Rhodamine-functionalised rhodium(iii) complexes: dual role as bioimaging agents and controllable reactive oxygen species photosensitisers for photocytotoxicity applications.
Jiang, Katherine Gui-Min; Wei, Fangfang; Leung, Peter Kam-Keung; Wu, Siye; Lo, Kenneth Kam-Wing; Wong, Keith Man-Chung; Chemical science 16 (2025) 22127–22135; doi:10.1039/d5sc05257b

data_1576049
_publ_section_title
;
 Rhodamine-functionalised rhodium(iii) complexes: dual role as bioimaging
 agents and controllable reactive oxygen species photosensitisers for
 photocytotoxicity applications.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              22127
_journal_page_last               22135
_journal_paper_doi               10.1039/d5sc05257b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'2(C52 H34 N6 Rh S4), 2(F6 P), 4(C H2 Cl2), C Cl2'
_chemical_formula_sum            'C109 H76 Cl10 F12 N12 P2 Rh2 S8'
_chemical_formula_weight         2660.55
_chemical_name_systematic        '[Rh(dtbq)2Me2-bpy](PF6)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2m8kxd
_audit_creation_date             2025-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-02-16 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                82.958(2)
_cell_angle_beta                 86.247(3)
_cell_angle_gamma                74.635(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9995(5)
_cell_length_b                   13.8501(5)
_cell_length_c                   16.0709(6)
_cell_measurement_reflns_used    9460
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.31
_cell_measurement_theta_min      2.77
_cell_volume                     2767.36(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.17
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35167
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.370
_diffrn_reflns_theta_max         65.370
_diffrn_reflns_theta_min         2.772
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.953
_exptl_absorpt_correction_T_max  0.3165
_exptl_absorpt_correction_T_min  0.1463
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1090 before and 0.0708 after correction. The Ratio of minimum to maximum transmission is 0.4622. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0657P)^2^+7.6196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7678
_reflns_number_total             9424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05257b2.cif
_cod_data_source_block           rh-dtbq-dimebpy
_cod_depositor_comments
'Adding full bibliography for 1576047--1576050.cif.'
_cod_database_code               1576049
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.384
_shelx_estimated_absorpt_t_min   0.323
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{S4, C38A}
{S4A, C38}
3. Uiso/Uaniso restraints and constraints
Uanis(Cl4A) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S4) = Uanis(C38A)
Uanis(S4A) = Uanis(C38)
4. Others
 Sof(F6A)=1-FVAR(1)
 Sof(F6)=FVAR(1)
 Fixed Sof: S4(0.6) S4A(0.4) H39A(0.4) H39(0.6) H40(0.6) H40A(0.4) H53A(0.5)
 H53B(0.5) H53C(0.5) H53D(0.5) H54C(0.4) H54D(0.4) H54A(0.6) H54B(0.6) C55(0.5)
 Cl2(0.5) Cl2A(0.5) Cl4A(0.4) Cl4(0.6) C38A(0.4) H38A(0.4) C38(0.6) H38(0.6)
5.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C53(H53C,H53D), C54(H54C,H54D), C54(H54A,H54B)
5.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C34(H34), C27(H27), C50(H50), C7(H7), C2(H2), C3(H3), C42(H42),
 C14(H14), C32(H32), C41(H41), C22(H22), C30(H30), C9(H9), C44(H44), C18(H18),
 C31(H31), C29(H29), C49(H49), C10(H10), C39(H39A), C39(H39), C40(H40),
 C40(H40A), C23(H23), C19(H19), C12(H12), C11(H11), C20(H20), C38A(H38A),
 C38(H38)
5.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              90932
_olex2_submission_special_instructions 'No special instructions were received'