Chirality in charge-transfer salts of BEDT-TTF of tris(oxalato)chromate(III)
Martin, Lee; Akutsu, Hiroki; Horton, Peter N.; Hursthouse, Michael B.; CrystEngComm 17 (2015) 2783–; doi:10.1039/C5CE00121H

data_7219555
_publ_section_title
;
 Chirality in charge-transfer salts of BEDT-TTF of
 tris(oxalato)chromate(III)
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2783
_journal_paper_doi               10.1039/C5CE00121H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C6 Cr Na O12, 3(C10 H8 S8), C2 H6 O'
_chemical_formula_sum            'C38 H30 Cr Na O13 S24'
_chemical_formula_weight         1539.05
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-11-19 deposited with the CCDC.
2015-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                81.9380(10)
_cell_angle_beta                 77.4830(10)
_cell_angle_gamma                68.0910(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8372(2)
_cell_length_b                   9.5138(2)
_cell_length_c                   18.1928(4)
_cell_measurement_reflns_used    6303
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1382.39(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    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30757
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.956
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.7645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            'Opaque dark purple'
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       Plate
_exptl_crystal_F_000             781
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
 The suggested pseudo symmetry does not truly exist due to the
 nature of the oxalate sheet with different M-O lengths required
 The solvent ethanol is disordered over 2 positions, with the
 smaller component left isotropic, and geometrical restraints
 (SAME and DFIX) employed.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12284
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0057P)^2^+1.1395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11150
_reflns_number_total             12284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00121h1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7219555--7219557.cif.'
_cod_database_code               7219555
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-4
_shelx_res_checksum              55825