Thia-bridged triarylamine heterohelicene radical cations as redox-driven molecular switches
S. Menichetti; S. Cecchi; P. Procacci; M. Innocenti; L. Becucci; L. Franco; C. Viglianisi; Chem.Commun. 51 (2015) 11452–; doi:10.1039/C5cc04007H

data_7117423
_publ_section_title
;
 Thia-bridged triarylamine heterohelicene radical cations as redox-driven
 molecular switches
;
_journal_name_full               Chem.Commun.
_journal_page_first              11452
_journal_paper_doi               10.1039/C5cc04007H
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C22 H19 Cl2 F6 N O3 S2 Sb'
_chemical_formula_sum            'C22 H19 Cl2 F6 N O3 S2 Sb'
_chemical_formula_weight         716.15
_chemical_name_systematic
;
2,3,4-trimethoxybenzo[5,6][1,4]thiazino[2,3,4-kl]phenothiazinyl
hexafluoroantimonate, free radical
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
;
'Wed May 09 15:26:04 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_audit_update_record
;
2013-03-27 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                102.819(5)
_cell_angle_beta                 97.906(4)
_cell_angle_gamma                112.771(5)
_cell_formula_units_Z            2
_cell_length_a                   9.106(1)
_cell_length_b                   10.580(1)
_cell_length_c                   15.856(1)
_cell_measurement_reflns_used    3037
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      61.7253
_cell_measurement_theta_min      4.7500
_cell_volume                     1330.3(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    Ortep3
_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 J.Appl.Cryst.38,381-388'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
1 omega -25.00 62.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.4688 77.0000 0.0000 87

2 omega -75.00 -35.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.4688 179.0000 90.0000 40

3 omega 34.00 70.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.4688 37.0000 -90.0000 36

4 omega -121.00 -90.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -77.8666 125.0000 -90.0000 31

5 omega -37.00 -6.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -77.8666 125.0000 -90.0000 31

6 omega -33.00 -7.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -77.8666 77.0000 -120.0000 26

7 omega -103.00 -55.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- -77.8666 77.0000 -120.0000 48

8 omega 46.00 71.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -37.0000 30.0000 25

9 omega 75.00 143.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 37.0000 -150.0000 68

10 omega 15.00 70.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -37.0000 90.0000 55

11 omega 15.00 96.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -77.0000 -60.0000 81

12 omega 16.00 80.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -77.0000 -120.0000 64

13 omega 14.00 109.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -77.0000 30.0000 95

14 omega 13.00 67.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 -37.0000 -60.0000 54

15 omega 76.00 150.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ frames
- 78.8041 37.0000 90.0000 74
;
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7657
_diffrn_reflns_theta_full        61.82
_diffrn_reflns_theta_max         61.82
_diffrn_reflns_theta_min         4.75
_diffrn_standards_decay_%        50
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.175
_exptl_absorpt_correction_T_max  0.6145
_exptl_absorpt_correction_T_min  0.3776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            darkviolet
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1219P)^2^+1.2492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                2857
_reflns_number_total             4050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc04007h2.cif
_cod_data_source_block           exp_711
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7117423