Reactivity of the phosphaethynolate anion with stabilized carbocations: mechanistic studies and synthetic applications.
Nguyen, Thi Hong Van; Chelli, Saloua; Mallet-Ladeira, Sonia; Breugst, Martin; Lakhdar, Sami; Chemical science 15 (2024) 14406–14414; doi:10.1039/d4sc03518f

data_1572779
_publ_section_title
;
 Reactivity of the phosphaethynolate anion with stabilized carbocations:
 mechanistic studies and synthetic applications.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14406
_journal_page_last               14414
_journal_paper_doi               10.1039/d4sc03518f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C19 H27 N2 O P, C H2 Cl2'
_chemical_formula_sum            'C20 H29 Cl2 N2 O P'
_chemical_formula_weight         415.32
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-02-09 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                61.101(2)
_cell_angle_beta                 89.292(3)
_cell_angle_gamma                66.734(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8087(8)
_cell_length_b                   11.2182(8)
_cell_length_c                   11.3752(8)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.60
_cell_volume                     1081.66(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22682
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.456
_diffrn_reflns_theta_min         3.285
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+1.8005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1743
_reflns_Friedel_coverage         0
_reflns_number_gt                4583
_reflns_number_total             5322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03518f74.cif
_cod_data_source_block           10a
_cod_database_code               1572779
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              60241
_shelx_hkl_checksum              17241