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_1556409
_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         'C37 H47 B N3 O P'
_chemical_formula_sum            'C37 H47 B N3 O P'
_chemical_formula_weight         591.55
_chemical_name_systematic
;
 [{(Mes)N}(OCP)C]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                 101.118(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6925(3)
_cell_length_b                   19.6374(5)
_cell_length_c                   17.0321(5)
_cell_measurement_reflns_used    26014
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.8450
_cell_measurement_theta_min      4.4660
_cell_volume                     3509.16(17)
_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 0.985
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.487
_diffrn_reflns_theta_min         4.503
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92587
_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            yellow
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0826P)^2^+1.6499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6142
_reflns_number_total             7355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05969e2.cif
_cod_data_source_block           DW343
_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               1556409
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.757
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              63394