Electrochemical Synthesis and Crystallization of a Novel Tetraarylaurate Anion: Synthesis, Structure, and Physical Properties of (BEDT-TTF)Au(C6Cl5)4
John A. Schlueter; Urs Geiser; H. Hau Wang; Michael L. VanZile; Shannon B. Fox; Jack M. Williams; Antonio Laguna; Mariano Laguna; Dieter Naumann; Thomas Roy; Inorganic Chemistry 36 (1997) 4265–4269; doi:10.1021/ic970274w

data_4324027
_publ_contact_author
;
Dr. Urs Geiser
Chemistry and Materials Science Divisions
Argonne National Laboratory
9700 South Cass Avenue
Argonne, IL 60439, USA
;
_publ_contact_author_email       geiser@anchx4.chm.anl.gov
_publ_contact_author_fax         '(630) 252-9151'
_publ_contact_author_phone       '(630) 252-3509'
_publ_section_title
;
 Electrochemical Synthesis and Crystallization of a Novel Tetraarylaurate
 Anion: Synthesis, Structure, and Physical Properties of
 (BEDT-TTF)Au(C6Cl5)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4265
_journal_page_last               4269
_journal_paper_doi               10.1021/ic970274w
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
Crystal grown by electrocrystallization
;
_chemical_formula_moiety         '(C10 H8 S8)+, (C24 Au Cl20)-'
_chemical_formula_sum            'C34 H8 Au Cl20 S8'
_chemical_formula_weight         1578.85
_chemical_name_common
;
Bis(ethylenedithio)tetrathiafulvalenium Tetrakis(pentachlorophenyl)aurate(III)
;
_chemical_name_systematic        ' ?'
_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'
_cell_angle_alpha                90
_cell_angle_beta                 101.3960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7835(9)
_cell_length_b                   20.2270(12)
_cell_length_c                   16.7303(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    25
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.00
_cell_volume                     4904.2(5)
_computing_cell_refinement       'SAINT v.4.0.5 (Siemens Co., 1996)'
_computing_data_collection       'SMART v.4.0.5 (Siemens Co., 1996)'
_computing_data_reduction        'SAINT v.4.0.5 (Siemens Co., 1996)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material
'Locally modified UCLA package: TABLES and PUBLIST (Strouse, 1985)'
_computing_structure_refinement
'Locally modified ORFLS (Busing & Levy, 1980)'
_computing_structure_solution
;
MULTAN-80 (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980)
;
_diffrn_ambient_temperature      25(2)
_diffrn_measurement_device
;
Siemens SMART diffractometer with CCD-based area detector
;
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18821
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    4.46
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       block
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.75
_refine_ls_extinction_coef       0.006(4)
_refine_ls_extinction_expression 'Larson (1967)'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_obs   1.629
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     592
_refine_ls_number_reflns         6046
_refine_ls_R_factor_obs          0.065
_refine_ls_shift/esd_max         0.15
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0004F^2^)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.061
_reflns_number_observed          6046
_reflns_number_total             6984
_reflns_observed_criterion       'F > 4.0 sigma(F)'
_cod_data_source_file            ic970274w.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/(\s^2^(F)+0.0004F^2^)'
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^(F)+0.0004F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4904.3(5)
_cod_database_code               4324027