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_1542300
_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         'C41 H40 Ir N6 S2, C F3 O3 S'
_chemical_formula_sum            'C42 H40 F3 Ir N6 O3 S3'
_chemical_formula_weight         1022.18
_chemical_name_systematic        '[(Hbta)2Ir(dib)]OTf'
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jyfxt
_audit_creation_date             2015-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4973)
;
_audit_update_record
;
2015-09-29 deposited with the CCDC.
2016-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3460(5)
_cell_length_b                   19.6302(7)
_cell_length_c                   30.1437(11)
_cell_measurement_reflns_used    9264
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.09
_cell_measurement_theta_min      2.93
_cell_volume                     7897.2(5)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            144642
_diffrn_reflns_theta_full        67.61
_diffrn_reflns_theta_max         67.61
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.566
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/Et2O'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+12.7141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                7011
_reflns_number_total             7057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04458h2.cif
_cod_data_source_block           david60_0m-pbca
_cod_depositor_comments
'Adding full bibliography for 1542299--1542302.cif.'
_cod_database_code               1542300
_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:
 C39(H39A,H39B), C38(H38A,H38B), C40(H40A,H40B), C30(H30A,H30B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C28(H28), C22(H22), C15(H15), C16(H16), C17(H17), C5(H5), C2(H2),
 C33(H33), C9(H9), C12(H12), C10(H10), C29(H29), C3(H3), C32(H32), C11(H11),
 C24(H24), C23(H23), C4(H4), C18(H18)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C37(H37A,H37B,H37C)
;
_olex2_date_sample_data_collection 23/05/2014
_olex2_date_sample_submission    13/05/2014
_olex2_submission_special_instructions 'No special instructions were received'