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_4107544
_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
'(C10H4S8)7 (Re6S6Cl8)0.5 (Re6S7Cl7)0.5 (CH2Cl2)'
_chemical_formula_sum            'C71 H30 Cl8 Re6 S64'
_chemical_formula_weight         4335.59
_chemical_name_common            (BDT-TTP)7(Re6S6Cl8)0.5(Re6S7Cl7)0.5(CH2Cl2)
_chemical_name_systematic
; 
heptakis (2,5-bis(1,3-dithiol-2-ylidene)-1,3,4,6-tetrathiapentalenium) 
hemi (hexa-\m~eq~3-sulfido-di-\m~eq~3-chloro-hexachloro-octahedro-
hexarhenate(III)) hemi (hepta-\m~eq~3-sulfido-mono-\m~eq~3-chloro-
hexachloro-octahedro-hexarhenate(III)) 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                74.815(12)
_cell_angle_beta                 80.498(12)
_cell_angle_gamma                81.427(13)
_cell_formula_units_Z            1
_cell_length_a                   11.5401(12)
_cell_length_b                   13.4522(14)
_cell_length_c                   22.280(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.65
_cell_volume                     3271.8(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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Oscillation, \D\f=1.0%'
_diffrn_radiation_detector       'area detector'
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12691
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.752
_exptl_absorpt_correction_T_max  0.8737
_exptl_absorpt_correction_T_min  0.1832
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT (Stoe IPDS)'
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             2066
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.763
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         12691
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                7010
_reflns_number_total             12691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074774s-file004.cif
_cod_data_source_block           spe97a
_cod_original_cell_volume        3271.7(6)
_cod_database_code               4107544