Synthesis, Characterization, and Reaction of a Ketone-Derived 1,4-Dienolate Compound
Gerald Kagan; Weibin Li; Chengzao Sun; Russell Hopson; Paul G. Williard; Journal of Organic Chemistry 76 (2011) 65–70; doi:10.1021/jo1015163

data_4025926
_publ_contact_author_address
;324 Brook Street
Department of Chemistry
Brown University
Providence, Rhode Island 02912
USA
;
_publ_contact_author_email       pgw@brown.edu
_publ_contact_author_name        'Paul G. Williard'
_publ_contact_author_phone       401-863-3589
_publ_section_title
;
 Synthesis, Characterization, and Reaction of a Ketone-Derived
 1,4-Dienolate Compound
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              65
_journal_page_last               70
_journal_paper_doi               10.1021/jo1015163
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C40 H72 Li4 O8'
_chemical_formula_weight         708.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-08-02 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.303(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.739(3)
_cell_length_b                   11.6636(18)
_cell_length_c                   19.941(3)
_cell_measurement_temperature    213(2)
_cell_volume                     4542.9(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21593
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.9752
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1917
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2397
_reflns_number_gt                3619
_reflns_number_total             8893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1015163_si_002_1.cif
_cod_data_source_block           cs21
_cod_original_cell_volume        4542.7(12)
_cod_database_code               4025926