#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/85/2018519.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_2018519
loop_
_publ_author_name
'Schmidt, Horst'
'Asztalos, Annifrid'
'Bok, Frank'
'Voigt, Wolfgang'
_publ_section_title
;
 New iron(III) nitrate hydrates: Fe(NO₃)₃·xH₂O with
 x = 4, 5 and 6
;
_journal_coeditor_code           YP3012
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i29
_journal_page_last               i33
_journal_paper_doi               10.1107/S0108270112015855
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Fe (H2 O1)6] (N O3)3'
_chemical_formula_moiety         'N3 O9 Fe, 6(H2 O)'
_chemical_formula_sum            'Fe H12 N3 O15'
_chemical_formula_weight         349.98
_chemical_melting_point          317.68
_chemical_name_common            'iron nitrate hexahydrate'
_chemical_name_systematic        'hexaaquairon(III) trinitrate'
_space_group_IT_number           206
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7962(2)
_cell_length_b                   13.7962(2)
_cell_length_c                   13.7962(2)
_cell_measurement_reflns_used    692
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.8
_cell_volume                     2625.90(7)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Kappa APEXII'
_diffrn_measurement_method       'ω and φ 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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0087
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9913
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.7149
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(APEX2; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         505
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0278
_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)+(0.0420P)²+3.9345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                432
_reflns_number_total             505
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL data_feno3_3_6h2o
CELL 0.71073  13.7962  13.7962  13.7962  90.000  90.000  90.000
ZERR   8.00   0.0021   0.0021   0.0021   0.000   0.000   0.000
LATT 2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SFAC Fe H  N  O
UNIT 8  96  24  120
OMIT -3 55
L.S. 10
ACTA
Bond lengths and angles
FMAP 2
PLAN -1
EQIV $1 -z+1, -x+3/2, y
HTAB O1 O3_$1
HTAB O1 O3
HTAB O1 O2
HTAB O1 N1
SIZE 0.292 0.350 0.425
DANG 1.3 0.02 H1 H2
DFIX 0.82 0.005 O1 H2  O1 H1
WGHT   0.042000   3.934500
FVAR 0.070380
TEMP 23.000
MOLE 2
Fe1    1   0.500000   0.500000   0.500000  10.166670   0.015260 =
           0.015260   0.015260  -0.000360  -0.000360  -0.000360
N1     3   0.713417   0.500000   0.250000  10.500000   0.023560 =
           0.051960   0.022780  -0.004460   0.000000   0.000000
O1     4   0.625587   0.560879   0.463676  11.000000   0.020110 =
           0.019980   0.025560  -0.003880   0.006270  -0.003890
O2     4   0.626078   0.500000   0.250000  10.500000   0.023660 =
           0.166710   0.036330  -0.019610   0.000000   0.000000
O3     4   0.757971   0.518653   0.326354  11.000000   0.027760 =
           0.082660   0.031120  -0.021320  -0.009130   0.014650
H1     2   0.635216   0.618047   0.475013  11.000000   0.050140
H2     2   0.660202   0.543062   0.419251  11.000000   0.054960
HKLF 4
END
Q1     1   0.250000   0.250000   0.250000  10.166670   0.050000 0.580000
HKLF 4
REM  data_feno3_3_6h2o
REM R1=  0.0278 for    432 Fo > 4sig(Fo)  and  0.0338 for all    505 data
REM     39 parameters refined using      3 restraints
;
_cod_data_source_file            yp3012.cif
_cod_data_source_block           I
_cod_database_code               2018519
_cod_database_fobs_code          2018519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.5000 0.5000 0.5000 0.0153(2) Uani d S 1 6
N N1 0.71342(19) 0.5000 0.2500 0.0328(6) Uani d S 1 2
O O1 0.62559(9) 0.56088(9) 0.46368(9) 0.0219(3) Uani d D 1 1
O O2 0.62608(19) 0.5000 0.2500 0.0756(11) Uani d S 1 2
O O3 0.75797(11) 0.51865(15) 0.32635(12) 0.0472(5) Uani d . 1 1
H H1 0.6352(19) 0.6180(6) 0.4750(18) 0.050(8) Uiso d D 1 1
H H2 0.6602(16) 0.5431(18) 0.4193(14) 0.055(9) Uiso d D 1 1
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
Fe1 0.0153(2) 0.0153(2) 0.0153(2) -0.00036(11) -0.00036(11) -0.00036(11)
N1 0.0236(13) 0.0520(16) 0.0228(12) 0.000 0.000 -0.0045(10)
O1 0.0201(6) 0.0200(6) 0.0256(7) -0.0039(5) 0.0063(5) -0.0039(5)
O2 0.0237(12) 0.167(4) 0.0363(14) 0.000 0.000 -0.0196(17)
O3 0.0278(8) 0.0827(14) 0.0311(9) 0.0146(7) -0.0091(6) -0.0213(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'
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
O1 Fe1 O1 9 . 87.60(5)
O1 Fe1 O1 9 33_666 180.0
O1 Fe1 O1 . 33_666 92.40(5)
O1 Fe1 O1 9 5 87.60(5)
O1 Fe1 O1 . 5 87.60(5)
O1 Fe1 O1 33_666 5 92.40(5)
O1 Fe1 O1 9 29_666 92.40(5)
O1 Fe1 O1 . 29_666 92.40(5)
O1 Fe1 O1 33_666 29_666 87.60(5)
O1 Fe1 O1 5 29_666 180.00(6)
O1 Fe1 O1 9 25_666 92.40(5)
O1 Fe1 O1 . 25_666 180.00(6)
O1 Fe1 O1 33_666 25_666 87.60(5)
O1 Fe1 O1 5 25_666 92.40(5)
O1 Fe1 O1 29_666 25_666 87.60(5)
O2 N1 O3 . . 119.55(13)
O2 N1 O3 . 16_455 119.55(13)
O3 N1 O3 . 16_455 120.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 O1 9 1.9896(12)
Fe1 O1 . 1.9896(12)
Fe1 O1 33_666 1.9896(12)
Fe1 O1 5 1.9896(12)
Fe1 O1 29_666 1.9896(12)
Fe1 O1 25_666 1.9896(12)
N1 O2 . 1.205(4)
N1 O3 . 1.246(2)
N1 O3 16_455 1.246(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H2 O3 . 0.815(5) 1.891(8) 2.695(2) 169(3)
O1 H1 O3 19_564 0.815(5) 1.889(7) 2.6946(19) 169(3)
