Tribasic Lead Maleate and Lead Maleate: Synthesis and Structural and Spectroscopic Characterizations
François Bonhomme; Todd M. Alam; Aaron J. Celestian; David R. Tallant; Timothy J. Boyle; Brian R. Cherry; Ralph G. Tissot; Mark A. Rodriguez; John B. Parise; May Nyman; Inorganic Chemistry 44 (2005) 7394–7402; doi:10.1021/ic050611y

data_4309744
_publ_contact_author
;
Ralph G. Tissot
PO Box 5800
MS 1411
Sandia National Laboratories
Albuquerque, New Mexico  87185-1411  USA
;
_publ_contact_author_email       rgtisso@sandia.gov
_publ_contact_author_fax         1-505-844-9781
_publ_contact_author_phone       1-505-844-4187
_publ_section_title
;
Tribasic Lead Maleate and Lead Maleate: Synthesis and Structural and
Spectroscopic Characterizations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7394
_journal_page_last               7402
_journal_paper_doi               10.1021/ic050611y
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C4 H2 O4 Pb1'
_chemical_formula_sum            'C4 H2 O4 Pb'
_chemical_formula_weight         321.2
_chemical_name_common            'Lead maleate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.094(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.920(3)
_cell_length_b                   6.9793(18)
_cell_length_c                   8.293(2)
_cell_measurement_reflns_used    1724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.309
_cell_measurement_theta_min      7.321
_cell_volume                     535.7(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker P4 '
_diffrn_measurement_method       'Bruker SMART 1000 CCD'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3739
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    31.421
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.009
_refine_diff_density_max         2.437
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.338
_refine_ls_extinction_coef       0.0040(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+2.3334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                1034
_reflns_number_total             1242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050611ysi20050420_112447_1.cif
_cod_data_source_block           pbmal
_cod_original_formula_sum        'C4 H2 O4 Pb1'
_cod_database_code               4309744