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_7709283
_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         'C48 H42 Cu2 N18, 2(B F4)'
_chemical_formula_sum            'C48 H42 B2 Cu2 F8 N18'
_chemical_formula_weight         1171.69
_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             2021-03-06
_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                107.070(3)
_cell_angle_beta                 101.629(4)
_cell_angle_gamma                90.142(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0872(6)
_cell_length_b                   12.9737(4)
_cell_length_c                   18.0164(7)
_cell_measurement_reflns_used    6078
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.1910
_cell_measurement_theta_min      1.7130
_cell_volume                     2639.6(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -349.73  10.27   1.00    5.00  15.59  -6.80 -31.50    --   360
  2  \w   -102.46  21.54   1.00    5.00    --   -6.80 -59.25 -51.92  124
  3  \w    -72.97  19.03   1.00    5.00    --  -27.79  86.55  52.84   92
  4  \w    -49.21  23.79   1.00    5.00    --   -6.86  81.46-164.70   73
  5  \f    -10.27 349.73   1.00    5.00  84.06  -6.80  31.50    --   360
  6  \w    -65.62 -11.62   1.00    5.00    --   -6.86 111.31 -20.43   54
  7  \w   -102.46  21.54   1.00    5.00    --   -6.80 -59.25-123.92  124
  8  \f   -339.92  20.08   1.00    5.00  22.29  -6.80 -59.25    --   360
;
_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      -0.0589527000
_diffrn_orient_matrix_UB_12      -0.0032210000
_diffrn_orient_matrix_UB_13      -0.0161097000
_diffrn_orient_matrix_UB_21      -0.0082915000
_diffrn_orient_matrix_UB_22      0.0367976000
_diffrn_orient_matrix_UB_23      0.0359902000
_diffrn_orient_matrix_UB_31      0.0077995000
_diffrn_orient_matrix_UB_32      0.0438252000
_diffrn_orient_matrix_UB_33      -0.0148595000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1751
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            112347
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22474
_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            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.083
_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     773
_refine_ls_number_reflns         9294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0823P)^2^+0.8431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5946
_reflns_number_total             9294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03934b2.cif
_cod_data_source_block           Cu_[3](BF4)2
_cod_original_cell_volume        2639.61(19)
_cod_database_code               7709283
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNCuBF4Cl
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.866
_reflns_odcompleteness_completeness 64.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     38.56
_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. Others
 Sof(F4B)=Sof(F1B)=Sof(F2B)=Sof(F5B)=Sof(F7B)=Sof(F8B)=Sof(F6B)=1-FVAR(1)
 Sof(F4A)=Sof(F1A)=Sof(F2A)=Sof(F5A)=Sof(F7A)=Sof(F8A)=Sof(F6A)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C6(H6), C29(H29), C14(H14), C3(H3), C18(H18), C13(H13),
 C28(H28), C11(H11), C12(H12), C5(H5), C34(H34), C4(H4), C21(H21), C42(H42),
 C45(H45), C37(H37), C19(H19), C35(H35), C44(H44), C20(H20), C43(H43), C36(H36)
3.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C47(H47A,H47B,H47C), C39(H39A,H39B,H39C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66277
_shelx_hkl_checksum              62245
_shelx_fab_checksum              41243
_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 3.894
_oxdiff_exptl_absorpt_empirical_full_min 0.716