#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:34:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178876 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/05/4110519.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4110519
loop_
_publ_author_name
'Luminita Marilena Toma'
'Rodrigue Lescouëzec'
'Jorge Pasán'
'Catalina Ruiz-Pérez'
'Jacqueline Vaissermann'
'Joan Cano'
'Rosa Carrasco'
'Wolfgang Wernsdorfer'
'Francesc Lloret'
'Miguel Julve'
_publ_section_title
;
 [Fe(bpym)(CN)4]-: A New Building Block for Designing Single-Chain Magnets
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4842
_journal_page_last               4853
_journal_paper_doi               10.1021/ja058030v
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C24 H28 Fe Mn N16 O8'
_chemical_formula_weight         779.41
_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                66.882(4)
_cell_angle_beta                 81.549(5)
_cell_angle_gamma                86.828(5)
_cell_formula_units_Z            2
_cell_length_a                   7.1305(3)
_cell_length_b                   10.7429(6)
_cell_length_c                   12.7093(7)
_cell_measurement_temperature    293(2)
_cell_volume                     885.66(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9804
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         5.03
_exptl_absorpt_coefficient_mu    1.666
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_F_000             798
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0338P)²+0.6510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                3499
_reflns_number_total             4941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja058030vsi20060216_100938_5.cif
_cod_data_source_block           import_COMPOUND5[FeMn]
_cod_database_code               4110519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.56783(5) 0.09122(4) 0.69262(3) 0.01995(10) Uani 1 1 d .
Mn1 Mn 0.0000 0.0000 1.0000 0.02452(14) Uani 1 2 d S
N3 N 0.2901(3) 0.0047(3) 0.9140(2) 0.0375(6) Uani 1 1 d .
N4 N 0.8899(3) 0.0153(3) 0.8426(2) 0.0364(6) Uani 1 1 d .
N1 N 0.5524(5) -0.2042(3) 0.7209(3) 0.0595(8) Uani 1 1 d .
N2 N 0.1995(3) 0.1666(3) 0.5795(2) 0.0352(5) Uani 1 1 d .
N11 N 0.5923(3) 0.2813(2) 0.67678(18) 0.0233(4) Uani 1 1 d .
N12 N 0.7172(3) 0.4954(2) 0.5465(2) 0.0326(5) Uani 1 1 d .
N9 N 0.7299(3) 0.1651(2) 0.54043(17) 0.0211(4) Uani 1 1 d .
N10 N 0.8654(3) 0.3685(2) 0.39788(19) 0.0343(5) Uani 1 1 d .
C3 C 0.4006(3) 0.0335(3) 0.8339(2) 0.0267(5) Uani 1 1 d .
C4 C 0.7783(3) 0.0426(3) 0.7821(2) 0.0239(5) Uani 1 1 d .
C1 C 0.5573(4) -0.0922(3) 0.7067(2) 0.0315(6) Uani 1 1 d .
C2 C 0.3381(3) 0.1379(3) 0.6189(2) 0.0248(5) Uani 1 1 d .
C14 C 0.5253(4) 0.3349(3) 0.7543(3) 0.0344(6) Uani 1 1 d .
C15 C 0.5543(5) 0.4688(3) 0.7300(3) 0.0408(7) Uani 1 1 d .
C16 C 0.6484(4) 0.5463(3) 0.6246(3) 0.0383(7) Uani 1 1 d .
C13 C 0.6884(3) 0.3649(3) 0.5771(2) 0.0236(5) Uani 1 1 d .
C12 C 0.7672(3) 0.2977(3) 0.4992(2) 0.0231(5) Uani 1 1 d .
C9 C 0.7980(4) 0.0982(3) 0.4739(2) 0.0289(6) Uani 1 1 d .
C10 C 0.9020(4) 0.1638(3) 0.3677(3) 0.0370(7) Uani 1 1 d .
C11 C 0.9329(4) 0.2990(3) 0.3330(3) 0.0404(7) Uani 1 1 d .
O1W O -0.0035(3) -0.2262(2) 1.05883(19) 0.0458(5) Uani 1 1 d .
O2W O -0.0408(3) -0.3426(2) 1.29134(19) 0.0506(6) Uani 1 1 d .
O3W O 0.7153(8) 0.3538(4) 0.0508(4) 0.154(2) Uani 1 1 d .
O4W O 0.7370(7) 0.6402(5) 0.9826(5) 0.1419(17) Uani 1 1 d .
H9 H 0.465(4) 0.280(3) 0.825(3) 0.041(9) Uiso 1 1 d .
H10 H 0.509(4) 0.503(3) 0.778(3) 0.036(8) Uiso 1 1 d .
H11 H 0.670(4) 0.638(3) 0.606(3) 0.039(8) Uiso 1 1 d .
H14 H 0.776(4) 0.008(3) 0.503(3) 0.036(8) Uiso 1 1 d .
H15 H 0.947(5) 0.117(4) 0.322(3) 0.051(10) Uiso 1 1 d .
H16 H 1.001(4) 0.348(3) 0.259(3) 0.043(9) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C3 Fe1 C1 85.57(11) . .
C3 Fe1 C4 88.28(10) . .
C1 Fe1 C4 88.94(12) . .
C3 Fe1 C2 85.43(10) . .
C1 Fe1 C2 91.99(11) . .
C4 Fe1 C2 173.55(10) . .
C3 Fe1 N9 175.33(10) . .
C1 Fe1 N9 97.89(10) . .
C4 Fe1 N9 94.91(9) . .
C2 Fe1 N9 91.29(9) . .
C3 Fe1 N11 96.19(10) . .
C1 Fe1 N11 177.23(10) . .
C4 Fe1 N11 88.97(10) . .
C2 Fe1 N11 90.30(10) . .
N9 Fe1 N11 80.48(8) . .
N3 Mn1 N3 180.0 2_557 .
N3 Mn1 N4 90.06(9) 2_557 2_657
N3 Mn1 N4 89.94(9) . 2_657
N3 Mn1 N4 89.94(9) 2_557 1_455
N3 Mn1 N4 90.06(9) . 1_455
N4 Mn1 N4 180.0 2_657 1_455
N3 Mn1 O1W 90.22(9) 2_557 .
N3 Mn1 O1W 89.78(9) . .
N4 Mn1 O1W 91.25(9) 2_657 .
N4 Mn1 O1W 88.75(9) 1_455 .
N3 Mn1 O1W 89.78(9) 2_557 2_557
N3 Mn1 O1W 90.22(9) . 2_557
N4 Mn1 O1W 88.75(9) 2_657 2_557
N4 Mn1 O1W 91.25(9) 1_455 2_557
O1W Mn1 O1W 180.000(1) . 2_557
C3 N3 Mn1 152.4(2) . .
C4 N4 Mn1 153.6(2) . 1_655
C13 N11 C14 116.7(2) . .
C13 N11 Fe1 115.68(16) . .
C14 N11 Fe1 127.59(19) . .
C13 N12 C16 116.0(2) . .
C9 N9 C12 117.3(2) . .
C9 N9 Fe1 127.15(18) . .
C12 N9 Fe1 115.51(16) . .
C12 N10 C11 116.0(3) . .
N3 C3 Fe1 174.8(2) . .
N4 C4 Fe1 173.6(2) . .
N1 C1 Fe1 176.5(3) . .
N2 C2 Fe1 177.0(2) . .
N11 C14 C15 120.4(3) . .
C16 C15 C14 118.3(3) . .
N12 C16 C15 122.4(3) . .
N12 C13 N11 126.1(2) . .
N12 C13 C12 120.1(2) . .
N11 C13 C12 113.8(2) . .
N10 C12 N9 125.6(2) . .
N10 C12 C13 120.0(2) . .
N9 C12 C13 114.4(2) . .
N9 C9 C10 120.9(3) . .
C11 C10 C9 117.6(3) . .
N10 C11 C10 122.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C3 1.900(3) .
Fe1 C1 1.912(3) .
Fe1 C4 1.940(2) .
Fe1 C2 1.950(3) .
Fe1 N9 1.986(2) .
Fe1 N11 1.987(2) .
Mn1 N3 2.186(2) 2_557
Mn1 N3 2.186(2) .
Mn1 N4 2.198(2) 2_657
Mn1 N4 2.198(2) 1_455
Mn1 O1W 2.245(2) .
Mn1 O1W 2.245(2) 2_557
N3 C3 1.139(3) .
N4 C4 1.136(3) .
N4 Mn1 2.198(2) 1_655
N1 C1 1.146(4) .
N2 C2 1.146(3) .
N11 C13 1.342(3) .
N11 C14 1.345(3) .
N12 C13 1.319(3) .
N12 C16 1.333(4) .
N9 C9 1.336(3) .
N9 C12 1.338(3) .
N10 C12 1.323(3) .
N10 C11 1.339(4) .
C14 C15 1.368(4) .
C15 C16 1.363(4) .
C13 C12 1.473(3) .
C9 C10 1.373(4) .
C10 C11 1.363(4) .
