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_7124664
_publ_section_title
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 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         'C92 H96 N16 O12, 6(C H4 O)'
_chemical_formula_sum            'C98 H120 N16 O18'
_chemical_formula_weight         1810.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-07 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            4
_cell_length_a                   15.4204(2)
_cell_length_b                   15.4204(2)
_cell_length_c                   43.9852(6)
_cell_measurement_reflns_used    9417
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.98
_cell_measurement_theta_min      3.04
_cell_volume                     10459.2(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            71295
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.037
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9101
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.9101.
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    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9215
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+5.6564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8320
_reflns_number_total             9215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03296f2.cif
_cod_data_source_block           x1204022
_cod_original_cell_volume        10459.2(3)
_cod_database_code               7124664
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H8A,H8B,H8C} of C8, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, {H24A,H24B,H24C} of C24, {H48A,H48B,H48C} of C48, {H49A,
  H49B,H49C} of C49, {H47A,H47B,H47C} of C47
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C0AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C21(H21), C44(H44)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C25(H25A,H25B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
3.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), N2(H2), C2(H2A), C3(H3), C4(H4), N5(H5), C5(H5A), N6(H6),
 C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C33(H33), C35(H35), C36(H36), C38(H38), C39(H39), N46(H46)
3.d Tetrahedral OH refined with riding coordinates:
 O9(H9), O7(H7), O8(H8)
3.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C49(H49A,H49B,H49C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              44675
_shelx_hkl_checksum              98621
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'