Side-Chain Chiral Centers of Amino Acid and Helical-Screw Handedness of Its Peptides
Masakazu Tanaka; Kosuke Anan; Yosuke Demizu; Masaaki Kurihara; Mitsunobu Doi; Hiroshi Suemune; Journal of the American Chemical Society 127 (2005) 11570–11571; doi:10.1021/ja053842c

data_4111876
_publ_section_title
;
 Side-Chain Chiral Centers of Amino Acid and Helical-Screw Handedness of
 Its Peptides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11570
_journal_page_last               11571
_journal_paper_doi               10.1021/ja053842c
_journal_volume                  127
_journal_year                    2005
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C67 H92 N6 O9, 0.5(C2 H6 O)'
_chemical_formula_sum            'C68 H95 N6 O9.5'
_chemical_formula_weight         1148.50
_chemical_melting_point          513
_chemical_name_common            Boc-[(R,R)-Ab5,6=c]6-OEt
_chemical_name_systematic
; 
 Ethyl 8-{{8-{{8-{{8-{{8-{[(1R,6R)-8-(tert-Butoxycarbonylamino)
bicyclo[4.3.0]non-3-en-8-yl]carbonylamino}-(1R,6R)-bicyclo[4.3.0]non-
3-en-8-yl}carbonylamino}-(1R,6R)-bicyclo[4.3.0]non-3-en-8-yl}-
carbonylamino}-(1R,6R)-bicyclo[4.3.0]non-3-en-8-yl}carbonylamino}-
(1R,6R)-bicyclo[4.3.0]non-3-en-8-yl}carbonylamino}-
(1R,6R)-bicyclo[4.3.0]non-3-en-8-carboxylate 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.22(3)
_cell_angle_beta                 82.32(3)
_cell_angle_gamma                75.39(3)
_cell_formula_units_Z            4
_cell_length_a                   15.765(12)
_cell_length_b                   16.535(10)
_cell_length_c                   26.90(2)
_cell_measurement_reflns_used    43732
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     6514(8)
_computing_cell_refinement       'RIGAKU/MSC CrystalClear'
_computing_data_collection       'RIGAKU/MSC CrystalClear'
_computing_data_reduction        'RIGAKU PROCESS-AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.1
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'RIGAKU RAPID'
_diffrn_measurement_method       \f-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62528
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.513
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.3(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3045
_refine_ls_number_reflns         29059
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1552
_reflns_number_gt                14531
_reflns_number_total             29059
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja053842csi20050611_042212.cif
_cod_data_source_block           cdi5
_cod_original_formula_sum        'C68 H95 N6 O9.50'
_cod_database_code               4111876