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_4025927
_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 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            'C19 H28 O3'
_chemical_formula_weight         304.41
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.389(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   45.395(13)
_cell_length_b                   9.133(3)
_cell_length_c                   16.710(5)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    196(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.28
_cell_volume                     6711(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      196(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39032
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         0.93
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9765
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      0
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0092(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0782P)^2^+2.1463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                5853
_reflns_number_total             8079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1015163_si_002_2.cif
_cod_data_source_block           czs24_0m
_cod_original_cell_volume        6711(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4025927