Microwave assisted synthesis, crystal structure and modelling of cytotoxic dehydroacetic acid enamine: a natural alkaloid from Fusarium incarnatum (HKI0504)
Seijas, Julio A.; Crecente-Campo, José; Feás, Xesús; Vázquez-Tato, M. Pilar; RSC Adv. 4 (2014) 17054–; doi:10.1039/C4RA00582A

data_7235488
_publ_section_title
;
 Microwave assisted synthesis, crystal structure and modelling of
 cytotoxic dehydroacetic acid enamine: a natural alkaloid from Fusarium
 incarnatum (HKI0504)
;
_journal_issue                   33
_journal_name_full               'RSC Adv.'
_journal_page_first              17054
_journal_paper_doi               10.1039/C4RA00582A
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C16 H18 N2 O6'
_chemical_formula_weight         334.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                92.24(2)
_cell_angle_beta                 98.98(2)
_cell_angle_gamma                111.168(19)
_cell_formula_units_Z            2
_cell_length_a                   6.650(3)
_cell_length_b                   8.898(4)
_cell_length_c                   13.970(6)
_cell_measurement_temperature    100(2)
_cell_volume                     757.3(6)
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.943
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.1380
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3506
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         1.484
_exptl_absorpt_coefficient_mu    0.113
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0842P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1756
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra00582a2.cif
_cod_data_source_block           twin5
_cod_database_code               7235488
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2012-9
_shelx_res_checksum              7709