Room Temperature Reduction of CO2 to Methanol by Al-Based Frustrated Lewis Pairs and Ammonia Borane
Gabriel Ménard; Douglas W. Stephan; Journal of the American Chemical Society 132 (2010) 1796–1797; doi:10.1021/ja9104792

data_4101894
_publ_section_title
;
 Room Temperature Reduction of CO2 to Methanol by Al-Based Frustrated
 Lewis Pairs and Ammonia Borane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1796
_journal_page_last               1797
_journal_paper_doi               10.1021/ja9104792
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C30 H36 Al Br0.5 Cl3 P'
_chemical_formula_weight         600.84
_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                89.470(3)
_cell_angle_beta                 88.254(3)
_cell_angle_gamma                80.848(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3628(5)
_cell_length_b                   11.1182(5)
_cell_length_c                   13.0439(6)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1483.03(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26346
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+1.4480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                5206
_reflns_number_total             7205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9104792_si_001_1.cif
_cod_data_source_block           Mes3P(AlCl3)(0.5C6H5Br)
_cod_original_formula_sum        'C30 H36 Al Br0.50 Cl3 P'
_cod_database_code               4101894