4-<i>tert</i>-Butyloxycarbonyl-6(<i>S</i>)-(hydroxymethyl)-3(<i>S</i>)-(1-methylethyl)piperazin-2-one
Kolter, T.; Rübsam, F.; Giannis, A.; Nieger, M.; Acta Crystallographica Section C 52 (1996) 978–980; doi:10.1107/S0108270195013278

data_2004755
_publ_contact_author
;
        Dr. Athanassios Giannis
        Institut f\"ur Organische Chemie und Biochemie der Universit\"at
        Gerhard-Domagk-Str. 1
        53121 Bonn
        Germany
;
_publ_section_title
4-<i>tert</i>-Butyloxycarbonyl-6(<i>S</i>)-(hydroxymethyl)-3(<i>S</i>)-(1-methylethyl)piperazin-2-one
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              978
_journal_page_last               980
_journal_paper_doi               10.1107/S0108270195013278
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C13 H24 N2 O4'
_chemical_formula_sum            'C13 H24 N2 O4'
_chemical_formula_weight         272.34
_chemical_name_systematic
;
 4-tert-Butyloxycarbonyl-6(S)-hydroxymethyl-3(S)-methylethyl-
 piperazin-2-one
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8900(10)
_cell_length_b                   11.7520(10)
_cell_length_c                   17.0280(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46
_cell_measurement_theta_min      40
_cell_volume                     1578.9(3)
_computing_cell_refinement       CAD4-Express
_computing_data_collection       'CAD4-Express (Enraf-Nonius, 1989)'
_computing_data_reduction        'locally modified XCAD4 (Sheldrick, 1992)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1989)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1989)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       2\q/2\w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2328
_diffrn_reflns_theta_max         59.96
_diffrn_reflns_theta_min         4.57
_diffrn_standards_decay_%        '+-1 variation not decay'
_diffrn_standards_interval_count '200 (orientation)'
_diffrn_standards_interval_time  '120 min (intensity)'
_diffrn_standards_number         '2 (orientation), 3 (intensity)'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack
' -0.03(70), absolute structure cannot be determined reliably'
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_method     'SHELXL (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    'riding, H (on O and N) free'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_obs          0.0674
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^) + (0.128P)^2^ + 0.6321P] where
 P=(F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.2097
_refine_ls_wR_factor_obs         0.1845
_reflns_number_observed          1545
_reflns_number_total             2019
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1074.cif
_cod_data_source_block           sh02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 212121'
_cod_database_code               2004755