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_7155084
_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_moiety         'C9 H12 N4 O5 S'
_chemical_formula_sum            'C9 H12 N4 O5 S'
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_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-05-22 deposited with the CCDC.
2016-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2462(4)
_cell_length_b                   9.5487(7)
_cell_length_c                   20.1585(15)
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.36
_cell_volume                     1202.32(15)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'BRUKER APEX II'
_diffrn_ambient_temperature      100(2)
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_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8429
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         27.042
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5959
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.593
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_exptl_crystal_density_method    calculated
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_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.203
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_refine_diff_density_max         0.338
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
; 
 Flack x determined using 901 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0429P)^2^+0.2382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2328
_reflns_number_total             2613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob00565a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7155081--7155085.cif.'
_cod_database_code               7155084
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2013-4
_shelx_res_checksum              42185