Crystal Chemistry and Physical Properties of Superconducting and Semiconducting Charge Transfer Salts of the Type (BEDT-TTF)4[AIMIII(C2O4)3].PhCN (AI= H3O, NH4, K; MIII= Cr, Fe, Co, Al; BEDT-TTF = Bis(ethylenedithio)tetrathiafulvalene)
Lee Martin; Scott S. Turner; Peter Day; Philippe Guionneau; Judith A. K. Howard; Dai E. Hibbs; Mark E. Light; Michael B. Hursthouse; Mikio Uruichi; Kyuyo Yakushi; Inorganic Chemistry 40 (2001) 1363–1371; doi:10.1021/ic001193u

data_4319425
_publ_section_title
;
 Crystal Chemistry and Physical Properties of Superconducting and
 Semiconducting Charge Transfer Salts of the Type
 (BEDT-TTF)4[AIMIII(C2O4)3].PhCN (AI= H3O, NH4, K; MIII= Cr, Fe, Co, Al;
 BEDT-TTF = Bis(ethylenedithio)tetrathiafulvalene)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1363
_journal_page_last               1371
_journal_paper_doi               10.1021/ic001193u
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C53 H41 Al N2 O12 S32'
_chemical_formula_weight         1950.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.318(7)
_cell_length_b                   19.460(4)
_cell_length_c                   35.808(8)
_cell_measurement_reflns_used    na
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      na
_cell_measurement_theta_min      na
_cell_volume                     7190(5)
_computing_cell_refinement       'MADNES, ABSURD'
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES, ABSURD'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      423(2)
_diffrn_measurement_device       'Enraf Nonius FAST TV area Detector'
_diffrn_measurement_method       'Phi and Ci scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf Nonius FR591 Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_sigmaI/netI    0.2627
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25018
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        na
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  2.127
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_F_000             3956
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.673
_refine_ls_goodness_of_fit_obs   0.946
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.673
_refine_ls_restrained_S_obs      0.946
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_obs          0.0437
_refine_ls_shift/esd_max         0.108
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1058
_refine_ls_wR_factor_obs         0.0887
_reflns_number_observed          2287
_reflns_number_total             5658
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001193u_2.cif
_cod_data_source_block           AloxalateET
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7189.8(53)
_cod_original_formula_sum        'C53 H41 Al1 N2 O12 S32'
_cod_database_code               4319425