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_4133224
_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            'C51 H49 N O P Si V'
_chemical_formula_weight         843.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                91.307(18)
_cell_angle_beta                 101.044(18)
_cell_angle_gamma                92.562(17)
_cell_formula_units_Z            2
_cell_length_a                   10.070(8)
_cell_length_b                   11.163(9)
_cell_length_c                   20.610(18)
_cell_measurement_reflns_used    898
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      19.7
_cell_measurement_theta_min      2.59
_cell_volume                     2270(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'bruker kappa apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14945
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.608
_diffrn_reflns_theta_min         1.007
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.745349
_exptl_absorpt_correction_T_min  0.593313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         8370
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1703
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4101
_reflns_number_total             8370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09063_si_009.cif
_cod_data_source_block           final_a
_cod_original_formula_sum        'C51 H49 N1 O P Si V'
_cod_database_code               4133224
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              85398
_shelx_hkl_checksum              75538