Allosteric Modulation of Substrate Binding within a Tetracationic Molecular Receptor.
Henkelis, James J.; Blackburn, Anthea K.; Dale, Edward J.; Vermeulen, Nicolaas A.; Nassar, Majed S.; Stoddart, J. Fraser; Journal of the American Chemical Society 137 (2015) 13252–13255; doi:10.1021/jacs.5b08656

data_4129601
_publ_section_title
;
 Allosteric Modulation of Substrate Binding within a Tetracationic
 Molecular Receptor.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13252
_journal_page_last               13255
_journal_paper_doi               10.1021/jacs.5b08656
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C44 H36 N8, 4(F6 P), 6(C2 H3 N)'
_chemical_formula_sum            'C56 H54 F24 N14 P4'
_chemical_formula_weight         1503.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                70.750(3)
_cell_angle_beta                 84.112(2)
_cell_angle_gamma                70.850(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0907(6)
_cell_length_b                   14.3187(6)
_cell_length_c                   17.7215(7)
_cell_measurement_reflns_used    7034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.299
_cell_measurement_theta_min      3.321
_cell_volume                     3188.7(2)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23141
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.377
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0601 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8439.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         10530
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0925
_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^)+(0.1130P)^2^+17.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2484
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8368
_reflns_number_total             10530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08656_si_002.cif
_cod_data_source_block           p-1
_cod_database_code               4129601
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12A,H12B,H12C} of C12S, All C(H,H) groups
 At 1.5 times of:
  {H4SA,H4SB,H4SC} of C4S, {H10A,H10B,H10C} of C10S, {H8SA,H8SB,H8SC} of C8S,
  {H6SA,H6SB,H6SC} of C6S, {H2SA,H2SB,H2SC} of C2S
2. Rigid bond restraints
 P4, F41, F43A, F41A, F46A, F43, F45, F45A, F46, F42A, F44, F42, F44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
P4 \\sim F41 \\sim F43A \\sim F41A \\sim F46A \\sim F43 \\sim F45 \\sim F45A
\\sim F46 \\sim F42A \\sim F44 \\sim F42 \\sim F44A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.001
4. Others
 Sof(F41A)=Sof(F42A)=Sof(F43A)=Sof(F44A)=Sof(F45A)=Sof(F46A)=1-FVAR(1)
 Sof(F41)=Sof(F42)=Sof(F43)=Sof(F44)=Sof(F45)=Sof(F46)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
 C37(H37), C40(H40), C41(H41), C42(H42)
5.c Idealised Me refined as rotating group:
 C8S(H8SA,H8SB,H8SC), C6S(H6SA,H6SB,H6SC), C10S(H10A,H10B,H10C), C4S(H4SA,H4SB,
 H4SC), C2S(H2SA,H2SB,H2SC), C12S(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'