#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:57:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179086 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/48/4304830.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_4304830
loop_
_publ_author_name
'Donatella Armentano'
'Teresa F. Mastropietro'
'Giovanni De Munno'
'Patrizia Rossi'
'Francesc Lloret'
'Miguel Julve'
_publ_section_title
;
New Extended Magnetic Systems Based on Oxalate and Iron(III) Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3772
_journal_page_last               3786
_journal_paper_doi               10.1021/ic702403h
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C8 H18 Cl4 Fe2 N2 O9'
_chemical_formula_weight         539.74
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.56(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.959(3)
_cell_length_b                   13.998(4)
_cell_length_c                   13.594(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     1988.2(10)
_computing_cell_refinement       'Bruker P3'
_computing_data_collection       'Bruker P3'
_computing_data_reduction        'Bruker XDISK'
_computing_molecular_graphics    'SHELXTL NT Bruker XP'
_computing_publication_material  'SHELXTL NT Package Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V automatic four-circle diffractometer'
_diffrn_measurement_method       omega/2-theta-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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3793
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0699
_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)+(0.1469P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                2524
_reflns_number_total             3518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702403h-file007.cif
_cod_data_source_block           compound_9
_cod_database_code               4304830
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.72714(8) 0.07908(7) 0.61864(6) 0.0362(3) Uani 1 1 d . . .
Fe2 Fe 0.73779(8) -0.05770(7) 0.99568(6) 0.0368(3) Uani 1 1 d . . .
Cl1 Cl 0.92840(17) 0.06935(15) 0.61026(15) 0.0566(5) Uani 1 1 d . . .
Cl2 Cl 0.6738(2) 0.22654(14) 0.55353(15) 0.0639(6) Uani 1 1 d . . .
Cl3 Cl 0.7097(2) -0.21235(14) 1.03769(14) 0.0595(5) Uani 1 1 d . . .
Cl4 Cl 0.93415(16) -0.03391(16) 1.10463(13) 0.0570(5) Uani 1 1 d . . .
O1 O 0.7486(4) 0.1273(3) 0.7659(3) 0.0390(10) Uani 1 1 d . . .
O2 O 0.7512(4) -0.0523(3) 0.7012(3) 0.0401(10) Uani 1 1 d . . .
C1 C 0.7502(6) 0.0618(4) 0.8301(4) 0.0350(13) Uani 1 1 d . . .
C2 C 0.7576(5) -0.0401(4) 0.7944(5) 0.0335(13) Uani 1 1 d . . .
O3 O 0.7658(4) -0.1053(3) 0.8603(3) 0.0361(9) Uani 1 1 d . . .
O4 O 0.7442(4) 0.0733(3) 0.9194(3) 0.0426(11) Uani 1 1 d . . .
O5 O 0.6515(4) 0.0031(3) 0.4848(3) 0.0414(10) Uani 1 1 d . . .
C3 C 0.5353(6) -0.0165(4) 0.4612(4) 0.0342(13) Uani 1 1 d . . .
O6 O 0.5308(4) 0.0569(3) 0.6168(3) 0.0447(11) Uani 1 1 d . . .
O7 O 0.5395(4) -0.0541(4) 0.8997(3) 0.0475(12) Uani 1 1 d . . .
C4 C 0.5318(6) 0.0182(5) 1.0561(4) 0.0371(14) Uani 1 1 d . . .
O8 O 0.6509(4) 0.0065(4) 1.0906(3) 0.0428(11) Uani 1 1 d . . .
N1 N 0.3970(9) 0.2111(7) 0.6894(8) 0.080(3) Uiso 0.880(19) 1 d P . .
N1A N 0.323(3) 0.225(3) 0.734(3) 0.026(13) Uiso 0.120(19) 1 d P . .
C5 C 0.2887(13) 0.1519(9) 0.6965(8) 0.099(3) Uani 1 1 d . . .
C6 C 0.4770(11) 0.2530(10) 0.7839(9) 0.100(4) Uani 1 1 d . . .
N2 N 0.9614(15) 0.1541(11) 0.3518(12) 0.104(6) Uiso 0.67(2) 1 d P . .
N2A N 0.869(3) 0.1463(19) 0.250(2) 0.085(10) Uiso 0.33(2) 1 d P . .
C7 C 0.9959(11) 0.1969(10) 0.2722(13) 0.112(4) Uani 1 1 d . . .
C8 C 0.8146(13) 0.1212(10) 0.3225(9) 0.103(4) Uani 1 1 d . . .
O9 O 0.9627(11) 0.2824(8) 0.5078(10) 0.158(4) Uani 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'
Cl Cl 0.1484 0.1585 '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
O5 Fe1 O1 158.22(18) . . ?
O5 Fe1 O2 88.41(17) . . ?
O1 Fe1 O2 79.08(16) . . ?
O5 Fe1 O6 77.38(16) . . ?
O1 Fe1 O6 83.09(17) . . ?
O2 Fe1 O6 81.21(18) . . ?
O5 Fe1 Cl1 93.67(13) . . ?
O1 Fe1 Cl1 104.09(14) . . ?
O2 Fe1 Cl1 90.40(14) . . ?
O6 Fe1 Cl1 167.81(14) . . ?
O5 Fe1 Cl2 98.00(15) . . ?
O1 Fe1 Cl2 91.25(13) . . ?
O2 Fe1 Cl2 167.14(13) . . ?
O6 Fe1 Cl2 89.30(15) . . ?
Cl1 Fe1 Cl2 100.24(8) . . ?
O8 Fe2 O3 159.00(17) . . ?
O8 Fe2 O4 91.09(19) . . ?
O3 Fe2 O4 78.90(16) . . ?
O8 Fe2 O7 78.18(16) . . ?
O3 Fe2 O7 82.14(16) . . ?
O4 Fe2 O7 81.99(19) . . ?
O8 Fe2 Cl4 93.16(13) . . ?
O3 Fe2 Cl4 105.42(13) . . ?
O4 Fe2 Cl4 91.60(14) . . ?
O7 Fe2 Cl4 169.05(15) . . ?
O8 Fe2 Cl3 97.84(15) . . ?
O3 Fe2 Cl3 89.09(13) . . ?
O4 Fe2 Cl3 165.95(13) . . ?
O7 Fe2 Cl3 89.22(15) . . ?
Cl4 Fe2 Cl3 98.67(8) . . ?
C1 O1 Fe1 114.1(4) . . ?
C2 O2 Fe1 112.0(4) . . ?
O4 C1 O1 125.9(6) . . ?
O4 C1 C2 117.2(5) . . ?
O1 C1 C2 117.0(5) . . ?
O2 C2 O3 125.9(5) . . ?
O2 C2 C1 117.2(5) . . ?
O3 C2 C1 116.9(5) . . ?
C2 O3 Fe2 113.6(4) . . ?
C1 O4 Fe2 112.6(4) . . ?
C3 O5 Fe1 116.8(4) . . ?
O6 C3 O5 127.9(5) 3_656 . ?
O6 C3 C3 116.1(6) 3_656 3_656 ?
O5 C3 C3 116.0(6) . 3_656 ?
C3 O6 Fe1 113.6(4) 3_656 . ?
C4 O7 Fe2 112.7(4) 3_657 . ?
O7 C4 O8 127.9(5) 3_657 . ?
O7 C4 C4 116.7(7) 3_657 3_657 ?
O8 C4 C4 115.4(6) . 3_657 ?
C4 O8 Fe2 117.0(4) . . ?
N1A N1 C6 78(2) . . ?
N1A N1 C5 50.5(19) . . ?
C6 N1 C5 117.1(9) . . ?
N1 N1A C5 79(3) . . ?
N1 N1A C6 58.4(17) . . ?
C5 N1A C6 123(3) . . ?
N1A C5 N1 50.5(19) . . ?
N1 C6 N1A 43.2(14) . . ?
C7 N2 N2A 64.0(14) . . ?
C7 N2 C8 114.9(12) . . ?
N2A N2 C8 52.1(13) . . ?
C8 N2A N2 69.7(15) . . ?
C8 N2A C7 124(2) . . ?
N2 N2A C7 55.8(13) . . ?
N2 C7 N2A 60.2(13) . . ?
N2A C8 N2 58.2(13) . . ?
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
Fe1 O5 2.054(4) . ?
Fe1 O1 2.058(4) . ?
Fe1 O2 2.129(4) . ?
Fe1 O6 2.167(4) . ?
Fe1 Cl1 2.247(2) . ?
Fe1 Cl2 2.252(2) . ?
Fe2 O8 2.030(4) . ?
Fe2 O3 2.065(4) . ?
Fe2 O4 2.118(5) . ?
Fe2 O7 2.171(4) . ?
Fe2 Cl4 2.239(2) . ?
Fe2 Cl3 2.283(2) . ?
O1 C1 1.262(7) . ?
O2 C2 1.259(7) . ?
C1 O4 1.246(7) . ?
C1 C2 1.516(8) . ?
C2 O3 1.264(7) . ?
O5 C3 1.246(7) . ?
C3 O6 1.227(7) 3_656 ?
C3 C3 1.554(10) 3_656 ?
O6 C3 1.227(7) 3_656 ?
O7 C4 1.227(7) 3_657 ?
C4 O7 1.227(7) 3_657 ?
C4 O8 1.257(7) . ?
C4 C4 1.560(11) 3_657 ?
N1 N1A 1.16(4) . ?
N1 C6 1.444(15) . ?
N1 C5 1.475(15) . ?
N1A C5 1.16(4) . ?
N1A C6 1.66(4) . ?
N2 C7 1.385(19) . ?
N2 N2A 1.45(3) . ?
N2 C8 1.604(19) . ?
N2A C8 1.35(3) . ?
N2A C7 1.51(3) . ?
