# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. #============================================================================== _journal_coden_Cambridge 0182 loop_ _publ_author_name I.Rothwell P.E.Fanwick M.G.Thorn L.E.Turner _publ_contact_author_name 'Dr Ian Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Drive West Lafayette Indiana 47907-1393 UNITED STATES OF AMERICA ; _publ_contact_author_email ROTHWELL@PURDUE.EDU _publ_section_title ; Facile Resolution of Constrained Geometry Indenyl-Phenoxide Ligation. ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., 'Guagliardi, A., Moliterni, A.G.G, Burla, M.C., Polidori, G., Camalli, M., & Spagna R. (1999). J. Appl. Cryst., 32, 115-119 Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Hall S.R. & du Boulay, D. (1995) Editors U. of Western Aurtralia 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. (1996). 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 Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; data_LTPHAT _database_code_CSD 201167 _audit_creation_date 5-09-00 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.36 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C27 H38 N2 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 454.52 _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 12.4594(3) _cell_length_b 11.7575(3) _cell_length_c 18.0226(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.1734(13) _cell_angle_gamma 90.00 _cell_volume 2508.5(2) _cell_measurement_reflns_used 19483 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.355 _cell_measurement_temperature 150 _exptl_crystal_F_000 976 # 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 0.6962 _exptl_absorpt_correction_T_max 0.8792 _diffrn_reflns_number 19483 _reflns_number_total 5700 _reflns_number_gt 4769 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 22 # 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 0.099 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 5694 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.4621P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.31 _refine_diff_density_min -0.40 _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 0.69825(2) 0.19106(3) 0.123647(17) 0.01904(9) Uani ? O(1) 0.78127(9) 0.06746(10) 0.10174(6) 0.0209(3) Uani ? N(2) 0.58277(13) 0.12819(13) 0.15986(9) 0.0270(5) Uani ? N(3) 0.61507(12) 0.23705(13) 0.01983(8) 0.0246(4) Uani ? C(11) 0.88942(14) 0.03843(14) 0.14214(9) 0.0184(4) Uani ? C(12) 0.94865(14) 0.11204(14) 0.20265(9) 0.0195(5) Uani ? C(13) 1.05981(14) 0.08914(15) 0.24614(9) 0.0221(5) Uani ? C(14) 1.11430(14) -0.00789(14) 0.23154(9) 0.0202(4) Uani ? C(15) 1.05258(14) -0.07957(14) 0.17130(9) 0.0196(5) Uani ? C(16) 0.94154(14) -0.05972(14) 0.12445(9) 0.0182(4) Uani ? C(21) 0.54367(17) 0.1395(2) 0.22729(12) 0.0374(6) Uani ? C(22) 0.52453(18) 0.03321(19) 0.11136(13) 0.0396(7) Uani ? C(31) 0.50752(18) 0.2966(2) 0.00017(13) 0.0419(7) Uani ? C(32) 0.66103(17) 0.24150(18) -0.04486(10) 0.0332(6) Uani ? C(121) 0.88370(14) 0.21534(14) 0.20994(9) 0.0206(4) Uani ? C(122) 0.80982(15) 0.23108(15) 0.25449(10) 0.0244(5) Uani ? C(123) 0.74041(16) 0.32691(15) 0.22663(10) 0.0257(5) Uani ? C(124) 0.77514(15) 0.37737(14) 0.16592(10) 0.0243(5) Uani ? C(125) 0.73635(18) 0.47281(16) 0.11622(11) 0.0328(6) Uani ? C(126) 0.78730(19) 0.49719(17) 0.06135(12) 0.0374(7) Uani ? C(127) 0.87553(18) 0.42949(17) 0.05174(11) 0.0358(6) Uani ? C(128) 0.91351(16) 0.33546(16) 0.09691(10) 0.0270(5) Uani ? C(129) 0.86451(14) 0.30844(14) 0.15573(10) 0.0210(5) Uani ? C(141) 1.23579(15) -0.03921(15) 0.27957(10) 0.0242(5) Uani ? C(142) 1.30207(16) 0.06409(18) 0.32095(12) 0.0371(6) Uani ? C(143) 1.2314(2) -0.1284(2) 0.34007(14) 0.0551(8) Uani ? C(144) 1.30089(16) -0.08794(19) 0.22734(12) 0.0369(6) Uani ? C(161) 0.88065(14) -0.13811(14) 0.05620(9) 0.0198(4) Uani ? C(162) 0.77191(15) -0.18546(15) 0.06707(11) 0.0252(5) Uani ? C(163) 0.95486(16) -0.23933(16) 0.04961(11) 0.0283(5) Uani ? C(164) 0.84999(17) -0.07169(16) -0.02111(10) 0.0290(5) Uani ? H(13) 1.0983 0.1391 0.2854 0.0290 Uiso calc H(15) 1.0880 -0.1451 0.1618 0.0260 Uiso calc H(122) 0.8071 0.1853 0.2960 0.0320 Uiso calc H(123) 0.6824 0.3525 0.2447 0.0330 Uiso calc H(125) 0.6774 0.5176 0.1211 0.0430 Uiso calc H(126) 0.7633 0.5603 0.0293 0.0490 Uiso calc H(127) 0.9086 0.4493 0.0139 0.0470 Uiso calc H(128) 0.9703 0.2903 0.0891 0.0350 Uiso calc H(14A) 1.2680 0.0930 0.3581 0.0480 Uiso calc H(14B) 1.3012 0.1220 0.2832 0.0480 Uiso calc H(14C) 1.3787 0.0422 0.3475 0.0480 Uiso calc H(14D) 1.3069 -0.1476 0.3713 0.0720 Uiso calc H(14E) 1.1938 -0.1953 0.3140 0.0720 Uiso calc H(14F) 1.1908 -0.0984 0.3731 0.0720 Uiso calc H(14G) 1.3776 -0.1026 0.2582 0.0480 Uiso calc H(14H) 1.2998 -0.0342 0.1870 0.0480 Uiso calc H(14I) 1.2660 -0.1576 0.2040 0.0480 Uiso calc H(16A) 0.7320 -0.2294 0.0220 0.0330 Uiso calc H(16B) 0.7251 -0.1236 0.0733 0.0330 Uiso calc H(16C) 0.7905 -0.2330 0.1126 0.0330 Uiso calc H(16D) 0.9736 -0.2831 0.0969 0.0370 Uiso calc H(16E) 1.0229 -0.2119 0.0415 0.0370 Uiso calc H(16F) 0.9145 -0.2863 0.0063 0.0370 Uiso calc H(16G) 0.8083 -0.1201 -0.0631 0.0380 Uiso calc H(16H) 0.9179 -0.0465 -0.0305 0.0380 Uiso calc H(16I) 0.8047 -0.0069 -0.0180 0.0380 Uiso calc H(21A) 0.4640 0.1546 0.2102 0.0490 Uiso calc H(21B) 0.5827 0.2013 0.2593 0.0490 Uiso calc H(21C) 0.5584 0.0703 0.2570 0.0490 Uiso calc H(22A) 0.5365 -0.0350 0.1422 0.0510 Uiso calc H(22B) 0.5538 0.0232 0.0684 0.0510 Uiso calc H(22C) 0.4451 0.0492 0.0917 0.0510 Uiso calc H(31A) 0.5193 0.3761 -0.0068 0.0550 Uiso calc H(31B) 0.4751 0.2872 0.0416 0.0550 Uiso calc H(31C) 0.4571 0.2660 -0.0473 0.0550 Uiso calc H(32A) 0.6083 0.2079 -0.0902 0.0430 Uiso calc H(32B) 0.7310 0.2003 -0.0314 0.0430 Uiso calc H(32C) 0.6741 0.3193 -0.0557 0.0430 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 0.01722(16) 0.02037(16) 0.01880(16) 0.00030(12) 0.00458(12) -0.00046(12) O(1) 0.0170(6) 0.0220(6) 0.0200(6) 0.0006(5) 0.0006(5) -0.0026(5) N(2) 0.0216(8) 0.0319(9) 0.0280(8) -0.0009(6) 0.0086(6) 0.0004(7) N(3) 0.0204(8) 0.0262(8) 0.0244(7) -0.0015(6) 0.0028(6) 0.0017(6) C(11) 0.0166(8) 0.0198(8) 0.0171(8) -0.0007(6) 0.0030(6) 0.0010(6) C(12) 0.0197(9) 0.0192(8) 0.0179(8) 0.0003(7) 0.0034(6) -0.0009(6) C(13) 0.0217(9) 0.0240(9) 0.0175(8) -0.0016(7) 0.0016(7) -0.0027(7) C(14) 0.0180(8) 0.0238(8) 0.0164(8) 0.0002(7) 0.0018(6) 0.0011(7) C(15) 0.0207(9) 0.0186(8) 0.0193(8) 0.0022(7) 0.0058(6) 0.0007(6) C(16) 0.0197(8) 0.0193(8) 0.0153(7) -0.0017(6) 0.0049(6) -0.0004(6) C(21) 0.0301(11) 0.0509(13) 0.0361(11) -0.0021(9) 0.0175(9) 0.0020(10) C(22) 0.0339(12) 0.0444(12) 0.0426(12) -0.0141(10) 0.0149(9) -0.0069(10) C(31) 0.0269(11) 0.0510(14) 0.0406(12) 0.0090(10) -0.0001(9) 0.0104(10) C(32) 0.0355(11) 0.0392(11) 0.0219(9) -0.0080(9) 0.0047(8) 0.0039(8) C(121) 0.0198(8) 0.0203(8) 0.0182(8) -0.0016(7) 0.0009(6) -0.0042(7) C(122) 0.0295(10) 0.0254(9) 0.0176(8) 0.0010(7) 0.0063(7) -0.0007(7) C(123) 0.0261(9) 0.0263(9) 0.0236(9) 0.0047(7) 0.0062(7) -0.0060(7) C(124) 0.0258(9) 0.0182(8) 0.0241(9) -0.0004(7) 0.0008(7) -0.0036(7) C(125) 0.0375(11) 0.0199(9) 0.0313(10) 0.0022(8) -0.0033(8) -0.0043(8) C(126) 0.0511(14) 0.0204(9) 0.0315(11) -0.0081(9) -0.0004(9) 0.0036(8) C(127) 0.0415(12) 0.0351(11) 0.0274(10) -0.0189(9) 0.0060(8) 0.0011(8) C(128) 0.0243(10) 0.0311(10) 0.0240(9) -0.0093(8) 0.0053(7) -0.0032(7) C(129) 0.0196(9) 0.0200(8) 0.0202(8) -0.0031(7) 0.0014(7) -0.0047(7) C(141) 0.0198(9) 0.0266(9) 0.0209(8) 0.0011(7) -0.0014(7) 0.0007(7) C(142) 0.0216(10) 0.0397(12) 0.0428(12) 0.0034(8) -0.0004(8) -0.0143(9) C(143) 0.0319(12) 0.0740(18) 0.0484(14) -0.0001(12) -0.0032(10) 0.0355(13) C(144) 0.0220(10) 0.0440(12) 0.0378(11) 0.0074(9) -0.0007(8) -0.0096(9) C(161) 0.0188(8) 0.0197(8) 0.0196(8) -0.0027(7) 0.0042(6) -0.0019(7) C(162) 0.0247(9) 0.0224(9) 0.0301(9) -0.0054(7) 0.0109(7) -0.0051(7) C(163) 0.0259(10) 0.0309(10) 0.0266(9) -0.0001(8) 0.0059(7) -0.0126(8) C(164) 0.0348(11) 0.0310(10) 0.0175(8) -0.0080(8) 0.0028(7) -0.0020(7) # 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) 1.8953(12) ? Ti N(2) 1.9048(15) ? Ti N(3) 1.9126(15) ? Ti C(121) 2.3659(17) ? Ti C(123) 2.3799(17) ? Ti C(122) 2.3812(17) ? Ti C(129) 2.4048(17) ? Ti C(124) 2.4170(17) ? O(1) C(11) 1.3602(19) ? N(2) C(21) 1.450(2) ? N(2) C(22) 1.464(2) ? N(3) C(32) 1.451(2) ? N(3) C(31) 1.455(2) ? C(11) C(12) 1.407(2) ? C(11) C(16) 1.409(2) ? C(12) C(13) 1.388(2) ? C(12) C(121) 1.488(2) ? C(13) C(14) 1.394(2) ? C(14) C(15) 1.400(2) ? C(14) C(141) 1.536(2) ? C(15) C(16) 1.397(2) ? C(16) C(161) 1.535(2) ? C(121) C(122) 1.410(2) ? C(121) C(129) 1.437(2) ? C(122) C(123) 1.414(2) ? C(123) C(124) 1.426(3) ? C(124) C(125) 1.423(3) ? C(124) C(129) 1.435(2) ? C(125) C(126) 1.362(3) ? C(126) C(127) 1.411(3) ? C(127) C(128) 1.367(3) ? C(128) C(129) 1.415(2) ? C(141) C(142) 1.526(3) ? C(141) C(143) 1.526(3) ? C(141) C(144) 1.533(3) ? C(161) C(162) 1.533(2) ? C(161) C(163) 1.534(2) ? C(161) C(164) 1.538(2) ? 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 N(2) 107.07(6) ? O(1) Ti N(3) 100.22(6) ? N(2) Ti N(3) 102.02(6) ? O(1) Ti C(121) 75.22(5) ? N(2) Ti C(121) 120.58(6) ? N(3) Ti C(121) 136.81(6) ? O(1) Ti C(123) 132.45(6) ? N(2) Ti C(123) 89.99(7) ? N(3) Ti C(123) 119.58(6) ? C(121) Ti C(123) 58.24(6) ? O(1) Ti C(122) 99.78(6) ? N(2) Ti C(122) 90.42(6) ? N(3) Ti C(122) 152.10(7) ? C(121) Ti C(122) 34.55(6) ? C(123) Ti C(122) 34.55(6) ? O(1) Ti C(129) 90.28(5) ? N(2) Ti C(129) 145.73(6) ? N(3) Ti C(129) 103.66(6) ? C(121) Ti C(129) 35.04(6) ? C(123) Ti C(129) 57.54(6) ? C(122) Ti C(129) 57.00(6) ? O(1) Ti C(124) 124.90(6) ? N(2) Ti C(124) 120.74(6) ? N(3) Ti C(124) 95.31(6) ? C(121) Ti C(124) 58.24(6) ? C(123) Ti C(124) 34.57(6) ? C(122) Ti C(124) 57.12(6) ? C(129) Ti C(124) 34.62(6) ? C(11) O(1) Ti 126.50(10) ? C(21) N(2) C(22) 109.71(15) ? C(21) N(2) Ti 137.64(13) ? C(22) N(2) Ti 112.22(12) ? C(32) N(3) C(31) 110.56(15) ? C(32) N(3) Ti 124.54(12) ? C(31) N(3) Ti 123.46(13) ? O(1) C(11) C(12) 116.93(14) ? O(1) C(11) C(16) 122.29(14) ? C(12) C(11) C(16) 120.78(15) ? C(13) C(12) C(11) 120.52(15) ? C(13) C(12) C(121) 125.64(15) ? C(11) C(12) C(121) 113.72(14) ? C(12) C(13) C(14) 120.73(15) ? C(13) C(14) C(15) 117.19(15) ? C(13) C(14) C(141) 122.84(14) ? C(15) C(14) C(141) 119.95(15) ? C(16) C(15) C(14) 124.68(15) ? C(15) C(16) C(11) 116.07(14) ? C(15) C(16) C(161) 122.19(14) ? C(11) C(16) C(161) 121.71(14) ? C(122) C(121) C(129) 106.71(15) ? C(122) C(121) C(12) 128.84(15) ? C(129) C(121) C(12) 122.81(15) ? C(122) C(121) Ti 73.32(10) ? C(129) C(121) Ti 73.96(9) ? C(12) C(121) Ti 106.86(10) ? C(121) C(122) C(123) 109.76(15) ? C(121) C(122) Ti 72.13(9) ? C(123) C(122) Ti 72.68(10) ? C(122) C(123) C(124) 107.81(16) ? C(122) C(123) Ti 72.77(10) ? C(124) C(123) Ti 74.14(10) ? C(125) C(124) C(123) 133.36(18) ? C(125) C(124) C(129) 119.33(17) ? C(123) C(124) C(129) 107.26(15) ? C(125) C(124) Ti 119.53(12) ? C(123) C(124) Ti 71.29(10) ? C(129) C(124) Ti 72.23(9) ? C(126) C(125) C(124) 118.64(19) ? C(125) C(126) C(127) 121.86(18) ? C(128) C(127) C(126) 121.43(18) ? C(127) C(128) C(129) 118.54(18) ? C(128) C(129) C(124) 120.17(16) ? C(128) C(129) C(121) 131.42(16) ? C(124) C(129) C(121) 108.34(15) ? C(128) C(129) Ti 119.30(11) ? C(124) C(129) Ti 73.16(10) ? C(121) C(129) Ti 71.00(9) ? C(142) C(141) C(143) 109.40(17) ? C(142) C(141) C(144) 106.75(16) ? C(143) C(141) C(144) 109.00(18) ? C(142) C(141) C(14) 111.88(15) ? C(143) C(141) C(14) 108.61(15) ? C(144) C(141) C(14) 111.15(14) ? C(162) C(161) C(163) 107.83(14) ? C(162) C(161) C(16) 110.57(13) ? C(163) C(161) C(16) 111.63(14) ? C(162) C(161) C(164) 108.70(14) ? C(163) C(161) C(164) 108.01(14) ? C(16) C(161) C(164) 110.01(13) ? #============================================================================== data_LT2P69 _database_code_CSD 201168 _audit_creation_date 11-07-01 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour orange-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 'C29 H42 N2 O1 Ti1' _chemical_formula_structural ? _chemical_formula_weight 482.57 _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 10.0202(2) _cell_length_b 13.0802(3) _cell_length_c 22.0926(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.3111(13) _cell_angle_gamma 90.00 _cell_volume 2829.01(19) _cell_measurement_reflns_used 21787 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.318 _cell_measurement_temperature 209 _exptl_crystal_F_000 1040 # 6. DATA COLLECTION _diffrn_ambient_temperature 209 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.3552 _exptl_absorpt_correction_T_max 0.9610 _diffrn_reflns_number 21787 _diffrn_measured_fraction_theta_max 0.9200 _reflns_number_total 6044 _reflns_number_gt 4920 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 28 # 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 0.160 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6040 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0863P)^2^+1.6189P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.82 _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 Direct_methods_(SIR97,_Altomare_et_al.,_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_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 0.85895(5) 0.30091(3) 0.57975(2) 0.02760(13) Uani ? O(1) 0.8238(2) 0.15895(13) 0.57893(8) 0.0321(5) Uani ? N(7) 0.8048(3) 0.34194(18) 0.49415(11) 0.0388(7) Uani ? N(8) 1.0518(3) 0.29912(18) 0.58984(11) 0.0374(7) Uani ? C(1) 0.7419(3) 0.10790(18) 0.61070(11) 0.0275(7) Uani ? C(2) 0.6863(3) 0.16595(18) 0.65284(11) 0.0295(7) Uani ? C(3) 0.6005(3) 0.1207(2) 0.68686(12) 0.0331(7) Uani ? C(4) 0.5672(3) 0.0180(2) 0.67973(12) 0.0344(7) Uani ? C(5) 0.6238(3) -0.03764(19) 0.63693(11) 0.0329(7) Uani ? C(6) 0.7103(3) 0.00387(18) 0.60164(11) 0.0295(7) Uani ? C(21) 0.7240(3) 0.27564(18) 0.65419(11) 0.0300(7) Uani ? C(22) 0.6526(3) 0.35104(19) 0.61309(12) 0.0319(7) Uani ? C(23) 0.7356(3) 0.43963(19) 0.61642(13) 0.0343(7) Uani ? C(24) 0.8540(3) 0.42170(19) 0.66348(12) 0.0330(7) Uani ? C(25) 0.9675(4) 0.4852(2) 0.68950(15) 0.0459(9) Uani ? C(26) 1.0661(4) 0.4486(3) 0.73617(16) 0.0554(10) Uani ? C(27) 1.0610(4) 0.3471(3) 0.75752(14) 0.0561(10) Uani ? C(28) 0.9551(4) 0.2827(2) 0.73350(13) 0.0449(9) Uani ? C(29) 0.8473(3) 0.3204(2) 0.68704(12) 0.0335(7) Uani ? C(41) 0.4735(3) -0.0335(2) 0.71752(14) 0.0444(9) Uani ? C(61) 0.7674(4) -0.0587(2) 0.55409(13) 0.0390(8) Uani ? C(62) 0.7227(5) -0.1712(2) 0.55300(17) 0.0591(12) Uani ? C(63) 0.9229(4) -0.0568(2) 0.56892(17) 0.0513(10) Uani ? C(64) 0.7133(5) -0.0135(3) 0.48908(13) 0.0559(12) Uani ? C(71) 0.6794(4) 0.3856(3) 0.45911(15) 0.0551(10) Uani ? C(72) 0.8823(5) 0.3016(3) 0.45091(16) 0.0662(14) Uani ? C(81) 1.1448(4) 0.2241(3) 0.62434(15) 0.0499(10) Uani ? C(82) 1.1238(4) 0.3888(3) 0.57380(17) 0.0525(10) Uani ? C(221) 0.5122(3) 0.3355(2) 0.57479(14) 0.0417(8) Uani ? C(231) 0.7002(4) 0.5424(2) 0.58625(16) 0.0487(9) Uani ? C(42A) 0.3511(12) -0.0820(12) 0.6745(4) 0.093(4) Uani ? C(42B) 0.449(2) -0.1464(8) 0.7012(9) 0.135(8) Uani ? C(43A) 0.5554(10) -0.1178(7) 0.7577(5) 0.069(3) Uani ? C(43B) 0.5456(13) -0.0233(15) 0.7861(4) 0.132(6) Uani ? C(44A) 0.4183(14) 0.0408(6) 0.7600(5) 0.087(4) Uani ? C(44B) 0.3390(9) 0.0230(10) 0.7062(6) 0.092(4) Uani ? H(3) 0.5650 0.1599 0.7148 0.0400 Uiso calc H(5) 0.6022 -0.1067 0.6318 0.0400 Uiso calc H(25) 0.9737 0.5511 0.6745 0.0550 Uiso calc H(26) 1.1381 0.4909 0.7544 0.0670 Uiso calc H(27) 1.1315 0.3233 0.7888 0.0670 Uiso calc H(28) 0.9543 0.2157 0.7475 0.0540 Uiso calc H(22A) 0.4778 0.3992 0.5561 0.0630 Uiso calc H(22B) 0.4532 0.3112 0.6007 0.0630 Uiso calc H(22C) 0.5152 0.2861 0.5430 0.0630 Uiso calc H(23A) 0.6141 0.5379 0.5573 0.0730 Uiso calc H(23B) 0.7700 0.5624 0.5649 0.0730 Uiso calc H(23C) 0.6940 0.5922 0.6174 0.0730 Uiso calc H(42A) 0.2911 -0.1107 0.6986 0.1400 Uiso calc H(42B) 0.3819 -0.1351 0.6508 0.1400 Uiso calc H(42C) 0.3031 -0.0310 0.6470 0.1400 Uiso calc H(42D) 0.3859 -0.1742 0.7242 0.2020 Uiso calc H(42E) 0.5337 -0.1829 0.7116 0.2020 Uiso calc H(42F) 0.4111 -0.1530 0.6577 0.2020 Uiso calc H(43A) 0.6307 -0.0877 0.7863 0.1040 Uiso calc H(43B) 0.5895 -0.1655 0.7315 0.1040 Uiso calc H(43C) 0.4973 -0.1530 0.7801 0.1040 Uiso calc H(43D) 0.4999 0.0276 0.8056 0.1990 Uiso calc H(43E) 0.6389 -0.0033 0.7889 0.1990 Uiso calc H(43F) 0.5429 -0.0878 0.8066 0.1990 Uiso calc H(44A) 0.3671 0.0940 0.7355 0.1300 Uiso calc H(44B) 0.4933 0.0704 0.7892 0.1300 Uiso calc H(44C) 0.3601 0.0046 0.7820 0.1300 Uiso calc H(44D) 0.3023 0.0276 0.6625 0.1390 Uiso calc H(44E) 0.3532 0.0905 0.7234 0.1390 Uiso calc H(44F) 0.2760 -0.0132 0.7256 0.1390 Uiso calc H(62A) 0.7613 -0.2081 0.5233 0.0890 Uiso calc H(62B) 0.6248 -0.1751 0.5417 0.0890 Uiso calc H(62C) 0.7539 -0.2007 0.5933 0.0890 Uiso calc H(63A) 0.9541 0.0122 0.5667 0.0770 Uiso calc H(63B) 0.9563 -0.0984 0.5395 0.0770 Uiso calc H(63C) 0.9564 -0.0831 0.6099 0.0770 Uiso calc H(64A) 0.7436 0.0559 0.4881 0.0840 Uiso calc H(64B) 0.6153 -0.0154 0.4796 0.0840 Uiso calc H(64C) 0.7473 -0.0530 0.4590 0.0840 Uiso calc H(71A) 0.6998 0.4310 0.4282 0.0830 Uiso calc H(71B) 0.6346 0.4229 0.4865 0.0830 Uiso calc H(71C) 0.6206 0.3319 0.4394 0.0830 Uiso calc H(72A) 0.8330 0.2459 0.4281 0.0990 Uiso calc H(72B) 0.9694 0.2776 0.4734 0.0990 Uiso calc H(72C) 0.8957 0.3545 0.4227 0.0990 Uiso calc H(81A) 1.2137 0.2073 0.6017 0.0750 Uiso calc H(81B) 1.0948 0.1635 0.6301 0.0750 Uiso calc H(81C) 1.1872 0.2518 0.6640 0.0750 Uiso calc H(82A) 1.1707 0.4220 0.6110 0.0790 Uiso calc H(82B) 1.0593 0.4353 0.5499 0.0790 Uiso calc H(82C) 1.1887 0.3680 0.5499 0.0790 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 0.0262(3) 0.0265(2) 0.0312(2) 0.00130(18) 0.00861(17) 0.00194(16) O(1) 0.0360(12) 0.0257(8) 0.0399(9) 0.0004(7) 0.0202(9) 0.0002(7) N(7) 0.0430(16) 0.0381(12) 0.0353(11) 0.0015(10) 0.0086(10) 0.0059(9) N(8) 0.0290(14) 0.0387(12) 0.0458(13) 0.0015(10) 0.0109(10) -0.0016(10) C(1) 0.0298(15) 0.0260(11) 0.0277(11) -0.0007(10) 0.0083(10) 0.0025(9) C(2) 0.0332(16) 0.0265(12) 0.0305(12) 0.0022(10) 0.0104(10) 0.0028(9) C(3) 0.0351(16) 0.0359(13) 0.0305(12) 0.0029(11) 0.0116(11) 0.0039(10) C(4) 0.0346(16) 0.0371(14) 0.0327(12) -0.0040(11) 0.0101(11) 0.0101(10) C(5) 0.0381(17) 0.0273(12) 0.0324(12) -0.0059(11) 0.0052(11) 0.0037(9) C(6) 0.0334(16) 0.0280(12) 0.0265(11) -0.0002(10) 0.0050(10) 0.0011(9) C(21) 0.0332(16) 0.0277(12) 0.0329(12) 0.0000(10) 0.0153(11) -0.0033(9) C(22) 0.0322(16) 0.0292(12) 0.0373(13) 0.0043(10) 0.0140(11) -0.0010(10) C(23) 0.0333(16) 0.0291(12) 0.0418(14) 0.0036(11) 0.0111(12) -0.0025(10) C(24) 0.0371(17) 0.0296(12) 0.0344(12) -0.0006(11) 0.0123(11) -0.0053(10) C(25) 0.046(2) 0.0426(16) 0.0500(16) -0.0079(14) 0.0120(14) -0.0124(13) C(26) 0.046(2) 0.063(2) 0.0512(18) -0.0119(16) -0.0033(15) -0.0165(15) C(27) 0.045(2) 0.079(2) 0.0369(16) 0.0020(17) -0.0075(14) -0.0054(15) C(28) 0.050(2) 0.0509(17) 0.0319(14) 0.0042(14) 0.0043(13) 0.0001(11) C(29) 0.0359(17) 0.0351(13) 0.0315(12) 0.0025(11) 0.0119(11) -0.0051(10) C(41) 0.044(2) 0.0490(17) 0.0443(16) -0.0050(14) 0.0183(14) 0.0167(13) C(61) 0.056(2) 0.0270(13) 0.0355(13) -0.0013(12) 0.0132(13) -0.0035(10) C(62) 0.088(3) 0.0349(16) 0.059(2) -0.0103(17) 0.026(2) -0.0145(14) C(63) 0.058(2) 0.0366(16) 0.066(2) 0.0121(15) 0.0283(18) -0.0014(14) C(64) 0.082(3) 0.0552(19) 0.0308(14) 0.0051(18) 0.0126(15) -0.0040(13) C(71) 0.047(2) 0.072(2) 0.0438(17) 0.0068(17) 0.0042(14) 0.0129(15) C(72) 0.078(3) 0.077(3) 0.0435(18) 0.029(2) 0.0126(18) -0.0073(16) C(81) 0.036(2) 0.060(2) 0.0525(18) 0.0098(14) 0.0069(14) -0.0004(14) C(82) 0.036(2) 0.0558(19) 0.068(2) -0.0115(15) 0.0165(16) -0.0005(15) C(221) 0.0302(17) 0.0483(16) 0.0456(15) 0.0014(12) 0.0057(12) 0.0023(12) C(231) 0.051(2) 0.0310(14) 0.0631(19) 0.0043(13) 0.0101(16) 0.0093(13) C(42A) 0.068(7) 0.146(11) 0.068(5) -0.070(7) 0.019(5) 0.010(6) C(42B) 0.163(17) 0.077(7) 0.212(18) -0.015(8) 0.146(16) 0.023(9) C(43A) 0.079(7) 0.069(5) 0.063(5) -0.009(5) 0.025(5) 0.038(4) C(43B) 0.074(9) 0.264(19) 0.060(6) -0.017(10) 0.016(5) 0.087(9) C(44A) 0.129(10) 0.067(5) 0.094(7) -0.026(6) 0.092(8) -0.001(5) C(44B) 0.043(6) 0.134(9) 0.110(8) 0.004(5) 0.038(6) 0.066(7) # 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) 1.8894(18) YES Ti N(8) 1.898(3) YES Ti N(7) 1.929(2) YES Ti C(21) 2.365(2) YES Ti C(29) 2.411(2) YES Ti C(22) 2.428(3) YES Ti C(23) 2.430(3) YES Ti C(24) 2.441(2) YES O(1) C(1) 1.363(3) YES N(7) C(71) 1.445(4) YES N(7) C(72) 1.453(4) YES N(8) C(81) 1.452(4) YES N(8) C(82) 1.460(4) YES C(1) C(6) 1.402(3) YES C(1) C(2) 1.405(3) YES C(2) C(3) 1.390(4) YES C(2) C(21) 1.482(3) YES C(3) C(4) 1.385(4) YES C(4) C(5) 1.405(4) YES C(4) C(41) 1.538(4) YES C(5) C(6) 1.393(4) YES C(6) C(61) 1.535(3) YES C(21) C(29) 1.419(4) YES C(21) C(22) 1.425(4) YES C(22) C(23) 1.419(4) YES C(22) C(221) 1.494(4) YES C(23) C(24) 1.421(4) YES C(23) C(231) 1.508(4) YES C(24) C(25) 1.426(4) YES C(24) C(29) 1.431(4) YES C(25) C(26) 1.354(5) YES C(26) C(27) 1.414(5) YES C(27) C(28) 1.370(5) YES C(28) C(29) 1.411(4) YES C(41) C(44B) 1.510(9) YES C(41) C(42A) 1.521(8) YES C(41) C(42B) 1.527(10) YES C(41) C(44A) 1.535(7) YES C(41) C(43A) 1.538(8) YES C(41) C(43B) 1.539(10) YES C(61) C(63) 1.522(5) YES C(61) C(62) 1.537(4) YES C(61) C(64) 1.541(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 N(8) 99.92(9) YES O(1) Ti N(7) 104.55(10) YES N(8) Ti N(7) 100.66(11) YES O(1) Ti C(21) 74.70(8) YES N(8) Ti C(21) 129.48(10) YES N(7) Ti C(21) 129.62(11) YES O(1) Ti C(29) 93.73(8) YES N(8) Ti C(29) 98.48(11) YES N(7) Ti C(29) 150.67(10) YES C(21) Ti C(29) 34.55(10) YES O(1) Ti C(22) 95.69(8) YES N(8) Ti C(22) 151.56(10) YES N(7) Ti C(22) 98.20(10) YES C(21) Ti C(22) 34.56(9) YES C(29) Ti C(22) 56.66(10) YES O(1) Ti C(23) 129.04(9) YES N(8) Ti C(23) 123.22(10) YES N(7) Ti C(23) 93.58(10) YES C(21) Ti C(23) 57.68(9) YES C(29) Ti C(23) 57.23(9) YES C(22) Ti C(23) 33.96(9) YES O(1) Ti C(24) 127.55(8) YES N(8) Ti C(24) 95.95(10) YES N(7) Ti C(24) 121.06(10) YES C(21) Ti C(24) 57.08(9) YES C(29) Ti C(24) 34.29(9) YES C(22) Ti C(24) 55.89(10) YES C(23) Ti C(24) 33.92(10) YES C(1) O(1) Ti 127.46(15) YES C(71) N(7) C(72) 108.5(3) YES C(71) N(7) Ti 131.7(2) YES C(72) N(7) Ti 117.7(2) YES C(81) N(8) C(82) 112.1(3) YES C(81) N(8) Ti 126.4(2) YES C(82) N(8) Ti 120.3(2) YES O(1) C(1) C(6) 123.0(2) YES O(1) C(1) C(2) 116.3(2) YES C(6) C(1) C(2) 120.7(2) YES C(3) C(2) C(1) 120.4(2) YES C(3) C(2) C(21) 125.9(2) YES C(1) C(2) C(21) 113.7(2) YES C(4) C(3) C(2) 120.9(2) YES C(3) C(4) C(5) 117.1(2) YES C(3) C(4) C(41) 121.5(2) YES C(5) C(4) C(41) 121.3(2) YES C(6) C(5) C(4) 124.3(2) YES C(5) C(6) C(1) 116.5(2) YES C(5) C(6) C(61) 122.8(2) YES C(1) C(6) C(61) 120.6(2) YES C(29) C(21) C(22) 107.7(2) YES C(29) C(21) C(2) 126.8(2) YES C(22) C(21) C(2) 124.5(3) YES C(29) C(21) Ti 74.53(15) YES C(22) C(21) Ti 75.15(14) YES C(2) C(21) Ti 107.58(15) YES C(23) C(22) C(21) 108.9(3) YES C(23) C(22) C(221) 127.7(3) YES C(21) C(22) C(221) 123.4(2) YES C(23) C(22) Ti 73.09(16) YES C(21) C(22) Ti 70.28(14) YES C(221) C(22) Ti 123.49(18) YES C(22) C(23) C(24) 107.0(2) YES C(22) C(23) C(231) 128.7(3) YES C(24) C(23) C(231) 123.4(3) YES C(22) C(23) Ti 72.95(14) YES C(24) C(23) Ti 73.47(15) YES C(231) C(23) Ti 127.3(2) YES C(23) C(24) C(25) 132.0(3) YES C(23) C(24) C(29) 108.8(2) YES C(25) C(24) C(29) 119.2(3) YES C(23) C(24) Ti 72.61(14) YES C(25) C(24) Ti 122.6(2) YES C(29) C(24) Ti 71.72(14) YES C(26) C(25) C(24) 119.4(3) YES C(25) C(26) C(27) 120.9(3) YES C(28) C(27) C(26) 121.9(3) YES C(27) C(28) C(29) 118.5(3) YES C(28) C(29) C(21) 132.6(3) YES C(28) C(29) C(24) 120.0(3) YES C(21) C(29) C(24) 107.4(2) YES C(28) C(29) Ti 119.23(19) YES C(21) C(29) Ti 70.92(14) YES C(24) C(29) Ti 73.99(14) YES C(44B) C(41) C(42A) 61.9(8) YES C(44B) C(41) C(42B) 109.8(10) YES C(42A) C(41) C(42B) 51.7(9) YES C(44B) C(41) C(44A) 50.6(7) YES C(42A) C(41) C(44A) 107.4(8) YES C(42B) C(41) C(44A) 134.0(5) YES C(44B) C(41) C(4) 108.8(4) YES C(42A) C(41) C(4) 110.4(4) YES C(42B) C(41) C(4) 112.5(4) YES C(44A) C(41) C(4) 113.3(3) YES C(44B) C(41) C(43A) 142.5(5) YES C(42A) C(41) C(43A) 108.7(7) YES C(42B) C(41) C(43A) 58.8(9) YES C(44A) C(41) C(43A) 108.6(6) YES C(4) C(41) C(43A) 108.3(4) YES C(44B) C(41) C(43B) 109.6(9) YES C(42A) C(41) C(43B) 142.9(6) YES C(42B) C(41) C(43B) 109.5(11) YES C(44A) C(41) C(43B) 59.8(8) YES C(4) C(41) C(43B) 106.5(5) YES C(43A) C(41) C(43B) 54.1(7) YES C(63) C(61) C(6) 111.0(2) YES C(63) C(61) C(62) 107.5(3) YES C(6) C(61) C(62) 111.8(2) YES C(63) C(61) C(64) 109.6(3) YES C(6) C(61) C(64) 109.0(2) YES C(62) C(61) C(64) 108.0(3) YES #======================================================================= #====== data_LTZRIP _database_code_CSD 201169 _audit_creation_date 17-03-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C27 H38 N2 O1 Zr1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 497.84 _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 12.9534(3) _cell_length_b 14.0719(4) _cell_length_c 15.2631(4) _cell_angle_alpha 96.9498(9) _cell_angle_beta 109.8424(10) _cell_angle_gamma 91.8953(14) _cell_volume 2589.5(2) _cell_measurement_reflns_used 27287 _cell_measurement_theta_min 5 _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 0.435 _cell_measurement_temperature 150 _exptl_crystal_F_000 1048 # 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,_ _exptl_absorpt_correction_T_min 0.1181 _exptl_absorpt_correction_T_max 0.9067 _diffrn_reflns_number 27287 _reflns_number_total 11660 _reflns_number_gt 9145 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_max 18 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.40' # 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 0.048 _refine_ls_wR_factor_ref 0.118 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 11659 _refine_ls_number_parameters 610 _refine_ls_number_restraints 6 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.59 _refine_diff_density_min -1.23 _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 Zr(1) Zr 0.18546(2) 0.124281(19) 0.215290(18) 0.02120(9) Uani 1 1 d . . . Zr(2) Zr 0.18763(2) -0.391910(19) -0.284695(18) 0.02024(9) Uani 1 1 d . . . O(11) O 0.17311(15) 0.20379(14) 0.11060(14) 0.0245(4) Uani 1 1 d . . . O(21) O 0.16962(15) -0.30619(14) -0.38623(13) 0.0238(4) Uani 1 1 d . . . N(17) N 0.0309(2) 0.0750(2) 0.20208(19) 0.0365(7) Uani 1 1 d . . . N(18) N 0.2391(2) 0.22100(19) 0.33504(18) 0.0316(6) Uani 1 1 d . . . N(27) N 0.03396(19) -0.43483(19) -0.28846(18) 0.0301(6) Uani 1 1 d . . . N(28) N 0.2539(2) -0.30335(18) -0.16067(17) 0.0269(6) Uani 1 1 d . . . C(11) C 0.2166(2) 0.1895(2) 0.04088(19) 0.0206(6) Uani 1 1 d . . . C(12) C 0.2848(2) 0.11308(19) 0.04298(19) 0.0203(6) Uani 1 1 d . . . C(13) C 0.3354(2) 0.0966(2) -0.0232(2) 0.0226(6) Uani 1 1 d . . . C(14) C 0.3180(2) 0.1534(2) -0.09513(19) 0.0216(6) Uani 1 1 d . . . C(15) C 0.2476(2) 0.2263(2) -0.0969(2) 0.0227(6) Uani 1 1 d . . . C(16) C 0.1951(2) 0.2470(2) -0.0319(2) 0.0229(6) Uani 1 1 d . . . C(21) C 0.2121(2) -0.3138(2) -0.45679(19) 0.0193(6) Uani 1 1 d . . . C(22) C 0.2778(2) -0.39071(19) -0.46136(19) 0.0189(6) Uani 1 1 d . . . C(23) C 0.3286(2) -0.40055(19) -0.52814(19) 0.0211(6) Uani 1 1 d . . . C(24) C 0.3137(2) -0.33644(19) -0.59349(19) 0.0198(6) Uani 1 1 d . A . C(25) C 0.2444(2) -0.2636(2) -0.58944(19) 0.0216(6) Uani 1 1 d . . . C(26) C 0.1917(2) -0.2495(2) -0.5236(2) 0.0211(6) Uani 1 1 d . . . C(121) C 0.2948(2) 0.0527(2) 0.1184(2) 0.0226(6) Uani 1 1 d . . . C(122) C 0.2195(2) -0.0228(2) 0.1169(2) 0.0282(7) Uani 1 1 d . . . C(123) C 0.2414(3) -0.0459(2) 0.2086(2) 0.0310(7) Uani 1 1 d . . . C(124) C 0.3372(2) 0.0116(2) 0.2690(2) 0.0288(7) Uani 1 1 d . . . C(125) C 0.3979(3) 0.0211(2) 0.3674(2) 0.0391(8) Uani 1 1 d . . . C(126) C 0.4857(3) 0.0878(3) 0.4055(3) 0.0446(9) Uani 1 1 d . . . C(127) C 0.5182(2) 0.1481(2) 0.3502(2) 0.0367(8) Uani 1 1 d . . . C(128) C 0.4621(2) 0.1422(2) 0.2560(2) 0.0269(7) Uani 1 1 d . . . C(129) C 0.3709(2) 0.0729(2) 0.2131(2) 0.0232(6) Uani 1 1 d . . . C(141) C 0.3747(3) 0.1331(2) -0.1684(2) 0.0266(7) Uani 1 1 d . . . C(142) C 0.3548(3) 0.0267(3) -0.2087(3) 0.0525(10) Uani 1 1 d . . . C(143) C 0.3330(4) 0.1907(3) -0.2503(3) 0.0592(12) Uani 1 1 d . . . C(144) C 0.4973(3) 0.1544(3) -0.1220(3) 0.0530(11) Uani 1 1 d . . . C(161) C 0.1153(2) 0.3268(2) -0.0389(2) 0.0295(7) Uani 1 1 d . . . C(162) C 0.0987(3) 0.3756(3) -0.1270(3) 0.0469(10) Uani 1 1 d . . . C(163) C 0.0015(2) 0.2851(3) -0.0444(3) 0.0404(9) Uani 1 1 d . . . C(164) C 0.1618(3) 0.4047(2) 0.0462(2) 0.0361(8) Uani 1 1 d . . . C(171) C -0.0364(3) -0.0127(4) 0.1514(3) 0.0851(18) Uani 1 1 d . . . C(172) C -0.0297(3) 0.1270(4) 0.2532(5) 0.104(2) Uani 1 1 d . . . C(181) C 0.3070(3) 0.3089(2) 0.3502(2) 0.0380(8) Uani 1 1 d . . . C(182) C 0.2309(4) 0.1974(3) 0.4229(3) 0.0647(13) Uani 1 1 d . . . C(221) C 0.2870(2) -0.4579(2) -0.39177(19) 0.0209(6) Uani 1 1 d . . . C(222) C 0.2098(2) -0.5329(2) -0.3969(2) 0.0235(6) Uani 1 1 d . . . C(223) C 0.2350(2) -0.5648(2) -0.3083(2) 0.0266(7) Uani 1 1 d . . . C(224) C 0.3351(2) -0.5139(2) -0.2472(2) 0.0241(6) Uani 1 1 d . . . C(225) C 0.4026(2) -0.5171(2) -0.1519(2) 0.0321(7) Uani 1 1 d . . . C(226) C 0.4946(3) -0.4546(3) -0.1125(2) 0.0395(8) Uani 1 1 d . . . C(227) C 0.5245(2) -0.3880(2) -0.1631(2) 0.0342(8) Uani 1 1 d . . . C(228) C 0.4628(2) -0.3826(2) -0.2546(2) 0.0268(7) Uani 1 1 d . . . C(229) C 0.3679(2) -0.4471(2) -0.2987(2) 0.0218(6) Uani 1 1 d . . . C(22A) C 0.4252(11) -0.2477(8) -0.6658(11) 0.047(4) Uani 0.331(9) 1 d P A 1 C(22B) C 0.3463(6) -0.2708(4) -0.7337(5) 0.051(2) Uani 0.669(9) 1 d P A 2 C(23A) C 0.2806(11) -0.3659(14) -0.7609(7) 0.070(6) Uani 0.331(9) 1 d PU A 1 C(23B) C 0.3234(7) -0.4456(5) -0.7333(5) 0.066(3) Uani 0.669(9) 1 d P A 2 C(241) C 0.3679(3) -0.3484(2) -0.6688(2) 0.0268(7) Uani 1 1 d . . . C(24A) C 0.4532(13) -0.4162(10) -0.6487(11) 0.055(5) Uani 0.331(9) 1 d P A 1 C(24B) C 0.4905(5) -0.3517(7) -0.6249(5) 0.059(2) Uani 0.669(9) 1 d P A 2 C(261) C 0.1154(2) -0.1681(2) -0.5236(2) 0.0266(7) Uani 1 1 d . . . C(262) C 0.0999(3) -0.1115(3) -0.6065(3) 0.0411(9) Uani 1 1 d . . . C(263) C 0.0011(2) -0.2094(3) -0.5319(3) 0.0379(8) Uani 1 1 d . . . C(264) C 0.1660(3) -0.0974(2) -0.4339(2) 0.0410(8) Uani 1 1 d . . . C(271) C -0.0414(3) -0.5109(3) -0.3519(3) 0.0519(11) Uani 1 1 d . . . C(272) C -0.0164(3) -0.3904(3) -0.2229(3) 0.0522(10) Uani 1 1 d . . . C(281) C 0.3200(2) -0.2136(2) -0.1458(2) 0.0338(7) Uani 1 1 d . . . C(282) C 0.2591(3) -0.3348(3) -0.0718(2) 0.0463(9) Uani 1 1 d . . . H(13) H 0.3818 0.0471 -0.0199 0.029 Uiso 1 1 calc R . . H(15) H 0.2347 0.2639 -0.1450 0.030 Uiso 1 1 calc R . . H(23) H 0.3734 -0.4507 -0.5294 0.027 Uiso 1 1 calc R . . H(25) H 0.2326 -0.2215 -0.6338 0.028 Uiso 1 1 calc R . . H(122) H 0.1636 -0.0529 0.0633 0.037 Uiso 1 1 calc R . . H(123) H 0.2006 -0.0907 0.2263 0.040 Uiso 1 1 calc R . . H(125) H 0.3778 -0.0177 0.4051 0.051 Uiso 1 1 calc R . . H(126) H 0.5253 0.0938 0.4696 0.058 Uiso 1 1 calc R . . H(127) H 0.5788 0.1925 0.3785 0.048 Uiso 1 1 calc R . . H(128) H 0.4831 0.1829 0.2203 0.035 Uiso 1 1 calc R . . H(14A) H 0.3890 0.0145 -0.2553 0.068 Uiso 1 1 calc R . . H(14B) H 0.2771 0.0096 -0.2370 0.068 Uiso 1 1 calc R . . H(14C) H 0.3859 -0.0110 -0.1590 0.068 Uiso 1 1 calc R . . H(14D) H 0.3510 0.2579 -0.2274 0.077 Uiso 1 1 calc R . . H(14E) H 0.2546 0.1784 -0.2790 0.077 Uiso 1 1 calc R . . H(14F) H 0.3671 0.1719 -0.2958 0.077 Uiso 1 1 calc R . . H(14G) H 0.5329 0.1351 -0.1664 0.069 Uiso 1 1 calc R . . H(14H) H 0.5234 0.1197 -0.0693 0.069 Uiso 1 1 calc R . . H(14I) H 0.5137 0.2220 -0.1006 0.069 Uiso 1 1 calc R . . H(16A) H 0.0685 0.3288 -0.1822 0.061 Uiso 1 1 calc R . . H(16B) H 0.1683 0.4034 -0.1251 0.061 Uiso 1 1 calc R . . H(16C) H 0.0490 0.4251 -0.1288 0.061 Uiso 1 1 calc R . . H(16D) H -0.0289 0.2388 -0.1000 0.053 Uiso 1 1 calc R . . H(16E) H -0.0466 0.3360 -0.0469 0.053 Uiso 1 1 calc R . . H(16F) H 0.0090 0.2547 0.0102 0.053 Uiso 1 1 calc R . . H(16G) H 0.1106 0.4531 0.0426 0.047 Uiso 1 1 calc R . . H(16H) H 0.2305 0.4332 0.0468 0.047 Uiso 1 1 calc R . . H(16I) H 0.1737 0.3767 0.1029 0.047 Uiso 1 1 calc R . . H(17A) H -0.0552 -0.0476 0.1949 0.111 Uiso 1 1 calc R . . H(17B) H 0.0040 -0.0517 0.1205 0.111 Uiso 1 1 calc R . . H(17C) H -0.1026 0.0034 0.1054 0.111 Uiso 1 1 calc R . . H(17D) H -0.0913 0.1525 0.2099 0.135 Uiso 1 1 calc R . . H(17E) H 0.0175 0.1787 0.2967 0.135 Uiso 1 1 calc R . . H(17F) H -0.0557 0.0844 0.2872 0.135 Uiso 1 1 calc R . . H(18A) H 0.2775 0.3601 0.3796 0.049 Uiso 1 1 calc R . . H(18B) H 0.3082 0.3242 0.2909 0.049 Uiso 1 1 calc R . . H(18C) H 0.3806 0.3010 0.3902 0.049 Uiso 1 1 calc R . . H(18D) H 0.3033 0.1920 0.4666 0.084 Uiso 1 1 calc R . . H(18E) H 0.1876 0.1375 0.4111 0.084 Uiso 1 1 calc R . . H(18F) H 0.1965 0.2472 0.4490 0.084 Uiso 1 1 calc R . . H(222) H 0.1509 -0.5578 -0.4506 0.031 Uiso 1 1 calc R . . H(223) H 0.1936 -0.6108 -0.2927 0.035 Uiso 1 1 calc R . . H(225) H 0.3844 -0.5607 -0.1173 0.042 Uiso 1 1 calc R . . H(226) H 0.5387 -0.4562 -0.0504 0.051 Uiso 1 1 calc R . . H(227) H 0.5876 -0.3468 -0.1336 0.044 Uiso 1 1 calc R . . H(228) H 0.4827 -0.3376 -0.2871 0.035 Uiso 1 1 calc R . . H(22A) H 0.4499 -0.2487 -0.7185 0.071 Uiso 0.331(9) 1 calc PR A 1 H(22B) H 0.4872 -0.2330 -0.6084 0.071 Uiso 0.331(9) 1 calc PR A 1 H(22C) H 0.3738 -0.1996 -0.6686 0.071 Uiso 0.331(9) 1 calc PR A 1 H(22D) H 0.3797 -0.2856 -0.7805 0.077 Uiso 0.669(9) 1 calc PR A 2 H(22E) H 0.3772 -0.2096 -0.6973 0.077 Uiso 0.669(9) 1 calc PR A 2 H(22F) H 0.2683 -0.2687 -0.7639 0.077 Uiso 0.669(9) 1 calc PR A 2 H(23A) H 0.3127 -0.3731 -0.8093 0.105 Uiso 0.331(9) 1 calc PR A 1 H(23B) H 0.2354 -0.3126 -0.7688 0.105 Uiso 0.331(9) 1 calc PR A 1 H(23C) H 0.2362 -0.4234 -0.7651 0.105 Uiso 0.331(9) 1 calc PR A 1 H(23D) H 0.2447 -0.4472 -0.7615 0.100 Uiso 0.669(9) 1 calc PR A 2 H(23E) H 0.3424 -0.4973 -0.6966 0.100 Uiso 0.669(9) 1 calc PR A 2 H(23F) H 0.3554 -0.4524 -0.7817 0.100 Uiso 0.669(9) 1 calc PR A 2 H(24A) H 0.4196 -0.4800 -0.6569 0.082 Uiso 0.331(9) 1 calc PR A 1 H(24B) H 0.5026 -0.3997 -0.5850 0.082 Uiso 0.331(9) 1 calc PR A 1 H(24C) H 0.4934 -0.4135 -0.6910 0.082 Uiso 0.331(9) 1 calc PR A 1 H(24D) H 0.5219 -0.3634 -0.6735 0.088 Uiso 0.669(9) 1 calc PR A 2 H(24E) H 0.5060 -0.4024 -0.5866 0.088 Uiso 0.669(9) 1 calc PR A 2 H(24F) H 0.5220 -0.2915 -0.5866 0.088 Uiso 0.669(9) 1 calc PR A 2 H(26A) H 0.0693 -0.1543 -0.6646 0.053 Uiso 1 1 calc R . . H(26B) H 0.1698 -0.0826 -0.6024 0.053 Uiso 1 1 calc R . . H(26C) H 0.0508 -0.0624 -0.6044 0.053 Uiso 1 1 calc R . . H(26D) H -0.0318 -0.2495 -0.5913 0.049 Uiso 1 1 calc R . . H(26E) H -0.0443 -0.1578 -0.5275 0.049 Uiso 1 1 calc R . . H(26F) H 0.0078 -0.2468 -0.4819 0.049 Uiso 1 1 calc R . . H(26G) H 0.1184 -0.0467 -0.4335 0.053 Uiso 1 1 calc R . . H(26H) H 0.2364 -0.0709 -0.4313 0.053 Uiso 1 1 calc R . . H(26I) H 0.1751 -0.1301 -0.3804 0.053 Uiso 1 1 calc R . . H(27A) H -0.0527 -0.5603 -0.3172 0.068 Uiso 1 1 calc R . . H(27B) H -0.0112 -0.5372 -0.3982 0.068 Uiso 1 1 calc R . . H(27C) H -0.1104 -0.4857 -0.3827 0.068 Uiso 1 1 calc R . . H(27D) H -0.0798 -0.3594 -0.2568 0.068 Uiso 1 1 calc R . . H(27E) H 0.0359 -0.3437 -0.1767 0.068 Uiso 1 1 calc R . . H(27F) H -0.0384 -0.4388 -0.1921 0.068 Uiso 1 1 calc R . . H(28A) H 0.2932 -0.1645 -0.1116 0.044 Uiso 1 1 calc R . . H(28B) H 0.3150 -0.1951 -0.2056 0.044 Uiso 1 1 calc R . . H(28C) H 0.3953 -0.2217 -0.1106 0.044 Uiso 1 1 calc R . . H(28D) H 0.3344 -0.3405 -0.0346 0.060 Uiso 1 1 calc R . . H(28E) H 0.2181 -0.3960 -0.0840 0.060 Uiso 1 1 calc R . . H(28F) H 0.2280 -0.2887 -0.0383 0.060 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 Zr(1) 0.02048(16) 0.02351(16) 0.02177(17) 0.00224(11) 0.00860(12) 0.00746(12) Zr(2) 0.01971(16) 0.02324(16) 0.01817(16) 0.00093(11) 0.00691(12) 0.00361(11) O(11) 0.0280(10) 0.0266(11) 0.0246(11) 0.0096(8) 0.0140(9) 0.0086(9) O(21) 0.0295(11) 0.0267(11) 0.0210(10) 0.0096(8) 0.0152(9) 0.0046(8) N(17) 0.0243(13) 0.0516(18) 0.0356(16) -0.0042(12) 0.0107(12) 0.0151(14) N(18) 0.0355(15) 0.0297(15) 0.0316(15) 0.0025(11) 0.0150(12) 0.0014(11) N(27) 0.0232(13) 0.0404(16) 0.0266(14) -0.0026(11) 0.0063(11) 0.0129(12) N(28) 0.0268(13) 0.0309(14) 0.0212(13) -0.0007(10) 0.0073(11) 0.0008(10) C(11) 0.0192(13) 0.0232(14) 0.0209(14) 0.0007(11) 0.0085(12) 0.0045(11) C(12) 0.0203(14) 0.0193(14) 0.0202(14) 0.0012(10) 0.0051(12) 0.0043(11) C(13) 0.0235(14) 0.0195(14) 0.0254(15) 0.0027(11) 0.0091(12) 0.0033(12) C(14) 0.0246(14) 0.0209(14) 0.0187(14) -0.0004(11) 0.0075(12) 0.0014(11) C(15) 0.0258(15) 0.0229(15) 0.0202(15) 0.0020(11) 0.0070(12) 0.0084(12) C(16) 0.0213(14) 0.0231(15) 0.0226(15) 0.0033(11) 0.0046(12) 0.0056(12) C(21) 0.0202(14) 0.0223(14) 0.0165(14) 0.0014(10) 0.0077(11) 0.0028(11) C(22) 0.0197(13) 0.0189(13) 0.0169(14) -0.0002(10) 0.0051(11) 0.0025(11) C(23) 0.0218(14) 0.0195(14) 0.0220(15) 0.0027(10) 0.0079(12) 0.0015(11) C(24) 0.0228(14) 0.0194(14) 0.0185(14) 0.0016(10) 0.0096(12) 0.0006(11) C(25) 0.0238(14) 0.0220(14) 0.0187(14) 0.0022(11) 0.0061(12) 0.0057(11) C(26) 0.0190(13) 0.0209(14) 0.0239(15) 0.0047(10) 0.0075(12) 0.0039(11) C(121) 0.0261(15) 0.0208(14) 0.0249(15) 0.0073(11) 0.0123(13) 0.0059(12) C(122) 0.0347(17) 0.0201(15) 0.0317(17) 0.0000(12) 0.0141(14) 0.0034(13) C(123) 0.0389(18) 0.0217(15) 0.0389(19) 0.0022(12) 0.0193(15) 0.0119(13) C(124) 0.0359(17) 0.0260(16) 0.0323(17) 0.0122(13) 0.0167(14) 0.0169(13) C(125) 0.045(2) 0.041(2) 0.0353(19) 0.0145(16) 0.0115(16) 0.0231(16) C(126) 0.044(2) 0.051(2) 0.033(2) 0.0177(17) 0.0009(16) 0.0178(17) C(127) 0.0250(16) 0.0401(19) 0.0372(19) 0.0054(13) -0.0002(15) 0.0069(15) C(128) 0.0204(14) 0.0278(16) 0.0342(17) 0.0057(11) 0.0092(13) 0.0107(13) C(129) 0.0227(14) 0.0236(15) 0.0260(16) 0.0079(11) 0.0097(12) 0.0086(12) C(141) 0.0386(17) 0.0235(15) 0.0217(15) 0.0019(12) 0.0160(14) 0.0025(12) C(142) 0.078(3) 0.038(2) 0.053(2) -0.0062(19) 0.044(2) -0.0098(18) C(143) 0.084(3) 0.075(3) 0.041(2) 0.041(2) 0.041(2) 0.028(2) C(144) 0.047(2) 0.078(3) 0.042(2) -0.004(2) 0.0281(19) 0.002(2) C(161) 0.0321(16) 0.0321(17) 0.0322(18) 0.0150(13) 0.0156(14) 0.0175(14) C(162) 0.059(2) 0.052(2) 0.043(2) 0.0306(18) 0.0246(18) 0.0277(19) C(163) 0.0269(17) 0.052(2) 0.046(2) 0.0152(15) 0.0118(16) 0.0184(18) C(164) 0.0446(19) 0.0263(17) 0.046(2) 0.0166(14) 0.0241(17) 0.0083(15) C(171) 0.039(2) 0.118(5) 0.080(4) -0.025(3) 0.020(2) -0.044(3) C(172) 0.038(2) 0.063(3) 0.204(7) 0.001(2) 0.049(3) -0.026(4) C(181) 0.0301(18) 0.0390(19) 0.040(2) 0.0008(14) 0.0094(15) -0.0030(15) C(182) 0.095(3) 0.069(3) 0.033(2) -0.017(3) 0.030(2) 0.001(2) C(221) 0.0224(14) 0.0207(14) 0.0203(14) 0.0049(11) 0.0073(12) 0.0049(11) C(222) 0.0278(15) 0.0214(14) 0.0197(15) -0.0002(11) 0.0066(12) 0.0023(11) C(223) 0.0331(16) 0.0199(15) 0.0297(17) -0.0005(12) 0.0133(14) 0.0086(12) C(224) 0.0268(15) 0.0257(15) 0.0227(15) 0.0059(12) 0.0103(13) 0.0081(12) C(225) 0.0339(17) 0.0370(18) 0.0295(17) 0.0092(14) 0.0119(14) 0.0161(14) C(226) 0.0314(18) 0.058(2) 0.0250(17) 0.0048(16) 0.0014(14) 0.0152(16) C(227) 0.0196(15) 0.046(2) 0.0354(19) -0.0009(13) 0.0068(14) 0.0073(15) C(228) 0.0231(15) 0.0294(16) 0.0300(17) 0.0059(12) 0.0104(13) 0.0073(13) C(229) 0.0241(15) 0.0251(15) 0.0199(14) 0.0081(11) 0.0109(12) 0.0059(12) C(22A) 0.056(8) 0.032(6) 0.073(10) 0.002(5) 0.046(8) 0.015(6) C(22B) 0.075(5) 0.046(4) 0.062(5) 0.023(3) 0.054(4) 0.024(3) C(23A) 0.078(10) 0.118(16) 0.018(6) -0.015(9) 0.033(6) -0.013(7) C(23B) 0.108(6) 0.047(4) 0.057(4) -0.029(4) 0.059(5) -0.024(3) C(241) 0.0376(17) 0.0248(15) 0.0268(16) 0.0056(12) 0.0211(14) 0.0071(12) C(24A) 0.097(12) 0.038(7) 0.077(10) 0.057(8) 0.076(10) 0.045(8) C(24B) 0.058(4) 0.085(6) 0.050(4) 0.015(4) 0.040(3) 0.012(4) C(261) 0.0304(16) 0.0268(16) 0.0271(16) 0.0125(12) 0.0131(13) 0.0088(13) C(262) 0.049(2) 0.039(2) 0.049(2) 0.0234(16) 0.0278(18) 0.0237(17) C(263) 0.0287(17) 0.044(2) 0.048(2) 0.0154(14) 0.0170(16) 0.0191(17) C(264) 0.051(2) 0.0287(18) 0.047(2) 0.0148(15) 0.0222(18) 0.0011(16) C(271) 0.0319(19) 0.080(3) 0.038(2) -0.0188(19) 0.0115(17) -0.006(2) C(272) 0.034(2) 0.053(2) 0.070(3) 0.0059(17) 0.022(2) -0.002(2) C(281) 0.0303(17) 0.0337(18) 0.0344(18) -0.0049(13) 0.0108(15) -0.0032(14) C(282) 0.063(2) 0.047(2) 0.0271(19) -0.0081(18) 0.0160(18) 0.0026(16) # 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. ; #======================================================================= #====== data_LTP33C _database_code_CSD 201170 _audit_creation_date 6-02-03 _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 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C49 H54 O3 Si2 Ti1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 795.05 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9436(10) _cell_length_b 13.1268(10) _cell_length_c 16.1538(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.861(4) _cell_angle_gamma 90.00 _cell_volume 2469.1(6) _cell_measurement_reflns_used 12676 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.07 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.252 _cell_measurement_temperature 150 _exptl_crystal_F_000 844 # 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,_ _exptl_absorpt_correction_T_min 0.7689 _exptl_absorpt_correction_T_max 0.9390 _diffrn_reflns_number 12676 _reflns_number_total 7600 _reflns_friedl_coverage 0.7584 _reflns_number_gt 7385 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 25.70 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 19 # 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 0.087 _refine_ls_wR_factor_ref 0.187 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7586 _refine_ls_number_parameters 508 _refine_ls_number_restraints 1 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+4.8002P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.005 _refine_diff_density_max 0.69 _refine_diff_density_min -0.36 _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) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) # 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 0.58378(8) 0.74058(8) 0.89545(6) 0.0213(2) Uani 1 1 d . . . Si(22) Si 0.44980(15) 0.74257(17) 1.13366(11) 0.0327(4) Uani 1 1 d . . . Si(32) Si 0.81450(14) 0.58497(14) 0.74179(9) 0.0236(4) Uani 1 1 d . . . O(1) O 0.4644(3) 0.6894(3) 0.8117(2) 0.0230(9) Uani 1 1 d . . . O(2) O 0.5633(3) 0.6629(3) 0.9860(2) 0.0251(9) Uani 1 1 d . . . O(3) O 0.7284(3) 0.6962(3) 0.8841(2) 0.0235(9) Uani 1 1 d . . . C(1) C 0.3756(5) 0.7426(6) 0.7605(3) 0.0223(11) Uani 1 1 d . . . C(2) C 0.3833(5) 0.8479(5) 0.7661(4) 0.0230(13) Uani 1 1 d . . . C(3) C 0.3030(5) 0.9093(5) 0.7145(3) 0.0234(13) Uani 1 1 d . . . C(4) C 0.2113(5) 0.8648(5) 0.6573(3) 0.0243(13) Uani 1 1 d . . . C(5) C 0.2033(5) 0.7590(5) 0.6564(3) 0.0220(13) Uani 1 1 d . . . C(6) C 0.2836(5) 0.6940(5) 0.7069(3) 0.0219(12) Uani 1 1 d . . . C(11) C 0.4820(5) 0.8854(4) 0.8313(4) 0.0227(13) Uani 1 1 d . . . C(12) C 0.4853(6) 0.8858(5) 0.9207(4) 0.0266(14) Uani 1 1 d . . . C(13) C 0.6022(5) 0.8981(5) 0.9650(4) 0.0259(14) Uani 1 1 d . . . C(14) C 0.6697(5) 0.9111(4) 0.9046(4) 0.0279(14) Uani 1 1 d . . . C(15) C 0.7901(6) 0.9295(5) 0.9132(5) 0.0398(18) Uani 1 1 d . . . C(16) C 0.8300(7) 0.9390(6) 0.8393(6) 0.050(2) Uani 1 1 d . . . C(17) C 0.7575(6) 0.9303(6) 0.7588(6) 0.0424(18) Uani 1 1 d . . . C(18) C 0.6449(6) 0.9101(5) 0.7495(4) 0.0327(15) Uani 1 1 d . . . C(19) C 0.5976(5) 0.9014(4) 0.8212(4) 0.0256(13) Uani 1 1 d . . . C(21) C 0.6421(5) 0.6737(5) 1.0607(3) 0.0216(13) Uani 1 1 d . . . C(22) C 0.6044(5) 0.7162(4) 1.1308(4) 0.0235(13) Uani 1 1 d . . . C(23) C 0.6878(5) 0.7360(6) 1.2021(4) 0.0296(13) Uani 1 1 d . . . C(24) C 0.8061(5) 0.7184(4) 1.2092(3) 0.0241(14) Uani 1 1 d . . . C(25) C 0.8912(6) 0.7446(6) 1.2818(4) 0.0356(15) Uani 1 1 d . . . C(26) C 1.0042(6) 0.7261(5) 1.2868(4) 0.0378(17) Uani 1 1 d . . . C(27) C 1.0392(6) 0.6781(5) 1.2176(4) 0.0304(15) Uani 1 1 d . . . C(28) C 0.9592(5) 0.6504(5) 1.1473(4) 0.0226(13) Uani 1 1 d . . . C(29) C 0.8419(5) 0.6696(5) 1.1393(3) 0.0222(13) Uani 1 1 d . . . C(2A) C 0.7547(5) 0.6443(4) 1.0648(3) 0.0208(12) Uani 1 1 d . . . C(31) C 0.7807(5) 0.6072(4) 0.9145(3) 0.0216(13) Uani 1 1 d . . . C(32) C 0.8275(5) 0.5482(5) 0.8567(4) 0.0232(14) Uani 1 1 d . . . C(33) C 0.8829(5) 0.4580(5) 0.8861(4) 0.0242(13) Uani 1 1 d . . . C(34) C 0.8845(5) 0.4199(5) 0.9684(4) 0.0249(13) Uani 1 1 d . . . C(35) C 0.9300(6) 0.3226(5) 0.9939(4) 0.0297(15) Uani 1 1 d . . . C(36) C 0.9238(5) 0.2831(5) 1.0696(4) 0.0293(15) Uani 1 1 d . . . C(37) C 0.8706(5) 0.3384(5) 1.1235(4) 0.0257(13) Uani 1 1 d . . . C(38) C 0.8279(5) 0.4343(4) 1.1026(3) 0.0223(13) Uani 1 1 d . . . C(39) C 0.8333(5) 0.4778(4) 1.0236(4) 0.0195(12) Uani 1 1 d . . . C(3A) C 0.7882(5) 0.5786(4) 0.9975(3) 0.0182(11) Uani 1 1 d . . . C(41) C 0.1173(6) 0.9316(5) 0.6005(4) 0.0296(15) Uani 1 1 d . . . C(42) C 0.0319(6) 0.9634(6) 0.6527(4) 0.0388(17) Uani 1 1 d . . . C(43) C 0.0532(7) 0.8730(6) 0.5214(4) 0.046(2) Uani 1 1 d . . . C(44) C 0.1697(7) 1.0249(6) 0.5701(5) 0.0446(19) Uani 1 1 d . . . C(61) C 0.2652(5) 0.5787(5) 0.7064(4) 0.0239(13) Uani 1 1 d . . . C(62) C 0.2543(6) 0.5447(5) 0.7961(4) 0.0348(16) Uani 1 1 d . . . C(63) C 0.3679(6) 0.5238(5) 0.6829(4) 0.0326(15) Uani 1 1 d . . . C(64) C 0.1557(6) 0.5458(5) 0.6423(4) 0.0353(16) Uani 1 1 d . . . C(221) C 0.4299(8) 0.6926(8) 1.2395(5) 0.065(3) Uani 1 1 d . . . C(222) C 0.4275(6) 0.8832(6) 1.1361(5) 0.0418(18) Uani 1 1 d . . . C(223) C 0.3450(6) 0.6799(7) 1.0469(5) 0.0441(18) Uani 1 1 d . . . C(321) C 0.6638(6) 0.6123(7) 0.6872(4) 0.047(2) Uani 1 1 d . . . C(322) C 0.8626(7) 0.4730(6) 0.6876(4) 0.0395(18) Uani 1 1 d . . . C(323) C 0.9060(6) 0.6956(5) 0.7307(4) 0.0323(15) Uani 1 1 d . . . H(3) H 0.3100 0.9798 0.7178 0.030 Uiso 1 1 calc R . . H(5) H 0.1404 0.7295 0.6199 0.029 Uiso 1 1 calc R . . H(12) H 0.4224 0.8793 0.9454 0.035 Uiso 1 1 calc R . . H(13) H 0.6291 0.8977 1.0236 0.034 Uiso 1 1 calc R . . H(15) H 0.8395 0.9350 0.9664 0.052 Uiso 1 1 calc R . . H(16) H 0.9077 0.9515 0.8434 0.065 Uiso 1 1 calc R . . H(17) H 0.7875 0.9387 0.7109 0.055 Uiso 1 1 calc R . . H(18) H 0.5985 0.9019 0.6955 0.042 Uiso 1 1 calc R . . H(23) H 0.6650 0.7628 1.2490 0.038 Uiso 1 1 calc R . . H(25) H 0.8690 0.7755 1.3274 0.046 Uiso 1 1 calc R . . H(26) H 1.0585 0.7445 1.3352 0.049 Uiso 1 1 calc R . . H(27) H 1.1167 0.6658 1.2205 0.039 Uiso 1 1 calc R . . H(28) H 0.9832 0.6176 1.1032 0.029 Uiso 1 1 calc R . . H(33) H 0.9201 0.4216 0.8508 0.031 Uiso 1 1 calc R . . H(35) H 0.9650 0.2852 0.9577 0.039 Uiso 1 1 calc R . . H(36) H 0.9548 0.2192 1.0858 0.038 Uiso 1 1 calc R . . H(37) H 0.8638 0.3098 1.1749 0.033 Uiso 1 1 calc R . . H(38) H 0.7953 0.4708 1.1406 0.029 Uiso 1 1 calc R . . H(22A) H 0.4818 0.7271 1.2847 0.084 Uiso 1 1 calc R . . H(22B) H 0.4455 0.6208 1.2431 0.084 Uiso 1 1 calc R . . H(22C) H 0.3523 0.7045 1.2442 0.084 Uiso 1 1 calc R . . H(22D) H 0.4430 0.9132 1.0856 0.054 Uiso 1 1 calc R . . H(22E) H 0.4785 0.9115 1.1851 0.054 Uiso 1 1 calc R . . H(22F) H 0.3495 0.8970 1.1388 0.054 Uiso 1 1 calc R . . H(22G) H 0.2711 0.6780 1.0610 0.057 Uiso 1 1 calc R . . H(22H) H 0.3699 0.6117 1.0394 0.057 Uiso 1 1 calc R . . H(22I) H 0.3396 0.7176 0.9952 0.057 Uiso 1 1 calc R . . H(32A) H 0.6387 0.6737 0.7099 0.061 Uiso 1 1 calc R . . H(32B) H 0.6156 0.5567 0.6960 0.061 Uiso 1 1 calc R . . H(32C) H 0.6591 0.6208 0.6275 0.061 Uiso 1 1 calc R . . H(32D) H 0.8598 0.4897 0.6293 0.051 Uiso 1 1 calc R . . H(32E) H 0.8128 0.4162 0.6902 0.051 Uiso 1 1 calc R . . H(32F) H 0.9398 0.4554 0.7154 0.051 Uiso 1 1 calc R . . H(32G) H 0.9854 0.6758 0.7459 0.042 Uiso 1 1 calc R . . H(32H) H 0.8925 0.7495 0.7674 0.042 Uiso 1 1 calc R . . H(32I) H 0.8878 0.7189 0.6729 0.042 Uiso 1 1 calc R . . H(42A) H 0.0714 0.9996 0.7023 0.050 Uiso 1 1 calc R . . H(42B) H -0.0041 0.9040 0.6696 0.050 Uiso 1 1 calc R . . H(42C) H -0.0255 1.0068 0.6192 0.050 Uiso 1 1 calc R . . H(43A) H -0.0010 0.9176 0.4862 0.059 Uiso 1 1 calc R . . H(43B) H 0.0133 0.8162 0.5388 0.059 Uiso 1 1 calc R . . H(43C) H 0.1073 0.8488 0.4901 0.059 Uiso 1 1 calc R . . H(44A) H 0.2092 1.0637 0.6182 0.058 Uiso 1 1 calc R . . H(44B) H 0.1102 1.0658 0.5361 0.058 Uiso 1 1 calc R . . H(44C) H 0.2231 1.0046 0.5367 0.058 Uiso 1 1 calc R . . H(62A) H 0.3230 0.5628 0.8368 0.045 Uiso 1 1 calc R . . H(62B) H 0.2436 0.4723 0.7966 0.045 Uiso 1 1 calc R . . H(62C) H 0.1896 0.5781 0.8103 0.045 Uiso 1 1 calc R . . H(63A) H 0.3770 0.5473 0.6285 0.042 Uiso 1 1 calc R . . H(63B) H 0.3542 0.4517 0.6805 0.042 Uiso 1 1 calc R . . H(63C) H 0.4365 0.5381 0.7250 0.042 Uiso 1 1 calc R . . H(64A) H 0.0901 0.5771 0.6569 0.046 Uiso 1 1 calc R . . H(64B) H 0.1482 0.4730 0.6437 0.046 Uiso 1 1 calc R . . H(64C) H 0.1606 0.5667 0.5863 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0201(5) 0.0156(5) 0.0257(5) 0.0015(5) -0.0001(4) -0.0009(5) Si(22) 0.0286(9) 0.0312(10) 0.0410(9) 0.0056(9) 0.0137(7) -0.0045(9) Si(32) 0.0237(8) 0.0257(9) 0.0215(8) -0.0022(7) 0.0056(6) -0.0006(7) O(1) 0.020(2) 0.018(2) 0.029(2) 0.0012(17) 0.0009(17) -0.0008(17) O(2) 0.027(2) 0.022(2) 0.023(2) 0.0001(18) -0.0005(17) 0.0008(16) O(3) 0.023(2) 0.021(2) 0.025(2) 0.0027(17) 0.0030(16) 0.0033(16) C(1) 0.021(3) 0.024(3) 0.022(3) 0.007(3) 0.005(2) 0.007(3) C(2) 0.023(3) 0.019(3) 0.027(3) 0.001(2) 0.006(2) 0.004(2) C(3) 0.029(3) 0.016(3) 0.025(3) -0.001(3) 0.006(3) 0.004(2) C(4) 0.026(3) 0.027(4) 0.019(3) 0.000(3) 0.003(2) 0.000(2) C(5) 0.027(3) 0.018(3) 0.021(3) -0.001(2) 0.006(2) 0.000(2) C(6) 0.020(3) 0.027(3) 0.019(3) 0.001(3) 0.005(2) 0.000(2) C(11) 0.024(3) 0.008(3) 0.034(3) 0.001(2) 0.002(2) 0.001(2) C(12) 0.034(4) 0.010(3) 0.037(3) 0.001(3) 0.012(3) -0.006(2) C(13) 0.031(3) 0.010(3) 0.032(3) 0.003(2) -0.005(3) -0.004(2) C(14) 0.026(3) 0.005(3) 0.050(4) 0.004(2) 0.002(3) 0.000(3) C(15) 0.021(3) 0.014(3) 0.079(5) -0.002(3) -0.001(3) -0.008(3) C(16) 0.032(4) 0.019(4) 0.103(7) -0.004(3) 0.024(4) -0.004(4) C(17) 0.026(4) 0.028(4) 0.079(5) 0.005(3) 0.024(4) 0.005(4) C(18) 0.034(4) 0.012(3) 0.054(4) 0.003(3) 0.014(3) 0.008(3) C(19) 0.032(3) 0.007(3) 0.038(3) 0.003(2) 0.006(3) 0.004(2) C(21) 0.028(3) 0.017(3) 0.019(3) -0.007(2) 0.004(2) 0.002(2) C(22) 0.026(3) 0.014(3) 0.032(3) 0.007(2) 0.010(2) 0.004(2) C(23) 0.044(4) 0.018(3) 0.029(3) 0.001(3) 0.015(3) -0.001(3) C(24) 0.035(4) 0.011(3) 0.024(3) -0.001(2) 0.003(2) -0.001(2) C(25) 0.049(4) 0.027(3) 0.029(3) 0.001(4) 0.004(3) -0.008(3) C(26) 0.036(4) 0.028(4) 0.040(3) -0.009(3) -0.012(3) -0.005(3) C(27) 0.026(3) 0.020(4) 0.041(4) -0.006(3) -0.001(3) 0.007(3) C(28) 0.020(3) 0.020(3) 0.028(3) -0.004(2) 0.006(2) 0.001(2) C(29) 0.027(3) 0.015(3) 0.025(3) -0.003(2) 0.008(2) 0.008(2) C(2A) 0.025(3) 0.014(3) 0.022(3) -0.002(2) 0.004(2) 0.003(2) C(31) 0.021(3) 0.015(3) 0.025(3) -0.001(2) -0.002(2) 0.001(2) C(32) 0.016(3) 0.026(4) 0.029(3) -0.002(2) 0.008(2) -0.003(2) C(33) 0.018(3) 0.028(3) 0.028(3) 0.003(3) 0.007(2) -0.002(3) C(34) 0.017(3) 0.023(3) 0.035(3) 0.000(2) 0.008(2) -0.005(3) C(35) 0.035(4) 0.028(4) 0.026(3) 0.007(3) 0.007(3) -0.004(3) C(36) 0.030(3) 0.023(3) 0.033(3) 0.010(3) 0.002(3) 0.003(3) C(37) 0.030(3) 0.021(3) 0.029(3) 0.002(3) 0.011(3) 0.007(2) C(38) 0.029(3) 0.016(3) 0.023(3) 0.002(2) 0.007(2) 0.000(2) C(39) 0.014(3) 0.015(3) 0.028(3) 0.003(2) 0.003(2) -0.006(2) C(3A) 0.017(3) 0.013(3) 0.024(3) -0.001(2) 0.004(2) 0.001(2) C(41) 0.028(3) 0.028(4) 0.031(3) 0.008(3) 0.003(3) 0.007(3) C(42) 0.033(4) 0.042(5) 0.039(4) 0.018(3) 0.003(3) 0.007(3) C(43) 0.046(4) 0.044(5) 0.036(4) 0.009(4) -0.015(3) 0.005(3) C(44) 0.047(5) 0.044(5) 0.037(4) 0.000(4) -0.003(3) 0.016(3) C(61) 0.020(3) 0.019(3) 0.030(3) -0.001(3) -0.002(2) -0.004(3) C(62) 0.038(4) 0.024(4) 0.043(4) -0.005(3) 0.010(3) 0.004(3) C(63) 0.030(4) 0.017(3) 0.048(4) 0.000(3) 0.004(3) -0.008(3) C(64) 0.028(4) 0.026(4) 0.045(4) -0.004(3) -0.006(3) -0.007(3) C(221) 0.062(6) 0.081(7) 0.064(5) 0.005(5) 0.042(5) -0.003(5) C(222) 0.029(4) 0.030(4) 0.066(5) 0.009(3) 0.010(3) -0.015(3) C(223) 0.031(4) 0.046(5) 0.057(5) -0.002(3) 0.015(3) -0.011(4) C(321) 0.037(4) 0.069(6) 0.031(4) -0.004(4) 0.000(3) 0.007(3) C(322) 0.067(5) 0.033(4) 0.022(3) -0.010(4) 0.015(3) -0.007(3) C(323) 0.037(4) 0.029(4) 0.033(3) -0.009(3) 0.011(3) -0.001(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 Ti O(2) 1.844(4) . ? Ti O(1) 1.859(4) . ? Ti O(3) 1.871(4) . ? Ti C(12) 2.323(6) . ? Ti C(13) 2.340(6) . ? Ti C(11) 2.367(6) . ? Ti C(19) 2.452(6) . ? Ti C(14) 2.453(6) . ? Si(22) C(223) 1.851(7) . ? Si(22) C(222) 1.866(8) . ? Si(22) C(22) 1.889(6) . ? Si(22) C(221) 1.895(8) . ? Si(32) C(323) 1.851(7) . ? Si(32) C(321) 1.855(7) . ? Si(32) C(322) 1.866(7) . ? Si(32) C(32) 1.891(6) . ? O(1) C(1) 1.380(7) . ? O(2) C(21) 1.362(6) . ? O(3) C(31) 1.363(7) . ? C(1) C(2) 1.387(9) . ? C(1) C(6) 1.394(8) . ? C(2) C(3) 1.382(8) . ? C(2) C(11) 1.479(8) . ? C(3) C(4) 1.394(8) . ? C(4) C(5) 1.392(9) . ? C(4) C(41) 1.553(8) . ? C(5) C(6) 1.402(8) . ? C(6) C(61) 1.529(9) . ? C(11) C(12) 1.435(9) . ? C(11) C(19) 1.442(9) . ? C(12) C(13) 1.430(9) . ? C(13) C(14) 1.407(9) . ? C(14) C(15) 1.434(9) . ? C(14) C(19) 1.433(9) . ? C(15) C(16) 1.387(12) . ? C(16) C(17) 1.397(12) . ? C(17) C(18) 1.345(10) . ? C(18) C(19) 1.402(9) . ? C(21) C(2A) 1.386(8) . ? C(21) C(22) 1.423(8) . ? C(22) C(23) 1.369(8) . ? C(23) C(24) 1.410(9) . ? C(24) C(25) 1.412(8) . ? C(24) C(29) 1.443(8) . ? C(25) C(26) 1.356(10) . ? C(26) C(27) 1.424(10) . ? C(27) C(28) 1.361(8) . ? C(28) C(29) 1.401(8) . ? C(29) C(2A) 1.445(8) . ? C(2A) C(3A) 1.509(8) . ? C(31) C(3A) 1.376(8) . ? C(31) C(32) 1.420(9) . ? C(32) C(33) 1.388(9) . ? C(33) C(34) 1.417(9) . ? C(34) C(39) 1.411(8) . ? C(34) C(35) 1.413(9) . ? C(35) C(36) 1.346(9) . ? C(36) C(37) 1.392(9) . ? C(37) C(38) 1.371(8) . ? C(38) C(39) 1.413(8) . ? C(39) C(3A) 1.455(8) . ? C(41) C(44) 1.506(10) . ? C(41) C(42) 1.520(9) . ? C(41) C(43) 1.540(9) . ? C(61) C(64) 1.538(8) . ? C(61) C(63) 1.541(9) . ? C(61) C(62) 1.548(9) . ? 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(2) Ti O(1) 99.33(18) . . ? O(2) Ti O(3) 101.18(18) . . ? O(1) Ti O(3) 113.03(18) . . ? O(2) Ti C(12) 98.8(2) . . ? O(1) Ti C(12) 95.1(2) . . ? O(3) Ti C(12) 142.0(2) . . ? O(2) Ti C(13) 97.1(2) . . ? O(1) Ti C(13) 130.1(2) . . ? O(3) Ti C(13) 109.4(2) . . ? C(12) Ti C(13) 35.7(2) . . ? O(2) Ti C(11) 130.2(2) . . ? O(1) Ti C(11) 74.68(19) . . ? O(3) Ti C(11) 127.1(2) . . ? C(12) Ti C(11) 35.6(2) . . ? C(13) Ti C(11) 59.0(2) . . ? O(2) Ti C(19) 154.1(2) . . ? O(1) Ti C(19) 94.6(2) . . ? O(3) Ti C(19) 93.2(2) . . ? C(12) Ti C(19) 58.1(2) . . ? C(13) Ti C(19) 57.6(2) . . ? C(11) Ti C(19) 34.8(2) . . ? O(2) Ti C(14) 125.8(2) . . ? O(1) Ti C(14) 128.1(2) . . ? O(3) Ti C(14) 84.7(2) . . ? C(12) Ti C(14) 57.4(2) . . ? C(13) Ti C(14) 34.0(2) . . ? C(11) Ti C(14) 57.4(2) . . ? C(19) Ti C(14) 34.0(2) . . ? C(223) Si(22) C(222) 112.3(4) . . ? C(223) Si(22) C(22) 113.6(3) . . ? C(222) Si(22) C(22) 109.1(3) . . ? C(223) Si(22) C(221) 109.3(4) . . ? C(222) Si(22) C(221) 106.0(4) . . ? C(22) Si(22) C(221) 106.1(4) . . ? C(323) Si(32) C(321) 109.5(4) . . ? C(323) Si(32) C(322) 108.8(3) . . ? C(321) Si(32) C(322) 107.3(4) . . ? C(323) Si(32) C(32) 112.0(3) . . ? C(321) Si(32) C(32) 112.0(3) . . ? C(322) Si(32) C(32) 107.0(3) . . ? C(1) O(1) Ti 128.0(4) . . ? C(21) O(2) Ti 117.2(4) . . ? C(31) O(3) Ti 126.2(4) . . ? O(1) C(1) C(2) 115.8(5) . . ? O(1) C(1) C(6) 122.4(6) . . ? C(2) C(1) C(6) 121.9(5) . . ? C(3) C(2) C(1) 121.0(5) . . ? C(3) C(2) C(11) 124.9(6) . . ? C(1) C(2) C(11) 114.1(5) . . ? C(2) C(3) C(4) 119.6(6) . . ? C(5) C(4) C(3) 117.8(5) . . ? C(5) C(4) C(41) 121.2(5) . . ? C(3) C(4) C(41) 120.8(6) . . ? C(4) C(5) C(6) 124.4(5) . . ? C(1) C(6) C(5) 115.2(6) . . ? C(1) C(6) C(61) 123.3(5) . . ? C(5) C(6) C(61) 121.4(5) . . ? C(12) C(11) C(19) 107.5(5) . . ? C(12) C(11) C(2) 123.9(6) . . ? C(19) C(11) C(2) 126.8(5) . . ? C(12) C(11) Ti 70.5(3) . . ? C(19) C(11) Ti 75.8(3) . . ? C(2) C(11) Ti 107.1(4) . . ? C(13) C(12) C(11) 108.0(6) . . ? C(13) C(12) Ti 72.8(3) . . ? C(11) C(12) Ti 73.9(3) . . ? C(14) C(13) C(12) 108.2(5) . . ? C(14) C(13) Ti 77.3(4) . . ? C(12) C(13) Ti 71.5(3) . . ? C(13) C(14) C(15) 132.0(6) . . ? C(13) C(14) C(19) 108.9(5) . . ? C(15) C(14) C(19) 119.1(6) . . ? C(13) C(14) Ti 68.6(3) . . ? C(15) C(14) Ti 123.9(4) . . ? C(19) C(14) Ti 73.0(3) . . ? C(16) C(15) C(14) 117.5(7) . . ? C(15) C(16) C(17) 122.2(7) . . ? C(18) C(17) C(16) 121.2(8) . . ? C(17) C(18) C(19) 120.0(7) . . ? C(18) C(19) C(14) 120.1(6) . . ? C(18) C(19) C(11) 132.7(6) . . ? C(14) C(19) C(11) 107.2(5) . . ? C(18) C(19) Ti 123.9(4) . . ? C(14) C(19) Ti 73.0(3) . . ? C(11) C(19) Ti 69.4(3) . . ? O(2) C(21) C(2A) 119.0(5) . . ? O(2) C(21) C(22) 117.8(5) . . ? C(2A) C(21) C(22) 123.1(5) . . ? C(23) C(22) C(21) 116.3(5) . . ? C(23) C(22) Si(22) 118.5(5) . . ? C(21) C(22) Si(22) 125.1(4) . . ? C(22) C(23) C(24) 124.5(5) . . ? C(23) C(24) C(25) 123.4(6) . . ? C(23) C(24) C(29) 118.3(5) . . ? C(25) C(24) C(29) 118.3(6) . . ? C(26) C(25) C(24) 121.9(6) . . ? C(25) C(26) C(27) 119.7(6) . . ? C(28) C(27) C(26) 119.9(6) . . ? C(27) C(28) C(29) 122.0(6) . . ? C(28) C(29) C(2A) 123.8(5) . . ? C(28) C(29) C(24) 118.2(5) . . ? C(2A) C(29) C(24) 118.0(5) . . ? C(21) C(2A) C(29) 119.2(5) . . ? C(21) C(2A) C(3A) 122.3(5) . . ? C(29) C(2A) C(3A) 118.3(5) . . ? O(3) C(31) C(3A) 120.7(5) . . ? O(3) C(31) C(32) 116.4(5) . . ? C(3A) C(31) C(32) 122.9(5) . . ? C(33) C(32) C(31) 117.9(6) . . ? C(33) C(32) Si(32) 118.9(5) . . ? C(31) C(32) Si(32) 123.3(5) . . ? C(32) C(33) C(34) 121.9(6) . . ? C(39) C(34) C(35) 119.8(6) . . ? C(39) C(34) C(33) 119.0(6) . . ? C(35) C(34) C(33) 121.1(6) . . ? C(36) C(35) C(34) 121.1(6) . . ? C(35) C(36) C(37) 119.6(6) . . ? C(38) C(37) C(36) 121.4(6) . . ? C(37) C(38) C(39) 120.3(5) . . ? C(38) C(39) C(34) 117.8(5) . . ? C(38) C(39) C(3A) 122.8(5) . . ? C(34) C(39) C(3A) 119.5(5) . . ? C(31) C(3A) C(39) 118.0(5) . . ? C(31) C(3A) C(2A) 125.2(5) . . ? C(39) C(3A) C(2A) 116.8(5) . . ? C(44) C(41) C(42) 109.6(6) . . ? C(44) C(41) C(43) 107.6(6) . . ? C(42) C(41) C(43) 109.0(6) . . ? C(44) C(41) C(4) 110.7(6) . . ? C(42) C(41) C(4) 108.2(5) . . ? C(43) C(41) C(4) 111.6(6) . . ? C(6) C(61) C(64) 112.4(5) . . ? C(6) C(61) C(63) 110.1(5) . . ? C(64) C(61) C(63) 107.9(5) . . ? C(6) C(61) C(62) 108.8(5) . . ? C(64) C(61) C(62) 108.3(6) . . ? C(63) C(61) C(62) 109.5(5) . . ? #======================================================================= #====== data_LTDMI2 _database_code_CSD 201172 _audit_creation_date 6-02-03 _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 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C51 H58 O3 Si2 Ti1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 823.10 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.0012(4) _cell_length_b 13.6234(5) _cell_length_c 16.3611(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.5417(14) _cell_angle_gamma 90.00 _cell_volume 2577.2(3) _cell_measurement_reflns_used 20741 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.06 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.243 _cell_measurement_temperature 149 _exptl_crystal_F_000 876 # 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,_ _exptl_absorpt_correction_T_min 0.5190 _exptl_absorpt_correction_T_max 0.9074 _diffrn_reflns_number 20741 _diffrn_measured_fraction_theta_max 0.9860 _diffrn_reflns_theta_full 24.1 _reflns_number_total 10232 _reflns_friedl_coverage 0.8231 _reflns_number_gt 9711 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 21 # 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 0.053 _refine_ls_wR_factor_ref 0.148 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10199 _refine_ls_number_parameters 528 _refine_ls_number_restraints 1 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.6708P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.39 _refine_diff_density_min -0.34 _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) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) # 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 0.60674(4) 0.35079(4) 0.38623(3) 0.02315(13) Uani 1 1 d . . . Si(2) Si 0.47721(7) 0.32716(6) 0.64164(6) 0.0310(2) Uani 1 1 d . . . Si(3) Si 0.81921(8) 0.18186(7) 0.24215(5) 0.0302(2) Uani 1 1 d . . . O(1) O 0.47760(17) 0.30051(16) 0.30699(13) 0.0279(4) Uani 1 1 d . . . O(2) O 0.58246(17) 0.28714(16) 0.48069(12) 0.0268(4) Uani 1 1 d . . . O(3) O 0.74912(17) 0.29968(16) 0.38148(12) 0.0270(4) Uani 1 1 d . . . C(1) C 0.3855(2) 0.3521(2) 0.25795(16) 0.0255(5) Uani 1 1 d . . . C(2) C 0.3953(2) 0.4543(2) 0.26434(18) 0.0260(6) Uani 1 1 d . . . C(3) C 0.3111(3) 0.5149(3) 0.21345(19) 0.0301(6) Uani 1 1 d . . . C(4) C 0.2157(2) 0.4742(2) 0.15673(18) 0.0288(6) Uani 1 1 d . . . C(5) C 0.2054(2) 0.3722(2) 0.15470(17) 0.0284(6) Uani 1 1 d . . . C(6) C 0.2874(2) 0.3077(2) 0.20422(17) 0.0263(6) Uani 1 1 d . . . C(11) C 0.5078(2) 0.4881(2) 0.32240(18) 0.0261(6) Uani 1 1 d . . . C(12) C 0.5367(3) 0.5034(2) 0.41096(19) 0.0281(6) Uani 1 1 d . . . C(13) C 0.6601(3) 0.5093(2) 0.44130(19) 0.0270(6) Uani 1 1 d . . . C(14) C 0.7051(3) 0.5100(2) 0.3688(2) 0.0289(6) Uani 1 1 d . . . C(15) C 0.8183(3) 0.5254(3) 0.3606(2) 0.0370(7) Uani 1 1 d . . . C(16) C 0.8332(3) 0.5277(3) 0.2809(3) 0.0418(8) Uani 1 1 d . . . C(17) C 0.7405(3) 0.5117(3) 0.2078(2) 0.0429(8) Uani 1 1 d . . . C(18) C 0.6315(3) 0.4930(3) 0.2137(2) 0.0353(7) Uani 1 1 d . . . C(19) C 0.6119(3) 0.4951(2) 0.29572(19) 0.0274(6) Uani 1 1 d . . . C(21) C 0.6643(2) 0.2869(2) 0.55707(18) 0.0254(6) Uani 1 1 d . . . C(22) C 0.6303(3) 0.3233(2) 0.62911(18) 0.0279(6) Uani 1 1 d . . . C(23) C 0.7181(3) 0.3398(3) 0.70173(19) 0.0321(6) Uani 1 1 d . . . C(24) C 0.8361(3) 0.3214(2) 0.70652(18) 0.0301(6) Uani 1 1 d . . . C(25) C 0.9258(3) 0.3453(3) 0.7809(2) 0.0395(7) Uani 1 1 d . . . C(26) C 1.0376(3) 0.3231(3) 0.7873(2) 0.0407(8) Uani 1 1 d . . . C(27) C 1.0671(3) 0.2756(3) 0.7185(2) 0.0368(7) Uani 1 1 d . . . C(28) C 0.9830(3) 0.2517(2) 0.6462(2) 0.0296(6) Uani 1 1 d . . . C(29) C 0.8646(2) 0.2745(2) 0.63764(18) 0.0262(6) Uani 1 1 d . . . C(2A) C 0.7756(2) 0.2526(2) 0.56240(18) 0.0248(6) Uani 1 1 d . . . C(31) C 0.7917(2) 0.2109(2) 0.41247(18) 0.0244(6) Uani 1 1 d . . . C(32) C 0.8283(3) 0.1472(2) 0.35540(19) 0.0276(6) Uani 1 1 d . . . C(33) C 0.8723(3) 0.0564(2) 0.3850(2) 0.0311(6) Uani 1 1 d . . . C(34) C 0.8747(2) 0.0230(2) 0.46699(19) 0.0278(6) Uani 1 1 d . . . C(35) C 0.9110(3) -0.0730(3) 0.4932(2) 0.0356(7) Uani 1 1 d . . . C(36) C 0.9095(3) -0.1081(3) 0.5716(2) 0.0356(7) Uani 1 1 d . . . C(37) C 0.8714(3) -0.0462(3) 0.6273(2) 0.0339(7) Uani 1 1 d . . . C(38) C 0.8383(2) 0.0486(2) 0.60510(19) 0.0281(6) Uani 1 1 d . . . C(39) C 0.8394(2) 0.0872(2) 0.52444(18) 0.0254(6) Uani 1 1 d . . . C(3A) C 0.8012(2) 0.1856(2) 0.49740(17) 0.0249(6) Uani 1 1 d . . . C(41) C 0.1213(3) 0.5380(3) 0.0992(2) 0.0352(7) Uani 1 1 d . . . C(42) C 0.1712(4) 0.6339(4) 0.0762(3) 0.0578(11) Uani 1 1 d . . . C(43) C 0.0655(4) 0.4855(3) 0.0152(2) 0.0531(10) Uani 1 1 d . . . C(44) C 0.0287(4) 0.5617(4) 0.1439(3) 0.0580(12) Uani 1 1 d . . . C(61) C 0.2699(3) 0.1963(2) 0.2001(2) 0.0318(7) Uani 1 1 d . . . C(62) C 0.1591(3) 0.1658(3) 0.1363(2) 0.0410(8) Uani 1 1 d . . . C(63) C 0.2651(4) 0.1594(3) 0.2883(2) 0.0445(9) Uani 1 1 d . . . C(64) C 0.3715(3) 0.1458(3) 0.1755(3) 0.0465(9) Uani 1 1 d . . . C(121) C 0.4543(3) 0.5113(3) 0.4643(2) 0.0346(7) Uani 1 1 d . . . C(131) C 0.7309(3) 0.5260(3) 0.5307(2) 0.0367(7) Uani 1 1 d . . . C(221) C 0.4801(3) 0.2441(3) 0.7336(3) 0.0464(9) Uani 1 1 d . . . C(222) C 0.4395(4) 0.4525(3) 0.6733(3) 0.0460(9) Uani 1 1 d . . . C(223) C 0.3686(3) 0.2772(3) 0.5486(3) 0.0437(8) Uani 1 1 d . . . C(321) C 0.8675(4) 0.0752(3) 0.1902(2) 0.0484(9) Uani 1 1 d . . . C(322) C 0.9132(3) 0.2888(3) 0.2352(2) 0.0398(8) Uani 1 1 d . . . C(323) C 0.6671(3) 0.2070(4) 0.1812(2) 0.0527(11) Uani 1 1 d . . . H(3) H 0.3192 0.5828 0.2177 0.036 Uiso 1 1 calc R . . H(5) H 0.1398 0.3451 0.1180 0.034 Uiso 1 1 calc R . . H(15) H 0.8806 0.5336 0.4082 0.044 Uiso 1 1 calc R . . H(16) H 0.9065 0.5402 0.2744 0.050 Uiso 1 1 calc R . . H(17) H 0.7544 0.5140 0.1546 0.052 Uiso 1 1 calc R . . H(18) H 0.5718 0.4793 0.1656 0.042 Uiso 1 1 calc R . . H(23) H 0.6993 0.3639 0.7495 0.039 Uiso 1 1 calc R . . H(25) H 0.9069 0.3769 0.8258 0.047 Uiso 1 1 calc R . . H(26) H 1.0947 0.3387 0.8364 0.049 Uiso 1 1 calc R . . H(27) H 1.1440 0.2607 0.7225 0.044 Uiso 1 1 calc R . . H(28) H 1.0037 0.2201 0.6020 0.036 Uiso 1 1 calc R . . H(33) H 0.9012 0.0159 0.3497 0.037 Uiso 1 1 calc R . . H(35) H 0.9367 -0.1137 0.4564 0.043 Uiso 1 1 calc R . . H(36) H 0.9333 -0.1719 0.5876 0.043 Uiso 1 1 calc R . . H(37) H 0.8685 -0.0698 0.6800 0.041 Uiso 1 1 calc R . . H(38) H 0.8148 0.0885 0.6435 0.034 Uiso 1 1 calc R . . H(12A) H 0.4372 0.5791 0.4710 0.052 Uiso 1 1 calc R . . H(12B) H 0.4884 0.4828 0.5189 0.052 Uiso 1 1 calc R . . H(12C) H 0.3842 0.4770 0.4373 0.052 Uiso 1 1 calc R . . H(13A) H 0.7614 0.5915 0.5360 0.055 Uiso 1 1 calc R . . H(13B) H 0.7935 0.4798 0.5445 0.055 Uiso 1 1 calc R . . H(13C) H 0.6831 0.5175 0.5687 0.055 Uiso 1 1 calc R . . H(22A) H 0.4028 0.2352 0.7386 0.070 Uiso 1 1 calc R . . H(22B) H 0.5272 0.2728 0.7848 0.070 Uiso 1 1 calc R . . H(22C) H 0.5117 0.1816 0.7245 0.070 Uiso 1 1 calc R . . H(22D) H 0.4155 0.4932 0.6238 0.069 Uiso 1 1 calc R . . H(22E) H 0.5060 0.4811 0.7122 0.069 Uiso 1 1 calc R . . H(22F) H 0.3777 0.4474 0.7001 0.069 Uiso 1 1 calc R . . H(22G) H 0.3952 0.2154 0.5327 0.066 Uiso 1 1 calc R . . H(22H) H 0.3576 0.3224 0.5021 0.066 Uiso 1 1 calc R . . H(22I) H 0.2966 0.2678 0.5626 0.066 Uiso 1 1 calc R . . H(32A) H 0.8605 0.0904 0.1317 0.073 Uiso 1 1 calc R . . H(32B) H 0.8202 0.0193 0.1935 0.073 Uiso 1 1 calc R . . H(32C) H 0.9468 0.0607 0.2183 0.073 Uiso 1 1 calc R . . H(32D) H 0.9917 0.2742 0.2653 0.060 Uiso 1 1 calc R . . H(32E) H 0.8874 0.3454 0.2599 0.060 Uiso 1 1 calc R . . H(32F) H 0.9089 0.3019 0.1768 0.060 Uiso 1 1 calc R . . H(32G) H 0.6366 0.2597 0.2077 0.079 Uiso 1 1 calc R . . H(32H) H 0.6211 0.1491 0.1803 0.079 Uiso 1 1 calc R . . H(32I) H 0.6651 0.2252 0.1241 0.079 Uiso 1 1 calc R . . H(42A) H 0.1130 0.6679 0.0339 0.087 Uiso 1 1 calc R . . H(42B) H 0.2361 0.6199 0.0543 0.087 Uiso 1 1 calc R . . H(42C) H 0.1957 0.6743 0.1259 0.087 Uiso 1 1 calc R . . H(43A) H 0.0246 0.4285 0.0261 0.080 Uiso 1 1 calc R . . H(43B) H 0.1245 0.4660 -0.0111 0.080 Uiso 1 1 calc R . . H(43C) H 0.0124 0.5293 -0.0219 0.080 Uiso 1 1 calc R . . H(44A) H -0.0336 0.5963 0.1057 0.087 Uiso 1 1 calc R . . H(44B) H 0.0612 0.6020 0.1926 0.087 Uiso 1 1 calc R . . H(44C) H -0.0001 0.5019 0.1616 0.087 Uiso 1 1 calc R . . H(62A) H 0.0945 0.1961 0.1504 0.062 Uiso 1 1 calc R . . H(62B) H 0.1513 0.0957 0.1373 0.062 Uiso 1 1 calc R . . H(62C) H 0.1614 0.1862 0.0806 0.062 Uiso 1 1 calc R . . H(63A) H 0.2040 0.1926 0.3049 0.067 Uiso 1 1 calc R . . H(63B) H 0.3375 0.1727 0.3290 0.067 Uiso 1 1 calc R . . H(63C) H 0.2507 0.0900 0.2859 0.067 Uiso 1 1 calc R . . H(64A) H 0.3550 0.0771 0.1660 0.070 Uiso 1 1 calc R . . H(64B) H 0.4410 0.1538 0.2205 0.070 Uiso 1 1 calc R . . H(64C) H 0.3816 0.1750 0.1245 0.070 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 0.0197(2) 0.0231(3) 0.0242(2) 0.00309(19) 0.00167(17) -0.00121(19) Si(2) 0.0291(4) 0.0274(5) 0.0395(4) 0.0028(3) 0.0145(3) -0.0026(3) Si(3) 0.0312(4) 0.0350(5) 0.0245(4) 0.0005(3) 0.0078(3) -0.0030(3) O(1) 0.0245(10) 0.0256(11) 0.0289(10) 0.0027(8) -0.0010(8) 0.0016(8) O(2) 0.0232(10) 0.0293(11) 0.0261(10) 0.0060(8) 0.0031(8) -0.0010(8) O(3) 0.0248(10) 0.0286(11) 0.0263(10) 0.0046(8) 0.0049(8) 0.0019(8) C(1) 0.0225(12) 0.0291(15) 0.0229(12) 0.0045(12) 0.0025(10) 0.0049(12) C(2) 0.0206(13) 0.0282(16) 0.0270(13) 0.0006(11) 0.0025(11) 0.0021(11) C(3) 0.0234(14) 0.0338(17) 0.0312(15) 0.0031(12) 0.0039(12) 0.0087(13) C(4) 0.0219(14) 0.0353(17) 0.0267(14) 0.0023(11) 0.0021(11) 0.0082(12) C(5) 0.0233(13) 0.0361(18) 0.0227(13) -0.0029(11) 0.0007(10) 0.0029(12) C(6) 0.0223(13) 0.0304(16) 0.0253(13) -0.0001(11) 0.0049(11) 0.0017(11) C(11) 0.0201(13) 0.0258(15) 0.0289(14) 0.0032(11) 0.0008(11) 0.0040(11) C(12) 0.0255(14) 0.0220(15) 0.0341(15) 0.0029(11) 0.0035(12) -0.0001(12) C(13) 0.0279(14) 0.0189(14) 0.0314(14) 0.0023(11) 0.0029(12) -0.0019(11) C(14) 0.0244(14) 0.0219(15) 0.0375(16) 0.0004(11) 0.0035(12) -0.0020(12) C(15) 0.0237(15) 0.0273(17) 0.057(2) -0.0011(12) 0.0059(14) -0.0016(15) C(16) 0.0301(17) 0.0359(19) 0.064(2) -0.0015(14) 0.0210(16) -0.0012(17) C(17) 0.047(2) 0.042(2) 0.0450(19) 0.0013(16) 0.0211(16) 0.0003(16) C(18) 0.0357(17) 0.0338(18) 0.0363(16) 0.0028(13) 0.0097(14) 0.0011(13) C(19) 0.0256(14) 0.0220(15) 0.0332(15) 0.0023(11) 0.0056(12) 0.0011(11) C(21) 0.0249(13) 0.0230(14) 0.0271(13) 0.0007(11) 0.0049(11) -0.0018(11) C(22) 0.0304(14) 0.0230(15) 0.0316(14) 0.0007(11) 0.0107(12) -0.0028(11) C(23) 0.0370(15) 0.0308(17) 0.0300(14) -0.0002(13) 0.0117(12) -0.0090(13) C(24) 0.0306(15) 0.0293(16) 0.0281(14) -0.0035(12) 0.0038(12) -0.0028(12) C(25) 0.0460(18) 0.0380(19) 0.0295(14) -0.0074(16) 0.0015(13) -0.0078(14) C(26) 0.0367(17) 0.041(2) 0.0354(16) -0.0125(14) -0.0062(13) -0.0009(14) C(27) 0.0232(14) 0.0342(18) 0.0462(18) -0.0052(13) -0.0022(13) 0.0022(14) C(28) 0.0264(15) 0.0276(16) 0.0312(15) -0.0004(11) 0.0015(12) 0.0033(12) C(29) 0.0252(14) 0.0239(15) 0.0275(14) -0.0014(11) 0.0035(11) -0.0003(11) C(2A) 0.0256(14) 0.0225(14) 0.0255(13) 0.0027(11) 0.0052(11) 0.0005(11) C(31) 0.0175(12) 0.0264(15) 0.0277(13) 0.0010(10) 0.0035(10) -0.0024(11) C(32) 0.0270(15) 0.0270(16) 0.0281(14) 0.0011(12) 0.0063(12) -0.0021(11) C(33) 0.0317(16) 0.0287(16) 0.0335(15) 0.0022(12) 0.0100(13) -0.0059(12) C(34) 0.0254(14) 0.0259(15) 0.0316(14) 0.0027(11) 0.0064(11) -0.0028(12) C(35) 0.0354(17) 0.0285(17) 0.0408(17) 0.0069(13) 0.0066(14) -0.0073(13) C(36) 0.0399(18) 0.0261(16) 0.0364(16) 0.0054(13) 0.0024(13) 0.0046(13) C(37) 0.0364(17) 0.0295(17) 0.0330(15) 0.0008(13) 0.0047(13) 0.0035(13) C(38) 0.0251(14) 0.0260(16) 0.0333(15) -0.0002(11) 0.0079(12) -0.0006(12) C(39) 0.0203(13) 0.0263(15) 0.0271(14) 0.0027(10) 0.0023(11) -0.0018(11) C(3A) 0.0198(13) 0.0264(15) 0.0276(13) 0.0024(11) 0.0045(10) -0.0013(12) C(41) 0.0267(15) 0.042(2) 0.0328(15) 0.0053(13) 0.0011(12) 0.0109(14) C(42) 0.050(2) 0.053(3) 0.060(3) -0.0025(19) -0.0039(19) 0.028(2) C(43) 0.050(2) 0.057(3) 0.039(2) 0.0048(19) -0.0122(16) 0.0088(17) C(44) 0.047(2) 0.080(3) 0.047(2) 0.029(2) 0.0122(18) 0.020(2) C(61) 0.0274(15) 0.0302(17) 0.0342(15) -0.0008(12) 0.0023(12) -0.0041(13) C(62) 0.0362(18) 0.037(2) 0.0421(18) -0.0030(14) -0.0031(14) -0.0059(15) C(63) 0.053(2) 0.035(2) 0.0384(18) -0.0148(16) -0.0011(15) 0.0087(14) C(64) 0.0373(18) 0.037(2) 0.060(2) -0.0002(15) 0.0037(17) -0.0160(17) C(121) 0.0356(17) 0.0308(17) 0.0380(16) 0.0082(13) 0.0111(13) 0.0002(13) C(131) 0.0403(18) 0.0284(17) 0.0340(16) 0.0009(14) -0.0027(13) -0.0004(13) C(221) 0.045(2) 0.043(2) 0.057(2) 0.0035(16) 0.0248(18) 0.0081(17) C(222) 0.050(2) 0.039(2) 0.056(2) 0.0094(16) 0.0265(18) -0.0060(17) C(223) 0.0296(17) 0.040(2) 0.060(2) -0.0014(14) 0.0097(16) -0.0044(17) C(321) 0.070(3) 0.042(2) 0.0388(18) 0.0013(19) 0.0251(19) -0.0065(16) C(322) 0.0423(19) 0.041(2) 0.0394(17) -0.0020(15) 0.0167(15) -0.0029(15) C(323) 0.0375(19) 0.080(3) 0.0359(18) 0.0033(19) 0.0021(15) 0.0014(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(2) 1.862(2) . ? Ti O(1) 1.864(2) . ? Ti O(3) 1.866(2) . ? Ti C(11) 2.310(3) . ? Ti C(12) 2.318(3) . ? Ti C(13) 2.361(3) . ? Ti C(19) 2.472(3) . ? Ti C(14) 2.522(3) . ? Si(2) C(223) 1.849(4) . ? Si(2) C(222) 1.875(4) . ? Si(2) C(221) 1.876(4) . ? Si(2) C(22) 1.903(3) . ? Si(3) C(321) 1.853(4) . ? Si(3) C(323) 1.863(4) . ? Si(3) C(322) 1.865(4) . ? Si(3) C(32) 1.887(3) . ? O(1) C(1) 1.373(3) . ? O(2) C(21) 1.367(4) . ? O(3) C(31) 1.357(4) . ? C(1) C(2) 1.399(5) . ? C(1) C(6) 1.404(4) . ? C(2) C(3) 1.395(4) . ? C(2) C(11) 1.500(4) . ? C(3) C(4) 1.382(4) . ? C(4) C(5) 1.395(5) . ? C(4) C(41) 1.534(4) . ? C(5) C(6) 1.403(4) . ? C(6) C(61) 1.531(5) . ? C(11) C(12) 1.412(4) . ? C(11) C(19) 1.433(4) . ? C(12) C(13) 1.432(4) . ? C(12) C(121) 1.487(4) . ? C(13) C(14) 1.430(4) . ? C(13) C(131) 1.499(4) . ? C(14) C(19) 1.415(4) . ? C(14) C(15) 1.416(4) . ? C(15) C(16) 1.363(5) . ? C(16) C(17) 1.415(6) . ? C(17) C(18) 1.361(5) . ? C(18) C(19) 1.424(4) . ? C(21) C(2A) 1.395(4) . ? C(21) C(22) 1.435(4) . ? C(22) C(23) 1.379(4) . ? C(23) C(24) 1.419(4) . ? C(24) C(29) 1.415(4) . ? C(24) C(25) 1.430(4) . ? C(25) C(26) 1.351(5) . ? C(26) C(27) 1.424(5) . ? C(27) C(28) 1.373(5) . ? C(28) C(29) 1.424(4) . ? C(29) C(2A) 1.428(4) . ? C(2A) C(3A) 1.495(4) . ? C(31) C(3A) 1.406(4) . ? C(31) C(32) 1.428(4) . ? C(32) C(33) 1.380(4) . ? C(33) C(34) 1.410(4) . ? C(34) C(35) 1.409(5) . ? C(34) C(39) 1.428(4) . ? C(35) C(36) 1.375(5) . ? C(36) C(37) 1.405(5) . ? C(37) C(38) 1.371(5) . ? C(38) C(39) 1.424(4) . ? C(39) C(3A) 1.448(4) . ? C(41) C(44) 1.520(5) . ? C(41) C(42) 1.526(6) . ? C(41) C(43) 1.534(5) . ? C(61) C(62) 1.512(4) . ? C(61) C(63) 1.544(5) . ? C(61) C(64) 1.546(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(2) Ti O(1) 96.91(9) . . ? O(2) Ti O(3) 102.09(9) . . ? O(1) Ti O(3) 115.72(9) . . ? O(2) Ti C(11) 125.21(10) . . ? O(1) Ti C(11) 75.65(10) . . ? O(3) Ti C(11) 130.47(10) . . ? O(2) Ti C(12) 97.35(10) . . ? O(1) Ti C(12) 100.26(10) . . ? O(3) Ti C(12) 136.12(10) . . ? C(11) Ti C(12) 35.53(11) . . ? O(2) Ti C(13) 101.29(10) . . ? O(1) Ti C(13) 133.73(10) . . ? O(3) Ti C(13) 101.51(10) . . ? C(11) Ti C(13) 59.07(11) . . ? C(12) Ti C(13) 35.63(10) . . ? O(2) Ti C(19) 154.45(10) . . ? O(1) Ti C(19) 91.45(10) . . ? O(3) Ti C(19) 95.83(9) . . ? C(11) Ti C(19) 34.67(10) . . ? C(12) Ti C(19) 57.31(10) . . ? C(13) Ti C(19) 56.88(10) . . ? O(2) Ti C(14) 132.58(10) . . ? O(1) Ti C(14) 124.36(10) . . ? O(3) Ti C(14) 81.64(10) . . ? C(11) Ti C(14) 56.76(10) . . ? C(12) Ti C(14) 56.71(10) . . ? C(13) Ti C(14) 33.85(10) . . ? C(19) Ti C(14) 32.91(10) . . ? C(223) Si(2) C(222) 113.21(19) . . ? C(223) Si(2) C(221) 107.2(2) . . ? C(222) Si(2) C(221) 106.37(19) . . ? C(223) Si(2) C(22) 112.89(15) . . ? C(222) Si(2) C(22) 111.51(16) . . ? C(221) Si(2) C(22) 105.01(15) . . ? C(321) Si(3) C(323) 106.3(2) . . ? C(321) Si(3) C(322) 108.42(18) . . ? C(323) Si(3) C(322) 110.2(2) . . ? C(321) Si(3) C(32) 108.14(16) . . ? C(323) Si(3) C(32) 111.26(16) . . ? C(322) Si(3) C(32) 112.26(15) . . ? C(1) O(1) Ti 127.4(2) . . ? C(21) O(2) Ti 121.73(18) . . ? C(31) O(3) Ti 125.03(17) . . ? O(1) C(1) C(2) 115.3(3) . . ? O(1) C(1) C(6) 123.6(3) . . ? C(2) C(1) C(6) 121.0(3) . . ? C(3) C(2) C(1) 120.8(3) . . ? C(3) C(2) C(11) 125.6(3) . . ? C(1) C(2) C(11) 113.3(2) . . ? C(4) C(3) C(2) 120.0(3) . . ? C(3) C(4) C(5) 117.9(3) . . ? C(3) C(4) C(41) 121.8(3) . . ? C(5) C(4) C(41) 120.2(3) . . ? C(4) C(5) C(6) 124.5(3) . . ? C(5) C(6) C(1) 115.6(3) . . ? C(5) C(6) C(61) 121.9(3) . . ? C(1) C(6) C(61) 122.5(3) . . ? C(12) C(11) C(19) 107.9(3) . . ? C(12) C(11) C(2) 128.8(3) . . ? C(19) C(11) C(2) 122.5(3) . . ? C(12) C(11) Ti 72.57(17) . . ? C(19) C(11) Ti 78.88(17) . . ? C(2) C(11) Ti 107.7(2) . . ? C(11) C(12) C(13) 108.1(3) . . ? C(11) C(12) C(121) 126.4(3) . . ? C(13) C(12) C(121) 125.5(3) . . ? C(11) C(12) Ti 71.90(17) . . ? C(13) C(12) Ti 73.80(16) . . ? C(121) C(12) Ti 119.7(2) . . ? C(14) C(13) C(12) 107.4(3) . . ? C(14) C(13) C(131) 124.5(3) . . ? C(12) C(13) C(131) 127.6(3) . . ? C(14) C(13) Ti 79.26(18) . . ? C(12) C(13) Ti 70.57(17) . . ? C(131) C(13) Ti 122.4(2) . . ? C(19) C(14) C(15) 120.2(3) . . ? C(19) C(14) C(13) 108.1(3) . . ? C(15) C(14) C(13) 131.7(3) . . ? C(19) C(14) Ti 71.62(17) . . ? C(15) C(14) Ti 128.9(2) . . ? C(13) C(14) Ti 66.89(17) . . ? C(16) C(15) C(14) 117.9(3) . . ? C(15) C(16) C(17) 122.0(3) . . ? C(18) C(17) C(16) 121.5(3) . . ? C(17) C(18) C(19) 117.8(3) . . ? C(14) C(19) C(18) 120.4(3) . . ? C(14) C(19) C(11) 108.0(3) . . ? C(18) C(19) C(11) 131.6(3) . . ? C(14) C(19) Ti 75.47(18) . . ? C(18) C(19) Ti 125.8(2) . . ? C(11) C(19) Ti 66.45(16) . . ? O(2) C(21) C(2A) 120.0(2) . . ? O(2) C(21) C(22) 117.2(2) . . ? C(2A) C(21) C(22) 122.9(3) . . ? C(23) C(22) C(21) 116.3(3) . . ? C(23) C(22) Si(2) 116.1(2) . . ? C(21) C(22) Si(2) 126.4(2) . . ? C(22) C(23) C(24) 122.7(3) . . ? C(29) C(24) C(23) 119.1(3) . . ? C(29) C(24) C(25) 119.5(3) . . ? C(23) C(24) C(25) 121.3(3) . . ? C(26) C(25) C(24) 121.4(3) . . ? C(25) C(26) C(27) 119.5(3) . . ? C(28) C(27) C(26) 120.5(3) . . ? C(27) C(28) C(29) 121.1(3) . . ? C(24) C(29) C(28) 117.9(3) . . ? C(24) C(29) C(2A) 119.7(3) . . ? C(28) C(29) C(2A) 122.4(3) . . ? C(21) C(2A) C(29) 117.8(3) . . ? C(21) C(2A) C(3A) 122.4(3) . . ? C(29) C(2A) C(3A) 119.5(2) . . ? O(3) C(31) C(3A) 120.7(2) . . ? O(3) C(31) C(32) 116.6(2) . . ? C(3A) C(31) C(32) 122.7(3) . . ? C(33) C(32) C(31) 118.1(3) . . ? C(33) C(32) Si(3) 119.0(2) . . ? C(31) C(32) Si(3) 122.9(2) . . ? C(32) C(33) C(34) 122.1(3) . . ? C(35) C(34) C(33) 121.0(3) . . ? C(35) C(34) C(39) 119.3(3) . . ? C(33) C(34) C(39) 119.7(3) . . ? C(36) C(35) C(34) 121.8(3) . . ? C(35) C(36) C(37) 118.9(3) . . ? C(38) C(37) C(36) 121.1(3) . . ? C(37) C(38) C(39) 121.2(3) . . ? C(38) C(39) C(34) 117.6(3) . . ? C(38) C(39) C(3A) 122.9(3) . . ? C(34) C(39) C(3A) 119.4(3) . . ? C(31) C(3A) C(39) 117.6(3) . . ? C(31) C(3A) C(2A) 125.1(3) . . ? C(39) C(3A) C(2A) 117.2(2) . . ? C(44) C(41) C(42) 108.8(4) . . ? C(44) C(41) C(43) 109.2(3) . . ? C(42) C(41) C(43) 106.5(3) . . ? C(44) C(41) C(4) 109.9(3) . . ? C(42) C(41) C(4) 111.2(3) . . ? C(43) C(41) C(4) 111.1(3) . . ? C(62) C(61) C(6) 112.8(3) . . ? C(62) C(61) C(63) 108.1(3) . . ? C(6) C(61) C(63) 108.7(3) . . ? C(62) C(61) C(64) 107.8(3) . . ? C(6) C(61) C(64) 110.1(3) . . ? C(63) C(61) C(64) 109.2(3) . . ? #======================================================================= #====== data_LTZRBN _database_code_CSD 201174 _audit_creation_date 6-02-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C68 H86 O6 Si2 Zr1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 1146.83 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.5231(3) _cell_length_b 19.2231(4) _cell_length_c 25.9127(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6238.0(4) _cell_measurement_reflns_used 40505 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.257 _cell_measurement_temperature 150 _exptl_crystal_F_000 2440 # 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,_ _exptl_absorpt_correction_T_min 0.4796 _exptl_absorpt_correction_T_max 0.9684 _diffrn_reflns_number 40505 _reflns_number_total 12567 _reflns_friedl_coverage 0.8976 _reflns_number_gt 12110 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.076 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_max 32 # 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 0.063 _refine_ls_wR_factor_ref 0.136 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12553 _refine_ls_number_parameters 707 _refine_ls_number_restraints 3 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0423P)^2^+9.6460P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.031 _refine_diff_density_max 0.85 _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) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) # 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 Zr Zr 0.96636(3) 0.95858(2) 0.781879(16) 0.02525(10) Uani 1 1 d . . . Si(22) Si 0.78483(11) 0.81431(7) 0.65230(5) 0.0337(3) Uani 1 1 d . . . Si(32) Si 0.83739(12) 1.08749(8) 0.93196(5) 0.0398(3) Uani 1 1 d . . . O(1) O 1.0910(2) 0.90752(15) 0.74310(12) 0.0282(7) Uani 1 1 d . . . O(2) O 0.8424(2) 0.92489(15) 0.73891(12) 0.0286(7) Uani 1 1 d . . . O(3) O 0.8706(2) 0.97179(15) 0.84742(11) 0.0266(6) Uani 1 1 d . . . O(4) O 1.0987(2) 0.95943(19) 0.84819(11) 0.0342(7) Uani 1 1 d . . . O(5) O 0.9534(3) 0.84585(15) 0.81703(12) 0.0323(7) Uani 1 1 d . . . O(9) O 0.6409(8) 0.7365(5) 0.0531(4) 0.169(4) Uani 1 1 d . . . C(1) C 1.1631(3) 0.9344(2) 0.70916(17) 0.0273(9) Uani 1 1 d . . . C(2) C 1.1497(4) 1.0042(2) 0.69519(17) 0.0285(9) Uani 1 1 d . . . C(3) C 1.2168(3) 1.0363(3) 0.65914(17) 0.0329(9) Uani 1 1 d . . . C(4) C 1.2987(4) 1.0002(2) 0.63594(18) 0.0326(10) Uani 1 1 d . . . C(5) C 1.3145(4) 0.9309(3) 0.65271(19) 0.0340(10) Uani 1 1 d . . . C(6) C 1.2506(4) 0.8962(2) 0.68888(18) 0.0287(10) Uani 1 1 d . . . C(11) C 1.0603(3) 1.0410(2) 0.72073(17) 0.0281(8) Uani 1 1 d . . . C(12) C 1.0617(3) 1.0725(2) 0.77027(17) 0.0294(10) Uani 1 1 d . . . C(13) C 0.9572(4) 1.09180(18) 0.78408(19) 0.0297(9) Uani 1 1 d . . . C(14) C 0.8903(4) 1.0793(2) 0.74105(18) 0.0298(9) Uani 1 1 d . . . C(15) C 0.7800(4) 1.0924(2) 0.7321(2) 0.0407(12) Uani 1 1 d . . . C(16) C 0.7390(4) 1.0766(3) 0.6849(2) 0.0503(14) Uani 1 1 d . . . C(17) C 0.8027(4) 1.0459(3) 0.6456(2) 0.0496(13) Uani 1 1 d . . . C(18) C 0.9074(4) 1.0303(2) 0.65334(19) 0.0377(11) Uani 1 1 d . . . C(19) C 0.9524(3) 1.0478(2) 0.70191(16) 0.0281(9) Uani 1 1 d . . . C(21) C 0.7603(3) 0.8826(2) 0.75262(17) 0.0252(9) Uani 1 1 d . . . C(22) C 0.7422(3) 0.8213(2) 0.72184(19) 0.0291(9) Uani 1 1 d . . . C(23) C 0.6683(4) 0.7739(2) 0.74053(18) 0.0309(10) Uani 1 1 d . . . C(24) C 0.6128(3) 0.7824(2) 0.78721(19) 0.0293(9) Uani 1 1 d . . . C(25) C 0.5447(4) 0.7308(2) 0.80773(19) 0.0377(11) Uani 1 1 d . . . C(26) C 0.4896(4) 0.7424(3) 0.8530(2) 0.0381(11) Uani 1 1 d . . . C(27) C 0.5003(4) 0.8048(3) 0.8789(2) 0.0367(11) Uani 1 1 d . . . C(28) C 0.5648(4) 0.8569(2) 0.86003(19) 0.0334(10) Uani 1 1 d . . . C(29) C 0.6241(3) 0.8472(2) 0.81402(18) 0.0281(9) Uani 1 1 d . . . C(2A) C 0.6961(3) 0.8994(2) 0.79428(16) 0.0258(9) Uani 1 1 d . . . C(31) C 0.7721(3) 1.0012(2) 0.84491(17) 0.0268(9) Uani 1 1 d . . . C(32) C 0.7544(4) 1.0635(2) 0.87450(18) 0.0303(10) Uani 1 1 d . . . C(33) C 0.6586(4) 1.0989(2) 0.86632(19) 0.0349(11) Uani 1 1 d . . . C(34) C 0.5780(4) 1.0742(2) 0.83136(19) 0.0293(10) Uani 1 1 d . . . C(35) C 0.4832(4) 1.1121(2) 0.8228(2) 0.0381(11) Uani 1 1 d . . . C(36) C 0.4067(4) 1.0872(2) 0.7905(2) 0.0392(12) Uani 1 1 d . . . C(37) C 0.4226(4) 1.0229(2) 0.76455(19) 0.0357(11) Uani 1 1 d . . . C(38) C 0.5130(3) 0.9854(2) 0.77314(18) 0.0333(10) Uani 1 1 d . . . C(39) C 0.5952(3) 1.0088(2) 0.80705(18) 0.0293(9) Uani 1 1 d . . . C(3A) C 0.6913(3) 0.9706(2) 0.81618(17) 0.0270(9) Uani 1 1 d . . . C(41) C 1.3769(4) 1.0313(3) 0.59648(18) 0.0370(11) Uani 1 1 d . . . C(42) C 1.4861(4) 1.0421(3) 0.6224(2) 0.0482(12) Uani 1 1 d . . . C(43) C 1.3376(5) 1.1020(3) 0.5772(2) 0.0475(13) Uani 1 1 d . . . C(44) C 1.3892(5) 0.9832(3) 0.5501(2) 0.0502(14) Uani 1 1 d . . . C(61) C 1.2757(4) 0.8213(2) 0.70477(18) 0.0329(10) Uani 1 1 d . . . C(62) C 1.2872(5) 0.8158(3) 0.7632(2) 0.0441(13) Uani 1 1 d . . . C(63) C 1.3807(4) 0.7940(3) 0.6818(2) 0.0495(14) Uani 1 1 d . . . C(64) C 1.1854(4) 0.7736(3) 0.6853(2) 0.0420(12) Uani 1 1 d . . . C(221) C 0.9249(4) 0.8390(3) 0.6377(2) 0.0487(14) Uani 1 1 d . . . C(222) C 0.6922(5) 0.8717(4) 0.6163(2) 0.0623(17) Uani 1 1 d . . . C(223) C 0.7680(6) 0.7226(3) 0.6312(3) 0.0658(19) Uani 1 1 d . . . C(321) C 0.8309(5) 1.0124(3) 0.9768(2) 0.0489(13) Uani 1 1 d . . . C(322) C 0.9791(5) 1.1112(4) 0.9185(2) 0.0631(17) Uani 1 1 d . . . C(323) C 0.7732(7) 1.1627(3) 0.9650(2) 0.070(2) Uani 1 1 d . . . C(401) C 1.2129(4) 0.9724(4) 0.8394(2) 0.0509(14) Uani 1 1 d . . . C(402) C 1.2702(5) 0.9340(4) 0.8803(3) 0.075(2) Uani 1 1 d . . . C(403) C 1.1932(6) 0.9372(5) 0.9249(2) 0.086(3) Uani 1 1 d . . . C(404) C 1.0888(5) 0.9306(4) 0.9003(2) 0.066(2) Uani 1 1 d . . . C(501) C 0.8932(5) 0.8225(3) 0.8627(2) 0.0443(13) Uani 1 1 d . . . C(502) C 0.8993(10) 0.7483(3) 0.8642(3) 0.120(4) Uani 1 1 d . . . C(503) C 0.9402(7) 0.7223(3) 0.8165(3) 0.075(2) Uani 1 1 d . . . C(504) C 0.9848(4) 0.7844(2) 0.7881(2) 0.0371(11) Uani 1 1 d . . . C(901) C 0.0938(9) 0.9139(5) 0.5093(4) 0.097(3) Uani 1 1 d . . . C(902) C 0.0437(12) 0.9245(6) 0.4636(4) 0.127(4) Uani 1 1 d . . . C(903) C -0.0016(16) 0.9889(6) 0.4524(5) 0.175(7) Uani 1 1 d . . . C(904) C 0.0049(9) 1.0439(6) 0.4858(3) 0.114(3) Uani 1 1 d . . . C(905) C 0.0495(8) 1.0316(6) 0.5308(3) 0.100(3) Uani 1 1 d . . . C(906) C 0.0920(6) 0.9659(5) 0.5448(3) 0.082(2) Uani 1 1 d . . . C(907) C 0.1392(10) 0.8459(7) 0.5228(5) 0.143(5) Uani 1 1 d . . . C(911) C 0.7250(10) 0.7744(9) 0.0764(6) 0.165(6) Uani 1 1 d D . . C(912) C 0.7885(12) 0.8060(11) 0.0345(6) 0.213(9) Uani 1 1 d D . . C(913) C 0.7160(12) 0.8036(10) -0.0112(6) 0.171(6) Uani 1 1 d D . . C(914) C 0.6158(12) 0.7764(8) 0.0112(5) 0.147(5) Uani 1 1 d D . . H(3) H 1.2059 1.0828 0.6507 0.039 Uiso 1 1 calc R . . H(5) H 1.3717 0.9065 0.6386 0.041 Uiso 1 1 calc R . . H(12) H 1.1222 1.0792 0.7905 0.035 Uiso 1 1 calc R . . H(13) H 0.9358 1.1096 0.8158 0.036 Uiso 1 1 calc R . . H(15) H 0.7371 1.1112 0.7578 0.049 Uiso 1 1 calc R . . H(16) H 0.6675 1.0861 0.6782 0.060 Uiso 1 1 calc R . . H(17) H 0.7719 1.0363 0.6137 0.060 Uiso 1 1 calc R . . H(18) H 0.9480 1.0089 0.6278 0.045 Uiso 1 1 calc R . . H(23) H 0.6547 0.7343 0.7211 0.037 Uiso 1 1 calc R . . H(25) H 0.5370 0.6886 0.7906 0.045 Uiso 1 1 calc R . . H(26) H 0.4450 0.7080 0.8661 0.046 Uiso 1 1 calc R . . H(27) H 0.4632 0.8118 0.9096 0.044 Uiso 1 1 calc R . . H(28) H 0.5696 0.8989 0.8777 0.040 Uiso 1 1 calc R . . H(33) H 0.6465 1.1401 0.8842 0.042 Uiso 1 1 calc R . . H(35) H 0.4730 1.1544 0.8393 0.046 Uiso 1 1 calc R . . H(36) H 0.3441 1.1123 0.7854 0.047 Uiso 1 1 calc R . . H(37) H 0.3712 1.0064 0.7417 0.043 Uiso 1 1 calc R . . H(38) H 0.5215 0.9431 0.7563 0.040 Uiso 1 1 calc R . . H(22A) H 0.9299 0.8541 0.6025 0.073 Uiso 1 1 calc R . . H(22B) H 0.9706 0.7995 0.6428 0.073 Uiso 1 1 calc R . . H(22C) H 0.9466 0.8760 0.6602 0.073 Uiso 1 1 calc R . . H(22D) H 0.6909 0.9168 0.6322 0.093 Uiso 1 1 calc R . . H(22E) H 0.6217 0.8521 0.6169 0.093 Uiso 1 1 calc R . . H(22F) H 0.7159 0.8759 0.5812 0.093 Uiso 1 1 calc R . . H(22G) H 0.6940 0.7099 0.6333 0.099 Uiso 1 1 calc R . . H(22H) H 0.8092 0.6927 0.6531 0.099 Uiso 1 1 calc R . . H(22I) H 0.7922 0.7178 0.5962 0.099 Uiso 1 1 calc R . . H(32A) H 0.7581 1.0049 0.9871 0.073 Uiso 1 1 calc R . . H(32B) H 0.8736 1.0219 1.0067 0.073 Uiso 1 1 calc R . . H(32C) H 0.8574 0.9715 0.9598 0.073 Uiso 1 1 calc R . . H(32D) H 1.0170 1.1162 0.9505 0.095 Uiso 1 1 calc R . . H(32E) H 0.9814 1.1543 0.8998 0.095 Uiso 1 1 calc R . . H(32F) H 1.0119 1.0752 0.8982 0.095 Uiso 1 1 calc R . . H(32G) H 0.7052 1.1487 0.9785 0.105 Uiso 1 1 calc R . . H(32H) H 0.7633 1.1998 0.9407 0.105 Uiso 1 1 calc R . . H(32I) H 0.8181 1.1783 0.9927 0.105 Uiso 1 1 calc R . . H(40A) H 1.2283 1.0218 0.8416 0.061 Uiso 1 1 calc R . . H(40B) H 1.2342 0.9558 0.8056 0.061 Uiso 1 1 calc R . . H(40C) H 1.3373 0.9564 0.8888 0.090 Uiso 1 1 calc R . . H(40D) H 1.2839 0.8863 0.8701 0.090 Uiso 1 1 calc R . . H(40E) H 1.2056 0.8994 0.9490 0.104 Uiso 1 1 calc R . . H(40F) H 1.1992 0.9811 0.9432 0.104 Uiso 1 1 calc R . . H(40G) H 1.0353 0.9560 0.9197 0.080 Uiso 1 1 calc R . . H(40H) H 1.0677 0.8821 0.8987 0.080 Uiso 1 1 calc R . . H(42A) H 1.5139 0.9980 0.6334 0.072 Uiso 1 1 calc R . . H(42B) H 1.4781 1.0721 0.6517 0.072 Uiso 1 1 calc R . . H(42C) H 1.5346 1.0629 0.5982 0.072 Uiso 1 1 calc R . . H(43A) H 1.3837 1.1182 0.5501 0.071 Uiso 1 1 calc R . . H(43B) H 1.3382 1.1348 0.6051 0.071 Uiso 1 1 calc R . . H(43C) H 1.2662 1.0974 0.5641 0.071 Uiso 1 1 calc R . . H(44A) H 1.4365 1.0041 0.5254 0.075 Uiso 1 1 calc R . . H(44B) H 1.3207 0.9757 0.5345 0.075 Uiso 1 1 calc R . . H(44C) H 1.4182 0.9395 0.5612 0.075 Uiso 1 1 calc R . . H(50A) H 0.9239 0.8422 0.8939 0.053 Uiso 1 1 calc R . . H(50B) H 0.8193 0.8374 0.8603 0.053 Uiso 1 1 calc R . . H(50C) H 0.9455 0.7339 0.8923 0.144 Uiso 1 1 calc R . . H(50D) H 0.8288 0.7291 0.8704 0.144 Uiso 1 1 calc R . . H(50E) H 0.8838 0.7005 0.7966 0.090 Uiso 1 1 calc R . . H(50F) H 0.9958 0.6882 0.8227 0.090 Uiso 1 1 calc R . . H(50G) H 1.0620 0.7813 0.7860 0.045 Uiso 1 1 calc R . . H(50H) H 0.9562 0.7864 0.7533 0.045 Uiso 1 1 calc R . . H(62A) H 1.3496 0.8408 0.7741 0.066 Uiso 1 1 calc R . . H(62B) H 1.2940 0.7678 0.7728 0.066 Uiso 1 1 calc R . . H(62C) H 1.2252 0.8353 0.7795 0.066 Uiso 1 1 calc R . . H(63A) H 1.3763 0.7947 0.6448 0.074 Uiso 1 1 calc R . . H(63B) H 1.3927 0.7472 0.6933 0.074 Uiso 1 1 calc R . . H(63C) H 1.4387 0.8231 0.6928 0.074 Uiso 1 1 calc R . . H(64A) H 1.1183 0.7894 0.6989 0.063 Uiso 1 1 calc R . . H(64B) H 1.1984 0.7268 0.6966 0.063 Uiso 1 1 calc R . . H(64C) H 1.1831 0.7749 0.6483 0.063 Uiso 1 1 calc R . . H(902) H 0.0396 0.8886 0.4396 0.152 Uiso 1 1 calc R . . H(903) H -0.0373 0.9948 0.4212 0.209 Uiso 1 1 calc R . . H(904) H -0.0210 1.0877 0.4772 0.137 Uiso 1 1 calc R . . H(905) H 0.0535 1.0678 0.5545 0.120 Uiso 1 1 calc R . . H(906) H 0.1183 0.9584 0.5779 0.098 Uiso 1 1 calc R . . H(90A) H 0.1494 0.8433 0.5595 0.214 Uiso 1 1 calc R . . H(90B) H 0.2067 0.8401 0.5057 0.214 Uiso 1 1 calc R . . H(90C) H 0.0913 0.8097 0.5120 0.214 Uiso 1 1 calc R . . H(91A) H 0.7694 0.7436 0.0969 0.198 Uiso 1 1 calc R . . H(91B) H 0.6964 0.8103 0.0988 0.198 Uiso 1 1 calc R . . H(91C) H 0.8531 0.7795 0.0281 0.256 Uiso 1 1 calc R . . H(91D) H 0.8078 0.8535 0.0428 0.256 Uiso 1 1 calc R . . H(91E) H 0.7058 0.8495 -0.0258 0.205 Uiso 1 1 calc R . . H(91F) H 0.7436 0.7727 -0.0376 0.205 Uiso 1 1 calc R . . H(91G) H 0.5700 0.8147 0.0215 0.177 Uiso 1 1 calc R . . H(91H) H 0.5780 0.7487 -0.0142 0.177 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 Zr 0.02306(18) 0.02225(17) 0.03046(19) 0.00157(16) 0.00060(19) -0.00101(18) Si(22) 0.0316(7) 0.0364(7) 0.0331(7) -0.0017(5) 0.0027(6) -0.0080(6) Si(32) 0.0468(8) 0.0388(8) 0.0339(7) -0.0071(6) -0.0010(6) -0.0053(6) O(1) 0.0236(15) 0.0296(16) 0.0314(16) -0.0003(12) 0.0023(13) -0.0009(13) O(2) 0.0266(16) 0.0263(15) 0.0329(16) -0.0038(12) 0.0052(13) -0.0001(13) O(3) 0.0221(14) 0.0273(16) 0.0306(15) 0.0025(12) -0.0003(12) 0.0005(13) O(4) 0.0266(15) 0.0437(18) 0.0324(16) 0.0004(16) -0.0026(13) 0.0003(16) O(5) 0.0351(18) 0.0254(15) 0.0365(17) 0.0024(13) 0.0091(15) 0.0038(12) O(9) 0.172(9) 0.170(9) 0.166(8) -0.032(7) -0.034(7) 0.047(7) C(1) 0.022(2) 0.027(2) 0.033(2) 0.0021(15) 0.0003(18) -0.0021(17) C(2) 0.026(2) 0.033(2) 0.027(2) -0.0001(18) 0.0004(18) -0.0053(18) C(3) 0.030(2) 0.035(2) 0.034(2) 0.000(2) 0.0037(19) 0.002(2) C(4) 0.025(2) 0.039(3) 0.033(2) -0.0031(19) 0.0042(19) -0.005(2) C(5) 0.024(2) 0.041(3) 0.037(3) 0.0063(19) 0.009(2) -0.002(2) C(6) 0.028(2) 0.026(2) 0.032(2) 0.0028(17) 0.0012(19) 0.0012(18) C(11) 0.0257(19) 0.0275(19) 0.031(2) 0.0027(16) 0.0039(17) 0.002(2) C(12) 0.027(2) 0.031(2) 0.030(2) -0.0021(16) 0.0037(17) -0.0003(18) C(13) 0.038(2) 0.0138(16) 0.037(2) -0.0050(17) 0.008(2) 0.0007(18) C(14) 0.028(2) 0.023(2) 0.039(2) 0.0027(18) 0.006(2) 0.0000(19) C(15) 0.034(3) 0.033(2) 0.055(3) 0.007(2) 0.005(2) 0.010(2) C(16) 0.034(3) 0.049(3) 0.068(4) 0.009(2) -0.010(3) 0.009(3) C(17) 0.049(3) 0.054(3) 0.045(3) 0.003(3) -0.012(2) 0.008(3) C(18) 0.041(3) 0.034(3) 0.038(3) 0.002(2) -0.005(2) 0.002(2) C(19) 0.027(2) 0.0223(19) 0.035(2) 0.0009(18) -0.0030(17) 0.0014(17) C(21) 0.023(2) 0.022(2) 0.031(2) -0.0011(16) -0.0023(18) 0.0013(17) C(22) 0.029(2) 0.023(2) 0.035(2) 0.0020(16) 0.000(2) -0.004(2) C(23) 0.031(2) 0.027(2) 0.034(2) 0.0021(18) -0.004(2) -0.0030(19) C(24) 0.027(2) 0.0205(19) 0.040(3) -0.0013(15) 0.002(2) -0.0030(19) C(25) 0.032(2) 0.032(2) 0.049(3) -0.008(2) 0.002(2) 0.000(2) C(26) 0.033(3) 0.036(3) 0.045(3) 0.0000(19) 0.005(2) 0.007(2) C(27) 0.032(2) 0.041(3) 0.037(3) -0.0020(19) 0.0056(19) 0.006(2) C(28) 0.030(2) 0.034(2) 0.036(3) 0.0007(18) 0.0025(19) -0.003(2) C(29) 0.026(2) 0.025(2) 0.033(2) -0.0002(17) 0.0009(19) 0.0003(18) C(2A) 0.025(2) 0.0199(19) 0.032(2) 0.0007(16) -0.0033(18) -0.0002(16) C(31) 0.025(2) 0.026(2) 0.029(2) 0.0020(17) 0.0047(18) 0.0016(18) C(32) 0.026(2) 0.027(2) 0.038(3) -0.0003(17) 0.0071(19) -0.0038(19) C(33) 0.034(3) 0.028(2) 0.042(3) 0.0017(19) 0.007(2) -0.003(2) C(34) 0.024(2) 0.025(2) 0.039(3) -0.0002(17) 0.0060(19) 0.0030(19) C(35) 0.025(2) 0.028(2) 0.061(3) 0.0065(19) 0.008(2) -0.003(2) C(36) 0.028(2) 0.034(2) 0.056(3) 0.0074(18) 0.002(2) 0.014(2) C(37) 0.032(2) 0.033(2) 0.043(3) -0.0019(18) -0.001(2) 0.009(2) C(38) 0.031(2) 0.034(2) 0.036(3) -0.0008(17) 0.0010(19) 0.0023(19) C(39) 0.026(2) 0.028(2) 0.034(2) 0.0011(18) 0.0062(19) 0.0007(19) C(3A) 0.025(2) 0.025(2) 0.032(2) 0.0025(17) 0.0033(17) -0.0002(17) C(41) 0.036(2) 0.040(3) 0.035(2) -0.001(2) 0.005(2) 0.004(2) C(42) 0.034(3) 0.063(3) 0.048(3) -0.004(3) 0.005(2) 0.008(3) C(43) 0.042(3) 0.055(3) 0.045(3) 0.002(2) 0.007(2) 0.010(3) C(44) 0.056(3) 0.060(4) 0.035(3) 0.001(3) 0.014(3) -0.005(2) C(61) 0.027(2) 0.034(2) 0.038(3) 0.0059(19) 0.0019(19) -0.0025(19) C(62) 0.045(3) 0.041(3) 0.047(3) 0.012(2) 0.000(2) 0.009(2) C(63) 0.038(3) 0.040(3) 0.071(4) 0.020(2) 0.009(3) -0.003(3) C(64) 0.041(3) 0.035(3) 0.050(3) 0.002(2) 0.001(2) -0.004(2) C(221) 0.044(3) 0.063(4) 0.040(3) -0.004(3) 0.011(2) -0.010(3) C(222) 0.060(4) 0.084(5) 0.043(3) 0.018(3) -0.002(3) 0.002(3) C(223) 0.078(5) 0.058(4) 0.062(4) -0.022(3) 0.028(3) -0.026(3) C(321) 0.043(3) 0.058(3) 0.046(3) 0.002(3) -0.002(2) -0.001(3) C(322) 0.055(4) 0.084(5) 0.050(3) -0.024(3) -0.014(3) -0.001(3) C(323) 0.117(6) 0.049(4) 0.044(3) -0.002(4) -0.009(4) -0.013(3) C(401) 0.029(2) 0.076(4) 0.048(3) 0.003(3) 0.000(2) -0.004(3) C(402) 0.051(4) 0.118(7) 0.056(4) 0.029(4) -0.009(3) -0.001(4) C(403) 0.067(4) 0.154(9) 0.038(3) 0.025(5) -0.007(3) 0.004(4) C(404) 0.046(3) 0.110(6) 0.044(3) -0.013(3) -0.005(3) 0.025(3) C(501) 0.052(3) 0.043(3) 0.038(3) 0.003(2) 0.014(2) 0.012(2) C(502) 0.223(11) 0.029(3) 0.107(6) 0.002(5) 0.107(7) 0.006(4) C(503) 0.120(7) 0.026(3) 0.078(4) -0.004(3) 0.039(4) 0.005(3) C(504) 0.040(3) 0.024(2) 0.048(3) -0.0010(18) 0.012(2) -0.007(2) C(901) 0.115(7) 0.097(7) 0.080(6) -0.008(6) -0.025(5) 0.013(5) C(902) 0.194(12) 0.109(8) 0.077(6) -0.015(8) -0.045(7) 0.000(5) C(903) 0.33(2) 0.079(7) 0.118(9) -0.004(11) -0.052(12) -0.004(6) C(904) 0.173(11) 0.096(6) 0.072(5) -0.004(7) -0.030(6) 0.005(5) C(905) 0.108(7) 0.109(7) 0.083(6) -0.019(6) -0.001(5) 0.012(5) C(906) 0.083(5) 0.098(6) 0.064(4) 0.006(5) -0.006(4) -0.013(5) C(907) 0.156(11) 0.141(10) 0.133(10) 0.062(9) 0.031(8) 0.025(8) C(911) 0.100(8) 0.237(17) 0.156(12) -0.058(10) -0.068(9) 0.037(11) C(912) 0.108(10) 0.30(2) 0.229(18) -0.072(12) -0.056(12) 0.123(17) C(913) 0.138(11) 0.241(18) 0.135(11) -0.022(12) -0.010(10) 0.039(12) C(914) 0.162(13) 0.154(12) 0.126(10) -0.008(10) -0.030(9) 0.049(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_site_symmetry_2 _geom_bond_publ_flag Zr O(2) 2.017(3) . ? Zr O(3) 2.095(3) . ? Zr O(1) 2.100(3) . ? Zr O(5) 2.356(3) . ? Zr O(4) 2.387(3) . ? Zr C(12) 2.511(4) . ? Zr C(11) 2.531(4) . ? Zr C(13) 2.564(4) . ? Zr C(19) 2.696(4) . ? Zr C(14) 2.723(4) . ? Si(22) C(222) 1.852(6) . ? Si(22) C(221) 1.856(6) . ? Si(22) C(223) 1.858(6) . ? Si(22) C(22) 1.884(5) . ? Si(32) C(321) 1.856(6) . ? Si(32) C(323) 1.861(7) . ? Si(32) C(322) 1.865(7) . ? Si(32) C(32) 1.874(5) . ? O(1) C(1) 1.362(5) . ? O(2) C(21) 1.358(5) . ? O(3) C(31) 1.359(5) . ? O(4) C(404) 1.465(6) . ? O(4) C(401) 1.470(6) . ? O(5) C(504) 1.454(5) . ? O(5) C(501) 1.474(6) . ? C(1) C(2) 1.400(6) . ? C(1) C(6) 1.421(6) . ? C(2) C(3) 1.400(6) . ? C(2) C(11) 1.481(6) . ? C(3) C(4) 1.377(6) . ? C(4) C(5) 1.415(7) . ? C(4) C(41) 1.538(6) . ? C(5) C(6) 1.401(6) . ? C(6) C(61) 1.529(6) . ? C(11) C(12) 1.419(6) . ? C(11) C(19) 1.442(5) . ? C(12) C(13) 1.407(6) . ? C(13) C(14) 1.415(7) . ? C(14) C(19) 1.414(6) . ? C(14) C(15) 1.423(7) . ? C(15) C(16) 1.359(8) . ? C(16) C(17) 1.422(8) . ? C(17) C(18) 1.361(7) . ? C(18) C(19) 1.420(6) . ? C(21) C(2A) 1.384(6) . ? C(21) C(22) 1.442(6) . ? C(22) C(23) 1.385(6) . ? C(23) C(24) 1.405(6) . ? C(24) C(25) 1.412(6) . ? C(24) C(29) 1.433(6) . ? C(25) C(26) 1.378(7) . ? C(26) C(27) 1.382(7) . ? C(27) C(28) 1.376(6) . ? C(28) C(29) 1.417(6) . ? C(29) C(2A) 1.443(6) . ? C(2A) C(3A) 1.482(6) . ? C(31) C(3A) 1.387(6) . ? C(31) C(32) 1.439(6) . ? C(32) C(33) 1.394(6) . ? C(33) C(34) 1.437(7) . ? C(34) C(35) 1.410(6) . ? C(34) C(39) 1.422(6) . ? C(35) C(36) 1.358(7) . ? C(36) C(37) 1.422(7) . ? C(37) C(38) 1.359(6) . ? C(38) C(39) 1.426(6) . ? C(39) C(3A) 1.431(6) . ? C(41) C(44) 1.524(7) . ? C(41) C(43) 1.529(7) . ? C(41) C(42) 1.537(7) . ? C(61) C(62) 1.525(7) . ? C(61) C(63) 1.536(6) . ? C(61) C(64) 1.541(7) . ? C(401) C(402) 1.476(8) . ? C(402) C(403) 1.506(9) . ? C(403) C(404) 1.460(9) . ? C(501) C(502) 1.430(8) . ? C(502) C(503) 1.429(9) . ? C(503) C(504) 1.510(7) . ? C(903) C(904) 1.370(14) . ? C(903) C(902) 1.393(15) . ? C(904) C(905) 1.312(11) . ? C(905) C(906) 1.419(13) . ? C(906) C(901) 1.359(12) . ? C(901) C(902) 1.355(12) . ? C(901) C(907) 1.469(14) . ? O(9) C(914) 1.366(13) . ? O(9) C(911) 1.416(13) . ? C(911) C(912) 1.477(13) . ? C(913) C(914) 1.478(13) . ? C(913) C(912) 1.491(13) . ? 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(2) Zr O(3) 92.63(12) . . ? O(2) Zr O(1) 99.08(11) . . ? O(3) Zr O(1) 150.49(12) . . ? O(2) Zr O(5) 82.25(12) . . ? O(3) Zr O(5) 76.03(11) . . ? O(1) Zr O(5) 78.83(11) . . ? O(2) Zr O(4) 159.02(12) . . ? O(3) Zr O(4) 79.22(11) . . ? O(1) Zr O(4) 80.30(11) . . ? O(5) Zr O(4) 77.05(12) . . ? O(2) Zr C(12) 125.41(13) . . ? O(3) Zr C(12) 105.28(13) . . ? O(1) Zr C(12) 89.82(13) . . ? O(5) Zr C(12) 151.72(13) . . ? O(4) Zr C(12) 75.54(13) . . ? O(2) Zr C(11) 102.30(13) . . ? O(3) Zr C(11) 134.25(13) . . ? O(1) Zr C(11) 69.37(12) . . ? O(5) Zr C(11) 148.20(12) . . ? O(4) Zr C(11) 97.11(12) . . ? C(12) Zr C(11) 32.69(14) . . ? O(2) Zr C(13) 107.36(14) . . ? O(3) Zr C(13) 80.51(13) . . ? O(1) Zr C(13) 120.72(13) . . ? O(5) Zr C(13) 155.07(13) . . ? O(4) Zr C(13) 90.48(14) . . ? C(12) Zr C(13) 32.16(14) . . ? C(11) Zr C(13) 53.80(14) . . ? O(2) Zr C(19) 74.34(12) . . ? O(3) Zr C(19) 120.61(12) . . ? O(1) Zr C(19) 88.72(12) . . ? O(5) Zr C(19) 151.39(12) . . ? O(4) Zr C(19) 126.43(12) . . ? C(12) Zr C(19) 51.98(13) . . ? C(11) Zr C(19) 31.83(12) . . ? C(13) Zr C(19) 51.59(14) . . ? O(2) Zr C(14) 77.88(13) . . ? O(3) Zr C(14) 90.66(12) . . ? O(1) Zr C(14) 118.19(13) . . ? O(5) Zr C(14) 155.52(13) . . ? O(4) Zr C(14) 121.11(13) . . ? C(12) Zr C(14) 51.44(14) . . ? C(11) Zr C(14) 52.08(13) . . ? C(13) Zr C(14) 30.86(14) . . ? C(19) Zr C(14) 30.26(13) . . ? C(222) Si(22) C(221) 109.7(3) . . ? C(222) Si(22) C(223) 110.2(4) . . ? C(221) Si(22) C(223) 106.8(3) . . ? C(222) Si(22) C(22) 105.2(2) . . ? C(221) Si(22) C(22) 116.4(2) . . ? C(223) Si(22) C(22) 108.5(2) . . ? C(321) Si(32) C(323) 107.3(3) . . ? C(321) Si(32) C(322) 110.4(3) . . ? C(323) Si(32) C(322) 107.9(4) . . ? C(321) Si(32) C(32) 106.4(2) . . ? C(323) Si(32) C(32) 108.5(3) . . ? C(322) Si(32) C(32) 116.1(2) . . ? C(1) O(1) Zr 128.6(3) . . ? C(21) O(2) Zr 129.1(3) . . ? C(31) O(3) Zr 122.1(3) . . ? C(404) O(4) C(401) 106.8(4) . . ? C(404) O(4) Zr 127.0(3) . . ? C(401) O(4) Zr 124.5(3) . . ? C(504) O(5) C(501) 107.8(3) . . ? C(504) O(5) Zr 121.9(3) . . ? C(501) O(5) Zr 128.7(3) . . ? O(1) C(1) C(2) 116.8(4) . . ? O(1) C(1) C(6) 123.7(4) . . ? C(2) C(1) C(6) 119.5(4) . . ? C(3) C(2) C(1) 121.6(4) . . ? C(3) C(2) C(11) 122.8(4) . . ? C(1) C(2) C(11) 115.7(4) . . ? C(4) C(3) C(2) 121.0(5) . . ? C(3) C(4) C(5) 116.4(4) . . ? C(3) C(4) C(41) 124.6(4) . . ? C(5) C(4) C(41) 118.8(4) . . ? C(6) C(5) C(4) 125.0(4) . . ? C(5) C(6) C(1) 116.2(4) . . ? C(5) C(6) C(61) 120.8(4) . . ? C(1) C(6) C(61) 123.0(4) . . ? C(12) C(11) C(19) 106.2(3) . . ? C(12) C(11) C(2) 126.8(4) . . ? C(19) C(11) C(2) 126.9(4) . . ? C(12) C(11) Zr 72.9(2) . . ? C(19) C(11) Zr 80.4(2) . . ? C(2) C(11) Zr 109.4(3) . . ? C(13) C(12) C(11) 109.3(4) . . ? C(13) C(12) Zr 76.0(2) . . ? C(11) C(12) Zr 74.4(2) . . ? C(12) C(13) C(14) 107.8(4) . . ? C(12) C(13) Zr 71.9(2) . . ? C(14) C(13) Zr 80.8(2) . . ? C(19) C(14) C(13) 108.2(4) . . ? C(19) C(14) C(15) 119.5(4) . . ? C(13) C(14) C(15) 132.3(4) . . ? C(19) C(14) Zr 73.8(2) . . ? C(13) C(14) Zr 68.4(2) . . ? C(15) C(14) Zr 123.6(3) . . ? C(16) C(15) C(14) 118.3(5) . . ? C(15) C(16) C(17) 121.7(5) . . ? C(18) C(17) C(16) 121.7(5) . . ? C(17) C(18) C(19) 117.5(5) . . ? C(14) C(19) C(18) 121.3(4) . . ? C(14) C(19) C(11) 108.1(4) . . ? C(18) C(19) C(11) 130.6(4) . . ? C(14) C(19) Zr 75.9(2) . . ? C(18) C(19) Zr 123.8(3) . . ? C(11) C(19) Zr 67.8(2) . . ? O(2) C(21) C(2A) 120.3(4) . . ? O(2) C(21) C(22) 117.6(4) . . ? C(2A) C(21) C(22) 122.1(4) . . ? C(23) C(22) C(21) 116.7(4) . . ? C(23) C(22) Si(22) 118.5(3) . . ? C(21) C(22) Si(22) 122.8(3) . . ? C(22) C(23) C(24) 123.8(4) . . ? C(23) C(24) C(25) 122.8(4) . . ? C(23) C(24) C(29) 118.0(4) . . ? C(25) C(24) C(29) 119.2(4) . . ? C(26) C(25) C(24) 120.6(4) . . ? C(25) C(26) C(27) 120.4(4) . . ? C(28) C(27) C(26) 121.0(5) . . ? C(27) C(28) C(29) 120.8(4) . . ? C(28) C(29) C(24) 118.0(4) . . ? C(28) C(29) C(2A) 122.3(4) . . ? C(24) C(29) C(2A) 119.7(4) . . ? C(21) C(2A) C(29) 118.5(4) . . ? C(21) C(2A) C(3A) 122.5(4) . . ? C(29) C(2A) C(3A) 118.8(4) . . ? O(3) C(31) C(3A) 120.7(4) . . ? O(3) C(31) C(32) 117.4(4) . . ? C(3A) C(31) C(32) 121.8(4) . . ? C(33) C(32) C(31) 117.2(4) . . ? C(33) C(32) Si(32) 118.5(3) . . ? C(31) C(32) Si(32) 122.9(3) . . ? C(32) C(33) C(34) 122.6(4) . . ? C(35) C(34) C(39) 120.9(4) . . ? C(35) C(34) C(33) 121.4(4) . . ? C(39) C(34) C(33) 117.7(4) . . ? C(36) C(35) C(34) 120.6(4) . . ? C(35) C(36) C(37) 119.8(4) . . ? C(38) C(37) C(36) 120.0(5) . . ? C(37) C(38) C(39) 122.3(4) . . ? C(34) C(39) C(38) 116.3(4) . . ? C(34) C(39) C(3A) 120.5(4) . . ? C(38) C(39) C(3A) 123.2(4) . . ? C(31) C(3A) C(39) 119.0(4) . . ? C(31) C(3A) C(2A) 124.6(4) . . ? C(39) C(3A) C(2A) 116.4(4) . . ? C(44) C(41) C(43) 108.3(4) . . ? C(44) C(41) C(42) 109.6(4) . . ? C(43) C(41) C(42) 108.1(5) . . ? C(44) C(41) C(4) 110.6(4) . . ? C(43) C(41) C(4) 111.0(4) . . ? C(42) C(41) C(4) 109.2(4) . . ? C(62) C(61) C(6) 110.6(4) . . ? C(62) C(61) C(63) 106.3(4) . . ? C(6) C(61) C(63) 113.1(4) . . ? C(62) C(61) C(64) 110.7(4) . . ? C(6) C(61) C(64) 108.8(4) . . ? C(63) C(61) C(64) 107.3(4) . . ? O(4) C(401) C(402) 106.1(5) . . ? C(401) C(402) C(403) 102.7(5) . . ? C(404) C(403) C(402) 103.5(5) . . ? C(403) C(404) O(4) 107.1(5) . . ? C(502) C(501) O(5) 107.3(5) . . ? C(503) C(502) C(501) 110.2(6) . . ? C(502) C(503) C(504) 106.2(5) . . ? O(5) C(504) C(503) 106.9(4) . . ? C(904) C(903) C(902) 122.0(12) . . ? C(905) C(904) C(903) 116.7(11) . . ? C(904) C(905) C(906) 123.2(10) . . ? C(901) C(906) C(905) 119.1(8) . . ? C(902) C(901) C(906) 118.3(10) . . ? C(902) C(901) C(907) 121.4(11) . . ? C(906) C(901) C(907) 119.9(9) . . ? C(901) C(902) C(903) 120.2(11) . . ? C(914) O(9) C(911) 102.8(11) . . ? O(9) C(911) C(912) 107.4(11) . . ? C(914) C(913) C(912) 102.5(11) . . ? O(9) C(914) C(913) 108.4(11) . . ? C(911) C(912) C(913) 104.1(11) . . ?