Visible-light driven H<sub>2</sub> reductive elimination unlocks reactivity in polyhydrido niobium iridium clusters.
Dubrawski, Zachary; Aïssiou, Samy; Jeanneau, Erwann; Thieuleux, Chloé; Camp, Clément; Dalton transactions (Cambridge, England : 2003) 55 (2026) 620–629; doi:10.1039/d5dt02432c

data_7720499
_publ_section_title
;
 Visible-light driven H<sub>2</sub> reductive elimination unlocks
 reactivity in polyhydrido niobium iridium clusters.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              620
_journal_page_last               629
_journal_paper_doi               10.1039/d5dt02432c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C24 H42 Ir2 N2 Nb'
_chemical_formula_sum            'C24 H42 Ir2 N2 Nb'
_chemical_formula_weight         835.90
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-01
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-09-11 deposited with the CCDC.	2025-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.588(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1262(3)
_cell_length_b                   11.8871(3)
_cell_length_c                   23.4515(6)
_cell_measurement_reflns_used    24333
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2800
_cell_measurement_theta_min      3.0000
_cell_volume                     2783.45(13)
_computing_cell_refinement       'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.114a 64-bit (release 13-06-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -85.00 -25.00   0.50    3.34    --   -5.33 -25.00  50.00  120
  2  \w    -73.00 -25.00   0.50    3.34    --    6.43 -25.00  50.00   96
  3  \w     -4.00  87.00   0.50    3.34    --    6.43  25.00-145.00  182
  4  \w    -26.00  19.00   0.50    3.34    --   -5.33 -77.00 150.00   90
  5  \w    -59.00   9.00   0.50    3.34    --   -5.33 -57.00 150.00  136
  6  \w    -84.00 -40.00   0.50    3.34    --   -5.33 -19.00 -60.00   88
  7  \w    -84.00 -40.00   0.50    3.34    --   -5.33 -19.00-150.00   88
  8  \w    -73.00 -40.00   0.50    3.34    --    6.43 -19.00 120.00   66
  9  \w     -8.00  38.00   0.50    3.34    --    6.43  57.00 -30.00   92
 10  \w    -84.00 -40.00   0.50    3.34    --   -5.33 -19.00   0.00   88
 11  \w     -7.00  42.00   0.50    3.34    --    6.43 -99.00  30.00   98
 12  \w     -7.00  42.00   0.50    3.34    --    6.43 -99.00 -60.00   98
 13  \w     -7.00  26.00   0.50    3.34    --    6.43 -99.00 120.00   66
 14  \w     -7.00  42.00   0.50    3.34    --    6.43 -99.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0576264000
_diffrn_orient_matrix_UB_12      -0.0130916000
_diffrn_orient_matrix_UB_13      0.0122593000
_diffrn_orient_matrix_UB_21      -0.0414640000
_diffrn_orient_matrix_UB_22      0.0142710000
_diffrn_orient_matrix_UB_23      -0.0264531000
_diffrn_orient_matrix_UB_31      0.0028505000
_diffrn_orient_matrix_UB_32      -0.0564346000
_diffrn_orient_matrix_UB_33      -0.0095243000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            63066
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.428
_diffrn_reflns_theta_min         2.909
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.111a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.164
_refine_diff_density_max         2.602
_refine_diff_density_min         -2.876
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         7441
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+22.5452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6152
_reflns_number_total             7441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02432c2.cif
_cod_data_source_block           zd519_autored
_cod_database_code               7720499
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H42 Ir2 N2 Nb1'
_shelx_estimated_absorpt_t_max   0.292
_shelx_estimated_absorpt_t_min   0.152
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              26902
_shelx_hkl_checksum              97915
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD519
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.629
_oxdiff_exptl_absorpt_empirical_full_min 0.391