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_4133223
_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            'C71 H62 Co F10.5 N O P V'
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 97.977(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.851(3)
_cell_length_b                   17.848(4)
_cell_length_c                   41.744(10)
_cell_measurement_reflns_used    549
_cell_measurement_temperature    100(2)
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_cell_volume                     11695(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.1306
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            21187
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.502
_diffrn_reflns_theta_max         24.502
_diffrn_reflns_theta_min         0.985
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             5468
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.00105(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         9604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.2109
_refine_ls_R_factor_gt           0.1751
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1352.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4086
_refine_ls_wR_factor_ref         0.4246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6798
_reflns_number_total             9604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09063_si_003.cif
_cod_data_source_block           cjx170511_0m
_cod_original_cell_volume        11696(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C71 H62 Co F10.50 N1 O P V'
_cod_database_code               4133223
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              55593
_shelx_hkl_checksum              87116