# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1479 data_2b.8.6CH2Cl2 _publ_contact_author_name 'Maarten B. Dinger and Michael J. Scott' _publ_contact_author_address ; Department of Chemistry University of Florida P.O. Box 117200 Gainesville, FL 32611-7200 ; _publ_requested_journal 'Chemical Commnications' _publ_section_title ; Shape Selective Recognition Using Sodium Salts of Linked, C3 Symmetric Aryloxides ; _audit_creation_method SHELXL-97 _diffrn_measurement_device_type 'Siemens SMART CCD' _chemical_formula_sum 'C106.60 H163.20 Cl17.20 Na6 O6' _chemical_formula_weight 2288.45 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.4230(16) _cell_length_b 14.4230(16) _cell_length_c 50.468(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9092(2) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.254 _exptl_crystal_F_000 3628 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.626345 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16493 _diffrn_reflns_av_R_equivalents 0.1427 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3568 _reflns_number_gt 3138 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. The the central carbon of triarylmethane system lies on one of the 3-fold positions. Residual electron density associated with two disordered solvent molecules was located in difference maps. These were both modelled as dichloromethanes. The first is full occupancy, and lies near a 2-fold. The 2nd is severely disordered over the other 3-fold position, and refined with 0.3 site occupancy. One of the chlorines is disordered over two positions with a site occupancy of 0.15 for each. This molecule produced larger than usual thermal parameters, although given the complexity of the disorder these are within tolerable limits. Hydrogen atoms for these molecules are not included. ; _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^)+(0.0988P)^2^+24.2015P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3568 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1928 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.003 _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 Na1 Na 0.88297(7) 0.06984(8) 0.019878(19) 0.0246(3) Uani 1 1 d . . . O1 O 1.06751(13) 0.17583(13) 0.02452(3) 0.0215(4) Uani 1 1 d . . . C1 C 1.0000 0.0000 0.06077(8) 0.0193(8) Uani 1 3 d S . . H1A H 1.0000 0.0000 0.0414 0.029 Uiso 1 3 calc SR . . C2 C 1.02402(18) 0.11293(18) 0.06920(5) 0.0198(5) Uani 1 1 d . B . C3 C 1.06319(18) 0.19737(18) 0.05008(5) 0.0188(5) Uani 1 1 d . . . C4 C 1.09628(19) 0.30357(19) 0.05927(5) 0.0216(5) Uani 1 1 d . . . C5 C 1.1424(2) 0.40085(19) 0.04032(5) 0.0243(5) Uani 1 1 d . . . C6 C 1.1879(2) 0.5079(2) 0.05518(6) 0.0327(6) Uani 1 1 d . . . H6A H 1.2427 0.5152 0.0672 0.049 Uiso 1 1 calc R . . H6B H 1.1316 0.5096 0.0649 0.049 Uiso 1 1 calc R . . H6C H 1.2178 0.5658 0.0427 0.049 Uiso 1 1 calc R . . C7 C 1.2358(2) 0.4086(2) 0.02410(6) 0.0352(7) Uani 1 1 d . . . H7A H 1.2907 0.4142 0.0359 0.053 Uiso 1 1 calc R . . H7B H 1.2645 0.4709 0.0130 0.053 Uiso 1 1 calc R . . H7C H 1.2109 0.3458 0.0133 0.053 Uiso 1 1 calc R . . C8 C 1.0546(2) 0.3914(2) 0.02126(6) 0.0338(6) Uani 1 1 d . . . H8A H 1.0873 0.4485 0.0083 0.041 Uiso 1 1 calc R . . H8B H 1.0258 0.3240 0.0118 0.041 Uiso 1 1 calc R . . C9 C 0.9623(3) 0.3967(3) 0.03437(8) 0.0466(8) Uani 1 1 d . . . H9A H 0.9120 0.3907 0.0211 0.070 Uiso 1 1 calc R . . H9B H 0.9894 0.4638 0.0435 0.070 Uiso 1 1 calc R . . H9C H 0.9275 0.3390 0.0468 0.070 Uiso 1 1 calc R . . C10 C 1.0860(2) 0.3190(2) 0.08599(5) 0.0255(5) Uani 1 1 d . . . H10A H 1.1093 0.3884 0.0918 0.031 Uiso 1 1 calc R . . C11 C 1.0427(2) 0.2364(2) 0.10476(5) 0.0273(6) Uani 1 1 d . B . C12 C 1.0339(3) 0.2602(2) 0.13403(5) 0.0369(7) Uani 1 1 d . . . C16 C 0.8834(4) 0.3021(4) 0.12392(8) 0.0640(11) Uani 1 1 d . . . H16A H 0.8327 0.2948 0.1372 0.096 Uiso 0.60 1 calc PR A 1 H16B H 0.8589 0.2345 0.1153 0.096 Uiso 0.60 1 calc PR A 1 H16C H 0.8903 0.3544 0.1111 0.096 Uiso 0.60 1 calc PR A 1 H16D H 0.8715 0.3494 0.1350 0.096 Uiso 0.40 1 d PR A 2 H16E H 0.8177 0.2523 0.1153 0.096 Uiso 0.40 1 d PR A 2 H16F H 0.9364 0.3431 0.1108 0.096 Uiso 0.40 1 d PR A 2 C13A C 1.1465(6) 0.3186(6) 0.14476(11) 0.0553(16) Uani 0.60 1 d P B 1 H13A H 1.1835 0.3901 0.1378 0.083 Uiso 0.60 1 calc PR B 1 H13B H 1.1834 0.2815 0.1396 0.083 Uiso 0.60 1 calc PR B 1 H13C H 1.1443 0.3214 0.1637 0.083 Uiso 0.60 1 calc PR B 1 C14A C 0.9660(7) 0.1598(5) 0.14949(11) 0.0563(18) Uani 0.60 1 d P B 1 H14A H 0.8918 0.1370 0.1467 0.085 Uiso 0.60 1 calc PR B 1 H14B H 0.9826 0.1733 0.1680 0.085 Uiso 0.60 1 calc PR B 1 H14C H 0.9800 0.1046 0.1436 0.085 Uiso 0.60 1 calc PR B 1 C15A C 0.9857(5) 0.3362(5) 0.13610(10) 0.0456(13) Uani 0.60 1 d P B 1 H15A H 0.9797 0.3486 0.1548 0.055 Uiso 0.60 1 calc PR B 1 H15D H 1.0370 0.4046 0.1284 0.055 Uiso 0.60 1 calc PR B 1 C13B C 1.1197(8) 0.3721(8) 0.14404(17) 0.056(2) Uani 0.40 1 d P B 2 H13D H 1.1165 0.4264 0.1337 0.083 Uiso 0.40 1 calc PR B 2 H13E H 1.1894 0.3796 0.1423 0.083 Uiso 0.40 1 calc PR B 2 H13F H 1.1065 0.3799 0.1623 0.083 Uiso 0.40 1 calc PR B 2 C14B C 1.0511(11) 0.1798(9) 0.15369(16) 0.058(3) Uani 0.40 1 d P B 2 H14D H 1.0830 0.1457 0.1439 0.088 Uiso 0.40 1 calc PR B 2 H14E H 0.9830 0.1263 0.1606 0.088 Uiso 0.40 1 calc PR B 2 H14F H 1.0972 0.2202 0.1681 0.088 Uiso 0.40 1 calc PR B 2 C15B C 0.9235(8) 0.2424(8) 0.14076(16) 0.048(2) Uani 0.40 1 d P B 2 H15B H 0.8726 0.1664 0.1394 0.058 Uiso 0.40 1 calc PR B 2 H15C H 0.9241 0.2627 0.1591 0.058 Uiso 0.40 1 calc PR B 2 C17 C 1.01128(19) 0.1341(2) 0.09554(5) 0.0239(5) Uani 1 1 d . . . H17A H 0.9804 0.0773 0.1074 0.029 Uiso 1 1 calc R B . C101 C 0.7334(3) 0.0405(3) 0.08528(7) 0.0452(8) Uani 1 1 d . . . H10B H 0.7302 -0.0273 0.0820 0.054 Uiso 1 1 calc R . . H10C H 0.7958 0.0841 0.0961 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.74529(8) 0.10636(7) 0.054729(18) 0.0533(3) Uani 1 1 d . . . Cl2 Cl 0.61809(11) 0.01794(13) 0.10212(3) 0.0871(5) Uani 1 1 d . . . C201 C 0.6274(16) 0.296(3) 0.0619(3) 0.100(7) Uani 0.33 1 d P . . Cl3 Cl 0.7233(3) 0.3525(4) 0.08458(9) 0.0906(11) Uani 0.33 1 d P . . Cl4 Cl 0.6667 0.3333 0.02912(4) 0.0760(6) Uani 1 3 d S . . C301 C 0.350(3) -0.297(2) 0.1433(7) 0.043(9) Uiso 0.10 1 d P . . Cl5A Cl 0.3333 -0.3333 0.1230(4) 0.097(5) Uiso 0.15 3 d SP . 1 Cl5B Cl 0.370(2) -0.273(3) 0.1222(6) 0.089(7) Uiso 0.05 1 d P . 2 Cl6 Cl 0.344(8) -0.296(3) 0.1586(6) 0.19(2) Uiso 0.10 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 Na1 0.0253(5) 0.0257(5) 0.0216(5) -0.0008(4) 0.0004(4) 0.0117(4) O1 0.0255(9) 0.0204(8) 0.0177(8) -0.0010(6) 0.0000(6) 0.0109(7) C1 0.0187(12) 0.0187(12) 0.0206(19) 0.000 0.000 0.0094(6) C2 0.0171(11) 0.0194(11) 0.0229(12) -0.0021(9) 0.0010(9) 0.0091(9) C3 0.0169(11) 0.0208(11) 0.0187(11) -0.0012(9) -0.0001(8) 0.0095(9) C4 0.0201(11) 0.0209(12) 0.0234(12) -0.0012(9) 0.0006(9) 0.0099(10) C5 0.0263(12) 0.0179(12) 0.0267(13) -0.0006(10) 0.0013(10) 0.0096(10) C6 0.0375(15) 0.0202(13) 0.0366(15) -0.0024(11) 0.0007(12) 0.0115(11) C7 0.0350(15) 0.0243(13) 0.0410(16) 0.0033(11) 0.0125(12) 0.0108(11) C8 0.0436(16) 0.0274(13) 0.0332(14) -0.0008(11) -0.0054(12) 0.0197(12) C9 0.0424(17) 0.0460(18) 0.059(2) -0.0103(15) -0.0146(15) 0.0280(15) C10 0.0277(13) 0.0225(12) 0.0264(13) -0.0052(10) 0.0010(10) 0.0125(10) C11 0.0312(13) 0.0290(13) 0.0240(13) -0.0027(10) 0.0054(10) 0.0169(11) C12 0.0536(18) 0.0366(15) 0.0242(14) -0.0053(11) 0.0060(12) 0.0253(14) C16 0.076(3) 0.087(3) 0.055(2) -0.002(2) 0.016(2) 0.059(3) C13A 0.071(4) 0.078(5) 0.023(3) -0.019(3) -0.011(3) 0.042(4) C14A 0.106(6) 0.049(3) 0.022(3) 0.008(2) 0.027(3) 0.045(4) C15A 0.070(4) 0.044(3) 0.031(3) -0.004(2) 0.017(2) 0.034(3) C13B 0.061(6) 0.053(5) 0.029(4) -0.011(4) 0.007(4) 0.011(5) C14B 0.098(8) 0.086(7) 0.018(4) -0.002(4) -0.001(4) 0.066(7) C15B 0.063(5) 0.063(6) 0.029(4) -0.003(4) 0.011(4) 0.039(5) C17 0.0249(12) 0.0265(13) 0.0212(12) 0.0020(10) 0.0044(9) 0.0135(10) C101 0.0477(18) 0.0519(19) 0.0448(18) -0.0048(15) 0.0025(14) 0.0314(16) Cl1 0.0617(6) 0.0581(5) 0.0550(5) 0.0078(4) 0.0132(4) 0.0411(5) Cl2 0.0823(8) 0.1206(11) 0.0824(8) 0.0298(7) 0.0419(7) 0.0688(8) C201 0.051(11) 0.11(2) 0.077(9) 0.014(11) -0.019(7) -0.002(8) Cl3 0.077(2) 0.106(3) 0.090(3) -0.018(2) -0.0257(19) 0.047(3) Cl4 0.0730(8) 0.0730(8) 0.0821(13) 0.000 0.000 0.0365(4) _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 Na1 O1 2.2455(19) 12_545 ? Na1 O1 2.2800(19) 2_645 ? Na1 O1 2.3254(19) . ? Na1 C3 2.772(2) . ? Na1 Cl1 2.8914(13) . ? Na1 C3 2.986(2) 2_645 ? Na1 C2 3.075(3) . ? O1 C3 1.336(3) . ? O1 Na1 2.2455(19) 11_665 ? O1 Na1 2.2800(19) 3_765 ? C1 C2 1.546(2) 2_645 ? C1 C2 1.546(2) 3_765 ? C1 C2 1.546(2) . ? C2 C17 1.397(3) . ? C2 C3 1.430(3) . ? C3 C4 1.435(3) . ? C3 Na1 2.986(2) 3_765 ? C4 C10 1.387(4) . ? C4 C5 1.547(3) . ? C5 C7 1.532(4) . ? C5 C6 1.537(3) . ? C5 C8 1.541(4) . ? C8 C9 1.522(4) . ? C10 C11 1.401(4) . ? C11 C17 1.389(4) . ? C11 C12 1.536(3) . ? C12 C14A 1.499(6) . ? C12 C13A 1.507(7) . ? C12 C15B 1.520(9) . ? C12 C13B 1.548(9) . ? C12 C15A 1.568(6) . ? C12 C14B 1.636(9) . ? C16 C15A 1.440(8) . ? C16 C15B 1.516(10) . ? C101 Cl2 1.747(3) . ? C101 Cl1 1.774(3) . ? C201 Cl3 1.660(15) . ? C201 Cl4 1.744(16) . ? C301 C301 0.78(5) 2_545 ? C301 C301 0.78(5) 3_655 ? C301 Cl5B 1.47(5) 2_545 ? C301 Cl5B 1.53(4) 3_655 ? C301 Cl6 1.67(6) 15_445 ? C301 Cl6 1.83(5) 13_545 ? Cl5A C301 1.12(3) 2_545 ? Cl5A C301 1.12(3) 3_655 ? Cl5A Cl6 1.86(3) 2_545 ? Cl5A Cl6 1.86(3) 3_655 ? Cl5B Cl5B 1.31(5) 3_655 ? Cl5B Cl5B 1.31(5) 2_545 ? Cl5B C301 1.47(5) 3_655 ? Cl5B C301 1.53(4) 2_545 ? Cl5B Cl6 2.08(6) 3_655 ? Cl5B Cl6 2.18(5) 2_545 ? Cl6 Cl6 0.94(5) 15_445 ? Cl6 Cl6 1.26(7) 13_545 ? Cl6 C301 1.63(6) 15_445 ? Cl6 C301 1.83(5) 13_545 ? Cl6 Cl5B 2.08(6) 2_545 ? Cl6 Cl5B 2.18(5) 3_655 ? 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 O1 Na1 O1 94.46(7) 12_545 2_645 ? O1 Na1 O1 93.22(7) 12_545 . ? O1 Na1 O1 112.90(8) 2_645 . ? O1 Na1 C3 121.19(7) 12_545 . ? O1 Na1 C3 112.85(7) 2_645 . ? O1 Na1 C3 28.71(6) . . ? O1 Na1 Cl1 131.18(6) 12_545 . ? O1 Na1 Cl1 103.92(5) 2_645 . ? O1 Na1 Cl1 118.91(6) . . ? C3 Na1 Cl1 92.65(6) . . ? O1 Na1 C3 119.45(7) 12_545 2_645 ? O1 Na1 C3 25.10(6) 2_645 2_645 ? O1 Na1 C3 110.43(7) . 2_645 ? C3 Na1 C3 98.41(10) . 2_645 ? Cl1 Na1 C3 84.58(5) . 2_645 ? O1 Na1 C2 140.76(7) 12_545 . ? O1 Na1 C2 88.87(7) 2_645 . ? O1 Na1 C2 50.32(6) . . ? C3 Na1 C2 27.70(7) . . ? Cl1 Na1 C2 85.18(5) . . ? C3 Na1 C2 71.18(7) 2_645 . ? C3 O1 Na1 161.47(15) . 11_665 ? C3 O1 Na1 108.51(14) . 3_765 ? Na1 O1 Na1 86.36(6) 11_665 3_765 ? C3 O1 Na1 94.54(13) . . ? Na1 O1 Na1 85.28(6) 11_665 . ? Na1 O1 Na1 125.03(8) 3_765 . ? C2 C1 C2 112.74(15) 2_645 3_765 ? C2 C1 C2 112.74(15) 2_645 . ? C2 C1 C2 112.74(15) 3_765 . ? C17 C2 C3 119.7(2) . . ? C17 C2 C1 120.5(2) . . ? C3 C2 C1 119.8(2) . . ? C17 C2 Na1 131.96(16) . . ? C3 C2 Na1 64.26(12) . . ? C1 C2 Na1 77.72(15) . . ? O1 C3 C2 119.9(2) . . ? O1 C3 C4 122.1(2) . . ? C2 C3 C4 118.0(2) . . ? O1 C3 Na1 56.76(11) . . ? C2 C3 Na1 88.04(14) . . ? C4 C3 Na1 125.96(16) . . ? O1 C3 Na1 46.40(10) . 3_765 ? C2 C3 Na1 94.14(14) . 3_765 ? C4 C3 Na1 129.42(15) . 3_765 ? Na1 C3 Na1 90.33(8) . 3_765 ? C10 C4 C3 118.7(2) . . ? C10 C4 C5 119.2(2) . . ? C3 C4 C5 122.1(2) . . ? C7 C5 C6 105.6(2) . . ? C7 C5 C8 109.1(2) . . ? C6 C5 C8 108.2(2) . . ? C7 C5 C4 111.1(2) . . ? C6 C5 C4 112.5(2) . . ? C8 C5 C4 110.1(2) . . ? C9 C8 C5 115.1(2) . . ? C4 C10 C11 124.0(2) . . ? C17 C11 C10 116.5(2) . . ? C17 C11 C12 122.7(2) . . ? C10 C11 C12 120.8(2) . . ? C14A C12 C13A 110.7(5) . . ? C14A C12 C15B 66.2(5) . . ? C13A C12 C15B 139.4(4) . . ? C14A C12 C11 111.8(3) . . ? C13A C12 C11 106.5(3) . . ? C15B C12 C11 112.0(4) . . ? C14A C12 C13B 129.3(5) . . ? C13A C12 C13B 39.1(5) . . ? C15B C12 C13B 109.1(6) . . ? C11 C12 C13B 115.8(4) . . ? C14A C12 C15A 109.7(4) . . ? C13A C12 C15A 108.4(4) . . ? C15B C12 C15A 46.3(4) . . ? C11 C12 C15A 109.6(3) . . ? C13B C12 C15A 69.6(6) . . ? C14A C12 C14B 42.0(5) . . ? C13A C12 C14B 71.1(6) . . ? C15B C12 C14B 105.2(6) . . ? C11 C12 C14B 111.5(4) . . ? C13B C12 C14B 102.5(7) . . ? C15A C12 C14B 137.1(4) . . ? C15A C16 C15B 48.5(5) . . ? C16 C15A C12 118.0(4) . . ? C16 C15B C12 116.4(6) . . ? C11 C17 C2 122.8(2) . . ? Cl2 C101 Cl1 110.56(19) . . ? C101 Cl1 Na1 108.83(11) . . ? Cl3 C201 Cl4 116.2(8) . . ? C301 C301 C301 60.00(5) 2_545 3_655 ? C301 C301 Cl5B 48(2) 2_545 2_545 ? C301 C301 Cl5B 79(3) 3_655 2_545 ? C301 C301 Cl5B 71(3) 2_545 3_655 ? C301 C301 Cl5B 44.4(18) 3_655 3_655 ? Cl5B C301 Cl5B 52(2) 2_545 3_655 ? C301 C301 Cl6 73(4) 2_545 15_445 ? C301 C301 Cl6 89(3) 3_655 15_445 ? Cl5B C301 Cl6 118(4) 2_545 15_445 ? Cl5B C301 Cl6 131(4) 3_655 15_445 ? C301 C301 Cl6 66(3) 2_545 13_545 ? C301 C301 Cl6 63(2) 3_655 13_545 ? Cl5B C301 Cl6 114(3) 2_545 13_545 ? Cl5B C301 Cl6 106(2) 3_655 13_545 ? Cl6 C301 Cl6 27(2) 15_445 13_545 ? C301 Cl5A C301 41(3) 2_545 3_655 ? C301 Cl5A Cl6 10(3) 2_545 2_545 ? C301 Cl5A Cl6 32(3) 3_655 2_545 ? C301 Cl5A Cl6 35(3) 2_545 3_655 ? C301 Cl5A Cl6 10(3) 3_655 3_655 ? Cl6 Cl5A Cl6 26(2) 2_545 3_655 ? Cl5B Cl5B Cl5B 60.000(4) 3_655 2_545 ? Cl5B Cl5B C301 46.8(18) 3_655 3_655 ? Cl5B Cl5B C301 66(2) 2_545 3_655 ? Cl5B Cl5B C301 62(2) 3_655 2_545 ? Cl5B Cl5B C301 45.4(15) 2_545 2_545 ? C301 Cl5B C301 30.0(17) 3_655 2_545 ? Cl5B Cl5B Cl6 62(2) 3_655 3_655 ? Cl5B Cl5B Cl6 76(3) 2_545 3_655 ? C301 Cl5B Cl6 16(3) 3_655 3_655 ? C301 Cl5B Cl6 33(3) 2_545 3_655 ? Cl5B Cl5B Cl6 68(3) 3_655 2_545 ? Cl5B Cl5B Cl6 58.8(12) 2_545 2_545 ? C301 Cl5B Cl6 26(3) 3_655 2_545 ? C301 Cl5B Cl6 13.5(17) 2_545 2_545 ? Cl6 Cl5B Cl6 22.3(17) 3_655 2_545 ? Cl6 Cl6 Cl6 41(2) 15_445 13_545 ? Cl6 Cl6 C301 17(4) 15_445 15_445 ? Cl6 Cl6 C301 44(3) 13_545 15_445 ? Cl6 Cl6 C301 27(4) 15_445 13_545 ? Cl6 Cl6 C301 20(2) 13_545 13_545 ? C301 Cl6 C301 25.2(16) 15_445 13_545 ? Cl6 Cl6 Cl5B 122(3) 15_445 2_545 ? Cl6 Cl6 Cl5B 110(5) 13_545 2_545 ? C301 Cl6 Cl5B 139(6) 15_445 2_545 ? C301 Cl6 Cl5B 127(3) 13_545 2_545 ? Cl6 Cl6 Cl5B 135(4) 15_445 3_655 ? Cl6 Cl6 Cl5B 100(4) 13_545 3_655 ? C301 Cl6 Cl5B 144(3) 15_445 3_655 ? C301 Cl6 Cl5B 120(2) 13_545 3_655 ? Cl5B Cl6 Cl5B 35.8(15) 2_545 3_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.754 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.101 #===END data_2 _publ_requested_journal 'Chemical Commnications' _publ_section_title ; Shape Selective Recognition Using Sodium Salts of Linked, C3 Symmetric Aryloxides ; _audit_creation_method 'SHELXL-97' _diffrn_measurement_device_type 'Siemens SMART CCD' _chemical_formula_sum 'C153.6 H234 O18.4 Na6' _chemical_formula_weight 2519.13 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P(2)1/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.9111(13) _cell_length_b 15.5275(10) _cell_length_c 24.8733(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.0510(10) _cell_angle_gamma 90.00 _cell_volume 7688.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2738 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 1.000000 _exptl_absorpt_correction_T_max 0.804172 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 45869 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15676 _reflns_number_gt 9656 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The structure was solved (SHELXS) and refined (SHELXL) routinely. Residual electron density associated with a disordered solvent molecule was located in difference maps. This was successfully modelled as a diethyl ether whose oxygen lies on the inversion centre (0.4 site occupancy). The alkyl group is disordered over two positions each with a site occupancy of 0.2. Hydrogen atoms for this molecule are included in calaculated positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+4.6427P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calaculated _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 15676 _refine_ls_number_parameters 856 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2395 _refine_ls_wR_factor_gt 0.2032 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 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 Na1 Na -0.00375(6) 0.08750(7) 0.08539(4) 0.0268(3) Uani 1 1 d . . . Na2 Na 0.11508(6) -0.07822(7) 0.00218(4) 0.0291(3) Uani 1 1 d . . . Na3 Na -0.09240(6) -0.11913(7) 0.01142(4) 0.0277(3) Uani 1 1 d . . . O1 O 0.10235(10) 0.03122(12) 0.06304(7) 0.0258(4) Uani 1 1 d . . . O2 O 0.01563(10) -0.16042(11) -0.00661(7) 0.0252(4) Uani 1 1 d . . . O3 O -0.09476(9) -0.00149(12) 0.07242(7) 0.0247(4) Uani 1 1 d . . . C1 C 0.01854(14) -0.10539(17) 0.10314(10) 0.0226(6) Uani 1 1 d . . . H1A H 0.0114 -0.0711 0.0705 0.027 Uiso 1 1 calc R . . C2 C 0.07111(14) -0.05676(17) 0.13742(10) 0.0233(6) Uani 1 1 d . . . C3 C 0.11392(14) 0.00534(17) 0.11371(10) 0.0242(6) Uani 1 1 d . . . C4 C 0.16787(14) 0.03980(18) 0.14622(11) 0.0270(6) Uani 1 1 d . . . C5 C 0.21714(16) 0.1066(2) 0.12314(12) 0.0332(7) Uani 1 1 d . . . C6 C 0.24823(17) 0.0735(2) 0.07112(13) 0.0406(8) Uani 1 1 d . . . H6A H 0.2134 0.0643 0.0445 0.061 Uiso 1 1 calc R . . H6B H 0.2712 0.0202 0.0782 0.061 Uiso 1 1 calc R . . H6C H 0.2795 0.1152 0.0581 0.061 Uiso 1 1 calc R . . C7 C 0.27632(17) 0.1257(2) 0.16197(14) 0.0440(8) Uani 1 1 d . . . H7A H 0.2993 0.0731 0.1706 0.066 Uiso 1 1 calc R . . H7B H 0.2597 0.1512 0.1943 0.066 Uiso 1 1 calc R . . H7C H 0.3068 0.1649 0.1452 0.066 Uiso 1 1 calc R . . C8 C 0.18011(17) 0.1919(2) 0.11180(12) 0.0376(7) Uani 1 1 d . . . H8A H 0.2109 0.2309 0.0943 0.045 Uiso 1 1 calc R . . H8B H 0.1434 0.1805 0.0866 0.045 Uiso 1 1 calc R . . C9 C 0.15200(19) 0.2370(2) 0.16056(14) 0.0474(9) Uani 1 1 d . . . H9A H 0.1265 0.2864 0.1491 0.071 Uiso 1 1 calc R . . H9B H 0.1883 0.2551 0.1839 0.071 Uiso 1 1 calc R . . H9C H 0.1234 0.1981 0.1795 0.071 Uiso 1 1 calc R . . C10 C 0.17384(15) 0.01404(18) 0.19964(11) 0.0291(6) Uani 1 1 d . . . H10A H 0.2094 0.0361 0.2201 0.035 Uiso 1 1 calc R . . C11 C 0.13002(15) -0.04253(18) 0.22435(11) 0.0276(6) Uani 1 1 d . . . C12 C 0.13923(16) -0.0666(2) 0.28439(11) 0.0332(7) Uani 1 1 d . . . C13 C 0.1429(2) 0.0169(3) 0.31805(14) 0.0521(10) Uani 1 1 d . . . H13A H 0.1784 0.0527 0.3052 0.078 Uiso 1 1 calc R . . H13B H 0.1514 0.0026 0.3551 0.078 Uiso 1 1 calc R . . H13C H 0.1010 0.0472 0.3148 0.078 Uiso 1 1 calc R . . C14 C 0.20520(19) -0.1153(2) 0.29182(14) 0.0479(9) Uani 1 1 d . . . H14A H 0.2025 -0.1692 0.2730 0.072 Uiso 1 1 calc R . . H14B H 0.2134 -0.1258 0.3294 0.072 Uiso 1 1 calc R . . H14C H 0.2413 -0.0816 0.2777 0.072 Uiso 1 1 calc R . . C15 C 0.0808(2) -0.1232(3) 0.30294(13) 0.0524(10) Uani 1 1 d . . . H15A H 0.0807 -0.1758 0.2819 0.063 Uiso 1 1 calc R . . H15B H 0.0391 -0.0932 0.2948 0.063 Uiso 1 1 calc R . . C16 C 0.0815(3) -0.1477(4) 0.36283(15) 0.0785(15) Uani 1 1 d . . . H16A H 0.0450 -0.1864 0.3697 0.118 Uiso 1 1 calc R . . H16B H 0.0765 -0.0967 0.3842 0.118 Uiso 1 1 calc R . . H16C H 0.1233 -0.1752 0.3720 0.118 Uiso 1 1 calc R . . C17 C 0.07885(14) -0.07642(18) 0.19205(11) 0.0256(6) Uani 1 1 d . . . H17A H 0.0483 -0.1139 0.2075 0.031 Uiso 1 1 calc R . . C18 C 0.04532(14) -0.19350(17) 0.08462(11) 0.0253(6) Uani 1 1 d . A . C19 C 0.03919(14) -0.21678(17) 0.02965(11) 0.0249(6) Uani 1 1 d . . . C20 C 0.06114(15) -0.30181(18) 0.01448(11) 0.0274(6) Uani 1 1 d . . . C21 C 0.05829(16) -0.33165(18) -0.04466(11) 0.0314(7) Uani 1 1 d . . . C22 C 0.10786(17) -0.2784(2) -0.07754(12) 0.0386(7) Uani 1 1 d . . . H22A H 0.0986 -0.2182 -0.0729 0.058 Uiso 1 1 calc R . . H22B H 0.1031 -0.2932 -0.1149 0.058 Uiso 1 1 calc R . . H22C H 0.1529 -0.2904 -0.0654 0.058 Uiso 1 1 calc R . . C23 C 0.0788(2) -0.4266(2) -0.05126(13) 0.0429(8) Uani 1 1 d . . . H23A H 0.0765 -0.4419 -0.0886 0.064 Uiso 1 1 calc R . . H23B H 0.0488 -0.4625 -0.0315 0.064 Uiso 1 1 calc R . . H23C H 0.1239 -0.4345 -0.0378 0.064 Uiso 1 1 calc R . . C24 C -0.01307(16) -0.32149(18) -0.06968(11) 0.0313(7) Uani 1 1 d . . . H24A H -0.0227 -0.2605 -0.0734 0.038 Uiso 1 1 calc R . . H24B H -0.0132 -0.3462 -0.1055 0.038 Uiso 1 1 calc R . . C25 C -0.06860(18) -0.3626(2) -0.03842(14) 0.0453(8) Uani 1 1 d . . . H25A H -0.1109 -0.3523 -0.0565 0.068 Uiso 1 1 calc R . . H25B H -0.0695 -0.3383 -0.0030 0.068 Uiso 1 1 calc R . . H25C H -0.0609 -0.4235 -0.0359 0.068 Uiso 1 1 calc R . . C26 C 0.08603(16) -0.35648(18) 0.05444(12) 0.0318(7) Uani 1 1 d . . . H26A H 0.0981 -0.4121 0.0446 0.038 Uiso 1 1 calc R . . C27 C 0.09398(16) -0.33312(19) 0.10824(12) 0.0320(7) Uani 1 1 d . A . C28 C 0.11775(18) -0.3987(2) 0.15044(13) 0.0405(8) Uani 1 1 d . . . C29 C 0.1419(4) -0.3567(3) 0.20121(18) 0.099(2) Uani 1 1 d . A . H29A H 0.1791 -0.3195 0.1936 0.148 Uiso 1 1 calc R . . H29B H 0.1560 -0.4000 0.2265 0.148 Uiso 1 1 calc R . . H29C H 0.1061 -0.3234 0.2162 0.148 Uiso 1 1 calc R . . C30 C 0.1733(3) -0.4555(4) 0.12905(18) 0.0906(19) Uani 1 1 d . A . H30A H 0.2115 -0.4206 0.1206 0.136 Uiso 1 1 calc R . . H30B H 0.1576 -0.4846 0.0972 0.136 Uiso 1 1 calc R . . H30C H 0.1861 -0.4972 0.1558 0.136 Uiso 1 1 calc R . . C31A C 0.0574(7) -0.4631(6) 0.1579(3) 0.068(3) Uani 0.70 1 d P A 1 H31A H 0.0167 -0.4294 0.1614 0.082 Uiso 0.70 1 calc PR A 1 H31B H 0.0525 -0.4969 0.1253 0.082 Uiso 0.70 1 calc PR A 1 C32A C 0.0614(6) -0.5229(5) 0.2034(3) 0.102(3) Uani 0.70 1 d P A 1 H32A H 0.0653 -0.4909 0.2363 0.154 Uiso 0.70 1 calc PR A 1 H32B H 0.1000 -0.5593 0.1998 0.154 Uiso 0.70 1 calc PR A 1 H32C H 0.0216 -0.5577 0.2040 0.154 Uiso 0.70 1 calc PR A 1 C31B C 0.0603(12) -0.430(2) 0.1809(15) 0.136(14) Uani 0.30 1 d P A 2 H31C H 0.0808 -0.4748 0.2029 0.163 Uiso 0.30 1 calc PR A 2 H31D H 0.0529 -0.3827 0.2056 0.163 Uiso 0.30 1 calc PR A 2 C32B C 0.0005(7) -0.4593(8) 0.1738(5) 0.045(3) Uani 0.30 1 d P A 2 H32D H -0.0194 -0.4694 0.2081 0.068 Uiso 0.30 1 calc PR A 2 H32E H 0.0021 -0.5123 0.1540 0.068 Uiso 0.30 1 calc PR A 2 H32F H -0.0260 -0.4180 0.1540 0.068 Uiso 0.30 1 calc PR A 2 C33 C 0.07430(15) -0.25037(18) 0.12159(11) 0.0291(6) Uani 1 1 d . . . H33A H 0.0807 -0.2320 0.1569 0.035 Uiso 1 1 calc R A . C34 C -0.05036(14) -0.11142(17) 0.13036(10) 0.0243(6) Uani 1 1 d . . . C35 C -0.10286(14) -0.05336(17) 0.11465(10) 0.0243(6) Uani 1 1 d . . . C36 C -0.16369(15) -0.0551(2) 0.14482(12) 0.0314(6) Uani 1 1 d . . . C37 C -0.22295(15) 0.0049(2) 0.13091(13) 0.0376(7) Uani 1 1 d . . . C38 C -0.2802(2) -0.0034(3) 0.17205(19) 0.0688(13) Uani 1 1 d . . . H38A H -0.2625 0.0068 0.2076 0.103 Uiso 1 1 calc R . . H38B H -0.2990 -0.0602 0.1701 0.103 Uiso 1 1 calc R . . H38C H -0.3145 0.0383 0.1639 0.103 Uiso 1 1 calc R . . C39 C -0.20012(18) 0.0989(2) 0.13320(15) 0.0440(8) Uani 1 1 d . . . H39A H -0.1893 0.1142 0.1697 0.066 Uiso 1 1 calc R . . H39B H -0.2356 0.1353 0.1198 0.066 Uiso 1 1 calc R . . H39C H -0.1612 0.1061 0.1115 0.066 Uiso 1 1 calc R . . C40 C -0.25117(18) -0.0185(3) 0.07476(16) 0.0538(10) Uani 1 1 d . . . H40A H -0.2173 -0.0048 0.0486 0.065 Uiso 1 1 calc R . . H40B H -0.2581 -0.0804 0.0736 0.065 Uiso 1 1 calc R . . C41 C -0.3149(3) 0.0239(5) 0.0576(3) 0.110(2) Uani 1 1 d . . . H41A H -0.3266 0.0064 0.0216 0.166 Uiso 1 1 calc R . . H41B H -0.3092 0.0853 0.0586 0.166 Uiso 1 1 calc R . . H41C H -0.3500 0.0075 0.0814 0.166 Uiso 1 1 calc R . . C42 C -0.16898(16) -0.1132(2) 0.18679(12) 0.0363(7) Uani 1 1 d . . . H42A H -0.2081 -0.1126 0.2066 0.044 Uiso 1 1 calc R . . C43 C -0.11923(16) -0.1727(2) 0.20126(12) 0.0358(7) Uani 1 1 d . . . C44 C -0.12951(19) -0.2319(2) 0.25018(14) 0.0485(9) Uani 1 1 d . . . C45 C -0.0770(3) -0.3035(3) 0.2516(2) 0.0885(18) Uani 1 1 d . . . H45A H -0.0787 -0.3346 0.2183 0.133 Uiso 1 1 calc R . . H45B H -0.0862 -0.3421 0.2807 0.133 Uiso 1 1 calc R . . H45C H -0.0332 -0.2788 0.2568 0.133 Uiso 1 1 calc R . . C46 C -0.1986(2) -0.2742(3) 0.24756(17) 0.0650(12) Uani 1 1 d . . . H46A H -0.2045 -0.3030 0.2137 0.097 Uiso 1 1 calc R . . H46B H -0.2327 -0.2309 0.2511 0.097 Uiso 1 1 calc R . . H46C H -0.2022 -0.3152 0.2762 0.097 Uiso 1 1 calc R . . C47 C -0.1222(3) -0.1750(4) 0.30039(15) 0.0831(16) Uani 1 1 d . . . H47A H -0.1540 -0.1279 0.2968 0.100 Uiso 1 1 calc R . . H47B H -0.0776 -0.1499 0.3005 0.100 Uiso 1 1 calc R . . C48 C -0.1325(5) -0.2174(5) 0.3556(2) 0.135(3) Uani 1 1 d . . . H48A H -0.1225 -0.1765 0.3835 0.202 Uiso 1 1 calc R . . H48B H -0.1032 -0.2662 0.3593 0.202 Uiso 1 1 calc R . . H48C H -0.1783 -0.2360 0.3583 0.202 Uiso 1 1 calc R . . C49 C -0.06117(16) -0.17152(19) 0.17145(11) 0.0311(6) Uani 1 1 d . . . H49A H -0.0280 -0.2122 0.1790 0.037 Uiso 1 1 calc R . . O101 O -0.01100(13) 0.15345(17) 0.16592(9) 0.0495(6) Uani 1 1 d . . . O102 O -0.12643(18) 0.2114(2) 0.34684(14) 0.0860(11) Uani 1 1 d . . . C101 C -0.01834(16) 0.1631(2) 0.21376(13) 0.0394(8) Uani 1 1 d . . . C102 C -0.0024(2) 0.2458(3) 0.24265(15) 0.0520(9) Uani 1 1 d . . . H10B H 0.0057 0.2906 0.2164 0.062 Uiso 1 1 calc R . . H10C H 0.0384 0.2384 0.2641 0.062 Uiso 1 1 calc R . . C103 C -0.05931(19) 0.2741(2) 0.27931(14) 0.0484(9) Uani 1 1 d . . . C104 C -0.0822(2) 0.2008(3) 0.31438(15) 0.0530(10) Uani 1 1 d . . . C105 C -0.0476(2) 0.1147(3) 0.30757(16) 0.0588(11) Uani 1 1 d . . . H10D H -0.0010 0.1241 0.3196 0.071 Uiso 1 1 calc R . . C106 C -0.0436(2) 0.0912(3) 0.24850(15) 0.0553(10) Uani 1 1 d . . . H10E H -0.0141 0.0419 0.2449 0.066 Uiso 1 1 calc R . . H10F H -0.0879 0.0742 0.2356 0.066 Uiso 1 1 calc R . . C107 C -0.0374(2) 0.3490(3) 0.31415(18) 0.0694(13) Uani 1 1 d . . . H10G H -0.0014 0.3311 0.3378 0.104 Uiso 1 1 calc R . . H10H H -0.0746 0.3683 0.3350 0.104 Uiso 1 1 calc R . . H10I H -0.0223 0.3952 0.2918 0.104 Uiso 1 1 calc R . . C108 C -0.1202(2) 0.3032(3) 0.24246(19) 0.0744(14) Uani 1 1 d . . . H10J H -0.1576 0.3181 0.2645 0.112 Uiso 1 1 calc R . . H10K H -0.1329 0.2569 0.2188 0.112 Uiso 1 1 calc R . . H10L H -0.1074 0.3524 0.2216 0.112 Uiso 1 1 calc R . . C109 C -0.0736(4) 0.0454(4) 0.3429(2) 0.101(2) Uani 1 1 d . . . H10M H -0.0748 0.0657 0.3793 0.152 Uiso 1 1 calc R . . H10N H -0.0445 -0.0039 0.3411 0.152 Uiso 1 1 calc R . . H10O H -0.1180 0.0295 0.3310 0.152 Uiso 1 1 calc R . . O201 O 0.20945(14) -0.16026(19) 0.01305(12) 0.0647(8) Uani 1 1 d . . . O202 O 0.40590(18) -0.2838(2) 0.13299(14) 0.0865(11) Uani 1 1 d . . . C201 C 0.2459(2) -0.2016(3) 0.04377(18) 0.0621(11) Uani 1 1 d . . . C202 C 0.2854(3) -0.2784(4) 0.0259(2) 0.0859(16) Uani 1 1 d . . . H20A H 0.2633 -0.3302 0.0383 0.103 Uiso 1 1 calc R . . H20B H 0.2851 -0.2799 -0.0131 0.103 Uiso 1 1 calc R . . C203 C 0.3566(2) -0.2790(3) 0.04595(17) 0.0641(12) Uani 1 1 d . . . C204 C 0.36349(19) -0.2555(3) 0.10447(16) 0.0556(10) Uani 1 1 d . . . C205 C 0.3211(3) -0.1783(6) 0.1242(2) 0.129(3) Uani 1 1 d . . . H20C H 0.3416 -0.1259 0.1100 0.154 Uiso 1 1 calc R . . C206 C 0.2509(2) -0.1825(3) 0.10196(18) 0.0639(11) Uani 1 1 d . . . H20D H 0.2266 -0.2265 0.1213 0.077 Uiso 1 1 calc R . . H20E H 0.2290 -0.1278 0.1086 0.077 Uiso 1 1 calc R . . C207 C 0.3920(3) -0.3634(4) 0.0333(2) 0.0988(19) Uani 1 1 d . . . H20F H 0.3726 -0.4091 0.0539 0.148 Uiso 1 1 calc R . . H20G H 0.4389 -0.3584 0.0425 0.148 Uiso 1 1 calc R . . H20H H 0.3869 -0.3759 -0.0043 0.148 Uiso 1 1 calc R . . C208 C 0.3935(4) -0.2090(5) 0.0135(2) 0.127(3) Uani 1 1 d . . . H20I H 0.3727 -0.1541 0.0194 0.191 Uiso 1 1 calc R . . H20J H 0.3910 -0.2228 -0.0241 0.191 Uiso 1 1 calc R . . H20K H 0.4398 -0.2066 0.0251 0.191 Uiso 1 1 calc R . . C209 C 0.3229(4) -0.1709(8) 0.1849(2) 0.181(5) Uani 1 1 d . . . H20L H 0.2969 -0.1220 0.1956 0.271 Uiso 1 1 calc R . . H20M H 0.3685 -0.1640 0.1973 0.271 Uiso 1 1 calc R . . H20N H 0.3044 -0.2222 0.2004 0.271 Uiso 1 1 calc R . . O301 O -0.16339(14) -0.22577(16) 0.03694(10) 0.0535(7) Uani 1 1 d . . . O302 O -0.30025(19) -0.5095(2) 0.06613(13) 0.0841(10) Uani 1 1 d . . . C301 C -0.20173(19) -0.2797(2) 0.05389(13) 0.0451(9) Uani 1 1 d . . . C302 C -0.2745(2) -0.2813(3) 0.03929(15) 0.0524(10) Uani 1 1 d . . . H30D H -0.2826 -0.2429 0.0091 0.063 Uiso 1 1 calc R . . H30E H -0.3000 -0.2601 0.0694 0.063 Uiso 1 1 calc R . . C303 C -0.2994(2) -0.3715(3) 0.02434(14) 0.0555(10) Uani 1 1 d . . . C304 C -0.2803(2) -0.4362(3) 0.06835(15) 0.0517(9) Uani 1 1 d . . . C305 C -0.23472(19) -0.4054(2) 0.11361(14) 0.0476(9) Uani 1 1 d . . . H30F H -0.2619 -0.3676 0.1361 0.057 Uiso 1 1 calc R . . C306 C -0.1779(2) -0.3497(3) 0.09156(14) 0.0502(9) Uani 1 1 d . . . H30G H -0.1537 -0.3235 0.1215 0.060 Uiso 1 1 calc R . . H30H H -0.1468 -0.3865 0.0728 0.060 Uiso 1 1 calc R . . C307 C -0.3762(2) -0.3714(4) 0.01571(17) 0.0780(15) Uani 1 1 d . . . H30I H -0.3912 -0.4289 0.0079 0.117 Uiso 1 1 calc R . . H30J H -0.3879 -0.3342 -0.0138 0.117 Uiso 1 1 calc R . . H30K H -0.3973 -0.3512 0.0477 0.117 Uiso 1 1 calc R . . C308 C -0.2659(3) -0.4024(3) -0.02761(16) 0.0777(15) Uani 1 1 d . . . H30L H -0.2182 -0.4061 -0.0217 0.116 Uiso 1 1 calc R . . H30M H -0.2754 -0.3622 -0.0561 0.116 Uiso 1 1 calc R . . H30N H -0.2831 -0.4580 -0.0374 0.116 Uiso 1 1 calc R . . C309 C -0.2095(2) -0.4779(3) 0.14998(17) 0.0640(11) Uani 1 1 d . . . H30O H -0.2472 -0.5078 0.1647 0.096 Uiso 1 1 calc R . . H30P H -0.1824 -0.4542 0.1787 0.096 Uiso 1 1 calc R . . H30Q H -0.1831 -0.5173 0.1295 0.096 Uiso 1 1 calc R . . O401 O -0.5000 0.0000 0.0000 0.158(7) Uiso 0.40 2 d SP . . C401 C -0.509(2) 0.013(3) 0.0521(19) 0.132(14) Uiso 0.20 1 d P B 3 H40C H -0.4656 0.0091 0.0706 0.159 Uiso 0.20 1 calc PR B 3 H40D H -0.5373 -0.0322 0.0659 0.159 Uiso 0.20 1 calc PR B 3 C402 C -0.5377(19) 0.093(3) 0.0632(18) 0.114(11) Uiso 0.20 1 d P B 3 H40E H -0.5419 0.0995 0.1014 0.171 Uiso 0.20 1 calc PR B 3 H40F H -0.5813 0.0963 0.0463 0.171 Uiso 0.20 1 calc PR B 3 H40G H -0.5097 0.1381 0.0497 0.171 Uiso 0.20 1 calc PR B 3 C404 C -0.5345(18) 0.054(3) 0.0894(14) 0.105(10) Uiso 0.20 1 d P B 4 H40H H -0.5616 0.1019 0.0998 0.158 Uiso 0.20 1 calc PR B 4 H40I H -0.4900 0.0600 0.1043 0.158 Uiso 0.20 1 calc PR B 4 H40J H -0.5542 0.0014 0.1024 0.158 Uiso 0.20 1 calc PR B 4 C403 C -0.532(2) 0.051(3) 0.0352(14) 0.106(10) Uiso 0.20 1 d P B 4 H40L H -0.5783 0.0473 0.0238 0.128 Uiso 0.20 1 calc PR B 4 H40K H -0.5171 0.1083 0.0256 0.128 Uiso 0.20 1 calc PR B 4 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 Na1 0.0315(6) 0.0263(6) 0.0223(5) 0.0001(4) -0.0029(4) -0.0001(5) Na2 0.0320(6) 0.0273(6) 0.0277(6) 0.0017(4) -0.0073(5) 0.0008(5) Na3 0.0317(6) 0.0260(6) 0.0253(6) 0.0007(4) -0.0025(5) -0.0024(5) O1 0.0304(10) 0.0260(10) 0.0206(9) 0.0032(7) -0.0071(8) -0.0027(8) O2 0.0339(11) 0.0200(9) 0.0216(9) 0.0015(7) -0.0051(8) 0.0027(8) O3 0.0275(10) 0.0261(10) 0.0203(9) 0.0024(7) -0.0011(8) 0.0003(8) C1 0.0264(14) 0.0203(13) 0.0210(13) 0.0009(10) -0.0043(11) -0.0011(11) C2 0.0258(14) 0.0207(13) 0.0233(13) 0.0005(10) -0.0049(11) 0.0020(11) C3 0.0280(15) 0.0228(13) 0.0216(13) -0.0011(10) -0.0042(11) 0.0014(11) C4 0.0307(15) 0.0249(14) 0.0254(14) 0.0005(11) -0.0045(12) -0.0031(12) C5 0.0343(16) 0.0346(16) 0.0304(15) 0.0032(12) -0.0080(13) -0.0110(13) C6 0.0401(18) 0.0448(19) 0.0367(17) 0.0033(14) -0.0013(14) -0.0096(15) C7 0.0389(18) 0.051(2) 0.0414(18) 0.0070(15) -0.0132(15) -0.0197(16) C8 0.0475(19) 0.0297(16) 0.0353(17) 0.0018(13) -0.0089(14) -0.0114(14) C9 0.052(2) 0.0404(19) 0.050(2) -0.0084(16) -0.0081(17) -0.0046(16) C10 0.0312(15) 0.0308(15) 0.0249(14) -0.0024(12) -0.0098(12) -0.0028(12) C11 0.0314(15) 0.0276(15) 0.0236(14) -0.0010(11) -0.0049(12) 0.0007(12) C12 0.0378(17) 0.0392(17) 0.0224(14) 0.0013(12) -0.0068(12) -0.0022(14) C13 0.062(2) 0.061(2) 0.0329(18) -0.0113(16) -0.0075(17) 0.0052(19) C14 0.055(2) 0.053(2) 0.0344(18) 0.0049(15) -0.0096(16) 0.0057(18) C15 0.057(2) 0.072(3) 0.0274(17) 0.0079(17) -0.0061(16) -0.011(2) C16 0.082(3) 0.118(4) 0.035(2) 0.019(2) -0.004(2) -0.034(3) C17 0.0278(15) 0.0256(14) 0.0233(14) -0.0007(11) -0.0033(11) -0.0024(12) C18 0.0257(14) 0.0208(13) 0.0290(14) -0.0015(11) -0.0061(11) -0.0008(11) C19 0.0263(14) 0.0210(13) 0.0272(14) 0.0020(11) -0.0048(11) 0.0006(11) C20 0.0334(16) 0.0230(14) 0.0256(14) -0.0013(11) -0.0037(12) 0.0006(12) C21 0.0439(18) 0.0248(15) 0.0253(14) -0.0026(11) -0.0010(13) 0.0044(13) C22 0.0410(18) 0.0419(18) 0.0330(16) -0.0014(14) 0.0033(14) 0.0026(15) C23 0.062(2) 0.0304(17) 0.0361(17) -0.0055(13) -0.0061(16) 0.0151(16) C24 0.0439(18) 0.0231(14) 0.0266(14) -0.0030(11) -0.0053(13) -0.0011(13) C25 0.049(2) 0.0424(19) 0.0444(19) 0.0021(15) -0.0030(16) -0.0111(16) C26 0.0415(17) 0.0214(14) 0.0321(15) -0.0007(12) -0.0057(13) 0.0063(13) C27 0.0400(17) 0.0246(15) 0.0310(15) 0.0017(12) -0.0108(13) 0.0033(13) C28 0.057(2) 0.0279(16) 0.0360(17) 0.0060(13) -0.0151(15) 0.0059(15) C29 0.187(6) 0.044(2) 0.061(3) 0.002(2) -0.079(3) 0.015(3) C30 0.121(4) 0.093(4) 0.057(3) 0.013(2) -0.022(3) 0.067(3) C31A 0.119(8) 0.055(5) 0.029(3) 0.004(3) -0.017(4) -0.033(5) C32A 0.176(9) 0.054(4) 0.077(5) 0.020(4) -0.006(5) -0.018(5) C31B 0.071(14) 0.11(2) 0.22(3) 0.15(2) -0.01(2) 0.008(15) C32B 0.047(7) 0.038(6) 0.050(7) 0.005(5) -0.006(6) -0.013(6) C33 0.0361(16) 0.0263(15) 0.0245(14) -0.0019(11) -0.0088(12) -0.0003(12) C34 0.0285(14) 0.0243(14) 0.0198(13) -0.0018(10) -0.0027(11) -0.0058(11) C35 0.0308(15) 0.0222(13) 0.0197(13) -0.0003(10) -0.0018(11) -0.0039(11) C36 0.0283(15) 0.0331(16) 0.0327(15) 0.0005(12) 0.0010(12) -0.0028(13) C37 0.0274(16) 0.0419(18) 0.0438(18) 0.0039(14) 0.0059(14) 0.0044(14) C38 0.044(2) 0.079(3) 0.085(3) 0.030(2) 0.024(2) 0.014(2) C39 0.0430(19) 0.0394(19) 0.050(2) 0.0009(15) 0.0087(16) 0.0101(15) C40 0.0364(19) 0.062(2) 0.062(2) -0.0036(19) -0.0160(17) 0.0017(17) C41 0.090(4) 0.141(6) 0.100(4) 0.000(4) -0.006(3) 0.028(4) C42 0.0331(17) 0.0424(18) 0.0336(16) 0.0050(14) 0.0056(13) -0.0069(14) C43 0.0378(17) 0.0376(17) 0.0319(16) 0.0096(13) -0.0034(13) -0.0105(14) C44 0.051(2) 0.054(2) 0.0397(19) 0.0195(16) -0.0055(16) -0.0177(18) C45 0.077(3) 0.092(4) 0.097(4) 0.071(3) 0.012(3) 0.005(3) C46 0.067(3) 0.071(3) 0.057(2) 0.026(2) 0.000(2) -0.030(2) C47 0.121(4) 0.097(4) 0.031(2) 0.010(2) -0.007(2) -0.044(3) C48 0.215(9) 0.142(6) 0.047(3) 0.018(3) 0.003(4) -0.057(6) C49 0.0352(16) 0.0263(15) 0.0317(15) 0.0050(12) -0.0045(13) -0.0055(13) O101 0.0575(16) 0.0610(16) 0.0298(12) -0.0116(11) -0.0020(11) 0.0103(13) O102 0.091(2) 0.083(2) 0.086(2) -0.0160(18) 0.053(2) 0.0045(19) C101 0.0336(17) 0.050(2) 0.0345(17) -0.0111(15) -0.0012(13) 0.0074(15) C102 0.053(2) 0.057(2) 0.047(2) -0.0154(17) 0.0079(17) -0.0030(18) C103 0.048(2) 0.053(2) 0.045(2) -0.0170(17) 0.0059(16) 0.0061(17) C104 0.048(2) 0.066(3) 0.045(2) -0.0188(18) 0.0126(17) -0.0013(19) C105 0.069(3) 0.058(2) 0.050(2) -0.0091(19) 0.024(2) -0.002(2) C106 0.062(2) 0.054(2) 0.050(2) -0.0151(18) 0.0088(19) 0.0033(19) C107 0.069(3) 0.073(3) 0.066(3) -0.034(2) 0.005(2) -0.001(2) C108 0.058(3) 0.090(3) 0.074(3) -0.026(3) -0.006(2) 0.022(2) C109 0.156(6) 0.071(3) 0.079(3) 0.000(3) 0.060(4) 0.009(4) O201 0.0482(16) 0.0660(18) 0.0791(19) 0.0101(15) -0.0237(14) 0.0126(14) O202 0.095(2) 0.077(2) 0.085(2) -0.0089(17) -0.054(2) 0.0334(19) C201 0.048(2) 0.064(3) 0.074(3) 0.000(2) -0.022(2) 0.013(2) C202 0.086(4) 0.080(3) 0.090(4) -0.015(3) -0.038(3) 0.024(3) C203 0.062(3) 0.076(3) 0.053(2) -0.001(2) -0.011(2) 0.023(2) C204 0.041(2) 0.070(3) 0.055(2) 0.010(2) -0.0107(18) 0.0036(19) C205 0.085(4) 0.240(9) 0.059(3) -0.044(4) -0.026(3) 0.090(5) C206 0.054(2) 0.063(3) 0.074(3) 0.002(2) -0.013(2) 0.016(2) C207 0.092(4) 0.107(4) 0.097(4) -0.012(3) -0.019(3) 0.045(4) C208 0.161(7) 0.139(6) 0.083(4) 0.003(4) 0.017(4) -0.046(5) C209 0.106(5) 0.377(15) 0.059(3) -0.065(6) -0.027(3) 0.109(7) O301 0.0699(18) 0.0465(15) 0.0447(14) -0.0065(11) 0.0156(13) -0.0256(13) O302 0.112(3) 0.062(2) 0.079(2) -0.0028(16) 0.0003(19) -0.0425(19) C301 0.058(2) 0.047(2) 0.0301(16) -0.0103(14) 0.0109(16) -0.0150(18) C302 0.058(2) 0.060(2) 0.0393(19) 0.0085(17) 0.0023(17) -0.0125(19) C303 0.058(2) 0.075(3) 0.0338(18) -0.0047(18) 0.0063(17) -0.025(2) C304 0.058(2) 0.052(2) 0.045(2) -0.0082(17) 0.0138(18) -0.0175(19) C305 0.053(2) 0.048(2) 0.0419(19) 0.0003(16) 0.0107(17) -0.0040(17) C306 0.052(2) 0.057(2) 0.0426(19) 0.0014(17) 0.0064(17) -0.0115(18) C307 0.064(3) 0.124(4) 0.046(2) 0.011(3) -0.004(2) -0.029(3) C308 0.093(4) 0.104(4) 0.037(2) -0.018(2) 0.019(2) -0.047(3) C309 0.072(3) 0.059(3) 0.062(3) 0.013(2) 0.013(2) 0.003(2) _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 Na1 O101 2.257(2) . ? Na1 O2 2.272(2) 3 ? Na1 O3 2.297(2) . ? Na1 O1 2.362(2) . ? Na1 C3 2.748(3) . ? Na1 C2 2.974(3) . ? Na1 C35 3.043(3) . ? Na1 C1 3.059(3) . ? Na1 Na2 3.0826(15) 3 ? Na1 Na3 3.1423(15) 3 ? Na1 Na3 4.0837(15) . ? Na1 Na2 4.0844(16) . ? Na2 O3 2.261(2) 3 ? Na2 O201 2.282(3) . ? Na2 O1 2.293(2) . ? Na2 O2 2.363(2) . ? Na2 C19 2.723(3) . ? Na2 C3 3.063(3) . ? Na2 C18 3.073(3) . ? Na2 Na1 3.0826(15) 3 ? Na2 Na3 3.1149(15) 3 ? Na2 Na3 4.1902(16) . ? Na3 O301 2.275(3) . ? Na3 O2 2.297(2) . ? Na3 O1 2.306(2) 3 ? Na3 O3 2.376(2) . ? Na3 C35 2.775(3) . ? Na3 C19 3.054(3) . ? Na3 C34 3.062(3) . ? Na3 Na2 3.1149(15) 3 ? Na3 Na1 3.1423(15) 3 ? O1 C3 1.339(3) . ? O1 Na3 2.306(2) 3 ? O2 C19 1.336(3) . ? O2 Na1 2.272(2) 3 ? O3 C35 1.336(3) . ? O3 Na2 2.261(2) 3 ? C1 C2 1.536(4) . ? C1 C18 1.542(4) . ? C1 C34 1.544(4) . ? C2 C17 1.399(4) . ? C2 C3 1.422(4) . ? C3 C4 1.436(4) . ? C4 C10 1.391(4) . ? C4 C5 1.546(4) . ? C5 C6 1.533(5) . ? C5 C7 1.539(4) . ? C5 C8 1.539(4) . ? C8 C9 1.516(5) . ? C10 C11 1.389(4) . ? C11 C17 1.389(4) . ? C11 C12 1.547(4) . ? C12 C14 1.524(5) . ? C12 C15 1.536(5) . ? C12 C13 1.543(5) . ? C15 C16 1.537(5) . ? C18 C33 1.392(4) . ? C18 C19 1.417(4) . ? C19 C20 1.443(4) . ? C20 C26 1.392(4) . ? C20 C21 1.542(4) . ? C21 C22 1.535(4) . ? C21 C23 1.539(4) . ? C21 C24 1.549(4) . ? C24 C25 1.505(5) . ? C26 C27 1.393(4) . ? C27 C33 1.385(4) . ? C27 C28 1.531(4) . ? C28 C31B 1.47(3) . ? C28 C29 1.493(5) . ? C28 C30 1.519(6) . ? C28 C31A 1.578(12) . ? C31A C32A 1.465(11) . ? C31B C32B 1.28(3) . ? C34 C49 1.403(4) . ? C34 C35 1.429(4) . ? C35 C36 1.437(4) . ? C36 C42 1.385(4) . ? C36 C37 1.538(4) . ? C37 C39 1.529(5) . ? C37 C40 1.540(5) . ? C37 C38 1.551(5) . ? C40 C41 1.485(7) . ? C42 C43 1.396(5) . ? C43 C49 1.385(4) . ? C43 C44 1.542(4) . ? C44 C46 1.525(5) . ? C44 C45 1.526(6) . ? C44 C47 1.535(6) . ? C47 C48 1.540(6) . ? O101 C101 1.211(4) . ? O102 C104 1.217(4) . ? C101 C102 1.503(5) . ? C101 C106 1.504(5) . ? C102 C103 1.532(5) . ? C103 C107 1.510(5) . ? C103 C104 1.509(6) . ? C103 C108 1.573(6) . ? C104 C105 1.514(6) . ? C105 C109 1.488(6) . ? C105 C106 1.518(5) . ? O201 C201 1.225(4) . ? O202 C204 1.178(4) . ? C201 C206 1.479(6) . ? C201 C202 1.500(6) . ? C202 C203 1.495(6) . ? C203 C204 1.505(6) . ? C203 C207 1.524(7) . ? C203 C208 1.548(8) . ? C204 C205 1.551(7) . ? C205 C206 1.496(7) . ? C205 C209 1.514(7) . ? O301 C301 1.214(4) . ? O302 C304 1.206(5) . ? C301 C302 1.487(5) . ? C301 C306 1.506(5) . ? C302 C303 1.529(6) . ? C303 C304 1.529(6) . ? C303 C307 1.539(6) . ? C303 C308 1.542(5) . ? C304 C305 1.511(5) . ? C305 C309 1.523(5) . ? C305 C306 1.533(5) . ? O401 C401 1.33(5) . ? O401 C401 1.33(5) 3_455 ? O401 C403 1.34(4) . ? O401 C403 1.34(4) 3_455 ? C401 C402 1.40(6) . ? C404 C403 1.35(5) . ? 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 O101 Na1 O2 122.15(9) . 3 ? O101 Na1 O3 109.54(9) . . ? O2 Na1 O3 96.27(8) 3 . ? O101 Na1 O1 116.67(9) . . ? O2 Na1 O1 93.49(7) 3 . ? O3 Na1 O1 116.82(8) . . ? O101 Na1 C3 92.94(9) . . ? O2 Na1 C3 121.82(9) 3 . ? O3 Na1 C3 115.05(8) . . ? O1 Na1 C3 29.14(7) . . ? O101 Na1 C2 89.73(9) . . ? O2 Na1 C2 142.58(8) 3 . ? O3 Na1 C2 89.76(8) . . ? O1 Na1 C2 51.71(7) . . ? C3 Na1 C2 28.43(8) . . ? O101 Na1 C35 93.53(9) . . ? O2 Na1 C35 120.45(8) 3 . ? O3 Na1 C35 24.19(7) . . ? O1 Na1 C35 112.16(8) . . ? C3 Na1 C35 99.13(8) . . ? C2 Na1 C35 71.13(8) . . ? O101 Na1 C1 109.13(9) . . ? O2 Na1 C1 128.69(8) 3 . ? O3 Na1 C1 62.82(7) . . ? O1 Na1 C1 62.85(7) . . ? C3 Na1 C1 52.24(8) . . ? C2 Na1 C1 29.47(7) . . ? C35 Na1 C1 49.81(7) . . ? O101 Na1 Na2 126.27(8) . 3 ? O2 Na1 Na2 49.58(6) 3 3 ? O3 Na1 Na2 46.95(5) . 3 ? O1 Na1 Na2 116.82(6) . 3 ? C3 Na1 Na2 139.29(7) . 3 ? C2 Na1 Na2 128.35(6) . 3 ? C35 Na1 Na2 70.99(6) . 3 ? C1 Na1 Na2 99.01(6) . 3 ? O101 Na1 Na3 131.23(8) . 3 ? O2 Na1 Na3 46.87(6) 3 3 ? O3 Na1 Na3 118.46(6) . 3 ? O1 Na1 Na3 46.95(5) . 3 ? C3 Na1 Na3 74.95(7) . 3 ? C2 Na1 Na3 98.26(6) . 3 ? C35 Na1 Na3 134.63(6) . 3 ? C1 Na1 Na3 100.07(6) . 3 ? Na2 Na1 Na3 84.61(4) 3 3 ? O101 Na1 Na3 136.24(8) . . ? O2 Na1 Na3 88.03(6) 3 . ? O3 Na1 Na3 29.62(5) . . ? O1 Na1 Na3 89.11(5) . . ? C3 Na1 Na3 96.33(6) . . ? C2 Na1 Na3 79.24(6) . . ? C35 Na1 Na3 42.79(5) . . ? C1 Na1 Na3 49.91(5) . . ? Na2 Na1 Na3 49.12(3) 3 . ? Na3 Na1 Na3 92.40(3) 3 . ? O101 Na1 Na2 141.52(8) . . ? O2 Na1 Na2 85.93(6) 3 . ? O3 Na1 Na2 90.73(6) . . ? O1 Na1 Na2 28.20(5) . . ? C3 Na1 Na2 48.58(6) . . ? C2 Na1 Na2 57.02(6) . . ? C35 Na1 Na2 93.02(6) . . ? C1 Na1 Na2 51.12(6) . . ? Na2 Na1 Na2 91.62(4) 3 . ? Na3 Na1 Na2 48.96(3) 3 . ? Na3 Na1 Na2 61.73(3) . . ? O3 Na2 O201 122.51(10) 3 . ? O3 Na2 O1 96.66(8) 3 . ? O201 Na2 O1 115.86(10) . . ? O3 Na2 O2 94.75(7) 3 . ? O201 Na2 O2 113.34(10) . . ? O1 Na2 O2 111.03(8) . . ? O3 Na2 C19 123.14(8) 3 . ? O201 Na2 C19 89.35(10) . . ? O1 Na2 C19 110.56(9) . . ? O2 Na2 C19 29.37(7) . . ? O3 Na2 C3 120.48(8) 3 . ? O201 Na2 C3 98.57(10) . . ? O1 Na2 C3 23.85(7) . . ? O2 Na2 C3 107.00(8) . . ? C19 Na2 C3 95.39(8) . . ? O3 Na2 C18 142.22(8) 3 . ? O201 Na2 C18 88.68(10) . . ? O1 Na2 C18 86.23(8) . . ? O2 Na2 C18 50.11(7) . . ? C19 Na2 C18 27.47(8) . . ? C3 Na2 C18 68.37(7) . . ? O3 Na2 Na1 47.94(5) 3 3 ? O201 Na2 Na1 129.61(9) . 3 ? O1 Na2 Na1 114.49(6) . 3 ? O2 Na2 Na1 47.06(5) . 3 ? C19 Na2 Na1 75.24(6) . 3 ? C3 Na2 Na1 129.98(7) . 3 ? C18 Na2 Na1 96.68(6) . 3 ? O3 Na2 Na3 49.38(5) 3 3 ? O201 Na2 Na3 132.80(9) . 3 ? O1 Na2 Na3 47.55(5) . 3 ? O2 Na2 Na3 113.70(6) . 3 ? C19 Na2 Na3 136.42(7) . 3 ? C3 Na2 Na3 71.23(6) . 3 ? C18 Na2 Na3 125.39(7) . 3 ? Na1 Na2 Na3 82.44(4) 3 3 ? O3 Na2 Na1 88.54(6) 3 . ? O201 Na2 Na1 140.80(9) . . ? O1 Na2 Na1 29.13(5) . . ? O2 Na2 Na1 83.97(6) . . ? C19 Na2 Na1 92.37(7) . . ? C3 Na2 Na1 42.28(5) . . ? C18 Na2 Na1 75.86(6) . . ? Na1 Na2 Na1 88.38(4) 3 . ? Na3 Na2 Na1 49.54(3) 3 . ? O3 Na2 Na3 88.07(6) 3 . ? O201 Na2 Na3 136.00(9) . . ? O1 Na2 Na3 87.43(6) . . ? O2 Na2 Na3 25.54(5) . . ? C19 Na2 Na3 46.71(6) . . ? C3 Na2 Na3 89.47(6) . . ? C18 Na2 Na3 54.33(5) . . ? Na1 Na2 Na3 48.30(3) 3 . ? Na3 Na2 Na3 90.80(4) 3 . ? Na1 Na2 Na3 59.13(3) . . ? O301 Na3 O2 116.12(10) . . ? O301 Na3 O1 127.60(10) . 3 ? O2 Na3 O1 94.32(8) . 3 ? O301 Na3 O3 111.21(9) . . ? O2 Na3 O3 111.65(8) . . ? O1 Na3 O3 93.18(7) 3 . ? O301 Na3 C35 87.26(9) . . ? O2 Na3 C35 111.71(8) . . ? O1 Na3 C35 121.23(8) 3 . ? O3 Na3 C35 28.74(7) . . ? O301 Na3 C19 97.64(10) . . ? O2 Na3 C19 23.98(7) . . ? O1 Na3 C19 118.29(8) 3 . ? O3 Na3 C19 108.29(8) . . ? C35 Na3 C19 97.13(8) . . ? O301 Na3 C34 85.36(9) . . ? O2 Na3 C34 87.66(8) . . ? O1 Na3 C34 140.41(8) 3 . ? O3 Na3 C34 50.29(7) . . ? C35 Na3 C34 27.79(8) . . ? C19 Na3 C34 69.96(8) . . ? O301 Na3 Na2 131.06(9) . 3 ? O2 Na3 Na2 112.82(6) . 3 ? O1 Na3 Na2 47.19(5) 3 3 ? O3 Na3 Na2 46.25(5) . 3 ? C35 Na3 Na2 74.05(6) . 3 ? C19 Na3 Na2 128.82(7) . 3 ? C34 Na3 Na2 95.91(6) . 3 ? O301 Na3 Na1 135.88(8) . 3 ? O2 Na3 Na1 46.21(5) . 3 ? O1 Na3 Na1 48.45(6) 3 3 ? O3 Na3 Na1 112.88(6) . 3 ? C35 Na3 Na1 135.13(7) . 3 ? C19 Na3 Na1 70.02(6) . 3 ? C34 Na3 Na1 125.08(7) . 3 ? Na2 Na3 Na1 81.50(4) 3 3 ? O301 Na3 Na1 135.38(7) . . ? O2 Na3 Na1 84.76(6) . . ? O1 Na3 Na1 85.81(5) 3 . ? O3 Na3 Na1 28.55(5) . . ? C35 Na3 Na1 48.17(6) . . ? C19 Na3 Na1 87.74(6) . . ? C34 Na3 Na1 54.95(5) . . ? Na2 Na3 Na1 48.44(3) 3 . ? Na1 Na3 Na1 87.60(3) 3 . ? O301 Na3 Na2 138.06(9) . . ? O2 Na3 Na2 26.33(5) . . ? O1 Na3 Na2 86.36(6) 3 . ? O3 Na3 Na2 87.11(6) . . ? C35 Na3 Na2 94.92(6) . . ? C19 Na3 Na2 40.48(5) . . ? C34 Na3 Na2 78.16(6) . . ? Na2 Na3 Na2 89.20(4) 3 . ? Na1 Na3 Na2 47.09(3) 3 . ? Na1 Na3 Na2 59.15(3) . . ? C3 O1 Na2 112.32(16) . . ? C3 O1 Na3 160.81(17) . 3 ? Na2 O1 Na3 85.25(7) . 3 ? C3 O1 Na1 91.64(16) . . ? Na2 O1 Na1 122.66(9) . . ? Na3 O1 Na1 84.61(7) 3 . ? C19 O2 Na1 159.86(18) . 3 ? C19 O2 Na3 111.69(17) . . ? Na1 O2 Na3 86.91(7) 3 . ? C19 O2 Na2 90.47(15) . . ? Na1 O2 Na2 83.36(7) 3 . ? Na3 O2 Na2 128.13(9) . . ? C35 O3 Na2 162.40(17) . 3 ? C35 O3 Na1 111.01(15) . . ? Na2 O3 Na1 85.11(7) 3 . ? C35 O3 Na3 92.45(15) . . ? Na2 O3 Na3 84.38(7) 3 . ? Na1 O3 Na3 121.83(9) . . ? C2 C1 C18 111.5(2) . . ? C2 C1 C34 112.8(2) . . ? C18 C1 C34 113.1(2) . . ? C2 C1 Na1 72.20(13) . . ? C18 C1 Na1 151.15(18) . . ? C34 C1 Na1 89.71(15) . . ? C17 C2 C3 119.7(2) . . ? C17 C2 C1 119.6(2) . . ? C3 C2 C1 120.7(2) . . ? C17 C2 Na1 129.24(19) . . ? C3 C2 Na1 66.94(14) . . ? C1 C2 Na1 78.33(14) . . ? O1 C3 C2 120.0(2) . . ? O1 C3 C4 122.2(2) . . ? C2 C3 C4 117.8(2) . . ? O1 C3 Na1 59.22(13) . . ? C2 C3 Na1 84.63(16) . . ? C4 C3 Na1 126.64(18) . . ? O1 C3 Na2 43.83(12) . . ? C2 C3 Na2 95.91(16) . . ? C4 C3 Na2 130.53(19) . . ? Na1 C3 Na2 89.15(8) . . ? C10 C4 C3 118.7(3) . . ? C10 C4 C5 120.3(2) . . ? C3 C4 C5 120.9(2) . . ? C6 C5 C7 106.1(3) . . ? C6 C5 C8 109.5(3) . . ? C7 C5 C8 107.9(3) . . ? C6 C5 C4 110.9(2) . . ? C7 C5 C4 112.4(2) . . ? C8 C5 C4 109.9(3) . . ? C9 C8 C5 115.7(3) . . ? C11 C10 C4 124.1(3) . . ? C10 C11 C17 116.3(2) . . ? C10 C11 C12 121.0(2) . . ? C17 C11 C12 122.6(3) . . ? C14 C12 C15 109.6(3) . . ? C14 C12 C13 108.6(3) . . ? C15 C12 C13 110.2(3) . . ? C14 C12 C11 108.9(3) . . ? C15 C12 C11 110.5(2) . . ? C13 C12 C11 109.0(3) . . ? C12 C15 C16 116.1(3) . . ? C11 C17 C2 123.1(3) . . ? C33 C18 C19 120.2(3) . . ? C33 C18 C1 120.5(2) . . ? C19 C18 C1 119.4(2) . . ? C33 C18 Na2 128.5(2) . . ? C19 C18 Na2 62.41(15) . . ? C1 C18 Na2 81.11(15) . . ? O2 C19 C18 120.5(2) . . ? O2 C19 C20 121.8(2) . . ? C18 C19 C20 117.7(2) . . ? O2 C19 Na2 60.17(13) . . ? C18 C19 Na2 90.13(17) . . ? C20 C19 Na2 119.01(19) . . ? O2 C19 Na3 44.33(12) . . ? C18 C19 Na3 94.30(17) . . ? C20 C19 Na3 132.73(19) . . ? Na2 C19 Na3 92.81(8) . . ? C26 C20 C19 118.5(2) . . ? C26 C20 C21 120.3(2) . . ? C19 C20 C21 121.2(2) . . ? C22 C21 C23 106.6(3) . . ? C22 C21 C20 109.5(2) . . ? C23 C21 C20 112.6(2) . . ? C22 C21 C24 109.0(2) . . ? C23 C21 C24 107.3(2) . . ? C20 C21 C24 111.7(2) . . ? C25 C24 C21 115.2(3) . . ? C20 C26 C27 124.1(3) . . ? C33 C27 C26 116.4(3) . . ? C33 C27 C28 122.5(3) . . ? C26 C27 C28 120.9(3) . . ? C31B C28 C29 87.2(16) . . ? C31B C28 C30 124.7(13) . . ? C29 C28 C30 108.9(4) . . ? C31B C28 C27 109.9(8) . . ? C29 C28 C27 112.3(3) . . ? C30 C28 C27 111.3(3) . . ? C31B C28 C31A 29.0(17) . . ? C29 C28 C31A 114.3(4) . . ? C30 C28 C31A 103.6(5) . . ? C27 C28 C31A 106.0(4) . . ? C32A C31A C28 117.5(8) . . ? C32B C31B C28 141(3) . . ? C27 C33 C18 123.1(3) . . ? C49 C34 C35 119.8(3) . . ? C49 C34 C1 120.6(2) . . ? C35 C34 C1 119.5(2) . . ? C49 C34 Na3 129.40(18) . . ? C35 C34 Na3 64.84(14) . . ? C1 C34 Na3 78.93(14) . . ? O3 C35 C34 119.8(2) . . ? O3 C35 C36 122.5(2) . . ? C34 C35 C36 117.7(2) . . ? O3 C35 Na3 58.81(12) . . ? C34 C35 Na3 87.36(16) . . ? C36 C35 Na3 123.69(19) . . ? O3 C35 Na1 44.80(12) . . ? C34 C35 Na1 92.55(16) . . ? C36 C35 Na1 134.03(19) . . ? Na3 C35 Na1 89.04(8) . . ? C42 C36 C35 118.8(3) . . ? C42 C36 C37 119.7(3) . . ? C35 C36 C37 121.5(3) . . ? C39 C37 C36 110.1(3) . . ? C39 C37 C40 111.3(3) . . ? C36 C37 C40 109.0(3) . . ? C39 C37 C38 106.0(3) . . ? C36 C37 C38 111.8(3) . . ? C40 C37 C38 108.6(3) . . ? C41 C40 C37 116.8(4) . . ? C36 C42 C43 124.1(3) . . ? C49 C43 C42 116.7(3) . . ? C49 C43 C44 123.7(3) . . ? C42 C43 C44 119.6(3) . . ? C46 C44 C45 107.7(4) . . ? C46 C44 C47 110.8(4) . . ? C45 C44 C47 110.2(4) . . ? C46 C44 C43 110.8(3) . . ? C45 C44 C43 110.6(3) . . ? C47 C44 C43 106.7(3) . . ? C44 C47 C48 117.8(4) . . ? C43 C49 C34 122.6(3) . . ? C101 O101 Na1 159.9(3) . . ? O101 C101 C102 123.2(3) . . ? O101 C101 C106 121.4(3) . . ? C102 C101 C106 115.4(3) . . ? C101 C102 C103 112.2(3) . . ? C107 C103 C104 109.6(3) . . ? C107 C103 C102 110.7(3) . . ? C104 C103 C102 111.2(3) . . ? C107 C103 C108 109.0(3) . . ? C104 C103 C108 108.4(3) . . ? C102 C103 C108 107.9(3) . . ? O102 C104 C103 120.7(4) . . ? O102 C104 C105 122.0(4) . . ? C103 C104 C105 117.3(3) . . ? C109 C105 C104 114.2(4) . . ? C109 C105 C106 114.9(4) . . ? C104 C105 C106 110.7(4) . . ? C101 C106 C105 113.7(3) . . ? C201 O201 Na2 147.5(3) . . ? O201 C201 C206 122.3(4) . . ? O201 C201 C202 122.6(4) . . ? C206 C201 C202 115.0(4) . . ? C203 C202 C201 113.9(4) . . ? C202 C203 C204 113.0(4) . . ? C202 C203 C207 112.1(4) . . ? C204 C203 C207 112.0(4) . . ? C202 C203 C208 106.2(5) . . ? C204 C203 C208 107.3(4) . . ? C207 C203 C208 105.7(5) . . ? O202 C204 C203 122.9(4) . . ? O202 C204 C205 119.0(4) . . ? C203 C204 C205 117.0(3) . . ? C206 C205 C209 112.2(5) . . ? C206 C205 C204 111.0(5) . . ? C209 C205 C204 111.8(5) . . ? C201 C206 C205 114.7(4) . . ? C301 O301 Na3 175.5(2) . . ? O301 C301 C302 122.9(4) . . ? O301 C301 C306 121.4(4) . . ? C302 C301 C306 115.7(3) . . ? C301 C302 C303 112.7(3) . . ? C304 C303 C302 110.6(3) . . ? C304 C303 C307 109.5(3) . . ? C302 C303 C307 110.5(4) . . ? C304 C303 C308 106.8(4) . . ? C302 C303 C308 110.1(3) . . ? C307 C303 C308 109.1(3) . . ? O302 C304 C305 121.7(4) . . ? O302 C304 C303 120.6(4) . . ? C305 C304 C303 117.7(3) . . ? C304 C305 C309 113.3(3) . . ? C304 C305 C306 110.4(3) . . ? C309 C305 C306 113.1(3) . . ? C301 C306 C305 113.8(3) . . ? C401 O401 C401 180(6) . 3_455 ? C401 O401 C403 37(2) . . ? C401 O401 C403 143(2) 3_455 . ? C401 O401 C403 143(2) . 3_455 ? C401 O401 C403 37(2) 3_455 3_455 ? C403 O401 C403 180(5) . 3_455 ? O401 C401 C402 113(4) . . ? O401 C403 C404 135(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.836 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.076 #===END