# Electronic Supplementary Material (ESI) for CrystEngComm # 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_CCDC-762697 _database_code_depnum_ccdc_archive 'CCDC 762697' #TrackingRef 'CCDC_762697.cif' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '17 January 2013' # ======================================================================= #============================================================================ # start Validation Reply Form #Alerts level A _vrf_ATOM007_I ; PROBLEM: _atom_site_aniso_label is missing RESPONSE: All the atoms have been refined isotropically. The poor diffraction data did not allow a adequate anisotropic refinement. ; _vrf_PLAT026_I ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 29 Perc. RESPONSE: This low value comes from the overall poor diffraction quality of the crystal. ; _vrf_PLAT201_I ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 77 RESPONSE: Please see our response to _vrf_ATOM007_I. ; _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for C20 RESPONSE: Since this atom has been refined isotropically, only the use of common isotropic displacement factors would eventually eliminate this warning. ; _vrf_PLAT417_I ; PROBLEM: Short Inter D-H..H-D H7C .. H7C .. 1.23 Ang. RESPONSE: This alert appears with level A for the short intermolecular distances H7C .. H7C and H30 .. H33. Other alerts of the same kind were deemed a level B. Some atoms may have an ill-defined connectivity or are subjected to a unresolved spatial disorder. These factors contribute for inaccurate automatic placement of the hydrogen atoms. ; #Alerts level B _vrf_RFACR01_I ; PROBLEM: The value of the weighted R factor is > 0.35 Weighted R factor given 0.394 RESPONSE: Please see our response to _vrf_PLAT026_I. ; _vrf_PLAT084_I ; PROBLEM: High wR2 Value ................................. 0.39 RESPONSE: Please see our response to _vrf_PLAT026_I. ; _vrf_PLAT210_I ; PROBLEM: No Anisotropic ADP's Found in CIF .............. ? RESPONSE: Please see our response to _vrf_ATOM007_I. ; _vrf_PLAT242_I ; PROBLEM: Check Low Ueq as Compared to Neighbors for C19 RESPONSE: Please see our response to _vrf_PLAT241_I. ; _vrf_PLAT340_I ; PROBLEM:Low Bond Precision on C-C Bonds ............... 0.0215 Ang RESPONSE: Please see our response to _vrf_PLAT026_I. ; _vrf_PLAT416_I ; PROBLEM: Short Intra D-H..H-D H1C .. H2A .. 1.62 Ang. RESPONSE: Please see our response to _vrf_PLAT417_I. ; _vrf_PLAT420_I ; PROBLEM:D-H Without Acceptor O29 - H29 ... ? RESPONSE: This alert was actived for the groups O29 - H29 and O31 - H31. The hydrogen atom is probably donated to an unlocated water molecule. ; # end Validation Reply Form #============================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H70 O35' _chemical_formula_sum 'C42 H70 O35' _chemical_formula_weight 1134.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.056(5) _cell_length_b 24.415(6) _cell_length_c 15.698(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.463(13) _cell_angle_gamma 90.00 _cell_volume 6886(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1103 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 17.93 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9904 _exptl_absorpt_correction_T_max 0.9981 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; _exptl_special_details ; Hydrogen atoms attached to carbon and to the terminal hydroxyl groups were located at their idealised positions and included in the structural model in subsequent refinement cycles in riding-motion approximation with Uiso = 1.2 (aromatic carbon) or 1.5 (CH3 and OH groups) of Ueq of the parent atom. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16078 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.3006 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9408 _reflns_number_gt 2764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 ' _computing_data_reduction 'SAINT+ (Bruker, 1997-2005)' _computing_structure_solution 'SHELXTL (Bruker 2001)' _computing_structure_refinement 'SHELXTL ' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL ' _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. Although a large number of single-crystals could be directly isolated from the reaction media of distinct batches, all of them systematically exhibited very poor diffraction above ca. 1 . All non-hydrogen atoms were directly located from difference Fourier maps and refined with independent isotropic displacement parameters because the smeared-out electron density surrounding the CD chemical moieties (see below) prevented a sensible refinement of the atoms using anisotropic displacement parameters. A considerable smeared-out electron density was found in the empty spaces available in the structure, which prevented a sensible location and refinement of all guest and the vast majority of the solvent molecules. ; _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^)+(0.1988P)^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 constr _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(4) _chemical_absolute_configuration syn _refine_ls_number_reflns 9408 _refine_ls_number_parameters 312 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.2548 _refine_ls_R_factor_gt 0.1366 _refine_ls_wR_factor_ref 0.3942 _refine_ls_wR_factor_gt 0.3486 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.919 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.3150(5) 1.2056(5) 0.3752(6) 0.063(3) Uiso 1 1 d . . . H1C H 0.2915 1.1762 0.3733 0.094 Uiso 1 1 calc R . . O2 O 0.1749(6) 1.1485(5) 0.3347(7) 0.075(3) Uiso 1 1 d . . . H2A H 0.2018 1.1740 0.3271 0.112 Uiso 1 1 calc R . . O3 O 0.1516(5) 1.0303(4) 0.3428(6) 0.050(3) Uiso 1 1 d . . . H3A H 0.1660 1.0470 0.3924 0.076 Uiso 1 1 calc R . . O4 O 0.1449(6) 0.9199(4) 0.3451(6) 0.064(3) Uiso 1 1 d . . . H4A H 0.1846 0.9240 0.3887 0.096 Uiso 1 1 calc R . . O5 O 0.2541(5) 0.8302(4) 0.3733(6) 0.062(3) Uiso 1 1 d . . . H5A H 0.2984 0.8191 0.3906 0.093 Uiso 1 1 calc R . . O6 O 0.3674(5) 0.7548(4) 0.3872(6) 0.049(2) Uiso 1 1 d . . . H6A H 0.3253 0.7697 0.3677 0.073 Uiso 1 1 calc R . . O7 O 0.5207(5) 0.7606(4) 0.4205(6) 0.060(3) Uiso 1 1 d . . . H7C H 0.5021 0.7629 0.4619 0.090 Uiso 1 1 calc R . . O8 O 0.6746(5) 0.7760(4) 0.4460(6) 0.053(3) Uiso 1 1 d . . . H8A H 0.6716 0.8006 0.4821 0.080 Uiso 1 1 calc R . . O9 O 0.7660(5) 0.8710(4) 0.4715(6) 0.060(3) Uiso 1 1 d . . . H9A H 0.7568 0.8596 0.5171 0.091 Uiso 1 1 calc R . . O10 O 0.8423(6) 0.9683(5) 0.4835(7) 0.074(3) Uiso 1 1 d . . . H10A H 0.8151 0.9777 0.5135 0.111 Uiso 1 1 calc R . . O11 O 0.8049(6) 1.0783(5) 0.4844(7) 0.075(3) Uiso 1 1 d . . . H11A H 0.7761 1.1038 0.4871 0.112 Uiso 1 1 calc R . . O12 O 0.7461(5) 1.1833(4) 0.4723(6) 0.062(3) Uiso 1 1 d . . . H12A H 0.7345 1.1993 0.5131 0.093 Uiso 1 1 calc R . . O13 O 0.6001(6) 1.2239(5) 0.4490(7) 0.081(3) Uiso 1 1 d . . . H13C H 0.6267 1.2113 0.4991 0.122 Uiso 1 1 calc R . . O14 O 0.4543(5) 1.2589(5) 0.3964(6) 0.064(3) Uiso 1 1 d . . . H14A H 0.4525 1.2331 0.4311 0.096 Uiso 1 1 calc R . . O15 O 0.4936(4) 1.2009(4) 0.2723(6) 0.052(3) Uiso 1 1 d D . . O16 O 0.2650(5) 1.1401(4) 0.2204(6) 0.061(3) Uiso 1 1 d D . . O17 O 0.1889(5) 0.9692(4) 0.2112(7) 0.069(3) Uiso 1 1 d D . . O18 O 0.3279(5) 0.8257(4) 0.2449(6) 0.054(3) Uiso 1 1 d D . . O19 O 0.5696(5) 0.8134(4) 0.2866(6) 0.059(3) Uiso 1 1 d D . . O20 O 0.7305(6) 0.9397(4) 0.3152(7) 0.074(3) Uiso 1 1 d D . . O21 O 0.6995(5) 1.1158(4) 0.3197(6) 0.066(3) Uiso 1 1 d D . . O22 O 0.3867(6) 1.2347(4) 0.1602(7) 0.069(3) Uiso 1 1 d D . . O23 O 0.1664(6) 1.1044(4) 0.1087(7) 0.069(3) Uiso 1 1 d D . . O24 O 0.1494(5) 0.8952(4) 0.1175(6) 0.060(3) Uiso 1 1 d D . . O25 O 0.3763(7) 0.7662(6) 0.1617(8) 0.092(4) Uiso 1 1 d D . . O26 O 0.6527(5) 0.8059(4) 0.2122(6) 0.054(3) Uiso 1 1 d D . . O27 O 0.7822(6) 0.9984(5) 0.2397(7) 0.075(3) Uiso 1 1 d D . . O28 O 0.6714(5) 1.1953(4) 0.2260(6) 0.058(3) Uiso 1 1 d D . . O29 O 0.5722(5) 1.2715(4) 0.1188(6) 0.063(3) Uiso 1 1 d D . . H29 H 0.5521 1.2846 0.0668 0.095 Uiso 1 1 calc R . . O30 O 0.2530(10) 1.2209(8) 0.0308(11) 0.159(7) Uiso 1 1 d D . . H30 H 0.2770 1.2504 0.0388 0.239 Uiso 1 1 calc R . . O31 O 0.0879(11) 1.0273(10) -0.0044(14) 0.204(9) Uiso 1 1 d D . . H31 H 0.0723 1.0113 -0.0547 0.306 Uiso 1 1 calc R . . O33 O 0.1742(5) 0.8018(4) 0.0343(6) 0.065(3) Uiso 1 1 d D . . H33 H 0.1753 0.7870 -0.0136 0.098 Uiso 1 1 calc R . . O35 O 0.4901(11) 0.7474(9) 0.0903(12) 0.177(7) Uiso 1 1 d D . . H35 H 0.4501 0.7301 0.0811 0.266 Uiso 1 1 calc R . . O37 O 0.7567(9) 0.8527(7) 0.1424(11) 0.148(6) Uiso 1 1 d D . . H37 H 0.7701 0.8350 0.1911 0.222 Uiso 1 1 calc R . . O38 O 0.6941(14) 1.0474(10) 0.0795(14) 0.235(10) Uiso 1 1 d D . . H38 H 0.6862 1.0151 0.0925 0.352 Uiso 1 1 calc R . . C1 C 0.1610(11) 1.0180(6) 0.0341(9) 0.101(6) Uiso 1 1 d D . . H1A H 0.1887 1.0331 -0.0038 0.122 Uiso 1 1 calc R . . H1B H 0.1710 0.9782 0.0418 0.122 Uiso 1 1 calc R . . C2 C 0.1849(9) 1.0468(4) 0.1267(8) 0.058(4) Uiso 1 1 d D . . H2 H 0.2404 1.0445 0.1518 0.070 Uiso 1 1 calc R . . C3 C 0.1583(8) 1.0263(5) 0.1924(8) 0.041(3) Uiso 1 1 d D . . H3 H 0.1027 1.0255 0.1695 0.049 Uiso 1 1 calc R . . C4 C 0.1861(8) 1.0541(6) 0.2825(9) 0.044(4) Uiso 1 1 d . . . H4 H 0.2416 1.0546 0.3087 0.053 Uiso 1 1 calc R . . C5 C 0.1494(9) 1.1170(7) 0.2562(10) 0.065(5) Uiso 1 1 d . . . H5 H 0.0938 1.1157 0.2320 0.078 Uiso 1 1 calc R . . C6 C 0.1835(6) 1.1397(7) 0.1812(9) 0.058(4) Uiso 1 1 d D . . H6 H 0.1643 1.1773 0.1609 0.070 Uiso 1 1 calc R . . C7 C 0.2198(8) 0.8458(6) 0.0533(10) 0.062(4) Uiso 1 1 d D . . H7A H 0.2037 0.8705 0.0004 0.074 Uiso 1 1 calc R . . H7B H 0.2704 0.8328 0.0593 0.074 Uiso 1 1 calc R . . C8 C 0.2255(6) 0.8780(6) 0.1325(8) 0.037(3) Uiso 1 1 d D . . H8 H 0.2591 0.9102 0.1379 0.045 Uiso 1 1 calc R . . C9 C 0.2502(6) 0.8414(6) 0.2269(8) 0.041(4) Uiso 1 1 d D . . H9 H 0.2187 0.8078 0.2175 0.050 Uiso 1 1 calc R . . C10 C 0.2422(7) 0.8706(6) 0.2951(8) 0.040(4) Uiso 1 1 d . . . H10 H 0.2764 0.9029 0.3116 0.049 Uiso 1 1 calc R . . C11 C 0.1599(7) 0.8862(6) 0.2739(8) 0.042(4) Uiso 1 1 d . . . H11 H 0.1283 0.8525 0.2621 0.051 Uiso 1 1 calc R . . C12 C 0.1366(8) 0.9218(6) 0.1960(9) 0.054(4) Uiso 1 1 d D . . H12 H 0.0838 0.9340 0.1816 0.065 Uiso 1 1 calc R . . C13 C 0.4795(17) 0.8002(10) 0.1050(18) 0.163(10) Uiso 1 1 d D . . H13A H 0.4450 0.8178 0.0501 0.195 Uiso 1 1 calc R . . H13B H 0.5272 0.8205 0.1246 0.195 Uiso 1 1 calc R . . C14 C 0.4436(9) 0.7978(8) 0.1843(12) 0.094(6) Uiso 1 1 d D . . H14 H 0.4300 0.8362 0.1943 0.113 Uiso 1 1 calc R . . C15 C 0.4996(8) 0.7819(7) 0.2626(11) 0.078(5) Uiso 1 1 d D . . H15 H 0.5124 0.7431 0.2533 0.093 Uiso 1 1 calc R . . C16 C 0.4700(7) 0.7815(6) 0.3395(9) 0.046(4) Uiso 1 1 d . . . H16 H 0.4585 0.8202 0.3510 0.055 Uiso 1 1 calc R . . C17 C 0.3994(9) 0.7504(7) 0.3120(10) 0.070(5) Uiso 1 1 d . . . H17 H 0.4107 0.7110 0.3048 0.084 Uiso 1 1 calc R . . C18 C 0.3407(10) 0.7680(5) 0.2305(11) 0.076(5) Uiso 1 1 d D . . H18 H 0.2947 0.7451 0.2156 0.091 Uiso 1 1 calc R . . C19 C 0.6940(9) 0.8811(7) 0.1351(10) 0.070(5) Uiso 1 1 d D . . H19A H 0.6541 0.8715 0.0781 0.084 Uiso 1 1 calc R . . H19B H 0.7036 0.9210 0.1349 0.084 Uiso 1 1 calc R . . C20 C 0.6689(14) 0.8649(7) 0.2215(15) 0.128(8) Uiso 1 1 d D . . H20 H 0.6223 0.8852 0.2172 0.154 Uiso 1 1 calc R . . C21 C 0.7305(8) 0.8799(5) 0.3126(9) 0.050(4) Uiso 1 1 d D . . H21 H 0.7802 0.8649 0.3161 0.060 Uiso 1 1 calc R . . C22 C 0.7051(8) 0.8590(6) 0.3926(9) 0.051(4) Uiso 1 1 d . . . H22 H 0.6579 0.8766 0.3930 0.062 Uiso 1 1 calc R . . C23 C 0.6971(7) 0.7994(5) 0.3774(8) 0.036(3) Uiso 1 1 d . . . H23 H 0.7458 0.7833 0.3791 0.043 Uiso 1 1 calc R . . C24 C 0.6340(8) 0.7855(7) 0.2817(11) 0.071(5) Uiso 1 1 d D . . H24 H 0.6249 0.7451 0.2747 0.085 Uiso 1 1 calc R . . C25 C 0.7247(12) 1.0765(9) 0.1566(13) 0.111(7) Uiso 1 1 d D . . H25A H 0.6935 1.1090 0.1563 0.133 Uiso 1 1 calc R . . H25B H 0.7749 1.0893 0.1603 0.133 Uiso 1 1 calc R . . C26 C 0.7298(9) 1.0426(6) 0.2334(10) 0.066(5) Uiso 1 1 d D . . H26 H 0.6798 1.0278 0.2291 0.079 Uiso 1 1 calc R . . C27 C 0.7584(7) 1.0790(6) 0.3121(9) 0.050(4) Uiso 1 1 d D . . H27 H 0.8040 1.0993 0.3123 0.060 Uiso 1 1 calc R . . C28 C 0.7706(8) 1.0462(6) 0.4034(8) 0.044(4) Uiso 1 1 d . . . H28 H 0.7228 1.0296 0.4042 0.053 Uiso 1 1 calc R . . C29 C 0.8266(11) 1.0023(8) 0.4049(11) 0.091(6) Uiso 1 1 d . . . H29D H 0.8740 1.0209 0.4075 0.109 Uiso 1 1 calc R . . C30 C 0.8027(8) 0.9641(8) 0.3187(12) 0.088(6) Uiso 1 1 d D . . H30D H 0.8412 0.9361 0.3193 0.106 Uiso 1 1 calc R . . C31 C 0.5558(8) 1.2178(5) 0.1181(9) 0.055(4) Uiso 1 1 d D . . H31A H 0.5716 1.1994 0.0712 0.066 Uiso 1 1 calc R . . H31B H 0.5012 1.2136 0.1009 0.066 Uiso 1 1 calc R . . C32 C 0.5922(6) 1.1892(6) 0.2072(9) 0.052(4) Uiso 1 1 d D . . H32 H 0.5784 1.1495 0.2018 0.063 Uiso 1 1 calc R . . C33 C 0.5709(6) 1.2163(6) 0.2879(8) 0.043(4) Uiso 1 1 d D . . H33D H 0.5777 1.2570 0.2900 0.051 Uiso 1 1 calc R . . C34 C 0.6175(7) 1.1906(6) 0.3674(8) 0.040(3) Uiso 1 1 d . . . H34 H 0.6070 1.1505 0.3684 0.048 Uiso 1 1 calc R . . C35 C 0.6913(9) 1.2009(8) 0.3781(11) 0.076(5) Uiso 1 1 d . . . H35D H 0.6971 1.2412 0.3712 0.091 Uiso 1 1 calc R . . C36 C 0.7213(8) 1.1730(5) 0.3169(9) 0.049(4) Uiso 1 1 d D . . H36 H 0.7758 1.1788 0.3296 0.059 Uiso 1 1 calc R . . C37 C 0.3010(11) 1.1784(8) 0.0524(12) 0.100(6) Uiso 1 1 d D . . H37A H 0.3350 1.1798 0.0165 0.120 Uiso 1 1 calc R . . H37B H 0.2736 1.1433 0.0400 0.120 Uiso 1 1 calc R . . C38 C 0.3449(8) 1.1837(6) 0.1526(9) 0.056(4) Uiso 1 1 d D . . H38A H 0.3803 1.1523 0.1720 0.067 Uiso 1 1 calc R . . C39 C 0.3052(8) 1.1920(6) 0.2206(10) 0.067(5) Uiso 1 1 d D . . H39 H 0.2699 1.2235 0.2031 0.080 Uiso 1 1 calc R . . C40 C 0.3625(8) 1.2011(6) 0.3112(9) 0.049(4) Uiso 1 1 d . . . H40 H 0.3988 1.1700 0.3289 0.059 Uiso 1 1 calc R . . C41 C 0.3984(9) 1.2511(7) 0.3105(9) 0.061(4) Uiso 1 1 d . . . H41 H 0.3623 1.2823 0.2946 0.073 Uiso 1 1 calc R . . C42 C 0.4337(8) 1.2427(6) 0.2419(10) 0.066(5) Uiso 1 1 d D . . H42 H 0.4595 1.2779 0.2389 0.079 Uiso 1 1 calc R . . _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 C40 1.564(16) . ? O1 H1C 0.8400 . ? O2 C5 1.396(17) . ? O2 H2A 0.8400 . ? O3 C4 1.441(15) . ? O3 H3A 0.8400 . ? O4 C11 1.489(15) . ? O4 H4A 0.8400 . ? O5 C10 1.530(15) . ? O5 H5A 0.8400 . ? O6 C17 1.502(17) . ? O6 H6A 0.8400 . ? O7 C16 1.412(15) . ? O7 H7C 0.8400 . ? O8 C23 1.406(14) . ? O8 H8A 0.8400 . ? O9 C22 1.417(15) . ? O9 H9A 0.8400 . ? O10 C29 1.432(19) . ? O10 H10A 0.8400 . ? O11 C28 1.451(15) . ? O11 H11A 0.8400 . ? O12 C35 1.559(18) . ? O12 H12A 0.8400 . ? O13 C34 1.641(16) . ? O13 H13C 0.8400 . ? O14 C41 1.426(16) . ? O14 H14A 0.8400 . ? O15 C33 1.460(9) . ? O15 C42 1.487(9) . ? O16 C6 1.469(9) . ? O16 C39 1.480(10) . ? O17 C12 1.494(9) . ? O17 C3 1.502(9) . ? O18 C18 1.459(10) . ? O18 C9 1.463(9) . ? O19 C24 1.429(10) . ? O19 C15 1.476(10) . ? O20 C21 1.460(9) . ? O20 C30 1.485(10) . ? O21 C36 1.462(9) . ? O21 C27 1.473(9) . ? O22 C42 1.311(16) . ? O22 C38 1.462(10) . ? O23 C6 1.377(16) . ? O23 C2 1.452(10) . ? O24 C8 1.451(10) . ? O24 C12 1.482(16) . ? O25 C14 1.436(11) . ? O25 C18 1.456(19) . ? O26 C24 1.350(16) . ? O26 C20 1.472(11) . ? O27 C30 1.438(18) . ? O27 C26 1.451(11) . ? O28 C32 1.447(10) . ? O28 C36 1.528(16) . ? O29 C31 1.348(11) . ? O29 H29 0.8400 . ? O30 C37 1.349(12) . ? O30 H30 0.8400 . ? O31 C1 1.341(12) . ? O31 H31 0.8400 . ? O33 C7 1.350(11) . ? O33 H33 0.8400 . ? O35 C13 1.337(13) . ? O35 H35 0.8400 . ? O37 C19 1.353(12) . ? O37 H37 0.8400 . ? O38 C25 1.356(12) . ? O38 H38 0.8400 . ? C1 C2 1.5403(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.385(17) . ? C2 H2 1.0000 . ? C3 C4 1.497(16) . ? C3 H3 1.0000 . ? C4 C5 1.68(2) . ? C4 H4 1.0000 . ? C5 C6 1.62(2) . ? C5 H5 1.0000 . ? C6 H6 1.0000 . ? C7 C8 1.444(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.659(17) . ? C8 H8 1.0000 . ? C9 C10 1.336(16) . ? C9 H9 1.0000 . ? C10 C11 1.540(18) . ? C10 H10 1.0000 . ? C11 C12 1.444(18) . ? C11 H11 1.0000 . ? C12 H12 1.0000 . ? C13 C14 1.61(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.39(2) . ? C14 H14 1.0000 . ? C15 C16 1.49(2) . ? C15 H15 1.0000 . ? C16 C17 1.48(2) . ? C16 H16 1.0000 . ? C17 C18 1.46(2) . ? C17 H17 1.0000 . ? C18 H18 1.0000 . ? C19 C20 1.63(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.56(2) . ? C20 H20 1.0000 . ? C21 C22 1.574(19) . ? C21 H21 1.0000 . ? C22 C23 1.474(18) . ? C22 H22 1.0000 . ? C23 C24 1.617(19) . ? C23 H23 1.0000 . ? C24 H24 1.0000 . ? C25 C26 1.44(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.471(19) . ? C26 H26 1.0000 . ? C27 C28 1.591(18) . ? C27 H27 1.0000 . ? C28 C29 1.51(2) . ? C28 H28 1.0000 . ? C29 C30 1.58(2) . ? C29 H29D 1.0000 . ? C30 H30D 1.0000 . ? C31 C32 1.510(18) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.596(18) . ? C32 H32 1.0000 . ? C33 C34 1.416(17) . ? C33 H33D 1.0000 . ? C34 C35 1.381(19) . ? C34 H34 1.0000 . ? C35 C36 1.44(2) . ? C35 H35D 1.0000 . ? C36 H36 1.0000 . ? C37 C38 1.52(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.512(19) . ? C38 H38A 1.0000 . ? C39 C40 1.493(19) . ? C39 H39 1.0000 . ? C40 C41 1.401(19) . ? C40 H40 1.0000 . ? C41 C42 1.462(19) . ? C41 H41 1.0000 . ? C42 H42 1.0000 . ? 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 C40 O1 H1C 109.5 . . ? C5 O2 H2A 109.5 . . ? C4 O3 H3A 109.5 . . ? C11 O4 H4A 109.5 . . ? C10 O5 H5A 109.5 . . ? C17 O6 H6A 109.5 . . ? C16 O7 H7C 109.5 . . ? C23 O8 H8A 109.5 . . ? C22 O9 H9A 109.5 . . ? C29 O10 H10A 109.5 . . ? C28 O11 H11A 109.5 . . ? C35 O12 H12A 109.5 . . ? C34 O13 H13C 109.5 . . ? C41 O14 H14A 109.5 . . ? C33 O15 C42 120.0(10) . . ? C6 O16 C39 118.8(11) . . ? C12 O17 C3 119.6(10) . . ? C18 O18 C9 115.7(11) . . ? C24 O19 C15 117.1(11) . . ? C21 O20 C30 113.2(12) . . ? C36 O21 C27 110.4(10) . . ? C42 O22 C38 112.5(12) . . ? C6 O23 C2 118.0(10) . . ? C8 O24 C12 115.1(10) . . ? C14 O25 C18 113.5(13) . . ? C24 O26 C20 112.6(14) . . ? C30 O27 C26 118.3(13) . . ? C32 O28 C36 115.9(10) . . ? C31 O29 H29 109.5 . . ? C37 O30 H30 109.5 . . ? C1 O31 H31 109.5 . . ? C7 O33 H33 109.5 . . ? C13 O35 H35 109.5 . . ? C19 O37 H37 109.5 . . ? C25 O38 H38 109.5 . . ? O31 C1 C2 106.5(16) . . ? O31 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O31 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? C3 C2 O23 111.7(11) . . ? C3 C2 C1 118.1(13) . . ? O23 C2 C1 106.3(12) . . ? C3 C2 H2 106.7 . . ? O23 C2 H2 106.7 . . ? C1 C2 H2 106.7 . . ? C2 C3 C4 116.0(11) . . ? C2 C3 O17 105.5(10) . . ? C4 C3 O17 104.1(9) . . ? C2 C3 H3 110.3 . . ? C4 C3 H3 110.3 . . ? O17 C3 H3 110.3 . . ? O3 C4 C3 110.0(11) . . ? O3 C4 C5 106.6(11) . . ? C3 C4 C5 101.2(10) . . ? O3 C4 H4 112.7 . . ? C3 C4 H4 112.7 . . ? C5 C4 H4 112.7 . . ? O2 C5 C6 110.3(12) . . ? O2 C5 C4 107.0(11) . . ? C6 C5 C4 104.8(11) . . ? O2 C5 H5 111.5 . . ? C6 C5 H5 111.5 . . ? C4 C5 H5 111.5 . . ? O23 C6 O16 106.0(11) . . ? O23 C6 C5 110.2(12) . . ? O16 C6 C5 108.8(11) . . ? O23 C6 H6 110.6 . . ? O16 C6 H6 110.6 . . ? C5 C6 H6 110.6 . . ? O33 C7 C8 118.8(12) . . ? O33 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? O33 C7 H7B 107.6 . . ? C8 C7 H7B 107.6 . . ? H7A C7 H7B 107.0 . . ? C7 C8 O24 103.6(10) . . ? C7 C8 C9 113.1(11) . . ? O24 C8 C9 105.8(9) . . ? C7 C8 H8 111.3 . . ? O24 C8 H8 111.3 . . ? C9 C8 H8 111.3 . . ? C10 C9 O18 111.3(10) . . ? C10 C9 C8 110.8(11) . . ? O18 C9 C8 106.4(9) . . ? C10 C9 H9 109.4 . . ? O18 C9 H9 109.4 . . ? C8 C9 H9 109.4 . . ? C9 C10 O5 105.9(11) . . ? C9 C10 C11 109.8(11) . . ? O5 C10 C11 101.6(10) . . ? C9 C10 H10 112.9 . . ? O5 C10 H10 112.9 . . ? C11 C10 H10 112.9 . . ? C12 C11 O4 102.8(11) . . ? C12 C11 C10 109.5(11) . . ? O4 C11 C10 114.2(10) . . ? C12 C11 H11 110.0 . . ? O4 C11 H11 110.0 . . ? C10 C11 H11 110.0 . . ? C11 C12 O24 110.6(11) . . ? C11 C12 O17 109.4(11) . . ? O24 C12 O17 100.7(10) . . ? C11 C12 H12 111.9 . . ? O24 C12 H12 111.9 . . ? O17 C12 H12 111.9 . . ? O35 C13 C14 103(2) . . ? O35 C13 H13A 111.2 . . ? C14 C13 H13A 111.2 . . ? O35 C13 H13B 111.2 . . ? C14 C13 H13B 111.2 . . ? H13A C13 H13B 109.1 . . ? C15 C14 O25 115.4(14) . . ? C15 C14 C13 107.2(17) . . ? O25 C14 C13 113.8(16) . . ? C15 C14 H14 106.6 . . ? O25 C14 H14 106.6 . . ? C13 C14 H14 106.6 . . ? C14 C15 O19 116.3(13) . . ? C14 C15 C16 109.3(14) . . ? O19 C15 C16 110.4(12) . . ? C14 C15 H15 106.8 . . ? O19 C15 H15 106.8 . . ? C16 C15 H15 106.8 . . ? O7 C16 C17 111.1(11) . . ? O7 C16 C15 113.6(12) . . ? C17 C16 C15 108.6(11) . . ? O7 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C15 C16 H16 107.8 . . ? C18 C17 C16 117.6(14) . . ? C18 C17 O6 106.0(13) . . ? C16 C17 O6 107.6(12) . . ? C18 C17 H17 108.5 . . ? C16 C17 H17 108.5 . . ? O6 C17 H17 108.5 . . ? C17 C18 O25 103.3(13) . . ? C17 C18 O18 105.5(12) . . ? O25 C18 O18 106.7(12) . . ? C17 C18 H18 113.5 . . ? O25 C18 H18 113.5 . . ? O18 C18 H18 113.5 . . ? O37 C19 C20 107.5(15) . . ? O37 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O37 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? O26 C20 C21 112.9(14) . . ? O26 C20 C19 105.4(15) . . ? C21 C20 C19 111.5(16) . . ? O26 C20 H20 109.0 . . ? C21 C20 H20 109.0 . . ? C19 C20 H20 109.0 . . ? O20 C21 C20 104.7(10) . . ? O20 C21 C22 107.4(11) . . ? C20 C21 C22 108.6(13) . . ? O20 C21 H21 111.9 . . ? C20 C21 H21 111.9 . . ? C22 C21 H21 111.9 . . ? O9 C22 C23 110.9(11) . . ? O9 C22 C21 104.5(11) . . ? C23 C22 C21 103.6(11) . . ? O9 C22 H22 112.4 . . ? C23 C22 H22 112.4 . . ? C21 C22 H22 112.4 . . ? O8 C23 C22 108.6(11) . . ? O8 C23 C24 107.8(10) . . ? C22 C23 C24 111.2(11) . . ? O8 C23 H23 109.8 . . ? C22 C23 H23 109.8 . . ? C24 C23 H23 109.8 . . ? O26 C24 O19 109.3(11) . . ? O26 C24 C23 111.1(12) . . ? O19 C24 C23 103.6(10) . . ? O26 C24 H24 110.9 . . ? O19 C24 H24 110.9 . . ? C23 C24 H24 110.9 . . ? O38 C25 C26 110(2) . . ? O38 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? O38 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C25 C26 O27 109.7(14) . . ? C25 C26 C27 105.0(14) . . ? O27 C26 C27 109.8(11) . . ? C25 C26 H26 110.7 . . ? O27 C26 H26 110.7 . . ? C27 C26 H26 110.7 . . ? C26 C27 O21 110.9(11) . . ? C26 C27 C28 110.7(12) . . ? O21 C27 C28 96.9(9) . . ? C26 C27 H27 112.4 . . ? O21 C27 H27 112.4 . . ? C28 C27 H27 112.4 . . ? O11 C28 C29 105.1(12) . . ? O11 C28 C27 113.9(11) . . ? C29 C28 C27 105.2(11) . . ? O11 C28 H28 110.8 . . ? C29 C28 H28 110.8 . . ? C27 C28 H28 110.8 . . ? O10 C29 C28 111.6(14) . . ? O10 C29 C30 108.3(15) . . ? C28 C29 C30 113.9(15) . . ? O10 C29 H29D 107.6 . . ? C28 C29 H29D 107.6 . . ? C30 C29 H29D 107.6 . . ? O27 C30 O20 102.6(12) . . ? O27 C30 C29 108.3(15) . . ? O20 C30 C29 105.5(13) . . ? O27 C30 H30D 113.2 . . ? O20 C30 H30D 113.2 . . ? C29 C30 H30D 113.2 . . ? O29 C31 C32 114.1(12) . . ? O29 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? O29 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? O28 C32 C31 105.5(11) . . ? O28 C32 C33 108.7(10) . . ? C31 C32 C33 112.6(11) . . ? O28 C32 H32 110.0 . . ? C31 C32 H32 110.0 . . ? C33 C32 H32 110.0 . . ? C34 C33 O15 109.5(10) . . ? C34 C33 C32 105.4(11) . . ? O15 C33 C32 105.6(9) . . ? C34 C33 H33D 112.0 . . ? O15 C33 H33D 112.0 . . ? C32 C33 H33D 112.0 . . ? C35 C34 C33 109.9(12) . . ? C35 C34 O13 106.1(11) . . ? C33 C34 O13 103.7(11) . . ? C35 C34 H34 112.2 . . ? C33 C34 H34 112.2 . . ? O13 C34 H34 112.2 . . ? C34 C35 C36 116.5(14) . . ? C34 C35 O12 113.5(13) . . ? C36 C35 O12 102.3(13) . . ? C34 C35 H35D 108.1 . . ? C36 C35 H35D 108.1 . . ? O12 C35 H35D 108.1 . . ? C35 C36 O21 104.6(12) . . ? C35 C36 O28 101.1(11) . . ? O21 C36 O28 105.9(10) . . ? C35 C36 H36 114.6 . . ? O21 C36 H36 114.6 . . ? O28 C36 H36 114.6 . . ? O30 C37 C38 106.7(16) . . ? O30 C37 H37A 110.4 . . ? C38 C37 H37A 110.4 . . ? O30 C37 H37B 110.4 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? O22 C38 C39 102.5(10) . . ? O22 C38 C37 104.6(12) . . ? C39 C38 C37 120.7(13) . . ? O22 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? O16 C39 C40 110.1(11) . . ? O16 C39 C38 105.3(11) . . ? C40 C39 C38 108.3(12) . . ? O16 C39 H39 111.0 . . ? C40 C39 H39 111.0 . . ? C38 C39 H39 111.0 . . ? C41 C40 C39 109.0(11) . . ? C41 C40 O1 109.4(11) . . ? C39 C40 O1 103.0(11) . . ? C41 C40 H40 111.7 . . ? C39 C40 H40 111.7 . . ? O1 C40 H40 111.7 . . ? C40 C41 O14 108.8(12) . . ? C40 C41 C42 103.2(13) . . ? O14 C41 C42 109.4(13) . . ? C40 C41 H41 111.7 . . ? O14 C41 H41 111.7 . . ? C42 C41 H41 111.7 . . ? O22 C42 C41 114.2(13) . . ? O22 C42 O15 114.4(11) . . ? C41 C42 O15 110.6(12) . . ? O22 C42 H42 105.6 . . ? C41 C42 H42 105.6 . . ? O15 C42 H42 105.6 . . ? 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 C6 O23 C2 C3 50.8(17) . . . . ? C6 O23 C2 C1 -179.0(12) . . . . ? O31 C1 C2 C3 68(2) . . . . ? O31 C1 C2 O23 -59(2) . . . . ? O23 C2 C3 C4 -59.0(15) . . . . ? C1 C2 C3 C4 177.2(13) . . . . ? O23 C2 C3 O17 -173.6(10) . . . . ? C1 C2 C3 O17 62.6(16) . . . . ? C12 O17 C3 C2 -120.0(12) . . . . ? C12 O17 C3 C4 117.4(12) . . . . ? C2 C3 C4 O3 177.5(11) . . . . ? O17 C3 C4 O3 -67.1(13) . . . . ? C2 C3 C4 C5 65.0(14) . . . . ? O17 C3 C4 C5 -179.6(11) . . . . ? O3 C4 C5 O2 68.2(14) . . . . ? C3 C4 C5 O2 -176.7(12) . . . . ? O3 C4 C5 C6 -174.6(10) . . . . ? C3 C4 C5 C6 -59.5(13) . . . . ? C2 O23 C6 O16 65.1(15) . . . . ? C2 O23 C6 C5 -52.5(15) . . . . ? C39 O16 C6 O23 117.2(13) . . . . ? C39 O16 C6 C5 -124.3(13) . . . . ? O2 C5 C6 O23 171.9(11) . . . . ? C4 C5 C6 O23 57.1(13) . . . . ? O2 C5 C6 O16 56.1(16) . . . . ? C4 C5 C6 O16 -58.7(14) . . . . ? O33 C7 C8 O24 -57.8(16) . . . . ? O33 C7 C8 C9 56.2(16) . . . . ? C12 O24 C8 C7 170.4(10) . . . . ? C12 O24 C8 C9 51.2(13) . . . . ? C18 O18 C9 C10 130.9(13) . . . . ? C18 O18 C9 C8 -108.3(12) . . . . ? C7 C8 C9 C10 -169.2(11) . . . . ? O24 C8 C9 C10 -56.6(13) . . . . ? C7 C8 C9 O18 69.7(13) . . . . ? O24 C8 C9 O18 -177.7(9) . . . . ? O18 C9 C10 O5 -70.9(13) . . . . ? C8 C9 C10 O5 171.0(9) . . . . ? O18 C9 C10 C11 -179.8(10) . . . . ? C8 C9 C10 C11 62.1(14) . . . . ? C9 C10 C11 C12 -64.1(15) . . . . ? O5 C10 C11 C12 -175.9(10) . . . . ? C9 C10 C11 O4 -178.8(11) . . . . ? O5 C10 C11 O4 69.4(13) . . . . ? O4 C11 C12 O24 178.5(9) . . . . ? C10 C11 C12 O24 56.7(13) . . . . ? O4 C11 C12 O17 68.5(13) . . . . ? C10 C11 C12 O17 -53.4(14) . . . . ? C8 O24 C12 C11 -56.5(13) . . . . ? C8 O24 C12 O17 59.1(13) . . . . ? C3 O17 C12 C11 -132.1(12) . . . . ? C3 O17 C12 O24 111.4(12) . . . . ? C18 O25 C14 C15 61(2) . . . . ? C18 O25 C14 C13 -175.0(15) . . . . ? O35 C13 C14 C15 71(2) . . . . ? O35 C13 C14 O25 -58(3) . . . . ? O25 C14 C15 O19 179.4(14) . . . . ? C13 C14 C15 O19 52(2) . . . . ? O25 C14 C15 C16 -55(2) . . . . ? C13 C14 C15 C16 177.3(15) . . . . ? C24 O19 C15 C14 -112.5(17) . . . . ? C24 O19 C15 C16 122.3(14) . . . . ? C14 C15 C16 O7 174.0(13) . . . . ? O19 C15 C16 O7 -56.8(17) . . . . ? C14 C15 C16 C17 49.8(18) . . . . ? O19 C15 C16 C17 178.9(12) . . . . ? O7 C16 C17 C18 178.6(13) . . . . ? C15 C16 C17 C18 -55.7(18) . . . . ? O7 C16 C17 O6 59.1(15) . . . . ? C15 C16 C17 O6 -175.2(12) . . . . ? C16 C17 C18 O25 56.3(16) . . . . ? O6 C17 C18 O25 176.6(11) . . . . ? C16 C17 C18 O18 -55.6(18) . . . . ? O6 C17 C18 O18 64.7(15) . . . . ? C14 O25 C18 C17 -55.0(16) . . . . ? C14 O25 C18 O18 56.0(17) . . . . ? C9 O18 C18 C17 -130.4(12) . . . . ? C9 O18 C18 O25 120.1(12) . . . . ? C24 O26 C20 C21 55(2) . . . . ? C24 O26 C20 C19 177.3(12) . . . . ? O37 C19 C20 O26 -63(2) . . . . ? O37 C19 C20 C21 60.3(18) . . . . ? C30 O20 C21 C20 -119.1(15) . . . . ? C30 O20 C21 C22 125.6(13) . . . . ? O26 C20 C21 O20 -171.6(15) . . . . ? C19 C20 C21 O20 69.9(16) . . . . ? O26 C20 C21 C22 -57(2) . . . . ? C19 C20 C21 C22 -175.6(12) . . . . ? O20 C21 C22 O9 -71.1(13) . . . . ? C20 C21 C22 O9 176.2(11) . . . . ? O20 C21 C22 C23 172.7(11) . . . . ? C20 C21 C22 C23 60.0(14) . . . . ? O9 C22 C23 O8 68.2(14) . . . . ? C21 C22 C23 O8 179.8(10) . . . . ? O9 C22 C23 C24 -173.4(10) . . . . ? C21 C22 C23 C24 -61.8(14) . . . . ? C20 O26 C24 O19 59.4(18) . . . . ? C20 O26 C24 C23 -54.4(16) . . . . ? C15 O19 C24 O26 110.5(14) . . . . ? C15 O19 C24 C23 -131.1(12) . . . . ? O8 C23 C24 O26 -178.8(10) . . . . ? C22 C23 C24 O26 62.3(14) . . . . ? O8 C23 C24 O19 63.9(13) . . . . ? C22 C23 C24 O19 -54.9(15) . . . . ? O38 C25 C26 O27 66(2) . . . . ? O38 C25 C26 C27 -176.1(19) . . . . ? C30 O27 C26 C25 171.9(14) . . . . ? C30 O27 C26 C27 57.0(17) . . . . ? C25 C26 C27 O21 76.2(16) . . . . ? O27 C26 C27 O21 -166.0(11) . . . . ? C25 C26 C27 C28 -177.4(13) . . . . ? O27 C26 C27 C28 -59.5(16) . . . . ? C36 O21 C27 C26 -121.5(13) . . . . ? C36 O21 C27 C28 123.1(11) . . . . ? C26 C27 C28 O11 174.9(11) . . . . ? O21 C27 C28 O11 -69.6(13) . . . . ? C26 C27 C28 C29 60.3(15) . . . . ? O21 C27 C28 C29 175.8(11) . . . . ? O11 C28 C29 O10 60.5(16) . . . . ? C27 C28 C29 O10 -178.9(13) . . . . ? O11 C28 C29 C30 -176.4(13) . . . . ? C27 C28 C29 C30 -55.9(17) . . . . ? C26 O27 C30 O20 61.0(16) . . . . ? C26 O27 C30 C29 -50.3(16) . . . . ? C21 O20 C30 O27 121.9(13) . . . . ? C21 O20 C30 C29 -124.8(14) . . . . ? O10 C29 C30 O27 176.2(12) . . . . ? C28 C29 C30 O27 51.3(17) . . . . ? O10 C29 C30 O20 66.9(18) . . . . ? C28 C29 C30 O20 -58.0(18) . . . . ? C36 O28 C32 C31 176.0(10) . . . . ? C36 O28 C32 C33 55.0(14) . . . . ? O29 C31 C32 O28 -60.5(16) . . . . ? O29 C31 C32 C33 57.8(16) . . . . ? C42 O15 C33 C34 138.4(12) . . . . ? C42 O15 C33 C32 -108.6(12) . . . . ? O28 C32 C33 C34 -55.0(13) . . . . ? C31 C32 C33 C34 -171.4(11) . . . . ? O28 C32 C33 O15 -170.8(10) . . . . ? C31 C32 C33 O15 72.7(13) . . . . ? O15 C33 C34 C35 174.5(12) . . . . ? C32 C33 C34 C35 61.3(15) . . . . ? O15 C33 C34 O13 -72.4(12) . . . . ? C32 C33 C34 O13 174.4(9) . . . . ? C33 C34 C35 C36 -72.2(18) . . . . ? O13 C34 C35 C36 176.3(12) . . . . ? C33 C34 C35 O12 169.5(12) . . . . ? O13 C34 C35 O12 57.9(16) . . . . ? C34 C35 C36 O21 -48.8(18) . . . . ? O12 C35 C36 O21 75.5(13) . . . . ? C34 C35 C36 O28 61.0(16) . . . . ? O12 C35 C36 O28 -174.7(10) . . . . ? C27 O21 C36 C35 -144.3(11) . . . . ? C27 O21 C36 O28 109.4(11) . . . . ? C32 O28 C36 C35 -54.0(14) . . . . ? C32 O28 C36 O21 54.8(14) . . . . ? C42 O22 C38 C39 59.8(14) . . . . ? C42 O22 C38 C37 -173.5(12) . . . . ? O30 C37 C38 O22 -64.4(19) . . . . ? O30 C37 C38 C39 50(2) . . . . ? C6 O16 C39 C40 133.9(13) . . . . ? C6 O16 C39 C38 -109.7(13) . . . . ? O22 C38 C39 O16 -176.7(11) . . . . ? C37 C38 C39 O16 67.8(17) . . . . ? O22 C38 C39 C40 -59.0(14) . . . . ? C37 C38 C39 C40 -174.5(13) . . . . ? O16 C39 C40 C41 -178.4(12) . . . . ? C38 C39 C40 C41 67.0(15) . . . . ? O16 C39 C40 O1 -62.3(14) . . . . ? C38 C39 C40 O1 -176.8(10) . . . . ? C39 C40 C41 O14 -178.5(12) . . . . ? O1 C40 C41 O14 69.5(14) . . . . ? C39 C40 C41 C42 -62.4(15) . . . . ? O1 C40 C41 C42 -174.3(10) . . . . ? C38 O22 C42 C41 -65.5(15) . . . . ? C38 O22 C42 O15 63.4(16) . . . . ? C40 C41 C42 O22 63.8(16) . . . . ? O14 C41 C42 O22 179.5(12) . . . . ? C40 C41 C42 O15 -66.9(15) . . . . ? O14 C41 C42 O15 48.7(16) . . . . ? C33 O15 C42 O22 113.7(14) . . . . ? C33 O15 C42 C41 -115.6(13) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note 1: Data are Listed for all Voids in the Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.007 -0.020 558 216 ' ' 2 0.000 0.502 -0.027 638 272 ' ' 3 0.500 1.002 0.039 638 272 ' ' 4 0.500 0.507 0.015 558 216 ' ' _platon_squeeze_details # Note 2: From other experimental data, the expect formula for the # crystal is C42 H70 O35, C11H12N2O5Cl2, 6H2O # The missing atoms add up to C44H96N8O44Cl8 in the Unit Cell. # These correspond to 904 electrons, comparable with the determined # value of 976 electrons by SQUEEZE. Conversely the total volume of # 1196 A would allow a volume of about 23 A per non-hydrogen atom. ; ; _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.570 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.099 # ===== END ===== #