Probing Hydrogen Atom Transfer at a Phosphorus(V) Oxide Bond Using a "Bulky Hydrogen Atom" Surrogate: Analogies to PCET.
Chu, Jiaxiang; Carroll, Timothy G.; Wu, Guang; Telser, Joshua; Dobrovetsky, Roman; Ménard, Gabriel; Journal of the American Chemical Society 140 (2018) 15375–15383; doi:10.1021/jacs.8b09063

data_4133219
_publ_section_title
;
 Probing Hydrogen Atom Transfer at a Phosphorus(V) Oxide Bond Using a
 &quot;Bulky Hydrogen Atom&quot; Surrogate: Analogies to PCET.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15375
_journal_page_last               15383
_journal_paper_doi               10.1021/jacs.8b09063
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C54 H53 Cl4 F3 N O4 P S Si V'
_chemical_formula_weight         1162.86
_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-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 92.53(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.989(14)
_cell_length_b                   13.604(11)
_cell_length_c                   31.33(6)
_cell_measurement_reflns_used    170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10.48
_cell_measurement_theta_min      1.55
_cell_volume                     5531(13)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.5168
_diffrn_reflns_av_unetI/netI     0.7621
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20502
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        24.421
_diffrn_reflns_theta_max         24.421
_diffrn_reflns_theta_min         1.301
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.4669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.4212
_refine_ls_R_factor_gt           0.1316
_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^)+(0.0961P)^2^+0.5062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.3371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2029
_reflns_number_total             8793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09063_si_007.cif
_cod_data_source_block           cjx171106_0m_a
_cod_original_cell_volume        5531(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C54 H53 Cl4 F3 N1 O4 P S Si V'
_cod_database_code               4133219
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              73288
_shelx_hkl_checksum              80720