data_cu_140408lt_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 O6' _chemical_formula_weight 372.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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' _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.862(3) _cell_length_b 12.539(4) _cell_length_c 16.776(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1864.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5474 _cell_measurement_theta_min 5.6461 _cell_measurement_theta_max 66.3692 _exptl_crystal_description Lump _exptl_crystal_colour Colorless _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.327 _exptl_crystal_F_000 792 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_absorpt_coefficient_mu 0.800 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7820 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 6658 _diffrn_reflns_av_unetI/netI 0.0374 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.646 _diffrn_reflns_theta_max 66.464 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_Laue_measured_fraction_full 0.947 _diffrn_reflns_point_group_measured_fraction_max 0.923 _diffrn_reflns_point_group_measured_fraction_full 0.899 _reflns_number_total 3026 _reflns_number_gt 2996 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.648 _reflns_Friedel_fraction_max 0.855 _reflns_Friedel_fraction_full 0.833 _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 'APEX2 (Bruker AXS, 2010)' _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL' _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^)+(0.0548P)^2^+0.3507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1173 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.12(5) _chemical_absolute_configuration ? _refine_ls_number_reflns 3026 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration rm 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 0.1690(2) 0.44156(17) 0.98178(13) 0.0186(5) Uani 1 1 d . . . . . H1 H 0.0924 0.4062 0.9469 0.022 Uiso 1 1 calc R U . . . C2 C 0.0933(3) 0.46363(18) 1.06301(13) 0.0206(5) Uani 1 1 d . . . . . H2A H 0.0720 0.3949 1.0898 0.025 Uiso 1 1 calc R U . . . H2B H 0.1641 0.5042 1.0971 0.025 Uiso 1 1 calc R U . . . C3 C -0.0495(2) 0.52475(18) 1.05513(13) 0.0183(4) Uani 1 1 d . . . . . C4 C -0.1283(3) 0.59368(18) 1.10231(13) 0.0195(5) Uani 1 1 d . . . . . C5 C -0.2545(3) 0.63157(19) 1.05612(14) 0.0219(5) Uani 1 1 d . . . . . H5 H -0.3298 0.6807 1.0727 0.026 Uiso 1 1 calc R U . . . C6 C -0.2441(3) 0.58323(19) 0.98481(14) 0.0207(5) Uani 1 1 d . . . . . C7 C -0.3134(3) 0.59031(19) 0.90523(13) 0.0224(5) Uani 1 1 d . . . . . H7 H -0.3343 0.5206 0.8784 0.027 Uiso 1 1 calc R U . . . C8 C -0.2724(3) 0.68004(19) 0.85143(14) 0.0226(5) Uani 1 1 d . . . . . C9 C -0.2680(3) 0.6576(2) 0.76290(14) 0.0252(5) Uani 1 1 d . . . . . H9A H -0.2698 0.7263 0.7339 0.030 Uiso 1 1 calc R U . . . H9B H -0.3602 0.6176 0.7480 0.030 Uiso 1 1 calc R U . . . C10 C -0.1294(3) 0.59366(19) 0.73574(13) 0.0231(5) Uani 1 1 d . . . . . H10 H -0.1239 0.5974 0.6763 0.028 Uiso 1 1 calc R U . . . C11 C 0.0219(3) 0.62398(18) 0.76860(13) 0.0214(5) Uani 1 1 d . . . . . H11 H 0.0660 0.6927 0.7638 0.026 Uiso 1 1 calc R U . . . C12 C 0.0863(3) 0.54139(18) 0.80550(12) 0.0196(5) Uani 1 1 d . . . . . C13 C 0.2340(3) 0.53479(18) 0.84849(13) 0.0198(5) Uani 1 1 d . . . . . H13A H 0.3014 0.5918 0.8285 0.024 Uiso 1 1 calc R U . . . H13B H 0.2820 0.4654 0.8362 0.024 Uiso 1 1 calc R U . . . C14 C 0.2188(2) 0.54589(17) 0.93970(13) 0.0191(5) Uani 1 1 d . . . . . H14A H 0.1442 0.6025 0.9516 0.023 Uiso 1 1 calc R U . . . H14B H 0.3171 0.5687 0.9619 0.023 Uiso 1 1 calc R U . . . C15 C 0.2991(3) 0.3643(2) 0.99212(14) 0.0251(5) Uani 1 1 d . . . . . C16 C 0.3001(4) 0.2722(2) 0.95156(19) 0.0419(7) Uani 1 1 d . . . . . H16A H 0.3799 0.2227 0.9592 0.050 Uiso 1 1 calc R U . . . H16B H 0.2211 0.2565 0.9152 0.050 Uiso 1 1 calc R U . . . C17 C 0.4203(3) 0.3924(3) 1.04969(19) 0.0439(7) Uani 1 1 d . . . . . H17A H 0.4928 0.3335 1.0531 0.066 Uiso 1 1 calc R U . . . H17B H 0.3759 0.4051 1.1023 0.066 Uiso 1 1 calc R U . . . H17C H 0.4722 0.4570 1.0316 0.066 Uiso 1 1 calc R U . . . C18 C -0.0839(3) 0.62284(18) 1.18420(13) 0.0209(5) Uani 1 1 d . . . . . C19 C -0.1797(3) 0.7727(2) 0.88039(15) 0.0291(5) Uani 1 1 d . . . . . H19A H -0.2104 0.8375 0.8521 0.044 Uiso 1 1 calc R U . . . H19B H -0.0727 0.7586 0.8702 0.044 Uiso 1 1 calc R U . . . H19C H -0.1958 0.7823 0.9377 0.044 Uiso 1 1 calc R U . . . C20 C -0.0177(3) 0.44911(18) 0.79626(12) 0.0200(5) Uani 1 1 d . . . . . C21 C -0.1402(3) 0.7325(2) 1.29451(13) 0.0272(5) Uani 1 1 d . . . . . H21A H -0.2093 0.6932 1.3294 0.041 Uiso 1 1 calc R U . . . H21B H -0.1566 0.8093 1.3010 0.041 Uiso 1 1 calc R U . . . H21C H -0.0358 0.7150 1.3087 0.041 Uiso 1 1 calc R U . . . O1 O -0.12063(17) 0.51622(12) 0.98311(9) 0.0190(3) Uani 1 1 d . . . . . O2 O -0.41959(19) 0.67392(15) 0.88932(10) 0.0281(4) Uani 1 1 d . . . . . O3 O -0.14506(19) 0.48229(13) 0.75848(9) 0.0233(4) Uani 1 1 d . . . . . O4 O -0.16779(18) 0.70286(13) 1.21259(9) 0.0204(4) Uani 1 1 d . . . . . O5 O 0.0155(2) 0.57912(15) 1.22090(10) 0.0307(4) Uani 1 1 d . . . . . O6 O -0.0001(2) 0.35680(12) 0.81548(10) 0.0258(4) 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 0.0170(10) 0.0211(10) 0.0177(10) 0.0001(9) -0.0012(9) 0.0007(9) C2 0.0206(11) 0.0233(11) 0.0179(10) 0.0002(9) -0.0010(9) 0.0017(9) C3 0.0162(10) 0.0231(10) 0.0156(10) 0.0017(8) -0.0014(8) -0.0026(9) C4 0.0184(10) 0.0234(10) 0.0167(10) 0.0005(9) 0.0012(9) -0.0002(9) C5 0.0160(10) 0.0267(11) 0.0230(11) -0.0009(9) 0.0009(9) 0.0011(9) C6 0.0146(10) 0.0267(11) 0.0208(10) 0.0003(9) 0.0006(9) 0.0024(9) C7 0.0173(10) 0.0290(11) 0.0208(10) -0.0034(9) -0.0026(9) 0.0037(9) C8 0.0176(11) 0.0273(11) 0.0229(11) -0.0012(9) -0.0016(9) 0.0078(9) C9 0.0254(12) 0.0290(12) 0.0212(11) 0.0010(9) -0.0054(9) 0.0065(10) C10 0.0260(12) 0.0268(11) 0.0165(10) 0.0018(9) -0.0015(9) 0.0048(10) C11 0.0227(11) 0.0236(10) 0.0179(10) 0.0019(9) 0.0038(9) 0.0005(9) C12 0.0198(10) 0.0224(10) 0.0164(10) -0.0016(8) 0.0044(9) -0.0002(9) C13 0.0158(10) 0.0223(10) 0.0212(11) 0.0002(9) 0.0027(9) -0.0005(9) C14 0.0156(10) 0.0214(10) 0.0202(10) -0.0011(9) -0.0006(8) -0.0006(8) C15 0.0238(11) 0.0306(12) 0.0209(10) 0.0029(9) 0.0027(9) 0.0089(10) C16 0.0378(15) 0.0333(14) 0.0547(17) -0.0043(13) 0.0029(14) 0.0122(12) C17 0.0290(13) 0.0575(19) 0.0452(16) -0.0034(14) -0.0115(14) 0.0144(14) C18 0.0196(11) 0.0254(11) 0.0178(10) 0.0009(9) 0.0031(9) -0.0015(9) C19 0.0320(13) 0.0267(12) 0.0286(11) -0.0050(10) 0.0017(11) 0.0029(10) C20 0.0198(10) 0.0240(11) 0.0163(10) -0.0042(8) -0.0007(9) 0.0013(9) C21 0.0250(11) 0.0368(12) 0.0197(11) -0.0093(10) -0.0021(9) -0.0012(11) O1 0.0161(7) 0.0247(7) 0.0163(7) -0.0015(6) -0.0007(6) 0.0023(6) O2 0.0176(8) 0.0402(10) 0.0265(8) 0.0006(8) -0.0010(7) 0.0097(7) O3 0.0238(8) 0.0240(8) 0.0223(8) -0.0042(6) -0.0054(7) 0.0016(7) O4 0.0202(8) 0.0256(8) 0.0155(7) -0.0035(6) 0.0000(6) -0.0004(6) O5 0.0290(9) 0.0430(10) 0.0200(7) -0.0035(8) -0.0047(7) 0.0109(8) O6 0.0288(9) 0.0200(8) 0.0287(8) -0.0035(6) -0.0065(8) 0.0001(7) _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 C15 1.515(3) . ? C1 C2 1.544(3) . ? C1 C14 1.551(3) . ? C1 H1 1.0000 . ? C2 C3 1.486(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.364(3) . ? C3 O1 1.367(3) . ? C4 C5 1.441(3) . ? C4 C18 1.475(3) . ? C5 C6 1.344(3) . ? C5 H5 0.9500 . ? C6 O1 1.380(3) . ? C6 C7 1.472(3) . ? C7 O2 1.434(3) . ? C7 C8 1.487(4) . ? C7 H7 1.0000 . ? C8 O2 1.453(3) . ? C8 C19 1.503(3) . ? C8 C9 1.512(3) . ? C9 C10 1.536(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O3 1.454(3) . ? C10 C11 1.499(3) . ? C10 H10 1.0000 . ? C11 C12 1.335(3) . ? C11 H11 0.9500 . ? C12 C20 1.488(3) . ? C12 C13 1.497(3) . ? C13 C14 1.542(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.341(4) . ? C15 C17 1.487(4) . ? C16 H16A 0.9500 . ? C16 H16B 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O5 1.206(3) . ? C18 O4 1.337(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.212(3) . ? C20 O3 1.359(3) . ? C21 O4 1.445(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 C15 C1 C2 110.13(18) . . ? C15 C1 C14 112.01(19) . . ? C2 C1 C14 111.98(18) . . ? C15 C1 H1 107.5 . . ? C2 C1 H1 107.5 . . ? C14 C1 H1 107.5 . . ? C3 C2 C1 112.59(18) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 O1 109.06(19) . . ? C4 C3 C2 135.3(2) . . ? O1 C3 C2 115.54(18) . . ? C3 C4 C5 107.1(2) . . ? C3 C4 C18 124.1(2) . . ? C5 C4 C18 128.8(2) . . ? C6 C5 C4 106.1(2) . . ? C6 C5 H5 127.0 . . ? C4 C5 H5 127.0 . . ? C5 C6 O1 110.3(2) . . ? C5 C6 C7 138.7(2) . . ? O1 C6 C7 110.41(19) . . ? O2 C7 C6 119.12(19) . . ? O2 C7 C8 59.61(14) . . ? C6 C7 C8 119.6(2) . . ? O2 C7 H7 115.7 . . ? C6 C7 H7 115.7 . . ? C8 C7 H7 115.7 . . ? O2 C8 C7 58.37(15) . . ? O2 C8 C19 112.94(19) . . ? C7 C8 C19 121.4(2) . . ? O2 C8 C9 116.3(2) . . ? C7 C8 C9 117.5(2) . . ? C19 C8 C9 116.6(2) . . ? C8 C9 C10 114.16(19) . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O3 C10 C11 103.42(18) . . ? O3 C10 C9 110.3(2) . . ? C11 C10 C9 118.30(19) . . ? O3 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C9 C10 H10 108.1 . . ? C12 C11 C10 110.9(2) . . ? C12 C11 H11 124.6 . . ? C10 C11 H11 124.6 . . ? C11 C12 C20 106.9(2) . . ? C11 C12 C13 129.8(2) . . ? C20 C12 C13 123.3(2) . . ? C12 C13 C14 113.37(18) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C1 113.60(18) . . ? C13 C14 H14A 108.8 . . ? C1 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C1 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C17 121.9(3) . . ? C16 C15 C1 119.8(2) . . ? C17 C15 C1 118.2(2) . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? 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 . . ? O5 C18 O4 124.4(2) . . ? O5 C18 C4 123.9(2) . . ? O4 C18 C4 111.68(19) . . ? C8 C19 H19A 109.5 . . ? C8 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C8 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 O3 121.5(2) . . ? O6 C20 C12 129.5(2) . . ? O3 C20 C12 108.98(19) . . ? O4 C21 H21A 109.5 . . ? O4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 O1 C6 107.44(17) . . ? C7 O2 C8 62.02(15) . . ? C20 O3 C10 109.70(18) . . ? C18 O4 C21 115.95(18) . . ? _refine_diff_density_max 0.347 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.076 _shelxl_version_number 2013-4 _shelx_res_file ; TITL cu_140408lt_0m in P2(1)2(1)2(1) CELL 1.54178 8.8620 12.5386 16.7758 90.000 90.000 90.000 ZERR 4.00 0.0028 0.0040 0.0054 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O UNIT 84 96 24 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.054800 0.350700 FVAR 1.14300 MOLE 1 C1 1 0.169009 0.441556 0.981781 11.00000 0.01698 0.02111 = 0.01774 0.00014 -0.00125 0.00072 AFIX 13 H1 2 0.092357 0.406225 0.946905 11.00000 -1.20000 AFIX 0 C2 1 0.093305 0.463635 1.063012 11.00000 0.02062 0.02334 = 0.01790 0.00023 -0.00097 0.00174 AFIX 23 H2A 2 0.071985 0.394886 1.089759 11.00000 -1.20000 H2B 2 0.164135 0.504187 1.097128 11.00000 -1.20000 AFIX 0 C3 1 -0.049545 0.524748 1.055125 11.00000 0.01625 0.02312 = 0.01560 0.00166 -0.00139 -0.00255 C4 1 -0.128318 0.593677 1.102306 11.00000 0.01845 0.02335 = 0.01673 0.00051 0.00118 -0.00024 C5 1 -0.254494 0.631570 1.056122 11.00000 0.01595 0.02667 = 0.02304 -0.00092 0.00092 0.00110 AFIX 43 H5 2 -0.329766 0.680741 1.072706 11.00000 -1.20000 AFIX 0 C6 1 -0.244090 0.583231 0.984809 11.00000 0.01462 0.02674 = 0.02075 0.00031 0.00056 0.00240 C7 1 -0.313370 0.590306 0.905228 11.00000 0.01730 0.02902 = 0.02080 -0.00337 -0.00260 0.00372 AFIX 13 H7 2 -0.334323 0.520643 0.878400 11.00000 -1.20000 AFIX 0 C8 1 -0.272423 0.680041 0.851428 11.00000 0.01757 0.02730 = 0.02286 -0.00123 -0.00162 0.00784 C9 1 -0.268024 0.657579 0.762897 11.00000 0.02541 0.02905 = 0.02123 0.00098 -0.00537 0.00654 AFIX 23 H9A 2 -0.269794 0.726299 0.733853 11.00000 -1.20000 H9B 2 -0.360178 0.617648 0.747999 11.00000 -1.20000 AFIX 0 C10 1 -0.129450 0.593664 0.735738 11.00000 0.02596 0.02675 = 0.01648 0.00180 -0.00147 0.00481 AFIX 13 H10 2 -0.123898 0.597374 0.676265 11.00000 -1.20000 AFIX 0 C11 1 0.021895 0.623980 0.768602 11.00000 0.02271 0.02360 = 0.01789 0.00189 0.00377 0.00047 AFIX 43 H11 2 0.066016 0.692734 0.763811 11.00000 -1.20000 AFIX 0 C12 1 0.086326 0.541386 0.805498 11.00000 0.01979 0.02245 = 0.01644 -0.00164 0.00438 -0.00024 C13 1 0.234006 0.534788 0.848490 11.00000 0.01579 0.02230 = 0.02124 0.00021 0.00269 -0.00047 AFIX 23 H13A 2 0.301355 0.591810 0.828480 11.00000 -1.20000 H13B 2 0.282025 0.465429 0.836174 11.00000 -1.20000 AFIX 0 C14 1 0.218802 0.545889 0.939696 11.00000 0.01564 0.02144 = 0.02021 -0.00113 -0.00059 -0.00056 AFIX 23 H14A 2 0.144234 0.602485 0.951592 11.00000 -1.20000 H14B 2 0.317106 0.568736 0.961928 11.00000 -1.20000 AFIX 0 C15 1 0.299090 0.364332 0.992122 11.00000 0.02382 0.03063 = 0.02089 0.00293 0.00274 0.00887 C16 1 0.300145 0.272211 0.951556 11.00000 0.03777 0.03332 = 0.05469 -0.00425 0.00294 0.01219 AFIX 93 H16A 2 0.379939 0.222663 0.959211 11.00000 -1.20000 H16B 2 0.221097 0.256481 0.915157 11.00000 -1.20000 AFIX 0 C17 1 0.420327 0.392363 1.049685 11.00000 0.02897 0.05748 = 0.04517 -0.00336 -0.01153 0.01439 AFIX 137 H17A 2 0.492796 0.333501 1.053084 11.00000 -1.50000 H17B 2 0.375886 0.405067 1.102329 11.00000 -1.50000 H17C 2 0.472213 0.456997 1.031587 11.00000 -1.50000 AFIX 0 C18 1 -0.083888 0.622835 1.184200 11.00000 0.01958 0.02537 = 0.01783 0.00092 0.00307 -0.00154 C19 1 -0.179745 0.772670 0.880393 11.00000 0.03205 0.02667 = 0.02860 -0.00503 0.00169 0.00288 AFIX 137 H19A 2 -0.210362 0.837532 0.852095 11.00000 -1.50000 H19B 2 -0.072691 0.758577 0.870223 11.00000 -1.50000 H19C 2 -0.195762 0.782291 0.937746 11.00000 -1.50000 AFIX 0 C20 1 -0.017727 0.449113 0.796257 11.00000 0.01981 0.02398 = 0.01632 -0.00425 -0.00074 0.00131 C21 1 -0.140158 0.732468 1.294511 11.00000 0.02502 0.03683 = 0.01972 -0.00926 -0.00206 -0.00119 AFIX 137 H21A 2 -0.209320 0.693237 1.329411 11.00000 -1.50000 H21B 2 -0.156645 0.809261 1.301024 11.00000 -1.50000 H21C 2 -0.035762 0.714997 1.308679 11.00000 -1.50000 AFIX 0 O1 3 -0.120630 0.516224 0.983111 11.00000 0.01608 0.02466 = 0.01630 -0.00154 -0.00068 0.00234 O2 3 -0.419587 0.673921 0.889321 11.00000 0.01762 0.04019 = 0.02654 0.00057 -0.00100 0.00971 O3 3 -0.145059 0.482286 0.758482 11.00000 0.02378 0.02398 = 0.02227 -0.00418 -0.00544 0.00161 O4 3 -0.167794 0.702857 1.212588 11.00000 0.02022 0.02562 = 0.01546 -0.00349 0.00001 -0.00044 O5 3 0.015506 0.579117 1.220903 11.00000 0.02901 0.04295 = 0.02004 -0.00353 -0.00467 0.01093 O6 3 -0.000146 0.356797 0.815476 11.00000 0.02877 0.01996 = 0.02871 -0.00349 -0.00654 0.00015 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cu_140408lt_0m in P2(1)2(1)2(1) REM R1 = 0.0330 for 2996 Fo > 4sig(Fo) and 0.0332 for all 3026 data REM 247 parameters refined using 0 restraints END WGHT 0.0544 0.3651 REM Highest difference peak 0.347, deepest hole -0.261, 1-sigma level 0.076 Q1 1 0.4764 0.4148 1.0042 11.00000 0.05 0.35 Q2 1 -0.5218 0.7197 0.9608 11.00000 0.05 0.24 Q3 1 -0.0339 0.5821 1.0753 11.00000 0.05 0.24 Q4 1 0.0175 0.6601 1.0232 11.00000 0.05 0.23 Q5 1 0.5217 0.2458 0.9985 11.00000 0.05 0.21 ; 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4.73385 2 4 -2 0 376.010 24.1488 2 4 2 0 395.747 24.5054 2 5 2 0 456.666 29.1781 2 6 -2 0 133.101 10.3213 2 6 2 0 99.7254 9.92578 2 -7 2 0 12.8840 1.57945 4 -8 -2 0 534.761 16.3861 3 8 -2 0 524.908 18.1949 1 -8 2 0 555.892 16.3842 4 9 2 0 13.8420 1.90145 1 9 -2 0 17.0715 2.17429 1 -9 -2 0 13.2556 1.64158 3 10 -2 0 3.49659 1.11530 1 -10 -2 0 5.43548 1.02285 3 10 2 0 5.79094 1.10748 1 1 -3 0 6567.74 376.936 2 2 3 0 329.452 20.2189 2 2 -3 0 319.135 19.9476 2 3 3 0 1782.28 100.100 2 3 -3 0 1636.62 99.5614 2 4 3 0 563.885 37.6303 2 4 -3 0 658.224 37.4896 2 5 3 0 534.865 34.2297 2 6 -3 0 1449.75 87.4044 2 -6 3 0 1473.03 42.9496 4 7 -3 0 1030.72 32.9437 1 -7 3 0 1042.61 31.3477 4 -7 -3 0 1068.91 29.7548 3 -8 -3 0 233.576 8.18342 3 8 -3 0 236.256 9.34710 1 -8 3 0 244.532 8.18662 4 -9 -3 0 188.713 6.79330 3 9 -3 0 202.672 7.95870 1 10 -3 0 -0.0734 0.70482 1 -10 -3 0 0.25765 0.59232 3 1 -4 0 3323.25 191.640 2 2 -4 0 1667.28 97.2282 2 3 4 0 1696.89 95.3001 2 3 -4 0 1539.41 94.6507 2 4 -4 0 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0 15.3273 2.04937 5 3 -6 0 16.8267 3.28660 2 4 -6 0 3.65556 2.04700 2 4 -6 0 7.12864 1.60933 5 4 6 0 4.32859 2.69729 2 5 6 0 396.201 27.5955 2 5 -6 0 402.537 16.8799 5 5 -6 0 400.449 26.8668 2 6 -6 0 517.318 17.5362 1 -6 -6 0 535.053 15.5979 3 -7 -6 0 40.0804 2.40046 3 7 -6 0 37.5577 3.19244 1 -8 6 0 8.75931 1.47426 4 -8 -6 0 9.05939 1.21873 3 8 -6 0 8.44101 1.55888 1 -9 -6 0 30.7320 1.67434 3 -9 6 0 31.5548 1.42649 4 9 -6 0 26.0683 2.22271 1 0 -7 0 1.19036 0.76726 5 1 -7 0 361.555 14.6754 5 2 -7 0 641.521 24.9811 5 3 7 0 134.248 11.0190 2 3 -7 0 118.924 6.47408 5 3 -7 0 121.975 10.1142 2 4 7 0 7.43176 3.35274 2 4 -7 0 9.51464 2.97839 2 4 -7 0 14.7963 2.40000 5 5 -7 0 115.210 6.67711 5 6 -7 0 41.4582 2.95991 1 -6 -7 0 43.4331 2.46789 3 6 -7 0 43.1600 3.82444 5 7 -7 0 31.7227 2.79161 1 -7 -7 0 28.3666 2.11486 3 8 -7 0 319.979 11.4418 1 -8 -7 0 333.208 10.0515 3 -8 7 0 340.401 11.0734 4 9 -7 0 27.4130 1.86287 1 -9 -7 0 28.6720 1.28658 3 0 -8 0 95.0555 5.06792 5 1 -8 0 2169.20 79.8529 5 2 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0 35.8341 2.02386 3 5 -12 0 0.63467 0.60710 4 -5 12 0 1.98562 0.78934 1 -5 -12 0 0.89094 0.53232 3 0 13 0 0.44155 0.77198 1 -1 13 0 122.494 5.16854 1 -1 -13 0 115.580 4.75542 3 -2 13 0 2.13249 0.87864 1 -2 -13 0 1.45734 0.76467 3 -3 -13 0 0.50510 0.60070 3 -3 13 0 -0.0318 0.70733 1 -4 13 0 107.671 4.44389 1 -4 -13 0 114.165 3.84490 3 -5 13 0 30.8348 1.74176 1 0 -14 0 62.9047 3.02956 3 0 14 0 70.2438 3.23356 1 1 14 0 4.93945 0.91325 1 -1 14 0 3.43036 0.85855 1 -1 -14 0 5.79995 1.01049 3 -2 -14 0 2.54038 0.72793 3 -2 14 0 3.48273 0.86550 1 -3 -14 0 29.9071 1.53826 3 -3 14 0 32.9709 1.91368 1 1 0 -1 194.149 11.8025 2 3 0 1 622.439 37.2129 2 4 0 -1 19.6176 3.42359 2 5 0 1 37.0423 4.29631 2 5 0 -1 27.9496 4.01887 2 6 0 -1 69.3081 7.26481 2 6 0 1 80.2071 7.46668 2 -7 0 1 679.897 20.3055 4 -7 0 -1 672.741 19.5564 4 -8 0 -1 122.621 5.17613 3 8 0 -1 117.415 5.73923 1 8 0 1 129.959 5.83271 1 9 0 1 93.5924 4.83408 1 9 0 -1 98.5475 4.98708 1 -9 0 -1 103.446 4.48218 3 10 0 1 44.3295 2.73093 1 10 0 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199.320 6.92457 3 -10 -1 1 213.875 7.01930 3 10 -1 -1 221.294 7.85604 1 0 -2 -1 23.9316 2.06259 2 2 -2 1 3505.96 210.131 2 2 2 -1 3938.77 210.602 2 2 -2 -1 3531.25 210.317 2 2 2 1 3646.13 210.365 2 3 -2 1 4204.29 251.832 2 3 2 -1 4661.00 252.326 2 3 -2 -1 4265.05 251.987 2 4 -2 1 3117.60 179.174 2 4 2 -1 2975.24 179.490 2 4 -2 -1 3190.68 179.399 2 5 2 -1 434.279 26.6066 2 5 -2 1 394.605 25.9871 2 5 -2 -1 394.918 26.2008 2 6 -2 1 2216.17 130.434 2 -6 -2 1 2144.62 63.2280 4 -6 2 -1 2169.05 63.8618 4 6 -2 -1 2342.84 130.952 2 -7 2 1 194.236 7.27203 4 -7 2 -1 201.972 6.97454 4 -8 2 1 91.1167 3.96028 4 8 2 -1 94.8352 4.82570 1 -8 -2 -1 92.4598 4.15308 3 8 -2 1 92.2691 4.88460 1 -8 -2 1 87.5940 4.27139 3 8 -2 -1 97.1479 4.97380 1 -8 2 -1 92.9941 3.35045 4 -9 -2 -1 97.8627 4.23489 3 9 2 -1 96.1705 4.82787 1 9 -2 1 103.608 5.05207 1 -9 -2 1 97.0621 4.39122 3 9 -2 -1 103.485 5.06520 1 10 2 -1 150.555 6.04633 1 -10 -2 -1 153.734 5.37075 3 10 -2 1 159.538 6.28691 1 10 -2 -1 170.783 6.38498 1 -10 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29.8719 2.53711 1 5 -9 9 31.4588 2.56690 1 5 9 -9 26.7506 2.46764 1 -5 9 -9 34.1787 2.54296 4 -6 9 9 12.3988 1.43808 1 6 -9 9 12.5352 1.47561 1 6 9 -9 12.5657 1.58373 1 -6 9 -9 12.3006 1.01097 4 0 10 -9 0.36505 0.82661 1 0 -10 -9 2.10638 0.72958 3 -1 -10 -9 1001.64 27.3281 3 1 10 -9 985.573 30.9323 1 1 -10 -9 1024.92 28.0429 3 -1 10 -9 971.162 30.7634 1 -1 -10 9 955.804 29.9197 4 2 10 -9 134.635 5.83156 1 -2 -10 -9 130.682 3.97268 3 -2 -10 9 132.989 5.42522 4 2 -10 -9 138.278 5.28092 3 -3 10 9 175.253 6.77965 1 3 10 -9 170.447 6.95224 1 -3 -10 9 168.574 6.06170 4 4 10 -9 56.4109 3.33746 1 -4 10 9 57.7394 3.22814 1 5 10 -9 84.0037 4.03195 1 -5 10 9 90.8638 3.99109 1 -5 10 -9 82.0164 3.73351 4 6 10 -9 146.679 5.49314 1 -6 10 9 139.693 5.24365 1 0 11 -9 22.6491 2.20274 1 0 -11 -9 21.2383 1.61647 3 0 -11 9 22.9892 2.20273 4 -1 -11 -9 108.185 3.54372 3 1 11 -9 93.5232 4.59523 1 1 -11 -9 103.920 4.09829 3 -1 11 -9 106.749 4.64420 1 -1 -11 9 103.535 4.41145 4 2 11 -9 38.4051 2.63022 1 2 -11 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282.438 12.3240 5 -1 3 -10 281.631 12.1704 5 -2 -3 -10 313.496 13.8036 5 2 -3 -10 330.706 13.9284 5 -2 3 -10 319.308 13.8410 5 -3 -3 -10 2784.12 99.2545 5 -3 3 -10 2650.30 77.2481 4 3 -3 -10 2665.81 99.1947 5 -4 3 -10 561.881 16.5970 4 -5 -3 -10 411.246 11.4942 3 -5 3 10 427.542 14.1178 1 5 -3 10 402.546 14.0070 1 5 3 -10 409.898 14.3318 1 6 -3 10 706.556 22.9845 1 6 3 -10 715.020 23.3241 1 -6 3 10 743.697 22.9779 1 -6 3 -10 699.849 20.8507 3 7 3 -10 391.573 13.4717 1 7 -3 10 377.143 13.1270 1 -7 3 -10 390.189 12.0054 3 -7 -3 10 383.856 12.8386 4 8 3 -10 130.868 5.44830 1 8 -3 10 126.544 5.27176 1 -8 -3 10 131.771 4.50050 4 -8 3 -10 131.456 4.71451 3 0 -4 -10 281.479 12.4811 5 0 4 -10 280.957 12.1713 5 -1 -4 -10 153.816 7.77773 5 1 -4 -10 173.851 8.09495 5 1 -4 -10 142.542 4.93725 4 -2 -4 -10 1373.36 51.1874 5 -2 4 -10 1331.87 40.0000 4 2 -4 -10 1332.25 39.4168 4 2 -4 -10 1394.39 51.4369 5 -3 -4 -10 243.150 11.1589 5 -3 4 -10 233.645 8.40115 4 3 -4 -10 251.085 8.49012 4 3 -4 -10 256.390 11.4938 5 -4 4 10 107.943 4.91254 1 -4 4 -10 107.428 4.22339 4 4 -4 -10 110.548 4.86749 4 5 -4 10 1577.35 48.0049 1 5 4 -10 1557.45 48.2100 1 -5 4 10 1578.25 47.8882 1 6 -4 10 272.206 9.95664 1 -6 4 10 263.457 9.68091 1 6 4 -10 273.159 10.1005 1 -6 -4 10 251.456 9.59051 4 7 -4 10 90.4127 4.42383 1 7 4 -10 94.5666 4.62937 1 -7 4 10 94.1494 4.23515 1 -7 4 -10 86.3700 3.98936 3 -7 -4 10 89.3987 4.05393 4 8 -4 10 131.874 5.30450 1 8 4 -10 125.349 5.28560 1 -8 4 -10 126.996 4.65697 3 0 -5 -10 125.474 6.89896 5 -1 -5 -10 727.440 29.1600 5 1 -5 -10 757.767 29.4934 5 -2 -5 -10 457.701 18.8281 5 2 -5 -10 485.003 19.2300 5 -2 5 -10 425.537 14.6693 4 2 -5 -10 445.369 13.6922 4 -3 5 -10 256.345 9.00991 4 3 -5 -10 252.708 8.56589 4 3 -5 -10 253.550 11.9290 5 -4 5 10 1076.28 33.8466 1 4 5 -10 1085.54 34.1442 1 4 -5 10 1097.26 33.9867 1 4 -5 -10 1107.81 32.6323 4 4 -5 -10 1062.66 42.0205 5 -4 5 -10 1123.18 32.3749 4 5 5 -10 268.985 10.1838 1 5 -5 10 281.026 10.0789 1 -5 5 10 259.876 9.82426 1 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