Metalation of 2,4,6-Trimethylacetophenone Using Organozinc Reagents: The Role of the Base in Determining Composition and Structure of the Developing Enolate
Armstrong, David R.; Drummond, Allison M.; Balloch, Liam; Graham, David V.; Hevia, Eva; Kennedy, Alan R.; Organometallics 27 (2008) 5860–; doi:10.1021/om800658s

data_4072195
_publ_section_title
;
 Metalation of 2,4,6-Trimethylacetophenone Using Organozinc Reagents: The
 Role of the Base in Determining Composition and Structure of the
 Developing Enolate
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5860
_journal_paper_doi               10.1021/om800658s
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C34 H58 Li2 N4 O2'
_chemical_formula_weight         568.72
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.4657(8)
_cell_length_b                   12.1496(6)
_cell_length_c                   8.7833(5)
_cell_measurement_reflns_used    897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.46
_cell_volume                     1757.11(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Oxford Diffraction Xcaliber'
_diffrn_measurement_method       'omega scans'
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4268
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.17 (release 11-02-2008 CrysAlis171 .NET)
(compiled Feb 11 2008,09:33:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.126
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2280
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                1447
_reflns_number_total             2280
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800658s_si_002.cif
_cod_data_source_block           rab3
_cod_original_sg_symbol_H-M      Pnn2
_cod_database_code               4072195