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_7127067
_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         'C42 H34 N2 O6 Re2 Ru2, 2(F6 P)'
_chemical_formula_sum            'C42 H34 F12 N2 O6 P2 Re2 Ru2'
_chemical_formula_weight         1527.19
_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             2020-06-02
_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                99.0170(10)
_cell_angle_beta                 103.0770(10)
_cell_angle_gamma                102.8080(10)
_cell_formula_units_Z            1
_cell_length_a                   9.53370(10)
_cell_length_b                   10.99430(10)
_cell_length_c                   11.15720(10)
_cell_measurement_reflns_used    27102
_cell_measurement_temperature    160.03(18)
_cell_measurement_theta_max      79.5430
_cell_measurement_theta_min      4.1470
_cell_volume                     1084.12(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_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      160.03(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_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      1.00  29.00   0.50    0.59    --   49.37 -99.00 -60.00   56
  2  \w     41.00 110.00   0.50    0.59    --  110.00 -94.00 -30.00  138
  3  \w     73.00 112.00   0.50    0.59    --  110.00-111.00 -30.00   78
  4  \w     62.00  91.00   0.50    0.59    --  110.00 -94.00 -90.00   58
  5  \w     82.00 108.00   0.50    0.59    --  110.00-111.00-120.00   52
  6  \w     80.00 112.00   0.50    0.59    --  110.00-111.00-180.00   64
  7  \w     42.00  76.00   0.50    0.59    --  110.00-111.00-180.00   68
  8  \w     50.00  77.00   0.50    0.59    --  110.00-111.00-120.00   54
  9  \w     46.00 112.00   0.50    0.59    --  110.00-110.00 -87.00  132
 10  \w     48.00  81.00   0.50    0.59    --  110.00 -94.00  30.00   66
 11  \w     63.00 111.00   0.50    0.59    --  110.00-111.00  90.00   96
 12  \w     87.00 112.00   0.50    0.59    --  110.00-111.00 120.00   50
 13  \w     74.00 100.00   0.50    0.59    --  110.00 -77.00 120.00   52
 14  \w     39.00  65.00   0.50    0.59    --  110.00 -61.00  90.00   52
 15  \w     37.00  70.00   0.50    0.59    --  110.00 -77.00  90.00   66
 16  \w     40.00  68.00   0.50    0.59    --  110.00 -61.00 150.00   56
 17  \w     36.00  70.00   0.50    0.59    --  110.00 -77.00 120.00   68
 18  \w     33.00  59.00   0.50    0.59    --  110.00-111.00  90.00   52
 19  \w     34.00 103.00   0.50    0.59    --  110.00 -94.00  90.00  138
 20  \w     39.00  66.00   0.50    0.59    --  110.00 -61.00   0.00   54
 21  \w     36.00  70.00   0.50    0.59    --  110.00 -94.00 -60.00   68
 22  \w     36.00  71.00   0.50    0.59    --  110.00 -77.00 -30.00   70
 23  \w     95.00 168.00   0.50    0.59    --  110.00  15.00-120.00  146
 24  \w    100.00 177.00   0.50    0.59    --  110.00  30.00 -60.00  154
 25  \w    142.00 172.00   0.50    0.59    --  110.00  15.00  30.00   60
 26  \w     96.00 170.00   0.50    0.59    --  110.00  30.00 -90.00  148
 27  \w    106.00 131.00   0.50    0.59    --  110.00 111.00  30.00   50
 28  \w     86.00 111.00   0.50    0.59    --  110.00 178.00 -60.00   50
 29  \w    121.00 148.00   0.50    0.59    --  110.00 178.00 -60.00   54
 30  \w     98.00 178.00   0.50    0.59    --  110.00  30.00 -30.00  160
 31  \w     98.00 124.00   0.50    0.59    --  110.00  30.00  30.00   52
 32  \w     99.00 138.00   0.50    0.59    --  110.00  15.00  30.00   78
 33  \w     30.00 121.00   0.50    0.59    --   49.37  77.00   0.00  182
 34  \w     38.00  67.00   0.50    0.59    --  110.00 -61.00-180.00   58
 35  \w    -91.00 -12.00   0.50    0.59    --  -49.87 125.00 -90.00  158
 36  \w    -64.00 -34.00   0.50    0.59    --  -88.50  61.00-180.00   60
 37  \w     -3.00  27.00   0.50    0.59    --  -49.87  19.00-180.00   60
 38  \w    -35.00 -10.00   0.50    0.59    --  -88.50  30.00  90.00   50
 39  \w    -64.00  23.00   0.50    0.59    --  -49.87  57.00 150.00  174
 40  \w   -123.00 -78.00   0.50    0.59    --  -49.87-110.00 -87.00   90
 41  \w   -160.00-100.00   0.50    0.59    --  -88.50-111.00 120.00  120
 42  \w   -123.00 -70.00   0.50    0.59    --  -49.87-125.00 150.00  106
 43  \w     32.00  87.00   0.50    0.59    --   48.00  60.00-162.80  110
 44  \w     33.00  60.00   0.50    0.59    --   48.00  58.00 -26.23   54
 45  \w     68.00  94.00   0.50    0.59    --   48.00  58.00 -26.23   52
 46  \w     74.00 101.00   0.50    0.59    --   49.37  57.00 -60.00   54
 47  \w     33.00  60.00   0.50    0.59    --   49.37  57.00 -90.00   54
 48  \w     52.00  86.00   0.50    0.59    --   49.37  19.00  90.00   68
 49  \w     33.00  60.00   0.50    0.59    --   49.37  57.00  90.00   54
 50  \w     94.00 121.00   0.50    0.59    --   49.37  57.00 -90.00   54
 51  \w     33.00  59.00   0.50    0.59    --   49.37  57.00-120.00   52
 52  \w     33.00  69.00   0.50    0.59    --   49.37  57.00 -60.00   72
 53  \w     37.00  67.00   0.50    0.59    --   49.37  38.00-180.00   60
 54  \w     37.00  82.00   0.50    0.59    --   49.37  38.00 -60.00   90
 55  \w     85.00 112.00   0.50    0.59    --   52.00  58.00 109.01   54
 56  \w     38.00  76.00   0.50    0.59    --   52.00  58.00 109.01   76
 57  \w     37.00  89.00   0.50    0.59    --   52.00  56.00 161.76  104
 58  \w     40.00  89.00   0.50    0.59    --   56.00  58.00  -6.85   98
 59  \w    108.00 133.00   0.50    0.59    --   60.00  58.00  32.89   50
 60  \w     48.00  74.00   0.50    0.59    --   60.00  58.00  32.89   52
 61  \w     43.00  69.00   0.50    0.59    --   60.00  59.00 121.88   52
 62  \w     43.00 112.00   0.50    0.59    --   60.00  59.00 151.99  138
 63  \w     49.00 110.00   0.50    0.59    --   64.00  59.00-137.99  122
 64  \w     52.00  93.00   0.50    0.59    --   68.00  60.00 115.38   82
 65  \w     52.00 107.00   0.50    0.59    --   68.00  56.00  65.87  110
 66  \w     55.00  81.00   0.50    0.59    --   72.00  60.00-165.66   52
 67  \w     68.00  94.00   0.50    0.59    --   84.00  56.00-154.44   52
 68  \w     67.00  93.00   0.50    0.59    --   84.00  59.00   5.31   52
 69  \w     79.00 120.00   0.50    0.59    --   96.00  58.00   8.60   82
 70  \w     79.00 106.00   0.50    0.59    --   96.00  58.00-122.92   54
 71  \w    142.00 168.00   0.50    0.59    --   96.00  60.00  24.80   52
 72  \w     81.00 109.00   0.50    0.59    --   96.00  60.00  24.80   56
 73  \w     87.00 113.00   0.50    0.59    --  104.00  59.00 166.42   52
 74  \w     88.00 114.00   0.50    0.59    --  104.00  33.00 -49.36   52
 75  \w    138.00 174.00   0.50    0.59    --  104.00  59.00 166.42   72
 76  \w    141.00 177.00   0.50    0.59    --  110.00  51.00  41.07   72
 77  \w     95.00 122.00   0.50    0.59    --  110.00  51.00  41.07   54
 78  \w    153.00 178.00   0.50    0.59    --  110.00  55.00 -34.82   50
 79  \w     97.00 141.00   0.50    0.59    --  110.00  45.00 150.00   88
 80  \w    153.00 178.00   0.50    0.59    --  110.00  45.00-180.00   50
 81  \w     99.00 138.00   0.50    0.59    --  110.00  45.00-180.00   78
 82  \w     94.00 123.00   0.50    0.59    --  110.00  55.00 -34.82   58
 83  \w    136.00 172.00   0.50    0.59    --  110.00  37.00 143.22   72
 84  \w     95.00 132.00   0.50    0.59    --  110.00  37.00 143.22   74
 85  \w     98.00 124.00   0.50    0.59    --  110.00  45.00   0.00   52
 86  \w    138.00 165.00   0.50    0.59    --  110.00  39.00 119.87   54
 87  \w     97.00 124.00   0.50    0.59    --  110.00  45.00 -60.00   54
 88  \w     96.00 131.00   0.50    0.59    --  110.00  39.00 119.87   70
 89  \w    143.00 170.00   0.50    0.59    --  110.00  45.00-120.00   54
 90  \w     97.00 123.00   0.50    0.59    --  110.00  45.00-120.00   52
 91  \w    148.00 174.00   0.50    0.59    --  110.00  45.00-150.00   52
 92  \w    145.00 174.00   0.50    0.59    --  110.00  45.00   0.00   58
 93  \w     96.00 122.00   0.50    0.59    --  110.00  45.00-150.00   52
 94  \w    141.00 176.00   0.50    0.59    --  110.00  50.00  77.93   70
 95  \w    149.00 176.00   0.50    0.59    --  110.00  45.00  90.00   54
 96  \w    102.00 134.00   0.50    0.59    --  110.00  45.00  90.00   64
 97  \w     95.00 122.00   0.50    0.59    --  110.00  50.00  77.93   54
 98  \w    140.00 169.00   0.50    0.59    --  110.00  45.00  60.00   58
 99  \w     96.00 134.00   0.50    0.59    --  110.00  45.00  60.00   76
100  \w    150.00 178.00   0.50    0.59    --  110.00  45.00 150.00   56
101  \w     96.00 122.00   0.50    0.59    --  110.00  45.00 -90.00   52
102  \w     96.00 123.00   0.50    0.59    --  110.00  57.00 -48.27   54
103  \w     31.00 121.00   0.50    0.59    --   48.00  58.00 -26.23  180
104  \w     31.00 120.00   0.50    0.59    --   48.00  60.00 129.72  178
105  \w     35.00 128.00   0.50    0.59    --   49.37  38.00 -90.00  186
106  \w     33.00 123.00   0.50    0.59    --   49.37  57.00 -30.00  180
107  \w     33.00 123.00   0.50    0.59    --   49.37  57.00-180.00  180
108  \w     35.00 128.00   0.50    0.59    --   49.37  38.00  30.00  186
109  \w     33.00 123.00   0.50    0.59    --   49.37  57.00 -60.00  180
110  \w     33.00 123.00   0.50    0.59    --   49.37  57.00 120.00  180
111  \w     35.00 128.00   0.50    0.59    --   49.37  38.00  90.00  186
112  \w     33.00 123.00   0.50    0.59    --   49.37  57.00  30.00  180
113  \w     33.00 123.00   0.50    0.59    --   49.37  57.00-120.00  180
114  \w    -43.00  29.00   0.50    0.59    --  -49.87  38.00   0.00  144
115  \w    -66.00  23.00   0.50    0.59    --  -49.87  57.00 -90.00  178
116  \w     36.00 125.00   0.50    0.59    --   52.00  57.00  62.34  178
117  \w     35.00 124.00   0.50    0.59    --   52.00  60.00  -9.24  178
118  \w     39.00 129.00   0.50    0.59    --   56.00  58.00  -6.85  180
119  \w     43.00 133.00   0.50    0.59    --   60.00  59.00 151.99  180
120  \w     47.00 137.00   0.50    0.59    --   64.00  59.00-137.99  180
121  \w     51.00 140.00   0.50    0.59    --   68.00  60.00 115.38  178
122  \w     53.00 145.00   0.50    0.59    --   68.00  44.00-136.55  184
123  \w     53.00 147.00   0.50    0.59    --   68.00  32.00 -63.36  188
124  \w     52.00 142.00   0.50    0.59    --   68.00  56.00  65.87  180
125  \w     55.00 144.00   0.50    0.59    --   72.00  60.00-165.66  178
126  \w     61.00 154.00   0.50    0.59    --   76.00  36.00   0.25  186
;
_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      0.0949288000
_diffrn_orient_matrix_UB_12      -0.0432932000
_diffrn_orient_matrix_UB_13      0.1079353000
_diffrn_orient_matrix_UB_21      -0.0108983000
_diffrn_orient_matrix_UB_22      -0.1239820000
_diffrn_orient_matrix_UB_23      -0.0920301000
_diffrn_orient_matrix_UB_31      0.1432049000
_diffrn_orient_matrix_UB_32      0.0665744000
_diffrn_orient_matrix_UB_33      -0.0312315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.453
_diffrn_reflns_theta_min         4.168
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.812
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.339
_exptl_crystal_description       needle
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+2.4747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4333
_reflns_number_total             4611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04180g2.cif
_cod_data_source_block           dhv-lw-07-02_isomer2dimer_270919
_cod_depositor_comments
'Adding full bibliography for 7127067--7127069.cif.'
_cod_original_cell_volume        1084.116(19)
_cod_database_code               7127067
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H34 F12 N2 O6 P2 Re2'
_diffrn_oxdiff_digest_frames
;
012d7677090e282f365af6c7a84d7333f411826c62d
;
_diffrn_oxdiff_digest_hkl
;
01401ae57b7d682e39fc3c7033b9f539e436b2
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C19(H19), C3(H3), C18(H18), C7(H7), C6(H6), C16(H16), C17(H17), C5(H5),
 C8(H8), C4(H4), C12(H12), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              89621
_shelx_hkl_checksum              59264
_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 2.329
_oxdiff_exptl_absorpt_empirical_full_min 0.574