#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:24:56 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186382 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/00/7040007.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_7040007
loop_
_publ_author_name
'Shang, Yu'
'Jin, Bo'
'Peng, Rufang'
'Liu, Qiangqiang'
'Tan, Bisheng'
'Guo, Zhicheng'
'Zhao, Jun'
'Zhang, Qingchun'
_publ_section_title
;
 A novel 3D energetic MOF of high energy content: synthesis and superior
 explosive performance of a Pb(ii) compound with
 5,5'-bistetrazole-1,1'-diolate.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13881
_journal_page_last               13887
_journal_paper_doi               10.1039/c6dt02558g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C2 H2 N8 O3 Pb'
_chemical_formula_weight         393.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-30 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.850(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3106(3)
_cell_length_b                   6.57573(17)
_cell_length_c                   8.4715(3)
_cell_measurement_reflns_used    5034
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      37.1630
_cell_measurement_theta_min      2.7780
_cell_volume                     683.32(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1637
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.032
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    24.690
_exptl_absorpt_correction_T_max  0.01242
_exptl_absorpt_correction_T_min  0.00091
_exptl_absorpt_correction_type   refdelf
_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.
DIFABS
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.823
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0424P)²+0.4702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1614
_reflns_number_total             1637
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02558g2.cif
_cod_data_source_block           difabs
_cod_depositor_comments          'Adding full bibliography for 7040007.cif.'
_cod_database_code               7040007
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.060
_shelx_estimated_absorpt_t_max   0.095
_shelx_res_file
; 
  
    difabs.res created by SHELXL-2014/7 
  
  
TITL m20151210e_a.res in I2/a 
CELL 0.71073 12.310567 6.575725 8.471472 90 94.8499 90 
ZERR 4 0.000284 0.000167 0.000263 0 0.0025 0 
LATT 2 
SYMM 0.5-X,+Y,-Z 
SFAC C H N O Pb 
UNIT 8 8 32 12 4 
  
L.S. 4 
PLAN  20 
SIZE 0.26 0.24 0.18 
TEMP -160 
BOND $H 
CONF 
fmap 2 
acta 52 
htab 
EQIV $1 x, -y+3/2, z-1/2 
HTAB O2 O1_$1 
HTAB O2 N1_$1 
EQIV $2 -x+1/2, -y+3/2, -z+3/2 
HTAB O2 O1_$2 
EQIV $3 -x+1, y+1/2, -z+3/2 
HTAB O2 N4_$3 
WGHT    0.042400    0.470200 
FVAR       1.00680 
PB1   5    0.250000    0.344941    0.500000    10.50000    0.02007    0.02510 = 
         0.02068    0.00000    0.00053    0.00000 
O1    4    0.323809    0.453186    0.801538    11.00000    0.01940    0.02995 = 
         0.02217   -0.00131    0.00193   -0.00203 
O2    4    0.250000    0.726391    0.500000    10.50000    0.02866    0.02390 = 
         0.02189    0.00000    0.00339    0.00000 
AFIX   7 
H2A   2    0.299773    0.772893    0.439590    10.50000   -1.50000 
H2B   2    0.264903    0.772893    0.597508    10.50000   -1.50000 
AFIX   0 
N1    3    0.429420    0.488372    0.798264    11.00000    0.02202    0.02520 = 
         0.01730   -0.00003    0.00190   -0.00098 
N2    3    0.473642    0.508587    0.659603    11.00000    0.02161    0.02851 = 
         0.01916   -0.00040    0.00203   -0.00181 
N3    3    0.578116    0.547835    0.696909    11.00000    0.02237    0.03018 = 
         0.01839    0.00019    0.00299   -0.00173 
N4    3    0.600896    0.553174    0.854654    11.00000    0.02210    0.02655 = 
         0.01980   -0.00012    0.00324   -0.00298 
C1    1    0.507921    0.510748    0.917547    11.00000    0.02053    0.02360 = 
         0.01742    0.00074    0.00078   -0.00201 
HKLF 4 
  
REM  m20151210e_a.res in I2/a 
REM R1 =  0.0211 for    1614 Fo > 4sig(Fo)  and  0.0214 for all    1637 data 
REM     66 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0425      0.4518 
  
REM Instructions for potential hydrogen bonds 
HTAB O2 O1_$1 
HTAB O2 N1_$1 
HTAB O2 O1_$2 
HTAB O2 N4_$3 
  
REM Highest difference peak  1.586,  deepest hole -1.878,  1-sigma level  0.221 
Q1    1   0.2585  0.2428  0.5193  11.00000  0.05    1.59 
Q2    1   0.1890  0.4667  0.4605  11.00000  0.05    0.96 
Q3    1   0.2509  0.4755  0.5342  11.00000  0.05    0.86 
Q4    1   0.3333  0.8249  0.6397  11.00000  0.05    0.79 
Q5    1   0.2333  0.3937  0.3782  11.00000  0.05    0.72 
Q6    1   0.2110  0.3508  0.3968  11.00000  0.05    0.68 
Q7    1   0.6562  0.5204  0.5840  11.00000  0.05    0.63 
Q8    1   0.6399  0.4770  0.7385  11.00000  0.05    0.62 
Q9    1   0.6261  0.5801  0.6727  11.00000  0.05    0.62 
Q10   1   0.6259  0.6481  0.8762  11.00000  0.05    0.60 
Q11   1   0.6077  0.4546  0.8622  11.00000  0.05    0.60 
Q12   1   0.4374  0.7744  0.6630  11.00000  0.05    0.60 
Q13   1   0.7179  0.5524  0.8703  11.00000  0.05    0.58 
Q14   1   0.3358  0.4844  0.6393  11.00000  0.05    0.56 
Q15   1   0.1799  0.4066  0.5285  11.00000  0.05    0.54 
Q16   1   0.5324  0.3580  0.6099  11.00000  0.05    0.53 
Q17   1   0.3620  0.3450  0.7581  11.00000  0.05    0.53 
Q18   1   0.5563  0.2735  0.9931  11.00000  0.05    0.51 
Q19   1   0.3309  0.8999  0.6037  11.00000  0.05    0.51 
Q20   1   0.6159  0.3504  0.8225  11.00000  0.05    0.51 
;
_shelx_res_checksum              86094
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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
Pb1 Pb 0.2500 0.34494(2) 0.5000 0.02202(5) Uani 1 2 d S T P
O1 O 0.32381(15) 0.4532(3) 0.8015(3) 0.0238(3) Uani 1 1 d . . .
O2 O 0.2500 0.7264(5) 0.5000 0.0247(5) Uani 1 2 d S T P
H2A H 0.2998 0.7729 0.4396 0.037 Uiso 0.5 1 d R U P
H2B H 0.2649 0.7729 0.5975 0.037 Uiso 0.5 1 d R U P
N1 N 0.42942(18) 0.4884(3) 0.7983(3) 0.0215(3) Uani 1 1 d . . .
N2 N 0.47364(19) 0.5086(4) 0.6596(3) 0.0231(4) Uani 1 1 d . . .
N3 N 0.57812(19) 0.5478(4) 0.6969(3) 0.0236(4) Uani 1 1 d . . .
N4 N 0.60090(18) 0.5532(3) 0.8547(3) 0.0227(3) Uani 1 1 d . . .
C1 C 0.5079(2) 0.5107(4) 0.9175(3) 0.0206(3) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02007(7) 0.02510(7) 0.02068(8) 0.000 0.00053(5) 0.000
O1 0.0194(7) 0.0299(9) 0.0222(8) -0.0013(6) 0.0019(6) -0.0020(6)
O2 0.0287(11) 0.0239(11) 0.0219(11) 0.000 0.0034(9) 0.000
N1 0.0220(8) 0.0252(8) 0.0173(8) 0.0000(6) 0.0019(6) -0.0010(6)
N2 0.0216(8) 0.0285(9) 0.0192(9) -0.0004(7) 0.0020(7) -0.0018(6)
N3 0.0224(8) 0.0302(10) 0.0184(8) 0.0002(7) 0.0030(7) -0.0017(7)
N4 0.0221(8) 0.0266(9) 0.0198(8) -0.0001(7) 0.0032(7) -0.0030(6)
C1 0.0205(8) 0.0236(9) 0.0174(8) 0.0007(7) 0.0008(7) -0.0020(6)
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
O2 Pb1 O1 74.90(4) . 2_556
O2 Pb1 O1 74.90(4) . .
O1 Pb1 O1 149.80(9) 2_556 .
N1 O1 Pb1 106.00(15) . .
Pb1 O2 H2A 110.2 . .
Pb1 O2 H2B 110.2 . .
H2A O2 H2B 108.7 . .
O1 N1 N2 120.5(2) . .
O1 N1 C1 130.4(2) . .
N2 N1 C1 109.1(2) . .
N3 N2 N1 105.6(2) . .
N2 N3 N4 111.1(2) . .
C1 N4 N3 106.2(2) . .
N4 C1 N1 108.0(2) . .
N4 C1 C1 127.1(3) . 5_667
N1 C1 C1 124.9(3) . 5_667
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.508(3) .
Pb1 O1 2.732(2) 2_556
Pb1 O1 2.732(2) .
O1 N1 1.323(3) .
O2 H2A 0.8854 .
O2 H2B 0.8854 .
N1 N2 1.342(3) .
N1 C1 1.346(3) .
N2 N3 1.324(3) .
N3 N4 1.342(3) .
N4 C1 1.332(3) .
C1 C1 1.434(5) 5_667
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O1 0.89 2.18 2.890(3) 136.6 8_564
O2 H2A N1 0.89 2.60 3.458(3) 162.9 8_564
O2 H2B O1 0.89 2.31 2.890(3) 123.2 7_566
O2 H2B N4 0.89 2.49 3.020(3) 119.4 4_556
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_4
Pb1 O1 N1 N2 13.7(3) .
Pb1 O1 N1 C1 -166.7(2) .
O1 N1 N2 N3 178.2(2) .
C1 N1 N2 N3 -1.4(3) .
N1 N2 N3 N4 -0.1(3) .
N2 N3 N4 C1 1.6(3) .
N3 N4 C1 N1 -2.4(3) .
N3 N4 C1 C1 176.9(3) 5_667
O1 N1 C1 N4 -177.2(2) .
N2 N1 C1 N4 2.5(3) .
O1 N1 C1 C1 3.5(5) 5_667
N2 N1 C1 C1 -176.8(3) 5_667
