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_4101898
_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            'C27 H35 Al Br4 P'
_chemical_formula_weight         737.14
_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                102.707(3)
_cell_angle_beta                 93.952(3)
_cell_angle_gamma                102.129(3)
_cell_formula_units_Z            4
_cell_length_a                   13.5700(7)
_cell_length_b                   15.0537(8)
_cell_length_c                   15.6353(8)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3023.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            151500
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    5.420
_exptl_absorpt_correction_T_max  0.4776
_exptl_absorpt_correction_T_min  0.1394
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         13744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+9.4781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                10456
_reflns_number_total             13744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9104792_si_002.cif
_cod_data_source_block           '[Mes3PH][AlBr4]'
_cod_database_code               4101898