Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email TJBOYLE@SANDIA.GOV _publ_contact_author_name 'Dr Timothy J. Boyle' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Advanced Materials Laboratory Sandia National Laboratories 1001 University Blvd. SE Albuquerque NM UNITED STATES OF AMERICA ; _publ_section_title ; Dihydroxypyridimine, a Selective Bridging Ligand for Controlled Metal Alkoxide Structures. ; loop_ _publ_author_name T.J.Boyle 'Todd M. Alam' 'Mark A. Rodriguez' data_tjb136s _database_code_CSD 218027 _chemical_name_common Ti4(u-DHP)2(u-OPri)2(OPri)10(Py)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H98 N6 O16 Ti4' _chemical_formula_weight 1278.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.787(3) _cell_length_b 11.751(3) _cell_length_c 13.251(3) _cell_angle_alpha 90.901(4) _cell_angle_beta 91.650(4) _cell_angle_gamma 92.000(4) _cell_volume 1677.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description spherical _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7803 _exptl_absorpt_correction_T_max 0.8183 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13728 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6802 _reflns_number_gt 4680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+0.3085P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6802 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1983 _refine_ls_wR_factor_gt 0.1775 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.268 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.43584(5) 0.08568(5) -0.07647(4) 0.0373(2) Uani 1 1 d . . . Ti2 Ti 0.05971(5) 0.26478(5) 0.30152(5) 0.0418(2) Uani 1 1 d . . . N1 N 0.3154(2) 0.1395(2) 0.0525(2) 0.0405(7) Uani 1 1 d . . . N2 N 0.1866(2) 0.1969(2) 0.1821(2) 0.0430(7) Uani 1 1 d . . . N3 N 0.0404(2) 0.0741(2) 0.3315(2) 0.0379(6) Uani 1 1 d . . . O1 O 0.2467(2) 0.0822(2) -0.09890(18) 0.0433(6) Uani 1 1 d . . . O2 O -0.0167(2) 0.2092(2) 0.16122(18) 0.0451(6) Uani 1 1 d . . . O3 O 0.41627(19) -0.07270(19) -0.01022(18) 0.0407(5) Uani 1 1 d . . . O4 O 0.4655(2) 0.0192(2) -0.19587(18) 0.0460(6) Uani 1 1 d . . . O5 O 0.4524(2) 0.2306(2) -0.11231(19) 0.0468(6) Uani 1 1 d . . . O6 O 0.0763(2) 0.4069(2) 0.2557(2) 0.0527(7) Uani 1 1 d . . . O7 O 0.1830(2) 0.2712(2) 0.39859(18) 0.0457(6) Uani 1 1 d . . . O8 O -0.0831(2) 0.27621(19) 0.3706(2) 0.0516(7) Uani 1 1 d . . . C1 C 0.2965(3) 0.1753(3) 0.1458(3) 0.0411(8) Uani 1 1 d . . . H1 H 0.3670 0.1863 0.1900 0.049 Uiso 1 1 calc R . . C2 C 0.0839(3) 0.1804(3) 0.1177(3) 0.0426(8) Uani 1 1 d . . . C3 C 0.0948(3) 0.1384(3) 0.0201(3) 0.0422(8) Uani 1 1 d . . . H3 H 0.0243 0.1232 -0.0233 0.051 Uiso 1 1 calc R . . C4 C 0.2142(3) 0.1199(3) -0.0105(3) 0.0398(8) Uani 1 1 d . . . C5 C 0.3150(3) -0.1544(3) -0.0358(3) 0.0558(11) Uani 1 1 d . . . H5 H 0.2553 -0.1160 -0.0821 0.067 Uiso 1 1 calc R . . C6 C 0.2475(3) -0.1848(4) 0.0582(4) 0.0697(14) Uani 1 1 d . . . H6A H 0.3043 -0.2214 0.1056 0.105 Uiso 1 1 calc R . . H6B H 0.1773 -0.2373 0.0407 0.105 Uiso 1 1 calc R . . H6C H 0.2170 -0.1155 0.0896 0.105 Uiso 1 1 calc R . . C7 C 0.3636(5) -0.2538(4) -0.0919(4) 0.0837(16) Uani 1 1 d . . . H7A H 0.4037 -0.2274 -0.1531 0.126 Uiso 1 1 calc R . . H7B H 0.2948 -0.3074 -0.1105 0.126 Uiso 1 1 calc R . . H7C H 0.4242 -0.2920 -0.0488 0.126 Uiso 1 1 calc R . . C8 C 0.4604(4) 0.0597(4) -0.2969(3) 0.0556(10) Uani 1 1 d . . . H8 H 0.4097 0.1293 -0.2988 0.067 Uiso 1 1 calc R . . C9 C 0.3977(5) -0.0310(4) -0.3639(3) 0.0754(13) Uani 1 1 d . . . H9A H 0.4503 -0.0972 -0.3673 0.113 Uiso 1 1 calc R . . H9B H 0.3847 -0.0010 -0.4319 0.113 Uiso 1 1 calc R . . H9C H 0.3175 -0.0537 -0.3362 0.113 Uiso 1 1 calc R . . C10 C 0.5889(5) 0.0906(5) -0.3282(4) 0.0939(18) Uani 1 1 d . . . H10A H 0.6260 0.1486 -0.2815 0.141 Uiso 1 1 calc R . . H10B H 0.5859 0.1209 -0.3967 0.141 Uiso 1 1 calc R . . H10C H 0.6392 0.0228 -0.3270 0.141 Uiso 1 1 calc R . . C11 C 0.4215(8) 0.3485(7) -0.1066(6) 0.060(2) Uani 0.70 1 d P . . C11' C 0.396(2) 0.335(2) -0.153(3) 0.125(14) Uani 0.30 1 d P . . C12 C 0.5119(9) 0.4196(7) -0.1576(10) 0.095(3) Uani 0.70 1 d P . . C12' C 0.509(2) 0.3860(17) -0.2208(13) 0.069(5) Uani 0.30 1 d P . . C13 C 0.2892(6) 0.3558(6) -0.1602(6) 0.0697(19) Uani 0.70 1 d P . . C13' C 0.340(3) 0.3978(16) -0.075(3) 0.133(12) Uani 0.30 1 d P . . C14 C 0.0466(5) 0.4824(4) 0.1766(4) 0.0714(13) Uani 1 1 d . . . H14 H -0.0354 0.4566 0.1455 0.086 Uiso 1 1 calc R . . C15 C 0.1419(6) 0.4786(5) 0.0962(4) 0.0927(17) Uani 1 1 d . . . H15A H 0.2241 0.4987 0.1261 0.139 Uiso 1 1 calc R . . H15B H 0.1215 0.5330 0.0434 0.139 Uiso 1 1 calc R . . H15C H 0.1423 0.4017 0.0666 0.139 Uiso 1 1 calc R . . C16 C 0.0337(7) 0.5993(4) 0.2200(5) 0.112(2) Uani 1 1 d . . . H16A H -0.0339 0.5984 0.2678 0.169 Uiso 1 1 calc R . . H16B H 0.0151 0.6521 0.1655 0.169 Uiso 1 1 calc R . . H16C H 0.1114 0.6241 0.2551 0.169 Uiso 1 1 calc R . . C17 C 0.2763(9) 0.3474(8) 0.4275(7) 0.057(2) Uani 0.50 1 d P . . C17' C 0.3129(7) 0.2891(7) 0.4152(6) 0.0438(18) Uani 0.50 1 d P . . C18 C 0.3338(6) 0.3033(6) 0.5321(4) 0.114(3) Uani 1 1 d . . . C19 C 0.3662(5) 0.3850(6) 0.3624(4) 0.0930(18) Uani 1 1 d . . . C20 C -0.1610(4) 0.3694(3) 0.3892(3) 0.0559(10) Uani 1 1 d . . . C21 C -0.2794(7) 0.3391(7) 0.4105(9) 0.066(2) Uani 0.50 1 d P . . C21' C -0.2447(7) 0.3352(6) 0.4932(6) 0.0483(18) Uani 0.50 1 d P . . C22 C -0.0806(7) 0.4488(7) 0.4578(7) 0.057(2) Uani 0.50 1 d P . . C22' C -0.2545(8) 0.3738(8) 0.3091(7) 0.064(2) Uani 0.50 1 d P . . C23 C 0.1127(3) 0.0254(3) 0.4016(3) 0.0418(8) Uani 1 1 d . . . H23 H 0.1795 0.0697 0.4320 0.050 Uiso 1 1 calc R . . C24 C 0.0951(3) -0.0855(3) 0.4316(3) 0.0485(9) Uani 1 1 d . . . H24 H 0.1476 -0.1158 0.4826 0.058 Uiso 1 1 calc R . . C25 C 0.0004(4) -0.1521(3) 0.3870(3) 0.0534(10) Uani 1 1 d . . . H25 H -0.0140 -0.2287 0.4067 0.064 Uiso 1 1 calc R . . C26 C -0.0729(4) -0.1048(3) 0.3130(3) 0.0553(10) Uani 1 1 d . . . H26 H -0.1374 -0.1492 0.2795 0.066 Uiso 1 1 calc R . . C27 C -0.0515(3) 0.0084(3) 0.2877(3) 0.0489(9) Uani 1 1 d . . . H27 H -0.1037 0.0407 0.2377 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0289(3) 0.0385(3) 0.0448(4) 0.0169(3) -0.0013(2) 0.0012(2) Ti2 0.0357(4) 0.0361(3) 0.0539(4) 0.0140(3) -0.0014(3) 0.0011(2) N1 0.0268(14) 0.0474(16) 0.0476(17) 0.0171(13) -0.0044(12) 0.0016(11) N2 0.0312(15) 0.0502(17) 0.0478(17) 0.0138(13) -0.0023(12) 0.0007(12) N3 0.0339(14) 0.0355(14) 0.0448(16) 0.0035(12) 0.0067(12) 0.0032(11) O1 0.0322(12) 0.0497(14) 0.0482(15) 0.0126(11) -0.0032(10) 0.0035(10) O2 0.0301(12) 0.0488(14) 0.0570(15) 0.0127(11) 0.0024(11) 0.0041(10) O3 0.0287(11) 0.0380(12) 0.0548(14) 0.0171(10) -0.0076(10) -0.0074(9) O4 0.0410(13) 0.0497(14) 0.0479(14) 0.0130(11) 0.0000(11) 0.0072(11) O5 0.0407(13) 0.0394(13) 0.0613(16) 0.0216(11) 0.0018(11) 0.0045(10) O6 0.0541(15) 0.0417(14) 0.0616(17) 0.0193(12) -0.0092(12) -0.0052(11) O7 0.0455(14) 0.0408(13) 0.0505(14) 0.0113(11) -0.0054(11) -0.0033(10) O8 0.0407(14) 0.0335(12) 0.0813(19) 0.0042(12) 0.0056(13) 0.0084(10) C1 0.0296(17) 0.0471(19) 0.047(2) 0.0163(16) -0.0047(14) 0.0001(14) C2 0.0298(17) 0.0422(18) 0.056(2) 0.0199(16) -0.0033(15) 0.0003(14) C3 0.0306(17) 0.048(2) 0.048(2) 0.0131(16) -0.0062(14) 0.0020(14) C4 0.0339(17) 0.0386(18) 0.047(2) 0.0182(15) -0.0037(14) -0.0010(13) C5 0.0366(19) 0.046(2) 0.083(3) 0.025(2) -0.0167(19) -0.0093(16) C6 0.0298(19) 0.065(3) 0.115(4) 0.047(3) 0.000(2) -0.0063(17) C7 0.069(3) 0.060(3) 0.120(4) -0.012(3) -0.013(3) -0.014(2) C8 0.058(2) 0.064(3) 0.046(2) 0.0126(18) 0.0090(18) 0.0160(19) C9 0.071(3) 0.095(4) 0.060(3) -0.006(3) -0.004(2) 0.011(3) C10 0.087(4) 0.124(5) 0.071(3) 0.016(3) 0.022(3) -0.018(3) C11 0.061(5) 0.044(4) 0.074(5) 0.014(4) -0.026(4) 0.012(3) C11' 0.068(13) 0.075(14) 0.23(3) 0.11(2) -0.101(19) -0.043(10) C12 0.065(5) 0.045(4) 0.177(11) 0.038(6) 0.017(7) -0.003(4) C12' 0.091(13) 0.053(11) 0.065(11) 0.036(9) 0.005(10) -0.002(9) C13 0.058(4) 0.050(4) 0.104(5) 0.031(4) -0.004(4) 0.017(3) C13' 0.13(2) 0.036(9) 0.24(3) -0.021(14) 0.08(2) -0.007(11) C14 0.086(3) 0.052(3) 0.076(3) 0.025(2) -0.003(3) 0.001(2) C15 0.111(4) 0.079(4) 0.088(4) 0.032(3) 0.013(3) -0.013(3) C16 0.190(7) 0.048(3) 0.102(4) 0.029(3) 0.022(4) 0.015(3) C17 0.062(6) 0.054(6) 0.052(5) -0.004(4) -0.012(4) -0.007(5) C17' 0.037(4) 0.044(5) 0.051(5) 0.012(4) -0.003(3) 0.006(3) C18 0.135(5) 0.148(6) 0.053(3) 0.032(3) -0.036(3) -0.069(5) C19 0.078(3) 0.129(5) 0.068(3) 0.011(3) 0.002(3) -0.051(3) C20 0.054(2) 0.042(2) 0.071(3) -0.0103(18) -0.017(2) 0.0203(17) C21 0.036(4) 0.060(5) 0.102(8) -0.015(5) 0.015(5) 0.008(4) C21' 0.049(4) 0.050(4) 0.047(4) 0.007(4) 0.013(4) 0.014(3) C22 0.046(4) 0.050(4) 0.077(6) -0.019(4) 0.003(4) 0.009(3) C22' 0.049(5) 0.080(6) 0.063(5) 0.019(5) -0.010(4) 0.013(4) C23 0.0371(18) 0.0390(18) 0.050(2) 0.0056(15) 0.0043(15) 0.0037(14) C24 0.048(2) 0.0394(19) 0.059(2) 0.0091(17) 0.0050(17) 0.0121(16) C25 0.060(2) 0.0321(18) 0.069(3) 0.0077(17) 0.012(2) 0.0042(16) C26 0.054(2) 0.039(2) 0.073(3) 0.0016(18) 0.000(2) -0.0029(17) C27 0.045(2) 0.044(2) 0.058(2) 0.0056(17) 0.0016(17) 0.0032(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.779(2) . ? Ti1 O4 1.796(3) . ? Ti1 O3 1.951(2) 2_655 ? Ti1 O1 2.052(2) . ? Ti1 O3 2.077(2) . ? Ti1 N1 2.271(3) . ? Ti1 C4 2.611(3) . ? Ti1 Ti1 3.2000(12) 2_655 ? Ti2 O6 1.791(2) . ? Ti2 O8 1.822(3) . ? Ti2 O7 1.822(2) . ? Ti2 O2 2.097(3) . ? Ti2 N2 2.275(3) . ? Ti2 N3 2.285(3) . ? Ti2 C2 2.639(4) . ? N1 C1 1.323(4) . ? N1 C4 1.366(4) . ? N2 C1 1.323(4) . ? N2 C2 1.384(4) . ? N3 C23 1.343(4) . ? N3 C27 1.348(4) . ? O1 C4 1.308(4) . ? O2 C2 1.297(4) . ? O3 C5 1.458(4) . ? O3 Ti1 1.951(2) 2_655 ? O4 C8 1.428(4) . ? O5 C11 1.438(8) . ? O5 C11' 1.49(2) . ? O6 C14 1.420(5) . ? O7 C17 1.365(9) . ? O7 C17' 1.419(8) . ? O8 C20 1.426(4) . ? C2 C3 1.387(5) . ? C3 C4 1.385(5) . ? C5 C7 1.494(6) . ? C5 C6 1.502(6) . ? C8 C10 1.493(6) . ? C8 C9 1.505(6) . ? C11 C12 1.450(13) . ? C11 C13 1.581(10) . ? C11' C13' 1.41(5) . ? C11' C12' 1.65(4) . ? C14 C16 1.494(7) . ? C14 C15 1.504(7) . ? C17 C19 1.381(11) . ? C17 C18 1.604(10) . ? C17' C19 1.447(10) . ? C17' C18 1.564(10) . ? C20 C21 1.353(9) . ? C20 C22' 1.446(9) . ? C20 C22 1.523(9) . ? C20 C21' 1.715(8) . ? C23 C24 1.377(5) . ? C24 C25 1.379(5) . ? C25 C26 1.377(6) . ? C26 C27 1.389(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 O5 Ti1 O4 98.78(12) . . ? O5 Ti1 O3 100.46(10) . 2_655 ? O4 Ti1 O3 107.79(11) . 2_655 ? O5 Ti1 O1 92.99(10) . . ? O4 Ti1 O1 94.68(11) . . ? O3 Ti1 O1 151.48(10) 2_655 . ? O5 Ti1 O3 170.45(11) . . ? O4 Ti1 O3 90.62(10) . . ? O3 Ti1 O3 74.83(9) 2_655 . ? O1 Ti1 O3 87.90(9) . . ? O5 Ti1 N1 89.44(11) . . ? O4 Ti1 N1 154.95(11) . . ? O3 Ti1 N1 93.75(10) 2_655 . ? O1 Ti1 N1 61.11(10) . . ? O3 Ti1 N1 82.67(10) . . ? O5 Ti1 C4 90.93(10) . . ? O4 Ti1 C4 124.11(11) . . ? O3 Ti1 C4 124.32(11) 2_655 . ? O1 Ti1 C4 29.60(10) . . ? O3 Ti1 C4 85.15(9) . . ? N1 Ti1 C4 31.52(10) . . ? O5 Ti1 Ti1 138.66(8) . 2_655 ? O4 Ti1 Ti1 101.14(8) . 2_655 ? O3 Ti1 Ti1 38.79(6) 2_655 2_655 ? O1 Ti1 Ti1 120.79(7) . 2_655 ? O3 Ti1 Ti1 36.04(6) . 2_655 ? N1 Ti1 Ti1 87.54(7) . 2_655 ? C4 Ti1 Ti1 106.79(7) . 2_655 ? O6 Ti2 O8 100.09(12) . . ? O6 Ti2 O7 99.02(11) . . ? O8 Ti2 O7 104.75(12) . . ? O6 Ti2 O2 90.29(11) . . ? O8 Ti2 O2 99.00(11) . . ? O7 Ti2 O2 152.42(11) . . ? O6 Ti2 N2 91.91(12) . . ? O8 Ti2 N2 156.61(12) . . ? O7 Ti2 N2 92.96(11) . . ? O2 Ti2 N2 60.64(9) . . ? O6 Ti2 N3 170.15(12) . . ? O8 Ti2 N3 85.62(10) . . ? O7 Ti2 N3 87.14(10) . . ? O2 Ti2 N3 80.84(10) . . ? N2 Ti2 N3 80.05(10) . . ? O6 Ti2 C2 90.83(12) . . ? O8 Ti2 C2 127.32(11) . . ? O7 Ti2 C2 124.28(11) . . ? O2 Ti2 C2 29.01(9) . . ? N2 Ti2 C2 31.64(10) . . ? N3 Ti2 C2 79.34(10) . . ? C1 N1 C4 118.0(3) . . ? C1 N1 Ti1 154.0(2) . . ? C4 N1 Ti1 88.1(2) . . ? C1 N2 C2 117.5(3) . . ? C1 N2 Ti2 153.4(2) . . ? C2 N2 Ti2 88.8(2) . . ? C23 N3 C27 117.1(3) . . ? C23 N3 Ti2 121.0(2) . . ? C27 N3 Ti2 121.6(2) . . ? C4 O1 Ti1 99.61(19) . . ? C2 O2 Ti2 99.3(2) . . ? C5 O3 Ti1 131.1(2) . 2_655 ? C5 O3 Ti1 123.47(19) . . ? Ti1 O3 Ti1 105.17(9) 2_655 . ? C8 O4 Ti1 132.3(2) . . ? C11 O5 C11' 26.6(13) . . ? C11 O5 Ti1 153.0(4) . . ? C11' O5 Ti1 149.4(8) . . ? C14 O6 Ti2 146.0(3) . . ? C17 O7 C17' 34.1(4) . . ? C17 O7 Ti2 135.8(4) . . ? C17' O7 Ti2 143.7(4) . . ? C20 O8 Ti2 132.2(2) . . ? N1 C1 N2 124.8(3) . . ? O2 C2 N2 111.2(3) . . ? O2 C2 C3 127.3(3) . . ? N2 C2 C3 121.5(3) . . ? O2 C2 Ti2 51.67(17) . . ? N2 C2 Ti2 59.55(19) . . ? C3 C2 Ti2 178.5(2) . . ? C4 C3 C2 116.2(3) . . ? O1 C4 N1 111.2(3) . . ? O1 C4 C3 126.8(3) . . ? N1 C4 C3 122.0(3) . . ? O1 C4 Ti1 50.79(15) . . ? N1 C4 Ti1 60.40(18) . . ? C3 C4 Ti1 177.4(3) . . ? O3 C5 C7 109.8(3) . . ? O3 C5 C6 109.4(3) . . ? C7 C5 C6 114.4(4) . . ? O4 C8 C10 109.0(4) . . ? O4 C8 C9 108.6(3) . . ? C10 C8 C9 112.8(4) . . ? O5 C11 C12 111.1(7) . . ? O5 C11 C13 105.9(6) . . ? C12 C11 C13 110.4(7) . . ? C13' C11' O5 111(3) . . ? C13' C11' C12' 124(2) . . ? O5 C11' C12' 101(2) . . ? O6 C14 C16 109.1(4) . . ? O6 C14 C15 110.6(4) . . ? C16 C14 C15 112.6(4) . . ? O7 C17 C19 122.7(7) . . ? O7 C17 C18 106.6(6) . . ? C19 C17 C18 112.8(7) . . ? O7 C17' C19 114.5(6) . . ? O7 C17' C18 106.0(6) . . ? C19 C17' C18 111.4(6) . . ? C17' C18 C17 29.9(4) . . ? C17 C19 C17' 33.5(4) . . ? C21 C20 O8 114.6(5) . . ? C21 C20 C22' 61.9(6) . . ? O8 C20 C22' 109.3(5) . . ? C21 C20 C22 122.4(6) . . ? O8 C20 C22 103.5(4) . . ? C22' C20 C22 140.3(6) . . ? C21 C20 C21' 41.9(5) . . ? O8 C20 C21' 106.6(4) . . ? C22' C20 C21' 103.5(5) . . ? C22 C20 C21' 87.6(5) . . ? N3 C23 C24 123.4(3) . . ? C23 C24 C25 119.2(3) . . ? C26 C25 C24 118.4(3) . . ? C25 C26 C27 119.4(4) . . ? N3 C27 C26 122.5(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.569 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.086 #===END data_tjb149s _database_code_CSD 218028 _chemical_name_common Ti4(DHP)2(u-OPri)4(OPri)8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H86 N4 O16 Ti4' _chemical_formula_weight 1118.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.361(3) _cell_length_b 9.3285(18) _cell_length_c 21.262(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.721(4) _cell_angle_gamma 90.00 _cell_volume 3107.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max .123 _exptl_crystal_size_mid .075 _exptl_crystal_size_min .033 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9351 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19025 _diffrn_reflns_av_R_equivalents 0.1168 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4489 _reflns_number_gt 2544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1794P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4489 _refine_ls_number_parameters 315 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1516 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2750 _refine_ls_wR_factor_gt 0.2241 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.423 _refine_ls_shift/su_mean 0.030 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.20673(8) 0.80247(15) 1.02730(7) 0.0317(5) Uani 1 1 d . . . Ti2 Ti 0.16510(9) 1.02978(16) 0.90804(7) 0.0333(5) Uani 1 1 d . . . N1 N 0.0845(4) 0.8591(7) 1.0488(3) 0.0305(15) Uani 1 1 d . . . N2 N 0.0426(4) 1.0840(6) 0.9285(3) 0.0299(15) Uani 1 1 d . . . O1 O 0.2206(3) 1.0046(5) 1.0088(2) 0.0312(13) Uani 1 1 d . . . O2 O 0.1473(3) 0.8293(5) 0.9272(2) 0.0299(12) Uani 1 1 d . . . O3 O 0.1175(3) 0.6436(5) 1.0222(3) 0.0365(14) Uani 1 1 d . . . O4 O 0.2536(3) 0.7936(6) 1.1139(2) 0.0405(14) Uani 1 1 d . . . O5 O 0.2882(3) 0.7046(6) 1.0053(3) 0.0417(14) Uani 1 1 d . . . O6 O 0.1454(3) 1.2378(5) 0.9316(2) 0.0357(13) Uani 1 1 d . . . O7 O 0.1089(3) 1.0445(6) 0.8227(2) 0.0428(14) Uani 1 1 d . . . O8 O 0.2709(3) 1.0521(6) 0.8999(3) 0.0433(15) Uani 1 1 d . . . C1 C 0.0330(5) 0.9524(9) 1.0659(3) 0.0303(19) Uani 1 1 d . . . C2 C 0.0587(5) 0.7188(8) 1.0365(4) 0.035(2) Uani 1 1 d . . . C3 C 0.0708(5) 1.2230(8) 0.9402(4) 0.0328(19) Uani 1 1 d . . . C4 C 0.0200(5) 1.3251(8) 0.9593(4) 0.0344(19) Uani 1 1 d . . . H4 H 0.0390 1.4210 0.9691 0.041 Uiso 1 1 calc R . . C5 C 0.2776(5) 1.1101(9) 1.0480(4) 0.041(2) Uani 1 1 d . . . H5 H 0.2781 1.1940 1.0188 0.049 Uiso 1 1 calc R . . C6 C 0.2426(6) 1.1627(9) 1.1027(4) 0.049(2) Uani 1 1 d . . . H6A H 0.1904 1.2182 1.0838 0.074 Uiso 1 1 calc R . . H6B H 0.2852 1.2236 1.1328 0.074 Uiso 1 1 calc R . . H6C H 0.2296 1.0803 1.1268 0.074 Uiso 1 1 calc R . . C7 C 0.3673(5) 1.0537(10) 1.0708(5) 0.058(3) Uani 1 1 d . . . H7A H 0.3708 0.9788 1.1038 0.087 Uiso 1 1 calc R . . H7B H 0.4064 1.1319 1.0902 0.087 Uiso 1 1 calc R . . H7C H 0.3831 1.0134 1.0334 0.087 Uiso 1 1 calc R . . C8 C 0.1278(6) 0.7015(10) 0.8855(4) 0.047(2) Uani 1 1 d . . . H8 H 0.1438 0.6144 0.9138 0.057 Uiso 1 1 calc R . . C9 C 0.0326(6) 0.6986(10) 0.8521(5) 0.066(3) Uani 1 1 d . . . H9A H 0.0020 0.6923 0.8854 0.098 Uiso 1 1 calc R . . H9B H 0.0186 0.6153 0.8229 0.098 Uiso 1 1 calc R . . H9C H 0.0158 0.7865 0.8264 0.098 Uiso 1 1 calc R . . C10 C 0.1816(8) 0.7060(11) 0.8373(5) 0.079(3) Uani 1 1 d . . . H10A H 0.1596 0.7809 0.8045 0.118 Uiso 1 1 calc R . . H10B H 0.1784 0.6130 0.8153 0.118 Uiso 1 1 calc R . . H10C H 0.2411 0.7270 0.8613 0.118 Uiso 1 1 calc R . . C11 C 0.2515(8) 0.7718(14) 1.1798(5) 0.079(4) Uani 1 1 d . . . H11 H 0.2077 0.8381 1.1882 0.095 Uiso 1 1 calc R . . C12 C 0.3379(7) 0.8139(15) 1.2257(5) 0.094(4) Uani 1 1 d . . . H12A H 0.3816 0.7480 1.2196 0.140 Uiso 1 1 calc R . . H12B H 0.3359 0.8091 1.2712 0.140 Uiso 1 1 calc R . . H12C H 0.3518 0.9119 1.2157 0.140 Uiso 1 1 calc R . . C13 C 0.2267(14) 0.629(2) 1.1890(7) 0.235(14) Uani 1 1 d . . . H13A H 0.1785 0.6007 1.1517 0.353 Uiso 1 1 calc R . . H13B H 0.2099 0.6232 1.2296 0.353 Uiso 1 1 calc R . . H13C H 0.2748 0.5638 1.1921 0.353 Uiso 1 1 calc R . . C14 C 0.3653(7) 0.6265(11) 1.0309(6) 0.076(3) Uani 1 1 d . . . H14 H 0.3893 0.6562 1.0778 0.091 Uiso 1 1 calc R . . C15 C 0.3427(9) 0.4749(13) 1.0313(8) 0.130(6) Uani 1 1 d . . . H15A H 0.2995 0.4629 1.0546 0.196 Uiso 1 1 calc R . . H15B H 0.3937 0.4193 1.0535 0.196 Uiso 1 1 calc R . . H15C H 0.3199 0.4408 0.9860 0.196 Uiso 1 1 calc R . . C16 C 0.4263(9) 0.6698(16) 0.9971(11) 0.186(9) Uani 1 1 d . . . H16A H 0.4063 0.6389 0.9512 0.279 Uiso 1 1 calc R . . H16B H 0.4817 0.6254 1.0183 0.279 Uiso 1 1 calc R . . H16C H 0.4323 0.7743 0.9990 0.279 Uiso 1 1 calc R . . C17 C 0.0370(12) 1.1007(14) 0.7674(5) 0.134(7) Uani 1 1 d D . . C18 C 0.0343(16) 1.000(2) 0.7097(10) 0.080(7) Uiso 0.50 1 d PD . . C18' C 0.0831(19) 1.092(4) 0.7108(13) 0.118(10) Uiso 0.50 1 d PD . . C19 C 0.0640(19) 1.263(2) 0.7690(13) 0.094(9) Uiso 0.50 1 d PD . . C19' C 0.019(2) 1.260(2) 0.7734(14) 0.099(9) Uiso 0.50 1 d PD . . C20 C 0.3097(7) 1.0994(13) 0.8518(6) 0.074(3) Uani 1 1 d . . . H20 H 0.2710 1.0692 0.8082 0.089 Uiso 1 1 calc R . . C21 C 0.3125(11) 1.2560(17) 0.8511(7) 0.137(6) Uani 1 1 d . . . H21A H 0.2547 1.2942 0.8440 0.206 Uiso 1 1 calc R . . H21B H 0.3351 1.2881 0.8155 0.206 Uiso 1 1 calc R . . H21C H 0.3494 1.2907 0.8932 0.206 Uiso 1 1 calc R . . C22 C 0.3898(10) 1.021(2) 0.8609(8) 0.157(8) Uani 1 1 d . . . H22A H 0.4320 1.0550 0.9008 0.235 Uiso 1 1 calc R . . H22B H 0.4111 1.0365 0.8229 0.235 Uiso 1 1 calc R . . H22C H 0.3797 0.9181 0.8653 0.235 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0268(8) 0.0321(9) 0.0357(9) -0.0037(7) 0.0081(6) 0.0035(6) Ti2 0.0302(9) 0.0387(9) 0.0325(9) -0.0016(7) 0.0116(6) 0.0024(7) N1 0.027(4) 0.030(4) 0.032(4) 0.000(3) 0.005(3) 0.001(3) N2 0.028(4) 0.030(4) 0.033(4) 0.001(3) 0.010(3) -0.001(3) O1 0.028(3) 0.033(3) 0.032(3) -0.006(2) 0.008(2) -0.003(2) O2 0.029(3) 0.028(3) 0.030(3) -0.006(2) 0.004(2) 0.003(2) O3 0.032(3) 0.026(3) 0.053(4) -0.005(3) 0.014(3) 0.004(2) O4 0.035(3) 0.044(4) 0.039(3) 0.001(3) 0.005(3) 0.007(3) O5 0.026(3) 0.044(4) 0.054(4) -0.007(3) 0.010(3) 0.006(3) O6 0.027(3) 0.035(3) 0.049(3) 0.001(3) 0.017(3) -0.005(2) O7 0.042(3) 0.055(4) 0.032(3) 0.001(3) 0.013(3) 0.005(3) O8 0.037(3) 0.053(4) 0.045(3) -0.002(3) 0.019(3) -0.002(3) C1 0.026(4) 0.045(5) 0.017(4) 0.003(3) 0.002(3) -0.001(4) C2 0.042(5) 0.031(5) 0.029(4) 0.005(4) 0.007(4) 0.009(4) C3 0.036(5) 0.034(5) 0.027(4) 0.002(4) 0.007(4) 0.001(4) C4 0.035(5) 0.027(5) 0.038(5) -0.007(4) 0.005(4) -0.005(4) C5 0.042(5) 0.034(5) 0.043(5) -0.007(4) 0.007(4) -0.012(4) C6 0.064(6) 0.039(5) 0.045(5) -0.017(4) 0.016(5) -0.005(4) C7 0.034(5) 0.056(6) 0.073(7) -0.014(5) -0.002(5) -0.010(5) C8 0.053(6) 0.044(6) 0.041(5) -0.010(4) 0.010(4) 0.002(4) C9 0.057(7) 0.053(6) 0.071(7) -0.022(5) -0.008(5) 0.003(5) C10 0.122(10) 0.066(7) 0.063(7) -0.025(6) 0.051(7) -0.001(7) C11 0.080(8) 0.108(10) 0.034(6) 0.011(6) -0.008(5) -0.013(7) C12 0.076(8) 0.144(12) 0.043(6) 0.014(7) -0.011(6) 0.009(8) C13 0.29(3) 0.28(2) 0.068(10) 0.089(13) -0.065(12) -0.20(2) C14 0.069(8) 0.051(7) 0.117(10) 0.018(6) 0.041(7) 0.035(6) C15 0.080(9) 0.054(8) 0.246(19) 0.029(10) 0.027(11) 0.020(7) C16 0.087(11) 0.093(12) 0.42(3) 0.006(15) 0.137(16) 0.024(9) C17 0.260(19) 0.105(11) 0.019(6) 0.011(6) 0.011(8) 0.064(12) C20 0.061(7) 0.095(9) 0.086(8) -0.002(7) 0.052(6) -0.023(6) C21 0.194(17) 0.113(13) 0.148(14) 0.016(10) 0.119(13) -0.035(12) C22 0.109(13) 0.21(2) 0.191(18) 0.046(14) 0.115(13) 0.036(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.782(5) . ? Ti1 O5 1.785(5) . ? Ti1 O1 1.952(5) . ? Ti1 O3 2.061(5) . ? Ti1 O2 2.084(5) . ? Ti1 N1 2.240(6) . ? Ti1 C2 2.606(8) . ? Ti1 Ti2 3.224(2) . ? Ti2 O7 1.788(5) . ? Ti2 O8 1.802(5) . ? Ti2 O2 1.954(5) . ? Ti2 O6 2.053(5) . ? Ti2 O1 2.086(5) . ? Ti2 N2 2.228(6) . ? Ti2 C3 2.589(8) . ? N1 C1 1.332(9) . ? N1 C2 1.377(10) . ? N2 C1 1.321(9) 3_577 ? N2 C3 1.375(9) . ? O1 C5 1.445(9) . ? O2 C8 1.466(9) . ? O3 C2 1.296(9) . ? O4 C11 1.425(11) . ? O5 C14 1.423(11) . ? O6 C3 1.292(9) . ? O7 C17 1.498(14) . ? O8 C20 1.419(10) . ? C1 N2 1.321(9) 3_577 ? C2 C4 1.378(11) 3_577 ? C3 C4 1.399(10) . ? C4 C2 1.378(11) 3_577 ? C5 C7 1.502(11) . ? C5 C6 1.518(11) . ? C8 C9 1.514(12) . ? C8 C10 1.532(12) . ? C11 C13 1.425(19) . ? C11 C12 1.519(14) . ? C14 C15 1.463(15) . ? C14 C16 1.444(18) . ? C17 C18 1.533(16) . ? C17 C19' 1.533(18) . ? C17 C19 1.578(17) . ? C17 C18' 1.594(18) . ? C20 C21 1.462(17) . ? C20 C22 1.465(17) . ? 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 O4 Ti1 O5 96.6(2) . . ? O4 Ti1 O1 102.3(2) . . ? O5 Ti1 O1 107.6(2) . . ? O4 Ti1 O3 96.2(2) . . ? O5 Ti1 O3 100.9(2) . . ? O1 Ti1 O3 143.6(2) . . ? O4 Ti1 O2 175.1(2) . . ? O5 Ti1 O2 87.6(2) . . ? O1 Ti1 O2 74.08(19) . . ? O3 Ti1 O2 85.3(2) . . ? O4 Ti1 N1 86.8(2) . . ? O5 Ti1 N1 162.2(2) . . ? O1 Ti1 N1 88.6(2) . . ? O3 Ti1 N1 61.3(2) . . ? O2 Ti1 N1 89.9(2) . . ? O4 Ti1 C2 92.3(2) . . ? O5 Ti1 C2 130.3(2) . . ? O1 Ti1 C2 117.9(2) . . ? O3 Ti1 C2 29.4(2) . . ? O2 Ti1 C2 86.7(2) . . ? N1 Ti1 C2 31.9(2) . . ? O4 Ti1 Ti2 140.72(19) . . ? O5 Ti1 Ti2 97.76(19) . . ? O1 Ti1 Ti2 38.47(14) . . ? O3 Ti1 Ti2 116.46(15) . . ? O2 Ti1 Ti2 35.64(14) . . ? N1 Ti1 Ti2 90.39(16) . . ? C2 Ti1 Ti2 105.41(16) . . ? O7 Ti2 O8 97.0(2) . . ? O7 Ti2 O2 102.8(2) . . ? O8 Ti2 O2 109.7(2) . . ? O7 Ti2 O6 96.0(2) . . ? O8 Ti2 O6 97.9(2) . . ? O2 Ti2 O6 144.1(2) . . ? O7 Ti2 O1 174.8(2) . . ? O8 Ti2 O1 88.0(2) . . ? O2 Ti2 O1 74.01(19) . . ? O6 Ti2 O1 84.7(2) . . ? O7 Ti2 N2 87.2(2) . . ? O8 Ti2 N2 159.4(3) . . ? O2 Ti2 N2 88.8(2) . . ? O6 Ti2 N2 61.6(2) . . ? O1 Ti2 N2 88.6(2) . . ? O7 Ti2 C3 92.5(2) . . ? O8 Ti2 C3 127.4(3) . . ? O2 Ti2 C3 118.4(2) . . ? O6 Ti2 C3 29.5(2) . . ? O1 Ti2 C3 85.6(2) . . ? N2 Ti2 C3 32.1(2) . . ? O7 Ti2 Ti1 141.19(19) . . ? O8 Ti2 Ti1 99.23(19) . . ? O2 Ti2 Ti1 38.44(14) . . ? O6 Ti2 Ti1 116.26(15) . . ? O1 Ti2 Ti1 35.61(14) . . ? N2 Ti2 Ti1 89.67(16) . . ? C3 Ti2 Ti1 104.91(17) . . ? C1 N1 C2 119.3(7) . . ? C1 N1 Ti1 151.8(5) . . ? C2 N1 Ti1 88.9(5) . . ? C1 N2 C3 120.0(7) 3_577 . ? C1 N2 Ti2 151.4(5) 3_577 . ? C3 N2 Ti2 88.6(4) . . ? C5 O1 Ti1 129.5(5) . . ? C5 O1 Ti2 122.2(5) . . ? Ti1 O1 Ti2 105.9(2) . . ? C8 O2 Ti2 132.2(5) . . ? C8 O2 Ti1 118.5(5) . . ? Ti2 O2 Ti1 105.9(2) . . ? C2 O3 Ti1 99.3(5) . . ? C11 O4 Ti1 153.9(6) . . ? C14 O5 Ti1 144.0(6) . . ? C3 O6 Ti2 98.9(4) . . ? C17 O7 Ti2 151.8(6) . . ? C20 O8 Ti2 138.3(6) . . ? N2 C1 N1 122.6(7) 3_577 . ? O3 C2 N1 110.5(7) . . ? O3 C2 C4 128.7(7) . 3_577 ? N1 C2 C4 120.8(7) . 3_577 ? O3 C2 Ti1 51.3(4) . . ? N1 C2 Ti1 59.3(4) . . ? C4 C2 Ti1 179.3(6) 3_577 . ? O6 C3 N2 110.9(7) . . ? O6 C3 C4 129.3(7) . . ? N2 C3 C4 119.8(7) . . ? O6 C3 Ti2 51.6(4) . . ? N2 C3 Ti2 59.3(4) . . ? C4 C3 Ti2 178.3(6) . . ? C2 C4 C3 117.4(7) 3_577 . ? O1 C5 C7 110.9(7) . . ? O1 C5 C6 109.8(6) . . ? C7 C5 C6 114.5(7) . . ? O2 C8 C9 108.3(7) . . ? O2 C8 C10 108.4(7) . . ? C9 C8 C10 113.4(9) . . ? O4 C11 C13 110.9(11) . . ? O4 C11 C12 108.2(9) . . ? C13 C11 C12 113.7(11) . . ? O5 C14 C15 107.5(9) . . ? O5 C14 C16 109.3(10) . . ? C15 C14 C16 119.0(11) . . ? O7 C17 C18 104.5(12) . . ? O7 C17 C19' 113.7(14) . . ? C18 C17 C19' 134.4(16) . . ? O7 C17 C19 99.7(15) . . ? C18 C17 C19 123.2(17) . . ? C19' C17 C19 28.8(14) . . ? O7 C17 C18' 98.1(16) . . ? C18 C17 C18' 43.8(13) . . ? C19' C17 C18' 105(2) . . ? C19 C17 C18' 82.7(19) . . ? O8 C20 C21 109.9(9) . . ? O8 C20 C22 108.4(10) . . ? C21 C20 C22 118.2(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.126 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.125 #===END data_tjb219p _database_code_CSD 218029 _chemical_name_common Ti4(u-DHP)2(u-OPri)4(OPri)8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H88 N4 O16 Ti4' _chemical_formula_weight 1120.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.732(5) _cell_length_b 15.003(6) _cell_length_c 17.776(7) _cell_angle_alpha 96.204(6) _cell_angle_beta 98.401(6) _cell_angle_gamma 103.870(6) _cell_volume 2972(2) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.556 _exptl_crystal_size_mid 0.460 _exptl_crystal_size_min 0.456 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7391 _exptl_absorpt_correction_T_max 0.7783 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24842 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.18 _reflns_number_total 12945 _reflns_number_gt 10049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+2.5172P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12945 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.124 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.28046(4) 0.81113(3) 1.06728(3) 0.03128(13) Uani 1 1 d . . . Ti2 Ti 0.40835(5) 0.74209(3) 0.93174(3) 0.03161(13) Uani 1 1 d . . . Ti3 Ti 0.73515(4) 0.78851(3) 0.43910(3) 0.03001(13) Uani 1 1 d . . . Ti4 Ti 0.94660(4) 0.76966(3) 0.56944(3) 0.02964(13) Uani 1 1 d . . . N1 N 0.5129(2) 0.88828(16) 0.93237(13) 0.0313(5) Uani 1 1 d . . . N2 N 0.3795(2) 0.95883(16) 1.06711(13) 0.0310(5) Uani 1 1 d . . . N3 N 1.05126(19) 0.91494(15) 0.56679(13) 0.0279(5) Uani 1 1 d . . . N4 N 0.83604(19) 0.93478(15) 0.43551(13) 0.0284(5) Uani 1 1 d . . . O1 O 0.38850(19) 0.80077(14) 0.83250(11) 0.0384(5) Uani 1 1 d . . . O2 O 0.39112(19) 0.88425(13) 1.16662(11) 0.0372(5) Uani 1 1 d . . . O3 O 0.26346(17) 0.79185(13) 0.95562(11) 0.0317(4) Uani 1 1 d . . . O4 O 0.43107(17) 0.76869(13) 1.04318(11) 0.0318(4) Uani 1 1 d . . . O5 O 0.23125(19) 0.70079(14) 1.09831(12) 0.0408(5) Uani 1 1 d . . . O6 O 0.30452(19) 0.63012(13) 0.89854(12) 0.0394(5) Uani 1 1 d . . . O7 O 0.15406(19) 0.85324(15) 1.08055(13) 0.0422(5) Uani 1 1 d . . . O8 O 0.53943(19) 0.70798(14) 0.91681(12) 0.0406(5) Uani 1 1 d . . . O9 O 0.99174(18) 0.86485(13) 0.66983(11) 0.0346(4) Uani 1 1 d . . . O10 O 0.77990(18) 0.82401(13) 0.33585(11) 0.0357(5) Uani 1 1 d . . . O11 O 0.78794(16) 0.81035(13) 0.55047(11) 0.0298(4) Uani 1 1 d . . . O12 O 0.89906(16) 0.75492(12) 0.45816(11) 0.0304(4) Uani 1 1 d . . . O13 O 0.66816(18) 0.66669(13) 0.40693(13) 0.0393(5) Uani 1 1 d . . . O14 O 0.60180(17) 0.82507(14) 0.43196(12) 0.0384(5) Uani 1 1 d . . . O15 O 0.86388(17) 0.66932(13) 0.60394(12) 0.0368(5) Uani 1 1 d . . . O16 O 1.08406(17) 0.73829(14) 0.57822(13) 0.0388(5) Uani 1 1 d . . . C1 C 0.5906(2) 0.96682(19) 0.96637(16) 0.0294(6) Uani 1 1 d . . . H1 H 0.6272 0.9697 1.0182 0.035 Uiso 1 1 calc R . . C2 C 0.4305(3) 0.9622(2) 1.14166(16) 0.0327(6) Uani 1 1 d . . . C3 C 0.4858(3) 0.9580(2) 0.81785(16) 0.0369(7) Uani 1 1 d . . . H3 H 0.4485 0.9553 0.7662 0.044 Uiso 1 1 calc R . . C4 C 0.4605(3) 0.8827(2) 0.85783(16) 0.0332(6) Uani 1 1 d . . . C5 C 0.1591(3) 0.7785(2) 0.89728(18) 0.0411(7) Uani 1 1 d . . . H5 H 0.1758 0.7495 0.8481 0.049 Uiso 1 1 calc R . . C6 C 0.0535(3) 0.7117(3) 0.9184(2) 0.0608(10) Uani 1 1 d . . . H6A H 0.0735 0.6531 0.9258 0.091 Uiso 1 1 calc R . . H6B H -0.0156 0.7000 0.8770 0.091 Uiso 1 1 calc R . . H6C H 0.0344 0.7389 0.9661 0.091 Uiso 1 1 calc R . . C7 C 0.1384(4) 0.8721(3) 0.8850(2) 0.0586(10) Uani 1 1 d . . . H7A H 0.1199 0.9015 0.9320 0.088 Uiso 1 1 calc R . . H7B H 0.0715 0.8637 0.8425 0.088 Uiso 1 1 calc R . . H7C H 0.2104 0.9117 0.8724 0.088 Uiso 1 1 calc R . . C8 C 0.5030(3) 0.7364(2) 1.10206(18) 0.0402(7) Uani 1 1 d . . . H8 H 0.4724 0.7460 1.1511 0.048 Uiso 1 1 calc R . . C9 C 0.6315(3) 0.7950(3) 1.1143(2) 0.0587(10) Uani 1 1 d . . . H9A H 0.6638 0.7863 1.0670 0.088 Uiso 1 1 calc R . . H9B H 0.6796 0.7758 1.1563 0.088 Uiso 1 1 calc R . . H9C H 0.6338 0.8606 1.1274 0.088 Uiso 1 1 calc R . . C10 C 0.4886(3) 0.6330(2) 1.0807(2) 0.0539(9) Uani 1 1 d . . . H10A H 0.4036 0.6005 1.0697 0.081 Uiso 1 1 calc R . . H10B H 0.5288 0.6096 1.1237 0.081 Uiso 1 1 calc R . . H10C H 0.5241 0.6222 1.0351 0.081 Uiso 1 1 calc R . . C11 C 0.1367(3) 0.6476(2) 1.1280(2) 0.0570(10) Uani 1 1 d . . . H11 H 0.0616 0.6645 1.1081 0.068 Uiso 1 1 calc R . . C12 C 0.1212(5) 0.5472(3) 1.1018(3) 0.0887(16) Uani 1 1 d . . . H12A H 0.1062 0.5353 1.0454 0.133 Uiso 1 1 calc R . . H12B H 0.0533 0.5106 1.1209 0.133 Uiso 1 1 calc R . . H12C H 0.1937 0.5296 1.1217 0.133 Uiso 1 1 calc R . . C13 C 0.1614(8) 0.6691(4) 1.2124(3) 0.163(4) Uani 1 1 d . . . H13A H 0.2467 0.6780 1.2312 0.244 Uiso 1 1 calc R . . H13B H 0.1154 0.6176 1.2340 0.244 Uiso 1 1 calc R . . H13C H 0.1385 0.7260 1.2283 0.244 Uiso 1 1 calc R . . C14 C 0.3031(3) 0.5439(2) 0.8559(2) 0.0498(9) Uani 1 1 d . . . H14 H 0.3871 0.5393 0.8579 0.060 Uiso 1 1 calc R . . C15 C 0.2485(5) 0.5413(4) 0.7750(3) 0.103(2) Uani 1 1 d . . . H15A H 0.1656 0.5443 0.7724 0.155 Uiso 1 1 calc R . . H15B H 0.2506 0.4834 0.7445 0.155 Uiso 1 1 calc R . . H15C H 0.2932 0.5943 0.7545 0.155 Uiso 1 1 calc R . . C16 C 0.2368(5) 0.4672(3) 0.8931(4) 0.0934(17) Uani 1 1 d . . . H16A H 0.2735 0.4750 0.9474 0.140 Uiso 1 1 calc R . . H16B H 0.2403 0.4072 0.8670 0.140 Uiso 1 1 calc R . . H16C H 0.1534 0.4694 0.8892 0.140 Uiso 1 1 calc R . . C17 C 0.0931(4) 0.9210(3) 1.0993(3) 0.0663(11) Uani 1 1 d . . . H17 H 0.1119 0.9692 1.0651 0.080 Uiso 1 1 calc R . . C18 C -0.0375(4) 0.8807(4) 1.0817(4) 0.125(3) Uani 1 1 d . . . H18A H -0.0619 0.8556 1.0269 0.187 Uiso 1 1 calc R . . H18B H -0.0779 0.9291 1.0941 0.187 Uiso 1 1 calc R . . H18C H -0.0594 0.8308 1.1123 0.187 Uiso 1 1 calc R . . C19 C 0.1362(5) 0.9682(4) 1.1788(3) 0.113(2) Uani 1 1 d . . . H19A H 0.1176 0.9234 1.2144 0.169 Uiso 1 1 calc R . . H19B H 0.0970 1.0180 1.1883 0.169 Uiso 1 1 calc R . . H19C H 0.2227 0.9945 1.1866 0.169 Uiso 1 1 calc R . . C20 C 0.6520(4) 0.7170(3) 0.8954(3) 0.0711(12) Uani 1 1 d . . . H20 H 0.7074 0.7710 0.9314 0.085 Uiso 1 1 calc R . . C21 C 0.6967(6) 0.6404(5) 0.9077(6) 0.197(5) Uani 1 1 d . . . H21A H 0.6840 0.6233 0.9581 0.296 Uiso 1 1 calc R . . H21B H 0.7823 0.6562 0.9062 0.296 Uiso 1 1 calc R . . H21C H 0.6552 0.5880 0.8675 0.296 Uiso 1 1 calc R . . C22 C 0.6549(10) 0.7403(9) 0.8217(6) 0.291(9) Uani 1 1 d . . . H22A H 0.6266 0.6837 0.7838 0.437 Uiso 1 1 calc R . . H22B H 0.7369 0.7716 0.8179 0.437 Uiso 1 1 calc R . . H22C H 0.6032 0.7818 0.8117 0.437 Uiso 1 1 calc R . . C23 C 1.1093(2) 0.97967(17) 0.53126(15) 0.0262(5) Uani 1 1 d . . . H23 H 1.1117 0.9635 0.4785 0.031 Uiso 1 1 calc R . . C24 C 0.8371(2) 0.91049(19) 0.35946(16) 0.0298(6) Uani 1 1 d . . . C25 C 0.8945(2) 0.97465(19) 0.31682(16) 0.0318(6) Uani 1 1 d . . . H25 H 0.8954 0.9588 0.2637 0.038 Uiso 1 1 calc R . . C26 C 1.0494(2) 0.93643(18) 0.64330(16) 0.0291(6) Uani 1 1 d . . . C27 C 0.7225(3) 0.8210(2) 0.61273(18) 0.0396(7) Uani 1 1 d . . . H27 H 0.7717 0.8130 0.6612 0.047 Uiso 1 1 calc R . . C28 C 0.7061(3) 0.9184(3) 0.6225(2) 0.0540(9) Uani 1 1 d . . . H28A H 0.7844 0.9635 0.6350 0.081 Uiso 1 1 calc R . . H28B H 0.6616 0.9258 0.6643 0.081 Uiso 1 1 calc R . . H28C H 0.6617 0.9290 0.5747 0.081 Uiso 1 1 calc R . . C29 C 0.6058(3) 0.7450(3) 0.5976(2) 0.0587(10) Uani 1 1 d . . . H29A H 0.5529 0.7548 0.5529 0.088 Uiso 1 1 calc R . . H29B H 0.5671 0.7471 0.6427 0.088 Uiso 1 1 calc R . . H29C H 0.6223 0.6843 0.5872 0.088 Uiso 1 1 calc R . . C30 C 0.9383(3) 0.7039(2) 0.39741(19) 0.0427(7) Uani 1 1 d . . . H30 H 0.8807 0.6982 0.3486 0.051 Uiso 1 1 calc R . . C31 C 0.9363(3) 0.6066(2) 0.4147(2) 0.0560(10) Uani 1 1 d . . . H31A H 0.9946 0.6104 0.4611 0.084 Uiso 1 1 calc R . . H31B H 0.9566 0.5712 0.3712 0.084 Uiso 1 1 calc R . . H31C H 0.8564 0.5756 0.4227 0.084 Uiso 1 1 calc R . . C32 C 1.0596(3) 0.7601(3) 0.3870(2) 0.0628(11) Uani 1 1 d . . . H32A H 1.0520 0.8184 0.3694 0.094 Uiso 1 1 calc R . . H32B H 1.0900 0.7244 0.3487 0.094 Uiso 1 1 calc R . . H32C H 1.1151 0.7736 0.4361 0.094 Uiso 1 1 calc R . . C33 C 0.5525(3) 0.6070(2) 0.37698(19) 0.0409(7) Uani 1 1 d . . . H33 H 0.4927 0.6288 0.4038 0.049 Uiso 1 1 calc R . . C34 C 0.5546(3) 0.5107(2) 0.3942(3) 0.0632(11) Uani 1 1 d . . . H34A H 0.6124 0.4887 0.3675 0.095 Uiso 1 1 calc R . . H34B H 0.4751 0.4683 0.3764 0.095 Uiso 1 1 calc R . . H34C H 0.5776 0.5128 0.4497 0.095 Uiso 1 1 calc R . . C35 C 0.5222(4) 0.6103(3) 0.2930(2) 0.0702(12) Uani 1 1 d . . . H35A H 0.5208 0.6737 0.2851 0.105 Uiso 1 1 calc R . . H35B H 0.4435 0.5680 0.2721 0.105 Uiso 1 1 calc R . . H35C H 0.5823 0.5913 0.2667 0.105 Uiso 1 1 calc R . . C36 C 0.5194(4) 0.8784(3) 0.4171(3) 0.0758(13) Uani 1 1 d . . . H36 H 0.5359 0.9250 0.4647 0.091 Uiso 1 1 calc R . . C37 C 0.3995(5) 0.8256(6) 0.4138(7) 0.224(6) Uani 1 1 d . . . H37A H 0.3636 0.7989 0.3604 0.336 Uiso 1 1 calc R . . H37B H 0.3531 0.8662 0.4338 0.336 Uiso 1 1 calc R . . H37C H 0.3993 0.7756 0.4450 0.336 Uiso 1 1 calc R . . C38 C 0.5367(6) 0.9300(7) 0.3606(5) 0.191(5) Uani 1 1 d . . . H38A H 0.6194 0.9679 0.3704 0.287 Uiso 1 1 calc R . . H38B H 0.4825 0.9705 0.3588 0.287 Uiso 1 1 calc R . . H38C H 0.5208 0.8891 0.3113 0.287 Uiso 1 1 calc R . . C39 C 0.8924(3) 0.5926(2) 0.6350(2) 0.0432(8) Uani 1 1 d . . . H39 H 0.9623 0.5801 0.6138 0.052 Uiso 1 1 calc R . . C40 C 0.7906(4) 0.5092(3) 0.6101(3) 0.0804(14) Uani 1 1 d . . . H40A H 0.7215 0.5192 0.6315 0.121 Uiso 1 1 calc R . . H40B H 0.8126 0.4553 0.6285 0.121 Uiso 1 1 calc R . . H40C H 0.7704 0.4980 0.5538 0.121 Uiso 1 1 calc R . . C41 C 0.9283(5) 0.6174(4) 0.7198(3) 0.0920(16) Uani 1 1 d . . . H41A H 0.9939 0.6742 0.7321 0.138 Uiso 1 1 calc R . . H41B H 0.9546 0.5667 0.7412 0.138 Uiso 1 1 calc R . . H41C H 0.8602 0.6279 0.7421 0.138 Uiso 1 1 calc R . . C42 C 1.2054(4) 0.7454(3) 0.6018(5) 0.123(3) Uani 1 1 d . . . H42 H 1.2239 0.7720 0.5544 0.148 Uiso 1 1 calc R . . C43 C 1.2384(4) 0.6620(4) 0.5748(5) 0.127(3) Uani 1 1 d . . . H43A H 1.3210 0.6668 0.5983 0.191 Uiso 1 1 calc R . . H43B H 1.2313 0.6549 0.5187 0.191 Uiso 1 1 calc R . . H43C H 1.1853 0.6079 0.5891 0.191 Uiso 1 1 calc R . . C44 C 1.2750(6) 0.8143(6) 0.6424(6) 0.243(7) Uani 1 1 d . . . H44A H 1.3286 0.8478 0.6114 0.364 Uiso 1 1 calc R . . H44B H 1.3220 0.7948 0.6847 0.364 Uiso 1 1 calc R . . H44C H 1.2298 0.8552 0.6633 0.364 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0313(3) 0.0275(3) 0.0322(3) 0.0054(2) 0.0079(2) 0.0004(2) Ti2 0.0358(3) 0.0251(3) 0.0319(3) 0.0044(2) 0.0068(2) 0.0034(2) Ti3 0.0255(3) 0.0233(2) 0.0392(3) 0.0068(2) 0.0062(2) 0.00123(19) Ti4 0.0273(3) 0.0232(2) 0.0404(3) 0.0112(2) 0.0092(2) 0.0055(2) N1 0.0345(13) 0.0298(12) 0.0281(12) 0.0049(9) 0.0076(10) 0.0042(10) N2 0.0309(12) 0.0315(12) 0.0275(12) 0.0033(9) 0.0064(9) 0.0022(10) N3 0.0275(11) 0.0244(11) 0.0318(12) 0.0076(9) 0.0049(9) 0.0058(9) N4 0.0263(11) 0.0250(11) 0.0328(12) 0.0077(9) 0.0056(9) 0.0029(9) O1 0.0466(12) 0.0293(11) 0.0315(11) 0.0021(8) 0.0040(9) -0.0021(9) O2 0.0455(12) 0.0310(11) 0.0304(10) 0.0083(8) 0.0065(9) -0.0006(9) O3 0.0303(10) 0.0297(10) 0.0320(10) 0.0032(8) 0.0022(8) 0.0048(8) O4 0.0326(10) 0.0322(10) 0.0300(10) 0.0090(8) 0.0043(8) 0.0062(8) O5 0.0413(12) 0.0339(11) 0.0455(12) 0.0109(9) 0.0158(10) -0.0005(9) O6 0.0412(12) 0.0269(10) 0.0469(12) 0.0005(9) 0.0080(10) 0.0050(9) O7 0.0355(11) 0.0410(12) 0.0481(13) 0.0025(10) 0.0121(10) 0.0053(9) O8 0.0437(12) 0.0360(11) 0.0446(12) 0.0078(9) 0.0149(10) 0.0105(10) O9 0.0374(11) 0.0304(10) 0.0364(11) 0.0126(8) 0.0094(9) 0.0046(9) O10 0.0373(11) 0.0272(10) 0.0364(11) 0.0022(8) 0.0041(9) -0.0010(8) O11 0.0267(10) 0.0279(10) 0.0379(11) 0.0102(8) 0.0116(8) 0.0071(8) O12 0.0280(10) 0.0250(10) 0.0384(11) 0.0033(8) 0.0094(8) 0.0060(8) O13 0.0321(11) 0.0258(10) 0.0540(13) 0.0060(9) 0.0052(9) -0.0027(8) O14 0.0275(10) 0.0382(12) 0.0512(13) 0.0145(10) 0.0077(9) 0.0077(9) O15 0.0339(11) 0.0272(10) 0.0532(13) 0.0179(9) 0.0121(9) 0.0078(8) O16 0.0300(11) 0.0300(11) 0.0585(14) 0.0122(9) 0.0091(9) 0.0082(9) C1 0.0299(14) 0.0315(14) 0.0265(13) 0.0053(11) 0.0051(11) 0.0071(11) C2 0.0368(15) 0.0331(15) 0.0280(14) 0.0066(11) 0.0091(12) 0.0056(12) C3 0.0453(17) 0.0355(16) 0.0239(14) 0.0054(11) 0.0017(12) 0.0014(13) C4 0.0374(16) 0.0307(15) 0.0290(14) 0.0019(11) 0.0069(12) 0.0050(12) C5 0.0354(16) 0.0442(18) 0.0371(16) -0.0004(13) -0.0038(13) 0.0068(14) C6 0.0382(19) 0.070(3) 0.057(2) -0.0072(19) -0.0028(16) -0.0044(18) C7 0.060(2) 0.062(2) 0.053(2) 0.0108(18) -0.0073(18) 0.0241(19) C8 0.0426(17) 0.0449(18) 0.0358(16) 0.0178(14) 0.0059(13) 0.0120(14) C9 0.042(2) 0.072(3) 0.057(2) 0.0207(19) -0.0051(17) 0.0094(18) C10 0.062(2) 0.053(2) 0.058(2) 0.0248(17) 0.0152(18) 0.0271(18) C11 0.054(2) 0.046(2) 0.079(3) 0.0275(19) 0.035(2) 0.0071(17) C12 0.101(4) 0.043(2) 0.111(4) 0.010(2) 0.039(3) -0.016(2) C13 0.283(10) 0.096(4) 0.080(4) -0.004(3) 0.104(5) -0.043(5) C14 0.0395(18) 0.0323(17) 0.071(2) -0.0108(16) 0.0038(16) 0.0079(14) C15 0.125(5) 0.104(4) 0.070(3) -0.044(3) -0.017(3) 0.053(4) C16 0.081(3) 0.032(2) 0.161(5) 0.007(3) 0.032(3) -0.001(2) C17 0.066(3) 0.058(2) 0.081(3) 0.003(2) 0.025(2) 0.025(2) C18 0.050(3) 0.125(5) 0.180(7) -0.059(5) 0.006(3) 0.033(3) C19 0.072(3) 0.132(5) 0.121(5) -0.052(4) 0.027(3) 0.025(3) C20 0.058(2) 0.073(3) 0.086(3) 0.010(2) 0.042(2) 0.007(2) C21 0.140(6) 0.175(7) 0.394(14) 0.184(9) 0.193(8) 0.117(6) C22 0.348(14) 0.430(17) 0.355(15) 0.314(14) 0.318(13) 0.331(14) C23 0.0244(13) 0.0258(13) 0.0296(13) 0.0074(10) 0.0056(10) 0.0071(10) C24 0.0270(13) 0.0287(14) 0.0324(14) 0.0052(11) 0.0028(11) 0.0059(11) C25 0.0341(15) 0.0325(15) 0.0279(14) 0.0050(11) 0.0071(11) 0.0057(12) C26 0.0264(13) 0.0281(14) 0.0347(15) 0.0112(11) 0.0066(11) 0.0072(11) C27 0.0356(16) 0.0477(18) 0.0412(17) 0.0150(14) 0.0150(13) 0.0134(14) C28 0.060(2) 0.059(2) 0.053(2) 0.0063(17) 0.0191(18) 0.0302(19) C29 0.0405(19) 0.068(3) 0.072(3) 0.030(2) 0.0268(18) 0.0050(18) C30 0.0431(18) 0.0365(17) 0.0475(18) -0.0038(14) 0.0119(14) 0.0104(14) C31 0.053(2) 0.0364(18) 0.074(3) -0.0109(17) 0.0035(18) 0.0168(16) C32 0.056(2) 0.063(2) 0.069(3) -0.006(2) 0.035(2) 0.0066(19) C33 0.0312(15) 0.0295(15) 0.0531(19) 0.0024(13) 0.0036(13) -0.0048(12) C34 0.052(2) 0.0344(19) 0.092(3) 0.0141(19) 0.006(2) -0.0075(16) C35 0.076(3) 0.065(3) 0.061(3) 0.005(2) -0.010(2) 0.019(2) C36 0.060(3) 0.079(3) 0.106(4) 0.047(3) 0.016(2) 0.035(2) C37 0.048(3) 0.188(8) 0.501(18) 0.218(10) 0.082(6) 0.062(4) C38 0.107(5) 0.329(11) 0.258(9) 0.247(9) 0.109(6) 0.150(7) C39 0.0407(17) 0.0365(17) 0.060(2) 0.0261(15) 0.0150(15) 0.0130(14) C40 0.072(3) 0.034(2) 0.129(4) 0.033(2) 0.006(3) -0.0011(19) C41 0.136(5) 0.085(3) 0.060(3) 0.034(3) 0.011(3) 0.034(3) C42 0.024(2) 0.061(3) 0.260(8) -0.032(4) 0.000(3) 0.005(2) C43 0.044(3) 0.072(3) 0.256(8) -0.015(4) -0.002(4) 0.032(2) C44 0.092(4) 0.211(8) 0.348(12) -0.213(9) -0.139(6) 0.108(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O7 1.781(2) . ? Ti1 O5 1.792(2) . ? Ti1 O3 1.948(2) . ? Ti1 O2 2.058(2) . ? Ti1 O4 2.101(2) . ? Ti1 N2 2.242(2) . ? Ti1 C2 2.596(3) . ? Ti1 Ti2 3.2235(11) . ? Ti2 O8 1.779(2) . ? Ti2 O6 1.802(2) . ? Ti2 O4 1.944(2) . ? Ti2 O1 2.063(2) . ? Ti2 O3 2.092(2) . ? Ti2 N1 2.240(2) . ? Ti2 C4 2.601(3) . ? Ti3 O14 1.770(2) . ? Ti3 O13 1.800(2) . ? Ti3 O11 1.953(2) . ? Ti3 O10 2.070(2) . ? Ti3 O12 2.092(2) . ? Ti3 N4 2.242(2) . ? Ti3 C24 2.605(3) . ? Ti3 Ti4 3.2251(11) . ? Ti4 O16 1.776(2) . ? Ti4 O15 1.805(2) . ? Ti4 O12 1.949(2) . ? Ti4 O9 2.077(2) . ? Ti4 O11 2.087(2) . ? Ti4 N3 2.240(2) . ? Ti4 C26 2.611(3) . ? N1 C1 1.325(3) . ? N1 C4 1.361(4) . ? N2 C1 1.319(3) 2_677 ? N2 C2 1.362(4) . ? N3 C23 1.322(3) . ? N3 C26 1.368(4) . ? N4 C23 1.319(3) 2_776 ? N4 C24 1.364(4) . ? O1 C4 1.303(3) . ? O2 C2 1.300(3) . ? O3 C5 1.443(3) . ? O4 C8 1.446(3) . ? O5 C11 1.408(4) . ? O6 C14 1.422(4) . ? O7 C17 1.414(4) . ? O8 C20 1.407(4) . ? O9 C26 1.299(3) . ? O10 C24 1.301(3) . ? O11 C27 1.452(3) . ? O12 C30 1.448(3) . ? O13 C33 1.425(3) . ? O14 C36 1.410(4) . ? O15 C39 1.418(3) . ? O16 C42 1.399(5) . ? C1 N2 1.319(3) 2_677 ? C2 C3 1.400(4) 2_677 ? C3 C4 1.394(4) . ? C3 C2 1.400(4) 2_677 ? C5 C7 1.514(5) . ? C5 C6 1.517(5) . ? C8 C10 1.519(5) . ? C8 C9 1.523(5) . ? C11 C13 1.472(7) . ? C11 C12 1.487(6) . ? C14 C15 1.480(6) . ? C14 C16 1.500(6) . ? C17 C19 1.468(7) . ? C17 C18 1.479(6) . ? C20 C22 1.396(9) . ? C20 C21 1.398(7) . ? C23 N4 1.319(3) 2_776 ? C24 C25 1.397(4) . ? C25 C26 1.398(4) 2_776 ? C26 C25 1.398(4) 2_776 ? C27 C28 1.514(5) . ? C27 C29 1.525(5) . ? C30 C32 1.518(5) . ? C30 C31 1.519(5) . ? C33 C35 1.492(5) . ? C33 C34 1.514(5) . ? C36 C38 1.342(6) . ? C36 C37 1.429(7) . ? C39 C40 1.482(5) . ? C39 C41 1.485(6) . ? C42 C44 1.232(7) . ? C42 C43 1.451(6) . ? 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 O7 Ti1 O5 97.50(10) . . ? O7 Ti1 O3 101.77(9) . . ? O5 Ti1 O3 108.53(9) . . ? O7 Ti1 O2 96.78(10) . . ? O5 Ti1 O2 99.84(9) . . ? O3 Ti1 O2 143.43(8) . . ? O7 Ti1 O4 174.68(9) . . ? O5 Ti1 O4 87.06(9) . . ? O3 Ti1 O4 74.06(8) . . ? O2 Ti1 O4 85.09(9) . . ? O7 Ti1 N2 87.25(10) . . ? O5 Ti1 N2 161.03(10) . . ? O3 Ti1 N2 88.27(8) . . ? O2 Ti1 N2 61.29(8) . . ? O4 Ti1 N2 89.30(8) . . ? O7 Ti1 C2 93.09(10) . . ? O5 Ti1 C2 129.44(10) . . ? O3 Ti1 C2 117.35(9) . . ? O2 Ti1 C2 29.66(8) . . ? O4 Ti1 C2 86.07(9) . . ? N2 Ti1 C2 31.64(8) . . ? O7 Ti1 Ti2 140.42(8) . . ? O5 Ti1 Ti2 97.18(7) . . ? O3 Ti1 Ti2 38.65(6) . . ? O2 Ti1 Ti2 116.52(7) . . ? O4 Ti1 Ti2 35.50(5) . . ? N2 Ti1 Ti2 90.54(6) . . ? C2 Ti1 Ti2 105.26(7) . . ? O8 Ti2 O6 96.85(10) . . ? O8 Ti2 O4 102.50(9) . . ? O6 Ti2 O4 109.68(9) . . ? O8 Ti2 O1 95.92(9) . . ? O6 Ti2 O1 99.12(9) . . ? O4 Ti2 O1 143.32(8) . . ? O8 Ti2 O3 175.20(9) . . ? O6 Ti2 O3 87.67(9) . . ? O4 Ti2 O3 74.34(8) . . ? O1 Ti2 O3 84.91(8) . . ? O8 Ti2 N1 86.97(10) . . ? O6 Ti2 N1 160.32(9) . . ? O4 Ti2 N1 88.14(8) . . ? O1 Ti2 N1 61.24(8) . . ? O3 Ti2 N1 89.30(8) . . ? O8 Ti2 C4 92.30(10) . . ? O6 Ti2 C4 128.78(10) . . ? O4 Ti2 C4 117.21(9) . . ? O1 Ti2 C4 29.69(8) . . ? O3 Ti2 C4 86.07(9) . . ? N1 Ti2 C4 31.56(8) . . ? O8 Ti2 Ti1 141.37(7) . . ? O6 Ti2 Ti1 98.24(7) . . ? O4 Ti2 Ti1 38.87(6) . . ? O1 Ti2 Ti1 116.35(7) . . ? O3 Ti2 Ti1 35.57(5) . . ? N1 Ti2 Ti1 90.46(6) . . ? C4 Ti2 Ti1 105.19(7) . . ? O14 Ti3 O13 97.56(10) . . ? O14 Ti3 O11 100.80(9) . . ? O13 Ti3 O11 109.86(9) . . ? O14 Ti3 O10 97.20(9) . . ? O13 Ti3 O10 97.76(9) . . ? O11 Ti3 O10 144.42(8) . . ? O14 Ti3 O12 174.07(9) . . ? O13 Ti3 O12 86.97(9) . . ? O11 Ti3 O12 73.96(8) . . ? O10 Ti3 O12 85.93(8) . . ? O14 Ti3 N4 89.01(9) . . ? O13 Ti3 N4 158.63(10) . . ? O11 Ti3 N4 88.65(8) . . ? O10 Ti3 N4 61.13(8) . . ? O12 Ti3 N4 88.10(8) . . ? O14 Ti3 C24 94.35(9) . . ? O13 Ti3 C24 127.21(10) . . ? O11 Ti3 C24 117.98(8) . . ? O10 Ti3 C24 29.58(8) . . ? O12 Ti3 C24 85.87(8) . . ? N4 Ti3 C24 31.56(8) . . ? O14 Ti3 Ti4 139.30(8) . . ? O13 Ti3 Ti4 98.03(7) . . ? O11 Ti3 Ti4 38.50(5) . . ? O10 Ti3 Ti4 117.51(7) . . ? O12 Ti3 Ti4 35.54(6) . . ? N4 Ti3 Ti4 89.89(6) . . ? C24 Ti3 Ti4 105.41(7) . . ? O16 Ti4 O15 96.34(9) . . ? O16 Ti4 O12 101.66(9) . . ? O15 Ti4 O12 108.73(9) . . ? O16 Ti4 O9 96.19(9) . . ? O15 Ti4 O9 99.91(9) . . ? O12 Ti4 O9 144.03(8) . . ? O16 Ti4 O11 175.19(9) . . ? O15 Ti4 O11 87.35(8) . . ? O12 Ti4 O11 74.16(8) . . ? O9 Ti4 O11 86.17(8) . . ? O16 Ti4 N3 87.30(9) . . ? O15 Ti4 N3 160.93(9) . . ? O12 Ti4 N3 88.70(8) . . ? O9 Ti4 N3 61.05(8) . . ? O11 Ti4 N3 90.20(8) . . ? O16 Ti4 C26 92.12(9) . . ? O15 Ti4 C26 129.36(10) . . ? O12 Ti4 C26 118.18(8) . . ? O9 Ti4 C26 29.46(8) . . ? O11 Ti4 C26 87.88(8) . . ? N3 Ti4 C26 31.59(8) . . ? O16 Ti4 Ti3 140.28(8) . . ? O15 Ti4 Ti3 97.61(7) . . ? O12 Ti4 Ti3 38.62(6) . . ? O9 Ti4 Ti3 117.59(6) . . ? O11 Ti4 Ti3 35.63(5) . . ? N3 Ti4 Ti3 91.28(6) . . ? C26 Ti4 Ti3 106.91(6) . . ? C1 N1 C4 118.6(2) . . ? C1 N1 Ti2 152.38(19) . . ? C4 N1 Ti2 89.03(16) . . ? C1 N2 C2 118.6(2) 2_677 . ? C1 N2 Ti1 152.74(19) 2_677 . ? C2 N2 Ti1 88.65(16) . . ? C23 N3 C26 118.6(2) . . ? C23 N3 Ti4 151.96(19) . . ? C26 N3 Ti4 89.35(15) . . ? C23 N4 C24 118.9(2) 2_776 . ? C23 N4 Ti3 151.95(19) 2_776 . ? C24 N4 Ti3 89.05(16) . . ? C4 O1 Ti2 98.69(17) . . ? C2 O2 Ti1 98.77(17) . . ? C5 O3 Ti1 129.96(18) . . ? C5 O3 Ti2 120.70(18) . . ? Ti1 O3 Ti2 105.78(9) . . ? C8 O4 Ti2 130.59(18) . . ? C8 O4 Ti1 119.99(17) . . ? Ti2 O4 Ti1 105.63(9) . . ? C11 O5 Ti1 141.6(2) . . ? C14 O6 Ti2 137.8(2) . . ? C17 O7 Ti1 155.9(2) . . ? C20 O8 Ti2 156.5(2) . . ? C26 O9 Ti4 98.70(17) . . ? C24 O10 Ti3 98.64(17) . . ? C27 O11 Ti3 130.79(18) . . ? C27 O11 Ti4 120.38(17) . . ? Ti3 O11 Ti4 105.87(9) . . ? C30 O12 Ti4 130.32(19) . . ? C30 O12 Ti3 121.04(18) . . ? Ti4 O12 Ti3 105.84(9) . . ? C33 O13 Ti3 138.10(19) . . ? C36 O14 Ti3 161.1(2) . . ? C39 O15 Ti4 135.16(19) . . ? C42 O16 Ti4 159.0(3) . . ? N2 C1 N1 124.2(3) 2_677 . ? O2 C2 N2 111.3(2) . . ? O2 C2 C3 127.5(3) . 2_677 ? N2 C2 C3 121.2(3) . 2_677 ? O2 C2 Ti1 51.57(14) . . ? N2 C2 Ti1 59.71(14) . . ? C3 C2 Ti1 178.1(2) 2_677 . ? C4 C3 C2 116.0(3) . 2_677 ? O1 C4 N1 111.0(2) . . ? O1 C4 C3 127.7(3) . . ? N1 C4 C3 121.3(3) . . ? O1 C4 Ti2 51.62(13) . . ? N1 C4 Ti2 59.42(14) . . ? C3 C4 Ti2 178.8(2) . . ? O3 C5 C7 109.2(3) . . ? O3 C5 C6 110.0(3) . . ? C7 C5 C6 114.1(3) . . ? O4 C8 C10 109.6(3) . . ? O4 C8 C9 109.2(2) . . ? C10 C8 C9 114.1(3) . . ? O5 C11 C13 109.3(4) . . ? O5 C11 C12 109.7(3) . . ? C13 C11 C12 111.4(4) . . ? O6 C14 C15 108.7(3) . . ? O6 C14 C16 108.3(3) . . ? C15 C14 C16 113.1(4) . . ? O7 C17 C19 111.7(4) . . ? O7 C17 C18 110.9(4) . . ? C19 C17 C18 113.2(4) . . ? C22 C20 C21 113.4(6) . . ? C22 C20 O8 113.0(5) . . ? C21 C20 O8 112.1(4) . . ? N4 C23 N3 124.1(3) 2_776 . ? O10 C24 N4 111.1(2) . . ? O10 C24 C25 127.8(3) . . ? N4 C24 C25 121.1(2) . . ? O10 C24 Ti3 51.78(13) . . ? N4 C24 Ti3 59.38(13) . . ? C25 C24 Ti3 178.3(2) . . ? C24 C25 C26 116.2(3) . 2_776 ? O9 C26 N3 110.9(2) . . ? O9 C26 C25 128.0(3) . 2_776 ? N3 C26 C25 121.1(2) . 2_776 ? O9 C26 Ti4 51.84(14) . . ? N3 C26 Ti4 59.06(13) . . ? C25 C26 Ti4 179.3(2) 2_776 . ? O11 C27 C28 109.2(2) . . ? O11 C27 C29 109.7(3) . . ? C28 C27 C29 113.8(3) . . ? O12 C30 C32 108.5(3) . . ? O12 C30 C31 110.3(3) . . ? C32 C30 C31 114.0(3) . . ? O13 C33 C35 109.5(3) . . ? O13 C33 C34 107.3(3) . . ? C35 C33 C34 112.7(3) . . ? C38 C36 O14 115.1(4) . . ? C38 C36 C37 115.5(6) . . ? O14 C36 C37 111.8(4) . . ? O15 C39 C40 109.6(3) . . ? O15 C39 C41 109.1(3) . . ? C40 C39 C41 113.9(4) . . ? C44 C42 O16 123.3(4) . . ? C44 C42 C43 124.3(5) . . ? O16 C42 C43 112.4(4) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.816 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.075 #===END data_tjb112p _database_code_CSD 218030 _chemical_name_common Ti2(DHP)(ONep)6(Py)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H39 N4 O8 Ti2' _chemical_formula_weight 847.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.250(7) _cell_length_b 16.064(12) _cell_length_c 16.906(12) _cell_angle_alpha 71.802(13) _cell_angle_beta 86.040(16) _cell_angle_gamma 88.807(14) _cell_volume 2638(3) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8734 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9296 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.1374 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 21.05 _reflns_number_total 5497 _reflns_number_gt 2414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1964P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5497 _refine_ls_number_parameters 433 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1939 _refine_ls_R_factor_gt 0.1051 _refine_ls_wR_factor_ref 0.3327 _refine_ls_wR_factor_gt 0.2743 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.123 _refine_ls_shift/su_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.57820(19) 0.65167(13) 0.18760(12) 0.0726(8) Uani 1 1 d . . . Ti2 Ti 0.3135(2) 0.24608(12) 0.24557(12) 0.0746(8) Uani 1 1 d . . . N1 N 0.4829(8) 0.5221(5) 0.2044(5) 0.057(2) Uani 1 1 d . . . N2 N 0.3907(7) 0.3829(5) 0.2253(5) 0.053(2) Uani 1 1 d . . . N3 N 0.4028(9) 0.7005(5) 0.1088(6) 0.063(2) Uani 1 1 d . . . N4 N 0.1592(10) 0.3193(5) 0.1551(6) 0.072(3) Uani 1 1 d . . . O1 O 0.6228(6) 0.5867(5) 0.0992(4) 0.0689(19) Uani 1 1 d . . . O2 O 0.4410(7) 0.3021(5) 0.1422(4) 0.071(2) Uani 1 1 d . . . O3 O 0.6522(7) 0.7527(5) 0.1273(4) 0.091(2) Uani 1 1 d D . . O4 O 0.4791(7) 0.6725(5) 0.2719(4) 0.087(2) Uani 1 1 d D . . O5 O 0.7099(7) 0.5997(5) 0.2486(5) 0.099(3) Uani 1 1 d D . . O6 O 0.2719(9) 0.1559(5) 0.2147(5) 0.114(3) Uani 1 1 d D . . O7 O 0.1978(7) 0.2517(5) 0.3284(4) 0.086(2) Uani 1 1 d D . . O8 O 0.4457(8) 0.2026(5) 0.3092(5) 0.111(3) Uani 1 1 d D . . C1 C 0.4067(10) 0.4558(8) 0.2443(6) 0.060(3) Uani 1 1 d . . . H1 H 0.3574 0.4606 0.2924 0.072 Uiso 1 1 calc R . . C2 C 0.5508(10) 0.5158(8) 0.1339(6) 0.061(3) Uani 1 1 d . . . C3 C 0.5446(9) 0.4431(7) 0.1077(6) 0.051(2) Uani 1 1 d . . . H3 H 0.5937 0.4388 0.0593 0.061 Uiso 1 1 calc R . . C4 C 0.4637(9) 0.3780(7) 0.1553(6) 0.053(3) Uani 1 1 d . . . C5 C 0.2927(14) 0.7228(8) 0.1412(7) 0.085(3) Uani 1 1 d . . . H5 H 0.2833 0.7130 0.1997 0.102 Uiso 1 1 calc R . . C6 C 0.1912(14) 0.7597(9) 0.0941(11) 0.107(4) Uani 1 1 d . . . H6 H 0.1120 0.7735 0.1198 0.128 Uiso 1 1 calc R . . C7 C 0.2046(15) 0.7768(7) 0.0079(10) 0.097(4) Uani 1 1 d . . . H7 H 0.1354 0.8025 -0.0263 0.117 Uiso 1 1 calc R . . C8 C 0.3205(15) 0.7554(7) -0.0261(8) 0.084(3) Uani 1 1 d . . . H8 H 0.3339 0.7660 -0.0846 0.100 Uiso 1 1 calc R . . C9 C 0.4136(11) 0.7198(7) 0.0243(8) 0.071(3) Uani 1 1 d . . . H9 H 0.4941 0.7065 -0.0004 0.085 Uiso 1 1 calc R . . C10 C 0.6177(16) 0.8458(9) 0.0929(10) 0.110(5) Uiso 0.80 1 d PD . . C10' C 0.727(6) 0.820(2) 0.083(3) 0.074(15) Uiso 0.20 1 d PD . . C11 C 0.7198(12) 0.8985(8) 0.1188(7) 0.104(4) Uiso 1 1 d D . . C12 C 0.8508(16) 0.8819(12) 0.0735(11) 0.136(7) Uiso 0.80 1 d PD . . C12' C 0.774(6) 0.991(2) 0.071(4) 0.10(2) Uiso 0.20 1 d PD . . C13 C 0.725(2) 0.8764(13) 0.2139(9) 0.131(7) Uiso 0.80 1 d PD . . C13' C 0.790(4) 0.860(3) 0.2014(19) 0.046(13) Uiso 0.20 1 d PD . . C14 C 0.679(2) 0.9960(11) 0.0813(13) 0.146(8) Uiso 0.80 1 d PD . . C14' C 0.569(2) 0.897(6) 0.132(5) 0.15(3) Uiso 0.20 1 d PD . . C15 C 0.5209(19) 0.6558(19) 0.3572(10) 0.094(9) Uiso 0.50 1 d PD . . C15' C 0.473(3) 0.6168(16) 0.3603(11) 0.144(14) Uiso 0.50 1 d PD . . C16 C 0.4044(12) 0.6690(8) 0.4132(7) 0.098(4) Uiso 1 1 d D . . C17 C 0.4429(19) 0.6376(12) 0.5047(10) 0.186(7) Uiso 1 1 d D . . C18 C 0.295(3) 0.606(2) 0.409(2) 0.158(12) Uiso 0.50 1 d PD . . C18' C 0.263(2) 0.695(2) 0.3941(18) 0.127(10) Uiso 0.50 1 d PD . . C19 C 0.327(3) 0.7537(17) 0.3859(19) 0.136(11) Uiso 0.50 1 d PD . . C19' C 0.454(4) 0.7642(16) 0.384(3) 0.205(17) Uiso 0.50 1 d PD . . C20 C 0.8420(16) 0.5831(14) 0.2255(12) 0.193(8) Uiso 1 1 d D . . C21 C 0.9209(14) 0.5467(10) 0.3031(9) 0.122(5) Uiso 1 1 d D . . C22 C 0.818(4) 0.482(3) 0.291(3) 0.24(2) Uiso 0.50 1 d PD . . C22' C 0.894(5) 0.465(2) 0.382(2) 0.23(2) Uiso 0.50 1 d PD . . C23 C 1.0595(17) 0.5208(12) 0.2719(11) 0.181(7) Uiso 1 1 d D . . C24 C 0.882(3) 0.557(2) 0.3902(14) 0.120(9) Uiso 0.50 1 d PD . . C24' C 0.932(4) 0.625(2) 0.339(2) 0.175(14) Uiso 0.50 1 d PD . . C25 C 0.0390(14) 0.3290(8) 0.1838(8) 0.082(3) Uani 1 1 d . . . H25 H 0.0195 0.3112 0.2424 0.098 Uiso 1 1 calc R . . C26 C -0.0611(14) 0.3644(10) 0.1311(11) 0.116(5) Uani 1 1 d . . . H26 H -0.1461 0.3717 0.1541 0.139 Uiso 1 1 calc R . . C27 C -0.0366(17) 0.3885(10) 0.0471(11) 0.127(5) Uani 1 1 d . . . H27 H -0.1031 0.4141 0.0106 0.152 Uiso 1 1 calc R . . C28 C 0.0857(19) 0.3751(11) 0.0165(9) 0.129(6) Uani 1 1 d . . . H28 H 0.1046 0.3871 -0.0418 0.155 Uiso 1 1 calc R . . C29 C 0.1819(13) 0.3435(8) 0.0720(9) 0.102(4) Uani 1 1 d . . . H29 H 0.2686 0.3388 0.0500 0.123 Uiso 1 1 calc R . . C30 C 0.290(2) 0.0803(12) 0.1858(13) 0.084(7) Uiso 0.50 1 d PD . . C30' C 0.165(3) 0.1125(17) 0.190(3) 0.24(2) Uiso 0.50 1 d PD . . C31 C 0.1826(15) 0.0152(10) 0.2272(8) 0.117(5) Uiso 1 1 d D . . C32 C 0.171(3) -0.0647(16) 0.1927(17) 0.129(10) Uiso 0.50 1 d PD . . C32' C 0.311(3) -0.018(3) 0.186(2) 0.197(16) Uiso 0.50 1 d PD . . C33 C 0.2139(19) -0.0194(12) 0.3238(10) 0.185(7) Uiso 1 1 d D . . C34 C 0.067(4) 0.061(3) 0.171(3) 0.224(18) Uiso 0.50 1 d PD . . C34' C 0.047(3) 0.004(4) 0.278(3) 0.30(3) Uiso 0.50 1 d PD . . C35 C 0.2152(15) 0.2687(10) 0.4082(8) 0.145(6) Uiso 1 1 d D . . C36 C 0.1274(11) 0.2090(8) 0.4777(7) 0.091(4) Uiso 1 1 d D . . C37 C 0.126(4) 0.1128(14) 0.474(2) 0.147(12) Uiso 0.50 1 d PD . . C37' C 0.230(4) 0.134(2) 0.490(3) 0.207(17) Uiso 0.50 1 d PD . . C38 C -0.002(2) 0.2638(19) 0.4625(18) 0.123(10) Uiso 0.50 1 d PD . . C38' C -0.0184(18) 0.2070(18) 0.4573(15) 0.101(8) Uiso 0.50 1 d PD . . C39 C 0.185(3) 0.186(2) 0.5664(13) 0.126(11) Uiso 0.50 1 d PD . . C39' C 0.134(4) 0.238(3) 0.5576(18) 0.178(15) Uiso 0.50 1 d PD . . C40 C 0.555(2) 0.1615(19) 0.2750(18) 0.290(13) Uiso 1 1 d D . . C41 C 0.6522(15) 0.1312(10) 0.3437(9) 0.123(5) Uiso 1 1 d D . . C42 C 0.778(2) 0.0941(15) 0.3170(14) 0.235(10) Uiso 1 1 d D . . C43 C 0.631(2) 0.1133(15) 0.4346(13) 0.232(10) Uiso 1 1 d D . . C44 C 0.682(3) 0.2293(17) 0.314(2) 0.349(17) Uiso 1 1 d 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 Ti1 0.0676(14) 0.0824(15) 0.0784(15) -0.0413(12) 0.0034(11) -0.0157(11) Ti2 0.0828(16) 0.0600(13) 0.0745(15) -0.0136(11) 0.0052(12) -0.0012(11) N1 0.050(5) 0.066(6) 0.052(6) -0.017(5) 0.012(4) -0.016(5) N2 0.052(5) 0.056(6) 0.055(5) -0.024(4) 0.009(4) 0.000(4) N3 0.067(7) 0.065(6) 0.066(7) -0.035(5) 0.018(5) -0.008(5) N4 0.086(8) 0.073(6) 0.058(7) -0.024(5) 0.011(5) -0.021(5) O1 0.064(5) 0.081(5) 0.062(4) -0.025(4) 0.014(4) -0.007(4) O2 0.084(5) 0.067(5) 0.064(4) -0.027(4) 0.005(4) 0.005(4) O3 0.094(6) 0.087(5) 0.103(6) -0.046(5) 0.009(5) -0.033(5) O4 0.097(6) 0.108(6) 0.068(5) -0.047(4) 0.001(4) -0.006(5) O5 0.070(5) 0.142(7) 0.100(6) -0.061(5) -0.003(4) -0.008(5) O6 0.132(8) 0.071(5) 0.135(7) -0.028(5) 0.009(6) -0.022(5) O7 0.083(5) 0.107(6) 0.055(4) -0.004(4) -0.009(4) -0.011(4) O8 0.103(6) 0.102(6) 0.107(6) -0.008(5) 0.008(5) 0.025(5) C1 0.047(7) 0.085(8) 0.055(7) -0.035(7) 0.001(5) 0.019(7) C2 0.049(7) 0.073(8) 0.051(7) -0.009(6) 0.007(6) -0.006(6) C3 0.048(6) 0.060(7) 0.052(6) -0.030(6) 0.008(5) 0.002(6) C4 0.042(6) 0.058(7) 0.062(7) -0.024(6) 0.001(6) 0.006(6) C5 0.085(10) 0.102(10) 0.064(8) -0.023(7) -0.002(8) 0.003(8) C6 0.105(12) 0.109(11) 0.112(12) -0.048(9) 0.010(10) 0.020(9) C7 0.109(12) 0.063(8) 0.122(13) -0.026(8) -0.040(10) 0.019(8) C8 0.100(11) 0.081(9) 0.079(9) -0.039(7) -0.007(9) 0.016(8) C9 0.066(8) 0.075(8) 0.079(9) -0.037(7) -0.004(7) 0.005(6) C25 0.072(9) 0.106(10) 0.076(8) -0.041(7) -0.008(8) -0.002(8) C26 0.088(11) 0.164(14) 0.097(11) -0.039(10) -0.007(10) -0.011(10) C27 0.106(14) 0.160(14) 0.105(14) -0.022(11) -0.019(11) -0.045(11) C28 0.113(13) 0.186(16) 0.068(10) -0.004(10) -0.018(11) -0.032(12) C29 0.088(10) 0.134(12) 0.070(10) -0.012(8) 0.012(8) -0.021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.778(7) . ? Ti1 O5 1.786(8) . ? Ti1 O4 1.805(7) . ? Ti1 O1 2.095(7) . ? Ti1 N1 2.246(9) . ? Ti1 N3 2.290(9) . ? Ti1 C2 2.639(13) . ? Ti2 O6 1.755(9) . ? Ti2 O8 1.782(8) . ? Ti2 O7 1.794(7) . ? Ti2 O2 2.079(7) . ? Ti2 N2 2.267(8) . ? Ti2 N4 2.315(9) . ? Ti2 C4 2.642(11) . ? N1 C1 1.308(11) . ? N1 C2 1.368(12) . ? N2 C1 1.324(11) . ? N2 C4 1.379(11) . ? N3 C5 1.313(13) . ? N3 C9 1.361(12) . ? N4 C25 1.317(13) . ? N4 C29 1.340(13) . ? O1 C2 1.321(11) . ? O2 C4 1.332(11) . ? O3 C10' 1.33(5) . ? O3 C10 1.470(13) . ? O4 C15 1.476(14) . ? O4 C15' 1.481(15) . ? O5 C20 1.427(14) . ? O6 C30 1.448(14) . ? O6 C30' 1.463(17) . ? O7 C35 1.480(13) . ? O8 C40 1.462(16) . ? C2 C3 1.377(12) . ? C3 C4 1.360(12) . ? C5 C6 1.364(15) . ? C6 C7 1.394(16) . ? C7 C8 1.368(16) . ? C8 C9 1.322(13) . ? C10 C11 1.529(13) . ? C10' C11 1.550(17) . ? C11 C13 1.540(13) . ? C11 C12' 1.547(17) . ? C11 C14' 1.551(17) . ? C11 C14 1.553(13) . ? C11 C12 1.559(13) . ? C11 C13' 1.561(16) . ? C15 C16 1.525(15) . ? C15' C16 1.533(16) . ? C16 C19 1.520(16) . ? C16 C18' 1.528(15) . ? C16 C19' 1.539(17) . ? C16 C18 1.541(16) . ? C16 C17 1.546(13) . ? C20 C21 1.539(14) . ? C21 C24 1.559(16) . ? C21 C22' 1.567(17) . ? C21 C22 1.567(18) . ? C21 C24' 1.569(17) . ? C21 C23 1.575(14) . ? C25 C26 1.398(15) . ? C26 C27 1.357(16) . ? C27 C28 1.361(18) . ? C28 C29 1.386(16) . ? C30 C31 1.51(2) . ? C30' C31 1.50(3) . ? C31 C34' 1.57(2) . ? C31 C32 1.576(17) . ? C31 C32' 1.596(19) . ? C31 C34 1.596(19) . ? C31 C33 1.605(15) . ? C35 C36 1.516(13) . ? C36 C37' 1.558(17) . ? C36 C38' 1.560(15) . ? C36 C39' 1.566(16) . ? C36 C38 1.569(15) . ? C36 C37 1.570(16) . ? C36 C39 1.579(15) . ? C40 C41 1.54(3) . ? C41 C43 1.473(17) . ? C41 C42 1.508(17) . ? C41 C44 1.527(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 O3 Ti1 O5 101.0(4) . . ? O3 Ti1 O4 107.2(3) . . ? O5 Ti1 O4 96.4(3) . . ? O3 Ti1 O1 95.5(3) . . ? O5 Ti1 O1 92.2(3) . . ? O4 Ti1 O1 153.6(3) . . ? O3 Ti1 N1 153.8(3) . . ? O5 Ti1 N1 91.7(3) . . ? O4 Ti1 N1 93.9(3) . . ? O1 Ti1 N1 60.9(3) . . ? O3 Ti1 N3 85.0(3) . . ? O5 Ti1 N3 172.5(3) . . ? O4 Ti1 N3 86.0(3) . . ? O1 Ti1 N3 82.7(3) . . ? N1 Ti1 N3 81.1(3) . . ? O3 Ti1 C2 124.6(3) . . ? O5 Ti1 C2 91.4(3) . . ? O4 Ti1 C2 124.9(3) . . ? O1 Ti1 C2 29.7(2) . . ? N1 Ti1 C2 31.2(3) . . ? N3 Ti1 C2 81.4(3) . . ? O6 Ti2 O8 101.3(4) . . ? O6 Ti2 O7 107.9(4) . . ? O8 Ti2 O7 96.7(4) . . ? O6 Ti2 O2 95.5(4) . . ? O8 Ti2 O2 91.8(3) . . ? O7 Ti2 O2 152.9(3) . . ? O6 Ti2 N2 155.0(3) . . ? O8 Ti2 N2 89.2(3) . . ? O7 Ti2 N2 93.1(3) . . ? O2 Ti2 N2 61.3(3) . . ? O6 Ti2 N4 84.3(3) . . ? O8 Ti2 N4 172.2(4) . . ? O7 Ti2 N4 86.5(3) . . ? O2 Ti2 N4 82.3(3) . . ? N2 Ti2 N4 83.6(3) . . ? O6 Ti2 C4 125.0(4) . . ? O8 Ti2 C4 89.8(3) . . ? O7 Ti2 C4 124.2(3) . . ? O2 Ti2 C4 29.8(3) . . ? N2 Ti2 C4 31.5(3) . . ? N4 Ti2 C4 82.6(3) . . ? C1 N1 C2 115.9(9) . . ? C1 N1 Ti1 153.6(7) . . ? C2 N1 Ti1 90.5(7) . . ? C1 N2 C4 114.9(8) . . ? C1 N2 Ti2 155.5(7) . . ? C4 N2 Ti2 89.5(6) . . ? C5 N3 C9 116.4(10) . . ? C5 N3 Ti1 121.5(8) . . ? C9 N3 Ti1 121.5(8) . . ? C25 N4 C29 116.9(10) . . ? C25 N4 Ti2 120.3(8) . . ? C29 N4 Ti2 122.3(9) . . ? C2 O1 Ti1 98.6(6) . . ? C4 O2 Ti2 99.2(6) . . ? C10' O3 C10 50(2) . . ? C10' O3 Ti1 170(2) . . ? C10 O3 Ti1 139.5(9) . . ? C15 O4 C15' 31.1(16) . . ? C15 O4 Ti1 124.6(8) . . ? C15' O4 Ti1 125.8(9) . . ? C20 O5 Ti1 131.6(9) . . ? C30 O6 C30' 56.4(18) . . ? C30 O6 Ti2 158.6(10) . . ? C30' O6 Ti2 144.5(16) . . ? C35 O7 Ti2 131.5(8) . . ? C40 O8 Ti2 118.7(15) . . ? N1 C1 N2 127.3(9) . . ? O1 C2 N1 110.0(10) . . ? O1 C2 C3 127.2(10) . . ? N1 C2 C3 122.8(10) . . ? O1 C2 Ti1 51.7(5) . . ? N1 C2 Ti1 58.3(6) . . ? C3 C2 Ti1 176.2(7) . . ? C4 C3 C2 115.7(9) . . ? O2 C4 C3 126.7(10) . . ? O2 C4 N2 110.0(9) . . ? C3 C4 N2 123.3(9) . . ? O2 C4 Ti2 50.9(5) . . ? C3 C4 Ti2 177.3(8) . . ? N2 C4 Ti2 59.1(5) . . ? N3 C5 C6 122.5(11) . . ? C5 C6 C7 119.5(13) . . ? C8 C7 C6 117.9(12) . . ? C9 C8 C7 118.5(12) . . ? C8 C9 N3 125.0(11) . . ? O3 C10 C11 107.3(11) . . ? O3 C10' C11 114(3) . . ? C10 C11 C13 113.8(12) . . ? C10 C11 C12' 129(3) . . ? C13 C11 C12' 112(3) . . ? C10 C11 C10' 46(2) . . ? C13 C11 C10' 117(2) . . ? C12' C11 C10' 124(3) . . ? C10 C11 C14' 49(3) . . ? C13 C11 C14' 88(3) . . ? C12' C11 C14' 112(4) . . ? C10' C11 C14' 95(4) . . ? C10 C11 C14 105.4(12) . . ? C13 C11 C14 109.1(14) . . ? C12' C11 C14 37(2) . . ? C10' C11 C14 133(2) . . ? C14' C11 C14 76(3) . . ? C10 C11 C12 104.8(12) . . ? C13 C11 C12 114.0(13) . . ? C12' C11 C12 75(3) . . ? C10' C11 C12 62(2) . . ? C14' C11 C12 153(3) . . ? C14 C11 C12 109.3(13) . . ? C10 C11 C13' 121.8(19) . . ? C13 C11 C13' 28.1(18) . . ? C12' C11 C13' 110(3) . . ? C10' C11 C13' 102(3) . . ? C14' C11 C13' 113(3) . . ? C14 C11 C13' 125(2) . . ? C12 C11 C13' 86(2) . . ? O4 C15 C16 109.0(12) . . ? O4 C15' C16 108.2(13) . . ? C19 C16 C15 118.9(18) . . ? C19 C16 C18' 43.6(15) . . ? C15 C16 C18' 131.0(15) . . ? C19 C16 C15' 129.6(16) . . ? C15 C16 C15' 30.0(15) . . ? C18' C16 C15' 115(2) . . ? C19 C16 C19' 50.9(17) . . ? C15 C16 C19' 83(2) . . ? C18' C16 C19' 94(2) . . ? C15' C16 C19' 111(2) . . ? C19 C16 C18 97(2) . . ? C15 C16 C18 107.7(18) . . ? C18' C16 C18 54.1(16) . . ? C15' C16 C18 78(2) . . ? C19' C16 C18 146(2) . . ? C19 C16 C17 116.8(17) . . ? C15 C16 C17 108.6(12) . . ? C18' C16 C17 119.8(15) . . ? C15' C16 C17 112.6(13) . . ? C19' C16 C17 101.1(19) . . ? C18 C16 C17 105.4(16) . . ? O5 C20 C21 110.8(13) . . ? C20 C21 C24 124.7(15) . . ? C20 C21 C22' 130(2) . . ? C24 C21 C22' 59.1(19) . . ? C20 C21 C22 65.0(19) . . ? C24 C21 C22 106(2) . . ? C22' C21 C22 67(2) . . ? C20 C21 C24' 104.6(18) . . ? C24 C21 C24' 47.4(15) . . ? C22' C21 C24' 105(2) . . ? C22 C21 C24' 141(3) . . ? C20 C21 C23 106.8(12) . . ? C24 C21 C23 126.8(15) . . ? C22' C21 C23 99(2) . . ? C22 C21 C23 108(2) . . ? C24' C21 C23 110.9(19) . . ? N4 C25 C26 122.4(12) . . ? C27 C26 C25 120.0(14) . . ? C26 C27 C28 118.3(15) . . ? C27 C28 C29 118.8(14) . . ? N4 C29 C28 123.4(12) . . ? O6 C30 C31 108.3(14) . . ? O6 C30' C31 107.8(17) . . ? C30' C31 C30 54.3(17) . . ? C30' C31 C34' 93(3) . . ? C30 C31 C34' 144(3) . . ? C30' C31 C32 133(2) . . ? C30 C31 C32 116.1(16) . . ? C34' C31 C32 97(3) . . ? C30' C31 C32' 111(2) . . ? C30 C31 C32' 61.0(16) . . ? C34' C31 C32' 155(3) . . ? C32 C31 C32' 61.3(17) . . ? C30' C31 C34 54.7(18) . . ? C30 C31 C34 99(2) . . ? C34' C31 C34 67(2) . . ? C32 C31 C34 88(2) . . ? C32' C31 C34 120(2) . . ? C30' C31 C33 116(2) . . ? C30 C31 C33 104.6(13) . . ? C34' C31 C33 74(2) . . ? C32 C31 C33 110.0(15) . . ? C32' C31 C33 100.1(18) . . ? C34 C31 C33 139(2) . . ? O7 C35 C36 110.4(11) . . ? C35 C36 C37' 90.6(19) . . ? C35 C36 C38' 114.8(13) . . ? C37' C36 C38' 128(2) . . ? C35 C36 C39' 108.7(18) . . ? C37' C36 C39' 104(2) . . ? C38' C36 C39' 109(2) . . ? C35 C36 C38 98.9(14) . . ? C37' C36 C38 164(2) . . ? C38' C36 C38 35.8(13) . . ? C39' C36 C38 86(2) . . ? C35 C36 C37 112.2(16) . . ? C37' C36 C37 45.4(17) . . ? C38' C36 C37 82.5(18) . . ? C39' C36 C37 127(2) . . ? C38 C36 C37 118(2) . . ? C35 C36 C39 113.5(15) . . ? C37' C36 C39 68.7(19) . . ? C38' C36 C39 127.9(17) . . ? C39' C36 C39 35.3(16) . . ? C38 C36 C39 118.4(19) . . ? C37 C36 C39 96.4(19) . . ? O8 C40 C41 106.5(18) . . ? C43 C41 C42 114.2(17) . . ? C43 C41 C44 102.1(19) . . ? C42 C41 C44 101.6(19) . . ? C43 C41 C40 129.8(17) . . ? C42 C41 C40 114.2(15) . . ? C44 C41 C40 80.4(17) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 21.05 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.683 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.111 #===END data_tjb137s _database_code_CSD 218031 _chemical_name_common Ti2(DHP)(OPri)4.5(OBut)1.5(Py)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 N4 O8 Ti2' _chemical_formula_weight 720.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5723(12) _cell_length_b 18.416(2) _cell_length_c 24.619(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.200(3) _cell_angle_gamma 90.00 _cell_volume 4257.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max .210 _exptl_crystal_size_mid .175 _exptl_crystal_size_min .135 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9174 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26554 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.28 _reflns_number_total 6133 _reflns_number_gt 3678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1854P)^2^+5.3652P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6133 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.3076 _refine_ls_wR_factor_gt 0.2657 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.27990(13) 0.47643(7) 0.17823(5) 0.0493(5) Uani 1 1 d . . . Ti2 Ti 0.41286(14) 0.76481(7) 0.01528(6) 0.0536(5) Uani 1 1 d . . . N1 N 0.3164(6) 0.5698(3) 0.1230(2) 0.0425(13) Uani 1 1 d . . . N2 N 0.3514(6) 0.6660(3) 0.0644(2) 0.0447(14) Uani 1 1 d . . . N3 N 0.1734(6) 0.4293(3) 0.0941(2) 0.0486(15) Uani 1 1 d . . . N4 N 0.2735(6) 0.7074(3) -0.0610(2) 0.0535(15) Uani 1 1 d . . . O1 O 0.4549(5) 0.4726(2) 0.13723(18) 0.0472(12) Uani 1 1 d . . . O2 O 0.5271(5) 0.6679(3) 0.0182(2) 0.0546(13) Uani 1 1 d . . . O3 O 0.1003(5) 0.5072(3) 0.1822(2) 0.0564(13) Uani 1 1 d . . . O4 O 0.2900(6) 0.3827(3) 0.2002(2) 0.0619(14) Uani 1 1 d . . . O5 O 0.3787(5) 0.5199(3) 0.2384(2) 0.0614(14) Uani 1 1 d . . . O6 O 0.5122(5) 0.7982(3) 0.0791(2) 0.0666(15) Uani 1 1 d . . . O7 O 0.5033(6) 0.8049(3) -0.0338(2) 0.0726(16) Uani 1 1 d . . . O8 O 0.2510(6) 0.8164(3) 0.0147(2) 0.0650(15) Uani 1 1 d . . . C1 C 0.2824(7) 0.6338(4) 0.0999(3) 0.0443(17) Uani 1 1 d . . . C2 C 0.4323(7) 0.5333(4) 0.1108(3) 0.0471(18) Uani 1 1 d . . . C3 C 0.5094(7) 0.5633(4) 0.0734(3) 0.0513(18) Uani 1 1 d . . . H3 H 0.5882 0.5385 0.0638 0.062 Uiso 1 1 calc R . . C4 C 0.4664(7) 0.6310(4) 0.0507(3) 0.0463(17) Uani 1 1 d . . . C5 C 0.0387(8) 0.4465(4) 0.0693(3) 0.0538(19) Uani 1 1 d . . . H5 H -0.0113 0.4826 0.0855 0.065 Uiso 1 1 calc R . . C6 C -0.0281(9) 0.4126(5) 0.0208(3) 0.063(2) Uani 1 1 d . . . H6 H -0.1211 0.4270 0.0031 0.075 Uiso 1 1 calc R . . C7 C 0.0413(9) 0.3580(5) -0.0015(3) 0.070(2) Uani 1 1 d . . . H7 H -0.0037 0.3333 -0.0341 0.084 Uiso 1 1 calc R . . C8 C 0.1765(9) 0.3402(5) 0.0244(3) 0.072(2) Uani 1 1 d . . . H8 H 0.2264 0.3025 0.0099 0.087 Uiso 1 1 calc R . . C9 C 0.2407(8) 0.3770(5) 0.0716(3) 0.063(2) Uani 1 1 d . . . H9 H 0.3355 0.3647 0.0886 0.076 Uiso 1 1 calc R . . C10 C 0.0439(11) 0.5612(6) 0.2128(4) 0.087(3) Uani 1 1 d . . . C11 C -0.0895(16) 0.5931(9) 0.1738(7) 0.163(6) Uani 1 1 d . . . C12 C 0.0129(15) 0.5220(9) 0.2648(5) 0.139(5) Uani 1 1 d . . . C13 C 0.3668(11) 0.3386(5) 0.2430(4) 0.087(3) Uani 1 1 d . . . C14 C 0.5057(14) 0.3146(9) 0.2281(6) 0.144(5) Uani 1 1 d . . . C15 C 0.2689(14) 0.2811(8) 0.2563(6) 0.147(6) Uani 1 1 d . . . C16 C 0.4897(10) 0.5560(6) 0.2747(4) 0.088(3) Uani 1 1 d . . . C17 C 0.4503(19) 0.5683(12) 0.3283(5) 0.134(8) Uani 0.67 1 d P . . C18 C 0.6232(15) 0.5118(11) 0.2792(10) 0.150(10) Uani 0.67 1 d P . . C19 C 0.522(2) 0.6280(9) 0.2478(7) 0.126(7) Uani 0.67 1 d P . . C20 C 0.1420(8) 0.7324(4) -0.0834(3) 0.060(2) Uani 1 1 d . . . H20 H 0.1049 0.7715 -0.0653 0.072 Uiso 1 1 calc R . . C21 C 0.0590(9) 0.7047(5) -0.1307(4) 0.069(2) Uani 1 1 d . . . H21 H -0.0332 0.7239 -0.1444 0.083 Uiso 1 1 calc R . . C22 C 0.1120(10) 0.6482(5) -0.1581(3) 0.071(2) Uani 1 1 d . . . H22 H 0.0573 0.6281 -0.1910 0.085 Uiso 1 1 calc R . . C23 C 0.2458(9) 0.6221(5) -0.1364(3) 0.069(2) Uani 1 1 d . . . H23 H 0.2855 0.5837 -0.1542 0.082 Uiso 1 1 calc R . . C24 C 0.3222(8) 0.6525(4) -0.0880(3) 0.058(2) Uani 1 1 d . . . H24 H 0.4139 0.6335 -0.0732 0.070 Uiso 1 1 calc R . . C25 C 0.6367(12) 0.8101(8) 0.1195(5) 0.115(4) Uani 1 1 d . . . C26 C 0.604(2) 0.787(3) 0.1721(8) 0.36(4) Uani 0.67 1 d P . . C27 C 0.7583(15) 0.7738(12) 0.1094(7) 0.138(9) Uani 0.67 1 d P . . C28 C 0.641(3) 0.8814(13) 0.1369(18) 0.29(3) Uani 0.67 1 d P . . C29 C 0.5200(14) 0.8549(7) -0.0739(6) 0.139(6) Uani 1 1 d . . . C30 C 0.6606(14) 0.8507(9) -0.0901(6) 0.152(6) Uani 1 1 d . . . C31 C 0.406(2) 0.8907(16) -0.0973(11) 0.33(2) Uani 1 1 d . . . C32 C 0.1968(13) 0.8665(6) 0.0481(4) 0.101(4) Uani 1 1 d . . . C33 C 0.243(4) 0.9346(12) 0.0484(19) 0.27(2) Uani 0.67 1 d P . . C34 C 0.057(4) 0.8965(19) 0.0107(9) 0.25(2) Uani 0.67 1 d P . . C35 C 0.150(2) 0.8335(8) 0.0942(7) 0.129(8) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0454(8) 0.0601(9) 0.0411(8) 0.0014(6) 0.0054(6) -0.0024(6) Ti2 0.0497(8) 0.0534(9) 0.0566(9) 0.0075(7) 0.0079(6) -0.0021(6) N1 0.038(3) 0.049(4) 0.040(3) 0.000(3) 0.004(2) 0.001(3) N2 0.040(3) 0.048(3) 0.044(3) 0.001(3) 0.003(3) 0.002(3) N3 0.044(3) 0.056(4) 0.046(3) 0.000(3) 0.009(3) 0.000(3) N4 0.051(4) 0.057(4) 0.054(4) 0.007(3) 0.013(3) 0.008(3) O1 0.046(3) 0.048(3) 0.047(3) 0.010(2) 0.005(2) 0.005(2) O2 0.047(3) 0.064(3) 0.056(3) 0.015(3) 0.017(2) 0.004(2) O3 0.045(3) 0.071(3) 0.055(3) -0.007(3) 0.013(2) -0.002(2) O4 0.070(3) 0.061(3) 0.053(3) 0.012(3) 0.007(3) -0.004(3) O5 0.053(3) 0.079(4) 0.047(3) -0.004(3) 0.000(2) -0.006(3) O6 0.059(3) 0.066(3) 0.071(4) 0.002(3) 0.003(3) -0.008(3) O7 0.075(4) 0.068(4) 0.075(4) 0.021(3) 0.014(3) -0.009(3) O8 0.068(3) 0.061(3) 0.064(3) 0.002(3) 0.007(3) 0.014(3) C1 0.043(4) 0.052(5) 0.034(4) -0.002(3) 0.000(3) -0.003(3) C2 0.038(4) 0.063(5) 0.040(4) -0.006(4) 0.007(3) -0.002(4) C3 0.037(4) 0.059(5) 0.057(4) -0.002(4) 0.007(3) 0.007(3) C4 0.034(4) 0.058(5) 0.046(4) 0.005(4) 0.006(3) 0.001(3) C5 0.047(4) 0.057(5) 0.057(5) 0.006(4) 0.009(4) -0.001(4) C6 0.058(5) 0.075(6) 0.050(5) -0.004(4) -0.003(4) -0.012(4) C7 0.065(6) 0.095(7) 0.047(5) -0.017(5) 0.004(4) -0.011(5) C8 0.060(5) 0.095(7) 0.066(5) -0.034(5) 0.021(5) -0.007(5) C9 0.042(4) 0.085(6) 0.064(5) -0.022(5) 0.015(4) -0.004(4) C10 0.094(7) 0.090(7) 0.079(7) -0.019(5) 0.024(6) 0.008(6) C11 0.142(12) 0.174(14) 0.172(14) 0.005(11) 0.025(10) 0.113(11) C12 0.146(11) 0.210(15) 0.072(8) -0.025(8) 0.050(8) 0.002(10) C13 0.100(8) 0.080(6) 0.076(6) 0.034(5) 0.004(6) -0.003(6) C14 0.106(9) 0.173(13) 0.148(12) 0.055(10) 0.016(9) 0.054(9) C15 0.134(11) 0.164(13) 0.133(11) 0.081(10) 0.004(9) -0.046(10) C16 0.083(7) 0.115(8) 0.061(6) -0.019(5) -0.002(5) -0.033(6) C17 0.120(13) 0.24(2) 0.042(8) -0.056(11) 0.016(8) -0.106(15) C18 0.039(8) 0.164(18) 0.22(2) -0.104(16) -0.050(11) 0.030(10) C19 0.174(18) 0.076(10) 0.113(13) -0.022(9) -0.009(12) -0.086(12) C20 0.061(5) 0.059(5) 0.058(5) 0.011(4) 0.008(4) 0.008(4) C21 0.056(5) 0.075(6) 0.070(6) 0.007(5) -0.003(4) 0.001(4) C22 0.080(6) 0.078(6) 0.050(5) 0.003(4) 0.004(4) -0.008(5) C23 0.063(5) 0.086(6) 0.059(5) -0.007(5) 0.018(4) -0.002(5) C24 0.053(5) 0.068(5) 0.055(5) 0.005(4) 0.014(4) 0.000(4) C25 0.089(8) 0.151(11) 0.089(8) -0.045(8) -0.020(6) -0.016(8) C26 0.055(11) 0.98(11) 0.041(11) 0.03(3) -0.002(9) 0.01(3) C27 0.051(9) 0.23(2) 0.114(13) -0.098(15) -0.025(9) 0.055(11) C28 0.24(3) 0.114(17) 0.41(5) -0.16(3) -0.23(3) 0.053(18) C29 0.128(10) 0.147(11) 0.165(12) 0.117(10) 0.088(9) 0.066(9) C30 0.104(9) 0.191(14) 0.179(14) 0.080(11) 0.071(10) 0.012(9) C31 0.188(18) 0.47(4) 0.38(3) 0.37(3) 0.17(2) 0.18(2) C32 0.147(10) 0.066(7) 0.092(7) -0.013(6) 0.024(7) 0.033(7) C33 0.28(4) 0.080(15) 0.53(6) -0.13(2) 0.27(4) -0.064(19) C34 0.30(3) 0.33(4) 0.119(17) -0.02(2) -0.010(19) 0.30(3) C35 0.24(2) 0.071(10) 0.118(13) 0.017(9) 0.134(15) 0.045(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.785(5) . ? Ti1 O4 1.807(5) . ? Ti1 O3 1.831(5) . ? Ti1 O1 2.118(5) . ? Ti1 N1 2.262(6) . ? Ti1 N3 2.294(6) . ? Ti1 C2 2.631(7) . ? Ti2 O7 1.779(5) . ? Ti2 O6 1.780(5) . ? Ti2 O8 1.815(5) . ? Ti2 O2 2.087(5) . ? Ti2 N2 2.323(6) . ? Ti2 N4 2.335(6) . ? Ti2 C4 2.631(7) . ? N1 C1 1.319(8) . ? N1 C2 1.379(8) . ? N2 C1 1.334(8) . ? N2 C4 1.373(8) . ? N3 C9 1.338(9) . ? N3 C5 1.353(9) . ? N4 C24 1.341(9) . ? N4 C20 1.353(9) . ? O1 C2 1.291(8) . ? O2 C4 1.274(8) . ? O3 C10 1.415(10) . ? O4 C13 1.416(10) . ? O5 C16 1.414(9) . ? O6 C25 1.413(11) . ? O7 C29 1.381(10) . ? O8 C32 1.401(10) . ? C2 C3 1.401(10) . ? C3 C4 1.395(10) . ? C5 C6 1.390(10) . ? C6 C7 1.376(11) . ? C7 C8 1.367(11) . ? C8 C9 1.381(10) . ? C10 C12 1.549(16) . ? C10 C11 1.556(16) . ? C13 C15 1.493(14) . ? C13 C14 1.512(15) . ? C16 C17 1.461(17) . ? C16 C18 1.501(17) . ? C16 C19 1.539(18) . ? C20 C21 1.374(11) . ? C21 C22 1.389(12) . ? C22 C23 1.375(11) . ? C23 C24 1.389(11) . ? C25 C28 1.38(2) . ? C25 C27 1.406(17) . ? C25 C26 1.46(3) . ? C29 C31 1.312(18) . ? C29 C30 1.478(16) . ? C32 C33 1.33(2) . ? C32 C35 1.435(17) . ? C32 C34 1.57(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ti1 O4 101.0(2) . . ? O5 Ti1 O3 99.7(2) . . ? O4 Ti1 O3 106.0(2) . . ? O5 Ti1 O1 94.0(2) . . ? O4 Ti1 O1 96.3(2) . . ? O3 Ti1 O1 150.8(2) . . ? O5 Ti1 N1 92.2(2) . . ? O4 Ti1 N1 154.4(2) . . ? O3 Ti1 N1 93.0(2) . . ? O1 Ti1 N1 60.65(18) . . ? O5 Ti1 N3 171.9(2) . . ? O4 Ti1 N3 84.1(2) . . ? O3 Ti1 N3 84.7(2) . . ? O1 Ti1 N3 79.12(19) . . ? N1 Ti1 N3 80.7(2) . . ? O5 Ti1 C2 94.3(2) . . ? O4 Ti1 C2 124.5(2) . . ? O3 Ti1 C2 123.5(2) . . ? O1 Ti1 C2 29.05(18) . . ? N1 Ti1 C2 31.6(2) . . ? N3 Ti1 C2 77.6(2) . . ? O7 Ti2 O6 102.1(3) . . ? O7 Ti2 O8 107.8(3) . . ? O6 Ti2 O8 97.8(3) . . ? O7 Ti2 O2 93.2(2) . . ? O6 Ti2 O2 94.5(2) . . ? O8 Ti2 O2 152.7(2) . . ? O7 Ti2 N2 152.2(2) . . ? O6 Ti2 N2 87.6(2) . . ? O8 Ti2 N2 96.4(2) . . ? O2 Ti2 N2 59.78(19) . . ? O7 Ti2 N4 85.3(2) . . ? O6 Ti2 N4 171.9(2) . . ? O8 Ti2 N4 82.9(2) . . ? O2 Ti2 N4 81.6(2) . . ? N2 Ti2 N4 84.3(2) . . ? O7 Ti2 C4 121.6(3) . . ? O6 Ti2 C4 89.7(2) . . ? O8 Ti2 C4 127.1(2) . . ? O2 Ti2 C4 28.46(18) . . ? N2 Ti2 C4 31.40(19) . . ? N4 Ti2 C4 83.5(2) . . ? C1 N1 C2 118.9(6) . . ? C1 N1 Ti1 152.0(5) . . ? C2 N1 Ti1 89.1(4) . . ? C1 N2 C4 118.3(6) . . ? C1 N2 Ti2 153.9(5) . . ? C4 N2 Ti2 86.8(4) . . ? C9 N3 C5 118.4(6) . . ? C9 N3 Ti1 118.8(5) . . ? C5 N3 Ti1 122.4(5) . . ? C24 N4 C20 116.2(7) . . ? C24 N4 Ti2 122.7(5) . . ? C20 N4 Ti2 120.9(5) . . ? C2 O1 Ti1 98.1(4) . . ? C4 O2 Ti2 100.2(4) . . ? C10 O3 Ti1 134.8(5) . . ? C13 O4 Ti1 139.5(5) . . ? C16 O5 Ti1 161.3(5) . . ? C25 O6 Ti2 155.1(7) . . ? C29 O7 Ti2 154.3(6) . . ? C32 O8 Ti2 138.8(6) . . ? N1 C1 N2 124.6(6) . . ? O1 C2 N1 112.1(6) . . ? O1 C2 C3 128.0(6) . . ? N1 C2 C3 120.0(7) . . ? O1 C2 Ti1 52.8(3) . . ? N1 C2 Ti1 59.3(3) . . ? C3 C2 Ti1 178.0(5) . . ? C4 C3 C2 117.6(7) . . ? O2 C4 N2 112.9(6) . . ? O2 C4 C3 126.4(6) . . ? N2 C4 C3 120.6(6) . . ? O2 C4 Ti2 51.3(3) . . ? N2 C4 Ti2 61.8(4) . . ? C3 C4 Ti2 173.2(5) . . ? N3 C5 C6 121.4(7) . . ? C7 C6 C5 119.6(8) . . ? C8 C7 C6 118.4(7) . . ? C7 C8 C9 120.1(8) . . ? N3 C9 C8 122.0(7) . . ? O3 C10 C12 105.5(9) . . ? O3 C10 C11 106.8(8) . . ? C12 C10 C11 114.8(11) . . ? O4 C13 C15 108.2(8) . . ? O4 C13 C14 110.0(8) . . ? C15 C13 C14 117.7(11) . . ? O5 C16 C17 110.4(9) . . ? O5 C16 C18 108.4(9) . . ? C17 C16 C18 112.5(15) . . ? O5 C16 C19 108.8(9) . . ? C17 C16 C19 111.4(13) . . ? C18 C16 C19 105.0(14) . . ? N4 C20 C21 123.8(8) . . ? C20 C21 C22 119.0(8) . . ? C23 C22 C21 118.2(8) . . ? C22 C23 C24 119.2(8) . . ? N4 C24 C23 123.5(7) . . ? C28 C25 C27 122(2) . . ? C28 C25 O6 109.7(13) . . ? C27 C25 O6 114.6(10) . . ? C28 C25 C26 90(3) . . ? C27 C25 C26 110(2) . . ? O6 C25 C26 106.4(13) . . ? C31 C29 O7 116.5(11) . . ? C31 C29 C30 129.3(11) . . ? O7 C29 C30 113.3(10) . . ? C33 C32 O8 117.7(16) . . ? C33 C32 C35 123(2) . . ? O8 C32 C35 113.2(9) . . ? C33 C32 C34 85(2) . . ? O8 C32 C34 105.0(10) . . ? C35 C32 C34 104.4(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.773 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.116 #===END data_tjb211s _database_code_CSD 218032 _chemical_name_common Ti2(DHP)(OBut)2(OPri)4(Py)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 N4 O8 Ti2' _chemical_formula_weight 734.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6835(12) _cell_length_b 16.271(2) _cell_length_c 27.414(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.913(3) _cell_angle_gamma 90.00 _cell_volume 4296.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.211 _exptl_crystal_size_mid 0.145 _exptl_crystal_size_min 0.122 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9172 _exptl_absorpt_correction_T_max 0.9509 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29779 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.78 _reflns_number_total 7348 _reflns_number_gt 4373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7348 _refine_ls_number_parameters 429 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.1823 _refine_ls_R_factor_gt 0.1251 _refine_ls_wR_factor_ref 0.3887 _refine_ls_wR_factor_gt 0.3545 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_restrained_S_all 1.345 _refine_ls_shift/su_max 0.203 _refine_ls_shift/su_mean 0.014 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.67064(15) 0.76433(9) 0.50207(5) 0.0450(5) Uani 1 1 d . . . Ti2 Ti 0.88426(15) 0.51368(10) 0.32099(5) 0.0471(5) Uani 1 1 d . . . N1 N 0.7318(6) 0.6747(4) 0.4450(2) 0.0429(16) Uani 1 1 d . . . N2 N 0.8005(6) 0.5866(4) 0.3833(2) 0.0392(15) Uani 1 1 d . . . N3 N 0.6170(7) 0.6441(4) 0.5409(2) 0.0469(17) Uani 1 1 d . . . N4 N 0.7949(7) 0.4015(4) 0.3612(3) 0.0532(18) Uani 1 1 d . . . O1 O 0.8685(5) 0.7080(3) 0.51132(18) 0.0485(14) Uani 1 1 d . . . O2 O 1.0040(6) 0.5256(4) 0.3887(2) 0.0543(15) Uani 1 1 d . . . O3 O 0.4877(6) 0.7627(4) 0.4787(2) 0.0579(16) Uani 1 1 d . . . O4 O 0.6821(6) 0.8082(3) 0.5631(2) 0.0565(16) Uani 1 1 d . . . O5 O 0.7297(6) 0.8467(3) 0.4676(2) 0.0532(15) Uani 1 1 d . . . O6 O 0.9427(6) 0.6098(4) 0.2991(2) 0.0621(17) Uani 1 1 d . . . O7 O 1.0006(6) 0.4419(4) 0.2980(2) 0.0668(18) Uani 1 1 d . . . O8 O 0.7223(6) 0.5085(3) 0.2825(2) 0.0568(16) Uani 1 1 d . . . C1 C 0.7094(8) 0.6374(5) 0.4012(3) 0.043(2) Uani 1 1 d . . . C2 C 0.8587(8) 0.6641(5) 0.4720(3) 0.0423(19) Uani 1 1 d . . . C3 C 0.9582(8) 0.6111(5) 0.4567(3) 0.048(2) Uani 1 1 d . . . C4 C 0.9234(8) 0.5732(5) 0.4109(3) 0.0414(19) Uani 1 1 d . . . C5 C 0.7086(10) 0.6133(6) 0.5762(3) 0.067(3) Uani 1 1 d . . . C6 C 0.6854(10) 0.5474(7) 0.6038(4) 0.078(3) Uani 1 1 d . . . C7 C 0.5553(12) 0.5060(7) 0.5962(5) 0.092(4) Uani 1 1 d . . . C8 C 0.4616(12) 0.5359(7) 0.5561(5) 0.092(4) Uani 1 1 d . . . C9 C 0.4960(10) 0.6056(6) 0.5301(3) 0.061(2) Uani 1 1 d . . . C10 C 0.8707(9) 0.3639(6) 0.3981(3) 0.058(2) Uani 1 1 d . . . C11 C 0.8277(11) 0.2915(6) 0.4217(4) 0.073(3) Uani 1 1 d . . . C12 C 0.6941(13) 0.2607(7) 0.4049(5) 0.090(4) Uani 1 1 d . . . C13 C 0.6157(12) 0.3010(7) 0.3669(4) 0.089(4) Uani 1 1 d . . . C14 C 0.6658(10) 0.3727(6) 0.3458(4) 0.071(3) Uani 1 1 d . . . C15 C 0.3905(11) 0.8009(7) 0.4455(4) 0.090(4) Uani 1 1 d D . . C16 C 0.4230(18) 0.8047(12) 0.3951(4) 0.137(8) Uani 0.78 1 d PD . . C17 C 0.2594(15) 0.7457(11) 0.4430(8) 0.173(11) Uani 0.78 1 d PD . . C18 C 0.352(2) 0.8783(9) 0.4656(6) 0.149(9) Uani 0.78 1 d PD . . C19 C 0.7225(15) 0.8772(8) 0.5941(5) 0.132(6) Uani 1 1 d D . . C20 C 0.8747(15) 0.8846(13) 0.5953(7) 0.160(10) Uani 0.78 1 d PD . . C21 C 0.656(3) 0.952(2) 0.5735(16) 0.41(3) Uiso 0.78 1 d PD . . C22 C 0.687(3) 0.869(2) 0.6455(9) 0.31(2) Uiso 0.78 1 d PD . . C23 C 0.8159(16) 0.8944(7) 0.4399(5) 0.125(5) Uani 1 1 d D . . C24 C 0.954(2) 0.9042(15) 0.4692(8) 0.198(11) Uiso 0.78 1 d PD . . C25 C 0.7537(16) 0.9761(7) 0.4296(6) 0.100(6) Uani 0.78 1 d PD . . C26 C 0.846(3) 0.8553(14) 0.3929(8) 0.206(12) Uiso 0.78 1 d PD . . C27 C 1.0400(12) 0.6731(7) 0.3010(5) 0.110(5) Uani 1 1 d D . . C28 C 1.023(2) 0.7409(15) 0.3360(8) 0.209(12) Uiso 0.78 1 d PD . . C29 C 1.1853(11) 0.6462(8) 0.3026(5) 0.081(4) Uani 0.78 1 d PD . . C30 C 1.006(3) 0.7158(16) 0.2513(7) 0.209(12) Uiso 0.78 1 d PD . . C31 C 1.0340(12) 0.3836(8) 0.2612(5) 0.108(4) Uani 1 1 d D . . C32 C 1.097(2) 0.4362(14) 0.2244(9) 0.200(12) Uiso 0.78 1 d PD . . C33 C 1.1359(18) 0.3245(12) 0.2808(8) 0.161(9) Uiso 0.78 1 d PD . . C34 C 0.9073(13) 0.3457(10) 0.2371(6) 0.110(6) Uani 0.78 1 d PD . . C35 C 0.6270(11) 0.5514(7) 0.2475(3) 0.093(4) Uani 1 1 d D . . C36 C 0.5544(19) 0.6168(10) 0.2720(6) 0.152(10) Uani 0.78 1 d PD . . C37 C 0.5168(17) 0.4865(11) 0.2277(6) 0.154(10) Uani 0.78 1 d PD . . C38 C 0.6987(15) 0.5810(10) 0.2047(4) 0.094(5) Uani 0.78 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0498(10) 0.0440(9) 0.0405(9) -0.0014(7) 0.0015(7) -0.0069(7) Ti2 0.0444(9) 0.0578(10) 0.0386(9) -0.0054(7) 0.0024(7) 0.0035(7) N1 0.034(4) 0.052(4) 0.042(4) -0.006(3) 0.001(3) 0.001(3) N2 0.032(3) 0.045(4) 0.039(4) -0.006(3) -0.002(3) -0.005(3) N3 0.047(4) 0.048(4) 0.048(4) 0.000(3) 0.013(3) -0.003(3) N4 0.058(5) 0.050(4) 0.050(4) -0.007(3) -0.004(3) 0.002(4) O1 0.050(3) 0.056(4) 0.038(3) -0.005(3) -0.001(2) -0.010(3) O2 0.050(4) 0.064(4) 0.048(3) -0.003(3) -0.001(3) 0.004(3) O3 0.048(4) 0.065(4) 0.059(4) 0.005(3) -0.001(3) 0.002(3) O4 0.068(4) 0.055(4) 0.045(3) -0.007(3) -0.005(3) -0.005(3) O5 0.063(4) 0.042(3) 0.054(3) 0.006(3) 0.007(3) -0.012(3) O6 0.065(4) 0.078(4) 0.045(3) 0.002(3) 0.010(3) -0.011(3) O7 0.069(4) 0.078(5) 0.055(4) -0.019(3) 0.014(3) 0.014(3) O8 0.057(4) 0.064(4) 0.046(3) -0.009(3) -0.011(3) 0.007(3) C1 0.052(5) 0.040(5) 0.038(4) -0.004(4) 0.002(4) -0.017(4) C2 0.045(5) 0.047(5) 0.034(4) 0.003(4) -0.001(4) -0.014(4) C3 0.050(5) 0.055(5) 0.038(5) 0.006(4) 0.003(4) -0.007(4) C4 0.039(4) 0.042(5) 0.043(5) -0.002(4) 0.005(4) -0.004(4) C5 0.058(6) 0.086(7) 0.058(6) 0.026(5) 0.005(5) 0.006(5) C6 0.059(6) 0.077(7) 0.101(8) 0.039(6) 0.019(6) 0.007(5) C7 0.068(8) 0.097(9) 0.112(10) 0.034(8) 0.014(7) -0.010(6) C8 0.069(7) 0.091(8) 0.116(10) 0.032(8) 0.012(7) -0.021(6) C9 0.063(6) 0.055(6) 0.067(6) -0.006(5) 0.016(5) -0.017(5) C10 0.062(6) 0.058(6) 0.052(5) -0.003(5) -0.005(5) 0.012(5) C11 0.074(7) 0.060(6) 0.080(7) -0.005(6) -0.010(6) 0.001(5) C12 0.106(10) 0.075(8) 0.085(8) 0.011(6) -0.011(7) -0.014(7) C13 0.088(8) 0.086(8) 0.089(8) 0.025(7) -0.016(7) -0.023(7) C14 0.063(6) 0.077(7) 0.070(7) -0.004(6) -0.006(5) -0.023(5) C15 0.079(8) 0.121(10) 0.067(7) 0.024(7) -0.012(6) 0.030(7) C16 0.155(17) 0.21(2) 0.041(8) 0.021(11) -0.005(9) 0.071(16) C17 0.057(10) 0.19(2) 0.25(3) 0.08(2) -0.078(14) -0.031(12) C18 0.20(2) 0.079(12) 0.149(18) -0.012(12) -0.064(15) 0.056(13) C19 0.191(16) 0.105(11) 0.091(10) -0.010(8) -0.032(10) -0.073(11) C20 0.086(12) 0.22(2) 0.18(2) -0.134(19) 0.016(12) -0.080(14) C23 0.210(17) 0.093(10) 0.073(8) 0.023(7) 0.016(10) -0.040(10) C25 0.134(14) 0.052(8) 0.126(14) 0.043(9) 0.067(11) 0.007(8) C27 0.113(11) 0.071(8) 0.153(13) -0.005(8) 0.052(10) -0.024(7) C29 0.041(7) 0.066(9) 0.133(13) 0.020(8) -0.004(7) 0.004(6) C31 0.113(10) 0.113(10) 0.097(9) -0.049(8) 0.006(8) 0.022(9) C34 0.077(11) 0.123(14) 0.123(14) -0.062(12) -0.026(10) -0.002(10) C35 0.087(8) 0.138(11) 0.054(6) 0.034(7) 0.006(6) 0.045(8) C36 0.22(2) 0.153(17) 0.075(11) 0.010(11) -0.018(12) 0.138(17) C37 0.118(15) 0.161(18) 0.159(18) 0.071(15) -0.098(14) -0.079(14) C38 0.096(11) 0.142(14) 0.046(7) 0.034(9) 0.012(7) -0.004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O5 1.768(5) . ? Ti1 O4 1.812(6) . ? Ti1 O3 1.821(6) . ? Ti1 O1 2.115(6) . ? Ti1 N1 2.263(6) . ? Ti1 N3 2.312(7) . ? Ti1 C2 2.640(9) . ? Ti2 O7 1.783(6) . ? Ti2 O6 1.788(6) . ? Ti2 O8 1.800(6) . ? Ti2 O2 2.094(6) . ? Ti2 N2 2.296(6) . ? Ti2 N4 2.344(7) . ? Ti2 C4 2.640(8) . ? N1 C1 1.341(9) . ? N1 C2 1.379(10) . ? N2 C1 1.339(9) . ? N2 C4 1.360(9) . ? N3 C9 1.335(10) . ? N3 C5 1.340(11) . ? N4 C10 1.334(10) . ? N4 C14 1.361(11) . ? O1 C2 1.289(9) . ? O2 C4 1.295(9) . ? O3 C15 1.387(11) . ? O4 C19 1.439(12) . ? O5 C23 1.418(13) . ? O6 C27 1.393(12) . ? O7 C31 1.444(12) . ? O8 C35 1.442(11) . ? C2 C3 1.388(11) . ? C3 C4 1.409(11) . ? C5 C6 1.345(13) . ? C6 C7 1.425(15) . ? C7 C8 1.437(16) . ? C8 C9 1.397(14) . ? C10 C11 1.426(13) . ? C11 C12 1.419(15) . ? C12 C13 1.389(15) . ? C13 C14 1.410(14) . ? C15 C18 1.440(12) . ? C15 C16 1.448(12) . ? C15 C17 1.550(13) . ? C16 C17 2.362(17) . ? C16 C18 2.433(16) . ? C17 C18 2.392(17) . ? C19 C21 1.463(15) . ? C19 C20 1.476(13) . ? C19 C22 1.489(15) . ? C20 C22 2.401(18) . ? C20 C21 2.406(18) . ? C21 C22 2.381(18) . ? C23 C25 1.476(12) . ? C23 C26 1.491(14) . ? C23 C24 1.493(14) . ? C24 C26 2.374(18) . ? C24 C25 2.422(17) . ? C25 C26 2.421(17) . ? C27 C29 1.470(12) . ? C27 C28 1.483(14) . ? C27 C30 1.532(14) . ? C28 C30 2.347(18) . ? C28 C29 2.445(16) . ? C29 C30 2.400(17) . ? C31 C33 1.441(13) . ? C31 C34 1.468(12) . ? C31 C32 1.498(14) . ? C32 C33 2.388(17) . ? C32 C34 2.407(17) . ? C33 C34 2.430(16) . ? C35 C36 1.474(13) . ? C35 C38 1.501(12) . ? C35 C37 1.559(14) . ? C36 C37 2.45(2) . ? C36 C38 2.494(18) . ? C37 C38 2.468(18) . ? 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 O5 Ti1 O4 101.7(3) . . ? O5 Ti1 O3 100.3(3) . . ? O4 Ti1 O3 107.2(3) . . ? O5 Ti1 O1 93.1(2) . . ? O4 Ti1 O1 95.2(2) . . ? O3 Ti1 O1 150.7(2) . . ? O5 Ti1 N1 89.8(2) . . ? O4 Ti1 N1 153.8(3) . . ? O3 Ti1 N1 93.5(3) . . ? O1 Ti1 N1 60.4(2) . . ? O5 Ti1 N3 171.1(3) . . ? O4 Ti1 N3 84.4(3) . . ? O3 Ti1 N3 83.9(3) . . ? O1 Ti1 N3 79.7(2) . . ? N1 Ti1 N3 82.0(2) . . ? O5 Ti1 C2 91.7(3) . . ? O4 Ti1 C2 123.6(3) . . ? O3 Ti1 C2 123.9(3) . . ? O1 Ti1 C2 28.9(2) . . ? N1 Ti1 C2 31.5(2) . . ? N3 Ti1 C2 79.4(2) . . ? O7 Ti2 O6 102.8(3) . . ? O7 Ti2 O8 107.8(3) . . ? O6 Ti2 O8 97.6(3) . . ? O7 Ti2 O2 93.6(3) . . ? O6 Ti2 O2 92.9(3) . . ? O8 Ti2 O2 153.3(3) . . ? O7 Ti2 N2 152.5(3) . . ? O6 Ti2 N2 86.9(2) . . ? O8 Ti2 N2 96.2(2) . . ? O2 Ti2 N2 59.9(2) . . ? O7 Ti2 N4 86.2(3) . . ? O6 Ti2 N4 169.7(3) . . ? O8 Ti2 N4 84.1(3) . . ? O2 Ti2 N4 81.5(2) . . ? N2 Ti2 N4 82.9(2) . . ? O7 Ti2 C4 122.4(3) . . ? O6 Ti2 C4 88.4(3) . . ? O8 Ti2 C4 126.7(3) . . ? O2 Ti2 C4 28.9(2) . . ? N2 Ti2 C4 31.0(2) . . ? N4 Ti2 C4 82.6(2) . . ? C1 N1 C2 118.5(7) . . ? C1 N1 Ti1 151.7(6) . . ? C2 N1 Ti1 89.5(5) . . ? C1 N2 C4 117.9(6) . . ? C1 N2 Ti2 152.6(5) . . ? C4 N2 Ti2 88.6(4) . . ? C9 N3 C5 119.0(8) . . ? C9 N3 Ti1 121.9(6) . . ? C5 N3 Ti1 119.1(6) . . ? C10 N4 C14 119.6(8) . . ? C10 N4 Ti2 120.8(6) . . ? C14 N4 Ti2 119.6(6) . . ? C2 O1 Ti1 98.8(5) . . ? C4 O2 Ti2 99.6(5) . . ? C15 O3 Ti1 142.6(6) . . ? C19 O4 Ti1 147.2(7) . . ? C23 O5 Ti1 160.5(7) . . ? C27 O6 Ti2 150.6(7) . . ? C31 O7 Ti2 150.7(6) . . ? C35 O8 Ti2 145.8(6) . . ? N2 C1 N1 123.7(7) . . ? O1 C2 N1 111.4(7) . . ? O1 C2 C3 127.0(7) . . ? N1 C2 C3 121.6(7) . . ? O1 C2 Ti1 52.4(4) . . ? N1 C2 Ti1 59.0(4) . . ? C3 C2 Ti1 179.3(6) . . ? C2 C3 C4 115.5(7) . . ? O2 C4 N2 111.7(7) . . ? O2 C4 C3 125.5(7) . . ? N2 C4 C3 122.7(7) . . ? O2 C4 Ti2 51.5(4) . . ? N2 C4 Ti2 60.4(4) . . ? C3 C4 Ti2 172.6(6) . . ? N3 C5 C6 124.6(9) . . ? C5 C6 C7 119.4(10) . . ? C6 C7 C8 115.5(10) . . ? C9 C8 C7 120.0(10) . . ? N3 C9 C8 121.1(9) . . ? N4 C10 C11 124.0(8) . . ? C12 C11 C10 116.3(9) . . ? C13 C12 C11 119.1(10) . . ? C12 C13 C14 120.9(10) . . ? N4 C14 C13 120.1(9) . . ? O3 C15 C18 109.1(10) . . ? O3 C15 C16 116.4(10) . . ? C18 C15 C16 114.7(10) . . ? O3 C15 C17 105.4(10) . . ? C18 C15 C17 106.1(10) . . ? C16 C15 C17 103.9(10) . . ? C15 C16 C17 39.6(6) . . ? C15 C16 C18 32.5(6) . . ? C17 C16 C18 59.8(4) . . ? C15 C17 C16 36.5(5) . . ? C15 C17 C18 35.3(5) . . ? C16 C17 C18 61.6(5) . . ? C15 C18 C17 38.5(6) . . ? C15 C18 C16 32.7(6) . . ? C17 C18 C16 58.6(4) . . ? O4 C19 C21 110(2) . . ? O4 C19 C20 106.6(12) . . ? C21 C19 C20 109.9(13) . . ? O4 C19 C22 114.7(19) . . ? C21 C19 C22 107.5(13) . . ? C20 C19 C22 108.2(12) . . ? C19 C20 C22 36.1(7) . . ? C19 C20 C21 34.9(7) . . ? C22 C20 C21 59.4(5) . . ? C19 C21 C22 36.6(7) . . ? C19 C21 C20 35.2(7) . . ? C22 C21 C20 60.2(5) . . ? C19 C22 C21 35.9(7) . . ? C19 C22 C20 35.7(7) . . ? C21 C22 C20 60.4(5) . . ? O5 C23 C25 110.2(11) . . ? O5 C23 C26 114.1(15) . . ? C25 C23 C26 109.4(11) . . ? O5 C23 C24 108.2(14) . . ? C25 C23 C24 109.4(11) . . ? C26 C23 C24 105.4(11) . . ? C23 C24 C26 37.3(6) . . ? C23 C24 C25 35.1(6) . . ? C26 C24 C25 60.6(5) . . ? C23 C25 C26 35.5(6) . . ? C23 C25 C24 35.5(6) . . ? C26 C25 C24 58.7(5) . . ? C23 C26 C24 37.3(6) . . ? C23 C26 C25 35.1(6) . . ? C24 C26 C25 60.7(5) . . ? O6 C27 C29 115.0(10) . . ? O6 C27 C28 116.9(14) . . ? C29 C27 C28 111.8(11) . . ? O6 C27 C30 102.8(16) . . ? C29 C27 C30 106.1(10) . . ? C28 C27 C30 102.2(11) . . ? C27 C28 C30 39.7(6) . . ? C27 C28 C29 33.9(6) . . ? C30 C28 C29 60.1(5) . . ? C27 C29 C30 37.8(6) . . ? C27 C29 C28 34.3(6) . . ? C30 C29 C28 57.9(4) . . ? C27 C30 C28 38.2(6) . . ? C27 C30 C29 36.0(6) . . ? C28 C30 C29 62.0(5) . . ? C33 C31 O7 111.8(14) . . ? C33 C31 C34 113.3(11) . . ? O7 C31 C34 110.6(10) . . ? C33 C31 C32 108.7(11) . . ? O7 C31 C32 103.4(15) . . ? C34 C31 C32 108.5(11) . . ? C31 C32 C33 34.9(6) . . ? C31 C32 C34 35.3(6) . . ? C33 C32 C34 60.9(5) . . ? C31 C33 C32 36.5(6) . . ? C31 C33 C34 33.7(6) . . ? C32 C33 C34 59.9(5) . . ? C31 C34 C32 36.2(6) . . ? C31 C34 C33 33.0(6) . . ? C32 C34 C33 59.2(4) . . ? O8 C35 C36 110.4(9) . . ? O8 C35 C38 111.1(9) . . ? C36 C35 C38 113.9(10) . . ? O8 C35 C37 105.8(10) . . ? C36 C35 C37 107.8(10) . . ? C38 C35 C37 107.5(9) . . ? C35 C36 C37 37.3(6) . . ? C35 C36 C38 33.4(5) . . ? C37 C36 C38 59.9(4) . . ? C35 C37 C36 35.0(5) . . ? C35 C37 C38 35.4(5) . . ? C36 C37 C38 60.9(4) . . ? C35 C38 C37 37.0(5) . . ? C35 C38 C36 32.7(5) . . ? C37 C38 C36 59.2(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.422 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.133 #===END data_tjb131s _database_code_CSD 218033 _chemical_name_common Zr2(DHP)(ONep)6(Py)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 N4 O8 Zr2' _chemical_formula_weight 889.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.757(13) _cell_length_b 9.969(7) _cell_length_c 28.15(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.761(15) _cell_angle_gamma 90.00 _cell_volume 4701(6) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max .075 _exptl_crystal_size_mid ? _exptl_crystal_size_min .195 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9105 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details 'SADABS ver 2.03, Sheldrick (1999).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37427 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.47 _reflns_number_total 9679 _reflns_number_gt 6109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+3.8264P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9679 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.277 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.25718(3) 0.68405(5) 0.011595(18) 0.04237(15) Uani 1 1 d . . . Zr2 Zr -0.00502(3) 0.93586(4) 0.183550(17) 0.03948(14) Uani 1 1 d . . . N1 N 0.1621(2) 0.7649(3) 0.06606(13) 0.0360(9) Uani 1 1 d . . . N2 N 0.0714(2) 0.8430(3) 0.12118(13) 0.0377(9) Uani 1 1 d . . . N3 N 0.1337(2) 0.6133(4) -0.03036(14) 0.0447(10) Uani 1 1 d . . . N4 N -0.1152(2) 0.8432(4) 0.13582(15) 0.0528(11) Uani 1 1 d . . . O1 O 0.19275(18) 0.8781(3) 0.00107(11) 0.0425(8) Uani 1 1 d . . . O2 O 0.00892(18) 1.0385(3) 0.11377(12) 0.0445(8) Uani 1 1 d . . . O3 O 0.25560(18) 0.5006(3) 0.03550(11) 0.0439(8) Uani 1 1 d . . . O4 O 0.3043(2) 0.6790(4) -0.04953(13) 0.0651(11) Uani 1 1 d . . . O5 O 0.34291(19) 0.7594(3) 0.04948(14) 0.0569(9) Uani 1 1 d . . . O6 O -0.0835(2) 1.0532(3) 0.20916(12) 0.0535(9) Uani 1 1 d . . . O7 O 0.09134(18) 1.0135(3) 0.20895(12) 0.0487(8) Uani 1 1 d . . . O8 O -0.00915(18) 0.7702(3) 0.21933(12) 0.0444(8) Uani 1 1 d . . . C1 C 0.1498(3) 0.8778(4) 0.03861(16) 0.0360(10) Uani 1 1 d . . . C2 C 0.0961(3) 0.9755(4) 0.05182(16) 0.0382(11) Uani 1 1 d . . . H2 H 0.0858 1.0523 0.0326 0.046 Uiso 1 1 calc R . . C3 C 0.0581(3) 0.9560(4) 0.09446(17) 0.0376(11) Uani 1 1 d . . . C4 C 0.1234(3) 0.7551(4) 0.10567(16) 0.0366(10) Uani 1 1 d . . . H4 H 0.1337 0.6783 0.1248 0.044 Uiso 1 1 calc R . . C5 C 0.2855(3) 0.3976(5) 0.06521(19) 0.0517(13) Uani 1 1 d . . . C6 C 0.2322(4) 0.2753(5) 0.0594(2) 0.0660(16) Uani 1 1 d . . . H6A H 0.1777 0.2984 0.0682 0.099 Uiso 1 1 calc R . . H6B H 0.2525 0.2031 0.0801 0.099 Uiso 1 1 calc R . . H6C H 0.2319 0.2452 0.0263 0.099 Uiso 1 1 calc R . . C7 C 0.3683(4) 0.3657(8) 0.0498(4) 0.122(3) Uani 1 1 d . . . H7A H 0.3661 0.3350 0.0167 0.182 Uiso 1 1 calc R . . H7B H 0.3912 0.2950 0.0702 0.182 Uiso 1 1 calc R . . H7C H 0.4016 0.4464 0.0525 0.182 Uiso 1 1 calc R . . C8 C 0.2838(6) 0.4472(7) 0.1158(2) 0.110(3) Uani 1 1 d . . . H8A H 0.3157 0.5293 0.1189 0.165 Uiso 1 1 calc R . . H8B H 0.3062 0.3783 0.1372 0.165 Uiso 1 1 calc R . . H8C H 0.2286 0.4660 0.1241 0.165 Uiso 1 1 calc R . . C9 C 0.3544(3) 0.6913(6) -0.08772(18) 0.0521(13) Uani 1 1 d . . . C10 C 0.3104(6) 0.6712(12) -0.1326(3) 0.175(5) Uani 1 1 d . . . H10A H 0.2723 0.5974 -0.1292 0.263 Uiso 1 1 calc R . . H10B H 0.3478 0.6490 -0.1575 0.263 Uiso 1 1 calc R . . H10C H 0.2815 0.7534 -0.1412 0.263 Uiso 1 1 calc R . . C11 C 0.4107(5) 0.5740(11) -0.0832(4) 0.164(5) Uani 1 1 d . . . H11A H 0.4446 0.5844 -0.0544 0.246 Uiso 1 1 calc R . . H11B H 0.4443 0.5706 -0.1111 0.246 Uiso 1 1 calc R . . H11C H 0.3799 0.4908 -0.0812 0.246 Uiso 1 1 calc R . . C12 C 0.3948(8) 0.8181(10) -0.0869(3) 0.219(8) Uani 1 1 d . . . H12A H 0.3559 0.8903 -0.0921 0.328 Uiso 1 1 calc R . . H12B H 0.4339 0.8202 -0.1120 0.328 Uiso 1 1 calc R . . H12C H 0.4223 0.8303 -0.0559 0.328 Uiso 1 1 calc R . . C13 C 0.4015(3) 0.8376(6) 0.0739(2) 0.0623(15) Uani 1 1 d . . . C14 C 0.3972(5) 0.9738(7) 0.0532(4) 0.158(5) Uani 1 1 d . . . H14A H 0.3757 0.9686 0.0205 0.237 Uiso 1 1 calc R . . H14B H 0.4508 1.0132 0.0532 0.237 Uiso 1 1 calc R . . H14C H 0.3622 1.0300 0.0721 0.237 Uiso 1 1 calc R . . C15 C 0.4807(4) 0.7821(9) 0.0640(4) 0.152(4) Uani 1 1 d . . . H15A H 0.4857 0.6923 0.0780 0.228 Uiso 1 1 calc R . . H15B H 0.5222 0.8406 0.0779 0.228 Uiso 1 1 calc R . . H15C H 0.4870 0.7763 0.0296 0.228 Uiso 1 1 calc R . . C16 C 0.3843(8) 0.8346(15) 0.1249(3) 0.227(8) Uani 1 1 d . . . H16A H 0.3311 0.8717 0.1297 0.340 Uiso 1 1 calc R . . H16B H 0.4242 0.8882 0.1425 0.340 Uiso 1 1 calc R . . H16C H 0.3863 0.7417 0.1363 0.340 Uiso 1 1 calc R . . C17 C 0.0918(3) 0.6951(5) -0.05899(19) 0.0550(14) Uani 1 1 d . . . C18 C 0.0259(4) 0.6570(6) -0.0859(2) 0.0758(19) Uani 1 1 d . . . C19 C -0.0156(9) 0.5315(14) -0.0729(6) 0.062(4) Uani 0.50 1 d P . . C19' C 0.0209(10) 0.5176(17) -0.0929(6) 0.067(4) Uani 0.50 1 d P . . C20 C 0.0219(7) 0.4482(11) -0.0415(4) 0.051(3) Uani 0.50 1 d P . . C20' C 0.0657(7) 0.4304(11) -0.0653(5) 0.056(3) Uani 0.50 1 d P . . C21 C 0.0949(8) 0.4863(15) -0.0188(5) 0.050(4) Uani 0.50 1 d P . . C21' C 0.1251(8) 0.4846(13) -0.0356(5) 0.043(3) Uani 0.50 1 d P . . C22 C -0.1505(3) 0.9115(6) 0.0997(2) 0.0597(15) Uani 1 1 d . . . C23 C -0.2182(4) 0.8689(8) 0.0746(2) 0.085(2) Uani 1 1 d . . . C24 C -0.2639(9) 0.7845(15) 0.0934(5) 0.064(4) Uani 0.50 1 d P . . C24' C -0.2347(9) 0.7107(18) 0.0817(5) 0.070(4) Uani 0.50 1 d P . . C25 C -0.2346(7) 0.7163(12) 0.1343(4) 0.058(3) Uani 0.50 1 d P . . C25' C -0.1894(8) 0.6361(14) 0.1149(5) 0.075(4) Uani 0.50 1 d P . . C26 C -0.1599(7) 0.7564(12) 0.1530(4) 0.046(3) Uani 0.50 1 d P . . C26' C -0.1271(8) 0.6936(12) 0.1426(5) 0.058(3) Uani 0.50 1 d P . . C27 C -0.1284(3) 1.1415(6) 0.2357(2) 0.0605(15) Uani 1 1 d . . . C28 C -0.1295(5) 1.2728(7) 0.2076(3) 0.120(3) Uani 1 1 d . . . H28A H -0.0748 1.3060 0.2049 0.181 Uiso 1 1 calc R . . H28B H -0.1615 1.3395 0.2241 0.181 Uiso 1 1 calc R . . H28C H -0.1529 1.2570 0.1758 0.181 Uiso 1 1 calc R . . C29 C -0.2111(4) 1.0865(9) 0.2397(3) 0.106(3) Uani 1 1 d . . . H29A H -0.2316 1.0591 0.2082 0.158 Uiso 1 1 calc R . . H29B H -0.2460 1.1558 0.2525 0.158 Uiso 1 1 calc R . . H29C H -0.2099 1.0088 0.2610 0.158 Uiso 1 1 calc R . . C30 C -0.0875(5) 1.1638(9) 0.2833(2) 0.116(3) Uani 1 1 d . . . H30A H -0.0846 1.0788 0.3007 0.173 Uiso 1 1 calc R . . H30B H -0.1178 1.2293 0.3014 0.173 Uiso 1 1 calc R . . H30C H -0.0334 1.1978 0.2787 0.173 Uiso 1 1 calc R . . C31 C 0.1596(3) 1.0932(5) 0.21641(19) 0.0511(13) Uani 1 1 d . . . C32 C 0.1402(5) 1.2307(7) 0.1971(3) 0.127(3) Uani 1 1 d . . . H32A H 0.1222 1.2233 0.1638 0.190 Uiso 1 1 calc R . . H32B H 0.1881 1.2872 0.1994 0.190 Uiso 1 1 calc R . . H32C H 0.0979 1.2710 0.2157 0.190 Uiso 1 1 calc R . . C33 C 0.1799(5) 1.1018(9) 0.2674(2) 0.115(3) Uani 1 1 d . . . H33A H 0.1328 1.1301 0.2846 0.173 Uiso 1 1 calc R . . H33B H 0.2229 1.1673 0.2727 0.173 Uiso 1 1 calc R . . H33C H 0.1976 1.0137 0.2791 0.173 Uiso 1 1 calc R . . C34 C 0.2255(4) 1.0388(9) 0.1874(3) 0.117(3) Uani 1 1 d . . . H34A H 0.2415 0.9503 0.1995 0.176 Uiso 1 1 calc R . . H34B H 0.2713 1.0998 0.1894 0.176 Uiso 1 1 calc R . . H34C H 0.2069 1.0306 0.1541 0.176 Uiso 1 1 calc R . . C35 C 0.0154(3) 0.6752(5) 0.25365(17) 0.0437(11) Uani 1 1 d . . . C36 C -0.0583(4) 0.6032(6) 0.2712(2) 0.0801(19) Uani 1 1 d . . . H36A H -0.0954 0.6690 0.2840 0.120 Uiso 1 1 calc R . . H36B H -0.0423 0.5392 0.2961 0.120 Uiso 1 1 calc R . . H36C H -0.0845 0.5551 0.2447 0.120 Uiso 1 1 calc R . . C37 C 0.0707(4) 0.5757(7) 0.2305(2) 0.086(2) Uani 1 1 d . . . H37A H 0.0436 0.5365 0.2024 0.129 Uiso 1 1 calc R . . H37B H 0.0849 0.5043 0.2532 0.129 Uiso 1 1 calc R . . H37C H 0.1193 0.6219 0.2209 0.129 Uiso 1 1 calc R . . C38 C 0.0582(4) 0.7447(6) 0.2946(2) 0.0749(18) Uani 1 1 d . . . H38A H 0.1061 0.7894 0.2833 0.112 Uiso 1 1 calc R . . H38B H 0.0736 0.6784 0.3189 0.112 Uiso 1 1 calc R . . H38C H 0.0227 0.8114 0.3083 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0378(3) 0.0388(3) 0.0511(3) 0.0100(2) 0.0104(2) 0.0016(2) Zr2 0.0364(3) 0.0337(2) 0.0484(3) -0.0050(2) 0.0024(2) -0.0006(2) N1 0.037(2) 0.031(2) 0.040(2) 0.0056(17) 0.0025(18) -0.0027(16) N2 0.036(2) 0.031(2) 0.046(2) -0.0002(17) 0.0008(17) -0.0025(16) N3 0.053(3) 0.035(2) 0.046(2) -0.0025(19) -0.001(2) 0.0000(19) N4 0.050(3) 0.062(3) 0.046(3) -0.003(2) 0.010(2) -0.019(2) O1 0.0432(18) 0.0346(17) 0.050(2) 0.0086(15) 0.0064(16) -0.0006(14) O2 0.0443(19) 0.0333(17) 0.056(2) 0.0006(15) 0.0030(16) 0.0074(14) O3 0.0437(18) 0.0381(18) 0.050(2) 0.0107(16) 0.0017(15) 0.0039(15) O4 0.055(2) 0.074(3) 0.069(3) 0.023(2) 0.0343(19) 0.0156(19) O5 0.044(2) 0.044(2) 0.083(3) 0.0097(19) 0.0018(19) -0.0041(16) O6 0.053(2) 0.047(2) 0.061(2) -0.0089(17) 0.0077(17) 0.0107(17) O7 0.0440(19) 0.0422(19) 0.060(2) -0.0028(16) -0.0004(16) -0.0121(15) O8 0.0385(18) 0.0379(18) 0.057(2) 0.0031(15) 0.0023(15) -0.0041(14) C1 0.032(2) 0.031(2) 0.044(3) 0.001(2) 0.000(2) -0.0072(19) C2 0.040(3) 0.029(2) 0.045(3) 0.004(2) -0.004(2) -0.0005(19) C3 0.035(2) 0.025(2) 0.053(3) 0.000(2) -0.005(2) -0.0024(19) C4 0.039(3) 0.026(2) 0.045(3) 0.003(2) -0.002(2) -0.0033(19) C5 0.060(3) 0.037(3) 0.058(3) 0.006(2) -0.006(3) 0.003(2) C6 0.091(4) 0.042(3) 0.066(4) 0.013(3) 0.003(3) 0.000(3) C7 0.053(4) 0.089(5) 0.223(10) 0.055(6) 0.012(5) 0.020(4) C8 0.198(9) 0.063(4) 0.065(5) 0.011(4) -0.047(5) -0.012(5) C9 0.047(3) 0.063(3) 0.047(3) -0.001(3) 0.008(2) -0.004(3) C10 0.188(10) 0.261(13) 0.074(6) 0.039(7) -0.044(6) -0.131(10) C11 0.108(7) 0.219(12) 0.168(10) 0.047(8) 0.072(7) 0.068(8) C12 0.357(17) 0.179(10) 0.129(8) -0.078(7) 0.141(10) -0.200(12) C13 0.049(3) 0.058(4) 0.080(4) -0.012(3) 0.001(3) -0.005(3) C14 0.134(8) 0.060(5) 0.275(14) 0.012(7) -0.075(8) -0.033(5) C15 0.060(5) 0.149(8) 0.244(12) -0.098(8) -0.048(6) 0.014(5) C16 0.248(14) 0.349(19) 0.087(7) -0.073(10) 0.047(8) -0.171(14) C17 0.058(3) 0.053(3) 0.053(3) 0.010(3) -0.007(3) 0.003(3) C18 0.097(5) 0.053(4) 0.074(4) 0.011(3) -0.039(4) -0.004(3) C19 0.068(10) 0.043(7) 0.073(11) -0.009(7) -0.023(8) -0.005(7) C19' 0.070(11) 0.068(10) 0.063(10) 0.002(8) -0.011(7) -0.012(8) C20 0.045(7) 0.045(6) 0.064(8) -0.006(6) -0.006(6) -0.003(5) C20' 0.055(7) 0.037(6) 0.075(9) -0.003(6) -0.018(7) 0.000(6) C21 0.050(9) 0.052(7) 0.050(9) -0.003(6) 0.017(6) -0.020(6) C21' 0.053(9) 0.039(6) 0.039(8) 0.004(6) -0.001(6) -0.013(6) C22 0.051(3) 0.065(4) 0.063(4) -0.007(3) -0.009(3) 0.006(3) C23 0.056(4) 0.121(6) 0.076(5) -0.006(4) -0.003(3) -0.026(4) C24 0.064(9) 0.069(9) 0.059(9) 0.004(7) -0.001(7) -0.016(7) C24' 0.056(9) 0.102(12) 0.051(8) -0.012(8) -0.008(7) -0.021(8) C25 0.066(8) 0.059(7) 0.049(7) 0.006(6) -0.003(6) -0.027(6) C25' 0.075(9) 0.086(10) 0.065(9) -0.014(8) 0.005(8) -0.039(8) C26 0.056(8) 0.040(7) 0.041(6) 0.006(5) -0.006(5) -0.010(6) C26' 0.065(8) 0.036(7) 0.074(9) -0.008(6) 0.002(7) -0.015(6) C27 0.047(3) 0.066(4) 0.069(4) -0.023(3) 0.005(3) 0.007(3) C28 0.092(6) 0.063(5) 0.205(10) -0.008(6) -0.014(6) 0.018(4) C29 0.057(4) 0.153(7) 0.108(6) -0.041(5) 0.027(4) -0.017(4) C30 0.101(6) 0.186(9) 0.060(4) -0.050(5) 0.004(4) 0.009(6) C31 0.046(3) 0.047(3) 0.060(3) -0.005(3) -0.007(3) -0.008(2) C32 0.111(6) 0.080(5) 0.187(9) 0.036(6) -0.039(6) -0.051(5) C33 0.104(6) 0.178(8) 0.063(5) -0.014(5) -0.012(4) -0.075(6) C34 0.056(4) 0.170(8) 0.126(7) -0.050(6) 0.014(4) -0.022(5) C35 0.043(3) 0.042(3) 0.047(3) -0.002(2) 0.006(2) 0.005(2) C36 0.078(4) 0.080(4) 0.083(5) 0.021(4) 0.010(4) -0.022(4) C37 0.094(5) 0.089(5) 0.074(4) -0.003(4) 0.004(4) 0.048(4) C38 0.096(5) 0.068(4) 0.060(4) 0.001(3) -0.021(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O4 1.916(4) . ? Zr1 O5 1.916(4) . ? Zr1 O3 1.949(3) . ? Zr1 O1 2.231(3) . ? Zr1 N1 2.385(4) . ? Zr1 N3 2.454(4) . ? Zr1 C1 2.763(5) . ? Zr2 O7 1.910(3) . ? Zr2 O6 1.917(3) . ? Zr2 O8 1.937(3) . ? Zr2 O2 2.233(3) . ? Zr2 N2 2.391(4) . ? Zr2 N4 2.431(4) . ? Zr2 C3 2.759(5) . ? N1 C4 1.310(5) . ? N1 C1 1.377(5) . ? N2 C4 1.320(5) . ? N2 C3 1.369(5) . ? N3 C21' 1.299(14) . ? N3 C17 1.332(6) . ? N3 C21 1.464(14) . ? N4 C26 1.252(11) . ? N4 C22 1.346(7) . ? N4 C26' 1.518(12) . ? O1 C1 1.297(5) . ? O2 C3 1.296(5) . ? O3 C5 1.406(6) . ? O4 C9 1.390(6) . ? O5 C13 1.415(6) . ? O6 C27 1.391(6) . ? O7 C31 1.403(5) . ? O8 C35 1.405(5) . ? C1 C2 1.384(6) . ? C2 C3 1.390(6) . ? C5 C7 1.501(8) . ? C5 C8 1.507(8) . ? C5 C6 1.518(7) . ? C9 C12 1.433(9) . ? C9 C10 1.456(9) . ? C9 C11 1.505(10) . ? C13 C15 1.473(9) . ? C13 C16 1.473(10) . ? C13 C14 1.478(9) . ? C17 C18 1.374(8) . ? C18 C19' 1.405(17) . ? C18 C19 1.483(16) . ? C19 C20 1.354(18) . ? C19' C20' 1.375(19) . ? C20 C21 1.414(18) . ? C20' C21' 1.389(17) . ? C22 C23 1.384(8) . ? C23 C24 1.266(14) . ? C23 C24' 1.615(18) . ? C24 C25 1.412(17) . ? C24' C25' 1.40(2) . ? C25 C26 1.402(15) . ? C25' C26' 1.405(17) . ? C27 C29 1.498(8) . ? C27 C30 1.503(8) . ? C27 C28 1.528(9) . ? C31 C33 1.469(8) . ? C31 C34 1.496(8) . ? C31 C32 1.506(8) . ? C35 C38 1.508(7) . ? C35 C37 1.518(7) . ? C35 C36 1.524(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 O4 Zr1 O5 100.81(17) . . ? O4 Zr1 O3 107.21(15) . . ? O5 Zr1 O3 101.15(14) . . ? O4 Zr1 O1 96.59(14) . . ? O5 Zr1 O1 94.91(14) . . ? O3 Zr1 O1 147.98(12) . . ? O4 Zr1 N1 152.64(14) . . ? O5 Zr1 N1 90.80(15) . . ? O3 Zr1 N1 94.51(13) . . ? O1 Zr1 N1 57.47(12) . . ? O4 Zr1 N3 85.69(16) . . ? O5 Zr1 N3 170.81(14) . . ? O3 Zr1 N3 82.89(13) . . ? O1 Zr1 N3 77.76(13) . . ? N1 Zr1 N3 80.60(14) . . ? O4 Zr1 C1 123.75(14) . . ? O5 Zr1 C1 93.23(14) . . ? O3 Zr1 C1 123.03(13) . . ? O1 Zr1 C1 27.56(12) . . ? N1 Zr1 C1 29.91(12) . . ? N3 Zr1 C1 77.70(13) . . ? O7 Zr2 O6 101.18(15) . . ? O7 Zr2 O8 101.21(14) . . ? O6 Zr2 O8 106.77(15) . . ? O7 Zr2 O2 91.92(13) . . ? O6 Zr2 O2 98.22(14) . . ? O8 Zr2 O2 148.69(13) . . ? O7 Zr2 N2 88.06(14) . . ? O6 Zr2 N2 154.33(14) . . ? O8 Zr2 N2 94.61(13) . . ? O2 Zr2 N2 57.22(12) . . ? O7 Zr2 N4 168.40(14) . . ? O6 Zr2 N4 85.50(15) . . ? O8 Zr2 N4 85.69(15) . . ? O2 Zr2 N4 77.65(14) . . ? N2 Zr2 N4 82.05(14) . . ? O7 Zr2 C3 88.13(14) . . ? O6 Zr2 C3 125.75(14) . . ? O8 Zr2 C3 123.75(13) . . ? O2 Zr2 C3 27.60(11) . . ? N2 Zr2 C3 29.74(12) . . ? N4 Zr2 C3 80.28(14) . . ? C4 N1 C1 118.0(4) . . ? C4 N1 Zr1 151.6(3) . . ? C1 N1 Zr1 90.4(3) . . ? C4 N2 C3 117.5(4) . . ? C4 N2 Zr2 150.9(3) . . ? C3 N2 Zr2 90.2(3) . . ? C21' N3 C17 118.8(7) . . ? C21' N3 C21 28.7(6) . . ? C17 N3 C21 115.7(7) . . ? C21' N3 Zr1 115.3(7) . . ? C17 N3 Zr1 122.5(3) . . ? C21 N3 Zr1 121.1(7) . . ? C26 N4 C22 112.8(7) . . ? C26 N4 C26' 35.9(6) . . ? C22 N4 C26' 122.3(6) . . ? C26 N4 Zr2 120.1(6) . . ? C22 N4 Zr2 122.3(3) . . ? C26' N4 Zr2 113.9(6) . . ? C1 O1 Zr1 99.7(3) . . ? C3 O2 Zr2 99.4(3) . . ? C5 O3 Zr1 151.9(3) . . ? C9 O4 Zr1 165.4(4) . . ? C13 O5 Zr1 169.5(3) . . ? C27 O6 Zr2 167.7(3) . . ? C31 O7 Zr2 164.1(3) . . ? C35 O8 Zr2 156.6(3) . . ? O1 C1 N1 112.5(4) . . ? O1 C1 C2 126.8(4) . . ? N1 C1 C2 120.8(4) . . ? O1 C1 Zr1 52.8(2) . . ? N1 C1 Zr1 59.7(2) . . ? C2 C1 Zr1 179.5(4) . . ? C1 C2 C3 116.9(4) . . ? O2 C3 N2 112.7(4) . . ? O2 C3 C2 126.0(4) . . ? N2 C3 C2 121.3(4) . . ? O2 C3 Zr2 53.0(2) . . ? N2 C3 Zr2 60.1(2) . . ? C2 C3 Zr2 173.7(3) . . ? N1 C4 N2 125.5(4) . . ? O3 C5 C7 107.3(5) . . ? O3 C5 C8 107.8(4) . . ? C7 C5 C8 112.7(6) . . ? O3 C5 C6 109.0(4) . . ? C7 C5 C6 110.2(5) . . ? C8 C5 C6 109.7(5) . . ? O4 C9 C12 111.2(5) . . ? O4 C9 C10 110.9(6) . . ? C12 C9 C10 111.3(7) . . ? O4 C9 C11 105.0(5) . . ? C12 C9 C11 112.9(8) . . ? C10 C9 C11 105.4(8) . . ? O5 C13 C15 108.5(5) . . ? O5 C13 C16 107.9(6) . . ? C15 C13 C16 112.3(8) . . ? O5 C13 C14 106.9(5) . . ? C15 C13 C14 107.8(7) . . ? C16 C13 C14 113.2(8) . . ? N3 C17 C18 124.4(5) . . ? C17 C18 C19' 113.1(8) . . ? C17 C18 C19 118.1(7) . . ? C19' C18 C19 34.4(6) . . ? C20 C19 C18 117.9(11) . . ? C20' C19' C18 121.1(13) . . ? C19 C20 C21 120.5(12) . . ? C19' C20' C21' 117.6(12) . . ? C20 C21 N3 121.1(12) . . ? N3 C21' C20' 121.8(12) . . ? N4 C22 C23 124.4(6) . . ? C24 C23 C22 119.2(9) . . ? C24 C23 C24' 36.0(7) . . ? C22 C23 C24' 112.1(7) . . ? C23 C24 C25 117.5(12) . . ? C25' C24' C23 120.7(10) . . ? C26 C25 C24 117.0(10) . . ? C24' C25' C26' 122.1(13) . . ? N4 C26 C25 126.2(10) . . ? C25' C26' N4 115.5(11) . . ? O6 C27 C29 109.0(5) . . ? O6 C27 C30 109.4(5) . . ? C29 C27 C30 112.7(6) . . ? O6 C27 C28 105.2(5) . . ? C29 C27 C28 110.8(6) . . ? C30 C27 C28 109.4(6) . . ? O7 C31 C33 110.1(5) . . ? O7 C31 C34 109.0(5) . . ? C33 C31 C34 113.8(6) . . ? O7 C31 C32 107.2(4) . . ? C33 C31 C32 109.9(6) . . ? C34 C31 C32 106.7(6) . . ? O8 C35 C38 109.8(4) . . ? O8 C35 C37 108.4(4) . . ? C38 C35 C37 110.3(5) . . ? O8 C35 C36 108.5(4) . . ? C38 C35 C36 109.9(5) . . ? C37 C35 C36 110.0(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.664 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.078 #===END