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_4120381
_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, C36 H44 O10, 4(F6 P), 8(C2 H3 N)'
_chemical_formula_sum            'C112 H116 F24 N12 O10 P4'
_chemical_formula_weight         2370.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2012-11-29
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                88.5705(13)
_cell_angle_beta                 86.4287(12)
_cell_angle_gamma                72.7606(11)
_cell_formula_units_Z            1
_cell_length_a                   10.8213(3)
_cell_length_b                   13.5278(3)
_cell_length_c                   21.9030(6)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.71
_cell_measurement_theta_min      4.63
_cell_volume                     3056.28(14)
_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, Beta test 
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Kappa 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  0.0241
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24907
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        64.990
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         4.28
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0583 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.7833.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         10092
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+1.7686P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8836
_reflns_number_total             10092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_014.cif
_cod_data_source_block           n2216
_cod_database_code               4120381
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H15A of C15A, H14A of C14A, H18A of C18A, H17A of C17A, H26 of C26, H27 of
  C27, H29 of C29, H30 of C30, H32 of C32, H33 of C33, H34 of C34, H37 of C37,
  H38 of C38, H39 of C39, {H41A,H41B} of C41, {H42A,H42B,H42C,H42D} of C42,
  {H43A,H43B} of C43, {H44A,H44B} of C44, {H45A,H45B} of C45, {H46A,H46B,H46C,
  H46D} of C46, {H1A,H1B} of C1, H2 of C2, H3 of C3, H5 of C5, H6 of C6, H8 of
  C8, H9 of C9, H11 of C11, H12 of C12, H14 of C14, H15 of C15, H17 of C17, H18
  of C18, H20 of C20, H21 of C21, H22 of C22, H23 of C23, {H24A,H24B} of C24,
  {H45C,H45D} of C45A, {H44C,H44D} of C44A, {H43C,H43D} of C43A, {H48A,H48B} of
  C48, {H47A,H47B} of C47
 At 1.5 times of:
  {H56A,H56B,H56C} of C56, {H54A,H54B,H54C} of C54, {H52A,H52B,H52C} of C52,
  {H50A,H50B,H50C} of C50
2. Restrained distances
 O2A-C42 ~ O2-C42 ~ O2A-C43A ~ O2-C43 ~ O3-C44 ~ O3A-C44A ~ O3-C45 ~ O3A-C45A
 with sigma of 0.02
 C44-C43 ~ C44A-C43A ~ C46-C45A ~ C46-C45
 with sigma of 0.02
 C43-O3 ~ C43A-O3A ~ C45A-O4 ~ C45-O4
 with sigma of 0.02
 C44A-C45A ~ C44-C45 ~ C43A-C42 ~ C43-C42
 with sigma of 0.02
3. others
 Sof(O2)=Sof(O3)=Sof(H42A)=Sof(H42B)=1-Sof(O3)=1-Sof(O3)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H46A)=
 Sof(H46B)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-
 Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)=1-Sof(O3)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=1-
 Sof(H14)=1-Sof(H14)=1-Sof(H14)=1-Sof(H14)=1-Sof(H14)=1-Sof(H14)=1-Sof(H14)=1-
 Sof(H14)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C24(H24A,H24B), C41(H41A,H41B), C42(H42A,H42B), C42(H42C,H42D),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C46(H46C,H46D),
  C47(H47A,H47B), C48(H48A,H48B), C43A(H43C,H43D), C44A(H44C,H44D), C45A(H45C,
 H45D)
4.b Me refined with riding coordinates:
 C56(H56A,H56B,H56C)
4.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),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C37(H37),
 C38(H38), C39(H39), C15A(H15A), C14A(H14A), C18A(H18A), C17A(H17A)
4.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_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 model are
reported in the formula here.

Total solvent accessible volume / cell = 312.6 Ang^3^ [10.2%]
Total electron count / cell = 39.1
;
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.561
_shelx_res_checksum              75417
_shelxl_version_number           2012-6