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_7127068
_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             2019-05-24
_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                 102.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.55040(10)
_cell_length_b                   17.4219(2)
_cell_length_c                   14.64830(10)
_cell_measurement_reflns_used    38859
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      79.1650
_cell_measurement_theta_min      3.9850
_cell_volume                     2625.50(4)
_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      160.00(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 0.990
_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    -60.00  22.00   0.50    0.71    --  -49.62  57.00 150.00  164
  2  \w    -58.00 -21.00   0.50    2.85    --  -88.50  30.00 120.00   74
  3  \w    -66.00 -40.00   0.50    2.85    --  -88.50  30.00  60.00   52
  4  \w   -111.00 -70.00   0.50    0.71    --  -49.62-125.00 150.00   82
  5  \w   -121.00 -74.00   0.50    0.71    --  -49.62-125.00 -30.00   94
  6  \w   -121.00 -91.00   0.50    0.71    --  -49.62-125.00-180.00   60
  7  \w     44.00  96.00   0.50    0.71    --   49.62-125.00   0.00  104
  8  \w     57.00  99.00   0.50    2.85    --  110.00 -94.00  90.00   84
  9  \w     43.00  69.00   0.50    2.85    --  110.00 -45.00  30.00   52
 10  \w     95.00 125.00   0.50    2.85    --  110.00 -15.00  60.00   60
 11  \w    102.00 127.00   0.50    2.85    --  110.00 -61.00 -60.00   50
 12  \w     97.00 127.00   0.50    2.85    --  110.00 -77.00 -60.00   60
 13  \w     86.00 112.00   0.50    2.85    --  110.00 -15.00 -90.00   52
 14  \w     70.00  95.00   0.50    2.85    --  110.00 -61.00 -60.00   50
 15  \w     43.00  98.00   0.50    2.85    --  110.00-111.00-120.00  110
 16  \w     38.00  77.00   0.50    2.85    --  110.00 -45.00 -60.00   78
 17  \w     48.00  73.00   0.50    2.85    --  110.00 -45.00   0.00   50
 18  \w     46.00  79.00   0.50    2.85    --  110.00 -15.00  60.00   66
 19  \w     36.00  67.00   0.50    2.85    --  110.00 -45.00 120.00   62
 20  \w     41.00  67.00   0.50    2.85    --  110.00 -45.00  60.00   52
 21  \w     31.00  66.00   0.50    2.85    --  110.00 -30.00 120.00   70
 22  \w     32.00  67.00   0.50    2.85    --  110.00 -30.00  30.00   70
 23  \w     34.00  66.00   0.50    2.85    --  110.00 -30.00 -60.00   64
 24  \w     35.00  61.00   0.50    2.85    --  110.00 -45.00 -90.00   52
 25  \w     36.00  84.00   0.50    2.85    --  110.00 -77.00 -60.00   96
 26  \w     32.00  69.00   0.50    2.85    --  110.00 -30.00-150.00   74
 27  \w     38.00  97.00   0.50    2.85    --  110.00 -61.00-180.00  118
 28  \w     35.00  74.00   0.50    2.85    --  110.00 -45.00-150.00   78
 29  \w     32.00  57.00   0.50    2.85    --  110.00 -15.00 -90.00   50
 30  \w     -2.00  23.00   0.50    0.71    --  -49.62  57.00  90.00   50
 31  \w     -4.00  22.00   0.50    0.71    --  -49.62  19.00   0.00   52
 32  \w    -33.00  -7.00   0.50    0.71    --  -49.62  19.00   0.00   52
 33  \w    -64.00 -27.00   0.50    0.71    --  -49.62  57.00  90.00   74
 34  \w     54.00  80.00   0.50    0.71    --   49.62  57.00 150.00   52
 35  \w     74.00 112.00   0.50    0.71    --   49.62  57.00  90.00   76
 36  \w     86.00 111.00   0.50    0.71    --   49.62  57.00-180.00   50
 37  \w     65.00 107.00   0.50    0.71    --   49.62  57.00   0.00   84
 38  \w     35.00  68.00   0.50    0.71    --   49.62  57.00  90.00   66
 39  \w     44.00  70.00   0.50    0.71    --   49.62  57.00-180.00   52
 40  \w     35.00  81.00   0.50    0.71    --   49.62  57.00-150.00   92
 41  \w    -68.00 -42.00   0.50    2.85    --  -88.50  41.00  59.64   52
 42  \w    -69.00 -43.00   0.50    2.85    --  -88.50  30.00   0.00   52
 43  \w    -71.00 -38.00   0.50    2.85    --  -88.50  59.00   9.61   66
 44  \w    106.00 133.00   0.50    2.85    --  110.00  30.00 -60.00   54
 45  \w    144.00 178.00   0.50    2.85    --  110.00  30.00-150.00   68
 46  \w    112.00 167.00   0.50    2.85    --  110.00  30.00 120.00  110
 47  \w     95.00 140.00   0.50    2.85    --  110.00  30.00-150.00   90
 48  \w     97.00 125.00   0.50    2.85    --  110.00  45.00 -30.00   56
 49  \w    108.00 134.00   0.50    2.85    --  110.00  30.00   0.00   52
 50  \w     95.00 124.00   0.50    2.85    --  110.00  48.00   4.86   58
 51  \w    100.00 142.00   0.50    2.85    --  110.00  45.00 150.00   84
 52  \w    114.00 169.00   0.50    2.85    --  110.00  45.00  90.00  110
 53  \w     99.00 142.00   0.50    2.85    --  110.00  45.00  30.00   86
 54  \w     96.00 121.00   0.50    2.85    --  110.00  45.00   0.00   50
 55  \w    124.00 164.00   0.50    2.85    --  110.00  15.00-120.00   80
 56  \w    144.00 178.00   0.50    2.85    --  110.00  45.00  60.00   68
 57  \w    102.00 128.00   0.50    2.85    --  110.00  45.00 -60.00   52
 58  \w    125.00 178.00   0.50    2.85    --  110.00  45.00-180.00  106
 59  \w    108.00 134.00   0.50    2.85    --  110.00  30.00  30.00   52
 60  \w    101.00 126.00   0.50    2.85    --  110.00  30.00 150.00   50
 61  \w    104.00 129.00   0.50    2.85    --  110.00  45.00  60.00   50
 62  \w     95.00 152.00   0.50    2.85    --  110.00  53.00 -52.67  114
 63  \w     99.00 178.00   0.50    2.85    --  110.00  47.00 165.30  158
 64  \w      4.00  29.00   0.50    0.71    --  -49.62  38.00 -60.00   50
 65  \w     94.00 120.00   0.50    2.85    --  110.00  54.00 -79.45   52
 66  \w     94.00 119.00   0.50    2.85    --  110.00  53.00 -15.32   50
 67  \w    -66.00  24.00   0.50    0.71    --  -49.62  57.00-120.00  180
 68  \w     33.00 123.00   0.50    0.71    --   49.62  57.00 -90.00  180
 69  \w     33.00 123.00   0.50    0.71    --   49.62  57.00 120.00  180
 70  \w     33.00 123.00   0.50    0.71    --   49.62  57.00 -30.00  180
 71  \w     33.00 123.00   0.50    0.71    --   49.62  57.00-135.69  180
 72  \w     33.00 123.00   0.50    0.71    --   49.62  57.00  30.00  180
 73  \w     33.00 123.00   0.50    0.71    --   49.62  57.00  60.00  180
 74  \w     33.00 123.00   0.50    0.71    --   49.62  57.00-180.00  180
 75  \w     33.00 103.00   0.50    0.71    --   49.62  57.00 150.00  140
 76  \w     33.00 123.00   0.50    0.71    --   49.62  57.00 -60.00  180
;
_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      0.0966604000
_diffrn_orient_matrix_UB_12      -0.0671658000
_diffrn_orient_matrix_UB_13      0.0072763000
_diffrn_orient_matrix_UB_21      0.0318029000
_diffrn_orient_matrix_UB_22      0.0243708000
_diffrn_orient_matrix_UB_23      -0.0935531000
_diffrn_orient_matrix_UB_31      0.1098228000
_diffrn_orient_matrix_UB_32      0.0520904000
_diffrn_orient_matrix_UB_33      0.0531840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56056
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.556
_diffrn_reflns_theta_min         4.002
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.359
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
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    2.139
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.230
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0420P)^2^+6.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5443
_reflns_number_total             5651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04180g2.cif
_cod_data_source_block           dhv-230-01_peak2_230119
_cod_depositor_comments
'Adding full bibliography for 7127067--7127069.cif.'
_cod_database_code               7127068
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C25 H17 N O7 Re Ru F6'
_diffrn_oxdiff_digest_frames
;
01704dc373fa4543a7560dbf2565dae83b064586dfe
;
_diffrn_oxdiff_digest_hkl
;
013f2c87de60a93fbbcc22a8a420737feaef1f
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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
 1.89611 with sigma of 0.02
 Ru1-H1
 2.844534 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              9011
_shelx_hkl_checksum              77350
_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 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.763