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_7700128
_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(26-F2-IPh)
_chemical_name_systematic
;
  rhodium(cycloocatdienyl)(1,3-bis(2,6-difluorophenyl)imidazol-2-ylidene)chloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 97.959(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7678(8)
_cell_length_b                   10.2888(6)
_cell_length_c                   30.2124(18)
_cell_measurement_reflns_used    3080
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      22.9890
_cell_measurement_theta_min      3.4360
_cell_volume                     4238.5(4)
_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(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -36.00  37.00   1.00    5.00    --   21.65 -57.00 -30.00   73
  2  \w      9.00  82.00   1.00    5.00    --   21.65-126.00 -32.00   73
  3  \w    -45.00  96.00   1.00    5.00    --   21.65  19.00 150.00  141
  4  \w     35.00  92.00   1.00    5.00    --   21.65 178.00 -60.00   57
  5  \w     28.00  63.00   1.00    5.00    --   21.65  57.00-180.00   35
  6  \w    -81.00 -32.00   1.00    5.00    --  -20.32 126.00  43.00   49
;
_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      0.0453237000
_diffrn_orient_matrix_UB_12      0.0011395000
_diffrn_orient_matrix_UB_13      0.0143934000
_diffrn_orient_matrix_UB_21      0.0225093000
_diffrn_orient_matrix_UB_22      0.0307334000
_diffrn_orient_matrix_UB_23      -0.0169628000
_diffrn_orient_matrix_UB_31      -0.0120530000
_diffrn_orient_matrix_UB_32      0.0617118000
_diffrn_orient_matrix_UB_33      0.0082028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_unetI/netI     0.1204
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14924
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31413
_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    1.689
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2160
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0103P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             4160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01219b2.cif
_cod_data_source_block           aab16
_cod_depositor_comments
'Adding full bibliography for 7700125--7700129.cif.'
_cod_database_code               7700128
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C23H20F4N2RhCl
_chemical_oxdiff_usercomment     PJC
_reflns_odcompleteness_completeness 99.87
_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 Fixed occupancy and ADP/Uiso:
 C23, H23A, H23B
2.b Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C20(H20), C21(H21)
2.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              25099
_olex2_date_sample_data_collection 2017-12-15
_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 3.112
_oxdiff_exptl_absorpt_empirical_full_min 0.534