Coordination Chemistry of a π-Extended, Rigid and Redox-Active Tetrathiafulvalene-Fused Schiff-Base Ligand
Jin-Cai Wu; Shi-Xia Liu; Tony D. Keene; Antonia Neels; Valeriu Mereacre; Annie K. Powell; Silvio Decurtins; Inorganic Chemistry 47 (2008) 3452–3459; doi:10.1021/ic800138x

data_4304989
_publ_section_title
;
Coordination Chemistry of a \p-Extended, Rigid and Redox-Active
Tetrathiafulvalene-Fused Schiff-Base Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3452
_journal_page_last               3459
_journal_paper_doi               10.1021/ic800138x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C66 H66 Fe2 N6 O7 S12'
_chemical_formula_weight         1551.67
_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                83.321(14)
_cell_angle_beta                 71.904(12)
_cell_angle_gamma                79.767(14)
_cell_formula_units_Z            2
_cell_length_a                   13.601(2)
_cell_length_b                   13.671(3)
_cell_length_c                   19.739(3)
_cell_measurement_reflns_used    4477
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      1.59
_cell_volume                     3425.9(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.3558
_diffrn_reflns_av_sigmaI/netI    0.5428
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38072
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS, (PLATON03, Speck, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.666
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.666
_refine_ls_R_factor_all          0.2923
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                2889
_reflns_number_total             12205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800138x-file002_1.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        3425.9(10)
_cod_database_code               4304989