#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:43:51 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252771 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/38/7703876.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_7703876
loop_
_publ_author_name
'Hao, Wenjia'
'Jin, Bo'
'Zhang, Jinhao'
'Li, Xiaoyi'
'Huang, Tao'
'Shen, Juan'
'Peng, Rufang'
_publ_section_title
;
 Novel energetic metal-organic frameworks assembled from the energetic
 combination of furazan and tetrazole.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6295
_journal_page_last               6301
_journal_paper_doi               10.1039/d0dt00862a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(C6 H8 N12 O10 Pb2)'
_chemical_formula_sum            'C3 H4 N6 O5 Pb'
_chemical_formula_weight         411.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-30 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.481(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7154(7)
_cell_length_b                   4.4053(2)
_cell_length_c                   14.5814(9)
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      30.4790
_cell_measurement_theta_min      4.5910
_cell_volume                     807.85(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_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    -87.00   0.00   1.00    5.00    --  -16.11 -38.00 -60.00   87
  2  ω    -75.00  12.00   1.00    5.00    --  -16.11 -57.00-150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0476093000
_diffrn_orient_matrix_UB_12      -0.0100982000
_diffrn_orient_matrix_UB_13      -0.0198037000
_diffrn_orient_matrix_UB_21      0.0291212000
_diffrn_orient_matrix_UB_22      -0.0280087000
_diffrn_orient_matrix_UB_23      0.0445088000
_diffrn_orient_matrix_UB_31      -0.0081812000
_diffrn_orient_matrix_UB_32      -0.1582619000
_diffrn_orient_matrix_UB_33      -0.0066246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1416
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.973
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         737
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0174
_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)+(0.0269P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                732
_reflns_number_total             737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00862a2.cif
_cod_data_source_block           pb
_cod_depositor_comments
'Adding full bibliography for 7703875--7703876.cif.'
_cod_database_code               7703876
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C11 H10 N O'
_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_max   0.188
_shelx_estimated_absorpt_t_min   0.117
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Shared sites
{N1, C33}
{N3, O4}
2. Restrained distances
 O1W-H1WA
 0.86 with sigma of 0.02
 O1W-H1WB
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C33)
Uanis(N3) = Uanis(O4)
4. Others
 Fixed Sof: N1(0.5) N3(0.5) C33(0.5) O4(0.5)
;
_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 1.979
_oxdiff_exptl_absorpt_empirical_full_min 0.576
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.22306(5) 0.2500 0.01200(11) Uani 1 2 d S T P A .
O1 O 0.5482(3) 0.7247(6) 0.3412(3) 0.0172(8) Uani 1 1 d . . . . .
O1W O 0.2898(3) 0.2097(8) 0.2133(3) 0.0216(9) Uani 1 1 d D . . . .
H1WA H 0.256(5) 0.350(13) 0.239(5) 0.06(2) Uiso 1 1 d D . . . .
H1WB H 0.273(7) 0.219(11) 0.1539(16) 0.05(3) Uiso 1 1 d D . . . .
N1 N 0.5787(4) 0.7614(7) 0.4300(4) 0.0117(10) Uani 0.5 1 d . . . A 1
N2 N 0.6503(3) 0.9667(8) 0.4644(2) 0.0152(8) Uani 1 1 d . . . . .
N3 N 0.6565(2) 0.9469(8) 0.5583(2) 0.0174(7) Uani 0.5 1 d . . . A 3
N4 N 0.5887(4) 0.7306(7) 0.5825(4) 0.0171(10) Uani 1 1 d . . . . .
C1 C 0.5408(3) 0.6162(10) 0.5038(3) 0.0119(8) Uani 1 1 d . . . . .
C33 C 0.5787(4) 0.7614(7) 0.4300(4) 0.0117(10) Uani 0.5 1 d . . . A 2
O4 O 0.6565(2) 0.9469(8) 0.5583(2) 0.0174(7) Uani 0.5 1 d . . . A 4
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
_geom_angle_publ_flag
O1 Pb1 O1 64.29(16) 2_645 1_545 ?
O1 Pb1 O1 179.83(6) 1_545 2_655 ?
O1 Pb1 O1 115.88(15) 2_645 2_655 ?
O1 Pb1 O1 115.88(15) 1_545 . ?
O1 Pb1 O1 179.83(6) 2_645 . ?
O1 Pb1 O1 63.95(16) 2_655 . ?
O1 Pb1 O1W 76.20(12) . 2_655 ?
O1 Pb1 O1W 73.90(12) 1_545 2_655 ?
O1 Pb1 O1W 103.88(12) 1_545 . ?
O1 Pb1 O1W 103.88(12) 2_645 2_655 ?
O1 Pb1 O1W 76.20(12) 2_655 . ?
O1 Pb1 O1W 106.03(12) . . ?
O1 Pb1 O1W 73.90(12) 2_645 . ?
O1 Pb1 O1W 106.03(12) 2_655 2_655 ?
O1W Pb1 O1W 177.46(15) . 2_655 ?
Pb1 O1 Pb1 115.88(15) 1_565 . ?
N1 O1 Pb1 128.6(2) . . ?
N1 O1 Pb1 114.6(2) . 1_565 ?
Pb1 O1W H1WA 117(5) . . ?
Pb1 O1W H1WB 107(6) . . ?
H1WA O1W H1WB 109(6) . . ?
O1 N1 N2 123.1(4) . . ?
O1 N1 C1 128.4(4) . . ?
N2 N1 C1 108.4(4) . . ?
N2 N3 N4 111.1(3) . . ?
C1 N4 N3 105.6(4) . . ?
N1 C1 C1 126.0(5) . 5_666 ?
N4 C1 N1 109.2(4) . . ?
N4 C1 C1 124.8(5) . 5_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.593(3) 2_645 ?
Pb1 O1 2.593(3) 1_545 ?
Pb1 O1 2.605(3) . ?
Pb1 O1 2.605(3) 2_655 ?
Pb1 O1W 2.647(4) . ?
Pb1 O1W 2.647(4) 2_655 ?
O1 Pb1 2.593(3) 1_565 ?
O1 N1 1.305(7) . ?
O1W H1WA 0.87(2) . ?
O1W H1WB 0.86(2) . ?
N1 N2 1.329(6) . ?
N1 C1 1.398(6) . ?
N2 N3 1.362(5) . ?
N3 N4 1.367(5) . ?
N4 C1 1.317(6) . ?
C1 C1 1.450(8) 5_666 ?
