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_7720882
_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, C4 H10 O'
_chemical_formula_sum            'C30 H40 N3 O4 Re'
_chemical_formula_weight         692.85
_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_creation_date             2025-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-10 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0758(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.67065(7)
_cell_length_b                   11.75682(6)
_cell_length_c                   17.06503(10)
_cell_measurement_reflns_used    31360
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.8890
_cell_measurement_theta_min      3.0980
_cell_volume                     2888.56(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.121a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.121a 64-bit (release 04-09-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.121a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (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 0.995
_diffrn_measured_fraction_theta_max 0.973
_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    -75.00 -14.00   0.50    2.00    --  -42.23 127.00  57.00  122
  2  \w     36.00  91.00   0.50    2.00    --   42.23-127.00 -18.00  110
  3  \w    -75.00 -23.00   0.50    5.00    --  -96.00 127.00  57.00  104
  4  \w   -152.00 -89.00   0.50    5.00    --  -96.00-127.00 -18.00  126
  5  \w    111.00 176.00   0.50    5.00    --  117.50 127.00  57.00  130
  6  \w     44.00 101.00   0.50    5.00    --  117.50-127.00 -18.00  114
  7  \w    -19.00  35.00   0.50    2.00    --  -42.23  38.00-120.00  108
  8  \w    -45.00  32.00   0.50    2.00    --  -42.23  57.00 -30.00  154
  9  \w    -45.00  32.00   0.50    2.00    --  -42.23  57.00 -30.00  154
 10  \w    -19.00  35.00   0.50    2.00    --  -42.23  38.00 -60.00  108
 11  \w     28.00  60.00   0.50    2.00    --   42.23  55.00-133.32   64
 12  \w     26.00  54.00   0.50    2.00    --   42.23  61.00  45.52   56
 13  \w     27.00  59.00   0.50    2.00    --   42.23  58.00-162.53   64
 14  \w     34.00  90.00   0.50    2.00    --   42.23-125.00-180.00  112
 15  \w    -35.00  19.00   0.50    2.00    --   42.23 -38.00-120.00  108
 16  \w     34.00  90.00   0.50    2.00    --   42.23-125.00  60.00  112
 17  \w    -67.00 -22.00   0.50    5.00    --  -96.00  77.00  30.00   90
 18  \w    -51.00 -22.00   0.50    5.00    --  -96.00  61.00  60.00   58
 19  \w   -136.00 -81.00   0.50    5.00    --  -96.00 -15.00-150.00  110
 20  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00   0.00   96
 21  \w    109.00 178.00   0.50    5.00    --  117.50  61.00 -30.00  138
 22  \w    103.00 136.00   0.50    5.00    --  117.50  15.00 -60.00   66
 23  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00  30.00   96
 24  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00 120.00   96
 25  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00-180.00   96
 26  \w    103.00 136.00   0.50    5.00    --  117.50  15.00  90.00   66
 27  \w    104.00 166.00   0.50    5.00    --  117.50  30.00 -90.00  124
 28  \w    103.00 136.00   0.50    5.00    --  117.50  15.00 150.00   66
 29  \w     44.00 101.00   0.50    5.00    --  117.50-125.00-120.00  114
 30  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00  90.00   96
 31  \w    103.00 136.00   0.50    5.00    --  117.50  15.00-120.00   66
 32  \w     44.00 101.00   0.50    5.00    --  117.50-125.00 -60.00  114
 33  \w    112.00 178.00   0.50    5.00    --  117.50 125.00-180.00  132
 34  \w    112.00 178.00   0.50    5.00    --  117.50 125.00-180.00  132
 35  \w    103.00 136.00   0.50    5.00    --  117.50  15.00-180.00   66
 36  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00 -60.00   96
 37  \w     44.00 101.00   0.50    5.00    --  117.50-125.00   0.00  114
 38  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00 -30.00   96
 39  \w     44.00  92.00   0.50    5.00    --  117.50 -95.00  60.00   96
 40  \w     44.00 101.00   0.50    5.00    --  117.50-125.00  30.00  114
 41  \w     44.00  75.00   0.50    5.00    --  117.50 -77.00 120.00   62
 42  \w     44.00  75.00   0.50    5.00    --  117.50 -77.00-150.00   62
 43  \w   -119.00 -28.00   0.50    2.00    --  -42.23 -38.00-180.00  182
 44  \w   -122.00 -28.00   0.50    2.00    --  -42.23 -19.00 -90.00  188
 45  \w     26.00  54.00   0.50    2.00    --   42.23  61.00 161.39   56
 46  \w     27.00  57.00   0.50    2.00    --   42.23  60.00 113.69   60
 47  \w     26.00  54.00   0.50    2.00    --   42.23  61.00  -0.09   56
 48  \w     26.00  54.00   0.50    2.00    --   42.23  61.00 -44.38   56
 49  \w     26.00  54.00   0.50    2.00    --   42.23  61.00  78.76   56
 50  \w     26.00  54.00   0.50    2.00    --   42.23  61.00 -88.61   56
 51  \w   -170.00 -83.00   0.50    5.00    --  -96.00 -55.00  84.55  174
 52  \w   -170.00 -82.50   0.50    5.00    --  -96.00 -52.00  59.41  175
;
_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      -0.0032365000
_diffrn_orient_matrix_UB_12      -0.1235781000
_diffrn_orient_matrix_UB_13      -0.0304784000
_diffrn_orient_matrix_UB_21      -0.0118160000
_diffrn_orient_matrix_UB_22      -0.0427692000
_diffrn_orient_matrix_UB_23      0.0828034000
_diffrn_orient_matrix_UB_31      -0.1062720000
_diffrn_orient_matrix_UB_32      0.0085049000
_diffrn_orient_matrix_UB_33      -0.0260680000
_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  0.0216
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41023
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.105
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.538
_exptl_absorpt_correction_T_max  0.21890
_exptl_absorpt_correction_T_min  0.11392
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.121a (Rigaku Oxford Diffraction, 2025)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'lustrous dark red'
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.253
_refine_diff_density_max         1.895
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0365P)^2^+5.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5931
_reflns_number_total             6125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00370b2.cif
_cod_data_source_block           felix325
_cod_depositor_comments
'Adding full bibliography for 7720880--7720882.cif.'
_cod_database_code               7720882
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C26H30N3O3Re
_chemical_oxdiff_usercomment     Re(VII)TriP
_diffrn_oxdiff_digest_hkl
;
435981cf634e4cf9e387f070f7bb162b746f86
;
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name Felix325.par
_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:
 C5(H5A,H5B), C8(H8A,H8B), C14(H14A,H14B), C25(H25A,H25B), C101(H10A,H10B),
 C102(H10C,H10D)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C103(H10E,H10F,H10G), C104(H10H,H10I,
 H10J)
;
_shelx_res_checksum              72934
_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.703