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_4101896
_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            'C28 H33 Al2 Cl6 O2 P'
_chemical_formula_weight         699.17
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5382(10)
_cell_length_b                   20.0664(15)
_cell_length_c                   31.987(3)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     6764.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1449
_diffrn_reflns_av_sigmaI/netI    0.1446
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            32202
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6019
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.2184
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+25.7929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2189
_refine_ls_wR_factor_ref         0.2715
_reflns_number_gt                3481
_reflns_number_total             7807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9104792_si_001_3.cif
_cod_data_source_block           Mes3P(CO2)(AlCl3)2
_cod_original_cell_volume        6764.2(10)
_cod_database_code               4101896