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_1576961
_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         'C32 H32 Ir N7, C H2 Cl2, Cl'
_chemical_formula_sum            'C33 H34 Cl3 Ir N7'
_chemical_formula_weight         827.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-03
_audit_creation_method
; 
Olex2 1.5 
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) 
;
_audit_update_record
;
2025-12-23 deposited with the CCDC.	2026-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1935(12)
_cell_length_b                   30.004(2)
_cell_length_c                   12.5245(8)
_cell_measurement_reflns_used    6357
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.24
_cell_volume                     6836.8(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0830
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47306
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         1.762
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.174
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0670 before and 0.0399 after correction. 
The Ratio of minimum to maximum transmission is 0.7371. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.145
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7882
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+41.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5022
_reflns_number_total             7882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00822d2.cif
_cod_data_source_block           ppz-dmp-Me
_cod_depositor_comments
'Adding full bibliography for 1576959--1576965.cif.'
_cod_original_cell_volume        6836.9(8)
_cod_original_sg_symbol_H-M      Pnna
_cod_database_code               1576961
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.731
_shelx_estimated_absorpt_t_min   0.349
_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. Rigid bond restraints 
 All non-hydrogen atoms 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 
3. Uiso/Uaniso restraints and constraints 
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma 
for terminal atoms of 0.08 within 2A 
4. Others 
 Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1) 
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C1S(H1SA,H1SB) 
5.b Aromatic/amide H refined with riding coordinates: 
 N1(H1), C5(H5), C14(H14), C15(H15), C11(H11), C11(H11A), C12(H12), C12A(H12A), 
  C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), 
 C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49) 
5.c Idealised Me refined as rotating group: 
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C31(H31A,H31B,H31C), C13(H13A,H13B, 
 H13C), C13A(H13D,H13E,H13F) 
;
_shelx_res_checksum              12386
_olex2_submission_special_instructions 'No special instructions were received'