Reactivity of the geminal phosphinoborane tBu <sub>2</sub> PCH <sub>2</sub> BPh <sub>2</sub> towards alkynes, nitriles, and nitrilium triflates
Habraken, Evi R. M.; Mens, Lars C.; Nieger, Martin; Lutz, Martin; Ehlers, Andreas W.; Slootweg, J. Chris; Dalton Transactions 46 (2017) 12284–12292; doi:10.1039/C7DT02570J

data_1546902
_publ_section_title
;
 Reactivity of the geminal phosphinoborane tBu <sub>2</sub> PCH
 <sub>2</sub> BPh <sub>2</sub> towards alkynes, nitriles, and nitrilium
 triflates
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              12284
_journal_page_last               12292
_journal_paper_doi               10.1039/C7DT02570J
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H40 B N P, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C36 H42 B Cl2 F3 N O3 P S'
_chemical_formula_weight         738.44
_chemical_name_systematic
'4,4-di-tert-butyl-1,2,2,5-tetraphenyl-3,4-dihydro-2H-1\l^4^,4,2\l^4^-azaphosphaborol-4-ium trifluoromethanesulfonate dichloromethane solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0882(5)
_cell_length_b                   17.6065(7)
_cell_length_c                   18.5479(9)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     3621.0(3)
_computing_cell_refinement       APEX3
_computing_data_collection       APEX3
_computing_data_reduction        SAINT
_computing_molecular_graphics    shelxtl
_computing_publication_material  publCIF
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE with Photon100 detector'
_diffrn_measurement_method       'rotation in \f and \w, 1\%, shutterless'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            157311
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'INCOATEC microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 3342 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0590P)^2^+5.4513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7827
_reflns_number_total             8349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02570j2.cif
_cod_data_source_block           jcs074_compound_7a
_cod_database_code               1546902
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              70483