Regioselective transformation of 3-phosphoryl benzyne intermediates to diverse phosphorus-substituted arenes
Wang, Jing; Li, Zenghui; You, Gaoqiang; Xu, Liang; Gao, Pin; Rao, Bin; New Journal of Chemistry 46 (2022) 17049–17054; doi:10.1039/D2NJ03638J

data_7061758
_publ_section_title
;
 Regioselective transformation of 3-phosphoryl benzyne intermediates to
 diverse phosphorus-substituted arenes
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17049
_journal_page_last               17054
_journal_paper_doi               10.1039/D2NJ03638J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C25 H22 N O P'
_chemical_formula_weight         383.40
_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   mixed
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.269(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6473(11)
_cell_length_b                   12.3611(9)
_cell_length_c                   13.8580(11)
_cell_measurement_reflns_used    2052
_cell_measurement_temperature    302.(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.25
_cell_volume                     2068.8(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      302.(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20127
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                2746
_reflns_number_total             4737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03638j2.cif
_cod_data_source_block           202010709WJ
_cod_depositor_comments
'Adding full bibliography for 7061758--7061760.cif.'
_cod_database_code               7061758
_shelx_res_checksum              2783