Hydride oxidation from a titanium–aluminum bimetallic complex: insertion, thermal and electrochemical reactivity
Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D.; Hohloch, Stephan; Arnold, John; Chem. Sci.  (2017) –; doi:10.1039/C7SC01835E

data_1546176
_publ_section_title
;
 Hydride oxidation from a titanium--aluminum bimetallic complex:
 insertion, thermal and electrochemical reactivity
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01835E
_journal_year                    2017
_chemical_formula_moiety         'C21 H39 Al F3 O3 S Si3 Ti'
_chemical_formula_sum            'C21 H39 Al F3 O3 S Si3 Ti'
_chemical_formula_weight         587.73
_chemical_name_common            (Cp)2Ti(u-H)(u-OTf)Al(H)C(TMS)3
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-31 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.756(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9334(5)
_cell_length_b                   8.8807(2)
_cell_length_c                   41.2358(12)
_cell_measurement_reflns_used    9488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.50
_cell_volume                     5828.1(3)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            127278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.361
_diffrn_reflns_theta_min         1.349
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             2472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.7024
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+8.3207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7979
_reflns_number_total             10668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01835e2.cif
_cod_data_source_block           shelx
_cod_database_code               1546176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              22216