#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:12:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178940 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/69/4116912.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_4116912
loop_
_publ_author_name
'M. Matzapetakis'
'C. P. Raptopoulou'
'A. Tsohos'
'V. Papaefthymiou'
'N. Moon'
'A. Salifoglou'
_publ_section_title
;
 Synthesis, Spectroscopic and Structural Characterization of the First
 Mononuclear, Water Soluble Iron-Citrate Complex, (NH4)5Fe(C6H4O7)2.2H2O
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13266
_journal_page_last               13267
_journal_paper_doi               10.1021/ja9807035
_journal_volume                  120
_journal_year                    1998
_chemical_formula_analytical     '[(NH4)5Fe(C6H4O7)2]2H2O'
_chemical_formula_structural     '[(NH4)5Fe(citrate)2]2H2O'
_chemical_formula_sum            'C12 H32 Fe N5 O16'
_chemical_formula_weight         558.27
_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
_cell_angle_alpha                90.93(2)
_cell_angle_beta                 105.69(2)
_cell_angle_gamma                118.58(2)
_cell_formula_units_Z            1
_cell_length_a                   9.669(7)
_cell_length_b                   9.714(7)
_cell_length_c                   7.265(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      6.5
_cell_volume                     568.3(7)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scan'
_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  0.0096
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2192
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      1.61
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             293
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.243(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_obs          0.0304
_refine_ls_shift/esd_max         0.046
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0217P)²+0.4719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_obs         0.0816
_reflns_number_observed          1981
_reflns_number_total             2017
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9807035.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+0.4719P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0217P)^2^+0.4719P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        568.2(7)
_cod_database_code               4116912
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Fe Fe 0.0000 0.0000 0.0000 0.0200(2) Uani 1 d S
O1 O -0.0041(2) 0.1974(2) -0.0972(2) 0.0304(3) Uani 1 d .
O3 O 0.1939(2) 0.14392(15) 0.2196(2) 0.0218(3) Uani 1 d .
O4 O 0.4016(2) 0.2533(2) -0.1380(3) 0.0441(4) Uani 1 d .
C1 C 0.1094(2) 0.3444(2) -0.0497(3) 0.0246(4) Uani 1 d .
O2 O 0.0879(2) 0.4504(2) -0.1204(2) 0.0405(4) Uani 1 d .
C2 C 0.2755(2) 0.3932(2) 0.1008(3) 0.0250(4) Uani 1 d .
C3 C 0.3142(2) 0.2585(2) 0.1443(3) 0.0211(4) Uani 1 d .
C4 C 0.3026(2) 0.1795(2) -0.0510(3) 0.0256(4) Uani 1 d .
O5 O 0.1760(2) 0.0398(2) -0.1223(2) 0.0313(4) Uani 1 d .
C5 C 0.4882(2) 0.3311(2) 0.2921(3) 0.0290(5) Uani 1 d .
C6 C 0.5544(3) 0.2173(3) 0.3393(3) 0.0320(5) Uani 1 d .
O6 O 0.6614(3) 0.2534(3) 0.5026(3) 0.0603(6) Uani 1 d .
O7 O 0.5113(3) 0.1051(2) 0.2125(4) 0.0679(7) Uani 1 d .
N2 N 0.2951(3) -0.2276(3) 0.0931(4) 0.0399(5) Uani 1 d .
N1 N 0.2285(3) -0.0317(3) -0.4850(3) 0.0413(5) Uani 1 d .
OW O 0.1221(4) 0.2612(3) 0.5022(4) 0.0606(6) Uani 1 d .
N3 N 0.0000 0.5000 0.5000 0.075(2) Uani 1 d S
H2A H 0.3560(32) 0.4721(31) 0.0654(36) 0.031(6) Uiso 1 d .
H2B H 0.2768(28) 0.4388(28) 0.2212(37) 0.027(6) Uiso 1 d .
H5A H 0.4852(28) 0.3757(28) 0.4130(36) 0.027(6) Uiso 1 d .
H5B H 0.5668(35) 0.4174(34) 0.2463(40) 0.041(7) Uiso 1 d .
HN1A H 0.2796(44) -0.0902(43) -0.4851(51) 0.067(10) Uiso 1 d .
HN1B H 0.2679(53) 0.0288(53) -0.3813(72) 0.092(14) Uiso 1 d .
HN1C H 0.2328(38) 0.0247(38) -0.5832(51) 0.053(8) Uiso 1 d .
HN1D H 0.1203(53) -0.0966(46) -0.4936(54) 0.074(11) Uiso 1 d .
HN2A H 0.2215(51) -0.3233(52) 0.0156(61) 0.079(11) Uiso 1 d .
HN2B H 0.2338(60) -0.1862(56) 0.0664(68) 0.100(15) Uiso 1 d .
HN2C H 0.3799(68) -0.1797(62) 0.0614(80) 0.119(18) Uiso 1 d .
HN2D H 0.3293(46) -0.2248(43) 0.2217(64) 0.071(11) Uiso 1 d .
HN3A H 0.0242(82) 0.4911(78) 0.6023(100) 0.044(19) Uiso 0.50 d P
HN3B H 0.0784(62) 0.5477(64) 0.4970(86) 0.027(16) Uiso 0.50 d P
HOWA H 0.1492(46) 0.2233(44) 0.4078(59) 0.077(11) Uiso 1 d .
HOWB H 0.0755(50) 0.2902(50) 0.4404(60) 0.071(15) Uiso 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'
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'
N N 0.0061 0.0033 '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
O3 Fe O3 180.0 . 2
O3 Fe O5 98.14(8) . 2
O3 Fe O5 81.86(8) 2 2
O3 Fe O5 81.86(8) . .
O3 Fe O5 98.14(8) 2 .
O5 Fe O5 180.0 2 .
O3 Fe O1 91.83(7) . 2
O3 Fe O1 88.17(7) 2 2
O5 Fe O1 88.69(7) 2 2
O5 Fe O1 91.31(7) . 2
O3 Fe O1 88.17(7) . .
O3 Fe O1 91.83(7) 2 .
O5 Fe O1 91.31(7) 2 .
O5 Fe O1 88.69(7) . .
O1 Fe O1 180.0 2 .
C1 O1 Fe 129.66(13) . .
C3 O3 Fe 107.79(11) . .
O2 C1 O1 122.2(2) . .
O2 C1 C2 118.0(2) . .
O1 C1 C2 119.8(2) . .
C1 C2 C3 115.9(2) . .
O3 C3 C5 110.6(2) . .
O3 C3 C2 109.4(2) . .
C5 C3 C2 108.3(2) . .
O3 C3 C4 109.26(15) . .
C5 C3 C4 112.0(2) . .
C2 C3 C4 107.2(2) . .
O4 C4 O5 122.9(2) . .
O4 C4 C3 121.1(2) . .
O5 C4 C3 115.8(2) . .
C4 O5 Fe 110.13(13) . .
C6 C5 C3 115.7(2) . .
O7 C6 O6 124.4(2) . .
O7 C6 C5 119.3(2) . .
O6 C6 C5 116.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe O3 1.953(2) .
Fe O3 1.953(2) 2
Fe O5 2.008(2) 2
Fe O5 2.008(2) .
Fe O1 2.068(2) 2
Fe O1 2.068(2) .
O1 C1 1.281(3) .
O3 C3 1.419(2) .
O4 C4 1.231(3) .
C1 O2 1.237(3) .
C1 C2 1.518(3) .
C2 C3 1.539(3) .
C3 C5 1.531(3) .
C3 C4 1.553(3) .
C4 O5 1.286(3) .
C5 C6 1.523(3) .
C6 O7 1.239(3) .
C6 O6 1.256(3) .
