Residue-based program of a β-peptoid twisted strand shape via a cyclopentane constraint
Kim, Jungyeon; Kobayashi, Hiroka; Yokomine, Marin; Shiratori, Yota; Ueda, Takumi; Takeuchi, Koh; Umezawa, Koji; Kuroda, Daisuke; Tsumoto, Kouhei; Morimoto, Jumpei; Sando, Shinsuke; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB01300B

data_7158836
_publ_section_title
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 Residue-based program of a \b-peptoid twisted strand shape via a
 cyclopentane constraint
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_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01300B
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H77 N5 O5, C2 H F3 O2'
_chemical_formula_sum            'C46 H78 F3 N5 O7'
_chemical_formula_weight         870.157
_chemical_name_systematic        'N-isobutyl ACPC tetramer'
_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_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-08
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2022-05-16 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.422(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3139(3)
_cell_length_b                   10.3854(3)
_cell_length_c                   24.6159(7)
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.8430
_cell_measurement_theta_min      4.7440
_cell_volume                     2381.00(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9862
_diffrn_measured_fraction_theta_max 0.9649
_diffrn_measurement_details
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List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     50.00  80.00   0.50    3.02    --    5.00  18.00  60.00   60
  2  \w    -66.00 -34.00   0.50    3.02    --    5.00  18.00  60.00   64
  3  \w     16.00  94.00   0.50    3.02    --    5.00  37.00 -30.00  156
  4  \w    -84.00  -6.00   0.50    3.02    --    5.00  37.00 -30.00  156
  5  \w   -184.00  -7.00   0.50    3.02    --  -96.70  28.00  90.00  354
  6  \w    -91.00 -23.00   0.50    3.02    --  -96.70  53.00  18.56  136
  7  \w   -186.00 -78.00   0.50    3.02    --  -96.70  46.00 -60.00  216
  8  \w   -172.00-138.00   0.50    3.02    --  -96.70  37.00 -60.00   68
  9  \w   -180.00 -28.00   0.50    3.02    --  -96.70  55.00   0.98  304
 10  \w   -127.00 -98.00   0.50    3.02    --  -96.70  37.00 -60.00   58
 11  \w   -108.00 -15.00   0.50    3.02    --  -96.70  37.00  60.00  186
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_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.9862
_diffrn_reflns_Laue_measured_fraction_max 0.9649
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13543
_diffrn_reflns_point_group_measured_fraction_full 0.7468
_diffrn_reflns_point_group_measured_fraction_max 0.7209
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.05
_diffrn_reflns_theta_min         4.62
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             947.131
_refine_diff_density_max         0.1578
_refine_diff_density_min         -0.1682
_refine_diff_density_rms         0.0350
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.04(12)
_refine_ls_d_res_high            0.8103
_refine_ls_d_res_low             9.5686
_refine_ls_goodness_of_fit_ref   1.0556
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    118
_refine_ls_number_parameters     562
_refine_ls_number_reflns         6755
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0556
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.6785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.446
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -10
_reflns_limit_l_max              29
_reflns_limit_l_min              -27
_reflns_number_gt                6333
_reflns_number_total             6755
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2ob01300b2.cif
_cod_data_source_block           exp_963
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7158836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00M(H00M), C00P(H00P), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C014(H014), C01E(H01z), C01F(H01)
2.b Secondary CH2 refined with riding coordinates:
 C00J(H00a,H00b), C00L(H00c,H00d), C00Q(H00e,H00f), C00R(H00g,H00h), C00T(H00j,
 H00l), C00V(H00n,H00o), C010(H01a,H01b), C011(H01c,H01d), C012(H01e,H01f),
 C015(H01g,H01h), C019(H01o,H01p), C01B(H01t,H01u), C01H(H2,Hd), C01I(H3,He),
 C01J(H4,Hf), C01K(H5,Hg)
2.c Idealised Me refined as rotating group:
 C016(H01i,H01j,H01k), C017(H01l,H01m,H01n), C01A(H01q,H01r,H01s), C01C(H01v,
 H01w,H01x), C01D(H01y,H,Ha), C01G(H1,Hb,Hc), C01L(H6,Hh,Hi), C01M(H7,Hj,Hk),
 C01N(H8,Hl,Hm), C01O(H9,Hn,Ho), C01P(H10,Hp,Hq)
2.d Idealised tetrahedral OH refined as rotating group:
 O008(H008)
;
_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
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_publcif_funding_html
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