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_1565714
_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         'C36 H29 N8 Os, Cl O4, 1.5(C6 H6)'
_chemical_formula_sum            'C45 H38 Cl N8 O4 Os'
_chemical_formula_weight         980.48
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                67.070(2)
_cell_angle_beta                 76.321(2)
_cell_angle_gamma                67.853(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8605(2)
_cell_length_b                   13.5233(3)
_cell_length_c                   14.3278(3)
_cell_measurement_reflns_used    15215
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1630
_cell_measurement_theta_min      2.2090
_cell_volume                     1949.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  70.00   0.50    8.00    --  -20.00   0.00 -36.00  360
  2  \w    -63.00  19.00   0.50    8.00    --  -20.00 -72.00 108.00  164
  3  \w    -69.00  19.00   0.50    8.00    --  -20.00 -72.00 -36.00  176
  4  \w    -34.50   3.00   0.50    8.00    --  -20.00 -72.00-180.00   75
  5  \w    -59.00 -44.50   0.50    8.00    --  -20.00  72.00 -36.00   29
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172481000
_diffrn_orient_matrix_UB_12      0.0354330000
_diffrn_orient_matrix_UB_13      -0.0486182000
_diffrn_orient_matrix_UB_21      0.0600600000
_diffrn_orient_matrix_UB_22      -0.0392263000
_diffrn_orient_matrix_UB_23      0.0008968000
_diffrn_orient_matrix_UB_31      -0.0176285000
_diffrn_orient_matrix_UB_32      -0.0285453000
_diffrn_orient_matrix_UB_33      -0.0236024000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0367P)^2^+2.1352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6370
_reflns_number_total             6844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           3
_cod_database_code               1565714
_reflns_odcompleteness_completeness 88.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.04
_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:
 C00B(H00B), C00E(H00E), N00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C012(H012), C013(H013), C014(H014), C015(H015),
 C016(H016), C017(H017), C018(H018), C01A(H01A), C01B(H01B), C01C(H01C),
 C01D(H01D), C01F(H01F), C01H(H01H), C01J(H01J), C01K(H01K), C1(H1), C2(H2),
 C3(H3)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.827