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_7700125
_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 H20 Cl F4 N2 Rh'
_chemical_formula_sum            'C23 H20 Cl F4 N2 Rh'
_chemical_formula_weight         538.77
_chemical_name_common            Rh(cod)Cl(2,4-F2-IPh)
_chemical_name_systematic
;
  rhodium(cycloocatdienyl)(1,3-bis(2,4-difluorophenyl)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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                87.485(9)
_cell_angle_beta                 72.410(9)
_cell_angle_gamma                67.014(9)
_cell_formula_units_Z            2
_cell_length_a                   9.8017(8)
_cell_length_b                   11.1592(11)
_cell_length_c                   11.2845(13)
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      23.9140
_cell_measurement_theta_min      2.8630
_cell_volume                     1079.3(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -32.00  35.00   1.00    2.79    --  -20.40  57.00  30.00   67
  2  \w    -33.00  50.00   1.00    2.79    --  -20.40  57.00-120.00   83
  3  \w      4.00  75.00   1.00    2.79    --   21.65-116.00 -28.00   71
  4  \w     72.00  99.00   1.00    2.79    --   21.65-178.00 -60.00   27
  5  \w    -96.00  21.00   1.00    2.79    --  -20.40 -19.00  60.00  117
  6  \w    -75.00 -27.00   1.00    2.79    --  -20.40 116.00  59.00   48
;
_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      0.0139205000
_diffrn_orient_matrix_UB_12      0.0150380000
_diffrn_orient_matrix_UB_13      -0.0631427000
_diffrn_orient_matrix_UB_21      -0.0001302000
_diffrn_orient_matrix_UB_22      -0.0603675000
_diffrn_orient_matrix_UB_23      -0.0170659000
_diffrn_orient_matrix_UB_31      -0.0814975000
_diffrn_orient_matrix_UB_32      0.0305116000
_diffrn_orient_matrix_UB_33      0.0100502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7818
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         3.410
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52444
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       irregular
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0482P)^2^+0.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3181
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01219b2.cif
_cod_data_source_block           exp_2794
_cod_depositor_comments
'Adding full bibliography for 7700125--7700129.cif.'
_cod_database_code               7700125
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C23H20F4N2RhCl
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.761
_reflns_odcompleteness_completeness 99.86
_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. Restrained distances
 F1A-C9 \\sim F1-C9
 with sigma of 0.002
3. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(F1A)=1-FVAR(1)
 Sof(F1)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C20(H20), C23(H23)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C21(H21A,H21B), C22(H22A,H22B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C12(H12), C14(H14), C15(H15)
;
_shelx_res_checksum              60263
_olex2_date_sample_data_collection 2018-01-12
_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 1.945
_oxdiff_exptl_absorpt_empirical_full_min 0.459