Implications of CO2Activation by Frustrated Lewis Pairs in the Catalytic Hydroboration of CO2: A View Using N/Si+Frustrated Lewis Pairs
von Wolff, N.; Lefèvre, G.; Berthet, J.-C.; Thuéry, P.; Cantat, T.; ACS Catalysis  (2016) 4526–; doi:10.1021/acscatal.6b00421

data_4513891
_publ_section_title
;
 Implications of CO2Activation by Frustrated Lewis Pairs in the Catalytic
 Hydroboration of CO2: A View Using N/Si+Frustrated Lewis Pairs
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              4526
_journal_paper_doi               10.1021/acscatal.6b00421
_journal_year                    2016
_chemical_formula_sum            'C22 H36 F12 N8 O8 S4 Si2'
_chemical_formula_weight         953.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0441(10)
_cell_length_b                   17.1344(5)
_cell_length_c                   26.8405(15)
_cell_measurement_reflns_used    203924
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.27
_cell_volume                     7838.5(7)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two \f and six \w scans with 2\% steps (459 frames)'
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            203924
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.268
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
N: Total Potential Solvent Accessible Void Vol ..................  2350.3 Ang^3
N: Electron Count / Cell =   1140 - To be included in D(calc), F000 & Mol.Wght.

The added electron count is 143 per asymmetric unit, which matches
the electron count of 138 for the bis-triflimide anion. This anion was
thus added in the formula sum. 
;
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7424
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1433P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4918
_reflns_number_total             7424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b00421_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        7838.5(5)
_cod_database_code               4513891
_shelxl_version_number           2014-3
_shelx_res_checksum              61036
_shelx_hkl_checksum              92943