Simple NMR predictors of catalytic hydrogenation activity for [Rh(cod)Cl(NHC)] complexes featuring fluorinated NHC ligands.
Jamil, Mohamad Shazwan Shah; Alkaabi, Sultan; Brisdon, Alan K.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9317–9327; doi:10.1039/c9dt01219b

data_7700129
_publ_section_title
;
 Simple NMR predictors of catalytic hydrogenation activity for
 [Rh(cod)Cl(NHC)] complexes featuring fluorinated NHC ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9317
_journal_page_last               9327
_journal_paper_doi               10.1039/c9dt01219b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C23 H18 Cl F6 N2 Rh'
_chemical_formula_sum            'C23 H18 Cl F6 N2 Rh'
_chemical_formula_weight         574.76
_chemical_name_systematic
;
  rhodium(cycloocatdienyl)(1,3-bis(2,4,6-trifluorophenyl)imidazol-2-ylidene)chloride
;
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-12 deposited with the CCDC.    2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                94.178(4)
_cell_angle_beta                 100.162(5)
_cell_angle_gamma                98.840(5)
_cell_formula_units_Z            2
_cell_length_a                   7.6327(5)
_cell_length_b                   10.2120(5)
_cell_length_c                   13.8732(8)
_cell_measurement_reflns_used    3049
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      27.6250
_cell_measurement_theta_min      3.1270
_cell_volume                     1046.17(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.8609
_diffrn_measured_fraction_theta_max 0.8609
_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    -64.00 -19.00   1.00    2.00    --  -20.40  96.00 118.00   45
  2  \w    -85.00  44.00   1.00    2.00    --  -20.40  19.00 -90.00  129
  3  \w     39.00  66.00   1.00    2.00    --   21.65 178.00-150.00   27
  4  \w    -93.00  11.00   1.00    2.00    --  -20.40 -77.00 -60.00  104
  5  \w     46.00 104.00   1.00    2.00    --   21.65-178.00 -30.00   58
  6  \w     48.00  99.00   1.00    2.00    --   21.65-178.00 150.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0515123000
_diffrn_orient_matrix_UB_12      -0.0493674000
_diffrn_orient_matrix_UB_13      0.0217681000
_diffrn_orient_matrix_UB_21      0.0146718000
_diffrn_orient_matrix_UB_22      0.0435967000
_diffrn_orient_matrix_UB_23      0.0439217000
_diffrn_orient_matrix_UB_31      -0.0794260000
_diffrn_orient_matrix_UB_32      0.0256118000
_diffrn_orient_matrix_UB_33      -0.0179955000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8198
_diffrn_reflns_theta_full        28.8714
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.8244
_exptl_crystal_description       irregular
_exptl_crystal_F_000             570.3982
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.0975
_refine_diff_density_min         -1.2587
_refine_diff_density_rms         0.1895
_refine_ls_d_res_high            0.7360
_refine_ls_d_res_low             6.7916
_refine_ls_goodness_of_fit_ref   1.0320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0320
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.9563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3833
_reflns_number_total             4733
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt01219b2.cif
_cod_data_source_block           aab18
_cod_depositor_comments
'Adding full bibliography for 7700125--7700129.cif.'
_cod_database_code               7700129
_chemical_oxdiff_formula         C23H28F6N2RhCl
_chemical_oxdiff_usercomment     PJC
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C19(H19), C16(H16), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C22(H22a,H22b), C17(H17a,H17b), C18(H18a,H18b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C2(H2), C6(H6), C14(H14), C12(H12)
;
_olex2_date_sample_data_collection 2017-12-16
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.759
_oxdiff_exptl_absorpt_empirical_full_min 0.671