Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_EtOH-Na5 _database_code_CSD 154914 _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Horiuchi, Takayuki' 'Iki, Nobuhiko' 'Koyama, Katsuyoshi' 'Miyano, Sotaro' 'Morohashi, Naoya' 'Oka, Hiromi' _publ_contact_author_name 'Dr Nobuhiko Iki' _publ_contact_author_address ; Department of Biomolecular Engineering Graduate School of Engineering Tohoku University Aramaki-Aoba 07 Aoba-ku Sendai 980 -8579 JAPAN ; _publ_contact_author_email 'IKI@ORGSYNTH.CHE.TOHOKU.AC.JP' _publ_section_title ; Energy Transfer Luminescence of Tb3+ Ion Complexed with Calix[4]arenetetrasulfonate and the Thia and Sulfonyl Analogue. The Effect of Bridging Groups ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C26 H35 Na5 O34 S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 1262.97 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.9774(9) _cell_length_b 25.096(1) _cell_length_c 14.9633(5) _cell_angle_alpha 90 _cell_angle_beta 90.4770(4) _cell_angle_gamma 90 _cell_volume 4497.5(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9448 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.4 _cell_measurement_temperature 180.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.920 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36087 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9075 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9075 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9352 _reflns_number_gt 7401 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0655 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7401 _refine_ls_number_parameters 655 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_weighting_scheme unit _refine_ls_shift/su_max 0.0068 _refine_diff_density_max 0.45 _refine_diff_density_min -0.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Na' 'Na' 0.036 0.025 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S 0.92620(9) 0.22538(5) -0.03268(7) 0.0107(3) Uani 1.00 d . . . S(2) S 1.16448(9) 0.23604(5) 0.29002(8) 0.0120(3) Uani 1.00 d . . . S(3) S 0.76288(9) 0.21744(5) 0.46621(8) 0.0127(3) Uani 1.00 d . . . S(4) S 0.52345(9) 0.23062(5) 0.15182(8) 0.0117(3) Uani 1.00 d . . . S(5) S 1.2076(1) 0.06771(5) 0.07152(9) 0.0226(3) Uani 1.00 d . . . S(6) S 1.11151(10) 0.09181(5) 0.55925(8) 0.0132(3) Uani 1.00 d . . . S(7) S 0.4355(1) 0.07465(5) 0.38908(8) 0.0136(3) Uani 1.00 d . . . S(8) S 0.6023(1) 0.08015(5) -0.10024(8) 0.0150(3) Uani 1.00 d . . . Na(1) Na 1.2694(2) 0.00186(9) 0.2668(1) 0.0263(6) Uani 1.00 d . . . Na(2) Na 0.8839(2) 0.34444(8) 0.0756(1) 0.0184(5) Uani 1.00 d . . . Na(3) Na 0.3754(2) 0.01906(9) -0.0865(1) 0.0230(6) Uani 1.00 d . . . Na(4) Na 1.0112(2) 0.13817(9) 0.7675(1) 0.0210(5) Uani 1.00 d . . . Na(5) Na 0.6291(2) -0.03215(8) 0.3840(1) 0.0221(5) Uani 1.00 d . . . O(1) O 0.9245(3) 0.2824(1) -0.0307(2) 0.0130(8) Uani 1.00 d . . . O(2) O 0.9583(3) 0.1993(1) -0.1138(2) 0.0145(8) Uani 1.00 d . . . O(3) O 1.1389(3) 0.2922(1) 0.2831(2) 0.0160(9) Uani 1.00 d . . . O(4) O 1.2762(3) 0.2206(1) 0.3102(2) 0.0169(9) Uani 1.00 d . . . O(5) O 0.7606(3) 0.2744(1) 0.4573(2) 0.0194(9) Uani 1.00 d . . . O(6) O 0.7350(3) 0.1935(2) 0.5507(2) 0.0193(9) Uani 1.00 d . . . O(7) O 0.5431(3) 0.2868(1) 0.1620(2) 0.0164(9) Uani 1.00 d . . . O(8) O 0.4138(3) 0.2133(1) 0.1260(2) 0.0169(9) Uani 1.00 d . . . O(9) O 0.4888(3) 0.0275(1) 0.3520(3) 0.0245(10) Uani 1.00 d . . . O(10) O 0.6013(3) 0.0372(1) -0.0362(3) 0.026(1) Uani 1.00 d . . . O(11) O 0.4372(3) 0.0756(2) 0.4861(2) 0.024(1) Uani 1.00 d . . . O(12) O 1.0385(3) 0.0892(1) 0.6361(2) 0.0195(9) Uani 1.00 d . . . O(13) O 1.2252(3) 0.1054(2) 0.5827(3) 0.0227(10) Uani 1.00 d . . . O(14) O 1.1046(3) 0.0436(1) 0.5061(2) 0.024(1) Uani 1.00 d . . . O(15) O 0.4904(3) 0.0928(2) -0.1330(2) 0.0231(10) Uani 1.00 d . . . O(16) O 0.3266(3) 0.0824(2) 0.3493(3) 0.025(1) Uani 1.00 d . . . O(17) O 0.6821(3) 0.0728(1) -0.1723(2) 0.0217(10) Uani 1.00 d . . . O(18) O 1.0083(3) 0.2797(1) 0.1396(2) 0.0153(8) Uani 1.00 d . . . O(19) O 0.7690(3) 0.2648(1) 0.1074(2) 0.0191(9) Uani 1.00 d . . . O(20) O 0.7216(3) 0.2531(1) 0.2737(2) 0.0156(8) Uani 1.00 d . . . O(21) O 0.9249(3) 0.2527(2) 0.3123(2) 0.0207(9) Uani 1.00 d . . . O(22) O 1.3325(9) 0.0797(4) 0.0956(7) 0.047(2) Uiso 0.50 d P . . O(22') O 1.2795(7) 0.0573(4) 0.1414(6) 0.035(2) Uiso 0.50 d P . . O(23) O 1.1635(7) 0.0303(3) 0.1291(6) 0.030(2) Uiso 0.50 d P . . O(23') O 1.108(1) 0.0292(5) 0.0674(8) 0.064(3) Uiso 0.50 d P . . O(24) O 1.1999(7) 0.0587(3) -0.0229(5) 0.022(2) Uiso 0.50 d P . . O(24') O 1.2507(8) 0.0723(4) -0.0147(6) 0.037(2) Uiso 0.50 d P . . O(100) O 0.8807(4) 0.0465(2) 0.2836(3) 0.046(1) Uani 1.00 d . . . O(101) O 0.9801(3) 0.3961(2) 0.1786(2) 0.0233(10) Uani 1.00 d . . . O(102) O 0.9884(5) 0.0633(2) 0.8659(3) 0.050(2) Uani 1.00 d . . . O(103) O 1.3082(3) -0.0661(2) 0.3792(3) 0.028(1) Uani 1.00 d . . . O(104) O 1.0860(3) 0.0045(2) 0.3318(3) 0.030(1) Uani 1.00 d . . . O(105) O 0.7534(4) 0.0357(2) 0.4439(3) 0.030(1) Uani 1.00 d . . . O(106) O 1.1969(3) 0.1357(2) 0.8265(3) 0.027(1) Uani 1.00 d . . . O(107) O 0.4684(4) -0.0461(2) -0.1633(3) 0.038(1) Uani 1.00 d . . . O(108) O 0.2778(3) 0.0328(2) -0.2367(3) 0.025(1) Uani 1.00 d . . . O(109) O 0.8237(3) 0.1413(2) 0.7147(3) 0.030(1) Uani 1.00 d . . . C(1) C 1.0179(4) 0.2012(2) 0.0517(3) 0.012(1) Uani 1.00 d . . . C(2) C 1.0479(4) 0.2307(2) 0.1280(3) 0.012(1) Uani 1.00 d . . . C(3) C 1.1230(4) 0.2061(2) 0.1879(3) 0.012(1) Uani 1.00 d . . . C(4) C 1.1707(4) 0.1565(2) 0.1706(3) 0.015(1) Uani 1.00 d . . . C(5) C 1.1421(4) 0.1298(2) 0.0936(3) 0.017(1) Uani 1.00 d . . . C(6) C 1.0642(4) 0.1516(2) 0.0356(3) 0.015(1) Uani 1.00 d . . . C(7) C 1.0784(4) 0.2062(2) 0.3706(3) 0.013(1) Uani 1.00 d . . . C(8) C 0.9638(4) 0.2197(2) 0.3742(3) 0.014(1) Uani 1.00 d . . . C(9) C 0.8995(4) 0.1957(2) 0.4420(3) 0.013(1) Uani 1.00 d . . . C(10) C 0.9464(4) 0.1575(2) 0.4979(3) 0.015(1) Uani 1.00 d . . . C(11) C 1.0578(4) 0.1430(2) 0.4890(3) 0.014(1) Uani 1.00 d . . . C(12) C 1.1250(4) 0.1674(2) 0.4273(3) 0.012(1) Uani 1.00 d . . . C(13) C 0.6705(4) 0.1901(2) 0.3862(3) 0.013(1) Uani 1.00 d . . . C(14) C 0.6553(4) 0.2159(2) 0.3020(3) 0.012(1) Uani 1.00 d . . . C(15) C 0.5613(4) 0.1979(2) 0.2514(3) 0.012(1) Uani 1.00 d . . . C(16) C 0.4952(4) 0.1554(2) 0.2772(3) 0.013(1) Uani 1.00 d . . . C(17) C 0.5191(4) 0.1295(2) 0.3564(3) 0.013(1) Uani 1.00 d . . . C(18) C 0.6048(4) 0.1471(2) 0.4113(3) 0.012(1) Uani 1.00 d . . . C(19) C 0.6174(4) 0.2045(2) 0.0711(3) 0.012(1) Uani 1.00 d . . . C(20) C 0.7258(4) 0.2247(2) 0.0594(3) 0.011(1) Uani 1.00 d . . . C(21) C 0.7918(4) 0.2009(2) -0.0062(3) 0.012(1) Uani 1.00 d . . . C(22) C 0.7548(4) 0.1569(2) -0.0545(3) 0.013(1) Uani 1.00 d . . . C(23) C 0.6483(4) 0.1370(2) -0.0404(3) 0.012(1) Uani 1.00 d . . . C(24) C 0.5796(4) 0.1612(2) 0.0215(3) 0.014(1) Uani 1.00 d . . . C(25) C 0.8950(9) 0.0909(5) 0.2264(8) 0.091(4) Uani 1.00 d . . . C(26) C 0.809(1) 0.1036(7) 0.180(1) 0.182(8) Uani 1.00 d . . . H(1) H 0.8966 0.1411 0.5448 0.0234 Uiso 1.00 calc . . . H(2) H 1.1946 0.1579 0.4171 0.0074 Uiso 1.00 calc . . . H(3) H 0.4331 0.1439 0.2381 0.0130 Uiso 1.00 calc . . . H(4) H 0.6237 0.1301 0.4680 0.0139 Uiso 1.00 calc . . . H(5) H 1.2169 0.1443 0.2110 0.0139 Uiso 1.00 calc . . . H(6) H 1.0436 0.1343 -0.0124 0.0136 Uiso 1.00 calc . . . H(7) H 0.8029 0.1407 -0.0962 0.0152 Uiso 1.00 calc . . . H(8) H 0.5184 0.1511 0.0292 0.0119 Uiso 1.00 calc . . . H(9) H 1.0370 0.4063 0.1664 0.0332 Uiso 1.00 calc . . . H(10) H 0.9717 0.3974 0.2378 0.0369 Uiso 1.00 calc . . . H(11) H 1.2207 0.1682 0.8185 0.0372 Uiso 1.00 calc . . . H(12) H 0.5333 -0.0508 -0.1416 0.0314 Uiso 1.00 calc . . . H(13) H 0.4826 -0.0375 -0.2097 0.0223 Uiso 1.00 calc . . . H(14) H 0.9389 0.0420 0.8754 0.0369 Uiso 1.00 calc . . . H(15) H 0.8005 0.0126 0.4570 0.0193 Uiso 1.00 calc . . . H(16) H 0.7835 0.0475 0.4023 0.0371 Uiso 1.00 calc . . . H(17) H 0.9082 0.1232 0.2566 0.2669 Uiso 1.00 calc . . . H(18) H 0.9624 0.0773 0.1763 0.1781 Uiso 1.00 calc . . . H(19) H 0.7505 0.1144 0.2215 0.2262 Uiso 1.00 calc . . . H(20) H 0.8257 0.1335 0.1438 0.2262 Uiso 1.00 calc . . . H(21) H 0.7841 0.0749 0.1467 0.2262 Uiso 1.00 calc . . . H(22) H 1.3020 -0.0562 0.4293 0.0463 Uiso 1.00 calc . . . H(23) H 1.2689 -0.0923 0.3653 0.0425 Uiso 1.00 calc . . . H(24) H 1.2181 0.1268 0.8759 0.0571 Uiso 1.00 calc . . . H(25) H 0.8060 0.1722 0.6919 0.0548 Uiso 1.00 calc . . . H(26) H 0.7771 0.1407 0.7523 0.0298 Uiso 1.00 calc . . . H(27) H 0.2178 0.0112 -0.2461 0.0662 Uiso 1.00 calc . . . H(28) H 0.2539 0.0647 -0.2323 0.0662 Uiso 1.00 calc . . . H(29) H 1.0558 0.0544 0.8936 0.0810 Uiso 1.00 calc . . . H(30) H 0.8498 0.2553 0.3119 0.0372 Uiso 1.00 calc . . . H(31) H 1.0280 0.2905 0.1801 0.0185 Uiso 0.50 calc P . . H(32) H 0.7515 0.2690 0.1447 0.0195 Uiso 0.50 calc P . . H(33) H 0.7246 0.2609 0.2303 0.1071 Uiso 1.00 calc . . . H(34) H 0.9564 0.0281 0.2964 0.0180 Uiso 1.00 calc . . . H(35) H 1.0568 -0.0324 0.3388 0.0180 Uiso 1.00 calc . . . H(36) H 1.0884 0.0200 0.3799 0.0180 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0105(5) 0.0131(5) 0.0084(5) -0.0002(4) -0.0007(4) 0.0010(4) S(2) 0.0100(5) 0.0164(6) 0.0095(5) -0.0016(4) -0.0007(4) -0.0014(4) S(3) 0.0099(5) 0.0180(6) 0.0101(5) 0.0020(4) -0.0006(4) 0.0005(4) S(4) 0.0104(5) 0.0145(5) 0.0102(5) 0.0012(4) 0.0006(4) 0.0005(4) S(5) 0.0348(8) 0.0160(6) 0.0170(6) 0.0114(5) 0.0019(5) -0.0009(5) S(6) 0.0131(6) 0.0134(5) 0.0129(6) 0.0013(4) 0.0004(4) 0.0018(4) S(7) 0.0165(6) 0.0122(5) 0.0120(6) -0.0010(4) 0.0017(4) 0.0007(4) S(8) 0.0181(6) 0.0135(6) 0.0134(6) -0.0041(4) 0.0005(5) -0.0022(4) Na(1) 0.030(1) 0.023(1) 0.026(1) 0.0003(9) 0.0021(9) 0.0014(9) Na(2) 0.018(1) 0.0161(10) 0.021(1) 0.0033(8) -0.0015(8) -0.0013(8) Na(3) 0.024(1) 0.021(1) 0.023(1) 0.0005(9) 0.0050(9) 0.0013(9) Na(4) 0.022(1) 0.024(1) 0.017(1) -0.0007(9) 0.0017(8) -0.0032(8) Na(5) 0.028(1) 0.017(1) 0.022(1) -0.0004(9) 0.0030(9) 0.0013(8) O(1) 0.014(2) 0.014(2) 0.011(2) -0.001(1) 0.000(1) 0.002(1) O(2) 0.014(2) 0.019(2) 0.011(2) 0.002(1) 0.002(1) -0.001(1) O(3) 0.018(2) 0.015(2) 0.015(2) -0.004(1) -0.002(1) -0.001(1) O(4) 0.010(2) 0.024(2) 0.016(2) -0.001(1) -0.006(1) -0.001(1) O(5) 0.018(2) 0.020(2) 0.020(2) 0.002(1) -0.002(1) -0.005(1) O(6) 0.016(2) 0.030(2) 0.011(2) 0.001(2) 0.000(1) 0.003(1) O(7) 0.020(2) 0.012(2) 0.017(2) 0.005(1) -0.002(1) 0.000(1) O(8) 0.008(2) 0.026(2) 0.017(2) 0.001(1) 0.000(1) 0.002(1) O(9) 0.033(2) 0.013(2) 0.028(2) 0.001(2) 0.009(2) 0.001(2) O(10) 0.042(2) 0.014(2) 0.022(2) -0.006(2) -0.001(2) 0.001(1) O(11) 0.035(2) 0.022(2) 0.016(2) -0.009(2) 0.006(2) 0.002(1) O(12) 0.023(2) 0.020(2) 0.015(2) 0.001(1) 0.004(1) 0.003(1) O(13) 0.019(2) 0.023(2) 0.026(2) -0.002(2) -0.004(2) 0.010(2) O(14) 0.033(2) 0.017(2) 0.022(2) 0.005(2) 0.002(2) 0.000(2) O(15) 0.023(2) 0.026(2) 0.020(2) -0.005(2) -0.006(2) -0.004(2) O(16) 0.018(2) 0.021(2) 0.036(2) -0.002(2) -0.004(2) 0.008(2) O(17) 0.025(2) 0.020(2) 0.021(2) -0.006(2) 0.005(2) -0.007(1) O(18) 0.020(2) 0.014(2) 0.013(2) 0.003(1) 0.000(1) -0.002(1) O(19) 0.023(2) 0.021(2) 0.013(2) -0.006(1) 0.004(1) -0.010(1) O(20) 0.010(2) 0.021(2) 0.016(2) -0.004(1) 0.001(1) 0.004(1) O(21) 0.011(2) 0.032(2) 0.019(2) 0.006(1) 0.001(1) 0.013(2) O(100) 0.032(2) 0.057(3) 0.049(3) -0.010(2) -0.008(2) 0.028(3) O(101) 0.023(2) 0.026(2) 0.021(2) -0.002(2) -0.002(2) -0.003(2) O(102) 0.070(4) 0.037(3) 0.042(3) -0.021(3) -0.015(3) 0.003(2) O(103) 0.032(2) 0.026(2) 0.025(2) -0.002(2) 0.002(2) -0.004(2) O(104) 0.032(2) 0.031(2) 0.026(2) -0.009(2) -0.001(2) -0.006(2) O(105) 0.035(2) 0.028(2) 0.029(2) 0.008(2) -0.001(2) 0.000(2) O(106) 0.030(2) 0.021(2) 0.029(2) -0.003(2) -0.003(2) 0.000(2) O(107) 0.049(3) 0.044(3) 0.020(2) 0.011(2) 0.002(2) -0.004(2) O(108) 0.028(2) 0.026(2) 0.021(2) 0.000(2) 0.001(2) 0.004(2) O(109) 0.019(2) 0.049(3) 0.022(2) 0.003(2) 0.003(2) -0.011(2) C(1) 0.009(2) 0.013(2) 0.014(2) 0.000(2) -0.001(2) 0.006(2) C(2) 0.011(2) 0.014(2) 0.012(2) -0.003(2) 0.002(2) 0.002(2) C(3) 0.012(2) 0.016(2) 0.009(2) 0.000(2) 0.001(2) -0.001(2) C(4) 0.011(2) 0.022(3) 0.011(2) 0.004(2) -0.002(2) 0.002(2) C(5) 0.021(3) 0.013(2) 0.018(2) 0.003(2) 0.004(2) 0.000(2) C(6) 0.018(2) 0.014(2) 0.013(2) -0.001(2) -0.001(2) 0.000(2) C(7) 0.016(2) 0.016(2) 0.008(2) 0.000(2) 0.001(2) -0.002(2) C(8) 0.014(2) 0.014(2) 0.014(2) 0.002(2) 0.003(2) -0.001(2) C(9) 0.009(2) 0.015(2) 0.014(2) 0.003(2) 0.000(2) -0.003(2) C(10) 0.018(2) 0.013(2) 0.015(2) -0.001(2) 0.001(2) -0.002(2) C(11) 0.013(2) 0.014(2) 0.014(2) 0.003(2) -0.003(2) -0.002(2) C(12) 0.011(2) 0.017(2) 0.007(2) 0.001(2) -0.001(2) -0.001(2) C(13) 0.007(2) 0.013(2) 0.020(2) 0.001(2) -0.003(2) 0.000(2) C(14) 0.012(2) 0.012(2) 0.011(2) 0.004(2) 0.002(2) 0.001(2) C(15) 0.010(2) 0.013(2) 0.014(2) 0.005(2) 0.000(2) 0.003(2) C(16) 0.012(2) 0.014(2) 0.014(2) 0.004(2) 0.003(2) -0.002(2) C(17) 0.017(2) 0.010(2) 0.012(2) 0.002(2) 0.004(2) -0.001(2) C(18) 0.013(2) 0.015(2) 0.009(2) 0.002(2) 0.001(2) 0.002(2) C(19) 0.013(2) 0.015(2) 0.007(2) -0.001(2) 0.001(2) -0.001(2) C(20) 0.013(2) 0.013(2) 0.008(2) 0.001(2) -0.003(2) -0.001(2) C(21) 0.011(2) 0.013(2) 0.013(2) 0.000(2) -0.001(2) 0.003(2) C(22) 0.016(2) 0.013(2) 0.010(2) 0.004(2) -0.001(2) -0.001(2) C(23) 0.020(2) 0.011(2) 0.006(2) -0.003(2) -0.003(2) -0.001(2) C(24) 0.010(2) 0.017(2) 0.017(2) -0.005(2) 0.000(2) 0.004(2) C(25) 0.086(7) 0.084(8) 0.103(8) -0.029(6) -0.006(6) 0.064(7) C(26) 0.12(1) 0.20(2) 0.23(2) -0.05(1) -0.06(1) 0.19(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(1) O(1) 1.432(4) . . yes S(1) O(2) 1.435(3) . . yes S(1) C(1) 1.774(5) . . yes S(1) C(21) 1.771(5) . . yes S(2) O(3) 1.446(4) . . yes S(2) O(4) 1.423(4) . . yes S(2) C(3) 1.770(5) . . yes S(2) C(7) 1.761(5) . . yes S(3) O(5) 1.436(4) . . yes S(3) O(6) 1.441(4) . . yes S(3) C(9) 1.765(5) . . yes S(3) C(13) 1.762(5) . . yes S(4) O(7) 1.437(4) . . yes S(4) O(8) 1.433(3) . . yes S(4) C(15) 1.758(5) . . yes S(4) C(19) 1.783(5) . . yes S(5) O(22) 1.57(1) . . yes S(5) O(23) 1.382(9) . . yes S(5) O(24) 1.433(8) . . yes S(5) O(22') 1.374(9) . . yes S(5) O(23') 1.54(1) . . yes S(5) O(24') 1.399(10) . . yes S(5) C(5) 1.777(5) . . yes S(6) O(12) 1.451(4) . . yes S(6) O(13) 1.445(4) . . yes S(6) O(14) 1.450(4) . . yes S(6) C(11) 1.778(5) . . yes S(7) O(9) 1.456(4) . . yes S(7) O(11) 1.452(4) . . yes S(7) O(16) 1.442(4) . . yes S(7) C(17) 1.774(5) . . yes S(8) O(10) 1.441(4) . . yes S(8) O(15) 1.458(4) . . yes S(8) O(17) 1.458(4) . . yes S(8) C(23) 1.769(5) . . yes Na(1) O(16) 2.462(4) . 1_655 yes Na(1) O(17) 2.421(4) . 3_755 yes Na(1) O(23) 2.514(9) . . yes Na(1) O(103) 2.438(4) . . yes Na(1) O(104) 2.410(5) . . yes Na(1) O(22') 2.341(9) . . yes Na(2) Na(5) 3.159(3) . 2_655 yes Na(2) O(1) 2.281(4) . . yes Na(2) O(11) 2.499(4) . 4_554 yes Na(2) O(13) 2.282(4) . 4_454 yes Na(2) O(18) 2.399(4) . . yes Na(2) O(19) 2.475(4) . . yes Na(2) O(101) 2.313(4) . . yes Na(3) O(10) 2.332(4) . 3_655 yes Na(3) O(15) 2.413(4) . . yes Na(3) O(24) 2.519(8) . 1_455 yes Na(3) O(107) 2.292(5) . . yes Na(3) O(108) 2.547(4) . . yes Na(3) O(24') 2.28(1) . 1_455 yes Na(4) O(2) 2.434(4) . 1_556 yes Na(4) O(7) 2.489(4) . 4_555 yes Na(4) O(12) 2.344(4) . . yes Na(4) O(102) 2.404(5) . . yes Na(4) O(106) 2.386(4) . . yes Na(4) O(109) 2.376(4) . . yes Na(5) O(9) 2.298(4) . . yes Na(5) O(11) 2.371(4) . 3_656 yes Na(5) O(13) 2.581(4) . 3_756 yes Na(5) O(101) 2.411(4) . 2_645 yes Na(5) O(105) 2.427(5) . . yes Na(5) O(108) 2.479(4) . 3_655 yes O(18) C(2) 1.329(6) . . yes O(19) C(20) 1.337(6) . . yes O(20) C(14) 1.299(6) . . yes O(21) C(8) 1.324(6) . . yes O(100) C(25) 1.42(1) . . yes C(1) C(2) 1.406(7) . . yes C(1) C(6) 1.383(7) . . yes C(2) C(3) 1.407(7) . . yes C(3) C(4) 1.394(7) . . yes C(4) C(5) 1.374(7) . . yes C(5) C(6) 1.381(7) . . yes C(7) C(8) 1.415(7) . . yes C(7) C(12) 1.403(7) . . yes C(8) C(9) 1.414(7) . . yes C(9) C(10) 1.387(7) . . yes C(10) C(11) 1.390(7) . . yes C(11) C(12) 1.374(7) . . yes C(13) C(14) 1.428(7) . . yes C(13) C(18) 1.389(7) . . yes C(14) C(15) 1.425(6) . . yes C(15) C(16) 1.383(7) . . yes C(16) C(17) 1.380(7) . . yes C(17) C(18) 1.381(7) . . yes C(19) C(20) 1.406(7) . . yes C(19) C(24) 1.389(7) . . yes C(20) C(21) 1.401(7) . . yes C(21) C(22) 1.390(7) . . yes C(22) C(23) 1.388(7) . . yes C(23) C(24) 1.385(7) . . yes C(25) C(26) 1.27(2) . . yes O(18) H(31) 0.704 . . no O(19) H(32) 0.607 . . no O(20) H(33) 0.679 . . no O(21) H(30) 0.902 . . no O(100) H(34) 1.035 . . no O(101) H(9) 0.751 . . no O(101) H(10) 0.893 . . no O(102) H(14) 0.811 . . no O(102) H(29) 0.931 . . no O(103) H(22) 0.794 . . no O(103) H(23) 0.833 . . no O(104) H(35) 0.996 . . no O(104) H(36) 0.819 . . no O(105) H(15) 0.831 . . no O(105) H(16) 0.779 . . no O(106) H(11) 0.872 . . no O(106) H(24) 0.811 . . no O(107) H(12) 0.849 . . no O(107) H(13) 0.748 . . no O(108) H(27) 0.911 . . no O(108) H(28) 0.853 . . no O(109) H(25) 0.872 . . no O(109) H(26) 0.796 . . no C(4) H(5) 0.872 . . no C(6) H(6) 0.874 . . no C(10) H(1) 1.012 . . no C(12) H(2) 0.881 . . no C(16) H(3) 0.986 . . no C(18) H(4) 0.975 . . no C(22) H(7) 0.944 . . no C(24) H(8) 0.785 . . no C(25) H(17) 0.939 . . no C(25) H(18) 1.157 . . no C(26) H(19) 0.981 . . no C(26) H(20) 0.947 . . no C(26) H(21) 0.927 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) S(1) O(2) 118.5(2) . . . yes O(1) S(1) C(1) 109.7(2) . . . yes O(1) S(1) C(21) 109.2(2) . . . yes O(2) S(1) C(1) 106.1(2) . . . yes O(2) S(1) C(21) 106.3(2) . . . yes C(1) S(1) C(21) 106.3(2) . . . yes O(3) S(2) O(4) 118.6(2) . . . yes O(3) S(2) C(3) 107.1(2) . . . yes O(3) S(2) C(7) 109.8(2) . . . yes O(4) S(2) C(3) 108.9(2) . . . yes O(4) S(2) C(7) 107.1(2) . . . yes C(3) S(2) C(7) 104.4(2) . . . yes O(5) S(3) O(6) 119.4(2) . . . yes O(5) S(3) C(9) 107.8(2) . . . yes O(5) S(3) C(13) 108.3(2) . . . yes O(6) S(3) C(9) 105.9(2) . . . yes O(6) S(3) C(13) 106.6(2) . . . yes C(9) S(3) C(13) 108.5(2) . . . yes O(7) S(4) O(8) 118.3(2) . . . yes O(7) S(4) C(15) 109.1(2) . . . yes O(7) S(4) C(19) 109.2(2) . . . yes O(8) S(4) C(15) 108.4(2) . . . yes O(8) S(4) C(19) 106.8(2) . . . yes C(15) S(4) C(19) 104.0(2) . . . yes O(22) S(5) O(23) 110.9(5) . . . yes O(22) S(5) O(24) 108.1(5) . . . yes O(22) S(5) C(5) 102.2(4) . . . yes O(23) S(5) O(24) 119.1(5) . . . yes O(23) S(5) C(5) 108.0(4) . . . yes O(24) S(5) C(5) 107.2(4) . . . yes O(22') S(5) O(23') 113.2(6) . . . yes O(22') S(5) O(24') 118.9(6) . . . yes O(22') S(5) C(5) 107.5(4) . . . yes O(23') S(5) O(24') 107.9(6) . . . yes O(23') S(5) C(5) 102.4(5) . . . yes O(24') S(5) C(5) 105.4(4) . . . yes O(12) S(6) O(13) 113.0(2) . . . yes O(12) S(6) O(14) 111.4(2) . . . yes O(12) S(6) C(11) 106.5(2) . . . yes O(13) S(6) O(14) 112.4(2) . . . yes O(13) S(6) C(11) 108.0(2) . . . yes O(14) S(6) C(11) 105.1(2) . . . yes O(9) S(7) O(11) 113.0(2) . . . yes O(9) S(7) O(16) 110.5(2) . . . yes O(9) S(7) C(17) 106.0(2) . . . yes O(11) S(7) O(16) 114.6(2) . . . yes O(11) S(7) C(17) 105.0(2) . . . yes O(16) S(7) C(17) 107.0(2) . . . yes O(10) S(8) O(15) 111.9(2) . . . yes O(10) S(8) O(17) 113.9(2) . . . yes O(10) S(8) C(23) 105.7(2) . . . yes O(15) S(8) O(17) 112.6(2) . . . yes O(15) S(8) C(23) 106.1(2) . . . yes O(17) S(8) C(23) 105.8(2) . . . yes O(16) Na(1) O(17) 149.4(2) 1_655 . 3_755 yes O(16) Na(1) O(23) 108.3(2) 1_655 . . yes O(16) Na(1) O(103) 100.3(2) 1_655 . . yes O(16) Na(1) O(104) 91.5(2) 1_655 . . yes O(17) Na(1) O(23) 82.1(2) 3_755 . . yes O(17) Na(1) O(103) 79.4(1) 3_755 . . yes O(17) Na(1) O(104) 118.8(2) 3_755 . . yes O(23) Na(1) O(103) 148.9(2) . . . yes O(23) Na(1) O(104) 82.4(2) . . . yes O(103) Na(1) O(104) 84.9(2) . . . yes Na(5) Na(2) O(1) 144.4(1) 2_655 . . yes Na(5) Na(2) O(11) 47.80(10) 2_655 . 4_554 yes Na(5) Na(2) O(13) 53.7(1) 2_655 . 4_454 yes Na(5) Na(2) O(18) 128.3(1) 2_655 . . yes Na(5) Na(2) O(19) 136.6(1) 2_655 . . yes Na(5) Na(2) O(101) 49.3(1) 2_655 . . yes O(1) Na(2) O(11) 96.7(1) . . 4_554 yes O(1) Na(2) O(13) 126.2(2) . . 4_454 yes O(1) Na(2) O(18) 71.4(1) . . . yes O(1) Na(2) O(19) 72.9(1) . . . yes O(1) Na(2) O(101) 137.6(2) . . . yes O(11) Na(2) O(13) 78.4(1) 4_554 . 4_454 yes O(11) Na(2) O(18) 126.7(1) 4_554 . . yes O(11) Na(2) O(19) 153.7(1) 4_554 . . yes O(11) Na(2) O(101) 77.2(1) 4_554 . . yes O(13) Na(2) O(18) 150.4(2) 4_454 . . yes O(13) Na(2) O(19) 88.3(1) 4_454 . . yes O(13) Na(2) O(101) 94.0(2) 4_454 . . yes O(18) Na(2) O(19) 73.8(1) . . . yes O(18) Na(2) O(101) 79.1(1) . . . yes O(19) Na(2) O(101) 126.8(1) . . . yes O(10) Na(3) O(15) 128.8(2) 3_655 . . yes O(10) Na(3) O(24) 92.1(2) 3_655 . 1_455 yes O(10) Na(3) O(107) 84.7(2) 3_655 . . yes O(10) Na(3) O(108) 145.9(2) 3_655 . . yes O(15) Na(3) O(24) 106.6(2) . . 1_455 yes O(15) Na(3) O(107) 96.9(2) . . . yes O(15) Na(3) O(108) 84.3(1) . . . yes O(24) Na(3) O(107) 151.8(2) 1_455 . . yes O(24) Na(3) O(108) 84.4(2) 1_455 . . yes O(107) Na(3) O(108) 82.9(2) . . . yes O(2) Na(4) O(7) 91.6(1) 1_556 . 4_555 yes O(2) Na(4) O(12) 168.9(2) 1_556 . . yes O(2) Na(4) O(102) 90.8(2) 1_556 . . yes O(2) Na(4) O(106) 89.6(1) 1_556 . . yes O(2) Na(4) O(109) 88.3(1) 1_556 . . yes O(7) Na(4) O(12) 80.9(1) 4_555 . . yes O(7) Na(4) O(102) 177.1(2) 4_555 . . yes O(7) Na(4) O(106) 96.1(1) 4_555 . . yes O(7) Na(4) O(109) 85.1(1) 4_555 . . yes O(12) Na(4) O(102) 97.0(2) . . . yes O(12) Na(4) O(106) 99.3(2) . . . yes O(12) Na(4) O(109) 82.9(1) . . . yes O(102) Na(4) O(106) 82.2(2) . . . yes O(102) Na(4) O(109) 96.7(2) . . . yes O(106) Na(4) O(109) 177.6(2) . . . yes Na(2) Na(5) O(9) 129.9(1) 2_645 . . yes Na(2) Na(5) O(11) 51.3(1) 2_645 . 3_656 yes Na(2) Na(5) O(13) 45.48(10) 2_645 . 3_756 yes Na(2) Na(5) O(101) 46.7(1) 2_645 . 2_645 yes Na(2) Na(5) O(105) 130.4(1) 2_645 . . yes Na(2) Na(5) O(108) 100.8(1) 2_645 . 3_655 yes O(9) Na(5) O(11) 102.7(2) . . 3_656 yes O(9) Na(5) O(13) 175.2(2) . . 3_756 yes O(9) Na(5) O(101) 90.7(1) . . 2_645 yes O(9) Na(5) O(105) 93.8(2) . . . yes O(9) Na(5) O(108) 98.8(2) . . 3_655 yes O(11) Na(5) O(13) 75.2(1) 3_656 . 3_756 yes O(11) Na(5) O(101) 77.9(1) 3_656 . 2_645 yes O(11) Na(5) O(105) 103.2(2) 3_656 . . yes O(11) Na(5) O(108) 151.9(2) 3_656 . 3_655 yes O(13) Na(5) O(101) 84.6(1) 3_756 . 2_645 yes O(13) Na(5) O(105) 91.0(1) 3_756 . . yes O(13) Na(5) O(108) 81.9(1) 3_756 . 3_655 yes O(101) Na(5) O(105) 175.0(2) 2_645 . . yes O(101) Na(5) O(108) 84.0(1) 2_645 . 3_655 yes O(105) Na(5) O(108) 93.1(2) . . 3_655 yes S(1) O(1) Na(2) 134.4(2) . . . yes S(1) O(2) Na(4) 168.0(2) . . 1_554 yes S(4) O(7) Na(4) 141.6(2) . . 4_454 yes S(7) O(9) Na(5) 140.5(2) . . . yes S(8) O(10) Na(3) 167.0(3) . . 3_655 yes S(7) O(11) Na(2) 123.2(2) . . 4_455 yes S(7) O(11) Na(5) 144.1(2) . . 3_656 yes Na(2) O(11) Na(5) 80.8(1) 4_455 . 3_656 yes S(6) O(12) Na(4) 136.9(2) . . . yes S(6) O(13) Na(2) 154.5(2) . . 4_555 yes S(6) O(13) Na(5) 120.8(2) . . 3_756 yes Na(2) O(13) Na(5) 80.8(1) 4_555 . 3_756 yes S(8) O(15) Na(3) 105.2(2) . . . yes S(7) O(16) Na(1) 110.1(2) . . 1_455 yes S(8) O(17) Na(1) 133.8(2) . . 3_755 yes Na(2) O(18) C(2) 142.7(3) . . . yes Na(2) O(19) C(20) 135.8(3) . . . yes S(5) O(23) Na(1) 120.7(5) . . . yes S(5) O(24) Na(3) 112.8(4) . . 1_655 yes S(5) O(22') Na(1) 133.4(5) . . . yes S(5) O(24') Na(3) 129.4(6) . . 1_655 yes Na(2) O(101) Na(5) 83.9(1) . . 2_655 yes Na(3) O(108) Na(5) 125.3(2) . . 3_655 yes S(1) C(1) C(2) 123.4(4) . . . yes S(1) C(1) C(6) 115.6(4) . . . yes C(2) C(1) C(6) 121.0(4) . . . yes O(18) C(2) C(1) 120.3(4) . . . yes O(18) C(2) C(3) 123.3(4) . . . yes C(1) C(2) C(3) 116.4(4) . . . yes S(2) C(3) C(2) 122.5(4) . . . yes S(2) C(3) C(4) 115.3(3) . . . yes C(2) C(3) C(4) 122.2(4) . . . yes C(3) C(4) C(5) 119.5(4) . . . yes S(5) C(5) C(4) 118.5(4) . . . yes S(5) C(5) C(6) 121.9(4) . . . yes C(4) C(5) C(6) 119.7(5) . . . yes C(1) C(6) C(5) 121.1(4) . . . yes S(2) C(7) C(8) 119.8(4) . . . yes S(2) C(7) C(12) 118.5(4) . . . yes C(8) C(7) C(12) 121.7(4) . . . yes O(21) C(8) C(7) 117.4(4) . . . yes O(21) C(8) C(9) 125.3(4) . . . yes C(7) C(8) C(9) 117.3(4) . . . yes S(3) C(9) C(8) 121.8(4) . . . yes S(3) C(9) C(10) 117.4(4) . . . yes C(8) C(9) C(10) 120.5(4) . . . yes C(9) C(10) C(11) 120.5(4) . . . yes S(6) C(11) C(10) 118.4(4) . . . yes S(6) C(11) C(12) 120.5(4) . . . yes C(10) C(11) C(12) 121.0(4) . . . yes C(7) C(12) C(11) 118.8(4) . . . yes S(3) C(13) C(14) 119.9(3) . . . yes S(3) C(13) C(18) 118.2(4) . . . yes C(14) C(13) C(18) 121.5(4) . . . yes O(20) C(14) C(13) 122.7(4) . . . yes O(20) C(14) C(15) 122.6(4) . . . yes C(13) C(14) C(15) 114.7(4) . . . yes S(4) C(15) C(14) 119.9(3) . . . yes S(4) C(15) C(16) 116.9(3) . . . yes C(14) C(15) C(16) 123.3(4) . . . yes C(15) C(16) C(17) 119.1(4) . . . yes S(7) C(17) C(16) 119.2(4) . . . yes S(7) C(17) C(18) 120.2(4) . . . yes C(16) C(17) C(18) 120.6(4) . . . yes C(13) C(18) C(17) 120.5(4) . . . yes S(4) C(19) C(20) 122.7(3) . . . yes S(4) C(19) C(24) 116.4(3) . . . yes C(20) C(19) C(24) 120.9(4) . . . yes O(19) C(20) C(19) 123.9(4) . . . yes O(19) C(20) C(21) 118.7(4) . . . yes C(19) C(20) C(21) 117.4(4) . . . yes S(1) C(21) C(20) 121.8(4) . . . yes S(1) C(21) C(22) 116.5(4) . . . yes C(20) C(21) C(22) 121.7(4) . . . yes C(21) C(22) C(23) 119.7(4) . . . yes S(8) C(23) C(22) 119.7(4) . . . yes S(8) C(23) C(24) 120.5(4) . . . yes C(22) C(23) C(24) 119.7(4) . . . yes C(19) C(24) C(23) 120.5(4) . . . yes O(100) C(25) C(26) 115(1) . . . yes Na(2) O(18) H(31) 106.4 . . . no C(2) O(18) H(31) 110.7 . . . no Na(2) O(19) H(32) 103.5 . . . no C(20) O(19) H(32) 119.4 . . . no C(14) O(20) H(33) 123.7 . . . no C(8) O(21) H(30) 113.2 . . . no C(25) O(100) H(34) 110.7 . . . no Na(2) O(101) H(9) 118.6 . . . no Na(2) O(101) H(10) 128.3 . . . no Na(5) O(101) H(9) 98.1 2_655 . . no Na(5) O(101) H(10) 107.1 2_655 . . no H(9) O(101) H(10) 109.8 . . . no Na(4) O(102) H(14) 135.2 . . . no Na(4) O(102) H(29) 110.9 . . . no H(14) O(102) H(29) 113.4 . . . no Na(1) O(103) H(22) 114.4 . . . no Na(1) O(103) H(23) 105.9 . . . no H(22) O(103) H(23) 115.3 . . . no Na(1) O(104) H(35) 109.8 . . . no Na(1) O(104) H(36) 110.0 . . . no H(35) O(104) H(36) 110.9 . . . no Na(5) O(105) H(15) 90.7 . . . no Na(5) O(105) H(16) 105.0 . . . no H(15) O(105) H(16) 97.8 . . . no Na(4) O(106) H(11) 103.3 . . . no Na(4) O(106) H(24) 128.9 . . . no H(11) O(106) H(24) 106.6 . . . no Na(3) O(107) H(12) 110.8 . . . no Na(3) O(107) H(13) 112.0 . . . no H(12) O(107) H(13) 100.4 . . . no Na(3) O(108) H(27) 114.3 . . . no Na(3) O(108) H(28) 102.2 . . . no Na(5) O(108) H(27) 102.6 3_655 . . no Na(5) O(108) H(28) 103.2 3_655 . . no H(27) O(108) H(28) 107.8 . . . no Na(4) O(109) H(25) 112.7 . . . no Na(4) O(109) H(26) 115.6 . . . no H(25) O(109) H(26) 97.2 . . . no C(3) C(4) H(5) 116.3 . . . no C(5) C(4) H(5) 124.2 . . . no C(1) C(6) H(6) 118.6 . . . no C(5) C(6) H(6) 120.3 . . . no C(9) C(10) H(1) 117.5 . . . no C(11) C(10) H(1) 122.1 . . . no C(7) C(12) H(2) 117.1 . . . no C(11) C(12) H(2) 123.8 . . . no C(15) C(16) H(3) 119.4 . . . no C(17) C(16) H(3) 121.5 . . . no C(13) C(18) H(4) 116.5 . . . no C(17) C(18) H(4) 122.9 . . . no C(21) C(22) H(7) 119.4 . . . no C(23) C(22) H(7) 120.8 . . . no C(19) C(24) H(8) 118.3 . . . no C(23) C(24) H(8) 121.2 . . . no O(100) C(25) H(17) 114.0 . . . no O(100) C(25) H(18) 104.3 . . . no C(26) C(25) H(17) 100.3 . . . no C(26) C(25) H(18) 106.5 . . . no H(17) C(25) H(18) 116.8 . . . no C(25) C(26) H(19) 107.9 . . . no C(25) C(26) H(20) 110.0 . . . no C(25) C(26) H(21) 111.1 . . . no H(19) C(26) H(20) 107.1 . . . no H(19) C(26) H(21) 108.8 . . . no H(20) C(26) H(21) 111.8 . . . no #------------------------------------------------------------------------------