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_1565713
_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         'C37 H27 Cl N7 Ru'
_chemical_formula_sum            'C37 H27 Cl N7 Ru'
_chemical_formula_weight         706.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 97.376(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4893(9)
_cell_length_b                   29.335(2)
_cell_length_c                   24.2604(17)
_cell_measurement_reflns_used    3948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6310
_cell_measurement_theta_min      2.1840
_cell_volume                     8109.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  39.00   0.50    8.00    --  -20.00   0.00-180.00  298
  2  \w    -94.00  59.00   0.50    8.00    --  -20.00   0.00 -36.00  306
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.1321
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22929
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.626
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01524
_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            purple
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       prism
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.00053(18)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6979
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1563P)^2^+2.0681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.2968
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4036
_reflns_number_total             6979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           2
_cod_original_cell_volume        8109.1(11)
_cod_database_code               1565713
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C29(H29), C30(H30), C28(H28), C17(H17), C23(H23), C31(H31),
 C33(H33), C18(H18), C34(H34), C20(H20), C37(H37), C35(H35), C36(H36), C11(H11),
  C2(H2), C10(H10), C3(H3), C5(H5), C19(H19), C4(H4), C16(H16), C15(H15),
 C13(H13), C8(H8), C14(H14), C9(H9)
;