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_7133174
_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      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             2023-10-31
_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                 109.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.405(9)
_cell_length_b                   18.494(13)
_cell_length_c                   13.748(10)
_cell_measurement_reflns_used    2511
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      19.90
_cell_measurement_theta_min      3.08
_cell_volume                     2494(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      110.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.1374
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46093
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.715
_diffrn_reflns_theta_min         1.919
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.492
_exptl_absorpt_correction_T_max  0.7897
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.7765.
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    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.3019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3531
_reflns_number_total             4738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01435a3.cif
_cod_data_source_block           b24061_0m
_cod_depositor_comments
'Adding full bibliography for 7133173--7133175.cif.'
_cod_database_code               7133174
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.604
_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:
 C10(H10), C6(H6), C5(H5), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C8(H8A,H8B), C12(H12A,H12B), C7(H7A,H7B), C3(H3A,H3B), C9(H9A,
 H9B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C15(H15B,
 H15A,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              3483
_shelx_hkl_checksum              99437
_olex2_submission_special_instructions 'No special instructions were received'