Stereochemistry of Protected Ornithine Side Chains of Gramicidin S Derivatives: X-ray Crystal Structure of the Bis-Boc-tetra-N-methyl Derivative of Gramicidin S
Keiichi Yamada; Masafumi Unno; Kyoko Kobayashi; Hiroyuki Oku; Hatsuo Yamamura; Shuki Araki; Hideyuki Matsumoto; Ryoichi Katakai; Masao Kawai; Journal of the American Chemical Society 124 (2002) 12684–12688; doi:10.1021/ja020307t

data_4115225
_publ_contact_author_address
;
Department of Applied Chemistry
Nagoya Institute of Technology
Gokiso-cho
Nagoya 466-8555
Japan
;
_publ_contact_author_email       ' kawai@ach.nitech.ac.jp '
_publ_contact_author_fax         ' 81(52)7355215 '
_publ_contact_author_name        ' Masao Kawai'
_publ_contact_author_phone       ' 81(52)7355215 '
_publ_section_title
;
 Stereochemistry of Protected Ornithine Side Chains of Gramicidin S
 Derivatives: X-ray Crystal Structure of the Bis-Boc-tetra-N-methyl
 Derivative of Gramicidin S
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12684
_journal_page_last               12688
_journal_paper_doi               10.1021/ja020307t
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C76 H130 N12 O19 S'
_chemical_formula_weight         1547.99
_chemical_melting_point          434(1)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Tue Mar 12 20:33:41 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.201(1)
_cell_length_b                   19.401(2)
_cell_length_c                   40.438(6)
_cell_measurement_reflns_used    34062
_cell_measurement_temperature    253.2
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      1.0
_cell_volume                     8787.6(18)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7092
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            30373
_diffrn_reflns_theta_max         32.32
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   International_Tables
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_crystal_size_rad          0.300
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0095
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.464
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     947
_refine_ls_number_reflns         16096
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          -0.0550
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                16096
_reflns_number_total             23650
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja020307t.cif
_cod_data_source_block           GS
_cod_original_cell_volume        8787(1)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C76 H130 N12 O19 S '
_cod_database_code               4115225