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_7043856
_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_absolute_configuration syn
_chemical_formula_moiety         'C4 H2 N18 O2 Pb3, H2 O'
_chemical_formula_sum            'C4 H4 N18 O3 Pb3'
_chemical_formula_weight         973.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.523(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.106(3)
_cell_length_b                   10.342(3)
_cell_length_c                   15.143(5)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.428
_cell_measurement_theta_min      2.73
_cell_volume                     1560.9(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9022
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.728
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    32.340
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1430 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.3042. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.548
_refine_diff_density_min         -3.050
_refine_diff_density_rms         0.493
_refine_ls_abs_structure_details
;
 Flack x determined using 1434 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0670P)^2^+13.7430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                3306
_reflns_number_total             3458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02582c2.cif
_cod_data_source_block           mo_2017020_0m
_cod_original_cell_volume        1560.9(9)
_cod_database_code               7043856
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H3A-H3B
 1.46 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. 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
5.a Free rotating group:
 O3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 N14(H14), N1AA(H1AA)
;
_olex2_submission_special_instructions 'No special instructions were received'