Low coordinate Zn(II) organocations bearing extremely bulky NHC ligands: structural features, air-/water-tolerance and use in hydrosilylation and hydrogenation catalysis.
Xu, Xuejuan; Parmentier, Jordan; Gourlaouen, Christophe; Jacques, Béatrice; Dagorne, Samuel; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15849–15858; doi:10.1039/d4dt02152e

data_7716996
_publ_section_title
;
 Low coordinate Zn(II) organocations bearing extremely bulky NHC ligands:
 structural features, air-/water-tolerance and use in hydrosilylation and
 hydrogenation catalysis.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15849
_journal_page_last               15858
_journal_paper_doi               10.1039/d4dt02152e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 B F20, C25 H37 N2 Zn'
_chemical_formula_sum            'C49 H37 B F20 N2 Zn'
_chemical_formula_weight         1109.98
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-07-26 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4956(3)
_cell_length_b                   21.2784(6)
_cell_length_c                   17.7779(5)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.24
_cell_volume                     4685.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            81255
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule
 of the pentane solvent [88/4 = 22 e per asymmetric unit; half
 a molecule of C5H12 would give 21e].
;
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+3.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9227
_reflns_number_total             11229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02152e3.cif
_cod_data_source_block           sdjp210412
_cod_depositor_comments
'Adding full bibliography for 7716994--7716999.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7716996
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.927
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              13425
_shelx_hkl_checksum              35781
_shelx_fab_checksum              88800