The influence of backbone fluorination on the helicity of α/γ-hybrid peptides
Patel, Alpesh Ramanlal; Lawer, Aggie; Bhadbhade, Mohan; Hunter, Luke; Organic & Biomolecular Chemistry 22 (2024) 1608–1612; doi:10.1039/D3OB02016A

data_7159791
_publ_section_title
;
 The influence of backbone fluorination on the helicity of \a/\g-hybrid
 peptides
;
_journal_issue                   8
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1608
_journal_page_last               1612
_journal_paper_doi               10.1039/D3OB02016A
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         '1.5(C H2 Cl2), C57 H100 N10 O11'
_chemical_formula_sum            'C58.5 H103 Cl3 N10 O11'
_chemical_formula_weight         1228.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-03 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.447(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8607(6)
_cell_length_b                   10.4771(3)
_cell_length_c                   36.3667(11)
_cell_measurement_reflns_used    2292
_cell_measurement_temperature    154.56
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     7186.0(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      154.56
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            56738
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.120
_exptl_absorpt_coefficient_mu    0.185
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.091
_refine_diff_density_max         2.743
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         14103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0929
_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^)+(0.1856P)^2^+9.3375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2733
_refine_ls_wR_factor_ref         0.3042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10025
_reflns_number_total             14103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob02016a2.cif
_cod_data_source_block           alpesh_02march15_a
_cod_depositor_comments
'Adding full bibliography for 7159791--7159792.cif.'
_cod_original_formula_sum        'C58.50 H103 Cl3 N10 O11'
_cod_database_code               7159791
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1E(0.5) Cl2E(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1D(H1DA,H1DB), C1E(H1EA,H1EB), C4(H4A,H4B), C6(H6A,H6B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C18(H18A,H18B), C22(H22A,H22B),
  C24(H24A,H24B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C172(H17A,H17B), C173(H17C,H17D), C174(H17E,H17F),
 C175(H17G,H17H), C176(H17I,H17J), C232(H23A,H23B), C233(H23C,H23D), C234(H23E,
 H23F), C235(H23G,H23H), C236(H23I,H23J)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9(H9),
 N10(H10)
3.c Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC), C2D(H2DA,H2DB,H2DC), C3B(H3BA,H3BB,
 H3BC), C4B(H4BA,H4BB,H4BC), C28(H28A,H28B,H28C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C141(H14A,H14B,H14C), C142(H14D,H14E,H14F), C201(H20A,H20B,H20C),
 C202(H20D,H20E,H20F), C261(H26A,H26B,H26C), C262(H26D,H26E,H26F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49092
_shelx_fab_checksum              2798
_olex2_submission_special_instructions 'No special instructions were received'