Crystal structure of <i>N</i>-(<i>tert</i>-butoxycarbonyl)phenylalanyldehydroalanine isopropyl ester (Boc–Phe–ΔAla–OiPr)
Lenartowicz, Paweł; Makowski, Maciej; Zarychta, Bartosz; Ejsmont, Krzysztof; Acta Crystallographica Section E 70 (2014) 599–602; doi:10.1107/S1600536814025197

data_2240260
_publ_section_title
;
 Crystal structure of
 <i>N</i>-(<i>tert</i>-butoxycarbonyl)phenylalanyldehydroalanine isopropyl
 ester (Boc--Phe--\DAla--OiPr)
;
_journal_coeditor_code           ZS2321
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              599
_journal_page_last               602
_journal_paper_doi               10.1107/S1600536814025197
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C20 H28 N2 O5'
_chemical_formula_moiety         'C20 H28 N2 O5'
_chemical_formula_sum            'C20 H28 N2 O5'
_chemical_formula_weight         376.44
_chemical_melting_point_gt       367
_chemical_melting_point_lt       369
_chemical_name_common
'<i>N</i>-(tert-butoxycarbonyl)phenylalanyldehydroalanine isopropyl ester'
_chemical_name_systematic
;
<i>N</i>-(<i>tert</i>-Butoxycarbonyl)phenylalanyldehydroalanine
isopropyl ester
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2123(2)
_cell_length_b                   9.5031(3)
_cell_length_c                   41.3363(17)
_cell_measurement_reflns_used    4025
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.996
_cell_measurement_theta_min      3.266
_cell_volume                     2047.51(13)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXL2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0460
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            14003
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         3.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.217
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1095 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                3235
_reflns_number_total             4025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2321sup1.cif
_cod_data_source_block           I
_cod_database_code               2240260
_cod_database_fobs_code          2240260
_shelx_hkl_checksum              60118
_shelx_res_checksum              10865
_shelxl_version_number           .2013