Mechanistic investigations via DFT support the cooperative heterobimetallic C-H and O-H bond activation across Ta[double bond, length as m-dash]Ir multiple bonds.
Del Rosal, Iker; Lassalle, Sébastien; Dinoi, Chiara; Thieuleux, Chloé; Maron, Laurent; Camp, Clément; Dalton transactions (Cambridge, England : 2003) 50 (2021) 504–510; doi:10.1039/d0dt03818k

data_7706453
_publ_section_title
;
 Mechanistic investigations via DFT support the cooperative
 heterobimetallic C-H and O-H bond activation across Ta[double bond,
 length as m-dash]Ir multiple bonds.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              504
_journal_page_last               510
_journal_paper_doi               10.1039/d0dt03818k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C42 H51 Ir O4 Ta, C7 H8'
_chemical_formula_sum            'C49 H59 Ir O4 Ta'
_chemical_formula_weight         1085.11
_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             2019-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.14450(10)
_cell_length_b                   21.29120(10)
_cell_length_c                   18.95870(10)
_cell_measurement_reflns_used    30605
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3180
_cell_measurement_theta_min      3.7810
_cell_volume                     4419.79(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9897
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_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    -20.00  25.00   1.00   10.00    --  -14.17 -99.00  90.00   45
  2  \w    -13.00  88.00   1.00   10.00    --   16.83  19.00-180.00  101
  3  \w      0.00  84.00   1.00   10.00    --   16.83  57.00-120.00   84
  4  \w    -33.00  55.00   1.00   10.00    --  -14.17  38.00-120.00   88
  5  \w    -87.00 -34.00   1.00   10.00    --  -14.17 178.00 -60.00   53
  6  \w      0.00  84.00   1.00   10.00    --   16.83  57.00 -30.00   84
  7  \w    -20.00  27.00   1.00   10.00    --   16.83 -99.00   0.00   47
  8  \w    -20.00  56.00   1.00   10.00    --   16.83 -99.00 150.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0634465000
_diffrn_orient_matrix_UB_12      0.0060009000
_diffrn_orient_matrix_UB_13      -0.0103984000
_diffrn_orient_matrix_UB_21      -0.0012223000
_diffrn_orient_matrix_UB_22      0.0124136000
_diffrn_orient_matrix_UB_23      0.0345746000
_diffrn_orient_matrix_UB_31      0.0130705000
_diffrn_orient_matrix_UB_32      0.0303246000
_diffrn_orient_matrix_UB_33      -0.0120915000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60033
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.723
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.523
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       plate
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.047
_refine_diff_density_max         2.144
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         11121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+10.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9897
_reflns_number_total             11121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03818k2.cif
_cod_data_source_block           pc37
_cod_database_code               7706453
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C49 H60 Ir1 O4 Ta1'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C21(H21), C13(H13), C4(H4), C11(H11), C3(H3), C19(H19), C12(H12),
 C29(H29), C20(H20), C27(H27), C28(H28), C47(H47), C44(H44), C46(H46), C45(H45),
  C48(H48)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C31(H31A,H31B,
 H31C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C42(H42A,
 H42B,H42C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C32(H32A,H32B,H32C),
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              28711
_olex2_date_sample_data_collection 2019-04-30
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id PC37
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.695