Tetrameric psuedo-peptide receptors with allosteric properties.
Chung, Mee-Kyung; Lee, Stephen J.; Waters, Marcey L.; Gagné, Michel R; Chemical communications (Cambridge, England) 52 (2016) 8103–8106; doi:10.1039/c6cc03296f

data_7124665
_publ_section_title
;
 Tetrameric psuedo-peptide receptors with allosteric properties.
;
_journal_issue                   52
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8103
_journal_page_last               8106
_journal_paper_doi               10.1039/c6cc03296f
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C68 H80 N16 O12'
_chemical_formula_sum            'C68 H80 N16 O12'
_chemical_formula_weight         1313.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-08 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2194(6)
_cell_length_b                   26.8073(8)
_cell_length_c                   30.7909(8)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100
_cell_measurement_theta_max      62.46
_cell_measurement_theta_min      2.19
_cell_volume                     18340.4(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40540
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        49.995
_diffrn_reflns_theta_max         49.995
_diffrn_reflns_theta_min         2.185
_diffrn_source                   'sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.6
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0738 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.7763.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.951
_exptl_crystal_description       plate
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 3129 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1649
_refine_ls_number_reflns         17305
_refine_ls_number_restraints     2719
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.859
_reflns_number_gt                11145
_reflns_number_total             17305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03296f2.cif
_cod_data_source_block           x1007002
_cod_database_code               7124665
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.805
_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. Restrained distances
 C93-N89
 1.4 with sigma of 0.02
 C28-N30 = C28-C27
 1.5 with sigma of 0.02
 N24-C27 = N24-C22
 1.5 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.02
 C20-C19
 1.5 with sigma of 0.02
 C19-C18
 1.5 with sigma of 0.02
 C18-N17
 1.5 with sigma of 0.02
 C21-N17
 1.5 with sigma of 0.02
 O140-C139
 1.2 with sigma of 0.02
 O123-C122
 1.2 with sigma of 0.02
 C121-C122 = N124-C122
 1.5 with sigma of 0.02
 C9-C8
 1.5 with sigma of 0.02
 N7-C8
 1.3 with sigma of 0.02
 O95-C94
 1.2 with sigma of 0.02
 O29-C28
 1.2 with sigma of 0.02
 O16-C15
 1.2 with sigma of 0.02
 N155-C156
 1.3 with sigma of 0.02
 O116-C115
 1.2 with sigma of 0.02
 N141-C139 = C139-C136
 1.4 with sigma of 0.02
 O147-C146
 1.2 with sigma of 0.02
 N148-C146 = N148-C151
 1.45 with sigma of 0.02
 N96-C3 = N96-C94
 1.45 with sigma of 0.02
 C92-C91 = C92-C93 = C90-C91
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.05 and sigma
for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C21(H21), C45(H45), C69(H69), C93(H93), C121(H121), C145(H145), C169(H169),
 C193(H193)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C118(H11A,H11B), C119(H11C,
 H11D), C120(H12A,H12B), C142(H14A,H14B), C143(H14C,H14D), C144(H14E,H14F),
 C166(H16A,H16B), C167(H16C,H16D), C168(H16E,H16F), C190(H19C,H19D), C191(H19E,
 H19F), C192(H19G,H19H)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C14(H14), C10(H10), C11(H11), C32(H32), C38(H38), C37(H37),
 C35(H35), C34(H34), C56(H56), C59(H59), C58(H58), C62(H62), C61(H61), C80(H80),
  C82(H82), C86(H86), C85(H85), C83(H83), C108(H108), C113(H113), C114(H114),
 C110(H110), C111(H111), C132(H132), C134(H134), C135(H135), C137(H137),
 C138(H138), C156(H156), C161(H161), C162(H162), C158(H158), C159(H159),
 C180(H180), C186(H186), C182(H182), C183(H183), C185(H185), N6(H6), N24(H24),
 N30(H30), N48(H48), N54(H54), N72(H72), N78(H78), N96(H96), N106(H106),
 N124(H124), N130(H130), N148(H148), N154(H154), N172(H172), N178(H178),
 N196(H196)
5.d Fitted hexagon refined as free rotating group:
 C12(C13,C14,C9,C10,C11), C33(C38,C37,C36,C35,C34), C59(C58,C57,C62,C61,C60),
 C82(C81,C86,C85,C84,C83), C112(C113,C114,C109,C110,C111), C133(C134,C135,C136,
 C137,C138), C161(C162,C157,C158,C159,C160), C186(C181,C182,C183,C184,C185)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C125(H12C,H12D,H12E),
 C126(H12F,H12G,H12H), C149(H14G,H14H,H14I), C150(H15A,H15B,H15C), C173(H17A,
 H17B,H17C), C174(H17D,H17E,H17F)
;
_shelx_res_checksum              341
_shelx_hkl_checksum              67031
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'