Hydrogen bonded anion ribbons, networks and clusters and sulfur-anion interactions in novel radical cation salts of BEDT-TTF with sulfamate, pentaborate and bromide.
Brooks, Andrew C.; Martin, Lee; Day, Peter; Lopes, Elsa B.; Almeida, Manuel; Kikuchi, Koichi; Fujita, Wataru; Sasamori, Kota; Aktusu, Hiroki; Wallis, John D.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 6645–6654; doi:10.1039/c3dt32430c

data_7022630
_publ_section_title
;
 Hydrogen bonded anion ribbons, networks and clusters and sulfur-anion
 interactions in novel radical cation salts of BEDT-TTF with sulfamate,
 pentaborate and bromide.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6645
_journal_page_last               6654
_journal_paper_doi               10.1039/c3dt32430c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         '5(C10 H8 S8), 4(Br), (H2 O), (H3 O)'
_chemical_formula_sum            'C50 H45 Br4 O2 S40'
_chemical_formula_weight         2280.11
_chemical_melting_point          482
_chemical_name_systematic
;
Penta-bis(ethylenedithio)tetrathiafulvalene tetrabromide
hydroxonium hydrate
;
_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_method           SHELXL-97
_cell_angle_alpha                75.8770(10)
_cell_angle_beta                 89.9950(10)
_cell_angle_gamma                72.0850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1312(2)
_cell_length_b                   18.0651(4)
_cell_length_c                   20.7862(4)
_cell_measurement_reflns_used    102788
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3844.19(14)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62725
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    3.223
_exptl_absorpt_correction_T_max  0.7826
_exptl_absorpt_correction_T_min  0.6794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut slab'
_exptl_crystal_F_000             2282
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         17616
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+16.7542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                15225
_reflns_number_total             17619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32430c.txt
_cod_data_source_block           etbrbig
_cod_original_cell_volume        3844.19(13)
_cod_database_code               7022630