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_7717637
_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         'C32 H21 Cl N5 O Ru, F6 P, 1.5(C3 H6 O)'
_chemical_formula_sum            'C36.5 H30 Cl F6 N5 O2.5 P Ru'
_chemical_formula_weight         860.14
_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     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
;
2024-10-16 deposited with the CCDC.	2024-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.034(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7628(7)
_cell_length_b                   27.6833(18)
_cell_length_c                   14.6097(12)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      25.114
_cell_measurement_theta_min      2.322
_cell_volume                     3530.4(5)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      300.00
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'Bruker PHOTON II CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_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  0.1322
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            85572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.030
_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    0.641
_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    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6474
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0265P)^2^+9.6251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4787
_reflns_number_total             6474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02562h2.cif
_cod_data_source_block           mpd1cl
_cod_depositor_comments
'Adding full bibliography for 7717636--7717637.cif.'
_cod_original_formula_sum        'C36.50 H30 Cl F6 N5 O2.50 P Ru'
_cod_database_code               7717637
_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. Uiso/Uaniso restraints and constraints
O2S \\sim C4S \\sim C6S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C5S: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O2S \\sim C4S \\sim C6S \\sim C5S: within 2A with sigma of 0.05 and sigma for
terminal atoms of 0.002 within 2A
3. Rigid body (RIGU) restrains
 O2S, C4S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O2S(0.5) C4S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) H5SC(0.5)
5.a Free rotating group:
 O2S(C4S,C6S)
5.b Aromatic/amide H refined with riding coordinates:
 C9'(H9'), C6(H6), C9(H9), C9"(H9"), C7'(H7'), C10A(H10A), C4A(H4A), C8'(H8'),
 C3(H3), C6"(H6"), C7"(H7"), C8"(H8"), C6'(H6'), C8A(H8A), C9A(H9A), C2A(H2A),
 C3'(H3'), C1(H1), C2'(H2'), C3A(H3A), C2(H2)
5.c Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C6S(H6SA,H6SB,H6SC), C5S(H5SA,H5SB,
 H5SC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.959
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              85944
_shelx_hkl_checksum              90429