In situ synthesized 3D metal-organic frameworks (MOFs) constructed from transition metal cations and tetrazole derivatives : a family of insensitive energetic materials
Xu, Yuangang; Liu, wei; li, dongxue; Chen, Houhe; Lu, Ming; Dalton Trans.  (2017) –; doi:10.1039/C7DT02582C

data_7043853
_publ_section_title
;
 In situ synthesized 3D metal-organic frameworks (MOFs) constructed from
 transition metal cations and tetrazole derivatives : a family of
 insensitive energetic materials
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02582C
_journal_year                    2017
_chemical_formula_moiety         '0.25(C24 H8 N56 Pb4), O'
_chemical_formula_sum            'C6 H2 N14 O Pb'
_chemical_formula_weight         493.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.05.22 svn.r3414 for OlexSys, GUI svn.r5347)
;
_audit_update_record
;
2017-06-05 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.743(4)
_cell_length_b                   6.963(2)
_cell_length_c                   13.777(4)
_cell_measurement_reflns_used    2546
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      3.26
_cell_volume                     1318.4(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7862
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.297
_diffrn_reflns_theta_min         1.478
_exptl_absorpt_coefficient_mu    12.827
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker;SADABS;2012
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.486
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1522
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0574
_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/[\s^2^(Fo^2^)+28.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1424
_reflns_number_total             1522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02582c2.cif
_cod_data_source_block           tt
_cod_database_code               7043853
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 3(10)
 0.12(6) -2(10) 0.30(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{C4, N7}
{C9, N8}
4. Restrained distances
 C1_$1-C1_$2 = C1-C1_$3
 1.455 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
N3 \\sim C9 \\sim C2 \\sim N1 \\sim N2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) = Uanis(N7)
Uanis(C9) = Uanis(N8)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C4(0.5) H4(0.5) N7(0.5) C9(0.5) H9(0.5) N8(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'