Building Blocks for Molecule-Based Magnets: Radical Anions and Dianions of Substituted 3,6-Dimethylenecyclohexane-1,2,4,5-tetrones as Paramagnetic Bridging Ligands
Andrzej W. Misiołek; Andrew S. Ichimura; Robert A. Gentner; Rui H. Huang; Vanessa P. McCaffrey; James E. Jackson; Inorganic Chemistry 48 (2009) 9005–9017; doi:10.1021/ic901390n

data_4303217
_publ_section_title
;
Building Blocks for Molecule-Based Magnets: Radical Anions and Dianions of
Substituted 3,6-Dimethylenecyclohexane-1,2,4,5-tetrones as Paramagnetic
Bridging Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9005
_journal_page_last               9017
_journal_paper_doi               10.1021/ic901390n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C46 H58 N4 O7 S3'
_chemical_formula_weight         875.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.092(4)
_cell_length_b                   8.0588(16)
_cell_length_c                   26.781(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4463.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.1328
_diffrn_reflns_av_sigmaI/netI    0.1821
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            37199
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.221
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.468
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         10489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1556
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                4496
_reflns_number_total             10489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901390n_si_002_4.cif
_cod_data_source_block           5.(Me2SO)3
_cod_original_cell_volume        4463.7(15)
_cod_database_code               4303217