A simply accessible organometallic system to gauge electronic properties of N-heterocyclic carbenes.
Bru, Francis; Charman, Rex S. C.; Bourda, Laurens; Van Hecke, Kristof; Grimaud, Laurence; Liptrot, David J.; Cazin, Catherine S. J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16030–16037; doi:10.1039/d4dt02584a

data_7717041
_publ_section_title
;
 A simply accessible organometallic system to gauge electronic properties
 of N-heterocyclic carbenes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16030
_journal_page_last               16037
_journal_paper_doi               10.1039/d4dt02584a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H47 N2 O3 Rh, C H2 Cl2'
_chemical_formula_sum            'C35 H49 Cl2 N2 O3 Rh'
_chemical_formula_weight         719.57
_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
_audit_creation_date             2022-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.36820(10)
_cell_length_b                   23.62040(10)
_cell_length_c                   14.93630(10)
_cell_measurement_reflns_used    21168
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7610
_cell_measurement_theta_min      3.5690
_cell_volume                     3528.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -70.00  31.00   1.00    1.00    --  -41.68  57.00 150.00  101
  2  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-180.00   81
  3  \w     17.00 116.00   1.00    1.00    --   41.68  38.00  60.00   99
  4  \w     33.00 132.00   1.00    2.50    --  106.01 -45.00  60.00   99
  5  \w     30.00 139.00   1.00    2.50    --  106.01 -77.00 -90.00  109
  6  \w    103.00 178.00   1.00    2.50    --  106.01  77.00 -90.00   75
  7  \w     77.00 178.00   1.00    2.50    --  106.01  61.00  60.00  101
  8  \w     30.00 134.00   1.00    2.50    --  106.01 -30.00-120.00  104
  9  \w     14.00 115.00   1.00    1.00    --   41.68  57.00 120.00  101
 10  \w     17.00 116.00   1.00    1.00    --   41.68  38.00 -60.00   99
 11  \w     14.00 115.00   1.00    1.00    --   41.68  57.00-180.00  101
 12  \w     33.00 112.00   1.00    2.50    --  106.01-125.00-120.00   79
 13  \w     77.00 178.00   1.00    2.50    --  106.01  61.00   0.00  101
 14  \w     78.00 178.00   1.00    2.50    --  106.01  30.00 150.00  100
 15  \w     23.00 107.00   1.00    2.50    --  106.01 -94.00  60.00   84
 16  \w     78.00 178.00   1.00    2.50    --  106.01  30.00 -60.00  100
 17  \w     77.00 178.00   1.00    2.50    --  106.01  61.00-150.00  101
 18  \w    -87.00  -6.00   1.00    1.00    --  -41.68 125.00 -60.00   81
 19  \w     14.00 115.00   1.00    1.00    --   41.68  57.00-120.00  101
 20  \w     14.00 115.00   1.00    1.00    --   41.68  57.00 -30.00  101
 21  \w     77.00 149.00   1.00    2.50    --  106.01  61.00-120.00   72
 22  \w     77.00 178.00   1.00    2.50    --  106.01  61.00 -30.00  101
 23  \w     80.00 178.00   1.00    2.50    --  106.01  45.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0682841000
_diffrn_orient_matrix_UB_12      -0.0582727000
_diffrn_orient_matrix_UB_13      -0.0053402000
_diffrn_orient_matrix_UB_21      -0.0870124000
_diffrn_orient_matrix_UB_22      0.0221096000
_diffrn_orient_matrix_UB_23      0.0616684000
_diffrn_orient_matrix_UB_31      -0.1072436000
_diffrn_orient_matrix_UB_32      0.0191552000
_diffrn_orient_matrix_UB_33      -0.0872284000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47282
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.823
_diffrn_reflns_theta_min         3.594
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.580
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.2245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6055
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02584a2.cif
_cod_data_source_block           fb226
_cod_depositor_comments
'Adding full bibliography for 7717040--7717041.cif.'
_cod_database_code               7717041
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CRhNOH
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.106
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C31(H31)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              48520
_shelx_hkl_checksum              7656
_olex2_date_sample_data_collection 2022-10-11
_olex2_exptl_crystal_mounting_method 'Mounted on a LythoLoop'
_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 2.699
_oxdiff_exptl_absorpt_empirical_full_min 0.580