Synergistic C-H bond activation across molybdenum-iridium multiply bonded complexes: a cascade of transformations.
Dubrawski, Zachary; Del Rosal, Iker; Jeanneau, Erwann; Maron, Laurent; Thieuleux, Chloé; Camp, Clément; Chemical science 16 (2025) 14564–14577; doi:10.1039/d5sc03465e

data_1575156
_publ_section_title
;
 Synergistic C-H bond activation across molybdenum-iridium multiply bonded
 complexes: a cascade of transformations.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              14564
_journal_page_last               14577
_journal_paper_doi               10.1039/d5sc03465e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C21 H42 Ir Mo N4 O'
_chemical_formula_sum            'C21 H42 Ir Mo N4 O'
_chemical_formula_weight         654.72
_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
_audit_creation_date             2024-09-03
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                100.1480(10)
_cell_angle_beta                 101.6170(10)
_cell_angle_gamma                98.0710(10)
_cell_formula_units_Z            4
_cell_length_a                   10.5680(2)
_cell_length_b                   14.3581(2)
_cell_length_c                   17.6451(2)
_cell_measurement_reflns_used    71454
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.7220
_cell_measurement_theta_min      2.5530
_cell_volume                     2538.22(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_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(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.868
_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     -3.00  70.00   0.50    1.73    --   -2.17  45.00 164.00  146
  2  \w    -75.00  -1.00   0.50    1.73    --   -2.17 -45.00  14.00  148
  3  \w    -59.00   2.00   0.50    1.73    --   -2.17 -57.00-120.00  122
  4  \w    -59.00   2.00   0.50    1.73    --   -2.17 -57.00  60.00  122
  5  \w    -59.00   2.00   0.50    1.73    --   -2.17 -57.00 -30.00  122
  6  \w    -59.00   2.00   0.50    1.73    --   -2.17 -57.00 150.00  122
  7  \w    -70.00 -40.00   0.50    1.73    --    2.64 -19.00 -30.00   60
  8  \w    -70.00 -40.00   0.50    1.73    --    2.64 -19.00  60.00   60
  9  \w    -70.00 -40.00   0.50    1.73    --    2.64 -19.00 -90.00   60
 10  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00 -90.00  146
 11  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00 120.00  146
 12  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00  30.00  146
 13  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00 -30.00  146
 14  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00-180.00  146
 15  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00  90.00  146
 16  \w    -70.00 -40.00   0.50    1.73    --    2.64 -19.00  90.00   60
 17  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00 -60.00  146
 18  \w     -3.00  28.00   0.50    1.73    --   -2.17  19.00   0.00   62
 19  \w     -3.00  70.00   0.50    1.73    --   -2.17  19.00-120.00  146
;
_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      -0.0549863000
_diffrn_orient_matrix_UB_12      -0.0347906000
_diffrn_orient_matrix_UB_13      -0.0003623000
_diffrn_orient_matrix_UB_21      0.0239368000
_diffrn_orient_matrix_UB_22      -0.0354715000
_diffrn_orient_matrix_UB_23      -0.0237828000
_diffrn_orient_matrix_UB_31      0.0355013000
_diffrn_orient_matrix_UB_32      -0.0116909000
_diffrn_orient_matrix_UB_33      0.0345943000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112854
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.731
_diffrn_reflns_theta_min         2.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
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    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.219
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         13733
_refine_ls_number_restraints     2607
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+9.3522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12780
_reflns_number_total             13733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03465e2.cif
_cod_data_source_block           ov_zd234_auto
_cod_depositor_comments
'Adding full bibliography for 1575153--1575159.cif.'
_cod_database_code               1575156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Mo Ir '
_shelx_estimated_absorpt_t_max   0.366
_shelx_estimated_absorpt_t_min   0.186
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5B-C23B = N5B-C22B
 1.4 with sigma of 0.01
 C22B-C23B
 2.42 with sigma of 0.01
 C24B-C22B
 2.44 with sigma of 0.01
 Ir2A-Mo2A \\sim Ir2B-Mo2B
 with sigma of 0.02
 Mo2A-N7A \\sim Mo2B-N7B
 with sigma of 0.02
 Mo2A-N8A \\sim Mo2B-N8B
 with sigma of 0.02
 Mo2A-N5A \\sim Mo2B-N5B
 with sigma of 0.02
 Mo2A-N6A \\sim Mo2B-N6B
 with sigma of 0.02
 N7A-C30A \\sim N7B-C30B
 with sigma of 0.02
 N7A-C29A \\sim N7B-C29B
 with sigma of 0.02
 N8A-C31A \\sim N8B-C31B
 with sigma of 0.02
 N8A-C32A \\sim N8B-C32B
 with sigma of 0.02
 C33A-C38A \\sim C37B-C42B
 with sigma of 0.02
 N5A-C24A \\sim N5B-C24B
 with sigma of 0.02
 N5A-C22A \\sim N5B-C22B
 with sigma of 0.02
 N5A-C23A \\sim N5B-C23B
 with sigma of 0.02
 N6A-C25A \\sim N6B-C25B
 with sigma of 0.02
 N6A-C24A \\sim N6B-C24B
 with sigma of 0.02
 C36A-C41A \\sim C35B-C40B
 with sigma of 0.02
 C35A-C40A \\sim C34B-C39B
 with sigma of 0.02
 C34A-C39A \\sim C33B-C38B
 with sigma of 0.02
 C42A-C37A \\sim C41B-C36B
 with sigma of 0.02
 C25A-C27A \\sim C25B-C27B
 with sigma of 0.02
 C25A-C28A \\sim C25B-C26B
 with sigma of 0.02
 C25A-C26A \\sim C25B-C28B
 with sigma of 0.02
 O2A-C24A \\sim O2B-C24B
 with sigma of 0.02
 Ir2A-N7A \\sim Ir2B-N7B
 with sigma of 0.04
 Ir2A-N8A \\sim Ir2B-N8B
 with sigma of 0.04
 Ir2A-C33A \\sim Ir2B-C37B
 with sigma of 0.04
 Ir2A-N5A \\sim Ir2B-N5B
 with sigma of 0.04
 Ir2A-N6A \\sim Ir2B-N6B
 with sigma of 0.04
 Ir2A-C36A \\sim Ir2B-C35B
 with sigma of 0.04
 Ir2A-C35A \\sim Ir2B-C34B
 with sigma of 0.04
 Ir2A-C34A \\sim Ir2B-C33B
 with sigma of 0.04
 Ir2A-C42A \\sim Ir2B-C41B
 with sigma of 0.04
 Ir2A-C38A \\sim Ir2B-C42B
 with sigma of 0.04
 Ir2A-C40A \\sim Ir2B-C39B
 with sigma of 0.04
 Ir2A-C37A \\sim Ir2B-C36B
 with sigma of 0.04
 Ir2A-C39A \\sim Ir2B-C38B
 with sigma of 0.04
 Ir2A-C41A \\sim Ir2B-C40B
 with sigma of 0.04
 Mo2A-C33A \\sim Mo2B-C37B
 with sigma of 0.04
 Mo2A-C36A \\sim Mo2B-C35B
 with sigma of 0.04
 Mo2A-C35A \\sim Mo2B-C34B
 with sigma of 0.04
 Mo2A-C34A \\sim Mo2B-C33B
 with sigma of 0.04
 Mo2A-C30A \\sim Mo2B-C30B
 with sigma of 0.04
 Mo2A-C25A \\sim Mo2B-C25B
 with sigma of 0.04
 Mo2A-C37A \\sim Mo2B-C36B
 with sigma of 0.04
 Mo2A-C29A \\sim Mo2B-C29B
 with sigma of 0.04
 Mo2A-C31A \\sim Mo2B-C31B
 with sigma of 0.04
 Mo2A-C24A \\sim Mo2B-C24B
 with sigma of 0.04
 Mo2A-C32A \\sim Mo2B-C32B
 with sigma of 0.04
 Mo2A-C22A \\sim Mo2B-C22B
 with sigma of 0.04
 Mo2A-C23A \\sim Mo2B-C23B
 with sigma of 0.04
 N7A-N8A \\sim N7B-N8B
 with sigma of 0.04
 N7A-N5A \\sim N7B-N5B
 with sigma of 0.04
 N7A-N6A \\sim N7B-N6B
 with sigma of 0.04
 N8A-N5A \\sim N8B-N5B
 with sigma of 0.04
 N8A-N6A \\sim N8B-N6B
 with sigma of 0.04
 C33A-C36A \\sim C37B-C35B
 with sigma of 0.04
 C33A-C35A \\sim C37B-C34B
 with sigma of 0.04
 C33A-C34A \\sim C37B-C33B
 with sigma of 0.04
 C33A-C42A \\sim C37B-C41B
 with sigma of 0.04
 C33A-C37A \\sim C37B-C36B
 with sigma of 0.04
 C33A-C39A \\sim C37B-C38B
 with sigma of 0.04
 N5A-N6A \\sim N5B-N6B
 with sigma of 0.04
 N5A-O2A \\sim N5B-O2B
 with sigma of 0.04
 N6A-C27A \\sim N6B-C27B
 with sigma of 0.04
 N6A-O2A \\sim N6B-O2B
 with sigma of 0.04
 N6A-C28A \\sim N6B-C26B
 with sigma of 0.04
 N6A-C26A \\sim N6B-C28B
 with sigma of 0.04
 C36A-C35A \\sim C35B-C34B
 with sigma of 0.04
 C36A-C34A \\sim C35B-C33B
 with sigma of 0.04
 C36A-C42A \\sim C35B-C41B
 with sigma of 0.04
 C36A-C40A \\sim C35B-C39B
 with sigma of 0.04
 C36A-C37A \\sim C35B-C36B
 with sigma of 0.04
 C35A-C34A \\sim C34B-C33B
 with sigma of 0.04
 C35A-C37A \\sim C34B-C36B
 with sigma of 0.04
 C35A-C39A \\sim C34B-C38B
 with sigma of 0.04
 C35A-C41A \\sim C34B-C40B
 with sigma of 0.04
 C34A-C38A \\sim C33B-C42B
 with sigma of 0.04
 C34A-C40A \\sim C33B-C39B
 with sigma of 0.04
 C34A-C37A \\sim C33B-C36B
 with sigma of 0.04
 C38A-C37A \\sim C42B-C36B
 with sigma of 0.04
 C30A-C29A \\sim C30B-C29B
 with sigma of 0.04
 C25A-C24A \\sim C25B-C24B
 with sigma of 0.04
 C37A-C41A \\sim C36B-C40B
 with sigma of 0.04
 C31A-C32A \\sim C31B-C32B
 with sigma of 0.04
 C27A-C28A \\sim C27B-C26B
 with sigma of 0.04
 C27A-C26A \\sim C27B-C28B
 with sigma of 0.04
 C24A-C22A \\sim C24B-C22B
 with sigma of 0.04
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.04
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.04
 C28A-C26A \\sim C26B-C28B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Ir2A \\sim Mo2A \\sim O2A \\sim N5A \\sim N6A \\sim N7A \\sim N8A \\sim C22A
\\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A
\\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A
\\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A \\sim C42A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Ir2A \\sim Mo2A \\sim O2A \\sim N5A \\sim N6A \\sim N7A \\sim N8A \\sim C22A
\\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A
\\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A
\\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A \\sim C42A \\sim Ir2B
\\sim Mo2B \\sim O2B \\sim N5B \\sim N6B \\sim N7B \\sim N8B \\sim C22B \\sim
C23B \\sim C24B \\sim C25B \\sim C26B \\sim C27B \\sim C28B \\sim C29B \\sim
C30B \\sim C31B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim
C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B \\sim C42B: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Ir2A \\sim Mo2A \\sim O2A \\sim N5A \\sim N6A \\sim N7A \\sim N8A \\sim C22A
\\sim H22A \\sim H22B \\sim H22C \\sim C23A \\sim H23A \\sim H23B \\sim H23C
\\sim C24A \\sim C25A \\sim C26A \\sim H26A \\sim H26B \\sim H26C \\sim C27A
\\sim H27A \\sim H27B \\sim H27C \\sim C28A \\sim H28A \\sim H28B \\sim H28C
\\sim C29A \\sim H29A \\sim H29B \\sim H29C \\sim C30A \\sim H30A \\sim H30B
\\sim H30C \\sim C31A \\sim H31A \\sim H31B \\sim H31C \\sim C32A \\sim H32A
\\sim H32B \\sim H32C \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A
\\sim C38A \\sim H38A \\sim H38B \\sim H38C \\sim C39A \\sim H39A \\sim H39B
\\sim H39C \\sim C40A \\sim H40A \\sim H40B \\sim H40C \\sim C41A \\sim H41A
\\sim H41B \\sim H41C \\sim C42A \\sim H42A \\sim H42B \\sim H42C \\sim Ir2B
\\sim Mo2B \\sim O2B \\sim N5B \\sim N6B \\sim N7B \\sim N8B \\sim C22B \\sim
C23B \\sim C24B \\sim C25B \\sim C26B \\sim H26D \\sim H26E \\sim H26F \\sim
C27B \\sim H27D \\sim H27E \\sim H27F \\sim C28B \\sim H28D \\sim H28E \\sim
H28F \\sim C29B \\sim H29D \\sim H29E \\sim H29F \\sim C30B \\sim H30D \\sim
H30E \\sim H30F \\sim C31B \\sim H31D \\sim H31E \\sim H31F \\sim C32B \\sim
H32D \\sim H32E \\sim H32F \\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim
C37B \\sim C38B \\sim H38D \\sim H38E \\sim H38F \\sim C39B \\sim H39D \\sim
H39E \\sim H39F \\sim C40B \\sim H40D \\sim H40E \\sim H40F \\sim C41B \\sim
H41D \\sim H41E \\sim H41F \\sim C42B \\sim H42D \\sim H42E \\sim H42F: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Ir2A, Mo2A, O2A, N5A, N6A, N7A, N8A, C22A, C23A, C24A, C25A, C26A, C27A, C28A,
  C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C37A, C38A, C39A, C40A, C41A,
 C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Ir2B, Mo2B, O2B, N5B, N6B, N7B, N8B, C22B, C23B, C24B, C25B, C26B, C27B, C28B,
  C29B, C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B, C40B, C41B,
 C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Ir2B)=Sof(Mo2B)=Sof(O2B)=Sof(N5B)=Sof(N6B)=Sof(N7B)=Sof(N8B)=Sof(C22B)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 Sof(C24B)=Sof(C25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(C34B)=Sof(C35B)=Sof(C36B)=Sof(C37B)=
 Sof(C38B)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39B)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41B)=Sof(H41D)=
 Sof(H41E)=Sof(H41F)=Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(Ir2A)=Sof(Mo2A)=Sof(O2A)=Sof(N5A)=Sof(N6A)=Sof(N7A)=Sof(N8A)=Sof(C22A)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27A)=
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(C34A)=Sof(C35A)=Sof(C36A)=Sof(C37A)=
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41A)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C),
 C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,
 H29B,H29C), C30A(H30A,H30B,H30C), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C),
 C38A(H38A,H38B,H38C), C39A(H39A,H39B,H39C), C40A(H40A,H40B,H40C), C41A(H41A,
 H41B,H41C), C42A(H42A,H42B,H42C), C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F),
 C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F), C29B(H29D,
 H29E,H29F), C30B(H30D,H30E,H30F), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F),
 C38B(H38D,H38E,H38F), C39B(H39D,H39E,H39F), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C42B(H42D,H42E,H42F)
;
_shelx_res_checksum              84284
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZD234
_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 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.770