Imidazolidene Carboxylate Bound MBPh4 Complexes (M = Li, Na) and Their Relevance in Transcarboxylation Reactions
Bret R. Van Ausdall; Nils F. Poth; Virginia A. Kincaid; Atta M. Arif; Janis Louie; Journal of Organic Chemistry 76 (2011) 8413–8420; doi:10.1021/jo201647b

data_4026665
_publ_section_title
;
 Imidazolidene Carboxylate Bound MBPh4 Complexes (M = Li, Na) and Their
 Relevance in Transcarboxylation Reactions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8413
_journal_page_last               8420
_journal_paper_doi               10.1021/jo201647b
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C40 H60 Li N2 O5,B 4(C6 H5)'
_chemical_formula_sum            'C64 H80 B Li N2 O5'
_chemical_formula_weight         975.05
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.4843(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8430(2)
_cell_length_b                   24.0388(5)
_cell_length_c                   12.5088(3)
_cell_measurement_reflns_used    7035
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2919.30(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11711
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         11711
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.6535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                8056
_reflns_number_total             11711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo201647b_si_004.cif
_cod_data_source_block           jl018
_cod_database_code               4026665