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_4517364
_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 O4'
_chemical_formula_sum            'C27 H29 N3 O4'
_chemical_formula_weight         459.53
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.648(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9113(3)
_cell_length_b                   18.1972(8)
_cell_length_c                   10.1370(4)
_cell_measurement_reflns_used    4706
_cell_measurement_temperature    298(4)
_cell_measurement_theta_max      24.9910
_cell_measurement_theta_min      2.3330
_cell_volume                     1227.64(9)
_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      air
_diffrn_ambient_temperature      298(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -11.00  104.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0898   57.0000    0.0000 115

  2 omega  -59.00  115.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0898   19.0000 -180.0000 174

  3 omega  -20.00    5.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6054  -99.0000   30.0000 25

  4 omega -122.00  -55.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6054  178.0000  150.0000 67

  5 omega  -20.00   31.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6054  -99.0000 -150.0000 51

  6 omega  -11.00  104.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0898   57.0000 -120.0000 115

  7 omega   35.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0898  178.0000 -150.0000 89
;
_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      0.0203930000
_diffrn_orient_matrix_UB_12      -0.0008233000
_diffrn_orient_matrix_UB_13      0.0724126000
_diffrn_orient_matrix_UB_21      -0.0768281000
_diffrn_orient_matrix_UB_22      0.0263380000
_diffrn_orient_matrix_UB_23      -0.0032910000
_diffrn_orient_matrix_UB_31      -0.0710216000
_diffrn_orient_matrix_UB_32      -0.0287187000
_diffrn_orient_matrix_UB_33      -0.0051111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10027
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38572
_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_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.2458
_exptl_crystal_size_mid          0.2358
_exptl_crystal_size_min          0.1587
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 1519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.25(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0470
_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          0.1506
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                3822
_reflns_number_total             4315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03532_si_001.cif
_cod_data_source_block           npap
_cod_database_code               4517364
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N H O'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.980
_reflns_odcompleteness_completeness 93.19
_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
2.a Ternary CH refined with riding coordinates:
 C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C1(H1A), C2(H2A), C3(H3A), C4(H4), C5(H5), C8(H8),
 C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C27(H27C,H27A,H27B)
;
_olex2_date_sample_data_collection 2018-04-05
_olex2_submission_special_instructions 'No special instructions were received'