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_7719879
_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         'C14 H9 Br N5 O3 Re'
_chemical_formula_sum            'C14 H9 Br N5 O3 Re'
_chemical_formula_weight         561.37
_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.cc2dlrj9
_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                 92.1110(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.87749(3)
_cell_length_b                   11.42838(6)
_cell_length_c                   19.41606(9)
_cell_measurement_reflns_used    30954
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2970
_cell_measurement_theta_min      3.7940
_cell_volume                     1525.039(13)
_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 0.984
_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     24.00 119.00   0.50    0.05    --   46.07  77.00  60.00  190
  2  \w     24.00 119.00   0.50    0.05    --   46.07  77.00 120.00  190
  3  \w     24.00 119.00   0.50    0.05    --   46.07  77.00 150.00  190
  4  \w     24.00 119.00   0.50    0.05    --   46.07  77.00 -30.00  190
  5  \w     24.00 119.00   0.50    0.05    --   46.07  77.00-150.00  190
  6  \w     24.00 119.00   0.50    0.05    --   46.07  77.00 -90.00  190
  7  \w     31.00 119.00   0.50    0.05    --   46.07  57.00-150.00  176
  8  \w     34.00 119.00   0.50    0.05    --   46.07  38.00 -60.00  170
  9  \w     31.00 119.00   0.50    0.05    --   46.07  57.00 -60.00  176
 10  \w     31.00 119.00   0.50    0.05    --   46.07  57.00  60.00  176
 11  \w     24.00 119.00   0.50    0.05    --   46.07  77.00   0.00  190
 12  \w     34.00 119.00   0.50    0.05    --   46.07  38.00-180.00  170
 13  \w    -28.00  26.00   0.50    0.05    --   46.07 -19.00-150.00  108
 14  \w    -28.00  26.00   0.50    0.05    --   46.07 -19.00 -90.00  108
 15  \w     30.00  71.00   0.50    0.05    --  102.29 -61.00-150.00   82
 16  \w     30.00  71.00   0.50    0.05    --  102.29 -61.00-120.00   82
 17  \w    -28.00  26.00   0.50    0.05    --   46.07 -19.00   0.00  108
 18  \w     30.00 105.00   0.50    0.05    --  102.29 -77.00  90.00  150
 19  \w     30.00  71.00   0.50    0.05    --  102.29 -61.00  30.00   82
 20  \w     26.00 108.00   0.50    0.05    --   46.07-149.00-100.00  164
 21  \w     30.00 105.00   0.50    0.05    --  102.29 -94.00 -90.00  150
 22  \w     30.00 129.00   0.50    0.05    --  102.29-149.00-100.00  198
 23  \w     30.00 111.00   0.50    0.05    --  102.29-125.00  30.00  162
 24  \w     30.00 110.00   0.50    0.05    --  102.29-123.00  63.00  160
 25  \w     12.00  93.00   0.50    0.05    --   46.07-123.00  63.00  162
 26  \w   -110.00 -30.00   0.50    0.05    -- -102.29 123.00 143.00  160
 27  \w   -121.00 -30.00   0.50    0.05    -- -102.29 138.00  83.96  182
 28  \w   -111.00 -30.00   0.50    0.05    -- -102.29 125.00  60.00  162
 29  \w   -128.00 -30.00   0.50    0.05    -- -102.29 149.00 -52.00  196
 30  \w   -111.00 -30.00   0.50    0.05    -- -102.29 125.00 -60.00  162
 31  \w   -111.00 -30.00   0.50    0.05    -- -102.29 125.00-120.00  162
 32  \w   -107.00 -25.00   0.50    0.05    --  -46.07 149.00 -52.00  164
 33  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
 34  \w    -71.00 -30.00   0.50    0.05    -- -102.29  61.00  90.00   82
 35  \w    -92.00 -11.00   0.50    0.05    --  -46.07 123.00 143.00  162
 36  \w     90.00 174.00   0.50    0.05    --  102.29  45.00-120.00  168
 37  \w     74.00 119.00   0.50    0.05    --   46.07 125.00-180.00   90
 38  \w     57.00 119.00   0.50    0.05    --   46.07 149.00 -52.00  124
 39  \w     57.00 166.00   0.50    0.05    --  102.29 149.00 -52.00  218
 40  \w     75.00 174.00   0.50    0.05    --  102.29 123.00 143.00  198
 41  \w     90.00 174.00   0.50    0.05    --  102.29  45.00 -60.00  168
 42  \w   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00  40.95  188
 43  \w   -174.00-109.00   0.50    0.05    -- -102.29 -70.00  68.39  130
 44  \w   -174.00 -85.00   0.50    0.05    -- -102.29 -63.00 150.52  178
 45  \w   -174.00 -88.00   0.50    0.05    -- -102.29 -48.00  98.74  172
 46  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -60.00  85.78  176
 47  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -12.12  176
 48  \w   -174.00 -87.00   0.50    0.05    -- -102.29 -59.00 -28.46  174
 49  \w   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -90.00  176
 50  \w   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-150.00  168
 51  \w   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-180.00  168
 52  \w   -119.00 -57.00   0.50    0.05    --  -46.07-149.00-100.00  124
 53  \w   -166.00 -57.00   0.50    0.05    -- -102.29-149.00-100.00  218
 54  \w   -174.00 -75.00   0.50    0.05    -- -102.29-123.00  63.00  198
 55  \w   -119.00 -73.00   0.50    0.05    --  -46.07-125.00  90.00   92
 56  \w   -119.00 -73.00   0.50    0.05    --  -46.07-125.00 120.00   92
;
_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      -0.2131846000
_diffrn_orient_matrix_UB_12      0.0312468000
_diffrn_orient_matrix_UB_13      0.0134090000
_diffrn_orient_matrix_UB_21      -0.0463662000
_diffrn_orient_matrix_UB_22      -0.1305654000
_diffrn_orient_matrix_UB_23      0.0103892000
_diffrn_orient_matrix_UB_31      0.0515159000
_diffrn_orient_matrix_UB_32      0.0120890000
_diffrn_orient_matrix_UB_33      0.0775634000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44552
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.491
_diffrn_reflns_theta_min         4.490
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'grown from the slow evaporation of an acetonitrile solution'
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0253P)^2^+4.6815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3102
_reflns_number_total             3118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01745a2.cif
_cod_data_source_block           mxm551rm
_cod_original_cell_volume        1525.038(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719879
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Re1 C14 H9 O3 N5 Br1'
_chemical_oxdiff_usercomment     'Lee Cameron'
_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), C11(H11), C7(H7), C12(H12), C13(H13), C8(H8)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              20903
_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 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.757