Structural Transitions from Triangular to Square Molecular Arrangements in the Quasi-One-Dimensional Molecular Conductors (DMEDO-TTF)2XF6 (X = P, As, and Sb)
Takashi Shirahata; Keita Shiratori; Shouhei Kumeta; Tadashi Kawamoto; Tadahiko Ishikawa; Shin-ya Koshihara; Yoshiaki Nakano; Hideki Yamochi; Misaki, Yohji; Takehiko Mori; Journal of the American Chemical Society 134 (2012) 13330–13340; doi:10.1021/ja303435n

data_4118501
_publ_contact_author_address
;
Department of Applied Chemistry, 
Graduate School of Science and Engineering, 
Ehime University, 
3 Bunkyo-cho, Matsuyama 790-8577, Japan
;
_publ_contact_author_email       shirahata.takashi.mj@ehime-u.ac.jp
_publ_contact_author_fax         +81-89-927-9922
_publ_contact_author_name        'Dr Takashi Shirahata'
_publ_contact_author_phone       +81-89-927-8537
_publ_section_title
;
 Structural Transitions from Triangular to Square Molecular Arrangements
 in the Quasi-One-Dimensional Molecular Conductors (DMEDO-TTF)2XF6 (X = P,
 As, and Sb)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13330
_journal_page_last               13340
_journal_paper_doi               10.1021/ja303435n
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C10 H10 O2 S4'
_chemical_formula_weight         290.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.853(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.462(12)
_cell_length_b                   8.271(7)
_cell_length_c                   11.139(10)
_cell_measurement_reflns_used    3524
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.13
_cell_volume                     1159.0(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13621
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.4661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                2279
_reflns_number_total             2649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303435n_si_002_2.cif
_cod_data_source_block           DMEDO-TTF
_cod_database_code               4118501