# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Levason, W.' _publ_contact_author_email wxl@soton.ac.uk _publ_section_title ; Taking TiF4 complexes to extremes the first examples with phosphine co-ligands ; loop_ _publ_author_name W.Levason G.Reid M.Webster W.Zhang M.Jura E.Petts # Attachment '- TiF4_all7_1.cif' data_08mj52 _database_code_depnum_ccdc_archive 'CCDC 783180' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-10 _audit_author_name 'Webster, M.' _chemical_name_systematic ; cis-tetrafluorobis(tetrahydrofuran)titanium(IV) ; _chemical_name_common cis-tetrafluorobis(tetrahydrofuran)titanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 F4 O2 Ti' _chemical_formula_sum 'C8 H16 F4 O2 Ti' _chemical_formula_weight 268.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 21/n' _space_group_IT_number 14 _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 6.3523(15) _cell_length_b 11.003(3) _cell_length_c 15.840(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.46(2) _cell_angle_gamma 90.00 _cell_volume 1103.8(5) # shelxl (4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2606 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5815 # _exptl_absorpt_correction_T_max 0.7456 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19259 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.91 _diffrn_reflns_theta_max 27.56 _reflns_number_total 2516 _reflns_number_gt 2187 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.9784P] 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 2516 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.57015(6) 0.84745(3) 0.33039(2) 0.02098(12) Uani 1 1 d . . . F1 F 0.4710(2) 0.71536(11) 0.27433(8) 0.0311(3) Uani 1 1 d . . . F2 F 0.6758(2) 0.76928(12) 0.42324(8) 0.0322(3) Uani 1 1 d . . . F3 F 0.81767(19) 0.85731(11) 0.28148(8) 0.0261(3) Uani 1 1 d . . . F4 F 0.32161(19) 0.88927(11) 0.37106(8) 0.0268(3) Uani 1 1 d . . . O1 O 0.6641(2) 1.01820(13) 0.38094(9) 0.0239(3) Uani 1 1 d . . . O2 O 0.4541(2) 0.95102(13) 0.22290(9) 0.0254(3) Uani 1 1 d . . . C1 C 0.8833(3) 1.06122(18) 0.38981(14) 0.0247(4) Uani 1 1 d . . . H1A H 0.9356 1.0779 0.3337 0.030 Uiso 1 1 calc R . . H1B H 0.9766 1.0003 0.4197 0.030 Uiso 1 1 calc R . . C2 C 0.8751(4) 1.17713(19) 0.44137(14) 0.0275(5) Uani 1 1 d . . . H2A H 0.9898 1.2336 0.4288 0.033 Uiso 1 1 calc R . . H2B H 0.8851 1.1596 0.5028 0.033 Uiso 1 1 calc R . . C3 C 0.6589(4) 1.22876(18) 0.41169(14) 0.0271(5) Uani 1 1 d . . . H3A H 0.6077 1.2854 0.4541 0.033 Uiso 1 1 calc R . . H3B H 0.6635 1.2718 0.3570 0.033 Uiso 1 1 calc R . . C4 C 0.5204(4) 1.11623(18) 0.40230(15) 0.0273(5) Uani 1 1 d . . . H4A H 0.4560 1.0981 0.4558 0.033 Uiso 1 1 calc R . . H4B H 0.4065 1.1274 0.3567 0.033 Uiso 1 1 calc R . . C5 C 0.5750(4) 1.0268(2) 0.16875(14) 0.0293(5) Uani 1 1 d . . . H5A H 0.6682 0.9762 0.1358 0.035 Uiso 1 1 calc R . . H5B H 0.6630 1.0857 0.2030 0.035 Uiso 1 1 calc R . . C6 C 0.4131(4) 1.0917(2) 0.11076(16) 0.0328(5) Uani 1 1 d . . . H6A H 0.4683 1.1090 0.0553 0.039 Uiso 1 1 calc R . . H6B H 0.3689 1.1689 0.1362 0.039 Uiso 1 1 calc R . . C7 C 0.2301(4) 1.0008(2) 0.10167(15) 0.0324(5) Uani 1 1 d . . . H7A H 0.0943 1.0424 0.0863 0.039 Uiso 1 1 calc R . . H7B H 0.2540 0.9384 0.0584 0.039 Uiso 1 1 calc R . . C8 C 0.2330(3) 0.9452(2) 0.18897(15) 0.0288(5) Uani 1 1 d . . . H8A H 0.1415 0.9917 0.2251 0.035 Uiso 1 1 calc R . . H8B H 0.1833 0.8599 0.1856 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0259(2) 0.01459(19) 0.0231(2) -0.00078(13) 0.00567(14) 0.00037(14) F1 0.0397(7) 0.0183(6) 0.0360(7) -0.0065(5) 0.0082(6) -0.0046(5) F2 0.0395(7) 0.0280(7) 0.0293(7) 0.0061(5) 0.0042(5) 0.0073(6) F3 0.0255(6) 0.0251(6) 0.0285(7) -0.0035(5) 0.0078(5) 0.0017(5) F4 0.0267(6) 0.0238(6) 0.0310(7) -0.0007(5) 0.0097(5) -0.0002(5) O1 0.0235(7) 0.0170(7) 0.0314(8) -0.0041(6) 0.0043(6) 0.0016(6) O2 0.0233(7) 0.0244(7) 0.0284(8) 0.0052(6) 0.0019(6) -0.0046(6) C1 0.0233(10) 0.0215(10) 0.0291(11) -0.0022(8) 0.0012(8) -0.0011(8) C2 0.0318(11) 0.0203(10) 0.0302(11) -0.0027(8) 0.0008(9) -0.0015(8) C3 0.0359(12) 0.0160(9) 0.0294(11) -0.0009(8) 0.0028(9) 0.0009(8) C4 0.0305(11) 0.0170(9) 0.0350(12) -0.0047(8) 0.0061(9) 0.0048(8) C5 0.0290(11) 0.0273(11) 0.0319(12) 0.0113(9) 0.0049(9) -0.0042(9) C6 0.0343(12) 0.0276(11) 0.0367(12) 0.0097(9) 0.0053(10) 0.0027(10) C7 0.0296(12) 0.0335(12) 0.0336(12) 0.0027(9) -0.0003(9) 0.0002(9) C8 0.0231(10) 0.0268(11) 0.0361(12) 0.0034(9) -0.0006(9) -0.0030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F2 1.7886(13) . ? Ti1 F1 1.7918(13) . ? Ti1 F3 1.8094(13) . ? Ti1 F4 1.8104(13) . ? Ti1 O1 2.1103(15) . ? Ti1 O2 2.1321(15) . ? O1 C1 1.467(3) . ? O1 C4 1.470(2) . ? O2 C5 1.457(2) . ? O2 C8 1.466(3) . ? C1 C2 1.517(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.526(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.505(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.532(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 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 F2 Ti1 F1 96.45(7) . . ? F2 Ti1 F3 95.63(6) . . ? F1 Ti1 F3 96.89(6) . . ? F2 Ti1 F4 96.39(6) . . ? F1 Ti1 F4 95.74(6) . . ? F3 Ti1 F4 161.45(6) . . ? F2 Ti1 O1 92.25(6) . . ? F1 Ti1 O1 171.26(6) . . ? F3 Ti1 O1 83.08(6) . . ? F4 Ti1 O1 82.38(6) . . ? F2 Ti1 O2 176.29(6) . . ? F1 Ti1 O2 87.22(6) . . ? F3 Ti1 O2 83.33(6) . . ? F4 Ti1 O2 83.77(6) . . ? O1 Ti1 O2 84.09(6) . . ? C1 O1 C4 110.07(15) . . ? C1 O1 Ti1 124.20(11) . . ? C4 O1 Ti1 125.34(12) . . ? C5 O2 C8 110.07(16) . . ? C5 O2 Ti1 127.64(13) . . ? C8 O2 Ti1 122.08(12) . . ? O1 C1 C2 104.53(16) . . ? O1 C1 H1A 110.8 . . ? C2 C1 H1A 110.8 . . ? O1 C1 H1B 110.8 . . ? C2 C1 H1B 110.8 . . ? H1A C1 H1B 108.9 . . ? C1 C2 C3 102.39(17) . . ? C1 C2 H2A 111.3 . . ? C3 C2 H2A 111.3 . . ? C1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C4 C3 C2 103.13(17) . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? O1 C4 C3 104.78(17) . . ? O1 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? O1 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? O2 C5 C6 105.33(18) . . ? O2 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? O2 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C5 C6 C7 103.00(18) . . ? C5 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? C5 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C8 C7 C6 102.90(18) . . ? C8 C7 H7A 111.2 . . ? C6 C7 H7A 111.2 . . ? C8 C7 H7B 111.2 . . ? C6 C7 H7B 111.2 . . ? H7A C7 H7B 109.1 . . ? O2 C8 C7 105.13(17) . . ? O2 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? O2 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # F1 Ti1 O1 C1 -112.5(4) . . . . ? # F1 Ti1 O1 C4 59.6(5) . . . . ? # F2 Ti1 O2 C5 52.3(10) . . . . ? # F2 Ti1 O2 C8 -133.5(9) . . . . ? F2 Ti1 O1 C1 73.25(15) . . . . ? F3 Ti1 O1 C1 -22.15(15) . . . . ? F4 Ti1 O1 C1 169.40(15) . . . . ? O2 Ti1 O1 C1 -106.12(15) . . . . ? F2 Ti1 O1 C4 -114.72(16) . . . . ? F3 Ti1 O1 C4 149.88(16) . . . . ? F4 Ti1 O1 C4 -18.57(15) . . . . ? O2 Ti1 O1 C4 65.91(16) . . . . ? F1 Ti1 O2 C5 -118.95(17) . . . . ? F3 Ti1 O2 C5 -21.68(17) . . . . ? F4 Ti1 O2 C5 144.96(17) . . . . ? O1 Ti1 O2 C5 62.02(17) . . . . ? F1 Ti1 O2 C8 55.34(15) . . . . ? F3 Ti1 O2 C8 152.61(16) . . . . ? F4 Ti1 O2 C8 -40.75(15) . . . . ? O1 Ti1 O2 C8 -123.70(15) . . . . ? C4 O1 C1 C2 15.8(2) . . . . ? Ti1 O1 C1 C2 -171.08(13) . . . . ? O1 C1 C2 C3 -33.6(2) . . . . ? C1 C2 C3 C4 38.7(2) . . . . ? C1 O1 C4 C3 8.6(2) . . . . ? Ti1 O1 C4 C3 -164.37(13) . . . . ? C2 C3 C4 O1 -29.4(2) . . . . ? C8 O2 C5 C6 12.7(2) . . . . ? Ti1 O2 C5 C6 -172.43(14) . . . . ? O2 C5 C6 C7 -30.6(2) . . . . ? C5 C6 C7 C8 36.8(2) . . . . ? C5 O2 C8 C7 10.8(2) . . . . ? Ti1 O2 C8 C7 -164.36(14) . . . . ? C6 C7 C8 O2 -29.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.254 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.062 #===END OF CIF ============================================================== # 08mj71b.cif data_08mj71 _database_code_depnum_ccdc_archive 'CCDC 783181' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-06-11 _audit_author_name 'Webster, M.' _audit_update_record ; 2010-06-11 Relabelled some C and moved F2 ; _chemical_name_systematic ; cis-tetrafluorobis(triphenylphosphine oxide-O)titanium(IV) dichloromethane solvate ; # Non-solvated structure reported (CSD refcode: IBEGIG. # E.G. Il'in, G.B. Nikiforov, G.G. Aleksandrov, # Doklady Akademii Nauk, 396 (2004) p500. _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 F4 O2 P2 Ti, 2(C H2 Cl2)' _chemical_formula_sum 'C38 H34 Cl4 F4 O2 P2 Ti' _chemical_formula_structural '(((C6 H5)3 P O) Ti F4) (C H2 Cl2)2' _chemical_formula_weight 850.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.083(2) _cell_length_b 15.8121(15) _cell_length_c 16.004(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3816.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4952 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8220 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12705 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.87 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2576 _reflns_number_gt 2203 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+2.9269P] 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 2576 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.11612(3) 0.7500 0.01551(19) Uani 1 2 d S . . F1 F -0.08573(9) 0.12363(8) 0.66858(8) 0.0245(3) Uani 1 1 d . . . F2 F -0.06537(9) 0.03814(8) 0.80468(9) 0.0255(3) Uani 1 1 d . . . P1 P -0.06046(4) 0.26344(4) 0.89165(4) 0.01708(19) Uani 1 1 d . . . O1 O -0.06471(10) 0.20947(10) 0.81325(10) 0.0194(4) Uani 1 1 d . . . C1 C 0.02661(17) 0.34118(15) 0.88884(14) 0.0217(5) Uani 1 1 d . . . C2 C 0.0087(2) 0.42736(17) 0.8878(2) 0.0424(8) Uani 1 1 d . . . H2 H -0.0509 0.4467 0.8866 0.051 Uiso 1 1 calc R . . C3 C 0.0778(2) 0.48514(19) 0.8884(3) 0.0562(10) Uani 1 1 d . . . H3 H 0.0652 0.5440 0.8871 0.067 Uiso 1 1 calc R . . C4 C 0.1640(2) 0.45819(19) 0.89078(19) 0.0410(7) Uani 1 1 d . . . H4 H 0.2109 0.4983 0.8914 0.049 Uiso 1 1 calc R . . C5 C 0.18309(19) 0.37248(18) 0.89228(17) 0.0321(6) Uani 1 1 d . . . H5 H 0.2429 0.3539 0.8945 0.039 Uiso 1 1 calc R . . C6 C 0.11482(17) 0.31409(16) 0.89049(16) 0.0268(6) Uani 1 1 d . . . H6 H 0.1279 0.2553 0.8904 0.032 Uiso 1 1 calc R . . C7 C -0.04560(15) 0.20307(14) 0.98548(15) 0.0182(5) Uani 1 1 d . . . C8 C -0.00856(16) 0.24016(15) 1.05624(15) 0.0223(5) Uani 1 1 d . . . H8 H 0.0169 0.2950 1.0528 0.027 Uiso 1 1 calc R . . C9 C -0.00873(17) 0.19723(16) 1.13155(16) 0.0270(6) Uani 1 1 d . . . H9 H 0.0162 0.2228 1.1799 0.032 Uiso 1 1 calc R . . C10 C -0.04530(17) 0.11691(16) 1.13654(16) 0.0268(6) Uani 1 1 d . . . H10 H -0.0467 0.0882 1.1886 0.032 Uiso 1 1 calc R . . C11 C -0.07978(16) 0.07852(16) 1.06611(16) 0.0253(6) Uani 1 1 d . . . H11 H -0.1028 0.0227 1.0695 0.030 Uiso 1 1 calc R . . C12 C -0.08091(16) 0.12137(15) 0.99040(16) 0.0219(5) Uani 1 1 d . . . H12 H -0.1055 0.0954 0.9422 0.026 Uiso 1 1 calc R . . C13 C -0.16372(16) 0.31832(14) 0.90312(15) 0.0193(5) Uani 1 1 d . . . C14 C -0.20291(17) 0.33031(15) 0.98126(16) 0.0233(5) Uani 1 1 d . . . H14 H -0.1751 0.3084 1.0300 0.028 Uiso 1 1 calc R . . C15 C -0.28280(17) 0.37432(15) 0.98807(17) 0.0261(6) Uani 1 1 d . . . H15 H -0.3099 0.3820 1.0411 0.031 Uiso 1 1 calc R . . C16 C -0.32207(17) 0.40668(15) 0.91680(18) 0.0274(6) Uani 1 1 d . . . H16 H -0.3758 0.4377 0.9214 0.033 Uiso 1 1 calc R . . C17 C -0.28421(18) 0.39449(16) 0.83900(18) 0.0305(6) Uani 1 1 d . . . H17 H -0.3124 0.4162 0.7905 0.037 Uiso 1 1 calc R . . C18 C -0.20502(17) 0.35048(15) 0.83189(16) 0.0257(6) Uani 1 1 d . . . H18 H -0.1789 0.3422 0.7785 0.031 Uiso 1 1 calc R . . C19 C 0.7703(2) 0.3825(2) 0.28558(19) 0.0414(7) Uani 1 1 d . . . H19A H 0.7685 0.4408 0.2630 0.050 Uiso 1 1 calc R . . H19B H 0.7086 0.3611 0.2878 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.83253(5) 0.31822(5) 0.21758(5) 0.0434(2) Uani 1 1 d . . . Cl2 Cl 0.81374(6) 0.38517(6) 0.38688(5) 0.0517(3) 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 Ti1 0.0168(3) 0.0143(3) 0.0154(3) 0.000 0.0005(2) 0.000 F1 0.0247(7) 0.0272(7) 0.0216(7) -0.0023(5) -0.0050(6) 0.0003(6) F2 0.0284(8) 0.0194(7) 0.0287(8) 0.0030(6) 0.0058(6) -0.0028(6) P1 0.0189(3) 0.0167(3) 0.0157(3) 0.0000(2) 0.0006(2) 0.0014(2) O1 0.0227(9) 0.0198(8) 0.0157(8) -0.0007(6) 0.0011(7) 0.0018(6) C1 0.0271(13) 0.0196(12) 0.0184(12) 0.0000(9) 0.0010(10) -0.0037(10) C2 0.0363(16) 0.0232(14) 0.067(2) 0.0021(13) 0.0053(15) -0.0005(12) C3 0.055(2) 0.0203(15) 0.093(3) 0.0005(16) 0.0098(19) -0.0085(14) C4 0.0436(18) 0.0352(16) 0.0442(18) -0.0060(13) 0.0063(14) -0.0219(13) C5 0.0281(15) 0.0413(16) 0.0270(15) -0.0031(12) -0.0009(11) -0.0103(12) C6 0.0264(14) 0.0265(13) 0.0276(14) -0.0019(10) -0.0027(11) -0.0034(11) C7 0.0178(12) 0.0191(11) 0.0178(11) -0.0004(9) 0.0033(9) 0.0050(9) C8 0.0228(12) 0.0220(12) 0.0221(13) -0.0021(10) -0.0018(10) 0.0020(10) C9 0.0254(13) 0.0357(14) 0.0198(13) -0.0039(11) -0.0031(11) 0.0065(11) C10 0.0255(13) 0.0354(15) 0.0196(13) 0.0076(11) 0.0034(11) 0.0115(11) C11 0.0261(13) 0.0226(13) 0.0271(14) 0.0060(10) 0.0031(11) 0.0025(10) C12 0.0206(12) 0.0240(13) 0.0210(12) 0.0002(10) -0.0001(10) 0.0002(10) C13 0.0213(12) 0.0142(11) 0.0225(12) -0.0013(9) -0.0012(10) -0.0003(9) C14 0.0252(13) 0.0236(12) 0.0212(13) 0.0000(10) -0.0007(10) 0.0013(10) C15 0.0241(13) 0.0222(13) 0.0320(14) -0.0051(10) 0.0050(11) 0.0005(10) C16 0.0195(12) 0.0187(12) 0.0442(16) -0.0056(11) -0.0016(12) 0.0019(10) C17 0.0317(14) 0.0266(13) 0.0331(15) -0.0002(11) -0.0098(12) 0.0056(11) C18 0.0288(13) 0.0256(13) 0.0228(13) 0.0012(10) -0.0009(11) 0.0044(11) C19 0.0360(16) 0.0572(19) 0.0309(16) -0.0036(14) -0.0004(13) 0.0166(14) Cl1 0.0526(5) 0.0422(4) 0.0355(4) 0.0008(3) 0.0100(3) 0.0075(3) Cl2 0.0514(5) 0.0681(6) 0.0356(4) -0.0051(4) -0.0074(3) 0.0154(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F2 1.8050(13) 3_556 ? Ti1 F2 1.8050(13) . ? Ti1 F1 1.8396(13) 3_556 ? Ti1 F1 1.8396(13) . ? Ti1 O1 2.0387(16) 3_556 ? Ti1 O1 2.0387(16) . ? P1 O1 1.5188(17) . ? P1 C7 1.793(2) . ? P1 C13 1.792(2) . ? P1 C1 1.799(2) . ? C1 C2 1.389(4) . ? C1 C6 1.398(4) . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.369(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.392(4) . ? C7 C12 1.400(3) . ? C8 C9 1.383(4) . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.396(4) . ? C13 C18 1.395(4) . ? C14 C15 1.396(4) . ? C14 H14 0.9500 . ? C15 C16 1.383(4) . ? C15 H15 0.9500 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 Cl2 1.749(3) . ? C19 Cl1 1.761(3) . ? C19 H19A 0.9900 . ? C19 H19B 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 F2 Ti1 F2 93.83(9) 3_556 . ? F2 Ti1 F1 90.20(6) 3_556 3_556 ? F2 Ti1 F1 94.85(6) . 3_556 ? F2 Ti1 F1 94.85(6) 3_556 . ? F2 Ti1 F1 90.20(6) . . ? F1 Ti1 F1 172.60(9) 3_556 . ? F2 Ti1 O1 89.56(6) 3_556 3_556 ? F2 Ti1 O1 175.43(6) . 3_556 ? F1 Ti1 O1 88.20(6) 3_556 3_556 ? F1 Ti1 O1 86.45(6) . 3_556 ? F2 Ti1 O1 175.43(7) 3_556 . ? F2 Ti1 O1 89.56(6) . . ? F1 Ti1 O1 86.45(6) 3_556 . ? F1 Ti1 O1 88.20(6) . . ? O1 Ti1 O1 87.22(9) 3_556 . ? O1 P1 C7 113.45(10) . . ? O1 P1 C13 108.65(10) . . ? C7 P1 C13 106.29(11) . . ? O1 P1 C1 113.20(10) . . ? C7 P1 C1 107.06(11) . . ? C13 P1 C1 107.82(11) . . ? P1 O1 Ti1 142.83(10) . . ? C2 C1 C6 119.0(2) . . ? C2 C1 P1 121.9(2) . . ? C6 C1 P1 119.00(18) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C8 C7 C12 119.7(2) . . ? C8 C7 P1 120.46(18) . . ? C12 C7 P1 119.40(18) . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 119.7(2) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 119.6(2) . . ? C14 C13 P1 121.69(19) . . ? C18 C13 P1 118.74(19) . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.3(2) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.9(2) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? Cl2 C19 Cl1 112.75(16) . . ? Cl2 C19 H19A 109.0 . . ? Cl1 C19 H19A 109.0 . . ? Cl2 C19 H19B 109.0 . . ? Cl1 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.279 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.050 #===END OF CIF ============================================================== # 09wzsam01a.cif data_09wzsam01 _database_code_depnum_ccdc_archive 'CCDC 783182' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-12-18 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrafluoro(2,2'-bipyridyl-N,N')titanium(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 F4 N2 Ti' _chemical_formula_sum 'C10 H8 F4 N2 Ti' _chemical_formula_weight 280.08 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' F F 0.0171 0.0103 '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 hexagonal _symmetry_space_group_name_H-M 'P 64' _space_group_IT_number 172 _space_group_name_Hall 'P 64' # Note: P62 (171) and P64 (172) are an enantiomorphous pair. loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z' 'y, -x+y, z+1/3' 'x-y, x, z+2/3' _cell_length_a 11.6262(10) _cell_length_b 11.6262(10) _cell_length_c 20.761(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2430.3(4) _cell_formula_units_Z 9 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 18256 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7853 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18547 _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3659 _reflns_number_gt 2870 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+10.0014P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 3659 _refine_ls_number_parameters 231 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.5000 0.5000 0.74969(7) 0.0343(4) Uani 1 2 d SD . . Ti2 Ti 0.80669(14) 0.15157(13) 0.74784(6) 0.0572(4) Uani 1 1 d D . . F1 F 0.4882(4) 0.3723(5) 0.6972(2) 0.0683(16) Uani 1 1 d D . . F2 F 0.6803(3) 0.5788(4) 0.7584(2) 0.0421(10) Uani 1 1 d D . . F3 F 0.6721(7) 0.1399(6) 0.7928(3) 0.128(3) Uani 1 1 d D . . F4 F 0.9180(7) 0.1565(6) 0.8076(3) 0.134(4) Uani 1 1 d D . . F5 F 0.8944(5) 0.3319(4) 0.7405(2) 0.0687(15) Uani 1 1 d D . . F6 F 0.7260(4) -0.0272(4) 0.7348(2) 0.0571(12) Uani 1 1 d D . . N1 N 0.4913(5) 0.3839(5) 0.8344(2) 0.0297(11) Uani 1 1 d DU . . N2 N 0.7148(5) 0.1552(6) 0.6575(3) 0.0389(12) Uani 1 1 d DU . . N3 N 0.9402(5) 0.1619(5) 0.6713(3) 0.0374(12) Uani 1 1 d DU . . C1 C 0.4864(7) 0.2659(6) 0.8303(4) 0.0490(18) Uani 1 1 d DU . . H1 H 0.4820 0.2288 0.7890 0.059 Uiso 1 1 calc R . . C2 C 0.4876(8) 0.1973(8) 0.8842(5) 0.066(2) Uani 1 1 d DU . . H2 H 0.4837 0.1140 0.8801 0.079 Uiso 1 1 calc R . . C3 C 0.4945(8) 0.2511(8) 0.9434(5) 0.065(2) Uani 1 1 d DU . . H3 H 0.4954 0.2049 0.9810 0.078 Uiso 1 1 calc R . . C4 C 0.5003(6) 0.3710(7) 0.9492(3) 0.0410(15) Uani 1 1 d DU . . H4 H 0.5060 0.4093 0.9903 0.049 Uiso 1 1 calc R . . C5 C 0.4976(5) 0.4355(5) 0.8934(3) 0.0283(12) Uani 1 1 d DU . . C6 C 0.6009(8) 0.1608(8) 0.6551(6) 0.081(3) Uani 1 1 d DU . . H6 H 0.5586 0.1624 0.6940 0.097 Uiso 1 1 calc R . . C7 C 0.5473(11) 0.1642(11) 0.5975(8) 0.121(5) Uani 1 1 d DU . . H7 H 0.4666 0.1660 0.5966 0.146 Uiso 1 1 calc R . . C8 C 0.6067(12) 0.1649(10) 0.5418(7) 0.118(5) Uani 1 1 d DU . . H8 H 0.5692 0.1679 0.5017 0.142 Uiso 1 1 calc R . . C9 C 0.7217(10) 0.1613(7) 0.5444(4) 0.075(3) Uani 1 1 d DU . . H9 H 0.7649 0.1613 0.5056 0.090 Uiso 1 1 calc R . . C10 C 0.7759(6) 0.1575(5) 0.6026(3) 0.0322(12) Uani 1 1 d DU . . C11 C 0.9027(6) 0.1615(6) 0.6096(3) 0.0346(13) Uani 1 1 d DU . . C12 C 0.9829(9) 0.1654(7) 0.5601(5) 0.080(3) Uani 1 1 d DU . . H12 H 0.9567 0.1649 0.5167 0.096 Uiso 1 1 calc R . . C13 C 1.1007(11) 0.1699(11) 0.5732(7) 0.131(5) Uani 1 1 d DU . . H13 H 1.1567 0.1726 0.5392 0.157 Uiso 1 1 calc R . . C14 C 1.1356(10) 0.1704(10) 0.6351(8) 0.125(5) Uani 1 1 d DU . . H14 H 1.2179 0.1753 0.6445 0.150 Uiso 1 1 calc R . . C15 C 1.0557(7) 0.1641(7) 0.6846(6) 0.077(3) Uani 1 1 d DU . . H15 H 1.0805 0.1613 0.7279 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0271(8) 0.0459(9) 0.0186(7) 0.000 0.000 0.0098(7) Ti2 0.0624(9) 0.0429(8) 0.0199(5) -0.0007(6) 0.0036(7) -0.0085(6) F1 0.049(3) 0.084(4) 0.043(3) -0.031(2) 0.016(2) 0.011(2) F2 0.0319(19) 0.056(2) 0.033(2) 0.0037(17) 0.0034(17) 0.0174(17) F3 0.125(6) 0.087(4) 0.080(4) -0.034(3) 0.074(4) -0.015(4) F4 0.130(6) 0.096(5) 0.057(3) 0.048(3) -0.055(4) -0.033(4) F5 0.082(3) 0.040(2) 0.038(2) -0.012(2) 0.013(2) -0.004(2) F6 0.053(2) 0.040(2) 0.050(3) 0.022(2) 0.003(2) 0.0024(19) N1 0.015(2) 0.034(3) 0.038(3) 0.004(2) 0.005(2) 0.011(2) N2 0.034(3) 0.037(3) 0.045(3) -0.005(2) -0.001(2) 0.017(3) N3 0.028(3) 0.027(3) 0.048(3) 0.010(2) -0.003(2) 0.006(2) C1 0.043(4) 0.031(3) 0.073(5) -0.004(3) 0.012(4) 0.017(3) C2 0.041(4) 0.041(4) 0.124(7) 0.032(4) 0.030(5) 0.027(4) C3 0.036(4) 0.059(5) 0.093(5) 0.048(4) 0.009(4) 0.018(4) C4 0.024(3) 0.051(4) 0.034(3) 0.012(3) -0.002(3) 0.008(3) C5 0.016(3) 0.035(3) 0.028(3) 0.003(2) 0.003(2) 0.009(2) C6 0.043(5) 0.042(5) 0.160(9) -0.040(6) -0.009(5) 0.022(4) C7 0.061(6) 0.041(5) 0.268(14) -0.036(10) -0.092(8) 0.029(5) C8 0.127(10) 0.029(4) 0.172(10) 0.006(7) -0.117(8) 0.019(6) C9 0.098(6) 0.030(4) 0.060(5) 0.011(3) -0.047(4) 0.005(4) C10 0.045(3) 0.018(3) 0.028(3) -0.001(2) -0.012(2) 0.011(3) C11 0.036(3) 0.018(3) 0.041(3) 0.004(2) 0.013(2) 0.007(3) C12 0.091(6) 0.024(3) 0.088(6) -0.021(4) 0.067(5) 0.000(4) C13 0.078(7) 0.047(5) 0.241(12) -0.021(10) 0.110(9) 0.012(6) C14 0.029(5) 0.023(4) 0.314(15) 0.008(10) 0.037(7) 0.006(4) C15 0.036(4) 0.015(3) 0.164(8) 0.022(5) -0.028(5) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F1 1.791(5) . ? Ti1 F1 1.791(5) 4_665 ? Ti1 F2 1.829(3) . ? Ti1 F2 1.829(3) 4_665 ? Ti1 N1 2.188(5) 4_665 ? Ti1 N1 2.188(5) . ? Ti2 F3 1.768(6) . ? Ti2 F4 1.773(6) . ? Ti2 F5 1.822(4) . ? Ti2 F6 1.823(4) . ? Ti2 N2 2.170(6) . ? Ti2 N3 2.182(6) . ? N1 C1 1.346(8) . ? N1 C5 1.351(7) . ? N2 C10 1.336(8) . ? N2 C6 1.358(9) . ? N3 C11 1.352(8) . ? N3 C15 1.359(8) . ? C1 C2 1.378(10) . ? C1 H1 0.9500 . ? C2 C3 1.364(11) . ? C2 H2 0.9500 . ? C3 C4 1.367(10) . ? C3 H3 0.9500 . ? C4 C5 1.387(8) . ? C4 H4 0.9500 . ? C5 C5 1.473(10) 4_665 ? C6 C7 1.358(13) . ? C6 H6 0.9500 . ? C7 C8 1.345(14) . ? C7 H7 0.9500 . ? C8 C9 1.359(13) . ? C8 H8 0.9500 . ? C9 C10 1.374(8) . ? C9 H9 0.9500 . ? C10 C11 1.459(8) . ? C11 C12 1.373(8) . ? C12 C13 1.371(14) . ? C12 H12 0.9500 . ? C13 C14 1.346(15) . ? C13 H13 0.9500 . ? C14 C15 1.362(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? 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 F1 Ti1 F1 105.0(4) . 4_665 ? F1 Ti1 F2 94.0(2) . . ? F1 Ti1 F2 92.9(2) 4_665 . ? F1 Ti1 F2 92.9(2) . 4_665 ? F1 Ti1 F2 94.0(2) 4_665 4_665 ? F2 Ti1 F2 168.6(3) . 4_665 ? F1 Ti1 N1 164.0(3) . 4_665 ? F1 Ti1 N1 91.0(2) 4_665 4_665 ? F2 Ti1 N1 85.60(18) . 4_665 ? F2 Ti1 N1 85.27(18) 4_665 4_665 ? F1 Ti1 N1 91.0(2) . . ? F1 Ti1 N1 164.0(3) 4_665 . ? F2 Ti1 N1 85.27(18) . . ? F2 Ti1 N1 85.60(18) 4_665 . ? N1 Ti1 N1 73.1(3) 4_665 . ? F3 Ti2 F4 103.7(4) . . ? F3 Ti2 F5 95.6(3) . . ? F4 Ti2 F5 92.4(3) . . ? F3 Ti2 F6 93.4(3) . . ? F4 Ti2 F6 95.3(3) . . ? F5 Ti2 F6 166.5(2) . . ? F3 Ti2 N2 91.9(3) . . ? F4 Ti2 N2 164.4(3) . . ? F5 Ti2 N2 84.4(2) . . ? F6 Ti2 N2 85.2(2) . . ? F3 Ti2 N3 165.1(3) . . ? F4 Ti2 N3 91.2(3) . . ? F5 Ti2 N3 84.4(2) . . ? F6 Ti2 N3 84.3(2) . . ? N2 Ti2 N3 73.3(2) . . ? C1 N1 C5 118.3(5) . . ? C1 N1 Ti1 123.0(5) . . ? C5 N1 Ti1 118.7(4) . . ? C10 N2 C6 119.4(7) . . ? C10 N2 Ti2 118.4(4) . . ? C6 N2 Ti2 122.2(6) . . ? C11 N3 C15 120.4(7) . . ? C11 N3 Ti2 118.1(4) . . ? C15 N3 Ti2 121.5(6) . . ? N1 C1 C2 122.2(7) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.8(7) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.5(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.3(7) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C5 114.7(3) . 4_665 ? C4 C5 C5 123.4(4) . 4_665 ? C7 C6 N2 120.3(10) . . ? C7 C6 H6 119.8 . . ? N2 C6 H6 119.8 . . ? C8 C7 C6 121.0(10) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 118.4(10) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C8 C9 C10 120.6(10) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N2 C10 C9 120.2(7) . . ? N2 C10 C11 115.8(5) . . ? C9 C10 C11 124.0(7) . . ? N3 C11 C12 119.8(7) . . ? N3 C11 C10 114.4(5) . . ? C12 C11 C10 125.8(7) . . ? C13 C12 C11 120.1(10) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 118.9(10) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 121.6(10) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? N3 C15 C14 119.2(10) . . ? N3 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.684 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.095 #===END OF CIF ============================================================== # 09mj44d.cif data_09mj44 _database_code_depnum_ccdc_archive 'CCDC 783183' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-05-07 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluorobis(triphenylarsine oxide)titanium(IV) dichloromethane solvate ; # C18H16AsO ligand = # triphenylarsine oxide (ACD iLab defaults) # triphenylarsane oxide (ACD iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 As2 F4 O2 Ti, 2(C H2 Cl2)' _chemical_formula_sum 'C38 H34 As2 Cl4 F4 O2 Ti' _chemical_formula_weight 938.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.091(3) _cell_length_b 16.284(5) _cell_length_c 16.152(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3969.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2435 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 61.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 6.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8086 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Sapphire3 (Gemini Cu)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7366 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 61.76 _reflns_number_total 3046 _reflns_number_gt 2346 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3046 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.5000 0.11829(5) 0.2500 0.0295(2) Uani 1 2 d S . . As1 As 0.55919(2) 0.26061(2) 0.10881(2) 0.03247(16) Uani 1 1 d . . . F1 F 0.57525(13) 0.12549(13) 0.33983(13) 0.0444(5) Uani 1 1 d . . . F2 F 0.57113(13) 0.04053(13) 0.20333(14) 0.0466(5) Uani 1 1 d . . . O1 O 0.57246(15) 0.20613(15) 0.19535(15) 0.0372(6) Uani 1 1 d . . . C1 C 0.4620(3) 0.3363(2) 0.1128(2) 0.0437(9) Uani 1 1 d . . . C2 C 0.3764(3) 0.3085(3) 0.1094(2) 0.0497(10) Uani 1 1 d . . . H2 H 0.3651 0.2523 0.1082 0.060 Uiso 1 1 calc R . . C3 C 0.3069(3) 0.3638(3) 0.1077(3) 0.0639(13) Uani 1 1 d . . . H3 H 0.2489 0.3447 0.1057 0.077 Uiso 1 1 calc R . . C4 C 0.3224(4) 0.4449(4) 0.1091(3) 0.0817(17) Uani 1 1 d . . . H4 H 0.2753 0.4817 0.1079 0.098 Uiso 1 1 calc R . . C5 C 0.4076(4) 0.4732(4) 0.1122(5) 0.115(3) Uani 1 1 d . . . H5 H 0.4182 0.5294 0.1131 0.138 Uiso 1 1 calc R . . C6 C 0.4784(4) 0.4188(3) 0.1138(4) 0.089(2) Uani 1 1 d . . . H6 H 0.5363 0.4383 0.1156 0.106 Uiso 1 1 calc R . . C7 C 0.5467(2) 0.1951(2) 0.0115(2) 0.0357(8) Uani 1 1 d . . . C8 C 0.5132(3) 0.2312(2) -0.0592(2) 0.0484(10) Uani 1 1 d . . . H8 H 0.4909 0.2844 -0.0576 0.058 Uiso 1 1 calc R . . C9 C 0.5132(3) 0.1875(3) -0.1321(3) 0.0597(12) Uani 1 1 d . . . H9 H 0.4913 0.2115 -0.1802 0.072 Uiso 1 1 calc R . . C10 C 0.5453(3) 0.1085(3) -0.1344(3) 0.0529(12) Uani 1 1 d . . . H10 H 0.5463 0.0798 -0.1842 0.063 Uiso 1 1 calc R . . C11 C 0.5755(3) 0.0724(3) -0.0641(3) 0.0473(10) Uani 1 1 d . . . H11 H 0.5955 0.0184 -0.0657 0.057 Uiso 1 1 calc R . . C12 C 0.5769(2) 0.1155(2) 0.0105(2) 0.0399(9) Uani 1 1 d . . . H12 H 0.5978 0.0909 0.0586 0.048 Uiso 1 1 calc R . . C13 C 0.6662(3) 0.3225(2) 0.0967(2) 0.0377(9) Uani 1 1 d . . . C14 C 0.7047(3) 0.3332(2) 0.0196(3) 0.0474(10) Uani 1 1 d . . . H14 H 0.6788 0.3103 -0.0272 0.057 Uiso 1 1 calc R . . C15 C 0.7815(3) 0.3779(2) 0.0131(3) 0.0550(11) Uani 1 1 d . . . H15 H 0.8075 0.3863 -0.0384 0.066 Uiso 1 1 calc R . . C16 C 0.8201(3) 0.4105(3) 0.0837(3) 0.0573(12) Uani 1 1 d . . . H16 H 0.8725 0.4402 0.0792 0.069 Uiso 1 1 calc R . . C17 C 0.7822(3) 0.3996(3) 0.1597(3) 0.0634(13) Uani 1 1 d . . . H17 H 0.8082 0.4225 0.2065 0.076 Uiso 1 1 calc R . . C18 C 0.7056(3) 0.3545(3) 0.1669(3) 0.0545(11) Uani 1 1 d . . . H18 H 0.6804 0.3457 0.2186 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.81701(18) 0.11544(17) 0.11776(12) 0.1546(10) Uani 1 1 d . . . Cl2 Cl 0.83398(13) 0.17817(11) 0.28361(11) 0.1136(6) Uani 1 1 d . . . C19 C 0.7736(4) 0.1221(4) 0.2137(4) 0.0946(19) Uani 1 1 d . . . H19A H 0.7664 0.0669 0.2353 0.114 Uiso 1 1 calc R . . H19B H 0.7150 0.1462 0.2094 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0344(5) 0.0267(4) 0.0275(5) 0.000 0.0019(4) 0.000 As1 0.0381(2) 0.0300(2) 0.0292(3) 0.00020(16) 0.00101(17) -0.00382(17) F1 0.0468(12) 0.0504(13) 0.0361(12) 0.0060(10) -0.0079(10) -0.0001(10) F2 0.0517(12) 0.0387(12) 0.0493(13) -0.0067(10) 0.0089(11) 0.0069(10) O1 0.0432(13) 0.0378(13) 0.0306(14) 0.0019(11) 0.0015(11) -0.0078(11) C1 0.054(2) 0.039(2) 0.037(2) 0.0020(18) -0.0005(19) 0.0041(19) C2 0.048(2) 0.045(2) 0.056(3) 0.002(2) -0.006(2) 0.005(2) C3 0.055(3) 0.071(3) 0.066(3) 0.010(3) -0.006(2) 0.018(2) C4 0.078(4) 0.076(4) 0.091(4) 0.006(3) 0.001(3) 0.037(3) C5 0.101(5) 0.039(3) 0.204(8) -0.002(4) 0.002(5) 0.023(3) C6 0.067(3) 0.044(3) 0.155(6) -0.009(3) 0.001(4) 0.007(3) C7 0.0369(19) 0.0376(19) 0.033(2) 0.0014(16) 0.0012(17) -0.0078(16) C8 0.065(3) 0.043(2) 0.037(2) 0.0040(18) -0.006(2) -0.005(2) C9 0.082(3) 0.068(3) 0.029(2) 0.006(2) -0.012(2) -0.019(3) C10 0.054(3) 0.068(3) 0.036(2) -0.016(2) 0.010(2) -0.022(2) C11 0.052(2) 0.045(2) 0.045(2) -0.012(2) 0.008(2) -0.0054(19) C12 0.043(2) 0.043(2) 0.034(2) -0.0001(17) -0.0017(17) -0.0005(17) C13 0.044(2) 0.0300(18) 0.039(2) 0.0033(16) 0.0010(17) -0.0048(16) C14 0.057(2) 0.045(2) 0.040(2) 0.0032(19) 0.004(2) -0.010(2) C15 0.053(2) 0.050(2) 0.062(3) 0.010(2) 0.014(2) -0.009(2) C16 0.043(2) 0.044(2) 0.085(3) 0.016(2) -0.004(2) -0.011(2) C17 0.065(3) 0.058(3) 0.067(3) 0.004(2) -0.021(3) -0.020(2) C18 0.063(3) 0.055(2) 0.046(3) -0.003(2) -0.003(2) -0.018(2) Cl1 0.182(2) 0.191(2) 0.0912(14) -0.0232(14) 0.0316(14) -0.0794(19) Cl2 0.1372(14) 0.1122(13) 0.0914(11) -0.0047(10) -0.0280(11) -0.0158(12) C19 0.068(3) 0.124(5) 0.092(4) -0.003(4) -0.012(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F2 1.823(2) 3_655 ? Ti1 F2 1.823(2) . ? Ti1 F1 1.846(2) . ? Ti1 F1 1.846(2) 3_655 ? Ti1 O1 2.005(2) 3_655 ? Ti1 O1 2.005(2) . ? As1 O1 1.668(2) . ? As1 C7 1.909(4) . ? As1 C1 1.917(4) . ? As1 C13 1.913(4) . ? C1 C2 1.370(5) . ? C1 C6 1.366(6) . ? C2 C3 1.384(6) . ? C2 H2 0.9300 . ? C3 C4 1.341(7) . ? C3 H3 0.9300 . ? C4 C5 1.367(8) . ? C4 H4 0.9300 . ? C5 C6 1.389(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.373(5) . ? C7 C8 1.382(5) . ? C8 C9 1.376(6) . ? C8 H8 0.9300 . ? C9 C10 1.375(7) . ? C9 H9 0.9300 . ? C10 C11 1.358(6) . ? C10 H10 0.9300 . ? C11 C12 1.394(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.382(5) . ? C13 C14 1.385(5) . ? C14 C15 1.372(5) . ? C14 H14 0.9300 . ? C15 C16 1.386(6) . ? C15 H15 0.9300 . ? C16 C17 1.367(6) . ? C16 H16 0.9300 . ? C17 C18 1.374(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? Cl1 C19 1.685(6) . ? Cl2 C19 1.715(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? 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 F2 Ti1 F2 92.02(14) 3_655 . ? F2 Ti1 F1 94.67(10) 3_655 . ? F2 Ti1 F1 90.39(10) . . ? F2 Ti1 F1 90.39(10) 3_655 3_655 ? F2 Ti1 F1 94.67(10) . 3_655 ? F1 Ti1 F1 172.72(14) . 3_655 ? F2 Ti1 O1 89.56(10) 3_655 3_655 ? F2 Ti1 O1 176.88(10) . 3_655 ? F1 Ti1 O1 86.80(10) . 3_655 ? F1 Ti1 O1 88.01(10) 3_655 3_655 ? F2 Ti1 O1 176.88(10) 3_655 . ? F2 Ti1 O1 89.56(10) . . ? F1 Ti1 O1 88.01(10) . . ? F1 Ti1 O1 86.80(10) 3_655 . ? O1 Ti1 O1 88.99(15) 3_655 . ? O1 As1 C7 113.85(14) . . ? O1 As1 C1 113.92(14) . . ? C7 As1 C1 108.19(16) . . ? O1 As1 C13 105.33(14) . . ? C7 As1 C13 107.07(15) . . ? C1 As1 C13 108.09(17) . . ? As1 O1 Ti1 133.08(14) . . ? C2 C1 C6 119.8(4) . . ? C2 C1 As1 120.5(3) . . ? C6 C1 As1 119.6(3) . . ? C1 C2 C3 120.0(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.7(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.2(5) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C12 C7 C8 120.8(4) . . ? C12 C7 As1 120.4(3) . . ? C8 C7 As1 118.6(3) . . ? C9 C8 C7 119.2(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 118.8(4) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C18 C13 C14 120.6(4) . . ? C18 C13 As1 118.6(3) . . ? C14 C13 As1 120.8(3) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.8(4) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 119.7(4) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? Cl1 C19 Cl2 115.6(3) . . ? Cl1 C19 H19A 108.4 . . ? Cl2 C19 H19A 108.4 . . ? Cl1 C19 H19B 108.4 . . ? Cl2 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 61.76 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.834 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.072 #===END OF CIF ============================================================== # 10bl327a1.cif data_10bl327a _database_code_depnum_ccdc_archive 'CCDC 783184' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-30 _audit_author_name 'Zhang, Wenjian' _chemical_name_systematic ; benzene-1,2-diylbis(diphenylphosphonium) hexakis(mu2-fluoro)dodecafluoro-tetratitanium(IV) ; # [o-C6H4{P(H)Ph2}2]2+ = # 1,2-phenylenebis(diphenylphosphonium) (iLab defaults) # benzene-1,2-diylbis(diphenylphosphonium) (ACD/iLab selected options) # [Ti4F18]2- = hexakis(mu2-fluoro)dodecafluorotetratitanium(IV) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 P2 2+, F18 Ti4 2-' _chemical_formula_sum 'C30 H26 F18 P2 Ti4' _chemical_formula_weight 982.05 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'P 21/n' _space_group_IT_number 14 _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 15.2643(15) _cell_length_b 14.9245(15) _cell_length_c 16.7471(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.312(7) _cell_angle_gamma 90.00 _cell_volume 3696.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 27899 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7355 # shelxl 0.8861 _exptl_absorpt_correction_T_max 1.0000 # 0.9219 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39584 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0811 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7245 _reflns_number_gt 5056 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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_hydrogen_treatment 'constr (C-H), refxyz (P-H)' P-H distances restrained to be the same with Hs having a common refined Uiso. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+32.8641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed # 'constr (C-H), refxyz (P-H)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7245 _refine_ls_number_parameters 494 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.89295(8) 0.65515(8) 0.03578(7) 0.0210(3) Uani 1 1 d . . . Ti2 Ti 0.65128(8) 0.58624(8) 0.04145(7) 0.0194(3) Uani 1 1 d . . . Ti3 Ti 0.71836(8) 0.83653(7) 0.04761(7) 0.0201(3) Uani 1 1 d . . . Ti4 Ti 0.69312(8) 0.70046(8) -0.15153(7) 0.0191(3) Uani 1 1 d . . . F1 F 0.8293(2) 0.7647(2) 0.0584(2) 0.0229(8) Uani 1 1 d . . . F2 F 0.7830(2) 0.5946(2) 0.0576(2) 0.0220(8) Uani 1 1 d . . . F3 F 0.6665(2) 0.7177(2) 0.0673(2) 0.0227(8) Uani 1 1 d . . . F4 F 0.8121(2) 0.6694(2) -0.0763(2) 0.0217(8) Uani 1 1 d . . . F5 F 0.6477(2) 0.6243(2) -0.0718(2) 0.0234(8) Uani 1 1 d . . . F6 F 0.6935(2) 0.7933(2) -0.0670(2) 0.0208(8) Uani 1 1 d . . . F7 F 0.9277(3) 0.5504(3) 0.0060(2) 0.0311(9) Uani 1 1 d . . . F8 F 0.9473(3) 0.6474(3) 0.1415(2) 0.0326(9) Uani 1 1 d . . . F9 F 0.9743(3) 0.7228(3) 0.0056(2) 0.0308(9) Uani 1 1 d . . . F10 F 0.6510(3) 0.4736(2) 0.0118(2) 0.0290(9) Uani 1 1 d . . . F11 F 0.6650(2) 0.5650(2) 0.1490(2) 0.0257(8) Uani 1 1 d . . . F12 F 0.5326(2) 0.6054(2) 0.0227(2) 0.0260(8) Uani 1 1 d . . . F13 F 0.7717(3) 0.9325(2) 0.0197(2) 0.0276(9) Uani 1 1 d . . . F14 F 0.6067(3) 0.8806(2) 0.0292(2) 0.0295(9) Uani 1 1 d . . . F15 F 0.7495(3) 0.8559(3) 0.1552(2) 0.0288(9) Uani 1 1 d . . . F16 F 0.7007(3) 0.6045(2) -0.2118(2) 0.0284(9) Uani 1 1 d . . . F17 F 0.5810(2) 0.7297(2) -0.2007(2) 0.0272(9) Uani 1 1 d . . . F18 F 0.7500(2) 0.7748(2) -0.2045(2) 0.0267(9) Uani 1 1 d . . . P1 P 0.02690(12) 0.14561(11) 0.28823(10) 0.0229(4) Uani 1 1 d D . . P2 P 0.09049(11) 0.30147(11) 0.44479(10) 0.0197(4) Uani 1 1 d D . . H1 H -0.031(4) 0.119(4) 0.330(3) 0.017(11) Uiso 1 1 d D . . H2 H 0.006(3) 0.275(4) 0.423(4) 0.017(11) Uiso 1 1 d D . . C1 C 0.0259(4) 0.0609(4) 0.2137(4) 0.0225(14) Uani 1 1 d . . . C2 C 0.0712(5) 0.0741(5) 0.1503(4) 0.0301(16) Uani 1 1 d . . . H2A H 0.0997 0.1297 0.1453 0.036 Uiso 1 1 calc R . . C3 C 0.0732(5) 0.0049(5) 0.0958(4) 0.0343(17) Uani 1 1 d . . . H3 H 0.1041 0.0125 0.0535 0.041 Uiso 1 1 calc R . . C4 C 0.0304(5) -0.0754(5) 0.1030(5) 0.0378(18) Uani 1 1 d . . . H4 H 0.0324 -0.1225 0.0653 0.045 Uiso 1 1 calc R . . C5 C -0.0149(5) -0.0884(5) 0.1635(4) 0.0337(17) Uani 1 1 d . . . H5 H -0.0445 -0.1437 0.1669 0.040 Uiso 1 1 calc R . . C6 C -0.0174(5) -0.0208(5) 0.2196(4) 0.0331(17) Uani 1 1 d . . . H6 H -0.0482 -0.0297 0.2618 0.040 Uiso 1 1 calc R . . C7 C -0.0172(4) 0.2493(4) 0.2433(4) 0.0208(13) Uani 1 1 d . . . C8 C -0.1049(4) 0.2727(5) 0.2445(4) 0.0268(15) Uani 1 1 d . . . H8 H -0.1390 0.2354 0.2714 0.032 Uiso 1 1 calc R . . C9 C -0.1422(5) 0.3507(5) 0.2062(4) 0.0317(16) Uani 1 1 d . . . H9 H -0.2016 0.3679 0.2081 0.038 Uiso 1 1 calc R . . C10 C -0.0931(5) 0.4039(5) 0.1650(4) 0.0309(16) Uani 1 1 d . . . H10 H -0.1201 0.4562 0.1370 0.037 Uiso 1 1 calc R . . C11 C -0.0054(5) 0.3818(4) 0.1641(4) 0.0291(16) Uani 1 1 d . . . H11 H 0.0283 0.4194 0.1369 0.035 Uiso 1 1 calc R . . C12 C 0.0330(4) 0.3048(5) 0.2029(4) 0.0250(15) Uani 1 1 d . . . H12 H 0.0931 0.2891 0.2024 0.030 Uiso 1 1 calc R . . C13 C 0.1395(4) 0.1546(4) 0.3547(4) 0.0198(13) Uani 1 1 d . . . C14 C 0.2030(5) 0.0937(4) 0.3429(4) 0.0264(15) Uani 1 1 d . . . H14 H 0.1865 0.0512 0.2995 0.032 Uiso 1 1 calc R . . C15 C 0.2902(5) 0.0928(5) 0.3926(4) 0.0305(16) Uani 1 1 d . . . H15 H 0.3330 0.0504 0.3831 0.037 Uiso 1 1 calc R . . C16 C 0.3146(5) 0.1537(5) 0.4561(4) 0.0304(16) Uani 1 1 d . . . H16 H 0.3743 0.1538 0.4905 0.036 Uiso 1 1 calc R . . C17 C 0.2515(5) 0.2150(5) 0.4695(4) 0.0281(15) Uani 1 1 d . . . H17 H 0.2690 0.2572 0.5130 0.034 Uiso 1 1 calc R . . C18 C 0.1640(4) 0.2163(4) 0.4215(4) 0.0216(14) Uani 1 1 d . . . C19 C 0.1205(4) 0.3185(4) 0.5539(4) 0.0224(14) Uani 1 1 d . . . C20 C 0.0980(5) 0.2528(5) 0.6046(4) 0.0264(15) Uani 1 1 d . . . H20 H 0.0644 0.2015 0.5813 0.032 Uiso 1 1 calc R . . C21 C 0.1251(5) 0.2632(5) 0.6888(4) 0.0292(16) Uani 1 1 d . . . H21 H 0.1084 0.2200 0.7241 0.035 Uiso 1 1 calc R . . C22 C 0.1772(5) 0.3370(5) 0.7222(4) 0.0298(16) Uani 1 1 d . . . H22 H 0.1970 0.3430 0.7804 0.036 Uiso 1 1 calc R . . C23 C 0.2005(5) 0.4017(5) 0.6722(4) 0.0312(16) Uani 1 1 d . . . H23 H 0.2365 0.4515 0.6958 0.037 Uiso 1 1 calc R . . C24 C 0.1707(5) 0.3934(5) 0.5864(4) 0.0269(15) Uani 1 1 d . . . H24 H 0.1846 0.4382 0.5512 0.032 Uiso 1 1 calc R . . C25 C 0.0995(5) 0.4021(4) 0.3887(4) 0.0226(14) Uani 1 1 d . . . C26 C 0.0297(5) 0.4646(4) 0.3749(4) 0.0280(15) Uani 1 1 d . . . H26 H -0.0218 0.4551 0.3960 0.034 Uiso 1 1 calc R . . C27 C 0.0366(5) 0.5403(5) 0.3303(5) 0.0330(17) Uani 1 1 d . . . H27 H -0.0102 0.5838 0.3206 0.040 Uiso 1 1 calc R . . C28 C 0.1123(5) 0.5534(5) 0.2992(4) 0.0271(15) Uani 1 1 d . . . H28 H 0.1156 0.6050 0.2669 0.033 Uiso 1 1 calc R . . C29 C 0.1813(5) 0.4935(5) 0.3141(4) 0.0289(16) Uani 1 1 d . . . H29 H 0.2335 0.5046 0.2943 0.035 Uiso 1 1 calc R . . C30 C 0.1755(5) 0.4158(5) 0.3585(4) 0.0268(15) Uani 1 1 d . . . H30 H 0.2228 0.3728 0.3680 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0181(6) 0.0230(6) 0.0227(6) 0.0000(5) 0.0062(5) 0.0026(5) Ti2 0.0191(6) 0.0201(6) 0.0205(6) -0.0001(5) 0.0073(5) -0.0003(5) Ti3 0.0225(6) 0.0173(6) 0.0220(6) -0.0033(5) 0.0087(5) 0.0011(5) Ti4 0.0214(6) 0.0192(6) 0.0176(6) -0.0004(5) 0.0064(5) 0.0018(5) F1 0.0210(19) 0.0223(19) 0.026(2) -0.0024(15) 0.0071(16) 0.0012(16) F2 0.0210(19) 0.0189(18) 0.027(2) 0.0012(15) 0.0079(16) 0.0019(15) F3 0.029(2) 0.0187(18) 0.0236(19) -0.0027(15) 0.0125(16) 0.0023(15) F4 0.0222(19) 0.0218(19) 0.0221(19) -0.0003(15) 0.0071(15) 0.0010(15) F5 0.027(2) 0.0221(19) 0.0220(19) -0.0014(15) 0.0081(16) -0.0016(16) F6 0.0222(19) 0.0205(18) 0.0207(18) -0.0022(15) 0.0071(15) 0.0020(15) F7 0.032(2) 0.025(2) 0.037(2) -0.0013(18) 0.0110(18) 0.0101(18) F8 0.025(2) 0.043(2) 0.026(2) 0.0014(18) 0.0001(16) 0.0039(19) F9 0.025(2) 0.030(2) 0.040(2) 0.0001(18) 0.0119(18) -0.0016(17) F10 0.035(2) 0.0194(19) 0.035(2) -0.0034(17) 0.0130(18) -0.0033(17) F11 0.028(2) 0.031(2) 0.0197(19) 0.0052(16) 0.0085(16) -0.0006(17) F12 0.0196(19) 0.027(2) 0.032(2) 0.0021(17) 0.0074(16) 0.0009(16) F13 0.036(2) 0.0161(18) 0.033(2) -0.0006(16) 0.0136(18) -0.0030(16) F14 0.027(2) 0.026(2) 0.039(2) -0.0017(17) 0.0140(18) 0.0090(17) F15 0.035(2) 0.029(2) 0.0223(19) -0.0032(16) 0.0080(17) -0.0004(18) F16 0.037(2) 0.027(2) 0.024(2) -0.0039(16) 0.0118(17) 0.0029(18) F17 0.026(2) 0.029(2) 0.025(2) -0.0005(16) 0.0033(16) 0.0035(17) F18 0.028(2) 0.029(2) 0.025(2) 0.0066(16) 0.0122(17) 0.0007(17) P1 0.0245(9) 0.0229(9) 0.0230(9) -0.0004(7) 0.0091(7) -0.0019(7) P2 0.0217(8) 0.0192(8) 0.0183(8) -0.0006(7) 0.0050(7) -0.0005(7) C1 0.024(3) 0.021(3) 0.021(3) -0.002(3) 0.004(3) 0.000(3) C2 0.035(4) 0.029(4) 0.027(4) -0.003(3) 0.011(3) -0.007(3) C3 0.040(4) 0.037(4) 0.026(4) -0.009(3) 0.008(3) 0.000(3) C4 0.047(5) 0.031(4) 0.032(4) -0.014(3) 0.003(4) -0.005(4) C5 0.039(4) 0.026(4) 0.031(4) -0.001(3) -0.001(3) -0.004(3) C6 0.036(4) 0.034(4) 0.030(4) 0.000(3) 0.008(3) -0.007(3) C7 0.020(3) 0.023(3) 0.019(3) -0.002(3) 0.004(3) 0.001(3) C8 0.021(3) 0.034(4) 0.026(4) -0.001(3) 0.006(3) -0.001(3) C9 0.029(4) 0.034(4) 0.034(4) 0.002(3) 0.012(3) 0.008(3) C10 0.038(4) 0.030(4) 0.025(4) 0.005(3) 0.008(3) 0.005(3) C11 0.038(4) 0.022(3) 0.030(4) 0.002(3) 0.015(3) -0.003(3) C12 0.020(3) 0.033(4) 0.023(3) -0.004(3) 0.007(3) -0.004(3) C13 0.026(3) 0.017(3) 0.018(3) 0.006(2) 0.008(3) -0.002(3) C14 0.034(4) 0.023(3) 0.023(3) -0.001(3) 0.008(3) 0.000(3) C15 0.031(4) 0.037(4) 0.027(4) 0.002(3) 0.015(3) 0.009(3) C16 0.019(3) 0.036(4) 0.033(4) 0.003(3) 0.001(3) 0.005(3) C17 0.029(4) 0.029(4) 0.024(4) 0.003(3) 0.002(3) 0.003(3) C18 0.022(3) 0.018(3) 0.025(3) 0.003(3) 0.008(3) 0.001(3) C19 0.022(3) 0.025(3) 0.020(3) 0.003(3) 0.005(3) 0.002(3) C20 0.030(4) 0.026(4) 0.023(3) -0.003(3) 0.006(3) -0.008(3) C21 0.025(4) 0.034(4) 0.029(4) 0.012(3) 0.009(3) 0.003(3) C22 0.026(4) 0.044(4) 0.020(3) -0.001(3) 0.006(3) 0.013(3) C23 0.031(4) 0.031(4) 0.029(4) -0.003(3) 0.002(3) -0.002(3) C24 0.028(4) 0.028(4) 0.025(4) -0.002(3) 0.007(3) -0.003(3) C25 0.033(4) 0.024(3) 0.012(3) -0.005(3) 0.008(3) -0.004(3) C26 0.025(4) 0.025(4) 0.039(4) 0.002(3) 0.017(3) 0.004(3) C27 0.039(4) 0.020(3) 0.045(4) 0.006(3) 0.019(4) 0.004(3) C28 0.035(4) 0.023(3) 0.026(4) -0.004(3) 0.012(3) -0.002(3) C29 0.033(4) 0.029(4) 0.030(4) -0.002(3) 0.018(3) -0.001(3) C30 0.023(4) 0.027(4) 0.032(4) 0.007(3) 0.012(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F7 1.762(4) . ? Ti1 F8 1.764(4) . ? Ti1 F9 1.769(4) . ? Ti1 F1 1.986(4) . ? Ti1 F4 1.987(4) . ? Ti1 F2 2.016(4) . ? Ti2 F10 1.753(4) . ? Ti2 F12 1.783(4) . ? Ti2 F11 1.790(4) . ? Ti2 F2 1.966(4) . ? Ti2 F5 1.967(4) . ? Ti2 F3 2.010(4) . ? Ti3 F13 1.767(4) . ? Ti3 F15 1.770(4) . ? Ti3 F14 1.781(4) . ? Ti3 F6 1.971(3) . ? Ti3 F1 1.975(4) . ? Ti3 F3 2.002(4) . ? Ti4 F17 1.761(4) . ? Ti4 F16 1.772(4) . ? Ti4 F18 1.776(4) . ? Ti4 F6 1.980(3) . ? Ti4 F4 1.992(4) . ? Ti4 F5 2.005(4) . ? P1 C1 1.774(6) . ? P1 C7 1.779(6) . ? P1 C13 1.807(7) . ? P1 H1 1.31(4) . ? P2 C19 1.789(6) . ? P2 C25 1.794(7) . ? P2 C18 1.802(6) . ? P2 H2 1.31(4) . ? C1 C6 1.402(9) . ? C1 C2 1.416(9) . ? C2 C3 1.384(10) . ? C2 H2A 0.9500 . ? C3 C4 1.384(10) . ? C3 H3 0.9500 . ? C4 C5 1.374(11) . ? C4 H4 0.9500 . ? C5 C6 1.385(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.388(9) . ? C7 C12 1.410(9) . ? C8 C9 1.382(10) . ? C8 H8 0.9500 . ? C9 C10 1.388(10) . ? C9 H9 0.9500 . ? C10 C11 1.383(10) . ? C10 H10 0.9500 . ? C11 C12 1.377(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.377(9) . ? C13 C18 1.425(9) . ? C14 C15 1.386(10) . ? C14 H14 0.9500 . ? C15 C16 1.379(10) . ? C15 H15 0.9500 . ? C16 C17 1.386(10) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 H17 0.9500 . ? C19 C24 1.387(9) . ? C19 C20 1.395(9) . ? C20 C21 1.377(9) . ? C20 H20 0.9500 . ? C21 C22 1.393(10) . ? C21 H21 0.9500 . ? C22 C23 1.381(10) . ? C22 H22 0.9500 . ? C23 C24 1.401(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.391(9) . ? C25 C26 1.392(9) . ? C26 C27 1.373(9) . ? C26 H26 0.9500 . ? C27 C28 1.393(10) . ? C27 H27 0.9500 . ? C28 C29 1.357(10) . ? C28 H28 0.9500 . ? C29 C30 1.391(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 F7 Ti1 F8 97.24(19) . . ? F7 Ti1 F9 98.30(19) . . ? F8 Ti1 F9 97.74(19) . . ? F7 Ti1 F1 168.62(18) . . ? F8 Ti1 F1 89.62(17) . . ? F9 Ti1 F1 89.71(17) . . ? F7 Ti1 F4 89.33(17) . . ? F8 Ti1 F4 169.67(17) . . ? F9 Ti1 F4 89.15(17) . . ? F1 Ti1 F4 82.69(15) . . ? F7 Ti1 F2 88.60(17) . . ? F8 Ti1 F2 89.72(17) . . ? F9 Ti1 F2 169.08(17) . . ? F1 Ti1 F2 82.34(15) . . ? F4 Ti1 F2 82.45(15) . . ? F10 Ti2 F12 99.96(18) . . ? F10 Ti2 F11 96.16(18) . . ? F12 Ti2 F11 93.83(17) . . ? F10 Ti2 F2 91.74(17) . . ? F12 Ti2 F2 166.92(17) . . ? F11 Ti2 F2 90.68(16) . . ? F10 Ti2 F5 90.33(17) . . ? F12 Ti2 F5 89.92(16) . . ? F11 Ti2 F5 171.82(17) . . ? F2 Ti2 F5 84.13(15) . . ? F10 Ti2 F3 171.56(17) . . ? F12 Ti2 F3 86.55(16) . . ? F11 Ti2 F3 88.69(16) . . ? F2 Ti2 F3 81.27(15) . . ? F5 Ti2 F3 84.29(15) . . ? F13 Ti3 F15 96.44(18) . . ? F13 Ti3 F14 97.94(18) . . ? F15 Ti3 F14 96.94(18) . . ? F13 Ti3 F6 89.87(16) . . ? F15 Ti3 F6 169.59(17) . . ? F14 Ti3 F6 90.35(17) . . ? F13 Ti3 F1 91.32(17) . . ? F15 Ti3 F1 89.27(17) . . ? F14 Ti3 F1 168.17(17) . . ? F6 Ti3 F1 82.29(15) . . ? F13 Ti3 F3 171.27(17) . . ? F15 Ti3 F3 89.66(16) . . ? F14 Ti3 F3 87.46(17) . . ? F6 Ti3 F3 83.22(14) . . ? F1 Ti3 F3 82.50(15) . . ? F17 Ti4 F16 97.32(18) . . ? F17 Ti4 F18 98.66(18) . . ? F16 Ti4 F18 96.38(18) . . ? F17 Ti4 F6 89.47(16) . . ? F16 Ti4 F6 169.65(17) . . ? F18 Ti4 F6 90.27(16) . . ? F17 Ti4 F4 169.10(17) . . ? F16 Ti4 F4 89.68(17) . . ? F18 Ti4 F4 88.81(16) . . ? F6 Ti4 F4 82.52(14) . . ? F17 Ti4 F5 89.75(17) . . ? F16 Ti4 F5 90.19(16) . . ? F18 Ti4 F5 168.55(17) . . ? F6 Ti4 F5 82.00(14) . . ? F4 Ti4 F5 81.85(15) . . ? Ti3 F1 Ti1 151.5(2) . . ? Ti2 F2 Ti1 150.74(19) . . ? Ti3 F3 Ti2 149.12(19) . . ? Ti1 F4 Ti4 151.49(19) . . ? Ti2 F5 Ti4 151.0(2) . . ? Ti3 F6 Ti4 153.0(2) . . ? C1 P1 C7 112.7(3) . . ? C1 P1 C13 109.1(3) . . ? C7 P1 C13 113.5(3) . . ? C1 P1 H1 106(3) . . ? C7 P1 H1 105(3) . . ? C13 P1 H1 111(3) . . ? C19 P2 C25 112.5(3) . . ? C19 P2 C18 107.8(3) . . ? C25 P2 C18 110.2(3) . . ? C19 P2 H2 109(3) . . ? C25 P2 H2 108(3) . . ? C18 P2 H2 110(3) . . ? C6 C1 C2 120.0(6) . . ? C6 C1 P1 119.5(5) . . ? C2 C1 P1 120.5(5) . . ? C3 C2 C1 119.0(7) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C4 C3 C2 120.1(7) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 121.4(7) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120.0(7) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.5(7) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C8 C7 C12 120.0(6) . . ? C8 C7 P1 118.6(5) . . ? C12 C7 P1 121.3(5) . . ? C9 C8 C7 119.6(6) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.1(7) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.8(7) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 119.9(6) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 118.8(6) . . ? C14 C13 P1 117.3(5) . . ? C18 C13 P1 123.8(5) . . ? C13 C14 C15 121.7(6) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 119.6(6) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 121.7(7) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C13 118.6(6) . . ? C17 C18 P2 116.6(5) . . ? C13 C18 P2 124.7(5) . . ? C24 C19 C20 121.5(6) . . ? C24 C19 P2 119.5(5) . . ? C20 C19 P2 118.9(5) . . ? C21 C20 C19 119.2(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 119.8(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 119.5(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 118.8(6) . . ? C19 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C30 C25 C26 120.9(6) . . ? C30 C25 P2 119.5(5) . . ? C26 C25 P2 119.6(5) . . ? C27 C26 C25 118.9(6) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 120.0(7) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 121.1(7) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 119.9(6) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 119.1(6) . . ? C25 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.626 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.138 #===END OF CIF ============================================================== # 10wz520a1.cif data_10wz520a _database_code_depnum_ccdc_archive 'CCDC 783185' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-05-23 _audit_author_name 'Wenjian Zhang' _chemical_name_systematic ; Tetrafluoro(1,2-bis(diethylphosphino)ethane-P,P')titanium(IV) ; # Et2PCH2CH2PEt2 = C10H24P2 # ethane-1,2-diylbis(diethylphosphine) (iLab defaults) # ethane-1,2-diylbis(diethylphosphane) (iLab selected options) # 2-diethylphosphanylethyl-diethyl-phosphane (chemspider) # 1,2-Bis(diethylphosphino)ethane (chemspider alternative) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H24 F4 P2 Ti' _chemical_formula_sum 'C10 H24 F4 P2 Ti' _chemical_formula_weight 330.13 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.0424(10) _cell_length_b 11.7804(15) _cell_length_c 14.6584(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.764(10) _cell_angle_gamma 90.00 _cell_volume 1509.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1801 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8408 # 0.9102 _exptl_absorpt_correction_T_max 1.0000 # 0.9462 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10414 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1732 _reflns_number_gt 1632 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+3.5078P] 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 1732 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.78085(4) 0.2500 0.01872(14) Uani 1 2 d S . . P1 P 0.16339(5) 0.60421(4) 0.32771(3) 0.01620(14) Uani 1 1 d . . . F1 F 0.11570(12) 0.75718(9) 0.15669(8) 0.0241(3) Uani 1 1 d . . . F2 F 0.13800(13) 0.87308(10) 0.32514(9) 0.0299(3) Uani 1 1 d . . . C1 C 0.4534(2) 0.70434(17) 0.38394(15) 0.0254(4) Uani 1 1 d . . . H1A H 0.5601 0.7017 0.3805 0.038 Uiso 1 1 calc R . . H1B H 0.4492 0.6966 0.4498 0.038 Uiso 1 1 calc R . . H1C H 0.4078 0.7770 0.3588 0.038 Uiso 1 1 calc R . . C2 C 0.3643(2) 0.60709(16) 0.32574(13) 0.0210(4) Uani 1 1 d . . . H2A H 0.4125 0.5341 0.3505 0.025 Uiso 1 1 calc R . . H2B H 0.3708 0.6145 0.2596 0.025 Uiso 1 1 calc R . . C3 C 0.2441(3) 0.46695(18) 0.49248(14) 0.0291(4) Uani 1 1 d . . . H3A H 0.2359 0.4586 0.5575 0.044 Uiso 1 1 calc R . . H3B H 0.3522 0.4723 0.4922 0.044 Uiso 1 1 calc R . . H3C H 0.1979 0.4009 0.4554 0.044 Uiso 1 1 calc R . . C4 C 0.1607(2) 0.57438(17) 0.44943(13) 0.0220(4) Uani 1 1 d . . . H4A H 0.2066 0.6398 0.4890 0.026 Uiso 1 1 calc R . . H4B H 0.0528 0.5686 0.4523 0.026 Uiso 1 1 calc R . . C5 C 0.08771(19) 0.47687(15) 0.26071(13) 0.0189(4) Uani 1 1 d . . . H5A H 0.1196 0.4752 0.2010 0.023 Uiso 1 1 calc R . . H5B H 0.1290 0.4084 0.2976 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0174(2) 0.0150(2) 0.0214(2) 0.000 0.00063(17) 0.000 P1 0.0150(2) 0.0163(2) 0.0172(2) -0.00006(16) 0.00389(16) 0.00088(16) F1 0.0185(5) 0.0190(5) 0.0304(6) 0.0046(4) -0.0018(4) -0.0044(4) F2 0.0257(6) 0.0225(6) 0.0354(7) -0.0064(5) -0.0035(5) -0.0030(5) C1 0.0174(9) 0.0221(9) 0.0342(11) 0.0003(8) 0.0021(8) -0.0001(7) C2 0.0155(8) 0.0231(9) 0.0247(9) -0.0009(7) 0.0056(7) 0.0008(7) C3 0.0354(11) 0.0266(10) 0.0235(9) 0.0051(8) 0.0039(8) 0.0043(9) C4 0.0225(9) 0.0253(10) 0.0180(8) 0.0022(7) 0.0050(7) 0.0040(8) C5 0.0192(9) 0.0156(8) 0.0209(8) -0.0015(7) 0.0033(7) 0.0016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F2 1.8028(12) . ? Ti1 F2 1.8028(12) 2 ? Ti1 F1 1.9423(12) . ? Ti1 F1 1.9423(12) 2 ? Ti1 P1 2.6369(6) 2 ? Ti1 P1 2.6369(6) . ? P1 C2 1.8243(18) . ? P1 C4 1.8248(19) . ? P1 C5 1.8277(18) . ? C1 C2 1.529(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.525(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C5 1.536(3) 2 ? C5 H5A 0.9900 . ? C5 H5B 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 F2 Ti1 F2 105.88(8) . 2 ? F2 Ti1 F1 95.95(5) . . ? F2 Ti1 F1 93.98(5) 2 . ? F2 Ti1 F1 93.98(5) . 2 ? F2 Ti1 F1 95.95(5) 2 2 ? F1 Ti1 F1 163.49(7) . 2 ? F2 Ti1 P1 164.56(4) . 2 ? F2 Ti1 P1 89.27(4) 2 2 ? F1 Ti1 P1 85.73(4) . 2 ? F1 Ti1 P1 81.25(4) 2 2 ? F2 Ti1 P1 89.27(4) . . ? F2 Ti1 P1 164.56(4) 2 . ? F1 Ti1 P1 81.25(4) . . ? F1 Ti1 P1 85.73(4) 2 . ? P1 Ti1 P1 75.78(2) 2 . ? C2 P1 C4 106.30(9) . . ? C2 P1 C5 104.17(8) . . ? C4 P1 C5 105.71(9) . . ? C2 P1 Ti1 115.40(6) . . ? C4 P1 Ti1 115.39(6) . . ? C5 P1 Ti1 108.89(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 P1 112.96(13) . . ? C1 C2 H2A 109.0 . . ? P1 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? P1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C3 C4 P1 115.84(14) . . ? C3 C4 H4A 108.3 . . ? P1 C4 H4A 108.3 . . ? C3 C4 H4B 108.3 . . ? P1 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C5 C5 P1 109.61(9) 2 . ? C5 C5 H5A 109.7 2 . ? P1 C5 H5A 109.7 . . ? C5 C5 H5B 109.7 2 . ? P1 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C5 C5 P1 58.8(2) . . 2 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.653 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.068 #===END OF CIF ============================================================== # 10mj040c.cif data_10mj040 _database_code_depnum_ccdc_archive 'CCDC 783186' #TrackingRef '- TiF4_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-06-18 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(2-(pyridin-2-yl)pyridinium) hexafluorotitanate(IV) nitromethane solvate ; # C10H9N2+ = bipyH+ # 2-(pyridin-2-yl)pyridinium (iLab defaults & selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H9 N2 1+)2, F6 Ti 2-, C H3 N O2' _chemical_formula_sum 'C21 H21 F6 N5 O2 Ti' _chemical_formula_weight 537.33 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _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 8.180(6) _cell_length_b 28.488(8) _cell_length_c 10.674(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.12(5) _cell_angle_gamma 90.00 _cell_volume 2320(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3589 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7016 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; During attempts to grow crystals of [TiF4(bipy)] from nitromethane a few crystals were obtained which proved to be the compound reported here. ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_detector_area_resol_mean 15.9745 _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12165 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 29.05 _reflns_number_total 5390 _reflns_number_gt 3483 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The H bonded to one of the N atoms in each 2,2'-bypyridyl residue was convincingly identified as the two largest peaks in a late difference electron-density map. Adding these two H atoms gave two N-H...F H-bonds. The two pronated bipyridyl residues have approximately a planar structure with the torsion N-C-C-N close to zero (rather that 180 deg). Several observations support this: the Uiso for C4/N1, C14/N3; the location of a plausible C-H for C4,C14 and non for the two N atoms; a too close H...H distance (eg N1-H...H-C4) is avoided; and a lower R1 value. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # geom (C-H) difmap (N-H) _refine_ls_hydrogen_treatment 'constr (C-H) refxyz (N-H)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5390 _refine_ls_number_parameters 322 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.67318(4) 0.381210(13) 0.22667(3) 0.03605(11) Uani 1 1 d . . . F1 F 0.55837(17) 0.32667(5) 0.23156(15) 0.0676(4) Uani 1 1 d . . . F2 F 0.60296(17) 0.40771(5) 0.35660(11) 0.0606(4) Uani 1 1 d . . . F3 F 0.47496(15) 0.40506(5) 0.09535(11) 0.0561(3) Uani 1 1 d . . . F4 F 0.74693(16) 0.35776(5) 0.09242(11) 0.0571(3) Uani 1 1 d . . . F5 F 0.87748(14) 0.35752(5) 0.35514(11) 0.0513(3) Uani 1 1 d . . . F6 F 0.78990(16) 0.43688(5) 0.22427(12) 0.0597(3) Uani 1 1 d . . . N1 N 0.8110(3) 0.33120(8) 0.82490(19) 0.0661(6) Uani 1 1 d . . . N2 N 0.6776(2) 0.41117(7) 0.86916(17) 0.0477(4) Uani 1 1 d D . . N3 N 0.2236(3) 0.31554(8) 0.6181(2) 0.0742(6) Uani 1 1 d . . . N4 N 0.0572(2) 0.39692(7) 0.59149(16) 0.0492(5) Uani 1 1 d D . . C1 C 0.8737(4) 0.28967(11) 0.8063(3) 0.0856(10) Uani 1 1 d . . . H1 H 0.9435 0.2732 0.8819 0.103 Uiso 1 1 calc R . . C2 C 0.8420(4) 0.26949(10) 0.6825(3) 0.0797(9) Uani 1 1 d . . . H2 H 0.8906 0.2406 0.6747 0.096 Uiso 1 1 calc R . . C3 C 0.7376(4) 0.29311(10) 0.5722(3) 0.0738(8) Uani 1 1 d . . . H3 H 0.7142 0.2808 0.4868 0.089 Uiso 1 1 calc R . . C4 C 0.6669(3) 0.33538(9) 0.5880(2) 0.0583(6) Uani 1 1 d . . . H4 H 0.5933 0.3518 0.5137 0.070 Uiso 1 1 calc R . . C5 C 0.7064(3) 0.35319(8) 0.7153(2) 0.0446(5) Uani 1 1 d . . . C6 C 0.6419(3) 0.39923(8) 0.73993(19) 0.0411(5) Uani 1 1 d . . . C7 C 0.5531(3) 0.43154(8) 0.6439(2) 0.0519(6) Uani 1 1 d . . . H7 H 0.5226 0.4244 0.5533 0.062 Uiso 1 1 calc R . . C8 C 0.5095(3) 0.47435(9) 0.6815(2) 0.0599(6) Uani 1 1 d . . . H8 H 0.4495 0.4960 0.6160 0.072 Uiso 1 1 calc R . . C9 C 0.5531(3) 0.48558(9) 0.8144(3) 0.0650(7) Uani 1 1 d . . . H9 H 0.5258 0.5148 0.8401 0.078 Uiso 1 1 calc R . . C10 C 0.6376(3) 0.45272(9) 0.9073(2) 0.0588(6) Uani 1 1 d . . . H10 H 0.6675 0.4593 0.9982 0.071 Uiso 1 1 calc R . . C11 C 0.2969(4) 0.27289(13) 0.6307(4) 0.1032(12) Uani 1 1 d . . . H11 H 0.2828 0.2560 0.5530 0.124 Uiso 1 1 calc R . . C12 C 0.3925(4) 0.25268(12) 0.7533(5) 0.1020(12) Uani 1 1 d . . . H12 H 0.4374 0.2224 0.7581 0.122 Uiso 1 1 calc R . . C13 C 0.4187(4) 0.27799(15) 0.8651(4) 0.1021(12) Uani 1 1 d . . . H13 H 0.4872 0.2659 0.9484 0.123 Uiso 1 1 calc R . . C14 C 0.3456(3) 0.32112(11) 0.8568(3) 0.0739(8) Uani 1 1 d . . . H14 H 0.3616 0.3386 0.9339 0.089 Uiso 1 1 calc R . . C15 C 0.2469(3) 0.33859(8) 0.7317(2) 0.0511(5) Uani 1 1 d . . . C16 C 0.1594(2) 0.38402(8) 0.71599(19) 0.0455(5) Uani 1 1 d . . . C17 C 0.1709(3) 0.41538(10) 0.8186(2) 0.0615(7) Uani 1 1 d . . . H17 H 0.2389 0.4081 0.9070 0.074 Uiso 1 1 calc R . . C18 C 0.0806(4) 0.45731(10) 0.7883(3) 0.0701(7) Uani 1 1 d . . . H18 H 0.0877 0.4782 0.8570 0.084 Uiso 1 1 calc R . . C19 C -0.0182(3) 0.46833(10) 0.6599(3) 0.0694(7) Uani 1 1 d . . . H19 H -0.0773 0.4968 0.6396 0.083 Uiso 1 1 calc R . . C20 C -0.0294(3) 0.43738(9) 0.5627(2) 0.0623(6) Uani 1 1 d . . . H20 H -0.0984 0.4443 0.4742 0.075 Uiso 1 1 calc R . . O1 O 0.2175(3) 0.43015(9) 0.3438(3) 0.1095(8) Uani 1 1 d . . . O2 O 0.1099(3) 0.44128(10) 0.1310(3) 0.1132(8) Uani 1 1 d . . . N5 N 0.1649(3) 0.41613(10) 0.2282(3) 0.0792(7) Uani 1 1 d . . . C21 C 0.1684(3) 0.36495(12) 0.2086(3) 0.0881(9) Uani 1 1 d . . . H21A H 0.2803 0.3560 0.2058 0.132 Uiso 1 1 calc R . . H21B H 0.0777 0.3564 0.1256 0.132 Uiso 1 1 calc R . . H21C H 0.1496 0.3491 0.2816 0.132 Uiso 1 1 calc R . . H22 H 0.728(3) 0.3897(7) 0.9279(18) 0.050 Uiso 1 1 d D . . H23 H 0.045(3) 0.3754(6) 0.5363(19) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.03437(18) 0.0397(2) 0.03006(17) -0.00118(16) 0.00672(13) 0.00124(15) F1 0.0581(8) 0.0482(8) 0.0935(10) 0.0033(8) 0.0236(8) -0.0096(6) F2 0.0695(8) 0.0713(10) 0.0464(7) -0.0001(6) 0.0273(6) 0.0159(7) F3 0.0458(7) 0.0622(9) 0.0451(7) -0.0003(6) -0.0020(5) 0.0116(6) F4 0.0676(8) 0.0663(9) 0.0376(6) -0.0010(6) 0.0191(6) 0.0166(7) F5 0.0487(7) 0.0558(8) 0.0379(6) -0.0004(6) 0.0017(5) 0.0108(6) F6 0.0610(8) 0.0487(8) 0.0635(7) 0.0020(6) 0.0154(6) -0.0134(6) N1 0.0780(14) 0.0667(15) 0.0589(12) 0.0172(11) 0.0313(11) 0.0300(12) N2 0.0585(11) 0.0459(12) 0.0401(10) 0.0080(8) 0.0196(9) 0.0058(9) N3 0.0571(12) 0.0657(16) 0.0846(16) -0.0192(13) 0.0071(11) 0.0091(11) N4 0.0529(10) 0.0472(12) 0.0365(9) -0.0055(8) 0.0029(8) -0.0020(9) C1 0.097(2) 0.079(2) 0.091(2) 0.0344(18) 0.0466(18) 0.0416(18) C2 0.100(2) 0.0470(17) 0.119(3) 0.0042(18) 0.072(2) 0.0163(15) C3 0.097(2) 0.0552(18) 0.0826(19) -0.0127(15) 0.0486(17) -0.0015(15) C4 0.0775(16) 0.0470(15) 0.0526(13) -0.0002(11) 0.0262(12) 0.0033(12) C5 0.0495(12) 0.0430(13) 0.0473(12) 0.0091(10) 0.0247(10) 0.0030(9) C6 0.0446(11) 0.0450(12) 0.0374(10) 0.0036(9) 0.0192(9) -0.0011(9) C7 0.0607(14) 0.0539(15) 0.0410(11) 0.0102(11) 0.0183(10) 0.0084(11) C8 0.0707(16) 0.0511(16) 0.0645(15) 0.0197(12) 0.0322(13) 0.0176(12) C9 0.0891(19) 0.0445(15) 0.0760(17) 0.0048(13) 0.0474(16) 0.0082(13) C10 0.0810(17) 0.0516(16) 0.0537(13) -0.0043(12) 0.0361(13) -0.0013(13) C11 0.0650(19) 0.080(2) 0.151(3) -0.043(2) 0.022(2) -0.0007(17) C12 0.0614(18) 0.053(2) 0.188(4) 0.021(2) 0.040(3) 0.0072(15) C13 0.079(2) 0.094(3) 0.135(3) 0.057(3) 0.039(2) 0.018(2) C14 0.0627(16) 0.083(2) 0.0692(17) 0.0281(16) 0.0149(14) 0.0069(14) C15 0.0401(11) 0.0510(15) 0.0552(13) 0.0030(11) 0.0089(10) -0.0082(10) C16 0.0390(11) 0.0527(14) 0.0382(10) 0.0006(10) 0.0058(9) -0.0095(10) C17 0.0614(15) 0.078(2) 0.0358(11) -0.0090(12) 0.0059(11) -0.0125(13) C18 0.0746(17) 0.0638(19) 0.0721(17) -0.0292(15) 0.0268(15) -0.0142(14) C19 0.0614(15) 0.0519(16) 0.0853(19) -0.0097(15) 0.0149(15) -0.0017(12) C20 0.0602(15) 0.0495(15) 0.0587(14) 0.0016(12) -0.0011(12) -0.0001(11) O1 0.0750(14) 0.118(2) 0.1246(19) -0.0393(17) 0.0233(14) 0.0070(13) O2 0.1048(18) 0.111(2) 0.143(2) 0.0305(18) 0.0682(17) 0.0232(15) N5 0.0504(13) 0.085(2) 0.111(2) -0.0057(19) 0.0387(15) 0.0056(13) C21 0.0652(17) 0.083(2) 0.127(3) -0.019(2) 0.0483(18) -0.0049(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 F1 1.8259(14) . ? Ti1 F2 1.8431(14) . ? Ti1 F3 1.8487(17) . ? Ti1 F6 1.8561(14) . ? Ti1 F5 1.8647(17) . ? Ti1 F4 1.8672(14) . ? N1 C5 1.331(3) . ? N1 C1 1.333(3) . ? N2 C10 1.331(3) . ? N2 C6 1.347(3) . ? N2 H22 0.866(15) . ? N3 C15 1.331(3) . ? N3 C11 1.340(4) . ? N4 C20 1.330(3) . ? N4 C16 1.341(3) . ? N4 H23 0.831(15) . ? C1 C2 1.377(4) . ? C1 H1 0.9300 . ? C2 C3 1.358(4) . ? C2 H2 0.9300 . ? C3 C4 1.372(4) . ? C3 H3 0.9300 . ? C4 C5 1.375(3) . ? C4 H4 0.9300 . ? C5 C6 1.473(3) . ? C6 C7 1.375(3) . ? C7 C8 1.371(3) . ? C7 H7 0.9300 . ? C8 C9 1.369(3) . ? C8 H8 0.9300 . ? C9 C10 1.358(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.385(5) . ? C11 H11 0.9300 . ? C12 C13 1.343(5) . ? C12 H12 0.9300 . ? C13 C14 1.355(4) . ? C13 H13 0.9300 . ? C14 C15 1.380(3) . ? C14 H14 0.9300 . ? C15 C16 1.459(3) . ? C16 C17 1.390(3) . ? C17 C18 1.380(4) . ? C17 H17 0.9300 . ? C18 C19 1.353(4) . ? C18 H18 0.9300 . ? C19 C20 1.339(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O1 N5 1.218(3) . ? O2 N5 1.207(3) . ? N5 C21 1.475(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 F1 Ti1 F2 91.39(7) . . ? F1 Ti1 F3 90.85(7) . . ? F2 Ti1 F3 89.66(7) . . ? F1 Ti1 F6 179.13(6) . . ? F2 Ti1 F6 87.80(7) . . ? F3 Ti1 F6 89.45(7) . . ? F1 Ti1 F5 90.28(7) . . ? F2 Ti1 F5 91.98(7) . . ? F3 Ti1 F5 177.99(6) . . ? F6 Ti1 F5 89.44(7) . . ? F1 Ti1 F4 91.67(7) . . ? F2 Ti1 F4 176.77(6) . . ? F3 Ti1 F4 89.27(7) . . ? F6 Ti1 F4 89.14(7) . . ? F5 Ti1 F4 89.03(7) . . ? C5 N1 C1 116.5(2) . . ? C10 N2 C6 123.5(2) . . ? C10 N2 H22 120.7(14) . . ? C6 N2 H22 115.8(14) . . ? C15 N3 C11 116.4(3) . . ? C20 N4 C16 123.8(2) . . ? C20 N4 H23 124.0(15) . . ? C16 N4 H23 111.9(15) . . ? N1 C1 C2 124.3(3) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 117.8(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.9(2) . . ? N1 C5 C6 114.86(19) . . ? C4 C5 C6 122.2(2) . . ? N2 C6 C7 117.2(2) . . ? N2 C6 C5 116.63(19) . . ? C7 C6 C5 126.18(19) . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.9(2) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 118.0(2) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N2 C10 C9 120.4(2) . . ? N2 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? N3 C11 C12 123.5(3) . . ? N3 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C13 C12 C11 118.1(3) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C15 C14 123.0(2) . . ? N3 C15 C16 115.4(2) . . ? C14 C15 C16 121.5(2) . . ? N4 C16 C17 116.5(2) . . ? N4 C16 C15 117.49(19) . . ? C17 C16 C15 126.1(2) . . ? C18 C17 C16 119.6(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 120.8(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N4 C20 C19 120.6(2) . . ? N4 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? O2 N5 O1 124.2(3) . . ? O2 N5 C21 119.0(3) . . ? O1 N5 C21 116.8(3) . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C5 C6 N2 -7.7(3) . . . . ? N3 C15 C16 N4 3.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H22 F4 0.866(15) 1.933(17) 2.710(2) 148.5(19) 1_556 N4 H23 F5 0.831(15) 1.993(18) 2.667(3) 138(2) 1_455 _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.360 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.047 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================