# 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_new #TrackingRef 'new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H64 N8 O14' _chemical_formula_sum 'C44 H64 N8 O14' _chemical_formula_weight 929.03 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 '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 P2(1) _symmetry_space_group_name_Hall 'P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.639(2) _cell_length_b 10.4737(16) _cell_length_c 18.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.117(7) _cell_angle_gamma 90.00 _cell_volume 2490.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 560 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 13.24 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9853 _exptl_absorpt_correction_T_max 0.9889 _exptl_absorpt_process_details ' SADABS (Bruker,2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11623 _diffrn_reflns_av_R_equivalents 0.1175 _diffrn_reflns_av_sigmaI/netI 0.2170 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.41 _reflns_number_total 6534 _reflns_number_gt 2719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. ; _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^)+(0.1000P)^2^+0.1765P] 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 -2(3) _refine_ls_number_reflns 6534 _refine_ls_number_parameters 609 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2144 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2396 _refine_ls_wR_factor_gt 0.1678 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.015 _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 C1A C 0.3012(15) 1.0424(14) 0.1522(8) 0.123(7) Uani 1 1 d . . . H1A1 H 0.2781 1.1262 0.1385 0.184 Uiso 1 1 calc R . . H1A2 H 0.3724 1.0469 0.1699 0.184 Uiso 1 1 calc R . . H1A3 H 0.2556 1.0100 0.1887 0.184 Uiso 1 1 calc R . . C2A C 0.3833(12) 0.9881(15) 0.0380(8) 0.116(6) Uani 1 1 d . . . H2A1 H 0.3735 1.0731 0.0202 0.175 Uiso 1 1 calc R . . H2A2 H 0.3800 0.9284 -0.0006 0.175 Uiso 1 1 calc R . . H2A3 H 0.4510 0.9819 0.0609 0.175 Uiso 1 1 calc R . . C3A C 0.2975(14) 0.9579(13) 0.0909(8) 0.085(4) Uani 1 1 d . . . C4A C 0.1887(12) 0.9449(14) 0.0581(8) 0.105(5) Uani 1 1 d . . . H4A1 H 0.1395 0.9166 0.0936 0.157 Uiso 1 1 calc R . . H4A2 H 0.1911 0.8838 0.0201 0.157 Uiso 1 1 calc R . . H4A3 H 0.1664 1.0262 0.0398 0.157 Uiso 1 1 calc R . . C5A C 0.3260(8) 0.7250(12) 0.0838(7) 0.054(3) Uani 1 1 d . . . C6A C 0.3493(9) 0.4935(10) 0.0998(6) 0.053(3) Uani 1 1 d . . . H6A H 0.3707 0.4962 0.0498 0.063 Uiso 1 1 calc R . . C7A C 0.4273(10) 0.4137(11) 0.1395(7) 0.078(4) Uani 1 1 d . . . H7A1 H 0.4964 0.4511 0.1356 0.117 Uiso 1 1 calc R . . H7A2 H 0.4284 0.3291 0.1198 0.117 Uiso 1 1 calc R . . H7A3 H 0.4074 0.4094 0.1886 0.117 Uiso 1 1 calc R . . C8A C 0.2382(9) 0.4355(10) 0.1036(7) 0.047(3) Uani 1 1 d . . . C9A C 0.1129(8) 0.2993(9) 0.0344(5) 0.036(3) Uani 1 1 d . . . C10A C 0.0911(9) 0.2662(11) -0.0340(6) 0.057(3) Uani 1 1 d . . . H10A H 0.1344 0.2962 -0.0702 0.068 Uiso 1 1 calc R . . C11A C 0.0085(10) 0.1912(11) -0.0503(6) 0.060(3) Uani 1 1 d . . . H11A H -0.0030 0.1675 -0.0974 0.072 Uiso 1 1 calc R . . C12A C -0.0609(8) 0.1479(10) 0.0029(6) 0.049(3) Uani 1 1 d . . . H12A H -0.1185 0.0961 -0.0079 0.059 Uiso 1 1 calc R . . C13A C -0.0393(8) 0.1863(9) 0.0728(5) 0.043(3) Uani 1 1 d . . . C14A C 0.0482(8) 0.2606(9) 0.0879(5) 0.037(3) Uani 1 1 d . . . H14A H 0.0629 0.2841 0.1345 0.044 Uiso 1 1 calc R . . C15A C -0.1111(11) 0.1419(12) 0.1312(6) 0.059(3) Uani 1 1 d . . . C16A C -0.2884(9) 0.0740(10) 0.1658(7) 0.060(4) Uani 1 1 d . . . H16A H -0.2529 0.0704 0.2121 0.072 Uiso 1 1 calc R . . C17A C -0.3796(12) 0.1611(14) 0.1742(9) 0.116(6) Uani 1 1 d . . . H17A H -0.3555 0.2416 0.1925 0.173 Uiso 1 1 calc R . . H17B H -0.4295 0.1242 0.2067 0.173 Uiso 1 1 calc R . . H17C H -0.4130 0.1741 0.1289 0.173 Uiso 1 1 calc R . . C18A C -0.3176(8) -0.0601(11) 0.1472(7) 0.052(3) Uani 1 1 d . . . C19A C -0.3619(10) -0.2682(11) 0.1922(5) 0.055(3) Uani 1 1 d . . . H19A H -0.4039 -0.2801 0.1488 0.066 Uiso 1 1 calc R . . C20A C -0.4255(11) -0.3211(13) 0.2572(7) 0.089(4) Uani 1 1 d . . . H20A H -0.3852 -0.3086 0.2999 0.133 Uiso 1 1 calc R . . H20B H -0.4387 -0.4106 0.2505 0.133 Uiso 1 1 calc R . . H20C H -0.4917 -0.2765 0.2609 0.133 Uiso 1 1 calc R . . C21A C -0.2612(12) -0.3420(13) 0.1857(6) 0.063(4) Uani 1 1 d . . . C22A C -0.1825(13) -0.5358(15) 0.1490(9) 0.130(7) Uani 1 1 d . . . H22A H -0.1281 -0.4912 0.1236 0.195 Uiso 1 1 calc R . . H22B H -0.2008 -0.6125 0.1239 0.195 Uiso 1 1 calc R . . H22C H -0.1572 -0.5572 0.1957 0.195 Uiso 1 1 calc R . . C1B C 0.6858(11) -0.5468(15) 0.4419(8) 0.104(5) Uani 1 1 d . . . H1B1 H 0.6689 -0.6263 0.4647 0.157 Uiso 1 1 calc R . . H1B2 H 0.6359 -0.5308 0.4044 0.157 Uiso 1 1 calc R . . H1B3 H 0.6825 -0.4789 0.4761 0.157 Uiso 1 1 calc R . . C2B C 0.8848(14) -0.5859(13) 0.4621(9) 0.125(6) Uani 1 1 d . . . H2B1 H 0.9518 -0.5836 0.4382 0.188 Uiso 1 1 calc R . . H2B2 H 0.8731 -0.6697 0.4811 0.188 Uiso 1 1 calc R . . H2B3 H 0.8848 -0.5247 0.5001 0.188 Uiso 1 1 calc R . . C3B C 0.7996(14) -0.6442(14) 0.3479(8) 0.115(6) Uani 1 1 d . . . H3B1 H 0.8687 -0.6448 0.3269 0.172 Uiso 1 1 calc R . . H3B2 H 0.7486 -0.6163 0.3133 0.172 Uiso 1 1 calc R . . H3B3 H 0.7819 -0.7287 0.3636 0.172 Uiso 1 1 calc R . . C4B C 0.7987(11) -0.5540(13) 0.4106(7) 0.074(4) Uani 1 1 d . . . C5B C 0.8303(9) -0.3222(11) 0.4162(7) 0.057(3) Uani 1 1 d . . . C6B C 0.8470(9) -0.0921(9) 0.4005(6) 0.051(3) Uani 1 1 d . . . H6B H 0.8671 -0.0957 0.4508 0.061 Uiso 1 1 calc R . . C7B C 0.9291(10) -0.0114(12) 0.3614(7) 0.084(4) Uani 1 1 d . . . H7B1 H 0.9987 -0.0346 0.3772 0.127 Uiso 1 1 calc R . . H7B2 H 0.9168 0.0774 0.3713 0.127 Uiso 1 1 calc R . . H7B3 H 0.9232 -0.0261 0.3112 0.127 Uiso 1 1 calc R . . C8B C 0.7386(8) -0.0317(10) 0.3954(6) 0.039(3) Uani 1 1 d . . . C9B C 0.6154(8) 0.1030(9) 0.4653(5) 0.035(2) Uani 1 1 d . . . C10B C 0.5477(9) 0.1446(10) 0.4123(6) 0.048(3) Uani 1 1 d . . . H10B H 0.5617 0.1234 0.3652 0.058 Uiso 1 1 calc R . . C11B C 0.4612(9) 0.2160(10) 0.4279(5) 0.047(3) Uani 1 1 d . . . C12B C 0.4401(9) 0.2503(11) 0.4979(6) 0.053(3) Uani 1 1 d . . . H12B H 0.3811 0.2996 0.5089 0.064 Uiso 1 1 calc R . . C13B C 0.5069(11) 0.2105(12) 0.5498(6) 0.070(4) Uani 1 1 d . . . H13B H 0.4939 0.2341 0.5966 0.084 Uiso 1 1 calc R . . C14B C 0.5935(10) 0.1359(11) 0.5345(6) 0.063(4) Uani 1 1 d . . . H14B H 0.6374 0.1078 0.5711 0.075 Uiso 1 1 calc R . . C15B C 0.3885(11) 0.2595(11) 0.3700(7) 0.063(3) Uani 1 1 d . . . C16B C 0.2111(11) 0.3258(14) 0.3353(8) 0.087(5) Uani 1 1 d . . . H16B H 0.2480 0.3313 0.2896 0.104 Uiso 1 1 calc R . . C17B C 0.1230(13) 0.2450(15) 0.3238(9) 0.125(6) Uani 1 1 d . . . H17D H 0.1398 0.1837 0.2877 0.188 Uiso 1 1 calc R . . H17E H 0.0635 0.2952 0.3089 0.188 Uiso 1 1 calc R . . H17F H 0.1061 0.2013 0.3672 0.188 Uiso 1 1 calc R . . C18B C 0.1821(9) 0.4618(12) 0.3552(8) 0.060(3) Uani 1 1 d . . . C19B C 0.1377(9) 0.6685(13) 0.3069(6) 0.062(3) Uani 1 1 d . . . H19B H 0.0954 0.6817 0.3498 0.074 Uiso 1 1 calc R . . C20B C 0.0750(11) 0.7200(14) 0.2425(7) 0.086(4) Uani 1 1 d . . . H20D H 0.1138 0.7034 0.1997 0.129 Uiso 1 1 calc R . . H20E H 0.0648 0.8104 0.2477 0.129 Uiso 1 1 calc R . . H20F H 0.0074 0.6783 0.2401 0.129 Uiso 1 1 calc R . . C21B C 0.2394(11) 0.7399(13) 0.3148(6) 0.062(3) Uani 1 1 d . . . C22B C 0.3175(15) 0.9327(18) 0.3509(10) 0.147(7) Uani 1 1 d . . . H22D H 0.3558 0.9106 0.3932 0.220 Uiso 1 1 calc R . . H22E H 0.2968 1.0208 0.3531 0.220 Uiso 1 1 calc R . . H22F H 0.3617 0.9194 0.3101 0.220 Uiso 1 1 calc R . . N1A N 0.3485(7) 0.6238(8) 0.1271(5) 0.060(3) Uani 1 1 d . . . H1A H 0.3624 0.6371 0.1712 0.072 Uiso 1 1 calc R . . N2A N 0.2067(7) 0.3706(7) 0.0467(4) 0.040(2) Uani 1 1 d . . . H2A H 0.2502 0.3720 0.0116 0.048 Uiso 1 1 calc R . . N3A N -0.2103(7) 0.1225(8) 0.1152(5) 0.049(2) Uani 1 1 d . . . H3A H -0.2309 0.1390 0.0726 0.058 Uiso 1 1 calc R . . N4A N -0.3431(7) -0.1346(8) 0.2025(4) 0.057(3) Uani 1 1 d . . . H4A H -0.3482 -0.1020 0.2443 0.068 Uiso 1 1 calc R . . N1B N 0.8472(8) -0.2223(8) 0.3727(5) 0.070(3) Uani 1 1 d . . . H1B H 0.8581 -0.2352 0.3282 0.084 Uiso 1 1 calc R . . N2B N 0.7092(6) 0.0315(7) 0.4544(4) 0.041(2) Uani 1 1 d . . . H2B H 0.7525 0.0283 0.4896 0.049 Uiso 1 1 calc R . . N3B N 0.2882(8) 0.2780(8) 0.3860(5) 0.060(3) Uani 1 1 d . . . H3B H 0.2675 0.2609 0.4285 0.072 Uiso 1 1 calc R . . N4B N 0.1580(8) 0.5344(9) 0.2994(5) 0.065(3) Uani 1 1 d . . . H4B H 0.1546 0.5002 0.2579 0.078 Uiso 1 1 calc R . . O1A O 0.3241(7) 0.8308(7) 0.1233(4) 0.071(2) Uani 1 1 d . . . O2A O 0.3150(7) 0.7148(8) 0.0220(5) 0.071(2) Uani 1 1 d . . . O3A O 0.1846(6) 0.4439(8) 0.1574(4) 0.065(2) Uani 1 1 d . . . O4A O -0.0754(8) 0.1270(11) 0.1914(5) 0.110(4) Uani 1 1 d . . . O5A O -0.3201(6) -0.1002(7) 0.0863(4) 0.062(2) Uani 1 1 d . . . O6A O -0.1773(8) -0.3041(9) 0.2059(5) 0.082(3) Uani 1 1 d . . . O7A O -0.2762(8) -0.4539(9) 0.1551(5) 0.098(3) Uani 1 1 d . . . O1B O 0.8230(6) -0.4279(7) 0.3765(4) 0.066(2) Uani 1 1 d . . . O2B O 0.8171(7) -0.3146(8) 0.4785(5) 0.082(3) Uani 1 1 d . . . O3B O 0.6838(6) -0.0390(8) 0.3424(4) 0.070(2) Uani 1 1 d . . . O4B O 0.4246(8) 0.2761(11) 0.3092(5) 0.108(4) Uani 1 1 d . . . O5B O 0.1787(6) 0.5033(7) 0.4152(4) 0.065(2) Uani 1 1 d . . . O6B O 0.3246(7) 0.7044(9) 0.2933(5) 0.090(3) Uani 1 1 d . . . O7B O 0.2250(9) 0.8541(10) 0.3452(5) 0.104(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.20(2) 0.046(9) 0.123(15) -0.025(9) 0.003(13) -0.004(10) C2A 0.129(15) 0.091(12) 0.129(15) 0.029(10) -0.028(12) -0.028(11) C3A 0.126(14) 0.044(9) 0.085(11) -0.002(8) -0.002(10) -0.025(9) C4A 0.120(14) 0.052(9) 0.142(16) 0.002(9) -0.040(11) 0.018(10) C5A 0.041(8) 0.055(9) 0.066(9) -0.002(8) -0.019(7) 0.000(6) C6A 0.060(9) 0.047(8) 0.050(8) -0.005(5) -0.014(6) 0.018(6) C7A 0.095(11) 0.050(8) 0.091(10) 0.015(7) -0.022(8) 0.012(7) C8A 0.042(8) 0.036(6) 0.062(9) -0.006(6) -0.015(6) 0.010(6) C9A 0.048(7) 0.031(6) 0.029(7) -0.007(5) -0.023(6) 0.016(5) C10A 0.060(9) 0.074(9) 0.035(8) -0.003(6) -0.003(6) 0.001(7) C11A 0.062(9) 0.074(9) 0.042(7) -0.023(6) -0.015(7) -0.002(7) C12A 0.037(7) 0.056(7) 0.053(8) -0.008(6) -0.006(6) -0.016(6) C13A 0.047(7) 0.040(6) 0.041(7) -0.009(5) -0.009(6) -0.004(6) C14A 0.043(7) 0.045(7) 0.023(6) -0.003(5) 0.010(5) -0.012(5) C15A 0.066(10) 0.073(9) 0.037(8) 0.012(6) 0.007(7) -0.005(7) C16A 0.053(8) 0.046(8) 0.081(9) -0.009(6) 0.028(7) -0.013(6) C17A 0.090(12) 0.082(11) 0.175(16) -0.016(11) 0.038(11) 0.003(10) C18A 0.055(8) 0.048(8) 0.054(9) -0.005(7) 0.011(6) 0.005(6) C19A 0.068(9) 0.062(8) 0.034(7) -0.012(6) 0.007(6) -0.029(7) C20A 0.094(10) 0.106(11) 0.065(9) -0.001(8) 0.006(8) -0.051(9) C21A 0.082(11) 0.068(10) 0.039(8) 0.005(7) 0.016(8) -0.013(9) C22A 0.142(16) 0.068(11) 0.18(2) -0.011(11) 0.057(13) 0.013(12) C1B 0.124(14) 0.082(11) 0.108(13) -0.003(9) 0.032(10) -0.020(10) C2B 0.176(18) 0.047(10) 0.152(17) 0.024(9) -0.026(14) 0.015(10) C3B 0.172(18) 0.055(10) 0.118(15) -0.012(9) 0.006(12) -0.005(9) C4B 0.086(11) 0.055(9) 0.082(11) 0.010(8) 0.019(8) 0.004(8) C5B 0.056(8) 0.048(8) 0.068(9) -0.003(8) 0.012(7) 0.008(6) C6B 0.068(9) 0.040(7) 0.045(7) 0.000(5) -0.007(6) 0.014(6) C7B 0.089(11) 0.061(9) 0.102(11) 0.009(7) 0.022(9) -0.014(8) C8B 0.041(7) 0.043(7) 0.034(7) 0.005(6) -0.005(6) -0.004(5) C9B 0.038(7) 0.036(6) 0.032(7) -0.001(5) 0.003(6) -0.001(5) C10B 0.059(8) 0.049(7) 0.036(7) -0.005(5) 0.011(6) -0.005(6) C11B 0.057(8) 0.046(7) 0.037(7) 0.001(5) -0.011(6) 0.012(6) C12B 0.044(7) 0.069(8) 0.048(8) -0.009(6) 0.007(6) 0.014(6) C13B 0.087(10) 0.086(10) 0.038(8) 0.001(6) 0.009(8) 0.022(8) C14B 0.074(10) 0.076(9) 0.039(8) 0.003(6) 0.006(7) -0.011(8) C15B 0.061(10) 0.065(9) 0.063(10) -0.015(7) 0.010(8) 0.007(7) C16B 0.076(11) 0.090(12) 0.095(12) -0.034(9) -0.050(9) 0.014(9) C17B 0.104(14) 0.074(11) 0.198(19) -0.022(11) -0.053(12) -0.008(11) C18B 0.045(8) 0.064(9) 0.071(10) -0.003(8) -0.020(7) 0.008(7) C19B 0.046(8) 0.103(11) 0.036(7) -0.017(7) -0.003(6) 0.003(8) C20B 0.093(11) 0.098(11) 0.067(9) -0.012(8) -0.026(8) 0.019(9) C21B 0.077(11) 0.068(9) 0.042(8) 0.003(7) -0.018(7) 0.011(8) C22B 0.166(19) 0.088(14) 0.19(2) -0.002(13) -0.039(15) -0.033(15) N1A 0.084(8) 0.044(6) 0.052(6) 0.001(5) -0.015(5) -0.001(5) N2A 0.046(6) 0.051(5) 0.024(5) -0.006(4) -0.004(4) -0.002(5) N3A 0.045(6) 0.057(6) 0.043(6) 0.002(4) 0.004(5) -0.014(5) N4A 0.087(8) 0.051(6) 0.031(6) -0.008(5) 0.025(5) -0.025(5) N1B 0.119(9) 0.041(6) 0.050(6) 0.004(5) 0.031(6) 0.008(6) N2B 0.044(6) 0.049(5) 0.030(5) -0.001(4) -0.007(4) 0.000(5) N3B 0.062(7) 0.053(6) 0.064(7) -0.002(5) -0.013(6) 0.011(5) N4B 0.097(9) 0.051(7) 0.045(7) -0.016(5) -0.011(6) 0.021(6) O1A 0.095(7) 0.051(6) 0.067(6) -0.005(5) -0.014(5) -0.003(5) O2A 0.094(7) 0.070(6) 0.050(6) 0.003(5) -0.023(5) 0.005(5) O3A 0.062(5) 0.104(7) 0.030(5) -0.028(4) 0.017(4) -0.026(5) O4A 0.086(7) 0.184(11) 0.061(7) 0.050(7) 0.008(6) -0.020(7) O5A 0.071(6) 0.075(6) 0.039(5) -0.006(4) 0.009(4) -0.015(4) O6A 0.071(7) 0.100(8) 0.074(6) -0.015(5) 0.007(5) 0.011(6) O7A 0.122(9) 0.065(7) 0.107(8) -0.020(6) 0.029(6) -0.021(6) O1B 0.096(7) 0.042(5) 0.059(6) 0.000(4) 0.018(5) 0.000(4) O2B 0.116(8) 0.070(6) 0.060(6) -0.006(5) 0.028(5) -0.018(5) O3B 0.068(6) 0.099(7) 0.042(6) -0.025(5) -0.006(5) 0.027(5) O4B 0.090(7) 0.161(10) 0.072(7) 0.032(6) 0.003(6) 0.013(7) O5B 0.090(7) 0.064(6) 0.043(5) -0.012(4) -0.009(5) 0.001(4) O6B 0.064(7) 0.112(8) 0.092(7) -0.019(6) 0.005(5) -0.003(6) O7B 0.140(11) 0.068(7) 0.105(8) -0.022(6) -0.024(7) 0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C3A 1.455(17) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C3A 1.506(17) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C3A O1A 1.502(16) . ? C3A C4A 1.512(17) . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C5A O2A 1.177(12) . ? C5A O1A 1.334(13) . ? C5A N1A 1.367(14) . ? C6A N1A 1.458(13) . ? C6A C7A 1.492(15) . ? C6A C8A 1.531(15) . ? C6A H6A 0.9800 . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A O3A 1.221(11) . ? C8A N2A 1.330(13) . ? C9A C10A 1.360(13) . ? C9A C14A 1.360(13) . ? C9A N2A 1.419(13) . ? C10A C11A 1.341(15) . ? C10A H10A 0.9300 . ? C11A C12A 1.408(14) . ? C11A H11A 0.9300 . ? C12A C13A 1.402(13) . ? C12A H12A 0.9300 . ? C13A C14A 1.381(13) . ? C13A C15A 1.501(14) . ? C14A H14A 0.9300 . ? C15A O4A 1.228(13) . ? C15A N3A 1.304(14) . ? C16A N3A 1.463(12) . ? C16A C17A 1.479(17) . ? C16A C18A 1.493(15) . ? C16A H16A 0.9800 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A O5A 1.220(12) . ? C18A N4A 1.340(13) . ? C19A N4A 1.433(12) . ? C19A C21A 1.494(17) . ? C19A C20A 1.566(14) . ? C19A H19A 0.9800 . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? C21A O6A 1.194(14) . ? C21A O7A 1.319(14) . ? C22A O7A 1.467(16) . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C1B C4B 1.547(15) . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C2B C4B 1.492(18) . ? C2B H2B1 0.9600 . ? C2B H2B2 0.9600 . ? C2B H2B3 0.9600 . ? C3B C4B 1.512(18) . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? C4B O1B 1.501(14) . ? C5B O2B 1.186(12) . ? C5B O1B 1.339(13) . ? C5B N1B 1.345(14) . ? C6B N1B 1.460(13) . ? C6B C8B 1.513(14) . ? C6B C7B 1.529(14) . ? C6B H6B 0.9800 . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B O3B 1.215(11) . ? C8B N2B 1.344(12) . ? C9B C14B 1.377(13) . ? C9B C10B 1.383(14) . ? C9B N2B 1.417(12) . ? C10B C11B 1.357(14) . ? C10B H10B 0.9300 . ? C11B C12B 1.393(13) . ? C11B C15B 1.495(16) . ? C12B C13B 1.354(15) . ? C12B H12B 0.9300 . ? C13B C14B 1.376(16) . ? C13B H13B 0.9300 . ? C14B H14B 0.9300 . ? C15B O4B 1.245(13) . ? C15B N3B 1.319(13) . ? C16B C17B 1.414(18) . ? C16B N3B 1.452(15) . ? C16B C18B 1.518(18) . ? C16B H16B 0.9800 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B O5B 1.211(13) . ? C18B N4B 1.331(14) . ? C19B N4B 1.435(14) . ? C19B C21B 1.495(17) . ? C19B C20B 1.543(16) . ? C19B H19B 0.9800 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B O6B 1.210(13) . ? C21B O7B 1.339(14) . ? C22B O7B 1.434(18) . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? N1A H1A 0.8600 . ? N2A H2A 0.8600 . ? N3A H3A 0.8600 . ? N4A H4A 0.8600 . ? N1B H1B 0.8600 . ? N2B H2B 0.8600 . ? N3B H3B 0.8600 . ? N4B H4B 0.8600 . ? 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 C3A C1A H1A1 109.5 . . ? C3A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C3A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3A C2A H2A1 109.5 . . ? C3A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C3A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C1A C3A O1A 102.2(12) . . ? C1A C3A C2A 111.9(14) . . ? O1A C3A C2A 107.0(12) . . ? C1A C3A C4A 113.9(15) . . ? O1A C3A C4A 106.8(10) . . ? C2A C3A C4A 113.9(14) . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? O2A C5A O1A 128.6(12) . . ? O2A C5A N1A 122.9(11) . . ? O1A C5A N1A 108.5(11) . . ? N1A C6A C7A 110.6(9) . . ? N1A C6A C8A 110.3(9) . . ? C7A C6A C8A 111.1(10) . . ? N1A C6A H6A 108.2 . . ? C7A C6A H6A 108.2 . . ? C8A C6A H6A 108.2 . . ? C6A C7A H7A1 109.5 . . ? C6A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C6A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? O3A C8A N2A 122.6(10) . . ? O3A C8A C6A 121.4(10) . . ? N2A C8A C6A 115.9(10) . . ? C10A C9A C14A 120.2(11) . . ? C10A C9A N2A 117.1(9) . . ? C14A C9A N2A 122.6(9) . . ? C11A C10A C9A 121.5(11) . . ? C11A C10A H10A 119.3 . . ? C9A C10A H10A 119.3 . . ? C10A C11A C12A 120.7(11) . . ? C10A C11A H11A 119.6 . . ? C12A C11A H11A 119.6 . . ? C13A C12A C11A 117.0(10) . . ? C13A C12A H12A 121.5 . . ? C11A C12A H12A 121.5 . . ? C14A C13A C12A 120.6(9) . . ? C14A C13A C15A 120.6(10) . . ? C12A C13A C15A 118.8(10) . . ? C9A C14A C13A 119.9(9) . . ? C9A C14A H14A 120.1 . . ? C13A C14A H14A 120.1 . . ? O4A C15A N3A 123.0(11) . . ? O4A C15A C13A 119.5(12) . . ? N3A C15A C13A 117.5(11) . . ? N3A C16A C17A 112.5(11) . . ? N3A C16A C18A 109.9(8) . . ? C17A C16A C18A 114.4(11) . . ? N3A C16A H16A 106.5 . . ? C17A C16A H16A 106.5 . . ? C18A C16A H16A 106.5 . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? O5A C18A N4A 121.5(10) . . ? O5A C18A C16A 123.3(11) . . ? N4A C18A C16A 115.2(11) . . ? N4A C19A C21A 112.1(10) . . ? N4A C19A C20A 109.0(9) . . ? C21A C19A C20A 108.6(10) . . ? N4A C19A H19A 109.0 . . ? C21A C19A H19A 109.0 . . ? C20A C19A H19A 109.0 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? O6A C21A O7A 124.1(14) . . ? O6A C21A C19A 123.9(13) . . ? O7A C21A C19A 111.9(13) . . ? O7A C22A H22A 109.5 . . ? O7A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? O7A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C4B C1B H1B1 109.5 . . ? C4B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C4B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C4B C2B H2B1 109.5 . . ? C4B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C4B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C4B C3B H3B1 109.5 . . ? C4B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B O1B 109.0(11) . . ? C2B C4B C3B 111.1(13) . . ? O1B C4B C3B 102.4(10) . . ? C2B C4B C1B 115.8(13) . . ? O1B C4B C1B 108.0(10) . . ? C3B C4B C1B 109.6(13) . . ? O2B C5B O1B 126.6(11) . . ? O2B C5B N1B 124.9(11) . . ? O1B C5B N1B 108.3(10) . . ? N1B C6B C8B 111.7(10) . . ? N1B C6B C7B 110.0(8) . . ? C8B C6B C7B 110.7(9) . . ? N1B C6B H6B 108.1 . . ? C8B C6B H6B 108.1 . . ? C7B C6B H6B 108.1 . . ? C6B C7B H7B1 109.5 . . ? C6B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C6B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? O3B C8B N2B 123.4(10) . . ? O3B C8B C6B 122.7(10) . . ? N2B C8B C6B 113.9(10) . . ? C14B C9B C10B 118.5(10) . . ? C14B C9B N2B 116.1(10) . . ? C10B C9B N2B 125.4(9) . . ? C11B C10B C9B 121.0(9) . . ? C11B C10B H10B 119.5 . . ? C9B C10B H10B 119.5 . . ? C10B C11B C12B 120.2(10) . . ? C10B C11B C15B 120.3(10) . . ? C12B C11B C15B 119.5(11) . . ? C13B C12B C11B 118.8(10) . . ? C13B C12B H12B 120.6 . . ? C11B C12B H12B 120.6 . . ? C12B C13B C14B 121.3(11) . . ? C12B C13B H13B 119.3 . . ? C14B C13B H13B 119.3 . . ? C13B C14B C9B 120.1(11) . . ? C13B C14B H14B 120.0 . . ? C9B C14B H14B 120.0 . . ? O4B C15B N3B 123.0(13) . . ? O4B C15B C11B 119.1(12) . . ? N3B C15B C11B 117.9(11) . . ? C17B C16B N3B 114.9(14) . . ? C17B C16B C18B 114.1(12) . . ? N3B C16B C18B 108.9(10) . . ? C17B C16B H16B 106.1 . . ? N3B C16B H16B 106.1 . . ? C18B C16B H16B 106.1 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? O5B C18B N4B 121.5(12) . . ? O5B C18B C16B 125.1(13) . . ? N4B C18B C16B 113.4(12) . . ? N4B C19B C21B 110.2(10) . . ? N4B C19B C20B 110.9(10) . . ? C21B C19B C20B 110.1(11) . . ? N4B C19B H19B 108.5 . . ? C21B C19B H19B 108.5 . . ? C20B C19B H19B 108.5 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O6B C21B O7B 122.7(13) . . ? O6B C21B C19B 125.4(13) . . ? O7B C21B C19B 111.8(13) . . ? O7B C22B H22D 109.5 . . ? O7B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? O7B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C5A N1A C6A 121.2(10) . . ? C5A N1A H1A 119.4 . . ? C6A N1A H1A 119.4 . . ? C8A N2A C9A 130.5(9) . . ? C8A N2A H2A 114.8 . . ? C9A N2A H2A 114.8 . . ? C15A N3A C16A 123.6(10) . . ? C15A N3A H3A 118.2 . . ? C16A N3A H3A 118.2 . . ? C18A N4A C19A 120.2(9) . . ? C18A N4A H4A 119.9 . . ? C19A N4A H4A 119.9 . . ? C5B N1B C6B 120.5(9) . . ? C5B N1B H1B 119.8 . . ? C6B N1B H1B 119.8 . . ? C8B N2B C9B 127.7(9) . . ? C8B N2B H2B 116.1 . . ? C9B N2B H2B 116.1 . . ? C15B N3B C16B 123.0(11) . . ? C15B N3B H3B 118.5 . . ? C16B N3B H3B 118.5 . . ? C18B N4B C19B 121.5(10) . . ? C18B N4B H4B 119.3 . . ? C19B N4B H4B 119.3 . . ? C5A O1A C3A 120.9(10) . . ? C21A O7A C22A 116.0(13) . . ? C5B O1B C4B 120.2(9) . . ? C21B O7B C22B 115.7(13) . . ? 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 N1A C6A C8A O3A -47.2(14) . . . . ? C7A C6A C8A O3A 75.9(14) . . . . ? N1A C6A C8A N2A 136.2(9) . . . . ? C7A C6A C8A N2A -100.7(11) . . . . ? C14A C9A C10A C11A -2.6(16) . . . . ? N2A C9A C10A C11A 175.2(10) . . . . ? C9A C10A C11A C12A 2.3(18) . . . . ? C10A C11A C12A C13A -0.2(17) . . . . ? C11A C12A C13A C14A -1.6(15) . . . . ? C11A C12A C13A C15A -179.8(10) . . . . ? C10A C9A C14A C13A 0.7(14) . . . . ? N2A C9A C14A C13A -176.9(9) . . . . ? C12A C13A C14A C9A 1.4(15) . . . . ? C15A C13A C14A C9A 179.6(10) . . . . ? C14A C13A C15A O4A -28.0(17) . . . . ? C12A C13A C15A O4A 150.2(12) . . . . ? C14A C13A C15A N3A 151.2(10) . . . . ? C12A C13A C15A N3A -30.6(15) . . . . ? N3A C16A C18A O5A -32.7(16) . . . . ? C17A C16A C18A O5A 95.1(14) . . . . ? N3A C16A C18A N4A 148.5(10) . . . . ? C17A C16A C18A N4A -83.8(14) . . . . ? N4A C19A C21A O6A 19.6(15) . . . . ? C20A C19A C21A O6A -100.9(13) . . . . ? N4A C19A C21A O7A -160.5(9) . . . . ? C20A C19A C21A O7A 79.1(12) . . . . ? N1B C6B C8B O3B -45.2(14) . . . . ? C7B C6B C8B O3B 77.8(14) . . . . ? N1B C6B C8B N2B 135.6(9) . . . . ? C7B C6B C8B N2B -101.4(11) . . . . ? C14B C9B C10B C11B -0.3(15) . . . . ? N2B C9B C10B C11B -178.0(9) . . . . ? C9B C10B C11B C12B 1.0(16) . . . . ? C9B C10B C11B C15B -179.6(10) . . . . ? C10B C11B C12B C13B -0.4(17) . . . . ? C15B C11B C12B C13B -179.8(11) . . . . ? C11B C12B C13B C14B -1.0(18) . . . . ? C12B C13B C14B C9B 1.7(18) . . . . ? C10B C9B C14B C13B -1.0(15) . . . . ? N2B C9B C14B C13B 176.9(10) . . . . ? C10B C11B C15B O4B -28.3(17) . . . . ? C12B C11B C15B O4B 151.1(11) . . . . ? C10B C11B C15B N3B 151.4(11) . . . . ? C12B C11B C15B N3B -29.2(15) . . . . ? C17B C16B C18B O5B 97.1(16) . . . . ? N3B C16B C18B O5B -32.7(19) . . . . ? C17B C16B C18B N4B -81.8(16) . . . . ? N3B C16B C18B N4B 148.4(12) . . . . ? N4B C19B C21B O6B 25.1(16) . . . . ? C20B C19B C21B O6B -97.6(14) . . . . ? N4B C19B C21B O7B -159.0(9) . . . . ? C20B C19B C21B O7B 78.4(12) . . . . ? O2A C5A N1A C6A -6.5(17) . . . . ? O1A C5A N1A C6A 176.0(9) . . . . ? C7A C6A N1A C5A 149.1(11) . . . . ? C8A C6A N1A C5A -87.6(12) . . . . ? O3A C8A N2A C9A -0.9(17) . . . . ? C6A C8A N2A C9A 175.6(9) . . . . ? C10A C9A N2A C8A 165.9(10) . . . . ? C14A C9A N2A C8A -16.4(16) . . . . ? O4A C15A N3A C16A -3.6(18) . . . . ? C13A C15A N3A C16A 177.3(9) . . . . ? C17A C16A N3A C15A 122.7(13) . . . . ? C18A C16A N3A C15A -108.5(13) . . . . ? O5A C18A N4A C19A 7.5(17) . . . . ? C16A C18A N4A C19A -173.6(10) . . . . ? C21A C19A N4A C18A 78.6(13) . . . . ? C20A C19A N4A C18A -161.1(11) . . . . ? O2B C5B N1B C6B -2.0(19) . . . . ? O1B C5B N1B C6B 173.3(10) . . . . ? C8B C6B N1B C5B -92.3(13) . . . . ? C7B C6B N1B C5B 144.4(11) . . . . ? O3B C8B N2B C9B -2.5(16) . . . . ? C6B C8B N2B C9B 176.8(9) . . . . ? C14B C9B N2B C8B 166.8(9) . . . . ? C10B C9B N2B C8B -15.5(15) . . . . ? O4B C15B N3B C16B -3.3(18) . . . . ? C11B C15B N3B C16B 177.0(10) . . . . ? C17B C16B N3B C15B 122.2(15) . . . . ? C18B C16B N3B C15B -108.4(13) . . . . ? O5B C18B N4B C19B 6.6(18) . . . . ? C16B C18B N4B C19B -174.4(11) . . . . ? C21B C19B N4B C18B 77.8(13) . . . . ? C20B C19B N4B C18B -160.0(11) . . . . ? O2A C5A O1A C3A 5.0(18) . . . . ? N1A C5A O1A C3A -177.8(10) . . . . ? C1A C3A O1A C5A 178.1(11) . . . . ? C2A C3A O1A C5A -64.2(15) . . . . ? C4A C3A O1A C5A 58.2(15) . . . . ? O6A C21A O7A C22A 2.4(18) . . . . ? C19A C21A O7A C22A -177.5(10) . . . . ? O2B C5B O1B C4B -1.8(18) . . . . ? N1B C5B O1B C4B -177.0(10) . . . . ? C2B C4B O1B C5B -61.5(14) . . . . ? C3B C4B O1B C5B -179.2(11) . . . . ? C1B C4B O1B C5B 65.1(15) . . . . ? O6B C21B O7B C22B -0.1(18) . . . . ? C19B C21B O7B C22B -176.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.720 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.173 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.044 _vrf_PLAT029_new ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.821 RESPONSE: Even though crystal data was collected up to 0.73 \%A resolution, the crystal (the largest available) still diffracted quite weakly at high angle. On repeated recrystallisation we could get only small sized crystals. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 923387'