data_007-15075 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 Li N5 O9, 2(H2 O)' _chemical_formula_sum 'C18 H40 Li N5 O11' _chemical_formula_weight 509.49 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' 'Li' 'Li' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.5430(8) _cell_length_b 7.5993(5) _cell_length_c 14.3503(10) _cell_angle_alpha 90 _cell_angle_beta 99.189(4) _cell_angle_gamma 90 _cell_volume 1242.64(15) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 454 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 68.3 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.362 _exptl_crystal_F_000 548 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.943 _shelx_estimated_absorpt_T_min 0.834 _shelx_estimated_absorpt_T_max 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'Sealed Tube' _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 38051 _diffrn_reflns_av_unetI/netI 0.0771 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.119 _diffrn_reflns_theta_max 67.552 _diffrn_reflns_theta_full 67.552 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_point_group_measured_fraction_full 0.967 _reflns_number_total 4336 _reflns_number_gt 3700 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.810 _reflns_Friedel_fraction_max 0.942 _reflns_Friedel_fraction_full 0.943 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ; Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: A complete structure solution, refinement and analysis program (2009). J. Appl. Cryst., 42, 339-341. ; _computing_publication_material 'SHELXL-2013/2 (Sheldrick, 2014)' _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. The hydrogen atoms were first found in the difference map, then generated geometrically and refined as riding atoms with C-H dis Several reflection ([3 -5 13] and [1 -8 0]) were omitted due to pixel saturation which resulted in improper recording of the ref ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1259 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.08(10) _chemical_absolute_configuration ad _refine_ls_number_reflns 4336 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.09374(15) 0.9130(2) 0.77123(11) 0.0227(4) Uani 1 1 d . . . . . O2 O 0.15480(15) 0.6591(2) 0.71738(11) 0.0208(4) Uani 1 1 d . . . . . O3 O 0.28820(16) 0.5468(2) 0.92172(11) 0.0205(4) Uani 1 1 d . . . . . O4 O 0.49121(15) 0.2103(2) 0.76852(11) 0.0215(4) Uani 1 1 d . . . . . O5 O 0.20176(15) 0.2096(2) 0.49942(11) 0.0215(4) Uani 1 1 d . . . . . O6 O 0.22865(15) 0.49761(19) 0.48252(11) 0.0202(4) Uani 1 1 d . . . . . O7 O 0.00003(19) 0.0639(2) 0.60149(13) 0.0200(4) Uani 1 1 d . . . . . H7A H 0.030(3) 0.008(4) 0.658(2) 0.045(10) Uiso 1 1 d . . . . . H7B H -0.072(4) 0.032(5) 0.582(2) 0.055(12) Uiso 1 1 d . . . . . O8 O 0.20306(16) -0.1752(3) 0.56176(14) 0.0225(4) Uani 1 1 d . . . . . H8A H 0.185(3) -0.225(5) 0.617(3) 0.068(12) Uiso 1 1 d . . . . . H8B H 0.208(3) -0.272(5) 0.527(2) 0.051(10) Uiso 1 1 d . . . . . O9 O 0.01226(18) -0.0666(3) 0.39282(12) 0.0222(4) Uani 1 1 d . . . . . H9A H -0.049(4) -0.016(5) 0.360(3) 0.064(12) Uiso 1 1 d . . . . . H9B H -0.001(3) -0.170(5) 0.384(2) 0.045(11) Uiso 1 1 d . . . . . N1 N 0.09951(19) 0.4718(3) 0.86426(14) 0.0159(5) Uani 1 1 d . . . . . H1 H 0.054(2) 0.382(3) 0.8417(17) 0.019(7) Uiso 1 1 d . . . . . N2 N 0.35991(17) 0.2111(3) 0.86922(12) 0.0163(5) Uani 1 1 d . . . . . N3 N 0.3836(2) 0.5256(3) 0.64324(14) 0.0177(5) Uani 1 1 d . . . . . H3 H 0.331(3) 0.598(4) 0.663(2) 0.028(8) Uiso 1 1 d . . . . . N4 N 0.53308(18) 0.6974(3) 0.71992(13) 0.0186(5) Uani 1 1 d . . . . . N5 N 0.57323(18) 0.4872(2) 0.61169(14) 0.0178(5) Uani 1 1 d . . . . . C1 C 0.1072(2) 0.7488(3) 0.77459(16) 0.0176(6) Uani 1 1 d . . . . . C2 C 0.0510(2) 0.6509(3) 0.85070(16) 0.0170(6) Uani 1 1 d . . . . . C3 C 0.0644(2) 0.7520(3) 0.94370(16) 0.0194(6) Uani 1 1 d . . . . . H3A H 0.0346 0.6801 0.9914 0.029 Uiso 1 1 calc R U . . . H3B H 0.0197 0.8619 0.9345 0.029 Uiso 1 1 calc R U . . . H3C H 0.1475 0.7787 0.9649 0.029 Uiso 1 1 calc R U . . . C4 C -0.0788(2) 0.6299(3) 0.80956(18) 0.0220(6) Uani 1 1 d . . . . . H4A H -0.1157 0.7461 0.8009 0.033 Uiso 1 1 calc R U . . . H4B H -0.1179 0.5602 0.8529 0.033 Uiso 1 1 calc R U . . . H4C H -0.0861 0.5697 0.7485 0.033 Uiso 1 1 calc R U . . . C5 C 0.2122(2) 0.4360(3) 0.89384(15) 0.0158(6) Uani 1 1 d . . . . . C6 C 0.2427(2) 0.2400(3) 0.89416(16) 0.0171(5) Uani 1 1 d . . . . . H6 H 0.1820 0.1737 0.8503 0.020 Uiso 1 1 calc R U . . . C7 C 0.2536(2) 0.1652(3) 0.99519(17) 0.0219(6) Uani 1 1 d . . . . . H7C H 0.2659 0.2609 1.0426 0.026 Uiso 1 1 calc R U . . . H7D H 0.1822 0.0986 1.0035 0.026 Uiso 1 1 calc R U . . . C8 C 0.3606(2) 0.0437(3) 1.00467(17) 0.0206(6) Uani 1 1 d . . . . . H8C H 0.3965 0.0287 1.0716 0.025 Uiso 1 1 calc R U . . . H8D H 0.3395 -0.0732 0.9766 0.025 Uiso 1 1 calc R U . . . C9 C 0.4421(2) 0.1419(3) 0.94973(17) 0.0195(6) Uani 1 1 d . . . . . H9C H 0.4838 0.2382 0.9877 0.023 Uiso 1 1 calc R U . . . H9D H 0.5004 0.0617 0.9286 0.023 Uiso 1 1 calc R U . . . C10 C 0.3890(2) 0.2310(3) 0.78284(16) 0.0168(6) Uani 1 1 d . . . . . C11 C 0.2896(2) 0.2705(3) 0.70158(16) 0.0176(6) Uani 1 1 d . . . . . H11A H 0.2467 0.1605 0.6819 0.021 Uiso 1 1 calc R U . . . H11B H 0.2338 0.3540 0.7233 0.021 Uiso 1 1 calc R U . . . C12 C 0.3373(2) 0.3494(3) 0.61739(16) 0.0165(6) Uani 1 1 d . . . . . H12 H 0.4045 0.2745 0.6052 0.020 Uiso 1 1 calc R U . . . C13 C 0.4970(2) 0.5686(3) 0.65785(15) 0.0155(6) Uani 1 1 d . . . . . C14 C 0.4595(2) 0.7559(4) 0.78743(18) 0.0246(6) Uani 1 1 d . . . . . H14A H 0.4015 0.8407 0.7570 0.037 Uiso 1 1 calc R U . . . H14B H 0.5085 0.8120 0.8413 0.037 Uiso 1 1 calc R U . . . H14C H 0.4190 0.6545 0.8094 0.037 Uiso 1 1 calc R U . . . C15 C 0.6287(2) 0.8171(3) 0.70685(17) 0.0234(6) Uani 1 1 d . . . . . H15A H 0.6630 0.7798 0.6518 0.035 Uiso 1 1 calc R U . . . H15B H 0.6891 0.8145 0.7632 0.035 Uiso 1 1 calc R U . . . H15C H 0.5980 0.9370 0.6968 0.035 Uiso 1 1 calc R U . . . C16 C 0.6918(2) 0.4392(4) 0.65851(17) 0.0253(6) Uani 1 1 d . . . . . H16A H 0.7500 0.5085 0.6316 0.038 Uiso 1 1 calc R U . . . H16B H 0.7052 0.3137 0.6488 0.038 Uiso 1 1 calc R U . . . H16C H 0.6991 0.4635 0.7263 0.038 Uiso 1 1 calc R U . . . C17 C 0.5424(2) 0.4281(4) 0.51404(16) 0.0226(6) Uani 1 1 d . . . . . H17A H 0.5419 0.2992 0.5121 0.034 Uiso 1 1 calc R U . . . H17B H 0.6003 0.4728 0.4769 0.034 Uiso 1 1 calc R U . . . H17C H 0.4644 0.4727 0.4876 0.034 Uiso 1 1 calc R U . . . C18 C 0.2465(2) 0.3543(3) 0.52551(16) 0.0162(6) Uani 1 1 d . . . . . Li1 Li 0.1034(4) 0.0178(5) 0.5079(3) 0.0212(10) Uani 1 1 d . . . . . O10 O -0.0580(2) 1.1781(3) 0.81776(13) 0.0276(5) Uani 1 1 d . . . . . H10A H -0.128(3) 1.161(4) 0.836(2) 0.039(10) Uiso 1 1 d . . . . . H10B H -0.033(3) 1.081(5) 0.803(2) 0.048(11) Uiso 1 1 d . . . . . O11 O 0.71759(19) 0.1283(3) 0.87395(16) 0.0300(5) Uani 1 1 d . . . . . H11C H 0.713(3) 0.121(4) 0.937(3) 0.048(10) Uiso 1 1 d . . . . . H11D H 0.649(3) 0.163(5) 0.844(2) 0.054(11) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0285(11) 0.0155(9) 0.0232(9) 0.0011(8) 0.0016(8) 0.0026(8) O2 0.0257(11) 0.0210(9) 0.0164(9) -0.0002(7) 0.0058(8) 0.0009(8) O3 0.0177(10) 0.0201(9) 0.0229(9) -0.0033(7) 0.0007(8) -0.0037(8) O4 0.0161(10) 0.0273(10) 0.0213(9) 0.0017(8) 0.0036(7) 0.0026(8) O5 0.0235(11) 0.0186(9) 0.0218(9) -0.0029(7) 0.0014(8) -0.0047(8) O6 0.0213(11) 0.0160(9) 0.0227(10) 0.0020(7) 0.0014(8) 0.0005(8) O7 0.0190(12) 0.0219(9) 0.0187(10) -0.0002(8) 0.0019(9) 0.0002(9) O8 0.0273(12) 0.0191(9) 0.0221(10) 0.0018(9) 0.0074(8) 0.0033(8) O9 0.0250(12) 0.0173(11) 0.0222(11) 0.0002(8) -0.0029(9) -0.0009(9) N1 0.0144(13) 0.0152(11) 0.0175(11) -0.0005(9) 0.0010(9) -0.0010(10) N2 0.0133(11) 0.0197(11) 0.0158(10) 0.0003(9) 0.0021(8) 0.0020(9) N3 0.0140(13) 0.0140(10) 0.0248(12) -0.0027(9) 0.0018(10) 0.0021(10) N4 0.0198(12) 0.0189(11) 0.0161(10) -0.0033(9) 0.0003(9) -0.0062(9) N5 0.0139(13) 0.0218(11) 0.0177(11) -0.0014(9) 0.0026(9) -0.0020(9) C1 0.0144(14) 0.0215(15) 0.0149(12) -0.0013(11) -0.0039(11) 0.0002(12) C2 0.0156(15) 0.0160(12) 0.0186(13) -0.0002(10) 0.0005(11) 0.0016(11) C3 0.0195(15) 0.0203(12) 0.0181(13) -0.0003(11) 0.0025(11) 0.0019(11) C4 0.0180(16) 0.0252(14) 0.0226(14) -0.0022(11) 0.0028(12) 0.0020(12) C5 0.0173(16) 0.0199(13) 0.0106(12) 0.0004(11) 0.0032(10) 0.0000(12) C6 0.0131(14) 0.0196(13) 0.0184(12) 0.0010(11) 0.0024(10) -0.0018(11) C7 0.0215(16) 0.0214(13) 0.0234(14) 0.0009(11) 0.0050(11) -0.0003(12) C8 0.0229(16) 0.0186(13) 0.0204(13) 0.0030(11) 0.0033(12) 0.0000(12) C9 0.0195(15) 0.0205(13) 0.0171(13) 0.0022(11) -0.0015(11) 0.0017(12) C10 0.0149(15) 0.0148(12) 0.0208(13) -0.0004(10) 0.0030(11) -0.0002(12) C11 0.0134(14) 0.0226(13) 0.0164(13) -0.0010(10) 0.0011(10) -0.0005(11) C12 0.0161(15) 0.0140(12) 0.0193(13) -0.0027(10) 0.0025(11) -0.0016(11) C13 0.0161(16) 0.0151(12) 0.0140(13) 0.0033(11) -0.0012(11) 0.0012(12) C14 0.0251(16) 0.0256(14) 0.0234(13) -0.0065(11) 0.0047(12) -0.0012(12) C15 0.0228(16) 0.0227(13) 0.0239(14) -0.0012(12) 0.0010(12) -0.0076(13) C16 0.0194(16) 0.0302(15) 0.0254(15) 0.0019(12) 0.0011(12) 0.0043(12) C17 0.0262(17) 0.0221(13) 0.0207(14) -0.0040(11) 0.0069(12) -0.0043(12) C18 0.0149(15) 0.0194(14) 0.0151(13) -0.0011(11) 0.0048(11) 0.0002(11) Li1 0.022(3) 0.020(2) 0.021(2) -0.0004(17) 0.0002(19) -0.001(2) O10 0.0265(13) 0.0219(11) 0.0364(11) -0.0070(9) 0.0112(9) -0.0043(10) O11 0.0189(12) 0.0469(12) 0.0239(12) -0.0011(9) 0.0020(9) 0.0023(10) _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 O1 C1 1.258(3) . ? O2 C1 1.258(3) . ? O3 C5 1.236(3) . ? O4 C10 1.239(3) . ? O5 C18 1.247(3) . ? O5 Li1 1.863(5) . ? O6 C18 1.252(3) . ? O7 Li1 1.966(5) . ? O7 H7A 0.93(3) . ? O7 H7B 0.86(4) . ? O8 Li1 1.946(4) . ? O8 H8A 0.93(4) . ? O8 H8B 0.90(4) . ? O9 Li1 1.921(4) . ? O9 H9A 0.88(4) . ? O9 H9B 0.81(4) . ? N1 C5 1.330(3) . ? N1 C2 1.473(3) . ? N1 H1 0.89(3) . ? N2 C10 1.344(3) . ? N2 C9 1.470(3) . ? N2 C6 1.470(3) . ? N3 C13 1.333(3) . ? N3 C12 1.467(3) . ? N3 H3 0.90(3) . ? N4 C13 1.344(3) . ? N4 C14 1.456(3) . ? N4 C15 1.465(3) . ? N5 C13 1.335(3) . ? N5 C17 1.460(3) . ? N5 C16 1.471(3) . ? C1 C2 1.547(4) . ? C2 C3 1.526(3) . ? C2 C4 1.529(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.531(3) . ? C6 C7 1.543(4) . ? C6 H6 1.0000 . ? C7 C8 1.530(4) . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 C9 1.517(4) . ? C8 H8C 0.9900 . ? C8 H8D 0.9900 . ? C9 H9C 0.9900 . ? C9 H9D 0.9900 . ? C10 C11 1.529(3) . ? C11 C12 1.528(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C18 1.548(3) . ? C12 H12 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O10 H10A 0.89(4) . ? O10 H10B 0.84(4) . ? O11 H11C 0.92(4) . ? O11 H11D 0.88(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 O5 Li1 153.9(2) . . ? Li1 O7 H7A 109(2) . . ? Li1 O7 H7B 113(2) . . ? H7A O7 H7B 111(3) . . ? Li1 O8 H8A 117(2) . . ? Li1 O8 H8B 119(2) . . ? H8A O8 H8B 100(3) . . ? Li1 O9 H9A 127(2) . . ? Li1 O9 H9B 122(2) . . ? H9A O9 H9B 103(3) . . ? C5 N1 C2 124.2(2) . . ? C5 N1 H1 116.9(16) . . ? C2 N1 H1 117.9(16) . . ? C10 N2 C9 122.7(2) . . ? C10 N2 C6 125.68(19) . . ? C9 N2 C6 111.44(18) . . ? C13 N3 C12 124.9(2) . . ? C13 N3 H3 119.7(18) . . ? C12 N3 H3 113.7(18) . . ? C13 N4 C14 120.8(2) . . ? C13 N4 C15 121.8(2) . . ? C14 N4 C15 115.3(2) . . ? C13 N5 C17 122.7(2) . . ? C13 N5 C16 121.81(19) . . ? C17 N5 C16 115.4(2) . . ? O1 C1 O2 125.2(2) . . ? O1 C1 C2 116.1(2) . . ? O2 C1 C2 118.4(2) . . ? N1 C2 C3 111.49(18) . . ? N1 C2 C4 106.4(2) . . ? C3 C2 C4 110.3(2) . . ? N1 C2 C1 110.1(2) . . ? C3 C2 C1 112.37(19) . . ? C4 C2 C1 105.87(18) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 N1 124.9(2) . . ? O3 C5 C6 120.7(2) . . ? N1 C5 C6 114.4(2) . . ? N2 C6 C5 111.4(2) . . ? N2 C6 C7 103.51(18) . . ? C5 C6 C7 110.20(19) . . ? N2 C6 H6 110.5 . . ? C5 C6 H6 110.5 . . ? C7 C6 H6 110.5 . . ? C8 C7 C6 104.4(2) . . ? C8 C7 H7C 110.9 . . ? C6 C7 H7C 110.9 . . ? C8 C7 H7D 110.9 . . ? C6 C7 H7D 110.9 . . ? H7C C7 H7D 108.9 . . ? C9 C8 C7 102.47(19) . . ? C9 C8 H8C 111.3 . . ? C7 C8 H8C 111.3 . . ? C9 C8 H8D 111.3 . . ? C7 C8 H8D 111.3 . . ? H8C C8 H8D 109.2 . . ? N2 C9 C8 102.0(2) . . ? N2 C9 H9C 111.4 . . ? C8 C9 H9C 111.4 . . ? N2 C9 H9D 111.4 . . ? C8 C9 H9D 111.4 . . ? H9C C9 H9D 109.2 . . ? O4 C10 N2 121.6(2) . . ? O4 C10 C11 121.1(2) . . ? N2 C10 C11 117.2(2) . . ? C12 C11 C10 111.1(2) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N3 C12 C11 108.7(2) . . ? N3 C12 C18 111.29(19) . . ? C11 C12 C18 113.8(2) . . ? N3 C12 H12 107.6 . . ? C11 C12 H12 107.6 . . ? C18 C12 H12 107.6 . . ? N3 C13 N5 121.1(2) . . ? N3 C13 N4 118.4(2) . . ? N5 C13 N4 120.5(2) . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 O6 126.24(19) . . ? O5 C18 C12 115.2(2) . . ? O6 C18 C12 118.5(2) . . ? O5 Li1 O9 117.5(2) . . ? O5 Li1 O8 106.7(2) . . ? O9 Li1 O8 107.3(2) . . ? O5 Li1 O7 110.3(2) . . ? O9 Li1 O7 109.8(2) . . ? O8 Li1 O7 104.3(2) . . ? H10A O10 H10B 108(3) . . ? H11C O11 H11D 108(3) . . ? 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 C5 N1 C2 C3 -63.8(3) . . . . ? C5 N1 C2 C4 175.9(2) . . . . ? C5 N1 C2 C1 61.6(3) . . . . ? O1 C1 C2 N1 -164.6(2) . . . . ? O2 C1 C2 N1 20.3(3) . . . . ? O1 C1 C2 C3 -39.7(3) . . . . ? O2 C1 C2 C3 145.2(2) . . . . ? O1 C1 C2 C4 80.7(2) . . . . ? O2 C1 C2 C4 -94.3(2) . . . . ? C2 N1 C5 O3 6.9(4) . . . . ? C2 N1 C5 C6 -175.0(2) . . . . ? C10 N2 C6 C5 -72.0(3) . . . . ? C9 N2 C6 C5 112.8(2) . . . . ? C10 N2 C6 C7 169.6(2) . . . . ? C9 N2 C6 C7 -5.5(2) . . . . ? O3 C5 C6 N2 -37.0(3) . . . . ? N1 C5 C6 N2 144.82(19) . . . . ? O3 C5 C6 C7 77.3(3) . . . . ? N1 C5 C6 C7 -100.9(2) . . . . ? N2 C6 C7 C8 -19.5(2) . . . . ? C5 C6 C7 C8 -138.8(2) . . . . ? C6 C7 C8 C9 36.6(2) . . . . ? C10 N2 C9 C8 -146.9(2) . . . . ? C6 N2 C9 C8 28.4(2) . . . . ? C7 C8 C9 N2 -39.1(2) . . . . ? C9 N2 C10 O4 -8.1(3) . . . . ? C6 N2 C10 O4 177.2(2) . . . . ? C9 N2 C10 C11 168.6(2) . . . . ? C6 N2 C10 C11 -6.0(3) . . . . ? O4 C10 C11 C12 -22.4(3) . . . . ? N2 C10 C11 C12 160.9(2) . . . . ? C13 N3 C12 C11 109.3(3) . . . . ? C13 N3 C12 C18 -124.6(2) . . . . ? C10 C11 C12 N3 -68.3(3) . . . . ? C10 C11 C12 C18 167.1(2) . . . . ? C12 N3 C13 N5 30.9(3) . . . . ? C12 N3 C13 N4 -149.5(2) . . . . ? C17 N5 C13 N3 35.4(3) . . . . ? C16 N5 C13 N3 -140.0(2) . . . . ? C17 N5 C13 N4 -144.2(2) . . . . ? C16 N5 C13 N4 40.5(3) . . . . ? C14 N4 C13 N3 16.1(3) . . . . ? C15 N4 C13 N3 -146.4(2) . . . . ? C14 N4 C13 N5 -164.3(2) . . . . ? C15 N4 C13 N5 33.2(3) . . . . ? Li1 O5 C18 O6 -111.0(4) . . . . ? Li1 O5 C18 C12 72.4(5) . . . . ? N3 C12 C18 O5 -179.1(2) . . . . ? C11 C12 C18 O5 -55.8(3) . . . . ? N3 C12 C18 O6 4.0(3) . . . . ? C11 C12 C18 O6 127.3(2) . . . . ? C18 O5 Li1 O9 136.3(4) . . . . ? C18 O5 Li1 O8 -103.2(5) . . . . ? C18 O5 Li1 O7 9.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O1 0.93(3) 1.83(4) 2.753(3) 176(3) 1_545 O7 H7B O6 0.86(4) 1.92(4) 2.768(3) 168(3) 2_546 O8 H8A O2 0.93(4) 1.77(4) 2.698(3) 174(3) 1_545 O8 H8B O6 0.90(4) 1.89(4) 2.770(3) 166(3) 1_545 O9 H9A O2 0.88(4) 2.01(4) 2.861(3) 163(3) 2_546 O9 H9B O7 0.81(4) 2.03(4) 2.813(3) 162(3) 2_546 N1 H1 O10 0.89(3) 2.01(3) 2.889(3) 168(2) 1_545 N3 H3 O2 0.90(3) 2.33(3) 3.167(3) 153(2) . N3 H3 O8 0.90(3) 2.56(3) 3.178(3) 126(2) 1_565 C3 H3C O3 0.98 2.54 3.076(3) 114.4 . C4 H4C O9 0.98 2.54 3.459(3) 155.7 2_556 C6 H6 O1 1.00 2.43 3.358(3) 154.9 1_545 C11 H11B O2 0.99 2.49 3.362(3) 147.1 . C14 H14C O3 0.98 2.51 3.371(3) 146.0 . C16 H16A O5 0.98 2.55 3.429(3) 148.8 2_656 O10 H10A O11 0.89(4) 1.96(4) 2.858(3) 179(3) 1_465 O10 H10B O1 0.84(4) 2.04(4) 2.819(3) 154(3) . O11 H11C O3 0.92(4) 2.10(4) 3.008(3) 167(3) 2_647 O11 H11D O4 0.88(4) 2.00(4) 2.871(3) 172(3) . _refine_diff_density_max 0.179 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.041 _shelx_res_file ; 007-15075.res created by SHELXL-2014/7 TITL BK2-268-F24-45 007-15075 CELL 1.54178 11.543 7.5993 14.3503 90 99.189 90 ZERR 2 0.0008 0.0005 0.001 0 0.004 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Li N O UNIT 36 80 2 10 22 EQIV $1 x, y-1, z HTAB O7 O1_$1 EQIV $2 -x, y-1/2, -z+1 HTAB O7 O6_$2 HTAB O8 O2_$1 HTAB O8 O6_$1 HTAB O9 O2_$2 HTAB O9 O7_$2 HTAB N1 O10_$1 HTAB N3 O2 EQIV $3 x, y+1, z HTAB N3 O8_$3 HTAB C3 O3 EQIV $4 -x, y+1/2, -z+1 HTAB C4 O9_$4 HTAB C6 O1_$1 HTAB C11 O2 HTAB C14 O3 EQIV $5 -x+1, y+1/2, -z+1 HTAB C16 O5_$5 EQIV $6 x-1, y+1, z HTAB O10 O11_$6 HTAB O10 O1 EQIV $7 -x+1, y-1/2, -z+2 HTAB O11 O3_$7 HTAB O11 O4 OMIT 3 -5 13 OMIT 1 -8 0 L.S. 10 SIZE 0.20 0.10 0.06 TEMP -180 BOND $H MORE -1 CONF ACTA WGHT 0.021100 FVAR 0.92533 O1 5 0.093745 0.913017 0.771226 11.00000 0.02845 0.01553 = 0.02320 0.00112 0.00162 0.00264 O2 5 0.154805 0.659090 0.717377 11.00000 0.02568 0.02098 = 0.01641 -0.00017 0.00581 0.00091 O3 5 0.288196 0.546807 0.921719 11.00000 0.01773 0.02007 = 0.02291 -0.00332 0.00066 -0.00374 O4 5 0.491205 0.210275 0.768524 11.00000 0.01611 0.02733 = 0.02127 0.00174 0.00365 0.00256 O5 5 0.201758 0.209620 0.499423 11.00000 0.02346 0.01862 = 0.02180 -0.00289 0.00143 -0.00471 O6 5 0.228654 0.497610 0.482521 11.00000 0.02125 0.01602 = 0.02271 0.00203 0.00140 0.00049 O7 5 0.000033 0.063939 0.601488 11.00000 0.01902 0.02189 = 0.01874 -0.00020 0.00193 0.00019 H7A 2 0.030021 0.008318 0.657760 11.00000 0.04526 H7B 2 -0.071664 0.032438 0.582022 11.00000 0.05482 O8 5 0.203062 -0.175172 0.561763 11.00000 0.02733 0.01912 = 0.02208 0.00184 0.00738 0.00327 H8A 2 0.185291 -0.225426 0.617220 11.00000 0.06812 H8B 2 0.208187 -0.272132 0.527000 11.00000 0.05099 O9 5 0.012257 -0.066587 0.392817 11.00000 0.02495 0.01735 = 0.02216 0.00018 -0.00286 -0.00087 H9A 2 -0.049437 -0.015550 0.359860 11.00000 0.06396 H9B 2 -0.000951 -0.170244 0.383530 11.00000 0.04541 N1 4 0.099506 0.471794 0.864256 11.00000 0.01440 0.01523 = 0.01750 -0.00046 0.00101 -0.00103 H1 2 0.053877 0.382400 0.841651 11.00000 0.01936 N2 4 0.359913 0.211114 0.869215 11.00000 0.01327 0.01965 = 0.01582 0.00032 0.00211 0.00202 N3 4 0.383561 0.525564 0.643245 11.00000 0.01397 0.01405 = 0.02481 -0.00273 0.00180 0.00211 H3 2 0.330840 0.598247 0.663294 11.00000 0.02830 N4 4 0.533077 0.697380 0.719924 11.00000 0.01982 0.01892 = 0.01611 -0.00334 0.00032 -0.00618 N5 4 0.573227 0.487157 0.611691 11.00000 0.01394 0.02177 = 0.01770 -0.00140 0.00262 -0.00203 C1 1 0.107241 0.748751 0.774588 11.00000 0.01439 0.02150 = 0.01488 -0.00128 -0.00388 0.00022 C2 1 0.051035 0.650942 0.850703 11.00000 0.01559 0.01597 = 0.01862 -0.00020 0.00047 0.00158 C3 1 0.064395 0.751960 0.943702 11.00000 0.01945 0.02033 = 0.01813 -0.00028 0.00253 0.00187 AFIX 137 H3A 2 0.034628 0.680129 0.991435 11.00000 -1.50000 H3B 2 0.019666 0.861910 0.934479 11.00000 -1.50000 H3C 2 0.147472 0.778720 0.964919 11.00000 -1.50000 AFIX 0 C4 1 -0.078825 0.629853 0.809559 11.00000 0.01800 0.02520 = 0.02259 -0.00217 0.00284 0.00199 AFIX 137 H4A 2 -0.115676 0.746138 0.800893 11.00000 -1.50000 H4B 2 -0.117878 0.560191 0.852929 11.00000 -1.50000 H4C 2 -0.086143 0.569717 0.748487 11.00000 -1.50000 AFIX 0 C5 1 0.212168 0.436006 0.893837 11.00000 0.01728 0.01995 = 0.01059 0.00043 0.00316 0.00002 C6 1 0.242686 0.239989 0.894164 11.00000 0.01309 0.01964 = 0.01842 0.00103 0.00239 -0.00181 AFIX 13 H6 2 0.182022 0.173731 0.850254 11.00000 -1.20000 AFIX 0 C7 1 0.253597 0.165231 0.995189 11.00000 0.02154 0.02135 = 0.02342 0.00093 0.00503 -0.00027 AFIX 23 H7C 2 0.265943 0.260875 1.042578 11.00000 -1.20000 H7D 2 0.182226 0.098648 1.003467 11.00000 -1.20000 AFIX 0 C8 1 0.360589 0.043749 1.004668 11.00000 0.02286 0.01858 = 0.02045 0.00302 0.00328 0.00001 AFIX 23 H8C 2 0.396490 0.028680 1.071593 11.00000 -1.20000 H8D 2 0.339495 -0.073207 0.976603 11.00000 -1.20000 AFIX 0 C9 1 0.442106 0.141920 0.949728 11.00000 0.01949 0.02051 = 0.01710 0.00216 -0.00153 0.00167 AFIX 23 H9C 2 0.483767 0.238193 0.987727 11.00000 -1.20000 H9D 2 0.500354 0.061738 0.928624 11.00000 -1.20000 AFIX 0 C10 1 0.389020 0.230993 0.782837 11.00000 0.01491 0.01478 = 0.02078 -0.00043 0.00297 -0.00019 C11 1 0.289632 0.270504 0.701578 11.00000 0.01344 0.02263 = 0.01640 -0.00103 0.00111 -0.00050 AFIX 23 H11A 2 0.246674 0.160487 0.681865 11.00000 -1.20000 H11B 2 0.233761 0.353992 0.723324 11.00000 -1.20000 AFIX 0 C12 1 0.337262 0.349404 0.617394 11.00000 0.01611 0.01398 = 0.01928 -0.00272 0.00246 -0.00158 AFIX 13 H12 2 0.404455 0.274482 0.605167 11.00000 -1.20000 AFIX 0 C13 1 0.496982 0.568631 0.657848 11.00000 0.01613 0.01506 = 0.01404 0.00331 -0.00117 0.00123 C14 1 0.459506 0.755927 0.787429 11.00000 0.02514 0.02557 = 0.02339 -0.00653 0.00472 -0.00122 AFIX 137 H14A 2 0.401518 0.840666 0.756962 11.00000 -1.50000 H14B 2 0.508531 0.812042 0.841322 11.00000 -1.50000 H14C 2 0.418955 0.654478 0.809436 11.00000 -1.50000 AFIX 0 C15 1 0.628717 0.817082 0.706846 11.00000 0.02284 0.02266 = 0.02386 -0.00121 0.00105 -0.00759 AFIX 137 H15A 2 0.662994 0.779841 0.651802 11.00000 -1.50000 H15B 2 0.689144 0.814484 0.763183 11.00000 -1.50000 H15C 2 0.597970 0.936968 0.696807 11.00000 -1.50000 AFIX 0 C16 1 0.691770 0.439217 0.658509 11.00000 0.01943 0.03016 = 0.02538 0.00187 0.00108 0.00430 AFIX 137 H16A 2 0.749972 0.508526 0.631623 11.00000 -1.50000 H16B 2 0.705221 0.313678 0.648834 11.00000 -1.50000 H16C 2 0.699110 0.463500 0.726268 11.00000 -1.50000 AFIX 0 C17 1 0.542430 0.428103 0.514035 11.00000 0.02623 0.02206 = 0.02068 -0.00401 0.00687 -0.00429 AFIX 137 H17A 2 0.541856 0.299193 0.512141 11.00000 -1.50000 H17B 2 0.600327 0.472774 0.476856 11.00000 -1.50000 H17C 2 0.464439 0.472714 0.487572 11.00000 -1.50000 AFIX 0 C18 1 0.246529 0.354310 0.525508 11.00000 0.01488 0.01938 = 0.01508 -0.00105 0.00476 0.00022 LI1 3 0.103397 0.017805 0.507855 11.00000 0.02215 0.01989 = 0.02060 -0.00044 0.00015 -0.00149 O10 5 -0.058009 1.178117 0.817763 11.00000 0.02649 0.02191 = 0.03642 -0.00699 0.01121 -0.00434 H10A 2 -0.127712 1.161188 0.836008 11.00000 0.03924 H10B 2 -0.032585 1.080619 0.802766 11.00000 0.04809 O11 5 0.717594 0.128289 0.873949 11.00000 0.01890 0.04688 = 0.02390 -0.00107 0.00199 0.00231 H11C 2 0.713172 0.121212 0.937234 11.00000 0.04792 H11D 2 0.648882 0.163022 0.843951 11.00000 0.05352 HKLF 4 REM BK2-268-F24-45 007-15075 REM R1 = 0.0342 for 3700 Fo > 4sig(Fo) and 0.0519 for all 4336 data REM 370 parameters refined using 1 restraints END WGHT 0.0192 0.0000 REM Highest difference peak 0.179, deepest hole -0.193, 1-sigma level 0.041 Q1 1 0.2381 0.2439 0.4483 11.00000 0.05 0.18 Q2 1 -0.0195 0.6157 0.7208 11.00000 0.05 0.16 Q3 1 -0.1634 -0.0037 0.6399 11.00000 0.05 0.15 Q4 1 0.0780 0.7091 0.8265 11.00000 0.05 0.15 Q5 1 0.0217 0.0829 0.5342 11.00000 0.05 0.14 Q6 1 0.3947 0.7068 0.8485 11.00000 0.05 0.14 Q7 1 0.5752 0.2741 0.7450 11.00000 0.05 0.14 Q8 1 0.7153 0.8359 0.8593 11.00000 0.05 0.14 Q9 1 0.5185 0.4974 0.8232 11.00000 0.05 0.13 Q10 1 0.2008 0.1556 0.4283 11.00000 0.05 0.13 Q11 1 0.7640 0.4464 0.6209 11.00000 0.05 0.13 Q12 1 -0.0818 0.4719 0.7578 11.00000 0.05 0.13 Q13 1 0.5240 0.1529 0.8771 11.00000 0.05 0.13 Q14 1 0.2763 0.1998 1.0244 11.00000 0.05 0.13 Q15 1 0.4640 -0.0295 1.1596 11.00000 0.05 0.13 Q16 1 0.6086 0.3746 0.8206 11.00000 0.05 0.13 Q17 1 0.0562 -0.0902 0.3223 11.00000 0.05 0.13 Q18 1 0.3275 0.0338 1.0756 11.00000 0.05 0.13 Q19 1 0.5980 0.0628 0.8969 11.00000 0.05 0.13 Q20 1 0.4746 0.8160 0.8825 11.00000 0.05 0.13 ; _shelx_res_checksum 27653 _shelx_hkl_file ; 0 0 -1 127.40 20.24 0 0 1 111.42 17.71 0 0 1 110.22 17.84 0 0 -1 106.89 17.22 0 0 1 100.80 18.13 0 0 -1 144.31 24.80 0 0 -1 118.11 18.82 0 0 1 130.13 20.69 0 0 1 125.26 19.93 0 0 -1 133.59 21.24 0 0 1 127.24 20.18 0 0 -1 124.75 19.80 0 0 -1 133.69 21.33 0 0 1 130.75 20.98 0 0 1 120.57 19.31 0 0 -1 121.80 19.51 0 0 1 155.06 137.08 0 0 -2 51.64 8.33 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51.29 0 3 -8 340.57 42.91 0 -3 -8 416.41 52.51 0 -3 8 272.81 66.31 0 3 8 345.63 43.78 0 3 -9 9.76 3.67 0 -3 -9 4.36 2.35 0 -3 9 3.44 4.33 0 3 9 1.87 2.96 0 -3 9 39.47 16.45 0 3 9 13.11 8.78 0 3 -9 7.11 4.65 0 -3 -9 8.02 4.18 0 3 -9 19.38 9.24 0 -3 9 2.95 5.40 0 3 9 23.56 9.29 0 -3 -9 2.00 3.75 0 3 -9 6.98 2.38 0 -3 -9 3.82 1.62 0 -3 9 7.07 3.65 0 3 9 8.20 2.76 0 3 -9 17.35 5.78 0 3 9 8.80 4.05 0 -3 9 -13.89 19.95 0 3 9 5.40 5.33 0 3 -9 6.60 2.16 0 -3 9 13.87 7.85 0 3 9 14.02 8.33 0 3 9 0.75 4.56 0 -3 -9 10.67 3.55 0 3 -9 24.56 7.16 0 3 -9 2.11 4.80 0 3 9 12.05 3.96 0 3 -9 6.60 6.27 0 3 -9 0.27 2.55 0 3 9 15.15 5.31 0 3 -9 6.96 2.24 0 -3 -9 2.85 3.11 0 -3 9 -98.15 74.22 0 3 9 12.09 4.98 0 3 -10 617.29 98.42 0 -3 -10 597.80 95.33 0 -3 10 612.40 97.77 0 3 10 602.27 96.09 0 -3 10 610.82 98.86 0 3 -10 604.40 96.66 0 -3 -10 625.73 99.89 0 3 -10 632.67 101.04 0 -3 10 664.91 106.20 0 3 10 625.69 100.33 0 3 -10 617.25 98.37 0 -3 -10 617.58 98.42 0 -3 10 628.16 100.17 0 3 10 628.04 100.13 0 3 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249.52 23.24 0 4 4 291.46 27.15 0 4 4 280.73 26.29 0 4 -4 272.55 25.24 0 4 4 273.83 25.47 0 4 -4 284.34 26.51 0 4 4 257.52 24.04 0 4 -4 228.41 21.16 0 4 4 265.64 24.75 0 4 -4 238.82 22.33 0 4 4 271.44 25.31 0 4 -4 262.93 24.55 0 4 -4 273.01 25.47 0 4 4 246.28 23.18 0 4 -4 266.86 24.76 0 -4 -4 266.13 24.67 0 4 4 252.28 23.60 0 4 -4 290.44 26.91 0 4 5 104.26 10.40 0 4 -5 106.42 10.04 0 -4 -5 95.91 9.69 0 -4 5 92.38 9.24 0 -4 5 94.08 10.31 0 4 5 115.06 12.49 0 4 5 103.73 10.62 0 4 -5 92.69 9.18 0 -4 -5 107.44 10.35 0 4 -5 106.02 10.93 0 4 5 82.64 9.64 0 4 -5 104.51 10.22 0 -4 -5 98.18 9.82 0 -4 5 106.44 15.15 0 4 -5 98.58 9.16 0 -4 -5 94.37 8.85 0 -4 5 96.66 9.27 0 4 5 119.33 11.75 0 4 5 96.97 10.22 0 4 -5 108.09 10.15 0 4 5 106.57 10.22 0 4 -5 86.48 8.29 0 4 5 103.31 10.13 0 4 -5 97.64 9.22 0 4 5 98.95 10.38 0 4 -5 110.49 10.96 0 4 -5 96.88 9.60 0 -4 5 119.86 13.82 0 4 5 93.75 9.09 0 4 -5 90.98 9.15 0 4 -5 93.38 9.16 0 4 5 106.77 10.44 0 4 -5 101.06 9.65 0 -4 -5 110.86 10.44 0 -4 5 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87.86 23.40 0 5 5 89.75 23.24 0 5 5 90.71 23.07 0 5 -5 87.89 22.49 0 -5 -5 95.20 24.06 0 5 -5 79.37 20.69 0 5 5 77.55 21.49 0 5 -5 89.46 22.44 0 -5 -5 70.98 18.24 0 5 -5 83.37 20.67 0 -5 5 76.55 19.20 0 -5 -5 97.48 24.35 0 5 5 95.66 24.04 0 5 -5 96.78 24.02 0 5 5 94.37 23.60 0 5 -5 90.13 22.58 0 5 5 75.84 19.02 0 5 -5 86.86 21.56 0 5 5 80.38 20.27 0 5 -5 74.86 18.82 0 5 -5 94.93 24.18 0 -5 5 94.00 25.04 0 5 5 87.17 21.78 0 5 -5 90.88 22.91 0 5 -5 97.86 24.60 0 5 5 80.15 20.29 0 5 -5 95.06 23.64 0 -5 -5 93.93 23.36 0 -5 5 126.22 32.13 0 5 5 93.17 23.38 0 5 -6 502.40 84.58 0 -5 6 505.60 85.24 0 -5 6 521.60 88.57 0 5 6 478.30 80.69 0 -5 -6 557.92 94.04 0 5 -6 491.21 83.00 0 -5 6 544.45 91.75 0 5 6 560.72 94.98 0 -5 -6 522.03 88.00 0 -5 6 519.34 87.44 0 -5 -6 547.92 92.24 0 5 6 563.94 94.95 0 5 -6 572.45 96.31 0 5 6 559.34 94.17 0 5 -6 582.71 98.08 0 5 6 495.21 83.53 0 5 -6 539.78 90.82 0 5 6 560.43 94.42 0 5 -6 567.07 95.64 0 5 -6 554.94 93.58 0 -5 6 394.52 68.95 0 5 6 541.85 91.24 0 5 -6 537.14 90.49 0 5 -6 553.42 93.17 0 5 6 516.58 87.08 0 5 -6 569.27 95.78 0 -5 -6 526.92 88.69 0 -5 6 465.65 79.40 0 5 6 503.49 84.78 0 -5 7 364.41 48.15 0 5 7 329.92 43.06 0 -5 -7 311.99 40.36 0 -5 7 357.57 46.20 0 5 7 316.26 41.47 0 -5 -7 371.12 47.98 0 5 -7 354.81 45.55 0 -5 7 364.90 47.00 0 -5 -7 395.74 50.91 0 5 7 437.16 56.29 0 5 -7 430.05 55.24 0 5 7 421.54 54.31 0 5 -7 387.08 49.73 0 5 -7 442.81 56.87 0 5 7 410.34 52.84 0 5 -7 387.32 50.06 0 5 -7 376.01 48.66 0 5 7 400.48 51.55 0 5 -7 384.16 49.55 0 5 -7 403.90 52.04 0 5 7 395.74 50.93 0 5 -7 346.28 44.49 0 -5 -7 394.61 50.80 0 -5 7 168.48 33.06 0 5 7 363.74 46.82 0 -5 8 423.81 72.58 0 5 8 388.25 65.77 0 -5 -8 399.96 67.49 0 5 -8 430.63 72.71 0 5 8 378.12 64.22 0 -5 -8 384.57 64.98 0 5 -8 414.72 69.64 0 -5 8 426.68 71.78 0 -5 -8 432.72 72.75 0 -5 8 445.94 78.95 0 5 -8 459.61 77.18 0 5 8 443.90 74.71 0 5 -8 411.01 69.02 0 5 8 429.54 72.31 0 5 -8 450.74 75.84 0 5 -8 464.96 78.31 0 5 8 402.03 67.58 0 5 -8 446.74 75.35 0 5 -8 441.01 74.11 0 5 8 441.92 74.33 0 5 -8 416.67 69.98 0 -5 -8 418.81 70.38 0 -5 8 436.16 83.44 0 5 8 406.01 68.22 0 -5 9 60.62 23.49 0 -5 -9 83.66 31.87 0 -5 9 52.78 29.71 0 5 9 67.33 25.98 0 5 -9 63.91 24.27 0 5 9 74.69 28.60 0 5 -9 80.09 30.36 0 5 9 92.84 35.44 0 5 -9 79.86 30.47 0 5 -9 86.00 33.11 0 5 9 67.27 25.76 0 5 -9 75.42 29.20 0 5 -9 74.95 28.53 0 5 9 61.77 23.71 0 5 -9 65.09 24.73 0 -5 -9 76.00 29.09 0 5 9 52.64 20.29 0 5 -10 16.80 6.07 0 -5 10 10.38 5.22 0 -5 -10 39.40 14.53 0 -5 10 -5.11 26.87 0 5 10 5.95 5.07 0 -5 10 39.95 17.55 0 5 10 14.44 6.38 0 5 10 19.29 7.35 0 5 -10 15.53 6.73 0 5 -10 13.78 7.45 0 5 10 17.80 6.87 0 5 -10 18.00 8.53 0 5 -10 32.96 11.93 0 5 10 18.51 8.09 0 5 -10 15.65 5.71 0 -5 -10 18.89 7.40 0 -5 10 17.91 84.66 0 5 10 16.71 6.80 0 5 -11 91.46 34.33 0 -5 11 95.37 36.06 0 -5 -11 89.18 33.66 0 -5 11 22.02 25.66 0 5 11 112.26 42.38 0 -5 11 32.04 18.51 0 5 11 50.29 19.36 0 5 11 74.15 28.06 0 5 -11 97.31 36.67 0 5 -11 99.91 38.56 0 5 -11 107.55 40.75 0 5 11 98.40 37.24 0 -5 -11 115.35 43.47 0 -5 11 -112.11 76.40 0 5 -12 10.00 4.85 0 -5 12 -2.73 3.51 0 -5 -12 -2.22 4.75 0 -5 12 -47.07 20.64 0 5 12 6.60 5.05 0 -5 12 35.87 23.89 0 5 12 1.95 5.56 0 -5 -12 -1.33 4.04 0 5 -12 7.53 4.42 0 5 -12 1.60 8.16 0 5 -12 12.76 7.05 0 5 12 6.75 4.67 0 -5 -12 1.44 5.22 0 -5 -13 76.67 33.91 0 -5 13 -14.44 22.49 0 -5 13 90.04 40.15 0 5 13 44.35 19.53 0 -5 -13 69.07 29.98 0 5 14 10.75 7.42 0 -6 0 90.89 17.09 0 6 0 126.84 22.18 0 6 0 93.40 16.60 0 -6 0 132.79 23.75 0 6 0 115.62 19.67 0 6 0 98.42 16.95 0 6 0 122.22 20.80 0 -6 0 89.22 15.53 0 6 0 129.04 21.87 0 6 0 117.84 20.16 0 6 0 105.22 17.95 0 6 0 100.26 17.16 0 -6 -1 113.00 19.82 0 -6 1 97.68 17.49 0 6 1 118.33 20.46 0 6 -1 89.93 16.25 0 6 1 119.13 20.95 0 6 -1 104.77 18.16 0 -6 -1 118.20 21.38 0 -6 1 124.57 22.07 0 6 1 107.57 18.26 0 6 -1 122.17 20.69 0 6 1 110.02 19.04 0 6 -1 101.58 17.44 0 6 1 107.37 18.33 0 6 -1 121.26 20.51 0 -6 -1 122.49 20.95 0 -6 1 118.39 20.33 0 6 -1 137.79 23.76 0 6 1 134.79 22.82 0 6 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37.71 13 2 1 86.44 38.00 -13 2 -1 74.17 32.58 13 3 -2 133.26 43.49 13 3 -1 25.20 16.18 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 53073