Reactions of Organotitanoxane Fluorides with AlR3 (R = Me, Et, CH2Ph) and Me3SiCl: X-ray Crystal Structures of [C5Me5Ti(μ-O)]4F[(μ-F)AlMe3]3, [C5Me5Ti(μ-O)]4F3[(μ-F)Al(CH2Ph)3], [C5Me5Ti(μ-O)Et]4, and (C5Me5)4Ti4O5X2 (X = Cl and F)
Peihua Yu; Thomas Pape; Isabel Usón; Musa A. Said; Herbert W. Roesky; Mavis L. Montero; Hans-Georg Schmidt; Alojz Demsar; Inorganic Chemistry 37 (1998) 5117–5124; doi:10.1021/ic980450g

data_4323079
_publ_contact_author
;
       Herbert W. Roesky
       Institut f\"ur Anorganische Chemie
       Universit\"at G\"ottingen
       Tammannstr. 4
       37077 G\"ottingen
       Germany
;
_publ_contact_author_fax         '49 551 39 3373'
_publ_contact_author_phone       '49 551 39 3001'
_publ_section_title
;
 Reactions of Organotitanoxane Fluorides with AlR3 (R = Me, Et, CH2Ph) and
 Me3SiCl: X-ray Crystal Structures of [C5Me5Ti(\m-O)]4F[(\m-F)AlMe3]3,
 [C5Me5Ti(\m-O)]4F3[(\m-F)Al(CH2Ph)3], [C5Me5Ti(\m-O)Et]4, and
 (C5Me5)4Ti4O5X2 (X = Cl and F)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5117
_journal_page_last               5124
_journal_paper_doi               10.1021/ic980450g
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C40 H60 F2 O5 Ti4'
_chemical_formula_weight         850.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                86.04(3)
_cell_angle_beta                 86.68(1)
_cell_angle_gamma                68.11(1)
_cell_formula_units_Z            2
_cell_length_a                   10.872(2)
_cell_length_b                   11.892(3)
_cell_length_c                   17.678(4)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2114.5(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens/STOE AED2'
_diffrn_measurement_method       '2theta/omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10367
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        <3%
_diffrn_standards_interval_count 180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.6127
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.90
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+2.7541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                5384
_reflns_number_total             5384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980450g_2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+2.7541P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+2.7541P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2114.7(8)
_cod_database_code               4323079