Activation of P-H Bond by a Frustrated Lewis Pair and its Application in Catalytic Z-selective Hydrophosphonylation of Terminal Ynones
Liu, Yizhen; Fan, Xiaoting; Li, Zhenhua; Wang, Huadong; Chem. Commun.  (2017) –; doi:10.1039/C7CC05028C

data_7120479
_publ_section_title
;
 Activation of P-H Bond by a Frustrated Lewis Pair and its Application in
 Catalytic Z-selective Hydrophosphonylation of Terminal Ynones
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05028C
_journal_year                    2017
_chemical_formula_sum            'C32 H32 B F15 N O3 P'
_chemical_formula_weight         805.36
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-10 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.758(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1359(14)
_cell_length_b                   14.9346(18)
_cell_length_c                   19.614(2)
_cell_measurement_reflns_used    7589
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.18
_cell_volume                     3503.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21201
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.128
_diffrn_reflns_theta_min         1.844
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.3156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             7706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05028c2.cif
_cod_data_source_block           mo_70308a
_cod_database_code               7120479
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              83678