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_7720501
_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         'C33 H51 Ir3 N Nb O2, C5 H12'
_chemical_formula_sum            'C38 H63 Ir3 N Nb O2'
_chemical_formula_weight         1235.40
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-23
_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                73.274(2)
_cell_angle_beta                 86.167(2)
_cell_angle_gamma                79.895(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1224(3)
_cell_length_b                   11.6146(3)
_cell_length_c                   16.8916(4)
_cell_measurement_reflns_used    22237
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      30.3680
_cell_measurement_theta_min      3.0360
_cell_volume                     2057.05(9)
_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(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.841
_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    -72.00  15.00   0.50   12.71    --    6.43 -51.00  19.00  174
  2  \w     -5.00  85.00   0.50   12.71    --    6.43  51.00 165.00  180
  3  \w     -3.00  74.00   0.50   12.71    --   -5.33  19.00-180.00  154
  4  \w    -84.00 -40.00   0.50   12.71    --   -5.33 -19.00 -90.00   88
  5  \w    -20.00  38.00   0.50   12.71    --   -5.33  57.00  90.00  116
  6  \w    -26.00  19.00   0.50   12.71    --   -5.33 -77.00-180.00   90
  7  \w    -26.00  19.00   0.50   12.71    --   -5.33 -77.00   0.00   90
  8  \w    -26.00  19.00   0.50   12.71    --   -5.33 -77.00 -60.00   90
  9  \w    -73.00 -40.00   0.50   12.71    --    6.43 -19.00-120.00   66
 10  \w     -7.00  42.00   0.50   12.71    --    6.43 -99.00  90.00   98
 11  \w    -73.00 -40.00   0.50   12.71    --    6.43 -19.00  30.00   66
 12  \w     -8.00  38.00   0.50   12.71    --    6.43  57.00 -30.00   92
 13  \w    -72.00  15.00   0.50   12.71    --    6.43 -51.00  19.00  174
 14  \w    -73.00 -48.00   0.50   12.71    --    6.43 -19.00-150.00   50
 15  \w     -7.00  42.00   0.50   12.71    --    6.43 -99.00 -60.00   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      -0.0594741000
_diffrn_orient_matrix_UB_12      0.0345361000
_diffrn_orient_matrix_UB_13      -0.0010790000
_diffrn_orient_matrix_UB_21      0.0182995000
_diffrn_orient_matrix_UB_22      0.0295302000
_diffrn_orient_matrix_UB_23      0.0274706000
_diffrn_orient_matrix_UB_31      0.0180351000
_diffrn_orient_matrix_UB_32      0.0459688000
_diffrn_orient_matrix_UB_33      -0.0341654000
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53801
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.302
_diffrn_reflns_theta_min         2.960
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.975
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.161
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.111a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       needle
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.987
_refine_diff_density_min         -2.006
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         10372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0177P)^2^+60.0579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8279
_reflns_number_total             10372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02432c2.cif
_cod_data_source_block           zd492_autored
_cod_database_code               7720501
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H63 Ir3 Nb1 N1 O2'
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.172
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              1163
_shelx_hkl_checksum              7188
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD492
_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 1.777
_oxdiff_exptl_absorpt_empirical_full_min 0.655