#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 4 _journal_year 2020 _journal_page_first 285 _journal_page_last 290 #============================================================================== data_2018ncs0001_k1_100k_twn_twin1_hklf4 _audit_creation_date 2018-02-12 _audit_creation_method ; Olex2 1.2-alpha (compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5467) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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 'C15 H15 N5 O2' _chemical_formula_sum 'C15 H15 N5 O2' _chemical_formula_weight 297.32 _chemical_melting_point ? _chemical_oxdiff_formula 'C15 H15 N5 O2' _chemical_oxdiff_usercomment TS4 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' _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 8.3683(3) _cell_length_b 13.9986(4) _cell_length_c 12.1610(4) _cell_angle_alpha 90 _cell_angle_beta 97.512(3) _cell_angle_gamma 90 _cell_volume 1412.37(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24269 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.7380 _cell_measurement_theta_min 3.3520 _shelx_estimated_absorpt_T_max 0.998 _shelx_estimated_absorpt_T_min 0.983 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84880 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 624 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 5 0 0.0250 0 0 1 0.0900 -1 -5 0 0.0250 0 0 -1 0.0800 -5 0 1 0.0050 5 0 -1 0.0200 _exptl_crystal_recrystallization_method 'The material was recrystallised from methanol.' _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.025 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9982 4.9901 -0.0008 0.1260 0.0193 0.2344 0.0002 0.0007 0.9978 0.0527 0.0029 -0.0257 -0.9982 -4.9901 0.0008 -0.1260 -0.0193 -0.2344 -0.0002 -0.0007 -0.9978 -0.0527 -0.0029 0.0257 -4.9903 -0.0016 0.9989 -0.0255 -0.4090 -0.1053 4.9903 0.0016 -0.9989 0.0255 0.4090 0.1053 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6057 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.481 _diffrn_reflns_theta_min 2.854 _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.989 _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 -32.00 84.00 1.00 25.00 -- -5.80 63.00 13.32 116 2 \w -34.00 84.00 1.00 25.00 -- -5.80 70.00 -37.72 118 3 \w -34.00 84.00 1.00 25.00 -- -5.80 71.00 78.74 118 4 \w -95.00 14.00 1.00 25.00 -- -5.80 -38.00 150.00 109 5 \w -95.00 19.00 1.00 25.00 -- -5.80 -57.00 -30.00 114 6 \w -34.00 84.00 1.00 25.00 -- -5.80 72.00-180.00 118 7 \w -34.00 84.00 1.00 25.00 -- -5.80 71.00 -95.25 118 8 \w -30.00 84.00 1.00 25.00 -- -5.80 57.00-120.00 114 9 \w -32.00 81.00 1.00 25.00 -- -5.80 63.00 43.83 113 10 \w -31.00 84.00 1.00 25.00 -- -5.80 60.00 138.86 115 ; _diffrn_measurement_device 'four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 FRE-HF' _diffrn_measurement_device_type2 'Rigaku AFC12 (Right)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen MicroMesh' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0156777000 _diffrn_orient_matrix_UB_12 0.0221151000 _diffrn_orient_matrix_UB_13 0.0527856000 _diffrn_orient_matrix_UB_21 0.0825454000 _diffrn_orient_matrix_UB_22 -0.0126500000 _diffrn_orient_matrix_UB_23 0.0029305000 _diffrn_orient_matrix_UB_31 0.0159301000 _diffrn_orient_matrix_UB_32 0.0437849000 _diffrn_orient_matrix_UB_33 -0.0258056000 _diffrn_radiation_collimation 0.3 _diffrn_radiation_monochromator 'Confocal mirrors, HF Varimax' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_current 55.0 _diffrn_source_power 2.475 _diffrn_source_target Mo _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_source_voltage 45.0 _diffrn_special_details ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4474 _reflns_number_total 6057 _reflns_special_details ; _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 1.171.39.34b (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _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 0.279 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 6057 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0474 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1447P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1475 _refine_ls_wR_factor_ref 0.1971 _refine_special_details 'Crystal found to be a non-merohedral twin, Component 2 [41.4(2)%]' _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.586(2) 0.414(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 3.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15) 3.b Idealised Me refined as rotating group: C7(H7A,H7B,H7C) 3.c Idealised tetrahedral OH refined as rotating group: O2(H2A) ; _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 C1 C 0.7587(3) 0.78731(18) -0.0030(2) 0.0248(6) Uani 1 1 d . . . . . H1 H 0.7986 0.8100 -0.0678 0.030 Uiso 1 1 calc R . . . . C2 C 0.7739(3) 0.69069(18) 0.0216(2) 0.0236(6) Uani 1 1 d . . . . . H2 H 0.8228 0.6486 -0.0254 0.028 Uiso 1 1 calc R . . . . C3 C 0.7168(3) 0.65718(17) 0.1152(2) 0.0212(5) Uani 1 1 d . . . . . H3 H 0.7252 0.5913 0.1340 0.025 Uiso 1 1 calc R . . . . C4 C 0.6471(3) 0.72057(16) 0.1815(2) 0.0193(5) Uani 1 1 d . . . . . H4 H 0.6072 0.6991 0.2469 0.023 Uiso 1 1 calc R . . . . C5 C 0.6359(3) 0.81720(16) 0.15099(19) 0.0162(5) Uani 1 1 d . . . . . C6 C 0.5646(3) 0.88769(16) 0.22208(19) 0.0163(5) Uani 1 1 d . . . . . C7 C 0.5665(3) 0.99256(16) 0.1938(2) 0.0222(5) Uani 1 1 d . . . . . H7A H 0.4604 1.0204 0.1995 0.033 Uiso 1 1 calc GR . . . . H7B H 0.5920 1.0003 0.1179 0.033 Uiso 1 1 calc GR . . . . H7C H 0.6484 1.0251 0.2455 0.033 Uiso 1 1 calc GR . . . . C8 C 0.3747(3) 0.88237(16) 0.46301(19) 0.0160(5) Uani 1 1 d . . . . . C9 C 0.2254(3) 0.66091(16) 0.53725(19) 0.0163(5) Uani 1 1 d . . . . . H9 H 0.2512 0.6215 0.4785 0.020 Uiso 1 1 calc R . . . . C10 C 0.1457(3) 0.62067(16) 0.62567(19) 0.0158(5) Uani 1 1 d . . . . . C11 C 0.1069(3) 0.67657(16) 0.7149(2) 0.0169(5) Uani 1 1 d . . . . . C12 C 0.0277(3) 0.63514(18) 0.7967(2) 0.0215(5) Uani 1 1 d . . . . . H12 H 0.0004 0.6731 0.8562 0.026 Uiso 1 1 calc R . . . . C13 C -0.0115(3) 0.53882(19) 0.7918(2) 0.0243(5) Uani 1 1 d . . . . . H13 H -0.0659 0.5113 0.8480 0.029 Uiso 1 1 calc R . . . . C14 C 0.0283(3) 0.48220(17) 0.7052(2) 0.0230(5) Uani 1 1 d . . . . . H14 H 0.0022 0.4161 0.7023 0.028 Uiso 1 1 calc R . . . . C15 C 0.1060(3) 0.52301(16) 0.6237(2) 0.0191(5) Uani 1 1 d . . . . . H15 H 0.1334 0.4843 0.5648 0.023 Uiso 1 1 calc R . . . . N1 N 0.6909(2) 0.85051(14) 0.05959(17) 0.0202(5) Uani 1 1 d . . . . . N2 N 0.5020(2) 0.85256(13) 0.30396(15) 0.0157(4) Uani 1 1 d . . . . . N3 N 0.4453(2) 0.91733(13) 0.37563(16) 0.0174(4) Uani 1 1 d . . . . . H3A H 0.503(3) 0.974(2) 0.398(2) 0.023(7) Uiso 1 1 d . . . . . N4 N 0.3379(2) 0.78679(13) 0.45740(16) 0.0166(4) Uani 1 1 d . . . . . H4A H 0.353(4) 0.755(2) 0.391(3) 0.044(9) Uiso 1 1 d . . . . . N5 N 0.2608(2) 0.75019(13) 0.53904(16) 0.0161(4) Uani 1 1 d . . . . . O1 O 0.3439(2) 0.93393(11) 0.53910(14) 0.0202(4) Uani 1 1 d . . . . . O2 O 0.1469(2) 0.77061(11) 0.72654(14) 0.0205(4) Uani 1 1 d . . . . . H2A H 0.1906 0.7886 0.6717 0.031 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0289(13) 0.0283(13) 0.0193(12) -0.0025(10) 0.0105(10) -0.0042(10) C2 0.0209(12) 0.0266(13) 0.0249(13) -0.0092(10) 0.0091(10) -0.0014(10) C3 0.0199(12) 0.0175(11) 0.0260(13) -0.0028(9) 0.0018(10) 0.0004(9) C4 0.0200(11) 0.0197(11) 0.0184(12) 0.0007(9) 0.0032(9) -0.0006(9) C5 0.0140(10) 0.0187(11) 0.0155(11) -0.0014(9) 0.0005(8) -0.0025(8) C6 0.0158(11) 0.0158(11) 0.0173(11) -0.0013(9) 0.0017(9) -0.0009(8) C7 0.0297(13) 0.0176(11) 0.0204(12) 0.0011(9) 0.0077(10) -0.0009(9) C8 0.0152(10) 0.0155(10) 0.0171(11) -0.0010(9) 0.0014(9) -0.0003(8) C9 0.0173(11) 0.0165(11) 0.0151(11) -0.0028(9) 0.0017(9) 0.0010(8) C10 0.0139(10) 0.0161(11) 0.0169(11) 0.0012(9) -0.0007(9) -0.0007(8) C11 0.0154(10) 0.0166(11) 0.0185(11) 0.0014(9) 0.0013(9) 0.0008(8) C12 0.0177(11) 0.0279(13) 0.0197(12) 0.0010(10) 0.0057(9) -0.0005(9) C13 0.0186(11) 0.0316(13) 0.0227(12) 0.0102(10) 0.0031(10) -0.0039(10) C14 0.0232(12) 0.0185(11) 0.0260(13) 0.0061(10) -0.0017(10) -0.0044(9) C15 0.0199(11) 0.0166(11) 0.0198(12) -0.0001(9) -0.0014(9) -0.0013(9) N1 0.0227(10) 0.0210(10) 0.0174(10) -0.0019(8) 0.0042(8) -0.0031(8) N2 0.0184(9) 0.0147(9) 0.0142(10) -0.0024(7) 0.0033(8) -0.0003(7) N3 0.0225(10) 0.0139(9) 0.0169(10) -0.0033(8) 0.0070(8) -0.0030(7) N4 0.0214(10) 0.0146(9) 0.0148(10) -0.0014(7) 0.0062(8) -0.0033(7) N5 0.0178(9) 0.0164(9) 0.0140(9) 0.0006(7) 0.0020(8) -0.0007(7) O1 0.0255(9) 0.0165(8) 0.0197(9) -0.0048(6) 0.0072(7) -0.0029(6) O2 0.0283(9) 0.0156(8) 0.0193(9) -0.0017(7) 0.0095(7) -0.0007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1 0.9500 . ? C1 C2 1.387(4) . ? C1 N1 1.340(3) . ? C2 H2 0.9500 . ? C2 C3 1.374(3) . ? C3 H3 0.9500 . ? C3 C4 1.379(3) . ? C4 H4 0.9500 . ? C4 C5 1.403(3) . ? C5 C6 1.488(3) . ? C5 N1 1.341(3) . ? C6 C7 1.508(3) . ? C6 N2 1.282(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N3 1.372(3) . ? C8 N4 1.373(3) . ? C8 O1 1.227(3) . ? C9 H9 0.9500 . ? C9 C10 1.451(3) . ? C9 N5 1.284(3) . ? C10 C11 1.410(3) . ? C10 C15 1.406(3) . ? C11 C12 1.392(3) . ? C11 O2 1.361(3) . ? C12 H12 0.9500 . ? C12 C13 1.387(3) . ? C13 H13 0.9500 . ? C13 C14 1.394(4) . ? C14 H14 0.9500 . ? C14 C15 1.378(3) . ? C15 H15 0.9500 . ? N2 N3 1.384(3) . ? N3 H3A 0.95(3) . ? N4 H4A 0.95(3) . ? N4 N5 1.354(3) . ? O2 H2A 0.8400 . ? 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 C2 C1 H1 118.1 . . ? N1 C1 H1 118.1 . . ? N1 C1 C2 123.7(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 C1 118.6(2) . . ? C3 C2 H2 120.7 . . ? C2 C3 H3 120.5 . . ? C2 C3 C4 119.0(2) . . ? C4 C3 H3 120.5 . . ? C3 C4 H4 120.5 . . ? C3 C4 C5 119.0(2) . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.2(2) . . ? N1 C5 C4 122.5(2) . . ? N1 C5 C6 117.3(2) . . ? C5 C6 C7 119.72(19) . . ? N2 C6 C5 115.6(2) . . ? N2 C6 C7 124.6(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N4 115.22(19) . . ? O1 C8 N3 121.9(2) . . ? O1 C8 N4 122.9(2) . . ? C10 C9 H9 120.2 . . ? N5 C9 H9 120.2 . . ? N5 C9 C10 119.5(2) . . ? C11 C10 C9 121.95(19) . . ? C15 C10 C9 119.7(2) . . ? C15 C10 C11 118.4(2) . . ? C12 C11 C10 119.9(2) . . ? O2 C11 C10 122.6(2) . . ? O2 C11 C12 117.5(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C12 C13 H13 119.8 . . ? C12 C13 C14 120.4(2) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.3 . . ? C15 C14 C13 119.4(2) . . ? C15 C14 H14 120.3 . . ? C10 C15 H15 119.2 . . ? C14 C15 C10 121.5(2) . . ? C14 C15 H15 119.2 . . ? C1 N1 C5 117.2(2) . . ? C6 N2 N3 116.51(18) . . ? C8 N3 N2 118.15(18) . . ? C8 N3 H3A 109.7(17) . . ? N2 N3 H3A 121.2(16) . . ? C8 N4 H4A 117(2) . . ? N5 N4 C8 117.26(19) . . ? N5 N4 H4A 125(2) . . ? C9 N5 N4 119.14(19) . . ? C11 O2 H2A 109.5 . . ? 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 N3 H3A O1 0.95(3) 1.91(3) 2.836(3) 166(2) 3_676 O2 H2A N5 0.84 1.87 2.600(2) 145.0 . 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 C1 C2 C3 C4 -0.2(4) . . . . ? C2 C1 N1 C5 0.3(4) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 -178.7(2) . . . . ? C3 C4 C5 N1 -0.1(3) . . . . ? C4 C5 C6 C7 174.6(2) . . . . ? C4 C5 C6 N2 -6.5(3) . . . . ? C4 C5 N1 C1 -0.2(3) . . . . ? C5 C6 N2 N3 175.54(18) . . . . ? C6 C5 N1 C1 178.4(2) . . . . ? C6 N2 N3 C8 178.8(2) . . . . ? C7 C6 N2 N3 -5.7(3) . . . . ? C8 N4 N5 C9 -179.4(2) . . . . ? C9 C10 C11 C12 178.8(2) . . . . ? C9 C10 C11 O2 -2.7(3) . . . . ? C9 C10 C15 C14 -179.1(2) . . . . ? C10 C9 N5 N4 178.73(18) . . . . ? C10 C11 C12 C13 0.8(3) . . . . ? C11 C10 C15 C14 1.2(3) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? C13 C14 C15 C10 -0.2(4) . . . . ? C15 C10 C11 C12 -1.5(3) . . . . ? C15 C10 C11 O2 177.0(2) . . . . ? N1 C1 C2 C3 -0.1(4) . . . . ? N1 C5 C6 C7 -4.0(3) . . . . ? N1 C5 C6 N2 174.8(2) . . . . ? N3 C8 N4 N5 -176.78(19) . . . . ? N4 C8 N3 N2 -12.9(3) . . . . ? N5 C9 C10 C11 -0.6(3) . . . . ? N5 C9 C10 C15 179.7(2) . . . . ? O1 C8 N3 N2 168.7(2) . . . . ? O1 C8 N4 N5 1.6(3) . . . . ? O2 C11 C12 C13 -177.8(2) . . . . ? _shelx_res_file ; 2018ncs0001_k1_100k_twn_twin1_hklf4.res created by SHELXL-2014/7 TITL 2018ncs0001_k1_100k_twn_twin1_hklf4_a.res in P2(1)/c REM Old TITL 2018ncs0001_K1_100K_TWN_twin1_hklf4 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.122, Rweak 0.006, Alpha 0.025, Orientation as input REM Formula found by SHELXT: C15 N5 O2 CELL 0.71075 8.3683 13.9986 12.161 90 97.512 90 ZERR 4 0.0003 0.0004 0.0004 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 60 60 20 8 EQIV $1 1-X,2-Y,1-Z L.S. 40 PLAN 6 SIZE 0.025 0.06 0.175 TEMP -173(2) HTAB N3 O1_$1 HTAB O2 N5 BOND $H fmap 2 acta MORE -1 CONF OMIT -3 57 OMIT -2 8 -6 REM REM REM WGHT 0.144700 BASF 0.41371 FVAR 7.99915 C1 1 0.758710 0.787314 -0.002964 11.00000 0.02889 0.02831 = 0.01926 -0.00252 0.01050 -0.00425 AFIX 43 H1 2 0.798603 0.809961 -0.067802 11.00000 -1.20000 AFIX 0 C2 1 0.773929 0.690693 0.021575 11.00000 0.02094 0.02658 = 0.02487 -0.00917 0.00907 -0.00137 AFIX 43 H2 2 0.822825 0.648574 -0.025399 11.00000 -1.20000 AFIX 0 C3 1 0.716810 0.657177 0.115240 11.00000 0.01986 0.01747 = 0.02597 -0.00280 0.00179 0.00042 AFIX 43 H3 2 0.725245 0.591336 0.134031 11.00000 -1.20000 AFIX 0 C4 1 0.647071 0.720575 0.181526 11.00000 0.02001 0.01967 = 0.01842 0.00071 0.00318 -0.00062 AFIX 43 H4 2 0.607173 0.699139 0.246877 11.00000 -1.20000 AFIX 0 C5 1 0.635941 0.817203 0.150986 11.00000 0.01396 0.01873 = 0.01547 -0.00141 0.00050 -0.00248 C6 1 0.564560 0.887691 0.222080 11.00000 0.01578 0.01583 = 0.01728 -0.00134 0.00166 -0.00087 C7 1 0.566505 0.992558 0.193766 11.00000 0.02972 0.01761 = 0.02039 0.00111 0.00768 -0.00088 AFIX 137 H7A 2 0.460427 1.020356 0.199483 11.00000 -1.50000 H7B 2 0.591994 1.000342 0.117883 11.00000 -1.50000 H7C 2 0.648359 1.025108 0.245535 11.00000 -1.50000 AFIX 0 C8 1 0.374725 0.882365 0.463005 11.00000 0.01522 0.01551 = 0.01710 -0.00099 0.00144 -0.00031 C9 1 0.225401 0.660914 0.537249 11.00000 0.01732 0.01655 = 0.01506 -0.00276 0.00168 0.00102 AFIX 43 H9 2 0.251215 0.621491 0.478473 11.00000 -1.20000 AFIX 0 C10 1 0.145710 0.620665 0.625671 11.00000 0.01386 0.01609 = 0.01687 0.00123 -0.00066 -0.00067 C11 1 0.106862 0.676573 0.714886 11.00000 0.01543 0.01663 = 0.01852 0.00139 0.00133 0.00079 C12 1 0.027718 0.635141 0.796673 11.00000 0.01767 0.02789 = 0.01973 0.00097 0.00565 -0.00048 AFIX 43 H12 2 0.000374 0.673086 0.856234 11.00000 -1.20000 AFIX 0 C13 1 -0.011527 0.538824 0.791840 11.00000 0.01865 0.03157 = 0.02269 0.01016 0.00315 -0.00392 AFIX 43 H13 2 -0.065903 0.511288 0.847954 11.00000 -1.20000 AFIX 0 C14 1 0.028325 0.482205 0.705174 11.00000 0.02323 0.01851 = 0.02602 0.00613 -0.00170 -0.00437 AFIX 43 H14 2 0.002190 0.416134 0.702292 11.00000 -1.20000 AFIX 0 C15 1 0.106028 0.523007 0.623679 11.00000 0.01990 0.01662 = 0.01976 -0.00012 -0.00143 -0.00134 AFIX 43 H15 2 0.133415 0.484256 0.564793 11.00000 -1.20000 AFIX 0 N1 3 0.690936 0.850514 0.059589 11.00000 0.02266 0.02102 = 0.01737 -0.00187 0.00422 -0.00307 N2 3 0.502003 0.852561 0.303964 11.00000 0.01842 0.01466 = 0.01421 -0.00243 0.00334 -0.00035 N3 3 0.445294 0.917334 0.375632 11.00000 0.02250 0.01390 = 0.01691 -0.00330 0.00703 -0.00296 H3A 2 0.503372 0.973631 0.397542 11.00000 0.02317 N4 3 0.337892 0.786793 0.457402 11.00000 0.02138 0.01463 = 0.01484 -0.00138 0.00617 -0.00326 H4A 2 0.352734 0.754798 0.390715 11.00000 0.04423 N5 3 0.260759 0.750191 0.539040 11.00000 0.01783 0.01636 = 0.01404 0.00058 0.00200 -0.00066 O1 4 0.343917 0.933932 0.539102 11.00000 0.02554 0.01654 = 0.01968 -0.00481 0.00724 -0.00288 O2 4 0.146870 0.770607 0.726544 11.00000 0.02827 0.01558 = 0.01926 -0.00171 0.00947 -0.00068 AFIX 147 H2A 2 0.190563 0.788561 0.671691 11.00000 -1.50000 AFIX 0 HKLF 5 REM 2018ncs0001_k1_100k_twn_twin1_hklf4_a.res in P2(1)/c REM R1 = 0.0474 for 4474 Fo > 4sig(Fo) and 0.0698 for all 6057 data REM 210 parameters refined using 0 restraints END WGHT 0.1447 0.0000 REM Highest difference peak 0.279, deepest hole -0.233, 1-sigma level 0.052 Q1 1 0.1234 0.5679 0.6310 11.00000 0.05 0.25 Q2 1 0.6232 0.7497 0.1591 11.00000 0.05 0.24 Q3 1 0.1018 0.6481 0.6592 11.00000 0.05 0.23 Q4 1 0.0278 0.5148 0.7591 11.00000 0.05 0.23 Q5 1 0.4660 0.8898 0.3412 11.00000 0.05 0.22 Q6 1 0.0291 0.5825 0.7958 11.00000 0.05 0.22 ; _shelx_res_checksum 9376 _shelx_hkl_file ; 0 0 -2 2966.92 144.142 1 0 0 4 158457. 2504.23 1 1 0 -6 23682.5 495.214 -2 0 0 -6 23682.5 495.214 1 0 0 8 7916.66 364.178 1 0 0 10 622.090 360.096 1 -2 0 12 182132. 1303.89 -2 0 0 12 182132. 1303.89 1 0 0 14 716.212 431.841 1 0 1 2 169597. 1927.38 1 0 1 3 32664.7 252.890 1 0 -1 -4 1384.06 151.479 1 -1 -1 5 73254.7 603.375 -2 0 1 5 73254.7 603.375 1 0 -1 6 23591.9 605.441 1 -1 -1 6 36728.9 406.490 -2 0 1 6 36728.9 406.490 1 0 -1 -7 1276.07 188.373 1 0 -1 -8 1702.29 206.550 1 0 -1 -9 1210.48 223.754 1 0 1 10 15243.0 380.637 1 -2 1 11 1541.86 358.693 -2 0 -1 11 1541.86 358.693 1 -2 -1 12 12826.5 443.983 -2 0 1 12 12826.5 443.983 1 0 -1 13 6825.76 350.630 1 0 -1 14 4929.89 351.355 1 0 1 15 2277.34 346.902 1 0 2 2 112660. 1201.45 1 0 2 3 1809.96 141.177 1 0 2 4 113338. 479.155 1 -1 -2 5 3307.83 242.309 -2 0 2 5 3307.83 242.309 1 1 2 -6 3687.99 311.633 -2 0 -2 -6 3687.99 311.633 1 0 -2 -7 8321.51 235.647 1 0 -2 8 115.922 205.052 1 0 2 9 222.061 224.154 1 0 -2 10 10565.9 344.523 1 2 2 -10 10152.8 855.066 -2 0 -2 -10 10152.8 855.066 1 -2 -2 11 94517.8 867.730 -2 0 2 11 94517.8 867.730 1 0 2 12 5696.71 618.771 1 -2 -2 12 5270.43 403.002 -2 0 2 12 5270.43 403.002 1 0 2 13 28717.3 526.498 1 0 -2 14 1035.63 348.153 1 0 -2 15 45.6568 331.622 1 0 3 1 6065.64 87.3349 1 0 3 1 10737.7 262.600 -2 0 -3 1 10737.7 262.600 1 0 -3 -2 27854.1 173.788 1 0 -3 -3 82954.4 343.925 1 0 -3 -4 118842. 448.435 1 1 3 -5 68068.3 444.385 -2 0 -3 -5 68068.3 444.385 1 0 -3 -6 31567.6 3955.54 1 -1 -3 6 244742. 1228.52 -2 0 3 6 244742. 1228.52 1 0 3 7 3551.94 213.087 1 0 -3 -8 4261.58 233.992 1 0 -3 -9 3647.17 245.243 1 0 -3 10 611.790 329.124 1 -2 -3 10 1719.98 562.701 -2 0 3 10 1719.98 562.701 1 -2 -3 11 14244.7 473.964 -2 0 3 11 14244.7 473.964 1 2 3 -12 1807.11 397.335 -2 0 -3 -12 1807.11 397.335 1 0 3 13 25512.4 504.427 1 0 3 14 88.9661 315.464 1 0 -3 15 386.553 336.677 1 0 4 0 435.192 109.505 -2 0 -4 0 435.192 109.505 1 0 -4 -1 731.629 90.0493 1 0 4 1 1264.06 190.603 -2 0 -4 1 1264.06 190.603 1 0 -4 2 12685.9 134.518 1 0 -4 3 8491.16 166.444 1 0 4 4 27061.9 267.519 1 -1 -4 5 70302.1 529.928 -2 0 4 5 70302.1 529.928 1 1 4 -6 4333.46 282.606 -2 0 -4 -6 4333.46 282.606 1 0 4 7 78157.4 675.706 1 0 4 8 155.564 219.929 1 0 -4 -9 190.829 232.615 1 0 -4 10 752.961 362.931 1 2 4 -10 4699.55 508.237 -2 0 -4 -10 4699.55 508.237 1 -2 4 11 5852.06 413.715 -2 0 -4 11 5852.06 413.715 1 -2 -4 12 6080.05 510.635 -2 0 4 12 6080.05 510.635 1 0 -4 13 2547.11 329.928 1 0 4 14 293.812 355.901 1 0 4 15 206.712 351.796 1 0 5 1 27861.6 175.251 1 0 -5 2 10597.2 127.363 1 0 5 3 6934.97 140.887 1 0 5 4 8888.33 180.885 1 1 5 -5 59687.0 400.255 -2 0 -5 -5 59687.0 400.255 1 0 5 6 15051.5 372.343 1 1 5 -6 42870.3 467.194 -2 0 -5 -6 42870.3 467.194 1 0 -5 -7 2975.70 217.892 1 0 5 8 3643.96 272.749 1 0 -5 9 102.592 239.128 1 0 -5 10 609.471 498.300 1 -2 -5 10 7008.50 448.484 -2 0 5 10 7008.50 448.484 1 -2 -5 11 323.345 332.039 -2 0 5 11 323.345 332.039 1 -2 -5 12 6781.91 422.785 -2 0 5 12 6781.91 422.785 1 0 5 13 1673.23 323.386 1 0 5 14 239.233 357.890 1 0 -6 0 92321.4 612.779 -2 0 6 0 92321.4 612.779 1 0 -6 1 90804.3 350.655 1 0 -6 1 154702. 522.638 -2 0 6 1 154702. 522.638 1 0 6 2 30032.6 189.157 1 0 -6 3 10928.2 164.615 1 0 -6 4 5511.05 148.832 1 -1 -6 5 45763.3 381.620 -2 0 6 5 45763.3 381.620 1 0 6 6 599.608 299.988 1 -1 6 6 11456.7 287.908 -2 0 -6 6 11456.7 287.908 1 0 6 7 14668.3 296.234 1 0 6 8 9702.43 325.196 1 0 6 9 20.0417 282.049 1 0 -6 10 8609.55 644.974 1 -2 -6 10 11251.1 477.878 -2 0 6 10 11251.1 477.878 1 -2 6 11 4664.63 422.600 -2 0 -6 11 4664.63 422.600 1 -2 -6 12 963.793 408.631 -2 0 6 12 963.793 408.631 1 0 6 13 23.0964 314.315 1 0 -6 14 3165.46 396.693 1 0 7 1 125259. 439.241 1 0 -7 1 218327. 805.237 -2 0 7 1 218327. 805.237 1 0 -7 -2 8126.02 146.731 1 0 -7 -3 113.514 110.331 1 0 -7 4 20164.9 254.480 1 0 7 5 737.663 252.627 1 -1 -7 5 580.904 182.752 -2 0 7 5 580.904 182.752 1 1 7 -6 10028.4 291.172 -2 0 -7 -6 10028.4 291.172 1 0 -7 -7 9276.37 239.767 1 0 -7 -8 18642.2 304.812 1 0 7 9 5450.12 281.953 1 0 -7 10 640.417 545.280 1 2 7 -10 910.362 432.488 -2 0 -7 -10 910.362 432.488 1 -2 -7 11 29623.0 733.783 -2 0 7 11 29623.0 733.783 1 2 7 -12 1007.37 424.490 -2 0 -7 -12 1007.37 424.490 1 0 -7 13 7367.08 531.380 1 0 -7 14-145.085 386.486 1 0 8 0 40917.7 331.822 -2 0 -8 0 40917.7 331.822 1 0 -8 1 58092.7 746.705 1 0 8 1 98514.6 344.242 -2 0 -8 1 98514.6 344.242 1 0 -8 2 31417.2 216.237 1 0 -8 3 19123.0 188.499 1 0 -8 4 913.057 135.796 1 0 8 -5 2974.96 272.126 1 -1 8 5 4021.17 220.093 -2 0 -8 5 4021.17 220.093 1 -1 8 6 12625.4 319.858 -2 0 -8 6 12625.4 319.858 1 0 -8 -7 17680.7 283.877 1 0 8 8 4681.80 262.748 1 0 8 9 7446.79 277.798 1 0 -8 10 3602.38 537.864 1 2 8 -10 20403.1 553.808 -2 0 -8 -10 20403.1 553.808 1 -2 -8 11 266.059 324.452 -2 0 8 11 266.059 324.452 1 -2 8 12 6277.94 514.913 -2 0 -8 12 6277.94 514.913 1 0 -8 13 299.409 367.699 1 0 9 1 20.9687 144.253 -2 0 -9 1 20.9687 144.253 1 0 -9 2 3999.83 134.223 1 0 -9 -3 4545.18 145.387 1 0 9 4 46808.3 342.365 1 0 9 5 1318.20 312.746 1 -1 -9 5 6896.53 266.729 -2 0 9 5 6896.53 266.729 1 0 -9 -6 25106.9 567.160 1 -1 9 6 45759.8 496.336 -2 0 -9 6 45759.8 496.336 1 0 9 7 4467.52 211.845 1 0 -9 8 2094.15 196.197 1 0 9 9 18518.4 427.644 1 0 -9 10 2576.11 333.447 1 -2 -9 10 3092.66 468.384 -2 0 9 10 3092.66 468.384 1 -2 -9 11 4737.02 512.137 -2 0 9 11 4737.02 512.137 1 0 9 12 1922.20 547.019 1 -2 9 12 5518.55 516.273 -2 0 -9 12 5518.55 516.273 1 0 -9 13 827.897 397.377 1 0 10 0 2076.77 188.232 -2 0 -10 0 2076.77 188.232 1 0 -10 1 2096.22 167.137 -2 0 10 1 2096.22 167.137 1 0 -10 2 1345.56 133.595 1 0 -10 3 26478.7 238.944 1 0 10 4 548.470 162.768 1 0 10 5 10148.5 584.279 1 1 10 -5 11168.7 290.571 -2 0 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452.689 2 -1 -15 7 1983.32 393.961 2 -1 -15 4 23.2992 242.437 2 -1 15 3 257.465 214.692 2 -1 15 2 2375.65 227.566 2 1 15 -1 88.0307 521.661 2 1 15 1 33.7370 318.387 2 1 15 2 134.967 207.380 2 1 -15 3 4794.59 303.368 2 1 15 4 221.089 261.206 2 1 15 6 1655.16 556.284 2 1 15 7 584.093 266.607 2 1 -15 8 405.852 479.711 2 -1 -16 7 1615.59 639.713 2 -1 -16 4 241.889 411.430 2 -1 -16 3 48.5799 308.099 2 -1 -16 2 1685.15 287.579 2 1 16 1 4448.52 403.504 2 1 16 2 2111.79 309.080 2 1 16 3 31.5604 317.151 2 1 16 4 4315.79 360.402 2 1 -16 7 162.750 487.783 2 -1 -17 4 1857.02 599.501 2 -1 -17 3 5454.91 499.804 2 -1 -17 2 5.93342 338.691 2 -1 -17 -1 597.944 523.385 2 1 -17 2-84.6331 382.117 2 1 -17 3 3933.95 667.291 2 1 -17 4 1048.83 461.076 2 -1 -18 -1 15.9468 546.302 2 -2 0 14 1435.15 435.605 2 -2 0 10 121642. 990.922 2 -2 0 8 22860.2 617.382 2 -2 0 4 121659. 1012.60 2 -2 0 -4 2304.91 105.854 2 2 0 8 764.643 146.631 2 2 0 10 2951.72 199.851 2 2 0 12 214.356 204.457 2 2 0 14 21072.6 949.060 2 -2 1 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2 -8 1339.38 155.453 2 -2 2 -9 4512.37 194.809 2 2 -2 10 1475.60 244.180 2 2 -2 13 3209.20 270.892 2 2 2 14 1503.41 492.255 2 -2 3 15 248.533 324.105 2 -2 3 14 2333.02 328.343 2 -2 3 13 25.9361 292.089 2 -2 3 12 24.5008 621.590 2 -2 3 10 1206.67 331.833 2 -2 -3 9 1849.39 248.622 2 -2 -3 8 747.118 225.685 2 -2 -3 7 2813.53 225.704 2 2 -3 -6 815.010 263.645 2 2 3 -4 28235.1 414.877 2 2 3 -3 496.924 145.764 2 2 3 -2 60665.7 348.396 2 2 3 -1 28469.2 195.474 2 2 3 1 14503.2 102.882 2 -2 3 -2 5052.26 78.4115 2 2 -3 3 7851.45 90.1563 2 2 -3 4 1623.37 138.384 2 -2 3 -6-227.335 367.681 2 -2 3 -7 9277.73 186.429 2 -2 3 -8 4602.03 179.617 2 -2 3 -9 3078.09 196.556 2 2 -3 10 423.750 255.734 2 2 -3 13 6308.19 274.929 2 2 -3 14 7501.49 340.252 2 -2 -4 15 537.617 322.256 2 -2 4 14 28.5093 285.782 2 -2 4 13 74.9876 298.597 2 -2 -4 10 3539.65 419.987 2 -2 -4 9 24.0130 242.242 2 -2 -4 8 3646.31 251.894 2 -2 -4 7 3.90474 241.852 2 2 4 -4 107370. 542.292 2 2 4 -3 35628.4 276.610 2 2 4 -2 2091.28 113.369 2 2 4 -1 3141.90 153.867 2 -2 4 -1 1756.18 74.1272 2 -2 4 -2 268.445 74.8907 2 2 -4 3 3347.87 85.5449 2 2 -4 4 1388.30 105.396 2 2 4 5 2110.13 116.003 2 2 -4 6 15185.9 401.798 2 2 -4 7 896.673 168.694 2 -2 4 -8 3227.76 183.735 2 -2 4 -9 11210.6 243.203 2 2 -4 10 1042.45 243.922 2 2 -4 13 8779.33 336.311 2 2 -4 14-19.2225 301.484 2 -2 -5 15 2951.16 352.080 2 -2 -5 14 596.476 309.737 2 -2 5 13 6193.48 343.139 2 -2 5 10 6033.29 598.671 2 2 5 -9 386.454 252.761 2 2 5 -8 774.650 269.766 2 2 5 -7 1825.50 261.846 2 -2 5 6-39432.7 514.143 2 2 5 -4 24.6560 149.742 2 2 5 -3 3484.23 160.104 2 -2 -5 2 41437.8 252.018 2 2 5 -1 6187.14 187.300 2 2 5 1 7360.09 119.292 2 -2 5 -2 2764.68 95.0192 2 -2 5 -3 28613.9 184.348 2 2 -5 4 1230.69 99.7310 2 2 -5 7 396.991 68.2181 2 2 -5 8 776.869 197.006 2 2 -5 9 56.5064 189.645 2 2 -5 10 17.0582 247.881 2 -2 -5 -11 305.104 328.644 2 2 -5 13 3688.90 288.975 2 2 -5 14 2883.51 337.205 2 -2 6 14 552.024 354.480 2 -2 6 13 2819.33 330.325 2 -2 6 10 1691.76 549.843 2 2 6 -9 7674.16 349.683 2 2 6 -8 1699.74 284.227 2 2 6 -7 1949.58 199.160 2 2 6 -6 9479.73 371.955 2 2 6 -4 28717.0 300.674 2 -2 -6 3 1665.04 148.457 2 -2 -6 2 1760.23 117.496 2 2 6 -1 2379.78 175.823 2 2 6 1 261.535 128.594 2 -2 -6 -2 65731.7 265.028 2 -2 6 -3 18585.8 153.700 2 2 -6 4 3626.59 123.339 2 -2 -6 -6 1727.97 498.396 2 2 -6 7 3899.55 143.594 2 2 -6 8 19543.0 194.023 2 2 -6 9 796.005 217.215 2 2 -6 10 3722.69 540.332 2 2 -6 13 45.2032 277.119 2 2 -6 14 1131.74 462.040 2 -2 7 14-80.6323 360.616 2 -2 -7 13 371.563 353.508 2 -2 7 10 165.747 526.512 2 2 7 -9 3729.28 267.987 2 2 7 -8 722.337 233.177 2 2 7 -7 8429.01 245.532 2 -2 -7 4 16822.8 259.380 2 -2 7 3 9625.97 157.868 2 -2 -7 2 11217.5 157.770 2 2 7 -1 31747.1 384.328 2 2 7 1 101293. 545.857 2 -2 7 -2 1470.94 93.5130 2 2 -7 3 74.3004 95.3696 2 2 -7 4 1601.04 119.254 2 2 -7 7 10868.4 188.792 2 2 7 8 630.097 129.311 2 2 -7 9 17804.9 210.895 2 -2 7 -13 6308.83 330.809 2 -2 8 14-6.90147 372.998 2 -2 -8 13 1991.25 379.651 2 -2 8 10 15824.5 688.976 2 -2 -8 9 4902.57 292.577 2 -2 -8 8 353.391 217.943 2 -2 -8 7 351.613 210.139 2 -2 -8 4 22010.2 239.653 2 -2 -8 3 1249.38 130.171 2 -2 -8 2 640.625 118.219 2 2 8 -1 1456.54 284.605 2 -2 -8 -1 839.172 174.441 2 -2 8 -2 16372.8 155.984 2 -2 8 -3 19753.2 182.719 2 2 -8 4 59.1554 117.778 2 2 -8 5 41.2247 394.614 2 2 -8 7 2017.42 150.462 2 2 -8 8 2012.09 154.537 2 2 -8 9 2712.03 128.174 2 2 8 10 36.2051 108.881 2 2 -8 13 567.817 301.521 2 -2 -9 13 1257.62 299.501 2 -2 9 10-38.1485 522.567 2 -2 -9 9 8500.17 296.719 2 -2 -9 8 666.365 208.671 2 -2 -9 7 63767.7 592.389 2 2 -9 -5 3107.51 322.852 2 -2 -9 4 5145.65 181.740 2 -2 -9 3 11782.5 187.725 2 -2 -9 2 19391.7 205.540 2 2 9 -1 2984.73 333.472 2 2 9 1 10803.5 346.675 2 -2 9 -2 180.680 105.339 2 -2 9 -3 2498.39 130.702 2 -2 9 -4 64.3303 134.175 2 2 9 7 708.227 166.787 2 2 -9 8 5890.51 192.608 2 2 -9 9 295.855 160.760 2 2 9 10 62.3184 142.428 2 -2 -10 13 2053.08 414.266 2 -2 10 10 1734.58 357.075 2 -2 -10 9 1214.42 230.208 2 -2 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2 -2 12 3 38369.7 317.563 2 -2 12 2 223.620 161.245 2 2 12 1 1288.51 374.924 2 -2 12 -2-57.3000 148.548 2 -2 12 -3 7534.00 196.783 2 -2 12 -4 567.620 171.975 2 -2 12 -5 8157.88 761.893 2 2 -12 7 47.1498 217.698 2 2 -12 8 9191.86 298.609 2 2 -12 9 15865.4 323.757 2 2 12 10 1900.26 472.070 2 -2 -13 10 148.218 384.189 2 -2 -13 9 276.203 331.138 2 -2 -13 8 3780.14 354.868 2 -2 -13 7 8013.70 327.376 2 -2 -13 5 2632.97 683.119 2 -2 -13 4 9019.88 252.856 2 -2 13 3-30.4402 177.317 2 -2 13 2 2431.04 186.966 2 -2 -13 -1 3397.75 401.140 2 -2 13 -2 719.059 162.677 2 -2 13 -3 7180.60 221.181 2 2 -13 4 2190.76 203.902 2 2 -13 7 7756.96 310.629 2 2 -13 8 1403.18 244.875 2 2 -13 9 1745.98 317.996 2 -2 -14 9 1.12557 450.472 2 -2 -14 8 79.4410 422.291 2 -2 14 7 8277.25 472.258 2 -2 14 4 238.551 210.514 2 -2 14 3 277.711 190.644 2 -2 14 2 926.360 188.778 2 2 14 1 382.743 291.808 2 -2 14 -2 48.8449 171.836 2 -2 14 -3 310.851 216.006 2 2 14 4 1498.49 252.004 2 2 -14 7 3247.84 265.960 2 2 -14 8 990.587 323.266 2 2 -14 9-39.2255 681.641 2 -2 -15 8 14676.2 600.303 2 -2 -15 7 868.482 572.017 2 -2 -15 4 1101.60 328.384 2 -2 -15 3 1388.83 267.662 2 -2 -15 2 6542.26 342.517 2 2 15 1 417.664 319.654 2 2 15 2 316.627 208.599 2 2 15 3 2316.97 309.820 2 2 15 4 5581.30 336.779 2 2 15 7 169.533 350.690 2 -2 -16 7 448.521 597.840 2 2 -16 -5 111.514 625.380 2 -2 -16 4 1958.22 423.613 2 -2 -16 3 351.373 280.934 2 -2 -16 2 608.900 279.331 2 2 16 -1 167.477 575.215 2 2 16 1 295.632 345.551 2 2 16 2 731.123 291.769 2 2 16 3 1242.02 331.374 2 2 16 4 1917.18 329.302 2 -2 -17 4 975.203 445.193 2 -2 -17 3 217.190 345.224 2 -2 -17 2 225.004 335.154 2 2 -17 -1 7246.75 699.830 2 -2 -17 -1 55.6259 366.115 2 2 17 2 166.598 308.514 2 2 17 3 492.832 398.075 2 2 -17 4 1503.72 699.771 2 -3 0 14 1503.46 463.031 2 -3 0 10 8238.07 484.251 2 -3 0 8 100476. 1227.99 2 -3 0 6 3714.03 457.548 2 -3 0 4 2720.40 490.974 2 -3 0 2 26820.6 609.739 2 3 0 2 50198.7 281.690 2 3 0 4 4696.33 124.815 2 3 0 8 4982.21 454.950 2 3 0 10 9424.75 602.662 2 3 0 14 1301.74 656.568 2 -3 1 15 207.285 348.036 2 -3 1 14 7059.54 382.354 2 -3 1 13 771.526 325.962 2 -3 1 10 57777.9 739.395 2 -3 1 9 23.3623 304.849 2 -3 1 8 1705.05 290.936 2 -3 -1 7 2903.44 286.021 2 3 1 -4 175.965 261.301 2 -3 -1 3 2402.95 313.793 2 -3 1 2 111.784 182.765 2 -3 -1 1 23965.4 511.374 2 -3 1 -1 34212.9 150.444 2 3 1 2 8384.12 98.3060 2 3 1 3 16012.2 134.136 2 3 -1 4 94.0029 108.153 2 -3 1 -6 14605.9 543.708 2 -3 1 -7 3541.89 175.342 2 3 1 8 22107.7 278.884 2 -3 1 -9 1375.23 205.699 2 3 -1 10 2184.92 492.644 2 3 1 13 8854.59 509.160 2 3 1 14 483.922 459.289 2 -3 2 15-373.330 348.507 2 -3 2 14 1503.92 375.334 2 -3 2 13 3949.36 354.924 2 -3 2 10 3422.14 390.725 2 -3 -2 9 218.572 266.139 2 -3 -2 8 15514.3 390.635 2 -3 -2 7 6894.65 271.851 2 -3 -2 6 6867.62 847.641 2 -3 -2 4 139622. 869.490 2 -3 -2 3 172.213 197.052 2 -3 -2 2 7498.12 220.301 2 -3 2 1 9786.66 190.115 2 3 2 0 47.9738 264.100 2 -3 -2 -1 79802.3 343.057 2 -3 2 -2 40519.8 252.650 2 3 -2 3 13.0372 81.7519 2 3 -2 4 20274.6 194.522 2 -3 -2 -5 2451.85 476.241 2 -3 2 -7 2151.64 165.445 2 -3 2 -8 8250.59 239.373 2 -3 2 -9 573.873 212.266 2 3 2 10 3265.62 500.464 2 3 2 13 1886.79 443.691 2 3 2 14 2932.44 498.367 2 -3 3 15 12.0976 354.108 2 -3 3 14 8004.09 397.662 2 -3 3 13 354.834 351.839 2 -3 3 10 20566.0 767.752 2 -3 -3 9 21763.8 389.924 2 -3 -3 8 1486.12 256.903 2 -3 -3 7 689.298 231.099 2 -3 -3 6 2318.43 329.495 2 -3 -3 4 156390. 850.082 2 -3 -3 3 21274.2 311.960 2 -3 -3 2 10838.5 319.871 2 -3 -3 1 230.256 116.022 2 -3 3 -1 65.9699 117.129 2 -3 3 -2 14228.2 166.183 2 3 -3 3 8406.82 132.775 2 3 -3 4 42.9600 123.425 2 3 -3 7 2423.36 183.202 2 3 -3 8 434.577 151.687 2 3 -3 9 2853.82 185.100 2 3 -3 10 1102.94 214.450 2 -3 -3 -11 91.5468 389.938 2 3 3 13 4893.41 477.014 2 -3 4 15 1980.74 369.833 2 -3 4 14 281.750 382.168 2 -3 4 13 2429.01 337.623 2 -3 4 10 12697.1 741.601 2 -3 -4 9 10868.0 334.965 2 -3 -4 8 5977.24 291.822 2 -3 -4 7 10899.4 338.004 2 3 4 -4 11863.9 238.623 2 3 4 -3 50088.2 542.902 2 3 4 -2 4390.32 148.264 2 3 4 -1 6564.03 278.470 2 3 4 1 4696.93 154.178 2 3 4 2 4201.58 126.117 2 -3 4 -3 17020.0 125.888 2 3 -4 4 879.969 75.4481 2 3 -4 5 4242.34 299.001 2 3 -4 7 290.104 150.030 2 3 -4 8 625.847 165.748 2 3 -4 9 19010.8 267.667 2 3 -4 10 519.347 232.575 2 -3 -4 -11-26.6489 384.669 2 3 -4 13 215.970 440.234 2 -3 5 14 58.2648 379.183 2 -3 5 13 24.6224 335.113 2 -3 -5 10 1932.40 401.514 2 -3 -5 9 372.089 270.659 2 -3 -5 8 490.332 294.342 2 -3 -5 7 3557.99 289.118 2 -3 5 5 192.893 221.507 2 3 5 -4 17447.1 261.491 2 3 5 -3 20105.9 248.344 2 3 5 -2 3542.68 131.324 2 3 5 -1 72.6517 156.889 2 -3 -5 -1 754.923 69.3444 2 -3 5 -2 2997.19 91.2742 2 -3 5 -3 10679.9 118.131 2 3 5 4 4893.91 98.0750 2 3 5 5 88.7494 395.798 2 3 -5 7 3082.00 176.393 2 3 -5 8 30264.8 309.643 2 3 -5 9 6953.82 223.830 2 3 5 10-233.402 511.386 2 -3 -5 -11 81.7794 408.379 2 3 -5 13 3957.10 464.020 2 -3 -6 14 2634.70 397.830 2 -3 6 13 535.751 369.022 2 -3 6 10 5471.47 683.041 2 3 6 -9 288.364 311.608 2 -3 -6 8 4677.94 267.301 2 3 6 -7 2942.10 243.476 2 3 6 -6 9342.31 367.779 2 3 6 -4 1055.56 160.973 2 -3 -6 3 827.615 144.168 2 -3 -6 2 5.09973 116.127 2 3 6 -1 395.440 199.163 2 3 6 1 20705.6 179.556 2 -3 6 -2 57782.3 243.854 2 -3 6 -3 1191.26 92.1185 2 3 -6 4 15575.2 148.710 2 3 -6 7 3843.21 261.372 2 3 -6 8 10261.2 241.267 2 3 -6 9 7698.60 240.874 2 3 -6 10 7592.76 362.155 2 3 -6 13 963.986 314.307 2 -3 7 14 262.951 390.384 2 -3 -7 13 3326.02 404.627 2 -3 7 10 146.181 399.531 2 3 7 -9 14179.9 356.464 2 3 7 -8-25.6998 250.847 2 3 7 -7 2221.72 242.723 2 -3 -7 4 791.733 164.800 2 -3 -7 3 7932.24 187.549 2 -3 -7 2 527.706 125.604 2 3 7 -1 5098.22 245.762 2 3 7 1 12463.0 174.654 2 -3 7 -2 6265.82 129.897 2 -3 7 -3 11132.4 147.382 2 -3 -7 -4 7629.12 134.216 2 -3 7 -5-223.240 415.339 2 3 7 7 6722.87 133.668 2 3 -7 8 2110.50 183.572 2 3 -7 9 16074.0 244.091 2 3 -7 10 763.750 412.077 2 3 -7 13 744.553 323.165 2 -3 -8 13 655.894 396.986 2 -3 8 10 58.3797 508.866 2 3 8 -9 3783.39 303.185 2 3 8 -8 939.373 262.538 2 3 8 -7 768.531 246.763 2 3 -8 -5 59.2335 369.037 2 -3 -8 4 468.181 173.412 2 -3 -8 3 5226.31 157.864 2 -3 8 2 83.9786 121.276 2 3 8 -1 735.128 215.846 2 3 8 1 2279.05 139.398 2 -3 8 -2 1721.34 121.413 2 -3 8 -3 672.158 117.486 2 -3 8 -4 2032.51 121.971 2 3 8 5 7268.04 441.890 2 3 -8 7 1278.76 149.942 2 3 -8 8 736.467 190.148 2 3 -8 9 102.763 198.848 2 3 8 10 4536.09 296.900 2 -3 -9 13 3779.45 438.800 2 -3 -9 9 18118.3 404.154 2 -3 -9 8 20.0160 269.681 2 -3 -9 7-99.4488 260.023 2 -3 -9 4 27373.0 307.909 2 -3 -9 3 24335.4 237.791 2 -3 -9 2-68.7124 130.603 2 3 9 -1 7815.08 368.241 2 3 9 1 1038.44 151.908 2 -3 9 -2 16191.1 200.593 2 -3 9 -3 11784.9 183.407 2 3 9 4 257.143 129.266 2 3 -9 7 5717.12 189.301 2 3 -9 8 1174.27 152.572 2 3 -9 9 75.3844 212.690 2 3 -9 10 4963.55 369.648 2 -3 -10 9 2193.13 268.504 2 -3 -10 8 1912.25 231.154 2 -3 -10 7 12412.2 303.873 2 -3 -10 4 6701.59 211.824 2 -3 -10 3 95.1741 148.737 2 -3 -10 2 8069.75 184.402 2 3 10 -1 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576.702 296.063 2 3 15 2 3874.78 284.981 2 3 15 3 167.784 284.937 2 3 15 4 2079.96 291.329 2 3 -15 7 923.847 658.198 2 -3 -16 4 844.177 338.775 2 -3 -16 3 281.425 285.890 2 -3 -16 2 859.674 276.120 2 3 16 -1 3422.30 606.187 2 -3 -16 -1 975.013 331.292 2 3 16 2 1920.50 330.336 2 3 16 3 3970.53 357.925 2 3 -16 4 597.252 432.806 2 -3 -17 4 2512.94 576.439 2 -3 -17 3 61.3399 418.761 2 -3 -17 2 129.107 331.324 2 3 17 -1 4957.78 663.608 2 -3 -17 -1-176.801 421.839 2 3 -17 2 214.619 452.983 2 -4 0 14 597.147 519.212 2 -4 0 10 58449.7 1140.41 2 -4 0 8 8338.19 622.412 2 4 0 -6 363.448 690.621 2 -4 0 4-87.8788 493.251 2 -4 0 2 2989.77 207.299 2 4 0 2 6447.15 154.933 2 4 0 4 46288.4 375.829 2 4 0 8 68.3203 374.856 2 4 0 10 4468.57 496.791 2 -4 1 15 2558.64 400.726 2 -4 1 14-128.905 365.836 2 -4 1 13 56.8331 351.061 2 4 -1 -12 4751.73 683.074 2 -4 1 10 251.714 592.998 2 -4 1 9 46319.6 722.224 2 -4 -1 8 39719.5 665.013 2 -4 -1 7 1238.99 368.290 2 -4 -1 6-1951.00 351.541 2 -4 1 4 50066.2 647.977 2 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468.673 280.190 2 -7 7 -8 1025.91 336.520 2 -7 -8 9-23.9244 408.593 2 -7 -8 8 194.191 401.127 2 -7 -8 7 126.670 371.614 2 -7 -8 4 192.651 210.532 2 -7 -8 3 1513.37 183.153 2 -7 8 2 404.692 89.5153 2 -7 8 -2 505.180 221.829 2 -7 8 -3 801.741 213.269 2 -7 8 -4 1980.09 207.612 2 -7 8 -7 155.362 340.023 2 -7 8 -8 1464.89 352.800 2 -7 -9 9 109.014 448.741 2 -7 -9 8 2642.88 441.293 2 -7 -9 7 2443.87 395.551 2 7 9 -5 3228.82 502.167 2 -7 -9 4 195.091 212.722 2 -7 -9 3 4004.24 203.820 2 -7 9 2 30621.1 233.678 2 -7 9 -2 176.478 214.702 2 -7 9 -3 4435.98 255.346 2 -7 -9 -4 44.3620 204.668 2 -7 9 -7 345.703 376.397 2 -7 -10 9 1818.05 466.472 2 -7 -10 8 110.260 396.033 2 -7 -10 7 846.790 366.111 2 -7 -10 5 87.8270 654.310 2 -7 -10 4 1519.34 250.853 2 -7 -10 3 5208.88 238.073 2 -7 10 2 2201.44 152.589 2 -7 10 -2 3480.96 247.426 2 -7 10 -3 761.725 230.736 2 -7 -10 -4 532.906 266.948 2 -7 -11 7 4860.42 422.273 2 -7 -11 4-13.7683 253.304 2 -7 -11 3 3460.17 230.243 2 -7 -11 2 1846.30 175.780 2 -7 11 1-29.7063 599.287 2 7 -11 2 4757.68 336.093 2 7 -11 3-116.197 278.991 2 7 -11 4 5998.12 350.496 2 7 11 5 3929.53 732.997 2 -7 -12 4 454.972 266.591 2 -7 -12 3 8464.25 305.013 2 -7 -12 2 90.7470 175.888 2 -7 -12 -2 2672.69 335.804 2 -7 -12 -3-175.650 338.653 2 -7 -12 -4 193.296 358.647 2 -7 -13 4 2254.99 277.939 2 -7 -13 3 2362.76 643.954 2 -7 -13 2 12.7895 595.062 2 -7 13 0 185.173 702.242 2 -7 -13 -2 427.384 367.520 2 -8 0 8 936.113 409.644 2 -8 0 4 495.115 276.457 2 -8 0 2 442.178 231.324 2 -8 0 -2 15.8216 232.024 2 -8 0 -4 5830.40 513.656 2 -8 1 9 221.132 373.075 2 -8 1 8 587.005 361.985 2 -8 -1 7 14283.0 371.100 2 -8 -1 4 249.992 206.161 2 -8 -1 3 29.9450 179.493 2 -8 -1 2 7181.21 207.349 2 -8 1 -2 434.424 239.554 2 -8 -1 -3 11.3976 231.406 2 -8 -1 -4 200.537 154.892 2 -8 1 -5 6873.91 777.030 2 -8 1 -7 5607.35 139.421 2 8 -1 8 1554.94 337.497 2 -8 2 10 1908.29 849.553 2 -8 2 9-182.132 335.537 2 -8 -2 8 6753.93 373.202 2 -8 -2 7 634.150 362.754 2 -8 -2 4 7059.97 253.207 2 -8 -2 3 157.554 179.057 2 -8 -2 2 1301.82 161.753 2 -8 -2 -2 1830.31 259.041 2 -8 -2 -3 52.0572 177.847 2 -8 -2 -4 117.457 155.107 2 -8 -2 -5 11703.1 885.838 2 -8 2 -7 8457.91 210.310 2 8 -2 8 3438.56 396.796 2 -8 -3 9 6.47003 423.602 2 -8 -3 8 7.90393 311.876 2 -8 -3 7 2739.79 325.853 2 -8 -3 6 21742.8 935.382 2 -8 -3 4 3225.47 177.376 2 -8 -3 3-46.0541 168.489 2 -8 -3 2 709.002 147.518 2 8 -3 0-346.636 527.622 2 -8 3 -2 1093.07 209.884 2 -8 3 -3 1343.99 191.332 2 -8 3 -4 618.461 180.791 2 -8 3 -7 10582.4 267.952 2 8 -3 8-127.623 384.491 2 -8 -4 9 60.4308 416.334 2 -8 -4 8 183.200 327.452 2 -8 -4 7 3611.38 340.413 2 -8 -4 6 12758.5 800.946 2 -8 4 5 409.500 435.643 2 -8 -4 4 36.7091 148.111 2 -8 -4 3 69.4523 164.821 2 -8 4 2 2968.41 327.971 2 -8 4 -2 1138.14 226.228 2 -8 4 -3 1112.95 200.685 2 8 -4 4 1288.91 192.209 2 8 -4 7 556.504 332.799 2 8 -4 8 1829.69 438.005 2 -8 -5 9 1129.58 437.224 2 -8 -5 8 51.0729 400.635 2 -8 -5 7 3153.22 326.263 2 -8 5 5 126.763 673.829 2 -8 -5 4 331.769 145.294 2 -8 5 3 309.838 160.027 2 -8 5 2 1877.04 323.564 2 -8 5 -2 2804.81 221.730 2 -8 5 -3 2518.57 217.643 2 -8 5 -4 2697.05 208.373 2 8 -5 7 745.972 365.195 2 8 -5 8 318.133 449.324 2 -8 -6 9 2037.45 433.248 2 -8 -6 8 7217.38 465.601 2 -8 -6 7 589.264 284.906 2 -8 6 4 803.708 156.745 2 -8 -6 3 6764.12 150.277 2 -8 6 2 14174.8 463.011 2 -8 6 -2 140.369 208.977 2 -8 6 -3 1281.29 212.685 2 -8 -6 -4 1163.48 201.697 2 8 -6 7 3150.48 401.535 2 -8 -7 9 491.640 424.599 2 -8 -7 8 248.523 397.919 2 -8 -7 7-82.7833 388.705 2 -8 -7 4 58.1456 210.708 2 -8 -7 3 853.311 98.5152 2 -8 7 2 1687.52 365.799 2 -8 7 -2 1337.81 226.455 2 -8 7 -3 757.193 214.868 2 -8 -7 -4 385.235 202.553 2 -8 7 -5-864.619 410.889 2 8 -7 7 1060.15 474.247 2 -8 -8 9 310.065 418.826 2 -8 -8 8 45.6974 426.507 2 -8 -8 7 142.450 378.155 2 8 8 -6-12.8404 513.996 2 -8 -8 4 175.020 195.203 2 -8 8 3 47.5102 58.1273 2 -8 8 2 5177.34 419.149 2 -8 -8 -2 1469.05 239.531 2 -8 -8 -3 3908.27 286.809 2 -8 8 -4 1112.25 221.166 2 -8 -8 -5 643.294 599.349 2 -8 -9 7 572.220 375.145 2 -8 -9 4 360.084 212.145 2 -8 -9 3 158.276 500.013 2 8 9 -2 2805.48 487.723 2 -8 9 -2 3201.55 288.785 2 -8 -9 -3 1704.63 308.211 2 8 -9 4 2878.23 296.612 2 -8 10 5-322.642 840.656 2 -8 -10 4 52.3318 206.673 2 -8 -10 3 406.465 618.290 2 8 10 -2 12764.0 601.115 2 -8 -10 -2-105.365 321.762 2 8 -10 3 14069.2 437.732 2 -8 -11 4 44.3475 674.065 2 -8 -11 3 6089.26 710.880 2 -8 -11 2 1956.29 615.398 2 8 -11 2 1323.06 361.014 2 -8 -11 -3 1541.11 418.147 2 -8 -12 3 6376.71 747.441 2 -9 0 8 2534.74 458.927 2 -9 0 4 8286.63 374.882 2 -9 0 2 2233.25 277.801 2 -9 0 -2-1.01181 547.716 2 -9 0 -4 287.105 251.095 2 -9 1 9-100.020 311.113 2 -9 1 8 556.688 303.751 2 -9 -1 7 49.2906 290.525 2 -9 -1 4 4653.40 240.162 2 -9 -1 3 1276.91 195.024 2 -9 -1 2 742.786 180.109 2 -9 -1 -2 403.007 248.867 2 -9 -1 -3 441.974 244.839 2 -9 1 -4 61.1353 190.067 2 9 -1 5 4.64962 881.731 2 -9 2 9 452.153 346.866 2 -9 2 8 39.0565 255.653 2 -9 -2 7 3038.78 262.354 2 -9 -2 4 12322.3 238.914 2 -9 -2 3 8.33019 141.375 2 -9 -2 2 199.624 202.916 2 -9 2 1 1610.35 211.867 2 -9 -2 -2 5196.41 303.102 2 -9 -2 -3-177.042 441.507 2 -9 -2 -4 605.634 201.935 2 -9 -3 9 1376.28 477.910 2 -9 -3 8 924.979 297.743 2 -9 -3 7 1295.98 240.704 2 -9 -3 4 3650.14 178.613 2 -9 -3 3 648.778 173.288 2 -9 -3 2 62.6528 105.448 2 -9 3 -1 256.166 372.919 2 -9 -3 -2 709.300 276.382 2 -9 -3 -3 1803.10 230.423 2 -9 -3 -4 568.502 176.269 2 -9 -4 9 4875.00 488.550 2 -9 -4 8 770.864 426.723 2 -9 -4 7 1556.76 238.729 2 -9 -4 4 4190.01 225.390 2 -9 -4 3 136.807 156.505 2 -9 4 2 32.5920 300.174 2 -9 4 -2-61.6890 308.225 2 -9 4 -3 2560.69 223.436 2 -9 -4 -4 102.345 198.172 2 -9 4 -5 2589.33 539.470 2 -9 -5 9-175.408 439.950 2 -9 -5 8 395.048 415.135 2 -9 -5 7 4365.46 656.271 2 -9 5 4 17.4777 139.733 2 -9 -5 3 2544.81 137.567 2 -9 5 2 1117.19 358.719 2 -9 5 -2 44.7837 259.848 2 9 -5 3 1183.57 219.968 2 9 -5 4 495.239 202.539 2 -9 -5 -5 2171.67 875.085 2 -9 6 8 2138.69 1052.29 2 -9 -6 7 438.201 372.852 2 -9 6 4 3283.64 199.089 2 -9 6 3 39.1059 356.816 2 -9 6 2 81.9361 351.408 2 -9 6 -2 323.298 231.425 2 -9 6 -3 60.2701 222.762 2 9 -6 4 2215.92 306.843 2 9 6 5 481.488 708.157 2 -9 -7 8 1598.18 409.728 2 -9 -7 7 34.1964 355.401 2 -9 -7 4 1262.69 189.757 2 -9 7 3 507.233 400.952 2 -9 7 2 17.4047 380.811 2 -9 7 1-355.991 664.971 2 -9 7 -2 2438.86 284.205 2 -9 -7 -3 146.642 304.734 2 -9 7 -4 95.4651 597.545 2 -9 8 7 16.6638 1030.96 2 -9 -8 4 4736.67 751.047 2 -9 -8 3 1241.42 663.625 2 -9 -8 2 240.888 633.923 2 -9 -8 -2 7850.39 399.812 2 -9 -8 -3 5814.14 425.873 2 -9 -9 4 666.891 703.318 2 -9 -9 3 299.794 672.100 2 -9 -9 2-95.8633 587.668 2 -9 -9 -2 1900.25 358.896 2 -9 -10 3 1020.43 719.927 2 -10 0 8 783.202 928.476 2 -10 0 4 649.333 307.277 2 -10 0 2 100.829 267.588 2 -10 0 -2 4684.05 662.097 2 -10 0 -4 254.009 495.044 2 -10 1 7 212.366 262.388 2 10 -1 -5 5151.39 597.492 2 -10 -1 4 9922.99 301.397 2 -10 -1 3 1259.39 205.271 2 -10 -1 2 333.946 172.698 2 -10 1 1 320.310 295.184 2 -10 -1 -2 3270.51 442.643 2 -10 -1 -3 998.166 507.710 2 -10 1 -4-71.9856 548.820 2 -10 2 7-49.4382 531.889 2 -10 -2 4 2874.43 352.460 2 -10 -2 3 4836.89 362.226 2 -10 2 2 54.2105 191.667 2 -10 -2 -2 91.8478 409.550 2 -10 -2 -3-11.4869 468.356 2 -10 3 7 482.800 953.238 2 -10 -3 4 18.9773 343.949 2 -10 3 3-10.0362 328.049 2 -10 3 2 319.648 317.835 2 -10 -3 1-64.7002 693.676 2 -10 -3 -2 1780.10 441.383 2 -10 3 -3 514.029 336.601 2 -10 -4 4 16293.4 567.749 2 -10 4 3 2346.45 353.769 2 -10 4 2 58.1045 336.925 2 -10 -4 -2-31.0448 315.538 2 -10 5 4 738.604 368.287 2 -10 5 3 51.0598 353.942 2 -10 5 2 953.779 359.661 2 -10 -5 -2 770.517 429.606 2 -10 -6 4 250.517 579.936 2 -10 6 3 789.173 361.078 2 -10 6 2 952.633 518.298 2 ; _shelx_hkl_checksum 78996 _olex2_date_sample_data_collection 2018-01-25 _olex2_date_sample_submission 2018-01-03 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in perfluoroether oil' _olex2_submission_original_sample_id TS4 _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 2.305 _oxdiff_exptl_absorpt_empirical_full_min 0.647 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.586(2) 7865 5030 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.414(2) 7692 5030 nmt -0.9999 -0.0003 -0.1801 0.0000 -1.0003 0.0003 0.0009 0.0002 1.0004 _twin_special_details ; Component 2 rotated by 180.0000\% around [-0.09 -0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct) ; _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{d174dad5-dc24-4a04-b3fc-e7d672ccb279}" "_publcif_info_datablock.publ_exptl" "{d174dad5-dc24-4a04-b3fc-e7d672ccb279}" "_geom_hbond_atom_site_label_D" loop_ _publcif_info_cif.paper_type EE loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{d174dad5-dc24-4a04-b3fc-e7d672ccb279}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? ;