Syntheses, Crystal Structures, and Magnetic Properties of the Oxalato-Bridged Mixed-Valence Complexes [FeII(bpm)3]2[FeIII2(ox)5].8H2O and FeII(bpm)3Na(H2O)2Fe(ox)3.4H2O (bpm = 2,2'-Bipyrimidine)
Donatella Armentano; Giovanni De Munno; Juan Faus; Francesc Lloret; Miguel Julve; Inorganic Chemistry 40 (2001) 655–660; doi:10.1021/ic000258q

data_4319223
_publ_contact_author
;
     Prof. G. De Munno
     Dipartimento di Chimica
     Universit\'a della Calabria
     I-87030 Arcavacata di Rende, Cosenza
     Italy
;
_publ_contact_author_email       demunno@unical.it
_publ_contact_author_fax         '39 984 492044'
_publ_contact_author_phone       '39 984 492068'
_publ_section_title
;
 Syntheses, Crystal Structures, and Magnetic Properties of the
 Oxalato-Bridged Mixed-Valence Complexes [FeII(bpm)3]2[FeIII2(ox)5].8H2O
 and FeII(bpm)3Na(H2O)2Fe(ox)3.4H2O (bpm = 2,2'-Bipyrimidine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              655
_journal_page_last               660
_journal_paper_doi               10.1021/ic000258q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'FeII(bpm)3Na(H2O)2Fe(ox)3 . 4H2O'
_chemical_formula_sum            'C30 H30 Fe2 N12 Na O18'
_chemical_formula_weight         981.4
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.609(2)
_cell_length_b                   19.670(5)
_cell_length_c                   15.843(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3875.9(14)
_computing_cell_refinement       'Bruker P3/V'
_computing_data_collection       'Bruker P3/V,(VMS vers 4.21/V, 1990)'
_computing_data_reduction        'Bruker SHELXTL PLUS,(VMS vers 4.21/V, 1990)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker R3m/v Diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9290
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red_brown
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.665
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0852
_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^)+(0.1347P)^2^+7.8938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2507
_reflns_number_gt                5612
_reflns_number_total             8501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000258q_2.cif
_cod_data_source_block           (2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 2/m 1'
_cod_database_code               4319223