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_7022627
_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         '3(C10 H8 S8), 2(H2 N O3 S), 2(H2 O)'
_chemical_formula_sum            'C30 H32 N2 O8 S26'
_chemical_formula_weight         1382.14
_chemical_melting_point          491
_chemical_name_common            ET3(H2NSO3)2.2H2O
_chemical_name_systematic
;
Tris(bis(ethylenedithio)tetrathiafulvalene) bis(sulfamate) dihydrate
;
_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                90.0380(10)
_cell_angle_beta                 93.6690(10)
_cell_angle_gamma                96.9530(10)
_cell_formula_units_Z            1
_cell_length_a                   6.57440(10)
_cell_length_b                   11.5052(3)
_cell_length_c                   16.3531(4)
_cell_measurement_reflns_used    15400
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1225.29(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.982
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20949
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.7644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0335
_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^+2.2975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                4944
_reflns_number_total             5602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32430c.txt
_cod_data_source_block           c:\xraydata\etsulf\1081
_cod_database_code               7022627