#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:25:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178898 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/27/4112765.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_4112765
loop_
_publ_author_name
'Hiroki Oshio'
'Norihisa Hoshino'
'Tasuku Ito'
'Motohiro Nakano'
_publ_section_title
;
 Single-Molecule Magnets of Ferrous Cubes: Structurally Controlled
 Magnetic Anisotropy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8805
_journal_page_last               8812
_journal_paper_doi               10.1021/ja0487933
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C44 H60 Fe4 N4 O14'
_chemical_formula_weight         1044.32
_chemical_name_common            '[Fe4(sap)4(MeOH)4]2H2O  '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.7925(6)
_cell_length_b                   16.7925(6)
_cell_length_c                   17.4560(9)
_cell_measurement_temperature    203
_cell_volume                     4922.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19811
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2379
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+6.6750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                2040
_reflns_number_total             2427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0487933si20040302_071945.cif
_cod_data_source_block           '[Fe4(sap)4(MeOH)4]2H2O'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4112765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.404474(17) 0.777092(17) 1.061942(18) 0.02872(13) Uani 1 1 d .
O1 O 0.30672(9) 0.70616(10) 1.05858(9) 0.0392(4) Uani 1 1 d .
O2 O 0.51433(8) 0.82945(8) 1.06581(8) 0.0284(3) Uani 1 1 d .
O3 O 0.35013(12) 0.89325(11) 1.09056(13) 0.0548(5) Uani 1 1 d .
N1 N 0.37994(12) 0.80796(12) 0.94612(11) 0.0401(5) Uani 1 1 d .
C1 C 0.26227(13) 0.68283(14) 1.00000(15) 0.0395(5) Uani 1 1 d .
C2 C 0.20458(14) 0.62329(16) 1.01202(18) 0.0475(6) Uani 1 1 d .
C3 C 0.15642(17) 0.59719(19) 0.9526(2) 0.0592(8) Uani 1 1 d .
C4 C 0.16269(19) 0.6288(2) 0.8804(2) 0.0663(9) Uani 1 1 d .
C5 C 0.21769(19) 0.68704(19) 0.8678(2) 0.0578(8) Uani 1 1 d .
C6 C 0.26915(14) 0.71532(15) 0.92542(15) 0.0437(6) Uani 1 1 d .
C7 C 0.32491(16) 0.77759(16) 0.90450(16) 0.0458(6) Uani 1 1 d .
C8 C 0.42366(18) 0.87650(17) 0.91350(18) 0.0491(6) Uani 1 1 d .
C9 C 0.51179(16) 0.87773(16) 0.93320(15) 0.0445(6) Uani 1 1 d .
C10 C 0.53133(15) 0.89442(13) 1.01607(15) 0.0382(5) Uani 1 1 d .
C11 C 0.29132(18) 0.94335(19) 1.0610(2) 0.0542(7) Uani 1 1 d .
O1S O 0.5000 0.7500 0.7386(6) 0.290(6) Uani 1 2 d S
H1 H 0.2001(16) 0.6005(16) 1.0640(16) 0.043(7) Uiso 1 1 d .
H2 H 0.125(2) 0.558(2) 0.9638(19) 0.065(10) Uiso 1 1 d .
H3 H 0.131(2) 0.605(2) 0.840(2) 0.069(10) Uiso 1 1 d .
H4 H 0.223(2) 0.708(2) 0.823(2) 0.065(10) Uiso 1 1 d .
H5 H 0.3179(17) 0.7982(16) 0.8546(18) 0.050(8) Uiso 1 1 d .
H6 H 0.4190(17) 0.8769(17) 0.863(2) 0.054(8) Uiso 1 1 d .
H7 H 0.3981(16) 0.9266(17) 0.9374(14) 0.044(7) Uiso 1 1 d .
H8 H 0.5366(17) 0.8274(18) 0.9195(17) 0.051(8) Uiso 1 1 d .
H9 H 0.5374(15) 0.9216(16) 0.9032(16) 0.044(7) Uiso 1 1 d .
H10 H 0.5886(18) 0.9083(16) 1.0175(16) 0.050(8) Uiso 1 1 d .
H11 H 0.5006(15) 0.9424(16) 1.0351(15) 0.041(7) Uiso 1 1 d .
H12 H 0.382(2) 0.914(2) 1.122(2) 0.070(11) Uiso 1 1 d .
H13 H 0.254(2) 0.957(2) 1.096(2) 0.075(11) Uiso 1 1 d .
H14 H 0.2666(18) 0.9174(18) 1.0166(19) 0.058(9) Uiso 1 1 d .
H15 H 0.315(2) 0.994(3) 1.043(2) 0.099(13) 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'
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'
Fe Fe 0.3463 0.8444 '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
O1 Fe1 O2 169.52(6) . .
O1 Fe1 N1 87.64(7) . .
O2 Fe1 N1 95.81(7) . .
O1 Fe1 O2 94.09(6) . 12_768
O2 Fe1 O2 84.11(6) . 12_768
N1 Fe1 O2 170.58(7) . 12_768
O1 Fe1 O3 100.98(8) . .
O2 Fe1 O3 89.17(7) . .
N1 Fe1 O3 85.40(8) . .
O2 Fe1 O3 85.18(7) 12_768 .
O1 Fe1 O2 91.40(6) . 6_564
O2 Fe1 O2 78.13(6) . 6_564
N1 Fe1 O2 109.85(7) . 6_564
O2 Fe1 O2 79.39(6) 12_768 6_564
O3 Fe1 O2 160.87(7) . 6_564
C1 O1 Fe1 130.66(16) . .
C10 O2 Fe1 119.37(13) . .
C10 O2 Fe1 119.12(13) . 15_567
Fe1 O2 Fe1 100.12(6) . 15_567
C10 O2 Fe1 118.01(13) . 6_564
Fe1 O2 Fe1 101.76(6) . 6_564
Fe1 O2 Fe1 93.95(5) 15_567 6_564
C11 O3 Fe1 137.8(2) . .
C7 N1 C8 116.7(2) . .
C7 N1 Fe1 125.56(19) . .
C8 N1 Fe1 117.34(17) . .
O1 C1 C2 118.9(2) . .
O1 C1 C6 123.3(2) . .
C2 C1 C6 117.8(2) . .
C3 C2 C1 120.9(3) . .
C4 C3 C2 121.4(3) . .
C5 C4 C3 118.6(3) . .
C4 C5 C6 122.8(3) . .
C5 C6 C1 118.5(3) . .
C5 C6 C7 117.3(3) . .
C1 C6 C7 124.2(2) . .
N1 C7 C6 127.6(2) . .
N1 C8 C9 114.0(2) . .
C10 C9 C8 115.5(2) . .
O2 C10 C9 113.50(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0290(16) .
Fe1 O2 2.0447(15) .
Fe1 N1 2.127(2) .
Fe1 O2 2.1616(15) 12_768
Fe1 O3 2.2107(17) .
Fe1 O2 2.2505(14) 6_564
O1 C1 1.325(3) .
O2 C10 1.423(3) .
O2 Fe1 2.1616(15) 15_567
O2 Fe1 2.2505(14) 6_564
O3 C11 1.396(3) .
N1 C7 1.281(3) .
N1 C8 1.479(3) .
C1 C2 1.408(4) .
C1 C6 1.416(4) .
C2 C3 1.387(4) .
C3 C4 1.371(5) .
C4 C5 1.363(5) .
C5 C6 1.409(4) .
C6 C7 1.450(4) .
C8 C9 1.519(4) .
C9 C10 1.510(4) .
