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_1546906
_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_formula_moiety         'C26 H39 B N P'
_chemical_formula_sum            'C26 H39 B N P'
_chemical_formula_weight         407.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-21 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.698(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4364(4)
_cell_length_b                   14.5007(5)
_cell_length_c                   14.8879(6)
_cell_measurement_reflns_used    59068
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35.05
_cell_measurement_theta_min      2.22
_cell_volume                     2463.81(16)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71268
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.008
_diffrn_reflns_theta_min         2.271
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 4312 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         10849
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0743P)^2^+0.5075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9694
_reflns_number_total             10849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02570j2.cif
_cod_data_source_block           l0825b
_cod_original_cell_volume        2463.80(16)
_cod_database_code               1546906
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              64814