Structure Assignment of Lagunapyrone B by Fluorous Mixture Synthesis of Four Candidate Stereoisomers
Fanglong Yang; Jeffery J. Newsome; Dennis P. Curran; Journal of the American Chemical Society 128 (2006) 14200–14205; doi:10.1021/ja064812s

data_4111037
_publ_section_title
;
 Structure Assignment of Lagunapyrone B by Fluorous Mixture Synthesis of
 Four Candidate Stereoisomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14200
_journal_page_last               14205
_journal_paper_doi               10.1021/ja064812s
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C20 H28 N O5'
_chemical_formula_weight         362.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 110.7240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7705(6)
_cell_length_b                   8.6569(5)
_cell_length_c                   11.6622(7)
_cell_measurement_reflns_used    2105
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.69
_cell_measurement_theta_min      2.21
_cell_volume                     1017.02(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9965
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             390
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.0(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4574
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.220
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                2804
_reflns_number_total             4574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064812ssi20060707_125743.cif
_cod_data_source_block           fy0415s
_cod_database_code               4111037