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_7709281
_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         'C36 H42 N6 O8 Ru2, Cl O4'
_chemical_formula_sum            'C36 H42 Cl N6 O12 Ru2'
_chemical_formula_weight         988.34
_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
_audit_creation_date             2021-03-05
_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                90
_cell_angle_beta                 91.1157(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.4670(4)
_cell_length_b                   18.9358(3)
_cell_length_c                   15.8522(3)
_cell_measurement_reflns_used    11962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.8910
_cell_measurement_theta_min      2.8010
_cell_volume                     8243.3(2)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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   -182.00 -77.00   1.00    4.00    -- -101.00 -72.00  36.00  105
  2  \w    -66.00  58.00   1.00    4.00    --  -32.00  72.00 108.00  124
  3  \w   -124.00 -11.00   1.00    4.00    -- -101.00  72.00 -36.00  113
  4  \w   -127.00 -34.00   1.00    4.00    -- -101.00  72.00-180.00   93
  5  \w   -153.00 -29.00   1.00    4.00    -- -101.00   0.00  36.00  124
  6  \w    -89.00   1.00   1.00    4.00    --  -32.00 -72.00-180.00   90
  7  \w   -178.00 -90.00   1.00    4.00    -- -101.00 -72.00 108.00   88
  8  \w   -106.00 -75.00   1.00    4.00    -- -101.00  72.00 108.00   31
  9  \w   -109.00 -68.00   1.00    4.00    -- -101.00  72.00-108.00   41
 10  \w   -135.00 -33.00   1.00    4.00    -- -101.00  72.00  36.00  102
 11  \w   -169.00 -67.00   1.00    4.00    -- -101.00 -72.00-108.00  102
 12  \w    -85.00  29.00   1.00    4.00    --  -32.00   0.00-180.00  114
 13  \w   -173.00 -86.00   1.00    4.00    -- -101.00 -72.00 -36.00   87
 14  \w    -66.00 -22.00   1.00    4.00    --  -32.00  72.00-108.00   44
 15  \w   -160.00-128.00   1.00    4.00    -- -101.00   0.00-108.00   32
 16  \w    -57.00 -13.00   1.00    4.00    --  -32.00 -72.00 108.00   44
 17  \w   -122.00 -67.00   1.00    4.00    -- -101.00 -72.00-180.00   55
 18  \w    -49.00 -19.00   1.00    4.00    --  -32.00 -72.00  36.00   30
 19  \w   -191.00 -11.00   1.00    4.00    -- -101.00   0.00 -36.00  180
 20  \w    -66.00  58.00   1.00    4.00    --  -32.00  72.00-180.00  124
 21  \w    -50.00 -49.00   1.00    4.00    --  -32.00  72.00  36.00    1
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0375905000
_diffrn_orient_matrix_UB_12      0.0603629000
_diffrn_orient_matrix_UB_13      0.0029022000
_diffrn_orient_matrix_UB_21      0.0416303000
_diffrn_orient_matrix_UB_22      -0.0544002000
_diffrn_orient_matrix_UB_23      -0.0018130000
_diffrn_orient_matrix_UB_31      -0.0007668000
_diffrn_orient_matrix_UB_32      0.0028142000
_diffrn_orient_matrix_UB_33      -0.0972053000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44211
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        64.981
_diffrn_reflns_theta_max         64.981
_diffrn_reflns_theta_min         2.835
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34742
_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 dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1142P)^2^+12.8473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5503
_reflns_number_total             6940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03934b2.cif
_cod_data_source_block           '[2]ClO4'
_cod_database_code               7709281
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNORuCl
_reflns_odcompleteness_completeness 96.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.70
_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:
 C14(H14), C11(H11), C12(H12), C13(H13), C29(H29), C6(H6), C3(H3), C24(H24),
 C5(H5), C4(H4), C34(H34), C19(H19)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C8(H8A,H8B,
 H8C), C22(H22A,H22B,H22C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C21(H21A,
 H21B,H21C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              99141
_shelx_hkl_checksum              89544
_shelx_fab_checksum              85094
_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 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.414