Turn Conformation of β-Amino Acid Based Short Peptides Promoted by an Amidothiourea Moiety at C-Terminus.
Zhang, Yanhan; Yan, Xiaosheng; Cao, Jinlian; Weng, Peimin; Miao, Daiyu; Li, Zhao; Jiang, Yun-Bao; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01139

data_4038565
_publ_section_title
;
 Turn Conformation of \b-Amino Acid Based Short Peptides Promoted by an
 Amidothiourea Moiety at C-Terminus.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01139
_journal_year                    2020
_chemical_formula_moiety         '2(C12 H16 N4 O2 S), 0.5(C4 H6 N2)'
_chemical_formula_sum            'C26 H35 N9 O4 S2'
_chemical_formula_weight         601.75
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7556(2)
_cell_length_b                   7.9327(2)
_cell_length_c                   17.5581(4)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7340
_cell_measurement_theta_min      5.0600
_cell_volume                     1487.10(6)
_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_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.751
_diffrn_reflns_theta_min         4.141
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0568P)^2^+1.1386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2862
_reflns_number_total             3045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01139_si_002.cif
_cod_data_source_block           a32
_cod_database_code               4038565
_shelx_shelxl_version_number     2014/7
_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. Others
 Sof(H00I)=Sof(C00H)=Sof(H00J)=Sof(C00I)=Sof(H00K)=Sof(C00K)=Sof(H00M)=
 Sof(C00M)=Sof(H00O)=1-FVAR(1)
 Sof(H00H)=Sof(C00J)=Sof(H00L)=Sof(C00L)=Sof(H00N)=Sof(C00N)=Sof(H00P)=
 Sof(C00O)=Sof(H00Q)=FVAR(1)
 Fixed Sof: C00P(0.5) C0AA(0.5) N1(0.5) H00R(0.5) H00S(0.5) H00T(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C00B(H00A,H00B), C00D(H00C,H00D)
3.b Aromatic/amide H refined with riding coordinates:
 N004(H004), N005(H005), N006(H006), N007(H007), C00F(H00I), C00F(H00H),
 C00H(H00J), C00I(H00K), C00J(H00L), C00K(H00M), C00L(H00N), C00M(H00O),
 C00N(H00P), C00O(H00Q)
3.c Idealised Me refined as rotating group:
 C00E(H00E,H00F,H00G)
;
_shelx_res_checksum              18158
_shelx_hkl_checksum              23341
_olex2_submission_special_instructions 'No special instructions were received'