# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Norbert Mitzel' 'Jochen Niemeyer' 'Alexander Willner' _publ_contact_author_name 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Bis-Hydroxylaminato Group 4 Halfsandwich Complexes - Syntheses, Structures and Polymerisation Activity Studies ; # Attachment 'merged.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 712228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cp*TiMe(ONMe)2CH2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 N2 O2 Ti' _chemical_formula_weight 302.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1352(13) _cell_length_b 8.6112(14) _cell_length_c 12.593(2) _cell_angle_alpha 78.397(18) _cell_angle_beta 86.828(18) _cell_angle_gamma 65.249(16) _cell_volume 784.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.56 _cell_measurement_theta_max 26.9 _exptl_crystal_description Plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7719 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details ; absorption correction was done with the program abscor from the STOE IPDS-1 sotware package. abscor works similar to the well known difabs but uses Fo^2^ values instead of Fo. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12203 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 26.90 _reflns_number_total 3118 _reflns_number_gt 2745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.2927P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3118 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.68574(4) 0.72819(4) 0.81044(2) 0.01485(11) Uani 1 1 d . . . O1 O 0.50834(17) 0.76321(16) 0.92172(10) 0.0196(3) Uani 1 1 d . . . O2 O 0.90998(17) 0.51473(15) 0.84099(10) 0.0204(3) Uani 1 1 d . . . N1 N 0.6768(2) 0.68617(18) 0.98025(11) 0.0174(3) Uani 1 1 d . . . N2 N 0.7746(2) 0.46173(18) 0.89157(12) 0.0189(3) Uani 1 1 d . . . C1 C 0.5014(3) 0.7018(2) 0.68339(14) 0.0219(4) Uani 1 1 d . . . C2 C 0.4253(3) 0.8789(2) 0.69302(14) 0.0210(4) Uani 1 1 d . . . C3 C 0.5503(3) 0.9492(2) 0.65262(14) 0.0215(4) Uani 1 1 d . . . C4 C 0.7037(3) 0.8154(2) 0.61870(14) 0.0234(4) Uani 1 1 d . . . C5 C 0.6726(3) 0.6635(2) 0.63595(14) 0.0235(4) Uani 1 1 d . . . C6 C 0.4069(3) 0.5823(3) 0.70873(18) 0.0359(5) Uani 1 1 d . . . H6A H 0.3624 0.5713 0.6411 0.050(8) Uiso 1 1 calc R . . H6B H 0.3047 0.6305 0.7551 0.056(9) Uiso 1 1 calc R . . H6C H 0.4920 0.4672 0.7465 0.089(12) Uiso 1 1 calc R . . C7 C 0.2425(3) 0.9741(3) 0.73684(17) 0.0325(5) Uani 1 1 d . . . H7A H 0.2281 1.0906 0.7433 0.065(9) Uiso 1 1 calc R . . H7B H 0.2324 0.9090 0.8084 0.066(9) Uiso 1 1 calc R . . H7C H 0.1478 0.9847 0.6874 0.056(9) Uiso 1 1 calc R . . C8 C 0.5183(3) 1.1373(3) 0.63750(17) 0.0342(5) Uani 1 1 d . . . H8A H 0.4818 1.1947 0.5618 0.072(10) Uiso 1 1 calc R . . H8B H 0.6301 1.1446 0.6559 0.080(11) Uiso 1 1 calc R . . H8C H 0.4222 1.1955 0.6850 0.072(10) Uiso 1 1 calc R . . C9 C 0.8671(3) 0.8318(4) 0.56615(18) 0.0395(5) Uani 1 1 d . . . H9A H 0.8611 0.9475 0.5672 0.071(10) Uiso 1 1 calc R . . H9B H 0.8701 0.8164 0.4909 0.071(10) Uiso 1 1 calc R . . H9C H 0.9767 0.7421 0.6059 0.065(10) Uiso 1 1 calc R . . C10 C 0.7956(4) 0.4960(3) 0.60340(18) 0.0381(5) Uani 1 1 d . . . H10A H 0.8184 0.5182 0.5258 0.054(8) Uiso 1 1 calc R . . H10B H 0.7385 0.4140 0.6180 0.067(10) Uiso 1 1 calc R . . H10C H 0.9105 0.4460 0.6451 0.047(8) Uiso 1 1 calc R . . C11 C 0.6769(3) 0.7696(2) 1.06930(14) 0.0231(4) Uani 1 1 d . . . H11A H 0.7959 0.7109 1.1068 0.030(6) Uiso 1 1 calc R . . H11B H 0.5839 0.7618 1.1202 0.032(6) Uiso 1 1 calc R . . H11C H 0.6511 0.8924 1.0411 0.037(7) Uiso 1 1 calc R . . C12 C 0.7479(3) 0.4968(2) 1.00171(14) 0.0199(4) Uani 1 1 d . . . H12A H 0.6600 0.4553 1.0402 0.029(6) Uiso 1 1 calc R . . H12B H 0.8635 0.4423 1.0445 0.025(6) Uiso 1 1 calc R . . C13 C 0.8119(3) 0.2843(2) 0.88411(17) 0.0285(4) Uani 1 1 d . . . H13A H 0.9302 0.2049 0.9188 0.040(7) Uiso 1 1 calc R . . H13B H 0.8128 0.2756 0.8077 0.038(7) Uiso 1 1 calc R . . H13C H 0.7178 0.2524 0.9208 0.047(8) Uiso 1 1 calc R . . C14 C 0.8126(3) 0.8964(2) 0.82783(16) 0.0246(4) Uani 1 1 d . . . H14A H 0.9103 0.8357 0.8834 0.049(8) Uiso 1 1 calc R . . H14B H 0.7227 1.0023 0.8495 0.070(10) Uiso 1 1 calc R . . H14C H 0.8628 0.9281 0.7585 0.059(9) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01481(19) 0.01379(16) 0.01606(17) -0.00341(11) -0.00005(11) -0.00580(12) O1 0.0144(7) 0.0226(6) 0.0180(6) -0.0027(5) -0.0033(5) -0.0042(5) O2 0.0172(7) 0.0176(6) 0.0255(6) -0.0041(5) 0.0035(5) -0.0067(5) N1 0.0154(8) 0.0164(7) 0.0174(7) -0.0029(5) -0.0039(5) -0.0033(5) N2 0.0191(8) 0.0161(7) 0.0227(7) -0.0046(5) 0.0014(6) -0.0083(6) C1 0.0264(11) 0.0255(9) 0.0170(8) -0.0032(7) -0.0042(7) -0.0136(7) C2 0.0184(10) 0.0258(9) 0.0164(8) -0.0031(6) -0.0045(6) -0.0068(7) C3 0.0264(11) 0.0199(8) 0.0167(8) 0.0000(6) -0.0047(7) -0.0093(7) C4 0.0243(11) 0.0297(9) 0.0168(8) -0.0025(7) 0.0008(7) -0.0128(8) C5 0.0290(11) 0.0235(9) 0.0172(8) -0.0080(7) 0.0001(7) -0.0084(7) C6 0.0460(15) 0.0416(12) 0.0323(11) -0.0032(9) -0.0064(9) -0.0310(11) C7 0.0189(11) 0.0431(12) 0.0280(10) -0.0069(9) -0.0026(8) -0.0053(8) C8 0.0493(15) 0.0219(9) 0.0297(11) 0.0022(8) -0.0105(9) -0.0149(9) C9 0.0360(14) 0.0597(15) 0.0276(11) -0.0072(10) 0.0112(9) -0.0264(11) C10 0.0477(15) 0.0307(11) 0.0294(11) -0.0148(9) 0.0026(9) -0.0062(10) C11 0.0227(11) 0.0236(9) 0.0207(9) -0.0076(7) -0.0018(7) -0.0057(7) C12 0.0210(10) 0.0163(8) 0.0207(8) -0.0008(6) -0.0012(7) -0.0072(7) C13 0.0325(12) 0.0168(8) 0.0379(11) -0.0081(7) 0.0000(8) -0.0104(8) C14 0.0263(11) 0.0225(9) 0.0289(10) -0.0025(7) -0.0039(7) -0.0144(8) _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 Ti1 O1 1.9285(13) . ? Ti1 O2 1.9596(14) . ? Ti1 N1 2.0983(15) . ? Ti1 N2 2.1403(15) . ? Ti1 C14 2.1489(18) . ? Ti1 C1 2.3575(19) . ? Ti1 C2 2.3730(19) . ? Ti1 C5 2.3914(18) . ? Ti1 C4 2.3955(18) . ? Ti1 C3 2.3981(18) . ? Ti1 C12 2.7182(18) . ? O1 N1 1.4194(19) . ? O2 N2 1.4325(19) . ? N1 C11 1.449(2) . ? N1 C12 1.455(2) . ? N2 C13 1.450(2) . ? N2 C12 1.464(2) . ? C1 C2 1.414(3) . ? C1 C5 1.417(3) . ? C1 C6 1.501(3) . ? C2 C3 1.412(3) . ? C2 C7 1.503(3) . ? C3 C4 1.415(3) . ? C3 C8 1.502(2) . ? C4 C5 1.407(3) . ? C4 C9 1.499(3) . ? C5 C10 1.494(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O2 116.58(6) . . ? O1 Ti1 N1 41.01(6) . . ? O2 Ti1 N1 82.59(6) . . ? O1 Ti1 N2 82.16(6) . . ? O2 Ti1 N2 40.60(5) . . ? N1 Ti1 N2 64.36(6) . . ? O1 Ti1 C14 104.06(7) . . ? O2 Ti1 C14 94.20(7) . . ? N1 Ti1 C14 84.96(7) . . ? N2 Ti1 C14 125.08(7) . . ? O1 Ti1 C1 94.39(6) . . ? O2 Ti1 C1 109.89(6) . . ? N1 Ti1 C1 129.52(7) . . ? N2 Ti1 C1 93.21(6) . . ? C14 Ti1 C1 138.97(7) . . ? O1 Ti1 C2 83.04(6) . . ? O2 Ti1 C2 143.64(6) . . ? N1 Ti1 C2 123.86(6) . . ? N2 Ti1 C2 123.76(6) . . ? C14 Ti1 C2 111.13(7) . . ? C1 Ti1 C2 34.79(6) . . ? O1 Ti1 C5 128.85(7) . . ? O2 Ti1 C5 87.73(6) . . ? N1 Ti1 C5 154.78(6) . . ? N2 Ti1 C5 93.41(6) . . ? C14 Ti1 C5 119.07(7) . . ? C1 Ti1 C5 34.71(7) . . ? C2 Ti1 C5 57.52(7) . . ? O1 Ti1 C4 139.90(6) . . ? O2 Ti1 C4 100.70(6) . . ? N1 Ti1 C4 171.04(6) . . ? N2 Ti1 C4 123.32(6) . . ? C14 Ti1 C4 86.48(7) . . ? C1 Ti1 C4 57.38(7) . . ? C2 Ti1 C4 57.35(7) . . ? C5 Ti1 C4 34.18(6) . . ? O1 Ti1 C3 107.89(6) . . ? O2 Ti1 C3 134.84(6) . . ? N1 Ti1 C3 140.96(6) . . ? N2 Ti1 C3 148.86(6) . . ? C14 Ti1 C3 82.01(7) . . ? C1 Ti1 C3 57.35(6) . . ? C2 Ti1 C3 34.41(6) . . ? C5 Ti1 C3 57.00(6) . . ? C4 Ti1 C3 34.34(7) . . ? O1 Ti1 C12 58.44(5) . . ? O2 Ti1 C12 58.16(6) . . ? N1 Ti1 C12 32.00(5) . . ? N2 Ti1 C12 32.37(5) . . ? C14 Ti1 C12 106.25(7) . . ? C1 Ti1 C12 114.62(6) . . ? C2 Ti1 C12 131.56(6) . . ? C5 Ti1 C12 125.02(6) . . ? C4 Ti1 C12 155.34(6) . . ? C3 Ti1 C12 165.07(6) . . ? N1 O1 Ti1 75.93(8) . . ? N2 O2 Ti1 76.50(8) . . ? O1 N1 C11 113.07(13) . . ? O1 N1 C12 111.12(13) . . ? C11 N1 C12 117.93(14) . . ? O1 N1 Ti1 63.06(7) . . ? C11 N1 Ti1 140.30(12) . . ? C12 N1 Ti1 98.18(10) . . ? O2 N2 C13 112.05(14) . . ? O2 N2 C12 109.70(13) . . ? C13 N2 C12 114.72(14) . . ? O2 N2 Ti1 62.90(7) . . ? C13 N2 Ti1 147.53(13) . . ? C12 N2 Ti1 96.09(10) . . ? C2 C1 C5 108.14(16) . . ? C2 C1 C6 125.15(19) . . ? C5 C1 C6 126.43(18) . . ? C2 C1 Ti1 73.20(10) . . ? C5 C1 Ti1 73.95(11) . . ? C6 C1 Ti1 123.49(13) . . ? C3 C2 C1 107.72(16) . . ? C3 C2 C7 126.72(17) . . ? C1 C2 C7 125.55(18) . . ? C3 C2 Ti1 73.77(10) . . ? C1 C2 Ti1 72.00(11) . . ? C7 C2 Ti1 120.69(12) . . ? C2 C3 C4 108.11(16) . . ? C2 C3 C8 125.93(18) . . ? C4 C3 C8 125.69(18) . . ? C2 C3 Ti1 71.82(10) . . ? C4 C3 Ti1 72.73(10) . . ? C8 C3 Ti1 125.92(13) . . ? C5 C4 C3 108.17(17) . . ? C5 C4 C9 124.76(19) . . ? C3 C4 C9 126.95(18) . . ? C5 C4 Ti1 72.75(10) . . ? C3 C4 Ti1 72.93(10) . . ? C9 C4 Ti1 123.33(14) . . ? C4 C5 C1 107.84(16) . . ? C4 C5 C10 125.2(2) . . ? C1 C5 C10 126.87(19) . . ? C4 C5 Ti1 73.07(10) . . ? C1 C5 Ti1 71.34(10) . . ? C10 C5 Ti1 123.88(14) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 N2 101.35(13) . . ? N1 C12 Ti1 49.83(8) . . ? N2 C12 Ti1 51.53(8) . . ? N1 C12 H12A 111.5 . . ? N2 C12 H12A 111.5 . . ? Ti1 C12 H12A 126.2 . . ? N1 C12 H12B 111.5 . . ? N2 C12 H12B 111.5 . . ? Ti1 C12 H12B 124.5 . . ? H12A C12 H12B 109.3 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Ti1 C14 H14A 109.5 . . ? Ti1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Ti1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.90 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.281 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.057 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 712229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cp*Ti(Me)(ONMeCH2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 N2 O2 Ti' _chemical_formula_weight 316.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 13.138(2) _cell_length_b 15.3130(18) _cell_length_c 16.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3344.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.54 _cell_measurement_theta_max 26.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.515 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45620 _diffrn_reflns_av_R_equivalents 0.0979 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3265 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+33.0178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3265 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.1103 _refine_ls_wR_factor_ref 0.2490 _refine_ls_wR_factor_gt 0.2468 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.70803(8) 0.06676(7) 0.36176(7) 0.0226(3) Uani 1 1 d . . . O1 O 0.6215(5) 0.0561(3) 0.4549(4) 0.0548(18) Uani 1 1 d . . . O2 O 0.6073(4) 0.0661(3) 0.2783(3) 0.0413(13) Uani 1 1 d . . . N1 N 0.6624(7) -0.0288(4) 0.4465(5) 0.064(3) Uani 1 1 d . . . N2 N 0.6213(5) -0.0232(4) 0.2945(5) 0.0427(17) Uani 1 1 d . . . C1 C 0.8534(5) 0.1624(4) 0.3806(3) 0.0210(13) Uani 1 1 d . . . C2 C 0.8133(4) 0.1784(4) 0.3029(3) 0.0178(12) Uani 1 1 d . . . C3 C 0.7151(4) 0.2148(4) 0.3118(4) 0.0209(12) Uani 1 1 d . . . C4 C 0.6925(5) 0.2174(4) 0.3950(4) 0.0271(14) Uani 1 1 d . . . C5 C 0.7785(6) 0.1865(4) 0.4367(4) 0.0336(17) Uani 1 1 d . . . C6 C 0.9614(5) 0.1372(5) 0.3981(4) 0.0342(16) Uani 1 1 d . . . H6A H 1.0022 0.1900 0.4066 0.051 Uiso 1 1 calc R . . H6B H 0.9890 0.1042 0.3525 0.051 Uiso 1 1 calc R . . H6C H 0.9636 0.1009 0.4466 0.051 Uiso 1 1 calc R . . C7 C 0.8649(5) 0.1652(4) 0.2238(4) 0.0290(15) Uani 1 1 d . . . H7A H 0.8855 0.2219 0.2019 0.044 Uiso 1 1 calc R . . H7B H 0.8178 0.1367 0.1864 0.044 Uiso 1 1 calc R . . H7C H 0.9251 0.1283 0.2313 0.044 Uiso 1 1 calc R . . C8 C 0.6462(5) 0.2450(4) 0.2452(5) 0.0315(15) Uani 1 1 d . . . H8A H 0.6590 0.3068 0.2339 0.047 Uiso 1 1 calc R . . H8B H 0.5750 0.2373 0.2615 0.047 Uiso 1 1 calc R . . H8C H 0.6595 0.2105 0.1967 0.047 Uiso 1 1 calc R . . C9 C 0.5960(7) 0.2492(5) 0.4320(6) 0.054(3) Uani 1 1 d . . . H9A H 0.5944 0.3131 0.4306 0.081 Uiso 1 1 calc R . . H9B H 0.5922 0.2292 0.4880 0.081 Uiso 1 1 calc R . . H9C H 0.5378 0.2260 0.4019 0.081 Uiso 1 1 calc R . . C10 C 0.7906(9) 0.1836(6) 0.5266(4) 0.059(3) Uani 1 1 d . . . H10A H 0.8099 0.2416 0.5463 0.089 Uiso 1 1 calc R . . H10B H 0.8437 0.1414 0.5407 0.089 Uiso 1 1 calc R . . H10C H 0.7261 0.1659 0.5513 0.089 Uiso 1 1 calc R . . C11 C 0.7192(14) -0.0537(7) 0.5212(6) 0.111(6) Uani 1 1 d . . . H11A H 0.6715 -0.0776 0.5608 0.167 Uiso 1 1 calc R . . H11B H 0.7527 -0.0020 0.5436 0.167 Uiso 1 1 calc R . . H11C H 0.7706 -0.0979 0.5080 0.167 Uiso 1 1 calc R . . C12 C 0.5886(8) -0.0928(6) 0.4234(8) 0.076(4) Uani 1 1 d . . . H12A H 0.5383 -0.1017 0.4670 0.091 Uiso 1 1 calc R . . H12B H 0.6221 -0.1492 0.4115 0.091 Uiso 1 1 calc R . . C13 C 0.5383(7) -0.0578(6) 0.3505(9) 0.078(4) Uani 1 1 d . . . H13A H 0.4908 -0.0102 0.3653 0.093 Uiso 1 1 calc R . . H13B H 0.4991 -0.1045 0.3234 0.093 Uiso 1 1 calc R . . C14 C 0.6429(9) -0.0715(6) 0.2232(7) 0.074(3) Uani 1 1 d . . . H14A H 0.5794 -0.0834 0.1943 0.111 Uiso 1 1 calc R . . H14B H 0.6757 -0.1268 0.2375 0.111 Uiso 1 1 calc R . . H14C H 0.6885 -0.0375 0.1886 0.111 Uiso 1 1 calc R . . C15 C 0.8336(6) -0.0226(5) 0.3385(5) 0.0409(18) Uani 1 1 d . . . H15A H 0.8067 -0.0812 0.3279 0.061 Uiso 1 1 calc R . . H15B H 0.8785 -0.0246 0.3856 0.061 Uiso 1 1 calc R . . H15C H 0.8722 -0.0023 0.2917 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0251(6) 0.0151(5) 0.0277(6) -0.0022(5) 0.0080(5) -0.0013(5) O1 0.079(4) 0.024(3) 0.061(4) -0.006(3) 0.052(3) -0.003(3) O2 0.035(3) 0.018(2) 0.071(4) -0.004(2) -0.016(3) 0.001(2) N1 0.111(7) 0.020(3) 0.061(5) 0.004(3) 0.051(5) 0.000(4) N2 0.035(3) 0.017(3) 0.075(5) -0.004(3) -0.022(3) -0.001(3) C1 0.027(3) 0.021(3) 0.015(3) 0.000(2) -0.002(2) -0.006(2) C2 0.020(3) 0.017(3) 0.016(3) 0.001(2) 0.007(2) -0.013(2) C3 0.019(3) 0.014(3) 0.030(3) -0.002(2) 0.006(3) -0.005(2) C4 0.028(3) 0.018(3) 0.035(4) -0.004(3) 0.015(3) -0.004(3) C5 0.062(5) 0.021(3) 0.018(3) -0.005(3) 0.010(3) -0.010(3) C6 0.034(4) 0.037(4) 0.031(4) -0.001(3) -0.014(3) -0.007(3) C7 0.035(4) 0.031(3) 0.021(3) 0.000(3) 0.005(3) -0.004(3) C8 0.019(3) 0.023(3) 0.053(4) 0.010(3) -0.004(3) 0.000(3) C9 0.064(6) 0.031(4) 0.066(6) -0.009(4) 0.046(5) -0.002(4) C10 0.119(9) 0.042(4) 0.016(3) -0.006(3) 0.010(4) -0.016(5) C11 0.223(18) 0.052(6) 0.057(7) 0.024(5) 0.041(9) 0.011(9) C12 0.069(7) 0.029(4) 0.129(10) -0.001(5) 0.058(7) -0.009(4) C13 0.032(4) 0.027(4) 0.174(13) 0.019(6) 0.000(6) -0.010(4) C14 0.090(8) 0.039(5) 0.093(8) -0.030(5) -0.040(7) 0.005(5) C15 0.034(4) 0.025(3) 0.063(5) -0.003(3) 0.000(4) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.917(5) . ? Ti1 O1 1.928(5) . ? Ti1 N2 2.108(6) . ? Ti1 N1 2.118(7) . ? Ti1 C15 2.179(7) . ? Ti1 C4 2.381(6) . ? Ti1 C5 2.402(6) . ? Ti1 C2 2.406(5) . ? Ti1 C3 2.416(6) . ? Ti1 C1 2.427(6) . ? O1 N1 1.414(8) . ? O2 N2 1.404(7) . ? N1 C12 1.430(13) . ? N1 C11 1.499(16) . ? N2 C14 1.427(11) . ? N2 C13 1.529(12) . ? C1 C5 1.405(9) . ? C1 C2 1.416(8) . ? C1 C6 1.500(9) . ? C2 C3 1.413(8) . ? C2 C7 1.493(8) . ? C3 C4 1.414(9) . ? C3 C8 1.504(9) . ? C4 C5 1.407(10) . ? C4 C9 1.491(9) . ? C5 C10 1.504(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.480(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 O2 Ti1 O1 100.0(3) . . ? O2 Ti1 N2 40.5(2) . . ? O1 Ti1 N2 93.0(3) . . ? O2 Ti1 N1 106.4(3) . . ? O1 Ti1 N1 40.6(2) . . ? N2 Ti1 N1 75.4(3) . . ? O2 Ti1 C15 113.0(3) . . ? O1 Ti1 C15 122.4(3) . . ? N2 Ti1 C15 84.6(3) . . ? N1 Ti1 C15 84.2(3) . . ? O2 Ti1 C4 96.5(2) . . ? O1 Ti1 C4 81.1(2) . . ? N2 Ti1 C4 135.2(2) . . ? N1 Ti1 C4 119.4(2) . . ? C15 Ti1 C4 135.6(3) . . ? O2 Ti1 C5 130.2(2) . . ? O1 Ti1 C5 82.8(2) . . ? N2 Ti1 C5 169.0(3) . . ? N1 Ti1 C5 107.0(3) . . ? C15 Ti1 C5 106.3(3) . . ? C4 Ti1 C5 34.2(2) . . ? O2 Ti1 C2 96.1(2) . . ? O1 Ti1 C2 136.5(2) . . ? N2 Ti1 C2 124.0(2) . . ? N1 Ti1 C2 157.5(3) . . ? C15 Ti1 C2 86.5(2) . . ? C4 Ti1 C2 57.0(2) . . ? C5 Ti1 C2 56.4(2) . . ? O2 Ti1 C3 77.5(2) . . ? O1 Ti1 C3 112.2(2) . . ? N2 Ti1 C3 116.8(2) . . ? N1 Ti1 C3 152.6(2) . . ? C15 Ti1 C3 120.0(3) . . ? C4 Ti1 C3 34.3(2) . . ? C5 Ti1 C3 56.4(2) . . ? C2 Ti1 C3 34.1(2) . . ? O2 Ti1 C1 129.8(2) . . ? O1 Ti1 C1 114.3(2) . . ? N2 Ti1 C1 152.6(3) . . ? N1 Ti1 C1 123.7(3) . . ? C15 Ti1 C1 78.8(2) . . ? C4 Ti1 C1 56.8(2) . . ? C5 Ti1 C1 33.8(2) . . ? C2 Ti1 C1 34.07(19) . . ? C3 Ti1 C1 56.5(2) . . ? N1 O1 Ti1 77.0(3) . . ? N2 O2 Ti1 77.1(3) . . ? O1 N1 C12 113.5(8) . . ? O1 N1 C11 109.9(8) . . ? C12 N1 C11 112.7(8) . . ? O1 N1 Ti1 62.5(3) . . ? C12 N1 Ti1 119.1(7) . . ? C11 N1 Ti1 125.9(8) . . ? O2 N2 C14 111.8(7) . . ? O2 N2 C13 111.2(6) . . ? C14 N2 C13 117.9(7) . . ? O2 N2 Ti1 62.4(3) . . ? C14 N2 Ti1 132.2(6) . . ? C13 N2 Ti1 106.8(6) . . ? C5 C1 C2 107.4(6) . . ? C5 C1 C6 127.0(6) . . ? C2 C1 C6 125.0(6) . . ? C5 C1 Ti1 72.1(4) . . ? C2 C1 Ti1 72.2(3) . . ? C6 C1 Ti1 127.9(4) . . ? C3 C2 C1 108.2(5) . . ? C3 C2 C7 124.1(6) . . ? C1 C2 C7 127.7(6) . . ? C3 C2 Ti1 73.3(3) . . ? C1 C2 Ti1 73.8(3) . . ? C7 C2 Ti1 121.5(4) . . ? C2 C3 C4 107.8(6) . . ? C2 C3 C8 126.4(6) . . ? C4 C3 C8 125.8(6) . . ? C2 C3 Ti1 72.6(3) . . ? C4 C3 Ti1 71.5(3) . . ? C8 C3 Ti1 121.2(4) . . ? C5 C4 C3 107.7(6) . . ? C5 C4 C9 126.1(7) . . ? C3 C4 C9 126.2(7) . . ? C5 C4 Ti1 73.7(4) . . ? C3 C4 Ti1 74.2(3) . . ? C9 C4 Ti1 119.0(5) . . ? C1 C5 C4 108.9(5) . . ? C1 C5 C10 125.3(8) . . ? C4 C5 C10 125.8(7) . . ? C1 C5 Ti1 74.1(3) . . ? C4 C5 Ti1 72.1(4) . . ? C10 C5 Ti1 122.2(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 106.0(7) . . ? N1 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? N1 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C12 C13 N2 107.8(7) . . ? C12 C13 H13A 110.1 . . ? N2 C13 H13A 110.1 . . ? C12 C13 H13B 110.1 . . ? N2 C13 H13B 110.1 . . ? H13A C13 H13B 108.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Ti1 C15 H15A 109.5 . . ? Ti1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Ti1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.735 _refine_diff_density_min -1.484 _refine_diff_density_rms 0.119 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 712230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cp*ZrMe(ONMECH2)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 N2 O2 Zr' _chemical_formula_weight 359.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1653(12) _cell_length_b 27.663(5) _cell_length_c 8.4512(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.931(15) _cell_angle_gamma 90.00 _cell_volume 1731.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.03 _cell_measurement_theta_max 25.65 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23381 _diffrn_reflns_av_R_equivalents 0.1592 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 25.65 _reflns_number_total 3077 _reflns_number_gt 2542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+0.8583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3077 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.65887(3) 0.133148(8) 0.93476(3) 0.02033(11) Uani 1 1 d . . . O2 O 0.6610(3) 0.20361(7) 0.8632(3) 0.0292(5) Uani 1 1 d . . . O1 O 0.9132(3) 0.11100(7) 0.9711(2) 0.0284(4) Uani 1 1 d . . . N2 N 0.6405(3) 0.17808(8) 0.7081(3) 0.0260(5) Uani 1 1 d . . . N1 N 0.8067(3) 0.09269(8) 0.7996(3) 0.0278(5) Uani 1 1 d . . . C1 C 0.5582(4) 0.10035(10) 1.1639(4) 0.0263(6) Uani 1 1 d . . . C2 C 0.7483(4) 0.09693(10) 1.2355(3) 0.0265(6) Uani 1 1 d . . . C3 C 0.8188(4) 0.14471(10) 1.2574(3) 0.0241(6) Uani 1 1 d . . . C4 C 0.6716(4) 0.17729(9) 1.2008(3) 0.0229(6) Uani 1 1 d . . . C5 C 0.5103(4) 0.14995(10) 1.1396(3) 0.0238(6) Uani 1 1 d . . . C6 C 0.4281(5) 0.05937(11) 1.1385(5) 0.0408(8) Uani 1 1 d . . . H6A H 0.4183 0.0531 1.2483 0.061 Uiso 1 1 calc R . . H6B H 0.4721 0.0303 1.1027 0.061 Uiso 1 1 calc R . . H6C H 0.3091 0.0681 1.0481 0.061 Uiso 1 1 calc R . . C7 C 0.8580(5) 0.05138(11) 1.2870(4) 0.0388(8) Uani 1 1 d . . . H7A H 0.9038 0.0467 1.4134 0.058 Uiso 1 1 calc R . . H7B H 0.9598 0.0538 1.2548 0.058 Uiso 1 1 calc R . . H7C H 0.7821 0.0238 1.2265 0.058 Uiso 1 1 calc R . . C8 C 1.0150(4) 0.15765(12) 1.3354(4) 0.0348(7) Uani 1 1 d . . . H8A H 1.0641 0.1551 1.4628 0.052 Uiso 1 1 calc R . . H8B H 1.0294 0.1909 1.3029 0.052 Uiso 1 1 calc R . . H8C H 1.0800 0.1355 1.2917 0.052 Uiso 1 1 calc R . . C9 C 0.6820(5) 0.23159(10) 1.2085(4) 0.0309(7) Uani 1 1 d . . . H9A H 0.6295 0.2435 1.2862 0.046 Uiso 1 1 calc R . . H9B H 0.6146 0.2449 1.0912 0.046 Uiso 1 1 calc R . . H9C H 0.8086 0.2417 1.2532 0.046 Uiso 1 1 calc R . . C10 C 0.3227(4) 0.17066(12) 1.0681(4) 0.0342(7) Uani 1 1 d . . . H10A H 0.3160 0.1955 1.1480 0.051 Uiso 1 1 calc R . . H10B H 0.2360 0.1449 1.0560 0.051 Uiso 1 1 calc R . . H10C H 0.2939 0.1852 0.9536 0.051 Uiso 1 1 calc R . . C11 C 0.8428(5) 0.04122(11) 0.7934(5) 0.0428(8) Uani 1 1 d . . . H11A H 0.9691 0.0366 0.8139 0.064 Uiso 1 1 calc R . . H11B H 0.7636 0.0283 0.6785 0.064 Uiso 1 1 calc R . . H11C H 0.8198 0.0242 0.8837 0.064 Uiso 1 1 calc R . . C12 C 0.8441(4) 0.12067(12) 0.6700(4) 0.0335(7) Uani 1 1 d . . . H12A H 0.7643 0.1095 0.5509 0.040 Uiso 1 1 calc R . . H12B H 0.9710 0.1157 0.6886 0.040 Uiso 1 1 calc R . . C13 C 0.8108(4) 0.17425(11) 0.6891(4) 0.0318(7) Uani 1 1 d . . . H13A H 0.9115 0.1879 0.7930 0.038 Uiso 1 1 calc R . . H13B H 0.8022 0.1923 0.5848 0.038 Uiso 1 1 calc R . . C14 C 0.4890(5) 0.19685(12) 0.5568(4) 0.0393(8) Uani 1 1 d . . . H14A H 0.5101 0.2310 0.5407 0.059 Uiso 1 1 calc R . . H14D H 0.3783 0.1937 0.5743 0.059 Uiso 1 1 calc R . . H14B H 0.4763 0.1785 0.4530 0.059 Uiso 1 1 calc R . . C15 C 0.4037(4) 0.09210(11) 0.7544(4) 0.0356(7) Uani 1 1 d . . . H15D H 0.3914 0.0938 0.6341 0.053 Uiso 1 1 calc R . . H15A H 0.2976 0.1068 0.7611 0.053 Uiso 1 1 calc R . . H15B H 0.4134 0.0582 0.7912 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02090(16) 0.02075(14) 0.01985(15) -0.00045(10) 0.00908(10) -0.00048(10) O2 0.0440(13) 0.0244(9) 0.0215(10) -0.0006(8) 0.0159(9) 0.0003(8) O1 0.0256(11) 0.0375(11) 0.0212(10) -0.0021(8) 0.0089(8) 0.0013(8) N2 0.0313(14) 0.0288(12) 0.0201(11) 0.0024(9) 0.0131(10) 0.0022(9) N1 0.0288(14) 0.0306(13) 0.0263(12) -0.0037(10) 0.0140(10) -0.0004(10) C1 0.0316(17) 0.0242(13) 0.0268(14) -0.0009(11) 0.0158(12) -0.0036(11) C2 0.0351(17) 0.0248(13) 0.0219(13) 0.0029(11) 0.0143(12) 0.0023(11) C3 0.0229(15) 0.0291(14) 0.0203(13) 0.0019(10) 0.0092(11) 0.0002(11) C4 0.0290(16) 0.0203(13) 0.0231(13) 0.0006(10) 0.0146(11) -0.0007(10) C5 0.0282(16) 0.0252(13) 0.0215(13) 0.0009(10) 0.0140(11) 0.0012(11) C6 0.052(2) 0.0300(16) 0.0440(19) 0.0005(14) 0.0241(17) -0.0117(14) C7 0.053(2) 0.0295(15) 0.0376(18) 0.0092(13) 0.0234(16) 0.0139(14) C8 0.0272(18) 0.0459(18) 0.0275(15) -0.0003(13) 0.0080(13) -0.0009(13) C9 0.0438(19) 0.0208(13) 0.0316(16) -0.0026(11) 0.0191(13) -0.0018(12) C10 0.0286(18) 0.0418(17) 0.0347(16) 0.0068(13) 0.0156(13) 0.0059(13) C11 0.054(2) 0.0305(16) 0.051(2) -0.0043(15) 0.0296(18) 0.0094(15) C12 0.0308(18) 0.0451(17) 0.0309(15) -0.0014(13) 0.0190(13) 0.0033(13) C13 0.0340(18) 0.0370(16) 0.0304(15) 0.0040(12) 0.0193(13) -0.0037(13) C14 0.039(2) 0.0490(19) 0.0265(15) 0.0056(14) 0.0105(14) 0.0104(14) C15 0.0290(17) 0.0413(17) 0.0326(16) -0.0038(13) 0.0091(13) -0.0084(13) _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 Zr1 O2 2.0431(19) . ? Zr1 O1 2.060(2) . ? Zr1 N2 2.235(2) . ? Zr1 N1 2.275(2) . ? Zr1 C15 2.297(3) . ? Zr1 C3 2.498(3) . ? Zr1 C4 2.522(3) . ? Zr1 C2 2.536(3) . ? Zr1 C5 2.540(3) . ? Zr1 C1 2.567(3) . ? O2 N2 1.435(3) . ? O1 N1 1.432(3) . ? N2 C14 1.450(4) . ? N2 C13 1.470(4) . ? N1 C11 1.459(4) . ? N1 C12 1.474(4) . ? C1 C2 1.411(4) . ? C1 C5 1.418(4) . ? C1 C6 1.506(4) . ? C2 C3 1.422(4) . ? C2 C7 1.500(4) . ? C3 C4 1.415(4) . ? C3 C8 1.496(4) . ? C4 C5 1.414(4) . ? C4 C9 1.504(4) . ? C5 C10 1.503(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.527(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14D 0.9800 . ? C14 H14B 0.9800 . ? C15 H15D 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? 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 O2 Zr1 O1 101.20(8) . . ? O2 Zr1 N2 38.88(8) . . ? O1 Zr1 N2 89.57(8) . . ? O2 Zr1 N1 104.37(8) . . ? O1 Zr1 N1 38.17(8) . . ? N2 Zr1 N1 72.63(9) . . ? O2 Zr1 C15 113.19(10) . . ? O1 Zr1 C15 121.82(10) . . ? N2 Zr1 C15 89.53(10) . . ? N1 Zr1 C15 87.05(11) . . ? O2 Zr1 C3 97.77(8) . . ? O1 Zr1 C3 81.09(9) . . ? N2 Zr1 C3 132.82(9) . . ? N1 Zr1 C3 117.84(9) . . ? C15 Zr1 C3 134.28(11) . . ? O2 Zr1 C4 78.45(8) . . ? O1 Zr1 C4 110.54(8) . . ? N2 Zr1 C4 117.23(8) . . ? N1 Zr1 C4 148.70(9) . . ? C15 Zr1 C4 121.06(11) . . ? C3 Zr1 C4 32.72(9) . . ? O2 Zr1 C2 129.70(8) . . ? O1 Zr1 C2 83.50(9) . . ? N2 Zr1 C2 164.93(9) . . ? N1 Zr1 C2 108.61(9) . . ? C15 Zr1 C2 105.49(11) . . ? C3 Zr1 C2 32.81(9) . . ? C4 Zr1 C2 53.95(9) . . ? O2 Zr1 C5 95.35(8) . . ? O1 Zr1 C5 133.92(8) . . ? N2 Zr1 C5 127.11(9) . . ? N1 Zr1 C5 159.85(9) . . ? C15 Zr1 C5 89.00(11) . . ? C3 Zr1 C5 54.05(9) . . ? C4 Zr1 C5 32.44(9) . . ? C2 Zr1 C5 53.69(9) . . ? O2 Zr1 C1 127.28(8) . . ? O1 Zr1 C1 113.92(9) . . ? N2 Zr1 C1 156.34(9) . . ? N1 Zr1 C1 127.67(9) . . ? C15 Zr1 C1 80.60(11) . . ? C3 Zr1 C1 53.71(9) . . ? C4 Zr1 C1 53.45(9) . . ? C2 Zr1 C1 32.10(10) . . ? C5 Zr1 C1 32.22(9) . . ? N2 O2 Zr1 77.79(12) . . ? N1 O1 Zr1 79.09(13) . . ? O2 N2 C14 110.9(2) . . ? O2 N2 C13 112.6(2) . . ? C14 N2 C13 115.1(2) . . ? O2 N2 Zr1 63.33(11) . . ? C14 N2 Zr1 132.8(2) . . ? C13 N2 Zr1 109.20(17) . . ? O1 N1 C11 109.6(2) . . ? O1 N1 C12 109.8(2) . . ? C11 N1 C12 112.2(2) . . ? O1 N1 Zr1 62.74(12) . . ? C11 N1 Zr1 131.0(2) . . ? C12 N1 Zr1 115.74(18) . . ? C2 C1 C5 108.3(2) . . ? C2 C1 C6 126.4(3) . . ? C5 C1 C6 125.0(3) . . ? C2 C1 Zr1 72.72(16) . . ? C5 C1 Zr1 72.84(15) . . ? C6 C1 Zr1 126.1(2) . . ? C1 C2 C3 107.8(2) . . ? C1 C2 C7 126.5(3) . . ? C3 C2 C7 125.7(3) . . ? C1 C2 Zr1 75.17(16) . . ? C3 C2 Zr1 72.14(15) . . ? C7 C2 Zr1 120.5(2) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 C8 126.6(3) . . ? C2 C3 C8 125.4(3) . . ? C4 C3 Zr1 74.56(15) . . ? C2 C3 Zr1 75.05(16) . . ? C8 C3 Zr1 118.79(19) . . ? C3 C4 C5 108.1(2) . . ? C3 C4 C9 126.7(3) . . ? C5 C4 C9 125.2(3) . . ? C3 C4 Zr1 72.71(15) . . ? C5 C4 Zr1 74.49(15) . . ? C9 C4 Zr1 120.15(18) . . ? C4 C5 C1 107.9(2) . . ? C4 C5 C10 125.3(3) . . ? C1 C5 C10 126.8(3) . . ? C4 C5 Zr1 73.07(15) . . ? C1 C5 Zr1 74.94(16) . . ? C10 C5 Zr1 119.61(18) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 109.2(2) . . ? N1 C12 H12A 109.8 . . ? C13 C12 H12A 109.8 . . ? N1 C12 H12B 109.8 . . ? C13 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? N2 C13 C12 107.5(2) . . ? N2 C13 H13A 110.2 . . ? C12 C13 H13A 110.2 . . ? N2 C13 H13B 110.2 . . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14D 109.5 . . ? H14A C14 H14D 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14D C14 H14B 109.5 . . ? Zr1 C15 H15D 109.5 . . ? Zr1 C15 H15A 109.5 . . ? H15D C15 H15A 109.5 . . ? Zr1 C15 H15B 109.5 . . ? H15D C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.410 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.074 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 712231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cp*HfMe(ONMeCH2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 Hf N2 O2' _chemical_formula_weight 446.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5774(14) _cell_length_b 12.692(2) _cell_length_c 15.920(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.200(18) _cell_angle_gamma 90.00 _cell_volume 1733.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 4.74 _cell_measurement_theta_max 26.89 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 6.022 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26431 _diffrn_reflns_av_R_equivalents 0.1501 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.74 _diffrn_reflns_theta_max 26.89 _reflns_number_total 3493 _reflns_number_gt 2902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS-1 software package' _computing_cell_refinement 'STOE IPDS-1 software package' _computing_data_reduction 'STOE IPDS-1 software package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+65.0715P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3493 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.308 _refine_ls_restrained_S_all 1.308 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.74400(7) 0.73223(4) 0.05623(3) 0.01659(18) Uani 1 1 d . . . O1 O 0.9409(13) 0.6411(9) 0.0495(7) 0.031(3) Uani 1 1 d . . . O2 O 0.5799(14) 0.6202(9) 0.0465(6) 0.034(3) Uani 1 1 d . . . N1 N 0.930(2) 0.6834(13) -0.0341(10) 0.049(5) Uani 1 1 d . . . N2 N 0.636(2) 0.6280(13) -0.0382(9) 0.045(4) Uani 1 1 d . . . C1 C 0.751(2) 0.8824(11) 0.1609(9) 0.025(3) Uani 1 1 d . . . C2 C 0.608(2) 0.8287(11) 0.1735(10) 0.028(4) Uani 1 1 d . . . C3 C 0.635(2) 0.7326(14) 0.2015(10) 0.039(5) Uani 1 1 d . . . C4 C 0.797(3) 0.7135(12) 0.2090(9) 0.039(5) Uani 1 1 d . . . C5 C 0.876(2) 0.8103(14) 0.1842(11) 0.037(4) Uani 1 1 d . . . C6 C 0.775(3) 0.9969(13) 0.1406(12) 0.046(5) Uani 1 1 d . . . H6A H 0.7785 1.0378 0.1928 0.069 Uiso 1 1 calc R . . H6B H 0.6889 1.0221 0.1054 0.069 Uiso 1 1 calc R . . H6C H 0.8736 1.0055 0.1104 0.069 Uiso 1 1 calc R . . C7 C 0.454(2) 0.8802(15) 0.1558(13) 0.047(5) Uani 1 1 d . . . H7A H 0.3892 0.8781 0.2066 0.070 Uiso 1 1 calc R . . H7B H 0.4004 0.8424 0.1104 0.070 Uiso 1 1 calc R . . H7C H 0.4704 0.9536 0.1391 0.070 Uiso 1 1 calc R . . C8 C 0.509(2) 0.6519(14) 0.2221(11) 0.037(4) Uani 1 1 d . . . H8A H 0.4382 0.6813 0.2643 0.055 Uiso 1 1 calc R . . H8B H 0.5575 0.5877 0.2442 0.055 Uiso 1 1 calc R . . H8C H 0.4498 0.6350 0.1710 0.055 Uiso 1 1 calc R . . C9 C 0.873(3) 0.6152(17) 0.2389(12) 0.059(7) Uani 1 1 d . . . H9A H 0.8370 0.5994 0.2959 0.089 Uiso 1 1 calc R . . H9B H 0.9860 0.6242 0.2391 0.089 Uiso 1 1 calc R . . H9C H 0.8443 0.5569 0.2014 0.089 Uiso 1 1 calc R . . C10 C 1.046(2) 0.830(2) 0.1822(17) 0.079(9) Uani 1 1 d . . . H10A H 1.0814 0.8542 0.2375 0.119 Uiso 1 1 calc R . . H10B H 1.0695 0.8832 0.1398 0.119 Uiso 1 1 calc R . . H10C H 1.1004 0.7640 0.1680 0.119 Uiso 1 1 calc R . . C11 C 1.078(2) 0.7376(17) -0.0545(14) 0.054(5) Uani 1 1 d . . . H11A H 1.1616 0.6855 -0.0592 0.081 Uiso 1 1 calc R . . H11B H 1.1032 0.7880 -0.0099 0.081 Uiso 1 1 calc R . . H11C H 1.0662 0.7751 -0.1080 0.081 Uiso 1 1 calc R . . C12 C 0.893(2) 0.6002(15) -0.0900(12) 0.042(4) Uani 1 1 d . . . H12A H 0.9815 0.5502 -0.0923 0.051 Uiso 1 1 calc R . . H12B H 0.8768 0.6291 -0.1471 0.051 Uiso 1 1 calc R . . C13 C 0.752(2) 0.5438(11) -0.0633(10) 0.033(4) Uani 1 1 d . . . H13A H 0.7751 0.4969 -0.0152 0.039 Uiso 1 1 calc R . . H13B H 0.7096 0.5008 -0.1100 0.039 Uiso 1 1 calc R . . C14 C 0.511(3) 0.6392(17) -0.0967(13) 0.053(5) Uani 1 1 d . . . H14A H 0.4544 0.5722 -0.1014 0.079 Uiso 1 1 calc R . . H14B H 0.5519 0.6590 -0.1518 0.079 Uiso 1 1 calc R . . H14C H 0.4391 0.6940 -0.0770 0.079 Uiso 1 1 calc R . . C15 C 0.698(3) 0.8706(15) -0.0305(14) 0.061(7) Uani 1 1 d . . . H15A H 0.6826 0.8449 -0.0880 0.092 Uiso 1 1 calc R . . H15B H 0.7869 0.9188 -0.0289 0.092 Uiso 1 1 calc R . . H15C H 0.6038 0.9078 -0.0121 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.0218(3) 0.0125(3) 0.0155(3) 0.0007(2) 0.00281(19) 0.0002(2) O1 0.022(6) 0.047(7) 0.025(5) 0.009(5) 0.012(5) 0.019(5) O2 0.035(7) 0.049(7) 0.019(5) -0.005(5) 0.014(5) -0.025(5) N1 0.055(11) 0.051(10) 0.041(9) 0.016(7) 0.025(8) 0.030(8) N2 0.048(11) 0.056(10) 0.032(8) 0.005(7) 0.009(7) -0.025(8) C1 0.039(10) 0.016(7) 0.020(7) -0.009(5) 0.007(6) 0.003(6) C2 0.033(9) 0.022(8) 0.030(8) -0.015(6) 0.006(7) -0.005(6) C3 0.058(12) 0.031(8) 0.027(8) -0.016(7) 0.021(8) -0.027(8) C4 0.078(15) 0.023(9) 0.015(7) 0.002(5) -0.010(8) 0.018(8) C5 0.037(10) 0.040(9) 0.034(9) -0.022(7) 0.005(8) -0.005(8) C6 0.072(15) 0.025(9) 0.042(10) -0.006(7) -0.001(10) -0.015(9) C7 0.033(11) 0.052(11) 0.055(12) -0.026(9) 0.017(9) -0.008(8) C8 0.036(11) 0.039(9) 0.036(9) -0.007(7) 0.010(8) -0.019(8) C9 0.081(18) 0.067(14) 0.030(10) 0.000(9) -0.012(10) 0.052(13) C10 0.013(10) 0.13(2) 0.091(18) -0.069(17) -0.014(11) 0.014(12) C11 0.034(11) 0.062(13) 0.066(13) 0.006(11) 0.020(10) -0.004(9) C12 0.034(11) 0.045(11) 0.048(11) 0.004(8) 0.001(9) 0.017(8) C13 0.053(11) 0.020(7) 0.024(8) -0.006(6) 0.005(7) 0.004(7) C14 0.059(15) 0.051(12) 0.048(12) -0.005(9) 0.002(11) -0.018(10) C15 0.10(2) 0.031(10) 0.053(12) 0.018(9) 0.016(13) 0.009(11) _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 Hf1 O2 2.006(10) . ? Hf1 O1 2.050(10) . ? Hf1 N2 2.203(16) . ? Hf1 N1 2.239(14) . ? Hf1 C15 2.268(18) . ? Hf1 C4 2.484(15) . ? Hf1 C3 2.496(14) . ? Hf1 C2 2.521(14) . ? Hf1 C5 2.531(17) . ? Hf1 C1 2.532(13) . ? O1 N1 1.438(18) . ? O2 N2 1.438(17) . ? N1 C12 1.42(3) . ? N1 C11 1.48(2) . ? N2 C14 1.43(3) . ? N2 C13 1.51(2) . ? C1 C2 1.41(2) . ? C1 C5 1.46(2) . ? C1 C6 1.50(2) . ? C2 C3 1.32(3) . ? C2 C7 1.51(3) . ? C3 C4 1.42(3) . ? C3 C8 1.53(2) . ? C4 C5 1.46(2) . ? C4 C9 1.48(2) . ? C5 C10 1.48(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.47(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 O2 Hf1 O1 100.0(5) . . ? O2 Hf1 N2 39.6(4) . . ? O1 Hf1 N2 88.2(6) . . ? O2 Hf1 N1 104.8(6) . . ? O1 Hf1 N1 38.9(5) . . ? N2 Hf1 N1 72.1(7) . . ? O2 Hf1 C15 112.4(8) . . ? O1 Hf1 C15 123.2(7) . . ? N2 Hf1 C15 88.7(8) . . ? N1 Hf1 C15 86.9(7) . . ? O2 Hf1 C4 97.7(6) . . ? O1 Hf1 C4 81.3(5) . . ? N2 Hf1 C4 133.3(6) . . ? N1 Hf1 C4 118.2(6) . . ? C15 Hf1 C4 134.5(7) . . ? O2 Hf1 C3 78.9(5) . . ? O1 Hf1 C3 111.1(6) . . ? N2 Hf1 C3 118.4(5) . . ? N1 Hf1 C3 149.9(7) . . ? C15 Hf1 C3 119.8(7) . . ? C4 Hf1 C3 33.1(7) . . ? O2 Hf1 C2 94.3(5) . . ? O1 Hf1 C2 134.1(5) . . ? N2 Hf1 C2 127.1(6) . . ? N1 Hf1 C2 160.4(6) . . ? C15 Hf1 C2 89.7(7) . . ? C4 Hf1 C2 53.5(6) . . ? C3 Hf1 C2 30.5(6) . . ? O2 Hf1 C5 130.7(5) . . ? O1 Hf1 C5 84.0(5) . . ? N2 Hf1 C5 166.0(6) . . ? N1 Hf1 C5 107.9(6) . . ? C15 Hf1 C5 105.3(8) . . ? C4 Hf1 C5 33.8(6) . . ? C3 Hf1 C5 54.6(6) . . ? C2 Hf1 C5 54.6(5) . . ? O2 Hf1 C1 126.8(5) . . ? O1 Hf1 C1 116.2(5) . . ? N2 Hf1 C1 155.5(6) . . ? N1 Hf1 C1 128.1(6) . . ? C15 Hf1 C1 79.7(7) . . ? C4 Hf1 C1 54.8(5) . . ? C3 Hf1 C1 52.9(5) . . ? C2 Hf1 C1 32.5(5) . . ? C5 Hf1 C1 33.5(6) . . ? N1 O1 Hf1 77.7(7) . . ? N2 O2 Hf1 77.6(7) . . ? C12 N1 O1 108.5(14) . . ? C12 N1 C11 113.5(15) . . ? O1 N1 C11 108.9(16) . . ? C12 N1 Hf1 116.8(13) . . ? O1 N1 Hf1 63.5(6) . . ? C11 N1 Hf1 128.7(14) . . ? C14 N2 O2 111.2(15) . . ? C14 N2 C13 113.0(15) . . ? O2 N2 C13 115.0(14) . . ? C14 N2 Hf1 134.3(14) . . ? O2 N2 Hf1 62.8(7) . . ? C13 N2 Hf1 109.4(12) . . ? C2 C1 C5 107.4(13) . . ? C2 C1 C6 128.1(16) . . ? C5 C1 C6 123.9(16) . . ? C2 C1 Hf1 73.3(8) . . ? C5 C1 Hf1 73.2(8) . . ? C6 C1 Hf1 126.1(11) . . ? C3 C2 C1 110.1(16) . . ? C3 C2 C7 128.2(16) . . ? C1 C2 C7 121.7(14) . . ? C3 C2 Hf1 73.7(9) . . ? C1 C2 Hf1 74.2(8) . . ? C7 C2 Hf1 118.8(11) . . ? C2 C3 C4 111.0(15) . . ? C2 C3 C8 124.7(19) . . ? C4 C3 C8 124.3(18) . . ? C2 C3 Hf1 75.8(9) . . ? C4 C3 Hf1 73.0(8) . . ? C8 C3 Hf1 117.7(10) . . ? C3 C4 C5 106.8(14) . . ? C3 C4 C9 126.7(19) . . ? C5 C4 C9 127(2) . . ? C3 C4 Hf1 73.9(9) . . ? C5 C4 Hf1 74.9(9) . . ? C9 C4 Hf1 118.3(11) . . ? C4 C5 C1 104.8(15) . . ? C4 C5 C10 127(2) . . ? C1 C5 C10 128(2) . . ? C4 C5 Hf1 71.4(9) . . ? C1 C5 Hf1 73.3(9) . . ? C10 C5 Hf1 119.1(12) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 111.4(15) . . ? N1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 N2 105.9(13) . . ? C12 C13 H13A 110.6 . . ? N2 C13 H13A 110.6 . . ? C12 C13 H13B 110.6 . . ? N2 C13 H13B 110.6 . . ? H13A C13 H13B 108.7 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Hf1 C15 H15A 109.5 . . ? Hf1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Hf1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 26.89 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 3.199 _refine_diff_density_min -5.025 _refine_diff_density_rms 0.288 #===END data_2xAlMe3 _database_code_depnum_ccdc_archive 'CCDC 712232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[cp*Ti(Me)(ONMeCH2)2] AlMe3 Adduct' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H37 Al N2 O2 Ti' _chemical_formula_weight 388.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6725(13) _cell_length_b 9.9179(15) _cell_length_c 13.241(2) _cell_angle_alpha 77.701(3) _cell_angle_beta 79.992(3) _cell_angle_gamma 75.798(3) _cell_volume 1069.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 30.03 _exptl_crystal_description prism _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method '\w and \phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12365 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6139 _reflns_number_gt 4195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT ans SADABS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. ; _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6139 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.23885(4) 0.84491(4) 0.24159(3) 0.02296(12) Uani 1 1 d . . . Al1 Al 0.62170(8) 0.56440(7) 0.19190(6) 0.02979(18) Uani 1 1 d . . . O1 O 0.41266(17) 0.66133(16) 0.23849(12) 0.0281(3) Uani 1 1 d . . . O2 O 0.07394(19) 0.8949(2) 0.15710(13) 0.0485(5) Uani 1 1 d . . . N1 N 0.2611(2) 0.6193(2) 0.25694(16) 0.0322(5) Uani 1 1 d . . . N2 N 0.2019(2) 0.8268(2) 0.09184(15) 0.0335(5) Uani 1 1 d . . . C1 C 0.1255(3) 1.0462(2) 0.32046(17) 0.0266(5) Uani 1 1 d . . . C2 C 0.0171(2) 0.9553(2) 0.35108(17) 0.0251(4) Uani 1 1 d . . . C3 C 0.0926(2) 0.8307(2) 0.41415(17) 0.0252(4) Uani 1 1 d . . . C4 C 0.2485(3) 0.8451(2) 0.42270(17) 0.0265(5) Uani 1 1 d . . . C5 C 0.2676(3) 0.9787(2) 0.36575(18) 0.0281(5) Uani 1 1 d . . . C6 C 0.0928(3) 1.1896(2) 0.2526(2) 0.0389(6) Uani 1 1 d . . . H6A H 0.0144 1.2557 0.2914 0.058 Uiso 1 1 calc R . . H6B H 0.0501 1.1832 0.1903 0.058 Uiso 1 1 calc R . . H6C H 0.1928 1.2235 0.2317 0.058 Uiso 1 1 calc R . . C7 C -0.1518(2) 0.9860(3) 0.3274(2) 0.0341(5) Uani 1 1 d . . . H7A H -0.2253 1.0205 0.3860 0.051 Uiso 1 1 calc R . . H7B H -0.1766 0.8994 0.3163 0.051 Uiso 1 1 calc R . . H7C H -0.1642 1.0582 0.2643 0.051 Uiso 1 1 calc R . . C8 C 0.0051(3) 0.7191(3) 0.47455(19) 0.0344(5) Uani 1 1 d . . . H8A H -0.0815 0.7607 0.5243 0.052 Uiso 1 1 calc R . . H8B H 0.0801 0.6424 0.5124 0.052 Uiso 1 1 calc R . . H8C H -0.0401 0.6816 0.4263 0.052 Uiso 1 1 calc R . . C9 C 0.3685(3) 0.7430(3) 0.4872(2) 0.0399(6) Uani 1 1 d . . . H9A H 0.4024 0.7928 0.5331 0.060 Uiso 1 1 calc R . . H9B H 0.4620 0.7030 0.4412 0.060 Uiso 1 1 calc R . . H9C H 0.3194 0.6668 0.5294 0.060 Uiso 1 1 calc R . . C10 C 0.4043(3) 1.0460(3) 0.3674(2) 0.0413(6) Uani 1 1 d . . . H10A H 0.3826 1.0930 0.4280 0.062 Uiso 1 1 calc R . . H10B H 0.4159 1.1158 0.3034 0.062 Uiso 1 1 calc R . . H10C H 0.5035 0.9732 0.3717 0.062 Uiso 1 1 calc R . . C11 C 0.2608(4) 0.5044(3) 0.3475(2) 0.0513(8) Uani 1 1 d . . . H11A H 0.3328 0.4178 0.3290 0.077 Uiso 1 1 calc R . . H11B H 0.1518 0.4884 0.3688 0.077 Uiso 1 1 calc R . . H11C H 0.2976 0.5303 0.4052 0.077 Uiso 1 1 calc R . . C12 C 0.2236(3) 0.5771(3) 0.1660(3) 0.0500(8) Uani 1 1 d . . . H12A H 0.3185 0.5094 0.1394 0.060 Uiso 1 1 calc R . . H12B H 0.1348 0.5266 0.1890 0.060 Uiso 1 1 calc R . . C13 C 0.1787(6) 0.6917(4) 0.0810(3) 0.0952(16) Uani 1 1 d . . . H13A H 0.2420 0.6664 0.0154 0.114 Uiso 1 1 calc R . . H13B H 0.0642 0.7012 0.0749 0.114 Uiso 1 1 calc R . . C14 C 0.2279(3) 0.9189(3) -0.00946(19) 0.0422(6) Uani 1 1 d . . . H14A H 0.1407 0.9264 -0.0499 0.063 Uiso 1 1 calc R . . H14B H 0.3305 0.8788 -0.0476 0.063 Uiso 1 1 calc R . . H14C H 0.2299 1.0131 0.0016 0.063 Uiso 1 1 calc R . . C15 C 0.4287(3) 0.9481(3) 0.16101(19) 0.0337(5) Uani 1 1 d . . . H15A H 0.4657 0.9187 0.0932 0.050 Uiso 1 1 calc R . . H15B H 0.5181 0.9218 0.2026 0.050 Uiso 1 1 calc R . . H15C H 0.3886 1.0508 0.1506 0.050 Uiso 1 1 calc R . . C16 C 0.6184(3) 0.3626(3) 0.2032(2) 0.0369(6) Uani 1 1 d . . . H16A H 0.5387 0.3548 0.1618 0.055 Uiso 1 1 calc R . . H16B H 0.5903 0.3218 0.2764 0.055 Uiso 1 1 calc R . . H16C H 0.7246 0.3113 0.1771 0.055 Uiso 1 1 calc R . . C17 C 0.7520(3) 0.5956(3) 0.2905(2) 0.0468(7) Uani 1 1 d . . . H17A H 0.7635 0.6941 0.2741 0.070 Uiso 1 1 calc R . . H17B H 0.8583 0.5326 0.2841 0.070 Uiso 1 1 calc R . . H17C H 0.6987 0.5756 0.3619 0.070 Uiso 1 1 calc R . . C18 C 0.6822(4) 0.6485(3) 0.0458(2) 0.0530(8) Uani 1 1 d . . . H18A H 0.6850 0.7478 0.0416 0.079 Uiso 1 1 calc R . . H18B H 0.6033 0.6428 0.0030 0.079 Uiso 1 1 calc R . . H18C H 0.7884 0.5968 0.0202 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02169(19) 0.0247(2) 0.0221(2) -0.00525(15) -0.00422(14) -0.00233(14) Al1 0.0301(4) 0.0266(4) 0.0301(4) -0.0065(3) -0.0036(3) -0.0004(3) O1 0.0268(8) 0.0256(8) 0.0330(9) -0.0064(6) -0.0071(7) -0.0043(6) O2 0.0242(8) 0.0904(16) 0.0272(9) -0.0210(10) -0.0064(7) 0.0057(9) N1 0.0304(10) 0.0267(10) 0.0377(11) -0.0053(9) 0.0036(9) -0.0086(8) N2 0.0358(11) 0.0384(11) 0.0261(10) -0.0085(9) -0.0031(8) -0.0060(9) C1 0.0279(11) 0.0258(11) 0.0273(11) -0.0092(9) -0.0032(9) -0.0044(9) C2 0.0210(10) 0.0291(11) 0.0265(11) -0.0120(9) -0.0028(8) -0.0024(8) C3 0.0254(10) 0.0269(11) 0.0230(10) -0.0077(9) 0.0003(8) -0.0047(8) C4 0.0257(10) 0.0332(12) 0.0220(10) -0.0100(9) -0.0052(8) -0.0028(9) C5 0.0247(10) 0.0351(12) 0.0280(11) -0.0129(9) -0.0029(9) -0.0072(9) C6 0.0409(14) 0.0257(12) 0.0473(16) -0.0044(11) -0.0048(12) -0.0046(10) C7 0.0203(10) 0.0396(14) 0.0413(14) -0.0112(11) -0.0041(10) -0.0007(9) C8 0.0342(12) 0.0340(13) 0.0326(13) -0.0053(10) 0.0031(10) -0.0083(10) C9 0.0364(13) 0.0468(15) 0.0341(13) -0.0054(11) -0.0135(11) 0.0001(11) C10 0.0344(13) 0.0526(17) 0.0470(16) -0.0211(13) -0.0045(12) -0.0181(12) C11 0.0586(18) 0.0291(13) 0.0547(18) 0.0008(12) 0.0170(14) -0.0118(12) C12 0.0407(15) 0.0403(16) 0.080(2) -0.0265(15) -0.0200(15) -0.0062(12) C13 0.206(5) 0.070(3) 0.0371(18) -0.0046(17) -0.027(3) -0.078(3) C14 0.0499(15) 0.0458(15) 0.0259(12) -0.0010(11) -0.0076(11) -0.0040(12) C15 0.0348(12) 0.0308(12) 0.0328(13) -0.0045(10) 0.0023(10) -0.0079(10) C16 0.0393(13) 0.0301(12) 0.0373(14) -0.0076(10) -0.0064(11) 0.0019(10) C17 0.0326(13) 0.0507(17) 0.0614(19) -0.0197(14) -0.0101(13) -0.0058(12) C18 0.0657(19) 0.0399(16) 0.0405(16) -0.0052(13) 0.0112(14) -0.0017(14) _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 Ti1 O2 1.8747(17) . ? Ti1 O1 2.0622(15) . ? Ti1 N2 2.114(2) . ? Ti1 C15 2.156(2) . ? Ti1 N1 2.167(2) . ? Ti1 C1 2.369(2) . ? Ti1 C2 2.381(2) . ? Ti1 C5 2.400(2) . ? Ti1 C3 2.407(2) . ? Ti1 C4 2.414(2) . ? Al1 O1 1.8975(16) . ? Al1 C18 1.972(3) . ? Al1 C16 1.982(3) . ? Al1 C17 1.983(3) . ? O1 N1 1.441(2) . ? O2 N2 1.408(3) . ? N1 C12 1.465(4) . ? N1 C11 1.468(3) . ? N2 C13 1.443(4) . ? N2 C14 1.469(3) . ? C1 C2 1.410(3) . ? C1 C5 1.417(3) . ? C1 C6 1.502(3) . ? C2 C3 1.416(3) . ? C2 C7 1.496(3) . ? C3 C4 1.419(3) . ? C3 C8 1.505(3) . ? C4 C5 1.411(3) . ? C4 C9 1.504(3) . ? C5 C10 1.501(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.450(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 O2 Ti1 O1 121.91(8) . . ? O2 Ti1 N2 40.78(7) . . ? O1 Ti1 N2 86.64(7) . . ? O2 Ti1 C15 107.63(9) . . ? O1 Ti1 C15 84.60(8) . . ? N2 Ti1 C15 85.58(9) . . ? O2 Ti1 N1 94.76(9) . . ? O1 Ti1 N1 39.74(6) . . ? N2 Ti1 N1 77.85(8) . . ? C15 Ti1 N1 121.93(8) . . ? O2 Ti1 C1 90.34(8) . . ? O1 Ti1 C1 147.60(7) . . ? N2 Ti1 C1 124.42(8) . . ? C15 Ti1 C1 88.60(9) . . ? N1 Ti1 C1 145.34(8) . . ? O2 Ti1 C2 77.60(7) . . ? O1 Ti1 C2 141.91(7) . . ? N2 Ti1 C2 118.37(8) . . ? C15 Ti1 C2 122.97(9) . . ? N1 Ti1 C2 113.78(7) . . ? C1 Ti1 C2 34.53(7) . . ? O2 Ti1 C5 124.88(8) . . ? O1 Ti1 C5 113.19(7) . . ? N2 Ti1 C5 152.36(8) . . ? C15 Ti1 C5 77.78(9) . . ? N1 Ti1 C5 129.74(8) . . ? C1 Ti1 C5 34.57(7) . . ? C2 Ti1 C5 57.11(7) . . ? O2 Ti1 C3 102.33(7) . . ? O1 Ti1 C3 107.74(7) . . ? N2 Ti1 C3 137.50(8) . . ? C15 Ti1 C3 134.33(9) . . ? N1 Ti1 C3 88.24(8) . . ? C1 Ti1 C3 57.23(7) . . ? C2 Ti1 C3 34.40(7) . . ? C5 Ti1 C3 56.77(8) . . ? O2 Ti1 C4 134.12(8) . . ? O1 Ti1 C4 93.63(7) . . ? N2 Ti1 C4 171.03(8) . . ? C15 Ti1 C4 103.38(9) . . ? N1 Ti1 C4 96.65(8) . . ? C1 Ti1 C4 57.27(8) . . ? C2 Ti1 C4 57.15(7) . . ? C5 Ti1 C4 34.09(8) . . ? C3 Ti1 C4 34.24(7) . . ? O1 Al1 C18 108.89(10) . . ? O1 Al1 C16 108.27(9) . . ? C18 Al1 C16 110.42(12) . . ? O1 Al1 C17 102.27(10) . . ? C18 Al1 C17 113.49(14) . . ? C16 Al1 C17 113.01(12) . . ? N1 O1 Al1 130.78(13) . . ? N1 O1 Ti1 74.05(10) . . ? Al1 O1 Ti1 150.82(9) . . ? N2 O2 Ti1 78.76(11) . . ? O1 N1 C12 112.92(19) . . ? O1 N1 C11 109.31(19) . . ? C12 N1 C11 110.6(2) . . ? O1 N1 Ti1 66.22(9) . . ? C12 N1 Ti1 114.01(16) . . ? C11 N1 Ti1 132.76(19) . . ? O2 N2 C13 111.5(3) . . ? O2 N2 C14 110.85(19) . . ? C13 N2 C14 112.2(2) . . ? O2 N2 Ti1 60.45(10) . . ? C13 N2 Ti1 116.33(17) . . ? C14 N2 Ti1 130.19(18) . . ? C2 C1 C5 107.91(19) . . ? C2 C1 C6 125.3(2) . . ? C5 C1 C6 126.8(2) . . ? C2 C1 Ti1 73.23(13) . . ? C5 C1 Ti1 73.94(13) . . ? C6 C1 Ti1 119.15(16) . . ? C1 C2 C3 108.09(19) . . ? C1 C2 C7 126.8(2) . . ? C3 C2 C7 125.0(2) . . ? C1 C2 Ti1 72.24(12) . . ? C3 C2 Ti1 73.78(12) . . ? C7 C2 Ti1 122.52(16) . . ? C2 C3 C4 108.02(19) . . ? C2 C3 C8 123.1(2) . . ? C4 C3 C8 128.0(2) . . ? C2 C3 Ti1 71.82(12) . . ? C4 C3 Ti1 73.17(12) . . ? C8 C3 Ti1 128.91(16) . . ? C5 C4 C3 107.68(19) . . ? C5 C4 C9 125.2(2) . . ? C3 C4 C9 127.0(2) . . ? C5 C4 Ti1 72.41(13) . . ? C3 C4 Ti1 72.59(12) . . ? C9 C4 Ti1 124.25(16) . . ? C4 C5 C1 108.29(19) . . ? C4 C5 C10 125.2(2) . . ? C1 C5 C10 125.8(2) . . ? C4 C5 Ti1 73.50(13) . . ? C1 C5 Ti1 71.49(13) . . ? C10 C5 Ti1 128.09(16) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N1 115.3(2) . . ? C13 C12 H12A 108.4 . . ? N1 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? N1 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? N2 C13 C12 114.8(3) . . ? N2 C13 H13A 108.6 . . ? C12 C13 H13A 108.6 . . ? N2 C13 H13B 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Ti1 C15 H15A 109.5 . . ? Ti1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Ti1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Al1 C16 H16A 109.5 . . ? Al1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Al1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Al1 C17 H17A 109.5 . . ? Al1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Al1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Al1 C18 H18A 109.5 . . ? Al1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.418 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.074