Complete Relative Stereochemistry of Multiple Stereocenters Using Only Residual Dipolar Couplings
Jiangli Yan; Frank Delaglio; Andreas Kaerner; Allen D. Kline; Huaping Mo; Michael J. Shapiro; Tim A. Smitka; Gregory A. Stephenson; Edward R. Zartler; Journal of the American Chemical Society 126 (2004) 5008–5017; doi:10.1021/ja037605q

data_4112453
_publ_section_title
;
 Complete Relative Stereochemistry of Multiple Stereocenters Using Only
 Residual Dipolar Couplings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5008
_journal_page_last               5017
_journal_paper_doi               10.1021/ja037605q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C8 H10 F N O4'
_chemical_formula_weight         203.17
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 96.042(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.065(11)
_cell_length_b                   5.741(3)
_cell_length_c                   7.394(4)
_cell_measurement_temperature    150(2)
_cell_volume                     847.0(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.1339
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2920
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       Bladed
_exptl_crystal_F_000             424
_exptl_crystal_size_max          .11
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .42
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.8(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1691
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                1036
_reflns_number_total             1691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037605qsi20030731_044008.cif
_cod_data_source_block           2061xm
_cod_database_code               4112453