Crystal structure of <i>N</i>-(<i>tert</i>-butoxycarbonyl)glycyl-(<i>Z</i>)-β-bromodehydroalanine methyl ester [Boc–Gly–(β-Br)^(<i>Z^)</i>ΔAla–OMe]
Lenartowicz, Paweł; Makowski, Maciej; Zarychta, Bartosz; Ejsmont, Krzysztof; Acta Crystallographica Section E 70 (2014) 596–598; doi:10.1107/S1600536814025677

data_2240265
_publ_section_title
;
 Crystal structure of
 <i>N</i>-(<i>tert</i>-butoxycarbonyl)glycyl-(<i>Z</i>)-\b-bromodehydroalanine
 methyl ester [Boc--Gly--(\b-Br)^(<i>Z^)</i>\DAla--OMe]
;
_journal_coeditor_code           HB7312
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              596
_journal_page_last               598
_journal_paper_doi               10.1107/S1600536814025677
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C11 H17 Br N2 O5'
_chemical_formula_moiety         'C11 H17 Br N2 O5'
_chemical_formula_sum            'C11 H17 Br N2 O5'
_chemical_formula_weight         337.17
_chemical_name_common
'N-(tert-butoxycarbonyl)glycyl-(Z)-\b-bromo-dehydroalanine methyl ester'
_chemical_name_systematic
;
<i>N</i>-(<i>tert</i>-Butoxycarbonyl)glycyl-(<i>Z</i>)-\b-bromodehydroalanine
methyl ester
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                83.381(3)
_cell_angle_beta                 75.420(4)
_cell_angle_gamma                64.863(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0431(4)
_cell_length_b                   9.3160(4)
_cell_length_c                   9.7540(4)
_cell_measurement_reflns_used    4860
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.2
_cell_volume                     719.92(6)
_computing_cell_refinement
;
CrysAlisRED (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlisCCD (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlisRED (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 1024
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w scan'
_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  0.0158
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         3.224
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                2490
_reflns_number_total             2780
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7312sup1.cf
_cod_data_source_block           I
_cod_database_code               2240265
_cod_database_fobs_code          2240265
_shelx_hkl_checksum              78956
_shelx_res_checksum              77381
_shelxl_version_number           .2013