Heavy alkali metal complexes of N-heterocyclic carbenes.
Groth, Lucie J.; Bockfeld, Dirk; Tamm, Matthias; Chemical communications (Cambridge, England) 61 (2025) 15806–15809; doi:10.1039/d5cc04534g

data_7134934
_publ_section_title
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 Heavy alkali metal complexes of N-heterocyclic carbenes.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15806
_journal_page_last               15809
_journal_paper_doi               10.1039/d5cc04534g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C53 H51 B F15 N2 Na O2 [+ 0.5 (C6 H5 Cl)]'
_chemical_formula_sum            'C56 H53.5 B Cl0.5 F15 N2 Na O2'
_chemical_formula_weight         1123.03
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-08-06 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.631(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4137(2)
_cell_length_b                   21.3940(4)
_cell_length_c                   23.4007(6)
_cell_measurement_reflns_used    16741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1340
_cell_measurement_theta_min      2.8010
_cell_volume                     5188.30(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_publication_material
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68923
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.842
_diffrn_reflns_theta_min         2.805
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.119a (Rigaku Oxford Diffraction, 2024)
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            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10667
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0651P)^2^+4.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7783
_reflns_number_total             10667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04534g2.cif
_cod_data_source_block           lgr17db
_cod_depositor_comments
'Adding full bibliography for 7134934--7134942.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C56 H53.50 B Cl0.50 F15 N2 Na O2'
_cod_database_code               7134934
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.947
_oxdiff_exptl_absorpt_empirical_full_min 0.731
_oxdiff_exptl_absorpt_empirical_full_max 2.248
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
A solvent mask was calculated and 114 electrons were 
found in a volume of 324\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C6H5Cl] per formula unit 
which account for 116 electrons 
per unit cell.
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_shelx_res_checksum              54186
_shelx_fab_checksum              50485