Photoinduced charge shift and charge recombination through an alkynyl spacer for an expanded acridinium-based dyad.
Benniston, Andrew C.; Hagon, Jerry; He, Xiaoyan; Lemmetyinen, Helge; Tkachenko, Nikolai V.; Clegg, William; Harrington, Ross W.; Physical chemistry chemical physics : PCCP 14 (2012) 3194–3199; doi:10.1039/c2cp23273a

data_7207311
_publ_section_title
;
 Photoinduced charge shift and charge recombination through an alkynyl
 spacer for an expanded acridinium-based dyad.
;
_journal_issue                   9
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              3194
_journal_page_last               3199
_journal_paper_doi               10.1039/c2cp23273a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C34 H20 N O S +,P F6 -,C2 H3 N'
_chemical_formula_sum            'C36 H23 F6 N2 O P S'
_chemical_formula_weight         676.59
_chemical_name_common
;
7-(Methylsulfinyl)-14-phenylbenzo(5,6)tetraceno(1,12,11,10-
jklmna)acridin-14-ium hexafluorophosphate(V), acetonitrile solvate
;
_chemical_name_systematic
;
7-(Methylsulfinyl)-14-phenylbenzo[5,6]tetraceno[1,12,11,10-jklmna]acridin-14-ium
hexafluorophosphate(V), acetonitrile solvate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.715(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.773(4)
_cell_length_b                   6.7999(18)
_cell_length_c                   15.291(4)
_cell_measurement_reflns_used    2863
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.53
_cell_volume                     1422.3(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10624
_diffrn_reflns_theta_full        23.54
_diffrn_reflns_theta_max         23.54
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         2705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0755
_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^)+(0.1474P)^2^+0.7861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2342
_reflns_number_gt                2070
_reflns_number_total             2705
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cp23273a.txt
_cod_data_source_block           acb24
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7207311
_computing_special_details
;
TITL acb24 in P2(1)/m
CELL 0.6709 13.773 6.7999 15.291 90.000 96.715 90.000
ZERR 2.00 0.004 0.0018 0.004 0.000 0.003 0.000
LATT 1
SYMM -X, 0.5+Y, -Z
SFAC C H N F P S O
DISP P 0.09297 0.08419 318.32
DISP S 0.11369 0.11037 417.30
UNIT 72 46 4 12 2 2 2

REM orange needle
SIZE 0.25 0.03 0.02
TEMP -153
SHEL 5.8 0.84

L.S. 8
ACTA
BOND $H
CONF
FMAP 2
PLAN 10

rem EXTI 0.010559 insignificant
WGHT 0.147400 0.786100
FVAR 0.40280
C1 1 0.462633 0.250000 0.529066 10.50000 0.03451 0.03045 =
0.04016 0.00000 0.01160 0.00000
C2 1 0.387230 0.250000 0.584243 10.50000 0.04302 0.03604 =
0.04007 0.00000 0.01758 0.00000
C3 1 0.412992 0.250000 0.676960 10.50000 0.04111 0.04834 =
0.04332 0.00000 0.02265 0.00000
AFIX 43
H3 2 0.362474 0.250000 0.714273 10.50000 -1.20000
AFIX 0
C4 1 0.507337 0.250000 0.713825 10.50000 0.05249 0.05787 =
0.02786 0.00000 0.01971 0.00000
AFIX 43
H4 2 0.522363 0.250000 0.776064 10.50000 -1.20000
AFIX 0
C5 1 0.583982 0.250000 0.658662 10.50000 0.03988 0.04404 =
0.03371 0.00000 0.01107 0.00000
C6 1 0.562058 0.250000 0.566995 10.50000 0.04208 0.03591 =
0.02828 0.00000 0.01489 0.00000
N7 3 0.679792 0.250000 0.695729 10.50000 0.04388 0.06115 =
0.02346 0.00000 0.01101 0.00000
C8 1 0.755925 0.250000 0.645276 10.50000 0.03868 0.05331 =
0.03110 0.00000 0.01082 0.00000
C9 1 0.736198 0.250000 0.553127 10.50000 0.03973 0.04185 =
0.02822 0.00000 0.01309 0.00000
C10 1 0.638288 0.250000 0.512784 10.50000 0.03371 0.03256 =
0.03266 0.00000 0.01055 0.00000
C11 1 0.854157 0.250000 0.685645 10.50000 0.04939 0.08375 =
0.02601 0.00000 0.00738 0.00000
AFIX 43
H11 2 0.867733 0.250000 0.748004 10.50000 -1.20000
AFIX 0
C12 1 0.927997 0.250000 0.635170 10.50000 0.03639 0.09390 =
0.03716 0.00000 0.00763 0.00000
AFIX 43
H12 2 0.993362 0.250000 0.663053 10.50000 -1.20000
AFIX 0
C13 1 0.911587 0.250000 0.541611 10.50000 0.04368 0.06833 =
0.03798 0.00000 0.01492 0.00000
C14 1 0.814676 0.250000 0.499427 10.50000 0.03892 0.04274 =
0.03411 0.00000 0.01491 0.00000
C15 1 0.796037 0.250000 0.407605 10.50000 0.04244 0.04171 =
0.03313 0.00000 0.01443 0.00000
C16 1 0.695184 0.250000 0.365790 10.50000 0.04114 0.03897 =
0.03131 0.00000 0.01291 0.00000
C17 1 0.617509 0.250000 0.419566 10.50000 0.04312 0.03508 =
0.02788 0.00000 0.01270 0.00000
C18 1 0.518606 0.250000 0.380634 10.50000 0.03743 0.04091 =
0.03551 0.00000 0.00818 0.00000
C19 1 0.439269 0.250000 0.436798 10.50000 0.04161 0.03544 =
0.03489 0.00000 0.01026 0.00000
C20 1 0.988201 0.250000 0.491035 10.50000 0.03379 0.09927 =
0.04793 0.00000 0.01662 0.00000
AFIX 43
H20 2 1.053678 0.250000 0.518647 10.50000 -1.20000
AFIX 0
C21 1 0.969816 0.250000 0.400272 10.50000 0.04142 0.09935 =
0.03880 0.00000 0.02073 0.00000
AFIX 43
H21 2 1.023041 0.250000 0.365965 10.50000 -1.20000
AFIX 0
C22 1 0.875751 0.250000 0.358829 10.50000 0.04365 0.06133 =
0.03588 0.00000 0.01843 0.00000
AFIX 43
H22 2 0.864780 0.250000 0.296325 10.50000 -1.20000
AFIX 0
C23 1 0.341653 0.250000 0.402658 10.50000 0.04040 0.04472 =
0.04158 0.00000 0.00850 0.00000
AFIX 43
H23 2 0.324903 0.250000 0.340600 10.50000 -1.20000
AFIX 0
C24 1 0.267395 0.250000 0.457204 10.50000 0.03679 0.04769 =
0.04867 0.00000 0.00954 0.00000
AFIX 43
H24 2 0.201022 0.250000 0.431921 10.50000 -1.20000
AFIX 0
C25 1 0.289145 0.250000 0.546835 10.50000 0.03833 0.03988 =
0.05330 0.00000 0.02075 0.00000
AFIX 43
H25 2 0.238107 0.250000 0.583596 10.50000 -1.20000
AFIX 0
C26 1 0.672383 0.250000 0.275491 10.50000 0.04804 0.06689 =
0.03146 0.00000 0.01595 0.00000
AFIX 43
H26 2 0.723271 0.250000 0.238570 10.50000 -1.20000
AFIX 0
C27 1 0.576950 0.250000 0.238862 10.50000 0.04573 0.09755 =
0.02960 0.00000 0.00985 0.00000
C28 1 0.500936 0.250000 0.289731 10.50000 0.04213 0.09568 =
0.03284 0.00000 0.00580 0.00000
AFIX 43
H28 2 0.435477 0.250000 0.262075 10.50000 -1.20000
AFIX 0
C29 1 0.702107 0.250000 0.791505 10.50000 0.04271 0.08446 =
0.02752 0.00000 0.01091 0.00000
C30 1 0.713560 0.423321 0.835412 11.00000 0.09244 0.10916 =
0.03469 -0.01591 0.01551 -0.03268
AFIX 43
H30 2 0.704983 0.544194 0.804314 11.00000 -1.20000
AFIX 0
C31 1 0.737675 0.422832 0.925256 11.00000 0.11474 0.15390 =
0.03463 -0.02165 0.01575 -0.04957
AFIX 43
H31 2 0.745912 0.543501 0.956554 11.00000 -1.20000
AFIX 0
C32 1 0.749615 0.250000 0.968876 10.50000 0.06259 0.18996 =
0.02857 0.00000 0.01184 0.00000
AFIX 43
H32 2 0.766596 0.250002 1.030907 10.50000 -1.20000
AFIX 0
PART -1
S33 6 0.549165 0.186551 0.122373 10.50000 0.06154 0.11500 =
0.02471 -0.00712 0.00698 -0.01075
O34 7 0.444736 0.151206 0.106839 10.50000 0.08337 0.26035 =
0.03582 -0.02005 0.01058 -0.04231
C35 1 0.569351 0.437824 0.089222 10.50000 0.11380 0.10543 =
0.03424 0.02932 0.02888 0.02052
AFIX 33
H35A 2 0.558963 0.447254 0.024854 10.50000 -1.50000
H35B 2 0.636527 0.476873 0.110261 10.50000 -1.50000
H35C 2 0.523476 0.525177 0.114631 10.50000 -1.50000
AFIX 0
PART 0
N36 3 0.134681 0.250000 1.243817 10.50000 0.06919 0.09957 =
0.05088 0.00000 0.02383 0.00000
C37 1 0.083377 0.250000 1.180555 10.50000 0.05859 0.09290 =
0.04914 0.00000 0.03045 0.00000
C38 1 0.017268 0.250000 1.098361 10.50000 0.07751 0.14096 =
0.04844 0.00000 0.02062 0.00000
AFIX 33
H38A 2 -0.050596 0.250000 1.111761 10.50000 -1.20000
H38B 2 0.029061 0.132327 1.064137 10.50000 -1.20000
H38C 2 0.029061 0.367673 1.064137 10.50000 -1.20000
AFIX 0
P 5 0.161122 0.250000 0.831546 10.50000 0.05392 0.08979 =
0.02261 0.00000 0.01309 0.00000
F1 4 0.165061 0.478498 0.833790 11.00000 0.21236 0.09527 =
0.11973 0.02534 0.09153 0.01152
F2 4 0.048111 0.250000 0.818163 10.50000 0.04938 0.32157 =
0.04212 0.00000 0.00825 0.00000
F3 4 0.275952 0.250000 0.845492 10.50000 0.06279 0.25283 =
0.05434 0.00000 0.01115 0.00000
F4 4 0.167192 0.250000 0.729017 10.50000 0.06979 0.22949 =
0.02289 0.00000 0.01943 0.00000
F5 4 0.156515 0.250000 0.934150 10.50000 0.09514 0.13060 =
0.02517 0.00000 0.01833 0.00000

HKLF 4

REM acb24 in P2(1)/m
REM R1 = 0.0755 for 2070 Fo > 4sig(Fo) and 0.0909 for all 2705 data
REM 283 parameters refined using 0 restraints

END

;