Recognition of Topological Isomerism: Synthesis, Structure, and Magnetic Properties of Two Pentanuclear High-Spin Molecules of the Type [NiII(N-N)2]3[FeIII(CN)6]2
Curtis P. Berlinguette; José Ramón Galán-Mascarós; Kim R. Dunbar; Inorganic Chemistry 42 (2003) 3416–3422; doi:10.1021/ic0205031

data_4313673
_publ_section_title
;
 Recognition of Topological Isomerism: Synthesis, Structure, and Magnetic
 Properties of Two Pentanuclear High-Spin Molecules of the Type
 [NiII(N-N)2]3[FeIII(CN)6]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3416
_journal_page_last               3422
_journal_paper_doi               10.1021/ic0205031
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C72 H74 Fe2 N24 Ni3 O12.5'
_chemical_formula_weight         1763.38
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.58(3)
_cell_angle_beta                 103.29(3)
_cell_angle_gamma                95.18(3)
_cell_formula_units_Z            2
_cell_length_a                   13.264(3)
_cell_length_b                   17.607(4)
_cell_length_c                   18.057(4)
_cell_measurement_temperature    110(2)
_cell_volume                     4065.2(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.5932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18620
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    1.104
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1820
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         18620
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.3060
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.474
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.2523
_reflns_number_gt                4093
_reflns_number_total             18620
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic0205031_2.cif
_cod_data_source_block
'[Ni(bpy)2(H2O)]{[Ni(bpy)2]2[Fe(CN)6]2}(2)*24H2O'
_cod_original_cell_volume        4065.2(16)
_cod_original_formula_sum        'C72 H74 Fe2 N24 Ni3 O12.50'
_cod_database_code               4313673