#------------------------------------------------------------------------------
#$Date: 2021-03-10 11:51:11 +0200 (Wed, 10 Mar 2021) $
#$Revision: 262967 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/09/1560991.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_1560991
loop_
_publ_author_name
'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'
_publ_section_title
;
 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0151P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_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   0.537
_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)
;
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
Cd1 Cd 0.08378(2) 1.11157(2) 0.12851(2) 0.01437(7) Uani 1 1 d . . . . .
Cd2 Cd 0.0000 1.42183(2) 0.2500 0.01394(7) Uani 1 2 d S T P . .
N11 N 0.04251(10) 1.2212(2) -0.01774(11) 0.0184(4) Uani 1 1 d . . . . .
N12 N -0.01811(11) 1.1406(2) -0.10320(12) 0.0191(4) Uani 1 1 d . . . . .
N13 N 0.01082(11) 1.38185(19) -0.14292(12) 0.0197(4) Uani 1 1 d . . . . .
N14 N 0.11420(15) 1.4814(3) 0.01544(17) 0.0313(5) Uani 1 1 d . . . . .
H14A H 0.106(2) 1.574(4) -0.005(2) 0.069(11) Uiso 1 1 d . . . . .
H14B H 0.1329(17) 1.467(3) 0.073(2) 0.047(9) Uiso 1 1 d . . . . .
N21 N 0.16690(11) 1.3221(2) 0.22953(12) 0.0219(4) Uani 1 1 d . . . . .
N22 N 0.15067(11) 1.40510(19) 0.29346(12) 0.0187(4) Uani 1 1 d . . . . .
N23 N 0.28603(10) 1.4745(2) 0.32555(12) 0.0215(4) Uani 1 1 d . . . . .
N24 N 0.23353(17) 1.6002(3) 0.41967(17) 0.0343(5) Uani 1 1 d . . . . .
H24A H 0.2859(19) 1.607(3) 0.465(2) 0.046(9) Uiso 1 1 d . . . . .
H24B H 0.202(2) 1.575(4) 0.443(2) 0.071(11) Uiso 1 1 d . . . . .
N31 N -0.03862(11) 1.2111(2) 0.13229(12) 0.0206(4) Uani 1 1 d . U . . .
N32 N -0.08646(12) 1.1151(2) 0.14019(13) 0.0242(4) Uani 1 1 d . U . . .
N33 N -0.13159(14) 1.0255(3) 0.14942(17) 0.0468(6) Uani 1 1 d . . . . .
C11 C -0.03402(13) 1.2406(2) -0.17334(14) 0.0224(5) Uani 1 1 d . . . . .
H11 H -0.0731 1.2161 -0.2389 0.027 Uiso 1 1 calc R . . . .
C12 C 0.05654(13) 1.3646(2) -0.04563(15) 0.0174(4) Uani 1 1 d . . . . .
C21 C 0.24689(14) 1.3667(3) 0.25167(15) 0.0260(5) Uani 1 1 d . . . . .
H21 H 0.2740 1.3276 0.2194 0.031 Uiso 1 1 calc R . . . .
C22 C 0.22363(12) 1.4921(2) 0.34913(14) 0.0182(4) Uani 1 1 d . . . . .
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'
Cd Cd -0.8075 1.2024 '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'
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
N11 Cd1 N12 108.62(6) . 5_575
N11 Cd1 N21 100.04(6) . .
N11 Cd1 N23 104.34(6) . 4_545
N11 Cd1 N31 95.50(6) . .
N12 Cd1 N31 86.24(6) 5_575 .
N21 Cd1 N12 151.19(6) . 5_575
N21 Cd1 N23 89.18(6) . 4_545
N21 Cd1 N31 88.29(6) . .
N23 Cd1 N12 86.54(6) 4_545 5_575
N23 Cd1 N31 160.14(6) 4_545 .
N13 Cd2 N13 90.82(8) 6_586 5_585
N13 Cd2 N22 84.12(6) 5_585 .
N13 Cd2 N22 100.60(6) 5_585 2
N13 Cd2 N22 84.12(6) 6_586 2
N13 Cd2 N22 100.60(6) 6_586 .
N13 Cd2 N31 91.99(6) 6_586 2
N13 Cd2 N31 169.41(6) 6_586 .
N13 Cd2 N31 91.99(6) 5_585 .
N13 Cd2 N31 169.41(6) 5_585 2
N22 Cd2 N22 173.34(8) . 2
N22 Cd2 N31 85.33(6) . 2
N22 Cd2 N31 85.33(6) 2 .
N22 Cd2 N31 89.84(5) 2 2
N22 Cd2 N31 89.85(5) . .
N31 Cd2 N31 87.09(8) 2 .
N12 N11 Cd1 120.17(12) . .
C12 N11 Cd1 133.82(13) . .
C12 N11 N12 105.62(15) . .
N11 N12 Cd1 131.06(12) . 5_575
C11 N12 Cd1 123.74(13) . 5_575
C11 N12 N11 105.20(16) . .
C11 N13 Cd2 122.20(13) . 5_585
C12 N13 Cd2 135.64(13) . 5_585
C12 N13 C11 102.14(16) . .
H14A N14 H14B 119(3) . .
C12 N14 H14A 117(2) . .
C12 N14 H14B 114.9(19) . .
N22 N21 Cd1 126.39(12) . .
C21 N21 Cd1 126.54(14) . .
C21 N21 N22 105.96(15) . .
N21 N22 Cd2 116.66(11) . .
C22 N22 Cd2 134.94(13) . .
C22 N22 N21 105.18(15) . .
C21 N23 Cd1 124.39(13) . 4
C21 N23 C22 101.98(16) . .
C22 N23 Cd1 132.90(14) . 4
H24A N24 H24B 107(3) . .
C22 N24 H24A 112.2(19) . .
C22 N24 H24B 113(2) . .
Cd1 N31 Cd2 113.26(7) . .
N32 N31 Cd1 118.65(13) . .
N32 N31 Cd2 108.07(13) . .
N33 N32 N31 178.6(2) . .
N12 C11 N13 114.32(18) . .
N12 C11 H11 122.8 . .
N13 C11 H11 122.8 . .
N11 C12 N13 112.70(17) . .
N11 C12 N14 125.3(2) . .
N13 C12 N14 121.88(19) . .
N21 C21 N23 113.55(18) . .
N21 C21 H21 123.2 . .
N23 C21 H21 123.2 . .
N22 C22 N23 113.32(18) . .
N22 C22 N24 124.14(19) . .
N23 C22 N24 122.36(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N11 2.2591(16) .
Cd1 N12 2.3032(17) 5_575
Cd1 N21 2.2972(17) .
Cd1 N23 2.3016(16) 4_545
Cd1 N31 2.3404(17) .
Cd2 N13 2.2982(16) 6_586
Cd2 N13 2.2982(16) 5_585
Cd2 N22 2.3684(17) 2
Cd2 N22 2.3683(17) .
Cd2 N31 2.3893(16) 2
Cd2 N31 2.3894(16) .
N11 N12 1.389(2) .
N11 C12 1.330(2) .
N12 Cd1 2.3032(17) 5_575
N12 C11 1.304(2) .
N13 Cd2 2.2982(16) 5_585
N13 C11 1.343(2) .
N13 C12 1.342(2) .
N14 H14A 0.81(3) .
N14 H14B 0.82(3) .
N14 C12 1.368(3) .
N21 N22 1.388(2) .
N21 C21 1.312(3) .
N22 C22 1.324(2) .
N23 Cd1 2.3016(16) 4
N23 C21 1.347(3) .
N23 C22 1.350(2) .
N24 H24A 0.83(3) .
N24 H24B 0.85(3) .
N24 C22 1.381(3) .
N31 N32 1.211(2) .
N32 N33 1.151(3) .
C11 H11 0.9300 .
C21 H21 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Cd1 N11 N12 Cd1 -5.1(2) . . . 5_575
Cd1 N11 N12 C11 174.29(13) . . . .
Cd1 N11 C12 N13 -173.66(13) . . . .
Cd1 N11 C12 N14 9.6(3) . . . .
Cd1 N12 C11 N13 179.67(12) 5_575 . . .
Cd1 N21 N22 Cd2 -29.1(2) . . . .
Cd1 N21 N22 C22 168.13(13) . . . .
Cd1 N21 C21 N23 -168.83(14) . . . .
Cd1 N23 C21 N21 -170.44(14) 4 . . .
Cd1 N23 C22 N22 169.05(13) 4 . . .
Cd1 N23 C22 N24 -6.3(3) 4 . . .
Cd2 N13 C11 N12 177.87(13) 5_585 . . .
Cd2 N13 C12 N11 -177.25(14) 5_585 . . .
Cd2 N13 C12 N14 -0.4(3) 5_585 . . .
Cd2 N22 C22 N23 -157.03(14) . . . .
Cd2 N22 C22 N24 18.3(3) . . . .
N11 N12 C11 N13 0.2(2) . . . .
N12 N11 C12 N13 -1.2(2) . . . .
N12 N11 C12 N14 -177.9(2) . . . .
N21 N22 C22 N23 1.0(2) . . . .
N21 N22 C22 N24 176.3(2) . . . .
N22 N21 C21 N23 -0.3(2) . . . .
C11 N13 C12 N11 1.3(2) . . . .
C11 N13 C12 N14 178.1(2) . . . .
C12 N11 N12 Cd1 -178.83(14) . . . 5_575
C12 N11 N12 C11 0.6(2) . . . .
C12 N13 C11 N12 -0.9(2) . . . .
C21 N21 N22 Cd2 162.36(14) . . . .
C21 N21 N22 C22 -0.4(2) . . . .
C21 N23 C22 N22 -1.2(2) . . . .
C21 N23 C22 N24 -176.5(2) . . . .
C22 N23 C21 N21 0.9(2) . . . .
