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_7709282
_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'
_chemical_formula_sum            'C36 H42 N6 O8 Ru2'
_chemical_formula_weight         888.89
_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             2020-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2022-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                68.586(2)
_cell_angle_beta                 89.761(2)
_cell_angle_gamma                76.019(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6157(2)
_cell_length_b                   11.8944(3)
_cell_length_c                   15.6228(3)
_cell_measurement_reflns_used    25230
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1070
_cell_measurement_theta_min      1.8440
_cell_volume                     1941.48(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  20.08   0.50    3.00  20.13  -8.96 -59.24    --   720
  2  \w    -69.41 -12.41   0.50    3.00    --   -9.01 114.06 164.95  114
  3  \w    -50.81  25.69   0.50    3.00    --   -9.01  80.44 -27.87  153
  4  \w   -104.62  19.88   0.50    3.00    --   -8.96 -59.25 -51.92  249
  5  \w    -52.62  22.38   0.50    3.00    --   -9.01  83.69  57.22  150
  6  \w   -104.62  19.88   0.50    3.00    --   -8.96 -59.25 164.08  249
  7  \f   -349.73   8.77   0.50    3.00  13.43  -8.96 -31.50    --   717
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0102150000
_diffrn_orient_matrix_UB_12      0.0435579000
_diffrn_orient_matrix_UB_13      -0.0463019000
_diffrn_orient_matrix_UB_21      0.0532904000
_diffrn_orient_matrix_UB_22      -0.0341325000
_diffrn_orient_matrix_UB_23      -0.0106910000
_diffrn_orient_matrix_UB_31      -0.0324089000
_diffrn_orient_matrix_UB_32      -0.0365110000
_diffrn_orient_matrix_UB_33      -0.0118716000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            81212
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.308
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.602
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         12094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0450P)^2^+4.2137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9466
_reflns_number_total             12094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03934b2.cif
_cod_data_source_block           2
_cod_database_code               7709282
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N6O8Ru2
_reflns_odcompleteness_completeness 87.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.24
_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:
 C11(H11), C14(H14), C29(H29), C13(H13), C3(H3), C12(H12), C34(H34), C19(H19),
 C24(H24), C6(H6), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C16(H16A,H16B,
 H16C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C26(H26A,
 H26B,H26C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84508
_shelx_hkl_checksum              85902
_shelx_fab_checksum              12730
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.705