Synthesis and Characterization of New Mixed-Metal Sodium−Magnesium Enolates Derived from 2,4,6-Trimethylacetophenone†
Hevia, Eva; Henderson, Kenneth W.; Kennedy, Alan R.; Mulvey, Robert E.; Organometallics 25 (2006) 1778–; doi:10.1021/om051076c

data_4074982
_publ_section_title
;
 Synthesis and Characterization of New Mixed-Metal Sodium&#x2212;Magnesium
 Enolates Derived from 2,4,6-Trimethylacetophenone&#x2020;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1778
_journal_paper_doi               10.1021/om051076c
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C56 H84 Mg N4 Na2 O4'
_chemical_formula_weight         947.56
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   16.8170(3)
_cell_length_b                   18.4174(3)
_cell_length_c                   37.6423(6)
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      0.41
_cell_volume                     11658.8(3)
_computing_data_collection       'Denzo & Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16944
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated plate'
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+9.4109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                4768
_reflns_number_total             9129
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om051076csi20051216_120730.cif
_cod_data_source_block           grem180
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4074982