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_4119145
_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, C18 H12, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C70 H58 F24 N6 P4'
_chemical_formula_weight         1563.10
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-03
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
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_cell_angle_alpha                72.955(4)
_cell_angle_beta                 82.376(5)
_cell_angle_gamma                63.569(4)
_cell_formula_units_Z            1
_cell_length_a                   10.5607(6)
_cell_length_b                   11.1014(6)
_cell_length_c                   18.0247(11)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.46
_cell_measurement_theta_min      4.65
_cell_volume                     1809.17(19)
_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
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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_structure_refinement
;
XL, 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(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker Kappa APEX2 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  0.0343
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9232
_diffrn_reflns_theta_full        62.03
_diffrn_reflns_theta_max         62.03
_diffrn_reflns_theta_min         4.65
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.926
_exptl_absorpt_correction_T_max  0.7521
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0529 before and 0.0380 after correction.
The Ratio of minimum to maximum transmission is 0.8592.
The \l/2 correction factor is 0.0015.
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.444
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     605
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      1.453
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.1251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3593
_refine_ls_wR_factor_ref         0.3872
_reflns_number_gt                3407
_reflns_number_total             5453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307360n_si_010.cif
_cod_data_source_block           n1983b
_cod_original_cell_volume        1809.18(18)
_cod_database_code               4119145
_smtbx_masks_special_details
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The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 149.4 Ang^3^ [8.3%]
Total electron count / cell = 7.2

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