#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:34:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178876 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/05/4110518.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_4110518
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 Cu Fe N16 O8'
_chemical_formula_weight         788.01
_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                69.210(7)
_cell_angle_beta                 81.602(7)
_cell_angle_gamma                87.821(6)
_cell_formula_units_Z            2
_cell_length_a                   6.9927(6)
_cell_length_b                   10.8763(8)
_cell_length_c                   12.2831(13)
_cell_measurement_temperature    293(2)
_cell_volume                     863.90(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.1790
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10407
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    2.208
_exptl_crystal_density_diffrn    3.029
_exptl_crystal_F_000             806
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                2538
_reflns_number_total             4964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja058030vsi20060216_100938_4.cif
_cod_data_source_block           import_COMPOUND4[FeCu]
_cod_original_cell_volume        863.90(13)
_cod_database_code               4110518
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 0.43419(7) 0.39823(6) 0.80934(5) 0.01737(18) Uani 1 1 d .
Cu1 Cu 1.0000 0.5000 0.5000 0.0250(2) Uani 1 2 d S
N1 N 0.4528(6) 0.6837(4) 0.7938(4) 0.0474(12) Uani 1 1 d .
N4 N 0.8049(5) 0.3275(4) 0.9266(3) 0.0307(9) Uani 1 1 d .
N3 N 0.7447(5) 0.4791(4) 0.5959(3) 0.0293(9) Uani 1 1 d .
N2 N 0.1269(4) 0.4698(4) 0.6414(3) 0.0282(9) Uani 1 1 d .
N9 N 0.2634(4) 0.3298(3) 0.9626(3) 0.0179(8) Uani 1 1 d .
N10 N 0.1275(5) 0.1330(4) 1.1067(3) 0.0296(9) Uani 1 1 d .
N11 N 0.4088(4) 0.2117(3) 0.8223(3) 0.0196(8) Uani 1 1 d .
N12 N 0.2830(5) 0.0043(4) 0.9533(4) 0.0295(9) Uani 1 1 d .
C1 C 0.4451(5) 0.5764(5) 0.8019(4) 0.0246(10) Uani 1 1 d .
C4 C 0.6659(5) 0.3535(4) 0.8880(4) 0.0222(10) Uani 1 1 d .
C3 C 0.6195(5) 0.4526(4) 0.6715(4) 0.0232(10) Uani 1 1 d .
C2 C 0.2297(5) 0.4437(4) 0.7095(4) 0.0201(9) Uani 1 1 d .
C9 C 0.1909(6) 0.3960(5) 1.0324(4) 0.0258(11) Uani 1 1 d .
C10 C 0.0854(6) 0.3347(5) 1.1386(4) 0.0308(11) Uani 1 1 d .
C11 C 0.0561(6) 0.2030(5) 1.1738(5) 0.0351(12) Uani 1 1 d .
C12 C 0.2277(5) 0.2003(4) 1.0036(4) 0.0201(9) Uani 1 1 d .
C13 C 0.3104(5) 0.1324(4) 0.9234(4) 0.0219(10) Uani 1 1 d .
C14 C 0.4793(6) 0.1560(5) 0.7442(5) 0.0310(12) Uani 1 1 d .
C15 C 0.4521(7) 0.0268(5) 0.7664(5) 0.0364(13) Uani 1 1 d .
C16 C 0.3548(6) -0.0461(5) 0.8719(5) 0.0326(12) Uani 1 1 d .
O1W O 1.0094(4) 0.2554(3) 0.5437(3) 0.0458(9) Uani 1 1 d .
O2W O 0.0404(4) -0.1528(3) 1.2142(3) 0.0461(9) Uani 1 1 d .
O4W O 0.3292(6) 0.1575(4) 0.4364(5) 0.0912(16) Uani 1 1 d .
O3W O 0.2587(6) 0.8806(5) 0.5235(5) 0.0964(17) Uani 1 1 d .
H9 H 0.202(6) 0.475(4) 1.010(4) 0.026(14) Uiso 1 1 d .
H10 H 0.033(5) 0.375(4) 1.194(4) 0.030(12) Uiso 1 1 d .
H11 H -0.025(5) 0.153(4) 1.250(4) 0.024(11) Uiso 1 1 d .
H14 H 0.529(5) 0.205(4) 0.681(4) 0.017(12) Uiso 1 1 d .
H15 H 0.493(6) -0.007(4) 0.719(4) 0.027(13) Uiso 1 1 d .
H16 H 0.335(5) -0.134(4) 0.893(4) 0.020(11) 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'
Cu Cu 0.3201 1.2651 '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'
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 85.64(18) . .
C3 Fe1 C2 88.84(17) . .
C1 Fe1 C2 89.94(17) . .
C3 Fe1 C4 82.81(17) . .
C1 Fe1 C4 91.83(17) . .
C2 Fe1 C4 171.30(18) . .
C3 Fe1 N9 173.67(14) . .
C1 Fe1 N9 96.64(16) . .
C2 Fe1 N9 97.05(15) . .
C4 Fe1 N9 91.20(15) . .
C3 Fe1 N11 97.24(17) . .
C1 Fe1 N11 176.89(15) . .
C2 Fe1 N11 88.94(15) . .
C4 Fe1 N11 89.70(15) . .
N9 Fe1 N11 80.61(14) . .
N3 Cu1 N3 180.000(1) 2_766 .
N3 Cu1 N2 90.39(14) 2_766 2_666
N3 Cu1 N2 89.61(14) . 2_666
N3 Cu1 N2 89.61(14) 2_766 1_655
N3 Cu1 N2 90.39(14) . 1_655
N2 Cu1 N2 180.000(1) 2_666 1_655
C3 N3 Cu1 164.6(4) . .
C2 N2 Cu1 165.8(4) . 1_455
C12 N9 C9 116.7(4) . .
C12 N9 Fe1 115.3(3) . .
C9 N9 Fe1 127.8(3) . .
C12 N10 C11 116.0(4) . .
C14 N11 C13 116.4(4) . .
C14 N11 Fe1 128.3(3) . .
C13 N11 Fe1 115.2(3) . .
C13 N12 C16 115.4(4) . .
N1 C1 Fe1 177.9(4) . .
N4 C4 Fe1 175.6(4) . .
N3 C3 Fe1 173.0(4) . .
N2 C2 Fe1 172.2(4) . .
N9 C9 C10 121.5(5) . .
C9 C10 C11 118.1(5) . .
N10 C11 C10 122.2(5) . .
N10 C12 N9 125.5(4) . .
N10 C12 C13 120.0(4) . .
N9 C12 C13 114.4(4) . .
N12 C13 N11 125.7(4) . .
N12 C13 C12 120.2(4) . .
N11 C13 C12 114.1(4) . .
N11 C14 C15 121.5(5) . .
C14 C15 C16 117.9(5) . .
N12 C16 C15 123.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C3 1.898(5) .
Fe1 C1 1.911(5) .
Fe1 C2 1.955(4) .
Fe1 C4 1.964(4) .
Fe1 N9 1.985(3) .
Fe1 N11 1.991(3) .
Cu1 N3 1.963(3) 2_766
Cu1 N3 1.963(3) .
Cu1 N2 1.984(4) 2_666
Cu1 N2 1.984(4) 1_655
N1 C1 1.139(5) .
N4 C4 1.126(4) .
N3 C3 1.142(5) .
N2 C2 1.135(5) .
N2 Cu1 1.984(4) 1_455
N9 C12 1.336(5) .
N9 C9 1.339(6) .
N10 C12 1.323(5) .
N10 C11 1.344(6) .
N11 C14 1.335(6) .
N11 C13 1.339(5) .
N12 C13 1.322(5) .
N12 C16 1.332(6) .
C9 C10 1.353(6) .
C10 C11 1.356(7) .
C12 C13 1.473(6) .
C14 C15 1.348(7) .
C15 C16 1.351(7) .
