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_7712810
_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 Ce I N12'
_chemical_formula_sum            'C36 H40 B2 Ce I N12'
_chemical_formula_weight         929.44
_chemical_name_systematic
'bis(Phenyl tris(3-methylimidazol-1-yl-2-ylidene)borate)-cerium(iii)iodide'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.7150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.61860(10)
_cell_length_b                   21.6975(3)
_cell_length_c                   20.3758(3)
_cell_measurement_reflns_used    46284
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      31.2830
_cell_measurement_theta_min      2.1090
_cell_volume                     3806.04(9)
_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(11)
_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 1.000
_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    -18.00  25.00   0.50   10.54    --    4.95  77.00 -60.00   86
  2  \w     -7.00  78.00   0.50   10.54    --    4.95  37.00-150.00  170
  3  \w     -8.00  80.00   0.50   10.54    --    4.95  19.00-180.00  176
  4  \w     -1.00  25.00   0.50   10.54    --   -5.34 -99.00-150.00   52
  5  \w     12.00  37.00   0.50   10.54    --   -5.34-123.00 -83.51   50
  6  \w    -25.00  28.00   0.50   10.54    --    4.95 -77.00 -90.00  106
  7  \w    -25.00  28.00   0.50   10.54    --    4.95 -77.00   0.00  106
  8  \w      9.00  49.00   0.50   10.54    --    4.95-119.00  77.11   80
  9  \w     -7.00  38.00   0.50   10.54    --    4.95 -99.00 150.00   90
 10  \w    -25.00  28.00   0.50   10.54    --    4.95 -77.00  60.00  106
 11  \w    -59.00  10.00   0.50   10.54    --   -5.34 -57.00 -30.00  138
 12  \w    -69.00  -5.00   0.50   10.54    --    4.95 -19.00-180.00  128
 13  \w    -76.00 -42.00   0.50   10.54    --   -5.34 -19.00  60.00   68
;
_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      0.0145838000
_diffrn_orient_matrix_UB_12      -0.0241362000
_diffrn_orient_matrix_UB_13      0.0229535000
_diffrn_orient_matrix_UB_21      -0.0051099000
_diffrn_orient_matrix_UB_22      -0.0218439000
_diffrn_orient_matrix_UB_23      -0.0259048000
_diffrn_orient_matrix_UB_31      0.0809334000
_diffrn_orient_matrix_UB_32      0.0029733000
_diffrn_orient_matrix_UB_33      -0.0040900000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79661
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.051
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1844
_exptl_crystal_preparation       'Salt metathesis from CeI3 and Li[TCMe]'
_exptl_crystal_recrystallization_method 'From thf and diethyl ether'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0186P)^2^+5.2228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6974
_reflns_number_total             7779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00718a2.cif
_cod_data_source_block           pla21008_refin_092222
_cod_database_code               7712810
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce1 N12  C36  H40 I1 B2'
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.578
_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:
 C22(H22), C21(H21), C18(H18), C15(H15), C17(H17), C23(H23), C13(H13),
 C19(H19), C36(H36), C29(H29), C35(H35), C14(H14), C26(H26), C16(H16), C30(H30),
  C34(H34), C24(H24), C20(H20), C32(H32), C33(H33), C28(H28), C27(H27)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              58193
_shelx_hkl_checksum              97848
_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.804