 12 -2 0 24.16 4.12 12 2 0 24.67 3.93 -13 2 0 -1.74 1.7 -13 2 0 -1.68 1.37 13 2 0 3.44 2.12 -13 -2 0 1.26 1.16 -13 -2 0 -0.98 0.97 13 -2 0 -2.2 1.08 13 -2 0 0.38 1.83 13 2 0 2.68 2.01 13 -2 0 -1.21 1.2 13 2 0 -0.29 0.76 -14 -2 0 34.65 5.22 14 2 0 43.28 6.09 -14 2 0 42.64 4.79 14 -2 0 39.43 5.57 14 2 0 37.3 4.18 -14 2 0 44.74 6.1 14 -2 0 32.11 5.99 14 -2 0 31.48 5.3 14 2 0 44.13 5.74 -14 -2 0 39.29 5.32 15 -2 0 16.39 3.83 -15 -2 0 21.69 4.28 -15 2 0 12.39 3.36 15 2 0 17.52 4.07 15 -2 0 17.31 3.81 -15 -2 0 15.2 3.6 15 -2 0 11.85 3.9 15 2 0 14.91 3.66 15 2 0 16.31 3.12 -15 2 0 11.52 2.6 16 -2 0 400.57 21.95 16 2 0 510.22 21.9 16 -2 0 447.23 20.76 -16 2 0 447.68 18.01 -16 -2 0 502.24 21.26 16 2 0 487.18 22.83 16 2 0 461.6 17.09 -16 -2 0 481.98 20.94 -16 2 0 472.24 21.97 16 -2 0 499.86 22.29 -17 2 0 257.53 13.64 17 -2 0 243.78 16.83 17 -2 0 256.74 16.29 17 2 0 264.17 13.02 17 -2 0 272.15 16.24 17 2 0 274.07 17.32 -17 2 0 279.27 16.91 -17 -2 0 291.25 16.46 17 2 0 258.07 16.08 -17 -2 0 295.7 16.38 18 -2 0 13.65 4.25 18 2 0 21.42 4.82 18 2 0 26.56 5.78 18 2 0 15.1 3.27 18 -2 0 21.16 5.12 -18 -2 0 17.19 4.11 -18 2 0 17.57 4.31 -18 2 0 22.41 3.9 18 -2 0 22.68 5.45 -18 -2 0 19.94 4.28 -19 -2 0 161.66 12.7 19 -2 0 139.48 13.13 -19 -2 0 154.73 12.58 19 -2 0 146.12 12.52 -19 2 0 144.2 13.04 19 2 0 153.58 13.99 19 2 0 139.63 9.86 19 -2 0 152.8 13.16 -19 2 0 133 10.16 19 2 0 139.47 12.43 20 -2 0 8.53 2.91 20 -2 0 12.45 4.56 -20 2 0 14.75 4.45 20 2 0 8.89 3.54 20 2 0 12.84 3.12 -20 2 0 8.44 2.64 20 -2 0 12.43 4.41 -20 -2 0 10.3 3.49 20 2 0 8.76 3.62 -20 -2 0 13.43 4.83 21 -2 0 6.13 2.61 21 2 0 3.84 2.3 -21 -2 0 -2.7 2.46 -21 2 0 3.73 3.14 21 2 0 4.49 2.47 21 2 0 1.21 2.77 -21 2 0 5.54 2.66 21 -2 0 -0.41 1.57 -21 -2 0 1.78 1.61 21 -2 0 6.1 2.97 -22 2 0 12.35 3.6 -22 -2 0 12.74 3.82 22 -2 0 24.48 5.56 22 -2 0 14.14 4.71 22 -2 0 17.24 5.04 22 2 0 22.7 5.78 22 2 0 17.1 5.47 -22 2 0 12.88 4.05 -22 -2 0 20.91 5.32 23 -2 0 1.84 3.35 -23 2 0 1.51 2.37 -23 -2 0 -4.33 3.16 23 2 0 2.83 2.76 23 -2 0 -1.04 1.76 23 2 0 0.49 2.23 23 -2 0 -0.65 2.29 -23 -2 0 -5.41 3.31 24 2 0 -3.06 2.4 -24 -2 0 0.48 2.12 24 -2 0 1.38 2.2 24 2 0 3.09 3 24 -2 0 1.56 2.48 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4.62 2 3 0 89.22 4.21 -2 -3 0 104.7 6.37 2 -3 0 88.46 5.2 -2 3 0 74.25 5.34 3 -3 0 130.15 4.82 -3 -3 0 125.02 4.3 -3 -3 0 128.96 7.17 3 -3 0 133.85 6.41 3 -3 0 128.21 6.94 3 3 0 132.37 4.05 3 3 0 127.25 5.65 -3 3 0 133.77 7.21 3 3 0 127.12 6.57 3 -3 0 126.88 6.21 4 3 0 -0.51 0.42 4 3 0 0.84 0.44 4 -3 0 -0.4 0.74 -4 3 0 -0.02 0.39 4 3 0 1.2 0.79 4 -3 0 -1.13 0.81 4 -3 0 0.73 0.58 -4 3 0 0.44 0.53 4 -3 0 1.18 0.58 -5 3 0 192.52 8.35 5 -3 0 208.5 7.66 5 -3 0 196.72 9.61 -5 -3 0 190.98 9.52 5 3 0 198.06 6.61 -5 3 0 192.78 9.55 5 3 0 189.3 8.86 5 3 0 190.89 8.34 5 -3 0 185.49 8.89 -6 3 0 51.29 4.87 6 3 0 40.12 2.13 6 3 0 56.81 4.72 -6 -3 0 43.14 4.58 6 -3 0 50.13 3.92 6 -3 0 43.05 4.66 6 3 0 50.95 3.47 6 -3 0 45.22 4.58 6 3 0 53.25 4.66 -6 3 0 47.29 4.02 7 3 0 500.31 10.93 -7 -3 0 559.67 18.17 7 3 0 555.99 14.69 -7 3 0 559.02 15.88 7 3 0 539.8 17.03 7 3 0 555.49 17.03 7 -3 0 478.35 17.3 7 -3 0 545.82 15.72 -7 3 0 545.72 18.43 7 -3 0 528.5 18.14 8 3 0 118.88 6.53 -8 -3 0 111.68 7.41 8 3 0 122.68 7.93 8 3 0 123.9 7.69 8 -3 0 119.82 7.16 8 -3 0 128.43 8.4 8 3 0 116.87 4.44 -8 -3 0 112.65 7.82 -8 3 0 122.28 6.88 8 -3 0 131.38 8.51 -8 3 0 133.41 8.97 -9 3 0 -1.19 1.14 9 -3 0 0.42 0.98 -9 3 0 -0.78 1.37 -9 -3 0 -0.23 0.92 9 3 0 0.92 0.72 9 3 0 0.42 0.66 -9 -3 0 -0.23 0.7 9 3 0 0.16 0.56 9 -3 0 -2.06 1.58 9 -3 0 -0.64 1.11 10 3 0 81.85 7.21 10 -3 0 61.71 6.89 10 -3 0 93.06 7.11 10 3 0 86.31 6.4 -10 3 0 74.21 6.95 10 3 0 84.41 4.36 -10 -3 0 80.47 7.14 -10 -3 0 77.08 6.57 -10 3 0 84.75 6.03 10 -3 0 85.07 7.45 -11 -3 0 301.72 13.81 11 -3 0 297.98 14.93 11 3 0 296.52 9.61 11 3 0 296.75 14.63 -11 3 0 286.55 12.15 11 -3 0 303.59 13.86 11 -3 0 291.22 15.44 -11 3 0 308.85 15.41 -11 -3 0 301.61 14.66 11 3 0 311.01 13.23 -12 3 0 1.09 0.7 12 3 0 1.43 0.95 12 -3 0 0.3 1.19 12 -3 0 1.18 1.27 12 -3 0 1.24 1.32 -12 3 0 1.91 0.71 -12 -3 0 4.55 2 -12 -3 0 1.31 1.47 12 3 0 -0.81 0.93 12 3 0 1.99 1.51 13 -3 0 132.95 9.75 -13 -3 0 133.2 9.72 -13 3 0 136.2 8.62 -13 -3 0 146.49 10.7 -13 3 0 141.47 10.91 13 3 0 145.81 11 13 3 0 137.89 6.96 13 -3 0 153.17 11.12 13 3 0 144.29 9.7 13 -3 0 125.51 10.81 -14 -3 0 114.67 9.78 14 3 0 119.39 6.87 -14 -3 0 120.59 9.49 14 -3 0 88.34 9.89 14 3 0 122.37 10.43 14 3 0 129.35 9.68 14 -3 0 124.13 10.41 14 -3 0 125.82 9.87 -14 3 0 107.29 7.88 -14 3 0 99.51 9.54 15 3 0 14.29 2.5 -15 3 0 13.29 3.62 15 -3 0 13.42 3.77 15 3 0 9.04 3.11 -15 -3 0 13.96 3.38 15 3 0 13.24 3.4 15 -3 0 13.81 3.32 -15 3 0 12.15 2.74 15 -3 0 11.54 3.49 -15 -3 0 11.07 3.5 16 3 0 27.61 5.18 -16 -3 0 24.46 4.44 16 -3 0 22.81 5.28 16 -3 0 29.26 5.3 -16 -3 0 31.29 5.39 -16 3 0 25.24 5.07 16 3 0 23.32 4.25 16 3 0 24.47 3.36 16 -3 0 31.1 5.73 -16 3 0 26.16 4.04 -17 -3 0 118.47 10.61 17 -3 0 105.9 11.01 -17 -3 0 121.82 10.94 17 -3 0 130.25 11.4 17 3 0 92.9 7.11 17 3 0 113.28 10.26 17 3 0 131.32 11.93 -17 3 0 112.98 8.83 -17 3 0 116.5 11.08 17 -3 0 117.3 10.86 18 -3 0 361.39 20.08 18 3 0 354.19 14.82 18 -3 0 349.78 20.17 18 3 0 393.25 21.97 18 3 0 398.13 20.27 18 -3 0 397.53 22.38 -18 3 0 378.76 17.21 -18 3 0 385.65 21.48 -18 -3 0 414.34 21.16 -18 -3 0 381.71 19.95 19 -3 0 42.75 6.97 19 -3 0 51.22 8.37 -19 -3 0 38.7 6.55 -19 3 0 55.73 8.16 19 3 0 44.04 7.7 19 -3 0 36.66 6.76 -19 -3 0 45.42 6.89 -19 3 0 37.44 5.3 19 3 0 45.7 7.06 -20 -3 0 -1.24 2.12 -20 3 0 -0.8 1.33 20 -3 0 -1.2 1.81 20 -3 0 0.5 2.87 -20 3 0 -1.93 2.66 20 -3 0 0.28 2.24 20 3 0 -1.58 1.39 20 3 0 -0.62 2.09 -20 -3 0 -4.17 2.13 21 3 0 12.97 4.15 -21 3 0 14.35 4.87 -21 -3 0 21.29 5.38 21 -3 0 15.8 5.2 -21 -3 0 10.79 3.61 21 -3 0 14.95 4.65 21 -3 0 14.35 4.48 -21 3 0 6.62 2.44 21 3 0 8.27 4.14 -22 -3 0 3.03 2.87 22 3 0 0.6 1.54 22 -3 0 1.73 2.24 22 -3 0 -0.45 2.82 22 3 0 -0.35 2.21 22 -3 0 -1.05 2.55 -22 -3 0 -2.24 2.4 -22 3 0 -0.92 2.81 -23 3 0 26.9 6.63 -23 -3 0 26.65 6.44 -23 -3 0 32.14 6.56 23 3 0 37.05 7.89 23 -3 0 33.37 7.17 23 3 0 29.22 6.71 23 -3 0 22.16 6.13 23 -3 0 26.63 6.62 24 -3 0 22.75 6.19 -24 3 0 30.23 6.98 24 -3 0 37.84 7.61 24 3 0 24.41 5.84 -24 -3 0 13.37 4.01 24 3 0 13.6 4.69 -24 -3 0 28.23 6.43 24 -3 0 17.18 6.27 -25 3 0 -5.89 4.37 -25 -3 0 5.38 2.97 25 3 0 -4.42 3.58 25 -3 0 1.64 2.07 25 -3 0 5.99 4.05 25 -3 0 4.38 2.1 -25 -3 0 -0.91 2.62 25 3 0 3.12 2 26 3 0 9.83 4.17 26 -3 0 10.16 5.38 26 -3 0 8.32 4.66 -26 3 0 11.97 5.42 -26 -3 0 9.57 4.64 26 3 0 9.89 4.31 26 -3 0 10.93 4.64 27 -3 0 14.24 5.54 27 3 0 12.17 5.58 27 3 0 11.08 5.14 27 -3 0 17.29 6.45 -27 3 0 17.46 6.6 27 -3 0 20.1 6.65 28 3 0 3.17 5.11 28 -3 0 0.68 2.83 28 -3 0 0.5 3.59 -28 3 0 -1.14 4.63 29 -3 0 0.66 3.91 29 3 0 4.61 4.59 30 -3 0 11.31 7.1 30 3 0 5.5 3.56 0 -4 0 184.86 9.13 0 4 0 190.04 9.22 0 -4 0 190.5 8.06 0 -4 0 184.96 5.93 0 4 0 180.99 5.74 -1 4 0 7.94 1.86 -1 -4 0 15.76 4.52 1 -4 0 8.17 1.4 1 -4 0 6.69 1.96 -1 -4 0 8.31 1.18 -1 4 0 6.19 0.91 1 -4 0 3.5 1.11 1 4 0 20.12 4.14 -1 -4 0 26.38 3.66 -2 4 0 944.34 17.75 -2 -4 0 1014.85 20.4 -2 -4 0 1012.27 25.38 2 4 0 1001.27 24.29 2 -4 0 1019.27 23.83 2 -4 0 1026.05 20.96 -2 4 0 1022.68 25.18 2 -4 0 936.44 23.66 2 4 0 985.85 19.84 2 4 0 816.55 16.29 3 -4 0 1150.74 24.46 -3 -4 0 1134.96 28.09 -3 -4 0 1169.75 21.71 3 -4 0 1120.34 21.01 -3 4 0 1151.53 28.23 3 4 0 1138.07 26.86 3 -4 0 1157.98 27.17 3 -4 0 1098.13 26.21 3 4 0 1123.06 23.23 3 4 0 979.27 18.75 4 4 0 283.91 10.06 -4 -4 0 280.54 12.58 4 4 0 281.48 11.63 4 -4 0 268.28 11.01 4 -4 0 288.05 10.9 4 -4 0 288.62 12.11 4 -4 0 296.62 8.73 -4 4 0 300.9 12.78 4 4 0 266.52 7.06 5 4 0 125.51 6.9 -5 4 0 123.06 8.22 5 4 0 114.87 7.27 5 -4 0 123.17 5.8 -5 -4 0 131.67 8.5 5 -4 0 122.82 7.16 5 -4 0 119.16 8.03 5 4 0 124.12 4.9 5 -4 0 118.44 7.32 6 -4 0 249.38 12.21 6 4 0 267.1 8.35 6 4 0 268.99 11.99 6 -4 0 250.57 10.78 6 4 0 272.78 11.09 6 -4 0 253.32 11.56 -6 4 0 281.02 12.96 6 -4 0 250.88 9.44 -6 4 0 260.79 11.2 -6 -4 0 258.65 12.51 -7 4 0 55.89 5.95 -7 4 0 54.21 4.8 7 -4 0 64.96 6.24 -7 -4 0 62.88 6.1 7 4 0 67.29 4.23 7 4 0 66.08 5.58 7 -4 0 62.66 4.68 7 4 0 46.9 2.35 7 4 0 60.9 5.69 7 -4 0 65.36 5.3 7 -4 0 55.32 5.72 8 -4 0 17.73 3.21 -8 4 0 19.27 3.07 8 4 0 18.03 2.47 8 -4 0 21.02 3.95 -8 -4 0 16.72 3.42 -8 4 0 18.16 3.72 8 4 0 12.99 1.19 8 4 0 21.57 3.36 8 4 0 19.12 3.25 8 -4 0 18.1 2.68 9 -4 0 37.55 4.11 9 4 0 33.35 4.59 9 -4 0 39.75 5.32 9 4 0 34.25 3.54 9 4 0 34.21 4.52 9 -4 0 33.03 4.87 -9 4 0 33.72 4 -9 -4 0 25.53 4.44 -9 4 0 30.13 4.64 9 4 0 19.07 1.62 10 -4 0 66.65 6.96 -10 4 0 63.72 5.61 -10 -4 0 67.4 6.96 10 -4 0 70.2 6.01 10 4 0 53.51 2.94 10 4 0 65.35 5.31 -10 -4 0 74.58 6.56 10 4 0 73.32 6.75 -10 4 0 64.84 6.99 10 4 0 73.1 6.64 10 -4 0 55.56 6.69 11 4 0 8.65 2.31 11 -4 0 6.07 2 -11 -4 0 9.49 2.82 11 4 0 7.89 1.93 -11 -4 0 7.7 2.59 11 -4 0 10.87 3.08 -11 4 0 7.49 2.68 -11 4 0 6.03 1.94 11 4 0 6.21 1.13 11 -4 0 5.91 2.87 -12 -4 0 191.84 11.67 12 4 0 221.91 13.17 -12 -4 0 196.15 12.77 -12 4 0 197.2 10.61 12 -4 0 193.52 11.38 12 -4 0 188.81 12.98 -12 4 0 193.95 13.07 12 -4 0 202.88 13.25 12 4 0 215.68 11.23 13 -4 0 8.39 3.34 13 4 0 22.99 3.96 -13 -4 0 19.6 3.84 -13 -4 0 27.01 4.36 13 -4 0 22.41 4.21 13 -4 0 23.98 4.8 -13 4 0 18.21 3.24 -13 4 0 21.08 4.65 13 4 0 24.47 4.59 -14 4 0 82.25 7.18 14 -4 0 85.22 9.17 -14 -4 0 74.47 7.65 14 4 0 95.15 9.23 14 4 0 96.41 7.97 14 -4 0 78.04 8.91 14 -4 0 86.24 8.23 -14 -4 0 97.34 9.5 -14 4 0 81.05 8.96 -15 -4 0 153.65 12.08 -15 4 0 139.11 11.86 -15 -4 0 124.32 10.35 15 -4 0 136.3 12.41 15 -4 0 147.82 12.39 15 -4 0 151.48 11.54 -15 4 0 128.1 9.14 15 4 0 152.25 10.7 15 4 0 145.14 11.85 -16 -4 0 121.94 10.64 -16 4 0 112.52 11.06 16 -4 0 121.05 11.37 16 -4 0 128.21 11.97 -16 4 0 114.65 8.86 16 4 0 119.89 11.23 16 4 0 138.03 10.49 -16 -4 0 129.8 11.6 16 -4 0 125.9 10.84 17 -4 0 95.15 9.65 17 -4 0 79.82 10.22 -17 -4 0 100.97 9.94 17 -4 0 83.48 9.82 -17 4 0 94.04 8.09 17 4 0 94.85 9.21 -17 -4 0 85.38 9.71 -17 4 0 81.12 9.41 17 4 0 93.68 10.37 -18 -4 0 1.09 1.68 18 -4 0 5.58 3.09 18 4 0 13.45 4.65 18 -4 0 6.96 3.11 -18 -4 0 10.1 3.05 -18 4 0 7 3.36 18 -4 0 7.07 3.24 -18 4 0 -0.09 1.59 18 4 0 10.78 3.47 19 -4 0 6.33 3.21 19 4 0 6.86 3.41 19 -4 0 4.59 2.78 -19 4 0 0.27 1.94 -19 -4 0 3.04 2.3 -19 4 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26 -4 0 -5.38 4.73 -26 4 0 0.54 3.28 26 4 0 1.01 2.99 27 4 0 -6.14 3.81 27 -4 0 -5.06 4.04 -27 4 0 0.11 2.6 27 -4 0 0.11 2.26 27 -4 0 1.11 3.75 -28 4 0 10.04 4.87 28 4 0 10.43 5.72 28 -4 0 0.13 3.33 29 -4 0 3.93 4.62 29 4 0 2.6 3.49 30 -4 0 1.85 3.53 0 -5 0 -0.28 0.74 0 -5 0 -0.14 0.35 0 -5 0 0.09 0.85 0 5 0 1.11 0.89 0 5 0 0.07 0.28 1 5 0 0.84 0.64 1 5 0 -0.03 0.94 -1 5 0 -2.77 1.35 1 -5 0 -0.31 0.54 -1 -5 0 0.01 0.33 1 -5 0 2 1.49 -1 -5 0 -0.98 1.09 -1 5 0 0.66 0.41 -1 -5 0 0.99 0.48 1 -5 0 1.37 1.02 2 -5 0 52.63 5.08 2 -5 0 55.9 5.4 -2 -5 0 54.78 5.62 2 5 0 41.07 2.24 -2 5 0 53.52 5.51 -2 5 0 55.08 2.94 2 5 0 60.84 3.83 -2 -5 0 53.39 4.1 2 5 0 55.37 5.41 2 -5 0 57.38 4.17 -3 -5 0 233.24 12.06 3 -5 0 225.92 9.12 -3 5 0 232.65 11.77 3 5 0 241.89 8.73 -3 -5 0 222.31 8.12 3 -5 0 222.3 11.03 3 5 0 156.89 4.8 -3 5 0 214.01 6.66 3 -5 0 231.4 11.1 3 5 0 231.03 11.25 -4 5 0 4 1.42 4 -5 0 6.59 1.93 4 5 0 5.43 0.84 -4 -5 0 7.18 1.84 4 -5 0 5.82 1.7 4 -5 0 7 1.23 4 5 0 7.3 1.91 -4 -5 0 6.1 1.16 4 -5 0 5.43 1.89 4 5 0 7.04 1.58 5 -5 0 291.73 13.82 5 -5 0 293.21 12.8 -5 5 0 290.57 14.22 5 -5 0 293.31 9.49 5 5 0 282.48 7.65 5 5 0 315 11.7 5 -5 0 301.24 12.33 -5 -5 0 309.21 14.66 5 5 0 294.02 13.25 6 5 0 453.73 11.39 -6 -5 0 492.49 19.24 6 -5 0 469.73 16.78 6 5 0 454.36 17.22 6 -5 0 492.38 17.04 6 -5 0 459.98 13.5 -6 5 0 475.2 19.07 6 -5 0 472.81 18.57 6 5 0 470.98 15.71 7 5 0 440.06 15.55 -7 5 0 463.9 18.94 -7 -5 0 448.24 18.38 7 -5 0 439.61 18.09 7 -5 0 444.89 16.71 7 5 0 450.36 11.65 7 -5 0 450.65 16.06 7 5 0 292.41 8.06 7 5 0 455.14 17.05 7 -5 0 436.04 13.4 8 5 0 44.18 3.62 8 5 0 40.9 4.97 8 5 0 44.87 5 8 -5 0 48.08 5.69 8 -5 0 42.77 5.58 -8 -5 0 35.07 5.24 8 -5 0 40.23 4.02 8 -5 0 46.47 4.98 -8 5 0 46.25 6 -9 5 0 83.75 6.95 9 -5 0 94.92 7.19 -9 5 0 93.25 8.64 9 5 0 105.38 8.06 -9 -5 0 80.25 8.03 9 -5 0 102.12 6.97 9 5 0 111.72 6.29 9 -5 0 96.12 8.28 9 5 0 82.68 7.68 9 -5 0 108.8 9.33 -10 5 0 227.25 14.23 -10 5 0 221.82 11.65 10 -5 0 234.68 11.31 10 -5 0 240.02 13.81 10 -5 0 216.76 11.47 10 5 0 238.04 12.85 10 5 0 193.09 9.4 10 -5 0 233.65 14.18 10 5 0 230.73 12.95 -10 -5 0 236.33 14 11 -5 0 13.39 3.13 -11 -5 0 12.13 3.43 -11 -5 0 9.25 2.57 11 5 0 8.71 2.46 11 5 0 13.7 2.58 11 -5 0 8.06 2.17 11 -5 0 7.32 2.98 11 5 0 8.37 2.52 -11 5 0 8.95 2.22 -11 5 0 16.54 3.72 -12 -5 0 289.45 16.72 12 5 0 339.91 13.83 -12 -5 0 308.27 16.09 -12 5 0 305.02 14.35 12 -5 0 332.58 15.02 12 5 0 311.86 16.04 12 -5 0 332.47 17.46 12 5 0 318.17 16.31 -12 5 0 307.59 17.58 12 -5 0 343.89 18.54 13 -5 0 -1.9 1.42 13 -5 0 1.86 1.28 -13 -5 0 -0.74 1.04 -13 5 0 0.17 1.96 13 5 0 1.02 1.13 13 -5 0 -1.09 0.95 -13 5 0 0.94 1.03 -13 -5 0 1.91 1.88 13 5 0 0.15 1.06 14 -5 0 294.77 17.55 -14 5 0 292.68 14.49 14 -5 0 313.84 18.24 14 5 0 291.96 16.91 -14 5 0 314.92 18.44 -14 -5 0 314.14 16.69 -14 -5 0 293.23 17.57 14 5 0 317.2 14.68 14 -5 0 305.81 15.8 -15 -5 0 1.51 1.73 15 5 0 2.4 1.95 15 5 0 1.32 1.19 15 -5 0 1.54 1.58 15 -5 0 4.23 2.57 -15 -5 0 0.85 2.02 -15 5 0 4.13 1.19 -15 5 0 -0.69 1.42 15 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84.34 8.35 8 6 0 85.71 7.12 8 -6 0 88.64 7.84 8 6 0 82.15 4.67 8 6 0 83.04 7.72 -8 6 0 82.78 8.6 -8 -6 0 96.28 9.04 -9 -6 0 14.51 3.54 9 -6 0 10.41 2.23 -9 6 0 10.84 3.06 9 -6 0 11.14 2.5 9 -6 0 13.07 3.5 9 6 0 12.88 3.02 9 6 0 11.54 1.93 9 -6 0 9.67 3.42 9 6 0 11.42 2.99 10 6 0 212.11 13.07 -10 6 0 212.63 14.64 -10 -6 0 226.09 14.64 10 6 0 217.39 12.58 10 -6 0 236.11 14.95 10 -6 0 205.02 11.76 10 6 0 206.02 9.09 10 -6 0 202.62 10.47 10 -6 0 209.1 13.35 11 6 0 -0.58 1.54 11 6 0 -0.44 0.72 -11 6 0 1.49 1.73 11 -6 0 0.81 0.79 11 6 0 1.21 1.4 -11 -6 0 -1.5 2.06 11 -6 0 2.45 2.08 11 -6 0 1.7 0.95 11 -6 0 -0.36 1.02 12 6 0 204.77 10.2 -12 6 0 207.16 14.71 -12 -6 0 193.36 14.29 -12 -6 0 198.27 13.23 12 -6 0 203.74 14.78 12 -6 0 187.78 11.79 -12 6 0 200.72 12.03 12 6 0 218.19 13.72 12 -6 0 194.93 13.73 12 -6 0 206.7 11.73 12 6 0 206.55 13.33 13 6 0 41.53 5.99 13 6 0 34.4 4.36 -13 6 0 35.4 5.03 13 -6 0 35.19 4.77 13 6 0 44.73 6.19 -13 -6 0 40.52 5.99 -13 -6 0 47.48 7.11 13 -6 0 40.57 5.22 -13 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56.46 7.37 0 5 10 68.36 9.81 0 5 10 54.89 8.88 1 -5 10 218.09 17.22 1 -5 10 216.02 15.96 1 5 10 209.86 18.29 1 5 10 222.4 18.29 -1 5 -10 209.32 18.64 -1 -5 -10 187.41 15.47 -1 5 -10 215.43 15.91 -2 5 -10 6.57 3.55 2 -5 10 13.23 4.42 2 -5 10 9.01 2.67 -2 5 -10 9.79 4.32 2 5 10 13.04 5.17 -2 -5 -10 11.22 4.59 2 5 10 12.75 4.68 3 -5 10 20.47 5.2 3 -5 10 32.27 6.47 -3 5 -10 13.12 4.13 3 5 10 24.39 6.14 -3 -5 -10 22.96 5.6 3 5 10 18.09 5.26 4 -5 10 76.13 10.59 4 -5 10 75.39 9.96 -4 5 -10 87.7 12.43 4 5 10 83.19 11.43 4 5 10 67.74 10.39 -4 -5 -10 83.89 11.25 5 -5 10 12.25 4.44 5 -5 10 11.37 3.99 -5 5 -10 9.78 4.41 5 5 10 11.36 4.53 5 5 10 4.84 3.06 -5 -5 -10 3.87 2.06 6 -5 10 139.58 14.95 6 -5 10 176.77 15.8 -6 5 -10 155.65 17.24 6 5 10 177.44 16.75 6 5 10 188.69 17.41 -6 -5 -10 149.59 15.8 7 -5 10 15.46 5.67 7 5 10 9.31 4.35 7 -5 10 20.04 5.8 -7 5 -10 14.82 4.82 7 5 10 12.53 4.95 7 5 10 19.77 5.52 -7 -5 -10 15.55 5.28 8 -5 10 36.44 7.74 8 5 10 31.15 7.57 8 -5 10 30.42 7.36 -8 5 -10 19.32 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5.1 0 0 14 0.84 2.63 1 0 14 65.7 11.73 1 0 14 67.06 12.93 1 0 14 61.65 11.53 2 0 14 0.24 3.11 2 0 14 1.22 3.1 3 0 14 7.6 4.92 3 0 14 0.49 2.55 4 0 14 10.56 6.58 4 0 14 1.24 2.54 5 0 14 14.5 6.6 5 0 14 7.26 4.61 6 0 14 26.22 7.71 6 0 14 26.42 8.6 -12 1 14 16.58 7.05 -11 1 14 -6.22 5.03 -11 1 14 -2.36 4.21 11 -1 -14 -2.28 4.67 -10 1 14 9.99 4.99 -10 1 14 15.16 5.77 10 -1 -14 5.73 5.64 -9 1 14 52.62 10.6 -9 1 14 43.4 10.92 9 -1 -14 65.06 12.81 -8 -1 14 7.29 4.92 -8 1 14 7.16 5.04 -8 1 14 -2.46 4.81 8 -1 -14 5.92 5.22 -7 -1 14 -1.06 2.7 -7 1 14 3.37 3.82 -7 1 14 -7.11 4.26 -6 -1 14 2.78 3.61 -6 -1 14 7.71 4.1 -6 1 14 6.22 4.64 -6 1 14 4.15 3.59 -5 -1 14 -0.34 3.62 -5 -1 14 6.18 4.71 -5 -1 14 2.71 4.74 -5 1 14 -2.52 2.92 -5 1 14 -0.49 3.53 -4 -1 14 1.92 2.45 -4 1 14 2.09 3.66 -4 -1 14 8.25 5.28 -4 1 14 5.72 4.7 -4 1 14 -1.83 2.57 -3 -1 14 3.99 2.8 -3 1 14 1.17 2.55 -3 -1 14 -1.16 2.44 -3 1 14 3.65 5.19 -3 1 14 0.11 2.69 -2 -1 14 3.92 4 -2 1 14 4.13 4.36 -2 -1 14 3.95 3.57 -2 1 14 5.1 5.63 -2 1 14 0.23 4.05 -1 -1 14 -0.47 2.77 -1 1 14 -2.5 4.35 -1 -1 14 -0.93 2.3 -1 1 14 -3.51 3.12 -1 1 14 2.85 3.36 0 -1 14 13.18 5.84 0 1 14 11.03 5.46 0 -1 14 5.88 4.31 0 1 14 14.47 6.76 0 1 14 6.07 4.69 1 -1 14 0.83 2.68 1 1 14 -4.35 4.01 1 -1 14 -1.19 4.48 1 1 14 -0.73 3.69 1 1 14 1.84 2.55 2 -1 14 5.43 4.28 2 -1 14 -1.92 2.78 2 1 14 -1.97 3.56 2 1 14 4.53 4.63 3 -1 14 3.67 4.55 3 1 14 -1.73 4.01 3 -1 14 3.87 4.76 3 1 14 -0.75 3.48 3 1 14 1.76 4.07 4 -1 14 19.75 6.58 4 1 14 15.98 6.17 4 -1 14 7.33 5.65 4 1 14 9.31 5.7 5 -1 14 6.81 5.3 5 1 14 -5.18 5.05 5 -1 14 0.62 4.4 5 1 14 -0.25 3.94 6 -1 14 0.64 4.06 6 1 14 0.26 3.08 6 1 14 9.76 5.93 -13 2 14 17.84 6.78 -12 2 14 5.44 3.87 -11 2 14 -7.36 6.1 -11 2 14 2.16 3.23 11 -2 -14 -0.14 3.48 -10 2 14 0.99 3.36 -10 2 14 -1.77 4.31 10 -2 -14 7.93 4.58 -9 2 14 10.35 4.95 -9 2 14 10.67 5.3 9 -2 -14 14.66 6.86 -8 2 14 -4.57 2.89 -8 2 14 -9 6.1 8 -2 -14 3.91 3.96 -7 2 14 1.31 3.33 -7 2 14 4.12 4.55 7 -2 -14 -1.48 2.58 -6 2 14 4.26 3.9 -6 2 14 -0.25 3.17 -5 2 14 4.71 4.07 -5 2 14 9.84 5.54 -4 2 14 -1.88 3.6 -4 2 14 1.49 4.17 -3 -2 14 31.15 8.09 -3 2 14 45.17 10.16 -3 2 14 38.89 10 -2 -2 14 -4.68 3.33 -2 2 14 -1.56 3.15 -2 2 14 -2.97 3.47 -2 2 14 -5.39 4.85 -1 -2 14 5.2 4.69 -1 2 14 1.21 3.19 -1 2 14 -0.37 3.28 -1 2 14 6.21 4.16 0 -2 14 -1.41 2.54 0 2 14 5.95 4.4 0 2 14 4.22 3.07 0 2 14 9.08 5.8 1 -2 14 1.78 4.26 1 2 14 -0.12 3.1 1 2 14 -0.62 3.9 1 2 14 1.54 2.82 2 -2 14 7.24 4.16 2 2 14 1.6 3.03 2 2 14 2.13 3.55 2 2 14 7.3 4.43 3 -2 14 5.39 5.02 3 2 14 14.2 7.13 3 2 14 13.39 5.95 3 2 14 11.46 6.11 4 -2 14 7.85 4.67 4 2 14 9.56 4.46 4 2 14 9.57 6.51 4 2 14 4.02 5.08 5 -2 14 -3.16 3.27 5 2 14 3.05 4.23 5 2 14 3.6 4.7 6 2 14 1.8 3.5 6 2 14 0.65 4.89 -12 3 14 -6.47 4.88 -11 3 14 11.86 5.69 11 -3 -14 10.93 6.73 -10 3 14 17.9 7.4 -10 3 14 21.85 7.46 10 -3 -14 9.14 5.31 -9 3 14 8.35 4.53 -9 3 14 3.59 4.99 9 -3 -14 -3.07 3.67 -8 3 14 12.93 6.29 -8 3 14 3.96 4.07 8 -3 -14 11.49 6.15 -7 3 14 -2.08 3.92 -7 3 14 1.41 3.54 7 -3 -14 3.44 3.32 -6 3 14 -2.19 3.35 -6 3 14 0.77 4.11 -5 3 14 5.21 3.82 -5 3 14 2.8 4.61 -4 3 14 13.43 6.62 -4 3 14 8 5.53 -3 3 14 6.4 2.99 -3 3 14 10.01 6.37 -2 3 14 2.17 3.58 -2 3 14 5.07 4.33 -1 3 14 0.13 3.72 -1 3 14 -3.38 3.2 0 3 14 0.86 3.37 0 3 14 6.43 3.96 0 3 14 -4.01 4.09 1 3 14 5.84 4.08 1 3 14 -1.27 3.67 1 3 14 0.37 4.72 2 3 14 -1 3.05 2 3 14 8.14 5.15 2 3 14 1.23 3.42 3 3 14 7.82 4.75 3 3 14 1.41 2.86 3 3 14 -1.86 3.76 4 3 14 -0.13 2.95 4 3 14 1.16 3.41 4 3 14 0.25 3.67 5 3 14 -0.78 3.21 -10 4 14 24.12 7.74 -10 4 14 11.66 6.14 10 -4 -14 21.82 7.6 -9 4 14 -5.11 3.03 -9 4 14 2.63 3.88 9 -4 -14 -3.44 4.85 -8 4 14 4.29 4.58 -8 4 14 -5.23 3.61 8 -4 -14 10.81 4.57 -7 4 14 4.77 3.62 -7 4 14 4.04 5.23 7 -4 -14 7.92 5.22 -6 4 14 67.07 12.41 -6 4 14 56.74 12.49 -5 4 14 15.85 6.32 -5 4 14 26.31 8.07 -4 4 14 -3.61 4.46 -4 4 14 -7.66 5.5 -3 4 14 -3.97 2.94 -3 4 14 -3.37 4.11 -2 4 14 -6.94 4.25 -2 4 14 1.55 3.9 -1 4 14 -0.5 3.87 -1 4 14 -0.52 4.25 0 4 14 -1.81 3.51 0 4 14 -3.51 3.39 1 4 14 5.81 4.01 1 4 14 -1.16 2.71 1 4 14 11.34 5.88 2 4 14 -6.1 3.02 2 4 14 -6.08 4.78 2 4 14 -5.33 3.74 3 4 14 38.5 10.01 -6 5 14 14.54 6.55 -5 5 14 2.95 3.97 -5 5 14 -1.87 5.25 -4 5 14 -0.9 4.24 -4 5 14 -4.91 4.69 -3 5 14 13.26 6.68 -3 5 14 14.83 6.88 -2 5 14 -1.02 3.58 -1 5 14 3.08 4.98 _iucr_refine_instructions_details ; amx-f13-et-100k.res created by SHELXL-2014/7 TITL amx-f13-et-100k_a.res in P2(1)/c REM Old TITL AMX-F13-ET-100K in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.185, Rweak 0.002, Alpha 0.010, Orientation as input REM Formula found by SHELXT: C21 N3 O5 F CELL 0.71073 20.5724 9.8586 9.7866 90 97.143 90 ZERR 4 0.0006 0.0003 0.0003 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O UNIT 84 80 4 12 20 L.S. 10 PLAN 20 BOND $H list 4 Htab fmap 2 acta 50 REM REM REM WGHT 0.101600 1.083800 FVAR 0.48775 O3 5 0.021556 1.048199 0.862265 11.00000 0.02462 0.03080 = 0.02286 0.00078 0.00332 0.00151 O1 5 0.373537 0.794501 0.968052 11.00000 0.02461 0.02902 = 0.02167 0.00101 0.00248 0.00235 O5 5 0.122797 0.973936 0.506394 11.00000 0.03419 0.02958 = 0.02976 0.00169 0.00986 0.00554 O4 5 0.100293 1.113408 0.328874 11.00000 0.04002 0.03813 = 0.02619 0.00107 0.00636 0.00288 O2 5 0.089893 0.949872 0.734774 11.00000 0.03654 0.03263 = 0.02706 0.00414 0.00627 0.01247 N2 4 0.240841 0.632163 0.666388 11.00000 0.01854 0.02077 = 0.02635 -0.00235 0.00149 0.00113 N3 4 0.113521 0.520280 0.582179 11.00000 0.01997 0.02504 = 0.02616 -0.00122 0.00229 -0.00123 AFIX 23 H3A 2 0.079766 0.506748 0.517430 11.00000 -1.20000 H3B 2 0.104575 0.480182 0.659154 11.00000 -1.20000 AFIX 0 N1 4 0.345554 0.582473 0.767000 11.00000 0.02099 0.02463 = 0.02424 0.00157 0.00213 0.00048 C4 1 0.285796 0.911071 0.638984 11.00000 0.02080 0.02384 = 0.02366 -0.00109 0.00253 0.00170 AFIX 43 H4 2 0.264285 0.876326 0.557255 11.00000 -1.20000 AFIX 0 C8 1 0.409565 0.617068 0.822878 11.00000 0.02053 0.02578 = 0.02457 0.00475 0.00253 0.00164 C1 1 0.301799 0.673147 0.732357 11.00000 0.02015 0.02221 = 0.02067 -0.00133 0.00407 -0.00085 C6 1 0.324415 1.105828 0.778466 11.00000 0.02753 0.02199 = 0.03000 -0.00264 0.00496 -0.00098 AFIX 43 H6 2 0.327611 1.199357 0.789744 11.00000 -1.20000 AFIX 0 C13 1 0.424611 0.719519 0.921528 11.00000 0.02284 0.02647 = 0.02244 0.00224 0.00228 0.00043 C21 1 0.047863 1.040545 0.754875 11.00000 0.02357 0.02303 = 0.02409 -0.00136 0.00232 0.00083 C3 1 0.344778 0.879127 0.864377 11.00000 0.02138 0.02534 = 0.02205 -0.00053 0.00423 -0.00007 C2 1 0.310734 0.823477 0.745606 11.00000 0.01883 0.02272 = 0.02537 -0.00207 0.00361 -0.00097 C7 1 0.350426 1.018590 0.883122 11.00000 0.02376 0.02605 = 0.02599 -0.00643 0.00431 -0.00065 AFIX 43 H7 2 0.371488 1.053478 0.965212 11.00000 -1.20000 AFIX 0 C17 1 0.232600 0.485165 0.643718 11.00000 0.02087 0.02040 = 0.02856 -0.00097 0.00159 0.00062 AFIX 23 H17A 2 0.226337 0.440876 0.729617 11.00000 -1.20000 H17B 2 0.271659 0.447811 0.611844 11.00000 -1.20000 AFIX 0 C19 1 0.048465 1.162245 0.522092 11.00000 0.02550 0.02449 = 0.02618 0.00102 0.00037 0.00124 AFIX 43 H19 2 0.031006 1.237782 0.473778 11.00000 -1.20000 AFIX 0 C5 1 0.293485 1.050146 0.656437 11.00000 0.02179 0.02170 = 0.02744 0.00108 0.00413 0.00190 C18 1 0.093370 1.078641 0.447170 11.00000 0.02528 0.02537 = 0.02463 -0.00281 0.00294 -0.00164 C14 1 0.181928 0.692469 0.713349 11.00000 0.01988 0.02520 = 0.02795 -0.00445 0.00428 0.00019 AFIX 23 H14A 2 0.188499 0.789101 0.727728 11.00000 -1.20000 H14B 2 0.174318 0.651985 0.800291 11.00000 -1.20000 AFIX 0 C20 1 0.029211 1.146874 0.646389 11.00000 0.02382 0.02495 = 0.02630 -0.00072 0.00177 0.00370 AFIX 43 H20 2 -0.000289 1.211820 0.669725 11.00000 -1.20000 AFIX 0 C15 1 0.122819 0.668732 0.606780 11.00000 0.01986 0.02448 = 0.03048 0.00024 0.00109 0.00092 AFIX 23 H15A 2 0.084016 0.706732 0.639154 11.00000 -1.20000 H15B 2 0.129309 0.713650 0.521338 11.00000 -1.20000 AFIX 0 C16 1 0.173867 0.459181 0.537612 11.00000 0.02313 0.02450 = 0.02589 -0.00359 0.00358 0.00033 AFIX 23 H16A 2 0.181660 0.497960 0.450019 11.00000 -1.20000 H16B 2 0.167701 0.362223 0.525109 11.00000 -1.20000 AFIX 0 C9 1 0.461414 0.538352 0.787578 11.00000 0.02386 0.02878 = 0.02613 0.00341 0.00311 0.00335 AFIX 43 H9 2 0.452853 0.468136 0.724443 11.00000 -1.20000 AFIX 0 C10 1 0.525386 0.562906 0.844863 11.00000 0.02175 0.03663 = 0.03252 0.00615 0.00472 0.00392 AFIX 43 H10 2 0.559250 0.509876 0.819256 11.00000 -1.20000 AFIX 0 C11 1 0.539115 0.666607 0.940536 11.00000 0.02121 0.03873 = 0.03087 0.00535 -0.00138 -0.00135 AFIX 43 H11 2 0.582117 0.683528 0.978131 11.00000 -1.20000 AFIX 0 C12 1 0.488140 0.745173 0.979919 11.00000 0.02422 0.03222 = 0.02715 0.00189 -0.00156 -0.00133 AFIX 43 H12 2 0.496797 0.813957 1.044657 11.00000 -1.20000 AFIX 0 CL1 3 0.265735 1.157506 0.520864 11.00000 0.03403 0.02244 = 0.03208 0.00297 0.00029 0.00302 H5 2 0.109377 0.973507 0.609419 11.00000 0.07622 HKLF 4 REM amx-f13-et-100k_a.res in P2(1)/c REM R1 = 0.0677 for 4998 Fo > 4sig(Fo) and 0.0997 for all 7218 data REM 275 parameters refined using 0 restraints END WGHT 0.1017 1.0819 REM Instructions for potential hydrogen bonds EQIV $1 x, -y+3/2, z-1/2 HTAB N3 O3_$1 EQIV $2 x, -y+3/2, z+1/2 HTAB N3 O4_$2 EQIV $3 x, -y+5/2, z-1/2 HTAB C19 O3_$3 HTAB C14 O2 HTAB C15 O2 HTAB C15 O5 EQIV $4 x, y-1, z HTAB C16 Cl1_$4 HTAB O5 O2 HTAB O2 O5 REM Highest difference peak 1.478, deepest hole -0.374, 1-sigma level 0.098 Q1 1 0.3009 0.9826 0.6448 11.00000 0.05 0.50 Q2 1 0.3070 0.7517 0.7356 11.00000 0.05 0.47 Q3 1 0.4176 0.6800 0.8619 11.00000 0.05 0.46 Q4 1 0.1211 0.5962 0.5953 11.00000 0.05 0.43 Q5 1 0.3492 0.9676 0.8746 11.00000 0.05 0.41 Q6 1 0.0476 1.0985 0.7074 11.00000 0.05 0.41 Q7 1 0.0998 1.1943 0.3262 11.00000 0.05 0.38 Q8 1 0.4346 0.5679 0.8228 11.00000 0.05 0.37 Q9 1 0.0543 0.9477 0.8325 11.00000 0.05 0.37 Q10 1 0.5129 0.6791 0.9751 11.00000 0.05 0.36 Q11 1 0.2606 0.5257 0.5257 11.00000 0.05 0.36 Q12 1 0.0195 0.8974 0.8597 11.00000 0.05 0.35 Q13 1 0.2010 1.1514 0.4543 11.00000 0.05 0.34 Q14 1 0.1477 0.6597 0.6697 11.00000 0.05 0.34 Q15 1 0.0677 1.1008 0.4776 11.00000 0.05 0.34 Q16 1 0.0784 1.1509 0.4901 11.00000 0.05 0.34 Q17 1 0.0871 1.0112 0.7474 11.00000 0.05 0.33 Q18 1 0.2028 0.4659 0.5977 11.00000 0.05 0.33 Q19 1 0.3339 1.0637 0.8415 11.00000 0.05 0.33 Q20 1 0.3415 0.8238 0.8245 11.00000 0.05 0.32 REM The information below was added by Olex2. REM REM R1 = 0.0677 for 4998 Fo > 4sig(Fo) and 0.0997 for all 44718 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.48, deepest hole -0.37 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0997 REM R1_gt = 0.0677 REM wR_ref = 0.1989 REM GOOF = 1.076 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 44718 REM Reflections_gt = 4998 REM Parameters = n/a REM Hole = -0.37 REM Peak = 1.48 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.095 _oxdiff_exptl_absorpt_empirical_full_min 0.923