Two novel lead(II) carboxyphosphonates with a layered and a 3D framework structure: syntheses, crystal structures, reversible dehydration/hydration, and luminescence properties.
Chu, Wei; Sun, Zhen-Gang; Jiao, Cheng-Qi; Zhu, Yan-Yu; Sun, Shou-Hui; Tian, Hui; Zheng, Ming-Jing; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8009–8017; doi:10.1039/c3dt00125c

data_7022591
_publ_section_title
;
 Two novel lead(II) carboxyphosphonates with a layered and a 3D framework
 structure: syntheses, crystal structures, reversible
 dehydration/hydration, and luminescence properties.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8009
_journal_page_last               8017
_journal_paper_doi               10.1039/c3dt00125c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C16 H16 N O11 P Pb2'
_chemical_formula_weight         843.65
_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                102.497(3)
_cell_angle_beta                 92.402(3)
_cell_angle_gamma                99.285(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7505(13)
_cell_length_b                   9.3424(19)
_cell_length_c                   16.747(3)
_cell_measurement_reflns_used    1052
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.27
_cell_volume                     1014.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Smart Apex II CCD'
_diffrn_measurement_method       'omega 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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5425
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.716
_exptl_absorpt_correction_T_max  0.7204
_exptl_absorpt_correction_T_min  0.3670
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.930
_refine_diff_density_min         -2.830
_refine_diff_density_rms         0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+3.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                2629
_reflns_number_total             4057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt00125c.txt
_cod_data_source_block           szg196
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1014.4(4)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7022591