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_7121068
_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 Cl4 F6 O2 Rh2'
_chemical_formula_sum            'C32 H32 Cl4 F6 O2 Rh2'
_chemical_formula_weight         910.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                89.827(6)
_cell_angle_beta                 70.323(7)
_cell_angle_gamma                65.775(8)
_cell_formula_units_Z            2
_cell_length_a                   11.1207(9)
_cell_length_b                   11.2919(8)
_cell_length_c                   16.0905(10)
_cell_measurement_reflns_used    5411
_cell_measurement_temperature    294
_cell_measurement_theta_max      28.4480
_cell_measurement_theta_min      2.2080
_cell_volume                     1713.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_details
;
  1 omega  -35.00   57.00   1.0000    7.1750
omega____ theta____ kappa____ phi______ frames
    -       -9.9495   57.0000  -30.0000 92

  2 omega  -80.00   15.00   1.0000    7.1750
omega____ theta____ kappa____ phi______ frames
    -       -9.9495  -57.0000 -180.0000 95

  3 omega   34.00  100.00   1.0000    7.1750
omega____ theta____ kappa____ phi______ frames
    -       11.9027  179.0000 -180.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0403655000
_diffrn_orient_matrix_UB_12      -0.0686786000
_diffrn_orient_matrix_UB_13      -0.0036834000
_diffrn_orient_matrix_UB_21      -0.0581937000
_diffrn_orient_matrix_UB_22      -0.0108541000
_diffrn_orient_matrix_UB_23      -0.0005830000
_diffrn_orient_matrix_UB_31      0.0253287000
_diffrn_orient_matrix_UB_32      -0.0055258000
_diffrn_orient_matrix_UB_33      -0.0472597000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12210
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.591
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.764
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.3352
_exptl_crystal_size_mid          0.1289
_exptl_crystal_size_min          0.0865
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7832
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6014
_reflns_number_total             7832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09352g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7121066--7121070.cif.'
_cod_original_cell_volume        1713.4(2)
_cod_database_code               7121068
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H32 Cl4 F6 O2 Rh2'
_reflns_odcompleteness_completeness 98.87
_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
 H2-O2
 1 with sigma of 0.02
 H1-O1
 1 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C), C60(H60A,H60B,H60C), C56(H56A,H56B,H56C), C58(H58A,
 H58B,H58C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              79745
_olex2_submission_special_instructions 'No special instructions were received'