Solid- and Solution-Phase Structures of Zinc Enolates of Amides and Ketones
Greco, Jeffrey F.; McNevin, Michael J.; Shoemaker, Richard K.; Hagadorn, John R.; Organometallics 27 (2008) 1948–; doi:10.1021/om800070j

data_4071267
_publ_section_title
;
 Solid- and Solution-Phase Structures of Zinc Enolates of Amides and
 Ketones
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1948
_journal_paper_doi               10.1021/om800070j
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C20 H40 Br2 N2 O4 Zn2'
_chemical_formula_weight         663.10
_chemical_name_common            '{BrZn[CH2C(O)NEt2](thf)}2, (1a)'
_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                 99.5370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6870(5)
_cell_length_b                   8.8254(4)
_cell_length_c                   14.8247(7)
_cell_measurement_temperature    151(2)
_cell_volume                     1378.90(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      151(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1018
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10751
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  0.6528
_exptl_absorpt_correction_T_min  0.4557
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                2383
_reflns_number_total             3280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800070j-file001.cif
_cod_data_source_block           jrh083
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071267