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_4330160
_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            'C18 H25 N3 O9 Pb'
_chemical_formula_weight         634.61
_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                98.16(3)
_cell_angle_beta                 94.54(3)
_cell_angle_gamma                95.00(3)
_cell_formula_units_Z            2
_cell_length_a                   7.108(6)
_cell_length_b                   9.965(7)
_cell_length_c                   15.570(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      5.5
_cell_volume                     1082.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       '\q/2\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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3937
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.241
_refine_diff_density_min         -2.804
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.065(3)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0519
_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^)+(0.1180P)^2^+0.6824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                3535
_reflns_number_total             3784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300850g_si_002.cif
_cod_data_source_block           salpb247
_cod_database_code               4330160