Isolation and structural characterisation of rhodium(iii) η<sup>2</sup>-fluoroarene complexes: experimental verification of predicted regioselectivity.
Gyton, Matthew R.; Kynman, Amy E.; Leforestier, Baptiste; Gallo, Angelo; Lewandowski, Józef R; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5791–5793; doi:10.1039/d0dt01137a

data_7704385
_publ_section_title
;
 Isolation and structural characterisation of rhodium(iii)
 \h<sup>2</sup>-fluoroarene complexes: experimental verification of
 predicted regioselectivity.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5791
_journal_page_last               5793
_journal_paper_doi               10.1039/d0dt01137a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C31 H26 F N5 Rh, C32 H12 B F24'
_chemical_formula_sum            'C63 H38 B F25 N5 Rh'
_chemical_formula_weight         1453.70
_chemical_melting_point          ?
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                106.1628(9)
_cell_angle_beta                 100.1945(9)
_cell_angle_gamma                91.6660(9)
_cell_formula_units_Z            2
_cell_length_a                   12.05682(13)
_cell_length_b                   12.73132(13)
_cell_length_c                   20.3856(2)
_cell_measurement_reflns_used    46215
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6140
_cell_measurement_theta_min      3.6520
_cell_volume                     2947.87(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -74.00  34.00   1.00    1.00    --  -41.82  77.00  60.00  108
  2  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00 -60.00  100
  3  \w    -21.00  74.00   1.00    1.00    --   41.82 -77.00-150.00   95
  4  \w     14.00 115.00   1.00    1.00    --   41.82  57.00-180.00  101
  5  \w     34.00 112.00   1.00    2.00    --  107.00-125.00-120.00   78
  6  \w     35.00 136.00   1.00    2.00    --  107.00 -61.00  30.00  101
  7  \w    103.00 178.00   1.00    2.00    --  107.00  77.00  30.00   75
  8  \w     34.00 112.00   1.00    2.00    --  107.00-125.00 -30.00   78
  9  \w     81.00 178.00   1.00    2.00    --  107.00  45.00 120.00   97
 10  \w     31.00 140.00   1.00    2.00    --  107.00 -77.00  30.00  109
 11  \w     24.00 107.00   1.00    2.00    --  107.00 -94.00  30.00   83
 12  \w    103.00 178.00   1.00    2.00    --  107.00  77.00-120.00   75
 13  \w     97.00 178.00   1.00    2.00    --  107.00 125.00   0.00   81
 14  \w    103.00 178.00   1.00    2.00    --  107.00  77.00  90.00   75
 15  \w     81.00 178.00   1.00    2.00    --  107.00  45.00-180.00   97
 16  \w     34.00 112.00   1.00    2.00    --  107.00-125.00  30.00   78
 17  \w     24.00 107.00   1.00    2.00    --  107.00 -94.00  90.00   83
 18  \w     81.00 178.00   1.00    2.00    --  107.00  45.00 150.00   97
 19  \w     34.00 112.00   1.00    2.00    --  107.00-125.00-150.00   78
 20  \w     31.00 140.00   1.00    2.00    --  107.00 -77.00-150.00  109
 21  \w     97.00 178.00   1.00    2.00    --  107.00 125.00  30.00   81
 22  \w     24.00 107.00   1.00    2.00    --  107.00 -94.00-120.00   83
 23  \w     34.00 112.00   1.00    2.00    --  107.00-125.00  90.00   78
 24  \w     34.00 112.00   1.00    2.00    --  107.00-125.00 150.00   78
 25  \w     36.00 126.00   1.00    2.00    --  107.00-142.00 -93.41   90
 26  \w     34.00 133.00   1.00    2.00    --  107.00 -45.00-120.00   99
 27  \w     24.00 107.00   1.00    2.00    --  107.00 -94.00  60.00   83
 28  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00  30.00   99
 29  \w      8.00  42.00   1.00    1.00    --   41.82  81.00  75.25   34
 30  \w      7.00  33.00   1.00    1.00    --   41.82  84.00 -83.59   26
 31  \w      9.00  42.00   1.00    1.00    --   41.82  79.00 133.30   33
 32  \w      7.00  33.00   1.00    1.00    --   41.82  84.00-121.96   26
 33  \w     81.00 178.00   1.00    2.00    --  107.00  45.00-120.00   97
 34  \w     79.00 178.00   1.00    2.00    --  107.00  56.00  -1.20   99
 35  \w     81.00 178.00   1.00    2.00    --  107.00  45.00 -30.00   97
 36  \w     81.00 178.00   1.00    2.00    --  107.00  45.00-150.00   97
 37  \w     78.00 178.00   1.00    2.00    --  107.00  61.00  60.00  100
 38  \w     78.00 178.00   1.00    2.00    --  107.00  61.00 -90.00  100
 39  \w     78.00 178.00   1.00    2.00    --  107.00  61.00 -60.00  100
 40  \w     78.00 178.00   1.00    2.00    --  107.00  61.00  90.00  100
 41  \w     78.00  90.00   1.00    2.00    --  107.00  61.00-120.00   12
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0506931000
_diffrn_orient_matrix_UB_12      -0.0996894000
_diffrn_orient_matrix_UB_13      0.0191526000
_diffrn_orient_matrix_UB_21      0.1136684000
_diffrn_orient_matrix_UB_22      0.0325684000
_diffrn_orient_matrix_UB_23      -0.0165801000
_diffrn_orient_matrix_UB_31      0.0384801000
_diffrn_orient_matrix_UB_32      0.0705930000
_diffrn_orient_matrix_UB_33      0.0760786000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.076
_diffrn_reflns_theta_max         70.076
_diffrn_reflns_theta_min         6.473
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.484
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.252
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_recrystallization_method
'Crystals grown from FC6H5-hexane at 293 K'
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         11183
_refine_ls_number_restraints     454
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0448P)^2^+2.1558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10916
_reflns_number_total             11183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01137a3.cif
_cod_data_source_block           0536abc19s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2947.86(6)
_cod_database_code               7704385
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 F1A-C4 \\sim F1-C1
 with sigma of 0.01
 C207-F11 \\sim C207-F12 \\sim C207-F13 \\sim C207-F11A \\sim C207-F12A \\sim
C207-F13A
 with sigma of 0.01
 F11-F12 \\sim F12-F13 \\sim F13-F11 \\sim F11A-F12A \\sim F12A-F13A \\sim
F13A-F11A
 with sigma of 0.01
 C203-F11 \\sim C203-F12 \\sim C203-F13 \\sim C203-F11A \\sim C203-F12A \\sim
C203-F13A
 with sigma of 0.01
 C208-F14 \\sim C208-F15 \\sim C208-F16 \\sim C208-F14A \\sim C208-F15A \\sim
C208-F16A
 with sigma of 0.01
 F14-F15 \\sim F15-F16 \\sim F16-F14 \\sim F14A-F15A \\sim F15A-F16A \\sim
F16A-F14A
 with sigma of 0.01
 C205-F14 \\sim C205-F15 \\sim C205-F16 \\sim C205-F14A \\sim C205-F15A \\sim
C205-F16A
 with sigma of 0.01
 C223-F23 \\sim C223-F24 \\sim C223-F25 \\sim C223-F23A \\sim C223-F24A \\sim
C223-F25A
 with sigma of 0.01
 F23-F24 \\sim F24-F25 \\sim F25-F23 \\sim F23A-F24A \\sim F24A-F25A \\sim
F25A-F23A
 with sigma of 0.01
 C219-F23 \\sim C219-F24 \\sim C219-F25 \\sim C219-F23A \\sim C219-F24A \\sim
C219-F25A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1A \\sim F1 \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F13A
\\sim F14 \\sim F14A \\sim F15 \\sim F15A \\sim F16 \\sim F16A \\sim F17 \\sim
F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F23A \\sim F24
\\sim F24A \\sim F25 \\sim F25A \\sim F26 \\sim F27 \\sim F28 \\sim F29 \\sim
F30 \\sim F31 \\sim F32 \\sim F33 \\sim F34: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F1A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13) \\sim Ueq,
Uanis(F13A) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F16A) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20)
\\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq,
Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq, Uanis(F25)
\\sim Ueq, Uanis(F25A) \\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F27) \\sim Ueq,
Uanis(F28) \\sim Ueq, Uanis(F29) \\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(F31)
\\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F34) \\sim Ueq:
with sigma of 0.007 and sigma for terminal atoms of 0.014
4. Others
 Sof(F1A)=Sof(H1)=1-FVAR(1)
 Sof(F1)=Sof(H4)=FVAR(1)
 Sof(F14A)=Sof(F15A)=Sof(F16A)=1-FVAR(2)
 Sof(F14)=Sof(F15)=Sof(F16)=FVAR(2)
 Sof(F11A)=Sof(F12A)=Sof(F13A)=1-FVAR(3)
 Sof(F11)=Sof(F12)=Sof(F13)=FVAR(3)
 Fixed Sof: F23(0.5) F23A(0.5) F24(0.5) F24A(0.5) F25(0.5) F25A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230),
 C35(H35), C24(H24), C22(H22), C14(H14), C16(H16), C1(H1), C2(H2), C15(H15),
 C3(H3), C17(H17), C4(H4), C5(H5), C23(H23), C6(H6), C30(H30), C8(H8), C34(H34),
  C9(H9), C10(H10), C11(H11), C29(H29)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              91039
_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 20.925
_oxdiff_exptl_absorpt_empirical_full_min 0.667