Structural Analysis, Spectroscopic, and Magnetic Properties of the 1D Triple-Bridged Compounds [M(dca)2(bpa)] (M = Mn, Fe, Co, Zn; dca = dicyanamide; bpa = 1,2-bis(4-pyridyl)ethane) and the 3D [Ni(dca)(bpa)2]dca.6H2O
Noelia de la Pinta; Susana Martín; M. Karmele Urtiaga; M. Gotzone Barandika; María I. Arriortua; Luis Lezama; Gotzon Madariaga; Roberto Cortés; Inorganic Chemistry 49 (2010) 10445–10454; doi:10.1021/ic1014626

data_4317025
_publ_contact_author
;
   Prof. Roberto Cortes Montero
   Facultad de Ciencia y Tecnolog\'ia
   Dpto. de Qu\'imica Inorg\'anica 
   Universidad del Pa\'is Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       roberto.cortes@ehu.es
_publ_contact_author_fax         '34 4 6013500'
_publ_contact_author_phone       '34 4 6015521'
_publ_section_title
;
 Structural Analysis, Spectroscopic, and Magnetic Properties of the 1D
 Triple-Bridged Compounds [M(dca)2(bpa)] (M = Mn, Fe, Co, Zn; dca =
 dicyanamide; bpa = 1,2-bis(4-pyridyl)ethane) and the 3D
 [Ni(dca)(bpa)2]dca.6H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10445
_journal_page_last               10454
_journal_paper_doi               10.1021/ic1014626
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C16 H12 Fe N8'
_chemical_formula_sum            'C16 H12 Fe N8'
_chemical_formula_weight         372.19
_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                 123.16(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.588(5)
_cell_length_b                   9.661(3)
_cell_length_c                   12.970(5)
_cell_measurement_reflns_used    1213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.57
_cell_volume                     1740.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.969
_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  0.1461
_diffrn_reflns_av_sigmaI/netI    0.1997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6560
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.9319
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.653
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.653
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0091P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                619
_reflns_number_total             1636
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic1014626_si_001_3.cif
_cod_data_source_block           febpadca
_cod_original_cell_volume        1739.9(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4317025