Stereochemical investigation on the construction of poly-functionalized bicyclo[3.3.1]nonenones by successive Michael reactions of 2-cyclohexenones.
Takagi, Ryukichi; Miwa, Yukiko; Nerio, Takashi; Inoue, Yuta; Matsumura, Shuji; Ohkata, Katsuo; Organic & biomolecular chemistry 5 (2007) 286–300; doi:10.1039/b615702e

data_7151061
_publ_section_title
;
 Stereochemical investigation on the construction of
 poly-functionalized bicyclo[3.3.1]nonenones by successive Michael
 reactions of 2-cyclohexenones.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              286
_journal_page_last               300
_journal_paper_doi               10.1039/b615702e
_journal_volume                  5
_journal_year                    2007
_chemical_formula_moiety         'C18 H56 O12'
_chemical_formula_sum            'C19 H28 O6'
_chemical_formula_weight         352.43
_chemical_melting_point          351.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Jul 2 21:45:00 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                85.225(1)
_cell_angle_beta                 77.416(1)
_cell_angle_gamma                68.107(1)
_cell_formula_units_Z            4
_cell_length_a                   9.8930(3)
_cell_length_b                   11.1740(2)
_cell_length_c                   19.1870(7)
_cell_measurement_temperature    273.2
_cell_volume                     1920.77(10)
_computing_cell_refinement       Scalepack
_computing_data_collection       Denzo
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.8854
_diffrn_measured_fraction_theta_max 0.8854
_diffrn_measurement_device_type  'MacScience DIP2030'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8161
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.132
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7906
_refine_ls_R_factor_gt           0.1225
_refine_ls_shift/su_max          0.1377
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.20000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4492
_reflns_number_gt                6944
_reflns_number_total             8161
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b615702e.txt
_cod_data_source_block           g-3-EtO-6-(EtO2C)bicyclo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '78C' was changed to '351.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C19 H28 O6 '
_cod_database_code               7151061