A novel luminescent Pb(II) - organic framework exhibiting rapid and selective detection of trace amount of NACs and Fe3+ with excellent recyclability
Luo, Xuan; Zhang, Xiao; Duan, Yuanling; Wang, Xiaolin; Zhao, Jiaming; Dalton Trans.  (2017) –; doi:10.1039/C7DT00715A

data_7042702
_publ_section_title
;
 A novel luminescent Pb(II) - organic framework exhibiting rapid and
 selective detection of trace amount of NACs and Fe3+ with excellent
 recyclability
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00715A
_journal_year                    2017
_chemical_formula_moiety         '0.25(C28 H16 N16 O12 Pb12)'
_chemical_formula_sum            'C7 H4 N4 O3 Pb3'
_chemical_formula_weight         813.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2288(3)
_cell_length_b                   21.6436(6)
_cell_length_c                   5.79719(18)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6840
_cell_measurement_theta_min      3.9710
_cell_volume                     1157.96(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9737
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  87.00   1.00    8.79    --   18.81  19.00  90.00  114
  2  \w    -72.00 -46.00   1.00    8.79    --  -19.74 130.00 -69.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0212645000
_diffrn_orient_matrix_UB_12      0.0297060000
_diffrn_orient_matrix_UB_13      -0.0392058000
_diffrn_orient_matrix_UB_21      0.0737762000
_diffrn_orient_matrix_UB_22      -0.0081297000
_diffrn_orient_matrix_UB_23      0.0155569000
_diffrn_orient_matrix_UB_31      0.0027760000
_diffrn_orient_matrix_UB_32      -0.0112022000
_diffrn_orient_matrix_UB_33      -0.1148967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1335
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.340
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         3.585
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    43.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.00133(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                553
_reflns_number_total             620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00715a2.cif
_cod_data_source_block           160616-27-2
_cod_database_code               7042702
_chemical_oxdiff_formula         'C cH N O Pb'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C2(0.5) H2(0.5) C3(0.5) H3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
;
_shelx_res_checksum              90601
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.486
_oxdiff_exptl_absorpt_empirical_full_min 0.559