# 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