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_7012319
_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         'C40 H80 Cl8 O24 Ti, 4(C7 H8), 2(H2 O)'
_chemical_formula_sum            'C68 H116 Cl8 O26 Ti4'
_chemical_formula_weight         1824.81
_chemical_name_systematic
; 
cyclo-tetrakis((mu-oxo)-dichloro-(1,4,7,10,13-pentaoxacyclopentadecane)-
titanium(IV)) toluene solvate hydrate
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.353(3)
_cell_length_b                   20.353(3)
_cell_length_c                   10.739(2)
_cell_measurement_reflns_used    26637
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4448.6(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.1785
_diffrn_reflns_av_sigmaI/netI    0.1917
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16577
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.8295
_exptl_absorpt_correction_T_min  0.8134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1935
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.2180
_reflns_number_gt                1722
_reflns_number_total             3883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210012f.txt
_cod_data_source_block           ticl15
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7012319