# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/406 data_Compound9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C23 H43 N O9 Si' _chemical_formula_sum 'C23 H43 N O9 Si' _chemical_formula_weight 505.67 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.824(2) _cell_length_b 13.368(2) _cell_length_c 22.340(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2933.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 9.7 _cell_measurement_theta_max 19.2 _exptl_crystal_description needle _exptl_crystal_colour white _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 496 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10536 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 22.00 _reflns_number_total 3588 _reflns_number_gt 2369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1490P)^2^+2.7544P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(7) _refine_ls_number_reflns 3588 _refine_ls_number_parameters 307 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2709 _refine_ls_wR_factor_gt 0.2280 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 1.3358(4) 0.1348(4) -0.1973(2) 0.1700(18) Uani 1 d DU . . O7A O 0.8829(5) 0.4555(4) -0.0402(3) 0.1009(19) Uani 1 d . . . O7B O 0.6688(6) 0.4096(4) -0.0331(4) 0.119(2) Uani 1 d . . . O8 O 0.9656(5) 0.2792(4) -0.0075(4) 0.118(2) Uani 1 d . . . O10 O 0.7371(5) 0.1147(4) 0.0816(2) 0.0842(15) Uani 1 d . . . O12 O 0.7048(6) -0.0567(4) 0.0739(3) 0.0882(16) Uani 1 d . . . O13 O 0.8791(6) -0.2088(3) 0.0206(3) 0.0978(18) Uani 1 d . . . O15 O 0.7693(4) 0.0431(3) -0.0760(2) 0.0719(13) Uani 1 d . . . O17 O 0.9431(8) 0.1311(8) -0.2347(4) 0.169(4) Uani 1 d . . . O18 O 1.1962(7) 0.1126(6) -0.1624(4) 0.136(3) Uani 1 d U . . N9 N 0.7533(5) 0.2222(4) 0.0013(3) 0.0753(18) Uani 1 d . . . H9 H 0.6686 0.2366 -0.0032 0.090 Uiso 1 calc R . . C7 C 0.7865(7) 0.3914(5) -0.0290(4) 0.076(2) Uani 1 d . . . C7A C 0.8443(10) 0.5554(7) -0.0586(5) 0.121(4) Uani 1 d . . . H7A1 H 0.9247 0.5949 -0.0648 0.182 Uiso 0.50 calc PR . . H7A2 H 0.7896 0.5857 -0.0279 0.182 Uiso 0.50 calc PR . . H7A3 H 0.7931 0.5520 -0.0951 0.182 Uiso 0.50 calc PR . . H7A4 H 0.7469 0.5601 -0.0604 0.182 Uiso 0.50 calc PR . . H7A5 H 0.8820 0.5694 -0.0973 0.182 Uiso 0.50 calc PR . . H7A6 H 0.8785 0.6031 -0.0301 0.182 Uiso 0.50 calc PR . . C8 C 0.8441(7) 0.2909(5) -0.0111(4) 0.074(2) Uani 1 d . . . C10 C 0.7891(6) 0.1233(5) 0.0220(4) 0.0684(19) Uani 1 d . . . H10 H 0.8882 0.1151 0.0221 0.082 Uiso 1 calc R . . C10A C 0.7687(10) 0.0199(7) 0.1045(4) 0.098(3) Uani 1 d . . . H10A H 0.8664 0.0100 0.1025 0.117 Uiso 1 calc R . . H10B H 0.7421 0.0172 0.1463 0.117 Uiso 1 calc R . . C11 C 0.7235(6) 0.0429(5) -0.0162(3) 0.0627(17) Uani 1 d . . . H11 H 0.6257 0.0575 -0.0172 0.075 Uiso 1 calc R . . C12 C 0.7391(6) -0.0606(5) 0.0114(3) 0.0677(19) Uani 1 d . . . H12 H 0.6726 -0.1045 -0.0081 0.081 Uiso 1 calc R . . C13 C 0.8801(7) -0.1056(5) 0.0003(3) 0.0705(19) Uani 1 d . . . H13 H 0.9484 -0.0678 0.0230 0.085 Uiso 1 calc R . . C13A C 0.9336(12) -0.2247(8) 0.0776(5) 0.128(4) Uani 1 d . . . H13A H 0.9288 -0.2946 0.0872 0.191 Uiso 0.50 calc PR . . H13B H 0.8826 -0.1871 0.1065 0.191 Uiso 0.50 calc PR . . H13C H 1.0269 -0.2033 0.0782 0.191 Uiso 0.50 calc PR . . H13D H 0.9634 -0.1621 0.0941 0.191 Uiso 0.50 calc PR . . H13E H 1.0096 -0.2696 0.0748 0.191 Uiso 0.50 calc PR . . H13F H 0.8653 -0.2534 0.1031 0.191 Uiso 0.50 calc PR . . C14 C 0.9160(8) -0.1035(6) -0.0657(4) 0.079(2) Uani 1 d . . . C14A C 0.8188(9) -0.1724(6) -0.1025(4) 0.099(3) Uani 1 d . . . H14A H 0.8282 -0.2402 -0.0891 0.148 Uiso 0.50 calc PR . . H14B H 0.8419 -0.1683 -0.1442 0.148 Uiso 0.50 calc PR . . H14C H 0.7264 -0.1509 -0.0969 0.148 Uiso 0.50 calc PR . . H14D H 0.7694 -0.1327 -0.1311 0.148 Uiso 0.50 calc PR . . H14E H 0.7558 -0.2046 -0.0759 0.148 Uiso 0.50 calc PR . . H14F H 0.8713 -0.2221 -0.1232 0.148 Uiso 0.50 calc PR . . C14B C 1.0650(8) -0.1382(7) -0.0724(4) 0.099(3) Uani 1 d . . . H14G H 1.0729 -0.2065 -0.0597 0.148 Uiso 0.50 calc PR . . H14H H 1.1228 -0.0968 -0.0482 0.148 Uiso 0.50 calc PR . . H14I H 1.0920 -0.1328 -0.1136 0.148 Uiso 0.50 calc PR . . H14J H 1.1190 -0.0843 -0.0880 0.148 Uiso 0.50 calc PR . . H14K H 1.0690 -0.1940 -0.0994 0.148 Uiso 0.50 calc PR . . H14L H 1.0998 -0.1579 -0.0340 0.148 Uiso 0.50 calc PR . . C15 C 0.9035(7) 0.0054(5) -0.0870(4) 0.073(2) Uani 1 d . . . H15 H 0.9679 0.0459 -0.0638 0.087 Uiso 1 calc R . . C16 C 0.9312(8) 0.0229(7) -0.1520(4) 0.086(2) Uani 1 d . . . H16A H 1.0105 -0.0157 -0.1635 0.103 Uiso 1 calc R . . H16B H 0.8545 -0.0019 -0.1750 0.103 Uiso 1 calc R . . C17 C 0.9550(10) 0.1299(8) -0.1685(5) 0.117(3) Uani 1 d . . . H17 H 0.8801 0.1697 -0.1520 0.140 Uiso 1 calc R . . C17A C 0.8968(19) 0.2117(16) -0.2623(8) 0.245(11) Uani 1 d . . . H17A H 0.8953 0.2000 -0.3047 0.368 Uiso 0.50 calc PR . . H17B H 0.9552 0.2675 -0.2537 0.368 Uiso 0.50 calc PR . . H17C H 0.8063 0.2262 -0.2486 0.368 Uiso 0.50 calc PR . . H17D H 0.8759 0.2625 -0.2333 0.368 Uiso 0.50 calc PR . . H17E H 0.8160 0.1950 -0.2843 0.368 Uiso 0.50 calc PR . . H17F H 0.9649 0.2363 -0.2894 0.368 Uiso 0.50 calc PR . . C18 C 1.0864(10) 0.1740(7) -0.1465(5) 0.110(3) Uani 1 d U . . H18A H 1.0988 0.2399 -0.1639 0.132 Uiso 1 calc R . . H18B H 1.0831 0.1812 -0.1034 0.132 Uiso 1 calc R . . C19 C 1.4701(14) 0.2080(13) -0.1576(8) 0.258(8) Uani 1 d DU . . H19A H 1.4317 0.2692 -0.1427 0.388 Uiso 0.50 calc PR . . H19B H 1.5427 0.2229 -0.1849 0.388 Uiso 0.50 calc PR . . H19C H 1.5048 0.1694 -0.1247 0.388 Uiso 0.50 calc PR . . H19D H 1.5545 0.1718 -0.1588 0.388 Uiso 0.50 calc PR . . H19E H 1.4434 0.2180 -0.1167 0.388 Uiso 0.50 calc PR . . H19F H 1.4814 0.2716 -0.1768 0.388 Uiso 0.50 calc PR . . C20 C 1.304(2) 0.2333(14) -0.2545(9) 0.276(9) Uani 1 d DU . . H20A H 1.2600 0.2896 -0.2360 0.414 Uiso 0.50 calc PR . . H20B H 1.2464 0.2069 -0.2855 0.414 Uiso 0.50 calc PR . . H20C H 1.3889 0.2543 -0.2716 0.414 Uiso 0.50 calc PR . . H20D H 1.3368 0.2110 -0.2927 0.414 Uiso 0.50 calc PR . . H20E H 1.3505 0.2936 -0.2433 0.414 Uiso 0.50 calc PR . . H20F H 1.2079 0.2462 -0.2571 0.414 Uiso 0.50 calc PR . . C21 C 1.4176(10) 0.0169(5) -0.2218(6) 0.186(5) Uani 1 d DU . . C22 C 1.5551(13) 0.0335(14) -0.2526(7) 0.257(9) Uani 1 d DU . . H22A H 1.6174 0.0637 -0.2249 0.385 Uiso 0.50 calc PR . . H22B H 1.5432 0.0769 -0.2865 0.385 Uiso 0.50 calc PR . . H22C H 1.5910 -0.0295 -0.2658 0.385 Uiso 0.50 calc PR . . H22D H 1.5503 0.0103 -0.2932 0.385 Uiso 0.50 calc PR . . H22E H 1.6245 -0.0029 -0.2316 0.385 Uiso 0.50 calc PR . . H22F H 1.5768 0.1036 -0.2523 0.385 Uiso 0.50 calc PR . . C23 C 1.3145(17) -0.0319(18) -0.2644(9) 0.381(15) Uani 1 d DU . . H23A H 1.2309 -0.0440 -0.2434 0.571 Uiso 0.50 calc PR . . H23B H 1.3504 -0.0941 -0.2788 0.571 Uiso 0.50 calc PR . . H23C H 1.2975 0.0120 -0.2976 0.571 Uiso 0.50 calc PR . . H23D H 1.3550 -0.0401 -0.3032 0.571 Uiso 0.50 calc PR . . H23E H 1.2354 0.0100 -0.2677 0.571 Uiso 0.50 calc PR . . H23F H 1.2884 -0.0961 -0.2489 0.571 Uiso 0.50 calc PR . . C24 C 1.4362(17) -0.0462(16) -0.1650(8) 0.353(15) Uani 1 d DU . . H24A H 1.3490 -0.0588 -0.1472 0.530 Uiso 0.50 calc PR . . H24B H 1.4926 -0.0106 -0.1371 0.530 Uiso 0.50 calc PR . . H24C H 1.4787 -0.1086 -0.1751 0.530 Uiso 0.50 calc PR . . H24D H 1.5312 -0.0598 -0.1591 0.530 Uiso 0.50 calc PR . . H24E H 1.3876 -0.1081 -0.1692 0.530 Uiso 0.50 calc PR . . H24F H 1.4015 -0.0100 -0.1311 0.530 Uiso 0.50 calc PR . . 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 Si1 0.147(3) 0.184(4) 0.178(3) 0.034(3) 0.079(3) 0.025(3) O7A 0.060(3) 0.062(3) 0.180(6) 0.020(4) 0.001(3) -0.007(3) O7B 0.057(3) 0.072(4) 0.228(8) 0.030(4) -0.003(4) 0.007(3) O8 0.040(3) 0.085(4) 0.228(8) 0.032(5) -0.006(4) 0.000(3) O10 0.077(3) 0.079(4) 0.096(4) 0.000(3) 0.004(3) 0.015(3) O12 0.089(4) 0.076(3) 0.099(4) 0.012(3) 0.011(3) -0.004(3) O13 0.105(4) 0.052(3) 0.137(5) 0.020(3) 0.001(4) 0.007(3) O15 0.054(3) 0.068(3) 0.093(4) 0.009(3) -0.009(3) 0.007(2) O17 0.153(7) 0.223(10) 0.131(6) 0.084(7) 0.009(5) 0.049(7) O18 0.100(4) 0.117(5) 0.190(7) 0.042(5) 0.036(4) 0.018(3) N9 0.036(3) 0.047(3) 0.142(5) 0.004(4) -0.004(3) 0.004(2) C7 0.048(4) 0.060(4) 0.121(6) 0.002(4) 0.014(4) -0.001(4) C7A 0.089(6) 0.084(6) 0.190(11) 0.030(6) 0.004(6) -0.009(5) C8 0.040(3) 0.063(4) 0.117(6) -0.003(4) 0.005(4) 0.001(3) C10 0.041(3) 0.056(4) 0.108(6) 0.003(4) -0.011(4) 0.004(3) C10A 0.098(6) 0.102(7) 0.093(6) -0.006(5) -0.006(5) 0.009(6) C11 0.041(3) 0.065(4) 0.082(5) 0.007(4) -0.002(3) 0.004(3) C12 0.056(4) 0.058(4) 0.089(5) 0.007(4) 0.000(4) 0.001(3) C13 0.066(4) 0.049(4) 0.097(6) 0.011(4) -0.011(4) 0.003(3) C13A 0.144(9) 0.092(7) 0.146(9) 0.044(7) -0.024(8) 0.026(7) C14 0.076(5) 0.062(4) 0.099(6) -0.006(4) -0.003(4) 0.009(4) C14A 0.101(6) 0.072(5) 0.123(7) -0.014(5) -0.019(5) -0.007(5) C14B 0.083(5) 0.089(6) 0.124(7) -0.002(5) 0.005(5) 0.026(5) C15 0.058(4) 0.060(4) 0.100(6) 0.013(4) 0.010(4) 0.002(3) C16 0.080(5) 0.098(6) 0.080(5) 0.018(5) 0.006(4) 0.003(4) C17 0.099(7) 0.108(7) 0.144(9) 0.042(7) 0.032(6) 0.039(6) C17A 0.203(15) 0.30(2) 0.230(17) 0.196(19) -0.016(14) 0.023(16) C18 0.117(6) 0.080(5) 0.133(8) 0.016(5) 0.038(6) 0.002(4) C19 0.168(11) 0.214(16) 0.39(2) -0.002(12) 0.109(10) -0.076(11) C20 0.32(2) 0.199(14) 0.307(19) 0.124(13) 0.153(12) 0.045(14) C21 0.135(9) 0.197(8) 0.227(14) 0.028(6) 0.063(8) 0.039(7) C22 0.174(12) 0.29(2) 0.31(2) 0.049(16) 0.133(13) 0.070(12) C23 0.30(2) 0.31(3) 0.54(4) -0.16(2) -0.03(2) -0.03(3) C24 0.24(2) 0.32(2) 0.50(3) 0.29(3) 0.105(18) 0.070(18) _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 Si1 O18 1.606(7) . ? Si1 C21 1.853(3) . ? Si1 C20 1.863(3) . ? Si1 C19 1.865(3) . ? O7A C7 1.301(8) . ? O7A C7A 1.448(10) . ? O7B C7 1.185(8) . ? O8 C8 1.207(8) . ? O10 C10A 1.402(11) . ? O10 C10 1.431(9) . ? O12 C10A 1.382(10) . ? O12 C12 1.438(9) . ? O13 C13A 1.399(11) . ? O13 C13 1.452(8) . ? O15 C11 1.410(8) . ? O15 C15 1.434(8) . ? O17 C17A 1.323(16) . ? O17 C17 1.484(14) . ? O18 C18 1.401(11) . ? N9 C8 1.309(8) . ? N9 C10 1.444(9) . ? C7 C8 1.512(10) . ? C10 C11 1.515(10) . ? C11 C12 1.522(9) . ? C12 C13 1.530(9) . ? C13 C14 1.516(11) . ? C14 C15 1.536(10) . ? C14 C14B 1.543(10) . ? C14 C14A 1.561(11) . ? C15 C16 1.496(11) . ? C16 C17 1.495(13) . ? C17 C18 1.501(14) . ? C21 C22 1.532(3) . ? C21 C23 1.535(3) . ? C21 C24 1.535(3) . ? 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 O18 Si1 C21 110.9(5) . . ? O18 Si1 C20 108.7(7) . . ? C21 Si1 C20 118.1(8) . . ? O18 Si1 C19 118.1(7) . . ? C21 Si1 C19 106.3(8) . . ? C20 Si1 C19 94.3(11) . . ? C7 O7A C7A 118.1(6) . . ? C10A O10 C10 109.5(6) . . ? C10A O12 C12 113.7(6) . . ? C13A O13 C13 115.2(7) . . ? C11 O15 C15 117.1(5) . . ? C17A O17 C17 120.1(13) . . ? C18 O18 Si1 132.2(6) . . ? C8 N9 C10 123.0(5) . . ? O7B C7 O7A 124.1(7) . . ? O7B C7 C8 124.6(6) . . ? O7A C7 C8 111.3(6) . . ? O8 C8 N9 124.7(7) . . ? O8 C8 C7 120.2(6) . . ? N9 C8 C7 115.1(5) . . ? O10 C10 N9 106.6(6) . . ? O10 C10 C11 108.3(5) . . ? N9 C10 C11 111.4(6) . . ? O12 C10A O10 112.8(7) . . ? O15 C11 C10 113.3(5) . . ? O15 C11 C12 110.6(6) . . ? C10 C11 C12 112.0(6) . . ? O12 C12 C11 109.6(5) . . ? O12 C12 C13 112.5(6) . . ? C11 C12 C13 112.6(6) . . ? O13 C13 C14 108.8(6) . . ? O13 C13 C12 108.4(6) . . ? C14 C13 C12 111.1(6) . . ? C13 C14 C15 107.5(6) . . ? C13 C14 C14B 108.0(7) . . ? C15 C14 C14B 109.3(7) . . ? C13 C14 C14A 111.1(7) . . ? C15 C14 C14A 110.3(7) . . ? C14B C14 C14A 110.6(7) . . ? O15 C15 C16 106.1(6) . . ? O15 C15 C14 110.7(6) . . ? C16 C15 C14 115.8(7) . . ? C17 C16 C15 114.7(8) . . ? O17 C17 C16 104.1(10) . . ? O17 C17 C18 112.9(8) . . ? C16 C17 C18 115.5(8) . . ? O18 C18 C17 110.4(8) . . ? C22 C21 C23 111.5(5) . . ? C22 C21 C24 110.3(4) . . ? C23 C21 C24 110.9(5) . . ? C22 C21 Si1 113.1(8) . . ? C23 C21 Si1 105.0(11) . . ? C24 C21 Si1 105.9(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Si1 O18 C18 -164.8(10) . . . . ? C20 Si1 O18 C18 -33.4(14) . . . . ? C19 Si1 O18 C18 72.2(13) . . . . ? C7A O7A C7 O7B 0.3(13) . . . . ? C7A O7A C7 C8 179.5(8) . . . . ? C10 N9 C8 O8 1.1(14) . . . . ? C10 N9 C8 C7 -176.9(7) . . . . ? O7B C7 C8 O8 -179.2(9) . . . . ? O7A C7 C8 O8 1.6(12) . . . . ? O7B C7 C8 N9 -1.2(13) . . . . ? O7A C7 C8 N9 179.6(7) . . . . ? C10A O10 C10 N9 -179.9(6) . . . . ? C10A O10 C10 C11 60.1(7) . . . . ? C8 N9 C10 O10 115.1(8) . . . . ? C8 N9 C10 C11 -126.9(7) . . . . ? C12 O12 C10A O10 59.7(9) . . . . ? C10 O10 C10A O12 -64.9(9) . . . . ? C15 O15 C11 C10 74.0(7) . . . . ? C15 O15 C11 C12 -52.7(7) . . . . ? O10 C10 C11 O15 -178.9(5) . . . . ? N9 C10 C11 O15 64.1(7) . . . . ? O10 C10 C11 C12 -52.9(7) . . . . ? N9 C10 C11 C12 -169.9(6) . . . . ? C10A O12 C12 C11 -49.3(8) . . . . ? C10A O12 C12 C13 76.7(7) . . . . ? O15 C11 C12 O12 174.2(5) . . . . ? C10 C11 C12 O12 46.8(7) . . . . ? O15 C11 C12 C13 48.2(7) . . . . ? C10 C11 C12 C13 -79.3(7) . . . . ? C13A O13 C13 C14 140.7(7) . . . . ? C13A O13 C13 C12 -98.4(8) . . . . ? O12 C12 C13 O13 63.5(7) . . . . ? C11 C12 C13 O13 -172.1(6) . . . . ? O12 C12 C13 C14 -177.0(6) . . . . ? C11 C12 C13 C14 -52.5(8) . . . . ? O13 C13 C14 C15 175.0(6) . . . . ? C12 C13 C14 C15 55.7(8) . . . . ? O13 C13 C14 C14B -67.2(8) . . . . ? C12 C13 C14 C14B 173.5(6) . . . . ? O13 C13 C14 C14A 54.2(8) . . . . ? C12 C13 C14 C14A -65.1(8) . . . . ? C11 O15 C15 C16 -174.8(6) . . . . ? C11 O15 C15 C14 58.8(8) . . . . ? C13 C14 C15 O15 -57.5(8) . . . . ? C14B C14 C15 O15 -174.5(6) . . . . ? C14A C14 C15 O15 63.8(8) . . . . ? C13 C14 C15 C16 -178.3(6) . . . . ? C14B C14 C15 C16 64.7(9) . . . . ? C14A C14 C15 C16 -57.1(9) . . . . ? O15 C15 C16 C17 72.2(8) . . . . ? C14 C15 C16 C17 -164.5(7) . . . . ? C17A O17 C17 C16 148.9(12) . . . . ? C17A O17 C17 C18 -85.2(14) . . . . ? C15 C16 C17 O17 -165.6(7) . . . . ? C15 C16 C17 C18 70.2(10) . . . . ? Si1 O18 C18 C17 126.7(10) . . . . ? O17 C17 C18 O18 -68.2(11) . . . . ? C16 C17 C18 O18 51.4(12) . . . . ? O18 Si1 C21 C22 -177.1(8) . . . . ? C20 Si1 C21 C22 56.6(12) . . . . ? C19 Si1 C21 C22 -47.6(10) . . . . ? O18 Si1 C21 C23 61.2(9) . . . . ? C20 Si1 C21 C23 -65.1(12) . . . . ? C19 Si1 C21 C23 -169.3(10) . . . . ? O18 Si1 C21 C24 -56.3(9) . . . . ? C20 Si1 C21 C24 177.4(12) . . . . ? C19 Si1 C21 C24 73.2(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N9 H9 O8 0.86 2.02 2.830(7) 156.7 2_455 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.664 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.058 data_pk3 _audit_creation_date 1998-09-10T08:40:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H39 N O7 Se' _chemical_formula_structural 'C29 H39 N O7 Se' _chemical_formula_sum 'C29 H39 N O7 Se' _chemical_formula_weight 592.57 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5035(5) _cell_length_b 10.0704(9) _cell_length_c 17.6777(6) _cell_angle_alpha 90 _cell_angle_beta 103.768(3) _cell_angle_gamma 90 _cell_volume 1470.31(17) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.18 _cell_measurement_theta_max 20.09 _cell_measurement_wavelength 0.71073 loop_ _cell_measurement_refln_index_h _cell_measurement_refln_index_k _cell_measurement_refln_index_l _cell_measurement_refln_theta 1 1 -16 18.96 -1 1 16 18.96 -1 6 12 18.71 1 4 -14 18.38 0 4 -9 13.49 6 0 7 18.91 5 1 -7 13.37 -1 4 14 18.38 6 -1 6 18.26 2 6 0 13.18 0 4 9 13.48 4 4 -6 13.51 5 2 1 13.38 2 3 8 13.26 6 1 6 18.26 1 2 -11 13.41 5 0 -7 13.22 2 3 -10 13.28 3 1 8 13.6 5 3 -2 13.53 2 5 -7 13.36 2 2 -11 13.53 5 2 -6 13.41 1 6 -12 18.71 3 0 14 20.09 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_factor_muR 0.183 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 7 Theta correction was applied. Averaged transmission function was used. Fourier smoothing - Window value 4 ; _exptl_absorpt_correction_T_min 0.6815 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_correction_T_ave 0.7745 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 13.78 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.36162E-1 _diffrn_orient_matrix_ub_12 0.7662E-2 _diffrn_orient_matrix_ub_13 -0.57953E-1 _diffrn_orient_matrix_ub_21 -0.10945 _diffrn_orient_matrix_ub_22 0.29504E-1 _diffrn_orient_matrix_ub_23 0.4901E-2 _diffrn_orient_matrix_ub_31 0.37063E-1 _diffrn_orient_matrix_ub_32 0.09457 _diffrn_orient_matrix_ub_33 0.00319 loop_ _diffrn_orient_refln_angle_chi _diffrn_orient_refln_angle_kappa _diffrn_orient_refln_angle_phi _diffrn_orient_refln_angle_psi _diffrn_orient_refln_index_h _diffrn_orient_refln_index_k _diffrn_orient_refln_index_l 5.005 6.534 -102.096 0.001 1 1 -16 6.828 8.915 73.31 0.002 -1 1 16 38.967 51.612 43.363 0 -1 6 12 24.588 32.271 -104.794 0.004 1 4 -14 32.034 42.216 -96.322 0.01 0 4 -9 15.579 20.379 128.404 0.002 6 0 7 23.258 30.507 -167.095 0.006 5 1 -7 25.753 33.819 57.256 0.008 -1 4 14 9.634 12.585 134.877 0.002 6 -1 6 85.616 124.981 96.865 0.643 2 6 0 38.23 50.606 54.835 0.006 0 4 9 50.346 67.445 -169.431 0.058 4 4 -6 35.361 46.707 139.684 0.019 5 2 1 36.369 48.073 84.094 0.011 2 3 8 22.41 29.385 127.456 0.009 6 1 6 16.958 22.191 -106.797 0.008 1 2 -11 14.644 19.151 -165.027 -0.001 5 0 -7 30.173 39.719 -121.771 0.014 2 3 -10 20.444 26.786 105.999 0.007 3 1 8 44.549 59.303 154.806 0.038 5 3 -2 53.573 72.059 -130.939 0.037 2 5 -7 20.199 26.461 -118.814 0.008 2 2 -11 32.918 43.407 -174.943 0.014 5 2 -6 38.71 51.262 -106.43 0.014 1 6 -12 9.314 12.166 101.857 0.003 3 0 14 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.024 _diffrn_standards_decay_corr_min 0.976 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 3 8 -2 4 -3 -4 -1 1 _diffrn_reflns_number 4104 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 3402 _reflns_number_gt 2097 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3402 _refine_ls_number_parameters 332 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(11) _refine_diff_density_max 0.233 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C -1.0681(5) -0.2110(6) -0.1918(2) 0.0478(13) Uani 1 1 d . B . H2 H -1.1175 -0.299 -0.1928 0.057 Uiso 1 1 calc R . . C2A C -1.1671(6) -0.1151(7) -0.1575(3) 0.0688(18) Uani 1 1 d . . . H2A1 H -1.1579 -0.1367 -0.1037 0.083 Uiso 1 1 calc R . . H2A2 H -1.2785 -0.1208 -0.1854 0.083 Uiso 1 1 calc R . . H2A3 H -1.1282 -0.0264 -0.1614 0.083 Uiso 1 1 calc R . . C3 C -0.8910(5) -0.2231(6) -0.1513(2) 0.0489(14) Uani 1 1 d . . . H3 H -0.8838 -0.2498 -0.0973 0.059 Uiso 1 1 calc R . . C3A C -0.7969(6) -0.0941(7) -0.1498(3) 0.0674(16) Uani 1 1 d . . . H3A1 H -0.692 -0.1032 -0.1151 0.081 Uiso 1 1 calc R . . H3A2 H -0.8546 -0.0231 -0.1323 0.081 Uiso 1 1 calc R . . H3A3 H -0.7847 -0.0746 -0.2013 0.081 Uiso 1 1 calc R . . C4 C -0.8211(5) -0.3358(6) -0.1916(2) 0.0464(13) Uani 1 1 d . B . H4 H -0.8753 -0.4181 -0.1824 0.056 Uiso 1 1 calc R . . C4A C -0.6387(5) -0.3587(7) -0.1637(2) 0.0587(17) Uani 1 1 d . . . H4A1 H -0.5813 -0.2764 -0.1667 0.07 Uiso 1 1 calc R A 1 H4A2 H -0.6039 -0.4235 -0.1969 0.07 Uiso 1 1 calc R A 1 C5 C -0.8665(5) -0.3094(6) -0.2789(2) 0.0421(12) Uani 1 1 d . . . H5 H -0.8066 -0.3493 -0.3103 0.051 Uiso 1 1 calc R B . C6 C -0.9891(5) -0.2314(6) -0.3110(2) 0.0431(12) Uani 1 1 d . B . C7 C -1.0395(6) -0.1934(6) -0.3945(2) 0.0476(14) Uani 1 1 d . . . C8 C -0.9614(5) -0.2569(6) -0.4567(2) 0.0400(12) Uani 1 1 d . B . C10 C -0.9320(5) -0.2167(6) -0.5883(2) 0.0422(13) Uani 1 1 d . B . H10 H -0.8307 -0.2667 -0.5721 0.051 Uiso 1 1 calc R . . C10A C -0.9810(6) -0.3185(7) -0.7086(3) 0.0664(17) Uani 1 1 d . B . H10A H -1.0518 -0.379 -0.7437 0.08 Uiso 1 1 calc R . . H10B H -0.8775 -0.3624 -0.6899 0.08 Uiso 1 1 calc R . . C11 C -0.9029(5) -0.0858(6) -0.6262(2) 0.0393(12) Uani 1 1 d . . . H11 H -1.0066 -0.0385 -0.6391 0.047 Uiso 1 1 calc R . . C12 C -0.8524(5) -0.1082(6) -0.7029(2) 0.0453(13) Uani 1 1 d . B . H12 H -0.8701 -0.0237 -0.7312 0.054 Uiso 1 1 calc R . . C13 C -0.6743(5) -0.1410(6) -0.6918(2) 0.0439(12) Uani 1 1 d . . . H13 H -0.6556 -0.2313 -0.671 0.053 Uiso 1 1 calc R . . C13A C -0.6015(8) -0.2590(8) -0.7959(3) 0.100(2) Uani 1 1 d . . . H13A H -0.506 -0.297 -0.7629 0.12 Uiso 1 1 calc R . . H13B H -0.5848 -0.2467 -0.8473 0.12 Uiso 1 1 calc R . . H13C H -0.6917 -0.3176 -0.7984 0.12 Uiso 1 1 calc R . . C14 C -0.5654(5) -0.0446(6) -0.6346(3) 0.0455(13) Uani 1 1 d . . . C14A C -0.3904(5) -0.0941(7) -0.6191(3) 0.0642(16) Uani 1 1 d . . . H14A H -0.3584 -0.1008 -0.6675 0.077 Uiso 1 1 calc R . . H14B H -0.3827 -0.1798 -0.5947 0.077 Uiso 1 1 calc R . . H14C H -0.3205 -0.0328 -0.5854 0.077 Uiso 1 1 calc R . . C14B C -0.5755(5) 0.0969(7) -0.6683(3) 0.0633(14) Uani 1 1 d . . . H14D H -0.5758 0.0928 -0.7225 0.076 Uiso 1 1 calc R . . H14E H -0.4838 0.1475 -0.641 0.076 Uiso 1 1 calc R . . H14F H -0.6733 0.1388 -0.6622 0.076 Uiso 1 1 calc R . . C15 C -0.6255(5) -0.0463(6) -0.5595(2) 0.0468(13) Uani 1 1 d . . . H15 H -0.6198 -0.138 -0.5404 0.056 Uiso 1 1 calc R . . C16 C -0.5360(5) 0.0423(6) -0.4928(3) 0.0618(15) Uani 1 1 d . . . H16A H -0.421 0.0228 -0.4814 0.074 Uiso 1 1 calc R . . H16B H -0.5509 0.1347 -0.5084 0.074 Uiso 1 1 calc R . . C17 C -0.5978(7) 0.0205(8) -0.4206(3) 0.0816(19) Uani 1 1 d . . . H17 H -0.7023 0.0496 -0.4222 0.098 Uiso 1 1 calc R . . C18 C -0.5209(9) -0.0337(8) -0.3580(4) 0.108(3) Uani 1 1 d . . . H18A H -0.4159 -0.0644 -0.3536 0.129 Uiso 1 1 calc R . . H18B H -0.5694 -0.0428 -0.3163 0.129 Uiso 1 1 calc R . . C21A C -0.3654(5) -0.3849(10) -0.0278(5) 0.045(5) Uiso 0.591(18) 1 d PG B 1 C22A C -0.2493(10) -0.4523(9) -0.0565(5) 0.060(4) Uiso 0.591(18) 1 d PG B 1 H22A H -0.2807 -0.5166 -0.0948 0.072 Uiso 0.591(18) 1 calc PR B 1 C23A C -0.0861(8) -0.4234(12) -0.0279(6) 0.057(3) Uiso 0.591(18) 1 d PG B 1 H23A H -0.0083 -0.4685 -0.0471 0.068 Uiso 0.591(18) 1 calc PR B 1 C24A C -0.0390(7) -0.3272(14) 0.0294(5) 0.053(3) Uiso 0.591(18) 1 d PG B 1 H24A H 0.0702 -0.3079 0.0486 0.063 Uiso 0.591(18) 1 calc PR B 1 C25A C -0.1552(13) -0.2599(11) 0.0581(4) 0.068(3) Uiso 0.591(18) 1 d PG B 1 H25A H -0.1237 -0.1955 0.0965 0.082 Uiso 0.591(18) 1 calc PR B 1 C26A C -0.3184(11) -0.2887(9) 0.0295(5) 0.064(3) Uiso 0.591(18) 1 d PG B 1 H26A H -0.3961 -0.2436 0.0487 0.077 Uiso 0.591(18) 1 calc PR B 1 C21B C -0.3585(7) -0.3673(14) -0.0243(7) 0.051(8) Uiso 0.409(18) 1 d PG B 2 C22B C -0.2669(15) -0.2869(11) 0.0336(6) 0.045(4) Uiso 0.409(18) 1 d PG B 2 H22B H -0.318 -0.2292 0.0611 0.054 Uiso 0.409(18) 1 calc PR B 2 C23B C -0.0988(15) -0.2927(13) 0.0504(5) 0.034(3) Uiso 0.409(18) 1 d PG B 2 H23B H -0.0375 -0.2389 0.0891 0.041 Uiso 0.409(18) 1 calc PR B 2 C24B C -0.0223(7) -0.3789(17) 0.0092(7) 0.049(3) Uiso 0.409(18) 1 d PG B 2 H24B H 0.0901 -0.3828 0.0204 0.059 Uiso 0.409(18) 1 calc PR B 2 C25B C -0.1139(14) -0.4594(15) -0.0488(7) 0.067(5) Uiso 0.409(18) 1 d PG B 2 H25B H -0.0628 -0.5171 -0.0763 0.08 Uiso 0.409(18) 1 calc PR B 2 C26B C -0.2820(13) -0.4536(13) -0.0655(7) 0.065(6) Uiso 0.409(18) 1 d PG B 2 H26B H -0.3433 -0.5074 -0.1043 0.078 Uiso 0.409(18) 1 calc PR B 2 N9 N -0.9987(5) -0.1904(6) -0.5230(2) 0.0437(11) Uani 1 1 d . . . H9 H -1.056(5) -0.123(5) -0.526(3) 0.045(17) Uiso 1 1 d . . . O1 O -1.0863(4) -0.1674(5) -0.27160(16) 0.0500(9) Uani 1 1 d . . . O2 O -1.1448(5) -0.1131(5) -0.41680(19) 0.0751(14) Uani 1 1 d . B . O3 O -0.8773(4) -0.3561(5) -0.44532(16) 0.0657(12) Uani 1 1 d . . . O4 O -1.0482(3) -0.2903(5) -0.64518(15) 0.0553(9) Uani 1 1 d . . . O5 O -0.9583(4) -0.2028(5) -0.74989(16) 0.0598(10) Uani 1 1 d . . . O6 O -0.7922(3) -0.0038(4) -0.57488(16) 0.0441(8) Uani 1 1 d . . . O7 O -0.6335(4) -0.1366(5) -0.76579(18) 0.0615(10) Uani 1 1 d . . . Se1A Se -0.5884(10) -0.4223(5) -0.0569(5) 0.0786(16) Uani 0.591(18) 1 d P B 1 Se1B Se -0.5878(14) -0.3743(13) -0.0464(5) 0.081(2) Uani 0.409(18) 1 d P B 2 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 C2 0.057(3) 0.054(4) 0.034(2) 0.008(2) 0.013(2) 0.002(3) C2A 0.075(4) 0.084(5) 0.049(3) 0.006(3) 0.020(3) 0.020(4) C3 0.060(3) 0.052(4) 0.033(2) -0.002(2) 0.008(2) -0.005(3) C3A 0.081(4) 0.062(4) 0.056(3) -0.007(3) 0.009(3) -0.009(4) C4 0.048(3) 0.051(4) 0.036(2) 0.004(2) 0.0018(19) -0.001(3) C4A 0.054(3) 0.084(5) 0.035(2) 0.010(3) 0.0047(19) 0.008(3) C5 0.043(2) 0.047(3) 0.033(2) -0.004(2) 0.0027(19) -0.001(3) C6 0.046(3) 0.050(3) 0.032(2) -0.004(2) 0.007(2) -0.002(3) C7 0.046(3) 0.057(4) 0.038(3) 0.001(3) 0.007(2) 0.009(3) C8 0.034(2) 0.049(4) 0.035(2) -0.001(3) 0.004(2) 0.000(3) C10 0.038(3) 0.056(4) 0.034(2) 0.002(3) 0.010(2) 0.003(3) C10A 0.080(4) 0.076(5) 0.046(3) -0.024(3) 0.020(3) -0.025(3) C11 0.038(3) 0.036(3) 0.040(3) 0.003(2) 0.002(2) 0.004(2) C12 0.048(3) 0.049(4) 0.038(2) 0.007(3) 0.008(2) 0.001(3) C13 0.051(3) 0.045(3) 0.041(2) 0.007(2) 0.019(2) 0.008(3) C13A 0.158(6) 0.087(6) 0.073(4) 0.001(4) 0.062(4) 0.025(5) C14 0.043(3) 0.041(3) 0.053(3) 0.007(3) 0.012(2) 0.002(3) C14A 0.043(3) 0.056(4) 0.091(4) 0.000(3) 0.011(3) 0.000(3) C14B 0.062(3) 0.054(4) 0.078(3) 0.020(4) 0.025(2) -0.002(4) C15 0.045(3) 0.042(3) 0.050(3) 0.000(2) 0.005(2) -0.001(3) C16 0.062(3) 0.052(4) 0.063(3) -0.015(3) -0.003(3) -0.011(3) C17 0.086(4) 0.084(5) 0.065(4) -0.028(4) -0.002(3) -0.016(4) C18 0.135(6) 0.103(7) 0.076(4) -0.010(5) 0.007(4) -0.005(5) N9 0.046(2) 0.052(3) 0.034(2) 0.008(2) 0.0124(18) 0.012(2) O1 0.056(2) 0.061(2) 0.0336(16) 0.0012(18) 0.0125(15) 0.010(2) O2 0.081(3) 0.107(4) 0.0432(19) 0.019(2) 0.0260(19) 0.051(3) O3 0.080(2) 0.072(3) 0.0492(17) 0.012(2) 0.0229(16) 0.032(2) O4 0.0542(18) 0.069(3) 0.0449(17) -0.0111(19) 0.0156(15) -0.0197(19) O5 0.061(2) 0.084(3) 0.0299(16) -0.012(2) 0.0030(15) -0.016(2) O6 0.0384(16) 0.045(2) 0.0467(17) -0.0085(17) 0.0056(14) 0.0002(17) O7 0.076(2) 0.066(3) 0.0520(19) 0.009(2) 0.0332(18) 0.004(2) Se1A 0.0591(15) 0.108(3) 0.060(2) 0.0385(19) -0.0022(16) -0.009(2) Se1B 0.060(2) 0.144(7) 0.0367(12) 0.015(3) 0.0067(12) 0.022(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 O1 1.450(5) . ? C2 C2A 1.501(7) . ? C2 C3 1.510(6) . ? C3 C3A 1.523(7) . ? C3 C4 1.534(6) . ? C4 C5 1.522(5) . ? C4 C4A 1.529(5) . ? C4A Se1A 1.942(8) . ? C4A Se1B 2.020(10) . ? C5 C6 1.321(6) . ? C6 O1 1.364(5) . ? C6 C7 1.485(6) . ? C7 O2 1.200(5) . ? C7 C8 1.551(6) . ? C8 O3 1.217(6) . ? C8 N9 1.323(6) . ? C10 N9 1.427(5) . ? C10 O4 1.436(5) . ? C10 C11 1.525(7) . ? C10A O4 1.403(5) . ? C10A O5 1.412(6) . ? C11 O6 1.409(5) . ? C11 C12 1.533(6) . ? C12 O5 1.433(5) . ? C12 C13 1.516(6) . ? C13 O7 1.431(5) . ? C13 C14 1.542(6) . ? C13A O7 1.395(7) . ? C14 C15 1.532(6) . ? C14 C14A 1.531(6) . ? C14 C14B 1.539(7) . ? C15 O6 1.444(5) . ? C15 C16 1.530(6) . ? C16 C17 1.506(7) . ? C17 C18 1.268(8) . ? C21A C22A 1.39 . ? C21A C26A 1.39 . ? C21A Se1A 1.881(9) . ? C22A C23A 1.39 . ? C23A C24A 1.39 . ? C24A C25A 1.39 . ? C25A C26A 1.39 . ? C21B C22B 1.39 . ? C21B C26B 1.39 . ? C21B Se1B 1.897(13) . ? C22B C23B 1.39 . ? C23B C24B 1.39 . ? C24B C25B 1.39 . ? C25B C26B 1.39 . ? 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 C2 C2A 105.0(4) . . ? O1 C2 C3 110.4(3) . . ? C2A C2 C3 116.9(4) . . ? C2 C3 C3A 113.6(4) . . ? C2 C3 C4 107.0(4) . . ? C3A C3 C4 112.3(4) . . ? C5 C4 C4A 110.3(3) . . ? C5 C4 C3 108.0(4) . . ? C4A C4 C3 115.9(4) . . ? C4 C4A Se1A 109.6(4) . . ? C4 C4A Se1B 107.2(4) . . ? Se1A C4A Se1B 14.8(4) . . ? C6 C5 C4 121.6(4) . . ? C5 C6 O1 125.0(4) . . ? C5 C6 C7 126.3(4) . . ? O1 C6 C7 108.6(4) . . ? O2 C7 C6 121.1(4) . . ? O2 C7 C8 117.2(4) . . ? C6 C7 C8 121.7(5) . . ? O3 C8 N9 124.7(4) . . ? O3 C8 C7 123.8(4) . . ? N9 C8 C7 111.5(5) . . ? N9 C10 O4 108.8(4) . . ? N9 C10 C11 109.4(4) . . ? O4 C10 C11 107.1(3) . . ? O4 C10A O5 112.2(5) . . ? O6 C11 C10 112.1(3) . . ? O6 C11 C12 111.7(4) . . ? C10 C11 C12 111.8(4) . . ? O5 C12 C13 113.6(4) . . ? O5 C12 C11 109.9(4) . . ? C13 C12 C11 113.5(3) . . ? O7 C13 C12 109.1(3) . . ? O7 C13 C14 110.0(4) . . ? C12 C13 C14 111.9(4) . . ? C15 C14 C14A 110.5(4) . . ? C15 C14 C13 106.8(4) . . ? C14A C14 C13 108.6(4) . . ? C15 C14 C14B 110.3(4) . . ? C14A C14 C14B 109.5(4) . . ? C13 C14 C14B 111.1(4) . . ? O6 C15 C16 105.0(4) . . ? O6 C15 C14 110.3(3) . . ? C16 C15 C14 117.0(4) . . ? C17 C16 C15 111.0(4) . . ? C18 C17 C16 126.2(6) . . ? C22A C21A C26A 120 . . ? C22A C21A Se1A 124.1(5) . . ? C26A C21A Se1A 115.8(5) . . ? C23A C22A C21A 120 . . ? C24A C23A C22A 120 . . ? C23A C24A C25A 120 . . ? C26A C25A C24A 120 . . ? C25A C26A C21A 120 . . ? C22B C21B C26B 120 . . ? C22B C21B Se1B 122.8(7) . . ? C26B C21B Se1B 117.1(7) . . ? C23B C22B C21B 120 . . ? C22B C23B C24B 120 . . ? C23B C24B C25B 120 . . ? C24B C25B C26B 120 . . ? C25B C26B C21B 120 . . ? C8 N9 C10 124.5(5) . . ? C6 O1 C2 114.7(4) . . ? C10A O4 C10 108.7(3) . . ? C10A O5 C12 113.2(3) . . ? C11 O6 C15 115.0(3) . . ? C13A O7 C13 115.7(4) . . ? C21A Se1A C4A 100.1(5) . . ? C21B Se1B C4A 99.6(6) . . ?