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_1546173
_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         'C30 H58 Al Si3 Ti'
_chemical_formula_sum            'C30 H58 Al Si3 Ti'
_chemical_formula_weight         577.91
_chemical_name_common            acb_1_088
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 115.3660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5367(5)
_cell_length_b                   11.3812(3)
_cell_length_c                   18.6758(5)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.16
_cell_volume                     3368.11(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44586
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         1.285
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       plates
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.6797
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+3.4533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5397
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01835e2.cif
_cod_data_source_block           shelx
_cod_database_code               1546173
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              87611