#------------------------------------------------------------------------------
#$Date: 2017-04-13 05:21:00 +0300 (Thu, 13 Apr 2017) $
#$Revision: 195406 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042702.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7042702
loop_
_publ_author_name
'Luo, Xuan'
'Zhang, Xiao'
'Duan, Yuanling'
'Wang, Xiaolin'
'Zhao, Jiaming'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  87.00   1.00    8.79    --   18.81  19.00  90.00  114
  2  ω    -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0354P)²] where P=(Fo²+2Fc²)/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 > 2σ(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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.56043(2) 0.7500 0.0173(2) Uani 1 4 d S T P . .
Pb2 Pb 0.75907(4) 0.43868(2) 0.7500 0.0193(2) Uani 1 2 d S T P . .
O1 O 1.0000 0.8906(5) 0.7500 0.029(2) Uani 1 4 d S T P A .
O2 O 0.6481(6) 0.5000 1.0000 0.0185(15) Uani 1 2 d S T P . .
N1 N 0.9311(10) 0.5393(4) 0.7500 0.025(2) Uani 1 2 d S T P . .
N2 N 0.8791(9) 0.5970(4) 0.7500 0.034(2) Uani 1 2 d S T P . .
C1 C 1.0000 0.8303(7) 0.7500 0.024(3) Uani 1 4 d S T P . .
C2 C 0.9038(15) 0.7966(7) 0.883(2) 0.031(4) Uani 0.5 1 d . . . A -1
H2 H 0.8378 0.8176 0.9753 0.037 Uiso 0.5 1 calc R . . A -1
C3 C 0.9020(14) 0.7311(7) 0.884(3) 0.030(4) Uani 0.5 1 d . . . A -1
H3 H 0.8351 0.7098 0.9735 0.036 Uiso 0.5 1 calc R . . A -1
C4 C 1.0000 0.6992(7) 0.7500 0.025(3) Uani 1 4 d S T P . .
C5 C 1.0000 0.6314(7) 0.7500 0.023(3) Uani 1 4 d S T P A .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Pb2 Pb1 Pb2 84.440(17) 3_656 .
O2 Pb1 Pb2 37.64(5) . .
O2 Pb1 Pb2 88.79(9) 10_557 3_656
O2 Pb1 Pb2 88.79(9) 9_667 .
O2 Pb1 Pb2 37.64(5) 2_664 3_656
O2 Pb1 Pb2 88.79(9) . 3_656
O2 Pb1 Pb2 37.64(5) 9_667 3_656
O2 Pb1 Pb2 88.79(9) 2_664 .
O2 Pb1 Pb2 37.64(5) 10_557 .
O2 Pb1 O2 113.43(10) 2_664 .
O2 Pb1 O2 70.0(2) 2_664 10_557
O2 Pb1 O2 74.91(12) 10_557 .
O2 Pb1 O2 74.91(12) 2_664 9_667
O2 Pb1 O2 113.42(10) 10_557 9_667
O2 Pb1 O2 70.0(2) 9_667 .
O1 Pb2 Pb1 71.3(2) 5_445 .
O1 Pb2 N1 149.6(3) 5_445 .
O2 Pb2 Pb1 41.05(7) 10_557 .
O2 Pb2 Pb1 41.05(7) . .
O2 Pb2 O1 79.3(2) 10_557 5_445
O2 Pb2 O1 79.3(2) . 5_445
O2 Pb2 O2 81.69(11) . 10_557
O2 Pb2 N1 77.78(17) . .
O2 Pb2 N1 77.78(17) 10_557 .
N1 Pb2 Pb1 78.32(18) . .
Pb2 O1 Pb2 133.0(4) 5 7_656
C1 O1 Pb2 113.5(2) . 5
C1 O1 Pb2 113.5(2) . 7_656
Pb1 O2 Pb1 110.0(2) . 9_667
Pb2 O2 Pb1 101.30(2) 11_566 9_667
Pb2 O2 Pb1 109.52(3) . 9_667
Pb2 O2 Pb1 109.52(3) 11_566 .
Pb2 O2 Pb1 101.30(2) . .
Pb2 O2 Pb2 124.9(3) 11_566 .
N1 N1 Pb2 126.09(18) 3_756 .
N1 N1 N2 111.1(6) 3_756 .
N2 N1 Pb2 122.9(7) . .
N1 N2 C5 102.7(9) . .
O1 C1 C2 121.9(8) . .
C1 C2 H2 118.8 . .
C1 C2 C3 122.5(13) . .
C3 C2 H2 118.8 . .
C2 C3 H3 120.3 . .
C4 C3 C2 119.5(13) . .
C4 C3 H3 120.3 . .
C3 C4 C5 120.1(8) . .
N2 C5 N2 112.6(13) . 3_756
N2 C5 C4 123.7(7) . .
N2 C5 C4 123.7(7) 3_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Pb2 3.5580(5) 3_656
Pb1 Pb2 3.5580(5) .
Pb1 O2 2.383(3) 9_667
Pb1 O2 2.383(3) 10_557
Pb1 O2 2.383(3) .
Pb1 O2 2.383(3) 2_664
Pb2 O1 2.607(4) 5_445
Pb2 O2 2.216(3) 10_557
Pb2 O2 2.216(3) .
Pb2 N1 2.695(11) .
O1 Pb2 2.607(4) 5
O1 Pb2 2.607(4) 7_656
O1 C1 1.305(17) .
O2 Pb1 2.383(3) 9_667
O2 Pb2 2.216(3) 11_566
N1 N1 1.271(19) 3_756
N1 N2 1.337(13) .
N2 C5 1.341(12) .
C1 C2 1.384(16) .
C2 H2 0.9300 .
C2 C3 1.42(2) .
C3 H3 0.9300 .
C3 C4 1.376(16) .
C4 C5 1.47(2) .
C5 N2 1.342(12) 3_756
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Pb2 O1 C1 C2 139.1(7) 5 .
Pb2 O1 C1 C2 -40.9(7) 7_656 .
Pb2 N1 N2 C5 180.0 . .
O1 C1 C2 C3 179.6(11) . .
N1 N1 N2 C5 0.0 3_756 .
N1 N2 C5 N2 0.0 . 3_756
N1 N2 C5 C4 180.0 . .
C1 C2 C3 C4 1(2) . .
C2 C3 C4 C5 179.6(11) . .
C3 C4 C5 N2 40.6(7) . .
C3 C4 C5 N2 -139.4(7) . 3_756
