pH-Specific Hydrothermal Assembly of Binary and Ternary Pb(II)-(O,N-Carboxylic Acid) Metal Organic Framework Compounds: Correlation of Aqueous Solution Speciation with Variable Dimensionality Solid-State Lattice Architecture and Spectroscopic Signatures
C. Gabriel; M. Perikli; C. P. Raptopoulou; A. Terzis; V. Psycharis; C. Mateescu; T. Jakusch; T. Kiss; M. Bertmer; A. Salifoglou; Inorganic Chemistry 51 (2012) 9282–9296; doi:10.1021/ic300850g

data_4330159
_publ_section_title
;
 pH-Specific Hydrothermal Assembly of Binary and Ternary
 Pb(II)-(O,N-Carboxylic Acid) Metal Organic Framework Compounds:
 Correlation of Aqueous Solution Speciation with Variable Dimensionality
 Solid-State Lattice Architecture and Spectroscopic Signatures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9282
_journal_page_last               9296
_journal_paper_doi               10.1021/ic300850g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C11 H13 N3 O12 Pb3'
_chemical_formula_weight         1000.81
_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                85.3710(10)
_cell_angle_beta                 81.9850(10)
_cell_angle_gamma                77.6700(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0129(3)
_cell_length_b                   10.0591(4)
_cell_length_c                   10.1818(4)
_cell_measurement_reflns_used    19368
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.20
_cell_volume                     891.76(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18687
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    28.322
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1146
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.727
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.000
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+8.1392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                3365
_reflns_number_total             3489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300850g_si_001.cif
_cod_data_source_block           salpb228
_cod_database_code               4330159