Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Martyn P. Coles' 'Sarah C. Cole' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Martyn P. Coles' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'M.P.COLES@SUSSEX.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Transition-Metal Imido-Boroxide Complexes: A Structural and Spectroscopic Investigation of the Influence of the Boron Atom ; data_(1)mar1402 _database_code_CSD 190539 _audit_creation_date 2002-03-22T14:19:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Zn{N(SiMe3)2}{MesNPPh2CHPPh2NMes}]' _chemical_formula_moiety 'C44 H62 B2 Mo N2 O2' _chemical_formula_sum 'C44 H62 B2 Mo N2 O2' _chemical_formula_weight 768.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Aba2 _symmetry_Int_Tables_number 41 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 19.0505(6) _cell_length_b 27.3517(7) _cell_length_c 8.4738(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4415.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10905 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7779 _exptl_absorpt_correction_T_max 0.8449 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.86479E-1 _diffrn_orient_matrix_ub_12 0.242136E-1 _diffrn_orient_matrix_ub_13 0.81954E-2 _diffrn_orient_matrix_ub_21 -0.767717E-1 _diffrn_orient_matrix_ub_22 0.273907E-1 _diffrn_orient_matrix_ub_23 -0.65379E-2 _diffrn_orient_matrix_ub_31 -0.235379E-1 _diffrn_orient_matrix_ub_32 -0.3765E-3 _diffrn_orient_matrix_ub_33 0.514345E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_unetI/netI 0.047 _diffrn_reflns_number 14970 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 25.96 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.912 _diffrn_measured_fraction_theta_max 0.912 _reflns_number_total 3706 _reflns_number_gt 2900 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0292P)^2^+8.4475P] 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 'riding; torsion refined for o-methyls' _refine_ls_extinction_method none _refine_ls_number_reflns 3706 _refine_ls_number_parameters 235 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(5) _refine_diff_density_max 0.308 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mo Mo 0 0 0.71597(8) 0.03085(12) Uani 1 2 d S . . B B 0.0073(2) 0.10453(15) 0.5483(5) 0.0313(10) Uani 1 1 d . . . O O -0.00527(14) 0.05732(9) 0.5869(3) 0.0390(7) Uani 1 1 d . . . N N 0.07419(19) -0.00009(11) 0.8329(5) 0.0474(9) Uani 1 1 d . . . C1 C 0.1207(3) 0.00028(18) 0.9706(7) 0.0678(16) Uani 1 1 d . . . C2 C 0.1211(3) 0.05137(19) 1.0395(6) 0.0663(15) Uani 1 1 d . . . H2A H 0.1383 0.0745 0.9601 0.1 Uiso 1 1 calc R . . H2B H 0.1519 0.0522 1.1321 0.1 Uiso 1 1 calc R . . H2C H 0.0733 0.0604 1.0708 0.1 Uiso 1 1 calc R . . C3 C 0.1947(4) -0.0119(3) 0.9101(10) 0.126(3) Uani 1 1 d . . . H3A H 0.2095 0.0131 0.8341 0.189 Uiso 1 1 calc R . . H3B H 0.1941 -0.0439 0.8585 0.189 Uiso 1 1 calc R . . H3C H 0.2275 -0.0125 0.999 0.189 Uiso 1 1 calc R . . C4 C 0.0947(5) -0.0366(3) 1.0895(9) 0.160(5) Uani 1 1 d . . . H4A H 0.095 -0.0693 1.042 0.24 Uiso 1 1 calc R . . H4B H 0.0468 -0.0282 1.1215 0.24 Uiso 1 1 calc R . . H4C H 0.1255 -0.0363 1.1822 0.24 Uiso 1 1 calc R . . C5 C -0.03942(19) 0.12810(14) 0.4153(5) 0.0329(9) Uani 1 1 d . . . C6 C -0.0100(2) 0.15594(14) 0.2919(5) 0.0375(9) Uani 1 1 d . . . C7 C -0.0536(2) 0.17659(16) 0.1770(5) 0.0438(12) Uani 1 1 d . . . H7 H -0.0331 0.1945 0.0927 0.053 Uiso 1 1 calc R . . C8 C -0.1260(2) 0.17173(15) 0.1827(5) 0.0469(13) Uani 1 1 d . . . C9 C -0.1546(2) 0.14500(15) 0.3048(6) 0.0463(11) Uani 1 1 d . . . H9 H -0.2042 0.1418 0.3106 0.056 Uiso 1 1 calc R . . C10 C -0.1132(2) 0.12244(14) 0.4207(5) 0.0390(10) Uani 1 1 d . . . C11 C 0.0684(2) 0.16398(16) 0.2763(6) 0.0476(13) Uani 1 1 d . . . H11A H 0.0781 0.1823 0.1794 0.071 Uiso 1 1 calc R . . H11B H 0.0923 0.1323 0.2718 0.071 Uiso 1 1 calc R . . H11C H 0.0854 0.1825 0.3675 0.071 Uiso 1 1 calc R . . C12 C -0.1720(3) 0.1953(2) 0.0587(7) 0.0703(16) Uani 1 1 d . . . H12A H -0.1426 0.2126 -0.0178 0.105 Uiso 0.5 1 calc PR . . H12B H -0.2041 0.2185 0.1093 0.105 Uiso 0.5 1 calc PR . . H12C H -0.1993 0.17 0.0042 0.105 Uiso 0.5 1 calc PR . . H12D H -0.2214 0.1881 0.0816 0.105 Uiso 0.5 1 calc PR . . H12E H -0.1599 0.1823 -0.0455 0.105 Uiso 0.5 1 calc PR . . H12F H -0.1647 0.2308 0.0596 0.105 Uiso 0.5 1 calc PR . . C13 C -0.1495(2) 0.09422(19) 0.5498(6) 0.0583(13) Uani 1 1 d . . . H13A H -0.1458 0.0591 0.5283 0.087 Uiso 1 1 calc R . . H13B H -0.1991 0.1036 0.5539 0.087 Uiso 1 1 calc R . . H13C H -0.1272 0.1016 0.6513 0.087 Uiso 1 1 calc R . . C14 C 0.0663(2) 0.13324(13) 0.6403(5) 0.0329(9) Uani 1 1 d . . . C15 C 0.0496(2) 0.17533(13) 0.7282(6) 0.0412(10) Uani 1 1 d . . . C16 C 0.1021(3) 0.19973(16) 0.8108(6) 0.0608(14) Uani 1 1 d . . . H16 H 0.0902 0.2276 0.8719 0.073 Uiso 1 1 calc R . . C17 C 0.1708(3) 0.1845(2) 0.8063(7) 0.0693(17) Uani 1 1 d . . . C18 C 0.1873(2) 0.14421(17) 0.7204(8) 0.0630(14) Uani 1 1 d . . . H18 H 0.2348 0.1337 0.7176 0.076 Uiso 1 1 calc R . . C19 C 0.1373(2) 0.11776(16) 0.6364(6) 0.0431(11) Uani 1 1 d . . . C20 C -0.0253(2) 0.19412(16) 0.7323(8) 0.0606(14) Uani 1 1 d . . . H20A H -0.0404 0.2024 0.625 0.091 Uiso 1 1 calc R . . H20B H -0.0277 0.2233 0.7991 0.091 Uiso 1 1 calc R . . H20C H -0.0562 0.1688 0.7754 0.091 Uiso 1 1 calc R . . C21 C 0.2273(4) 0.2130(2) 0.8949(8) 0.110(3) Uani 1 1 d . . . H21A H 0.2058 0.2407 0.9499 0.165 Uiso 0.5 1 calc PR . . H21B H 0.2623 0.2251 0.8197 0.165 Uiso 0.5 1 calc PR . . H21C H 0.2501 0.1915 0.9718 0.165 Uiso 0.5 1 calc PR . . H21D H 0.273 0.1975 0.8777 0.165 Uiso 0.5 1 calc PR . . H21E H 0.2165 0.2131 1.0079 0.165 Uiso 0.5 1 calc PR . . H21F H 0.2287 0.2467 0.8558 0.165 Uiso 0.5 1 calc PR . . C22 C 0.1600(2) 0.07474(18) 0.5359(7) 0.0608(14) Uani 1 1 d . . . H22A H 0.2052 0.0821 0.4861 0.091 Uiso 1 1 calc R . . H22B H 0.1247 0.0687 0.4542 0.091 Uiso 1 1 calc R . . H22C H 0.1648 0.0456 0.6026 0.091 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 Mo 0.0357(2) 0.01976(17) 0.0371(2) 0 0 0.0000(2) B 0.031(2) 0.030(2) 0.033(2) 0.0003(17) 0.005(2) 0.0019(19) O 0.0431(16) 0.0252(13) 0.0488(17) 0.0047(12) -0.0106(14) -0.0032(12) N 0.056(2) 0.0315(17) 0.055(2) 0.0024(19) -0.0203(18) 0.0007(17) C1 0.087(4) 0.047(3) 0.070(3) 0.007(3) -0.049(3) -0.005(3) C2 0.078(4) 0.065(3) 0.056(3) -0.007(3) -0.018(3) -0.012(3) C3 0.095(5) 0.132(6) 0.151(8) -0.066(5) -0.083(5) 0.054(5) C4 0.228(10) 0.115(6) 0.138(7) 0.090(6) -0.127(7) -0.091(7) C5 0.033(2) 0.030(2) 0.036(2) -0.0034(17) -0.0070(18) 0.0030(17) C6 0.045(3) 0.0303(19) 0.037(2) -0.0020(17) -0.008(2) 0.0012(19) C7 0.055(3) 0.045(2) 0.031(3) 0.0070(19) -0.008(2) 0.001(2) C8 0.057(3) 0.043(2) 0.040(4) -0.003(2) -0.018(2) 0.013(2) C9 0.039(2) 0.045(2) 0.055(3) -0.009(2) -0.014(2) 0.010(2) C10 0.041(2) 0.029(2) 0.047(3) -0.0035(18) -0.009(2) 0.0008(18) C11 0.046(3) 0.050(3) 0.047(3) 0.011(2) 0.001(2) -0.006(2) C12 0.068(4) 0.082(4) 0.060(3) 0.013(3) -0.026(3) 0.019(3) C13 0.038(2) 0.064(3) 0.073(4) 0.013(3) -0.005(3) -0.007(2) C14 0.039(2) 0.0294(19) 0.030(2) 0.0090(17) -0.0040(18) -0.0056(17) C15 0.055(2) 0.0351(19) 0.033(2) 0.003(2) -0.007(3) -0.0095(17) C16 0.099(4) 0.040(3) 0.043(3) 0.002(2) -0.025(3) -0.018(3) C17 0.071(4) 0.068(4) 0.069(4) 0.034(3) -0.040(3) -0.034(3) C18 0.044(2) 0.067(3) 0.078(3) 0.037(4) -0.026(3) -0.016(2) C19 0.035(2) 0.044(2) 0.051(3) 0.020(2) -0.007(2) -0.008(2) C20 0.075(3) 0.050(2) 0.057(4) -0.018(3) -0.005(4) 0.008(2) C21 0.128(6) 0.099(5) 0.103(5) 0.030(4) -0.076(5) -0.067(4) C22 0.041(3) 0.062(3) 0.079(4) 0.014(3) 0.006(3) 0.006(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N 1.726(3) . ? Mo N 1.726(3) 2 ? Mo O 1.914(2) 2 ? Mo O 1.914(2) . ? B O 1.353(5) . ? B C5 1.575(6) . ? B C14 1.577(6) . ? N C1 1.466(6) . ? C1 C4 1.509(8) . ? C1 C2 1.514(7) . ? C1 C3 1.536(9) . ? C5 C6 1.410(6) . ? C5 C10 1.415(5) . ? C6 C7 1.399(5) . ? C6 C11 1.514(5) . ? C7 C8 1.385(6) . ? C8 C9 1.380(6) . ? C8 C12 1.513(6) . ? C9 C10 1.403(6) . ? C10 C13 1.507(6) . ? C14 C15 1.408(6) . ? C14 C19 1.418(5) . ? C15 C16 1.392(6) . ? C15 C20 1.517(6) . ? C16 C17 1.373(7) . ? C17 C18 1.358(8) . ? C17 C21 1.526(7) . ? C18 C19 1.392(6) . ? C19 C22 1.515(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Mo N 110.0(3) . 2 ? N Mo O 106.48(14) . 2 ? N Mo O 111.83(14) 2 2 ? N Mo O 111.83(14) . . ? N Mo O 106.48(14) 2 . ? O Mo O 110.33(17) 2 . ? O B C5 117.6(4) . . ? O B C14 118.8(4) . . ? C5 B C14 123.6(3) . . ? B O Mo 155.5(3) . . ? C1 N Mo 162.2(4) . . ? N C1 C4 109.2(4) . . ? N C1 C2 108.4(4) . . ? C4 C1 C2 111.2(6) . . ? N C1 C3 106.7(5) . . ? C4 C1 C3 112.3(6) . . ? C2 C1 C3 108.9(5) . . ? C6 C5 C10 118.6(4) . . ? C6 C5 B 121.8(3) . . ? C10 C5 B 119.6(4) . . ? C7 C6 C5 119.8(4) . . ? C7 C6 C11 117.8(4) . . ? C5 C6 C11 122.3(4) . . ? C8 C7 C6 121.9(4) . . ? C9 C8 C7 118.1(4) . . ? C9 C8 C12 121.1(4) . . ? C7 C8 C12 120.8(4) . . ? C8 C9 C10 122.4(4) . . ? C9 C10 C5 119.2(4) . . ? C9 C10 C13 118.4(4) . . ? C5 C10 C13 122.3(4) . . ? C15 C14 C19 118.2(4) . . ? C15 C14 B 120.5(3) . . ? C19 C14 B 121.3(4) . . ? C16 C15 C14 119.7(4) . . ? C16 C15 C20 120.2(4) . . ? C14 C15 C20 120.1(4) . . ? C17 C16 C15 121.7(5) . . ? C18 C17 C16 118.8(4) . . ? C18 C17 C21 121.0(6) . . ? C16 C17 C21 120.3(6) . . ? C17 C18 C19 122.6(4) . . ? C18 C19 C14 119.1(4) . . ? C18 C19 C22 119.7(4) . . ? C14 C19 C22 121.1(4) . . ? #===END data_(2)feb1102 _database_code_CSD 190540 _audit_creation_date 2002-02-22T09:04:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Mo(OBMes2)2(NC6H3iPr2)2]' _chemical_formula_moiety 'C60 H78 B2 Mo N2 O2' _chemical_formula_sum 'C60 H78 B2 Mo N2 O2' _chemical_formula_weight 976.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbc2(1) _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 13.2134(4) _cell_length_b 19.0999(5) _cell_length_c 44.5065(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11232.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51265 _cell_measurement_theta_min 2 _cell_measurement_theta_max 22 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.954 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.1566 _diffrn_reflns_av_unetI/netI 0.1782 _diffrn_reflns_number 48346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 12794 _reflns_number_gt 6842 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Because of the rather weak diffraction and the large number of atoms in the two independent molecules, it was necessary to apply constraints (ISOR) to the ADPs of the carbon atoms to keep them positive-definite. 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^)+(0.0695P)^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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 12794 _refine_ls_number_parameters 1223 _refine_ls_number_restraints 721 _refine_ls_R_factor_all 0.1613 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 0.98 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.004 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(6) _refine_diff_density_max 0.385 _refine_diff_density_min -0.51 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mo Mo 0.10779(5) 0.35667(4) 0.079167(15) 0.0357(2) Uani 1 1 d . A 1 B1 B 0.1030(8) 0.2808(5) 0.1434(2) 0.040(3) Uani 1 1 d . A 1 B2 B 0.3431(8) 0.3851(5) 0.0690(2) 0.041(3) Uani 1 1 d . A 1 O1 O 0.1015(4) 0.3097(3) 0.11600(11) 0.0423(17) Uani 1 1 d . A 1 O2 O 0.2401(4) 0.3841(3) 0.06866(12) 0.0440(19) Uani 1 1 d . A 1 N1 N 0.0325(5) 0.4315(3) 0.08167(16) 0.036(2) Uani 1 1 d . A 1 N2 N 0.0555(5) 0.3045(3) 0.05123(14) 0.039(2) Uani 1 1 d . A 1 C1 C 0.0087(6) 0.2381(5) 0.1523(2) 0.034(3) Uani 1 1 d U A 1 C2 C -0.0410(7) 0.2521(4) 0.18071(19) 0.043(3) Uani 1 1 d U A 1 C3 C -0.1333(7) 0.2191(4) 0.1872(2) 0.049(3) Uani 1 1 d U A 1 H3 H -0.1679 0.2326 0.2049 0.059 Uiso 1 1 calc R A 1 C4 C -0.1752(7) 0.1703(5) 0.1700(2) 0.052(3) Uani 1 1 d U A 1 C5 C -0.1225(7) 0.1511(5) 0.14318(19) 0.053(3) Uani 1 1 d U A 1 H5 H -0.1486 0.1143 0.1311 0.064 Uiso 1 1 calc R A 1 C6 C -0.0338(7) 0.1847(5) 0.13427(19) 0.041(3) Uani 1 1 d U A 1 C7 C -0.0012(6) 0.3026(5) 0.2033(2) 0.051(4) Uani 1 1 d U A 1 H7A H 0.0625 0.3228 0.196 0.076 Uiso 0.5 1 calc PR A 1 H7B H 0.0109 0.2783 0.2223 0.076 Uiso 0.5 1 calc PR A 1 H7C H -0.0507 0.3401 0.2064 0.076 Uiso 0.5 1 calc PR A 1 H7D H -0.0474 0.3047 0.2205 0.076 Uiso 0.5 1 calc PR A 1 H7E H 0.0042 0.3492 0.1942 0.076 Uiso 0.5 1 calc PR A 1 H7F H 0.0658 0.2873 0.2101 0.076 Uiso 0.5 1 calc PR A 1 C8 C -0.2700(7) 0.1306(5) 0.1776(2) 0.069(3) Uani 1 1 d U A 1 H8A H -0.2839 0.0963 0.1617 0.104 Uiso 0.5 1 calc PR A 1 H8B H -0.3268 0.1633 0.1792 0.104 Uiso 0.5 1 calc PR A 1 H8C H -0.2609 0.1062 0.1968 0.104 Uiso 0.5 1 calc PR A 1 H8D H -0.2972 0.1476 0.1967 0.104 Uiso 0.5 1 calc PR A 1 H8E H -0.2543 0.0806 0.1793 0.104 Uiso 0.5 1 calc PR A 1 H8F H -0.3202 0.1377 0.1617 0.104 Uiso 0.5 1 calc PR A 1 C9 C 0.0209(7) 0.1617(5) 0.1068(2) 0.052(3) Uani 1 1 d U A 1 H9A H 0.0812 0.1909 0.1039 0.078 Uiso 0.5 1 calc PR A 1 H9B H -0.0236 0.1665 0.0893 0.078 Uiso 0.5 1 calc PR A 1 H9C H 0.0413 0.1127 0.109 0.078 Uiso 0.5 1 calc PR A 1 H9D H -0.0153 0.1225 0.0975 0.078 Uiso 0.5 1 calc PR A 1 H9E H 0.0895 0.1469 0.1122 0.078 Uiso 0.5 1 calc PR A 1 H9F H 0.0246 0.2007 0.0925 0.078 Uiso 0.5 1 calc PR A 1 C10 C 0.2055(6) 0.2923(4) 0.16171(17) 0.037(3) Uani 1 1 d U A 1 C11 C 0.2582(7) 0.2341(4) 0.17451(19) 0.047(3) Uani 1 1 d U A 1 C12 C 0.3533(7) 0.2417(5) 0.18701(19) 0.049(3) Uani 1 1 d U A 1 H12 H 0.3858 0.2023 0.1958 0.059 Uiso 1 1 calc R A 1 C13 C 0.4023(7) 0.3063(5) 0.18689(19) 0.053(3) Uani 1 1 d U A 1 C14 C 0.3505(7) 0.3638(5) 0.17659(18) 0.044(3) Uani 1 1 d U A 1 H14 H 0.3801 0.4089 0.1784 0.053 Uiso 1 1 calc R A 1 C15 C 0.2574(7) 0.3571(4) 0.16377(18) 0.041(3) Uani 1 1 d U A 1 C16 C 0.2117(7) 0.1611(4) 0.17472(19) 0.044(3) Uani 1 1 d U A 1 H16A H 0.1445 0.1627 0.1654 0.067 Uiso 0.5 1 calc PR A 1 H16B H 0.2054 0.1446 0.1955 0.067 Uiso 0.5 1 calc PR A 1 H16C H 0.2552 0.1289 0.1634 0.067 Uiso 0.5 1 calc PR A 1 H16D H 0.2589 0.1281 0.1841 0.067 Uiso 0.5 1 calc PR A 1 H16E H 0.198 0.1462 0.154 0.067 Uiso 0.5 1 calc PR A 1 H16F H 0.1482 0.1619 0.1861 0.067 Uiso 0.5 1 calc PR A 1 C17 C 0.5089(7) 0.3075(6) 0.2006(3) 0.069(4) Uani 1 1 d U A 1 H17A H 0.528 0.26 0.2067 0.103 Uiso 0.5 1 calc PR A 1 H17B H 0.5095 0.3384 0.2182 0.103 Uiso 0.5 1 calc PR A 1 H17C H 0.5573 0.3249 0.1857 0.103 Uiso 0.5 1 calc PR A 1 H17D H 0.5351 0.3555 0.2004 0.103 Uiso 0.5 1 calc PR A 1 H17E H 0.5537 0.2772 0.1889 0.103 Uiso 0.5 1 calc PR A 1 H17F H 0.5059 0.2906 0.2214 0.103 Uiso 0.5 1 calc PR A 1 C18 C 0.1985(8) 0.4237(5) 0.1530(2) 0.069(3) Uani 1 1 d U A 1 H18A H 0.1333 0.4096 0.1445 0.104 Uiso 0.5 1 calc PR A 1 H18B H 0.2384 0.4481 0.1377 0.104 Uiso 0.5 1 calc PR A 1 H18C H 0.1871 0.4549 0.1701 0.104 Uiso 0.5 1 calc PR A 1 H18D H 0.2393 0.4655 0.1571 0.104 Uiso 0.5 1 calc PR A 1 H18E H 0.1341 0.427 0.1639 0.104 Uiso 0.5 1 calc PR A 1 H18F H 0.1854 0.4202 0.1314 0.104 Uiso 0.5 1 calc PR A 1 C19 C 0.3965(6) 0.4465(4) 0.08594(17) 0.042(3) Uani 1 1 d U A 1 C20 C 0.4752(6) 0.4341(5) 0.1077(2) 0.039(3) Uani 1 1 d U A 1 C21 C 0.5144(7) 0.4818(6) 0.1236(2) 0.062(4) Uani 1 1 d U A 1 H21 H 0.5643 0.47 0.1381 0.075 Uiso 1 1 calc R A 1 C22 C 0.4848(7) 0.5529(6) 0.1199(2) 0.058(3) Uani 1 1 d U A 1 C23 C 0.4074(8) 0.5695(5) 0.0975(2) 0.075(3) Uani 1 1 d U A 1 H23 H 0.3883 0.6166 0.0937 0.09 Uiso 1 1 calc R A 1 C24 C 0.3632(6) 0.5152(5) 0.0823(2) 0.050(3) Uani 1 1 d U A 1 C25 C 0.5111(7) 0.3535(5) 0.1134(2) 0.055(3) Uani 1 1 d U A 1 H25A H 0.4747 0.3223 0.0997 0.082 Uiso 0.5 1 calc PR A 1 H25B H 0.4961 0.3401 0.1342 0.082 Uiso 0.5 1 calc PR A 1 H25C H 0.584 0.3495 0.1098 0.082 Uiso 0.5 1 calc PR A 1 H25D H 0.5619 0.3523 0.1295 0.082 Uiso 0.5 1 calc PR A 1 H25E H 0.5404 0.3345 0.0949 0.082 Uiso 0.5 1 calc PR A 1 H25F H 0.4525 0.3251 0.1193 0.082 Uiso 0.5 1 calc PR A 1 C26 C 0.5280(9) 0.6168(6) 0.1372(3) 0.105(4) Uani 1 1 d U A 1 H26A H 0.4895 0.6589 0.1319 0.158 Uiso 0.5 1 calc PR A 1 H26B H 0.5993 0.6235 0.1318 0.158 Uiso 0.5 1 calc PR A 1 H26C H 0.5226 0.6085 0.1589 0.158 Uiso 0.5 1 calc PR A 1 H26D H 0.5848 0.6017 0.1498 0.158 Uiso 0.5 1 calc PR A 1 H26E H 0.475 0.6371 0.1499 0.158 Uiso 0.5 1 calc PR A 1 H26F H 0.5516 0.652 0.1228 0.158 Uiso 0.5 1 calc PR A 1 C27 C 0.2812(9) 0.5328(5) 0.0594(2) 0.093(4) Uani 1 1 d U A 1 H27A H 0.2572 0.4897 0.0498 0.139 Uiso 0.5 1 calc PR A 1 H27B H 0.3092 0.5641 0.044 0.139 Uiso 0.5 1 calc PR A 1 H27C H 0.2246 0.556 0.0695 0.139 Uiso 0.5 1 calc PR A 1 H27D H 0.2701 0.5836 0.0591 0.139 Uiso 0.5 1 calc PR A 1 H27E H 0.2181 0.5091 0.0649 0.139 Uiso 0.5 1 calc PR A 1 H27F H 0.3028 0.5172 0.0394 0.139 Uiso 0.5 1 calc PR A 1 C28 C 0.4006(6) 0.3216(4) 0.05260(17) 0.038(2) Uani 1 1 d U A 1 C29 C 0.3839(6) 0.2522(5) 0.06020(19) 0.046(3) Uani 1 1 d U A 1 C30 C 0.4342(7) 0.1979(5) 0.0455(2) 0.056(3) Uani 1 1 d U A 1 H30 H 0.4227 0.1507 0.0512 0.067 Uiso 1 1 calc R A 1 C31 C 0.5016(6) 0.2136(6) 0.0223(2) 0.046(4) Uani 1 1 d U A 1 C32 C 0.5183(7) 0.2779(6) 0.0139(2) 0.055(3) Uani 1 1 d U A 1 H32 H 0.5615 0.2861 -0.0028 0.066 Uiso 1 1 calc R A 1 C33 C 0.4710(8) 0.3403(5) 0.0298(2) 0.045(3) Uani 1 1 d U A 1 C34 C 0.3085(6) 0.2318(4) 0.08446(19) 0.052(3) Uani 1 1 d U A 1 H34A H 0.2778 0.2742 0.0929 0.078 Uiso 0.5 1 calc PR A 1 H34B H 0.3436 0.206 0.1004 0.078 Uiso 0.5 1 calc PR A 1 H34C H 0.2556 0.2022 0.0757 0.078 Uiso 0.5 1 calc PR A 1 H34D H 0.3068 0.1807 0.0864 0.078 Uiso 0.5 1 calc PR A 1 H34E H 0.2411 0.2489 0.079 0.078 Uiso 0.5 1 calc PR A 1 H34F H 0.3291 0.2527 0.1036 0.078 Uiso 0.5 1 calc PR A 1 C35 C 0.5551(8) 0.1528(5) 0.0054(2) 0.078(3) Uani 1 1 d U A 1 H35A H 0.5356 0.108 0.0144 0.117 Uiso 0.5 1 calc PR A 1 H35B H 0.6286 0.1586 0.0068 0.117 Uiso 0.5 1 calc PR A 1 H35C H 0.5348 0.1534 -0.0158 0.117 Uiso 0.5 1 calc PR A 1 H35D H 0.5971 0.172 -0.0108 0.117 Uiso 0.5 1 calc PR A 1 H35E H 0.5041 0.1214 -0.0032 0.117 Uiso 0.5 1 calc PR A 1 H35F H 0.5979 0.1266 0.0194 0.117 Uiso 0.5 1 calc PR A 1 C36 C 0.4951(7) 0.4145(6) 0.0223(3) 0.080(4) Uani 1 1 d U A 1 H36A H 0.5465 0.4158 0.0065 0.12 Uiso 0.5 1 calc PR A 1 H36B H 0.521 0.4383 0.0403 0.12 Uiso 0.5 1 calc PR A 1 H36C H 0.4337 0.4382 0.0154 0.12 Uiso 0.5 1 calc PR A 1 H36D H 0.4543 0.4457 0.0349 0.12 Uiso 0.5 1 calc PR A 1 H36E H 0.4798 0.4232 0.0011 0.12 Uiso 0.5 1 calc PR A 1 H36F H 0.5671 0.4234 0.0261 0.12 Uiso 0.5 1 calc PR A 1 C37 C -0.0535(7) 0.4711(4) 0.0764(2) 0.044(3) Uani 1 1 d U A 1 C38 C -0.1279(7) 0.4741(5) 0.0983(2) 0.049(3) Uani 1 1 d U A 1 C39 C -0.2142(8) 0.5116(5) 0.0935(2) 0.069(3) Uani 1 1 d U A 1 H39 H -0.2662 0.5139 0.1082 0.083 Uiso 1 1 calc R A 1 C40 C -0.2232(9) 0.5467(5) 0.0659(3) 0.081(4) Uani 1 1 d U A 1 H40 H -0.284 0.5717 0.0621 0.097 Uiso 1 1 calc R A 1 C41 C -0.1529(8) 0.5471(5) 0.0452(2) 0.078(4) Uani 1 1 d U A 1 H41 H -0.161 0.5749 0.0277 0.093 Uiso 1 1 calc R A 1 C42 C -0.0656(7) 0.5066(5) 0.0490(2) 0.054(3) Uani 1 1 d U A 1 C43 C -0.1156(7) 0.4362(4) 0.12821(19) 0.048(3) Uani 1 1 d U A 1 H43 H -0.0528 0.4074 0.1262 0.058 Uiso 1 1 calc R A 1 C44 C -0.1982(9) 0.3856(6) 0.1358(3) 0.118(5) Uani 1 1 d U A 1 H44A H -0.1901 0.3696 0.1565 0.177 Uiso 1 1 calc R A 1 H44B H -0.1945 0.3453 0.1222 0.177 Uiso 1 1 calc R A 1 H44C H -0.264 0.4087 0.1335 0.177 Uiso 1 1 calc R A 1 C45 C -0.0947(10) 0.4873(7) 0.1538(3) 0.139(5) Uani 1 1 d U A 1 H45A H -0.1578 0.5107 0.1596 0.208 Uiso 1 1 calc R A 1 H45B H -0.0454 0.5224 0.1472 0.208 Uiso 1 1 calc R A 1 H45C H -0.0674 0.4618 0.1711 0.208 Uiso 1 1 calc R A 1 C46 C 0.0106(6) 0.5077(5) 0.0257(2) 0.036(3) Uani 1 1 d U A 1 H46 H 0.0695 0.4808 0.0338 0.043 Uiso 1 1 calc R A 1 C47 C -0.0259(8) 0.4662(6) -0.0038(2) 0.081(4) Uani 1 1 d U A 1 H47A H -0.0398 0.4173 0.0014 0.121 Uiso 1 1 calc R A 1 H47B H 0.0274 0.4681 -0.0191 0.121 Uiso 1 1 calc R A 1 H47C H -0.0875 0.4881 -0.0117 0.121 Uiso 1 1 calc R A 1 C48 C 0.0520(9) 0.5776(5) 0.0162(2) 0.085(4) Uani 1 1 d U A 1 H48A H -0.0012 0.6043 0.006 0.127 Uiso 1 1 calc R A 1 H48B H 0.1091 0.5706 0.0025 0.127 Uiso 1 1 calc R A 1 H48C H 0.0748 0.6035 0.034 0.127 Uiso 1 1 calc R A 1 C49 C 0.0036(6) 0.2806(5) 0.0247(2) 0.041(4) Uani 1 1 d U A 1 C50 C -0.1030(7) 0.2788(4) 0.0261(2) 0.049(3) Uani 1 1 d U A 1 C51 C -0.1550(8) 0.2553(5) -0.0007(2) 0.053(3) Uani 1 1 d U A 1 H51 H -0.2266 0.2515 -0.0014 0.063 Uiso 1 1 calc R A 1 C52 C -0.0973(7) 0.2394(5) -0.0243(2) 0.059(3) Uani 1 1 d U A 1 H52 H -0.1311 0.2279 -0.0425 0.071 Uiso 1 1 calc R A 1 C53 C 0.0044(7) 0.2382(5) -0.0247(3) 0.053(4) Uani 1 1 d U A 1 H53 H 0.039 0.2196 -0.0416 0.063 Uiso 1 1 calc R A 1 C54 C 0.0585(8) 0.2637(5) -0.0007(2) 0.051(3) Uani 1 1 d U A 1 C55 C -0.1624(7) 0.2983(5) 0.0544(2) 0.058(3) Uani 1 1 d U A 1 H55 H -0.1145 0.3165 0.0699 0.069 Uiso 1 1 calc R A 1 C56 C -0.2198(8) 0.2344(5) 0.0671(2) 0.077(3) Uani 1 1 d U A 1 H56A H -0.2519 0.2472 0.0862 0.115 Uiso 1 1 calc R A 1 H56B H -0.1721 0.1959 0.0705 0.115 Uiso 1 1 calc R A 1 H56C H -0.2718 0.2195 0.0528 0.115 Uiso 1 1 calc R A 1 C57 C -0.2440(7) 0.3547(5) 0.0477(2) 0.070(3) Uani 1 1 d U A 1 H57A H -0.2895 0.3377 0.0319 0.105 Uiso 1 1 calc R A 1 H57B H -0.2111 0.3979 0.041 0.105 Uiso 1 1 calc R A 1 H57C H -0.2831 0.364 0.066 0.105 Uiso 1 1 calc R A 1 C58 C 0.1741(7) 0.2683(4) -0.0016(2) 0.041(3) Uani 1 1 d U A 1 H58 H 0.1972 0.2633 0.0196 0.05 Uiso 1 1 calc R A 1 C59 C 0.2058(7) 0.3423(4) -0.0114(2) 0.062(3) Uani 1 1 d U A 1 H59A H 0.2793 0.3474 -0.0093 0.093 Uiso 1 1 calc R A 1 H59B H 0.1718 0.377 0.0013 0.093 Uiso 1 1 calc R A 1 H59C H 0.1865 0.3498 -0.0324 0.093 Uiso 1 1 calc R A 1 C60 C 0.2227(8) 0.2113(5) -0.0182(2) 0.083(4) Uani 1 1 d U A 1 H60A H 0.1947 0.1664 -0.0116 0.124 Uiso 1 1 calc R A 1 H60B H 0.2957 0.2121 -0.0144 0.124 Uiso 1 1 calc R A 1 H60C H 0.2102 0.2172 -0.0398 0.124 Uiso 1 1 calc R A 1 Mo1B Mo 0.60612(6) 0.10605(4) 0.346359(15) 0.0361(2) Uani 1 1 d . B 2 B1B B 0.6029(8) 0.0281(5) 0.2819(2) 0.039(3) Uani 1 1 d . B 2 B2B B 0.8422(9) 0.1329(5) 0.3564(2) 0.040(3) Uani 1 1 d . B 2 O1B O 0.5956(4) 0.0576(3) 0.30955(11) 0.0441(18) Uani 1 1 d . B 2 O2B O 0.7399(4) 0.1343(3) 0.35616(12) 0.0424(19) Uani 1 1 d . B 2 N1B N 0.5337(5) 0.1801(4) 0.34331(17) 0.040(2) Uani 1 1 d . B 2 N2B N 0.5567(5) 0.0539(3) 0.37507(14) 0.033(2) Uani 1 1 d . B 2 C1B C 0.5049(6) -0.0139(6) 0.2684(2) 0.035(3) Uani 1 1 d U B 2 C2B C 0.4631(8) -0.0650(5) 0.2879(2) 0.040(3) Uani 1 1 d U B 2 C3B C 0.3742(7) -0.0981(5) 0.2789(2) 0.053(3) Uani 1 1 d U B 2 H3B H 0.3452 -0.1337 0.2911 0.064 Uiso 1 1 calc R B 2 C4B C 0.3285(8) -0.0787(6) 0.2522(3) 0.067(3) Uani 1 1 d U B 2 C5B C 0.3714(7) -0.0278(5) 0.2334(2) 0.054(3) Uani 1 1 d U B 2 H5B H 0.342 -0.0167 0.2145 0.065 Uiso 1 1 calc R B 2 C6B C 0.4581(8) 0.0056(5) 0.2433(2) 0.053(3) Uani 1 1 d U B 2 C7B C 0.5077(6) -0.0890(6) 0.3182(2) 0.050(4) Uani 1 1 d U B 2 H7B1 H 0.5691 -0.062 0.3225 0.074 Uiso 0.5 1 calc PR B 2 H7B2 H 0.5246 -0.1389 0.3171 0.074 Uiso 0.5 1 calc PR B 2 H7B3 H 0.4579 -0.0814 0.3341 0.074 Uiso 0.5 1 calc PR B 2 H7B4 H 0.4653 -0.1262 0.3266 0.074 Uiso 0.5 1 calc PR B 2 H7B5 H 0.5098 -0.0493 0.3321 0.074 Uiso 0.5 1 calc PR B 2 H7B6 H 0.5765 -0.1068 0.315 0.074 Uiso 0.5 1 calc PR B 2 C8B C 0.2303(7) -0.1158(6) 0.2412(2) 0.084(4) Uani 1 1 d U B 2 H8B1 H 0.2074 -0.0942 0.2225 0.126 Uiso 0.5 1 calc PR B 2 H8B2 H 0.1775 -0.111 0.2566 0.126 Uiso 0.5 1 calc PR B 2 H8B3 H 0.2442 -0.1655 0.2378 0.126 Uiso 0.5 1 calc PR B 2 H8B4 H 0.212 -0.1529 0.2554 0.126 Uiso 0.5 1 calc PR B 2 H8B5 H 0.242 -0.1362 0.2213 0.126 Uiso 0.5 1 calc PR B 2 H8B6 H 0.1752 -0.0816 0.2401 0.126 Uiso 0.5 1 calc PR B 2 C9B C 0.5057(7) 0.0633(6) 0.2231(3) 0.064(4) Uani 1 1 d U B 2 H9B1 H 0.4637 0.0698 0.2051 0.095 Uiso 0.5 1 calc PR B 2 H9B2 H 0.574 0.049 0.217 0.095 Uiso 0.5 1 calc PR B 2 H9B3 H 0.5093 0.1074 0.2343 0.095 Uiso 0.5 1 calc PR B 2 H9B4 H 0.5676 0.081 0.2325 0.095 Uiso 0.5 1 calc PR B 2 H9B5 H 0.4574 0.1018 0.2206 0.095 Uiso 0.5 1 calc PR B 2 H9B6 H 0.522 0.0434 0.2033 0.095 Uiso 0.5 1 calc PR B 2 C10B C 0.7059(6) 0.0377(4) 0.26474(16) 0.023(2) Uani 1 1 d U B 2 C11B C 0.7554(6) -0.0177(4) 0.25169(17) 0.035(3) Uani 1 1 d U B 2 C12B C 0.8539(7) -0.0088(5) 0.23964(19) 0.053(3) Uani 1 1 d U B 2 H12B H 0.89 -0.0482 0.2322 0.064 Uiso 1 1 calc R B 2 C13B C 0.8966(7) 0.0552(5) 0.23869(19) 0.050(3) Uani 1 1 d U B 2 C14B C 0.8488(8) 0.1121(5) 0.2514(2) 0.054(3) Uani 1 1 d U B 2 H14B H 0.8821 0.1561 0.2522 0.065 Uiso 1 1 calc R B 2 C15B C 0.7501(7) 0.1050(4) 0.26348(19) 0.039(3) Uani 1 1 d U B 2 C16B C 0.7149(8) -0.0911(5) 0.2541(2) 0.062(3) Uani 1 1 d U B 2 H16G H 0.7603 -0.1233 0.2435 0.094 Uiso 0.5 1 calc PR B 2 H16H H 0.6474 -0.0932 0.245 0.094 Uiso 0.5 1 calc PR B 2 H16I H 0.7107 -0.1046 0.2753 0.094 Uiso 0.5 1 calc PR B 2 H16J H 0.6519 -0.0908 0.2657 0.094 Uiso 0.5 1 calc PR B 2 H16K H 0.7649 -0.1209 0.2642 0.094 Uiso 0.5 1 calc PR B 2 H16L H 0.7016 -0.1095 0.2339 0.094 Uiso 0.5 1 calc PR B 2 C17B C 1.0051(7) 0.0727(6) 0.2263(3) 0.067(4) Uani 1 1 d U B 2 H17G H 1.0182 0.1229 0.2286 0.1 Uiso 0.5 1 calc PR B 2 H17H H 1.009 0.06 0.205 0.1 Uiso 0.5 1 calc PR B 2 H17I H 1.0558 0.0461 0.2376 0.1 Uiso 0.5 1 calc PR B 2 H17J H 1.0371 0.0298 0.2189 0.1 Uiso 0.5 1 calc PR B 2 H17K H 1.0464 0.0927 0.2425 0.1 Uiso 0.5 1 calc PR B 2 H17L H 0.9995 0.1066 0.2099 0.1 Uiso 0.5 1 calc PR B 2 C18B C 0.7055(7) 0.1722(4) 0.27468(19) 0.048(3) Uani 1 1 d U B 2 H18G H 0.753 0.2106 0.271 0.072 Uiso 0.5 1 calc PR B 2 H18H H 0.6924 0.1684 0.2963 0.072 Uiso 0.5 1 calc PR B 2 H18I H 0.6418 0.1815 0.2641 0.072 Uiso 0.5 1 calc PR B 2 H18J H 0.6385 0.1631 0.2833 0.072 Uiso 0.5 1 calc PR B 2 H18K H 0.6991 0.2053 0.258 0.072 Uiso 0.5 1 calc PR B 2 H18L H 0.7496 0.1922 0.2901 0.072 Uiso 0.5 1 calc PR B 2 C19B C 0.8954(6) 0.1943(5) 0.33922(18) 0.042(3) Uani 1 1 d U B 2 C20B C 0.9718(8) 0.1844(6) 0.3190(2) 0.058(3) Uani 1 1 d U B 2 C21B C 1.0100(6) 0.2476(6) 0.3022(3) 0.051(3) Uani 1 1 d U B 2 H21B H 1.0611 0.2408 0.2875 0.061 Uiso 1 1 calc R B 2 C22B C 0.9762(9) 0.3123(6) 0.3068(3) 0.066(4) Uani 1 1 d U B 2 C23B C 0.9030(7) 0.3187(5) 0.3264(2) 0.065(3) Uani 1 1 d U B 2 H23B H 0.8776 0.3645 0.33 0.078 Uiso 1 1 calc R B 2 C24B C 0.8595(6) 0.2643(5) 0.3424(2) 0.051(3) Uani 1 1 d U B 2 C25B C 1.0167(7) 0.1187(6) 0.3127(3) 0.063(4) Uani 1 1 d U B 2 H25G H 1.0692 0.1247 0.2973 0.095 Uiso 0.5 1 calc PR B 2 H25H H 0.9648 0.0864 0.3052 0.095 Uiso 0.5 1 calc PR B 2 H25I H 1.0471 0.0997 0.331 0.095 Uiso 0.5 1 calc PR B 2 H25J H 0.9849 0.0825 0.3251 0.095 Uiso 0.5 1 calc PR B 2 H25K H 1.0892 0.1208 0.3172 0.095 Uiso 0.5 1 calc PR B 2 H25L H 1.007 0.1075 0.2914 0.095 Uiso 0.5 1 calc PR B 2 C26B C 1.0258(9) 0.3693(6) 0.2880(3) 0.092(4) Uani 1 1 d U B 2 H26G H 1.0806 0.3489 0.276 0.139 Uiso 0.5 1 calc PR B 2 H26H H 1.0534 0.4055 0.3013 0.139 Uiso 0.5 1 calc PR B 2 H26I H 0.9752 0.3902 0.2746 0.139 Uiso 0.5 1 calc PR B 2 H26J H 0.9922 0.4141 0.2919 0.139 Uiso 0.5 1 calc PR B 2 H26K H 1.0194 0.3575 0.2666 0.139 Uiso 0.5 1 calc PR B 2 H26L H 1.0975 0.3729 0.2933 0.139 Uiso 0.5 1 calc PR B 2 C27B C 0.7728(8) 0.2822(5) 0.3631(2) 0.066(3) Uani 1 1 d U B 2 H27G H 0.7475 0.2394 0.3727 0.098 Uiso 0.5 1 calc PR B 2 H27H H 0.7182 0.3042 0.3516 0.098 Uiso 0.5 1 calc PR B 2 H27I H 0.7965 0.3147 0.3787 0.098 Uiso 0.5 1 calc PR B 2 H27J H 0.7606 0.3328 0.3626 0.098 Uiso 0.5 1 calc PR B 2 H27K H 0.7899 0.268 0.3837 0.098 Uiso 0.5 1 calc PR B 2 H27L H 0.7117 0.2575 0.3566 0.098 Uiso 0.5 1 calc PR B 2 C28B C 0.8999(7) 0.0735(5) 0.37250(18) 0.041(3) Uani 1 1 d U B 2 C29B C 0.9683(7) 0.0833(5) 0.3957(2) 0.037(3) Uani 1 1 d U B 2 C30B C 1.0174(7) 0.0341(6) 0.4097(3) 0.054(3) Uani 1 1 d U B 2 H30B H 1.0657 0.0462 0.4246 0.065 Uiso 1 1 calc R B 2 C31B C 0.9997(7) -0.0385(7) 0.4027(3) 0.069(5) Uani 1 1 d U B 2 C32B C 0.9364(7) -0.0508(5) 0.3795(2) 0.054(3) Uani 1 1 d U B 2 H32B H 0.9281 -0.0979 0.373 0.065 Uiso 1 1 calc R B 2 C33B C 0.8828(7) 0.0007(5) 0.36452(19) 0.044(3) Uani 1 1 d U B 2 C34B C 0.9934(6) 0.1571(6) 0.4063(3) 0.056(4) Uani 1 1 d U B 2 H34G H 0.953 0.191 0.395 0.084 Uiso 0.5 1 calc PR B 2 H34H H 1.0655 0.1664 0.403 0.084 Uiso 0.5 1 calc PR B 2 H34I H 0.9779 0.1614 0.4278 0.084 Uiso 0.5 1 calc PR B 2 H34J H 1.0446 0.1548 0.4222 0.084 Uiso 0.5 1 calc PR B 2 H34K H 0.9321 0.1795 0.4142 0.084 Uiso 0.5 1 calc PR B 2 H34L H 1.0197 0.1845 0.3894 0.084 Uiso 0.5 1 calc PR B 2 C35B C 1.0536(9) -0.0953(5) 0.4191(2) 0.082(3) Uani 1 1 d U B 2 H35G H 1.03 -0.1409 0.4118 0.124 Uiso 0.5 1 calc PR B 2 H35H H 1.0397 -0.0913 0.4406 0.124 Uiso 0.5 1 calc PR B 2 H35I H 1.1265 -0.0911 0.4156 0.124 Uiso 0.5 1 calc PR B 2 H35J H 1.1008 -0.0746 0.4336 0.124 Uiso 0.5 1 calc PR B 2 H35K H 1.0911 -0.1242 0.4047 0.124 Uiso 0.5 1 calc PR B 2 H35L H 1.0043 -0.1244 0.4298 0.124 Uiso 0.5 1 calc PR B 2 C36B C 0.8109(7) -0.0177(5) 0.3399(2) 0.062(3) Uani 1 1 d U B 2 H36G H 0.7801 0.0252 0.3319 0.093 Uiso 0.5 1 calc PR B 2 H36H H 0.7578 -0.0484 0.3478 0.093 Uiso 0.5 1 calc PR B 2 H36I H 0.8475 -0.0418 0.3238 0.093 Uiso 0.5 1 calc PR B 2 H36J H 0.8102 -0.0686 0.3371 0.093 Uiso 0.5 1 calc PR B 2 H36K H 0.8325 0.005 0.3212 0.093 Uiso 0.5 1 calc PR B 2 H36L H 0.7428 -0.0016 0.3452 0.093 Uiso 0.5 1 calc PR B 2 C37B C 0.4458(7) 0.2222(4) 0.3479(2) 0.045(3) Uani 1 1 d U B 2 C38B C 0.4361(8) 0.2585(5) 0.3759(2) 0.060(3) Uani 1 1 d U B 2 C39B C 0.3419(8) 0.2965(5) 0.3790(3) 0.073(3) Uani 1 1 d U B 2 H39B H 0.3301 0.3223 0.3969 0.087 Uiso 1 1 calc R B 2 C40B C 0.2669(9) 0.2967(5) 0.3564(3) 0.084(4) Uani 1 1 d U B 2 H40B H 0.2055 0.3216 0.3595 0.101 Uiso 1 1 calc R B 2 C41B C 0.2822(8) 0.2620(5) 0.3308(3) 0.076(3) Uani 1 1 d U B 2 H41B H 0.2313 0.2628 0.3157 0.091 Uiso 1 1 calc R B 2 C42B C 0.3734(7) 0.2239(5) 0.3255(2) 0.052(3) Uani 1 1 d U B 2 C43B C 0.5175(9) 0.2526(7) 0.4005(3) 0.088(4) Uani 1 1 d U B 2 H43B H 0.5743 0.2224 0.3932 0.106 Uiso 1 1 calc R B 2 C44B C 0.4724(9) 0.2213(6) 0.4288(3) 0.079(4) Uani 1 1 d U B 2 H44D H 0.4229 0.2539 0.4373 0.119 Uiso 1 1 calc R B 2 H44E H 0.5263 0.2127 0.4434 0.119 Uiso 1 1 calc R B 2 H44F H 0.4388 0.177 0.4238 0.119 Uiso 1 1 calc R B 2 C45B C 0.5580(10) 0.3273(5) 0.4076(3) 0.100(4) Uani 1 1 d U B 2 H45D H 0.5924 0.3462 0.3898 0.149 Uiso 1 1 calc R B 2 H45E H 0.6058 0.3249 0.4244 0.149 Uiso 1 1 calc R B 2 H45F H 0.5013 0.3579 0.413 0.149 Uiso 1 1 calc R B 2 C46B C 0.3897(7) 0.1860(5) 0.2962(2) 0.061(3) Uani 1 1 d U B 2 H46B H 0.4427 0.1495 0.2994 0.074 Uiso 1 1 calc R B 2 C47B C 0.2920(11) 0.1490(7) 0.2846(3) 0.138(5) Uani 1 1 d U B 2 H47D H 0.2389 0.184 0.2812 0.207 Uiso 1 1 calc R B 2 H47E H 0.2688 0.1149 0.2995 0.207 Uiso 1 1 calc R B 2 H47F H 0.3068 0.1248 0.2656 0.207 Uiso 1 1 calc R B 2 C48B C 0.4270(9) 0.2353(6) 0.2727(2) 0.100(4) Uani 1 1 d U B 2 H48D H 0.3765 0.2721 0.2693 0.15 Uiso 1 1 calc R B 2 H48E H 0.4385 0.2097 0.2539 0.15 Uiso 1 1 calc R B 2 H48F H 0.4906 0.2567 0.2794 0.15 Uiso 1 1 calc R B 2 C49B C 0.4991(6) 0.0330(5) 0.3986(3) 0.035(4) Uani 1 1 d U B 2 C50B C 0.5558(8) 0.0135(4) 0.4254(2) 0.041(3) Uani 1 1 d U B 2 C51B C 0.5012(7) -0.0049(6) 0.4517(3) 0.056(4) Uani 1 1 d U B 2 H51B H 0.5366 -0.0134 0.4699 0.067 Uiso 1 1 calc R B 2 C52B C 0.3963(8) -0.0105(5) 0.4510(2) 0.059(3) Uani 1 1 d U B 2 H52B H 0.3597 -0.0263 0.4681 0.071 Uiso 1 1 calc R B 2 C53B C 0.3455(9) 0.0080(5) 0.4240(2) 0.059(3) Uani 1 1 d U B 2 H53B H 0.2737 0.006 0.4239 0.07 Uiso 1 1 calc R B 2 C54B C 0.3922(8) 0.0284(4) 0.3983(2) 0.048(3) Uani 1 1 d U B 2 C55B C 0.6677(8) 0.0194(5) 0.4252(2) 0.056(3) Uani 1 1 d U B 2 H55B H 0.6911 0.0141 0.404 0.068 Uiso 1 1 calc R B 2 C56B C 0.7248(8) -0.0382(5) 0.4450(2) 0.077(3) Uani 1 1 d U B 2 H56D H 0.7211 -0.0251 0.4663 0.115 Uiso 1 1 calc R B 2 H56E H 0.7958 -0.0409 0.4388 0.115 Uiso 1 1 calc R B 2 H56F H 0.6924 -0.0838 0.4421 0.115 Uiso 1 1 calc R B 2 C57B C 0.7061(9) 0.0898(6) 0.4369(3) 0.091(4) Uani 1 1 d U B 2 H57D H 0.673 0.1278 0.4258 0.137 Uiso 1 1 calc R B 2 H57E H 0.7795 0.0927 0.4339 0.137 Uiso 1 1 calc R B 2 H57F H 0.6904 0.094 0.4583 0.137 Uiso 1 1 calc R B 2 C58B C 0.3338(7) 0.0502(5) 0.3721(2) 0.051(3) Uani 1 1 d U B 2 H58B H 0.3824 0.0684 0.3567 0.061 Uiso 1 1 calc R B 2 C59B C 0.2611(8) 0.1085(5) 0.3796(3) 0.077(4) Uani 1 1 d U B 2 H59D H 0.2077 0.0905 0.3928 0.116 Uiso 1 1 calc R B 2 H59E H 0.2308 0.1267 0.3611 0.116 Uiso 1 1 calc R B 2 H59F H 0.2977 0.1462 0.3899 0.116 Uiso 1 1 calc R B 2 C60B C 0.2804(8) -0.0134(5) 0.3586(2) 0.070(3) Uani 1 1 d U B 2 H60D H 0.3307 -0.0489 0.3532 0.104 Uiso 1 1 calc R B 2 H60E H 0.2429 0.0008 0.3406 0.104 Uiso 1 1 calc R B 2 H60F H 0.2333 -0.0329 0.3734 0.104 Uiso 1 1 calc R B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0355(4) 0.0349(5) 0.0365(4) 0.0031(4) -0.0038(5) 0.0018(4) B1 0.053(7) 0.023(6) 0.045(7) -0.022(5) 0.005(7) 0.003(6) B2 0.041(7) 0.038(7) 0.045(7) 0.009(6) -0.011(6) 0.004(6) O1 0.054(4) 0.039(3) 0.035(3) 0.014(3) 0.004(3) 0.005(3) O2 0.029(4) 0.047(4) 0.056(4) 0.015(3) -0.008(3) -0.005(3) N1 0.054(4) 0.015(4) 0.040(4) -0.004(4) -0.013(5) 0.001(4) N2 0.044(5) 0.037(4) 0.036(4) -0.007(4) -0.024(4) -0.009(4) C1 0.042(5) 0.043(5) 0.019(5) 0.000(4) 0.009(4) -0.001(4) C2 0.048(5) 0.042(5) 0.039(5) 0.018(4) 0.002(5) 0.006(5) C3 0.053(6) 0.054(5) 0.040(5) 0.005(4) 0.009(4) 0.001(5) C4 0.044(5) 0.056(5) 0.057(5) -0.005(5) 0.006(5) -0.010(5) C5 0.060(5) 0.050(5) 0.051(5) 0.006(5) -0.007(5) -0.007(5) C6 0.040(5) 0.046(5) 0.037(5) 0.014(4) -0.011(4) -0.009(5) C7 0.052(6) 0.052(6) 0.048(6) 0.005(5) 0.008(4) -0.005(4) C8 0.065(6) 0.076(6) 0.068(6) -0.001(5) -0.001(5) -0.008(5) C9 0.057(5) 0.051(6) 0.047(6) -0.008(5) 0.004(5) -0.006(5) C10 0.046(5) 0.031(5) 0.035(5) 0.011(4) 0.012(4) 0.003(4) C11 0.053(5) 0.044(5) 0.043(5) 0.007(4) 0.002(4) -0.006(5) C12 0.052(5) 0.057(5) 0.040(5) -0.003(4) 0.000(4) 0.004(5) C13 0.052(5) 0.066(5) 0.040(5) -0.007(5) -0.002(5) -0.004(5) C14 0.046(5) 0.044(5) 0.042(5) -0.007(4) 0.001(4) -0.017(4) C15 0.048(5) 0.045(5) 0.030(5) -0.001(4) 0.010(4) -0.004(5) C16 0.042(5) 0.041(5) 0.050(5) 0.013(4) -0.016(4) -0.009(4) C17 0.062(6) 0.071(6) 0.073(6) -0.006(5) -0.005(5) -0.009(5) C18 0.079(6) 0.066(6) 0.062(6) -0.004(5) 0.012(5) -0.006(5) C19 0.033(4) 0.050(5) 0.043(5) 0.006(4) -0.002(4) -0.010(4) C20 0.022(4) 0.055(6) 0.040(5) -0.011(5) 0.007(4) -0.014(4) C21 0.059(6) 0.076(6) 0.052(6) 0.001(5) 0.007(5) 0.012(5) C22 0.053(6) 0.060(6) 0.060(6) -0.011(5) 0.025(5) -0.032(5) C23 0.078(6) 0.067(6) 0.079(6) -0.003(5) 0.006(5) -0.009(5) C24 0.050(5) 0.048(5) 0.053(5) -0.004(5) -0.009(5) -0.007(4) C25 0.055(6) 0.070(6) 0.040(5) 0.000(5) -0.001(4) 0.022(5) C26 0.102(7) 0.116(7) 0.098(7) -0.029(6) 0.007(6) -0.034(6) C27 0.104(7) 0.070(6) 0.105(7) 0.012(5) -0.005(6) -0.006(6) C28 0.033(5) 0.046(5) 0.035(4) 0.000(4) -0.005(4) -0.003(4) C29 0.041(5) 0.048(5) 0.050(5) -0.001(4) -0.003(4) -0.003(5) C30 0.044(5) 0.056(5) 0.068(6) -0.010(5) 0.001(5) -0.008(5) C31 0.048(6) 0.048(6) 0.043(6) -0.024(5) -0.005(4) -0.002(4) C32 0.048(5) 0.072(6) 0.044(6) -0.006(5) -0.005(4) -0.001(5) C33 0.053(5) 0.041(5) 0.042(5) 0.000(5) 0.000(5) 0.005(5) C34 0.051(5) 0.043(5) 0.061(6) 0.012(4) 0.017(5) -0.002(4) C35 0.065(6) 0.084(6) 0.086(6) -0.028(5) 0.009(5) 0.002(5) C36 0.077(7) 0.089(7) 0.073(7) 0.014(6) 0.022(5) 0.004(5) C37 0.049(5) 0.031(5) 0.050(5) 0.002(5) -0.008(5) 0.006(4) C38 0.044(5) 0.036(5) 0.065(5) -0.006(4) -0.018(5) 0.007(4) C39 0.054(6) 0.075(6) 0.078(6) -0.017(5) 0.002(5) 0.013(5) C40 0.073(6) 0.068(6) 0.100(7) -0.007(5) -0.027(5) 0.018(5) C41 0.082(6) 0.074(6) 0.078(6) 0.005(5) -0.025(5) 0.017(5) C42 0.056(6) 0.047(5) 0.057(5) -0.001(5) -0.009(5) 0.008(5) C43 0.039(5) 0.040(5) 0.065(5) -0.019(4) 0.000(5) 0.009(4) C44 0.100(7) 0.118(7) 0.136(8) 0.021(6) 0.003(6) -0.013(6) C45 0.173(8) 0.130(8) 0.114(7) -0.008(6) -0.010(7) -0.004(7) C46 0.040(5) 0.027(5) 0.041(5) 0.014(4) -0.022(4) -0.004(4) C47 0.093(7) 0.075(6) 0.074(6) 0.007(5) -0.005(5) -0.009(5) C48 0.103(6) 0.070(6) 0.082(6) 0.012(5) -0.019(6) -0.016(6) C49 0.047(6) 0.034(6) 0.044(6) 0.000(5) -0.003(4) -0.003(4) C50 0.045(5) 0.044(5) 0.057(5) 0.010(4) -0.008(5) -0.003(5) C51 0.049(5) 0.046(5) 0.062(6) -0.003(5) -0.014(5) -0.003(5) C52 0.071(6) 0.052(5) 0.055(5) -0.006(5) -0.018(5) -0.004(5) C53 0.067(6) 0.044(6) 0.046(6) 0.006(5) -0.004(5) 0.010(5) C54 0.055(6) 0.044(5) 0.052(5) 0.011(5) 0.002(5) 0.000(5) C55 0.055(5) 0.048(5) 0.070(6) -0.013(5) -0.004(5) -0.010(5) C56 0.074(6) 0.072(6) 0.083(6) -0.005(5) 0.000(5) 0.006(5) C57 0.064(6) 0.060(6) 0.087(6) -0.013(5) -0.010(5) 0.005(5) C58 0.043(5) 0.051(5) 0.030(5) 0.004(4) 0.002(4) 0.002(5) C59 0.058(6) 0.063(6) 0.065(6) 0.014(5) -0.002(5) -0.020(5) C60 0.084(6) 0.079(6) 0.085(6) -0.001(5) 0.012(5) 0.004(5) Mo1B 0.0362(4) 0.0355(5) 0.0366(4) -0.0029(4) 0.0031(6) -0.0007(4) B1B 0.032(7) 0.026(6) 0.061(8) -0.002(6) 0.005(7) 0.021(6) B2B 0.049(7) 0.051(8) 0.020(7) -0.011(5) -0.013(6) -0.032(6) O1B 0.064(4) 0.044(4) 0.024(3) -0.010(3) 0.014(3) 0.000(3) O2B 0.035(4) 0.040(4) 0.052(4) -0.006(3) -0.003(3) -0.013(3) N1B 0.029(4) 0.041(5) 0.049(5) -0.010(5) 0.005(5) 0.012(4) N2B 0.033(5) 0.040(5) 0.027(4) -0.014(4) 0.000(4) -0.004(4) C1B 0.031(6) 0.039(6) 0.034(6) -0.013(5) -0.005(4) -0.001(4) C2B 0.038(5) 0.040(5) 0.043(5) -0.008(5) 0.001(5) -0.001(5) C3B 0.059(6) 0.046(5) 0.054(5) -0.001(5) 0.010(5) 0.001(5) C4B 0.056(6) 0.067(6) 0.079(6) -0.013(5) -0.005(5) -0.009(5) C5B 0.059(6) 0.058(5) 0.044(5) 0.005(5) -0.012(5) 0.005(5) C6B 0.056(5) 0.042(5) 0.059(6) -0.002(5) 0.004(5) -0.001(5) C7B 0.054(6) 0.052(6) 0.043(6) 0.001(5) -0.008(4) -0.008(4) C8B 0.061(6) 0.101(7) 0.089(6) -0.002(5) -0.013(5) -0.023(5) C9B 0.071(7) 0.069(6) 0.051(6) 0.028(5) -0.011(4) -0.012(5) C10B 0.027(5) 0.023(4) 0.020(4) -0.006(4) 0.001(4) 0.005(4) C11B 0.040(5) 0.042(5) 0.025(4) 0.004(4) -0.013(4) 0.001(4) C12B 0.052(6) 0.064(6) 0.044(5) 0.000(5) -0.005(4) 0.007(5) C13B 0.049(5) 0.062(6) 0.040(5) 0.012(5) 0.003(5) 0.000(5) C14B 0.059(6) 0.057(5) 0.046(5) 0.008(5) 0.001(5) -0.006(5) C15B 0.041(5) 0.041(5) 0.035(5) 0.010(4) 0.009(4) -0.002(4) C16B 0.069(6) 0.057(6) 0.061(6) -0.013(5) -0.011(5) 0.017(5) C17B 0.061(7) 0.069(7) 0.070(7) 0.005(5) 0.002(5) 0.004(5) C18B 0.050(5) 0.042(5) 0.053(5) 0.003(4) 0.008(5) -0.014(5) C19B 0.034(5) 0.052(5) 0.040(5) 0.007(4) -0.007(4) -0.002(5) C20B 0.055(5) 0.063(6) 0.055(6) 0.009(5) -0.006(5) -0.016(5) C21B 0.038(6) 0.074(7) 0.040(6) 0.009(5) -0.007(4) -0.029(5) C22B 0.071(6) 0.065(6) 0.061(6) 0.012(6) -0.010(5) -0.006(6) C23B 0.064(6) 0.060(6) 0.071(6) 0.002(5) -0.011(5) -0.013(5) C24B 0.050(5) 0.046(5) 0.056(5) 0.002(5) -0.001(5) -0.006(4) C25B 0.051(6) 0.079(7) 0.060(6) 0.003(5) 0.004(5) -0.029(5) C26B 0.093(7) 0.095(7) 0.089(7) 0.017(6) -0.015(6) -0.046(6) C27B 0.074(6) 0.042(5) 0.081(6) -0.006(5) 0.012(5) 0.002(5) C28B 0.038(5) 0.048(5) 0.037(5) -0.003(4) 0.012(4) -0.003(5) C29B 0.029(5) 0.044(5) 0.038(5) -0.007(5) 0.013(5) -0.001(5) C30B 0.042(6) 0.069(6) 0.051(6) 0.006(5) 0.004(5) -0.014(5) C31B 0.067(7) 0.068(7) 0.070(7) 0.016(6) 0.012(5) 0.008(5) C32B 0.049(6) 0.054(6) 0.061(6) 0.007(5) 0.008(5) 0.003(5) C33B 0.042(5) 0.042(5) 0.049(5) -0.001(4) 0.006(4) -0.005(5) C34B 0.056(6) 0.062(7) 0.050(6) -0.007(5) -0.002(4) 0.010(5) C35B 0.083(6) 0.067(6) 0.097(6) 0.027(6) -0.007(6) -0.004(6) C36B 0.058(6) 0.069(6) 0.059(6) -0.011(5) -0.002(5) -0.006(5) C37B 0.051(5) 0.038(5) 0.045(5) 0.006(5) 0.008(5) 0.005(5) C38B 0.066(6) 0.041(5) 0.074(6) 0.005(5) 0.015(5) 0.001(5) C39B 0.083(6) 0.062(6) 0.073(6) -0.005(5) 0.032(5) 0.007(5) C40B 0.083(7) 0.074(6) 0.096(7) 0.021(6) 0.015(6) 0.022(5) C41B 0.068(6) 0.082(6) 0.077(6) 0.015(5) 0.007(6) 0.010(6) C42B 0.041(5) 0.052(6) 0.062(5) 0.007(5) 0.018(5) 0.019(4) C43B 0.093(7) 0.078(7) 0.092(8) -0.017(6) 0.011(6) -0.003(6) C44B 0.095(7) 0.073(7) 0.070(7) 0.000(6) 0.010(6) -0.003(6) C45B 0.114(7) 0.078(7) 0.107(7) -0.014(6) 0.014(6) -0.013(6) C46B 0.051(5) 0.069(6) 0.064(6) 0.012(5) 0.002(5) 0.002(5) C47B 0.116(8) 0.149(8) 0.149(8) -0.020(7) 0.012(7) -0.020(7) C48B 0.134(8) 0.087(7) 0.080(6) 0.009(6) 0.013(6) 0.013(6) C49B 0.039(6) 0.025(6) 0.040(6) -0.004(5) 0.009(4) -0.010(4) C50B 0.043(5) 0.030(5) 0.048(5) 0.000(5) 0.004(5) 0.000(5) C51B 0.073(7) 0.052(6) 0.042(6) -0.002(5) 0.001(5) -0.001(5) C52B 0.073(6) 0.048(5) 0.057(5) 0.000(5) 0.025(5) -0.002(5) C53B 0.058(6) 0.060(6) 0.058(6) 0.011(5) 0.016(5) 0.001(5) C54B 0.057(6) 0.027(5) 0.059(5) -0.001(4) 0.018(5) -0.003(5) C55B 0.063(6) 0.062(6) 0.044(6) 0.006(5) -0.002(5) -0.002(5) C56B 0.086(6) 0.069(6) 0.074(6) 0.004(5) -0.013(5) 0.006(5) C57B 0.092(7) 0.091(7) 0.090(7) -0.010(6) 0.001(6) -0.011(6) C58B 0.045(5) 0.049(5) 0.057(5) 0.007(5) 0.004(5) 0.008(5) C59B 0.071(6) 0.065(6) 0.096(7) 0.014(5) 0.017(5) 0.004(5) C60B 0.064(6) 0.061(6) 0.083(6) 0.005(5) -0.007(5) -0.006(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N2 1.737(6) . ? Mo N1 1.745(6) . ? Mo O1 1.870(5) . ? Mo O2 1.883(5) . ? B1 O1 1.338(11) . ? B1 C1 1.542(13) . ? B1 C10 1.596(13) . ? B2 O2 1.361(11) . ? B2 C19 1.564(13) . ? B2 C28 1.606(13) . ? N1 C37 1.384(11) . ? N2 C49 1.439(11) . ? C1 C6 1.413(12) . ? C1 C2 1.450(12) . ? C2 C3 1.402(12) . ? C2 C7 1.490(12) . ? C3 C4 1.327(12) . ? C4 C5 1.431(12) . ? C4 C8 1.502(12) . ? C5 C6 1.393(12) . ? C6 C9 1.488(13) . ? C10 C15 1.417(11) . ? C10 C11 1.430(11) . ? C11 C12 1.382(11) . ? C11 C16 1.525(11) . ? C12 C13 1.394(12) . ? C13 C14 1.372(12) . ? C13 C17 1.536(12) . ? C14 C15 1.363(11) . ? C15 C18 1.565(12) . ? C19 C24 1.393(11) . ? C19 C20 1.442(11) . ? C20 C21 1.263(13) . ? C20 C25 1.631(13) . ? C21 C22 1.424(14) . ? C22 C23 1.463(13) . ? C22 C26 1.551(15) . ? C23 C24 1.371(12) . ? C24 C27 1.527(13) . ? C28 C29 1.385(11) . ? C28 C33 1.422(12) . ? C29 C30 1.395(12) . ? C29 C34 1.519(11) . ? C30 C31 1.395(13) . ? C31 C32 1.303(14) . ? C31 C35 1.554(13) . ? C32 C33 1.521(13) . ? C33 C36 1.490(14) . ? C37 C38 1.385(12) . ? C37 C42 1.405(12) . ? C38 C39 1.365(12) . ? C38 C43 1.524(12) . ? C39 C40 1.401(13) . ? C40 C41 1.308(14) . ? C41 C42 1.399(13) . ? C42 C46 1.445(12) . ? C43 C44 1.496(13) . ? C43 C45 1.526(14) . ? C46 C48 1.504(12) . ? C46 C47 1.608(14) . ? C49 C54 1.382(13) . ? C49 C50 1.410(11) . ? C50 C51 1.448(13) . ? C50 C55 1.528(12) . ? C51 C52 1.333(13) . ? C52 C53 1.344(11) . ? C53 C54 1.374(14) . ? C54 C58 1.530(13) . ? C55 C56 1.546(12) . ? C55 C57 1.553(12) . ? C58 C60 1.463(12) . ? C58 C59 1.538(11) . ? Mo1B N1B 1.714(7) . ? Mo1B N2B 1.746(7) . ? Mo1B O1B 1.887(5) . ? Mo1B O2B 1.899(6) . ? B1B O1B 1.358(11) . ? B1B C10B 1.571(13) . ? B1B C1B 1.636(14) . ? B2B O2B 1.352(12) . ? B2B C28B 1.543(13) . ? B2B C19B 1.568(13) . ? N1B C37B 1.427(11) . ? N2B C49B 1.356(12) . ? C1B C6B 1.331(14) . ? C1B C2B 1.416(13) . ? C2B C3B 1.391(12) . ? C2B C7B 1.542(13) . ? C3B C4B 1.383(13) . ? C4B C5B 1.402(13) . ? C4B C8B 1.556(13) . ? C5B C6B 1.383(13) . ? C6B C9B 1.557(14) . ? C10B C11B 1.373(10) . ? C10B C15B 1.413(10) . ? C11B C12B 1.418(11) . ? C11B C16B 1.505(12) . ? C12B C13B 1.347(12) . ? C13B C14B 1.379(12) . ? C13B C17B 1.572(12) . ? C14B C15B 1.417(12) . ? C15B C18B 1.497(11) . ? C19B C20B 1.365(13) . ? C19B C24B 1.424(11) . ? C20B C25B 1.415(14) . ? C20B C21B 1.508(14) . ? C21B C22B 1.329(15) . ? C22B C23B 1.309(14) . ? C22B C26B 1.523(16) . ? C23B C24B 1.383(12) . ? C24B C27B 1.512(12) . ? C28B C29B 1.386(12) . ? C28B C33B 1.453(11) . ? C29B C30B 1.300(13) . ? C29B C34B 1.523(13) . ? C30B C31B 1.440(16) . ? C31B C32B 1.351(15) . ? C31B C35B 1.487(15) . ? C32B C33B 1.383(12) . ? C33B C36B 1.492(11) . ? C37B C42B 1.381(12) . ? C37B C38B 1.430(13) . ? C38B C39B 1.448(13) . ? C38B C43B 1.539(16) . ? C39B C40B 1.410(15) . ? C40B C41B 1.335(14) . ? C41B C42B 1.429(12) . ? C42B C46B 1.506(13) . ? C43B C44B 1.516(17) . ? C43B C45B 1.558(15) . ? C46B C48B 1.491(13) . ? C46B C47B 1.561(15) . ? C49B C54B 1.415(12) . ? C49B C50B 1.456(14) . ? C50B C51B 1.420(14) . ? C50B C55B 1.483(14) . ? C51B C52B 1.391(12) . ? C52B C53B 1.422(13) . ? C53B C54B 1.355(13) . ? C54B C58B 1.462(12) . ? C55B C57B 1.528(13) . ? C55B C56B 1.597(13) . ? C58B C59B 1.509(12) . ? C58B C60B 1.526(12) . ? 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 N2 Mo N1 106.8(3) . . ? N2 Mo O1 109.6(3) . . ? N1 Mo O1 108.2(3) . . ? N2 Mo O2 110.5(3) . . ? N1 Mo O2 108.5(3) . . ? O1 Mo O2 113.1(2) . . ? O1 B1 C1 116.1(8) . . ? O1 B1 C10 114.9(8) . . ? C1 B1 C10 128.8(8) . . ? O2 B2 C19 117.8(8) . . ? O2 B2 C28 117.2(8) . . ? C19 B2 C28 124.9(8) . . ? B1 O1 Mo 174.5(6) . . ? B2 O2 Mo 158.4(6) . . ? C37 N1 Mo 154.7(6) . . ? C49 N2 Mo 163.4(6) . . ? C6 C1 C2 116.6(8) . . ? C6 C1 B1 123.9(8) . . ? C2 C1 B1 119.5(8) . . ? C3 C2 C1 119.3(8) . . ? C3 C2 C7 117.4(8) . . ? C1 C2 C7 123.3(8) . . ? C4 C3 C2 124.1(9) . . ? C3 C4 C5 117.2(9) . . ? C3 C4 C8 125.1(9) . . ? C5 C4 C8 117.6(8) . . ? C6 C5 C4 121.9(8) . . ? C5 C6 C1 120.4(8) . . ? C5 C6 C9 120.5(8) . . ? C1 C6 C9 119.1(8) . . ? C15 C10 C11 114.6(8) . . ? C15 C10 B1 124.3(7) . . ? C11 C10 B1 120.7(7) . . ? C12 C11 C10 121.5(8) . . ? C12 C11 C16 117.4(8) . . ? C10 C11 C16 121.2(8) . . ? C11 C12 C13 120.8(9) . . ? C14 C13 C12 118.6(9) . . ? C14 C13 C17 125.3(9) . . ? C12 C13 C17 115.9(8) . . ? C15 C14 C13 121.0(8) . . ? C14 C15 C10 123.1(8) . . ? C14 C15 C18 120.1(8) . . ? C10 C15 C18 116.7(8) . . ? C24 C19 C20 117.4(8) . . ? C24 C19 B2 120.5(8) . . ? C20 C19 B2 121.9(7) . . ? C21 C20 C19 123.6(9) . . ? C21 C20 C25 118.3(9) . . ? C19 C20 C25 118.0(7) . . ? C20 C21 C22 120.7(10) . . ? C21 C22 C23 118.5(9) . . ? C21 C22 C26 126.4(10) . . ? C23 C22 C26 115.1(9) . . ? C24 C23 C22 118.1(9) . . ? C23 C24 C19 121.4(9) . . ? C23 C24 C27 117.8(8) . . ? C19 C24 C27 120.7(8) . . ? C29 C28 C33 121.3(8) . . ? C29 C28 B2 122.5(8) . . ? C33 C28 B2 116.2(8) . . ? C28 C29 C30 121.4(8) . . ? C28 C29 C34 121.5(8) . . ? C30 C29 C34 117.1(8) . . ? C29 C30 C31 119.5(9) . . ? C32 C31 C30 121.5(10) . . ? C32 C31 C35 119.2(9) . . ? C30 C31 C35 119.3(9) . . ? C31 C32 C33 122.4(9) . . ? C28 C33 C36 122.6(9) . . ? C28 C33 C32 113.8(8) . . ? C36 C33 C32 123.6(9) . . ? C38 C37 N1 119.1(8) . . ? C38 C37 C42 120.7(8) . . ? N1 C37 C42 120.2(8) . . ? C39 C38 C37 120.3(9) . . ? C39 C38 C43 118.4(8) . . ? C37 C38 C43 121.3(8) . . ? C38 C39 C40 117.4(9) . . ? C41 C40 C39 123.9(11) . . ? C40 C41 C42 119.9(10) . . ? C41 C42 C37 117.7(9) . . ? C41 C42 C46 118.8(9) . . ? C37 C42 C46 123.4(8) . . ? C44 C43 C38 115.2(8) . . ? C44 C43 C45 112.2(9) . . ? C38 C43 C45 111.6(8) . . ? C42 C46 C48 117.9(8) . . ? C42 C46 C47 111.7(7) . . ? C48 C46 C47 108.4(8) . . ? C54 C49 C50 123.7(9) . . ? C54 C49 N2 119.6(8) . . ? C50 C49 N2 116.7(8) . . ? C49 C50 C51 116.4(9) . . ? C49 C50 C55 122.9(9) . . ? C51 C50 C55 120.7(9) . . ? C52 C51 C50 116.7(9) . . ? C51 C52 C53 125.8(10) . . ? C52 C53 C54 120.3(10) . . ? C53 C54 C49 116.4(9) . . ? C53 C54 C58 121.2(9) . . ? C49 C54 C58 122.3(9) . . ? C50 C55 C56 111.2(7) . . ? C50 C55 C57 111.7(8) . . ? C56 C55 C57 106.1(8) . . ? C60 C58 C54 114.2(8) . . ? C60 C58 C59 115.0(8) . . ? C54 C58 C59 109.4(7) . . ? N1B Mo1B N2B 108.7(3) . . ? N1B Mo1B O1B 107.1(3) . . ? N2B Mo1B O1B 109.2(3) . . ? N1B Mo1B O2B 107.7(3) . . ? N2B Mo1B O2B 110.0(3) . . ? O1B Mo1B O2B 114.1(2) . . ? O1B B1B C10B 117.0(8) . . ? O1B B1B C1B 118.6(8) . . ? C10B B1B C1B 124.4(8) . . ? O2B B2B C28B 120.8(8) . . ? O2B B2B C19B 115.4(8) . . ? C28B B2B C19B 123.8(9) . . ? B1B O1B Mo1B 170.4(6) . . ? B2B O2B Mo1B 158.0(6) . . ? C37B N1B Mo1B 155.3(6) . . ? C49B N2B Mo1B 160.7(7) . . ? C6B C1B C2B 121.6(9) . . ? C6B C1B B1B 122.5(10) . . ? C2B C1B B1B 115.1(9) . . ? C3B C2B C1B 117.9(9) . . ? C3B C2B C7B 116.0(8) . . ? C1B C2B C7B 126.1(9) . . ? C4B C3B C2B 119.5(9) . . ? C3B C4B C5B 121.4(9) . . ? C3B C4B C8B 120.8(10) . . ? C5B C4B C8B 117.7(10) . . ? C6B C5B C4B 117.7(9) . . ? C1B C6B C5B 121.5(9) . . ? C1B C6B C9B 119.8(10) . . ? C5B C6B C9B 118.5(9) . . ? C11B C10B C15B 119.1(8) . . ? C11B C10B B1B 121.9(7) . . ? C15B C10B B1B 118.9(7) . . ? C10B C11B C12B 120.4(8) . . ? C10B C11B C16B 121.2(8) . . ? C12B C11B C16B 117.6(8) . . ? C13B C12B C11B 120.3(9) . . ? C12B C13B C14B 120.7(9) . . ? C12B C13B C17B 125.9(9) . . ? C14B C13B C17B 113.2(9) . . ? C13B C14B C15B 120.2(9) . . ? C10B C15B C14B 118.8(8) . . ? C10B C15B C18B 127.1(8) . . ? C14B C15B C18B 114.0(8) . . ? C20B C19B C24B 116.2(8) . . ? C20B C19B B2B 123.3(9) . . ? C24B C19B B2B 120.3(8) . . ? C19B C20B C25B 124.4(10) . . ? C19B C20B C21B 117.6(9) . . ? C25B C20B C21B 118.0(10) . . ? C22B C21B C20B 123.7(10) . . ? C23B C22B C21B 116.0(11) . . ? C23B C22B C26B 128.1(12) . . ? C21B C22B C26B 115.8(11) . . ? C22B C23B C24B 125.3(11) . . ? C23B C24B C19B 121.1(9) . . ? C23B C24B C27B 117.2(8) . . ? C19B C24B C27B 121.7(8) . . ? C29B C28B C33B 114.4(8) . . ? C29B C28B B2B 124.6(8) . . ? C33B C28B B2B 120.9(8) . . ? C30B C29B C28B 125.7(10) . . ? C30B C29B C34B 114.4(10) . . ? C28B C29B C34B 119.9(9) . . ? C29B C30B C31B 120.9(10) . . ? C32B C31B C30B 115.6(11) . . ? C32B C31B C35B 122.9(12) . . ? C30B C31B C35B 121.3(11) . . ? C31B C32B C33B 124.2(10) . . ? C32B C33B C28B 118.9(8) . . ? C32B C33B C36B 120.8(8) . . ? C28B C33B C36B 120.2(8) . . ? C42B C37B N1B 118.2(9) . . ? C42B C37B C38B 123.7(9) . . ? N1B C37B C38B 118.0(9) . . ? C37B C38B C39B 113.7(9) . . ? C37B C38B C43B 121.4(9) . . ? C39B C38B C43B 124.7(10) . . ? C40B C39B C38B 122.5(10) . . ? C41B C40B C39B 120.1(11) . . ? C40B C41B C42B 121.4(11) . . ? C37B C42B C41B 118.5(9) . . ? C37B C42B C46B 121.0(8) . . ? C41B C42B C46B 120.5(9) . . ? C44B C43B C38B 110.2(10) . . ? C44B C43B C45B 109.1(11) . . ? C38B C43B C45B 108.5(10) . . ? C48B C46B C42B 110.6(8) . . ? C48B C46B C47B 109.1(9) . . ? C42B C46B C47B 112.8(9) . . ? N2B C49B C54B 124.9(10) . . ? N2B C49B C50B 114.8(8) . . ? C54B C49B C50B 120.3(9) . . ? C51B C50B C49B 118.5(9) . . ? C51B C50B C55B 122.0(9) . . ? C49B C50B C55B 119.3(9) . . ? C52B C51B C50B 120.4(11) . . ? C51B C52B C53B 118.1(10) . . ? C54B C53B C52B 124.7(11) . . ? C53B C54B C49B 117.7(10) . . ? C53B C54B C58B 121.0(10) . . ? C49B C54B C58B 121.1(9) . . ? C50B C55B C57B 113.3(9) . . ? C50B C55B C56B 114.6(8) . . ? C57B C55B C56B 105.2(8) . . ? C54B C58B C59B 111.5(8) . . ? C54B C58B C60B 109.3(8) . . ? C59B C58B C60B 112.4(8) . . ? #===END data_(3)may2202 _database_code_CSD 190541 _audit_creation_date 2002-05-17T16:47:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Mo(NtBu)2(OCHMes2)2]' _chemical_formula_moiety 'C46 H64 Mo1 N2 O2' _chemical_formula_structural 'C46 H64 MO N2 O2' _chemical_formula_sum 'C46 H64 Mo N2 O2' _chemical_formula_weight 772.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 19.4544(3) _cell_length_b 11.2123(2) _cell_length_c 19.7023(3) _cell_angle_alpha 90 _cell_angle_beta 94.658(2) _cell_angle_gamma 90 _cell_volume 4283.44(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33739 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _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_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.982 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 35268 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.73 _diffrn_reflns_theta_full 25.73 _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _reflns_number_total 7830 _reflns_number_gt 6626 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0416P)^2^+4.5139P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7830 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.086 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.325 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mo1 Mo 0.779298(10) 0.462681(17) 0.503877(10) 0.02121(8) Uani 1 1 d . . . O1 O 0.68551(8) 0.42517(15) 0.51237(8) 0.0286(4) Uani 1 1 d . . . O2 O 0.79196(8) 0.61086(14) 0.45884(8) 0.0278(4) Uani 1 1 d . . . N1 N 0.82731(10) 0.47093(17) 0.58230(10) 0.0272(4) Uani 1 1 d . . . N2 N 0.81081(10) 0.34955(18) 0.45454(10) 0.0282(5) Uani 1 1 d . . . C1 C 0.87918(13) 0.4436(2) 0.63783(13) 0.0297(6) Uani 1 1 d . . . C2 C 0.94997(14) 0.4369(3) 0.61003(16) 0.0433(7) Uani 1 1 d . . . H2A H 0.9607 0.5136 0.5895 0.065 Uiso 1 1 calc R . . H2B H 0.9498 0.374 0.5755 0.065 Uiso 1 1 calc R . . H2C H 0.9849 0.4187 0.6473 0.065 Uiso 1 1 calc R . . C3 C 0.86079(15) 0.3253(3) 0.66993(15) 0.0447(7) Uani 1 1 d . . . H3A H 0.8149 0.3312 0.6868 0.067 Uiso 1 1 calc R . . H3B H 0.8948 0.3069 0.7079 0.067 Uiso 1 1 calc R . . H3C H 0.8608 0.2618 0.6357 0.067 Uiso 1 1 calc R . . C4 C 0.87725(16) 0.5439(3) 0.68991(17) 0.0521(8) Uani 1 1 d . . . H4A H 0.8315 0.5468 0.7074 0.078 Uiso 1 1 calc R . . H4B H 0.8867 0.6202 0.6682 0.078 Uiso 1 1 calc R . . H4C H 0.9123 0.5294 0.7276 0.078 Uiso 1 1 calc R . . C5 C 0.85105(13) 0.2497(2) 0.43156(14) 0.0335(6) Uani 1 1 d . . . C6 C 0.81321(17) 0.2010(3) 0.36650(14) 0.0448(7) Uani 1 1 d . . . H6A H 0.7676 0.1721 0.3764 0.067 Uiso 1 1 calc R . . H6B H 0.8398 0.1352 0.349 0.067 Uiso 1 1 calc R . . H6C H 0.808 0.2645 0.3323 0.067 Uiso 1 1 calc R . . C7 C 0.92226(16) 0.2968(3) 0.41717(19) 0.0608(10) Uani 1 1 d . . . H7A H 0.9461 0.3265 0.4595 0.091 Uiso 1 1 calc R . . H7B H 0.917 0.3618 0.3839 0.091 Uiso 1 1 calc R . . H7C H 0.9493 0.2322 0.3989 0.091 Uiso 1 1 calc R . . C8 C 0.85644(17) 0.1541(3) 0.48673(15) 0.0474(8) Uani 1 1 d . . . H8A H 0.8101 0.1263 0.4951 0.071 Uiso 1 1 calc R . . H8B H 0.879 0.1876 0.5288 0.071 Uiso 1 1 calc R . . H8C H 0.8837 0.087 0.4718 0.071 Uiso 1 1 calc R . . C9 C 0.62988(11) 0.4337(2) 0.55525(12) 0.0241(5) Uani 1 1 d . . . H9 H 0.6107 0.5158 0.548 0.029 Uiso 1 1 calc R . . C10 C 0.57077(12) 0.3487(2) 0.53217(12) 0.0249(5) Uani 1 1 d . . . C11 C 0.57466(13) 0.2546(2) 0.48543(13) 0.0293(6) Uani 1 1 d . . . C12 C 0.51623(13) 0.1838(2) 0.47004(14) 0.0346(6) Uani 1 1 d . . . H12 H 0.5193 0.1196 0.4389 0.042 Uiso 1 1 calc R . . C13 C 0.45429(13) 0.2029(2) 0.49803(14) 0.0374(7) Uani 1 1 d . . . C14 C 0.45043(13) 0.2992(2) 0.54129(14) 0.0341(6) Uani 1 1 d . . . H14 H 0.4078 0.316 0.5597 0.041 Uiso 1 1 calc R . . C15 C 0.50692(12) 0.3726(2) 0.55887(12) 0.0286(5) Uani 1 1 d . . . C16 C 0.63787(14) 0.2223(3) 0.44898(15) 0.0407(7) Uani 1 1 d . . . H16A H 0.6287 0.1496 0.4222 0.061 Uiso 1 1 calc R . . H16B H 0.6771 0.2088 0.4826 0.061 Uiso 1 1 calc R . . H16C H 0.6487 0.2878 0.4187 0.061 Uiso 1 1 calc R . . C17 C 0.39357(15) 0.1205(3) 0.48179(18) 0.0528(8) Uani 1 1 d . . . H17A H 0.4063 0.0587 0.45 0.079 Uiso 0.5 1 calc PR . . H17B H 0.3545 0.1665 0.461 0.079 Uiso 0.5 1 calc PR . . H17C H 0.3806 0.0831 0.5238 0.079 Uiso 0.5 1 calc PR . . H17D H 0.3546 0.1468 0.5066 0.079 Uiso 0.5 1 calc PR . . H17E H 0.4064 0.039 0.4955 0.079 Uiso 0.5 1 calc PR . . H17F H 0.3803 0.1224 0.4327 0.079 Uiso 0.5 1 calc PR . . C18 C 0.49699(13) 0.4762(2) 0.60584(14) 0.0353(6) Uani 1 1 d . . . H18A H 0.4478 0.4854 0.6121 0.053 Uiso 1 1 calc R . . H18B H 0.5143 0.5493 0.5859 0.053 Uiso 1 1 calc R . . H18C H 0.5224 0.4613 0.65 0.053 Uiso 1 1 calc R . . C19 C 0.65511(11) 0.4275(2) 0.63052(12) 0.0233(5) Uani 1 1 d . . . C20 C 0.66415(12) 0.3200(2) 0.66711(13) 0.0276(5) Uani 1 1 d . . . C21 C 0.68274(13) 0.3243(2) 0.73740(13) 0.0310(6) Uani 1 1 d . . . H21 H 0.688 0.2514 0.7618 0.037 Uiso 1 1 calc R . . C22 C 0.69363(12) 0.4298(2) 0.77247(13) 0.0306(6) Uani 1 1 d . . . C23 C 0.68730(13) 0.5348(2) 0.73538(13) 0.0304(6) Uani 1 1 d . . . H23 H 0.6957 0.6085 0.7583 0.036 Uiso 1 1 calc R . . C24 C 0.66901(12) 0.5354(2) 0.66585(13) 0.0280(5) Uani 1 1 d . . . C25 C 0.65641(16) 0.1987(2) 0.63440(15) 0.0416(7) Uani 1 1 d . . . H25A H 0.6074 0.1822 0.6226 0.062 Uiso 1 1 calc R . . H25B H 0.6756 0.1379 0.6663 0.062 Uiso 1 1 calc R . . H25C H 0.6812 0.1971 0.593 0.062 Uiso 1 1 calc R . . C26 C 0.71328(16) 0.4312(3) 0.84847(14) 0.0432(7) Uani 1 1 d . . . H26A H 0.7193 0.5138 0.8641 0.065 Uiso 0.5 1 calc PR . . H26B H 0.7566 0.3874 0.8583 0.065 Uiso 0.5 1 calc PR . . H26C H 0.6767 0.3932 0.8722 0.065 Uiso 0.5 1 calc PR . . H26D H 0.7158 0.3491 0.8656 0.065 Uiso 0.5 1 calc PR . . H26E H 0.6785 0.4755 0.8714 0.065 Uiso 0.5 1 calc PR . . H26F H 0.7583 0.4697 0.8575 0.065 Uiso 0.5 1 calc PR . . C27 C 0.66427(16) 0.6548(2) 0.62995(15) 0.0418(7) Uani 1 1 d . . . H27A H 0.6921 0.6529 0.5907 0.063 Uiso 1 1 calc R . . H27B H 0.6815 0.7175 0.6615 0.063 Uiso 1 1 calc R . . H27C H 0.6161 0.6713 0.6144 0.063 Uiso 1 1 calc R . . C28 C 0.80186(12) 0.6384(2) 0.38955(12) 0.0242(5) Uani 1 1 d . . . H28 H 0.8116 0.5613 0.3666 0.029 Uiso 1 1 calc R . . C29 C 0.86487(11) 0.7199(2) 0.38257(12) 0.0238(5) Uani 1 1 d . . . C30 C 0.88571(12) 0.7341(2) 0.31622(12) 0.0270(5) Uani 1 1 d . . . C31 C 0.93858(12) 0.8134(2) 0.30436(14) 0.0316(6) Uani 1 1 d . . . H31 H 0.9514 0.8233 0.2592 0.038 Uiso 1 1 calc R . . C32 C 0.97297(12) 0.8784(2) 0.35654(14) 0.0325(6) Uani 1 1 d . . . C33 C 0.95431(12) 0.8578(2) 0.42166(14) 0.0317(6) Uani 1 1 d . . . H33 H 0.9784 0.8994 0.4583 0.038 Uiso 1 1 calc R . . C34 C 0.90196(12) 0.7792(2) 0.43652(13) 0.0280(5) Uani 1 1 d . . . C35 C 0.85325(15) 0.6645(3) 0.25659(13) 0.0391(6) Uani 1 1 d . . . H35A H 0.8759 0.685 0.2155 0.059 Uiso 1 1 calc R . . H35B H 0.8041 0.6842 0.2497 0.059 Uiso 1 1 calc R . . H35C H 0.8586 0.5789 0.2657 0.059 Uiso 1 1 calc R . . C36 C 1.02854(15) 0.9668(3) 0.34258(18) 0.0472(8) Uani 1 1 d . . . H36A H 1.0342 0.9688 0.2936 0.071 Uiso 0.5 1 calc PR . . H36B H 1.0721 0.9429 0.3672 0.071 Uiso 0.5 1 calc PR . . H36C H 1.0154 1.0462 0.3578 0.071 Uiso 0.5 1 calc PR . . H36D H 1.047 1.0031 0.3855 0.071 Uiso 0.5 1 calc PR . . H36E H 1.009 1.0291 0.3119 0.071 Uiso 0.5 1 calc PR . . H36F H 1.0657 0.9257 0.3213 0.071 Uiso 0.5 1 calc PR . . C37 C 0.88959(15) 0.7663(3) 0.51151(13) 0.0411(7) Uani 1 1 d . . . H37A H 0.8414 0.7853 0.518 0.062 Uiso 1 1 calc R . . H37B H 0.9199 0.8211 0.5386 0.062 Uiso 1 1 calc R . . H37C H 0.8995 0.6841 0.5262 0.062 Uiso 1 1 calc R . . C38 C 0.73333(12) 0.6857(2) 0.35556(13) 0.0272(5) Uani 1 1 d . . . C39 C 0.68919(13) 0.6051(2) 0.31811(13) 0.0310(6) Uani 1 1 d . . . C40 C 0.62497(13) 0.6438(3) 0.29058(13) 0.0386(7) Uani 1 1 d . . . H40 H 0.5955 0.5885 0.266 0.046 Uiso 1 1 calc R . . C41 C 0.60249(14) 0.7593(3) 0.29761(15) 0.0433(7) Uani 1 1 d . . . C42 C 0.64640(14) 0.8378(3) 0.33383(16) 0.0434(7) Uani 1 1 d . . . H42 H 0.6319 0.918 0.339 0.052 Uiso 1 1 calc R . . C43 C 0.71118(13) 0.8037(2) 0.36309(14) 0.0352(6) Uani 1 1 d . . . C44 C 0.70802(15) 0.4766(3) 0.30666(15) 0.0424(7) Uani 1 1 d . . . H44A H 0.6689 0.4355 0.2825 0.064 Uiso 1 1 calc R . . H44B H 0.7195 0.4377 0.3507 0.064 Uiso 1 1 calc R . . H44C H 0.7479 0.4731 0.2794 0.064 Uiso 1 1 calc R . . C45 C 0.53079(16) 0.7987(4) 0.27022(18) 0.0651(10) Uani 1 1 d . . . H45A H 0.507 0.7321 0.2463 0.098 Uiso 0.5 1 calc PR . . H45B H 0.5346 0.8655 0.2386 0.098 Uiso 0.5 1 calc PR . . H45C H 0.5046 0.8241 0.3081 0.098 Uiso 0.5 1 calc PR . . H45D H 0.5238 0.8824 0.2824 0.098 Uiso 0.5 1 calc PR . . H45E H 0.4962 0.749 0.2901 0.098 Uiso 0.5 1 calc PR . . H45F H 0.5262 0.7903 0.2205 0.098 Uiso 0.5 1 calc PR . . C46 C 0.75269(15) 0.8971(2) 0.4037(2) 0.0545(9) Uani 1 1 d . . . H46A H 0.7671 0.8656 0.449 0.082 Uiso 1 1 calc R . . H46B H 0.7244 0.9685 0.4081 0.082 Uiso 1 1 calc R . . H46C H 0.7936 0.9177 0.3802 0.082 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 Mo1 0.02002(12) 0.01905(11) 0.02488(13) 0.00143(8) 0.00373(8) -0.00230(8) O1 0.0215(8) 0.0359(10) 0.0290(9) 0.0018(7) 0.0055(7) -0.0049(7) O2 0.0308(9) 0.0227(9) 0.0305(9) 0.0040(7) 0.0072(7) -0.0017(7) N1 0.0258(11) 0.0257(11) 0.0298(11) 0.0003(9) 0.0015(8) -0.0034(8) N2 0.0298(11) 0.0258(11) 0.0299(11) -0.0003(9) 0.0085(9) -0.0016(9) C1 0.0256(13) 0.0307(14) 0.0323(14) -0.0013(11) -0.0004(10) 0.0007(10) C2 0.0286(14) 0.0467(17) 0.0545(19) 0.0058(14) 0.0031(13) 0.0032(12) C3 0.0429(17) 0.0467(18) 0.0439(17) 0.0159(14) -0.0006(13) 0.0004(14) C4 0.0389(17) 0.063(2) 0.0524(19) -0.0263(16) -0.0072(14) -0.0002(15) C5 0.0359(14) 0.0290(14) 0.0364(15) -0.0060(11) 0.0077(11) 0.0041(11) C6 0.062(2) 0.0380(16) 0.0349(16) -0.0093(13) 0.0069(14) 0.0024(14) C7 0.0400(18) 0.069(2) 0.076(2) -0.0193(19) 0.0248(17) -0.0024(16) C8 0.0587(19) 0.0363(16) 0.0465(18) -0.0043(13) -0.0007(15) 0.0154(14) C9 0.0210(12) 0.0225(12) 0.0296(13) 0.0036(10) 0.0066(10) -0.0008(9) C10 0.0205(12) 0.0275(13) 0.0264(13) 0.0074(10) -0.0004(9) -0.0032(9) C11 0.0278(13) 0.0289(13) 0.0308(14) 0.0063(11) -0.0008(10) -0.0024(10) C12 0.0371(15) 0.0279(13) 0.0372(15) 0.0055(11) -0.0073(12) -0.0070(11) C13 0.0282(14) 0.0363(15) 0.0456(16) 0.0176(13) -0.0088(12) -0.0106(12) C14 0.0229(13) 0.0399(15) 0.0394(15) 0.0165(13) 0.0011(11) -0.0032(11) C15 0.0251(12) 0.0319(13) 0.0287(13) 0.0122(11) 0.0015(10) 0.0000(10) C16 0.0407(16) 0.0381(16) 0.0441(17) -0.0112(13) 0.0093(13) -0.0055(12) C17 0.0360(16) 0.0464(18) 0.073(2) 0.0180(16) -0.0127(15) -0.0174(14) C18 0.0276(13) 0.0430(16) 0.0364(15) 0.0053(12) 0.0086(11) 0.0031(12) C19 0.0187(11) 0.0250(12) 0.0269(13) 0.0035(10) 0.0054(9) 0.0006(9) C20 0.0252(12) 0.0250(13) 0.0331(14) 0.0035(10) 0.0052(10) -0.0001(10) C21 0.0298(13) 0.0300(14) 0.0337(14) 0.0097(11) 0.0065(11) 0.0003(11) C22 0.0241(13) 0.0383(15) 0.0304(14) 0.0009(11) 0.0078(10) 0.0019(11) C23 0.0276(13) 0.0285(13) 0.0352(14) -0.0044(11) 0.0038(11) 0.0017(10) C24 0.0257(12) 0.0246(13) 0.0338(14) 0.0032(11) 0.0030(10) -0.0001(10) C25 0.0594(19) 0.0239(14) 0.0401(16) 0.0047(12) -0.0045(13) 0.0024(13) C26 0.0454(17) 0.0536(18) 0.0307(15) 0.0016(13) 0.0032(12) 0.0037(14) C27 0.0528(18) 0.0231(13) 0.0478(17) 0.0038(12) -0.0064(14) -0.0039(12) C28 0.0251(12) 0.0197(12) 0.0279(13) 0.0009(10) 0.0033(10) -0.0032(9) C29 0.0217(12) 0.0197(12) 0.0304(13) 0.0023(10) 0.0035(10) 0.0020(9) C30 0.0217(12) 0.0280(13) 0.0315(14) 0.0031(10) 0.0029(10) 0.0033(10) C31 0.0256(13) 0.0336(14) 0.0368(15) 0.0104(12) 0.0103(11) 0.0031(11) C32 0.0197(12) 0.0258(13) 0.0527(17) 0.0079(12) 0.0060(11) 0.0010(10) C33 0.0250(13) 0.0242(13) 0.0452(16) -0.0035(11) -0.0015(11) -0.0002(10) C34 0.0266(13) 0.0237(12) 0.0340(14) -0.0008(10) 0.0048(10) 0.0021(10) C35 0.0433(16) 0.0461(16) 0.0280(14) 0.0033(12) 0.0041(12) -0.0068(13) C36 0.0330(15) 0.0401(17) 0.069(2) 0.0125(15) 0.0048(14) -0.0089(13) C37 0.0481(17) 0.0430(17) 0.0324(15) -0.0105(13) 0.0045(12) -0.0123(13) C38 0.0211(12) 0.0269(13) 0.0343(14) 0.0090(11) 0.0062(10) -0.0029(10) C39 0.0296(13) 0.0362(14) 0.0275(13) 0.0082(11) 0.0033(10) -0.0067(11) C40 0.0298(14) 0.0563(19) 0.0295(14) 0.0102(13) 0.0013(11) -0.0073(13) C41 0.0260(14) 0.066(2) 0.0387(16) 0.0232(15) 0.0070(12) 0.0047(14) C42 0.0328(15) 0.0414(16) 0.0580(19) 0.0215(14) 0.0154(13) 0.0102(13) C43 0.0267(13) 0.0304(14) 0.0500(17) 0.0103(12) 0.0113(12) -0.0020(11) C44 0.0414(16) 0.0398(16) 0.0439(17) -0.0005(13) -0.0103(13) -0.0106(13) C45 0.0358(17) 0.102(3) 0.057(2) 0.023(2) 0.0010(15) 0.0178(18) C46 0.0337(16) 0.0212(14) 0.110(3) -0.0065(16) 0.0143(17) 0.0022(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.740(2) . ? Mo1 N1 1.742(2) . ? Mo1 O1 1.8930(16) . ? Mo1 O2 1.9089(16) . ? O1 C9 1.429(3) . ? O2 C28 1.428(3) . ? N1 C1 1.459(3) . ? N2 C5 1.459(3) . ? C1 C2 1.525(4) . ? C1 C3 1.524(4) . ? C1 C4 1.525(4) . ? C5 C8 1.524(4) . ? C5 C7 1.530(4) . ? C5 C6 1.526(4) . ? C9 C19 1.525(3) . ? C9 C10 1.534(3) . ? C10 C11 1.406(4) . ? C10 C15 1.414(3) . ? C11 C12 1.399(3) . ? C11 C16 1.517(4) . ? C12 C13 1.382(4) . ? C13 C14 1.382(4) . ? C13 C17 1.513(4) . ? C14 C15 1.394(4) . ? C15 C18 1.507(4) . ? C19 C24 1.410(3) . ? C19 C20 1.409(3) . ? C20 C21 1.404(4) . ? C20 C25 1.507(4) . ? C21 C22 1.378(4) . ? C22 C23 1.385(4) . ? C22 C26 1.515(4) . ? C23 C24 1.387(4) . ? C24 C27 1.514(3) . ? C28 C38 1.537(3) . ? C28 C29 1.544(3) . ? C29 C34 1.403(3) . ? C29 C30 1.409(3) . ? C30 C31 1.394(3) . ? C30 C35 1.506(4) . ? C31 C32 1.387(4) . ? C32 C33 1.381(4) . ? C32 C36 1.509(4) . ? C33 C34 1.396(3) . ? C34 C37 1.523(4) . ? C38 C43 1.404(4) . ? C38 C39 1.412(4) . ? C39 C40 1.390(4) . ? C39 C44 1.508(4) . ? C40 C41 1.377(4) . ? C41 C42 1.384(4) . ? C41 C45 1.520(4) . ? C42 C43 1.396(4) . ? C43 C46 1.511(4) . ? 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 N2 Mo1 N1 110.27(10) . . ? N2 Mo1 O1 105.86(8) . . ? N1 Mo1 O1 112.62(8) . . ? N2 Mo1 O2 108.07(8) . . ? N1 Mo1 O2 106.62(8) . . ? O1 Mo1 O2 113.34(7) . . ? C9 O1 Mo1 144.99(15) . . ? C28 O2 Mo1 131.69(14) . . ? C1 N1 Mo1 160.41(18) . . ? C5 N2 Mo1 162.78(18) . . ? N1 C1 C2 109.3(2) . . ? N1 C1 C3 108.8(2) . . ? C2 C1 C3 110.8(2) . . ? N1 C1 C4 107.2(2) . . ? C2 C1 C4 110.5(2) . . ? C3 C1 C4 110.1(2) . . ? N2 C5 C8 109.0(2) . . ? N2 C5 C7 108.0(2) . . ? C8 C5 C7 111.3(3) . . ? N2 C5 C6 107.5(2) . . ? C8 C5 C6 110.4(2) . . ? C7 C5 C6 110.5(2) . . ? O1 C9 C19 111.87(18) . . ? O1 C9 C10 111.65(19) . . ? C19 C9 C10 115.77(19) . . ? C11 C10 C15 118.8(2) . . ? C11 C10 C9 125.5(2) . . ? C15 C10 C9 115.6(2) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 C16 116.0(2) . . ? C10 C11 C16 125.3(2) . . ? C13 C12 C11 123.0(3) . . ? C12 C13 C14 117.4(2) . . ? C12 C13 C17 120.8(3) . . ? C14 C13 C17 121.8(3) . . ? C13 C14 C15 122.2(2) . . ? C14 C15 C10 119.6(2) . . ? C14 C15 C18 118.0(2) . . ? C10 C15 C18 122.4(2) . . ? C24 C19 C20 118.1(2) . . ? C24 C19 C9 118.4(2) . . ? C20 C19 C9 123.6(2) . . ? C21 C20 C19 119.1(2) . . ? C21 C20 C25 117.5(2) . . ? C19 C20 C25 123.3(2) . . ? C22 C21 C20 122.8(2) . . ? C21 C22 C23 117.5(2) . . ? C21 C22 C26 121.4(2) . . ? C23 C22 C26 121.2(2) . . ? C22 C23 C24 122.0(2) . . ? C23 C24 C19 120.4(2) . . ? C23 C24 C27 117.8(2) . . ? C19 C24 C27 121.7(2) . . ? O2 C28 C38 108.15(18) . . ? O2 C28 C29 112.50(18) . . ? C38 C28 C29 115.09(19) . . ? C34 C29 C30 118.7(2) . . ? C34 C29 C28 125.2(2) . . ? C30 C29 C28 116.1(2) . . ? C31 C30 C29 120.0(2) . . ? C31 C30 C35 117.9(2) . . ? C29 C30 C35 122.1(2) . . ? C32 C31 C30 121.9(2) . . ? C33 C32 C31 117.0(2) . . ? C33 C32 C36 121.7(3) . . ? C31 C32 C36 121.3(3) . . ? C32 C33 C34 123.5(2) . . ? C33 C34 C29 118.7(2) . . ? C33 C34 C37 116.0(2) . . ? C29 C34 C37 125.3(2) . . ? C43 C38 C39 118.6(2) . . ? C43 C38 C28 122.8(2) . . ? C39 C38 C28 118.4(2) . . ? C40 C39 C38 119.5(3) . . ? C40 C39 C44 117.5(2) . . ? C38 C39 C44 123.0(2) . . ? C41 C40 C39 122.5(3) . . ? C40 C41 C42 117.5(2) . . ? C40 C41 C45 121.9(3) . . ? C42 C41 C45 120.5(3) . . ? C43 C42 C41 122.5(3) . . ? C42 C43 C38 119.3(3) . . ? C42 C43 C46 117.0(3) . . ? C38 C43 C46 123.6(2) . . ? #===END data_(4)jan702 _database_code_CSD 190542 _audit_creation_date 2002-01-11T16:10:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Ti(NtBu)(py)(OBMes2)2].1/2(hexane)' _chemical_formula_moiety '(C50 H63 B2 N3 O1 Ti1).1/2(C6 H14)'' _chemical_formula_sum 'C53 H70 B2 N3 O2 Ti' _chemical_formula_weight 850.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7856(6) _cell_length_b 11.9638(4) _cell_length_c 17.5685(9) _cell_angle_alpha 93.029(3) _cell_angle_beta 98.130(2) _cell_angle_gamma 91.726(3) _cell_volume 2447.07(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8348 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.922 _exptl_absorpt_correction_T_max 0.964 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_unetI/netI 0.0727 _diffrn_reflns_number 14981 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8545 _reflns_number_gt 6318 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The hexane solvate molecule is poorly defined and distance constraints (SADI) were applied to it. 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^)+(0.0671P)^2^+2.4260P] 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 'riding mode' _refine_ls_extinction_method none _refine_ls_number_reflns 8545 _refine_ls_number_parameters 565 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.765 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.77583(4) 0.28631(4) 0.18370(3) 0.02379(16) Uani 1 1 d . . . O1 O 0.89814(17) 0.38902(16) 0.23009(12) 0.0286(5) Uani 1 1 d . . . O2 O 0.68288(17) 0.17387(15) 0.22391(12) 0.0277(5) Uani 1 1 d . . . N1 N 0.6527(2) 0.41561(19) 0.21381(14) 0.0252(5) Uani 1 1 d . . . N2 N 0.9096(2) 0.1582(2) 0.18048(17) 0.0365(7) Uani 1 1 d . . . N3 N 0.7381(2) 0.3012(2) 0.08750(14) 0.0292(6) Uani 1 1 d . . . C1 C 0.6817(3) 0.5245(2) 0.2130(2) 0.0353(8) Uani 1 1 d . . . H1 H 0.7596 0.5453 0.2111 0.042 Uiso 1 1 calc R . . C2 C 0.6040(3) 0.6075(3) 0.2148(2) 0.0422(9) Uani 1 1 d . . . H2 H 0.6281 0.6838 0.2137 0.051 Uiso 1 1 calc R . . C3 C 0.4915(3) 0.5790(3) 0.2181(2) 0.0420(9) Uani 1 1 d . . . H3 H 0.4361 0.635 0.2186 0.05 Uiso 1 1 calc R . . C4 C 0.4599(3) 0.4679(3) 0.2206(2) 0.0406(8) Uani 1 1 d . . . H4 H 0.3827 0.4457 0.2238 0.049 Uiso 1 1 calc R . . C5 C 0.5431(3) 0.3891(2) 0.21845(19) 0.0323(7) Uani 1 1 d . . . H5 H 0.5212 0.3124 0.2204 0.039 Uiso 1 1 calc R . . C6 C 0.9530(3) 0.1277(3) 0.1166(3) 0.0566(11) Uani 1 1 d . . . H6 H 0.9245 0.1609 0.0701 0.068 Uiso 1 1 calc R . . C7 C 1.0374(4) 0.0502(4) 0.1150(4) 0.0776(16) Uani 1 1 d . . . H7 H 1.0668 0.0316 0.0685 0.093 Uiso 1 1 calc R . . C8 C 1.0772(4) 0.0013(4) 0.1804(4) 0.0851(19) Uani 1 1 d . . . H8 H 1.1337 -0.0537 0.1802 0.102 Uiso 1 1 calc R . . C9 C 1.0361(4) 0.0312(4) 0.2466(4) 0.0739(15) Uani 1 1 d . . . H9 H 1.0643 -0.0012 0.2934 0.089 Uiso 1 1 calc R . . C10 C 0.9517(3) 0.1105(3) 0.2445(3) 0.0525(10) Uani 1 1 d . . . H10 H 0.923 0.1314 0.2908 0.063 Uiso 1 1 calc R . . C11 C 1.0190(2) 0.5310(2) 0.32205(17) 0.0261(6) Uani 1 1 d . . . C12 C 1.0987(3) 0.6219(3) 0.32109(18) 0.0318(7) Uani 1 1 d . . . C13 C 1.1023(3) 0.7128(3) 0.37513(19) 0.0345(8) Uani 1 1 d . . . H13 H 1.1556 0.7733 0.3731 0.041 Uiso 1 1 calc R . . C14 C 1.0310(3) 0.7175(3) 0.43132(18) 0.0342(7) Uani 1 1 d . . . C15 C 0.9561(3) 0.6270(3) 0.43349(18) 0.0349(7) Uani 1 1 d . . . H15 H 0.908 0.6276 0.4726 0.042 Uiso 1 1 calc R . . C16 C 0.9480(3) 0.5348(2) 0.38057(17) 0.0289(7) Uani 1 1 d . . . C17 C 1.1819(3) 0.6253(3) 0.2635(2) 0.0463(9) Uani 1 1 d . . . H17A H 1.2096 0.7027 0.2603 0.069 Uiso 1 1 calc R . . H17B H 1.1433 0.5966 0.2129 0.069 Uiso 1 1 calc R . . H17C H 1.247 0.5789 0.28 0.069 Uiso 1 1 calc R . . C18 C 1.0358(3) 0.8175(3) 0.4885(2) 0.0440(9) Uani 1 1 d . . . H18A H 1.1002 0.8109 0.5298 0.066 Uiso 1 1 calc R . . H18B H 0.964 0.8197 0.5106 0.066 Uiso 1 1 calc R . . H18C H 1.0464 0.8864 0.4622 0.066 Uiso 1 1 calc R . . C19 C 0.8650(3) 0.4403(3) 0.39126(19) 0.0381(8) Uani 1 1 d . . . H19A H 0.8492 0.444 0.4446 0.057 Uiso 1 1 calc R . . H19B H 0.8985 0.3685 0.3798 0.057 Uiso 1 1 calc R . . H19C H 0.7933 0.4471 0.3563 0.057 Uiso 1 1 calc R . . C20 C 1.1086(2) 0.3694(2) 0.22534(17) 0.0246(6) Uani 1 1 d . . . C21 C 1.1178(2) 0.3665(2) 0.14608(17) 0.0265(7) Uani 1 1 d . . . C22 C 1.2003(3) 0.3023(2) 0.11726(18) 0.0292(7) Uani 1 1 d . . . H22 H 1.2068 0.3033 0.064 0.035 Uiso 1 1 calc R . . C23 C 1.2731(3) 0.2370(2) 0.16343(18) 0.0290(7) Uani 1 1 d . . . C24 C 1.2665(3) 0.2422(2) 0.24169(18) 0.0284(7) Uani 1 1 d . . . H24 H 1.3174 0.2 0.2748 0.034 Uiso 1 1 calc R . . C25 C 1.1867(3) 0.3079(2) 0.27305(17) 0.0278(7) Uani 1 1 d . . . C26 C 1.0389(3) 0.4310(3) 0.09097(18) 0.0354(8) Uani 1 1 d . . . H26A H 1.052 0.4115 0.0381 0.053 Uiso 1 1 calc R . . H26B H 1.0543 0.5115 0.1026 0.053 Uiso 1 1 calc R . . H26C H 0.9591 0.4119 0.0963 0.053 Uiso 1 1 calc R . . C27 C 1.3538(3) 0.1606(3) 0.1286(2) 0.0401(8) Uani 1 1 d . . . H27A H 1.3115 0.0923 0.1059 0.06 Uiso 1 1 calc R . . H27B H 1.4152 0.141 0.1688 0.06 Uiso 1 1 calc R . . H27C H 1.3871 0.1988 0.0886 0.06 Uiso 1 1 calc R . . C28 C 1.1817(3) 0.3070(3) 0.35839(19) 0.0438(9) Uani 1 1 d . . . H28A H 1.1094 0.2703 0.3668 0.066 Uiso 1 1 calc R . . H28B H 1.1861 0.3841 0.3806 0.066 Uiso 1 1 calc R . . H28C H 1.2462 0.266 0.3831 0.066 Uiso 1 1 calc R . . C29 C 0.5529(3) 0.0613(2) 0.29879(17) 0.0257(6) Uani 1 1 d . . . C30 C 0.5570(3) 0.1314(2) 0.36659(17) 0.0279(7) Uani 1 1 d . . . C31 C 0.4757(3) 0.1177(3) 0.41626(19) 0.0359(8) Uani 1 1 d . . . H31 H 0.4811 0.1648 0.462 0.043 Uiso 1 1 calc R . . C32 C 0.3872(3) 0.0370(3) 0.4005(2) 0.0364(8) Uani 1 1 d . . . C33 C 0.3825(3) -0.0307(3) 0.3336(2) 0.0368(8) Uani 1 1 d . . . H33 H 0.3217 -0.0856 0.3215 0.044 Uiso 1 1 calc R . . C34 C 0.4632(3) -0.0215(2) 0.28372(19) 0.0313(7) Uani 1 1 d . . . C35 C 0.6509(3) 0.2206(3) 0.38957(19) 0.0382(8) Uani 1 1 d . . . H35A H 0.6319 0.2879 0.3616 0.057 Uiso 1 1 calc R . . H35B H 0.7237 0.1928 0.3769 0.057 Uiso 1 1 calc R . . H35C H 0.658 0.239 0.4451 0.057 Uiso 1 1 calc R . . C36 C 0.2992(3) 0.0238(3) 0.4550(2) 0.0548(10) Uani 1 1 d . . . H36A H 0.2988 -0.053 0.4717 0.082 Uiso 1 1 calc R . . H36B H 0.2231 0.0397 0.4284 0.082 Uiso 1 1 calc R . . H36C H 0.319 0.0763 0.5 0.082 Uiso 1 1 calc R . . C37 C 0.4497(3) -0.1018(3) 0.2131(2) 0.0427(9) Uani 1 1 d . . . H37A H 0.5098 -0.1568 0.2191 0.064 Uiso 1 1 calc R . . H37B H 0.4562 -0.06 0.1673 0.064 Uiso 1 1 calc R . . H37C H 0.3743 -0.1407 0.2072 0.064 Uiso 1 1 calc R . . C38 C 0.7107(3) -0.0347(2) 0.21384(17) 0.0264(7) Uani 1 1 d . . . C39 C 0.7105(3) -0.0594(2) 0.13450(17) 0.0287(7) Uani 1 1 d . . . C40 C 0.7736(3) -0.1470(2) 0.10997(18) 0.0330(7) Uani 1 1 d . . . H40 H 0.7724 -0.1626 0.0563 0.04 Uiso 1 1 calc R . . C41 C 0.8385(3) -0.2126(2) 0.16135(19) 0.0325(7) Uani 1 1 d . . . C42 C 0.8366(3) -0.1904(2) 0.23884(19) 0.0317(7) Uani 1 1 d . . . H42 H 0.8796 -0.2351 0.2748 0.038 Uiso 1 1 calc R . . C43 C 0.7732(3) -0.1039(2) 0.26607(18) 0.0296(7) Uani 1 1 d . . . C44 C 0.6424(3) 0.0078(3) 0.07459(18) 0.0390(8) Uani 1 1 d . . . H44A H 0.687 0.0758 0.0671 0.058 Uiso 1 1 calc R . . H44B H 0.5701 0.0284 0.0921 0.058 Uiso 1 1 calc R . . H44C H 0.6261 -0.0373 0.0258 0.058 Uiso 1 1 calc R . . C45 C 0.9107(3) -0.3030(3) 0.1325(2) 0.0479(9) Uani 1 1 d . . . H45A H 0.9786 -0.2687 0.1155 0.072 Uiso 1 1 calc R . . H45B H 0.8657 -0.3467 0.0891 0.072 Uiso 1 1 calc R . . H45C H 0.9346 -0.3525 0.174 0.072 Uiso 1 1 calc R . . C46 C 0.7773(4) -0.0836(3) 0.3516(2) 0.0502(10) Uani 1 1 d . . . H46A H 0.8184 -0.1436 0.3782 0.075 Uiso 1 1 calc R . . H46B H 0.699 -0.0824 0.3643 0.075 Uiso 1 1 calc R . . H46C H 0.8172 -0.0115 0.3682 0.075 Uiso 1 1 calc R . . C47 C 0.6907(3) 0.3285(3) 0.00992(18) 0.0374(8) Uani 1 1 d . . . C48 C 0.6993(4) 0.4559(3) 0.0042(2) 0.0535(10) Uani 1 1 d . . . H48A H 0.6547 0.4923 0.0408 0.08 Uiso 1 1 calc R . . H48B H 0.6689 0.4749 -0.0482 0.08 Uiso 1 1 calc R . . H48C H 0.7798 0.482 0.0162 0.08 Uiso 1 1 calc R . . C49 C 0.7586(4) 0.2711(4) -0.0475(2) 0.0570(11) Uani 1 1 d . . . H49A H 0.8393 0.2967 -0.0361 0.086 Uiso 1 1 calc R . . H49B H 0.7275 0.29 -0.0998 0.086 Uiso 1 1 calc R . . H49C H 0.7527 0.1898 -0.0437 0.086 Uiso 1 1 calc R . . C50 C 0.5652(3) 0.2892(3) -0.0068(2) 0.0510(10) Uani 1 1 d . . . H50A H 0.5592 0.2077 -0.0038 0.076 Uiso 1 1 calc R . . H50B H 0.5329 0.3094 -0.0585 0.076 Uiso 1 1 calc R . . H50C H 0.5227 0.3253 0.0313 0.076 Uiso 1 1 calc R . . C51 C 0.5283(10) 0.5497(5) 0.4941(4) 0.159(4) Uani 1 1 d D . . H51A H 0.5287 0.6006 0.5404 0.191 Uiso 1 1 calc R . . H51B H 0.6091 0.5333 0.4899 0.191 Uiso 1 1 calc R . . C52 C 0.485(2) 0.6056(11) 0.4309(7) 0.48(2) Uani 1 1 d D . . H52A H 0.436 0.6681 0.4429 0.578 Uiso 1 1 calc R . . H52B H 0.4459 0.5559 0.3877 0.578 Uiso 1 1 calc R . . C53 C 0.6112(11) 0.645(2) 0.4204(9) 0.50(3) Uani 1 1 d D . . H53A H 0.6303 0.6108 0.3721 0.751 Uiso 1 1 calc R . . H53B H 0.6655 0.6212 0.4636 0.751 Uiso 1 1 calc R . . H53C H 0.6159 0.7266 0.419 0.751 Uiso 1 1 calc R . . B1 B 1.0037(3) 0.4288(3) 0.2574(2) 0.0253(7) Uani 1 1 d . . . B2 B 0.6491(3) 0.0736(3) 0.24359(19) 0.0241(7) Uani 1 1 d . . . 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 Ti 0.0231(3) 0.0230(3) 0.0256(3) 0.0002(2) 0.0044(2) 0.0027(2) O1 0.0237(11) 0.0277(11) 0.0340(12) -0.0026(9) 0.0042(9) 0.0033(8) O2 0.0296(12) 0.0229(10) 0.0314(12) 0.0016(8) 0.0065(9) 0.0029(8) N1 0.0247(14) 0.0226(12) 0.0287(14) 0.0016(10) 0.0045(11) 0.0027(10) N2 0.0280(15) 0.0275(14) 0.0537(19) -0.0023(13) 0.0069(13) -0.0016(11) N3 0.0284(14) 0.0334(14) 0.0258(14) -0.0005(10) 0.0048(11) -0.0001(11) C1 0.0282(18) 0.0277(17) 0.051(2) 0.0039(14) 0.0072(15) -0.0009(13) C2 0.035(2) 0.0245(17) 0.069(3) 0.0076(16) 0.0133(18) 0.0014(14) C3 0.035(2) 0.0252(17) 0.067(3) 0.0017(15) 0.0096(18) 0.0086(14) C4 0.0245(18) 0.0335(18) 0.065(2) 0.0019(16) 0.0111(17) 0.0015(14) C5 0.0248(17) 0.0253(16) 0.047(2) 0.0005(14) 0.0075(15) -0.0016(12) C6 0.048(2) 0.048(2) 0.075(3) -0.017(2) 0.020(2) 0.0055(18) C7 0.054(3) 0.055(3) 0.126(5) -0.026(3) 0.030(3) 0.012(2) C8 0.039(3) 0.037(2) 0.181(7) -0.004(3) 0.023(3) 0.0075(19) C9 0.038(2) 0.054(3) 0.129(5) 0.030(3) -0.004(3) 0.011(2) C10 0.038(2) 0.049(2) 0.071(3) 0.014(2) 0.003(2) 0.0065(17) C11 0.0212(16) 0.0280(15) 0.0288(16) 0.0024(12) 0.0022(13) 0.0028(12) C12 0.0267(17) 0.0341(17) 0.0352(19) 0.0003(13) 0.0075(14) 0.0009(13) C13 0.0312(18) 0.0299(17) 0.042(2) -0.0037(14) 0.0060(15) -0.0053(13) C14 0.0319(18) 0.0375(18) 0.0308(18) -0.0052(14) -0.0014(14) 0.0021(14) C15 0.0310(18) 0.0467(19) 0.0271(17) -0.0024(14) 0.0069(14) 0.0000(14) C16 0.0249(17) 0.0340(17) 0.0270(17) 0.0024(13) 0.0012(13) 0.0004(13) C17 0.042(2) 0.046(2) 0.054(2) -0.0087(17) 0.0240(18) -0.0107(16) C18 0.046(2) 0.044(2) 0.040(2) -0.0119(16) 0.0035(17) -0.0009(16) C19 0.039(2) 0.0441(19) 0.0312(18) -0.0005(14) 0.0095(15) -0.0087(15) C20 0.0212(15) 0.0253(15) 0.0269(16) 0.0020(12) 0.0024(12) -0.0015(11) C21 0.0229(16) 0.0271(15) 0.0297(17) 0.0038(12) 0.0033(13) 0.0035(12) C22 0.0303(17) 0.0322(16) 0.0257(16) -0.0003(12) 0.0068(13) 0.0024(13) C23 0.0257(17) 0.0254(15) 0.0357(18) 0.0010(13) 0.0033(14) 0.0017(12) C24 0.0230(16) 0.0277(16) 0.0343(18) 0.0057(13) 0.0012(13) 0.0041(12) C25 0.0235(16) 0.0312(16) 0.0285(17) 0.0042(13) 0.0029(13) -0.0018(12) C26 0.0357(19) 0.0424(19) 0.0308(18) 0.0068(14) 0.0100(15) 0.0128(15) C27 0.0346(19) 0.0422(19) 0.043(2) -0.0042(15) 0.0041(16) 0.0142(15) C28 0.042(2) 0.058(2) 0.0322(19) 0.0103(16) 0.0052(16) 0.0141(17) C29 0.0274(16) 0.0204(14) 0.0297(17) 0.0044(12) 0.0036(13) 0.0060(12) C30 0.0295(17) 0.0282(16) 0.0267(17) 0.0043(12) 0.0048(13) 0.0041(12) C31 0.040(2) 0.0397(19) 0.0286(18) 0.0027(14) 0.0066(15) 0.0067(15) C32 0.0332(19) 0.0400(19) 0.040(2) 0.0144(15) 0.0126(15) 0.0047(14) C33 0.0324(19) 0.0295(17) 0.050(2) 0.0092(15) 0.0082(16) -0.0001(13) C34 0.0326(18) 0.0236(15) 0.0387(19) 0.0036(13) 0.0074(15) 0.0049(13) C35 0.044(2) 0.0413(19) 0.0284(18) -0.0057(14) 0.0080(15) -0.0038(15) C36 0.052(2) 0.064(3) 0.055(3) 0.015(2) 0.026(2) -0.0017(19) C37 0.037(2) 0.0295(17) 0.060(2) -0.0101(16) 0.0080(17) -0.0042(14) C38 0.0278(17) 0.0243(15) 0.0273(17) 0.0007(12) 0.0050(13) 0.0013(12) C39 0.0331(18) 0.0236(15) 0.0297(17) 0.0012(12) 0.0055(14) 0.0014(12) C40 0.042(2) 0.0308(17) 0.0269(17) -0.0038(13) 0.0082(15) 0.0046(14) C41 0.0335(18) 0.0212(15) 0.044(2) -0.0029(13) 0.0097(15) 0.0035(13) C42 0.0311(18) 0.0256(16) 0.0382(19) 0.0053(13) 0.0025(14) 0.0063(13) C43 0.0308(17) 0.0274(16) 0.0315(17) 0.0023(13) 0.0062(14) 0.0044(13) C44 0.052(2) 0.0381(18) 0.0257(18) -0.0030(14) 0.0007(16) 0.0109(16) C45 0.055(2) 0.039(2) 0.054(2) -0.0009(16) 0.0176(19) 0.0181(17) C46 0.070(3) 0.052(2) 0.030(2) 0.0083(16) 0.0030(18) 0.0303(19) C47 0.041(2) 0.0449(19) 0.0253(17) 0.0074(14) 0.0016(15) -0.0064(15) C48 0.071(3) 0.049(2) 0.038(2) 0.0160(17) -0.0041(19) -0.0073(19) C49 0.066(3) 0.078(3) 0.028(2) -0.0016(18) 0.0111(19) -0.001(2) C50 0.042(2) 0.065(2) 0.042(2) 0.0178(18) -0.0087(17) -0.0087(18) C51 0.248(12) 0.126(7) 0.095(6) -0.046(6) 0.027(7) -0.038(7) C52 1.06(7) 0.285(19) 0.086(9) -0.080(10) 0.06(2) 0.17(3) C53 0.132(10) 1.10(7) 0.230(18) -0.35(3) 0.027(10) 0.083(19) B1 0.0237(18) 0.0247(17) 0.0278(19) 0.0069(14) 0.0033(15) 0.0020(13) B2 0.0240(18) 0.0246(17) 0.0229(17) 0.0004(13) -0.0003(14) 0.0033(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N3 1.706(3) . ? Ti O1 1.925(2) . ? Ti O2 1.934(2) . ? Ti N2 2.236(3) . ? Ti N1 2.246(2) . ? O1 B1 1.332(4) . ? O2 B2 1.331(4) . ? N1 C5 1.335(4) . ? N1 C1 1.338(4) . ? N2 C10 1.327(5) . ? N2 C6 1.335(5) . ? N3 C47 1.455(4) . ? C1 C2 1.373(4) . ? C2 C3 1.370(5) . ? C3 C4 1.374(4) . ? C4 C5 1.383(4) . ? C6 C7 1.383(6) . ? C7 C8 1.349(8) . ? C8 C9 1.356(8) . ? C9 C10 1.394(6) . ? C11 C16 1.415(4) . ? C11 C12 1.417(4) . ? C11 B1 1.613(4) . ? C12 C13 1.401(4) . ? C12 C17 1.507(4) . ? C13 C14 1.383(5) . ? C14 C15 1.382(5) . ? C14 C18 1.515(4) . ? C15 C16 1.397(4) . ? C16 C19 1.509(4) . ? C20 C25 1.407(4) . ? C20 C21 1.411(4) . ? C20 B1 1.600(4) . ? C21 C22 1.390(4) . ? C21 C26 1.505(4) . ? C22 C23 1.384(4) . ? C23 C24 1.386(4) . ? C23 C27 1.507(4) . ? C24 C25 1.397(4) . ? C25 C28 1.509(4) . ? C29 C34 1.413(4) . ? C29 C30 1.414(4) . ? C29 B2 1.601(4) . ? C30 C31 1.396(4) . ? C30 C35 1.511(4) . ? C31 C32 1.388(5) . ? C32 C33 1.384(5) . ? C32 C36 1.518(5) . ? C33 C34 1.388(4) . ? C34 C37 1.516(4) . ? C38 C39 1.409(4) . ? C38 C43 1.413(4) . ? C38 B2 1.603(4) . ? C39 C40 1.388(4) . ? C39 C44 1.513(4) . ? C40 C41 1.390(4) . ? C41 C42 1.377(4) . ? C41 C45 1.507(4) . ? C42 C43 1.398(4) . ? C43 C46 1.504(4) . ? C47 C50 1.522(5) . ? C47 C49 1.522(5) . ? C47 C48 1.535(5) . ? C51 C52 1.371(13) . ? C51 C51 1.385(12) 2_666 ? C52 C53 1.585(19) . ? 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 N3 Ti O1 113.19(11) . . ? N3 Ti O2 113.26(11) . . ? O1 Ti O2 133.50(9) . . ? N3 Ti N2 100.14(11) . . ? O1 Ti N2 86.66(9) . . ? O2 Ti N2 87.42(9) . . ? N3 Ti N1 91.86(10) . . ? O1 Ti N1 87.55(8) . . ? O2 Ti N1 88.92(8) . . ? N2 Ti N1 167.95(10) . . ? B1 O1 Ti 159.91(19) . . ? B2 O2 Ti 158.92(19) . . ? C5 N1 C1 117.1(2) . . ? C5 N1 Ti 122.00(19) . . ? C1 N1 Ti 119.7(2) . . ? C10 N2 C6 116.8(3) . . ? C10 N2 Ti 120.0(2) . . ? C6 N2 Ti 123.1(3) . . ? C47 N3 Ti 169.4(2) . . ? N1 C1 C2 123.1(3) . . ? C3 C2 C1 119.2(3) . . ? C2 C3 C4 118.9(3) . . ? C3 C4 C5 118.5(3) . . ? N1 C5 C4 123.3(3) . . ? N2 C6 C7 123.1(5) . . ? C8 C7 C6 118.9(5) . . ? C7 C8 C9 119.6(4) . . ? C8 C9 C10 118.6(5) . . ? N2 C10 C9 122.9(4) . . ? C16 C11 C12 117.5(3) . . ? C16 C11 B1 120.0(3) . . ? C12 C11 B1 122.4(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 C17 117.5(3) . . ? C11 C12 C17 122.4(3) . . ? C14 C13 C12 122.4(3) . . ? C15 C14 C13 117.3(3) . . ? C15 C14 C18 121.4(3) . . ? C13 C14 C18 121.3(3) . . ? C14 C15 C16 122.7(3) . . ? C15 C16 C11 120.0(3) . . ? C15 C16 C19 117.1(3) . . ? C11 C16 C19 122.9(3) . . ? C25 C20 C21 117.7(3) . . ? C25 C20 B1 121.4(3) . . ? C21 C20 B1 120.5(3) . . ? C22 C21 C20 120.1(3) . . ? C22 C21 C26 118.6(3) . . ? C20 C21 C26 121.3(3) . . ? C23 C22 C21 122.3(3) . . ? C22 C23 C24 117.7(3) . . ? C22 C23 C27 120.5(3) . . ? C24 C23 C27 121.7(3) . . ? C23 C24 C25 121.6(3) . . ? C24 C25 C20 120.5(3) . . ? C24 C25 C28 118.8(3) . . ? C20 C25 C28 120.6(3) . . ? C34 C29 C30 117.2(3) . . ? C34 C29 B2 122.0(3) . . ? C30 C29 B2 120.7(3) . . ? C31 C30 C29 120.7(3) . . ? C31 C30 C35 117.5(3) . . ? C29 C30 C35 121.8(3) . . ? C32 C31 C30 121.6(3) . . ? C33 C32 C31 117.7(3) . . ? C33 C32 C36 121.5(3) . . ? C31 C32 C36 120.8(3) . . ? C32 C33 C34 122.4(3) . . ? C33 C34 C29 120.3(3) . . ? C33 C34 C37 117.4(3) . . ? C29 C34 C37 122.2(3) . . ? C39 C38 C43 117.9(3) . . ? C39 C38 B2 120.8(3) . . ? C43 C38 B2 121.2(3) . . ? C40 C39 C38 120.0(3) . . ? C40 C39 C44 118.7(3) . . ? C38 C39 C44 121.3(3) . . ? C39 C40 C41 122.2(3) . . ? C42 C41 C40 117.9(3) . . ? C42 C41 C45 121.5(3) . . ? C40 C41 C45 120.5(3) . . ? C41 C42 C43 121.8(3) . . ? C42 C43 C38 120.2(3) . . ? C42 C43 C46 118.6(3) . . ? C38 C43 C46 121.2(3) . . ? N3 C47 C50 109.5(3) . . ? N3 C47 C49 109.2(3) . . ? C50 C47 C49 110.2(3) . . ? N3 C47 C48 109.0(3) . . ? C50 C47 C48 109.1(3) . . ? C49 C47 C48 109.9(3) . . ? C52 C51 C51 116.8(15) . 2_666 ? C51 C52 C53 89.8(16) . . ? O1 B1 C20 117.6(3) . . ? O1 B1 C11 118.7(3) . . ? C20 B1 C11 123.7(3) . . ? O2 B2 C29 120.9(2) . . ? O2 B2 C38 118.6(3) . . ? C29 B2 C38 120.5(2) . . ? #===END data_(5)jun1102 _database_code_CSD 190543 _audit_creation_date 2002-06-14T14:45:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Ti(py)2(NtBu)(OCHMes2)2]' _chemical_formula_moiety 'C52 H65 N3 O2 Ti1' _chemical_formula_sum 'C52 H65 N3 O2 Ti' _chemical_formula_weight 811.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5789(1) _cell_length_b 19.5500(3) _cell_length_c 22.5063(3) _cell_angle_alpha 82.370(1) _cell_angle_beta 89.957(1) _cell_angle_gamma 83.821(1) _cell_volume 4586.3(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 55867 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9111 _exptl_absorpt_correction_T_max 0.9965 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_unetI/netI 0.0634 _diffrn_reflns_number 60894 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 24.76 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 15458 _reflns_number_gt 11334 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0429P)^2^+5.6436P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 15458 _refine_ls_number_parameters 1061 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.47 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.82263(5) 0.26398(3) 0.46716(2) 0.02135(14) Uani 1 1 d . . . O1 O 0.7309(2) 0.26381(11) 0.53909(9) 0.0267(5) Uani 1 1 d . . . O2 O 0.7453(2) 0.28299(11) 0.39109(9) 0.0291(5) Uani 1 1 d . . . N1 N 0.8204(2) 0.38065(13) 0.46425(12) 0.0275(6) Uani 1 1 d . . . N2 N 0.7891(3) 0.15232(14) 0.46799(11) 0.0285(6) Uani 1 1 d . . . N3 N 0.9856(2) 0.25393(13) 0.47162(11) 0.0276(6) Uani 1 1 d . . . C1 C 0.8104(3) 0.41202(18) 0.51335(16) 0.0366(8) Uani 1 1 d . . . H1 H 0.7979 0.3849 0.5507 0.044 Uiso 1 1 calc R . . C2 C 0.8174(4) 0.48212(19) 0.51233(18) 0.0501(10) Uani 1 1 d . . . H2 H 0.8091 0.5027 0.5483 0.06 Uiso 1 1 calc R . . C3 C 0.8365(4) 0.52154(19) 0.45906(19) 0.0506(11) Uani 1 1 d . . . H3 H 0.8412 0.57 0.4573 0.061 Uiso 1 1 calc R . . C4 C 0.8487(4) 0.49016(19) 0.40801(18) 0.0437(9) Uani 1 1 d . . . H4 H 0.8632 0.5163 0.3704 0.052 Uiso 1 1 calc R . . C5 C 0.8395(3) 0.41983(18) 0.41245(16) 0.0376(9) Uani 1 1 d . . . H5 H 0.847 0.3983 0.377 0.045 Uiso 1 1 calc R . . C6 C 0.6715(3) 0.13464(18) 0.47756(15) 0.0329(8) Uani 1 1 d . . . H6 H 0.6066 0.1695 0.4858 0.039 Uiso 1 1 calc R . . C7 C 0.6398(4) 0.06869(19) 0.47614(16) 0.0442(9) Uani 1 1 d . . . H7 H 0.5547 0.0585 0.4827 0.053 Uiso 1 1 calc R . . C8 C 0.7330(4) 0.0177(2) 0.46502(17) 0.0501(11) Uani 1 1 d . . . H8 H 0.7137 -0.0285 0.4642 0.06 Uiso 1 1 calc R . . C9 C 0.8545(4) 0.03465(19) 0.45512(17) 0.0466(10) Uani 1 1 d . . . H9 H 0.9207 0.0004 0.4471 0.056 Uiso 1 1 calc R . . C10 C 0.8793(3) 0.10246(17) 0.45701(15) 0.0351(8) Uani 1 1 d . . . H10 H 0.9636 0.114 0.4503 0.042 Uiso 1 1 calc R . . C11 C 1.1208(3) 0.26091(18) 0.47727(15) 0.0332(8) Uani 1 1 d . . . C12 C 1.1982(4) 0.1930(3) 0.4693(2) 0.0709(15) Uani 1 1 d . . . H12A H 1.1805 0.1807 0.4296 0.106 Uiso 1 1 calc R . . H12B H 1.1753 0.1564 0.5002 0.106 Uiso 1 1 calc R . . H12C H 1.2889 0.1981 0.473 0.106 Uiso 1 1 calc R . . C13 C 1.1487(4) 0.2801(2) 0.53942(17) 0.0446(9) Uani 1 1 d . . . H13A H 1.099 0.3241 0.5446 0.067 Uiso 1 1 calc R . . H13B H 1.2395 0.2848 0.5432 0.067 Uiso 1 1 calc R . . H13C H 1.1254 0.2435 0.5703 0.067 Uiso 1 1 calc R . . C14 C 1.1549(4) 0.3197(3) 0.43029(19) 0.0677(14) Uani 1 1 d . . . H14A H 1.1035 0.3629 0.4363 0.102 Uiso 1 1 calc R . . H14B H 1.1378 0.3084 0.3901 0.102 Uiso 1 1 calc R . . H14C H 1.2452 0.3254 0.4343 0.102 Uiso 1 1 calc R . . C15 C 0.7259(3) 0.24515(16) 0.60136(13) 0.0255(7) Uani 1 1 d . . . H15 H 0.8118 0.2512 0.6171 0.031 Uiso 1 1 calc R . . C16 C 0.6308(3) 0.29245(16) 0.63356(14) 0.0254(7) Uani 1 1 d . . . C17 C 0.5378(3) 0.34307(17) 0.60506(14) 0.0294(8) Uani 1 1 d . . . C18 C 0.4620(3) 0.38424(18) 0.63992(15) 0.0356(8) Uani 1 1 d . . . H18 H 0.3997 0.4184 0.6203 0.043 Uiso 1 1 calc R . . C19 C 0.4727(3) 0.37783(18) 0.70164(15) 0.0364(8) Uani 1 1 d . . . C20 C 0.5643(3) 0.32840(18) 0.72895(15) 0.0359(8) Uani 1 1 d . . . H20 H 0.5735 0.323 0.7714 0.043 Uiso 1 1 calc R . . C21 C 0.6440(3) 0.28601(17) 0.69637(14) 0.0300(8) Uani 1 1 d . . . C22 C 0.5074(3) 0.3547(2) 0.53837(15) 0.0417(9) Uani 1 1 d . . . H22A H 0.574 0.3787 0.5169 0.062 Uiso 1 1 calc R . . H22B H 0.4253 0.383 0.5311 0.062 Uiso 1 1 calc R . . H22C H 0.5032 0.3098 0.524 0.062 Uiso 1 1 calc R . . C23 C 0.3849(4) 0.4219(2) 0.73791(18) 0.0508(11) Uani 1 1 d . . . H23A H 0.3266 0.454 0.7108 0.076 Uiso 0.5 1 calc PR . . H23B H 0.4353 0.4486 0.7611 0.076 Uiso 0.5 1 calc PR . . H23C H 0.336 0.3919 0.7653 0.076 Uiso 0.5 1 calc PR . . H23D H 0.4054 0.409 0.7807 0.076 Uiso 0.5 1 calc PR . . H23E H 0.2966 0.4144 0.7304 0.076 Uiso 0.5 1 calc PR . . H23F H 0.3959 0.471 0.7262 0.076 Uiso 0.5 1 calc PR . . C24 C 0.7428(3) 0.23478(19) 0.73087(15) 0.0404(9) Uani 1 1 d . . . H24A H 0.7404 0.2413 0.7733 0.061 Uiso 1 1 calc R . . H24B H 0.8272 0.2423 0.715 0.061 Uiso 1 1 calc R . . H24C H 0.7251 0.1874 0.7268 0.061 Uiso 1 1 calc R . . C25 C 0.7132(3) 0.16689(16) 0.61506(13) 0.0259(7) Uani 1 1 d . . . C26 C 0.8264(3) 0.12124(17) 0.61932(13) 0.0279(7) Uani 1 1 d . . . C27 C 0.8212(3) 0.05022(18) 0.62699(15) 0.0363(9) Uani 1 1 d . . . H27 H 0.8986 0.0203 0.6299 0.044 Uiso 1 1 calc R . . C28 C 0.7083(4) 0.02138(18) 0.63052(15) 0.0385(9) Uani 1 1 d . . . C29 C 0.5975(3) 0.06609(18) 0.62716(15) 0.0377(9) Uani 1 1 d . . . H29 H 0.5185 0.0471 0.6304 0.045 Uiso 1 1 calc R . . C30 C 0.5970(3) 0.13780(17) 0.61923(15) 0.0319(8) Uani 1 1 d . . . C31 C 0.9558(3) 0.14791(19) 0.61534(16) 0.0389(9) Uani 1 1 d . . . H31A H 1.022 0.1088 0.6152 0.058 Uiso 1 1 calc R . . H31B H 0.9691 0.1721 0.6499 0.058 Uiso 1 1 calc R . . H31C H 0.9601 0.1801 0.5783 0.058 Uiso 1 1 calc R . . C32 C 0.7062(4) -0.05651(19) 0.6378(2) 0.0566(12) Uani 1 1 d . . . H32A H 0.6179 -0.0674 0.6393 0.085 Uiso 0.5 1 calc PR . . H32B H 0.7507 -0.0774 0.6751 0.085 Uiso 0.5 1 calc PR . . H32C H 0.7486 -0.0752 0.6037 0.085 Uiso 0.5 1 calc PR . . H32D H 0.7936 -0.0792 0.6394 0.085 Uiso 0.5 1 calc PR . . H32E H 0.6607 -0.0693 0.6037 0.085 Uiso 0.5 1 calc PR . . H32F H 0.6629 -0.0715 0.675 0.085 Uiso 0.5 1 calc PR . . C33 C 0.4688(3) 0.1807(2) 0.6131(2) 0.0519(11) Uani 1 1 d . . . H33A H 0.4019 0.15 0.6113 0.078 Uiso 1 1 calc R . . H33B H 0.4662 0.2138 0.5764 0.078 Uiso 1 1 calc R . . H33C H 0.4552 0.2059 0.6478 0.078 Uiso 1 1 calc R . . C34 C 0.7450(3) 0.27957(17) 0.32927(14) 0.0290(7) Uani 1 1 d . . . H34 H 0.8272 0.2956 0.3143 0.035 Uiso 1 1 calc R . . C35 C 0.6394(3) 0.32864(16) 0.29337(13) 0.0255(7) Uani 1 1 d . . . C36 C 0.5439(3) 0.37173(17) 0.31843(14) 0.0288(7) Uani 1 1 d . . . C37 C 0.4580(3) 0.41648(18) 0.28034(15) 0.0346(8) Uani 1 1 d . . . H37 H 0.395 0.4458 0.2977 0.042 Uiso 1 1 calc R . . C38 C 0.4603(3) 0.42012(18) 0.21882(15) 0.0340(8) Uani 1 1 d . . . C39 C 0.5547(3) 0.37767(18) 0.19508(14) 0.0336(8) Uani 1 1 d . . . H39 H 0.5583 0.3791 0.1528 0.04 Uiso 1 1 calc R . . C40 C 0.6443(3) 0.33310(16) 0.23023(14) 0.0264(7) Uani 1 1 d . . . C41 C 0.5229(3) 0.3737(2) 0.38474(15) 0.0407(9) Uani 1 1 d . . . H41A H 0.5179 0.3265 0.4049 0.061 Uiso 1 1 calc R . . H41B H 0.4434 0.4026 0.3905 0.061 Uiso 1 1 calc R . . H41C H 0.5939 0.3933 0.4018 0.061 Uiso 1 1 calc R . . C42 C 0.3645(4) 0.4688(2) 0.17955(17) 0.0490(10) Uani 1 1 d . . . H42A H 0.306 0.4942 0.2048 0.074 Uiso 0.5 1 calc PR . . H42B H 0.3164 0.4419 0.1555 0.074 Uiso 0.5 1 calc PR . . H42C H 0.4089 0.5018 0.1529 0.074 Uiso 0.5 1 calc PR . . H42D H 0.3815 0.4644 0.1373 0.074 Uiso 0.5 1 calc PR . . H42E H 0.3711 0.5167 0.1866 0.074 Uiso 0.5 1 calc PR . . H42F H 0.2786 0.4568 0.1893 0.074 Uiso 0.5 1 calc PR . . C43 C 0.7463(3) 0.29272(19) 0.19842(14) 0.0354(8) Uani 1 1 d . . . H43A H 0.7408 0.3091 0.1553 0.053 Uiso 1 1 calc R . . H43B H 0.7345 0.2433 0.2053 0.053 Uiso 1 1 calc R . . H43C H 0.83 0.2995 0.2139 0.053 Uiso 1 1 calc R . . C44 C 0.7503(3) 0.20284(17) 0.31860(13) 0.0279(7) Uani 1 1 d . . . C45 C 0.6424(3) 0.16715(18) 0.32308(14) 0.0324(8) Uani 1 1 d . . . C46 C 0.6537(4) 0.09807(19) 0.31288(15) 0.0402(9) Uani 1 1 d . . . H46 H 0.5795 0.0745 0.315 0.048 Uiso 1 1 calc R . . C47 C 0.7679(4) 0.06220(19) 0.29975(15) 0.0423(9) Uani 1 1 d . . . C48 C 0.8748(4) 0.09781(19) 0.29771(15) 0.0395(9) Uani 1 1 d . . . H48 H 0.9548 0.0742 0.2895 0.047 Uiso 1 1 calc R . . C49 C 0.8688(3) 0.16685(18) 0.30732(14) 0.0318(8) Uani 1 1 d . . . C50 C 0.5145(3) 0.1995(2) 0.34135(18) 0.0473(10) Uani 1 1 d . . . H50A H 0.5238 0.2186 0.379 0.071 Uiso 1 1 calc R . . H50B H 0.4551 0.1641 0.3469 0.071 Uiso 1 1 calc R . . H50C H 0.4816 0.2368 0.31 0.071 Uiso 1 1 calc R . . C51 C 0.7763(5) -0.0140(2) 0.29184(19) 0.0622(12) Uani 1 1 d . . . H51A H 0.864 -0.0304 0.2826 0.093 Uiso 0.5 1 calc PR . . H51B H 0.7198 -0.0199 0.2589 0.093 Uiso 0.5 1 calc PR . . H51C H 0.7506 -0.0409 0.3289 0.093 Uiso 0.5 1 calc PR . . H51D H 0.6923 -0.0304 0.2976 0.093 Uiso 0.5 1 calc PR . . H51E H 0.8365 -0.0409 0.3214 0.093 Uiso 0.5 1 calc PR . . H51F H 0.8057 -0.02 0.2514 0.093 Uiso 0.5 1 calc PR . . C52 C 0.9912(3) 0.2001(2) 0.30665(17) 0.0429(9) Uani 1 1 d . . . H52A H 1.0629 0.1654 0.3014 0.064 Uiso 1 1 calc R . . H52B H 1.0016 0.2183 0.3447 0.064 Uiso 1 1 calc R . . H52C H 0.9885 0.2382 0.2735 0.064 Uiso 1 1 calc R . . Ti1B Ti 0.68432(5) 0.74017(3) 0.01466(2) 0.02228(15) Uani 1 1 d . . . O1B O 0.7803(2) 0.73482(11) 0.08617(9) 0.0279(5) Uani 1 1 d . . . O2B O 0.7574(2) 0.72678(11) -0.05944(9) 0.0302(5) Uani 1 1 d . . . N1B N 0.6864(2) 0.62365(13) 0.03279(11) 0.0252(6) Uani 1 1 d . . . N2B N 0.7172(3) 0.85226(14) -0.00585(12) 0.0299(6) Uani 1 1 d . . . N3B N 0.5218(2) 0.74987(13) 0.02013(11) 0.0276(6) Uani 1 1 d . . . C1B C 0.6761(3) 0.59270(17) 0.08869(14) 0.0311(8) Uani 1 1 d . . . H1B H 0.6771 0.6201 0.1205 0.037 Uiso 1 1 calc R . . C2B C 0.6641(3) 0.52318(17) 0.10270(15) 0.0348(8) Uani 1 1 d . . . H2B H 0.6558 0.5032 0.1432 0.042 Uiso 1 1 calc R . . C3B C 0.6643(4) 0.48312(19) 0.05675(16) 0.0410(9) Uani 1 1 d . . . H3B H 0.6574 0.4347 0.0651 0.049 Uiso 1 1 calc R . . C4B C 0.6746(4) 0.51397(19) -0.00110(16) 0.0435(9) Uani 1 1 d . . . H4B H 0.6744 0.4874 -0.0335 0.052 Uiso 1 1 calc R . . C5B C 0.6851(3) 0.58420(18) -0.01159(15) 0.0349(8) Uani 1 1 d . . . H5B H 0.6917 0.6055 -0.0518 0.042 Uiso 1 1 calc R . . C6B C 0.8358(3) 0.86832(18) -0.00453(15) 0.0364(8) Uani 1 1 d . . . H6B H 0.902 0.8322 0.0071 0.044 Uiso 1 1 calc R . . C7B C 0.8675(4) 0.93566(19) -0.01948(17) 0.0449(10) Uani 1 1 d . . . H7B H 0.9536 0.9452 -0.0179 0.054 Uiso 1 1 calc R . . C8B C 0.7734(4) 0.9876(2) -0.03631(17) 0.0519(11) Uani 1 1 d . . . H8B H 0.7926 1.0341 -0.0462 0.062 Uiso 1 1 calc R . . C9B C 0.6504(4) 0.9719(2) -0.03878(19) 0.0544(11) Uani 1 1 d . . . H9B H 0.5831 1.0072 -0.051 0.065 Uiso 1 1 calc R . . C10B C 0.6260(4) 0.90356(19) -0.02311(18) 0.0472(10) Uani 1 1 d . . . H10B H 0.5407 0.8929 -0.0248 0.057 Uiso 1 1 calc R . . C11B C 0.3872(3) 0.74187(18) 0.02621(15) 0.0322(8) Uani 1 1 d . . . C12B C 0.3098(4) 0.8116(2) 0.0138(2) 0.0743(15) Uani 1 1 d . . . H12D H 0.3264 0.8331 -0.0269 0.111 Uiso 1 1 calc R . . H12E H 0.3333 0.8415 0.0427 0.111 Uiso 1 1 calc R . . H12F H 0.2192 0.8057 0.0175 0.111 Uiso 1 1 calc R . . C13B C 0.3598(4) 0.7088(2) 0.08948(18) 0.0573(12) Uani 1 1 d . . . H13D H 0.4101 0.6634 0.098 0.086 Uiso 1 1 calc R . . H13E H 0.2692 0.7029 0.0927 0.086 Uiso 1 1 calc R . . H13F H 0.3826 0.7389 0.1184 0.086 Uiso 1 1 calc R . . C14B C 0.3512(4) 0.6931(3) -0.0173(2) 0.092(2) Uani 1 1 d . . . H14D H 0.4031 0.6482 -0.0084 0.137 Uiso 1 1 calc R . . H14E H 0.3665 0.7135 -0.0585 0.137 Uiso 1 1 calc R . . H14F H 0.2611 0.6863 -0.0128 0.137 Uiso 1 1 calc R . . C15B C 0.7833(3) 0.74883(17) 0.14569(14) 0.0277(7) Uani 1 1 d . . . H15B H 0.6983 0.7396 0.1626 0.033 Uiso 1 1 calc R . . C16B C 0.8822(3) 0.70129(16) 0.18665(13) 0.0267(7) Uani 1 1 d . . . C17B C 0.9783(3) 0.65377(17) 0.16702(14) 0.0305(8) Uani 1 1 d . . . C18B C 1.0607(3) 0.61368(18) 0.20930(16) 0.0374(8) Uani 1 1 d . . . H18B H 1.1254 0.5822 0.1956 0.045 Uiso 1 1 calc R . . C19B C 1.0536(3) 0.61715(19) 0.27013(16) 0.0385(9) Uani 1 1 d . . . C20B C 0.9569(4) 0.66309(19) 0.28858(15) 0.0393(9) Uani 1 1 d . . . H20B H 0.9484 0.6661 0.3302 0.047 Uiso 1 1 calc R . . C21B C 0.8724(3) 0.70476(18) 0.24863(15) 0.0328(8) Uani 1 1 d . . . C22B C 1.0000(3) 0.64200(19) 0.10282(15) 0.0385(9) Uani 1 1 d . . . H22D H 1.0789 0.6113 0.1003 0.058 Uiso 1 1 calc R . . H22E H 1.0068 0.6866 0.078 0.058 Uiso 1 1 calc R . . H22F H 0.9285 0.6205 0.0884 0.058 Uiso 1 1 calc R . . C23B C 1.1451(4) 0.5720(2) 0.31450(18) 0.0557(11) Uani 1 1 d . . . H23G H 1.2058 0.5432 0.2929 0.084 Uiso 0.5 1 calc PR . . H23H H 1.0975 0.5421 0.3426 0.084 Uiso 0.5 1 calc PR . . H23I H 1.1912 0.6016 0.3368 0.084 Uiso 0.5 1 calc PR . . H23J H 1.1239 0.5814 0.3553 0.084 Uiso 0.5 1 calc PR . . H23K H 1.2322 0.5825 0.3056 0.084 Uiso 0.5 1 calc PR . . H23L H 1.1385 0.523 0.3114 0.084 Uiso 0.5 1 calc PR . . C24B C 0.7706(4) 0.7527(2) 0.27462(15) 0.0458(10) Uani 1 1 d . . . H24D H 0.7732 0.7427 0.3185 0.069 Uiso 1 1 calc R . . H24E H 0.6868 0.7454 0.2597 0.069 Uiso 1 1 calc R . . H24F H 0.7862 0.8011 0.2625 0.069 Uiso 1 1 calc R . . C25B C 0.7904(3) 0.82722(17) 0.14501(14) 0.0281(7) Uani 1 1 d . . . C26B C 0.6751(3) 0.87065(18) 0.14484(15) 0.0354(8) Uani 1 1 d . . . C27B C 0.6773(4) 0.94220(19) 0.13879(17) 0.0431(9) Uani 1 1 d . . . H27B H 0.5987 0.9708 0.1383 0.052 Uiso 1 1 calc R . . C28B C 0.7879(4) 0.97347(19) 0.13347(16) 0.0426(9) Uani 1 1 d . . . C29B C 0.9005(4) 0.93027(18) 0.13469(15) 0.0390(9) Uani 1 1 d . . . H29B H 0.9784 0.9505 0.1318 0.047 Uiso 1 1 calc R . . C30B C 0.9044(3) 0.85792(17) 0.13998(14) 0.0312(8) Uani 1 1 d . . . C31B C 0.5473(3) 0.8422(2) 0.1490(2) 0.0529(11) Uani 1 1 d . . . H31D H 0.4792 0.8807 0.1443 0.079 Uiso 1 1 calc R . . H31E H 0.5405 0.8143 0.1881 0.079 Uiso 1 1 calc R . . H31F H 0.5396 0.8131 0.1172 0.079 Uiso 1 1 calc R . . C32B C 0.7866(5) 1.0512(2) 0.1261(2) 0.0639(13) Uani 1 1 d . . . H32G H 0.8741 1.0633 0.1227 0.096 Uiso 0.5 1 calc PR . . H32H H 0.7467 1.0692 0.161 0.096 Uiso 0.5 1 calc PR . . H32I H 0.7383 1.0716 0.0897 0.096 Uiso 0.5 1 calc PR . . H32J H 0.6986 1.0727 0.1262 0.096 Uiso 0.5 1 calc PR . . H32K H 0.826 1.0669 0.088 0.096 Uiso 0.5 1 calc PR . . H32L H 0.8344 1.0645 0.1592 0.096 Uiso 0.5 1 calc PR . . C33B C 1.0329(3) 0.8172(2) 0.13695(18) 0.0456(10) Uani 1 1 d . . . H33D H 1.0535 0.7889 0.1757 0.068 Uiso 1 1 calc R . . H33E H 1.0973 0.8493 0.1275 0.068 Uiso 1 1 calc R . . H33F H 1.0314 0.7869 0.1056 0.068 Uiso 1 1 calc R . . C34B C 0.7537(3) 0.73162(17) -0.12227(13) 0.0293(8) Uani 1 1 d . . . H34B H 0.6685 0.7185 -0.1326 0.035 Uiso 1 1 calc R . . C35B C 0.8513(3) 0.68007(17) -0.14849(14) 0.0267(7) Uani 1 1 d . . . C36B C 0.9486(3) 0.63546(17) -0.11557(14) 0.0283(7) Uani 1 1 d . . . C37B C 1.0244(3) 0.58779(17) -0.14508(15) 0.0320(8) Uani 1 1 d . . . H37B H 1.0876 0.557 -0.1224 0.038 Uiso 1 1 calc R . . C38B C 1.0125(3) 0.58299(17) -0.20550(15) 0.0323(8) Uani 1 1 d . . . C39B C 0.9169(3) 0.62678(17) -0.23681(15) 0.0318(8) Uani 1 1 d . . . H39B H 0.9059 0.6245 -0.2784 0.038 Uiso 1 1 calc R . . C40B C 0.8363(3) 0.67412(17) -0.20986(14) 0.0287(7) Uani 1 1 d . . . C41B C 0.9836(3) 0.6363(2) -0.05064(15) 0.0396(9) Uani 1 1 d . . . H41D H 0.9914 0.6841 -0.0437 0.059 Uiso 1 1 calc R . . H41E H 1.0649 0.6078 -0.0412 0.059 Uiso 1 1 calc R . . H41F H 0.9173 0.6175 -0.0249 0.059 Uiso 1 1 calc R . . C42B C 1.1037(4) 0.53477(19) -0.23604(17) 0.0432(9) Uani 1 1 d . . . H42G H 1.164 0.5082 -0.2064 0.065 Uiso 0.5 1 calc PR . . H42H H 1.1503 0.5619 -0.2667 0.065 Uiso 0.5 1 calc PR . . H42I H 1.0562 0.5028 -0.2549 0.065 Uiso 0.5 1 calc PR . . H42J H 1.083 0.5405 -0.279 0.065 Uiso 0.5 1 calc PR . . H42K H 1.0967 0.4867 -0.2186 0.065 Uiso 0.5 1 calc PR . . H42L H 1.1908 0.5458 -0.2304 0.065 Uiso 0.5 1 calc PR . . C43B C 0.7338(3) 0.71722(19) -0.24904(15) 0.0384(9) Uani 1 1 d . . . H43D H 0.7319 0.7001 -0.288 0.058 Uiso 1 1 calc R . . H43E H 0.7516 0.7658 -0.2549 0.058 Uiso 1 1 calc R . . H43F H 0.6512 0.7138 -0.2297 0.058 Uiso 1 1 calc R . . C44B C 0.7535(3) 0.80847(17) -0.14893(14) 0.0306(8) Uani 1 1 d . . . C45B C 0.8644(3) 0.84196(18) -0.15447(15) 0.0356(8) Uani 1 1 d . . . C46B C 0.8547(4) 0.91219(19) -0.17679(16) 0.0460(10) Uani 1 1 d . . . H46B H 0.9306 0.9342 -0.1813 0.055 Uiso 1 1 calc R . . C47B C 0.7409(5) 0.9514(2) -0.19269(16) 0.0495(11) Uani 1 1 d . . . C48B C 0.6321(4) 0.9168(2) -0.18711(16) 0.0486(11) Uani 1 1 d . . . H48B H 0.5524 0.9422 -0.1989 0.058 Uiso 1 1 calc R . . C49B C 0.6354(3) 0.84678(19) -0.16492(15) 0.0406(9) Uani 1 1 d . . . C50B C 0.9930(3) 0.8058(2) -0.13494(19) 0.0480(10) Uani 1 1 d . . . H50D H 0.9965 0.7955 -0.0911 0.072 Uiso 1 1 calc R . . H50E H 1.0586 0.8358 -0.1485 0.072 Uiso 1 1 calc R . . H50F H 1.0077 0.7623 -0.1525 0.072 Uiso 1 1 calc R . . C51B C 0.7347(5) 1.0287(2) -0.21288(19) 0.0709(15) Uani 1 1 d . . . H51G H 0.6463 1.0475 -0.2223 0.106 Uiso 0.5 1 calc PR . . H51H H 0.7865 1.037 -0.2487 0.106 Uiso 0.5 1 calc PR . . H51I H 0.7673 1.0515 -0.1808 0.106 Uiso 0.5 1 calc PR . . H51J H 0.8204 1.0432 -0.2122 0.106 Uiso 0.5 1 calc PR . . H51K H 0.6803 1.0537 -0.1858 0.106 Uiso 0.5 1 calc PR . . H51L H 0.6994 1.0392 -0.2537 0.106 Uiso 0.5 1 calc PR . . C52B C 0.5113(4) 0.8154(2) -0.15829(19) 0.0568(12) Uani 1 1 d . . . H52D H 0.4411 0.8511 -0.1714 0.085 Uiso 1 1 calc R . . H52E H 0.5 0.797 -0.1162 0.085 Uiso 1 1 calc R . . H52F H 0.5121 0.7777 -0.183 0.085 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 Ti 0.0215(3) 0.0222(3) 0.0200(3) -0.0028(2) 0.0015(2) -0.0006(2) O1 0.0305(12) 0.0254(12) 0.0234(12) -0.0036(9) 0.0070(9) 0.0003(10) O2 0.0356(13) 0.0289(12) 0.0217(12) -0.0009(9) -0.0042(9) -0.0011(10) N1 0.0253(15) 0.0270(15) 0.0299(15) -0.0029(12) 0.0004(11) -0.0017(12) N2 0.0328(16) 0.0294(15) 0.0230(14) -0.0045(12) -0.0002(11) -0.0010(13) N3 0.0248(15) 0.0278(15) 0.0303(15) -0.0057(12) 0.0025(11) -0.0003(12) C1 0.043(2) 0.034(2) 0.034(2) -0.0079(16) -0.0057(16) -0.0028(17) C2 0.071(3) 0.033(2) 0.049(3) -0.0157(19) -0.012(2) -0.008(2) C3 0.061(3) 0.022(2) 0.069(3) -0.010(2) -0.008(2) -0.0056(18) C4 0.050(2) 0.031(2) 0.049(2) 0.0031(18) 0.0069(18) -0.0083(18) C5 0.043(2) 0.032(2) 0.038(2) -0.0036(16) 0.0086(16) -0.0056(17) C6 0.034(2) 0.032(2) 0.0337(19) -0.0043(15) -0.0024(15) -0.0043(16) C7 0.055(3) 0.040(2) 0.039(2) -0.0035(18) -0.0007(18) -0.019(2) C8 0.083(3) 0.029(2) 0.040(2) -0.0051(17) 0.005(2) -0.014(2) C9 0.068(3) 0.027(2) 0.043(2) -0.0100(17) 0.003(2) 0.006(2) C10 0.041(2) 0.032(2) 0.0314(19) -0.0054(15) 0.0039(15) 0.0032(17) C11 0.0223(18) 0.041(2) 0.037(2) -0.0063(16) 0.0018(14) -0.0022(15) C12 0.027(2) 0.079(3) 0.114(4) -0.053(3) -0.007(2) 0.009(2) C13 0.037(2) 0.052(2) 0.049(2) -0.0133(19) -0.0028(17) -0.0162(18) C14 0.040(2) 0.105(4) 0.056(3) 0.018(3) 0.002(2) -0.031(3) C15 0.0234(17) 0.0304(18) 0.0213(16) -0.0011(14) 0.0038(13) 0.0000(14) C16 0.0244(17) 0.0257(17) 0.0266(17) -0.0046(14) 0.0049(13) -0.0037(14) C17 0.0308(19) 0.0310(19) 0.0263(17) -0.0042(14) 0.0049(14) -0.0018(15) C18 0.031(2) 0.034(2) 0.039(2) -0.0016(16) 0.0088(15) 0.0064(16) C19 0.044(2) 0.033(2) 0.035(2) -0.0121(16) 0.0154(16) -0.0058(17) C20 0.046(2) 0.041(2) 0.0231(18) -0.0079(16) 0.0061(15) -0.0103(18) C21 0.0325(19) 0.0325(19) 0.0253(18) -0.0027(15) 0.0030(14) -0.0065(15) C22 0.032(2) 0.056(2) 0.032(2) -0.0036(17) -0.0007(15) 0.0168(18) C23 0.063(3) 0.047(2) 0.046(2) -0.0211(19) 0.023(2) -0.001(2) C24 0.045(2) 0.048(2) 0.0270(19) -0.0028(17) -0.0015(16) -0.0028(18) C25 0.0288(18) 0.0267(17) 0.0209(16) -0.0013(13) 0.0039(13) 0.0004(14) C26 0.0261(18) 0.0329(19) 0.0226(17) 0.0019(14) 0.0062(13) 0.0000(15) C27 0.040(2) 0.031(2) 0.034(2) 0.0026(15) 0.0088(16) 0.0081(17) C28 0.053(2) 0.031(2) 0.032(2) -0.0044(16) 0.0130(17) -0.0060(18) C29 0.037(2) 0.040(2) 0.038(2) -0.0063(17) 0.0094(16) -0.0109(17) C30 0.0275(19) 0.034(2) 0.0340(19) -0.0058(15) 0.0068(14) 0.0000(15) C31 0.0265(19) 0.039(2) 0.046(2) 0.0054(17) 0.0017(16) 0.0052(16) C32 0.076(3) 0.027(2) 0.067(3) -0.007(2) 0.015(2) -0.009(2) C33 0.026(2) 0.052(3) 0.079(3) -0.013(2) 0.0016(19) -0.0060(18) C34 0.0269(18) 0.0336(19) 0.0247(17) 0.0014(14) -0.0008(13) -0.0022(15) C35 0.0238(17) 0.0285(18) 0.0239(17) 0.0009(14) -0.0015(13) -0.0073(14) C36 0.0271(18) 0.0315(19) 0.0276(18) -0.0027(15) 0.0001(14) -0.0036(15) C37 0.035(2) 0.0322(19) 0.035(2) -0.0028(16) -0.0004(15) 0.0026(16) C38 0.036(2) 0.0325(19) 0.0314(19) 0.0046(15) -0.0043(15) -0.0049(16) C39 0.041(2) 0.038(2) 0.0212(17) 0.0038(15) -0.0031(15) -0.0111(17) C40 0.0258(17) 0.0265(17) 0.0272(18) -0.0013(14) 0.0016(13) -0.0069(14) C41 0.037(2) 0.052(2) 0.0294(19) -0.0065(17) 0.0010(15) 0.0098(18) C42 0.049(2) 0.048(2) 0.044(2) 0.0091(19) -0.0080(18) 0.004(2) C43 0.037(2) 0.045(2) 0.0236(18) -0.0003(16) 0.0016(14) -0.0084(17) C44 0.0312(19) 0.0323(19) 0.0184(16) 0.0010(14) -0.0024(13) -0.0006(15) C45 0.035(2) 0.034(2) 0.0262(18) 0.0037(15) -0.0060(14) -0.0057(16) C46 0.049(2) 0.038(2) 0.034(2) 0.0007(16) -0.0098(17) -0.0127(18) C47 0.070(3) 0.031(2) 0.0251(19) -0.0028(15) -0.0056(18) -0.004(2) C48 0.050(2) 0.040(2) 0.0255(19) -0.0045(16) 0.0020(16) 0.0092(19) C49 0.036(2) 0.036(2) 0.0217(17) -0.0016(15) 0.0012(14) 0.0004(16) C50 0.032(2) 0.044(2) 0.062(3) 0.0116(19) -0.0006(18) -0.0077(18) C51 0.099(4) 0.038(2) 0.050(3) -0.012(2) -0.005(2) -0.001(2) C52 0.0265(19) 0.051(2) 0.050(2) -0.0052(19) 0.0034(16) 0.0004(17) Ti1B 0.0217(3) 0.0236(3) 0.0214(3) -0.0040(2) 0.0014(2) -0.0006(2) O1B 0.0303(12) 0.0275(12) 0.0271(12) -0.0090(10) -0.0043(9) -0.0014(10) O2B 0.0350(13) 0.0302(13) 0.0243(12) -0.0033(10) 0.0076(9) 0.0012(10) N1B 0.0263(15) 0.0285(15) 0.0207(14) -0.0029(12) 0.0022(11) -0.0038(12) N2B 0.0331(17) 0.0282(15) 0.0283(15) -0.0045(12) 0.0021(12) -0.0018(13) N3B 0.0233(14) 0.0280(15) 0.0320(15) -0.0068(12) 0.0023(11) -0.0020(12) C1B 0.036(2) 0.0311(19) 0.0269(19) -0.0066(15) 0.0052(14) -0.0029(15) C2B 0.044(2) 0.033(2) 0.0271(18) 0.0003(15) 0.0018(15) -0.0056(16) C3B 0.054(2) 0.029(2) 0.042(2) -0.0053(17) 0.0019(18) -0.0105(17) C4B 0.065(3) 0.036(2) 0.032(2) -0.0110(17) 0.0015(18) -0.0116(19) C5B 0.047(2) 0.033(2) 0.0258(18) -0.0065(15) -0.0037(15) -0.0055(17) C6B 0.038(2) 0.036(2) 0.036(2) -0.0071(16) 0.0027(16) -0.0063(17) C7B 0.054(3) 0.040(2) 0.045(2) -0.0088(18) 0.0072(18) -0.019(2) C8B 0.082(3) 0.033(2) 0.043(2) -0.0026(18) 0.005(2) -0.017(2) C9B 0.065(3) 0.031(2) 0.062(3) 0.0043(19) -0.003(2) 0.006(2) C10B 0.043(2) 0.035(2) 0.061(3) -0.0019(19) -0.0037(19) 0.0041(18) C11B 0.0230(18) 0.041(2) 0.0343(19) -0.0084(16) 0.0017(14) -0.0046(15) C12B 0.028(2) 0.071(3) 0.110(4) 0.023(3) 0.009(2) 0.012(2) C13B 0.035(2) 0.076(3) 0.059(3) 0.011(2) 0.0042(19) -0.020(2) C14B 0.050(3) 0.153(6) 0.099(4) -0.089(4) 0.017(3) -0.047(3) C15B 0.0221(17) 0.0328(19) 0.0290(18) -0.0077(14) 0.0009(13) -0.0023(14) C16B 0.0277(18) 0.0299(18) 0.0236(17) -0.0050(14) -0.0006(13) -0.0066(15) C17B 0.0328(19) 0.0272(18) 0.0313(18) -0.0033(15) -0.0030(15) -0.0031(15) C18B 0.038(2) 0.033(2) 0.040(2) -0.0058(16) -0.0059(16) 0.0012(16) C19B 0.041(2) 0.037(2) 0.036(2) 0.0027(16) -0.0116(16) -0.0071(17) C20B 0.051(2) 0.041(2) 0.0266(19) -0.0019(16) -0.0043(16) -0.0155(19) C21B 0.034(2) 0.035(2) 0.0309(19) -0.0063(15) 0.0008(15) -0.0078(16) C22B 0.033(2) 0.045(2) 0.037(2) -0.0141(17) -0.0029(15) 0.0092(17) C23B 0.063(3) 0.054(3) 0.047(2) 0.005(2) -0.024(2) -0.004(2) C24B 0.052(2) 0.060(3) 0.0256(19) -0.0124(18) 0.0070(17) -0.003(2) C25B 0.0296(19) 0.0304(18) 0.0256(17) -0.0099(14) -0.0046(13) -0.0010(15) C26B 0.032(2) 0.039(2) 0.037(2) -0.0185(16) -0.0094(15) 0.0035(16) C27B 0.042(2) 0.038(2) 0.049(2) -0.0189(18) -0.0151(18) 0.0103(18) C28B 0.064(3) 0.033(2) 0.032(2) -0.0101(16) -0.0134(18) -0.004(2) C29B 0.047(2) 0.037(2) 0.034(2) -0.0069(16) -0.0020(16) -0.0103(18) C30B 0.0329(19) 0.035(2) 0.0261(18) -0.0045(15) -0.0026(14) -0.0037(16) C31B 0.027(2) 0.058(3) 0.079(3) -0.037(2) -0.0076(19) 0.0050(19) C32B 0.085(3) 0.035(2) 0.071(3) -0.010(2) -0.012(3) 0.002(2) C33B 0.028(2) 0.049(2) 0.060(3) -0.004(2) 0.0033(17) -0.0083(18) C34B 0.0261(18) 0.037(2) 0.0233(17) -0.0023(15) 0.0034(13) 0.0009(15) C35B 0.0217(17) 0.0315(18) 0.0267(17) -0.0020(14) 0.0065(13) -0.0040(14) C36B 0.0266(18) 0.0325(19) 0.0253(17) -0.0026(14) 0.0045(14) -0.0019(15) C37B 0.0276(19) 0.0301(19) 0.037(2) -0.0017(15) 0.0024(15) 0.0003(15) C38B 0.036(2) 0.0290(19) 0.0335(19) -0.0079(15) 0.0109(15) -0.0055(16) C39B 0.036(2) 0.036(2) 0.0251(17) -0.0078(15) 0.0053(15) -0.0075(16) C40B 0.0252(18) 0.0337(19) 0.0265(18) 0.0005(15) 0.0044(13) -0.0061(15) C41B 0.030(2) 0.053(2) 0.033(2) -0.0082(17) -0.0059(15) 0.0112(17) C42B 0.049(2) 0.039(2) 0.044(2) -0.0160(18) 0.0112(18) -0.0003(18) C43B 0.037(2) 0.047(2) 0.0295(19) 0.0001(16) -0.0005(15) -0.0043(17) C44B 0.033(2) 0.0360(19) 0.0213(17) -0.0039(14) 0.0053(14) 0.0042(16) C45B 0.047(2) 0.033(2) 0.0276(19) -0.0107(15) 0.0070(16) 0.0022(17) C46B 0.069(3) 0.039(2) 0.033(2) -0.0129(17) 0.0137(19) -0.008(2) C47B 0.086(3) 0.033(2) 0.025(2) -0.0006(16) 0.009(2) 0.011(2) C48B 0.064(3) 0.043(2) 0.031(2) 0.0008(17) 0.0054(18) 0.021(2) C49B 0.040(2) 0.046(2) 0.0309(19) -0.0003(17) 0.0054(16) 0.0129(18) C50B 0.035(2) 0.048(2) 0.065(3) -0.020(2) 0.0027(19) -0.0067(18) C51B 0.127(4) 0.036(2) 0.043(3) 0.002(2) 0.013(3) 0.007(3) C52B 0.036(2) 0.065(3) 0.063(3) 0.001(2) 0.006(2) 0.015(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N3 1.715(3) . ? Ti O2 1.872(2) . ? Ti O1 1.887(2) . ? Ti N2 2.247(3) . ? Ti N1 2.271(3) . ? O1 C15 1.403(3) . ? O2 C34 1.402(4) . ? N1 C1 1.332(4) . ? N1 C5 1.335(4) . ? N2 C6 1.336(4) . ? N2 C10 1.336(4) . ? N3 C11 1.458(4) . ? C1 C2 1.377(5) . ? C2 C3 1.364(6) . ? C3 C4 1.372(5) . ? C4 C5 1.379(5) . ? C6 C7 1.371(5) . ? C7 C8 1.372(5) . ? C8 C9 1.373(6) . ? C9 C10 1.385(5) . ? C11 C12 1.514(5) . ? C11 C14 1.528(5) . ? C11 C13 1.532(5) . ? C15 C16 1.539(4) . ? C15 C25 1.540(4) . ? C16 C17 1.408(4) . ? C16 C21 1.408(4) . ? C17 C18 1.391(4) . ? C17 C22 1.517(5) . ? C18 C19 1.382(5) . ? C19 C20 1.376(5) . ? C19 C23 1.512(5) . ? C20 C21 1.395(5) . ? C21 C24 1.506(5) . ? C25 C30 1.407(5) . ? C25 C26 1.410(4) . ? C26 C27 1.383(5) . ? C26 C31 1.515(5) . ? C27 C28 1.372(5) . ? C28 C29 1.381(5) . ? C28 C32 1.512(5) . ? C29 C30 1.389(5) . ? C30 C33 1.512(5) . ? C34 C35 1.544(4) . ? C34 C44 1.545(5) . ? C35 C36 1.411(4) . ? C35 C40 1.413(4) . ? C36 C37 1.399(4) . ? C36 C41 1.514(4) . ? C37 C38 1.377(5) . ? C38 C39 1.382(5) . ? C38 C42 1.512(5) . ? C39 C40 1.387(4) . ? C40 C43 1.505(4) . ? C44 C45 1.397(5) . ? C44 C49 1.411(5) . ? C45 C46 1.392(5) . ? C45 C50 1.512(5) . ? C46 C47 1.382(5) . ? C47 C48 1.388(5) . ? C47 C51 1.517(5) . ? C48 C49 1.390(5) . ? C49 C52 1.509(5) . ? Ti1B N3B 1.716(3) . ? Ti1B O2B 1.875(2) . ? Ti1B O1B 1.889(2) . ? Ti1B N2B 2.243(3) . ? Ti1B N1B 2.258(3) . ? O1B C15B 1.404(4) . ? O2B C34B 1.405(4) . ? N1B C1B 1.331(4) . ? N1B C5B 1.341(4) . ? N2B C6B 1.327(4) . ? N2B C10B 1.333(4) . ? N3B C11B 1.453(4) . ? C1B C2B 1.373(5) . ? C2B C3B 1.377(5) . ? C3B C4B 1.370(5) . ? C4B C5B 1.379(5) . ? C6B C7B 1.392(5) . ? C7B C8B 1.358(6) . ? C8B C9B 1.372(6) . ? C9B C10B 1.387(5) . ? C11B C12B 1.506(5) . ? C11B C13B 1.524(5) . ? C11B C14B 1.529(5) . ? C15B C25B 1.541(4) . ? C15B C16B 1.541(4) . ? C16B C21B 1.409(4) . ? C16B C17B 1.413(4) . ? C17B C18B 1.391(5) . ? C17B C22B 1.507(5) . ? C18B C19B 1.381(5) . ? C19B C20B 1.388(5) . ? C19B C23B 1.515(5) . ? C20B C21B 1.386(5) . ? C21B C24B 1.519(5) . ? C25B C30B 1.401(5) . ? C25B C26B 1.409(5) . ? C26B C27B 1.390(5) . ? C26B C31B 1.515(5) . ? C27B C28B 1.376(5) . ? C28B C29B 1.382(5) . ? C28B C32B 1.504(5) . ? C29B C30B 1.400(5) . ? C30B C33B 1.506(5) . ? C34B C35B 1.537(4) . ? C34B C44B 1.542(5) . ? C35B C40B 1.412(4) . ? C35B C36B 1.416(4) . ? C36B C37B 1.399(4) . ? C36B C41B 1.510(4) . ? C37B C38B 1.382(5) . ? C38B C39B 1.381(5) . ? C38B C42B 1.505(5) . ? C39B C40B 1.389(5) . ? C40B C43B 1.507(5) . ? C44B C45B 1.401(5) . ? C44B C49B 1.407(5) . ? C45B C46B 1.391(5) . ? C45B C50B 1.502(5) . ? C46B C47B 1.377(6) . ? C47B C48B 1.393(6) . ? C47B C51B 1.513(5) . ? C48B C49B 1.391(5) . ? C49B C52B 1.506(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ti O2 118.29(11) . . ? N3 Ti O1 118.21(11) . . ? O2 Ti O1 123.24(10) . . ? N3 Ti N2 99.08(11) . . ? O2 Ti N2 88.33(9) . . ? O1 Ti N2 88.10(9) . . ? N3 Ti N1 90.58(11) . . ? O2 Ti N1 86.56(9) . . ? O1 Ti N1 87.84(9) . . ? N2 Ti N1 170.32(10) . . ? C15 O1 Ti 149.44(19) . . ? C34 O2 Ti 151.8(2) . . ? C1 N1 C5 117.4(3) . . ? C1 N1 Ti 122.6(2) . . ? C5 N1 Ti 119.8(2) . . ? C6 N2 C10 117.5(3) . . ? C6 N2 Ti 118.7(2) . . ? C10 N2 Ti 123.7(2) . . ? C11 N3 Ti 167.8(2) . . ? N1 C1 C2 122.9(3) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 119.0(4) . . ? C3 C4 C5 118.6(4) . . ? N1 C5 C4 123.0(3) . . ? N2 C6 C7 123.3(3) . . ? C6 C7 C8 118.9(4) . . ? C7 C8 C9 118.8(4) . . ? C8 C9 C10 119.1(4) . . ? N2 C10 C9 122.4(4) . . ? N3 C11 C12 109.9(3) . . ? N3 C11 C14 108.9(3) . . ? C12 C11 C14 111.1(4) . . ? N3 C11 C13 109.5(3) . . ? C12 C11 C13 109.4(3) . . ? C14 C11 C13 108.2(3) . . ? O1 C15 C16 114.7(2) . . ? O1 C15 C25 109.2(2) . . ? C16 C15 C25 115.3(2) . . ? C17 C16 C21 118.5(3) . . ? C17 C16 C15 125.3(3) . . ? C21 C16 C15 116.2(3) . . ? C18 C17 C16 118.9(3) . . ? C18 C17 C22 115.8(3) . . ? C16 C17 C22 125.2(3) . . ? C19 C18 C17 123.2(3) . . ? C20 C19 C18 117.3(3) . . ? C20 C19 C23 121.3(3) . . ? C18 C19 C23 121.4(3) . . ? C19 C20 C21 122.1(3) . . ? C20 C21 C16 120.0(3) . . ? C20 C21 C24 117.5(3) . . ? C16 C21 C24 122.6(3) . . ? C30 C25 C26 117.9(3) . . ? C30 C25 C15 124.7(3) . . ? C26 C25 C15 117.2(3) . . ? C27 C26 C25 120.1(3) . . ? C27 C26 C31 118.3(3) . . ? C25 C26 C31 121.6(3) . . ? C28 C27 C26 122.4(3) . . ? C27 C28 C29 117.5(3) . . ? C27 C28 C32 120.9(3) . . ? C29 C28 C32 121.5(4) . . ? C28 C29 C30 122.6(3) . . ? C29 C30 C25 119.5(3) . . ? C29 C30 C33 117.1(3) . . ? C25 C30 C33 123.4(3) . . ? O2 C34 C35 114.6(3) . . ? O2 C34 C44 109.2(2) . . ? C35 C34 C44 114.5(3) . . ? C36 C35 C40 118.0(3) . . ? C36 C35 C34 125.2(3) . . ? C40 C35 C34 116.7(3) . . ? C37 C36 C35 119.2(3) . . ? C37 C36 C41 115.2(3) . . ? C35 C36 C41 125.6(3) . . ? C38 C37 C36 123.2(3) . . ? C37 C38 C39 116.8(3) . . ? C37 C38 C42 121.2(3) . . ? C39 C38 C42 122.0(3) . . ? C38 C39 C40 123.0(3) . . ? C39 C40 C35 119.8(3) . . ? C39 C40 C43 117.5(3) . . ? C35 C40 C43 122.7(3) . . ? C45 C44 C49 119.1(3) . . ? C45 C44 C34 121.9(3) . . ? C49 C44 C34 118.9(3) . . ? C46 C45 C44 119.0(3) . . ? C46 C45 C50 118.3(3) . . ? C44 C45 C50 122.6(3) . . ? C47 C46 C45 123.0(4) . . ? C46 C47 C48 117.1(3) . . ? C46 C47 C51 121.0(4) . . ? C48 C47 C51 121.8(4) . . ? C47 C48 C49 122.3(3) . . ? C48 C49 C44 119.4(3) . . ? C48 C49 C52 118.2(3) . . ? C44 C49 C52 122.4(3) . . ? N3B Ti1B O2B 119.08(11) . . ? N3B Ti1B O1B 117.39(11) . . ? O2B Ti1B O1B 123.25(10) . . ? N3B Ti1B N2B 99.17(11) . . ? O2B Ti1B N2B 87.71(9) . . ? O1B Ti1B N2B 88.75(9) . . ? N3B Ti1B N1B 90.37(11) . . ? O2B Ti1B N1B 86.85(9) . . ? O1B Ti1B N1B 87.64(9) . . ? N2B Ti1B N1B 170.42(10) . . ? C15B O1B Ti1B 147.27(19) . . ? C34B O2B Ti1B 152.6(2) . . ? C1B N1B C5B 117.6(3) . . ? C1B N1B Ti1B 120.0(2) . . ? C5B N1B Ti1B 122.1(2) . . ? C6B N2B C10B 117.5(3) . . ? C6B N2B Ti1B 118.2(2) . . ? C10B N2B Ti1B 124.1(2) . . ? C11B N3B Ti1B 167.7(2) . . ? N1B C1B C2B 123.3(3) . . ? C1B C2B C3B 118.5(3) . . ? C4B C3B C2B 119.1(3) . . ? C3B C4B C5B 119.0(3) . . ? N1B C5B C4B 122.5(3) . . ? N2B C6B C7B 123.0(3) . . ? C8B C7B C6B 118.9(4) . . ? C7B C8B C9B 119.1(4) . . ? C8B C9B C10B 118.8(4) . . ? N2B C10B C9B 122.8(4) . . ? N3B C11B C12B 110.0(3) . . ? N3B C11B C13B 110.3(3) . . ? C12B C11B C13B 109.0(3) . . ? N3B C11B C14B 108.7(3) . . ? C12B C11B C14B 111.1(4) . . ? C13B C11B C14B 107.7(4) . . ? O1B C15B C25B 108.4(2) . . ? O1B C15B C16B 114.9(2) . . ? C25B C15B C16B 115.0(3) . . ? C21B C16B C17B 118.3(3) . . ? C21B C16B C15B 116.5(3) . . ? C17B C16B C15B 125.2(3) . . ? C18B C17B C16B 118.9(3) . . ? C18B C17B C22B 115.9(3) . . ? C16B C17B C22B 125.2(3) . . ? C19B C18B C17B 123.6(3) . . ? C18B C19B C20B 116.6(3) . . ? C18B C19B C23B 121.7(4) . . ? C20B C19B C23B 121.8(3) . . ? C21B C20B C19B 122.6(3) . . ? C20B C21B C16B 120.1(3) . . ? C20B C21B C24B 117.4(3) . . ? C16B C21B C24B 122.5(3) . . ? C30B C25B C26B 118.5(3) . . ? C30B C25B C15B 123.5(3) . . ? C26B C25B C15B 117.8(3) . . ? C27B C26B C25B 119.5(3) . . ? C27B C26B C31B 118.3(3) . . ? C25B C26B C31B 122.2(3) . . ? C28B C27B C26B 123.0(3) . . ? C27B C28B C29B 117.0(3) . . ? C27B C28B C32B 121.6(4) . . ? C29B C28B C32B 121.4(4) . . ? C28B C29B C30B 122.6(4) . . ? C29B C30B C25B 119.4(3) . . ? C29B C30B C33B 117.2(3) . . ? C25B C30B C33B 123.3(3) . . ? O2B C34B C35B 114.5(3) . . ? O2B C34B C44B 108.7(3) . . ? C35B C34B C44B 115.8(3) . . ? C40B C35B C36B 117.9(3) . . ? C40B C35B C34B 116.4(3) . . ? C36B C35B C34B 125.5(3) . . ? C37B C36B C35B 118.8(3) . . ? C37B C36B C41B 115.4(3) . . ? C35B C36B C41B 125.8(3) . . ? C38B C37B C36B 123.6(3) . . ? C39B C38B C37B 116.8(3) . . ? C39B C38B C42B 121.8(3) . . ? C37B C38B C42B 121.3(3) . . ? C38B C39B C40B 122.5(3) . . ? C39B C40B C35B 120.4(3) . . ? C39B C40B C43B 116.8(3) . . ? C35B C40B C43B 122.8(3) . . ? C45B C44B C49B 119.4(3) . . ? C45B C44B C34B 122.7(3) . . ? C49B C44B C34B 117.8(3) . . ? C46B C45B C44B 118.9(3) . . ? C46B C45B C50B 118.5(4) . . ? C44B C45B C50B 122.6(3) . . ? C47B C46B C45B 123.3(4) . . ? C46B C47B C48B 116.7(4) . . ? C46B C47B C51B 121.2(4) . . ? C48B C47B C51B 122.1(4) . . ? C49B C48B C47B 122.7(4) . . ? C48B C49B C44B 118.9(4) . . ? C48B C49B C52B 118.3(3) . . ? C44B C49B C52B 122.8(3) . . ? #===END