Chelate Complexes of Lead(II) with Nitrilotris(methylenephosphonic) Acid [Pb{5-NH(CH2PO3H)3}] and Na4[Pb2(H2O)2{3-N(CH2PO3)3H2}2] 10H2O: Synthesis, Structure, and Asymmetry of Lone 6s Pair
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Reshetnikov, S.M.; Shishkin, A.S.; Shumilova, M.A.; Aleksandrov, V.A.; Petrov, V.G.; Crystallography Reports 62 (2017) 857–867; doi:10.1134/S1063774517050224

data_1564826
_publ_section_title
;
 Chelate Complexes of Lead(II) with Nitrilotris(methylenephosphonic) Acid
 [Pb{5-NH(CH2PO3H)3}] and Na4[Pb2(H2O)2{3-N(CH2PO3)3H2}2] 10H2O:
 Synthesis, Structure, and Asymmetry of Lone 6s Pair
;
_journal_issue                   6
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              857
_journal_page_last               867
_journal_paper_doi               10.1134/S1063774517050224
_journal_volume                  62
_journal_year                    2017
_chemical_formula_sum            'C6 H40 N2 Na4 O30 P6 Pb2'
_chemical_formula_weight         1312.56
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-12-17T15:25:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                65.885(3)
_cell_angle_beta                 82.401(2)
_cell_angle_gamma                83.143(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8942(3)
_cell_length_b                   13.1882(4)
_cell_length_c                   14.0016(4)
_cell_measurement_reflns_used    19244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.945
_cell_measurement_theta_min      3.37
_cell_volume                     1815.23(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.024172
_diffrn_orient_matrix_UB_12      -0.0328228
_diffrn_orient_matrix_UB_13      -0.0215757
_diffrn_orient_matrix_UB_21      0.0564791
_diffrn_orient_matrix_UB_22      0.0015988
_diffrn_orient_matrix_UB_23      -0.0320831
_diffrn_orient_matrix_UB_31      0.023726
_diffrn_orient_matrix_UB_32      -0.0490971
_diffrn_orient_matrix_UB_33      0.0401481
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.106
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.677
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         12373
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+1.1003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0
_reflns_number_gt                10956
_reflns_number_total             12373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp_u_hczeo
_cod_data_source_block           pbatmp
_cod_database_code               1564826