Crown ether complexes of titanium(iv) chloride and bromide and the structures of the hydrolysis products [Ti2Cl6(µ-O)(18-crown-6)2] and [Ti4Cl8(µ-O)4(15-crown-5)4]
Levason, William; Popham, Michael C.; Reid, Gillian; Webster, Michael; Dalton Transactions  (2003) 291–; doi:10.1039/b210012f

data_7012318
_publ_section_title
;
 Crown ether complexes of titanium(iv) chloride and bromide and the
 structures of the hydrolysis products
 [Ti2Cl6(&#x00B5;-O)(18-crown-6)2] and
 [Ti4Cl8(&#x00B5;-O)4(15-crown-5)4]
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              291
_journal_paper_doi               10.1039/b210012f
_journal_year                    2003
_chemical_formula_moiety         'C24 H48 Cl6 O13 Ti2, 0.5(C7 H8)'
_chemical_formula_sum            'C27.5 H52 Cl6 O13 Ti2'
_chemical_formula_weight         899.19
_chemical_name_systematic
; 
mu-oxo-bis(trichloro(1,4,7,10,13,16-hexaoxacyclooctadecane)titanium(IV))
toluene solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                84.669(3)
_cell_angle_beta                 81.909(3)
_cell_angle_gamma                79.892(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2483(5)
_cell_length_b                   13.8350(10)
_cell_length_c                   14.7207(10)
_cell_measurement_reflns_used    8816
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     2029.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38655
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.8515
_exptl_absorpt_correction_T_min  0.8048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.5908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                8071
_reflns_number_total             9239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210012f.txt
_cod_data_source_block           d059
_cod_original_formula_sum        'C27.50 H52 Cl6 O13 Ti2'
_cod_database_code               7012318