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_7720390
_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         'C21 H34 Cl2 N O3 Re S'
_chemical_formula_sum            'C21 H34 Cl2 N O3 Re S'
_chemical_formula_weight         637.65
_chemical_name_systematic
'(2,4-t-butyl-6-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenolato)-dichlorido-(dimethyl sulfide)-oxido-rhenium(v)'
_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             2025-09-25
_audit_creation_method
;
Olex2 1.5-ac7-018
(compiled 2025.08.06 svn.rb7424aed for Rigaku Oxford Diffraction, GUI svn.r7314)
;
_audit_update_record
;
2025-11-04 deposited with the CCDC.	2026-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                67.984(2)
_cell_angle_beta                 83.086(2)
_cell_angle_gamma                89.813(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0035(2)
_cell_length_b                   11.1092(2)
_cell_length_c                   12.0885(3)
_cell_measurement_reflns_used    27083
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      33.7820
_cell_measurement_theta_min      2.7740
_cell_volume                     1235.11(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -7.00  46.00   0.50    4.00    --    9.08 -99.00 150.00  106
  2  \w     -8.00  60.00   0.50    4.00    --    9.08  57.00  90.00  136
  3  \w    -60.00   6.00   0.50    4.00    --  -10.95 -57.00-120.00  132
  4  \w    -48.00  66.00   0.50    4.00    --  -10.95  19.00  60.00  228
  5  \w    -25.00  14.00   0.50    4.00    --  -10.95 -77.00  60.00   78
  6  \w     -7.00  26.00   0.50    4.00    --  -10.95 -99.00 150.00   66
  7  \w    -60.00   6.00   0.50    4.00    --  -10.95 -57.00 150.00  132
  8  \w    -48.00  66.00   0.50    4.00    --  -10.95  19.00  60.00  228
  9  \w    -35.00  25.00   0.50    4.00    --  -10.95  77.00   0.00  120
 10  \w    -88.00   5.00   0.50    4.00    --  -10.95 -19.00-150.00  186
 11  \w    -25.00  34.00   0.50    4.00    --    9.08 -77.00 -90.00  118
 12  \w    -35.00 -10.00   0.50    4.00    --  -10.95  77.00-180.00   50
;
_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      0.0494143000
_diffrn_orient_matrix_UB_12      -0.0203711000
_diffrn_orient_matrix_UB_13      0.0399059000
_diffrn_orient_matrix_UB_21      0.0417371000
_diffrn_orient_matrix_UB_22      0.0554422000
_diffrn_orient_matrix_UB_23      -0.0367961000
_diffrn_orient_matrix_UB_31      -0.0304670000
_diffrn_orient_matrix_UB_32      0.0355534000
_diffrn_orient_matrix_UB_33      0.0335643000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.241
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.142a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloroethane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0060P)^2^+3.3327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6990
_reflns_number_total             7537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00039h2.cif
_cod_data_source_block           ad124
_cod_depositor_comments
'Adding full bibliography for 7720387--7720392.cif.'
_cod_database_code               7720390
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C21 H34 N1 O3 S1 Cl2 Re1 '
_chemical_oxdiff_usercomment     JSA-COR-C2A
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.420
_diffrn_oxdiff_digest_hkl
;
439206172f8de7583aab4460eb2ab2c4ce9790
;
_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:
 C8(H81,H82)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
2.c Idealised Me refined as rotating group:
 C10(H101,H102,H103), C11(H111,H112,H113), C13(H131,H132,H133), C14(H141,H142,
 H143), C15(H151,H152,H153), C17(H171,H172,H173), C18(H181,H182,H183), C19(H191,
 H192,H193), C20(H201,H202,H203), C21(H211,H212,H213)
;
_shelx_res_checksum              67752
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MiTeGen loop'
_olex2_submission_original_sample_id JSA-COR-C2A
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.885