data_tx2452 _audit_creation_date 2020-07-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _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. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C44 H30 F N5' _chemical_formula_sum 'C44 H30 F N5' _chemical_formula_weight 647.73 _chemical_melting_point ? _chemical_oxdiff_formula CHONFCl 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' 'F' 'F' 0.0727 0.0534 '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' _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 61 _space_group_name_H-M_alt 'P b c a' _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' '-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 12.2187(3) _cell_length_b 21.3171(4) _cell_length_c 26.3276(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6857.5(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8130 _cell_measurement_temperature 170.00(16) _cell_measurement_theta_max 71.9230 _cell_measurement_theta_min 3.9350 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.45753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 2704 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 26732 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.639 _diffrn_reflns_theta_min 3.357 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 170.00(16) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.966 _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 -116.00 -32.00 0.50 1.00 -- -46.70 -55.00 6.00 168 2 \w 40.00 65.00 0.50 2.00 -- 103.25 -55.00 6.00 50 3 \w 90.00 141.00 0.50 2.00 -- 103.25 55.00 149.00 102 4 \w 87.00 162.00 0.50 2.00 -- 103.25 123.00 22.00 150 5 \w 38.00 78.00 0.50 2.00 -- 103.25 -66.00-179.00 80 6 \w -13.00 28.00 0.50 1.00 -- -46.70 19.00 -60.00 82 7 \w 27.00 85.00 0.50 1.00 -- 46.70-125.00-150.00 116 8 \w -58.00 -33.00 0.50 2.00 -- -99.00 61.00 -60.00 50 9 \w -68.00 -43.00 0.50 2.00 -- -99.00 61.00-180.00 50 10 \w -64.00 -39.00 0.50 2.00 -- -99.00 61.00 90.00 50 11 \w -59.00 -33.00 0.50 2.00 -- -99.00 61.00 0.00 52 12 \w 74.00 111.00 0.50 2.00 -- 103.25-125.00 0.00 74 13 \w 34.00 59.00 0.50 2.00 -- 103.25-125.00 0.00 50 14 \w 92.00 117.00 0.50 2.00 -- 103.25 30.00 90.00 50 15 \w 31.00 58.00 0.50 2.00 -- 103.25 -61.00 0.00 54 16 \w 37.00 62.00 0.50 2.00 -- 103.25 -61.00 -30.00 50 17 \w 129.00 169.00 0.50 2.00 -- 103.25 30.00 90.00 80 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0356425000 _diffrn_orient_matrix_UB_12 0.0097445000 _diffrn_orient_matrix_UB_13 0.0555096000 _diffrn_orient_matrix_UB_21 -0.0884413000 _diffrn_orient_matrix_UB_22 0.0466808000 _diffrn_orient_matrix_UB_23 -0.0176167000 _diffrn_orient_matrix_UB_31 -0.0825573000 _diffrn_orient_matrix_UB_32 -0.0543523000 _diffrn_orient_matrix_UB_33 -0.0051357000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5365 _reflns_number_total 6884 _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _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 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _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 0.263 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 479 _refine_ls_number_reflns 6884 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0745 _refine_ls_restrained_S_all 1.059 _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^)+(0.0619P)^2^+6.3773P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1803 _refine_ls_wR_factor_ref 0.1892 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances F46-C2 = F46A-C6 1.36 with sigma of 0.01 C6-C47 = C47A-C2 1.43 with sigma of 0.01 N48-C47 = N48A-C47A 1.15 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints N48 \\sim C47 \\sim F46A \\sim F46 \\sim C47A \\sim N48A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(N48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(F46A) \\sim Ueq, Uanis(F46) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(N48A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Sof(C47A)=Sof(N48A)=Sof(F46A)=1-FVAR(1) Sof(F46)=Sof(C47)=Sof(N48)=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: C35(H35), C26(H26), C39(H39), C13(H13), C25(H25), C38(H38), C36(H36), C12(H12), C19(H19), C22(H22), C15(H15), C37(H37), C32(H32), C41(H41), C11(H11), C18(H18), C24(H24), C17(H17), C23(H23), C16(H16), C45(H45), C9(H9), C28(H28), C10(H10), C44(H44), C42(H42), C43(H43), C31(H31), C30(H30), C29(H29) ; _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 F46 F 0.7051(3) 0.78062(14) 0.62420(15) 0.0507(9) Uani 0.736(6) 1 d D U P A 1 N33 N 0.86834(19) 0.54179(10) 0.66796(9) 0.0518(5) Uani 1 1 d . . . . . N20 N 0.86648(19) 0.76862(10) 0.69720(8) 0.0510(5) Uani 1 1 d . . . . . N7 N 0.62493(18) 0.67770(12) 0.57006(9) 0.0548(6) Uani 1 1 d . . . . . C47 C 0.722(2) 0.5612(6) 0.5829(5) 0.055(2) Uani 0.736(6) 1 d D U P A 1 C34 C 0.8255(2) 0.51270(12) 0.71226(10) 0.0468(6) Uani 1 1 d . . . . . C5 C 0.8298(2) 0.60252(12) 0.65535(10) 0.0486(6) Uani 1 1 d . . . . . C21 C 0.9108(2) 0.81911(12) 0.66813(10) 0.0472(6) Uani 1 1 d . . . . . N50 N 1.0265(2) 0.64317(13) 0.74558(11) 0.0688(7) Uani 1 1 d . . . . . C49 C 0.9541(2) 0.64706(13) 0.71801(10) 0.0495(6) Uani 1 1 d . . . . . C3 C 0.8294(2) 0.71551(13) 0.67107(10) 0.0489(6) Uani 1 1 d . . . . . C4 C 0.8677(2) 0.65483(13) 0.68178(10) 0.0492(6) Uani 1 1 d . . . . . C2 C 0.7496(2) 0.72165(12) 0.63302(11) 0.0513(6) Uani 1 1 d D . . . . C8 C 0.6280(2) 0.72455(13) 0.53248(11) 0.0506(6) Uani 1 1 d . . . . . C6 C 0.7544(2) 0.61172(12) 0.61584(10) 0.0501(6) Uani 1 1 d D . . . . C1 C 0.7110(2) 0.67125(13) 0.60521(10) 0.0501(6) Uani 1 1 d . . . . . C27 C 0.8558(2) 0.77251(13) 0.75042(11) 0.0518(6) Uani 1 1 d . . . . . C35 C 0.8793(2) 0.46169(13) 0.73425(11) 0.0538(7) Uani 1 1 d . . . . . H35 H 0.943834 0.446703 0.720002 0.065 Uiso 1 1 calc R . . . . C26 C 0.8842(2) 0.88096(13) 0.67817(11) 0.0526(6) Uani 1 1 d . . . . . H26 H 0.837093 0.890586 0.704797 0.063 Uiso 1 1 calc R . . . . C39 C 0.7306(2) 0.53537(14) 0.73444(11) 0.0543(7) Uani 1 1 d . . . . . H39 H 0.694549 0.569565 0.720241 0.065 Uiso 1 1 calc R . . . . C14 C 0.5291(2) 0.64001(14) 0.57873(11) 0.0544(7) Uani 1 1 d . . . . . C40 C 0.9252(2) 0.50725(15) 0.62945(10) 0.0556(7) Uani 1 1 d . . . . . C13 C 0.5332(2) 0.75293(14) 0.51453(13) 0.0593(7) Uani 1 1 d . . . . . H13 H 0.465611 0.741214 0.527711 0.071 Uiso 1 1 calc R . . . . C25 C 0.9273(3) 0.92820(14) 0.64881(12) 0.0618(8) Uani 1 1 d . . . . . H25 H 0.909390 0.969726 0.655714 0.074 Uiso 1 1 calc R . . . . C38 C 0.6892(3) 0.50700(15) 0.77790(12) 0.0609(8) Uani 1 1 d . . . . . H38 H 0.625636 0.522431 0.792752 0.073 Uiso 1 1 calc R . . . . C36 C 0.8366(2) 0.43342(15) 0.77720(11) 0.0586(7) Uani 1 1 d . . . . . H36 H 0.872043 0.398958 0.791326 0.070 Uiso 1 1 calc R . . . . C12 C 0.5386(2) 0.79837(14) 0.47726(14) 0.0645(8) Uani 1 1 d . . . . . H12 H 0.474459 0.816734 0.465448 0.077 Uiso 1 1 calc R . . . . C19 C 0.4806(2) 0.60740(15) 0.53920(12) 0.0595(7) Uani 1 1 d . . . . . H19 H 0.508703 0.610389 0.506458 0.071 Uiso 1 1 calc R . . . . C22 C 0.9822(3) 0.80531(14) 0.62876(11) 0.0590(7) Uani 1 1 d . . . . . H22 H 1.001260 0.763906 0.621992 0.071 Uiso 1 1 calc R . . . . C15 C 0.4876(2) 0.63517(16) 0.62731(12) 0.0633(8) Uani 1 1 d . . . . . H15 H 0.519540 0.657580 0.653753 0.076 Uiso 1 1 calc R . . . . C37 C 0.7420(3) 0.45593(15) 0.79927(12) 0.0618(8) Uani 1 1 d . . . . . H37 H 0.713872 0.436941 0.828276 0.074 Uiso 1 1 calc R . . . . C32 C 0.9361(3) 0.80210(15) 0.77920(12) 0.0678(9) Uani 1 1 d . . . . . H32 H 0.998381 0.817833 0.763390 0.081 Uiso 1 1 calc R . . . . C41 C 0.8942(3) 0.44703(15) 0.61577(12) 0.0674(9) Uani 1 1 d . . . . . H41 H 0.836636 0.427639 0.632695 0.081 Uiso 1 1 calc R . . . . C11 C 0.6366(2) 0.81672(15) 0.45754(13) 0.0645(8) Uani 1 1 d . . . . . H11 H 0.639564 0.847425 0.432482 0.077 Uiso 1 1 calc R . . . . C18 C 0.3893(2) 0.57006(15) 0.54891(14) 0.0656(8) Uani 1 1 d . . . . . H18 H 0.355233 0.548811 0.522420 0.079 Uiso 1 1 calc R . . . . C24 C 0.9972(3) 0.91436(16) 0.60913(13) 0.0687(9) Uani 1 1 d . . . . . H24 H 1.025149 0.946396 0.588964 0.082 Uiso 1 1 calc R . . . . C17 C 0.3497(3) 0.56459(16) 0.59734(15) 0.0695(9) Uani 1 1 d . . . . . H17 H 0.289636 0.538980 0.603716 0.083 Uiso 1 1 calc R . . . . C23 C 1.0251(3) 0.85335(16) 0.59959(13) 0.0703(9) Uani 1 1 d . . . . . H23 H 1.073280 0.844099 0.573291 0.084 Uiso 1 1 calc R . . . . C16 C 0.3981(3) 0.59672(17) 0.63659(14) 0.0730(9) Uani 1 1 d . . . . . H16 H 0.370951 0.592705 0.669423 0.088 Uiso 1 1 calc R . . . . C45 C 1.0112(3) 0.5365(2) 0.60438(12) 0.0723(9) Uani 1 1 d . . . . . H45 H 1.033141 0.576811 0.613359 0.087 Uiso 1 1 calc R . . . . C9 C 0.7260(2) 0.74377(18) 0.51214(14) 0.0777(11) Uani 1 1 d . . . . . H9 H 0.790670 0.725666 0.523577 0.093 Uiso 1 1 calc R . . . . C28 C 0.7657(3) 0.74745(19) 0.77474(13) 0.0736(9) Uani 1 1 d . . . . . H28 H 0.711316 0.727434 0.756083 0.088 Uiso 1 1 calc R . . . . C10 C 0.7301(3) 0.78951(19) 0.47502(15) 0.0835(12) Uani 1 1 d . . . . . H10 H 0.797355 0.801813 0.461836 0.100 Uiso 1 1 calc R . . . . C44 C 1.0642(3) 0.5038(3) 0.56508(13) 0.0898(13) Uani 1 1 d . . . . . H44 H 1.121183 0.522840 0.547449 0.108 Uiso 1 1 calc R . . . . C42 C 0.9475(4) 0.4157(2) 0.57763(13) 0.0869(12) Uani 1 1 d . . . . . H42 H 0.925825 0.375279 0.568813 0.104 Uiso 1 1 calc R . . . . N48 N 0.6996(3) 0.52283(17) 0.55469(15) 0.0717(13) Uani 0.736(6) 1 d D U P A 1 C43 C 1.0326(4) 0.4438(2) 0.55245(15) 0.0945(14) Uani 1 1 d . . . . . H43 H 1.069012 0.422297 0.526786 0.113 Uiso 1 1 calc R . . . . C31 C 0.9240(5) 0.80819(19) 0.83060(15) 0.1001(16) Uani 1 1 d . . . . . H31 H 0.976946 0.829297 0.849347 0.120 Uiso 1 1 calc R . . . . C30 C 0.8348(6) 0.7836(3) 0.85462(17) 0.118(2) Uani 1 1 d . . . . . H30 H 0.826746 0.787911 0.889568 0.141 Uiso 1 1 calc R . . . . C29 C 0.7568(4) 0.7522(3) 0.82664(17) 0.1047(15) Uani 1 1 d . . . . . H29 H 0.697367 0.734012 0.843070 0.126 Uiso 1 1 calc R . . . . C47A C 0.688(2) 0.7765(8) 0.6398(9) 0.073(7) Uani 0.264(6) 1 d D U P A 2 N48A N 0.6601(10) 0.8235(5) 0.6262(5) 0.094(4) Uani 0.264(6) 1 d D U P A 2 F46A F 0.722(3) 0.5559(8) 0.5949(8) 0.064(5) Uani 0.264(6) 1 d D U P A 2 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 F46 0.0474(18) 0.0454(15) 0.059(2) 0.0010(11) -0.0130(16) 0.0020(12) N33 0.0548(13) 0.0512(12) 0.0496(13) 0.0010(10) 0.0024(10) 0.0022(10) N20 0.0541(13) 0.0516(12) 0.0472(12) -0.0034(10) -0.0043(10) -0.0103(10) N7 0.0402(11) 0.0706(15) 0.0537(13) 0.0026(11) -0.0099(10) -0.0144(11) C47 0.053(4) 0.051(4) 0.063(4) -0.006(3) -0.008(4) -0.002(3) C34 0.0422(13) 0.0484(14) 0.0498(14) -0.0036(11) -0.0022(11) -0.0059(11) C5 0.0469(14) 0.0481(14) 0.0508(15) 0.0006(11) 0.0004(12) -0.0049(11) C21 0.0444(13) 0.0502(14) 0.0471(14) -0.0024(11) -0.0062(11) -0.0046(11) N50 0.0687(17) 0.0723(17) 0.0655(16) -0.0021(13) -0.0105(14) 0.0022(14) C49 0.0487(15) 0.0553(15) 0.0446(14) 0.0008(12) -0.0078(12) -0.0008(12) C3 0.0468(14) 0.0518(15) 0.0482(14) 0.0001(12) -0.0050(12) -0.0087(12) C4 0.0496(15) 0.0532(15) 0.0447(14) 0.0029(11) -0.0058(12) -0.0047(12) C2 0.0497(14) 0.0472(14) 0.0569(16) 0.0019(12) -0.0090(13) -0.0023(12) C8 0.0395(13) 0.0594(16) 0.0529(15) -0.0033(12) -0.0068(12) -0.0051(11) C6 0.0452(14) 0.0489(14) 0.0560(15) -0.0050(12) -0.0034(12) -0.0085(11) C1 0.0431(13) 0.0559(15) 0.0513(15) 0.0011(12) -0.0060(12) -0.0090(12) C27 0.0522(15) 0.0542(15) 0.0491(15) -0.0021(12) -0.0032(12) 0.0029(12) C35 0.0462(14) 0.0595(16) 0.0556(16) 0.0006(13) -0.0064(12) -0.0023(12) C26 0.0448(14) 0.0534(15) 0.0597(16) -0.0052(13) -0.0043(12) 0.0033(12) C39 0.0473(15) 0.0551(16) 0.0605(17) -0.0023(13) -0.0008(13) -0.0031(12) C14 0.0440(14) 0.0632(17) 0.0561(16) -0.0014(13) -0.0043(12) -0.0134(12) C40 0.0508(15) 0.0707(18) 0.0453(15) -0.0003(13) -0.0021(12) 0.0143(14) C13 0.0360(13) 0.0569(16) 0.085(2) -0.0086(15) -0.0051(14) -0.0019(12) C25 0.0673(18) 0.0514(16) 0.0668(19) 0.0015(14) -0.0077(16) 0.0017(14) C38 0.0526(16) 0.0648(18) 0.0652(19) -0.0041(15) 0.0090(14) -0.0096(14) C36 0.0553(16) 0.0637(18) 0.0568(17) 0.0057(14) -0.0090(14) -0.0071(14) C12 0.0471(16) 0.0543(16) 0.092(2) -0.0014(16) -0.0175(16) 0.0020(13) C19 0.0515(16) 0.0682(18) 0.0587(17) -0.0043(14) -0.0054(13) -0.0131(14) C22 0.0681(18) 0.0549(16) 0.0540(17) -0.0030(13) 0.0037(14) 0.0033(14) C15 0.0554(17) 0.077(2) 0.0576(18) -0.0032(15) -0.0010(14) -0.0142(15) C37 0.0629(18) 0.0659(18) 0.0566(17) 0.0035(14) 0.0011(15) -0.0174(15) C32 0.086(2) 0.0573(17) 0.0596(18) -0.0053(14) -0.0200(17) -0.0011(16) C41 0.085(2) 0.0605(18) 0.0562(18) -0.0039(14) -0.0019(16) 0.0209(17) C11 0.0550(17) 0.0656(18) 0.073(2) 0.0093(15) -0.0093(15) -0.0018(14) C18 0.0512(16) 0.0641(18) 0.082(2) -0.0027(16) -0.0169(16) -0.0135(14) C24 0.082(2) 0.0637(19) 0.0606(19) 0.0092(15) -0.0015(17) -0.0121(17) C17 0.0505(16) 0.0674(19) 0.090(2) 0.0138(18) -0.0036(17) -0.0145(15) C23 0.081(2) 0.072(2) 0.0578(18) 0.0020(15) 0.0122(17) -0.0027(18) C16 0.0575(18) 0.088(2) 0.074(2) 0.0068(18) 0.0073(16) -0.0131(17) C45 0.0555(18) 0.109(3) 0.0520(18) -0.0022(17) -0.0004(15) -0.0008(18) C9 0.0356(14) 0.103(3) 0.094(3) 0.038(2) -0.0040(15) 0.0025(16) C28 0.0629(19) 0.089(2) 0.069(2) 0.0076(18) 0.0115(17) 0.0049(18) C10 0.0435(17) 0.107(3) 0.100(3) 0.042(2) 0.0045(17) 0.0070(17) C44 0.0556(19) 0.163(4) 0.0509(19) 0.007(2) 0.0036(15) 0.021(2) C42 0.116(3) 0.090(3) 0.055(2) -0.0064(18) 0.001(2) 0.037(2) N48 0.073(2) 0.062(2) 0.080(3) -0.014(2) -0.021(2) 0.0033(18) C43 0.105(3) 0.119(4) 0.059(2) -0.014(2) -0.008(2) 0.054(3) C31 0.172(5) 0.069(2) 0.059(2) -0.0108(18) -0.038(3) 0.017(3) C30 0.194(6) 0.106(4) 0.054(2) -0.006(2) 0.010(3) 0.045(4) C29 0.113(3) 0.123(4) 0.077(3) 0.019(3) 0.040(3) 0.030(3) C47A 0.062(9) 0.077(9) 0.079(11) -0.001(7) 0.004(7) -0.008(6) N48A 0.092(8) 0.045(6) 0.146(10) -0.010(6) -0.063(7) 0.015(5) F46A 0.049(6) 0.056(7) 0.086(11) -0.012(6) -0.013(9) -0.002(5) _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 F46 C2 1.389(3) . ? N33 C34 1.421(3) . ? N33 C5 1.417(3) . ? N33 C40 1.433(4) . ? N20 C21 1.427(3) . ? N20 C3 1.400(3) . ? N20 C27 1.410(4) . ? N7 C8 1.406(4) . ? N7 C1 1.407(3) . ? N7 C14 1.439(3) . ? C47 C6 1.437(6) . ? C47 N48 1.139(6) . ? C34 C35 1.396(4) . ? C34 C39 1.386(4) . ? C5 C4 1.393(4) . ? C5 C6 1.404(4) . ? C21 C26 1.384(4) . ? C21 C22 1.386(4) . ? N50 C49 1.148(4) . ? C49 C4 1.432(4) . ? C3 C4 1.404(4) . ? C3 C2 1.404(4) . ? C2 C1 1.383(4) . ? C2 C47A 1.405(9) . ? C8 C13 1.389(4) . ? C8 C9 1.374(4) . ? C6 C1 1.404(4) . ? C6 F46A 1.372(9) . ? C27 C32 1.391(4) . ? C27 C28 1.381(4) . ? C35 C36 1.383(4) . ? C26 C25 1.374(4) . ? C39 C38 1.389(4) . ? C14 C19 1.385(4) . ? C14 C15 1.379(4) . ? C40 C41 1.386(4) . ? C40 C45 1.389(4) . ? C13 C12 1.380(4) . ? C25 C24 1.381(5) . ? C38 C37 1.385(5) . ? C36 C37 1.380(4) . ? C12 C11 1.362(4) . ? C19 C18 1.394(4) . ? C22 C23 1.383(4) . ? C15 C16 1.388(4) . ? C32 C31 1.368(5) . ? C41 C42 1.370(5) . ? C11 C10 1.361(4) . ? C18 C17 1.369(5) . ? C24 C23 1.368(5) . ? C17 C16 1.374(5) . ? C45 C44 1.406(5) . ? C9 C10 1.381(5) . ? C28 C29 1.374(5) . ? C44 C43 1.377(6) . ? C42 C43 1.371(6) . ? C31 C30 1.365(8) . ? C30 C29 1.378(7) . ? C47A N48A 1.115(9) . ? 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 C34 N33 C40 122.4(2) . . ? C5 N33 C34 118.0(2) . . ? C5 N33 C40 117.7(2) . . ? C3 N20 C21 118.0(2) . . ? C3 N20 C27 120.4(2) . . ? C27 N20 C21 121.6(2) . . ? C8 N7 C1 120.8(2) . . ? C8 N7 C14 122.0(2) . . ? C1 N7 C14 116.7(2) . . ? N48 C47 C6 176.4(16) . . ? C35 C34 N33 120.5(2) . . ? C39 C34 N33 120.1(3) . . ? C39 C34 C35 119.4(3) . . ? C4 C5 N33 120.3(2) . . ? C4 C5 C6 118.4(2) . . ? C6 C5 N33 121.3(2) . . ? C26 C21 N20 121.8(2) . . ? C26 C21 C22 119.5(3) . . ? C22 C21 N20 118.7(2) . . ? N50 C49 C4 176.3(3) . . ? N20 C3 C4 122.6(2) . . ? N20 C3 C2 120.0(2) . . ? C2 C3 C4 117.4(2) . . ? C5 C4 C49 119.0(2) . . ? C5 C4 C3 121.7(2) . . ? C3 C4 C49 119.1(2) . . ? F46 C2 C3 118.4(3) . . ? C3 C2 C47A 111.2(13) . . ? C1 C2 F46 118.7(3) . . ? C1 C2 C3 122.8(2) . . ? C1 C2 C47A 121.9(14) . . ? C13 C8 N7 121.8(2) . . ? C9 C8 N7 120.6(3) . . ? C9 C8 C13 117.6(3) . . ? C5 C6 C47 121.4(9) . . ? C5 C6 C1 121.5(2) . . ? C1 C6 C47 117.0(9) . . ? F46A C6 C5 111.6(12) . . ? F46A C6 C1 126.5(13) . . ? C2 C1 N7 121.8(3) . . ? C2 C1 C6 117.9(2) . . ? C6 C1 N7 120.1(2) . . ? C32 C27 N20 120.2(3) . . ? C28 C27 N20 120.8(3) . . ? C28 C27 C32 119.0(3) . . ? C36 C35 C34 120.1(3) . . ? C25 C26 C21 120.0(3) . . ? C34 C39 C38 120.0(3) . . ? C19 C14 N7 120.6(3) . . ? C15 C14 N7 119.2(3) . . ? C15 C14 C19 120.2(3) . . ? C41 C40 N33 121.9(3) . . ? C41 C40 C45 119.9(3) . . ? C45 C40 N33 118.2(3) . . ? C12 C13 C8 120.5(3) . . ? C26 C25 C24 120.4(3) . . ? C37 C38 C39 120.5(3) . . ? C37 C36 C35 120.5(3) . . ? C11 C12 C13 121.0(3) . . ? C14 C19 C18 119.4(3) . . ? C23 C22 C21 119.8(3) . . ? C14 C15 C16 119.8(3) . . ? C36 C37 C38 119.5(3) . . ? C31 C32 C27 120.4(4) . . ? C42 C41 C40 120.9(4) . . ? C10 C11 C12 119.1(3) . . ? C17 C18 C19 120.2(3) . . ? C23 C24 C25 119.7(3) . . ? C18 C17 C16 120.4(3) . . ? C24 C23 C22 120.5(3) . . ? C17 C16 C15 120.1(3) . . ? C40 C45 C44 118.4(4) . . ? C8 C9 C10 121.2(3) . . ? C29 C28 C27 119.7(4) . . ? C11 C10 C9 120.6(3) . . ? C43 C44 C45 120.6(4) . . ? C41 C42 C43 120.0(4) . . ? C42 C43 C44 120.2(4) . . ? C30 C31 C32 120.6(5) . . ? C31 C30 C29 119.4(4) . . ? C28 C29 C30 120.8(5) . . ? N48A C47A C2 150(2) . . ? _shelx_res_file ; TITL tx2452_a.res in Pbca tx2452.res created by SHELXL-2018/3 at 15:13:55 on 06-Jul-2020 REM Old TITL TX2452 in Pbca REM SHELXT solution in Pbca: R1 0.184, Rweak 0.207, Alpha 0.034 REM 1.591 for 697 systematic absences, Orientation as input REM Formula found by SHELXT: C44 C5 F CELL 1.54184 12.2187 21.3171 26.3276 90 90 90 ZERR 8 0.0003 0.0004 0.0008 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 F N UNIT 352 240 8 40 DFIX 1.36 0.01 F46 C2 F46A C6 DFIX 1.43 0.01 C6 C47 C47A C2 DFIX 1.15 0.01 N48 C47 N48A C47A SIMU 0.02 0.04 1.7 N48 C47 F46A F46 C47A N48A ISOR 0.01 0.02 N48 C47 F46A F46 C47A N48A L.S. 4 PLAN 7 BOND LIST 6 fmap 2 acta REM REM REM WGHT 0.061900 6.377300 FVAR 0.27927 0.73581 PART 1 F46 3 0.705085 0.780618 0.624198 21.00000 0.04743 0.04544 = 0.05935 0.00102 -0.01304 0.00200 PART 0 N33 4 0.868343 0.541792 0.667958 11.00000 0.05476 0.05121 = 0.04956 0.00103 0.00238 0.00217 N20 4 0.866481 0.768623 0.697196 11.00000 0.05409 0.05161 = 0.04719 -0.00344 -0.00426 -0.01033 N7 4 0.624934 0.677701 0.570060 11.00000 0.04017 0.07056 = 0.05373 0.00259 -0.00989 -0.01436 PART 1 C47 1 0.722462 0.561185 0.582870 21.00000 0.05268 0.05122 = 0.06254 -0.00587 -0.00755 -0.00181 PART 0 C34 1 0.825506 0.512703 0.712261 11.00000 0.04219 0.04843 = 0.04975 -0.00360 -0.00225 -0.00589 C5 1 0.829845 0.602522 0.655347 11.00000 0.04687 0.04807 = 0.05085 0.00063 0.00043 -0.00492 C21 1 0.910827 0.819110 0.668129 11.00000 0.04443 0.05015 = 0.04711 -0.00237 -0.00619 -0.00458 N50 4 1.026478 0.643174 0.745577 11.00000 0.06871 0.07225 = 0.06551 -0.00213 -0.01053 0.00215 C49 1 0.954055 0.647063 0.718007 11.00000 0.04872 0.05530 = 0.04459 0.00082 -0.00783 -0.00079 C3 1 0.829387 0.715511 0.671069 11.00000 0.04682 0.05177 = 0.04823 0.00015 -0.00497 -0.00874 C4 1 0.867705 0.654825 0.681776 11.00000 0.04956 0.05323 = 0.04469 0.00294 -0.00583 -0.00473 C2 1 0.749643 0.721655 0.633018 11.00000 0.04966 0.04720 = 0.05692 0.00188 -0.00896 -0.00234 C8 1 0.627976 0.724554 0.532484 11.00000 0.03955 0.05943 = 0.05292 -0.00334 -0.00679 -0.00507 C6 1 0.754395 0.611719 0.615843 11.00000 0.04524 0.04893 = 0.05600 -0.00495 -0.00336 -0.00851 C1 1 0.710963 0.671254 0.605210 11.00000 0.04312 0.05590 = 0.05128 0.00112 -0.00602 -0.00905 C27 1 0.855755 0.772506 0.750418 11.00000 0.05215 0.05425 = 0.04913 -0.00214 -0.00323 0.00291 C35 1 0.879281 0.461690 0.734249 11.00000 0.04619 0.05953 = 0.05561 0.00062 -0.00641 -0.00233 AFIX 43 H35 2 0.943834 0.446703 0.720002 11.00000 -1.20000 AFIX 0 C26 1 0.884205 0.880964 0.678169 11.00000 0.04475 0.05336 = 0.05965 -0.00521 -0.00430 0.00331 AFIX 43 H26 2 0.837093 0.890586 0.704797 11.00000 -1.20000 AFIX 0 C39 1 0.730576 0.535371 0.734442 11.00000 0.04726 0.05512 = 0.06046 -0.00229 -0.00082 -0.00314 AFIX 43 H39 2 0.694549 0.569565 0.720241 11.00000 -1.20000 AFIX 0 C14 1 0.529052 0.640011 0.578733 11.00000 0.04397 0.06323 = 0.05612 -0.00143 -0.00427 -0.01343 C40 1 0.925158 0.507250 0.629446 11.00000 0.05081 0.07071 = 0.04531 -0.00028 -0.00210 0.01428 C13 1 0.533204 0.752926 0.514528 11.00000 0.03599 0.05689 = 0.08489 -0.00863 -0.00515 -0.00194 AFIX 43 H13 2 0.465611 0.741214 0.527711 11.00000 -1.20000 AFIX 0 C25 1 0.927346 0.928196 0.648812 11.00000 0.06729 0.05143 = 0.06677 0.00146 -0.00768 0.00170 AFIX 43 H25 2 0.909390 0.969726 0.655714 11.00000 -1.20000 AFIX 0 C38 1 0.689233 0.507003 0.777900 11.00000 0.05260 0.06477 = 0.06521 -0.00405 0.00900 -0.00961 AFIX 43 H38 2 0.625636 0.522431 0.792752 11.00000 -1.20000 AFIX 0 C36 1 0.836647 0.433417 0.777202 11.00000 0.05532 0.06371 = 0.05677 0.00570 -0.00901 -0.00710 AFIX 43 H36 2 0.872043 0.398958 0.791326 11.00000 -1.20000 AFIX 0 C12 1 0.538638 0.798373 0.477263 11.00000 0.04709 0.05430 = 0.09222 -0.00137 -0.01751 0.00197 AFIX 43 H12 2 0.474459 0.816734 0.465448 11.00000 -1.20000 AFIX 0 C19 1 0.480599 0.607404 0.539196 11.00000 0.05155 0.06822 = 0.05873 -0.00431 -0.00538 -0.01314 AFIX 43 H19 2 0.508703 0.610389 0.506458 11.00000 -1.20000 AFIX 0 C22 1 0.982246 0.805314 0.628760 11.00000 0.06808 0.05490 = 0.05405 -0.00299 0.00370 0.00333 AFIX 43 H22 2 1.001260 0.763906 0.621992 11.00000 -1.20000 AFIX 0 C15 1 0.487631 0.635168 0.627311 11.00000 0.05544 0.07699 = 0.05759 -0.00319 -0.00099 -0.01419 AFIX 43 H15 2 0.519540 0.657580 0.653753 11.00000 -1.20000 AFIX 0 C37 1 0.741992 0.455929 0.799274 11.00000 0.06290 0.06589 = 0.05664 0.00352 0.00114 -0.01736 AFIX 43 H37 2 0.713872 0.436941 0.828276 11.00000 -1.20000 AFIX 0 C32 1 0.936092 0.802103 0.779197 11.00000 0.08644 0.05725 = 0.05960 -0.00531 -0.02001 -0.00109 AFIX 43 H32 2 0.998381 0.817833 0.763390 11.00000 -1.20000 AFIX 0 C41 1 0.894246 0.447026 0.615768 11.00000 0.08547 0.06051 = 0.05618 -0.00385 -0.00185 0.02092 AFIX 43 H41 2 0.836636 0.427639 0.632695 11.00000 -1.20000 AFIX 0 C11 1 0.636591 0.816724 0.457541 11.00000 0.05504 0.06561 = 0.07282 0.00927 -0.00927 -0.00180 AFIX 43 H11 2 0.639564 0.847425 0.432482 11.00000 -1.20000 AFIX 0 C18 1 0.389307 0.570061 0.548909 11.00000 0.05119 0.06408 = 0.08156 -0.00275 -0.01690 -0.01352 AFIX 43 H18 2 0.355233 0.548811 0.522420 11.00000 -1.20000 AFIX 0 C24 1 0.997196 0.914358 0.609127 11.00000 0.08180 0.06367 = 0.06056 0.00922 -0.00150 -0.01212 AFIX 43 H24 2 1.025149 0.946396 0.588964 11.00000 -1.20000 AFIX 0 C17 1 0.349699 0.564595 0.597343 11.00000 0.05045 0.06744 = 0.09048 0.01382 -0.00358 -0.01448 AFIX 43 H17 2 0.289636 0.538980 0.603716 11.00000 -1.20000 AFIX 0 C23 1 1.025106 0.853351 0.599593 11.00000 0.08097 0.07223 = 0.05784 0.00197 0.01216 -0.00271 AFIX 43 H23 2 1.073280 0.844099 0.573291 11.00000 -1.20000 AFIX 0 C16 1 0.398143 0.596720 0.636591 11.00000 0.05752 0.08783 = 0.07372 0.00682 0.00732 -0.01306 AFIX 43 H16 2 0.370951 0.592705 0.669423 11.00000 -1.20000 AFIX 0 C45 1 1.011174 0.536541 0.604375 11.00000 0.05553 0.10937 = 0.05197 -0.00224 -0.00043 -0.00077 AFIX 43 H45 2 1.033141 0.576811 0.613359 11.00000 -1.20000 AFIX 0 C9 1 0.725954 0.743774 0.512142 11.00000 0.03556 0.10341 = 0.09403 0.03778 -0.00403 0.00250 AFIX 43 H9 2 0.790670 0.725666 0.523577 11.00000 -1.20000 AFIX 0 C28 1 0.765711 0.747446 0.774737 11.00000 0.06287 0.08878 = 0.06929 0.00758 0.01151 0.00493 AFIX 43 H28 2 0.711316 0.727434 0.756083 11.00000 -1.20000 AFIX 0 C10 1 0.730082 0.789505 0.475015 11.00000 0.04351 0.10671 = 0.10024 0.04182 0.00446 0.00696 AFIX 43 H10 2 0.797355 0.801813 0.461836 11.00000 -1.20000 AFIX 0 C44 1 1.064206 0.503792 0.565076 11.00000 0.05562 0.16281 = 0.05092 0.00721 0.00363 0.02055 AFIX 43 H44 2 1.121183 0.522840 0.547449 11.00000 -1.20000 AFIX 0 C42 1 0.947453 0.415666 0.577628 11.00000 0.11556 0.09016 = 0.05512 -0.00636 0.00119 0.03736 AFIX 43 H42 2 0.925825 0.375279 0.568813 11.00000 -1.20000 AFIX 0 PART 1 N48 4 0.699573 0.522833 0.554688 21.00000 0.07325 0.06217 = 0.07980 -0.01377 -0.02114 0.00329 PART 0 C43 1 1.032571 0.443797 0.552451 11.00000 0.10470 0.11940 = 0.05937 -0.01430 -0.00818 0.05387 AFIX 43 H43 2 1.069012 0.422297 0.526786 11.00000 -1.20000 AFIX 0 C31 1 0.923976 0.808194 0.830599 11.00000 0.17180 0.06922 = 0.05917 -0.01079 -0.03763 0.01658 AFIX 43 H31 2 0.976946 0.829297 0.849347 11.00000 -1.20000 AFIX 0 C30 1 0.834791 0.783561 0.854618 11.00000 0.19418 0.10555 = 0.05398 -0.00602 0.00951 0.04531 AFIX 43 H30 2 0.826746 0.787911 0.889568 11.00000 -1.20000 AFIX 0 C29 1 0.756801 0.752199 0.826635 11.00000 0.11342 0.12321 = 0.07746 0.01897 0.03989 0.02971 AFIX 43 H29 2 0.697367 0.734012 0.843070 11.00000 -1.20000 AFIX 0 PART 2 C47A 1 0.687566 0.776494 0.639754 -21.00000 0.06232 0.07722 = 0.07886 -0.00141 0.00407 -0.00806 N48A 4 0.660125 0.823487 0.626151 -21.00000 0.09185 0.04544 = 0.14569 -0.01002 -0.06340 0.01453 F46A 3 0.721695 0.555854 0.594898 -21.00000 0.04899 0.05573 = 0.08598 -0.01233 -0.01335 -0.00159 HKLF 4 REM tx2452_a.res in Pbca REM wR2 = 0.1892, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0745 for 5365 Fo > 4sig(Fo) and 0.0897 for all 6884 data REM 479 parameters refined using 78 restraints END WGHT 0.0619 6.3774 REM Highest difference peak 0.263, deepest hole -0.319, 1-sigma level 0.047 Q1 1 1.0993 0.5352 0.5612 11.00000 0.05 0.26 Q2 1 1.0161 0.4304 0.5806 11.00000 0.05 0.22 Q3 1 0.8237 0.6059 0.6202 11.00000 0.05 0.19 Q4 1 0.5230 0.8081 0.5123 11.00000 0.05 0.19 Q5 1 0.6392 0.8192 0.6507 11.00000 0.05 0.18 Q6 1 1.0797 0.4743 0.5555 11.00000 0.05 0.17 Q7 1 0.7003 0.8184 0.6026 11.00000 0.05 0.15 ; _shelx_res_checksum 4767 _shelx_hkl_file ; 0 0 -2 1164.31 42.80 0 0 -3 -0.04 0.24 0 0 -4 2171.42 79.82 0 0 -5 4.54 0.62 0 0 -6 350.50 12.96 0 0 -7 4.21 0.75 0 0 -8 818.16 30.16 0 0 -9 3.89 0.78 0 0 -10 415.55 15.42 0 0 -11 0.58 0.96 0 0 -12 307.26 11.51 0 0 -13 0.23 1.23 0 0 -14 206.52 7.95 0 0 -15 0.34 1.33 0 0 16 9.35 0.89 0 0 -16 10.01 1.60 0 0 17 2.71 0.88 0 0 -17 3.28 1.68 0 0 18 262.94 10.08 0 0 -18 284.19 10.48 0 0 19 -0.19 1.07 0 0 -19 -2.39 1.99 0 0 20 388.34 14.63 0 0 -20 398.00 15.06 0 0 21 1.46 1.23 0 0 22 0.29 1.34 0 0 23 0.45 1.45 0 0 24 31.58 2.14 0 0 25 0.58 1.65 0 0 26 28.80 2.15 0 0 27 1.66 1.69 0 0 28 20.53 1.88 0 0 29 0.45 1.51 0 0 30 7.74 1.48 0 0 31 0.44 1.21 0 0 32 1.61 1.01 0 1 -1 0.58 0.08 0 1 -2 -0.06 0.15 0 1 -3 -0.17 0.27 0 1 -4 0.82 0.49 0 1 -5 0.57 0.56 0 1 -6 5.16 0.71 0 1 -7 2.08 0.75 0 1 -8 0.06 0.68 0 1 -9 0.17 0.74 0 1 -10 -0.51 0.84 0 1 -11 0.30 0.95 0 1 -12 0.32 1.08 0 1 -13 0.76 1.21 0 1 -14 0.90 1.26 0 1 -15 0.06 1.34 0 1 16 0.94 0.76 0 1 -16 -1.00 1.47 0 1 17 0.89 0.86 0 1 -17 2.96 1.67 0 1 18 -1.71 1.00 0 1 -18 -0.51 1.84 0 1 19 -0.02 1.07 0 1 -19 -1.14 1.99 0 1 20 -0.39 1.19 0 1 -20 -3.42 2.12 0 1 21 0.15 1.26 0 1 22 0.60 1.33 0 1 23 0.25 1.47 0 1 24 -0.07 1.59 0 1 25 -0.71 1.65 0 1 26 2.85 1.71 0 1 27 1.19 1.69 0 1 28 -0.14 1.66 0 1 29 -0.44 1.53 0 1 30 2.33 1.44 0 1 31 -0.81 1.21 0 1 32 0.10 1.00 0 -2 0 1007.98 37.08 0 -2 -1 424.57 15.85 0 -2 -1 441.75 15.80 0 2 -1 419.34 15.80 0 -2 -2 311.32 10.99 0 2 -2 286.94 10.99 0 -2 -3 2708.77 99.51 0 2 -3 2706.29 99.51 0 2 -4 700.92 25.59 0 -2 -4 689.88 25.59 0 -2 -5 2101.84 79.24 0 2 -5 2207.58 79.24 0 2 -6 7363.44 270.62 0 -2 -6 7364.49 270.63 0 -2 -7 91.76 3.56 0 2 -7 94.82 3.57 0 -2 -8 913.35 34.39 0 2 -8 952.24 34.38 0 -2 -9 533.96 19.54 0 2 -9 523.09 19.53 0 2 -10 42.16 1.90 0 -2 -10 43.26 1.89 0 -2 -11 3.06 0.98 0 2 -11 2.36 0.97 0 2 -12 129.59 5.06 0 -2 -12 130.12 5.08 0 -2 -13 50.10 2.44 0 2 -13 54.40 2.44 0 -2 -14 299.43 11.41 0 2 -14 304.68 11.41 0 2 -15 5.10 1.36 0 -2 -15 3.63 1.37 0 2 16 78.05 3.11 0 -2 16 74.66 3.10 0 -2 -16 80.01 3.56 0 2 17 2.59 0.88 0 -2 17 1.26 0.86 0 2 -17 2.87 1.65 0 -2 -17 2.95 1.66 0 -2 18 415.98 16.01 0 2 18 435.19 16.03 0 2 -18 449.71 16.36 0 -2 -18 438.45 16.36 0 -2 19 21.83 1.43 0 2 19 21.87 1.46 0 -2 -19 20.70 2.25 0 2 -19 24.75 2.29 0 2 20 157.37 5.98 0 -2 20 154.28 5.96 0 2 -20 144.72 6.47 0 -2 -20 150.92 6.52 0 2 21 11.94 1.40 0 2 22 4.51 1.40 0 2 23 18.80 1.74 0 2 24 21.92 1.90 0 2 25 0.53 1.64 0 2 26 22.62 2.03 0 2 27 2.44 1.72 0 2 28 12.90 1.80 0 2 29 10.46 1.67 0 2 30 2.55 1.43 0 2 31 0.13 1.23 0 2 32 3.82 1.02 0 -3 0 2.27 0.62 0 -3 0 2.71 0.59 0 -3 -1 0.32 0.70 0 -3 -1 -0.35 0.55 0 3 -1 -0.09 0.19 0 -3 -1 -0.09 0.23 0 -3 -2 1.11 0.33 0 3 -2 0.81 0.30 0 -3 -3 1.12 0.42 0 3 -3 1.47 0.42 0 -3 -4 1.07 0.46 0 3 -4 0.67 0.46 0 -3 -5 2.26 0.56 0 3 -5 3.53 0.57 0 3 -6 3.63 0.66 0 -3 -6 0.24 0.59 0 3 -7 -0.64 0.61 0 -3 -7 -0.05 0.61 0 -3 -8 0.43 0.69 0 3 -8 1.09 0.65 0 -3 -9 0.81 0.74 0 3 -9 0.05 0.72 0 3 -10 1.00 0.82 0 -3 -10 0.76 0.88 0 3 -11 0.70 0.94 0 -3 -11 -0.48 0.99 0 -3 -12 1.52 1.14 0 3 -12 -1.03 1.06 0 3 -13 0.87 1.15 0 -3 -13 -0.32 1.16 0 3 -14 0.83 1.19 0 -3 -14 -0.71 1.28 0 3 -15 0.09 1.31 0 -3 -15 -0.28 1.33 0 -3 16 1.02 0.70 0 3 16 -0.20 0.77 0 -3 16 1.04 0.76 0 -3 -16 -1.63 1.49 0 3 -16 -0.08 1.47 0 -3 17 0.30 0.79 0 -3 17 0.12 0.86 0 3 17 -0.24 0.87 0 3 -17 0.24 1.57 0 -3 -17 -1.59 1.61 0 -3 18 0.75 0.95 0 3 18 -1.79 1.02 0 3 -18 0.25 1.74 0 -3 19 -0.08 1.03 0 3 19 1.02 1.09 0 -3 -19 -2.46 1.84 0 3 -19 1.81 1.87 0 3 20 -0.72 1.20 0 -3 20 0.09 1.12 0 3 -20 1.06 1.95 0 3 21 -0.53 1.26 0 -3 21 -0.28 1.17 0 3 22 0.67 1.39 0 -3 22 -0.21 1.31 0 3 23 -0.01 1.50 0 -3 23 0.81 1.38 0 -3 24 -0.04 1.49 0 3 24 0.77 1.63 0 3 25 0.34 1.66 0 -3 26 -1.18 1.59 0 3 26 -0.61 1.73 0 3 27 -0.01 1.70 0 -3 27 -1.06 1.52 0 -3 28 -0.47 1.51 0 3 28 -0.19 1.62 0 3 29 0.77 1.55 0 -3 29 0.26 1.39 0 -3 30 0.09 1.25 0 3 30 -0.01 1.39 0 -3 31 1.55 1.06 0 3 31 1.26 1.20 0 -3 32 -0.40 0.84 0 3 32 -0.51 0.96 0 -4 0 4803.18 178.51 0 -4 0 4899.35 178.49 0 -4 1 245.33 9.10 0 -4 -1 244.01 9.12 0 -4 -1 244.08 9.08 0 -4 -2 257.00 9.67 0 -4 -2 247.32 9.61 0 4 -2 268.65 9.54 0 -4 -2 251.60 9.55 0 -4 -3 6.91 1.12 0 -4 -3 8.53 0.49 0 -4 -4 3429.12 124.32 0 4 -4 3339.07 124.32 0 -4 -5 2850.73 105.33 0 4 -5 2879.27 105.33 0 4 -6 587.54 21.75 0 -4 -6 592.55 21.75 0 4 -7 515.58 18.50 0 -4 -7 486.63 18.50 0 -4 -8 230.98 8.47 0 4 -8 223.55 8.46 0 -4 -9 1.45 0.81 0 4 -9 2.69 0.76 0 4 -10 16.37 1.13 0 -4 -10 17.37 1.17 0 4 -11 171.63 6.51 0 -4 -11 170.04 6.53 0 4 -12 331.38 12.22 0 -4 -12 321.07 12.23 0 4 -13 10.66 1.23 0 -4 -13 7.56 1.26 0 4 -14 113.27 4.42 0 -4 -14 104.63 4.43 0 4 -15 13.44 1.48 0 -4 -15 11.79 1.52 0 -4 16 5.59 0.77 0 4 16 4.89 0.85 0 -4 16 5.35 0.83 0 -4 -16 5.59 1.51 0 4 -16 5.15 1.45 0 -4 17 99.03 3.85 0 -4 17 96.15 3.87 0 4 17 99.33 3.89 0 -4 -17 97.47 4.32 0 4 -17 101.87 4.30 0 -4 18 2.81 0.91 0 4 18 2.44 0.98 0 -4 18 1.55 0.95 0 -4 -18 1.56 1.70 0 4 -18 2.84 1.68 0 -4 19 5.60 1.09 0 4 19 8.58 1.13 0 4 -19 7.55 1.83 0 -4 -19 8.92 1.86 0 4 20 31.14 1.75 0 -4 20 27.65 1.68 0 -4 21 0.30 1.17 0 4 21 -0.31 1.25 0 4 22 0.81 1.38 0 -4 22 0.54 1.26 0 -4 23 0.54 1.38 0 4 23 0.67 1.49 0 -4 24 1.77 1.46 0 4 24 1.42 1.60 0 -4 25 137.64 5.75 0 4 25 150.82 5.85 0 -4 26 43.67 2.49 0 4 26 50.58 2.68 0 4 27 1.01 1.68 0 -4 27 0.91 1.45 0 4 28 45.13 2.46 0 -4 28 39.50 2.26 0 4 29 37.00 2.16 0 -4 29 32.39 1.98 0 -4 30 34.92 1.96 0 4 30 42.39 2.15 0 -4 31 -0.62 0.98 0 4 31 0.36 1.15 0 -4 32 0.51 0.75 0 4 32 0.41 0.87 0 -5 0 1.99 0.87 0 -5 0 2.87 0.81 0 -5 1 0.20 0.87 0 -5 -1 0.55 0.77 0 -5 -1 0.52 0.96 0 -5 -2 1.30 1.05 0 -5 -2 0.97 0.81 0 5 -2 0.13 0.39 0 -5 -3 1.62 1.10 0 -5 -3 1.86 0.47 0 5 -3 1.96 0.43 0 -5 -4 0.39 1.19 0 -5 -4 0.61 0.50 0 5 -4 0.36 0.45 0 -5 -5 3.02 1.18 0 -5 -5 3.33 0.58 0 5 -5 2.08 0.52 0 5 -6 1.62 0.53 0 -5 -6 2.96 0.65 0 -5 -7 1.31 0.72 0 5 -7 1.34 0.61 0 5 -8 0.96 0.69 0 -5 -8 1.43 0.76 0 5 -9 -0.20 0.79 0 -5 -9 -0.13 0.88 0 -5 -10 0.29 0.97 0 5 -10 0.57 0.89 0 5 -11 1.00 0.97 0 -5 -11 0.39 1.01 0 5 -12 0.51 1.01 0 -5 -12 0.45 1.08 0 5 -13 0.79 1.09 0 -5 -13 1.31 1.17 0 -5 -14 0.27 1.26 0 5 -14 -0.01 1.22 0 -5 15 -0.35 0.67 0 -5 -15 -0.30 1.32 0 5 -15 -0.28 1.25 0 -5 16 0.71 0.73 0 -5 16 0.73 0.79 0 5 16 -0.37 0.79 0 -5 -16 0.56 1.43 0 5 -16 1.71 1.41 0 -5 17 -0.18 0.80 0 -5 17 0.69 0.86 0 5 17 0.50 0.89 0 -5 -17 -1.34 1.55 0 5 -17 0.89 1.53 0 -5 18 -0.15 0.93 0 -5 18 0.30 0.93 0 5 18 0.15 0.96 0 -5 -18 0.75 1.64 0 5 -18 0.91 1.59 0 5 19 1.08 1.08 0 -5 19 0.20 1.02 0 -5 20 0.13 1.11 0 5 20 -0.18 1.15 0 -5 21 -0.31 1.18 0 5 21 0.31 1.26 0 -5 22 -1.10 1.30 0 5 22 1.17 1.38 0 5 23 0.10 1.50 0 -5 23 0.96 1.38 0 -5 24 0.49 1.41 0 5 24 1.14 1.59 0 -5 25 -0.38 1.45 0 5 25 -0.67 1.67 0 5 26 -0.29 1.65 0 -5 26 -2.37 1.48 0 5 27 0.74 1.61 0 -5 27 -0.11 1.41 0 -5 28 0.08 1.30 0 5 28 2.13 1.54 0 5 29 -0.02 1.43 0 -5 29 0.68 1.21 0 5 30 0.29 1.25 0 -5 30 -0.53 1.06 0 5 31 1.01 1.05 0 -5 31 -0.17 0.88 0 -6 0 1013.90 37.60 0 -6 0 1024.51 37.58 0 -6 -1 2332.42 87.47 0 -6 -1 2359.51 87.44 0 -6 1 2435.27 87.45 0 -6 -2 354.00 13.55 0 -6 -2 372.08 13.51 0 -6 -3 1278.38 47.00 0 6 -3 1273.61 46.88 0 -6 -4 24.43 1.54 0 6 -4 26.65 1.08 0 -6 -4 22.69 1.09 0 -6 -5 1164.12 43.83 0 6 -5 1197.25 43.69 0 -6 -5 1184.52 43.70 0 -6 -6 934.42 35.95 0 -6 -6 973.15 35.80 0 6 -6 983.55 35.79 0 -6 -7 1380.27 51.99 0 6 -7 1411.64 51.83 0 -6 -7 1415.78 51.84 0 6 -8 569.39 21.03 0 -6 -8 569.13 21.05 0 6 -9 530.06 19.37 0 -6 -9 515.85 19.39 0 -6 -10 6.53 1.04 0 6 -10 4.09 0.90 0 6 -11 7.27 1.01 0 -6 -11 5.59 1.12 0 -6 -12 5.34 1.15 0 6 -12 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1.00 5 -5 29 1.99 0.87 -5 -5 29 0.96 1.03 5 -6 0 1.30 1.32 -5 -6 0 0.20 1.34 5 -6 1 76.05 3.18 5 -6 -1 75.70 3.15 5 -6 2 115.79 4.59 5 -6 -2 111.89 4.54 -5 -6 -2 109.27 4.59 5 -6 -3 3.08 1.32 5 -6 3 3.99 1.44 -5 -6 -3 4.07 1.40 5 6 -4 267.65 9.54 5 -6 -4 254.25 9.49 5 -6 4 250.83 9.61 5 -6 -4 235.65 9.57 -5 -6 -4 247.49 9.65 -5 -6 -5 4.27 1.43 5 6 -5 4.48 1.07 5 -6 -5 3.14 0.94 -5 -6 -6 36.84 2.20 5 6 -6 38.87 1.85 5 -6 -6 36.71 1.77 -5 -6 -7 183.85 7.31 5 6 -7 188.41 7.07 5 -6 -7 176.39 7.02 -5 -6 7 188.28 6.92 5 -6 -8 109.30 4.24 5 6 -8 109.63 4.28 -5 -6 -8 99.79 4.58 -5 -6 -9 10.26 1.81 5 6 -9 11.63 1.15 5 -6 -9 11.16 1.11 -5 -6 -10 28.62 2.23 5 6 -10 26.29 1.52 5 -6 -10 22.43 1.44 5 6 -11 74.12 3.09 5 -6 -11 68.69 3.04 5 -6 -12 3.11 1.00 5 6 -12 1.78 1.09 -5 -6 -12 2.85 1.93 -5 -6 12 0.69 0.61 5 6 -13 2.59 1.13 5 -6 -13 2.55 1.07 -5 -6 -13 1.66 1.98 -5 -6 13 1.96 0.63 5 6 -14 18.06 1.50 5 -6 -14 20.55 1.48 5 -6 14 22.29 1.09 -5 -6 -14 18.65 2.36 5 -6 15 43.83 1.85 -5 -6 15 37.99 2.16 5 6 -15 40.75 2.25 5 -6 -15 40.45 2.17 5 -6 16 64.40 2.61 -5 -6 16 61.27 2.91 5 6 -16 60.96 3.04 5 -6 -16 62.78 3.02 5 -6 17 0.99 0.85 -5 -6 -17 3.77 2.21 -5 -6 17 -0.78 1.40 5 6 -17 -0.26 1.52 5 -6 -17 0.24 1.37 5 6 -18 60.37 3.28 5 -6 -18 58.52 3.17 5 -6 19 2.03 0.93 -5 -6 -19 1.55 2.32 5 6 -19 0.23 1.59 5 -6 -19 1.13 1.53 5 -6 20 15.41 1.17 -5 -6 -20 14.63 2.52 5 6 -20 10.32 1.86 5 -6 -20 12.62 1.78 -5 -6 -21 210.03 8.21 5 -6 -21 163.62 7.61 5 6 -21 156.28 7.67 5 -6 21 205.13 7.18 5 -6 22 17.63 1.31 5 -6 23 -0.10 1.05 5 6 23 1.16 1.21 5 -6 23 0.29 1.01 5 6 24 3.14 1.24 5 -6 24 4.28 1.12 5 6 25 20.47 1.49 5 -6 25 15.39 1.30 5 -6 26 7.82 1.13 5 6 26 11.93 1.31 5 6 27 12.17 1.28 5 -6 27 12.58 1.12 -5 -6 28 0.66 1.20 -5 -6 -28 0.09 1.71 5 6 28 -0.23 1.05 -5 -6 29 2.06 0.75 -5 -6 -29 0.45 1.43 5 6 29 2.19 0.91 -5 -6 29 2.08 0.98 5 -7 0 1.15 1.33 -5 -7 0 0.08 1.31 5 -7 1 701.30 25.52 5 -7 -1 681.72 25.50 -5 -7 -1 675.72 25.55 5 -7 2 11.78 1.52 5 -7 -2 11.91 1.46 -5 -7 -2 15.17 1.53 5 7 -3 1.85 1.04 5 -7 -3 3.03 0.89 5 -7 3 1.88 1.43 5 -7 -3 1.70 1.28 -5 -7 -3 2.57 1.40 5 7 -4 1.70 1.02 5 -7 -4 2.50 0.88 5 -7 -4 2.30 1.29 5 -7 4 2.63 1.43 -5 -7 -4 2.44 1.42 5 7 -5 97.19 3.96 -5 -7 -5 89.09 4.22 -5 -7 6 80.00 3.23 5 7 -6 87.17 3.41 5 -7 -6 91.75 3.37 -5 -7 -6 77.94 3.71 -5 -7 7 284.21 10.03 -5 -7 -7 250.42 10.37 5 7 -7 268.25 10.13 5 -7 -7 255.84 10.10 -5 -7 8 89.89 3.09 5 7 -8 83.55 3.24 5 -7 -8 76.40 3.19 5 -7 8 68.28 3.04 -5 -7 -8 80.40 3.66 5 7 -9 282.18 9.60 5 -7 -9 269.69 9.55 5 -7 9 232.17 9.45 -5 -7 -9 246.31 9.59 -5 -7 -9 262.62 9.92 5 7 -10 161.12 5.55 5 -7 -10 144.30 5.50 -5 -7 -10 153.00 6.02 5 7 -11 30.38 1.61 -5 -7 -11 31.39 2.40 -5 -7 11 26.59 1.33 5 7 -12 2.42 1.06 5 -7 -12 3.39 1.04 -5 -7 -12 3.86 1.97 -5 -7 12 1.92 0.70 5 -7 -13 52.24 2.55 -5 -7 13 52.92 2.36 5 7 -14 0.13 1.20 5 -7 -14 -0.23 1.11 5 -7 14 0.55 0.76 -5 -7 -14 0.26 2.06 -5 -7 14 -0.34 0.70 5 7 -15 40.50 2.21 5 -7 -15 41.93 2.19 5 -7 15 42.77 1.83 -5 -7 15 38.37 1.83 5 7 -16 31.77 2.07 5 -7 -16 28.30 1.94 5 -7 16 34.26 1.55 -5 -7 16 28.32 1.51 5 7 -17 1.30 1.47 5 -7 -17 1.57 1.37 5 -7 17 2.77 0.89 -5 -7 -17 3.95 2.24 -5 -7 17 -0.18 0.75 5 7 -18 30.67 2.30 5 -7 -18 29.30 2.20 -5 -7 -19 35.23 2.91 5 -7 19 33.81 1.58 5 -7 -19 22.98 2.05 5 7 -19 27.12 2.22 5 -7 20 1.22 0.94 -5 -7 -20 3.90 2.21 5 7 -20 1.19 1.65 5 -7 -20 3.11 1.60 -5 -7 -21 9.82 2.30 5 -7 21 11.47 1.12 5 7 22 4.22 1.20 5 -7 22 3.77 1.07 5 -7 22 4.14 1.02 5 7 23 0.70 1.20 5 -7 23 0.50 1.02 5 -7 23 -0.18 0.99 5 7 24 1.46 1.19 5 -7 24 1.74 1.01 5 7 25 1.03 1.18 5 -7 25 -0.02 0.97 5 7 26 0.34 1.12 5 -7 26 0.27 0.93 -5 -7 -27 1.40 1.84 5 7 27 7.95 1.13 -5 -7 28 2.15 0.85 -5 -7 28 1.66 1.16 -5 -7 -28 0.35 1.59 5 7 28 1.67 0.96 -5 -7 -29 1.59 1.30 -5 -7 29 0.87 0.91 -5 -7 29 0.76 0.66 5 -8 0 0.46 1.32 -5 -8 0 -0.04 1.33 5 -8 1 242.58 8.68 5 -8 -1 227.77 8.65 5 -8 -2 62.91 2.74 5 -8 2 69.61 3.04 5 -8 -2 65.00 2.99 5 -8 -3 93.44 3.95 5 8 -3 111.35 4.05 5 -8 3 104.15 4.24 5 -8 -3 94.95 4.18 -5 -8 -3 105.49 4.27 5 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2.07 1.48 5 -8 19 2.42 0.97 5 8 -20 28.32 2.33 5 -8 -20 29.10 2.22 5 8 21 0.86 1.13 5 -8 21 0.80 0.97 5 -8 21 1.36 0.98 5 8 22 2.81 1.17 5 -8 22 2.16 0.98 5 -8 22 2.25 1.01 5 8 23 4.77 1.17 5 -8 23 2.25 0.97 5 -8 23 2.40 0.99 5 8 24 -0.34 1.13 5 -8 24 1.02 0.94 5 8 25 1.32 1.08 5 8 26 0.26 1.06 5 8 27 4.00 0.97 -5 -8 27 6.03 1.30 -5 -8 27 2.70 0.92 -5 -8 28 1.35 1.08 -5 -8 28 -0.20 0.76 -5 -8 29 0.93 0.82 -5 -8 29 1.10 0.56 5 -9 0 0.94 1.33 5 -9 1 137.20 5.43 5 -9 -1 134.14 5.42 5 -9 -1 135.36 5.19 5 -9 2 332.42 12.84 5 -9 -2 328.68 12.82 5 9 -2 320.55 12.69 5 -9 -2 365.39 12.66 5 -9 3 547.46 21.67 5 -9 -3 551.26 21.67 5 9 -3 579.15 21.54 5 -9 -3 613.90 21.51 -5 -9 -4 2.45 1.11 -5 -9 4 2.27 0.59 5 -9 4 2.67 1.54 5 9 -4 3.05 0.89 5 -9 -4 2.45 0.70 5 -9 4 4.01 0.62 5 -9 5 24.46 1.81 5 9 -5 23.65 1.30 5 -9 -5 22.50 1.20 -5 -9 -5 22.99 1.51 5 -9 6 13.57 1.60 5 9 -6 11.90 1.02 5 -9 -6 10.54 0.92 5 -9 7 14.32 1.62 -5 -9 -7 13.17 1.29 5 9 -7 14.49 1.08 5 -9 -7 12.90 0.95 -5 -9 8 79.56 3.34 -5 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3.26 1.21 -5 -9 28 0.16 0.66 -5 -9 28 -0.08 0.98 -5 -9 29 0.94 0.70 5 -9 29 0.35 0.42 5 -10 0 4.19 1.35 5 10 0 3.86 0.82 5 -10 0 3.37 0.68 5 -10 1 13.74 1.50 5 -10 -1 12.38 1.47 5 10 -1 10.51 0.94 5 -10 -1 10.81 0.81 -5 -10 1 9.52 0.92 5 -10 2 34.26 1.48 -5 -10 2 30.65 1.58 5 -10 2 34.34 2.03 5 -10 -2 34.87 2.02 5 10 -2 36.39 1.57 5 -10 -2 34.99 1.46 5 -10 3 194.73 7.32 -5 -10 -3 220.10 7.48 -5 -10 3 186.54 7.37 -5 -10 -3 165.18 7.35 5 -10 3 195.68 7.59 5 -10 -3 187.52 7.57 5 10 -3 212.45 7.35 5 -10 -3 198.92 7.30 -5 -10 3 192.91 7.34 5 -10 4 87.10 3.66 -5 -10 -4 102.31 3.89 5 -10 4 91.01 4.03 5 10 -4 102.27 3.71 5 -10 -4 92.84 3.64 -5 -10 4 93.88 3.73 5 -10 5 1.59 0.58 5 -10 5 3.34 1.55 5 -10 -5 1.92 0.62 5 10 -5 2.66 0.77 -5 -10 5 2.64 0.91 -5 -10 -5 2.57 1.19 -5 -10 -6 199.75 7.43 5 10 -6 212.96 7.32 5 -10 -6 194.90 7.26 5 -10 6 190.98 7.58 -5 -10 -7 33.75 1.88 5 10 -7 31.30 1.58 5 -10 -7 35.47 1.54 5 -10 7 35.36 2.19 -5 -10 -8 2.48 1.22 5 -10 8 3.30 1.51 5 10 -8 1.84 0.80 5 -10 -8 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102.45 4.08 -8 -8 9 92.32 3.94 -8 -8 9 78.64 3.72 8 -8 9 103.09 3.73 8 8 -9 98.82 4.02 8 -8 -9 82.19 3.82 -8 -8 -9 97.12 4.04 -8 -8 -9 98.85 4.25 8 -8 9 97.57 4.13 -8 -8 10 14.53 1.84 -8 -8 10 9.69 1.12 -8 -8 10 11.31 1.59 8 8 -10 13.18 1.47 8 -8 -10 10.87 1.21 -8 -8 -10 16.61 1.85 -8 -8 -10 14.26 1.86 8 -8 10 14.84 1.77 -8 -8 11 65.68 2.99 -8 -8 11 46.05 2.49 -8 -8 -11 72.71 3.04 8 -8 11 72.36 3.15 -8 -8 -11 67.13 3.23 8 8 -11 59.23 2.84 8 -8 -11 56.76 2.66 8 8 -12 3.60 1.38 8 -8 -12 9.85 1.17 -8 -8 12 7.20 1.79 -8 -8 12 2.86 0.95 -8 -8 -12 9.82 1.86 -8 -8 -12 11.21 1.86 8 -8 12 8.77 1.68 -8 -8 -13 190.96 6.07 8 -8 13 139.12 6.07 -8 -8 -13 177.23 6.36 8 8 -13 145.64 5.99 8 -8 -13 119.87 5.80 8 8 -14 38.49 2.49 8 -8 -14 39.19 2.30 -8 -8 -14 52.72 2.73 8 -8 14 57.51 2.15 -8 -8 -14 51.30 2.89 8 -8 14 42.10 2.59 -8 -8 -15 27.48 2.21 -8 -8 -15 25.65 2.24 8 -8 15 22.25 1.97 8 -8 15 30.48 1.49 8 -8 16 2.33 0.91 -8 -8 -16 2.49 1.82 8 -8 17 0.52 0.87 -8 -8 -17 0.65 1.79 -8 -8 18 3.79 1.71 8 -8 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4.13 0.72 -13 7 3 5.22 0.87 13 -7 -4 2.29 0.69 -13 7 4 2.32 0.80 13 -7 -5 17.20 1.06 -13 7 5 20.28 1.10 13 -7 -6 1.12 0.69 -13 7 6 2.46 0.72 13 -7 -7 3.28 0.70 -13 7 7 3.78 0.67 13 -7 -8 0.41 0.63 -13 7 8 0.58 0.59 13 -7 -9 1.30 0.61 13 -7 9 0.64 0.47 13 -7 9 0.50 0.54 -13 7 9 1.37 0.61 13 -7 -10 5.21 0.66 13 -7 10 4.23 0.46 13 -7 -11 3.74 0.61 13 -7 -12 0.77 0.54 13 -7 -13 0.43 0.49 13 -7 -14 0.90 0.44 13 -8 0 -0.19 0.60 13 -8 1 10.27 0.77 13 -8 -1 10.24 0.78 -13 8 2 3.58 0.87 13 -8 2 4.67 0.67 13 -8 -2 3.25 0.69 -13 8 3 62.07 2.56 13 -8 3 63.88 2.49 13 -8 -3 62.25 2.54 -13 8 4 4.74 0.78 13 -8 -4 2.85 0.72 -13 8 5 3.72 0.71 13 -8 -5 4.77 0.70 -13 8 6 0.60 0.62 13 -8 -6 1.06 0.65 -13 8 7 2.05 0.58 13 -8 -7 3.17 0.66 -13 8 8 5.51 0.60 13 -8 -8 6.32 0.70 13 -8 8 6.31 0.64 13 -8 -9 1.24 0.59 13 -8 9 0.57 0.49 13 -8 9 0.52 0.47 13 -8 10 1.35 0.42 13 -8 -10 1.26 0.57 13 -8 11 1.30 0.35 13 -8 -11 0.91 0.54 13 -8 -12 0.64 0.49 13 -9 0 1.27 0.60 13 -9 1 13.60 0.81 13 -9 -1 9.93 0.79 13 -9 2 14.79 0.86 13 -9 -2 14.64 0.89 -13 9 2 12.80 0.97 13 -9 -3 10.28 0.77 -13 9 3 8.19 0.84 13 -9 -4 22.64 1.07 -13 9 4 17.53 1.05 13 -9 -5 0.09 0.61 -13 9 5 0.33 0.58 13 -9 6 1.32 0.65 13 -9 -6 1.78 0.67 13 -9 -6 2.20 0.61 -13 9 6 1.67 0.53 13 -9 -7 0.54 0.59 13 -9 7 0.90 0.59 13 -9 -7 0.29 0.63 13 -9 -8 0.24 0.56 13 -9 8 0.31 0.52 13 -9 8 0.35 0.50 13 -9 -9 1.26 0.55 13 -9 9 0.56 0.42 13 -9 9 0.78 0.46 13 -9 10 0.65 0.41 13 -9 -10 1.27 0.52 13 -10 0 1.32 0.58 13 -10 1 6.32 0.65 13 -10 -1 4.57 0.63 13 -10 1 5.23 0.83 13 -10 2 30.82 1.49 13 -10 -2 36.76 1.39 -13 10 3 33.01 1.55 13 -10 3 33.44 1.63 -13 10 4 21.08 1.09 13 -10 4 23.57 1.22 13 -10 -4 24.32 1.26 13 -10 5 2.39 0.64 13 -10 -5 3.22 0.68 13 -10 -5 3.17 0.60 -13 10 5 2.83 0.51 13 -10 -6 1.00 0.54 13 -10 6 1.55 0.59 13 -10 -6 1.63 0.61 13 -10 -7 0.36 0.52 13 -10 7 0.30 0.50 13 -10 -7 -0.67 0.54 13 -10 -8 1.32 0.52 13 -10 8 1.09 0.44 13 -10 8 1.52 0.49 13 -10 9 1.24 0.43 13 -10 10 0.72 0.38 13 -10 -12 0.04 0.34 13 -11 0 0.80 0.68 13 -11 0 0.77 0.52 -13 11 0 0.31 0.58 13 -11 1 2.30 0.70 13 -11 -1 3.02 0.55 -13 11 1 1.23 0.59 13 -11 2 1.19 0.68 13 -11 -2 1.51 0.53 -13 11 2 0.67 0.53 13 -11 -3 4.57 0.56 13 -11 3 2.20 0.65 13 -11 -4 2.13 0.53 13 -11 4 1.33 0.59 13 -11 -4 1.69 0.65 13 -11 -5 2.11 0.51 13 -11 5 1.53 0.55 13 -11 -5 1.45 0.59 13 -11 6 2.30 0.53 13 -11 -6 3.17 0.56 13 -11 7 0.63 0.44 13 -11 7 0.56 0.47 13 -11 8 3.58 0.47 13 -11 9 3.11 0.42 13 -11 -10 0.31 0.36 13 -12 0 -0.25 0.61 -13 12 -1 1.08 0.51 13 -12 1 2.86 0.61 13 -12 2 1.71 0.59 13 -12 -2 1.40 0.47 13 -12 3 4.07 0.58 13 -12 -3 3.06 0.62 13 -12 -3 3.63 0.50 13 -12 4 0.32 0.53 13 -12 -4 -0.23 0.57 13 -12 5 1.59 0.50 13 -12 -5 1.07 0.52 13 -12 6 2.84 0.48 13 -12 -6 3.45 0.49 13 -12 6 3.42 0.44 13 -12 7 0.47 0.41 13 -12 -8 1.09 0.36 13 -12 8 0.66 0.37 13 -12 -9 -0.24 0.30 13 -13 0 0.25 0.51 13 -13 1 1.54 0.52 13 -13 2 1.09 0.49 13 -13 -3 3.19 0.55 13 -13 3 3.63 0.50 13 -13 4 0.45 0.45 13 -13 -4 0.55 0.47 13 -13 -5 0.64 0.41 13 -13 5 0.05 0.40 13 -13 -6 1.88 0.34 13 -13 6 2.35 0.38 13 -14 0 -0.16 0.41 13 -14 1 0.39 0.42 13 -14 2 -0.07 0.38 13 -14 3 1.65 0.36 -14 0 0 4.32 0.71 -14 0 -1 0.81 0.68 -14 0 -2 4.06 0.71 -14 0 -3 2.06 0.68 -14 0 -4 13.79 0.90 -14 0 5 1.13 0.64 -14 0 -5 -0.30 0.64 -14 0 6 9.42 0.78 -14 0 7 -0.10 0.65 -14 0 9 0.22 0.60 14 0 -9 0.00 0.28 -14 0 10 0.27 0.56 -14 0 11 0.49 0.51 -14 0 12 0.30 0.47 -14 0 13 1.55 0.42 -14 -1 0 8.51 0.77 -14 -1 1 1.27 0.65 -14 1 -1 0.79 0.71 -14 -1 -1 2.50 0.66 -14 -1 2 2.38 0.66 -14 1 -2 2.69 0.72 -14 -1 -2 1.94 0.66 -14 1 -3 8.15 0.80 -14 -1 -3 7.09 0.75 -14 1 3 8.99 0.79 -14 1 -4 27.68 1.33 -14 -1 -4 27.39 1.29 -14 1 4 29.32 1.31 -14 1 5 -0.02 0.61 -14 1 -5 0.36 0.67 14 -1 -5 -0.08 0.33 -14 1 6 0.42 0.62 -14 1 -6 0.97 0.64 14 -1 -6 -0.08 0.32 -14 1 7 2.50 0.68 14 -1 -7 0.92 0.34 14 -1 -8 0.08 0.32 -14 1 9 0.18 0.59 14 -1 -9 0.18 0.32 -14 1 10 15.13 0.68 14 -1 -10 3.97 0.44 -14 1 11 2.19 0.51 14 -1 -11 0.70 0.30 -14 1 12 5.25 0.52 -14 -2 0 1.23 0.63 -14 -2 -1 3.00 0.64 -14 -2 1 2.73 0.65 -14 -2 2 16.19 0.83 -14 2 2 17.31 0.88 -14 -2 -2 15.07 0.81 -14 -2 3 0.55 0.65 -14 2 -3 0.86 0.72 -14 2 3 0.09 0.66 14 -2 -3 -0.08 0.33 -14 -2 4 14.16 0.79 -14 2 -4 13.65 0.85 -14 2 4 13.81 0.80 -14 2 5 0.25 0.62 -14 2 -5 -0.30 0.67 14 -2 -5 -0.73 0.36 -14 2 -6 2.87 0.67 -14 2 6 2.51 0.62 14 -2 -6 1.46 0.38 -14 2 -7 0.66 0.60 -14 2 7 0.81 0.62 14 -2 -7 0.16 0.36 -14 2 8 1.43 0.60 14 -2 -8 0.19 0.35 14 -2 -9 2.53 0.40 14 -2 -10 0.15 0.34 14 -2 -11 0.51 0.32 -14 -3 0 1.51 0.60 -14 3 0 2.16 0.71 14 -3 0 1.27 0.34 -14 -3 -1 0.23 0.57 -14 -3 1 0.38 0.61 -14 3 1 0.16 0.68 14 -3 -1 0.13 0.33 -14 -3 2 10.75 0.75 -14 3 2 11.41 0.80 -14 -3 3 4.55 0.68 -14 3 3 4.68 0.69 14 -3 -3 2.45 0.40 -14 3 4 2.25 0.65 -14 3 -4 1.66 0.68 -14 -3 4 2.09 0.67 14 -3 -4 1.39 0.38 -14 3 5 2.02 0.62 -14 -3 5 2.30 0.64 14 -3 -5 0.98 0.40 -14 3 6 4.13 0.62 14 -3 -6 1.50 0.42 -14 3 7 0.89 0.60 14 -3 -7 0.19 0.37 -14 3 8 1.90 0.60 14 -3 -8 0.28 0.37 14 -3 -9 -0.11 0.37 14 -3 -10 0.69 0.35 14 -3 -11 0.21 0.33 -14 4 0 10.30 0.80 14 -4 0 6.51 0.48 -14 -4 1 9.72 0.70 -14 4 -1 6.88 0.78 -14 4 1 8.77 0.76 14 -4 1 4.30 0.42 14 -4 -1 5.20 0.45 -14 4 2 0.76 0.66 -14 -4 2 0.78 0.66 14 -4 -2 -0.34 0.39 -14 4 3 1.73 0.65 -14 -4 3 1.86 0.63 14 -4 -3 1.11 0.40 -14 4 4 5.64 0.67 14 -4 -4 3.20 0.44 -14 4 5 0.41 0.60 14 -4 -5 0.49 0.40 -14 4 6 3.02 0.59 14 -4 -6 2.56 0.43 -14 4 7 2.05 0.58 14 -4 -7 0.96 0.41 -14 4 8 0.64 0.55 14 -4 -8 0.60 0.38 14 -4 -9 0.34 0.38 14 -4 -10 0.90 0.36 14 -4 -11 -0.14 0.32 -14 5 0 0.79 0.69 14 -5 0 0.49 0.37 -14 5 -1 3.52 0.71 -14 5 1 2.56 0.69 14 -5 1 3.12 0.39 14 -5 -1 2.06 0.41 -14 5 -2 9.46 0.78 -14 5 2 9.11 0.74 -14 5 3 0.74 0.61 14 -5 -3 -0.40 0.41 -14 5 4 1.52 0.61 14 -5 -4 0.34 0.40 -14 5 5 18.62 0.86 14 -5 -5 11.67 0.73 -14 5 6 2.96 0.57 14 -5 -6 0.48 0.42 -14 5 7 0.79 0.53 14 -5 -7 0.61 0.40 14 -5 -8 0.51 0.40 14 -5 -9 3.11 0.43 14 -5 -10 0.03 0.35 14 -5 -11 0.25 0.31 -14 6 0 4.77 0.68 14 -6 0 2.93 0.43 -14 6 -1 0.46 0.65 -14 6 1 0.35 0.65 14 -6 -1 -0.05 0.39 -14 6 -2 5.86 0.73 -14 6 2 6.81 0.70 14 -6 -2 6.51 0.51 -14 6 3 6.18 0.65 14 -6 -3 3.83 0.48 -14 6 4 7.56 0.64 14 -6 -4 5.08 0.51 -14 6 5 3.05 0.57 14 -6 -5 1.42 0.43 -14 6 6 6.74 0.59 14 -6 -6 5.14 0.50 -14 6 7 3.54 0.55 14 -6 -7 3.08 0.44 14 -6 -8 0.04 0.37 14 -6 -9 1.16 0.37 14 -6 -10 1.41 0.35 -14 7 0 2.16 0.63 14 -7 0 1.77 0.40 -14 7 -1 0.72 0.62 -14 7 1 0.20 0.59 14 -7 -1 0.11 0.40 -14 7 -2 1.14 0.61 -14 7 2 1.28 0.57 14 -7 -2 0.83 0.40 -14 7 3 8.63 0.66 14 -7 -3 7.39 0.54 -14 7 4 2.49 0.53 14 -7 -4 2.82 0.43 -14 7 5 2.01 0.47 14 -7 -5 1.80 0.41 14 -7 6 0.94 0.50 14 -7 -6 1.29 0.38 14 -7 7 1.19 0.40 14 -7 -7 0.95 0.38 14 -7 -8 1.64 0.37 14 -7 -9 0.41 0.32 14 -7 -10 0.32 0.29 -14 8 0 13.20 0.82 -14 8 -1 23.45 1.16 -14 8 1 23.12 1.11 14 -8 -1 25.51 1.06 -14 8 -2 0.31 0.62 -14 8 2 1.18 0.51 14 -8 -2 0.13 0.41 -14 8 3 7.91 0.60 14 -8 3 8.58 0.70 14 -8 4 2.03 0.56 14 -8 -4 2.24 0.62 14 -8 -4 1.77 0.41 14 -8 -5 6.60 0.61 14 -8 5 5.99 0.58 14 -8 -5 6.18 0.48 14 -8 -6 0.48 0.36 14 -8 6 0.44 0.39 14 -8 -6 0.90 0.48 14 -8 -7 0.93 0.34 14 -8 -8 0.01 0.30 14 -8 -9 0.74 0.29 14 -9 0 24.85 1.15 -14 9 0 21.39 1.03 14 -9 1 17.98 0.86 -14 9 -1 11.84 0.82 -14 9 -2 -0.67 0.55 14 -9 2 0.89 0.53 14 -9 -2 0.10 0.38 -14 9 -3 0.82 0.49 14 -9 -3 0.71 0.36 14 -9 3 0.45 0.49 14 -9 -3 1.11 0.53 14 -9 -4 4.72 0.42 14 -9 4 5.35 0.51 14 -9 -4 5.52 0.55 14 -9 5 0.44 0.42 14 -9 -5 0.59 0.45 14 -9 -5 1.07 0.34 14 -9 -6 0.41 0.32 14 -9 -7 3.95 0.37 14 -10 0 1.41 0.51 14 -10 1 9.97 0.64 14 -10 2 0.77 0.45 14 -10 3 0.20 0.43 14 -10 -3 1.17 0.45 14 -10 -4 2.88 0.43 14 -10 -4 2.39 0.33 14 -10 -5 0.60 0.28 14 -11 0 5.71 0.49 -15 0 0 0.32 0.43 -15 0 -1 0.03 0.40 -15 0 1 0.27 0.44 -15 0 -2 4.28 0.45 -15 1 0 -0.25 0.43 -15 -1 0 0.57 0.45 -15 1 -1 1.78 0.42 -15 -1 1 2.00 0.46 -15 1 -2 1.98 0.42 -15 -1 2 1.23 0.46 -15 1 4 0.62 0.42 -15 2 -2 0.29 0.41 -15 2 2 0.58 0.42 -15 2 -3 1.57 0.41 -15 2 3 1.92 0.44 -15 2 4 0.15 0.42 -15 3 1 2.31 0.42 -15 3 2 4.51 0.47 0 0 0 0.00 0.00 TITL TX2452 in Pbca REM Pbca (#61 in standard setting) CELL 1.54184 12.218731 21.317109 26.327565 90.0000 90.0000 90.0000 ZERR 77.00 0.000269 0.000428 0.000750 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 F Cl UNIT 77.00 77.00 77.00 77.00 77.00 77.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 79773 _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 1.900 _oxdiff_exptl_absorpt_empirical_full_min 0.503