Mixed valence radical cations and intermolecular complexes derived from indenofluorene-extended tetrathiafulvalenes
Mikkel A. Christensen; Christian R. Parker; Thomas Just Sorensen; Sebastian de Graaf; Thorbjorn J. Morsing; Theis Brock-Nannestad; Jesper Bendix; Michael M. Haley; Peter Rapta; Andrey Danilov; Sergey Kubatkin; Ole Hammerich; Mogens Brondsted Nielsen; Journal of Materials Chemistry C 2 (2014) 10428–10438; doi:10.1039/C4TC02178A

data_7233949
_publ_section_title
;
 Mixed valence radical cations and intermolecular complexes derived from
 indenofluorene-extended tetrathiafulvalenes
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10428
_journal_page_last               10438
_journal_paper_doi               10.1039/C4TC02178A
_journal_volume                  2
_journal_year                    2014
_chemical_formula_moiety         'C34 H30 S8'
_chemical_formula_sum            'C34 H30 S8'
_chemical_formula_weight         695.14
_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_Int_Tables_number      15
_cell_angle_alpha                90
_cell_angle_beta                 104.828(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.306(3)
_cell_length_b                   24.770(3)
_cell_length_c                   6.7903(6)
_cell_measurement_reflns_used    2054
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.39
_cell_volume                     3952.0(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            15137
_diffrn_reflns_theta_full        22.7174
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0866 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.8210.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_density_diffrn    1.1682
_exptl_crystal_F_000             1452.3322
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.7960
_refine_diff_density_min         -0.5534
_refine_diff_density_rms         0.1507
_refine_ls_d_res_high            0.9202
_refine_ls_d_res_low             8.5236
_refine_ls_goodness_of_fit_ref   1.0265
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.0257
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1864P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2443
_refine_ls_wR_factor_ref         0.2860
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              -26
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                1562
_reflns_number_total             2661
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            1000003.cif
_cod_data_source_block           PCOD1000003
_cod_original_cell_volume        3952.1(7)
_cod_database_code               7233949
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S4-C16a \\sim S4-C16b
 with sigma of 0.02
 C16a-C18 \\sim C16b-C18
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C16a)
5. Others
 Sof(H18d)=Sof(H18e)=Sof(H18f)=Sof(C16b)=Sof(H16c)=Sof(H16d)=1-FVAR(1)
 Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(C16a)=Sof(H16a)=Sof(H16b)=FVAR(1)
6.a Riding coordinates:
 C18(H18a,H18b,H18c), C18(H18d,H18e,H18f), C15(H15a,H15b,H15c)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C16a(H16a,H16b), C16b(H16c,H16d)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C2(H2), C7(H7), C8(H8), C9(H9)
;