<i>N</i>-[<i>tert</i>-Butoxycarbonylglycyl-(<i>E</i>)-α,β-dehydrophenylalanylglycylglycyl-(<i>E</i>)-α,β-dehydrophenylalanyl]glycine
Makowski, Maciej; Lisowski, Marek; Iwona Mikołajczyk; Lis, Tadeusz; Acta Crystallographica Section E 63 (2007) o19–o21; doi:10.1107/S1600536806049841

data_2211879
_publ_section_title
<i>N</i>-[<i>tert</i>-Butoxycarbonylglycyl-(<i>E</i>)-\a,\b-dehydrophenylalanylglycylglycyl-(<i>E</i>)-\a,\b-dehydrophenylalanyl]glycine
_journal_coeditor_code           LH2225
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o19
_journal_page_last               o21
_journal_paper_doi               10.1107/S1600536806049841
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C31 H36 N6 O9'
_chemical_formula_moiety         'C31 H36 N6 O9'
_chemical_formula_sum            'C31 H36 N6 O9'
_chemical_formula_weight         636.66
_chemical_name_systematic
;
N-[tert-butoxycarbonyl-glycyl-(E)-\a,\b-dehydrophenylalanylglycylglycyl-
(E)-\a,\b-dehydrophenylalanyl]glycine
;
_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            4
_cell_length_a                   9.552(2)
_cell_length_b                   14.008(3)
_cell_length_c                   24.214(5)
_cell_measurement_reflns_used    20397
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3239.9(12)
_computing_cell_refinement       'CrysAlis CCD'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis CCD'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Xcalibur PX \k-geometry CCD detector'
_diffrn_measurement_method       '\w and \q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25776
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         76.73
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.30
_refine_ls_extinction_coef       0.0031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         3590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0573
_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^)+(0.088P)^2^+1.68P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                3139
_reflns_number_total             3590
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2225.cif
_cod_data_source_block           I
_cod_database_code               2211879
_cod_database_fobs_code          2211879