# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global #=============================================================================== _journal_coden_Cambridge 182 loop_ _publ_author_name 'Nief, Francois' 'Ricard, Louis' 'Turcitu, Daniela' _publ_contact_author_name 'Dr Francois Nief' _publ_contact_author_address ; DCPH Laboratoire Hétéroéléments et Coordination, UMR 7653 Ecole Polytechnique Palaisau 91128 FRANCE ; _publ_contact_author_phone '01-69-33-45-72' _publ_contact_author_fax '01-69-33-39-90' _publ_contact_author_email louis.ricard@polytechnique.fr _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_section_title ; Synthesis and Structure of Phospholyl- and Arsolylthulium(II) Complexes. ; #=============================================================================== _publ_section_exptl_prep ; All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gšttingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; #=============================================================================== data_tmas _database_code_CSD 185425 _audit_creation_date 05-03-02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 As2 O Si4 Tm' _chemical_formula_weight 839.86 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tm' 'Tm' -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.659(5) _cell_length_b 17.230(5) _cell_length_c 20.156(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 94.300(5) _cell_angle_gamma 90.000(5) _cell_volume 3691(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'deep green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 4.331 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5094 _exptl_absorpt_correction_T_max 0.6713 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17595 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10768 _reflns_number_gt 8056 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+11.8930P] 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_number_reflns 10768 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.903793(19) 0.230672(11) 0.155229(11) 0.02764(7) Uani 1 1 d . . . As1 As 0.66616(4) 0.31818(3) 0.16550(3) 0.02860(11) Uani 1 1 d . . . As2 As 0.99432(4) 0.08701(3) 0.09220(3) 0.02683(11) Uani 1 1 d . . . Si1 Si 0.75348(14) 0.41681(8) 0.03926(8) 0.0334(3) Uani 1 1 d . . . Si2 Si 0.71444(14) 0.29033(8) 0.32494(7) 0.0326(3) Uani 1 1 d . . . Si3 Si 0.73585(13) 0.10310(8) -0.00392(7) 0.0321(3) Uani 1 1 d . . . Si4 Si 1.11390(15) 0.06175(10) 0.24548(9) 0.0424(4) Uani 1 1 d . . . O1 O 1.1046(4) 0.2757(2) 0.1233(3) 0.0507(12) Uani 1 1 d . . . C1 C 0.7899(4) 0.3754(3) 0.1238(2) 0.0270(9) Uani 1 1 d . . . C2 C 0.8935(4) 0.3920(3) 0.1691(2) 0.0271(9) Uani 1 1 d . . . C3 C 0.8868(4) 0.3603(3) 0.2343(2) 0.0267(9) Uani 1 1 d . . . C4 C 0.7759(4) 0.3178(3) 0.2441(2) 0.0277(10) Uani 1 1 d . . . C5 C 0.8551(6) 0.3750(5) -0.0236(3) 0.0604(19) Uani 1 1 d . . . H5A H 0.8273 0.3946 -0.0679 0.091 Uiso 1 1 calc R . . H5B H 0.8485 0.3182 -0.0232 0.091 Uiso 1 1 calc R . . H5C H 0.9428 0.3902 -0.0125 0.091 Uiso 1 1 calc R . . C6 C 0.5842(5) 0.3977(4) 0.0121(3) 0.0478(14) Uani 1 1 d . . . H6A H 0.5303 0.4222 0.0434 0.072 Uiso 1 1 calc R . . H6B H 0.5689 0.3416 0.0111 0.072 Uiso 1 1 calc R . . H6C H 0.5648 0.4193 -0.0325 0.072 Uiso 1 1 calc R . . C7 C 0.7726(7) 0.5244(4) 0.0396(4) 0.064(2) Uani 1 1 d . . . H7A H 0.7267 0.5468 0.0754 0.096 Uiso 1 1 calc R . . H7B H 0.7391 0.5456 -0.0032 0.096 Uiso 1 1 calc R . . H7C H 0.8621 0.5375 0.0469 0.096 Uiso 1 1 calc R . . C8 C 1.0001(5) 0.4446(3) 0.1526(3) 0.0368(12) Uani 1 1 d . . . H8A H 1.0063 0.4452 0.1044 0.055 Uiso 1 1 calc R . . H8B H 1.0791 0.4253 0.1747 0.055 Uiso 1 1 calc R . . H8C H 0.9840 0.4973 0.1682 0.055 Uiso 1 1 calc R . . C9 C 0.9878(5) 0.3760(3) 0.2898(3) 0.0359(11) Uani 1 1 d . . . H9A H 1.0684 0.3555 0.2773 0.054 Uiso 1 1 calc R . . H9B H 0.9650 0.3506 0.3307 0.054 Uiso 1 1 calc R . . H9C H 0.9952 0.4321 0.2973 0.054 Uiso 1 1 calc R . . C10 C 0.5595(6) 0.2400(4) 0.3092(3) 0.0441(14) Uani 1 1 d . . . H10A H 0.5282 0.2245 0.3518 0.066 Uiso 1 1 calc R . . H10B H 0.5702 0.1939 0.2818 0.066 Uiso 1 1 calc R . . H10C H 0.4991 0.2753 0.2859 0.066 Uiso 1 1 calc R . . C11 C 0.6915(6) 0.3803(3) 0.3737(3) 0.0477(15) Uani 1 1 d . . . H11A H 0.7710 0.4091 0.3791 0.072 Uiso 1 1 calc R . . H11B H 0.6643 0.3665 0.4175 0.072 Uiso 1 1 calc R . . H11C H 0.6272 0.4128 0.3500 0.072 Uiso 1 1 calc R . . C12 C 0.8224(7) 0.2253(3) 0.3772(3) 0.0507(15) Uani 1 1 d . . . H12A H 0.8862 0.2567 0.4023 0.076 Uiso 1 1 calc R . . H12B H 0.8638 0.1890 0.3484 0.076 Uiso 1 1 calc R . . H12C H 0.7738 0.1961 0.4081 0.076 Uiso 1 1 calc R . . C13 C 0.8178(4) 0.1024(2) 0.0805(2) 0.0267(9) Uani 1 1 d . . . C14 C 0.7629(4) 0.0941(2) 0.1425(3) 0.0274(10) Uani 1 1 d . . . C15 C 0.8475(5) 0.0809(2) 0.1983(2) 0.0286(10) Uani 1 1 d . . . C16 C 0.9762(5) 0.0790(3) 0.1856(3) 0.0300(10) Uani 1 1 d . . . C17 C 0.6731(5) 0.0036(3) -0.0237(3) 0.0422(13) Uani 1 1 d . . . H17A H 0.7432 -0.0330 -0.0249 0.063 Uiso 1 1 calc R . . H17B H 0.6251 0.0043 -0.0672 0.063 Uiso 1 1 calc R . . H17C H 0.6180 -0.0125 0.0105 0.063 Uiso 1 1 calc R . . C18 C 0.8504(6) 0.1286(4) -0.0665(3) 0.0458(14) Uani 1 1 d . . . H18A H 0.8842 0.1807 -0.0571 0.069 Uiso 1 1 calc R . . H18B H 0.8075 0.1276 -0.1112 0.069 Uiso 1 1 calc R . . H18C H 0.9194 0.0909 -0.0639 0.069 Uiso 1 1 calc R . . C19 C 0.6020(6) 0.1740(4) -0.0126(3) 0.0549(17) Uani 1 1 d . . . H19A H 0.5248 0.1486 -0.0002 0.082 Uiso 1 1 calc R . . H19B H 0.5904 0.1918 -0.0589 0.082 Uiso 1 1 calc R . . H19C H 0.6208 0.2185 0.0167 0.082 Uiso 1 1 calc R . . C20 C 0.6220(5) 0.0914(3) 0.1472(3) 0.0372(12) Uani 1 1 d . . . H20A H 0.5939 0.0372 0.1467 0.056 Uiso 1 1 calc R . . H20B H 0.5799 0.1190 0.1093 0.056 Uiso 1 1 calc R . . H20C H 0.6008 0.1161 0.1887 0.056 Uiso 1 1 calc R . . C21 C 0.8020(6) 0.0594(3) 0.2651(3) 0.0414(13) Uani 1 1 d . . . H21A H 0.7718 0.0056 0.2637 0.062 Uiso 1 1 calc R . . H21B H 0.7332 0.0941 0.2754 0.062 Uiso 1 1 calc R . . H21C H 0.8714 0.0644 0.2996 0.062 Uiso 1 1 calc R . . C22 C 1.1315(7) 0.1414(6) 0.3103(4) 0.075(2) Uani 1 1 d . . . H22A H 1.1029 0.1907 0.2903 0.112 Uiso 1 1 calc R . . H22B H 1.2200 0.1458 0.3268 0.112 Uiso 1 1 calc R . . H22C H 1.0806 0.1288 0.3473 0.112 Uiso 1 1 calc R . . C23 C 1.1027(8) -0.0327(5) 0.2899(6) 0.106(4) Uani 1 1 d . . . H23A H 1.0227 -0.0352 0.3108 0.160 Uiso 1 1 calc R . . H23B H 1.1725 -0.0371 0.3243 0.160 Uiso 1 1 calc R . . H23C H 1.1071 -0.0755 0.2581 0.160 Uiso 1 1 calc R . . C24 C 1.2622(5) 0.0574(4) 0.2018(3) 0.0476(14) Uani 1 1 d . . . H24A H 1.2647 0.0087 0.1768 0.071 Uiso 1 1 calc R . . H24B H 1.3348 0.0599 0.2346 0.071 Uiso 1 1 calc R . . H24C H 1.2649 0.1013 0.1711 0.071 Uiso 1 1 calc R . . C25 C 1.2183(7) 0.2731(4) 0.1685(4) 0.0589(18) Uani 1 1 d . . . H25A H 1.2173 0.2269 0.1977 0.071 Uiso 1 1 calc R . . H25B H 1.2246 0.3202 0.1967 0.071 Uiso 1 1 calc R . . C26 C 1.3250(6) 0.2690(4) 0.1259(4) 0.064(2) Uani 1 1 d . . . H26A H 1.3615 0.3211 0.1197 0.077 Uiso 1 1 calc R . . H26B H 1.3915 0.2340 0.1455 0.077 Uiso 1 1 calc R . . C27 C 1.2694(7) 0.2380(4) 0.0623(4) 0.0603(19) Uani 1 1 d . . . H27A H 1.2646 0.1806 0.0634 0.072 Uiso 1 1 calc R . . H27B H 1.3189 0.2539 0.0249 0.072 Uiso 1 1 calc R . . C28 C 1.1412(6) 0.2731(4) 0.0558(4) 0.0598(19) Uani 1 1 d . . . H28A H 1.1435 0.3259 0.0366 0.072 Uiso 1 1 calc R . . H28B H 1.0823 0.2407 0.0274 0.072 Uiso 1 1 calc R . . 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 Tm1 0.02336(11) 0.02174(10) 0.03897(13) -0.00736(8) 0.00999(9) -0.00318(7) As1 0.0218(2) 0.0311(2) 0.0332(3) -0.0038(2) 0.00432(19) -0.00293(18) As2 0.0223(2) 0.0245(2) 0.0339(3) -0.00490(19) 0.00364(19) 0.00366(17) Si1 0.0337(7) 0.0326(7) 0.0337(8) 0.0029(6) 0.0021(6) 0.0029(6) Si2 0.0395(8) 0.0287(6) 0.0309(7) -0.0051(5) 0.0103(6) -0.0031(6) Si3 0.0302(7) 0.0312(7) 0.0342(8) -0.0070(6) -0.0026(6) 0.0030(5) Si4 0.0346(8) 0.0479(9) 0.0435(9) 0.0162(7) -0.0051(7) 0.0014(7) O1 0.028(2) 0.038(2) 0.089(3) -0.016(2) 0.023(2) -0.0092(16) C1 0.028(2) 0.024(2) 0.029(2) -0.0020(18) 0.0024(19) -0.0029(18) C2 0.026(2) 0.0215(19) 0.034(3) -0.0040(18) 0.0046(19) -0.0015(17) C3 0.029(2) 0.0221(19) 0.028(2) -0.0087(18) 0.0005(19) -0.0009(17) C4 0.028(2) 0.024(2) 0.031(3) -0.0062(18) 0.0067(19) 0.0004(17) C5 0.049(4) 0.091(5) 0.040(4) -0.006(4) 0.001(3) 0.014(4) C6 0.039(3) 0.045(3) 0.058(4) 0.005(3) -0.006(3) 0.010(3) C7 0.071(5) 0.038(3) 0.082(5) 0.019(3) -0.004(4) -0.008(3) C8 0.033(3) 0.031(2) 0.047(3) 0.000(2) 0.003(2) -0.008(2) C9 0.032(3) 0.039(3) 0.036(3) -0.006(2) -0.003(2) -0.003(2) C10 0.043(3) 0.050(3) 0.040(3) -0.005(3) 0.014(3) -0.006(3) C11 0.066(4) 0.038(3) 0.042(3) -0.010(2) 0.023(3) -0.001(3) C12 0.069(4) 0.036(3) 0.046(4) 0.001(3) -0.006(3) -0.003(3) C13 0.025(2) 0.0207(19) 0.034(3) -0.0051(18) 0.0031(19) 0.0001(17) C14 0.020(2) 0.0168(18) 0.045(3) -0.0051(18) 0.0047(19) -0.0040(16) C15 0.035(3) 0.0197(19) 0.030(3) -0.0027(17) -0.002(2) -0.0042(18) C16 0.030(2) 0.027(2) 0.033(3) -0.0038(19) 0.000(2) 0.0038(19) C17 0.038(3) 0.043(3) 0.044(3) -0.016(3) 0.001(2) -0.007(2) C18 0.057(4) 0.046(3) 0.035(3) 0.000(2) 0.007(3) -0.005(3) C19 0.051(4) 0.056(4) 0.054(4) -0.015(3) -0.018(3) 0.020(3) C20 0.027(2) 0.031(2) 0.054(4) -0.007(2) 0.010(2) -0.007(2) C21 0.046(3) 0.042(3) 0.038(3) 0.001(2) 0.011(2) -0.004(2) C22 0.060(5) 0.123(7) 0.040(4) -0.003(4) -0.003(3) -0.009(5) C23 0.055(5) 0.091(6) 0.171(11) 0.092(7) -0.009(5) 0.006(4) C24 0.034(3) 0.049(3) 0.059(4) 0.002(3) -0.008(3) 0.010(3) C25 0.052(4) 0.054(4) 0.071(5) -0.013(3) 0.009(4) -0.011(3) C26 0.028(3) 0.069(5) 0.096(6) -0.009(4) 0.011(3) -0.007(3) C27 0.051(4) 0.070(5) 0.063(5) 0.001(4) 0.027(4) -0.002(3) C28 0.047(4) 0.054(4) 0.079(5) 0.025(4) 0.004(4) -0.004(3) _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 Tm1 O1 2.410(4) . ? Tm1 C3 2.759(4) . ? Tm1 C4 2.772(4) . ? Tm1 C16 2.780(5) . ? Tm1 C13 2.791(4) . ? Tm1 C14 2.792(4) . ? Tm1 C2 2.796(4) . ? Tm1 C15 2.801(4) . ? Tm1 C1 2.824(5) . ? Tm1 As1 2.9683(12) . ? Tm1 As2 2.9759(8) . ? As1 C1 1.893(5) . ? As1 C4 1.897(5) . ? As2 C13 1.897(5) . ? As2 C16 1.912(5) . ? Si1 C1 1.861(5) . ? Si1 C7 1.866(6) . ? Si1 C5 1.872(6) . ? Si1 C6 1.875(6) . ? Si2 C11 1.861(5) . ? Si2 C4 1.863(5) . ? Si2 C10 1.871(6) . ? Si2 C12 1.873(6) . ? Si3 C13 1.854(5) . ? Si3 C17 1.872(5) . ? Si3 C18 1.872(6) . ? Si3 C19 1.876(6) . ? Si4 C16 1.852(5) . ? Si4 C23 1.866(7) . ? Si4 C24 1.868(6) . ? Si4 C22 1.894(9) . ? O1 C28 1.443(9) . ? O1 C25 1.461(9) . ? C1 C2 1.408(7) . ? C2 C3 1.430(7) . ? C2 C8 1.509(6) . ? C3 C4 1.417(6) . ? C3 C9 1.517(7) . ? C13 C14 1.425(7) . ? C14 C15 1.407(7) . ? C14 C20 1.513(6) . ? C15 C16 1.415(7) . ? C15 C21 1.512(7) . ? C25 C26 1.478(10) . ? C26 C27 1.472(11) . ? C27 C28 1.491(10) . ? 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 Tm1 C3 89.55(14) . . ? O1 Tm1 C4 119.23(14) . . ? C3 Tm1 C4 29.69(13) . . ? O1 Tm1 C16 97.11(14) . . ? C3 Tm1 C16 131.52(15) . . ? C4 Tm1 C16 120.55(14) . . ? O1 Tm1 C13 111.92(14) . . ? C3 Tm1 C13 156.96(13) . . ? C4 Tm1 C13 128.31(13) . . ? C16 Tm1 C13 56.57(14) . . ? O1 Tm1 C14 136.80(13) . . ? C3 Tm1 C14 132.63(14) . . ? C4 Tm1 C14 103.21(14) . . ? C16 Tm1 C14 50.73(14) . . ? C13 Tm1 C14 29.58(14) . . ? O1 Tm1 C2 75.46(13) . . ? C3 Tm1 C2 29.84(14) . . ? C4 Tm1 C2 51.14(13) . . ? C16 Tm1 C2 157.59(15) . . ? C13 Tm1 C2 145.84(14) . . ? C14 Tm1 C2 145.26(13) . . ? O1 Tm1 C15 126.47(14) . . ? C3 Tm1 C15 122.81(14) . . ? C4 Tm1 C15 99.86(14) . . ? C16 Tm1 C15 29.36(14) . . ? C13 Tm1 C15 50.83(14) . . ? C14 Tm1 C15 29.13(14) . . ? C2 Tm1 C15 150.87(14) . . ? O1 Tm1 C1 91.80(14) . . ? C3 Tm1 C1 50.86(14) . . ? C4 Tm1 C1 56.15(14) . . ? C16 Tm1 C1 170.70(14) . . ? C13 Tm1 C1 117.40(14) . . ? C14 Tm1 C1 120.27(14) . . ? C2 Tm1 C1 29.01(13) . . ? C15 Tm1 C1 141.65(14) . . ? O1 Tm1 As1 129.42(10) . . ? C3 Tm1 As1 56.96(10) . . ? C4 Tm1 As1 38.41(11) . . ? C16 Tm1 As1 133.35(10) . . ? C13 Tm1 As1 101.10(10) . . ? C14 Tm1 As1 88.77(10) . . ? C2 Tm1 As1 56.50(9) . . ? C15 Tm1 As1 104.04(10) . . ? C1 Tm1 As1 38.05(9) . . ? O1 Tm1 As2 80.25(9) . . ? C3 Tm1 As2 163.31(10) . . ? C4 Tm1 As2 156.49(10) . . ? C16 Tm1 As2 38.62(11) . . ? C13 Tm1 As2 38.25(9) . . ? C14 Tm1 As2 56.58(9) . . ? C2 Tm1 As2 152.35(10) . . ? C15 Tm1 As2 56.63(10) . . ? C1 Tm1 As2 141.84(10) . . ? As1 Tm1 As2 139.288(16) . . ? C1 As1 C4 88.0(2) . . ? C1 As1 Tm1 66.85(14) . . ? C4 As1 Tm1 65.18(13) . . ? C13 As2 C16 87.7(2) . . ? C13 As2 Tm1 65.59(13) . . ? C16 As2 Tm1 65.13(14) . . ? C1 Si1 C7 111.2(3) . . ? C1 Si1 C5 112.4(3) . . ? C7 Si1 C5 108.5(4) . . ? C1 Si1 C6 109.3(3) . . ? C7 Si1 C6 106.1(3) . . ? C5 Si1 C6 109.1(3) . . ? C11 Si2 C4 108.6(2) . . ? C11 Si2 C10 109.0(3) . . ? C4 Si2 C10 109.5(3) . . ? C11 Si2 C12 107.5(3) . . ? C4 Si2 C12 113.7(3) . . ? C10 Si2 C12 108.4(3) . . ? C13 Si3 C17 109.0(2) . . ? C13 Si3 C18 109.5(3) . . ? C17 Si3 C18 108.2(3) . . ? C13 Si3 C19 113.1(3) . . ? C17 Si3 C19 108.6(3) . . ? C18 Si3 C19 108.3(3) . . ? C16 Si4 C23 112.1(3) . . ? C16 Si4 C24 110.9(3) . . ? C23 Si4 C24 106.1(4) . . ? C16 Si4 C22 111.4(3) . . ? C23 Si4 C22 107.9(5) . . ? C24 Si4 C22 108.1(3) . . ? C28 O1 C25 108.5(5) . . ? C28 O1 Tm1 123.4(4) . . ? C25 O1 Tm1 122.3(4) . . ? C2 C1 Si1 128.0(4) . . ? C2 C1 As1 110.9(3) . . ? Si1 C1 As1 120.1(3) . . ? C2 C1 Tm1 74.4(3) . . ? Si1 C1 Tm1 126.9(2) . . ? As1 C1 Tm1 75.10(15) . . ? C1 C2 C3 115.3(4) . . ? C1 C2 C8 123.1(5) . . ? C3 C2 C8 121.4(4) . . ? C1 C2 Tm1 76.6(3) . . ? C3 C2 Tm1 73.6(2) . . ? C8 C2 Tm1 122.6(3) . . ? C4 C3 C2 115.1(4) . . ? C4 C3 C9 122.9(4) . . ? C2 C3 C9 121.9(4) . . ? C4 C3 Tm1 75.7(2) . . ? C2 C3 Tm1 76.5(2) . . ? C9 C3 Tm1 119.8(3) . . ? C3 C4 Si2 127.2(4) . . ? C3 C4 As1 110.5(4) . . ? Si2 C4 As1 119.7(3) . . ? C3 C4 Tm1 74.7(2) . . ? Si2 C4 Tm1 130.6(2) . . ? As1 C4 Tm1 76.41(15) . . ? C14 C13 Si3 127.5(4) . . ? C14 C13 As2 110.2(4) . . ? Si3 C13 As2 120.6(2) . . ? C14 C13 Tm1 75.3(2) . . ? Si3 C13 Tm1 127.1(2) . . ? As2 C13 Tm1 76.16(15) . . ? C15 C14 C13 115.9(4) . . ? C15 C14 C20 121.6(5) . . ? C13 C14 C20 122.2(5) . . ? C15 C14 Tm1 75.8(2) . . ? C13 C14 Tm1 75.2(2) . . ? C20 C14 Tm1 123.4(3) . . ? C14 C15 C16 115.6(4) . . ? C14 C15 C21 121.5(5) . . ? C16 C15 C21 122.4(5) . . ? C14 C15 Tm1 75.1(2) . . ? C16 C15 Tm1 74.5(3) . . ? C21 C15 Tm1 126.4(3) . . ? C15 C16 Si4 128.2(4) . . ? C15 C16 As2 110.3(4) . . ? Si4 C16 As2 121.3(3) . . ? C15 C16 Tm1 76.2(3) . . ? Si4 C16 Tm1 119.2(2) . . ? As2 C16 Tm1 76.24(16) . . ? O1 C25 C26 106.1(6) . . ? C27 C26 C25 104.3(6) . . ? C26 C27 C28 103.6(6) . . ? O1 C28 C27 104.0(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 6.555 _refine_diff_density_min -4.126 _refine_diff_density_rms 0.162 #=============================================================================== data_tmtbu _database_code_CSD 185426 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 O P2 Tm' _chemical_formula_weight 687.64 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tm' 'Tm' -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I41/a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 23.589(5) _cell_length_b 23.589(5) _cell_length_c 23.060(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 12832(5) _cell_formula_units_Z 16 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5680 _exptl_absorpt_coefficient_mu 2.887 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5959 _exptl_absorpt_correction_T_max 0.5959 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15144 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 30.02 _reflns_number_total 9370 _reflns_number_gt 7089 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] 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_number_reflns 9370 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.503527(5) 0.025307(5) 0.719177(6) 0.01986(6) Uani 1 1 d . . . P1 P 0.62359(3) 0.05885(3) 0.72411(4) 0.02283(17) Uani 1 1 d . . . P2 P 0.39685(3) -0.03130(3) 0.75513(4) 0.02523(18) Uani 1 1 d . . . O1 O 0.52375(9) 0.00180(9) 0.82079(10) 0.0283(5) Uani 1 1 d . . . C1 C 0.57679(12) 0.11767(12) 0.72852(13) 0.0218(6) Uani 1 1 d . . . C2 C 0.54926(12) 0.12654(12) 0.67495(14) 0.0220(6) Uani 1 1 d . . . C3 C 0.56488(13) 0.08661(12) 0.63111(13) 0.0233(6) Uani 1 1 d . . . C4 C 0.60477(13) 0.04597(12) 0.65113(14) 0.0245(6) Uani 1 1 d . . . C5 C 0.57448(13) 0.15601(13) 0.78223(13) 0.0234(6) Uani 1 1 d . . . C6 C 0.60971(15) 0.13126(15) 0.83197(15) 0.0355(8) Uani 1 1 d . . . H6A H 0.5946 0.0940 0.8426 0.053 Uiso 1 1 calc R . . H6B H 0.6078 0.1567 0.8655 0.053 Uiso 1 1 calc R . . H6C H 0.6492 0.1273 0.8195 0.053 Uiso 1 1 calc R . . C7 C 0.51387(13) 0.16309(14) 0.80577(16) 0.0311(7) Uani 1 1 d . . . H7A H 0.4906 0.1828 0.7769 0.047 Uiso 1 1 calc R . . H7B H 0.5149 0.1853 0.8416 0.047 Uiso 1 1 calc R . . H7C H 0.4976 0.1257 0.8137 0.047 Uiso 1 1 calc R . . C8 C 0.59952(15) 0.21457(14) 0.76794(16) 0.0337(8) Uani 1 1 d . . . H8A H 0.6394 0.2103 0.7567 0.051 Uiso 1 1 calc R . . H8B H 0.5969 0.2391 0.8022 0.051 Uiso 1 1 calc R . . H8C H 0.5782 0.2316 0.7359 0.051 Uiso 1 1 calc R . . C9 C 0.51328(14) 0.17714(13) 0.65880(15) 0.0316(7) Uani 1 1 d . . . H9A H 0.4999 0.1960 0.6941 0.047 Uiso 1 1 calc R . . H9B H 0.4806 0.1645 0.6359 0.047 Uiso 1 1 calc R . . H9C H 0.5359 0.2038 0.6359 0.047 Uiso 1 1 calc R . . C10 C 0.54591(16) 0.09483(15) 0.56920(15) 0.0363(8) Uani 1 1 d . . . H10A H 0.5764 0.1129 0.5470 0.054 Uiso 1 1 calc R . . H10B H 0.5121 0.1190 0.5684 0.054 Uiso 1 1 calc R . . H10C H 0.5369 0.0579 0.5520 0.054 Uiso 1 1 calc R . . C11 C 0.63729(13) 0.00276(13) 0.61394(15) 0.0281(7) Uani 1 1 d . . . C12 C 0.67926(17) 0.03436(16) 0.57436(19) 0.0486(11) Uani 1 1 d . . . H12A H 0.7074 0.0542 0.5982 0.073 Uiso 1 1 calc R . . H12B H 0.6586 0.0619 0.5506 0.073 Uiso 1 1 calc R . . H12C H 0.6985 0.0071 0.5491 0.073 Uiso 1 1 calc R . . C13 C 0.59927(17) -0.03384(16) 0.57573(18) 0.0440(10) Uani 1 1 d . . . H13A H 0.6223 -0.0627 0.5561 0.066 Uiso 1 1 calc R . . H13B H 0.5806 -0.0099 0.5467 0.066 Uiso 1 1 calc R . . H13C H 0.5705 -0.0524 0.5998 0.066 Uiso 1 1 calc R . . C14 C 0.67145(16) -0.03719(15) 0.65185(18) 0.0418(9) Uani 1 1 d . . . H14A H 0.6973 -0.0152 0.6763 0.063 Uiso 1 1 calc R . . H14B H 0.6934 -0.0630 0.6273 0.063 Uiso 1 1 calc R . . H14C H 0.6457 -0.0592 0.6765 0.063 Uiso 1 1 calc R . . C15 C 0.38206(13) 0.02367(13) 0.70498(15) 0.0272(7) Uani 1 1 d . . . C16 C 0.40535(13) 0.01138(14) 0.65033(15) 0.0293(7) Uani 1 1 d . . . C17 C 0.43526(12) -0.04176(13) 0.64849(14) 0.0266(7) Uani 1 1 d . . . C18 C 0.43619(12) -0.06937(13) 0.70306(14) 0.0234(6) Uani 1 1 d . . . C19 C 0.34449(14) 0.07402(15) 0.72225(17) 0.0352(8) Uani 1 1 d . . . C20 C 0.29185(16) 0.07870(17) 0.6829(2) 0.0491(11) Uani 1 1 d . . . H20A H 0.2676 0.1096 0.6967 0.074 Uiso 1 1 calc R . . H20B H 0.2706 0.0430 0.6841 0.074 Uiso 1 1 calc R . . H20C H 0.3038 0.0864 0.6430 0.074 Uiso 1 1 calc R . . C21 C 0.32263(19) 0.0671(2) 0.78380(19) 0.0584(13) Uani 1 1 d . . . H21A H 0.3547 0.0670 0.8109 0.088 Uiso 1 1 calc R . . H21B H 0.3019 0.0312 0.7870 0.088 Uiso 1 1 calc R . . H21C H 0.2972 0.0986 0.7932 0.088 Uiso 1 1 calc R . . C22 C 0.37720(18) 0.12949(18) 0.7184(3) 0.0719(17) Uani 1 1 d . . . H22A H 0.3517 0.1612 0.7267 0.108 Uiso 1 1 calc R . . H22B H 0.3928 0.1338 0.6792 0.108 Uiso 1 1 calc R . . H22C H 0.4082 0.1292 0.7467 0.108 Uiso 1 1 calc R . . C23 C 0.39574(16) 0.04526(17) 0.59544(17) 0.0449(10) Uani 1 1 d . . . H23A H 0.3633 0.0296 0.5743 0.067 Uiso 1 1 calc R . . H23B H 0.4297 0.0433 0.5710 0.067 Uiso 1 1 calc R . . H23C H 0.3880 0.0849 0.6055 0.067 Uiso 1 1 calc R . . C24 C 0.45309(15) -0.06632(17) 0.59148(16) 0.0392(9) Uani 1 1 d . . . H24A H 0.4808 -0.0966 0.5981 0.059 Uiso 1 1 calc R . . H24B H 0.4703 -0.0366 0.5676 0.059 Uiso 1 1 calc R . . H24C H 0.4199 -0.0818 0.5715 0.059 Uiso 1 1 calc R . . C25 C 0.46569(13) -0.12605(13) 0.71777(15) 0.0281(7) Uani 1 1 d . . . C26 C 0.52972(14) -0.12129(17) 0.70813(17) 0.0376(9) Uani 1 1 d . . . H26A H 0.5481 -0.1568 0.7198 0.056 Uiso 1 1 calc R . . H26B H 0.5448 -0.0900 0.7314 0.056 Uiso 1 1 calc R . . H26C H 0.5373 -0.1141 0.6670 0.056 Uiso 1 1 calc R . . C27 C 0.44284(16) -0.17518(15) 0.6806(2) 0.0461(10) Uani 1 1 d . . . H27A H 0.4502 -0.1673 0.6396 0.069 Uiso 1 1 calc R . . H27B H 0.4019 -0.1790 0.6868 0.069 Uiso 1 1 calc R . . H27C H 0.4618 -0.2105 0.6918 0.069 Uiso 1 1 calc R . . C28 C 0.45578(17) -0.14174(17) 0.78133(18) 0.0436(10) Uani 1 1 d . . . H28A H 0.4760 -0.1770 0.7903 0.065 Uiso 1 1 calc R . . H28B H 0.4151 -0.1471 0.7881 0.065 Uiso 1 1 calc R . . H28C H 0.4699 -0.1112 0.8063 0.065 Uiso 1 1 calc R . . C29 C 0.57493(14) -0.02726(15) 0.84027(15) 0.0329(8) Uani 1 1 d . . . H29A H 0.6063 0.0001 0.8455 0.039 Uiso 1 1 calc R . . H29B H 0.5868 -0.0561 0.8115 0.039 Uiso 1 1 calc R . . C30 C 0.56043(18) -0.0547(2) 0.8964(2) 0.0596(13) Uani 1 1 d . . . H30A H 0.5939 -0.0571 0.9222 0.072 Uiso 1 1 calc R . . H30B H 0.5448 -0.0932 0.8904 0.072 Uiso 1 1 calc R . . C31 C 0.5165(3) -0.0152(3) 0.9207(2) 0.090(2) Uani 1 1 d . . . H31A H 0.4897 -0.0361 0.9459 0.108 Uiso 1 1 calc R . . H31B H 0.5347 0.0151 0.9438 0.108 Uiso 1 1 calc R . . C32 C 0.48707(16) 0.00863(17) 0.87110(16) 0.0380(8) Uani 1 1 d . . . H32A H 0.4790 0.0493 0.8778 0.046 Uiso 1 1 calc R . . H32B H 0.4507 -0.0114 0.8648 0.046 Uiso 1 1 calc R . . 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 Tm1 0.02104(8) 0.02066(8) 0.01788(8) 0.00093(5) -0.00065(5) -0.00080(4) P1 0.0202(4) 0.0244(4) 0.0239(4) -0.0007(3) 0.0026(3) 0.0020(3) P2 0.0222(4) 0.0294(4) 0.0242(4) -0.0014(3) 0.0024(3) -0.0007(3) O1 0.0253(11) 0.0372(12) 0.0224(12) 0.0065(10) -0.0001(9) 0.0053(9) C1 0.0216(14) 0.0207(14) 0.0230(16) -0.0035(12) 0.0042(12) -0.0014(11) C2 0.0252(15) 0.0170(14) 0.0238(16) 0.0002(12) 0.0034(12) -0.0016(11) C3 0.0283(16) 0.0203(14) 0.0212(16) 0.0007(12) 0.0041(13) -0.0025(11) C4 0.0270(16) 0.0238(15) 0.0226(16) -0.0028(12) 0.0076(13) 0.0003(11) C5 0.0235(15) 0.0251(15) 0.0215(16) -0.0060(12) 0.0048(12) -0.0013(12) C6 0.041(2) 0.042(2) 0.0238(18) -0.0086(15) -0.0036(15) -0.0009(15) C7 0.0265(17) 0.0372(18) 0.0296(18) -0.0079(15) 0.0097(14) -0.0025(13) C8 0.0392(19) 0.0251(16) 0.037(2) -0.0087(14) 0.0126(16) -0.0081(14) C9 0.0402(19) 0.0267(16) 0.0279(18) 0.0048(14) 0.0025(15) 0.0078(13) C10 0.051(2) 0.0369(19) 0.0211(17) 0.0017(15) 0.0016(16) 0.0057(16) C11 0.0299(16) 0.0218(15) 0.0326(19) -0.0050(13) 0.0115(14) -0.0017(12) C12 0.053(2) 0.036(2) 0.058(3) -0.0033(19) 0.034(2) -0.0029(17) C13 0.052(2) 0.0336(19) 0.047(2) -0.0133(17) 0.0101(19) -0.0032(16) C14 0.040(2) 0.0325(19) 0.053(3) -0.0039(18) 0.0121(18) 0.0150(15) C15 0.0223(15) 0.0260(16) 0.0334(19) -0.0003(14) -0.0046(13) -0.0012(12) C16 0.0270(16) 0.0323(17) 0.0288(18) 0.0064(14) -0.0068(14) -0.0074(13) C17 0.0231(15) 0.0323(17) 0.0245(17) -0.0029(13) -0.0011(13) -0.0048(12) C18 0.0183(14) 0.0244(15) 0.0274(17) -0.0027(13) 0.0012(12) -0.0030(11) C19 0.0255(17) 0.0307(18) 0.050(2) -0.0059(16) -0.0073(16) 0.0015(13) C20 0.032(2) 0.043(2) 0.072(3) 0.000(2) -0.014(2) 0.0087(16) C21 0.057(3) 0.065(3) 0.053(3) -0.022(2) 0.000(2) 0.030(2) C22 0.040(2) 0.036(2) 0.140(5) -0.026(3) -0.008(3) 0.0006(18) C23 0.045(2) 0.052(2) 0.037(2) 0.0174(19) -0.0118(18) -0.0076(17) C24 0.0365(19) 0.056(2) 0.0254(18) -0.0076(17) 0.0008(15) -0.0022(16) C25 0.0223(15) 0.0260(16) 0.036(2) -0.0010(14) -0.0022(13) 0.0004(12) C26 0.0252(17) 0.049(2) 0.039(2) -0.0010(17) 0.0003(15) 0.0004(15) C27 0.039(2) 0.0284(18) 0.071(3) -0.0148(19) -0.013(2) 0.0033(15) C28 0.046(2) 0.034(2) 0.050(3) 0.0179(18) 0.0088(19) 0.0098(16) C29 0.0331(18) 0.0376(19) 0.0280(18) 0.0054(15) -0.0082(15) 0.0076(14) C30 0.046(2) 0.075(3) 0.057(3) 0.032(3) -0.006(2) 0.010(2) C31 0.091(4) 0.148(6) 0.032(3) 0.028(3) 0.008(3) 0.046(4) C32 0.043(2) 0.049(2) 0.0221(19) 0.0014(16) 0.0078(15) 0.0113(17) _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 Tm1 O1 2.455(2) . ? Tm1 C18 2.766(3) . ? Tm1 C17 2.784(3) . ? Tm1 C1 2.789(3) . ? Tm1 C2 2.812(3) . ? Tm1 C16 2.827(3) . ? Tm1 C3 2.883(3) . ? Tm1 C15 2.884(3) . ? Tm1 C4 2.899(3) . ? Tm1 P1 2.9428(10) . ? Tm1 P2 2.9670(10) . ? P1 C4 1.767(3) . ? P1 C1 1.776(3) . ? P2 C18 1.763(3) . ? P2 C15 1.772(3) . ? O1 C32 1.456(4) . ? O1 C29 1.459(4) . ? C1 C2 1.411(4) . ? C1 C5 1.535(4) . ? C2 C3 1.430(4) . ? C2 C9 1.511(4) . ? C3 C4 1.420(4) . ? C3 C10 1.509(5) . ? C4 C11 1.537(4) . ? C5 C6 1.532(5) . ? C5 C8 1.538(4) . ? C5 C7 1.538(4) . ? C11 C14 1.517(5) . ? C11 C13 1.525(5) . ? C11 C12 1.539(5) . ? C15 C16 1.405(5) . ? C15 C19 1.535(5) . ? C16 C17 1.439(5) . ? C16 C23 1.514(5) . ? C17 C18 1.417(4) . ? C17 C24 1.497(5) . ? C18 C25 1.545(4) . ? C19 C21 1.519(6) . ? C19 C22 1.522(5) . ? C19 C20 1.542(5) . ? C25 C28 1.530(5) . ? C25 C26 1.531(5) . ? C25 C27 1.539(5) . ? C29 C30 1.488(5) . ? C30 C31 1.501(6) . ? C31 C32 1.452(6) . ? 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 Tm1 C18 93.29(8) . . ? O1 Tm1 C17 122.88(9) . . ? C18 Tm1 C17 29.58(9) . . ? O1 Tm1 C1 88.99(8) . . ? C18 Tm1 C1 175.56(9) . . ? C17 Tm1 C1 147.92(9) . . ? O1 Tm1 C2 117.62(8) . . ? C18 Tm1 C2 149.03(9) . . ? C17 Tm1 C2 119.48(9) . . ? C1 Tm1 C2 29.18(9) . . ? O1 Tm1 C16 131.99(9) . . ? C18 Tm1 C16 50.22(9) . . ? C17 Tm1 C16 29.70(9) . . ? C1 Tm1 C16 129.92(9) . . ? C2 Tm1 C16 102.08(9) . . ? O1 Tm1 C3 133.49(8) . . ? C18 Tm1 C3 126.78(9) . . ? C17 Tm1 C3 99.38(9) . . ? C1 Tm1 C3 49.57(9) . . ? C2 Tm1 C3 29.05(9) . . ? C16 Tm1 C3 94.24(9) . . ? O1 Tm1 C15 107.36(9) . . ? C18 Tm1 C15 53.37(9) . . ? C17 Tm1 C15 49.56(9) . . ? C1 Tm1 C15 129.40(9) . . ? C2 Tm1 C15 110.57(9) . . ? C16 Tm1 C15 28.46(10) . . ? C3 Tm1 C15 115.18(9) . . ? O1 Tm1 C4 113.24(8) . . ? C18 Tm1 C4 122.42(9) . . ? C17 Tm1 C4 104.78(9) . . ? C1 Tm1 C4 53.13(8) . . ? C2 Tm1 C4 49.07(8) . . ? C16 Tm1 C4 112.98(10) . . ? C3 Tm1 C4 28.44(8) . . ? C15 Tm1 C4 139.40(10) . . ? O1 Tm1 P1 80.61(5) . . ? C18 Tm1 P1 140.81(6) . . ? C17 Tm1 P1 137.05(7) . . ? C1 Tm1 P1 35.97(6) . . ? C2 Tm1 P1 54.30(6) . . ? C16 Tm1 P1 147.29(7) . . ? C3 Tm1 P1 53.79(6) . . ? C15 Tm1 P1 164.60(7) . . ? C4 Tm1 P1 35.20(7) . . ? O1 Tm1 P2 78.25(5) . . ? C18 Tm1 P2 35.61(7) . . ? C17 Tm1 P2 54.36(7) . . ? C1 Tm1 P2 148.81(6) . . ? C2 Tm1 P2 144.00(6) . . ? C16 Tm1 P2 53.83(7) . . ? C3 Tm1 P2 148.05(6) . . ? C15 Tm1 P2 35.23(7) . . ? C4 Tm1 P2 157.77(6) . . ? P1 Tm1 P2 157.89(2) . . ? C4 P1 C1 91.87(14) . . ? C4 P1 Tm1 71.04(10) . . ? C1 P1 Tm1 67.30(10) . . ? C18 P2 C15 91.82(15) . . ? C18 P2 Tm1 65.95(10) . . ? C15 P2 Tm1 69.83(10) . . ? C32 O1 C29 107.4(2) . . ? C32 O1 Tm1 128.31(19) . . ? C29 O1 Tm1 124.11(19) . . ? C2 C1 C5 127.1(3) . . ? C2 C1 P1 110.6(2) . . ? C5 C1 P1 121.9(2) . . ? C2 C1 Tm1 76.29(16) . . ? C5 C1 Tm1 120.04(19) . . ? P1 C1 Tm1 76.73(10) . . ? C1 C2 C3 113.7(3) . . ? C1 C2 C9 126.2(3) . . ? C3 C2 C9 119.4(3) . . ? C1 C2 Tm1 74.53(17) . . ? C3 C2 Tm1 78.23(16) . . ? C9 C2 Tm1 123.0(2) . . ? C4 C3 C2 112.7(3) . . ? C4 C3 C10 126.2(3) . . ? C2 C3 C10 120.5(3) . . ? C4 C3 Tm1 76.41(17) . . ? C2 C3 Tm1 72.72(16) . . ? C10 C3 Tm1 125.6(2) . . ? C3 C4 C11 126.6(3) . . ? C3 C4 P1 111.1(2) . . ? C11 C4 P1 121.3(2) . . ? C3 C4 Tm1 75.15(17) . . ? C11 C4 Tm1 126.99(19) . . ? P1 C4 Tm1 73.76(10) . . ? C6 C5 C1 111.1(3) . . ? C6 C5 C8 107.1(3) . . ? C1 C5 C8 110.0(3) . . ? C6 C5 C7 106.3(3) . . ? C1 C5 C7 112.4(3) . . ? C8 C5 C7 109.6(3) . . ? C14 C11 C13 107.1(3) . . ? C14 C11 C4 110.8(3) . . ? C13 C11 C4 113.8(3) . . ? C14 C11 C12 107.5(3) . . ? C13 C11 C12 108.0(3) . . ? C4 C11 C12 109.3(3) . . ? C16 C15 C19 128.2(3) . . ? C16 C15 P2 110.9(2) . . ? C19 C15 P2 120.7(3) . . ? C16 C15 Tm1 73.51(18) . . ? C19 C15 Tm1 122.3(2) . . ? P2 C15 Tm1 74.94(10) . . ? C15 C16 C17 113.5(3) . . ? C15 C16 C23 125.6(3) . . ? C17 C16 C23 120.6(3) . . ? C15 C16 Tm1 78.03(18) . . ? C17 C16 Tm1 73.51(17) . . ? C23 C16 Tm1 122.1(2) . . ? C18 C17 C16 112.4(3) . . ? C18 C17 C24 126.7(3) . . ? C16 C17 C24 120.1(3) . . ? C18 C17 Tm1 74.47(17) . . ? C16 C17 Tm1 76.78(18) . . ? C24 C17 Tm1 124.9(2) . . ? C17 C18 C25 126.8(3) . . ? C17 C18 P2 111.3(2) . . ? C25 C18 P2 121.9(2) . . ? C17 C18 Tm1 75.94(17) . . ? C25 C18 Tm1 114.24(19) . . ? P2 C18 Tm1 78.44(11) . . ? C21 C19 C22 108.6(4) . . ? C21 C19 C15 110.8(3) . . ? C22 C19 C15 110.9(3) . . ? C21 C19 C20 106.5(3) . . ? C22 C19 C20 108.2(3) . . ? C15 C19 C20 111.6(3) . . ? C28 C25 C26 107.9(3) . . ? C28 C25 C27 107.3(3) . . ? C26 C25 C27 108.7(3) . . ? C28 C25 C18 110.5(3) . . ? C26 C25 C18 110.4(3) . . ? C27 C25 C18 111.8(3) . . ? O1 C29 C30 106.4(3) . . ? C29 C30 C31 102.3(3) . . ? C32 C31 C30 106.1(4) . . ? C31 C32 O1 107.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.117 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.135 #=====================================================================