<i>N</i>-(<i>tert</i>-Butoxycarbonyl)-<small>L</small>-valyl-<small>L</small>-valine methyl ester: a twisted parallel β-sheet in the crystal structure of a protected dipeptide
Jacobsen, Øyvind; Gebreslasie, Hadgu Girmay; Klaveness, Jo; Rongved, Pål; Görbitz, Carl Henrik; Acta Crystallographica Section C 67 (2011) o278–o282; doi:10.1107/S0108270111022293

data_2018190
_publ_section_title
;
 <i>N</i>-(<i>tert</i>-Butoxycarbonyl)-<small>L</small>-valyl-<small>L</small>-valine
 methyl ester: a twisted parallel \b-sheet in the crystal structure of
 a protected dipeptide
;
_journal_coeditor_code           JZ3205
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o278
_journal_page_last               o282
_journal_paper_doi               10.1107/S0108270111022293
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H30 N2 O5'
_chemical_formula_sum            'C16 H30 N2 O5'
_chemical_formula_weight         330.42
_chemical_name_common            Boc-L-Val-L-Val-OMe
_chemical_name_systematic
;
<i>N</i>-(<i>tert</i>-Butoxycarbonyl)-L-valyl-L-valine methyl ester
;
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   11.6937(12)
_cell_length_b                   18.6458(19)
_cell_length_c                   27.047(3)
_cell_measurement_reflns_used    7630
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.86
_cell_volume                     5897.3(11)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method
'Sets of exposures each taken over 0.5\% \w rotation'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38750
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         5757
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0439P)^2^+1.1632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                4918
_reflns_number_total             5757
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jz3205.cif
_cod_data_source_block           I
_cod_original_cell_volume        5897.3(10)
_cod_database_code               2018190
_cod_database_fobs_code          2018190