Methylated regioisomers of Re(I) and Ir(III) tetrazole complexes: photophysical properties and optical imaging of brain tissue
Dallerba, Elena; Cameron, Lee; Armstrong, Blake I.; Ellison, Gaewyn; Turner, Eva; Innes, Evelyn; Strickling, Georgia L.; Pangiarella, Joel Ethan; O'Conghaile, Peter; Nesbit, Michael; Moggach, Stephen A.; Raiteri, Paolo; Stagni, Stefano; Pearson, Emma; Hackett, Mark; Massi, Massimiliano; Dalton Transactions  (2025) –; doi:10.1039/D5DT01745A

data_7719881
_publ_section_title
;
 Methylated regioisomers of Re(I) and Ir(III) tetrazole complexes:
 photophysical properties and optical imaging of brain tissue
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT01745A
_journal_year                    2025
_chemical_formula_moiety         'C10 H7 Br N5 O3 Re'
_chemical_formula_sum            'C10 H7 Br N5 O3 Re'
_chemical_formula_weight         511.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrg7
_audit_creation_date             2022-10-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1458(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.92166(4)
_cell_length_b                   11.90491(10)
_cell_length_c                   16.62188(11)
_cell_measurement_reflns_used    29702
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9960
_cell_measurement_theta_min      3.6820
_cell_volume                     1348.254(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     24.00  68.00   0.50    0.05    --   46.32  77.00 -60.00   88
  2  \w     24.00 118.00   0.50    0.05    --   46.32  77.00 120.00  188
  3  \w     32.00 118.00   0.50    0.05    --   46.32  57.00  90.00  172
  4  \w     34.00 121.00   0.50    0.05    --   46.32  18.00  36.00  174
  5  \w     24.00 118.00   0.50    0.05    --   46.32  77.00  90.00  188
  6  \w     24.00 118.00   0.50    0.05    --   46.32  77.00 150.00  188
  7  \w   -105.00 -30.00   0.50    0.05    -- -102.29  77.00 150.00  150
  8  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 150.00   82
  9  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 120.00   82
 10  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 -30.00   82
 11  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-120.00   82
 12  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
 13  \w     80.00 174.00   0.50    0.05    --  102.29  77.00 150.00  188
 14  \w     86.00 174.00   0.50    0.05    --  102.29  61.00 120.00  176
 15  \w     90.00 174.00   0.50    0.05    --  102.29  45.00 150.00  168
 16  \w     80.00 174.00   0.50    0.05    --  102.29  77.00 120.00  188
 17  \w     80.00 174.00   0.50    0.05    --  102.29  77.00  60.00  188
 18  \w     80.00 174.00   0.50    0.05    --  102.29  77.00  30.00  188
 19  \w     89.00 177.00   0.50    0.05    --  102.29  18.00  36.00  176
 20  \w     90.00 174.00   0.50    0.05    --  102.29  45.00-150.00  168
 21  \w    -28.00  26.00   0.50    0.05    --   46.32 -18.00-131.00  108
 22  \w    -26.00  43.00   0.50    0.05    --   46.32 -38.00  90.00  138
 23  \w     30.00 105.00   0.50    0.05    --  102.29 -77.00  60.00  150
 24  \w     30.00  71.00   0.50    0.05    --  102.29 -61.00-150.00   82
 25  \w     13.00  94.00   0.50    0.05    --   46.32-125.00-180.00  162
 26  \w     30.00 111.00   0.50    0.05    --  102.29-125.00-150.00  162
 27  \w    -26.00  29.00   0.50    0.05    --  -46.32  18.00  36.00  110
 28  \w    -43.00  27.00   0.50    0.05    --  -46.32  38.00 -30.00  140
 29  \w   -121.00 -33.00   0.50    0.05    --  -46.32 -18.00-131.00  176
 30  \w   -119.00 -33.00   0.50    0.05    --  -46.32 -38.00-180.00  172
 31  \w   -174.00 -79.00   0.50    0.05    -- -102.29 -78.00-152.37  190
 32  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 120.00  188
 33  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 122.94  188
 34  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00  89.57  188
 35  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -76.00 139.99  188
 36  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00 148.98  188
 37  \w   -174.00 -82.00   0.50    0.05    -- -102.29 -70.00 178.81  184
 38  \w   -174.00 -84.00   0.50    0.05    -- -102.29 -67.00 154.95  180
 39  \w   -174.00 -83.00   0.50    0.05    -- -102.29 -69.00 119.48  182
 40  \w   -174.00 -84.00   0.50    0.05    -- -102.29 -67.00 164.37  180
 41  \w   -174.00 -82.00   0.50    0.05    -- -102.29 -70.00  70.52  184
 42  \w   -174.00 -85.00   0.50    0.05    -- -102.29 -63.00  85.75  178
 43  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  90.00  176
 44  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 124.85  176
 45  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00-164.12  176
 46  \w   -174.00 -84.00   0.50    0.05    -- -102.29 -66.00-177.27  180
 47  \w   -174.00 -83.00   0.50    0.05    -- -102.29 -68.00-140.33  182
 48  \w   -111.00 -30.00   0.50    0.05    -- -102.29 125.00 150.00  162
 49  \w   -174.00 -89.00   0.50    0.05    -- -102.29 -52.00 136.41  170
 50  \w   -174.00 -89.00   0.50    0.05    -- -102.29 -52.00 129.41  170
 51  \w   -174.00 -88.00   0.50    0.05    -- -102.29 -53.00 105.83  172
 52  \w   -177.00 -89.00   0.50    0.05    -- -102.29 -18.00-131.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0590219000
_diffrn_orient_matrix_UB_12      0.0208523000
_diffrn_orient_matrix_UB_13      -0.0925206000
_diffrn_orient_matrix_UB_21      0.2129815000
_diffrn_orient_matrix_UB_22      -0.0224863000
_diffrn_orient_matrix_UB_23      -0.0109805000
_diffrn_orient_matrix_UB_31      -0.0479857000
_diffrn_orient_matrix_UB_32      -0.1257505000
_diffrn_orient_matrix_UB_33      -0.0133593000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38508
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.509
_diffrn_reflns_theta_min         4.593
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.266
_exptl_absorpt_correction_T_max  0.321
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'grown from the slow evaporation of acetone from an acetone and water solution'
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+4.8808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2750
_reflns_number_total             2757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01745a2.cif
_cod_data_source_block           mxm544vm
_cod_original_cell_volume        1348.253(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H7 C10 O3 N5 Br1 Re1'
_chemical_oxdiff_usercomment     'Lee Cameron'
_shelx_estimated_absorpt_t_max   0.186
_shelx_estimated_absorpt_t_min   0.073
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              94521
_olex2_exptl_crystal_mounting_method
'mounted on a glass fibre using silicon oil'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.724