Synthesis, Structure, and Magnetic Properties of Valence Ambiguous Dinuclear Antiferromagnetically Coupled Cobalt and Ferromagnetically Coupled Iron Complexes Containing the Chloranilate(2-) and the Significantly Stronger Coupling Chloranilate(.3-) Radical Trianion
Kil Sik Min; Antonio G. DiPasquale; James A. Golen; Arnold L. Rheingold; Joel S. Miller; Journal of the American Chemical Society 129 (2007) 2360–2368; doi:10.1021/ja067208q

data_4109115
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of Valence Ambiguous
 Dinuclear Antiferromagnetically Coupled Cobalt and Ferromagnetically
 Coupled Iron Complexes Containing the Chloranilate(2-) and the
 Significantly Stronger Coupling Chloranilate(.3-) Radical Trianion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2360
_journal_page_last               2368
_journal_paper_doi               10.1021/ja067208q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C42 H36 Cl2 Co2 N8 O4,3(B F4),4(C2 H3 N)'
_chemical_formula_sum            'C50 H48 B3 Cl2 Co2 F12 N12 O4'
_chemical_formula_weight         1330.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.9883(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3216(6)
_cell_length_b                   15.5835(4)
_cell_length_c                   16.6696(3)
_cell_measurement_reflns_used    32821
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     5630.0(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11636
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.8595
_exptl_absorpt_correction_T_min  0.7828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       prism
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0398P)^2^+10.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                4854
_reflns_number_total             6451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067208qsi20061008_025122.cif
_cod_data_source_block           jsm058
_cod_database_code               4109115