A Tris(triphenylphosphine)aluminum Ambiphilic Precatalyst for the Reduction of Carbon Dioxide with Catecholborane
Courtemanche, Marc-André; Larouche, Jérémie; Légaré, Marc-André; Bi, Wenhua; Maron, Laurent; Fontaine, Frédéric-Georges; Organometallics 32 (2013) 6804–; doi:10.1021/om400645s

data_4089594
_publ_section_title
;
 A Tris(triphenylphosphine)aluminum Ambiphilic Precatalyst for the
 Reduction of Carbon Dioxide with Catecholborane
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6804
_journal_paper_doi               10.1021/om400645s
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C54 H42 Al P3'
_chemical_formula_sum            'C54 H42 Al P3'
_chemical_formula_weight         810.77
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                87.5550(10)
_cell_angle_beta                 82.8900(10)
_cell_angle_gamma                77.3160(10)
_cell_formula_units_Z            4
_cell_length_a                   11.0020(2)
_cell_length_b                   13.1765(2)
_cell_length_c                   31.9414(6)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.4
_cell_volume                     4482.16(14)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT+ (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2007)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18131
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The heavily disordered guest molecule of Toluene was squeezed out of the 
crystal srtucture in order to improve the structural model.
;
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         18131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0692P)^2^+0.5661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                12258
_reflns_number_total             18131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400645s_si_002.cif
_cod_data_source_block           I
_cod_database_code               4089594