Synthesis, electronic structure and redox properties of the diruthenium sandwich complexes [Cp*Ru(μ-C<sub>10</sub>H<sub>8</sub>)RuCp*]<sup>x</sup> (x = 0, 1+; Cp* = C<sub>5</sub>Me<sub>5</sub>; C<sub>10</sub>H<sub>8</sub> = naphthalene).
Herrmann, Dirk; Rödl, Christian; de Bruin, Bas; Hartl, František; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11058–11069; doi:10.1039/c8dt02003e

data_7046960
_publ_section_title
;
 Synthesis, electronic structure and redox properties of the diruthenium
 sandwich complexes
 [Cp*Ru(\m-C<sub>10</sub>H<sub>8</sub>)RuCp*]<sup>x</sup> (x = 0, 1+; Cp*
 = C<sub>5</sub>Me<sub>5</sub>; C<sub>10</sub>H<sub>8</sub> =
 naphthalene).
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11058
_journal_page_last               11069
_journal_paper_doi               10.1039/c8dt02003e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H38 Ru2'
_chemical_formula_sum            'C30 H38 Ru2'
_chemical_formula_weight         600.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-20 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.186(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6703(3)
_cell_length_b                   11.0228(3)
_cell_length_c                   13.1457(4)
_cell_measurement_reflns_used    5981
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.4250
_cell_measurement_theta_min      3.3590
_cell_volume                     1256.08(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -66.00  -23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   57.0000  -30.0000 43

  2 omega  -22.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   57.0000  -30.0000 47

  3 omega -109.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000 -180.0000 94

  4 omega    4.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000   90.0000 35

  5 omega   82.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   60.0000 63

  6 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  150.0000 79

  7 omega   45.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   30.0000 31

  8 omega   42.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   60.0000 35

  9 omega   39.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   60.0000 32

 10 omega   43.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 26

 11 omega   40.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 26

 12 omega   45.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 32

 13 omega   32.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -103.0000 -108.0000 71

 14 omega   85.00  155.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -60.0000 70

 15 omega   43.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000    0.0000 33

 16 omega   38.00   67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 29

 17 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000   90.0000 103

 18 omega  -98.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  120.0000 96

 19 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000    0.0000 103

 20 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  -90.0000 103

 21 omega   82.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   90.0000 76

 22 omega   82.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 76

 23 omega   35.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 19
;
_diffrn_measurement_device_type  'SuperNova, Single source at ofset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1115593000
_diffrn_orient_matrix_UB_12      -0.0725713000
_diffrn_orient_matrix_UB_13      -0.0664706000
_diffrn_orient_matrix_UB_21      -0.0245343000
_diffrn_orient_matrix_UB_22      -0.1127861000
_diffrn_orient_matrix_UB_23      0.0669260000
_diffrn_orient_matrix_UB_31      -0.1361513000
_diffrn_orient_matrix_UB_32      -0.0392110000
_diffrn_orient_matrix_UB_33      -0.0696265000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2565
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.528
_diffrn_reflns_theta_min         5.237
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.219
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.00080(16)
_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   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0431P)^2^+20.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2470
_reflns_number_total             2565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02003e2.cif
_cod_data_source_block           1mb
_cod_depositor_comments          'Adding full bibliography for 7046960.cif.'
_cod_database_code               7046960
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.874(7)
 0.126(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C11(H11), C13(H13), C12(H12)
;
_shelx_res_checksum              77514
_olex2_submission_special_instructions 'No special instructions were received'