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_4026663
_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         'C72 H108 N4 O8 Na2,C48 H40 B2,C4 H10 O1'
_chemical_formula_sum            'C124 H158 B2 N4 Na2 O9'
_chemical_formula_weight         1916.14
_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                 102.5110(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.5229(3)
_cell_length_b                   15.4122(3)
_cell_length_c                   21.8343(4)
_cell_measurement_reflns_used    14047
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      1.018
_cell_volume                     5756.69(18)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20130
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_correction_T_min  0.9723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       prism
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11530
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1052P)^2^+2.2022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                7962
_reflns_number_total             11530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo201647b_si_002.cif
_cod_data_source_block           jl015
_cod_database_code               4026663