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_7704382
_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 H25 F2 N5 Rh, C32 H12 B F24'
_chemical_formula_sum            'C63 H37 B F26 N5 Rh'
_chemical_formula_weight         1471.69
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 106.8752(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.68561(11)
_cell_length_b                   27.25348(15)
_cell_length_c                   18.40461(13)
_cell_measurement_reflns_used    28114
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3700
_cell_measurement_theta_min      2.9360
_cell_volume                     6088.98(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (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   -117.00 -18.00   1.00    3.50    --  -42.07 -37.00-150.00   99
  2  \w    -92.00  -2.00   1.00    3.50    --  -42.07 125.00 150.00   90
  3  \w    -92.00  -2.00   1.00    3.50    --  -42.07 125.00  90.00   90
  4  \w      1.00  83.00   1.00    3.50    --   42.07 -99.00  90.00   82
  5  \w     24.00 110.00   1.00   14.00    --  107.00 -94.00-150.00   86
  6  \w     34.00 118.00   1.00   14.00    --  107.00-125.00  90.00   84
  7  \w     34.00 133.00   1.00   14.00    --  107.00 -45.00  90.00   99
  8  \w     34.00 118.00   1.00   14.00    --  107.00-125.00   0.00   84
  9  \w     94.00 178.00   1.00   14.00    --  107.00 125.00-150.00   84
 10  \w     74.00 178.00   1.00   14.00    --  107.00  77.00 120.00  104
 11  \w     94.00 178.00   1.00   14.00    --  107.00 125.00 -90.00   84
 12  \w     81.00 178.00   1.00   14.00    --  107.00  45.00-150.00   97
 13  \w     78.00 178.00   1.00   14.00    --  107.00  61.00-120.00  100
 14  \w     35.00 136.00   1.00   14.00    --  107.00 -61.00-120.00  101
 15  \w   -114.00 -14.00   1.00    3.50    --  -42.07 -57.00 -30.00  100
 16  \w   -118.00 -68.00   1.00    3.50    --  -42.07 -77.00 120.00   50
 17  \w    -32.00  59.00   1.00    3.50    --   42.07 -37.00 -90.00   91
;
_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      0.0687437000
_diffrn_orient_matrix_UB_12      -0.0474984000
_diffrn_orient_matrix_UB_13      0.0122335000
_diffrn_orient_matrix_UB_21      0.0897810000
_diffrn_orient_matrix_UB_22      0.0264281000
_diffrn_orient_matrix_UB_23      -0.0264310000
_diffrn_orient_matrix_UB_31      0.0576356000
_diffrn_orient_matrix_UB_32      0.0155092000
_diffrn_orient_matrix_UB_33      0.0824729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54052
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.072
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         6.497
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.406
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (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    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2936
_exptl_crystal_recrystallization_method
'Crystals grown from 1,2-F2C6H4-hexane at 293 K'
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         11552
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+11.9245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10640
_reflns_number_total             11552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01137a3.cif
_cod_data_source_block           0519abc19s
_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_database_code               7704382
_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
 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
 C215-F17 \\sim C215-F18 \\sim C215-F19 \\sim C215-F17A \\sim C215-F18A \\sim
C215-F19A
 with sigma of 0.01
 F17-F18 \\sim F18-F19 \\sim F19-F17 \\sim F17A-F18A \\sim F18A-F19A \\sim
F19A-F17A
 with sigma of 0.01
 C211-F17 \\sim C211-F18 \\sim C211-F19 \\sim C211-F17A \\sim C211-F18A \\sim
C211-F19A
 with sigma of 0.01
 C216-F20 \\sim C216-F21 \\sim C216-F22 \\sim C216-F20A \\sim C216-F21A \\sim
C216-F22A
 with sigma of 0.01
 F20-F21 \\sim F21-F22 \\sim F22-F20 \\sim F20A-F21A \\sim F21A-F22A \\sim
F22A-F20A
 with sigma of 0.01
 C213-F20 \\sim C213-F21 \\sim C213-F22 \\sim C213-F20A \\sim C213-F21A \\sim
C213-F22A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F14A \\sim F15 \\sim
F15A \\sim F16 \\sim F16A \\sim F17 \\sim F17A \\sim F18 \\sim F18A \\sim F19
\\sim F19A \\sim F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22 \\sim F22A \\sim
F23 \\sim F24 \\sim F25 \\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(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F13) \\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(F17A) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F18A) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20)
\\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(F25) \\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(F20A)=Sof(F21A)=Sof(F22A)=1-FVAR(1)
 Sof(F20)=Sof(F21)=Sof(F22)=FVAR(1)
 Sof(F14A)=Sof(F15A)=Sof(F16A)=1-FVAR(2)
 Sof(F14)=Sof(F15)=Sof(F16)=FVAR(2)
 Sof(F17A)=Sof(F18A)=Sof(F19A)=1-FVAR(3)
 Sof(F17)=Sof(F18)=Sof(F19)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30),
  C34(H34), C35(H35), C202(H202), C204(H204), C206(H206), C210(H210),
 C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226),
 C228(H228), C230(H230)
5.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              23018
_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 23.556
_oxdiff_exptl_absorpt_empirical_full_min 0.417