The rippled β-sheet layer configuration—a novel supramolecular architecture based on predictions by Pauling and Corey
Hazari, Amaruka; Sawaya, Michael R.; Vlahakis, Niko; Johnstone, Timothy C.; Boyer, David; Rodriguez, Jose; Eisenberg, David; Raskatov, Jevgenij A.; Chemical Science  (2022) –; doi:10.1039/D2SC02531K

data_1567280
_publ_section_title
;
 The rippled \b-sheet layer configuration---a novel supramolecular
 architecture based on predictions by Pauling and Corey
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02531K
_journal_year                    2022
_chemical_formula_moiety         'C29 H30 N4 O4, 0.5[C2H3F3O], 0.5[H2O]'
_chemical_formula_sum            'C30 H32.5 F1.5 N4 O5'
_chemical_formula_weight         557.614
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.05.31 svn.r152b0213 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.040(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.5344(5)
_cell_length_b                   23.7071(16)
_cell_length_c                   24.8206(12)
_cell_measurement_reflns_used    8225
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      76.0270
_cell_measurement_theta_min      2.5670
_cell_volume                     5540.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9873
_diffrn_measured_fraction_theta_max 0.9873
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00   7.00   0.50   60.00    --  -49.41  76.00 -15.00   68
  2  \w   -121.00 -29.00   0.50   60.00    --  -49.41 -76.00-142.00  184
  3  \w     51.00  76.00   0.50   60.00    --   49.41  76.00 -15.00   50
  4  \w     -6.00  69.00   0.50   60.00    --   49.41 -76.00-142.00  150
  5  \w    -47.00 -20.00   0.50   60.00    --  -84.25  76.00 -15.00   54
  6  \w   -134.00-109.00   0.50   60.00    --  -84.25 -76.00-142.00   50
  7  \w     89.00 139.00   0.50   60.00    --  105.75  76.00 -15.00  100
  8  \w     34.00 100.00   0.50   60.00    --  105.75 -76.00-142.00  132
  9  \w   -119.00 -92.00   0.50   60.00    --  -49.41-125.00  60.00   54
 10  \w   -121.00 -96.00   0.50   60.00    --  -49.41 -57.00 -90.00   50
 11  \w    -16.00  23.00   0.50   60.00    --  -49.41  19.00   0.00   78
 12  \w   -121.00 -82.00   0.50   60.00    --  -49.41 -57.00   0.00   78
 13  \w   -114.00 -86.00   0.50   60.00    --  -49.41 -57.00  30.00   56
 14  \w     36.00  95.00   0.50   60.00    --   49.41-125.00-120.00  118
 15  \w   -110.00 -85.00   0.50   60.00    --  -84.25 -76.00-142.00   50
 16  \w    -42.00 -13.00   0.50   60.00    --  -84.25  38.00-180.00   58
 17  \w     34.00  60.00   0.50   60.00    --  105.75 -57.00   0.00   52
 18  \w    141.00 167.00   0.50   60.00    --  105.75 125.00 -90.00   52
 19  \w     34.00  65.00   0.50   60.00    --  105.75 -57.00  60.00   62
 20  \w     35.00  61.00   0.50   60.00    --  105.75 -57.00 150.00   52
 21  \w     35.00  64.00   0.50   60.00    --  105.75 -57.00 -60.00   58
 22  \w     42.00  67.00   0.50   60.00    --  105.75 -57.00 -90.00   50
 23  \w     98.00 166.00   0.50   60.00    --  105.75  19.00 -60.00  136
 24  \w     40.00  65.00   0.50   60.00    --  105.75 -57.00 120.00   50
 25  \w     38.00  64.00   0.50   60.00    --  105.75 -77.00 -90.00   52
 26  \w     76.00 102.00   0.50   60.00    --  105.75 -77.00 -90.00   52
 27  \w     34.00  59.00   0.50   60.00    --  105.75 -57.00-180.00   50
 28  \w     35.00  61.00   0.50   60.00    --  105.75 -57.00  90.00   52
 29  \w     98.00 124.00   0.50   60.00    --  105.75 125.00 -90.00   52
 30  \w    104.00 175.00   0.50   60.00    --  105.75  19.00 -90.00  142
 31  \w     39.00  64.00   0.50   60.00    --  105.75-125.00-120.00   50
 32  \w     67.00  93.00   0.50   60.00    --  105.75 -77.00-120.00   52
 33  \w     37.00  62.00   0.50   60.00    --  105.75 -57.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.9873
_diffrn_reflns_Laue_measured_fraction_max 0.9873
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42109
_diffrn_reflns_point_group_measured_fraction_full 0.9873
_diffrn_reflns_point_group_measured_fraction_max 0.9873
_diffrn_reflns_theta_full        67.0781
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       needle
_exptl_crystal_F_000             2360.654
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.0975
_refine_diff_density_min         -0.7032
_refine_diff_density_rms         0.1296
_refine_ls_d_res_high            0.8370
_refine_ls_d_res_low             17.0410
_refine_ls_goodness_of_fit_ref   1.0297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    110
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9787
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.0269
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1688P)^2^+1.8094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2327
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                5493
_reflns_number_total             9787
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc02531k2.cif
_cod_data_source_block           FWF_fwf
_cod_original_cell_volume        5540.6(6)
_cod_database_code               1567280
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 C303, C301, C304, C305, C309, C307, C308, C306
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C201(H20a), C501(H50a), C601(H60a), C101(H101), C301(H30a), C401(H401)
3.b Secondary CH2 refined with riding coordinates:
 C103(H10d,H10e), C203(H20b,H20c), C403(H40d,H40e), C503(H50b,H50c), C603(H60b,
 H60c), C303(H30b,H30c)
3.c Aromatic/amide H refined with riding coordinates:
 N201(H201), N601(H601), N301(H301), N501(H501), N502(H502), C105(H105),
 C510(H510), N202(H202), C106(H106), C405(H405), C509(H509), C406(H406),
 C107(H107), C508(H508), C409(H409), C505(H505), C210(H210), C407(H407),
 C108(H108), C408(H408), C109(H109), C507(H507), C609(H609), C209(H209),
 C205(H205), C208(H208), C207(H207), C608(H608), C605(H605), C306(H306),
 C607(H607), C307(H307), C305(H305), C606(H606), C309(H309), C308(H308)
3.d Idealised Me refined as rotating group:
 N101(H10a,H10b,H10c), N401(H40a,H40b,H40c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 262 electrons were 
found in a volume of 706\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 0.5[C2H3F3O], 0.5[H2O] per Formula Unit 
which account for 240 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;