Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Consiglia Tedesco' _publ_contact_author_address ; Chemistry University of Salerno via S. Allende 43 Baronissi I-84081 ITALY ; _publ_contact_author_email CTEDESCO@UNISA.IT _publ_section_title ; Interconnected Water Channels and Isolated Hydrophobic Cavities in a Calixarene-Based, Nanoporous Supramolecular Architecture ; loop_ _publ_author_name 'Consiglia Tedesco' 'L. Gregoli' 'I. Immediata' 'Attilio Immirzi' 'Placido Neri' 'Vincenzo Vitagliano' data_ce10 _database_code_depnum_ccdc_archive 'CCDC 263811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C38 H44.67 O6.33), 3.22 (H2 O)' _chemical_formula_sum 'C38 H51.12 O9.56' _chemical_formula_weight 660.72 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P n -3 n' _symmetry_space_group_name_Hall '-P 4a 2bc 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 36.412(4) _cell_length_b 36.412(4) _cell_length_c 36.412(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 48276(9) _cell_formula_units_Z 48 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description hexagonal _exptl_crystal_colour white _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.103 #_exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17260 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.93931 _diffrn_radiation_type synchrotron _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3386 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min 2 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.58 _reflns_number_total 3386 _reflns_number_gt 3303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'TRY (Immirzi, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.2 (CCDC, 2004)' _computing_publication_material ? _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^)+(0.2000P)^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_number_reflns 3386 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.3841 _refine_ls_wR_factor_gt 0.3804 _refine_ls_goodness_of_fit_ref 2.105 _refine_ls_restrained_S_all 2.105 _refine_ls_shift/su_max 0.408 _refine_ls_shift/su_mean 0.003 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 C1 C 0.87802(12) 0.06531(13) 0.62700(11) 0.172(2) Uani 1 1 d . . . H1A H 0.8973 0.0527 0.6404 0.207 Uiso 1 1 calc R . . H1B H 0.8749 0.0894 0.6380 0.207 Uiso 1 1 calc R . . C2 C 0.89035(10) 0.07019(12) 0.58717(10) 0.156(2) Uani 1 1 d . . . C3 C 0.91161(9) 0.04201(11) 0.57056(11) 0.151(2) Uani 1 1 d . . . H3 H 0.9185 0.0214 0.5840 0.182 Uiso 1 1 calc R . . C4 C 0.92177(10) 0.04563(10) 0.53474(12) 0.152(2) Uani 1 1 d . . . C5 C 0.91051(9) 0.07450(11) 0.51330(10) 0.151(2) Uani 1 1 d . . . H5 H 0.9168 0.0753 0.4886 0.182 Uiso 1 1 calc R . . C6 C 0.88965(9) 0.10257(10) 0.52860(11) 0.149(2) Uani 1 1 d . . . C7 C 0.88094(10) 0.09990(11) 0.56633(13) 0.154(2) Uani 1 1 d . . . C8 C 0.87622(9) 0.13411(10) 0.50592(12) 0.154(2) Uani 1 1 d . . . H8A H 0.8946 0.1398 0.4875 0.185 Uiso 1 1 calc R . . H8B H 0.8738 0.1555 0.5217 0.185 Uiso 1 1 calc R . . C9 C 0.84013(10) 0.12754(9) 0.48691(12) 0.148(2) Uani 1 1 d . . . C10 C 0.80601(12) 0.13099(8) 0.50342(10) 0.143(2) Uani 1 1 d . . . C11 C 0.77348(10) 0.12543(8) 0.48496(12) 0.143(2) Uani 1 1 d . . . C12 C 0.77432(10) 0.11534(10) 0.44956(13) 0.152(2) Uani 1 1 d . . . H12 H 0.7524 0.1116 0.4371 0.183 Uiso 1 1 calc R . . C13 C 0.80794(11) 0.11026(12) 0.43088(12) 0.159(2) Uani 1 1 d . . . C14 C 0.84019(11) 0.11687(10) 0.44953(13) 0.155(2) Uani 1 1 d . . . H14 H 0.8625 0.1143 0.4373 0.186 Uiso 1 1 calc R . . C15 C 0.73609(9) 0.12868(10) 0.50397(10) 0.149(2) Uani 1 1 d . . . H15A H 0.7363 0.1501 0.5199 0.179 Uiso 1 1 calc R . . H15B H 0.7173 0.1324 0.4855 0.179 Uiso 1 1 calc R . . C16 C 0.72652(9) 0.09543(9) 0.52631(10) 0.139(2) Uani 1 1 d . . . C17 C 0.73258(8) 0.09428(10) 0.56416(11) 0.142(2) Uani 1 1 d . . . C18 C 0.72739(9) 0.06236(11) 0.58457(9) 0.144(2) Uani 1 1 d . . . C19 C 0.71221(7) 0.03208(10) 0.56666(10) 0.139(2) Uani 1 1 d . . . H19 H 0.7081 0.0107 0.5800 0.167 Uiso 1 1 calc R . . C20 C 0.70287(8) 0.03278(10) 0.52902(9) 0.137(2) Uani 1 1 d . . . C21 C 0.71152(8) 0.06429(10) 0.50994(10) 0.138(2) Uani 1 1 d . . . H21 H 0.7071 0.0648 0.4848 0.166 Uiso 1 1 calc R . . C22 C 0.73800(10) 0.05922(11) 0.62469(9) 0.155(2) Uani 1 1 d . . . H22A H 0.7195 0.0450 0.6375 0.186 Uiso 1 1 calc R . . H22B H 0.7384 0.0836 0.6355 0.186 Uiso 1 1 calc R . . C23 C 0.77529(10) 0.04118(13) 0.63022(9) 0.150(2) Uani 1 1 d . . . C24 C 0.80763(11) 0.06159(13) 0.62820(9) 0.151(2) Uani 1 1 d . . . C25 C 0.84265(11) 0.04397(15) 0.63127(10) 0.156(2) Uani 1 1 d . . . C26 C 0.84334(12) 0.00786(16) 0.63694(10) 0.163(2) Uani 1 1 d . . . H26 H 0.8661 -0.0036 0.6392 0.195 Uiso 1 1 calc R . . C27 C 0.81160(13) -0.01393(12) 0.63971(11) 0.164(2) Uani 1 1 d . . . C28 C 0.77812(11) 0.00389(14) 0.63625(10) 0.160(2) Uani 1 1 d . . . H28 H 0.7567 -0.0099 0.6381 0.192 Uiso 1 1 calc R . . C29 C 0.68235(9) 0.00111(10) 0.51163(9) 0.143(2) Uani 1 1 d . . . C30 C 0.81404(14) -0.05542(17) 0.64906(18) 0.204(3) Uani 1 1 d . . . O1 O 0.94449(8) 0.01875(8) 0.51926(8) 0.178(2) Uani 1 1 d . . . H1 H 0.9489 0.0029 0.5346 0.267 Uiso 1 1 calc R . . O2 O 0.86345(7) 0.12876(7) 0.58401(7) 0.168(2) Uani 1 1 d . . . H2 H 0.8600 0.1455 0.5694 0.252 Uiso 1 1 calc R . . O3 O 0.80651(7) 0.14276(8) 0.54013(8) 0.172(2) Uani 1 1 d . . . H3A H 0.7854 0.1444 0.5478 0.258 Uiso 1 1 calc R . . O4 O 0.80705(7) 0.10060(12) 0.39504(9) 0.207(2) Uani 1 1 d . . . H4 H 0.8281 0.0978 0.3875 0.311 Uiso 1 1 calc R . . O5 O 0.74493(7) 0.12602(7) 0.58106(7) 0.163(2) Uani 1 1 d . . . O6 O 0.80616(7) 0.09820(10) 0.62189(8) 0.177(2) Uani 1 1 d . . . C31 C 0.71535(13) 0.14936(14) 0.59430(16) 0.197(2) Uani 1 1 d . . . H31A H 0.7255 0.1707 0.6059 0.295 Uiso 1 1 calc R . . H31B H 0.7008 0.1360 0.6117 0.295 Uiso 1 1 calc R . . H31C H 0.7002 0.1568 0.5740 0.295 Uiso 1 1 calc R . . C32 C 0.80511(19) 0.1206(2) 0.6541(2) 0.238(3) Uani 1 1 d . . . H32A H 0.8041 0.1460 0.6470 0.357 Uiso 1 1 calc R . . H32B H 0.8268 0.1164 0.6685 0.357 Uiso 1 1 calc R . . H32C H 0.7838 0.1146 0.6683 0.357 Uiso 1 1 calc R . . C33 C 0.6985(3) -0.03536(18) 0.5238(3) 0.313(6) Uani 1 1 d . . . H33A H 0.6969 -0.0374 0.5500 0.469 Uiso 0.50 1 calc PR . . H33B H 0.7238 -0.0367 0.5164 0.469 Uiso 0.50 1 calc PR . . H33C H 0.6851 -0.0551 0.5126 0.469 Uiso 0.50 1 calc PR . . H33D H 0.7069 -0.0487 0.5026 0.469 Uiso 0.50 1 calc PR . . H33E H 0.6800 -0.0494 0.5362 0.469 Uiso 0.50 1 calc PR . . H33F H 0.7187 -0.0310 0.5401 0.469 Uiso 0.50 1 calc PR . . C34 C 0.6874(2) -0.00264(18) 0.47189(17) 0.242(4) Uani 1 1 d . . . H34A H 0.6775 0.0186 0.4597 0.363 Uiso 0.50 1 calc PR . . H34B H 0.6749 -0.0243 0.4634 0.363 Uiso 0.50 1 calc PR . . H34C H 0.7131 -0.0047 0.4665 0.363 Uiso 0.50 1 calc PR . . H34D H 0.6995 -0.0255 0.4667 0.363 Uiso 0.50 1 calc PR . . H34E H 0.7021 0.0173 0.4630 0.363 Uiso 0.50 1 calc PR . . H34F H 0.6639 -0.0022 0.4600 0.363 Uiso 0.50 1 calc PR . . C35 C 0.64415(16) 0.0035(3) 0.5220(3) 0.342(7) Uani 1 1 d . . . H35A H 0.6421 0.0022 0.5482 0.513 Uiso 0.50 1 calc PR . . H35B H 0.6309 -0.0165 0.5111 0.513 Uiso 0.50 1 calc PR . . H35C H 0.6341 0.0263 0.5134 0.513 Uiso 0.50 1 calc PR . . H35D H 0.6293 0.0058 0.5003 0.513 Uiso 0.50 1 calc PR . . H35E H 0.6405 0.0246 0.5374 0.513 Uiso 0.50 1 calc PR . . H35F H 0.6372 -0.0183 0.5351 0.513 Uiso 0.50 1 calc PR . . C36 C 0.8495(3) -0.0721(3) 0.6366(6) 0.401(11) Uani 1 1 d . . . H36A H 0.8521 -0.0688 0.6106 0.601 Uiso 0.50 1 calc PR . . H36B H 0.8495 -0.0979 0.6423 0.601 Uiso 0.50 1 calc PR . . H36C H 0.8696 -0.0604 0.6490 0.601 Uiso 0.50 1 calc PR . . H36D H 0.8620 -0.0826 0.6573 0.601 Uiso 0.50 1 calc PR . . H36E H 0.8646 -0.0535 0.6257 0.601 Uiso 0.50 1 calc PR . . H36F H 0.8446 -0.0910 0.6189 0.601 Uiso 0.50 1 calc PR . . C37 C 0.78465(19) -0.07642(16) 0.6299(2) 0.230(3) Uani 1 1 d . . . H37A H 0.7886 -0.0752 0.6038 0.346 Uiso 0.50 1 calc PR . . H37B H 0.7611 -0.0660 0.6357 0.346 Uiso 0.50 1 calc PR . . H37C H 0.7853 -0.1016 0.6376 0.346 Uiso 0.50 1 calc PR . . H37D H 0.7681 -0.0867 0.6476 0.346 Uiso 0.50 1 calc PR . . H37E H 0.7955 -0.0958 0.6157 0.346 Uiso 0.50 1 calc PR . . H37F H 0.7714 -0.0603 0.6138 0.346 Uiso 0.50 1 calc PR . . C38 C 0.8124(7) -0.0597(3) 0.6879(3) 0.508(18) Uani 1 1 d . . . H38A H 0.7893 -0.0505 0.6968 0.762 Uiso 0.50 1 calc PR . . H38B H 0.8321 -0.0461 0.6991 0.762 Uiso 0.50 1 calc PR . . H38C H 0.8146 -0.0852 0.6941 0.762 Uiso 0.50 1 calc PR . . H38D H 0.8347 -0.0707 0.6965 0.762 Uiso 0.50 1 calc PR . . H38E H 0.7919 -0.0751 0.6942 0.762 Uiso 0.50 1 calc PR . . H38F H 0.8094 -0.0360 0.6992 0.762 Uiso 0.50 1 calc PR . . OW1 O 0.94889(14) -0.05111(14) 0.55111(14) 0.258(3) Uiso 1 3 d S . . OW2 O 0.7500 0.2500 0.7500 0.48(2) Uiso 1 8 d S . . OW3 O 0.7261(9) 0.1778(8) 0.6821(8) 0.305(17) Uiso 0.26(2) 1 d P . . OW4 O 0.7500 0.1012(8) 0.7500 0.443(12) Uiso 1 4 d S . . OW5 O 0.7285(7) 0.1981(7) 0.3991(10) 0.59(2) Uiso 1.00(5) 1 d . . . OW6 O 0.6409(8) 0.2397(8) 0.6744(7) 0.447(17) Uiso 0.61(3) 1 d P . . OW7 O 0.7500 0.1563(11) 0.7500 0.40(2) Uiso 0.61(5) 4 d SP . . OW8 O 0.7233(17) 0.0540(16) 0.764(3) 0.49(4) Uiso 0.28(3) 1 d P . . OW9 O 0.7220(10) 0.2551(11) 0.5595(10) 0.51(3) Uiso 0.55(6) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.155(3) 0.212(4) 0.149(4) -0.009(2) -0.0191(19) -0.018(2) C2 0.127(3) 0.181(4) 0.160(4) 0.005(3) -0.0133(19) -0.025(2) C3 0.136(3) 0.167(3) 0.151(4) 0.018(2) -0.0134(18) -0.003(2) C4 0.133(3) 0.159(3) 0.162(4) 0.009(2) -0.007(2) 0.0003(19) C5 0.135(3) 0.157(3) 0.161(3) -0.004(2) -0.0041(17) -0.006(2) C6 0.127(3) 0.148(3) 0.171(4) 0.008(2) -0.0132(19) -0.0280(18) C7 0.144(3) 0.147(3) 0.172(4) -0.006(3) -0.017(2) -0.0204(19) C8 0.138(3) 0.149(3) 0.175(3) 0.012(2) -0.0059(19) -0.0167(16) C9 0.144(4) 0.130(3) 0.171(4) 0.0090(18) 0.002(2) -0.0073(15) C10 0.154(4) 0.130(3) 0.145(3) -0.0047(16) 0.006(2) -0.0004(15) C11 0.138(3) 0.126(3) 0.164(4) 0.0075(17) 0.002(2) -0.0002(14) C12 0.149(3) 0.158(3) 0.150(3) 0.002(2) -0.004(2) 0.0036(18) C13 0.140(4) 0.177(4) 0.161(4) 0.003(2) 0.016(2) 0.0077(19) C14 0.139(3) 0.157(3) 0.170(4) 0.003(2) 0.008(2) -0.0063(17) C15 0.130(3) 0.152(3) 0.166(3) -0.0077(18) 0.0015(17) 0.0101(15) C16 0.126(3) 0.152(3) 0.139(3) -0.0024(19) 0.0032(15) 0.0081(16) C17 0.123(3) 0.149(3) 0.153(4) -0.014(2) 0.0016(15) 0.0025(16) C18 0.127(3) 0.175(4) 0.131(3) -0.001(2) 0.0060(16) 0.0040(18) C19 0.118(3) 0.157(3) 0.143(3) -0.0060(18) 0.0025(15) 0.0001(15) C20 0.120(3) 0.154(3) 0.136(3) -0.004(2) 0.0025(15) 0.0103(16) C21 0.124(3) 0.143(3) 0.148(3) -0.006(2) -0.0006(15) 0.0061(16) C22 0.137(3) 0.179(3) 0.150(3) -0.0135(19) 0.0074(16) -0.004(2) C23 0.141(4) 0.186(4) 0.123(3) -0.0114(18) -0.0051(14) -0.002(3) C24 0.130(4) 0.180(4) 0.144(3) -0.012(2) -0.0136(15) -0.001(3) C25 0.158(4) 0.181(5) 0.128(3) -0.0045(19) -0.0131(16) -0.011(3) C26 0.154(3) 0.191(5) 0.143(3) -0.002(2) -0.0113(18) 0.010(3) C27 0.167(4) 0.166(4) 0.160(3) 0.004(2) -0.019(2) -0.004(3) C28 0.147(4) 0.185(5) 0.148(3) 0.002(2) -0.0141(17) -0.009(2) C29 0.131(3) 0.154(3) 0.145(3) -0.0005(18) 0.0052(15) -0.0027(18) C30 0.182(4) 0.195(5) 0.236(6) 0.004(4) -0.043(3) 0.004(3) O1 0.167(3) 0.185(3) 0.181(3) 0.0199(16) 0.0070(14) 0.0219(17) O2 0.165(3) 0.158(3) 0.182(3) -0.0259(15) -0.0031(13) -0.0112(13) O3 0.160(2) 0.179(3) 0.176(3) -0.0155(15) 0.0024(13) -0.0081(12) O4 0.155(3) 0.310(5) 0.157(3) -0.029(2) 0.0101(14) 0.0126(19) O5 0.149(3) 0.168(3) 0.172(3) -0.0203(14) 0.0048(12) -0.0011(14) O6 0.158(3) 0.168(3) 0.206(3) -0.0061(19) -0.0175(14) -0.0102(15) C31 0.185(4) 0.185(4) 0.220(4) -0.042(3) 0.028(3) 0.022(3) C32 0.227(6) 0.207(5) 0.280(7) -0.070(5) -0.013(4) 0.020(4) C33 0.409(12) 0.171(5) 0.358(10) 0.008(5) -0.191(9) -0.064(6) C34 0.319(8) 0.243(6) 0.164(4) -0.045(3) 0.041(4) -0.103(5) C35 0.126(4) 0.433(12) 0.467(13) -0.285(11) 0.035(5) -0.052(5) C36 0.236(9) 0.201(7) 0.77(4) 0.000(11) -0.013(12) 0.009(5) C37 0.233(6) 0.181(4) 0.277(7) 0.010(4) -0.029(4) -0.005(3) C38 1.02(5) 0.241(8) 0.258(11) 0.039(7) -0.27(2) -0.063(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C25 1.512(6) . ? C1 C2 1.529(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.365(6) . ? C2 C3 1.420(6) . ? C3 C4 1.362(5) . ? C3 H3 0.9300 . ? C4 C5 1.372(5) . ? C4 O1 1.400(5) . ? C5 C6 1.390(5) . ? C5 H5 0.9300 . ? C6 C7 1.413(5) . ? C6 C8 1.497(5) . ? C7 O2 1.387(5) . ? C8 C9 1.505(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.386(5) . ? C9 C14 1.416(6) . ? C10 C11 1.377(5) . ? C10 O3 1.404(4) . ? C11 C12 1.341(5) . ? C11 C15 1.532(5) . ? C12 C13 1.413(5) . ? C12 H12 0.9300 . ? C13 O4 1.352(5) . ? C13 C14 1.378(6) . ? C14 H14 0.9300 . ? C15 C16 1.499(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.393(5) . ? C16 C17 1.397(5) . ? C17 O5 1.384(4) . ? C17 C18 1.392(5) . ? C18 C19 1.395(5) . ? C18 C22 1.515(5) . ? C19 C20 1.412(5) . ? C19 H19 0.9300 . ? C20 C21 1.378(5) . ? C20 C29 1.513(5) . ? C21 H21 0.9300 . ? C22 C23 1.522(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.379(5) . ? C23 C24 1.394(5) . ? C24 O6 1.354(5) . ? C24 C25 1.432(6) . ? C25 C26 1.331(6) . ? C26 C27 1.405(6) . ? C26 H26 0.9300 . ? C27 C28 1.387(6) . ? C27 C30 1.551(8) . ? C28 H28 0.9300 . ? C29 C35 1.443(7) . ? C29 C34 1.465(7) . ? C29 C33 1.518(8) . ? C30 C38 1.424(13) . ? C30 C37 1.489(9) . ? C30 C36 1.498(12) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O3 H3A 0.8200 . ? O4 H4 0.8200 . ? O5 C31 1.454(5) . ? O6 C32 1.429(7) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C33 H33D 0.9600 . ? C33 H33E 0.9600 . ? C33 H33F 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C34 H34D 0.9600 . ? C34 H34E 0.9600 . ? C34 H34F 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C35 H35D 0.9600 . ? C35 H35E 0.9600 . ? C35 H35F 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C36 H36D 0.9600 . ? C36 H36E 0.9600 . ? C36 H36F 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C37 H37D 0.9600 . ? C37 H37E 0.9600 . ? C37 H37F 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C38 H38D 0.9600 . ? C38 H38E 0.9600 . ? C38 H38F 0.9600 . ? OW5 OW6 1.74(3) 36_656 ? OW5 OW9 1.84(4) 39_656 ? OW6 OW5 1.74(3) 30_656 ? OW8 OW8 1.56(6) 21_556 ? OW8 OW8 1.56(6) 23_655 ? OW9 OW5 1.84(4) 40_666 ? 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 C25 C1 C2 114.0(3) . . ? C25 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? C25 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C7 C2 C3 118.2(4) . . ? C7 C2 C1 123.1(4) . . ? C3 C2 C1 118.7(4) . . ? C4 C3 C2 119.1(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 122.5(3) . . ? C3 C4 O1 118.6(3) . . ? C5 C4 O1 118.9(4) . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 117.5(3) . . ? C5 C6 C8 121.4(4) . . ? C7 C6 C8 121.1(4) . . ? C2 C7 O2 117.3(4) . . ? C2 C7 C6 122.6(4) . . ? O2 C7 C6 120.1(4) . . ? C6 C8 C9 114.7(3) . . ? C6 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C6 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C14 116.3(3) . . ? C10 C9 C8 124.7(4) . . ? C14 C9 C8 119.0(3) . . ? C11 C10 C9 123.1(4) . . ? C11 C10 O3 121.4(3) . . ? C9 C10 O3 115.4(3) . . ? C12 C11 C10 119.4(3) . . ? C12 C11 C15 118.4(3) . . ? C10 C11 C15 122.2(4) . . ? C11 C12 C13 121.2(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? O4 C13 C14 122.8(3) . . ? O4 C13 C12 118.5(4) . . ? C14 C13 C12 118.6(4) . . ? C13 C14 C9 121.4(4) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? C16 C15 C11 112.9(3) . . ? C16 C15 H15A 109.0 . . ? C11 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C11 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 117.4(3) . . ? C21 C16 C15 121.1(3) . . ? C17 C16 C15 121.5(3) . . ? O5 C17 C18 120.2(3) . . ? O5 C17 C16 117.7(3) . . ? C18 C17 C16 122.0(3) . . ? C17 C18 C19 117.6(3) . . ? C17 C18 C22 122.9(3) . . ? C19 C18 C22 119.5(3) . . ? C18 C19 C20 122.3(3) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C21 C20 C19 116.7(3) . . ? C21 C20 C29 122.4(3) . . ? C19 C20 C29 120.7(3) . . ? C20 C21 C16 123.5(3) . . ? C20 C21 H21 118.3 . . ? C16 C21 H21 118.3 . . ? C18 C22 C23 112.8(3) . . ? C18 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C18 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C28 C23 C24 118.0(3) . . ? C28 C23 C22 120.8(4) . . ? C24 C23 C22 121.1(4) . . ? O6 C24 C23 120.0(3) . . ? O6 C24 C25 119.3(4) . . ? C23 C24 C25 120.6(4) . . ? C26 C25 C24 118.1(4) . . ? C26 C25 C1 120.5(4) . . ? C24 C25 C1 121.3(5) . . ? C25 C26 C27 123.6(4) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C28 C27 C26 116.9(4) . . ? C28 C27 C30 121.7(4) . . ? C26 C27 C30 121.2(4) . . ? C23 C28 C27 122.7(4) . . ? C23 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C35 C29 C34 112.6(5) . . ? C35 C29 C20 108.7(3) . . ? C34 C29 C20 115.0(3) . . ? C35 C29 C33 110.5(7) . . ? C34 C29 C33 99.0(6) . . ? C20 C29 C33 110.7(3) . . ? C38 C30 C37 112.3(9) . . ? C38 C30 C36 107.0(12) . . ? C37 C30 C36 105.6(8) . . ? C38 C30 C27 108.7(7) . . ? C37 C30 C27 110.8(4) . . ? C36 C30 C27 112.3(6) . . ? C4 O1 H1 109.5 . . ? C7 O2 H2 109.5 . . ? C10 O3 H3A 109.5 . . ? C13 O4 H4 109.5 . . ? C17 O5 C31 113.3(3) . . ? C24 O6 C32 115.1(4) . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 H32A 109.5 . . ? O6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C33 H33D 109.5 . . ? H33A C33 H33D 141.1 . . ? H33B C33 H33D 56.3 . . ? H33C C33 H33D 56.3 . . ? C29 C33 H33E 109.5 . . ? H33A C33 H33E 56.3 . . ? H33B C33 H33E 141.1 . . ? H33C C33 H33E 56.3 . . ? H33D C33 H33E 109.5 . . ? C29 C33 H33F 109.5 . . ? H33A C33 H33F 56.3 . . ? H33B C33 H33F 56.3 . . ? H33C C33 H33F 141.1 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C34 H34D 109.5 . . ? H34A C34 H34D 141.1 . . ? H34B C34 H34D 56.3 . . ? H34C C34 H34D 56.3 . . ? C29 C34 H34E 109.5 . . ? H34A C34 H34E 56.3 . . ? H34B C34 H34E 141.1 . . ? H34C C34 H34E 56.3 . . ? H34D C34 H34E 109.5 . . ? C29 C34 H34F 109.5 . . ? H34A C34 H34F 56.3 . . ? H34B C34 H34F 56.3 . . ? H34C C34 H34F 141.1 . . ? H34D C34 H34F 109.5 . . ? H34E C34 H34F 109.5 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C29 C35 H35D 109.5 . . ? H35A C35 H35D 141.1 . . ? H35B C35 H35D 56.3 . . ? H35C C35 H35D 56.3 . . ? C29 C35 H35E 109.5 . . ? H35A C35 H35E 56.3 . . ? H35B C35 H35E 141.1 . . ? H35C C35 H35E 56.3 . . ? H35D C35 H35E 109.5 . . ? C29 C35 H35F 109.5 . . ? H35A C35 H35F 56.3 . . ? H35B C35 H35F 56.3 . . ? H35C C35 H35F 141.1 . . ? H35D C35 H35F 109.5 . . ? H35E C35 H35F 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C36 H36D 109.5 . . ? H36A C36 H36D 141.1 . . ? H36B C36 H36D 56.3 . . ? H36C C36 H36D 56.3 . . ? C30 C36 H36E 109.5 . . ? H36A C36 H36E 56.3 . . ? H36B C36 H36E 141.1 . . ? H36C C36 H36E 56.3 . . ? H36D C36 H36E 109.5 . . ? C30 C36 H36F 109.5 . . ? H36A C36 H36F 56.3 . . ? H36B C36 H36F 56.3 . . ? H36C C36 H36F 141.1 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C37 H37D 109.5 . . ? H37A C37 H37D 141.1 . . ? H37B C37 H37D 56.3 . . ? H37C C37 H37D 56.3 . . ? C30 C37 H37E 109.5 . . ? H37A C37 H37E 56.3 . . ? H37B C37 H37E 141.1 . . ? H37C C37 H37E 56.3 . . ? H37D C37 H37E 109.5 . . ? C30 C37 H37F 109.5 . . ? H37A C37 H37F 56.3 . . ? H37B C37 H37F 56.3 . . ? H37C C37 H37F 141.1 . . ? H37D C37 H37F 109.5 . . ? H37E C37 H37F 109.5 . . ? C30 C38 H38A 109.5 . . ? C30 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C30 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C30 C38 H38D 109.5 . . ? H38A C38 H38D 141.1 . . ? H38B C38 H38D 56.3 . . ? H38C C38 H38D 56.3 . . ? C30 C38 H38E 109.5 . . ? H38A C38 H38E 56.3 . . ? H38B C38 H38E 141.1 . . ? H38C C38 H38E 56.3 . . ? H38D C38 H38E 109.5 . . ? C30 C38 H38F 109.5 . . ? H38A C38 H38F 56.3 . . ? H38B C38 H38F 56.3 . . ? H38C C38 H38F 141.1 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? OW6 OW5 OW9 147(3) 36_656 39_656 ? OW8 OW8 OW8 90.00(3) 21_556 23_655 ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.58 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.001 _refine_diff_density_min -0.001 _refine_diff_density_rms 0.000