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_4120370
_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, 2(C2 H3 N), 1.5(C14 H10), 4(F6 P)'
_chemical_formula_sum            'C85 H69 F24 N6 P4'
_chemical_formula_weight         1754.34
_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
_audit_creation_date             2012-10-25
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                77.9314(18)
_cell_angle_beta                 85.6033(18)
_cell_angle_gamma                65.5596(16)
_cell_formula_units_Z            1
_cell_length_a                   10.0609(3)
_cell_length_b                   11.2203(4)
_cell_length_c                   21.7538(7)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.22
_cell_volume                     2186.11(13)
_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 
;
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59360
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.255
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0643 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.8059.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             897
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12946
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1601P)^2^+2.5359P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.2967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8548
_reflns_number_total             12946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4052763_si_003.cif
_cod_data_source_block           n2247
_cod_database_code               4120370
_refinement_special_details
;

 Distance restraints were refined for the disordered anthracene.
 A group anistropic displacement parameter was refined for the
 disordered anthracene. It was also restrained esd (0.01) that its
 Uij components approximate to isotropic. The enhanced rigid-bond
 restraint (SHELX keyword RIGU) was applied to the disordered
 fluorine atoms and anthracene. (Acta Cryst. A68 (2012) 448-451).
 The highest peaks in the difference map were located around the
 disordered anthracene indicating some more possible disorder.
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.955
_shelx_res_checksum              68305
_shelxl_version_number           2012-6