Anomalous NMR Behavior of Meso Compounds with Remote Stereogenic Centers on Addition of Chiral Shift Reagent or Chiral Solvating Agent
Serap Beşli; Simon J. Coles; David B. Davies; Robert J. Eaton; Michael B. Hursthouse; Adem Kiliç; Robert A. Shaw; Gönül Yenilmez Çiftçi; Serkan Yeşilot; Journal of the American Chemical Society 125 (2003) 4943–4950; doi:10.1021/ja028871r

data_4113662
_publ_section_title
;
 Anomalous NMR Behavior of Meso Compounds with Remote Stereogenic Centers
 on Addition of Chiral Shift Reagent or Chiral Solvating Agent
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4943
_journal_page_last               4950
_journal_paper_doi               10.1021/ja028871r
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C26 H62 Cl4 N14 P6'
_chemical_formula_weight         898.52
_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                   21.039(4)
_cell_length_b                   9.6447(19)
_cell_length_c                   43.486(9)
_cell_measurement_reflns_used    24485
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     8824(3)
_computing_cell_refinement       'DENZO & COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1666
_diffrn_reflns_av_sigmaI/netI    0.2008
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            37555
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9948
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       blade
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                4479
_reflns_number_total             9445
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja028871rsi20030205_052527.cif
_cod_data_source_block           1b(meso)
_cod_database_code               4113662