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_4304991
_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            'C32 H28 Cl6 Cu N2 O2 S6'
_chemical_formula_weight         941.16
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.426(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.121(6)
_cell_length_b                   5.3371(5)
_cell_length_c                   20.584(3)
_cell_measurement_reflns_used    6324
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      1.12
_cell_volume                     3779.6(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1450
_diffrn_reflns_av_sigmaI/netI    0.1402
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12179
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS, (PLATON03, Speck, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6050
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0930
_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^)+(0.1403P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2506
_reflns_number_gt                3131
_reflns_number_total             6050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800138x-file002_3.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        3779.7(9)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4304991