# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2044 data_global _publ_contact_autor ; Guido Pampaloni Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone '050 918218' _publ_contact_author_fax '050 20237' _publ_contact_author_email 'Pampa@dcci.unipi.it' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #==================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reactivity of SeOCl2 with Titanium and Zirconium Tetrachlorides. The Unexpected Formation of a \m-Oxo-Bridged Titanium(IV) Derivative ; loop_ _publ_author_name _publ_author_address 'Calderazzo, Fausto' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'DAttoma, Michele' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali e delle Materie Prime e Metallurgia Universita'' "La Sapienza" di Roma Via del Castro Laurenziano, 7 I-00185 Roma Italy ; 'Pampaloni, Guido' ; Dipartimento di Chimica e Chimica Industriale Universita'' di Pisa Via Risorgimento, 35 I-56126 Pisa Italy ; #==================================================================== data_tic _audit_creation_method SHELXL-97 _chemical_name_systematic ; Oxobis[trichlorobis(seleninylchloride)titanium(IV)] dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '\m-O(TiCl3(OSeCl2)2)2.CH2Cl2' _chemical_formula_sum 'C H2 Cl16 O5 Se4 Ti2' _chemical_formula_weight 1072.87 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.7530(10) _cell_length_b 8.4950(5) _cell_length_c 13.3500(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.58(2) _cell_angle_gamma 90.00 _cell_volume 1439.44(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.77 _cell_measurement_theta_max 12.96 _exptl_crystal_description 'Prismatic stick' _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max '0.67_mm' _exptl_crystal_size_mid '0.17_mm' _exptl_crystal_size_min '0.08_mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 7.112 _exptl_absorpt_correction_type 'Integration' _exptl_absorpt_correction_T_min 0.3036 _exptl_absorpt_correction_T_max 0.5871 _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 1.00 0.3400 -1.00 0.00 0.00 0.2350 0.00 1.00 0.00 0.0900 0.00 -1.00 0.00 0.0900 -1.00 0.00 1.00 0.0400 1.00 0.00 -1.00 0.0400 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 3327 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2538 _reflns_number_gt 1862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+2.6867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2538 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.61190(9) 0.00618(13) 0.22570(8) 0.0328(3) Uani 1 1 d . . . O1 O 0.7500 0.0430(7) 0.2500 0.0363(14) Uani 1 2 d S . . Cl1 Cl 0.63858(12) -0.11352(19) 0.06475(11) 0.0395(4) Uani 1 1 d . . . Cl2 Cl 0.56895(15) 0.24227(19) 0.15682(14) 0.0511(5) Uani 1 1 d . . . Cl3 Cl 0.56472(16) 0.0623(2) 0.38203(13) 0.0576(5) Uani 1 1 d . . . Se1 Se 0.63877(5) -0.27511(9) 0.39471(5) 0.0433(2) Uani 1 1 d . . . O2 O 0.6361(3) -0.2232(5) 0.2762(3) 0.0385(10) Uani 1 1 d . . . Cl4 Cl 0.71266(19) -0.5004(2) 0.38844(17) 0.0738(6) Uani 1 1 d . . . Cl5 Cl 0.48054(17) -0.3568(3) 0.40350(18) 0.0847(8) Uani 1 1 d . . . Se2 Se 0.41456(5) -0.17008(8) 0.08616(5) 0.04125(19) Uani 1 1 d . . . O3 O 0.4564(3) -0.0750(5) 0.1901(3) 0.0408(11) Uani 1 1 d . . . Cl6 Cl 0.4486(2) -0.4132(2) 0.12178(18) 0.0798(7) Uani 1 1 d . . . Cl7 Cl 0.24923(15) -0.1761(3) 0.10469(18) 0.0782(7) Uani 1 1 d . . . C C 0.2500 0.228(3) 0.2500 0.242(16) Uani 1 2 d S . . H1A H 0.1939 0.1592 0.2678 0.291 Uiso 0.50 1 calc PR . . H1B H 0.3061 0.1592 0.2322 0.291 Uiso 0.50 1 calc PR . . Cl8 Cl 0.2070(4) 0.3116(6) 0.1512(3) 0.197(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0320(6) 0.0333(6) 0.0321(6) 0.0032(5) -0.0022(5) 0.0025(5) O1 0.037(3) 0.036(3) 0.035(3) 0.000 -0.002(3) 0.000 Cl1 0.0405(9) 0.0448(9) 0.0325(8) -0.0012(7) 0.0002(7) 0.0037(7) Cl2 0.0616(11) 0.0331(9) 0.0558(11) 0.0053(8) -0.0079(9) 0.0088(8) Cl3 0.0658(13) 0.0670(12) 0.0407(10) -0.0079(9) 0.0083(9) 0.0114(10) Se1 0.0406(4) 0.0518(4) 0.0368(4) 0.0140(3) 0.0009(3) 0.0042(3) O2 0.045(3) 0.038(2) 0.032(2) 0.0106(19) -0.0001(19) 0.002(2) Cl4 0.0846(16) 0.0550(12) 0.0802(15) 0.0230(11) 0.0008(12) 0.0231(12) Cl5 0.0475(12) 0.114(2) 0.0949(17) 0.0435(15) 0.0181(11) -0.0059(13) Se2 0.0419(4) 0.0398(4) 0.0400(4) 0.0050(3) -0.0066(3) -0.0041(3) O3 0.034(2) 0.047(3) 0.040(2) -0.003(2) -0.0008(19) -0.003(2) Cl6 0.110(2) 0.0379(10) 0.0876(16) 0.0081(11) -0.0106(14) -0.0033(12) Cl7 0.0395(11) 0.1080(19) 0.0848(15) 0.0050(14) -0.0054(10) -0.0218(12) C 0.44(5) 0.119(19) 0.16(2) 0.000 0.01(3) 0.000 Cl8 0.269(6) 0.226(5) 0.084(2) -0.001(3) -0.051(3) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O1 1.7872(15) . ? Ti O2 2.075(4) . ? Ti O3 2.110(4) . ? Ti Cl2 2.2517(19) . ? Ti Cl3 2.278(2) . ? Ti Cl1 2.4308(19) . ? O1 Ti 1.7872(15) 2_655 ? Se1 O2 1.639(4) . ? Se1 Cl4 2.139(2) . ? Se1 Cl5 2.148(2) . ? Se2 O3 1.649(4) . ? Se2 Cl7 2.147(2) . ? Se2 Cl6 2.154(2) . ? C Cl8 1.551(11) 2 ? C Cl8 1.551(11) . ? 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 O1 Ti O2 89.6(2) . . ? O1 Ti O3 170.5(2) . . ? O2 Ti O3 82.70(17) . . ? O1 Ti Cl2 96.57(18) . . ? O2 Ti Cl2 172.58(13) . . ? O3 Ti Cl2 90.76(13) . . ? O1 Ti Cl3 98.08(8) . . ? O2 Ti Cl3 86.74(13) . . ? O3 Ti Cl3 87.03(14) . . ? Cl2 Ti Cl3 96.45(8) . . ? O1 Ti Cl1 90.77(10) . . ? O2 Ti Cl1 82.25(12) . . ? O3 Ti Cl1 82.75(13) . . ? Cl2 Ti Cl1 93.50(7) . . ? Cl3 Ti Cl1 165.82(9) . . ? Ti O1 Ti 159.8(4) . 2_655 ? O2 Se1 Cl4 99.83(16) . . ? O2 Se1 Cl5 102.01(17) . . ? Cl4 Se1 Cl5 97.64(10) . . ? Se1 O2 Ti 123.7(2) . . ? O3 Se2 Cl7 98.95(17) . . ? O3 Se2 Cl6 104.01(17) . . ? Cl7 Se2 Cl6 97.51(10) . . ? Se2 O3 Ti 124.7(2) . . ? Cl8 C Cl8 125.3(15) 2 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.658 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.117 #===END