Dynamic dimer-monomer equilibrium in a cycloruthenated complex of [Re(η<sup>6</sup>-C<sub>6</sub>H<sub>6</sub>)<sub>2</sub>]<sup/>.
Hernández-Valdés, Daniel; Wettstein, Lionel; Fernández-Terán, Ricardo; Probst, Benjamin; Fox, Thomas; Spingler, Bernhard; Nadeem, Qaisar; Alberto, Roger; Chemical communications (Cambridge, England) 56 (2020) 10658–10661; doi:10.1039/d0cc04180g

data_7127069
_publ_section_title
;
 Dynamic dimer-monomer equilibrium in a cycloruthenated complex of
 [Re(\h<sup>6</sup>-C<sub>6</sub>H<sub>6</sub>)<sub>2</sub>]<sup/>.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10658
_journal_page_last               10661
_journal_paper_doi               10.1039/d0cc04180g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C23 H18 F3 N O5 Re Ru, C2 F3 O2'
_chemical_formula_sum            'C25 H18 F6 N O7 Re Ru'
_chemical_formula_weight         845.67
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-02 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.256(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5216(2)
_cell_length_b                   12.3888(2)
_cell_length_c                   16.6363(3)
_cell_measurement_reflns_used    28808
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      79.6250
_cell_measurement_theta_min      4.0240
_cell_volume                     2521.93(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (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_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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     -4.00  56.00   0.50   13.82    --   49.87 -99.00 -90.00  120
  2  \w     41.00  68.00   0.50   13.82    --  110.00 -61.00  30.00   54
  3  \w     41.00  70.00   0.50   13.82    --  110.00 -61.00  60.00   58
  4  \w     43.00  71.00   0.50   13.82    --  110.00 -61.00   0.00   56
  5  \w     55.00  92.00   0.50   13.82    --  110.00 -77.00 -60.00   74
  6  \w     39.00  71.00   0.50   13.82    --  110.00 -61.00-150.00   64
  7  \w     75.00 105.00   0.50   13.82    --  110.00 -77.00-180.00   60
  8  \w     96.00 122.00   0.50   13.82    --  110.00  45.00 -90.00   52
  9  \w     98.00 177.00   0.50   13.82    --  110.00  61.00 -90.00  158
 10  \w    148.00 178.00   0.50   13.82    --  110.00  77.00   0.00   60
 11  \w    153.00 178.00   0.50   13.82    --  110.00 111.00  30.00   50
 12  \w    134.00 172.00   0.50   13.82    --  110.00  15.00  30.00   76
 13  \w    104.00 130.00   0.50   13.82    --  110.00  77.00   0.00   52
 14  \w    101.00 130.00   0.50   13.82    --  110.00 111.00  30.00   58
 15  \w     94.00 171.00   0.50   13.82    --  110.00  15.00  60.00  154
 16  \w    104.00 176.00   0.50   13.82    --  110.00 111.00-120.00  144
 17  \w     36.00 101.00   0.50   13.82    --  110.00 -77.00 150.00  130
 18  \w     37.00 106.00   0.50   13.82    --  110.00 -94.00 150.00  138
 19  \w     42.00 109.00   0.50   13.82    --  110.00 -94.00  90.00  134
 20  \w    -17.00  20.00   0.50   13.82    --  -49.87  19.00-180.00   74
 21  \w    -35.00 -10.00   0.50   13.82    --  -88.50  30.00-180.00   50
 22  \w   -109.00 -83.00   0.50   13.82    --  -49.87 -99.00-150.00   52
 23  \w    -49.00 -24.00   0.50   13.82    --  -88.50  45.00  60.00   50
 24  \w   -123.00 -36.00   0.50   13.82    --  -49.87 -57.00  30.00  174
 25  \w   -124.00 -85.00   0.50   13.82    --  -49.87-128.00  83.00   78
 26  \w   -120.00 -94.00   0.50   13.82    --  -49.87 -99.00 -90.00   52
 27  \w    -39.00  -2.00   0.50   13.82    --  -49.87  38.00  90.00   74
 28  \w    -38.00  20.00   0.50   13.82    --  -49.87  38.00 120.00  116
 29  \w    -35.00  22.00   0.50   13.82    --  -49.87  38.00-120.00  114
 30  \w     -6.00  25.00   0.50   13.82    --  -49.87  19.00 -90.00   62
 31  \w    -23.00  30.00   0.50   13.82    --  -49.87  19.00   0.00  106
 32  \w     73.00 112.00   0.50   13.82    --   49.87  57.00  60.00   78
 33  \w    -64.00 -38.00   0.50   13.82    --  -88.50  58.00 -88.17   52
 34  \w    -51.00 -24.00   0.50   13.82    --  -88.50  60.00-155.46   54
 35  \w    -47.00 -11.00   0.50   13.82    --  -88.50  42.00  53.26   72
 36  \w     97.00 141.00   0.50   13.82    --  110.00  45.00 -30.00   88
 37  \w    145.00 171.00   0.50   13.82    --  110.00  30.00  90.00   52
 38  \w     97.00 123.00   0.50   13.82    --  110.00  45.00  60.00   52
 39  \w    148.00 173.00   0.50   13.82    --  110.00  45.00 150.00   50
 40  \w    123.00 169.00   0.50   13.82    --  110.00  50.00-163.36   92
 41  \w    102.00 133.00   0.50   13.82    --  110.00  30.00  90.00   62
 42  \w    150.00 178.00   0.50   13.82    --  110.00  51.00  25.30   56
 43  \w    110.00 177.00   0.50   13.82    --  110.00  30.00   0.00  134
 44  \w    149.00 176.00   0.50   13.82    --  110.00  45.00-180.00   54
 45  \w     98.00 123.00   0.50   13.82    --  110.00  45.00   0.00   50
 46  \w     95.00 120.00   0.50   13.82    --  110.00  51.00  25.30   50
 47  \w     96.00 123.00   0.50   13.82    --  110.00  45.00-180.00   54
 48  \w    101.00 138.00   0.50   13.82    --  110.00  30.00 -90.00   74
 49  \w    101.00 132.00   0.50   13.82    --  110.00  30.00  30.00   62
 50  \w     96.00 131.00   0.50   13.82    --  110.00  45.00  90.00   70
 51  \w    103.00 129.00   0.50   13.82    --  110.00  30.00  60.00   52
 52  \w     98.00 124.00   0.50   13.82    --  110.00  45.00 150.00   52
 53  \w     98.00 123.00   0.50   13.82    --  110.00  45.00-120.00   50
 54  \w    119.00 145.00   0.50   13.82    --  110.00  30.00-120.00   52
 55  \w    149.00 175.00   0.50   13.82    --  110.00  30.00-120.00   52
 56  \w     97.00 123.00   0.50   13.82    --  110.00  45.00  30.00   52
 57  \w    150.00 175.00   0.50   13.82    --  110.00  45.00-150.00   50
 58  \w     96.00 178.00   0.50   13.82    --  110.00  45.00 -60.00  164
 59  \w    148.00 174.00   0.50   13.82    --  110.00  45.00  30.00   52
 60  \w    117.00 154.00   0.50   13.82    --  110.00  30.00-180.00   74
 61  \w    152.00 178.00   0.50   13.82    --  110.00  45.00 -30.00   52
 62  \w     99.00 124.00   0.50   13.82    --  110.00  30.00 120.00   50
 63  \w    150.00 175.00   0.50   13.82    --  110.00  42.00  57.14   50
 64  \w     96.00 122.00   0.50   13.82    --  110.00  42.00  57.14   52
 65  \w     95.00 121.00   0.50   13.82    --  110.00  60.00  45.34   52
 66  \w    142.00 168.00   0.50   13.82    --  110.00  60.00  45.34   52
 67  \w    150.00 176.00   0.50   13.82    --  110.00  53.00 164.53   52
 68  \w    152.00 178.00   0.50   13.82    --  110.00  60.00 -31.55   52
 69  \w    153.00 178.00   0.50   13.82    --  110.00  54.00  -1.23   50
 70  \w    152.00 178.00   0.50   13.82    --  110.00  52.00 -18.55   52
 71  \w     95.00 121.00   0.50   13.82    --  110.00  56.00-121.20   52
 72  \w     95.00 129.00   0.50   13.82    --  110.00  53.00  68.38   68
 73  \w     95.00 121.00   0.50   13.82    --  110.00  54.00-179.06   52
 74  \w    146.00 172.00   0.50   13.82    --  110.00  54.00-179.06   52
 75  \w    153.00 178.00   0.50   13.82    --  110.00  58.00 -47.58   50
 76  \w    100.00 126.00   0.50   13.82    --  110.00  47.00  20.59   52
 77  \w    102.00 129.00   0.50   13.82    --  110.00  41.00-130.92   54
 78  \w     33.00 123.00   0.50   13.82    --   49.87  57.00 -60.00  180
 79  \w     33.00  97.00   0.50   13.82    --   49.87  57.00 120.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0880201000
_diffrn_orient_matrix_UB_12      0.0764387000
_diffrn_orient_matrix_UB_13      -0.0480268000
_diffrn_orient_matrix_UB_21      -0.0152719000
_diffrn_orient_matrix_UB_22      0.0498629000
_diffrn_orient_matrix_UB_23      0.0815879000
_diffrn_orient_matrix_UB_31      0.0887882000
_diffrn_orient_matrix_UB_32      0.0843609000
_diffrn_orient_matrix_UB_33      -0.0050084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            49374
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.919
_diffrn_reflns_theta_min         4.034
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.017
_refine_diff_density_max         2.265
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5442
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0561P)^2^+9.8898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4847
_reflns_number_total             5442
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -123.5339\% 
 around [0.10 0.99 0.07] (reciprocal) or [0.11 0.99 0.06] (direct)
;
_cod_data_source_file            d0cc04180g2.cif
_cod_data_source_block           dhv-230-01_peak1_180219_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7127067--7127069.cif.'
_cod_database_code               7127069
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C23 H17 N O5 Re Ru F3'
_diffrn_oxdiff_digest_frames
;
013a71f4f19c56dbd87c10da2b043dc11c05802ea14
;
_diffrn_oxdiff_digest_hkl
;
014732d41c1f6568d8d5374e105732b64b5d61
;
_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, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 C13-H1
 1.928907 with sigma of 0.02
 Ru1-H1
 2.905182 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C19(H19), C17(H17), C3(H3), C6(H6), C4(H4), C5(H5),
 C8(H8), C9(H9), C10(H10), C12(H12), C7(H7), C11(H11)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              66532
_shelx_hkl_checksum              12770
_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 2.114
_oxdiff_exptl_absorpt_empirical_full_min 0.511
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2