Hydrogen-Bonding-Driven 3D Supramolecular Assembly of Peptidomimetic Zipper.
Teng, Peng; Niu, Zheng; She, Fengyu; Zhou, Mi; Sang, Peng; Gray, Geoffrey M.; Verma, Gaurav; Wojtas, Lukasz; van der Vaart, Arjan; Ma, Shengqian; Cai, Jianfeng; Journal of the American Chemical Society 140 (2018) 5661–5665; doi:10.1021/jacs.7b11997

data_4131880
_publ_section_title
;
 Hydrogen-Bonding-Driven 3D Supramolecular Assembly of Peptidomimetic
 Zipper.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5661
_journal_page_last               5665
_journal_paper_doi               10.1021/jacs.7b11997
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_sum            'C260 H378 Cl12 N56 O71.5 S14'
_chemical_formula_weight         6306.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 110.983(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.981(5)
_cell_length_b                   25.970(7)
_cell_length_c                   21.424(6)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.37
_cell_measurement_theta_min      2.15
_cell_volume                     9860(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Pilatus3 X CdTe 1M'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.44281
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128797
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        12.795
_diffrn_reflns_theta_max         12.795
_diffrn_reflns_theta_min         0.867
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.047
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (2016/2)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       plate
_exptl_crystal_F_000             3330
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 4882 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2281
_refine_ls_number_reflns         20552
_refine_ls_number_restraints     5223
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.1308
_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^)+(0.2939P)^2^+2.5700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3394
_refine_ls_wR_factor_ref         0.3905
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                13363
_reflns_number_total             20552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11997_si_003.cif
_cod_data_source_block           HTP_H_011
_cod_original_cell_volume        9860(4)
_cod_original_sg_symbol_H-M      'P 2'
_cod_original_formula_sum        'C260 H378 Cl12 N56 O71.50 S14'
_cod_database_code               4131880
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              6583
_shelx_hkl_checksum              55312