New Lead Inorganic-Organic Hybrid Microporous and Layered Materials: Synthesis, Properties, and Crystal Structures
Jiang-Gao Mao; Zhike Wang; Abraham Clearfield; Inorganic Chemistry 41 (2002) 6106–6111; doi:10.1021/ic020396a

data_4318831
_publ_section_title
;
 New Lead Inorganic-Organic Hybrid Microporous and Layered Materials:
 Synthesis, Properties, and Crystal Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6106
_journal_page_last               6111
_journal_paper_doi               10.1021/ic020396a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C5 H9 N O8.5 P Pb2'
_chemical_formula_weight         664.48
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.317(7)
_cell_length_b                   17.317(7)
_cell_length_c                   7.507(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2251(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'hemisphere, narrow frame method'
_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  0.1071
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13225
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    30.054
_exptl_absorpt_correction_T_max  0.493
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.665
_refine_diff_density_min         -2.137
_refine_diff_density_rms         0.653
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0789P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                1902
_reflns_number_total             2635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020396a_1.cif
_cod_data_source_block           maoc16
_cod_original_cell_volume        2251.1(19)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C5 H9 N O8.50 P Pb2'
_cod_database_code               4318831