Chiral Semiconductor Phases: The Optically Pure D3[MIII(S,S-EDDS)]2 (D = TTF, TSF) Family
Nikola Paul Chmel; Guy J. Clarkson; Alessandro Troisi; Scott S. Turner; Peter Scott; Inorganic Chemistry 50 (2011) 4039–4046; doi:10.1021/ic102522k

data_4324962
_publ_section_title
;
 Chiral Semiconductor Phases: The Optically Pure D3[MIII(S,S-EDDS)]2 (D =
 TTF, TSF) Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4039
_journal_page_last               4046
_journal_paper_doi               10.1021/ic102522k
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_sum            'C38 H48 Fe2 N4 O22 Se12'
_chemical_formula_weight         1972.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.188(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9413(5)
_cell_length_b                   10.4374(4)
_cell_length_c                   25.0015(11)
_cell_measurement_reflns_used    41795
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2847.5(2)
_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    'WINGGX (Farrugia, 1999)'
_computing_publication_material  'WINGGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1892
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41116
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    8.257
_exptl_absorpt_correction_T_max  0.7898
_exptl_absorpt_correction_T_min  0.1908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.477
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.302
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.074(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         41116
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.7256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1889
_reflns_number_gt                25321
_reflns_number_total             41116
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic102522k_si_001_5.cif
_cod_data_source_block           TSFFeEDDS
_cod_database_code               4324962