Tridentate κ<sup>3</sup>-<i>P</i>,<i>P</i>,<i>C</i> iridium complexes: influence of ligand saturation on intramolecular C-H bond activation.
Demchuk, Mitchell J.; Zurakowski, Joseph A.; Drover, Marcus W.; Chemical communications (Cambridge, England) 60 (2024) 7566–7569; doi:10.1039/d4cc01435a

data_7133173
_publ_section_title
;
 Tridentate &#x3ba;<sup>3</sup>-<i>P</i>,<i>P</i>,<i>C</i> iridium
 complexes: influence of ligand saturation on intramolecular C-H bond
 activation.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7566
_journal_page_last               7569
_journal_paper_doi               10.1039/d4cc01435a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C25 H47 Ir P2'
_chemical_formula_sum            'C25 H47 Ir P2'
_chemical_formula_weight         601.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2024-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.0014(3)
_cell_length_b                   17.1635(5)
_cell_length_c                   28.5541(9)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.46
_cell_volume                     4901.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            90741
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_min         2.373
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.588
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0990 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.6338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.000103(17)
_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   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         6082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0076P)^2^+10.6565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5609
_reflns_number_total             6082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01435a3.cif
_cod_data_source_block           final11
_cod_depositor_comments
'Adding full bibliography for 7133173--7133175.cif.'
_cod_database_code               7133173
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.488
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C22(H22), C23(H23), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C24(H24A,H24B), C20(H20A,H20B),
 C25(H25A,H25B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              61657
_shelx_hkl_checksum              19504
_olex2_submission_special_instructions 'No special instructions were received'