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_7720503
_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         'C40 H60 Ir4 Nb'
_chemical_formula_sum            'C40 H60 Ir4 Nb'
_chemical_formula_weight         1402.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-02
_audit_creation_method
;
Olex2 1.5-ac7-018
(compiled 2025.08.06 svn.rb7424aed for Rigaku Oxford Diffraction, GUI svn.r7314)
;
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2025-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7793(2)
_cell_length_b                   24.6740(3)
_cell_length_c                   13.8521(2)
_cell_measurement_reflns_used    45484
_cell_measurement_temperature    100.02(12)
_cell_measurement_theta_max      76.8370
_cell_measurement_theta_min      3.5570
_cell_volume                     4280.25(11)
_computing_cell_refinement       'CrysAlisPro 1.171.44.114a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.111a 64-bit (release 13-05-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.114a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(12)
_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 0.971
_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    -56.00  26.00   0.50    0.77    --  -47.53  65.00 -40.00  164
  2  \w    -24.00  56.00   0.50    0.77    --   49.03 -65.00-175.00  160
  3  \w   -155.00 -83.00   0.50    3.06    --  -81.95 -65.00-175.00  144
  4  \w   -155.00 -83.00   0.50    3.06    --  -81.95 -65.00-175.00  144
  5  \w    -56.00  -9.00   0.50    3.06    --  -81.95  65.00 -40.00   94
  6  \w     27.00  56.00   0.50    3.06    --   99.76 -65.00-175.00   58
  7  \w    105.00 173.00   0.50    3.06    --   99.76  65.00 -40.00  136
  8  \w    -19.00  31.00   0.50    0.77    --  -47.53  38.00-120.00  100
  9  \w    -56.00  26.00   0.50    0.77    --  -47.53  65.00 -40.00  164
 10  \w    -19.00  31.00   0.50    0.77    --  -47.53  38.00  30.00  100
 11  \w    -19.00  31.00   0.50    0.77    --  -47.53  38.00  90.00  100
 12  \w    -26.00  45.00   0.50    0.77    --   49.03 -57.00 -90.00  142
 13  \w    -51.00  -8.00   0.50    3.06    --  -81.95  61.00  30.00   86
 14  \w    -51.00  -8.00   0.50    3.06    --  -81.95  61.00 -90.00   86
 15  \w    -74.00  -9.00   0.50    3.06    --  -81.95 125.00  90.00  130
 16  \w   -151.00 -99.00   0.50    3.06    --  -81.95 -77.00 -90.00  104
 17  \w     31.00  75.00   0.50    3.06    --   99.76 -77.00   0.00   88
 18  \w     31.00 100.00   0.50    3.06    --   99.76-125.00 -60.00  138
 19  \w     87.00 136.00   0.50    3.06    --   99.76  15.00  60.00   98
 20  \w    121.00 169.00   0.50    3.06    --   99.76  77.00-150.00   96
 21  \w     87.00 136.00   0.50    3.06    --   99.76  15.00 120.00   98
 22  \w     98.00 136.00   0.50    3.06    --  111.05  15.00-120.00   76
 23  \w     42.00  75.00   0.50    3.06    --  111.05 -77.00  60.00   66
 24  \w     42.00  75.00   0.50    3.06    --  111.05 -77.00 -90.00   66
 25  \w     98.00 136.00   0.50    3.06    --  111.05  15.00 -90.00   76
 26  \w     42.00  75.00   0.50    3.06    --  111.05 -77.00  90.00   66
 27  \w     42.00  75.00   0.50    3.06    --  111.05 -77.00-150.00   66
 28  \w     40.00  92.00   0.50    3.06    --  111.05 -95.00 -30.00  104
 29  \w     42.00  75.00   0.50    3.06    --  111.05 -77.00  30.00   66
 30  \w    105.00 178.00   0.50    3.06    --  111.05  65.00 -40.00  146
 31  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00 -60.00  168
 32  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00  90.00  168
 33  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00   0.00  168
 34  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00-180.00  168
 35  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00-120.00  168
 36  \w   -125.00 -41.00   0.50    0.77    --  -47.53 -38.00  30.00  168
 37  \w   -159.00 -75.00   0.50    3.06    --  -81.95 -45.00   0.00  168
 38  \w   -159.00 -75.00   0.50    3.06    --  -81.95 -45.00 120.00  168
 39  \w   -159.00 -75.00   0.50    3.06    --  -81.95 -45.00 -60.00  168
 40  \w   -156.00-131.00   0.50    3.06    --  -81.95 -61.00-150.00   50
 41  \w   -156.00 -79.00   0.50    3.06    --  -81.95 -61.00  60.00  154
 42  \w   -159.00 -75.00   0.50    3.06    --  -81.95 -45.00-120.00  168
 43  \w     31.00 100.00   0.50    3.06    --   99.76-125.00 150.00  138
 44  \w     98.00 136.00   0.50    3.06    --  111.05  15.00-150.00   76
 45  \w     98.00 136.00   0.50    3.06    --  111.05  15.00 -60.00   76
 46  \w     98.00 136.00   0.50    3.06    --  111.05  15.00  90.00   76
 47  \w     98.00 136.00   0.50    3.06    --  111.05  15.00 -30.00   76
 48  \w     40.00  92.00   0.50    3.06    --  111.05 -95.00 150.00  104
 49  \w     98.00 136.00   0.50    3.06    --  111.05  15.00 150.00   76
;
_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      0.0368887000
_diffrn_orient_matrix_UB_12      0.0150353000
_diffrn_orient_matrix_UB_13      0.1095415000
_diffrn_orient_matrix_UB_21      0.0724868000
_diffrn_orient_matrix_UB_22      0.0446030000
_diffrn_orient_matrix_UB_23      -0.0287585000
_diffrn_orient_matrix_UB_31      -0.0921438000
_diffrn_orient_matrix_UB_32      0.0410144000
_diffrn_orient_matrix_UB_33      -0.0089865000
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            80880
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.934
_diffrn_reflns_theta_min         3.583
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.749
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.114a (Rigaku Oxford Diffraction, 2025)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_description       block
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.051
_refine_diff_density_max         2.741
_refine_diff_density_min         -3.177
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     2856
_refine_ls_restrained_S_all      79.086
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+79.6710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8216
_reflns_number_total             8988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02432c2.cif
_cod_data_source_block           zd473_CCDC2487219
_cod_database_code               7720503
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H70 Ir4 N '
_diffrn_oxdiff_digest_hkl
;
439fd440b9019cdf5b00b9e279afacd5ae5784
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name ZD473.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24B-C25B = C24B-C23B = C25B-C21B = C21B-C22B = C22B-C23B
 1.42 with sigma of 0.02
 C24B-C29B = C23B-C28B
 1.5 with sigma of 0.02
 C25B-C13 = C21B-C26B = C22B-C27B
 1.51 with sigma of 0.02
 C4B-C5B = C4B-C3B = C5B-C1B = C1B-C2B = C2B-C3B
 1.42 with sigma of 0.02
 C4B-C9B = C3B-C8B
 1.5 with sigma of 0.02
 C5B-C10B = C1B-C6B = C2B-C7B
 1.51 with sigma of 0.02
 C15B-C14B = C15B-C11B = C14B-C13B = C13B-C12B = C12B-C11B
 1.42 with sigma of 0.02
 C15B-C20B = C11B-C16B
 1.5 with sigma of 0.02
 C14B-C19B = C13B-C18B = C12B-C17B
 1.51 with sigma of 0.02
 C24B-C21B = C24B-C22B
 2.29 with sigma of 0.04
 C24B-C13 = C24B-C28B = C25B-C26B
 2.6 with sigma of 0.04
 C25B-C22B = C21B-C23B
 2.3 with sigma of 0.04
 C21B-C27B = C22B-C28B
 2.61 with sigma of 0.04
 C4B-C1B = C4B-C2B
 2.29 with sigma of 0.04
 C4B-C10B = C4B-C8B = C5B-C6B
 2.6 with sigma of 0.04
 C5B-C2B = C1B-C3B
 2.3 with sigma of 0.04
 C1B-C7B = C2B-C8B
 2.61 with sigma of 0.04
 C15B-C13B = C15B-C12B
 2.29 with sigma of 0.04
 C15B-C19B = C15B-C16B = C14B-C18B
 2.6 with sigma of 0.04
 C14B-C12B = C13B-C11B
 2.3 with sigma of 0.04
 C13B-C17B = C12B-C16B
 2.61 with sigma of 0.04
 C24B-C25B \\sim C25B-C21B \\sim C21B-C22B \\sim C22B-C23B \\sim C23B-C24B
 with sigma of 0.02
 C24B-C21B \\sim C25B-C22B \\sim C21B-C23B \\sim C23B-C25B \\sim C24B-C22B
 with sigma of 0.04
 C24B-C29B \\sim C25B-C13 \\sim C21B-C26B \\sim C22B-C27B \\sim C23B-C28B
 with sigma of 0.02
 C29B-C25B \\sim C29B-C23B \\sim C13-C24B \\sim C13-C21B \\sim C26B-C25B \\sim
C26B-C22B \\sim C27B-
 C21B \\sim C27B-C23B \\sim C28B-C22B \\sim C28B-C24B
 with sigma of 0.04
 C24B-C25B \\sim C33-C34
 with sigma of 0.02
 C24B-C23B \\sim C33-C32_$1
 with sigma of 0.02
 C24B-C29B \\sim C33-C38
 with sigma of 0.02
 C25B-C21B \\sim C34-C35
 with sigma of 0.02
 C25B-C13 \\sim C34-C39
 with sigma of 0.02
 C21B-C22B \\sim C35-C31_$1
 with sigma of 0.02
 C21B-C26B \\sim C35-C40_$2
 with sigma of 0.02
 C22B-C23B \\sim C31-C32
 with sigma of 0.02
 C22B-C27B \\sim C31-C36
 with sigma of 0.02
 C23B-C28B \\sim C32-C37
 with sigma of 0.02
 Ir3A-C24B \\sim Ir3A-C33
 with sigma of 0.04
 Ir3A-C25B \\sim Ir3A-C34
 with sigma of 0.04
 Ir3A-C21B \\sim Ir3A-C35
 with sigma of 0.04
 Ir3A-C22B \\sim Ir3A-C31_$1
 with sigma of 0.04
 Ir3A-C23B \\sim Ir3A-C32_$1
 with sigma of 0.04
 Ir3A-C28B \\sim Ir3A-C37_$1
 with sigma of 0.04
 Ir3A-C27B \\sim Ir3A-C36_$1
 with sigma of 0.04
 Ir3A-C26B \\sim Ir3A-C40_$2
 with sigma of 0.04
 Ir3A-C13 \\sim Ir3A-C39
 with sigma of 0.04
 Ir3A-C29B \\sim Ir3A-C38
 with sigma of 0.04
 Ir3B-C24B \\sim Ir3B-C33
 with sigma of 0.04
 Ir3B-C25B \\sim Ir3B-C34
 with sigma of 0.04
 Ir3B-C21B \\sim Ir3B-C35
 with sigma of 0.04
 Ir3B-C22B \\sim Ir3B-C31_$1
 with sigma of 0.04
 Ir3B-C23B \\sim Ir3B-C32_$1
 with sigma of 0.04
 Ir3B-C27B \\sim Ir3B-C36_$1
 with sigma of 0.04
 Ir3B-C26B \\sim Ir3B-C40_$2
 with sigma of 0.04
 Ir3B-C13 \\sim Ir3B-C39
 with sigma of 0.04
 C24B-C21B \\sim C33-C35
 with sigma of 0.04
 C24B-C22B \\sim C33-C31_$1
 with sigma of 0.04
 C24B-C28B \\sim C33-C37_$1
 with sigma of 0.04
 C24B-C13 \\sim C33-C39
 with sigma of 0.04
 C25B-C22B \\sim C34-C31_$1
 with sigma of 0.04
 C25B-C23B \\sim C34-C32_$1
 with sigma of 0.04
 C25B-C26B \\sim C34-C40_$2
 with sigma of 0.04
 C25B-C29B \\sim C34-C38
 with sigma of 0.04
 C21B-C23B \\sim C35-C32_$1
 with sigma of 0.04
 C21B-C27B \\sim C35-C36_$1
 with sigma of 0.04
 C21B-C13 \\sim C35-C39
 with sigma of 0.04
 C22B-C28B \\sim C31-C37
 with sigma of 0.04
 C22B-C26B \\sim C31_$1-C40_$2
 with sigma of 0.04
 C23B-C27B \\sim C32-C36
 with sigma of 0.04
 C23B-C29B \\sim C32_$1-C38
 with sigma of 0.04
 C34-C33 \\sim C25B-C24B \\sim C23B-C24B \\sim C32_$1-C33 \\sim C32-C31 \\sim
C23B-C22B \\sim C31_$1-
 C35 \\sim C22B-C21B \\sim C35-C34 \\sim C21B-C25B
 with sigma of 0.01
 C21B-C26B \\sim C34-C39 \\sim C25B-C13 \\sim C33-C38 \\sim C24B-C29B \\sim
C32-C37 \\sim C23B-C28B ~
 C31-C36 \\sim C22B-C27B \\sim C35-C40_$2
 with sigma of 0.01
 C4B-C5B \\sim C5B-C1B \\sim C1B-C2B \\sim C2B-C3B \\sim C3B-C4B
 with sigma of 0.02
 C4B-C1B \\sim C5B-C2B \\sim C1B-C3B \\sim C3B-C5B \\sim C4B-C2B
 with sigma of 0.04
 C4B-C9B \\sim C5B-C10B \\sim C1B-C6B \\sim C2B-C7B \\sim C3B-C8B
 with sigma of 0.02
 C9B-C5B \\sim C9B-C3B \\sim C10B-C4B \\sim C10B-C1B \\sim C6B-C5B \\sim
C6B-C2B \\sim C7B-C1B \\sim C7B-
 C3B \\sim C8B-C2B \\sim C8B-C4B
 with sigma of 0.04
 C4B-C5B \\sim C3A-C4A
 with sigma of 0.02
 C4B-C3B \\sim C3A-C2A
 with sigma of 0.02
 C4B-C9B \\sim C3A-C8A
 with sigma of 0.02
 C5B-C1B \\sim C4A-C5A
 with sigma of 0.02
 C5B-C10B \\sim C4A-C9A
 with sigma of 0.02
 C1B-C2B \\sim C5A-C1A
 with sigma of 0.02
 C1B-C6B \\sim C5A-C10A
 with sigma of 0.02
 C2B-C3B \\sim C1A-C2A
 with sigma of 0.02
 C2B-C7B \\sim C1A-C6A
 with sigma of 0.02
 C3B-C8B \\sim C2A-C7A
 with sigma of 0.02
 Ir1A-C4B \\sim Ir1A-C3A
 with sigma of 0.04
 Ir1A-C5B \\sim Ir1A-C4A
 with sigma of 0.04
 Ir1A-C1B \\sim Ir1A-C5A
 with sigma of 0.04
 Ir1A-C2B \\sim Ir1A-C1A
 with sigma of 0.04
 Ir1A-C3B \\sim Ir1A-C2A
 with sigma of 0.04
 Ir1A-C8B \\sim Ir1A-C7A
 with sigma of 0.04
 Ir1A-C7B \\sim Ir1A-C6A
 with sigma of 0.04
 Ir1A-C6B \\sim Ir1A-C10A
 with sigma of 0.04
 Ir1A-C10B \\sim Ir1A-C9A
 with sigma of 0.04
 Ir1A-C9B \\sim Ir1A-C8A
 with sigma of 0.04
 Ir1B-C4B \\sim Ir1B-C3A
 with sigma of 0.04
 Ir1B-C5B \\sim Ir1B-C4A
 with sigma of 0.04
 Ir1B-C1B \\sim Ir1B-C5A
 with sigma of 0.04
 Ir1B-C2B \\sim Ir1B-C1A
 with sigma of 0.04
 Ir1B-C3B \\sim Ir1B-C2A
 with sigma of 0.04
 Ir1B-C8B \\sim Ir1B-C7A
 with sigma of 0.04
 Ir1B-C7B \\sim Ir1B-C6A
 with sigma of 0.04
 Ir1B-C6B \\sim Ir1B-C10A
 with sigma of 0.04
 Ir1B-C10B \\sim Ir1B-C9A
 with sigma of 0.04
 Ir1B-C9B \\sim Ir1B-C8A
 with sigma of 0.04
 C4B-C1B \\sim C3A-C5A
 with sigma of 0.04
 C4B-C2B \\sim C3A-C1A
 with sigma of 0.04
 C4B-C8B \\sim C3A-C7A
 with sigma of 0.04
 C4B-C10B \\sim C3A-C9A
 with sigma of 0.04
 C5B-C2B \\sim C4A-C1A
 with sigma of 0.04
 C5B-C3B \\sim C4A-C2A
 with sigma of 0.04
 C5B-C6B \\sim C4A-C10A
 with sigma of 0.04
 C5B-C9B \\sim C4A-C8A
 with sigma of 0.04
 C1B-C3B \\sim C5A-C2A
 with sigma of 0.04
 C1B-C7B \\sim C5A-C6A
 with sigma of 0.04
 C1B-C10B \\sim C5A-C9A
 with sigma of 0.04
 C2B-C8B \\sim C1A-C7A
 with sigma of 0.04
 C2B-C6B \\sim C1A-C10A
 with sigma of 0.04
 C3B-C7B \\sim C2A-C6A
 with sigma of 0.04
 C3B-C9B \\sim C2A-C8A
 with sigma of 0.04
 C7B-C2B \\sim C6A-C1A \\sim C6B-C1B \\sim C10A-C5A \\sim C10B-C5B \\sim
C9A-C4A \\sim C9B-C4B \\sim C8A-
 C3A \\sim C8B-C3B \\sim C7A-C2A
 with sigma of 0.01
 C2A-C1A \\sim C2B-C1B \\sim C1A-C5A \\sim C1B-C5B \\sim C5A-C4A \\sim C5B-C4B
\\sim C4A-C3A \\sim C3B-C4B
 \\sim C2A-C3A \\sim C3B-C2B
 with sigma of 0.01
 C15B-C14B \\sim C14B-C13B \\sim C13B-C12B \\sim C12B-C11B \\sim C11B-C15B
 with sigma of 0.02
 C15B-C13B \\sim C14B-C12B \\sim C13B-C11B \\sim C11B-C14B \\sim C15B-C12B
 with sigma of 0.04
 C15B-C20B \\sim C14B-C19B \\sim C13B-C18B \\sim C12B-C17B \\sim C11B-C16B
 with sigma of 0.02
 C20B-C14B \\sim C20B-C11B \\sim C19B-C15B \\sim C19B-C13B \\sim C18B-C14B
\\sim C18B-C12B \\sim C17B-
 C13B \\sim C17B-C11B \\sim C16B-C12B \\sim C16B-C15B
 with sigma of 0.04
 C15B-C14B \\sim C13A-C12A
 with sigma of 0.02
 C15B-C11B \\sim C13A-C14A
 with sigma of 0.02
 C15B-C20B \\sim C13A-C18A
 with sigma of 0.02
 C14B-C13B \\sim C12A-C11A
 with sigma of 0.02
 C14B-C19B \\sim C12A-C17A
 with sigma of 0.02
 C13B-C12B \\sim C11A-C15A
 with sigma of 0.02
 C13B-C18B \\sim C11A-C16A
 with sigma of 0.02
 C12B-C11B \\sim C15A-C14A
 with sigma of 0.02
 C12B-C17B \\sim C15A-C20A
 with sigma of 0.02
 C11B-C16B \\sim C14A-C19A
 with sigma of 0.02
 Ir2B-C15B \\sim Ir2B-C13A
 with sigma of 0.04
 Ir2B-C14B \\sim Ir2B-C12A
 with sigma of 0.04
 Ir2B-C13B \\sim Ir2B-C11A
 with sigma of 0.04
 Ir2B-C12B \\sim Ir2B-C15A
 with sigma of 0.04
 Ir2B-C11B \\sim Ir2B-C14A
 with sigma of 0.04
 Ir2B-C17B \\sim Ir2B-C20A
 with sigma of 0.04
 Ir2B-C18B \\sim Ir2B-C16A
 with sigma of 0.04
 Ir2B-C19B \\sim Ir2B-C17A
 with sigma of 0.04
 Ir2B-C20B \\sim Ir2B-C18A
 with sigma of 0.04
 Ir2A-C15B \\sim Ir2A-C13A
 with sigma of 0.04
 Ir2A-C14B \\sim Ir2A-C12A
 with sigma of 0.04
 Ir2A-C13B \\sim Ir2A-C11A
 with sigma of 0.04
 Ir2A-C12B \\sim Ir2A-C15A
 with sigma of 0.04
 Ir2A-C11B \\sim Ir2A-C14A
 with sigma of 0.04
 Ir2A-C16B \\sim Ir2A-C19A
 with sigma of 0.04
 Ir2A-C17B \\sim Ir2A-C20A
 with sigma of 0.04
 Ir2A-C18B \\sim Ir2A-C16A
 with sigma of 0.04
 Ir2A-C19B \\sim Ir2A-C17A
 with sigma of 0.04
 Ir2A-C20B \\sim Ir2A-C18A
 with sigma of 0.04
 C15B-C13B \\sim C13A-C11A
 with sigma of 0.04
 C15B-C12B \\sim C13A-C15A
 with sigma of 0.04
 C15B-C16B \\sim C13A-C19A
 with sigma of 0.04
 C15B-C19B \\sim C13A-C17A
 with sigma of 0.04
 C14B-C12B \\sim C12A-C15A
 with sigma of 0.04
 C14B-C11B \\sim C12A-C14A
 with sigma of 0.04
 C14B-C18B \\sim C12A-C16A
 with sigma of 0.04
 C14B-C20B \\sim C12A-C18A
 with sigma of 0.04
 C13B-C11B \\sim C11A-C14A
 with sigma of 0.04
 C13B-C17B \\sim C11A-C20A
 with sigma of 0.04
 C13B-C19B \\sim C11A-C17A
 with sigma of 0.04
 C12B-C16B \\sim C15A-C19A
 with sigma of 0.04
 C12B-C18B \\sim C15A-C16A
 with sigma of 0.04
 C11B-C17B \\sim C14A-C20A
 with sigma of 0.04
 C11B-C20B \\sim C14A-C18A
 with sigma of 0.04
 C20B-C15B \\sim C12A-C17A \\sim C14B-C19B \\sim C11A-C16A \\sim C13B-C18B
\\sim C15A-C20A \\sim C12B-
 C17B \\sim C14A-C19A \\sim C16B-C11B \\sim C13A-C18A
 with sigma of 0.01
 C13B-C14B \\sim C11A-C12A \\sim C14B-C15B \\sim C12A-C13A \\sim C11B-C15B
\\sim C14A-C13A \\sim C12B-
 C11B \\sim C15A-C14A \\sim C15A-C11A \\sim C12B-C13B
 with sigma of 0.01
3. Restrained planarity
 C13, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B
 with sigma of 0.1
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma of 0.1
 C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C13 \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim
C27B \\sim C28B \\sim C29B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C13 \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim
C27B \\sim C28B \\sim C29B \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35
\\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A
\\sim C7A \\sim C8A \\sim C9A \\sim C10A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C13 \\sim C21A \\sim C21B \\sim C22A \\sim C22B \\sim C23A
\\sim C23B \\sim C24A \\sim C24B \\sim C25A \\sim C25B \\sim C26A \\sim C26B
\\sim C27A \\sim C27B \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim C30A
\\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A
\\sim C9A \\sim C10A \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B \\sim
C18B \\sim C19B \\sim C20B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B \\sim
C18B \\sim C19B \\sim C20B \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim
C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C13, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B, C31, C32, C33, C34,
  C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C1A, C2A, C3A, C4A, C5A,
 C6A, C7A, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C13, C21A, C21B, C22A,
 C22B, C23A, C23B, C24A, C24B, C25A, C25B, C26A, C26B, C27A, C27B, C28A, C28B,
 C29A, C29B, C30A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C31, C32,
 C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B, C11A, C12A, C13A,
 C14A, C15A, C16A, C17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Ir1A(0.8) Ir1B(0.2) Ir2A(0.8) Ir3B(0.2) C1B(0.2) C2B(0.2) C3B(0.2)
 C4B(0.2) C5B(0.2) C6B(0.2) H6BA(0.2) H6BB(0.2) H6BC(0.2) C7B(0.2) H7BA(0.2)
 H7BB(0.2) H7BC(0.2) C8B(0.2) H8BA(0.2) H8BB(0.2) H8BC(0.2) C9B(0.2) H9BA(0.2)
 H9BB(0.2) H9BC(0.2) C10B(0.2) H10A(0.2) H10B(0.2) H10C(0.2) C11B(0.8)
 C12B(0.8) C13(0.2) H13A(0.2) H13B(0.2) H13C(0.2) C13B(0.8) C14B(0.8) C15B(0.8)
 C16B(0.8) H16A(0.8) H16B(0.8) H16C(0.8) C17B(0.8) H17A(0.8) H17B(0.8)
 H17C(0.8) C18B(0.8) H18A(0.8) H18B(0.8) H18C(0.8) C19B(0.8) H19A(0.8)
 H19B(0.8) H19C(0.8) C20B(0.8) H20A(0.8) H20B(0.8) H20C(0.8) C21B(0.2)
 C22B(0.2) C23B(0.2) C24B(0.2) C25B(0.2) C26B(0.2) H26D(0.2) H26E(0.2)
 H26F(0.2) C27B(0.2) H27D(0.2) H27E(0.2) H27F(0.2) C28B(0.2) H28D(0.2)
 H28E(0.2) H28F(0.2) C29B(0.2) H29D(0.2) H29E(0.2) H29F(0.2) Ir2B(0.2)
 Ir3A(0.8) C1A(0.8) C2A(0.8) C3A(0.8) C4A(0.8) C5A(0.8) C6A(0.8) H6AA(0.8)
 H6AB(0.8) H6AC(0.8) C7A(0.8) H7AA(0.8) H7AB(0.8) H7AC(0.8) C8A(0.8) H8AA(0.8)
 H8AB(0.8) H8AC(0.8) C9A(0.8) H9AA(0.8) H9AB(0.8) H9AC(0.8) C10A(0.8) H10D(0.8)
 H10E(0.8) H10F(0.8) C11A(0.2) C12A(0.2) C13A(0.2) C14A(0.2) C15A(0.2)
 C16A(0.2) H16D(0.2) H16E(0.2) H16F(0.2) C17A(0.2) H17D(0.2) H17E(0.2)
 H17F(0.2) C18A(0.2) H18D(0.2) H18E(0.2) H18F(0.2) C19A(0.2) H19D(0.2)
 H19E(0.2) H19F(0.2) C20A(0.2) H20D(0.2) H20E(0.2) H20F(0.2) C31(0.8) C32(0.8)
 C33(0.8) C34(0.8) C35(0.8) C36(0.8) H36A(0.8) H36B(0.8) H36C(0.8) C37(0.8)
 H37A(0.8) H37B(0.8) H37C(0.8) C38(0.8) H38A(0.8) H38B(0.8) H38C(0.8) C39(0.8)
 H39A(0.8) H39B(0.8) H39C(0.8) C40(0.8) H40A(0.8) H40B(0.8) H40C(0.8)
 Fixed X: Ir1A(0.483191) Ir1B(0.509763) Ir2A(0.272657) Ir3B(0.181426)
 Ir4(0.238214) Nb1(0.303988) C1B(0.664062) C2B(0.607606) C3B(0.58869)
 C4B(0.631337) C5B(0.677505) C6B(0.706244) C7B(0.578226) C8B(0.536088)
 C9B(0.626584) C10B(0.733394) C11B(0.184862) C12B(0.238995) C13(0.259933)
 C13B(0.192794) C14B(0.110086) C15B(0.103675) C16B(0.203909) C17B(0.325728)
 C18B(0.219905) C19B(0.03966) C20B(0.017268) C21A(0.179605) C21B(0.154831)
 C22A(0.275105) C22B(0.053022) C23A(0.35479) C23B(0.000587) C24A(0.303288)
 C24B(0.070189) C25A(0.197641) C25B(0.165774) C26A(0.071692) C26B(0.236814)
 C27A(0.296594) C27B(0.005979) C28A(0.472459) C28B(-0.111753) C29A(0.356965)
 C29B(0.044644) C30A(0.116893) Ir2B(0.234046) Ir3A(0.141274) C1A(0.615892)
 C2A(0.565825) C3A(0.568007) C4A(0.627978) C5A(0.656305) C6A(0.624875)
 C7A(0.526355) C8A(0.523634) C9A(0.653872) C10A(0.721334) C11A(0.185723)
 C12A(0.109021) C13A(0.123919) C14A(0.218753) C15A(0.258931) C16A(0.188498)
 C17A(0.006021) C18A(0.050446) C19A(0.265218) C20A(0.351974) C31(-0.009254)
 C32(-0.008032) C33(0.091216) C34(0.149394) C35(0.087399) C36(-0.0968) C37(-
 0.096753) C38(0.123487) C39(0.249104) C40(0.109277)
 Fixed Y: Ir1A(0.585385) Ir1B(0.599422) Ir2A(0.658696) Ir3B(0.600553)
 Ir4(0.706264) Nb1(0.634068) C1B(0.612103) C2B(0.579681) C3B(0.528798)
 C4B(0.53021) C5B(0.581805) C6B(0.668428) C7B(0.59411) C8B(0.480081)
 C9B(0.484393) C10B(0.600266) C11B(0.73243) C12B(0.712328) C13(0.478786)
 C13B(0.66133) C14B(0.650596) C15B(0.695053) C16B(0.786413) C17B(0.739921)
 C18B(0.626054) C19B(0.600986) C20B(0.702847) C21A(0.759151) C21B(0.54008)
 C22A(0.72973) C22B(0.565002) C23A(0.749745) C23B(0.552171) C24A(0.786801)
 C24B(0.519622) C25A(0.792974) C25B(0.512339) C26A(0.752165) C26B(0.541853)
 C27A(0.69383) C27B(0.598125) C28A(0.73744) C28B(0.567918) C29A(0.822155)
 C29B(0.496415) C30A(0.831581) Ir2B(0.628551) Ir3A(0.598927) C1A(0.574031)
 C2A(0.523089) C3A(0.505794) C4A(0.544435) C5A(0.586226) C6A(0.601219)
 C7A(0.486817) C8A(0.453403) C9A(0.538607) C10A(0.634315) C11A(0.644545)
 C12A(0.64889) C13A(0.700063) C14A(0.72353) C15A(0.688231) C16A(0.601238)
 C17A(0.617051) C18A(0.726171) C19A(0.77695) C20A(0.699484) C31(0.568192)
 C32(0.542933) C33(0.516026) C34(0.522964) C35(0.557262) C36(0.604347)
 C37(0.539419) C38(0.478541) C39(0.492685) C40(0.572924)
 Fixed Z: Ir1A(0.300051) Ir1B(0.297399) Ir2A(0.499945) Ir3B(0.176282)
 Ir4(0.199203) Nb1(0.314807) C1B(0.266397) C2B(0.189027) C3B(0.229115)
 C4B(0.331461) C5B(0.354764) C6B(0.258337) C7B(0.08151) C8B(0.17508)
 C9B(0.401834) C10B(0.455242) C11B(0.523079) C12B(0.616003) C13(0.21406)
 C13B(0.630744) C14B(0.548051) C15B(0.482051) C16B(0.478683) C17B(0.689728)
 C18B(0.721484) C19B(0.531751) C20B(0.391644) C21A(0.057278) C21B(0.073174)
 C22A(0.052773) C22B(0.05287) C23A(0.133524) C23B(0.130733) C24A(0.188272)
 C24B(0.199311) C25A(0.13693) C25B(0.164046) C26A(-0.015015) C26B(0.008423)
 C27A(-0.026258) C27B(-0.037035) C28A(0.152656) C28B(0.137802) C29A(0.269245)
 C29B(0.292747) C30A(0.165174) Ir2B(0.476861) Ir3A(0.208921) C1A(0.223536)
 C2A(0.223425) C3A(0.320971) C4A(0.383738) C5A(0.323977) C6A(0.128551)
 C7A(0.137004) C8A(0.351068) C9A(0.49404) C10A(0.366685) C11A(0.619553)
 C12A(0.530107) C13A(0.487577) C14A(0.54292) C15A(0.622869) C16A(0.697052)
 C17A(0.507154) C18A(0.401278) C19A(0.519044) C20A(0.706326) C31(0.089581)
 C32(0.180886) C33(0.206482) C34(0.130527) C35(0.059024) C36(0.034981)
 C37(0.238107) C38(0.29365) C39(0.120337) C40(-0.040491)
;
_shelx_res_checksum              21181
_shelx_hkl_checksum              21123
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD473
_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 2.742
_oxdiff_exptl_absorpt_empirical_full_min 0.495