Protein-Protein Interface Mimicry by an Oxazoline Piperidine-2,4-dione.
Li, Xun; Taechalertpaisarn, Jaru; Xin, Dongyue; Burgess, Kevin; Organic letters 17 (2015) 632–635; doi:10.1021/ol5036547

data_1518645
_publ_section_title
;
 Protein-Protein Interface Mimicry by an Oxazoline Piperidine-2,4-dione.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              632
_journal_page_last               635
_journal_paper_doi               10.1021/ol5036547
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C24 H35 N3 O2'
_chemical_formula_sum            'C24 H35 N3 O2'
_chemical_formula_weight         398.05
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-09-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.667(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8948(11)
_cell_length_b                   9.7854(8)
_cell_length_c                   18.3889(16)
_cell_measurement_reflns_used    1334
_cell_measurement_temperature    110
_cell_measurement_theta_max      43.22
_cell_measurement_theta_min      2.41
_cell_volume                     2312.6(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_detector                 'MWPC area detector'
_diffrn_detector_type            'Bruker Hi_Star area detector'
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_collimation    0.5mm
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_unetI/netI     0.1331
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24722
_diffrn_reflns_point_group_measured_fraction_full 0.879
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.927
_diffrn_reflns_theta_min         4.037
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0815 after correction.
The Ratio of minimum to maximum transmission is 0.8853.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(4)
_refine_ls_extinction_coef       0.0070(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7347
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1819
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.846
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                5105
_reflns_number_total             7347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5036547_si_002.cif
_cod_data_source_block           kb93
_cod_depositor_comments
;
        Adding full bibliography for 1518645.cif.

2019-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C24 H35 N3 O2)'
_cod_original_formula_sum        'C48 H71 N6 O4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     796.10
_cod_database_code               1518645
_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:
 C1A(H1A), C1B(H1B), C13A(H13A), C13B(H13B), C14A(H14A), C14B(H14B),
 C19A(H19A), C19B(H19B), C21A(H21A), C21B(H21B)
2.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C16A(H16A,
 H16B), C16B(H16C,H16D), C20A(H20A,H20B), C20B(H20C,H20D), C23A(H23A,H23B),
 C23B(H23C,H23D)
2.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C8A(H8A), C8B(H8B), C9A(H9A), C9B(H9B), C10A(H10A),
 C10B(H10B), C11A(H11A), C11B(H11B), C12A(H12A), C12B(H12B), N1A(H1AA),
 N1B(H1BA), N2A(H2A), N2B(H2B)
2.d Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C24A(H24A,H24B,H24C),
 C24B(H24D,H24E,H24F)
;
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.972
_shelx_hkl_checksum              62451
_shelx_res_checksum              42276
_shelxl_version_number           2013-4