Tuning the size of a redox-active tetrathiafulvalene-based self-assembled ring.
Bivaud, Sébastien; Goeb, Sébastien; Croué, Vincent; Allain, Magali; Pop, Flavia; Sallé, Marc; Beilstein journal of organic chemistry 11 (2015) 966–971; doi:10.3762/bjoc.11.108

data_4031095
_publ_section_title
;
 Tuning the size of a redox-active tetrathiafulvalene-based self-assembled
 ring.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              966
_journal_page_last               971
_journal_paper_doi               10.3762/bjoc.11.108
_journal_volume                  11
_journal_year                    2015
_chemical_formula_moiety         'C132 H120 N24 Pd6 S12, 4(CF3SO3)'
_chemical_formula_sum            'C136 H120 F12 N24 O12 Pd6 S16'
_chemical_formula_weight         3661.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-06T11:49:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.391(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4015(2)
_cell_length_b                   34.9475(2)
_cell_length_c                   39.9599(4)
_cell_measurement_reflns_used    151068
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.091
_cell_measurement_theta_min      1.46
_cell_volume                     32670.5(5)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, V1.171.36.28'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, V1.171.36.28'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, V1.171.36.28'
_computing_molecular_graphics    'DIAMOND 3.2i (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.293
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67
_diffrn_reflns_av_R_equivalents  0.1101
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            701627
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The unit cell contains anions and solvent molecules which were not
 modelled but the corresponding scattering contribution were taken into account
 using SQUEEZE/PLATON procedure. The unit cell contains 1 void of 20881 A3
 containing about 8104 electrons from which 2336 electrons can be attributed to
 the 32 missing CF3SO3 anions in the unit cell. The others 5768 electrons can be
  attributed to solvent molecules. As the solvent composition is not well known,
 it has not been included in the calculation of the empirical formula, formula
 weight, density, linear absorption coefficient and F(000).
;
_refine_diff_density_max         2.823
_refine_diff_density_min         -1.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1855
_refine_ls_number_reflns         62714
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1919P)^2^+14.1335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2636
_refine_ls_wR_factor_ref         0.2787
_reflns_number_gt                49042
_reflns_number_total             62714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-11-108-S2.cif
_cod_data_source_block           squeezed
_cod_depositor_comments          'Adding full bibliography for 4031095.cif.'
_cod_database_code               4031095