Direct synthesis of a geminal zwitterionic phosphonium/hydridoborate system - developing an alternative tool for generating frustrated Lewis pair hydrogen activation systems.
Yu, Jiangang; Kehr, Gerald; Daniliuc, Constantin G.; Bannwarth, Christoph; Grimme, Stefan; Erker, Gerhard; Organic & biomolecular chemistry 13 (2015) 5783–5792; doi:10.1039/c5ob00634a

data_7154483
_publ_section_title
;
 Direct synthesis of a geminal zwitterionic phosphonium/hydridoborate
 system - developing an alternative tool for generating frustrated Lewis
 pair hydrogen activation systems.
;
_journal_issue                   20
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5783
_journal_page_last               5792
_journal_paper_doi               10.1039/c5ob00634a
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C40 H34 B Cl2 F10 P'
_chemical_formula_weight         817.35
_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
;
2015-03-20 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.2660(10)
_cell_angle_beta                 108.6870(10)
_cell_angle_gamma                103.1290(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2185(2)
_cell_length_b                   11.8258(2)
_cell_length_c                   15.1455(3)
_cell_measurement_reflns_used    4994
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     1847.10(6)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.050
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18017
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.9425
_exptl_absorpt_correction_T_min  0.9023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0524P)^2^+1.2715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                7139
_reflns_number_total             8925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob00634a2.cif
_cod_data_source_block           erk7652
_cod_depositor_comments
'Adding full bibliography for 7154478--7154486.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7154483