Nitrilotris(methylenephosphonato)potassium K[6-NH(CH2PO3)3H4]: Synthesis, Structure, and the Nature of the KO Chemical Bond
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Crystallography Reports 61 (2016) 606–610; doi:10.1134/S1063774516040209

data_1564820
_publ_section_title
;
 Nitrilotris(methylenephosphonato)potassium K[6-NH(CH2PO3)3H4]: Synthesis,
 Structure, and the Nature of the KO Chemical Bond
;
_journal_issue                   4
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              606
_journal_page_last               610
_journal_paper_doi               10.1134/S1063774516040209
_journal_volume                  61
_journal_year                    2016
_chemical_formula_sum            'C3 H11 K N O9 P3'
_chemical_formula_weight         337.14
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_space_group_name_Hall           '-P 1'
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_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   difmap
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_cell_angle_alpha                85.396(4)
_cell_angle_beta                 89.884(4)
_cell_angle_gamma                73.999(4)
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_cell_length_a                   6.2553(3)
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_cell_measurement_temperature    293(2)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
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        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 0.994
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_21      -0.0460138
_diffrn_orient_matrix_UB_22      -0.0357589
_diffrn_orient_matrix_UB_23      0.0490019
_diffrn_orient_matrix_UB_31      -0.0067278
_diffrn_orient_matrix_UB_32      0.0725713
_diffrn_orient_matrix_UB_33      0.0302309
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_point_group_measured_fraction_full 0.994
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.827
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.789
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;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       prism
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.3656
_exptl_crystal_size_mid          0.2973
_exptl_crystal_size_min          0.1972
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.058(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5756
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.0845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0
_reflns_number_gt                5496
_reflns_number_total             5756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmpvu89zf6h
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