#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:01:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180368 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/37/7203702.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_7203702
loop_
_publ_author_name
'Armentano, Donatella'
'De Munno, Giovanni'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Bis and tris(oxalato)ferrate(iii) complexes as precursors of
 polynuclear compounds
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              57
_journal_paper_doi               10.1039/b417251e
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C6 H10 Fe Na3 O17'
_chemical_formula_weight         478.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.46(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.404(4)
_cell_length_b                   12.702(3)
_cell_length_c                   15.220(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     3308.7(16)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            3944
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        2.9
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0570
_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)+(0.0772P)²+12.8908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                2988
_reflns_number_total             3629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417251e.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3308.7(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7203702
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.19164(3) 0.13442(4) 0.73278(4) 0.02342(17) Uani 1 1 d . . .
O1 O 0.26811(15) 0.1034(2) 0.65219(18) 0.0317(6) Uani 1 1 d . . .
O2 O 0.29220(15) 0.1715(2) 0.81618(18) 0.0303(6) Uani 1 1 d . . .
C1 C 0.3406(2) 0.1176(3) 0.6873(3) 0.0264(8) Uani 1 1 d . . .
C2 C 0.3548(2) 0.1522(3) 0.7863(3) 0.0251(8) Uani 1 1 d . . .
O3 O 0.39657(16) 0.1080(3) 0.6487(2) 0.0379(7) Uani 1 1 d . . .
O4 O 0.42193(16) 0.1598(2) 0.82757(19) 0.0328(6) Uani 1 1 d . . .
Na1 Na 0.5000 0.00220(18) 0.7500 0.0377(6) Uani 1 2 d S . .
O5 O 0.10322(16) 0.0578(2) 0.65358(18) 0.0304(6) Uani 1 1 d . . .
O6 O 0.19392(16) -0.0017(2) 0.80016(19) 0.0324(6) Uani 1 1 d . . .
C3 C 0.1399(2) -0.0677(3) 0.7699(2) 0.0258(7) Uani 1 1 d . . .
C4 C 0.0851(2) -0.0325(3) 0.6825(2) 0.0263(8) Uani 1 1 d . . .
O7 O 0.03159(17) -0.0895(2) 0.6488(2) 0.0382(7) Uani 1 1 d . . .
O8 O 0.12823(17) -0.1525(2) 0.8042(2) 0.0340(7) Uani 1 1 d . . .
Na2 Na 0.0000 -0.22967(17) 0.7500 0.0327(5) Uani 1 2 d S . .
O9 O 0.12927(17) 0.1995(2) 0.81847(19) 0.0338(6) Uani 1 1 d . . .
O10 O 0.16442(17) 0.2714(2) 0.67124(18) 0.0318(6) Uani 1 1 d . . .
C5 C 0.1045(2) 0.2932(3) 0.7989(3) 0.0315(8) Uani 1 1 d . . .
C6 C 0.1251(2) 0.3364(3) 0.7111(3) 0.0279(8) Uani 1 1 d . . .
O11 O 0.0671(2) 0.3478(3) 0.8427(2) 0.0516(9) Uani 1 1 d . . .
O12 O 0.10352(18) 0.4237(2) 0.6831(2) 0.0414(7) Uani 1 1 d . . .
Na3 Na 0.04287(11) 0.11190(16) 0.50017(13) 0.0451(5) Uani 1 1 d . . .
Na4 Na 0.12115(15) 0.36955(19) 0.51643(15) 0.0621(6) Uani 1 1 d . . .
O13 O -0.0032(2) 0.2943(3) 0.5040(2) 0.0543(9) Uani 1 1 d D . .
H1W H -0.040(2) 0.314(5) 0.4506(18) 0.060 Uiso 1 1 d D . .
H2W H -0.035(2) 0.315(5) 0.547(2) 0.060 Uiso 1 1 d D . .
O14 O -0.0831(2) 0.0651(3) 0.5364(2) 0.0498(8) Uani 1 1 d D . .
H3W H -0.129(2) 0.088(4) 0.497(3) 0.060 Uiso 1 1 d D . .
H4W H -0.087(3) 0.099(4) 0.5916(18) 0.060 Uiso 1 1 d D . .
O15 O 0.1647(2) 0.1940(3) 0.4843(2) 0.0518(9) Uani 1 1 d D . .
H5W H 0.2158(15) 0.174(5) 0.516(3) 0.060 Uiso 1 1 d D . .
H6W H 0.171(3) 0.174(5) 0.4253(14) 0.060 Uiso 1 1 d D . .
O16 O 0.2028(4) 0.5053(6) 0.5253(3) 0.117(3) Uani 1 1 d D . .
H7W H 0.237(2) 0.518(5) 0.5812(16) 0.060 Uiso 1 1 d D . .
H8W H 0.238(2) 0.503(5) 0.484(2) 0.060 Uiso 1 1 d D . .
O17 O 0.2863(4) 0.6567(8) 0.4310(7) 0.196(5) Uani 1 1 d D . .
H9W H 0.2370(18) 0.621(4) 0.423(3) 0.060 Uiso 1 1 d D . .
H10W H 0.290(3) 0.666(5) 0.3696(13) 0.060 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 '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
O10 Fe1 O1 90.66(12) . . ?
O10 Fe1 O6 166.83(12) . . ?
O1 Fe1 O6 100.94(13) . . ?
O10 Fe1 O9 80.57(11) . . ?
O1 Fe1 O9 165.82(12) . . ?
O6 Fe1 O9 89.17(12) . . ?
O10 Fe1 O2 101.33(12) . . ?
O1 Fe1 O2 80.49(11) . . ?
O6 Fe1 O2 86.86(12) . . ?
O9 Fe1 O2 90.27(12) . . ?
O10 Fe1 O5 92.87(12) . . ?
O1 Fe1 O5 93.36(12) . . ?
O6 Fe1 O5 80.35(11) . . ?
O9 Fe1 O5 98.16(12) . . ?
O2 Fe1 O5 164.53(12) . . ?
C1 O1 Fe1 115.3(2) . . ?
C2 O2 Fe1 115.4(2) . . ?
O3 C1 O1 126.0(4) . . ?
O3 C1 C2 119.5(3) . . ?
O1 C1 C2 114.6(3) . . ?
O4 C2 O2 126.7(4) . . ?
O4 C2 C1 119.4(3) . . ?
O2 C2 C1 113.8(3) . . ?
C1 O3 Na4 120.4(3) . 7_556 ?
C1 O3 Na1 107.4(3) . . ?
Na4 O3 Na1 128.21(13) 7_556 . ?
C1 O3 Na2 98.1(3) . 3 ?
Na4 O3 Na2 113.30(12) 7_556 3 ?
Na1 O3 Na2 75.89(10) . 3 ?
C2 O4 Na2 111.4(2) . 3 ?
C2 O4 Na1 102.6(2) . . ?
Na2 O4 Na1 81.36(10) 3 . ?
O12 Na1 O12 131.72(17) 3_545 4_546 ?
O12 Na1 O3 88.49(11) 3_545 2_656 ?
O12 Na1 O3 117.41(10) 4_546 2_656 ?
O12 Na1 O3 117.41(10) 3_545 . ?
O12 Na1 O3 88.49(11) 4_546 . ?
O3 Na1 O3 115.90(17) 2_656 . ?
O12 Na1 O11 75.85(12) 3_545 4_546 ?
O12 Na1 O11 67.69(11) 4_546 4_546 ?
O3 Na1 O11 160.26(14) 2_656 4_546 ?
O3 Na1 O11 82.45(12) . 4_546 ?
O12 Na1 O11 67.69(11) 3_545 3_545 ?
O12 Na1 O11 75.85(12) 4_546 3_545 ?
O3 Na1 O11 82.45(12) 2_656 3_545 ?
O3 Na1 O11 160.26(14) . 3_545 ?
O11 Na1 O11 80.5(2) 4_546 3_545 ?
O12 Na1 O4 70.37(9) 3_545 2_656 ?
O12 Na1 O4 157.08(12) 4_546 2_656 ?
O3 Na1 O4 62.05(10) 2_656 2_656 ?
O3 Na1 O4 73.11(10) . 2_656 ?
O11 Na1 O4 121.43(10) 4_546 2_656 ?
O11 Na1 O4 124.78(10) 3_545 2_656 ?
O12 Na1 O4 157.08(12) 3_545 . ?
O12 Na1 O4 70.37(9) 4_546 . ?
O3 Na1 O4 73.11(10) 2_656 . ?
O3 Na1 O4 62.05(10) . . ?
O11 Na1 O4 124.78(10) 4_546 . ?
O11 Na1 O4 121.43(10) 3_545 . ?
O4 Na1 O4 88.64(14) 2_656 . ?
C4 O5 Fe1 115.6(2) . . ?
C4 O5 Na3 118.7(2) . . ?
Fe1 O5 Na3 125.05(13) . . ?
C3 O6 Fe1 115.8(2) . . ?
O8 C3 O6 126.0(4) . . ?
O8 C3 C4 119.5(3) . . ?
O6 C3 C4 114.5(3) . . ?
O7 C4 O5 127.0(4) . . ?
O7 C4 C3 119.6(3) . . ?
O5 C4 C3 113.4(3) . . ?
C4 O7 Na3 134.9(3) . 5_556 ?
C4 O7 Na2 113.8(3) . . ?
Na3 O7 Na2 110.89(12) 5_556 . ?
C3 O8 Na2 114.8(3) . . ?
O4 Na2 O4 108.65(17) 3_445 4_546 ?
O4 Na2 O8 129.17(10) 3_445 . ?
O4 Na2 O8 80.61(10) 4_546 . ?
O4 Na2 O8 80.61(10) 3_445 2_556 ?
O4 Na2 O8 129.17(10) 4_546 2_556 ?
O8 Na2 O8 132.65(16) . 2_556 ?
O4 Na2 O7 84.57(11) 3_445 2_556 ?
O4 Na2 O7 158.71(10) 4_546 2_556 ?
O8 Na2 O7 78.11(11) . 2_556 ?
O8 Na2 O7 68.25(10) 2_556 2_556 ?
O4 Na2 O7 158.71(10) 3_445 . ?
O4 Na2 O7 84.57(11) 4_546 . ?
O8 Na2 O7 68.25(10) . . ?
O8 Na2 O7 78.11(11) 2_556 . ?
O7 Na2 O7 88.26(17) 2_556 . ?
O4 Na2 O3 60.52(10) 3_445 3_445 ?
O4 Na2 O3 71.59(10) 4_546 3_445 ?
O8 Na2 O3 152.04(11) . 3_445 ?
O8 Na2 O3 70.91(9) 2_556 3_445 ?
O7 Na2 O3 129.60(9) 2_556 3_445 ?
O7 Na2 O3 110.91(9) . 3_445 ?
O4 Na2 O3 71.59(10) 3_445 4_546 ?
O4 Na2 O3 60.52(10) 4_546 4_546 ?
O8 Na2 O3 70.91(9) . 4_546 ?
O8 Na2 O3 152.04(11) 2_556 4_546 ?
O7 Na2 O3 110.91(9) 2_556 4_546 ?
O7 Na2 O3 129.60(9) . 4_546 ?
O3 Na2 O3 92.32(14) 3_445 4_546 ?
C5 O9 Fe1 115.3(2) . . ?
C6 O10 Fe1 116.0(2) . . ?
C6 O10 Na4 91.6(2) . . ?
Fe1 O10 Na4 146.45(14) . . ?
O11 C5 O9 126.0(4) . . ?
O11 C5 C6 119.9(4) . . ?
O9 C5 C6 114.2(3) . . ?
O12 C6 O10 124.8(4) . . ?
O12 C6 C5 121.2(4) . . ?
O10 C6 C5 113.9(3) . . ?
C5 O11 Na1 111.5(3) . 3_455 ?
C6 O12 Na1 115.4(3) . 3_455 ?
C6 O12 Na4 90.9(3) . . ?
Na1 O12 Na4 135.68(15) 3_455 . ?
O15 Na3 O7 106.76(13) . 5_556 ?
O15 Na3 O14 166.81(16) . . ?
O7 Na3 O14 80.31(13) 5_556 . ?
O15 Na3 O14 94.67(14) . 5_556 ?
O7 Na3 O14 78.76(13) 5_556 5_556 ?
O14 Na3 O14 97.68(13) . 5_556 ?
O15 Na3 O13 83.76(14) . . ?
O7 Na3 O13 90.66(13) 5_556 . ?
O14 Na3 O13 85.05(14) . . ?
O14 Na3 O13 168.40(15) 5_556 . ?
O15 Na3 O5 89.11(12) . . ?
O7 Na3 O5 156.26(13) 5_556 . ?
O14 Na3 O5 87.92(12) . . ?
O14 Na3 O5 82.51(12) 5_556 . ?
O13 Na3 O5 108.91(13) . . ?
O16 Na4 O13 153.2(3) . . ?
O16 Na4 O15 120.3(3) . . ?
O13 Na4 O15 85.78(15) . . ?
O16 Na4 O3 86.17(17) . 7_556 ?
O13 Na4 O3 91.24(14) . 7_556 ?
O15 Na4 O3 83.57(13) . 7_556 ?
O16 Na4 O10 103.6(2) . . ?
O13 Na4 O10 89.39(13) . . ?
O15 Na4 O10 72.50(13) . . ?
O3 Na4 O10 155.96(15) 7_556 . ?
O16 Na4 O12 85.74(16) . . ?
O13 Na4 O12 85.36(14) . . ?
O15 Na4 O12 121.01(14) . . ?
O3 Na4 O12 154.72(15) 7_556 . ?
O10 Na4 O12 49.22(9) . . ?
Na4 O13 Na3 94.93(16) . . ?
Na3 O14 Na3 82.32(13) . 5_556 ?
Na3 O15 Na4 93.71(15) . . ?
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 O10 1.992(3) . ?
Fe1 O1 2.006(3) . ?
Fe1 O6 2.006(3) . ?
Fe1 O9 2.019(3) . ?
Fe1 O2 2.022(3) . ?
Fe1 O5 2.024(3) . ?
O1 C1 1.289(5) . ?
O2 C2 1.278(4) . ?
C1 O3 1.232(5) . ?
C1 C2 1.547(5) . ?
C2 O4 1.225(5) . ?
C2 Na2 3.073(4) 3 ?
O3 Na4 2.493(4) 7_556 ?
O3 Na1 2.533(3) . ?
O3 Na2 2.977(4) 3 ?
O4 Na2 2.407(3) 3 ?
O4 Na1 2.798(3) . ?
Na1 O12 2.437(3) 3_545 ?
Na1 O12 2.437(3) 4_546 ?
Na1 O3 2.533(3) 2_656 ?
Na1 O11 2.569(4) 4_546 ?
Na1 O11 2.569(4) 3_545 ?
Na1 O4 2.798(3) 2_656 ?
Na1 Na2 3.406(3) 3 ?
O5 C4 1.288(5) . ?
O5 Na3 2.477(3) . ?
O6 C3 1.282(5) . ?
C3 O8 1.230(5) . ?
C3 C4 1.555(5) . ?
C4 O7 1.216(5) . ?
O7 Na3 2.415(4) 5_556 ?
O7 Na2 2.481(3) . ?
O8 Na2 2.440(3) . ?
Na2 O4 2.407(3) 3_445 ?
Na2 O4 2.407(3) 4_546 ?
Na2 O8 2.440(3) 2_556 ?
Na2 O7 2.481(3) 2_556 ?
Na2 O3 2.977(4) 3_445 ?
Na2 O3 2.977(4) 4_546 ?
O9 C5 1.283(5) . ?
O10 C6 1.292(5) . ?
O10 Na4 2.651(4) . ?
C5 O11 1.227(5) . ?
C5 C6 1.545(5) . ?
C6 O12 1.223(5) . ?
O11 Na1 2.569(4) 3_455 ?
O12 Na1 2.437(3) 3_455 ?
O12 Na4 2.700(4) . ?
Na3 O15 2.413(4) . ?
Na3 O7 2.415(4) 5_556 ?
Na3 O14 2.429(4) . ?
Na3 O14 2.448(4) 5_556 ?
Na3 O13 2.456(5) . ?
Na4 O16 2.223(5) . ?
Na4 O13 2.342(5) . ?
Na4 O15 2.433(5) . ?
Na4 O3 2.493(4) 7_556 ?
O14 Na3 2.448(4) 5_556 ?
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
O13 H1W O4 0.966(10) 1.901(19) 2.824(5) 159(4) 8_455
O13 H2W O11 0.969(10) 1.907(17) 2.844(5) 162(4) 2_556
O14 H3W O17 0.954(10) 1.844(16) 2.788(7) 170(5) 3_445
O14 H4W O9 0.954(10) 2.11(2) 3.014(5) 159(4) 2_556
O15 H6W O8 0.961(10) 1.88(3) 2.750(5) 149(4) 6
O16 H7W O6 0.959(10) 2.00(2) 2.926(7) 163(5) 4_556
O16 H8W O17 0.953(10) 2.33(5) 2.937(8) 121(4) .
O17 H9W O16 0.957(10) 2.30(4) 2.937(8) 123(4) .
O17 H10W O2 0.956(10) 2.22(5) 2.809(6) 119(5) 6_565
