Holo- and Hemidirected Lead(II) in the Polymeric [Pb4(μ-3,4-TDTA)2(H2O)2].4H2O Complex. N,N,N',N'-Tetraacetate Ligands Derived fromo-Phenylenediamines as Sequestering Agents for Lead(II)
Joaquín Sanchiz; Pedro Esparza; Diego Villagra; Sixto Domínguez; Alfredo Mederos; Felipe Brito; Lorena Araujo; Agustin Sánchez; Juan Manuel Arrieta; Inorganic Chemistry 41 (2002) 6048–6055; doi:10.1021/ic0201304

data_4318810
_publ_section_title
;
 Holo- and Hemidirected Lead(II) in the Polymeric
 [Pb4(\m-3,4-TDTA)2(H2O)2].4H2O Complex. N,N,N',N'-Tetraacetate Ligands
 Derived fromo-Phenylenediamines as Sequestering Agents for Lead(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6048
_journal_page_last               6055
_journal_paper_doi               10.1021/ic0201304
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H20 N2 O11 Pb2'
_chemical_formula_weight         818.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.410(10)
_cell_angle_beta                 75.26(2)
_cell_angle_gamma                69.61(2)
_cell_formula_units_Z            2
_cell_length_a                   8.911(3)
_cell_length_b                   9.601(2)
_cell_length_c                   13.052(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      5.
_cell_volume                     992.1(4)
_computing_cell_refinement       cad4
_computing_data_collection       cad4
_computing_data_reduction        xtal
_computing_molecular_graphics    ortep
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Cad4
_diffrn_measurement_method       'omega/2theta scans (0.8+0.35tg(theta))'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12301
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '1 hour'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.011
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prismatic Triangular'
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2mm
_refine_diff_density_max         2.602
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.134
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4912
_reflns_number_total             5781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201304.cif
_cod_data_source_block           plomo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.8955P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        ' C15 H20 N2 O11 Pb2'
_cod_database_code               4318810