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_4120369
_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, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C64 H54 F24 N6 P4'
_chemical_formula_weight         1487.01
_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             2012-08-30
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.579(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.2776(8)
_cell_length_b                   12.0433(5)
_cell_length_c                   14.5105(7)
_cell_measurement_reflns_used    1946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.268
_cell_measurement_theta_min      4.332
_cell_volume                     3358.9(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
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, 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 0.915
_diffrn_measured_fraction_theta_max 0.973
_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_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5570
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.105
_diffrn_reflns_theta_min         2.299
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.582718
_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 0.0721 before and 0.0501 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 0.0777 before and 0.0535 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0653P)^2^+0.3527P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4166
_reflns_number_total             5570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_002.cif
_cod_data_source_block           n2110
_cod_database_code               4120369
_diffrn_reflns_sigmai/neti       0.0489
_refinement_special_details
;
?

 The crystal under investigation was found to be non-merohedrally twinned. 
 The orientation matrices for the two components were identified using the 
 program Cell_Now (Sheldrick, 2005), and the data were processed using both 
 orientation matrices with SAINT, The exact twin matrix identified 
 by the integration program was found to be 
    -0.99975 -0.00027  0.00057
     0.00013 -1.00000 -0.00012
     0.89137 -0.00018  0.99975
 The second domain is rotated from first domain by 180 \% about the reciprocal 
 lattice c axis (non-standard setting). The absorption correction was carried
 out using TWINABS V2008/4 (Sheldrick, 2008) to create an hklf5 file which was
 used in all refinements; the structure was solved using direct methods with
 only the non-overlapping reflections of component 1. The twin fraction refined
 to a value of 0.4162(15).
;
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.714
_shelx_res_checksum              55334
_shelxl_version_number           2012-4