Tris(chloranilato)ferrate(III) Anionic Building Block Containing the (Dihydroxo)oxodiiron(III) Dimer Cation: Synthesis and Characterization of [(TPA)(OH)FeIIIOFeIII(OH)(TPA)][Fe(CA)3]0.5(BF4)0.5.1.5MeOH.H2O [TPA = tris(2-pyridylmethyl)amine; CA = chloranilate]
Kil Sik Min; Arnold L. Rhinegold; Joel S. Miller; Journal of the American Chemical Society 128 (2006) 40–41; doi:10.1021/ja0566984

data_4110343
_publ_section_title
;
 Tris(chloranilato)ferrate(III) Anionic Building Block Containing the
 (Dihydroxo)oxodiiron(III) Dimer Cation: Synthesis and Characterization of
 [(TPA)(OH)FeIIIOFeIII(OH)(TPA)][Fe(CA)3]0.5(BF4)0.5.1.5MeOH.H2O [TPA =
 tris(2-pyridylmethyl)amine; CA = chloranilate]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              40
_journal_page_last               41
_journal_paper_doi               10.1021/ja0566984
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C93 H92 B Cl6 F4 Fe5 N16 O23'
_chemical_formula_weight         2380.59
_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                 105.100(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.026(16)
_cell_length_b                   14.541(6)
_cell_length_c                   19.374(9)
_cell_measurement_temperature    223(2)
_cell_volume                     10071(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36348
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.950
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             4876
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         11806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.185
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+12.1211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                8871
_reflns_number_total             11806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0566984si20051010_030307.cif
_cod_data_source_block           C93H92BCl6F4Fe5N16O23
_cod_database_code               4110343