(2<i>S</i>,3<i>R</i>,5<i>S</i>)-2-Benzyl-<i>N</i>-(<i>tert</i>-butoxycarbonyl)-3-hydroxy-5-methylpyrrolidine at 158K
Bats, Jan W.; Heinrich, Timo; Reggelin, Michael; Acta Crystallographica Section C 54 (1998) IUC9800039–; doi:10.1107/S0108270198099429

data_2007557
_publ_section_title
;(2<i>S</i>,3<i>R</i>,5<i>S</i>)-2-Benzyl-<i>N</i>-(<i>tert</i>-butoxycarbonyl)-3-hydroxy-5-methylpyrrolidine
 at 158K
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800039
_journal_paper_doi               10.1107/S0108270198099429
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C17 H25 N O3'
_chemical_formula_sum            'C17 H25 N O3'
_chemical_formula_weight         291.39
_chemical_name_systematic
;
 (2S,3R,5S)-2-benzyl-N-(tert-butoxycarbonyl)-3-hydroxy-5-methyl-
 pyrrolidine
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.59(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.4346(12)
_cell_length_b                   9.837(2)
_cell_length_c                   13.116(2)
_cell_measurement_reflns_used    117
_cell_measurement_temperature    158
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     830.2(3)
_computing_cell_refinement       SMART_(Siemens,_1995)
_computing_data_collection       SMART_(Siemens,_1995)
_computing_data_reduction        SAINT_(Siemens,_1995)
_computing_molecular_graphics    XP_in_SHELXTL_(Sheldrick,_1996)
_computing_publication_material  CIF_in_SHELXL_(Sheldrick,_1996)
_computing_structure_refinement  SHELXL-97_(Sheldrick,_1997)
_computing_structure_solution
Direct_methods_(SHELXS_in_SHELXTL,_Sheldrick,_1996)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device       SIEMENS_SMART
_diffrn_measurement_method       \w
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12906
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  540
_diffrn_standards_number         166
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.174
_refine_ls_abs_structure_details
;
 The absolute configuration of the compound is given by the known
 2S-configuration
;
_refine_ls_abs_structure_Flack   -1.0(10)
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.470
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.470
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                2958
_reflns_number_total             3962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qb0045.cif
_cod_data_source_block           hei395
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2007557
_cod_database_fobs_code          2007557