Ir<sup>I</sup>(η<sup>4</sup>-diene) precatalyst activation by strong bases: formation of an anionic Ir<sup>III</sup> tetrahydride.
Kisten, Paven; Manoury, Eric; Lledós, Agustí; Whitwood, Adrian C.; Lynam, Jason M.; Slattery, John M.; Duckett, Simon B.; Poli, Rinaldo; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2495–2505; doi:10.1039/d2dt04036k

data_7712199
_publ_section_title
;
 Ir<sup>I</sup>(&#x3b7;<sup>4</sup>-diene) precatalyst activation by
 strong bases: formation of an anionic Ir<sup>III</sup> tetrahydride.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2495
_journal_page_last               2505
_journal_paper_doi               10.1039/d2dt04036k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C34 H36 Cl Ir P2'
_chemical_formula_sum            'C34 H36 Cl Ir P2'
_chemical_formula_weight         734.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-15
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.11.04 svn.r5db059d7 for OlexSys, GUI svn.r6419)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8366(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0891(2)
_cell_length_b                   10.14941(14)
_cell_length_c                   20.5215(3)
_cell_measurement_reflns_used    6179
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      29.0980
_cell_measurement_theta_min      3.5090
_cell_volume                     2934.18(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (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      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -48.00  57.00   1.00    6.00    --   18.08 -19.00   0.00  105
  2  \w     39.00  92.00   1.00    6.00    --   18.08 178.00-120.00   53
  3  \w    -42.00   2.00   1.00    6.00    --  -18.40 -77.00-150.00   44
  4  \w    -28.00  11.00   1.00    6.00    --  -18.40 -77.00 -30.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0169601000
_diffrn_orient_matrix_UB_12      -0.0632733000
_diffrn_orient_matrix_UB_13      0.0092547000
_diffrn_orient_matrix_UB_21      -0.0456786000
_diffrn_orient_matrix_UB_22      -0.0165504000
_diffrn_orient_matrix_UB_23      0.0115567000
_diffrn_orient_matrix_UB_31      -0.0128172000
_diffrn_orient_matrix_UB_32      -0.0247423000
_diffrn_orient_matrix_UB_33      -0.0311898000
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12585
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.773
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and toluene'
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.181
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+1.6211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5072
_reflns_number_total             5993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04036k2.cif
_cod_data_source_block           sbd21004
_cod_depositor_comments
'Adding full bibliography for 7712198--7712199.cif.'
_cod_original_cell_volume        2934.17(8)
_cod_database_code               7712199
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H36 Cl1 Ir1 P2'
_chemical_oxdiff_usercomment     IrCl(COD)(dppe)]_PK892_111121
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.367
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C21(H21A,H21B), C22(H22A,
 H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              28309
_olex2_date_sample_data_collection 2021-11-15
_olex2_date_sample_submission    2021-11-11
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id '[IrCl(COD)(dppe)]_PK892_111121'
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.801