data_baran531_a _audit_creation_date 2015-07-22 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2014-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H22 N2 O3' _chemical_formula_sum 'C12 H22 N2 O3' _chemical_formula_weight 242.31 _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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4547(10) _cell_length_b 8.8610(7) _cell_length_c 11.0710(10) _cell_angle_alpha 90 _cell_angle_beta 93.662(3) _cell_angle_gamma 90 _cell_volume 1317.21(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2952 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.333 _cell_measurement_theta_min 2.754 _shelx_estimated_absorpt_T_max 0.978 _shelx_estimated_absorpt_T_min 0.973 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 0.0916 _exptl_absorpt_correction_T_min 0.0669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0528 before and 0.0464 after correction. The Ratio of minimum to maximum transmission is 0.7303. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7814 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.345 _diffrn_reflns_theta_min 2.754 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX CCD' _diffrn_detector_area_resol_mean 8.0 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker X8 APEX Mo' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type fine-focus _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1907 _reflns_number_total 2406 _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 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2008)' _refine_diff_density_max 0.152 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 242 _refine_ls_number_reflns 2406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0395 _refine_ls_restrained_S_all 1.050 _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^)+(0.0428P)^2^+0.2923P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.0951 _refine_special_details ; ? ; _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary ? _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 O1 O 0.80442(7) 0.54909(11) 0.15941(9) 0.0217(3) Uani 1 1 d . . . . . O2 O 0.28567(8) 0.58855(13) 0.45940(9) 0.0259(3) Uani 1 1 d . . . . . O3 O 0.22858(7) 0.56714(11) 0.26021(9) 0.0201(3) Uani 1 1 d . . . . . N1 N 0.60513(8) 0.60190(13) 0.22534(11) 0.0161(3) Uani 1 1 d . . . . . N2 N 0.38914(9) 0.60501(15) 0.30709(11) 0.0224(3) Uani 1 1 d . . . . . C1 C 0.63431(11) 0.62297(18) 0.10126(14) 0.0202(4) Uani 1 1 d . . . . . H1A H 0.6532(12) 0.7320(19) 0.0866(14) 0.025(4) Uiso 1 1 d . . . . . H1B H 0.5769(12) 0.5966(17) 0.0423(14) 0.021(4) Uiso 1 1 d . . . . . C2 C 0.72074(11) 0.51955(19) 0.07734(15) 0.0219(4) Uani 1 1 d . . . . . H2A H 0.7005(11) 0.4140(18) 0.0860(13) 0.016(4) Uiso 1 1 d . . . . . H2B H 0.7430(12) 0.5395(18) -0.0043(16) 0.027(4) Uiso 1 1 d . . . . . C3 C 0.77694(11) 0.53167(19) 0.28142(14) 0.0225(4) Uani 1 1 d . . . . . H3A H 0.7581(11) 0.4232(18) 0.2954(14) 0.023(4) Uiso 1 1 d . . . . . H3B H 0.8371(13) 0.5571(17) 0.3345(14) 0.024(4) Uiso 1 1 d . . . . . C4 C 0.69178(11) 0.63567(18) 0.30804(15) 0.0205(4) Uani 1 1 d . . . . . H4A H 0.7132(12) 0.742(2) 0.2982(14) 0.028(4) Uiso 1 1 d . . . . . H4B H 0.6744(11) 0.6180(17) 0.3916(14) 0.022(4) Uiso 1 1 d . . . . . C5 C 0.47794(11) 0.6644(2) 0.37332(14) 0.0225(4) Uani 1 1 d . . . . . H5A H 0.5138(13) 0.5872(19) 0.4257(15) 0.030(5) Uiso 1 1 d . . . . . H5B H 0.4641(12) 0.7541(19) 0.4244(15) 0.028(4) Uiso 1 1 d . . . . . C6 C 0.52137(10) 0.69949(17) 0.25005(13) 0.0179(3) Uani 1 1 d . . . . . H6 H 0.5373(11) 0.8074(18) 0.2380(13) 0.020(4) Uiso 1 1 d . . . . . C7 C 0.42043(11) 0.64890(18) 0.18749(14) 0.0193(3) Uani 1 1 d . . . . . H7A H 0.3796(11) 0.7305(18) 0.1471(14) 0.020(4) Uiso 1 1 d . . . . . H7B H 0.4246(11) 0.5633(18) 0.1296(14) 0.023(4) Uiso 1 1 d . . . . . C8 C 0.29818(11) 0.58791(16) 0.35157(14) 0.0183(3) Uani 1 1 d . . . . . C9 C 0.12143(10) 0.55347(16) 0.28557(14) 0.0198(4) Uani 1 1 d . . . . . C10 C 0.10524(13) 0.41147(19) 0.35775(17) 0.0259(4) Uani 1 1 d . . . . . H10A H 0.1270(13) 0.321(2) 0.3154(16) 0.035(5) Uiso 1 1 d . . . . . H10B H 0.1417(13) 0.418(2) 0.4398(17) 0.039(5) Uiso 1 1 d . . . . . H10C H 0.0329(14) 0.399(2) 0.3665(15) 0.037(5) Uiso 1 1 d . . . . . C11 C 0.08875(13) 0.6935(2) 0.35067(19) 0.0306(4) Uani 1 1 d . . . . . H11A H 0.1195(15) 0.700(2) 0.436(2) 0.053(6) Uiso 1 1 d . . . . . H11B H 0.1044(14) 0.784(2) 0.3057(17) 0.044(5) Uiso 1 1 d . . . . . H11C H 0.0154(14) 0.689(2) 0.3573(16) 0.039(5) Uiso 1 1 d . . . . . C12 C 0.07191(12) 0.5433(2) 0.15917(16) 0.0297(4) Uani 1 1 d . . . . . H12A H 0.0943(13) 0.451(2) 0.1182(16) 0.037(5) Uiso 1 1 d . . . . . H12B H 0.0883(13) 0.632(2) 0.1114(17) 0.040(5) Uiso 1 1 d . . . . . H12C H -0.0032(15) 0.5373(19) 0.1612(16) 0.037(5) 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 0.0147(5) 0.0250(6) 0.0256(6) 0.0003(5) 0.0036(4) -0.0001(4) O2 0.0227(6) 0.0351(7) 0.0202(6) 0.0006(5) 0.0045(5) -0.0022(5) O3 0.0123(5) 0.0262(6) 0.0218(6) 0.0000(5) 0.0027(4) -0.0025(4) N1 0.0123(6) 0.0178(6) 0.0181(7) 0.0001(5) 0.0014(5) 0.0006(5) N2 0.0159(6) 0.0344(8) 0.0169(7) -0.0022(6) 0.0012(5) -0.0049(6) C1 0.0165(8) 0.0236(9) 0.0206(9) 0.0023(6) 0.0017(7) 0.0018(6) C2 0.0174(8) 0.0252(9) 0.0234(9) -0.0011(7) 0.0033(7) 0.0012(6) C3 0.0154(8) 0.0281(9) 0.0237(9) 0.0013(7) -0.0005(7) 0.0007(6) C4 0.0165(8) 0.0249(9) 0.0199(9) -0.0014(7) 0.0003(6) -0.0016(6) C5 0.0165(8) 0.0308(9) 0.0202(9) -0.0050(7) 0.0018(7) -0.0024(7) C6 0.0157(8) 0.0171(8) 0.0209(8) -0.0022(6) 0.0017(6) 0.0009(6) C7 0.0152(8) 0.0237(9) 0.0192(8) -0.0006(7) 0.0024(6) 0.0015(6) C8 0.0173(8) 0.0154(7) 0.0223(8) -0.0014(6) 0.0024(6) 0.0003(6) C9 0.0104(7) 0.0202(8) 0.0293(9) 0.0007(7) 0.0042(6) -0.0016(6) C10 0.0215(9) 0.0212(9) 0.0353(10) 0.0015(7) 0.0039(8) -0.0030(7) C11 0.0209(9) 0.0215(9) 0.0503(13) -0.0034(8) 0.0083(8) 0.0011(7) C12 0.0162(9) 0.0416(11) 0.0312(10) 0.0059(9) 0.0009(7) -0.0046(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 O1 C2 1.4252(18) . ? O1 C3 1.4314(18) . ? O2 C8 1.2162(17) . ? O3 C8 1.3464(18) . ? O3 C9 1.4913(16) . ? N1 C1 1.4645(18) . ? N1 C4 1.4665(19) . ? N1 C6 1.4602(18) . ? N2 C5 1.460(2) . ? N2 C7 1.4672(19) . ? N2 C8 1.3567(18) . ? C1 H1A 1.014(17) . ? C1 H1B 1.007(16) . ? C1 C2 1.517(2) . ? C2 H2A 0.981(16) . ? C2 H2B 0.986(17) . ? C3 H3A 1.009(16) . ? C3 H3B 0.995(17) . ? C3 C4 1.514(2) . ? C4 H4A 0.993(17) . ? C4 H4B 0.981(15) . ? C5 H5A 1.001(17) . ? C5 H5B 1.000(17) . ? C5 C6 1.550(2) . ? C6 H6 0.991(16) . ? C6 C7 1.551(2) . ? C7 H7A 0.996(16) . ? C7 H7B 0.997(16) . ? C9 C10 1.514(2) . ? C9 C11 1.514(2) . ? C9 C12 1.514(2) . ? C10 H10A 0.983(19) . ? C10 H10B 1.006(19) . ? C10 H10C 0.990(19) . ? C11 H11A 1.00(2) . ? C11 H11B 0.97(2) . ? C11 H11C 0.995(19) . ? C12 H12A 0.994(19) . ? C12 H12B 0.984(19) . ? C12 H12C 1.014(19) . ? 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 O1 C3 109.92(11) . . ? C8 O3 C9 120.26(11) . . ? C1 N1 C4 108.03(11) . . ? C6 N1 C1 110.89(11) . . ? C6 N1 C4 110.76(11) . . ? C5 N2 C7 94.87(11) . . ? C8 N2 C5 125.90(12) . . ? C8 N2 C7 132.43(13) . . ? N1 C1 H1A 110.9(9) . . ? N1 C1 H1B 109.8(8) . . ? N1 C1 C2 109.95(12) . . ? H1A C1 H1B 107.9(12) . . ? C2 C1 H1A 110.1(9) . . ? C2 C1 H1B 108.2(9) . . ? O1 C2 C1 111.15(13) . . ? O1 C2 H2A 109.0(9) . . ? O1 C2 H2B 106.1(10) . . ? C1 C2 H2A 109.8(9) . . ? C1 C2 H2B 109.4(9) . . ? H2A C2 H2B 111.3(13) . . ? O1 C3 H3A 109.3(9) . . ? O1 C3 H3B 106.5(9) . . ? O1 C3 C4 111.25(13) . . ? H3A C3 H3B 109.2(12) . . ? C4 C3 H3A 110.4(9) . . ? C4 C3 H3B 110.1(9) . . ? N1 C4 C3 109.61(12) . . ? N1 C4 H4A 110.5(10) . . ? N1 C4 H4B 109.1(9) . . ? C3 C4 H4A 109.1(9) . . ? C3 C4 H4B 108.4(9) . . ? H4A C4 H4B 110.1(13) . . ? N2 C5 H5A 113.2(10) . . ? N2 C5 H5B 113.3(9) . . ? N2 C5 C6 88.42(11) . . ? H5A C5 H5B 108.4(13) . . ? C6 C5 H5A 116.9(9) . . ? C6 C5 H5B 115.7(9) . . ? N1 C6 C5 112.66(12) . . ? N1 C6 H6 111.7(9) . . ? N1 C6 C7 114.17(12) . . ? C5 C6 H6 114.2(8) . . ? C5 C6 C7 88.09(11) . . ? C7 C6 H6 114.2(9) . . ? N2 C7 C6 88.12(11) . . ? N2 C7 H7A 114.5(9) . . ? N2 C7 H7B 114.2(9) . . ? C6 C7 H7A 115.6(9) . . ? C6 C7 H7B 115.1(9) . . ? H7A C7 H7B 108.4(13) . . ? O2 C8 O3 127.22(13) . . ? O2 C8 N2 122.71(14) . . ? O3 C8 N2 110.05(12) . . ? O3 C9 C10 109.90(12) . . ? O3 C9 C11 109.67(12) . . ? O3 C9 C12 101.80(12) . . ? C10 C9 C11 111.95(14) . . ? C12 C9 C10 111.66(14) . . ? C12 C9 C11 111.39(14) . . ? C9 C10 H10A 111.6(10) . . ? C9 C10 H10B 110.5(10) . . ? C9 C10 H10C 108.5(10) . . ? H10A C10 H10B 109.5(14) . . ? H10A C10 H10C 106.5(14) . . ? H10B C10 H10C 110.1(14) . . ? C9 C11 H11A 112.1(12) . . ? C9 C11 H11B 110.6(11) . . ? C9 C11 H11C 108.8(10) . . ? H11A C11 H11B 110.1(16) . . ? H11A C11 H11C 106.6(15) . . ? H11B C11 H11C 108.6(15) . . ? C9 C12 H12A 110.1(10) . . ? C9 C12 H12B 110.4(11) . . ? C9 C12 H12C 111.3(10) . . ? H12A C12 H12B 109.5(14) . . ? H12A C12 H12C 107.3(14) . . ? H12B C12 H12C 108.2(14) . . ? _shelx_res_file ; TITL Baran531 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.134, Rweak 0.003, Alpha 0.016, Orientation as input REM Formula found by SHELXT: C12 N2 O3 CELL 0.71073 13.4547 8.861 11.071 90 93.662 90 ZERR 4 0.001 0.0007 0.001 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 48 88 8 12 L.S. 10 PLAN 20 SIZE 0.25 0.3 0.32 TEMP -173.15 BOND $H MORE -1 fmap 2 acta 50 REM REM REM WGHT 0.042800 0.292300 FVAR 0.56631 O1 4 0.804418 0.549090 0.159406 11.00000 0.01466 0.02499 = 0.02561 0.00026 0.00364 -0.00011 O2 4 0.285671 0.588555 0.459405 11.00000 0.02266 0.03507 = 0.02025 0.00056 0.00450 -0.00215 O3 4 0.228585 0.567144 0.260207 11.00000 0.01230 0.02623 = 0.02184 -0.00001 0.00267 -0.00255 N1 3 0.605132 0.601901 0.225342 11.00000 0.01235 0.01780 = 0.01810 0.00009 0.00138 0.00065 N2 3 0.389145 0.605007 0.307086 11.00000 0.01594 0.03443 = 0.01686 -0.00220 0.00123 -0.00494 C1 1 0.634312 0.622966 0.101264 11.00000 0.01651 0.02356 = 0.02063 0.00227 0.00170 0.00184 H1A 2 0.653202 0.731960 0.086587 11.00000 0.02453 H1B 2 0.576911 0.596624 0.042271 11.00000 0.02057 C2 1 0.720735 0.519548 0.077338 11.00000 0.01739 0.02517 = 0.02345 -0.00111 0.00335 0.00115 H2A 2 0.700498 0.413999 0.086038 11.00000 0.01625 H2B 2 0.742961 0.539544 -0.004346 11.00000 0.02749 C3 1 0.776940 0.531667 0.281416 11.00000 0.01538 0.02806 = 0.02373 0.00127 -0.00054 0.00065 H3A 2 0.758056 0.423166 0.295443 11.00000 0.02252 H3B 2 0.837084 0.557097 0.334523 11.00000 0.02415 C4 1 0.691782 0.635669 0.308043 11.00000 0.01648 0.02487 = 0.01993 -0.00142 0.00029 -0.00156 H4A 2 0.713192 0.742020 0.298197 11.00000 0.02790 H4B 2 0.674351 0.618011 0.391555 11.00000 0.02176 C5 1 0.477937 0.664436 0.373324 11.00000 0.01651 0.03076 = 0.02018 -0.00499 0.00184 -0.00237 H5A 2 0.513798 0.587204 0.425691 11.00000 0.02958 H5B 2 0.464113 0.754098 0.424423 11.00000 0.02791 C6 1 0.521373 0.699495 0.250054 11.00000 0.01572 0.01713 = 0.02090 -0.00218 0.00172 0.00090 H6 2 0.537328 0.807409 0.237994 11.00000 0.01967 C7 1 0.420432 0.648901 0.187490 11.00000 0.01524 0.02368 = 0.01917 -0.00062 0.00239 0.00147 H7A 2 0.379609 0.730486 0.147118 11.00000 0.01951 H7B 2 0.424565 0.563255 0.129583 11.00000 0.02319 C8 1 0.298176 0.587913 0.351571 11.00000 0.01727 0.01538 = 0.02234 -0.00140 0.00241 0.00027 C9 1 0.121429 0.553467 0.285566 11.00000 0.01036 0.02020 = 0.02928 0.00068 0.00419 -0.00160 C10 1 0.105244 0.411465 0.357753 11.00000 0.02145 0.02123 = 0.03532 0.00150 0.00393 -0.00296 H10A 2 0.127037 0.321015 0.315430 11.00000 0.03548 H10B 2 0.141736 0.417937 0.439775 11.00000 0.03881 H10C 2 0.032905 0.399416 0.366509 11.00000 0.03712 C11 1 0.088748 0.693481 0.350670 11.00000 0.02091 0.02153 = 0.05025 -0.00343 0.00827 0.00112 H11A 2 0.119511 0.699705 0.435540 11.00000 0.05294 H11B 2 0.104414 0.783754 0.305688 11.00000 0.04399 H11C 2 0.015381 0.688960 0.357259 11.00000 0.03928 C12 1 0.071912 0.543327 0.159175 11.00000 0.01621 0.04160 = 0.03121 0.00587 0.00092 -0.00459 H12A 2 0.094271 0.450627 0.118182 11.00000 0.03745 H12B 2 0.088337 0.632493 0.111412 11.00000 0.04047 H12C 2 -0.003241 0.537303 0.161179 11.00000 0.03689 HKLF 4 REM Baran531 in P2(1)/c REM R1 = 0.0395 for 1907 Fo > 4sig(Fo) and 0.0544 for all 2406 data REM 242 parameters refined using 0 restraints END WGHT 0.0428 0.2923 REM Highest difference peak 0.152, deepest hole -0.244, 1-sigma level 0.048 Q1 1 0.5766 0.5155 0.2488 11.00000 0.05 0.15 Q2 1 0.5085 0.6944 0.3203 11.00000 0.05 0.14 Q3 1 0.5620 0.8869 0.2383 11.00000 0.05 0.14 Q4 1 0.4574 0.8008 0.0621 11.00000 0.05 0.13 Q5 1 0.5618 0.6410 0.2449 11.00000 0.05 0.13 Q6 1 0.7026 0.8653 0.3544 11.00000 0.05 0.13 Q7 1 0.7387 0.3109 0.3459 11.00000 0.05 0.13 Q8 1 0.1180 0.5092 0.0964 11.00000 0.05 0.13 Q9 1 0.1199 0.7825 0.3745 11.00000 0.05 0.12 Q10 1 0.6161 0.4004 0.2386 11.00000 0.05 0.12 Q11 1 0.6876 0.3164 0.0941 11.00000 0.05 0.12 Q12 1 0.6818 0.8055 0.0765 11.00000 0.05 0.12 Q13 1 0.3840 0.8448 0.1813 11.00000 0.05 0.12 Q14 1 0.1023 0.4880 0.3300 11.00000 0.05 0.12 Q15 1 0.7170 0.5955 0.5244 11.00000 0.05 0.12 Q16 1 0.6590 0.7890 0.3137 11.00000 0.05 0.11 Q17 1 0.7803 0.4105 0.3369 11.00000 0.05 0.11 Q18 1 0.5949 0.8888 0.3263 11.00000 0.05 0.11 Q19 1 0.5162 0.8813 0.3572 11.00000 0.05 0.11 Q20 1 0.3573 0.5687 0.3217 11.00000 0.05 0.11 ; _shelx_res_checksum 10029 _shelx_hkl_file ; 0 0 1 -7.60 0.40 0 0 -1 -7.10 0.50 0 0 -2 6108.09 224.38 0 0 2 6620.14 224.98 0 0 2 6668.63 225.28 0 0 -2 6705.13 224.88 0 0 -3 0.70 0.90 0 0 3 -1.00 0.90 0 0 3 -0.70 0.90 0 0 -3 -0.40 1.10 0 0 4 103.59 4.90 0 0 -4 106.19 4.90 0 0 -4 99.09 4.80 0 0 4 99.19 4.80 0 0 5 -0.50 1.10 0 0 5 0.00 1.10 0 0 -5 -0.20 0.90 0 0 -5 0.90 1.10 0 0 -6 22.20 2.30 0 0 6 18.90 2.50 0 0 -6 23.10 2.60 0 0 7 -0.50 1.20 0 0 -7 -0.30 1.10 0 0 8 1.10 1.50 0 0 -8 1.40 1.60 0 0 -9 -0.50 1.70 0 0 -10 61.29 5.10 0 0 -11 0.20 2.10 0 0 -12 1.90 2.30 0 0 -13 -1.70 2.10 0 1 0 -2.80 0.40 0 1 0 -3.10 0.30 0 -1 0 -4.00 0.30 0 -1 0 -3.60 0.30 0 1 1 53.69 2.40 0 1 1 49.50 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4 7 36.40 4.10 -2 -4 -7 30.90 3.60 2 -4 7 38.40 3.60 2 4 8 12.90 2.80 2 -4 8 12.00 2.60 -2 -4 -8 13.80 2.80 2 4 9 238.58 11.40 -2 -4 -9 214.78 10.80 2 -4 9 241.28 11.20 2 4 10 6.20 2.70 2 -4 10 -0.50 1.80 -2 -4 -10 2.10 1.80 2 4 11 24.40 4.20 -2 -4 -11 27.30 4.00 2 -4 11 28.00 4.10 2 4 12 -3.90 1.90 2 -4 12 -1.20 2.10 -2 -4 -12 -0.50 2.50 -2 5 11 2.60 2.30 2 -5 -11 2.60 2.50 -2 5 10 54.19 5.30 2 -5 -10 53.09 5.10 -2 5 9 5.60 2.00 2 -5 -9 4.80 2.50 -2 5 8 3.70 2.20 2 -5 -8 -0.80 2.10 2 5 -7 71.59 3.60 -2 5 7 77.29 5.20 2 -5 -7 72.19 5.30 2 5 -6 1.80 0.80 -2 5 6 -1.10 1.70 2 -5 -6 1.60 1.80 -2 5 5 13.70 2.60 2 5 -5 17.80 1.40 -2 -5 5 21.00 2.10 2 -5 -5 10.50 2.40 2 5 -4 54.09 2.70 -2 5 4 63.69 4.50 -2 5 4 62.19 3.90 2 -5 -4 49.90 3.90 -2 -5 4 62.59 3.30 -2 5 3 25.90 2.40 -2 5 3 22.90 2.80 2 5 -3 23.20 1.60 2 -5 -3 26.80 3.10 -2 -5 3 23.40 1.70 -2 5 2 57.89 4.00 2 5 -2 54.49 2.80 -2 5 2 56.99 3.30 -2 -5 2 54.79 2.40 -2 -5 2 51.59 2.50 -2 5 1 284.67 11.20 2 5 -1 268.47 10.20 -2 5 1 271.77 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54.59 5.00 10 -5 -7 46.20 4.70 -10 5 6 -4.20 1.90 10 -5 -6 2.60 2.10 -10 5 5 32.30 4.40 10 -5 -5 28.60 3.60 -10 5 4 26.00 3.70 -10 5 4 31.00 4.30 10 -5 -4 31.00 3.50 -10 5 3 -0.50 1.70 -10 5 3 -0.30 2.00 10 -5 -3 1.90 1.70 10 -5 -3 -0.60 1.90 -10 5 2 84.09 6.30 -10 5 2 77.49 5.70 10 -5 -2 87.99 5.40 10 -5 -2 80.79 5.90 -10 5 1 4.70 2.40 -10 5 1 7.30 2.60 10 -5 -1 11.40 2.60 -10 5 0 12.00 2.80 10 5 0 14.80 1.80 10 -5 0 15.20 3.20 10 5 1 71.49 3.90 -10 5 -1 61.69 5.10 10 -5 1 61.59 5.10 -10 5 -2 -1.20 1.70 10 5 2 2.50 1.30 10 -5 2 2.90 2.30 10 5 3 21.20 2.40 10 -5 3 16.40 3.30 10 5 4 2.70 1.50 10 -5 4 1.00 1.60 10 5 5 40.30 3.60 10 -5 5 30.80 4.30 10 5 6 30.80 3.20 10 -5 6 30.60 4.20 10 5 7 6.80 2.30 10 -5 7 3.70 2.20 -10 6 7 18.40 3.60 10 -6 -7 11.80 3.00 -10 6 6 24.40 4.30 10 -6 -6 16.70 3.20 -10 6 5 0.70 2.50 10 -6 -5 -1.00 1.80 -10 6 4 9.80 3.00 10 -6 -4 8.80 2.40 -10 6 3 -1.70 1.60 -10 6 3 -1.10 2.00 10 -6 -3 -0.20 2.00 10 -6 -3 -0.90 1.70 -10 6 2 70.89 5.60 -10 6 2 48.10 5.10 10 -6 -2 53.69 5.00 10 -6 -2 51.39 4.40 -10 6 1 7.30 2.60 -10 6 1 6.00 2.80 10 -6 -1 6.90 2.50 -10 6 0 56.69 5.20 -10 6 0 58.79 5.00 10 -6 0 58.89 4.90 -10 6 -1 8.70 2.60 10 -6 1 9.50 2.70 -10 6 -2 11.00 2.70 10 -6 2 14.30 2.80 -10 6 -3 101.49 6.60 10 -6 3 86.69 6.50 -10 6 -4 16.20 3.10 10 -6 4 22.40 3.70 10 -6 5 52.79 5.30 10 -6 6 2.40 2.30 -10 7 6 6.90 2.90 10 -7 -6 -0.20 2.10 -10 7 5 24.30 4.20 10 -7 -5 19.80 3.50 -10 7 4 27.50 4.40 10 -7 -4 23.90 3.70 -10 7 3 74.99 6.00 10 -7 -3 74.89 6.10 10 -7 -3 75.29 5.70 -10 7 2 7.90 2.80 -10 7 2 8.50 3.10 10 -7 -2 4.70 2.20 10 -7 -2 11.60 3.10 -10 7 1 1.70 2.30 -10 7 1 10.60 3.10 10 -7 -1 5.90 2.50 -10 7 0 3.10 2.20 -10 7 0 5.10 2.60 10 -7 0 6.80 2.30 -10 7 -1 47.40 4.70 -10 7 -1 42.50 5.20 10 -7 1 42.30 4.90 -10 7 -2 3.90 2.40 10 -7 2 14.90 3.10 -10 7 -3 72.59 5.60 10 -7 3 70.09 5.80 -10 7 -4 19.00 3.30 10 -7 4 15.90 3.40 -10 7 -5 6.80 2.70 10 -7 5 10.10 3.00 -10 8 3 12.80 3.20 10 -8 -3 13.50 3.20 -10 8 2 -0.70 1.70 10 -8 -2 2.70 2.30 10 -8 -2 5.20 2.50 -10 8 1 3.50 2.60 10 -8 -1 6.70 2.60 -10 8 0 4.10 2.80 -10 8 0 6.20 2.60 10 -8 0 0.50 2.10 -10 8 -1 6.60 2.40 -10 8 -1 3.40 2.70 10 -8 1 3.00 2.40 -10 8 -2 28.60 4.50 -10 8 -2 31.50 4.40 10 -8 2 23.70 4.00 11 0 -10 53.99 4.80 11 0 -9 1.40 2.00 -11 0 9 -2.00 2.40 -11 0 8 28.20 3.40 11 0 -8 28.90 3.30 11 0 -7 0.00 1.40 -11 0 7 -4.00 1.30 -11 0 6 7.90 2.40 11 0 -6 4.70 1.70 -11 0 6 10.90 2.30 -11 0 5 -0.20 1.80 -11 0 5 0.80 1.50 11 0 -5 -0.90 1.10 -11 0 4 51.49 4.40 -11 0 4 50.69 3.90 11 0 -4 42.70 2.80 11 0 -3 -1.30 1.60 -11 0 3 -0.70 1.60 11 0 -3 -0.20 0.70 11 0 -2 37.50 4.00 11 0 -2 41.90 1.80 11 0 -1 0.50 1.80 11 0 0 1.00 1.90 11 0 1 -0.50 1.60 11 0 2 1671.83 60.09 11 0 3 1.50 1.90 11 0 3 0.20 0.60 11 0 4 684.83 26.60 11 0 5 0.80 1.90 11 0 6 19.60 3.40 11 0 7 -2.70 1.80 11 0 8 23.40 4.00 11 0 9 3.20 2.40 -11 1 10 -0.40 1.90 11 1 -10 1.90 1.90 11 -1 -10 4.10 2.30 11 1 -9 42.30 4.10 -11 1 9 37.40 4.20 11 -1 -9 41.80 3.90 11 1 -8 11.60 2.20 -11 1 8 14.60 3.00 11 -1 -8 11.90 2.60 11 1 -7 23.80 2.80 -11 1 7 25.10 3.50 -11 -1 7 26.90 3.10 -11 -1 7 24.30 3.40 11 -1 -7 26.20 3.10 -11 1 6 13.70 2.60 11 1 -6 9.80 1.90 -11 1 6 7.90 2.60 -11 -1 6 7.10 2.30 11 -1 -6 10.80 2.00 -11 -1 6 2.90 1.60 -11 1 5 0.90 1.60 -11 1 5 0.60 1.50 -11 -1 5 1.00 1.40 11 -1 -5 3.50 1.50 -11 -1 5 -2.40 1.40 -11 1 4 22.50 3.50 -11 1 4 22.60 3.10 -11 -1 4 20.90 3.10 11 -1 -4 18.90 2.10 -11 -1 4 24.60 2.90 -11 1 3 12.70 2.80 -11 1 3 12.40 2.50 11 1 -3 12.00 2.40 11 -1 -3 7.00 2.40 11 -1 -3 16.10 1.80 11 1 -2 45.50 3.90 11 -1 -2 46.80 2.60 11 -1 -2 49.99 4.10 11 1 -1 9.80 2.40 11 -1 -1 6.80 1.00 11 -1 -1 5.00 2.10 11 1 0 9.60 2.10 11 -1 0 5.60 2.30 11 -1 0 7.30 1.00 11 1 1 64.39 4.50 11 -1 1 57.59 2.80 11 -1 1 55.89 2.70 11 -1 1 71.29 5.10 11 1 2 95.19 5.80 11 -1 2 102.99 6.30 11 -1 2 89.19 4.10 11 1 3 131.79 7.20 11 -1 3 138.69 7.70 11 -1 3 126.09 5.60 11 1 4 23.20 3.20 11 -1 4 29.10 3.60 11 1 5 0.10 1.90 11 -1 5 0.50 1.50 11 1 6 0.50 1.90 11 -1 6 1.30 2.20 11 1 7 46.60 4.70 11 -1 7 35.70 4.50 11 1 8 17.50 3.40 11 -1 8 11.00 3.10 11 1 9 1.50 2.40 11 -1 9 2.10 2.40 -11 2 10 -0.20 2.20 11 -2 -10 -2.40 2.00 -11 2 9 -0.20 2.00 11 -2 -9 -1.70 1.80 -11 2 8 82.39 5.90 11 -2 -8 80.09 5.50 -11 2 7 -1.40 1.70 11 -2 -7 -0.90 1.40 -11 -2 7 -1.90 1.30 -11 2 6 2.90 2.10 -11 2 6 3.00 2.40 11 -2 -6 2.30 1.50 -11 -2 6 2.70 1.70 -11 2 5 1.40 2.20 -11 2 5 8.30 2.50 -11 -2 5 4.80 1.50 -11 -2 5 5.60 2.10 11 -2 -5 7.80 1.80 -11 2 4 2.20 1.80 -11 2 4 1.90 1.90 11 -2 -4 4.10 1.50 11 -2 -4 2.50 2.20 -11 -2 4 3.10 1.90 -11 -2 4 2.60 1.30 -11 2 3 22.10 3.40 -11 2 3 27.50 3.80 11 -2 -3 25.60 2.40 11 -2 -3 26.50 3.70 11 2 -2 0.20 1.30 -11 2 2 1.20 1.60 11 -2 -2 0.60 1.90 11 -2 -2 0.80 1.10 11 2 -1 1.60 1.50 11 -2 -1 1.50 1.10 11 -2 -1 1.00 2.00 11 2 0 4.30 1.70 11 -2 0 7.80 1.30 11 -2 0 4.90 2.30 11 2 1 339.17 14.00 11 -2 1 334.77 14.70 11 2 2 356.26 14.70 11 -2 2 363.66 15.40 11 -2 2 346.07 13.50 11 2 3 531.15 21.20 11 -2 3 571.04 22.00 11 -2 3 528.45 20.50 11 2 4 149.39 7.80 11 -2 4 126.69 7.80 11 2 5 59.79 4.80 11 -2 5 72.59 5.70 11 2 6 26.90 3.60 11 -2 6 23.20 3.90 11 2 7 2.20 2.10 11 -2 7 -0.20 1.50 11 2 8 -0.60 1.90 11 -2 8 -0.50 2.30 -11 3 9 16.80 3.30 11 -3 -9 16.30 3.20 -11 3 8 2.10 2.40 11 -3 -8 2.80 2.10 -11 3 7 2.80 2.30 11 -3 -7 12.00 2.60 -11 3 6 -0.30 2.20 -11 3 6 -1.70 1.90 11 -3 -6 -1.10 1.30 -11 -3 6 -0.50 1.20 -11 3 5 118.79 7.70 -11 3 5 117.49 7.40 11 -3 -5 129.19 6.40 -11 -3 5 115.89 6.40 -11 3 4 147.49 8.40 -11 3 4 151.38 8.70 11 -3 -4 148.29 7.20 -11 -3 4 143.79 7.00 11 -3 -4 146.49 8.60 -11 -3 4 157.28 7.60 -11 3 3 190.28 10.00 -11 3 3 195.08 10.20 11 -3 -3 182.58 9.80 11 -3 -3 198.68 8.50 -11 3 2 45.20 4.50 11 3 -2 39.80 3.60 11 -3 -2 41.30 3.20 11 -3 -2 42.90 4.60 -11 3 1 15.80 3.10 11 3 -1 21.90 2.70 11 -3 -1 11.50 2.00 11 -3 -1 9.60 2.90 11 3 0 -0.30 1.30 11 -3 0 0.50 1.20 11 -3 0 -0.30 1.90 11 3 1 18.90 2.60 11 -3 1 25.20 3.40 11 3 2 144.49 7.10 11 -3 2 127.79 7.80 11 3 3 11.80 2.30 11 -3 3 7.80 2.30 11 3 4 0.20 1.50 11 -3 4 -2.90 1.70 11 3 5 1.40 1.70 11 -3 5 3.30 1.90 11 3 6 16.60 3.10 11 -3 6 14.50 2.90 11 3 7 8.50 2.40 11 -3 7 2.40 2.20 11 3 8 10.10 2.80 11 -3 8 15.00 3.40 -11 4 8 21.90 4.00 11 -4 -8 28.00 3.60 -11 4 7 26.60 4.20 11 -4 -7 32.10 3.70 -11 4 6 28.90 4.30 11 -4 -6 20.90 3.20 -11 4 5 22.40 3.70 -11 4 5 20.40 3.70 -11 -4 5 20.00 2.70 11 -4 -5 19.10 2.80 -11 4 4 13.00 2.90 -11 4 4 7.80 2.90 11 -4 -4 9.70 2.90 -11 -4 4 13.30 2.30 11 -4 -4 12.90 2.30 -11 4 3 4.90 2.50 -11 4 3 4.80 2.50 11 -4 -3 2.40 2.00 11 -4 -3 1.30 1.60 -11 4 2 1.90 2.20 -11 4 2 2.10 2.30 11 -4 -2 -2.60 1.90 11 -4 -2 -1.50 1.40 -11 4 1 1.30 1.60 11 4 -1 3.80 1.40 11 -4 -1 5.60 2.40 11 -4 -1 4.60 1.60 11 4 0 23.70 2.60 -11 4 0 25.70 3.80 11 -4 0 24.90 3.80 11 4 1 143.99 6.70 11 -4 1 129.69 7.70 11 4 2 96.19 5.30 11 -4 2 86.09 6.00 11 4 3 177.18 8.30 11 -4 3 172.78 9.50 11 4 4 10.70 2.30 11 -4 4 9.20 2.90 11 4 5 84.29 5.50 11 -4 5 83.99 6.40 11 4 6 2.30 2.00 11 -4 6 3.30 2.40 11 4 7 53.79 4.60 11 -4 7 42.40 4.50 -11 5 8 8.20 3.40 11 -5 -8 15.50 3.10 -11 5 7 51.49 5.80 11 -5 -7 52.19 4.90 -11 5 6 21.00 3.90 11 -5 -6 25.70 3.40 -11 5 5 4.40 2.70 11 -5 -5 6.10 2.10 -11 5 4 135.09 8.60 -11 5 4 152.98 8.80 11 -5 -4 147.09 7.70 -11 5 3 14.60 3.30 -11 5 3 7.40 2.80 11 -5 -3 5.90 2.20 11 -5 -3 4.50 2.50 -11 5 2 17.30 3.20 -11 5 2 30.70 4.50 11 -5 -2 25.30 3.60 11 -5 -2 19.90 2.80 -11 5 1 28.10 4.20 -11 5 1 24.70 4.00 11 -5 -1 35.00 4.40 11 -5 -1 34.00 3.60 -11 5 0 2.20 2.10 11 5 0 5.00 1.30 11 -5 0 4.10 2.30 -11 5 -1 56.79 4.80 11 5 1 62.19 3.80 11 -5 1 53.19 5.10 -11 5 -2 13.70 3.00 11 5 2 17.90 2.20 11 -5 2 16.50 3.20 11 5 3 20.60 2.50 11 -5 3 14.20 3.20 11 5 4 -1.40 1.20 11 -5 4 -0.50 2.10 11 5 5 -0.30 1.50 11 -5 5 3.00 2.30 11 5 6 3.10 1.70 11 -5 6 4.10 2.60 -11 6 6 1.50 2.50 11 -6 -6 -1.70 1.80 -11 6 5 37.70 5.10 11 -6 -5 53.69 4.60 -11 6 4 9.30 3.10 11 -6 -4 4.20 2.40 -11 6 3 2.80 2.50 -11 6 3 -0.70 2.20 11 -6 -3 1.40 1.70 11 -6 -3 0.10 1.70 -11 6 2 4.90 2.60 -11 6 2 4.80 2.70 11 -6 -2 4.50 2.40 11 -6 -2 6.50 2.10 -11 6 1 6.60 2.30 -11 6 1 3.80 2.50 11 -6 -1 8.20 2.70 11 -6 -1 5.60 2.30 -11 6 0 2.80 1.90 11 -6 0 4.20 2.50 -11 6 -1 3.90 2.30 11 -6 1 0.30 2.10 -11 6 -2 65.69 5.40 11 -6 2 46.10 5.00 -11 6 -3 22.20 3.60 11 -6 3 20.70 3.80 -11 6 -4 36.60 4.70 11 -6 4 34.50 4.60 11 -6 5 34.00 4.60 -11 7 4 2.80 2.70 11 -7 -4 0.50 1.90 -11 7 3 7.50 2.50 11 -7 -3 3.80 2.30 11 -7 -3 0.50 2.30 -11 7 2 2.10 2.40 -11 7 2 2.40 2.40 11 -7 -2 -1.30 2.10 11 -7 -2 1.20 2.10 -11 7 1 -1.10 2.00 -11 7 1 6.10 2.90 11 -7 -1 -3.20 1.90 11 -7 -1 2.00 2.20 -11 7 0 15.50 3.70 -11 7 0 27.80 4.10 11 -7 0 29.00 4.30 -11 7 -1 33.70 4.50 -11 7 -1 31.80 4.30 11 -7 1 29.70 4.30 -11 7 -2 3.70 2.50 11 -7 2 1.20 2.20 -11 7 -3 4.50 2.30 11 -7 3 2.60 2.30 12 0 -9 1.20 1.70 12 0 -8 24.90 3.10 -12 0 8 26.90 3.80 -12 0 7 0.10 1.30 -12 0 7 2.30 1.90 12 0 -7 2.60 1.60 -12 0 6 32.70 3.40 -12 0 6 33.80 4.20 12 0 -6 39.10 3.10 12 0 -5 -0.70 1.10 -12 0 5 -1.10 1.80 -12 0 5 0.40 1.40 -12 0 4 9.90 2.30 12 0 -4 12.30 1.50 -12 0 4 12.30 2.80 12 0 -3 0.50 1.70 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3.90 12 -2 1 43.50 4.50 12 -2 1 38.70 2.60 12 2 2 77.19 5.20 12 -2 2 84.49 6.00 12 2 3 28.90 3.40 12 -2 3 23.10 3.60 12 2 4 -1.90 1.40 12 -2 4 -0.40 2.00 12 2 5 0.50 1.90 12 -2 5 -0.90 1.50 12 2 6 2.40 2.10 12 -2 6 0.10 2.00 12 2 7 3.20 2.40 12 -2 7 0.20 2.20 -12 3 8 62.29 5.50 12 -3 -8 56.49 4.80 -12 3 7 4.10 2.40 12 -3 -7 -0.60 1.80 -12 3 6 67.99 5.80 -12 3 6 73.89 6.20 -12 -3 6 83.69 5.20 12 -3 -6 73.69 4.80 -12 3 5 17.30 3.50 -12 3 5 13.40 3.10 -12 -3 5 14.60 2.70 12 -3 -5 12.80 2.30 -12 3 4 122.59 7.80 -12 3 4 129.29 8.30 12 -3 -4 137.39 8.10 -12 -3 4 152.18 7.50 12 -3 -4 128.19 6.50 -12 3 3 9.10 2.90 -12 3 3 7.00 2.80 12 -3 -3 4.00 2.50 12 -3 -3 10.50 1.80 12 3 -2 1.40 1.70 -12 3 2 1.60 1.70 12 -3 -2 0.60 1.70 12 -3 -2 -0.20 1.20 -12 3 1 33.30 4.40 12 3 -1 46.40 3.80 12 -3 -1 47.00 4.80 12 -3 -1 41.70 3.20 12 3 0 106.09 6.20 12 -3 0 118.89 7.20 12 -3 0 117.59 5.60 12 3 1 29.20 3.30 12 -3 1 27.10 3.80 12 3 2 107.69 5.90 12 -3 2 91.59 6.30 12 3 3 10.20 2.50 12 -3 3 5.10 2.50 12 3 4 -0.40 1.50 12 -3 4 0.50 2.10 12 3 5 -1.10 1.80 12 -3 5 -1.20 1.40 12 3 6 22.20 3.30 12 -3 6 12.90 2.90 12 3 7 18.40 3.20 12 -3 7 24.50 4.10 -12 4 8 23.20 4.10 12 -4 -8 28.00 3.70 -12 4 7 7.30 2.90 12 -4 -7 8.40 2.50 -12 4 6 -0.20 2.10 12 -4 -6 1.40 1.60 -12 4 5 5.50 2.60 -12 4 5 -1.60 1.50 12 -4 -5 0.50 1.70 -12 4 4 3.70 2.10 -12 4 4 7.10 2.80 -12 -4 4 3.50 1.80 12 -4 -4 2.20 2.50 12 -4 -4 3.60 1.80 -12 4 3 2.90 2.30 -12 4 3 4.40 2.40 12 -4 -3 0.70 1.50 12 -4 -3 -1.70 1.90 -12 4 2 5.20 2.20 -12 4 2 4.60 2.40 12 -4 -2 6.10 1.80 12 -4 -2 4.80 2.50 12 4 -1 45.30 3.70 -12 4 1 61.39 5.40 12 -4 -1 54.99 5.20 12 -4 -1 51.29 3.70 -12 4 0 0.60 2.10 12 4 0 10.20 2.10 12 -4 0 9.60 2.00 12 -4 0 6.90 2.70 12 4 1 165.38 7.70 12 -4 1 153.68 9.10 12 4 2 27.20 3.00 12 -4 2 24.50 3.80 12 4 3 1.00 1.40 12 -4 3 4.90 2.40 12 4 4 41.50 3.60 12 -4 4 31.00 4.40 12 4 5 4.00 1.80 12 -4 5 0.00 2.20 12 4 6 23.60 3.30 12 -4 6 19.20 3.70 -12 5 7 29.00 4.60 12 -5 -7 19.40 3.30 -12 5 6 18.80 3.90 12 -5 -6 17.20 3.20 -12 5 5 4.90 2.90 -12 5 5 -0.40 2.30 12 -5 -5 0.80 1.80 -12 5 4 0.80 2.20 -12 5 4 -0.10 2.10 12 -5 -4 2.90 1.70 -12 5 3 10.30 3.20 -12 5 3 9.40 3.00 12 -5 -3 11.50 2.30 12 -5 -3 11.80 3.20 -12 5 2 18.00 3.40 -12 5 2 16.80 3.50 12 -5 -2 11.20 2.30 12 -5 -2 14.00 3.20 -12 5 1 8.90 3.00 -12 5 1 8.40 3.00 12 -5 -1 8.20 2.20 12 -5 -1 14.90 3.20 -12 5 0 43.40 5.10 12 -5 0 52.09 5.10 -12 5 -1 48.70 4.60 12 -5 1 49.30 5.00 -12 5 -2 20.10 3.60 12 -5 2 32.30 4.30 12 -5 3 57.19 5.00 12 -5 4 1.70 2.30 12 -5 5 9.30 2.80 -12 6 5 -1.50 2.50 12 -6 -5 0.60 1.90 -12 6 4 7.60 3.20 -12 6 4 2.50 2.60 12 -6 -4 5.60 2.20 -12 6 3 8.50 3.20 -12 6 3 8.00 2.90 12 -6 -3 6.80 2.40 12 -6 -3 5.50 2.40 -12 6 2 5.60 2.80 -12 6 2 2.90 2.70 12 -6 -2 1.70 1.90 12 -6 -2 3.60 1.90 -12 6 1 5.60 2.70 -12 6 1 3.70 2.10 12 -6 -1 5.60 2.80 12 -6 -1 6.80 2.10 -12 6 0 56.19 5.60 12 -6 0 63.39 5.80 -12 6 -1 19.80 3.70 12 -6 1 20.30 3.80 -12 6 -2 4.60 2.50 12 -6 2 4.10 2.60 -12 6 -3 91.99 6.60 12 -6 3 86.59 6.70 -12 6 -4 14.60 3.30 12 -6 4 16.80 3.70 -12 7 2 -5.70 1.90 -12 7 2 3.50 2.60 12 -7 -2 3.50 2.20 12 -7 -2 2.40 2.40 -12 7 1 2.10 2.40 -12 7 1 0.70 2.50 12 -7 -1 -3.20 1.90 12 -7 -1 1.90 2.20 -12 7 0 -0.90 2.00 -12 7 0 -2.50 2.10 12 -7 0 -2.90 2.10 -12 7 -1 11.00 3.20 -12 7 -1 11.70 3.30 12 -7 1 13.00 3.50 -13 0 7 -0.50 1.80 -13 0 7 -1.20 1.80 -13 0 6 1.20 2.00 -13 0 6 0.70 1.50 -13 0 5 -0.30 2.00 -13 0 5 0.40 1.80 -13 0 4 210.78 11.00 -13 0 4 232.28 10.70 13 0 -3 0.40 1.90 -13 0 3 2.00 2.20 13 0 -2 106.29 6.70 13 0 -1 -3.50 1.50 13 0 0 69.09 5.40 13 0 1 -0.50 1.80 13 0 2 131.69 7.70 13 0 3 1.50 2.00 13 0 4 10.60 2.80 13 0 5 0.60 2.10 13 0 6 25.30 4.00 13 0 7 1.90 2.20 -13 1 8 0.80 2.30 -13 1 7 4.20 2.00 -13 1 7 0.80 2.20 -13 -1 7 5.50 2.20 -13 1 6 10.10 2.60 -13 1 6 10.00 3.00 -13 -1 6 10.80 2.90 -13 1 5 93.69 6.20 -13 1 5 104.09 7.00 -13 -1 5 94.09 5.60 -13 -1 5 95.19 6.40 -13 1 4 240.08 11.60 -13 1 4 258.67 12.40 -13 -1 4 250.17 11.10 13 -1 -4 246.38 12.10 -13 -1 4 249.08 11.90 13 1 -3 144.69 8.20 -13 1 3 161.18 9.00 -13 1 3 167.08 8.80 -13 -1 3 150.98 8.40 13 -1 -3 154.28 8.80 13 1 -2 113.39 6.70 -13 1 2 98.39 7.10 13 -1 -2 119.99 7.30 13 1 -1 9.40 2.50 13 -1 -1 11.50 2.90 13 1 0 -0.50 1.60 13 -1 0 0.00 1.60 13 1 1 24.70 3.40 13 -1 1 16.90 3.20 13 1 2 27.50 3.60 13 -1 2 29.50 3.90 13 1 3 4.70 2.20 13 -1 3 2.10 2.30 13 1 4 2.20 2.00 13 -1 4 4.40 2.20 13 1 5 -2.50 1.70 13 -1 5 -1.90 1.90 13 1 6 6.20 2.40 13 -1 6 4.10 2.60 13 1 7 17.60 3.40 13 -1 7 26.70 4.20 -13 2 8 16.20 3.20 13 -2 -8 8.60 2.90 -13 2 7 10.20 2.90 13 -2 -7 13.00 2.80 -13 -2 7 11.90 2.40 -13 2 6 1.10 2.30 -13 2 6 5.50 2.50 13 -2 -6 4.20 1.80 -13 -2 6 3.80 2.10 -13 2 5 2.90 2.20 -13 2 5 6.30 2.40 13 -2 -5 2.80 1.50 -13 -2 5 2.60 2.00 -13 2 4 54.69 5.00 -13 2 4 60.29 5.20 13 -2 -4 52.29 5.40 13 -2 -4 56.89 3.70 -13 -2 4 54.69 4.60 -13 2 3 59.39 5.20 -13 2 3 53.69 5.20 13 -2 -3 58.09 3.90 13 -2 -3 54.29 5.20 -13 2 2 -0.20 2.10 13 2 -2 2.50 1.70 13 -2 -2 -1.10 1.90 13 2 -1 26.20 3.30 13 -2 -1 23.00 3.70 13 2 0 -0.30 1.70 13 -2 0 -0.20 2.10 13 2 1 201.18 9.80 13 -2 1 207.38 10.60 13 2 2 72.59 5.20 13 -2 2 77.39 6.00 13 2 3 7.10 2.30 13 -2 3 7.80 2.80 13 2 4 1.00 1.80 13 -2 4 -2.00 2.10 13 2 5 6.20 2.40 13 -2 5 14.30 3.00 13 2 6 0.40 2.00 13 -2 6 0.40 1.80 -13 3 7 1.60 2.20 13 -3 -7 0.20 1.70 -13 3 6 23.60 3.90 -13 3 6 26.80 4.40 13 -3 -6 31.00 3.30 -13 3 5 158.98 9.10 -13 3 5 154.08 9.30 -13 -3 5 155.68 8.30 13 -3 -5 158.48 7.60 -13 3 4 34.50 4.40 -13 3 4 29.10 4.50 -13 -3 4 35.00 3.60 13 -3 -4 35.60 3.20 13 -3 -4 30.30 4.50 -13 3 3 120.79 7.90 -13 3 3 107.69 7.50 13 -3 -3 121.59 7.80 13 -3 -3 119.09 6.00 -13 3 2 36.70 4.60 13 3 -2 39.60 3.90 13 -3 -2 45.10 3.20 13 -3 -2 36.50 4.80 13 3 -1 -2.80 1.50 -13 3 1 -0.60 2.00 13 -3 -1 -2.50 1.80 13 -3 -1 -0.90 1.10 13 3 0 34.10 3.60 13 -3 0 36.20 2.90 13 -3 0 39.00 4.70 13 3 1 6.10 2.10 13 -3 1 8.80 2.90 13 -3 1 1.40 1.90 13 3 2 41.90 3.70 13 -3 2 28.50 4.00 13 3 3 2.60 1.70 13 -3 3 0.50 2.10 13 3 4 23.90 3.30 13 -3 4 27.00 4.00 13 3 5 3.90 2.40 13 -3 5 3.50 2.50 13 3 6 18.20 3.30 13 -3 6 13.60 3.50 -13 4 6 4.60 2.60 13 -4 -6 3.40 2.00 -13 4 5 23.90 4.10 -13 4 5 24.50 4.20 13 -4 -5 30.00 3.50 -13 4 4 7.00 2.90 -13 4 4 4.30 2.70 13 -4 -4 1.60 1.70 13 -4 -4 7.00 3.00 -13 -4 4 4.60 1.80 -13 4 3 2.60 2.50 -13 4 3 1.80 2.40 13 -4 -3 2.80 2.50 13 -4 -3 2.20 1.70 -13 4 2 4.80 2.60 -13 4 2 0.20 1.70 13 -4 -2 2.70 2.40 13 -4 -2 4.50 1.70 13 4 -1 8.50 2.10 -13 4 1 3.10 2.10 13 -4 -1 8.80 2.80 13 -4 -1 7.40 1.90 -13 4 0 25.30 3.80 13 4 0 28.50 3.20 13 -4 0 22.30 3.80 13 -4 0 25.40 2.80 13 4 1 108.19 5.80 -13 4 -1 88.29 6.80 13 -4 1 95.39 6.60 13 4 2 14.00 2.50 13 -4 2 11.60 3.00 13 4 3 47.80 4.20 13 -4 3 54.29 5.20 13 4 4 1.50 1.60 13 -4 4 -2.30 1.80 13 4 5 1.60 1.80 13 -4 5 1.60 2.50 -13 5 5 7.30 3.00 -13 5 5 9.60 3.00 13 -5 -5 9.80 2.40 -13 5 4 71.79 6.20 -13 5 4 56.19 5.40 13 -5 -4 60.09 4.70 -13 5 3 2.80 2.10 -13 5 3 4.00 2.80 13 -5 -3 5.50 2.80 13 -5 -3 1.60 1.80 -13 5 2 2.30 2.40 -13 5 2 3.60 2.10 13 -5 -2 2.50 2.40 13 -5 -2 1.00 1.80 -13 5 1 2.10 2.40 -13 5 1 1.40 2.40 13 -5 -1 0.00 1.70 13 -5 -1 0.10 1.50 -13 5 0 48.00 5.00 13 -5 0 33.00 3.40 13 -5 0 35.40 4.90 -13 5 -1 11.60 3.20 13 -5 1 17.90 3.40 -13 5 -2 -0.40 1.70 13 -5 2 3.20 2.50 13 -5 3 10.30 2.70 13 -5 4 0.10 2.20 -13 6 3 1.70 2.80 -13 6 3 6.60 3.10 13 -6 -3 3.80 2.00 13 -6 -3 11.00 3.30 -13 6 2 -0.10 2.40 -13 6 2 -0.50 2.10 13 -6 -2 -1.50 1.70 13 -6 -2 -1.80 2.00 -13 6 1 -2.40 1.40 -13 6 1 -1.30 2.10 13 -6 -1 0.50 1.80 13 -6 -1 1.80 1.60 -13 6 0 10.00 3.30 -13 6 0 11.10 3.30 13 -6 0 6.80 2.40 13 -6 0 11.00 3.30 -13 6 -1 18.90 3.80 13 -6 1 20.20 3.90 -13 6 -2 18.80 3.80 13 -6 2 27.30 4.20 -14 0 7 3.00 2.20 -14 0 6 16.20 3.60 -14 0 6 6.10 2.70 -14 0 5 -1.40 1.40 -14 0 5 -0.60 2.00 -14 0 4 28.20 4.10 -14 0 4 20.10 3.20 14 0 -3 -2.80 1.70 -14 0 3 1.40 2.30 14 0 -2 82.59 5.90 14 0 -1 0.00 1.90 14 0 0 16.00 3.00 14 0 1 0.20 1.80 14 0 2 17.00 3.10 14 0 3 -1.40 1.70 14 0 4 -0.60 1.90 14 0 5 -0.90 2.10 -14 1 7 -1.20 1.70 -14 1 7 -2.70 2.30 -14 -1 7 0.50 1.70 -14 1 6 1.50 2.30 -14 1 6 2.60 2.30 -14 -1 6 -2.60 1.70 -14 1 5 23.00 3.90 -14 1 5 22.70 3.50 -14 -1 5 13.20 3.20 -14 1 4 31.90 4.10 -14 1 4 26.50 4.20 -14 -1 4 27.60 3.40 -14 -1 4 29.40 4.20 -14 1 3 39.00 4.90 -14 1 3 38.80 4.60 14 1 -3 45.40 4.50 14 -1 -3 49.00 4.90 -14 -1 3 36.00 4.60 14 1 -2 22.60 3.40 -14 1 2 26.60 4.20 14 -1 -2 33.70 4.30 14 1 -1 39.40 4.30 14 -1 -1 33.00 4.10 14 1 0 4.80 2.40 14 -1 0 4.00 2.30 14 1 1 0.30 1.80 14 -1 1 1.40 2.10 14 1 2 0.60 1.70 14 -1 2 1.10 2.00 14 1 3 53.79 4.90 14 -1 3 57.29 5.20 14 1 4 2.70 2.20 14 -1 4 0.50 2.20 14 1 5 3.20 2.30 14 -1 5 -1.10 2.10 -14 2 6 -0.50 2.10 -14 2 6 -0.60 2.40 -14 -2 6 -0.20 1.60 -14 2 5 22.40 4.00 -14 2 5 18.10 3.40 -14 -2 5 11.40 2.80 -14 2 4 17.00 3.40 -14 2 4 24.10 4.10 14 -2 -4 7.60 3.00 -14 -2 4 13.70 2.90 -14 2 3 67.09 5.90 -14 2 3 85.79 6.20 14 -2 -3 59.79 5.80 14 2 -2 26.80 3.70 -14 2 2 22.60 4.00 14 -2 -2 36.20 4.60 14 2 -1 1.20 2.10 -14 2 1 2.10 2.20 14 -2 -1 1.50 1.70 14 2 0 38.30 4.00 14 -2 0 34.80 4.40 14 2 1 -0.70 1.80 14 -2 1 -0.40 2.20 14 2 2 6.80 2.30 14 -2 2 12.50 2.90 14 2 3 43.50 4.30 14 -2 3 53.19 5.30 14 2 4 14.90 2.90 14 -2 4 16.40 3.40 14 2 5 1.80 2.20 14 -2 5 -0.90 2.20 -14 3 6 5.70 2.50 -14 3 6 12.10 3.20 -14 3 5 35.00 4.90 -14 3 5 34.20 4.60 -14 -3 5 39.10 4.20 -14 3 4 -3.00 1.90 -14 3 4 -1.20 1.60 14 -3 -4 1.70 2.50 -14 -3 4 2.50 1.70 -14 3 3 88.69 6.70 -14 3 3 88.39 6.90 14 -3 -3 77.79 6.50 -14 3 2 0.60 2.30 14 3 -2 -1.10 1.60 -14 3 2 0.50 1.70 14 -3 -2 -2.10 1.90 -14 3 1 1.20 2.30 14 3 -1 2.00 1.80 14 -3 -1 4.80 2.50 -14 3 0 1.30 2.30 14 3 0 0.20 1.50 14 -3 0 -1.40 2.00 14 3 1 6.50 2.30 14 -3 1 7.10 2.70 14 3 2 -3.20 1.30 14 -3 2 1.00 2.20 14 3 3 3.50 2.20 14 -3 3 0.20 2.30 14 3 4 6.40 2.50 14 -3 4 9.20 3.00 -14 4 5 18.50 3.80 -14 4 5 20.30 4.10 -14 4 4 1.20 2.40 -14 4 4 1.90 2.40 14 -4 -4 0.20 2.40 -14 4 3 63.39 6.00 -14 4 3 57.99 5.40 14 -4 -3 60.29 5.40 -14 4 2 0.70 1.70 -14 4 2 6.00 2.70 14 -4 -2 -1.20 2.00 -14 4 1 -3.20 1.80 14 4 -1 0.30 1.80 14 -4 -1 6.90 2.90 14 4 0 23.00 3.10 -14 4 0 21.70 4.00 14 -4 0 22.80 3.80 -14 4 -1 31.70 4.60 14 4 1 29.40 3.50 14 -4 1 29.80 4.40 14 -4 2 84.19 6.80 14 4 3 2.90 1.80 14 -4 3 2.30 2.30 -14 5 3 29.30 4.60 -14 5 3 31.20 4.80 14 -5 -3 29.90 5.20 -14 5 2 2.70 2.00 -14 5 2 -1.30 2.10 14 -5 -2 -4.80 1.90 -14 5 1 9.10 3.10 -14 5 1 -1.10 2.50 14 -5 -1 6.20 2.60 -14 5 0 70.69 5.80 14 -5 0 66.29 6.20 -14 5 -1 -0.20 2.40 14 -5 1 -0.90 2.30 -15 0 5 2.50 3.10 -15 0 5 0.00 2.20 -15 0 4 99.39 7.20 -15 0 4 106.39 6.60 15 0 -3 2.50 2.10 -15 0 3 -1.10 2.10 -15 0 3 1.50 2.10 15 0 -2 0.70 2.00 15 0 -1 2.70 2.20 15 0 0 5.50 2.50 15 0 1 -0.30 1.90 15 0 2 1.20 1.90 15 0 3 2.80 2.30 15 0 4 157.18 9.10 -15 1 5 0.90 2.30 -15 1 5 0.00 1.90 -15 -1 5 0.20 1.90 -15 1 4 1.70 2.10 -15 1 4 -1.40 2.10 -15 -1 4 4.40 2.50 -15 1 3 33.50 4.40 -15 1 3 36.70 5.00 15 1 -3 47.10 4.60 15 -1 -3 32.80 4.60 -15 -1 3 36.60 3.70 -15 -1 3 36.30 4.70 -15 1 2 -3.50 1.80 15 1 -2 3.60 2.20 15 -1 -2 -2.30 1.90 15 1 -1 30.70 4.10 15 -1 -1 35.20 4.60 15 1 0 30.00 4.00 15 -1 0 29.70 4.40 15 1 1 11.40 2.90 15 -1 1 19.60 3.50 15 1 2 1.50 1.90 15 -1 2 1.60 2.10 15 1 3 95.79 6.50 15 -1 3 84.29 6.60 15 1 4 63.29 5.50 15 -1 4 51.39 5.40 -15 2 5 56.19 5.90 -15 2 5 58.89 5.60 -15 -2 5 66.19 5.30 -15 2 4 148.09 8.60 -15 2 4 138.19 9.00 15 -2 -4 142.89 8.60 -15 -2 4 125.79 8.00 -15 2 3 -0.90 2.20 -15 2 3 2.30 2.40 15 -2 -3 2.80 2.00 -15 2 2 12.70 3.40 15 2 -2 19.80 3.40 15 -2 -2 19.20 3.60 15 2 -1 15.40 2.90 -15 2 1 16.60 3.70 15 -2 -1 24.10 3.90 15 2 0 1.60 1.90 15 -2 0 -1.50 2.00 15 2 1 2.00 1.80 15 -2 1 6.90 2.80 15 2 2 12.10 3.00 15 -2 2 5.30 2.70 15 2 3 27.50 3.80 15 -2 3 18.30 3.90 -15 3 4 21.50 3.90 -15 3 4 28.20 4.20 -15 -3 4 24.00 3.60 15 -3 -4 26.90 5.10 -15 3 3 15.60 3.60 -15 3 3 22.80 4.20 15 -3 -3 23.40 4.20 -15 3 2 6.80 2.90 -15 3 2 5.90 2.90 15 3 -2 6.60 2.30 15 -3 -2 2.80 2.60 15 3 -1 4.90 1.90 -15 3 1 3.00 2.10 15 -3 -1 1.10 2.30 -15 3 0 23.10 4.10 15 3 0 16.60 2.90 15 -3 0 18.10 3.80 15 3 1 92.59 5.90 15 -3 1 84.69 6.90 15 3 2 9.10 2.60 15 -3 2 12.60 3.50 -15 4 1 2.60 2.50 -16 0 2 1.30 2.30 16 0 -2 -1.00 1.90 16 0 -1 -1.10 2.00 16 0 0 27.90 4.10 16 0 1 -0.80 2.00 -16 1 2 4.10 2.80 16 1 -2 4.30 2.50 16 -1 -2 2.80 2.60 16 1 -1 5.60 2.50 16 -1 -1 11.50 3.30 16 1 0 2.60 2.20 16 -1 0 3.60 2.70 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23893 _olex2_submission_special_instructions 'No special instructions were received'