Ultrasonic-assisted synthesis of nano-structured lead(II) coordination polymers as precursors for preparation of lead(II) oxide nanoparticles
Morsalia, Ali; Panjehpour, Akram; Inorganica Chimica Acta 391 (2012) 210–217; doi:10.1016/j.ica.2012.04.024

data_1508137
_publ_section_title
;
 Ultrasonic-assisted synthesis of nano-structured lead(II) coordination
 polymers as precursors for preparation of lead(II) oxide nanoparticles
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              210
_journal_page_last               217
_journal_paper_doi               10.1016/j.ica.2012.04.024
_journal_volume                  391
_journal_year                    2012
_chemical_formula_moiety         'C21 H16 N8 O9 Pb2'
_chemical_formula_sum            'C21 H16 N8 O9 Pb2'
_chemical_formula_weight         938.82
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.9210(10)
_cell_angle_beta                 88.2860(10)
_cell_angle_gamma                72.9450(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1006(4)
_cell_length_b                   10.2621(6)
_cell_length_c                   16.5790(9)
_cell_measurement_reflns_used    8667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.69
_cell_measurement_theta_min      2.58
_cell_volume                     1257.10(12)
_computing_cell_refinement       'SAINTPlus, v. 6.2 (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINTPlus, v. 6.2 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16064
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    13.444
_exptl_absorpt_correction_T_max  0.162
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.516
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                6109
_reflns_number_total             7313
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            PB75.CIF
_cod_data_source_block           Pb-75
_cod_database_code               1508137