Cancer phototherapy by CO releasing terpyridine-based Re(I) tricarbonyl complexes <i>via</i> ROS generation and NADH oxidation.
Kushwaha, Rajesh; Upadhyay, Aarti; Saha, Sukanta; Yadav, Ashish Kumar; Bera, Arpan; Dutta, Arnab; Banerjee, Samya; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13591–13601; doi:10.1039/d4dt01309c

data_7716730
_publ_section_title
;
 Cancer phototherapy by CO releasing terpyridine-based Re(I) tricarbonyl
 complexes <i>via</i> ROS generation and NADH oxidation.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13591
_journal_page_last               13601
_journal_paper_doi               10.1039/d4dt01309c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H19 Cl N3 O3 Re, 0.334[C7H8]'
_chemical_formula_sum            'C34.33 H21.67 Cl N3 O3 Re'
_chemical_formula_weight         745.83
_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_creation_date             2024-06-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                89.027(2)
_cell_angle_beta                 82.586(3)
_cell_angle_gamma                79.332(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7233(2)
_cell_length_b                   13.4308(4)
_cell_length_c                   14.3953(5)
_cell_measurement_reflns_used    10771
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.0740
_cell_measurement_theta_min      2.6960
_cell_volume                     1455.11(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     44.00  76.00   0.50    3.54    --   11.61-148.00  86.00   64
  2  \w     20.00  60.00   0.50    3.54    --   11.61-124.00-108.00   80
  3  \w    -23.00   3.00   0.50    3.54    --  -11.38 -99.00-120.00   52
  4  \w    -23.00  23.00   0.50    3.54    --  -11.38 -99.00 -60.00   92
  5  \w    -79.00  10.00   0.50    3.54    --  -11.38 -57.00  30.00  178
  6  \w    -76.00 -23.00   0.50    3.54    --  -11.38 -77.00-150.00  106
  7  \w    -20.00   6.00   0.50    3.54    --  -11.38 -77.00   0.00   52
  8  \w    -78.00 -28.00   0.50    3.54    --  -11.38 -77.00   0.00  100
  9  \w    -17.00   8.00   0.50    3.54    --  -11.38 -99.00   0.00   50
 10  \w    -75.00 -50.00   0.50    3.54    --  -11.38 -38.00 -90.00   50
 11  \w     -9.00  16.00   0.50    3.54    --  -11.38 -77.00-150.00   50
 12  \w    -61.00   4.00   0.50    3.54    --  -11.38 -38.00-180.00  130
 13  \w    -14.00  22.00   0.50    3.54    --  -11.38 -99.00  90.00   72
 14  \w    -69.00  13.00   0.50    3.54    --  -11.38 -77.00  30.00  164
 15  \w     -6.00  19.00   0.50    3.54    --  -11.38 -99.00-180.00   50
 16  \w    -35.00 -10.00   0.50    3.54    --  -11.38 -38.00 -90.00   50
 17  \w    -16.00  10.00   0.50    3.54    --  -11.38 -99.00 120.00   52
 18  \w    -38.00   0.00   0.50    3.54    --   11.61 -19.00-150.00   76
 19  \w    -28.00  -3.00   0.50    3.54    --   11.61 -19.00  30.00   50
 20  \w     13.00  42.00   0.50    3.54    --   11.61-125.00 150.00   58
 21  \w     12.00  37.00   0.50    3.54    --   11.61-125.00  30.00   50
 22  \w    -60.00 -34.00   0.50    3.54    --   11.61 -19.00  30.00   52
 23  \w    -15.00  19.00   0.50    3.54    --   11.61 -38.00 120.00   68
 24  \w    -50.00 -24.00   0.50    3.54    --   11.61 -38.00 120.00   52
 25  \w    -48.00  28.00   0.50    3.54    --   11.61 -57.00 -90.00  152
 26  \w    -61.00 -30.00   0.50    3.54    --   11.61 -19.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21186
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.706
_exptl_absorpt_coefficient_mu    4.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.83a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             729
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.125
_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     331
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3706
_reflns_number_total             5030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01309c2.cif
_cod_data_source_block           re_tp2_auto
_cod_depositor_comments
'Adding full bibliography for 7716730--7716731.cif.'
_cod_database_code               7716730
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C22) = Uanis(C21)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C3(H3), C9(H9), C12(H12), C15(H15), C7(H7), C2(H2), C14(H14),
 C13(H13), C23(H23), C18(H18), C25(H25), C28(H28), C21(H21), C20(H20), C27(H27),
  C19(H19), C26(H26)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5274
_shelx_fab_checksum              22023
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;