[Ru(tmphen)<sub>3</sub>]<sub>2</sub>[Fe(CN)<sub>6</sub>] and [Ru(phen)<sub>3</sub>][Fe(CN)<sub>5</sub>(NO)] complexes and formation of a heterostructured RuO<sub>2</sub>-Fe<sub>2</sub>O<sub>3</sub> nanocomposite as an efficient alkaline HER and OER electrocatalyst.
Mosallaei, Hamta; Hadadzadeh, Hassan; Foelske, Annette; Sauer, Markus; Amiri Rudbari, Hadi; Blacque, Olivier; Dalton transactions (Cambridge, England : 2003) 51 (2022) 6314–6331; doi:10.1039/d2dt00398h

data_7710090
_publ_section_title
;
 [Ru(tmphen)<sub>3</sub>]<sub>2</sub>[Fe(CN)<sub>6</sub>] and
 [Ru(phen)<sub>3</sub>][Fe(CN)<sub>5</sub>(NO)] complexes and formation of
 a heterostructured RuO<sub>2</sub>-Fe<sub>2</sub>O<sub>3</sub>
 nanocomposite as an efficient alkaline HER and OER electrocatalyst.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6314
_journal_page_last               6331
_journal_paper_doi               10.1039/d2dt00398h
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         '2(C48 H48 N6 Ru1), C6 Fe1 N6, 8(H2 O)'
_chemical_formula_sum            'C102 H112 Fe N18 O8 Ru2'
_chemical_formula_weight         1976.08
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.3228(3)
_cell_length_b                   16.3228(3)
_cell_length_c                   32.3748(9)
_cell_measurement_reflns_used    8410
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.7170
_cell_measurement_theta_min      3.4040
_cell_volume                     7470.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -97.00 -20.00   0.50    1.84    --  -51.54 139.00-138.00  154
  2  \w    -91.00 -15.00   0.50    1.84    --  -51.54 131.00  47.00  152
  3  \w     41.00 107.00   0.50    1.84    --   51.54-139.00 161.00  132
  4  \w     37.00 102.00   0.50    1.84    --   51.54-131.00 -24.00  130
  5  \w   -158.00 -84.00   0.50    6.34    --  -86.25-139.00 161.00  148
  6  \w    107.00 158.00   0.50    6.34    --  107.75 131.00  47.00  102
  7  \w    139.00 170.00   0.50    6.34    --  107.75 139.00-138.00   62
  8  \w    -83.00 -38.00   0.50    1.84    --  -51.54 -57.00-180.00   90
  9  \w   -125.00 -76.00   0.50    1.84    --  -51.54-125.00  90.00   98
 10  \w     96.00 140.00   0.50    6.34    --  107.75  30.00 -30.00   88
 11  \w     64.00 142.00   0.50    6.34    --  107.75 178.00   0.00  156
 12  \w     63.00  90.00   0.50    6.34    --  107.75 178.00 -60.00   54
 13  \w     99.00 145.00   0.50    6.34    --  107.75 178.00 -60.00   92
 14  \w     61.00 117.00   0.50    6.34    --  107.75 -45.00 -30.00  112
 15  \w     39.00 122.00   0.50    6.34    --  107.75 -61.00 -60.00  166
 16  \w    104.00 175.00   0.50    6.34    --  107.75 111.00-120.00  142
 17  \w     98.00 145.00   0.50    6.34    --  107.75  15.00-120.00   94
 18  \w    149.00 177.00   0.50    6.34    --  107.75  15.00-120.00   56
 19  \w    107.00 176.00   0.50    6.34    --  107.75 111.00 -60.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185058000
_diffrn_orient_matrix_UB_12      -0.0188321000
_diffrn_orient_matrix_UB_13      0.0466361000
_diffrn_orient_matrix_UB_21      0.0804837000
_diffrn_orient_matrix_UB_22      0.1011326000
_diffrn_orient_matrix_UB_23      0.0093104000
_diffrn_orient_matrix_UB_31      -0.0712455000
_diffrn_orient_matrix_UB_32      0.0357601000
_diffrn_orient_matrix_UB_33      -0.0016071000
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            17962
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.481
_diffrn_reflns_theta_min         4.097
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1339P)^2^+0.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3081
_reflns_number_total             3398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00398h2.cif
_cod_data_source_block           hadi2904
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7710090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.384
_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. Others
 Fixed Sof: O1(0.25) H1A(0.25) H1B(0.25) O2(0.5) H2A(0.5) H2B(0.5) O3(0.5)
 H3A(0.5) H3B(0.5) O4(0.08333) H4A(0.08333) H4B(0.08333)
 Fixed X: H1A(0.29295) H1B(0.38345) H4A(0.36743) H4B(0.279119)
 Fixed Y: H1A(0.59966) H1B(0.63014) H4A(0.705) H4B(0.634529)
 Fixed Z: H1A(0.54185) H1B(0.52702) H4A(0.22935) H4B(0.23708)
3.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C11(H11), C12(H12)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              62830