Inner-sphere electron transfer at the ruthenium-azo interface
Lahiri, Goutam Kumar; Panda, Sanjib; Huang, Kuo-Wei; Singh, Aditi; Dey, Sanchaita; Dalton Transactions  (2022) –; doi:10.1039/D1DT03934B

data_7709280
_publ_section_title
;
 Inner-sphere electron transfer at the ruthenium-azo interface
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03934B
_journal_year                    2022
_chemical_formula_moiety         'C26 H28 N6 O4 Ru, C6 H6'
_chemical_formula_sum            'C32 H34 N6 O4 Ru'
_chemical_formula_weight         667.72
_chemical_name_systematic        C32H35N6O4Ru
_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
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-15 deposited with the CCDC.	2022-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                104.342(2)
_cell_angle_beta                 98.741(2)
_cell_angle_gamma                94.354(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0985(3)
_cell_length_b                   12.2520(3)
_cell_length_c                   12.9961(3)
_cell_measurement_reflns_used    13676
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.7320
_cell_measurement_theta_min      3.5490
_cell_volume                     1528.89(7)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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   -191.00 -11.00   1.00    8.00    -- -101.00   0.00 -36.00  180
  2  \w   -122.00  40.00   1.00    8.00    --  -32.00   0.00 108.00  162
  3  \w   -107.00 -11.00   1.00    8.00    -- -101.00  72.00-180.00   96
  4  \w    -97.00 -11.00   1.00    8.00    -- -101.00  72.00  36.00   86
  5  \w   -104.00 -23.00   1.00    8.00    -- -101.00  72.00 -72.00   81
  6  \w   -104.00 -21.00   1.00    8.00    -- -101.00  72.00 108.00   83
  7  \w    -66.00 -18.00   1.00    8.00    --  -32.00  72.00 -36.00   48
  8  \w    -94.00 -22.00   1.00    8.00    -- -101.00  72.00   0.00   72
  9  \w    -65.00 -12.00   1.00    8.00    --  -32.00  72.00 144.00   53
 10  \w   -100.00 -23.00   1.00    8.00    -- -101.00  72.00-108.00   77
 11  \w   -115.00 -34.00   1.00    8.00    -- -101.00  43.00-180.00   81
 12  \w   -171.00-112.00   1.00    8.00    -- -101.00 -72.00-180.00   59
 13  \w    -97.00 -22.00   1.00    8.00    -- -101.00  72.00-144.00   75
 14  \w    -97.00 -67.00   1.00    8.00    -- -101.00  72.00 -36.00   30
 15  \w    -30.00   0.00   1.00    8.00    --  -32.00 -72.00 -36.00   30
 16  \w    -99.00 -68.00   1.00    8.00    -- -101.00  72.00 144.00   31
 17  \w   -191.00 -67.00   1.00    8.00    -- -101.00 -72.00  72.00  124
 18  \w   -191.00 -67.00   1.00    8.00    -- -101.00 -72.00 144.00  124
 19  \w   -135.00 -42.00   1.00    8.00    -- -101.00  72.00  72.00   93
 20  \w   -122.00 -21.00   1.00    8.00    --  -32.00   0.00-180.00  101
;
_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      0.1428978000
_diffrn_orient_matrix_UB_12      -0.0178343000
_diffrn_orient_matrix_UB_13      0.0490100000
_diffrn_orient_matrix_UB_21      -0.0086063000
_diffrn_orient_matrix_UB_22      0.0885783000
_diffrn_orient_matrix_UB_23      0.1053188000
_diffrn_orient_matrix_UB_31      -0.0605693000
_diffrn_orient_matrix_UB_32      -0.0944461000
_diffrn_orient_matrix_UB_33      0.0442657000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16587
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        64.995
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38098
_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            'metallic blackish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0984P)^2^+0.0273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4863
_reflns_number_total             5113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03934b2.cif
_cod_data_source_block           1
_cod_database_code               7709280
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H13N4O8Ru
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.624
_reflns_odcompleteness_completeness 96.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.64
_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.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C24(H24), C3(H3), C11(H11), C4(H4), C5(H5), C14(H14), C6(H6),
 C12(H12), C13(H13), C28(H28), C32(H32), C29(H29), C31(H31), C27(H27), C30(H30)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              65318
_shelx_hkl_checksum              42125
_olex2_submission_special_instructions 'No special instructions were received'
_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 2.819
_oxdiff_exptl_absorpt_empirical_full_min 0.501