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_1573268
_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         'C27 H63 Mo N2 P4, C24 H20 B'
_chemical_formula_sum            'C51 H83 B Mo N2 P4'
_chemical_formula_weight         954.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 90.4360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.28860(10)
_cell_length_b                   25.1547(2)
_cell_length_c                   20.9232(2)
_cell_measurement_reflns_used    64208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.3620
_cell_measurement_theta_min      2.7280
_cell_volume                     5941.21(9)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112023
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        65.075
_diffrn_reflns_theta_max         65.075
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.488(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         19997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+14.7783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                19255
_reflns_number_total             19997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04345f3.cif
_cod_data_source_block           NDN200722
_cod_depositor_comments
'Adding full bibliography for 1573265--1573268.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1573268
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              4361
_shelx_fab_checksum              25801