# 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_cu_d060412_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 O3' _chemical_formula_sum 'C28 H30 O3' _chemical_formula_weight 414.52 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_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 6.3443(8) _cell_length_b 18.518(2) _cell_length_c 19.686(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2312.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3137 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 49.96 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0862 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.8757. The \l/2 correction factor is 0.0000. ; _exptl_absorpt_correction_T_min 0.9106 _exptl_absorpt_correction_T_max 0.9941 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12081 _diffrn_reflns_av_R_equivalents 0.1423 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 50.45 _reflns_number_total 2411 _reflns_number_gt 2129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The phenol group not involved in H-bonding is disordered and has been refined isotropically over two positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.0000P] 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 H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(4) _refine_ls_number_reflns 2411 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4526(3) -0.18861(12) -0.06134(11) 0.0297(6) Uani 1 1 d . . . H1 H 0.5384 -0.2332 -0.0596 0.045 Uiso 1 1 calc R . . O2 O 1.2640(9) 0.2083(2) 0.2911(3) 0.0413(17) Uani 0.616(8) 1 d P A 1 H2 H 1.3921 0.2141 0.2819 0.062 Uiso 0.616(8) 1 calc PR A 1 O2A O 1.4152(14) 0.2235(5) 0.2534(4) 0.046(3) Uani 0.384(8) 1 d P A 2 H2A H 1.4077 0.2768 0.2513 0.069 Uiso 0.384(8) 1 calc PR A 2 O3 O 1.1699(3) -0.19148(11) 0.04421(11) 0.0288(6) Uani 1 1 d . . . H3 H 1.2617 -0.1841 0.0041 0.043 Uiso 1 1 calc R . . C1 C 1.3136(7) 0.1871(2) -0.1508(2) 0.0370(10) Uani 1 1 d . . . C2 C 1.2039(6) 0.1385(2) -0.13363(18) 0.0287(9) Uani 1 1 d . . . C3 C 1.0610(6) 0.08266(18) -0.11415(19) 0.0277(9) Uani 1 1 d . . . C4 C 1.0358(5) 0.06737(16) -0.04968(19) 0.0261(9) Uani 1 1 d . . . C5 C 0.9960(5) 0.05262(17) 0.01475(19) 0.0231(9) Uani 1 1 d . A . C6 C 1.0902(5) -0.0102(2) 0.04515(18) 0.0266(9) Uani 1 1 d . . . C7 C 1.1507(5) -0.0660(2) 0.06916(18) 0.0263(9) Uani 1 1 d . . . C8 C 1.2172(5) -0.13742(18) 0.09496(18) 0.0271(9) Uani 1 1 d . . . C9 C 1.0854(6) -0.15803(18) 0.15712(18) 0.0326(9) Uani 1 1 d . . . H9A H 0.9201 -0.1623 0.1426 0.049 Uiso 1 1 calc R . . H9B H 1.1026 -0.1167 0.1961 0.049 Uiso 1 1 calc R . . H9C H 1.1395 -0.2098 0.1770 0.049 Uiso 1 1 calc R . . C10 C 1.4533(5) -0.13785(19) 0.11129(18) 0.0300(9) Uani 1 1 d . . . H10A H 1.4985 -0.1910 0.1302 0.045 Uiso 1 1 calc R . . H10B H 1.4868 -0.0973 0.1499 0.045 Uiso 1 1 calc R . . H10C H 1.5426 -0.1256 0.0654 0.045 Uiso 1 1 calc R . . C11 C 0.9375(5) 0.04326(17) -0.17121(17) 0.0267(9) Uani 1 1 d . . . C12 C 0.7961(6) 0.0981(2) -0.20761(19) 0.0365(10) Uani 1 1 d . . . H12A H 0.7017 0.0704 -0.2458 0.055 Uiso 1 1 calc R . . H12B H 0.8938 0.1389 -0.2321 0.055 Uiso 1 1 calc R . . H12C H 0.6923 0.1239 -0.1708 0.055 Uiso 1 1 calc R . . C13 C 1.0997(5) 0.01456(19) -0.22262(17) 0.0311(9) Uani 1 1 d . . . H13A H 1.2071 -0.0226 -0.1971 0.047 Uiso 1 1 calc R . . H13B H 1.1889 0.0596 -0.2437 0.047 Uiso 1 1 calc R . . H13C H 1.0181 -0.0137 -0.2634 0.047 Uiso 1 1 calc R . . C14 C 0.8104(5) -0.01799(18) -0.14016(17) 0.0246(9) Uani 1 1 d . . . C15 C 0.6063(5) -0.00835(18) -0.11700(17) 0.0282(9) Uani 1 1 d . . . H15 H 0.5354 0.0446 -0.1204 0.034 Uiso 1 1 calc R . . C16 C 0.4896(5) -0.06502(19) -0.08936(19) 0.0299(9) Uani 1 1 d . . . H16 H 0.3303 -0.0557 -0.0722 0.036 Uiso 1 1 calc R . . C17 C 0.5758(5) -0.13201(18) -0.08401(17) 0.0231(8) Uani 1 1 d . . . C18 C 0.7824(6) -0.1429(2) -0.1034(2) 0.0509(13) Uani 1 1 d . . . H18 H 0.8561 -0.1950 -0.0969 0.061 Uiso 1 1 calc R . . C19 C 0.8942(6) -0.0854(2) -0.1313(2) 0.0526(12) Uani 1 1 d . . . H19 H 1.0554 -0.0946 -0.1468 0.063 Uiso 1 1 calc R . . C20 C 0.8452(5) 0.09796(17) 0.05782(17) 0.0268(9) Uani 1 1 d . . . C21 C 0.6637(6) 0.0484(2) 0.0800(2) 0.0474(11) Uani 1 1 d . A . H21A H 0.5845 0.0270 0.0352 0.071 Uiso 1 1 calc R . . H21B H 0.5516 0.0791 0.1104 0.071 Uiso 1 1 calc R . . H21C H 0.7263 0.0039 0.1101 0.071 Uiso 1 1 calc R . . C22 C 0.7547(6) 0.16070(19) 0.0167(2) 0.0337(9) Uani 1 1 d . A . H22A H 0.8832 0.1936 -0.0030 0.050 Uiso 1 1 calc R . . H22B H 0.6545 0.1937 0.0493 0.050 Uiso 1 1 calc R . . H22C H 0.6617 0.1396 -0.0254 0.050 Uiso 1 1 calc R . . C23 C 0.9540(16) 0.1248(5) 0.1191(5) 0.023(4) Uiso 0.616(8) 1 d P A 1 C23A C 0.994(3) 0.1325(9) 0.1159(9) 0.025(7) Uiso 0.384(8) 1 d P A 2 C24 C 0.8630(13) 0.1210(3) 0.1835(3) 0.0320(19) Uiso 0.616(8) 1 d P A 1 H24 H 0.7103 0.0959 0.1889 0.038 Uiso 0.616(8) 1 calc PR A 1 C24A C 0.966(2) 0.1213(5) 0.1841(5) 0.027(3) Uiso 0.384(8) 1 d P A 2 H24A H 0.8369 0.0875 0.2004 0.033 Uiso 0.384(8) 1 calc PR A 2 C25 C 0.9621(13) 0.1484(3) 0.2412(3) 0.037(2) Uiso 0.616(8) 1 d P A 1 H25 H 0.8868 0.1452 0.2903 0.044 Uiso 0.616(8) 1 calc PR A 1 C25A C 1.095(2) 0.1511(7) 0.2329(5) 0.031(3) Uiso 0.384(8) 1 d P A 2 H25A H 1.0672 0.1429 0.2865 0.037 Uiso 0.384(8) 1 calc PR A 2 C26 C 1.1598(13) 0.1801(4) 0.2343(3) 0.0213(19) Uiso 0.616(8) 1 d P A 1 C26A C 1.2699(18) 0.1939(5) 0.2083(7) 0.025(3) Uiso 0.384(8) 1 d P A 2 C27 C 1.2561(11) 0.1863(4) 0.1721(5) 0.0324(19) Uiso 0.616(8) 1 d P A 1 H27 H 1.4095 0.2110 0.1673 0.039 Uiso 0.616(8) 1 calc PR A 1 C27A C 1.3010(15) 0.2054(5) 0.1388(6) 0.025(3) Uiso 0.384(8) 1 d P A 2 H27A H 1.4297 0.2389 0.1215 0.031 Uiso 0.384(8) 1 calc PR A 2 C28 C 1.1500(14) 0.1596(4) 0.1150(4) 0.031(2) Uiso 0.616(8) 1 d P A 1 H28 H 1.2221 0.1661 0.0656 0.038 Uiso 0.616(8) 1 calc PR A 1 C28A C 1.1669(17) 0.1738(5) 0.0925(7) 0.023(3) Uiso 0.384(8) 1 d P A 2 H28A H 1.1936 0.1805 0.0387 0.028 Uiso 0.384(8) 1 calc PR A 2 H1A H 1.396(6) 0.227(2) -0.163(2) 0.057(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0275(13) 0.0294(13) 0.0321(14) 0.0016(11) 0.0030(13) 0.0018(11) O2 0.040(3) 0.049(3) 0.035(3) -0.009(2) -0.017(3) 0.005(2) O2A 0.050(6) 0.052(5) 0.035(5) -0.009(4) -0.030(5) 0.011(4) O3 0.0290(14) 0.0301(14) 0.0272(14) -0.0046(11) 0.0022(12) -0.0050(11) C1 0.033(2) 0.035(2) 0.043(3) -0.001(2) 0.000(2) -0.001(2) C2 0.029(2) 0.029(2) 0.028(2) 0.0018(18) 0.001(2) 0.000(2) C3 0.025(2) 0.028(2) 0.030(2) 0.0028(17) 0.005(2) 0.0045(18) C4 0.019(2) 0.023(2) 0.036(3) -0.0025(18) 0.000(2) 0.0028(15) C5 0.019(2) 0.027(2) 0.023(2) -0.0042(17) 0.0010(18) -0.0018(17) C6 0.025(2) 0.029(2) 0.027(2) -0.0054(19) 0.0096(18) -0.002(2) C7 0.020(2) 0.031(2) 0.027(2) -0.0043(19) 0.0063(18) -0.0017(18) C8 0.028(2) 0.027(2) 0.027(2) -0.0020(17) -0.0019(18) -0.0022(17) C9 0.034(2) 0.035(2) 0.028(2) -0.0014(17) 0.003(2) -0.0048(17) C10 0.023(2) 0.036(2) 0.031(2) 0.0020(17) -0.0041(18) 0.0002(17) C11 0.0254(19) 0.030(2) 0.024(2) 0.0039(17) -0.0005(19) 0.0012(17) C12 0.028(2) 0.046(2) 0.035(2) 0.0100(19) 0.004(2) 0.0013(19) C13 0.028(2) 0.044(2) 0.022(2) -0.0049(17) 0.0058(18) -0.0038(18) C14 0.026(2) 0.027(2) 0.020(2) 0.0004(16) -0.0003(18) -0.0001(18) C15 0.025(2) 0.033(2) 0.026(2) 0.0011(17) -0.0011(19) 0.0066(19) C16 0.026(2) 0.031(2) 0.032(2) 0.0002(18) 0.0044(19) -0.0005(19) C17 0.026(2) 0.024(2) 0.0195(18) 0.0006(16) -0.0043(19) -0.0085(19) C18 0.032(2) 0.036(3) 0.085(4) 0.009(2) 0.021(2) 0.011(2) C19 0.030(2) 0.037(3) 0.090(4) 0.016(2) 0.023(3) 0.002(2) C20 0.022(2) 0.0305(19) 0.028(2) 0.0000(17) 0.0042(19) 0.0016(18) C21 0.033(2) 0.042(2) 0.067(3) -0.005(2) 0.022(2) -0.005(2) C22 0.0267(19) 0.041(2) 0.033(2) -0.0035(19) -0.0053(19) 0.0086(17) _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 C17 1.381(4) . ? O1 H1 0.9900 . ? O2 C26 1.399(8) . ? O2 H2 0.8400 . ? O2A C26A 1.392(13) . ? O2A H2A 0.9900 . ? O3 C8 1.446(4) . ? O3 H3 0.9900 . ? C1 C2 1.187(5) . ? C1 H1A 0.93(4) . ? C2 C3 1.428(6) . ? C3 C4 1.310(5) . ? C3 C11 1.552(5) . ? C4 C5 1.322(5) . ? C5 C6 1.439(5) . ? C5 C20 1.529(5) . ? C6 C7 1.199(5) . ? C7 C8 1.477(5) . ? C8 C9 1.531(5) . ? C8 C10 1.532(5) . ? C9 H9A 1.0899 . ? C9 H9B 1.0899 . ? C9 H9C 1.0899 . ? C10 H10A 1.0899 . ? C10 H10B 1.0899 . ? C10 H10C 1.0899 . ? C11 C14 1.520(5) . ? C11 C12 1.532(5) . ? C11 C13 1.538(5) . ? C12 H12A 1.0899 . ? C12 H12B 1.0899 . ? C12 H12C 1.0899 . ? C13 H13A 1.0899 . ? C13 H13B 1.0899 . ? C13 H13C 1.0899 . ? C14 C19 1.369(5) . ? C14 C15 1.384(4) . ? C15 C16 1.395(4) . ? C15 H15 1.0800 . ? C16 C17 1.360(4) . ? C16 H16 1.0800 . ? C17 C18 1.380(5) . ? C18 C19 1.392(5) . ? C18 H18 1.0800 . ? C19 H19 1.0800 . ? C20 C23 1.476(11) . ? C20 C22 1.527(5) . ? C20 C21 1.536(5) . ? C20 C23A 1.614(19) . ? C21 H21A 1.0899 . ? C21 H21B 1.0899 . ? C21 H21C 1.0899 . ? C22 H22A 1.0899 . ? C22 H22B 1.0899 . ? C22 H22C 1.0899 . ? C23 C24 1.396(12) . ? C23 C28 1.403(14) . ? C23A C24A 1.37(2) . ? C23A C28A 1.42(2) . ? C24 C25 1.393(10) . ? C24 H24 1.0800 . ? C24A C25A 1.376(16) . ? C24A H24A 1.0800 . ? C25 C26 1.391(12) . ? C25 H25 1.0800 . ? C25A C26A 1.447(18) . ? C25A H25A 1.0800 . ? C26 C27 1.374(11) . ? C26A C27A 1.399(17) . ? C27 C28 1.400(11) . ? C27 H27 1.0800 . ? C27A C28A 1.378(14) . ? C27A H27A 1.0800 . ? C28 H28 1.0800 . ? C28A H28A 1.0800 . ? 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 C17 O1 H1 109.5 . . ? C26A O2A H2A 109.5 . . ? C8 O3 H3 109.5 . . ? C2 C1 H1A 177(3) . . ? C1 C2 C3 176.5(4) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 C11 122.5(3) . . ? C2 C3 C11 117.8(3) . . ? C3 C4 C5 176.0(4) . . ? C4 C5 C6 119.1(3) . . ? C4 C5 C20 122.5(3) . . ? C6 C5 C20 118.3(3) . . ? C7 C6 C5 173.6(3) . . ? C6 C7 C8 176.0(4) . . ? O3 C8 C7 108.8(3) . . ? O3 C8 C9 105.5(2) . . ? C7 C8 C9 110.0(3) . . ? O3 C8 C10 110.1(3) . . ? C7 C8 C10 110.8(3) . . ? C9 C8 C10 111.4(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 111.8(3) . . ? C14 C11 C13 111.2(3) . . ? C12 C11 C13 108.2(3) . . ? C14 C11 C3 109.1(3) . . ? C12 C11 C3 108.8(3) . . ? C13 C11 C3 107.5(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 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 116.1(3) . . ? C19 C14 C11 121.7(3) . . ? C15 C14 C11 122.2(3) . . ? C14 C15 C16 121.9(3) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.6(3) . . ? C16 C17 O1 119.3(3) . . ? C18 C17 O1 121.1(3) . . ? C17 C18 C19 118.8(4) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C14 C19 C18 123.3(4) . . ? C14 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? C23 C20 C22 110.6(4) . . ? C23 C20 C5 110.2(5) . . ? C22 C20 C5 111.1(3) . . ? C23 C20 C21 108.6(5) . . ? C22 C20 C21 108.9(3) . . ? C5 C20 C21 107.4(3) . . ? C23 C20 C23A 9.7(8) . . ? C22 C20 C23A 107.0(6) . . ? C5 C20 C23A 104.2(6) . . ? C21 C20 C23A 118.2(7) . . ? 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 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 116.2(8) . . ? C24 C23 C20 122.2(8) . . ? C28 C23 C20 121.5(8) . . ? C24A C23A C28A 120.0(17) . . ? C24A C23A C20 124.1(15) . . ? C28A C23A C20 115.9(12) . . ? C25 C24 C23 122.4(8) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C23A C24A C25A 123.2(13) . . ? C23A C24A H24A 118.4 . . ? C25A C24A H24A 118.4 . . ? C26 C25 C24 118.8(7) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C24A C25A C26A 116.2(10) . . ? C24A C25A H25A 121.9 . . ? C26A C25A H25A 121.9 . . ? C27 C26 C25 121.5(7) . . ? C27 C26 O2 118.1(9) . . ? C25 C26 O2 120.4(6) . . ? O2A C26A C27A 118.1(10) . . ? O2A C26A C25A 120.7(12) . . ? C27A C26A C25A 121.3(11) . . ? C26 C27 C28 118.2(7) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C28A C27A C26A 119.7(11) . . ? C28A C27A H27A 120.2 . . ? C26A C27A H27A 120.2 . . ? C27 C28 C23 122.8(8) . . ? C27 C28 H28 118.6 . . ? C23 C28 H28 118.6 . . ? C27A C28A C23A 119.6(13) . . ? C27A C28A H28A 120.2 . . ? C23A C28A H28A 120.2 . . ? 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 -110(6) . . . . ? C1 C2 C3 C11 69(6) . . . . ? C2 C3 C4 C5 126(5) . . . . ? C11 C3 C4 C5 -53(5) . . . . ? C3 C4 C5 C6 133(5) . . . . ? C3 C4 C5 C20 -45(5) . . . . ? C4 C5 C6 C7 -97(3) . . . . ? C20 C5 C6 C7 81(3) . . . . ? C5 C6 C7 C8 37(7) . . . . ? C6 C7 C8 O3 13(5) . . . . ? C6 C7 C8 C9 -102(5) . . . . ? C6 C7 C8 C10 134(5) . . . . ? C4 C3 C11 C14 -6.1(4) . . . . ? C2 C3 C11 C14 175.1(3) . . . . ? C4 C3 C11 C12 116.1(4) . . . . ? C2 C3 C11 C12 -62.7(4) . . . . ? C4 C3 C11 C13 -126.9(3) . . . . ? C2 C3 C11 C13 54.3(4) . . . . ? C12 C11 C14 C19 151.8(4) . . . . ? C13 C11 C14 C19 30.7(5) . . . . ? C3 C11 C14 C19 -87.8(4) . . . . ? C12 C11 C14 C15 -30.5(4) . . . . ? C13 C11 C14 C15 -151.6(3) . . . . ? C3 C11 C14 C15 89.9(4) . . . . ? C19 C14 C15 C16 -3.1(5) . . . . ? C11 C14 C15 C16 179.2(3) . . . . ? C14 C15 C16 C17 0.5(5) . . . . ? C15 C16 C17 C18 2.8(5) . . . . ? C15 C16 C17 O1 -175.1(3) . . . . ? C16 C17 C18 C19 -3.3(6) . . . . ? O1 C17 C18 C19 174.5(4) . . . . ? C15 C14 C19 C18 2.5(6) . . . . ? C11 C14 C19 C18 -179.7(4) . . . . ? C17 C18 C19 C14 0.6(7) . . . . ? C4 C5 C20 C23 -123.8(5) . . . . ? C6 C5 C20 C23 59.0(5) . . . . ? C4 C5 C20 C22 -0.8(4) . . . . ? C6 C5 C20 C22 -178.0(3) . . . . ? C4 C5 C20 C21 118.1(4) . . . . ? C6 C5 C20 C21 -59.1(4) . . . . ? C4 C5 C20 C23A -115.7(7) . . . . ? C6 C5 C20 C23A 67.1(7) . . . . ? C22 C20 C23 C24 102.8(8) . . . . ? C5 C20 C23 C24 -133.9(7) . . . . ? C21 C20 C23 C24 -16.6(9) . . . . ? C23A C20 C23 C24 173(6) . . . . ? C22 C20 C23 C28 -73.2(8) . . . . ? C5 C20 C23 C28 50.0(8) . . . . ? C21 C20 C23 C28 167.4(6) . . . . ? C23A C20 C23 C28 -3(4) . . . . ? C23 C20 C23A C24A 9(4) . . . . ? C22 C20 C23A C24A 122.2(12) . . . . ? C5 C20 C23A C24A -120.1(12) . . . . ? C21 C20 C23A C24A -1.1(15) . . . . ? C23 C20 C23A C28A -174(6) . . . . ? C22 C20 C23A C28A -60.8(12) . . . . ? C5 C20 C23A C28A 56.9(11) . . . . ? C21 C20 C23A C28A 175.9(8) . . . . ? C28 C23 C24 C25 -1.6(11) . . . . ? C20 C23 C24 C25 -177.8(6) . . . . ? C28A C23A C24A C25A 3(2) . . . . ? C20 C23A C24A C25A 179.8(10) . . . . ? C23 C24 C25 C26 -0.6(10) . . . . ? C23A C24A C25A C26A -2.0(17) . . . . ? C24 C25 C26 C27 1.5(10) . . . . ? C24 C25 C26 O2 180.0(5) . . . . ? C24A C25A C26A O2A -176.9(9) . . . . ? C24A C25A C26A C27A 1.5(15) . . . . ? C25 C26 C27 C28 -0.1(9) . . . . ? O2 C26 C27 C28 -178.6(6) . . . . ? O2A C26A C27A C28A 176.6(9) . . . . ? C25A C26A C27A C28A -1.9(14) . . . . ? C26 C27 C28 C23 -2.3(10) . . . . ? C24 C23 C28 C27 3.1(11) . . . . ? C20 C23 C28 C27 179.3(7) . . . . ? C26A C27A C28A C23A 2.6(15) . . . . ? C24A C23A C28A C27A -3.1(18) . . . . ? C20 C23A C28A C27A 179.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 50.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.235 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 926014' ####################################################################### # # 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_cu_d050412_0m _audit_creation_date 2013-06-04 _audit_creation_method ; Olex2 1.2 (compiled Apr 9 2013 14:10:59, GUI svn.r4458) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C H2 Cl2, C100 H88 O8, 2(C3.5 H8)' _chemical_formula_sum 'C108 H106 Cl2 O8' _chemical_formula_weight 1602.83 _chemical_absolute_configuration unk _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 0.0181 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' Cl Cl 0.3639 0.7018 '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 5 _space_group_name_H-M_alt 'C 1 2 1' _space_group_name_Hall 'C 2y' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z' _cell_length_a 27.930(3) _cell_length_b 8.9770(9) _cell_length_c 20.9383(15) _cell_angle_alpha 90.00 _cell_angle_beta 111.190(6) _cell_angle_gamma 90.00 _cell_volume 4894.8(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5471 _cell_measurement_temperature 100 _cell_measurement_theta_max 49.48 _cell_measurement_theta_min 3.33 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_T_max 0.7499 _exptl_absorpt_correction_T_min 0.5764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0957 before and 0.0514 after correction. The Ratio of minimum to maximum transmission is 0.7686. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 1704 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 9424 _diffrn_reflns_theta_full 50.08 _diffrn_reflns_theta_max 50.08 _diffrn_reflns_theta_min 2.26 _diffrn_ambient_temperature 99.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_number_gt 2392 _reflns_number_total 2706 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; 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_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 ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.560 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.087 _refine_ls_abs_structure_details ; 'Flack H D (1983), Acta Cryst. A39, 876-881' ; _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.408 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 546 _refine_ls_number_reflns 2706 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.1055 _refine_ls_restrained_S_all 1.410 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2781 _refine_ls_wR_factor_ref 0.2893 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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, All O(H) groups 2. Restrained distances C61-C60 = C62-C61 = C63-C62 1.53 with sigma of 0.02 C57-C56 1.53 with sigma of 0.02 C57-C58 1.53 with sigma of 0.02 C58-C59 1.53 with sigma of 0.02 Cl1-C55 = Cl2-C55 1.77 with sigma of 0.02 C60-C62 = C61-C63 2.45 with sigma of 0.04 C56-C58 2.45 with sigma of 0.04 C57-C59 2.45 with sigma of 0.04 Cl1-Cl2 2.93 with sigma of 0.04 3. Others Fixed Sof: Cl1(0.5) Cl2(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.25) H59A(0.25) H59B(0.25) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.25) H63A(0.25) H63B(0.25) Fixed X: C59(0) Fixed Z: C59(0) 4.a Secondary CH2 refined with riding coordinates: C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C61(H61A, H61B), C62(H62A,H62B), C63(H63A,H63B) 4.b Aromatic/amide H refined with riding coordinates: C19(H19), C20(H20), C22(H22), C23(H23), C29(H29), C30(H30), C32(H32), C33(H33), C39(H39), C40(H40), C42(H42), C43(H43), C49(H49), C50(H50), C52(H52), C53(H53) 4.c Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,H27B, H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C47(H47A, H47B,H47C), C56(H56A,H56B,H56C), C60(H60A,H60B,H60C) 4.d Idealised tetrahedral OH refined as rotating group: O24(H24), O34(H34), O44(H44), O54(H54) ; _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.0616(7) 0.342(2) 1.4896(9) 0.221(6) Uani 0.50 1 d PD A -1 Cl2 Cl 0.0018(19) 0.564(5) 1.525(2) 0.41(2) Uiso 0.50 1 d PD A -1 C55 C 0.009(3) 0.463(9) 1.454(2) 0.29(4) Uiso 0.50 1 d PD A -1 H55A H -0.0261 0.3996 1.4274 0.349 Uiso 0.50 1 calc PR A -1 H55B H 0.0156 0.5397 1.4183 0.349 Uiso 0.50 1 calc PR A -1 O24 O -0.1642(5) 0.4149(13) 0.4742(4) 0.128(4) Uani 1 1 d . . . H24 H -0.1438 0.3231 0.4838 0.193 Uiso 1 1 calc R . . O34 O -0.0922(6) 0.8590(17) 0.4540(4) 0.173(6) Uani 1 1 d . . . H34 H -0.1219 0.8171 0.4173 0.260 Uiso 1 1 calc R . . O44 O 0.0546(4) 0.1048(15) 0.5702(4) 0.122(3) Uani 1 1 d . . . H44 H 0.0709 0.0096 0.5674 0.183 Uiso 1 1 calc R . . O54 O 0.1386(3) 0.6053(11) 0.6057(3) 0.090(2) Uani 1 1 d . . . H54 H 0.1523 0.5217 0.5875 0.134 Uiso 1 1 calc R . . C1 C -0.2002(3) 0.6251(11) 0.7496(4) 0.044(2) Uani 1 1 d . . . C2 C -0.1633(3) 0.7009(11) 0.7410(3) 0.045(2) Uani 1 1 d . . . C3 C -0.1238(3) 0.7742(12) 0.7347(4) 0.053(2) Uani 1 1 d . . . C4 C -0.0757(4) 0.6968(14) 0.7572(4) 0.061(3) Uani 1 1 d . . . C5 C -0.0360(4) 0.6356(15) 0.7769(4) 0.067(3) Uani 1 1 d . . . C6 C 0.0116(4) 0.5585(15) 0.8015(5) 0.075(4) Uani 1 1 d . . . C7 C 0.0524(3) 0.4905(16) 0.8278(5) 0.074(3) Uani 1 1 d . . . C8 C 0.0971(4) 0.4161(15) 0.8581(4) 0.065(3) Uani 1 1 d . . . C9 C 0.1407(4) 0.4938(13) 0.8935(5) 0.065(3) Uani 1 1 d . . . C10 C 0.1822(3) 0.5663(11) 0.9290(4) 0.048(2) Uani 1 1 d . . . C11 C 0.1921(3) 0.5892(11) 0.9997(5) 0.052(2) Uani 1 1 d . . . C12 C 0.1986(3) 0.6096(12) 1.0585(5) 0.051(2) Uani 1 1 d . . . C13 C 0.2040(3) 0.6252(12) 1.1266(5) 0.057(2) Uani 1 1 d . . . C14 C 0.2046(3) 0.6294(12) 1.1854(5) 0.056(2) Uani 1 1 d . . . C15 C -0.2379(4) 0.5275(13) 0.6947(4) 0.062(3) Uani 1 1 d . . . C16 C -0.2916(4) 0.5991(17) 0.6729(6) 0.090(4) Uani 1 1 d . . . H16A H -0.3040 0.6030 0.7167 0.135 Uiso 1 1 calc R . . H16B H -0.3188 0.5330 0.6322 0.135 Uiso 1 1 calc R . . H16C H -0.2901 0.7119 0.6544 0.135 Uiso 1 1 calc R . . C17 C -0.2403(6) 0.3717(14) 0.7264(6) 0.094(4) Uani 1 1 d . . . H17A H -0.2024 0.3203 0.7435 0.141 Uiso 1 1 calc R . . H17B H -0.2676 0.3011 0.6879 0.141 Uiso 1 1 calc R . . H17C H -0.2526 0.3848 0.7698 0.141 Uiso 1 1 calc R . . C18 C -0.2196(4) 0.5071(14) 0.6340(5) 0.070(3) Uani 1 1 d . . . C19 C -0.1737(5) 0.4360(14) 0.6453(5) 0.084(3) Uani 1 1 d . . . H19 H -0.1516 0.4005 0.6969 0.101 Uiso 1 1 calc R . . C20 C -0.1537(7) 0.4065(15) 0.5932(8) 0.114(5) Uani 1 1 d . . . H20 H -0.1163 0.3562 0.6054 0.136 Uiso 1 1 calc R . . C21 C -0.1824(7) 0.4427(16) 0.5280(6) 0.095(4) Uani 1 1 d . . . C22 C -0.2297(5) 0.5144(19) 0.5120(5) 0.091(4) Uani 1 1 d . . . H22 H -0.2517 0.5439 0.4595 0.109 Uiso 1 1 calc R . . C23 C -0.2497(5) 0.5500(15) 0.5665(5) 0.091(4) Uani 1 1 d . . . H23 H -0.2859 0.6067 0.5552 0.109 Uiso 1 1 calc R . . C25 C -0.1251(3) 0.9302(13) 0.7054(4) 0.062(3) Uani 1 1 d . . . C26 C -0.0841(4) 1.0220(16) 0.7585(5) 0.083(4) Uani 1 1 d . . . H26A H -0.0938 1.0337 0.8042 0.124 Uiso 1 1 calc R . . H26B H -0.0819 1.1318 0.7376 0.124 Uiso 1 1 calc R . . H26C H -0.0471 0.9662 0.7718 0.124 Uiso 1 1 calc R . . C27 C -0.1781(4) 0.9961(12) 0.6928(5) 0.067(3) Uani 1 1 d . . . H27A H -0.2075 0.9227 0.6589 0.101 Uiso 1 1 calc R . . H27B H -0.1809 1.1053 0.6689 0.101 Uiso 1 1 calc R . . H27C H -0.1838 1.0073 0.7414 0.101 Uiso 1 1 calc R . . C28 C -0.1142(4) 0.9148(12) 0.6400(4) 0.061(3) Uani 1 1 d . . . C29 C -0.0768(5) 0.994(2) 0.6282(5) 0.111(5) Uani 1 1 d . . . H29 H -0.0550 1.0746 0.6655 0.133 Uiso 1 1 calc R . . C30 C -0.0656(8) 0.972(3) 0.5677(8) 0.168(10) Uani 1 1 d . . . H30 H -0.0321 1.0186 0.5609 0.201 Uiso 1 1 calc R . . C31 C -0.1045(7) 0.878(2) 0.5139(6) 0.124(6) Uani 1 1 d . . . C32 C -0.1389(4) 0.8040(15) 0.5254(5) 0.079(3) Uani 1 1 d . . . H32 H -0.1624 0.7265 0.4876 0.095 Uiso 1 1 calc R . . C33 C -0.1464(4) 0.8230(14) 0.5877(5) 0.072(3) Uani 1 1 d . . . H33 H -0.1778 0.7656 0.5957 0.086 Uiso 1 1 calc R . . C35 C 0.0975(4) 0.2487(17) 0.8510(5) 0.080(4) Uani 1 1 d . . . C36 C 0.1514(6) 0.1835(18) 0.8894(7) 0.121(6) Uani 1 1 d . . . H36A H 0.1784 0.2291 0.8678 0.182 Uiso 1 1 calc R . . H36B H 0.1500 0.0626 0.8840 0.182 Uiso 1 1 calc R . . H36C H 0.1638 0.2126 0.9435 0.182 Uiso 1 1 calc R . . C37 C 0.0577(5) 0.185(2) 0.8775(7) 0.119(6) Uani 1 1 d . . . H37A H 0.0595 0.2447 0.9238 0.179 Uiso 1 1 calc R . . H37B H 0.0654 0.0674 0.8893 0.179 Uiso 1 1 calc R . . H37C H 0.0195 0.1982 0.8385 0.179 Uiso 1 1 calc R . . C38 C 0.0860(3) 0.2097(16) 0.7755(5) 0.078(3) Uani 1 1 d . . . C39 C 0.0954(4) 0.307(2) 0.7301(5) 0.095(4) Uani 1 1 d . . . H39 H 0.1124 0.4138 0.7493 0.114 Uiso 1 1 calc R . . C40 C 0.0842(4) 0.275(2) 0.6613(7) 0.097(4) Uani 1 1 d . . . H40 H 0.0904 0.3564 0.6270 0.117 Uiso 1 1 calc R . . C41 C 0.0656(5) 0.142(2) 0.6395(7) 0.093(4) Uani 1 1 d . . . C42 C 0.0561(5) 0.0340(19) 0.6797(7) 0.104(4) Uani 1 1 d . . . H42 H 0.0415 -0.0741 0.6592 0.124 Uiso 1 1 calc R . . C43 C 0.0663(5) 0.0706(17) 0.7502(6) 0.091(4) Uani 1 1 d . . . H43 H 0.0586 -0.0101 0.7836 0.109 Uiso 1 1 calc R . . C45 C 0.2217(3) 0.6138(11) 0.8975(4) 0.051(2) Uani 1 1 d . . . C46 C 0.2683(3) 0.5159(14) 0.9288(4) 0.059(3) Uani 1 1 d . . . H46A H 0.2831 0.5297 0.9842 0.089 Uiso 1 1 calc R . . H46B H 0.2977 0.5475 0.9085 0.089 Uiso 1 1 calc R . . H46C H 0.2576 0.3999 0.9161 0.089 Uiso 1 1 calc R . . C47 C 0.2371(4) 0.7775(12) 0.9192(4) 0.062(3) Uani 1 1 d . . . H47A H 0.2033 0.8485 0.9002 0.093 Uiso 1 1 calc R . . H47B H 0.2653 0.8145 0.8978 0.093 Uiso 1 1 calc R . . H47C H 0.2537 0.7845 0.9749 0.093 Uiso 1 1 calc R . . C48 C 0.1984(3) 0.6063(12) 0.8188(4) 0.055(2) Uani 1 1 d . . . C49 C 0.1578(4) 0.6948(14) 0.7843(5) 0.070(3) Uani 1 1 d . . . H49 H 0.1414 0.7672 0.8122 0.085 Uiso 1 1 calc R . . C50 C 0.1374(4) 0.6919(16) 0.7130(5) 0.079(3) Uani 1 1 d . . . H50 H 0.1044 0.7598 0.6855 0.095 Uiso 1 1 calc R . . C51 C 0.1592(4) 0.6025(15) 0.6772(4) 0.067(3) Uani 1 1 d . . . C52 C 0.1985(4) 0.5143(13) 0.7102(4) 0.061(3) Uani 1 1 d . . . H52 H 0.2146 0.4422 0.6818 0.073 Uiso 1 1 calc R . . C53 C 0.2190(3) 0.5149(12) 0.7819(4) 0.056(2) Uani 1 1 d . . . H53 H 0.2512 0.4436 0.8087 0.068 Uiso 1 1 calc R . . C56 C 0.1240(10) 0.271(4) 0.1012(14) 0.105(8) Uiso 0.50 1 d PD B 1 H56A H 0.1230 0.2798 0.0488 0.157 Uiso 0.50 1 calc PR B 1 H56B H 0.1219 0.1545 0.1141 0.157 Uiso 0.50 1 calc PR B 1 H56C H 0.1596 0.3195 0.1362 0.157 Uiso 0.50 1 calc PR B 1 C57 C 0.0789(14) 0.355(7) 0.1073(19) 0.25(3) Uiso 0.50 1 d PD B 1 H57A H 0.0545 0.2748 0.1202 0.294 Uiso 0.50 1 calc PR B 1 H57B H 0.0935 0.4323 0.1500 0.294 Uiso 0.50 1 calc PR B 1 C58 C 0.0464(14) 0.440(5) 0.045(2) 0.202(19) Uiso 0.50 1 d PD B 1 H58A H 0.0697 0.4715 0.0156 0.242 Uiso 0.50 1 calc PR B 1 H58B H 0.0329 0.5417 0.0617 0.242 Uiso 0.50 1 calc PR B 1 C59 C 0.0000 0.349(8) 0.0000 0.17(2) Uiso 0.50 2 d SPD . 1 H59A H -0.0125 0.2772 0.0329 0.204 Uiso 0.25 1 calc PR . 1 H59B H 0.0125 0.2771 -0.0329 0.204 Uiso 0.25 1 calc PR . 1 C60 C 0.0785(17) 0.856(8) -0.0036(19) 0.191(17) Uiso 0.50 1 d PD . . H60A H 0.0511 0.7751 -0.0352 0.286 Uiso 0.50 1 calc PR . . H60B H 0.1172 0.8249 0.0002 0.286 Uiso 0.50 1 calc PR . . H60C H 0.0693 0.9662 -0.0269 0.286 Uiso 0.50 1 calc PR . . C61 C 0.0757(11) 0.860(6) 0.0676(17) 0.174(16) Uiso 0.50 1 d PD . . H61A H 0.0941 0.9595 0.0953 0.209 Uiso 0.50 1 calc PR . . H61B H 0.0942 0.7618 0.0971 0.209 Uiso 0.50 1 calc PR . . C62 C 0.0172(12) 0.860(5) 0.0534(19) 0.171(15) Uiso 0.50 1 d PD . . H62A H 0.0090 0.8342 0.0994 0.205 Uiso 0.50 1 calc PR . . H62B H -0.0006 0.9661 0.0323 0.205 Uiso 0.50 1 calc PR . . C63 C 0.0000 0.733(6) 0.0000 0.17(2) Uiso 0.50 2 d SPD . . H63A H -0.0313 0.6650 0.0033 0.208 Uiso 0.25 1 calc PR . . H63B H 0.0313 0.6650 -0.0033 0.208 Uiso 0.25 1 calc PR . . 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 Cl1 0.274(16) 0.202(14) 0.227(14) -0.017(12) 0.139(12) -0.024(14) O24 0.216(11) 0.119(8) 0.081(5) -0.019(6) 0.091(7) -0.011(8) O34 0.272(14) 0.211(13) 0.053(5) -0.039(7) 0.079(7) -0.126(12) O44 0.151(8) 0.141(9) 0.092(6) -0.020(6) 0.067(5) -0.023(8) O54 0.110(6) 0.119(7) 0.041(4) -0.002(4) 0.029(3) 0.000(5) C1 0.044(5) 0.056(6) 0.033(5) 0.001(4) 0.016(4) 0.005(5) C2 0.037(5) 0.066(6) 0.031(4) -0.005(4) 0.008(4) 0.005(5) C3 0.048(5) 0.077(7) 0.037(5) -0.005(5) 0.020(4) -0.010(5) C4 0.044(6) 0.097(8) 0.044(5) -0.004(5) 0.017(4) -0.003(6) C5 0.044(6) 0.110(9) 0.048(5) 0.010(6) 0.019(4) 0.011(6) C6 0.061(7) 0.119(10) 0.052(5) -0.017(6) 0.029(5) -0.017(7) C7 0.025(5) 0.136(11) 0.061(6) 0.001(6) 0.015(4) 0.016(6) C8 0.047(6) 0.107(10) 0.040(5) -0.010(6) 0.014(4) -0.010(7) C9 0.058(7) 0.092(8) 0.060(6) 0.014(6) 0.039(6) 0.024(7) C10 0.027(5) 0.066(7) 0.047(5) -0.006(4) 0.009(4) 0.000(4) C11 0.058(5) 0.059(6) 0.044(7) 0.003(5) 0.025(4) 0.006(5) C12 0.061(6) 0.061(6) 0.038(6) 0.005(5) 0.026(4) 0.011(5) C13 0.059(6) 0.058(6) 0.063(7) 0.002(5) 0.034(4) 0.003(5) C14 0.059(6) 0.065(6) 0.051(6) -0.007(5) 0.031(4) -0.003(5) C15 0.076(6) 0.070(7) 0.051(5) -0.001(5) 0.036(5) -0.016(6) C16 0.052(6) 0.118(10) 0.098(8) -0.031(8) 0.023(5) -0.026(7) C17 0.155(11) 0.067(8) 0.094(8) -0.022(6) 0.086(8) -0.032(8) C18 0.089(7) 0.068(7) 0.058(6) -0.002(5) 0.030(5) -0.022(7) C19 0.143(11) 0.069(8) 0.065(6) -0.003(6) 0.067(7) -0.004(8) C20 0.213(16) 0.069(8) 0.113(12) 0.008(8) 0.124(12) 0.013(10) C21 0.160(13) 0.079(8) 0.063(8) -0.009(7) 0.060(8) -0.021(9) C22 0.106(9) 0.133(11) 0.032(5) -0.018(7) 0.022(6) -0.040(10) C23 0.111(9) 0.087(9) 0.067(7) -0.014(6) 0.022(6) -0.044(8) C25 0.056(6) 0.076(7) 0.049(5) -0.011(5) 0.013(4) -0.022(5) C26 0.095(8) 0.106(9) 0.062(6) -0.028(6) 0.044(6) -0.042(8) C27 0.072(7) 0.054(6) 0.078(6) -0.005(5) 0.030(5) -0.009(5) C28 0.068(6) 0.073(7) 0.043(5) -0.004(5) 0.022(4) -0.019(6) C29 0.132(10) 0.148(13) 0.063(7) -0.015(8) 0.047(7) -0.077(11) C30 0.226(18) 0.21(2) 0.112(10) -0.077(13) 0.112(11) -0.154(18) C31 0.195(15) 0.139(14) 0.063(7) -0.024(8) 0.079(9) -0.076(13) C32 0.086(7) 0.094(9) 0.057(6) -0.011(6) 0.025(5) -0.024(7) C33 0.080(7) 0.080(8) 0.051(6) -0.001(6) 0.018(5) -0.013(6) C35 0.060(6) 0.112(11) 0.058(6) -0.002(7) 0.010(5) -0.023(7) C36 0.119(11) 0.081(9) 0.100(9) 0.011(8) -0.038(8) -0.016(8) C37 0.125(10) 0.160(15) 0.089(8) -0.035(10) 0.058(7) -0.062(11) C38 0.040(5) 0.108(11) 0.076(7) -0.009(8) 0.009(5) -0.004(6) C39 0.085(7) 0.157(14) 0.050(6) -0.021(8) 0.033(5) -0.035(8) C40 0.081(8) 0.118(13) 0.101(10) -0.005(9) 0.042(6) -0.037(8) C41 0.096(9) 0.124(13) 0.082(8) 0.005(9) 0.061(7) -0.003(9) C42 0.102(9) 0.110(11) 0.110(10) -0.017(9) 0.051(8) 0.018(9) C43 0.095(8) 0.104(11) 0.083(8) -0.005(8) 0.043(6) 0.001(8) C45 0.056(5) 0.062(6) 0.041(5) 0.007(5) 0.023(4) 0.007(5) C46 0.041(5) 0.087(7) 0.052(5) 0.009(5) 0.019(4) 0.009(5) C47 0.067(6) 0.074(7) 0.046(5) -0.003(5) 0.021(4) 0.001(5) C48 0.053(5) 0.069(6) 0.045(5) 0.002(5) 0.021(4) 0.008(6) C49 0.079(7) 0.086(8) 0.050(6) 0.000(6) 0.028(5) 0.017(7) C50 0.071(6) 0.099(9) 0.054(6) 0.017(6) 0.007(5) 0.017(7) C51 0.069(6) 0.094(8) 0.039(5) 0.000(6) 0.020(5) 0.010(7) C52 0.069(6) 0.076(7) 0.050(6) -0.003(6) 0.035(5) -0.008(6) C53 0.057(5) 0.065(6) 0.057(6) 0.003(5) 0.032(4) 0.003(5) _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 Cl1 C55 1.77(2) . ? Cl2 C55 1.79(2) . ? C55 H55A 1.0900 . ? C55 H55B 1.0900 . ? O24 H24 0.9801 . ? O24 C21 1.415(15) . ? O34 H34 0.9801 . ? O34 C31 1.425(16) . ? O44 H44 0.9801 . ? O44 C41 1.410(15) . ? O54 H54 0.9801 . ? O54 C51 1.398(11) . ? C1 C2 1.301(13) . ? C1 C14 1.410(13) 2_557 ? C1 C15 1.523(14) . ? C2 C3 1.332(13) . ? C3 C4 1.432(16) . ? C3 C25 1.523(16) . ? C4 C5 1.172(14) . ? C5 C6 1.420(17) . ? C6 C7 1.233(15) . ? C7 C8 1.354(16) . ? C8 C9 1.367(16) . ? C8 C35 1.510(19) . ? C9 C10 1.302(14) . ? C10 C11 1.419(13) . ? C10 C45 1.537(12) . ? C11 C12 1.192(12) . ? C12 C13 1.384(16) . ? C13 C14 1.226(12) . ? C14 C1 1.410(13) 2_557 ? C15 C16 1.543(16) . ? C15 C17 1.559(17) . ? C15 C18 1.543(14) . ? C16 H16A 1.0899 . ? C16 H16B 1.0899 . ? C16 H16C 1.0899 . ? C17 H17A 1.0899 . ? C17 H17B 1.0899 . ? C17 H17C 1.0899 . ? C18 C19 1.373(16) . ? C18 C23 1.413(15) . ? C19 H19 1.0800 . ? C19 C20 1.420(16) . ? C20 H20 1.0800 . ? C20 C21 1.35(2) . ? C21 C22 1.397(19) . ? C22 H22 1.0800 . ? C22 C23 1.476(17) . ? C23 H23 1.0800 . ? C25 C26 1.519(14) . ? C25 C27 1.526(14) . ? C25 C28 1.513(13) . ? C26 H26A 1.0899 . ? C26 H26B 1.0899 . ? C26 H26C 1.0899 . ? C27 H27A 1.0899 . ? C27 H27B 1.0899 . ? C27 H27C 1.0899 . ? C28 C29 1.356(15) . ? C28 C33 1.406(14) . ? C29 H29 1.0800 . ? C29 C30 1.424(18) . ? C30 H30 1.0800 . ? C30 C31 1.51(2) . ? C31 C32 1.262(18) . ? C32 H32 1.0800 . ? C32 C33 1.405(15) . ? C33 H33 1.0800 . ? C35 C36 1.543(18) . ? C35 C37 1.521(17) . ? C35 C38 1.537(16) . ? C36 H36A 1.0899 . ? C36 H36B 1.0899 . ? C36 H36C 1.0899 . ? C37 H37A 1.0899 . ? C37 H37B 1.0899 . ? C37 H37C 1.0899 . ? C38 C39 1.384(19) . ? C38 C43 1.390(19) . ? C39 H39 1.0800 . ? C39 C40 1.390(17) . ? C40 H40 1.0800 . ? C40 C41 1.32(2) . ? C41 C42 1.37(2) . ? C42 H42 1.0800 . ? C42 C43 1.437(17) . ? C43 H43 1.0800 . ? C45 C46 1.509(13) . ? C45 C47 1.553(16) . ? C45 C48 1.539(12) . ? C46 H46A 1.0899 . ? C46 H46B 1.0899 . ? C46 H46C 1.0899 . ? C47 H47A 1.0899 . ? C47 H47B 1.0899 . ? C47 H47C 1.0899 . ? C48 C49 1.359(14) . ? C48 C53 1.386(13) . ? C49 H49 1.0800 . ? C49 C50 1.394(13) . ? C50 H50 1.0800 . ? C50 C51 1.381(16) . ? C51 C52 1.325(14) . ? C52 H52 1.0800 . ? C52 C53 1.400(12) . ? C53 H53 1.0800 . ? C56 H56A 1.0899 . ? C56 H56B 1.0899 . ? C56 H56C 1.0899 . ? C56 C57 1.51(2) . ? C57 H57A 1.0900 . ? C57 H57B 1.0900 . ? C57 C58 1.50(2) . ? C58 H58A 1.0900 . ? C58 H58B 1.0900 . ? C58 C59 1.54(2) . ? C59 C58 1.54(2) 2 ? C59 H59A 1.0900 . ? C59 H59B 1.0900 . ? C60 H60A 1.0899 . ? C60 H60B 1.0899 . ? C60 H60C 1.0899 . ? C60 C61 1.52(2) . ? C61 H61A 1.0900 . ? C61 H61B 1.0900 . ? C61 C62 1.55(2) . ? C62 H62A 1.0900 . ? C62 H62B 1.0900 . ? C62 C63 1.55(2) . ? C63 C62 1.55(2) 2 ? C63 H63A 1.0900 . ? C63 H63B 1.0900 . ? 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 Cl1 C55 Cl2 107(2) . . ? Cl1 C55 H55A 110.4 . . ? Cl1 C55 H55B 110.4 . . ? Cl2 C55 H55A 110.4 . . ? Cl2 C55 H55B 110.4 . . ? H55A C55 H55B 108.6 . . ? C21 O24 H24 109.5 . . ? C31 O34 H34 109.5 . . ? C41 O44 H44 109.5 . . ? C51 O54 H54 109.5 . . ? C2 C1 C14 118.0(7) . 2_557 ? C2 C1 C15 124.2(7) . . ? C14 C1 C15 117.8(8) 2_557 . ? C1 C2 C3 177.0(9) . . ? C2 C3 C4 116.1(10) . . ? C2 C3 C25 126.4(9) . . ? C4 C3 C25 117.5(8) . . ? C5 C4 C3 178.4(11) . . ? C4 C5 C6 178.5(12) . . ? C7 C6 C5 175.0(9) . . ? C6 C7 C8 178.6(9) . . ? C7 C8 C9 119.5(12) . . ? C7 C8 C35 118.9(10) . . ? C9 C8 C35 121.6(10) . . ? C10 C9 C8 178.2(9) . . ? C9 C10 C11 117.8(8) . . ? C9 C10 C45 121.4(7) . . ? C11 C10 C45 120.5(7) . . ? C12 C11 C10 177.5(8) . . ? C11 C12 C13 176.2(10) . . ? C14 C13 C12 173.5(10) . . ? C13 C14 C1 173.6(9) . 2_557 ? C1 C15 C16 108.5(9) . . ? C1 C15 C17 108.6(8) . . ? C1 C15 C18 110.2(8) . . ? C16 C15 C17 108.2(9) . . ? C18 C15 C16 112.5(8) . . ? C18 C15 C17 108.7(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C15 118.7(9) . . ? C19 C18 C23 118.6(11) . . ? C23 C18 C15 122.5(11) . . ? C18 C19 H19 118.1 . . ? C18 C19 C20 123.8(13) . . ? C20 C19 H19 118.1 . . ? C19 C20 H20 120.7 . . ? C21 C20 C19 118.6(16) . . ? C21 C20 H20 120.7 . . ? C20 C21 O24 120.7(15) . . ? C20 C21 C22 121.2(11) . . ? C22 C21 O24 118.1(12) . . ? C21 C22 H22 119.9 . . ? C21 C22 C23 120.3(10) . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 117.4(13) . . ? C18 C23 H23 121.3 . . ? C22 C23 H23 121.3 . . ? C26 C25 C3 107.6(8) . . ? C26 C25 C27 110.2(9) . . ? C27 C25 C3 107.9(8) . . ? C28 C25 C3 107.3(8) . . ? C28 C25 C26 111.4(8) . . ? C28 C25 C27 112.2(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C25 122.6(9) . . ? C29 C28 C33 118.8(9) . . ? C33 C28 C25 118.4(9) . . ? C28 C29 H29 119.3 . . ? C28 C29 C30 121.5(11) . . ? C30 C29 H29 119.3 . . ? C29 C30 H30 122.9 . . ? C29 C30 C31 114.2(12) . . ? C31 C30 H30 122.9 . . ? O34 C31 C30 112.7(12) . . ? C32 C31 O34 123.1(13) . . ? C32 C31 C30 123.1(11) . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.4(11) . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 121.8(10) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C8 C35 C36 111.6(10) . . ? C8 C35 C37 107.7(12) . . ? C8 C35 C38 108.7(10) . . ? C36 C35 C38 104.5(10) . . ? C37 C35 C36 111.9(12) . . ? C37 C35 C38 112.5(9) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C35 122.8(12) . . ? C39 C38 C43 117.0(11) . . ? C43 C38 C35 120.2(12) . . ? C38 C39 H39 118.2 . . ? C38 C39 C40 123.7(14) . . ? C40 C39 H39 118.2 . . ? C39 C40 H40 121.4 . . ? C41 C40 C39 117.3(14) . . ? C41 C40 H40 121.4 . . ? C40 C41 O44 118.8(13) . . ? C40 C41 C42 124.6(13) . . ? C42 C41 O44 116.5(15) . . ? C41 C42 H42 121.3 . . ? C41 C42 C43 117.3(15) . . ? C43 C42 H42 121.3 . . ? C38 C43 C42 120.1(13) . . ? C38 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C10 C45 C47 107.7(7) . . ? C10 C45 C48 111.0(7) . . ? C46 C45 C10 107.0(7) . . ? C46 C45 C47 108.6(7) . . ? C46 C45 C48 113.8(7) . . ? C48 C45 C47 108.7(7) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C45 119.4(8) . . ? C49 C48 C53 119.0(8) . . ? C53 C48 C45 121.6(8) . . ? C48 C49 H49 120.1 . . ? C48 C49 C50 119.9(10) . . ? C50 C49 H49 120.1 . . ? C49 C50 H50 120.0 . . ? C51 C50 C49 120.1(10) . . ? C51 C50 H50 120.0 . . ? C50 C51 O54 118.5(10) . . ? C52 C51 O54 120.8(9) . . ? C52 C51 C50 120.6(8) . . ? C51 C52 H52 120.1 . . ? C51 C52 C53 119.8(9) . . ? C53 C52 H52 120.1 . . ? C48 C53 C52 120.5(9) . . ? C48 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C56 C57 H57A 108.2 . . ? C56 C57 H57B 108.2 . . ? H57A C57 H57B 107.4 . . ? C58 C57 C56 116(3) . . ? C58 C57 H57A 108.2 . . ? C58 C57 H57B 108.2 . . ? C57 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C57 C58 C59 112(3) . . ? H58A C58 H58B 107.9 . . ? C59 C58 H58A 109.2 . . ? C59 C58 H58B 109.2 . . ? C58 C59 C58 116(4) . 2 ? C58 C59 H59A 108.3 . . ? C58 C59 H59A 108.3 2 . ? C58 C59 H59B 108.3 . . ? C58 C59 H59B 108.3 2 . ? H59A C59 H59B 107.4 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? C60 C61 H61A 111.0 . . ? C60 C61 H61B 111.0 . . ? C60 C61 C62 104(2) . . ? H61A C61 H61B 109.0 . . ? C62 C61 H61A 111.0 . . ? C62 C61 H61B 111.0 . . ? C61 C62 H62A 111.9 . . ? C61 C62 H62B 111.9 . . ? H62A C62 H62B 109.6 . . ? C63 C62 C61 100(2) . . ? C63 C62 H62A 111.9 . . ? C63 C62 H62B 111.9 . . ? C62 C63 C62 85(4) . 2 ? C62 C63 H63A 114.5 . . ? C62 C63 H63A 114.5 2 . ? C62 C63 H63B 114.5 . . ? C62 C63 H63B 114.5 2 . ? H63A C63 H63B 111.6 . . ? 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 O24 C21 C22 C23 -178.2(11) . . . . ? O34 C31 C32 C33 176.0(16) . . . . ? O44 C41 C42 C43 -179.0(10) . . . . ? O54 C51 C52 C53 179.1(9) . . . . ? C1 C2 C3 C4 23(18) . . . . ? C1 C2 C3 C25 -158(17) . . . . ? C1 C15 C18 C19 62.9(13) . . . . ? C1 C15 C18 C23 -121.3(11) . . . . ? C2 C1 C15 C16 -112.3(10) . . . . ? C2 C1 C15 C17 130.3(10) . . . . ? C2 C1 C15 C18 11.2(14) . . . . ? C2 C3 C4 C5 -108(44) . . . . ? C2 C3 C25 C26 125.9(9) . . . . ? C2 C3 C25 C27 7.0(11) . . . . ? C2 C3 C25 C28 -114.1(9) . . . . ? C3 C4 C5 C6 97(66) . . . . ? C3 C25 C28 C29 -127.0(12) . . . . ? C3 C25 C28 C33 57.5(12) . . . . ? C4 C3 C25 C26 -54.9(10) . . . . ? C4 C3 C25 C27 -173.7(7) . . . . ? C4 C3 C25 C28 65.1(9) . . . . ? C4 C5 C6 C7 -44(52) . . . . ? C5 C6 C7 C8 -8(68) . . . . ? C6 C7 C8 C9 -80(57) . . . . ? C6 C7 C8 C35 101(57) . . . . ? C7 C8 C9 C10 106(35) . . . . ? C7 C8 C35 C36 -179.5(10) . . . . ? C7 C8 C35 C37 -56.3(12) . . . . ? C7 C8 C35 C38 65.8(12) . . . . ? C8 C9 C10 C11 -17(35) . . . . ? C8 C9 C10 C45 158(34) . . . . ? C8 C35 C38 C39 24.3(14) . . . . ? C8 C35 C38 C43 -157.0(10) . . . . ? C9 C8 C35 C36 1.3(15) . . . . ? C9 C8 C35 C37 124.5(10) . . . . ? C9 C8 C35 C38 -113.4(9) . . . . ? C9 C10 C11 C12 -42(24) . . . . ? C9 C10 C45 C46 -108.1(10) . . . . ? C9 C10 C45 C47 135.3(9) . . . . ? C9 C10 C45 C48 16.5(12) . . . . ? C10 C11 C12 C13 64(31) . . . . ? C10 C45 C48 C49 62.5(12) . . . . ? C10 C45 C48 C53 -119.8(10) . . . . ? C11 C10 C45 C46 66.4(11) . . . . ? C11 C10 C45 C47 -50.2(10) . . . . ? C11 C10 C45 C48 -169.0(8) . . . . ? C11 C12 C13 C14 -15(21) . . . . ? C12 C13 C14 C1 -7(16) . . . 2_557 ? C14 C1 C2 C3 61(18) 2_557 . . . ? C14 C1 C15 C16 69.9(11) 2_557 . . . ? C14 C1 C15 C17 -47.5(12) 2_557 . . . ? C14 C1 C15 C18 -166.6(9) 2_557 . . . ? C15 C1 C2 C3 -117(17) . . . . ? C15 C18 C19 C20 177.9(11) . . . . ? C15 C18 C23 C22 -175.5(11) . . . . ? C16 C15 C18 C19 -175.9(11) . . . . ? C16 C15 C18 C23 -0.1(14) . . . . ? C17 C15 C18 C19 -56.1(13) . . . . ? C17 C15 C18 C23 119.7(12) . . . . ? C18 C19 C20 C21 -4(2) . . . . ? C19 C18 C23 C22 0.3(16) . . . . ? C19 C20 C21 O24 -179.7(12) . . . . ? C19 C20 C21 C22 3(2) . . . . ? C20 C21 C22 C23 -1(2) . . . . ? C21 C22 C23 C18 -0.8(18) . . . . ? C23 C18 C19 C20 1.9(18) . . . . ? C25 C3 C4 C5 72(44) . . . . ? C25 C28 C29 C30 176.9(16) . . . . ? C25 C28 C33 C32 179.6(10) . . . . ? C26 C25 C28 C29 -9.5(16) . . . . ? C26 C25 C28 C33 175.0(11) . . . . ? C27 C25 C28 C29 114.6(13) . . . . ? C27 C25 C28 C33 -60.9(13) . . . . ? C28 C29 C30 C31 11(3) . . . . ? C29 C28 C33 C32 3.9(18) . . . . ? C29 C30 C31 O34 179.8(19) . . . . ? C29 C30 C31 C32 -12(3) . . . . ? C30 C31 C32 C33 9(3) . . . . ? C31 C32 C33 C28 -5(2) . . . . ? C33 C28 C29 C30 -8(2) . . . . ? C35 C8 C9 C10 -74(35) . . . . ? C35 C38 C39 C40 -178.4(11) . . . . ? C35 C38 C43 C42 -179.4(10) . . . . ? C36 C35 C38 C39 -95.0(14) . . . . ? C36 C35 C38 C43 83.7(13) . . . . ? C37 C35 C38 C39 143.5(13) . . . . ? C37 C35 C38 C43 -37.8(17) . . . . ? C38 C39 C40 C41 -3(2) . . . . ? C39 C38 C43 C42 -0.6(17) . . . . ? C39 C40 C41 O44 -178.9(11) . . . . ? C39 C40 C41 C42 1(2) . . . . ? C40 C41 C42 C43 1(2) . . . . ? C41 C42 C43 C38 -1.3(17) . . . . ? C43 C38 C39 C40 2.8(18) . . . . ? C45 C10 C11 C12 144(23) . . . . ? C45 C48 C49 C50 178.2(10) . . . . ? C45 C48 C53 C52 -177.5(9) . . . . ? C46 C45 C48 C49 -176.9(10) . . . . ? C46 C45 C48 C53 0.9(13) . . . . ? C47 C45 C48 C49 -55.7(11) . . . . ? C47 C45 C48 C53 122.0(10) . . . . ? C48 C49 C50 C51 -1.8(18) . . . . ? C49 C48 C53 C52 0.3(15) . . . . ? C49 C50 C51 O54 -178.4(10) . . . . ? C49 C50 C51 C52 2.6(19) . . . . ? C50 C51 C52 C53 -1.9(17) . . . . ? C51 C52 C53 C48 0.4(15) . . . . ? C53 C48 C49 C50 0.3(16) . . . . ? C56 C57 C58 C59 94(5) . . . . ? C57 C58 C59 C58 155(4) . . . 2 ? C60 C61 C62 C63 47(5) . . . . ? C61 C62 C63 C62 -101(3) . . . 2 ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -2 0 0 24 0.96 -2 0 0 23.88 0.99 -2 0 0 23.61 1.01 2 0 0 23.25 0.96 2 0 0 23.66 0.98 2 0 0 23.25 1.01 -4 0 0 50.6 2.16 4 0 0 50.08 2.04 4 0 0 50.52 2.08 4 0 0 48.91 2.14 -4 0 0 50.33 2.1 -4 0 0 51.29 2.05 6 0 0 124.33 4.66 6 0 0 107.73 4.78 -6 0 0 113.36 4.68 -6 0 0 112.81 4.81 6 0 0 116.22 4.6 -6 0 0 116.12 4.61 8 0 0 105.27 4.14 -8 0 0 102.66 4.29 -8 0 0 96.28 4.06 8 0 0 100.69 4.07 8 0 0 98.5 4.25 -8 0 0 98.77 4.16 -10 0 0 0.64 0.31 10 0 0 0.84 0.38 -10 0 0 1.22 0.42 10 0 0 0.4 0.38 -10 0 0 0.81 0.16 12 0 0 1.89 0.54 -12 0 0 2.36 0.18 -12 0 0 1.99 0.43 12 0 0 1.84 0.18 14 0 0 29.07 1.57 -14 0 0 29.78 1.17 14 0 0 29.57 1.16 -16 0 0 0.39 0.17 16 0 0 0.21 0.16 -18 0 0 4.84 0.39 18 0 0 5.08 0.38 -20 0 0 3.41 0.31 -22 0 0 0.39 0.26 -24 0 0 0.38 0.26 1 -1 0 25.41 1.2 -1 -1 0 26.28 1.13 -1 -1 0 27.65 1.14 1 -1 0 28.04 1.2 1 -1 0 26.93 1.13 1 -1 0 26.47 1.13 -1 -1 0 27.05 1.2 -1 -1 0 26.56 1.19 1 1 0 26.74 1.13 -1 1 0 28.57 1.14 -1 1 0 27.19 1.14 1 1 0 27.82 1.15 1 1 0 27.49 1.21 -1 1 0 26.38 1.2 -1 1 0 27.18 1.21 3 -1 0 365.6 14.54 3 -1 0 337.67 15.02 -3 -1 0 375.36 14.54 3 -1 0 360.2 14.05 -3 -1 0 339.5 14.05 -3 -1 0 358.29 14.08 3 -1 0 357.96 14.06 -3 1 0 377.03 14.55 -3 1 0 370.58 15.03 -3 1 0 352.89 14.07 3 1 0 348.18 14.53 3 1 0 362.57 14.06 3 1 0 343.49 14.08 -3 1 0 367.62 14.06 -5 -1 0 978.12 38.56 -5 -1 0 967.25 37.35 5 -1 0 950.78 38.57 5 -1 0 924.99 37.3 -5 -1 0 991.24 37.31 5 -1 0 944.4 37.33 5 -1 0 880.5 39.88 5 1 0 981.35 37.31 5 1 0 1000 37.37 5 1 0 905.25 38.56 -5 1 0 975.38 37.37 -5 1 0 946.18 37.34 -5 1 0 951.79 38.56 -7 -1 0 87.54 3.57 -7 -1 0 90.65 3.75 -7 -1 0 89.54 3.65 7 -1 0 86.94 3.61 7 -1 0 88.42 3.58 7 -1 0 87.64 3.76 -7 1 0 88.86 3.57 -7 1 0 84.64 3.62 -7 1 0 87.72 3.74 7 1 0 86.37 3.66 7 1 0 86.82 3.75 7 1 0 88.41 3.58 -9 -1 0 34.29 1.52 -9 -1 0 35.6 1.69 9 -1 0 32.83 1.7 -9 -1 0 31.85 1.28 9 -1 0 35.72 1.58 9 1 0 31.8 1.65 -9 1 0 33.4 1.5 -9 1 0 33.69 1.68 9 1 0 35.04 1.65 9 1 0 32.31 1.51 -11 -1 0 13.13 0.82 -11 -1 0 11.96 0.56 11 -1 0 11.8 0.56 11 -1 0 13.14 0.9 -11 1 0 12.93 0.56 11 1 0 11.72 0.56 -11 1 0 12.56 0.76 11 1 0 13.74 0.96 -13 -1 0 4.08 0.35 13 -1 0 3.45 0.54 13 -1 0 3.38 0.35 13 1 0 3.63 0.34 -13 1 0 4.1 0.35 13 1 0 4.02 0.64 -15 -1 0 12.13 0.57 15 -1 0 11.97 0.57 -15 1 0 12.58 0.57 15 1 0 11.3 0.56 17 -1 0 7.95 0.46 -17 -1 0 7.65 0.45 17 1 0 7.57 0.46 -17 1 0 7.82 0.47 -19 -1 0 2.32 0.26 19 -1 0 1.89 0.24 -19 1 0 2.07 0.25 -21 -1 0 4.28 0.44 -21 1 0 4.67 0.44 -23 -1 0 1.29 0.28 -23 1 0 1.17 0.27 -25 -1 0 3.65 0.41 -25 1 0 3.39 0.33 0 -2 0 376.99 17.41 0 -2 0 415.35 16.88 0 -2 0 428.58 16.32 0 -2 0 430.31 16.31 0 2 0 440.99 16.33 0 2 0 419.43 17.42 0 2 0 395.41 16.3 2 -2 0 212.53 8.61 -2 -2 0 216.13 8.94 2 -2 0 210.01 9.19 2 -2 0 212.88 8.93 -2 -2 0 216.47 8.91 2 -2 0 227.18 8.62 -2 -2 0 220.29 8.61 -2 -2 0 213.96 8.63 2 2 0 211.19 8.61 -2 2 0 215.17 8.62 2 2 0 217.43 8.64 2 2 0 219.56 9.2 -2 2 0 230.77 9.21 -2 2 0 221.42 8.94 -2 2 0 221.65 8.62 -4 -2 0 340.72 13.45 -4 -2 0 330.33 13.03 -4 -2 0 328.77 12.99 4 -2 0 339.54 13.01 4 -2 0 335.23 13.47 4 -2 0 322.86 12.99 -4 2 0 343.02 13.01 -4 2 0 330.72 13.02 -4 2 0 343.19 13.9 4 2 0 289.49 12.99 4 2 0 318.46 13.45 4 2 0 328.84 13.05 -4 2 0 338.75 13.47 6 -2 0 41.57 1.93 6 -2 0 41.74 1.79 6 -2 0 39.28 1.76 -6 -2 0 40.74 1.76 -6 -2 0 42.44 1.9 6 2 0 39.32 1.78 6 2 0 37.96 1.9 6 2 0 38.56 1.86 -6 2 0 42.93 1.93 -6 2 0 41.81 1.78 -6 2 0 44.46 1.97 -8 -2 0 124.14 4.69 -8 -2 0 130.93 5.12 8 -2 0 128.09 5.15 8 -2 0 127.83 5.38 8 -2 0 120.36 4.68 -8 2 0 130.47 5.13 8 2 0 121.26 5.13 -8 2 0 134.33 5.38 8 2 0 123.76 5.36 8 2 0 133.1 5.26 -8 2 0 119.52 4.68 -10 -2 0 8.1 0.62 10 -2 0 6.62 0.41 -10 -2 0 7.39 0.73 10 -2 0 6.69 0.65 -10 -2 0 6.22 0.4 10 2 0 8.26 0.84 -10 2 0 6.54 0.38 -10 2 0 6.77 0.59 12 -2 0 25.73 1.42 -12 -2 0 28.15 1.08 12 -2 0 28.06 1.08 12 2 0 26.54 1.57 12 2 0 26.47 1.07 -12 2 0 27.97 1.07 -12 2 0 26.22 1.36 14 -2 0 31.06 1.17 -14 -2 0 30.56 1.16 14 2 0 23.96 1.62 14 2 0 28.49 1.15 -14 2 0 30.35 1.16 -16 -2 0 5.45 0.39 16 -2 0 5.33 0.41 16 2 0 4.84 0.37 -16 2 0 4.96 0.37 18 -2 0 4.77 0.42 -18 -2 0 5.14 0.42 -18 2 0 5.24 0.4 -20 -2 0 2.86 0.3 20 -2 0 2.72 0.28 -20 2 0 2.82 0.29 -22 -2 0 3.2 0.34 -22 2 0 3.47 0.33 -24 -2 0 1.56 0.29 -24 2 0 1.51 0.27 1 -3 0 4.62 0.45 -1 -3 0 5.17 0.49 -1 -3 0 4.12 0.49 -1 -3 0 4.8 0.45 1 -3 0 3.64 0.47 1 3 0 3.97 0.44 1 3 0 4.56 0.55 -1 3 0 4.35 0.53 1 3 0 5.01 0.51 -1 3 0 5.01 0.49 -1 3 0 3.99 0.47 -1 3 0 3.18 0.46 3 -3 0 3.05 0.38 -3 -3 0 3.36 0.39 -3 -3 0 3.15 0.47 -3 -3 0 3.22 0.24 3 -3 0 2.92 0.44 3 3 0 2.95 0.37 3 3 0 3.42 0.47 -3 3 0 2.52 0.36 -3 3 0 2.81 0.45 -3 3 0 3.38 0.42 -3 3 0 3.16 0.4 3 3 0 3.2 0.44 5 -3 0 12.76 0.57 -5 -3 0 12.66 0.56 5 -3 0 13.12 0.78 -5 -3 0 13.96 0.93 5 -3 0 14.03 1.01 -5 -3 0 13.18 1.01 -5 -3 0 12.78 0.75 -5 3 0 13.18 0.88 5 3 0 14.76 0.91 -5 3 0 13.99 0.98 5 3 0 13.35 0.91 5 3 0 12.07 0.8 -5 3 0 13.49 0.78 7 -3 0 5.37 0.35 -7 -3 0 5.69 0.64 -7 -3 0 5.07 0.35 -7 -3 0 4.84 0.53 -7 3 0 6.89 0.75 7 3 0 5.58 0.7 -7 3 0 5.3 0.55 7 3 0 5.63 0.63 -7 3 0 4.94 0.33 9 -3 0 54.89 2.44 -9 -3 0 54.35 2.59 -9 -3 0 56.5 2.06 9 -3 0 52.89 2.06 -9 3 0 53.76 2.06 9 3 0 54.24 2.59 -9 3 0 56.53 2.66 -9 3 0 54.29 2.42 11 -3 0 16.6 0.71 -11 -3 0 17.09 0.72 11 3 0 16.81 1.23 -11 3 0 16.19 0.7 -13 -3 0 19.04 0.78 13 -3 0 18.71 0.77 -13 3 0 19.43 0.77 13 3 0 16.3 0.76 -15 -3 0 4.42 0.36 15 -3 0 4.15 0.35 -15 3 0 4.06 0.34 17 -3 0 4.18 0.39 -17 -3 0 4.52 0.4 -17 3 0 4.17 0.38 19 -3 0 0.27 0.21 -19 -3 0 0.24 0.24 -19 3 0 0.54 0.22 -21 -3 0 2.67 0.31 -21 3 0 2.46 0.3 -23 -3 0 -0.02 0.25 -23 3 0 -0.11 0.24 0 -4 0 16.69 0.69 0 -4 0 16.45 1.15 0 -4 0 16.53 0.96 0 4 0 15.18 1.03 0 4 0 18.06 1.08 -2 -4 0 6.06 0.67 2 -4 0 5.76 0.59 2 -4 0 5.71 0.35 -2 -4 0 5.75 0.59 -2 4 0 6 0.71 2 4 0 6.47 0.72 -2 4 0 6.3 0.68 2 4 0 7.62 0.77 -4 -4 0 50.96 2.4 4 -4 0 50.34 2.24 -4 -4 0 49.65 1.9 4 -4 0 49.85 1.9 -4 4 0 50.66 2.28 4 4 0 50.52 2.41 4 4 0 48.28 2.33 -4 4 0 51.96 2.41 -6 -4 0 34.22 1.28 6 -4 0 32.67 1.28 6 4 0 35.09 1.78 -6 4 0 30.36 1.62 6 4 0 33.33 1.76 -6 4 0 33.21 1.75 -8 -4 0 9.38 0.47 8 -4 0 8.9 0.47 8 4 0 9 0.87 -8 4 0 8.47 0.91 8 4 0 9.29 0.94 -8 4 0 8.25 0.72 10 -4 0 12.7 0.57 -10 -4 0 12.26 0.56 10 4 0 11.01 0.99 10 4 0 11.19 1.08 -12 -4 0 9.64 0.5 12 -4 0 10.15 0.51 -12 4 0 9.74 0.49 14 -4 0 1.26 0.2 -14 -4 0 1.37 0.22 -14 4 0 1.38 0.19 -16 -4 0 2.4 0.26 16 -4 0 2 0.24 -16 4 0 1.95 0.24 -18 -4 0 2.67 0.3 18 -4 0 2.65 0.28 -18 4 0 3.14 0.29 20 -4 0 5.99 0.46 -20 -4 0 6.61 0.46 -20 4 0 5.54 0.46 -22 -4 0 5.28 0.42 1 -5 0 9.82 0.47 -1 -5 0 10.24 0.47 -1 5 0 9.49 0.84 -1 5 0 7.42 0.82 1 5 0 8.39 0.87 1 5 0 9.07 0.86 3 -5 0 19.38 0.77 -3 -5 0 20.67 0.78 -3 5 0 16.35 1.16 3 5 0 15.42 1.21 -3 5 0 18.36 1.2 3 5 0 18.36 1.21 -5 -5 0 11.18 0.51 5 -5 0 10.31 0.51 5 5 0 10.92 0.96 -5 5 0 10.14 0.91 -7 -5 0 5 0.36 7 -5 0 5.41 0.36 7 5 0 3.75 0.69 -9 -5 0 4.32 0.38 9 -5 0 4.11 0.35 -11 -5 0 7.5 0.44 11 -5 0 6.6 0.42 -13 -5 0 0.73 0.21 13 -5 0 0.72 0.19 15 -5 0 0.78 0.21 -15 -5 0 0.53 0.22 17 -5 0 11.02 0.57 -17 -5 0 10.51 0.59 -19 -5 0 2.48 0.3 19 -5 0 2.34 0.27 -21 -5 0 1.22 0.26 0 -6 0 1.08 0.19 -2 -6 0 1.99 0.21 2 -6 0 1.83 0.21 -4 -6 0 3.54 0.35 4 -6 0 3.77 0.36 6 -6 0 6.11 0.4 -6 -6 0 5.8 0.4 -8 -6 0 4.35 0.4 8 -6 0 4.93 0.38 10 -6 0 6.94 0.43 -10 -6 0 6.9 0.46 12 -6 0 16.47 0.75 -12 -6 0 16.97 0.77 -14 -6 0 8.3 0.53 14 -6 0 9.65 0.52 -16 -6 0 2.37 0.29 16 -6 0 2.64 0.27 -18 -6 0 0.91 0.25 18 -6 0 1.1 0.23 -1 -7 0 -0.09 0.22 1 -7 0 0.03 0.21 -3 -7 0 1.59 0.26 3 -7 0 1.63 0.25 5 -7 0 1.26 0.25 -5 -7 0 1.2 0.25 -7 -7 0 3.77 0.41 7 -7 0 4.23 0.41 -9 -7 0 10.57 0.58 9 -7 0 11.04 0.57 11 -7 0 13.87 0.65 -11 -7 0 13.56 0.67 -13 -7 0 3.85 0.39 13 -7 0 4.45 0.39 15 -7 0 1.69 0.25 -15 -7 0 1.48 0.26 0 -8 0 0.56 0.25 2 -8 0 2.36 0.29 -2 -8 0 1.89 0.28 4 -8 0 3.12 0.3 -4 -8 0 3.05 0.31 -6 -8 0 2.91 0.32 6 -8 0 3.86 0.38 -8 -8 0 3.48 0.38 8 -8 0 4.05 0.39 10 -8 0 2.11 0.28 -10 -8 0 2.16 0.28 -26 0 1 0.94 0.26 -24 0 1 13.73 0.69 22 0 -1 4.77 0.44 -22 0 1 4.72 0.45 -20 0 1 0.36 0.22 20 0 -1 0.36 0.22 18 0 -1 3.82 0.37 -18 0 1 4.68 0.38 16 0 -1 6.52 0.43 -16 0 1 5.96 0.42 14 0 -1 4.89 0.66 -14 0 1 5.45 0.38 14 0 -1 5.26 0.38 12 0 -1 0.35 0.47 -12 0 1 0.34 0.39 12 0 -1 0.32 0.14 -12 0 1 0.76 0.18 -10 0 1 82.31 3.65 10 0 -1 79.43 3.6 10 0 -1 87.33 3.52 -10 0 1 83.93 3.45 8 0 -1 18.38 0.89 8 0 -1 16.39 0.95 -8 0 1 18.38 1.1 8 0 -1 18.43 1.05 -8 0 1 19.25 0.91 -8 0 1 18.34 1.04 6 0 -1 4.65 0.48 -6 0 1 4.66 0.52 6 0 -1 5.68 0.42 6 0 -1 4.79 0.44 -6 0 1 5.41 0.48 -6 0 1 6.02 0.43 4 0 -1 8.64 0.53 4 0 -1 7.54 0.42 -4 0 1 8.69 0.5 -4 0 1 8.06 0.44 -4 0 1 7.98 0.54 4 0 -1 9.25 0.49 -2 0 1 29.43 1.26 -2 0 1 31.42 1.21 2 0 -1 29.11 1.22 2 0 -1 29.59 1.26 2 0 -1 30.78 1.21 -2 0 1 29.23 1.23 0 0 -1 112.14 4.7 0 0 1 111.72 4.7 2 0 1 6.13 0.32 2 0 1 6.69 0.4 2 0 1 7.2 0.36 -2 0 -1 6.23 0.31 -2 0 -1 6.53 0.39 2 0 1 6.1 0.43 4 0 1 244.35 9.5 -4 0 -1 238.62 9.54 -4 0 -1 243.7 9.84 4 0 1 252.41 9.54 -4 0 -1 238.15 9.49 4 0 1 231.02 9.83 -6 0 -1 0.07 0.31 -6 0 -1 0.41 0.34 -6 0 -1 0.23 0.22 6 0 1 -0.13 0.28 6 0 1 0.23 0.3 6 0 1 0.3 0.23 -8 0 -1 8.46 0.56 8 0 1 8.22 0.55 8 0 1 8.28 0.63 8 0 1 8.45 0.78 -10 0 -1 12.61 1.03 -10 0 -1 12.43 0.56 10 0 1 13.65 0.87 -10 0 -1 13.34 0.77 10 0 1 11.57 0.75 -12 0 -1 28.75 1.11 -12 0 -1 27.85 1.66 12 0 1 29.21 1.51 12 0 1 27.82 1.12 14 0 1 0.14 0.46 14 0 1 0.08 0.15 -14 0 -1 -0.06 0.15 16 0 1 1.89 0.2 -16 0 -1 1.84 0.21 -18 0 -1 18.5 0.81 -20 0 -1 3.47 0.39 -22 0 -1 11.55 0.61 -24 0 -1 4.55 0.42 -25 -1 1 3.03 0.32 -25 1 1 2.88 0.31 -23 -1 1 8.28 0.53 -23 1 1 7.47 0.52 -21 -1 1 2.22 0.28 21 -1 -1 1.79 0.26 -21 1 1 1.9 0.27 21 1 -1 2.23 0.27 -19 -1 1 1.66 0.24 19 -1 -1 1.47 0.23 19 1 -1 1.64 0.23 -19 1 1 1.67 0.23 -17 -1 1 2.91 0.24 17 -1 -1 2.55 0.23 17 1 -1 2.42 0.22 -17 1 1 2.24 0.22 -15 -1 1 11.06 0.55 15 -1 -1 11.22 0.53 -15 1 1 11.09 0.53 15 1 -1 9.93 0.52 -13 -1 1 43.85 1.64 13 -1 -1 42.71 2.02 -13 -1 1 42.33 1.97 13 -1 -1 43.98 1.63 -13 1 1 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-18 0.73 0.19 13 -3 -18 1.18 0.24 13 3 -18 0.54 0.22 11 -3 -18 4.25 0.47 11 -3 -18 3.87 0.33 11 -3 -18 3.76 0.36 11 3 -18 3.2 0.47 9 -3 -18 1.06 0.24 9 -3 -18 1.06 0.21 9 -3 -18 1.05 0.2 9 3 -18 0.78 0.23 7 -3 -18 1.25 0.25 7 -3 -18 1.25 0.21 7 -3 -18 1.64 0.23 7 3 -18 1.06 0.24 5 -3 -18 1.53 0.26 5 -3 -18 1.55 0.22 5 -3 -18 1.94 0.24 3 -3 -18 2.65 0.31 3 -3 -18 1.46 0.27 3 3 -18 1.62 0.28 1 -3 -18 2.24 0.3 12 -4 -18 0.01 0.16 12 -4 -18 0.1 0.17 10 -4 -18 1.07 0.2 10 -4 -18 1.45 0.21 8 -4 -18 0.96 0.21 8 -4 -18 0.86 0.19 6 -4 -18 1.3 0.22 6 -4 -18 1.03 0.2 4 -4 -18 -0.09 0.18 18 0 -19 12.01 0.7 18 0 -19 8.89 0.62 16 0 -19 -0.08 0.22 16 0 -19 -0.33 0.18 14 0 -19 0.56 0.23 14 0 -19 0.02 0.19 12 0 -19 3.08 0.44 12 0 -19 2.76 0.36 12 0 -19 2.55 0.29 10 0 -19 -0.35 0.21 10 0 -19 -0.05 0.19 10 0 -19 0.33 0.22 8 0 -19 4.8 0.43 8 0 -19 5.46 0.44 8 0 -19 5.98 0.52 6 0 -19 4.02 0.45 6 0 -19 3.4 0.37 6 0 -19 2.91 0.37 4 0 -19 1.21 0.23 4 0 -19 0.78 0.21 4 0 -19 1.61 0.26 2 0 -19 3.15 0.31 2 0 -19 3.74 0.46 0 0 -19 0.14 0.24 19 -1 -19 0.75 0.24 19 1 -19 0.48 0.2 17 -1 -19 0 0.18 17 -1 -19 0.52 0.23 17 1 -19 0.68 0.22 15 -1 -19 7.65 0.52 15 -1 -19 9.06 0.61 15 1 -19 8.39 0.6 15 1 -19 6.87 0.53 13 -1 -19 2.45 0.26 13 -1 -19 2.01 0.27 13 -1 -19 3.09 0.43 13 1 -19 2.04 0.27 13 1 -19 3 0.44 11 -1 -19 1.47 0.27 11 -1 -19 0.96 0.21 11 -1 -19 0.69 0.21 11 1 -19 0.74 0.22 11 1 -19 1.27 0.27 9 -1 -19 3.3 0.35 9 -1 -19 3.4 0.37 9 -1 -19 4.05 0.47 9 1 -19 3.1 0.38 9 1 -19 4.12 0.47 9 1 -19 2.57 0.33 7 -1 -19 0.74 0.21 7 -1 -19 1.14 0.24 7 -1 -19 0.96 0.21 7 1 -19 1.23 0.25 7 1 -19 0.47 0.22 7 1 -19 0.39 0.24 5 -1 -19 2.61 0.32 5 -1 -19 2.29 0.26 5 -1 -19 2.85 0.31 5 1 -19 2.36 0.3 5 1 -19 2.87 0.31 3 -1 -19 0.42 0.19 3 -1 -19 0.76 0.24 3 -1 -19 -0.13 0.18 3 1 -19 0.82 0.25 1 -1 -19 0.56 0.24 1 -1 -19 0.38 0.19 1 1 -19 0.22 0.25 18 -2 -19 1.94 0.27 16 -2 -19 0.91 0.2 16 -2 -19 1.43 0.26 16 2 -19 0.83 0.22 14 -2 -19 1.59 0.23 14 -2 -19 1.58 0.24 14 -2 -19 2.39 0.29 14 2 -19 2.33 0.3 12 -2 -19 0.5 0.19 12 -2 -19 0.79 0.24 12 -2 -19 0.36 0.19 12 2 -19 0.66 0.22 10 -2 -19 0.42 0.18 10 -2 -19 0.66 0.19 10 -2 -19 0.32 0.23 10 2 -19 0.38 0.22 8 -2 -19 1.84 0.24 8 -2 -19 2.29 0.25 8 -2 -19 2.41 0.3 8 2 -19 2.23 0.3 6 -2 -19 1.16 0.25 6 -2 -19 1.44 0.22 6 -2 -19 0.85 0.2 6 2 -19 1.03 0.26 4 -2 -19 2.88 0.31 4 -2 -19 2.41 0.26 4 -2 -19 3.4 0.33 4 2 -19 3.34 0.35 2 -2 -19 0.26 0.18 2 -2 -19 -0.2 0.23 15 -3 -19 3.38 0.43 13 -3 -19 2.41 0.29 13 -3 -19 3.42 0.43 13 -3 -19 3.07 0.32 13 3 -19 2.18 0.28 11 -3 -19 1.3 0.25 11 -3 -19 1.4 0.21 11 -3 -19 1.07 0.2 11 3 -19 0.67 0.22 9 -3 -19 2.21 0.29 9 -3 -19 2.01 0.24 9 -3 -19 2.03 0.27 9 3 -19 1.59 0.26 7 -3 -19 -0.18 0.17 7 -3 -19 -0.41 0.16 5 -3 -19 1.14 0.24 5 -3 -19 1.78 0.22 5 3 -19 1.36 0.26 16 0 -20 -0.06 0.22 14 0 -20 -0.06 0.22 12 0 -20 0.16 0.19 12 0 -20 0.46 0.24 10 0 -20 9.66 0.62 10 0 -20 7.72 0.53 10 0 -20 6.9 0.51 8 0 -20 5.77 0.48 8 0 -20 4.7 0.42 8 0 -20 4.72 0.41 6 0 -20 -0.24 0.2 4 0 -20 7.3 0.53 4 0 -20 9.58 0.62 15 -1 -20 0.98 0.2 15 1 -20 0.25 0.22 15 1 -20 1.7 0.26 13 -1 -20 0.44 0.23 13 -1 -20 1.12 0.21 13 1 -20 0.77 0.22 13 1 -20 1.5 0.27 11 -1 -20 1.09 0.25 11 -1 -20 0.57 0.22 11 -1 -20 0.65 0.2 11 1 -20 1.13 0.26 11 1 -20 0.28 0.22 9 -1 -20 1.44 0.24 9 -1 -20 2 0.28 9 -1 -20 1.47 0.23 9 1 -20 2.08 0.28 7 -1 -20 0.52 0.21 7 -1 -20 0.84 0.23 7 -1 -20 0.26 0.18 7 1 -20 0.74 0.24 5 -1 -20 0.36 0.2 5 -1 -20 0.64 0.23 5 1 -20 0.68 0.24 3 -1 -20 0.91 0.24 3 1 -20 1.04 0.26 12 -2 -20 1.73 0.23 12 -2 -20 2.66 0.3 12 2 -20 1.85 0.26 10 -2 -20 0.61 0.2 10 -2 -20 0.89 0.23 10 -2 -20 0.64 0.19 10 2 -20 0.68 0.22 8 -2 -20 0.46 0.19 8 -2 -20 0.46 0.21 8 2 -20 0.43 0.21 6 -2 -20 0.84 0.23 6 2 -20 0.84 0.23 _shelx_res_file ; TITL cu_d050412_0m in C2 CELL 1.54178 27.9297 8.977 20.9383 90 111.19 90 ZERR 2 0.0027 0.0009 0.0015 0 0.006 0 LATT -7 SYMM -X,+Y,-Z SFAC C H Cl O UNIT 216 212 4 16 DFIX 1.53 C61 C60 C62 C61 C63 C62 DFIX 1.53 C57 C56 DFIX 1.53 C57 C58 DFIX 1.53 C58 C59 DFIX 1.77 Cl1 C55 Cl2 C55 DANG 2.45 C60 C62 C61 C63 DANG 2.45 C56 C58 DANG 2.45 C57 C59 DANG 2.93 Cl1 Cl2 L.S. 10 PLAN -8 0 0 SIZE 0.02 0.08 0.12 TEMP -173.16 BOND $H conf htab fmap 2 acta MERG 3 REM D:/SMoCC_Strukturen/d050412/work/cu_d050412_0m.hkl WGHT 0.200000 FVAR 0.09675 PART -1 CL1 3 0.061605 0.341562 1.489594 10.50000 0.27386 0.20237 = 0.22689 -0.01654 0.13863 -0.02383 CL2 3 0.001798 0.563657 1.524611 10.50000 0.40833 C55 1 0.008657 0.462980 1.454371 10.50000 0.29093 AFIX 23 1.0900 H55A 2 -0.026095 0.399600 1.427445 10.50000 -1.20000 H55B 2 0.015551 0.539723 1.418276 10.50000 -1.20000 AFIX 0 PART 0 O24 4 -0.164183 0.414874 0.474176 11.00000 0.21609 0.11867 = 0.08108 -0.01917 0.09078 -0.01128 AFIX 147 0.9801 H24 2 -0.143823 0.323055 0.483803 11.00000 -1.50000 AFIX 0 O34 4 -0.092219 0.859007 0.454035 11.00000 0.27200 0.21136 = 0.05287 -0.03865 0.07899 -0.12647 AFIX 147 0.9801 H34 2 -0.121912 0.817110 0.417258 11.00000 -1.50000 AFIX 0 O44 4 0.054571 0.104766 0.570177 11.00000 0.15072 0.14107 = 0.09248 -0.01964 0.06675 -0.02343 AFIX 147 0.9801 H44 2 0.070904 0.009587 0.567416 11.00000 -1.50000 AFIX 0 O54 4 0.138555 0.605262 0.605666 11.00000 0.11040 0.11868 = 0.04127 -0.00169 0.02923 -0.00033 AFIX 147 0.9801 H54 2 0.152345 0.521706 0.587547 11.00000 -1.50000 AFIX 0 C1 1 -0.200191 0.625051 0.749624 11.00000 0.04449 0.05627 = 0.03270 0.00073 0.01626 0.00469 C2 1 -0.163302 0.700886 0.741016 11.00000 0.03683 0.06556 = 0.03051 -0.00474 0.00819 0.00477 C3 1 -0.123784 0.774247 0.734714 11.00000 0.04822 0.07689 = 0.03748 -0.00488 0.01987 -0.01016 C4 1 -0.075725 0.696806 0.757184 11.00000 0.04374 0.09740 = 0.04391 -0.00389 0.01742 -0.00250 C5 1 -0.035985 0.635611 0.776855 11.00000 0.04377 0.11029 = 0.04810 0.00973 0.01873 0.01086 C6 1 0.011610 0.558526 0.801530 11.00000 0.06099 0.11940 = 0.05184 -0.01720 0.02930 -0.01704 C7 1 0.052410 0.490542 0.827751 11.00000 0.02549 0.13593 = 0.06102 0.00110 0.01450 0.01571 C8 1 0.097056 0.416121 0.858076 11.00000 0.04746 0.10673 = 0.04029 -0.01038 0.01393 -0.00987 C9 1 0.140697 0.493785 0.893505 11.00000 0.05751 0.09241 = 0.05983 0.01360 0.03891 0.02408 C10 1 0.182183 0.566286 0.929035 11.00000 0.02699 0.06599 = 0.04654 -0.00590 0.00944 0.00039 C11 1 0.192146 0.589169 0.999743 11.00000 0.05808 0.05886 = 0.04414 0.00348 0.02493 0.00594 C12 1 0.198559 0.609572 1.058535 11.00000 0.06128 0.06122 = 0.03824 0.00460 0.02638 0.01091 C13 1 0.203957 0.625229 1.126569 11.00000 0.05854 0.05806 = 0.06296 0.00205 0.03358 0.00304 C14 1 0.204598 0.629435 1.185405 11.00000 0.05949 0.06536 = 0.05091 -0.00659 0.03079 -0.00252 C15 1 -0.237862 0.527518 0.694746 11.00000 0.07620 0.06986 = 0.05086 -0.00081 0.03572 -0.01646 C16 1 -0.291636 0.599099 0.672893 11.00000 0.05207 0.11812 = 0.09757 -0.03119 0.02328 -0.02598 AFIX 137 1.0899 H16A 2 -0.303954 0.603018 0.716675 11.00000 -1.50000 H16B 2 -0.318821 0.532988 0.632160 11.00000 -1.50000 H16C 2 -0.290116 0.711851 0.654410 11.00000 -1.50000 AFIX 0 C17 1 -0.240285 0.371713 0.726368 11.00000 0.15534 0.06653 = 0.09351 -0.02183 0.08589 -0.03175 AFIX 137 1.0899 H17A 2 -0.202375 0.320328 0.743509 11.00000 -1.50000 H17B 2 -0.267552 0.301115 0.687853 11.00000 -1.50000 H17C 2 -0.252622 0.384795 0.769844 11.00000 -1.50000 AFIX 0 C18 1 -0.219568 0.507088 0.634045 11.00000 0.08874 0.06757 = 0.05767 -0.00150 0.02985 -0.02172 C19 1 -0.173712 0.436022 0.645315 11.00000 0.14291 0.06858 = 0.06483 -0.00292 0.06742 -0.00353 AFIX 43 1.0800 H19 2 -0.151561 0.400476 0.696853 11.00000 -1.20000 AFIX 0 C20 1 -0.153715 0.406537 0.593157 11.00000 0.21308 0.06870 = 0.11322 0.00818 0.12441 0.01272 AFIX 43 1.0800 H20 2 -0.116338 0.356161 0.605417 11.00000 -1.20000 AFIX 0 C21 1 -0.182361 0.442741 0.527990 11.00000 0.16003 0.07890 = 0.06300 -0.00933 0.05993 -0.02065 C22 1 -0.229651 0.514437 0.512002 11.00000 0.10602 0.13298 = 0.03208 -0.01793 0.02214 -0.03951 AFIX 43 1.0800 H22 2 -0.251660 0.543931 0.459540 11.00000 -1.20000 AFIX 0 C23 1 -0.249661 0.550044 0.566497 11.00000 0.11137 0.08709 = 0.06653 -0.01362 0.02185 -0.04380 AFIX 43 1.0800 H23 2 -0.285903 0.606740 0.555186 11.00000 -1.20000 AFIX 0 C25 1 -0.125110 0.930170 0.705440 11.00000 0.05599 0.07614 = 0.04923 -0.01149 0.01293 -0.02243 C26 1 -0.084062 1.021966 0.758519 11.00000 0.09497 0.10560 = 0.06160 -0.02837 0.04433 -0.04160 AFIX 137 1.0899 H26A 2 -0.093764 1.033675 0.804228 11.00000 -1.50000 H26B 2 -0.081914 1.131849 0.737575 11.00000 -1.50000 H26C 2 -0.047055 0.966239 0.771839 11.00000 -1.50000 AFIX 0 C27 1 -0.178105 0.996089 0.692771 11.00000 0.07161 0.05405 = 0.07762 -0.00527 0.02966 -0.00910 AFIX 137 1.0899 H27A 2 -0.207464 0.922726 0.658941 11.00000 -1.50000 H27B 2 -0.180914 1.105309 0.668949 11.00000 -1.50000 H27C 2 -0.183797 1.007327 0.741372 11.00000 -1.50000 AFIX 0 C28 1 -0.114167 0.914844 0.640040 11.00000 0.06834 0.07272 = 0.04283 -0.00444 0.02248 -0.01874 C29 1 -0.076760 0.993627 0.628214 11.00000 0.13170 0.14760 = 0.06281 -0.01492 0.04718 -0.07730 AFIX 43 1.0800 H29 2 -0.054964 1.074640 0.665544 11.00000 -1.20000 AFIX 0 C30 1 -0.065583 0.971902 0.567665 11.00000 0.22589 0.20678 = 0.11247 -0.07670 0.11161 -0.15429 AFIX 43 1.0800 H30 2 -0.032108 1.018584 0.560856 11.00000 -1.20000 AFIX 0 C31 1 -0.104493 0.878162 0.513921 11.00000 0.19548 0.13914 = 0.06308 -0.02420 0.07933 -0.07650 C32 1 -0.138925 0.803967 0.525371 11.00000 0.08619 0.09392 = 0.05705 -0.01146 0.02468 -0.02354 AFIX 43 1.0800 H32 2 -0.162447 0.726459 0.487563 11.00000 -1.20000 AFIX 0 C33 1 -0.146403 0.823045 0.587732 11.00000 0.07985 0.08018 = 0.05134 -0.00068 0.01836 -0.01331 AFIX 43 1.0800 H33 2 -0.177769 0.765621 0.595688 11.00000 -1.20000 AFIX 0 C35 1 0.097472 0.248743 0.851042 11.00000 0.06044 0.11244 = 0.05822 -0.00158 0.00950 -0.02299 C36 1 0.151381 0.183475 0.889389 11.00000 0.11858 0.08090 = 0.09953 0.01142 -0.03757 -0.01605 AFIX 137 1.0899 H36A 2 0.178403 0.229064 0.867804 11.00000 -1.50000 H36B 2 0.150039 0.062636 0.883961 11.00000 -1.50000 H36C 2 0.163779 0.212622 0.943489 11.00000 -1.50000 AFIX 0 C37 1 0.057652 0.185295 0.877532 11.00000 0.12462 0.16008 = 0.08914 -0.03502 0.05827 -0.06222 AFIX 137 1.0899 H37A 2 0.059548 0.244741 0.923773 11.00000 -1.50000 H37B 2 0.065414 0.067448 0.889254 11.00000 -1.50000 H37C 2 0.019467 0.198245 0.838543 11.00000 -1.50000 AFIX 0 C38 1 0.086001 0.209657 0.775472 11.00000 0.04008 0.10840 = 0.07603 -0.00899 0.00947 -0.00444 C39 1 0.095387 0.307079 0.730107 11.00000 0.08478 0.15734 = 0.04955 -0.02073 0.03348 -0.03519 AFIX 43 1.0800 H39 2 0.112377 0.413799 0.749282 11.00000 -1.20000 AFIX 0 C40 1 0.084169 0.275232 0.661263 11.00000 0.08113 0.11797 = 0.10089 -0.00503 0.04200 -0.03711 AFIX 43 1.0800 H40 2 0.090410 0.356379 0.626990 11.00000 -1.20000 AFIX 0 C41 1 0.065586 0.141829 0.639484 11.00000 0.09637 0.12407 = 0.08154 0.00518 0.06135 -0.00255 C42 1 0.056080 0.034004 0.679660 11.00000 0.10208 0.10979 = 0.10955 -0.01693 0.05095 0.01803 AFIX 43 1.0800 H42 2 0.041495 -0.074147 0.659154 11.00000 -1.20000 AFIX 0 C43 1 0.066290 0.070552 0.750175 11.00000 0.09508 0.10352 = 0.08285 -0.00536 0.04347 0.00073 AFIX 43 1.0800 H43 2 0.058643 -0.010127 0.783552 11.00000 -1.20000 AFIX 0 C45 1 0.221675 0.613809 0.897471 11.00000 0.05554 0.06182 = 0.04057 0.00731 0.02326 0.00687 C46 1 0.268255 0.515938 0.928752 11.00000 0.04108 0.08672 = 0.05221 0.00921 0.01884 0.00916 AFIX 137 1.0899 H46A 2 0.283147 0.529743 0.984219 11.00000 -1.50000 H46B 2 0.297710 0.547513 0.908538 11.00000 -1.50000 H46C 2 0.257551 0.399873 0.916091 11.00000 -1.50000 AFIX 0 C47 1 0.237142 0.777522 0.919226 11.00000 0.06675 0.07354 = 0.04594 -0.00266 0.02117 0.00066 AFIX 137 1.0899 H47A 2 0.203251 0.848494 0.900231 11.00000 -1.50000 H47B 2 0.265349 0.814508 0.897790 11.00000 -1.50000 H47C 2 0.253683 0.784463 0.974926 11.00000 -1.50000 AFIX 0 C48 1 0.198432 0.606279 0.818782 11.00000 0.05316 0.06883 = 0.04474 0.00195 0.02110 0.00842 C49 1 0.157804 0.694773 0.784319 11.00000 0.07919 0.08622 = 0.04988 -0.00012 0.02810 0.01707 AFIX 43 1.0800 H49 2 0.141382 0.767158 0.812183 11.00000 -1.20000 AFIX 0 C50 1 0.137373 0.691928 0.712953 11.00000 0.07128 0.09939 = 0.05401 0.01691 0.00650 0.01744 AFIX 43 1.0800 H50 2 0.104403 0.759796 0.685547 11.00000 -1.20000 AFIX 0 C51 1 0.159230 0.602452 0.677242 11.00000 0.06896 0.09397 = 0.03880 0.00010 0.02001 0.01037 C52 1 0.198475 0.514314 0.710209 11.00000 0.06900 0.07563 = 0.04963 -0.00286 0.03502 -0.00809 AFIX 43 1.0800 H52 2 0.214558 0.442213 0.681839 11.00000 -1.20000 AFIX 0 C53 1 0.219016 0.514936 0.781884 11.00000 0.05663 0.06451 = 0.05742 0.00251 0.03211 0.00275 AFIX 43 1.0800 H53 2 0.251172 0.443647 0.808660 11.00000 -1.20000 AFIX 0 PART 1 C56 1 0.124001 0.271331 0.101152 10.50000 0.10465 AFIX 137 1.0899 H56A 2 0.123038 0.279815 0.048774 10.50000 -1.50000 H56B 2 0.121862 0.154523 0.114072 10.50000 -1.50000 H56C 2 0.159649 0.319486 0.136163 10.50000 -1.50000 AFIX 0 C57 1 0.078947 0.354620 0.107306 10.50000 0.24532 AFIX 23 1.0900 H57A 2 0.054473 0.274755 0.120226 10.50000 -1.20000 H57B 2 0.093475 0.432316 0.150002 10.50000 -1.20000 AFIX 0 C58 1 0.046429 0.439855 0.045434 10.50000 0.20169 AFIX 23 1.0900 H58A 2 0.069718 0.471508 0.015592 10.50000 -1.20000 H58B 2 0.032899 0.541683 0.061733 10.50000 -1.20000 AFIX 0 C59 1 10.000000 0.349025 10.000000 10.25000 0.17009 AFIX 23 1.0900 H59A 2 -0.012507 0.277156 0.032938 10.25000 -1.20000 H59B 2 0.012506 0.277147 -0.032936 10.25000 -1.20000 AFIX 0 PART 0 C60 1 0.078522 0.856204 -0.003624 10.50000 0.19062 AFIX 137 1.0899 H60A 2 0.051066 0.775110 -0.035161 10.50000 -1.50000 H60B 2 0.117167 0.824864 0.000206 10.50000 -1.50000 H60C 2 0.069333 0.966162 -0.026939 10.50000 -1.50000 AFIX 0 C61 1 0.075732 0.859660 0.067597 10.50000 0.17400 AFIX 23 1.0900 H61A 2 0.094051 0.959521 0.095346 10.50000 -1.20000 H61B 2 0.094154 0.761850 0.097132 10.50000 -1.20000 AFIX 0 C62 1 0.017185 0.860078 0.053445 10.50000 0.17107 AFIX 23 1.0900 H62A 2 0.009039 0.834198 0.099360 10.50000 -1.20000 H62B 2 -0.000552 0.966071 0.032312 10.50000 -1.20000 AFIX 0 C63 1 0.000000 0.733267 0.000000 10.25000 0.17360 AFIX 23 1.0900 H63A 2 -0.031286 0.664996 0.003332 10.25000 -1.20000 H63B 2 0.031287 0.664998 -0.003331 10.25000 -1.20000 HKLF 4 REM cu_d050412_0m in C2 REM R1 = 0.1055 for 2392 Fo > 4sig(Fo) and 0.1131 for all 2706 data REM 546 parameters refined using 14 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.560, deepest hole -0.342, 1-sigma level 0.087 Q1 1 0.1001 0.3621 0.1304 11.00000 0.05 0.56 Q2 1 0.0681 0.2635 0.0715 11.00000 0.05 0.55 Q3 1 0.0325 0.3719 0.3539 11.00000 0.05 0.55 Q4 1 0.0083 0.6524 0.3805 11.00000 0.05 0.49 Q5 1 0.0277 0.8175 -0.0017 11.00000 0.05 0.49 Q6 1 0.0305 0.3393 0.0314 11.00000 0.05 0.47 Q7 1 0.0555 0.4156 0.0717 11.00000 0.05 0.45 Q8 1 0.0303 0.5160 0.3813 11.00000 0.05 0.45 REM The information below was added by Olex2. REM REM R1 = 0.1055 for 2392 Fo > 4sig(Fo) and 0.1131 for all 9424 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.56, deepest hole -0.34 REM Mean Shift 0.001, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1131 REM R1_gt = 0.1055 REM wR_ref = 0.2893 REM GOOF = 1.408 REM Shift_max = 0 REM Shift_mean = 0.001 REM Reflections_all = 9424 REM Reflections_gt = 2392 REM Parameters = n/a REM Hole = 0.56 REM Peak = -0.34 REM Flack = 0.1(2) ; _database_code_depnum_ccdc_archive 'CCDC 926015'