Improved δ-valerolactam templates for the assembly of Aβ-miniamyloids by boronic ester formation.
Wuttke, André; Fischer, Sebastian Nils; Nebel, Annika; Marsch, Michael; Geyer, Armin; Organic & biomolecular chemistry 14 (2016) 5032–5048; doi:10.1039/c6ob00565a

data_7155085
_publ_section_title
;
 Improved \d-valerolactam templates for the assembly of A\b-miniamyloids
 by boronic ester formation.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5032
_journal_page_last               5048
_journal_paper_doi               10.1039/c6ob00565a
_journal_volume                  14
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_sum            'C17 H19 B N2 O7 S'
_chemical_formula_weight         406.21
_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_creation_method           SHELXL-97
_audit_update_record
;
2014-05-22 deposited with the CCDC.
2016-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4782(3)
_cell_length_b                   9.8389(4)
_cell_length_c                   28.4710(12)
_cell_measurement_reflns_used    133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.5532
_cell_measurement_theta_min      3.8189
_cell_volume                     1814.69(14)
_computing_cell_refinement       'APEX2 v2013.4-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.28'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            17673
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.8243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                3578
_reflns_number_total             4032
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ob00565a2.cif
_cod_data_source_block           an23_0m
_cod_depositor_comments
'Adding full bibliography for 7155081--7155085.cif.'
_cod_database_code               7155085