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_4119137
_publ_contact_author_name
;
;
_publ_section_title
;
 ExBox: A Polycyclic Aromatic Hydrocarbon Scavenger
;
_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, 4(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C54 H49 F24 N7 P4'
_chemical_formula_weight         1375.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-12
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.513(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.9198(6)
_cell_length_b                   16.2998(5)
_cell_length_c                   36.9045(11)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.29
_cell_measurement_theta_min      4.43
_cell_volume                     13040.3(7)
_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
;
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  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            52258
_diffrn_reflns_theta_full        64.89
_diffrn_reflns_theta_max         64.89
_diffrn_reflns_theta_min         4.08
_diffrn_source                   microsource
_diffrn_source_current           0.64
_diffrn_source_power             0.0286144
_diffrn_source_voltage           44.71
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0730 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8635.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         10885
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1540P)^2^+30.7509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                8470
_reflns_number_total             10885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307360n_si_002.cif
_cod_data_source_block           n1659
_cod_database_code               4119137
_smtbx_masks_special_details
;
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 = 1880.4 Ang^3^ [14.4%]
Total electron count / cell = 184.6
;