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_4037635
_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            'C13 H23 N5 O2'
_chemical_formula_weight         281.36
_chemical_name_common
;
 Azidocarbonyl-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     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                107.580(3)
_cell_angle_beta                 91.726(3)
_cell_angle_gamma                106.465(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1653(3)
_cell_length_b                   9.4255(3)
_cell_length_c                   10.5148(3)
_cell_measurement_reflns_used    6995
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.795
_cell_measurement_theta_min      4.450
_cell_volume                     823.74(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2014 (Burla et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.814
_diffrn_reflns_theta_min         4.447
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+0.1255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2981
_reflns_number_total             3269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b02544_si_004.cif
_cod_data_source_block           mc310
_cod_original_cell_volume        823.73(5)
_cod_database_code               4037635
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.882