Supplementary Material (ESI) for Chemical Science This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Kongprakaiwoot, Natcharee' 'Quiroz-Guzman, Mauricio' 'Oliver, Allen' 'Brown, Seth' _publ_contact_author_name 'Brown, Seth' _publ_contact_author_email seth.n.brown.114@nd.edu _publ_section_title ; electronic dissymmetry in bis-chelates of titanium(IV) using sterically and electronically variable 2,2'-biphenoxides ; # Attachment 'BiPhenOx-composite.cif' data_bobme4 _database_code_depnum_ccdc_archive 'CCDC 791673' #TrackingRef 'BiPhenOx-composite.cif' # Collected at the synchrotron as nd40 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,2'-Biphenylbis(4-p-tolyl-2,4-butanedionato))- (3,3',5,5'-tetramethylbiphenyl-2,2'-diolato)titanium(IV) hemihexane solvate ; _chemical_name_common '(Bob)Ti(O2C12H4Me4) . 0.5 C6H14' _chemical_melting_point ? _chemical_formula_moiety 'C50 H44 O6 Ti, 0.5 (C6 H14)' _chemical_formula_sum 'C53 H51 O6 Ti' _chemical_formula_weight 831.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.3056 0.5263 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5360(15) _cell_length_b 10.7745(17) _cell_length_c 21.214(3) _cell_angle_alpha 87.903(2) _cell_angle_beta 87.712(3) _cell_angle_gamma 88.606(2) _cell_volume 2175.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1462 _cell_measurement_theta_min 4.22 _cell_measurement_theta_max 20.88 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9891 _exptl_absorpt_correction_T_max 0.9973 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany. ; _exptl_crystal_recrystallization_method ; Crystals were deposited from a saturated solution of the complex in hexane at room temperature. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 11691 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 20.99 _reflns_number_total 3568 _reflns_number_gt 2563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0575P)^2^+0.4964P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3568 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.63777(8) 0.88260(8) 0.75900(4) 0.0347(3) Uani 1 1 d . . . O1 O 0.5609(3) 0.7657(3) 0.82922(13) 0.0355(8) Uani 1 1 d . . . O2 O 0.7234(3) 0.7285(3) 0.72678(13) 0.0372(8) Uani 1 1 d . . . O3 O 0.4591(3) 0.8388(3) 0.71749(13) 0.0383(8) Uani 1 1 d . . . O4 O 0.5160(3) 1.0120(3) 0.79729(13) 0.0361(8) Uani 1 1 d . . . O5 O 0.7090(3) 0.9762(3) 0.69140(12) 0.0331(8) Uani 1 1 d . . . O6 O 0.7820(3) 0.9251(3) 0.80963(12) 0.0333(8) Uani 1 1 d . . . C1 C 0.4362(4) 0.5980(4) 0.8776(2) 0.0377(13) Uani 1 1 d . . . H1A H 0.4799 0.6046 0.9189 0.045 Uiso 1 1 calc R . . H1B H 0.4230 0.5088 0.8706 0.045 Uiso 1 1 calc R . . C2 C 0.5346(4) 0.6499(5) 0.8264(2) 0.0328(12) Uani 1 1 d . . . C3 C 0.5916(5) 0.5735(4) 0.7800(2) 0.0372(12) Uani 1 1 d . . . H3 H 0.5632 0.4896 0.7803 0.045 Uiso 1 1 calc R . . C4 C 0.6878(5) 0.6135(5) 0.7331(2) 0.0329(12) Uani 1 1 d . . . C5 C 0.2230(5) 0.7803(4) 0.7067(2) 0.0348(12) Uani 1 1 d . . . H5A H 0.2253 0.8015 0.6609 0.042 Uiso 1 1 calc R . . H5B H 0.1285 0.8035 0.7242 0.042 Uiso 1 1 calc R . . C6 C 0.3309(5) 0.8564(4) 0.7376(2) 0.0336(12) Uani 1 1 d . . . C7 C 0.2901(5) 0.9404(4) 0.7835(2) 0.0342(12) Uani 1 1 d . . . H7 H 0.1939 0.9445 0.7970 0.041 Uiso 1 1 calc R . . C8 C 0.3823(5) 1.0183(4) 0.8108(2) 0.0327(12) Uani 1 1 d . . . C11 C 0.1957(5) 0.6514(4) 0.8333(2) 0.0306(12) Uani 1 1 d . . . C12 C 0.2940(5) 0.6634(4) 0.8803(2) 0.0323(12) Uani 1 1 d . . . C13 C 0.2603(5) 0.7413(5) 0.9302(2) 0.0431(13) Uani 1 1 d . . . H13 H 0.3269 0.7523 0.9616 0.052 Uiso 1 1 calc R . . C14 C 0.1308(6) 0.8029(5) 0.9347(2) 0.0463(14) Uani 1 1 d . . . H14 H 0.1097 0.8557 0.9688 0.056 Uiso 1 1 calc R . . C15 C 0.0331(5) 0.7876(4) 0.8899(2) 0.0414(13) Uani 1 1 d . . . H15 H -0.0561 0.8285 0.8934 0.050 Uiso 1 1 calc R . . C16 C 0.0653(5) 0.7128(4) 0.8399(2) 0.0387(13) Uani 1 1 d . . . H16 H -0.0027 0.7026 0.8091 0.046 Uiso 1 1 calc R . . C21 C 0.2302(4) 0.5795(5) 0.7759(2) 0.0325(12) Uani 1 1 d . . . C22 C 0.2458(4) 0.6397(4) 0.7162(2) 0.0344(12) Uani 1 1 d . . . C23 C 0.2842(5) 0.5699(5) 0.6646(2) 0.0437(13) Uani 1 1 d . . . H23 H 0.2958 0.6101 0.6241 0.052 Uiso 1 1 calc R . . C24 C 0.3061(5) 0.4423(5) 0.6707(3) 0.0486(14) Uani 1 1 d . . . H24 H 0.3333 0.3963 0.6347 0.058 Uiso 1 1 calc R . . C25 C 0.2886(5) 0.3822(5) 0.7286(3) 0.0450(13) Uani 1 1 d . . . H25 H 0.3024 0.2947 0.7327 0.054 Uiso 1 1 calc R . . C26 C 0.2504(4) 0.4504(5) 0.7810(2) 0.0373(12) Uani 1 1 d . . . H26 H 0.2378 0.4089 0.8210 0.045 Uiso 1 1 calc R . . C31 C 0.7569(5) 0.5285(5) 0.6877(2) 0.0366(12) Uani 1 1 d . . . C32 C 0.8744(5) 0.5692(5) 0.6515(2) 0.0457(13) Uani 1 1 d . . . H32 H 0.9103 0.6492 0.6575 0.055 Uiso 1 1 calc R . . C33 C 0.9381(5) 0.4933(5) 0.6072(2) 0.0536(15) Uani 1 1 d . . . H33 H 1.0190 0.5214 0.5838 0.064 Uiso 1 1 calc R . . C34 C 0.8869(6) 0.3773(5) 0.5960(2) 0.0495(14) Uani 1 1 d . . . C35 C 0.7725(6) 0.3371(5) 0.6326(3) 0.0527(15) Uani 1 1 d . . . H35 H 0.7368 0.2571 0.6263 0.063 Uiso 1 1 calc R . . C36 C 0.7084(5) 0.4107(5) 0.6783(2) 0.0480(14) Uani 1 1 d . . . H36 H 0.6309 0.3802 0.7033 0.058 Uiso 1 1 calc R . . C37 C 0.9550(6) 0.2975(5) 0.5457(2) 0.0718(18) Uani 1 1 d . . . H37A H 0.9382 0.2098 0.5566 0.108 Uiso 1 1 calc R . . H37B H 1.0562 0.3115 0.5431 0.108 Uiso 1 1 calc R . . H37C H 0.9147 0.3196 0.5049 0.108 Uiso 1 1 calc R . . C41 C 0.3376(5) 1.1129(4) 0.8571(2) 0.0332(12) Uani 1 1 d . . . C42 C 0.4378(5) 1.1906(4) 0.8800(2) 0.0375(13) Uani 1 1 d . . . H42 H 0.5314 1.1866 0.8630 0.045 Uiso 1 1 calc R . . C43 C 0.4031(5) 1.2725(4) 0.9265(2) 0.0403(13) Uani 1 1 d . . . H43 H 0.4744 1.3223 0.9417 0.048 Uiso 1 1 calc R . . C44 C 0.2682(5) 1.2848(4) 0.9517(2) 0.0362(12) Uani 1 1 d . . . C45 C 0.1669(5) 1.2103(4) 0.9281(2) 0.0377(12) Uani 1 1 d . . . H45 H 0.0728 1.2177 0.9442 0.045 Uiso 1 1 calc R . . C46 C 0.1991(5) 1.1250(4) 0.8816(2) 0.0364(12) Uani 1 1 d . . . H46 H 0.1277 1.0753 0.8664 0.044 Uiso 1 1 calc R . . C47 C 0.2306(5) 1.3757(5) 1.0022(2) 0.0547(15) Uani 1 1 d . . . H47A H 0.2568 1.3400 1.0433 0.082 Uiso 1 1 calc R . . H47B H 0.1293 1.3935 1.0029 0.082 Uiso 1 1 calc R . . H47C H 0.2812 1.4529 0.9932 0.082 Uiso 1 1 calc R . . C51 C 0.9310(5) 1.0677(4) 0.7109(2) 0.0306(12) Uani 1 1 d . . . C52 C 0.8455(5) 0.9988(4) 0.6734(2) 0.0292(11) Uani 1 1 d . . . C53 C 0.8950(5) 0.9552(4) 0.6152(2) 0.0328(12) Uani 1 1 d . . . C54 C 1.0335(5) 0.9800(4) 0.5955(2) 0.0371(12) Uani 1 1 d . . . H54 H 1.0692 0.9482 0.5567 0.045 Uiso 1 1 calc R . . C55 C 1.1204(5) 1.0491(4) 0.6305(2) 0.0334(12) Uani 1 1 d . . . C56 C 1.0670(5) 1.0924(4) 0.6874(2) 0.0323(12) Uani 1 1 d . . . H56 H 1.1253 1.1410 0.7116 0.039 Uiso 1 1 calc R . . C57 C 0.7985(5) 0.8859(4) 0.5746(2) 0.0459(13) Uani 1 1 d . . . H57A H 0.7234 0.9424 0.5601 0.069 Uiso 1 1 calc R . . H57B H 0.7575 0.8163 0.5994 0.069 Uiso 1 1 calc R . . H57C H 0.8522 0.8542 0.5380 0.069 Uiso 1 1 calc R . . C58 C 1.2703(5) 1.0766(4) 0.6081(2) 0.0453(13) Uani 1 1 d . . . H58A H 1.2800 1.1664 0.6009 0.068 Uiso 1 1 calc R . . H58B H 1.2925 1.0343 0.5687 0.068 Uiso 1 1 calc R . . H58C H 1.3351 1.0468 0.6403 0.068 Uiso 1 1 calc R . . C61 C 0.8819(4) 1.1190(4) 0.7730(2) 0.0301(12) Uani 1 1 d . . . C62 C 0.8161(4) 1.0451(4) 0.8209(2) 0.0289(11) Uani 1 1 d . . . C63 C 0.7824(4) 1.0909(5) 0.8800(2) 0.0328(12) Uani 1 1 d . . . C64 C 0.8112(4) 1.2148(5) 0.8896(2) 0.0343(12) Uani 1 1 d . . . H64 H 0.7871 1.2476 0.9297 0.041 Uiso 1 1 calc R . . C65 C 0.8734(4) 1.2928(4) 0.8436(2) 0.0338(12) Uani 1 1 d . . . C66 C 0.9090(4) 1.2411(4) 0.7858(2) 0.0344(12) Uani 1 1 d . . . H66 H 0.9537 1.2917 0.7537 0.041 Uiso 1 1 calc R . . C67 C 0.7131(5) 1.0094(4) 0.9312(2) 0.0429(13) Uani 1 1 d . . . H67A H 0.6389 0.9620 0.9132 0.064 Uiso 1 1 calc R . . H67B H 0.6722 1.0615 0.9645 0.064 Uiso 1 1 calc R . . H67C H 0.7833 0.9519 0.9492 0.064 Uiso 1 1 calc R . . C68 C 0.8998(5) 1.4263(4) 0.8561(2) 0.0441(13) Uani 1 1 d . . . H68A H 0.8148 1.4645 0.8752 0.066 Uiso 1 1 calc R . . H68B H 0.9249 1.4708 0.8163 0.066 Uiso 1 1 calc R . . H68C H 0.9769 1.4307 0.8851 0.066 Uiso 1 1 calc R . . C71 C 0.4450(6) 0.7917(6) 0.5134(3) 0.091(2) Uani 1 1 d . . . H71A H 0.5050 0.8587 0.5255 0.136 Uiso 1 1 calc R . . H71B H 0.3644 0.7851 0.5434 0.136 Uiso 1 1 calc R . . H71C H 0.4116 0.8098 0.4709 0.136 Uiso 1 1 calc R . . C72 C 0.5252(6) 0.6747(6) 0.5142(3) 0.085(2) Uani 1 1 d . . . H72A H 0.6070 0.6860 0.4845 0.103 Uiso 1 1 calc R . . H72B H 0.5627 0.6629 0.5569 0.103 Uiso 1 1 calc R . . C73 C 0.4615(6) 0.5586(5) 0.4993(3) 0.0700(17) Uani 1 1 d . . . H73A H 0.3786 0.5484 0.5284 0.084 Uiso 1 1 calc R . . H73B H 0.4254 0.5703 0.4563 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0358(5) 0.0324(6) 0.0363(6) -0.0091(4) 0.0038(4) -0.0079(4) O1 0.0399(19) 0.030(2) 0.0368(19) -0.0100(16) 0.0029(15) -0.0075(16) O2 0.0414(19) 0.032(2) 0.039(2) -0.0107(16) 0.0064(15) -0.0077(17) O3 0.040(2) 0.037(2) 0.038(2) -0.0089(16) 0.0039(17) -0.0093(17) O4 0.033(2) 0.035(2) 0.040(2) -0.0066(16) 0.0064(16) -0.0069(16) O5 0.033(2) 0.0338(19) 0.0327(18) -0.0057(15) -0.0001(15) -0.0095(15) O6 0.0347(18) 0.031(2) 0.0347(19) -0.0048(15) 0.0008(14) -0.0079(16) C1 0.039(3) 0.038(3) 0.037(3) 0.000(3) -0.004(3) -0.010(3) C2 0.027(3) 0.037(4) 0.034(3) -0.004(3) -0.003(3) -0.005(3) C3 0.040(3) 0.029(3) 0.043(3) -0.002(3) 0.001(3) -0.009(3) C4 0.032(3) 0.029(4) 0.040(3) -0.008(3) -0.009(3) -0.004(3) C5 0.040(3) 0.032(3) 0.034(3) -0.005(2) -0.008(2) -0.005(2) C6 0.037(3) 0.029(3) 0.035(3) 0.006(3) -0.005(3) -0.009(3) C7 0.038(3) 0.027(3) 0.038(3) 0.000(3) -0.001(3) -0.006(3) C8 0.040(4) 0.027(3) 0.032(3) 0.000(3) -0.001(3) -0.008(3) C11 0.036(3) 0.023(3) 0.033(3) 0.000(2) 0.004(3) -0.010(3) C12 0.037(3) 0.026(3) 0.034(3) 0.003(3) 0.007(3) -0.011(3) C13 0.048(4) 0.049(3) 0.033(3) -0.001(3) 0.002(3) -0.007(3) C14 0.054(4) 0.048(4) 0.037(3) -0.006(3) 0.011(3) -0.004(3) C15 0.037(3) 0.040(3) 0.046(3) 0.000(3) 0.010(3) -0.001(3) C16 0.040(3) 0.035(3) 0.041(3) -0.006(3) 0.006(3) -0.009(3) C21 0.028(3) 0.034(4) 0.037(4) -0.009(3) 0.000(2) -0.009(2) C22 0.026(3) 0.042(4) 0.036(4) -0.010(3) -0.006(2) -0.010(2) C23 0.052(3) 0.043(4) 0.036(3) -0.003(3) -0.001(3) -0.014(3) C24 0.056(3) 0.042(4) 0.050(4) -0.021(3) 0.000(3) -0.009(3) C25 0.049(3) 0.032(3) 0.055(4) -0.007(4) 0.001(3) -0.013(3) C26 0.038(3) 0.035(4) 0.039(3) -0.003(3) -0.003(2) -0.012(3) C31 0.044(3) 0.031(4) 0.035(3) -0.009(3) -0.004(3) 0.000(3) C32 0.048(3) 0.040(3) 0.049(3) -0.015(3) 0.008(3) 0.000(3) C33 0.056(4) 0.055(4) 0.049(4) -0.005(3) 0.008(3) 0.006(3) C34 0.070(4) 0.038(4) 0.040(3) -0.003(3) -0.005(3) 0.016(3) C35 0.074(4) 0.037(3) 0.048(4) -0.008(3) -0.008(3) 0.000(3) C36 0.056(3) 0.046(4) 0.042(3) -0.012(3) 0.001(3) 0.002(3) C37 0.105(5) 0.060(4) 0.049(4) -0.017(3) 0.007(3) 0.027(4) C41 0.033(3) 0.033(3) 0.034(3) 0.002(3) 0.000(3) -0.003(3) C42 0.031(3) 0.036(3) 0.046(3) -0.001(3) -0.001(3) -0.007(3) C43 0.043(4) 0.038(3) 0.041(3) -0.011(3) -0.001(3) -0.004(3) C44 0.046(4) 0.033(3) 0.030(3) -0.001(3) -0.001(3) -0.001(3) C45 0.036(3) 0.040(3) 0.037(3) -0.004(3) 0.004(3) -0.001(3) C46 0.040(4) 0.032(3) 0.038(3) -0.004(3) -0.001(3) -0.007(2) C47 0.055(3) 0.057(4) 0.053(3) -0.016(3) 0.004(3) -0.006(3) C51 0.038(3) 0.024(3) 0.031(3) -0.004(3) -0.001(3) -0.004(3) C52 0.034(3) 0.029(3) 0.025(3) -0.007(3) 0.004(3) -0.003(2) C53 0.045(3) 0.024(3) 0.030(3) 0.000(2) 0.000(3) -0.003(2) C54 0.050(4) 0.033(3) 0.028(3) -0.005(3) 0.009(3) 0.001(3) C55 0.039(3) 0.030(3) 0.031(3) -0.002(3) 0.004(3) -0.008(3) C56 0.036(3) 0.031(3) 0.030(3) -0.002(3) -0.004(3) -0.008(2) C57 0.055(3) 0.049(3) 0.036(3) -0.015(3) -0.001(3) -0.009(3) C58 0.049(3) 0.050(3) 0.038(3) -0.007(3) 0.007(3) -0.007(3) C61 0.026(3) 0.034(3) 0.031(3) -0.009(3) -0.001(2) -0.007(2) C62 0.029(3) 0.025(3) 0.033(3) -0.007(3) -0.004(2) -0.006(2) C63 0.030(3) 0.041(4) 0.028(3) -0.010(3) 0.002(2) 0.000(3) C64 0.034(3) 0.039(4) 0.031(3) -0.014(3) 0.001(2) -0.005(3) C65 0.030(3) 0.034(3) 0.038(3) -0.012(3) -0.002(2) -0.006(3) C66 0.035(3) 0.036(4) 0.033(3) -0.004(3) -0.002(2) -0.011(3) C67 0.050(3) 0.043(3) 0.035(3) -0.011(3) 0.007(3) -0.005(3) C68 0.045(3) 0.044(3) 0.044(3) -0.017(3) 0.003(2) -0.004(3) C71 0.076(4) 0.074(5) 0.123(6) -0.015(4) 0.005(4) -0.005(4) C72 0.072(4) 0.069(5) 0.116(6) -0.017(4) 0.010(4) -0.009(4) C73 0.060(4) 0.073(5) 0.078(4) -0.018(4) 0.003(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O5 1.840(3) . ? Ti O6 1.854(3) . ? Ti O2 1.966(3) . ? Ti O4 1.970(3) . ? Ti O3 2.022(3) . ? Ti O1 2.040(3) . ? O1 C2 1.283(5) . ? O2 C4 1.293(5) . ? O3 C6 1.290(5) . ? O4 C8 1.296(5) . ? O5 C52 1.367(5) . ? O6 C62 1.372(5) . ? C1 C2 1.507(6) . ? C1 C12 1.513(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.393(6) . ? C3 C4 1.390(6) . ? C3 H3 0.9500 . ? C4 C31 1.478(6) . ? C5 C6 1.515(6) . ? C5 C22 1.532(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.393(6) . ? C7 C8 1.387(6) . ? C7 H7 0.9500 . ? C8 C41 1.485(6) . ? C11 C16 1.398(6) . ? C11 C12 1.408(6) . ? C11 C21 1.488(6) . ? C12 C13 1.398(6) . ? C13 C14 1.388(6) . ? C13 H13 0.9500 . ? C14 C15 1.374(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.400(6) . ? C21 C22 1.407(6) . ? C22 C23 1.383(6) . ? C23 C24 1.388(6) . ? C23 H23 0.9500 . ? C24 C25 1.373(6) . ? C24 H24 0.9500 . ? C25 C26 1.386(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.385(6) . ? C31 C32 1.402(6) . ? C32 C33 1.382(6) . ? C32 H32 0.9500 . ? C33 C34 1.384(7) . ? C33 H33 0.9500 . ? C34 C35 1.383(7) . ? C34 C37 1.511(7) . ? C35 C36 1.389(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.397(6) . ? C41 C46 1.404(6) . ? C42 C43 1.373(6) . ? C42 H42 0.9500 . ? C43 C44 1.379(6) . ? C43 H43 0.9500 . ? C44 C45 1.391(6) . ? C44 C47 1.504(6) . ? C45 C46 1.393(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C56 1.399(6) . ? C51 C52 1.404(6) . ? C51 C61 1.501(6) . ? C52 C53 1.398(6) . ? C53 C54 1.398(6) . ? C53 C57 1.513(6) . ? C54 C55 1.383(6) . ? C54 H54 0.9500 . ? C55 C56 1.384(6) . ? C55 C58 1.521(6) . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 C66 1.385(6) . ? C61 C62 1.405(6) . ? C62 C63 1.387(6) . ? C63 C64 1.393(6) . ? C63 C67 1.514(6) . ? C64 C65 1.389(6) . ? C64 H64 0.9500 . ? C65 C66 1.391(6) . ? C65 C68 1.502(6) . ? C66 H66 0.9500 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C71 C72 1.458(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.454(7) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C73 1.446(10) 2_666 ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? 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 Ti O6 92.28(12) . . ? O5 Ti O2 92.39(13) . . ? O6 Ti O2 97.85(13) . . ? O5 Ti O4 98.05(12) . . ? O6 Ti O4 89.81(13) . . ? O2 Ti O4 166.80(13) . . ? O5 Ti O3 95.47(12) . . ? O6 Ti O3 170.07(13) . . ? O2 Ti O3 88.02(12) . . ? O4 Ti O3 82.99(12) . . ? O5 Ti O1 175.05(13) . . ? O6 Ti O1 90.15(12) . . ? O2 Ti O1 83.01(12) . . ? O4 Ti O1 86.26(12) . . ? O3 Ti O1 82.59(12) . . ? C2 O1 Ti 128.2(3) . . ? C4 O2 Ti 132.4(3) . . ? C6 O3 Ti 128.5(3) . . ? C8 O4 Ti 132.5(3) . . ? C52 O5 Ti 129.6(3) . . ? C62 O6 Ti 124.1(3) . . ? C2 C1 C12 113.5(4) . . ? C2 C1 H1A 108.9 . . ? C12 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? C12 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O1 C2 C3 123.8(4) . . ? O1 C2 C1 115.9(4) . . ? C3 C2 C1 120.4(4) . . ? C4 C3 C2 123.5(4) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? O2 C4 C3 121.7(4) . . ? O2 C4 C31 115.6(4) . . ? C3 C4 C31 122.7(5) . . ? C6 C5 C22 113.8(3) . . ? C6 C5 H5A 108.8 . . ? C22 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? C22 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? O3 C6 C7 123.9(4) . . ? O3 C6 C5 115.5(4) . . ? C7 C6 C5 120.7(4) . . ? C8 C7 C6 123.5(4) . . ? C8 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? O4 C8 C7 121.3(4) . . ? O4 C8 C41 115.2(4) . . ? C7 C8 C41 123.5(4) . . ? C16 C11 C12 118.8(4) . . ? C16 C11 C21 119.8(4) . . ? C12 C11 C21 121.3(4) . . ? C13 C12 C11 118.7(4) . . ? C13 C12 C1 119.0(4) . . ? C11 C12 C1 122.3(4) . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 120.3(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 121.7(4) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? C26 C21 C22 118.9(4) . . ? C26 C21 C11 120.2(4) . . ? C22 C21 C11 120.9(4) . . ? C23 C22 C21 118.9(4) . . ? C23 C22 C5 119.1(4) . . ? C21 C22 C5 122.0(4) . . ? C22 C23 C24 121.2(5) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 121.2(4) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C36 C31 C32 118.4(5) . . ? C36 C31 C4 122.5(5) . . ? C32 C31 C4 119.0(5) . . ? C33 C32 C31 120.2(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 121.6(5) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 117.8(5) . . ? C35 C34 C37 121.4(5) . . ? C33 C34 C37 120.8(6) . . ? C34 C35 C36 121.7(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C31 C36 C35 120.3(5) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C42 C41 C46 117.7(4) . . ? C42 C41 C8 119.3(4) . . ? C46 C41 C8 123.0(4) . . ? C43 C42 C41 121.1(4) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 122.2(4) . . ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? C43 C44 C45 117.2(4) . . ? C43 C44 C47 121.9(4) . . ? C45 C44 C47 121.0(4) . . ? C44 C45 C46 122.1(4) . . ? C44 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C45 C46 C41 119.8(4) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C56 C51 C52 117.5(4) . . ? C56 C51 C61 119.1(4) . . ? C52 C51 C61 123.4(4) . . ? O5 C52 C53 117.5(4) . . ? O5 C52 C51 121.1(4) . . ? C53 C52 C51 121.3(4) . . ? C54 C53 C52 118.2(4) . . ? C54 C53 C57 121.7(4) . . ? C52 C53 C57 120.1(4) . . ? C55 C54 C53 122.3(4) . . ? C55 C54 H54 118.8 . . ? C53 C54 H54 118.8 . . ? C54 C55 C56 117.8(4) . . ? C54 C55 C58 121.7(4) . . ? C56 C55 C58 120.5(4) . . ? C55 C56 C51 122.8(4) . . ? C55 C56 H56 118.6 . . ? C51 C56 H56 118.6 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C66 C61 C62 118.0(4) . . ? C66 C61 C51 119.7(4) . . ? C62 C61 C51 122.1(4) . . ? O6 C62 C63 118.3(4) . . ? O6 C62 C61 120.2(4) . . ? C63 C62 C61 121.5(4) . . ? C62 C63 C64 117.7(4) . . ? C62 C63 C67 120.7(4) . . ? C64 C63 C67 121.6(4) . . ? C65 C64 C63 123.2(4) . . ? C65 C64 H64 118.4 . . ? C63 C64 H64 118.4 . . ? C64 C65 C66 116.8(4) . . ? C64 C65 C68 121.1(4) . . ? C66 C65 C68 122.2(4) . . ? C61 C66 C65 122.8(4) . . ? C61 C66 H66 118.6 . . ? C65 C66 H66 118.6 . . ? C63 C67 H67A 109.5 . . ? C63 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C63 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C71 121.4(5) . . ? C73 C72 H72A 107.0 . . ? C71 C72 H72A 107.0 . . ? C73 C72 H72B 107.0 . . ? C71 C72 H72B 107.0 . . ? H72A C72 H72B 106.7 . . ? C73 C73 C72 122.3(6) 2_666 . ? C73 C73 H73A 106.8 2_666 . ? C72 C73 H73A 106.8 . . ? C73 C73 H73B 106.8 2_666 . ? C72 C73 H73B 106.8 . . ? H73A C73 H73B 106.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.198 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.039 _vrf_THETM01_bobme4 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Despite data collection on a synchrotron source the diffracted intensities still dropped-off rapidly with increasing sin\q/\l. However, the final refined structure is satisfactory and meets the necessities of the discussion presented. This results in a number of alerts being issued by the checking routine. ; _vrf_PLAT023_bobme4 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 20.99 Deg. RESPONSE: See Above. ; #========END data_hobbiph _database_code_depnum_ccdc_archive 'CCDC 791674' #TrackingRef 'BiPhenOx-composite.cif' # Collected as mqg003 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2'-(4-p-tolyl-2,4-butanedionato)-biphenyl-2-N-methylacetohydroxamato)- (3,3',5,5'-tetramethylbiphenyl-2,2'-diolato)titanium(IV) deuteriochloroform solvate ; _chemical_name_common '(Hob)Ti(O2C12H4Me4) . CDCl3' _chemical_melting_point ? _chemical_formula_moiety 'C42 H39 N O6 Ti, C D Cl3' _chemical_formula_sum 'C43 H39 D Cl3 N O6 Ti' _chemical_formula_weight 822.01 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0648(5) _cell_length_b 12.6467(5) _cell_length_c 14.4497(14) _cell_angle_alpha 109.3684(14) _cell_angle_beta 96.4954(15) _cell_angle_gamma 106.9980(17) _cell_volume 1934.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 26.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8845 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany. ; _exptl_crystal_recrystallization_method ; Crystals were deposited from a concentrated solution of the complex in CDCl3. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 28893 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.67 _reflns_number_total 7854 _reflns_number_gt 6583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. Hydrogen atoms were found on difference Fourier maps and refined isotropically, except for the hydrogens on the 5,5'-methyl groups of the biphenoxide ligand, which were placed in calculated positions. ; _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^)+(0.0464P)^2^+1.2134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7854 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.45194(3) 0.08248(3) 0.22130(2) 0.01538(9) Uani 1 1 d . . . O1 O 0.38910(11) -0.07630(11) 0.23878(9) 0.0177(3) Uani 1 1 d . . . O2 O 0.55962(11) 0.12709(11) 0.35021(9) 0.0183(3) Uani 1 1 d . . . O3 O 0.56895(11) 0.00785(11) 0.15455(9) 0.0167(3) Uani 1 1 d . . . O4 O 0.36490(11) -0.01202(11) 0.08242(9) 0.0171(3) Uani 1 1 d . . . O5 O 0.51421(11) 0.22862(11) 0.21047(9) 0.0169(3) Uani 1 1 d . . . O6 O 0.32235(11) 0.12012(11) 0.25822(9) 0.0170(3) Uani 1 1 d . . . N N 0.40859(13) -0.09909(13) 0.03285(11) 0.0152(3) Uani 1 1 d . . . C1 C 0.37931(17) -0.25124(17) 0.26702(14) 0.0179(4) Uani 1 1 d . . . C2 C 0.44008(16) -0.12084(16) 0.28995(13) 0.0155(4) Uani 1 1 d . . . C3 C 0.54340(17) -0.05525(17) 0.36629(14) 0.0186(4) Uani 1 1 d . . . C4 C 0.59644(16) 0.06616(17) 0.39581(13) 0.0167(4) Uani 1 1 d . . . C5 C 0.58083(17) -0.17079(17) 0.03184(14) 0.0166(4) Uani 1 1 d . . . C6 C 0.51733(16) -0.08465(16) 0.07371(13) 0.0148(4) Uani 1 1 d . . . C7 C 0.32203(18) -0.19594(18) -0.05255(15) 0.0188(4) Uani 1 1 d . . . C11 C 0.42761(16) -0.35074(16) 0.09829(14) 0.0160(4) Uani 1 1 d . . . C12 C 0.34330(16) -0.32909(16) 0.15567(14) 0.0167(4) Uani 1 1 d . . . C13 C 0.22354(18) -0.38295(17) 0.10824(15) 0.0207(4) Uani 1 1 d . . . C14 C 0.18641(18) -0.45941(18) 0.00749(16) 0.0232(4) Uani 1 1 d . . . C15 C 0.26907(18) -0.48383(17) -0.04756(16) 0.0221(4) Uani 1 1 d . . . C16 C 0.38881(18) -0.42860(16) -0.00239(15) 0.0186(4) Uani 1 1 d . . . C21 C 0.55725(16) -0.29158(16) 0.14443(14) 0.0161(4) Uani 1 1 d . . . C22 C 0.62959(16) -0.20798(16) 0.11312(14) 0.0159(4) Uani 1 1 d . . . C23 C 0.74857(17) -0.15336(18) 0.16130(15) 0.0210(4) Uani 1 1 d . . . C24 C 0.79662(18) -0.17789(18) 0.24035(16) 0.0245(4) Uani 1 1 d . . . C25 C 0.72616(18) -0.26116(18) 0.27019(15) 0.0232(4) Uani 1 1 d . . . C26 C 0.60810(17) -0.31870(17) 0.22156(14) 0.0190(4) Uani 1 1 d . . . C51 C 0.41780(16) 0.36929(16) 0.28457(14) 0.0166(4) Uani 1 1 d . . . C52 C 0.52030(17) 0.33833(16) 0.27408(13) 0.0162(4) Uani 1 1 d . . . C53 C 0.63284(17) 0.42027(17) 0.32850(13) 0.0173(4) Uani 1 1 d . . . C54 C 0.63997(18) 0.53138(17) 0.39583(14) 0.0191(4) Uani 1 1 d . . . C55 C 0.54073(17) 0.56485(17) 0.40958(14) 0.0187(4) Uani 1 1 d . . . C56 C 0.43104(17) 0.48316(17) 0.35270(14) 0.0182(4) Uani 1 1 d . . . C57 C 0.74238(18) 0.3882(2) 0.31290(16) 0.0220(4) Uani 1 1 d . . . C58 C 0.55268(18) 0.68592(17) 0.48481(15) 0.0225(4) Uani 1 1 d . . . H58A H 0.5282 0.6773 0.5451 0.034 Uiso 1 1 calc R . . H58B H 0.5018 0.7193 0.4546 0.034 Uiso 1 1 calc R . . H58C H 0.6359 0.7397 0.5036 0.034 Uiso 1 1 calc R . . C61 C 0.29663(16) 0.28755(16) 0.22552(14) 0.0173(4) Uani 1 1 d . . . C62 C 0.25398(16) 0.16786(16) 0.21431(13) 0.0164(4) Uani 1 1 d . . . C63 C 0.13838(17) 0.09422(17) 0.16091(14) 0.0185(4) Uani 1 1 d . . . C64 C 0.06564(18) 0.14289(18) 0.11950(15) 0.0215(4) Uani 1 1 d . . . C65 C 0.10363(18) 0.26147(18) 0.13028(16) 0.0251(4) Uani 1 1 d . . . C66 C 0.21919(18) 0.33143(18) 0.18234(15) 0.0217(4) Uani 1 1 d . . . C67 C 0.0957(2) -0.03214(19) 0.15412(17) 0.0240(4) Uani 1 1 d . . . C68 C 0.0204(2) 0.3130(2) 0.0882(2) 0.0400(6) Uani 1 1 d . . . H68A H 0.0524 0.4005 0.1211 0.060 Uiso 1 1 calc R . . H68B H -0.0585 0.2824 0.1009 0.060 Uiso 1 1 calc R . . H68C H 0.0135 0.2892 0.0153 0.060 Uiso 1 1 calc R . . C31 C 0.69972(16) 0.13665(17) 0.48276(14) 0.0174(4) Uani 1 1 d . . . C32 C 0.74411(18) 0.26026(18) 0.51184(14) 0.0205(4) Uani 1 1 d . . . C33 C 0.84172(18) 0.32885(19) 0.59065(15) 0.0227(4) Uani 1 1 d . . . C34 C 0.89990(17) 0.27728(18) 0.64225(15) 0.0225(4) Uani 1 1 d . . . C35 C 0.85542(19) 0.1547(2) 0.61382(16) 0.0264(5) Uani 1 1 d . . . C36 C 0.75655(19) 0.08516(19) 0.53595(16) 0.0252(4) Uani 1 1 d . . . C37 C 1.0092(2) 0.3527(2) 0.72486(18) 0.0302(5) Uani 1 1 d . . . C0 C 1.0305(2) 0.22683(19) 0.36248(17) 0.0279(5) Uani 1 1 d . . . Cl1 Cl 1.07802(6) 0.16042(6) 0.44190(5) 0.04865(18) Uani 1 1 d . . . Cl2 Cl 0.88220(5) 0.14784(5) 0.29791(4) 0.03565(15) Uani 1 1 d . . . Cl3 Cl 1.04873(5) 0.37644(5) 0.43289(4) 0.03489(14) Uani 1 1 d . . . H0 H 1.075(2) 0.223(2) 0.3137(18) 0.030(6) Uiso 1 1 d . . . H1A H 0.3077(19) -0.2560(18) 0.2933(15) 0.019(5) Uiso 1 1 d . . . H1B H 0.4276(19) -0.2781(19) 0.3025(16) 0.022(5) Uiso 1 1 d . . . H3 H 0.5728(19) -0.0965(19) 0.3989(16) 0.024(6) Uiso 1 1 d . . . H5A H 0.6450(18) -0.1286(17) 0.0083(14) 0.013(5) Uiso 1 1 d . . . H5B H 0.5309(19) -0.2396(19) -0.0272(16) 0.021(5) Uiso 1 1 d . . . H7A H 0.266(2) -0.240(2) -0.0294(18) 0.032(6) Uiso 1 1 d . . . H7B H 0.2860(19) -0.1615(19) -0.0953(16) 0.022(5) Uiso 1 1 d . . . H7C H 0.363(2) -0.243(2) -0.0899(17) 0.025(6) Uiso 1 1 d . . . H13 H 0.169(2) -0.368(2) 0.1445(17) 0.026(6) Uiso 1 1 d . . . H14 H 0.104(2) -0.4969(19) -0.0216(16) 0.025(6) Uiso 1 1 d . . . H15 H 0.248(2) -0.537(2) -0.1133(18) 0.031(6) Uiso 1 1 d . . . H16 H 0.4425(18) -0.4448(17) -0.0413(15) 0.012(5) Uiso 1 1 d . . . H23 H 0.7959(18) -0.0963(19) 0.1378(15) 0.018(5) Uiso 1 1 d . . . H24 H 0.877(2) -0.134(2) 0.2766(17) 0.032(6) Uiso 1 1 d . . . H25 H 0.7539(19) -0.2825(19) 0.3223(16) 0.023(6) Uiso 1 1 d . . . H26 H 0.5596(17) -0.3776(18) 0.2404(14) 0.012(5) Uiso 1 1 d . . . H54 H 0.713(2) 0.586(2) 0.4336(17) 0.027(6) Uiso 1 1 d . . . H56 H 0.3633(17) 0.5041(17) 0.3615(14) 0.011(5) Uiso 1 1 d . . . H57A H 0.806(2) 0.440(2) 0.3671(17) 0.025(6) Uiso 1 1 d . . . H57B H 0.733(2) 0.309(2) 0.3070(18) 0.037(7) Uiso 1 1 d . . . H57C H 0.763(2) 0.393(2) 0.2508(18) 0.028(6) Uiso 1 1 d . . . H64 H -0.010(2) 0.0957(19) 0.0866(16) 0.020(5) Uiso 1 1 d . . . H66 H 0.2477(18) 0.4099(19) 0.1857(15) 0.018(5) Uiso 1 1 d . . . H67A H 0.093(2) -0.035(2) 0.220(2) 0.043(7) Uiso 1 1 d . . . H67B H 0.021(2) -0.070(2) 0.1134(18) 0.033(6) Uiso 1 1 d . . . H67C H 0.146(2) -0.070(2) 0.1277(19) 0.040(7) Uiso 1 1 d . . . H32 H 0.704(2) 0.298(2) 0.4769(17) 0.030(6) Uiso 1 1 d . . . H33 H 0.8757(19) 0.416(2) 0.6119(16) 0.027(6) Uiso 1 1 d . . . H35 H 0.889(2) 0.116(2) 0.646(2) 0.047(8) Uiso 1 1 d . . . H36 H 0.7275(19) 0.002(2) 0.5217(16) 0.025(6) Uiso 1 1 d . . . H37A H 1.005(2) 0.429(2) 0.7595(19) 0.036(7) Uiso 1 1 d . . . H37B H 1.080(3) 0.362(2) 0.695(2) 0.055(8) Uiso 1 1 d . . . H37C H 1.018(2) 0.316(2) 0.774(2) 0.052(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01823(18) 0.01519(17) 0.01300(17) 0.00467(13) 0.00199(13) 0.00773(14) O1 0.0182(7) 0.0164(6) 0.0176(7) 0.0064(5) 0.0012(5) 0.0063(5) O2 0.0220(7) 0.0165(7) 0.0156(7) 0.0051(5) 0.0009(5) 0.0078(5) O3 0.0177(7) 0.0150(6) 0.0153(6) 0.0036(5) 0.0014(5) 0.0062(5) O4 0.0199(7) 0.0174(6) 0.0150(6) 0.0045(5) 0.0027(5) 0.0104(5) O5 0.0187(7) 0.0160(6) 0.0153(6) 0.0047(5) 0.0036(5) 0.0068(5) O6 0.0201(7) 0.0178(6) 0.0157(6) 0.0075(5) 0.0045(5) 0.0089(5) N 0.0180(8) 0.0149(8) 0.0125(7) 0.0035(6) 0.0046(6) 0.0072(6) C1 0.0174(10) 0.0187(10) 0.0183(10) 0.0086(8) 0.0046(8) 0.0057(8) C2 0.0175(9) 0.0182(9) 0.0135(9) 0.0064(7) 0.0077(7) 0.0081(7) C3 0.0197(10) 0.0200(10) 0.0176(10) 0.0088(8) 0.0019(8) 0.0079(8) C4 0.0177(9) 0.0218(10) 0.0128(9) 0.0065(8) 0.0044(7) 0.0098(8) C5 0.0178(9) 0.0169(9) 0.0164(9) 0.0061(8) 0.0055(8) 0.0076(8) C6 0.0166(9) 0.0156(9) 0.0137(9) 0.0078(7) 0.0039(7) 0.0053(7) C7 0.0176(10) 0.0193(10) 0.0155(9) 0.0035(8) 0.0027(8) 0.0048(8) C11 0.0185(9) 0.0128(9) 0.0182(9) 0.0083(7) 0.0026(7) 0.0056(7) C12 0.0187(9) 0.0139(9) 0.0189(9) 0.0089(8) 0.0031(8) 0.0055(7) C13 0.0187(10) 0.0208(10) 0.0233(10) 0.0096(8) 0.0062(8) 0.0058(8) C14 0.0159(10) 0.0219(10) 0.0268(11) 0.0093(9) -0.0003(8) 0.0016(8) C15 0.0249(10) 0.0160(9) 0.0187(10) 0.0029(8) -0.0006(8) 0.0045(8) C16 0.0220(10) 0.0153(9) 0.0195(10) 0.0067(8) 0.0048(8) 0.0080(8) C21 0.0165(9) 0.0152(9) 0.0151(9) 0.0027(7) 0.0042(7) 0.0071(7) C22 0.0179(9) 0.0156(9) 0.0161(9) 0.0051(7) 0.0050(7) 0.0093(7) C23 0.0187(10) 0.0179(10) 0.0263(11) 0.0086(9) 0.0057(8) 0.0059(8) C24 0.0156(10) 0.0243(11) 0.0288(11) 0.0081(9) -0.0016(8) 0.0050(8) C25 0.0244(11) 0.0259(11) 0.0208(10) 0.0093(9) 0.0000(8) 0.0124(9) C26 0.0213(10) 0.0183(9) 0.0198(10) 0.0080(8) 0.0052(8) 0.0091(8) C51 0.0192(9) 0.0166(9) 0.0154(9) 0.0084(8) 0.0024(7) 0.0063(7) C52 0.0213(9) 0.0158(9) 0.0135(9) 0.0072(7) 0.0043(7) 0.0072(7) C53 0.0198(9) 0.0198(9) 0.0138(9) 0.0083(8) 0.0031(7) 0.0071(8) C54 0.0193(10) 0.0188(10) 0.0168(9) 0.0076(8) -0.0006(8) 0.0039(8) C55 0.0250(10) 0.0160(9) 0.0155(9) 0.0072(8) 0.0025(8) 0.0070(8) C56 0.0211(10) 0.0185(9) 0.0199(10) 0.0098(8) 0.0060(8) 0.0105(8) C57 0.0179(10) 0.0241(11) 0.0194(10) 0.0041(9) 0.0019(8) 0.0066(8) C58 0.0284(11) 0.0174(9) 0.0184(10) 0.0033(8) 0.0010(8) 0.0090(8) C61 0.0186(9) 0.0175(9) 0.0153(9) 0.0052(8) 0.0041(7) 0.0071(8) C62 0.0202(9) 0.0182(9) 0.0136(9) 0.0062(8) 0.0056(7) 0.0098(8) C63 0.0204(10) 0.0191(9) 0.0158(9) 0.0061(8) 0.0058(8) 0.0068(8) C64 0.0167(10) 0.0217(10) 0.0219(10) 0.0067(8) 0.0015(8) 0.0040(8) C65 0.0217(10) 0.0250(11) 0.0277(11) 0.0108(9) -0.0004(9) 0.0085(8) C66 0.0223(10) 0.0166(10) 0.0252(11) 0.0086(8) 0.0012(8) 0.0061(8) C67 0.0238(11) 0.0201(10) 0.0265(12) 0.0097(9) 0.0046(9) 0.0050(9) C68 0.0264(12) 0.0294(12) 0.0606(17) 0.0225(12) -0.0096(11) 0.0061(10) C31 0.0160(9) 0.0215(10) 0.0148(9) 0.0062(8) 0.0044(7) 0.0072(8) C32 0.0225(10) 0.0222(10) 0.0175(10) 0.0094(8) 0.0052(8) 0.0069(8) C33 0.0234(10) 0.0210(10) 0.0209(10) 0.0081(9) 0.0059(8) 0.0035(8) C34 0.0152(9) 0.0267(11) 0.0203(10) 0.0047(9) 0.0033(8) 0.0051(8) C35 0.0237(11) 0.0287(11) 0.0257(11) 0.0088(9) -0.0027(9) 0.0129(9) C36 0.0260(11) 0.0203(11) 0.0271(11) 0.0074(9) 0.0002(9) 0.0093(9) C37 0.0200(11) 0.0313(12) 0.0288(12) 0.0031(11) -0.0016(9) 0.0067(9) C0 0.0260(11) 0.0266(11) 0.0268(11) 0.0050(9) 0.0074(9) 0.0086(9) Cl1 0.0572(4) 0.0398(4) 0.0510(4) 0.0202(3) 0.0033(3) 0.0203(3) Cl2 0.0268(3) 0.0300(3) 0.0359(3) 0.0011(2) 0.0062(2) 0.0036(2) Cl3 0.0324(3) 0.0231(3) 0.0391(3) 0.0040(2) 0.0040(2) 0.0063(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O6 1.8470(13) . ? Ti O5 1.8469(13) . ? Ti O4 1.9382(13) . ? Ti O2 1.9500(13) . ? Ti O1 2.0398(13) . ? Ti O3 2.0730(13) . ? O1 C2 1.272(2) . ? O2 C4 1.302(2) . ? O3 C6 1.274(2) . ? O4 N 1.3803(19) . ? O5 C52 1.362(2) . ? O6 C62 1.369(2) . ? N C6 1.310(2) . ? N C7 1.439(2) . ? C1 C2 1.498(3) . ? C1 C12 1.513(3) . ? C1 H1A 0.98(2) . ? C1 H1B 0.94(2) . ? C2 C3 1.392(3) . ? C3 C4 1.371(3) . ? C3 H3 0.92(2) . ? C4 C31 1.476(3) . ? C5 C6 1.515(3) . ? C5 C22 1.523(3) . ? C5 H5A 0.97(2) . ? C5 H5B 0.97(2) . ? C7 H7A 0.92(3) . ? C7 H7B 0.99(2) . ? C7 H7C 0.95(2) . ? C11 C16 1.390(3) . ? C11 C12 1.414(3) . ? C11 C21 1.483(2) . ? C12 C13 1.383(3) . ? C13 C14 1.386(3) . ? C13 H13 0.90(2) . ? C14 C15 1.385(3) . ? C14 H14 0.95(2) . ? C15 C16 1.377(3) . ? C15 H15 0.92(2) . ? C16 H16 0.93(2) . ? C21 C22 1.397(3) . ? C21 C26 1.399(3) . ? C22 C23 1.378(3) . ? C23 C24 1.388(3) . ? C23 H23 0.96(2) . ? C24 C25 1.371(3) . ? C24 H24 0.95(2) . ? C25 C26 1.371(3) . ? C25 H25 0.94(2) . ? C26 H26 0.94(2) . ? C51 C56 1.399(3) . ? C51 C52 1.411(3) . ? C51 C61 1.477(3) . ? C52 C53 1.390(3) . ? C53 C54 1.390(3) . ? C53 C57 1.511(3) . ? C54 C55 1.395(3) . ? C54 H54 0.92(2) . ? C55 C56 1.373(3) . ? C55 C58 1.509(3) . ? C56 H56 0.94(2) . ? C57 H57A 0.93(2) . ? C57 H57B 0.95(3) . ? C57 H57C 0.97(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61 C62 1.395(3) . ? C61 C66 1.404(3) . ? C62 C63 1.389(3) . ? C63 C64 1.396(3) . ? C63 C67 1.494(3) . ? C64 C65 1.382(3) . ? C64 H64 0.90(2) . ? C65 C66 1.376(3) . ? C65 C68 1.520(3) . ? C66 H66 0.93(2) . ? C67 H67A 0.97(3) . ? C67 H67B 0.91(3) . ? C67 H67C 0.93(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C31 C32 1.390(3) . ? C31 C36 1.400(3) . ? C32 C33 1.371(3) . ? C32 H32 0.97(2) . ? C33 C34 1.395(3) . ? C33 H33 0.98(2) . ? C34 C35 1.379(3) . ? C34 C37 1.492(3) . ? C35 C36 1.374(3) . ? C35 H35 0.92(3) . ? C36 H36 0.95(2) . ? C37 H37A 0.94(3) . ? C37 H37B 0.99(3) . ? C37 H37C 0.97(3) . ? C0 Cl2 1.740(2) . ? C0 Cl3 1.759(2) . ? C0 Cl1 1.767(2) . ? C0 H0 0.93(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 O6 Ti O5 90.23(6) . . ? O6 Ti O4 92.58(6) . . ? O5 Ti O4 98.58(6) . . ? O6 Ti O2 103.40(6) . . ? O5 Ti O2 95.52(6) . . ? O4 Ti O2 158.61(6) . . ? O6 Ti O1 90.64(5) . . ? O5 Ti O1 177.46(6) . . ? O4 Ti O1 83.76(5) . . ? O2 Ti O1 81.96(5) . . ? O6 Ti O3 167.33(5) . . ? O5 Ti O3 96.59(5) . . ? O4 Ti O3 75.88(5) . . ? O2 Ti O3 86.62(5) . . ? O1 Ti O3 83.01(5) . . ? C2 O1 Ti 130.15(12) . . ? C4 O2 Ti 133.61(12) . . ? C6 O3 Ti 113.22(11) . . ? N O4 Ti 113.43(10) . . ? C52 O5 Ti 128.42(11) . . ? C62 O6 Ti 128.10(11) . . ? C6 N O4 115.97(14) . . ? C6 N C7 130.69(16) . . ? O4 N C7 113.18(14) . . ? C2 C1 C12 113.88(16) . . ? C2 C1 H1A 105.0(12) . . ? C12 C1 H1A 108.9(12) . . ? C2 C1 H1B 109.9(13) . . ? C12 C1 H1B 110.7(13) . . ? H1A C1 H1B 108.2(18) . . ? O1 C2 C3 124.12(17) . . ? O1 C2 C1 116.02(16) . . ? C3 C2 C1 119.81(17) . . ? C4 C3 C2 121.91(18) . . ? C4 C3 H3 121.0(13) . . ? C2 C3 H3 117.0(13) . . ? O2 C4 C3 122.87(17) . . ? O2 C4 C31 115.56(16) . . ? C3 C4 C31 121.57(17) . . ? C6 C5 C22 110.65(15) . . ? C6 C5 H5A 106.3(12) . . ? C22 C5 H5A 110.7(11) . . ? C6 C5 H5B 112.3(13) . . ? C22 C5 H5B 111.5(13) . . ? H5A C5 H5B 105.2(17) . . ? O3 C6 N 115.69(16) . . ? O3 C6 C5 120.15(16) . . ? N C6 C5 124.16(16) . . ? N C7 H7A 108.6(14) . . ? N C7 H7B 108.5(12) . . ? H7A C7 H7B 111.5(19) . . ? N C7 H7C 107.6(13) . . ? H7A C7 H7C 111(2) . . ? H7B C7 H7C 109.3(18) . . ? C16 C11 C12 119.76(17) . . ? C16 C11 C21 119.50(17) . . ? C12 C11 C21 120.74(16) . . ? C13 C12 C11 118.54(17) . . ? C13 C12 C1 119.02(17) . . ? C11 C12 C1 122.43(16) . . ? C12 C13 C14 120.92(19) . . ? C12 C13 H13 118.8(14) . . ? C14 C13 H13 120.3(14) . . ? C13 C14 C15 120.39(19) . . ? C13 C14 H14 118.4(13) . . ? C15 C14 H14 121.1(13) . . ? C16 C15 C14 119.53(19) . . ? C16 C15 H15 117.6(14) . . ? C14 C15 H15 122.9(14) . . ? C15 C16 C11 120.81(19) . . ? C15 C16 H16 118.0(12) . . ? C11 C16 H16 121.2(12) . . ? C22 C21 C26 119.22(17) . . ? C22 C21 C11 121.18(16) . . ? C26 C21 C11 119.59(17) . . ? C23 C22 C21 118.31(17) . . ? C23 C22 C5 119.04(17) . . ? C21 C22 C5 122.58(16) . . ? C22 C23 C24 121.70(19) . . ? C22 C23 H23 116.2(12) . . ? C24 C23 H23 122.1(12) . . ? C25 C24 C23 120.04(19) . . ? C25 C24 H24 119.4(14) . . ? C23 C24 H24 120.4(14) . . ? C24 C25 C26 119.15(19) . . ? C24 C25 H25 123.9(13) . . ? C26 C25 H25 116.9(13) . . ? C25 C26 C21 121.50(19) . . ? C25 C26 H26 119.6(12) . . ? C21 C26 H26 118.9(12) . . ? C56 C51 C52 118.84(17) . . ? C56 C51 C61 118.15(17) . . ? C52 C51 C61 123.00(17) . . ? O5 C52 C53 117.09(16) . . ? O5 C52 C51 122.16(16) . . ? C53 C52 C51 120.74(17) . . ? C52 C53 C54 117.64(17) . . ? C52 C53 C57 120.26(17) . . ? C54 C53 C57 122.10(17) . . ? C53 C54 C55 123.38(18) . . ? C53 C54 H54 118.7(14) . . ? C55 C54 H54 117.9(14) . . ? C56 C55 C54 117.61(18) . . ? C56 C55 C58 120.90(18) . . ? C54 C55 C58 121.49(17) . . ? C55 C56 C51 121.75(18) . . ? C55 C56 H56 118.6(12) . . ? C51 C56 H56 119.6(12) . . ? C53 C57 H57A 109.4(14) . . ? C53 C57 H57B 113.4(15) . . ? H57A C57 H57B 108(2) . . ? C53 C57 H57C 111.6(13) . . ? H57A C57 H57C 109.4(19) . . ? H57B C57 H57C 105(2) . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62 C61 C66 118.19(17) . . ? C62 C61 C51 122.02(17) . . ? C66 C61 C51 119.74(17) . . ? O6 C62 C63 117.77(16) . . ? O6 C62 C61 121.54(16) . . ? C63 C62 C61 120.65(17) . . ? C62 C63 C64 118.54(17) . . ? C62 C63 C67 118.52(18) . . ? C64 C63 C67 122.89(18) . . ? C65 C64 C63 122.70(18) . . ? C65 C64 H64 118.8(14) . . ? C63 C64 H64 118.5(14) . . ? C66 C65 C64 117.22(18) . . ? C66 C65 C68 121.41(19) . . ? C64 C65 C68 121.36(18) . . ? C65 C66 C61 122.68(18) . . ? C65 C66 H66 118.0(13) . . ? C61 C66 H66 119.3(13) . . ? C63 C67 H67A 110.7(15) . . ? C63 C67 H67B 108.1(15) . . ? H67A C67 H67B 109(2) . . ? C63 C67 H67C 110.1(16) . . ? H67A C67 H67C 109(2) . . ? H67B C67 H67C 110(2) . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C32 C31 C36 118.43(18) . . ? C32 C31 C4 118.19(17) . . ? C36 C31 C4 123.36(17) . . ? C33 C32 C31 120.08(19) . . ? C33 C32 H32 120.4(13) . . ? C31 C32 H32 119.5(13) . . ? C32 C33 C34 121.47(19) . . ? C32 C33 H33 121.7(13) . . ? C34 C33 H33 116.8(13) . . ? C35 C34 C33 118.45(18) . . ? C35 C34 C37 120.8(2) . . ? C33 C34 C37 120.77(19) . . ? C36 C35 C34 120.6(2) . . ? C36 C35 H35 117.2(17) . . ? C34 C35 H35 122.2(17) . . ? C35 C36 C31 120.9(2) . . ? C35 C36 H36 117.1(13) . . ? C31 C36 H36 121.9(14) . . ? C34 C37 H37A 110.1(15) . . ? C34 C37 H37B 108.7(16) . . ? H37A C37 H37B 110(2) . . ? C34 C37 H37C 111.5(16) . . ? H37A C37 H37C 108(2) . . ? H37B C37 H37C 109(2) . . ? Cl2 C0 Cl3 109.61(12) . . ? Cl2 C0 Cl1 111.28(13) . . ? Cl3 C0 Cl1 110.53(12) . . ? Cl2 C0 H0 106.3(14) . . ? Cl3 C0 H0 110.2(14) . . ? Cl1 C0 H0 108.9(14) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.430 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.057 #=========END data_tetranitro _database_code_depnum_ccdc_archive 'CCDC 791675' #TrackingRef 'BiPhenOx-composite.cif' # Collected as mqg008 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2'-(4-p-tolyl-2,4-butanedionato)-biphenyl-2-N-methylacetohydroxamato)- (3,3',5,5'-tetranitrobiphenyl-2,2'-diolato)titanium(IV) dichloroform solvate ; _chemical_name_common '(Hob)Ti(O2C12H4[NO2]4) . 2 CHCl3' _chemical_melting_point ? _chemical_formula_moiety 'C38 H27 N5 O14 Ti, 2 (C H Cl3)' _chemical_formula_sum 'C40 H29 Cl6 N5 O14 Ti' _chemical_formula_weight 1064.28 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2931(4) _cell_length_b 13.3440(5) _cell_length_c 15.1141(6) _cell_angle_alpha 96.792(2) _cell_angle_beta 102.423(2) _cell_angle_gamma 93.434(3) _cell_volume 2200.11(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5632 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.94 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9139 _exptl_absorpt_correction_T_max 0.9571 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany. ; _exptl_crystal_recrystallization_method ; Crystals were grown by layering a concentrated solution of the complex in CHCl3 with hexane. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 33459 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.45 _reflns_number_total 9014 _reflns_number_gt 6501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. One of the lattice chloroforms (central carbon C01) was observed in two orientations, with the major orientation refining to 88.2(2)% occupancy. ; _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^)+(0.0514P)^2^+1.6477P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9014 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.54997(4) 0.73974(4) 0.10308(3) 0.01279(12) Uani 1 1 d . . . O1 O 0.51674(16) 0.83263(14) 0.00807(13) 0.0160(4) Uani 1 1 d . . . O2 O 0.42762(16) 0.80883(14) 0.15108(13) 0.0146(4) Uani 1 1 d . . . O3 O 0.41473(16) 0.64753(14) 0.02153(13) 0.0152(4) Uani 1 1 d . . . O4 O 0.63069(16) 0.65832(14) 0.02163(13) 0.0148(4) Uani 1 1 d . . . O5 O 0.58227(16) 0.66443(14) 0.20524(13) 0.0141(4) Uani 1 1 d . . . O6 O 0.70373(16) 0.81308(14) 0.15069(13) 0.0131(4) Uani 1 1 d . . . O11 O 0.42553(18) 0.72841(17) 0.41204(15) 0.0259(5) Uani 1 1 d . . . O12 O 0.41888(19) 0.60604(18) 0.30321(15) 0.0330(6) Uani 1 1 d . . . O21 O 0.8485(2) 0.80839(19) -0.05974(16) 0.0364(6) Uani 1 1 d . . . O22 O 0.8124(2) 0.92302(16) 0.04333(16) 0.0283(5) Uani 1 1 d . . . O31 O 0.82329(18) 0.80027(17) 0.61787(14) 0.0257(5) Uani 1 1 d . . . O32 O 0.98433(17) 0.79062(16) 0.56253(14) 0.0220(5) Uani 1 1 d . . . O41 O 1.1504(3) 0.5918(3) 0.08230(19) 0.0665(10) Uani 1 1 d . . . O42 O 1.14582(18) 0.55018(16) 0.21399(14) 0.0224(5) Uani 1 1 d . . . N N 0.5541(2) 0.60702(17) -0.05567(16) 0.0154(5) Uani 1 1 d . . . N1 N 0.4734(2) 0.67525(19) 0.35964(17) 0.0201(6) Uani 1 1 d . . . N2 N 0.8414(2) 0.8390(2) 0.01866(18) 0.0216(6) Uani 1 1 d . . . N3 N 0.8736(2) 0.78054(18) 0.55465(16) 0.0174(5) Uani 1 1 d . . . N4 N 1.1075(2) 0.5947(2) 0.14950(17) 0.0215(6) Uani 1 1 d . . . C1 C 0.4039(3) 0.9042(2) -0.1162(2) 0.0170(6) Uani 1 1 d . . . C2 C 0.4148(2) 0.8669(2) -0.02453(19) 0.0143(6) Uani 1 1 d . . . C3 C 0.3211(3) 0.8739(2) 0.0223(2) 0.0154(6) Uani 1 1 d . . . C4 C 0.3338(2) 0.8522(2) 0.11077(19) 0.0136(6) Uani 1 1 d . . . C5 C 0.3376(3) 0.5560(2) -0.1293(2) 0.0158(6) Uani 1 1 d . . . C6 C 0.4389(2) 0.6041(2) -0.05251(19) 0.0135(6) Uani 1 1 d . . . C7 C 0.6161(3) 0.5648(3) -0.1245(2) 0.0196(7) Uani 1 1 d . . . C11 C 0.3691(3) 0.7382(2) -0.22609(19) 0.0166(6) Uani 1 1 d . . . C12 C 0.4411(2) 0.8285(2) -0.18627(19) 0.0156(6) Uani 1 1 d . . . C13 C 0.5504(3) 0.8502(2) -0.2126(2) 0.0238(7) Uani 1 1 d . . . C14 C 0.5871(3) 0.7851(3) -0.2777(2) 0.0306(8) Uani 1 1 d . . . C15 C 0.5150(3) 0.6982(3) -0.3190(2) 0.0292(8) Uani 1 1 d . . . C16 C 0.4072(3) 0.6743(2) -0.2929(2) 0.0227(7) Uani 1 1 d . . . C21 C 0.2525(2) 0.7099(2) -0.19964(19) 0.0154(6) Uani 1 1 d . . . C22 C 0.2382(2) 0.6262(2) -0.15367(18) 0.0146(6) Uani 1 1 d . . . C23 C 0.1277(3) 0.6055(2) -0.1292(2) 0.0182(6) Uani 1 1 d . . . C24 C 0.0319(3) 0.6642(2) -0.1517(2) 0.0209(7) Uani 1 1 d . . . C25 C 0.0445(3) 0.7450(2) -0.1994(2) 0.0224(7) Uani 1 1 d . . . C26 C 0.1540(3) 0.7675(2) -0.2224(2) 0.0204(6) Uani 1 1 d . . . C51 C 0.7809(2) 0.7078(2) 0.30179(19) 0.0133(6) Uani 1 1 d . . . C52 C 0.6523(2) 0.6882(2) 0.28789(19) 0.0128(6) Uani 1 1 d . . . C53 C 0.6047(2) 0.6963(2) 0.36703(19) 0.0147(6) Uani 1 1 d . . . C54 C 0.6743(3) 0.7279(2) 0.4535(2) 0.0158(6) Uani 1 1 d . . . C55 C 0.7979(2) 0.7453(2) 0.46376(19) 0.0144(6) Uani 1 1 d . . . C56 C 0.8513(2) 0.7338(2) 0.38933(19) 0.0144(6) Uani 1 1 d . . . C61 C 0.8434(2) 0.7055(2) 0.22399(18) 0.0124(6) Uani 1 1 d . . . C62 C 0.8054(2) 0.7662(2) 0.15494(19) 0.0133(6) Uani 1 1 d . . . C63 C 0.8741(2) 0.7719(2) 0.08835(19) 0.0150(6) Uani 1 1 d . . . C64 C 0.9714(2) 0.7155(2) 0.0844(2) 0.0163(6) Uani 1 1 d . . . C65 C 1.0046(2) 0.6559(2) 0.15255(19) 0.0154(6) Uani 1 1 d . . . C66 C 0.9433(2) 0.6507(2) 0.2224(2) 0.0149(6) Uani 1 1 d . . . C31 C 0.2446(2) 0.8784(2) 0.16646(19) 0.0149(6) Uani 1 1 d . . . C32 C 0.2438(3) 0.8321(2) 0.2447(2) 0.0182(6) Uani 1 1 d . . . C33 C 0.1621(3) 0.8574(2) 0.2985(2) 0.0198(6) Uani 1 1 d . . . C34 C 0.0808(3) 0.9300(2) 0.2770(2) 0.0208(7) Uani 1 1 d . . . C35 C 0.0831(3) 0.9765(2) 0.1994(2) 0.0218(7) Uani 1 1 d . . . C36 C 0.1635(3) 0.9516(2) 0.1446(2) 0.0187(6) Uani 1 1 d . . . C37 C -0.0061(3) 0.9596(3) 0.3362(3) 0.0295(8) Uani 1 1 d . . . H1A H 0.321(3) 0.918(2) -0.140(2) 0.019(8) Uiso 1 1 d . . . H1B H 0.461(3) 0.969(2) -0.1052(19) 0.016(7) Uiso 1 1 d . . . H3 H 0.253(3) 0.897(2) -0.005(2) 0.014(8) Uiso 1 1 d . . . H5A H 0.308(3) 0.500(2) -0.108(2) 0.017(8) Uiso 1 1 d . . . H5B H 0.371(2) 0.532(2) -0.1794(19) 0.008(7) Uiso 1 1 d . . . H7A H 0.556(3) 0.526(2) -0.172(2) 0.029(9) Uiso 1 1 d . . . H7B H 0.655(3) 0.617(2) -0.147(2) 0.015(8) Uiso 1 1 d . . . H7C H 0.672(3) 0.521(3) -0.095(2) 0.036(10) Uiso 1 1 d . . . H13 H 0.597(3) 0.909(2) -0.185(2) 0.021(8) Uiso 1 1 d . . . H14 H 0.659(3) 0.800(2) -0.292(2) 0.031(9) Uiso 1 1 d . . . H15 H 0.533(3) 0.656(3) -0.367(3) 0.050(12) Uiso 1 1 d . . . H16 H 0.353(3) 0.611(2) -0.327(2) 0.026(9) Uiso 1 1 d . . . H23 H 0.122(3) 0.549(2) -0.091(2) 0.019(8) Uiso 1 1 d . . . H24 H -0.038(3) 0.648(2) -0.135(2) 0.019(8) Uiso 1 1 d . . . H25 H -0.022(3) 0.785(2) -0.218(2) 0.024(9) Uiso 1 1 d . . . H26 H 0.161(3) 0.823(2) -0.258(2) 0.026(9) Uiso 1 1 d . . . H54 H 0.640(3) 0.734(2) 0.499(2) 0.014(8) Uiso 1 1 d . . . H56 H 0.935(3) 0.748(2) 0.398(2) 0.019(8) Uiso 1 1 d . . . H64 H 1.014(3) 0.723(2) 0.038(2) 0.021(8) Uiso 1 1 d . . . H66 H 0.971(3) 0.614(2) 0.265(2) 0.022(9) Uiso 1 1 d . . . H32 H 0.295(3) 0.783(2) 0.258(2) 0.017(8) Uiso 1 1 d . . . H33 H 0.166(2) 0.824(2) 0.353(2) 0.012(7) Uiso 1 1 d . . . H35 H 0.030(3) 1.026(2) 0.186(2) 0.017(8) Uiso 1 1 d . . . H36 H 0.163(2) 0.985(2) 0.093(2) 0.013(7) Uiso 1 1 d . . . H37A H -0.082(4) 0.931(3) 0.313(3) 0.046(11) Uiso 1 1 d . . . H37B H -0.003(3) 1.030(3) 0.347(2) 0.036(10) Uiso 1 1 d . . . H37C H 0.021(4) 0.949(3) 0.402(3) 0.062(14) Uiso 1 1 d . . . C01 C 0.3683(3) -0.0364(3) 0.5748(2) 0.0293(8) Uani 1 1 d . . . H01 H 0.426(3) -0.087(3) 0.572(2) 0.029(9) Uiso 1 1 d . A 1 Cl11 Cl 0.42989(12) 0.05126(7) 0.67122(7) 0.0385(3) Uani 0.882(2) 1 d P B 1 Cl12 Cl 0.23105(10) -0.09939(10) 0.58393(8) 0.0400(3) Uani 0.882(2) 1 d P B 1 Cl13 Cl 0.34094(8) 0.02399(7) 0.47547(6) 0.0338(2) Uani 1 1 d . B . Cl14 Cl 0.3537(10) 0.0447(6) 0.6849(5) 0.0385(3) Uani 0.118(2) 1 d P B 2 Cl15 Cl 0.2613(9) -0.1397(8) 0.5698(7) 0.0400(3) Uani 0.118(2) 1 d P B 2 C02 C 0.2112(3) 0.5466(2) -0.5767(2) 0.0228(7) Uani 1 1 d . . . H02 H 0.234(3) 0.571(2) -0.630(2) 0.028(9) Uiso 1 1 d . . . Cl21 Cl 0.09749(9) 0.44590(7) -0.61284(7) 0.0495(3) Uani 1 1 d . . . Cl22 Cl 0.16003(9) 0.64580(8) -0.51255(7) 0.0443(2) Uani 1 1 d . . . Cl23 Cl 0.34584(7) 0.50633(6) -0.51275(6) 0.02825(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0108(2) 0.0143(3) 0.0137(3) 0.0016(2) 0.00331(19) 0.00336(19) O1 0.0138(9) 0.0178(10) 0.0174(11) 0.0051(8) 0.0038(8) 0.0033(8) O2 0.0116(9) 0.0168(10) 0.0166(10) 0.0025(8) 0.0046(8) 0.0044(8) O3 0.0144(9) 0.0168(10) 0.0146(11) 0.0008(8) 0.0043(8) 0.0030(8) O4 0.0113(9) 0.0179(10) 0.0144(10) -0.0009(8) 0.0020(8) 0.0044(8) O5 0.0123(9) 0.0147(10) 0.0154(10) 0.0008(8) 0.0036(8) 0.0016(8) O6 0.0118(9) 0.0143(10) 0.0148(10) 0.0028(8) 0.0046(7) 0.0047(8) O11 0.0188(11) 0.0365(13) 0.0269(13) 0.0054(10) 0.0137(9) 0.0066(10) O12 0.0223(11) 0.0482(15) 0.0242(13) -0.0071(11) 0.0077(10) -0.0165(11) O21 0.0525(16) 0.0445(15) 0.0236(13) 0.0181(11) 0.0198(11) 0.0270(12) O22 0.0339(13) 0.0214(12) 0.0383(14) 0.0153(10) 0.0185(11) 0.0131(10) O31 0.0222(11) 0.0404(14) 0.0147(11) -0.0004(10) 0.0068(9) 0.0037(10) O32 0.0134(10) 0.0303(12) 0.0209(12) 0.0013(9) 0.0020(8) 0.0009(9) O41 0.074(2) 0.116(3) 0.0417(17) 0.0475(18) 0.0448(16) 0.080(2) O42 0.0185(10) 0.0306(12) 0.0222(12) 0.0117(10) 0.0061(9) 0.0128(9) N 0.0168(12) 0.0160(13) 0.0130(12) 0.0007(10) 0.0023(9) 0.0044(10) N1 0.0145(12) 0.0293(15) 0.0178(14) 0.0069(12) 0.0054(10) -0.0019(11) N2 0.0193(13) 0.0249(15) 0.0264(16) 0.0119(12) 0.0116(11) 0.0092(11) N3 0.0184(12) 0.0192(13) 0.0148(13) 0.0017(10) 0.0036(10) 0.0039(10) N4 0.0182(12) 0.0298(15) 0.0192(14) 0.0053(12) 0.0064(11) 0.0116(11) C1 0.0180(15) 0.0135(15) 0.0195(16) 0.0038(12) 0.0032(12) 0.0024(12) C2 0.0172(14) 0.0098(14) 0.0148(15) 0.0005(11) 0.0023(11) -0.0001(11) C3 0.0130(14) 0.0140(15) 0.0192(16) 0.0048(12) 0.0005(11) 0.0052(11) C4 0.0113(13) 0.0093(13) 0.0198(15) 0.0001(11) 0.0035(11) 0.0020(11) C5 0.0189(14) 0.0112(14) 0.0179(16) 0.0013(12) 0.0050(12) 0.0027(12) C6 0.0175(14) 0.0092(13) 0.0148(15) 0.0043(11) 0.0032(11) 0.0043(11) C7 0.0183(15) 0.0255(18) 0.0160(16) -0.0008(14) 0.0067(13) 0.0064(14) C11 0.0186(14) 0.0173(15) 0.0147(15) 0.0044(12) 0.0035(11) 0.0039(12) C12 0.0177(14) 0.0179(15) 0.0135(15) 0.0058(12) 0.0054(11) 0.0055(11) C13 0.0240(16) 0.0215(17) 0.0284(18) 0.0088(14) 0.0088(14) -0.0001(14) C14 0.0278(18) 0.035(2) 0.036(2) 0.0074(16) 0.0192(16) 0.0046(15) C15 0.039(2) 0.0284(19) 0.0258(19) 0.0022(15) 0.0182(15) 0.0082(15) C16 0.0290(17) 0.0218(17) 0.0190(17) 0.0044(13) 0.0076(13) 0.0044(14) C21 0.0169(14) 0.0161(15) 0.0112(14) -0.0024(12) 0.0008(11) 0.0016(11) C22 0.0176(14) 0.0140(14) 0.0102(14) -0.0035(11) 0.0017(11) 0.0011(11) C23 0.0204(15) 0.0167(15) 0.0160(16) -0.0007(13) 0.0025(12) 0.0004(12) C24 0.0165(15) 0.0242(17) 0.0197(17) -0.0044(13) 0.0039(12) -0.0004(13) C25 0.0182(15) 0.0238(17) 0.0220(17) -0.0008(14) -0.0018(12) 0.0070(13) C26 0.0228(15) 0.0186(16) 0.0178(16) 0.0031(13) -0.0005(12) 0.0031(13) C51 0.0137(13) 0.0116(14) 0.0164(15) 0.0043(11) 0.0054(11) 0.0031(11) C52 0.0148(13) 0.0102(14) 0.0147(15) 0.0025(11) 0.0053(11) 0.0031(11) C53 0.0136(13) 0.0142(14) 0.0177(15) 0.0032(12) 0.0059(11) 0.0002(11) C54 0.0195(14) 0.0175(15) 0.0130(15) 0.0048(12) 0.0075(12) 0.0028(12) C55 0.0154(13) 0.0149(14) 0.0124(14) 0.0025(11) 0.0016(11) 0.0020(11) C56 0.0103(13) 0.0154(14) 0.0193(16) 0.0046(12) 0.0050(11) 0.0035(11) C61 0.0108(12) 0.0123(14) 0.0138(14) 0.0029(11) 0.0016(10) 0.0006(10) C62 0.0119(13) 0.0114(14) 0.0157(15) -0.0012(11) 0.0033(11) -0.0003(11) C63 0.0158(14) 0.0149(15) 0.0155(15) 0.0052(12) 0.0039(11) 0.0030(11) C64 0.0146(13) 0.0200(16) 0.0161(15) 0.0024(12) 0.0075(12) 0.0029(11) C65 0.0113(13) 0.0194(15) 0.0158(15) 0.0026(12) 0.0027(11) 0.0043(11) C66 0.0153(14) 0.0162(15) 0.0131(15) 0.0041(12) 0.0020(11) 0.0015(11) C31 0.0135(13) 0.0126(14) 0.0196(16) 0.0014(12) 0.0063(11) 0.0014(11) C32 0.0156(14) 0.0168(16) 0.0223(17) 0.0012(13) 0.0051(12) 0.0027(12) C33 0.0212(15) 0.0182(16) 0.0211(17) 0.0025(13) 0.0080(12) -0.0004(12) C34 0.0187(15) 0.0154(15) 0.0288(18) -0.0034(13) 0.0117(13) -0.0035(12) C35 0.0157(14) 0.0157(16) 0.036(2) 0.0030(14) 0.0097(13) 0.0059(13) C36 0.0179(14) 0.0147(15) 0.0264(18) 0.0060(13) 0.0086(12) 0.0038(12) C37 0.0262(18) 0.0229(19) 0.042(2) -0.0061(17) 0.0206(16) 0.0010(15) C01 0.0292(18) 0.0228(18) 0.038(2) 0.0056(15) 0.0115(15) 0.0026(15) Cl11 0.0558(8) 0.0250(5) 0.0286(5) 0.0029(4) -0.0019(5) -0.0024(5) Cl12 0.0318(6) 0.0426(8) 0.0496(7) 0.0053(6) 0.0202(5) -0.0032(5) Cl13 0.0328(4) 0.0356(5) 0.0319(5) 0.0045(4) 0.0056(4) 0.0006(4) Cl14 0.0558(8) 0.0250(5) 0.0286(5) 0.0029(4) -0.0019(5) -0.0024(5) Cl15 0.0318(6) 0.0426(8) 0.0496(7) 0.0053(6) 0.0202(5) -0.0032(5) C02 0.0234(16) 0.0234(17) 0.0210(17) 0.0052(14) 0.0032(13) 0.0004(13) Cl21 0.0480(6) 0.0398(5) 0.0500(6) 0.0213(5) -0.0140(5) -0.0206(5) Cl22 0.0422(5) 0.0529(6) 0.0394(6) 0.0024(5) 0.0083(4) 0.0286(5) Cl23 0.0282(4) 0.0273(4) 0.0293(5) 0.0056(3) 0.0033(3) 0.0114(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O6 1.8929(18) . ? Ti O5 1.9224(19) . ? Ti O2 1.9264(19) . ? Ti O4 1.9524(19) . ? Ti O3 1.9929(19) . ? Ti O1 1.9960(19) . ? O1 C2 1.284(3) . ? O2 C4 1.307(3) . ? O3 C6 1.288(3) . ? O4 N 1.374(3) . ? O5 C52 1.318(3) . ? O6 C62 1.334(3) . ? O11 N1 1.233(3) . ? O12 N1 1.216(3) . ? O21 N2 1.228(3) . ? O22 N2 1.226(3) . ? O31 N3 1.223(3) . ? O32 N3 1.228(3) . ? O41 N4 1.214(3) . ? O42 N4 1.215(3) . ? N C6 1.310(3) . ? N C7 1.453(4) . ? N1 C53 1.470(3) . ? N2 C63 1.464(4) . ? N3 C55 1.460(3) . ? N4 C65 1.465(4) . ? C1 C2 1.510(4) . ? C1 C12 1.520(4) . ? C1 H1A 0.97(3) . ? C1 H1B 1.02(3) . ? C2 C3 1.395(4) . ? C3 C4 1.382(4) . ? C3 H3 0.88(3) . ? C4 C31 1.477(4) . ? C5 C6 1.495(4) . ? C5 C22 1.517(4) . ? C5 H5A 0.93(3) . ? C5 H5B 0.95(3) . ? C7 H7A 0.95(3) . ? C7 H7B 0.94(3) . ? C7 H7C 0.96(4) . ? C11 C16 1.399(4) . ? C11 C12 1.405(4) . ? C11 C21 1.496(4) . ? C12 C13 1.401(4) . ? C13 C14 1.382(5) . ? C13 H13 0.92(3) . ? C14 C15 1.376(5) . ? C14 H14 0.90(3) . ? C15 C16 1.390(4) . ? C15 H15 0.93(4) . ? C16 H16 1.03(3) . ? C21 C26 1.395(4) . ? C21 C22 1.403(4) . ? C22 C23 1.397(4) . ? C23 C24 1.381(4) . ? C23 H23 1.00(3) . ? C24 C25 1.383(4) . ? C24 H24 0.89(3) . ? C25 C26 1.380(4) . ? C25 H25 0.96(3) . ? C26 H26 0.97(3) . ? C51 C56 1.382(4) . ? C51 C52 1.425(4) . ? C51 C61 1.495(4) . ? C52 C53 1.409(4) . ? C53 C54 1.375(4) . ? C54 C55 1.374(4) . ? C54 H54 0.86(3) . ? C55 C56 1.383(4) . ? C56 H56 0.93(3) . ? C61 C66 1.383(4) . ? C61 C62 1.406(4) . ? C62 C63 1.403(4) . ? C63 C64 1.376(4) . ? C64 C65 1.378(4) . ? C64 H64 0.95(3) . ? C65 C66 1.387(4) . ? C66 H66 0.87(3) . ? C31 C32 1.398(4) . ? C31 C36 1.398(4) . ? C32 C33 1.386(4) . ? C32 H32 0.91(3) . ? C33 C34 1.393(4) . ? C33 H33 0.97(3) . ? C34 C35 1.394(4) . ? C34 C37 1.504(4) . ? C35 C36 1.384(4) . ? C35 H35 0.93(3) . ? C36 H36 0.94(3) . ? C37 H37A 0.90(4) . ? C37 H37B 0.93(4) . ? C37 H37C 1.00(4) . ? C01 Cl11 1.744(4) . ? C01 Cl12 1.758(3) . ? C01 Cl15 1.761(10) . ? C01 Cl13 1.765(4) . ? C01 Cl14 1.919(9) . ? C01 H01 0.97(3) . ? C02 Cl22 1.748(3) . ? C02 Cl21 1.752(3) . ? C02 Cl23 1.767(3) . ? C02 H02 0.98(3) . ? 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 O6 Ti O5 88.14(8) . . ? O6 Ti O2 109.37(8) . . ? O5 Ti O2 91.45(8) . . ? O6 Ti O4 86.17(8) . . ? O5 Ti O4 98.45(8) . . ? O2 Ti O4 161.91(8) . . ? O6 Ti O3 161.69(8) . . ? O5 Ti O3 99.11(8) . . ? O2 Ti O3 87.37(8) . . ? O4 Ti O3 76.18(8) . . ? O6 Ti O1 88.84(8) . . ? O5 Ti O1 173.06(8) . . ? O2 Ti O1 83.66(8) . . ? O4 Ti O1 87.58(8) . . ? O3 Ti O1 85.62(8) . . ? C2 O1 Ti 127.40(17) . . ? C4 O2 Ti 131.34(18) . . ? C6 O3 Ti 115.36(16) . . ? N O4 Ti 114.78(15) . . ? C52 O5 Ti 131.19(17) . . ? C62 O6 Ti 120.19(16) . . ? C6 N O4 113.6(2) . . ? C6 N C7 132.3(2) . . ? O4 N C7 114.1(2) . . ? O12 N1 O11 124.0(2) . . ? O12 N1 C53 118.3(2) . . ? O11 N1 C53 117.7(2) . . ? O22 N2 O21 124.6(3) . . ? O22 N2 C63 117.6(2) . . ? O21 N2 C63 117.8(2) . . ? O31 N3 O32 123.9(2) . . ? O31 N3 C55 118.4(2) . . ? O32 N3 C55 117.7(2) . . ? O41 N4 O42 123.4(3) . . ? O41 N4 C65 117.8(2) . . ? O42 N4 C65 118.8(2) . . ? C2 C1 C12 112.7(2) . . ? C2 C1 H1A 110.4(18) . . ? C12 C1 H1A 108.0(18) . . ? C2 C1 H1B 106.5(16) . . ? C12 C1 H1B 108.9(16) . . ? H1A C1 H1B 110(2) . . ? O1 C2 C3 123.1(3) . . ? O1 C2 C1 115.6(2) . . ? C3 C2 C1 121.3(3) . . ? C4 C3 C2 122.7(3) . . ? C4 C3 H3 119.1(19) . . ? C2 C3 H3 118.1(19) . . ? O2 C4 C3 121.6(2) . . ? O2 C4 C31 115.8(2) . . ? C3 C4 C31 122.5(3) . . ? C6 C5 C22 112.3(2) . . ? C6 C5 H5A 104.3(18) . . ? C22 C5 H5A 110.5(19) . . ? C6 C5 H5B 108.5(16) . . ? C22 C5 H5B 113.2(17) . . ? H5A C5 H5B 108(2) . . ? O3 C6 N 116.3(2) . . ? O3 C6 C5 119.8(2) . . ? N C6 C5 123.8(3) . . ? N C7 H7A 107(2) . . ? N C7 H7B 110.3(18) . . ? H7A C7 H7B 111(3) . . ? N C7 H7C 106(2) . . ? H7A C7 H7C 110(3) . . ? H7B C7 H7C 113(3) . . ? C16 C11 C12 118.9(3) . . ? C16 C11 C21 119.6(3) . . ? C12 C11 C21 121.5(2) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 C1 118.6(3) . . ? C11 C12 C1 122.3(2) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H13 121.3(19) . . ? C12 C13 H13 117.8(19) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 120(2) . . ? C13 C14 H14 119(2) . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 123(2) . . ? C16 C15 H15 118(2) . . ? C15 C16 C11 121.1(3) . . ? C15 C16 H16 118.1(18) . . ? C11 C16 H16 120.7(18) . . ? C26 C21 C22 118.7(3) . . ? C26 C21 C11 119.3(3) . . ? C22 C21 C11 122.1(2) . . ? C23 C22 C21 119.0(3) . . ? C23 C22 C5 118.0(3) . . ? C21 C22 C5 123.0(2) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H23 120.9(17) . . ? C22 C23 H23 117.8(17) . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 118(2) . . ? C25 C24 H24 122(2) . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H25 119.2(19) . . ? C24 C25 H25 121.3(19) . . ? C25 C26 C21 121.7(3) . . ? C25 C26 H26 118.8(19) . . ? C21 C26 H26 119.5(19) . . ? C56 C51 C52 119.9(2) . . ? C56 C51 C61 117.9(2) . . ? C52 C51 C61 122.2(2) . . ? O5 C52 C53 122.2(2) . . ? O5 C52 C51 121.5(2) . . ? C53 C52 C51 116.4(2) . . ? C54 C53 C52 123.4(2) . . ? C54 C53 N1 116.2(2) . . ? C52 C53 N1 120.3(2) . . ? C55 C54 C53 118.1(3) . . ? C55 C54 H54 123(2) . . ? C53 C54 H54 119(2) . . ? C54 C55 C56 121.3(3) . . ? C54 C55 N3 119.1(2) . . ? C56 C55 N3 119.5(2) . . ? C51 C56 C55 120.7(3) . . ? C51 C56 H56 119.5(18) . . ? C55 C56 H56 119.7(18) . . ? C66 C61 C62 119.6(3) . . ? C66 C61 C51 121.0(2) . . ? C62 C61 C51 119.2(2) . . ? O6 C62 C63 121.1(2) . . ? O6 C62 C61 120.7(2) . . ? C63 C62 C61 118.1(2) . . ? C64 C63 C62 122.8(3) . . ? C64 C63 N2 117.6(2) . . ? C62 C63 N2 119.6(2) . . ? C63 C64 C65 117.1(3) . . ? C63 C64 H64 119.0(19) . . ? C65 C64 H64 123.8(19) . . ? C64 C65 C66 122.5(3) . . ? C64 C65 N4 118.2(2) . . ? C66 C65 N4 119.3(3) . . ? C61 C66 C65 119.7(3) . . ? C61 C66 H66 122(2) . . ? C65 C66 H66 118(2) . . ? C32 C31 C36 118.9(3) . . ? C32 C31 C4 119.6(3) . . ? C36 C31 C4 121.4(3) . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 120.7(19) . . ? C31 C32 H32 119.0(19) . . ? C32 C33 C34 121.1(3) . . ? C32 C33 H33 116.9(17) . . ? C34 C33 H33 121.9(17) . . ? C33 C34 C35 118.2(3) . . ? C33 C34 C37 121.4(3) . . ? C35 C34 C37 120.3(3) . . ? C36 C35 C34 121.3(3) . . ? C36 C35 H35 120.3(19) . . ? C34 C35 H35 118.4(19) . . ? C35 C36 C31 120.1(3) . . ? C35 C36 H36 118.9(18) . . ? C31 C36 H36 121.0(18) . . ? C34 C37 H37A 113(2) . . ? C34 C37 H37B 109(2) . . ? H37A C37 H37B 112(3) . . ? C34 C37 H37C 115(3) . . ? H37A C37 H37C 110(3) . . ? H37B C37 H37C 97(3) . . ? Cl11 C01 Cl12 111.5(2) . . ? Cl11 C01 Cl15 125.5(4) . . ? Cl12 C01 Cl15 22.6(3) . . ? Cl11 C01 Cl13 110.59(18) . . ? Cl12 C01 Cl13 108.81(19) . . ? Cl15 C01 Cl13 113.2(4) . . ? Cl11 C01 Cl14 28.9(3) . . ? Cl12 C01 Cl14 83.6(3) . . ? Cl15 C01 Cl14 100.9(4) . . ? Cl13 C01 Cl14 115.5(3) . . ? Cl11 C01 H01 107(2) . . ? Cl12 C01 H01 107.4(19) . . ? Cl15 C01 H01 85.6(19) . . ? Cl13 C01 H01 112(2) . . ? Cl14 C01 H01 124(2) . . ? Cl22 C02 Cl21 110.47(18) . . ? Cl22 C02 Cl23 110.42(17) . . ? Cl21 C02 Cl23 111.09(18) . . ? Cl22 C02 H02 109.6(19) . . ? Cl21 C02 H02 109.8(19) . . ? Cl23 C02 H02 105.4(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.743 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.076 _vrf_PLAT220_tetranitro ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.03 Ratio RESPONSE: O41 is a peripheral nitro oxygen exhibting some thermal motion. This slightly large thermal ellipse does not affect the structure or discussion based thereon. ; #==========END data_hoxbiphen _database_code_depnum_ccdc_archive 'CCDC 791676' #TrackingRef 'BiPhenOx-composite.cif' # Created as sb007 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,2'-Biphenylbis(N-methylacetohydroxamato))- (3,3',5,5'-tetramethylbiphenyl-2,2'-diolato)titanium(IV) deuterodichloromethane solvate ; _chemical_name_common '(Hox)Ti(O2C12H4Me4) . CD2Cl2' _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 N2 O6 Ti, C D2 Cl2' _chemical_formula_sum 'C35 H34 D2 Cl2 N2 O6 Ti' _chemical_formula_weight 701.46 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3148(13) _cell_length_b 13.2234(14) _cell_length_c 20.372(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.7950(16) _cell_angle_gamma 90.00 _cell_volume 3305.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.20 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.9635 _exptl_absorpt_process_details ; Blessing, R. H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G. M. (2004) SADABS, University of G\"ottingen, Germany. ; _exptl_crystal_recrystallization_method ; Crystals were deposited from a concentrated solution of the complex in CD2Cl2. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 47756 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6802 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0415P)^2^+1.7666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6802 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti -0.83629(2) -0.96424(2) -0.124817(13) 0.01277(8) Uani 1 1 d . . . O1 O -0.87813(8) -1.10618(8) -0.09226(5) 0.0159(2) Uani 1 1 d . . . O2 O -0.96573(9) -0.93979(8) -0.07745(5) 0.0156(2) Uani 1 1 d . . . O3 O -0.95239(9) -0.98954(8) -0.20160(5) 0.0163(2) Uani 1 1 d . . . O4 O -0.75762(9) -1.03660(8) -0.18982(5) 0.0177(2) Uani 1 1 d . . . O5 O -0.82343(8) -0.82636(8) -0.13982(5) 0.0146(2) Uani 1 1 d . . . O6 O -0.71405(8) -0.96206(8) -0.06483(5) 0.0148(2) Uani 1 1 d . . . N1 N -1.02923(10) -1.02506(10) -0.07362(6) 0.0149(3) Uani 1 1 d . . . N2 N -0.82355(11) -1.08555(10) -0.23773(6) 0.0170(3) Uani 1 1 d . . . C1 C -1.03285(14) -1.21206(13) -0.07681(8) 0.0188(3) Uani 1 1 d . . . C2 C -0.97879(12) -1.11085(12) -0.08144(7) 0.0151(3) Uani 1 1 d . . . C3 C -1.14416(13) -1.00401(15) -0.06904(9) 0.0206(4) Uani 1 1 d . . . C4 C -1.01153(14) -1.10208(13) -0.28978(8) 0.0183(3) Uani 1 1 d . . . C5 C -0.92593(13) -1.05778(12) -0.24153(8) 0.0153(3) Uani 1 1 d . . . C6 C -0.76933(16) -1.16420(15) -0.27244(10) 0.0253(4) Uani 1 1 d . . . C11 C -1.04415(13) -1.27412(12) -0.19625(8) 0.0176(3) Uani 1 1 d . . . C12 C -0.99973(13) -1.28242(12) -0.13062(8) 0.0176(3) Uani 1 1 d . . . C13 C -0.91981(14) -1.35532(13) -0.11511(9) 0.0227(4) Uani 1 1 d . . . C14 C -0.88337(15) -1.41851(14) -0.16270(10) 0.0267(4) Uani 1 1 d . . . C15 C -0.92598(14) -1.40998(13) -0.22756(9) 0.0250(4) Uani 1 1 d . . . C16 C -1.00642(14) -1.33858(13) -0.24365(9) 0.0208(4) Uani 1 1 d . . . C21 C -1.13303(13) -1.20001(13) -0.21600(8) 0.0177(3) Uani 1 1 d . . . C22 C -1.11756(13) -1.11894(13) -0.25864(8) 0.0183(3) Uani 1 1 d . . . C23 C -1.20285(15) -1.05055(15) -0.27255(9) 0.0257(4) Uani 1 1 d . . . C24 C -1.30329(15) -1.06389(16) -0.24769(10) 0.0313(4) Uani 1 1 d . . . C25 C -1.32006(15) -1.14592(17) -0.20838(10) 0.0310(4) Uani 1 1 d . . . C26 C -1.23517(14) -1.21305(15) -0.19196(9) 0.0241(4) Uani 1 1 d . . . C51 C -0.71898(12) -0.74412(11) -0.05022(7) 0.0138(3) Uani 1 1 d . . . C52 C -0.81553(12) -0.75491(11) -0.09164(7) 0.0136(3) Uani 1 1 d . . . C53 C -0.90396(12) -0.68912(12) -0.08644(8) 0.0158(3) Uani 1 1 d . . . C54 C -0.89564(13) -0.61529(12) -0.03777(8) 0.0167(3) Uani 1 1 d . . . C55 C -0.80317(13) -0.60499(12) 0.00615(8) 0.0167(3) Uani 1 1 d . . . C56 C -0.71583(13) -0.66950(12) -0.00133(8) 0.0155(3) Uani 1 1 d . . . C57 C -1.00423(14) -0.69928(15) -0.13365(9) 0.0217(4) Uani 1 1 d . . . C58 C -0.79844(15) -0.52723(14) 0.06018(9) 0.0220(4) Uani 1 1 d . . . C61 C -0.61915(12) -0.80337(12) -0.06081(7) 0.0145(3) Uani 1 1 d . . . C62 C -0.62062(12) -0.90874(12) -0.06912(7) 0.0141(3) Uani 1 1 d . . . C63 C -0.52497(13) -0.96186(12) -0.08007(7) 0.0151(3) Uani 1 1 d . . . C64 C -0.42817(13) -0.90809(13) -0.08157(8) 0.0177(3) Uani 1 1 d . . . C65 C -0.42299(13) -0.80366(13) -0.07238(8) 0.0176(3) Uani 1 1 d . . . C66 C -0.51902(13) -0.75288(12) -0.06232(8) 0.0156(3) Uani 1 1 d . . . C67 C -0.52936(14) -1.07444(13) -0.08923(9) 0.0192(3) Uani 1 1 d . . . C68 C -0.31586(14) -0.74818(15) -0.07361(10) 0.0255(4) Uani 1 1 d . . . C0 C -0.60930(17) -0.32516(14) -0.09895(9) 0.0261(4) Uani 1 1 d . . . Cl1 Cl -0.55090(5) -0.33052(4) -0.17463(3) 0.04428(15) Uani 1 1 d . . . Cl2 Cl -0.61809(4) -0.44680(4) -0.06372(2) 0.03472(12) Uani 1 1 d . . . H1A H -1.1122(16) -1.2055(14) -0.0769(9) 0.021(5) Uiso 1 1 d . . . H1B H -1.0082(15) -1.2398(14) -0.0358(10) 0.020(5) Uiso 1 1 d . . . H3A H -1.1799(18) -1.0647(18) -0.0554(11) 0.035(6) Uiso 1 1 d . . . H3B H -1.1783(17) -0.9779(15) -0.1113(11) 0.030(5) Uiso 1 1 d . . . H3C H -1.1519(16) -0.9529(16) -0.0354(11) 0.031(5) Uiso 1 1 d . . . H4A H -1.0221(15) -1.0543(15) -0.3240(10) 0.024(5) Uiso 1 1 d . . . H4B H -0.9860(15) -1.1632(15) -0.3085(9) 0.018(5) Uiso 1 1 d . . . H6A H -0.7483(18) -1.2186(18) -0.2417(11) 0.041(6) Uiso 1 1 d . . . H6B H -0.705(2) -1.1347(18) -0.2888(11) 0.044(6) Uiso 1 1 d . . . H6C H -0.8139(19) -1.1864(18) -0.3070(12) 0.041(6) Uiso 1 1 d . . . H13 H -0.8900(15) -1.3625(14) -0.0705(10) 0.022(5) Uiso 1 1 d . . . H14 H -0.8274(18) -1.4669(17) -0.1514(11) 0.035(6) Uiso 1 1 d . . . H15 H -0.9002(16) -1.4528(15) -0.2609(10) 0.023(5) Uiso 1 1 d . . . H16 H -1.0357(15) -1.3330(14) -0.2864(10) 0.017(5) Uiso 1 1 d . . . H23 H -1.1895(17) -0.9918(17) -0.2990(11) 0.035(6) Uiso 1 1 d . . . H24 H -1.3586(17) -1.0155(16) -0.2586(10) 0.028(5) Uiso 1 1 d . . . H25 H -1.3867(19) -1.1564(17) -0.1932(11) 0.037(6) Uiso 1 1 d . . . H26 H -1.2452(14) -1.2696(15) -0.1655(9) 0.017(5) Uiso 1 1 d . . . H54 H -0.9537(16) -0.5724(15) -0.0341(9) 0.022(5) Uiso 1 1 d . . . H56 H -0.6498(14) -0.6629(13) 0.0285(8) 0.014(4) Uiso 1 1 d . . . H57A H -0.9894(18) -0.6963(17) -0.1805(12) 0.042(6) Uiso 1 1 d . . . H57B H -1.0554(19) -0.6466(19) -0.1277(11) 0.045(7) Uiso 1 1 d . . . H57C H -1.0356(18) -0.7631(19) -0.1305(11) 0.037(6) Uiso 1 1 d . . . H58A H -0.8433(18) -0.5448(17) 0.0956(11) 0.039(6) Uiso 1 1 d . . . H58B H -0.8270(18) -0.4630(18) 0.0442(11) 0.037(6) Uiso 1 1 d . . . H58C H -0.7228(17) -0.5179(15) 0.0785(10) 0.028(5) Uiso 1 1 d . . . H64 H -0.3628(16) -0.9465(14) -0.0888(9) 0.021(5) Uiso 1 1 d . . . H66 H -0.5184(15) -0.6811(15) -0.0580(9) 0.021(5) Uiso 1 1 d . . . H67A H -0.5643(17) -1.0910(16) -0.1333(11) 0.032(5) Uiso 1 1 d . . . H67B H -0.5677(18) -1.1049(17) -0.0566(11) 0.035(6) Uiso 1 1 d . . . H67C H -0.4584(19) -1.1017(17) -0.0860(11) 0.038(6) Uiso 1 1 d . . . H68A H -0.2828(19) -0.7615(18) -0.1127(12) 0.046(7) Uiso 1 1 d . . . H68B H -0.326(2) -0.676(2) -0.0680(12) 0.052(7) Uiso 1 1 d . . . H68C H -0.265(2) -0.7709(18) -0.0383(12) 0.046(7) Uiso 1 1 d . . . D0A H -0.6800(16) -0.2997(14) -0.1082(9) 0.020(5) Uiso 1 1 d . . . D0B H -0.5667(17) -0.2822(16) -0.0697(10) 0.030(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01286(14) 0.01251(14) 0.01316(15) -0.00132(10) 0.00251(10) -0.00152(10) O1 0.0133(5) 0.0153(6) 0.0192(6) 0.0002(4) 0.0022(4) -0.0016(4) O2 0.0158(5) 0.0142(6) 0.0172(6) -0.0014(4) 0.0033(4) -0.0030(4) O3 0.0180(5) 0.0154(6) 0.0154(6) -0.0025(4) 0.0010(4) 0.0006(4) O4 0.0165(5) 0.0192(6) 0.0179(6) -0.0061(5) 0.0033(4) -0.0034(4) O5 0.0163(5) 0.0138(5) 0.0138(5) -0.0011(4) 0.0010(4) -0.0016(4) O6 0.0152(5) 0.0130(5) 0.0163(6) 0.0000(4) 0.0016(4) -0.0026(4) N1 0.0127(6) 0.0175(7) 0.0149(7) -0.0011(5) 0.0033(5) -0.0039(5) N2 0.0193(7) 0.0175(7) 0.0148(7) -0.0052(5) 0.0043(5) -0.0031(5) C1 0.0199(8) 0.0201(9) 0.0166(8) 0.0018(7) 0.0025(6) -0.0055(7) C2 0.0169(7) 0.0185(8) 0.0099(7) 0.0011(6) 0.0013(6) -0.0021(6) C3 0.0133(8) 0.0271(9) 0.0217(9) -0.0029(8) 0.0033(6) -0.0005(7) C4 0.0239(8) 0.0170(8) 0.0137(8) -0.0017(7) -0.0001(6) -0.0017(7) C5 0.0202(8) 0.0141(8) 0.0121(7) 0.0011(6) 0.0041(6) -0.0024(6) C6 0.0240(9) 0.0247(10) 0.0279(10) -0.0124(8) 0.0069(8) 0.0009(8) C11 0.0161(7) 0.0146(8) 0.0222(8) 0.0006(6) 0.0031(6) -0.0047(6) C12 0.0186(8) 0.0138(8) 0.0206(8) 0.0022(6) 0.0033(6) -0.0062(6) C13 0.0238(9) 0.0181(9) 0.0257(9) 0.0053(7) -0.0010(7) -0.0038(7) C14 0.0235(9) 0.0184(9) 0.0381(11) 0.0031(8) 0.0015(8) 0.0021(7) C15 0.0252(9) 0.0183(9) 0.0325(10) -0.0044(8) 0.0080(8) -0.0009(7) C16 0.0233(8) 0.0181(9) 0.0210(9) -0.0027(7) 0.0020(7) -0.0045(7) C21 0.0174(8) 0.0185(8) 0.0167(8) -0.0056(6) -0.0008(6) -0.0017(6) C22 0.0193(8) 0.0199(8) 0.0150(8) -0.0050(6) -0.0022(6) -0.0009(6) C23 0.0282(9) 0.0266(10) 0.0207(9) -0.0044(8) -0.0069(7) 0.0048(8) C24 0.0234(9) 0.0379(11) 0.0307(10) -0.0105(9) -0.0086(8) 0.0113(8) C25 0.0162(9) 0.0466(12) 0.0301(10) -0.0125(9) 0.0004(7) -0.0005(8) C26 0.0190(8) 0.0297(10) 0.0237(9) -0.0045(8) 0.0022(7) -0.0049(7) C51 0.0164(7) 0.0107(7) 0.0146(8) 0.0029(6) 0.0032(6) -0.0016(6) C52 0.0171(7) 0.0120(7) 0.0120(7) 0.0011(6) 0.0033(6) -0.0026(6) C53 0.0160(7) 0.0153(8) 0.0164(8) 0.0040(6) 0.0032(6) -0.0009(6) C54 0.0166(8) 0.0127(8) 0.0215(8) 0.0031(6) 0.0058(6) 0.0025(6) C55 0.0217(8) 0.0122(8) 0.0171(8) 0.0002(6) 0.0058(6) -0.0026(6) C56 0.0169(8) 0.0144(8) 0.0153(8) 0.0012(6) 0.0018(6) -0.0037(6) C57 0.0180(8) 0.0225(9) 0.0239(9) -0.0003(7) -0.0017(7) 0.0019(7) C58 0.0238(9) 0.0189(9) 0.0239(9) -0.0057(7) 0.0052(7) -0.0002(7) C61 0.0163(7) 0.0156(8) 0.0113(7) 0.0002(6) -0.0006(6) -0.0006(6) C62 0.0140(7) 0.0156(8) 0.0125(7) 0.0012(6) 0.0004(6) -0.0015(6) C63 0.0181(7) 0.0152(8) 0.0119(7) -0.0007(6) -0.0001(6) 0.0012(6) C64 0.0147(7) 0.0201(8) 0.0184(8) 0.0004(6) 0.0021(6) 0.0033(6) C65 0.0160(8) 0.0205(8) 0.0161(8) 0.0012(6) 0.0000(6) -0.0035(6) C66 0.0188(8) 0.0141(8) 0.0137(8) -0.0001(6) -0.0004(6) -0.0016(6) C67 0.0202(8) 0.0156(8) 0.0220(9) -0.0010(7) 0.0026(7) 0.0025(7) C68 0.0165(8) 0.0243(10) 0.0357(11) -0.0001(8) 0.0034(8) -0.0047(7) C0 0.0323(10) 0.0190(9) 0.0274(10) 0.0003(8) 0.0052(8) -0.0001(8) Cl1 0.0759(4) 0.0239(3) 0.0368(3) 0.0015(2) 0.0269(3) 0.0028(2) Cl2 0.0495(3) 0.0232(2) 0.0318(3) 0.00606(19) 0.0050(2) -0.0031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O5 1.8575(11) . ? Ti O6 1.8582(11) . ? Ti O4 1.9551(11) . ? Ti O2 1.9580(11) . ? Ti O3 2.0565(11) . ? Ti O1 2.0701(11) . ? O1 C2 1.2786(19) . ? O2 N1 1.3781(16) . ? O3 C5 1.2753(19) . ? O4 N2 1.3778(17) . ? O5 C52 1.3600(18) . ? O6 C62 1.3584(18) . ? N1 C2 1.309(2) . ? N1 C3 1.453(2) . ? N2 C5 1.309(2) . ? N2 C6 1.451(2) . ? C1 C2 1.501(2) . ? C1 C12 1.519(2) . ? C1 H1A 0.981(19) . ? C1 H1B 0.94(2) . ? C3 H3A 0.97(2) . ? C3 H3B 0.99(2) . ? C3 H3C 0.97(2) . ? C4 C5 1.499(2) . ? C4 C22 1.515(2) . ? C4 H4A 0.94(2) . ? C4 H4B 0.958(19) . ? C6 H6A 0.97(2) . ? C6 H6B 0.96(2) . ? C6 H6C 0.90(2) . ? C11 C16 1.396(2) . ? C11 C12 1.406(2) . ? C11 C21 1.499(2) . ? C12 C13 1.395(2) . ? C13 C14 1.383(3) . ? C13 H13 0.96(2) . ? C14 C15 1.385(3) . ? C14 H14 0.95(2) . ? C15 C16 1.388(3) . ? C15 H15 0.96(2) . ? C16 H16 0.917(19) . ? C21 C26 1.398(2) . ? C21 C22 1.403(2) . ? C22 C23 1.397(2) . ? C23 C24 1.386(3) . ? C23 H23 0.97(2) . ? C24 C25 1.374(3) . ? C24 H24 0.95(2) . ? C25 C26 1.391(3) . ? C25 H25 0.91(2) . ? C26 H26 0.936(19) . ? C51 C56 1.400(2) . ? C51 C52 1.407(2) . ? C51 C61 1.489(2) . ? C52 C53 1.405(2) . ? C53 C54 1.389(2) . ? C53 C57 1.506(2) . ? C54 C55 1.395(2) . ? C54 H54 0.92(2) . ? C55 C56 1.391(2) . ? C55 C58 1.504(2) . ? C56 H56 0.978(17) . ? C57 H57A 0.99(2) . ? C57 H57B 0.95(2) . ? C57 H57C 0.93(2) . ? C58 H58A 0.97(2) . ? C58 H58B 0.97(2) . ? C58 H58C 0.98(2) . ? C61 C62 1.404(2) . ? C61 C66 1.405(2) . ? C62 C63 1.405(2) . ? C63 C64 1.391(2) . ? C63 C67 1.501(2) . ? C64 C65 1.394(2) . ? C64 H64 0.973(19) . ? C65 C66 1.390(2) . ? C65 C68 1.512(2) . ? C66 H66 0.95(2) . ? C67 H67A 0.99(2) . ? C67 H67B 0.94(2) . ? C67 H67C 0.94(2) . ? C68 H68A 0.94(2) . ? C68 H68B 0.97(3) . ? C68 H68C 0.96(3) . ? C0 Cl1 1.7562(19) . ? C0 Cl2 1.7684(19) . ? C0 D0A 0.938(19) . ? C0 D0B 0.95(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 Ti O6 91.00(5) . . ? O5 Ti O4 108.36(5) . . ? O6 Ti O4 91.89(5) . . ? O5 Ti O2 90.18(5) . . ? O6 Ti O2 108.75(5) . . ? O4 Ti O2 152.20(5) . . ? O5 Ti O3 95.62(5) . . ? O6 Ti O3 167.49(5) . . ? O4 Ti O3 75.97(5) . . ? O2 Ti O3 81.89(5) . . ? O5 Ti O1 165.82(5) . . ? O6 Ti O1 90.75(5) . . ? O4 Ti O1 85.64(5) . . ? O2 Ti O1 75.94(4) . . ? O3 Ti O1 85.43(4) . . ? C2 O1 Ti 111.71(10) . . ? N1 O2 Ti 112.46(8) . . ? C5 O3 Ti 113.69(10) . . ? N2 O4 Ti 114.43(9) . . ? C52 O5 Ti 124.40(9) . . ? C62 O6 Ti 127.56(9) . . ? C2 N1 O2 115.14(12) . . ? C2 N1 C3 130.41(14) . . ? O2 N1 C3 114.03(13) . . ? C5 N2 O4 114.69(13) . . ? C5 N2 C6 130.70(14) . . ? O4 N2 C6 114.45(13) . . ? C2 C1 C12 110.70(13) . . ? C2 C1 H1A 111.6(11) . . ? C12 C1 H1A 112.4(11) . . ? C2 C1 H1B 107.0(11) . . ? C12 C1 H1B 108.4(11) . . ? H1A C1 H1B 106.4(15) . . ? O1 C2 N1 117.11(14) . . ? O1 C2 C1 119.68(14) . . ? N1 C2 C1 123.19(14) . . ? N1 C3 H3A 109.2(13) . . ? N1 C3 H3B 110.9(12) . . ? H3A C3 H3B 111.7(17) . . ? N1 C3 H3C 109.4(12) . . ? H3A C3 H3C 107.4(18) . . ? H3B C3 H3C 108.2(17) . . ? C5 C4 C22 111.49(13) . . ? C5 C4 H4A 105.6(12) . . ? C22 C4 H4A 109.7(12) . . ? C5 C4 H4B 110.7(11) . . ? C22 C4 H4B 111.4(11) . . ? H4A C4 H4B 107.6(16) . . ? O3 C5 N2 117.18(14) . . ? O3 C5 C4 119.44(14) . . ? N2 C5 C4 123.37(14) . . ? N2 C6 H6A 109.0(13) . . ? N2 C6 H6B 107.6(14) . . ? H6A C6 H6B 109.9(19) . . ? N2 C6 H6C 109.8(15) . . ? H6A C6 H6C 112(2) . . ? H6B C6 H6C 109(2) . . ? C16 C11 C12 118.98(15) . . ? C16 C11 C21 119.42(15) . . ? C12 C11 C21 121.58(15) . . ? C13 C12 C11 118.72(16) . . ? C13 C12 C1 119.11(15) . . ? C11 C12 C1 122.13(15) . . ? C14 C13 C12 121.53(17) . . ? C14 C13 H13 119.0(12) . . ? C12 C13 H13 119.5(12) . . ? C13 C14 C15 120.02(17) . . ? C13 C14 H14 120.5(13) . . ? C15 C14 H14 119.5(13) . . ? C14 C15 C16 119.13(17) . . ? C14 C15 H15 120.4(12) . . ? C16 C15 H15 120.4(12) . . ? C15 C16 C11 121.62(17) . . ? C15 C16 H16 119.7(12) . . ? C11 C16 H16 118.7(12) . . ? C26 C21 C22 118.94(16) . . ? C26 C21 C11 118.92(15) . . ? C22 C21 C11 122.14(14) . . ? C23 C22 C21 118.79(16) . . ? C23 C22 C4 118.65(16) . . ? C21 C22 C4 122.56(15) . . ? C24 C23 C22 121.48(18) . . ? C24 C23 H23 120.3(13) . . ? C22 C23 H23 118.2(13) . . ? C25 C24 C23 119.70(18) . . ? C25 C24 H24 122.0(13) . . ? C23 C24 H24 118.3(13) . . ? C24 C25 C26 119.82(18) . . ? C24 C25 H25 120.1(14) . . ? C26 C25 H25 120.1(14) . . ? C25 C26 C21 121.15(18) . . ? C25 C26 H26 121.0(11) . . ? C21 C26 H26 117.8(11) . . ? C56 C51 C52 118.03(14) . . ? C56 C51 C61 119.99(14) . . ? C52 C51 C61 121.78(14) . . ? O5 C52 C53 118.39(13) . . ? O5 C52 C51 120.62(13) . . ? C53 C52 C51 120.91(14) . . ? C54 C53 C52 118.53(14) . . ? C54 C53 C57 121.73(15) . . ? C52 C53 C57 119.73(15) . . ? C53 C54 C55 122.28(15) . . ? C53 C54 H54 118.6(12) . . ? C55 C54 H54 119.1(12) . . ? C56 C55 C54 117.84(15) . . ? C56 C55 C58 121.09(15) . . ? C54 C55 C58 121.06(15) . . ? C55 C56 C51 122.30(15) . . ? C55 C56 H56 119.2(10) . . ? C51 C56 H56 118.5(10) . . ? C53 C57 H57A 113.9(13) . . ? C53 C57 H57B 111.6(14) . . ? H57A C57 H57B 105.7(19) . . ? C53 C57 H57C 111.0(13) . . ? H57A C57 H57C 102.4(19) . . ? H57B C57 H57C 111.7(19) . . ? C55 C58 H58A 112.9(13) . . ? C55 C58 H58B 111.4(13) . . ? H58A C58 H58B 104.3(18) . . ? C55 C58 H58C 110.0(12) . . ? H58A C58 H58C 109.2(18) . . ? H58B C58 H58C 108.9(18) . . ? C62 C61 C66 118.14(14) . . ? C62 C61 C51 122.51(14) . . ? C66 C61 C51 119.34(14) . . ? O6 C62 C61 120.66(13) . . ? O6 C62 C63 118.46(14) . . ? C61 C62 C63 120.85(14) . . ? C64 C63 C62 118.65(14) . . ? C64 C63 C67 121.77(14) . . ? C62 C63 C67 119.58(14) . . ? C63 C64 C65 122.22(15) . . ? C63 C64 H64 117.3(11) . . ? C65 C64 H64 120.5(11) . . ? C66 C65 C64 117.92(14) . . ? C66 C65 C68 121.50(15) . . ? C64 C65 C68 120.58(15) . . ? C65 C66 C61 122.20(15) . . ? C65 C66 H66 119.6(11) . . ? C61 C66 H66 118.1(11) . . ? C63 C67 H67A 110.0(13) . . ? C63 C67 H67B 110.6(13) . . ? H67A C67 H67B 110.1(18) . . ? C63 C67 H67C 110.3(14) . . ? H67A C67 H67C 108.0(18) . . ? H67B C67 H67C 107.7(19) . . ? C65 C68 H68A 111.2(15) . . ? C65 C68 H68B 110.7(15) . . ? H68A C68 H68B 111(2) . . ? C65 C68 H68C 110.7(14) . . ? H68A C68 H68C 106(2) . . ? H68B C68 H68C 108(2) . . ? Cl1 C0 Cl2 111.29(10) . . ? Cl1 C0 D0A 106.2(11) . . ? Cl2 C0 D0A 108.7(12) . . ? Cl1 C0 D0B 109.3(12) . . ? Cl2 C0 D0B 109.8(13) . . ? D0A C0 D0B 111.5(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.365 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.050 #========END