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_7119971
_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 H46 B2 Cl4 F20 N O P'
_chemical_formula_weight         1311.32
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.022(1)
_cell_angle_beta                 80.922(1)
_cell_angle_gamma                72.511(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9911(2)
_cell_length_b                   12.2241(2)
_cell_length_c                   20.5637(4)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2836.41(9)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25959
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         9787
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0149P)^2^+6.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                7809
_reflns_number_total             9787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc02214j2.cif
_cod_data_source_block           erk8309
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7119971