# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 207/329 data_2 #--------------------------------------------------- _audit_creation_date 'Thu Dec 24 15:02:52 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 556.69 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H44 O8 ' _chemical_formula_moiety 'C32 H44 O8' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------- _cell_length_a 11.727(4) _cell_length_b 10.915(4) _cell_length_c 12.109(4) _cell_angle_alpha 90 _cell_angle_beta 112.25(2) _cell_angle_gamma 90 _cell_volume 1434.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.5 _cell_measurement_theta_max 20.0 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 600.00 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.057 _exptl_absorpt_correction_T_min 0.894 _exptl_special_details ; ? ; #----------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.27 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 -1 2 -2 -1 1 -2 0 _diffrn_reflns_number 4584 _reflns_number_total 4395 _reflns_number_observed 2939 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07426 _diffrn_orient_matrix_UB_12 -0.05162 _diffrn_orient_matrix_UB_13 0.04219 _diffrn_orient_matrix_UB_21 -0.04177 _diffrn_orient_matrix_UB_22 -0.03582 _diffrn_orient_matrix_UB_23 0.05083 _diffrn_orient_matrix_UB_31 -0.03505 _diffrn_orient_matrix_UB_32 -0.06668 _diffrn_orient_matrix_UB_33 -0.05997 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 88 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #---------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags O(1) 0.0647(1) 0.20385(9) 0.78662(9) 0.0427(3) Uani d . 1.00 . O(2) -0.18290(10) 0.25146(9) 0.70363(9) 0.0427(3) Uani d . 1.00 . O(3) 0.35377(8) 0.4527(1) 0.84446(9) 0.0467(3) Uani d . 1.00 . O(4) 0.36601(9) 0.6048(1) 0.47151(9) 0.0493(3) Uani d . 1.00 . C(1) 0.0733(1) 0.3053(1) 0.8655(1) 0.0320(3) Uani d . 1.00 . C(2) -0.0283(1) 0.3997(1) 0.8039(1) 0.0309(3) Uani d . 1.00 . C(3) -0.1591(1) 0.3560(1) 0.7837(1) 0.0344(3) Uani d . 1.00 . C(4) -0.1636(1) 0.3126(2) 0.9019(1) 0.0459(4) Uani d . 1.00 . C(5) -0.0682(1) 0.2137(2) 0.9600(1) 0.0488(4) Uani d . 1.00 . C(6) 0.0611(1) 0.2589(2) 0.9801(1) 0.0435(4) Uani d . 1.00 . C(7) 0.2020(1) 0.3588(1) 0.8972(1) 0.0368(3) Uani d . 1.00 . C(8) 0.2315(1) 0.4056(2) 0.7936(1) 0.0407(4) Uani d . 1.00 . C(9) 0.3958(1) 0.5276(1) 0.7770(1) 0.0355(3) Uani d . 1.00 . C(10) 0.3533(1) 0.5208(1) 0.6530(1) 0.0352(3) Uani d . 1.00 . C(11) 0.4019(1) 0.6015(1) 0.5930(1) 0.0363(3) Uani d . 1.00 . C(12) 0.4908(1) 0.6868(1) 0.6556(1) 0.0459(4) Uani d . 1.00 . C(13) 0.5316(1) 0.6898(2) 0.7781(1) 0.0541(4) Uani d . 1.00 . C(14) 0.4855(1) 0.6108(2) 0.8398(1) 0.0490(4) Uani d . 1.00 . C(15) 0.2818(1) 0.5138(1) 0.4012(1) 0.0393(3) Uani d . 1.00 . C(16) -0.2550(1) 0.4572(1) 0.7286(1) 0.0413(4) Uani d . 1.00 . H(1) -0.016(2) 0.192(2) 0.752(2) 0.072(6) Uiso calc . 1.00 . H(2) -0.261(2) 0.247(2) 0.664(2) 0.100(8) Uiso calc . 1.00 . H(3) -0.023(1) 0.426(1) 0.721(1) 0.040(4) Uiso calc . 1.00 . H(4) -0.012(1) 0.474(1) 0.861(1) 0.045(4) Uiso calc . 1.00 . H(5) -0.150(1) 0.391(2) 0.954(1) 0.047(4) Uiso calc . 1.00 . H(6) -0.247(2) 0.292(2) 0.892(2) 0.059(5) Uiso calc . 1.00 . H(7) -0.072(2) 0.188(2) 1.040(2) 0.063(5) Uiso calc . 1.00 . H(8) -0.085(1) 0.138(2) 0.902(2) 0.054(5) Uiso calc . 1.00 . H(9) 0.085(1) 0.332(2) 1.037(1) 0.042(4) Uiso calc . 1.00 . H(10) 0.124(2) 0.191(2) 1.011(2) 0.061(5) Uiso calc . 1.00 . H(11) 0.211(2) 0.428(2) 0.960(2) 0.054(5) Uiso calc . 1.00 . H(12) 0.260(2) 0.291(2) 0.937(1) 0.055(4) Uiso calc . 1.00 . H(13) 0.175(2) 0.475(2) 0.746(2) 0.054(5) Uiso calc . 1.00 . H(14) 0.226(2) 0.343(2) 0.739(2) 0.067(5) Uiso calc . 1.00 . H(15) 0.291(1) 0.463(1) 0.612(1) 0.043(4) Uiso calc . 1.00 . H(16) 0.512(2) 0.610(2) 0.916(2) 0.078(6) Uiso calc . 1.00 . H(17) 0.598(2) 0.748(2) 0.824(2) 0.081(6) Uiso calc . 1.00 . H(18) 0.519(1) 0.746(1) 0.608(1) 0.049(4) Uiso calc . 1.00 . H(19) 0.205(1) 0.515(1) 0.416(1) 0.038(4) Uiso calc . 1.00 . H(20) 0.323(1) 0.434(1) 0.426(1) 0.043(4) Uiso calc . 1.00 . H(21) -0.331(2) 0.435(2) 0.740(2) 0.059(5) Uiso calc . 1.00 . H(22) -0.224(1) 0.535(2) 0.779(1) 0.052(4) Uiso calc . 1.00 . 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 O(1) 0.0456(6) 0.0343(5) 0.0458(6) 0.0021(4) 0.0146(4) -0.0072(4) O(2) 0.0402(5) 0.0402(6) 0.0418(5) -0.0065(4) 0.0088(4) -0.0094(4) O(3) 0.0317(5) 0.0624(7) 0.0401(5) -0.0090(4) 0.0070(4) 0.0094(5) O(4) 0.0488(6) 0.0538(6) 0.0386(5) -0.0179(5) 0.0087(4) 0.0061(4) C(1) 0.0350(6) 0.0306(6) 0.0284(6) -0.0011(5) 0.0099(5) 0.0007(5) C(2) 0.0334(6) 0.0290(6) 0.0304(6) -0.0018(5) 0.0124(5) 0.0003(5) C(3) 0.0347(6) 0.0358(6) 0.0326(6) -0.0038(5) 0.0126(5) -0.0016(5) C(4) 0.0443(8) 0.0590(10) 0.0405(7) -0.0081(7) 0.0229(6) 0.0034(7) C(5) 0.0547(9) 0.0547(9) 0.0390(7) -0.0107(7) 0.0197(6) 0.0112(7) C(6) 0.0475(8) 0.0487(9) 0.0319(6) -0.0022(7) 0.0125(6) 0.0099(6) C(7) 0.0332(6) 0.0413(7) 0.0326(6) -0.0011(6) 0.0089(5) 0.0022(6) C(8) 0.0307(6) 0.0516(8) 0.0364(7) -0.0070(6) 0.0089(5) 0.0027(6) C(9) 0.0276(5) 0.0379(7) 0.0390(7) 0.0000(5) 0.0102(5) 0.0023(5) C(10) 0.0297(6) 0.0325(6) 0.0389(7) -0.0025(5) 0.0079(5) 0.0017(5) C(11) 0.0305(6) 0.0350(7) 0.0402(7) 0.0009(5) 0.0097(5) 0.0039(5) C(12) 0.0389(7) 0.0425(8) 0.0533(8) -0.0112(6) 0.0139(6) 0.0015(6) C(13) 0.0474(8) 0.0542(10) 0.0533(9) -0.0214(7) 0.0107(7) -0.0097(7) C(14) 0.0431(7) 0.0587(10) 0.0405(8) -0.0121(7) 0.0104(6) -0.0062(7) C(15) 0.0346(6) 0.0380(7) 0.0420(7) -0.0007(6) 0.0108(5) 0.0019(6) C(16) 0.0352(7) 0.0473(8) 0.0426(7) 0.0028(6) 0.0162(6) -0.0003(6) #-------------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2939 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0520 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.950 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.14 _refine_diff_density_max 0.19 #---------------------------------------------------------------------- _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 O(1) C(1) 1.441(2) 1_555 1_555 yes O(1) H(1) 0.89(2) 1_555 1_555 no O(2) C(3) 1.454(2) 1_555 1_555 yes O(2) H(2) 0.86(2) 1_555 1_555 no O(3) C(8) 1.425(2) 1_555 1_555 yes O(3) C(9) 1.372(2) 1_555 1_555 yes O(4) C(11) 1.369(2) 1_555 1_555 yes O(4) C(15) 1.432(2) 1_555 1_555 yes C(1) C(2) 1.538(2) 1_555 1_555 yes C(1) C(6) 1.533(2) 1_555 1_555 yes C(1) C(7) 1.525(2) 1_555 1_555 yes C(2) C(3) 1.534(2) 1_555 1_555 yes C(2) H(3) 1.07(2) 1_555 1_555 no C(2) H(4) 1.03(2) 1_555 1_555 no C(3) C(4) 1.527(2) 1_555 1_555 yes C(3) C(16) 1.537(2) 1_555 1_555 yes C(4) C(5) 1.522(2) 1_555 1_555 yes C(4) H(5) 1.04(2) 1_555 1_555 no C(4) H(6) 0.96(2) 1_555 1_555 no C(5) C(6) 1.524(2) 1_555 1_555 yes C(5) H(7) 1.02(2) 1_555 1_555 no C(5) H(8) 1.05(2) 1_555 1_555 no C(6) H(9) 1.02(2) 1_555 1_555 no C(6) H(10) 1.01(2) 1_555 1_555 no C(7) C(8) 1.511(2) 1_555 1_555 yes C(7) H(11) 1.04(2) 1_555 1_555 no C(7) H(12) 1.00(2) 1_555 1_555 no C(8) H(13) 1.02(2) 1_555 1_555 no C(8) H(14) 0.94(2) 1_555 1_555 no C(9) C(10) 1.394(2) 1_555 1_555 yes C(9) C(14) 1.380(2) 1_555 1_555 yes C(10) C(11) 1.393(2) 1_555 1_555 yes C(10) H(15) 0.95(2) 1_555 1_555 no C(11) C(12) 1.389(2) 1_555 1_555 yes C(12) C(13) 1.376(2) 1_555 1_555 yes C(12) H(18) 1.00(2) 1_555 1_555 no C(13) C(14) 1.378(2) 1_555 1_555 yes C(13) H(17) 0.99(2) 1_555 1_555 no C(14) H(16) 0.85(2) 1_555 1_555 no C(15) C(16) 1.515(2) 1_555 3_566 yes C(15) H(19) 0.98(1) 1_555 1_555 no C(15) H(20) 0.98(2) 1_555 1_555 no C(16) H(21) 0.99(2) 1_555 1_555 no C(16) H(22) 1.03(2) 1_555 1_555 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) H(1) O(2) 150(1) 1_555 1_555 1_555 no O(2) H(2) O(4) 122(2) 1_555 1_555 3_566 no O(2) H(2) O(3) 109(1) 1_555 1_555 2_546 no O(4) H(2) O(3) 124.5(9) 3_566 1_555 2_546 no O(2) H(3) O(1) 62.6(4) 1_555 1_555 1_555 no O(2) H(3) O(1) 127.9(5) 1_555 1_555 2_556 no O(1) H(3) O(1) 163.3(6) 1_555 1_555 2_556 no O(1) H(4) O(2) 109.4(5) 2_556 1_555 1_555 no O(1) H(4) O(1) 126.9(5) 2_556 1_555 1_555 no O(2) H(4) O(1) 49.3(2) 1_555 1_555 1_555 no O(2) H(6) O(4) 129.7(6) 1_555 1_555 2_546 no O(2) H(7) O(1) 55.4(3) 4_555 1_555 4_555 no O(2) H(8) O(1) 62.4(4) 1_555 1_555 1_555 no O(1) H(9) O(1) 146.6(6) 4_555 1_555 1_555 no O(3) H(11) O(1) 91.4(5) 1_555 1_555 1_555 no O(1) H(12) O(3) 111.7(6) 1_555 1_555 1_555 no O(3) H(13) O(2) 93.2(6) 1_555 1_555 2_556 no O(3) H(13) O(1) 100.6(6) 1_555 1_555 1_555 no O(2) H(13) O(1) 145.6(6) 2_556 1_555 1_555 no O(3) H(14) O(1) 129.4(9) 1_555 1_555 1_555 no O(3) H(15) O(4) 132.6(6) 1_555 1_555 1_555 no O(3) H(16) O(3) 104.4(7) 1_555 1_555 3_667 no O(4) H(18) O(3) 152.5(7) 1_555 1_555 2_656 no O(4) H(19) O(2) 68.3(4) 1_555 1_555 3_566 no O(4) H(19) O(1) 146.4(7) 1_555 1_555 4_554 no O(2) H(19) O(1) 121.1(5) 3_566 1_555 4_554 no O(4) H(20) O(1) 133.4(7) 1_555 1_555 4_554 no O(4) H(20) O(4) 83.5(5) 1_555 1_555 3_666 no O(1) H(20) O(4) 142.6(5) 4_554 1_555 3_666 no O(4) H(21) O(2) 65.2(4) 3_566 1_555 1_555 no O(1) H(22) O(4) 101.4(5) 2_556 1_555 3_566 no O(1) H(22) O(2) 109.8(5) 2_556 1_555 1_555 no O(4) H(22) O(2) 51.6(3) 3_566 1_555 1_555 no #------------------------------------------------------ #------------------------------------------------------------------------- _publ_requested_journal ' J.Chem.Soc.Perkin Trans.1' _publ_contact_author ; Dr. Tadashi Mizutani Department of Synthetic Chemistry and Biological Chemistry, Graduate School of Engineerin g, Kyoto University, Sakyo-ku, Kyoto 606-8501 Japan ; _publ_contact_letter ; Paper ref. 8/09834D ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-78-803-1348' _publ_contact_author_fax ' +81-78-803-0832' _publ_contact_author_email ' htakagi@kobe-u.ac.jp'