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_7155083
_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 unk
_chemical_formula_sum            'C11 H16 N2 O6 S'
_chemical_formula_weight         304.32
_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'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-05-21 deposited with the CCDC.
2016-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.53(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.813(9)
_cell_length_b                   9.696(14)
_cell_length_c                   11.51(2)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.9853
_cell_measurement_theta_min      1.6845
_cell_volume                     643.1(18)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13989
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.125
_diffrn_reflns_theta_max         27.203
_diffrn_reflns_theta_min         2.757
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
; 
 Flack x determined using 977 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.025(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   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0764P)^2^+0.9782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                2430
_reflns_number_total             2826
_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_original_cell_volume        642.9(17)
_cod_database_code               7155083
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-4
_shelx_res_checksum              1918