Azepane Quaternary Amino Acids As Effective Inducers of 310Helix Conformations
Diego Núñez-Villanueva; Lourdes Infantes; M. Teresa García-López; Rosario González-Muñiz; Mercedes Martín-Martínez; Journal of Organic Chemistry 77 (2012) 9833–9839; doi:10.1021/jo301379r

data_4027629
_publ_contact_author_address
;Department of Crystallography
Instituto de Quimica-Fisica Rocasolano
Serrano 119
28006-Madrid, Spain
;
_publ_contact_author_email       xlourdes@iqfr.csic.es
_publ_contact_author_fax         00(34)915619400
_publ_contact_author_name        'Infantes, L.'
_publ_contact_author_phone       00(34)915642431
_publ_section_title
;
 Azepane Quaternary Amino Acids As Effective Inducers of 310Helix
 Conformations
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9833
_journal_page_last               9839
_journal_paper_doi               10.1021/jo301379r
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C23 H39 N5 O6 , C4 H8 O2'
_chemical_formula_sum            'C27 H47 N5 O8'
_chemical_formula_weight         569.7
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-05-09
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6864(5)
_cell_length_b                   17.6725(12)
_cell_length_c                   20.2622(13)
_cell_measurement_reflns_used    2329
_cell_measurement_temperature    120(2)
_cell_volume                     3110.5(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD2000
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0068092
_diffrn_orient_matrix_UB_12      -0.0564106
_diffrn_orient_matrix_UB_13      -0.0025456
_diffrn_orient_matrix_UB_21      -0.0756638
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      -0.0371962
_diffrn_orient_matrix_UB_31      0.0864975
_diffrn_orient_matrix_UB_32      0.0044407
_diffrn_orient_matrix_UB_33      -0.032337
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4179
_diffrn_reflns_theta_full        57.89
_diffrn_reflns_theta_max         57.89
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.74
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.07
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         4179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.8162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                4024
_reflns_number_total             4179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301379r_si_002.cif
_cod_data_source_block           dn267
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_database_code               4027629