1H-Azepine-2-oxo-5-amino-5-carboxylic Acid: A 310 Helix Inducer and an Effective Tool for Functionalized Gold Nanoparticles.
Pellegrino, Sara; Bonetti, Andrea; Clerici, Francesca; Contini, Alessandro; Moretto, Alessandro; Soave, Raffaella; Gelmi, Maria Luisa; The Journal of organic chemistry 80 (2015) 5507–5516; doi:10.1021/acs.joc.5b00396

data_4030971
_publ_section_title
;
 1H-Azepine-2-oxo-5-amino-5-carboxylic Acid: A 310 Helix Inducer and an
 Effective Tool for Functionalized Gold Nanoparticles.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5507
_journal_page_last               5516
_journal_paper_doi               10.1021/acs.joc.5b00396
_journal_volume                  80
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C24 H27 N2 O4, B F4'
_chemical_formula_sum            'C24 H27 B F4 N2 O4'
_chemical_formula_weight         494.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 103.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.659(2)
_cell_length_b                   8.0066(16)
_cell_length_c                   14.918(3)
_cell_measurement_reflns_used    5966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.49
_cell_measurement_theta_min      5.32
_cell_volume                     1239.9(4)
_computing_cell_refinement       'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)'
_computing_data_collection       'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)'
_computing_data_reduction        'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)'
_computing_molecular_graphics    'Diamond v3.2i (Brandenburg, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS APEX CCD area-detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21631
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 1185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_coef       0.023(11)
_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   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1809P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2712
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3268
_reflns_number_total             5698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b00396_si_001.cif
_cod_data_source_block           ca72new
_cod_depositor_comments          'Adding full bibliography for 4030971.cif.'
_cod_original_cell_volume        1240.0(5)
_cod_database_code               4030971
_shelx_estimated_absorpt_t_min   0.8068
_shelx_estimated_absorpt_t_max   0.8623
_shelxl_version_number           2014/6
_shelx_res_checksum              15210
_shelx_hkl_checksum              61361