# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 #=============================================================================== _audit_creation_date 10-17-2005 _publ_contact_author_name 'Francois Nief' _publ_contact_author_address ; CNRS UMR 7653 Lab. Heteroelements et Coordination DCPH, Ecole Polytechnique Palaiseau 91128 FRANCE ; _publ_contact_author_email NIEF@POLY.POLYTECHNIQUE.FR _publ_section_title ; Synthesis of a new stable, neutral organothulium(II) complex by reduction of a thulium(III) precursor. ; _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 Gottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; loop_ _publ_author_name 'Francois Nief' 'Florian Jaroschik' 'Louis Ricard' #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #============================================================================= data_tmttbuazo _database_code_depnum_ccdc_archive 'CCDC 286776' #compound Cp(ttt)TmI _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58 I Tm' _chemical_formula_weight 762.63 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' I I -0.4742 1.8119 '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/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3340(10) _cell_length_b 15.7470(10) _cell_length_c 20.4740(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.4000(10) _cell_angle_gamma 90.00 _cell_volume 3287.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 3.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5922 _exptl_absorpt_correction_T_max 0.7112 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 17047 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 30.03 _reflns_number_total 9590 _reflns_number_gt 7786 _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^)+(0.1025P)^2^+9.4731P] 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 9590 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _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 0.002827(19) 0.209855(14) 0.128655(10) 0.01671(9) Uani 1 1 d . . . I1 I 0.00453(3) 0.02588(2) 0.135031(17) 0.02561(10) Uani 1 1 d . . . C1 C 0.1906(5) 0.2169(3) 0.2399(2) 0.0201(10) Uani 1 1 d . . . C2 C 0.1683(5) 0.3035(4) 0.2177(2) 0.0184(9) Uani 1 1 d . . . C3 C 0.0338(5) 0.3234(4) 0.2219(2) 0.0198(9) Uani 1 1 d . . . H3 H -0.0092 0.3754 0.2086 0.024 Uiso 1 1 calc R . . C4 C -0.0243(5) 0.2525(3) 0.2491(2) 0.0186(9) Uani 1 1 d . . . C5 C 0.0697(5) 0.1885(4) 0.2572(2) 0.0207(10) Uani 1 1 d . . . H5 H 0.0551 0.1328 0.2723 0.025 Uiso 1 1 calc R . . C6 C 0.3151(5) 0.1617(4) 0.2579(3) 0.0252(11) Uani 1 1 d . . . C7 C 0.2803(6) 0.0786(4) 0.2909(3) 0.0331(13) Uani 1 1 d . . . H7A H 0.2151 0.0471 0.2600 0.050 Uiso 1 1 calc R . . H7B H 0.2443 0.0919 0.3311 0.050 Uiso 1 1 calc R . . H7C H 0.3595 0.0439 0.3024 0.050 Uiso 1 1 calc R . . C8 C 0.4170(6) 0.2062(4) 0.3094(3) 0.0332(14) Uani 1 1 d . . . H8A H 0.4868 0.1660 0.3265 0.050 Uiso 1 1 calc R . . H8B H 0.3747 0.2266 0.3459 0.050 Uiso 1 1 calc R . . H8C H 0.4546 0.2544 0.2887 0.050 Uiso 1 1 calc R . . C9 C 0.3788(6) 0.1345(4) 0.1984(3) 0.0294(12) Uani 1 1 d . . . H9A H 0.4046 0.1850 0.1757 0.044 Uiso 1 1 calc R . . H9B H 0.3158 0.1012 0.1676 0.044 Uiso 1 1 calc R . . H9C H 0.4565 0.0998 0.2138 0.044 Uiso 1 1 calc R . . C10 C 0.2608(6) 0.3789(4) 0.2101(3) 0.0242(11) Uani 1 1 d . . . C11 C 0.3055(6) 0.4173(5) 0.2793(3) 0.0318(13) Uani 1 1 d . . . H11A H 0.3556 0.3749 0.3080 0.048 Uiso 1 1 calc R . . H11B H 0.2285 0.4345 0.2984 0.048 Uiso 1 1 calc R . . H11C H 0.3609 0.4671 0.2756 0.048 Uiso 1 1 calc R . . C12 C 0.3810(6) 0.3580(5) 0.1786(3) 0.0324(13) Uani 1 1 d . . . H12A H 0.3527 0.3374 0.1333 0.049 Uiso 1 1 calc R . . H12B H 0.4330 0.3140 0.2047 0.049 Uiso 1 1 calc R . . H12C H 0.4344 0.4092 0.1775 0.049 Uiso 1 1 calc R . . C13 C 0.1867(7) 0.4501(4) 0.1678(3) 0.0334(13) Uani 1 1 d . . . H13A H 0.2481 0.4956 0.1614 0.050 Uiso 1 1 calc R . . H13B H 0.1177 0.4729 0.1905 0.050 Uiso 1 1 calc R . . H13C H 0.1471 0.4271 0.1247 0.050 Uiso 1 1 calc R . . C14 C -0.1617(5) 0.2460(4) 0.2655(3) 0.0215(10) Uani 1 1 d . . . C15 C -0.1570(6) 0.2039(4) 0.3334(3) 0.0328(14) Uani 1 1 d . . . H15A H -0.1106 0.1496 0.3341 0.049 Uiso 1 1 calc R . . H15B H -0.2466 0.1941 0.3416 0.049 Uiso 1 1 calc R . . H15C H -0.1108 0.2412 0.3678 0.049 Uiso 1 1 calc R . . C16 C -0.2270(5) 0.3330(4) 0.2666(3) 0.0299(12) Uani 1 1 d . . . H16A H -0.1737 0.3693 0.2994 0.045 Uiso 1 1 calc R . . H16B H -0.3146 0.3262 0.2784 0.045 Uiso 1 1 calc R . . H16C H -0.2345 0.3593 0.2228 0.045 Uiso 1 1 calc R . . C17 C -0.2427(6) 0.1894(5) 0.2135(3) 0.0318(13) Uani 1 1 d . . . H17A H -0.2487 0.2159 0.1698 0.048 Uiso 1 1 calc R . . H17B H -0.3309 0.1822 0.2244 0.048 Uiso 1 1 calc R . . H17C H -0.2003 0.1338 0.2130 0.048 Uiso 1 1 calc R . . C18 C -0.1865(5) 0.2038(3) 0.0171(2) 0.0194(10) Uani 1 1 d . . . C19 C -0.1712(5) 0.2919(3) 0.0359(2) 0.0200(10) Uani 1 1 d . . . C20 C -0.0372(5) 0.3157(4) 0.0308(2) 0.0214(10) Uani 1 1 d . . . H20 H 0.0022 0.3694 0.0422 0.026 Uiso 1 1 calc R . . C21 C 0.0245(5) 0.2452(3) 0.0059(2) 0.0182(9) Uani 1 1 d . . . C22 C -0.0632(5) 0.1769(4) 0.0010(2) 0.0202(10) Uani 1 1 d . . . H22 H -0.0437 0.1207 -0.0112 0.024 Uiso 1 1 calc R . . C23 C -0.3073(5) 0.1440(4) 0.0016(3) 0.0240(11) Uani 1 1 d . . . C24 C -0.4099(5) 0.1820(5) -0.0537(3) 0.0333(13) Uani 1 1 d . . . H24A H -0.4758 0.1388 -0.0697 0.050 Uiso 1 1 calc R . . H24B H -0.3665 0.2007 -0.0903 0.050 Uiso 1 1 calc R . . H24C H -0.4527 0.2307 -0.0363 0.050 Uiso 1 1 calc R . . C25 C -0.3716(6) 0.1215(4) 0.0615(3) 0.0281(13) Uani 1 1 d . . . H25A H -0.4483 0.0854 0.0473 0.042 Uiso 1 1 calc R . . H25B H -0.3993 0.1737 0.0814 0.042 Uiso 1 1 calc R . . H25C H -0.3085 0.0911 0.0942 0.042 Uiso 1 1 calc R . . C26 C -0.2667(6) 0.0596(4) -0.0261(3) 0.0316(13) Uani 1 1 d . . . H26A H -0.1952 0.0344 0.0052 0.047 Uiso 1 1 calc R . . H26B H -0.2371 0.0696 -0.0686 0.047 Uiso 1 1 calc R . . H26C H -0.3419 0.0208 -0.0327 0.047 Uiso 1 1 calc R . . C27 C -0.2691(5) 0.3648(4) 0.0408(3) 0.0250(11) Uani 1 1 d . . . C28 C -0.2018(7) 0.4389(4) 0.0818(3) 0.0323(13) Uani 1 1 d . . . H28A H -0.2655 0.4845 0.0839 0.048 Uiso 1 1 calc R . . H28B H -0.1292 0.4603 0.0611 0.048 Uiso 1 1 calc R . . H28C H -0.1678 0.4191 0.1268 0.048 Uiso 1 1 calc R . . C29 C -0.3899(6) 0.3424(5) 0.0710(3) 0.0324(13) Uani 1 1 d . . . H29A H -0.4371 0.2956 0.0461 0.049 Uiso 1 1 calc R . . H29B H -0.4475 0.3920 0.0693 0.049 Uiso 1 1 calc R . . H29C H -0.3628 0.3251 0.1172 0.049 Uiso 1 1 calc R . . C30 C -0.3129(7) 0.4003(5) -0.0298(3) 0.0356(14) Uani 1 1 d . . . H30A H -0.3603 0.3562 -0.0578 0.053 Uiso 1 1 calc R . . H30B H -0.2357 0.4180 -0.0484 0.053 Uiso 1 1 calc R . . H30C H -0.3707 0.4493 -0.0278 0.053 Uiso 1 1 calc R . . C31 C 0.1645(5) 0.2418(4) -0.0088(3) 0.0213(10) Uani 1 1 d . . . C32 C 0.1693(6) 0.1910(5) -0.0722(3) 0.0293(12) Uani 1 1 d . . . H32A H 0.2604 0.1860 -0.0794 0.044 Uiso 1 1 calc R . . H32B H 0.1175 0.2203 -0.1099 0.044 Uiso 1 1 calc R . . H32C H 0.1328 0.1343 -0.0679 0.044 Uiso 1 1 calc R . . C33 C 0.2172(6) 0.3311(4) -0.0168(3) 0.0301(12) Uani 1 1 d . . . H33A H 0.2214 0.3622 0.0249 0.045 Uiso 1 1 calc R . . H33B H 0.1587 0.3610 -0.0519 0.045 Uiso 1 1 calc R . . H33C H 0.3052 0.3274 -0.0286 0.045 Uiso 1 1 calc R . . C34 C 0.2485(5) 0.1958(4) 0.0489(3) 0.0299(12) Uani 1 1 d . . . H34A H 0.2435 0.2260 0.0902 0.045 Uiso 1 1 calc R . . H34B H 0.3399 0.1942 0.0415 0.045 Uiso 1 1 calc R . . H34C H 0.2160 0.1377 0.0518 0.045 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 0.01762(12) 0.01708(13) 0.01510(12) -0.00010(7) 0.00162(8) -0.00063(7) I1 0.02941(19) 0.01823(19) 0.02914(19) -0.00002(12) 0.00461(14) 0.00033(12) C1 0.019(2) 0.026(3) 0.015(2) 0.0009(18) 0.0025(17) -0.0024(19) C2 0.017(2) 0.024(3) 0.015(2) -0.0019(18) 0.0037(16) -0.0055(18) C3 0.020(2) 0.022(3) 0.019(2) -0.0029(19) 0.0061(17) -0.0042(19) C4 0.027(2) 0.015(2) 0.0134(19) -0.0011(17) 0.0027(17) -0.0043(18) C5 0.020(2) 0.029(3) 0.013(2) 0.0042(19) 0.0027(16) -0.004(2) C6 0.019(2) 0.033(3) 0.023(2) 0.005(2) 0.0003(18) 0.002(2) C7 0.030(3) 0.034(3) 0.036(3) 0.014(3) 0.006(2) 0.005(3) C8 0.022(3) 0.049(4) 0.026(3) -0.001(3) -0.003(2) 0.003(2) C9 0.023(3) 0.040(4) 0.024(3) 0.000(2) 0.003(2) 0.006(2) C10 0.023(2) 0.027(3) 0.025(3) -0.005(2) 0.009(2) -0.009(2) C11 0.032(3) 0.035(3) 0.029(3) -0.009(3) 0.008(2) -0.013(3) C12 0.029(3) 0.041(4) 0.031(3) -0.007(3) 0.014(2) -0.013(3) C13 0.039(3) 0.027(3) 0.036(3) 0.004(2) 0.009(2) -0.007(3) C14 0.015(2) 0.026(3) 0.024(2) -0.002(2) 0.0061(18) -0.0020(18) C15 0.027(3) 0.047(4) 0.028(3) 0.007(3) 0.012(2) 0.000(2) C16 0.022(2) 0.033(3) 0.037(3) -0.006(2) 0.010(2) 0.001(2) C17 0.021(3) 0.040(4) 0.034(3) -0.012(3) 0.002(2) -0.003(2) C18 0.016(2) 0.025(3) 0.016(2) 0.0001(18) 0.0005(17) 0.0015(18) C19 0.021(2) 0.025(3) 0.014(2) 0.0002(18) 0.0022(17) 0.0028(18) C20 0.025(2) 0.021(2) 0.018(2) 0.0032(19) 0.0052(18) -0.001(2) C21 0.021(2) 0.024(3) 0.0114(18) -0.0023(18) 0.0054(16) -0.0024(18) C22 0.020(2) 0.023(3) 0.017(2) -0.0021(19) 0.0029(17) 0.0034(19) C23 0.018(2) 0.032(3) 0.022(2) -0.002(2) 0.0024(18) -0.004(2) C24 0.022(3) 0.051(4) 0.025(3) -0.006(3) -0.002(2) -0.001(3) C25 0.021(3) 0.040(4) 0.025(3) -0.003(2) 0.008(2) -0.009(2) C26 0.026(3) 0.033(3) 0.036(3) -0.011(3) 0.006(2) -0.006(2) C27 0.025(3) 0.031(3) 0.019(2) 0.000(2) 0.0035(19) 0.011(2) C28 0.041(3) 0.023(3) 0.034(3) -0.004(2) 0.010(3) 0.007(2) C29 0.028(3) 0.039(4) 0.031(3) 0.000(3) 0.009(2) 0.012(3) C30 0.039(3) 0.040(4) 0.028(3) 0.006(3) 0.006(2) 0.015(3) C31 0.017(2) 0.023(3) 0.024(2) -0.003(2) 0.0050(18) -0.0039(19) C32 0.026(3) 0.040(3) 0.024(3) -0.007(2) 0.010(2) -0.002(2) C33 0.026(3) 0.033(3) 0.032(3) 0.002(2) 0.009(2) -0.006(2) C34 0.020(2) 0.037(3) 0.031(3) 0.004(2) 0.000(2) -0.001(2) _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 C20 2.587(5) . ? Tm1 C3 2.597(5) . ? Tm1 C4 2.615(5) . ? Tm1 C21 2.619(5) . ? Tm1 C5 2.631(5) . ? Tm1 C22 2.643(5) . ? Tm1 C19 2.719(5) . ? Tm1 C2 2.721(5) . ? Tm1 C1 2.742(5) . ? Tm1 C18 2.756(5) . ? Tm1 I1 2.8999(5) . ? C1 C5 1.425(7) . ? C1 C2 1.445(8) . ? C1 C6 1.547(7) . ? C2 C3 1.440(7) . ? C2 C10 1.548(7) . ? C3 C4 1.424(7) . ? C4 C5 1.390(8) . ? C4 C14 1.515(7) . ? C6 C8 1.532(8) . ? C6 C9 1.538(8) . ? C6 C7 1.541(9) . ? C10 C12 1.526(8) . ? C10 C11 1.541(8) . ? C10 C13 1.542(9) . ? C14 C17 1.528(8) . ? C14 C16 1.530(8) . ? C14 C15 1.534(8) . ? C18 C22 1.431(7) . ? C18 C19 1.443(8) . ? C18 C23 1.554(7) . ? C19 C20 1.455(7) . ? C19 C27 1.543(7) . ? C20 C21 1.416(8) . ? C21 C22 1.400(7) . ? C21 C31 1.526(7) . ? C23 C25 1.529(8) . ? C23 C26 1.531(9) . ? C23 C24 1.540(8) . ? C27 C29 1.524(8) . ? C27 C28 1.536(9) . ? C27 C30 1.546(8) . ? C31 C33 1.526(8) . ? C31 C34 1.529(8) . ? C31 C32 1.533(8) . ? 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 C20 Tm1 C3 96.33(18) . . ? C20 Tm1 C4 122.47(17) . . ? C3 Tm1 C4 31.72(15) . . ? C20 Tm1 C21 31.57(17) . . ? C3 Tm1 C21 122.64(17) . . ? C4 Tm1 C21 152.83(17) . . ? C20 Tm1 C5 147.10(18) . . ? C3 Tm1 C5 51.12(18) . . ? C4 Tm1 C5 30.74(16) . . ? C21 Tm1 C5 159.60(15) . . ? C20 Tm1 C22 51.53(17) . . ? C3 Tm1 C22 147.46(17) . . ? C4 Tm1 C22 158.92(16) . . ? C21 Tm1 C22 30.85(16) . . ? C5 Tm1 C22 161.32(19) . . ? C20 Tm1 C19 31.70(16) . . ? C3 Tm1 C19 100.00(16) . . ? C4 Tm1 C19 112.08(16) . . ? C21 Tm1 C19 51.66(16) . . ? C5 Tm1 C19 142.63(16) . . ? C22 Tm1 C19 50.83(16) . . ? C20 Tm1 C2 99.97(17) . . ? C3 Tm1 C2 31.31(15) . . ? C4 Tm1 C2 51.77(15) . . ? C21 Tm1 C2 112.65(15) . . ? C5 Tm1 C2 50.61(16) . . ? C22 Tm1 C2 143.30(16) . . ? C19 Tm1 C2 118.79(17) . . ? C20 Tm1 C1 128.25(16) . . ? C3 Tm1 C1 51.41(16) . . ? C4 Tm1 C1 51.43(16) . . ? C21 Tm1 C1 128.95(15) . . ? C5 Tm1 C1 30.66(15) . . ? C22 Tm1 C1 149.63(15) . . ? C19 Tm1 C1 149.11(16) . . ? C2 Tm1 C1 30.66(16) . . ? C20 Tm1 C18 51.56(16) . . ? C3 Tm1 C18 128.21(16) . . ? C4 Tm1 C18 128.30(16) . . ? C21 Tm1 C18 51.13(15) . . ? C5 Tm1 C18 149.27(15) . . ? C22 Tm1 C18 30.65(15) . . ? C19 Tm1 C18 30.54(16) . . ? C2 Tm1 C18 149.03(15) . . ? C1 Tm1 C18 179.62(17) . . ? C20 Tm1 I1 132.65(12) . . ? C3 Tm1 I1 130.98(12) . . ? C4 Tm1 I1 102.41(11) . . ? C21 Tm1 I1 104.74(12) . . ? C5 Tm1 I1 80.13(13) . . ? C22 Tm1 I1 81.19(12) . . ? C19 Tm1 I1 120.32(11) . . ? C2 Tm1 I1 120.85(12) . . ? C1 Tm1 I1 90.26(11) . . ? C18 Tm1 I1 90.06(11) . . ? C5 C1 C2 105.9(5) . . ? C5 C1 C6 119.6(5) . . ? C2 C1 C6 133.6(5) . . ? C5 C1 Tm1 70.4(3) . . ? C2 C1 Tm1 73.9(3) . . ? C6 C1 Tm1 128.6(4) . . ? C3 C2 C1 107.0(4) . . ? C3 C2 C10 117.2(5) . . ? C1 C2 C10 133.4(5) . . ? C3 C2 Tm1 69.6(3) . . ? C1 C2 Tm1 75.5(3) . . ? C10 C2 Tm1 132.8(3) . . ? C4 C3 C2 108.9(5) . . ? C4 C3 Tm1 74.8(3) . . ? C2 C3 Tm1 79.1(3) . . ? C5 C4 C3 106.5(5) . . ? C5 C4 C14 125.9(5) . . ? C3 C4 C14 127.6(5) . . ? C5 C4 Tm1 75.3(3) . . ? C3 C4 Tm1 73.5(3) . . ? C14 C4 Tm1 116.1(3) . . ? C4 C5 C1 111.5(5) . . ? C4 C5 Tm1 74.0(3) . . ? C1 C5 Tm1 79.0(3) . . ? C8 C6 C9 109.8(5) . . ? C8 C6 C7 105.7(5) . . ? C9 C6 C7 105.7(5) . . ? C8 C6 C1 111.0(5) . . ? C9 C6 C1 114.5(4) . . ? C7 C6 C1 109.7(4) . . ? C12 C10 C11 109.3(5) . . ? C12 C10 C13 106.4(5) . . ? C11 C10 C13 106.1(5) . . ? C12 C10 C2 115.9(5) . . ? C11 C10 C2 107.8(5) . . ? C13 C10 C2 110.8(5) . . ? C4 C14 C17 108.2(4) . . ? C4 C14 C16 112.0(5) . . ? C17 C14 C16 109.9(5) . . ? C4 C14 C15 109.8(4) . . ? C17 C14 C15 108.2(5) . . ? C16 C14 C15 108.7(5) . . ? C22 C18 C19 106.5(5) . . ? C22 C18 C23 119.3(5) . . ? C19 C18 C23 133.4(5) . . ? C22 C18 Tm1 70.3(3) . . ? C19 C18 Tm1 73.3(3) . . ? C23 C18 Tm1 128.9(3) . . ? C18 C19 C20 107.0(5) . . ? C18 C19 C27 133.5(5) . . ? C20 C19 C27 117.1(5) . . ? C18 C19 Tm1 76.2(3) . . ? C20 C19 Tm1 69.2(3) . . ? C27 C19 Tm1 132.4(3) . . ? C21 C20 C19 108.3(5) . . ? C21 C20 Tm1 75.5(3) . . ? C19 C20 Tm1 79.1(3) . . ? C22 C21 C20 107.7(4) . . ? C22 C21 C31 125.7(5) . . ? C20 C21 C31 126.5(5) . . ? C22 C21 Tm1 75.5(3) . . ? C20 C21 Tm1 73.0(3) . . ? C31 C21 Tm1 114.5(3) . . ? C21 C22 C18 110.3(5) . . ? C21 C22 Tm1 73.6(3) . . ? C18 C22 Tm1 79.1(3) . . ? C25 C23 C26 106.1(5) . . ? C25 C23 C24 110.0(5) . . ? C26 C23 C24 105.2(5) . . ? C25 C23 C18 114.6(4) . . ? C26 C23 C18 110.0(4) . . ? C24 C23 C18 110.4(5) . . ? C29 C27 C28 106.3(5) . . ? C29 C27 C19 116.3(5) . . ? C28 C27 C19 110.9(5) . . ? C29 C27 C30 109.2(5) . . ? C28 C27 C30 105.9(5) . . ? C19 C27 C30 107.7(5) . . ? C33 C31 C21 110.8(5) . . ? C33 C31 C34 110.7(5) . . ? C21 C31 C34 107.5(4) . . ? C33 C31 C32 109.2(5) . . ? C21 C31 C32 110.3(4) . . ? C34 C31 C32 108.3(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 8.254 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.288 #END=== data_tmtristbu _database_code_depnum_ccdc_archive 'CCDC 286777' #compound Cp(ttt)Tm(THF) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 O Tm' _chemical_formula_weight 707.84 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' 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 10.2120(10) _cell_length_b 15.6790(10) _cell_length_c 23.3570(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.3800(10) _cell_angle_gamma 90.00 _cell_volume 3728.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 2.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6198 _exptl_absorpt_correction_T_max 0.7613 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 16147 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10291 _reflns_number_gt 7324 _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^)+(0.0383P)^2^+0.9539P] 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 10291 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 0.675944(14) 0.298366(9) 0.862972(6) 0.02545(5) Uani 1 1 d . . . C1 C 0.5859(3) 0.46128(19) 0.87262(14) 0.0245(7) Uani 1 1 d . . . H1 H 0.5596 0.4754 0.9096 0.029 Uiso 1 1 calc R . . O1 O 0.8306(2) 0.23825(14) 0.79715(10) 0.0328(6) Uani 1 1 d . . . C2 C 0.5005(3) 0.4275(2) 0.82695(14) 0.0264(7) Uani 1 1 d . . . C3 C 0.5810(3) 0.41504(19) 0.77959(14) 0.0261(7) Uani 1 1 d . . . C4 C 0.7108(3) 0.4416(2) 0.79876(15) 0.0275(7) Uani 1 1 d . . . H4 H 0.7842 0.4398 0.7761 0.033 Uiso 1 1 calc R . . C5 C 0.7149(3) 0.4709(2) 0.85546(14) 0.0264(7) Uani 1 1 d . . . C6 C 0.3509(3) 0.4331(2) 0.83186(16) 0.0331(8) Uani 1 1 d . . . C7 C 0.3069(3) 0.5248(2) 0.81534(16) 0.0393(9) Uani 1 1 d . . . H7A H 0.3203 0.5350 0.7748 0.059 Uiso 1 1 calc R . . H7B H 0.3589 0.5658 0.8392 0.059 Uiso 1 1 calc R . . H7C H 0.2137 0.5318 0.8215 0.059 Uiso 1 1 calc R . . C8 C 0.3187(4) 0.4186(3) 0.89475(16) 0.0443(10) Uani 1 1 d . . . H8A H 0.2234 0.4214 0.8972 0.067 Uiso 1 1 calc R . . H8B H 0.3614 0.4629 0.9192 0.067 Uiso 1 1 calc R . . H8C H 0.3509 0.3624 0.9076 0.067 Uiso 1 1 calc R . . C9 C 0.2651(4) 0.3711(3) 0.79593(19) 0.0513(11) Uani 1 1 d . . . H9A H 0.2758 0.3810 0.7551 0.077 Uiso 1 1 calc R . . H9B H 0.1729 0.3797 0.8035 0.077 Uiso 1 1 calc R . . H9C H 0.2912 0.3125 0.8060 0.077 Uiso 1 1 calc R . . C10 C 0.5477(4) 0.3868(2) 0.71692(15) 0.0330(8) Uani 1 1 d . . . C11 C 0.4966(5) 0.2946(2) 0.71278(19) 0.0481(11) Uani 1 1 d . . . H11A H 0.5644 0.2557 0.7294 0.072 Uiso 1 1 calc R . . H11B H 0.4751 0.2797 0.6724 0.072 Uiso 1 1 calc R . . H11C H 0.4177 0.2895 0.7339 0.072 Uiso 1 1 calc R . . C12 C 0.6711(4) 0.3888(3) 0.68272(15) 0.0460(10) Uani 1 1 d . . . H12A H 0.7042 0.4474 0.6814 0.069 Uiso 1 1 calc R . . H12B H 0.6485 0.3684 0.6435 0.069 Uiso 1 1 calc R . . H12C H 0.7389 0.3519 0.7015 0.069 Uiso 1 1 calc R . . C13 C 0.4483(4) 0.4476(2) 0.68547(16) 0.0378(9) Uani 1 1 d . . . H13A H 0.3651 0.4455 0.7038 0.057 Uiso 1 1 calc R . . H13B H 0.4334 0.4302 0.6452 0.057 Uiso 1 1 calc R . . H13C H 0.4830 0.5059 0.6874 0.057 Uiso 1 1 calc R . . C14 C 0.8318(3) 0.5095(2) 0.89078(15) 0.0304(8) Uani 1 1 d . . . C15 C 0.9062(5) 0.5703(3) 0.8542(2) 0.0680(15) Uani 1 1 d . . . H15A H 0.9270 0.5414 0.8189 0.102 Uiso 1 1 calc R . . H15B H 0.9878 0.5881 0.8757 0.102 Uiso 1 1 calc R . . H15C H 0.8518 0.6205 0.8446 0.102 Uiso 1 1 calc R . . C16 C 0.7893(4) 0.5561(3) 0.94341(19) 0.0517(11) Uani 1 1 d . . . H16A H 0.7310 0.6035 0.9312 0.078 Uiso 1 1 calc R . . H16B H 0.8668 0.5784 0.9658 0.078 Uiso 1 1 calc R . . H16C H 0.7425 0.5165 0.9671 0.078 Uiso 1 1 calc R . . C17 C 0.9240(4) 0.4381(3) 0.91104(19) 0.0567(12) Uani 1 1 d . . . H17A H 0.8769 0.3972 0.9336 0.085 Uiso 1 1 calc R . . H17B H 0.9984 0.4618 0.9349 0.085 Uiso 1 1 calc R . . H17C H 0.9563 0.4091 0.8777 0.085 Uiso 1 1 calc R . . C18 C 0.5448(4) 0.2156(2) 0.94282(16) 0.0329(8) Uani 1 1 d . . . H18 H 0.4633 0.2412 0.9500 0.039 Uiso 1 1 calc R . . C19 C 0.6662(4) 0.2354(2) 0.97330(15) 0.0302(8) Uani 1 1 d . . . C20 C 0.7637(4) 0.1843(2) 0.94834(15) 0.0304(8) Uani 1 1 d . . . C21 C 0.6953(4) 0.1360(2) 0.90367(15) 0.0322(8) Uani 1 1 d . . . H21 H 0.7363 0.0973 0.8793 0.039 Uiso 1 1 calc R . . C22 C 0.5602(4) 0.1527(2) 0.90026(15) 0.0308(8) Uani 1 1 d . A . C23 C 0.6628(4) 0.2844(2) 1.03087(15) 0.0350(8) Uani 1 1 d . . . C24 C 0.5564(4) 0.3539(3) 1.02594(18) 0.0491(10) Uani 1 1 d . . . H24A H 0.4707 0.3275 1.0159 0.074 Uiso 1 1 calc R . . H24B H 0.5762 0.3947 0.9960 0.074 Uiso 1 1 calc R . . H24C H 0.5545 0.3837 1.0627 0.074 Uiso 1 1 calc R . . C25 C 0.7894(4) 0.3297(3) 1.05242(17) 0.0464(10) Uani 1 1 d . . . H25A H 0.7767 0.3579 1.0890 0.070 Uiso 1 1 calc R . . H25B H 0.8120 0.3724 1.0242 0.070 Uiso 1 1 calc R . . H25C H 0.8607 0.2880 1.0579 0.070 Uiso 1 1 calc R . . C26 C 0.6262(5) 0.2207(3) 1.07680(18) 0.0541(12) Uani 1 1 d . . . H26A H 0.6922 0.1753 1.0806 0.081 Uiso 1 1 calc R . . H26B H 0.5400 0.1959 1.0656 0.081 Uiso 1 1 calc R . . H26C H 0.6230 0.2502 1.1136 0.081 Uiso 1 1 calc R . . C27 C 0.9094(4) 0.1639(2) 0.96621(15) 0.0334(8) Uani 1 1 d . . . C28 C 1.0032(4) 0.2406(3) 0.96546(18) 0.0459(10) Uani 1 1 d . . . H28A H 1.0071 0.2608 0.9259 0.069 Uiso 1 1 calc R . . H28B H 1.0912 0.2233 0.9808 0.069 Uiso 1 1 calc R . . H28C H 0.9712 0.2866 0.9891 0.069 Uiso 1 1 calc R . . C29 C 0.9212(4) 0.1213(3) 1.02556(17) 0.0512(11) Uani 1 1 d . . . H29A H 0.8976 0.1624 1.0546 0.077 Uiso 1 1 calc R . . H29B H 1.0118 0.1020 1.0345 0.077 Uiso 1 1 calc R . . H29C H 0.8617 0.0722 1.0254 0.077 Uiso 1 1 calc R . . C30 C 0.9627(4) 0.0993(2) 0.92440(17) 0.0440(10) Uani 1 1 d . . . H30A H 0.9110 0.0466 0.9248 0.066 Uiso 1 1 calc R . . H30B H 1.0548 0.0867 0.9362 0.066 Uiso 1 1 calc R . . H30C H 0.9562 0.1233 0.8856 0.066 Uiso 1 1 calc R . . C31 C 0.4531(4) 0.0985(2) 0.86987(16) 0.0369(8) Uani 1 1 d . . . C32 C 0.494(3) 0.049(2) 0.8226(10) 0.068(3) Uani 0.32(2) 1 d P A 1 H32A H 0.4192 0.0178 0.8046 0.103 Uiso 0.32(2) 1 calc PR A 1 H32B H 0.5630 0.0091 0.8365 0.103 Uiso 0.32(2) 1 calc PR A 1 H32C H 0.5290 0.0877 0.7942 0.103 Uiso 0.32(2) 1 calc PR A 1 C33 C 0.403(3) 0.0347(14) 0.9154(9) 0.051(6) Uani 0.32(2) 1 d P A 1 H33A H 0.3655 0.0670 0.9461 0.077 Uiso 0.32(2) 1 calc PR A 1 H33B H 0.4766 0.0001 0.9316 0.077 Uiso 0.32(2) 1 calc PR A 1 H33C H 0.3355 -0.0026 0.8967 0.077 Uiso 0.32(2) 1 calc PR A 1 C34 C 0.327(2) 0.1460(14) 0.8472(9) 0.043(5) Uani 0.32(2) 1 d P A 1 H34A H 0.2563 0.1045 0.8379 0.065 Uiso 0.32(2) 1 calc PR A 1 H34B H 0.3436 0.1782 0.8126 0.065 Uiso 0.32(2) 1 calc PR A 1 H34C H 0.2996 0.1853 0.8767 0.065 Uiso 0.32(2) 1 calc PR A 1 C32A C 0.4823(12) 0.0844(10) 0.8058(5) 0.068(3) Uani 0.68(2) 1 d P A 2 H32D H 0.4261 0.0386 0.7892 0.103 Uiso 0.68(2) 1 calc PR A 2 H32E H 0.5747 0.0685 0.8040 0.103 Uiso 0.68(2) 1 calc PR A 2 H32F H 0.4644 0.1371 0.7842 0.103 Uiso 0.68(2) 1 calc PR A 2 C33A C 0.4587(15) 0.0102(7) 0.8967(7) 0.080(4) Uani 0.68(2) 1 d P A 2 H33D H 0.4376 0.0141 0.9369 0.120 Uiso 0.68(2) 1 calc PR A 2 H33E H 0.5471 -0.0135 0.8950 0.120 Uiso 0.68(2) 1 calc PR A 2 H33F H 0.3949 -0.0271 0.8756 0.120 Uiso 0.68(2) 1 calc PR A 2 C34A C 0.3206(12) 0.1360(9) 0.8757(7) 0.077(4) Uani 0.68(2) 1 d P A 2 H34D H 0.3095 0.1474 0.9163 0.116 Uiso 0.68(2) 1 calc PR A 2 H34E H 0.2529 0.0958 0.8607 0.116 Uiso 0.68(2) 1 calc PR A 2 H34F H 0.3122 0.1894 0.8539 0.116 Uiso 0.68(2) 1 calc PR A 2 C35 C 0.9584(4) 0.2734(2) 0.78781(16) 0.0345(8) Uani 1 1 d . . . H35A H 1.0120 0.2794 0.8247 0.041 Uiso 1 1 calc R . . H35B H 0.9491 0.3302 0.7694 0.041 Uiso 1 1 calc R . . C36 C 1.0222(4) 0.2115(3) 0.7490(2) 0.0554(12) Uani 1 1 d . . . H36A H 1.0794 0.1707 0.7716 0.067 Uiso 1 1 calc R . . H36B H 1.0749 0.2419 0.7216 0.067 Uiso 1 1 calc R . . C37 C 0.9056(4) 0.1663(3) 0.71798(18) 0.0463(10) Uani 1 1 d . . . H37A H 0.8664 0.2006 0.6855 0.056 Uiso 1 1 calc R . . H37B H 0.9305 0.1095 0.7038 0.056 Uiso 1 1 calc R . . C38 C 0.8140(4) 0.1590(2) 0.76561(16) 0.0356(8) Uani 1 1 d . . . H38A H 0.7219 0.1521 0.7497 0.043 Uiso 1 1 calc R . . H38B H 0.8381 0.1097 0.7907 0.043 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 0.02847(8) 0.02317(8) 0.02472(8) 0.00029(7) 0.00206(6) 0.00060(7) C1 0.0241(16) 0.0245(15) 0.0253(17) 0.0031(14) 0.0036(13) 0.0009(13) O1 0.0332(14) 0.0256(12) 0.0398(15) -0.0027(11) 0.0042(11) 0.0015(10) C2 0.0263(17) 0.0244(16) 0.0286(17) 0.0038(14) 0.0029(14) 0.0010(13) C3 0.0300(18) 0.0207(16) 0.0272(17) 0.0019(13) -0.0009(14) 0.0015(13) C4 0.0242(17) 0.0260(17) 0.0328(18) 0.0030(14) 0.0058(14) 0.0005(13) C5 0.0274(17) 0.0205(16) 0.0315(18) 0.0006(14) 0.0031(14) 0.0033(13) C6 0.0241(18) 0.0373(19) 0.038(2) -0.0006(16) -0.0004(15) -0.0032(15) C7 0.0261(19) 0.049(2) 0.043(2) 0.0041(18) 0.0025(16) 0.0092(16) C8 0.028(2) 0.063(3) 0.043(2) 0.010(2) 0.0099(17) -0.0028(18) C9 0.036(2) 0.059(3) 0.058(3) 0.001(2) -0.002(2) -0.019(2) C10 0.040(2) 0.0300(18) 0.0286(18) 0.0004(15) -0.0020(15) 0.0037(16) C11 0.063(3) 0.034(2) 0.044(2) -0.0089(19) -0.013(2) 0.0032(19) C12 0.048(2) 0.065(3) 0.0251(19) -0.0019(19) 0.0038(17) 0.010(2) C13 0.045(2) 0.038(2) 0.0296(19) -0.0016(16) -0.0034(17) 0.0018(17) C14 0.0251(17) 0.0347(18) 0.0308(19) 0.0003(16) -0.0012(14) -0.0002(15) C15 0.060(3) 0.083(3) 0.058(3) 0.022(3) -0.018(2) -0.042(3) C16 0.036(2) 0.056(3) 0.062(3) -0.029(2) -0.006(2) 0.0015(19) C17 0.055(3) 0.063(3) 0.049(3) -0.011(2) -0.015(2) 0.021(2) C18 0.036(2) 0.0315(19) 0.0323(19) 0.0000(15) 0.0100(16) -0.0008(15) C19 0.038(2) 0.0263(16) 0.0264(18) 0.0029(15) 0.0036(15) -0.0015(15) C20 0.039(2) 0.0262(17) 0.0259(17) 0.0040(14) 0.0012(15) 0.0027(14) C21 0.049(2) 0.0235(16) 0.0242(17) -0.0022(14) 0.0011(16) 0.0014(15) C22 0.036(2) 0.0212(16) 0.036(2) 0.0035(15) 0.0053(16) -0.0030(14) C23 0.046(2) 0.0332(19) 0.0265(18) -0.0012(15) 0.0057(16) 0.0014(16) C24 0.055(3) 0.053(2) 0.040(2) -0.011(2) 0.008(2) 0.009(2) C25 0.054(3) 0.049(2) 0.036(2) -0.0118(19) 0.0014(19) 0.001(2) C26 0.077(3) 0.056(3) 0.031(2) 0.003(2) 0.014(2) -0.003(2) C27 0.039(2) 0.0301(18) 0.0296(19) -0.0001(16) -0.0043(16) 0.0079(16) C28 0.046(2) 0.042(2) 0.048(2) -0.003(2) -0.007(2) 0.0026(19) C29 0.065(3) 0.049(2) 0.038(2) 0.005(2) -0.004(2) 0.016(2) C30 0.046(2) 0.044(2) 0.041(2) -0.0027(19) -0.0057(19) 0.0146(19) C31 0.040(2) 0.0331(19) 0.036(2) 0.0018(17) -0.0011(17) -0.0101(17) C32 0.063(5) 0.107(10) 0.035(6) -0.011(5) 0.002(5) -0.046(7) C33 0.073(16) 0.035(10) 0.044(10) 0.013(8) -0.009(9) -0.023(9) C34 0.040(9) 0.039(8) 0.049(11) -0.012(8) -0.003(9) 0.016(7) C32A 0.063(5) 0.107(10) 0.035(6) -0.011(5) 0.002(5) -0.046(7) C33A 0.099(10) 0.043(6) 0.094(10) 0.009(6) -0.017(7) -0.027(6) C34A 0.049(5) 0.081(7) 0.101(10) -0.030(8) -0.009(7) -0.025(5) C35 0.0295(19) 0.0356(18) 0.038(2) -0.0059(17) 0.0039(16) -0.0033(15) C36 0.042(2) 0.060(3) 0.066(3) -0.028(2) 0.015(2) -0.010(2) C37 0.046(2) 0.048(2) 0.046(2) -0.018(2) 0.011(2) -0.0060(19) C38 0.037(2) 0.0283(18) 0.041(2) -0.0062(17) 0.0023(17) 0.0001(16) _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 2.473(2) . ? Tm1 C18 2.709(4) . ? Tm1 C21 2.720(3) . ? Tm1 C1 2.730(3) . ? Tm1 C4 2.739(3) . ? Tm1 C5 2.741(3) . ? Tm1 C22 2.744(3) . ? Tm1 C19 2.768(3) . ? Tm1 C20 2.776(3) . ? Tm1 C2 2.791(3) . ? Tm1 C3 2.791(3) . ? C1 C5 1.414(5) . ? C1 C2 1.427(4) . ? O1 C38 1.448(4) . ? O1 C35 1.449(4) . ? C2 C3 1.441(4) . ? C2 C6 1.544(5) . ? C3 C4 1.429(4) . ? C3 C10 1.542(5) . ? C4 C5 1.399(5) . ? C5 C14 1.525(5) . ? C6 C9 1.518(5) . ? C6 C7 1.546(5) . ? C6 C8 1.546(5) . ? C10 C11 1.538(5) . ? C10 C13 1.538(5) . ? C10 C12 1.543(5) . ? C14 C17 1.516(5) . ? C14 C15 1.520(5) . ? C14 C16 1.521(5) . ? C18 C19 1.416(5) . ? C18 C22 1.417(5) . ? C19 C20 1.436(5) . ? C19 C23 1.551(5) . ? C20 C21 1.428(5) . ? C20 C27 1.548(5) . ? C21 C22 1.401(5) . ? C22 C31 1.518(5) . ? C23 C25 1.526(5) . ? C23 C26 1.533(5) . ? C23 C24 1.537(5) . ? C27 C29 1.535(5) . ? C27 C30 1.535(5) . ? C27 C28 1.539(5) . ? C31 C32 1.44(3) . ? C31 C34A 1.491(13) . ? C31 C33A 1.519(11) . ? C31 C34 1.55(2) . ? C31 C32A 1.563(12) . ? C31 C33 1.57(2) . ? C35 C36 1.509(5) . ? C36 C37 1.521(6) . ? C37 C38 1.512(5) . ? 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 128.18(10) . . ? O1 Tm1 C21 80.07(10) . . ? C18 Tm1 C21 48.51(11) . . ? O1 Tm1 C1 130.02(9) . . ? C18 Tm1 C1 101.77(10) . . ? C21 Tm1 C1 149.66(10) . . ? O1 Tm1 C4 81.74(9) . . ? C18 Tm1 C4 149.49(10) . . ? C21 Tm1 C4 161.81(11) . . ? C1 Tm1 C4 48.44(10) . . ? O1 Tm1 C5 103.51(9) . . ? C18 Tm1 C5 126.77(10) . . ? C21 Tm1 C5 159.89(10) . . ? C1 Tm1 C5 29.96(10) . . ? C4 Tm1 C5 29.58(10) . . ? O1 Tm1 C22 101.01(9) . . ? C18 Tm1 C22 30.13(10) . . ? C21 Tm1 C22 29.70(10) . . ? C1 Tm1 C22 126.63(10) . . ? C4 Tm1 C22 158.99(10) . . ? C5 Tm1 C22 155.46(10) . . ? O1 Tm1 C19 120.85(9) . . ? C18 Tm1 C19 29.94(11) . . ? C21 Tm1 C19 49.28(10) . . ? C1 Tm1 C19 102.74(10) . . ? C4 Tm1 C19 144.84(10) . . ? C5 Tm1 C19 115.29(10) . . ? C22 Tm1 C19 50.26(10) . . ? O1 Tm1 C20 90.83(9) . . ? C18 Tm1 C20 49.18(11) . . ? C21 Tm1 C20 30.09(10) . . ? C1 Tm1 C20 129.49(10) . . ? C4 Tm1 C20 150.86(10) . . ? C5 Tm1 C20 129.89(10) . . ? C22 Tm1 C20 50.12(11) . . ? C19 Tm1 C20 30.02(10) . . ? O1 Tm1 C2 120.99(9) . . ? C18 Tm1 C2 102.44(10) . . ? C21 Tm1 C2 144.35(11) . . ? C1 Tm1 C2 29.93(9) . . ? C4 Tm1 C2 49.24(10) . . ? C5 Tm1 C2 50.03(10) . . ? C22 Tm1 C2 114.68(10) . . ? C19 Tm1 C2 118.13(10) . . ? C20 Tm1 C2 148.08(10) . . ? O1 Tm1 C3 91.17(9) . . ? C18 Tm1 C3 129.09(11) . . ? C21 Tm1 C3 150.40(10) . . ? C1 Tm1 C3 48.94(9) . . ? C4 Tm1 C3 29.92(9) . . ? C5 Tm1 C3 49.69(9) . . ? C22 Tm1 C3 129.19(10) . . ? C19 Tm1 C3 147.98(10) . . ? C20 Tm1 C3 177.99(10) . . ? C2 Tm1 C3 29.92(9) . . ? C5 C1 C2 110.9(3) . . ? C5 C1 Tm1 75.45(17) . . ? C2 C1 Tm1 77.39(18) . . ? C38 O1 C35 108.7(3) . . ? C38 O1 Tm1 126.0(2) . . ? C35 O1 Tm1 125.06(19) . . ? C1 C2 C3 105.8(3) . . ? C1 C2 C6 118.4(3) . . ? C3 C2 C6 133.7(3) . . ? C1 C2 Tm1 72.68(17) . . ? C3 C2 Tm1 75.07(18) . . ? C6 C2 Tm1 129.4(2) . . ? C4 C3 C2 106.8(3) . . ? C4 C3 C10 120.9(3) . . ? C2 C3 C10 132.1(3) . . ? C4 C3 Tm1 73.02(18) . . ? C2 C3 Tm1 75.02(18) . . ? C10 C3 Tm1 120.9(2) . . ? C5 C4 C3 110.6(3) . . ? C5 C4 Tm1 75.28(19) . . ? C3 C4 Tm1 77.05(18) . . ? C4 C5 C1 105.8(3) . . ? C4 C5 C14 127.5(3) . . ? C1 C5 C14 126.7(3) . . ? C4 C5 Tm1 75.15(18) . . ? C1 C5 Tm1 74.59(17) . . ? C14 C5 Tm1 118.0(2) . . ? C9 C6 C2 117.1(3) . . ? C9 C6 C7 108.2(3) . . ? C2 C6 C7 107.7(3) . . ? C9 C6 C8 106.0(3) . . ? C2 C6 C8 110.2(3) . . ? C7 C6 C8 107.2(3) . . ? C11 C10 C13 110.2(3) . . ? C11 C10 C3 112.3(3) . . ? C13 C10 C3 111.4(3) . . ? C11 C10 C12 105.9(3) . . ? C13 C10 C12 106.0(3) . . ? C3 C10 C12 110.9(3) . . ? C17 C14 C15 108.2(4) . . ? C17 C14 C16 108.1(3) . . ? C15 C14 C16 109.8(3) . . ? C17 C14 C5 108.5(3) . . ? C15 C14 C5 110.5(3) . . ? C16 C14 C5 111.6(3) . . ? C19 C18 C22 111.4(3) . . ? C19 C18 Tm1 77.4(2) . . ? C22 C18 Tm1 76.3(2) . . ? C18 C19 C20 106.3(3) . . ? C18 C19 C23 117.9(3) . . ? C20 C19 C23 133.6(3) . . ? C18 C19 Tm1 72.7(2) . . ? C20 C19 Tm1 75.29(19) . . ? C23 C19 Tm1 129.4(2) . . ? C21 C20 C19 106.1(3) . . ? C21 C20 C27 119.6(3) . . ? C19 C20 C27 133.5(3) . . ? C21 C20 Tm1 72.77(18) . . ? C19 C20 Tm1 74.69(19) . . ? C27 C20 Tm1 125.3(2) . . ? C22 C21 C20 111.5(3) . . ? C22 C21 Tm1 76.09(19) . . ? C20 C21 Tm1 77.14(18) . . ? C21 C22 C18 104.6(3) . . ? C21 C22 C31 126.4(3) . . ? C18 C22 C31 127.0(3) . . ? C21 C22 Tm1 74.21(19) . . ? C18 C22 Tm1 73.59(19) . . ? C31 C22 Tm1 129.1(2) . . ? C25 C23 C26 108.6(3) . . ? C25 C23 C24 105.7(3) . . ? C26 C23 C24 107.8(3) . . ? C25 C23 C19 116.3(3) . . ? C26 C23 C19 107.9(3) . . ? C24 C23 C19 110.4(3) . . ? C29 C27 C30 106.3(3) . . ? C29 C27 C28 110.2(3) . . ? C30 C27 C28 104.9(3) . . ? C29 C27 C20 109.9(3) . . ? C30 C27 C20 110.2(3) . . ? C28 C27 C20 115.0(3) . . ? C32 C31 C34A 127.1(13) . . ? C32 C31 C22 114.6(11) . . ? C34A C31 C22 111.3(5) . . ? C32 C31 C33A 80.0(10) . . ? C34A C31 C33A 109.1(7) . . ? C22 C31 C33A 108.3(5) . . ? C32 C31 C34 106.3(13) . . ? C34A C31 C34 26.1(7) . . ? C22 C31 C34 116.3(9) . . ? C33A C31 C34 125.7(11) . . ? C32 C31 C32A 25.7(12) . . ? C34A C31 C32A 112.6(7) . . ? C22 C31 C32A 110.1(5) . . ? C33A C31 C32A 105.2(6) . . ? C34 C31 C32A 87.5(8) . . ? C32 C31 C33 108.0(11) . . ? C34A C31 C33 81.1(9) . . ? C22 C31 C33 107.5(8) . . ? C33A C31 C33 31.3(7) . . ? C34 C31 C33 103.3(12) . . ? C32A C31 C33 130.7(8) . . ? O1 C35 C36 106.4(3) . . ? C35 C36 C37 103.2(3) . . ? C38 C37 C36 101.0(3) . . ? O1 C38 C37 104.8(3) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 2.282 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.110 #END===