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data_th2
_audit_creation_method     SHELXL
_chemical_name_systematic
;
(+)-(2S,3S,4S,5S)-(N-t-Butyloxycarbonyl)-2-benzyl-4,5-dimethyl-
3-hydroxy-pyrrolidine
;
_chemical_name_common     ?
_chemical_formula_moiety     ?
_chemical_formula_sum     'C18 H27 N O3'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_weight     305.41
_chemical_melting_point     ?
_symmetry_cell_setting     Monoclinic
_symmetry_space_group_name_H-M     P2(1)
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z'
_cell_length_a     5.9054(8)
_cell_length_b     9.2686(7)
_cell_length_c     15.946(2)
_cell_angle_alpha     90
_cell_angle_beta     97.138(6)
_cell_angle_gamma     90
_cell_volume     866.04(17)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     409
_cell_measurement_theta_min     1.00
_cell_measurement_theta_max     25.00
_cell_measurement_temperature     143
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     1.00
_exptl_crystal_size_mid     0.70
_exptl_crystal_size_min     0.50
_exptl_crystal_density_diffrn     1.171
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     332
_exptl_absorpt_coefficient_mu     0.079
_exptl_absorpt_correction_type     'Empirical, SADABS (Sheldrick,1996a)'
_exptl_absorpt_correction_T_min     0.6100
_exptl_absorpt_correction_T_max     1.0000
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     143
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     'highly oriented graphite crystal'
_diffrn_measurement_device     'Siemens CCD three circle diffractometer'
_diffrn_measurement_method     ω
_diffrn_reflns_number     15294
_diffrn_reflns_av_R_equivalents     0.0382
_diffrn_reflns_av_sigmaI/netI     0.0289
_diffrn_reflns_theta_min     2.55
_diffrn_reflns_theta_max     26.42
_diffrn_reflns_limit_h_min     -7
_diffrn_reflns_limit_h_max     7
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -19
_diffrn_reflns_limit_l_max     19
_diffrn_standards_number     265
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     720
_diffrn_standards_decay_%     0.0
_refine_special_details
;
 Refinement of F² against ALL reflections.  Weighted R-factors wR and all
 goodnesses of fit S are based on F², conventional R-factors R
 are based on F, with F set to zero for negative F². The observed criterion
 of F² > 2sigma(F²) is used only for calculating _R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     3539
_reflns_number_observed     3458
_reflns_observed_criterion     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0369
_refine_ls_R_factor_obs     0.0362
_refine_ls_wR_factor_all     0.0975
_refine_ls_wR_factor_obs     0.0970
_refine_ls_goodness_of_fit_all     1.052
_refine_ls_goodness_of_fit_obs     1.060
_refine_ls_restrained_S_all     1.052
_refine_ls_restrained_S_obs     1.060
_refine_ls_number_reflns     3539
_refine_ls_number_parameters     200
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     'see experimental section'
_refine_ls_weighting_scheme
         'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0829P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/esd_max     0.000
_refine_ls_shift/esd_mean     0.000
_refine_diff_density_max     0.188
_refine_diff_density_min     -0.133
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack     0.0(7)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Siemens SMART'
_computing_cell_refinement     'Siemens SMART'
_computing_data_reduction     'Siemens SAINT'
_computing_structure_solution     'SHELXS-96 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL-96 (Sheldrick, 1996b)'
_computing_molecular_graphics     'XP (Siemens XTL-Plus)'
_computing_publication_material     ?
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_thermal_displace_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_group
    N N1 0.33856(19) 0.64670(12) 0.26695(7) 0.0204(2) Uani d . 1 .
    C C2 0.3634(2) 0.69365(13) 0.35698(8) 0.0193(3) Uani d . 1 .
    H H2 0.2432 0.7670 0.3643 0.023 Uiso calc R 1 .
    C C3 0.5980(2) 0.76918(14) 0.36510(8) 0.0212(3) Uani d . 1 .
    H H3 0.6041 0.8448 0.4101 0.025 Uiso calc R 1 .
    O O31 0.78355(16) 0.67233(11) 0.38428(6) 0.0258(2) Uani d . 1 .
    H H31 0.8101 0.6301 0.3399 0.031 Uiso calc R 1 .
    C C4 0.5950(2) 0.84167(15) 0.27928(9) 0.0221(3) Uani d . 1 .
    H H4 0.4832 0.9231 0.2766 0.027 Uiso calc R 1 .
    C C41 0.8231(3) 0.90298(17) 0.26002(10) 0.0303(3) Uani d . 1 .
    H H41A 0.8760 0.9762 0.3023 0.045 Uiso calc R 1 .
    H H41B 0.8037 0.9469 0.2037 0.045 Uiso calc R 1 .
    H H41C 0.9358 0.8251 0.2617 0.045 Uiso calc R 1 .
    C C5 0.4952(2) 0.72532(14) 0.21664(8) 0.0210(3) Uani d . 1 .
    H H5 0.6194 0.6592 0.2031 0.025 Uiso calc R 1 .
    C C51 0.3764(3) 0.79213(18) 0.13564(9) 0.0319(3) Uani d . 1 .
    H H51A 0.3151 0.7154 0.0970 0.048 Uiso calc R 1 .
    H H51B 0.4863 0.8498 0.1087 0.048 Uiso calc R 1 .
    H H51C 0.2515 0.8542 0.1491 0.048 Uiso calc R 1 .
    C C11 0.1845(2) 0.54765(14) 0.23401(8) 0.0196(3) Uani d . 1 .
    O O11 0.01529(16) 0.50974(11) 0.26522(6) 0.0237(2) Uani d . 1 .
    O O12 0.24427(16) 0.49424(11) 0.16061(6) 0.0243(2) Uani d . 1 .
    C C13 0.0840(2) 0.40591(15) 0.10377(8) 0.0236(3) Uani d . 1 .
    C C14 0.2112(3) 0.3901(2) 0.02719(10) 0.0362(4) Uani d . 1 .
    H H14A 0.3550 0.3388 0.0434 0.054 Uiso calc R 1 .
    H H14B 0.2434 0.4859 0.0055 0.054 Uiso calc R 1 .
    H H14C 0.1172 0.3354 -0.0168 0.054 Uiso calc R 1 .
    C C15 -0.1403(3) 0.4850(2) 0.08037(10) 0.0360(4) Uani d . 1 .
    H H15A -0.1109 0.5783 0.0549 0.054 Uiso calc R 1 .
    H H15B -0.2144 0.5007 0.1313 0.054 Uiso calc R 1 .
    H H15C -0.2404 0.4271 0.0398 0.054 Uiso calc R 1 .
    C C16 0.0486(3) 0.26004(17) 0.14342(10) 0.0366(4) Uani d . 1 .
    H H16A 0.1965 0.2126 0.1580 0.055 Uiso calc R 1 .
    H H16B -0.0488 0.2000 0.1032 0.055 Uiso calc R 1 .
    H H16C -0.0249 0.2734 0.1947 0.055 Uiso calc R 1 .
    C C21 0.3501(2) 0.57258(14) 0.42143(8) 0.0219(3) Uani d . 1 .
    H H21A 0.1995 0.5245 0.4110 0.026 Uiso calc R 1 .
    H H21B 0.4695 0.4997 0.4153 0.026 Uiso calc R 1 .
    C C22 0.3836(2) 0.63399(14) 0.51016(8) 0.0201(3) Uani d . 1 .
    C C23 0.5909(2) 0.61798(14) 0.56184(9) 0.0234(3) Uani d . 1 .
    H H23 0.7125 0.5670 0.5415 0.028 Uiso calc R 1 .
    C C24 0.6207(2) 0.67607(16) 0.64302(9) 0.0267(3) Uani d . 1 .
    H H24 0.7626 0.6646 0.6776 0.032 Uiso calc R 1 .
    C C25 0.4440(3) 0.75077(15) 0.67379(8) 0.0269(3) Uani d . 1 .
    H H25 0.4646 0.7901 0.7292 0.032 Uiso calc R 1 .
    C C26 0.2372(3) 0.76739(15) 0.62273(9) 0.0266(3) Uani d . 1 .
    H H26 0.1158 0.8183 0.6433 0.032 Uiso calc R 1 .
    C C27 0.2079(2) 0.70968(15) 0.54180(9) 0.0242(3) Uani d . 1 .
    H H27 0.0659 0.7218 0.5073 0.029 Uiso calc R 1 .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    N1 0.0238(5) 0.0220(5) 0.0155(5) -0.0042(4) 0.0033(4) -0.0023(4)
    C2 0.0219(6) 0.0195(6) 0.0164(6) 0.0004(5) 0.0020(4) -0.0034(5)
    C3 0.0221(6) 0.0204(6) 0.0211(6) -0.0001(5) 0.0031(5) -0.0048(5)
    O31 0.0232(4) 0.0331(5) 0.0206(5) 0.0052(4) 0.0007(4) -0.0030(4)
    C4 0.0228(6) 0.0192(6) 0.0247(6) -0.0005(5) 0.0044(5) -0.0021(5)
    C41 0.0295(7) 0.0277(7) 0.0344(8) -0.0075(6) 0.0065(6) 0.0010(6)
    C5 0.0216(6) 0.0228(6) 0.0193(6) -0.0025(5) 0.0053(5) -0.0009(5)
    C51 0.0351(8) 0.0374(8) 0.0227(7) -0.0091(6) 0.0017(6) 0.0068(6)
    C11 0.0227(6) 0.0188(6) 0.0164(6) 0.0008(5) -0.0005(5) -0.0010(5)
    O11 0.0250(5) 0.0268(5) 0.0197(4) -0.0057(4) 0.0042(4) -0.0037(4)
    O12 0.0244(5) 0.0286(5) 0.0199(4) -0.0043(4) 0.0031(4) -0.0083(4)
    C13 0.0275(7) 0.0243(6) 0.0182(6) -0.0031(5) -0.0004(5) -0.0075(5)
    C14 0.0405(8) 0.0422(9) 0.0269(7) -0.0058(7) 0.0081(6) -0.0131(6)
    C15 0.0335(8) 0.0410(9) 0.0307(8) 0.0061(7) -0.0067(6) -0.0083(7)
    C16 0.0547(10) 0.0247(7) 0.0294(8) -0.0066(7) 0.0012(7) -0.0037(6)
    C21 0.0282(6) 0.0198(6) 0.0177(6) -0.0027(5) 0.0022(5) -0.0028(5)
    C22 0.0260(6) 0.0164(6) 0.0181(6) -0.0037(5) 0.0036(5) 0.0000(5)
    C23 0.0269(6) 0.0225(6) 0.0208(7) -0.0012(5) 0.0034(5) 0.0020(5)
    C24 0.0289(7) 0.0282(7) 0.0217(6) -0.0070(6) -0.0016(5) 0.0024(5)
    C25 0.0391(8) 0.0245(6) 0.0172(6) -0.0095(6) 0.0041(6) -0.0020(5)
    C26 0.0327(7) 0.0235(7) 0.0252(7) -0.0025(5) 0.0096(5) -0.0029(5)
    C27 0.0237(6) 0.0263(7) 0.0227(6) -0.0025(5) 0.0029(5) -0.0003(5)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    N1 C11 . 1.3520(16) ?
    N1 C5 . 1.4883(16) ?
    N1 C2 . 1.4898(15) ?
    C2 C21 . 1.5303(17) ?
    C2 C3 . 1.5433(18) ?
    C3 O31 . 1.4202(16) ?
    C3 C4 . 1.5227(19) ?
    C4 C41 . 1.5277(19) ?
    C4 C5 . 1.5368(18) ?
    C5 C51 . 1.5227(19) ?
    C11 O11 . 1.2219(17) ?
    C11 O12 . 1.3574(16) ?
    O12 C13 . 1.4745(15) ?
    C13 C14 . 1.518(2) ?
    C13 C16 . 1.518(2) ?
    C13 C15 . 1.519(2) ?
    C21 C22 . 1.5151(17) ?
    C22 C23 . 1.396(2) ?
    C22 C27 . 1.3979(19) ?
    C23 C24 . 1.393(2) ?
    C24 C25 . 1.392(2) ?
    C25 C26 . 1.390(2) ?
    C26 C27 . 1.388(2) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C11 N1 C5 . . 123.81(11) ?
    C11 N1 C2 . . 123.61(11) ?
    C5 N1 C2 . . 112.53(10) ?
    N1 C2 C21 . . 115.20(10) ?
    N1 C2 C3 . . 101.14(10) ?
    C21 C2 C3 . . 113.38(10) ?
    O31 C3 C4 . . 113.26(10) ?
    O31 C3 C2 . . 113.08(11) ?
    C4 C3 C2 . . 102.40(10) ?
    C3 C4 C41 . . 115.64(12) ?
    C3 C4 C5 . . 103.61(10) ?
    C41 C4 C5 . . 114.00(11) ?
    N1 C5 C51 . . 113.87(11) ?
    N1 C5 C4 . . 101.94(10) ?
    C51 C5 C4 . . 111.41(12) ?
    O11 C11 N1 . . 125.59(12) ?
    O11 C11 O12 . . 124.04(12) ?
    N1 C11 O12 . . 110.37(11) ?
    C11 O12 C13 . . 121.11(10) ?
    O12 C13 C14 . . 101.78(12) ?
    O12 C13 C16 . . 110.46(11) ?
    C14 C13 C16 . . 110.89(13) ?
    O12 C13 C15 . . 110.88(11) ?
    C14 C13 C15 . . 110.63(13) ?
    C16 C13 C15 . . 111.78(14) ?
    C22 C21 C2 . . 109.87(10) ?
    C23 C22 C27 . . 118.44(12) ?
    C23 C22 C21 . . 120.98(12) ?
    C27 C22 C21 . . 120.58(12) ?
    C24 C23 C22 . . 120.54(13) ?
    C25 C24 C23 . . 120.40(13) ?
    C26 C25 C24 . . 119.45(12) ?
    C27 C26 C25 . . 120.08(13) ?
    C26 C27 C22 . . 121.09(13) ?
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    C11 N1 C2 C21 . . . . 41.88(16) ?
    C5 N1 C2 C21 . . . . -140.53(11) ?
    C11 N1 C2 C3 . . . . 164.53(12) ?
    C5 N1 C2 C3 . . . . -17.88(13) ?
    N1 C2 C3 O31 . . . . -85.42(12) ?
    C21 C2 C3 O31 . . . . 38.49(15) ?
    N1 C2 C3 C4 . . . . 36.79(12) ?
    C21 C2 C3 C4 . . . . 160.70(10) ?
    O31 C3 C4 C41 . . . . -46.66(16) ?
    C2 C3 C4 C41 . . . . -168.76(11) ?
    O31 C3 C4 C5 . . . . 78.81(13) ?
    C2 C3 C4 C5 . . . . -43.28(12) ?
    C11 N1 C5 C51 . . . . 49.30(17) ?
    C2 N1 C5 C51 . . . . -128.28(12) ?
    C11 N1 C5 C4 . . . . 169.41(12) ?
    C2 N1 C5 C4 . . . . -8.18(13) ?
    C3 C4 C5 N1 . . . . 31.51(12) ?
    C41 C4 C5 N1 . . . . 158.03(11) ?
    C3 C4 C5 C51 . . . . 153.33(11) ?
    C41 C4 C5 C51 . . . . -80.16(15) ?
    C5 N1 C11 O11 . . . . -159.05(13) ?
    C2 N1 C11 O11 . . . . 18.3(2) ?
    C5 N1 C11 O12 . . . . 21.31(16) ?
    C2 N1 C11 O12 . . . . -161.37(11) ?
    O11 C11 O12 C13 . . . . 12.20(19) ?
    N1 C11 O12 C13 . . . . -168.15(11) ?
    C11 O12 C13 C14 . . . . 172.54(12) ?
    C11 O12 C13 C16 . . . . -69.64(16) ?
    C11 O12 C13 C15 . . . . 54.84(16) ?
    N1 C2 C21 C22 . . . . 178.58(10) ?
    C3 C2 C21 C22 . . . . 62.73(14) ?
    C2 C21 C22 C23 . . . . -103.27(14) ?
    C2 C21 C22 C27 . . . . 75.98(15) ?
    C27 C22 C23 C24 . . . . 0.10(19) ?
    C21 C22 C23 C24 . . . . 179.36(12) ?
    C22 C23 C24 C25 . . . . 0.1(2) ?
    C23 C24 C25 C26 . . . . -0.2(2) ?
    C24 C25 C26 C27 . . . . 0.1(2) ?
    C25 C26 C27 C22 . . . . 0.1(2) ?
    C23 C22 C27 C26 . . . . -0.22(19) ?
    C21 C22 C27 C26 . . . . -179.49(12) ?
data_global
_journal_data_validation_number     IUC9700028
_journal_date_recd_electronic     97-09-01
_journal_date_accepted     97-10-24
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     1997
_journal_volume     53
_journal_issue     12
_journal_paper_category     ZO
_journal_coeditor_code     QA0017
_publ_contact_author
;
      Dr. Michael Bolte
      Institut für Organische Chemie
      J. W. Goethe-Universität
      Marie-Curie-Str. 11
      60439 Frankfurt/Main
      Germany
;
_publ_contact_author_email     bolte@chemie.uni-frankfurt.de
_publ_contact_author_fax     '49 69 798 29128'
_publ_contact_author_phone     '49 69 798 29136'
_publ_section_title
;
(+)-(2S,3S,4S,5S)-2-Benzyl-N-(tert-butyloxycarbonyl)-3-hydroxy-
4,5-dimethylpyrrolidine at 143 K
;
loop_
    _publ_author_name
    _publ_author_address
    'Bolte, Michael'
;     Institut für Organische Chemie
      Universität Frankfurt
      Marie-Curie-Str. 11
      60439 Frankfurt/Main
      Germany
;
_publ_section_abstract
;
The structure determination of the title compound,
C₁₈H₂₇NO₃, was undertaken in order to
determine the relative and absolute configuration of the chiral centres.
The pyrrolidine ring exhibits a twist conformation, and
the N atom lies in a common plane with its neighbours.
The intermolecular packing is stabilized by a hydrogen bond.
;
_publ_section_comment
;
The X-ray structure determination was carried out in order to
determine the configuration of the chiral centres,
which all turned out to be S.  The S configuration at atom C2 was known in
advance, and served to establish the absolute configuration of the other chiral
centres. The pyrrolidine ring exhibits a twist conformation [q=0.421, φ =
94.4; (Cremer & Pople, 1975)], with an approximate C2-axis running through N1
and the centre of the C3-C4 bond.
The angles around the N atom show, that it lies in a common
plane with its neighbours.
The intermolecular packing is stabilized by a hydrogen bond
O11ⁱ..H31 2.119(3)Å, O11ⁱ..31-O31 153.9(6)°
[symmetry code: (i) 1+x,y,z].
The chemistry of the title compound is described by
Reggelin and Heinrich (1997).
;
_publ_section_acknowledgements
;
 I thank Dr. M. Reggelin and T. Heinrich, University of Frankfurt,
 for providing the sample.
;
_publ_section_references
;
Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 89, 1354-1358.
Reggelin, H. & Heinrich, T. (1997). Manuscript in preparation.
Sheldrick, G.M. (1991). SHELXTL-Plus. Release 4.1. Siemens
Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Sheldrick, G.M. (1990).  SHELXS-90. Program for the solution of crystal
structures.  Univ. of Göttingen, Federal Republic of Germany.
Sheldrick, G.M. (1996a).  SADABS. Program for empirical absorption
correction of area detector data.
Univ. of Göttingen, Federal Republic of Germany.
Sheldrick, G.M. (1996b).  SHELXL-96. Program for the refinement of crystal
structures.  Univ. of Göttingen, Federal Republic of Germany.
Siemens (1995). SMART and SAINT Area-Detector Control and Integration
Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
;
_publ_section_exptl_prep
;
Single crystals were obtained from an diethylether solution by
slow evaporation of the solvent.
;
_publ_section_exptl_refinement
;
All H atoms were located by difference Fourier synthesis and
refined with fixed individual displacement parameters [U(H) =
1.5Ueq(Cmethyl), U(H) = 1.2 Ueq(C) or U(H) = 1.2 Ueq(O)]
using a riding model with
C-H(methyl) = 0.98,
C-H(secondary) = 0.99,
C-H(tertiary) = 1.00,
C-H(aromatic) = 0.95 or
O-H = 0.84 Å,
respectively.
In additon, the torsion angle about the C-O bond
of the hydroxyl group was allowed to refine.
For a structure containing only C, H, N and O atoms and the
kind of radiation used, the absolute structure could not be determined from
anomalous dispersion effects.
;
