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_7720502
_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         'C32 H51 Ir3 N Nb'
_chemical_formula_sum            'C32 H51 Ir3 N Nb'
_chemical_formula_weight         1119.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-31
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.54910(10)
_cell_length_b                   13.87850(10)
_cell_length_c                   20.41610(10)
_cell_measurement_reflns_used    54188
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      78.0500
_cell_measurement_theta_min      3.4640
_cell_volume                     3555.72(4)
_computing_cell_refinement       'CrysAlisPro 1.171.44.101a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.98a 64-bit (release 07-03-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.101a (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      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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   -156.00 -79.00   0.50    0.72    --  -81.95 -61.00-150.00  154
  2  \w   -126.00 -79.00   0.50    0.18    --  -50.53 -57.00 -90.00   94
  3  \w   -126.00 -79.00   0.50    0.18    --  -50.53 -57.00 -30.00   94
  4  \w   -159.00 -75.00   0.50    0.72    --  -81.95 -45.00-120.00  168
  5  \w   -126.00 -79.00   0.50    0.18    --  -50.53 -57.00   0.00   94
  6  \w   -159.00 -75.00   0.50    0.72    --  -81.95 -45.00 -30.00  168
  7  \w   -159.00 -75.00   0.50    0.72    --  -81.95 -45.00   0.00  168
  8  \w   -159.00 -75.00   0.50    0.72    --  -81.95 -45.00 -60.00  168
  9  \w   -128.00 -44.00   0.50    0.18    --  -50.53 -38.00  30.00  168
 10  \w   -128.00 -44.00   0.50    0.18    --  -50.53 -38.00  90.00  168
 11  \w   -159.00 -74.00   0.50    0.72    --  -81.95 -47.00 157.00  170
 12  \w   -156.00 -79.00   0.50    0.72    --  -81.95 -61.00 120.00  154
 13  \w   -156.00 -79.00   0.50    0.72    --  -81.95 -61.00  60.00  154
 14  \w   -128.00 -44.00   0.50    0.18    --  -50.53 -38.00 -90.00  168
 15  \w   -128.00 -44.00   0.50    0.18    --  -50.53 -38.00-180.00  168
 16  \w    -66.00 -11.00   0.50    0.72    --  -81.95  99.00  44.00  110
 17  \w    -67.00 -12.00   0.50    0.72    --  -81.95  84.00 152.00  110
 18  \w    -19.00  28.00   0.50    0.18    --  -50.53  38.00  60.00   94
 19  \w    -31.00  -5.00   0.50    0.72    --  -81.95  47.00 -53.00   52
 20  \w    -19.00  28.00   0.50    0.18    --  -50.53  38.00 -90.00   94
 21  \w     31.00  75.00   0.50    0.72    --   99.76 -77.00 -30.00   88
 22  \w     42.00  75.00   0.50    0.72    --  111.05 -77.00  30.00   66
 23  \w     42.00  75.00   0.50    0.72    --  111.05 -77.00  60.00   66
 24  \w    120.00 170.00   0.50    0.72    --   99.76  84.00 152.00  100
 25  \w    119.00 171.00   0.50    0.72    --   99.76  99.00  44.00  104
 26  \w     31.00  75.00   0.50    0.72    --   99.76 -77.00-180.00   88
 27  \w     36.00 101.00   0.50    0.72    --  111.05-125.00 -90.00  130
 28  \w     40.00  92.00   0.50    0.72    --  111.05 -99.00 -61.00  104
 29  \w     29.00  92.00   0.50    0.72    --   99.76 -95.00  60.00  126
 30  \w     40.00  92.00   0.50    0.72    --  111.05 -95.00 120.00  104
 31  \w     36.00 101.00   0.50    0.72    --  111.05-125.00  30.00  130
 32  \w     29.00  92.00   0.50    0.72    --   99.76 -95.00-180.00  126
 33  \w     98.00 136.00   0.50    0.72    --  111.05  15.00-180.00   76
 34  \w    121.00 178.00   0.50    0.72    --  111.05  77.00-180.00  114
 35  \w    121.00 169.00   0.50    0.72    --   99.76  77.00-120.00   96
 36  \w    121.00 169.00   0.50    0.72    --   99.76  77.00 -90.00   96
 37  \w     92.00 177.00   0.50    0.72    --   99.76  47.00 -53.00  170
 38  \w     92.00 177.00   0.50    0.72    --   99.76  47.00 -53.00  170
 39  \w     98.00 136.00   0.50    0.72    --  111.05  15.00 -90.00   76
 40  \w     87.00 136.00   0.50    0.72    --   99.76  15.00  30.00   98
 41  \w     98.00 136.00   0.50    0.72    --  111.05  15.00  60.00   76
 42  \w     87.00 136.00   0.50    0.72    --   99.76  15.00  90.00   98
 43  \w     93.00 166.00   0.50    0.72    --   99.76  30.00 120.00  146
 44  \w   -152.00 -97.00   0.50    0.72    --  -81.95 -95.00 -90.00  110
;
_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      -0.0434104000
_diffrn_orient_matrix_UB_12      0.1037997000
_diffrn_orient_matrix_UB_13      0.0025131000
_diffrn_orient_matrix_UB_21      -0.0558289000
_diffrn_orient_matrix_UB_22      -0.0155454000
_diffrn_orient_matrix_UB_23      -0.0663421000
_diffrn_orient_matrix_UB_31      -0.1002597000
_diffrn_orient_matrix_UB_32      -0.0361629000
_diffrn_orient_matrix_UB_33      0.0359436000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67254
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.824
_diffrn_reflns_theta_min         3.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.101a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.911
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 3194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(7)
_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     351
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0349P)^2^+11.9592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                7399
_reflns_number_total             7433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02432c2.cif
_cod_data_source_block           zd433_autored
_cod_database_code               7720502
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H51 Ir3 N1 Nb1'
_chemical_oxdiff_usercomment     'CSD: MOHWOV'
_shelx_estimated_absorpt_t_max   0.381
_shelx_estimated_absorpt_t_min   0.099
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C),
 C32(H32A,H32B,H32C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              37218
_shelx_hkl_checksum              16700
_olex2_submission_original_sample_id ZD433
_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 4.474
_oxdiff_exptl_absorpt_empirical_full_min 0.647