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_7712198
_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         'C52 H49 Ir P4'
_chemical_formula_sum            'C52 H49 Ir P4'
_chemical_formula_weight         989.99
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7143(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.09632(17)
_cell_length_b                   20.7085(4)
_cell_length_c                   20.9765(3)
_cell_measurement_reflns_used    9199
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.9900
_cell_measurement_theta_min      4.7150
_cell_volume                     4385.42(13)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -1.00  42.00   1.00    1.00    --    0.00  77.00-180.00   43
  2  \w    -16.00  23.00   1.00    1.00    --    0.00 -77.00-120.00   39
  3  \w    -20.00  27.00   1.00    1.00    --    0.00 -77.00-180.00   47
  4  \w     42.00 105.00   1.00    1.50    --   54.00  57.00-150.00   63
  5  \w     37.00 110.00   1.00    1.50    --   54.00-125.00-180.00   73
  6  \w    -17.00  98.00   1.00    1.50    --   54.00 -19.00  30.00  115
  7  \w     68.00  93.00   1.00    1.50    --   54.00  57.00-180.00   25
  8  \w     64.00 146.00   1.00    1.50    --  108.00 178.00-150.00   82
  9  \w     37.00  64.00   1.00    1.50    --  108.00 -91.00  90.00   27
 10  \w     35.00  68.00   1.00    1.50    --  108.00 -25.00 -90.00   33
 11  \w     52.00 121.00   1.00    1.50    --  108.00 -63.00 -60.00   69
 12  \w     91.00 121.00   1.00    1.50    --  108.00  50.00 -90.00   30
 13  \w     82.00 178.00   1.00    1.50    --  108.00  38.00  90.00   96
 14  \w     90.00 176.00   1.00    1.50    --  108.00  25.00  30.00   86
 15  \w     85.00 129.00   1.00    1.50    --  108.00 -25.00 -90.00   44
 16  \w     84.00 109.00   1.00    1.50    --  108.00-111.00-180.00   25
;
_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      -0.1391041000
_diffrn_orient_matrix_UB_12      -0.0029920000
_diffrn_orient_matrix_UB_13      0.0291090000
_diffrn_orient_matrix_UB_21      -0.0591540000
_diffrn_orient_matrix_UB_22      -0.0179744000
_diffrn_orient_matrix_UB_23      -0.0657168000
_diffrn_orient_matrix_UB_31      0.0204439000
_diffrn_orient_matrix_UB_32      -0.0721351000
_diffrn_orient_matrix_UB_33      0.0152273000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15880
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         4.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.536
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.458
_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 orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             1992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran and toluene'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.2014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6644
_reflns_number_total             7820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04036k2.cif
_cod_data_source_block           sbd21001
_cod_depositor_comments
'Adding full bibliography for 7712198--7712199.cif.'
_cod_original_cell_volume        4385.44(13)
_cod_database_code               7712198
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H49 Ir1 P4'
_chemical_oxdiff_usercomment     'Paven Kisten [Ir(h)4(dppe)]-K+'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_shelx_res_checksum              18664
_olex2_date_sample_data_collection 2021-06-18
_olex2_date_sample_submission    2021-06-16
_olex2_exptl_crystal_mounting_method 'oil on 100 micrometre micromount'
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.799