Synthesis of a Rhenium(VII) Trioxo Complex Supported by a Triphyrin Ligand: Oxygenation Chemistry and Deposition on Au(111)
Nguyen, Manh Linh; Strunskus, Thomas; Nather, Christian; Krahmer, Jan; Tuczek, Felix; Dalton Transactions  (2026) –; doi:10.1039/D6DT00370B

data_7720881
_publ_section_title
;
 Synthesis of a rhenium(VII) trioxo complex supported by a triphyrin
 ligand: oxygenation chemistry and deposition on Au(111).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6944
_journal_page_last               6953
_journal_paper_doi               10.1039/d6dt00370b
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C26 H30 N3 O3 Re'
_chemical_formula_sum            'C26 H30 N3 O3 Re'
_chemical_formula_weight         618.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-21
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2026-02-10 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1324(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2187(3)
_cell_length_b                   11.70587(14)
_cell_length_c                   24.6546(3)
_cell_measurement_reflns_used    39219
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3210
_cell_measurement_theta_min      3.7430
_cell_volume                     5819.68(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.986
_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      6.00  37.00   0.50    5.00    --  -42.93  24.00 130.00   62
  2  \w   -122.00 -29.00   0.50    5.00    --  -42.93 -24.00 -33.00  186
  3  \w     30.00 122.00   0.50    5.00    --   42.93  24.00 130.00  184
  4  \w   -159.00 -78.00   0.50   15.00    --  -91.75 -24.00 -33.00  162
  5  \w    100.00 159.00   0.50   15.00    --  113.25  24.00 130.00  118
  6  \w    -19.00  34.00   0.50    5.00    --  -42.93  38.00 -90.00  106
  7  \w    -19.00  34.00   0.50    5.00    --  -42.93  38.00 150.00  106
  8  \w     34.00  91.00   0.50    5.00    --   42.93-125.00 -30.00  114
  9  \w    -51.00 -17.00   0.50   15.00    --  -91.75  61.00  90.00   68
 10  \w    -67.00 -17.00   0.50   15.00    --  -91.75  77.00 -90.00  100
 11  \w     40.00 101.00   0.50   15.00    --  113.25-125.00   0.00  122
 12  \w     98.00 136.00   0.50   15.00    --  113.25  15.00 -60.00   76
 13  \w     98.00 136.00   0.50   15.00    --  113.25  15.00 -90.00   76
 14  \w     98.00 136.00   0.50   15.00    --  113.25  15.00  30.00   76
 15  \w     40.00  75.00   0.50   15.00    --  113.25 -77.00 120.00   70
 16  \w    124.00 178.00   0.50   15.00    --  113.25  77.00-150.00  108
 17  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00-150.00  104
 18  \w     40.00  75.00   0.50   15.00    --  113.25 -77.00 150.00   70
 19  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00 -90.00  104
 20  \w     40.00 101.00   0.50   15.00    --  113.25-125.00 -90.00  122
 21  \w    124.00 178.00   0.50   15.00    --  113.25  77.00-180.00  108
 22  \w    124.00 178.00   0.50   15.00    --  113.25  77.00 -60.00  108
 23  \w     40.00  75.00   0.50   15.00    --  113.25 -77.00  60.00   70
 24  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00 120.00  104
 25  \w     40.00  75.00   0.50   15.00    --  113.25 -77.00   0.00   70
 26  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00-180.00  104
 27  \w     40.00  75.00   0.50   15.00    --  113.25 -77.00-120.00   70
 28  \w    100.00 166.00   0.50   15.00    --  113.25  30.00 -60.00  132
 29  \w    112.00 178.00   0.50   15.00    --  113.25 125.00   0.00  132
 30  \w     98.00 136.00   0.50   15.00    --  113.25  15.00  60.00   76
 31  \w    112.00 178.00   0.50   15.00    --  113.25 125.00 -60.00  132
 32  \w     98.00 136.00   0.50   15.00    --  113.25  15.00 120.00   76
 33  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00  30.00  104
 34  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00   0.00  104
 35  \w   -120.00 -28.00   0.50    5.00    --  -42.93 -38.00-120.00  184
 36  \w    -19.00  34.00   0.50    5.00    --  -42.93  38.00   0.00  106
 37  \w   -120.00 -28.00   0.50    5.00    --  -42.93 -38.00-180.00  184
 38  \w     30.00 120.00   0.50    5.00    --   42.93  38.00-180.00  180
 39  \w     18.00  77.00   0.50    5.00    --   42.93 -99.00 150.00  118
 40  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00-120.00  178
 41  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00 -60.00  178
 42  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00  60.00  178
 43  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00 -30.00  178
 44  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00-180.00  178
 45  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00 150.00  178
 46  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00-150.00  178
 47  \w   -167.00 -78.00   0.50   15.00    --  -91.75 -45.00  30.00  178
 48  \w     40.00 101.00   0.50   15.00    --  113.25-125.00 150.00  122
 49  \w     98.00 136.00   0.50   15.00    --  113.25  15.00  90.00   76
 50  \w     98.00 136.00   0.50   15.00    --  113.25  15.00-150.00   76
 51  \w    124.00 178.00   0.50   15.00    --  113.25  77.00  60.00  108
 52  \w    124.00 178.00   0.50   15.00    --  113.25  77.00 120.00  108
 53  \w    100.00 178.00   0.50   15.00    --  113.25  45.00   0.00  156
 54  \w     98.00 136.00   0.50   15.00    --  113.25  15.00-120.00   76
 55  \w     40.00  92.00   0.50   15.00    --  113.25 -95.00  60.00  104
 56  \w     98.00 136.00   0.50   15.00    --  113.25  15.00-180.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0636230000
_diffrn_orient_matrix_UB_12      -0.0271021000
_diffrn_orient_matrix_UB_13      0.0150619000
_diffrn_orient_matrix_UB_21      0.0421838000
_diffrn_orient_matrix_UB_22      -0.0308568000
_diffrn_orient_matrix_UB_23      0.0612992000
_diffrn_orient_matrix_UB_31      -0.0034460000
_diffrn_orient_matrix_UB_32      0.1249506000
_diffrn_orient_matrix_UB_33      0.0184191000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52207
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.693
_diffrn_reflns_theta_min         3.773
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.627
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0307P)^2^+29.3739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5860
_reflns_number_total             6122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00370b2.cif
_cod_data_source_block           felix248
_cod_depositor_comments
'Adding full bibliography for 7720880--7720882.cif.'
_cod_original_cell_volume        5819.70(14)
_cod_database_code               7720881
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C26H30N3O3Re
_chemical_oxdiff_usercomment     'Nguyen MLN91'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C10(H10), C11(H11), C16(H16)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9680
_shelx_fab_checksum              68607
_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 1.861
_oxdiff_exptl_absorpt_empirical_full_min 0.632