Tris(carbene)borates; alternatives to cyclopentadienyls in organolanthanide chemistry.
Price, Amy N.; Gupta, Ankur K.; de Jong, Wibe A.; Arnold, Polly L.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00718a

data_7712813
_publ_section_title
;
 Tris(carbene)borates; alternatives to cyclopentadienyls in
 organolanthanide chemistry.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00718a
_journal_year                    2023
_chemical_formula_moiety         'C36 H40 B2 N12 Yb, I'
_chemical_formula_sum            'C36 H40 B2 I N12 Yb'
_chemical_formula_weight         962.36
_chemical_name_systematic
'bis(Phenyl tris(3-methylimidazol-1-yl-2-ylidene)borate)-ytterbium(iii) iodide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-12 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.98200(10)
_cell_length_b                   21.9170(2)
_cell_length_c                   40.0903(3)
_cell_measurement_reflns_used    75704
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      77.0770
_cell_measurement_theta_min      4.0180
_cell_volume                     8770.78(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -89.00 -15.00   0.50    0.44    --  -50.02 129.00  31.00  148
  2  \w   -122.00 -71.00   0.50    0.44    --  -50.02-129.00 -41.00  102
  3  \w   -122.00 -63.00   0.50    0.44    --  -50.02-140.00 145.00  118
  4  \w    -97.00 -21.00   0.50    0.44    --  -50.02 140.00-155.00  152
  5  \w     43.00 104.00   0.50    0.44    --   50.02-140.00 145.00  122
  6  \w     37.00  98.00   0.50    0.44    --   50.02-129.00 -41.00  122
  7  \w    -89.00 -15.00   0.50    1.75    --  -84.25 129.00  31.00  148
  8  \w   -156.00 -71.00   0.50    1.75    --  -84.25-129.00 -41.00  170
  9  \w    -97.00 -21.00   0.50    1.75    --  -84.25 140.00-155.00  152
 10  \w     37.00 114.00   0.50    1.75    --  105.67-129.00 -41.00  154
 11  \w     43.00 123.00   0.50    1.75    --  105.67-140.00 145.00  160
 12  \w     85.00 173.00   0.50    1.75    --  105.67 140.00-155.00  176
 13  \w     93.00 178.00   0.50    1.75    --  105.67 129.00  31.00  170
 14  \w    -22.00  23.00   0.50    0.44    --  -50.02  19.00-180.00   90
 15  \w   -122.00 -82.00   0.50    0.44    --  -50.02 -57.00   0.00   80
 16  \w   -122.00 -87.00   0.50    0.44    --  -50.02-125.00   0.00   70
 17  \w   -122.00 -82.00   0.50    0.44    --  -50.02 -57.00-150.00   80
 18  \w   -122.00 -82.00   0.50    0.44    --  -50.02 -57.00 -60.00   80
 19  \w   -122.00 -82.00   0.50    0.44    --  -50.02 -57.00  90.00   80
 20  \w    -22.00  23.00   0.50    0.44    --  -50.02  19.00 -30.00   90
 21  \w   -122.00 -87.00   0.50    0.44    --  -50.02-125.00 -90.00   70
 22  \w    -40.00 -12.00   0.50    1.75    --  -84.25  37.00  90.00   56
 23  \w    -40.00 -12.00   0.50    1.75    --  -84.25  37.00 -90.00   56
 24  \w   -158.00 -77.00   0.50    1.75    --  -84.25 -19.00 120.00  162
 25  \w   -134.00 -76.00   0.50    1.75    --  -84.25 -37.00-180.00  116
 26  \w    -40.00 -14.00   0.50    1.75    --  -84.25  37.00   0.00   52
 27  \w   -134.00-109.00   0.50    1.75    --  -84.25-140.00 145.00   50
 28  \w     34.00  67.00   0.50    1.75    --  105.67 -57.00  90.00   66
 29  \w    115.00 141.00   0.50    1.75    --  105.67  19.00  30.00   52
 30  \w     34.00  66.00   0.50    1.75    --  105.67 -57.00   0.00   64
 31  \w     97.00 141.00   0.50    1.75    --  105.67 125.00 150.00   88
 32  \w     93.00 178.00   0.50    1.75    --  105.67  57.00 -60.00  170
 33  \w     37.00  63.00   0.50    1.75    --  105.67 -57.00 150.00   52
 34  \w     35.00  67.00   0.50    1.75    --  105.67 -57.00 -30.00   64
 35  \w     36.00 106.00   0.50    1.75    --  105.67 -99.00 -90.00  140
 36  \w     35.00  67.00   0.50    1.75    --  105.67 -57.00-180.00   64
 37  \w    122.00 177.00   0.50    1.75    --  105.67  77.00  30.00  110
 38  \w     35.00 106.00   0.50    1.75    --  105.67 -99.00-150.00  142
 39  \w     71.00 103.00   0.50    1.75    --  105.67-125.00  60.00   64
 40  \w     80.00 106.00   0.50    1.75    --  105.67 -99.00 120.00   52
 41  \w    153.00 178.00   0.50    1.75    --  105.67  19.00  30.00   50
 42  \w     34.00  66.00   0.50    1.75    --  105.67 -57.00  30.00   64
 43  \w     41.00 106.00   0.50    1.75    --  105.67 -99.00   0.00  130
 44  \w    112.00 177.00   0.50    1.75    --  105.67  37.00 -30.00  130
 45  \w     38.00  66.00   0.50    1.75    --  105.67 -57.00 -60.00   56
 46  \w     49.00 109.00   0.50    1.75    --  105.67-125.00 150.00  120
 47  \w     96.00 173.00   0.50    1.75    --  105.67 125.00  60.00  154
 48  \w     34.00 102.00   0.50    1.75    --  105.67 -99.00-180.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128645000
_diffrn_orient_matrix_UB_12      -0.0040321000
_diffrn_orient_matrix_UB_13      0.0382450000
_diffrn_orient_matrix_UB_21      -0.1516130000
_diffrn_orient_matrix_UB_22      -0.0114124000
_diffrn_orient_matrix_UB_23      -0.0035125000
_diffrn_orient_matrix_UB_31      0.0254932000
_diffrn_orient_matrix_UB_32      -0.0692397000
_diffrn_orient_matrix_UB_33      -0.0016507000
_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  0.0580
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            160321
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.498
_diffrn_reflns_theta_min         4.034
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.771
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       plate
_exptl_crystal_F_000             3784
_exptl_crystal_preparation       'methathesis from YbI3 and Li[TCMe]'
_exptl_crystal_recrystallization_method 'from thf'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0356P)^2^+43.5865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8696
_reflns_number_total             9095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00718a2.cif
_cod_data_source_block           pla21024_0_8refin
_cod_database_code               7712813
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Yb N12 B2 C40.8 H49.6  I1 O1.2 '
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.304
_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.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C24(H24), C18(H18), C30(H30), C15(H15), C9(H9), C26(H26), C23(H23),
 C21(H21), C20(H20), C14(H14), C29(H29), C8(H8), C27(H27), C36(H36), C12(H12),
 C28(H28), C32(H32), C33(H33), C11(H11), C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C16(H16A,H16B,H16C), C7(H7A,H7B,
 H7C), C13(H13A,H13B,H13C), C10(H10A,H10B,H10C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 402 electrons were 
found in a volume of 1696\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.25[C4H8O] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19349
_shelx_hkl_checksum              22615
_shelx_fab_checksum              70206
_olex2_exptl_crystal_mounting_method 'In fomblin on a glass fiber loop'
_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 1.771
_oxdiff_exptl_absorpt_empirical_full_min 0.612