<i>N</i>-[Glycyl-(<i>Z</i>)-α,β-dehydrophenylalanylglycyl-(<i>Z</i>)-α,β-dehydrophenylalanyl]glycine trifluoroacetate methanol solvate
Makowski, Maciej; Lisowski, Marek; Mikołajczyk, Iwona; Lis, Tadeusz; Acta Crystallographica Section E 63 (2007) o2709–o2710; doi:10.1107/S1600536807016613

data_2213473
_publ_section_title
;<i>N</i>-[Glycyl-(<i>Z</i>)-\a,\b-dehydrophenylalanylglycyl-(<i>Z</i>)-\a,\b-dehydrophenylalanyl]glycine
 trifluoroacetate methanol solvate
;
_journal_coeditor_code           LW2007
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2709
_journal_page_last               o2710
_journal_paper_doi               10.1107/S1600536807016613
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C24 H26 N5 O6 + , C2 F3 O2 - , C H4 O'
_chemical_formula_moiety         'C24 H26 N5 O6 + , C2 F3 O2 - , C H4 O'
_chemical_formula_sum            'C27 H30 F3 N5 O9'
_chemical_formula_weight         625.56
_chemical_name_systematic
;
N-[Glycyl-(<i>Z</i>)-\a,\b-dehydrophenylalanylglycyl-
(<i>Z</i>)-\a,\b-dehydrophenylalanyl]glycine trifluoroacetate methanol
solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.267(7)
_cell_length_b                   16.660(8)
_cell_length_c                   13.459(7)
_cell_measurement_reflns_used    12781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     2953(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type
'Oxford Excalibur PX \k-geometry diffractometer plus CCD area detector'
_diffrn_measurement_method       '\w and \f'
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24725
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         76.4
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    1.02
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.46
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0995P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.144
_reflns_number_gt                4191
_reflns_number_total             5723
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lw2007.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213473
_cod_database_fobs_code          2213473