Facile and E-Selective Intramolecular Ring-Closing Metathesis Reactions in 310-Helical Peptides: A 3D Structural Study
Amie K. Boal; Ivan Guryanov; Alessandro Moretto; Marco Crisma; Erica L. Lanni; Claudio Toniolo; Robert H. Grubbs; Daniel J. O'Leary; Journal of the American Chemical Society 129 (2007) 6986–6987; doi:10.1021/ja071148m

data_4109484
_publ_section_title
;
 Facile and E-Selective Intramolecular Ring-Closing Metathesis Reactions
 in 310-Helical Peptides: A 3D Structural Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6986
_journal_page_last               6987
_journal_paper_doi               10.1021/ja071148m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C40 H72 N8 O14'
_chemical_formula_weight         889.06
_chemical_name_systematic
;
 Boc-(Aib)3-L-Ser-(Aib)2-L-Ser-Aib-OMe
 [O4G-(CH2)4-O7G bridged]  monohydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.47(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.518(4)
_cell_length_b                   8.961(2)
_cell_length_c                   18.351(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     4995(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 2002 (Burla et al, 2003)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\q-2\q 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4636
_diffrn_reflns_theta_full        60.04
_diffrn_reflns_theta_max         60.04
_diffrn_reflns_theta_min         4.31
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.743
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     559
_refine_ls_number_reflns         4510
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+0.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                4187
_reflns_number_total             4510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071148msi20070216_112644.cif
_cod_data_source_block           mc106
_cod_original_cell_volume        4995.1(15)
_cod_database_code               4109484