Two near-infrared phosphorescent iridium(III) complexes for detection of GSH and photodynamic therapy
Tu, Rui; Liu, Jie; Chen, Weibin; Fu, Fengfu; Li, Mei-Jin; Dalton Transactions  (2023) –; doi:10.1039/D3DT01826A

data_7713761
_publ_section_title
;
 Two near-infrared phosphorescent iridium(III) complexes for detection of
 GSH and photodynamic therapy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01826A
_journal_year                    2023
_chemical_formula_moiety
'0.103(C52 Ir N4 O2 S2), 0.308(C Cl2), 0.103(F6 P), 0.103(N), 0.127[CH2Cl2]'
_chemical_formula_sum            'C55 H42 Cl6 F6 Ir N4 O2 P S2'
_chemical_formula_weight         1404.91
_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             2023-06-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-12 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.576(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3845(9)
_cell_length_b                   36.264(3)
_cell_length_c                   13.5902(9)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.25
_cell_volume                     5998.8(8)
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            86692
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.077
_diffrn_reflns_theta_max         25.077
_diffrn_reflns_theta_min         1.994
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5210
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.065
_refine_diff_density_min         -2.959
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         10610
_refine_ls_number_restraints     1294
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0304P)^2^+146.9410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8408
_reflns_number_total             10610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01826a2.cif
_cod_data_source_block           '[Ir(iqbt)2bpy-ace]PF6'
_cod_original_cell_volume        5998.7(7)
_cod_database_code               7713761
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Restrained distances
 P1-F3B \\sim P1-F3A
 with sigma of 0.02
 Cl1A-C53 \\sim Cl1B-C53
 with sigma of 0.02
 P1-F1B \\sim P1-F2
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F3B \\sim F3A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Cl1A \\sim Cl1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C25: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C25 \\sim C28 \\sim C11 \\sim C36 \\sim C27 \\sim C13 \\sim C6 \\sim C3 \\sim
C48 \\sim C5 \\sim C10 \\sim C9 \\sim C24 \\sim C12 \\sim C35 \\sim C18 \\sim
C29 \\sim C8 \\sim C30 \\sim C39 \\sim C46 \\sim C26 \\sim C47 \\sim C7 \\sim
C37 \\sim C50 \\sim C44 \\sim C1 \\sim C17 \\sim C38 \\sim C20 \\sim C2 \\sim
C23 \\sim C14 \\sim C31 \\sim C4 \\sim C51 \\sim C34 \\sim C15 \\sim C45 \\sim
C16 \\sim C40 \\sim C19 \\sim C33 \\sim C32 \\sim C49 \\sim C21 \\sim C22 \\sim
C42 \\sim C41 \\sim C43 \\sim C52 \\sim C53 \\sim C55 \\sim C54: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 F3A, P1, F4, F2, F6, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F3B, P1, F6, F2, F4, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Cl1B, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Cl1A, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F1B, P1, F1A, F6, F5, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F2, F1A, P1, F6, F5, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F3A)=1-FVAR(1)
 Sof(F3B)=FVAR(1)
 Sof(H53C)=Sof(H53D)=Sof(Cl1A)=1-FVAR(2)
 Sof(Cl1B)=Sof(H53A)=Sof(H53B)=FVAR(2)
 Sof(F2)=1-FVAR(3)
 Sof(F1B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C53(H53C,H53D), C55(H55A,H55B), C54(H54A,H54B)
5.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C13(H13), C6(H6), C5(H5), C24(H24), C35(H35), C18(H18), C30(H30),
 C47(H47), C7(H7), C50(H50), C44(H44), C1(H1), C38(H38), C2(H2), C23(H23),
 C14(H14), C31(H31), C4(H4), C15(H15), C45(H45), C16(H16), C40(H40), C19(H19),
 C33(H33), C32(H32), C49(H49), C21(H21), C22(H22), C41(H41)
5.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C52(H52A,H52B,H52C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 210 electrons were 
found in a volume of 790\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.13[CH2Cl2] per Asymmetric Unit 
which account for 213 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44570
_shelx_fab_checksum              20437
_olex2_submission_special_instructions 'No special instructions were received'