(3<i>S</i>,4<i>S</i>)-1-Benzyl-4-(<i>N</i>-octylcarbamoyloxy)pyrrolidin-3-yl <i>N</i>-octylcarbamate: a low-temperature redetermination
Cicchi, Stefano; Faggi, Cristina; Ghini, Giacomo; Guerri, Annalisa; Parlanti, Iacopo; Acta Crystallographica Section E 63 (2007) o3082–o3082; doi:10.1107/S160053680702572X

data_2214042
_publ_section_title
;
 (3<i>S</i>,4<i>S</i>)-1-Benzyl-4-(<i>N</i>-octylcarbamoyloxy)pyrrolidin-3-yl
 <i>N</i>-octylcarbamate: a low-temperature redetermination
;
_journal_coeditor_code           BG2057
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3082
_journal_page_last               o3082
_journal_paper_doi               10.1107/S160053680702572X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C29 H49 N3 O4'
_chemical_formula_moiety         'C29 H49 N3 O4'
_chemical_formula_sum            'C29 H49 N3 O4'
_chemical_formula_weight         503.71
_chemical_melting_point          94
_chemical_name_systematic
;
(3S,4S)-1-Benzyl-4-(N-octylcarbamoyloxy)pyrrolidin-3-yl N-octylcarbamate
;
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'from SHELXL97 CIF and IUCr SHELXL97 template'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.0390(10)
_cell_length_b                   15.8250(10)
_cell_length_c                   18.3300(10)
_cell_measurement_reflns_used    10467
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.2
_cell_measurement_theta_min      3.7
_cell_volume                     1461.5(3)
_computing_cell_refinement       'Crysalis CCD'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR PX Ultra CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Oxford Diffraction Enhance ULTRA assembly'
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23018
_diffrn_reflns_theta_full        74.22
_diffrn_reflns_theta_max         74.22
_diffrn_reflns_theta_min         3.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.215
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.02(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0542P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                4359
_reflns_number_total             5438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2057.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2214042
_cod_database_fobs_code          2214042