On-complex three-component cascade reactions involving phosphorescent cyclometalated Ir(iii) chloro-isocyanide complexes, nitriles, and propylamine
Phan, Son N. T.; Dang, Vinh Q.; Teets, Thomas S.; Chemical Science  (2026) –; doi:10.1039/D6SC00822D

data_1576963
_publ_section_title
;
 On-complex three-component cascade reactions involving phosphorescent
 cyclometalated Ir(iii) chloro-isocyanide complexes, nitriles, and
 propylamine.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              9591
_journal_page_last               9599
_journal_paper_doi               10.1039/d6sc00822d
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C38 H37 F4 Ir N5, F6 P'
_chemical_formula_sum            'C38 H37 F10 Ir N5 P'
_chemical_formula_weight         976.89
_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
_audit_creation_date             2025-11-14
_audit_creation_method
; 
Olex2 1.5 
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) 
;
_audit_update_record
;
2025-12-24 deposited with the CCDC.	2026-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.924(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3528(17)
_cell_length_b                   20.663(3)
_cell_length_c                   15.486(2)
_cell_measurement_reflns_used    6328
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      3.00
_cell_volume                     3836.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21356
_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         27.394
_diffrn_reflns_theta_min         2.998
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.605
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0716 before and 0.0321 after correction. 
The Ratio of minimum to maximum transmission is 0.7690. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6801
_reflns_number_total             8700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00822d2.cif
_cod_data_source_block           ts37_a
_cod_depositor_comments
'Adding full bibliography for 1576959--1576965.cif.'
_cod_original_cell_volume        3836.7(9)
_cod_database_code               1576963
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups, All N(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Restrained distances 
 N3-H3 
 0.88 with sigma of 0.02 
3.a Secondary CH2 refined with riding coordinates: 
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B) 
3.b Aromatic/amide H refined with riding coordinates: 
 N1(H1), C13(H13), C14(H14), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), 
 C34(H34), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44), C54(H54), C56(H56) 
3.c Idealised Me refined as rotating group: 
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C) 
;
_shelx_res_checksum              16538
_olex2_submission_special_instructions 'No special instructions were received'