Synthesis, Structure, and Properties of Nitrilo-tris(methylenephosphonato)-triaquairon(II) {Fe[μ-NH(CH2PO3H)3](H2O)3}, as an Ingredient of Anticorrosive Protective Coatings on the Steel Surface
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Shumilova, M.A.; Aleksandrov, V.A.; Petrov, V.G.; Crystallography Reports 60 (2015) 853–859; doi:10.1134/S1063774515060334

data_1564814
_publ_section_title
;
 Synthesis, Structure, and Properties of
 Nitrilo-tris(methylenephosphonato)-triaquairon(II)
 {Fe[\m-NH(CH2PO3H)3](H2O)3}, as an Ingredient of
 Anticorrosive Protective Coatings on the Steel Surface
;
_journal_issue                   6
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              853
_journal_page_last               859
_journal_paper_doi               10.1134/S1063774515060334
_journal_volume                  60
_journal_year                    2015
_chemical_formula_sum            'C3 H16 Fe N O12 P3'
_chemical_formula_weight         406.93
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2014-11-20T15:33:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 115.685(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2619(3)
_cell_length_b                   16.0548(3)
_cell_length_c                   9.7570(3)
_cell_measurement_reflns_used    21665
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.132
_cell_measurement_theta_min      4.074
_cell_volume                     1307.49(8)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0302
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0713124
_diffrn_orient_matrix_UB_12      0.0216777
_diffrn_orient_matrix_UB_13      0.0463984
_diffrn_orient_matrix_UB_21      -0.0461997
_diffrn_orient_matrix_UB_22      0.0331369
_diffrn_orient_matrix_UB_23      0.0082095
_diffrn_orient_matrix_UB_31      0.0006549
_diffrn_orient_matrix_UB_32      -0.019559
_diffrn_orient_matrix_UB_33      0.0655189
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27012
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.1244
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0
_reflns_number_gt                3864
_reflns_number_total             3963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp.cif
_cod_data_source_block           fe(ii)
_cod_original_cell_volume        1307.49(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564814