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_7061760
_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            'C21 H31 Br N5 O2 P'
_chemical_formula_weight         496.38
_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_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.2044(5)
_cell_length_b                   28.6736(9)
_cell_length_c                   21.3349(7)
_cell_measurement_reflns_used    4546
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.42
_cell_measurement_theta_min      2.55
_cell_volume                     9455.7(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            140593
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.360
_diffrn_reflns_theta_min         2.662
_exptl_absorpt_coefficient_mu    3.225
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.861
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         18651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+4.9757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16716
_reflns_number_total             18651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03638j2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
;
Adding full bibliography for 7061758--7061760.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C84 H124 Br4 N20 O8 P4'
_cod_original_formula_weight         1985.54
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7061760
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              57988