Dynamic 1H NMR Spectroscopic Study of the Ring Inversion in N-Sulfonyl Morpholines-Studies on N-S Interactions
Ali Reza Modarresi-Alam; Homeyra Alsadat Amirazizi; Hajar Bagheri; Hamid-Reza Bijanzadeh; Erich Kleinpeter; Journal of Organic Chemistry 74 (2009) 4740–4746; doi:10.1021/jo900454a

data_4024620
_publ_section_title
;
Dynamic 1H NMR Spectroscopic Study of the Ring Inversion in N-Sulfonyl
Morpholines-Studies on N-S Interactions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4740
_journal_page_last               4746
_journal_paper_doi               10.1021/jo900454a
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C11 H15 N O3 S'
_chemical_formula_weight         241.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.694(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.068(2)
_cell_length_b                   18.294(3)
_cell_length_c                   8.815(2)
_cell_measurement_reflns_used    10013
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.17
_cell_volume                     1208.8(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 180 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method, delta omega = 1.0 deg'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7731
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.23
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.26
_exptl_absorpt_correction_T_max  0.9040
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.475
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.1618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                1820
_reflns_number_total             2126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo900454a_si_002.cif
_cod_data_source_block           kp5ni
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4024620