Solid-state characterization and photoinduced intramolecular electron transfer in a nanoconfined octacationic homo[2]catenane.
Barnes, Jonathan C.; Frasconi, Marco; Young, Ryan M.; Khdary, Nezar H.; Liu, Wei-Guang; Dyar, Scott M.; McGonigal, Paul R.; Gibbs-Hall, Ian C; Diercks, Christian S.; Sarjeant, Amy A.; Stern, Charlotte L.; Goddard, 3rd, William A; Wasielewski, Michael R.; Stoddart, J. Fraser; Journal of the American Chemical Society 136 (2014) 10569–10572; doi:10.1021/ja505093d

data_4122296
_publ_section_title
;
 Solid-state characterization and photoinduced intramolecular electron
 transfer in a nanoconfined octacationic homo[2]catenane.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10569
_journal_page_last               10572
_journal_paper_doi               10.1021/ja505093d
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         '4(F6 Sb), C36 H32 N4, 4.5(C2 H3 N)'
_chemical_formula_sum            'C45 H45.5 F24 N8.5 Sb4'
_chemical_formula_weight         1648.39
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2014-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                86.675(2)
_cell_angle_beta                 78.450(2)
_cell_angle_gamma                71.512(2)
_cell_formula_units_Z            4
_cell_length_a                   16.4947(7)
_cell_length_b                   16.7464(7)
_cell_length_c                   22.8838(10)
_cell_measurement_reflns_used    9235
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.069
_cell_measurement_theta_min      2.783
_cell_volume                     5873.4(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79636
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.311
_diffrn_reflns_theta_min         1.970
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.493
_exptl_absorpt_correction_T_max  0.5691
_exptl_absorpt_correction_T_min  0.4139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0856 after correction.
The Ratio of minimum to maximum transmission is 0.7273.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.054
_refine_diff_density_max         7.768
_refine_diff_density_min         -4.300
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1476
_refine_ls_number_reflns         21245
_refine_ls_number_restraints     1245
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0886
_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^)+(0.1421P)^2^+53.9480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17450
_reflns_number_total             21245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505093d_si_002.cif
_cod_data_source_block           n3176g
_cod_depositor_comments          'Adding full bibliography for 4122296.cif.'
_cod_database_code               4122296
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.254
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C29(H29A,H29B), C36(H36A,H36B), C47(H47A,
 H47B), C54(H54A,H54B), C65(H65A,H65B), C72(H72A,H72B)
3.b Me refined with riding coordinates:
 C12S(H12A,H12B,H12C)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35),
 C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
  C49(H49), C50(H50), C52(H52), C53(H53), C55(H55), C56(H56), C58(H58),
 C59(H59), C61(H61), C62(H62), C63(H63), C64(H64), C67(H67), C68(H68), C70(H70),
  C71(H71)
3.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,
 H8SC), C10S(H10A,H10B,H10C), C14S(H14A,H14B,H14C), C16S(H16A,H16B,H16C),
 C18S(H18C,H18D,H18E)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of disordered and partially occupied acetonitrile 
solvent molecules from the refinement.  

Total solvent accessible volume / cell = 341.5 Ang^3^ [5.8%]
Total electron count / cell = 95.1
;
_shelx_res_checksum              33507
_shelx_hkl_checksum              45271