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_1565235
_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            'C44 H59 B2 N2 P'
_chemical_formula_weight         668.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 97.347(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.557(18)
_cell_length_b                   14.394(16)
_cell_length_c                   17.425(19)
_cell_measurement_reflns_used    6259
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.18
_cell_volume                     3870(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 0.982
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36660
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         1.841
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0337P)^2^+1.9111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5380
_reflns_number_total             6880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05135k2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565235
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014/5
_shelx_res_checksum              26106
_shelx_hkl_checksum              31095