#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:14:00 +0100 (vie 25 de mar de 2016) $
#$Revision: 179959 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/53/7025327.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_7025327
loop_
_publ_author_name
'Craig, Gavin A.'
'Barrios, Leoní A.'
'Costa, José Sánchez'
'Roubeau, Olivier'
'Ruiz, Eliseo'
'Teat, Simon J.'
'Wilson, Chick C.'
'Thomas, Lynne'
'Aromí, Guillem'
_publ_section_title
;
 Synthesis of a novel heptacoordinated Fe(iii) dinuclear complex:
 experimental and theoretical study of the magnetic properties
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4874
_journal_paper_doi               10.1039/b927032a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C52 H34 Fe2 N14 O8 S4, C H4 O'
_chemical_formula_sum            'C53 H38 Fe2 N14 O9 S4'
_chemical_formula_weight         1254.91
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.493(3)
_cell_length_b                   23.530(5)
_cell_length_c                   10.094(2)
_cell_measurement_reflns_used    3610
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      2.1
_cell_volume                     2571.2(11)
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       MxCube
_computing_data_reduction        'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'phi rotation at various kappa'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ESRF BM16'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75140
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2970
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         2970
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0620
_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/[σ²(Fo²)+(0.1390P)²+0.8603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                2316
_reflns_number_total             2970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b927032a.txt
_cod_data_source_block           cut
_cod_original_cell_volume        2571.2(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7025327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.56093(7) 0.11717(3) 0.55319(8) 0.0791(4) Uani 1 1 d .
S1 S 0.92977(13) 0.09955(7) 0.45148(16) 0.0923(6) Uani 1 1 d .
S2 S 0.24979(17) 0.04423(8) 0.6690(2) 0.1138(7) Uani 1 1 d .
O1 O 0.5966(3) 0.03235(16) 0.6494(4) 0.0819(10) Uani 1 1 d .
O2 O 0.4550(3) 0.05927(16) 0.3931(4) 0.0806(10) Uani 1 1 d .
O3 O 0.8148(4) -0.00325(18) 1.0179(5) 0.1032(13) Uani 1 1 d .
H3 H 0.7592 0.0000 1.0542 0.155 Uiso 1 1 calc R
O4 O 0.2727(4) 0.11165(16) -0.0123(5) 0.1011(13) Uani 1 1 d .
H4 H 0.2526 0.0871 -0.0765 0.152 Uiso 1 1 calc R
N1 N 0.6942(4) 0.12749(19) 0.7637(5) 0.0813(12) Uani 1 1 d .
N2 N 0.7601(4) 0.0888(2) 0.8579(5) 0.0833(12) Uani 1 1 d .
H2A H 0.7442 0.0521 0.8514 0.100 Uiso 1 1 calc R
N3 N 0.6058(4) 0.21050(19) 0.6025(5) 0.0795(12) Uani 1 1 d .
N4 N 0.3752(4) 0.1586(2) 0.2462(5) 0.0842(12) Uani 1 1 d .
H4B H 0.3548 0.1239 0.2144 0.101 Uiso 1 1 calc R
N5 N 0.4568(4) 0.1702(2) 0.3746(5) 0.0839(12) Uani 1 1 d .
N6 N 0.7011(5) 0.10877(19) 0.4868(5) 0.0817(12) Uani 1 1 d .
N7 N 0.4175(5) 0.1195(2) 0.6279(5) 0.0866(13) Uani 1 1 d .
C1 C 0.5402(5) -0.0082(3) 0.5728(6) 0.0785(14) Uani 1 1 d .
C2 C 0.9202(5) 0.0230(3) 1.1020(6) 0.0863(16) Uani 1 1 d .
C3 C 1.0048(5) -0.0064(3) 1.2085(6) 0.0851(15) Uani 1 1 d .
H3A H 0.9900 -0.0452 1.2238 0.102 Uiso 1 1 calc R
C4 C 1.1111(5) 0.0196(3) 1.2938(6) 0.0868(16) Uani 1 1 d .
H4A H 1.1691 -0.0011 1.3677 0.104 Uiso 1 1 calc R
C5 C 1.1326(5) 0.0758(3) 1.2709(6) 0.0886(16) Uani 1 1 d .
H5A H 1.2051 0.0942 1.3298 0.106 Uiso 1 1 calc R
C6 C 1.0486(5) 0.1051(2) 1.1624(6) 0.0820(15) Uani 1 1 d .
H6A H 1.0655 0.1435 1.1459 0.098 Uiso 1 1 calc R
C7 C 0.9401(5) 0.0801(2) 1.0765(5) 0.0801(14) Uani 1 1 d .
C8 C 0.8539(5) 0.1126(2) 0.9640(6) 0.0811(15) Uani 1 1 d .
C9 C 0.8460(5) 0.1707(2) 0.9350(6) 0.0833(15) Uani 1 1 d .
H9A H 0.8985 0.1996 0.9890 0.100 Uiso 1 1 calc R
C10 C 0.7471(5) 0.1779(2) 0.8127(6) 0.0812(15) Uani 1 1 d .
C11 C 0.6913(5) 0.2258(2) 0.7235(6) 0.0830(15) Uani 1 1 d .
C12 C 0.7218(5) 0.2822(3) 0.7562(6) 0.0900(16) Uani 1 1 d .
H12A H 0.7837 0.2925 0.8421 0.108 Uiso 1 1 calc R
C13 C 0.6592(5) 0.3236(3) 0.6597(6) 0.0899(16) Uani 1 1 d .
H13A H 0.6775 0.3627 0.6800 0.108 Uiso 1 1 calc R
C14 C 0.5714(5) 0.3080(3) 0.5360(6) 0.0874(16) Uani 1 1 d .
H14A H 0.5278 0.3359 0.4698 0.105 Uiso 1 1 calc R
C15 C 0.5470(5) 0.2500(2) 0.5087(6) 0.0819(15) Uani 1 1 d .
C16 C 0.4606(5) 0.2274(3) 0.3826(6) 0.0826(15) Uani 1 1 d .
C17 C 0.3824(5) 0.2510(2) 0.2583(6) 0.0825(15) Uani 1 1 d .
H17A H 0.3690 0.2903 0.2371 0.099 Uiso 1 1 calc R
C18 C 0.3279(5) 0.2061(2) 0.1715(6) 0.0802(15) Uani 1 1 d .
C19 C 0.2350(5) 0.2071(2) 0.0337(6) 0.0812(15) Uani 1 1 d .
C20 C 0.1672(5) 0.2572(2) -0.0134(6) 0.0863(16) Uani 1 1 d .
H20A H 0.1839 0.2896 0.0463 0.104 Uiso 1 1 calc R
C21 C 0.0771(5) 0.2605(2) -0.1442(6) 0.0883(16) Uani 1 1 d .
H21A H 0.0313 0.2946 -0.1731 0.106 Uiso 1 1 calc R
C22 C 0.0538(5) 0.2142(3) -0.2326(7) 0.0934(17) Uani 1 1 d .
H22A H -0.0078 0.2164 -0.3230 0.112 Uiso 1 1 calc R
C23 C 0.1198(5) 0.1647(3) -0.1901(7) 0.0909(16) Uani 1 1 d .
H23A H 0.1045 0.1330 -0.2519 0.109 Uiso 1 1 calc R
C24 C 0.2070(5) 0.1611(2) -0.0598(7) 0.0862(16) Uani 1 1 d .
C25 C 0.7981(6) 0.1051(2) 0.4727(6) 0.0813(15) Uani 1 1 d .
C26 C 0.3475(5) 0.0881(3) 0.6473(6) 0.0827(15) Uani 1 1 d .
O1S O 0.3814(9) -0.0367(4) 0.8909(12) 0.123(3) Uani 0.50 1 d PDU
H1S H 0.3472 -0.0236 0.8096 0.184 Uiso 0.50 1 calc PR
C1S C 0.491(4) -0.003(2) 0.963(3) 0.162(13) Uani 0.50 1 d PDU
H1S1 H 0.4697 0.0370 0.9526 0.244 Uiso 0.50 1 calc PR
H1S2 H 0.5548 -0.0114 0.9214 0.244 Uiso 0.50 1 calc PR
H1S3 H 0.5209 -0.0136 1.0627 0.244 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0018
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0038
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0069
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
S S 0.1150 0.1392
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.2117 0.9395
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
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
N6 Fe1 N7 175.50(18) . .
N6 Fe1 O2 90.13(16) . .
N7 Fe1 O2 88.36(17) . .
N6 Fe1 N1 87.40(18) . .
N7 Fe1 N1 91.56(19) . .
O2 Fe1 N1 147.08(16) . .
N6 Fe1 N5 93.52(18) . .
N7 Fe1 N5 90.14(18) . .
O2 Fe1 N5 74.20(17) . .
N1 Fe1 N5 138.71(17) . .
N6 Fe1 O1 90.39(16) . .
N7 Fe1 O1 85.12(16) . .
O2 Fe1 O1 74.41(14) . .
N1 Fe1 O1 72.79(16) . .
N5 Fe1 O1 148.36(17) . .
N6 Fe1 N3 91.15(17) . .
N7 Fe1 N3 92.57(17) . .
O2 Fe1 N3 143.72(16) . .
N1 Fe1 N3 69.18(17) . .
N5 Fe1 N3 69.53(18) . .
O1 Fe1 N3 141.82(17) . .
C1 O1 Fe1 115.8(4) . .
C1 O2 Fe1 116.2(3) 3_656 .
C2 O3 H3 109.5 . .
C24 O4 H4 109.5 . .
C10 N1 N2 105.0(4) . .
C10 N1 Fe1 122.6(4) . .
N2 N1 Fe1 131.0(4) . .
N1 N2 C8 112.6(5) . .
N1 N2 H2A 123.7 . .
C8 N2 H2A 123.7 . .
C11 N3 C15 120.2(5) . .
C11 N3 Fe1 120.3(4) . .
C15 N3 Fe1 119.6(4) . .
N5 N4 C18 112.7(4) . .
N5 N4 H4B 123.6 . .
C18 N4 H4B 123.6 . .
C16 N5 N4 105.0(4) . .
C16 N5 Fe1 121.5(4) . .
N4 N5 Fe1 133.4(4) . .
C25 N6 Fe1 167.6(5) . .
C26 N7 Fe1 138.0(5) . .
O2 C1 O1 126.5(5) 3_656 .
O2 C1 C1 118.2(7) 3_656 3_656
O1 C1 C1 115.3(7) . 3_656
C3 C2 O3 120.4(6) . .
C3 C2 C7 120.8(5) . .
O3 C2 C7 118.8(5) . .
C2 C3 C4 120.8(6) . .
C2 C3 H3A 119.6 . .
C4 C3 H3A 119.6 . .
C3 C4 C5 119.5(5) . .
C3 C4 H4A 120.3 . .
C5 C4 H4A 120.3 . .
C6 C5 C4 119.8(6) . .
C6 C5 H5A 120.1 . .
C4 C5 H5A 120.1 . .
C5 C6 C7 121.8(6) . .
C5 C6 H6A 119.1 . .
C7 C6 H6A 119.1 . .
C6 C7 C2 117.3(5) . .
C6 C7 C8 120.0(6) . .
C2 C7 C8 122.6(5) . .
N2 C8 C9 105.2(5) . .
N2 C8 C7 123.5(5) . .
C9 C8 C7 131.4(5) . .
C10 C9 C8 106.5(5) . .
C10 C9 H9A 126.7 . .
C8 C9 H9A 126.7 . .
N1 C10 C9 110.7(5) . .
N1 C10 C11 113.9(5) . .
C9 C10 C11 135.3(5) . .
N3 C11 C12 121.7(5) . .
N3 C11 C10 113.3(5) . .
C12 C11 C10 125.0(6) . .
C11 C12 C13 118.3(6) . .
C11 C12 H12A 120.9 . .
C13 C12 H12A 120.9 . .
C14 C13 C12 120.0(6) . .
C14 C13 H13A 120.0 . .
C12 C13 H13A 120.0 . .
C13 C14 C15 118.7(6) . .
C13 C14 H14A 120.7 . .
C15 C14 H14A 120.7 . .
N3 C15 C14 121.2(6) . .
N3 C15 C16 114.0(5) . .
C14 C15 C16 124.9(6) . .
N5 C16 C17 110.3(5) . .
N5 C16 C15 115.1(5) . .
C17 C16 C15 134.5(6) . .
C18 C17 C16 106.5(5) . .
C18 C17 H17A 126.7 . .
C16 C17 H17A 126.7 . .
N4 C18 C17 105.5(5) . .
N4 C18 C19 125.4(5) . .
C17 C18 C19 129.0(5) . .
C24 C19 C20 116.4(5) . .
C24 C19 C18 124.4(5) . .
C20 C19 C18 119.2(5) . .
C21 C20 C19 121.6(5) . .
C21 C20 H20A 119.2 . .
C19 C20 H20A 119.2 . .
C22 C21 C20 119.8(6) . .
C22 C21 H21A 120.1 . .
C20 C21 H21A 120.1 . .
C21 C22 C23 120.0(6) . .
C21 C22 H22A 120.0 . .
C23 C22 H22A 120.0 . .
C24 C23 C22 120.2(6) . .
C24 C23 H23A 119.9 . .
C22 C23 H23A 119.9 . .
C23 C24 O4 121.8(5) . .
C23 C24 C19 122.0(5) . .
O4 C24 C19 116.2(5) . .
N6 C25 S1 179.2(6) . .
N7 C26 S2 178.2(5) . .
C1S O1S H1S 109.5 . .
O1S C1S H1S1 109.5 . .
O1S C1S H1S2 109.5 . .
H1S1 C1S H1S2 109.5 . .
O1S C1S H1S3 109.5 . .
H1S1 C1S H1S3 109.5 . .
H1S2 C1S H1S3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N6 1.952(5) .
Fe1 N7 2.030(5) .
Fe1 O2 2.151(4) .
Fe1 N1 2.176(5) .
Fe1 N5 2.189(5) .
Fe1 O1 2.197(4) .
Fe1 N3 2.273(5) .
S1 C25 1.603(7) .
S2 C26 1.593(7) .
O1 C1 1.261(7) .
O2 C1 1.247(7) 3_656
O3 C2 1.371(7) .
O3 H3 0.8400 .
O4 C24 1.382(7) .
O4 H4 0.8400 .
N1 C10 1.349(7) .
N1 N2 1.351(6) .
N2 C8 1.359(7) .
N2 H2A 0.8800 .
N3 C11 1.334(7) .
N3 C15 1.338(7) .
N4 N5 1.348(6) .
N4 C18 1.356(7) .
N4 H4B 0.8800 .
N5 C16 1.347(7) .
N6 C25 1.173(7) .
N7 C26 1.158(7) .
C1 O2 1.247(7) 3_656
C1 C1 1.501(11) 3_656
C2 C3 1.370(8) .
C2 C7 1.402(8) .
C3 C4 1.379(8) .
C3 H3A 0.9500 .
C4 C5 1.380(8) .
C4 H4A 0.9500 .
C5 C6 1.377(8) .
C5 H5A 0.9500 .
C6 C7 1.389(7) .
C6 H6A 0.9500 .
C7 C8 1.450(8) .
C8 C9 1.394(8) .
C9 C10 1.380(7) .
C9 H9A 0.9500 .
C10 C11 1.450(8) .
C11 C12 1.385(8) .
C12 C13 1.394(8) .
C12 H12A 0.9500 .
C13 C14 1.366(8) .
C13 H13A 0.9500 .
C14 C15 1.400(8) .
C14 H14A 0.9500 .
C15 C16 1.429(8) .
C16 C17 1.391(7) .
C17 C18 1.382(8) .
C17 H17A 0.9500 .
C18 C19 1.441(8) .
C19 C24 1.402(8) .
C19 C20 1.405(7) .
C20 C21 1.380(7) .
C20 H20A 0.9500 .
C21 C22 1.376(8) .
C21 H21A 0.9500 .
C22 C23 1.378(8) .
C22 H22A 0.9500 .
C23 C24 1.363(8) .
C23 H23A 0.9500 .
O1S C1S 1.45(2) .
O1S H1S 0.8400 .
C1S H1S1 0.9800 .
C1S H1S2 0.9800 .
C1S H1S3 0.9800 .
