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_4026664
_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         'C68 H98 N6 Na2 O6,2(C24 H20 B),C4 H10 O'
_chemical_formula_sum            'C120 H148 B2 N6 Na2 O7'
_chemical_formula_weight         1854.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.1820(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.5568(4)
_cell_length_b                   14.9417(2)
_cell_length_c                   21.8429(5)
_cell_measurement_reflns_used    40044
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     5579.0(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23129
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Monor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       prism
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0040(6)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         12715
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0834P)^2^+2.8635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                7509
_reflns_number_total             12715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo201647b_si_003.cif
_cod_data_source_block           jl020
_cod_database_code               4026664