(<i>S</i>)-(<i>Z</i>)-Methyl 2-[2,3-bis(benzyloxycarbonyl)guanidino]-4-methylpentanoate
Fronczek, Chris F.; Kil, HyunJoo; McLaughlin, Mark L.; Fronczek, Frank R.; Acta Crystallographica Section E 67 (2011) o27–o28; doi:10.1107/S1600536810050130

data_2228836
_publ_section_title
;
 (<i>S</i>)-(<i>Z</i>)-Methyl
 2-[2,3-bis(benzyloxycarbonyl)guanidino]-4-methylpentanoate
;
_journal_coeditor_code           OM2385
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o27
_journal_page_last               o28
_journal_paper_doi               10.1107/S1600536810050130
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C24 H29 N3 O6'
_chemical_formula_sum            'C24 H29 N3 O6'
_chemical_formula_weight         455.50
_chemical_name_systematic
;
(<i>S</i>)-(<i>Z</i>)-Methyl
2-[2,3-bis(benzyloxycarbonyl)guanidino]-4-methylpentanoate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7203(5)
_cell_length_b                   14.2043(10)
_cell_length_c                   21.280(2)
_cell_measurement_reflns_used    5760
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      36.1
_cell_measurement_theta_min      2.5
_cell_volume                     2333.6(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare  <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device
'Nonius KappaCCD (with an Oxford Cryosystems Cryostream cooler)'
_diffrn_measurement_method       ' \w and \f'
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            43001
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.1
_diffrn_reflns_theta_min         2.8
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.276
_refine_ls_abs_structure_details 'Flack (1983), 4545 Friedel pairs'
_refine_ls_abs_structure_Flack   0.2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         10411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0473P)^2^+0.6349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                9219
_reflns_number_total             10411
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2385.cif
_cod_data_source_block           I
_cod_database_code               2228836
_cod_database_fobs_code          2228836