Cyclobutane Amino Acid Analogues of Furanomycin Obtained by a Formal [2 + 2] Cycloaddition Strategy Promoted by Methylaluminoxane
Alberto Avenoza; Jesús H. Busto; Noelia Canal; Francisco Corzana; Jesús M. Peregrina; Marta Pérez-Fernández; Fernando Rodríguez; Journal of Organic Chemistry 75 (2010) 545–552; doi:10.1021/jo9025258

data_4025212
_publ_contact_author_address     'Madre de Dios 51'
_publ_contact_author_email       hector.busto@unirioja.es
_publ_contact_author_name        'Hector Busto'
_publ_section_title
;
 Cyclobutane Amino Acid Analogues of Furanomycin Obtained by a Formal [2 +
 2] Cycloaddition Strategy Promoted by Methylaluminoxane
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              545
_journal_page_last               552
_journal_paper_doi               10.1021/jo9025258
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C10 H12 F3 N O4'
_chemical_formula_weight         267.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.1510(4)
_cell_length_b                   8.9090(6)
_cell_length_c                   17.2250(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2325.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13222
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.147
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0766P)^2^+1.6253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                1705
_reflns_number_total             2268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9025258_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4025212