Two pentadehydropeptides with different configurations of the ΔPhe residues
Makowski, Maciej; Lisowski, Marek; Maciag, Anna; Wiktor, Maciej; Szlachcic, Anna; Lis, Tadeusz; Acta Crystallographica Section C 66 (2010) o119–o123; doi:10.1107/S0108270110003094

data_2017574
_publ_section_title
;
 Two pentadehydropeptides with different configurations of the \DPhe
 residues
;
_journal_coeditor_code           SK3358
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o119
_journal_page_last               o123
_journal_paper_doi               10.1107/S0108270110003094
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C29 H33 N5 O8 , C H4 O'
_chemical_formula_moiety         'C29 H33 N5 O8 , C H4 O'
_chemical_formula_sum            'C30 H37 N5 O9'
_chemical_formula_weight         611.65
_chemical_name_common
;
Boc^0^--Gly^1^--\D^Z^Phe^2^--Gly^3^--\D^Z^Phe^4^--Gly^5^--OH
;
_chemical_name_systematic
;
(<i>Z</i>,<i>Z</i>)-<i>N</i>-(<i>tert</i>-
butoxycarbonyl)glycylphenylalanylglycylphenylalanylglycine 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'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.075(4)
_cell_length_b                   16.577(5)
_cell_length_c                   14.041(4)
_cell_measurement_reflns_used    11531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      4
_cell_volume                     3030.2(17)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type
'Oxford Xcalibur PX \k-geometry diffractometer with 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     1.54180
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22848
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.46
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2003);
analytical numeric absorption correction using a multifaceted
crystal model based on the expressions derived by Clark & Reid
(1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                3735
_reflns_number_total             5247
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3358.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2017574
_cod_database_fobs_code          2017574