# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_axm666 _audit_creation_date 2013-03-28 _audit_creation_method ; Olex2 1.2 (compiled 2013.03.22 svn.r2654, GUI svn.r4446) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H22 O4' _chemical_formula_sum 'C20 H22 O4' _chemical_formula_weight 326.37 _chemical_absolute_configuration ? _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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.0638(2) _cell_length_b 12.3120(4) _cell_length_c 17.2952(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1717.09(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25207 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.32 _cell_measurement_theta_min 2.03 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_correction_T_min 0.9624 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-RED' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_unetI/netI 0.0909 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 26308 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.759 _diffrn_reflns_theta_min 2.030 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _reflns_Friedel_coverage 0.740 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 3483 _reflns_number_total 3641 _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 'STOE X-AREA' _computing_data_collection 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_molecular_graphics ; DIAMOND ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.167 _refine_diff_density_min -0.170 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.0(7) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 218 _refine_ls_number_reflns 3641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0309 _refine_ls_restrained_S_all 1.051 _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^)+(0.0384P)^2^+0.1018P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.0614 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C15(H15) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B) 2.c Aromatic/amide H refined with riding coordinates: C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14) 2.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _atom_sites_solution_hydrogens geom _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 C1 C 0.08851(16) 0.33880(11) 0.30604(8) 0.0155(3) Uani 1 1 d . . . . . C2 C 0.12476(17) 0.37603(11) 0.38348(8) 0.0162(3) Uani 1 1 d . . . . . C3 C 0.21232(16) 0.31227(11) 0.43353(7) 0.0157(3) Uani 1 1 d . . . . . C4 C 0.26869(17) 0.20751(11) 0.40855(8) 0.0169(3) Uani 1 1 d . . . . . H4 H 0.3284 0.1621 0.4431 0.020 Uiso 1 1 calc R U . . . C5 C 0.23689(16) 0.17358(11) 0.33603(7) 0.0157(3) Uani 1 1 d . . . . . C6 C 0.04442(17) 0.48084(11) 0.40679(8) 0.0173(3) Uani 1 1 d . . . . . C7 C 0.0428(2) 0.67234(12) 0.38906(9) 0.0269(3) Uani 1 1 d . . . . . H7A H -0.0777 0.6650 0.3988 0.032 Uiso 1 1 calc R U . . . H7B H 0.0580 0.7217 0.3444 0.032 Uiso 1 1 calc R U . . . C8 C 0.1254(3) 0.72019(14) 0.45917(10) 0.0356(4) Uani 1 1 d . . . . . H8A H 0.2456 0.7225 0.4510 0.053 Uiso 1 1 calc R U . . . H8B H 0.1007 0.6752 0.5045 0.053 Uiso 1 1 calc R U . . . H8C H 0.0838 0.7940 0.4677 0.053 Uiso 1 1 calc R U . . . C9 C 0.25347(16) 0.34753(11) 0.51347(7) 0.0167(3) Uani 1 1 d . . . . . C10 C 0.31734(17) 0.45109(12) 0.52805(8) 0.0191(3) Uani 1 1 d . . . . . H10 H 0.3329 0.5006 0.4865 0.023 Uiso 1 1 calc R U . . . C11 C 0.35822(18) 0.48210(12) 0.60295(8) 0.0209(3) Uani 1 1 d . . . . . H11 H 0.4024 0.5524 0.6125 0.025 Uiso 1 1 calc R U . . . C12 C 0.33431(17) 0.41017(12) 0.66378(8) 0.0199(3) Uani 1 1 d . . . . . H12 H 0.3612 0.4313 0.7151 0.024 Uiso 1 1 calc R U . . . C13 C 0.27094(17) 0.30724(11) 0.64949(8) 0.0192(3) Uani 1 1 d . . . . . H13 H 0.2540 0.2583 0.6912 0.023 Uiso 1 1 calc R U . . . C14 C 0.23221(18) 0.27541(11) 0.57473(8) 0.0187(3) Uani 1 1 d . . . . . H14 H 0.1911 0.2043 0.5653 0.022 Uiso 1 1 calc R U . . . C15 C 0.28497(16) 0.06890(11) 0.29861(7) 0.0165(3) Uani 1 1 d . . . . . H15 H 0.1807 0.0331 0.2805 0.020 Uiso 1 1 calc R U . . . C16 C 0.36993(18) -0.00919(11) 0.35487(8) 0.0197(3) Uani 1 1 d . . . . . H16A H 0.2965 -0.0226 0.3998 0.024 Uiso 1 1 calc R U . . . H16B H 0.4740 0.0238 0.3741 0.024 Uiso 1 1 calc R U . . . C17 C 0.40873(19) -0.11692(12) 0.31444(9) 0.0224(3) Uani 1 1 d . . . . . H17A H 0.4695 -0.1650 0.3505 0.027 Uiso 1 1 calc R U . . . H17B H 0.3036 -0.1534 0.3003 0.027 Uiso 1 1 calc R U . . . C18 C 0.51257(18) -0.09974(12) 0.24183(9) 0.0236(3) Uani 1 1 d . . . . . H18A H 0.5279 -0.1702 0.2152 0.028 Uiso 1 1 calc R U . . . H18B H 0.6234 -0.0722 0.2567 0.028 Uiso 1 1 calc R U . . . C19 C 0.43101(18) -0.01954(12) 0.18651(9) 0.0234(3) Uani 1 1 d . . . . . H19A H 0.3263 -0.0510 0.1667 0.028 Uiso 1 1 calc R U . . . H19B H 0.5054 -0.0066 0.1419 0.028 Uiso 1 1 calc R U . . . C20 C 0.39424(18) 0.08850(12) 0.22689(8) 0.0205(3) Uani 1 1 d . . . . . H20A H 0.3364 0.1379 0.1907 0.025 Uiso 1 1 calc R U . . . H20B H 0.4995 0.1234 0.2427 0.025 Uiso 1 1 calc R U . . . O1 O 0.00737(12) 0.38611(8) 0.25779(6) 0.0195(2) Uani 1 1 d . . . . . O2 O 0.15011(12) 0.23835(8) 0.28576(5) 0.0163(2) Uani 1 1 d . . . . . O3 O -0.06849(13) 0.48638(9) 0.45200(6) 0.0250(2) Uani 1 1 d . . . . . O4 O 0.11290(13) 0.56597(8) 0.37086(6) 0.0223(2) Uani 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 C1 0.0148(6) 0.0149(6) 0.0170(6) 0.0007(5) 0.0019(5) -0.0017(5) C2 0.0177(6) 0.0148(6) 0.0161(6) 0.0000(5) 0.0016(5) -0.0011(5) C3 0.0161(6) 0.0163(6) 0.0147(6) 0.0008(5) 0.0013(5) -0.0021(5) C4 0.0178(6) 0.0162(6) 0.0168(6) 0.0008(5) -0.0001(5) 0.0002(5) C5 0.0140(6) 0.0159(6) 0.0171(6) 0.0019(5) 0.0004(5) -0.0005(5) C6 0.0205(6) 0.0174(6) 0.0141(6) 0.0004(5) -0.0029(5) 0.0012(5) C7 0.0388(9) 0.0139(7) 0.0280(8) 0.0014(6) -0.0022(7) 0.0053(6) C8 0.0531(11) 0.0210(8) 0.0328(9) -0.0046(7) -0.0066(8) 0.0045(8) C9 0.0160(6) 0.0181(6) 0.0159(6) -0.0015(5) -0.0004(5) 0.0030(5) C10 0.0211(7) 0.0183(7) 0.0178(6) 0.0011(5) 0.0007(5) 0.0003(5) C11 0.0217(7) 0.0191(7) 0.0218(7) -0.0029(6) -0.0012(5) -0.0011(6) C12 0.0180(6) 0.0256(7) 0.0160(6) -0.0040(6) -0.0014(5) 0.0048(5) C13 0.0211(6) 0.0204(7) 0.0162(6) 0.0029(5) 0.0002(5) 0.0043(5) C14 0.0203(7) 0.0168(6) 0.0190(6) -0.0006(5) -0.0006(5) 0.0023(5) C15 0.0171(6) 0.0159(6) 0.0166(6) -0.0022(5) -0.0005(5) -0.0006(5) C16 0.0229(6) 0.0178(7) 0.0183(6) -0.0015(5) -0.0009(5) 0.0021(5) C17 0.0261(7) 0.0176(7) 0.0236(7) -0.0021(6) -0.0028(6) 0.0046(6) C18 0.0209(7) 0.0205(7) 0.0293(8) -0.0072(6) 0.0008(6) 0.0025(6) C19 0.0259(7) 0.0232(7) 0.0210(7) -0.0047(6) 0.0044(6) 0.0007(6) C20 0.0222(7) 0.0198(7) 0.0194(7) -0.0005(5) 0.0032(6) 0.0010(6) O1 0.0215(5) 0.0197(5) 0.0174(5) 0.0024(4) -0.0026(4) 0.0015(4) O2 0.0179(5) 0.0160(5) 0.0151(4) -0.0001(4) -0.0016(4) 0.0008(4) O3 0.0260(5) 0.0223(5) 0.0265(5) -0.0008(4) 0.0065(4) 0.0032(4) O4 0.0299(5) 0.0152(5) 0.0217(5) 0.0022(4) 0.0025(4) 0.0013(4) _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 1.4455(18) . ? C1 O1 1.2099(17) . ? C1 O2 1.3782(16) . ? C2 C3 1.3653(19) . ? C2 C6 1.4991(19) . ? C3 C4 1.4341(19) . ? C3 C9 1.4868(18) . ? C4 H4 0.9500 . ? C4 C5 1.3467(18) . ? C5 C15 1.4933(18) . ? C5 O2 1.3717(16) . ? C6 O3 1.2021(17) . ? C6 O4 1.3378(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.504(2) . ? C7 O4 1.4608(17) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.398(2) . ? C9 C14 1.3931(19) . ? C10 H10 0.9500 . ? C10 C11 1.390(2) . ? C11 H11 0.9500 . ? C11 C12 1.389(2) . ? C12 H12 0.9500 . ? C12 C13 1.389(2) . ? C13 H13 0.9500 . ? C13 C14 1.3866(19) . ? C14 H14 0.9500 . ? C15 H15 1.0000 . ? C15 C16 1.5299(19) . ? C15 C20 1.5406(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.5317(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.524(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.524(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.531(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? 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 O1 C1 C2 126.57(13) . . ? O1 C1 O2 116.84(12) . . ? O2 C1 C2 116.59(11) . . ? C1 C2 C6 115.77(12) . . ? C3 C2 C1 120.64(12) . . ? C3 C2 C6 123.22(12) . . ? C2 C3 C4 119.35(12) . . ? C2 C3 C9 122.49(12) . . ? C4 C3 C9 118.16(12) . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 119.95(12) . . ? C5 C4 H4 120.0 . . ? C4 C5 C15 128.46(12) . . ? C4 C5 O2 120.47(12) . . ? O2 C5 C15 111.07(11) . . ? O3 C6 C2 123.44(13) . . ? O3 C6 O4 124.78(13) . . ? O4 C6 C2 111.78(11) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? O4 C7 H7A 109.5 . . ? O4 C7 H7B 109.5 . . ? O4 C7 C8 110.71(13) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C3 121.09(12) . . ? C14 C9 C3 119.59(12) . . ? C14 C9 C10 119.31(12) . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.39(13) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 120.1 . . ? C12 C11 C10 119.86(13) . . ? C12 C11 H11 120.1 . . ? C11 C12 H12 120.1 . . ? C13 C12 C11 119.89(13) . . ? C13 C12 H12 120.1 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.45(13) . . ? C14 C13 H13 119.8 . . ? C9 C14 H14 120.0 . . ? C13 C14 C9 120.09(13) . . ? C13 C14 H14 120.0 . . ? C5 C15 H15 107.3 . . ? C5 C15 C16 112.52(11) . . ? C5 C15 C20 111.24(11) . . ? C16 C15 H15 107.3 . . ? C16 C15 C20 110.76(11) . . ? C20 C15 H15 107.3 . . ? C15 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? C15 C16 C17 110.20(12) . . ? H16A C16 H16B 108.1 . . ? C17 C16 H16A 109.6 . . ? C17 C16 H16B 109.6 . . ? C16 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C18 C17 C16 111.61(12) . . ? C18 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C17 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? C17 C18 C19 111.72(12) . . ? H18A C18 H18B 107.9 . . ? C19 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C18 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C18 C19 C20 111.11(12) . . ? H19A C19 H19B 108.0 . . ? C20 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? C15 C20 H20A 109.7 . . ? C15 C20 H20B 109.7 . . ? C19 C20 C15 109.99(11) . . ? C19 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C5 O2 C1 122.98(10) . . ? C6 O4 C7 116.27(11) . . ? 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 0.11(19) . . . . ? C1 C2 C3 C9 179.56(12) . . . . ? C1 C2 C6 O3 107.65(15) . . . . ? C1 C2 C6 O4 -71.90(15) . . . . ? C2 C1 O2 C5 2.18(17) . . . . ? C2 C3 C4 C5 0.86(19) . . . . ? C2 C3 C9 C10 -46.55(19) . . . . ? C2 C3 C9 C14 135.13(14) . . . . ? C2 C6 O4 C7 179.57(12) . . . . ? C3 C2 C6 O3 -65.45(19) . . . . ? C3 C2 C6 O4 114.99(14) . . . . ? C3 C4 C5 C15 179.52(12) . . . . ? C3 C4 C5 O2 -0.3(2) . . . . ? C3 C9 C10 C11 -178.75(13) . . . . ? C3 C9 C14 C13 179.69(12) . . . . ? C4 C3 C9 C10 132.91(14) . . . . ? C4 C3 C9 C14 -45.41(18) . . . . ? C4 C5 C15 C16 4.7(2) . . . . ? C4 C5 C15 C20 -120.21(15) . . . . ? C4 C5 O2 C1 -1.29(19) . . . . ? C5 C15 C16 C17 177.27(11) . . . . ? C5 C15 C20 C19 -175.93(12) . . . . ? C6 C2 C3 C4 172.89(12) . . . . ? C6 C2 C3 C9 -7.7(2) . . . . ? C8 C7 O4 C6 87.18(16) . . . . ? C9 C3 C4 C5 -178.62(12) . . . . ? C9 C10 C11 C12 -0.5(2) . . . . ? C10 C9 C14 C13 1.3(2) . . . . ? C10 C11 C12 C13 0.5(2) . . . . ? C11 C12 C13 C14 0.4(2) . . . . ? C12 C13 C14 C9 -1.3(2) . . . . ? C14 C9 C10 C11 -0.4(2) . . . . ? C15 C5 O2 C1 178.86(11) . . . . ? C15 C16 C17 C18 55.64(16) . . . . ? C16 C15 C20 C19 58.14(15) . . . . ? C16 C17 C18 C19 -54.72(16) . . . . ? C17 C18 C19 C20 55.19(16) . . . . ? C18 C19 C20 C15 -56.55(15) . . . . ? C20 C15 C16 C17 -57.52(15) . . . . ? O1 C1 C2 C3 177.13(13) . . . . ? O1 C1 C2 C6 3.8(2) . . . . ? O1 C1 O2 C5 -176.64(11) . . . . ? O2 C1 C2 C3 -1.56(18) . . . . ? O2 C1 C2 C6 -174.86(11) . . . . ? O2 C5 C15 C16 -175.43(11) . . . . ? O2 C5 C15 C20 59.62(14) . . . . ? O3 C6 O4 C7 0.0(2) . . . . ? _shelx_estimated_absorpt_T_max 0.984 _shelx_estimated_absorpt_T_min 0.949 _shelx_hkl_checksum 62871 _shelx_hkl_file ; -2 0 0 22.98 0.41 0 2 0 0 22.84 0.40 0 -2 0 0 22.68 0.38 0 2 0 0 22.22 0.39 0 -4 0 0 0.39 0.11 0 -4 0 0 0.45 0.16 0 4 0 0 0.29 0.12 0 4 0 0 0.24 0.16 0 -6 0 0 14.50 0.26 0 6 0 0 13.28 0.22 0 -6 0 0 13.97 0.24 0 6 0 0 14.16 0.21 0 8 0 0 16.86 0.28 0 -8 0 0 15.41 0.23 0 8 0 0 14.22 0.27 0 -8 0 0 16.56 0.28 0 -10 0 0 0.56 0.24 0 10 0 0 0.39 0.19 0 -10 0 0 0.57 0.23 0 10 0 0 0.47 0.20 0 -1 -1 0 25.62 0.52 0 1 -1 0 24.41 0.52 0 1 1 0 25.15 0.51 0 1 -1 0 24.94 0.53 0 1 1 0 24.65 0.58 0 -1 1 0 24.42 0.50 0 -1 1 0 24.62 0.55 0 -2 -1 0 0.09 0.17 0 2 1 0 0.10 0.16 0 -2 1 0 0.13 0.17 0 2 -1 0 0.11 0.17 0 2 -1 0 0.08 0.17 0 2 1 0 0.05 0.12 0 -2 -1 0 0.08 0.17 0 -2 1 0 0.11 0.13 0 -3 -1 0 0.32 0.17 0 3 1 0 0.19 0.12 0 3 -1 0 0.20 0.11 0 3 1 0 0.14 0.16 0 -3 1 0 0.22 0.11 0 -3 -1 0 0.18 0.12 0 -3 1 0 0.21 0.12 0 3 -1 0 0.17 0.16 0 4 -1 0 0.46 0.11 0 -4 1 0 0.61 0.11 0 -4 1 0 0.65 0.17 0 4 1 0 0.48 0.12 0 4 -1 0 0.66 0.12 0 -4 -1 0 0.52 0.12 0 -4 -1 0 0.55 0.12 0 4 1 0 0.56 0.11 0 -5 1 0 10.82 0.20 0 5 -1 0 9.92 0.20 0 -5 -1 0 10.53 0.20 0 -5 -1 0 10.95 0.20 0 5 -1 0 10.55 0.21 0 5 1 0 10.64 0.23 0 -5 1 0 10.47 0.23 0 5 1 0 10.58 0.20 0 6 -1 0 0.71 0.17 0 6 1 0 0.54 0.16 0 6 1 0 0.78 0.16 0 -6 1 0 0.69 0.17 0 -6 1 0 0.68 0.12 0 -6 -1 0 0.59 0.13 0 -6 -1 0 0.51 0.13 0 6 -1 0 0.63 0.17 0 7 1 0 4.03 0.19 0 -7 1 0 4.11 0.15 0 7 -1 0 4.04 0.19 0 -7 1 0 4.21 0.16 0 -7 -1 0 4.33 0.16 0 7 1 0 4.08 0.19 0 -7 -1 0 4.53 0.16 0 7 -1 0 3.77 0.20 0 8 1 0 0.20 0.15 0 8 1 0 0.26 0.15 0 -8 1 0 0.46 0.20 0 -8 -1 0 0.35 0.21 0 8 -1 0 0.19 0.15 0 8 -1 0 0.43 0.18 0 -8 1 0 0.27 0.15 0 -8 -1 0 0.35 0.21 0 -9 -1 0 6.63 0.20 0 -9 -1 0 6.83 0.26 0 9 -1 0 4.89 0.23 0 9 1 0 6.94 0.26 0 9 1 0 5.55 0.23 0 9 -1 0 6.36 0.20 0 -9 1 0 6.73 0.24 0 -9 1 0 6.01 0.23 0 10 1 0 0.26 0.23 0 -10 1 0 0.23 0.18 0 -10 1 0 0.25 0.28 0 10 1 0 0.20 0.27 0 -10 -1 0 0.36 0.26 0 10 -1 0 0.13 0.18 0 -10 -1 0 0.23 0.20 0 10 -1 0 0.08 0.27 0 0 -2 0 34.82 1.05 0 0 2 0 33.89 0.55 0 0 2 0 34.74 0.56 0 0 2 0 35.96 1.05 0 -1 2 0 9.57 0.31 0 -1 -2 0 9.50 0.31 0 1 -2 0 8.92 0.31 0 1 2 0 9.33 0.42 0 1 2 0 9.65 0.28 0 -1 2 0 9.24 0.32 0 1 -2 0 9.47 0.30 0 -2 2 0 221.58 1.06 0 2 2 0 212.84 1.19 0 2 -2 0 224.70 1.12 0 2 2 0 216.65 1.02 0 -2 2 0 216.94 1.11 0 2 -2 0 212.08 1.03 0 -2 -2 0 223.86 1.04 0 -2 -2 0 54.36 0.60 0 3 -2 0 10.29 0.24 0 3 2 0 10.81 0.27 0 -3 -2 0 10.76 0.24 0 -3 2 0 10.94 0.25 0 3 2 0 10.79 0.23 0 -3 2 0 10.42 0.27 0 -3 -2 0 10.98 0.26 0 3 -2 0 11.14 0.25 0 -4 2 0 55.53 0.41 0 -4 -2 0 54.43 0.42 0 -4 -2 0 58.24 0.46 0 -4 2 0 56.28 0.46 0 4 -2 0 56.07 0.42 0 4 2 0 54.28 0.42 0 4 -2 0 55.46 0.46 0 4 2 0 58.17 0.47 0 -5 2 0 0.17 0.15 0 5 -2 0 0.16 0.11 0 -5 -2 0 0.23 0.16 0 -5 2 0 0.17 0.15 0 5 2 0 0.25 0.16 0 5 2 0 0.20 0.12 0 5 -2 0 0.31 0.14 0 -5 -2 0 0.21 0.16 0 6 2 0 4.92 0.17 0 -6 -2 0 4.58 0.17 0 -6 2 0 4.39 0.20 0 6 -2 0 4.46 0.19 0 -6 -2 0 4.80 0.21 0 6 2 0 4.50 0.16 0 -6 2 0 4.59 0.18 0 6 -2 0 4.62 0.18 0 -7 2 0 0.71 0.12 0 7 2 0 0.72 0.18 0 7 2 0 0.78 0.17 0 -7 2 0 0.85 0.19 0 -7 -2 0 0.81 0.18 0 7 -2 0 0.63 0.18 0 7 -2 0 0.66 0.16 0 -7 -2 0 0.78 0.19 0 8 2 0 6.31 0.19 0 -8 2 0 6.99 0.22 0 -8 2 0 7.14 0.22 0 -8 -2 0 7.55 0.23 0 -8 -2 0 7.90 0.24 0 8 2 0 7.12 0.24 0 8 -2 0 6.93 0.22 0 8 -2 0 6.07 0.18 0 -9 -2 0 4.79 0.25 0 -9 -2 0 4.88 0.22 0 -9 2 0 4.60 0.25 0 9 -2 0 3.78 0.19 0 9 2 0 4.02 0.22 0 -9 2 0 4.20 0.18 0 9 -2 0 4.55 0.24 0 9 2 0 4.32 0.23 0 -10 2 0 0.64 0.25 0 10 -2 0 0.89 0.26 0 10 2 0 0.64 0.19 0 10 -2 0 0.40 0.27 0 10 2 0 0.62 0.26 0 -10 -2 0 0.63 0.26 0 -10 2 0 0.59 0.23 0 -10 -2 0 0.85 0.24 0 1 3 0 48.78 0.92 0 -1 3 0 47.43 0.63 0 -1 -3 0 48.86 0.52 0 -1 -3 0 49.09 0.94 0 1 3 0 48.40 0.50 0 1 -3 0 48.30 0.63 0 -1 3 0 48.14 0.53 0 1 -3 0 48.43 0.54 0 2 3 0 66.79 0.53 0 -2 3 0 65.20 0.58 0 -2 -3 0 66.31 0.54 0 2 -3 0 65.62 0.58 0 2 3 0 64.86 0.69 0 -2 3 0 64.91 0.58 0 2 -3 0 65.29 0.57 0 -3 -3 0 13.12 0.24 0 -3 -3 0 13.47 0.29 0 3 3 0 12.97 0.30 0 -3 3 0 13.25 0.27 0 3 -3 0 12.95 0.24 0 3 -3 0 13.32 0.27 0 3 3 0 13.26 0.24 0 -3 3 0 13.13 0.28 0 4 3 0 37.98 0.39 0 4 -3 0 37.57 0.34 0 4 3 0 37.20 0.34 0 -4 -3 0 37.38 0.34 0 4 -3 0 39.93 0.39 0 -4 -3 0 39.89 0.40 0 -4 3 0 39.05 0.34 0 -4 3 0 37.74 0.36 0 -5 3 0 22.44 0.30 0 -5 3 0 21.83 0.28 0 -5 -3 0 24.32 0.30 0 5 -3 0 22.10 0.27 0 -5 -3 0 23.39 0.30 0 5 3 0 22.34 0.30 0 5 -3 0 22.35 0.28 0 5 3 0 21.84 0.27 0 -6 3 0 0.09 0.15 0 -6 -3 0 0.13 0.12 0 -6 3 0 0.14 0.17 0 6 -3 0 0.13 0.12 0 6 -3 0 0.09 0.12 0 6 3 0 -0.02 0.13 0 -6 -3 0 0.08 0.13 0 6 3 0 0.16 0.16 0 7 3 0 1.66 0.20 0 -7 3 0 1.91 0.19 0 7 -3 0 1.93 0.14 0 7 -3 0 1.84 0.15 0 -7 -3 0 1.88 0.15 0 -7 -3 0 1.96 0.18 0 -7 3 0 1.71 0.18 0 7 3 0 1.61 0.18 0 -8 -3 0 0.16 0.15 0 8 3 0 0.36 0.19 0 -8 3 0 0.38 0.19 0 -8 3 0 0.24 0.20 0 8 -3 0 0.23 0.14 0 8 3 0 0.26 0.22 0 -8 -3 0 0.21 0.20 0 8 -3 0 0.30 0.14 0 9 3 0 0.30 0.15 0 -9 -3 0 0.57 0.16 0 9 -3 0 0.25 0.24 0 -9 -3 0 0.53 0.22 0 -9 3 0 0.53 0.24 0 9 3 0 0.51 0.20 0 9 -3 0 0.31 0.16 0 -9 3 0 0.52 0.16 0 10 3 0 0.13 0.22 0 -10 -3 0 0.01 0.18 0 0 -4 0 15.66 0.55 0 0 4 0 14.33 0.30 0 0 4 0 14.62 0.28 0 1 4 0 0.41 0.26 0 1 4 0 0.41 0.16 0 -1 4 0 0.46 0.17 0 -1 -4 0 0.41 0.12 0 1 -4 0 0.40 0.18 0 -1 4 0 0.45 0.18 0 -1 -4 0 0.45 0.28 0 1 -4 0 0.35 0.18 0 -2 -4 0 25.08 0.33 0 2 4 0 24.70 0.31 0 2 -4 0 24.91 0.37 0 -2 4 0 24.22 0.35 0 2 4 0 25.42 0.48 0 -2 4 0 24.72 0.37 0 2 -4 0 24.20 0.33 0 -2 -4 0 24.88 0.48 0 -3 -4 0 35.34 0.34 0 3 4 0 36.60 0.46 0 3 4 0 36.31 0.35 0 -3 4 0 36.55 0.39 0 -3 4 0 36.02 0.36 0 3 -4 0 35.15 0.36 0 3 -4 0 37.04 0.38 0 4 -4 0 15.31 0.23 0 -4 4 0 16.29 0.27 0 4 4 0 15.98 0.29 0 -4 -4 0 15.52 0.26 0 -4 -4 0 16.05 0.25 0 -4 4 0 16.35 0.24 0 4 -4 0 15.66 0.27 0 4 4 0 14.93 0.23 0 5 -4 0 0.30 0.16 0 -5 4 0 0.24 0.15 0 -5 4 0 0.35 0.16 0 -5 -4 0 0.29 0.16 0 5 -4 0 0.30 0.12 0 -5 -4 0 0.31 0.15 0 5 4 0 0.25 0.15 0 5 4 0 0.25 0.16 0 6 4 0 0.43 0.17 0 6 4 0 0.35 0.17 0 -6 4 0 0.32 0.12 0 -6 -4 0 0.48 0.16 0 6 -4 0 0.41 0.12 0 -6 -4 0 0.33 0.18 0 6 -4 0 0.31 0.18 0 -6 4 0 0.24 0.18 0 7 4 0 0.48 0.14 0 7 -4 0 0.59 0.19 0 -7 4 0 0.52 0.13 0 -7 -4 0 0.55 0.19 0 -7 -4 0 0.41 0.18 0 7 4 0 0.63 0.19 0 -7 4 0 0.63 0.19 0 7 -4 0 0.54 0.13 0 -8 -4 0 5.91 0.24 0 -8 4 0 5.15 0.22 0 8 -4 0 5.29 0.18 0 8 4 0 5.52 0.24 0 -8 -4 0 5.35 0.22 0 -8 4 0 5.39 0.18 0 8 4 0 4.85 0.23 0 8 -4 0 4.71 0.21 0 9 -4 0 0.25 0.20 0 -9 -4 0 0.06 0.22 0 9 -4 0 0.04 0.22 0 -9 4 0 0.10 0.20 0 9 4 0 0.10 0.22 0 -9 4 0 0.06 0.22 0 -9 -4 0 0.06 0.23 0 9 4 0 0.21 0.23 0 -1 5 0 0.08 0.16 0 1 -5 0 0.05 0.12 0 -1 -5 0 0.14 0.27 0 -1 5 0 0.10 0.12 0 -1 -5 0 0.09 0.11 0 1 5 0 0.05 0.15 0 1 -5 0 0.11 0.16 0 -2 -5 0 51.81 0.41 0 2 -5 0 53.24 0.44 0 -2 5 0 53.65 0.45 0 2 -5 0 52.36 0.51 0 2 5 0 54.98 0.43 0 -2 -5 0 53.76 0.72 0 2 5 0 54.34 0.74 0 -2 5 0 54.93 0.52 0 3 5 0 9.72 0.28 0 -3 -5 0 9.35 0.22 0 3 -5 0 9.51 0.24 0 3 5 0 9.31 0.22 0 3 -5 0 9.49 0.23 0 -3 5 0 9.55 0.21 0 -3 5 0 9.79 0.21 0 -4 -5 0 0.04 0.15 0 -4 5 0 0.04 0.11 0 -4 5 0 0.04 0.11 0 4 -5 0 0.01 0.15 0 4 5 0 -0.03 0.15 0 -4 -5 0 -0.03 0.14 0 4 5 0 0.09 0.15 0 4 -5 0 0.06 0.16 0 -5 -5 0 3.00 0.19 0 5 5 0 3.26 0.19 0 5 -5 0 3.03 0.20 0 -5 5 0 3.10 0.18 0 -5 -5 0 3.16 0.18 0 5 -5 0 2.95 0.15 0 -5 5 0 2.92 0.15 0 5 5 0 3.09 0.18 0 -6 5 0 2.27 0.20 0 -6 -5 0 2.55 0.21 0 -6 5 0 2.14 0.18 0 6 -5 0 2.30 0.20 0 -6 -5 0 2.48 0.14 0 6 5 0 1.94 0.14 0 6 -5 0 2.37 0.18 0 6 5 0 2.31 0.19 0 -7 -5 0 1.13 0.20 0 7 -5 0 0.85 0.14 0 -7 5 0 1.00 0.18 0 7 5 0 0.98 0.18 0 7 -5 0 1.12 0.15 0 -7 -5 0 1.28 0.20 0 -7 5 0 1.04 0.19 0 7 5 0 1.15 0.15 0 -8 5 0 10.33 0.25 0 8 -5 0 8.74 0.25 0 -8 5 0 10.10 0.25 0 -8 -5 0 10.69 0.26 0 -8 -5 0 10.49 0.27 0 8 5 0 8.67 0.23 0 8 -5 0 10.48 0.21 0 8 5 0 10.49 0.28 0 -9 -5 0 2.06 0.26 0 9 5 0 1.79 0.18 0 9 -5 0 2.04 0.18 0 9 -5 0 1.37 0.23 0 9 5 0 1.97 0.23 0 -9 5 0 1.65 0.21 0 -9 5 0 1.91 0.23 0 -9 -5 0 2.17 0.24 0 0 -6 0 11.87 0.44 0 0 -6 0 11.44 0.43 0 0 6 0 11.78 0.24 0 0 6 0 11.47 0.22 0 1 -6 0 36.24 0.37 0 -1 6 0 34.59 0.35 0 1 -6 0 35.48 0.51 0 1 6 0 34.44 0.33 0 -1 6 0 36.99 0.52 0 2 -6 0 1.82 0.13 0 2 6 0 1.86 0.24 0 2 6 0 2.01 0.16 0 2 -6 0 1.67 0.18 0 -2 -6 0 1.80 0.13 0 -2 6 0 1.77 0.17 0 -2 6 0 1.93 0.18 0 -2 -6 0 1.87 0.25 0 3 6 0 16.06 0.37 0 3 6 0 15.13 0.24 0 3 -6 0 16.02 0.24 0 -3 6 0 15.78 0.26 0 -3 6 0 15.79 0.25 0 -3 -6 0 14.97 0.22 0 3 -6 0 15.42 0.26 0 -3 -6 0 16.10 0.37 0 -4 6 0 13.39 0.25 0 -4 -6 0 13.01 0.21 0 4 -6 0 13.33 0.25 0 -4 6 0 12.64 0.24 0 4 -6 0 12.88 0.22 0 4 6 0 13.16 0.30 0 4 6 0 12.82 0.21 0 5 -6 0 2.92 0.15 0 5 6 0 3.21 0.15 0 -5 -6 0 3.34 0.18 0 -5 -6 0 3.27 0.19 0 5 6 0 3.15 0.19 0 5 -6 0 2.86 0.15 0 -5 6 0 3.08 0.15 0 -5 6 0 3.16 0.19 0 -6 6 0 23.95 0.28 0 -6 6 0 22.72 0.29 0 6 6 0 23.36 0.28 0 6 -6 0 23.67 0.26 0 -6 -6 0 25.38 0.28 0 -6 -6 0 25.34 0.33 0 6 -6 0 21.58 0.27 0 6 6 0 24.34 0.32 0 7 6 0 17.78 0.24 0 7 -6 0 16.57 0.26 0 -7 -6 0 19.27 0.25 0 7 6 0 18.70 0.28 0 -7 6 0 19.70 0.29 0 7 -6 0 20.26 0.29 0 -7 -6 0 19.83 0.28 0 -7 6 0 17.38 0.24 0 8 6 0 1.88 0.23 0 -8 -6 0 2.19 0.21 0 8 -6 0 2.36 0.24 0 8 6 0 2.10 0.18 0 8 -6 0 1.83 0.24 0 -8 6 0 2.21 0.23 0 -8 -6 0 2.39 0.18 0 -8 6 0 2.31 0.25 0 9 -6 0 0.10 0.25 0 -9 6 0 0.15 0.22 0 9 -6 0 0.18 0.18 0 -9 6 0 0.05 0.22 0 9 6 0 0.14 0.17 0 -9 -6 0 0.12 0.22 0 9 6 0 0.15 0.24 0 -9 -6 0 -0.06 0.17 0 1 7 0 4.54 0.15 0 -1 7 0 4.92 0.24 0 -1 7 0 4.59 0.15 0 1 -7 0 4.63 0.23 0 1 7 0 4.36 0.15 0 -2 7 0 7.92 0.22 0 -2 -7 0 7.94 0.44 0 -2 -7 0 7.61 0.20 0 2 7 0 7.33 0.17 0 2 -7 0 7.73 0.24 0 2 7 0 7.88 0.44 0 -2 7 0 7.90 0.21 0 2 -7 0 7.69 0.18 0 3 -7 0 8.26 0.19 0 -3 7 0 8.51 0.23 0 3 7 0 8.18 0.21 0 -3 -7 0 8.64 0.32 0 3 7 0 8.38 0.32 0 -3 7 0 8.32 0.22 0 -3 -7 0 8.41 0.20 0 3 -7 0 8.19 0.22 0 -4 -7 0 0.37 0.18 0 4 7 0 0.37 0.18 0 4 -7 0 0.39 0.16 0 -4 7 0 0.38 0.17 0 -4 7 0 0.37 0.16 0 4 -7 0 0.30 0.17 0 -4 -7 0 0.36 0.12 0 4 7 0 0.41 0.17 0 -5 -7 0 0.42 0.18 0 -5 7 0 0.34 0.19 0 5 -7 0 0.33 0.18 0 5 -7 0 0.27 0.17 0 5 7 0 0.33 0.12 0 5 7 0 0.39 0.18 0 -5 7 0 0.30 0.13 0 6 -7 0 1.16 0.14 0 6 7 0 1.02 0.15 0 -6 7 0 1.20 0.17 0 6 -7 0 1.30 0.18 0 -6 7 0 1.30 0.18 0 -6 -7 0 1.28 0.20 0 -6 -7 0 1.16 0.18 0 6 7 0 1.23 0.20 0 7 -7 0 0.06 0.14 0 -7 -7 0 0.00 0.15 0 7 7 0 0.10 0.20 0 7 -7 0 0.06 0.19 0 -7 -7 0 0.05 0.19 0 -7 7 0 -0.00 0.14 0 -7 7 0 0.04 0.15 0 7 7 0 -0.04 0.15 0 -8 7 0 0.57 0.24 0 8 -7 0 1.01 0.18 0 8 7 0 0.81 0.21 0 -8 -7 0 0.94 0.21 0 8 -7 0 0.70 0.18 0 -8 -7 0 1.06 0.22 0 -8 7 0 0.95 0.18 0 8 7 0 0.93 0.21 0 9 -7 0 0.75 0.24 0 9 -7 0 0.71 0.26 0 -9 -7 0 0.87 0.26 0 -9 7 0 0.85 0.27 0 -9 -7 0 0.88 0.20 0 9 7 0 0.92 0.24 0 -9 7 0 0.72 0.20 0 9 7 0 0.66 0.23 0 0 -8 0 1.04 0.24 0 0 8 0 1.01 0.12 0 0 -8 0 1.00 0.25 0 0 8 0 0.97 0.16 0 1 -8 0 2.32 0.24 0 1 8 0 2.31 0.17 0 1 8 0 2.37 0.13 0 -1 8 0 2.60 0.21 0 -1 8 0 2.29 0.14 0 -1 8 0 2.45 0.14 0 2 8 0 51.55 0.38 0 -2 -8 0 50.05 0.37 0 -2 8 0 50.77 0.39 0 2 -8 0 50.19 0.49 0 2 -8 0 50.31 0.39 0 -2 8 0 53.07 0.51 0 -3 8 0 0.27 0.15 0 3 8 0 0.25 0.22 0 -3 8 0 0.38 0.16 0 3 -8 0 0.29 0.16 0 -3 -8 0 0.28 0.21 0 3 -8 0 0.30 0.12 0 -3 -8 0 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0.20 0 4 4 -10 10.18 0.22 0 -4 4 10 9.80 0.22 0 4 -4 10 10.28 0.22 0 5 4 10 3.22 0.21 0 -5 -4 10 3.23 0.15 0 5 4 10 3.10 0.21 0 5 4 10 3.09 0.21 0 -5 -4 10 3.06 0.18 0 5 4 10 2.85 0.21 0 5 -4 -10 3.21 0.18 0 5 -4 -10 2.97 0.18 0 5 -4 10 3.24 0.15 0 5 4 -10 3.18 0.16 0 5 4 -10 3.50 0.15 0 -5 4 10 3.06 0.15 0 -5 4 10 3.05 0.19 0 6 4 10 14.68 0.26 0 6 4 10 16.34 0.31 0 -6 -4 10 15.99 0.28 0 6 4 10 14.04 0.30 0 -6 -4 10 15.99 0.26 0 -6 4 -10 16.16 0.25 0 6 -4 -10 16.48 0.28 0 6 -4 -10 14.55 0.24 0 6 -4 10 16.46 0.22 0 -6 4 10 14.64 0.27 0 -6 4 10 15.66 0.26 0 6 4 -10 15.52 0.26 0 6 4 -10 15.39 0.28 0 -7 4 -10 6.36 0.44 0 -7 -4 10 6.05 0.19 0 -7 -4 10 6.52 0.25 0 7 4 10 4.91 0.24 0 -7 4 -10 6.47 0.21 0 7 -4 -10 6.56 0.19 0 7 4 10 5.96 0.21 0 7 -4 -10 5.96 0.24 0 7 -4 10 6.13 0.18 0 7 -4 10 5.54 0.43 0 -7 4 10 6.27 0.19 0 -7 4 10 5.61 0.22 0 7 4 -10 5.48 0.22 0 7 4 -10 6.46 0.20 0 -7 -4 -10 6.93 0.27 0 -8 4 -10 0.22 0.32 0 -8 -4 10 0.42 0.21 0 -8 4 -10 0.40 0.20 0 -8 -4 10 0.36 0.24 0 8 4 10 0.24 0.24 0 8 4 10 0.31 0.19 0 8 -4 -10 0.37 0.24 0 8 -4 -10 0.31 0.21 0 -8 -4 -10 0.33 0.24 0 8 -4 10 0.17 0.31 0 -8 4 10 0.30 0.17 0 8 4 -10 0.31 0.16 0 -8 -4 -10 0.32 0.18 0 -8 4 10 0.25 0.24 0 8 4 -10 0.27 0.24 0 8 -4 10 0.37 0.23 0 0 -5 -10 37.60 0.35 0 0 5 -10 34.20 0.31 0 0 -5 10 34.63 0.43 0 0 -5 -10 35.10 0.38 0 0 -5 10 35.66 0.33 0 0 5 10 35.29 0.37 0 0 5 10 34.95 0.35 0 1 5 10 2.25 0.14 0 1 -5 -10 2.64 0.14 0 -1 -5 10 2.42 0.17 0 1 -5 -10 2.31 0.14 0 -1 5 -10 2.32 0.21 0 1 5 10 2.32 0.14 0 -1 -5 10 2.42 0.18 0 -1 5 10 2.54 0.17 0 -1 -5 -10 2.47 0.18 0 1 5 -10 2.36 0.18 0 -1 -5 -10 2.11 0.18 0 1 -5 10 2.38 0.18 0 1 -5 10 2.50 0.15 0 1 5 -10 2.44 0.18 0 -1 5 10 2.28 0.14 0 -2 5 -10 8.82 0.38 0 2 5 10 8.21 0.22 0 2 -5 -10 8.97 0.23 0 2 5 10 8.86 0.23 0 -2 -5 10 8.80 0.22 0 2 5 10 8.29 0.22 0 -2 5 -10 8.57 0.37 0 2 -5 -10 8.81 0.20 0 2 5 10 8.37 0.22 0 -2 -5 10 8.95 0.23 0 -2 5 10 8.11 0.23 0 2 -5 10 8.20 0.23 0 2 5 -10 8.67 0.19 0 2 5 -10 8.13 0.19 0 -2 5 10 8.81 0.23 0 2 -5 10 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20 1.17 0.25 0 1 2 20 1.04 0.17 0 -1 -2 20 1.12 0.17 0 1 2 -20 1.18 0.23 0 1 -2 20 1.28 0.21 0 1 2 -20 1.23 0.23 0 1 -2 20 1.17 0.43 0 -1 2 20 0.98 0.25 0 1 -2 20 1.24 0.17 0 -1 2 20 1.07 0.19 0 2 -2 -20 1.93 0.23 0 2 2 20 1.73 0.30 0 2 -2 -20 2.23 0.19 0 -2 -2 20 2.37 0.26 0 2 2 20 1.78 0.31 0 2 2 20 1.61 0.25 0 2 2 20 2.13 0.25 0 -2 -2 20 2.18 0.17 0 2 2 -20 2.29 0.17 0 2 -2 20 2.14 0.24 0 2 -2 20 1.87 0.18 0 -2 2 20 1.93 0.23 0 2 2 -20 2.15 0.23 0 -2 2 20 1.67 0.18 0 -3 -2 20 0.22 0.24 0 3 -2 -20 0.16 0.18 0 3 -2 -20 0.31 0.19 0 3 2 20 0.11 0.48 0 -3 -2 20 0.13 0.23 0 3 2 20 0.14 0.50 0 3 2 20 0.27 0.22 0 3 2 20 0.21 0.25 0 -3 2 20 0.23 0.22 0 3 2 -20 0.40 0.22 0 3 -2 20 0.20 0.18 0 -3 2 20 0.25 0.22 0 3 -2 20 0.19 0.18 0 3 2 -20 0.05 0.23 0 0 3 -20 0.41 0.27 0 0 -3 -20 0.02 0.21 0 0 -3 -20 0.37 0.18 0 0 -3 20 0.38 0.27 0 0 3 20 0.27 0.26 0 0 -3 20 0.17 0.23 0 0 3 20 0.10 0.21 0 1 3 20 1.36 0.22 0 1 -3 -20 1.04 0.22 0 1 -3 -20 1.37 0.22 0 -1 -3 20 1.21 0.26 0 1 3 20 1.15 0.26 0 1 3 20 0.82 0.18 0 -1 -3 20 1.04 0.23 0 1 3 -20 1.17 0.21 0 -1 3 20 0.93 0.25 0 1 -3 20 1.03 0.21 0 1 -3 20 1.23 0.23 0 -1 3 20 1.06 0.18 0 1 3 -20 1.18 0.26 0 2 -3 -20 4.68 0.24 0 2 3 20 3.43 0.29 0 2 -3 -20 3.95 0.21 0 -2 -3 20 4.04 0.28 0 2 3 20 3.77 0.30 0 2 3 20 3.48 0.23 0 2 3 20 3.90 0.24 0 -2 -3 20 3.85 0.26 0 -2 3 20 3.28 0.20 0 2 3 -20 4.10 0.27 0 2 -3 20 4.19 0.25 0 2 -3 20 3.93 0.25 0 -2 3 20 4.15 0.24 0 2 3 -20 4.14 0.28 0 -3 -3 20 0.52 0.18 0 3 -3 -20 0.80 0.22 0 3 3 20 0.45 0.33 0 3 -3 -20 0.61 0.23 0 -3 -3 20 0.59 0.25 0 3 3 20 0.54 0.21 0 3 3 20 0.52 0.32 0 3 3 20 0.81 0.18 0 -3 3 20 0.60 0.19 0 3 3 -20 0.74 0.22 0 3 -3 20 0.61 0.25 0 -3 3 20 0.54 0.22 0 3 -3 20 0.72 0.23 0 3 3 -20 0.66 0.24 0 0 4 -20 1.94 0.30 0 0 -4 -20 1.87 0.26 0 0 -4 -20 2.09 0.25 0 0 -4 20 1.66 0.30 0 0 4 20 1.80 0.26 0 0 -4 20 1.73 0.19 0 0 4 20 1.18 0.18 0 1 -4 -20 0.70 0.24 0 1 -4 -20 0.69 0.18 0 -1 -4 20 0.72 0.29 0 1 4 20 0.72 0.26 0 1 4 20 0.41 0.22 0 -1 -4 20 0.49 0.17 0 1 4 20 0.85 0.23 0 1 4 -20 0.64 0.22 0 1 -4 20 0.74 0.24 0 1 -4 20 0.81 0.25 0 -1 4 20 0.77 0.23 0 1 4 -20 0.58 0.26 0 -1 4 20 0.57 0.21 0 2 -4 -20 1.91 0.25 0 2 4 20 1.20 0.31 0 2 -4 -20 1.30 0.18 0 -2 -4 20 1.65 0.27 0 2 4 20 1.57 0.26 0 2 4 20 1.31 0.26 0 2 4 20 1.35 0.28 0 -2 -4 20 1.53 0.23 0 -2 4 20 1.24 0.22 0 2 -4 20 1.81 0.25 0 2 4 -20 1.52 0.19 0 2 -4 20 1.52 0.19 0 -2 4 20 1.41 0.25 0 2 4 -20 -0.01 0.22 0 -3 -4 20 1.08 0.26 0 3 -4 -20 0.89 0.27 0 3 4 20 0.83 0.31 0 3 -4 -20 1.27 0.22 0 -3 -4 20 1.22 0.25 0 3 4 20 0.78 0.28 0 3 4 20 1.14 0.25 0 3 4 20 0.83 0.31 0 -3 4 20 0.82 0.22 0 3 4 -20 1.03 0.23 0 3 -4 20 1.23 0.26 0 3 -4 20 0.95 0.23 0 -3 4 20 0.90 0.24 0 3 4 -20 1.22 0.27 0 0 5 -20 0.26 0.28 0 0 -5 -20 0.23 0.23 0 0 -5 -20 0.35 0.19 0 0 -5 20 0.18 0.29 0 0 -5 20 0.29 0.22 0 0 5 20 0.22 0.26 0 0 -5 20 0.22 0.18 0 0 5 20 0.28 0.23 0 1 -5 -20 2.50 0.25 0 1 5 20 2.69 0.22 0 1 5 20 1.98 0.27 0 1 -5 -20 2.71 0.27 0 -1 -5 20 2.63 0.29 0 1 5 20 2.21 0.27 0 -1 -5 20 2.56 0.20 0 1 5 20 1.90 0.26 0 -1 5 20 1.92 0.24 0 1 -5 20 2.67 0.20 0 1 5 -20 2.56 0.20 0 1 -5 20 2.01 0.26 0 -1 5 20 2.22 0.28 0 1 5 -20 2.60 0.30 0 2 -5 -20 0.35 0.23 0 2 5 20 0.37 0.24 0 2 -5 -20 0.43 0.27 0 -2 -5 20 0.27 0.27 0 2 5 20 0.63 0.28 0 2 5 20 0.27 0.24 0 2 5 20 0.41 0.24 0 -2 -5 20 0.60 0.24 0 -2 5 20 0.32 0.24 0 2 -5 20 0.26 0.19 0 2 5 -20 0.45 0.24 0 2 -5 20 0.39 0.23 0 -2 5 20 0.44 0.25 0 0 -6 -20 8.91 0.32 0 0 -6 -20 8.97 0.26 0 0 -6 20 7.51 0.41 0 0 -6 20 8.88 0.24 0 0 -6 20 9.00 0.28 0 0 6 20 8.22 0.32 0 0 6 20 6.58 0.28 0 0 6 -20 8.65 0.40 0 1 -6 -20 0.19 0.22 0 1 6 20 0.15 0.27 0 1 -6 -20 0.26 0.24 0 -1 -6 20 0.26 0.27 0 1 6 20 0.20 0.27 0 -1 -6 20 0.23 0.19 0 1 6 20 0.23 0.19 0 -1 6 20 0.23 0.24 0 1 6 -20 0.30 0.24 0 1 -6 20 0.27 0.23 0 -1 6 20 0.30 0.22 0 1 -6 20 0.31 0.24 0 1 6 -20 0.17 0.31 0 1 0 21 2.26 0.19 0 1 0 -21 1.64 0.23 0 1 0 21 1.71 0.34 0 -1 0 21 1.75 0.27 0 1 0 21 1.96 0.26 0 -1 0 21 1.73 0.19 0 2 0 -21 2.59 0.25 0 2 0 -21 2.60 0.19 0 -2 0 21 2.86 0.28 0 2 0 21 3.23 0.25 0 2 0 21 2.43 0.27 0 -2 0 21 2.46 0.20 0 0 1 -21 2.31 0.28 0 0 -1 -21 2.48 0.28 0 0 1 -21 2.22 0.26 0 0 -1 -21 2.28 0.27 0 0 -1 21 2.16 0.29 0 0 1 21 2.10 0.28 0 0 -1 21 1.85 0.19 0 0 1 21 2.02 0.26 0 1 -1 -21 0.00 0.22 0 1 -1 -21 2.18 0.24 0 -1 -1 21 2.14 0.28 0 1 1 21 2.01 0.31 0 1 1 21 1.91 0.20 0 -1 -1 21 2.31 0.19 0 1 1 21 2.61 0.24 0 1 1 -21 2.47 0.25 0 1 -1 21 2.40 0.26 0 1 1 -21 2.35 0.19 0 1 -1 21 2.05 0.43 0 -1 1 21 2.08 0.27 0 1 -1 21 2.18 0.26 0 -1 1 21 2.18 0.23 0 2 -1 -21 5.38 0.27 0 2 -1 -21 5.03 0.28 0 2 1 21 3.72 0.54 0 2 1 21 4.17 0.53 0 -2 -1 21 4.80 0.27 0 2 1 21 5.53 0.22 0 2 1 21 4.35 0.25 0 -2 -1 21 4.46 0.25 0 2 1 -21 5.25 0.27 0 2 1 -21 5.14 0.25 0 2 -1 21 5.67 0.25 0 -2 1 21 4.72 0.30 0 2 -1 21 4.81 0.27 0 -2 1 21 4.48 0.22 0 0 2 -21 0.20 0.29 0 0 -2 -21 0.12 0.26 0 0 -2 -21 0.35 0.27 0 0 -2 21 0.13 0.29 0 0 2 21 0.15 0.26 0 0 -2 21 0.08 0.22 0 0 2 21 0.11 0.18 0 1 -2 -21 0.55 0.25 0 1 -2 -21 0.45 0.26 0 -1 -2 21 0.53 0.27 0 1 2 21 0.44 0.27 0 1 2 21 0.51 0.26 0 -1 -2 21 0.43 0.18 0 1 2 21 0.61 0.27 0 1 2 -21 0.58 0.27 0 1 2 -21 0.53 0.18 0 -1 2 21 0.53 0.26 0 1 -2 21 0.42 0.18 0 1 -2 21 0.64 0.22 0 -1 2 21 0.47 0.19 0 2 -2 -21 2.44 0.28 0 2 2 21 1.96 0.32 0 2 -2 -21 2.50 0.21 0 -2 -2 21 2.44 0.29 0 2 2 21 2.69 0.24 0 2 2 21 1.91 0.35 0 2 2 21 1.88 0.24 0 -2 -2 21 2.17 0.19 0 2 2 -21 2.43 0.25 0 -2 2 21 2.21 0.25 0 2 2 -21 2.34 0.18 0 2 -2 21 2.35 0.24 0 -2 2 21 2.29 0.25 0 2 -2 21 2.49 0.23 0 0 3 -21 1.07 0.30 0 0 -3 -21 0.97 0.25 0 0 -3 21 0.96 0.30 0 0 3 21 1.01 0.27 0 0 -3 21 0.53 0.22 0 0 3 21 0.89 0.18 0 1 -3 -21 0.67 0.24 0 1 3 21 0.36 0.28 0 1 3 21 0.59 0.18 0 1 -3 -21 0.64 0.25 0 -1 -3 21 0.48 0.28 0 1 3 21 0.48 0.28 0 1 3 21 0.57 0.24 0 -1 -3 21 0.29 0.25 0 1 3 -21 0.59 0.28 0 1 3 -21 0.47 0.19 0 1 -3 21 0.76 0.22 0 -1 3 21 0.66 0.27 0 1 -3 21 0.43 0.21 0 -1 3 21 0.49 0.22 0 2 -3 -21 1.74 0.24 0 2 3 -21 1.44 0.20 0 0 4 -21 0.38 0.32 0 0 -4 -21 0.49 0.27 0 0 -4 -21 0.44 0.24 0 0 -4 21 0.33 0.32 0 0 4 21 0.37 0.27 0 0 -4 21 0.25 0.26 0 0 4 21 0.30 0.23 0 1 -4 -21 1.57 0.25 0 1 4 21 0.90 0.29 0 1 -4 -21 1.02 0.23 0 -1 -4 21 1.38 0.29 0 1 4 21 1.17 0.29 0 -1 -4 21 1.42 0.23 0 -1 4 21 1.31 0.27 0 1 -4 21 1.22 0.19 0 1 4 -21 1.42 0.29 0 ; _shelx_res_checksum 27498 _shelx_res_file ; TITL AXM666 in P212121 #19 CELL 0.71073 8.0638 12.312 17.2952 90 90 90 ZERR 4 0.0002 0.0004 0.0005 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 80 88 16 L.S. 13 0 0 511 PLAN 10 SIZE 0.18 0.23 0.61 TEMP -173 REM reset to P212121 #19 BOND $h conf acta fmap 2 REM /home/harms/xray/OC/hilt/Miersch/AXM666/AXM666.hkc WGHT 0.038400 0.101800 FVAR 0.16282 C1 1 0.088506 0.338796 0.306038 11.00000 0.01475 0.01488 = 0.01697 0.00069 0.00192 -0.00168 C2 1 0.124757 0.376030 0.383478 11.00000 0.01775 0.01478 = 0.01606 0.00002 0.00158 -0.00114 C3 1 0.212317 0.312266 0.433525 11.00000 0.01612 0.01626 = 0.01474 0.00077 0.00128 -0.00208 C4 1 0.268688 0.207510 0.408552 11.00000 0.01778 0.01620 = 0.01678 0.00080 -0.00010 0.00019 AFIX 43 H4 2 0.328407 0.162090 0.443141 11.00000 -1.20000 AFIX 0 C5 1 0.236895 0.173577 0.336025 11.00000 0.01400 0.01591 = 0.01705 0.00187 0.00036 -0.00049 C6 1 0.044421 0.480839 0.406791 11.00000 0.02054 0.01739 = 0.01411 0.00044 -0.00293 0.00122 C7 1 0.042804 0.672340 0.389060 11.00000 0.03875 0.01393 = 0.02805 0.00142 -0.00224 0.00534 AFIX 23 H7A 2 -0.077659 0.664950 0.398774 11.00000 -1.20000 H7B 2 0.058004 0.721656 0.344408 11.00000 -1.20000 AFIX 0 C8 1 0.125416 0.720193 0.459166 11.00000 0.05307 0.02098 = 0.03278 -0.00458 -0.00661 0.00447 AFIX 137 H8A 2 0.245621 0.722536 0.450988 11.00000 -1.50000 H8B 2 0.100684 0.675229 0.504479 11.00000 -1.50000 H8C 2 0.083783 0.794002 0.467724 11.00000 -1.50000 AFIX 0 C9 1 0.253470 0.347532 0.513472 11.00000 0.01603 0.01815 = 0.01590 -0.00149 -0.00043 0.00296 C10 1 0.317345 0.451089 0.528054 11.00000 0.02106 0.01832 = 0.01783 0.00111 0.00071 0.00034 AFIX 43 H10 2 0.332907 0.500561 0.486530 11.00000 -1.20000 AFIX 0 C11 1 0.358221 0.482099 0.602951 11.00000 0.02169 0.01911 = 0.02177 -0.00294 -0.00119 -0.00114 AFIX 43 H11 2 0.402425 0.552353 0.612500 11.00000 -1.20000 AFIX 0 C12 1 0.334306 0.410173 0.663780 11.00000 0.01802 0.02563 = 0.01605 -0.00397 -0.00136 0.00482 AFIX 43 H12 2 0.361248 0.431349 0.715084 11.00000 -1.20000 AFIX 0 C13 1 0.270941 0.307238 0.649491 11.00000 0.02111 0.02040 = 0.01621 0.00289 0.00019 0.00426 AFIX 43 H13 2 0.254014 0.258293 0.691214 11.00000 -1.20000 AFIX 0 C14 1 0.232207 0.275406 0.574735 11.00000 0.02035 0.01677 = 0.01903 -0.00060 -0.00061 0.00229 AFIX 43 H14 2 0.191116 0.204320 0.565285 11.00000 -1.20000 AFIX 0 C15 1 0.284971 0.068902 0.298611 11.00000 0.01709 0.01593 = 0.01660 -0.00225 -0.00047 -0.00059 AFIX 13 H15 2 0.180678 0.033050 0.280521 11.00000 -1.20000 AFIX 0 C16 1 0.369929 -0.009190 0.354872 11.00000 0.02287 0.01783 = 0.01826 -0.00154 -0.00087 0.00214 AFIX 23 H16A 2 0.296530 -0.022596 0.399753 11.00000 -1.20000 H16B 2 0.473993 0.023799 0.374132 11.00000 -1.20000 AFIX 0 C17 1 0.408730 -0.116919 0.314438 11.00000 0.02611 0.01762 = 0.02361 -0.00210 -0.00280 0.00459 AFIX 23 H17A 2 0.469531 -0.164958 0.350542 11.00000 -1.20000 H17B 2 0.303595 -0.153415 0.300340 11.00000 -1.20000 AFIX 0 C18 1 0.512567 -0.099737 0.241830 11.00000 0.02094 0.02055 = 0.02929 -0.00723 0.00077 0.00251 AFIX 23 H18A 2 0.527936 -0.170217 0.215224 11.00000 -1.20000 H18B 2 0.623415 -0.072160 0.256665 11.00000 -1.20000 AFIX 0 C19 1 0.431008 -0.019538 0.186513 11.00000 0.02593 0.02322 = 0.02096 -0.00474 0.00438 0.00073 AFIX 23 H19A 2 0.326318 -0.050960 0.166671 11.00000 -1.20000 H19B 2 0.505358 -0.006560 0.141908 11.00000 -1.20000 AFIX 0 C20 1 0.394239 0.088496 0.226885 11.00000 0.02224 0.01978 = 0.01942 -0.00047 0.00316 0.00096 AFIX 23 H20A 2 0.336425 0.137917 0.190660 11.00000 -1.20000 H20B 2 0.499548 0.123380 0.242668 11.00000 -1.20000 AFIX 0 O1 3 0.007367 0.386108 0.257788 11.00000 0.02148 0.01971 = 0.01744 0.00241 -0.00263 0.00146 O2 3 0.150106 0.238345 0.285757 11.00000 0.01789 0.01598 = 0.01509 -0.00013 -0.00163 0.00076 O3 3 -0.068490 0.486376 0.451998 11.00000 0.02598 0.02233 = 0.02655 -0.00078 0.00647 0.00321 O4 3 0.112903 0.565965 0.370859 11.00000 0.02988 0.01525 = 0.02175 0.00217 0.00251 0.00130 HKLF 4 REM AXM666 in P212121 #19 REM R1 = 0.0309 for 3483 Fo > 4sig(Fo) and 0.0326 for all 3641 data REM 218 parameters refined using 0 restraints END WGHT 0.0384 0.1018 REM Highest difference peak 0.167, deepest hole -0.170, 1-sigma level 0.036 Q1 1 0.1124 0.3639 0.3465 11.00000 0.05 0.17 Q2 1 0.2573 0.4061 0.5258 11.00000 0.05 0.13 Q3 1 0.4623 -0.1114 0.2794 11.00000 0.05 0.12 Q4 1 0.2248 0.3290 0.4725 11.00000 0.05 0.12 Q5 1 0.3400 0.0789 0.2628 11.00000 0.05 0.11 Q6 1 0.4098 0.0329 0.2078 11.00000 0.05 0.11 Q7 1 0.0856 0.4234 0.3943 11.00000 0.05 0.11 Q8 1 0.2071 0.1782 0.3782 11.00000 0.05 0.11 Q9 1 -0.0667 0.6806 0.3545 11.00000 0.05 0.11 Q10 1 0.1194 0.2204 0.2388 11.00000 0.05 0.11 ; _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. ; _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957488' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AXM669_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 O4' _chemical_formula_weight 300.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7240(4) _cell_length_b 16.7441(6) _cell_length_c 9.1552(3) _cell_angle_alpha 90 _cell_angle_beta 104.301(2) _cell_angle_gamma 90 _cell_volume 1593.00(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 143 _cell_measurement_theta_min 2.6456 _cell_measurement_theta_max 21.9880 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.252 _exptl_crystal_F_000 640 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.130 _exptl_absorpt_coefficient_mu 0.088 _shelx_estimated_absorpt_T_min 0.968 _shelx_estimated_absorpt_T_max 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker D8 QUEST area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 19656 _diffrn_reflns_av_unetI/netI 0.0245 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.307 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2951 _reflns_number_gt 2449 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'BRUKER APEX II' _computing_cell_refinement 'APEX2 v2013.4-1 (Bruker AXS)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; ; _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^)+(0.0321P)^2^+0.6180P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2951 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.57133(8) 0.27796(5) 0.27127(10) 0.0179(2) Uani 1 1 d . . . . . O2 O 0.53822(9) 0.40765(6) 0.28782(11) 0.0241(2) Uani 1 1 d . . . . . O3 O 0.78244(9) 0.48420(5) 0.15507(11) 0.0228(2) Uani 1 1 d . . . . . O4 O 0.81637(10) 0.49045(6) 0.40722(11) 0.0262(2) Uani 1 1 d . . . . . C1 C 0.61464(13) 0.35600(8) 0.28025(14) 0.0170(3) Uani 1 1 d . . . . . C2 C 0.74776(12) 0.36797(7) 0.27769(14) 0.0155(3) Uani 1 1 d . . . . . C3 C 0.82211(12) 0.30602(8) 0.25265(13) 0.0143(3) Uani 1 1 d . . . . . C4 C 0.76645(12) 0.22743(7) 0.23700(14) 0.0157(3) Uani 1 1 d . . . . . H4 H 0.8161 0.1835 0.2178 0.019 Uiso 1 1 calc R U . . . C5 C 0.64581(12) 0.21487(7) 0.24895(14) 0.0154(3) Uani 1 1 d . . . . . C6 C 0.78736(12) 0.45400(8) 0.29069(15) 0.0172(3) Uani 1 1 d . . . . . C7 C 0.81831(14) 0.56792(8) 0.14927(18) 0.0288(4) Uani 1 1 d . . . . . H7A H 0.7902 0.5982 0.2284 0.035 Uiso 1 1 calc R U . . . H7B H 0.7744 0.5908 0.0502 0.035 Uiso 1 1 calc R U . . . C8 C 0.96132(15) 0.57594(9) 0.17273(19) 0.0314(4) Uani 1 1 d . . . . . H8A H 0.9828 0.6316 0.1569 0.047 Uiso 1 1 calc R U . . . H8B H 0.9903 0.5416 0.1009 0.047 Uiso 1 1 calc R U . . . H8C H 1.0042 0.5598 0.2758 0.047 Uiso 1 1 calc R U . . . C9 C 0.95739(12) 0.31584(7) 0.24194(14) 0.0147(3) Uani 1 1 d . . . . . C10 C 1.04105(12) 0.36985(7) 0.33367(14) 0.0159(3) Uani 1 1 d . . . . . H10 H 1.0112 0.4018 0.4038 0.019 Uiso 1 1 calc R U . . . C11 C 1.16711(13) 0.37713(8) 0.32295(15) 0.0179(3) Uani 1 1 d . . . . . H11 H 1.2228 0.4145 0.3849 0.021 Uiso 1 1 calc R U . . . C12 C 1.21247(13) 0.33031(8) 0.22262(15) 0.0202(3) Uani 1 1 d . . . . . H12 H 1.2994 0.3349 0.2167 0.024 Uiso 1 1 calc R U . . . C13 C 1.13033(13) 0.27666(8) 0.13077(16) 0.0209(3) Uani 1 1 d . . . . . H13 H 1.1608 0.2448 0.0610 0.025 Uiso 1 1 calc R U . . . C14 C 1.00399(13) 0.26938(8) 0.14055(15) 0.0178(3) Uani 1 1 d . . . . . H14 H 0.9485 0.2323 0.0775 0.021 Uiso 1 1 calc R U . . . C15 C 0.57508(12) 0.13660(8) 0.24359(15) 0.0176(3) Uani 1 1 d . . . . . C16 C 0.65957(14) 0.06737(8) 0.21630(17) 0.0253(3) Uani 1 1 d . . . . . H16A H 0.6827 0.0755 0.1203 0.038 Uiso 1 1 calc R U . . . H16B H 0.6122 0.0171 0.2128 0.038 Uiso 1 1 calc R U . . . H16C H 0.7380 0.0652 0.2983 0.038 Uiso 1 1 calc R U . . . C17 C 0.45083(13) 0.13948(8) 0.11645(16) 0.0220(3) Uani 1 1 d . . . . . H17A H 0.4724 0.1494 0.0201 0.033 Uiso 1 1 calc R U . . . H17B H 0.3954 0.1825 0.1365 0.033 Uiso 1 1 calc R U . . . H17C H 0.4055 0.0884 0.1118 0.033 Uiso 1 1 calc R U . . . C18 C 0.54028(14) 0.12418(9) 0.39481(16) 0.0240(3) Uani 1 1 d . . . . . H18A H 0.4937 0.0736 0.3925 0.036 Uiso 1 1 calc R U . . . H18B H 0.4857 0.1683 0.4123 0.036 Uiso 1 1 calc R U . . . H18C H 0.6192 0.1226 0.4762 0.036 Uiso 1 1 calc R U . . . 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 0.0136(5) 0.0166(5) 0.0249(5) -0.0005(4) 0.0075(4) -0.0002(4) O2 0.0196(5) 0.0194(5) 0.0366(6) -0.0004(4) 0.0129(4) 0.0048(4) O3 0.0239(5) 0.0187(5) 0.0243(5) 0.0042(4) 0.0034(4) -0.0058(4) O4 0.0309(6) 0.0224(5) 0.0277(6) -0.0090(4) 0.0116(4) -0.0025(4) C1 0.0183(7) 0.0175(7) 0.0159(7) -0.0002(5) 0.0054(5) 0.0004(5) C2 0.0152(6) 0.0168(7) 0.0146(6) 0.0000(5) 0.0042(5) -0.0008(5) C3 0.0132(6) 0.0187(7) 0.0106(6) 0.0014(5) 0.0022(5) -0.0002(5) C4 0.0136(7) 0.0149(6) 0.0189(7) -0.0010(5) 0.0048(5) 0.0008(5) C5 0.0152(7) 0.0160(7) 0.0146(6) 0.0010(5) 0.0027(5) 0.0025(5) C6 0.0119(6) 0.0184(7) 0.0226(7) -0.0004(6) 0.0066(5) 0.0027(5) C7 0.0281(8) 0.0172(7) 0.0397(9) 0.0075(6) 0.0055(7) -0.0061(6) C8 0.0292(9) 0.0251(8) 0.0418(9) -0.0031(7) 0.0123(7) -0.0097(6) C9 0.0144(6) 0.0133(6) 0.0162(6) 0.0037(5) 0.0035(5) 0.0006(5) C10 0.0170(7) 0.0137(6) 0.0165(7) 0.0016(5) 0.0035(5) 0.0007(5) C11 0.0156(7) 0.0173(7) 0.0190(7) 0.0018(5) 0.0008(5) -0.0035(5) C12 0.0127(7) 0.0234(7) 0.0249(7) 0.0036(6) 0.0054(6) -0.0015(5) C13 0.0177(7) 0.0238(7) 0.0233(7) -0.0035(6) 0.0087(6) 0.0007(5) C14 0.0162(7) 0.0179(7) 0.0192(7) -0.0024(5) 0.0040(5) -0.0022(5) C15 0.0136(7) 0.0183(7) 0.0208(7) 0.0004(5) 0.0042(5) -0.0027(5) C16 0.0198(7) 0.0152(7) 0.0421(9) -0.0011(6) 0.0098(7) -0.0032(5) C17 0.0158(7) 0.0270(7) 0.0223(7) -0.0017(6) 0.0031(6) -0.0054(6) C18 0.0221(7) 0.0275(8) 0.0221(7) 0.0046(6) 0.0052(6) -0.0046(6) _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 C5 1.3698(15) . ? O1 C1 1.3824(15) . ? O2 C1 1.2051(16) . ? O3 C6 1.3295(16) . ? O3 C7 1.4581(16) . ? O4 C6 1.2015(16) . ? C1 C2 1.4475(18) . ? C2 C3 1.3618(18) . ? C2 C6 1.4982(18) . ? C3 C4 1.4374(17) . ? C3 C9 1.4872(18) . ? C4 C5 1.3416(18) . ? C4 H4 0.9500 . ? C5 C15 1.5090(18) . ? C7 C8 1.501(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.3948(19) . ? C9 C10 1.3985(18) . ? C10 C11 1.3847(19) . ? C10 H10 0.9500 . ? C11 C12 1.384(2) . ? C11 H11 0.9500 . ? C12 C13 1.3871(19) . ? C12 H12 0.9500 . ? C13 C14 1.3851(19) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.5293(19) . ? C15 C18 1.5344(19) . ? C15 C17 1.5383(18) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C5 O1 C1 122.56(10) . . ? C6 O3 C7 116.72(11) . . ? O2 C1 O1 117.28(12) . . ? O2 C1 C2 126.09(12) . . ? O1 C1 C2 116.62(11) . . ? C3 C2 C1 121.20(12) . . ? C3 C2 C6 125.42(12) . . ? C1 C2 C6 113.15(11) . . ? C2 C3 C4 117.91(12) . . ? C2 C3 C9 123.24(12) . . ? C4 C3 C9 118.85(11) . . ? C5 C4 C3 121.36(12) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 O1 120.05(11) . . ? C4 C5 C15 128.36(12) . . ? O1 C5 C15 111.58(11) . . ? O4 C6 O3 125.30(12) . . ? O4 C6 C2 124.41(12) . . ? O3 C6 C2 110.27(11) . . ? O3 C7 C8 110.50(12) . . ? O3 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O3 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 118.56(12) . . ? C14 C9 C3 119.86(11) . . ? C10 C9 C3 121.57(12) . . ? C11 C10 C9 120.47(12) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.43(12) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.64(13) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.17(13) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.73(12) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C5 C15 C16 110.50(11) . . ? C5 C15 C18 108.70(11) . . ? C16 C15 C18 109.31(11) . . ? C5 C15 C17 109.38(11) . . ? C16 C15 C17 109.73(11) . . ? C18 C15 C17 109.19(11) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 O1 C1 O2 174.14(11) . . . . ? C5 O1 C1 C2 -5.10(17) . . . . ? O2 C1 C2 C3 -172.86(13) . . . . ? O1 C1 C2 C3 6.30(18) . . . . ? O2 C1 C2 C6 1.89(19) . . . . ? O1 C1 C2 C6 -178.96(10) . . . . ? C1 C2 C3 C4 -3.35(18) . . . . ? C6 C2 C3 C4 -177.42(12) . . . . ? C1 C2 C3 C9 177.09(11) . . . . ? C6 C2 C3 C9 3.0(2) . . . . ? C2 C3 C4 C5 -1.04(18) . . . . ? C9 C3 C4 C5 178.53(12) . . . . ? C3 C4 C5 O1 2.31(19) . . . . ? C3 C4 C5 C15 -176.61(12) . . . . ? C1 O1 C5 C4 0.95(18) . . . . ? C1 O1 C5 C15 -179.96(11) . . . . ? C7 O3 C6 O4 1.52(19) . . . . ? C7 O3 C6 C2 179.92(11) . . . . ? C3 C2 C6 O4 -105.09(16) . . . . ? C1 C2 C6 O4 80.43(16) . . . . ? C3 C2 C6 O3 76.50(16) . . . . ? C1 C2 C6 O3 -97.98(13) . . . . ? C6 O3 C7 C8 85.85(16) . . . . ? C2 C3 C9 C14 -143.73(13) . . . . ? C4 C3 C9 C14 36.72(17) . . . . ? C2 C3 C9 C10 37.53(18) . . . . ? C4 C3 C9 C10 -142.02(12) . . . . ? C14 C9 C10 C11 0.38(18) . . . . ? C3 C9 C10 C11 179.13(11) . . . . ? C9 C10 C11 C12 -0.82(19) . . . . ? C10 C11 C12 C13 1.0(2) . . . . ? C11 C12 C13 C14 -0.7(2) . . . . ? C12 C13 C14 C9 0.2(2) . . . . ? C10 C9 C14 C13 -0.09(19) . . . . ? C3 C9 C14 C13 -178.87(12) . . . . ? C4 C5 C15 C16 -1.83(19) . . . . ? O1 C5 C15 C16 179.18(11) . . . . ? C4 C5 C15 C18 118.13(15) . . . . ? O1 C5 C15 C18 -60.87(13) . . . . ? C4 C5 C15 C17 -122.73(14) . . . . ? O1 C5 C15 C17 58.27(14) . . . . ? _refine_diff_density_max 0.212 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.038 _shelxl_version_number 2013-3 _shelx_res_file ; TITL AXM669_0ma in P2(1)/c CELL 0.71073 10.7240 16.7441 9.1552 90.000 104.301 90.000 ZERR 4.00 0.0004 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H O UNIT 72 80 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 ACTA size .13 .16 .37 omit -2 51 L.S. 12 FMAP 2 PLAN -4 0 0.00 HTAB BOND $H CONF WGHT 0.032100 0.618000 FVAR 0.37726 O1 3 0.571334 0.277964 0.271275 11.00000 0.01363 0.01658 = 0.02493 -0.00054 0.00753 -0.00025 O2 3 0.538216 0.407645 0.287820 11.00000 0.01955 0.01942 = 0.03656 -0.00035 0.01286 0.00475 O3 3 0.782436 0.484201 0.155071 11.00000 0.02388 0.01872 = 0.02431 0.00418 0.00338 -0.00581 O4 3 0.816366 0.490449 0.407225 11.00000 0.03089 0.02236 = 0.02772 -0.00900 0.01158 -0.00255 C1 1 0.614640 0.356002 0.280247 11.00000 0.01833 0.01755 = 0.01588 -0.00021 0.00541 0.00036 C2 1 0.747764 0.367969 0.277688 11.00000 0.01520 0.01680 = 0.01463 0.00002 0.00420 -0.00077 C3 1 0.822105 0.306018 0.252646 11.00000 0.01318 0.01866 = 0.01061 0.00144 0.00219 -0.00016 C4 1 0.766447 0.227429 0.237004 11.00000 0.01357 0.01490 = 0.01892 -0.00103 0.00484 0.00083 AFIX 43 H4 2 0.816116 0.183474 0.217811 11.00000 -1.20000 AFIX 0 C5 1 0.645809 0.214867 0.248948 11.00000 0.01521 0.01599 = 0.01461 0.00100 0.00269 0.00246 C6 1 0.787358 0.454002 0.290688 11.00000 0.01189 0.01840 = 0.02261 -0.00044 0.00664 0.00275 C7 1 0.818308 0.567924 0.149272 11.00000 0.02811 0.01716 = 0.03974 0.00745 0.00546 -0.00611 AFIX 23 H7A 2 0.790184 0.598185 0.228377 11.00000 -1.20000 H7B 2 0.774378 0.590763 0.050177 11.00000 -1.20000 AFIX 0 C8 1 0.961320 0.575943 0.172733 11.00000 0.02921 0.02508 = 0.04178 -0.00313 0.01231 -0.00972 AFIX 137 H8A 2 0.982819 0.631637 0.156880 11.00000 -1.50000 H8B 2 0.990264 0.541629 0.100856 11.00000 -1.50000 H8C 2 1.004238 0.559798 0.275778 11.00000 -1.50000 AFIX 0 C9 1 0.957391 0.315839 0.241936 11.00000 0.01436 0.01333 = 0.01622 0.00374 0.00347 0.00063 C10 1 1.041053 0.369848 0.333667 11.00000 0.01702 0.01372 = 0.01651 0.00156 0.00351 0.00072 AFIX 43 H10 2 1.011190 0.401768 0.403832 11.00000 -1.20000 AFIX 0 C11 1 1.167108 0.377130 0.322948 11.00000 0.01559 0.01727 = 0.01904 0.00182 0.00081 -0.00353 AFIX 43 H11 2 1.222817 0.414504 0.384859 11.00000 -1.20000 AFIX 0 C12 1 1.212465 0.330310 0.222620 11.00000 0.01274 0.02342 = 0.02489 0.00357 0.00545 -0.00152 AFIX 43 H12 2 1.299377 0.334892 0.216697 11.00000 -1.20000 AFIX 0 C13 1 1.130332 0.276659 0.130768 11.00000 0.01768 0.02376 = 0.02328 -0.00355 0.00873 0.00067 AFIX 43 H13 2 1.160811 0.244824 0.060970 11.00000 -1.20000 AFIX 0 C14 1 1.003988 0.269383 0.140550 11.00000 0.01615 0.01785 = 0.01918 -0.00243 0.00399 -0.00215 AFIX 43 H14 2 0.948461 0.232344 0.077513 11.00000 -1.20000 AFIX 0 C15 1 0.575082 0.136596 0.243587 11.00000 0.01361 0.01827 = 0.02082 0.00038 0.00421 -0.00274 C16 1 0.659568 0.067372 0.216296 11.00000 0.01981 0.01520 = 0.04210 -0.00107 0.00982 -0.00320 AFIX 137 H16A 2 0.682692 0.075453 0.120269 11.00000 -1.50000 H16B 2 0.612184 0.017077 0.212791 11.00000 -1.50000 H16C 2 0.737971 0.065226 0.298339 11.00000 -1.50000 AFIX 0 C17 1 0.450830 0.139483 0.116448 11.00000 0.01579 0.02696 = 0.02229 -0.00168 0.00309 -0.00543 AFIX 137 H17A 2 0.472429 0.149363 0.020079 11.00000 -1.50000 H17B 2 0.395431 0.182548 0.136484 11.00000 -1.50000 H17C 2 0.405475 0.088377 0.111786 11.00000 -1.50000 AFIX 0 C18 1 0.540277 0.124179 0.394806 11.00000 0.02211 0.02746 = 0.02212 0.00462 0.00515 -0.00461 AFIX 137 H18A 2 0.493718 0.073646 0.392456 11.00000 -1.50000 H18B 2 0.485733 0.168321 0.412305 11.00000 -1.50000 H18C 2 0.619152 0.122640 0.476238 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM AXM669_0ma in P2(1)/c REM R1 = 0.0334 for 2449 Fo > 4sig(Fo) and 0.0466 for all 2951 data REM 203 parameters refined using 0 restraints END WGHT 0.0320 0.6180 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.212, deepest hole -0.183, 1-sigma level 0.038 Q1 1 0.6163 0.1715 0.2373 11.00000 0.05 0.21 Q2 1 0.7786 0.3439 0.2184 11.00000 0.05 0.21 Q3 1 0.5218 0.1389 0.1812 11.00000 0.05 0.19 Q4 1 0.9833 0.3606 0.2456 11.00000 0.05 0.19 ; _shelx_res_checksum 81774 _shelx_hkl_file ; -2 0 0 -0.7619 0.37333 1 2 0 0 -0.6756 0.29835 1 3 0 0 864.536 17.0779 1 -3 0 0 864.669 17.0636 1 -4 0 0 517.196 10.5975 1 4 0 0 521.472 10.6405 1 -5 0 0 2324.24 44.9036 1 5 0 0 2276.28 44.9342 1 -6 0 0 39.4587 1.63552 1 6 0 0 40.2779 1.65917 1 -7 0 0 16.2680 1.36496 1 7 0 0 16.4208 1.46014 1 8 0 0 120.951 3.67199 1 -8 0 0 125.961 3.55982 1 -9 0 0 71.0645 2.86086 1 9 0 0 83.8262 3.02284 1 10 0 0 70.4204 3.25930 1 -10 0 0 66.9195 2.92680 1 11 0 0 3.32486 1.42904 1 -11 0 0 4.26112 1.58751 1 -12 0 0 24.8311 2.62024 1 12 0 0 18.4379 2.28619 1 13 0 0 7.57768 2.86919 1 -13 0 0 7.15304 2.06029 1 -1 -1 0 479.309 9.95892 1 -1 -1 0 537.537 10.4018 3 -2 -1 0 1435.44 29.1103 3 2 -1 0 1472.19 29.3715 3 2 -1 0 1408.38 28.4987 1 -2 -1 0 1435.64 28.4184 1 -2 1 0 1390.66 28.4464 1 2 1 0 1414.63 28.1594 1 3 -1 0 67.7557 1.84126 1 -3 -1 0 67.1550 1.78637 1 -3 -1 0 70.1921 1.48180 3 3 -1 0 70.7677 1.59508 3 -3 1 0 67.2483 1.83632 1 3 1 0 67.8594 1.84768 1 4 -1 0 99.6673 2.18386 3 -4 -1 0 96.8266 2.51278 1 4 -1 0 99.7187 2.56974 1 -4 1 0 98.0351 2.54997 1 4 1 0 95.3258 2.54206 1 5 -1 0 140.102 2.96533 3 -5 -1 0 138.474 3.43616 1 5 -1 0 135.360 3.52156 1 -5 1 0 136.952 3.51030 1 5 1 0 139.629 3.46458 1 6 -1 0 10.4408 1.03919 1 -6 -1 0 9.78096 0.97145 1 6 1 0 9.22437 1.01227 1 -6 1 0 11.3250 0.99971 1 7 -1 0 8.89735 1.09745 1 -7 -1 0 7.86153 1.05163 1 7 1 0 10.7663 1.06615 1 -7 1 0 11.4389 1.17847 1 -8 -1 0 17.0970 1.55741 1 8 -1 0 19.0309 1.76880 1 -8 1 0 19.0420 1.71662 1 8 1 0 22.5078 1.56957 1 -9 -1 0 -0.9260 1.02020 1 9 -1 0 0.28013 1.18499 1 9 1 0 -0.0081 1.27279 1 -9 1 0 1.05848 1.07561 1 -10 -1 0 1.89695 0.99924 1 10 -1 0 3.98797 1.44764 1 10 1 0 -2.6267 1.48053 1 -10 1 0 -2.2071 1.19238 1 -11 -1 0 37.3981 2.49540 1 11 -1 0 39.7374 2.71252 1 11 1 0 45.1352 2.79696 1 -11 1 0 37.1708 2.69915 1 12 -1 0 5.38924 2.02992 1 -12 -1 0 4.92270 1.65529 1 12 1 0 -1.9045 2.25958 1 -12 1 0 7.54061 1.89182 1 -13 -1 0 -1.9551 2.19703 1 13 -1 0 1.62361 2.74440 1 -13 1 0 2.68879 2.01293 1 13 1 0 6.19364 2.25557 1 0 -2 0 133.897 2.98317 3 1 -2 0 2.46829 0.38358 3 -1 -2 0 1.72914 0.35182 1 -1 -2 0 2.62266 0.33562 3 1 -2 0 2.93205 0.37470 2 1 -2 0 2.27255 0.33966 1 1 2 0 2.02101 0.34836 1 -1 2 0 1.88225 0.34876 1 -1 2 0 2.19976 0.38138 2 1 2 0 2.20914 0.35476 1 2 -2 0 491.086 10.0772 1 -2 -2 0 514.658 10.4008 3 -2 -2 0 493.323 10.0087 1 2 -2 0 521.330 10.4832 3 -2 2 0 497.525 10.0896 1 2 2 0 503.206 10.0398 1 -3 -2 0 181.885 3.79682 3 3 -2 0 181.821 3.91338 3 3 -2 0 172.496 3.96814 1 -3 -2 0 176.054 3.88899 1 3 2 0 175.612 3.91629 1 -3 2 0 175.591 4.00587 1 -4 -2 0 76.2936 1.72438 3 4 -2 0 76.7081 1.88877 3 -4 -2 0 77.7531 2.10234 1 4 -2 0 74.6070 2.15341 1 -4 2 0 75.0379 2.16498 1 4 2 0 74.4238 2.08897 1 5 -2 0 3.94528 0.76199 1 -5 -2 0 4.06507 0.60634 1 5 -2 0 3.95396 0.48537 3 5 2 0 3.66735 0.71343 1 -5 2 0 3.92512 0.66094 1 6 -2 0 40.4312 1.78886 1 6 -2 0 39.5538 1.18074 3 -6 -2 0 37.4697 1.62340 1 6 2 0 41.5904 1.76286 1 -6 2 0 37.0472 1.68732 1 7 -2 0 151.136 4.01888 1 -7 -2 0 143.711 3.79436 1 7 -2 0 149.195 3.16125 3 7 2 0 145.266 3.92863 1 -7 2 0 140.175 3.95345 1 -8 -2 0 43.5245 1.98640 1 8 -2 0 44.1116 2.09186 1 8 2 0 41.5383 1.98325 1 -8 2 0 40.1824 2.12539 1 -9 -2 0 0.07788 1.01166 1 9 -2 0 2.68643 1.03083 1 -9 2 0 2.21366 1.15270 1 9 2 0 0.94354 1.04058 1 -10 -2 0 15.2548 1.60740 1 10 -2 0 20.1719 1.87134 1 -10 2 0 17.5574 1.59083 1 10 2 0 16.7161 1.76750 1 11 -2 0 0.17913 1.45963 1 -11 -2 0 2.85609 1.39259 1 -11 2 0 3.45341 1.25621 1 11 2 0 1.43897 1.48075 1 -12 -2 0 8.65640 1.66099 1 12 -2 0 7.18340 2.09155 1 12 2 0 4.74308 2.27984 1 -12 2 0 6.64005 1.90709 1 13 -2 0 -3.0617 2.22968 1 -13 -2 0 -1.4389 1.85799 1 13 2 0 1.01709 2.71586 1 -13 2 0 -1.0165 2.17600 1 0 -3 0 -0.2211 0.28669 1 0 -3 0 0.02225 0.35219 1 0 -3 0 -0.3384 0.29428 3 0 3 0 0.03899 0.33266 1 0 3 0 -0.3428 0.29963 1 1 -3 0 2.74929 0.44692 1 -1 -3 0 2.23326 0.41653 1 1 -3 0 2.24250 0.41505 3 -1 -3 0 2.81649 0.41714 3 -1 3 0 2.18866 0.41381 2 1 3 0 1.83489 0.41715 1 -1 3 0 2.76289 0.45060 1 1 3 0 2.65219 0.42433 1 2 -3 0 230.205 5.01087 1 -2 -3 0 240.369 5.12725 3 -2 -3 0 230.806 4.93468 1 2 -3 0 240.505 5.19401 3 2 3 0 238.913 4.98573 1 -2 3 0 233.729 5.46807 2 -2 3 0 230.613 5.02271 1 2 3 0 235.449 4.86516 1 3 -3 0 12.3227 0.78538 3 3 -3 0 15.0770 0.90585 1 -3 -3 0 13.2561 0.66756 3 -3 -3 0 14.0045 0.86785 1 3 3 0 14.6047 0.81635 1 -3 3 0 14.9531 0.90760 1 3 3 0 14.9878 0.71554 1 4 -3 0 7.37026 0.68699 3 -4 -3 0 7.87002 0.84377 1 4 -3 0 8.24902 0.85415 1 -4 -3 0 7.42382 0.57008 3 4 3 0 8.20060 0.74107 1 -4 3 0 8.20662 0.87984 1 5 -3 0 9.76693 1.00442 1 -5 -3 0 10.9794 0.61349 3 5 -3 0 11.6392 0.87624 3 -5 -3 0 10.4581 0.98538 1 -5 3 0 11.1267 1.03923 1 5 3 0 9.43510 1.01172 1 6 -3 0 201.086 4.59714 3 -6 -3 0 204.562 4.31347 3 -6 -3 0 207.723 4.83135 1 6 -3 0 207.267 5.03262 1 -6 3 0 204.765 5.05342 1 6 3 0 202.140 4.92120 1 -7 -3 0 31.4749 1.66811 1 7 -3 0 35.4906 1.26190 3 7 -3 0 34.7302 1.94336 1 -7 3 0 37.0278 1.97477 1 7 3 0 35.3246 1.69764 1 -8 -3 0 113.007 3.35613 1 8 -3 0 113.455 3.61977 1 8 -3 0 115.061 2.67260 3 8 3 0 115.437 3.60331 1 -8 3 0 115.631 3.54396 1 -9 -3 0 10.3931 1.30091 1 9 -3 0 13.1726 1.49511 1 9 3 0 11.9739 1.44164 1 -9 3 0 10.1338 1.27590 1 -10 -3 0 -0.2241 1.19392 1 10 -3 0 0.33107 1.20873 1 -10 3 0 0.01131 1.38083 1 10 3 0 0.18641 1.19637 1 11 -3 0 27.3680 2.59060 1 -11 -3 0 21.1996 2.18063 1 11 3 0 19.8680 2.09248 1 -11 3 0 17.9342 1.98574 1 12 -3 0 20.2079 2.80217 1 -12 -3 0 18.2283 1.92474 1 -12 3 0 14.0393 1.85023 1 12 3 0 19.2235 2.32608 1 13 -3 0 -2.7576 2.82119 1 -13 -3 0 2.53772 2.19202 1 13 3 0 -3.8261 2.26556 1 -13 3 0 6.58660 2.34226 1 0 -4 0 193.249 4.40176 3 0 -4 0 188.399 4.08303 1 0 -4 0 192.570 4.16787 1 0 4 0 189.651 4.10274 1 0 4 0 187.813 4.16222 1 -1 -4 0 673.630 13.8429 1 1 -4 0 697.937 13.8697 1 -1 -4 0 718.639 14.6176 3 1 -4 0 710.231 14.6483 3 1 4 0 689.120 13.8735 1 -1 4 0 683.540 13.9120 1 -1 4 0 722.817 14.9893 2 -1 4 0 695.347 13.8791 1 1 4 0 686.864 13.7782 1 2 -4 0 837.911 17.1097 3 -2 -4 0 836.114 17.0408 3 -2 -4 0 807.295 16.2133 1 2 -4 0 799.616 16.2741 1 -2 4 0 805.413 17.7204 2 -2 4 0 802.006 16.2951 1 2 4 0 857.489 16.1485 1 2 4 0 802.994 16.2400 1 3 -4 0 3.60260 0.52719 3 3 -4 0 3.54490 0.56764 1 -3 -4 0 3.31563 0.49431 3 -3 -4 0 3.26923 0.55485 1 3 4 0 3.66218 0.46074 1 -3 4 0 3.15349 0.60013 1 -3 4 0 3.56968 0.64042 2 3 4 0 2.59178 0.51155 1 4 -4 0 27.5842 1.20242 3 -4 -4 0 26.9118 1.03638 3 -4 -4 0 24.3316 1.21273 1 4 -4 0 27.3125 1.30899 1 4 4 0 26.5824 1.07741 1 4 4 0 24.7599 1.17126 1 -4 4 0 25.6898 1.32080 1 5 -4 0 94.2847 2.48875 3 -5 -4 0 90.5020 2.24597 3 5 -4 0 88.8658 2.67114 1 -5 -4 0 90.7201 2.55664 1 5 4 0 90.6985 2.63134 1 -5 4 0 87.3239 2.69564 1 6 -4 0 21.2402 1.41583 1 6 -4 0 20.5136 1.12307 3 -6 -4 0 20.0628 0.91053 3 -6 -4 0 20.2852 1.19895 1 6 4 0 21.6673 1.35851 1 -6 4 0 19.6713 1.57179 1 -7 -4 0 16.3714 0.79216 3 -7 -4 0 16.2478 1.36690 1 7 -4 0 16.8372 1.14926 3 7 -4 0 18.9592 1.51064 1 -7 4 0 18.2587 1.54830 1 7 4 0 17.3064 1.32234 1 8 -4 0 12.2085 1.15663 3 -8 -4 0 17.0081 1.53214 1 8 -4 0 14.9709 1.48233 1 8 4 0 14.5405 1.47310 1 -8 4 0 16.5340 1.66478 1 9 -4 0 51.9534 1.64234 3 -9 -4 0 52.0811 2.33553 1 9 -4 0 50.8123 2.85942 1 9 4 0 47.5007 2.60430 1 -9 4 0 53.5165 2.54915 1 10 -4 0 74.2752 3.25263 1 -10 -4 0 66.4967 2.81493 1 10 4 0 65.0458 3.02835 1 -10 4 0 72.8279 3.19460 1 11 -4 0 8.64458 2.13989 1 -11 -4 0 7.50132 1.41995 1 11 4 0 7.10972 1.61284 1 -11 4 0 14.4615 1.97552 1 12 -4 0 8.88506 2.18748 1 -12 -4 0 14.3468 1.77616 1 -12 4 0 10.2183 1.87892 1 12 4 0 13.3308 2.17229 1 13 -4 0 -1.6557 2.56384 1 -13 -4 0 3.40534 1.95522 1 -13 4 0 -4.3269 2.32474 1 0 -5 0 -0.2486 0.39884 3 0 -5 0 0.32140 0.46459 1 0 -5 0 -0.2790 0.38761 1 0 5 0 0.01016 0.42095 1 0 5 0 0.25852 0.45203 1 1 -5 0 252.943 5.68169 3 1 -5 0 240.006 5.31529 1 -1 -5 0 241.653 5.22890 1 -1 -5 0 240.446 5.31793 1 -1 -5 0 251.139 5.64544 3 -1 5 0 263.653 5.60486 2 -1 5 0 242.617 5.39805 1 1 5 0 244.529 5.24911 1 -1 5 0 244.810 5.32807 1 1 5 0 245.237 5.35549 1 -2 -5 0 8.68215 0.76051 3 -2 -5 0 9.28673 0.76626 1 2 -5 0 9.87486 0.83829 1 2 -5 0 9.80624 0.89310 3 2 5 0 8.70709 0.75577 1 2 5 0 8.28592 0.68430 1 -2 5 0 8.57465 0.85373 2 -2 5 0 8.53716 0.70065 1 -3 -5 0 111.712 2.85804 1 3 -5 0 115.940 3.01355 3 3 -5 0 114.994 2.98154 1 -3 -5 0 115.745 2.91123 3 3 5 0 114.720 2.89874 1 3 5 0 113.806 2.75114 1 -3 5 0 116.651 3.01440 1 -3 5 0 105.999 3.14609 2 -4 -5 0 57.3403 1.71197 3 4 -5 0 54.7920 1.95477 1 4 -5 0 55.9586 1.84227 3 -4 -5 0 55.8396 1.83150 1 -4 5 0 54.9544 1.99168 1 4 5 0 55.0764 1.89119 1 4 5 0 53.7158 1.73825 1 -5 -5 0 19.8167 1.11074 3 -5 -5 0 20.9438 1.12003 1 5 -5 0 17.9832 1.29895 1 5 -5 0 20.8617 1.25302 3 5 5 0 17.7668 1.15093 1 5 5 0 17.2369 1.26309 1 -5 5 0 18.8526 1.36149 1 6 -5 0 25.7556 1.72356 1 -6 -5 0 24.4476 1.13758 3 -6 -5 0 25.7230 1.43304 1 6 -5 0 26.3460 1.42171 3 6 5 0 29.0349 1.54723 1 6 5 0 27.4676 1.45622 1 -6 5 0 26.4427 1.59587 1 7 -5 0 50.0159 2.26319 1 -7 -5 0 47.9912 1.90904 1 7 -5 0 49.4363 1.80570 3 -7 -5 0 46.2938 1.55375 3 7 5 0 48.8640 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4 -11 -10 2.99951 1.99586 3 4 -11 -10 3.39181 2.11941 1 -4 -11 10 5.19056 3.81969 1 -4 11 10 2.63093 3.88279 1 4 11 -10 5.67653 2.51815 1 -3 -11 10 3.65219 4.61551 1 3 -11 -10 1.42630 1.80477 3 3 -11 -10 -1.5002 1.76628 1 3 -11 -10 -1.7954 1.36845 1 -3 11 10 0.71273 3.48444 1 3 11 -10 -2.8146 2.59912 1 2 -11 -10 -2.3066 1.81872 3 -2 -11 10 2.57996 3.62879 1 -2 11 10 -0.6548 3.11503 1 2 11 -10 -3.2781 2.26881 1 1 -11 -10 -0.2811 2.04534 3 -1 11 10 4.83357 2.89103 1 -8 0 11 4.66265 4.54124 1 -7 0 11 -5.5023 3.74577 1 6 0 -11 -1.5890 3.06240 1 -6 0 11 -1.3039 4.08482 1 5 0 -11 2.15194 2.65673 1 -5 0 11 -0.6038 3.36449 1 5 0 -11 -3.3887 1.48075 1 4 0 -11 -1.0027 2.04362 1 4 0 -11 -0.4985 1.49623 1 -4 0 11 -0.2267 3.16220 1 -3 0 11 3.80403 2.95339 1 3 0 -11 3.04562 1.41373 1 3 0 -11 0.13708 1.85180 1 -2 0 11 -0.9551 2.61981 1 2 0 -11 -0.0366 1.01114 1 2 0 -11 -2.1365 1.19191 1 -1 0 11 2.73336 2.38293 1 0 0 11 -2.9623 2.18374 1 -1 0 -11 -1.1544 2.48186 2 1 0 11 1.52716 1.98252 1 -8 -1 11 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-1 11 11.8788 2.63031 1 -1 -1 -11 7.78107 3.37962 2 1 1 11 16.6550 2.39414 1 -1 1 -11 15.8316 3.01946 2 8 -2 -11 10.2478 2.25003 3 -8 -2 11 6.60448 4.57679 1 -7 -2 11 -3.9316 3.99100 1 6 -2 -11 5.80071 3.00767 1 -6 -2 11 3.86701 3.52512 1 6 -2 -11 1.94958 1.76640 3 6 2 -11 8.24627 3.00466 1 -6 2 11 11.0299 4.34736 1 -5 -2 11 3.36954 3.24690 1 5 -2 -11 5.62029 2.51017 1 -5 2 11 3.35906 2.88555 1 5 2 -11 5.91960 3.04797 1 5 2 -11 5.92583 1.79421 1 -4 -2 11 30.9121 3.20096 1 4 -2 -11 35.7435 3.06012 1 4 -2 -11 28.1436 2.42295 1 -4 2 11 27.3108 3.10184 1 4 2 -11 29.7508 3.04172 1 4 2 -11 28.2551 2.63155 1 -3 -2 11 -1.3369 2.91836 1 3 -2 -11 1.03393 1.34453 1 3 -2 -11 -1.1710 1.63782 1 3 2 -11 -2.5606 1.29844 1 -3 2 11 1.21809 2.77232 1 3 2 -11 0.83129 2.30820 1 -2 -2 11 16.0290 2.49823 1 2 2 -11 11.7076 1.88284 1 -2 2 11 16.5586 2.99632 1 2 2 -11 11.9994 1.51295 1 -1 -2 11 14.0915 2.83593 1 -1 2 11 10.9537 2.47521 1 0 -2 -11 1.50469 2.96550 2 0 -2 11 -2.5831 2.38481 1 0 2 11 -1.2342 2.30234 1 1 -2 11 53.8303 3.81858 1 -1 2 -11 66.2774 4.81164 2 1 2 11 55.4441 3.40689 1 -8 -3 11 0.20473 4.66236 1 8 3 -11 6.22714 3.17937 1 -7 -3 11 8.42004 4.28172 1 -6 -3 11 11.0746 4.61707 1 6 -3 -11 8.40569 3.04411 1 6 3 -11 8.89576 3.06447 1 -6 3 11 10.2891 3.78067 1 -5 -3 11 -1.6153 4.07797 1 5 -3 -11 0.60522 2.33578 1 5 3 -11 -0.5946 1.76489 1 -5 3 11 -2.5376 3.54914 1 5 3 -11 2.59700 3.23864 1 4 -3 -11 0.70679 2.10223 1 -4 -3 11 5.71409 3.23188 1 4 -3 -11 -0.7728 1.25845 1 4 3 -11 -0.6042 1.52385 1 -4 3 11 3.88141 3.25326 1 4 3 -11 4.77367 2.81475 1 3 -3 -11 10.3463 1.36640 1 -3 -3 11 10.8567 3.19146 1 3 -3 -11 7.13245 1.52671 1 3 3 -11 6.68731 1.51372 1 -3 3 11 9.55015 3.06464 1 3 3 -11 10.2430 2.39464 1 -2 -3 11 3.31140 2.99790 1 2 3 -11 6.19471 1.46944 1 2 3 -11 5.19001 1.91967 1 -2 3 11 3.63503 2.63576 1 -1 -3 11 32.9355 3.43717 1 1 3 -11 34.1330 1.78303 1 -1 3 11 32.7034 3.34019 1 1 3 -11 36.1003 2.03929 1 0 -3 -11 -0.3846 2.12774 2 0 -3 11 4.82323 2.77625 1 0 3 11 4.04930 2.32050 1 -1 -3 -11 9.71157 2.81746 2 1 -3 11 7.93249 2.61924 1 -1 3 -11 5.21963 2.69302 2 1 3 11 5.05728 2.00002 1 -7 -4 11 4.55549 4.33094 1 6 -4 -11 0.26798 2.22354 1 -6 -4 11 -2.4696 3.81940 1 6 4 -11 5.96838 3.87461 1 6 4 -11 -0.2989 2.36026 1 -6 4 11 4.52005 4.13256 1 -5 -4 11 0.16245 3.56038 1 5 -4 -11 2.22451 1.62672 3 5 -4 -11 1.89393 2.65993 1 5 4 -11 -1.7364 1.43187 1 5 4 -11 1.43574 3.32069 1 -5 4 11 -4.4396 2.81525 1 -4 -4 11 21.5507 3.72048 1 4 -4 -11 24.8890 2.41158 1 4 -4 -11 23.4847 2.80329 3 4 4 -11 23.6059 3.32543 1 4 4 -11 21.3598 2.06743 1 -4 4 11 24.7781 3.67417 1 3 -4 -11 5.07366 1.25783 1 -3 -4 11 12.4263 2.94042 1 3 -4 -11 3.76602 2.12225 3 3 -4 -11 6.88630 1.47426 1 3 4 -11 8.78929 3.02274 1 -3 4 11 9.02786 3.17212 1 3 4 -11 8.11807 1.75875 1 -2 -4 11 -1.5797 2.91719 1 2 4 -11 2.52142 2.29558 1 -2 4 11 5.04286 2.73669 1 2 4 -11 -2.9575 1.47907 1 -1 -4 11 2.13220 3.02557 1 1 4 -11 0.78065 1.24435 1 1 4 -11 1.37511 1.54950 1 -1 4 11 3.59553 2.80201 1 0 -4 -11 3.07613 2.23751 2 0 -4 -11 5.74620 2.07345 3 0 -4 11 6.03298 2.85851 1 0 4 11 2.01365 2.06383 1 -1 -4 -11 21.1084 2.73856 3 1 -4 11 20.8270 3.03240 1 -1 -4 -11 21.3720 3.11581 2 1 4 11 21.1909 2.39487 1 -1 4 -11 25.3569 3.31115 2 -7 -5 11 12.1610 4.75808 1 7 5 -11 10.2331 3.08398 1 -6 -5 11 3.92646 4.86408 1 6 -5 -11 0.00655 2.83126 1 6 -5 -11 0.76109 1.82332 3 -6 5 11 1.93540 3.11169 1 -5 -5 11 9.96387 4.49869 1 5 -5 -11 8.22636 2.43767 1 5 5 -11 5.13178 1.79367 1 5 5 -11 9.40919 3.70671 1 -5 5 11 3.00001 3.57942 1 -4 -5 11 12.2489 3.64667 1 4 -5 -11 17.3519 2.18727 1 4 5 -11 17.0918 3.34133 1 -4 5 11 19.4323 3.05629 1 4 5 -11 17.0347 1.82001 1 3 -5 -11 0.71741 1.25471 1 -3 -5 11 -4.1957 3.30694 1 3 -5 -11 0.14041 1.16206 1 3 5 -11 2.83856 2.78544 1 -3 5 11 -1.5242 2.39136 1 3 5 -11 -0.8515 1.56893 1 -2 -5 11 3.42845 2.88867 1 2 -5 -11 6.54371 2.05984 3 -2 5 11 9.12035 2.98923 1 2 5 -11 4.26481 1.43848 1 2 5 -11 6.54031 2.67522 1 1 -5 -11 4.00863 2.53231 2 -1 -5 11 0.87740 3.13914 1 1 5 -11 2.58761 2.20316 1 -1 5 11 1.97653 2.72992 1 1 5 -11 -0.2761 1.50677 1 0 -5 -11 10.2444 2.64382 3 0 -5 -11 11.8774 2.96352 2 0 -5 11 9.43295 3.17782 1 0 5 11 11.3581 2.57464 1 -6 -6 11 2.86321 4.25169 1 6 -6 -11 -1.7048 2.97340 1 6 -6 -11 3.12155 2.30094 3 -5 -6 11 6.22044 3.98694 1 5 -6 -11 8.62274 2.41560 1 5 6 -11 12.7195 2.07361 1 -4 -6 11 -6.1939 4.16453 1 4 -6 -11 0.12190 2.08294 1 4 6 -11 2.29162 3.35282 1 -4 6 11 -0.8735 3.32719 1 4 6 -11 1.52080 1.64753 1 3 -6 -11 0.68901 1.01797 1 -3 -6 11 -2.7511 2.80508 1 3 -6 -11 -0.5254 1.14192 1 3 6 -11 2.81031 3.11616 1 -3 6 11 0.69909 3.06091 1 3 6 -11 -2.0119 1.65361 1 -2 -6 11 10.1212 3.64618 1 2 6 -11 -1.0441 1.73666 1 -2 6 11 -3.4916 2.79094 1 2 6 -11 -1.8743 2.54027 1 -1 -6 11 2.68372 3.34916 1 1 -6 -11 -0.2980 2.58080 2 1 6 -11 2.31805 1.80196 1 -1 6 11 1.00766 2.55677 1 1 6 -11 -1.2800 2.63417 1 0 -6 -11 -0.8519 2.05049 3 0 -6 -11 1.49303 2.79094 2 0 -6 11 4.03894 3.43125 1 0 6 11 2.85399 2.41812 1 0 6 -11 4.30585 1.79598 1 0 6 -11 4.15423 1.46142 1 6 7 -11 -1.6420 2.31379 1 5 -7 -11 1.17557 1.86930 1 5 -7 -11 0.82942 2.76693 1 -5 -7 11 3.49110 5.03518 1 5 7 -11 3.36497 2.16033 1 4 -7 -11 2.41133 1.53834 1 4 -7 -11 -0.6907 1.92820 1 -4 -7 11 4.87824 3.74057 1 4 7 -11 2.41740 1.74847 1 3 -7 -11 3.56875 1.01665 1 3 -7 -11 2.69300 1.10387 1 -3 -7 11 3.89877 3.85346 1 -3 7 11 6.13272 3.21883 1 3 7 -11 -1.3358 1.80788 1 3 7 -11 1.71037 3.34954 1 -2 -7 11 3.67644 3.08584 1 -2 7 11 1.97811 2.92516 1 2 7 -11 0.26486 1.66377 1 2 7 -11 1.23408 2.89350 1 1 -7 -11 2.33638 2.22428 3 1 -7 -11 2.45272 2.19663 2 1 7 -11 5.48900 2.79410 1 -1 7 11 1.86220 2.61825 1 1 7 -11 4.40948 1.88768 1 4 -8 -11 2.84236 2.16636 3 4 -8 -11 1.73871 1.55641 1 4 -8 -11 2.14324 2.23504 1 4 8 -11 3.48188 2.09195 1 2 8 -11 0.42144 3.37021 1 -2 8 11 1.14986 3.53992 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 44582 _database_code_depnum_ccdc_archive 'CCDC 957489' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_AXM690_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 O4' _chemical_formula_weight 272.29 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 8.0560(3) _cell_length_b 9.6155(3) _cell_length_c 9.8824(3) _cell_angle_alpha 95.471(2) _cell_angle_beta 104.231(2) _cell_angle_gamma 111.323(2) _cell_volume 676.61(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5635 _cell_measurement_theta_min 2.8476 _cell_measurement_theta_max 27.5534 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.337 _exptl_crystal_F_000 288 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.190 _exptl_absorpt_coefficient_mu 0.096 _shelx_estimated_absorpt_T_min 0.965 _shelx_estimated_absorpt_T_max 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed X-ray tube' _diffrn_measurement_device_type 'Bruker D8 QUEST area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 8740 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.323 _diffrn_reflns_theta_max 25.496 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 2514 _reflns_number_gt 2253 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'BRUKER APEX II' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_publication_material ? _refine_special_details ; ; _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^)+(0.0521P)^2^+0.2231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2514 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.94051(13) 0.83346(11) -0.23097(10) 0.0206(2) Uani 1 1 d . . . . . O2 O 0.68128(12) 0.86632(10) -0.23925(9) 0.0166(2) Uani 1 1 d . . . . . O3 O 1.14473(12) 0.82528(11) 0.05574(10) 0.0217(2) Uani 1 1 d . . . . . O4 O 0.92011(12) 0.62798(10) 0.09733(9) 0.0161(2) Uani 1 1 d . . . . . C1 C 0.82794(17) 0.83117(14) -0.16893(13) 0.0151(3) Uani 1 1 d . . . . . C2 C 0.82470(17) 0.79051(13) -0.03189(13) 0.0144(3) Uani 1 1 d . . . . . C3 C 0.68055(17) 0.78454(13) 0.02102(13) 0.0140(3) Uani 1 1 d . . . . . C4 C 0.53505(17) 0.82224(14) -0.05920(14) 0.0154(3) Uani 1 1 d . . . . . H4 H 0.4337 0.8173 -0.0242 0.018 Uiso 1 1 calc R U . . . C5 C 0.54149(17) 0.86465(14) -0.18402(14) 0.0159(3) Uani 1 1 d . . . . . C6 C 0.98253(17) 0.75330(14) 0.04354(13) 0.0146(3) Uani 1 1 d . . . . . C7 C 1.06153(18) 0.59635(15) 0.19609(14) 0.0193(3) Uani 1 1 d . . . . . H7A H 1.1525 0.6908 0.2652 0.023 Uiso 1 1 calc R U . . . H7B H 1.1298 0.5556 0.1438 0.023 Uiso 1 1 calc R U . . . C8 C 0.9620(2) 0.48060(16) 0.27237(16) 0.0252(3) Uani 1 1 d . . . . . H8A H 0.8923 0.5212 0.3214 0.038 Uiso 1 1 calc R U . . . H8B H 1.0536 0.4584 0.3423 0.038 Uiso 1 1 calc R U . . . H8C H 0.8751 0.3867 0.2031 0.038 Uiso 1 1 calc R U . . . C9 C 0.67030(17) 0.74443(14) 0.16120(13) 0.0142(3) Uani 1 1 d . . . . . C10 C 0.81428(18) 0.82621(14) 0.28634(14) 0.0168(3) Uani 1 1 d . . . . . H10 H 0.9226 0.9080 0.2828 0.020 Uiso 1 1 calc R U . . . C11 C 0.79965(19) 0.78847(15) 0.41604(14) 0.0189(3) Uani 1 1 d . . . . . H11 H 0.8970 0.8456 0.5015 0.023 Uiso 1 1 calc R U . . . C12 C 0.64301(19) 0.66727(15) 0.42140(14) 0.0201(3) Uani 1 1 d . . . . . H12 H 0.6337 0.6407 0.5102 0.024 Uiso 1 1 calc R U . . . C13 C 0.50061(19) 0.58534(16) 0.29697(15) 0.0206(3) Uani 1 1 d . . . . . H13 H 0.3941 0.5017 0.3005 0.025 Uiso 1 1 calc R U . . . C14 C 0.51227(18) 0.62454(15) 0.16683(14) 0.0169(3) Uani 1 1 d . . . . . H14 H 0.4126 0.5696 0.0820 0.020 Uiso 1 1 calc R U . . . C15 C 0.41077(19) 0.91954(15) -0.27434(14) 0.0200(3) Uani 1 1 d . . . . . H15A H 0.4772 1.0299 -0.2694 0.024 Uiso 1 1 calc R U . . . H15B H 0.3057 0.9064 -0.2347 0.024 Uiso 1 1 calc R U . . . C16 C 0.3317(2) 0.83702(17) -0.43063(15) 0.0255(3) Uani 1 1 d . . . . . H16A H 0.2608 0.7282 -0.4370 0.038 Uiso 1 1 calc R U . . . H16B H 0.4345 0.8500 -0.4712 0.038 Uiso 1 1 calc R U . . . H16C H 0.2489 0.8799 -0.4839 0.038 Uiso 1 1 calc R U . . . 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 0.0210(5) 0.0263(5) 0.0181(5) 0.0069(4) 0.0105(4) 0.0102(4) O2 0.0181(5) 0.0192(5) 0.0138(5) 0.0046(4) 0.0056(4) 0.0082(4) O3 0.0136(5) 0.0249(5) 0.0233(5) 0.0057(4) 0.0054(4) 0.0039(4) O4 0.0140(4) 0.0161(4) 0.0173(5) 0.0041(4) 0.0032(4) 0.0059(4) C1 0.0153(6) 0.0119(6) 0.0154(6) 0.0013(5) 0.0040(5) 0.0034(5) C2 0.0143(6) 0.0120(6) 0.0138(6) 0.0007(5) 0.0038(5) 0.0026(5) C3 0.0145(6) 0.0096(5) 0.0144(6) 0.0000(5) 0.0036(5) 0.0019(5) C4 0.0142(6) 0.0150(6) 0.0157(6) 0.0012(5) 0.0047(5) 0.0049(5) C5 0.0148(6) 0.0137(6) 0.0167(6) 0.0000(5) 0.0039(5) 0.0042(5) C6 0.0162(6) 0.0148(6) 0.0114(6) -0.0001(5) 0.0057(5) 0.0044(5) C7 0.0167(6) 0.0235(7) 0.0175(6) 0.0039(5) 0.0016(5) 0.0104(5) C8 0.0265(7) 0.0238(7) 0.0275(8) 0.0103(6) 0.0064(6) 0.0123(6) C9 0.0153(6) 0.0151(6) 0.0157(6) 0.0037(5) 0.0064(5) 0.0088(5) C10 0.0167(6) 0.0154(6) 0.0177(7) 0.0029(5) 0.0059(5) 0.0054(5) C11 0.0207(7) 0.0201(7) 0.0142(6) 0.0016(5) 0.0025(5) 0.0084(6) C12 0.0250(7) 0.0246(7) 0.0159(7) 0.0089(5) 0.0097(6) 0.0121(6) C13 0.0175(7) 0.0223(7) 0.0228(7) 0.0085(5) 0.0092(6) 0.0058(5) C14 0.0143(6) 0.0191(6) 0.0163(7) 0.0034(5) 0.0042(5) 0.0059(5) C15 0.0217(7) 0.0213(7) 0.0186(7) 0.0055(5) 0.0051(6) 0.0109(6) C16 0.0255(7) 0.0310(8) 0.0181(7) 0.0056(6) 0.0014(6) 0.0124(6) _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 1.2084(16) . ? O2 C5 1.3627(15) . ? O2 C1 1.3873(15) . ? O3 C6 1.2042(16) . ? O4 C6 1.3418(15) . ? O4 C7 1.4508(15) . ? C1 C2 1.4487(17) . ? C2 C3 1.3715(18) . ? C2 C6 1.4886(17) . ? C3 C4 1.4286(17) . ? C3 C9 1.4865(17) . ? C4 C5 1.3426(18) . ? C4 H4 0.9500 . ? C5 C15 1.4887(18) . ? C7 C8 1.5027(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.3902(18) . ? C9 C10 1.3925(18) . ? C10 C11 1.3858(18) . ? C10 H10 0.9500 . ? C11 C12 1.3887(19) . ? C11 H11 0.9500 . ? C12 C13 1.383(2) . ? C12 H12 0.9500 . ? C13 C14 1.3896(18) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.5283(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C5 O2 C1 122.83(10) . . ? C6 O4 C7 116.06(10) . . ? O1 C1 O2 116.27(11) . . ? O1 C1 C2 127.47(12) . . ? O2 C1 C2 116.22(11) . . ? C3 C2 C1 120.62(11) . . ? C3 C2 C6 123.25(11) . . ? C1 C2 C6 116.11(11) . . ? C2 C3 C4 119.22(11) . . ? C2 C3 C9 123.01(11) . . ? C4 C3 C9 117.75(11) . . ? C5 C4 C3 120.03(12) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 O2 121.01(11) . . ? C4 C5 C15 126.77(12) . . ? O2 C5 C15 112.18(11) . . ? O3 C6 O4 124.06(12) . . ? O3 C6 C2 125.13(11) . . ? O4 C6 C2 110.81(10) . . ? O4 C7 C8 107.06(10) . . ? O4 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O4 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 119.77(12) . . ? C14 C9 C3 119.02(11) . . ? C10 C9 C3 121.19(11) . . ? C11 C10 C9 120.07(12) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.15(12) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 119.77(12) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.46(12) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 119.76(12) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? C5 C15 C16 113.85(11) . . ? C5 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C5 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 O2 C1 O1 178.34(10) . . . . ? C5 O2 C1 C2 0.53(16) . . . . ? O1 C1 C2 C3 -176.04(12) . . . . ? O2 C1 C2 C3 1.49(17) . . . . ? O1 C1 C2 C6 2.65(19) . . . . ? O2 C1 C2 C6 -179.83(10) . . . . ? C1 C2 C3 C4 -1.37(17) . . . . ? C6 C2 C3 C4 -179.96(11) . . . . ? C1 C2 C3 C9 -179.64(11) . . . . ? C6 C2 C3 C9 1.77(18) . . . . ? C2 C3 C4 C5 -0.78(18) . . . . ? C9 C3 C4 C5 177.58(11) . . . . ? C3 C4 C5 O2 2.82(18) . . . . ? C3 C4 C5 C15 -174.60(12) . . . . ? C1 O2 C5 C4 -2.73(18) . . . . ? C1 O2 C5 C15 175.04(10) . . . . ? C7 O4 C6 O3 11.18(17) . . . . ? C7 O4 C6 C2 -168.59(10) . . . . ? C3 C2 C6 O3 -136.62(14) . . . . ? C1 C2 C6 O3 44.74(17) . . . . ? C3 C2 C6 O4 43.15(16) . . . . ? C1 C2 C6 O4 -135.49(11) . . . . ? C6 O4 C7 C8 164.84(11) . . . . ? C2 C3 C9 C14 -124.59(13) . . . . ? C4 C3 C9 C14 57.12(16) . . . . ? C2 C3 C9 C10 56.48(17) . . . . ? C4 C3 C9 C10 -121.81(13) . . . . ? C14 C9 C10 C11 -0.23(19) . . . . ? C3 C9 C10 C11 178.70(11) . . . . ? C9 C10 C11 C12 1.19(19) . . . . ? C10 C11 C12 C13 -0.7(2) . . . . ? C11 C12 C13 C14 -0.7(2) . . . . ? C12 C13 C14 C9 1.7(2) . . . . ? C10 C9 C14 C13 -1.19(19) . . . . ? C3 C9 C14 C13 179.86(11) . . . . ? C4 C5 C15 C16 -129.42(14) . . . . ? O2 C5 C15 C16 52.98(15) . . . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.052 _shelxl_version_number 2013-3 _shelx_res_file ; TITL AXM690_0m in P-1 CELL 0.71073 8.0560 9.6155 9.8824 95.471 104.231 111.323 ZERR 2.00 0.0003 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H O UNIT 32 32 8 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.19 0.30 0.38 ACTA L.S. 12 FMAP 2 PLAN -4 0 0.00 HTAB BOND $H CONF omit -2 51 WGHT 0.052100 0.223100 FVAR 0.98233 O1 3 0.940514 0.833462 -0.230970 11.00000 0.02101 0.02633 = 0.01814 0.00687 0.01045 0.01016 O2 3 0.681275 0.866315 -0.239246 11.00000 0.01812 0.01920 = 0.01381 0.00465 0.00560 0.00815 O3 3 1.144734 0.825277 0.055738 11.00000 0.01360 0.02490 = 0.02328 0.00571 0.00543 0.00392 O4 3 0.920110 0.627979 0.097330 11.00000 0.01398 0.01606 = 0.01729 0.00413 0.00317 0.00595 C1 1 0.827939 0.831173 -0.168927 11.00000 0.01530 0.01193 = 0.01542 0.00126 0.00400 0.00341 C2 1 0.824705 0.790511 -0.031885 11.00000 0.01429 0.01199 = 0.01375 0.00071 0.00375 0.00259 C3 1 0.680551 0.784545 0.021024 11.00000 0.01446 0.00957 = 0.01435 0.00004 0.00362 0.00195 C4 1 0.535046 0.822244 -0.059200 11.00000 0.01423 0.01501 = 0.01573 0.00119 0.00472 0.00488 AFIX 43 H4 2 0.433674 0.817305 -0.024210 11.00000 -1.20000 AFIX 0 C5 1 0.541494 0.864653 -0.184023 11.00000 0.01481 0.01368 = 0.01675 0.00002 0.00393 0.00415 C6 1 0.982527 0.753298 0.043538 11.00000 0.01623 0.01483 = 0.01143 -0.00006 0.00572 0.00436 C7 1 1.061533 0.596355 0.196094 11.00000 0.01673 0.02353 = 0.01748 0.00389 0.00163 0.01037 AFIX 23 H7A 2 1.152522 0.690809 0.265210 11.00000 -1.20000 H7B 2 1.129754 0.555604 0.143817 11.00000 -1.20000 AFIX 0 C8 1 0.961969 0.480605 0.272367 11.00000 0.02647 0.02381 = 0.02745 0.01032 0.00643 0.01228 AFIX 137 H8A 2 0.892273 0.521233 0.321445 11.00000 -1.50000 H8B 2 1.053636 0.458377 0.342274 11.00000 -1.50000 H8C 2 0.875070 0.386718 0.203121 11.00000 -1.50000 AFIX 0 C9 1 0.670303 0.744434 0.161204 11.00000 0.01526 0.01514 = 0.01569 0.00372 0.00644 0.00881 C10 1 0.814279 0.826213 0.286340 11.00000 0.01673 0.01542 = 0.01772 0.00294 0.00587 0.00538 AFIX 43 H10 2 0.922649 0.907962 0.282794 11.00000 -1.20000 AFIX 0 C11 1 0.799645 0.788473 0.416043 11.00000 0.02065 0.02012 = 0.01421 0.00160 0.00247 0.00841 AFIX 43 H11 2 0.896984 0.845645 0.501483 11.00000 -1.20000 AFIX 0 C12 1 0.643013 0.667271 0.421402 11.00000 0.02496 0.02458 = 0.01591 0.00887 0.00969 0.01213 AFIX 43 H12 2 0.633696 0.640719 0.510224 11.00000 -1.20000 AFIX 0 C13 1 0.500613 0.585339 0.296974 11.00000 0.01749 0.02226 = 0.02279 0.00853 0.00922 0.00582 AFIX 43 H13 2 0.394109 0.501692 0.300508 11.00000 -1.20000 REM ##### REM ##### AFIX 0 C14 1 0.512266 0.624537 0.166829 11.00000 0.01428 0.01910 = 0.01631 0.00338 0.00425 0.00592 AFIX 43 H14 2 0.412601 0.569602 0.082012 11.00000 -1.20000 AFIX 0 C15 1 0.410767 0.919538 -0.274342 11.00000 0.02167 0.02131 = 0.01864 0.00554 0.00508 0.01088 AFIX 23 H15A 2 0.477244 1.029947 -0.269419 11.00000 -1.20000 H15B 2 0.305698 0.906398 -0.234741 11.00000 -1.20000 AFIX 0 C16 1 0.331653 0.837023 -0.430628 11.00000 0.02549 0.03099 = 0.01810 0.00557 0.00144 0.01242 AFIX 137 H16A 2 0.260752 0.728180 -0.437041 11.00000 -1.50000 H16B 2 0.434538 0.850039 -0.471157 11.00000 -1.50000 H16C 2 0.248938 0.879939 -0.483902 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM AXM690_0m in P-1 REM R1 = 0.0332 for 2253 Fo > 4sig(Fo) and 0.0386 for all 2514 data REM 183 parameters refined using 0 restraints END WGHT 0.0521 0.2231 REM Instructions for potential hydrogen bonds EQIV $1 x-1, y, z HTAB C4 O3_$1 REM Highest difference peak 0.227, deepest hole -0.211, 1-sigma level 0.052 Q1 1 0.7651 0.7552 0.2149 11.00000 0.05 0.23 Q2 1 0.8913 0.7708 0.0035 11.00000 0.05 0.23 Q3 1 0.8096 0.7875 -0.1013 11.00000 0.05 0.21 Q4 1 0.5447 0.6558 0.3612 11.00000 0.05 0.20 ; _shelx_res_checksum 84522 _shelx_hkl_file ; 1 0 0 25.5644 1.14261 1 2 0 0 659.849 23.8343 1 2 0 0 554.465 30.8411 3 -3 0 0 17.7268 1.07621 1 3 0 0 18.1475 1.07531 1 3 0 0 16.2339 1.09254 1 -4 0 0 33.3193 1.82005 1 4 0 0 36.8770 1.86098 1 4 0 0 33.4274 1.81463 1 -5 0 0 126.740 5.38652 1 5 0 0 128.561 5.52027 1 5 0 0 118.868 5.43144 1 -6 0 0 501.766 19.7690 1 6 0 0 508.105 19.9247 1 6 0 0 464.748 19.8511 1 7 0 0 102.311 5.21220 1 7 0 0 101.730 4.89716 1 8 0 0 224.016 10.0137 1 8 0 0 217.423 9.68299 1 9 0 0 16.7872 2.78430 1 9 0 0 19.2481 2.68581 1 9 -1 0 1.82085 1.96358 1 9 -1 0 -4.5092 1.69715 1 -9 1 0 2.50946 1.54524 1 8 -1 0 271.277 12.0929 1 8 -1 0 290.904 12.2812 1 -8 1 0 291.132 11.8872 1 7 -1 0 1097.16 44.4693 1 7 -1 0 1137.49 44.5359 1 -7 1 0 1132.98 44.3214 1 6 -1 0 124.531 5.65550 1 6 -1 0 131.219 5.75263 1 -6 1 0 126.948 5.56613 1 5 -1 0 127.868 5.66768 1 -5 1 0 134.149 5.57126 1 4 -1 0 2.34929 0.50767 1 -4 1 0 1.04272 0.38576 1 3 -1 0 3.92166 0.48917 1 -3 1 0 3.90332 0.41079 1 2 -1 0 984.138 41.4930 1 -2 1 0 1006.58 41.5598 1 -2 1 0 1197.83 54.1909 3 1 -1 0 1321.36 56.0308 1 -1 1 0 1361.18 65.2049 2 -1 1 0 1607.78 73.1987 3 -1 1 0 1422.15 55.9654 1 0 -1 0 -5.4915 0.04967 1 -1 -1 0 4664.24 190.753 1 -1 -1 0 4821.21 190.746 1 1 1 0 4773.69 190.769 1 1 1 0 5477.53 248.702 3 1 1 0 4644.49 190.731 1 -2 -1 0 858.825 34.3577 1 2 1 0 944.729 44.6909 3 2 1 0 870.971 34.3749 1 2 1 0 829.353 34.3754 1 -3 -1 0 110.915 4.64049 1 3 1 0 109.033 5.75179 3 3 1 0 112.364 4.69925 1 3 1 0 102.178 4.66902 1 -4 -1 0 167.402 6.72711 1 4 1 0 166.706 6.80876 1 4 1 0 161.654 6.77276 1 4 1 0 145.038 8.28731 3 -5 -1 0 12.3853 1.31539 1 5 1 0 10.6148 1.10413 1 5 1 0 12.1617 1.24860 1 -6 -1 0 0.20873 0.67850 1 6 1 0 0.49450 0.65357 1 6 1 0 1.08582 0.97001 1 -7 -1 0 103.432 4.96820 1 7 1 0 95.8855 5.03245 1 7 1 0 95.1701 4.96455 1 -8 -1 0 3.89636 1.67966 1 8 1 0 6.18975 2.12156 1 8 1 0 3.75776 1.46850 1 9 -2 0 70.0481 4.52952 1 9 -2 0 65.5368 4.16666 1 -9 2 0 70.2281 3.88063 1 8 -2 0 64.0181 3.65055 1 8 -2 0 62.0467 3.85549 1 -8 2 0 71.2558 3.52568 1 7 -2 0 322.578 13.1779 1 7 -2 0 305.821 13.1262 1 -7 2 0 326.144 12.9863 1 6 -2 0 282.258 11.8437 1 -6 2 0 295.017 11.7194 1 5 -2 0 52.2316 2.54711 1 -5 2 0 50.8067 2.40766 1 4 -2 0 20.6341 1.26598 1 -4 2 0 24.1325 1.33929 3 -4 2 0 21.7243 1.18184 1 3 -2 0 20.1040 1.06438 1 -3 2 0 19.9458 1.01062 1 -3 2 0 22.2993 1.28427 3 2 -2 0 2395.70 101.668 1 -2 2 0 2887.77 132.840 3 -2 2 0 2577.81 118.316 2 -2 2 0 2527.27 101.606 1 1 -2 0 74.5606 3.10314 1 1 -2 0 73.4649 3.10205 1 -1 2 0 74.6974 3.09074 1 -1 2 0 88.0152 4.18651 3 -1 2 0 73.1333 3.09820 1 0 -2 0 3729.11 144.204 1 0 -2 0 3514.90 143.768 1 0 2 0 3463.76 143.991 1 0 2 0 4010.77 188.119 3 -1 -2 0 427.969 17.0354 1 -1 -2 0 415.474 17.0559 1 1 2 0 424.784 17.0381 1 1 2 0 475.314 22.2088 3 1 2 0 412.912 17.0429 1 -2 -2 0 121.567 5.10366 1 -2 -2 0 115.409 5.13458 1 2 2 0 117.362 5.10560 1 2 2 0 116.737 5.11867 1 2 2 0 134.721 6.52184 3 -3 -2 0 55.2455 2.68674 1 3 2 0 60.4434 3.31102 3 3 2 0 56.2170 2.78244 1 3 2 0 56.7303 2.77602 1 -4 -2 0 60.5760 2.97811 1 4 2 0 59.8810 3.09825 1 4 2 0 63.1569 3.03467 1 4 2 0 60.4742 3.49512 3 -5 -2 0 92.9601 4.14467 1 5 2 0 78.3825 4.74054 3 5 2 0 85.7296 4.14922 1 5 2 0 90.2153 4.19517 1 -6 -2 0 297.830 12.0497 1 6 2 0 272.900 12.0246 1 6 2 0 286.193 12.1555 1 -7 -2 0 236.856 10.0780 1 7 2 0 224.229 10.1201 1 7 2 0 233.989 10.4339 1 -8 -2 0 27.4174 2.90072 1 8 2 0 42.7111 4.46091 1 8 2 0 43.0981 3.30892 1 9 -3 0 9.99520 1.56046 1 9 -3 0 9.96344 1.86771 1 -9 3 0 9.53761 1.39704 1 8 -3 0 76.6106 4.14055 1 8 -3 0 74.8498 3.93600 1 -8 3 0 80.9545 3.77485 1 7 -3 0 208.219 8.91534 1 -7 3 0 211.046 8.66017 1 6 -3 0 792.897 31.7476 1 -6 3 0 810.853 31.5758 1 5 -3 0 6.11175 0.67268 1 -5 3 0 5.78673 0.63419 1 -5 3 0 6.73555 0.83437 3 4 -3 0 11.0481 0.80336 1 -4 3 0 9.69163 0.95248 2 -4 3 0 11.2490 0.73113 1 -4 3 0 11.9940 0.98428 3 3 -3 0 164.573 6.89890 1 -3 3 0 169.538 6.84109 1 -3 3 0 192.059 9.10328 3 -3 3 0 162.651 8.01875 2 2 -3 0 254.647 10.8602 1 -2 3 0 307.098 14.3705 3 -2 3 0 262.725 10.8415 1 -2 3 0 285.132 12.6932 2 -2 3 0 269.405 10.8235 1 1 -3 0 1348.62 54.8260 1 1 -3 0 1370.63 54.9237 1 -1 3 0 1351.35 54.8306 1 -1 3 0 1329.67 54.9044 1 -1 3 0 1594.67 71.4529 3 0 -3 0 4804.48 193.375 1 0 -3 0 4834.79 193.188 1 0 3 0 5328.14 252.083 3 0 3 0 4774.33 192.766 1 -1 -3 0 26.1638 1.47342 1 -1 -3 0 26.6691 1.44598 1 1 3 0 27.3438 1.38570 1 1 3 0 26.6470 1.83922 3 1 3 0 25.2806 1.38406 1 -2 -3 0 39.7087 2.04628 1 -2 -3 0 37.8594 2.03538 1 2 3 0 38.2781 2.03331 1 2 3 0 37.1212 1.98372 1 2 3 0 42.0348 2.52833 3 -3 -3 0 95.2202 4.25351 1 3 3 0 93.2350 4.31563 1 3 3 0 94.8037 4.32661 1 3 3 0 95.2251 5.34197 3 -4 -3 0 -0.0545 0.77913 1 4 3 0 0.31429 0.80863 1 4 3 0 1.26957 0.73827 1 4 3 0 1.48849 0.76240 3 -5 -3 0 33.4309 2.44593 1 5 3 0 32.6835 2.45930 3 5 3 0 32.0890 2.47772 1 5 3 0 32.9941 2.45804 1 -6 -3 0 24.8053 2.57454 1 6 3 0 21.5547 1.96277 3 6 3 0 25.7727 2.17194 1 6 3 0 23.0306 2.25120 1 -7 -3 0 -0.6427 1.21176 1 7 3 0 0.49093 1.40583 1 7 3 0 2.20082 2.06660 1 8 3 0 216.010 10.1625 1 8 3 0 222.572 10.9001 1 10 -4 0 43.2654 4.11812 1 -10 4 0 44.1077 3.19565 1 -10 4 0 48.7548 3.99123 2 9 -4 0 210.595 9.44327 1 9 -4 0 215.442 9.37705 1 -9 4 0 216.882 9.02017 1 -9 4 0 223.036 10.9558 2 8 -4 0 10.7960 1.42463 1 -8 4 0 10.7815 1.67103 2 -8 4 0 11.5372 1.06995 1 7 -4 0 1.11223 0.83547 1 -7 4 0 1.62900 0.54005 1 -7 4 0 1.55212 1.03122 2 -7 4 0 0.92454 0.54375 3 6 -4 0 5.42057 0.77287 1 -6 4 0 6.69682 0.87701 3 -6 4 0 7.20286 1.04163 2 -6 4 0 5.90468 0.58462 1 5 -4 0 138.914 6.08888 1 -5 4 0 152.936 7.89743 3 -5 4 0 146.948 5.93684 1 -5 4 0 148.058 7.06377 2 4 -4 0 592.291 24.4317 1 -4 4 0 618.072 24.3229 1 -4 4 0 605.970 28.4550 2 -4 4 0 669.493 32.0113 3 3 -4 0 348.514 14.1486 1 -3 4 0 373.586 16.5094 2 -3 4 0 337.747 14.0523 1 -3 4 0 384.235 18.6835 3 -3 4 0 350.362 14.0803 1 2 -4 0 572.949 22.2709 1 -2 4 0 550.346 22.2429 1 -2 4 0 564.859 22.2221 1 -2 4 0 583.119 29.2959 3 1 -4 0 2.41678 0.37358 1 1 -4 0 1.80351 0.33124 1 -1 4 0 2.50982 0.32475 1 -1 4 0 2.83747 0.71319 3 -1 4 0 2.65840 0.31148 1 0 -4 0 1232.09 49.8205 1 0 -4 0 1256.42 49.8032 1 0 4 0 1346.71 65.1301 3 0 4 0 1253.40 49.7839 1 -1 -4 0 652.491 25.8307 1 -1 -4 0 636.933 25.8676 1 1 4 0 696.126 33.7496 3 1 4 0 649.229 25.8241 1 1 4 0 630.590 25.8196 1 -2 -4 0 53.2657 2.74398 1 -2 -4 0 55.8148 2.87815 1 2 4 0 54.2246 2.68867 1 2 4 0 60.1148 3.55324 3 2 4 0 54.1890 2.76069 1 -3 -4 0 50.0222 2.70959 1 3 4 0 47.7169 3.25466 3 3 4 0 50.1215 2.61091 1 3 4 0 50.3046 2.72752 1 -4 -4 0 70.5577 3.52373 1 4 4 0 66.1142 3.50974 1 4 4 0 67.0302 4.30748 3 4 4 0 70.8017 3.53530 1 -5 -4 0 251.754 10.4312 1 5 4 0 247.256 10.4915 1 5 4 0 231.431 13.0350 3 5 4 0 243.120 10.4475 1 -6 -4 0 22.7897 2.04325 1 6 4 0 22.0928 2.35326 1 6 4 0 15.6937 2.08566 3 6 4 0 18.8853 2.31476 1 -7 -4 0 201.735 9.51181 1 7 4 0 206.157 9.33082 1 7 4 0 193.630 9.76458 1 10 -5 0 146.281 7.28152 1 9 -5 0 28.2893 2.62479 1 -9 5 0 26.9817 2.63182 2 -9 5 0 24.6394 1.65452 1 8 -5 0 5.57731 1.12528 1 -8 5 0 7.42672 1.36887 2 -8 5 0 6.61045 0.77798 1 7 -5 0 179.039 7.44260 1 -7 5 0 176.653 8.51140 2 -7 5 0 170.585 7.06146 1 -7 5 0 172.428 9.39053 3 6 -5 0 50.0290 2.58626 1 -6 5 0 53.0082 3.37085 3 -6 5 0 52.5569 2.29034 1 -6 5 0 56.9282 2.94785 2 5 -5 0 482.857 19.6105 1 -5 5 0 521.636 25.7208 3 -5 5 0 485.178 19.3998 1 -5 5 0 491.777 22.7801 2 4 -5 0 8.13633 0.66480 1 -4 5 0 8.61186 0.50725 1 -4 5 0 9.71061 1.26202 3 -4 5 0 8.75166 0.87841 2 -4 5 0 7.65837 0.46719 1 3 -5 0 2212.16 89.8887 1 -3 5 0 2159.39 89.9575 1 -3 5 0 2524.38 117.427 3 -3 5 0 2304.38 89.7312 1 2 -5 0 0.88149 0.27605 1 2 -5 0 0.95138 0.27768 1 -2 5 0 0.27949 0.63947 3 -2 5 0 0.90629 0.22787 1 -2 5 0 0.72450 0.26141 1 1 -5 0 10.7794 0.82317 1 1 -5 0 10.8395 0.83250 1 -1 5 0 12.6870 1.25609 3 -1 5 0 10.4046 0.79590 1 -1 5 0 10.2704 0.70445 1 0 -5 0 1129.69 44.3939 1 0 -5 0 1137.24 44.3676 1 0 5 0 1091.28 44.3206 1 0 5 0 1161.07 58.0340 3 -1 -5 0 310.086 12.3412 1 -1 -5 0 306.037 12.4084 1 1 5 0 297.047 12.3144 1 1 5 0 297.505 12.3049 1 1 5 0 306.950 16.1340 3 -2 -5 0 8.94059 0.98226 1 -2 -5 0 9.05034 1.16909 1 2 5 0 11.6131 1.13578 1 2 5 0 10.9793 1.38656 3 2 5 0 8.73852 1.04763 1 -3 -5 0 34.7984 2.22619 1 3 5 0 35.4538 2.67504 3 3 5 0 36.8746 2.36425 1 3 5 0 36.1069 2.21857 1 -4 -5 0 -0.1587 1.06740 1 4 5 0 -0.5023 1.09095 3 4 5 0 0.88609 1.12968 1 4 5 0 0.47512 1.16803 1 -5 -5 0 24.4899 2.35284 1 5 5 0 22.1847 2.51749 3 5 5 0 22.7366 2.31429 1 5 5 0 23.3190 2.22086 1 -6 -5 0 73.1853 4.70534 1 6 5 0 62.4639 4.42344 3 6 5 0 62.3806 4.58766 1 6 5 0 64.7115 4.02763 1 10 -6 0 191.332 8.81512 1 9 -6 0 32.7583 2.78173 1 -9 6 0 33.0655 2.94883 2 8 -6 0 53.2143 3.01782 1 -8 6 0 53.3889 3.60453 3 7 -6 0 3.58331 0.87997 1 -7 6 0 5.71005 1.04003 2 -7 6 0 5.58947 1.25241 3 -7 6 0 3.73085 0.40565 1 6 -6 0 200.902 8.32844 1 -6 6 0 200.175 9.56678 2 -6 6 0 206.377 11.0315 3 5 -6 0 9.51644 0.83182 1 -5 6 0 9.43914 1.37730 3 4 -6 0 212.215 8.46322 1 -4 6 0 207.581 8.28654 1 -4 6 0 204.392 8.26312 1 -4 6 0 216.468 11.3785 3 3 -6 0 82.5243 3.50526 1 -3 6 0 79.4053 3.36048 1 -3 6 0 80.6151 3.41179 1 -3 6 0 84.8622 4.88016 3 2 -6 0 39.8687 1.95260 1 2 -6 0 39.8872 1.95294 1 -2 6 0 41.0691 1.86231 1 -2 6 0 39.7969 1.88661 1 -2 6 0 41.9193 2.80634 3 1 -6 0 284.525 11.1788 1 1 -6 0 274.113 11.1819 1 -1 6 0 266.338 11.0967 1 -1 6 0 272.150 11.1135 1 -1 6 0 283.812 14.7963 3 0 -6 0 272.590 11.2411 1 0 -6 0 278.728 11.1898 1 0 6 0 280.899 14.7595 3 0 6 0 264.266 11.1164 1 -1 -6 0 3.66444 0.89546 1 -1 -6 0 2.58804 0.75541 1 1 6 0 2.41054 0.55856 1 1 6 0 4.13324 0.73546 1 1 6 0 1.89979 0.76074 3 -2 -6 0 187.960 7.79908 1 -2 -6 0 181.567 7.88422 1 2 6 0 177.937 10.0737 3 2 6 0 176.376 7.77208 1 2 6 0 178.253 7.79459 1 -3 -6 0 62.1492 3.40314 1 3 6 0 66.4679 3.65620 1 3 6 0 64.2353 4.50010 3 3 6 0 62.7604 3.53543 1 -4 -6 0 21.0764 2.02446 1 4 6 0 16.5670 2.00662 1 4 6 0 18.7731 2.19835 3 4 6 0 15.9461 1.71209 1 -5 -6 0 0.16925 1.33627 1 5 6 0 -0.9672 1.72656 1 5 6 0 1.05212 1.28493 1 5 6 0 -1.0016 1.43576 3 -6 -6 0 -0.5867 1.73623 1 6 6 0 -0.0049 1.63846 3 6 6 0 3.01986 2.41671 1 6 6 0 -1.5790 2.40696 1 9 -7 0 1.05117 1.26007 1 -9 7 0 2.75927 1.51982 3 8 -7 0 0.04446 1.11215 1 -8 7 0 -0.1589 1.24739 3 -8 7 0 0.20715 1.00774 2 7 -7 0 2.47332 0.75667 1 -7 7 0 2.85288 0.96792 3 -7 7 0 3.88868 0.93418 2 6 -7 0 153.625 6.44662 1 -6 7 0 154.638 8.69168 3 5 -7 0 15.2109 1.02601 1 -5 7 0 15.0544 1.72458 3 4 -7 0 64.1127 2.78060 1 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39.7598 4.05974 1 5 7 0 36.8979 3.52066 1 5 7 0 37.2508 3.82878 3 9 -8 0 55.7232 3.25985 1 -9 8 0 50.2555 4.00511 3 8 -8 0 13.8412 1.37041 1 -8 8 0 14.2812 2.14957 3 7 -8 0 4.35213 0.78614 1 -7 8 0 4.40966 1.59779 3 6 -8 0 7.10619 0.78574 1 -6 8 0 6.13315 1.33360 3 5 -8 0 1.78246 0.52065 1 -5 8 0 1.85258 1.27984 3 4 -8 0 9.34202 0.86817 1 -4 8 0 12.5324 1.83943 3 -4 8 0 9.77460 0.64537 1 -4 8 0 10.0465 0.75800 1 3 -8 0 388.127 15.4638 1 -3 8 0 376.526 15.2781 1 -3 8 0 389.165 15.3339 1 -3 8 0 387.171 20.5935 3 2 -8 0 52.0459 2.59733 1 2 -8 0 43.0319 2.43645 1 -2 8 0 49.0962 2.33432 1 -2 8 0 50.6156 2.41875 1 -2 8 0 47.9530 3.53665 3 1 -8 0 21.8055 1.77665 1 1 -8 0 23.9303 1.50560 1 -1 8 0 22.8827 2.51458 3 -1 8 0 20.3228 1.56657 1 -1 8 0 17.9980 1.26839 1 0 -8 0 8.12894 1.05363 1 0 8 0 7.04687 0.86660 1 0 8 0 6.46308 0.92473 1 -1 -8 0 19.1322 1.95412 1 -1 -8 0 20.6578 2.07641 1 1 8 0 19.6636 1.92992 1 1 8 0 22.2860 2.70756 3 1 8 0 15.4803 1.54384 1 -2 -8 0 45.3015 3.19804 1 -2 -8 0 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5 -11 119.639 7.85460 3 4 5 -11 109.050 6.32184 1 4 5 -11 110.670 6.05724 1 -4 -5 11 103.625 5.60282 1 -4 -5 11 109.820 7.08559 2 3 5 -11 43.9956 3.81090 1 3 5 -11 43.7326 3.41000 1 3 5 -11 50.9875 4.32121 3 -3 -5 11 46.3673 3.24391 1 -3 -5 11 45.5999 4.06977 2 2 5 -11 6.52922 2.27133 1 2 5 -11 -2.5941 1.18673 3 2 5 -11 0.16200 1.27576 1 -2 -5 11 -1.0108 1.63893 2 -2 -5 11 -0.3995 1.12465 1 1 5 -11 8.46971 2.13153 3 1 5 -11 10.6483 2.43259 1 -1 -5 11 8.20779 1.95305 1 -1 -5 11 9.77028 1.92854 2 0 5 -11 1.15092 2.01699 3 0 5 -11 2.65746 1.66380 1 0 -5 11 2.03071 1.14365 2 0 -5 11 1.32412 1.25730 1 -1 5 -11 -0.4203 2.35151 1 -1 5 -11 -0.1480 1.46469 3 1 -5 11 1.16752 1.43075 1 1 -5 11 1.45234 1.43347 2 -2 5 -11 162.577 10.4454 3 -2 5 -11 165.754 8.47847 1 2 -5 11 178.806 8.13635 1 5 4 -11 287.370 12.6912 1 5 4 -11 293.131 16.3886 3 5 4 -11 291.428 12.8831 1 -5 -4 11 290.052 12.4725 1 -5 -4 11 270.143 14.9099 2 4 4 -11 41.3348 3.37122 1 4 4 -11 46.3254 4.13787 3 4 4 -11 42.8412 3.23604 1 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