#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 3 _journal_year 2022 _journal_page_first 253 _journal_page_last 258 #============================================================================= data_shelx _audit_creation_date 2022-03-09 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _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 ? _chemical_name_common ? _chemical_name_systematic N'-acetyl-N'-phenyl-2-naphthohydrazide _chemical_formula_moiety 'C19 H16 N2 O2' _chemical_formula_sum 'C19 H16 N2 O2' _chemical_formula_weight 304.34 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9164(7) _cell_length_b 9.7058(9) _cell_length_c 17.7384(12) _cell_angle_alpha 88.308(7) _cell_angle_beta 89.744(6) _cell_angle_gamma 86.744(7) _cell_volume 1531.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3226 _cell_measurement_temperature 150.01(10) _cell_measurement_theta_max 27.9770 _cell_measurement_theta_min 2.2700 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Crys Alis Red' _exptl_absorpt_special_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour White _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description BLOCK _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 8450 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 2.103 _diffrn_ambient_temperature 150.01(10) _diffrn_detector_area_resol_mean 15.9974 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4639 _reflns_number_total 5935 _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 1.171.38.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.607 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 547 _refine_ls_number_reflns 5935 _refine_ls_number_restraints 936 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0580 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.2827P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1421 _refine_ls_wR_factor_ref 0.1579 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Restrained distances N12-H12 = N35-H35 = N35'-H35' 0.9 with sigma of 0.02 C34-O40 \\sim C34'-O40' with sigma of 0.02 N35-C34 \\sim N35'-C34' with sigma of 0.02 2. Uiso/Uaniso restraints and constraints C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim O40 \\sim N35 \\sim C24' \\sim C25' \\sim C26' \\sim C27' \\sim C28' \\sim C29' \\sim C30' \\sim C31' \\sim C32' \\sim C33' \\sim C34': within 3A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3A O40 \\sim O40': within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A N35 \\sim N35' \\sim H35 \\sim H35': within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A 3. Others Sof(C24')=Sof(C25')=Sof(H25')=Sof(C26')=Sof(C27')=Sof(H27')=Sof(C28')= Sof(H28')=Sof(C29')=Sof(H29')=Sof(C30')=Sof(H30')=Sof(C31')=Sof(C32')= Sof(H32')=Sof(C33')=Sof(H33')=Sof(C34')=Sof(O40')=Sof(N35')=Sof(H35')=1-FVAR(1) Sof(C24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(H28)= Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(C33)= Sof(H33)=Sof(C34)=Sof(O40)=Sof(N35)=Sof(H35)=FVAR(1) 4.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C25'(H25'), C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'), C32'(H32'), C33'(H33'), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 4.b Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C39(H39A,H39B,H39C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H12 H 0.331(3) 0.723(2) 0.3386(14) 0.050(8) Uiso 1 1 d D . . . . C1 C 0.2573(3) 0.8095(3) 0.46955(12) 0.0345(5) Uani 1 1 d . . . . . C2 C 0.1686(3) 0.8404(3) 0.53011(13) 0.0359(5) Uani 1 1 d . . . . . H2 H 0.116337 0.771106 0.553893 0.043 Uiso 1 1 calc R U . . . C3 C 0.1542(3) 0.9775(3) 0.55788(13) 0.0360(5) Uani 1 1 d . . . . . C4 C 0.0614(3) 1.0092(3) 0.62012(15) 0.0445(6) Uani 1 1 d . . . . . H4 H 0.010230 0.939896 0.644599 0.053 Uiso 1 1 calc R U . . . C5 C 0.0462(3) 1.1402(3) 0.64451(17) 0.0525(7) Uani 1 1 d . . . . . H5 H -0.013556 1.160314 0.686321 0.063 Uiso 1 1 calc R U . . . C6 C 0.1209(3) 1.2460(3) 0.60656(18) 0.0568(8) Uani 1 1 d . . . . . H6 H 0.107730 1.336066 0.622973 0.068 Uiso 1 1 calc R U . . . C7 C 0.2105(3) 1.2195(3) 0.54723(17) 0.0516(7) Uani 1 1 d . . . . . H7 H 0.259307 1.290942 0.523334 0.062 Uiso 1 1 calc R U . . . C8 C 0.2319(3) 1.0812(3) 0.52020(15) 0.0428(6) Uani 1 1 d . . . . . C9 C 0.3244(3) 1.0475(3) 0.45921(15) 0.0484(7) Uani 1 1 d . . . . . H9 H 0.377744 1.115705 0.435077 0.058 Uiso 1 1 calc R U . . . C10 C 0.3376(3) 0.9151(3) 0.43436(15) 0.0434(6) Uani 1 1 d . . . . . H10 H 0.400313 0.894405 0.393735 0.052 Uiso 1 1 calc R U . . . C11 C 0.2572(2) 0.6661(2) 0.44120(12) 0.0313(5) Uani 1 1 d . . . . . C14 C 0.4091(3) 0.4253(3) 0.34212(13) 0.0361(5) Uani 1 1 d . . . . . C16 C 0.5465(3) 0.4587(3) 0.38365(17) 0.0556(8) Uani 1 1 d . . . . . H16A H 0.614555 0.378471 0.386890 0.083 Uiso 1 1 calc R U . . . H16B H 0.519253 0.486913 0.433521 0.083 Uiso 1 1 calc R U . . . H16C H 0.594246 0.532180 0.357316 0.083 Uiso 1 1 calc R U . . . C18 C 0.1572(2) 0.5049(2) 0.29943(12) 0.0295(5) Uani 1 1 d . . . . . C19 C 0.1146(3) 0.5864(3) 0.23773(13) 0.0373(6) Uani 1 1 d . . . . . H19 H 0.177561 0.651967 0.218358 0.045 Uiso 1 1 calc R U . . . C20 C -0.0234(3) 0.5696(3) 0.20476(14) 0.0444(6) Uani 1 1 d . . . . . H20 H -0.053624 0.624600 0.163130 0.053 Uiso 1 1 calc R U . . . C21 C -0.1157(3) 0.4725(3) 0.23311(14) 0.0411(6) Uani 1 1 d . . . . . H21 H -0.207963 0.461210 0.210513 0.049 Uiso 1 1 calc R U . . . C22 C -0.0720(3) 0.3915(3) 0.29497(14) 0.0396(6) Uani 1 1 d . . . . . H22 H -0.134585 0.325274 0.313986 0.048 Uiso 1 1 calc R U . . . C23 C 0.0644(3) 0.4084(2) 0.32891(13) 0.0350(5) Uani 1 1 d . . . . . H23 H 0.093313 0.354941 0.371325 0.042 Uiso 1 1 calc R U . . . N12 N 0.3108(2) 0.6511(2) 0.36961(10) 0.0318(4) Uani 1 1 d D . . . . N13 N 0.2980(2) 0.52599(19) 0.33487(10) 0.0309(4) Uani 1 1 d . . . . . O15 O 0.3952(2) 0.31290(19) 0.31427(10) 0.0467(5) Uani 1 1 d . . . . . O17 O 0.21466(19) 0.56903(18) 0.47815(9) 0.0400(4) Uani 1 1 d . . . . . C24 C 0.5647(4) 0.3274(5) 0.1079(2) 0.0269(9) Uani 0.753(3) 1 d . U P A 1 C25 C 0.4909(4) 0.4415(4) 0.14300(19) 0.0301(7) Uani 0.753(3) 1 d . U P A 1 H25 H 0.416537 0.427060 0.178859 0.036 Uiso 0.753(3) 1 calc R U P A 1 C26 C 0.5281(4) 0.5717(4) 0.12454(18) 0.0323(7) Uani 0.753(3) 1 d . U P A 1 H26 H 0.480860 0.645741 0.149059 0.039 Uiso 0.753(3) 1 calc R U P A 1 C27 C 0.6380(4) 0.5972(4) 0.06847(18) 0.0297(7) Uani 0.753(3) 1 d . U P A 1 C28 C 0.6737(5) 0.7328(4) 0.0459(3) 0.0352(9) Uani 0.753(3) 1 d . U P A 1 H28 H 0.627109 0.808789 0.068937 0.042 Uiso 0.753(3) 1 calc R U P A 1 C29 C 0.7769(5) 0.7510(4) -0.0100(3) 0.0393(10) Uani 0.753(3) 1 d . U P A 1 H29 H 0.799311 0.840076 -0.025016 0.047 Uiso 0.753(3) 1 calc R U P A 1 C30 C 0.8499(4) 0.6383(4) -0.0453(2) 0.0438(9) Uani 0.753(3) 1 d . U P A 1 H30 H 0.920363 0.653153 -0.083029 0.053 Uiso 0.753(3) 1 calc R U P A 1 C31 C 0.8181(4) 0.5081(4) -0.02437(19) 0.0388(8) Uani 0.753(3) 1 d . U P A 1 H31 H 0.866844 0.433632 -0.047831 0.047 Uiso 0.753(3) 1 calc R U P A 1 C32 C 0.7102(11) 0.4841(8) 0.0334(5) 0.0282(13) Uani 0.753(3) 1 d . U P A 1 C33 C 0.6723(3) 0.3490(3) 0.05429(16) 0.0286(7) Uani 0.753(3) 1 d . U P A 1 H33 H 0.720932 0.273900 0.031398 0.034 Uiso 0.753(3) 1 calc R U P A 1 C34 C 0.5248(10) 0.1813(6) 0.1236(5) 0.0266(12) Uani 0.753(3) 1 d D U P A 1 O40 O 0.5668(6) 0.0872(4) 0.0835(3) 0.0333(9) Uani 0.753(3) 1 d D U P A 1 N35 N 0.4354(10) 0.1652(11) 0.1853(6) 0.0257(15) Uani 0.753(3) 1 d D U P A 1 C24' C 0.5931(14) 0.2780(13) 0.0916(7) 0.023(2) Uani 0.247(3) 1 d . U P A 2 C25' C 0.5453(13) 0.4015(14) 0.1156(7) 0.0222(19) Uani 0.247(3) 1 d . U P A 2 H25' H 0.472629 0.408145 0.153294 0.027 Uiso 0.247(3) 1 calc R U P A 2 C26' C 0.6064(11) 0.5272(11) 0.0832(6) 0.0263(18) Uani 0.247(3) 1 d . U P A 2 C27' C 0.5607(11) 0.6564(11) 0.1070(6) 0.0321(19) Uani 0.247(3) 1 d . U P A 2 H27' H 0.491213 0.665135 0.146040 0.038 Uiso 0.247(3) 1 calc R U P A 2 C28' C 0.6152(13) 0.7712(12) 0.0744(7) 0.033(2) Uani 0.247(3) 1 d . U P A 2 H28' H 0.581845 0.858482 0.089837 0.040 Uiso 0.247(3) 1 calc R U P A 2 C29' C 0.7230(16) 0.7561(14) 0.0168(8) 0.028(2) Uani 0.247(3) 1 d . U P A 2 H29' H 0.759221 0.835217 -0.005900 0.034 Uiso 0.247(3) 1 calc R U P A 2 C30' C 0.7761(11) 0.6322(10) -0.0070(6) 0.0329(19) Uani 0.247(3) 1 d . U P A 2 H30' H 0.849513 0.627897 -0.044413 0.039 Uiso 0.247(3) 1 calc R U P A 2 C31' C 0.722(4) 0.508(3) 0.0242(16) 0.029(3) Uani 0.247(3) 1 d . U P A 2 C32' C 0.7641(10) 0.3782(9) 0.0017(5) 0.0298(19) Uani 0.247(3) 1 d . U P A 2 H32' H 0.835006 0.368074 -0.036659 0.036 Uiso 0.247(3) 1 calc R U P A 2 C33' C 0.7064(10) 0.2629(10) 0.0334(5) 0.0298(18) Uani 0.247(3) 1 d . U P A 2 H33' H 0.739500 0.175627 0.017807 0.036 Uiso 0.247(3) 1 calc R U P A 2 C34' C 0.538(3) 0.1462(19) 0.1166(16) 0.028(3) Uani 0.247(3) 1 d D U P A 2 O40' O 0.553(2) 0.0366(11) 0.0858(10) 0.036(3) Uani 0.247(3) 1 d D U P A 2 N35' N 0.464(3) 0.144(4) 0.1841(19) 0.025(4) Uani 0.247(3) 1 d D U P A 2 C37 C 0.4587(3) -0.0671(3) 0.23926(12) 0.0337(5) Uani 1 1 d . . . . . C39 C 0.6114(3) -0.0376(3) 0.26620(16) 0.0532(8) Uani 1 1 d . . . . . H39A H 0.648772 -0.111687 0.299230 0.080 Uiso 1 1 calc R U . . . H39B H 0.605874 0.047116 0.292965 0.080 Uiso 1 1 calc R U . . . H39C H 0.677753 -0.029130 0.223771 0.080 Uiso 1 1 calc R U . . . C41 C 0.2319(2) 0.0195(2) 0.17267(12) 0.0307(5) Uani 1 1 d . . . . . C42 C 0.1174(3) 0.1104(3) 0.19457(15) 0.0422(6) Uani 1 1 d . . . . . H42 H 0.135607 0.178618 0.228592 0.051 Uiso 1 1 calc R U . . . C43 C -0.0247(3) 0.0999(3) 0.16569(16) 0.0490(7) Uani 1 1 d . . . . . H43 H -0.102446 0.161611 0.180004 0.059 Uiso 1 1 calc R U . . . C44 C -0.0519(3) -0.0015(3) 0.11585(15) 0.0444(6) Uani 1 1 d . . . . . H44 H -0.148031 -0.008952 0.096855 0.053 Uiso 1 1 calc R U . . . C45 C 0.0634(3) -0.0918(3) 0.09418(15) 0.0407(6) Uani 1 1 d . . . . . H45 H 0.045033 -0.160258 0.060336 0.049 Uiso 1 1 calc R U . . . C46 C 0.2065(3) -0.0817(2) 0.12231(14) 0.0365(5) Uani 1 1 d . . . . . H46 H 0.284661 -0.142567 0.107417 0.044 Uiso 1 1 calc R U . . . N36 N 0.3801(2) 0.03445(19) 0.20136(10) 0.0321(4) Uani 1 1 d . . . . . O38 O 0.40348(19) -0.17861(17) 0.25159(9) 0.0410(4) Uani 1 1 d . . . . . H35 H 0.421(4) 0.230(3) 0.2203(18) 0.028(7) Uiso 0.753(3) 1 d D U P A 1 H35' H 0.458(14) 0.202(11) 0.222(5) 0.025(8) Uiso 0.247(3) 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 C1 0.0321(12) 0.0430(14) 0.0287(11) -0.0071(10) -0.0090(9) -0.0017(10) C2 0.0349(12) 0.0414(14) 0.0314(12) -0.0019(10) -0.0108(10) -0.0011(10) C3 0.0294(12) 0.0488(15) 0.0292(12) -0.0051(10) -0.0124(9) 0.0053(10) C4 0.0379(14) 0.0511(16) 0.0441(14) -0.0070(12) -0.0075(11) 0.0035(12) C5 0.0439(16) 0.0563(18) 0.0570(17) -0.0160(14) -0.0115(13) 0.0083(13) C6 0.0498(17) 0.0474(17) 0.073(2) -0.0199(15) -0.0222(15) 0.0118(14) C7 0.0514(17) 0.0442(16) 0.0601(18) -0.0025(13) -0.0237(14) -0.0084(13) C8 0.0409(14) 0.0441(15) 0.0438(14) 0.0022(12) -0.0167(11) -0.0069(11) C9 0.0538(16) 0.0493(17) 0.0441(15) -0.0033(12) -0.0064(12) -0.0171(13) C10 0.0501(15) 0.0417(15) 0.0403(14) -0.0095(11) -0.0039(11) -0.0147(12) C11 0.0266(11) 0.0391(13) 0.0289(11) -0.0030(10) -0.0052(9) -0.0058(10) C14 0.0320(12) 0.0435(15) 0.0326(12) -0.0081(11) -0.0018(9) 0.0018(10) C16 0.0343(14) 0.073(2) 0.0596(18) -0.0235(15) -0.0107(12) 0.0078(13) C18 0.0291(11) 0.0319(12) 0.0278(11) -0.0054(9) -0.0040(9) -0.0028(9) C19 0.0381(13) 0.0425(14) 0.0318(12) 0.0011(10) -0.0023(10) -0.0066(11) C20 0.0440(15) 0.0548(17) 0.0341(13) 0.0054(12) -0.0108(11) -0.0032(12) C21 0.0330(13) 0.0506(16) 0.0404(14) -0.0067(12) -0.0115(10) -0.0051(11) C22 0.0343(13) 0.0387(14) 0.0469(14) -0.0031(11) -0.0037(11) -0.0090(10) C23 0.0347(12) 0.0353(13) 0.0351(12) 0.0015(10) -0.0047(10) -0.0048(10) N12 0.0387(11) 0.0288(10) 0.0288(10) -0.0046(8) -0.0016(8) -0.0091(8) N13 0.0310(10) 0.0312(10) 0.0311(10) -0.0051(8) -0.0060(8) -0.0054(8) O15 0.0487(11) 0.0430(11) 0.0485(11) -0.0173(9) -0.0046(8) 0.0055(8) O17 0.0460(10) 0.0424(10) 0.0322(9) 0.0016(8) -0.0001(7) -0.0113(8) C24 0.026(2) 0.029(3) 0.026(2) -0.0030(19) -0.0047(14) -0.005(2) C25 0.0281(16) 0.0342(19) 0.0279(16) -0.0011(14) -0.0012(13) -0.0018(14) C26 0.0326(16) 0.0312(18) 0.0330(16) -0.0022(14) -0.0052(13) 0.0007(14) C27 0.0297(16) 0.0306(18) 0.0294(16) 0.0005(14) -0.0122(13) -0.0089(14) C28 0.036(2) 0.034(2) 0.037(2) 0.0016(18) -0.0122(18) -0.0062(17) C29 0.038(2) 0.037(2) 0.044(2) 0.0128(18) -0.0168(17) -0.0179(18) C30 0.0375(19) 0.050(2) 0.044(2) 0.0121(16) -0.0018(16) -0.0142(16) C31 0.0357(17) 0.0420(19) 0.0393(17) 0.0037(14) 0.0039(14) -0.0101(14) C32 0.024(2) 0.035(3) 0.026(2) 0.0005(19) -0.0037(17) -0.009(2) C33 0.0282(15) 0.0310(17) 0.0273(15) -0.0024(13) -0.0037(12) -0.0053(13) C34 0.024(2) 0.032(3) 0.024(2) -0.002(2) -0.0072(17) -0.004(2) O40 0.0377(17) 0.028(3) 0.0349(16) -0.007(2) -0.0017(12) -0.008(2) N35 0.025(3) 0.024(4) 0.030(2) -0.003(2) 0.0006(19) -0.008(3) C24' 0.022(4) 0.026(5) 0.020(4) 0.000(4) -0.012(3) -0.002(4) C25' 0.017(4) 0.026(4) 0.024(4) -0.004(4) -0.004(3) 0.001(4) C26' 0.024(4) 0.026(4) 0.029(4) 0.002(3) -0.012(3) -0.003(3) C27' 0.029(4) 0.035(4) 0.032(4) 0.001(4) -0.004(3) -0.005(4) C28' 0.036(5) 0.029(4) 0.036(5) 0.002(4) -0.010(4) -0.009(4) C29' 0.029(5) 0.031(4) 0.026(5) 0.001(4) 0.003(4) -0.010(4) C30' 0.033(4) 0.036(4) 0.031(4) -0.001(3) -0.004(4) -0.010(3) C31' 0.027(4) 0.030(5) 0.029(5) 0.002(4) -0.013(4) -0.010(4) C32' 0.032(4) 0.030(4) 0.028(4) 0.000(3) 0.008(3) -0.003(3) C33' 0.034(4) 0.028(4) 0.026(4) 0.000(3) 0.002(3) 0.004(3) C34' 0.025(6) 0.029(7) 0.030(6) -0.001(6) -0.007(5) -0.004(6) O40' 0.045(6) 0.017(6) 0.047(5) -0.012(6) 0.002(4) -0.011(5) N35' 0.027(9) 0.013(7) 0.034(6) -0.005(5) 0.002(6) 0.006(5) C37 0.0362(13) 0.0396(14) 0.0260(11) 0.0024(10) -0.0046(9) -0.0099(10) C39 0.0439(15) 0.068(2) 0.0480(16) 0.0180(14) -0.0181(12) -0.0183(14) C41 0.0297(11) 0.0325(12) 0.0307(11) 0.0019(9) -0.0025(9) -0.0107(9) C42 0.0372(13) 0.0469(15) 0.0441(14) -0.0121(12) 0.0057(11) -0.0102(11) C43 0.0309(13) 0.0585(18) 0.0579(17) -0.0110(14) 0.0048(12) -0.0021(12) C44 0.0301(13) 0.0527(17) 0.0516(16) 0.0022(13) -0.0058(11) -0.0131(11) C45 0.0411(14) 0.0339(13) 0.0483(15) -0.0018(11) -0.0133(11) -0.0116(11) C46 0.0357(13) 0.0294(12) 0.0447(14) -0.0022(10) -0.0088(10) -0.0037(10) N36 0.0320(10) 0.0307(10) 0.0346(10) 0.0006(8) -0.0046(8) -0.0123(8) O38 0.0477(10) 0.0381(10) 0.0378(9) 0.0079(7) -0.0077(8) -0.0133(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 C1 C2 1.362(3) . ? C1 C10 1.412(4) . ? C1 C11 1.493(3) . ? C2 H2 0.9300 . ? C2 C3 1.431(3) . ? C3 C4 1.408(3) . ? C3 C8 1.406(4) . ? C4 H4 0.9300 . ? C4 C5 1.355(4) . ? C5 H5 0.9300 . ? C5 C6 1.409(4) . ? C6 H6 0.9300 . ? C6 C7 1.341(4) . ? C7 H7 0.9300 . ? C7 C8 1.441(4) . ? C8 C9 1.392(4) . ? C9 H9 0.9300 . ? C9 C10 1.370(4) . ? C10 H10 0.9300 . ? C11 N12 1.364(3) . ? C11 O17 1.210(3) . ? C14 C16 1.488(3) . ? C14 N13 1.356(3) . ? C14 O15 1.223(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C18 C19 1.373(3) . ? C18 C23 1.375(3) . ? C18 N13 1.434(3) . ? C19 H19 0.9300 . ? C19 C20 1.385(3) . ? C20 H20 0.9300 . ? C20 C21 1.369(4) . ? C21 H21 0.9300 . ? C21 C22 1.375(4) . ? C22 H22 0.9300 . ? C22 C23 1.380(3) . ? C23 H23 0.9300 . ? N12 H12 0.900(17) . ? N12 N13 1.388(2) . ? C24 C25 1.415(5) . ? C24 C33 1.367(5) . ? C24 C34 1.499(8) . ? C25 H25 0.9300 . ? C25 C26 1.356(5) . ? C26 H26 0.9300 . ? C26 C27 1.419(5) . ? C27 C28 1.418(6) . ? C27 C32 1.401(10) . ? C28 H28 0.9300 . ? C28 C29 1.363(6) . ? C29 H29 0.9300 . ? C29 C30 1.403(6) . ? C30 H30 0.9300 . ? C30 C31 1.352(5) . ? C31 H31 0.9300 . ? C31 C32 1.425(8) . ? C32 C33 1.412(7) . ? C33 H33 0.9300 . ? C34 O40 1.216(6) . ? C34 N35 1.363(6) . ? N35 N36 1.408(12) . ? N35 H35 0.897(18) . ? C24' C25' 1.331(15) . ? C24' C33' 1.446(15) . ? C24' C34' 1.45(3) . ? C25' H25' 0.9300 . ? C25' C26' 1.465(17) . ? C26' C27' 1.374(15) . ? C26' C31' 1.47(3) . ? C27' H27' 0.9300 . ? C27' C28' 1.354(15) . ? C28' H28' 0.9300 . ? C28' C29' 1.405(16) . ? C29' H29' 0.9300 . ? C29' C30' 1.346(17) . ? C30' H30' 0.9300 . ? C30' C31' 1.42(3) . ? C31' C32' 1.36(3) . ? C32' H32' 0.9300 . ? C32' C33' 1.364(13) . ? C33' H33' 0.9300 . ? C34' O40' 1.210(16) . ? C34' N35' 1.367(16) . ? N35' N36 1.36(4) . ? N35' H35' 0.89(2) . ? C37 C39 1.490(3) . ? C37 N36 1.342(3) . ? C37 O38 1.228(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C41 C42 1.373(3) . ? C41 C46 1.376(3) . ? C41 N36 1.435(3) . ? C42 H42 0.9300 . ? C42 C43 1.379(3) . ? C43 H43 0.9300 . ? C43 C44 1.374(4) . ? C44 H44 0.9300 . ? C44 C45 1.374(4) . ? C45 H45 0.9300 . ? C45 C46 1.382(3) . ? C46 H46 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C10 118.9(2) . . ? C2 C1 C11 117.6(2) . . ? C10 C1 C11 123.4(2) . . ? C1 C2 H2 119.4 . . ? C1 C2 C3 121.3(2) . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 121.1(2) . . ? C8 C3 C2 118.4(2) . . ? C8 C3 C4 120.5(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 120.0(3) . . ? C6 C5 H5 120.0 . . ? C5 C6 H6 119.4 . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6 119.4 . . ? C6 C7 H7 119.7 . . ? C6 C7 C8 120.5(3) . . ? C8 C7 H7 119.7 . . ? C3 C8 C7 117.4(3) . . ? C9 C8 C3 119.6(2) . . ? C9 C8 C7 123.0(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.7(3) . . ? C10 C9 H9 119.6 . . ? C1 C10 H10 119.5 . . ? C9 C10 C1 121.0(2) . . ? C9 C10 H10 119.5 . . ? N12 C11 C1 114.9(2) . . ? O17 C11 C1 123.6(2) . . ? O17 C11 N12 121.5(2) . . ? N13 C14 C16 117.3(2) . . ? O15 C14 C16 122.5(2) . . ? O15 C14 N13 120.2(2) . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C18 C23 120.9(2) . . ? C19 C18 N13 118.8(2) . . ? C23 C18 N13 120.2(2) . . ? C18 C19 H19 120.4 . . ? C18 C19 C20 119.1(2) . . ? C20 C19 H19 120.4 . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 120.0 . . ? C20 C21 C22 120.0(2) . . ? C22 C21 H21 120.0 . . ? C21 C22 H22 119.9 . . ? C21 C22 C23 120.2(2) . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 119.4(2) . . ? C18 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C11 N12 H12 123.4(18) . . ? C11 N12 N13 119.10(19) . . ? N13 N12 H12 115.4(18) . . ? C14 N13 C18 122.75(19) . . ? C14 N13 N12 120.06(18) . . ? N12 N13 C18 116.81(18) . . ? C25 C24 C34 122.8(4) . . ? C33 C24 C25 119.8(4) . . ? C33 C24 C34 117.3(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C25 C26 H26 119.4 . . ? C25 C26 C27 121.2(4) . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 122.1(4) . . ? C32 C27 C26 118.5(4) . . ? C32 C27 C28 119.4(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 C27 119.4(4) . . ? C29 C28 H28 120.3 . . ? C28 C29 H29 119.2 . . ? C28 C29 C30 121.5(4) . . ? C30 C29 H29 119.2 . . ? C29 C30 H30 120.0 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30 120.0 . . ? C30 C31 H31 119.8 . . ? C30 C31 C32 120.4(5) . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 119.2(5) . . ? C27 C32 C33 119.6(6) . . ? C33 C32 C31 121.2(7) . . ? C24 C33 C32 120.7(5) . . ? C24 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? O40 C34 C24 122.4(6) . . ? O40 C34 N35 123.7(7) . . ? N35 C34 C24 113.9(6) . . ? C34 N35 N36 118.6(8) . . ? C34 N35 H35 123(3) . . ? N36 N35 H35 117(3) . . ? C25' C24' C33' 121.6(12) . . ? C25' C24' C34' 126.1(14) . . ? C33' C24' C34' 112.2(13) . . ? C24' C25' H25' 119.7 . . ? C24' C25' C26' 120.5(12) . . ? C26' C25' H25' 119.7 . . ? C25' C26' C31' 116.4(13) . . ? C27' C26' C25' 122.2(12) . . ? C27' C26' C31' 121.4(15) . . ? C26' C27' H27' 119.5 . . ? C28' C27' C26' 121.0(12) . . ? C28' C27' H27' 119.5 . . ? C27' C28' H28' 120.6 . . ? C27' C28' C29' 118.8(12) . . ? C29' C28' H28' 120.6 . . ? C28' C29' H29' 118.5 . . ? C30' C29' C28' 122.9(13) . . ? C30' C29' H29' 118.5 . . ? C29' C30' H30' 119.5 . . ? C29' C30' C31' 121.0(17) . . ? C31' C30' H30' 119.5 . . ? C30' C31' C26' 115(2) . . ? C32' C31' C26' 120.0(18) . . ? C32' C31' C30' 125(2) . . ? C31' C32' H32' 118.8 . . ? C33' C32' C31' 122.4(14) . . ? C33' C32' H32' 118.8 . . ? C24' C33' H33' 120.5 . . ? C32' C33' C24' 119.1(10) . . ? C32' C33' H33' 120.5 . . ? O40' C34' C24' 128(2) . . ? O40' C34' N35' 115(2) . . ? N35' C34' C24' 117(2) . . ? C34' N35' H35' 132(9) . . ? N36 N35' C34' 119(3) . . ? N36 N35' H35' 109(9) . . ? N36 C37 C39 117.6(2) . . ? O38 C37 C39 122.4(2) . . ? O38 C37 N36 120.0(2) . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C41 C46 120.8(2) . . ? C42 C41 N36 118.8(2) . . ? C46 C41 N36 120.3(2) . . ? C41 C42 H42 120.3 . . ? C41 C42 C43 119.5(2) . . ? C43 C42 H42 120.3 . . ? C42 C43 H43 119.8 . . ? C44 C43 C42 120.3(2) . . ? C44 C43 H43 119.8 . . ? C43 C44 H44 120.1 . . ? C45 C44 C43 119.8(2) . . ? C45 C44 H44 120.1 . . ? C44 C45 H45 119.8 . . ? C44 C45 C46 120.4(2) . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 119.1(2) . . ? C41 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? N35 N36 C41 113.6(4) . . ? N35' N36 C41 123.8(14) . . ? C37 N36 N35 123.3(4) . . ? C37 N36 N35' 112.5(13) . . ? C37 N36 C41 123.11(19) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N35 H35 O15 0.897(18) 1.88(2) 2.747(11) 161(4) . yes N35 H35 O15 0.897(18) 1.88(2) 2.747(11) 161(4) . yes N35' H35' O15 0.89(2) 2.04(5) 2.92(3) 165(12) . yes N35' H35' O15 0.89(2) 2.04(5) 2.92(3) 165(12) . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 179.4(2) . . . . ? C1 C2 C3 C8 1.2(3) . . . . ? C1 C11 N12 N13 -172.06(18) . . . . ? C2 C1 C10 C9 -1.6(4) . . . . ? C2 C1 C11 N12 161.8(2) . . . . ? C2 C1 C11 O17 -18.9(3) . . . . ? C2 C3 C4 C5 -178.4(2) . . . . ? C2 C3 C8 C7 177.4(2) . . . . ? C2 C3 C8 C9 -2.4(3) . . . . ? C3 C4 C5 C6 1.4(4) . . . . ? C3 C8 C9 C10 1.6(4) . . . . ? C4 C3 C8 C7 -0.9(3) . . . . ? C4 C3 C8 C9 179.4(2) . . . . ? C4 C5 C6 C7 -1.6(4) . . . . ? C5 C6 C7 C8 0.5(4) . . . . ? C6 C7 C8 C3 0.7(4) . . . . ? C6 C7 C8 C9 -179.6(3) . . . . ? C7 C8 C9 C10 -178.1(2) . . . . ? C8 C3 C4 C5 -0.2(4) . . . . ? C8 C9 C10 C1 0.4(4) . . . . ? C10 C1 C2 C3 0.7(3) . . . . ? C10 C1 C11 N12 -14.6(3) . . . . ? C10 C1 C11 O17 164.7(2) . . . . ? C11 C1 C2 C3 -175.83(19) . . . . ? C11 C1 C10 C9 174.8(2) . . . . ? C11 N12 N13 C14 -90.0(3) . . . . ? C11 N12 N13 C18 83.2(2) . . . . ? C16 C14 N13 C18 -176.9(2) . . . . ? C16 C14 N13 N12 -4.1(3) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C19 C18 C23 C22 1.3(4) . . . . ? C19 C18 N13 C14 -121.2(2) . . . . ? C19 C18 N13 N12 65.9(3) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C23 0.3(4) . . . . ? C21 C22 C23 C18 -1.2(4) . . . . ? C23 C18 C19 C20 -0.6(4) . . . . ? C23 C18 N13 C14 61.5(3) . . . . ? C23 C18 N13 N12 -111.5(2) . . . . ? N13 C18 C19 C20 -177.9(2) . . . . ? N13 C18 C23 C22 178.6(2) . . . . ? O15 C14 N13 C18 4.1(4) . . . . ? O15 C14 N13 N12 176.9(2) . . . . ? O17 C11 N12 N13 8.6(3) . . . . ? C24 C25 C26 C27 1.8(5) . . . . ? C24 C34 N35 N36 174.4(7) . . . . ? C25 C24 C33 C32 -0.2(7) . . . . ? C25 C24 C34 O40 165.4(7) . . . . ? C25 C24 C34 N35 -13.3(10) . . . . ? C25 C26 C27 C28 177.0(3) . . . . ? C25 C26 C27 C32 -1.3(6) . . . . ? C26 C27 C28 C29 -177.9(3) . . . . ? C26 C27 C32 C31 178.5(5) . . . . ? C26 C27 C32 C33 0.1(9) . . . . ? C27 C28 C29 C30 -0.6(5) . . . . ? C27 C32 C33 C24 0.7(10) . . . . ? C28 C27 C32 C31 0.0(10) . . . . ? C28 C27 C32 C33 -178.4(5) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C29 C30 C31 C32 0.1(7) . . . . ? C30 C31 C32 C27 -0.3(10) . . . . ? C30 C31 C32 C33 178.1(5) . . . . ? C31 C32 C33 C24 -177.7(5) . . . . ? C32 C27 C28 C29 0.4(7) . . . . ? C33 C24 C25 C26 -1.0(5) . . . . ? C33 C24 C34 O40 -11.2(10) . . . . ? C33 C24 C34 N35 170.1(6) . . . . ? C34 C24 C25 C26 -177.6(5) . . . . ? C34 C24 C33 C32 176.5(6) . . . . ? C34 N35 N36 C37 83.8(9) . . . . ? C34 N35 N36 C41 -95.6(8) . . . . ? O40 C34 N35 N36 -4.3(14) . . . . ? C24' C25' C26' C27' -179.5(10) . . . . ? C24' C25' C26' C31' -0.4(19) . . . . ? C24' C34' N35' N36 165(2) . . . . ? C25' C24' C33' C32' -0.9(16) . . . . ? C25' C24' C34' O40' 163(3) . . . . ? C25' C24' C34' N35' -20(3) . . . . ? C25' C26' C27' C28' -177.8(9) . . . . ? C25' C26' C31' C30' 178.8(15) . . . . ? C25' C26' C31' C32' 1(3) . . . . ? C26' C27' C28' C29' -1.7(15) . . . . ? C26' C31' C32' C33' -2(3) . . . . ? C27' C26' C31' C30' -2(3) . . . . ? C27' C26' C31' C32' -179.8(16) . . . . ? C27' C28' C29' C30' -0.8(18) . . . . ? C28' C29' C30' C31' 2(2) . . . . ? C29' C30' C31' C26' 0(3) . . . . ? C29' C30' C31' C32' 177.2(19) . . . . ? C30' C31' C32' C33' -179.3(18) . . . . ? C31' C26' C27' C28' 3.1(19) . . . . ? C31' C32' C33' C24' 2(2) . . . . ? C33' C24' C25' C26' 0.3(17) . . . . ? C33' C24' C34' O40' -15(4) . . . . ? C33' C24' C34' N35' 163(2) . . . . ? C34' C24' C25' C26' -177.3(16) . . . . ? C34' C24' C33' C32' 177.0(15) . . . . ? C34' N35' N36 C37 91(3) . . . . ? C34' N35' N36 C41 -80(3) . . . . ? O40' C34' N35' N36 -17(4) . . . . ? C39 C37 N36 N35 0.8(6) . . . . ? C39 C37 N36 N35' 9.1(14) . . . . ? C39 C37 N36 C41 -179.8(2) . . . . ? C41 C42 C43 C44 0.5(4) . . . . ? C42 C41 C46 C45 -0.5(4) . . . . ? C42 C41 N36 N35 -57.3(5) . . . . ? C42 C41 N36 N35' -66.6(15) . . . . ? C42 C41 N36 C37 123.3(3) . . . . ? C42 C43 C44 C45 -0.6(4) . . . . ? C43 C44 C45 C46 0.2(4) . . . . ? C44 C45 C46 C41 0.4(4) . . . . ? C46 C41 C42 C43 0.1(4) . . . . ? C46 C41 N36 N35 120.8(5) . . . . ? C46 C41 N36 N35' 111.5(15) . . . . ? C46 C41 N36 C37 -58.7(3) . . . . ? N36 C41 C42 C43 178.1(2) . . . . ? N36 C41 C46 C45 -178.5(2) . . . . ? O38 C37 N36 N35 179.7(5) . . . . ? O38 C37 N36 N35' -172.0(14) . . . . ? O38 C37 N36 C41 -0.9(3) . . . . ? _shelx_res_file ; TITL gb_1408_lt_mo_a.res in P-1 shelx.res created by SHELXL-2018/3 at 21:31:33 on 18-Sep-2021 CELL 0.71073 8.9164 9.7058 17.7384 88.308 89.744 86.744 ZERR 4.00 0.0007 0.0009 0.0012 0.007 0.006 0.007 LATT 1 SFAC C H N O UNIT 76 64 8 8 MERG 2 OMIT -3.00 52.00 OMIT 0 6 0 SIMU 0.02 0.04 3.0 C24 > C34' SADI 0.02 C34 O40 C34' O40' SADI 0.02 N35 C34 N35' C34' SIMU 0.02 0.04 O40 O40' DFIX 0.90 0.02 N12 H12 N35 H35 N35' H35' SIMU 0.02 0.04 N35 N35' H35 H35' EQIV $1 x, y+1, z HTAB N12 O38_$1 HTAB N35 O15 HTAB N35' O15 HTAB N12 O38_$1 HTAB N35 O15 HTAB N35' O15 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 11 WGHT 0.053100 1.282700 FVAR 0.45892 0.75310 H12 2 0.331053 0.722729 0.338575 11.00000 0.05020 MOLE 1 C1 1 0.257277 0.809501 0.469546 11.00000 0.03206 0.04303 = 0.02872 -0.00715 -0.00903 -0.00172 C2 1 0.168600 0.840426 0.530110 11.00000 0.03494 0.04136 = 0.03144 -0.00189 -0.01082 -0.00114 AFIX 43 H2 2 0.116337 0.771106 0.553893 11.00000 -1.20000 AFIX 0 C3 1 0.154239 0.977452 0.557877 11.00000 0.02944 0.04876 = 0.02922 -0.00511 -0.01240 0.00526 C4 1 0.061379 1.009203 0.620118 11.00000 0.03789 0.05110 = 0.04411 -0.00699 -0.00745 0.00345 AFIX 43 H4 2 0.010230 0.939896 0.644599 11.00000 -1.20000 AFIX 0 C5 1 0.046184 1.140228 0.644514 11.00000 0.04395 0.05625 = 0.05699 -0.01596 -0.01148 0.00834 AFIX 43 H5 2 -0.013556 1.160314 0.686321 11.00000 -1.20000 AFIX 0 C6 1 0.120863 1.246047 0.606563 11.00000 0.04980 0.04743 = 0.07289 -0.01993 -0.02216 0.01181 AFIX 43 H6 2 0.107730 1.336066 0.622973 11.00000 -1.20000 AFIX 0 C7 1 0.210528 1.219501 0.547230 11.00000 0.05142 0.04422 = 0.06013 -0.00253 -0.02366 -0.00839 AFIX 43 H7 2 0.259307 1.290942 0.523334 11.00000 -1.20000 AFIX 0 C8 1 0.231918 1.081187 0.520195 11.00000 0.04095 0.04412 = 0.04380 0.00215 -0.01668 -0.00689 C9 1 0.324369 1.047519 0.459207 11.00000 0.05380 0.04926 = 0.04406 -0.00334 -0.00644 -0.01712 AFIX 43 H9 2 0.377744 1.115705 0.435077 11.00000 -1.20000 AFIX 0 C10 1 0.337564 0.915084 0.434364 11.00000 0.05010 0.04170 = 0.04028 -0.00949 -0.00387 -0.01468 AFIX 43 H10 2 0.400313 0.894405 0.393735 11.00000 -1.20000 AFIX 0 C11 1 0.257153 0.666147 0.441198 11.00000 0.02664 0.03907 = 0.02894 -0.00298 -0.00522 -0.00576 C14 1 0.409112 0.425255 0.342116 11.00000 0.03203 0.04354 = 0.03259 -0.00812 -0.00183 0.00175 C16 1 0.546485 0.458671 0.383647 11.00000 0.03430 0.07321 = 0.05956 -0.02350 -0.01067 0.00778 AFIX 137 H16A 2 0.614555 0.378471 0.386890 11.00000 -1.50000 H16B 2 0.519253 0.486913 0.433521 11.00000 -1.50000 H16C 2 0.594246 0.532180 0.357316 11.00000 -1.50000 AFIX 0 C18 1 0.157215 0.504858 0.299429 11.00000 0.02909 0.03192 = 0.02779 -0.00544 -0.00402 -0.00276 C19 1 0.114573 0.586367 0.237734 11.00000 0.03808 0.04247 = 0.03183 0.00115 -0.00232 -0.00656 AFIX 43 H19 2 0.177561 0.651967 0.218358 11.00000 -1.20000 AFIX 0 C20 1 -0.023443 0.569591 0.204758 11.00000 0.04404 0.05478 = 0.03410 0.00541 -0.01085 -0.00322 AFIX 43 H20 2 -0.053624 0.624600 0.163130 11.00000 -1.20000 AFIX 0 C21 1 -0.115708 0.472460 0.233105 11.00000 0.03299 0.05055 = 0.04041 -0.00671 -0.01154 -0.00505 AFIX 43 H21 2 -0.207963 0.461210 0.210513 11.00000 -1.20000 AFIX 0 C22 1 -0.072007 0.391531 0.294972 11.00000 0.03428 0.03870 = 0.04687 -0.00309 -0.00374 -0.00903 AFIX 43 H22 2 -0.134585 0.325274 0.313986 11.00000 -1.20000 AFIX 0 C23 1 0.064403 0.408361 0.328908 11.00000 0.03472 0.03526 = 0.03514 0.00151 -0.00469 -0.00478 AFIX 43 H23 2 0.093313 0.354941 0.371325 11.00000 -1.20000 AFIX 0 N12 3 0.310814 0.651076 0.369606 11.00000 0.03873 0.02879 = 0.02882 -0.00460 -0.00164 -0.00909 N13 3 0.297987 0.525994 0.334867 11.00000 0.03103 0.03120 = 0.03114 -0.00506 -0.00599 -0.00537 O15 4 0.395186 0.312905 0.314270 11.00000 0.04870 0.04304 = 0.04851 -0.01729 -0.00460 0.00552 O17 4 0.214659 0.569031 0.478146 11.00000 0.04605 0.04244 = 0.03221 0.00159 -0.00009 -0.01128 MOLE 2 PART 1 C24 1 0.564707 0.327417 0.107874 21.00000 0.02573 0.02949 = 0.02610 -0.00303 -0.00474 -0.00456 C25 1 0.490864 0.441477 0.143000 21.00000 0.02814 0.03424 = 0.02791 -0.00107 -0.00125 -0.00179 AFIX 43 H25 2 0.416537 0.427060 0.178859 21.00000 -1.20000 AFIX 0 C26 1 0.528127 0.571748 0.124544 21.00000 0.03262 0.03120 = 0.03305 -0.00219 -0.00517 0.00067 AFIX 43 H26 2 0.480860 0.645741 0.149059 21.00000 -1.20000 AFIX 0 C27 1 0.638005 0.597162 0.068467 21.00000 0.02975 0.03060 = 0.02945 0.00052 -0.01223 -0.00887 C28 1 0.673694 0.732844 0.045864 21.00000 0.03583 0.03365 = 0.03667 0.00158 -0.01218 -0.00624 AFIX 43 H28 2 0.627109 0.808789 0.068937 21.00000 -1.20000 AFIX 0 C29 1 0.776852 0.750970 -0.009965 21.00000 0.03831 0.03692 = 0.04365 0.01282 -0.01684 -0.01793 AFIX 43 H29 2 0.799311 0.840076 -0.025016 21.00000 -1.20000 AFIX 0 C30 1 0.849946 0.638267 -0.045254 21.00000 0.03746 0.04992 = 0.04448 0.01211 -0.00177 -0.01415 AFIX 43 H30 2 0.920363 0.653153 -0.083029 21.00000 -1.20000 AFIX 0 C31 1 0.818057 0.508075 -0.024370 21.00000 0.03572 0.04204 = 0.03935 0.00372 0.00390 -0.01014 AFIX 43 H31 2 0.866844 0.433632 -0.047831 21.00000 -1.20000 AFIX 0 C32 1 0.710164 0.484145 0.033366 21.00000 0.02442 0.03469 = 0.02610 0.00055 -0.00370 -0.00852 C33 1 0.672253 0.349021 0.054293 21.00000 0.02817 0.03104 = 0.02726 -0.00239 -0.00366 -0.00531 AFIX 43 H33 2 0.720932 0.273900 0.031398 21.00000 -1.20000 AFIX 0 C34 1 0.524759 0.181341 0.123550 21.00000 0.02374 0.03196 = 0.02432 -0.00227 -0.00719 -0.00350 O40 4 0.566841 0.087170 0.083452 21.00000 0.03769 0.02833 = 0.03493 -0.00682 -0.00165 -0.00773 N35 3 0.435383 0.165167 0.185336 21.00000 0.02466 0.02358 = 0.02974 -0.00331 0.00064 -0.00759 PART 2 C24' 1 0.593124 0.278046 0.091598 -21.00000 0.02246 0.02649 = 0.01997 0.00003 -0.01217 -0.00182 C25' 1 0.545335 0.401549 0.115619 -21.00000 0.01741 0.02554 = 0.02370 -0.00361 -0.00388 0.00089 AFIX 43 H25' 2 0.472629 0.408145 0.153294 -21.00000 -1.20000 AFIX 0 C26' 1 0.606363 0.527196 0.083180 -21.00000 0.02449 0.02584 = 0.02885 0.00161 -0.01210 -0.00343 C27' 1 0.560663 0.656421 0.106957 -21.00000 0.02948 0.03451 = 0.03244 0.00068 -0.00436 -0.00473 AFIX 43 H27' 2 0.491213 0.665135 0.146040 -21.00000 -1.20000 AFIX 0 C28' 1 0.615158 0.771235 0.074378 -21.00000 0.03587 0.02857 = 0.03575 0.00201 -0.00963 -0.00934 AFIX 43 H28' 2 0.581845 0.858482 0.089837 -21.00000 -1.20000 AFIX 0 C29' 1 0.722952 0.756112 0.016794 -21.00000 0.02915 0.03098 = 0.02599 0.00109 0.00284 -0.00976 AFIX 43 H29' 2 0.759221 0.835217 -0.005900 -21.00000 -1.20000 AFIX 0 C30' 1 0.776107 0.632248 -0.007014 -21.00000 0.03287 0.03569 = 0.03112 -0.00054 -0.00445 -0.01031 AFIX 43 H30' 2 0.849513 0.627897 -0.044413 -21.00000 -1.20000 AFIX 0 C31' 1 0.721643 0.507901 0.024193 -21.00000 0.02746 0.03009 = 0.02918 0.00172 -0.01292 -0.01019 C32' 1 0.764127 0.378193 0.001693 -21.00000 0.03199 0.02952 = 0.02782 0.00003 0.00760 -0.00334 AFIX 43 H32' 2 0.835006 0.368074 -0.036659 -21.00000 -1.20000 AFIX 0 C33' 1 0.706429 0.262851 0.033400 -21.00000 0.03409 0.02809 = 0.02644 -0.00050 0.00194 0.00398 AFIX 43 H33' 2 0.739500 0.175627 0.017807 -21.00000 -1.20000 AFIX 0 C34' 1 0.538019 0.146198 0.116584 -21.00000 0.02549 0.02850 = 0.02958 -0.00070 -0.00688 -0.00428 O40' 4 0.553396 0.036648 0.085836 -21.00000 0.04456 0.01744 = 0.04693 -0.01240 0.00165 -0.01121 N35' 3 0.463509 0.143571 0.184116 -21.00000 0.02683 0.01298 = 0.03449 -0.00510 0.00171 0.00625 PART 0 C37 1 0.458712 -0.067080 0.239258 11.00000 0.03615 0.03958 = 0.02602 0.00237 -0.00461 -0.00990 C39 1 0.611357 -0.037570 0.266203 11.00000 0.04393 0.06843 = 0.04799 0.01802 -0.01808 -0.01833 AFIX 137 H39A 2 0.648772 -0.111687 0.299230 11.00000 -1.50000 H39B 2 0.605874 0.047116 0.292965 11.00000 -1.50000 H39C 2 0.677753 -0.029130 0.223771 11.00000 -1.50000 AFIX 0 C41 1 0.231860 0.019545 0.172674 11.00000 0.02971 0.03247 = 0.03070 0.00187 -0.00254 -0.01066 C42 1 0.117445 0.110449 0.194565 11.00000 0.03725 0.04686 = 0.04407 -0.01211 0.00568 -0.01024 AFIX 43 H42 2 0.135607 0.178618 0.228592 11.00000 -1.20000 AFIX 0 C43 1 -0.024664 0.099860 0.165686 11.00000 0.03088 0.05855 = 0.05794 -0.01100 0.00483 -0.00210 AFIX 43 H43 2 -0.102446 0.161611 0.180004 11.00000 -1.20000 AFIX 0 C44 1 -0.051869 -0.001525 0.115847 11.00000 0.03006 0.05269 = 0.05165 0.00219 -0.00580 -0.01312 AFIX 43 H44 2 -0.148031 -0.008952 0.096855 11.00000 -1.20000 AFIX 0 C45 1 0.063412 -0.091841 0.094175 11.00000 0.04115 0.03395 = 0.04833 -0.00184 -0.01326 -0.01161 AFIX 43 H45 2 0.045033 -0.160258 0.060336 11.00000 -1.20000 AFIX 0 C46 1 0.206507 -0.081731 0.122314 11.00000 0.03571 0.02943 = 0.04469 -0.00223 -0.00881 -0.00374 AFIX 43 H46 2 0.284661 -0.142567 0.107417 11.00000 -1.20000 AFIX 0 N36 3 0.380053 0.034453 0.201361 11.00000 0.03204 0.03067 = 0.03460 0.00056 -0.00458 -0.01228 O38 4 0.403485 -0.178610 0.251590 11.00000 0.04768 0.03814 = 0.03781 0.00788 -0.00767 -0.01326 PART 1 H35 2 0.420581 0.229560 0.220254 21.00000 0.02756 PART 2 H35' 2 0.457862 0.202348 0.222026 -21.00000 0.02500 HKLF 4 REM gb_1408_lt_mo_a.res in P-1 REM wR2 = 0.1579, GooF = S = 1.060, Restrained GooF = 0.987 for all data REM R1 = 0.0580 for 4639 Fo > 4sig(Fo) and 0.0743 for all 5935 data REM 547 parameters refined using 936 restraints END WGHT 0.0531 1.2798 REM Highest difference peak 0.607, deepest hole -0.271, 1-sigma level 0.048 Q1 1 0.0918 0.8941 0.5850 11.00000 0.05 0.61 Q2 1 0.2743 1.2762 0.4983 11.00000 0.05 0.52 Q3 1 0.3158 1.1555 0.4693 11.00000 0.05 0.49 Q4 1 0.1244 1.1497 0.5914 11.00000 0.05 0.44 Q5 1 0.2610 1.0142 0.4949 11.00000 0.05 0.31 Q6 1 0.2745 0.8973 0.4702 11.00000 0.05 0.27 Q7 1 0.4097 0.3684 0.2723 11.00000 0.05 0.26 Q8 1 0.1805 1.2933 0.5660 11.00000 0.05 0.24 Q9 1 0.3416 -0.1229 0.2855 11.00000 0.05 0.21 Q10 1 0.3865 0.4956 0.3133 11.00000 0.05 0.18 Q11 1 0.2185 0.7786 0.4981 11.00000 0.05 0.17 Q12 1 0.5784 0.3387 0.0605 11.00000 0.05 0.16 Q13 1 0.6856 0.5383 0.0476 11.00000 0.05 0.16 Q14 1 0.4439 0.6036 0.2445 11.00000 0.05 0.16 Q15 1 0.3835 1.1390 0.4149 11.00000 0.05 0.16 Q16 1 -0.1577 0.3235 0.3419 11.00000 0.05 0.16 Q17 1 0.1638 0.0459 0.1986 11.00000 0.05 0.15 Q18 1 -0.1071 0.2134 0.1509 11.00000 0.05 0.15 Q19 1 0.1762 0.8366 0.4792 11.00000 0.05 0.15 Q20 1 0.5489 0.5522 0.4047 11.00000 0.05 0.15 Q21 1 0.1372 1.0328 0.5678 11.00000 0.05 0.14 Q22 1 0.0899 0.5173 0.3319 11.00000 0.05 0.14 Q23 1 0.0811 -0.1985 0.0289 11.00000 0.05 0.14 Q24 1 0.7071 -0.1676 0.2564 11.00000 0.05 0.14 Q25 1 0.1875 0.9662 0.5516 11.00000 0.05 0.14 ; _shelx_res_checksum 36609 _shelx_hkl_file ; 0 0 -2 54.24 1.16 0 0 -2 61.94 1.06 0 0 -3 96.98 1.88 0 0 -3 97.35 1.65 0 0 -4 0.13 0.12 0 0 -4 0.44 0.19 0 0 -5 74.94 1.87 0 0 -5 71.91 2.07 0 0 -6 12.33 0.85 0 0 -6 14.69 1.02 0 0 -7 173.68 3.82 0 0 -7 180.07 3.50 0 0 -8 7.08 0.86 0 0 -8 7.09 0.77 0 0 -9 240.43 5.17 0 0 -9 253.96 4.72 0 0 -10 16.41 1.46 0 0 -10 15.99 1.28 0 0 -11 48.78 2.56 0 0 -11 47.18 2.30 0 0 -12 60.01 2.97 0 0 -12 58.97 2.70 0 0 -13 3.20 0.68 0 0 -13 4.40 0.88 0 0 -14 111.06 4.05 0 0 -14 101.96 4.39 0 0 -15 0.29 0.26 0 0 -16 18.07 1.83 0 0 -17 4.16 0.91 0 0 -18 3.21 0.86 0 0 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2.65 10 -2 -10 5.58 1.26 10 -2 -10 4.55 1.19 10 -2 -9 0.90 0.46 10 -2 -8 7.78 1.46 10 -2 -7 3.62 0.98 10 -2 -6 0.19 0.38 10 -2 -5 -0.79 0.57 10 -2 -4 1.50 0.55 10 -2 -3 0.59 0.37 10 -2 -2 2.50 0.88 10 -2 -1 0.41 0.57 10 -2 0 5.46 1.27 10 -2 1 1.08 0.68 10 -2 2 2.59 0.88 10 -2 3 24.86 2.55 10 -2 4 4.13 1.06 10 -2 5 6.19 1.33 10 -2 6 28.72 2.73 10 -2 7 11.45 1.73 10 -2 8 1.23 0.59 10 -2 9 4.46 1.11 10 -2 10 2.08 0.82 -10 2 -11 1.32 0.63 -10 2 -12 -0.17 0.43 10 -1 -10 9.56 1.60 10 -1 -9 1.28 0.63 10 -1 -8 0.46 0.31 10 -1 -7 2.37 0.84 10 -1 -6 0.00 0.45 10 -1 -5 -0.38 0.54 10 -1 -4 -0.36 0.38 10 -1 -3 0.70 0.47 10 -1 -2 0.60 0.54 10 -1 -1 -0.56 0.61 10 -1 0 7.51 1.35 10 -1 1 3.35 0.95 10 -1 2 0.73 0.47 10 -1 3 0.53 0.29 10 -1 4 14.37 1.93 10 -1 5 2.07 0.72 10 -1 6 -0.15 0.48 10 -1 7 16.51 2.05 -10 1 -7 13.80 1.85 10 -1 8 4.77 1.07 -10 1 -8 5.02 1.13 10 -1 9 6.46 1.29 -10 1 -9 8.15 1.47 10 -1 10 4.89 1.13 -10 1 -10 5.48 1.22 -10 1 -11 -1.19 0.64 10 0 -10 3.57 1.00 10 0 -9 3.16 0.94 10 0 -8 7.52 1.40 10 0 -7 2.27 0.84 10 0 -6 0.51 0.48 10 0 -5 0.54 0.51 10 0 -4 0.46 0.31 10 0 -3 4.20 1.05 10 0 -2 15.14 1.97 10 0 -1 0.56 0.45 10 0 0 4.97 1.19 10 0 1 -0.06 0.41 10 0 2 5.84 1.26 10 0 3 3.55 0.99 10 0 4 8.12 1.44 -10 0 -4 6.09 1.23 10 0 5 3.54 1.00 -10 0 -5 3.64 0.93 10 0 6 13.56 1.84 -10 0 -6 16.34 2.02 10 0 7 -0.81 0.58 -10 0 -7 0.01 0.39 10 0 8 -0.88 0.69 -10 0 -8 -0.34 0.53 10 0 9 6.65 1.29 -10 0 -9 7.40 1.46 10 0 10 13.78 1.92 -10 0 -10 20.19 2.43 -10 0 -11 11.92 1.88 10 1 -10 9.63 1.60 10 1 -9 10.92 1.74 10 1 -8 -0.70 0.62 10 1 -7 10.25 1.65 10 1 -6 12.28 1.79 10 1 -5 1.56 0.72 10 1 -4 2.84 0.87 10 1 -3 3.00 0.90 10 1 -2 11.22 1.71 10 1 -1 5.98 1.27 10 1 0 32.62 2.91 10 1 1 4.78 1.13 10 1 2 1.45 0.55 10 1 3 2.73 0.78 -10 -1 -3 1.38 0.66 10 1 4 0.46 0.30 -10 -1 -4 0.97 0.41 10 1 5 0.63 0.54 -10 -1 -5 2.71 0.91 10 1 6 1.05 0.66 -10 -1 -6 0.92 0.55 10 1 7 1.64 0.66 -10 -1 -7 1.60 0.68 10 1 8 0.41 0.27 -10 -1 -8 -0.67 0.47 10 1 9 4.06 0.96 -10 -1 -9 4.98 1.21 10 1 10 0.31 0.31 -10 -1 -10 0.82 0.51 -10 -1 -11 0.29 0.31 10 2 -10 2.01 0.79 10 2 -9 2.36 0.84 10 2 -8 4.20 1.11 10 2 -7 1.31 0.61 10 2 -6 3.26 0.96 10 2 -5 6.53 1.33 10 2 -4 2.83 0.87 10 2 -3 22.86 2.45 10 2 -2 20.71 2.29 10 2 -1 2.26 0.82 10 2 0 19.62 2.25 10 2 1 1.30 0.52 10 2 2 2.85 0.85 10 2 3 2.26 0.77 10 2 4 0.53 0.42 10 2 5 2.79 0.94 -10 -2 -5 1.59 0.66 10 2 6 1.16 0.48 -10 -2 -6 2.59 0.93 10 2 7 2.27 0.79 -10 -2 -7 3.33 1.05 10 2 8 2.54 0.83 -10 -2 -8 2.98 0.89 10 2 9 5.82 1.26 -10 -2 -9 6.29 1.41 10 2 10 1.76 0.66 -10 -2 -10 1.45 0.72 10 3 -9 3.19 0.95 10 3 -8 4.39 1.15 10 3 -7 0.62 0.56 10 3 -6 3.01 0.96 10 3 -5 0.30 0.50 10 3 -4 5.85 1.22 10 3 -3 1.01 0.47 10 3 -2 10.65 1.70 10 3 -1 -0.29 0.38 10 3 0 0.49 0.52 10 3 1 -0.04 0.28 10 3 2 1.55 0.70 10 3 3 10.43 1.68 10 3 4 0.55 0.54 10 3 5 0.03 0.41 10 3 6 0.34 0.44 -10 -3 -6 0.00 0.47 10 3 7 0.24 0.42 -10 -3 -7 -0.21 0.43 10 3 8 -0.08 0.48 -10 -3 -8 -0.30 0.59 10 3 9 12.69 1.84 -10 -3 -9 12.73 2.03 10 3 10 5.79 1.23 10 4 -9 0.44 0.60 10 4 -8 8.22 1.52 10 4 -7 -0.31 0.38 10 4 -6 0.08 0.35 10 4 -5 1.33 0.68 10 4 -4 2.06 0.84 10 4 -3 2.33 0.81 10 4 -2 -1.34 0.66 10 4 -1 7.95 1.50 10 4 0 11.86 1.81 10 4 1 4.86 1.23 10 4 2 1.99 0.73 10 4 3 -0.09 0.30 10 4 4 0.32 0.51 10 4 5 0.28 0.39 10 4 6 0.33 0.44 10 4 7 2.21 0.82 -10 -4 -7 3.51 1.17 10 4 8 4.68 1.19 -10 -4 -8 4.74 1.27 10 4 9 3.04 0.92 10 4 10 0.02 0.29 10 5 -9 6.68 1.41 10 5 -8 2.52 0.95 10 5 -7 -0.01 0.31 10 5 -6 3.22 1.03 10 5 -5 1.00 0.60 10 5 -4 13.29 1.98 10 5 -3 6.41 1.36 10 5 -2 1.72 0.55 10 5 -1 5.02 1.23 10 5 0 0.22 0.34 10 5 1 36.70 3.26 10 5 2 53.19 3.92 10 5 3 10.99 1.79 10 5 4 0.71 0.32 10 5 5 3.77 1.03 10 5 6 5.39 1.29 10 5 7 4.88 1.22 10 5 8 0.17 0.35 10 5 9 0.01 0.31 10 5 10 2.02 0.73 10 6 -2 1.40 0.71 10 6 -1 -0.18 0.50 10 6 0 3.98 1.15 10 6 1 2.55 0.85 10 6 2 1.60 0.87 10 6 3 14.21 2.08 10 6 4 14.67 2.12 11 -1 -4 0.87 0.72 11 -1 -3 0.35 0.41 11 -1 -2 0.73 0.34 11 -1 -1 1.37 0.65 11 -1 0 -0.23 0.43 11 -1 1 6.14 1.35 11 -1 2 0.61 0.45 11 -1 3 0.11 0.42 11 -1 4 2.40 0.81 11 -1 5 7.40 1.49 11 0 -5 0.61 0.54 11 0 -4 4.36 1.13 11 0 -3 1.61 0.81 11 0 -2 -0.34 0.28 11 0 -1 0.29 0.51 11 0 0 10.07 1.71 11 0 1 0.38 0.36 11 0 2 1.65 0.71 11 0 3 0.48 0.51 11 0 4 -0.57 0.66 11 0 5 3.55 1.04 11 0 6 5.36 1.27 11 0 7 1.18 0.64 -11 0 -8 1.67 0.86 -11 0 -9 0.99 0.53 11 1 -6 10.78 1.82 11 1 -5 -0.20 0.57 11 1 -4 0.19 0.25 11 1 -3 1.28 0.66 11 1 -2 6.94 1.40 11 1 -1 3.74 1.07 11 1 0 7.72 1.53 11 1 1 0.22 0.38 11 1 2 7.68 1.56 11 1 3 0.27 0.39 11 1 4 3.01 0.96 11 1 5 -1.11 0.64 -11 -1 -5 0.89 0.56 11 1 6 -0.42 0.49 -11 -1 -6 0.73 0.49 11 1 7 0.17 0.46 -11 -1 -7 0.71 0.48 11 1 8 7.07 1.39 -11 -1 -8 7.60 1.50 11 2 -4 1.63 0.77 11 2 -3 23.70 2.67 11 2 -2 0.96 0.62 11 2 -1 19.41 2.39 11 2 0 -0.07 0.36 11 2 1 4.53 1.23 11 2 2 0.63 0.64 11 2 3 3.19 0.95 -11 -2 -3 2.69 0.87 11 2 4 -0.49 0.65 -11 -2 -4 0.03 0.39 11 2 5 3.71 1.12 -11 -2 -5 3.89 1.09 11 2 6 -0.50 0.45 -11 -2 -6 -0.86 0.60 -11 -2 -7 1.42 0.69 11 3 0 6.66 1.44 11 3 1 23.74 2.66 11 3 2 9.17 1.67 -11 -3 -5 0.19 0.46 -11 -3 -6 1.58 0.80 0 0 0 0.00 0.00 TITL GB_1408_Lt_Mo in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.916371 9.705826 17.738391 88.3083 89.7445 86.7441 ZERR 29.00 0.000655 0.000911 0.001209 0.0065 0.0057 0.0068 LATT 1 SFAC C H N O UNIT 29.00 29.00 29.00 29.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 24530 _olex2_submission_special_instructions 'No special instructions were received'