Remarkable Stability of a Molecular Ruthenium Complex in PEM Water Electrolysis
Bellini, Marco; Bösken, Jonas; Bartoli, Francesco; Miller, Hamish; Thöny, Debora; Poggini, Lorenzo; Wörle, Michael; Oberhauser, Werner; Gamboa-Carballo, Juan José; Lavacchi, Alessandro; Krumeich, Frank; Grützmacher, Hansjörg; Vizza, Francesco; Chemical Science  (2022) –; doi:10.1039/D1SC07234J

data_1566538
_publ_section_title
;
 Remarkable Stability of a Molecular Ruthenium Complex in PEM Water
 Electrolysis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC07234J
_journal_year                    2022
_chemical_formula_moiety         'C36 H35 N2 O Ru2, B F4'
_chemical_formula_sum            'C36 H35 B F4 N2 O Ru2'
_chemical_formula_weight         800.61
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                78.9600(10)
_cell_angle_beta                 76.8190(10)
_cell_angle_gamma                85.7730(10)
_cell_formula_units_Z            2
_cell_length_a                   9.54690(10)
_cell_length_b                   10.1082(2)
_cell_length_c                   17.4002(3)
_cell_measurement_reflns_used    25413
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      79.5270
_cell_measurement_theta_min      2.6480
_cell_volume                     1603.87(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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 -32.00   0.50    1.24    --  -26.00 162.00 172.10  128
  2  \w      2.00  34.00   0.50    1.24    --   34.00  94.00 103.24   64
  3  \w     30.00  55.00   0.50    1.24    --   54.00  77.00  61.45   50
  4  \w     33.00  63.00   0.50    1.24    --   48.62  57.00   0.00   60
  5  \w     45.00  72.00   0.50    1.24    --   48.62  38.00  30.00   54
  6  \w     83.00 116.00   0.50    1.24    --   48.62  38.00  30.00   66
  7  \w     86.00 113.00   0.50    1.24    --   74.00  73.00  21.28   54
  8  \w     93.00 145.00   0.50    4.94    --   82.00  78.00 103.89  104
  9  \w    116.00 152.00   0.50    4.94    --   86.00  75.00 137.15   72
 10  \w    147.00 174.00   0.50    4.94    --  110.00  77.00  90.00   54
 11  \w    153.00 178.00   0.50    4.94    --  110.00  57.00  60.00   50
 12  \w    149.00 176.00   0.50    4.94    --  110.00  77.00 120.00   54
 13  \w    131.00 175.00   0.50    4.94    --  110.00  77.00  30.00   88
 14  \w    137.00 162.00   0.50    4.94    --  102.00  75.00-132.95   50
 15  \w    111.00 151.00   0.50    4.94    --   86.00  77.00-161.51   80
 16  \w     97.00 161.00   0.50    4.94    --  110.00  57.00 -60.00  128
 17  \w     94.00 178.00   0.50    4.94    --  110.00  57.00   0.00  168
 18  \w     99.00 176.00   0.50    4.94    --  110.00  45.00  83.05  154
 19  \w     94.00 142.00   0.50    4.94    --  110.00  57.00  30.00   96
 20  \w     86.00 129.00   0.50    4.94    --  110.00  77.00  90.00   86
 21  \w     87.00 121.00   0.50    4.94    --  110.00  77.00  30.00   68
 22  \w     97.00 143.00   0.50    4.94    --  110.00  57.00  60.00   92
 23  \w     95.00 175.00   0.50    4.94    --  110.00  57.00 -30.00  160
 24  \w     95.00 177.00   0.50    4.94    --  110.00  57.00 -90.00  164
 25  \w     82.00 133.00   0.50    4.94    --  102.00  75.00-132.95  102
 26  \w     90.00 176.00   0.50    4.94    --  110.00  77.00-180.00  172
 27  \w     86.00 116.00   0.50    4.94    --  110.00  77.00-150.00   60
 28  \w     87.00 176.00   0.50    4.94    --  110.00  77.00-120.00  178
 29  \w     87.00 112.00   0.50    4.94    --  110.00  77.00 -30.00   50
 30  \w     69.00 120.00   0.50    4.94    --   86.00  67.00  40.31  102
 31  \w     87.00 141.00   0.50    4.94    --  110.00  77.00 120.00  108
 32  \w     86.00 174.00   0.50    4.94    --  110.00  77.00 150.00  176
 33  \w     73.00 106.00   0.50    4.94    --   90.00  60.00 -48.59   66
 34  \w     52.00  82.00   0.50    1.24    --   74.00  73.00  21.28   60
 35  \w     53.00  88.00   0.50    1.24    --   74.00  74.00 -24.86   70
 36  \w     51.00  86.00   0.50    1.24    --   74.00  77.00 -88.70   70
 37  \w     63.00 102.00   0.50    4.94    --   86.00  77.00-161.51   78
 38  \w     26.00  51.00   0.50    1.24    --   48.62  77.00-120.00   50
 39  \w     31.00  57.00   0.50    1.24    --   54.00  79.00 -56.30   52
 40  \w     36.00  93.00   0.50    1.24    --   48.62  38.00   0.00  114
 41  \w     58.00  83.00   0.50    4.94    --   82.00  78.00 103.89   50
 42  \w     63.00  96.00   0.50    4.94    --   86.00  75.00 137.15   66
 43  \w     45.00  78.00   0.50    1.24    --   70.00  80.00 149.34   66
 44  \w     34.00  60.00   0.50    1.24    --   58.00  79.00 161.93   52
 45  \w     34.00  93.00   0.50    1.24    --   58.00  79.00  89.01  118
 46  \w     27.00  52.00   0.50    1.24    --   48.62  77.00  30.00   50
 47  \w     62.00 120.00   0.50    1.24    --   48.62 178.00-150.00  116
 48  \w     39.00  68.00   0.50    4.94    --  110.00 -57.00 120.00   58
 49  \w     49.00  90.00   0.50    4.94    --  110.00 -99.00 150.00   82
 50  \w     75.00 112.00   0.50    4.94    --  110.00-125.00 120.00   74
 51  \w     48.00  74.00   0.50    4.94    --  110.00-125.00 120.00   52
 52  \w     40.00 104.00   0.50    4.94    --  110.00 -99.00 -30.00  128
 53  \w     81.00 106.00   0.50    4.94    --  110.00 -99.00-120.00   50
 54  \w     49.00 134.00   0.50    4.94    --  110.00 -77.00 -30.00  170
 55  \w     49.00  80.00   0.50    1.24    --   48.62 -99.00 -60.00   62
 56  \w     12.00  37.00   0.50    1.24    --   48.62 -99.00 -60.00   50
 57  \w     41.00  91.00   0.50    4.94    --  110.00 -99.00 -90.00  100
 58  \w     40.00 113.00   0.50    4.94    --  110.00-127.00-131.00  146
 59  \w     44.00  76.00   0.50    4.94    --  110.00 -99.00-120.00   64
 60  \w    -70.00 -35.00   0.50    1.24    --  -48.62 -19.00 -60.00   70
 61  \w    -65.00 -33.00   0.50    1.24    --  -48.62 -57.00 -60.00   64
 62  \w    -72.00 -47.00   0.50    4.94    --  -70.00 -77.00 -17.21   50
 63  \w    -66.00 -38.00   0.50    1.24    --  -48.62 -57.00  30.00   56
 64  \w    -72.00 -47.00   0.50    4.94    --  -70.00 -77.00  60.00   50
 65  \w    -90.00 -47.00   0.50    4.94    --  -70.00 -74.00 147.98   86
 66  \w    -88.00 -48.00   0.50    4.94    --  -70.00 -73.00 174.56   80
 67  \w    -71.00 -46.00   0.50    4.94    --  -70.00 -77.00  90.00   50
 68  \w    -73.00 -48.00   0.50    4.94    --  -70.00 -75.00 120.69   50
 69  \w    -81.00 -47.00   0.50    4.94    --  -70.00 -74.00  -5.28   68
 70  \w    -72.00 -46.00   0.50    4.94    --  -70.00 -77.00 -90.00   52
 71  \w    -78.00 -47.00   0.50    4.94    --  -70.00 -77.00-150.00   62
 72  \w    -78.00 -46.00   0.50    4.94    --  -70.00 -77.00-120.00   64
 73  \w    -82.00 -47.00   0.50    4.94    --  -70.00 -77.00 -60.00   70
 74  \w   -117.00 -85.00   0.50    1.24    --  -48.62 -19.00 -60.00   64
 75  \w   -122.00 -39.00   0.50    1.24    --  -48.62 -32.00-139.47  166
 76  \w   -112.00 -87.00   0.50    4.94    --  -70.00 -77.00 -60.00   50
 77  \w   -115.00 -72.00   0.50    1.24    --  -48.62-178.00   0.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40297
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.898
_diffrn_reflns_theta_min         2.651
_exptl_absorpt_coefficient_mu    8.098
_exptl_absorpt_correction_T_max  0.81358
_exptl_absorpt_correction_T_min  0.80674
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       sphere
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.017
_refine_diff_density_max         2.470
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+9.1077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6324
_reflns_number_total             6799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc07234j2.cif
_cod_data_source_block           lac110920_1_1
_cod_database_code               1566538
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ru1-H1A \\sim Ru1-H1B
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10), C21(H21), C22(H22), C25(H25), C26(H26)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36)
3.d Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              81459
_shelx_hkl_checksum              71797
_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
;