Cooperative Carbon Monoxide to Formyl Reduction at a Trifunctional PBB Frustrated Lewis Pair
Kehr, Gerald; Wang, Long; Daniliuc, Constantin Gabriel; Erker, Gerhard; Zhang, Senwang; Hasegawa, Yasuharu; Chem. Commun.  (2017) –; doi:10.1039/C7CC02214J

data_7119970
_publ_section_title
;
 Cooperative Carbon Monoxide to Formyl Reduction at a Trifunctional PBB
 Frustrated Lewis Pair
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02214J
_journal_year                    2017
_chemical_formula_sum            'C55 H48 B2 F20 N P'
_chemical_formula_weight         1155.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                78.257(2)
_cell_angle_beta                 81.650(2)
_cell_angle_gamma                71.145(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5829(4)
_cell_length_b                   13.9854(5)
_cell_length_c                   17.6337(6)
_cell_measurement_reflns_used    8569
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.9766
_cell_measurement_theta_min      3.3871
_cell_volume                     2864.56(17)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v.2014.1--1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'APEX2 v.2014.1--1 (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 v.2014.1--1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL--2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'KappaCCD APEXII'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51604
_diffrn_reflns_theta_full        68.33
_diffrn_reflns_theta_max         68.33
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
One and a half badly disordered dichloromethane molecules were found in 
the asymmetrical unit and could not be satisfactorily refined. 
The program SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) was 
therefore used to remove mathematically the effect of the solvent. 
The quoted formula and derived parameters are not included the squeezed
solvent molecules. 
;
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         10235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0637P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                6726
_reflns_number_total             10235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02214j2.cif
_cod_data_source_block           erk8322
_cod_database_code               7119970
_shelx_res_checksum              28077