Synthesis of Mixed Alkali-Metal−Zinc Enolate Complexes Derived from 2,4,6-Trimethylacetophenone: New Inverse Crown Structures
Baillie, Sharon E.; Hevia, Eva; Kennedy, Alan R.; Mulvey, Robert E.; Organometallics 26 (2007) 204–; doi:10.1021/om060878k

data_4072613
_publ_section_title
;
 Synthesis of Mixed Alkali-Metal&#x2212;Zinc Enolate Complexes Derived
 from 2,4,6-Trimethylacetophenone:&#x00A0; New Inverse Crown Structures
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              204
_journal_paper_doi               10.1021/om060878k
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C88 H106 Na2 O8 Zn2'
_chemical_formula_weight         1468.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.211(1)
_cell_angle_beta                 76.930(2)
_cell_angle_gamma                68.384(1)
_cell_formula_units_Z            1
_cell_length_a                   11.0238(3)
_cell_length_b                   12.6380(3)
_cell_length_c                   15.7638(4)
_cell_measurement_reflns_used    8856
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1979.71(9)
_computing_data_collection       'Denzo & Collect'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and 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  0.048
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38917
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'chip from prism'
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.9417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                6945
_reflns_number_total             9056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060878ksi20060925_115212.cif
_cod_data_source_block           grem170
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072613