Hidden aryl-exchange processes in stable 16e Rh<sup>III</sup> [RhCp*Ar<sub>2</sub>] complexes, and their unexpected transmetalation mechanism.
Peñas-Defrutos, M N; Bartolomé, C; García-Melchor, M; Espinet, P.; Chemical communications (Cambridge, England) 54 (2018) 984–987; doi:10.1039/c7cc09352g

data_7121069
_publ_section_title
;
 Hidden aryl-exchange processes in stable 16e Rh<sup>III</sup>
 [RhCp*Ar<sub>2</sub>] complexes, and their unexpected transmetalation
 mechanism.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              984
_journal_page_last               987
_journal_paper_doi               10.1039/c7cc09352g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C32 H32 F10 O2 Rh2'
_chemical_formula_sum            'C32 H32 F10 O2 Rh2'
_chemical_formula_weight         844.39
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-02 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.287(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8682(5)
_cell_length_b                   16.2215(7)
_cell_length_c                   18.4548(8)
_cell_measurement_reflns_used    6708
_cell_measurement_temperature    294
_cell_measurement_theta_max      27.2240
_cell_measurement_theta_min      2.5350
_cell_volume                     3251.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.866
_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    -19.00   7.00   1.00   29.43    --  -10.11 -99.00-120.00   26
  2  \w    -30.00  60.00   1.00   29.43    --  -10.11  57.00 150.00   90
  3  \w    -77.00   6.00   1.00   29.43    --  -10.11 -37.00   0.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0554890000
_diffrn_orient_matrix_UB_12      -0.0225776000
_diffrn_orient_matrix_UB_13      0.0054257000
_diffrn_orient_matrix_UB_21      0.0286353000
_diffrn_orient_matrix_UB_22      0.0353040000
_diffrn_orient_matrix_UB_23      0.0157511000
_diffrn_orient_matrix_UB_31      -0.0190158000
_diffrn_orient_matrix_UB_32      -0.0124530000
_diffrn_orient_matrix_UB_33      0.0346342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17945
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.497
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0323P)^2^+1.0913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5639
_reflns_number_total             7851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09352g2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7121066--7121070.cif.'
_cod_original_cell_volume        3251.0(3)
_cod_database_code               7121069
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H32 F10 O2 Rh2'
_chemical_oxdiff_usercomment     orange
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2
 0.96 with sigma of 0.02
 H2-O2
 0.96 with sigma of 0.02
 H1-O1
 1 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C39(H39A,H39B,H39C), C58(H58A,H58B,H58C), C38(H38A,H38B,
 H38C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C40(H40A,H40B,H40C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              75092
_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.691