Stable luminescent iridium(iii) complexes with bis(N-heterocyclic carbene) ligands: photo-stability, excited state properties, visible-light-driven radical cyclization and CO2reduction, and cellular imaging
Yang, Chen; Mehmood, Faisal; Lam, Tsz Lung; Chan, Sharon Lai-Fung; Wu, Yuan; Yeung, Chi-Shun; Guan, Xiangguo; Li, Kai; Chung, Clive Yik-Sham; Zhou, Cong-Ying; Zou, Taotao; Che, Chi-Ming; Chem. Sci. 7 (2016) 3123–; doi:10.1039/C5SC04458H

data_1542302
_publ_section_title
;
 Stable luminescent iridium(iii) complexes with bis(N-heterocyclic
 carbene) ligands: photo-stability, excited state properties,
 visible-light-driven radical cyclization and CO2reduction, and cellular
 imaging
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3123
_journal_paper_doi               10.1039/C5SC04458H
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C43 H44 Ir N6 S2, C F3 O3 S'
_chemical_formula_sum            'C44 H44 F3 Ir N6 O3 S3'
_chemical_formula_weight         1050.23
_chemical_name_systematic        (lpt)2Ir(dib)OTf
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jyfzw
_audit_creation_date             2015-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2015-09-29 deposited with the CCDC.
2016-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                74.683(2)
_cell_angle_beta                 86.255(2)
_cell_angle_gamma                83.689(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6716(7)
_cell_length_b                   12.4594(8)
_cell_length_c                   14.7489(9)
_cell_measurement_temperature    115
_cell_volume                     2054.6(2)
_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-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      115.04
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43882
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.465
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0903 before and 0.0367 after correction. The Ratio of minimum to maximum transmission is 0.8067. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/Et2O'
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00164(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0123
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+1.8364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0307
_refine_ls_wR_factor_ref         0.0309
_reflns_number_gt                7115
_reflns_number_total             7243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04458h2.cif
_cod_data_source_block           mo_chem0033_0mb
_cod_depositor_comments
'Adding full bibliography for 1542299--1542302.cif.'
_cod_database_code               1542302
_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 Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,
 H40B), C41(H41A,H41B), C42(H42A,H42B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C13(H13), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C26(H26), C27(H27), C30(H30), C31(H31),
  C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C39(H39A,H39B,H39C), C43(H43A,H43B,
 H43C)
;
_olex2_submission_special_instructions 'No special instructions were received'