A di-nuclear μ-oxido rhenium(VI) complex: from deep purple to catalytic applications.
Doliner, Tobias A.; Hartmann, Peter E.; Oberwinkler, Gernot; Belaj, Ferdinand; Dupé, Antoine; Boese, A. Daniel; Schachner, Jörg A; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4547–4559; doi:10.1039/d6dt00039h

data_7720389
_publ_section_title
;
 A di-nuclear &#x3bc;-oxido rhenium(VI) complex: from deep purple to
 catalytic applications.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4547
_journal_page_last               4559
_journal_paper_doi               10.1039/d6dt00039h
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C38 H56 Cl4 N2 O7 Re2, C6 H12'
_chemical_formula_sum            'C44 H68 Cl4 N2 O7 Re2'
_chemical_formula_weight         1251.20
_chemical_name_systematic
'(mu-oxido)-bis((2,4-t-butyl-6-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenolato)-dichlorido-oxido-rhenium(VI)) cyclohexane solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-16
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-11-04 deposited with the CCDC.	2026-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0500(2)
_cell_length_b                   19.9825(2)
_cell_length_c                   16.4972(2)
_cell_measurement_reflns_used    31998
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9060
_cell_measurement_theta_min      2.9790
_cell_volume                     4881.02(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.106a 64-bit (release 01-02-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -35.00  -2.00   0.50    0.20    --  -80.26  30.00-150.00   66
  2  \w    -35.00  -2.00   0.50    0.20    --  -80.26  30.00 -30.00   66
  3  \w    -71.00  -9.00   0.50    0.20    --  -80.26  61.00   0.00  124
  4  \w    -33.00  -3.00   0.50    0.20    --  -80.26  30.00  60.00   60
  5  \w    -68.00 -10.00   0.50    0.20    --  -80.26  61.00  90.00  116
  6  \w    -33.00  -4.00   0.50    0.20    --   12.00 113.00  43.29   58
  7  \w      0.00  26.00   0.50    0.20    --   24.00  76.00 112.24   52
  8  \w    -10.00  16.00   0.50    0.20    --   20.00  87.00 -48.97   52
  9  \w    -26.00   6.00   0.50    0.20    --   12.00 101.00 -97.48   64
 10  \w      8.00  34.00   0.50    0.20    --   28.00  69.00-153.84   52
 11  \w     71.00 116.00   0.50    0.60    --  110.00  19.00 -52.70   90
 12  \w     99.00 124.00   0.50    0.60    --  106.73  30.00-120.00   50
 13  \w    145.00 172.00   0.50    0.60    --  110.00  19.00 -52.70   54
 14  \w    100.00 126.00   0.50    0.60    --  106.73  77.00  90.00   52
 15  \w     72.00 104.00   0.50    0.60    --  110.00  18.00 100.01   64
 16  \w     87.00 122.00   0.50    0.60    --  110.00  19.00 121.23   70
 17  \w    144.00 169.00   0.50    0.60    --  110.00  18.00 100.01   50
 18  \w    104.00 155.00   0.50    0.60    --  110.00  12.00  59.54  102
 19  \w     71.00  97.00   0.50    0.60    --  110.00  17.00   4.63   52
 20  \w     47.00  87.00   0.50    0.60    --  110.00  12.00  59.54   80
 21  \w    108.00 167.00   0.50    0.60    --  110.00   7.00 -97.11  118
 22  \w     45.00 100.00   0.50    0.60    --  110.00   7.00 -97.11  110
 23  \w     46.00  72.00   0.50    0.60    --  110.00 -78.00 -92.07   52
 24  \w     44.00 103.00   0.50    0.60    --  110.00 -78.00-151.58  118
 25  \w     45.00  71.00   0.50    0.60    --  110.00 -80.00  83.35   52
 26  \w     98.00 134.00   0.50    0.60    --  110.00 -79.00  64.79   72
 27  \w     99.00 136.00   0.50    0.60    --  110.00 -81.00  33.80   74
 28  \w    103.00 130.00   0.50    0.60    --  110.00 -88.00 121.23   54
 29  \w     47.00  80.00   0.50    0.60    --  110.00 -88.00 121.23   66
 30  \w     43.00  87.00   0.50    0.60    --  110.00 -88.00  21.17   88
 31  \w     44.00 115.00   0.50    0.60    --  110.00 -88.00 -39.80  142
 32  \w    103.00 133.00   0.50    0.60    --  110.00 -88.00-121.28   60
 33  \w     43.00  89.00   0.50    0.60    --  110.00 -88.00-163.20   92
 34  \w     63.00  89.00   0.50    0.60    --  110.00 -88.00-121.28   52
 35  \w     59.00  85.00   0.50    0.60    --  110.00 -87.00 -55.66   52
 36  \w     50.00  78.00   0.50    0.60    --  110.00 -81.00  33.80   56
 37  \w     44.00  77.00   0.50    0.60    --  110.00 -87.00  77.59   66
 38  \w     88.00 114.00   0.50    0.60    --  110.00 -87.00  77.59   52
 39  \w     45.00 107.00   0.50    0.60    --  110.00 -87.00   3.42  124
 40  \w    112.00 137.00   0.50    0.60    --  110.00 -81.00-173.69   50
 41  \w   -139.00 -47.00   0.50    0.20    --  -64.00 -55.00 -31.34  184
 42  \w   -134.00-102.00   0.50    0.20    --  -80.26 -77.00 -90.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0345847000
_diffrn_orient_matrix_UB_12      0.0706410000
_diffrn_orient_matrix_UB_13      0.0266556000
_diffrn_orient_matrix_UB_21      -0.0920609000
_diffrn_orient_matrix_UB_22      0.0169305000
_diffrn_orient_matrix_UB_23      0.0233693000
_diffrn_orient_matrix_UB_31      0.0341494000
_diffrn_orient_matrix_UB_32      -0.0259418000
_diffrn_orient_matrix_UB_33      0.0879539000
_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  0.0517
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.379
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.951
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM / cyclohexane'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         10338
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0558P)^2^+20.3264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9639
_reflns_number_total             10338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00039h2.cif
_cod_data_source_block           ad32
_cod_depositor_comments
'Adding full bibliography for 7720387--7720392.cif.'
_cod_database_code               7720389
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H57 N2 O7 Cl4 Re2 '
_chemical_oxdiff_usercomment     JSA-TD11
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.285
_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. Restrained distances
 C41-C42 = C41-C46 = C42-C43 = C43-C44 = C44-C45 = C45-C46
 1.54 with sigma of 0.02
 C41-C43 = C41-C45 = C42-C44 = C43-C45 = C44-C46
 2.54 with sigma of 0.04
 C34-C36 \\sim C34-C56
 with sigma of 0.02
 C34-C35 \\sim C34-C55
 with sigma of 0.02
 C34-C37 \\sim C34-C57
 with sigma of 0.02
 C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41
 with sigma of 0.02
 C41-C45 \\sim C43-C45 \\sim C42-C46 \\sim C42-C44 \\sim C44-C46 \\sim C41-C43
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C55)=Sof(H551)=Sof(H552)=Sof(H553)=Sof(C56)=Sof(H561)=Sof(H562)=Sof(H563)=
 Sof(C57)=Sof(H571)=Sof(H572)=Sof(H573)=1-FVAR(1)
 Sof(C35)=Sof(H351)=Sof(H352)=Sof(H353)=Sof(C36)=Sof(H361)=Sof(H362)=Sof(H363)=
 Sof(C37)=Sof(H371)=Sof(H372)=Sof(H373)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H81,H82), C28(H281,H282), C41(H411,H412), C42(H421,H422), C43(H431,H432),
 C44(H441,H442), C45(H451,H452), C46(H461,H462)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C23(H23), C25(H25)
6.c Idealised Me refined as rotating group:
 C11(H111,H112,H113), C12(H121,H122,H123), C13(H131,H132,H133), C15(H151,H152,
 H153), C16(H161,H162,H163), C17(H171,H172,H173), C18(H181,H182,H183), C19(H191,
 H192,H193), C31(H311,H312,H313), C32(H321,H322,H323), C33(H331,H332,H333),
 C35(H351,H352,H353), C36(H361,H362,H363), C37(H371,H372,H373), C55(H551,H552,
 H553), C56(H561,H562,H563), C57(H571,H572,H573), C38(H381,H382,H383), C39(H391,
 H392,H393)
;
_shelx_res_checksum              90282
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a nylon loop'
_olex2_submission_original_sample_id JSA-TD11
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.764