The role of [Re(η6-arene)2]+ substituents in electro- and photocatalytic water reduction with [Co(terpy)2]3+ catalysts
Csucker, Joshua; Grundmann, Nora Sophie; Blacque, Olivier; Spingler, Bernhard; Alberto, Roger; Catalysis Science & Technology 15 (2025) 1627–1633; doi:10.1039/D4CY01282H

data_1573724
_publ_section_title
;
 The role of [Re(\h6-arene)2]+ substituents in electro- and photocatalytic
 water reduction with [Co(terpy)2]3+ catalysts
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1627
_journal_page_last               1633
_journal_paper_doi               10.1039/D4CY01282H
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C54 H44 Co N8 Re2, 4(F6 P)'
_chemical_formula_sum            'C54 H44 Co F24 N8 P4 Re2'
_chemical_formula_weight         1816.18
_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             2024-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-16 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1273(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.24728(16)
_cell_length_b                   27.2919(6)
_cell_length_c                   24.3585(4)
_cell_measurement_reflns_used    14877
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      78.2700
_cell_measurement_theta_min      3.2350
_cell_volume                     6122.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_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      159.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.950
_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    -96.00 -64.00   0.50    6.00    --  -50.79-143.00 -20.00   64
  2  \w    -75.00 -50.00   0.50    6.00    --  -50.79 127.00-135.00   50
  3  \w   -120.00 -80.00   0.50    6.00    --  -50.79-127.00 149.00   80
  4  \w     56.00  94.00   0.50    6.00    --   50.79-127.00 149.00   76
  5  \w     56.00 105.00   0.50    6.00    --   50.79-143.00 -20.00   98
  6  \w   -108.00 -82.00   0.50   24.00    --  -90.00-143.00 -20.00   52
  7  \w    -78.00 -53.00   0.50   24.00    --  -90.00 127.00-135.00   50
  8  \w     84.00 125.00   0.50   24.00    --  111.50-143.00 -20.00   82
  9  \w     77.00 112.00   0.50   24.00    --  111.50-127.00 149.00   70
 10  \w     53.00  79.00   0.50   24.00    --  111.50-143.00 -20.00   52
 11  \w     44.00  72.00   0.50   24.00    --  111.50-127.00 149.00   56
 12  \w    111.00 137.00   0.50   24.00    --  111.50 127.00-135.00   52
 13  \w    -24.00  20.00   0.50    6.00    --  -50.79  19.00-180.00   88
 14  \w    -26.00  21.00   0.50    6.00    --  -50.79  19.00 -90.00   94
 15  \w    -25.00  21.00   0.50    6.00    --  -50.79  19.00 -30.00   92
 16  \w    -70.00 -44.00   0.50    6.00    --  -50.79 143.00  33.00   52
 17  \w     -8.00  26.00   0.50    6.00    --   50.79 -19.00  60.00   68
 18  \w   -135.00 -94.00   0.50   24.00    --  -90.00   0.00   0.00   82
 19  \w    107.00 134.00   0.50   24.00    --  111.50  15.00 150.00   54
 20  \w    122.00 177.00   0.50   24.00    --  111.50  45.00 -30.00  110
 21  \w     41.00  71.00   0.50   24.00    --  111.50 -77.00 120.00   60
 22  \w     42.00 104.00   0.50   24.00    --  111.50 -95.00 -30.00  124
 23  \w     41.00 106.00   0.50   24.00    --  111.50 -95.00 150.00  130
 24  \w    131.00 158.00   0.50   24.00    --  111.50  61.00 150.00   54
 25  \w    122.00 158.00   0.50   24.00    --  111.50  45.00 -60.00   72
 26  \w     65.00  91.00   0.50   24.00    --  111.50 -95.00-180.00   52
 27  \w     66.00 103.00   0.50   24.00    --  111.50 -95.00 -60.00   74
 28  \w     44.00  70.00   0.50   24.00    --  111.50 -61.00   0.00   52
 29  \w     50.00  98.00   0.50   24.00    --  111.50 -77.00   0.00   96
 30  \w     41.00  68.00   0.50   24.00    --  111.50 -61.00 -90.00   54
 31  \w     44.00  70.00   0.50   24.00    --  111.50 -61.00-180.00   52
 32  \w     64.00 117.00   0.50   24.00    --  111.50   0.00 -30.00  106
 33  \w    128.00 163.00   0.50   24.00    --  111.50  61.00-180.00   70
 34  \w     44.00  69.00   0.50   24.00    --  111.50 -61.00 -60.00   50
 35  \w     41.00  70.00   0.50   24.00    --  111.50 -61.00  30.00   58
;
_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      -0.0131125000
_diffrn_orient_matrix_UB_12      0.0560606000
_diffrn_orient_matrix_UB_13      -0.0064093000
_diffrn_orient_matrix_UB_21      0.0395337000
_diffrn_orient_matrix_UB_22      0.0062169000
_diffrn_orient_matrix_UB_23      0.0623969000
_diffrn_orient_matrix_UB_31      0.1618569000
_diffrn_orient_matrix_UB_32      0.0030733000
_diffrn_orient_matrix_UB_33      -0.0099157000
_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  0.0773
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50273
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.307
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.74a (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    1.970
_exptl_crystal_description       needle
_exptl_crystal_F_000             3508
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.698
_refine_diff_density_min         -2.803
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         12738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+9.6208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9167
_reflns_number_total             12738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cy01282h2.cif
_cod_data_source_block           '[4](PF6)4'
_cod_depositor_comments
'Adding full bibliography for 1573721--1573724.cif.'
_cod_database_code               1573724
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C54 H44 Co F24 N8 P4 Re2'
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.399
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N8(H8), C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8A),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C17(H17), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C34(H34), C36(H36), C39(H39), C40(H40), C41(H41),
 C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              79877
_shelx_hkl_checksum              48906
_shelx_fab_checksum              3191
_platon_squeeze_void_probe_radius 1.20
_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 2.127
_oxdiff_exptl_absorpt_empirical_full_min 0.512