Stabilizing volatile azido in a 3D nitrogen-rich energetic metal‒organic framework with excellent energetic performance
Lin, Jian-Di; Li, Yang-Hua; Xu, Jian-Gang; Zheng, Fa-Kun; Guo, Guo-Cong; Lv, Ri-Xin; He, Wen-Cheng; Huang, Ze-Nan; Liu, Jin-Fu; Journal of Solid State Chemistry 265 (2018) 42–49; doi:10.1016/j.jssc.2018.05.026

data_1560991
_publ_section_title
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 Stabilizing volatile azido in a 3D nitrogen-rich energetic metal--organic
 framework with excellent energetic performance
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              42
_journal_page_last               49
_journal_paper_doi               10.1016/j.jssc.2018.05.026
_journal_volume                  265
_journal_year                    2018
_chemical_formula_moiety         '0.25(C32 H48 Cd12 N88)'
_chemical_formula_sum            'C8 H12 Cd3 N22'
_chemical_formula_weight         753.60
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 121.8956(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.647(3)
_cell_length_b                   8.2183(12)
_cell_length_c                   16.151(3)
_cell_measurement_reflns_used    3526
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_cell_volume                     1988.7(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1577
	          2theta: -15.1068
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1577
	          2theta: -15.1068
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.027331
_diffrn_orient_matrix_UB_12      -0.050586
_diffrn_orient_matrix_UB_13      -0.033895
_diffrn_orient_matrix_UB_21      -0.081840
_diffrn_orient_matrix_UB_22      0.015246
_diffrn_orient_matrix_UB_23      -0.088745
_diffrn_orient_matrix_UB_31      0.053944
_diffrn_orient_matrix_UB_32      0.010435
_diffrn_orient_matrix_UB_33      -0.047954
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6935
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.481
_diffrn_reflns_theta_min         3.512
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           80.0
_diffrn_source_power             4.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.232
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.517
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00165(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1808
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0142
_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/[\s^2^(Fo^2^)+(0.0151P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0311
_refine_ls_wR_factor_ref         0.0314
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1774
_reflns_number_total             1808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-265-42.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_database_code               1560991
_shelx_estimated_absorpt_t_max   0.537
_shelx_estimated_absorpt_t_min   0.444
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N31, N32
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
N31 \\sim N32: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
4.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21)
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_shelx_res_checksum              96841
_shelx_hkl_checksum              97117