Tetrathiafulvalene Hetero Radical Cation Dimerization in a Redox-Active [2]Catenane
Cheng Wang; Scott M. Dyar; Dennis Cao; Albert C. Fahrenbach; Noah Horwitz; Michael T. Colvin; Raanan Carmieli; Charlotte L. Stern; Sanjeev K. Dey; Michael R. Wasielewski; J. Fraser Stoddart; Journal of the American Chemical Society 134 (2012) 19136–19145; doi:10.1021/ja307577t

data_4118912
_publ_section_title
;
 Tetrathiafulvalene Hetero Radical Cation Dimerization in a Redox-Active
 [2]Catenane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19136
_journal_page_last               19145
_journal_paper_doi               10.1021/ja307577t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C74 H80 F24 N8 O8 P4 S10'
_chemical_formula_weight         2109.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.671(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1794(18)
_cell_length_b                   13.6101(10)
_cell_length_c                   29.949(2)
_cell_measurement_reflns_used    6940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.28
_cell_measurement_theta_min      2.97
_cell_volume                     8979.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32165
_diffrn_reflns_theta_full        67.27
_diffrn_reflns_theta_max         67.27
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    3.906
_exptl_absorpt_correction_T_max  0.6078
_exptl_absorpt_correction_T_min  0.2763
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.507
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1173P)^2^+79.9861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2291
_refine_ls_wR_factor_ref         0.2401
_reflns_number_gt                6416
_reflns_number_total             7626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307577t_si_001.cif
_cod_data_source_block           n0305
_cod_original_cell_volume        8979.4(12)
_cod_database_code               4118912