#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/16/2101643.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2101643
loop_
_publ_author_name
'Lee, Chi-Rung'
'Wang, Chih-Chieh'
'Wang, Yu'
_publ_section_title
;
 Structural relationship of various squarates
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              966
_journal_page_last               975
_journal_paper_doi               10.1107/S0108768196009639
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         '[Fe (H C4 O4 )2 (H2 O)4 ]'
_chemical_formula_sum            'C8 H10 Fe O12'
_chemical_formula_weight         354.00
_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'
_cell_angle_alpha                66.846(12)
_cell_angle_beta                 77.109(15)
_cell_angle_gamma                74.748(15)
_cell_formula_units_Z            1
_cell_length_a                   5.1577(10)
_cell_length_b                   7.4107(13)
_cell_length_c                   8.7823(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      16.82
_cell_measurement_theta_min      9.29
_cell_volume                     295.05(9)
_computing_data_reduction
' NRCVAX DATRD2 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
' NRCVAX (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_publication_material
' NRCVAX TABLES (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_structure_refinement
' NRCVAX LSTSQ (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_structure_solution
' NRCVAX SOLVER (Gabe, Le Page, Charland, Lee & White, 1989)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'θ/2θ b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1369
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.34
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   '\y scan (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             180
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.56
_refine_ls_extinction_coef       3.105(208)x10^3^
_refine_ls_extinction_method     'Secondary (Larson, 1970)'
_refine_ls_goodness_of_fit_obs   3.43
_refine_ls_hydrogen_treatment    'H atoms placed in calculated positions'
_refine_ls_matrix_type           atomblock
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1287
_refine_ls_R_factor_all          0.029
_refine_ls_R_factor_obs          0.028
_refine_ls_shift/esd_max         0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.028
_refine_ls_wR_factor_obs         0.028
_reflns_number_observed          1287
_reflns_number_total             1359
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            oa0002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2101643
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Fe 0.0137(2) 0.0224(3) 0.0186(3) -0.00019(18) -0.00281(17) -0.01149(19) Fe
O1 0.0248(9) 0.0359(10) 0.0253(9) 0.0002(7) 0.0019(7) -0.0204(8) O
O2 0.0153(8) 0.0287(9) 0.0207(8) 0.0051(6) -0.0072(6) -0.0129(7) O
O3 0.0161(8) 0.0333(9) 0.0258(9) 0.0059(7) -0.0043(7) -0.0196(8) O
O4 0.0231(8) 0.0308(9) 0.0272(9) 0.0051(7) -0.0134(7) -0.0147(7) O
O5 0.0174(8) 0.0381(10) 0.0195(8) 0.0021(7) -0.0050(6) -0.0124(7) O
O6 0.0180(8) 0.0235(8) 0.0233(8) -0.0013(6) -0.0061(6) -0.0103(7) O
C1 0.0151(10) 0.0191(11) 0.0167(10) -0.0034(9) -0.0001(8) -0.0070(9) C
C2 0.0142(10) 0.0175(10) 0.0177(10) -0.0009(8) -0.0013(8) -0.0075(9) C
C3 0.0134(10) 0.0186(11) 0.0187(11) -0.0015(8) -0.0025(8) -0.0082(9) C
C4 0.0165(11) 0.0184(11) 0.0194(11) -0.0016(9) -0.0024(8) -0.0084(9) C
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_refinement_flags
_atom_site_type_symbol
Fe 0.00000 0.00000 0.00000 0.0174(3) Uani S Fe
O1 -0.2615(3) 0.0862(2) 0.19066(19) 0.0278(10) Uani . O
O2 -0.1897(3) 0.1254(2) 0.53281(18) 0.0214(9) Uani . O
O3 -0.7711(3) 0.4117(2) 0.53689(18) 0.0241(9) Uani . O
O4 -0.8495(3) 0.3801(2) 0.19112(19) 0.0260(9) Uani . O
O5 0.2673(3) -0.1775(2) 0.16862(18) 0.0254(10) Uani . O
O6 -0.1909(3) -0.2555(2) 0.06518(18) 0.0209(9) Uani . O
C1 -0.3965(4) 0.1816(3) 0.2792(3) 0.0171(11) Uani . C
C2 -0.3689(4) 0.2009(3) 0.4323(3) 0.0167(11) Uani . C
C3 -0.6291(4) 0.3283(3) 0.4359(3) 0.0167(11) Uani . C
C4 -0.6668(4) 0.3156(3) 0.2802(3) 0.0179(11) Uani . C
H1 0.000 0.000 0.500 0.063(13) Uiso S H
H2 -1.000 0.500 0.500 0.15(3) Uiso S H
H3 0.227 -0.160 0.274 0.052(9) Uiso . H
H4 0.454 -0.227 0.139 0.092(13) Uiso . H
H5 -0.171 -0.290 -0.032 0.047(8) Uiso . H
H6 -0.096 -0.367 0.146 0.073(11) Uiso . H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe 0.301 0.845 'International Tables Vol. IV Table 2.2B'
C 0.002 0.002 'International Tables Vol. IV Table 2.2B'
O 0.008 0.006 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 0 0
0 5 0
0 0 5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Fe O1 ? 2_555 180.0 no
O1 Fe O5 ? ? 89.29(6) no
O1 Fe O5 ? 2_555 90.71(6) no
O1 Fe O6 ? ? 90.74(6) no
O1 Fe O6 ? 2_555 89.26(6) no
O1 Fe O5 2_555 ? 90.71(6) no
O1 Fe O5 2_555 2_555 89.29(6) no
O1 Fe O6 2_555 ? 89.26(6) no
O1 Fe O6 2_555 2_555 90.74(6) no
O5 Fe O5 ? 2_555 179.9 no
O5 Fe O6 ? ? 88.89(6) no
O5 Fe O6 ? 2_555 91.11(6) no
O5 Fe O6 2_555 ? 91.11(6) no
O5 Fe O6 2_555 2_555 88.89(6) no
O6 Fe O6 ? 2_555 180.0 no
Fe O1 C1 ? ? 164.15(15) no
C2 O2 H1 ? ? 115.29(14) no
C2 O2 H3 ? 2_556 124.53(13) no
H1 O2 H3 ? 2_556 119.38(10) no
C3 O3 H2 ? ? 113.84(14) no
C4 O4 H5 ? 2_455 119.80(14) no
Fe O5 H3 ? ? 115.55(12) no
Fe O5 H4 ? ? 124.81(12) no
H3 O5 H4 ? ? 113.91(15) no
Fe O6 H4 ? 1_455 117.85(7) no
Fe O6 H5 ? ? 109.23(11) no
Fe O6 H6 ? ? 108.17(10) no
H4 O6 H5 1_455 ? 104.80(11) no
H4 O6 H6 1_455 ? 109.01(11) no
H5 O6 H6 ? ? 107.32(14) no
O1 C1 C2 ? ? 135.84(19) no
O1 C1 C4 ? ? 135.32(19) no
C2 C1 C4 ? ? 88.74(16) no
O2 C2 C1 ? ? 134.84(18) no
O2 C2 C3 ? ? 133.10(18) no
C1 C2 C3 ? ? 91.96(16) no
O3 C3 C2 ? ? 134.22(19) no
O3 C3 C4 ? ? 135.38(19) no
C2 C3 C4 ? ? 90.36(16) no
O4 C4 C1 ? ? 135.05(19) no
O4 C4 C3 ? ? 135.92(19) no
C1 C4 C3 ? ? 88.95(16) no
O2 H1 O2 ? 2_556 179.9 no
O3 H2 O3 ? 2_366 180.0 no
O2 H3 O5 2_556 ? 173.86(10) no
O2 H3 H4 2_556 ? 141.44(5) no
O5 H3 H4 ? ? 32.91(9) no
O5 H4 O6 ? 1_655 165.62(11) no
O5 H4 H3 ? ? 33.17(9) no
O6 H4 H3 1_655 ? 142.97(5) no
O4 H5 O6 2_455 ? 172.76(10) no
O4 H5 H6 2_455 ? 139.07(5) no
O6 H5 H6 ? ? 36.19(9) no
O6 H6 H5 ? ? 36.49(9) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe O1 2.1002(15) no
Fe O5 2.0614(15) no
Fe O6 2.1815(15) no
O1 C1 1.233(3) no
O2 C2 1.284(3) no
O2 H1 1.2289(14) no
O3 C3 1.268(2) no
O3 H2 1.2349(14) no
O4 C4 1.235(3) no
O5 H3 0.9585(15) no
O5 H4 0.9519(15) no
O6 H5 0.9585(14) no
O6 H6 0.9519(15) no
C1 C2 1.448(3) no
C1 C4 1.484(3) no
C2 C3 1.425(3) no
C3 C4 1.465(3) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O2 H3 1.7713(14) 2_556 no
O4 H5 1.7458(15) 2_455 no
O6 H4 1.7876(15) 1_455 no
H3 H4 1.6014(3) ? no
H4 O6 1.7876(15) 1_655 no
H5 H6 1.5389(3) ? no
