Base induced isomerisation of a phosphaethynolato-borane: mechanistic insights into boryl migration and decarbonylation to afford a triplet phosphinidene
Wilson, Daniel W. N.; Franco, Mauricio P.; Myers, William K.; McGrady, John E.; Goicoechea, Jose M.; Chemical Science 11 (2020) 862–869; doi:10.1039/C9SC05969E

data_1556411
_publ_section_title
;
 Base induced isomerisation of a phosphaethynolato-borane: mechanistic
 insights into boryl migration and decarbonylation to afford a triplet
 phosphinidene
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              862
_journal_page_last               869
_journal_paper_doi               10.1039/C9SC05969E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C31 H45 B N3 P'
_chemical_formula_sum            'C31 H45 B N3 P'
_chemical_formula_weight         501.48
_chemical_name_systematic
;
 [{(tBu)NC}P]B[{N(2,6-iPr-C6H3)}2(CH)2]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-11-01 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5060(10)
_cell_angle_gamma                90
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_cell_length_c                   33.0859(4)
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.5550
_cell_measurement_theta_min      2.6860
_cell_volume                     6229.38(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25322
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.494
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         2.688
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+3.3990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8985
_reflns_number_total             10979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05969e2.cif
_cod_data_source_block           DW371
_cod_depositor_comments
;Adding full bibliography for 1556409--1556415.cif.

 Adding full bibliography for 1556409--1556415.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1556411
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              32390