#------------------------------------------------------------------------------
#$Date: 2016-02-18 10:40:55 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176722 $
#$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500001.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_3500001
loop_
_publ_author_name
'Miguel Quirós'
'Juan M. Salas'
_journal_name_full               'Personal communication to COD'
_journal_year                    2011
_chemical_formula_moiety         '2 (C9 H9 N4 O4 1+), Fe H12 O6 2+, 4 (H2 O)'
_chemical_formula_sum            'C18 H38 Fe N8 O18'
_chemical_formula_weight         710.41
_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                105.260(10)
_cell_angle_beta                 95.100(10)
_cell_angle_gamma                115.580(10)
_cell_formula_units_Z            1
_cell_length_a                   8.1720(10)
_cell_length_b                   9.1441(6)
_cell_length_c                   11.945(2)
_cell_measurement_temperature    293(2)
_cell_volume                     755.39(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_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  0.1513
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5131
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.596
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.596
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                3985
_reflns_number_total             4291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            feteof.cif
_cod_data_source_block           feteof
_cod_original_cell_volume        755.39(16)
_cod_database_code               3500001
_cod_database_fobs_code          3500001
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.5000 0.5000 0.5000 0.02431(10) Uani 1 2 d S . .
N1 N 0.73401(17) 0.42422(16) -0.02050(10) 0.0314(2) Uani 1 1 d . . .
C1 C 0.6160(3) 0.3920(3) -0.13346(15) 0.0463(4) Uani 1 1 d . . .
H11 H 0.6593 0.4945 -0.1547 0.056 Uiso 1 1 d R . .
H12 H 0.4882 0.3531 -0.1284 0.056 Uiso 1 1 d R . .
H13 H 0.6260 0.3046 -0.1932 0.056 Uiso 1 1 d R . .
C2 C 0.7440(2) 0.28227(18) -0.00516(12) 0.0309(3) Uani 1 1 d . . .
O2 O 0.66388(19) 0.14034(15) -0.08471(11) 0.0429(3) Uani 1 1 d . . .
N3 N 0.84736(19) 0.30621(16) 0.10092(11) 0.0322(3) Uani 1 1 d . . .
C3 C 0.8573(3) 0.1587(2) 0.12225(17) 0.0482(4) Uani 1 1 d . . .
H31 H 0.9235 0.1922 0.2028 0.058 Uiso 1 1 d R . .
H32 H 0.9234 0.1233 0.0679 0.058 Uiso 1 1 d R . .
H33 H 0.7346 0.0649 0.1084 0.058 Uiso 1 1 d R . .
C4 C 0.93325(19) 0.46548(18) 0.18775(12) 0.0288(3) Uani 1 1 d . . .
C5 C 0.92235(18) 0.60414(17) 0.17052(12) 0.0276(3) Uani 1 1 d . . .
C6 C 0.82087(19) 0.59242(18) 0.06318(12) 0.0295(3) Uani 1 1 d . . .
O6 O 0.80528(18) 0.71021(16) 0.04053(11) 0.0426(3) Uani 1 1 d . . .
N7 N 1.02696(17) 0.74006(16) 0.27596(11) 0.0318(3) Uani 1 1 d . . .
C8 C 1.0898(2) 0.6753(2) 0.34758(14) 0.0385(3) Uani 1 1 d . . .
H8 H 1.1624 0.7403 0.4248 0.046 Uiso 1 1 d R . .
N9 N 1.03804(19) 0.50833(18) 0.29749(12) 0.0368(3) Uani 1 1 d . . .
C10 C 1.05022(19) 0.91340(18) 0.30915(14) 0.0332(3) Uani 1 1 d . . .
H101 H 1.0681 0.9528 0.2411 0.040 Uiso 1 1 d R . .
H102 H 1.1618 0.9890 0.3726 0.040 Uiso 1 1 d R . .
C11 C 0.88411(18) 0.92668(17) 0.35088(11) 0.0266(2) Uani 1 1 d . . .
O11 O 0.74345(16) 0.79233(14) 0.34253(12) 0.0401(3) Uani 1 1 d . . .
O12 O 0.90365(16) 1.07577(14) 0.39032(12) 0.0394(3) Uani 1 1 d . . .
O1W O 0.59466(19) 0.46223(15) 0.33969(10) 0.0423(3) Uani 1 1 d D . .
H11W H 0.521(3) 0.382(2) 0.2752(17) 0.051 Uiso 1 1 d D . .
H12W H 0.649(3) 0.5584(19) 0.330(2) 0.051 Uiso 1 1 d D . .
O2W O 0.77898(15) 0.64065(15) 0.59844(12) 0.0417(3) Uani 1 1 d D . .
H21W H 0.865(3) 0.727(2) 0.585(2) 0.050 Uiso 1 1 d D . .
H22W H 0.831(3) 0.587(3) 0.625(2) 0.050 Uiso 1 1 d D . .
O3W O 0.49819(17) 0.72419(14) 0.48317(11) 0.0367(2) Uani 1 1 d D . .
H31W H 0.491(3) 0.798(3) 0.5403(15) 0.044 Uiso 1 1 d D . .
H32W H 0.564(3) 0.759(3) 0.4397(16) 0.044 Uiso 1 1 d D . .
O4W O 0.4035(3) 0.2110(2) 0.12145(15) 0.0754(6) Uani 1 1 d . . .
H41W H 0.3365 0.1021 0.1066 0.091 Uiso 1 1 d R . .
H42W H 0.3582 0.2439 0.0713 0.091 Uiso 1 1 d R . .
O5W O 0.5374(2) 1.0373(2) 0.34452(15) 0.0624(4) Uani 1 1 d D . .
H51W H 0.646(3) 1.045(4) 0.355(2) 0.075 Uiso 1 1 d D . .
H52W H 0.484(3) 0.995(4) 0.2685(16) 0.075 Uiso 1 1 d 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
_geom_angle_publ_flag
O2W Fe O2W 180.0 2_666 . ?
O2W Fe O3W 92.15(5) 2_666 2_666 ?
O2W Fe O3W 87.85(5) . 2_666 ?
O2W Fe O3W 87.85(5) 2_666 . ?
O2W Fe O3W 92.15(5) . . ?
O3W Fe O3W 180.0 2_666 . ?
O2W Fe O1W 89.48(6) 2_666 2_666 ?
O2W Fe O1W 90.52(6) . 2_666 ?
O3W Fe O1W 89.94(5) 2_666 2_666 ?
O3W Fe O1W 90.06(5) . 2_666 ?
O2W Fe O1W 90.52(6) 2_666 . ?
O2W Fe O1W 89.48(6) . . ?
O3W Fe O1W 90.06(5) 2_666 . ?
O3W Fe O1W 89.94(5) . . ?
O1W Fe O1W 180.0 2_666 . ?
C2 N1 C6 126.30(12) . . ?
C2 N1 C1 115.99(13) . . ?
C6 N1 C1 117.67(13) . . ?
N1 C1 H11 110.5 . . ?
N1 C1 H12 111.1 . . ?
H11 C1 H12 109.4 . . ?
N1 C1 H13 106.8 . . ?
H11 C1 H13 109.2 . . ?
H12 C1 H13 109.8 . . ?
O2 C2 N3 121.15(14) . . ?
O2 C2 N1 121.26(13) . . ?
N3 C2 N1 117.59(12) . . ?
C2 N3 C4 119.57(12) . . ?
C2 N3 C3 119.40(12) . . ?
C4 N3 C3 120.97(13) . . ?
N3 C3 H31 110.0 . . ?
N3 C3 H32 107.6 . . ?
H31 C3 H32 109.5 . . ?
N3 C3 H33 110.9 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.4 . . ?
N9 C4 N3 126.32(13) . . ?
N9 C4 C5 111.79(12) . . ?
N3 C4 C5 121.88(12) . . ?
C4 C5 N7 104.96(12) . . ?
C4 C5 C6 122.59(12) . . ?
N7 C5 C6 132.45(13) . . ?
O6 C6 N1 121.39(13) . . ?
O6 C6 C5 126.56(14) . . ?
N1 C6 C5 112.05(12) . . ?
C8 N7 C5 106.15(12) . . ?
C8 N7 C10 125.63(13) . . ?
C5 N7 C10 127.95(13) . . ?
N9 C8 N7 113.54(13) . . ?
N9 C8 H8 123.2 . . ?
N7 C8 H8 123.3 . . ?
C8 N9 C4 103.56(13) . . ?
N7 C10 C11 113.12(11) . . ?
N7 C10 H101 108.9 . . ?
C11 C10 H101 109.0 . . ?
N7 C10 H102 108.9 . . ?
C11 C10 H102 109.0 . . ?
H101 C10 H102 107.8 . . ?
O11 C11 O12 125.75(13) . . ?
O11 C11 C10 118.54(12) . . ?
O12 C11 C10 115.71(12) . . ?
Fe O1W H11W 120.5(15) . . ?
Fe O1W H12W 107.8(17) . . ?
H11W O1W H12W 112.5(17) . . ?
Fe O2W H21W 124.5(15) . . ?
Fe O2W H22W 119.3(15) . . ?
H21W O2W H22W 107.6(16) . . ?
Fe O3W H31W 122.7(14) . . ?
Fe O3W H32W 110.0(15) . . ?
H31W O3W H32W 117.7(18) . . ?
H41W O4W H42W 110.3 . . ?
H51W O5W H52W 110(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe O2W 2.1046(11) 2_666 ?
Fe O2W 2.1046(11) . ?
Fe O3W 2.1179(11) 2_666 ?
Fe O3W 2.1179(11) . ?
Fe O1W 2.1284(12) 2_666 ?
Fe O1W 2.1285(12) . ?
N1 C2 1.392(2) . ?
N1 C6 1.4108(18) . ?
N1 C1 1.4669(19) . ?
C1 H11 0.9600 . ?
C1 H12 0.9602 . ?
C1 H13 0.9600 . ?
C2 O2 1.2338(17) . ?
C2 N3 1.3680(18) . ?
N3 C4 1.3719(18) . ?
N3 C3 1.470(2) . ?
C3 H31 0.9601 . ?
C3 H32 0.9600 . ?
C3 H33 0.9601 . ?
C4 N9 1.3584(17) . ?
C4 C5 1.3747(19) . ?
C5 N7 1.3888(17) . ?
C5 C6 1.4159(19) . ?
C6 O6 1.2311(19) . ?
N7 C8 1.340(2) . ?
N7 C10 1.4496(18) . ?
C8 N9 1.336(2) . ?
C8 H8 0.9300 . ?
C10 C11 1.5285(19) . ?
C10 H101 0.9700 . ?
C10 H102 0.9700 . ?
C11 O11 1.2394(17) . ?
C11 O12 1.2516(17) . ?
O1W H11W 0.857(15) . ?
O1W H12W 0.842(14) . ?
O2W H21W 0.866(15) . ?
O2W H22W 0.869(14) . ?
O3W H31W 0.852(14) . ?
O3W H32W 0.806(14) . ?
O4W H41W 0.8615 . ?
O4W H42W 0.8598 . ?
O5W H51W 0.852(16) . ?
O5W H52W 0.873(16) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O4W 0.857(15) 1.901(16) 2.7455(19) 168(2) .
O1W H11W O4W 0.857(15) 1.901(16) 2.7455(19) 168(2) .
O1W H11W O4W 0.857(15) 1.901(16) 2.7455(19) 168(2) .
O1W H12W O11 0.842(14) 1.892(15) 2.7130(17) 165(2) .
O2W H21W O12 0.866(15) 1.895(17) 2.7232(16) 160(2) 2_776
O2W H22W N9 0.869(14) 1.957(15) 2.8209(18) 173(2) 2_766
O3W H31W O5W 0.852(14) 1.865(15) 2.7148(18) 175(2) 2_676
O3W H32W O11 0.806(14) 1.922(14) 2.7016(17) 163(2) .
O4W H41W O2 0.86 2.16 2.916(2) 146.1 2_655
O4W H42W O6 0.86 2.05 2.895(2) 167.2 2_665
O5W H52W O2 0.873(16) 2.150(17) 3.018(2) 173(3) 2_665
O5W H51W O12 0.852(16) 1.992(16) 2.842(2) 176(3) .
