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_4133222
_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            'C79 H47 B Cl2 F30 N O P Si V'
_chemical_formula_weight         1829.91
_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                 92.518(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   13.546(6)
_cell_length_c                   40.419(16)
_cell_measurement_reflns_used    299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      1.5
_cell_volume                     7513(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  Bruker-APEX-II
_diffrn_measurement_method       Omega-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2743
_diffrn_reflns_av_unetI/netI     0.3937
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            25233
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        23.183
_diffrn_reflns_theta_max         23.183
_diffrn_reflns_theta_min         1.009
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.3038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       needle
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.2855
_refine_ls_R_factor_gt           0.0931
_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^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3401
_reflns_number_total             10325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09063_si_004.cif
_cod_data_source_block           cjx171017_0m
_cod_original_cell_volume        7513(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C79 H47 B Cl2 F30 N1 O P Si V'
_cod_database_code               4133222
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              14321
_shelx_hkl_checksum              82019