data_r040 _audit_creation_date 2018-04-27 _audit_creation_method ; Olex2 1.2-alpha (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _shelx_SHELXL_version_number '2016/6' _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 'C24 H23 N O4' _chemical_formula_sum 'C24 H23 N O4' _chemical_formula_weight 389.43 _chemical_absolute_configuration unk _chemical_melting_point ? _chemical_oxdiff_formula 'C24 H23 N O4' _chemical_oxdiff_usercomment Leitner_Reiser_ML-202F1 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.74420(10) _cell_length_b 7.90290(10) _cell_length_c 36.0260(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1920.14(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15949 _cell_measurement_temperature 122.9(2) _cell_measurement_theta_max 74.5670 _cell_measurement_theta_min 4.9000 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 824 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 3 -17 0.1242 -1 -3 17 0.1026 -4 2 -11 0.1289 -4 -2 6 0.1535 0 -1 -23 0.0969 0 1 23 0.1023 -4 0 2 0.1343 4 0 0 0.1327 1 -4 -14 0.1656 -2 -4 -12 0.1788 1 4 14 0.1533 -1 4 14 0.1519 1 -5 3 0.1511 -3 -4 1 0.1671 -2 5 -3 0.1275 1 5 -2 0.1464 4 2 1 0.1426 -4 1 -12 0.1269 -2 2 -17 0.1226 0 -1 23 0.0998 -2 1 -21 0.1119 3 1 -17 0.1553 -1 1 -23 0.1088 0 -5 -5 0.1498 _exptl_crystal_size_max 0.304 _exptl_crystal_size_mid 0.273 _exptl_crystal_size_min 0.199 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 0.0003 2.9998 -17.0028 0.1623 0.9185 0.0158 -1.0001 -2.9998 17.0030 -0.1405 -0.9262 0.2114 -3.9990 2.0003 -11.0008 0.2021 0.5690 0.9183 -3.9999 -1.9996 6.0020 -0.1304 -0.4436 0.9157 -0.0027 -1.0004 -23.0038 -0.6413 0.7662 0.0880 0.0027 1.0004 23.0038 0.6413 -0.7662 -0.0880 -3.9990 0.0004 2.0013 0.1280 -0.1057 0.9023 3.9992 -0.0004 -0.0010 -0.0871 0.0308 -0.9088 0.9960 -4.0004 -14.0026 -0.9892 0.1547 -0.1290 -2.0032 -4.0001 -12.0015 -0.8829 0.0567 0.5462 1.0036 4.0002 14.0021 0.9457 -0.1393 -0.3255 -0.9960 4.0004 14.0026 0.9892 -0.1547 0.1290 0.9970 -5.0002 3.0002 -0.8112 -0.5754 -0.1711 -3.0018 -3.9998 1.0009 -0.5949 -0.4373 0.7311 -1.9968 5.0003 -3.0000 0.8329 0.5677 0.3983 1.0027 5.0000 -2.0005 0.7881 0.5534 -0.2866 4.0005 1.9997 0.9992 0.2737 0.1818 -0.9384 -3.9997 1.0002 -12.0009 0.0115 0.5122 0.9347 -1.9999 2.0000 -17.0023 0.0357 0.8088 0.4834 0.0015 -0.9997 23.0038 0.3009 -0.9545 -0.0617 -2.0009 0.9999 -21.0029 -0.2164 0.8643 0.5096 2.9984 0.9995 -17.0035 -0.2433 0.7532 -0.6395 -1.0013 0.9998 -23.0035 -0.2791 0.9468 0.2889 -0.0036 -5.0002 -5.0008 -0.9533 -0.2839 0.0821 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_unetI/netI 0.0167 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 22748 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.780 _diffrn_reflns_theta_min 4.910 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 122.9(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 4.2047 _diffrn_detector_type TitanS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _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 -125.00 -79.00 1.00 1.00 -- -43.98 -99.00 90.00 46 2 \w -97.00 -2.00 1.00 1.00 -- -43.98 125.00-180.00 95 3 \w 18.00 114.00 1.00 1.00 -- 43.98 57.00 120.00 96 4 \w -26.00 70.00 1.00 1.00 -- 43.98 -57.00 -30.00 96 5 \w 94.00 178.00 1.00 2.00 -- 107.00 125.00-180.00 84 6 \w 83.00 178.00 1.00 2.00 -- 107.00 45.00 30.00 95 7 \w 80.00 177.00 1.00 2.00 -- 107.00 61.00 60.00 97 8 \w 94.00 178.00 1.00 2.00 -- 107.00 125.00 -90.00 84 9 \w 83.00 178.00 1.00 2.00 -- 107.00 45.00-120.00 95 10 \w 24.00 109.00 1.00 2.00 -- 107.00 -94.00 -60.00 85 11 \w 33.00 121.00 1.00 2.00 -- 107.00-125.00 -60.00 88 12 \w 33.00 121.00 1.00 2.00 -- 107.00-125.00-120.00 88 13 \w 36.00 131.00 1.00 2.00 -- 107.00 -45.00 -90.00 95 14 \w 34.00 132.00 1.00 2.00 -- 107.00-145.00-177.00 98 15 \w -114.00 -18.00 1.00 1.00 -- -43.98 -57.00-150.00 96 16 \w -114.00 -18.00 1.00 1.00 -- -43.98 -57.00 -60.00 96 17 \w 20.00 116.00 1.00 1.00 -- 43.98 37.00 30.00 96 18 \w 80.00 127.00 1.00 2.00 -- 107.00 61.00-180.00 47 19 \w 80.00 178.00 1.00 2.00 -- 107.00 30.00 -30.00 98 20 \w 80.00 178.00 1.00 2.00 -- 107.00 30.00 150.00 98 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'GV1000, TitanS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0217524000 _diffrn_orient_matrix_UB_12 0.1701756000 _diffrn_orient_matrix_UB_13 0.0204781000 _diffrn_orient_matrix_UB_21 0.0077126000 _diffrn_orient_matrix_UB_22 0.0941713000 _diffrn_orient_matrix_UB_23 -0.0374027000 _diffrn_orient_matrix_UB_31 -0.2272559000 _diffrn_orient_matrix_UB_32 -0.0130347000 _diffrn_orient_matrix_UB_33 -0.0032318000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'gradient vaccum rotating-anode X-ray tube' _diffrn_source_type 'GV1000 (Cu) X-ray Source' _reflns_Friedel_coverage 0.697 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.984 _reflns_number_gt 3824 _reflns_number_total 3901 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.37b (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 0.155 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Flack x determined using 1544 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.06(5) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 3901 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0285 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.3129P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.0771 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C15(H15) 2.b Secondary CH2 refined with riding coordinates: C22(H22A,H22B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B) 2.c Aromatic/amide H refined with riding coordinates: C10(H10), C7(H7), C16(H16), C17(H17), C14(H14), C11(H11), C13(H13), C12(H12) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C23(H23A,H23B,H23C) ; _atom_sites_solution_hydrogens geom _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 O2 O 0.87604(18) 0.42967(16) 0.28233(3) 0.0250(3) Uani 1 1 d . . . . . O4 O 0.43849(18) -0.01819(15) 0.32039(3) 0.0251(3) Uani 1 1 d . . . . . O1 O 1.04775(17) 0.25954(16) 0.32037(3) 0.0263(3) Uani 1 1 d . . . . . O3 O 0.6254(2) 0.11881(17) 0.27867(3) 0.0309(3) Uani 1 1 d . . . . . N1 N 0.90371(18) 0.57643(16) 0.37530(3) 0.0174(3) Uani 1 1 d . . . . . C6 C 0.5688(2) 0.21858(19) 0.40436(4) 0.0163(3) Uani 1 1 d . . . . . C10 C 0.8906(2) 0.29124(19) 0.42933(4) 0.0164(3) Uani 1 1 d . . . . . H10 H 1.007568 0.353397 0.428157 0.020 Uiso 1 1 calc R . . . . C3 C 0.7266(2) 0.3486(2) 0.33876(4) 0.0161(3) Uani 1 1 d . . . . . C5 C 0.7411(2) 0.32337(19) 0.40483(4) 0.0154(3) Uani 1 1 d . . . . . C9 C 0.8680(2) 0.16236(19) 0.45678(4) 0.0177(3) Uani 1 1 d . . . . . C7 C 0.5422(2) 0.0950(2) 0.43025(4) 0.0186(3) Uani 1 1 d . . . . . H7 H 0.427978 0.029121 0.429858 0.022 Uiso 1 1 calc R . . . . C18 C 0.9009(2) 0.33842(19) 0.31311(4) 0.0181(3) Uani 1 1 d . . . . . C8 C 0.6896(2) 0.0667(2) 0.45797(4) 0.0184(3) Uani 1 1 d . . . . . C2 C 0.5695(2) 0.2444(2) 0.33776(4) 0.0173(3) Uani 1 1 d . . . . . C1 C 0.5482(2) 0.1123(2) 0.30887(4) 0.0188(3) Uani 1 1 d . . . . . C16 C 0.3769(2) 0.4426(2) 0.37542(4) 0.0199(3) Uani 1 1 d . . . . . H16 H 0.246353 0.480077 0.376597 0.024 Uiso 1 1 calc R . . . . C4 C 0.7364(2) 0.45988(19) 0.37422(4) 0.0156(3) Uani 1 1 d . . . . . C15 C 0.4333(2) 0.2568(2) 0.37153(4) 0.0180(3) Uani 1 1 d . . . . . H15 H 0.318343 0.181289 0.370097 0.022 Uiso 1 1 calc R . . . . C17 C 0.5312(2) 0.5452(2) 0.37695(4) 0.0192(3) Uani 1 1 d . . . . . H17 H 0.517060 0.661693 0.379524 0.023 Uiso 1 1 calc R . . . . C14 C 0.6653(3) -0.0549(2) 0.48664(5) 0.0237(3) Uani 1 1 d . . . . . H14 H 0.548557 -0.117144 0.488031 0.028 Uiso 1 1 calc R . . . . C11 C 1.0182(3) 0.1289(2) 0.48320(4) 0.0217(3) Uani 1 1 d . . . . . H11 H 1.136973 0.188438 0.482095 0.026 Uiso 1 1 calc R . . . . C22 C 0.9098(3) 0.6977(2) 0.34349(5) 0.0242(4) Uani 1 1 d . . . . . H22A H 0.784507 0.697362 0.330271 0.029 Uiso 1 1 calc R . . . . H22B H 1.014570 0.667259 0.326294 0.029 Uiso 1 1 calc R . . . . C13 C 0.8119(3) -0.0813(2) 0.51223(5) 0.0270(4) Uani 1 1 d . . . . . H13 H 0.793042 -0.160237 0.531041 0.032 Uiso 1 1 calc R . . . . C12 C 0.9909(3) 0.0097(2) 0.51041(5) 0.0260(4) Uani 1 1 d . . . . . H12 H 1.090714 -0.010865 0.527649 0.031 Uiso 1 1 calc R . . . . C19 C 0.9193(3) 0.6787(2) 0.40964(5) 0.0237(3) Uani 1 1 d . . . . . H19A H 0.985531 0.615967 0.429190 0.028 Uiso 1 1 calc R . . . . H19B H 0.789449 0.713551 0.418330 0.028 Uiso 1 1 calc R . . . . C20 C 1.0416(3) 0.8298(2) 0.39759(5) 0.0291(4) Uani 1 1 d . . . . . H20A H 1.180661 0.800550 0.395050 0.035 Uiso 1 1 calc R . . . . H20B H 1.028483 0.923160 0.414892 0.035 Uiso 1 1 calc R . . . . C24 C 0.4186(3) -0.1539(2) 0.29344(5) 0.0303(4) Uani 1 1 d . . . . . H24A H 0.357086 -0.110967 0.271337 0.046 Uiso 1 1 calc GR . . . . H24B H 0.338243 -0.242543 0.303710 0.046 Uiso 1 1 calc GR . . . . H24C H 0.547448 -0.197842 0.287475 0.046 Uiso 1 1 calc GR . . . . C23 C 1.0444(3) 0.4282(3) 0.25732(5) 0.0361(4) Uani 1 1 d . . . . . H23A H 1.015804 0.497341 0.236077 0.054 Uiso 1 1 calc GR . . . . H23B H 1.070076 0.314275 0.249404 0.054 Uiso 1 1 calc GR . . . . H23C H 1.158913 0.471952 0.269912 0.054 Uiso 1 1 calc GR . . . . C21 C 0.9494(3) 0.8717(2) 0.36034(5) 0.0347(4) Uani 1 1 d . . . . . H21A H 1.039927 0.936637 0.345027 0.042 Uiso 1 1 calc R . . . . H21B H 0.827179 0.934886 0.363400 0.042 Uiso 1 1 calc R . . . . 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 O2 0.0255(6) 0.0310(6) 0.0185(5) 0.0045(5) 0.0041(5) -0.0022(5) O4 0.0246(6) 0.0275(6) 0.0232(5) -0.0052(5) 0.0012(5) -0.0086(5) O1 0.0161(5) 0.0332(6) 0.0295(6) 0.0002(5) 0.0027(5) 0.0037(5) O3 0.0373(7) 0.0331(7) 0.0222(6) -0.0058(5) 0.0081(5) -0.0077(6) N1 0.0134(6) 0.0178(6) 0.0210(6) 0.0001(5) -0.0008(5) -0.0017(5) C6 0.0122(6) 0.0202(7) 0.0165(7) -0.0035(5) 0.0004(5) 0.0010(6) C10 0.0141(7) 0.0178(7) 0.0173(7) -0.0037(5) 0.0008(6) -0.0006(6) C3 0.0132(7) 0.0200(7) 0.0153(6) 0.0005(6) -0.0014(5) 0.0026(6) C5 0.0138(7) 0.0172(7) 0.0154(7) -0.0031(6) 0.0029(5) -0.0004(6) C9 0.0189(7) 0.0182(7) 0.0159(6) -0.0041(6) 0.0009(6) 0.0026(6) C7 0.0160(7) 0.0201(7) 0.0197(7) -0.0028(5) 0.0040(6) -0.0030(6) C18 0.0166(7) 0.0210(7) 0.0168(7) -0.0024(6) 0.0000(6) -0.0040(6) C8 0.0206(7) 0.0178(7) 0.0167(6) -0.0027(6) 0.0036(6) 0.0010(6) C2 0.0129(7) 0.0232(7) 0.0159(7) 0.0007(6) -0.0015(6) 0.0014(6) C1 0.0128(6) 0.0241(7) 0.0194(7) -0.0002(6) -0.0031(6) 0.0009(6) C16 0.0115(6) 0.0278(8) 0.0204(7) -0.0001(6) 0.0011(6) 0.0040(6) C4 0.0112(6) 0.0186(7) 0.0170(7) -0.0012(6) 0.0007(5) 0.0010(6) C15 0.0124(7) 0.0242(7) 0.0175(7) -0.0011(6) 0.0001(6) -0.0019(6) C17 0.0146(7) 0.0215(7) 0.0215(7) -0.0006(6) 0.0001(6) 0.0041(6) C14 0.0272(9) 0.0204(7) 0.0234(7) 0.0002(6) 0.0059(6) -0.0002(7) C11 0.0225(8) 0.0228(7) 0.0198(7) -0.0036(6) -0.0025(6) 0.0025(6) C22 0.0229(8) 0.0224(8) 0.0273(8) 0.0052(6) 0.0024(7) -0.0037(7) C13 0.0373(9) 0.0229(8) 0.0208(7) 0.0034(6) 0.0037(7) 0.0060(8) C12 0.0320(9) 0.0254(8) 0.0206(7) -0.0006(6) -0.0056(7) 0.0064(7) C19 0.0239(8) 0.0218(7) 0.0255(8) -0.0043(6) -0.0027(7) -0.0027(7) C20 0.0226(8) 0.0209(8) 0.0438(10) -0.0102(7) 0.0053(8) -0.0028(7) C24 0.0297(9) 0.0309(9) 0.0305(9) -0.0095(7) -0.0031(7) -0.0087(8) C23 0.0381(11) 0.0453(11) 0.0249(8) 0.0030(8) 0.0134(8) -0.0091(9) C21 0.0422(11) 0.0200(8) 0.0421(10) 0.0018(7) 0.0099(9) -0.0023(8) _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 O2 C18 1.3333(19) . ? O2 C23 1.450(2) . ? O4 C1 1.336(2) . ? O4 C24 1.4528(19) . ? O1 C18 1.199(2) . ? O3 C1 1.207(2) . ? N1 C4 1.4572(19) . ? N1 C22 1.4948(19) . ? N1 C19 1.4815(19) . ? C6 C5 1.427(2) . ? C6 C7 1.362(2) . ? C6 C15 1.525(2) . ? C10 C5 1.364(2) . ? C10 C9 1.428(2) . ? C3 C18 1.497(2) . ? C3 C2 1.343(2) . ? C3 C4 1.552(2) . ? C5 C4 1.543(2) . ? C9 C8 1.421(2) . ? C9 C11 1.415(2) . ? C7 C8 1.427(2) . ? C8 C14 1.420(2) . ? C2 C1 1.481(2) . ? C2 C15 1.528(2) . ? C16 C15 1.523(2) . ? C16 C17 1.321(2) . ? C4 C17 1.542(2) . ? C14 C13 1.368(3) . ? C11 C12 1.372(2) . ? C22 C21 1.526(2) . ? C13 C12 1.407(3) . ? C19 C20 1.515(2) . ? C20 C21 1.516(3) . ? 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 C18 O2 C23 114.46(14) . . ? C1 O4 C24 114.42(13) . . ? C4 N1 C22 113.97(12) . . ? C4 N1 C19 114.97(12) . . ? C19 N1 C22 106.77(12) . . ? C5 C6 C15 112.47(13) . . ? C7 C6 C5 121.01(14) . . ? C7 C6 C15 126.45(14) . . ? C5 C10 C9 120.13(14) . . ? C18 C3 C4 120.35(13) . . ? C2 C3 C18 124.75(14) . . ? C2 C3 C4 113.77(13) . . ? C6 C5 C4 112.35(12) . . ? C10 C5 C6 120.11(14) . . ? C10 C5 C4 127.45(13) . . ? C8 C9 C10 119.40(14) . . ? C11 C9 C10 121.51(15) . . ? C11 C9 C8 119.09(14) . . ? C6 C7 C8 119.98(14) . . ? O2 C18 C3 112.68(13) . . ? O1 C18 O2 124.50(14) . . ? O1 C18 C3 122.79(14) . . ? C9 C8 C7 119.03(14) . . ? C14 C8 C9 118.65(15) . . ? C14 C8 C7 122.32(15) . . ? C3 C2 C1 121.84(14) . . ? C3 C2 C15 114.43(13) . . ? C1 C2 C15 123.16(13) . . ? O4 C1 C2 112.30(13) . . ? O3 C1 O4 123.49(15) . . ? O3 C1 C2 124.18(15) . . ? C17 C16 C15 113.52(14) . . ? N1 C4 C3 114.39(12) . . ? N1 C4 C5 113.99(12) . . ? N1 C4 C17 114.62(12) . . ? C5 C4 C3 101.13(11) . . ? C17 C4 C3 105.21(12) . . ? C17 C4 C5 106.19(12) . . ? C6 C15 C2 104.16(12) . . ? C16 C15 C6 105.64(12) . . ? C16 C15 C2 106.59(12) . . ? C16 C17 C4 115.82(13) . . ? C13 C14 C8 120.66(16) . . ? C12 C11 C9 120.88(16) . . ? N1 C22 C21 106.11(13) . . ? C14 C13 C12 120.73(15) . . ? C11 C12 C13 119.94(16) . . ? N1 C19 C20 103.25(13) . . ? C19 C20 C21 101.68(15) . . ? C20 C21 C22 103.14(14) . . ? _shelx_res_file ; TITL r040_a.res in P2(1)2(1)2(1) r040.res created by SHELXL-2016/6 at 10:01:00 on 27-Apr-2018 REM Old TITL r040_a.res in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.088, Rweak 0.022, Alpha 0.001, Orientation as input REM Flack x = -0.002 ( 0.050 ) from Parsons' quotients REM Formula found by SHELXT: C24 N O4 CELL 1.54184 6.7442 7.9029 36.026 90 90 90 ZERR 4 0.0001 0.0001 0.0003 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 96 92 4 16 L.S. 4 PLAN 5 list 4 fmap 2 acta REM REM REM WGHT 0.047200 0.312900 FVAR 0.68722 O2 4 0.876039 0.429669 0.282333 11.00000 0.02547 0.03098 = 0.01847 0.00453 0.00410 -0.00219 O4 4 0.438491 -0.018187 0.320389 11.00000 0.02465 0.02750 = 0.02317 -0.00517 0.00122 -0.00858 O1 4 1.047754 0.259535 0.320372 11.00000 0.01606 0.03323 = 0.02949 0.00019 0.00268 0.00371 O3 4 0.625382 0.118808 0.278671 11.00000 0.03729 0.03309 = 0.02219 -0.00578 0.00812 -0.00766 N1 3 0.903709 0.576431 0.375301 11.00000 0.01344 0.01775 = 0.02103 0.00008 -0.00080 -0.00173 C6 1 0.568827 0.218578 0.404361 11.00000 0.01220 0.02022 = 0.01646 -0.00351 0.00043 0.00101 C10 1 0.890647 0.291238 0.429331 11.00000 0.01407 0.01783 = 0.01735 -0.00374 0.00084 -0.00058 AFIX 43 H10 2 1.007568 0.353397 0.428157 11.00000 -1.20000 AFIX 0 C3 1 0.726643 0.348609 0.338761 11.00000 0.01318 0.01995 = 0.01528 0.00054 -0.00141 0.00264 C5 1 0.741146 0.323369 0.404833 11.00000 0.01376 0.01719 = 0.01539 -0.00313 0.00291 -0.00036 C9 1 0.868000 0.162356 0.456778 11.00000 0.01891 0.01818 = 0.01592 -0.00411 0.00095 0.00261 C7 1 0.542209 0.095016 0.430251 11.00000 0.01603 0.02007 = 0.01971 -0.00284 0.00404 -0.00302 AFIX 43 H7 2 0.427978 0.029121 0.429858 11.00000 -1.20000 AFIX 0 C18 1 0.900887 0.338417 0.313110 11.00000 0.01664 0.02100 = 0.01677 -0.00239 0.00003 -0.00404 C8 1 0.689626 0.066719 0.457972 11.00000 0.02058 0.01781 = 0.01668 -0.00275 0.00364 0.00102 C2 1 0.569483 0.244381 0.337760 11.00000 0.01288 0.02322 = 0.01592 0.00066 -0.00146 0.00137 C1 1 0.548222 0.112326 0.308866 11.00000 0.01283 0.02413 = 0.01943 -0.00019 -0.00310 0.00092 C16 1 0.376899 0.442552 0.375419 11.00000 0.01151 0.02776 = 0.02044 -0.00006 0.00108 0.00395 AFIX 43 H16 2 0.246353 0.480077 0.376597 11.00000 -1.20000 AFIX 0 C4 1 0.736377 0.459877 0.374219 11.00000 0.01121 0.01863 = 0.01697 -0.00117 0.00066 0.00103 C15 1 0.433318 0.256836 0.371534 11.00000 0.01238 0.02422 = 0.01755 -0.00113 0.00012 -0.00186 AFIX 13 H15 2 0.318343 0.181289 0.370097 11.00000 -1.20000 AFIX 0 C17 1 0.531219 0.545224 0.376954 11.00000 0.01458 0.02147 = 0.02150 -0.00060 0.00006 0.00414 AFIX 43 H17 2 0.517060 0.661693 0.379524 11.00000 -1.20000 AFIX 0 C14 1 0.665317 -0.054857 0.486641 11.00000 0.02715 0.02045 = 0.02344 0.00017 0.00595 -0.00024 AFIX 43 H14 2 0.548557 -0.117144 0.488031 11.00000 -1.20000 AFIX 0 C11 1 1.018189 0.128878 0.483196 11.00000 0.02248 0.02282 = 0.01984 -0.00358 -0.00247 0.00254 AFIX 43 H11 2 1.136973 0.188438 0.482095 11.00000 -1.20000 AFIX 0 C22 1 0.909812 0.697744 0.343488 11.00000 0.02288 0.02241 = 0.02730 0.00520 0.00241 -0.00367 AFIX 23 H22A 2 0.784507 0.697362 0.330271 11.00000 -1.20000 H22B 2 1.014570 0.667259 0.326294 11.00000 -1.20000 AFIX 0 C13 1 0.811921 -0.081260 0.512233 11.00000 0.03726 0.02288 = 0.02078 0.00340 0.00370 0.00604 AFIX 43 H13 2 0.793042 -0.160237 0.531041 11.00000 -1.20000 AFIX 0 C12 1 0.990932 0.009734 0.510414 11.00000 0.03199 0.02538 = 0.02055 -0.00058 -0.00556 0.00642 AFIX 43 H12 2 1.090714 -0.010865 0.527649 11.00000 -1.20000 AFIX 0 C19 1 0.919312 0.678685 0.409645 11.00000 0.02394 0.02183 = 0.02545 -0.00429 -0.00271 -0.00273 AFIX 23 H19A 2 0.985531 0.615967 0.429190 11.00000 -1.20000 H19B 2 0.789449 0.713551 0.418330 11.00000 -1.20000 AFIX 0 C20 1 1.041637 0.829804 0.397587 11.00000 0.02261 0.02090 = 0.04382 -0.01017 0.00531 -0.00277 AFIX 23 H20A 2 1.180661 0.800550 0.395050 11.00000 -1.20000 H20B 2 1.028483 0.923160 0.414892 11.00000 -1.20000 AFIX 0 C24 1 0.418633 -0.153892 0.293443 11.00000 0.02974 0.03085 = 0.03045 -0.00954 -0.00311 -0.00873 AFIX 137 H24A 2 0.357086 -0.110967 0.271337 11.00000 -1.50000 H24B 2 0.338243 -0.242543 0.303710 11.00000 -1.50000 H24C 2 0.547448 -0.197842 0.287475 11.00000 -1.50000 AFIX 0 C23 1 1.044431 0.428184 0.257319 11.00000 0.03810 0.04532 = 0.02493 0.00304 0.01345 -0.00909 AFIX 137 H23A 2 1.015804 0.497341 0.236077 11.00000 -1.50000 H23B 2 1.070076 0.314275 0.249404 11.00000 -1.50000 H23C 2 1.158913 0.471952 0.269912 11.00000 -1.50000 AFIX 0 C21 1 0.949373 0.871670 0.360339 11.00000 0.04220 0.01995 = 0.04208 0.00176 0.00991 -0.00231 AFIX 23 H21A 2 1.039927 0.936637 0.345027 11.00000 -1.20000 H21B 2 0.827179 0.934886 0.363400 11.00000 -1.20000 AFIX 0 HKLF 4 REM r040_a.res in P2(1)2(1)2(1) REM R1 = 0.0285 for 3824 Fo > 4sig(Fo) and 0.0291 for all 3901 data REM 264 parameters refined using 0 restraints END WGHT 0.0472 0.3129 REM Highest difference peak 0.155, deepest hole -0.245, 1-sigma level 0.039 Q1 1 0.4982 0.2444 0.3531 11.00000 0.05 0.16 Q2 1 0.6362 0.5092 0.3749 11.00000 0.05 0.15 Q3 1 0.6551 0.2704 0.4043 11.00000 0.05 0.15 Q4 1 0.9321 0.1526 0.4714 11.00000 0.05 0.14 Q5 1 0.6794 0.0052 0.4713 11.00000 0.05 0.14 ; _shelx_res_checksum 15169 _shelx_hkl_file ; 0 0 3 -0.07 0.14 0 0 -3 0.73 0.21 0 0 4 2937.60 55.59 0 0 -4 3016.88 55.60 0 0 -5 -0.03 0.27 0 0 5 0.17 0.32 0 0 -6 1752.72 34.02 0 0 6 1760.52 34.03 0 0 -7 0.37 0.40 0 0 7 0.10 0.36 0 0 -8 867.36 18.06 0 0 8 821.86 18.02 0 0 -9 0.85 0.62 0 0 9 0.45 0.60 0 0 10 2274.41 44.18 0 0 -10 2176.86 44.01 0 0 11 -0.31 0.57 0 0 -11 0.40 0.66 0 0 12 0.98 0.70 0 0 -12 0.68 0.62 0 0 -13 0.61 0.78 0 0 13 1.10 0.77 0 0 -14 2.79 0.94 0 0 14 3.73 1.10 0 0 15 -0.62 0.84 0 0 -15 0.44 0.70 0 0 16 326.58 10.87 0 0 -16 335.77 10.71 0 0 -17 -0.11 0.88 0 0 17 0.35 0.77 0 0 -18 109.02 5.85 0 0 18 114.01 6.15 0 0 19 -0.02 1.06 0 0 -19 0.29 1.05 0 0 20 2040.62 44.08 0 0 -20 1876.74 43.00 0 0 21 0.20 1.12 0 0 -21 -0.22 1.23 0 0 -22 431.89 14.68 0 0 22 430.62 15.00 0 0 23 0.82 1.23 0 0 -23 1.20 1.18 0 0 24 283.69 12.19 0 0 -24 277.44 11.61 0 0 -25 -0.11 0.91 0 0 -25 0.31 0.98 0 0 25 0.80 1.22 0 0 -26 251.59 11.43 0 0 26 258.72 12.05 0 0 -26 260.10 8.62 0 0 -27 0.62 1.16 0 0 -27 -0.69 0.90 0 0 27 -0.89 1.34 0 0 27 3.14 0.93 0 0 -28 244.43 11.67 0 0 28 282.04 7.71 0 0 28 255.85 12.37 0 0 -28 265.22 9.36 0 0 -28 250.46 9.25 0 0 29 1.73 1.54 0 0 29 1.21 0.67 0 0 -29 -0.47 1.08 0 0 -29 2.87 1.45 0 0 -29 -0.15 1.23 0 0 30 215.02 11.26 0 0 30 212.99 6.82 0 0 -30 213.61 8.61 0 0 -30 204.39 10.59 0 0 -30 191.23 8.38 0 0 31 0.87 1.05 0 0 31 1.60 0.98 0 0 -31 -0.96 1.50 0 0 -31 -0.35 1.14 0 0 -31 0.34 1.28 0 0 31 -0.13 1.20 0 0 -32 880.57 22.80 0 0 -32 842.97 24.81 0 0 32 889.42 19.86 0 0 32 862.34 21.90 0 0 32 906.11 26.29 0 0 -32 863.82 22.60 0 0 33 3.10 1.36 0 0 -33 3.55 1.67 0 0 -33 1.87 1.29 0 0 34 1351.52 31.67 0 0 -34 1398.11 32.63 0 0 -34 1436.14 32.61 0 0 -35 3.76 1.59 0 0 35 3.34 1.49 0 0 -35 4.06 1.76 0 0 -35 3.78 1.58 0 0 -36 2088.16 45.21 0 0 -36 1987.69 44.32 0 0 36 2078.97 44.37 0 0 -37 3.12 1.38 0 0 -37 1.66 1.11 0 0 37 5.35 1.50 0 0 -37 2.56 1.50 0 0 38 181.90 7.15 0 0 -38 174.88 7.40 0 0 -38 169.08 6.89 0 0 -38 172.19 7.16 0 0 -39 2.08 1.14 0 0 -39 0.89 0.80 0 0 -39 0.17 0.99 0 0 39 1.18 0.85 0 0 40 7.55 1.36 0 0 -40 7.41 1.41 0 0 -40 8.46 1.68 0 0 41 0.33 0.72 0 0 -41 1.46 0.83 0 0 -41 -0.78 1.06 0 0 -42 19.43 2.02 0 0 42 15.67 1.60 0 0 -43 0.85 0.64 0 0 43 -0.44 0.44 0 0 44 -0.11 0.36 0 0 -44 0.36 0.59 0 0 -45 0.62 0.51 0 1 0 0.12 0.16 0 1 0 0.36 0.30 0 -1 1 2925.54 55.75 0 1 -1 2933.76 55.74 0 -1 -1 2967.40 55.65 0 1 -1 2977.11 55.04 0 1 1 2980.71 55.74 0 1 1 2975.64 55.09 0 1 2 679.89 13.45 0 1 -2 663.14 13.95 0 -1 2 665.00 13.98 0 1 2 663.17 13.88 0 1 2 685.34 13.61 0 1 -2 678.24 13.36 0 -1 -2 663.86 13.82 0 -1 -2 665.40 13.60 0 1 3 778.44 15.85 0 -1 -3 784.12 15.53 0 1 -3 792.50 15.64 0 -1 3 790.58 16.27 0 1 -3 845.58 16.28 0 -1 -3 755.04 15.93 0 1 3 740.74 15.96 0 1 -3 803.34 15.84 0 1 -4 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5.25 1.66 0 4 2 7.41 1.28 0 4 -3 343.63 12.25 0 -4 3 354.83 12.76 0 4 -3 361.00 9.81 0 4 3 346.68 9.91 0 -4 -3 333.07 11.51 0 4 3 342.83 12.13 0 -4 -3 352.29 12.72 0 -4 3 351.83 12.74 0 -4 -4 788.74 20.59 0 4 -4 809.82 18.55 0 -4 4 783.03 22.40 0 -4 -4 804.88 22.27 0 4 4 844.55 19.01 0 -4 4 822.89 22.41 0 4 4 817.31 21.64 0 4 -4 773.11 21.58 0 4 -5 1.30 1.04 0 -4 -5 2.39 1.17 0 4 -5 2.74 0.82 0 -4 5 0.67 1.25 0 4 5 2.51 0.89 0 4 5 1.10 1.00 0 -4 -5 1.76 1.07 0 -4 5 1.99 1.60 0 -4 -6 368.73 10.32 0 4 -6 352.41 9.99 0 -4 6 350.36 12.92 0 -4 -6 339.26 11.17 0 -4 6 348.99 13.36 0 4 6 354.97 10.42 0 -4 -6 356.71 11.53 0 -4 -6 363.46 13.08 0 4 -6 337.11 12.37 0 4 6 352.76 12.39 0 4 -7 20.27 1.96 0 -4 -7 21.93 2.05 0 4 7 20.91 2.17 0 -4 7 22.20 3.20 0 -4 -7 21.45 2.98 0 4 7 21.90 2.83 0 -4 7 21.40 2.93 0 -4 -7 18.74 2.24 0 4 -7 22.18 2.88 0 -4 -7 23.05 2.45 0 4 -8 1.38 1.00 0 4 8 0.94 1.09 0 -4 -8 3.37 1.08 0 -4 -8 3.47 1.69 0 -4 8 1.32 1.75 0 -4 -8 5.96 1.41 0 -4 -8 1.46 0.70 0 -4 8 2.87 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103.59 6.65 0 -5 23 101.36 5.91 0 -5 -24 18.84 2.84 0 -5 24 22.82 2.80 0 -5 24 19.90 2.43 0 5 -24 19.17 2.74 0 5 24 21.16 2.49 0 5 24 19.87 2.29 0 -5 -24 22.77 2.81 0 5 25 6.83 1.47 0 -5 25 8.23 1.74 0 -5 25 7.55 1.70 0 -5 -25 7.26 1.74 0 5 25 6.81 1.64 0 5 -25 7.24 1.83 0 -5 -25 8.08 2.23 0 -5 -26 13.80 2.37 0 -5 -26 14.89 2.57 0 5 -26 14.62 1.76 0 -5 26 14.50 2.09 0 5 26 14.00 1.91 0 5 -26 12.75 2.21 0 -5 26 14.60 2.26 0 5 26 14.82 2.16 0 -5 -27 23.41 2.87 0 5 27 27.92 2.55 0 -5 -27 23.30 3.15 0 5 -27 26.74 2.24 0 5 27 26.69 2.77 0 -5 27 24.20 2.88 0 5 -27 27.08 3.21 0 -5 27 24.48 2.56 0 5 28 68.86 3.91 0 -5 -28 72.14 5.47 0 5 -28 68.35 4.91 0 -5 -28 65.63 4.70 0 5 28 71.98 4.50 0 -5 28 70.34 4.76 0 -5 28 75.15 4.33 0 -5 -29 370.25 13.37 0 -5 29 360.27 11.04 0 5 -29 387.79 13.03 0 -5 29 366.39 12.23 0 5 29 386.68 11.89 0 -5 -29 394.10 12.72 0 5 29 396.12 10.69 0 -5 30 27.64 2.37 0 5 -30 26.69 3.02 0 -5 -30 26.69 3.22 0 -5 30 26.20 2.78 0 5 30 25.52 2.55 0 -5 -30 25.70 2.92 0 5 -31 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1 125.25 8.90 0 6 1 126.48 4.21 0 6 -1 122.70 8.25 0 -6 1 121.76 5.87 0 6 1 121.36 8.18 0 -6 -1 118.04 5.89 0 6 -1 123.71 4.37 0 6 -1 121.60 4.86 0 -6 -1 119.28 8.01 0 6 1 121.69 5.65 0 -6 -1 120.53 8.81 0 6 -1 129.88 5.73 0 -6 -1 119.36 6.18 0 -6 -1 113.48 8.10 0 6 1 114.42 4.82 0 -6 1 127.25 8.91 0 -6 2 22.46 3.76 0 -6 2 18.51 3.43 0 -6 2 22.09 2.40 0 -6 -2 20.33 2.44 0 6 -2 22.86 2.31 0 -6 -2 25.48 4.04 0 6 2 20.25 1.90 0 -6 -2 25.11 3.76 0 6 -2 23.63 3.54 0 -6 2 23.70 4.08 0 6 2 20.48 1.54 0 -6 -2 27.38 2.89 0 6 2 21.35 2.32 0 6 -2 21.33 1.96 0 6 -2 23.69 1.75 0 -6 -2 22.88 3.38 0 6 2 26.87 3.83 0 -6 2 25.87 2.87 0 6 3 65.25 4.06 0 -6 -3 67.10 6.53 0 -6 -3 66.70 4.52 0 6 -3 60.80 5.72 0 -6 3 56.03 6.14 0 -6 3 65.48 4.14 0 -6 -3 61.11 5.61 0 -6 -3 61.80 4.26 0 6 -3 67.73 3.95 0 -6 3 65.70 6.27 0 6 -3 69.74 3.14 0 -6 3 64.31 4.49 0 6 3 67.65 6.02 0 6 -3 65.14 3.34 0 6 3 67.84 2.78 0 -6 -3 71.52 5.72 0 -6 3 53.74 5.84 0 6 3 66.50 3.53 0 -6 4 12.32 1.82 0 -6 -4 17.15 2.37 0 6 -4 19.46 3.33 0 -6 -4 15.64 2.20 0 -6 4 16.72 3.27 0 -6 -4 22.20 3.95 0 6 -4 15.06 1.55 0 6 -4 15.09 1.67 0 -6 4 12.76 2.08 0 -6 -4 9.39 2.16 0 -6 4 24.36 4.06 0 6 4 17.14 2.06 0 6 4 16.22 1.74 0 6 4 12.16 1.16 0 6 -4 15.23 1.85 0 -6 4 11.69 2.93 0 6 4 12.49 2.60 0 -6 -4 14.91 2.96 0 6 -5 247.45 7.53 0 6 -5 227.13 11.49 0 -6 -5 265.14 13.37 0 -6 -5 244.48 9.18 0 6 5 242.41 7.92 0 -6 5 230.70 8.60 0 -6 5 274.41 13.29 0 -6 5 252.83 9.69 0 6 5 252.23 12.17 0 -6 -5 251.29 9.41 0 6 -5 249.08 7.29 0 -6 5 237.52 12.55 0 6 -5 253.53 8.43 0 -6 5 223.02 12.78 0 -6 -5 244.60 10.80 0 -6 -5 252.71 10.92 0 6 5 263.82 8.99 0 6 6 1.13 0.94 0 -6 -6 0.28 1.11 0 -6 6 -0.29 1.62 0 6 -6 2.40 0.75 0 -6 6 -0.13 1.11 0 6 -6 4.54 1.16 0 -6 -6 1.79 1.24 0 6 -6 1.27 1.34 0 -6 -6 3.27 1.69 0 -6 6 1.49 2.17 0 -6 -6 1.28 1.45 0 -6 -6 2.13 1.88 0 -6 6 1.32 1.00 0 6 6 0.44 0.84 0 6 6 -0.33 1.38 0 -6 6 -1.30 2.41 0 6 7 20.15 3.30 0 6 -7 22.41 2.19 0 -6 -7 18.87 3.60 0 -6 -7 20.24 2.58 0 6 7 20.64 2.13 0 6 7 19.83 2.32 0 6 -7 20.83 1.82 0 -6 7 20.46 2.60 0 -6 -7 17.65 2.35 0 -6 7 18.53 3.81 0 -6 7 19.33 2.10 0 -6 7 13.95 3.19 0 6 -7 21.40 2.45 0 6 -7 16.88 3.04 0 -6 8 179.22 7.97 0 -6 8 179.97 6.82 0 6 -8 176.92 6.64 0 -6 -8 180.65 8.03 0 -6 8 171.55 10.87 0 6 -8 175.66 7.38 0 6 -8 169.63 9.73 0 6 8 181.58 10.00 0 -6 -8 181.62 7.62 0 6 -8 192.03 6.36 0 -6 -8 184.69 11.03 0 6 8 178.54 6.72 0 6 8 168.70 7.20 0 -6 8 176.71 11.37 0 -6 9 36.54 5.36 0 6 9 41.63 2.98 0 6 -9 40.51 4.66 0 -6 9 31.88 4.68 0 6 -9 37.06 2.59 0 -6 -9 35.55 4.85 0 -6 -9 35.23 3.19 0 -6 -9 36.52 3.48 0 6 -9 33.50 3.09 0 6 9 34.71 3.04 0 -6 9 38.94 3.06 0 6 9 40.59 4.59 0 -6 9 39.89 3.64 0 -6 -10 127.38 8.88 0 -6 10 118.56 5.66 0 6 10 119.50 5.89 0 -6 10 107.29 9.02 0 6 -10 114.15 5.95 0 6 -10 118.02 7.67 0 6 10 120.07 7.97 0 -6 -10 117.96 6.51 0 6 -10 119.66 4.97 0 6 10 122.05 5.45 0 -6 -10 119.07 6.03 0 -6 10 111.19 6.21 0 -6 10 115.30 8.94 0 -6 11 103.94 8.88 0 -6 11 110.57 5.59 0 -6 -11 104.88 6.19 0 -6 -11 109.61 8.19 0 6 -11 112.88 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46.10 3.89 0 -6 -23 57.25 3.52 0 6 23 51.92 3.61 0 -6 23 53.03 3.97 0 6 23 52.73 3.84 0 -6 24 45.14 3.62 0 6 -24 48.00 4.01 0 -6 24 53.48 4.12 0 6 24 51.85 3.68 0 -6 -24 50.25 4.52 0 6 24 47.00 3.38 0 -6 -24 47.57 3.22 0 6 -24 57.80 3.86 0 -6 -25 0.84 1.01 0 6 25 0.29 0.77 0 6 -25 3.60 1.09 0 6 25 0.34 0.87 0 -6 25 0.46 0.87 0 -6 -25 1.04 1.41 0 -6 25 1.08 0.97 0 6 -25 1.34 1.05 0 -6 -26 -0.29 1.07 0 6 26 -0.03 0.86 0 6 26 -0.16 0.68 0 -6 26 0.01 0.99 0 6 -26 0.07 0.93 0 6 -26 -0.27 1.20 0 -6 26 0.44 0.84 0 -6 -26 -1.01 1.47 0 -6 -27 10.35 1.63 0 6 -27 8.28 1.76 0 -6 27 9.03 1.58 0 6 27 8.62 1.50 0 -6 27 8.83 1.78 0 6 27 5.99 1.16 0 -6 -27 5.74 1.77 0 6 -28 3.26 0.93 0 -6 28 1.89 0.98 0 -6 28 0.07 0.84 0 6 28 1.44 0.76 0 6 28 2.04 0.77 0 6 -28 1.61 1.25 0 -6 -28 2.00 1.15 0 -6 -28 1.58 1.05 0 6 29 62.67 3.63 0 -6 29 69.75 4.21 0 6 29 70.57 3.25 0 -6 29 63.82 3.45 0 -6 -29 61.55 4.43 0 6 -29 70.52 4.41 0 -6 -29 65.14 3.53 0 -6 -30 0.85 0.63 0 -6 30 2.20 1.00 0 -6 30 1.77 0.77 0 6 -30 3.35 1.29 0 6 30 3.36 0.90 0 -6 -30 4.37 1.42 0 -6 31 -0.52 0.56 0 -6 31 0.85 0.75 0 6 -31 -1.13 1.03 0 6 31 0.69 0.64 0 -6 -31 -0.13 0.60 0 -6 -31 0.51 0.87 0 6 32 26.90 2.04 0 -6 -32 28.69 2.62 0 -6 32 24.51 2.16 0 6 -32 27.86 2.38 0 -6 32 28.04 1.65 0 -6 -32 24.17 1.86 0 6 33 48.17 2.59 0 -6 33 48.71 2.84 0 6 -33 49.35 3.05 0 -6 -33 48.73 2.34 0 -6 -33 46.00 3.10 0 -6 -34 60.41 3.28 0 -6 34 61.32 2.97 0 6 34 58.94 2.70 0 6 -34 58.94 3.09 0 -6 -35 6.29 0.95 0 6 -35 4.71 0.94 0 -6 35 3.38 0.68 0 6 35 4.27 0.68 0 7 0 5.91 1.24 0 7 0 -0.84 0.86 0 7 0 1.19 1.03 0 -7 0 -0.04 1.18 0 7 0 2.78 1.47 0 -7 0 0.77 1.21 0 -7 0 -0.04 1.78 0 -7 0 -0.36 1.88 0 -7 0 1.47 2.03 0 7 -1 71.79 3.38 0 -7 1 64.06 4.96 0 -7 1 71.61 5.81 0 7 1 64.23 3.80 0 -7 -1 71.63 6.68 0 -7 -1 72.05 5.65 0 7 -1 67.35 4.47 0 -7 1 69.75 6.57 0 -7 1 68.99 6.06 0 7 -1 62.31 5.75 0 -7 1 70.82 4.79 0 7 1 70.03 3.23 0 7 -1 65.89 3.74 0 7 1 67.40 4.47 0 7 1 64.15 5.76 0 -7 -1 71.08 5.16 0 -7 -1 83.80 6.14 0 -7 -1 67.58 4.79 0 -7 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76.76 4.86 0 7 5 80.78 4.38 0 -7 5 84.02 6.90 0 -7 6 -1.28 1.75 0 7 6 0.29 1.53 0 7 6 -0.33 1.16 0 -7 -6 0.91 1.33 0 7 -6 0.67 1.51 0 -7 6 0.42 1.14 0 7 -6 0.43 0.81 0 -7 6 -0.50 2.79 0 -7 -6 0.76 1.10 0 7 -6 0.79 0.73 0 7 6 0.33 0.78 0 7 -6 0.77 1.00 0 7 7 26.72 2.50 0 -7 -7 32.58 3.55 0 7 -7 29.94 2.35 0 -7 -7 33.16 3.41 0 7 -7 26.72 2.85 0 -7 7 30.22 3.43 0 7 7 28.07 2.93 0 -7 -8 40.18 3.70 0 7 -8 37.64 3.42 0 -7 -8 39.25 3.84 0 -7 8 41.66 3.92 0 7 8 44.15 3.23 0 7 -8 40.12 2.72 0 7 8 41.73 3.61 0 -7 8 45.02 3.30 0 7 -9 1.68 0.85 0 -7 -9 0.35 0.98 0 -7 -9 1.75 1.71 0 7 -9 1.37 1.10 0 7 9 1.35 1.25 0 -7 9 1.01 1.26 0 -7 9 3.57 1.20 0 7 9 0.41 0.86 0 -7 10 309.39 10.27 0 -7 10 301.34 11.66 0 7 10 317.17 11.00 0 7 10 309.42 9.92 0 -7 -10 314.87 11.95 0 7 -10 301.98 10.87 0 7 -10 317.27 9.29 0 -7 -10 304.12 11.23 0 -7 -11 148.47 7.22 0 -7 -11 151.94 7.92 0 -7 11 152.72 6.75 0 -7 11 147.35 7.62 0 7 11 142.32 6.90 0 7 -11 148.82 7.14 0 7 11 149.57 6.40 0 7 12 66.32 4.08 0 -7 12 69.73 4.44 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0.55 0.67 -1 -9 -7 28.77 2.36 1 -9 7 31.20 2.59 1 9 -7 32.64 2.38 -1 -9 -6 12.68 1.62 1 -9 6 12.91 1.80 1 9 -6 14.16 1.70 1 -9 5 152.87 6.30 -1 -9 -5 154.07 5.81 1 9 -5 160.63 5.82 -1 -9 -4 71.04 3.69 1 -9 4 74.42 4.24 1 9 -4 71.83 3.72 1 -9 3 49.49 3.47 1 9 -3 53.51 3.22 -1 -9 -3 51.28 3.04 -1 -9 -2 125.34 4.89 1 -9 2 134.68 5.91 1 9 -2 125.73 5.09 -1 -9 -1 32.90 2.33 1 -9 1 37.74 3.03 1 9 -1 36.01 2.59 -1 -9 -1 34.14 2.27 -1 -9 0 41.81 2.73 1 -9 0 43.48 3.23 1 9 0 36.97 2.60 -1 -9 0 43.43 2.42 1 9 1 34.61 2.51 -1 -9 1 35.34 2.02 1 -9 -1 36.66 3.00 -1 -9 1 34.36 2.56 1 9 2 130.85 5.10 1 -9 -2 138.75 5.96 -1 -9 2 122.65 5.20 -1 9 -3 48.93 2.72 1 9 3 50.93 2.99 -1 -9 3 53.99 3.29 1 -9 -3 56.97 3.64 -1 9 -4 64.68 3.33 -1 -9 4 77.11 4.02 1 -9 -4 79.62 4.27 1 9 4 72.93 3.65 -1 9 -5 145.61 5.46 1 9 5 155.81 5.42 -1 -9 5 150.80 5.97 1 9 5 146.45 5.30 1 -9 -5 159.05 6.23 -1 9 -6 9.31 1.34 -1 -9 6 13.47 1.70 1 9 6 11.32 1.39 1 -9 -6 10.95 1.61 1 9 6 11.75 1.40 -1 9 -7 31.89 2.43 -1 -9 7 37.78 2.74 1 -9 -7 33.17 2.62 1 9 7 33.89 2.19 1 9 7 32.36 2.23 -1 9 -8 1.27 0.78 1 9 8 0.32 0.50 -1 -9 8 0.20 0.75 1 -9 -8 0.61 0.73 1 9 8 0.26 0.64 -1 -9 9 24.01 2.21 1 9 9 19.66 1.74 -1 9 -9 21.42 1.99 1 9 9 19.32 1.53 1 -9 -9 23.40 2.05 1 -9 -10 93.19 4.05 -1 -9 10 101.67 4.53 1 9 10 92.46 3.94 -1 9 -10 96.93 4.30 -1 9 -11 12.07 1.52 1 -9 -11 9.26 1.19 -1 -9 11 11.16 1.53 1 9 11 8.62 1.19 -1 9 -12 84.66 3.87 1 9 12 83.61 3.59 1 -9 -12 87.13 3.38 -1 -9 12 83.58 3.96 -1 9 -13 19.67 1.75 1 9 13 22.17 1.72 -1 -9 13 21.28 1.87 -1 9 -14 6.81 1.07 -1 -9 14 8.39 1.18 1 9 14 7.53 1.02 -1 9 -15 29.10 2.03 1 9 15 27.66 1.77 -1 -9 15 29.60 2.05 -1 9 -16 25.69 1.84 -1 -9 16 27.89 1.88 1 9 16 26.22 1.67 -1 9 -17 26.97 1.76 -1 -9 17 30.55 1.86 1 9 17 28.86 1.61 -2 0 0 9999.00 185.40 -2 0 0 9832.79 183.11 -2 0 1 690.72 16.86 -2 0 -1 655.57 14.99 -2 0 1 719.26 15.16 2 0 1 698.89 13.92 -2 0 -1 634.09 16.63 -2 0 2 822.41 19.73 -2 0 -2 809.80 19.83 -2 0 -2 824.38 18.04 -2 0 2 837.42 18.02 2 0 2 865.98 16.48 -2 0 3 1304.11 28.20 -2 0 -3 1250.35 28.40 2 0 -3 1307.35 26.68 -2 0 -3 1289.38 26.66 -2 0 3 1281.58 26.48 2 0 3 1316.45 24.47 -2 0 -4 326.68 8.54 -2 0 4 323.76 9.52 2 0 -4 308.13 8.45 -2 0 4 315.30 8.32 -2 0 -4 316.17 9.78 -2 0 5 105.16 4.78 2 0 5 121.77 3.10 -2 0 -5 104.00 5.05 -2 0 5 107.80 4.16 2 0 5 118.85 4.35 -2 0 -5 106.87 4.28 2 0 -5 103.13 4.22 -2 0 6 121.54 4.53 -2 0 6 120.06 5.16 -2 0 -6 119.36 4.69 2 0 6 116.94 4.57 -2 0 -6 111.90 5.31 2 0 -6 117.44 4.68 2 0 6 129.42 2.88 -2 0 7 34.42 2.54 -2 0 -7 33.05 2.74 -2 0 7 34.58 2.29 2 0 -7 32.68 2.32 2 0 7 36.24 2.41 2 0 -8 136.07 5.35 -2 0 8 127.66 5.27 2 0 8 141.78 5.31 -2 0 -8 126.14 5.64 -2 0 8 133.73 5.13 -2 0 -9 0.69 0.72 -2 0 9 1.03 0.52 2 0 9 0.64 0.67 -2 0 9 0.15 0.51 2 0 -9 0.67 0.69 2 0 10 389.78 11.08 2 0 -10 373.79 11.13 -2 0 -10 388.92 11.55 -2 0 10 397.11 11.00 -2 0 10 385.40 10.61 2 0 11 493.97 13.44 -2 0 11 488.88 12.59 -2 0 11 492.91 13.35 -2 0 -11 498.46 13.75 2 0 -11 492.85 13.68 2 0 12 520.47 14.36 -2 0 12 517.24 13.14 -2 0 12 538.23 14.30 2 0 -12 539.60 14.77 2 0 13 280.55 9.44 -2 0 13 259.07 7.76 2 0 -13 254.67 9.33 -2 0 13 265.54 9.04 -2 0 14 46.63 2.68 2 0 14 45.60 3.60 2 0 15 1805.95 40.13 -2 0 15 1855.25 39.88 2 0 -15 1837.22 40.54 2 0 16 1308.61 30.48 2 0 -16 1254.11 30.58 -2 0 16 1291.97 30.01 -2 0 17 2.74 1.25 2 0 17 1.19 0.93 2 0 -17 1.03 1.07 2 0 18 173.91 8.22 -2 0 18 166.13 7.86 2 0 -18 165.11 8.18 -2 0 19 204.30 9.10 2 0 -19 206.95 9.53 2 0 19 211.49 9.39 2 0 -20 192.73 9.34 -2 0 20 192.96 8.97 2 0 20 187.50 9.03 -2 0 21 65.44 5.17 2 0 -21 74.86 5.65 2 0 21 57.37 4.88 -2 0 -22 -0.21 0.95 -2 0 22 0.23 1.06 2 0 22 -0.08 0.99 -2 0 22 -0.26 0.79 -2 0 -22 2.60 1.19 2 0 -22 2.45 1.61 -2 0 -23 332.38 10.84 2 0 -23 332.93 13.72 -2 0 -23 324.33 10.98 -2 0 23 341.11 13.45 -2 0 -23 353.52 10.33 2 0 23 351.14 13.74 -2 0 23 366.89 10.49 -2 0 -24 198.34 8.15 -2 0 -24 223.01 7.78 -2 0 24 214.90 7.74 -2 0 -24 206.55 8.44 -2 0 24 213.05 10.36 2 0 -24 217.03 10.68 2 0 24 200.72 10.26 -2 0 -25 52.00 4.02 -2 0 25 53.42 3.64 -2 0 -25 46.10 3.94 -2 0 25 47.96 4.79 2 0 -25 40.32 4.53 -2 0 -25 50.08 3.53 2 0 25 50.12 5.05 -2 0 -26 53.69 3.83 -2 0 26 65.94 5.57 -2 0 -26 54.05 4.36 -2 0 26 60.32 3.96 -2 0 -26 56.60 4.30 2 0 -26 54.82 5.28 2 0 26 52.31 5.15 -2 0 27 6.73 1.53 -2 0 -27 10.14 1.96 -2 0 -27 10.78 1.89 -2 0 27 8.64 2.06 -2 0 -27 8.82 2.07 2 0 -27 6.55 2.08 2 0 27 13.48 2.92 -2 0 -28 90.71 5.24 -2 0 -28 80.83 5.41 -2 0 28 87.71 6.37 -2 0 28 88.58 5.04 2 0 28 92.99 7.08 -2 0 -28 83.96 5.65 2 0 -28 82.42 6.69 -2 0 28 85.75 6.62 -2 0 -29 10.20 2.10 -2 0 29 10.04 2.24 2 0 29 9.02 2.34 -2 0 29 10.22 1.74 -2 0 -29 9.66 1.82 -2 0 -29 10.42 2.17 2 0 -29 11.67 2.89 -2 0 -30 29.48 3.39 -2 0 30 31.27 3.00 -2 0 -30 32.21 3.18 2 0 30 35.13 4.23 -2 0 30 35.65 4.17 2 0 -30 30.99 3.99 -2 0 -30 34.61 3.74 -2 0 -31 12.34 2.38 -2 0 -31 13.84 2.27 2 0 -31 15.33 2.47 -2 0 31 17.89 2.31 -2 0 -31 11.51 2.36 -2 0 -32 8.10 2.14 -2 0 -32 7.45 1.76 -2 0 32 11.11 1.87 -2 0 -32 5.73 1.86 2 0 -32 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94.40 4.53 -7 -3 -2 61.48 4.08 -7 -3 -2 62.61 3.59 -7 3 2 65.60 3.76 -7 3 2 58.47 3.62 -7 -3 -1 10.78 1.44 -7 3 1 7.97 1.56 -7 -3 -1 7.25 1.55 -7 -3 -1 8.13 1.42 -7 3 1 6.86 1.38 -7 -3 0 67.53 4.25 -7 -3 0 68.69 3.88 -7 3 0 71.59 3.94 -7 3 0 73.97 4.30 -7 3 -1 5.83 1.30 -7 3 -1 7.18 1.56 -7 -3 1 8.66 1.70 -7 -3 1 6.20 1.28 -7 3 -1 8.32 1.53 -7 -3 2 61.58 4.01 -7 -3 2 59.78 3.69 -7 3 -2 67.80 3.87 -7 3 -2 59.56 4.06 -7 -3 3 95.05 4.91 -7 -3 3 93.51 4.74 -7 3 -3 96.26 4.69 -7 3 -3 86.88 4.97 -7 3 -3 106.25 4.71 -7 -3 4 115.60 5.40 -7 -3 4 120.28 5.39 -7 3 -4 114.25 5.15 -7 3 -4 111.84 5.77 -7 3 -4 122.98 5.16 -7 3 -5 0.89 1.02 -7 -3 5 -0.26 0.80 -7 -3 5 0.84 0.98 -7 -3 6 58.52 3.50 -7 -3 6 59.16 3.62 -7 3 -6 58.00 4.08 -7 3 -6 53.76 3.22 -7 -3 7 94.51 4.48 -7 -3 7 98.81 4.78 -7 3 -7 97.65 5.36 -7 3 -7 100.81 4.42 -7 -3 8 119.76 4.94 -7 -3 8 124.27 5.34 -7 3 -8 116.13 5.91 -7 3 -8 120.13 4.84 -7 3 -9 81.65 3.77 -7 -3 9 74.64 3.61 -7 -3 9 68.08 3.88 -7 3 -9 75.49 4.62 -7 3 -10 5.52 1.22 -7 3 -10 4.02 1.17 -7 -3 10 5.81 0.99 -7 -3 10 3.19 1.00 -7 3 -11 7.67 1.21 -7 3 -11 7.14 1.58 -7 -3 11 7.74 1.01 -7 -3 11 8.85 1.36 -7 -3 12 50.30 2.18 -7 -3 12 41.77 2.79 -7 3 -12 42.49 3.30 -7 3 -13 10.72 1.75 -7 -3 13 12.67 1.50 -7 -3 14 29.19 2.17 -7 3 -14 29.28 2.60 -7 -3 15 102.36 4.17 -7 3 -15 93.95 4.61 -7 -3 16 21.87 1.75 -7 3 -16 18.25 1.93 -7 -3 17 112.23 4.12 -7 3 -17 117.19 4.75 -7 -3 18 38.56 2.11 -7 3 -18 42.58 2.57 -7 3 -19 4.66 0.94 -7 -3 19 4.53 0.74 -7 3 -20 0.69 0.44 -7 -3 20 0.79 0.37 -7 -4 -15 6.72 0.82 -7 -4 -14 68.65 2.96 -7 -4 -13 5.34 0.95 -7 4 13 6.66 0.73 -7 -4 -12 32.28 2.27 -7 4 12 33.77 1.67 -7 -4 -11 145.79 5.48 -7 4 11 154.15 4.47 -7 -4 -10 87.91 4.16 -7 4 10 86.23 3.26 -7 -4 -9 29.35 2.40 -7 4 9 27.30 1.80 -7 -4 -8 2.75 1.03 -7 4 8 2.65 0.74 -7 -4 -7 85.46 4.36 -7 4 7 82.95 3.50 -7 -4 -6 9.26 1.56 -7 4 6 10.16 1.31 -7 -4 -5 63.48 3.71 -7 4 5 54.25 2.90 -7 -4 -4 6.23 1.24 -7 4 4 7.11 1.19 -7 -4 -3 5.25 1.27 -7 -4 -3 7.03 0.97 -7 4 3 8.31 1.37 -7 -4 -2 14.65 1.82 -7 -4 -2 14.72 1.42 -7 4 2 19.54 1.89 -7 -4 -1 35.80 2.74 -7 -4 -1 29.67 2.05 -7 4 0 4.59 1.02 -7 -4 0 2.84 1.00 -7 -4 0 3.03 0.86 -7 -4 1 33.73 2.58 -7 -4 1 30.42 2.17 -7 4 -1 32.61 2.41 -7 -4 2 16.64 1.81 -7 -4 2 13.94 1.50 -7 4 -2 16.94 1.81 -7 4 -3 4.56 1.12 -7 -4 3 8.17 1.30 -7 -4 3 6.80 1.13 -7 4 -4 5.46 1.23 -7 -4 4 7.05 1.20 -7 -4 4 6.31 1.13 -7 -4 5 61.79 3.22 -7 -4 5 64.05 3.31 -7 4 -5 62.14 3.63 -7 4 -6 9.25 1.47 -7 -4 6 9.88 1.23 -7 -4 6 9.79 1.33 -7 -4 7 84.99 3.43 -7 -4 7 79.07 3.76 -7 4 -7 82.60 4.25 -7 4 -8 4.22 1.19 -7 -4 8 5.68 0.87 -7 -4 8 4.74 1.03 -7 -4 9 29.14 1.58 -7 -4 9 25.96 2.06 -7 4 -9 29.06 2.45 -7 -4 10 88.49 3.87 -7 4 -10 86.76 4.28 -7 -4 11 152.50 5.28 -7 4 -11 150.68 5.79 -7 -4 12 40.72 2.43 -7 4 -12 35.72 2.59 -7 4 -13 6.45 1.20 -7 -4 13 6.26 0.97 -7 -4 14 67.44 3.02 -7 4 -14 70.08 3.46 -7 4 -15 8.49 1.17 -7 -4 15 8.79 1.06 -7 -4 16 16.29 1.31 -7 4 -16 18.30 1.58 -7 4 -17 5.85 0.84 -7 -4 17 5.03 0.67 -7 -5 -10 51.10 2.37 -7 -5 -9 1.22 0.59 -7 -5 -8 20.29 1.62 -7 -5 -7 51.15 2.66 -7 -5 -6 5.99 1.00 -7 -5 -5 22.99 1.81 -7 -5 -4 10.24 1.31 -7 -5 -3 15.06 1.47 -7 -5 -2 2.22 0.77 -7 -5 -1 20.08 1.66 -7 -5 0 7.98 1.09 -7 -5 1 20.24 1.54 -7 -5 2 3.70 0.75 -7 -5 3 16.08 1.23 -7 -5 4 9.43 0.88 -7 -5 5 23.42 1.32 -7 5 -6 5.22 0.80 -7 -5 6 3.65 0.61 -7 -5 7 48.93 2.07 -7 5 -7 54.31 2.41 -7 -5 8 22.04 1.31 -7 5 -8 20.32 1.43 -8 0 0 37.27 2.40 -8 0 0 36.60 1.92 -8 0 -1 186.86 5.97 -8 0 1 177.42 5.86 -8 0 1 180.96 5.21 -8 0 -2 7.50 1.13 -8 0 2 10.15 1.28 -8 0 2 7.55 0.96 -8 0 -3 44.02 2.57 -8 0 3 38.21 2.35 -8 0 3 39.39 2.15 -8 0 4 19.68 1.62 -8 0 4 18.99 1.49 -8 0 5 6.07 1.01 -8 0 5 5.24 0.86 -8 0 6 56.32 2.72 -8 0 6 55.76 2.63 -8 0 -6 62.34 3.31 -8 0 7 19.69 1.52 -8 0 7 22.28 1.61 -8 0 8 61.92 2.71 -8 0 8 66.50 2.87 -8 0 9 22.81 1.46 -8 0 9 22.49 1.58 -8 0 -9 22.44 1.87 -8 0 10 1.16 0.42 -8 0 10 -0.12 0.43 -8 0 11 33.18 1.51 -8 0 11 36.27 1.89 -8 0 -11 34.55 2.22 -8 0 12 98.25 3.38 -8 0 -12 104.24 3.95 -8 0 13 23.12 1.42 -8 0 -13 25.82 1.78 -8 0 -14 96.46 3.47 -8 1 13 29.90 1.61 -8 1 12 10.45 0.98 -8 -1 -12 13.36 1.21 -8 -1 -11 6.96 1.02 -8 1 11 8.27 0.96 -8 -1 -10 1.73 0.52 -8 1 10 1.53 0.57 -8 -1 -9 51.15 2.50 -8 1 9 53.39 2.53 -8 -1 -9 53.78 2.75 -8 -1 -8 73.76 3.28 -8 1 8 68.59 3.04 -8 -1 -7 62.29 3.09 -8 1 7 57.83 2.75 -8 -1 -7 62.21 3.12 -8 -1 -6 5.11 1.17 -8 -1 -6 4.13 0.92 -8 1 6 3.69 0.78 -8 -1 -5 13.28 1.52 -8 -1 -5 15.04 1.39 -8 1 5 11.54 1.28 -8 -1 -5 14.21 1.75 -8 -1 -4 84.66 3.89 -8 -1 -4 77.15 3.38 -8 1 4 79.95 3.39 -8 -1 -4 85.88 3.86 -8 -1 -3 35.38 2.47 -8 -1 -3 33.59 2.19 -8 1 3 32.70 2.10 -8 -1 -2 207.86 6.90 -8 -1 -2 212.91 6.45 -8 1 2 217.61 6.31 -8 -1 -1 21.54 1.97 -8 -1 -1 19.25 1.71 -8 1 1 22.44 1.71 -8 -1 0 15.96 1.70 -8 -1 0 13.82 1.46 -8 1 0 15.93 1.44 -8 -1 1 22.50 1.96 -8 -1 1 22.47 1.85 -8 1 -1 20.59 1.63 -8 -1 2 220.90 6.99 -8 -1 2 215.08 6.59 -8 -1 3 32.73 2.31 -8 -1 3 32.63 2.16 -8 -1 4 75.23 3.53 -8 -1 4 69.36 3.23 -8 -1 5 13.15 1.33 -8 1 -5 17.08 1.77 -8 1 -6 7.75 1.34 -8 -1 6 3.17 0.78 -8 -1 7 56.34 2.71 -8 1 -7 63.44 3.17 -8 -1 8 70.07 3.01 -8 1 -8 86.72 3.79 -8 -1 9 47.50 2.30 -8 1 -9 54.94 2.81 -8 1 -10 2.02 0.84 -8 -1 10 0.96 0.45 -8 1 -11 6.61 0.94 -8 -1 11 6.67 0.76 -8 1 -12 9.65 1.05 -8 2 11 15.36 1.08 -8 2 10 17.38 1.21 -8 -2 -9 53.12 2.33 -8 2 9 56.71 2.40 -8 -2 -8 133.43 4.37 -8 2 8 138.10 4.29 -8 -2 -7 11.89 1.25 -8 2 7 10.84 1.12 -8 -2 -6 67.62 3.12 -8 2 6 67.66 2.85 -8 -2 -5 10.06 1.19 -8 -2 -5 9.64 0.94 -8 2 5 8.59 1.03 -8 -2 -4 120.77 4.54 -8 -2 -4 119.55 3.89 -8 2 4 125.56 4.22 -8 -2 -3 56.72 2.95 -8 -2 -3 53.75 2.50 -8 2 3 57.28 2.67 -8 -2 -2 111.55 4.35 -8 -2 -2 111.06 3.91 -8 2 2 110.45 3.97 -8 -2 -1 27.40 2.02 -8 -2 -1 27.24 1.78 -8 2 1 28.86 1.91 -8 -2 0 78.53 3.54 -8 -2 0 77.00 3.23 -8 -2 1 26.86 1.99 -8 -2 1 27.94 1.85 -8 -2 2 113.23 4.25 -8 -2 2 110.48 4.01 -8 -2 3 53.87 2.74 -8 -2 3 57.86 2.72 -8 -2 4 120.83 4.23 -8 -2 4 112.77 4.06 -8 -2 5 9.51 1.13 -8 -2 5 8.41 1.04 -8 -2 6 64.26 2.67 -8 -2 6 65.05 2.82 -8 -2 7 11.64 1.15 -8 -2 8 125.37 4.04 -8 -2 9 49.31 2.21 -8 -2 10 15.06 1.10 -8 -3 -4 29.00 1.70 -8 -3 -3 122.52 3.98 -8 -3 -2 2.44 0.57 -8 -3 -1 72.93 2.87 -8 -3 0 10.04 1.00 -8 -3 1 77.71 2.87 0 0 0 0.00 0.00 TITL R040 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 6.744227 7.902923 36.026012 90.0000 90.0000 90.0000 ZERR 4.00 0.000060 0.000071 0.000295 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 96.00 92.00 4.00 16.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 91756 _olex2_date_sample_data_collection 2018-04-26 _olex2_date_sample_submission 2018-04-24 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder with inert oil' _olex2_submission_original_sample_id ML-202F1 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.350 _oxdiff_exptl_absorpt_empirical_full_min 0.706