Halogen bonding at the wet interfaces of an amyloid peptide structure
Pizzi, Andrea; Demitri, Nicola; Terraneo, Giancarlo; Metrangolo, Pierangelo; CrystEngComm 20 (2018) 5321–; doi:10.1039/C8CE01205A

data_7231390
_publ_section_title
;
 Halogen bonding at the wet interfaces of an amyloid peptide structure
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5321
_journal_paper_doi               10.1039/C8CE01205A
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H41 Cl2 N7 O9, 7 H2 O'
_chemical_formula_sum            'C32 H55 Cl2 N7 O16'
_chemical_formula_weight         864.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-09-13 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.685(5)
_cell_length_b                   4.809(1)
_cell_length_c                   36.125(7)
_cell_measurement_reflns_used    523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.299
_cell_measurement_theta_min      1.722
_cell_volume                     4419.8(17)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.1060
_diffrn_reflns_av_unetI/netI     0.1474
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6299
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        19.299
_diffrn_reflns_theta_max         19.299
_diffrn_reflns_theta_min         1.722
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.3578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker, 2012)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       'Thin needles'
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 347 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.27(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2411
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.2381
_refine_ls_R_factor_gt           0.1420
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0098P)^2^+148.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2954
_refine_ls_wR_factor_ref         0.3499
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    0.897
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                1373
_reflns_number_total             2411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01205a2.cif
_cod_data_source_block           DFClNKFCl
_cod_depositor_comments
'Adding full bibliography for 7231390--7231391.cif.'
_cod_database_code               7231390
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              3898