Proton to Hydride Umpolung at a Phosphonium Center Via Electron Relay: A New Strategy for Main-Group Based Water Reduction
Oishi, Takumi; Lugo-Fuentes, Leonardo I.; Jing, Yichuan; Jimenez-Halla, Jose Oscar Carlos; Barroso-Flores, Joaquín; Nakamoto, Masaaki; Yamamoto, Yohsuke; Tsunoji, Nao; Shang, Rong; Chemical Science  (2021) –; doi:10.1039/D1SC05135K

data_1565233
_publ_section_title
;
 Proton to Hydride Umpolung at a Phosphonium Center Via Electron Relay: A
 New Strategy for Main-Group Based Water Reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05135K
_journal_year                    2021
_chemical_formula_sum            'C60 H74 B4 O8 P2'
_chemical_formula_weight         1028.37
_chemical_name_systematic        2014/7
_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-2014/5
_audit_update_record
;
2021-07-14 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.883(2)
_cell_angle_beta                 91.015(2)
_cell_angle_gamma                99.535(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9474(18)
_cell_length_b                   14.320(2)
_cell_length_c                   19.292(3)
_cell_measurement_reflns_used    8165
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.19
_cell_volume                     2876.7(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34791
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         1.890
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         13873
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0628P)^2^+1.0459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9651
_reflns_number_total             13873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05135k2.cif
_cod_data_source_block           1a
_cod_database_code               1565233
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2014/5
_shelx_res_checksum              32447
_shelx_hkl_checksum              23966