[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_7710091
_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(C36 H24 N6 Ru), 2(C5 Fe N6 O), 5(H2 O)'
_chemical_formula_sum            'C82 H58 Fe2 N24 O7 Ru2'
_chemical_formula_weight         1805.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-23
_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                 100.7720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.99130(10)
_cell_length_b                   19.6017(2)
_cell_length_c                   19.5329(2)
_cell_measurement_reflns_used    24046
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1770
_cell_measurement_theta_min      3.2020
_cell_volume                     3758.04(7)
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -65.00  30.00   1.00    9.00    --  -42.49  37.00-120.00   95
  2  \w   -121.00  -6.00   1.00    9.00    --  -42.49 -19.00  60.00  115
  3  \w      6.00  82.00   1.00    9.00    --   42.49 -99.00 120.00   76
  4  \w     41.00 139.00   1.00   36.00    --  111.00 -61.00-180.00   98
  5  \w     36.00 109.00   1.00   36.00    --  111.00-111.00  90.00   73
  6  \w    103.00 178.00   1.00   36.00    --  111.00  77.00   0.00   75
  7  \w     87.00 178.00   1.00   36.00    --  111.00  45.00 -90.00   91
  8  \w     40.00 135.00   1.00   36.00    --  111.00 -45.00   0.00   95
  9  \w    103.00 178.00   1.00   36.00    --  111.00  77.00 -30.00   75
 10  \w     87.00 178.00   1.00   36.00    --  111.00  30.00 120.00   91
 11  \w     37.00 142.00   1.00   36.00    --  111.00 -77.00  30.00  105
 12  \w     66.00 178.00   1.00   36.00    --  111.00  15.00  60.00  112
 13  \w    103.00 178.00   1.00   36.00    --  111.00  77.00 -60.00   75
 14  \w     36.00 109.00   1.00   36.00    --  111.00-111.00 150.00   73
 15  \w   -113.00 -16.00   1.00    9.00    --  -42.49 -57.00-150.00   97
 16  \w    -87.00  -6.00   1.00    9.00    --  -42.49 125.00 -30.00   81
 17  \w   -113.00 -16.00   1.00    9.00    --  -42.49 -57.00  30.00   97
 18  \w   -113.00 -16.00   1.00    9.00    --  -42.49 -57.00 -60.00   97
 19  \w     87.00 178.00   1.00   36.00    --  111.00  30.00-180.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409167000
_diffrn_orient_matrix_UB_12      0.0253104000
_diffrn_orient_matrix_UB_13      0.0757287000
_diffrn_orient_matrix_UB_21      0.1406371000
_diffrn_orient_matrix_UB_22      0.0213269000
_diffrn_orient_matrix_UB_23      -0.0143513000
_diffrn_orient_matrix_UB_31      -0.0564637000
_diffrn_orient_matrix_UB_32      0.0712442000
_diffrn_orient_matrix_UB_33      -0.0225567000
_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  0.0223
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38937
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_min         3.223
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.849
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.540
_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    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         7691
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0317P)^2^+2.1601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7219
_reflns_number_total             7691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00398h2.cif
_cod_data_source_block           hadi2104
_cod_database_code               7710091
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.494
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H,H,H) groups
2. Restrained distances
 O4A-H4AA_$2
 0.82 with sigma of 0.01
 O4A-H4AB
 0.82 with sigma of 0.01
 H4AA-H4AB
 1.32 with sigma of 0.01
 N12B-N12A
 0.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O4A \\sim O4B: within 3A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 3A
N12A \\sim N12B: within 3A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 3A
4. Others
 Sof(N12B)=Sof(O1B)=1-FVAR(1)
 Sof(N12A)=Sof(O1A)=FVAR(1)
 Fixed Sof: O4A(0.25) O4B(0.25) H4AA(0.25) H4AB(0.25) H4BA(0.25) H4BB(0.25)
5.a Free rotating group:
 O4B(H4AA,H4AB,H4BA,H4BB)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              77684