Synthesis of the BCDE Molecular Fragment of Azadiradione Mediated by Titanocene(III)
A. Fernández-Mateos; S. Encinas Madrazo; P. Herrero Teijón; R. Rabanedo Clemente; R. Rubio González; F. Sanz González; Journal of Organic Chemistry 78 (2013) 9571–9578; doi:10.1021/jo401646g

data_4028648
_publ_contact_author_address
;
Departamento de Qu\'imica Org\'anica,
Universidad de Salamanca,
Plaza de los Ca\'idos,
37008-Salamanca. Spain
;
_publ_contact_author_email       afmateos@usal.es
_publ_contact_author_fax         '34 923294400'
_publ_contact_author_name        'A. Fer\n'andez-Mateos'
_publ_contact_author_phone       '34 923294574'
_publ_section_title
;
 Synthesis of the BCDE Molecular Fragment of Azadiradione Mediated by
 Titanocene(III)
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9571
_journal_page_last               9578
_journal_paper_doi               10.1021/jo401646g
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C17 H28 O2'
_chemical_formula_sum            'C17 H28 O2'
_chemical_formula_weight         264.39
_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                 105.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.878(2)
_cell_length_b                   9.0820(18)
_cell_length_c                   16.052(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      8
_cell_volume                     1526.4(5)
_computing_cell_refinement       'CRYSOM (Martinez-Ripoll et al., 1996)'
_computing_data_collection       'CRYSOM (Martinez-Ripoll et al., 1996)'
_computing_data_reduction        'XRAY-80 (University of Maryland, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2003)'
_computing_publication_material  'SHELXTL (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SEIFERT XRD 3003 SC'
_diffrn_measurement_method       2theta-omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2254
_diffrn_reflns_theta_full        59.95
_diffrn_reflns_theta_max         59.95
_diffrn_reflns_theta_min         4.41
_diffrn_standards_decay_%        'no decay, variation 0.5'
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.119
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.0163(9)
_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   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         2254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0557P)^2^+0.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                1873
_reflns_number_total             2254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo401646g_si_003.cif
_cod_data_source_block           inver
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4028648