Conformational Heterogeneity and Self-Assembly of α,β,γ-Hybrid Peptides Containing Fenamic Acid: Multistimuli-Responsive Phase-Selective Gelation
Chowdhury, Srayoshi Roy; Nandi, Sujay Kumar; Podder, Debasish; Haldar, Debasish; ACS Omega  (2020) –; doi:10.1021/acsomega.9b03532

data_4517362
_publ_section_title
;
 Conformational Heterogeneity and Self-Assembly of \a,\b,\g-Hybrid
 Peptides Containing Fenamic Acid: Multistimuli-Responsive Phase-Selective
 Gelation
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.9b03532
_journal_year                    2020
_chemical_absolute_configuration s
_chemical_formula_moiety         'C27 H29 N3 O5'
_chemical_formula_sum            'C27 H29 N3 O5'
_chemical_formula_weight         475.53
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.637(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9049(6)
_cell_length_b                   17.9673(13)
_cell_length_c                   10.1305(7)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      24.9720
_cell_measurement_theta_min      2.2420
_cell_volume                     1204.20(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   -5.00   26.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7617  -99.0000  -30.0000 31

  2 omega   50.00  110.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679  178.0000  -60.0000 60

  3 omega  -41.00   88.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679   19.0000   60.0000 129
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0272512000
_diffrn_orient_matrix_UB_12      0.0215006000
_diffrn_orient_matrix_UB_13      -0.0506814000
_diffrn_orient_matrix_UB_21      0.0534935000
_diffrn_orient_matrix_UB_22      -0.0308578000
_diffrn_orient_matrix_UB_23      -0.0156774000
_diffrn_orient_matrix_UB_31      -0.0888027000
_diffrn_orient_matrix_UB_32      -0.0120372000
_diffrn_orient_matrix_UB_33      -0.0502498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3435
_diffrn_reflns_point_group_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.644
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.098
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         2739
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0423
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.259
_reflns_Friedel_fraction_full    0.275
_reflns_Friedel_fraction_max     0.275
_reflns_number_gt                2588
_reflns_number_total             2739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03532_si_004.cif
_cod_data_source_block           npat
_cod_database_code               4517362
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 91.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 N007(H007)
2.b Ternary CH refined with riding coordinates:
 C00E(H00E)
2.c Secondary CH2 refined with riding coordinates:
 C00U(H00A,H00B)
2.d Aromatic/amide H refined with riding coordinates:
 N006(H006), N008(H008), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K),
 C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S),
 C00T(H00T), C00W(H00W), C00Y(H00Y)
2.e Idealised Me refined as rotating group:
 C00V(H00C,H00D,H00F), C00X(H00I,H00L,H00P), C00Z(H00U,H00V,H00X)
2.f Idealised tetrahedral OH refined as rotating group:
 O004(H004)
;
_olex2_date_sample_data_collection 2018-07-16
_olex2_submission_special_instructions 'No special instructions were received'