Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_uehara-150k _database_code_CSD 154471 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Hirama, Masahiro' 'Kosaka, Masashi' 'Le Brazidec, Jean-Yves' 'Nagumo, Yoko' 'Oishi, Tohru' 'Shoji, Mitsuru' 'Uehara, Hisatoshi' _publ_contact_author_name 'Prof. Masahiro Hirama' _publ_contact_author_address ; Prof. Masahiro Hirama Department of Chemistry Graduate School of Science Tohoku University Sendai 980-8578, JAPAN ; _publ_contact_author_email 'hirama@ykbsc.chem.tohoku.ac.jp' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C39 H48 Br2 O10 ' _chemical_formula_moiety 'C39 H48 Br2 O10 ' _chemical_formula_weight 836.61 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 5.5284(3) _cell_length_b 25.006(2) _cell_length_c 27.913(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3858.7(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5951 _cell_measurement_theta_min ? _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.806 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_reflns_number 27206 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.00 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7494 _reflns_number_gt 4740 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1518 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4740 _refine_ls_number_parameters 460 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0040 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.02(1) _refine_diff_density_max 0.67 _refine_diff_density_min -0.33 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 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 Br(1) Br -0.0588(2) 0.14862(4) -0.14530(3) 0.1138(4) Uani 1.00 d . . . Br(2) Br 1.1483(1) 0.38873(2) 0.26150(2) 0.0675(2) Uani 1.00 d . . . O(1) O -0.5731(6) -0.1443(1) -0.0710(1) 0.0496(8) Uani 1.00 d . . . O(2) O -0.1646(6) -0.1420(1) -0.0499(1) 0.0454(8) Uani 1.00 d . . . O(3) O -0.2216(6) -0.0234(1) 0.0269(1) 0.0479(8) Uani 1.00 d . . . O(4) O 0.1490(6) -0.0607(1) 0.1310(1) 0.0411(7) Uani 1.00 d . . . O(5) O 0.1224(7) 0.0834(1) 0.1508(1) 0.0511(9) Uani 1.00 d . . . O(6) O 0.2209(6) -0.1212(2) 0.0181(1) 0.0508(9) Uani 1.00 d . . . O(7) O 0.5096(7) 0.1642(1) 0.2234(1) 0.064(1) Uani 1.00 d . . . O(8) O 0.2458(9) 0.1637(2) 0.0884(2) 0.069(1) Uani 1.00 d . . . O(9) O -0.114(1) 0.2050(2) 0.0946(2) 0.096(2) Uani 1.00 d . . . O(10) O 0.3018(8) 0.1896(1) 0.2887(1) 0.060(1) Uani 1.00 d . . . C(1) C -0.281(1) -0.1704(3) -0.1268(2) 0.065(2) Uani 1.00 d . . . C(2) C -0.407(1) -0.2202(3) -0.1094(2) 0.071(2) Uani 1.00 d . . . C(3) C -0.603(1) -0.2010(2) -0.0759(3) 0.074(2) Uani 1.00 d . . . C(4) C -0.3365(10) -0.1297(2) -0.0868(2) 0.052(1) Uani 1.00 d . . . C(5) C -0.328(1) -0.0710(2) -0.0992(2) 0.057(1) Uani 1.00 d . . . C(6) C -0.354(1) -0.0357(2) -0.0539(2) 0.054(1) Uani 1.00 d . . . C(7) C -0.1752(9) -0.0538(2) -0.0157(2) 0.041(1) Uani 1.00 d . . . C(8) C -0.2022(7) -0.1125(2) -0.0058(2) 0.037(1) Uani 1.00 d . . . C(9) C -0.0224(8) -0.1367(2) 0.0291(2) 0.041(1) Uani 1.00 d . . . C(10) C -0.0642(8) -0.1245(2) 0.0824(2) 0.036(1) Uani 1.00 d . . . C(11) C -0.0511(8) -0.0654(2) 0.0981(2) 0.036(1) Uani 1.00 d . . . C(12) C -0.0242(9) -0.0222(2) 0.0598(2) 0.043(1) Uani 1.00 d . . . C(13) C -0.030(1) 0.0320(2) 0.0848(2) 0.047(1) Uani 1.00 d . . . C(14) C 0.1598(9) 0.0350(2) 0.1239(2) 0.042(1) Uani 1.00 d . . . C(15) C 0.1416(9) -0.0115(2) 0.1580(2) 0.042(1) Uani 1.00 d . . . C(16) C 0.348(1) -0.0162(2) 0.1945(2) 0.050(1) Uani 1.00 d . . . C(17) C 0.326(1) 0.0188(2) 0.2405(2) 0.053(1) Uani 1.00 d . . . C(18) C 0.466(1) 0.0711(2) 0.2392(2) 0.064(2) Uani 1.00 d . . . C(19) C 0.352(1) 0.1188(2) 0.2150(2) 0.056(1) Uani 1.00 d . . . C(20) C 0.329(1) 0.1155(2) 0.1606(2) 0.057(1) Uani 1.00 d . . . C(21) C -0.516(1) -0.0565(3) -0.1367(2) 0.079(2) Uani 1.00 d . . . C(22) C -0.308(2) 0.0230(2) -0.0659(3) 0.087(2) Uani 1.00 d . . . C(23) C 0.422(1) -0.0155(3) 0.2832(2) 0.076(2) Uani 1.00 d . . . C(24) C 0.289(1) 0.1698(2) 0.1391(2) 0.073(2) Uani 1.00 d . . . C(25) C 0.034(1) 0.1827(2) 0.0712(2) 0.064(2) Uani 1.00 d . . . C(26) C 0.018(1) 0.1733(2) 0.0186(2) 0.061(2) Uani 1.00 d . . . C(27) C -0.182(1) 0.1942(2) -0.0050(3) 0.070(2) Uani 1.00 d . . . C(28) C -0.203(1) 0.1870(3) -0.0542(3) 0.077(2) Uani 1.00 d . . . C(29) C -0.026(1) 0.1594(3) -0.0790(2) 0.071(2) Uani 1.00 d . . . C(30) C 0.170(1) 0.1387(3) -0.0555(2) 0.071(2) Uani 1.00 d . . . C(31) C 0.192(1) 0.1464(2) -0.0069(2) 0.059(1) Uani 1.00 d . . . C(32) C 0.460(1) 0.1970(2) 0.2607(2) 0.049(1) Uani 1.00 d . . . C(33) C 0.6301(9) 0.2436(2) 0.2603(2) 0.043(1) Uani 1.00 d . . . C(34) C 0.805(1) 0.2489(2) 0.2262(2) 0.069(2) Uani 1.00 d . . . C(35) C 0.961(1) 0.2908(3) 0.2267(2) 0.072(2) Uani 1.00 d . . . C(36) C 0.9361(9) 0.3290(2) 0.2618(2) 0.047(1) Uani 1.00 d . . . C(37) C 0.758(1) 0.3256(2) 0.2961(2) 0.053(1) Uani 1.00 d . . . C(38) C 0.606(1) 0.2822(2) 0.2952(2) 0.050(1) Uani 1.00 d . . . C(39) C -0.2968(10) -0.1499(2) 0.1000(2) 0.050(1) Uani 1.00 d . . . H(1) H -0.3390 -0.1594 -0.1571 0.0782 Uiso 1.00 calc . . . H(2) H -0.1076 -0.1764 -0.1297 0.0782 Uiso 1.00 calc . . . H(3) H -0.4710 -0.2395 -0.1364 0.0849 Uiso 1.00 calc . . . H(4) H -0.2928 -0.2434 -0.0937 0.0849 Uiso 1.00 calc . . . H(5) H -0.7596 -0.2109 -0.0886 0.1002 Uiso 1.00 calc . . . H(6) H -0.5877 -0.2193 -0.0454 0.1002 Uiso 1.00 calc . . . H(7) H -0.1674 -0.0630 -0.1143 0.0766 Uiso 1.00 calc . . . H(8) H -0.5210 -0.0399 -0.0419 0.0740 Uiso 1.00 calc . . . H(9) H -0.3632 -0.1199 0.0058 0.0490 Uiso 1.00 calc . . . H(10) H -0.0259 -0.1757 0.0244 0.0550 Uiso 1.00 calc . . . H(11) H 0.0605 -0.1429 0.1004 0.0417 Uiso 1.00 calc . . . H(12) H -0.1971 -0.0568 0.1162 0.0459 Uiso 1.00 calc . . . H(13) H 0.1264 -0.0268 0.0430 0.0536 Uiso 1.00 calc . . . H(14) H -0.0080 0.0605 0.0622 0.0573 Uiso 1.00 calc . . . H(15) H -0.1883 0.0373 0.0993 0.0573 Uiso 1.00 calc . . . H(16) H 0.3173 0.0370 0.1095 0.0519 Uiso 1.00 calc . . . H(17) H -0.0052 -0.0102 0.1760 0.0518 Uiso 1.00 calc . . . H(18) H 0.4937 -0.0050 0.1773 0.0629 Uiso 1.00 calc . . . H(19) H 0.3672 -0.0526 0.2027 0.0629 Uiso 1.00 calc . . . H(20) H 0.1267 0.0343 0.2431 0.1006 Uiso 1.00 calc . . . H(21) H 0.6201 0.0635 0.2232 0.0750 Uiso 1.00 calc . . . H(22) H 0.5075 0.0799 0.2719 0.0750 Uiso 1.00 calc . . . H(23) H 0.1940 0.1256 0.2287 0.0701 Uiso 1.00 calc . . . H(24) H -0.5084 -0.0776 -0.1651 0.0960 Uiso 1.00 calc . . . H(25) H -0.5202 -0.0199 -0.1449 0.0960 Uiso 1.00 calc . . . H(26) H -0.6834 -0.0642 -0.1234 0.0960 Uiso 1.00 calc . . . H(27) H -0.4225 0.0371 -0.0881 0.1005 Uiso 1.00 calc . . . H(28) H -0.1503 0.0291 -0.0768 0.1005 Uiso 1.00 calc . . . H(29) H -0.3284 0.0449 -0.0362 0.1005 Uiso 1.00 calc . . . H(30) H 0.3438 -0.0562 0.2892 0.1006 Uiso 1.00 calc . . . H(31) H 0.6412 -0.0287 0.2776 0.1006 Uiso 1.00 calc . . . H(32) H 0.3446 0.0102 0.3083 0.1006 Uiso 1.00 calc . . . H(33) H 0.4747 0.0990 0.1463 0.0720 Uiso 1.00 calc . . . H(34) H 0.1575 0.1883 0.1551 0.0883 Uiso 1.00 calc . . . H(35) H 0.4321 0.1936 0.1449 0.0883 Uiso 1.00 calc . . . H(36) H -0.3039 0.2131 0.0128 0.0788 Uiso 1.00 calc . . . H(37) H -0.3441 0.2009 -0.0715 0.0920 Uiso 1.00 calc . . . H(38) H 0.2865 0.1181 -0.0738 0.0894 Uiso 1.00 calc . . . H(39) H 0.3262 0.1304 0.0105 0.0727 Uiso 1.00 calc . . . H(40) H 0.8105 0.2219 0.2011 0.0755 Uiso 1.00 calc . . . H(41) H 1.0929 0.2943 0.2021 0.0790 Uiso 1.00 calc . . . H(42) H 0.7402 0.3528 0.3205 0.0609 Uiso 1.00 calc . . . H(43) H 0.4877 0.2779 0.3206 0.0544 Uiso 1.00 calc . . . H(44) H -0.3265 -0.1883 0.0978 0.1006 Uiso 1.00 calc . . . H(45) H -0.3862 -0.1421 0.1271 0.1006 Uiso 1.00 calc . . . H(46) H -0.4523 -0.1271 0.0869 0.1006 Uiso 1.00 calc . . . H(47) H 0.2961 -0.1366 -0.0189 0.1006 Uiso 1.00 calc . . . H(48) H -0.0088 -0.0468 -0.0269 0.1067 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 Br(1) 0.1557(9) 0.1162(7) 0.0697(5) 0.0205(6) -0.0280(5) 0.0067(4) Br(2) 0.0720(4) 0.0668(4) 0.0637(4) -0.0154(3) 0.0043(3) -0.0087(3) O(1) 0.042(2) 0.056(2) 0.051(2) -0.003(2) 0.005(2) -0.017(2) O(2) 0.035(2) 0.061(2) 0.040(2) 0.003(2) 0.004(2) -0.014(2) O(3) 0.052(2) 0.039(2) 0.053(2) 0.002(2) -0.012(2) -0.001(2) O(4) 0.046(2) 0.039(2) 0.039(2) 0.006(2) -0.004(2) -0.006(1) O(5) 0.053(2) 0.042(2) 0.059(2) 0.003(2) -0.001(2) -0.015(2) O(6) 0.032(2) 0.072(2) 0.049(2) 0.002(2) 0.000(1) -0.012(2) O(7) 0.065(3) 0.061(2) 0.065(2) -0.007(2) 0.006(2) -0.031(2) O(8) 0.091(3) 0.057(2) 0.058(2) -0.001(2) -0.005(2) -0.013(2) O(9) 0.087(4) 0.105(4) 0.096(4) 0.011(3) 0.018(3) -0.031(3) O(10) 0.072(3) 0.056(2) 0.051(2) -0.008(2) 0.005(2) -0.011(2) C(1) 0.054(4) 0.096(4) 0.045(3) 0.002(3) 0.004(3) -0.021(3) C(2) 0.060(4) 0.078(4) 0.076(4) 0.001(3) -0.001(3) -0.036(3) C(3) 0.061(4) 0.055(4) 0.106(5) -0.006(3) 0.016(4) -0.028(3) C(4) 0.043(3) 0.072(3) 0.041(3) -0.004(3) 0.002(2) -0.006(2) C(5) 0.062(4) 0.065(3) 0.043(3) -0.001(3) -0.009(3) -0.003(2) C(6) 0.059(3) 0.048(3) 0.057(3) -0.006(3) -0.019(3) 0.004(2) C(7) 0.041(3) 0.044(2) 0.039(2) -0.004(2) -0.006(2) -0.002(2) C(8) 0.035(2) 0.042(2) 0.034(2) -0.002(2) 0.004(2) -0.011(2) C(9) 0.036(3) 0.041(3) 0.046(3) 0.004(2) 0.006(2) -0.004(2) C(10) 0.038(2) 0.034(2) 0.036(2) 0.007(2) 0.000(2) 0.001(2) C(11) 0.034(2) 0.036(2) 0.037(2) -0.003(2) 0.001(2) -0.002(2) C(12) 0.041(3) 0.042(3) 0.046(3) -0.001(2) -0.006(2) -0.003(2) C(13) 0.057(3) 0.038(3) 0.047(3) -0.001(2) -0.002(3) 0.001(2) C(14) 0.044(3) 0.038(2) 0.044(2) 0.004(2) 0.002(2) -0.012(2) C(15) 0.042(3) 0.048(3) 0.037(2) 0.006(2) -0.002(2) -0.010(2) C(16) 0.057(3) 0.047(3) 0.046(3) 0.012(3) -0.005(3) -0.013(2) C(17) 0.068(3) 0.052(3) 0.040(3) 0.008(3) -0.008(3) -0.014(2) C(18) 0.070(4) 0.068(4) 0.053(3) 0.007(3) -0.011(3) -0.025(3) C(19) 0.063(3) 0.049(3) 0.056(3) 0.000(3) 0.001(3) -0.016(2) C(20) 0.063(3) 0.043(3) 0.064(3) -0.007(3) 0.004(3) -0.012(2) C(21) 0.103(5) 0.082(4) 0.053(3) -0.001(4) -0.028(4) 0.004(3) C(22) 0.129(7) 0.053(3) 0.079(4) -0.002(4) -0.032(5) 0.016(3) C(23) 0.113(6) 0.069(4) 0.045(3) 0.019(4) -0.005(4) -0.013(3) C(24) 0.105(5) 0.061(4) 0.054(3) -0.013(4) -0.003(3) -0.017(3) C(25) 0.069(4) 0.050(3) 0.074(4) -0.014(3) 0.006(4) -0.008(3) C(26) 0.064(4) 0.043(3) 0.075(4) -0.011(3) -0.002(3) 0.008(3) C(27) 0.063(4) 0.052(3) 0.094(5) 0.003(3) -0.005(4) -0.008(3) C(28) 0.078(5) 0.057(4) 0.096(5) 0.005(3) -0.024(4) 0.004(4) C(29) 0.083(5) 0.061(4) 0.068(4) -0.004(4) -0.016(4) 0.002(3) C(30) 0.067(4) 0.082(4) 0.065(4) 0.009(4) -0.001(3) -0.005(3) C(31) 0.052(3) 0.064(3) 0.062(3) 0.010(3) 0.001(3) 0.001(3) C(32) 0.059(3) 0.048(3) 0.040(3) 0.010(2) -0.010(3) -0.006(3) C(33) 0.051(3) 0.044(2) 0.035(2) 0.001(2) -0.007(3) -0.006(2) C(34) 0.077(4) 0.069(4) 0.063(4) -0.010(3) 0.009(3) -0.035(3) C(35) 0.060(4) 0.091(5) 0.066(4) -0.017(4) 0.017(3) -0.022(3) C(36) 0.051(3) 0.047(3) 0.043(3) -0.007(2) -0.010(3) -0.007(2) C(37) 0.072(4) 0.049(3) 0.040(3) 0.001(3) 0.001(3) -0.004(2) C(38) 0.066(4) 0.046(3) 0.036(2) 0.004(3) 0.005(2) 0.000(2) C(39) 0.049(3) 0.044(3) 0.056(3) -0.012(2) 0.010(2) 0.006(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution DirectMethod _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _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 Br(1) C(29) 1.878(7) . . yes Br(2) C(36) 1.899(5) . . yes O(1) C(3) 1.433(7) . . yes O(1) C(4) 1.428(6) . . yes O(2) C(4) 1.437(6) . . yes O(2) C(8) 1.450(5) . . yes O(3) C(7) 1.434(6) . . yes O(3) C(12) 1.427(6) . . yes O(4) C(11) 1.443(5) . . yes O(4) C(15) 1.444(5) . . yes O(5) C(14) 1.439(5) . . yes O(5) C(20) 1.422(7) . . yes O(6) C(9) 1.433(6) . . yes O(7) C(19) 1.452(7) . . yes O(7) C(32) 1.354(6) . . yes O(8) C(24) 1.444(7) . . yes O(8) C(25) 1.353(9) . . yes O(9) C(25) 1.182(9) . . yes O(10) C(32) 1.188(7) . . yes C(1) C(2) 1.510(9) . . yes C(1) C(4) 1.541(8) . . yes C(2) C(3) 1.509(9) . . yes C(4) C(5) 1.509(8) . . yes C(5) C(6) 1.548(7) . . yes C(5) C(21) 1.519(9) . . yes C(6) C(7) 1.523(7) . . yes C(6) C(22) 1.528(8) . . yes C(7) C(8) 1.503(6) . . yes C(8) C(9) 1.517(6) . . yes C(9) C(10) 1.536(6) . . yes C(10) C(11) 1.544(6) . . yes C(10) C(39) 1.516(7) . . yes C(11) C(12) 1.525(6) . . yes C(12) C(13) 1.526(7) . . yes C(13) C(14) 1.516(7) . . yes C(14) C(15) 1.506(6) . . yes C(15) C(16) 1.534(7) . . yes C(16) C(17) 1.557(7) . . yes C(17) C(18) 1.521(8) . . yes C(17) C(23) 1.561(8) . . yes C(18) C(19) 1.509(8) . . yes C(19) C(20) 1.524(8) . . yes C(20) C(24) 1.503(8) . . yes C(25) C(26) 1.492(9) . . yes C(26) C(27) 1.387(9) . . yes C(26) C(31) 1.372(8) . . yes C(27) C(28) 1.39(1) . . yes C(28) C(29) 1.385(10) . . yes C(29) C(30) 1.372(10) . . yes C(30) C(31) 1.375(9) . . yes C(32) C(33) 1.496(7) . . yes C(33) C(34) 1.363(8) . . yes C(33) C(38) 1.380(7) . . yes C(34) C(35) 1.354(9) . . yes C(35) C(36) 1.377(8) . . yes C(36) C(37) 1.375(8) . . yes C(37) C(38) 1.373(8) . . yes O(6) H(47) 1.176 . . no C(1) H(1) 0.944 . . no C(1) H(2) 0.974 . . no C(2) H(3) 0.961 . . no C(2) H(4) 0.963 . . no C(3) H(5) 0.968 . . no C(3) H(6) 0.972 . . no C(5) H(7) 1.005 . . no C(6) H(8) 0.984 . . no C(7) H(48) 0.986 . . no C(8) H(9) 0.965 . . no C(9) H(10) 0.982 . . no C(10) H(11) 0.970 . . no C(11) H(12) 0.977 . . no C(12) H(13) 0.963 . . no C(13) H(14) 0.959 . . no C(13) H(15) 0.973 . . no C(14) H(16) 0.960 . . no C(15) H(17) 0.954 . . no C(16) H(18) 0.980 . . no C(16) H(19) 0.942 . . no C(17) H(20) 1.168 . . no C(18) H(21) 0.982 . . no C(18) H(22) 0.967 . . no C(19) H(23) 0.967 . . no C(20) H(33) 0.989 . . no C(21) H(24) 0.952 . . no C(21) H(25) 0.944 . . no C(21) H(26) 1.015 . . no C(22) H(27) 0.953 . . no C(22) H(28) 0.935 . . no C(22) H(29) 1.000 . . no C(23) H(30) 1.119 . . no C(23) H(31) 1.268 . . no C(23) H(32) 1.041 . . no C(24) H(34) 0.970 . . no C(24) H(35) 1.003 . . no C(27) H(36) 0.963 . . no C(28) H(37) 0.980 . . no C(30) H(38) 0.969 . . no C(31) H(39) 0.974 . . no C(34) H(40) 0.975 . . no C(35) H(41) 1.007 . . no C(37) H(42) 0.966 . . no C(38) H(43) 0.971 . . no C(39) H(44) 0.977 . . no C(39) H(45) 0.924 . . no C(39) H(46) 1.095 . . 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 C(3) O(1) C(4) 109.2(4) . 1_555 1_555 yes C(4) O(2) C(8) 113.9(3) . 1_555 1_555 yes C(7) O(3) C(12) 114.1(4) . 1_555 1_555 yes C(11) O(4) C(15) 112.3(3) . 1_555 1_555 yes C(14) O(5) C(20) 117.4(4) . 1_555 1_555 yes C(19) O(7) C(32) 118.5(4) . 1_555 1_555 yes C(24) O(8) C(25) 116.9(5) . 1_555 1_555 yes C(2) C(1) C(4) 102.7(5) . 1_555 1_555 yes C(1) C(2) C(3) 105.5(5) . 1_555 1_555 yes O(1) C(3) C(2) 107.0(5) . 1_555 1_555 yes O(1) C(4) O(2) 109.2(4) . 1_555 1_555 yes O(1) C(4) C(1) 103.7(4) . 1_555 1_555 yes O(1) C(4) C(5) 110.3(4) . 1_555 1_555 yes O(2) C(4) C(1) 104.3(4) . 1_555 1_555 yes O(2) C(4) C(5) 110.7(4) . 1_555 1_555 yes C(1) C(4) C(5) 118.1(4) . 1_555 1_555 yes C(4) C(5) C(6) 111.3(4) . 1_555 1_555 yes C(4) C(5) C(21) 111.6(5) . 1_555 1_555 yes C(6) C(5) C(21) 111.4(5) . 1_555 1_555 yes C(5) C(6) C(7) 110.0(4) . 1_555 1_555 yes C(5) C(6) C(22) 110.5(5) . 1_555 1_555 yes C(7) C(6) C(22) 109.2(5) . 1_555 1_555 yes O(3) C(7) C(6) 107.9(4) . 1_555 1_555 yes O(3) C(7) C(8) 110.3(4) . 1_555 1_555 yes C(6) C(7) C(8) 110.7(4) . 1_555 1_555 yes O(2) C(8) C(7) 109.1(3) . 1_555 1_555 yes O(2) C(8) C(9) 104.3(3) . 1_555 1_555 yes C(7) C(8) C(9) 116.4(4) . 1_555 1_555 yes O(6) C(9) C(8) 111.7(4) . 1_555 1_555 yes O(6) C(9) C(10) 107.1(4) . 1_555 1_555 yes C(8) C(9) C(10) 116.3(4) . 1_555 1_555 yes C(9) C(10) C(11) 117.3(4) . 1_555 1_555 yes C(9) C(10) C(39) 111.0(4) . 1_555 1_555 yes C(11) C(10) C(39) 110.4(4) . 1_555 1_555 yes O(4) C(11) C(10) 107.1(3) . 1_555 1_555 yes O(4) C(11) C(12) 108.3(3) . 1_555 1_555 yes C(10) C(11) C(12) 118.9(4) . 1_555 1_555 yes O(3) C(12) C(11) 111.2(4) . 1_555 1_555 yes O(3) C(12) C(13) 107.3(4) . 1_555 1_555 yes C(11) C(12) C(13) 107.9(4) . 1_555 1_555 yes C(12) C(13) C(14) 111.0(4) . 1_555 1_555 yes O(5) C(14) C(13) 108.4(4) . 1_555 1_555 yes O(5) C(14) C(15) 108.1(4) . 1_555 1_555 yes C(13) C(14) C(15) 111.8(4) . 1_555 1_555 yes O(4) C(15) C(14) 109.1(3) . 1_555 1_555 yes O(4) C(15) C(16) 105.1(4) . 1_555 1_555 yes C(14) C(15) C(16) 115.4(4) . 1_555 1_555 yes C(15) C(16) C(17) 116.4(4) . 1_555 1_555 yes C(16) C(17) C(18) 115.1(4) . 1_555 1_555 yes C(16) C(17) C(23) 107.1(4) . 1_555 1_555 yes C(18) C(17) C(23) 108.4(5) . 1_555 1_555 yes C(17) C(18) C(19) 118.5(5) . 1_555 1_555 yes O(7) C(19) C(18) 107.1(4) . 1_555 1_555 yes O(7) C(19) C(20) 104.6(4) . 1_555 1_555 yes C(18) C(19) C(20) 115.9(4) . 1_555 1_555 yes O(5) C(20) C(19) 106.8(4) . 1_555 1_555 yes O(5) C(20) C(24) 108.3(5) . 1_555 1_555 yes C(19) C(20) C(24) 111.2(4) . 1_555 1_555 yes O(8) C(24) C(20) 108.7(5) . 1_555 1_555 yes O(8) C(25) O(9) 124.6(6) . 1_555 1_555 yes O(8) C(25) C(26) 110.1(5) . 1_555 1_555 yes O(9) C(25) C(26) 125.2(6) . 1_555 1_555 yes C(25) C(26) C(27) 117.1(6) . 1_555 1_555 yes C(25) C(26) C(31) 123.1(6) . 1_555 1_555 yes C(27) C(26) C(31) 119.8(6) . 1_555 1_555 yes C(26) C(27) C(28) 119.2(6) . 1_555 1_555 yes C(27) C(28) C(29) 119.9(6) . 1_555 1_555 yes Br(1) C(29) C(28) 119.8(5) . 1_555 1_555 yes Br(1) C(29) C(30) 119.6(5) . 1_555 1_555 yes C(28) C(29) C(30) 120.6(6) . 1_555 1_555 yes C(29) C(30) C(31) 119.2(6) . 1_555 1_555 yes C(26) C(31) C(30) 121.3(6) . 1_555 1_555 yes O(7) C(32) O(10) 124.1(5) . 1_555 1_555 yes O(7) C(32) C(33) 109.7(4) . 1_555 1_555 yes O(10) C(32) C(33) 126.1(5) . 1_555 1_555 yes C(32) C(33) C(34) 121.9(4) . 1_555 1_555 yes C(32) C(33) C(38) 118.6(4) . 1_555 1_555 yes C(34) C(33) C(38) 119.5(5) . 1_555 1_555 yes C(33) C(34) C(35) 121.3(5) . 1_555 1_555 yes C(34) C(35) C(36) 118.8(6) . 1_555 1_555 yes Br(2) C(36) C(35) 118.8(4) . 1_555 1_555 yes Br(2) C(36) C(37) 119.6(4) . 1_555 1_555 yes C(35) C(36) C(37) 121.6(5) . 1_555 1_555 yes C(36) C(37) C(38) 118.3(5) . 1_555 1_555 yes C(33) C(38) C(37) 120.5(5) . 1_555 1_555 yes C(9) O(6) H(47) 115.6 . 1_555 1_555 no C(2) C(1) H(1) 111.7 . 1_555 1_555 no C(2) C(1) H(2) 110.7 . 1_555 1_555 no C(4) C(1) H(1) 112.9 . 1_555 1_555 no C(4) C(1) H(2) 110.9 . 1_555 1_555 no H(1) C(1) H(2) 107.9 . 1_555 1_555 no C(1) C(2) H(3) 109.4 . 1_555 1_555 no C(1) C(2) H(4) 109.8 . 1_555 1_555 no C(3) C(2) H(3) 112.5 . 1_555 1_555 no C(3) C(2) H(4) 112.3 . 1_555 1_555 no H(3) C(2) H(4) 107.4 . 1_555 1_555 no O(1) C(3) H(5) 113.0 . 1_555 1_555 no O(1) C(3) H(6) 111.9 . 1_555 1_555 no C(2) C(3) H(5) 109.5 . 1_555 1_555 no C(2) C(3) H(6) 109.3 . 1_555 1_555 no H(5) C(3) H(6) 106.1 . 1_555 1_555 no C(4) C(5) H(7) 108.3 . 1_555 1_555 no C(6) C(5) H(7) 108.2 . 1_555 1_555 no C(21) C(5) H(7) 105.6 . 1_555 1_555 no C(5) C(6) H(8) 107.6 . 1_555 1_555 no C(7) C(6) H(8) 109.9 . 1_555 1_555 no C(22) C(6) H(8) 109.5 . 1_555 1_555 no O(3) C(7) H(48) 109.5 . 1_555 1_555 no C(6) C(7) H(48) 109.6 . 1_555 1_555 no C(8) C(7) H(48) 108.8 . 1_555 1_555 no O(2) C(8) H(9) 108.7 . 1_555 1_555 no C(7) C(8) H(9) 109.9 . 1_555 1_555 no C(9) C(8) H(9) 108.3 . 1_555 1_555 no O(6) C(9) H(10) 105.0 . 1_555 1_555 no C(8) C(9) H(10) 107.3 . 1_555 1_555 no C(10) C(9) H(10) 108.9 . 1_555 1_555 no C(9) C(10) H(11) 107.6 . 1_555 1_555 no C(11) C(10) H(11) 105.8 . 1_555 1_555 no C(39) C(10) H(11) 103.6 . 1_555 1_555 no O(4) C(11) H(12) 106.6 . 1_555 1_555 no C(10) C(11) H(12) 108.6 . 1_555 1_555 no C(12) C(11) H(12) 106.7 . 1_555 1_555 no O(3) C(12) H(13) 110.1 . 1_555 1_555 no C(11) C(12) H(13) 110.0 . 1_555 1_555 no C(13) C(12) H(13) 110.3 . 1_555 1_555 no C(12) C(13) H(14) 110.8 . 1_555 1_555 no C(12) C(13) H(15) 109.2 . 1_555 1_555 no C(14) C(13) H(14) 110.5 . 1_555 1_555 no C(14) C(13) H(15) 108.4 . 1_555 1_555 no H(14) C(13) H(15) 106.8 . 1_555 1_555 no O(5) C(14) H(16) 107.7 . 1_555 1_555 no C(13) C(14) H(16) 109.2 . 1_555 1_555 no C(15) C(14) H(16) 111.4 . 1_555 1_555 no O(4) C(15) H(17) 109.2 . 1_555 1_555 no C(14) C(15) H(17) 111.2 . 1_555 1_555 no C(16) C(15) H(17) 106.6 . 1_555 1_555 no C(15) C(16) H(18) 105.2 . 1_555 1_555 no C(15) C(16) H(19) 108.6 . 1_555 1_555 no C(17) C(16) H(18) 108.1 . 1_555 1_555 no C(17) C(16) H(19) 110.6 . 1_555 1_555 no H(18) C(16) H(19) 107.5 . 1_555 1_555 no C(16) C(17) H(20) 108.2 . 1_555 1_555 no C(18) C(17) H(20) 101.3 . 1_555 1_555 no C(23) C(17) H(20) 117.1 . 1_555 1_555 no C(17) C(18) H(21) 106.7 . 1_555 1_555 no C(17) C(18) H(22) 107.2 . 1_555 1_555 no C(19) C(18) H(21) 108.2 . 1_555 1_555 no C(19) C(18) H(22) 110.0 . 1_555 1_555 no H(21) C(18) H(22) 105.4 . 1_555 1_555 no O(7) C(19) H(23) 109.9 . 1_555 1_555 no C(18) C(19) H(23) 109.8 . 1_555 1_555 no C(20) C(19) H(23) 109.2 . 1_555 1_555 no O(5) C(20) H(33) 110.0 . 1_555 1_555 no C(19) C(20) H(33) 111.0 . 1_555 1_555 no C(24) C(20) H(33) 109.5 . 1_555 1_555 no C(5) C(21) H(24) 114.3 . 1_555 1_555 no C(5) C(21) H(25) 114.3 . 1_555 1_555 no C(5) C(21) H(26) 108.8 . 1_555 1_555 no H(24) C(21) H(25) 109.8 . 1_555 1_555 no H(24) C(21) H(26) 104.0 . 1_555 1_555 no H(25) C(21) H(26) 104.6 . 1_555 1_555 no C(6) C(22) H(27) 112.7 . 1_555 1_555 no C(6) C(22) H(28) 112.7 . 1_555 1_555 no C(6) C(22) H(29) 109.0 . 1_555 1_555 no H(27) C(22) H(28) 110.4 . 1_555 1_555 no H(27) C(22) H(29) 105.1 . 1_555 1_555 no H(28) C(22) H(29) 106.4 . 1_555 1_555 no C(17) C(23) H(30) 118.9 . 1_555 1_555 no C(17) C(23) H(31) 112.0 . 1_555 1_555 no C(17) C(23) H(32) 92.1 . 1_555 1_555 no H(30) C(23) H(31) 98.6 . 1_555 1_555 no H(30) C(23) H(32) 107.7 . 1_555 1_555 no H(31) C(23) H(32) 129.5 . 1_555 1_555 no O(8) C(24) H(34) 112.3 . 1_555 1_555 no O(8) C(24) H(35) 110.5 . 1_555 1_555 no C(20) C(24) H(34) 110.9 . 1_555 1_555 no C(20) C(24) H(35) 110.8 . 1_555 1_555 no H(34) C(24) H(35) 103.6 . 1_555 1_555 no C(26) C(27) H(36) 119.8 . 1_555 1_555 no C(28) C(27) H(36) 121.0 . 1_555 1_555 no C(27) C(28) H(37) 120.7 . 1_555 1_555 no C(29) C(28) H(37) 119.4 . 1_555 1_555 no C(29) C(30) H(38) 118.1 . 1_555 1_555 no C(31) C(30) H(38) 122.7 . 1_555 1_555 no C(26) C(31) H(39) 118.6 . 1_555 1_555 no C(30) C(31) H(39) 119.9 . 1_555 1_555 no C(33) C(34) H(40) 117.0 . 1_555 1_555 no C(35) C(34) H(40) 121.6 . 1_555 1_555 no C(34) C(35) H(41) 121.5 . 1_555 1_555 no C(36) C(35) H(41) 119.7 . 1_555 1_555 no C(36) C(37) H(42) 121.3 . 1_555 1_555 no C(38) C(37) H(42) 120.4 . 1_555 1_555 no C(33) C(38) H(43) 120.2 . 1_555 1_555 no C(37) C(38) H(43) 119.2 . 1_555 1_555 no C(10) C(39) H(44) 122.3 . 1_555 1_555 no C(10) C(39) H(45) 129.1 . 1_555 1_555 no C(10) C(39) H(46) 109.8 . 1_555 1_555 no H(44) C(39) H(45) 99.7 . 1_555 1_555 no H(44) C(39) H(46) 111.1 . 1_555 1_555 no H(45) C(39) H(46) 75.1 . 1_555 1_555 no #------------------------------------------------------------------------------ #===END