An insight into the redox activity of Ru and Os complexes of the N,N′-bis(2-pyridyl)benzene-1,2-diamine ligand: Structural, electrochemical and electronic structure analysis by density functional theory calculations
Deka, Rajesh; Junk, Peter C.; Turner, David R.; Deacon, Glen B.; Singh, Harkesh B.; Inorganica Chimica Acta 499 (2020) 119193–; doi:10.1016/j.ica.2019.119193

data_1565712
_publ_section_title
;
 An insight into the redox activity of Ru and Os complexes of the
 N,N&#x2032;-bis(2-pyridyl)benzene-1,2-diamine ligand: Structural,
 electrochemical and electronic structure analysis by density functional
 theory calculations
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119193
_journal_paper_doi               10.1016/j.ica.2019.119193
_journal_volume                  499
_journal_year                    2020
_chemical_formula_moiety         'C26 H26 N4 O4 Ru'
_chemical_formula_sum            'C26 H26 N4 O4 Ru'
_chemical_formula_weight         559.58
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.6783(2)
_cell_length_b                   10.6783(2)
_cell_length_c                   37.8191(7)
_cell_measurement_reflns_used    41145
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.1180
_cell_measurement_theta_min      2.1980
_cell_volume                     3734.62(12)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_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   -110.00  25.00   0.50    8.00    --  -20.00   0.00-180.00  270
  2  \w   -110.00  10.00   0.50    8.00    --  -20.00 -72.00-180.00  240
  3  \w    -70.00  19.00   0.50    8.00    --  -20.00 -72.00 -36.00  178
  4  \w    -43.50   1.00   0.50    8.00    --  -20.00  72.00 108.00   89
  5  \w    -44.00 -14.00   0.50    8.00    --  -20.00 -72.00-108.00   60
  6  \w   -110.00  44.00   0.50    8.00    --  -20.00   0.00-108.00  308
  7  \w    -61.00  19.00   0.50    8.00    --  -20.00 -72.00  36.00  160
  8  \w    -59.00  25.50   0.50    8.00    --  -20.00  72.00-108.00  169
  9  \w    -50.50   2.00   0.50    8.00    --  -20.00  72.00 -36.00  105
 10  \w    -42.00 -10.00   0.50    8.00    --  -20.00  72.00-180.00   64
 11  \w    -94.00  70.00   0.50    8.00    --  -20.00   0.00 -36.00  328
 12  \w    -62.00 -52.00   0.50    8.00    --  -20.00 -72.00 108.00   20
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            70939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.202
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic intense grey'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       needle
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 2016 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4377
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0423P)^2^+1.6138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4258
_reflns_number_total             4377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3734.62(16)
_cod_database_code               1565712
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C17B) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C17B) = Uanis(C17A)
3. Others
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C24(H24)
4.b Idealised Me refined as rotating group:
 C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C26(H26A,H26B,H26C)
;