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_4120377
_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, 0.5(C14 H8 O2), 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C69 H55 F24 N5 O P4'
_chemical_formula_weight         1550.06
_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     dual
_audit_creation_date             2012-11-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.223(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.0817(7)
_cell_length_b                   12.1032(4)
_cell_length_c                   14.4581(6)
_cell_measurement_reflns_used    3610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.13
_cell_measurement_theta_min      4.31
_cell_volume                     3374.2(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
;
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
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.673
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.673
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4115
_diffrn_reflns_point_group_measured_fraction_full 0.673
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         54.217
_diffrn_reflns_theta_min         2.291
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.067
_exptl_absorpt_correction_T_max  0.750698
_exptl_absorpt_correction_T_min  0.524051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1046 before and 0.0682 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1012 before and 0.0678 after correction.
 The Ratio of minimum to maximum transmission is 0.70.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         4115
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0994P)^2^+4.4386P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             4115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_010.cif
_cod_data_source_block           n2295
_cod_database_code               4120377
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H13 of C13, H14 of C14, H15 of C15, H34 of C34, H33 of C33, {H30A,H30B} of
  C30, H29 of C29, H28 of C28, H26 of C26, H25 of C25, {H23A,H23B} of C23, H22
  of C22, H21 of C21, H20 of C20, H19 of C19, H17 of C17, H35 of C35, H36 of
  C36, H11 of C11, H10 of C10, H8 of C8, H7 of C7, H5 of C5, H4 of C4, H2 of C2,
   H1 of C1
 At 1.5 times of:
  {H2SA,H2SB,H2SC} of C2S
2. others
 Fixed Sof: O1(0.5) C31(0.5) C32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) N1S(0.5) C1S(0.5) C2S(0.5)
 H2SA(0.5) H2SB(0.5) H2SC(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36)
3.c Fitted hexagon refined as free rotating group:
 C32(C33,C34,C35,C36,C37)
3.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.900
_shelx_res_checksum              29865
_shelxl_version_number           2012-6