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_4313672
_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            'C108 H124 Fe2 N24 Ni3 O14'
_chemical_formula_weight         2270.14
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.531(4)
_cell_length_b                   24.895(5)
_cell_length_c                   24.522(5)
_cell_measurement_temperature    110(2)
_cell_volume                     11787(4)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.2764
_diffrn_reflns_av_sigmaI/netI    0.6633
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            95305
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.778
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4752
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00438(16)
_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   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         28608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.3582
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.725
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.2750
_reflns_number_gt                5476
_reflns_number_total             28608
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic0205031_1.cif
_cod_data_source_block           '[Ni(tmphen)2]3[Fe(CN)6]2(1)*11H2O'
_cod_database_code               4313672