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_4133221
_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 H39 F10 N O P Si V'
_chemical_formula_weight         1023.86
_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                86.349(4)
_cell_angle_beta                 83.120(4)
_cell_angle_gamma                64.869(4)
_cell_formula_units_Z            2
_cell_length_a                   11.123(2)
_cell_length_b                   11.304(2)
_cell_length_c                   20.103(4)
_cell_measurement_reflns_used    2141
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      1.05
_cell_volume                     2271.7(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14224
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.268
_diffrn_reflns_theta_min         1.990
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0384P)^2^+0.6845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6933
_reflns_number_total             9784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09063_si_008.cif
_cod_data_source_block           final_a
_cod_original_cell_volume        2271.7(8)
_cod_original_formula_sum        'C51 H39 F10 N1 O P Si V'
_cod_database_code               4133221
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              72962
_shelx_hkl_checksum              46828