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_4324959
_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 H46 Fe2 N4 O21 S12'
_chemical_formula_weight         1391.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4392(2)
_cell_length_b                   10.5270(2)
_cell_length_c                   23.9133(3)
_cell_measurement_reflns_used    9501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2124
_cell_measurement_theta_min      2.7580
_cell_volume                     2627.92(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_molecular_graphics    'WINGX (Ferrugia, 1999)'
_computing_publication_material  'WINGX (Ferrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.690
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector Ruby(Gemini Mo)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39836
_diffrn_reflns_theta_full        2.50
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1949
_refine_ls_number_reflns         10133
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                8746
_reflns_number_total             39836
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic102522k_si_001_2.cif
_cod_data_source_block           TTFFeEDDS
_cod_database_code               4324959