Crystallographic Characterization of 12-Helical Secondary Structure in β-Peptides Containing Side Chain Groups
Soo Hyuk Choi; Ilia A. Guzei; Lara C. Spencer; Samuel H. Gellman; Journal of the American Chemical Society 132 (2010) 13879–13885; doi:10.1021/ja1062532

data_4103172
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Crystallographic Characterization of 12-Helical Secondary Structure in
 \b-Peptides Containing Side Chain Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13879
_journal_page_last               13885
_journal_paper_doi               10.1021/ja1062532
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_sum            'C62 H94 Br N7 O12'
_chemical_formula_weight         1209.35
_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
;
manual editing of the CIF file 
created by SHELXTL Ver. 6.10
and processed with modiCIfer-03272007. 
;
_audit_update_record
;
2008-05-28 # Formatted by publCIF
;
_cell_angle_alpha                105.2770(10)
_cell_angle_beta                 97.8850(10)
_cell_angle_gamma                94.0840(10)
_cell_formula_units_Z            2
_cell_length_a                   9.45820(10)
_cell_length_b                   15.6589(3)
_cell_length_c                   23.4440(4)
_cell_measurement_reflns_used    9245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.81
_cell_measurement_theta_min      2.94
_cell_volume                     3296.80(9)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47947
_diffrn_reflns_theta_full        69.57
_diffrn_reflns_theta_max         69.57
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.8332
_exptl_absorpt_correction_T_min  0.6206
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1255
_refine_ls_number_reflns         18942
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1382P)^2^+4.0399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                18435
_reflns_number_total             18942
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1062532_si_006.cif
_cod_data_source_block           gellman100b
_cod_database_code               4103172