data_burm002 _audit_creation_method SHELXL-2018/3 _shelx_SHELXL_version_number 2018/3 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C18 H22 N4 O3 S' _chemical_formula_sum 'C18 H22 N4 O3 S' _exptl_crystal_recrystallization_method ethanol _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 374.45 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 21/m' _space_group_name_Hall '-P 2yb' _chemical_absolute_configuration . loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _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. ; _cell_length_a 11.4315(3) _cell_length_b 6.6765(2) _cell_length_c 11.5969(3) _cell_angle_alpha 90 _cell_angle_beta 107.8509(5) _cell_angle_gamma 90 _cell_volume 842.49(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41475 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.30 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_F_000 396 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.245 _exptl_crystal_size_min 0.223 _exptl_absorpt_coefficient_mu 0.220 _shelx_estimated_absorpt_T_min 0.928 _shelx_estimated_absorpt_T_max 0.952 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8697 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details ; SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined by point group 2/m for scaling and error model Mean and maximum errors in direction cosine check function = 0.000 0.003 Restraint esd for equal adjacent scale factors = 0.0060 Maximum odd and even orders for spherical harmonics = 3 6 wR2(int) = 0.1284 (selected reflections only, before parameter refinement) wR2(int) = 0.0483 (selected reflections only, after parameter refinement) 66887 total and 2266 unique reflections assuming Friedel's law plus 3281 total and 1023 unique reflections in fast scans Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 66583 total and 2266 unique reflections left after |I-|/su test plus 3264 total and 1023 unique reflections in fast scans su^2 = [K*sigma(I)]^2 + [g]^2 where sigma(I) is from SAINT Error model 5: refine all K and overall g Run 2theta R(int) Incid. factors Diffr. factors K g I/s(lim) Total I>2sig(I) 1 29.6 0.0276 0.267 - 0.481 0.970 - 1.025 0.975 0.0253 39.5 4066 3610 2 29.6 0.0294 0.398 - 0.608 0.971 - 1.019 0.973 0.0253 39.5 4058 3547 3 29.6 0.0302 0.414 - 0.708 0.970 - 1.030 1.011 0.0253 39.5 4037 3474 4 29.6 0.0293 0.336 - 0.492 0.983 - 1.015 0.980 0.0253 39.5 4082 3612 5 14.6 0.0300 0.413 - 0.742 0.970 - 1.031 0.962 0.0253 39.5 4782 4179 6 29.6 0.0316 0.318 - 0.634 0.970 - 1.036 1.075 0.0253 39.5 6019 5316 7 29.6 0.0328 0.282 - 0.444 0.970 - 1.023 1.079 0.0253 39.5 6972 6224 8 68.3 0.0300 0.309 - 0.536 0.975 - 1.021 0.857 0.0253 39.5 2670 2395 9 68.3 0.0307 0.316 - 0.449 0.970 - 1.030 0.823 0.0253 39.5 2666 2406 10 68.3 0.0325 0.434 - 0.660 0.983 - 1.027 0.824 0.0253 39.5 2664 2404 11 68.3 0.0298 0.450 - 0.733 0.972 - 1.031 0.758 0.0253 39.5 2681 2440 12 68.3 0.0269 0.307 - 0.505 0.972 - 1.027 0.776 0.0253 39.5 2675 2449 13 68.3 0.0304 0.366 - 0.621 0.970 - 1.013 0.823 0.0253 39.5 2679 2431 14 68.3 0.0247 0.307 - 0.466 0.970 - 1.011 0.817 0.0253 39.5 2733 2580 15 53.3 0.0279 0.369 - 0.472 0.970 - 1.031 0.820 0.0253 39.5 3377 3119 16 53.3 0.0288 0.348 - 0.513 0.984 - 1.013 0.818 0.0253 39.5 2823 2616 17 0.0 0.0505 0.303 - 0.509 0.984 - 1.030 1.029 0.0253 39.5 4585 3547 18 0.0 0.0530 0.386 - 0.491 0.984 - 1.030 0.972 0.0253 39.5 3014 2305 19f 0.0 0.1326 3.764 - 4.799 0.970 - 1.015 0.957 0.0253 39.5 3264 1763 15 Overloads replaced by fast scan measurements 66598 Corrected reflections written to file hkl Estimated minimum and maximum transmission: 0.8697 0.9583 Additional spherical absorption correction applied with mu*r = 0.0300 3lambda correction factor = 0.00150 ; _exptl_absorpt_special_details ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus Mo X-ray tube' _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66553 _diffrn_reflns_av_unetI/netI 0.0098 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.845 _diffrn_reflns_theta_max 28.304 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2268 _reflns_number_gt 2195 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.3453P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2268 _refine_ls_number_parameters 198 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.11748(3) 0.250000 0.16989(3) 0.01499(10) Uani 1 2 d S T P . . O2 O 0.34840(10) 0.250000 0.61181(9) 0.0238(2) Uani 1 2 d S T P . . O5 O 0.84907(10) 0.250000 0.50665(11) 0.0293(3) Uani 1 2 d S T P . . O6 O 0.79572(10) 0.250000 0.74370(10) 0.0230(2) Uani 1 2 d S T P . . N1 N 0.35874(10) 0.250000 0.30851(10) 0.0146(2) Uani 1 2 d S T P . . N2 N 0.21887(10) 0.250000 0.41161(10) 0.0172(2) Uani 1 2 d S T P . . N3 N 0.59605(10) 0.250000 0.61213(10) 0.0155(2) Uani 1 2 d S T P . . N4 N 0.63594(10) 0.250000 0.43493(10) 0.0172(2) Uani 1 2 d S T P . . C1 C 0.24226(12) 0.250000 0.29968(12) 0.0139(2) Uani 1 2 d S T P . . C2 C 0.33113(12) 0.250000 0.50169(12) 0.0166(3) Uani 1 2 d S T P . . C3 C 0.41955(12) 0.250000 0.43302(12) 0.0139(2) Uani 1 2 d S T P . . C4 C 0.54281(12) 0.250000 0.48762(11) 0.0139(2) Uani 1 2 d S T P . . C5 C 0.74941(13) 0.250000 0.52257(13) 0.0196(3) Uani 1 2 d S T P . . C6 C 0.72209(12) 0.250000 0.64383(13) 0.0171(3) Uani 1 2 d S T P . . C11 C 0.18295(11) 0.250000 0.04309(11) 0.0133(2) Uani 1 2 d S T P . . C12 C 0.06737(12) 0.250000 -0.06854(12) 0.0167(3) Uani 1 2 d DS T P . . C13 C 0.25844(8) 0.43949(15) 0.04142(8) 0.01655(19) Uani 1 1 d D . . . . C14 C 0.10633(12) 0.250000 -0.18413(12) 0.0175(3) Uani 1 2 d DS T P . . C15 C 0.18319(9) 0.43690(16) -0.18616(9) 0.0193(2) Uani 1 1 d D . . . . C16 C 0.29791(9) 0.43739(15) -0.07429(8) 0.01809(19) Uani 1 1 d D . . . . C17 C 0.37502(12) 0.250000 -0.07526(13) 0.0200(3) Uani 1 2 d DS T P . . C20 C 0.09911(13) 0.250000 0.43272(14) 0.0244(3) Uani 1 2 d DS T P . . C40 C 0.61942(13) 0.250000 0.30498(13) 0.0225(3) Uani 1 2 d DS T P . . H3 H 0.5527(18) 0.250000 0.6615(18) 0.026(5) Uiso 1 2 d S . P . . H12 H 0.0188(10) 0.3695(13) -0.0668(11) 0.022(3) Uiso 1 1 d D . . . . H13A H 0.2096(10) 0.5590(13) 0.0422(11) 0.020(3) Uiso 1 1 d D . . . . H13B H 0.3311(8) 0.444(2) 0.1127(8) 0.021(3) Uiso 1 1 d D . . . . H14 H 0.0332(11) 0.250000 -0.2549(11) 0.024(5) Uiso 1 2 d DS . P . . H15A H 0.2076(11) 0.437(2) -0.2598(8) 0.022(3) Uiso 1 1 d D . . . . H15B H 0.1349(10) 0.5577(14) -0.1870(12) 0.024(3) Uiso 1 1 d D . . . . H16 H 0.3472(10) 0.5568(14) -0.0737(12) 0.022(3) Uiso 1 1 d D . . . . H17A H 0.4481(11) 0.250000 -0.0043(12) 0.027(5) Uiso 1 2 d DS . P . . H17B H 0.4054(16) 0.250000 -0.1453(11) 0.021(4) Uiso 1 2 d DS . P . . H20A H 0.114(2) 0.250000 0.5172(9) 0.039(6) Uiso 1 2 d DS . P . . H20B H 0.0541(12) 0.3643(18) 0.3972(13) 0.039(4) Uiso 1 1 d D . . . . H40A H 0.6986(11) 0.250000 0.2959(19) 0.033(5) Uiso 1 2 d DS . P . . H40B H 0.5747(11) 0.3651(17) 0.2699(12) 0.033(4) Uiso 1 1 d 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 S1 0.01077(16) 0.02193(18) 0.01161(16) 0.000 0.00247(11) 0.000 O2 0.0199(5) 0.0394(6) 0.0122(5) 0.000 0.0051(4) 0.000 O5 0.0137(5) 0.0460(7) 0.0282(6) 0.000 0.0061(4) 0.000 O6 0.0185(5) 0.0272(5) 0.0179(5) 0.000 -0.0025(4) 0.000 N1 0.0125(5) 0.0181(5) 0.0121(5) 0.000 0.0023(4) 0.000 N2 0.0137(5) 0.0264(6) 0.0117(5) 0.000 0.0043(4) 0.000 N3 0.0140(5) 0.0188(5) 0.0122(5) 0.000 0.0021(4) 0.000 N4 0.0130(5) 0.0246(6) 0.0139(5) 0.000 0.0037(4) 0.000 C1 0.0145(6) 0.0157(6) 0.0114(5) 0.000 0.0041(4) 0.000 C2 0.0155(6) 0.0201(6) 0.0141(6) 0.000 0.0041(5) 0.000 C3 0.0143(6) 0.0152(6) 0.0119(5) 0.000 0.0038(5) 0.000 C4 0.0153(6) 0.0131(5) 0.0127(6) 0.000 0.0035(5) 0.000 C5 0.0147(6) 0.0229(7) 0.0191(6) 0.000 0.0021(5) 0.000 C6 0.0160(6) 0.0152(6) 0.0178(6) 0.000 0.0018(5) 0.000 C11 0.0118(5) 0.0173(6) 0.0108(5) 0.000 0.0033(4) 0.000 C12 0.0115(5) 0.0251(7) 0.0124(6) 0.000 0.0022(4) 0.000 C13 0.0179(4) 0.0173(4) 0.0145(4) -0.0010(3) 0.0049(3) -0.0028(3) C14 0.0131(6) 0.0267(7) 0.0114(5) 0.000 0.0019(4) 0.000 C15 0.0205(4) 0.0229(5) 0.0144(4) 0.0041(3) 0.0052(3) 0.0021(4) C16 0.0181(4) 0.0210(4) 0.0155(4) 0.0003(3) 0.0056(3) -0.0048(4) C17 0.0127(6) 0.0319(8) 0.0156(6) 0.000 0.0046(5) 0.000 C20 0.0135(6) 0.0436(9) 0.0174(6) 0.000 0.0063(5) 0.000 C40 0.0183(6) 0.0357(8) 0.0143(6) 0.000 0.0064(5) 0.000 _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 S1 C1 1.7274(13) . ? S1 C11 1.8432(13) . ? O2 C2 1.2309(17) . ? O5 C5 1.2087(18) . ? O6 C6 1.2051(17) . ? N1 C1 1.3038(17) . ? N1 C3 1.3975(16) . ? N2 C2 1.3843(17) . ? N2 C1 1.4032(16) . ? N2 C20 1.4628(17) . ? N3 C6 1.3734(17) . ? N3 C4 1.3844(16) . ? N3 H3 0.86(2) . ? N4 C4 1.3804(16) . ? N4 C5 1.3810(17) . ? N4 C40 1.4603(17) . ? C2 C3 1.4660(18) . ? C3 C4 1.3563(18) . ? C5 C6 1.531(2) . ? C11 C13 1.5348(11) 4_565 ? C11 C13 1.5349(11) . ? C11 C12 1.5405(17) . ? C12 C14 1.5367(18) . ? C12 H12 0.976(6) . ? C12 H12 0.976(6) 4_565 ? C13 C16 1.5413(12) . ? C13 H13A 0.976(6) . ? C13 H13B 0.976(6) . ? C14 C15 1.5305(13) . ? C14 C15 1.5305(13) 4_565 ? C14 H14 0.976(6) . ? C15 C16 1.5362(13) . ? C15 H15A 0.976(6) . ? C15 H15B 0.976(6) . ? C16 C17 1.5325(13) . ? C16 H16 0.975(6) . ? C17 H17A 0.976(6) . ? C17 H17B 0.976(6) . ? C20 H20A 0.942(9) . ? C20 H20B 0.942(9) . ? C20 H20B 0.942(9) 4_565 ? C40 H40A 0.943(9) . ? C40 H40B 0.943(9) . ? C40 H40B 0.943(9) 4_565 ? 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 C1 S1 C11 105.45(6) . . ? C1 N1 C3 104.70(11) . . ? C2 N2 C1 107.62(11) . . ? C2 N2 C20 124.92(11) . . ? C1 N2 C20 127.46(11) . . ? C6 N3 C4 111.64(11) . . ? C6 N3 H3 126.1(13) . . ? C4 N3 H3 122.2(13) . . ? C4 N4 C5 110.61(11) . . ? C4 N4 C40 125.70(11) . . ? C5 N4 C40 123.69(12) . . ? N1 C1 N2 114.01(11) . . ? N1 C1 S1 128.25(10) . . ? N2 C1 S1 117.74(10) . . ? O2 C2 N2 126.85(13) . . ? O2 C2 C3 130.21(13) . . ? N2 C2 C3 102.95(11) . . ? C4 C3 N1 126.79(12) . . ? C4 C3 C2 122.48(12) . . ? N1 C3 C2 110.72(11) . . ? C3 C4 N4 128.70(12) . . ? C3 C4 N3 123.27(12) . . ? N4 C4 N3 108.03(11) . . ? O5 C5 N4 127.17(14) . . ? O5 C5 C6 127.41(13) . . ? N4 C5 C6 105.42(11) . . ? O6 C6 N3 128.58(13) . . ? O6 C6 C5 127.13(13) . . ? N3 C6 C5 104.29(11) . . ? C13 C11 C13 111.02(10) 4_565 . ? C13 C11 C12 109.27(7) 4_565 . ? C13 C11 C12 109.27(7) . . ? C13 C11 S1 112.18(6) 4_565 . ? C13 C11 S1 112.18(6) . . ? C12 C11 S1 102.54(8) . . ? C14 C12 C11 109.26(10) . . ? C14 C12 H12 109.7(8) . . ? C11 C12 H12 109.3(8) . . ? C14 C12 H12 109.7(8) . 4_565 ? C11 C12 H12 109.3(8) . 4_565 ? H12 C12 H12 109.7(15) . 4_565 ? C11 C13 C16 108.62(8) . . ? C11 C13 H13A 110.4(7) . . ? C16 C13 H13A 109.7(7) . . ? C11 C13 H13B 110.3(8) . . ? C16 C13 H13B 109.7(7) . . ? H13A C13 H13B 108.0(10) . . ? C15 C14 C15 109.24(11) . 4_565 ? C15 C14 C12 109.55(7) . . ? C15 C14 C12 109.55(7) 4_565 . ? C15 C14 H14 109.6(6) . . ? C15 C14 H14 109.6(6) 4_565 . ? C12 C14 H14 109.3(11) . . ? C14 C15 C16 109.53(8) . . ? C14 C15 H15A 109.4(8) . . ? C16 C15 H15A 109.9(7) . . ? C14 C15 H15B 110.4(8) . . ? C16 C15 H15B 109.9(8) . . ? H15A C15 H15B 107.8(11) . . ? C17 C16 C15 109.64(9) . . ? C17 C16 C13 109.65(9) . . ? C15 C16 C13 109.47(7) . . ? C17 C16 H16 109.6(8) . . ? C15 C16 H16 110.4(8) . . ? C13 C16 H16 108.0(8) . . ? C16 C17 C16 109.46(11) 4_565 . ? C16 C17 H17A 109.8(6) 4_565 . ? C16 C17 H17A 109.8(6) . . ? C16 C17 H17B 111.0(5) 4_565 . ? C16 C17 H17B 111.0(5) . . ? H17A C17 H17B 105.7(16) . . ? N2 C20 H20A 107.2(14) . . ? N2 C20 H20B 109.9(9) . . ? H20A C20 H20B 110.8(11) . . ? N2 C20 H20B 109.9(9) . 4_565 ? H20A C20 H20B 110.8(11) . 4_565 ? H20B C20 H20B 108.2(19) . 4_565 ? N4 C40 H40A 106.9(13) . . ? N4 C40 H40B 109.1(9) . . ? H40A C40 H40B 111.3(11) . . ? N4 C40 H40B 109.1(9) . 4_565 ? H40A C40 H40B 111.3(11) . 4_565 ? H40B C40 H40B 109.1(17) . 4_565 ? 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 C3 N1 C1 N2 0.000(0) . . . . ? C3 N1 C1 S1 180.000(0) . . . . ? C2 N2 C1 N1 0.000(0) . . . . ? C20 N2 C1 N1 180.000(0) . . . . ? C2 N2 C1 S1 180.000(0) . . . . ? C20 N2 C1 S1 0.000(0) . . . . ? C11 S1 C1 N1 0.000(0) . . . . ? C11 S1 C1 N2 180.000(0) . . . . ? C1 N2 C2 O2 180.000(0) . . . . ? C20 N2 C2 O2 0.000(0) . . . . ? C1 N2 C2 C3 0.000(0) . . . . ? C20 N2 C2 C3 180.000(0) . . . . ? C1 N1 C3 C4 180.000(0) . . . . ? C1 N1 C3 C2 0.000(0) . . . . ? O2 C2 C3 C4 0.000(1) . . . . ? N2 C2 C3 C4 180.000(0) . . . . ? O2 C2 C3 N1 180.000(0) . . . . ? N2 C2 C3 N1 0.000(0) . . . . ? N1 C3 C4 N4 0.000(0) . . . . ? C2 C3 C4 N4 180.000(0) . . . . ? N1 C3 C4 N3 180.000(0) . . . . ? C2 C3 C4 N3 0.000(0) . . . . ? C5 N4 C4 C3 180.000(0) . . . . ? C40 N4 C4 C3 0.000(0) . . . . ? C5 N4 C4 N3 0.000(0) . . . . ? C40 N4 C4 N3 180.000(0) . . . . ? C6 N3 C4 C3 180.000(0) . . . . ? C6 N3 C4 N4 0.000(0) . . . . ? C4 N4 C5 O5 180.000(0) . . . . ? C40 N4 C5 O5 0.000(0) . . . . ? C4 N4 C5 C6 0.000(0) . . . . ? C40 N4 C5 C6 180.000(0) . . . . ? C4 N3 C6 O6 180.000(0) . . . . ? C4 N3 C6 C5 0.000(0) . . . . ? O5 C5 C6 O6 0.000(1) . . . . ? N4 C5 C6 O6 180.000(0) . . . . ? O5 C5 C6 N3 180.000(0) . . . . ? N4 C5 C6 N3 0.000(0) . . . . ? C1 S1 C11 C13 62.88(7) . . . 4_565 ? C1 S1 C11 C13 -62.88(7) . . . . ? C1 S1 C11 C12 180.0 . . . . ? C13 C11 C12 C14 -60.83(7) 4_565 . . . ? C13 C11 C12 C14 60.83(7) . . . . ? S1 C11 C12 C14 180.000(0) . . . . ? C13 C11 C13 C16 59.51(12) 4_565 . . . ? C12 C11 C13 C16 -61.09(10) . . . . ? S1 C11 C13 C16 -174.09(7) . . . . ? C11 C12 C14 C15 -59.91(7) . . . . ? C11 C12 C14 C15 59.91(7) . . . 4_565 ? C15 C14 C15 C16 -60.30(12) 4_565 . . . ? C12 C14 C15 C16 59.72(11) . . . . ? C14 C15 C16 C17 60.01(10) . . . . ? C14 C15 C16 C13 -60.32(11) . . . . ? C11 C13 C16 C17 -59.47(10) . . . . ? C11 C13 C16 C15 60.85(10) . . . . ? C15 C16 C17 C16 -59.44(12) . . . 4_565 ? C13 C16 C17 C16 60.78(12) . . . 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N3 H3 O2 0.86(2) 2.23(2) 2.8299(15) 126.6(17) . yes _refine_diff_density_max 0.407 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.045 _shelx_res_file ; TITL burm002 in P2(1)/m shelx.res created by SHELXL-2018/3 at 13:38:19 on 07-Jan-2023 CELL 0.71073 11.43150 6.67650 11.59690 90.0000 107.8509 90.0000 ZERR 2.00 0.00030 0.00020 0.00030 0.0000 0.0005 0.0000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H N O S UNIT 36 44 8 6 2 MERG 2 SADI 0.005 C20 H20A C20 H20B C40 H40A C40 H40B SADI 0.005 C12 H12 C13 H13A C13 H13B C14 H14 C15 H15A C15 H15B = C16 H16 C17 H17A C17 H17B MORE -1 FMAP 2 PLAN 30 SIZE 0.223 0.245 0.345 ACTA HTAB N3 O2 BOND $H CONF LIST 4 L.S. 20 TEMP -173.15 WGHT 0.045300 0.345300 FVAR 0.93389 S1 5 0.117478 0.250000 0.169893 10.50000 0.01077 0.02193 = 0.01161 0.00000 0.00247 0.00000 O2 4 0.348400 0.250000 0.611813 10.50000 0.01989 0.03944 = 0.01223 0.00000 0.00508 0.00000 O5 4 0.849066 0.250000 0.506651 10.50000 0.01367 0.04602 = 0.02815 0.00000 0.00614 0.00000 O6 4 0.795718 0.250000 0.743700 10.50000 0.01849 0.02725 = 0.01791 0.00000 -0.00251 0.00000 N1 3 0.358736 0.250000 0.308509 10.50000 0.01249 0.01809 = 0.01208 0.00000 0.00229 0.00000 N2 3 0.218874 0.250000 0.411607 10.50000 0.01370 0.02637 = 0.01168 0.00000 0.00429 0.00000 N3 3 0.596048 0.250000 0.612130 10.50000 0.01405 0.01878 = 0.01219 0.00000 0.00205 0.00000 N4 3 0.635944 0.250000 0.434934 10.50000 0.01301 0.02455 = 0.01388 0.00000 0.00374 0.00000 C1 1 0.242259 0.250000 0.299681 10.50000 0.01453 0.01565 = 0.01144 0.00000 0.00406 0.00000 C2 1 0.331134 0.250000 0.501695 10.50000 0.01545 0.02010 = 0.01406 0.00000 0.00406 0.00000 C3 1 0.419548 0.250000 0.433024 10.50000 0.01426 0.01523 = 0.01191 0.00000 0.00377 0.00000 C4 1 0.542814 0.250000 0.487623 10.50000 0.01526 0.01314 = 0.01273 0.00000 0.00347 0.00000 C5 1 0.749410 0.250000 0.522573 10.50000 0.01467 0.02294 = 0.01905 0.00000 0.00212 0.00000 C6 1 0.722086 0.250000 0.643829 10.50000 0.01605 0.01516 = 0.01784 0.00000 0.00176 0.00000 C11 1 0.182950 0.250000 0.043093 10.50000 0.01176 0.01730 = 0.01080 0.00000 0.00327 0.00000 C12 1 0.067367 0.250000 -0.068544 10.50000 0.01155 0.02513 = 0.01238 0.00000 0.00215 0.00000 C13 1 0.258442 0.439486 0.041418 11.00000 0.01788 0.01727 = 0.01447 -0.00096 0.00491 -0.00282 C14 1 0.106331 0.250000 -0.184134 10.50000 0.01310 0.02665 = 0.01139 0.00000 0.00188 0.00000 C15 1 0.183190 0.436903 -0.186162 11.00000 0.02047 0.02292 = 0.01436 0.00406 0.00517 0.00208 C16 1 0.297911 0.437394 -0.074293 11.00000 0.01808 0.02102 = 0.01548 0.00027 0.00559 -0.00482 C17 1 0.375019 0.250000 -0.075261 10.50000 0.01271 0.03191 = 0.01559 0.00000 0.00463 0.00000 C20 1 0.099109 0.250000 0.432715 10.50000 0.01345 0.04356 = 0.01735 0.00000 0.00634 0.00000 C40 1 0.619421 0.250000 0.304977 10.50000 0.01831 0.03575 = 0.01428 0.00000 0.00643 0.00000 H3 2 0.552740 0.250000 0.661542 10.50000 0.02555 H12 2 0.018768 0.369515 -0.066822 11.00000 0.02241 H13A 2 0.209556 0.559048 0.042239 11.00000 0.01992 H13B 2 0.331073 0.443548 0.112729 11.00000 0.02086 H14 2 0.033191 0.250000 -0.254920 10.50000 0.02407 H15A 2 0.207607 0.436768 -0.259789 11.00000 0.02187 H15B 2 0.134852 0.557714 -0.186953 11.00000 0.02354 H16 2 0.347182 0.556807 -0.073721 11.00000 0.02164 H17A 2 0.448113 0.250000 -0.004335 10.50000 0.02693 H17B 2 0.405369 0.250000 -0.145316 10.50000 0.02127 H20A 2 0.113930 0.250000 0.517219 10.50000 0.03902 H20B 2 0.054093 0.364265 0.397161 11.00000 0.03927 H40A 2 0.698620 0.250000 0.295909 10.50000 0.03299 H40B 2 0.574744 0.365099 0.269867 11.00000 0.03287 HKLF 4 REM burm002 in P2(1)/m REM wR2 = 0.0800, GooF = S = 1.045, Restrained GooF = 1.034 for all data REM R1 = 0.0284 for 2195 Fo > 4sig(Fo) and 0.0292 for all 2268 data REM 198 parameters refined using 42 restraints END WGHT 0.0453 0.3453 REM Highest difference peak 0.407, deepest hole -0.215, 1-sigma level 0.045 Q1 1 0.3799 0.2500 0.4690 10.50000 0.05 0.41 Q2 1 0.7381 0.2500 0.5855 10.50000 0.05 0.37 Q3 1 0.1243 0.2500 -0.0153 10.50000 0.05 0.37 Q4 1 0.2215 0.3456 0.0413 11.00000 0.05 0.37 Q5 1 0.1489 0.3421 -0.1845 11.00000 0.05 0.36 Q6 1 0.2446 0.4337 -0.1287 11.00000 0.05 0.36 Q7 1 0.2789 0.4366 -0.0182 11.00000 0.05 0.35 Q8 1 0.0971 0.2500 -0.1238 10.50000 0.05 0.35 Q9 1 0.2284 0.2500 0.3529 10.50000 0.05 0.35 Q10 1 0.3357 0.3474 -0.0735 11.00000 0.05 0.33 Q11 1 0.4804 0.2500 0.4581 10.50000 0.05 0.33 Q12 1 0.6986 0.2500 0.4780 10.50000 0.05 0.29 Q13 1 0.2707 0.2500 0.4623 10.50000 0.05 0.29 Q14 1 0.1912 0.2500 0.2402 10.50000 0.05 0.29 Q15 1 0.6546 0.2500 0.6293 10.50000 0.05 0.26 Q16 1 0.5919 0.2500 0.4581 10.50000 0.05 0.26 Q17 1 0.1551 0.2500 0.1061 10.50000 0.05 0.26 Q18 1 0.3068 0.2500 0.2977 10.50000 0.05 0.26 Q19 1 0.6272 0.2500 0.3707 10.50000 0.05 0.26 Q20 1 0.3996 0.2500 0.3735 10.50000 0.05 0.25 Q21 1 0.5747 0.2500 0.5567 10.50000 0.05 0.24 Q22 1 0.1641 0.2500 0.4203 10.50000 0.05 0.22 Q23 1 0.0977 0.1117 0.1691 11.00000 0.05 0.16 Q24 1 0.3904 0.2500 0.2627 10.50000 0.05 0.14 Q25 1 0.4023 0.2500 -0.0476 10.50000 0.05 0.14 Q26 1 0.3806 0.1948 0.2790 11.00000 0.05 0.14 Q27 1 0.1086 0.1558 0.4970 11.00000 0.05 0.12 Q28 1 0.0451 0.2500 0.3749 10.50000 0.05 0.12 Q29 1 0.0365 0.2500 0.1767 10.50000 0.05 0.11 Q30 1 0.7559 0.1952 0.6895 11.00000 0.05 0.11 ; _shelx_res_checksum 68979 _shelx_hkl_file ; 1 0 0 37.9687 2.20070 17 1 0 0 37.1477 1.19019 1 -1 0 0 37.4178 1.29391 6 -1 0 0 36.4233 1.18817 4 -1 0 0 39.6972 1.18100 4 -1 0 0 36.3444 1.29144 2 -2 0 0 7996.02 232.936 19 2 0 0 8005.88 233.480 19 -3 0 0 3.93295 0.71237 2 -3 0 0 3.22360 0.46329 4 3 0 0 2.10465 0.54296 6 3 0 0 4.16670 0.54992 4 -3 0 0 3.60026 0.66387 6 3 0 0 3.10616 0.50217 1 -3 0 0 3.35616 0.66674 3 -3 0 0 4.01631 0.61280 1 3 0 0 2.69008 0.57431 6 -3 0 0 2.01708 0.50489 5 3 0 0 2.98879 0.64387 7 3 0 0 2.03781 0.51104 3 -3 0 0 4.55919 1.71970 17 3 0 0 8.14597 2.21816 17 -3 0 0 3.16260 0.59801 6 -3 0 0 3.83067 0.70236 7 3 0 0 3.48039 0.72287 7 3 0 0 4.66808 0.72215 5 -3 0 0 3.37127 0.52063 4 -4 0 0 2117.63 53.5206 1 -4 0 0 2097.83 53.4071 4 4 0 0 1999.25 53.4971 1 4 0 0 2076.83 54.1627 5 -4 0 0 2128.01 59.8168 17 4 0 0 2113.69 54.3517 6 4 0 0 1963.30 54.2376 7 -4 0 0 1937.46 53.5113 4 -4 0 0 2097.53 54.2030 2 -4 0 0 2158.32 54.3234 5 4 0 0 2217.42 54.3207 7 -4 0 0 2078.35 54.2837 6 -4 0 0 2111.32 54.2725 3 4 0 0 1932.57 53.4076 4 -4 0 0 1912.77 54.1409 7 4 0 0 2200.74 60.6047 17 -5 0 0 51.5543 2.30905 1 -5 0 0 53.7663 5.69753 17 5 0 0 54.9321 2.88635 7 5 0 0 50.0335 6.08979 17 -5 0 0 50.9092 2.82932 2 -5 0 0 50.8118 2.85190 7 -5 0 0 52.2287 2.89781 3 5 0 0 52.5204 2.83371 5 -5 0 0 52.6754 2.28977 4 5 0 0 52.8687 2.98656 6 -5 0 0 55.3083 2.99397 5 -5 0 0 48.9897 2.86685 6 -6 0 0 112.235 5.46339 2 -6 0 0 112.974 4.10526 4 -6 0 0 112.434 5.03157 6 -6 0 0 110.187 4.15181 1 -6 0 0 114.624 3.22793 16 6 0 0 107.851 9.63951 17 -6 0 0 120.858 5.11581 5 -6 0 0 115.264 5.03064 3 -6 0 0 117.736 5.02728 7 6 0 0 114.120 4.97724 5 6 0 0 113.205 4.90380 7 6 0 0 119.022 5.11587 6 -6 0 0 103.747 8.48611 17 -6 0 0 116.628 3.45101 15 -7 0 0 76.4028 2.53313 15 -7 0 0 75.0827 4.10144 7 7 0 0 75.5687 4.01948 7 -7 0 0 73.0652 4.05613 2 -7 0 0 70.2579 4.16236 6 7 0 0 80.0923 9.48447 17 -7 0 0 80.3046 4.28353 5 -7 0 0 74.7703 4.14389 3 -7 0 0 79.3124 3.26311 4 7 0 0 68.3499 4.05277 6 -7 0 0 74.6795 8.06587 17 -7 0 0 75.9819 2.39405 16 -7 0 0 79.8708 3.33231 1 7 0 0 66.8389 3.87152 5 -8 0 0 293.625 10.4937 3 8 0 0 300.784 18.9429 17 8 0 0 274.695 8.67706 1 -8 0 0 287.495 7.66361 16 -8 0 0 287.458 8.97632 4 8 0 0 276.809 10.3836 6 -8 0 0 290.856 8.01687 15 -8 0 0 281.606 10.4601 2 -8 0 0 268.767 16.4723 17 -8 0 0 293.552 10.6034 5 -8 0 0 290.228 9.03287 1 8 0 0 270.438 10.0648 7 -8 0 0 272.661 8.59149 10 -8 0 0 297.200 10.5135 7 -8 0 0 288.620 10.6686 6 -9 0 0 75.7472 3.58084 4 -9 0 0 75.8024 3.36518 10 9 0 0 81.7469 12.5820 17 -9 0 0 77.7605 4.77539 3 9 0 0 82.6228 4.67748 7 -9 0 0 79.1457 5.06099 6 -9 0 0 77.1968 2.46094 16 -9 0 0 76.9572 2.73813 11 -9 0 0 75.6763 3.58223 1 -9 0 0 87.3024 10.4536 17 9 0 0 81.6462 2.68032 13 -9 0 0 76.7290 4.84442 5 -9 0 0 73.4531 4.74087 2 -9 0 0 75.3933 2.89810 15 9 0 0 88.0860 5.06296 6 9 0 0 80.0732 3.45665 1 -9 0 0 80.0664 4.79787 7 10 0 0 8.71709 0.98954 13 -10 0 0 8.90460 2.10497 2 -10 0 0 9.50330 1.35508 10 -10 0 0 5.83084 1.82856 6 -10 0 0 8.08085 1.33865 1 -10 0 0 6.68990 0.57824 16 10 0 0 7.84188 1.25470 1 -10 0 0 -0.9529 5.43495 17 10 0 0 3.40865 6.71768 17 -10 0 0 7.99578 0.82818 8 10 0 0 10.9566 2.37649 6 -10 0 0 6.90194 1.28991 4 -10 0 0 7.56881 0.88410 15 -10 0 0 10.1909 1.03048 11 -10 0 0 11.3819 2.33286 5 10 0 0 8.89772 0.93731 8 10 0 0 9.24405 2.07368 7 -10 0 0 7.42987 1.85052 3 -11 0 0 113.166 8.17637 3 -11 0 0 115.684 3.46355 16 -11 0 0 111.171 3.93700 9 -11 0 0 122.251 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351.114 12.5068 3 9 -2 0 337.465 11.5016 1 9 -2 0 361.424 9.58104 14 -9 -2 0 364.140 10.7262 10 9 -2 0 343.643 21.7017 17 -9 -2 0 355.206 11.9337 4 -9 -2 0 356.037 12.8736 7 -9 -2 0 351.636 12.9787 6 9 -2 0 366.613 10.3434 8 -9 -2 0 352.449 12.9136 2 9 -2 0 344.418 12.4279 7 -9 -2 0 365.673 10.0211 14 -9 -2 0 357.806 9.78467 11 -9 -2 0 342.743 12.6983 5 -9 -2 0 353.249 20.3619 17 -9 2 0 304.321 18.7905 17 -9 2 0 364.023 10.8100 9 -9 2 0 368.355 12.2092 1 -9 2 0 368.563 10.0305 15 -9 2 0 366.333 13.4679 5 -9 2 0 358.530 10.2348 8 -9 2 0 344.688 10.8196 10 -9 2 0 355.599 13.0478 6 -9 2 0 345.969 10.3393 4 9 2 0 355.242 9.94192 13 9 2 0 374.117 13.2987 6 -9 2 0 345.710 13.3147 3 9 2 0 343.986 13.8692 7 -9 2 0 356.590 10.0032 11 -9 2 0 334.139 9.28825 16 -9 2 0 345.128 13.3228 2 -9 2 0 354.450 9.83599 12 -10 -2 0 3.33354 1.51144 7 10 -2 0 3.14929 0.50331 14 -10 -2 0 3.56482 0.59771 16 -10 -2 0 2.90952 0.53085 14 -10 -2 0 4.50904 0.69379 11 10 -2 0 3.01308 1.46059 7 -10 -2 0 0.93979 1.28487 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22.3745 7 1 -5 0 854.315 22.0111 7 -1 5 0 886.135 24.2792 9 -1 5 0 837.760 24.9082 2 1 5 0 855.352 24.8941 2 1 5 0 874.767 26.3891 3 -1 5 0 825.511 26.3553 5 1 5 0 833.057 23.7401 1 -1 5 0 841.512 24.6418 4 1 5 0 841.748 25.0798 4 -1 5 0 830.314 26.9268 3 -1 5 0 841.644 24.3912 1 -1 5 0 828.241 22.6223 11 -2 -5 0 171.805 5.98294 1 -2 -5 0 174.275 7.18731 2 -2 -5 0 178.830 5.81815 7 -2 -5 0 180.607 7.20711 3 -2 -5 0 179.255 7.06690 5 -2 -5 0 184.312 6.23736 18 -2 -5 0 178.845 5.98211 17 2 -5 0 182.300 5.32592 7 2 -5 0 185.219 5.52433 7 -2 -5 0 174.080 5.77334 17 2 -5 0 174.346 6.85126 1 -2 -5 0 172.798 5.72838 7 2 -5 0 186.545 7.61701 5 -2 -5 0 176.894 5.90787 18 -2 5 0 181.141 5.23892 16 -2 5 0 180.618 7.09427 4 -2 5 0 180.179 5.67405 9 2 5 0 173.374 7.36031 2 -2 5 0 170.375 5.83787 8 -2 5 0 181.031 8.95044 5 2 5 0 179.294 5.83920 16 -2 5 0 176.487 7.51526 2 2 5 0 182.970 7.76622 4 -2 5 0 174.440 7.21684 1 -2 5 0 185.889 5.69164 11 2 5 0 182.804 6.29121 1 2 5 0 185.989 5.23340 15 -2 5 0 172.850 5.30701 12 -2 5 0 181.832 5.43640 15 2 5 0 166.107 5.66765 10 -2 5 0 170.731 5.85235 10 -2 5 0 172.644 8.94060 3 -3 -5 0 18.3349 1.36721 1 3 -5 0 18.2222 1.32070 7 -3 -5 0 16.3052 3.13438 18 -3 -5 0 19.5005 1.63988 7 -3 -5 0 14.5226 2.17742 2 3 -5 0 16.1697 1.41458 7 -3 -5 0 20.3829 2.09982 5 -3 -5 0 17.3444 0.96656 15 -3 -5 0 12.8949 3.02329 17 -3 -5 0 19.1968 2.14443 3 3 -5 0 16.5078 2.01841 1 -3 -5 0 23.0735 3.06578 17 3 5 0 15.1587 2.24290 2 -3 5 0 15.6872 0.95000 16 3 5 0 20.1483 2.45306 4 -3 5 0 24.1366 3.90013 3 3 5 0 16.5206 1.73655 16 -3 5 0 17.9525 1.19077 6 -3 5 0 17.6653 2.41615 17 -3 5 0 18.6839 1.16635 12 -3 5 0 16.7989 1.30618 9 3 5 0 18.4397 1.51523 6 -3 5 0 20.1356 2.40767 2 -3 5 0 18.9276 1.98847 4 3 5 0 15.6887 0.98946 15 -3 5 0 18.8274 1.53879 10 -3 5 0 15.3902 2.22502 1 -3 5 0 18.3123 1.10628 6 -3 5 0 17.1025 1.15597 15 -3 5 0 18.9888 1.42186 8 3 5 0 17.3907 1.21109 13 3 5 0 19.1853 1.35650 10 -3 5 0 14.8558 1.29272 11 -3 5 0 21.6746 3.05163 18 3 5 0 18.9400 1.36077 6 -3 5 0 29.8497 4.18791 5 -4 -5 0 168.313 10.0387 17 -4 -5 0 174.976 6.33282 7 -4 -5 0 171.462 6.94883 3 -4 -5 0 166.049 7.31524 2 -4 -5 0 167.202 6.26729 7 -4 -5 0 168.067 9.62440 18 -4 -5 0 165.056 4.92799 15 -4 -5 0 167.416 5.21184 1 -4 -5 0 171.678 9.03089 17 4 -5 0 165.869 6.01847 7 -4 -5 0 166.278 7.42549 4 -4 -5 0 169.263 6.93316 5 4 -5 0 163.175 6.87360 1 4 -5 0 173.314 5.80352 7 -4 5 0 163.042 5.52420 9 -4 5 0 169.597 5.19616 12 -4 5 0 165.385 7.56141 2 4 5 0 168.782 6.04752 6 -4 5 0 157.221 5.62782 6 -4 5 0 165.007 7.85903 17 -4 5 0 161.842 4.83266 16 4 5 0 166.909 5.27744 16 4 5 0 166.169 4.95709 15 4 5 0 171.152 7.72701 4 -4 5 0 168.254 5.66382 8 -4 5 0 168.607 8.82661 18 -4 5 0 164.162 7.30989 1 -4 5 0 164.183 6.45552 4 4 5 0 166.690 5.98338 6 -4 5 0 168.157 5.48419 11 -4 5 0 168.125 8.88260 5 -4 5 0 164.651 5.87487 10 -4 5 0 171.833 9.03208 3 -4 5 0 167.731 5.23685 15 4 5 0 162.608 5.57053 10 -4 5 0 168.038 5.74291 6 -5 -5 0 43.9769 1.73815 11 5 -5 0 44.2469 3.28919 1 -5 -5 0 44.7780 3.56070 4 -5 -5 0 44.6527 3.09071 7 -5 -5 0 43.8955 2.99496 7 -5 -5 0 44.3197 3.28630 5 -5 -5 0 46.4102 5.91745 17 -5 -5 0 47.5805 3.75232 2 5 -5 0 43.1233 2.58447 7 -5 -5 0 43.5921 1.44789 14 -5 -5 0 44.4936 3.32461 3 5 -5 0 46.6952 2.94056 7 -5 -5 0 40.0487 6.33221 18 -5 -5 0 38.5412 6.69061 17 -5 -5 0 45.0491 2.25095 15 -5 -5 0 41.6701 1.77100 1 -5 5 0 42.5057 2.30131 8 5 5 0 44.0375 3.77605 4 -5 5 0 43.4785 2.23652 11 -5 5 0 42.6511 4.58993 3 -5 5 0 44.2471 2.80339 6 -5 5 0 40.0287 3.42086 1 -5 5 0 48.8899 4.81803 5 5 5 0 43.3752 2.84400 6 -5 5 0 44.4257 2.57225 10 -5 5 0 42.2752 2.63496 6 5 5 0 45.9096 1.82798 11 -5 5 0 43.6167 2.00664 12 5 5 0 42.3727 2.27256 10 -5 5 0 45.3363 2.83573 4 5 5 0 42.4741 2.88790 6 -5 5 0 43.3898 1.63054 16 5 5 0 45.4602 2.09230 16 -5 5 0 47.1984 2.33213 9 -5 5 0 34.6220 5.22498 17 -5 5 0 47.7490 6.56259 18 -5 5 0 43.5049 3.80355 2 5 5 0 46.6875 2.12361 13 -5 5 0 41.3246 2.00065 15 6 -5 0 46.2193 1.56506 14 -6 -5 0 52.0602 4.06271 2 -6 -5 0 47.1971 3.48107 3 6 -5 0 49.6963 3.37646 7 -6 -5 0 50.3370 3.92488 7 -6 -5 0 46.5174 3.39933 7 -6 -5 0 50.2908 3.69051 5 -6 -5 0 49.6870 6.91357 17 -6 -5 0 57.2740 8.80310 17 -6 -5 0 46.6103 4.44544 4 6 -5 0 46.9148 4.14627 1 -6 -5 0 48.9166 1.67355 14 6 -5 0 48.0408 3.36590 7 -6 -5 0 50.5828 7.86142 18 -6 -5 0 42.9447 2.43125 10 -6 -5 0 45.5115 1.87279 11 -6 5 0 51.5314 2.56186 8 6 5 0 46.5545 2.27406 13 6 5 0 50.5435 3.88933 6 -6 5 0 45.3737 5.81902 17 -6 5 0 45.8893 2.80403 10 -6 5 0 46.3660 2.36537 11 -6 5 0 43.4189 2.11216 15 -6 5 0 44.2332 4.02944 2 -6 5 0 38.7005 5.74469 18 -6 5 0 49.8521 4.94842 5 -6 5 0 51.1219 4.47401 1 6 5 0 48.0860 1.95202 11 6 5 0 44.2589 2.42457 10 -6 5 0 45.2658 2.13942 12 6 5 0 49.1180 2.23535 16 -6 5 0 45.3907 2.40836 9 -6 5 0 46.2007 3.26573 6 -6 5 0 43.8461 1.69435 16 6 5 0 54.2816 3.43351 6 6 5 0 42.3056 4.54908 4 -6 5 0 48.0566 4.78802 6 -6 5 0 47.7669 2.82132 4 -7 -5 0 55.4846 4.03264 7 7 -5 0 57.1612 1.88726 14 -7 -5 0 57.4661 4.31562 4 7 -5 0 55.0793 3.96213 1 7 -5 0 56.9004 3.50796 7 -7 -5 0 55.3214 4.39246 2 -7 -5 0 56.5494 2.86974 10 -7 -5 0 54.3941 1.96850 14 -7 -5 0 47.3063 2.49956 11 -7 -5 0 52.4116 7.72147 17 -7 -5 0 59.5583 3.97683 7 -7 -5 0 53.2312 2.22036 15 -7 -5 0 57.7592 4.14898 5 7 -5 0 54.1407 3.87041 7 -7 -5 0 57.3764 3.95146 3 -7 5 0 53.8392 3.73242 6 -7 5 0 60.9552 2.91977 8 7 5 0 57.3259 3.94349 6 -7 5 0 57.0768 3.21035 10 -7 5 0 65.6537 5.82191 3 -7 5 0 52.8199 4.58315 2 -7 5 0 53.1094 2.43709 15 -7 5 0 54.5206 2.75041 9 7 5 0 49.7453 4.27167 4 -7 5 0 57.8804 5.53856 5 -7 5 0 50.8891 3.87779 6 -7 5 0 60.7585 4.44231 1 -7 5 0 52.3679 1.82390 16 -7 5 0 55.1760 2.46282 12 7 5 0 53.7345 2.48191 16 7 5 0 53.7941 2.74978 10 -7 5 0 54.7584 2.62991 11 7 5 0 55.5692 2.56340 13 -7 5 0 57.1530 2.97782 4 -8 -5 0 128.036 7.08876 2 -8 -5 0 113.353 11.4518 17 -8 -5 0 116.104 6.26570 5 -8 -5 0 104.799 5.81759 3 8 -5 0 119.001 6.10425 1 -8 -5 0 125.968 6.30615 7 -8 -5 0 113.774 3.58076 14 8 -5 0 115.202 5.55602 7 -8 -5 0 111.413 6.19888 7 -8 -5 0 109.297 3.82326 15 8 -5 0 110.183 3.43217 14 -8 -5 0 111.391 3.70256 11 -8 -5 0 106.347 6.28425 4 8 -5 0 106.205 5.95589 7 -8 -5 0 113.491 4.70444 10 -8 5 0 109.942 4.06357 12 8 5 0 110.970 4.52476 10 -8 5 0 115.077 5.09940 10 8 5 0 110.716 4.20790 13 -8 5 0 112.062 4.52507 9 -8 5 0 114.295 4.54820 8 -8 5 0 106.791 7.68532 5 -8 5 0 112.253 7.13312 2 -8 5 0 108.029 7.82641 3 -8 5 0 109.054 6.36755 1 8 5 0 109.967 6.57491 4 -8 5 0 111.560 4.11642 15 8 5 0 131.907 6.37240 6 -8 5 0 110.454 4.33348 11 -8 5 0 108.265 4.29596 4 -8 5 0 115.337 6.10748 6 -9 -5 0 14.5140 1.13381 11 -9 -5 0 15.4933 1.07011 14 9 -5 0 14.9910 1.03292 14 -9 -5 0 5.20857 6.50523 17 -9 -5 0 9.51600 2.59938 2 9 -5 0 17.3229 2.78305 1 -9 -5 0 14.5771 2.70538 4 9 -5 0 21.1713 2.62873 7 -9 -5 0 16.7457 2.78649 7 -9 -5 0 17.0186 2.73487 3 -9 -5 0 15.7250 1.21471 15 -9 -5 0 19.2953 3.02418 5 -9 5 0 12.7070 2.15444 10 9 5 0 12.5626 1.54008 13 -9 5 0 15.5457 2.72555 6 -9 5 0 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8.81396 2 3 -7 0 179.848 7.77419 1 -3 -7 0 181.629 8.20622 3 -3 -7 0 178.840 8.05999 5 -3 7 0 173.379 5.60057 6 3 7 0 185.708 5.69293 11 3 7 0 174.542 5.88190 13 3 7 0 186.633 6.20220 6 3 7 0 159.521 5.35752 12 -3 7 0 177.801 6.27400 8 -3 7 0 186.088 6.27465 11 -3 7 0 168.710 8.48723 2 -3 7 0 177.529 10.8150 3 -3 7 0 178.301 5.75278 12 -3 7 0 171.543 8.21014 1 -3 7 0 180.776 6.53660 10 3 7 0 172.818 6.09138 6 -3 7 0 176.215 5.55587 13 -3 7 0 176.820 7.99421 4 3 7 0 180.195 8.66434 2 3 7 0 176.619 5.89862 16 3 7 0 181.082 5.56877 15 -3 7 0 167.758 10.1638 5 3 7 0 174.672 5.55436 9 -3 7 0 179.497 5.79546 15 -3 7 0 176.593 5.53206 16 3 7 0 179.168 6.30328 10 -3 7 0 179.265 5.79813 6 3 7 0 172.254 8.82558 4 -3 7 0 170.907 6.13327 9 4 -7 0 45.4929 3.70532 1 4 -7 0 43.3664 4.40049 5 -4 -7 0 41.5260 1.91795 15 4 -7 0 46.8798 2.37134 7 -4 -7 0 41.2762 2.84376 7 -4 -7 0 43.1881 1.85074 9 -4 -7 0 41.2752 4.24205 3 -4 -7 0 35.9739 2.28834 1 -4 -7 0 42.7862 2.79947 7 4 -7 0 38.9608 2.68703 7 -4 -7 0 37.3690 3.59529 5 -4 -7 0 36.8962 3.87867 2 -4 -7 0 34.6449 3.88054 4 -4 7 0 40.3284 2.16748 15 4 7 0 42.1459 2.02062 11 4 7 0 43.6825 2.58502 10 -4 7 0 33.2677 5.32901 5 4 7 0 39.0694 2.28586 13 -4 7 0 41.0311 2.64682 6 -4 7 0 47.4150 6.71788 3 -4 7 0 36.0958 2.11973 13 -4 7 0 38.4144 2.50031 11 4 7 0 44.1535 1.99653 15 -4 7 0 45.8578 3.98985 1 -4 7 0 39.6082 4.07115 2 -4 7 0 44.1488 3.66546 4 -4 7 0 45.3897 2.63093 6 4 7 0 42.5681 2.19675 9 4 7 0 45.9990 4.43897 4 4 7 0 41.3875 2.83801 6 -4 7 0 37.2938 2.08084 16 4 7 0 43.0744 2.76133 6 -4 7 0 41.3073 2.64409 10 -4 7 0 41.0761 2.47943 8 -5 -7 0 91.2997 6.04151 17 5 -7 0 79.6121 4.20059 7 -5 -7 0 83.6163 4.44422 7 -5 -7 0 79.4446 2.41715 14 -5 -7 0 80.8906 3.03130 15 -5 -7 0 80.5133 5.68465 2 -5 -7 0 84.6025 5.28459 5 5 -7 0 73.3813 2.28861 14 5 -7 0 82.5172 3.71458 7 -5 -7 0 82.8189 5.73505 4 5 -7 0 83.8535 5.27606 1 -5 -7 0 75.3479 2.78626 9 -5 -7 0 78.8894 2.92867 11 5 -7 0 86.4908 6.15906 5 -5 -7 0 78.6187 4.23875 7 -5 -7 0 92.6116 7.04378 18 -5 -7 0 86.4654 4.26936 1 -5 7 0 76.0003 2.84980 16 5 7 0 74.6536 2.98136 15 -5 7 0 77.2959 5.52608 1 -5 7 0 80.6602 4.60484 6 5 7 0 79.4266 3.03838 11 -5 7 0 76.4417 3.88799 11 -5 7 0 82.8814 5.76818 2 -5 7 0 74.5041 7.36915 3 -5 7 0 77.6842 3.71648 8 -5 7 0 81.1824 7.53076 5 -5 7 0 78.6630 4.15667 6 5 7 0 76.7369 3.37305 16 -5 7 0 77.4314 4.71114 4 5 7 0 81.6850 2.90056 9 5 7 0 86.7548 6.16100 4 5 7 0 78.5182 4.26200 6 5 7 0 81.1054 3.78569 13 -5 7 0 79.6566 3.99093 10 -5 7 0 81.2959 3.36075 15 5 7 0 81.3197 4.39797 6 -6 -7 0 2.65016 1.80737 2 -6 -7 0 2.43016 1.71064 4 6 -7 0 1.40539 0.34242 14 -6 -7 0 0.93499 0.53003 11 -6 -7 0 3.57427 1.63901 3 -6 -7 0 0.38571 1.07927 7 -6 -7 0 -0.1196 1.75402 7 6 -7 0 2.04118 1.49754 1 6 -7 0 1.51586 0.90622 7 -6 -7 0 1.65547 0.60151 15 -6 -7 0 0.25399 1.50888 5 6 -7 0 1.59481 1.40873 7 -6 7 0 2.81110 1.76111 6 -6 7 0 -0.6410 1.35593 4 -6 7 0 2.12959 2.75272 5 -6 7 0 2.42702 0.98735 15 6 7 0 -2.1320 1.42719 4 -6 7 0 2.56773 0.78521 12 6 7 0 0.90598 0.57037 11 -6 7 0 0.09928 1.06280 6 -6 7 0 3.87192 4.38364 17 -6 7 0 2.36881 1.70378 1 -6 7 0 2.75573 0.51965 16 -6 7 0 2.20198 2.67344 3 -6 7 0 1.40230 1.92298 2 6 7 0 2.65497 0.78988 16 -6 7 0 1.44103 1.01444 10 6 7 0 1.08996 0.78657 13 -6 7 0 1.54778 0.84624 9 -6 7 0 2.73187 4.14259 18 6 7 0 0.47600 1.13916 6 -6 7 0 0.56345 0.75347 11 -6 7 0 2.73770 0.94011 8 -7 -7 0 29.2204 3.60067 3 7 -7 0 34.2898 1.37995 14 -7 -7 0 30.9462 1.45670 14 -7 -7 0 34.4372 4.23427 2 -7 -7 0 37.4454 4.23482 5 -7 -7 0 31.0586 1.77812 15 -7 -7 0 35.9773 3.31770 7 -7 -7 0 21.5747 7.40465 18 7 -7 0 34.6230 3.73148 1 -7 -7 0 34.2044 1.75608 11 -7 -7 0 19.7987 6.74025 17 7 -7 0 32.0603 2.71826 7 -7 -7 0 28.5684 3.99973 4 -7 -7 0 31.0573 3.57356 7 -7 -7 0 31.4621 2.42558 10 -7 7 0 34.4093 3.47747 6 -7 7 0 28.0441 5.34122 3 7 7 0 29.9494 2.09220 16 -7 7 0 33.8457 2.12117 12 -7 7 0 37.3496 4.13349 1 -7 7 0 31.4671 3.02910 4 -7 7 0 25.7629 7.83626 17 7 7 0 37.7644 3.56645 6 -7 7 0 38.0305 7.70877 18 7 7 0 33.6847 2.31080 13 -7 7 0 34.3954 2.48713 11 -7 7 0 34.2115 4.67991 2 7 7 0 31.2280 2.35520 10 7 7 0 36.7468 4.42053 4 -7 7 0 28.9981 2.01615 15 -7 7 0 32.9027 2.43103 8 -7 7 0 40.7786 2.64445 9 -7 7 0 39.8888 2.92196 10 7 7 0 32.3142 1.82420 11 -8 -7 0 135.930 7.68190 5 -8 -7 0 141.570 4.69612 15 -8 -7 0 135.250 5.75203 10 -8 -7 0 135.439 8.13619 4 8 -7 0 137.493 4.10018 14 8 -7 0 137.792 6.29981 7 -8 -7 0 128.766 7.30367 3 -8 -7 0 131.705 4.52214 11 -8 -7 0 138.217 7.11121 7 -8 -7 0 134.931 4.26399 14 -8 -7 0 143.389 9.42474 2 8 -7 0 132.952 7.57035 1 -8 7 0 132.708 5.08355 15 -8 7 0 129.487 6.06097 10 -8 7 0 134.433 7.59984 6 8 7 0 134.056 5.58300 10 8 7 0 131.466 7.13303 6 8 7 0 132.421 5.27296 13 -8 7 0 132.318 8.46727 2 -8 7 0 134.343 5.58543 8 -8 7 0 120.732 13.3450 3 -8 7 0 137.753 5.05870 12 -8 7 0 123.039 5.46302 9 -8 7 0 150.574 10.9018 5 8 7 0 132.844 8.48840 4 -8 7 0 135.724 5.56692 11 -8 7 0 135.249 8.06233 1 0 -8 0 650.298 22.1147 2 0 -8 0 634.703 22.4469 3 0 -8 0 685.396 22.4477 5 0 -8 0 674.913 20.5314 1 0 -8 0 687.689 22.3051 4 0 8 0 700.421 19.0706 15 0 8 0 672.699 22.6606 4 0 8 0 684.341 19.0957 16 0 8 0 667.273 18.9421 8 0 8 0 685.961 18.4257 12 0 8 0 688.589 18.9219 11 0 8 0 646.249 18.6299 13 0 8 0 695.101 19.5244 10 0 8 0 703.154 18.9704 9 0 8 0 687.692 25.1217 3 0 8 0 686.497 22.8562 2 1 -8 0 2.93639 1.74762 4 -1 -8 0 0.66117 1.62938 2 1 -8 0 1.35464 1.99934 5 1 -8 0 -2.2502 1.07647 1 1 -8 0 2.02251 1.77114 3 -1 -8 0 2.03869 1.66621 4 1 -8 0 1.42717 1.61057 2 -1 -8 0 -1.9181 1.43822 3 -1 -8 0 0.42416 1.74012 5 -1 -8 0 1.81353 1.27365 1 1 8 0 -0.4312 1.69903 2 1 8 0 1.09880 0.78342 13 1 8 0 0.05177 1.65995 4 -1 8 0 0.29159 1.67917 4 1 8 0 -0.4038 0.56153 8 1 8 0 1.40598 0.75446 10 -1 8 0 0.68162 0.70718 13 -1 8 0 -0.4171 0.64383 9 -1 8 0 0.69408 0.59476 12 -1 8 0 1.91466 2.60471 3 -1 8 0 0.69520 0.76542 8 1 8 0 0.88677 0.71105 9 1 8 0 0.15736 0.52242 12 -1 8 0 1.32329 0.66418 15 -1 8 0 -0.3152 0.54492 16 -1 8 0 1.04690 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316.344 8.97042 8 -3 -4 -3 315.257 13.7712 18 3 -4 3 322.366 10.2523 1 3 -4 3 318.959 8.12854 14 -3 -4 -3 304.578 9.59102 7 -3 4 -3 311.349 12.8219 5 -3 4 -3 321.412 10.6874 4 3 4 3 294.541 9.09034 1 -3 4 -3 301.078 12.9159 3 -3 4 -3 306.847 9.60677 10 3 4 3 299.131 9.69349 5 3 4 3 310.527 8.88682 13 -3 4 -3 310.679 9.00211 9 -3 4 -3 329.736 8.59404 16 -3 4 -3 306.931 10.5728 6 -3 4 -3 315.619 8.81101 15 3 4 3 304.814 14.3046 17 3 4 3 294.143 10.7275 6 -3 4 -3 313.845 8.90191 8 -3 4 -3 307.340 11.8940 2 -3 4 -3 306.586 9.72558 6 -3 4 -3 313.514 8.67589 12 -3 4 -3 327.749 9.07826 11 -4 -4 -3 443.211 11.5425 15 -4 -4 -3 428.937 12.7146 3 -4 -4 -3 429.146 13.1544 5 4 -4 3 428.611 19.3347 17 -4 -4 -3 458.196 13.5631 7 -4 -4 -3 443.219 11.4060 14 -4 -4 -3 445.873 18.2486 18 4 -4 3 414.481 13.4830 7 4 -4 3 460.635 11.4732 14 4 -4 3 438.064 12.2933 8 -4 -4 -3 439.964 14.3404 4 -4 -4 -3 449.621 14.0775 5 4 -4 3 427.986 13.1836 7 -4 -4 -3 438.040 14.2430 2 4 -4 3 424.298 13.5548 1 -4 -4 -3 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0.97520 11 7 0 -15 10.4373 1.24502 16 7 0 -15 9.74252 0.94273 14 7 0 -15 5.33061 2.79257 7 -7 0 15 12.6552 2.67184 5 -7 0 15 10.7150 1.65419 9 -7 0 15 8.17254 1.18511 12 -7 0 15 10.0446 2.92364 1 -7 0 15 7.66305 2.71555 3 -6 0 15 69.6143 3.55846 9 -6 0 15 60.4706 3.68396 8 6 0 -15 63.9759 5.52855 4 -6 0 15 57.6448 5.61340 1 6 0 -15 66.7203 6.35747 7 6 0 -15 59.9338 2.52829 14 -6 0 15 62.5252 5.16581 3 -6 0 15 77.1309 4.76199 5 -6 0 15 72.6947 6.01703 6 -6 0 15 64.9491 2.50885 11 -6 0 15 58.5559 2.38249 15 6 0 -15 64.9771 2.88920 13 -6 0 15 64.7760 3.00494 12 6 0 -15 64.2635 2.92926 16 5 0 -15 7.22541 2.90606 7 -5 0 15 6.66748 1.29378 9 5 0 -15 6.20496 0.98834 13 5 0 -15 4.55368 2.17184 4 5 0 -15 6.39491 1.03524 16 -5 0 15 1.51683 1.87982 1 5 0 -15 5.16573 0.76314 14 -5 0 15 4.63914 1.33515 8 -5 0 15 6.07291 2.38926 6 -5 0 15 5.53859 0.95879 12 -5 0 15 6.50901 2.26959 3 -4 0 15 91.2624 5.72127 3 4 0 -15 75.7306 3.28162 13 -4 0 15 93.9506 6.97436 6 4 0 -15 93.1067 6.55267 4 4 0 -15 83.1857 6.69809 7 4 0 -15 82.7263 3.04576 14 -4 0 15 82.9839 4.45469 8 -4 0 15 89.7829 3.98668 9 -4 0 15 89.1402 3.55263 12 4 0 -15 87.8903 3.55232 16 -4 0 15 82.3188 6.38051 1 -3 0 15 2.11667 2.10864 6 3 0 -15 -1.0860 1.89977 4 -3 0 15 -1.1640 1.92063 1 -3 0 15 -0.6457 0.86386 8 3 0 -15 -1.0343 0.52926 16 3 0 -15 -1.0799 0.41974 14 -3 0 15 -0.9809 0.70165 9 -3 0 15 2.38752 2.01088 3 3 0 -15 1.28426 2.34015 7 -3 0 15 -0.7154 0.62000 12 2 0 -15 32.7883 1.63524 14 -2 0 15 33.5259 2.00440 12 -2 0 15 32.7643 2.02560 13 -2 0 15 45.3223 4.75719 1 2 0 -15 34.2014 4.68524 7 -2 0 15 31.3751 2.13550 9 2 0 -15 32.6321 2.03848 16 -2 0 15 34.4032 2.80694 8 -2 0 15 39.7725 4.81255 6 2 0 -15 32.7352 1.98224 13 2 0 -15 32.1153 4.73335 4 1 0 -15 2.66305 0.74594 13 -1 0 15 0.46354 2.16635 1 1 0 -15 3.66221 0.59210 14 1 0 -15 5.65177 2.31150 4 7 -1 -15 174.581 6.34246 16 -7 -1 15 161.047 8.10071 5 7 -1 -15 172.344 10.2369 7 -7 -1 15 165.831 6.48470 9 7 -1 -15 151.917 5.63983 14 -7 -1 15 184.610 9.42586 3 -7 -1 15 159.982 5.27541 15 -7 -1 15 163.544 10.2258 7 7 -1 -15 166.727 5.77155 13 -7 -1 15 172.071 9.69118 1 -7 -1 15 166.168 5.71568 12 -7 -1 15 166.658 6.55804 8 -7 -1 15 159.190 5.67003 11 7 -1 -15 167.093 8.64612 4 -7 1 15 177.099 6.53953 9 -7 1 15 166.489 9.78508 1 7 1 -15 175.125 5.64086 13 -7 1 15 173.437 7.00671 8 -7 1 15 161.707 9.12085 6 7 1 -15 162.765 9.15483 4 7 1 -15 162.180 5.75826 16 7 1 -15 174.558 10.4383 7 -7 1 15 173.231 8.53696 3 -7 1 15 178.333 5.90050 12 -6 -1 15 82.7660 4.17870 8 -6 -1 15 80.1350 3.37557 12 -6 -1 15 85.9958 7.20138 7 -6 -1 15 78.4956 6.58887 6 6 -1 -15 82.8167 6.15649 4 6 -1 -15 81.0934 3.43949 13 -6 -1 15 84.2598 4.01679 9 -6 -1 15 72.9364 5.85384 3 6 -1 -15 77.9002 2.98283 14 -6 -1 15 80.1928 5.47790 5 6 -1 -15 63.4044 6.55960 7 -6 -1 15 85.0225 3.04586 11 6 -1 -15 84.1500 3.33655 16 -6 -1 15 77.9778 2.93510 15 -6 -1 15 89.8541 6.62925 1 -6 1 15 87.3123 4.53036 8 -6 1 15 83.5432 3.48499 12 6 1 -15 75.7371 7.09966 7 6 1 -15 88.8805 6.55109 4 -6 1 15 66.6452 6.18813 1 -6 1 15 73.4822 5.98255 6 -6 1 15 79.1503 3.86142 9 6 1 -15 81.3632 3.46414 16 6 1 -15 77.7206 3.21050 13 -6 1 15 78.3102 5.57157 3 -5 -1 15 13.7782 3.23169 1 5 -1 -15 16.4996 1.17066 14 5 -1 -15 13.8124 3.49825 7 -5 -1 15 20.9494 1.94157 9 -5 -1 15 20.4958 1.20285 15 -5 -1 15 17.0872 2.99024 5 -5 -1 15 19.2191 3.88552 7 -5 -1 15 17.1347 3.17470 2 -5 -1 15 15.8085 3.41849 6 -5 -1 15 16.1667 2.96595 3 -5 -1 15 20.6289 1.56212 12 -5 -1 15 16.8864 2.17263 8 5 -1 -15 21.2474 1.59429 13 5 -1 -15 18.6755 1.47727 16 5 -1 -15 14.8184 3.10934 4 -5 -1 15 17.8637 1.23440 11 -5 1 15 18.3439 2.99293 3 5 1 -15 16.0740 1.50619 16 5 1 -15 22.9311 3.95258 4 -5 1 15 19.4078 1.81158 9 5 1 -15 20.2355 1.61525 13 -5 1 15 15.9623 1.49383 12 -5 1 15 17.7672 1.69413 13 -5 1 15 29.4895 4.68624 1 -5 1 15 13.8902 2.92933 6 -5 1 15 22.2514 2.33371 8 5 1 -15 18.4413 3.49839 2 5 1 -15 14.1330 3.62651 7 -4 -1 15 -0.9992 1.96820 5 -4 -1 15 0.33373 0.38676 15 4 -1 -15 0.08061 0.50996 16 -4 -1 15 -0.1502 0.47718 12 -4 -1 15 -0.1313 0.60169 9 4 -1 -15 0.55229 1.73432 4 4 -1 -15 0.03842 0.37193 14 -4 -1 15 -0.5961 1.87123 3 -4 -1 15 4.06643 2.80456 7 -4 -1 15 0.60310 0.47853 11 4 -1 -15 -3.8802 1.92524 7 -4 -1 15 0.43898 0.83298 8 -4 -1 15 0.03875 1.73743 1 4 -1 -15 0.31552 0.62062 13 -4 -1 15 -0.1302 2.17241 6 4 1 -15 0.94579 0.58470 13 4 1 -15 0.79037 1.72601 2 -4 1 15 0.44733 0.57457 12 -4 1 15 -0.6248 0.54351 9 4 1 -15 -0.8641 2.25039 7 -4 1 15 -3.6495 1.86167 3 -4 1 15 0.91955 1.91377 1 -4 1 15 -1.9763 1.65761 6 4 1 -15 0.96784 0.64554 16 -4 1 15 0.87590 0.98945 8 -4 1 15 1.11144 0.78839 13 -3 -1 15 1.23489 0.64976 12 -3 -1 15 2.65364 2.00598 1 3 -1 -15 -0.3106 2.20634 7 -3 -1 15 6.57022 3.12201 7 -3 -1 15 0.96014 2.02022 3 -3 -1 15 2.04140 1.11170 8 3 -1 -15 2.73652 0.60044 14 -3 -1 15 2.25457 0.96113 9 -3 -1 15 1.18286 2.46101 6 3 -1 -15 3.49181 0.80765 16 3 -1 -15 3.20988 0.87111 13 3 -1 -15 3.13423 2.05525 4 -3 1 15 2.46194 1.11544 8 3 1 -15 3.51221 0.71503 13 3 1 -15 0.84870 1.71377 2 -3 1 15 2.18706 0.91360 13 3 1 -15 -3.1409 2.33998 7 -3 1 15 1.59996 2.08953 6 -3 1 15 3.40671 0.82563 12 3 1 -15 0.41553 1.88287 4 -3 1 15 5.50667 2.62228 1 3 1 -15 2.51770 0.73527 16 -2 -1 15 130.423 4.67290 12 -2 -1 15 129.944 8.16473 1 -2 -1 15 129.634 5.87384 8 -2 -1 15 129.412 8.90497 7 2 -1 -15 120.588 7.70244 4 -2 -1 15 132.778 5.09899 9 2 -1 -15 134.468 4.77005 16 2 -1 -15 128.324 4.30668 14 2 -1 -15 136.686 8.27508 7 2 -1 -15 128.374 4.70077 13 2 1 -15 131.723 4.86172 16 -2 1 15 129.371 4.93282 9 -2 1 15 123.134 7.56125 6 -2 1 15 135.552 8.66501 1 -2 1 15 134.077 4.92133 13 2 1 -15 115.438 8.38789 7 -2 1 15 135.088 4.71987 12 2 1 -15 113.234 7.84091 4 2 1 -15 123.050 4.24910 13 -2 1 15 134.164 6.10122 8 -5 -2 15 116.652 8.63595 7 5 -2 -15 116.696 4.58840 13 -5 -2 15 118.043 7.80611 1 5 -2 -15 119.580 7.22181 4 5 -2 -15 116.458 3.95764 14 5 -2 -15 124.889 8.23715 7 -5 -2 15 124.124 7.61243 3 5 -2 -15 121.200 4.26755 16 -5 -2 15 117.795 6.06412 2 -5 -2 15 118.628 4.05246 11 -5 -2 15 120.811 5.05801 9 -5 -2 15 117.218 4.37379 12 -5 -2 15 114.431 5.14816 8 -5 -2 15 121.299 4.04701 15 -5 -2 15 101.646 6.79507 5 -5 2 15 118.158 4.50361 12 5 2 -15 112.413 4.04699 13 -5 2 15 121.727 8.09693 1 -5 2 15 119.413 4.83310 9 5 2 -15 113.762 7.82397 4 5 2 -15 122.232 8.78175 6 -5 2 15 112.246 4.71901 13 5 2 -15 119.766 4.59799 16 -5 2 15 111.017 5.57669 8 5 2 -15 106.877 6.28420 2 -4 -2 15 478.396 17.0527 3 4 -2 -15 430.885 17.8275 7 4 -2 -15 466.316 13.4084 13 -4 -2 15 447.179 18.3955 7 -4 -2 15 449.042 13.0803 12 4 -2 -15 464.600 13.0324 16 -4 -2 15 448.728 14.2169 8 4 -2 -15 463.758 12.6622 14 -4 -2 15 449.478 12.6470 15 -4 -2 15 450.067 12.8536 11 -4 -2 15 485.393 18.0520 1 -4 -2 15 448.750 15.9918 5 -4 -2 15 456.226 13.9091 9 4 -2 -15 480.865 17.1451 4 4 2 -15 440.575 12.6424 13 -4 2 15 452.742 13.5754 13 -4 2 15 459.324 13.5986 9 4 2 -15 444.445 18.3013 6 -4 2 15 472.841 13.2741 12 -4 2 15 471.674 14.9336 8 4 2 -15 465.549 13.4611 16 4 2 -15 450.985 18.0725 4 4 2 -15 432.856 15.7841 2 -4 2 15 467.435 18.1342 1 4 2 -15 448.451 12.8201 11 0 0 0 0.00 0.00 0 _chemical_formula_moiety 'C18 H22 N4 O3 S' _exptl_crystal_description prism _exptl_crystal_colour yellow _cell_measurement_reflns_used 41475 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.30 _exptl_absorpt_correction_T_min 0.8697 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ) SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined by point group 2/m for scaling and error model Mean and maximum errors in direction cosine check function = 0.000 0.003 Restraint esd for equal adjacent scale factors = 0.0060 Maximum odd and even orders for spherical harmonics = 3 6 wR2(int) = 0.1284 (selected reflections only, before parameter refinement) wR2(int) = 0.0483 (selected reflections only, after parameter refinement) 66887 total and 2266 unique reflections assuming Friedel's law plus 3281 total and 1023 unique reflections in fast scans Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 66583 total and 2266 unique reflections left after |I-|/su test plus 3264 total and 1023 unique reflections in fast scans su^2 = [K*sigma(I)]^2 + [g]^2 where sigma(I) is from SAINT Error model 5: refine all K and overall g Run 2theta R(int) Incid. factors Diffr. factors K g I/s(lim) Total I>2sig(I) 1 29.6 0.0276 0.267 - 0.481 0.970 - 1.025 0.975 0.0253 39.5 4066 3610 2 29.6 0.0294 0.398 - 0.608 0.971 - 1.019 0.973 0.0253 39.5 4058 3547 3 29.6 0.0302 0.414 - 0.708 0.970 - 1.030 1.011 0.0253 39.5 4037 3474 4 29.6 0.0293 0.336 - 0.492 0.983 - 1.015 0.980 0.0253 39.5 4082 3612 5 14.6 0.0300 0.413 - 0.742 0.970 - 1.031 0.962 0.0253 39.5 4782 4179 6 29.6 0.0316 0.318 - 0.634 0.970 - 1.036 1.075 0.0253 39.5 6019 5316 7 29.6 0.0328 0.282 - 0.444 0.970 - 1.023 1.079 0.0253 39.5 6972 6224 8 68.3 0.0300 0.309 - 0.536 0.975 - 1.021 0.857 0.0253 39.5 2670 2395 9 68.3 0.0307 0.316 - 0.449 0.970 - 1.030 0.823 0.0253 39.5 2666 2406 10 68.3 0.0325 0.434 - 0.660 0.983 - 1.027 0.824 0.0253 39.5 2664 2404 11 68.3 0.0298 0.450 - 0.733 0.972 - 1.031 0.758 0.0253 39.5 2681 2440 12 68.3 0.0269 0.307 - 0.505 0.972 - 1.027 0.776 0.0253 39.5 2675 2449 13 68.3 0.0304 0.366 - 0.621 0.970 - 1.013 0.823 0.0253 39.5 2679 2431 14 68.3 0.0247 0.307 - 0.466 0.970 - 1.011 0.817 0.0253 39.5 2733 2580 15 53.3 0.0279 0.369 - 0.472 0.970 - 1.031 0.820 0.0253 39.5 3377 3119 16 53.3 0.0288 0.348 - 0.513 0.984 - 1.013 0.818 0.0253 39.5 2823 2616 17 0.0 0.0505 0.303 - 0.509 0.984 - 1.030 1.029 0.0253 39.5 4585 3547 18 0.0 0.0530 0.386 - 0.491 0.984 - 1.030 0.972 0.0253 39.5 3014 2305 19f 0.0 0.1326 3.764 - 4.799 0.970 - 1.015 0.957 0.0253 39.5 3264 1763 15 Overloads replaced by fast scan measurements 66598 Corrected reflections written to file hkl Estimated minimum and maximum transmission: 0.8697 0.9583 Additional spherical absorption correction applied with mu*r = 0.0300 3lambda correction factor = 0.00150 ) loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4.00 0.00 3.00 0.1520 -4.00 -3.00 0.00 0.1580 -4.00 -1.00 -4.00 0.1350 -4.00 2.00 -3.00 0.1380 -3.00 -1.00 -4.00 0.1350 -3.00 -1.00 4.00 0.1320 -3.00 -1.00 -2.00 0.1400 -3.00 0.00 4.00 0.1450 -2.00 1.00 -4.00 0.1050 -2.00 2.00 -1.00 0.1340 -2.00 -3.00 -2.00 0.1190 -1.00 -4.00 -4.00 0.1180 -1.00 4.00 0.00 0.1230 -1.00 1.00 -4.00 0.1090 -1.00 4.00 -1.00 0.1170 -1.00 3.00 -2.00 0.1110 -1.00 -3.00 0.00 0.1090 -1.00 1.00 4.00 0.1440 -1.00 0.00 4.00 0.1250 -1.00 -1.00 4.00 0.1090 -1.00 -1.00 -4.00 0.1370 -1.00 2.00 -1.00 0.1170 -1.00 0.00 -1.00 0.1320 0.00 -2.00 -1.00 0.1210 0.00 -4.00 -3.00 0.1210 0.00 1.00 4.00 0.1190 0.00 1.00 -4.00 0.1220 0.00 3.00 -4.00 0.1060 0.00 -3.00 2.00 0.1140 0.00 -4.00 1.00 0.1060 1.00 -1.00 4.00 0.0850 1.00 3.00 0.00 0.1120 1.00 2.00 2.00 0.1170 1.00 2.00 3.00 0.1130 1.00 1.00 -2.00 0.1360 1.00 4.00 -1.00 0.1090 1.00 3.00 -2.00 0.1110 2.00 -1.00 4.00 0.0880 2.00 0.00 -1.00 0.1690 2.00 1.00 -4.00 0.1620 2.00 -4.00 3.00 0.1200 3.00 3.00 -1.00 0.1400 3.00 0.00 1.00 0.1410 3.00 2.00 -4.00 0.1470 3.00 4.00 -4.00 0.1270 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus Mo X-ray tube' _diffrn_source_type 'I\mS DIAMOND' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_detector 'PHOTON III' _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\f and \w scans' _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_molecular_graphics ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _computing_publication_material ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _refine_special_details ) Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ) CELL 0.71073 11.43150 6.67650 11.59690 90.0000 107.8509 90.0000 ZERR 2.00 0.00030 0.00020 0.00030 0.0000 0.0005 0.0000 LATT 1 SYMM - X, 1/2 + Y, - Z ; _shelx_hkl_checksum 70670