#------------------------------------------------------------------------------
#$Date: 2025-08-19 08:12:48 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301798 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/85/2018521.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_2018521
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 (N O3)2 (H2 O)3] N O3, H2 O'
_chemical_formula_moiety         'Fe H6 N2 O9 +, N O3 -, H2 O'
_chemical_formula_sum            'Fe H8 N3 O13'
_chemical_formula_weight         313.94
_chemical_melting_point          335.39
_chemical_name_common            'iron nitrate tetrahydrate'
_chemical_name_systematic
;
triaquadinitratoiron(III) nitrate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.508(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0696(7)
_cell_length_b                   15.1917(16)
_cell_length_c                   9.4264(7)
_cell_measurement_reflns_used    1424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.8
_cell_volume                     1005.86(16)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11328
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2303
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0216
_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)+(0.0258P)²+0.2256P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                1985
_reflns_number_total             2303
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yp3012.cif
_cod_data_source_block           III
_cod_database_code               2018521
_cod_database_fobs_code          2018521
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.32508(3) 0.404152(14) 0.21984(2) 0.01392(7) Uani d . 1 1
N N1 0.01759(19) 0.38468(9) 0.32872(15) 0.0208(3) Uani d . 1 1
N N2 0.87740(18) 0.61678(9) 0.24763(15) 0.0190(3) Uani d . 1 1
N N3 0.49724(19) 0.34257(9) 0.01723(14) 0.0194(3) Uani d . 1 1
O O1 0.43710(17) 0.30869(7) 0.34377(13) 0.0209(2) Uani d D 1 1
O O2 0.49853(16) 0.49024(7) 0.33518(13) 0.0200(2) Uani d D 1 1
O O3 0.20267(17) 0.49726(8) 0.08999(13) 0.0217(2) Uani d D 1 1
O O4 0.39942(17) 0.65649(8) 0.39764(13) 0.0218(3) Uani d D 1 1
O O5 0.56613(16) 0.40451(7) 0.09934(12) 0.0225(3) Uani d . 1 1
O O6 0.33141(15) 0.31698(7) 0.04514(12) 0.0208(2) Uani d . 1 1
O O7 0.57804(18) 0.31173(8) -0.07625(13) 0.0295(3) Uani d . 1 1
O O8 0.14734(16) 0.44070(8) 0.37318(12) 0.0224(3) Uani d . 1 1
O O9 0.05611(16) 0.34221(8) 0.21746(12) 0.0223(3) Uani d . 1 1
O O10 -0.12433(17) 0.37336(9) 0.38499(15) 0.0327(3) Uani d . 1 1
O O11 0.80194(16) 0.54484(8) 0.20639(13) 0.0247(3) Uani d . 1 1
O O12 1.04023(15) 0.63524(7) 0.20676(13) 0.0228(3) Uani d . 1 1
O O13 0.80185(18) 0.66812(9) 0.32247(14) 0.0326(3) Uani d . 1 1
H H1 0.443(3) 0.2564(5) 0.326(2) 0.048(7) Uiso d D 1 1
H H2 0.496(3) 0.3181(13) 0.4217(11) 0.037(6) Uiso d D 1 1
H H3 0.210(3) 0.4992(14) 0.0045(7) 0.047(7) Uiso d D 1 1
H H4 0.153(3) 0.5409(8) 0.1197(19) 0.035(6) Uiso d D 1 1
H H5 0.454(3) 0.5354(8) 0.365(2) 0.038(6) Uiso d D 1 1
H H6 0.5966(19) 0.5046(14) 0.303(2) 0.054(8) Uiso d D 1 1
H H7 0.452(3) 0.6857(13) 0.3409(19) 0.046(7) Uiso d D 1 1
H H8 0.2855(10) 0.6669(16) 0.382(3) 0.069(9) Uiso d D 1 1
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'
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'
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
O1 Fe1 O3 177.43(5)
O1 Fe1 O2 88.79(5)
O3 Fe1 O2 93.75(5)
O1 Fe1 O8 91.04(5)
O3 Fe1 O8 89.03(5)
O2 Fe1 O8 80.35(5)
O1 Fe1 O6 87.61(5)
O3 Fe1 O6 90.70(5)
O2 Fe1 O6 139.22(4)
O8 Fe1 O6 140.31(4)
O1 Fe1 O9 88.81(5)
O3 Fe1 O9 88.97(5)
O2 Fe1 O9 141.35(5)
O8 Fe1 O9 61.14(4)
O6 Fe1 O9 79.17(4)
O1 Fe1 O5 91.47(5)
O3 Fe1 O5 89.36(5)
O2 Fe1 O5 79.29(4)
O8 Fe1 O5 159.42(4)
O6 Fe1 O5 60.23(4)
O9 Fe1 O5 139.34(4)
O10 N1 O8 123.52(14)
O10 N1 O9 123.62(15)
O8 N1 O9 112.85(12)
O13 N2 O11 122.54(13)
O13 N2 O12 120.09(13)
O11 N2 O12 117.36(13)
O7 N3 O5 123.50(14)
O7 N3 O6 123.49(14)
O5 N3 O6 113.00(12)
N3 O5 Fe1 92.72(8)
N3 O6 Fe1 94.00(8)
N1 O8 Fe1 93.51(8)
N1 O9 Fe1 92.37(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 O1 1.9711(12)
Fe1 O3 2.0019(12)
Fe1 O2 2.0233(11)
Fe1 O8 2.0949(11)
Fe1 O6 2.1176(11)
Fe1 O9 2.1194(11)
Fe1 O5 2.1524(11)
N1 O10 1.1992(17)
N1 O8 1.2862(18)
N1 O9 1.2865(17)
N2 O13 1.2153(18)
N2 O11 1.2582(18)
N2 O12 1.2855(17)
N3 O7 1.1986(17)
N3 O5 1.2791(17)
N3 O6 1.2902(17)
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 H1 O12 2_645 0.815(5) 1.872(6) 2.6858(16) 177(2)
O1 H2 O4 3_666 0.814(5) 1.820(6) 2.6304(17) 173(2)
O3 H3 O11 3_665 0.814(5) 2.090(9) 2.8627(17) 158(2)
O3 H3 O5 3_665 0.814(5) 2.44(2) 2.9572(16) 122(2)
O3 H4 O12 1_455 0.815(5) 1.873(6) 2.6852(17) 173.9(19)
O2 H5 O4 . 0.817(5) 1.912(8) 2.7036(16) 162.9(19)
O2 H6 O11 . 0.817(5) 1.900(6) 2.7117(16) 172(2)
O4 H7 O9 2 0.815(5) 2.440(17) 3.0518(17) 132.7(19)
O4 H7 O7 3_665 0.815(5) 2.480(17) 3.0896(17) 132(2)
O4 H7 O13 . 0.815(5) 2.514(18) 3.0140(17) 120.8(17)
O4 H8 O12 1_455 0.817(5) 2.308(19) 2.9587(17) 137(2)
O4 H8 O6 2 0.817(5) 2.55(2) 3.0163(16) 118(2)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168307957
