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_4129602
_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 Cl4 N8 Pd2, 4(F6 P), 4(C2 H6 O S)'
_chemical_formula_sum            'C52 H60 Cl4 F24 N8 O4 P4 Pd2 S4'
_chemical_formula_weight         1923.80
_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     dual
_audit_creation_date             2015-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                89.642(4)
_cell_angle_beta                 87.887(4)
_cell_angle_gamma                78.405(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8489(7)
_cell_length_b                   14.2410(11)
_cell_length_c                   18.2764(14)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.322
_cell_measurement_theta_min      3.127
_cell_volume                     2254.6(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.06
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.795
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28643
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.335
_diffrn_reflns_theta_min         1.460
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0504 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.9329. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.404
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         6488
_refine_ls_number_restraints     706
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0980P)^2^+9.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5448
_reflns_number_total             6488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08656_si_003.cif
_cod_data_source_block           p-1_2
_cod_database_code               4129602
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S1S-O1S
 1.46 with sigma of 0.02
3. Rigid bond restraints
 O2T, S2T, C3T, C4T, C3S, S2S, O2S, C4S
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.01
 F14, P1, F14A, F12, F11A, F12A, F11, F16, F16A, F15A, F13, F15, F13A
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4S \\sim S2S \\sim O2S \\sim C3S \\sim C4T \\sim S2T \\sim O2T \\sim C3T:
within 2A with sigma of 0.1 and sigma for terminal atoms of 0.01
F13 \\sim P1 \\sim F14A \\sim F14 \\sim F12 \\sim F11A \\sim F12A \\sim F11
\\sim F16 \\sim F16A \\sim F15A \\sim F15 \\sim F13A: within 2A with sigma of
0.1 and sigma for terminal atoms of 0.01
Uanis(S2T) = Uanis(S2S) = Uanis(O2T) = Uanis(O2S) = Uanis(C3T) = Uanis(C3S) =
Uanis(C4T) = Uanis(C4S)
5. 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
6. Others
 Sof(H2SD)=Sof(H2SE)=Sof(H2SF)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=Sof(S1T)=1-FVAR(1)
 Sof(S1S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=FVAR(1)
 Sof(S2T)=Sof(O2T)=Sof(C3T)=Sof(H2TA)=Sof(H2TB)=Sof(H2TC)=Sof(C4T)=Sof(H4TA)=
 Sof(H4TB)=Sof(H4TC)=1-FVAR(2)
 Sof(S2S)=Sof(O2S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(C4S)=Sof(H4SA)=
 Sof(H4SB)=Sof(H4SC)=FVAR(2)
 Sof(F11A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F12A)=Sof(F13A)=1-FVAR(3)
 Sof(F11)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F12)=Sof(F13)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B)
7.b Me refined with riding coordinates:
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC), C2S(H2SD,H2SE,
 H2SF), C1S(H1SA,H1SB,H1SC), C1S(H1SD,H1SE,H1SF), C3T(H2TA,H2TB,H2TC), C4T(H4TA,
 H4TB,H4TC)
7.c 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)
;
_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 = 563.0 Ang^3 [25.0%]
Total electron count / cell = 269.8
;
_olex2_submission_special_instructions 'No special instructions were received'