Crystal structure of <i>N</i>-{<i>N</i>-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)-<small>L</small>-α-aspartyl]-<small>L</small>-α-aspartyl}-<small>L</small>-α-aspartic acid 1^4^,2^4^,3^4^-trimethyl ester 3^1^-2-oxo-2-phenylethyl ester {Boc-[Asp(OMe)]~3~-OPac}
Kato, Takuma; Kishimoto, Saki; Asano, Akiko; Doi, Mitsunobu; Acta Crystallographica Section E 75 (2019) 585–588; doi:10.1107/S2056989019004596

data_2242897
_publ_section_title
;
 Crystal structure of
 <i>N</i>-{<i>N</i>-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)-<small>L</small>-\a-aspartyl]-<small>L</small>-\a-aspartyl}-<small>L</small>-\a-aspartic
 acid 1^4^,2^4^,3^4^-trimethyl ester 3^1^-2-oxo-2-phenylethyl ester
 {Boc-[Asp(OMe)]~3~-OPac}
;
_journal_coeditor_code           IS5511
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              585
_journal_page_last               588
_journal_paper_doi               10.1107/S2056989019004596
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C28 H37 N3 O13'
_chemical_formula_moiety         'C28 H37 N3 O13'
_chemical_formula_sum            'C28 H37 N3 O13'
_chemical_formula_weight         623.60
_chemical_name_systematic
;<i>N</i>-{<i>N</i>-[<i>N</i>-(<i>tert</i>-butoxycarbonyl)-<i>L</i>-\a-aspartyl]-<i>L</i>-\a-aspartyl}-<i>L</i>-\a-aspartic acid
1^4^,2^4^,3^4^-trimethyl ester 3^1^-2-oxo-2-phenylethyl ester
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 114.2255(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7734(2)
_cell_length_b                   4.97864(4)
_cell_length_c                   18.7681(2)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.9490
_cell_measurement_theta_min      4.7570
_cell_volume                     1514.49(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7024
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.352
_diffrn_reflns_theta_min         2.582
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.182
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 629 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.06(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.766
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.768
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0741P)^2^+0.2745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                3832
_reflns_number_total             3952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5511sup1.cif
_cod_data_source_block           I
_cod_database_code               2242897
_cod_database_fobs_code          2242897
_shelx_hkl_checksum              84265
_shelx_res_checksum              16398