Fluorine-Substituted Cyclometallated Rhodium(III) Complexes with α-Diimine Ancillary Ligands: Synthesis, Structure, Photophysical and DNA-Binding Properties
Wójcik, Patryk; Latouche, Camille; Kamecka, Anna; Suwinska, Kinga; Masternak, Joanna; Urbaniak, Mariusz; Dalton Transactions  (2025) –; doi:10.1039/D5DT02369F

data_7719937
_publ_section_title
;
 Fluorine-Substituted Cyclometallated Rhodium(III) Complexes with
 \a-Diimine Ancillary Ligands: Synthesis, Structure, Photophysical and
 DNA-Binding Properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02369F
_journal_year                    2025
_chemical_formula_moiety         'C36 H20 F4 N8 Rh+, P F6-'
_chemical_formula_sum            'C36 H20 F10 N8 P Rh'
_chemical_formula_weight         888.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-09-24 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.9700(3)
_cell_length_b                   31.9700(3)
_cell_length_c                   13.8402(2)
_cell_measurement_reflns_used    9301
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      68.1632
_cell_measurement_theta_min      3.9108
_cell_measurement_wavelength     1.54178
_cell_volume                     14145.8(3)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.5.6'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            PhotonII_7
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  27.500 deg omega=   0.000 deg chi=  54.739 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  27.500 deg omega=   0.000 deg chi=  54.739 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  27.500 deg omega=   0.000 deg chi=  54.739 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi= 128.000 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi=  64.001 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta= -21.739 deg omega= 317.771 deg chi=  54.739 deg] 
measure for 1.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi=  95.999 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 252.2; len= 182.5; end= 434.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  36.739 deg phi=  90.000 deg chi=  54.739 deg] 
measure for 6.8 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi=  32.000 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi= 160.000 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 267.2; len= 182.5; end= 449.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  44.239 deg phi=   0.000 deg chi=  54.739 deg] 
measure for 12.3 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi= 256.000 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 267.2; len= 182.5; end= 449.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  44.239 deg phi= 270.000 deg chi=  54.739 deg] 
measure for 12.3 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Omega scan: start= 283.2; len= 180.5; end= 463.7 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg phi= 192.001 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start=  23.7; len= 256.5; end= 280.2 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta=  51.739 deg omega= 282.229 deg chi=  54.739 deg] 
measure for 20.0 seconds; frame angle 0.50 degrees, wavelength=1.54184>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 47.97 mm theta= -29.239 deg omega= 302.771 deg chi=  54.739 deg] 
measure for 3.2 seconds; frame angle 0.50 degrees, wavelength=1.54184>
;
_diffrn_measurement_device       'FIXEDCHI diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            95597
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.165
_diffrn_reflns_theta_min         2.764
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_target            Cu
_diffrn_source_type              'INCOATEC I\mS Compact'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.18
_exptl_absorpt_correction_T_max  0.463
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       prism
_exptl_crystal_F_000             7072
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0638P)^2^+31.5729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5276
_reflns_number_total             6409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02369f2.cif
_cod_data_source_block           cu_S332cf2_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7719937
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.7837
_shelx_estimated_absorpt_t_min   0.362
_shelx_estimated_absorpt_t_max   0.463
_bruker_diffrn_measurement_temperature_device Cryostream
_diffrn_measurement_bruker_total_exposure_time 75825.0
_diffrn_reflns_bruker_av_norm_i  7286.288
_diffrn_reflns_bruker_number_gt  85485
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              63457