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_7720880
_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         'C29 H30 N3 O3 Re'
_chemical_formula_sum            'C29 H30 N3 O3 Re'
_chemical_formula_weight         654.76
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-23
_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                92.0104(4)
_cell_angle_beta                 96.2968(5)
_cell_angle_gamma                97.2320(5)
_cell_formula_units_Z            2
_cell_length_a                   9.19418(7)
_cell_length_b                   10.16670(6)
_cell_length_c                   13.81606(6)
_cell_measurement_reflns_used    29286
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4170
_cell_measurement_theta_min      3.2030
_cell_volume                     1271.880(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_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 2014/4 (Sheldrick, 2014)'
_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 0.972
_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    -71.00  -6.00   0.50    0.25    --  -43.21 114.00 133.00  130
  2  \w     27.00  86.00   0.50    0.25    --   43.21-114.00  42.00  118
  3  \w    -71.00 -20.00   0.50    0.60    --  -96.00 114.00 133.00  102
  4  \w   -163.00 -96.00   0.50    0.60    --  -96.00-114.00  42.00  134
  5  \w     43.00  97.00   0.50    0.60    --  117.50-114.00  42.00  108
  6  \w    118.00 178.00   0.50    0.60    --  117.50 114.00 133.00  120
  7  \w   -120.00 -29.00   0.50    0.25    --  -43.21 -38.00  60.00  182
  8  \w     29.00  60.00   0.50    0.25    --   43.21  57.00 157.51   62
  9  \w     28.00  59.00   0.50    0.25    --   43.21  58.00 132.56   62
 10  \w     29.00  60.00   0.50    0.25    --   43.21  55.00-174.23   62
 11  \w    -34.00  19.00   0.50    0.25    --   43.21 -38.00  30.00  106
 12  \w      1.00  66.00   0.50    0.25    --   43.21 -77.00 120.00  130
 13  \w     27.00  54.00   0.50    0.25    --   43.21  61.00 -18.34   54
 14  \w     27.00  54.00   0.50    0.25    --   43.21  61.00 -84.92   54
 15  \w     28.00  59.00   0.50    0.25    --   43.21  58.00   4.58   62
 16  \w     27.00  54.00   0.50    0.25    --   43.21  61.00  34.60   54
 17  \w     27.00  54.00   0.50    0.25    --   43.21  61.00 -51.24   54
 18  \w    -34.00  19.00   0.50    0.25    --   43.21 -38.00 -30.00  106
 19  \w     27.00  54.00   0.50    0.25    --   43.21  61.00-111.35   54
 20  \w    -51.00 -22.00   0.50    0.60    --  -96.00  61.00 -90.00   58
 21  \w   -171.00 -82.00   0.50    0.60    --  -96.00 -47.00 116.20  178
 22  \w    -51.00 -22.00   0.50    0.60    --  -96.00  61.00  90.00   58
 23  \w    -51.00 -22.00   0.50    0.60    --  -96.00  61.00 -30.00   58
 24  \w   -136.00 -81.00   0.50    0.60    --  -96.00 -15.00-180.00  110
 25  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00 150.00   96
 26  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00 -30.00   96
 27  \w    103.00 136.00   0.50    0.60    --  117.50  15.00 -30.00   66
 28  \w     44.00 102.00   0.50    0.60    --  117.50-125.00-120.00  116
 29  \w    103.00 136.00   0.50    0.60    --  117.50  15.00-180.00   66
 30  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00-180.00   62
 31  \w     44.00 102.00   0.50    0.60    --  117.50-125.00 -30.00  116
 32  \w    124.00 178.00   0.50    0.60    --  117.50  77.00  90.00  108
 33  \w    103.00 136.00   0.50    0.60    --  117.50  15.00  60.00   66
 34  \w     44.00 102.00   0.50    0.60    --  117.50-125.00-180.00  116
 35  \w    112.00 178.00   0.50    0.60    --  117.50 125.00-150.00  132
 36  \w    124.00 178.00   0.50    0.60    --  117.50  77.00 -60.00  108
 37  \w    112.00 178.00   0.50    0.60    --  117.50 125.00-120.00  132
 38  \w    124.00 178.00   0.50    0.60    --  117.50  77.00-180.00  108
 39  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00-150.00   62
 40  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00  60.00   96
 41  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00-120.00   96
 42  \w    103.00 136.00   0.50    0.60    --  117.50  15.00-150.00   66
 43  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00 120.00   96
 44  \w    112.00 178.00   0.50    0.60    --  117.50 125.00  60.00  132
 45  \w     44.00  95.00   0.50    0.60    --  117.50 -91.00 167.25  102
 46  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00 -30.00   62
 47  \w    103.00 136.00   0.50    0.60    --  117.50  15.00   0.00   66
 48  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00 -90.00   62
 49  \w    105.00 178.00   0.50    0.60    --  117.50  45.00   0.00  146
 50  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00  30.00   96
 51  \w    105.00 178.00   0.50    0.60    --  117.50  45.00-120.00  146
 52  \w     44.00 102.00   0.50    0.60    --  117.50-125.00 -90.00  116
 53  \w    104.00 166.00   0.50    0.60    --  117.50  30.00  60.00  124
 54  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00 -60.00   96
 55  \w    103.00 136.00   0.50    0.60    --  117.50  15.00 -90.00   66
 56  \w     44.00 102.00   0.50    0.60    --  117.50-125.00-150.00  116
 57  \w    124.00 178.00   0.50    0.60    --  117.50  77.00-150.00  108
 58  \w    103.00 136.00   0.50    0.60    --  117.50  15.00  30.00   66
 59  \w    103.00 136.00   0.50    0.60    --  117.50  15.00 -60.00   66
 60  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00-120.00   62
 61  \w     44.00  75.00   0.50    0.60    --  117.50 -77.00  30.00   62
 62  \w    124.00 178.00   0.50    0.60    --  117.50  77.00 -90.00  108
 63  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00 -90.00   96
 64  \w     44.00 102.00   0.50    0.60    --  117.50-125.00  30.00  116
 65  \w     44.00  92.00   0.50    0.60    --  117.50 -95.00  90.00   96
 66  \w   -120.00 -29.00   0.50    0.25    --  -43.21 -38.00-120.00  182
 67  \w    -19.00  34.00   0.50    0.25    --  -43.21  38.00-120.00  106
 68  \w   -120.00 -29.00   0.50    0.25    --  -43.21 -38.00 150.00  182
 69  \w   -120.00 -29.00   0.50    0.25    --  -43.21 -38.00 -30.00  182
 70  \w     27.00  54.00   0.50    0.25    --   43.21  61.00 -68.28   54
 71  \w    -34.00  19.00   0.50    0.25    --   43.21 -38.00  90.00  106
 72  \w     28.00  59.00   0.50    0.25    --   43.21  58.00 104.28   62
 73  \w     28.00  59.00   0.50    0.25    --   43.21  59.00  65.73   62
 74  \w     28.00  57.00   0.50    0.25    --   43.21  60.00-169.68   58
 75  \w     18.00  77.00   0.50    0.25    --   43.21 -99.00 -60.00  118
 76  \w     28.00  59.00   0.50    0.25    --   43.21  59.00-139.98   62
 77  \w     30.00 120.00   0.50    0.25    --   43.21  38.00 -60.00  180
 78  \w     29.00  60.00   0.50    0.25    --   43.21  56.00  -5.24   62
 79  \w     29.00  60.00   0.50    0.25    --   43.21  55.00-141.06   62
 80  \w   -169.00 -83.00   0.50    0.60    --  -96.00 -53.00   9.74  172
 81  \w   -170.00 -83.00   0.50    0.60    --  -96.00 -55.00 -83.33  174
 82  \w   -171.00 -82.00   0.50    0.60    --  -96.00 -48.00 -48.38  178
 83  \w   -170.00 -83.00   0.50    0.60    --  -96.00 -55.00-168.75  174
 84  \w   -170.00 -82.00   0.50    0.60    --  -96.00 -52.00  77.63  176
 85  \w    103.00 136.00   0.50    0.60    --  117.50  15.00 120.00   66
 86  \w    103.00 136.00   0.50    0.60    --  117.50  15.00-120.00   66
 87  \w    103.00 136.00   0.50    0.60    --  117.50  15.00 150.00   66
;
_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      -0.1653794000
_diffrn_orient_matrix_UB_12      0.0146340000
_diffrn_orient_matrix_UB_13      -0.0050870000
_diffrn_orient_matrix_UB_21      -0.0184299000
_diffrn_orient_matrix_UB_22      -0.0344960000
_diffrn_orient_matrix_UB_23      -0.1105038000
_diffrn_orient_matrix_UB_31      -0.0349395000
_diffrn_orient_matrix_UB_32      -0.1482717000
_diffrn_orient_matrix_UB_33      0.0194633000
_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  0.0230
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31276
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.863
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.40a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00076(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0311P)^2^+1.7582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5383
_reflns_number_total             5386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00370b2.cif
_cod_data_source_block           felix241
_cod_depositor_comments
'Adding full bibliography for 7720880--7720882.cif.'
_cod_original_cell_volume        1271.880(13)
_cod_database_code               7720880
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C29H30N3O3Re
_chemical_oxdiff_usercomment     'Nguyen  MLN88'
_reflns_odcompleteness_completeness 98.73
_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), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C16(H16)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              86090
_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 1.173
_oxdiff_exptl_absorpt_empirical_full_min 0.830