Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ROTHWELL@PURDUE.EDU _publ_contact_author_name 'Dr Ian Rothwell' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 26-09-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Drive West Lafayette IN 47907-2038 UNITED STATES OF AMERICA ; _publ_section_title ; Synthesis, Stereochemistry, Bonding and Fluxionality of 2-(Inden-3-yl)phenols and their Cyclopentadienyl Titanium Derivatives. ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G, Polidori, G. Spagna R. (1999). J. Appl. Cryst., 32, 115-119 Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of Gottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands ; loop_ _publ_author_name 'Ian Rothwell' 'Robert W. Chesnut' 'Philip E. Fanwick' 'R. D. Swartz' 'Mathew G. Thorn' ; L.E.Turner ; #=================================================================== data_LTTI32 _database_code_CSD 218466 _audit_creation_date 28-10-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C31 H38 Cl2 O1 Ti1' _chemical_formula_moiety 'C31 H38 Cl2 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 545.45 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 13.5218(2) _cell_length_b 9.8978(2) _cell_length_c 21.7332(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.3954(14) _cell_angle_gamma 90.00 _cell_volume 2900.13(8) _cell_measurement_reflns_used 27797 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.25 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.497 _cell_measurement_temperature 150 _exptl_crystal_F_000 1152 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.8291 _exptl_absorpt_correction_T_max 0.9980 _diffrn_reflns_number 27797 _diffrn_measured_fraction_theta_max 0.9937 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9937 _reflns_number_total 6559 _reflns_number_gt 5401 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_max 27 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.119 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6542 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0614P)^2^+2.7344P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.63 _refine_diff_density_min -0.53 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.10790(3) 0.16214(4) 0.92337(2) 0.02711(13) Uani 1 1 d . . . Cl(1) Cl 0.02968(5) -0.03201(7) 0.89367(3) 0.04073(18) Uani 1 1 d . . . Cl(2) Cl 0.19798(5) 0.09249(7) 1.00941(3) 0.03638(17) Uani 1 1 d . . . O(1) O 0.19170(11) 0.18427(16) 0.86438(7) 0.0253(4) Uani 1 1 d . . . C(1) C -0.0368(2) 0.2810(4) 0.89542(16) 0.0548(9) Uani 1 1 d . . . C(2) C -0.0463(2) 0.2364(3) 0.95614(14) 0.0412(7) Uani 1 1 d . . . C(3) C 0.0265(2) 0.2985(3) 0.99409(14) 0.0431(7) Uani 1 1 d . . . C(4) C 0.0828(2) 0.3821(3) 0.9575(2) 0.0584(10) Uani 1 1 d . . . C(5) C 0.0419(3) 0.3712(3) 0.89646(19) 0.0616(11) Uani 1 1 d . . . C(11) C 0.24777(16) 0.2475(2) 0.82265(10) 0.0224(5) Uani 1 1 d . . . C(12) C 0.32092(17) 0.3383(2) 0.84577(10) 0.0235(5) Uani 1 1 d . . . C(13) C 0.38179(17) 0.4006(3) 0.80492(11) 0.0264(5) Uani 1 1 d . . . C(14) C 0.37245(17) 0.3742(2) 0.74217(10) 0.0256(5) Uani 1 1 d . . . C(15) C 0.29783(17) 0.2848(2) 0.72086(10) 0.0252(5) Uani 1 1 d . . . C(16) C 0.23378(17) 0.2198(2) 0.75864(10) 0.0244(5) Uani 1 1 d . . . C(21) C 0.33677(17) 0.3741(2) 0.91213(10) 0.0251(5) Uani 1 1 d . . . C(22) C 0.38072(17) 0.2945(3) 0.95666(11) 0.0272(5) Uani 1 1 d . . . C(23) C 0.39117(18) 0.3688(3) 1.01703(11) 0.0300(5) Uani 1 1 d . . . C(24) C 0.34868(17) 0.5062(3) 1.00122(11) 0.0270(5) Uani 1 1 d . . . C(25) C 0.33974(18) 0.6164(3) 1.03957(11) 0.0325(6) Uani 1 1 d . . . C(26) C 0.29827(19) 0.7332(3) 1.01252(12) 0.0370(6) Uani 1 1 d . . . C(27) C 0.26610(19) 0.7374(3) 0.95063(13) 0.0355(6) Uani 1 1 d . . . C(28) C 0.27355(17) 0.6259(3) 0.91125(11) 0.0288(5) Uani 1 1 d . . . C(29) C 0.31688(16) 0.5095(2) 0.93781(10) 0.0252(5) Uani 1 1 d . . . C(141) C 0.43765(19) 0.4425(3) 0.69660(11) 0.0322(6) Uani 1 1 d . . . C(142) C 0.4851(5) 0.3401(5) 0.6581(3) 0.131(3) Uani 1 1 d . . . C(143) C 0.3722(4) 0.5266(8) 0.6531(3) 0.167(4) Uani 1 1 d . . . C(144) C 0.5170(4) 0.5259(7) 0.72779(18) 0.141(3) Uani 1 1 d . . . C(161) C 0.15371(19) 0.1239(3) 0.72989(11) 0.0310(5) Uani 1 1 d . . . C(162) C 0.1532(2) 0.1192(3) 0.65933(12) 0.0418(7) Uani 1 1 d . . . C(163) C 0.1733(2) -0.0198(3) 0.75486(13) 0.0401(6) Uani 1 1 d . . . C(164) C 0.05026(19) 0.1732(3) 0.74455(13) 0.0414(7) Uani 1 1 d . . . C(221) C 0.42031(19) 0.1553(3) 0.95005(12) 0.0341(6) Uani 1 1 d . . . C(251) C 0.3741(2) 0.6104(3) 1.10706(12) 0.0422(7) Uani 1 1 d . . . C(281) C 0.2339(2) 0.6400(3) 0.84492(12) 0.0378(6) Uani 1 1 d . . . H(1) H -0.0772 0.2540 0.8599 0.066 Uiso 1 1 calc R . . H(2) H -0.0945 0.1744 0.9688 0.049 Uiso 1 1 calc R . . H(3) H 0.0370 0.2870 1.0375 0.052 Uiso 1 1 calc R . . H(4) H 0.1382 0.4359 0.9716 0.070 Uiso 1 1 calc R . . H(5) H 0.0642 0.4175 0.8618 0.074 Uiso 1 1 calc R . . H(13) H 0.4310 0.4627 0.8207 0.032 Uiso 1 1 calc R . . H(15) H 0.2901 0.2670 0.6778 0.030 Uiso 1 1 calc R . . H(26) H 0.2920 0.8115 1.0372 0.044 Uiso 1 1 calc R . . H(27) H 0.2379 0.8188 0.9341 0.043 Uiso 1 1 calc R . . H(14A) H 0.5222 0.3861 0.6273 0.197 Uiso 1 1 calc R . . H(14B) H 0.4338 0.2829 0.6372 0.197 Uiso 1 1 calc R . . H(14C) H 0.5305 0.2841 0.6845 0.197 Uiso 1 1 calc R . . H(14D) H 0.3546 0.6104 0.6737 0.250 Uiso 1 1 calc R . . H(14E) H 0.3117 0.4761 0.6405 0.250 Uiso 1 1 calc R . . H(14F) H 0.4074 0.5484 0.6166 0.250 Uiso 1 1 calc R . . H(14G) H 0.5617 0.4681 0.7538 0.211 Uiso 1 1 calc R . . H(14H) H 0.4875 0.5941 0.7535 0.211 Uiso 1 1 calc R . . H(14I) H 0.5544 0.5708 0.6968 0.211 Uiso 1 1 calc R . . H(16A) H 0.1413 0.2102 0.6425 0.063 Uiso 1 1 calc R . . H(16B) H 0.1006 0.0584 0.6427 0.063 Uiso 1 1 calc R . . H(16C) H 0.2175 0.0862 0.6476 0.063 Uiso 1 1 calc R . . H(16D) H 0.2377 -0.0515 0.7428 0.060 Uiso 1 1 calc R . . H(16E) H 0.1209 -0.0805 0.7378 0.060 Uiso 1 1 calc R . . H(16F) H 0.1737 -0.0190 0.8000 0.060 Uiso 1 1 calc R . . H(16G) H 0.0456 0.1728 0.7893 0.062 Uiso 1 1 calc R . . H(16H) H -0.0004 0.1131 0.7249 0.062 Uiso 1 1 calc R . . H(16I) H 0.0397 0.2652 0.7287 0.062 Uiso 1 1 calc R . . H(22A) H 0.4050 0.1238 0.9076 0.051 Uiso 1 1 calc R . . H(22B) H 0.3897 0.0946 0.9787 0.051 Uiso 1 1 calc R . . H(22C) H 0.4924 0.1559 0.9594 0.051 Uiso 1 1 calc R . . H(23A) H 0.4616 0.3755 1.0328 0.036 Uiso 1 1 calc R . . H(23B) H 0.3534 0.3233 1.0483 0.036 Uiso 1 1 calc R . . H(25A) H 0.3791 0.5159 1.1203 0.063 Uiso 1 1 calc R . . H(25B) H 0.3263 0.6577 1.1311 0.063 Uiso 1 1 calc R . . H(25C) H 0.4392 0.6538 1.1137 0.063 Uiso 1 1 calc R . . H(28A) H 0.2881 0.6647 0.8196 0.057 Uiso 1 1 calc R . . H(28B) H 0.1829 0.7105 0.8416 0.057 Uiso 1 1 calc R . . H(28C) H 0.2049 0.5540 0.8303 0.057 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0245(2) 0.0259(2) 0.0321(2) 0.00241(18) 0.00961(17) 0.00742(17) Cl(1) 0.0384(4) 0.0372(4) 0.0478(4) -0.0110(3) 0.0113(3) 0.0048(3) Cl(2) 0.0367(3) 0.0386(4) 0.0344(3) 0.0025(3) 0.0066(3) 0.0102(3) O(1) 0.0230(8) 0.0253(9) 0.0281(8) -0.0009(7) 0.0057(6) 0.0047(6) C(1) 0.0405(17) 0.069(2) 0.0556(19) 0.0298(17) 0.0095(14) 0.0154(16) C(2) 0.0282(13) 0.0421(17) 0.0559(17) 0.0073(12) 0.0193(12) 0.0070(13) C(3) 0.0403(16) 0.0372(16) 0.0538(17) 0.0104(13) 0.0173(13) -0.0036(13) C(4) 0.0403(17) 0.0239(15) 0.115(3) 0.0028(13) 0.0350(19) -0.0041(17) C(5) 0.059(2) 0.047(2) 0.085(3) 0.0325(17) 0.044(2) 0.0378(18) C(11) 0.0203(11) 0.0228(12) 0.0249(11) 0.0024(9) 0.0066(8) 0.0049(9) C(12) 0.0239(11) 0.0225(12) 0.0244(11) 0.0018(9) 0.0029(9) 0.0033(9) C(13) 0.0266(12) 0.0258(13) 0.0268(12) -0.0054(10) 0.0014(9) 0.0010(9) C(14) 0.0270(12) 0.0255(13) 0.0243(12) -0.0025(10) 0.0022(9) 0.0055(9) C(15) 0.0294(12) 0.0240(12) 0.0221(11) -0.0010(10) 0.0021(9) 0.0025(9) C(16) 0.0230(11) 0.0222(12) 0.0279(12) 0.0007(9) 0.0016(9) 0.0030(9) C(21) 0.0231(11) 0.0280(13) 0.0245(12) -0.0012(9) 0.0037(9) 0.0020(9) C(22) 0.0245(12) 0.0305(13) 0.0270(12) 0.0020(10) 0.0049(9) 0.0035(10) C(23) 0.0265(12) 0.0393(15) 0.0240(12) 0.0008(11) 0.0017(9) 0.0041(10) C(24) 0.0202(11) 0.0330(14) 0.0280(12) -0.0019(10) 0.0029(9) -0.0003(10) C(25) 0.0251(12) 0.0405(15) 0.0324(13) -0.0038(11) 0.0041(10) -0.0061(11) C(26) 0.0329(14) 0.0364(16) 0.0416(15) 0.0001(12) 0.0025(11) -0.0115(12) C(27) 0.0320(13) 0.0280(14) 0.0463(15) 0.0024(11) 0.0021(11) -0.0013(11) C(28) 0.0231(12) 0.0309(14) 0.0325(13) -0.0011(10) 0.0016(9) 0.0026(10) C(29) 0.0214(11) 0.0279(13) 0.0268(12) -0.0030(9) 0.0041(9) 0.0004(9) C(141) 0.0350(13) 0.0368(15) 0.0252(12) -0.0121(11) 0.0045(10) 0.0076(10) C(142) 0.193(6) 0.078(3) 0.143(5) -0.060(4) 0.144(5) -0.039(3) C(143) 0.070(3) 0.223(7) 0.212(7) 0.022(4) 0.044(4) 0.195(6) C(144) 0.150(5) 0.235(7) 0.041(2) -0.165(5) 0.032(2) -0.022(3) C(161) 0.0315(13) 0.0296(14) 0.0316(13) -0.0108(11) 0.0008(10) 0.0005(10) C(162) 0.0461(16) 0.0455(17) 0.0332(14) -0.0180(14) -0.0002(12) -0.0033(12) C(163) 0.0495(17) 0.0275(15) 0.0439(15) -0.0111(12) 0.0067(12) -0.0020(11) C(164) 0.0274(13) 0.0533(19) 0.0428(15) -0.0077(13) -0.0012(11) 0.0009(13) C(221) 0.0327(13) 0.0349(15) 0.0353(14) 0.0088(11) 0.0070(10) 0.0053(11) C(251) 0.0431(16) 0.0507(18) 0.0326(14) -0.0064(14) 0.0018(11) -0.0085(12) C(281) 0.0402(15) 0.0331(15) 0.0390(15) 0.0063(12) -0.0040(11) 0.0064(11) # 10. 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_publ_flag Ti O(1) 1.7885(15) YES Ti Cl(2) 2.2597(8) YES Ti Cl(1) 2.2634(8) YES Ti C(5) 2.311(3) YES Ti C(1) 2.324(3) YES Ti C(4) 2.333(3) YES Ti C(2) 2.372(2) YES Ti C(3) 2.378(3) YES O(1) C(11) 1.376(3) YES C(1) C(5) 1.389(5) YES C(1) C(2) 1.407(4) YES C(2) C(3) 1.380(4) YES C(3) C(4) 1.410(4) YES C(4) C(5) 1.401(6) YES C(11) C(12) 1.401(3) YES C(11) C(16) 1.416(3) YES C(12) C(13) 1.399(3) YES C(12) C(21) 1.485(3) YES C(13) C(14) 1.385(3) YES C(14) C(15) 1.394(3) YES C(14) C(141) 1.533(3) YES C(15) C(16) 1.396(3) YES C(16) C(161) 1.536(3) YES C(21) C(22) 1.350(3) YES C(21) C(29) 1.484(3) YES C(22) C(221) 1.489(4) YES C(22) C(23) 1.501(3) YES C(23) C(24) 1.506(4) YES C(24) C(25) 1.383(4) YES C(24) C(29) 1.412(3) YES C(25) C(26) 1.395(4) YES C(25) C(251) 1.505(4) YES C(26) C(27) 1.382(4) YES C(27) C(28) 1.405(4) YES C(28) C(29) 1.397(3) YES C(28) C(281) 1.506(4) YES C(141) C(144) 1.476(4) YES C(141) C(142) 1.490(5) YES C(141) C(143) 1.498(5) YES C(161) C(162) 1.534(4) YES C(161) C(164) 1.538(4) YES C(161) C(163) 1.538(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ti Cl(2) 107.43(6) YES O(1) Ti Cl(1) 101.97(6) YES Cl(2) Ti Cl(1) 100.80(3) YES O(1) Ti C(5) 87.84(9) YES Cl(2) Ti C(5) 130.98(12) YES Cl(1) Ti C(5) 121.68(12) YES O(1) Ti C(1) 108.52(10) YES Cl(2) Ti C(1) 139.51(9) YES Cl(1) Ti C(1) 89.40(11) YES C(5) Ti C(1) 34.87(13) YES O(1) Ti C(4) 103.24(10) YES Cl(2) Ti C(4) 95.98(11) YES Cl(1) Ti C(4) 143.77(9) YES C(5) Ti C(4) 35.12(14) YES C(1) Ti C(4) 58.04(14) YES O(1) Ti C(2) 142.89(9) YES Cl(2) Ti C(2) 106.06(8) YES Cl(1) Ti C(2) 86.92(8) YES C(5) Ti C(2) 57.81(10) YES C(1) Ti C(2) 34.85(10) YES C(4) Ti C(2) 57.51(11) YES O(1) Ti C(3) 138.05(9) YES Cl(2) Ti C(3) 83.40(8) YES Cl(1) Ti C(3) 115.92(8) YES C(5) Ti C(3) 57.76(12) YES C(1) Ti C(3) 57.29(12) YES C(4) Ti C(3) 34.82(11) YES C(2) Ti C(3) 33.79(11) YES C(11) O(1) Ti 159.93(15) YES C(5) C(1) C(2) 108.2(3) YES C(5) C(1) Ti 72.06(17) YES C(2) C(1) Ti 74.44(16) YES C(3) C(2) C(1) 107.9(3) YES C(3) C(2) Ti 73.35(15) YES C(1) C(2) Ti 70.70(15) YES C(2) C(3) C(4) 108.4(3) YES C(2) C(3) Ti 72.86(16) YES C(4) C(3) Ti 70.85(17) YES C(5) C(4) C(3) 107.4(3) YES C(5) C(4) Ti 71.57(19) YES C(3) C(4) Ti 74.33(17) YES C(1) C(5) C(4) 108.1(3) YES C(1) C(5) Ti 73.07(18) YES C(4) C(5) Ti 73.31(18) YES O(1) C(11) C(12) 117.71(19) YES O(1) C(11) C(16) 121.3(2) YES C(12) C(11) C(16) 120.9(2) YES C(13) C(12) C(11) 119.2(2) YES C(13) C(12) C(21) 117.6(2) YES C(11) C(12) C(21) 123.2(2) YES C(14) C(13) C(12) 121.9(2) YES C(13) C(14) C(15) 117.1(2) YES C(13) C(14) C(141) 122.7(2) YES C(15) C(14) C(141) 120.2(2) YES C(14) C(15) C(16) 124.3(2) YES C(15) C(16) C(11) 116.5(2) YES C(15) C(16) C(161) 119.7(2) YES C(11) C(16) C(161) 123.8(2) YES C(22) C(21) C(29) 109.9(2) YES C(22) C(21) C(12) 125.5(2) YES C(29) C(21) C(12) 124.3(2) YES C(21) C(22) C(221) 127.8(2) YES C(21) C(22) C(23) 110.3(2) YES C(221) C(22) C(23) 121.8(2) YES C(22) C(23) C(24) 103.54(19) YES C(25) C(24) C(29) 122.4(2) YES C(25) C(24) C(23) 128.6(2) YES C(29) C(24) C(23) 109.0(2) YES C(24) C(25) C(26) 116.8(2) YES C(24) C(25) C(251) 121.4(3) YES C(26) C(25) C(251) 121.8(2) YES C(27) C(26) C(25) 121.4(2) YES C(26) C(27) C(28) 122.5(3) YES C(29) C(28) C(27) 116.3(2) YES C(29) C(28) C(281) 125.4(2) YES C(27) C(28) C(281) 118.3(2) YES C(28) C(29) C(24) 120.6(2) YES C(28) C(29) C(21) 132.2(2) YES C(24) C(29) C(21) 107.2(2) YES C(144) C(141) C(142) 108.0(4) YES C(144) C(141) C(143) 110.7(5) YES C(142) C(141) C(143) 106.4(5) YES C(144) C(141) C(14) 112.6(2) YES C(142) C(141) C(14) 110.9(2) YES C(143) C(141) C(14) 108.2(2) YES C(162) C(161) C(16) 112.0(2) YES C(162) C(161) C(164) 106.4(2) YES C(16) C(161) C(164) 110.1(2) YES C(162) C(161) C(163) 108.2(2) YES C(16) C(161) C(163) 109.3(2) YES C(164) C(161) C(163) 110.8(2) YES data_MT42H _database_code_CSD 218467 _audit_creation_date 26-09-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description cube _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C61 H75 Cl2 O2 Ti2' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 1006.98 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2296(8) _cell_length_b 10.7280(10) _cell_length_c 13.6638(14) _cell_angle_alpha 102.861(5) _cell_angle_beta 102.520(5) _cell_angle_gamma 96.692(6) _cell_volume 1405.6(5) _cell_measurement_reflns_used 12936 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 1 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.415 _cell_measurement_temperature 203 _exptl_crystal_F_000 536 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.7950 _exptl_absorpt_correction_T_max 0.8922 _diffrn_reflns_number 12936 _reflns_number_total 0 _reflns_number_gt 0 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 16 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.00' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.099 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_ref 0.000 _refine_ls_wR_factor_gt 0.192 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6199 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+1.5334P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.64 _refine_diff_density_min -0.74 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.67E-01 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.09861(6) -0.35854(6) -0.49859(5) 0.0364(2) Uani 1 1 d . . . Cl Cl 0.05900(8) -0.58143(8) -0.59985(7) 0.0421(3) Uani 1 1 d . . . O(1) O 0.2629(2) -0.3384(2) -0.40762(18) 0.0373(5) Uani 1 1 d . . . C(1) C 0.1715(4) -0.1733(4) -0.5459(3) 0.0519(9) Uani 1 1 d . . . C(2) C 0.0722(5) -0.1436(4) -0.4942(4) 0.0562(10) Uani 1 1 d . . . C(3) C -0.0503(4) -0.2182(5) -0.5540(4) 0.0634(12) Uani 1 1 d . . . C(4) C -0.0266(5) -0.2972(4) -0.6420(4) 0.0639(13) Uani 1 1 d . . . C(5) C 0.1129(5) -0.2690(4) -0.6371(3) 0.0545(10) Uani 1 1 d . . . C(11) C 0.3938(3) -0.2799(3) -0.3594(3) 0.0353(7) Uani 1 1 d . . . C(12) C 0.4870(3) -0.2662(3) -0.4194(3) 0.0360(7) Uani 1 1 d . . . C(13) C 0.6198(3) -0.1995(3) -0.3702(3) 0.0382(7) Uani 1 1 d . . . C(14) C 0.6619(3) -0.1474(3) -0.2644(3) 0.0377(7) Uani 1 1 d . . . C(15) C 0.5673(3) -0.1675(3) -0.2067(3) 0.0385(7) Uani 1 1 d . . . C(16) C 0.4348(3) -0.2329(3) -0.2495(3) 0.0371(7) Uani 1 1 d . . . C(121) C 0.4527(3) -0.3236(3) -0.5328(3) 0.0348(7) Uani 1 1 d . . . C(122) C 0.3888(3) -0.4455(3) -0.5845(3) 0.0399(7) Uani 1 1 d . . . C(123) C 0.3820(4) -0.4723(4) -0.6982(3) 0.0441(8) Uani 1 1 d . . . C(124) C 0.4525(4) -0.3450(4) -0.7071(3) 0.0432(8) Uani 1 1 d . . . C(125) C 0.4784(4) -0.3080(4) -0.7925(3) 0.0548(10) Uani 1 1 d . . . C(126) C 0.5437(5) -0.1822(5) -0.7794(3) 0.0611(11) Uani 1 1 d . . . C(127) C 0.5823(4) -0.0951(4) -0.6832(3) 0.0552(10) Uani 1 1 d . . . C(128) C 0.5574(4) -0.1317(4) -0.5964(3) 0.0454(8) Uani 1 1 d . . . C(129) C 0.4930(3) -0.2578(3) -0.6085(3) 0.0377(7) Uani 1 1 d . . . C(141) C 0.8047(3) -0.0703(4) -0.2083(3) 0.0436(8) Uani 1 1 d . . . C(142) C 0.8939(3) -0.0591(4) -0.2834(3) 0.0479(9) Uani 1 1 d . . . C(143) C 0.8743(4) -0.1398(6) -0.1297(4) 0.0705(14) Uani 1 1 d . . . C(144) C 0.7931(5) 0.0675(5) -0.1535(5) 0.0790(16) Uani 1 1 d . . . C(161) C 0.3385(3) -0.2542(4) -0.1799(3) 0.0430(8) Uani 1 1 d . . . C(162) C 0.4128(4) -0.2124(5) -0.0645(3) 0.0581(11) Uani 1 1 d . . . C(163) C 0.2250(4) -0.1740(4) -0.1969(3) 0.0543(10) Uani 1 1 d . . . C(164) C 0.2790(4) -0.3992(4) -0.2040(3) 0.0528(10) Uani 1 1 d . . . C(901) C 0.779(3) 0.623(2) 0.0227(19) 0.173(8) Uiso 0.50 1 d P . . C(902) C 0.8914(18) 0.5975(16) 0.0288(13) 0.216(6) Uiso 1 1 d . . . C(903) C 0.9290(17) 0.492(2) -0.0262(18) 0.289(10) Uiso 1 1 d . . . H(1) H 0.2628 -0.1352 -0.5232 0.067 Uiso 1 1 calc R . . H(2) H 0.0856 -0.0841 -0.4304 0.073 Uiso 1 1 calc R . . H(3) H -0.1341 -0.2161 -0.5382 0.082 Uiso 1 1 calc R . . H(4) H -0.0915 -0.3577 -0.6947 0.083 Uiso 1 1 calc R . . H(5) H 0.1572 -0.3071 -0.6856 0.071 Uiso 1 1 calc R . . H(13) H 0.6813 -0.1902 -0.4103 0.050 Uiso 1 1 calc R . . H(15) H 0.5951 -0.1348 -0.1351 0.050 Uiso 1 1 calc R . . H(122) H 0.3533 -0.5056 -0.5533 0.052 Uiso 1 1 calc R . . H(125) H 0.4526 -0.3662 -0.8577 0.071 Uiso 1 1 calc R . . H(126) H 0.5617 -0.1564 -0.8365 0.079 Uiso 1 1 calc R . . H(127) H 0.6254 -0.0111 -0.6761 0.072 Uiso 1 1 calc R . . H(128) H 0.5834 -0.0729 -0.5314 0.059 Uiso 1 1 calc R . . H(12A) H 0.2886 -0.4935 -0.7395 0.057 Uiso 1 1 calc R . . H(12B) H 0.4295 -0.5427 -0.7197 0.057 Uiso 1 1 calc R . . H(14A) H 0.9089 -0.1438 -0.3148 0.062 Uiso 1 1 calc R . . H(14B) H 0.9795 -0.0048 -0.2462 0.062 Uiso 1 1 calc R . . H(14C) H 0.8492 -0.0215 -0.3362 0.062 Uiso 1 1 calc R . . H(14D) H 0.8232 -0.1428 -0.0789 0.092 Uiso 1 1 calc R . . H(14E) H 0.9648 -0.0933 -0.0960 0.092 Uiso 1 1 calc R . . H(14F) H 0.8786 -0.2266 -0.1652 0.092 Uiso 1 1 calc R . . H(14G) H 0.7488 0.1090 -0.2036 0.103 Uiso 1 1 calc R . . H(14H) H 0.8824 0.1163 -0.1191 0.103 Uiso 1 1 calc R . . H(14I) H 0.7410 0.0635 -0.1034 0.103 Uiso 1 1 calc R . . H(16A) H 0.3500 -0.2285 -0.0239 0.076 Uiso 1 1 calc R . . H(16B) H 0.4500 -0.1215 -0.0454 0.076 Uiso 1 1 calc R . . H(16C) H 0.4850 -0.2611 -0.0519 0.076 Uiso 1 1 calc R . . H(16D) H 0.1646 -0.1880 -0.1540 0.071 Uiso 1 1 calc R . . H(16E) H 0.1753 -0.2001 -0.2684 0.071 Uiso 1 1 calc R . . H(16F) H 0.2641 -0.0836 -0.1788 0.071 Uiso 1 1 calc R . . H(16G) H 0.3514 -0.4473 -0.1902 0.069 Uiso 1 1 calc R . . H(16H) H 0.2306 -0.4297 -0.2758 0.069 Uiso 1 1 calc R . . H(16I) H 0.2180 -0.4113 -0.1613 0.069 Uiso 1 1 calc R . . H(90A) H 0.9263 0.5988 0.1010 0.281 Uiso 1 1 calc R . . H(90B) H 0.9444 0.6718 0.0176 0.281 Uiso 1 1 calc R . . H(90C) H 0.9174 0.4936 -0.0983 0.376 Uiso 1 1 calc R . . H(90D) H 0.8777 0.4122 -0.0225 0.376 Uiso 1 1 calc R . . H(90E) H 0.7416 0.6308 -0.0460 0.224 Uiso 0.50 1 calc PR . . H(90F) H 0.7838 0.7036 0.0721 0.224 Uiso 0.50 1 calc PR . . H(90G) H 0.7225 0.5551 0.0372 0.224 Uiso 0.50 1 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0308(3) 0.0359(4) 0.0415(4) 0.0018(2) 0.0065(2) 0.0124(3) Cl 0.0365(4) 0.0395(5) 0.0484(5) -0.0003(3) 0.0129(3) 0.0088(4) O1 0.0317(11) 0.0387(12) 0.0413(13) 0.0025(9) 0.0093(9) 0.0118(10) C1 0.049(2) 0.045(2) 0.065(3) 0.0011(17) 0.0120(18) 0.0270(19) C2 0.072(3) 0.041(2) 0.063(3) 0.0172(19) 0.021(2) 0.0186(18) C3 0.048(2) 0.072(3) 0.092(3) 0.027(2) 0.026(2) 0.048(3) C4 0.065(3) 0.050(2) 0.066(3) -0.005(2) -0.015(2) 0.031(2) C5 0.071(3) 0.052(2) 0.049(2) 0.014(2) 0.0202(19) 0.0234(18) C11 0.0279(14) 0.0348(16) 0.0434(18) 0.0021(12) 0.0081(12) 0.0130(14) C12 0.0320(15) 0.0370(17) 0.0394(17) 0.0056(13) 0.0077(13) 0.0120(13) C13 0.0311(15) 0.0420(18) 0.0413(18) 0.0024(13) 0.0102(13) 0.0113(14) C14 0.0296(15) 0.0397(17) 0.0431(18) 0.0026(13) 0.0090(13) 0.0109(14) C15 0.0355(16) 0.0433(18) 0.0342(17) 0.0020(14) 0.0069(13) 0.0091(14) C16 0.0347(16) 0.0393(17) 0.0392(17) 0.0055(13) 0.0107(13) 0.0130(14) C121 0.0283(14) 0.0356(16) 0.0410(17) 0.0046(12) 0.0081(12) 0.0118(13) C122 0.0353(16) 0.0435(19) 0.0411(18) 0.0049(14) 0.0087(13) 0.0131(15) C123 0.0456(19) 0.0407(19) 0.0423(19) 0.0075(15) 0.0083(15) 0.0053(15) C124 0.0450(19) 0.0443(19) 0.0398(18) 0.0087(15) 0.0102(14) 0.0094(15) C125 0.067(3) 0.059(2) 0.038(2) 0.010(2) 0.0136(17) 0.0110(17) C126 0.073(3) 0.066(3) 0.047(2) 0.002(2) 0.018(2) 0.024(2) C127 0.063(2) 0.052(2) 0.053(2) 0.0004(19) 0.0157(19) 0.0214(19) C128 0.0471(19) 0.045(2) 0.0422(19) 0.0029(16) 0.0100(15) 0.0108(15) C129 0.0343(16) 0.0412(18) 0.0386(17) 0.0056(14) 0.0097(13) 0.0123(14) C141 0.0309(16) 0.050(2) 0.0433(19) 0.0003(14) 0.0074(13) 0.0027(15) C142 0.0309(16) 0.054(2) 0.053(2) -0.0030(15) 0.0073(15) 0.0122(17) C143 0.036(2) 0.115(4) 0.055(3) 0.000(2) 0.0011(17) 0.027(3) C144 0.049(2) 0.064(3) 0.101(4) -0.010(2) 0.025(2) -0.022(3) C161 0.0366(17) 0.052(2) 0.0393(18) 0.0017(15) 0.0108(14) 0.0113(15) C162 0.054(2) 0.079(3) 0.039(2) -0.002(2) 0.0165(17) 0.0128(19) C163 0.043(2) 0.063(3) 0.061(2) 0.0110(18) 0.0221(18) 0.013(2) C164 0.051(2) 0.057(2) 0.052(2) -0.0024(18) 0.0159(17) 0.0211(19) # 10. 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 Ti O(1) 1.819(2) . ? Ti C(1) 2.315(4) . ? Ti C(5) 2.329(4) . ? Ti C(2) 2.342(4) . ? Ti C(4) 2.366(4) . ? Ti C(3) 2.388(4) . ? Ti Cl 2.4196(10) . ? Ti Cl 2.4304(10) 2_544 ? Cl Ti 2.4304(10) 2_544 ? O(1) C(11) 1.363(4) . ? C(1) C(2) 1.385(6) . ? C(1) C(5) 1.389(6) . ? C(2) C(3) 1.382(7) . ? C(3) C(4) 1.395(7) . ? C(4) C(5) 1.408(6) . ? C(11) C(12) 1.402(5) . ? C(11) C(16) 1.423(5) . ? C(12) C(13) 1.405(4) . ? C(12) C(121) 1.480(5) . ? C(13) C(14) 1.379(5) . ? C(14) C(15) 1.401(5) . ? C(14) C(141) 1.535(4) . ? C(15) C(16) 1.386(5) . ? C(16) C(161) 1.541(5) . ? C(121) C(122) 1.351(5) . ? C(121) C(129) 1.477(5) . ? C(122) C(123) 1.501(5) . ? C(123) C(124) 1.510(5) . ? C(124) C(125) 1.381(5) . ? C(124) C(129) 1.403(5) . ? C(125) C(126) 1.389(6) . ? C(126) C(127) 1.379(6) . ? C(127) C(128) 1.393(5) . ? C(128) C(129) 1.392(5) . ? C(141) C(142) 1.528(5) . ? C(141) C(144) 1.532(6) . ? C(141) C(143) 1.538(6) . ? C(161) C(163) 1.532(5) . ? C(161) C(162) 1.533(5) . ? C(161) C(164) 1.537(5) . ? C(902) C(901) 1.20(2) . ? C(902) C(903) 1.35(2) . ? C(903) C(903) 1.45(3) 2_765 ? 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 O(1) Ti C(1) 90.19(13) . . ? O(1) Ti C(5) 112.44(14) . . ? C(1) Ti C(5) 34.81(15) . . ? O(1) Ti C(2) 102.43(14) . . ? C(1) Ti C(2) 34.61(15) . . ? C(5) Ti C(2) 57.90(15) . . ? O(1) Ti C(4) 146.13(14) . . ? C(1) Ti C(4) 57.30(15) . . ? C(5) Ti C(4) 34.87(16) . . ? C(2) Ti C(4) 57.09(16) . . ? O(1) Ti C(3) 136.06(15) . . ? C(1) Ti C(3) 56.78(15) . . ? C(5) Ti C(3) 57.39(16) . . ? C(2) Ti C(3) 33.95(16) . . ? C(4) Ti C(3) 34.11(17) . . ? O(1) Ti Cl 104.43(8) . . ? C(1) Ti Cl 127.67(12) . . ? C(5) Ti Cl 94.94(11) . . ? C(2) Ti Cl 147.67(12) . . ? C(4) Ti Cl 90.67(12) . . ? C(3) Ti Cl 118.45(14) . . ? O(1) Ti Cl 102.45(8) . 2_544 ? C(1) Ti Cl 136.08(11) . 2_544 ? C(5) Ti Cl 142.18(12) . 2_544 ? C(2) Ti Cl 101.52(11) . 2_544 ? C(4) Ti Cl 107.78(13) . 2_544 ? C(3) Ti Cl 87.45(11) . 2_544 ? Cl Ti Cl 89.96(3) . 2_544 ? Ti Cl Ti 90.04(3) . 2_544 ? C(11) O(1) Ti 154.7(2) . . ? C(2) C(1) C(5) 109.1(4) . . ? C(2) C(1) Ti 73.7(2) . . ? C(5) C(1) Ti 73.1(2) . . ? C(3) C(2) C(1) 107.9(4) . . ? C(3) C(2) Ti 74.9(2) . . ? C(1) C(2) Ti 71.7(2) . . ? C(2) C(3) C(4) 108.3(4) . . ? C(2) C(3) Ti 71.2(2) . . ? C(4) C(3) Ti 72.1(2) . . ? C(3) C(4) C(5) 107.9(4) . . ? C(3) C(4) Ti 73.8(2) . . ? C(5) C(4) Ti 71.1(2) . . ? C(1) C(5) C(4) 106.8(4) . . ? C(1) C(5) Ti 72.0(2) . . ? C(4) C(5) Ti 74.0(2) . . ? O(1) C(11) C(12) 119.1(3) . . ? O(1) C(11) C(16) 120.3(3) . . ? C(12) C(11) C(16) 120.5(3) . . ? C(11) C(12) C(13) 119.1(3) . . ? C(11) C(12) C(121) 122.5(3) . . ? C(13) C(12) C(121) 118.3(3) . . ? C(14) C(13) C(12) 122.1(3) . . ? C(13) C(14) C(15) 117.0(3) . . ? C(13) C(14) C(141) 123.6(3) . . ? C(15) C(14) C(141) 119.4(3) . . ? C(16) C(15) C(14) 124.2(3) . . ? C(15) C(16) C(11) 116.9(3) . . ? C(15) C(16) C(161) 120.9(3) . . ? C(11) C(16) C(161) 122.3(3) . . ? C(122) C(121) C(129) 108.1(3) . . ? C(122) C(121) C(12) 127.2(3) . . ? C(129) C(121) C(12) 124.6(3) . . ? C(121) C(122) C(123) 112.0(3) . . ? C(122) C(123) C(124) 102.4(3) . . ? C(125) C(124) C(129) 120.6(4) . . ? C(125) C(124) C(123) 130.5(3) . . ? C(129) C(124) C(123) 108.9(3) . . ? C(124) C(125) C(126) 118.8(4) . . ? C(127) C(126) C(125) 121.0(4) . . ? C(126) C(127) C(128) 120.6(4) . . ? C(129) C(128) C(127) 118.9(4) . . ? C(128) C(129) C(124) 120.0(3) . . ? C(128) C(129) C(121) 131.2(3) . . ? C(124) C(129) C(121) 108.7(3) . . ? C(142) C(141) C(144) 107.7(4) . . ? C(142) C(141) C(14) 112.0(3) . . ? C(144) C(141) C(14) 109.3(3) . . ? C(142) C(141) C(143) 108.0(3) . . ? C(144) C(141) C(143) 110.7(4) . . ? C(14) C(141) C(143) 109.2(3) . . ? C(163) C(161) C(162) 107.9(3) . . ? C(163) C(161) C(164) 110.8(3) . . ? C(162) C(161) C(164) 106.5(3) . . ? C(163) C(161) C(16) 109.5(3) . . ? C(162) C(161) C(16) 112.0(3) . . ? C(164) C(161) C(16) 110.1(3) . . ? C(901) C(902) C(903) 128(2) . . ? C(902) C(903) C(903) 102(3) . 2_765 ? #============================================================================== data_LTP34A _database_code_CSD 218468 #============================================================================== _audit_creation_date 10-08-00 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C28 H31 Cl1 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 466.91 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5121(4) _cell_length_b 14.3700(5) _cell_length_c 18.6606(7) _cell_angle_alpha 80.576(2) _cell_angle_beta 84.7992(19) _cell_angle_gamma 86.5059(12) _cell_volume 2503.2(3) _cell_measurement_reflns_used 14089 _cell_measurement_theta_min 5 _cell_measurement_theta_max 23 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.461 _cell_measurement_temperature 150 _exptl_crystal_F_000 984 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.3090 _exptl_absorpt_correction_T_max 0.9440 _diffrn_reflns_number 14089 _reflns_number_total 6962 _reflns_number_gt 5754 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 23.34 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 20 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.112 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6353 _refine_ls_d_res_high 0.93 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+3.1992P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.59 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ti(1) 0.06615(9) 1.20450(6) 0.36007(4) 0.0297(3) Uani ? Ti(2) 0.59519(8) 0.72031(5) 0.38848(4) 0.0273(3) Uani ? Cl(1) 0.20836(13) 1.08852(8) 0.42997(6) 0.0376(4) Uani ? Cl(2) 0.71167(13) 0.57739(8) 0.44182(6) 0.0396(4) Uani ? O(1) 0.0798(3) 1.13507(19) 0.28022(14) 0.0294(9) Uani ? O(2) 0.5449(3) 0.67205(19) 0.30539(14) 0.0300(9) Uani ? C(11) 0.1887(5) 1.1384(3) 0.2276(2) 0.0251(14) Uani ? C(12) 0.2776(5) 1.2137(3) 0.2209(2) 0.0269(16) Uani ? C(13) 0.3898(5) 1.2243(3) 0.1677(2) 0.0329(16) Uani ? C(14) 0.4180(5) 1.1586(3) 0.1212(2) 0.0326(16) Uani ? C(15) 0.3293(5) 1.0831(3) 0.1301(2) 0.0327(16) Uani ? C(16) 0.2138(5) 1.0690(3) 0.1824(2) 0.0283(14) Uani ? C(21) 0.6231(5) 0.6715(3) 0.2410(2) 0.0270(14) Uani ? C(22) 0.7416(5) 0.7269(3) 0.2292(2) 0.0260(14) Uani ? C(23) 0.8303(5) 0.7283(3) 0.1663(2) 0.0298(16) Uani ? C(24) 0.8019(5) 0.6760(3) 0.1131(2) 0.0315(16) Uani ? C(25) 0.6822(5) 0.6237(3) 0.1260(2) 0.0319(14) Uani ? C(26) 0.5886(5) 0.6185(3) 0.1886(2) 0.0265(14) Uani ? C(111) -0.1716(5) 1.1674(4) 0.3563(3) 0.0410(18) Uani ? C(112) -0.1691(5) 1.2608(4) 0.3696(3) 0.0463(19) Uani ? C(113) -0.1210(5) 1.2573(4) 0.4386(3) 0.0509(18) Uani ? C(114) -0.0917(5) 1.1636(4) 0.4668(3) 0.0494(19) Uani ? C(115) -0.1219(5) 1.1080(4) 0.4156(3) 0.0441(16) Uani ? C(121) 0.2366(5) 1.2772(3) 0.2750(2) 0.0280(16) Uani ? C(122) 0.2868(5) 1.2756(3) 0.3435(2) 0.0297(16) Uani ? C(123) 0.1976(5) 1.3316(3) 0.3843(2) 0.0386(16) Uani ? C(124) 0.0964(5) 1.3798(3) 0.3376(2) 0.0365(16) Uani ? C(125) -0.0088(6) 1.4525(4) 0.3458(3) 0.0514(19) Uani ? C(126) -0.0891(6) 1.4839(4) 0.2897(3) 0.063(2) Uani ? C(127) -0.0735(6) 1.4443(4) 0.2247(3) 0.061(2) Uani ? C(128) 0.0255(6) 1.3742(3) 0.2145(3) 0.0446(17) Uani ? C(129) 0.1165(5) 1.3430(3) 0.2713(2) 0.0334(16) Uani ? C(141) 0.5435(6) 1.1664(4) 0.0631(3) 0.0504(19) Uani ? C(142) 0.6428(6) 1.0822(5) 0.0775(3) 0.085(2) Uani ? C(143) 0.4894(7) 1.1629(5) -0.0136(3) 0.091(3) Uani ? C(144) 0.6108(10) 1.2570(6) 0.0536(6) 0.190(5) Uani ? C(161) 0.1236(5) 0.9826(3) 0.1919(2) 0.0358(16) Uani ? C(162) 0.1321(6) 0.9277(3) 0.2694(3) 0.0481(18) Uani ? C(163) 0.1750(6) 0.9148(4) 0.1389(3) 0.059(2) Uani ? C(164) -0.0312(5) 1.0137(4) 0.1797(3) 0.0493(18) Uani ? C(211) 0.3434(5) 0.7317(3) 0.4045(3) 0.0360(16) Uani ? C(212) 0.3966(5) 0.8125(3) 0.4239(2) 0.0347(16) Uani ? C(213) 0.4687(5) 0.7835(3) 0.4869(2) 0.0367(16) Uani ? C(214) 0.4614(5) 0.6860(4) 0.5056(2) 0.0411(18) Uani ? C(215) 0.3868(5) 0.6532(3) 0.4536(3) 0.0385(16) Uani ? C(221) 0.7586(4) 0.7776(3) 0.2902(2) 0.0244(16) Uani ? C(222) 0.8350(4) 0.7484(3) 0.3511(2) 0.0283(16) Uani ? C(223) 0.7927(5) 0.8055(3) 0.4053(2) 0.0308(16) Uani ? C(224) 0.6979(5) 0.8783(3) 0.3746(2) 0.0277(16) Uani ? C(225) 0.6340(5) 0.9608(3) 0.3993(3) 0.0347(16) Uani ? C(226) 0.5509(5) 1.0191(3) 0.3547(3) 0.0395(16) Uani ? C(227) 0.5212(5) 0.9992(3) 0.2861(3) 0.0386(16) Uani ? C(228) 0.5784(5) 0.9200(3) 0.2613(2) 0.0326(16) Uani ? C(229) 0.6715(5) 0.8591(3) 0.3042(2) 0.0259(16) Uani ? C(241) 0.9066(5) 0.6749(4) 0.0449(2) 0.0423(18) Uani ? C(242) 1.0525(5) 0.6380(4) 0.0687(3) 0.0507(19) Uani ? C(243) 0.8593(6) 0.6104(5) -0.0061(3) 0.068(2) Uani ? C(244) 0.9189(6) 0.7745(4) 0.0025(3) 0.064(2) Uani ? C(261) 0.4613(5) 0.5574(3) 0.2015(2) 0.0396(16) Uani ? C(262) 0.3258(5) 0.6182(4) 0.2141(3) 0.0566(19) Uani ? C(263) 0.4790(6) 0.4808(3) 0.2686(3) 0.057(2) Uani ? C(264) 0.4421(6) 0.5065(4) 0.1368(3) 0.0560(19) Uani ? H(13) 0.4463 1.2759 0.1634 0.0430 Uiso calc H(15) 0.3482 1.0387 0.0991 0.0420 Uiso calc H(23) 0.9097 0.7645 0.1593 0.0390 Uiso calc H(25) 0.6625 0.5893 0.0903 0.0410 Uiso calc H(111) -0.2015 1.1488 0.3149 0.0530 Uiso calc H(112) -0.1948 1.3150 0.3381 0.0600 Uiso calc H(113) -0.1105 1.3089 0.4615 0.0660 Uiso calc H(114) -0.0578 1.1414 0.5120 0.0640 Uiso calc H(115) -0.1106 1.0426 0.4206 0.0570 Uiso calc H(122) 0.3678 1.2421 0.3595 0.0390 Uiso calc H(123) 0.2030 1.3367 0.4330 0.0500 Uiso calc H(125) -0.0223 1.4780 0.3887 0.0670 Uiso calc H(126) -0.1564 1.5328 0.2940 0.0830 Uiso calc H(127) -0.1325 1.4667 0.1879 0.0790 Uiso calc H(128) 0.0335 1.3476 0.1720 0.0580 Uiso calc H(14A) 0.7202 1.0868 0.0405 0.1110 Uiso calc H(14B) 0.5938 1.0259 0.0768 0.1110 Uiso calc H(14C) 0.6781 1.0796 0.1244 0.1110 Uiso calc H(14D) 0.5678 1.1686 -0.0501 0.1180 Uiso calc H(14E) 0.4213 1.2140 -0.0250 0.1180 Uiso calc H(14F) 0.4464 1.1039 -0.0126 0.1180 Uiso calc H(14G) 0.6643 1.2591 0.0945 0.2470 Uiso calc H(14H) 0.5396 1.3075 0.0504 0.2470 Uiso calc H(14I) 0.6728 1.2640 0.0097 0.2470 Uiso calc H(16A) 0.2282 0.9063 0.2764 0.0630 Uiso calc H(16B) 0.0736 0.8744 0.2760 0.0630 Uiso calc H(16C) 0.0999 0.9683 0.3042 0.0630 Uiso calc H(16D) 0.1648 0.9456 0.0898 0.0770 Uiso calc H(16E) 0.1199 0.8597 0.1490 0.0770 Uiso calc H(16F) 0.2727 0.8966 0.1445 0.0770 Uiso calc H(16G) -0.0655 1.0556 0.2132 0.0640 Uiso calc H(16H) -0.0875 0.9592 0.1878 0.0640 Uiso calc H(16I) -0.0371 1.0457 0.1307 0.0640 Uiso calc H(211) 0.2888 0.7306 0.3658 0.0470 Uiso calc H(212) 0.3861 0.8740 0.3994 0.0450 Uiso calc H(213) 0.5135 0.8227 0.5117 0.0480 Uiso calc H(214) 0.4993 0.6489 0.5455 0.0540 Uiso calc H(215) 0.3695 0.5906 0.4522 0.0500 Uiso calc H(222) 0.9033 0.6991 0.3554 0.0370 Uiso calc H(223) 0.8217 0.7968 0.4523 0.0400 Uiso calc H(225) 0.6491 0.9742 0.4450 0.0450 Uiso calc H(226) 0.5118 1.0743 0.3698 0.0510 Uiso calc H(227) 0.4619 1.0405 0.2575 0.0500 Uiso calc H(228) 0.5565 0.9062 0.2167 0.0420 Uiso calc H(24A) 1.1175 0.6362 0.0265 0.0660 Uiso calc H(24B) 1.0456 0.5755 0.0961 0.0660 Uiso calc H(24C) 1.0857 0.6791 0.0986 0.0660 Uiso calc H(24D) 0.9272 0.6107 -0.0474 0.0880 Uiso calc H(24E) 0.7687 0.6332 -0.0223 0.0880 Uiso calc H(24F) 0.8525 0.5471 0.0199 0.0880 Uiso calc H(24G) 0.9468 0.8156 0.0339 0.0830 Uiso calc H(24H) 0.8293 0.7970 -0.0151 0.0830 Uiso calc H(24I) 0.9886 0.7738 -0.0380 0.0830 Uiso calc H(26A) 0.3299 0.6454 0.2575 0.0740 Uiso calc H(26B) 0.2455 0.5796 0.2196 0.0740 Uiso calc H(26C) 0.3173 0.6677 0.1732 0.0740 Uiso calc H(26D) 0.5614 0.4410 0.2597 0.0750 Uiso calc H(26E) 0.3971 0.4434 0.2778 0.0750 Uiso calc H(26F) 0.4897 0.5103 0.3103 0.0750 Uiso calc H(26G) 0.4319 0.5523 0.0938 0.0730 Uiso calc H(26H) 0.3590 0.4703 0.1473 0.0730 Uiso calc H(26I) 0.5232 0.4652 0.1291 0.0730 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0263(5) 0.0304(5) 0.0296(5) -0.0018(4) 0.0056(4) -0.0005(4) Ti(2) 0.0243(5) 0.0265(5) 0.0290(5) -0.0016(4) 0.0040(4) -0.0013(4) Cl(1) 0.0375(8) 0.0371(7) 0.0351(7) -0.0014(6) -0.0022(6) 0.0025(5) Cl(2) 0.0426(8) 0.0291(7) 0.0412(7) 0.0055(6) 0.0088(6) 0.0023(5) O(1) 0.0218(18) 0.0340(18) 0.0301(16) -0.0063(14) 0.0071(14) -0.0017(14) O(2) 0.0266(19) 0.0287(18) 0.0331(17) -0.0093(14) 0.0060(15) -0.0017(14) C(11) 0.018(3) 0.033(3) 0.021(2) -0.001(2) 0.003(2) 0.003(2) C(12) 0.020(3) 0.028(3) 0.031(3) -0.003(2) 0.002(2) -0.001(2) C(13) 0.027(3) 0.030(3) 0.038(3) -0.004(2) 0.007(2) 0.001(2) C(14) 0.030(3) 0.028(3) 0.038(3) -0.002(2) 0.007(2) -0.005(2) C(15) 0.032(3) 0.036(3) 0.031(3) -0.004(2) -0.001(2) -0.008(2) C(16) 0.025(3) 0.032(3) 0.028(2) 0.001(2) -0.004(2) -0.005(2) C(21) 0.026(3) 0.026(3) 0.025(2) 0.002(2) 0.004(2) 0.003(2) C(22) 0.026(3) 0.024(3) 0.025(2) -0.003(2) 0.003(2) 0.003(2) C(23) 0.027(3) 0.032(3) 0.029(3) -0.010(2) -0.003(2) 0.003(2) C(24) 0.023(3) 0.040(3) 0.029(3) -0.004(2) -0.005(2) 0.004(2) C(25) 0.033(3) 0.037(3) 0.026(2) -0.001(2) -0.007(2) -0.004(2) C(26) 0.024(3) 0.025(3) 0.029(2) -0.002(2) -0.002(2) 0.000(2) C(111) 0.018(3) 0.061(4) 0.042(3) -0.008(3) 0.009(2) -0.006(3) C(112) 0.031(3) 0.045(4) 0.054(4) 0.005(3) 0.019(3) 0.004(3) C(113) 0.036(3) 0.066(4) 0.048(3) -0.004(3) 0.023(3) -0.015(3) C(114) 0.038(4) 0.068(4) 0.034(3) -0.008(3) 0.015(3) 0.008(3) C(115) 0.034(3) 0.049(3) 0.045(3) -0.015(3) 0.011(3) 0.002(3) C(121) 0.024(3) 0.022(3) 0.035(3) -0.007(2) 0.008(2) 0.001(2) C(122) 0.025(3) 0.028(3) 0.035(3) -0.009(2) -0.002(2) 0.001(2) C(123) 0.043(3) 0.039(3) 0.033(3) -0.007(3) 0.011(3) -0.009(2) C(124) 0.040(3) 0.028(3) 0.037(3) 0.000(3) 0.015(3) -0.002(2) C(125) 0.054(4) 0.036(3) 0.058(4) 0.004(3) 0.018(3) -0.004(3) C(126) 0.064(5) 0.035(3) 0.076(4) 0.022(3) 0.030(4) 0.007(3) C(127) 0.053(4) 0.054(4) 0.062(4) 0.022(3) 0.008(3) 0.014(3) C(128) 0.047(4) 0.043(3) 0.038(3) 0.007(3) 0.005(3) 0.003(2) C(129) 0.035(3) 0.025(3) 0.035(3) 0.000(2) 0.009(2) 0.004(2) C(141) 0.040(4) 0.044(3) 0.064(4) -0.007(3) 0.026(3) -0.014(3) C(142) 0.038(4) 0.140(6) 0.062(4) 0.020(4) 0.021(3) 0.006(4) C(143) 0.074(5) 0.125(6) 0.054(4) 0.026(4) 0.025(4) 0.017(4) C(144) 0.183(10) 0.134(8) 0.257(11) -0.112(7) 0.198(9) -0.119(8) C(161) 0.028(3) 0.037(3) 0.045(3) -0.011(2) 0.004(2) -0.015(2) C(162) 0.045(4) 0.039(3) 0.058(3) -0.018(3) -0.001(3) 0.003(3) C(163) 0.056(4) 0.057(4) 0.071(4) -0.032(3) 0.020(3) -0.031(3) C(164) 0.034(3) 0.057(4) 0.060(3) -0.014(3) -0.009(3) -0.011(3) C(211) 0.023(3) 0.042(3) 0.041(3) -0.005(2) 0.005(2) -0.004(3) C(212) 0.025(3) 0.033(3) 0.042(3) 0.001(2) 0.008(2) -0.001(2) C(213) 0.032(3) 0.041(3) 0.037(3) 0.001(2) 0.009(2) -0.013(2) C(214) 0.040(3) 0.046(4) 0.031(3) 0.006(3) 0.015(2) 0.000(3) C(215) 0.026(3) 0.033(3) 0.051(3) -0.005(2) 0.022(3) -0.003(3) C(221) 0.018(3) 0.024(3) 0.029(3) -0.007(2) 0.005(2) 0.001(2) C(222) 0.013(3) 0.029(3) 0.040(3) -0.003(2) 0.001(2) 0.002(2) C(223) 0.025(3) 0.035(3) 0.032(3) -0.002(2) -0.004(2) -0.003(2) C(224) 0.019(3) 0.029(3) 0.034(3) -0.005(2) 0.001(2) -0.002(2) C(225) 0.029(3) 0.032(3) 0.044(3) -0.005(2) -0.002(2) -0.008(2) C(226) 0.029(3) 0.028(3) 0.062(3) -0.002(2) -0.003(3) -0.009(3) C(227) 0.027(3) 0.027(3) 0.058(3) 0.000(2) -0.010(3) 0.008(3) C(228) 0.029(3) 0.029(3) 0.039(3) -0.010(2) -0.004(2) 0.001(2) C(229) 0.023(3) 0.024(3) 0.028(3) -0.005(2) -0.001(2) 0.005(2) C(241) 0.037(3) 0.065(4) 0.023(3) -0.011(3) 0.003(2) -0.001(3) C(242) 0.038(4) 0.075(4) 0.037(3) -0.004(3) 0.009(3) -0.009(3) C(243) 0.053(4) 0.119(5) 0.036(3) -0.017(4) 0.010(3) -0.027(3) C(244) 0.052(4) 0.092(5) 0.037(3) -0.010(3) 0.009(3) 0.014(3) C(261) 0.040(3) 0.039(3) 0.041(3) -0.018(3) -0.001(2) -0.005(2) C(262) 0.030(3) 0.080(4) 0.066(4) -0.016(3) -0.006(3) -0.024(3) C(263) 0.076(5) 0.040(3) 0.054(3) -0.031(3) 0.002(3) 0.006(3) C(264) 0.055(4) 0.066(4) 0.052(3) -0.029(3) 0.002(3) -0.018(3) # 10. 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_publ_flag Ti(1) O(1) 1.915(3) ? Ti(1) C(121) 2.332(4) ? Ti(1) C(112) 2.334(5) ? Ti(1) C(122) 2.363(4) ? Ti(1) C(111) 2.365(5) ? Ti(1) C(113) 2.370(5) ? Ti(1) Cl(1) 2.3753(14) ? Ti(1) C(115) 2.386(5) ? Ti(1) C(114) 2.398(5) ? Ti(1) C(123) 2.399(5) ? Ti(1) C(129) 2.414(4) ? Ti(1) C(124) 2.514(5) ? Ti(2) O(2) 1.908(3) ? Ti(2) C(212) 2.348(4) ? Ti(2) C(222) 2.363(4) ? Ti(2) C(221) 2.366(4) ? Ti(2) C(223) 2.374(4) ? Ti(2) C(213) 2.378(4) ? Ti(2) Cl(2) 2.3852(14) ? Ti(2) C(211) 2.385(5) ? Ti(2) C(215) 2.397(4) ? Ti(2) C(214) 2.420(4) ? Ti(2) C(229) 2.433(4) ? Ti(2) C(224) 2.491(4) ? O(1) C(11) 1.359(5) ? O(2) C(21) 1.356(5) ? C(11) C(12) 1.397(6) ? C(11) C(16) 1.405(6) ? C(12) C(13) 1.387(6) ? C(12) C(121) 1.480(6) ? C(13) C(14) 1.384(6) ? C(14) C(15) 1.393(6) ? C(14) C(141) 1.534(6) ? C(15) C(16) 1.402(6) ? C(16) C(161) 1.529(6) ? C(21) C(22) 1.400(6) ? C(21) C(26) 1.405(6) ? C(22) C(23) 1.381(6) ? C(22) C(221) 1.475(6) ? C(23) C(24) 1.392(6) ? C(24) C(25) 1.384(6) ? C(24) C(241) 1.546(6) ? C(25) C(26) 1.397(6) ? C(26) C(261) 1.519(6) ? C(111) C(115) 1.383(7) ? C(111) C(112) 1.406(6) ? C(112) C(113) 1.398(7) ? C(113) C(114) 1.384(7) ? C(114) C(115) 1.401(7) ? C(121) C(122) 1.402(6) ? C(121) C(129) 1.437(6) ? C(122) C(123) 1.395(6) ? C(123) C(124) 1.427(6) ? C(124) C(129) 1.416(6) ? C(124) C(125) 1.420(7) ? C(125) C(126) 1.353(7) ? C(126) C(127) 1.414(7) ? C(127) C(128) 1.361(7) ? C(128) C(129) 1.427(6) ? C(141) C(144) 1.464(8) ? C(141) C(142) 1.493(7) ? C(141) C(143) 1.574(8) ? C(161) C(163) 1.528(6) ? C(161) C(162) 1.537(6) ? C(161) C(164) 1.538(6) ? C(211) C(215) 1.399(6) ? C(211) C(212) 1.406(6) ? C(212) C(213) 1.406(6) ? C(213) C(214) 1.391(6) ? C(214) C(215) 1.407(6) ? C(221) C(222) 1.396(6) ? C(221) C(229) 1.438(6) ? C(222) C(223) 1.419(6) ? C(223) C(224) 1.420(6) ? C(224) C(225) 1.424(6) ? C(224) C(229) 1.431(6) ? C(225) C(226) 1.352(6) ? C(226) C(227) 1.413(6) ? C(227) C(228) 1.362(6) ? C(228) C(229) 1.413(6) ? C(241) C(244) 1.524(7) ? C(241) C(242) 1.533(7) ? C(241) C(243) 1.543(6) ? C(261) C(262) 1.535(7) ? C(261) C(264) 1.539(6) ? C(261) C(263) 1.541(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ti(1) C(121) 74.28(13) ? O(1) Ti(1) C(112) 104.77(17) ? C(121) Ti(1) C(112) 122.93(17) ? O(1) Ti(1) C(122) 101.37(14) ? C(121) Ti(1) C(122) 34.72(14) ? C(112) Ti(1) C(122) 134.64(17) ? O(1) Ti(1) C(111) 78.23(15) ? C(121) Ti(1) C(111) 134.51(17) ? C(112) Ti(1) C(111) 34.80(16) ? C(122) Ti(1) C(111) 165.61(17) ? O(1) Ti(1) C(113) 135.25(17) ? C(121) Ti(1) C(113) 135.36(18) ? C(112) Ti(1) C(113) 34.57(17) ? C(122) Ti(1) C(113) 121.07(17) ? C(111) Ti(1) C(113) 57.10(18) ? O(1) Ti(1) Cl(1) 92.20(9) ? C(121) Ti(1) Cl(1) 100.88(12) ? C(112) Ti(1) Cl(1) 135.71(13) ? C(122) Ti(1) Cl(1) 78.53(11) ? C(111) Ti(1) Cl(1) 115.84(13) ? C(113) Ti(1) Cl(1) 108.50(15) ? O(1) Ti(1) C(115) 88.38(15) ? C(121) Ti(1) C(115) 162.20(17) ? C(112) Ti(1) C(115) 57.10(18) ? C(122) Ti(1) C(115) 159.76(17) ? C(111) Ti(1) C(115) 33.85(16) ? C(113) Ti(1) C(115) 56.66(19) ? Cl(1) Ti(1) C(115) 83.45(14) ? O(1) Ti(1) C(114) 122.17(17) ? C(121) Ti(1) C(114) 163.54(18) ? C(112) Ti(1) C(114) 56.82(18) ? C(122) Ti(1) C(114) 131.46(17) ? C(111) Ti(1) C(114) 56.47(18) ? C(113) Ti(1) C(114) 33.75(17) ? Cl(1) Ti(1) C(114) 79.39(14) ? C(115) Ti(1) C(114) 34.07(16) ? O(1) Ti(1) C(123) 132.06(14) ? C(121) Ti(1) C(123) 57.97(15) ? C(112) Ti(1) C(123) 104.35(18) ? C(122) Ti(1) C(123) 34.06(14) ? C(111) Ti(1) C(123) 139.08(17) ? C(113) Ti(1) C(123) 87.28(18) ? Cl(1) Ti(1) C(123) 92.72(13) ? C(115) Ti(1) C(123) 139.55(16) ? C(114) Ti(1) C(123) 105.60(18) ? O(1) Ti(1) C(129) 87.12(13) ? C(121) Ti(1) C(129) 35.19(15) ? C(112) Ti(1) C(129) 88.19(17) ? C(122) Ti(1) C(129) 56.73(16) ? C(111) Ti(1) C(129) 109.00(17) ? C(113) Ti(1) C(129) 103.76(18) ? Cl(1) Ti(1) C(129) 134.01(13) ? C(115) Ti(1) C(129) 142.39(18) ? C(114) Ti(1) C(129) 137.50(18) ? C(123) Ti(1) C(129) 56.75(16) ? O(1) Ti(1) C(124) 120.40(13) ? C(121) Ti(1) C(124) 56.89(14) ? C(112) Ti(1) C(124) 79.25(17) ? C(122) Ti(1) C(124) 55.53(16) ? C(111) Ti(1) C(124) 112.02(18) ? C(113) Ti(1) C(124) 78.57(17) ? Cl(1) Ti(1) C(124) 126.37(13) ? C(115) Ti(1) C(124) 133.43(17) ? C(114) Ti(1) C(124) 109.56(17) ? C(123) Ti(1) C(124) 33.67(15) ? C(129) Ti(1) C(124) 33.31(14) ? O(2) Ti(2) C(212) 105.17(15) ? O(2) Ti(2) C(222) 99.08(13) ? C(212) Ti(2) C(222) 135.34(16) ? O(2) Ti(2) C(221) 73.29(13) ? C(212) Ti(2) C(221) 121.78(15) ? C(222) Ti(2) C(221) 34.34(14) ? O(2) Ti(2) C(223) 131.00(14) ? C(212) Ti(2) C(223) 105.06(16) ? C(222) Ti(2) C(223) 34.86(14) ? C(221) Ti(2) C(223) 58.09(15) ? O(2) Ti(2) C(213) 135.30(15) ? C(212) Ti(2) C(213) 34.60(15) ? C(222) Ti(2) C(213) 123.34(16) ? C(221) Ti(2) C(213) 135.74(16) ? C(223) Ti(2) C(213) 88.65(16) ? O(2) Ti(2) Cl(2) 95.38(9) ? C(212) Ti(2) Cl(2) 134.72(12) ? C(222) Ti(2) Cl(2) 77.91(11) ? C(221) Ti(2) Cl(2) 102.54(11) ? C(223) Ti(2) Cl(2) 89.79(11) ? C(213) Ti(2) Cl(2) 105.88(12) ? O(2) Ti(2) C(211) 78.43(14) ? C(212) Ti(2) C(211) 34.55(15) ? C(222) Ti(2) C(211) 164.31(16) ? C(221) Ti(2) C(211) 132.44(16) ? C(223) Ti(2) C(211) 139.60(15) ? C(213) Ti(2) C(211) 56.90(16) ? Cl(2) Ti(2) C(211) 117.66(12) ? O(2) Ti(2) C(215) 87.79(15) ? C(212) Ti(2) C(215) 57.17(16) ? C(222) Ti(2) C(215) 161.54(16) ? C(221) Ti(2) C(215) 160.26(16) ? C(223) Ti(2) C(215) 141.19(16) ? C(213) Ti(2) C(215) 56.68(16) ? Cl(2) Ti(2) C(215) 84.43(12) ? C(211) Ti(2) C(215) 34.01(15) ? O(2) Ti(2) C(214) 121.43(16) ? C(212) Ti(2) C(214) 56.73(16) ? C(222) Ti(2) C(214) 134.29(17) ? C(221) Ti(2) C(214) 165.27(17) ? C(223) Ti(2) C(214) 107.34(17) ? C(213) Ti(2) C(214) 33.70(15) ? Cl(2) Ti(2) C(214) 78.07(12) ? C(211) Ti(2) C(214) 56.27(17) ? C(215) Ti(2) C(214) 33.96(15) ? O(2) Ti(2) C(229) 86.84(13) ? C(212) Ti(2) C(229) 87.50(15) ? C(222) Ti(2) C(229) 56.76(15) ? C(221) Ti(2) C(229) 34.84(14) ? C(223) Ti(2) C(229) 57.12(15) ? C(213) Ti(2) C(229) 103.98(16) ? Cl(2) Ti(2) C(229) 134.28(11) ? C(211) Ti(2) C(229) 107.55(16) ? C(215) Ti(2) C(229) 141.25(16) ? C(214) Ti(2) C(229) 137.68(16) ? O(2) Ti(2) C(224) 120.59(13) ? C(212) Ti(2) C(224) 79.16(15) ? C(222) Ti(2) C(224) 56.19(14) ? C(221) Ti(2) C(224) 56.98(13) ? C(223) Ti(2) C(224) 33.83(14) ? C(213) Ti(2) C(224) 79.01(15) ? Cl(2) Ti(2) C(224) 123.59(11) ? C(211) Ti(2) C(224) 111.53(15) ? C(215) Ti(2) C(224) 133.69(15) ? C(214) Ti(2) C(224) 110.17(16) ? C(229) Ti(2) C(224) 33.76(13) ? C(11) O(1) Ti(1) 124.8(3) ? C(21) O(2) Ti(2) 127.3(3) ? O(1) C(11) C(12) 116.9(4) ? O(1) C(11) C(16) 122.3(4) ? C(12) C(11) C(16) 120.8(4) ? C(13) C(12) C(11) 121.2(4) ? C(13) C(12) C(121) 126.2(4) ? C(11) C(12) C(121) 112.6(4) ? C(14) C(13) C(12) 120.3(4) ? C(13) C(14) C(15) 117.2(4) ? C(13) C(14) C(141) 121.8(4) ? C(15) C(14) C(141) 120.9(4) ? C(14) C(15) C(16) 125.1(4) ? C(15) C(16) C(11) 115.4(4) ? C(15) C(16) C(161) 122.8(4) ? C(11) C(16) C(161) 121.7(4) ? O(2) C(21) C(22) 116.2(4) ? O(2) C(21) C(26) 122.5(4) ? C(22) C(21) C(26) 121.3(4) ? C(23) C(22) C(21) 120.4(4) ? C(23) C(22) C(221) 126.7(4) ? C(21) C(22) C(221) 112.9(4) ? C(22) C(23) C(24) 120.5(4) ? C(25) C(24) C(23) 117.5(4) ? C(25) C(24) C(241) 122.9(4) ? C(23) C(24) C(241) 119.6(4) ? C(24) C(25) C(26) 125.0(4) ? C(25) C(26) C(21) 115.3(4) ? C(25) C(26) C(261) 123.1(4) ? C(21) C(26) C(261) 121.5(4) ? C(115) C(111) C(112) 108.0(5) ? C(115) C(111) Ti(1) 73.9(3) ? C(112) C(111) Ti(1) 71.4(3) ? C(113) C(112) C(111) 107.6(5) ? C(113) C(112) Ti(1) 74.1(3) ? C(111) C(112) Ti(1) 73.8(3) ? C(114) C(113) C(112) 108.1(5) ? C(114) C(113) Ti(1) 74.2(3) ? C(112) C(113) Ti(1) 71.3(3) ? C(113) C(114) C(115) 108.2(5) ? C(113) C(114) Ti(1) 72.0(3) ? C(115) C(114) Ti(1) 72.5(3) ? C(111) C(115) C(114) 108.1(5) ? C(111) C(115) Ti(1) 72.3(3) ? C(114) C(115) Ti(1) 73.4(3) ? C(122) C(121) C(129) 106.2(4) ? C(122) C(121) C(12) 128.7(4) ? C(129) C(121) C(12) 124.3(4) ? C(122) C(121) Ti(1) 73.8(2) ? C(129) C(121) Ti(1) 75.5(2) ? C(12) C(121) Ti(1) 108.2(3) ? C(123) C(122) C(121) 110.2(4) ? C(123) C(122) Ti(1) 74.4(3) ? C(121) C(122) Ti(1) 71.4(2) ? C(122) C(123) C(124) 107.5(4) ? C(122) C(123) Ti(1) 71.6(2) ? C(124) C(123) Ti(1) 77.6(3) ? C(129) C(124) C(125) 119.7(5) ? C(129) C(124) C(123) 107.2(4) ? C(125) C(124) C(123) 133.1(5) ? C(129) C(124) Ti(1) 69.5(2) ? C(125) C(124) Ti(1) 127.6(3) ? C(123) C(124) Ti(1) 68.7(3) ? C(126) C(125) C(124) 118.5(5) ? C(125) C(126) C(127) 121.8(5) ? C(128) C(127) C(126) 121.8(5) ? C(127) C(128) C(129) 117.7(5) ? C(124) C(129) C(128) 120.4(4) ? C(124) C(129) C(121) 108.4(4) ? C(128) C(129) C(121) 131.2(4) ? C(124) C(129) Ti(1) 77.2(3) ? C(128) C(129) Ti(1) 120.7(3) ? C(121) C(129) Ti(1) 69.3(2) ? C(144) C(141) C(142) 114.3(7) ? C(144) C(141) C(14) 113.2(4) ? C(142) C(141) C(14) 109.8(4) ? C(144) C(141) C(143) 104.1(6) ? C(142) C(141) C(143) 105.5(4) ? C(14) C(141) C(143) 109.4(4) ? C(163) C(161) C(16) 112.3(4) ? C(163) C(161) C(162) 107.3(4) ? C(16) C(161) C(162) 109.2(4) ? C(163) C(161) C(164) 108.5(4) ? C(16) C(161) C(164) 110.2(4) ? C(162) C(161) C(164) 109.4(4) ? C(215) C(211) C(212) 108.1(4) ? C(215) C(211) Ti(2) 73.5(3) ? C(212) C(211) Ti(2) 71.3(3) ? C(213) C(212) C(211) 107.6(4) ? C(213) C(212) Ti(2) 73.8(3) ? C(211) C(212) Ti(2) 74.2(3) ? C(214) C(213) C(212) 108.2(4) ? C(214) C(213) Ti(2) 74.8(3) ? C(212) C(213) Ti(2) 71.6(2) ? C(213) C(214) C(215) 108.2(4) ? C(213) C(214) Ti(2) 71.5(3) ? C(215) C(214) Ti(2) 72.1(2) ? C(211) C(215) C(214) 107.8(4) ? C(211) C(215) Ti(2) 72.5(3) ? C(214) C(215) Ti(2) 73.9(3) ? C(222) C(221) C(229) 107.1(4) ? C(222) C(221) C(22) 128.6(4) ? C(229) C(221) C(22) 123.1(4) ? C(222) C(221) Ti(2) 72.7(2) ? C(229) C(221) Ti(2) 75.1(2) ? C(22) C(221) Ti(2) 108.3(3) ? C(221) C(222) C(223) 109.7(4) ? C(221) C(222) Ti(2) 72.9(2) ? C(223) C(222) Ti(2) 73.0(2) ? C(222) C(223) C(224) 107.5(4) ? C(222) C(223) Ti(2) 72.1(2) ? C(224) C(223) Ti(2) 77.6(3) ? C(223) C(224) C(225) 133.1(4) ? C(223) C(224) C(229) 107.5(4) ? C(225) C(224) C(229) 119.4(4) ? C(223) C(224) Ti(2) 68.6(2) ? C(225) C(224) Ti(2) 127.1(3) ? C(229) C(224) Ti(2) 70.9(2) ? C(226) C(225) C(224) 118.4(4) ? C(225) C(226) C(227) 122.4(4) ? C(228) C(227) C(226) 120.7(4) ? C(227) C(228) C(229) 119.1(4) ? C(228) C(229) C(224) 119.9(4) ? C(228) C(229) C(221) 132.2(4) ? C(224) C(229) C(221) 107.9(4) ? C(228) C(229) Ti(2) 123.1(3) ? C(224) C(229) Ti(2) 75.3(2) ? C(221) C(229) Ti(2) 70.0(2) ? C(244) C(241) C(242) 108.8(4) ? C(244) C(241) C(243) 108.7(4) ? C(242) C(241) C(243) 108.3(4) ? C(244) C(241) C(24) 110.0(4) ? C(242) C(241) C(24) 109.2(4) ? C(243) C(241) C(24) 111.8(4) ? C(26) C(261) C(262) 110.1(4) ? C(26) C(261) C(264) 112.9(4) ? C(262) C(261) C(264) 107.4(4) ? C(26) C(261) C(263) 109.4(4) ? C(262) C(261) C(263) 109.6(4) ? C(264) C(261) C(263) 107.3(4) ? #============================================================================== data_LT2MIP _database_code_CSD 218469 #============================================================================== _audit_creation_date 7-10-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.36 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C24 H29.50 O1' _chemical_formula_moiety 'C24 H30 O1' _chemical_formula_structural ? _chemical_formula_weight 334.00 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 20.0248(5) _cell_length_b 10.2632(2) _cell_length_c 9.9894(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.5259(7) _cell_angle_gamma 90.00 _cell_volume 2018.46(8) _cell_measurement_reflns_used 17945 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.10 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.060 _cell_measurement_temperature 150 _exptl_crystal_F_000 728 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.5843 _exptl_absorpt_correction_T_max 0.9783 _diffrn_reflns_number 17945 _diffrn_measured_fraction_theta_max 0.9967 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9967 _reflns_number_total 4804 _reflns_number_gt 4047 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_max 13 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.123 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 4775 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.2229P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.22 _refine_diff_density_min -0.17 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(Shelxs97,_Sheldrick,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.2791(2) -0.1880(3) 0.1648(5) 0.0402(6) Uani 0.50 1 d P . . O(3) O 0.16230(10) 0.2217(2) 0.0923(2) 0.0381(5) Uani 0.50 1 d P . . C(1) C 0.27603(6) -0.05786(13) 0.15722(12) 0.0322(3) Uani 1 1 d . . . C(2) C 0.21530(6) 0.01162(12) 0.12661(11) 0.0292(3) Uani 1 1 d . . . C(3) C 0.21726(6) 0.14791(12) 0.12778(11) 0.0296(3) Uani 1 1 d . . . C(4) C 0.27877(6) 0.21552(12) 0.15835(11) 0.0312(3) Uani 1 1 d . A . C(5) C 0.33773(6) 0.14087(13) 0.18460(12) 0.0351(3) Uani 1 1 d . . . C(6) C 0.33872(6) 0.00523(14) 0.18507(12) 0.0357(3) Uani 1 1 d . B . C(21) C 0.14913(6) -0.05738(11) 0.09535(12) 0.0302(3) Uani 1 1 d . . . C(22) C 0.12902(7) -0.14671(12) -0.00361(12) 0.0340(3) Uani 1 1 d . . . C(23) C 0.05786(7) -0.19173(12) -0.00012(13) 0.0369(3) Uani 1 1 d . . . C(24) C 0.03848(6) -0.11648(12) 0.11544(12) 0.0331(3) Uani 1 1 d . . . C(25) C -0.02016(7) -0.11624(13) 0.17000(14) 0.0389(3) Uani 1 1 d . . . C(26) C -0.02318(7) -0.03830(13) 0.28286(14) 0.0410(3) Uani 1 1 d . . . C(27) C 0.03176(7) 0.03829(13) 0.33970(13) 0.0386(3) Uani 1 1 d . . . C(28) C 0.09049(7) 0.04064(12) 0.28435(12) 0.0333(3) Uani 1 1 d . . . C(29) C 0.09377(6) -0.03706(11) 0.17196(12) 0.0301(3) Uani 1 1 d . . . C(41) C 0.28255(7) 0.36507(13) 0.16286(12) 0.0389(3) Uani 1 1 d D . . C(61) C 0.40620(7) -0.06959(16) 0.21500(15) 0.0490(4) Uani 1 1 d D . . C(221) C 0.16728(8) -0.19785(14) -0.10734(14) 0.0430(3) Uani 1 1 d . . . C(42A) C 0.20561(14) 0.4274(3) 0.1530(3) 0.0407(6) Uani 0.50 1 d PD A 1 C(42B) C 0.25164(18) 0.4135(3) 0.2741(3) 0.0530(8) Uani 0.50 1 d PD A 2 C(43A) C 0.3065(2) 0.4196(3) 0.0396(3) 0.0502(8) Uani 0.50 1 d PD A 1 C(43B) C 0.2599(2) 0.4211(3) 0.0261(3) 0.0556(9) Uani 0.50 1 d PD A 2 C(44A) C 0.31994(15) 0.4174(3) 0.2954(3) 0.0416(6) Uani 0.50 1 d PD A 1 C(44B) C 0.36275(16) 0.4039(3) 0.2028(4) 0.0560(8) Uani 0.50 1 d PD A 2 C(62A) C 0.41545(17) -0.1461(3) 0.0924(3) 0.0494(7) Uani 0.50 1 d PD B 1 C(62B) C 0.44606(19) -0.0534(5) 0.1060(4) 0.0664(10) Uani 0.50 1 d PD B 2 C(63A) C 0.41258(17) -0.1426(3) 0.3432(3) 0.0505(7) Uani 0.50 1 d PD B 1 C(63B) C 0.44292(19) -0.0495(4) 0.3561(4) 0.0655(10) Uani 0.50 1 d PD B 2 C(64A) C 0.46818(15) 0.0373(3) 0.2368(4) 0.0573(8) Uani 0.50 1 d PD B 1 C(64B) C 0.38997(19) -0.2298(3) 0.2136(5) 0.0686(10) Uani 0.50 1 d PD B 2 H(1) H 0.236(3) -0.226(5) 0.150(5) 0.088(14) Uiso 0.50 1 d P . . H(3) H 0.1376(19) 0.182(4) 0.089(4) 0.052(12) Uiso 0.50 1 d P . . H(5) H 0.3800 0.1853 0.2034 0.042 Uiso 1 1 calc R . . H(1A) H 0.271(4) -0.168(7) 0.160(7) 0.039 Uiso 0.50 1 d P . . H(25) H -0.0579 -0.1685 0.1311 0.047 Uiso 1 1 calc R . . H(26) H -0.0632 -0.0376 0.3212 0.049 Uiso 1 1 calc R . . H(27) H 0.0292 0.0898 0.4176 0.046 Uiso 1 1 calc R . . H(28) H 0.1277 0.0944 0.3226 0.040 Uiso 1 1 calc R . . H(22A) H 0.2108 -0.1521 -0.0989 0.064 Uiso 1 1 calc R . . H(22B) H 0.1406 -0.1837 -0.1987 0.064 Uiso 1 1 calc R . . H(22C) H 0.1755 -0.2913 -0.0925 0.064 Uiso 1 1 calc R . . H(23A) H 0.0270 -0.1715 -0.0868 0.044 Uiso 1 1 calc R . . H(23B) H 0.0567 -0.2867 0.0168 0.044 Uiso 1 1 calc R . . H(42A) H 0.2087 0.5227 0.1570 0.061 Uiso 0.50 1 calc PR A 1 H(42B) H 0.1856 0.3955 0.2292 0.061 Uiso 0.50 1 calc PR A 1 H(42C) H 0.1771 0.4011 0.0668 0.061 Uiso 0.50 1 calc PR A 1 H(42D) H 0.2583 0.5079 0.2826 0.079 Uiso 0.50 1 calc PR A 2 H(42E) H 0.2729 0.3711 0.3592 0.079 Uiso 0.50 1 calc PR A 2 H(42F) H 0.2029 0.3941 0.2555 0.079 Uiso 0.50 1 calc PR A 2 H(43A) H 0.2762 0.3900 -0.0431 0.075 Uiso 0.50 1 calc PR A 1 H(43B) H 0.3528 0.3893 0.0386 0.075 Uiso 0.50 1 calc PR A 1 H(43C) H 0.3060 0.5150 0.0434 0.075 Uiso 0.50 1 calc PR A 1 H(43D) H 0.2111 0.4057 -0.0030 0.083 Uiso 0.50 1 calc PR A 2 H(43E) H 0.2846 0.3796 -0.0385 0.083 Uiso 0.50 1 calc PR A 2 H(43F) H 0.2688 0.5150 0.0288 0.083 Uiso 0.50 1 calc PR A 2 H(44A) H 0.3669 0.3856 0.3114 0.062 Uiso 0.50 1 calc PR A 1 H(44B) H 0.2975 0.3882 0.3695 0.062 Uiso 0.50 1 calc PR A 1 H(44C) H 0.3199 0.5129 0.2923 0.062 Uiso 0.50 1 calc PR A 1 H(44D) H 0.3870 0.3700 0.1335 0.084 Uiso 0.50 1 calc PR A 2 H(44E) H 0.3821 0.3662 0.2915 0.084 Uiso 0.50 1 calc PR A 2 H(44F) H 0.3673 0.4990 0.2074 0.084 Uiso 0.50 1 calc PR A 2 H(62A) H 0.4601 -0.1883 0.1097 0.074 Uiso 0.50 1 calc PR B 1 H(62B) H 0.4124 -0.0875 0.0140 0.074 Uiso 0.50 1 calc PR B 1 H(62C) H 0.3799 -0.2126 0.0731 0.074 Uiso 0.50 1 calc PR B 1 H(62D) H 0.4869 -0.1079 0.1256 0.100 Uiso 0.50 1 calc PR B 2 H(62E) H 0.4593 0.0381 0.1011 0.100 Uiso 0.50 1 calc PR B 2 H(62F) H 0.4185 -0.0798 0.0188 0.100 Uiso 0.50 1 calc PR B 2 H(63A) H 0.4570 -0.1854 0.3627 0.076 Uiso 0.50 1 calc PR B 1 H(63B) H 0.3766 -0.2085 0.3350 0.076 Uiso 0.50 1 calc PR B 1 H(63C) H 0.4083 -0.0825 0.4174 0.076 Uiso 0.50 1 calc PR B 1 H(63D) H 0.4129 -0.0712 0.4202 0.098 Uiso 0.50 1 calc PR B 2 H(63E) H 0.4571 0.0418 0.3683 0.098 Uiso 0.50 1 calc PR B 2 H(63F) H 0.4831 -0.1059 0.3732 0.098 Uiso 0.50 1 calc PR B 2 H(64A) H 0.4648 0.0928 0.3152 0.086 Uiso 0.50 1 calc PR B 1 H(64B) H 0.4649 0.0914 0.1550 0.086 Uiso 0.50 1 calc PR B 1 H(64C) H 0.5119 -0.0083 0.2534 0.086 Uiso 0.50 1 calc PR B 1 H(64D) H 0.4328 -0.2780 0.2354 0.103 Uiso 0.50 1 calc PR B 2 H(64E) H 0.3659 -0.2554 0.1231 0.103 Uiso 0.50 1 calc PR B 2 H(64F) H 0.3618 -0.2496 0.2815 0.103 Uiso 0.50 1 calc PR 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0437(14) 0.0271(13) 0.0499(11) 0.0002(10) 0.0085(10) 0.0019(10) O(3) 0.0250(10) 0.0339(10) 0.0526(12) -0.0021(8) -0.0001(8) 0.0025(8) C(1) 0.0376(7) 0.0310(7) 0.0287(6) 0.0028(5) 0.0075(5) -0.0003(5) C(2) 0.0314(6) 0.0305(6) 0.0254(5) -0.0030(5) 0.0046(4) -0.0014(4) C(3) 0.0316(6) 0.0305(6) 0.0258(6) -0.0005(5) 0.0027(4) -0.0009(4) C(4) 0.0384(7) 0.0330(6) 0.0223(5) -0.0067(5) 0.0054(5) -0.0022(4) C(5) 0.0302(6) 0.0466(8) 0.0290(6) -0.0081(5) 0.0066(5) -0.0037(5) C(6) 0.0321(7) 0.0470(7) 0.0283(6) 0.0060(5) 0.0066(5) -0.0002(5) C(21) 0.0327(6) 0.0280(6) 0.0293(6) -0.0029(5) 0.0040(5) 0.0020(4) C(22) 0.0404(7) 0.0301(6) 0.0311(6) -0.0056(5) 0.0054(5) 0.0002(5) C(23) 0.0419(7) 0.0320(6) 0.0353(7) -0.0094(5) 0.0028(5) -0.0004(5) C(24) 0.0349(7) 0.0287(6) 0.0341(6) -0.0022(5) 0.0020(5) 0.0063(5) C(25) 0.0335(7) 0.0344(7) 0.0474(7) -0.0033(5) 0.0040(6) 0.0097(6) C(26) 0.0371(7) 0.0377(7) 0.0507(8) 0.0063(6) 0.0146(6) 0.0117(6) C(27) 0.0425(8) 0.0351(7) 0.0393(7) 0.0077(6) 0.0109(6) 0.0030(5) C(28) 0.0351(7) 0.0312(6) 0.0326(6) 0.0012(5) 0.0032(5) 0.0009(5) C(29) 0.0317(6) 0.0268(6) 0.0305(6) 0.0001(5) 0.0025(5) 0.0047(4) C(41) 0.0524(8) 0.0330(7) 0.0312(6) -0.0109(6) 0.0077(6) -0.0033(5) C(61) 0.0343(8) 0.0651(10) 0.0474(8) 0.0146(7) 0.0071(6) -0.0003(7) C(221) 0.0546(9) 0.0385(7) 0.0377(7) -0.0094(6) 0.0134(6) -0.0078(5) C(42A) 0.0438(15) 0.0300(13) 0.0465(15) 0.0025(11) 0.0037(12) -0.0036(11) C(42B) 0.065(2) 0.0398(16) 0.0573(18) -0.0007(14) 0.0192(15) -0.0118(13) C(43A) 0.075(2) 0.0342(15) 0.0487(18) -0.0070(17) 0.0294(19) 0.0013(13) C(43B) 0.074(3) 0.0399(17) 0.0485(18) -0.0098(19) -0.0005(19) 0.0088(13) C(44A) 0.0447(16) 0.0358(14) 0.0420(14) -0.0063(12) 0.0017(12) -0.0106(11) C(44B) 0.0420(17) 0.0392(16) 0.084(2) -0.0118(13) 0.0025(16) -0.0046(15) C(62A) 0.0452(17) 0.0475(17) 0.0593(18) 0.0114(15) 0.0201(14) -0.0037(14) C(62B) 0.0461(19) 0.091(3) 0.066(2) 0.024(2) 0.0206(16) 0.007(2) C(63A) 0.0442(17) 0.0503(18) 0.0525(17) 0.0104(15) -0.0028(13) 0.0067(14) C(63B) 0.048(2) 0.085(3) 0.057(2) 0.022(2) -0.0055(16) 0.0018(19) C(64A) 0.0265(14) 0.0594(19) 0.085(2) 0.0046(13) 0.0076(14) -0.0031(17) C(64B) 0.052(2) 0.053(2) 0.098(3) 0.0178(16) 0.0069(18) 0.0008(19) # 10. 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_publ_flag O(1) C(1) 1.338(4) YES O(1) H(1) 0.94(5) YES O(1) H(1A) 0.26(6) YES O(3) C(3) 1.329(2) YES O(3) H(3) 0.63(4) YES C(1) C(6) 1.3946(18) YES C(1) C(2) 1.3947(17) YES C(1) H(1A) 1.13(7) YES C(2) C(3) 1.3992(17) YES C(2) C(21) 1.4844(16) YES C(3) C(4) 1.3981(17) YES C(4) C(5) 1.3918(18) YES C(4) C(41) 1.5369(17) YES C(5) C(6) 1.3922(19) YES C(6) C(61) 1.5353(19) YES C(21) C(22) 1.3544(17) YES C(21) C(29) 1.4724(17) YES C(22) C(221) 1.4921(19) YES C(22) C(23) 1.5044(18) YES C(23) C(24) 1.4978(18) YES C(24) C(25) 1.3819(19) YES C(24) C(29) 1.4072(17) YES C(25) C(26) 1.393(2) YES C(26) C(27) 1.387(2) YES C(27) C(28) 1.3882(19) YES C(28) C(29) 1.3884(17) YES C(41) C(42B) 1.455(3) YES C(41) C(43B) 1.476(3) YES C(41) C(44A) 1.497(3) YES C(41) C(43A) 1.508(3) YES C(41) C(44B) 1.632(3) YES C(41) C(42A) 1.655(3) YES C(61) C(63A) 1.469(3) YES C(61) C(62B) 1.472(4) YES C(61) C(63B) 1.480(4) YES C(61) C(62A) 1.495(3) YES C(61) C(64A) 1.641(4) YES C(61) C(64B) 1.676(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C(1) O(1) H(1) 112(3) YES C(1) O(1) H(1A) 35(10) YES H(1) O(1) H(1A) 77(10) YES C(3) O(3) H(3) 104(3) YES O(1) C(1) C(6) 114.98(19) YES O(1) C(1) C(2) 123.4(2) YES C(6) C(1) C(2) 121.56(12) YES O(1) C(1) H(1A) 7(4) YES C(6) C(1) H(1A) 122(4) YES C(2) C(1) H(1A) 116(3) YES C(1) C(2) C(3) 119.16(11) YES C(1) C(2) C(21) 120.75(11) YES C(3) C(2) C(21) 120.08(11) YES O(3) C(3) C(4) 115.40(14) YES O(3) C(3) C(2) 123.12(14) YES C(4) C(3) C(2) 121.35(11) YES C(5) C(4) C(3) 116.82(11) YES C(5) C(4) C(41) 120.57(11) YES C(3) C(4) C(41) 122.61(11) YES C(4) C(5) C(6) 124.20(11) YES C(5) C(6) C(1) 116.87(11) YES C(5) C(6) C(61) 120.81(12) YES C(1) C(6) C(61) 122.33(13) YES C(22) C(21) C(29) 108.87(11) YES C(22) C(21) C(2) 127.69(11) YES C(29) C(21) C(2) 123.43(10) YES C(21) C(22) C(221) 128.54(12) YES C(21) C(22) C(23) 110.34(11) YES C(221) C(22) C(23) 121.11(11) YES C(24) C(23) C(22) 103.85(10) YES C(25) C(24) C(29) 120.24(12) YES C(25) C(24) C(23) 131.55(12) YES C(29) C(24) C(23) 108.19(11) YES C(24) C(25) C(26) 119.08(12) YES C(27) C(26) C(25) 120.56(13) YES C(26) C(27) C(28) 120.89(12) YES C(27) C(28) C(29) 118.73(12) YES C(28) C(29) C(24) 120.47(12) YES C(28) C(29) C(21) 130.76(11) YES C(24) C(29) C(21) 108.74(11) YES C(42B) C(41) C(43B) 118.2(2) YES C(42B) C(41) C(44A) 54.22(19) YES C(43B) C(41) C(44A) 134.4(2) YES C(42B) C(41) C(43A) 137.7(2) YES C(43B) C(41) C(43A) 35.85(18) YES C(44A) C(41) C(43A) 114.0(2) YES C(42B) C(41) C(4) 109.75(16) YES C(43B) C(41) C(4) 110.89(16) YES C(44A) C(41) C(4) 113.49(14) YES C(43A) C(41) C(4) 111.60(15) YES C(42B) C(41) C(44B) 105.5(2) YES C(43B) C(41) C(44B) 104.7(2) YES C(44A) C(41) C(44B) 52.06(18) YES C(43A) C(41) C(44B) 70.3(2) YES C(4) C(41) C(44B) 107.00(15) YES C(42B) C(41) C(42A) 52.56(18) YES C(43B) C(41) C(42A) 70.6(2) YES C(44A) C(41) C(42A) 102.93(17) YES C(43A) C(41) C(42A) 103.8(2) YES C(4) C(41) C(42A) 110.13(13) YES C(44B) C(41) C(42A) 141.63(17) YES C(63A) C(61) C(62B) 136.8(2) YES C(63A) C(61) C(63B) 44.9(2) YES C(62B) C(61) C(63B) 116.5(3) YES C(63A) C(61) C(62A) 116.3(2) YES C(62B) C(61) C(62A) 44.6(2) YES C(63B) C(61) C(62A) 137.6(2) YES C(63A) C(61) C(6) 110.99(16) YES C(62B) C(61) C(6) 112.11(17) YES C(63B) C(61) C(6) 112.49(17) YES C(62A) C(61) C(6) 109.86(16) YES C(63A) C(61) C(64A) 106.4(2) YES C(62B) C(61) C(64A) 61.6(2) YES C(63B) C(61) C(64A) 63.1(2) YES C(62A) C(61) C(64A) 104.8(2) YES C(6) C(61) C(64A) 107.99(16) YES C(63A) C(61) C(64B) 59.5(2) YES C(62B) C(61) C(64B) 103.6(3) YES C(63B) C(61) C(64B) 101.9(2) YES C(62A) C(61) C(64B) 62.0(2) YES C(6) C(61) C(64B) 109.07(16) YES C(64A) C(61) C(64B) 142.94(19) YES data_LTDMIL _database_code_CSD 218470 _audit_creation_date 26-09-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C25 H32 O1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 348.53 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4964(4) _cell_length_b 10.5345(3) _cell_length_c 11.9256(4) _cell_angle_alpha 107.9647(18) _cell_angle_beta 106.6234(15) _cell_angle_gamma 98.9550(15) _cell_volume 1047.79(14) _cell_measurement_reflns_used 12627 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.10 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.061 _cell_measurement_temperature 149 _exptl_crystal_F_000 380 # 6. DATA COLLECTION _diffrn_ambient_temperature 149 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.9607 _exptl_absorpt_correction_T_max 0.9835 _diffrn_reflns_number 12627 _diffrn_measured_fraction_theta_max 0.9810 _diffrn_reflns_theta_full 25.4 _reflns_number_total 4699 _reflns_number_gt 3865 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 14 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.65' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.080 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.000 _refine_ls_wR_factor_gt 0.135 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 4693 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.2513P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.21 _refine_diff_density_min -0.18 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.62E-01 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(2) O 0.6859(2) 0.3738(2) 0.29472(17) 0.0285(4) Uani 0.50 1 d P . . O(6) O 0.1666(2) 0.1167(2) 0.07004(19) 0.0369(5) Uani 0.50 1 d P . . C(1) C 0.42512(16) 0.24913(14) 0.17749(13) 0.0281(3) Uani 1 1 d . . . C(2) C 0.55463(16) 0.30398(15) 0.28836(13) 0.0298(3) Uani 1 1 d . . . C(3) C 0.55187(16) 0.28457(15) 0.39802(13) 0.0301(3) Uani 1 1 d . A . C(4) C 0.41358(16) 0.21061(15) 0.39388(13) 0.0306(3) Uani 1 1 d . . . C(5) C 0.28064(16) 0.15597(14) 0.28667(13) 0.0281(3) Uani 1 1 d . . . C(6) C 0.28968(15) 0.17617(14) 0.17852(12) 0.0278(3) Uani 1 1 d . . . C(7) C 0.43157(16) 0.26353(14) 0.05872(13) 0.0285(3) Uani 1 1 d . . . C(8) C 0.52337(17) 0.21624(15) -0.00379(13) 0.0321(3) Uani 1 1 d . . . C(9) C 0.48829(18) 0.24152(16) -0.12583(14) 0.0354(4) Uani 1 1 d . . . C(10) C 0.36560(17) 0.31683(16) -0.12203(14) 0.0348(4) Uani 1 1 d . . . C(11) C 0.2890(2) 0.36945(18) -0.20705(16) 0.0442(4) Uani 1 1 d . . . C(12) C 0.1806(2) 0.4376(2) -0.17999(18) 0.0500(5) Uani 1 1 d . . . C(13) C 0.1510(2) 0.45275(19) -0.07089(18) 0.0481(4) Uani 1 1 d . . . C(14) C 0.22590(18) 0.39838(17) 0.01456(16) 0.0392(4) Uani 1 1 d . . . C(15) C 0.33299(16) 0.32923(15) -0.01224(13) 0.0308(3) Uani 1 1 d . . . C(31) C 0.69608(17) 0.33872(17) 0.51813(13) 0.0360(4) Uani 1 1 d . . . C(32) C 0.8178(3) 0.2660(3) 0.4921(2) 0.0381(6) Uani 0.674(3) 1 d P A 1 C(33) C 0.7504(3) 0.4913(3) 0.5693(2) 0.0455(7) Uani 0.674(3) 1 d P A 1 C(34) C 0.6608(3) 0.2968(3) 0.6274(2) 0.0430(7) Uani 0.674(3) 1 d P A 1 C(35) C 0.7576(7) 0.2286(6) 0.5320(6) 0.0513(17) Uani 0.326(3) 1 d P A 2 C(36) C 0.6686(7) 0.4304(7) 0.6264(5) 0.0560(18) Uani 0.326(3) 1 d P A 2 C(37) C 0.8307(6) 0.4475(7) 0.4975(5) 0.0579(19) Uani 0.326(3) 1 d P A 2 C(51) C 0.13105(17) 0.07297(17) 0.28490(14) 0.0358(4) Uani 1 1 d . . . C(52) C 0.1383(2) 0.0794(2) 0.41576(17) 0.0593(5) Uani 1 1 d . . . C(53) C -0.00169(19) 0.1305(2) 0.23370(19) 0.0511(5) Uani 1 1 d . . . C(54) C 0.0993(2) -0.07967(18) 0.20025(18) 0.0476(4) Uani 1 1 d . . . C(81) C 0.64445(19) 0.14671(18) 0.03408(16) 0.0405(4) Uani 1 1 d . . . C(91) C 0.4368(2) 0.10693(19) -0.24173(15) 0.0479(4) Uani 1 1 d . . . H(2) H 0.6784 0.3774 0.2256 0.043 Uiso 0.50 1 calc PR . . H(4) H 0.4098 0.1970 0.4665 0.037 Uiso 1 1 calc R . . H(6) H 0.1860 0.1377 0.0143 0.055 Uiso 0.50 1 calc PR . . H(9) H 0.5788 0.3028 -0.1238 0.042 Uiso 1 1 calc R . . H(11) H 0.3091 0.3597 -0.2807 0.053 Uiso 1 1 calc R . . H(12) H 0.1279 0.4732 -0.2364 0.060 Uiso 1 1 calc R . . H(13) H 0.0799 0.5000 -0.0539 0.058 Uiso 1 1 calc R . . H(14) H 0.2048 0.4081 0.0878 0.047 Uiso 1 1 calc R . . H(32A) H 0.9049 0.2960 0.5684 0.057 Uiso 0.674(3) 1 calc PR A 1 H(32B) H 0.8481 0.2889 0.4290 0.057 Uiso 0.674(3) 1 calc PR A 1 H(32C) H 0.7767 0.1676 0.4627 0.057 Uiso 0.674(3) 1 calc PR A 1 H(33A) H 0.8386 0.5215 0.6448 0.068 Uiso 0.674(3) 1 calc PR A 1 H(33B) H 0.6712 0.5302 0.5885 0.068 Uiso 0.674(3) 1 calc PR A 1 H(33C) H 0.7766 0.5215 0.5080 0.068 Uiso 0.674(3) 1 calc PR A 1 H(34A) H 0.6266 0.1978 0.5990 0.064 Uiso 0.674(3) 1 calc PR A 1 H(34B) H 0.5828 0.3368 0.6477 0.064 Uiso 0.674(3) 1 calc PR A 1 H(34C) H 0.7518 0.3307 0.7010 0.064 Uiso 0.674(3) 1 calc PR A 1 H(35A) H 0.8486 0.2638 0.6057 0.077 Uiso 0.326(3) 1 calc PR A 2 H(35B) H 0.7817 0.1851 0.4590 0.077 Uiso 0.326(3) 1 calc PR A 2 H(35C) H 0.6843 0.1621 0.5408 0.077 Uiso 0.326(3) 1 calc PR A 2 H(36A) H 0.5944 0.3778 0.6467 0.084 Uiso 0.326(3) 1 calc PR A 2 H(36B) H 0.6313 0.5028 0.6053 0.084 Uiso 0.326(3) 1 calc PR A 2 H(36C) H 0.7622 0.4704 0.6978 0.084 Uiso 0.326(3) 1 calc PR A 2 H(37A) H 0.9174 0.4910 0.5745 0.087 Uiso 0.326(3) 1 calc PR A 2 H(37B) H 0.7887 0.5171 0.4747 0.087 Uiso 0.326(3) 1 calc PR A 2 H(37C) H 0.8618 0.3957 0.4316 0.087 Uiso 0.326(3) 1 calc PR A 2 H(52A) H 0.2155 0.0378 0.4481 0.089 Uiso 1 1 calc R . . H(52B) H 0.0413 0.0302 0.4108 0.089 Uiso 1 1 calc R . . H(52C) H 0.1625 0.1744 0.4709 0.089 Uiso 1 1 calc R . . H(53A) H 0.0198 0.2264 0.2853 0.077 Uiso 1 1 calc R . . H(53B) H -0.0937 0.0794 0.2352 0.077 Uiso 1 1 calc R . . H(53C) H -0.0143 0.1215 0.1486 0.077 Uiso 1 1 calc R . . H(54A) H 0.0899 -0.0862 0.1162 0.071 Uiso 1 1 calc R . . H(54B) H 0.0062 -0.1324 0.1986 0.071 Uiso 1 1 calc R . . H(54C) H 0.1820 -0.1156 0.2331 0.071 Uiso 1 1 calc R . . H(81A) H 0.7427 0.2071 0.0551 0.061 Uiso 1 1 calc R . . H(81B) H 0.6287 0.0624 -0.0346 0.061 Uiso 1 1 calc R . . H(81C) H 0.6397 0.1260 0.1061 0.061 Uiso 1 1 calc R . . H(91A) H 0.3484 0.0468 -0.2436 0.072 Uiso 1 1 calc R . . H(91B) H 0.5175 0.0619 -0.2374 0.072 Uiso 1 1 calc R . . H(91C) H 0.4122 0.1277 -0.3168 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(2) 0.0241(9) 0.0358(11) 0.0250(9) -0.0002(8) 0.0058(8) 0.0172(9) O(6) 0.0326(11) 0.0457(13) 0.0284(10) 0.0050(9) 0.0068(9) 0.0147(9) C(1) 0.0289(7) 0.0283(7) 0.0255(7) 0.0086(6) 0.0080(6) 0.0092(6) C(2) 0.0257(7) 0.0304(7) 0.0293(7) 0.0078(6) 0.0070(6) 0.0083(6) C(3) 0.0283(7) 0.0311(7) 0.0248(7) 0.0120(6) 0.0048(6) 0.0049(6) C(4) 0.0335(8) 0.0357(8) 0.0238(7) 0.0136(6) 0.0092(6) 0.0113(6) C(5) 0.0278(7) 0.0299(7) 0.0263(7) 0.0092(6) 0.0091(6) 0.0099(6) C(6) 0.0266(7) 0.0288(7) 0.0251(7) 0.0075(6) 0.0063(5) 0.0090(6) C(7) 0.0273(7) 0.0292(7) 0.0259(7) 0.0047(6) 0.0071(6) 0.0096(6) C(8) 0.0316(8) 0.0334(8) 0.0300(7) 0.0067(6) 0.0098(6) 0.0123(6) C(9) 0.0376(8) 0.0390(8) 0.0316(8) 0.0080(7) 0.0142(6) 0.0152(7) C(10) 0.0360(8) 0.0336(8) 0.0301(7) 0.0038(6) 0.0074(6) 0.0125(6) C(11) 0.0487(10) 0.0462(10) 0.0363(8) 0.0104(8) 0.0084(7) 0.0208(8) C(12) 0.0445(10) 0.0544(11) 0.0523(10) 0.0137(8) 0.0053(8) 0.0324(9) C(13) 0.0388(9) 0.0522(10) 0.0600(11) 0.0189(8) 0.0153(8) 0.0287(9) C(14) 0.0353(8) 0.0415(9) 0.0408(9) 0.0110(7) 0.0115(7) 0.0168(7) C(15) 0.0288(7) 0.0281(7) 0.0292(7) 0.0027(6) 0.0047(6) 0.0100(6) C(31) 0.0300(8) 0.0414(9) 0.0255(7) 0.0122(7) 0.0011(6) 0.0045(6) C(32) 0.0303(13) 0.0446(15) 0.0340(13) 0.0144(11) 0.0065(10) 0.0102(11) C(33) 0.0429(15) 0.0351(13) 0.0390(14) 0.0076(11) -0.0005(11) 0.0031(11) C(34) 0.0384(13) 0.0621(17) 0.0241(11) 0.0130(12) 0.0045(9) 0.0169(11) C(35) 0.039(3) 0.046(3) 0.047(3) 0.009(3) -0.009(3) 0.011(3) C(36) 0.048(3) 0.067(4) 0.029(3) 0.014(3) 0.003(2) -0.002(3) C(37) 0.035(3) 0.072(4) 0.042(3) -0.013(3) -0.012(2) 0.025(3) C(51) 0.0319(8) 0.0437(9) 0.0351(8) 0.0075(7) 0.0130(6) 0.0194(7) C(52) 0.0591(12) 0.0765(14) 0.0443(10) 0.0006(10) 0.0231(9) 0.0292(10) C(53) 0.0319(9) 0.0626(12) 0.0668(12) 0.0138(8) 0.0213(8) 0.0307(10) C(54) 0.0429(10) 0.0406(9) 0.0545(11) 0.0020(8) 0.0127(8) 0.0199(8) C(81) 0.0399(9) 0.0455(9) 0.0411(9) 0.0182(7) 0.0162(7) 0.0179(7) C(91) 0.0583(11) 0.0515(10) 0.0320(8) 0.0149(9) 0.0175(8) 0.0116(8) # 10. 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 O(2) C(2) 1.314(2) . ? O(6) C(6) 1.356(2) . ? C(1) C(6) 1.3972(19) . ? C(1) C(2) 1.4042(19) . ? C(1) C(7) 1.4873(18) . ? C(2) C(3) 1.391(2) . ? C(3) C(4) 1.398(2) . ? C(3) C(31) 1.5437(19) . ? C(4) C(5) 1.3986(19) . ? C(5) C(6) 1.3939(19) . ? C(5) C(51) 1.539(2) . ? C(7) C(8) 1.357(2) . ? C(7) C(15) 1.4770(19) . ? C(8) C(81) 1.494(2) . ? C(8) C(9) 1.513(2) . ? C(9) C(10) 1.512(2) . ? C(9) C(91) 1.532(2) . ? C(10) C(11) 1.384(2) . ? C(10) C(15) 1.402(2) . ? C(11) C(12) 1.398(3) . ? C(12) C(13) 1.376(3) . ? C(13) C(14) 1.395(2) . ? C(14) C(15) 1.393(2) . ? C(31) C(35) 1.410(6) . ? C(31) C(36) 1.473(6) . ? C(31) C(33) 1.476(3) . ? C(31) C(32) 1.534(3) . ? C(31) C(34) 1.601(3) . ? C(31) C(37) 1.705(6) . ? C(51) C(52) 1.522(2) . ? C(51) C(53) 1.534(2) . ? C(51) C(54) 1.539(2) . ? 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 C(6) C(1) C(2) 119.08(12) . . ? C(6) C(1) C(7) 119.80(12) . . ? C(2) C(1) C(7) 121.09(12) . . ? O(2) C(2) C(3) 115.91(14) . . ? O(2) C(2) C(1) 122.59(14) . . ? C(3) C(2) C(1) 121.49(13) . . ? C(2) C(3) C(4) 117.11(12) . . ? C(2) C(3) C(31) 121.59(13) . . ? C(4) C(3) C(31) 121.28(13) . . ? C(3) C(4) C(5) 123.69(13) . . ? C(6) C(5) C(4) 117.10(13) . . ? C(6) C(5) C(51) 120.61(12) . . ? C(4) C(5) C(51) 122.26(12) . . ? O(6) C(6) C(5) 119.08(14) . . ? O(6) C(6) C(1) 119.28(14) . . ? C(5) C(6) C(1) 121.52(12) . . ? C(8) C(7) C(15) 109.11(12) . . ? C(8) C(7) C(1) 126.53(13) . . ? C(15) C(7) C(1) 124.34(13) . . ? C(7) C(8) C(81) 128.17(14) . . ? C(7) C(8) C(9) 110.81(13) . . ? C(81) C(8) C(9) 121.02(13) . . ? C(10) C(9) C(8) 102.48(12) . . ? C(10) C(9) C(91) 113.15(13) . . ? C(8) C(9) C(91) 112.45(13) . . ? C(11) C(10) C(15) 120.62(16) . . ? C(11) C(10) C(9) 129.97(15) . . ? C(15) C(10) C(9) 109.40(12) . . ? C(10) C(11) C(12) 118.65(16) . . ? C(13) C(12) C(11) 120.82(15) . . ? C(12) C(13) C(14) 121.02(17) . . ? C(15) C(14) C(13) 118.52(16) . . ? C(14) C(15) C(10) 120.34(14) . . ? C(14) C(15) C(7) 131.49(14) . . ? C(10) C(15) C(7) 108.14(13) . . ? C(35) C(31) C(36) 118.3(4) . . ? C(35) C(31) C(33) 136.3(3) . . ? C(36) C(31) C(33) 55.6(3) . . ? C(35) C(31) C(32) 37.5(3) . . ? C(36) C(31) C(32) 138.8(3) . . ? C(33) C(31) C(32) 113.72(19) . . ? C(35) C(31) C(3) 110.1(2) . . ? C(36) C(31) C(3) 110.8(3) . . ? C(33) C(31) C(3) 111.66(15) . . ? C(32) C(31) C(3) 109.83(14) . . ? C(35) C(31) C(34) 69.3(4) . . ? C(36) C(31) C(34) 54.0(3) . . ? C(33) C(31) C(34) 106.31(17) . . ? C(32) C(31) C(34) 104.35(17) . . ? C(3) C(31) C(34) 110.65(14) . . ? C(35) C(31) C(37) 106.0(4) . . ? C(36) C(31) C(37) 103.0(4) . . ? C(33) C(31) C(37) 48.8(3) . . ? C(32) C(31) C(37) 70.6(3) . . ? C(3) C(31) C(37) 107.8(2) . . ? C(34) C(31) C(37) 140.4(2) . . ? C(52) C(51) C(53) 107.31(15) . . ? C(52) C(51) C(5) 112.35(13) . . ? C(53) C(51) C(5) 110.32(12) . . ? C(52) C(51) C(54) 108.31(14) . . ? C(53) C(51) C(54) 109.69(14) . . ? C(5) C(51) C(54) 108.82(13) . . ? data_LTTM1P _database_code_CSD 218471 _audit_creation_date 26-09-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C26 H34 O1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 362.56 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 41.2752(17) _cell_length_b 6.1782(3) _cell_length_c 18.8466(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.707(2) _cell_angle_gamma 90.00 _cell_volume 4433.5(7) _cell_measurement_reflns_used 9394 _cell_measurement_theta_min 5 _cell_measurement_theta_max 22 _cell_formula_units_z 8 _exptl_crystal_density_diffrn 1.09 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.059 _cell_measurement_temperature 150 _exptl_crystal_F_000 1584 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.9728 _exptl_absorpt_correction_T_max 0.9867 _diffrn_reflns_number 9394 _diffrn_measured_fraction_theta_max 0.9948 _diffrn_reflns_theta_full 22.5 _diffrn_measured_fraction_theta_full 0.9948 _reflns_number_total 2830 _reflns_number_gt 2479 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 22.42 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_max 19 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.73' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.061 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.000 _refine_ls_wR_factor_gt 0.118 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 2828 _refine_ls_number_parameters 295 _refine_ls_number_restraints 15 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0460P)^2^+2.5615P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.15 _refine_diff_density_min -0.15 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(11) O 0.15510(8) 0.0006(5) 0.17476(17) 0.0460(8) Uani 0.50 1 d P . . O(12) O 0.12449(8) 0.2963(5) -0.06924(16) 0.0398(7) Uani 0.50 1 d P . . C(1) C 0.17723(6) 0.1166(4) 0.05948(11) 0.0369(6) Uani 1 1 d . . . C(2) C 0.18789(6) -0.0428(4) 0.02431(12) 0.0403(6) Uani 1 1 d . . . C(3) C 0.22670(6) -0.0280(4) 0.04430(13) 0.0431(6) Uani 1 1 d . . . C(4) C 0.23757(6) 0.1663(4) 0.09530(12) 0.0384(6) Uani 1 1 d . . . C(5) C 0.27061(6) 0.2600(4) 0.12965(13) 0.0449(6) Uani 1 1 d . . . C(6) C 0.27296(7) 0.4452(4) 0.17386(13) 0.0494(7) Uani 1 1 d . . . C(7) C 0.24412(6) 0.5269(4) 0.18487(13) 0.0467(6) Uani 1 1 d . . . C(8) C 0.21100(6) 0.4344(4) 0.15171(12) 0.0411(6) Uani 1 1 d . . . C(9) C 0.20803(6) 0.2513(3) 0.10522(11) 0.0355(5) Uani 1 1 d . . . C(11) C 0.14075(6) 0.1515(4) 0.05379(12) 0.0392(6) Uani 1 1 d . . . C(12) C 0.13112(6) 0.0852(4) 0.11380(12) 0.0414(6) Uani 1 1 d . . . C(13) C 0.09754(6) 0.1210(4) 0.11216(12) 0.0429(6) Uani 1 1 d . . . C(14) C 0.07410(6) 0.2299(4) 0.04851(13) 0.0438(6) Uani 1 1 d . . . C(15) C 0.08208(6) 0.2988(4) -0.01353(12) 0.0420(6) Uani 1 1 d . A . C(16) C 0.11581(6) 0.2537(4) -0.00982(12) 0.0405(6) Uani 1 1 d . . . C(21) C 0.16561(8) -0.2152(4) -0.02660(15) 0.0588(7) Uani 1 1 d . . . C(51) C 0.30205(7) 0.1642(5) 0.11969(15) 0.0609(8) Uani 1 1 d . . . C(81) C 0.18080(7) 0.5270(4) 0.16760(14) 0.0539(7) Uani 1 1 d . . . C(131) C 0.08726(6) 0.0390(4) 0.17779(14) 0.0510(7) Uani 1 1 d . . . C(132) C 0.05015(7) 0.1063(5) 0.16671(16) 0.0701(9) Uani 1 1 d . . . C(133) C 0.11198(8) 0.1369(6) 0.25482(14) 0.0688(9) Uani 1 1 d . . . C(134) C 0.08988(9) -0.2075(5) 0.18084(18) 0.0743(9) Uani 1 1 d . . . C(151) C 0.05458(6) 0.4174(4) -0.08181(13) 0.0526(7) Uani 1 1 d D . . C(152) C 0.04777(18) 0.6579(10) -0.0509(4) 0.068(2) Uani 0.449(5) 1 d PD A 1 C(153) C 0.02026(17) 0.3139(15) -0.1118(4) 0.073(2) Uani 0.449(5) 1 d PD A 1 C(154) C 0.06707(18) 0.4840(14) -0.1456(4) 0.072(2) Uani 0.449(5) 1 d PD A 1 C(155) C 0.02009(14) 0.4369(12) -0.0723(4) 0.0661(18) Uani 0.551(5) 1 d PD A 2 C(156) C 0.04587(13) 0.2571(9) -0.1549(2) 0.0652(18) Uani 0.551(5) 1 d PD A 2 C(157) C 0.06820(14) 0.6214(9) -0.0947(3) 0.0680(19) Uani 0.551(5) 1 d PD A 2 H(6) H 0.2945 0.5152 0.1964 0.059 Uiso 1 1 calc R . . H(7) H 0.2470 0.6487 0.2157 0.056 Uiso 1 1 calc R . . H(11) H 0.1727 -0.0248 0.1662 0.069 Uiso 0.50 1 calc PR . . H(12) H 0.1447 0.2568 -0.0594 0.060 Uiso 0.50 1 calc PR . . H(14) H 0.0517 0.2586 0.0471 0.053 Uiso 1 1 calc R . . H(3A) H 0.2386 -0.1570 0.0711 0.052 Uiso 1 1 calc R . . H(3B) H 0.2317 -0.0086 -0.0015 0.052 Uiso 1 1 calc R . . H(13A) H 0.0486 0.2613 0.1660 0.105 Uiso 1 1 calc R . . H(13B) H 0.0446 0.0506 0.2083 0.105 Uiso 1 1 calc R . . H(13C) H 0.0338 0.0493 0.1189 0.105 Uiso 1 1 calc R . . H(13D) H 0.1357 0.0930 0.2652 0.103 Uiso 1 1 calc R . . H(13E) H 0.1052 0.0869 0.2954 0.103 Uiso 1 1 calc R . . H(13F) H 0.1104 0.2920 0.2519 0.103 Uiso 1 1 calc R . . H(13G) H 0.0745 -0.2668 0.1324 0.111 Uiso 1 1 calc R . . H(13H) H 0.0832 -0.2607 0.2210 0.111 Uiso 1 1 calc R . . H(13I) H 0.1136 -0.2502 0.1910 0.111 Uiso 1 1 calc R . . H(15A) H 0.0311 0.7373 -0.0929 0.102 Uiso 0.449(5) 1 calc PR A 1 H(15B) H 0.0695 0.7364 -0.0306 0.102 Uiso 0.449(5) 1 calc PR A 1 H(15C) H 0.0388 0.6390 -0.0113 0.102 Uiso 0.449(5) 1 calc PR A 1 H(15D) H 0.0041 0.4016 -0.1521 0.110 Uiso 0.449(5) 1 calc PR A 1 H(15E) H 0.0118 0.2981 -0.0712 0.110 Uiso 0.449(5) 1 calc PR A 1 H(15F) H 0.0222 0.1739 -0.1320 0.110 Uiso 0.449(5) 1 calc PR A 1 H(15G) H 0.0724 0.3568 -0.1683 0.107 Uiso 0.449(5) 1 calc PR A 1 H(15H) H 0.0877 0.5722 -0.1241 0.107 Uiso 0.449(5) 1 calc PR A 1 H(15I) H 0.0489 0.5647 -0.1843 0.107 Uiso 0.449(5) 1 calc PR A 1 H(15J) H 0.0033 0.5086 -0.1164 0.099 Uiso 0.551(5) 1 calc PR A 2 H(15K) H 0.0234 0.5194 -0.0269 0.099 Uiso 0.551(5) 1 calc PR A 2 H(15L) H 0.0116 0.2951 -0.0676 0.099 Uiso 0.551(5) 1 calc PR A 2 H(15M) H 0.0367 0.1231 -0.1447 0.098 Uiso 0.551(5) 1 calc PR A 2 H(15N) H 0.0670 0.2294 -0.1634 0.098 Uiso 0.551(5) 1 calc PR A 2 H(15O) H 0.0288 0.3237 -0.1998 0.098 Uiso 0.551(5) 1 calc PR A 2 H(15P) H 0.0508 0.6931 -0.1378 0.102 Uiso 0.551(5) 1 calc PR A 2 H(15Q) H 0.0889 0.5968 -0.1053 0.102 Uiso 0.551(5) 1 calc PR A 2 H(15R) H 0.0741 0.7103 -0.0497 0.102 Uiso 0.551(5) 1 calc PR A 2 H(21A) H 0.1418 -0.1981 -0.0310 0.088 Uiso 1 1 calc R . . H(21B) H 0.1742 -0.3546 -0.0050 0.088 Uiso 1 1 calc R . . H(21C) H 0.1665 -0.2041 -0.0766 0.088 Uiso 1 1 calc R . . H(51A) H 0.3222 0.2546 0.1448 0.091 Uiso 1 1 calc R . . H(51B) H 0.2976 0.1547 0.0659 0.091 Uiso 1 1 calc R . . H(51C) H 0.3065 0.0221 0.1420 0.091 Uiso 1 1 calc R . . H(81A) H 0.1886 0.6524 0.1998 0.081 Uiso 1 1 calc R . . H(81B) H 0.1723 0.4205 0.1932 0.081 Uiso 1 1 calc R . . H(81C) H 0.1623 0.5671 0.1200 0.081 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(11) 0.047(2) 0.060(2) 0.0376(18) 0.0158(17) 0.0226(16) 0.0128(15) O(12) 0.0359(18) 0.0537(19) 0.0330(16) 0.0049(15) 0.0167(14) 0.0105(14) C(1) 0.0400(13) 0.0459(13) 0.0273(11) 0.0038(10) 0.0159(10) 0.0036(10) C(2) 0.0507(15) 0.0428(13) 0.0311(12) 0.0029(11) 0.0198(11) 0.0010(10) C(3) 0.0528(16) 0.0467(14) 0.0371(13) 0.0135(11) 0.0255(11) 0.0081(11) C(4) 0.0423(14) 0.0452(13) 0.0311(12) 0.0064(11) 0.0178(10) 0.0093(10) C(5) 0.0387(15) 0.0615(16) 0.0372(13) 0.0062(12) 0.0174(11) 0.0176(12) C(6) 0.0461(15) 0.0575(16) 0.0402(14) -0.0084(12) 0.0119(11) 0.0080(12) C(7) 0.0525(16) 0.0469(14) 0.0379(13) -0.0030(12) 0.0145(12) 0.0012(11) C(8) 0.0456(15) 0.0449(14) 0.0327(12) 0.0038(11) 0.0148(11) 0.0018(11) C(9) 0.0382(13) 0.0418(13) 0.0279(11) 0.0048(10) 0.0143(10) 0.0062(10) C(11) 0.0384(13) 0.0473(14) 0.0327(12) -0.0004(10) 0.0147(11) -0.0060(10) C(12) 0.0408(14) 0.0532(14) 0.0314(13) 0.0038(11) 0.0154(11) -0.0003(11) C(13) 0.0445(15) 0.0528(15) 0.0352(13) 0.0007(11) 0.0195(11) 0.0006(11) C(14) 0.0367(14) 0.0583(15) 0.0389(13) 0.0008(11) 0.0173(11) -0.0015(11) C(15) 0.0397(14) 0.0557(15) 0.0302(12) 0.0011(11) 0.0131(10) 0.0002(10) C(16) 0.0412(14) 0.0517(14) 0.0299(12) -0.0016(11) 0.0153(11) -0.0023(10) C(21) 0.076(2) 0.0528(16) 0.0490(15) -0.0014(14) 0.0263(14) -0.0098(12) C(51) 0.0446(16) 0.089(2) 0.0541(16) 0.0092(14) 0.0245(13) 0.0152(14) C(81) 0.0574(17) 0.0557(16) 0.0487(15) 0.0065(13) 0.0207(13) -0.0142(12) C(131) 0.0490(16) 0.0681(18) 0.0449(14) 0.0037(13) 0.0282(12) 0.0086(12) C(132) 0.0627(19) 0.098(2) 0.0644(18) 0.0032(16) 0.0409(15) 0.0158(16) C(133) 0.072(2) 0.102(2) 0.0403(15) 0.0051(17) 0.0305(14) 0.0043(15) C(134) 0.102(3) 0.069(2) 0.075(2) 0.0045(17) 0.0595(19) 0.0177(16) C(151) 0.0403(15) 0.0783(19) 0.0372(13) 0.0066(13) 0.0126(11) 0.0111(13) C(152) 0.074(5) 0.068(4) 0.057(4) 0.020(4) 0.019(3) 0.014(3) C(153) 0.052(4) 0.095(6) 0.055(5) -0.008(4) 0.002(4) 0.012(4) C(154) 0.074(5) 0.096(6) 0.041(4) 0.013(4) 0.020(3) 0.022(4) C(155) 0.048(3) 0.090(5) 0.056(4) 0.027(3) 0.016(3) 0.019(3) C(156) 0.051(3) 0.095(4) 0.037(3) 0.015(3) 0.004(2) -0.005(2) C(157) 0.065(4) 0.069(4) 0.068(4) 0.016(3) 0.024(3) 0.028(3) # 10. 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 O(11) C(12) 1.302(4) . ? O(12) C(16) 1.327(3) . ? C(1) C(2) 1.352(3) . ? C(1) C(11) 1.483(3) . ? C(1) C(9) 1.485(3) . ? C(2) C(21) 1.490(3) . ? C(2) C(3) 1.500(3) . ? C(3) C(4) 1.495(3) . ? C(4) C(5) 1.390(3) . ? C(4) C(9) 1.404(3) . ? C(5) C(6) 1.397(3) . ? C(5) C(51) 1.502(3) . ? C(6) C(7) 1.380(3) . ? C(7) C(8) 1.388(3) . ? C(8) C(9) 1.407(3) . ? C(8) C(81) 1.503(3) . ? C(11) C(16) 1.394(3) . ? C(11) C(12) 1.397(3) . ? C(12) C(13) 1.392(3) . ? C(13) C(14) 1.390(3) . ? C(13) C(131) 1.540(3) . ? C(14) C(15) 1.398(3) . ? C(15) C(16) 1.395(3) . ? C(15) C(151) 1.534(3) . ? C(131) C(132) 1.522(4) . ? C(131) C(134) 1.526(4) . ? C(131) C(133) 1.540(4) . ? C(151) C(157) 1.438(6) . ? C(151) C(153) 1.455(7) . ? C(151) C(155) 1.506(5) . ? C(151) C(154) 1.536(6) . ? C(151) C(156) 1.620(5) . ? C(151) C(152) 1.659(7) . ? 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 C(2) C(1) C(11) 125.7(2) . . ? C(2) C(1) C(9) 109.0(2) . . ? C(11) C(1) C(9) 125.33(18) . . ? C(1) C(2) C(21) 126.9(2) . . ? C(1) C(2) C(3) 110.5(2) . . ? C(21) C(2) C(3) 122.6(2) . . ? C(4) C(3) C(2) 103.68(17) . . ? C(5) C(4) C(9) 121.9(2) . . ? C(5) C(4) C(3) 129.1(2) . . ? C(9) C(4) C(3) 108.99(19) . . ? C(4) C(5) C(6) 116.6(2) . . ? C(4) C(5) C(51) 121.2(2) . . ? C(6) C(5) C(51) 122.2(2) . . ? C(7) C(6) C(5) 121.6(2) . . ? C(6) C(7) C(8) 122.6(2) . . ? C(7) C(8) C(9) 116.4(2) . . ? C(7) C(8) C(81) 120.1(2) . . ? C(9) C(8) C(81) 123.4(2) . . ? C(4) C(9) C(8) 120.8(2) . . ? C(4) C(9) C(1) 107.81(18) . . ? C(8) C(9) C(1) 131.4(2) . . ? C(16) C(11) C(12) 118.8(2) . . ? C(16) C(11) C(1) 121.33(19) . . ? C(12) C(11) C(1) 119.80(19) . . ? O(11) C(12) C(13) 119.7(2) . . ? O(11) C(12) C(11) 118.4(2) . . ? C(13) C(12) C(11) 121.8(2) . . ? C(14) C(13) C(12) 116.9(2) . . ? C(14) C(13) C(131) 122.5(2) . . ? C(12) C(13) C(131) 120.7(2) . . ? C(13) C(14) C(15) 124.0(2) . . ? C(16) C(15) C(14) 116.7(2) . . ? C(16) C(15) C(151) 122.57(19) . . ? C(14) C(15) C(151) 120.7(2) . . ? O(12) C(16) C(11) 117.7(2) . . ? O(12) C(16) C(15) 120.5(2) . . ? C(11) C(16) C(15) 121.7(2) . . ? C(132) C(131) C(134) 109.3(2) . . ? C(132) C(131) C(133) 106.7(2) . . ? C(134) C(131) C(133) 110.2(2) . . ? C(132) C(131) C(13) 112.0(2) . . ? C(134) C(131) C(13) 108.7(2) . . ? C(133) C(131) C(13) 109.9(2) . . ? C(157) C(151) C(153) 134.8(4) . . ? C(157) C(151) C(155) 113.5(4) . . ? C(153) C(151) C(155) 42.1(4) . . ? C(157) C(151) C(15) 110.5(3) . . ? C(153) C(151) C(15) 114.2(3) . . ? C(155) C(151) C(15) 111.4(3) . . ? C(157) C(151) C(154) 50.3(4) . . ? C(153) C(151) C(154) 112.6(5) . . ? C(155) C(151) C(154) 133.6(4) . . ? C(15) C(151) C(154) 114.9(3) . . ? C(157) C(151) C(156) 111.4(4) . . ? C(153) C(151) C(156) 62.4(5) . . ? C(155) C(151) C(156) 103.9(4) . . ? C(15) C(151) C(156) 105.7(2) . . ? C(154) C(151) C(156) 62.0(4) . . ? C(157) C(151) C(152) 53.5(4) . . ? C(153) C(151) C(152) 105.0(5) . . ? C(155) C(151) C(152) 65.8(4) . . ? C(15) C(151) C(152) 107.7(3) . . ? C(154) C(151) C(152) 100.9(4) . . ? C(156) C(151) C(152) 146.5(3) . . ? #============================================================================== data_MT38H _database_code_CSD 218472 _audit_creation_date 29-01-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C31 H35 Cl2 O Ti' _chemical_formula_structural ? _chemical_formula_weight 542.43 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/n 1' 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 12.2422(4) _cell_length_b 12.6093(4) _cell_length_c 18.9505(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.5167(19) _cell_angle_gamma 90.00 _cell_volume 2855.8(3) _cell_measurement_reflns_used 24792 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.505 _cell_measurement_temperature 203 _exptl_crystal_F_000 1140 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6512 _exptl_absorpt_correction_T_max 0.9389 _diffrn_reflns_number 24792 _reflns_number_total 5004 _reflns_number_gt 4070 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.47 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 26 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.111 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 5004 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+1.4369P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.44 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ti 0.07043(4) 0.03959(3) 0.36702(2) 0.03313(14) Uani ? Cl(1) -0.09534(6) 0.05894(8) 0.39953(4) 0.0658(3) Uani ? Cl(2) 0.09958(8) -0.13546(5) 0.38727(4) 0.0616(3) Uani ? O(1) 0.03549(13) 0.05251(12) 0.27095(8) 0.0341(4) Uani ? C(1) 0.1384(3) 0.1502(3) 0.46750(15) 0.0598(9) Uani ? C(2) 0.2150(2) 0.0691(2) 0.46980(14) 0.0507(8) Uani ? C(3) 0.2605(2) 0.0768(2) 0.40846(14) 0.0436(8) Uani ? C(4) 0.2125(2) 0.1638(2) 0.36784(14) 0.0451(8) Uani ? C(5) 0.1356(3) 0.2090(2) 0.40352(18) 0.0576(9) Uani ? C(11) 0.04170(18) 0.08748(18) 0.20329(11) 0.0296(6) Uani ? C(12) 0.14035(18) 0.07012(17) 0.17917(11) 0.0284(6) Uani ? C(13) 0.14885(18) 0.11011(17) 0.11182(11) 0.0301(6) Uani ? C(14) 0.06109(18) 0.16359(18) 0.06775(11) 0.0316(6) Uani ? C(15) -0.03692(19) 0.1750(2) 0.09303(12) 0.0367(7) Uani ? C(16) -0.05159(18) 0.1379(2) 0.15940(12) 0.0353(6) Uani ? C(121) 0.23509(18) 0.00728(18) 0.22168(11) 0.0298(6) Uani ? C(122) 0.2308(2) -0.09235(19) 0.24552(13) 0.0400(7) Uani ? C(123) 0.3428(2) -0.1285(2) 0.28757(14) 0.0467(8) Uani ? C(124) 0.4152(2) -0.03362(19) 0.28501(12) 0.0372(7) Uani ? C(125) 0.5270(2) -0.0148(2) 0.31642(13) 0.0470(8) Uani ? C(126) 0.5739(2) 0.0816(3) 0.30534(14) 0.0503(8) Uani ? C(127) 0.5109(2) 0.1594(2) 0.26343(14) 0.0472(8) Uani ? C(128) 0.39838(19) 0.14288(19) 0.23242(12) 0.0354(6) Uani ? C(129) 0.35045(18) 0.04600(17) 0.24401(11) 0.0300(6) Uani ? C(141) 0.0660(2) 0.2085(2) -0.00682(12) 0.0382(7) Uani ? C(142) 0.1767(3) 0.1866(3) -0.02683(16) 0.0709(12) Uani ? C(143) -0.0290(3) 0.1628(3) -0.06383(14) 0.0702(12) Uani ? C(144) 0.0514(3) 0.3299(2) -0.00491(16) 0.0632(10) Uani ? C(161) -0.1644(2) 0.1508(2) 0.18138(13) 0.0462(8) Uani ? C(162) -0.1523(2) 0.2263(2) 0.24568(16) 0.0545(9) Uani ? C(163) -0.2067(2) 0.0409(3) 0.19863(16) 0.0558(9) Uani ? C(164) -0.2541(2) 0.1989(3) 0.12026(17) 0.0743(11) Uani ? C(901) 0.4539(3) 0.0912(4) -0.0327(3) 0.0953(19) Uani ? C(902) 0.4626(3) 0.0751(4) 0.0402(3) 0.0883(16) Uani ? C(903) 0.5072(3) -0.0143(4) 0.0728(3) 0.0887(14) Uani ? H(1) 0.0962 0.1637 0.5018 0.0780 Uiso calc H(2) 0.2331 0.0182 0.5059 0.0660 Uiso calc H(3) 0.3138 0.0316 0.3967 0.0570 Uiso calc H(4) 0.2289 0.1874 0.3248 0.0590 Uiso calc H(5) 0.0905 0.2674 0.3880 0.0750 Uiso calc H(13) 0.2151 0.1006 0.0962 0.0390 Uiso calc H(15) -0.0967 0.2099 0.0635 0.0480 Uiso calc H(122) 0.1665 -0.1338 0.2371 0.0520 Uiso calc H(125) 0.5697 -0.0666 0.3446 0.0610 Uiso calc H(126) 0.6487 0.0945 0.3263 0.0650 Uiso calc H(127) 0.5443 0.2235 0.2559 0.0610 Uiso calc H(128) 0.3561 0.1953 0.2046 0.0460 Uiso calc H(12A) 0.3399 -0.1463 0.3369 0.0610 Uiso calc H(12B) 0.3694 -0.1895 0.2650 0.0610 Uiso calc H(14A) 0.2361 0.2174 0.0088 0.0920 Uiso calc H(14B) 0.1766 0.2171 -0.0733 0.0920 Uiso calc H(14C) 0.1879 0.1114 -0.0287 0.0920 Uiso calc H(14D) -0.0198 0.0874 -0.0666 0.0910 Uiso calc H(14E) -0.0282 0.1941 -0.1099 0.0910 Uiso calc H(14F) -0.0991 0.1780 -0.0511 0.0910 Uiso calc H(14G) -0.0184 0.3463 0.0078 0.0820 Uiso calc H(14H) 0.0518 0.3590 -0.0517 0.0820 Uiso calc H(14I) 0.1118 0.3600 0.0303 0.0820 Uiso calc H(16A) -0.0969 0.1992 0.2854 0.0710 Uiso calc H(16B) -0.2227 0.2324 0.2598 0.0710 Uiso calc H(16C) -0.1295 0.2949 0.2322 0.0710 Uiso calc H(16D) -0.2137 -0.0042 0.1571 0.0730 Uiso calc H(16E) -0.2783 0.0481 0.2110 0.0730 Uiso calc H(16F) -0.1545 0.0101 0.2385 0.0730 Uiso calc H(16G) -0.2307 0.2682 0.1085 0.0970 Uiso calc H(16H) -0.3236 0.2045 0.1358 0.0970 Uiso calc H(16I) -0.2642 0.1542 0.0784 0.0970 Uiso calc H(901) 0.4222 0.1532 -0.0546 0.1240 Uiso calc H(902) 0.4370 0.1272 0.0674 0.1150 Uiso calc H(903) 0.5119 -0.0242 0.1220 0.1150 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0388(3) 0.0391(3) 0.0219(2) -0.00339(18) 0.00749(17) 0.00296(17) Cl(1) 0.0470(4) 0.1121(7) 0.0433(4) 0.0006(4) 0.0209(3) 0.0156(4) Cl(2) 0.1026(6) 0.0386(4) 0.0444(4) -0.0044(4) 0.0175(4) 0.0073(3) O(1) 0.0341(8) 0.0440(9) 0.0242(8) -0.0049(7) 0.0061(6) 0.0055(7) C(1) 0.0603(18) 0.079(2) 0.0428(16) -0.0098(16) 0.0169(14) -0.0281(16) C(2) 0.0505(16) 0.0684(19) 0.0295(13) -0.0059(14) 0.0004(12) -0.0007(12) C(3) 0.0387(14) 0.0519(16) 0.0384(13) -0.0025(12) 0.0047(11) -0.0040(12) C(4) 0.0493(15) 0.0439(15) 0.0414(14) -0.0129(12) 0.0086(12) -0.0023(12) C(5) 0.0584(18) 0.0395(15) 0.073(2) 0.0005(13) 0.0101(15) -0.0139(15) C(11) 0.0316(12) 0.0357(12) 0.0203(10) -0.0084(10) 0.0029(9) 0.0037(9) C(12) 0.0316(12) 0.0290(11) 0.0227(10) -0.0073(9) 0.0016(9) -0.0013(9) C(13) 0.0314(12) 0.0333(12) 0.0254(11) -0.0051(9) 0.0060(9) 0.0000(9) C(14) 0.0328(12) 0.0385(13) 0.0222(11) -0.0090(10) 0.0032(9) 0.0012(9) C(15) 0.0274(12) 0.0503(15) 0.0294(12) -0.0028(10) -0.0003(9) 0.0098(11) C(16) 0.0275(11) 0.0498(14) 0.0273(11) -0.0076(10) 0.0031(9) 0.0048(10) C(121) 0.0355(12) 0.0316(12) 0.0219(10) 0.0002(10) 0.0055(9) -0.0004(9) C(122) 0.0498(15) 0.0319(13) 0.0361(13) -0.0038(11) 0.0047(11) 0.0004(11) C(123) 0.0629(17) 0.0336(13) 0.0398(14) 0.0097(12) 0.0026(12) 0.0024(11) C(124) 0.0425(14) 0.0398(13) 0.0294(12) 0.0091(11) 0.0079(10) -0.0043(10) C(125) 0.0431(15) 0.0638(18) 0.0324(13) 0.0222(13) 0.0046(11) -0.0059(12) C(126) 0.0319(13) 0.078(2) 0.0410(14) 0.0014(13) 0.0081(11) -0.0142(14) C(127) 0.0362(14) 0.0616(17) 0.0477(15) -0.0092(12) 0.0177(12) -0.0104(13) C(128) 0.0346(12) 0.0382(13) 0.0360(12) 0.0020(10) 0.0132(10) 0.0000(10) C(129) 0.0323(12) 0.0340(12) 0.0244(11) 0.0047(9) 0.0076(9) -0.0033(9) C(141) 0.0398(13) 0.0506(15) 0.0226(11) -0.0065(11) 0.0033(10) 0.0066(10) C(142) 0.069(2) 0.111(3) 0.0388(15) 0.0108(19) 0.0251(14) 0.0245(17) C(143) 0.078(2) 0.098(3) 0.0277(14) -0.0316(19) -0.0035(14) 0.0087(15) C(144) 0.089(2) 0.0606(19) 0.0419(16) -0.0072(17) 0.0184(15) 0.0133(14) C(161) 0.0283(12) 0.0737(19) 0.0374(13) -0.0024(12) 0.0089(10) 0.0154(13) C(162) 0.0484(16) 0.0631(18) 0.0572(18) 0.0081(14) 0.0229(14) 0.0140(15) C(163) 0.0363(14) 0.085(2) 0.0475(16) -0.0197(14) 0.0121(12) 0.0015(15) C(164) 0.0298(14) 0.133(3) 0.0596(19) 0.0100(17) 0.0089(13) 0.034(2) C(901) 0.048(2) 0.086(3) 0.156(5) -0.0031(19) 0.031(3) 0.007(3) C(902) 0.066(2) 0.085(3) 0.122(4) -0.010(2) 0.038(2) -0.036(3) C(903) 0.055(2) 0.114(3) 0.100(3) -0.013(2) 0.023(2) -0.016(3) # 10. 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_publ_flag Ti O(1) 1.7851(15) ? Ti Cl(2) 2.2554(8) ? Ti Cl(1) 2.2581(8) ? Ti C(5) 2.332(3) ? Ti C(3) 2.336(3) ? Ti C(4) 2.338(3) ? Ti C(2) 2.360(3) ? Ti C(1) 2.361(3) ? O(1) C(11) 1.374(2) ? C(1) C(2) 1.382(4) ? C(1) C(5) 1.415(4) ? C(2) C(3) 1.397(4) ? C(3) C(4) 1.394(4) ? C(4) C(5) 1.394(4) ? C(11) C(12) 1.398(3) ? C(11) C(16) 1.410(3) ? C(12) C(13) 1.397(3) ? C(12) C(121) 1.489(3) ? C(13) C(14) 1.385(3) ? C(14) C(15) 1.392(3) ? C(14) C(141) 1.535(3) ? C(15) C(16) 1.390(3) ? C(16) C(161) 1.536(3) ? C(121) C(122) 1.340(3) ? C(121) C(129) 1.467(3) ? C(122) C(123) 1.500(4) ? C(123) C(124) 1.496(4) ? C(124) C(125) 1.389(4) ? C(124) C(129) 1.404(3) ? C(125) C(126) 1.380(4) ? C(126) C(127) 1.386(4) ? C(127) C(128) 1.392(3) ? C(128) C(129) 1.393(3) ? C(141) C(142) 1.510(4) ? C(141) C(143) 1.519(3) ? C(141) C(144) 1.543(4) ? C(161) C(162) 1.528(4) ? C(161) C(164) 1.538(4) ? C(161) C(163) 1.539(4) ? C(901) C(903) 1.379(6) ? C(901) C(902) 1.377(6) ? C(902) C(903) 1.344(6) ? C(903) C(901) 1.379(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ti Cl(2) 104.89(6) ? O(1) Ti Cl(1) 103.74(6) ? Cl(2) Ti Cl(1) 100.24(4) ? O(1) Ti C(5) 102.12(10) ? Cl(2) Ti C(5) 144.54(8) ? Cl(1) Ti C(5) 95.17(8) ? O(1) Ti C(3) 109.00(8) ? Cl(2) Ti C(3) 91.73(7) ? Cl(1) Ti C(3) 140.80(7) ? C(5) Ti C(3) 57.60(10) ? O(1) Ti C(4) 87.66(8) ? Cl(2) Ti C(4) 124.35(7) ? Cl(1) Ti C(4) 129.58(7) ? C(5) Ti C(4) 34.74(10) ? C(3) Ti C(4) 34.70(9) ? O(1) Ti C(2) 142.97(9) ? Cl(2) Ti C(2) 87.21(8) ? Cl(1) Ti C(2) 108.38(7) ? C(5) Ti C(2) 57.55(11) ? C(3) Ti C(2) 34.60(9) ? C(4) Ti C(2) 57.66(10) ? O(1) Ti C(1) 137.15(10) ? Cl(2) Ti C(1) 115.19(9) ? Cl(1) Ti C(1) 84.07(8) ? C(5) Ti C(1) 35.09(11) ? C(3) Ti C(1) 57.25(10) ? C(4) Ti C(1) 57.82(10) ? C(2) Ti C(1) 34.03(10) ? C(11) O(1) Ti 158.73(14) ? C(2) C(1) C(5) 107.7(3) ? C(2) C(1) Ti 72.93(15) ? C(5) C(1) Ti 71.31(15) ? C(1) C(2) C(3) 108.2(3) ? C(1) C(2) Ti 73.04(15) ? C(3) C(2) Ti 71.77(15) ? C(4) C(3) C(2) 108.6(2) ? C(4) C(3) Ti 72.73(15) ? C(2) C(3) Ti 73.63(15) ? C(3) C(4) C(5) 107.5(3) ? C(3) C(4) Ti 72.57(15) ? C(5) C(4) Ti 72.37(16) ? C(4) C(5) C(1) 108.0(3) ? C(4) C(5) Ti 72.89(15) ? C(1) C(5) Ti 73.59(16) ? O(1) C(11) C(12) 118.78(19) ? O(1) C(11) C(16) 119.59(19) ? C(12) C(11) C(16) 121.63(19) ? C(11) C(12) C(13) 118.9(2) ? C(11) C(12) C(121) 122.22(19) ? C(13) C(12) C(121) 118.9(2) ? C(14) C(13) C(12) 121.7(2) ? C(13) C(14) C(15) 117.2(2) ? C(13) C(14) C(141) 123.7(2) ? C(15) C(14) C(141) 119.1(2) ? C(16) C(15) C(14) 124.5(2) ? C(15) C(16) C(11) 116.0(2) ? C(15) C(16) C(161) 120.7(2) ? C(11) C(16) C(161) 123.3(2) ? C(122) C(121) C(129) 108.7(2) ? C(122) C(121) C(12) 126.8(2) ? C(129) C(121) C(12) 124.55(19) ? C(121) C(122) C(123) 111.5(2) ? C(124) C(123) C(122) 102.7(2) ? C(125) C(124) C(129) 120.0(2) ? C(125) C(124) C(123) 131.1(2) ? C(129) C(124) C(123) 108.8(2) ? C(126) C(125) C(124) 119.3(2) ? C(125) C(126) C(127) 120.9(2) ? C(128) C(127) C(126) 120.8(3) ? C(127) C(128) C(129) 118.5(2) ? C(128) C(129) C(124) 120.5(2) ? C(128) C(129) C(121) 131.2(2) ? C(124) C(129) C(121) 108.3(2) ? C(142) C(141) C(143) 110.0(3) ? C(142) C(141) C(14) 112.3(2) ? C(143) C(141) C(14) 109.8(2) ? C(142) C(141) C(144) 107.6(2) ? C(143) C(141) C(144) 108.6(2) ? C(14) C(141) C(144) 108.5(2) ? C(162) C(161) C(16) 110.1(2) ? C(162) C(161) C(164) 106.5(3) ? C(16) C(161) C(164) 112.0(2) ? C(162) C(161) C(163) 111.8(2) ? C(16) C(161) C(163) 109.0(2) ? C(164) C(161) C(163) 107.3(2) ? C(903) C(901) C(902) 119.2(4) ? C(903) C(902) C(901) 121.4(4) ? C(902) C(903) C(901) 119.4(4) ? #============================================================================== data_LTTI31 _database_code_CSD 218473 #============================================================================== _audit_creation_date 28-10-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C29 H34 Cl2 O1 Ti1' _chemical_formula_moiety 'C29 H34 Cl2 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 517.40 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 13.1454(2) _cell_length_b 11.4807(2) _cell_length_c 18.2793(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.5146(8) _cell_angle_gamma 90.00 _cell_volume 2682.30(9) _cell_measurement_reflns_used 19312 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.534 _cell_measurement_temperature 150 _exptl_crystal_F_000 1088 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6608 _exptl_absorpt_correction_T_max 0.8295 _diffrn_reflns_number 19312 _diffrn_measured_fraction_theta_max 0.9813 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9813 _reflns_number_total 5981 _reflns_number_gt 5212 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 23 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.095 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 5967 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.7779P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.41 _refine_diff_density_min -0.49 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.20635(3) 0.22317(3) 0.218859(18) 0.01937(10) Uani 1 1 d . . . Cl(1) Cl 0.24851(4) 0.04009(4) 0.19187(3) 0.03017(13) Uani 1 1 d . . . Cl(2) Cl 0.29304(4) 0.23713(5) 0.34067(3) 0.03360(14) Uani 1 1 d . . . O(1) O 0.27896(10) 0.31772(11) 0.17256(7) 0.0183(3) Uani 1 1 d . . . C(1) C 0.05792(16) 0.3298(2) 0.16111(13) 0.0357(5) Uani 1 1 d . . . C(2) C 0.06833(18) 0.3373(2) 0.23931(14) 0.0386(6) Uani 1 1 d . . . C(3) C 0.05234(17) 0.2256(2) 0.26652(13) 0.0359(5) Uani 1 1 d . . . C(4) C 0.03411(16) 0.1491(2) 0.20557(12) 0.0320(5) Uani 1 1 d . . . C(5) C 0.03811(16) 0.2132(2) 0.14016(12) 0.0310(5) Uani 1 1 d . . . C(11) C 0.29603(13) 0.40152(15) 0.12331(10) 0.0165(4) Uani 1 1 d . . . C(12) C 0.26250(13) 0.37869(16) 0.04588(10) 0.0173(4) Uani 1 1 d . . . C(13) C 0.27604(14) 0.46386(16) -0.00528(10) 0.0201(4) Uani 1 1 d . . . C(14) C 0.32308(14) 0.57013(16) 0.01791(11) 0.0204(4) Uani 1 1 d . . . C(15) C 0.35780(14) 0.58818(16) 0.09485(11) 0.0204(4) Uani 1 1 d . . . C(16) C 0.34647(14) 0.50758(16) 0.14965(10) 0.0179(4) Uani 1 1 d . . . C(21) C 0.20916(14) 0.26918(16) 0.01558(10) 0.0168(4) Uani 1 1 d . . . C(22) C 0.25001(14) 0.16162(16) 0.01433(10) 0.0199(4) Uani 1 1 d . . . C(23) C 0.16725(15) 0.07802(17) -0.02669(11) 0.0227(4) Uani 1 1 d . . . C(24) C 0.07139(14) 0.15295(17) -0.04892(10) 0.0203(4) Uani 1 1 d . . . C(25) C -0.03118(15) 0.12780(18) -0.08551(11) 0.0260(4) Uani 1 1 d . . . C(26) C -0.10497(16) 0.21663(19) -0.09906(12) 0.0291(5) Uani 1 1 d . . . C(27) C -0.07733(16) 0.33023(19) -0.07697(12) 0.0275(4) Uani 1 1 d . . . C(28) C 0.02539(15) 0.35662(17) -0.04003(11) 0.0222(4) Uani 1 1 d . . . C(29) C 0.09872(14) 0.26750(16) -0.02506(10) 0.0172(4) Uani 1 1 d . . . C(141) C 0.33616(16) 0.66060(18) -0.04100(11) 0.0260(4) Uani 1 1 d . . . C(142) C 0.2295(2) 0.6843(3) -0.09374(16) 0.0530(7) Uani 1 1 d . . . C(143) C 0.4119(2) 0.6130(2) -0.08559(15) 0.0434(6) Uani 1 1 d . . . C(144) C 0.3789(2) 0.7763(2) -0.00485(15) 0.0424(6) Uani 1 1 d . . . C(161) C 0.38722(15) 0.53528(17) 0.23347(11) 0.0229(4) Uani 1 1 d . . . C(162) C 0.44615(18) 0.65178(18) 0.24550(13) 0.0339(5) Uani 1 1 d . . . C(163) C 0.29499(18) 0.54560(19) 0.27157(12) 0.0310(5) Uani 1 1 d . . . C(164) C 0.46432(16) 0.44071(18) 0.27139(12) 0.0291(5) Uani 1 1 d . . . C(221) C 0.36099(16) 0.12533(19) 0.04270(12) 0.0289(4) Uani 1 1 d . . . H(1) H 0.0634 0.3925 0.1284 0.043 Uiso 1 1 calc R . . H(2) H 0.0835 0.4061 0.2688 0.046 Uiso 1 1 calc R . . H(3) H 0.0537 0.2059 0.3172 0.043 Uiso 1 1 calc R . . H(4) H 0.0212 0.0679 0.2076 0.038 Uiso 1 1 calc R . . H(5) H 0.0290 0.1826 0.0908 0.037 Uiso 1 1 calc R . . H(13) H 0.2524 0.4488 -0.0576 0.024 Uiso 1 1 calc R . . H(15) H 0.3914 0.6600 0.1113 0.024 Uiso 1 1 calc R . . H(25) H -0.0508 0.0504 -0.1012 0.031 Uiso 1 1 calc R . . H(26) H -0.1753 0.1994 -0.1238 0.035 Uiso 1 1 calc R . . H(27) H -0.1285 0.3902 -0.0871 0.033 Uiso 1 1 calc R . . H(28) H 0.0449 0.4344 -0.0253 0.027 Uiso 1 1 calc R . . H(14A) H 0.2031 0.6127 -0.1208 0.079 Uiso 1 1 calc R . . H(14B) H 0.2366 0.7450 -0.1299 0.079 Uiso 1 1 calc R . . H(14C) H 0.1803 0.7104 -0.0643 0.079 Uiso 1 1 calc R . . H(14D) H 0.4810 0.6021 -0.0518 0.065 Uiso 1 1 calc R . . H(14E) H 0.4172 0.6683 -0.1254 0.065 Uiso 1 1 calc R . . H(14F) H 0.3859 0.5381 -0.1082 0.065 Uiso 1 1 calc R . . H(14G) H 0.3318 0.8067 0.0250 0.064 Uiso 1 1 calc R . . H(14H) H 0.3838 0.8324 -0.0443 0.064 Uiso 1 1 calc R . . H(14I) H 0.4486 0.7638 0.0279 0.064 Uiso 1 1 calc R . . H(16A) H 0.4731 0.6653 0.2995 0.051 Uiso 1 1 calc R . . H(16B) H 0.3984 0.7150 0.2240 0.051 Uiso 1 1 calc R . . H(16C) H 0.5046 0.6494 0.2206 0.051 Uiso 1 1 calc R . . H(16D) H 0.2564 0.4718 0.2663 0.047 Uiso 1 1 calc R . . H(16E) H 0.2482 0.6082 0.2476 0.047 Uiso 1 1 calc R . . H(16F) H 0.3216 0.5633 0.3251 0.047 Uiso 1 1 calc R . . H(16G) H 0.5245 0.4391 0.2483 0.044 Uiso 1 1 calc R . . H(16H) H 0.4294 0.3647 0.2649 0.044 Uiso 1 1 calc R . . H(16I) H 0.4883 0.4580 0.3252 0.044 Uiso 1 1 calc R . . H(22A) H 0.3904 0.1029 0.0002 0.043 Uiso 1 1 calc R . . H(22B) H 0.3643 0.0589 0.0768 0.043 Uiso 1 1 calc R . . H(22C) H 0.4013 0.1903 0.0698 0.043 Uiso 1 1 calc R . . H(23A) H 0.1867 0.0448 -0.0715 0.027 Uiso 1 1 calc R . . H(23B) H 0.1562 0.0137 0.0067 0.027 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.02307(19) 0.02015(18) 0.01546(18) -0.00267(13) 0.00567(13) 0.00117(13) Cl(1) 0.0318(3) 0.0201(2) 0.0373(3) -0.00185(19) 0.0053(2) -0.0007(2) Cl(2) 0.0425(3) 0.0414(3) 0.0155(2) -0.0070(2) 0.0039(2) 0.0027(2) O(1) 0.0228(6) 0.0177(6) 0.0141(6) -0.0026(5) 0.0036(5) -0.0008(5) C(1) 0.0244(11) 0.0417(14) 0.0425(13) 0.0077(9) 0.0110(9) 0.0132(11) C(2) 0.0303(12) 0.0393(13) 0.0493(15) 0.0037(10) 0.0159(10) -0.0125(11) C(3) 0.0305(12) 0.0547(15) 0.0274(12) -0.0029(10) 0.0165(9) -0.0027(10) C(4) 0.0253(10) 0.0404(13) 0.0332(12) -0.0090(9) 0.0127(9) -0.0011(10) C(5) 0.0207(10) 0.0473(14) 0.0252(11) -0.0019(9) 0.0061(8) -0.0002(10) C(11) 0.0167(8) 0.0163(9) 0.0169(9) -0.0006(7) 0.0046(7) 0.0006(7) C(12) 0.0178(9) 0.0164(9) 0.0183(9) -0.0010(7) 0.0052(7) -0.0007(7) C(13) 0.0225(9) 0.0217(9) 0.0161(9) -0.0017(7) 0.0046(7) 0.0004(7) C(14) 0.0178(9) 0.0203(9) 0.0238(10) 0.0007(7) 0.0064(7) 0.0043(8) C(15) 0.0186(9) 0.0161(9) 0.0259(10) -0.0023(7) 0.0043(7) -0.0011(7) C(16) 0.0172(9) 0.0164(9) 0.0193(9) -0.0006(7) 0.0028(7) -0.0026(7) C(21) 0.0208(9) 0.0195(9) 0.0106(8) -0.0035(7) 0.0049(7) -0.0012(7) C(22) 0.0228(9) 0.0223(10) 0.0144(9) -0.0011(7) 0.0041(7) -0.0003(7) C(23) 0.0282(10) 0.0170(9) 0.0231(10) -0.0028(7) 0.0062(8) -0.0033(8) C(24) 0.0239(9) 0.0211(9) 0.0170(9) -0.0037(7) 0.0072(7) -0.0026(7) C(25) 0.0274(10) 0.0256(10) 0.0253(10) -0.0098(8) 0.0072(8) -0.0065(8) C(26) 0.0213(10) 0.0380(12) 0.0279(11) -0.0058(9) 0.0054(8) -0.0033(9) C(27) 0.0220(10) 0.0329(11) 0.0280(11) 0.0027(8) 0.0064(8) -0.0024(9) C(28) 0.0241(10) 0.0216(9) 0.0215(10) -0.0006(8) 0.0069(7) -0.0031(8) C(29) 0.0206(9) 0.0192(9) 0.0123(8) -0.0032(7) 0.0050(7) -0.0021(7) C(141) 0.0274(10) 0.0236(10) 0.0277(11) -0.0018(8) 0.0077(8) 0.0078(8) C(142) 0.0430(14) 0.0552(17) 0.0538(17) -0.0068(12) -0.0028(12) 0.0350(14) C(143) 0.0570(16) 0.0373(13) 0.0457(14) -0.0034(11) 0.0317(12) 0.0084(11) C(144) 0.0590(16) 0.0259(12) 0.0459(15) -0.0076(11) 0.0199(12) 0.0099(10) C(161) 0.0280(10) 0.0188(9) 0.0194(9) -0.0031(8) 0.0005(7) -0.0046(7) C(162) 0.0432(13) 0.0225(11) 0.0298(11) -0.0090(9) -0.0038(9) -0.0057(9) C(163) 0.0425(13) 0.0296(11) 0.0216(10) -0.0004(9) 0.0090(9) -0.0084(9) C(164) 0.0303(11) 0.0256(11) 0.0255(11) -0.0037(8) -0.0055(8) -0.0012(8) C(221) 0.0271(10) 0.0270(11) 0.0311(11) 0.0029(8) 0.0036(8) -0.0002(9) # 10. 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_publ_flag Ti O(1) 1.7841(13) YES Ti Cl(1) 2.2574(6) YES Ti Cl(2) 2.2575(6) YES Ti C(1) 2.336(2) YES Ti C(2) 2.338(2) YES Ti C(5) 2.342(2) YES Ti C(4) 2.377(2) YES Ti C(3) 2.384(2) YES O(1) C(11) 1.371(2) YES C(1) C(5) 1.399(3) YES C(1) C(2) 1.406(3) YES C(2) C(3) 1.410(3) YES C(3) C(4) 1.394(3) YES C(4) C(5) 1.416(3) YES C(11) C(12) 1.405(2) YES C(11) C(16) 1.416(2) YES C(12) C(13) 1.393(3) YES C(12) C(21) 1.482(2) YES C(13) C(14) 1.389(3) YES C(14) C(15) 1.389(3) YES C(14) C(141) 1.534(3) YES C(15) C(16) 1.397(3) YES C(16) C(161) 1.533(3) YES C(21) C(22) 1.349(3) YES C(21) C(29) 1.468(2) YES C(22) C(221) 1.489(3) YES C(22) C(23) 1.512(3) YES C(23) C(24) 1.501(3) YES C(24) C(25) 1.388(3) YES C(24) C(29) 1.406(3) YES C(25) C(26) 1.389(3) YES C(26) C(27) 1.388(3) YES C(27) C(28) 1.395(3) YES C(28) C(29) 1.388(3) YES C(141) C(143) 1.527(3) YES C(141) C(142) 1.529(3) YES C(141) C(144) 1.531(3) YES C(161) C(164) 1.536(3) YES C(161) C(162) 1.536(3) YES C(161) C(163) 1.538(3) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ti Cl(1) 106.08(5) YES O(1) Ti Cl(2) 102.83(4) YES Cl(1) Ti Cl(2) 100.87(2) YES O(1) Ti C(1) 87.12(7) YES Cl(1) Ti C(1) 127.65(7) YES Cl(2) Ti C(1) 125.76(6) YES O(1) Ti C(2) 104.83(8) YES Cl(1) Ti C(2) 142.76(6) YES Cl(2) Ti C(2) 91.96(7) YES C(1) Ti C(2) 35.03(9) YES O(1) Ti C(5) 105.74(7) YES Cl(1) Ti C(5) 93.74(6) YES Cl(2) Ti C(5) 142.73(6) YES C(1) Ti C(5) 34.81(8) YES C(2) Ti C(5) 57.92(8) YES O(1) Ti C(4) 140.49(7) YES Cl(1) Ti C(4) 85.48(6) YES Cl(2) Ti C(4) 112.05(6) YES C(1) Ti C(4) 57.74(8) YES C(2) Ti C(4) 57.36(8) YES C(5) Ti C(4) 34.90(7) YES O(1) Ti C(3) 139.51(8) YES Cl(1) Ti C(3) 111.31(6) YES Cl(2) Ti C(3) 85.11(6) YES C(1) Ti C(3) 57.87(8) YES C(2) Ti C(3) 34.72(9) YES C(5) Ti C(3) 57.62(8) YES C(4) Ti C(3) 34.06(8) YES C(11) O(1) Ti 157.82(12) YES C(5) C(1) C(2) 107.7(2) YES C(5) C(1) Ti 72.85(12) YES C(2) C(1) Ti 72.57(13) YES C(1) C(2) C(3) 108.4(2) YES C(1) C(2) Ti 72.41(12) YES C(3) C(2) Ti 74.42(13) YES C(4) C(3) C(2) 107.6(2) YES C(4) C(3) Ti 72.71(12) YES C(2) C(3) Ti 70.86(12) YES C(3) C(4) C(5) 108.3(2) YES C(3) C(4) Ti 73.23(12) YES C(5) C(4) Ti 71.20(12) YES C(1) C(5) C(4) 107.9(2) YES C(1) C(5) Ti 72.34(12) YES C(4) C(5) Ti 73.90(12) YES O(1) C(11) C(12) 117.99(15) YES O(1) C(11) C(16) 121.02(15) YES C(12) C(11) C(16) 120.98(16) YES C(13) C(12) C(11) 119.08(16) YES C(13) C(12) C(21) 117.91(16) YES C(11) C(12) C(21) 122.97(16) YES C(14) C(13) C(12) 121.97(17) YES C(13) C(14) C(15) 117.24(17) YES C(13) C(14) C(141) 119.70(17) YES C(15) C(14) C(141) 123.06(17) YES C(14) C(15) C(16) 124.22(17) YES C(15) C(16) C(11) 116.46(16) YES C(15) C(16) C(161) 120.54(16) YES C(11) C(16) C(161) 123.00(16) YES C(22) C(21) C(29) 109.26(16) YES C(22) C(21) C(12) 128.86(16) YES C(29) C(21) C(12) 121.70(16) YES C(21) C(22) C(221) 127.72(17) YES C(21) C(22) C(23) 110.27(16) YES C(221) C(22) C(23) 121.87(17) YES C(24) C(23) C(22) 103.40(15) YES C(25) C(24) C(29) 119.54(18) YES C(25) C(24) C(23) 132.11(18) YES C(29) C(24) C(23) 108.34(16) YES C(24) C(25) C(26) 119.50(18) YES C(27) C(26) C(25) 120.88(19) YES C(26) C(27) C(28) 120.19(19) YES C(29) C(28) C(27) 118.97(18) YES C(28) C(29) C(24) 120.87(17) YES C(28) C(29) C(21) 130.46(17) YES C(24) C(29) C(21) 108.66(16) YES C(143) C(141) C(142) 110.1(2) YES C(143) C(141) C(144) 108.74(18) YES C(142) C(141) C(144) 107.9(2) YES C(143) C(141) C(14) 109.05(17) YES C(142) C(141) C(14) 109.05(17) YES C(144) C(141) C(14) 111.99(18) YES C(16) C(161) C(164) 110.12(16) YES C(16) C(161) C(162) 111.75(16) YES C(164) C(161) C(162) 107.07(16) YES C(16) C(161) C(163) 109.89(16) YES C(164) C(161) C(163) 110.92(17) YES C(162) C(161) C(163) 107.03(17) YES #============================================================================== data_LTTI30 _database_code_CSD 218474 _audit_creation_date 29-10-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C30 H36 Cl2 O1 Ti1' _chemical_formula_moiety 'C30 H36 Cl2 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 531.43 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 13.2652(2) _cell_length_b 11.7696(3) _cell_length_c 18.5253(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.9462(8) _cell_angle_gamma 90.00 _cell_volume 2794.43(11) _cell_measurement_reflns_used 20148 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.514 _cell_measurement_temperature 150 _exptl_crystal_F_000 1120 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7266 _exptl_absorpt_correction_T_max 0.8907 _diffrn_reflns_number 20148 _diffrn_measured_fraction_theta_max 0.9905 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9905 _reflns_number_total 6289 _reflns_number_gt 5225 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 23 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.122 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6272 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0536P)^2^+3.6483P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.59 _refine_diff_density_min -0.60 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti -0.29153(4) -0.26768(4) 0.21738(3) 0.02055(13) Uani 1 1 d . . . Cl(1) Cl -0.25380(6) -0.44823(6) 0.19162(4) 0.03194(18) Uani 1 1 d . . . Cl(2) Cl -0.20203(5) -0.25854(6) 0.33874(4) 0.03033(17) Uani 1 1 d . . . O(1) O -0.21972(13) -0.17588(15) 0.17198(10) 0.0196(4) Uani 1 1 d . . . C(1) C -0.4425(2) -0.2552(3) 0.26404(18) 0.0380(8) Uani 1 1 d . . . C(2) C -0.4283(2) -0.1508(3) 0.23117(19) 0.0375(7) Uani 1 1 d . . . C(3) C -0.4409(2) -0.1677(3) 0.15452(17) 0.0323(7) Uani 1 1 d . . . C(4) C -0.4605(2) -0.2829(3) 0.13927(16) 0.0301(6) Uani 1 1 d . . . C(5) C -0.4625(2) -0.3373(3) 0.20718(17) 0.0347(7) Uani 1 1 d . . . C(11) C -0.20355(18) -0.0949(2) 0.12229(14) 0.0179(5) Uani 1 1 d . . . C(12) C -0.24025(19) -0.1184(2) 0.04553(14) 0.0191(5) Uani 1 1 d . . . C(13) C -0.2262(2) -0.0377(2) -0.00591(15) 0.0218(5) Uani 1 1 d . . . C(14) C -0.17582(19) 0.0647(2) 0.01636(15) 0.0210(5) Uani 1 1 d . . . C(15) C -0.13869(19) 0.0836(2) 0.09306(15) 0.0206(5) Uani 1 1 d . . . C(16) C -0.15032(19) 0.0071(2) 0.14787(14) 0.0197(5) Uani 1 1 d . . . C(21) C -0.29499(19) -0.2256(2) 0.01648(14) 0.0190(5) Uani 1 1 d . . . C(22) C -0.2546(2) -0.3305(2) 0.01900(15) 0.0230(5) Uani 1 1 d . . . C(23) C -0.3376(2) -0.4158(2) -0.01795(17) 0.0279(6) Uani 1 1 d . . . C(24) C -0.4323(2) -0.3413(2) -0.04642(15) 0.0238(6) Uani 1 1 d . . . C(25) C -0.5327(2) -0.3680(3) -0.08644(16) 0.0302(6) Uani 1 1 d . . . C(26) C -0.6067(2) -0.2817(3) -0.10463(17) 0.0339(7) Uani 1 1 d . . . C(27) C -0.5801(2) -0.1698(3) -0.08420(17) 0.0326(7) Uani 1 1 d . . . C(28) C -0.4786(2) -0.1419(2) -0.04492(15) 0.0251(6) Uani 1 1 d . . . C(29) C -0.40525(19) -0.2282(2) -0.02562(14) 0.0191(5) Uani 1 1 d . . . C(141) C -0.1617(2) 0.1510(2) -0.04245(16) 0.0268(6) Uani 1 1 d . . . C(142) C -0.1070(3) 0.2592(3) -0.00648(19) 0.0369(7) Uani 1 1 d . . . C(143) C -0.0959(3) 0.0974(3) -0.0909(2) 0.0439(8) Uani 1 1 d . . . C(144) C -0.2696(2) 0.1838(3) -0.0915(2) 0.0416(8) Uani 1 1 d . . . C(161) C -0.1068(2) 0.0357(2) 0.23114(15) 0.0234(5) Uani 1 1 d . . . C(162) C -0.1969(2) 0.0478(3) 0.26867(16) 0.0304(6) Uani 1 1 d . . . C(163) C -0.0302(2) -0.0565(2) 0.26979(16) 0.0295(6) Uani 1 1 d . . . C(164) C -0.0472(2) 0.1491(2) 0.24213(17) 0.0335(7) Uani 1 1 d . . . C(221) C -0.1430(2) -0.3643(3) 0.04951(18) 0.0323(7) Uani 1 1 d . . . C(231) C -0.3095(3) -0.4895(3) -0.07637(18) 0.0378(7) Uani 1 1 d . . . H(1) H -0.4392 -0.2679 0.3152 0.046 Uiso 1 1 calc R . . H(2) H -0.4128 -0.0804 0.2567 0.045 Uiso 1 1 calc R . . H(3) H -0.4368 -0.1107 0.1191 0.039 Uiso 1 1 calc R . . H(4) H -0.4707 -0.3184 0.0919 0.036 Uiso 1 1 calc R . . H(5) H -0.4752 -0.4157 0.2131 0.042 Uiso 1 1 calc R . . H(13) H -0.2518 -0.0531 -0.0578 0.026 Uiso 1 1 calc R . . H(15) H -0.1033 0.1530 0.1089 0.025 Uiso 1 1 calc R . . H(23) H -0.3513 -0.4665 0.0218 0.034 Uiso 1 1 calc R . . H(25) H -0.5509 -0.4441 -0.1013 0.036 Uiso 1 1 calc R . . H(26) H -0.6762 -0.2994 -0.1313 0.041 Uiso 1 1 calc R . . H(27) H -0.6314 -0.1119 -0.0971 0.039 Uiso 1 1 calc R . . H(28) H -0.4601 -0.0653 -0.0316 0.030 Uiso 1 1 calc R . . H(14A) H -0.1480 0.2943 0.0247 0.055 Uiso 1 1 calc R . . H(14B) H -0.1006 0.3126 -0.0456 0.055 Uiso 1 1 calc R . . H(14C) H -0.0374 0.2401 0.0246 0.055 Uiso 1 1 calc R . . H(14D) H -0.0264 0.0788 -0.0595 0.066 Uiso 1 1 calc R . . H(14E) H -0.0893 0.1513 -0.1297 0.066 Uiso 1 1 calc R . . H(14F) H -0.1300 0.0279 -0.1144 0.066 Uiso 1 1 calc R . . H(14G) H -0.3043 0.1162 -0.1173 0.062 Uiso 1 1 calc R . . H(14H) H -0.2617 0.2405 -0.1284 0.062 Uiso 1 1 calc R . . H(14I) H -0.3118 0.2157 -0.0601 0.062 Uiso 1 1 calc R . . H(16A) H -0.2352 -0.0241 0.2646 0.046 Uiso 1 1 calc R . . H(16B) H -0.2442 0.1081 0.2438 0.046 Uiso 1 1 calc R . . H(16C) H -0.1688 0.0671 0.3215 0.046 Uiso 1 1 calc R . . H(16D) H -0.0650 -0.1306 0.2625 0.044 Uiso 1 1 calc R . . H(16E) H -0.0065 -0.0400 0.3234 0.044 Uiso 1 1 calc R . . H(16F) H 0.0300 -0.0579 0.2483 0.044 Uiso 1 1 calc R . . H(16G) H -0.0175 0.1626 0.2956 0.050 Uiso 1 1 calc R . . H(16H) H -0.0952 0.2110 0.2211 0.050 Uiso 1 1 calc R . . H(16I) H 0.0091 0.1460 0.2167 0.050 Uiso 1 1 calc R . . H(22A) H -0.1130 -0.3853 0.0082 0.048 Uiso 1 1 calc R . . H(22B) H -0.1390 -0.4293 0.0832 0.048 Uiso 1 1 calc R . . H(22C) H -0.1038 -0.3003 0.0771 0.048 Uiso 1 1 calc R . . H(23A) H -0.3682 -0.5398 -0.0987 0.057 Uiso 1 1 calc R . . H(23B) H -0.2480 -0.5354 -0.0531 0.057 Uiso 1 1 calc R . . H(23C) H -0.2940 -0.4414 -0.1153 0.057 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0211(2) 0.0239(3) 0.0167(2) -0.00376(18) 0.00500(17) 0.00088(18) Cl(1) 0.0373(4) 0.0231(3) 0.0335(4) -0.0028(3) 0.0056(3) -0.0008(3) Cl(2) 0.0333(4) 0.0383(4) 0.0176(3) -0.0027(3) 0.0034(3) 0.0019(3) O(1) 0.0204(9) 0.0210(9) 0.0164(9) -0.0031(7) 0.0030(7) -0.0003(7) C(1) 0.0244(14) 0.067(2) 0.0253(16) -0.0036(15) 0.0118(12) -0.0038(15) C(2) 0.0264(15) 0.0451(19) 0.0409(19) 0.0030(13) 0.0085(13) -0.0124(15) C(3) 0.0203(13) 0.0411(18) 0.0351(17) 0.0041(12) 0.0064(12) 0.0060(13) C(4) 0.0192(13) 0.0473(18) 0.0229(15) -0.0065(12) 0.0036(11) -0.0030(13) C(5) 0.0236(14) 0.0508(19) 0.0314(17) -0.0133(13) 0.0100(12) 0.0000(14) C(11) 0.0170(11) 0.0189(12) 0.0187(13) -0.0003(9) 0.0065(9) 0.0014(10) C(12) 0.0176(11) 0.0202(12) 0.0206(13) -0.0003(10) 0.0067(9) -0.0010(10) C(13) 0.0228(13) 0.0232(13) 0.0184(13) 0.0017(10) 0.0037(10) 0.0026(10) C(14) 0.0174(12) 0.0222(13) 0.0241(14) 0.0027(10) 0.0066(10) 0.0049(10) C(15) 0.0179(12) 0.0166(12) 0.0280(14) -0.0007(9) 0.0071(10) -0.0010(10) C(16) 0.0169(12) 0.0201(12) 0.0215(13) 0.0003(10) 0.0037(10) -0.0013(10) C(21) 0.0213(12) 0.0232(13) 0.0130(12) -0.0024(10) 0.0055(9) -0.0027(10) C(22) 0.0226(13) 0.0244(14) 0.0210(14) -0.0013(10) 0.0040(10) -0.0024(10) C(23) 0.0287(14) 0.0218(14) 0.0317(16) -0.0030(11) 0.0050(12) -0.0034(11) C(24) 0.0248(13) 0.0276(14) 0.0194(13) -0.0027(11) 0.0067(10) -0.0034(11) C(25) 0.0282(14) 0.0323(16) 0.0299(16) -0.0072(12) 0.0073(12) -0.0084(12) C(26) 0.0195(13) 0.0486(19) 0.0317(17) -0.0060(13) 0.0031(11) -0.0060(14) C(27) 0.0241(14) 0.0400(17) 0.0335(16) 0.0060(13) 0.0070(12) -0.0025(13) C(28) 0.0263(13) 0.0277(14) 0.0221(14) 0.0019(11) 0.0075(11) -0.0035(11) C(29) 0.0208(12) 0.0235(13) 0.0137(12) -0.0018(10) 0.0056(9) -0.0014(10) C(141) 0.0242(13) 0.0264(14) 0.0312(16) 0.0019(11) 0.0097(11) 0.0080(11) C(142) 0.0391(17) 0.0284(16) 0.0433(19) -0.0058(13) 0.0110(14) 0.0120(13) C(143) 0.060(2) 0.0377(18) 0.047(2) 0.0056(16) 0.0372(18) 0.0126(15) C(144) 0.0353(17) 0.0395(18) 0.046(2) 0.0002(14) 0.0024(14) 0.0201(15) C(161) 0.0259(13) 0.0219(13) 0.0204(13) -0.0048(11) 0.0025(10) -0.0040(10) C(162) 0.0388(16) 0.0318(15) 0.0220(14) -0.0035(13) 0.0105(12) -0.0074(12) C(163) 0.0257(14) 0.0295(15) 0.0275(15) -0.0045(12) -0.0035(11) -0.0012(12) C(164) 0.0407(16) 0.0253(15) 0.0286(16) -0.0101(13) -0.0018(13) -0.0039(12) C(221) 0.0248(14) 0.0312(15) 0.0382(17) 0.0042(12) 0.0033(12) -0.0011(13) C(231) 0.0411(18) 0.0323(17) 0.0378(18) 0.0022(14) 0.0065(14) -0.0051(13) # 10. 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_publ_flag Ti O(1) 1.7876(18) YES Ti Cl(2) 2.2581(8) YES Ti Cl(1) 2.2621(8) YES Ti C(3) 2.341(3) YES Ti C(4) 2.341(3) YES Ti C(2) 2.343(3) YES Ti C(5) 2.373(3) YES Ti C(1) 2.382(3) YES O(1) C(11) 1.380(3) YES C(1) C(5) 1.403(5) YES C(1) C(2) 1.406(5) YES C(2) C(3) 1.401(4) YES C(3) C(4) 1.395(4) YES C(4) C(5) 1.418(4) YES C(11) C(12) 1.407(4) YES C(11) C(16) 1.411(3) YES C(12) C(13) 1.392(4) YES C(12) C(21) 1.486(3) YES C(13) C(14) 1.388(4) YES C(14) C(15) 1.396(4) YES C(14) C(141) 1.535(4) YES C(15) C(16) 1.395(4) YES C(16) C(161) 1.538(4) YES C(21) C(22) 1.342(4) YES C(21) C(29) 1.470(3) YES C(22) C(221) 1.496(4) YES C(22) C(23) 1.517(4) YES C(23) C(231) 1.507(4) YES C(23) C(24) 1.511(4) YES C(24) C(25) 1.383(4) YES C(24) C(29) 1.407(4) YES C(25) C(26) 1.393(4) YES C(26) C(27) 1.390(4) YES C(27) C(28) 1.394(4) YES C(28) C(29) 1.388(4) YES C(141) C(142) 1.531(4) YES C(141) C(144) 1.533(4) YES C(141) C(143) 1.540(4) YES C(161) C(163) 1.532(4) YES C(161) C(162) 1.537(4) YES C(161) C(164) 1.538(4) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ti Cl(2) 103.44(6) YES O(1) Ti Cl(1) 107.15(6) YES Cl(2) Ti Cl(1) 99.59(3) YES O(1) Ti C(3) 87.00(9) YES Cl(2) Ti C(3) 129.18(8) YES Cl(1) Ti C(3) 124.92(8) YES O(1) Ti C(4) 107.27(9) YES Cl(2) Ti C(4) 142.47(8) YES Cl(1) Ti C(4) 91.53(8) YES C(3) Ti C(4) 34.68(11) YES O(1) Ti C(2) 102.60(11) YES Cl(2) Ti C(2) 94.97(8) YES Cl(1) Ti C(2) 142.59(9) YES C(3) Ti C(2) 34.80(11) YES C(4) Ti C(2) 57.79(11) YES O(1) Ti C(5) 141.78(10) YES Cl(2) Ti C(5) 110.00(8) YES Cl(1) Ti C(5) 85.29(9) YES C(3) Ti C(5) 57.62(11) YES C(4) Ti C(5) 35.01(10) YES C(2) Ti C(5) 57.32(12) YES O(1) Ti C(1) 137.18(11) YES Cl(2) Ti C(1) 84.91(8) YES Cl(1) Ti C(1) 112.76(9) YES C(3) Ti C(1) 57.74(11) YES C(4) Ti C(1) 57.86(11) YES C(2) Ti C(1) 34.60(12) YES C(5) Ti C(1) 34.32(11) YES C(11) O(1) Ti 157.65(16) YES C(5) C(1) C(2) 107.3(3) YES C(5) C(1) Ti 72.49(16) YES C(2) C(1) Ti 71.19(17) YES C(3) C(2) C(1) 108.7(3) YES C(3) C(2) Ti 72.50(17) YES C(1) C(2) Ti 74.21(18) YES C(4) C(3) C(2) 108.1(3) YES C(4) C(3) Ti 72.66(17) YES C(2) C(3) Ti 72.71(17) YES C(3) C(4) C(5) 107.7(3) YES C(3) C(4) Ti 72.65(16) YES C(5) C(4) Ti 73.74(16) YES C(1) C(5) C(4) 108.2(3) YES C(1) C(5) Ti 73.19(17) YES C(4) C(5) Ti 71.25(16) YES O(1) C(11) C(12) 117.7(2) YES O(1) C(11) C(16) 120.9(2) YES C(12) C(11) C(16) 121.3(2) YES C(13) C(12) C(11) 119.0(2) YES C(13) C(12) C(21) 118.1(2) YES C(11) C(12) C(21) 122.9(2) YES C(14) C(13) C(12) 121.9(2) YES C(13) C(14) C(15) 117.2(2) YES C(13) C(14) C(141) 120.0(2) YES C(15) C(14) C(141) 122.8(2) YES C(16) C(15) C(14) 124.2(2) YES C(15) C(16) C(11) 116.4(2) YES C(15) C(16) C(161) 120.3(2) YES C(11) C(16) C(161) 123.3(2) YES C(22) C(21) C(29) 109.5(2) YES C(22) C(21) C(12) 128.0(2) YES C(29) C(21) C(12) 122.4(2) YES C(21) C(22) C(221) 127.2(2) YES C(21) C(22) C(23) 110.9(2) YES C(221) C(22) C(23) 121.8(2) YES C(231) C(23) C(24) 114.9(2) YES C(231) C(23) C(22) 114.8(2) YES C(24) C(23) C(22) 102.4(2) YES C(25) C(24) C(29) 120.3(3) YES C(25) C(24) C(23) 130.9(3) YES C(29) C(24) C(23) 108.9(2) YES C(24) C(25) C(26) 119.0(3) YES C(27) C(26) C(25) 120.7(3) YES C(26) C(27) C(28) 120.6(3) YES C(29) C(28) C(27) 118.7(3) YES C(28) C(29) C(24) 120.6(2) YES C(28) C(29) C(21) 131.1(2) YES C(24) C(29) C(21) 108.3(2) YES C(142) C(141) C(144) 108.3(2) YES C(142) C(141) C(14) 111.8(2) YES C(144) C(141) C(14) 108.7(2) YES C(142) C(141) C(143) 108.5(2) YES C(144) C(141) C(143) 109.9(3) YES C(14) C(141) C(143) 109.5(2) YES C(163) C(161) C(162) 110.7(2) YES C(163) C(161) C(164) 107.2(2) YES C(162) C(161) C(164) 107.0(2) YES C(163) C(161) C(16) 110.2(2) YES C(162) C(161) C(16) 109.8(2) YES C(164) C(161) C(16) 111.7(2) YES data_LTIND _database_code_CSD 218475 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C32 H36 O2' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 452.64 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2956(2) _cell_length_b 10.0981(3) _cell_length_c 15.7158(6) _cell_angle_alpha 102.3307(11) _cell_angle_beta 93.1236(11) _cell_angle_gamma 91.625(2) _cell_volume 1283.15(13) _cell_measurement_reflns_used 13787 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.066 _cell_measurement_temperature 150 _exptl_crystal_F_000 488 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.9636 _exptl_absorpt_correction_T_max 0.9885 _diffrn_reflns_number 13787 _reflns_number_total 5758 _reflns_number_gt 4237 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 20 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.37' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.089 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.000 _refine_ls_wR_factor_gt 0.113 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 5758 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.18 _refine_diff_density_min -0.21 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(11) O 0.22035(12) 0.28576(12) 1.07309(7) 0.0366(3) Uani 1 1 d . . . O(31) O 0.53196(14) 0.76550(12) 0.82035(7) 0.0365(3) Uani 1 1 d . . . C(11) C 0.22061(16) 0.37467(16) 1.02946(10) 0.0272(3) Uani 1 1 d . . . C(12) C 0.13536(16) 0.36646(15) 0.94386(10) 0.0253(3) Uani 1 1 d . . . C(13) C 0.17289(17) 0.49663(15) 0.91389(10) 0.0266(3) Uani 1 1 d . . . C(14) C 0.28115(16) 0.57809(15) 0.98818(10) 0.0267(3) Uani 1 1 d . . . C(15) C 0.35315(18) 0.70686(16) 0.99634(11) 0.0333(4) Uani 1 1 d . . . C(16) C 0.44842(19) 0.76132(17) 1.07188(12) 0.0377(4) Uani 1 1 d . . . C(17) C 0.47253(18) 0.69104(17) 1.13796(11) 0.0362(4) Uani 1 1 d . . . C(18) C 0.40233(17) 0.56304(16) 1.13031(11) 0.0322(4) Uani 1 1 d . . . C(19) C 0.30674(16) 0.50786(15) 1.05409(10) 0.0271(3) Uani 1 1 d . . . C(21) C 0.04242(16) 0.25662(15) 0.90156(10) 0.0252(3) Uani 1 1 d . . . C(22) C 0.01437(18) 0.12931(15) 0.93674(11) 0.0304(4) Uani 1 1 d . . . C(23) C -0.09952(19) 0.03413(16) 0.86878(11) 0.0328(4) Uani 1 1 d . . . C(24) C -0.12425(16) 0.10706(15) 0.79574(10) 0.0272(3) Uani 1 1 d . . . C(25) C -0.21273(18) 0.06255(16) 0.71661(11) 0.0336(4) Uani 1 1 d . . . C(26) C -0.22552(18) 0.14791(17) 0.65870(11) 0.0359(4) Uani 1 1 d . . . C(27) C -0.15123(18) 0.27682(17) 0.67900(11) 0.0343(4) Uani 1 1 d . . . C(28) C -0.06058(17) 0.32133(16) 0.75683(10) 0.0298(4) Uani 1 1 d . . . C(29) C -0.04557(16) 0.23595(14) 0.81605(10) 0.0245(3) Uani 1 1 d . . . C(31) C 0.56964(17) 0.74089(15) 0.73457(10) 0.0269(3) Uani 1 1 d . . . C(32) C 0.45827(16) 0.77252(14) 0.67193(10) 0.0247(3) Uani 1 1 d . . . C(33) C 0.50669(16) 0.75169(14) 0.58656(10) 0.0245(3) Uani 1 1 d . . . C(34) C 0.65535(16) 0.69905(14) 0.56025(10) 0.0239(3) Uani 1 1 d . . . C(35) C 0.75833(17) 0.66639(15) 0.62461(10) 0.0273(3) Uani 1 1 d . . . C(36) C 0.71614(17) 0.68702(15) 0.71026(10) 0.0293(4) Uani 1 1 d . . . C(321) C 0.29316(17) 0.82996(14) 0.69638(10) 0.0280(4) Uani 1 1 d . . . C(322) C 0.3201(2) 0.97064(16) 0.75720(12) 0.0424(5) Uani 1 1 d . . . C(323) C 0.19811(18) 0.73450(16) 0.74190(11) 0.0352(4) Uani 1 1 d . . . C(324) C 0.18860(18) 0.84625(17) 0.61625(12) 0.0354(4) Uani 1 1 d . . . C(341) C 0.70059(17) 0.68502(14) 0.46565(10) 0.0263(3) Uani 1 1 d . . . C(342) C 0.7444(2) 0.82592(16) 0.45029(12) 0.0459(5) Uani 1 1 d . . . C(343) C 0.84523(19) 0.59571(17) 0.44603(11) 0.0378(4) Uani 1 1 d . . . C(344) C 0.56047(19) 0.62056(17) 0.40097(11) 0.0377(4) Uani 1 1 d . . . H(15) H 0.3379 0.7550 0.9525 0.043 Uiso 1 1 calc R . . H(16) H 0.4973 0.8472 1.0783 0.049 Uiso 1 1 calc R . . H(17) H 0.5365 0.7304 1.1879 0.047 Uiso 1 1 calc R . . H(18) H 0.4180 0.5151 1.1743 0.042 Uiso 1 1 calc R . . H(25) H -0.2627 -0.0236 0.7028 0.044 Uiso 1 1 calc R . . H(26) H -0.2845 0.1187 0.6056 0.047 Uiso 1 1 calc R . . H(27) H -0.1626 0.3337 0.6398 0.045 Uiso 1 1 calc R . . H(28) H -0.0100 0.4072 0.7698 0.039 Uiso 1 1 calc R . . H(31) H 0.382(2) 0.260(2) 1.1479(14) 0.066(7) Uiso 1 1 d . . . H(33) H 0.4359 0.7741 0.5444 0.032 Uiso 1 1 calc R . . H(35) H 0.8574 0.6300 0.6099 0.036 Uiso 1 1 calc R . . H(36) H 0.7873 0.6643 0.7522 0.038 Uiso 1 1 calc R . . H(13A) H 0.2281 0.4784 0.8600 0.035 Uiso 1 1 calc R . . H(13B) H 0.0750 0.5437 0.9052 0.035 Uiso 1 1 calc R . . H(22A) H -0.0344 0.1514 0.9925 0.040 Uiso 1 1 calc R . . H(22B) H 0.1158 0.0867 0.9447 0.040 Uiso 1 1 calc R . . H(23A) H -0.0510 -0.0523 0.8485 0.043 Uiso 1 1 calc R . . H(23B) H -0.2014 0.0183 0.8932 0.043 Uiso 1 1 calc R . . H(32A) H 0.3757 0.9618 0.8108 0.055 Uiso 1 1 calc R . . H(32B) H 0.2176 1.0099 0.7694 0.055 Uiso 1 1 calc R . . H(32C) H 0.3837 1.0281 0.7294 0.055 Uiso 1 1 calc R . . H(32D) H 0.1813 0.6471 0.7033 0.046 Uiso 1 1 calc R . . H(32E) H 0.0955 0.7717 0.7566 0.046 Uiso 1 1 calc R . . H(32F) H 0.2583 0.7253 0.7941 0.046 Uiso 1 1 calc R . . H(32G) H 0.2417 0.9093 0.5881 0.046 Uiso 1 1 calc R . . H(32H) H 0.0858 0.8797 0.6341 0.046 Uiso 1 1 calc R . . H(32I) H 0.1726 0.7600 0.5763 0.046 Uiso 1 1 calc R . . H(34A) H 0.6527 0.8820 0.4596 0.060 Uiso 1 1 calc R . . H(34B) H 0.7751 0.8179 0.3914 0.060 Uiso 1 1 calc R . . H(34C) H 0.8329 0.8663 0.4901 0.060 Uiso 1 1 calc R . . H(34D) H 0.9382 0.6376 0.4817 0.049 Uiso 1 1 calc R . . H(34E) H 0.8668 0.5849 0.3856 0.049 Uiso 1 1 calc R . . H(34F) H 0.8216 0.5084 0.4585 0.049 Uiso 1 1 calc R . . H(34G) H 0.5307 0.5330 0.4113 0.049 Uiso 1 1 calc R . . H(34H) H 0.5935 0.6106 0.3424 0.049 Uiso 1 1 calc R . . H(34I) H 0.4695 0.6777 0.4087 0.049 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(11) 0.0356(6) 0.0463(7) 0.0294(7) -0.0046(5) -0.0060(5) 0.0143(6) O(31) 0.0325(6) 0.0535(8) 0.0232(7) 0.0034(5) -0.0008(5) 0.0079(5) C(11) 0.0197(7) 0.0370(9) 0.0249(9) 0.0020(6) 0.0023(6) 0.0061(7) C(12) 0.0195(7) 0.0321(8) 0.0245(8) 0.0005(6) 0.0015(6) 0.0063(6) C(13) 0.0230(7) 0.0314(8) 0.0244(9) -0.0006(6) 0.0009(6) 0.0043(6) C(14) 0.0202(7) 0.0312(8) 0.0262(9) 0.0026(6) 0.0042(6) -0.0003(7) C(15) 0.0322(8) 0.0328(9) 0.0328(10) 0.0008(7) 0.0049(7) 0.0016(7) C(16) 0.0326(9) 0.0328(9) 0.0413(11) -0.0038(7) 0.0034(7) -0.0057(8) C(17) 0.0277(8) 0.0411(9) 0.0318(10) 0.0000(7) -0.0027(7) -0.0088(8) C(18) 0.0260(8) 0.0397(9) 0.0275(9) 0.0039(7) -0.0001(6) -0.0003(7) C(19) 0.0212(7) 0.0336(8) 0.0239(9) 0.0029(6) 0.0026(6) -0.0003(7) C(21) 0.0207(7) 0.0312(8) 0.0241(8) 0.0034(6) 0.0032(6) 0.0063(6) C(22) 0.0310(8) 0.0318(8) 0.0301(9) 0.0017(6) 0.0009(6) 0.0107(7) C(23) 0.0341(8) 0.0287(8) 0.0355(10) -0.0011(7) -0.0001(7) 0.0078(7) C(24) 0.0217(7) 0.0281(8) 0.0301(9) 0.0035(6) 0.0012(6) 0.0026(7) C(25) 0.0320(8) 0.0305(9) 0.0348(10) -0.0017(7) -0.0030(7) 0.0013(7) C(26) 0.0322(9) 0.0430(10) 0.0284(10) -0.0011(7) -0.0077(7) 0.0012(8) C(27) 0.0310(8) 0.0454(10) 0.0285(9) 0.0000(7) -0.0036(7) 0.0138(8) C(28) 0.0254(8) 0.0342(8) 0.0298(9) -0.0027(6) 0.0002(6) 0.0078(7) C(29) 0.0189(7) 0.0299(8) 0.0236(8) 0.0017(6) 0.0008(6) 0.0036(6) C(31) 0.0267(8) 0.0305(8) 0.0227(8) -0.0021(6) -0.0011(6) 0.0050(6) C(32) 0.0245(7) 0.0199(7) 0.0289(9) -0.0015(6) -0.0017(6) 0.0041(6) C(33) 0.0247(7) 0.0226(7) 0.0262(9) -0.0016(6) -0.0060(6) 0.0075(6) C(34) 0.0242(7) 0.0222(7) 0.0248(8) -0.0027(6) -0.0025(6) 0.0053(6) C(35) 0.0222(7) 0.0294(8) 0.0311(9) 0.0015(6) -0.0002(6) 0.0084(7) C(36) 0.0247(7) 0.0350(9) 0.0291(9) 0.0004(6) -0.0058(6) 0.0112(7) C(321) 0.0242(7) 0.0260(8) 0.0321(9) 0.0009(6) -0.0004(6) 0.0030(7) C(322) 0.0351(9) 0.0316(9) 0.0536(13) 0.0014(7) 0.0001(8) -0.0059(8) C(323) 0.0276(8) 0.0391(9) 0.0367(10) -0.0037(7) 0.0015(7) 0.0038(8) C(324) 0.0258(8) 0.0346(9) 0.0458(11) 0.0049(7) -0.0008(7) 0.0091(8) C(341) 0.0292(8) 0.0257(8) 0.0239(9) -0.0013(6) -0.0005(6) 0.0063(6) C(342) 0.0686(13) 0.0320(9) 0.0384(11) -0.0065(8) 0.0118(9) 0.0093(8) C(343) 0.0365(9) 0.0449(10) 0.0297(10) 0.0030(7) 0.0026(7) 0.0025(8) C(344) 0.0376(9) 0.0453(10) 0.0285(10) 0.0001(7) -0.0050(7) 0.0064(8) # 10. 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 O(11) C(11) 1.2406(18) . ? O(31) H(31) 0.92(2) 2_667 ? O(31) C(31) 1.3726(18) . ? H(31) O(31) 0.92(2) 2_667 ? C(11) C(12) 1.470(2) . ? C(11) C(19) 1.470(2) . ? C(12) C(21) 1.359(2) . ? C(12) C(13) 1.518(2) . ? C(13) C(14) 1.510(2) . ? C(14) C(19) 1.385(2) . ? C(14) C(15) 1.393(2) . ? C(15) C(16) 1.389(2) . ? C(16) C(17) 1.386(2) . ? C(17) C(18) 1.381(2) . ? C(18) C(19) 1.400(2) . ? C(21) C(29) 1.465(2) . ? C(21) C(22) 1.521(2) . ? C(22) C(23) 1.535(2) . ? C(23) C(24) 1.499(2) . ? C(24) C(25) 1.389(2) . ? C(24) C(29) 1.405(2) . ? C(25) C(26) 1.383(2) . ? C(26) C(27) 1.390(2) . ? C(27) C(28) 1.382(2) . ? C(28) C(29) 1.401(2) . ? C(31) C(36) 1.385(2) . ? C(31) C(32) 1.406(2) . ? C(32) C(33) 1.396(2) . ? C(32) C(321) 1.539(2) . ? C(33) C(34) 1.4048(19) . ? C(34) C(35) 1.388(2) . ? C(34) C(341) 1.531(2) . ? C(35) C(36) 1.383(2) . ? C(321) C(324) 1.531(2) . ? C(321) C(322) 1.536(2) . ? C(321) C(323) 1.541(2) . ? C(341) C(343) 1.527(2) . ? C(341) C(342) 1.530(2) . ? C(341) C(344) 1.534(2) . ? 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 H(31) O(31) C(31) 107.7(13) 2_667 . ? O(11) C(11) C(12) 126.46(14) . . ? O(11) C(11) C(19) 126.10(14) . . ? C(12) C(11) C(19) 107.45(13) . . ? C(21) C(12) C(11) 123.22(14) . . ? C(21) C(12) C(13) 128.34(14) . . ? C(11) C(12) C(13) 108.43(12) . . ? C(14) C(13) C(12) 103.33(12) . . ? C(19) C(14) C(15) 119.89(14) . . ? C(19) C(14) C(13) 111.31(13) . . ? C(15) C(14) C(13) 128.79(15) . . ? C(16) C(15) C(14) 118.12(16) . . ? C(17) C(16) C(15) 121.75(15) . . ? C(18) C(17) C(16) 120.58(15) . . ? C(17) C(18) C(19) 117.72(16) . . ? C(14) C(19) C(18) 121.93(14) . . ? C(14) C(19) C(11) 109.46(13) . . ? C(18) C(19) C(11) 128.60(15) . . ? C(12) C(21) C(29) 128.12(14) . . ? C(12) C(21) C(22) 124.33(14) . . ? C(29) C(21) C(22) 107.55(12) . . ? C(21) C(22) C(23) 106.41(13) . . ? C(24) C(23) C(22) 104.79(12) . . ? C(25) C(24) C(29) 120.56(15) . . ? C(25) C(24) C(23) 128.12(14) . . ? C(29) C(24) C(23) 111.32(13) . . ? C(26) C(25) C(24) 119.18(14) . . ? C(25) C(26) C(27) 120.72(15) . . ? C(28) C(27) C(26) 120.63(16) . . ? C(27) C(28) C(29) 119.42(14) . . ? C(28) C(29) C(24) 119.46(14) . . ? C(28) C(29) C(21) 130.72(13) . . ? C(24) C(29) C(21) 109.82(13) . . ? O(31) C(31) C(36) 120.41(14) . . ? O(31) C(31) C(32) 119.10(13) . . ? C(36) C(31) C(32) 120.49(14) . . ? C(33) C(32) C(31) 116.47(13) . . ? C(33) C(32) C(321) 121.67(13) . . ? C(31) C(32) C(321) 121.85(14) . . ? C(32) C(33) C(34) 124.26(14) . . ? C(35) C(34) C(33) 116.56(14) . . ? C(35) C(34) C(341) 122.93(13) . . ? C(33) C(34) C(341) 120.46(13) . . ? C(36) C(35) C(34) 121.12(14) . . ? C(35) C(36) C(31) 121.06(14) . . ? C(324) C(321) C(322) 107.85(13) . . ? C(324) C(321) C(32) 112.12(13) . . ? C(322) C(321) C(32) 108.98(11) . . ? C(324) C(321) C(323) 107.27(12) . . ? C(322) C(321) C(323) 110.04(13) . . ? C(32) C(321) C(323) 110.53(12) . . ? C(343) C(341) C(342) 108.54(13) . . ? C(343) C(341) C(34) 111.54(13) . . ? C(342) C(341) C(34) 108.89(12) . . ? C(343) C(341) C(344) 107.22(13) . . ? C(342) C(341) C(344) 109.14(14) . . ? C(34) C(341) C(344) 111.44(12) . . ?