(2<i>S</i>,4<i>R</i>)-1-Benzyl 2-<i>tert</i>-butyl 4-[<i>N</i>,<i>N</i>'-bis(<i>tert</i>-butyloxycarbonyl)hydrazino]-5-oxopyrrolidine-1,2-dicarboxylate
Krzysztof Kaczmarek; Wojciech M. Wolf; Janusz Zabrocki; Acta Crystallographica Section E 61 (2005) o629–o631; doi:10.1107/S1600536805003880

data_2205209
_publ_section_title
;(2<i>S</i>,4<i>R</i>)-1-Benzyl 2-<i>tert</i>-butyl
 4-[<i>N</i>,<i>N</i>'-bis(<i>tert</i>-butyloxycarbonyl)hydrazino]-5-oxopyrrolidine-1,2-dicarboxylate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o629
_journal_page_last               o631
_journal_paper_doi               10.1107/S1600536805003880
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C27 H39 N3 O9'
_chemical_formula_moiety         'C27 H39 N3 O9'
_chemical_formula_sum            'C27 H39 N3 O9'
_chemical_formula_weight         549.61
_chemical_melting_point          372
_chemical_name_systematic
;(3R,5S)-1-Benzyl
 2-tert-butyl
4-[N,N'-bis(tert-butyloxycarbonyl)hydrazino]-5-oxopyrrolidine-1,5-dicarboxylate
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.883(2)
_cell_length_b                   10.103(2)
_cell_length_c                   15.892(2)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     1520.7(5)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection       'KM-4 Software (Kuma, 1991)'
_computing_data_reduction        'DATAPROC (Kuma, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Kuma KM-4'
_diffrn_measurement_method       \w--2\q
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3512
_diffrn_reflns_theta_full        69.96
_diffrn_reflns_theta_max         69.96
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XPREP; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      1.17
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.266
_refine_ls_extinction_coef       0.0125(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         2805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0812P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                1442
_reflns_number_total             2805
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6586.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2205209