Stoichiometric Reduction of CO2to CO by Phosphine/AlX3-Based Frustrated Lewis Pairs
Ménard, Gabriel; Gilbert, Thomas M.; Hatnean, Jillian A.; Kraft, Anne; Krossing, Ingo; Stephan, Douglas W.; Organometallics 32 (2013) 4416–; doi:10.1021/om400619y

data_4081190
_publ_section_title
;
 Stoichiometric Reduction of CO2to CO by Phosphine/AlX3-Based Frustrated
 Lewis Pairs
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4416
_journal_paper_doi               10.1021/om400619y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C22 H21 Al2 I6 O2 P'
_chemical_formula_weight         1163.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9541(7)
_cell_length_b                   18.4541(13)
_cell_length_c                   16.5285(11)
_cell_measurement_temperature    150(2)
_cell_volume                     3336.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53121
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    5.705
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.239
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0307P)^2^+13.0678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                6665
_reflns_number_total             7633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400619y_si_003.cif
_cod_data_source_block           gm037_0m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C3.67 H3.50 Al0.33 I O0.33 P0.17'
_cod_database_code               4081190