Effect on the Conformation of a Terminally Blocked, (<i>E</i>) β,γ-Unsaturated δ-Amino Acid Residue Induced by Carbon Methylation.
Marafon, Giulia; Moretto, Alessandro; Zanuy, David; Alemán, Carlos; Crisma, Marco; Toniolo, Claudio; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02544

data_4037634
_publ_section_title
;
 Effect on the Conformation of a Terminally Blocked, (<i>E</i>)
 \b,\g-Unsaturated \d-Amino Acid Residue Induced by Carbon Methylation.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02544
_journal_year                    2019
_chemical_formula_sum            'C17 H32 N2 O3'
_chemical_formula_weight         312.44
_chemical_name_common
;
 Boc-5-amino-2,2,5,5-tetramethyl-pent-3-(E)-enoyl-NHiPr
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                88.95(5)
_cell_angle_beta                 87.04(8)
_cell_angle_gamma                80.67(7)
_cell_formula_units_Z            2
_cell_length_a                   5.990(2)
_cell_length_b                   8.937(2)
_cell_length_c                   17.928(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     945.7(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2002 (Burla et al. 2002)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\q-2\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        60.001
_diffrn_reflns_theta_max         60.001
_diffrn_reflns_theta_min         4.940
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+0.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2526
_reflns_number_total             2793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02544_si_003.cif
_cod_data_source_block           mc92p2
_cod_database_code               4037634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.943