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_4129603
_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 H48 N8, 4(F6 P), C10 H10 Fe'
_chemical_formula_sum            'C54 H58 F24 Fe N8 P4'
_chemical_formula_weight         1454.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_Hall           '-P 4ac 2ac'
_space_group_name_H-M_alt        'P 42/n c m :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.650(2)
_cell_length_b                   26.650(2)
_cell_length_c                   9.8528(9)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.07
_cell_measurement_theta_min      3.71
_cell_volume                     6997.7(10)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            57013
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.576
_diffrn_reflns_theta_min         2.344
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.530
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.9022.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1010
_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^)+(0.0720P)^2^+46.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2405
_refine_ls_wR_factor_ref         0.2480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2531
_reflns_number_total             3182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08656_si_004.cif
_cod_data_source_block           386jb_a
_cod_original_cell_volume        6997.8(13)
_cod_original_sg_symbol_H-M      'P 42/n c m'
_cod_database_code               4129603
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.594
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Shared sites
{N1, C1A}
{N2, C2A}
{C11, N11}
{C3, N3}
3. Restrained distances
 C15-C14 \\sim C14-C13 \\sim C17-C13 \\sim C17-C16 \\sim C16-C15 \\sim C22-C18
\\sim C19-C18 \\sim C20-C19
 \\sim C21-C20 \\sim C22-C21
 with sigma of 0.01
4. Rigid bond restraints
 C13, C14, C15, C16, C17, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim
C21 \\sim C22: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N1) = Uanis(C1A)
Uanis(N2) = Uanis(C2A)
Uanis(C11) = Uanis(N11)
Uanis(C3) = Uanis(N3)
6. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) H3(0.5) N11(0.5) H11(0.5) C1A(0.5)
 C2A(0.5) C3(0.5) H3A(0.5) H6A(0.5) H6B(0.5) H9A(0.5) H9B(0.5) C11(0.5)
 H11A(0.5) H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) Fe1(0.25) C13(0.25)
 H13(0.25) C14(0.25) H14(0.25) C15(0.25) H15(0.25) C16(0.25) H16(0.25)
 C17(0.25) H17(0.25) C18(0.25) H18(0.25) C19(0.25) H19(0.25) C20(0.25)
 H20(0.25) C21(0.25) H21(0.25) C22(0.25) H22(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C12(H12A,H12B), C12(H12C,H12D)
7.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N11(H11), C3(H3A), C5(H5), C6(H6A), C6(H6B), C8(H8), C9(H9A), C9(H9B),
  C11(H11A), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22)
;
_smtbx_masks_special_details
;
The solvent-masking procedure as implemented in Olex2 was used to remove
the electronic contribution of solvent molecules from the refinement.
As the exact solvent content is not known, only the atoms used in the
refinement are reported in the formula here.

Total solvent accessible volume / cell = 1245.3 Ang^3 [17.8%]
Total electron count / cell = 304.7
;
_shelx_res_checksum              61809
_shelx_hkl_checksum              33519
_olex2_submission_special_instructions 'No special instructions were received'