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_7043855
_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         '0.5(C36 H54 Cd10 N72)'
_chemical_formula_sum            'C18 H27 Cd5 N36'
_chemical_formula_weight         1309.75
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.149(2)
_cell_length_b                   13.149(2)
_cell_length_c                   13.596(3)
_cell_measurement_reflns_used    692
_cell_measurement_temperature    205
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.33
_cell_volume                     2035.8(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      205
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7105
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         1.788
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0633 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8448. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       needle
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.089
_refine_diff_density_min         -3.522
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         892
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1270P)^2^+23.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                715
_reflns_number_total             892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02582c2.cif
_cod_data_source_block           tt_sq_s
_cod_original_cell_volume        2035.8(8)
_cod_database_code               7043855
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C3, N5}
3. Restrained distances
 C2-C1
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3) = Uanis(N5)
5. Others
 Fixed Sof: C3(0.5) N5(0.5) H2A(0.25) H2C(0.25) H2B(0.25) C4(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5)
6.a Riding coordinates:
 C2(H2A,H2C,H2B)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'