data_shelx loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 8 _journal_issue 3 _journal_year 2017 _journal_page_first 248 _journal_page_last 251 _audit_creation_date 31-10-15 _audit_creation_method 'SHELXL-2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H36 O3' _chemical_formula_sum 'C21 H36 O3' _chemical_formula_weight 336.50 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 monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.4156(19) _cell_length_b 6.3672(6) _cell_length_c 12.7186(12) _cell_angle_alpha 90 _cell_angle_beta 90.509(5) _cell_angle_gamma 90 _cell_volume 1005.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.4250 _cell_measurement_theta_max 28.6427 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.112 _exptl_crystal_F_000 372 _exptl_transmission_factor_min 0.6829 _exptl_transmission_factor_max 0.7534 _exptl_crystal_size_max 0.111 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_min 0.053 _exptl_absorpt_coefficient_mu 0.562 _shelx_estimated_absorpt_T_min 0.940 _shelx_estimated_absorpt_T_max 0.971 _exptl_absorpt_correction_type empirical #Semi empirical from equivalents _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 12352 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.475 _diffrn_reflns_theta_max 71.924 _diffrn_reflns_theta_full 67.500 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_point_group_measured_fraction_full 0.991 _reflns_number_total 3777 _reflns_number_gt 3636 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.789 _reflns_Friedel_fraction_max 0.934 _reflns_Friedel_fraction_full 0.980 _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 'APEX3 (Bruker, 2016)' _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_reduction 'SAINT (Bruker, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia,2012)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2015b)' _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^+0.1015P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1584 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 3777 _refine_ls_number_parameters 221 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.43776(15) 0.5725(3) -0.02204(13) 0.0724(5) Uani 1 1 d . . . . . O2 O 0.14276(14) 0.5443(2) 0.56038(12) 0.0616(4) Uani 1 1 d . . . . . O3 O -0.04321(13) 0.4433(4) 0.66736(14) 0.0744(5) Uani 1 1 d . . . . . H3 H -0.037329 0.499824 0.609759 0.112 Uiso 1 1 calc R U . . . C1 C 0.46881(19) 0.5335(4) 0.06649(19) 0.0584(5) Uani 1 1 d . . . . . C2 C 0.58405(19) 0.5587(5) 0.1016(2) 0.0693(6) Uani 1 1 d . . . . . H2A H 0.622303 0.639485 0.049153 0.083 Uiso 1 1 calc R U . . . H2B H 0.617336 0.421055 0.105572 0.083 Uiso 1 1 calc R U . . . C3 C 0.59651(19) 0.6667(5) 0.2075(2) 0.0733(7) Uani 1 1 d . . . . . H3A H 0.585471 0.816339 0.198045 0.088 Uiso 1 1 calc R U . . . H3B H 0.669676 0.646282 0.232839 0.088 Uiso 1 1 calc R U . . . C4 C 0.51840(18) 0.5868(4) 0.29087(19) 0.0628(6) Uani 1 1 d . . . . . H4A H 0.524731 0.673879 0.353214 0.075 Uiso 1 1 calc R U . . . H4B H 0.537839 0.444390 0.310317 0.075 Uiso 1 1 calc R U . . . C5 C 0.40145(16) 0.5902(3) 0.25139(16) 0.0493(4) Uani 1 1 d . . . . . C6 C 0.39682(16) 0.4510(3) 0.15120(16) 0.0526(5) Uani 1 1 d . . . . . H6 H 0.425850 0.313616 0.171548 0.063 Uiso 1 1 calc R U . . . C7 C 0.27799(18) 0.4183(5) 0.12892(17) 0.0671(6) Uani 1 1 d . . . . . H7A H 0.265592 0.285736 0.093193 0.080 Uiso 1 1 calc R U . . . H7B H 0.249125 0.531248 0.085976 0.080 Uiso 1 1 calc R U . . . C8 C 0.22655(17) 0.4178(4) 0.23879(16) 0.0599(5) Uani 1 1 d . . . . . H8A H 0.197169 0.280269 0.254406 0.072 Uiso 1 1 calc R U . . . H8B H 0.168733 0.520049 0.241760 0.072 Uiso 1 1 calc R U . . . C9 C 0.31667(15) 0.4749(3) 0.31910(15) 0.0483(4) Uani 1 1 d . . . . . H9 H 0.349488 0.342450 0.342114 0.058 Uiso 1 1 calc R U . . . C10 C 0.3655(2) 0.8164(4) 0.2268(2) 0.0662(6) Uani 1 1 d . . . . . H10A H 0.290211 0.817215 0.208856 0.099 Uiso 1 1 calc R U . . . H10B H 0.406170 0.869680 0.168748 0.099 Uiso 1 1 calc R U . . . H10C H 0.377642 0.903397 0.287379 0.099 Uiso 1 1 calc R U . . . C11 C 0.27297(18) 0.5833(3) 0.41802(17) 0.0539(5) Uani 1 1 d . . . . . H11 H 0.238881 0.714739 0.395309 0.065 Uiso 1 1 calc R U . . . C12 C 0.3591(2) 0.6398(5) 0.4991(2) 0.0766(7) Uani 1 1 d . . . . . H12A H 0.405281 0.521033 0.510741 0.115 Uiso 1 1 calc R U . . . H12B H 0.325375 0.678380 0.563935 0.115 Uiso 1 1 calc R U . . . H12C H 0.400937 0.755768 0.473754 0.115 Uiso 1 1 calc R U . . . C13 C 0.18443(18) 0.4456(4) 0.46668(16) 0.0550(5) Uani 1 1 d . . . . . H13 H 0.125359 0.432857 0.415452 0.066 Uiso 1 1 calc R U . . . C14 C 0.2182(2) 0.2247(4) 0.50035(19) 0.0606(5) Uani 1 1 d . . . . . H14A H 0.203921 0.123147 0.445114 0.073 Uiso 1 1 calc R U . . . H14B H 0.294050 0.219766 0.519194 0.073 Uiso 1 1 calc R U . . . C15 C 0.1475(2) 0.1850(4) 0.59570(19) 0.0614(5) Uani 1 1 d . . . . . H15A H 0.075223 0.143265 0.575017 0.074 Uiso 1 1 calc R U . . . H15B H 0.178342 0.078868 0.641642 0.074 Uiso 1 1 calc R U . . . C16 C 0.14841(17) 0.4002(3) 0.64718(16) 0.0519(5) Uani 1 1 d . . . . . H16 H 0.217498 0.419547 0.683774 0.062 Uiso 1 1 calc R U . . . C17 C 0.05745(16) 0.4546(4) 0.72272(16) 0.0522(5) Uani 1 1 d . . . . . C18 C 0.07124(19) 0.6778(4) 0.76563(19) 0.0597(5) Uani 1 1 d . . . . . H18A H 0.068961 0.774589 0.706776 0.072 Uiso 1 1 calc R U . . . H18B H 0.010032 0.709199 0.809810 0.072 Uiso 1 1 calc R U . . . C19 C 0.1726(2) 0.7200(5) 0.8281(3) 0.0815(8) Uani 1 1 d . . . . . H19A H 0.233638 0.713164 0.782515 0.122 Uiso 1 1 calc R U . . . H19B H 0.180028 0.616557 0.882624 0.122 Uiso 1 1 calc R U . . . H19C H 0.168567 0.857252 0.859118 0.122 Uiso 1 1 calc R U . . . C20 C 0.0517(2) 0.2894(4) 0.8097(2) 0.0678(6) Uani 1 1 d . . . . . H20A H 0.035989 0.154305 0.777833 0.081 Uiso 1 1 calc R U . . . H20B H 0.121946 0.279147 0.843359 0.081 Uiso 1 1 calc R U . . . C21 C -0.0320(3) 0.3332(6) 0.8936(2) 0.0925(10) Uani 1 1 d . . . . . H21A H -0.099201 0.369654 0.860556 0.139 Uiso 1 1 calc R U . . . H21B H -0.007992 0.447459 0.937167 0.139 Uiso 1 1 calc R U . . . H21C H -0.041463 0.210061 0.936108 0.139 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 0.0848(11) 0.0739(11) 0.0586(9) 0.0059(8) 0.0074(8) -0.0002(9) O2 0.0796(10) 0.0499(8) 0.0555(8) 0.0105(7) 0.0150(7) 0.0109(7) O3 0.0541(8) 0.0999(14) 0.0692(9) -0.0014(10) -0.0074(7) -0.0046(9) C1 0.0642(12) 0.0508(12) 0.0603(12) -0.0001(10) 0.0106(10) 0.0025(9) C2 0.0556(12) 0.0726(15) 0.0801(15) 0.0026(13) 0.0140(11) -0.0039(11) C3 0.0519(12) 0.0779(16) 0.0900(17) -0.0030(14) 0.0030(11) -0.0138(12) C4 0.0533(11) 0.0697(14) 0.0653(12) -0.0018(11) -0.0046(9) -0.0071(11) C5 0.0478(10) 0.0466(10) 0.0534(10) 0.0015(9) 0.0000(8) -0.0017(9) C6 0.0512(10) 0.0515(11) 0.0552(11) -0.0005(9) 0.0026(8) -0.0012(9) C7 0.0557(12) 0.0911(18) 0.0544(11) -0.0087(12) 0.0009(9) -0.0084(12) C8 0.0491(10) 0.0727(14) 0.0580(11) -0.0013(11) 0.0019(8) -0.0064(10) C9 0.0494(10) 0.0437(10) 0.0517(10) 0.0019(8) 0.0003(8) -0.0012(8) C10 0.0758(15) 0.0505(12) 0.0724(14) 0.0063(10) 0.0103(12) 0.0028(11) C11 0.0619(12) 0.0458(10) 0.0542(10) 0.0016(9) 0.0065(9) -0.0017(9) C12 0.0873(17) 0.0811(18) 0.0616(13) -0.0139(13) 0.0057(12) -0.0243(14) C13 0.0589(11) 0.0539(12) 0.0523(10) 0.0026(10) 0.0054(9) 0.0014(9) C14 0.0685(13) 0.0474(11) 0.0658(13) -0.0040(9) 0.0062(11) -0.0026(10) C15 0.0740(14) 0.0475(11) 0.0628(12) 0.0045(10) 0.0046(10) -0.0065(10) C16 0.0550(10) 0.0453(10) 0.0555(10) 0.0075(8) -0.0019(8) -0.0012(8) C17 0.0507(10) 0.0527(11) 0.0532(10) 0.0057(9) -0.0026(8) -0.0043(9) C18 0.0638(12) 0.0522(11) 0.0632(12) 0.0064(10) 0.0080(10) 0.0024(10) C19 0.0813(17) 0.0705(16) 0.0926(19) -0.0227(15) -0.0022(14) -0.0097(14) C20 0.0824(16) 0.0564(13) 0.0646(13) 0.0105(11) 0.0057(12) -0.0120(12) C21 0.116(2) 0.091(2) 0.0712(16) 0.0076(16) 0.0256(16) -0.0264(19) _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 1.213(3) . ? O2 C16 1.437(2) . ? O2 C13 1.447(3) . ? O3 C17 1.431(3) . ? O3 H3 0.8200 . ? C1 C6 1.501(3) . ? C1 C2 1.504(3) . ? C2 C3 1.519(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.531(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.532(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.539(3) . ? C5 C9 1.551(3) . ? C5 C6 1.553(3) . ? C6 C7 1.514(3) . ? C6 H6 0.9800 . ? C7 C8 1.542(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.551(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.538(3) . ? C9 H9 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.522(4) . ? C11 C13 1.540(3) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.528(3) . ? C13 H13 0.9800 . ? C14 C15 1.525(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.519(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.529(3) . ? C16 H16 0.9800 . ? C17 C20 1.528(3) . ? C17 C18 1.531(3) . ? C18 C19 1.506(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.522(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 C16 O2 C13 109.87(16) . . ? C17 O3 H3 109.5 . . ? O1 C1 C6 123.5(2) . . ? O1 C1 C2 123.2(2) . . ? C6 C1 C2 113.3(2) . . ? C1 C2 C3 113.63(19) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 113.8(2) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 111.88(19) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C10 110.61(19) . . ? C4 C5 C9 117.21(17) . . ? C10 C5 C9 111.04(17) . . ? C4 C5 C6 106.79(17) . . ? C10 C5 C6 111.02(18) . . ? C9 C5 C6 99.50(15) . . ? C1 C6 C7 119.95(19) . . ? C1 C6 C5 111.81(17) . . ? C7 C6 C5 105.13(17) . . ? C1 C6 H6 106.4 . . ? C7 C6 H6 106.4 . . ? C5 C6 H6 106.4 . . ? C6 C7 C8 103.97(17) . . ? C6 C7 H7A 111.0 . . ? C8 C7 H7A 111.0 . . ? C6 C7 H7B 111.0 . . ? C8 C7 H7B 111.0 . . ? H7A C7 H7B 109.0 . . ? C7 C8 C9 107.11(16) . . ? C7 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? C7 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? C11 C9 C5 119.18(17) . . ? C11 C9 C8 112.71(17) . . ? C5 C9 C8 103.55(16) . . ? C11 C9 H9 106.9 . . ? C5 C9 H9 106.9 . . ? C8 C9 H9 106.9 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 114.17(19) . . ? C12 C11 C13 111.22(18) . . ? C9 C11 C13 109.33(17) . . ? C12 C11 H11 107.3 . . ? C9 C11 H11 107.3 . . ? C13 C11 H11 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C14 105.57(17) . . ? O2 C13 C11 110.18(18) . . ? C14 C13 C11 116.21(18) . . ? O2 C13 H13 108.2 . . ? C14 C13 H13 108.2 . . ? C11 C13 H13 108.2 . . ? C15 C14 C13 102.53(19) . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C16 C15 C14 101.03(18) . . ? C16 C15 H15A 111.6 . . ? C14 C15 H15A 111.6 . . ? C16 C15 H15B 111.6 . . ? C14 C15 H15B 111.6 . . ? H15A C15 H15B 109.4 . . ? O2 C16 C15 104.17(17) . . ? O2 C16 C17 107.87(16) . . ? C15 C16 C17 118.20(19) . . ? O2 C16 H16 108.7 . . ? C15 C16 H16 108.7 . . ? C17 C16 H16 108.7 . . ? O3 C17 C20 106.00(18) . . ? O3 C17 C16 109.04(17) . . ? C20 C17 C16 109.75(19) . . ? O3 C17 C18 108.45(18) . . ? C20 C17 C18 112.73(19) . . ? C16 C17 C18 110.69(18) . . ? C19 C18 C17 116.4(2) . . ? C19 C18 H18A 108.2 . . ? C17 C18 H18A 108.2 . . ? C19 C18 H18B 108.2 . . ? C17 C18 H18B 108.2 . . ? H18A C18 H18B 107.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C17 114.7(2) . . ? C21 C20 H20A 108.6 . . ? C17 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C17 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 2.34 2.766(2) 112.6 . C2 H2B O1 0.97 2.55 3.267(4) 130.7 2_645 _refine_diff_density_max 0.181 _refine_diff_density_min -0.129 _refine_diff_density_rms 0.028 _shelx_res_file ; TITL yf160700_2_0m_a.res in P2(1) shelx.res created by SHELXL-2014/7 at 09:23:38 on 13-Jan-2017 CELL 1.54178 12.4156 6.3672 12.7186 90 90.509 90 ZERR 2 0.0019 0.0006 0.0012 0 0.005 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O UNIT 42 72 6 L.S. 10 ACTA 135 BOND $H FMAP 2 PLAN 20 REM CONF HTAB 2.4 EQIV $1 -x+1, y-1/2, -z HTAB O3 O2 HTAB C2 O1_$1 SIZE 0.053 0.107 0.111 TEMP 23 WGHT 0.054800 0.101500 FVAR 0.90913 O1 3 0.437759 0.572471 -0.022035 11.00000 0.08477 0.07390 = 0.05859 0.00589 0.00737 -0.00025 O2 3 0.142760 0.544305 0.560381 11.00000 0.07956 0.04990 = 0.05545 0.01047 0.01500 0.01089 O3 3 -0.043208 0.443337 0.667363 11.00000 0.05410 0.09988 = 0.06921 -0.00137 -0.00739 -0.00456 AFIX 83 H3 2 -0.037329 0.499824 0.609759 11.00000 -1.50000 AFIX 0 C1 1 0.468805 0.533467 0.066494 11.00000 0.06416 0.05079 = 0.06031 -0.00011 0.01062 0.00253 C2 1 0.584046 0.558682 0.101601 11.00000 0.05557 0.07256 = 0.08008 0.00264 0.01404 -0.00393 AFIX 23 H2A 2 0.622303 0.639485 0.049153 11.00000 -1.20000 H2B 2 0.617336 0.421055 0.105572 11.00000 -1.20000 AFIX 0 C3 1 0.596515 0.666679 0.207464 11.00000 0.05194 0.07790 = 0.09000 -0.00302 0.00303 -0.01382 AFIX 23 H3A 2 0.585471 0.816339 0.198045 11.00000 -1.20000 H3B 2 0.669676 0.646282 0.232839 11.00000 -1.20000 AFIX 0 C4 1 0.518401 0.586833 0.290875 11.00000 0.05330 0.06970 = 0.06528 -0.00181 -0.00458 -0.00712 AFIX 23 H4A 2 0.524731 0.673879 0.353214 11.00000 -1.20000 H4B 2 0.537839 0.444390 0.310317 11.00000 -1.20000 AFIX 0 C5 1 0.401446 0.590201 0.251392 11.00000 0.04783 0.04661 = 0.05342 0.00149 -0.00004 -0.00172 C6 1 0.396822 0.450999 0.151200 11.00000 0.05120 0.05149 = 0.05521 -0.00052 0.00258 -0.00118 AFIX 13 H6 2 0.425850 0.313616 0.171548 11.00000 -1.20000 AFIX 0 C7 1 0.277993 0.418256 0.128920 11.00000 0.05567 0.09107 = 0.05441 -0.00868 0.00089 -0.00844 AFIX 23 H7A 2 0.265592 0.285736 0.093193 11.00000 -1.20000 H7B 2 0.249125 0.531248 0.085976 11.00000 -1.20000 AFIX 0 C8 1 0.226551 0.417822 0.238786 11.00000 0.04911 0.07266 = 0.05800 -0.00132 0.00186 -0.00643 AFIX 23 H8A 2 0.197169 0.280269 0.254406 11.00000 -1.20000 H8B 2 0.168733 0.520049 0.241760 11.00000 -1.20000 AFIX 0 C9 1 0.316667 0.474863 0.319103 11.00000 0.04942 0.04369 = 0.05173 0.00193 0.00034 -0.00117 AFIX 13 H9 2 0.349488 0.342450 0.342114 11.00000 -1.20000 AFIX 0 C10 1 0.365484 0.816404 0.226778 11.00000 0.07584 0.05045 = 0.07244 0.00631 0.01033 0.00282 AFIX 137 H10A 2 0.290211 0.817215 0.208856 11.00000 -1.50000 H10B 2 0.406170 0.869680 0.168748 11.00000 -1.50000 H10C 2 0.377642 0.903397 0.287379 11.00000 -1.50000 AFIX 0 C11 1 0.272967 0.583333 0.418020 11.00000 0.06194 0.04576 = 0.05420 0.00155 0.00654 -0.00167 AFIX 13 H11 2 0.238881 0.714739 0.395309 11.00000 -1.20000 AFIX 0 C12 1 0.359091 0.639846 0.499097 11.00000 0.08725 0.08109 = 0.06164 -0.01391 0.00571 -0.02432 AFIX 137 H12A 2 0.405281 0.521033 0.510741 11.00000 -1.50000 H12B 2 0.325375 0.678380 0.563935 11.00000 -1.50000 H12C 2 0.400937 0.755768 0.473754 11.00000 -1.50000 AFIX 0 C13 1 0.184431 0.445558 0.466676 11.00000 0.05894 0.05389 = 0.05225 0.00256 0.00540 0.00145 AFIX 13 H13 2 0.125359 0.432857 0.415452 11.00000 -1.20000 AFIX 0 C14 1 0.218216 0.224705 0.500346 11.00000 0.06853 0.04743 = 0.06580 -0.00405 0.00615 -0.00259 AFIX 23 H14A 2 0.203921 0.123147 0.445114 11.00000 -1.20000 H14B 2 0.294050 0.219766 0.519194 11.00000 -1.20000 AFIX 0 C15 1 0.147498 0.185019 0.595701 11.00000 0.07395 0.04753 = 0.06280 0.00455 0.00459 -0.00646 AFIX 23 H15A 2 0.075223 0.143265 0.575017 11.00000 -1.20000 H15B 2 0.178342 0.078868 0.641642 11.00000 -1.20000 AFIX 0 C16 1 0.148415 0.400209 0.647176 11.00000 0.05500 0.04526 = 0.05547 0.00751 -0.00185 -0.00121 AFIX 13 H16 2 0.217498 0.419547 0.683774 11.00000 -1.20000 AFIX 0 C17 1 0.057449 0.454619 0.722716 11.00000 0.05071 0.05269 = 0.05325 0.00567 -0.00265 -0.00432 C18 1 0.071242 0.677759 0.765632 11.00000 0.06381 0.05217 = 0.06324 0.00641 0.00805 0.00236 AFIX 23 H18A 2 0.068961 0.774589 0.706776 11.00000 -1.20000 H18B 2 0.010032 0.709199 0.809810 11.00000 -1.20000 AFIX 0 C19 1 0.172554 0.720014 0.828140 11.00000 0.08131 0.07055 = 0.09258 -0.02266 -0.00221 -0.00971 AFIX 137 H19A 2 0.233638 0.713164 0.782515 11.00000 -1.50000 H19B 2 0.180028 0.616557 0.882624 11.00000 -1.50000 H19C 2 0.168567 0.857252 0.859118 11.00000 -1.50000 AFIX 0 C20 1 0.051745 0.289416 0.809670 11.00000 0.08238 0.05644 = 0.06462 0.01052 0.00570 -0.01200 AFIX 23 H20A 2 0.035989 0.154305 0.777833 11.00000 -1.20000 H20B 2 0.121946 0.279147 0.843359 11.00000 -1.20000 AFIX 0 C21 1 -0.031958 0.333190 0.893629 11.00000 0.11590 0.09075 = 0.07117 0.00758 0.02563 -0.02642 AFIX 137 H21A 2 -0.099201 0.369654 0.860556 11.00000 -1.50000 H21B 2 -0.007992 0.447459 0.937167 11.00000 -1.50000 H21C 2 -0.041463 0.210061 0.936108 11.00000 -1.50000 AFIX 0 HKLF 4 REM yf160700_2_0m_a.res in P2(1) REM R1 = 0.0370 for 3636 Fo > 4sig(Fo) and 0.0384 for all 3777 data REM 221 parameters refined using 1 restraints END WGHT 0.0548 0.1015 REM Instructions for potential hydrogen bonds HTAB O3 O2 HTAB C2 O1_$1 HTAB C2 O1_$2 HTAB C6 O1_$2 HTAB C11 O3_$3 HTAB C14 O3_$4 REM Highest difference peak 0.181, deepest hole -0.129, 1-sigma level 0.028 Q1 1 0.4565 0.5707 0.2727 11.00000 0.05 0.18 Q2 1 0.4022 0.5247 0.2020 11.00000 0.05 0.14 Q3 1 0.2681 0.4543 0.2814 11.00000 0.05 0.14 Q4 1 0.3614 0.5441 0.2951 11.00000 0.05 0.12 Q5 1 0.1956 0.5471 0.6018 11.00000 0.05 0.12 Q6 1 0.3814 0.6917 0.2416 11.00000 0.05 0.12 Q7 1 0.3605 0.5601 -0.0467 11.00000 0.05 0.12 Q8 1 0.5787 0.5837 0.1543 11.00000 0.05 0.12 Q9 1 0.5317 0.5662 0.0808 11.00000 0.05 0.12 Q10 1 0.2234 0.6067 0.8455 11.00000 0.05 0.11 Q11 1 0.1915 0.3197 0.4674 11.00000 0.05 0.11 Q12 1 0.3417 0.3989 0.1412 11.00000 0.05 0.11 Q13 1 0.3375 0.4851 0.1306 11.00000 0.05 0.11 Q14 1 0.2327 0.5117 0.4449 11.00000 0.05 0.11 Q15 1 0.4358 0.6399 0.0258 11.00000 0.05 0.11 Q16 1 0.0674 0.5557 0.7466 11.00000 0.05 0.11 Q17 1 0.3225 0.5800 0.4559 11.00000 0.05 0.10 Q18 1 0.1205 0.6544 0.7990 11.00000 0.05 0.10 Q19 1 0.0579 0.3847 0.7665 11.00000 0.05 0.10 Q20 1 0.0050 0.3697 0.7061 11.00000 0.05 0.10 ; _shelx_res_checksum 78075 _shelx_hkl_file ; 1 0 0 1.10 0.10 1 0 0 1.40 0.20 -2 0 0 195.08 7.20 2 0 0 202.58 7.30 2 0 0 196.68 7.20 -3 0 0 23.20 1.20 3 0 0 23.90 1.30 3 0 0 22.90 1.00 -4 0 0 200.08 7.80 4 0 0 223.08 8.20 4 0 0 217.68 7.80 5 0 0 798.72 28.30 -5 0 0 685.13 27.30 5 0 0 813.52 28.20 6 0 0 65.99 2.80 6 0 0 65.99 3.40 7 0 0 18.40 1.70 7 0 0 18.50 1.20 -8 0 0 41.60 1.70 8 0 0 44.60 2.90 8 0 0 42.00 1.60 8 0 0 46.90 2.30 -8 0 0 42.90 1.70 -8 0 0 38.90 1.50 9 0 0 228.78 8.60 9 0 0 252.17 9.50 9 0 0 248.38 8.60 -9 0 0 248.58 8.80 -9 0 0 246.28 8.70 -9 0 0 245.78 8.60 -9 0 0 227.48 8.60 -10 0 0 24.30 1.20 -10 0 0 27.60 1.20 10 0 0 24.10 1.80 10 0 0 25.30 1.00 -11 0 0 76.89 2.90 -11 0 0 76.59 3.00 11 0 0 75.19 2.70 11 0 0 67.39 3.70 -12 0 0 3.70 0.50 -12 0 0 2.90 0.50 12 0 0 3.00 0.30 -13 0 0 0.70 0.30 -13 0 0 0.60 0.30 13 0 0 0.40 0.10 14 0 0 0.00 0.10 -14 0 0 0.00 0.20 15 0 0 6.80 0.30 15 0 0 6.70 0.50 0 -1 0 0.00 0.20 0 -1 0 0.00 0.10 0 -1 0 0.00 0.20 0 1 0 0.00 0.10 0 1 0 0.10 0.20 0 1 0 0.00 0.20 1 -1 0 4723.93 203.38 -1 -1 0 4645.94 212.48 1 -1 0 4118.09 186.88 -1 -1 0 4852.61 227.98 1 1 0 4795.42 244.48 -1 1 0 4649.94 197.08 -1 1 0 4551.54 190.38 1 1 0 4466.65 181.98 -2 -1 0 190.88 7.20 -2 -1 0 191.48 7.40 2 -1 0 197.08 7.10 2 1 0 197.78 7.00 2 1 0 170.68 6.50 -2 1 0 177.48 6.60 2 1 0 186.68 6.50 -2 1 0 178.58 6.60 3 -1 0 237.48 8.60 3 -1 0 237.58 8.70 -3 -1 0 233.38 8.80 3 1 0 244.08 9.00 3 1 0 243.08 8.40 3 1 0 213.88 8.30 4 -1 0 368.56 13.60 -4 -1 0 367.36 13.60 4 -1 0 370.46 13.40 4 1 0 369.46 13.80 4 1 0 382.26 13.30 4 1 0 348.77 13.10 5 -1 0 20.00 1.20 -5 -1 0 20.30 1.40 5 -1 0 20.80 1.40 5 1 0 20.80 1.60 5 1 0 21.00 1.10 6 -1 0 197.88 7.50 6 -1 0 188.58 7.80 6 1 0 189.68 7.10 6 1 0 185.58 7.90 7 -1 0 11.60 1.10 7 -1 0 10.90 1.20 -7 -1 0 10.30 0.40 7 1 0 12.70 1.00 7 1 0 11.00 1.40 -8 -1 0 6.20 0.30 -8 -1 0 6.10 0.40 8 -1 0 5.50 1.10 -8 -1 0 6.00 0.50 8 -1 0 6.80 0.90 -8 -1 0 6.00 0.30 8 -1 0 6.30 0.30 8 1 0 6.20 1.30 -8 1 0 6.00 0.40 8 1 0 6.20 0.80 8 1 0 5.70 0.30 8 1 0 6.10 0.30 -8 1 0 6.00 0.50 -9 -1 0 12.40 0.50 -9 -1 0 10.70 0.70 -9 -1 0 12.30 0.70 9 -1 0 12.00 0.50 -9 -1 0 11.40 0.50 9 -1 0 11.20 1.30 -9 1 0 11.00 0.60 9 1 0 12.50 1.10 9 1 0 11.80 0.50 -9 1 0 11.40 0.70 9 1 0 11.70 0.50 -10 -1 0 26.20 1.30 10 -1 0 27.70 1.10 10 -1 0 27.60 2.00 -10 -1 0 26.40 1.00 -10 -1 0 26.90 1.20 -10 1 0 28.80 1.30 -10 1 0 27.00 1.20 10 1 0 27.50 1.10 10 1 0 25.40 1.10 10 1 0 26.50 1.80 11 -1 0 8.70 0.50 -11 -1 0 8.60 0.40 -11 -1 0 8.70 0.50 11 -1 0 8.50 1.60 -11 -1 0 9.10 0.60 -11 -1 0 8.40 0.70 11 1 0 8.90 0.50 -11 1 0 9.20 0.60 11 1 0 8.20 1.30 -11 1 0 9.10 0.70 -12 -1 0 27.30 1.10 -12 -1 0 27.90 1.30 -12 -1 0 28.90 1.10 -12 -1 0 29.70 1.30 12 -1 0 27.20 1.10 -12 1 0 29.90 1.30 -12 1 0 27.50 1.40 12 1 0 27.80 1.10 13 -1 0 2.70 0.30 -13 -1 0 2.40 0.40 -13 -1 0 2.70 0.30 -13 -1 0 3.00 0.40 -13 1 0 3.00 0.40 13 1 0 2.60 0.30 -13 1 0 2.70 0.40 -14 -1 0 1.90 0.30 14 -1 0 1.40 0.20 -14 1 0 1.60 0.20 14 1 0 1.60 0.20 -14 1 0 1.70 0.40 -14 1 0 1.80 0.30 14 1 0 1.60 0.30 15 -1 0 2.30 0.20 15 -1 0 2.50 0.30 0 -2 0 1183.78 44.00 0 2 0 1234.18 43.20 0 2 0 1125.29 42.60 1 -2 0 1709.13 90.89 1 -2 0 1568.34 59.39 1 -2 0 1702.03 80.79 -1 -2 0 1665.33 59.89 1 2 0 1642.14 61.09 1 2 0 1734.03 60.29 -1 2 0 1641.94 60.19 2 -2 0 151.58 6.20 2 -2 0 154.78 6.30 -2 -2 0 188.38 7.70 -2 -2 0 166.08 6.60 2 -2 0 155.78 6.40 2 2 0 158.78 5.80 -2 2 0 157.28 5.90 3 -2 0 352.56 13.50 -3 -2 0 372.46 13.90 3 -2 0 382.76 13.70 3 2 0 356.26 12.60 -3 2 0 332.47 12.70 3 2 0 366.26 13.50 -4 -2 0 69.19 3.50 4 -2 0 75.79 3.40 4 -2 0 73.09 3.20 4 2 0 76.49 3.00 4 2 0 76.09 3.90 5 -2 0 16.00 1.40 5 -2 0 15.90 1.20 5 2 0 16.70 1.70 5 2 0 17.90 1.00 6 -2 0 23.00 1.50 6 -2 0 21.90 1.70 -6 -2 0 20.90 0.80 6 2 0 23.30 1.30 6 2 0 22.80 2.10 -7 -2 0 102.99 3.70 7 -2 0 106.09 3.80 7 -2 0 102.39 5.00 -7 -2 0 107.79 3.70 -7 -2 0 98.49 3.90 7 -2 0 111.49 4.80 7 2 0 99.79 3.70 7 2 0 99.29 5.50 7 2 0 102.59 3.70 7 2 0 111.09 4.20 -7 2 0 102.39 3.80 8 -2 0 10.60 1.20 -8 -2 0 8.50 0.60 -8 -2 0 9.00 0.60 -8 -2 0 9.40 0.40 -8 -2 0 9.40 0.40 8 -2 0 9.90 0.50 -8 2 0 7.70 0.50 -8 2 0 9.80 0.60 8 2 0 9.80 0.90 8 2 0 9.40 0.40 8 2 0 9.00 0.40 -9 -2 0 8.30 0.60 9 -2 0 8.70 0.50 -9 -2 0 8.30 0.60 9 -2 0 9.00 1.30 -9 -2 0 8.80 0.40 -9 2 0 8.40 0.60 9 2 0 9.20 0.90 9 2 0 8.90 0.50 9 2 0 8.40 0.40 -10 -2 0 8.90 0.40 10 -2 0 8.70 0.50 10 -2 0 8.40 1.40 -10 -2 0 8.80 0.60 -10 -2 0 9.00 0.70 10 2 0 7.00 0.90 -10 2 0 8.60 0.60 10 2 0 8.30 0.40 -10 2 0 6.40 0.50 11 -2 0 13.40 0.60 -11 -2 0 13.30 0.80 -11 -2 0 12.70 0.80 -11 -2 0 13.50 0.60 -11 -2 0 13.00 0.50 -11 2 0 11.60 0.70 -11 2 0 12.30 0.80 11 2 0 12.80 0.60 -12 -2 0 15.20 0.80 -12 -2 0 14.50 0.60 -12 -2 0 14.70 0.70 12 -2 0 14.80 0.70 -12 2 0 12.70 0.70 -12 2 0 14.60 0.90 12 2 0 13.80 0.60 -13 -2 0 0.10 0.10 -13 -2 0 0.10 0.10 13 -2 0 0.20 0.20 -13 -2 0 0.10 0.20 13 2 0 0.00 0.10 -13 2 0 0.00 0.10 -13 2 0 0.00 0.30 14 -2 0 5.30 0.30 -14 -2 0 5.00 0.30 -14 -2 0 6.00 0.40 -14 2 0 5.20 0.20 14 2 0 5.10 0.30 0 -3 0 -0.10 0.50 0 3 0 0.00 0.20 1 -3 0 274.47 11.00 -1 -3 0 290.57 11.20 1 3 0 263.47 11.10 -1 3 0 285.07 10.30 1 3 0 285.17 10.20 -2 -3 0 41.50 2.60 2 -3 0 41.50 2.50 2 3 0 43.10 1.90 2 3 0 42.40 2.70 -3 -3 0 97.79 4.80 3 -3 0 97.19 4.60 3 3 0 100.79 4.10 -3 3 0 94.29 4.60 3 3 0 121.49 5.80 4 -3 0 65.29 3.40 -4 -3 0 61.39 2.30 4 -3 0 62.99 3.10 4 3 0 64.19 3.80 4 3 0 67.09 2.80 -5 -3 0 72.49 2.60 5 -3 0 75.09 3.60 5 -3 0 75.39 2.70 5 -3 0 71.09 3.80 5 -3 0 71.89 2.60 -5 -3 0 69.89 2.60 5 3 0 69.29 4.30 5 3 0 76.29 3.10 6 -3 0 16.80 1.70 -6 -3 0 19.30 0.70 6 -3 0 18.10 0.80 6 -3 0 18.80 0.70 -6 -3 0 17.10 0.90 6 -3 0 18.00 1.60 6 3 0 17.20 0.70 6 3 0 17.90 0.70 6 3 0 18.40 1.10 7 -3 0 0.80 0.20 -7 -3 0 0.70 0.10 -7 -3 0 0.90 0.30 7 -3 0 0.60 0.10 -7 3 0 0.50 0.20 7 3 0 0.70 0.30 7 3 0 0.50 0.10 7 3 0 0.50 0.10 -8 -3 0 6.60 0.50 8 -3 0 6.10 0.30 -8 -3 0 6.50 0.30 8 -3 0 6.40 0.40 8 3 0 6.20 0.80 -8 3 0 5.30 0.50 8 3 0 5.80 0.30 9 -3 0 11.20 0.50 -9 -3 0 12.00 0.50 9 -3 0 12.60 0.60 -9 -3 0 11.90 0.70 -9 3 0 10.90 0.50 9 3 0 12.10 0.50 9 3 0 10.80 1.00 -9 3 0 10.40 0.70 -10 -3 0 7.40 0.40 -10 -3 0 7.60 0.60 10 -3 0 7.40 0.50 -10 3 0 6.60 0.30 10 3 0 6.50 0.40 -10 3 0 6.20 0.60 -11 -3 0 9.30 0.50 -11 -3 0 10.00 0.40 11 -3 0 9.70 0.50 -11 -3 0 9.70 0.60 -11 3 0 8.80 0.70 11 3 0 9.30 0.40 -11 3 0 9.10 0.40 -12 -3 0 10.30 0.70 -12 -3 0 11.20 0.50 12 -3 0 10.70 0.50 -12 -3 0 10.50 0.50 -12 3 0 10.10 0.70 -12 3 0 10.20 0.40 12 3 0 10.30 0.50 -13 -3 0 5.40 0.30 13 -3 0 5.10 0.30 -13 -3 0 5.80 0.50 -13 -3 0 5.00 0.30 13 3 0 4.90 0.30 -13 3 0 5.40 0.20 14 -3 0 -0.10 0.10 0 -4 0 21.80 0.80 0 -4 0 21.00 2.00 0 4 0 23.80 1.40 0 4 0 22.20 0.90 0 4 0 23.30 0.80 1 -4 0 300.37 11.00 -1 -4 0 355.96 13.50 1 -4 0 342.87 11.00 -1 -4 0 300.57 11.00 1 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1 -4 -13 1.70 0.20 0 -4 13 2.70 0.20 0 -4 13 3.00 0.20 0 -4 -13 2.70 0.20 -1 -4 -13 1.70 0.20 1 -4 13 1.80 0.20 2 -4 13 1.20 0.10 6 0 -14 10.40 0.40 -6 0 14 10.60 0.40 -5 0 14 12.70 0.50 -5 0 14 12.20 0.60 -5 0 14 11.80 0.50 5 0 -14 12.40 0.50 -4 0 14 0.00 0.10 -4 0 14 -0.10 0.10 4 0 -14 0.00 0.10 -4 0 14 0.00 0.10 -4 0 14 0.10 0.20 -3 0 14 1.30 0.20 -3 0 14 1.80 0.30 3 0 -14 1.40 0.20 -3 0 14 1.60 0.20 -3 0 14 1.50 0.10 -2 0 14 0.00 0.10 -2 0 14 0.10 0.10 -2 0 14 0.00 0.20 2 0 -14 0.00 0.10 -2 0 14 0.00 0.10 -1 0 14 5.00 0.30 -1 0 14 4.70 0.40 -1 0 14 5.70 0.30 -1 0 14 5.10 0.20 1 0 -14 4.90 0.30 0 0 14 0.50 0.10 0 0 14 0.80 0.20 0 0 14 0.60 0.10 0 0 14 0.20 0.20 0 0 -14 0.60 0.10 1 0 14 0.40 0.20 1 0 14 0.30 0.10 1 0 14 0.20 0.10 -1 0 -14 0.30 0.10 1 0 14 0.30 0.20 -2 0 -14 0.00 0.10 2 0 14 0.10 0.30 3 0 14 0.70 0.30 -3 0 -14 0.80 0.10 -4 0 -14 0.00 0.10 4 0 14 -0.10 0.20 5 0 14 0.10 0.20 6 0 14 4.10 0.40 -6 -1 14 2.80 0.20 6 -1 -14 2.80 0.20 -6 1 14 2.70 0.40 6 1 -14 2.80 0.20 -6 1 14 2.90 0.20 5 -1 -14 2.60 0.20 -5 -1 14 2.40 0.20 -5 -1 14 2.30 0.20 -5 -1 14 2.60 0.20 -5 1 14 3.00 0.20 -5 1 14 2.80 0.40 -5 1 14 2.60 0.20 5 1 -14 2.50 0.20 4 -1 -14 0.30 0.10 -4 -1 14 0.30 0.10 4 -1 -14 0.00 0.10 -4 -1 14 0.30 0.10 -4 -1 14 0.40 0.10 -4 1 14 0.40 0.10 4 1 -14 0.50 0.10 -4 1 14 0.10 0.20 -4 1 14 0.40 0.10 -3 -1 14 1.80 0.20 -3 -1 14 2.30 0.20 -3 -1 14 2.20 0.20 3 -1 -14 2.10 0.20 -3 1 14 2.20 0.20 3 1 -14 2.00 0.20 -3 1 14 2.90 0.30 -3 1 14 2.00 0.10 -2 -1 14 0.10 0.10 2 -1 -14 0.10 0.10 -2 -1 14 0.30 0.10 -2 -1 14 0.10 0.20 -2 -1 14 0.10 0.10 2 1 -14 0.20 0.10 -2 1 14 0.20 0.10 -2 1 14 0.10 0.10 -2 1 14 0.40 0.20 -1 -1 14 2.60 0.20 -1 -1 14 2.40 0.40 1 -1 -14 2.90 0.20 -1 -1 14 2.70 0.20 -1 -1 14 2.60 0.20 -1 1 14 2.30 0.30 1 1 -14 2.30 0.20 -1 1 14 2.60 0.20 -1 1 14 2.60 0.20 0 -1 14 9.80 0.40 0 -1 14 10.30 0.40 0 -1 -14 10.70 0.50 0 -1 14 9.30 0.60 0 -1 14 10.20 0.50 0 1 14 10.40 0.40 0 1 14 10.60 0.40 0 1 14 10.70 0.60 0 1 -14 10.60 0.50 1 -1 14 4.50 0.20 -1 -1 -14 4.60 0.30 1 -1 14 4.60 0.30 1 1 14 4.00 0.50 -1 1 -14 4.30 0.20 1 1 14 4.20 0.20 2 -1 14 7.00 0.40 -2 -1 -14 7.00 0.30 -2 -1 -14 6.00 0.40 2 -1 14 6.70 0.30 2 1 14 6.40 0.50 2 1 14 6.40 0.30 -3 -1 -14 6.80 0.30 3 1 14 5.30 0.50 -4 -1 -14 2.80 0.20 4 1 14 1.90 0.30 -5 -1 -14 3.40 0.20 5 1 14 3.80 0.40 6 1 14 0.30 0.20 -5 -2 14 4.60 0.20 5 -2 -14 4.60 0.40 -5 -2 14 3.90 0.30 -5 2 14 4.70 0.20 -5 2 14 4.20 0.40 4 -2 -14 7.80 0.40 -4 -2 14 8.10 0.30 -4 -2 14 7.90 0.40 -4 2 14 8.10 0.30 4 2 -14 7.40 0.30 -4 2 14 7.30 0.50 -3 -2 14 4.60 0.20 3 -2 -14 4.30 0.20 -3 -2 14 4.00 0.30 3 -2 -14 4.10 0.30 -3 2 14 4.00 0.20 -3 2 14 4.80 0.20 3 2 -14 4.10 0.20 -3 2 14 3.90 0.40 -2 -2 14 3.80 0.30 2 -2 -14 3.20 0.30 -2 -2 14 3.80 0.20 2 -2 -14 3.60 0.20 -2 2 14 3.60 0.20 -2 2 14 3.90 0.20 -2 2 14 2.80 0.40 2 2 -14 3.70 0.30 1 -2 -14 2.10 0.20 -1 -2 14 1.90 0.20 -1 -2 14 1.50 0.20 1 -2 -14 1.90 0.20 -1 2 14 1.80 0.10 -1 2 14 1.70 0.30 0 -2 14 1.40 0.10 0 -2 14 1.60 0.20 0 -2 -14 1.10 0.20 0 -2 -14 1.10 0.10 0 2 14 1.90 0.30 0 2 14 1.40 0.10 1 -2 14 7.40 0.40 -1 -2 -14 7.30 0.40 1 -2 14 7.50 0.30 -1 -2 -14 7.20 0.40 1 2 14 7.30 0.30 -2 -2 -14 4.00 0.20 2 -2 14 3.90 0.20 -2 -2 -14 4.10 0.30 2 2 14 4.00 0.40 -3 -2 -14 2.40 0.20 3 2 14 1.60 0.30 -4 -2 -14 1.30 0.10 4 2 14 0.80 0.20 -5 -2 -14 0.40 0.10 5 2 14 0.20 0.20 3 -3 -14 9.00 0.40 -3 -3 14 10.40 0.40 -3 -3 14 9.20 0.40 -2 -3 14 0.30 0.10 -2 -3 14 0.40 0.10 2 -3 -14 0.30 0.10 -2 3 14 0.20 0.20 1 -3 -14 0.90 0.10 1 -3 -14 0.80 0.10 -1 -3 14 1.10 0.10 -1 -3 14 1.00 0.10 -1 3 14 0.80 0.20 0 -3 -14 5.80 0.30 0 -3 14 6.20 0.30 0 -3 -14 5.60 0.30 0 -3 14 5.40 0.30 0 3 14 5.20 0.30 -1 -3 -14 1.30 0.10 1 -3 14 1.30 0.10 -1 -3 -14 1.20 0.10 1 3 14 1.10 0.20 -2 -3 -14 0.20 0.10 -3 -3 -14 10.00 0.50 -4 0 15 2.50 0.20 4 0 -15 2.50 0.20 -3 0 15 0.40 0.10 3 0 -15 0.50 0.10 -2 0 15 0.40 0.20 2 0 -15 0.40 0.10 -2 0 15 0.40 0.10 -1 0 15 0.20 0.20 1 0 -15 0.10 0.10 -1 0 15 0.10 0.10 0 0 15 0.80 0.10 0 0 15 0.80 0.20 0 0 -15 1.00 0.10 -1 0 -15 4.00 0.20 1 0 15 3.60 0.40 2 0 15 0.00 0.20 -2 0 -15 0.10 0.10 -3 -1 15 0.80 0.10 -3 -1 15 0.50 0.10 3 -1 -15 0.50 0.10 3 -1 -15 0.70 0.10 -3 1 15 0.60 0.20 2 -1 -15 2.10 0.20 -2 -1 15 2.20 0.20 -2 -1 15 2.30 0.20 -2 1 15 2.20 0.20 2 1 -15 2.10 0.20 -2 1 15 2.10 0.30 -1 -1 15 2.20 0.20 1 -1 -15 2.10 0.20 -1 -1 15 2.10 0.20 1 1 -15 2.00 0.20 -1 1 15 2.00 0.20 0 -1 -15 2.00 0.20 0 -1 -15 1.50 0.20 0 -1 15 2.00 0.10 0 -1 15 1.70 0.20 0 1 15 2.00 0.20 -1 -1 -15 0.80 0.10 -1 -1 -15 0.80 0.10 1 1 15 1.20 0.20 -2 -1 -15 3.20 0.20 1 -2 -15 0.30 0.10 -1 2 15 0.30 0.20 0 -2 -15 4.20 0.20 0 2 15 3.90 0.30 -1 -2 -15 2.60 0.20 1 2 15 1.80 0.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41183 _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{a2d2c8c0-4cca-42b6-83f2-4f8768fac38e}' y y y '{ff081758-1756-41b6-a40e-e3dd0988ebf5}' ? ? ? loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{ff081758-1756-41b6-a40e-e3dd0988ebf5}" "_publcif_info_datablock.publ_exptl" "{a2d2c8c0-4cca-42b6-83f2-4f8768fac38e}" "_geom_hbond_atom_site_label_D" loop_ _publcif_info_cif.paper_type EE