Terpyridine-based ruthenium complexes containing a 4,5-diazafluoren-9-one ligand with light-driven enhancement of biological activity.
de Alencar, Francisca Mayara Santos; Gouveia, Jr, Florencio Sousa; Oliveira, Geângela de Fátima Sousa de; Andrade, Alexandre Lopes; Vasconcelos, Mayron Alves de; Ayala, Alejandro Pedro; Gondim, Ana Claudia Silva; Carvalho, Idalina Maria Moreira de; Moraes, Carlos André Ferreira; Palmeira-Mello, Marcos V; Batista, Alzir Azevedo; Lopes, Luiz Gonzaga de França; Sousa, Eduardo Henrique Silva; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1850–1870; doi:10.1039/d4dt02562h

data_7717636
_publ_section_title
;
 Terpyridine-based ruthenium complexes containing a 4,5-diazafluoren-9-one
 ligand with light-driven enhancement of biological activity.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1850
_journal_page_last               1870
_journal_paper_doi               10.1039/d4dt02562h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C33 H23 Cl N5 O Ru, F6 P, 0.5[H2O]'
_chemical_formula_sum            'C33 H24 Cl F6 N5 O1.5 P Ru'
_chemical_formula_weight         796.06
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2024-10-13
_audit_creation_method
;FinalCif V143 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2024-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                96.811(9)
_cell_angle_beta                 98.431(8)
_cell_angle_gamma                99.510(8)
_cell_formula_units_Z            2
_cell_length_a                   8.746(2)
_cell_length_b                   13.317(3)
_cell_length_c                   13.892(4)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.114
_cell_measurement_theta_min      2.322
_cell_volume                     1561.5(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'APEX 5 (2024) Bruker AXS Inc., Madison, WI 53719-1173'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'Bruker PHOTON II CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu CPAD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42556
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.322
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.40
_diffrn_source_type              'Incoatec I\ms HB'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1445 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.7059.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull reddish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.981
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         5720
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.1165
_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^)+42.1271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2466
_refine_ls_wR_factor_ref         0.2959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3462
_reflns_number_total             5720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02562h2.cif
_cod_data_source_block           mpd2cl
_cod_depositor_comments
'Adding full bibliography for 7717636--7717637.cif.'
_cod_original_formula_sum        'C33 H24 Cl F6 N5 O1.50 P Ru'
_cod_database_code               7717636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1_1-F1_1 = P1_1-F2_1 = P1_1-F3_1 = P1_1-F4_1 = P1_1-F5_1 = P1_1-F6_1
 P1_2-F1_2 = P1_2-F2_2 = P1_2-F3_2 = P1_2-F4_2 = P1_2-F5_2 = P1_2-F6_2
 1.65 with sigma of 0.02
 C7A-C6A
 1.5 with sigma of 0.02
 C5A-C6A
 1.5 with sigma of 0.02
 P1_1-F1_1 \\sim P1_1-F2_1 \\sim P1_1-F3_1 \\sim P1_1-F4_1 \\sim P1_1-F5_1
\\sim P1_1-F6_1
 P1_2-F1_2 \\sim P1_2-F2_2 \\sim P1_2-F3_2 \\sim P1_2-F4_2 \\sim P1_2-F5_2
\\sim P1_2-F6_2
 with sigma of 0.02
 F1_1-F2_1 \\sim F1_1-F4_1 \\sim F1_1-F5_1 \\sim F1_1-F6_1 \\sim F3_1-F2_1
\\sim F3_1-F4_1 \\sim F3_1-
 F5_1 \\sim F3_1-F6_1
 F1_2-F2_2 \\sim F1_2-F4_2 \\sim F1_2-F5_2 \\sim F1_2-F6_2 \\sim F3_2-F2_2
\\sim F3_2-F4_2 \\sim F3_2-
 F5_2 \\sim F3_2-F6_2
 with sigma of 0.04
 F1_1-F3_1 \\sim F2_1-F4_1 \\sim F6_1-F5_1
 F1_2-F3_2 \\sim F2_2-F4_2 \\sim F6_2-F5_2
 with sigma of 0.05
3. 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
4. Rigid body (RIGU) restrains
 P1_1, F1_1, F2_1, F3_1, F4_1, F5_1, F6_1
 P1_2, F1_2, F2_2, F3_2, F4_2, F5_2, F6_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8'(H8'), C9"(H9"), C6'(H6'), C6"(H6"), C7'(H7'), C10A(H10A), C6(H6),
 C3(H3), C9A(H9A), C9'(H9'), C7"(H7"), C2(H2), C8A(H8A), C8"(H8"), C2A(H2A),
 C4A(H4A), C3A(H3A), C2'(H2'), C3'(H3')
6.b Idealised Me refined as rotating group:
 C10(H10B,H10C,H10D)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_special_details
;
A solvent mask was calculated and 10 electrons were 
found in a volume of 39\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[H2O] per formula unit 
which account for 10 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2019/1
_smtbx_masks_special_details
;
A solvent mask was calculated and 4 electrons were 
found in a volume of 48\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C3H6O] per formula unit 
which account for 64 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.919
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              76946
_shelx_hkl_checksum              20941
_shelx_fab_checksum              4781