Hydroboration route to geminal P/B frustrated Lewis pairs with a bulky secondary phosphane component and their reaction with carbon dioxide
Erker, Gerhard; Jian, Zhongbao; Kehr, Gerald; Daniliuc, Constantin Gabriel; Wibbeling, Birgit; Dalton Trans.  (2017) –; doi:10.1039/C7DT02315D

data_7043905
_publ_section_title
;
 Hydroboration route to geminal P/B frustrated Lewis pairs with a bulky
 secondary phosphane component and their reaction with carbon dioxide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02315D
_journal_year                    2017
_chemical_formula_sum            'C33 H27 B F10 N O P S'
_chemical_formula_weight         717.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-07-18 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5186(4)
_cell_length_b                   11.2948(3)
_cell_length_c                   17.6854(5)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      67.6981
_cell_measurement_theta_min      4.6769
_cell_volume                     3224.71(15)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55525
_diffrn_reflns_theta_full        68.19
_diffrn_reflns_theta_max         68.19
_diffrn_reflns_theta_min         4.68
_diffrn_source                   'fine--focus sealed tube'
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.77
_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    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.622
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0746
_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^)+19.7334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                5030
_reflns_number_total             5799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02315d2.cif
_cod_data_source_block           13b
_cod_database_code               7043905
_shelx_res_checksum              51268