ExBox: A Polycyclic Aromatic Hydrocarbon Scavenger
Jonathan C. Barnes; Michal Juríček; Nathan L. Strutt; Marco Frasconi; Srinivasan Sampath; Marc A. Giesener; Psaras L. McGrier; Carson J. Bruns; Charlotte L. Stern; Amy A. Sarjeant; J. Fraser Stoddart; Journal of the American Chemical Society 135 (2013) 183–192; doi:10.1021/ja307360n

data_4119138
_publ_contact_author_name
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;
_publ_section_title
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 ExBox: A Polycyclic Aromatic Hydrocarbon Scavenger
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              183
_journal_page_last               192
_journal_paper_doi               10.1021/ja307360n
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C48 H40 N4, 2(C10 H8), 4(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C74 H65 F24 N7 P4'
_chemical_formula_weight         1632.21
_chemical_name_systematic
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 ? 
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_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-21
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                71.6940(10)
_cell_angle_beta                 79.4480(10)
_cell_angle_gamma                65.8100(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0901(3)
_cell_length_b                   11.3816(3)
_cell_length_c                   18.0816(5)
_cell_measurement_reflns_used    9361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.90
_cell_measurement_theta_min      4.42
_cell_volume                     1794.77(9)
_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
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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
;
XL, 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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43173
_diffrn_reflns_theta_full        67.91
_diffrn_reflns_theta_max         67.91
_diffrn_reflns_theta_min         4.42
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0946 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.8689.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         6433
_refine_ls_number_restraints     687
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+2.0278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                6205
_reflns_number_total             6433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307360n_si_003.cif
_cod_data_source_block           n1844
_cod_database_code               4119138
_refinement_special_details
;
The two azulene molecules were disordered over symmetry positions and refined 
with PART -1 commands. The 1,2 C-C distances were refined with similarity 
restraints (SADI) as well as the 1,3 distances for the 8-membered ring carbons 
only. Each azulene was subjected to a flat restraint and displacement 
parameters for the carbon atoms were subjected to rigid bond (DELU) and 
similarity (SIMU) restraints. The disordered PF6 anions were refined with SADI 
restraints to regularize the environment around each P atom, and with rigid 
bond and similarity restraints on all atoms. The N-C, N-Me and C-C bond 
distances on the acetonitrile molecules were refined with similarity restraints
(SADI). All atoms of the disordered MeCN molecule were refined with global 
anisotropic displacement parameters.
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