Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_General #============================================================================== _journal_coden_Cambridge 182 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Robert M. Waymouth' _publ_contact_author_address ; Prof Robert Waymouth Department of Chemistry Stanford University Mail Code 5080 Stanford CA 94305-5080 UNITED STATES OF AMERICA ; _publ_contact_author_email 'waymouth@stanford.edu' _publ_contact_author_fax '650-736-2262' _publ_contact_author_phone '650-723-4515' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ChemComm' _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and molecular structure of titanium complexes containg a reduced TEMPO radical ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name 'Mahesh K. Mahanthappa' 'Kuo-Wei Huang' 'Adam P. Cole' 'Robert M. Waymouth' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 2.00. MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data__CpTiCl2(TEMPO) _database_code_CSD 178085 _audit_creation_date '2001-08-29' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H23 Cl2 N O Ti ' _chemical_formula_moiety 'C14 H23 Cl2 N O Ti ' _chemical_formula_weight 340.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' #------------------------------------------------------------------------------ _cell_length_a 7.83(0) _cell_length_b 12.02(0) _cell_length_c 17.93(0) _cell_angle_alpha 90 _cell_angle_beta 100.29(0) _cell_angle_gamma 90 _cell_volume 1661.3(0) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 273.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type empirical #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 4833 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 24.69 _diffrn_measured_fraction_theta_max 0.8547 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.8547 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2550 _reflns_number_gt 1544 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.0880 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2403 _refine_ls_number_parameters 195 _refine_ls_goodness_of_fit_ref 1.344 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.69 _refine_diff_density_min -0.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # 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 Ti1 Ti 0.959(0) 0.0880(1) 0.3499(0) 0.021(0) Uani 1.00 1 d . . . Cl1 Cl 0.892(0) -0.097(0) 0.3436(1) 0.031(0) Uani 1.00 1 d . . . Cl2 Cl 1.240(0) 0.093(0) 0.4116(1) 0.034(0) Uani 1.00 1 d . . . O1 O 0.982(0) 0.118(0) 0.257(0) 0.022(1) Uani 1.00 1 d . . . N1 N 0.949(0) 0.177(0) 0.187(0) 0.02(0) Uani 1.00 1 d . . . C1 C 0.882(1) 0.176(1) 0.457(0) 0.03(0) Uani 1.00 1 d . . . C2 C 0.746(1) 0.104(1) 0.429(0) 0.04(0) Uani 1.00 1 d . . . C3 C 0.676(1) 0.141(1) 0.355(0) 0.04(0) Uani 1.00 1 d . . . C4 C 0.767(1) 0.235(1) 0.340(0) 0.04(0) Uani 1.00 1 d . . . C5 C 0.897(1) 0.256(0) 0.403(0) 0.04(0) Uani 1.00 1 d . . . C6 C 0.876(1) 0.094(0) 0.128(0) 0.02(0) Uani 1.00 1 d . . . C7 C 0.853(1) 0.156(0) 0.051(0) 0.03(0) Uani 1.00 1 d . . . C8 C 1.021(1) 0.211(0) 0.038(0) 0.03(0) Uani 1.00 1 d . . . C9 C 1.076(1) 0.295(0) 0.102(0) 0.03(0) Uani 1.00 1 d . . . C10 C 1.110(1) 0.241(0) 0.181(0) 0.02(0) Uani 1.00 1 d . . . C11 C 0.694(1) 0.065(0) 0.143(0) 0.03(0) Uani 1.00 1 d . . . C12 C 0.979(1) -0.013(0) 0.127(0) 0.03(0) Uani 1.00 1 d . . . C13 C 1.125(1) 0.334(0) 0.240(0) 0.04(0) Uani 1.00 1 d . . . C14 C 1.277(1) 0.173(0) 0.193(0) 0.04(0) Uani 1.00 1 d . . . H1 H 0.953(1) 0.171(1) 0.506(0) 0.04(0) Uiso 1.00 1 c . . . H2 H 0.709(1) 0.042(1) 0.454(0) 0.05(0) Uiso 1.00 1 c . . . H3 H 0.582(1) 0.108(1) 0.322(0) 0.04(0) Uiso 1.00 1 c . . . H4 H 0.745(1) 0.277(1) 0.295(0) 0.05(0) Uiso 1.00 1 c . . . H5 H 0.981(1) 0.315(0) 0.407(0) 0.04(0) Uiso 1.00 1 c . . . H6 H 0.767(1) 0.212(0) 0.050(0) 0.03(0) Uiso 1.00 1 c . . . H7 H 0.817(1) 0.105(0) 0.011(0) 0.03(0) Uiso 1.00 1 c . . . H8 H 1.002(1) 0.248(0) -0.009(0) 0.04(0) Uiso 1.00 1 c . . . H9 H 1.109(1) 0.156(0) 0.039(0) 0.04(0) Uiso 1.00 1 c . . . H10 H 0.987(1) 0.349(0) 0.100(0) 0.04(0) Uiso 1.00 1 c . . . H11 H 1.180(1) 0.330(0) 0.094(0) 0.04(0) Uiso 1.00 1 c . . . H12 H 0.641(1) 0.013(0) 0.106(0) 0.04(0) Uiso 1.00 1 c . . . H13 H 0.625(1) 0.131(0) 0.140(0) 0.04(0) Uiso 1.00 1 c . . . H14 H 0.703(1) 0.034(0) 0.192(0) 0.04(0) Uiso 1.00 1 c . . . H15 H 0.988(1) -0.049(0) 0.174(0) 0.04(0) Uiso 1.00 1 c . . . H16 H 0.921(1) -0.060(0) 0.087(0) 0.04(0) Uiso 1.00 1 c . . . H17 H 1.092(1) 0.004(0) 0.117(0) 0.04(0) Uiso 1.00 1 c . . . H18 H 1.134(1) 0.302(0) 0.289(0) 0.05(0) Uiso 1.00 1 c . . . H19 H 1.026(1) 0.380(0) 0.230(0) 0.05(0) Uiso 1.00 1 c . . . H20 H 1.226(1) 0.377(0) 0.238(0) 0.05(0) Uiso 1.00 1 c . . . H21 H 1.295(1) 0.141(0) 0.243(0) 0.04(0) Uiso 1.00 1 c . . . H22 H 1.268(1) 0.115(0) 0.157(0) 0.04(0) Uiso 1.00 1 c . . . H23 H 1.372(1) 0.220(0) 0.189(0) 0.04(0) Uiso 1.00 1 c . . . 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 Ti1 0.021(1) 0.030(1) 0.013(1) 0.002(1) 0.007(0) 0.001(1) Cl1 0.038(1) 0.031(1) 0.026(1) -0.004(1) 0.009(1) 0.001(1) Cl2 0.025(1) 0.05(0) 0.029(1) 0.002(1) 0.001(1) -0.002(1) O1 0.02(0) 0.03(0) 0.01(0) 0.00(0) 0.01(0) 0.01(0) N1 0.02(0) 0.02(0) 0.02(0) 0.00(0) 0.00(0) 0.01(0) C1 0.04(0) 0.04(0) 0.02(0) 0.01(0) 0.01(0) -0.01(0) C2 0.04(0) 0.05(0) 0.03(0) 0.02(0) 0.03(0) 0.01(0) C3 0.02(0) 0.06(1) 0.03(0) 0.01(0) 0.01(0) -0.01(0) C4 0.05(0) 0.04(1) 0.02(0) 0.02(0) 0.02(0) 0.01(0) C5 0.04(0) 0.03(0) 0.05(0) 0.00(0) 0.02(0) -0.01(0) C6 0.03(0) 0.03(0) 0.01(0) -0.00(0) 0.01(0) -0.00(0) C7 0.03(0) 0.04(0) 0.02(0) 0.00(0) 0.00(0) 0.00(0) C8 0.04(0) 0.05(0) 0.02(0) -0.00(0) 0.01(0) 0.01(0) C9 0.03(0) 0.03(0) 0.03(0) -0.01(0) 0.01(0) 0.01(0) C10 0.02(0) 0.03(0) 0.02(0) -0.01(0) 0.01(0) 0.00(0) C11 0.03(0) 0.05(0) 0.03(0) -0.01(0) 0.00(0) -0.01(0) C12 0.04(0) 0.03(0) 0.02(0) -0.00(0) 0.01(0) -0.01(0) C13 0.04(0) 0.05(0) 0.03(0) -0.02(0) 0.01(0) -0.00(0) C14 0.02(0) 0.05(0) 0.04(0) -0.01(0) 0.01(0) 0.00(0) #============================================================================== _computing_data_collection 'Unknown' _computing_cell_refinement 'Unknown' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR92' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.2795(16) yes Ti1 . Cl2 . 2.2770(13) yes Ti1 . O1 . 1.753(3) yes Ti1 . C1 . 2.366(5) yes Ti1 . C2 . 2.376(4) yes Ti1 . C3 . 2.327(4) yes Ti1 . C4 . 2.305(5) yes Ti1 . C5 . 2.320(5) yes O1 . N1 . 1.412(4) yes N1 . C6 . 1.486(5) yes N1 . C10 . 1.502(5) yes C1 . C2 . 1.397(6) yes C1 . C5 . 1.394(6) yes C1 . H1 . 0.9500(1) no C2 . C3 . 1.406(6) yes C2 . H2 . 0.95002(9) no C3 . C4 . 1.385(6) yes C3 . H3 . 0.95003(8) no C4 . C5 . 1.400(7) yes C4 . H4 . 0.9500(1) no C5 . H5 . 0.94997(9) no C6 . C7 . 1.548(6) yes C6 . C11 . 1.540(5) yes C6 . C12 . 1.520(6) yes C7 . C8 . 1.524(6) yes C7 . H6 . 0.94998(9) no C7 . H7 . 0.94999(9) no C8 . C9 . 1.521(6) yes C8 . H8 . 0.9500(1) no C8 . H9 . 0.95000(9) no C9 . C10 . 1.537(6) yes C9 . H10 . 0.95000(9) no C9 . H11 . 0.9500(1) no C10 . C13 . 1.539(6) yes C10 . C14 . 1.526(6) yes C11 . H12 . 0.95003(8) no C11 . H13 . 0.9500(1) no C11 . H14 . 0.94994(11) no C12 . H15 . 0.9500(1) no C12 . H16 . 0.94998(8) no C12 . H17 . 0.94998(12) no C13 . H18 . 0.95000(11) no C13 . H19 . 0.9500(1) no C13 . H20 . 0.9500(1) no C14 . H21 . 0.95002(11) no C14 . H22 . 0.94997(9) no C14 . H23 . 0.94999(9) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl2 . 104.10(6) yes Cl1 . Ti1 . O1 . 102.58(11) yes Cl2 . Ti1 . O1 . 101.8(1) yes Cl1 . Ti1 . C1 . 112.71(14) yes Cl2 . Ti1 . C1 . 87.54(12) yes O1 . Ti1 . C1 . 140.09(18) yes Cl1 . Ti1 . C2 . 85.90(15) yes Cl2 . Ti1 . C2 . 115.33(13) yes O1 . Ti1 . C2 . 138.76(15) yes C1 . Ti1 . C2 . 34.26(16) yes Cl1 . Ti1 . C3 . 93.25(15) yes Cl2 . Ti1 . C3 . 144.81(13) yes O1 . Ti1 . C3 . 104.01(16) yes C1 . Ti1 . C3 . 57.39(17) yes C2 . Ti1 . C3 . 34.78(15) yes Cl1 . Ti1 . C4 . 126.88(15) yes Cl2 . Ti1 . C4 . 125.25(15) yes O1 . Ti1 . C4 . 86.77(16) yes C1 . Ti1 . C4 . 57.48(17) yes C2 . Ti1 . C4 . 57.72(18) yes Cl1 . Ti1 . C5 . 143.74(14) yes Cl2 . Ti1 . C5 . 91.86(13) yes O1 . Ti1 . C5 . 105.74(17) yes C1 . Ti1 . C5 . 34.60(16) yes C2 . Ti1 . C5 . 57.86(18) yes C3 . Ti1 . C4 . 34.78(16) yes C3 . Ti1 . C5 . 58.28(18) yes C4 . Ti1 . C5 . 35.23(16) yes Ti1 . O1 . N1 . 155.7(3) yes O1 . N1 . C6 . 106.8(3) yes O1 . N1 . C10 . 107.2(3) yes C6 . N1 . C10 . 120.3(3) yes Ti1 . C1 . C2 . 73.3(3) yes Ti1 . C1 . C5 . 70.9(3) yes C2 . C1 . C5 . 109.0(5) yes Ti1 . C1 . H1 . 121.99(12) no C2 . C1 . H1 . 125.5(3) no C5 . C1 . H1 . 125.5(3) no Ti1 . C2 . C1 . 72.5(3) yes Ti1 . C2 . C3 . 70.7(3) yes C1 . C2 . C3 . 107.0(5) yes Ti1 . C2 . H2 . 122.07(14) no C1 . C2 . H2 . 126.5(3) no C3 . C2 . H2 . 126.5(3) no Ti1 . C3 . C2 . 74.5(3) yes Ti1 . C3 . C4 . 71.7(3) yes C2 . C3 . C4 . 108.1(5) yes Ti1 . C3 . H3 . 119.68(13) no C2 . C3 . H3 . 125.9(3) no C4 . C3 . H3 . 125.9(3) no Ti1 . C4 . C3 . 73.5(3) yes Ti1 . C4 . C5 . 73.0(3) yes C3 . C4 . C5 . 108.7(5) yes Ti1 . C4 . H4 . 119.67(12) no C3 . C4 . H4 . 125.6(3) no C5 . C4 . H4 . 125.6(3) no Ti1 . C5 . C1 . 74.5(3) yes Ti1 . C5 . C4 . 71.8(3) yes C1 . C5 . C4 . 107.1(5) yes Ti1 . C5 . H5 . 119.17(13) no C1 . C5 . H5 . 126.5(3) no C4 . C5 . H5 . 126.5(3) no N1 . C6 . C7 . 106.5(4) yes N1 . C6 . C11 . 105.9(3) yes C7 . C6 . C11 . 107.6(4) yes N1 . C6 . C12 . 116.0(4) yes C7 . C6 . C12 . 111.7(4) yes C11 . C6 . C12 . 108.7(4) yes C6 . C7 . C8 . 112.2(4) yes C6 . C7 . H6 . 108.7(2) no C8 . C7 . H6 . 108.7(3) no C6 . C7 . H7 . 108.8(3) no C8 . C7 . H7 . 108.9(3) no H6 . C7 . H7 . 109.464(9) no C7 . C8 . C9 . 108.0(4) yes C7 . C8 . H8 . 109.8(2) no C9 . C8 . H8 . 109.8(3) no C7 . C8 . H9 . 109.8(3) no C9 . C8 . H9 . 109.9(3) no H8 . C8 . H9 . 109.460(9) no C8 . C9 . C10 . 112.9(4) yes C8 . C9 . H10 . 108.6(3) no C10 . C9 . H10 . 108.6(3) no C8 . C9 . H11 . 108.6(2) no C10 . C9 . H11 . 108.6(2) no H10 . C9 . H11 . 109.457(12) no N1 . C10 . C9 . 106.3(3) yes N1 . C10 . C13 . 106.3(4) yes C9 . C10 . C13 . 108.1(4) yes N1 . C10 . C14 . 115.2(4) yes C9 . C10 . C14 . 111.5(4) yes C13 . C10 . C14 . 109.0(4) yes C6 . C11 . H12 . 109.5(2) no C6 . C11 . H13 . 109.5(3) no H12 . C11 . H13 . 109.475(9) no C6 . C11 . H14 . 109.5(2) no H12 . C11 . H14 . 109.472(11) no H13 . C11 . H14 . 109.470(4) no C6 . C12 . H15 . 109.5(2) no C6 . C12 . H16 . 109.5(2) no H15 . C12 . H16 . 109.474(7) no C6 . C12 . H17 . 109.5(2) no H15 . C12 . H17 . 109.467(4) no H16 . C12 . H17 . 109.48(1) no C10 . C13 . H18 . 109.5(3) no C10 . C13 . H19 . 109.5(3) no H18 . C13 . H19 . 109.471(6) no C10 . C13 . H20 . 109.5(2) no H18 . C13 . H20 . 109.478(6) no H19 . C13 . H20 . 109.472(11) no C10 . C14 . H21 . 109.5(2) no C10 . C14 . H22 . 109.5(3) no H21 . C14 . H22 . 109.473(7) no C10 . C14 . H23 . 109.5(3) no H21 . C14 . H23 . 109.467(6) no H22 . C14 . H23 . 109.474(7) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl1 . Ti1 . O1 . N1 . 125.7(1) yes Cl2 . Ti1 . O1 . N1 . -126.8(1) yes C1 . Ti1 . O1 . N1 . -26.4(2) yes C2 . Ti1 . O1 . N1 . 27.4(2) yes C3 . Ti1 . O1 . N1 . 29.0(1) yes C4 . Ti1 . O1 . N1 . -1.5(1) yes C5 . Ti1 . O1 . N1 . -31.5(1) yes Cl1 . Ti1 . C1 . C2 . -41.2(1) yes Cl1 . Ti1 . C1 . C5 . -158.9(1) yes Cl2 . Ti1 . C1 . C2 . -145.5(1) yes Cl2 . Ti1 . C1 . C5 . 96.9(1) yes O1 . Ti1 . C1 . C2 . 109.1(1) yes O1 . Ti1 . C1 . C5 . -8.6(1) yes C2 . Ti1 . C1 . C2 . 0.0(0) yes C2 . Ti1 . C1 . C5 . -117.7(1) yes C3 . Ti1 . C1 . C2 . 37.5(1) yes C3 . Ti1 . C1 . C5 . -80.1(1) yes C4 . Ti1 . C1 . C2 . 79.1(1) yes C4 . Ti1 . C1 . C5 . -38.6(1) yes C5 . Ti1 . C1 . C2 . 117.7(1) yes C5 . Ti1 . C1 . C5 . 0.0(0) yes Cl1 . Ti1 . C2 . C1 . 142.5(1) yes Cl1 . Ti1 . C2 . C3 . -101.7(1) yes Cl2 . Ti1 . C2 . C1 . 38.8(1) yes Cl2 . Ti1 . C2 . C3 . 154.6(0) yes O1 . Ti1 . C2 . C1 . -113.1(1) yes O1 . Ti1 . C2 . C3 . 2.7(1) yes C1 . Ti1 . C2 . C1 . 0.0(0) yes C1 . Ti1 . C2 . C3 . 115.8(1) yes C3 . Ti1 . C2 . C1 . -115.8(1) yes C3 . Ti1 . C2 . C3 . 0.0(0) yes C4 . Ti1 . C2 . C1 . -78.4(1) yes C4 . Ti1 . C2 . C3 . 37.5(1) yes C5 . Ti1 . C2 . C1 . -36.4(1) yes C5 . Ti1 . C2 . C3 . 79.4(1) yes Cl1 . Ti1 . C3 . C2 . 78.0(1) yes Cl1 . Ti1 . C3 . C4 . -166.4(1) yes Cl2 . Ti1 . C3 . C2 . -42.2(1) yes Cl2 . Ti1 . C3 . C4 . 73.4(1) yes O1 . Ti1 . C3 . C2 . -178.1(1) yes O1 . Ti1 . C3 . C4 . -62.6(1) yes C1 . Ti1 . C3 . C2 . -37.0(1) yes C1 . Ti1 . C3 . C4 . 78.6(1) yes C2 . Ti1 . C3 . C2 . 0.0(0) yes C2 . Ti1 . C3 . C4 . 115.6(1) yes C4 . Ti1 . C3 . C2 . -115.6(1) yes C4 . Ti1 . C3 . C4 . 0.0(0) yes C5 . Ti1 . C3 . C2 . -78.1(1) yes C5 . Ti1 . C3 . C4 . 37.5(1) yes Cl1 . Ti1 . C4 . C3 . 17.1(1) yes Cl1 . Ti1 . C4 . C5 . 133.3(1) yes Cl2 . Ti1 . C4 . C3 . -137.5(1) yes Cl2 . Ti1 . C4 . C5 . -21.3(1) yes O1 . Ti1 . C4 . C3 . 120.4(1) yes O1 . Ti1 . C4 . C5 . -123.4(1) yes C1 . Ti1 . C4 . C3 . -78.3(1) yes C1 . Ti1 . C4 . C5 . 37.9(1) yes C2 . Ti1 . C4 . C3 . -37.5(1) yes C2 . Ti1 . C4 . C5 . 78.7(1) yes C3 . Ti1 . C4 . C3 . 0.0(0) yes C3 . Ti1 . C4 . C5 . 116.2(1) yes C5 . Ti1 . C4 . C3 . -116.2(1) yes C5 . Ti1 . C4 . C5 . 0.0(0) yes Cl1 . Ti1 . C5 . C1 . 34.2(1) yes Cl1 . Ti1 . C5 . C4 . -80.1(1) yes Cl2 . Ti1 . C5 . C1 . -83.0(1) yes Cl2 . Ti1 . C5 . C4 . 162.7(1) yes O1 . Ti1 . C5 . C1 . 174.3(1) yes O1 . Ti1 . C5 . C4 . 60.0(1) yes C1 . Ti1 . C5 . C1 . 0.0(0) yes C1 . Ti1 . C5 . C4 . -114.3(1) yes C2 . Ti1 . C5 . C1 . 36.1(1) yes C2 . Ti1 . C5 . C4 . -78.2(1) yes C3 . Ti1 . C5 . C1 . 77.3(1) yes C3 . Ti1 . C5 . C4 . -37.0(1) yes C4 . Ti1 . C5 . C1 . 114.3(1) yes C4 . Ti1 . C5 . C4 . 0.0(0) yes Ti1 . O1 . N1 . C6 . -118.5(1) yes Ti1 . O1 . N1 . C10 . 111.4(1) yes O1 . N1 . C6 . C7 . -175.6(0) yes O1 . N1 . C6 . C11 . 70.0(1) yes O1 . N1 . C6 . C12 . -50.6(1) yes C10 . N1 . C6 . C7 . -53.4(1) yes C10 . N1 . C6 . C11 . -167.7(1) yes C10 . N1 . C6 . C12 . 71.6(1) yes O1 . N1 . C10 . C9 . 175.2(0) yes O1 . N1 . C10 . C13 . -69.8(1) yes O1 . N1 . C10 . C14 . 51.1(1) yes C6 . N1 . C10 . C9 . 53.1(1) yes C6 . N1 . C10 . C13 . 168.2(1) yes C6 . N1 . C10 . C14 . -71.0(1) yes Ti1 . C1 . C2 . Ti1 . 0.0(1) yes Ti1 . C1 . C2 . C3 . -62.7(1) yes C5 . C1 . C2 . Ti1 . 62.3(1) yes C5 . C1 . C2 . C3 . -0.4(1) yes Ti1 . C1 . C5 . Ti1 . 0.0(1) yes Ti1 . C1 . C5 . C4 . 64.9(1) yes C2 . C1 . C5 . Ti1 . -63.8(1) yes C2 . C1 . C5 . C4 . 1.1(1) yes Ti1 . C2 . C3 . Ti1 . 0.0(1) yes Ti1 . C2 . C3 . C4 . -64.3(1) yes C1 . C2 . C3 . Ti1 . 63.8(1) yes C1 . C2 . C3 . C4 . -0.5(1) yes Ti1 . C3 . C4 . Ti1 . 0.0(1) yes Ti1 . C3 . C4 . C5 . -65.0(1) yes C2 . C3 . C4 . Ti1 . 66.1(1) yes C2 . C3 . C4 . C5 . 1.2(1) yes Ti1 . C4 . C5 . Ti1 . 0.0(1) yes Ti1 . C4 . C5 . C1 . -66.7(1) yes C3 . C4 . C5 . Ti1 . 65.3(1) yes C3 . C4 . C5 . C1 . -1.4(1) yes N1 . C6 . C7 . C8 . 54.4(1) yes C11 . C6 . C7 . C8 . 167.6(1) yes C12 . C6 . C7 . C8 . -73.1(1) yes C6 . C7 . C8 . C9 . -60.2(1) yes C7 . C8 . C9 . C10 . 60.4(1) yes C8 . C9 . C10 . N1 . -54.0(1) yes C8 . C9 . C10 . C13 . -167.8(1) yes C8 . C9 . C10 . C14 . 72.3(1) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Ti1 . Cl1 . 2.2795(16) yes Ti1 . Cl2 . 2.2770(13) yes Ti1 . O1 . 1.753(3) yes Ti1 . C1 . 2.366(5) yes Ti1 . C2 . 2.376(4) yes Ti1 . C3 . 2.327(4) yes Ti1 . C4 . 2.305(5) yes Ti1 . C5 . 2.320(5) yes Ti1 . H1 . 2.980(5) no Ti1 . H2 . 2.991(5) no Ti1 . H3 . 2.917(5) no Ti1 . H4 . 2.895(5) no Ti1 . H5 . 2.904(5) no Cl1 . H1 2_756 2.896(5) no Cl1 . H4 3_645 2.939(5) no Cl2 . H2 2_756 2.874(5) no Cl2 . H8 4_555 2.971(5) no O1 . N1 . 1.412(4) yes O1 . C4 . 2.816(5) yes O1 . C6 . 2.327(5) yes O1 . C10 . 2.345(5) yes O1 . C11 . 2.831(5) yes O1 . C12 . 2.811(5) yes O1 . C13 . 2.855(6) yes O1 . C14 . 2.826(5) yes O1 . H4 . 2.832(5) no O1 . H14 . 2.497(5) no O1 . H15 . 2.506(5) no O1 . H18 . 2.523(6) no O1 . H21 . 2.521(5) no N1 . C6 . 1.486(5) yes N1 . C7 . 2.432(5) yes N1 . C8 . 2.858(6) yes N1 . C9 . 2.431(6) yes N1 . C10 . 1.502(5) yes N1 . C11 . 2.416(5) yes N1 . C12 . 2.549(6) yes N1 . C13 . 2.433(6) yes N1 . C14 . 2.557(5) yes N1 . H4 . 2.972(6) no N1 . H6 . 2.640(5) no N1 . H10 . 2.639(6) no N1 . H13 . 2.585(5) no N1 . H14 . 2.588(6) no N1 . H15 . 2.747(6) no N1 . H17 . 2.759(6) no N1 . H18 . 2.605(6) no N1 . H19 . 2.601(6) no N1 . H21 . 2.752(5) no N1 . H22 . 2.759(5) no C1 . C2 . 1.397(6) yes C1 . C3 . 2.254(7) yes C1 . C4 . 2.246(7) yes C1 . C5 . 1.394(6) yes C1 . H1 . 0.9500(1) no C1 . H2 . 2.105(7) no C1 . H5 . 2.102(7) no C2 . C3 . 1.406(6) yes C2 . C4 . 2.260(7) yes C2 . C5 . 2.272(7) yes C2 . H1 . 2.096(6) no C2 . H2 . 0.95002(9) no C2 . H3 . 2.109(6) no C2 . H8 4_455 2.969(7) no C3 . C4 . 1.385(6) yes C3 . C5 . 2.263(7) yes C3 . H2 . 2.114(7) no C3 . H3 . 0.95003(8) no C3 . H4 . 2.086(7) no C4 . C5 . 1.400(7) yes C4 . H3 . 2.089(7) no C4 . H4 . 0.9500(1) no C4 . H5 . 2.108(7) no C5 . H1 . 2.094(7) no C5 . H4 . 2.100(7) no C5 . H5 . 0.94997(9) no C6 . C7 . 1.548(6) yes C6 . C8 . 2.550(6) yes C6 . C9 . 2.957(7) yes C6 . C10 . 2.591(6) yes C6 . C11 . 1.540(5) yes C6 . C12 . 1.520(6) yes C6 . H6 . 2.060(6) no C6 . H7 . 2.061(6) no C6 . H9 . 2.732(6) no C6 . H12 . 2.061(6) no C6 . H13 . 2.061(6) no C6 . H14 . 2.061(6) no C6 . H15 . 2.043(6) no C6 . H16 . 2.043(6) no C6 . H17 . 2.043(6) no C7 . C8 . 1.524(6) yes C7 . C9 . 2.464(7) yes C7 . C10 . 2.964(6) yes C7 . C11 . 2.492(6) yes C7 . C12 . 2.539(7) yes C7 . H6 . 0.94998(9) no C7 . H7 . 0.94999(9) no C7 . H8 . 2.051(6) no C7 . H9 . 2.050(6) no C7 . H10 . 2.625(7) no C7 . H12 . 2.705(6) no C7 . H13 . 2.611(6) no C7 . H16 . 2.709(7) no C7 . H17 . 2.728(6) no C8 . C9 . 1.521(6) yes C8 . C10 . 2.548(6) yes C8 . H6 . 2.038(6) no C8 . H7 . 2.040(6) no C8 . H8 . 0.9500(1) no C8 . H9 . 0.95000(9) no C8 . H10 . 2.035(7) no C8 . H11 . 2.035(6) no C8 . H16 2_755 2.992(6) no C8 . H17 . 2.867(7) no C8 . H22 . 2.855(7) no C9 . C10 . 1.537(6) yes C9 . C13 . 2.490(6) yes C9 . C14 . 2.532(7) yes C9 . H6 . 2.626(6) no C9 . H8 . 2.049(6) no C9 . H9 . 2.049(7) no C9 . H10 . 0.95000(9) no C9 . H11 . 0.9500(1) no C9 . H19 . 2.617(7) no C9 . H20 . 2.705(6) no C9 . H22 . 2.718(7) no C9 . H23 . 2.708(6) no C10 . C13 . 1.539(6) yes C10 . C14 . 1.526(6) yes C10 . H9 . 2.734(6) no C10 . H10 . 2.049(6) no C10 . H11 . 2.048(6) no C10 . H18 . 2.060(6) no C10 . H19 . 2.061(6) no C10 . H20 . 2.060(6) no C10 . H21 . 2.049(6) no C10 . H22 . 2.049(6) no C10 . H23 . 2.049(6) no C11 . C12 . 2.486(6) yes C11 . H6 . 2.559(6) no C11 . H7 . 2.743(6) no C11 . H12 . 0.95003(8) no C11 . H13 . 0.9500(1) no C11 . H14 . 0.94994(11) no C11 . H15 . 2.656(6) no C11 . H16 . 2.656(6) no C12 . H7 . 2.632(6) no C12 . H9 . 2.865(7) no C12 . H12 . 2.624(6) no C12 . H14 . 2.699(6) no C12 . H15 . 0.9500(1) no C12 . H16 . 0.94998(8) no C12 . H17 . 0.94998(12) no C12 . H22 . 2.710(6) no C13 . C14 . 2.496(7) yes C13 . H10 . 2.558(6) no C13 . H11 . 2.738(6) no C13 . H18 . 0.95000(11) no C13 . H19 . 0.9500(1) no C13 . H20 . 0.9500(1) no C13 . H21 . 2.667(7) no C13 . H23 . 2.668(6) no C14 . H9 . 2.856(7) no C14 . H11 . 2.624(7) no C14 . H17 . 2.712(7) no C14 . H18 . 2.704(7) no C14 . H20 . 2.638(7) no C14 . H21 . 0.95002(11) no C14 . H22 . 0.94997(9) no C14 . H23 . 0.94999(9) no H1 . H2 . 2.513(6) no H1 . H5 . 2.510(6) no H1 . H6 4_555 2.822(7) no H1 . H11 4_455 2.872(7) no H2 . H3 . 2.529(6) no H2 . H10 3_645 2.854(8) no H2 . H11 4_455 2.983(7) no H3 . H4 . 2.496(6) no H3 . H14 . 2.803(6) no H3 . H19 3_645 2.969(8) no H3 . H21 1_455 2.467(6) no H3 . H23 1_455 2.966(7) no H4 . H5 . 2.518(6) no H4 . H15 3_655 2.892(7) no H4 . H19 . 2.931(7) no H5 . H12 3_655 2.560(7) no H5 . H18 . 2.616(7) no H6 . H7 . 1.55125(15) no H6 . H8 . 2.329(6) no H6 . H9 . 2.800(6) no H6 . H10 . 2.431(7) no H6 . H12 . 2.844(7) no H6 . H13 . 2.322(6) no H7 . H8 . 2.330(6) no H7 . H9 . 2.336(6) no H7 . H12 . 2.617(6) no H7 . H13 . 2.976(6) no H7 . H16 . 2.458(7) no H7 . H16 2_755 2.991(6) no H7 . H17 . 2.870(6) no H7 . H17 2_755 2.852(6) no H8 . H9 . 1.55123(13) no H8 . H10 . 2.325(6) no H8 . H11 . 2.323(6) no H8 . H16 2_755 2.785(7) no H9 . H10 . 2.798(7) no H9 . H11 . 2.333(6) no H9 . H16 2_755 2.517(6) no H9 . H17 . 2.325(7) no H9 . H22 . 2.312(7) no H10 . H11 . 1.5512(2) no H10 . H19 . 2.327(6) no H10 . H20 . 2.843(6) no H11 . H19 . 2.979(7) no H11 . H20 . 2.613(6) no H11 . H22 . 2.861(7) no H11 . H23 . 2.455(7) no H12 . H13 . 1.55142(18) no H12 . H14 . 1.55133(19) no H12 . H15 . 2.870(6) no H12 . H16 . 2.441(6) no H13 . H14 . 1.55130(14) no H13 . H22 1_455 2.872(6) no H13 . H23 1_455 2.542(6) no H14 . H15 . 2.521(6) no H14 . H16 . 2.979(6) no H15 . H16 . 1.5514(2) no H15 . H17 . 1.55132(13) no H15 . H20 3_745 2.651(6) no H16 . H17 . 1.55136(16) no H17 . H22 . 1.957(7) no H18 . H19 . 1.55134(12) no H18 . H20 . 1.55145(12) no H18 . H21 . 2.528(7) no H18 . H23 . 2.985(6) no H19 . H20 . 1.5514(2) no H20 . H21 . 2.886(7) no H20 . H23 . 2.459(7) no H21 . H22 . 1.5513(2) no H21 . H23 . 1.55131(13) no H22 . H23 . 1.55133(15) no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data__TEMPOTiCl3 _database_code_CSD 178086 _audit_creation_date '2001-09-07' _audit_creation_method 'by CrystalStructure v2.00' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C9 H18 Cl3 N O Ti ' _chemical_formula_moiety 'C9 H18 Cl3 N O Ti ' _chemical_formula_weight 310.51 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,-y+1/2,-z' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' #------------------------------------------------------------------------------ _cell_length_a 8.796(1) _cell_length_b 12.27(0) _cell_length_c 12.56(0) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1355.4(0) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 273.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type empirical #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 6033 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 24.71 _diffrn_measured_fraction_theta_max 0.9817 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.9817 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1283 _reflns_number_gt 1067 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0800 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1328 _refine_ls_number_parameters 154 _refine_ls_goodness_of_fit_ref 0.741 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.46 _refine_diff_density_min -0.69 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cl' 'Cl' 0.174 0.200 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #============================================================================== # 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 Ti1 Ti 0.2636(1) 0.6401(1) 0.2609(1) 0.016(0) Uani 1.00 1 d . . . Cl1 Cl 0.307(0) 0.821(0) 0.271(0) 0.028(0) Uani 1.00 1 d . . . Cl2 Cl 0.389(0) 0.574(0) 0.400(0) 0.027(0) Uani 1.00 1 d . . . Cl3 Cl 0.416(0) 0.583(0) 0.132(0) 0.025(0) Uani 1.00 1 d . . . O1 O 0.097(0) 0.551(0) 0.249(0) 0.017(1) Uani 1.00 1 d . . . N1 N 0.025(0) 0.655(0) 0.250(0) 0.013(1) Uani 1.00 1 d . . . C1 C -0.071(1) 0.669(0) 0.350(0) 0.02(0) Uani 1.00 1 d . . . C2 C -0.150(1) 0.780(0) 0.343(0) 0.02(0) Uani 1.00 1 d . . . C3 C -0.237(1) 0.798(0) 0.241(0) 0.02(0) Uani 1.00 1 d . . . C4 C -0.127(1) 0.790(0) 0.149(0) 0.02(0) Uani 1.00 1 d . . . C5 C -0.049(1) 0.679(0) 0.141(0) 0.02(0) Uani 1.00 1 d . . . C6 C -0.156(1) 0.587(1) 0.107(0) 0.02(0) Uani 1.00 1 d . . . C7 C 0.079(1) 0.687(1) 0.058(0) 0.02(0) Uani 1.00 1 d . . . C8 C -0.185(1) 0.577(1) 0.363(1) 0.03(0) Uani 1.00 1 d . . . C9 C 0.035(1) 0.670(1) 0.446(0) 0.03(0) Uani 1.00 1 d . . . H1 H -0.218(1) 0.787(0) 0.401(0) 0.03(0) Uiso 1.00 1 c . . . H2 H -0.074(1) 0.835(0) 0.348(0) 0.03(0) Uiso 1.00 1 c . . . H3 H -0.314(1) 0.744(0) 0.235(0) 0.03(0) Uiso 1.00 1 c . . . H4 H -0.283(1) 0.868(0) 0.242(0) 0.03(0) Uiso 1.00 1 c . . . H5 H -0.182(1) 0.803(0) 0.085(0) 0.02(0) Uiso 1.00 1 c . . . H6 H -0.052(1) 0.845(0) 0.157(0) 0.02(0) Uiso 1.00 1 c . . . H7 H -0.101(1) 0.520(1) 0.105(0) 0.03(0) Uiso 1.00 1 c . . . H8 H -0.236(1) 0.581(1) 0.157(0) 0.03(0) Uiso 1.00 1 c . . . H9 H -0.196(1) 0.602(1) 0.039(0) 0.03(0) Uiso 1.00 1 c . . . H10 H 0.039(1) 0.708(1) -0.010(0) 0.03(0) Uiso 1.00 1 c . . . H11 H 0.128(1) 0.618(1) 0.052(0) 0.03(0) Uiso 1.00 1 c . . . H12 H 0.151(1) 0.740(1) 0.080(0) 0.03(0) Uiso 1.00 1 c . . . H13 H -0.132(1) 0.510(1) 0.367(1) 0.04(0) Uiso 1.00 1 c . . . H14 H -0.242(1) 0.588(1) 0.426(1) 0.04(0) Uiso 1.00 1 c . . . H15 H -0.252(1) 0.576(1) 0.303(1) 0.04(0) Uiso 1.00 1 c . . . H16 H 0.106(1) 0.728(1) 0.440(0) 0.03(0) Uiso 1.00 1 c . . . H17 H 0.089(1) 0.602(1) 0.449(0) 0.03(0) Uiso 1.00 1 c . . . H18 H -0.022(1) 0.679(1) 0.510(0) 0.03(0) Uiso 1.00 1 c . . . 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 Ti1 0.013(0) 0.017(1) 0.017(1) 0.001(0) -0.001(0) -0.000(0) Cl1 0.023(1) 0.019(1) 0.043(1) -0.003(1) -0.006(1) -0.001(1) Cl2 0.026(1) 0.033(1) 0.022(1) 0.008(1) -0.008(1) 0.001(1) Cl3 0.017(1) 0.035(1) 0.024(1) 0.004(1) 0.004(1) -0.000(1) O1 0.01(0) 0.01(0) 0.02(0) 0.00(0) -0.00(0) -0.00(0) N1 0.02(0) 0.01(0) 0.01(0) 0.00(0) 0.00(0) -0.00(0) C1 0.02(0) 0.03(0) 0.01(0) 0.01(0) 0.01(0) 0.00(0) C2 0.02(0) 0.02(0) 0.02(0) 0.00(0) 0.00(0) -0.00(0) C3 0.02(0) 0.02(0) 0.02(0) 0.00(0) 0.00(0) -0.00(0) C4 0.01(0) 0.02(0) 0.02(0) 0.00(0) -0.01(0) 0.00(0) C5 0.02(0) 0.02(0) 0.01(0) -0.00(0) -0.00(0) 0.00(0) C6 0.02(0) 0.03(0) 0.03(0) 0.00(0) -0.01(0) -0.01(0) C7 0.02(0) 0.03(0) 0.02(0) 0.01(0) 0.00(0) -0.00(0) C8 0.02(0) 0.02(0) 0.04(0) 0.00(0) 0.02(0) 0.01(0) C9 0.03(0) 0.04(0) 0.01(0) 0.01(0) 0.01(0) 0.00(0) #============================================================================== _computing_data_collection 'Unknown' _computing_cell_refinement 'Unknown' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS97' _computing_structure_refinement 'CRYSTALS' _computing_publication_material 'CrystalStructure Ver. 2.00' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.2577(15) yes Ti1 . Cl2 . 2.2157(15) yes Ti1 . Cl3 . 2.2178(16) yes Ti1 . O1 . 1.839(3) yes Ti1 . N1 . 2.112(4) yes O1 . N1 . 1.433(4) yes N1 . C1 . 1.527(6) yes N1 . C5 . 1.537(6) yes C1 . C2 . 1.528(7) yes C1 . C8 . 1.521(8) yes C1 . C9 . 1.522(7) yes C2 . C3 . 1.506(7) yes C2 . H1 . 0.94995(7) no C2 . H2 . 0.94996(7) no C3 . C4 . 1.515(7) yes C3 . H3 . 0.95004(7) no C3 . H4 . 0.94999(8) no C4 . C5 . 1.533(7) yes C4 . H5 . 0.95003(8) no C4 . H6 . 0.95002(7) no C5 . C6 . 1.532(7) yes C5 . C7 . 1.543(7) yes C6 . H7 . 0.94999(8) no C6 . H8 . 0.94998(7) no C6 . H9 . 0.95004(8) no C7 . H10 . 0.94997(8) no C7 . H11 . 0.94996(8) no C7 . H12 . 0.95002(6) no C8 . H13 . 0.94999(8) no C8 . H14 . 0.94999(7) no C8 . H15 . 0.95001(7) no C9 . H16 . 0.95007(7) no C9 . H17 . 0.94996(8) no C9 . H18 . 0.95003(7) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl2 . 103.56(7) yes Cl1 . Ti1 . Cl3 . 104.31(7) yes Cl2 . Ti1 . Cl3 . 99.13(6) yes Cl1 . Ti1 . O1 . 136.6(1) yes Cl2 . Ti1 . O1 . 104.12(11) yes Cl3 . Ti1 . O1 . 103.50(11) yes Cl1 . Ti1 . N1 . 94.79(11) yes Cl2 . Ti1 . N1 . 125.43(13) yes Cl3 . Ti1 . N1 . 125.48(13) yes O1 . Ti1 . N1 . 41.83(13) yes Ti1 . O1 . N1 . 79.35(19) yes Ti1 . N1 . O1 . 58.82(16) yes Ti1 . N1 . C1 . 120.2(3) yes O1 . N1 . C1 . 110.6(4) yes Ti1 . N1 . C5 . 119.6(3) yes O1 . N1 . C5 . 110.2(3) yes C1 . N1 . C5 . 118.8(3) yes N1 . C1 . C2 . 107.4(4) yes N1 . C1 . C8 . 111.4(4) yes C2 . C1 . C8 . 111.5(4) yes N1 . C1 . C9 . 108.6(4) yes C2 . C1 . C9 . 109.0(4) yes C8 . C1 . C9 . 108.9(5) yes C1 . C2 . C3 . 114.6(4) yes C1 . C2 . H1 . 108.4(3) no C3 . C2 . H1 . 108.4(3) no C1 . C2 . H2 . 108.0(3) no C3 . C2 . H2 . 107.8(3) no H1 . C2 . H2 . 109.461(6) no C2 . C3 . C4 . 108.4(4) yes C2 . C3 . H3 . 109.4(3) no C4 . C3 . H3 . 109.7(3) no C2 . C3 . H4 . 110.1(3) no C4 . C3 . H4 . 109.8(3) no H3 . C3 . H4 . 109.462(9) no C3 . C4 . C5 . 113.1(4) yes C3 . C4 . H5 . 108.6(3) no C5 . C4 . H5 . 108.5(3) no C3 . C4 . H6 . 108.4(3) no C5 . C4 . H6 . 108.7(3) no H5 . C4 . H6 . 109.461(5) no N1 . C5 . C4 . 107.6(4) yes N1 . C5 . C6 . 111.6(4) yes C4 . C5 . C6 . 113.4(4) yes N1 . C5 . C7 . 108.0(4) yes C4 . C5 . C7 . 108.2(4) yes C6 . C5 . C7 . 107.9(4) yes C5 . C6 . H7 . 109.5(3) no C5 . C6 . H8 . 109.0(3) no H7 . C6 . H8 . 109.471(7) no C5 . C6 . H9 . 110.0(3) no H7 . C6 . H9 . 109.472(3) no H8 . C6 . H9 . 109.475(9) no C5 . C7 . H10 . 110.5(3) no C5 . C7 . H11 . 108.9(3) no H10 . C7 . H11 . 109.474(7) no C5 . C7 . H12 . 109.0(3) no H10 . C7 . H12 . 109.469(4) no H11 . C7 . H12 . 109.472(6) no C1 . C8 . H13 . 109.3(3) no C1 . C8 . H14 . 109.6(3) no H13 . C8 . H14 . 109.470(4) no C1 . C8 . H15 . 109.6(3) no H13 . C8 . H15 . 109.469(6) no H14 . C8 . H15 . 109.473(7) no C1 . C9 . H16 . 109.2(3) no C1 . C9 . H17 . 109.2(3) no H16 . C9 . H17 . 109.471(9) no C1 . C9 . H18 . 110.0(3) no H16 . C9 . H18 . 109.475(6) no H17 . C9 . H18 . 109.474(4) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_site_symmetry_1 _geom_torsion_atom_site_label_2 _geom_torsion_site_symmetry_2 _geom_torsion_atom_site_label_3 _geom_torsion_site_symmetry_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl1 . Ti1 . O1 . N1 . -0.2(1) yes Cl2 . Ti1 . O1 . N1 . 128.0(0) yes Cl3 . Ti1 . O1 . N1 . -128.8(0) yes N1 . Ti1 . O1 . N1 . 0.0(0) yes Cl1 . Ti1 . N1 . O1 . 179.9(0) yes Cl1 . Ti1 . N1 . C1 . -83.1(1) yes Cl1 . Ti1 . N1 . C5 . 82.9(1) yes Cl2 . Ti1 . N1 . O1 . -69.8(0) yes Cl2 . Ti1 . N1 . C1 . 27.3(1) yes Cl2 . Ti1 . N1 . C5 . -166.7(1) yes Cl3 . Ti1 . N1 . O1 . 68.5(0) yes Cl3 . Ti1 . N1 . C1 . 165.6(1) yes Cl3 . Ti1 . N1 . C5 . -28.5(1) yes O1 . Ti1 . N1 . O1 . 0.0(0) yes O1 . Ti1 . N1 . C1 . 97.1(1) yes O1 . Ti1 . N1 . C5 . -97.0(1) yes Ti1 . O1 . N1 . Ti1 . 0.0(1) yes Ti1 . O1 . N1 . C1 . -113.6(0) yes Ti1 . O1 . N1 . C5 . 113.1(0) yes Ti1 . N1 . C1 . C2 . 117.8(1) yes Ti1 . N1 . C1 . C8 . -119.8(1) yes Ti1 . N1 . C1 . C9 . 0.1(1) yes O1 . N1 . C1 . C2 . -177.1(1) yes O1 . N1 . C1 . C8 . -54.7(1) yes O1 . N1 . C1 . C9 . 65.2(1) yes C5 . N1 . C1 . C2 . -48.2(1) yes C5 . N1 . C1 . C8 . 74.1(1) yes C5 . N1 . C1 . C9 . -166.0(1) yes Ti1 . N1 . C5 . C4 . -116.8(1) yes Ti1 . N1 . C5 . C6 . 118.2(1) yes Ti1 . N1 . C5 . C7 . -0.2(1) yes O1 . N1 . C5 . C4 . 178.3(1) yes O1 . N1 . C5 . C6 . 53.3(1) yes O1 . N1 . C5 . C7 . -65.1(1) yes C1 . N1 . C5 . C4 . 49.3(1) yes C1 . N1 . C5 . C6 . -75.7(1) yes C1 . N1 . C5 . C7 . 165.9(1) yes N1 . C1 . C2 . C3 . 52.5(1) yes C8 . C1 . C2 . C3 . -69.8(1) yes C9 . C1 . C2 . C3 . 170.0(1) yes C1 . C2 . C3 . C4 . -60.0(1) yes C2 . C3 . C4 . C5 . 60.3(1) yes C3 . C4 . C5 . N1 . -53.8(1) yes C3 . C4 . C5 . C6 . 70.2(1) yes C3 . C4 . C5 . C7 . -170.2(1) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_site_symmetry_1 _geom_contact_atom_site_label_2 _geom_contact_site_symmetry_2 _geom_contact_distance _geom_contact_publ_flag Ti1 . Cl1 . 2.2577(15) yes Ti1 . Cl2 . 2.2157(15) yes Ti1 . Cl3 . 2.2178(16) yes Ti1 . O1 . 1.839(3) yes Ti1 . N1 . 2.112(4) yes Ti1 . C1 . 3.168(5) yes Ti1 . C5 . 3.166(5) yes Ti1 . C7 . 3.079(5) yes Ti1 . C9 . 3.098(5) yes Ti1 . H4 3_545 3.338(5) no Ti1 . H11 . 2.896(5) no Ti1 . H12 . 2.766(5) no Ti1 . H16 . 2.852(5) no Ti1 . H17 . 2.857(5) no Cl1 . Cl2 . 3.515(2) yes Cl1 . Cl3 . 3.534(2) yes Cl1 . N1 . 3.218(4) yes Cl1 . H2 . 3.494(6) no Cl1 . H3 1_655 3.499(5) no Cl1 . H6 . 3.471(5) no Cl1 . H7 3_555 3.414(6) no Cl1 . H8 3_555 3.375(6) no Cl1 . H12 . 2.929(5) no Cl1 . H13 3_555 3.268(6) no Cl1 . H15 3_555 3.301(6) no Cl1 . H16 . 2.994(6) no Cl1 . H18 2_566 3.141(5) no Cl2 . Cl3 . 3.3745(18) yes Cl2 . O1 . 3.206(3) yes Cl2 . C9 . 3.380(6) yes Cl2 . H1 2_566 3.177(5) no Cl2 . H2 2_566 3.379(5) no Cl2 . H4 3_545 3.225(5) no Cl2 . H7 4_565 3.390(6) no Cl2 . H11 4_565 3.041(6) no Cl2 . H14 1_655 3.266(6) no Cl2 . H15 1_655 3.384(6) no Cl2 . H16 . 3.169(6) no Cl2 . H17 . 2.738(6) no Cl2 . H18 2_566 3.336(6) no Cl3 . O1 . 3.194(3) yes Cl3 . C7 . 3.356(6) yes Cl3 . H3 1_655 3.352(5) no Cl3 . H4 3_545 3.288(5) no Cl3 . H5 2_565 3.177(5) no Cl3 . H8 1_655 3.076(5) no Cl3 . H10 2_565 3.181(5) no Cl3 . H11 . 2.757(6) no Cl3 . H12 . 3.095(6) no Cl3 . H17 4_564 3.232(6) no O1 . N1 . 1.433(4) yes O1 . C1 . 2.434(6) yes O1 . C2 3_545 3.544(6) yes O1 . C3 3_545 3.334(6) yes O1 . C4 3_545 3.452(6) yes O1 . C5 . 2.437(6) yes O1 . C6 . 2.880(6) yes O1 . C7 . 2.933(6) yes O1 . C8 . 2.880(6) yes O1 . C9 . 2.930(6) yes O1 . H2 3_545 2.915(6) no O1 . H4 3_545 2.774(6) no O1 . H6 3_545 2.813(6) no O1 . H7 . 2.535(6) no O1 . H8 . 3.170(6) no O1 . H11 . 2.625(6) no O1 . H12 . 3.184(6) no O1 . H13 . 2.547(6) no O1 . H15 . 3.155(6) no O1 . H16 . 3.238(6) no O1 . H17 . 2.594(6) no N1 . C1 . 1.527(6) yes N1 . C2 . 2.463(6) yes N1 . C3 . 2.897(6) yes N1 . C4 . 2.477(6) yes N1 . C5 . 1.537(6) yes N1 . C6 . 2.539(6) yes N1 . C7 . 2.492(6) yes N1 . C8 . 2.518(6) yes N1 . C9 . 2.477(6) yes N1 . H1 . 3.282(7) no N1 . H2 . 2.672(6) no N1 . H3 . 3.175(6) no N1 . H5 . 3.296(6) no N1 . H6 . 2.685(6) no N1 . H7 . 2.700(6) no N1 . H8 . 2.730(6) no N1 . H9 . 3.355(6) no N1 . H10 . 3.324(6) no N1 . H11 . 2.687(6) no N1 . H12 . 2.618(6) no N1 . H13 . 2.692(7) no N1 . H14 . 3.333(6) no N1 . H15 . 2.703(6) no N1 . H16 . 2.641(6) no N1 . H17 . 2.644(6) no N1 . H18 . 3.306(6) no C1 . C2 . 1.528(7) yes C1 . C3 . 2.553(7) yes C1 . C4 . 2.976(8) yes C1 . C5 . 2.637(7) yes C1 . C6 . 3.305(7) yes C1 . C8 . 1.521(8) yes C1 . C9 . 1.522(7) yes C1 . H1 . 2.038(7) no C1 . H2 . 2.034(7) no C1 . H3 . 2.741(7) no C1 . H4 . 3.360(7) no C1 . H6 . 3.249(8) no C1 . H7 . 3.594(7) no C1 . H8 . 3.029(7) no C1 . H13 . 2.042(8) no C1 . H14 . 2.046(7) no C1 . H15 . 2.046(8) no C1 . H16 . 2.043(8) no C1 . H17 . 2.042(8) no C1 . H18 . 2.052(7) no C2 . C3 . 1.506(7) yes C2 . C4 . 2.449(7) yes C2 . C5 . 2.957(7) yes C2 . C8 . 2.520(8) yes C2 . C9 . 2.483(8) yes C2 . H1 . 0.94995(7) no C2 . H2 . 0.94996(7) no C2 . H3 . 2.030(7) no C2 . H4 . 2.037(7) no C2 . H5 . 3.268(7) no C2 . H6 . 2.612(7) no C2 . H8 . 3.458(8) no C2 . H13 . 3.333(8) no C2 . H14 . 2.707(8) no C2 . H15 . 2.700(8) no C2 . H16 . 2.632(8) no C2 . H16 2_466 3.478(8) no C2 . H17 . 3.304(8) no C2 . H18 . 2.686(7) no C3 . C4 . 1.515(7) yes C3 . C5 . 2.544(7) yes C3 . C6 . 3.175(7) yes C3 . C8 . 3.145(8) yes C3 . H1 . 2.018(7) no C3 . H2 . 2.011(7) no C3 . H3 . 0.95004(7) no C3 . H4 . 0.94999(8) no C3 . H5 . 2.029(7) no C3 . H6 . 2.027(7) no C3 . H8 . 2.863(7) no C3 . H9 . 3.524(7) no C3 . H10 2_465 3.517(7) no C3 . H14 . 3.474(8) no C3 . H15 . 2.833(8) no C4 . C5 . 1.533(7) yes C4 . C6 . 2.562(8) yes C4 . C7 . 2.492(7) yes C4 . H1 . 3.268(7) no C4 . H2 . 2.602(7) no C4 . H3 . 2.042(7) no C4 . H4 . 2.042(7) no C4 . H5 . 0.95003(8) no C4 . H6 . 0.95002(7) no C4 . H7 . 3.368(8) no C4 . H8 . 2.738(8) no C4 . H9 . 2.762(7) no C4 . H10 . 2.671(7) no C4 . H10 2_465 3.419(7) no C4 . H11 . 3.313(7) no C4 . H11 2_465 3.500(7) no C4 . H12 . 2.664(7) no C4 . H12 2_465 3.499(7) no C4 . H13 3_555 3.533(8) no C4 . H15 . 3.441(8) no C5 . C6 . 1.532(7) yes C5 . C7 . 1.543(7) yes C5 . C8 . 3.276(7) yes C5 . H2 . 3.234(7) no C5 . H3 . 2.728(7) no C5 . H4 . 3.355(7) no C5 . H5 . 2.044(7) no C5 . H6 . 2.046(7) no C5 . H7 . 2.054(8) no C5 . H8 . 2.049(7) no C5 . H9 . 2.060(7) no C5 . H10 . 2.077(7) no C5 . H11 . 2.057(7) no C5 . H12 . 2.059(7) no C5 . H13 . 3.585(8) no C5 . H15 . 2.985(7) no C6 . C7 . 2.486(8) yes C6 . C8 . 3.222(8) yes C6 . H3 . 2.864(7) no C6 . H5 . 2.672(8) no C6 . H6 . 3.355(8) no C6 . H7 . 0.94999(8) no C6 . H8 . 0.94998(7) no C6 . H9 . 0.95004(8) no C6 . H10 . 2.698(8) no C6 . H11 . 2.621(7) no C6 . H12 . 3.308(8) no C6 . H12 2_465 3.596(7) no C6 . H13 . 3.399(8) no C6 . H14 4_464 3.249(7) no C6 . H15 . 2.606(8) no C7 . H5 . 2.718(7) no C7 . H5 2_565 2.764(7) no C7 . H6 . 2.575(7) no C7 . H7 . 2.662(8) no C7 . H8 . 3.311(8) no C7 . H9 . 2.652(8) no C7 . H9 2_565 3.472(8) no C7 . H10 . 0.94997(8) no C7 . H11 . 0.94996(8) no C7 . H12 . 0.95002(6) no C8 . C9 . 2.476(8) yes C8 . H1 . 2.630(8) no C8 . H2 . 3.317(8) no C8 . H3 . 2.839(8) no C8 . H6 3_545 3.536(8) no C8 . H7 . 3.391(8) no C8 . H8 . 2.621(8) no C8 . H9 4_465 3.286(7) no C8 . H13 . 0.94999(8) no C8 . H14 . 0.94999(7) no C8 . H15 . 0.95001(7) no C8 . H16 . 3.298(8) no C8 . H17 . 2.655(8) no C8 . H18 . 2.649(8) no C9 . H1 . 2.710(8) no C9 . H1 2_566 2.944(8) no C9 . H2 . 2.565(8) no C9 . H13 . 2.648(8) no C9 . H14 . 2.649(8) no C9 . H15 . 3.301(8) no C9 . H16 . 0.95007(7) no C9 . H17 . 0.94996(8) no C9 . H18 . 0.95003(7) no H1 . H2 . 1.55118(11) no H1 . H3 . 2.312(7) no H1 . H4 . 2.305(7) no H1 . H6 . 3.471(8) no H1 . H13 . 3.507(8) no H1 . H14 . 2.471(8) no H1 . H15 . 2.871(8) no H1 . H16 . 2.977(8) no H1 . H16 2_466 2.537(8) no H1 . H17 . 3.570(8) no H1 . H17 2_466 2.880(8) no H1 . H18 . 2.570(8) no H1 . H18 2_466 2.928(8) no H2 . H3 . 2.775(7) no H2 . H4 . 2.303(7) no H2 . H5 . 3.462(7) no H2 . H6 . 2.406(7) no H2 . H7 3_555 2.805(8) no H2 . H14 . 3.518(8) no H2 . H15 . 3.581(8) no H2 . H16 . 2.358(8) no H2 . H17 . 3.437(8) no H2 . H18 . 2.837(8) no H3 . H4 . 1.55128(16) no H3 . H5 . 2.327(7) no H3 . H6 . 2.791(7) no H3 . H8 . 2.320(7) no H3 . H9 . 3.188(7) no H3 . H10 2_465 3.167(7) no H3 . H14 . 3.141(8) no H3 . H15 . 2.295(8) no H4 . H5 . 2.315(7) no H4 . H6 . 2.317(7) no H4 . H10 2_465 3.443(7) no H5 . H6 . 1.5513(1) no H5 . H7 . 3.548(8) no H5 . H8 . 2.904(8) no H5 . H9 . 2.533(8) no H5 . H10 . 2.555(7) no H5 . H10 2_465 2.636(7) no H5 . H11 . 3.564(7) no H5 . H11 2_465 2.585(7) no H5 . H12 . 3.023(8) no H5 . H12 2_465 2.597(7) no H6 . H9 . 3.568(8) no H6 . H10 . 2.805(7) no H6 . H11 . 3.460(7) no H6 . H12 . 2.398(7) no H6 . H13 3_555 2.605(8) no H6 . H17 3_555 3.444(7) no H7 . H8 . 1.5513(1) no H7 . H9 . 1.5514(1) no H7 . H10 . 2.982(8) no H7 . H11 . 2.445(8) no H7 . H12 . 3.511(8) no H7 . H13 . 3.297(8) no H7 . H14 4_464 2.950(7) no H7 . H15 . 2.901(8) no H8 . H9 . 1.55139(15) no H8 . H10 . 3.558(8) no H8 . H11 . 3.499(7) no H8 . H13 . 2.919(8) no H8 . H14 . 3.378(8) no H8 . H14 4_464 3.573(7) no H8 . H15 . 1.839(8) no H9 . H10 . 2.517(8) no H9 . H10 2_465 3.319(8) no H9 . H11 . 2.867(7) no H9 . H12 . 3.534(8) no H9 . H12 2_465 2.790(8) no H9 . H13 4_464 2.971(7) no H9 . H14 4_464 2.773(7) no H9 . H15 . 3.373(8) no H10 . H11 . 1.5513(1) no H10 . H12 . 1.55131(11) no H10 . H12 2_465 3.584(3) no H11 . H12 . 1.55134(15) no H12 . H13 3_555 3.374(8) no H13 . H14 . 1.5513(1) no H13 . H15 . 1.5513(1) no H13 . H16 . 3.517(8) no H13 . H17 . 2.475(8) no H13 . H18 . 2.910(8) no H14 . H15 . 1.55136(16) no H14 . H16 . 3.513(8) no H14 . H16 2_466 3.125(8) no H14 . H17 . 2.927(8) no H14 . H18 . 2.469(8) no H15 . H17 . 3.521(8) no H15 . H18 . 3.519(8) no H16 . H17 . 1.55136(16) no H16 . H18 . 1.5515(1) no H16 . H18 2_566 3.528(4) no H17 . H18 . 1.55136(9) no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================