Synthesis and Structure of Heptaaqua{nitrilotris(methylenephosphonato)}(dibarium)sodium Monohydrate [Na(H2O)3{6-NH(CH2PO3)3}(-H2O)3Ba2(H2O)] H2O
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Crystallography Reports 62 (2017) 232–237; doi:10.1134/S1063774517020262

data_1564822
_publ_section_title
;
 Synthesis and Structure of
 Heptaaqua{nitrilotris(methylenephosphonato)}(dibarium)sodium Monohydrate
 [Na(H2O)3{6-NH(CH2PO3)3}(-H2O)3Ba2(H2O)] H2O
;
_journal_issue                   2
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              232
_journal_page_last               237
_journal_paper_doi               10.1134/S1063774517020262
_journal_volume                  62
_journal_year                    2017
_chemical_formula_sum            'C3 H23 Ba2 N Na O17 P3'
_chemical_formula_weight         735.8
_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             2015-06-11T09:57:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 148.785(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9117(10)
_cell_length_b                   11.54030(10)
_cell_length_c                   24.1784(17)
_cell_measurement_reflns_used    14704
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.614
_cell_measurement_theta_min      3.69
_cell_volume                     2011.7(6)
_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      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0302
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.062235
_diffrn_orient_matrix_UB_12      -0.0376596
_diffrn_orient_matrix_UB_13      -0.0167325
_diffrn_orient_matrix_UB_21      0.0723827
_diffrn_orient_matrix_UB_22      -0.0409807
_diffrn_orient_matrix_UB_23      0.0391453
_diffrn_orient_matrix_UB_31      0.0238074
_diffrn_orient_matrix_UB_32      0.0260818
_diffrn_orient_matrix_UB_33      0.0373096
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.229
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   analytical
_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)
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    2.429
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.1403
_exptl_crystal_size_mid          0.0926
_exptl_crystal_size_min          0.0252
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6141
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0265P)^2^+0.8259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0
_reflns_number_gt                5347
_reflns_number_total             6141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmpeyq3z2_2
_cod_data_source_block           3_banaatmp
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564822