Base-Promoted, Remote C-H Activation at a Cationic (η<sup>5</sup>-C<sub>5</sub>Me<sub>5</sub>)Ir(III) Center Involving Reversible C-C Bond Formation of Bound C<sub>5</sub>Me<sub>5</sub>.
Moreno, Juan J.; Espada, María F; Campos, Jesús; López-Serrano, Joaquín; Macgregor, Stuart A.; Carmona, Ernesto; Journal of the American Chemical Society 141 (2019) 2205–2210; doi:10.1021/jacs.8b11752

data_4128213
_publ_section_title
;
 Base-Promoted, Remote C-H Activation at a Cationic
 (\h<sup>5</sup>-C<sub>5</sub>Me<sub>5</sub>)Ir(III) Center Involving
 Reversible C-C Bond Formation of Bound C<sub>5</sub>Me<sub>5</sub>.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2205
_journal_page_last               2210
_journal_paper_doi               10.1021/jacs.8b11752
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C42 H57 Ir P, C32 H12 B F24'
_chemical_formula_sum            'C74 H69 B F24 Ir P'
_chemical_formula_weight         1648.27
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5592(10)
_cell_length_b                   20.0983(12)
_cell_length_c                   20.2944(11)
_cell_measurement_reflns_used    9093
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.03
_cell_measurement_theta_min      2.27
_cell_volume                     7059.8(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            120133
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0641 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.8045.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         12750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+8.2671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                11508
_reflns_number_total             12750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b11752_si_004.cif
_cod_data_source_block           mf00915a_0m
_cod_database_code               4128213
_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 Ternary CH refined with riding coordinates:
 C35(H35), C38(H38), C23(H23)
2.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C13(H13), C14(H14), C15(H15), C31(H31), C32(H32),
 C33(H33), C72(H72), C56(H56), C70(H70), C68(H68), C48(H48), C46(H46), C44(H44),
  C54(H54), C52(H52), C60(H60), C62(H62), C64(H64), C19(H19)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C25(H25A,H25B,
 H25C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'