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_1565236
_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            'C22 H29 B2 Cl0.25 Li2.25 O P'
_chemical_formula_weight         386.52
_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   mixed
_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                90
_cell_angle_beta                 106.257(4)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.597(6)
_cell_length_b                   14.635(3)
_cell_length_c                   23.112(4)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.26
_cell_volume                     9286(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54701
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.010
_diffrn_reflns_theta_min         1.717
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.204
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         11216
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1527P)^2^+13.8358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8071
_reflns_number_total             11216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05135k2.cif
_cod_data_source_block           1Int
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1565236
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2014/5
_shelx_res_checksum              84574
_shelx_hkl_checksum              96653