Stabilization of 11/9-helical alpha/beta-peptide foldamers in protic solvents
Mihye Lee; Jihyun Shim; Philjae Kang; Moon-Gun Choi; Soo Hyuk Choi; Chem.Commun. 52 (2016) 5950–; doi:

data_7119040
_publ_section_title
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 Stabilization of 11/9-helical alpha/beta-peptide foldamers in protic
 solvents
;
_journal_name_full               Chem.Commun.
_journal_page_first              5950
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C H Cl3, C30 H51 N5 O8'
_chemical_formula_sum            'C31 H52 Cl3 N5 O8'
_chemical_formula_weight         729.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5052(17)
_cell_length_b                   17.583(3)
_cell_length_c                   23.471(4)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.44
_cell_measurement_theta_min      3.14
_cell_volume                     3922.7(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16765
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.338
_diffrn_reflns_theta_min         3.140
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.7637.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2850 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.053(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1348P)^2^+1.8496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                6826
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01189f2.cif
_cod_data_source_block           DAla-mACHC-DAla-ACHC-DAla_moon214
_cod_original_cell_volume        3922.8(11)
_cod_database_code               7119040
_shelxl_version_number           2013-3
_olex2_refinement_description
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1. Others
 Fixed Uiso: H5(0.04) H13(0.039) H16(0.038) H24(0.04) H27(0.034) H1A(0.165)
 H1B(0.165) H1C(0.165) H4(0.043) H7(0.047) H8A(0.061) H8B(0.061) H9A(0.06)
 H9B(0.06) H10(0.058) H11A(0.047) H11B(0.047) H12(0.043) H15(0.04) H18(0.044)
 H19A(0.056) H19B(0.056) H20A(0.065) H20B(0.065) H21A(0.065) H21B(0.065)
 H22A(0.052) H22B(0.052) H23(0.041) H26(0.035) H31A(0.134) H31B(0.134)
 H31C(0.134) H32A(0.082) H32B(0.082) H32C(0.082) H33A(0.167) H33B(0.167)
 H33C(0.167) H35A(0.064) H35B(0.064) H35C(0.064) H37A(0.1) H37B(0.1) H37C(0.1)
 H39A(0.071) H39B(0.071) H39C(0.071) H42A(0.061) H42B(0.061) H42C(0.061)
 H44(0.049) H48(0.341)
 Fixed X: H5(-0.9743) H13(-0.7078) H16(-0.7646) H24(-0.7648) H27(-0.4076) H1A(-
 1.1294) H1B(-0.9741) H1C(-1.0291) H4(-1.1267) H7(-0.7981) H8A(-0.6554) H8B(-
 0.8004) H9A(-0.7062) H9B(-0.5984) H10(-0.4472) H11A(-0.6483) H11B(-0.4999)
 H12(-0.5707) H15(-0.7716) H18(-0.9458) H19A(-1.1823) H19B(-1.1678) H20A(-
 1.3301) H20B(-1.2066) H21A(-1.2405) H21B(-1.2189) H22A(-1.0024) H22B(-1.0101)
 H23(-0.984) H26(-0.5429) H31A(-0.6676) H31B(-0.6001) H31C(-0.6003) H32A(-
 0.3367) H32B(-0.3416) H32C(-0.2407) H33A(-0.3396) H33B(-0.4165) H33C(-0.5058)
 H35A(-1.2492) H35B(-1.2796) H35C(-1.1713) H37A(-0.4199) H37B(-0.3654) H37C(-
 0.5144) H39A(-0.6067) H39B(-0.5243) H39C(-0.5268) H42A(-0.4171) H42B(-0.5688)
 H42C(-0.5431) H44(-1.0917) H48(-1.0797)
 Fixed Y: H5(-1.1373) H13(-1.1429) H16(-0.8908) H24(-0.944) H27(-0.7787) H1A(-
 1.2516) H1B(-1.2651) H1C(-1.1805) H4(-1.252) H7(-1.1669) H8A(-1.2496) H8B(-
 1.2942) H9A(-1.3709) H9B(-1.3724) H10(-1.2868) H11A(-1.2821) H11B(-1.239) H12(-
 1.1661) H15(-1.0286) H18(-0.8388) H19A(-0.8337) H19B(-0.8893) H20A(-0.9361)
 H20B(-0.9956) H21A(-0.9882) H21B(-0.8979) H22A(-1.0066) H22B(-0.9571) H23(-
 0.8438) H26(-0.9074) H31A(-0.6812) H31B(-0.6102) H31C(-0.6125) H32A(-0.5957)
 H32B(-0.59) H32C(-0.6507) H33A(-0.7691) H33B(-0.7139) H33C(-0.7755) H35A(-
 1.1411) H35B(-1.1579) H35C(-1.0924) H37A(-1.4177) H37B(-1.3625) H37C(-1.4041)
 H39A(-0.9399) H39B(-1.0149) H39C(-0.9416) H42A(-0.8604) H42B(-0.8919) H42C(-
 0.8023) H44(-0.9132) H48(-0.8951)
 Fixed Z: H5(-0.5944) H13(-0.6692) H16(-0.6495) H24(-0.512) H27(-0.5267) H1A(-
 0.8313) H1B(-0.8069) H1C(-0.8185) H4(-0.6424) H7(-0.5326) H8A(-0.4848) H8B(-
 0.4928) H9A(-0.5632) H9B(-0.5108) H10(-0.5573) H11A(-0.648) H11B(-0.6488) H12(-
 0.5682) H15(-0.6985) H18(-0.6045) H19A(-0.586) H19B(-0.6396) H20A(-0.5703)
 H20B(-0.5834) H21A(-0.4851) H21B(-0.4865) H22A(-0.5118) H22B(-0.4544) H23(-
 0.5072) H26(-0.5273) H31A(-0.6678) H31B(-0.7005) H31C(-0.6323) H32A(-0.6308)
 H32B(-0.6988) H32C(-0.6686) H33A(-0.7067) H33B(-0.7511) H33C(-0.7164) H35A(-
 0.612) H35B(-0.6779) H35C(-0.6602) H37A(-0.5812) H37B(-0.6308) H37C(-0.6367)
 H39A(-0.7307) H39B(-0.7111) H39C(-0.6707) H42A(-0.4456) H42B(-0.4277) H42C(-
 0.4332) H44(-0.8505) H48(-0.8395)
;