Ex2Box: Interdependent Modes of Binding in a Two-Nanometer-Long Synthetic Receptor
Michal Juríček; Jonathan C. Barnes; Edward J. Dale; Wei-Guang Liu; Nathan L. Strutt; Carson J. Bruns; Nicolaas A. Vermeulen; Kala C. Ghooray; Amy A. Sarjeant; Charlotte L. Stern; Youssry Y. Botros; William A. Goddard; J. Fraser Stoddart; Journal of the American Chemical Society 135 (2013) 12736–12746; doi:10.1021/ja4052763

data_4120378
_publ_section_title
;
 Ex2Box: Interdependent Modes of Binding in a Two-Nanometer-Long Synthetic
 Receptor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12736
_journal_page_last               12746
_journal_paper_doi               10.1021/ja4052763
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C60 H48 N4, C14 H8 O2, 4(F6 P), 2(C H Cl3)'
_chemical_formula_sum            'C76 H58 Cl6 F24 N4 O2 P4'
_chemical_formula_weight         1851.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.911(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7902(4)
_cell_length_b                   14.1309(6)
_cell_length_c                   27.6171(12)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.44
_cell_volume                     3800.4(3)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa 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  0.0520
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            57735
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.412
_diffrn_reflns_theta_min         1.483
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.9217.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         11430
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1282P)^2^+4.5335P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8157
_reflns_number_total             11430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_011.cif
_cod_data_source_block           n2539a
_cod_database_code               4120378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. others
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=1-FVAR(1)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=FVAR(1)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Fixed Sof: O1(0.5) O2(0.5) C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5)
 C34(0.5) C35(0.5) C36(0.5) H36(0.5) C37(0.5) C38(0.5) H38(0.5) C39(0.5)
 H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5) C43(0.5) H43(0.5)
 C44(0.5) Cl1(0.5) Cl2(0.5) Cl3(0.5) C45(0.5) H45(0.5) Cl4(0.5) Cl5(0.5)
 Cl6(0.5) C46(0.5) H46(0.5)
3.a Ternary CH refined with riding coordinates:
 C45(H45), C46(H46)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C14A(H14A), C15(H15), C15A(H15A), C17(H17), C17A(H17A), C18(H18), C18A(H18A),
 C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C29(H29), C30(H30),
  C32(H32), C33(H33), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43)
;
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.834
_shelx_res_checksum              7663
_shelxl_version_number           2012-9