<i>tert</i>-Butyl (3<i>S</i>,6<i>R</i>,9<i>R</i>)-(5-oxo-3-{[1(<i>R</i>)-phenylethyl]carbamoyl}-1,2,3,5,6,7,8,8a-octahydroindolizin-6-yl)carbamate monohydrate at 95K
Soave, Raffaella; Destro, Riccardo; Acta Crystallographica Section C 58 (2002) o507–o509; doi:10.1107/S0108270102011538

data_2012887
_publ_section_title
;<i>tert</i>-Butyl
 (3<i>S</i>,6<i>R</i>,9<i>R</i>)-(5-oxo-3-{[1(<i>R</i>)-phenylethyl]carbamoyl}-1,2,3,5,6,7,8,8a-octahydroindolizin-6-yl)carbamate
 monohydrate at 95K
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o507
_journal_page_last               o509
_journal_paper_doi               10.1107/S0108270102011538
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C22 H31 N3 O4, H2 O'
_chemical_formula_moiety         'C22 H31 N3 O4, H2 O'
_chemical_formula_sum            'C22 H33 N3 O5'
_chemical_formula_weight         419.51
_chemical_name_systematic
;
tert-Butyl (3S,6R,9R)-(5-oxo-3-{N-[1(R)-phenylethyl]carbamoyl}-
1,2,3,5,6,7,8,8a-octahydroindolizin-6-yl)carbamate monohydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.520(2)
_cell_length_b                   12.095(2)
_cell_length_c                   22.323(5)
_cell_measurement_reflns_used    4199
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      20.551
_cell_measurement_theta_min      2.350
_cell_volume                     2300.4(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23342
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         .335
_refine_diff_density_min         -.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         2992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0371P)^2^+1.2606P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                2933
_reflns_number_total             2992
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1142.cif
_cod_data_source_block           I
_cod_database_code               2012887
_cod_database_fobs_code          2012887