Total Synthesis and Structure Confirmation of Elatenyne: Success of Computational Methods for NMR Prediction with Highly Flexible Diastereomers
Bryony S. Dyson; Jonathan W. Burton; Te-ik Sohn; Byungsook Kim; Hoon Bae; Deukjoon Kim; Journal of the American Chemical Society 134 (2012) 11781–11790; doi:10.1021/ja304554e

data_4118275
_publ_section_title
;
 Total Synthesis and Structure Confirmation of Elatenyne: Success of
 Computational Methods for NMR Prediction with Highly Flexible
 Diastereomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11781
_journal_page_last               11790
_journal_paper_doi               10.1021/ja304554e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C12 H20 Br N O2'
_chemical_formula_sum            'C12 H20 Br N O2'
_chemical_formula_weight         290.20
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.4863(9)
_cell_length_b                   10.2943(8)
_cell_length_c                   15.4841(14)
_cell_measurement_reflns_used    7518
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      3.11
_cell_volume                     1352.7(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13134
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.035
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             600.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.550
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1300 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.001(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3075
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.4950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                2098
_reflns_number_total             3075
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja304554e_si_003.cif
_cod_data_source_block           23b
_cod_database_code               4118275