Structural features and molecular aggregations of designed triple-stranded β-sheets in single crystals.
Bandyopadhyay, Anupam; Misra, Rajkumar; Gopi, Hosahudya N.; Chemical communications (Cambridge, England) 52 (2016) 4938–4941; doi:10.1039/c6cc00127k

data_7118844
_publ_section_title
;
 Structural features and molecular aggregations of designed
 triple-stranded \b-sheets in single crystals.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4938
_journal_page_last               4941
_journal_paper_doi               10.1039/c6cc00127k
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C79 H134 N16 O16'
_chemical_formula_sum            'C79 H134 N16 O16'
_chemical_formula_weight         1564.01
_chemical_name_common            'Alpha-gamma hybrid peptide'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-03 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.224(6)
_cell_angle_beta                 97.197(6)
_cell_angle_gamma                113.827(4)
_cell_formula_units_Z            1
_cell_length_a                   12.367(3)
_cell_length_b                   13.818(3)
_cell_length_c                   16.091(5)
_cell_measurement_reflns_used    4937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.13
_cell_volume                     2342.2(11)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44301
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       'Rectangular block'
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
The SQUEEZE routine of the program PLATON was used

in order to eliminate the contribution of disordered solvents molecules,

thereby a final model based only on the ordered part of the crystal structure

was obtained.

The SQUEEZE routine suggested that

a total potential solvent area volume of 147.5Ang^3^[6.3% of cell volume],

and a void electron population of 17 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.

[R values before SQUEEZE]

R1 = 0.075, wR2 = 0.1732 for >2sigma(I) data

R1 = 0.1056, wR2 = 0.1939, GooF = S = 1.014 for all data

( 21007 data and 5 restraint / 1009 parameters)

;
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 4976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.5(5)
_refine_ls_extinction_coef       0.013(2)
_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   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         21007
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.853
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                14418
_reflns_number_total             21007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00127k2.cif
_cod_data_source_block           P1
_cod_depositor_comments
'Adding full bibliography for 7118843--7118844.cif.'
_cod_original_cell_volume        2342.2(10)
_cod_database_code               7118844
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-3
_shelx_res_checksum              29159