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_4323082
_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            'C54 H94 O4 Ti4'
_chemical_formula_weight         998.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.985(5)
_cell_length_b                   22.254(5)
_cell_length_c                   23.307(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     10927(5)
_computing_cell_refinement       'Siemens SMART (V. 4.050, Siemens 1996)'
_computing_data_collection       'Siemens SMART (V. 4.050, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 4.050, Siemens 1996)'
_computing_molecular_graphics    'Siemens SHELXTL (V. 5.05)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe-Siemens-Huber four circle diffrctmtr'
_diffrn_measurement_method       'phi and 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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19258
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.7133
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         19258
_refine_ls_number_restraints     746
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+17.5143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                16669
_reflns_number_total             19258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980450g_5.cif
_cod_data_source_block           4
_cod_original_cell_volume        10927(4)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4323082