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_4109117
_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_sum            'C22 H22 B Cl F4 Fe N4 O3'
_chemical_formula_weight         568.55
_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                 93.324(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.758(4)
_cell_length_b                   10.9760(17)
_cell_length_c                   16.503(3)
_cell_measurement_temperature    218(2)
_cell_volume                     4838.7(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20153
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.7959
_exptl_absorpt_correction_T_min  0.7959
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+12.9398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                4811
_reflns_number_total             5417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067208qsi20061008_025153.cif
_cod_data_source_block           jsm103s
_cod_original_cell_volume        4838.7(13)
_cod_database_code               4109117