Modulating the Framework Negative Charge Density in the System [BDT-TTP.+]/[Re6S5Cl91-]/[Re6(S/Se)6Cl82-]/[Re6S7Cl73-]: Templating by Isosteric Cluster Anions of Identical Symmetry and Shape, Variations of Incommensurate Band Filling, and Electronic Structure in 2D Metals
Sandrine Perruchas; Kamal Boubekeur; Enric Canadell; Yohji Misaki; Pascale Auban-Senzier; Claude Pasquier; Patrick Batail; Journal of the American Chemical Society 130 (2008) 3335–3348; doi:10.1021/ja074774s

data_4107546
_publ_section_title
;
 Modulating the Framework Negative Charge Density in the System
 [BDT-TTP.+]/[Re6S5Cl91-]/[Re6(S/Se)6Cl82-]/[Re6S7Cl73-]: Templating by
 Isosteric Cluster Anions of Identical Symmetry and Shape, Variations of
 Incommensurate Band Filling, and Electronic Structure in 2D Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3335
_journal_page_last               3348
_journal_paper_doi               10.1021/ja074774s
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C80 H32 S64 3+, Re6 S7 Cl7 3-, C4 H8 Cl8'
_chemical_formula_structural     '(C10H4S8)8 (Re6S7Cl7) (CH2Cl2)4'
_chemical_formula_sum            'C84 H40 Cl15 Re6 S71'
_chemical_formula_weight         4974.37
_chemical_name_common            (BDT-TTP)8[Re6S7Cl7].4(CH2Cl2)
_chemical_name_systematic
; 
octakis (2,5-bis(1,3-dithiol-2-ylidene)-1,3,4,6-tetrathiapentalenium) 
hepta-\m~eq~3-sulfido-mono-\m~eq~3-chloro-hexachloro-octahedro-
hexarhenate(III) tetrakis dichloromethane solvate  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.653(11)
_cell_angle_beta                 81.648(11)
_cell_angle_gamma                78.566(10)
_cell_formula_units_Z            1
_cell_length_a                   12.6684(11)
_cell_length_b                   13.9149(13)
_cell_length_c                   21.533(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      1.90
_cell_volume                     3553.9(6)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'stoe IPDS'
_diffrn_measurement_method       'Rotation, \D\f=1.1\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12860
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    6.459
_exptl_absorpt_correction_T_max  0.7737
_exptl_absorpt_correction_T_min  0.2237
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT stoe IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2385
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.292
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         12860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                9219
_reflns_number_total             12860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074774s-file006.cif
_cod_data_source_block           sp91m
_cod_database_code               4107546