Reactivity of metal hydrides with CO<sub>2</sub>: going beyond formate with a high-valent cationic pentahydride Mo(vi) complex.
Queyriaux, Nicolas; Cabrera-Trujillo, Jorge J; Durvin, Nina; Vendier, Laure; Miqueu, Karinne; Simonneau, Antoine; Chemical science 15 (2024) 20582–20589; doi:10.1039/d4sc04345f

data_1573267
_publ_section_title
;
 Reactivity of metal hydrides with CO<sub>2</sub>: going beyond formate
 with a high-valent cationic pentahydride Mo(vi) complex.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              20582
_journal_page_last               20589
_journal_paper_doi               10.1039/d4sc04345f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C21 H49 Mo O2 P4, C24 H20 B, 0.5(C4 H8 O)'
_chemical_formula_sum            'C47 H73 B Mo O2.5 P4'
_chemical_formula_weight         908.68
_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-2018/3
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                101.532(6)
_cell_angle_beta                 99.455(5)
_cell_angle_gamma                108.140(5)
_cell_formula_units_Z            4
_cell_length_a                   15.332(3)
_cell_length_b                   15.378(3)
_cell_length_c                   23.433(5)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.27
_cell_volume                     4989.8(18)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1241
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         0.914
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.7400
_exptl_absorpt_correction_T_min  0.6761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.728
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         16987
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+77.8036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11913
_reflns_number_total             16987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04345f3.cif
_cod_data_source_block           NDN200622
_cod_depositor_comments
;
Adding full bibliography for 1573265--1573268.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H146 B2 Mo2 O5 P8'
_cod_original_formula_weight         1817.37
_cod_original_formula_moiety     '2(C21 H49 Mo O2 P4), 2(C24 H20 B), C4 H8 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4989.8(16)
_cod_database_code               1573267
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              92597
_shelx_fab_checksum              3638