# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mx
_database_code_depnum_ccdc_archive 'CCDC 2081734'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Oct 11 20:16:04 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,2(ditetrazol-2-yl)ethan dicopper(II) tetrazide
;
_chemical_name_common            
'1,2(ditetrazol-2-yl)ethan dicopper(II) tetrazide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C2 H3 Cu2 N16'
_chemical_formula_sum            'C2 H3 Cu2 N16'
_chemical_formula_weight         378.28

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'



_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.5720(6)
_cell_length_b                   9.4130(12)
_cell_length_c                   11.5810(12)
_cell_angle_alpha                102.066(10)
_cell_angle_beta                 91.440(9)
_cell_angle_gamma                105.227(11)
_cell_volume                     571.08(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    654
_cell_measurement_theta_min      4.5840
_cell_measurement_theta_max      28.8320

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    3.747
_shelx_estimated_absorpt_T_min   0.529
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_F_000             370
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            4119
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.1440
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.188
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2235
_reflns_number_gt                1412
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2235
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0552252000
_diffrn_orient_matrix_UB_12      0.0738726000
_diffrn_orient_matrix_UB_13      0.0345030000
_diffrn_orient_matrix_UB_21      0.0193715000
_diffrn_orient_matrix_UB_22      0.0275129000
_diffrn_orient_matrix_UB_23      -0.0525183000
_diffrn_orient_matrix_UB_31      -0.1187601000
_diffrn_orient_matrix_UB_32      0.0143609000
_diffrn_orient_matrix_UB_33      0.0015348000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -108.00  -53.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
  2 omega  -60.00  -13.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  132.0000  158.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega   36.00  100.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  120.0000 64

#__ type_ start__ end____ width___ exp.time_
  4 omega   74.00  112.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  150.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   75.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega  -42.00   96.00   1.0000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -60.0000 138

;



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'
Cu Cu 0.3201 1.2651 '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_
_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
Cu1 Cu 0.31035(13) 0.07515(10) 0.45886(7) 0.0127(2) Uani 1 1 d . . . . .
Cu2 Cu 0.90367(12) 0.20880(9) 0.38043(7) 0.0145(2) Uani 1 1 d . . . . .
N1 N 0.5465(8) -0.0397(6) 0.3909(5) 0.0116(12) Uani 1 1 d . . . . .
N2 N 0.5200(10) -0.1304(8) 0.2957(6) 0.0289(16) Uani 1 1 d . . . . .
N3 N 0.5026(14) -0.2174(11) 0.2083(7) 0.081(3) Uani 1 1 d . . . . .
N4 N 0.0559(8) 0.1732(6) 0.5284(5) 0.0114(12) Uani 1 1 d . . . . .
N5 N 0.0766(9) 0.2696(7) 0.6199(6) 0.0183(13) Uani 1 1 d . . . . .
N6 N 0.0879(12) 0.3570(8) 0.7075(6) 0.043(2) Uani 1 1 d . . . . .
N7 N 0.1232(8) 0.0828(6) 0.3115(5) 0.0137(12) Uani 1 1 d . . . . .
N8 N 0.1259(9) 0.0152(7) 0.2108(6) 0.0210(14) Uani 1 1 d . . . . .
N9 N 0.1336(13) -0.0444(8) 0.1140(6) 0.048(2) Uani 1 1 d . . . . .
N10 N 0.6541(8) 0.2928(7) 0.4670(5) 0.0145(13) Uani 1 1 d . . . . .
N11 N 0.7120(8) 0.4213(7) 0.5251(5) 0.0150(13) Uani 1 1 d . . . . .
N12 N 0.7588(9) 0.5431(7) 0.5786(5) 0.0221(14) Uani 1 1 d . . . . .
N13 N 0.8031(8) 0.2623(6) 0.2328(5) 0.0150(12) Uani 1 1 d . . . . .
N15 N 0.9733(9) 0.3005(6) 0.1575(5) 0.0184(13) Uani 1 1 d . . . . .
N16 N 0.6286(9) 0.3559(7) 0.1039(5) 0.0239(14) Uani 1 1 d . . . . .
N17 N 0.8631(9) 0.3547(6) 0.0832(5) 0.0184(12) Uani 1 1 d . . . . .
C1 C 0.6006(11) 0.2993(8) 0.1978(6) 0.0202(16) Uani 1 1 d . . . . .
H1 H 0.4519 0.2856 0.2374 0.024 Uiso 1 1 calc R U . . .
C2 C 0.9924(12) 0.4156(7) -0.0105(6) 0.0230(17) Uani 1 1 d . . . . .
H2A H 0.9012 0.3615 -0.0884 0.028 Uiso 1 1 calc R U . . .
H2B H 1.1625 0.4018 -0.0106 0.028 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.986(5) . ?
Cu1 N1 1.991(5) . ?
Cu1 N7 2.001(5) . ?
Cu1 N1 2.022(5) 2_656 ?
Cu1 N10 2.392(5) . ?
Cu2 N10 1.970(5) . ?
Cu2 N13 1.987(5) . ?
Cu2 N7 1.989(5) 1_655 ?
Cu2 N4 2.021(5) 1_655 ?
N1 N2 1.224(8) . ?
N1 Cu1 2.022(5) 2_656 ?
N2 N3 1.145(8) . ?
N4 N5 1.223(7) . ?
N4 Cu2 2.021(5) 1_455 ?
N5 N6 1.153(8) . ?
N7 N8 1.209(7) . ?
N7 Cu2 1.989(5) 1_455 ?
N8 N9 1.151(8) . ?
N10 N11 1.210(7) . ?
N11 N12 1.142(7) . ?
N13 N15 1.335(7) . ?
N13 C1 1.343(8) . ?
N15 N17 1.304(7) . ?
N16 C1 1.302(8) . ?
N16 N17 1.337(6) . ?
N17 C2 1.451(8) . ?
C1 H1 0.9500 . ?
C2 C2 1.536(13) 2_765 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?

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
_geom_angle_publ_flag
N4 Cu1 N1 175.1(2) . . ?
N4 Cu1 N7 79.5(2) . . ?
N1 Cu1 N7 101.1(2) . . ?
N4 Cu1 N1 98.4(2) . 2_656 ?
N1 Cu1 N1 80.3(2) . 2_656 ?
N7 Cu1 N1 171.0(2) . 2_656 ?
N4 Cu1 N10 100.30(19) . . ?
N1 Cu1 N10 84.46(19) . . ?
N7 Cu1 N10 98.1(2) . . ?
N1 Cu1 N10 90.91(19) 2_656 . ?
N10 Cu2 N13 91.5(2) . . ?
N10 Cu2 N7 166.2(2) . 1_655 ?
N13 Cu2 N7 98.0(2) . 1_655 ?
N10 Cu2 N4 92.9(2) . 1_655 ?
N13 Cu2 N4 171.70(19) . 1_655 ?
N7 Cu2 N4 78.9(2) 1_655 1_655 ?
N2 N1 Cu1 127.8(4) . . ?
N2 N1 Cu1 122.3(5) . 2_656 ?
Cu1 N1 Cu1 99.7(2) . 2_656 ?
N3 N2 N1 177.2(7) . . ?
N5 N4 Cu1 128.6(4) . . ?
N5 N4 Cu2 117.4(4) . 1_455 ?
Cu1 N4 Cu2 99.9(2) . 1_455 ?
N6 N5 N4 177.3(7) . . ?
N8 N7 Cu2 130.3(4) . 1_455 ?
N8 N7 Cu1 128.8(4) . . ?
Cu2 N7 Cu1 100.5(2) 1_455 . ?
N9 N8 N7 177.5(7) . . ?
N11 N10 Cu2 120.4(4) . . ?
N11 N10 Cu1 134.6(4) . . ?
Cu2 N10 Cu1 103.4(2) . . ?
N12 N11 N10 177.6(6) . . ?
N15 N13 C1 105.9(5) . . ?
N15 N13 Cu2 119.8(4) . . ?
C1 N13 Cu2 132.9(4) . . ?
N17 N15 N13 104.9(5) . . ?
C1 N16 N17 101.2(5) . . ?
N15 N17 N16 114.8(5) . . ?
N15 N17 C2 121.8(5) . . ?
N16 N17 C2 123.3(5) . . ?
N16 C1 N13 113.2(6) . . ?
N16 C1 H1 123.4 . . ?
N13 C1 H1 123.4 . . ?
N17 C2 C2 109.0(7) . 2_765 ?
N17 C2 H2A 109.9 . . ?
C2 C2 H2A 109.9 2_765 . ?
N17 C2 H2B 109.9 . . ?
C2 C2 H2B 109.9 2_765 . ?
H2A C2 H2B 108.3 . . ?

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
_geom_torsion_publ_flag
C1 N13 N15 N17 -0.8(6) . . . . ?
Cu2 N13 N15 N17 -168.8(4) . . . . ?
N13 N15 N17 N16 0.2(7) . . . . ?
N13 N15 N17 C2 177.2(6) . . . . ?
C1 N16 N17 N15 0.5(7) . . . . ?
C1 N16 N17 C2 -176.4(6) . . . . ?
N17 N16 C1 N13 -1.1(8) . . . . ?
N15 N13 C1 N16 1.2(8) . . . . ?
Cu2 N13 C1 N16 167.0(5) . . . . ?
N15 N17 C2 C2 -116.5(8) . . . 2_765 ?
N16 N17 C2 C2 60.3(9) . . . 2_765 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N7 0.95 2.58 3.379(8) 141.7 .
C1 H1 N8 0.95 2.66 3.263(8) 121.6 .
C2 H2A N3 0.99 2.51 3.395(10) 149.2 2_655
C2 H2A N6 0.99 2.60 3.278(9) 125.4 1_654
C1 H1 N7 0.95 2.58 3.379(8) 141.7 .
C1 H1 N8 0.95 2.66 3.263(8) 121.6 .
C2 H2A N3 0.99 2.51 3.395(10) 149.2 2_655
C2 H2A N6 0.99 2.60 3.278(9) 125.4 1_654

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         1.489
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.149

_shelxl_version_number           2013-4


_olex2_submission_special_instructions 'No special instructions were received'


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nx234
_database_code_depnum_ccdc_archive 'CCDC 2081735'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;

_vrf_PLAT213_nx234               
; 
PROBLEM: Atom N19    has ADP max/min Ratio .....      4.3 prolat 
RESPONSE: Vibration of outer azide nitrogen atom
;

_vrf_PLAT220_nx234               
; 
PROBLEM: Non-Solvent  Resd 1  N   Ueq(max)/Ueq(min) Range     9.5 Ratio  
RESPONSE: cprobably caused by crytsal quality.
0.8 Angstrom from H1, no missing atom possible, 
;
_audit_creation_date             2018-06-22
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
di(1(2-azidoethyl)-5H-tetrazolyl octaazido tetracopper(II)
;
_chemical_name_common            
' di(1(2-azidoethyl)-5H-tetrazolyl octaazido tetracopper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H5 Cu2 N19'
_chemical_formula_sum            'C3 H5 Cu2 N19'
_chemical_formula_weight         434.34

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'



_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   5.6349(3)
_cell_length_b                   26.5998(16)
_cell_length_c                   9.6251(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.208(7)
_cell_angle_gamma                90
_cell_volume                     1392.16(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    1830
_cell_measurement_theta_min      4.3570
_cell_measurement_theta_max      27.8560

_exptl_crystal_description       rod
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    3.094
_shelx_estimated_absorpt_T_min   0.325
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_F_000             856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            11589
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.389
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2821
_reflns_number_gt                2128
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2821
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0633
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0792354000
_diffrn_orient_matrix_UB_12      -0.0064567000
_diffrn_orient_matrix_UB_13      -0.0436169000
_diffrn_orient_matrix_UB_21      0.0041047000
_diffrn_orient_matrix_UB_22      -0.0251777000
_diffrn_orient_matrix_UB_23      0.0247470000
_diffrn_orient_matrix_UB_31      -0.1035019000
_diffrn_orient_matrix_UB_32      -0.0059188000
_diffrn_orient_matrix_UB_33      -0.0576406000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -99.00 -35.80   0.80   35.00    --  -28.70-179.00-180.00   79
  2  ω    -79.00 -35.00   0.80   35.00    --  -28.70-179.00 120.00   55
  3  ω     54.00  98.00   0.80   35.00    --   29.79  57.00 120.00   55
  4  ω     38.00 101.20   0.80   35.00    --   29.79  38.00  90.00   79
  5  ω    -17.00  73.40   0.80   35.00    --   29.79 -99.00-180.00  113
  6  ω     64.00 111.20   0.80   35.00    --   29.79-179.00-180.00   59
  7  ω     37.00  70.60   0.80   35.00    --   29.79 -99.00 -30.00   42
  8  ω     38.00  62.80   0.80   35.00    --   29.79 179.00-150.00   31
  9  ω     11.00  97.40   0.80   35.00    --   29.79  38.00  30.00  108
;



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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu1 Cu 0.42459(7) 0.04623(2) 0.23872(5) 0.01450(12) Uani 1 1 d . . . . .
Cu2 Cu 0.81847(7) 0.01586(2) 0.08587(5) 0.01254(12) Uani 1 1 d . . . . .
N1 N 0.2376(5) 0.16364(11) 0.4635(3) 0.0186(7) Uani 1 1 d . . . . .
N2 N 0.4687(5) 0.17595(12) 0.4582(4) 0.0307(8) Uani 1 1 d . . . . .
N3 N 0.5345(5) 0.14293(12) 0.3793(4) 0.0277(8) Uani 1 1 d . . . . .
N4 N 0.3530(5) 0.10861(10) 0.3332(3) 0.0171(7) Uani 1 1 d . . . . .
N5 N 0.0047(7) 0.25684(15) 0.3573(4) 0.0441(10) Uani 1 1 d . . . . .
N6 N -0.2149(8) 0.26628(15) 0.3261(4) 0.0436(10) Uani 1 1 d . . . . .
N7 N -0.4151(8) 0.2764(2) 0.2836(5) 0.0800(17) Uani 1 1 d . . . . .
N8 N 0.6622(5) 0.07721(11) 0.1416(3) 0.0155(6) Uani 1 1 d . . . . .
N9 N 0.6859(5) 0.12119(12) 0.1141(3) 0.0204(7) Uani 1 1 d . . . . .
N10 N 0.7132(7) 0.16279(14) 0.0930(5) 0.0507(11) Uani 1 1 d . . . . .
N11 N 0.5550(4) -0.01510(10) 0.1617(3) 0.0136(6) Uani 1 1 d . . . . .
N12 N 0.5751(5) -0.05383(12) 0.2326(3) 0.0224(7) Uani 1 1 d . . . . .
N13 N 0.5861(8) -0.09032(14) 0.2945(5) 0.0533(12) Uani 1 1 d . . . . .
N14 N 0.1643(5) 0.00835(10) 0.2969(3) 0.0150(6) Uani 1 1 d . . . . .
N15 N 0.2086(4) -0.01253(11) 0.4123(3) 0.0142(6) Uani 1 1 d . . . . .
C1 C 0.1713(6) 0.12227(13) 0.3885(4) 0.0172(8) Uani 1 1 d . . . . .
H1 H 0.0192 0.1052 0.3761 0.021 Uiso 1 1 calc R U . . .
C2 C 0.1074(6) 0.19374(14) 0.5480(4) 0.0231(9) Uani 1 1 d . . . . .
H2A H 0.1850 0.1888 0.6519 0.028 Uiso 1 1 calc R U . . .
H2B H -0.0658 0.1825 0.5276 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1155(7) 0.24874(14) 0.5105(4) 0.0294(10) Uani 1 1 d . . . . .
H3A H 0.0258 0.2686 0.5673 0.035 Uiso 1 1 calc R U . . .
H3B H 0.2885 0.2604 0.5357 0.035 Uiso 1 1 calc R U . . .
N17 N 1.0696(4) 0.04682(10) -0.0007(3) 0.0108(6) Uani 1 1 d . . . . .
N16 N 0.2428(5) -0.03271(13) 0.5214(4) 0.0261(8) Uani 1 1 d . . . . .
N18 N 1.0387(6) 0.08610(14) -0.0698(4) 0.0365(9) Uani 1 1 d . . . . .
N19 N 1.0142(10) 0.12226(18) -0.1345(6) 0.104(2) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N14 1.978(3) . ?
Cu1 N4 1.984(3) . ?
Cu1 N8 2.001(3) . ?
Cu1 N11 2.009(3) . ?
Cu2 N8 1.993(3) . ?
Cu2 N11 1.996(3) . ?
Cu2 N17 1.999(3) . ?
Cu2 N17 2.030(3) 3_755 ?
Cu2 N14 2.426(3) 1_655 ?
N1 C1 1.316(4) . ?
N1 N2 1.357(4) . ?
N1 C2 1.467(4) . ?
N2 N3 1.278(4) . ?
N3 N4 1.356(4) . ?
N4 C1 1.323(4) . ?
N5 N6 1.220(5) . ?
N5 C3 1.458(5) . ?
N6 N7 1.127(5) . ?
N8 N9 1.214(4) . ?
N9 N10 1.143(4) . ?
N11 N12 1.224(4) . ?
N12 N13 1.132(4) . ?
N14 N15 1.207(4) . ?
N14 Cu2 2.426(3) 1_455 ?
N15 N16 1.150(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.510(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N17 N18 1.226(4) . ?
N17 Cu2 2.030(3) 3_755 ?
N18 N19 1.134(5) . ?

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
_geom_angle_publ_flag
N14 Cu1 N4 92.36(11) . . ?
N14 Cu1 N8 168.29(12) . . ?
N4 Cu1 N8 96.38(12) . . ?
N14 Cu1 N11 93.50(11) . . ?
N4 Cu1 N11 170.51(11) . . ?
N8 Cu1 N11 78.91(11) . . ?
N8 Cu2 N11 79.40(11) . . ?
N8 Cu2 N17 100.72(11) . . ?
N11 Cu2 N17 176.89(11) . . ?
N8 Cu2 N17 170.74(11) . 3_755 ?
N11 Cu2 N17 98.53(11) . 3_755 ?
N17 Cu2 N17 80.86(11) . 3_755 ?
N8 Cu2 N14 99.01(10) . 1_655 ?
N11 Cu2 N14 99.83(10) . 1_655 ?
N17 Cu2 N14 83.24(10) . 1_655 ?
N17 Cu2 N14 90.23(10) 3_755 1_655 ?
C1 N1 N2 108.6(3) . . ?
C1 N1 C2 130.5(3) . . ?
N2 N1 C2 120.9(3) . . ?
N3 N2 N1 106.7(3) . . ?
N2 N3 N4 110.2(3) . . ?
C1 N4 N3 106.3(3) . . ?
C1 N4 Cu1 133.3(2) . . ?
N3 N4 Cu1 119.1(2) . . ?
N6 N5 C3 114.6(4) . . ?
N7 N6 N5 172.8(5) . . ?
N9 N8 Cu2 130.4(2) . . ?
N9 N8 Cu1 128.6(2) . . ?
Cu2 N8 Cu1 100.69(13) . . ?
N10 N9 N8 177.6(4) . . ?
N12 N11 Cu2 125.6(2) . . ?
N12 N11 Cu1 117.8(2) . . ?
Cu2 N11 Cu1 100.31(12) . . ?
N13 N12 N11 177.4(4) . . ?
N15 N14 Cu1 120.3(2) . . ?
N15 N14 Cu2 137.3(2) . 1_455 ?
Cu1 N14 Cu2 102.30(12) . 1_455 ?
N16 N15 N14 177.8(3) . . ?
N1 C1 N4 108.2(3) . . ?
N1 C1 H1 125.9 . . ?
N4 C1 H1 125.9 . . ?
N1 C2 C3 110.2(3) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N5 C3 C2 110.6(3) . . ?
N5 C3 H3A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
N5 C3 H3B 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N18 N17 Cu2 124.2(2) . . ?
N18 N17 Cu2 119.7(3) . 3_755 ?
Cu2 N17 Cu2 99.14(11) . 3_755 ?
N19 N18 N17 178.6(4) . . ?

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
_geom_torsion_publ_flag
C1 N1 N2 N3 1.2(4) . . . . ?
C2 N1 N2 N3 179.0(3) . . . . ?
N1 N2 N3 N4 -0.6(4) . . . . ?
N2 N3 N4 C1 -0.2(4) . . . . ?
N2 N3 N4 Cu1 -169.0(3) . . . . ?
N2 N1 C1 N4 -1.3(4) . . . . ?
C2 N1 C1 N4 -178.9(3) . . . . ?
N3 N4 C1 N1 0.9(4) . . . . ?
Cu1 N4 C1 N1 167.4(3) . . . . ?
C1 N1 C2 C3 -131.9(4) . . . . ?
N2 N1 C2 C3 50.7(4) . . . . ?
N6 N5 C3 C2 91.3(4) . . . . ?
N1 C2 C3 N5 58.6(4) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2A N7 0.99 2.46 3.132(6) 125.0 4_666
C2 H2B N2 0.99 2.54 3.506(4) 166.0 1_455
C2 H2B N3 0.99 2.56 3.483(5) 156.0 1_455
C3 H3A N10 0.99 2.59 3.501(5) 152.5 4_466
C2 H2A N7 0.99 2.46 3.132(6) 125.0 4_666
C2 H2B N2 0.99 2.54 3.506(4) 166.0 1_455
C2 H2B N3 0.99 2.56 3.483(5) 156.0 1_455
C3 H3A N10 0.99 2.59 3.501(5) 152.5 4_466

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.600
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.100

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_uv645
_database_code_depnum_ccdc_archive 'CCDC 2081739'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
copper(II) azide 2-methy-5-aminotetrazole
;
_chemical_name_common            'copper(II) azide 2-methy-5-aminotetrazole'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H5 Cu2 N17'
_chemical_formula_sum            'C2 H5 Cu2 N17'
_chemical_formula_weight         394.31

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.7855(6)
_cell_length_b                   5.6009(2)
_cell_length_c                   14.8579(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.424(2)
_cell_angle_gamma                90
_cell_volume                     1196.80(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5971
_cell_measurement_theta_min      2.8327
_cell_measurement_theta_max      28.2278

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.583
_shelx_estimated_absorpt_T_min   0.716
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            11334
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.218
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2350
_reflns_number_gt                2018
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2350
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      1.222
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu2 Cu 0.02581(3) 0.28111(7) 0.06260(3) 0.00993(14) Uani 1 1 d . . . . .
Cu1 Cu 0.06377(3) -0.17856(7) 0.17801(3) 0.01115(15) Uani 1 1 d . . . . .
N5 N 0.0693(3) 0.0587(6) 0.3944(3) 0.0254(8) Uani 1 1 d . . . . .
N7 N 0.2932(2) -0.5146(5) 0.2230(2) 0.0156(6) Uani 1 1 d . . . . .
N1 N 0.0175(2) -0.2666(5) 0.2897(2) 0.0147(6) Uani 1 1 d . . . . .
C1 C 0.0205(3) -0.1415(6) 0.3692(2) 0.0174(8) Uani 1 1 d . . . . .
N6 N 0.2131(2) -0.4959(5) 0.19638(18) 0.0123(6) Uani 1 1 d . . . . .
N3 N -0.0707(2) -0.4260(6) 0.3639(2) 0.0222(7) Uani 1 1 d . . . . .
N9 N -0.0200(2) 0.1006(5) 0.15627(19) 0.0133(6) Uani 1 1 d . . . . .
N13 N 0.1848(2) -0.0293(5) 0.0683(2) 0.0170(6) Uani 1 1 d . . . . .
N8 N 0.13061(19) -0.4810(5) 0.1684(2) 0.0139(6) Uani 1 1 d . . . . .
N16 N -0.1397(2) 0.5565(5) 0.0561(2) 0.0179(7) Uani 1 1 d . . . . .
N4 N -0.0350(2) -0.2419(6) 0.4186(2) 0.0222(7) Uani 1 1 d . . . . .
N15 N -0.05882(19) 0.5681(5) 0.04842(18) 0.0116(6) Uani 1 1 d . . . . .
N2 N -0.0424(2) -0.4462(5) 0.2884(2) 0.0198(7) Uani 1 1 d . . . . .
N12 N 0.10203(19) -0.0213(5) 0.06930(19) 0.0126(6) Uani 1 1 d . . . . .
N10 N -0.0941(2) 0.1023(6) 0.1782(2) 0.0241(7) Uani 1 1 d . . . . .
N11 N -0.1628(3) 0.0969(7) 0.2013(3) 0.0385(9) Uani 1 1 d . . . . .
N17 N -0.2144(2) 0.5524(7) 0.0634(3) 0.0401(10) Uani 1 1 d . . . . .
N14 N 0.2618(2) -0.0421(7) 0.0683(2) 0.0313(8) Uani 1 1 d . . . . .
C2 C -0.1347(3) -0.5956(8) 0.3919(3) 0.0322(10) Uani 1 1 d . . . . .
H2A H -0.1709 -0.6779 0.3370 0.048 Uiso 1 1 calc R U . . .
H2B H -0.1768 -0.5092 0.4224 0.048 Uiso 1 1 calc R U . . .
H2C H -0.0990 -0.7129 0.4348 0.048 Uiso 1 1 calc R U . . .
H5B H 0.067(3) 0.111(8) 0.444(3) 0.031(13) Uiso 1 1 d . . . . .
H5A H 0.105(3) 0.069(8) 0.373(3) 0.024(14) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu2 N9 1.964(3) . ?
Cu2 N15 2.012(3) 3_565 ?
Cu2 N15 2.018(3) . ?
Cu2 N12 2.024(3) . ?
Cu2 N8 2.349(3) 1_565 ?
Cu1 N9 1.974(3) . ?
Cu1 N8 1.983(3) . ?
Cu1 N1 1.998(3) . ?
Cu1 N12 2.032(3) . ?
Cu1 N7 2.457(3) 2 ?
N5 C1 1.340(5) . ?
N5 H5B 0.79(5) . ?
N5 H5A 0.68(4) . ?
N7 N6 1.162(4) . ?
N7 Cu1 2.457(3) 2_545 ?
N1 N2 1.337(4) . ?
N1 C1 1.365(4) . ?
C1 N4 1.344(5) . ?
N6 N8 1.197(4) . ?
N3 N2 1.289(4) . ?
N3 N4 1.343(4) . ?
N3 C2 1.467(5) . ?
N9 N10 1.212(4) . ?
N13 N14 1.141(4) . ?
N13 N12 1.228(4) . ?
N8 Cu2 2.349(3) 1_545 ?
N16 N17 1.135(4) . ?
N16 N15 1.229(4) . ?
N15 Cu2 2.012(3) 3_565 ?
N10 N11 1.147(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
_geom_angle_publ_flag
N9 Cu2 N15 170.64(11) . 3_565 ?
N9 Cu2 N15 100.17(11) . . ?
N15 Cu2 N15 80.94(12) 3_565 . ?
N9 Cu2 N12 79.28(11) . . ?
N15 Cu2 N12 98.82(11) 3_565 . ?
N15 Cu2 N12 175.18(11) . . ?
N9 Cu2 N8 95.76(11) . 1_565 ?
N15 Cu2 N8 93.60(10) 3_565 1_565 ?
N15 Cu2 N8 85.10(10) . 1_565 ?
N12 Cu2 N8 99.71(10) . 1_565 ?
N9 Cu1 N8 165.71(12) . . ?
N9 Cu1 N1 90.48(12) . . ?
N8 Cu1 N1 96.98(12) . . ?
N9 Cu1 N12 78.85(11) . . ?
N8 Cu1 N12 94.45(12) . . ?
N1 Cu1 N12 168.34(12) . . ?
N9 Cu1 N7 102.84(11) . 2 ?
N8 Cu1 N7 89.32(10) . 2 ?
N1 Cu1 N7 90.48(11) . 2 ?
N12 Cu1 N7 87.37(10) . 2 ?
C1 N5 H5B 115(3) . . ?
C1 N5 H5A 112(4) . . ?
H5B N5 H5A 127(5) . . ?
N6 N7 Cu1 154.7(2) . 2_545 ?
N2 N1 C1 106.7(3) . . ?
N2 N1 Cu1 121.8(2) . . ?
C1 N1 Cu1 130.0(2) . . ?
N5 C1 N4 123.7(4) . . ?
N5 C1 N1 125.4(4) . . ?
N4 C1 N1 110.9(3) . . ?
N7 N6 N8 178.8(3) . . ?
N2 N3 N4 115.7(3) . . ?
N2 N3 C2 123.4(3) . . ?
N4 N3 C2 120.9(3) . . ?
N10 N9 Cu2 131.9(2) . . ?
N10 N9 Cu1 122.3(2) . . ?
Cu2 N9 Cu1 102.54(13) . . ?
N14 N13 N12 178.4(4) . . ?
N6 N8 Cu1 121.3(2) . . ?
N6 N8 Cu2 130.8(2) . 1_545 ?
Cu1 N8 Cu2 105.69(12) . 1_545 ?
N17 N16 N15 178.1(4) . . ?
N3 N4 C1 101.2(3) . . ?
N16 N15 Cu2 121.6(2) . 3_565 ?
N16 N15 Cu2 122.8(2) . . ?
Cu2 N15 Cu2 99.06(12) 3_565 . ?
N3 N2 N1 105.6(3) . . ?
N13 N12 Cu2 125.1(2) . . ?
N13 N12 Cu1 117.1(2) . . ?
Cu2 N12 Cu1 98.47(12) . . ?
N11 N10 N9 177.3(4) . . ?
N3 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

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
_geom_torsion_publ_flag
N2 N1 C1 N5 -176.9(4) . . . . ?
Cu1 N1 C1 N5 -10.9(6) . . . . ?
N2 N1 C1 N4 1.2(4) . . . . ?
Cu1 N1 C1 N4 167.2(3) . . . . ?
N2 N3 N4 C1 0.3(4) . . . . ?
C2 N3 N4 C1 178.0(3) . . . . ?
N5 C1 N4 N3 177.2(4) . . . . ?
N1 C1 N4 N3 -0.9(4) . . . . ?
N4 N3 N2 N1 0.4(4) . . . . ?
C2 N3 N2 N1 -177.2(3) . . . . ?
C1 N1 N2 N3 -0.9(4) . . . . ?
Cu1 N1 N2 N3 -168.3(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5B N4 0.79(5) 2.32(5) 3.112(5) 171(4) 3_556
N5 H5A N7 0.68(4) 2.34(5) 2.999(5) 161(5) 2

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.478
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.136

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mx469
_database_code_depnum_ccdc_archive 'CCDC 2084455'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Nov 10 18:59:52 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis-1-aminotriazolyl tetracopper(II) octaazide 
;
_chemical_name_common            
'bis-1-aminotriazolyl tetracopper(II) octaazide '
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 Cu2 N16'
_chemical_formula_sum            'C2 H4 Cu2 N16'
_chemical_formula_weight         379.29

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'



_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.7400(7)
_cell_length_b                   9.6530(13)
_cell_length_c                   11.1290(14)
_cell_angle_alpha                73.371(12)
_cell_angle_beta                 79.264(11)
_cell_angle_gamma                74.775(12)
_cell_volume                     565.98(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    1303
_cell_measurement_theta_min      4.6960
_cell_measurement_theta_max      31.9070

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.781
_shelx_estimated_absorpt_T_min   0.452
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_F_000             372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            4087
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.377
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2206
_reflns_number_gt                1712
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0250P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2206
_refine_ls_number_parameters     189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0608096000
_diffrn_orient_matrix_UB_12      0.0754906000
_diffrn_orient_matrix_UB_13      -0.0069223000
_diffrn_orient_matrix_UB_21      0.0757086000
_diffrn_orient_matrix_UB_22      0.0075717000
_diffrn_orient_matrix_UB_23      0.0402770000
_diffrn_orient_matrix_UB_31      0.0849207000
_diffrn_orient_matrix_UB_32      0.0207419000
_diffrn_orient_matrix_UB_33      -0.0530982000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -95.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000 -180.0000 131

#__ type_ start__ end____ width___ exp.time_
  2 omega -111.00  -81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega -100.00    2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000    0.0000 102

#__ type_ start__ end____ width___ exp.time_
  4 omega  -94.00  -60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -180.0000 34

#__ type_ start__ end____ width___ exp.time_
  5 omega   59.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
  6 omega  -21.00   73.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -150.0000 94

;



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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu1 Cu 0.83497(8) 0.42026(5) 0.46223(4) 0.01623(14) Uani 1 1 d . . . . .
Cu2 Cu 0.45575(8) 0.29402(5) 0.38595(4) 0.01715(15) Uani 1 1 d . . . . .
N1 N 0.7127(6) 0.4114(4) 0.3078(3) 0.0206(7) Uani 1 1 d . . . . .
N2 N 0.7485(7) 0.4818(4) 0.2001(3) 0.0305(8) Uani 1 1 d . . . . .
N3 N 0.7871(10) 0.5448(5) 0.0975(4) 0.0657(15) Uani 1 1 d . . . . .
N4 N 0.5564(6) 0.3223(3) 0.5391(3) 0.0181(7) Uani 1 1 d . . . . .
N5 N 0.5318(6) 0.2358(4) 0.6416(3) 0.0214(7) Uani 1 1 d . . . . .
N6 N 0.5007(8) 0.1566(5) 0.7371(3) 0.0472(12) Uani 1 1 d . . . . .
N7 N 1.1756(5) 0.2103(3) 0.4853(3) 0.0179(7) Uani 1 1 d . . . . .
N8 N 1.2027(5) 0.0800(3) 0.5336(3) 0.0175(7) Uani 1 1 d . . . . .
N9 N 1.2228(6) -0.0453(4) 0.5797(3) 0.0313(9) Uani 1 1 d . . . . .
N10 N 1.0975(5) 0.5336(3) 0.3832(3) 0.0152(7) Uani 1 1 d . . . . .
N11 N 1.0909(6) 0.6269(4) 0.2823(3) 0.0335(9) Uani 1 1 d . . . . .
N12 N 1.0914(10) 0.7135(6) 0.1876(4) 0.0728(17) Uani 1 1 d . . . . .
N13 N 0.2963(6) 0.1523(4) 0.1053(3) 0.0229(8) Uani 1 1 d . . . . .
N14 N 0.5214(7) 0.1709(4) 0.0521(3) 0.0322(9) Uani 1 1 d . . . . .
N15 N 0.4120(6) 0.2491(4) 0.2298(3) 0.0216(7) Uani 1 1 d . . . . .
N16 N 0.1573(8) 0.0872(6) 0.0557(4) 0.0315(9) Uani 1 1 d . . . . .
C1 C 0.2351(7) 0.1965(4) 0.2111(3) 0.0211(9) Uani 1 1 d . . . . .
H1 H 0.0870 0.1913 0.2652 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5832(8) 0.2299(5) 0.1294(4) 0.0315(11) Uani 1 1 d . . . . .
H2 H 0.7349 0.2573 0.1170 0.038 Uiso 1 1 calc R U . . .
H16B H 0.135(9) 0.134(6) -0.013(5) 0.040(16) Uiso 1 1 d . . . . .
H16A H 0.244(10) 0.010(6) 0.056(5) 0.06(2) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.001(3) . ?
Cu1 N1 2.004(3) . ?
Cu1 N10 2.015(3) . ?
Cu1 N10 2.022(3) 2_766 ?
Cu1 N7 2.409(3) . ?
Cu2 N15 1.981(3) . ?
Cu2 N7 1.992(3) 1_455 ?
Cu2 N4 2.008(3) . ?
Cu2 N1 2.013(3) . ?
N1 N2 1.206(4) . ?
N2 N3 1.142(5) . ?
N4 N5 1.214(4) . ?
N5 N6 1.132(4) . ?
N7 N8 1.199(4) . ?
N7 Cu2 1.992(3) 1_655 ?
N8 N9 1.155(4) . ?
N10 N11 1.222(5) . ?
N10 Cu1 2.022(3) 2_766 ?
N11 N12 1.143(5) . ?
N13 C1 1.322(4) . ?
N13 N14 1.352(4) . ?
N13 N16 1.401(5) . ?
N14 C2 1.300(5) . ?
N15 C1 1.319(5) . ?
N15 C2 1.365(4) . ?
N16 H16B 0.79(5) . ?
N16 H16A 0.78(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?

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
_geom_angle_publ_flag
N4 Cu1 N1 78.70(12) . . ?
N4 Cu1 N10 175.73(13) . . ?
N1 Cu1 N10 100.81(12) . . ?
N4 Cu1 N10 99.37(12) . 2_766 ?
N1 Cu1 N10 168.27(13) . 2_766 ?
N10 Cu1 N10 80.23(12) . 2_766 ?
N4 Cu1 N7 101.43(12) . . ?
N1 Cu1 N7 101.72(12) . . ?
N10 Cu1 N7 82.83(12) . . ?
N10 Cu1 N7 90.01(11) 2_766 . ?
N15 Cu2 N7 92.87(12) . 1_455 ?
N15 Cu2 N4 170.71(13) . . ?
N7 Cu2 N4 92.90(12) 1_455 . ?
N15 Cu2 N1 97.01(12) . . ?
N7 Cu2 N1 167.55(12) 1_455 . ?
N4 Cu2 N1 78.33(12) . . ?
N2 N1 Cu1 128.8(3) . . ?
N2 N1 Cu2 128.7(3) . . ?
Cu1 N1 Cu2 101.05(13) . . ?
N3 N2 N1 178.0(5) . . ?
N5 N4 Cu1 128.2(3) . . ?
N5 N4 Cu2 121.0(2) . . ?
Cu1 N4 Cu2 101.36(13) . . ?
N6 N5 N4 177.7(4) . . ?
N8 N7 Cu2 120.4(2) . 1_655 ?
N8 N7 Cu1 135.6(2) . . ?
Cu2 N7 Cu1 103.95(13) 1_655 . ?
N9 N8 N7 178.3(4) . . ?
N11 N10 Cu1 123.9(3) . . ?
N11 N10 Cu1 120.4(3) . 2_766 ?
Cu1 N10 Cu1 99.77(12) . 2_766 ?
N12 N11 N10 178.1(5) . . ?
C1 N13 N14 110.8(3) . . ?
C1 N13 N16 126.0(3) . . ?
N14 N13 N16 123.1(3) . . ?
C2 N14 N13 102.4(3) . . ?
C1 N15 C2 103.1(3) . . ?
C1 N15 Cu2 127.8(3) . . ?
C2 N15 Cu2 127.3(3) . . ?
N13 N16 H16B 109(4) . . ?
N13 N16 H16A 101(4) . . ?
H16B N16 H16A 112(5) . . ?
N15 C1 N13 109.3(3) . . ?
N15 C1 H1 125.3 . . ?
N13 C1 H1 125.3 . . ?
N14 C2 N15 114.3(4) . . ?
N14 C2 H2 122.8 . . ?
N15 C2 H2 122.8 . . ?

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
_geom_torsion_publ_flag
C1 N13 N14 C2 -1.3(5) . . . . ?
N16 N13 N14 C2 -178.3(4) . . . . ?
C2 N15 C1 N13 -1.2(5) . . . . ?
Cu2 N15 C1 N13 -166.8(3) . . . . ?
N14 N13 C1 N15 1.7(5) . . . . ?
N16 N13 C1 N15 178.5(4) . . . . ?
N13 N14 C2 N15 0.5(5) . . . . ?
C1 N15 C2 N14 0.4(5) . . . . ?
Cu2 N15 C2 N14 166.1(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N16 H16B N12 0.79(5) 2.43(6) 3.175(7) 158(5) 2_665
N16 H16A N14 0.78(6) 2.38(5) 3.086(6) 151(5) 2_655

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.647
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.105

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_wv537
_database_code_depnum_ccdc_archive 'CCDC 2081738'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;

_vrf_PLAT029_wv537               
; 
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.893 Why? 

RESPONSE: Crystals are twinned.
Solution was performed with hklf4, refinement with hklf5 and a BASF of 0.44193
;
_audit_creation_date             25.01.2019
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1-(3-azidopropyl)-5H-tetrazolyl copper(II) diazide
;
_chemical_name_common            
'1-(3-azidopropyl)-5H-tetrazolyl copper(II) diazide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H7 Cu N13'
_chemical_formula_sum            'C4 H7 Cu N13'
_chemical_formula_weight         300.77

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'



_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.3042(14)
_cell_length_b                   6.2946(5)
_cell_length_c                   10.6903(9)
_cell_angle_alpha                90
_cell_angle_beta                 106.287(3)
_cell_angle_gamma                90
_cell_volume                     1053.10(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    109(2)
_cell_measurement_reflns_used    2480
_cell_measurement_theta_min      3.8167
_cell_measurement_theta_max      28.3018

_exptl_crystal_description       platelet
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.083
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      109(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            2066
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.489
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measured_fraction_theta_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_point_group_measured_fraction_full 0.893
_reflns_number_total             2066
_reflns_number_gt                1905
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+2.0609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2066
_refine_ls_number_parameters     164
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
Cu Cu 0.3201 1.2651 '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_
_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
Cu1 Cu 0.46086(4) 0.54083(7) 0.61583(6) 0.00961(11) Uani 1 1 d . . . . .
N1 N 0.3449(2) 0.5372(6) 0.6412(3) 0.0103(7) Uani 1 1 d . . . . .
N2 N 0.2719(2) 0.4890(6) 0.5474(4) 0.0169(8) Uani 1 1 d . . . . .
N3 N 0.2062(2) 0.5188(6) 0.5906(4) 0.0171(8) Uani 1 1 d . . . . .
N4 N 0.2363(2) 0.5892(6) 0.7143(3) 0.0121(8) Uani 1 1 d . . . . .
N5 N 0.0301(2) 0.3535(7) 0.7203(4) 0.0251(10) Uani 1 1 d . . . . .
N6 N 0.0092(2) 0.2926(7) 0.6069(5) 0.0230(10) Uani 1 1 d . . . . .
N7 N -0.0171(3) 0.2469(8) 0.5004(5) 0.0323(11) Uani 1 1 d . . . . .
N8 N 0.5093(2) 0.6713(5) 0.7922(3) 0.0099(7) Uani 1 1 d . . . . .
N9 N 0.5505(2) 0.5528(5) 0.8755(4) 0.0120(7) Uani 1 1 d . . . . .
N10 N 0.5906(3) 0.4415(6) 0.9568(3) 0.0195(8) Uani 1 1 d . . . . .
N11 N 0.5718(2) 0.5599(6) 0.5699(3) 0.0128(8) Uani 1 1 d . . . . .
N12 N 0.6391(2) 0.5811(5) 0.6539(3) 0.0120(8) Uani 1 1 d . . . . .
N13 N 0.7011(2) 0.6019(6) 0.7358(4) 0.0187(8) Uani 1 1 d . . . . .
C1 C 0.3209(3) 0.5979(7) 0.7434(4) 0.0124(9) Uani 1 1 d . . . . .
H1 H 0.3581 0.6409 0.8249 0.015 Uiso 1 1 calc R U . . .
C2 C 0.1792(3) 0.6439(7) 0.7946(4) 0.0163(9) Uani 1 1 d . . . . .
H2A H 0.1234 0.6912 0.7371 0.020 Uiso 1 1 calc R U . . .
H2B H 0.2043 0.7636 0.8530 0.020 Uiso 1 1 calc R U . . .
C3 C 0.1651(3) 0.4554(8) 0.8768(5) 0.0228(10) Uani 1 1 d . . . . .
H3A H 0.2215 0.4020 0.9288 0.027 Uiso 1 1 calc R U . . .
H3B H 0.1341 0.5061 0.9386 0.027 Uiso 1 1 calc R U . . .
C4 C 0.1159(3) 0.2740(8) 0.7994(5) 0.0213(11) Uani 1 1 d . . . . .
H4A H 0.1478 0.2149 0.7409 0.026 Uiso 1 1 calc R U . . .
H4B H 0.1084 0.1598 0.8589 0.026 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.984(3) . ?
Cu1 N8 2.004(3) . ?
Cu1 N11 2.007(3) . ?
Cu1 N11 2.009(4) 3_666 ?
N1 C1 1.317(5) . ?
N1 N2 1.358(5) . ?
N2 N3 1.294(5) . ?
N3 N4 1.349(5) . ?
N4 C1 1.327(5) . ?
N4 C2 1.473(5) . ?
N5 N6 1.225(6) . ?
N5 C4 1.503(6) . ?
N6 N7 1.135(7) . ?
N8 N9 1.210(5) . ?
N9 N10 1.164(5) . ?
N11 N12 1.214(5) . ?
N11 Cu1 2.009(4) 3_666 ?
N12 N13 1.144(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.533(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.503(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?

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
_geom_angle_publ_flag
N1 Cu1 N8 90.91(14) . . ?
N1 Cu1 N11 173.33(15) . . ?
N8 Cu1 N11 93.47(14) . . ?
N1 Cu1 N11 97.61(14) . 3_666 ?
N8 Cu1 N11 169.86(14) . 3_666 ?
N11 Cu1 N11 77.57(15) . 3_666 ?
C1 N1 N2 106.0(3) . . ?
C1 N1 Cu1 128.8(3) . . ?
N2 N1 Cu1 124.9(3) . . ?
N3 N2 N1 110.2(3) . . ?
N2 N3 N4 106.7(3) . . ?
C1 N4 N3 108.2(3) . . ?
C1 N4 C2 129.7(3) . . ?
N3 N4 C2 122.1(3) . . ?
N6 N5 C4 114.2(4) . . ?
N7 N6 N5 173.5(5) . . ?
N9 N8 Cu1 115.5(3) . . ?
N10 N9 N8 179.0(4) . . ?
N12 N11 Cu1 121.0(3) . . ?
N12 N11 Cu1 134.4(3) . 3_666 ?
Cu1 N11 Cu1 102.43(15) . 3_666 ?
N13 N12 N11 177.9(4) . . ?
N1 C1 N4 108.9(4) . . ?
N1 C1 H1 125.6 . . ?
N4 C1 H1 125.6 . . ?
N4 C2 C3 112.0(4) . . ?
N4 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
N4 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 114.5(4) . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
N5 C4 C3 109.0(4) . . ?
N5 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
N5 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?

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
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.1(5) . . . . ?
Cu1 N1 N2 N3 -174.3(3) . . . . ?
N1 N2 N3 N4 0.5(5) . . . . ?
N2 N3 N4 C1 -0.7(5) . . . . ?
N2 N3 N4 C2 179.0(4) . . . . ?
N2 N1 C1 N4 -0.4(5) . . . . ?
Cu1 N1 C1 N4 173.6(3) . . . . ?
N3 N4 C1 N1 0.7(5) . . . . ?
C2 N4 C1 N1 -179.0(4) . . . . ?
C1 N4 C2 C3 -87.7(6) . . . . ?
N3 N4 C2 C3 92.6(5) . . . . ?
N4 C2 C3 C4 -67.2(5) . . . . ?
N6 N5 C4 C3 134.7(4) . . . . ?
C2 C3 C4 N5 -58.5(5) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N10 0.95 2.31 3.134(5) 145.1 3_667
C2 H2A N7 0.99 2.67 3.568(7) 150.8 3_566
C2 H2B N2 0.99 2.58 3.554(6) 166.7 4_576
C3 H3B N7 0.99 2.66 3.563(7) 152.1 2_556
C4 H4A N13 0.99 2.51 3.293(6) 135.9 2_646
C1 H1 N10 0.95 2.31 3.134(5) 145.1 3_667
C2 H2A N7 0.99 2.67 3.568(7) 150.8 3_566
C2 H2B N2 0.99 2.58 3.554(6) 166.7 4_576
C3 H3B N7 0.99 2.66 3.563(7) 152.1 2_556
C4 H4A N13 0.99 2.51 3.293(6) 135.9 2_646

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.739
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.099

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_vv605
_database_code_depnum_ccdc_archive 'CCDC 2081732'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             ' 11.09.2017'
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
di(1-methyl-5-aminotetrazolyl) tri-copper(II) hexazide
;
_chemical_name_common            
'di(1-methyl-5-aminotetrazolyl) tri-copper(II) hexazide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H10 Cu3 N28'
_chemical_formula_sum            'C4 H10 Cu3 N28'
_chemical_formula_weight         641.02

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2454(4)
_cell_length_b                   8.5723(5)
_cell_length_c                   10.1414(6)
_cell_angle_alpha                91.435(2)
_cell_angle_beta                 106.685(2)
_cell_angle_gamma                102.203(2)
_cell_volume                     506.20(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5974
_cell_measurement_theta_min      3.0747
_cell_measurement_theta_max      27.0945

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.189
_shelx_estimated_absorpt_T_min   0.784
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_F_000             317
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            8877
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.075
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1989
_reflns_number_gt                1801
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+0.2807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1989
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0524
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
Cu Cu 0.3201 1.2651 '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_
_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
Cu1 Cu 0.0000 0.0000 0.0000 0.02072(10) Uani 1 2 d S . P . .
Cu2 Cu -0.24179(4) 0.33340(3) -0.03166(2) 0.02170(9) Uani 1 1 d . . . . .
N1 N -0.2154(3) 0.12222(19) -0.11109(17) 0.0221(3) Uani 1 1 d . . . . .
N2 N -0.3739(3) 0.0589(2) -0.21202(19) 0.0282(4) Uani 1 1 d . . . . .
N3 N -0.5209(4) 0.0031(3) -0.3070(3) 0.0544(6) Uani 1 1 d . . . . .
N4 N -0.1761(3) 0.5498(2) 0.06751(19) 0.0291(4) Uani 1 1 d . . . . .
N5 N -0.2637(3) 0.65749(19) 0.02936(17) 0.0233(4) Uani 1 1 d . . . . .
N6 N -0.3405(3) 0.7676(2) -0.0019(2) 0.0352(4) Uani 1 1 d . . . . .
N7 N -0.0073(3) 0.2032(2) 0.36586(17) 0.0243(4) Uani 1 1 d . . . . .
N8 N 0.0620(3) 0.1021(2) 0.29255(17) 0.0253(4) Uani 1 1 d . . . . .
N9 N -0.0127(3) 0.12987(19) 0.16588(17) 0.0214(3) Uani 1 1 d . . . . .
N10 N -0.1318(3) 0.24735(19) 0.15175(16) 0.0210(3) Uani 1 1 d . . . . .
N11 N -0.2384(4) 0.3933(2) 0.31768(19) 0.0347(5) Uani 1 1 d . . . . .
H11A H -0.2460 0.3806 0.3867 0.042 Uiso 1 1 d R U . . .
H11B H -0.3102 0.4413 0.2550 0.042 Uiso 1 1 d R U . . .
N12 N -0.4112(3) 0.4008(2) -0.20635(19) 0.0335(4) Uani 1 1 d . . . . .
N13 N -0.3569(3) 0.4038(2) -0.3052(2) 0.0331(4) Uani 1 1 d . . . . .
N14 N -0.3108(6) 0.4105(5) -0.4076(3) 0.0823(10) Uani 1 1 d . . . . .
C1 C -0.1326(3) 0.2896(2) 0.2794(2) 0.0223(4) Uani 1 1 d . . . . .
C2 C 0.0478(5) 0.2079(3) 0.5160(2) 0.0381(6) Uani 1 1 d . . . . .
H2A H -0.0833 0.1507 0.5402 0.057 Uiso 1 1 calc R U . . .
H2B H 0.0881 0.3172 0.5548 0.057 Uiso 1 1 calc R U . . .
H2C H 0.1747 0.1587 0.5519 0.057 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.9901(16) 2 ?
Cu1 N1 1.9901(16) . ?
Cu1 N9 2.0239(16) 2 ?
Cu1 N9 2.0239(16) . ?
Cu2 N12 1.9557(18) . ?
Cu2 N4 1.9924(18) . ?
Cu2 N10 2.0062(16) . ?
Cu2 N1 2.0206(16) . ?
N1 N2 1.219(2) . ?
N2 N3 1.133(3) . ?
N4 N5 1.188(2) . ?
N5 N6 1.158(2) . ?
N7 N8 1.342(2) . ?
N7 C1 1.346(3) . ?
N7 C2 1.459(3) . ?
N8 N9 1.282(2) . ?
N9 N10 1.360(2) . ?
N10 C1 1.337(3) . ?
N11 C1 1.325(3) . ?
N11 H11A 0.7247 . ?
N11 H11B 0.8376 . ?
N12 N13 1.147(3) . ?
N13 N14 1.154(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
_geom_angle_publ_flag
N1 Cu1 N1 180.0 2 . ?
N1 Cu1 N9 85.39(6) 2 2 ?
N1 Cu1 N9 94.61(6) . 2 ?
N1 Cu1 N9 94.61(6) 2 . ?
N1 Cu1 N9 85.39(6) . . ?
N9 Cu1 N9 180.0 2 . ?
N12 Cu2 N4 92.91(8) . . ?
N12 Cu2 N10 168.28(8) . . ?
N4 Cu2 N10 88.66(7) . . ?
N12 Cu2 N1 96.51(7) . . ?
N4 Cu2 N1 164.45(7) . . ?
N10 Cu2 N1 84.63(6) . . ?
N2 N1 Cu1 121.78(13) . . ?
N2 N1 Cu2 115.11(13) . . ?
Cu1 N1 Cu2 120.65(8) . . ?
N3 N2 N1 178.6(2) . . ?
N5 N4 Cu2 127.23(15) . . ?
N6 N5 N4 176.4(2) . . ?
N8 N7 C1 109.49(16) . . ?
N8 N7 C2 122.07(17) . . ?
C1 N7 C2 128.42(18) . . ?
N9 N8 N7 106.06(15) . . ?
N8 N9 N10 111.79(15) . . ?
N8 N9 Cu1 125.97(12) . . ?
N10 N9 Cu1 121.75(12) . . ?
C1 N10 N9 105.49(15) . . ?
C1 N10 Cu2 133.27(13) . . ?
N9 N10 Cu2 121.02(12) . . ?
C1 N11 H11A 109.7 . . ?
C1 N11 H11B 116.5 . . ?
H11A N11 H11B 131.5 . . ?
N13 N12 Cu2 124.82(15) . . ?
N12 N13 N14 176.6(2) . . ?
N11 C1 N10 128.09(18) . . ?
N11 C1 N7 124.81(18) . . ?
N10 C1 N7 107.09(17) . . ?
N7 C2 H2A 109.5 . . ?
N7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

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
_geom_torsion_publ_flag
C1 N7 N8 N9 2.0(2) . . . . ?
C2 N7 N8 N9 -179.5(2) . . . . ?
N7 N8 N9 N10 -0.2(2) . . . . ?
N7 N8 N9 Cu1 -172.18(13) . . . . ?
N8 N9 N10 C1 -1.6(2) . . . . ?
Cu1 N9 N10 C1 170.75(13) . . . . ?
N8 N9 N10 Cu2 173.54(13) . . . . ?
Cu1 N9 N10 Cu2 -14.1(2) . . . . ?
N9 N10 C1 N11 -175.9(2) . . . . ?
Cu2 N10 C1 N11 9.8(3) . . . . ?
N9 N10 C1 N7 2.7(2) . . . . ?
Cu2 N10 C1 N7 -171.57(14) . . . . ?
N8 N7 C1 N11 175.7(2) . . . . ?
C2 N7 C1 N11 -2.8(4) . . . . ?
N8 N7 C1 N10 -3.0(2) . . . . ?
C2 N7 C1 N10 178.6(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11A N14 0.72 2.25 2.953(3) 162.3 1_556
N11 H11B N4 0.84 2.42 2.984(3) 125.4 .
N11 H11B N12 0.84 2.37 3.081(2) 142.4 2_465
C2 H2B N11 0.96 2.62 3.576(3) 173.3 2_566
C2 H2C N3 0.96 2.65 3.597(3) 167.2 1_656
N11 H11A N14 0.72 2.25 2.953(3) 162.3 1_556
N11 H11B N4 0.84 2.42 2.984(3) 125.4 .
N11 H11B N12 0.84 2.37 3.081(2) 142.4 2_465
C2 H2B N11 0.96 2.62 3.576(3) 173.3 2_566
C2 H2C N3 0.96 2.65 3.597(3) 167.2 1_656

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.264
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx334
_database_code_depnum_ccdc_archive 'CCDC 2081731'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Jul 08 08:41:56 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetra-copper(II) octa-azido ditetrazolylpropane
;
_chemical_name_common            
'tetra-copper(II) octa-azido ditetrazolylpropane'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H8 Cu4 N32'
_chemical_formula_sum            'C5 H8 Cu4 N32'
_chemical_formula_weight         770.59

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'


_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.
;

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'

_cell_length_a                   18.2752(11)
_cell_length_b                   5.5456(3)
_cell_length_c                   24.0470(13)
_cell_angle_alpha                90
_cell_angle_beta                 100.556(5)
_cell_angle_gamma                90
_cell_volume                     2395.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2304
_cell_measurement_theta_min      4.4620
_cell_measurement_theta_max      31.7020

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.574
_shelx_estimated_absorpt_T_min   0.268
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74931
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            9212
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         4.299
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2347
_reflns_number_gt                1894
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+0.3081P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2347
_refine_ls_number_parameters     186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0030128000
_diffrn_orient_matrix_UB_12      -0.0202021000
_diffrn_orient_matrix_UB_13      -0.0294675000
_diffrn_orient_matrix_UB_21      -0.0334718000
_diffrn_orient_matrix_UB_22      0.0677404000
_diffrn_orient_matrix_UB_23      -0.0052566000
_diffrn_orient_matrix_UB_31      0.0207337000
_diffrn_orient_matrix_UB_32      0.1065212000
_diffrn_orient_matrix_UB_33      -0.0022491000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -84.00   41.80   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000   30.0000 148

#__ type_ start__ end____ width___ exp.time_
  2 omega -102.00  -68.00   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -90.0000 40

#__ type_ start__ end____ width___ exp.time_
  3 omega  -97.00  -23.90   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000   30.0000 86

#__ type_ start__ end____ width___ exp.time_
  4 omega  -24.00   44.00   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  150.0000 80

#__ type_ start__ end____ width___ exp.time_
  5 omega  -23.00   74.75   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 115

#__ type_ start__ end____ width___ exp.time_
  6 omega   -1.00   87.40   0.8500   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -125.0000  151.0000 104

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
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'


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
Cu1 Cu 0.21065(2) 0.02649(7) 0.01906(2) 0.01129(13) Uani 1 1 d . . . . .
Cu2 Cu 0.14058(2) 0.56132(7) 0.05555(2) 0.01246(14) Uani 1 1 d . . . . .
N8 N 0.30566(19) 0.3509(5) 0.09750(15) 0.0285(8) Uani 1 1 d . . . . .
N10 N 0.10197(16) 0.2658(5) 0.01429(12) 0.0140(6) Uani 1 1 d . . . . .
N4 N 0.16157(16) -0.2753(5) -0.01418(12) 0.0124(6) Uani 1 1 d . . . . .
N5 N 0.12150(17) -0.3122(5) -0.05990(14) 0.0197(7) Uani 1 1 d . . . . .
N15 N 0.08522(16) 0.4514(5) 0.20670(12) 0.0172(7) Uani 1 1 d . . . . .
N16 N 0.06889(18) 0.2259(5) 0.19055(14) 0.0231(7) Uani 1 1 d . . . . .
C1 C 0.0882(2) 0.2198(6) 0.14046(16) 0.0202(8) Uani 1 1 d . . . . .
H1 H 0.0836 0.0813 0.1168 0.024 Uiso 1 1 calc R U . . .
N13 N 0.11500(16) 0.4326(5) 0.12667(12) 0.0153(6) Uani 1 1 d . . . . .
N14 N 0.11310(16) 0.5806(5) 0.16987(12) 0.0179(7) Uani 1 1 d . . . . .
C2 C 0.0714(2) 0.5562(7) 0.25932(16) 0.0255(9) Uani 1 1 d . . . . .
H2A H 0.1137 0.6611 0.2756 0.031 Uiso 1 1 calc R U . . .
H2B H 0.0678 0.4257 0.2868 0.031 Uiso 1 1 calc R U . . .
N1 N 0.20261(16) -0.1597(5) 0.08869(12) 0.0130(6) Uani 1 1 d . . . . .
N12 N -0.01759(18) 0.2304(5) -0.04173(14) 0.0238(7) Uani 1 1 d . . . . .
N6 N 0.0856(2) -0.3586(7) -0.10249(15) 0.0466(11) Uani 1 1 d . . . . .
C3 C 0.0000 0.7033(9) 0.2500 0.0293(14) Uani 1 2 d S T P . .
H3A H -0.0005 0.8089 0.2167 0.035 Uiso 0.5 1 calc R U P . .
H3B H 0.0005 0.8089 0.2833 0.035 Uiso 0.5 1 calc R U P . .
N9 N 0.3409(3) 0.3931(8) 0.14088(19) 0.0786(19) Uani 1 1 d . . . . .
N7 N 0.26672(16) 0.3191(5) 0.05198(12) 0.0131(6) Uani 1 1 d . . . . .
N11 N 0.04108(16) 0.2517(4) -0.01424(12) 0.0136(7) Uani 1 1 d . . . . .
N2 N 0.22920(17) -0.1101(5) 0.13771(14) 0.0204(7) Uani 1 1 d . . . . .
N3 N 0.2527(2) -0.0624(7) 0.18378(15) 0.0432(10) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.995(3) . ?
Cu1 N4 1.995(3) . ?
Cu1 N7 2.003(3) . ?
Cu1 N7 2.020(3) 7 ?
Cu1 N10 2.374(3) . ?
Cu2 N10 1.978(3) . ?
Cu2 N13 1.986(3) . ?
Cu2 N1 1.996(3) 1_565 ?
Cu2 N4 2.004(3) 1_565 ?
N8 N9 1.146(5) . ?
N8 N7 1.204(4) . ?
N10 N11 1.198(4) . ?
N4 N5 1.222(4) . ?
N4 Cu2 2.004(3) 1_545 ?
N5 N6 1.140(4) . ?
N15 N14 1.313(4) . ?
N15 N16 1.327(4) . ?
N15 C2 1.456(4) . ?
N16 C1 1.316(5) . ?
C1 N13 1.343(4) . ?
C1 H1 0.9500 . ?
N13 N14 1.329(4) . ?
C2 C3 1.520(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N1 N2 1.221(4) . ?
N1 Cu2 1.996(3) 1_545 ?
N12 N11 1.158(4) . ?
C3 C2 1.520(5) 2 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N7 Cu1 2.020(3) 7 ?
N2 N3 1.143(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
_geom_angle_publ_flag
N1 Cu1 N4 78.78(11) . . ?
N1 Cu1 N7 101.45(11) . . ?
N4 Cu1 N7 176.03(11) . . ?
N1 Cu1 N7 170.69(11) . 7 ?
N4 Cu1 N7 99.40(11) . 7 ?
N7 Cu1 N7 79.73(12) . 7 ?
N1 Cu1 N10 98.06(11) . . ?
N4 Cu1 N10 97.98(10) . . ?
N7 Cu1 N10 85.93(10) . . ?
N7 Cu1 N10 91.22(11) 7 . ?
N10 Cu2 N13 90.89(12) . . ?
N10 Cu2 N1 165.25(12) . 1_565 ?
N13 Cu2 N1 98.09(11) . 1_565 ?
N10 Cu2 N4 93.46(12) . 1_565 ?
N13 Cu2 N4 173.84(11) . 1_565 ?
N1 Cu2 N4 78.57(11) 1_565 1_565 ?
N9 N8 N7 176.3(5) . . ?
N11 N10 Cu2 123.4(2) . . ?
N11 N10 Cu1 132.2(2) . . ?
Cu2 N10 Cu1 102.74(12) . . ?
N5 N4 Cu1 130.7(2) . . ?
N5 N4 Cu2 120.2(2) . 1_545 ?
Cu1 N4 Cu2 100.65(12) . 1_545 ?
N6 N5 N4 176.4(4) . . ?
N14 N15 N16 114.3(3) . . ?
N14 N15 C2 121.3(3) . . ?
N16 N15 C2 124.4(3) . . ?
C1 N16 N15 102.0(3) . . ?
N16 C1 N13 112.0(3) . . ?
N16 C1 H1 124.0 . . ?
N13 C1 H1 124.0 . . ?
N14 N13 C1 106.7(3) . . ?
N14 N13 Cu2 119.7(2) . . ?
C1 N13 Cu2 133.0(2) . . ?
N15 N14 N13 105.0(3) . . ?
N15 C2 C3 111.5(3) . . ?
N15 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
N15 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N2 N1 Cu1 128.0(2) . . ?
N2 N1 Cu2 131.0(2) . 1_545 ?
Cu1 N1 Cu2 100.94(12) . 1_545 ?
C2 C3 C2 115.1(4) . 2 ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 2 . ?
C2 C3 H3B 108.5 . . ?
C2 C3 H3B 108.5 2 . ?
H3A C3 H3B 107.5 . . ?
N8 N7 Cu1 130.7(2) . . ?
N8 N7 Cu1 121.9(2) . 7 ?
Cu1 N7 Cu1 100.27(12) . 7 ?
N12 N11 N10 177.9(3) . . ?
N3 N2 N1 178.6(4) . . ?

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
_geom_torsion_publ_flag
N14 N15 N16 C1 -0.2(4) . . . . ?
C2 N15 N16 C1 177.4(3) . . . . ?
N15 N16 C1 N13 -0.1(4) . . . . ?
N16 C1 N13 N14 0.3(4) . . . . ?
N16 C1 N13 Cu2 -170.3(3) . . . . ?
N16 N15 N14 N13 0.3(4) . . . . ?
C2 N15 N14 N13 -177.3(3) . . . . ?
C1 N13 N14 N15 -0.3(4) . . . . ?
Cu2 N13 N14 N15 171.7(2) . . . . ?
N14 N15 C2 C3 78.8(4) . . . . ?
N16 N15 C2 C3 -98.6(4) . . . . ?
N15 C2 C3 C2 75.1(3) . . . 2 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N12 0.95 2.63 3.523(5) 157.1 5
C2 H2A N9 0.99 2.40 3.226(5) 140.5 4
C2 H2B N6 0.99 2.65 3.463(5) 139.6 6_556
C1 H1 N12 0.95 2.63 3.523(5) 157.1 5
C2 H2A N9 0.99 2.40 3.226(5) 140.5 4
C2 H2B N6 0.99 2.65 3.463(5) 139.6 6_556

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.771
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.109

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ox139
_database_code_depnum_ccdc_archive 'CCDC 2081737'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             2019-04-17
_audit_creation_method           SHELXL-2018/3


_chemical_name_systematic        
'tetrakis(triaminotriazole) hexakisazido tricopper(II) monohydrate'
_chemical_name_common            
'tetrakis(triaminotriazole) hexakisazido tricopper(II) monohydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Cu3 N42, 2(H O0.50)'
_chemical_formula_sum            'C8 H26 Cu3 N42 O'
_chemical_formula_weight         917.33

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2469(17)
_cell_length_b                   9.8260(10)
_cell_length_c                   10.3622(19)
_cell_angle_alpha                109.261(15)
_cell_angle_beta                 96.057(15)
_cell_angle_gamma                115.091(15)
_cell_volume                     771.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1029
_cell_measurement_theta_min      3.5640
_cell_measurement_theta_max      27.2100

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.140
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           ?


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_F_000             463
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            4240
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.557
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3113
_reflns_number_gt                2313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0311P)²+1.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3113
_refine_ls_number_parameters     296
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000



_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix.  The
cell esds are taken into account individually in the estimation
of esds in distances, angles and torsion angles; correlations
between esds in cell parameters are only used when they are
defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving
l.s. planes
;



_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0435213000
_diffrn_orient_matrix_UB_12      -0.0345168000
_diffrn_orient_matrix_UB_13      -0.0732552000
_diffrn_orient_matrix_UB_21      -0.0764514000
_diffrn_orient_matrix_UB_22      -0.0208381000
_diffrn_orient_matrix_UB_23      0.0174629000
_diffrn_orient_matrix_UB_31      0.0089053000
_diffrn_orient_matrix_UB_32      0.0778281000
_diffrn_orient_matrix_UB_33      0.0076496000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  48.00   1.00   30.00    --  -20.29  77.00 -30.00  101
  2  ω     -9.00  93.00   1.00   30.00    --   21.31  77.00-150.00  102
  3  ω     -9.00  93.00   1.00   30.00    --   21.31  77.00  90.00  102
;



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'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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'


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
Cu1 Cu 1.000000 0.500000 0.000000 0.0118(2) Uani 1 2 d S . P . .
Cu2 Cu 0.97122(8) 0.79830(7) 0.26604(6) 0.01531(18) Uani 1 1 d . . . . .
N1 N 0.9132(5) 0.4555(5) 0.1622(4) 0.0116(8) Uani 1 1 d . . . . .
N2 N 0.9153(5) 0.5843(5) 0.2777(4) 0.0150(9) Uani 1 1 d . . . . .
N3 N 0.8270(5) 0.3645(5) 0.3214(4) 0.0183(9) Uani 1 1 d . . . . .
N4 N 0.8460(7) 0.6031(6) 0.4953(5) 0.0235(11) Uani 1 1 d . . . . .
N5 N 0.7615(9) 0.2677(6) 0.3934(6) 0.0296(13) Uani 1 1 d . . . . .
N6 N 0.8316(6) 0.1746(5) 0.1110(5) 0.0272(11) Uani 1 1 d . . . . .
H6A H 0.830809 0.121084 0.155862 0.033 Uiso 1 1 d R U . . .
H6B H 0.896308 0.191184 0.073662 0.033 Uiso 1 1 d R U . . .
N7 N 0.8284(5) 0.5640(5) -0.0408(4) 0.0153(9) Uani 1 1 d . . . . .
N8 N 0.8034(5) 0.6730(5) 0.0718(4) 0.0184(9) Uani 1 1 d . . . . .
N9 N 0.6154(5) 0.5827(5) -0.1268(4) 0.0139(9) Uani 1 1 d . . . . .
N10 N 0.6045(8) 0.7679(8) 0.0795(6) 0.0393(15) Uani 1 1 d . . . . .
N11 N 0.4856(5) 0.5726(5) -0.2190(5) 0.0211(10) Uani 1 1 d . . . . .
H11B H 0.545893 0.639332 -0.253877 0.025 Uiso 1 1 d R U . . .
H11A H 0.391092 0.457432 -0.238378 0.025 Uiso 1 1 d R U . . .
N12 N 0.7025(7) 0.4230(6) -0.2942(5) 0.0238(11) Uani 1 1 d . . . . .
N13 N 1.1673(5) 0.7803(5) 0.1587(4) 0.0180(9) Uani 1 1 d . . . . .
N14 N 1.3127(6) 0.8675(6) 0.2091(5) 0.0244(10) Uani 1 1 d . . . . .
N15 N 1.4546(7) 0.9487(8) 0.2607(7) 0.0630(19) Uani 1 1 d . . . . .
N16 N 0.9986(8) 1.0099(6) 0.2681(5) 0.0330(13) Uani 1 1 d . . . . .
N19 N 1.1271(6) 0.9089(5) 0.4633(4) 0.0215(10) Uani 1 1 d . . . . .
N20 N 1.2069(5) 1.0533(5) 0.5347(5) 0.0206(10) Uani 1 1 d . . . . .
C1 C 0.8636(6) 0.5263(6) 0.3707(5) 0.0149(10) Uani 1 1 d . . . . .
C2 C 0.8595(6) 0.3261(6) 0.1922(5) 0.0178(11) Uani 1 1 d . . . . .
C3 C 0.6753(6) 0.6809(6) 0.0152(5) 0.0194(11) Uani 1 1 d . . . . .
C4 C 0.7159(6) 0.5146(6) -0.1581(5) 0.0145(10) Uani 1 1 d . . . . .
N21 N 1.2843(6) 1.1940(5) 0.6095(5) 0.0342(13) Uani 1 1 d . . . . .
N18A N 1.145(3) 1.106(2) 0.113(3) 0.042(7) Uani 0.44(3) 1 d . . P A 1
N17A N 1.0871(19) 1.0621(19) 0.193(2) 0.012(4) Uiso 0.44(3) 1 d . . P A 1
N18B N 1.225(2) 1.1633(19) 0.219(3) 0.052(6) Uani 0.56(3) 1 d . . P A 2
N17B N 1.1042(16) 1.0816(16) 0.242(2) 0.021(3) Uani 0.56(3) 1 d . . P A 2
O1 O 0.4517(17) 0.2857(18) -0.5683(15) 0.104(5) Uani 0.5 1 d . . P . .
H1A H 0.423020 0.172646 -0.679520 0.125 Uiso 0.5 1 d R U P . .
H1B H 0.361002 0.340536 -0.510042 0.125 Uiso 0.5 1 d R U P . .
H4A H 0.804(6) 0.542(6) 0.540(5) 0.015(14) Uiso 1 1 d . . . . .
H4B H 0.857(7) 0.686(7) 0.514(6) 0.016(16) Uiso 1 1 d . . . . .
H5B H 0.674(6) 0.182(6) 0.343(5) 0.005(14) Uiso 1 1 d . . . . .
H5A H 0.819(8) 0.226(9) 0.406(7) 0.05(2) Uiso 1 1 d . . . . .
H10A H 0.632(6) 0.812(6) 0.160(6) 0.015(15) Uiso 1 1 d . . . . .
H10B H 0.526(8) 0.752(8) 0.022(7) 0.05(2) Uiso 1 1 d . . . . .
H12B H 0.754(9) 0.379(9) -0.288(7) 0.06(2) Uiso 1 1 d . . . . .
H12A H 0.608(7) 0.370(7) -0.335(6) 0.026(18) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N7 1.993(4) . ?
Cu1 N7 1.993(4) 2_765 ?
Cu1 N1 2.033(4) 2_765 ?
Cu1 N1 2.033(4) . ?
Cu1 N13 2.355(4) 2_765 ?
Cu1 N13 2.355(4) . ?
Cu2 N16 1.977(4) . ?
Cu2 N2 1.991(4) . ?
Cu2 N19 2.005(4) . ?
Cu2 N8 2.015(4) . ?
Cu2 N13 2.264(4) . ?
N1 C2 1.311(6) . ?
N1 N2 1.417(5) . ?
N2 C1 1.308(6) . ?
N3 C2 1.369(6) . ?
N3 C1 1.369(6) . ?
N3 N5 1.380(6) . ?
N4 C1 1.330(6) . ?
N4 H4A 0.87(5) . ?
N4 H4B 0.74(5) . ?
N5 H5B 0.82(5) . ?
N5 H5A 0.82(7) . ?
N6 C2 1.339(6) . ?
N6 H6A 0.8066 . ?
N6 H6B 0.7363 . ?
N7 C4 1.308(6) . ?
N7 N8 1.416(5) . ?
N8 C3 1.309(6) . ?
N9 C3 1.357(6) . ?
N9 C4 1.365(6) . ?
N9 N11 1.400(5) . ?
N10 C3 1.339(7) . ?
N10 H10A 0.76(5) . ?
N10 H10B 0.81(6) . ?
N11 H11B 0.8716 . ?
N11 H11A 1.0292 . ?
N12 C4 1.358(7) . ?
N12 H12B 0.78(7) . ?
N12 H12A 0.78(6) . ?
N13 N14 1.181(6) . ?
N14 N15 1.152(7) . ?
N16 N17B 1.057(13) . ?
N16 N17A 1.259(18) . ?
N19 N20 1.187(6) . ?
N20 N21 1.167(6) . ?
N18A N17A 1.137(18) . ?
N18B N17B 1.177(15) . ?
O1 H1A 1.2140 . ?
O1 H1B 1.2780 . ?

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
_geom_angle_publ_flag
N7 Cu1 N7 180.0 . 2_765 ?
N7 Cu1 N1 90.62(15) . 2_765 ?
N7 Cu1 N1 89.38(15) 2_765 2_765 ?
N7 Cu1 N1 89.38(15) . . ?
N7 Cu1 N1 90.62(15) 2_765 . ?
N1 Cu1 N1 180.0 2_765 . ?
N7 Cu1 N13 95.01(15) . 2_765 ?
N7 Cu1 N13 84.99(15) 2_765 2_765 ?
N1 Cu1 N13 88.59(14) 2_765 2_765 ?
N1 Cu1 N13 91.41(15) . 2_765 ?
N7 Cu1 N13 84.99(15) . . ?
N7 Cu1 N13 95.01(15) 2_765 . ?
N1 Cu1 N13 91.41(14) 2_765 . ?
N1 Cu1 N13 88.59(14) . . ?
N13 Cu1 N13 180.0(3) 2_765 . ?
N16 Cu2 N2 171.10(19) . . ?
N16 Cu2 N19 92.7(2) . . ?
N2 Cu2 N19 87.03(16) . . ?
N16 Cu2 N8 90.7(2) . . ?
N2 Cu2 N8 89.18(16) . . ?
N19 Cu2 N8 175.58(17) . . ?
N16 Cu2 N13 99.27(19) . . ?
N2 Cu2 N13 89.63(15) . . ?
N19 Cu2 N13 93.58(17) . . ?
N8 Cu2 N13 88.66(16) . . ?
C2 N1 N2 106.8(4) . . ?
C2 N1 Cu1 132.9(3) . . ?
N2 N1 Cu1 120.1(3) . . ?
C1 N2 N1 107.8(4) . . ?
C1 N2 Cu2 132.5(3) . . ?
N1 N2 Cu2 119.4(3) . . ?
C2 N3 C1 106.5(4) . . ?
C2 N3 N5 130.8(4) . . ?
C1 N3 N5 122.6(4) . . ?
C1 N4 H4A 115(3) . . ?
C1 N4 H4B 118(4) . . ?
H4A N4 H4B 125(5) . . ?
N3 N5 H5B 113(3) . . ?
N3 N5 H5A 110(5) . . ?
H5B N5 H5A 98(6) . . ?
C2 N6 H6A 113.2 . . ?
C2 N6 H6B 103.0 . . ?
H6A N6 H6B 115.8 . . ?
C4 N7 N8 107.5(4) . . ?
C4 N7 Cu1 132.0(3) . . ?
N8 N7 Cu1 120.2(3) . . ?
C3 N8 N7 106.5(4) . . ?
C3 N8 Cu2 133.7(4) . . ?
N7 N8 Cu2 119.3(3) . . ?
C3 N9 C4 106.6(4) . . ?
C3 N9 N11 123.8(4) . . ?
C4 N9 N11 129.3(4) . . ?
C3 N10 H10A 119(4) . . ?
C3 N10 H10B 111(5) . . ?
H10A N10 H10B 129(6) . . ?
N9 N11 H11B 98.2 . . ?
N9 N11 H11A 100.5 . . ?
H11B N11 H11A 147.8 . . ?
C4 N12 H12B 106(5) . . ?
C4 N12 H12A 107(4) . . ?
H12B N12 H12A 119(7) . . ?
N14 N13 Cu2 125.5(3) . . ?
N14 N13 Cu1 133.3(3) . . ?
Cu2 N13 Cu1 95.80(15) . . ?
N15 N14 N13 177.5(6) . . ?
N17B N16 Cu2 117.2(6) . . ?
N17A N16 Cu2 114.5(7) . . ?
N20 N19 Cu2 126.5(4) . . ?
N21 N20 N19 177.3(5) . . ?
N2 C1 N4 128.8(5) . . ?
N2 C1 N3 109.2(4) . . ?
N4 C1 N3 122.0(5) . . ?
N1 C2 N6 127.7(5) . . ?
N1 C2 N3 109.7(4) . . ?
N6 C2 N3 122.6(5) . . ?
N8 C3 N10 128.6(5) . . ?
N8 C3 N9 110.1(4) . . ?
N10 C3 N9 121.4(5) . . ?
N7 C4 N12 128.3(5) . . ?
N7 C4 N9 109.2(4) . . ?
N12 C4 N9 122.3(5) . . ?
N18A N17A N16 169.6(16) . . ?
N16 N17B N18B 177.5(17) . . ?
H1A O1 H1B 133.4 . . ?

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
_geom_torsion_publ_flag
C2 N1 N2 C1 0.2(5) . . . . ?
Cu1 N1 N2 C1 -175.9(3) . . . . ?
C2 N1 N2 Cu2 -174.7(3) . . . . ?
Cu1 N1 N2 Cu2 9.1(4) . . . . ?
C4 N7 N8 C3 0.8(5) . . . . ?
Cu1 N7 N8 C3 -174.8(3) . . . . ?
C4 N7 N8 Cu2 -172.2(3) . . . . ?
Cu1 N7 N8 Cu2 12.3(5) . . . . ?
N1 N2 C1 N4 179.7(5) . . . . ?
Cu2 N2 C1 N4 -6.3(8) . . . . ?
N1 N2 C1 N3 -0.2(5) . . . . ?
Cu2 N2 C1 N3 173.8(3) . . . . ?
C2 N3 C1 N2 0.1(6) . . . . ?
N5 N3 C1 N2 -176.7(5) . . . . ?
C2 N3 C1 N4 -179.8(5) . . . . ?
N5 N3 C1 N4 3.4(8) . . . . ?
N2 N1 C2 N6 177.3(5) . . . . ?
Cu1 N1 C2 N6 -7.3(8) . . . . ?
N2 N1 C2 N3 -0.1(5) . . . . ?
Cu1 N1 C2 N3 175.3(3) . . . . ?
C1 N3 C2 N1 0.0(6) . . . . ?
N5 N3 C2 N1 176.5(6) . . . . ?
C1 N3 C2 N6 -177.6(5) . . . . ?
N5 N3 C2 N6 -1.1(9) . . . . ?
N7 N8 C3 N10 179.8(6) . . . . ?
Cu2 N8 C3 N10 -8.7(9) . . . . ?
N7 N8 C3 N9 0.5(6) . . . . ?
Cu2 N8 C3 N9 172.0(3) . . . . ?
C4 N9 C3 N8 -1.5(6) . . . . ?
N11 N9 C3 N8 -175.7(4) . . . . ?
C4 N9 C3 N10 179.1(5) . . . . ?
N11 N9 C3 N10 4.9(8) . . . . ?
N8 N7 C4 N12 172.7(5) . . . . ?
Cu1 N7 C4 N12 -12.5(8) . . . . ?
N8 N7 C4 N9 -1.7(5) . . . . ?
Cu1 N7 C4 N9 173.1(3) . . . . ?
C3 N9 C4 N7 2.0(5) . . . . ?
N11 N9 C4 N7 175.8(4) . . . . ?
C3 N9 C4 N12 -172.8(5) . . . . ?
N11 N9 C4 N12 1.0(8) . . . . ?
Cu2 N16 N17A N18A 115(8) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H6A N16 0.81 2.62 3.313(6) 145.5 1_545




_refine_diff_density_max         0.744
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.123

_shelxl_version_number           ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nx231
_database_code_depnum_ccdc_archive 'CCDC 2081733'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             2018-06-19
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1-(2-azidoethyl)tetrazolyl copper(II) diazide
;
_chemical_name_common            
' 1-(2-azidoethyl)tetrazolyl copper(II) diazide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H5 Cu N13'
_chemical_formula_sum            'C3 H5 Cu N13'
_chemical_formula_weight         286.74

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   10.6755(7)
_cell_length_b                   6.3077(5)
_cell_length_c                   28.327(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.465(7)
_cell_angle_gamma                90
_cell_volume                     1901.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    143
_cell_measurement_reflns_used    1898
_cell_measurement_theta_min      4.5800
_cell_measurement_theta_max      31.4210

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.302
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            10094
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         4.076
_diffrn_reflns_theta_max         32.437
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3170
_reflns_number_gt                2284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0277P)²+0.2787P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3170
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0313243000
_diffrn_orient_matrix_UB_12      0.0949202000
_diffrn_orient_matrix_UB_13      0.0073842000
_diffrn_orient_matrix_UB_21      0.0016189000
_diffrn_orient_matrix_UB_22      -0.0342714000
_diffrn_orient_matrix_UB_23      0.0238744000
_diffrn_orient_matrix_UB_31      0.0588656000
_diffrn_orient_matrix_UB_32      -0.0495364000
_diffrn_orient_matrix_UB_33      -0.0023670000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00 -58.00   1.00   18.00    --  -28.70-179.00   0.00   49
  2  ω   -111.00 -56.00   1.00   18.00    --  -28.70 179.00  90.00   55
  3  ω    -98.00   2.00   1.00   18.00    --  -28.70 -77.00-120.00  100
  4  ω    -16.00  44.00   1.00   18.00    --   29.79 -57.00   0.00   60
  5  ω     20.00  89.00   1.00   18.00    --   29.79-123.00  32.00   69
  6  ω    -28.00 105.00   1.00   18.00    --   29.79   0.00-150.00  133
;



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'
Cu Cu 0.3201 1.2651 '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_
_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
Cu1 Cu 0.61229(3) 0.28989(5) 0.22899(2) 0.01185(9) Uani 1 1 d . . . . .
N1 N 0.39241(19) 0.3379(4) 0.10480(7) 0.0161(5) Uani 1 1 d . . . . .
N2 N 0.4966(2) 0.2500(4) 0.08862(8) 0.0192(5) Uani 1 1 d . . . . .
N3 N 0.5749(2) 0.2204(4) 0.12501(8) 0.0194(5) Uani 1 1 d . . . . .
N4 N 0.52324(18) 0.2871(3) 0.16481(7) 0.0123(4) Uani 1 1 d . . . . .
N5 N 0.0858(2) 0.3212(4) 0.03471(9) 0.0274(6) Uani 1 1 d . . . . .
N6 N -0.0138(2) 0.2211(4) 0.02924(8) 0.0223(5) Uani 1 1 d . . . . .
N7 N -0.1083(2) 0.1462(5) 0.02033(9) 0.0317(6) Uani 1 1 d . . . . .
N8 N 0.71917(18) 0.3066(3) 0.28987(7) 0.0142(4) Uani 1 1 d . . . . .
N9 N 0.67526(18) 0.3362(3) 0.32757(7) 0.0137(4) Uani 1 1 d . . . . .
N10 N 0.6314(2) 0.3634(4) 0.36257(8) 0.0243(5) Uani 1 1 d . . . . .
N11 N 0.46262(18) 0.4208(3) 0.25585(7) 0.0132(4) Uani 1 1 d . . . . .
N12 N 0.40196(18) 0.3028(3) 0.27850(7) 0.0137(4) Uani 1 1 d . . . . .
C1 C 0.4100(2) 0.3576(4) 0.15132(9) 0.0148(5) Uani 1 1 d . . . . .
H1 H 0.3522 0.4119 0.1711 0.018 Uiso 1 1 calc R U . . .
C2 C 0.2853(2) 0.3992(5) 0.07223(9) 0.0195(6) Uani 1 1 d . . . . .
H2A H 0.3132 0.4154 0.0406 0.023 Uiso 1 1 calc R U . . .
H2B H 0.2535 0.5352 0.0819 0.023 Uiso 1 1 calc R U . . .
C3 C 0.1807(2) 0.2378(4) 0.07094(10) 0.0211(6) Uani 1 1 d . . . . .
H3A H 0.2104 0.0993 0.0620 0.025 Uiso 1 1 calc R U . . .
H3B H 0.1462 0.2269 0.1015 0.025 Uiso 1 1 calc R U . . .
N13 N 0.3422(2) 0.1938(4) 0.30045(9) 0.0238(5) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 1.985(2) . ?
Cu1 N8 1.995(2) . ?
Cu1 N11 2.001(2) . ?
Cu1 N8 2.011(2) 7_655 ?
N1 C1 1.322(3) . ?
N1 N2 1.354(3) . ?
N1 C2 1.464(3) . ?
N2 N3 1.290(3) . ?
N3 N4 1.360(3) . ?
N4 C1 1.317(3) . ?
N5 N6 1.237(3) . ?
N5 C3 1.481(3) . ?
N6 N7 1.124(3) . ?
N8 N9 1.214(3) . ?
N8 Cu1 2.011(2) 7_655 ?
N9 N10 1.142(3) . ?
N11 N12 1.204(3) . ?
N12 N13 1.152(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.510(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
_geom_angle_publ_flag
N4 Cu1 N8 173.23(8) . . ?
N4 Cu1 N11 90.70(8) . . ?
N8 Cu1 N11 93.97(8) . . ?
N4 Cu1 N8 97.39(8) . 7_655 ?
N8 Cu1 N8 77.43(9) . 7_655 ?
N11 Cu1 N8 169.61(8) . 7_655 ?
C1 N1 N2 108.6(2) . . ?
C1 N1 C2 130.2(2) . . ?
N2 N1 C2 121.1(2) . . ?
N3 N2 N1 106.7(2) . . ?
N2 N3 N4 109.8(2) . . ?
C1 N4 N3 106.7(2) . . ?
C1 N4 Cu1 128.78(17) . . ?
N3 N4 Cu1 124.45(15) . . ?
N6 N5 C3 116.1(2) . . ?
N7 N6 N5 172.1(3) . . ?
N9 N8 Cu1 122.32(16) . . ?
N9 N8 Cu1 134.05(17) . 7_655 ?
Cu1 N8 Cu1 102.57(9) . 7_655 ?
N10 N9 N8 178.5(3) . . ?
N12 N11 Cu1 115.22(16) . . ?
N13 N12 N11 178.4(2) . . ?
N4 C1 N1 108.2(2) . . ?
N4 C1 H1 125.9 . . ?
N1 C1 H1 125.9 . . ?
N1 C2 C3 112.2(2) . . ?
N1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N5 C3 C2 104.0(2) . . ?
N5 C3 H3A 111.0 . . ?
C2 C3 H3A 111.0 . . ?
N5 C3 H3B 111.0 . . ?
C2 C3 H3B 111.0 . . ?
H3A C3 H3B 109.0 . . ?

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
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.6(3) . . . . ?
C2 N1 N2 N3 177.9(2) . . . . ?
N1 N2 N3 N4 0.2(3) . . . . ?
N2 N3 N4 C1 0.3(3) . . . . ?
N2 N3 N4 Cu1 -176.04(17) . . . . ?
N3 N4 C1 N1 -0.7(3) . . . . ?
Cu1 N4 C1 N1 175.44(17) . . . . ?
N2 N1 C1 N4 0.8(3) . . . . ?
C2 N1 C1 N4 -177.5(2) . . . . ?
C1 N1 C2 C3 -81.1(4) . . . . ?
N2 N1 C2 C3 100.7(3) . . . . ?
N6 N5 C3 C2 -175.7(3) . . . . ?
N1 C2 C3 N5 -177.0(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         1.246
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.128

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mx220
_database_code_depnum_ccdc_archive 'CCDC 2081730'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed May 17 20:31:27 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(4-aminotriazolyl)copper(II) azide
;
_chemical_name_common            'bis(4-aminotriazolyl)copper(II) azide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Cu N14'
_chemical_formula_sum            'C4 H8 Cu N14'
_chemical_formula_weight         315.78

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.3987(4)
_cell_length_b                   6.9250(6)
_cell_length_c                   7.9095(5)
_cell_angle_alpha                114.207(7)
_cell_angle_beta                 92.421(5)
_cell_angle_gamma                93.172(7)
_cell_volume                     268.60(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    1219
_cell_measurement_theta_min      4.8960
_cell_measurement_theta_max      32.0050

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.050
_shelx_estimated_absorpt_T_min   0.502
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75303
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_F_000             159
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            1934
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.568
_diffrn_reflns_theta_max         25.981
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1057
_reflns_number_gt                1007
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+0.0835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1057
_refine_ls_number_parameters     96
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0789708000
_diffrn_orient_matrix_UB_12      -0.0844342000
_diffrn_orient_matrix_UB_13      -0.0239522000
_diffrn_orient_matrix_UB_21      0.1041828000
_diffrn_orient_matrix_UB_22      0.0721966000
_diffrn_orient_matrix_UB_23      0.0109340000
_diffrn_orient_matrix_UB_31      0.0176806000
_diffrn_orient_matrix_UB_32      0.0187253000
_diffrn_orient_matrix_UB_33      0.0949920000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -109.00  -78.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega  -90.00  -60.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega  -99.00   -2.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000   60.0000 97

#__ type_ start__ end____ width___ exp.time_
  4 omega  -96.00   34.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000   60.0000 130

#__ type_ start__ end____ width___ exp.time_
  5 omega  -21.00   74.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
  6 omega   59.00  110.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -90.0000 51

;



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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu1 Cu 0.0000 0.0000 0.0000 0.01449(15) Uani 1 2 d S . P . .
N1 N 0.2412(4) 0.2088(3) -0.0356(3) 0.0172(4) Uani 1 1 d . . . . .
N2 N 0.4583(4) 0.2302(3) 0.0082(2) 0.0146(4) Uani 1 1 d . . . . .
N3 N 0.6704(4) 0.2586(3) 0.0495(3) 0.0208(5) Uani 1 1 d . . . . .
N4 N 0.0669(4) 0.1385(3) 0.2769(3) 0.0155(4) Uani 1 1 d . . . . .
N5 N 0.2969(4) 0.1982(3) 0.3766(3) 0.0209(5) Uani 1 1 d . . . . .
N6 N 0.0004(3) 0.2860(3) 0.5697(3) 0.0142(4) Uani 1 1 d . . . . .
N7 N -0.1373(4) 0.3616(4) 0.7289(3) 0.0191(5) Uani 1 1 d . . . . .
C1 C -0.1066(4) 0.1927(4) 0.3957(3) 0.0153(5) Uani 1 1 d . . . . .
H1 H -0.2806 0.1697 0.3637 0.018 Uiso 1 1 calc R U . . .
C2 C 0.2499(5) 0.2852(4) 0.5520(3) 0.0212(5) Uani 1 1 d . . . . .
H2 H 0.3730 0.3403 0.6530 0.025 Uiso 1 1 calc R U . . .
H7A H -0.100(5) 0.300(5) 0.793(4) 0.020(7) Uiso 1 1 d . . . . .
H7B H -0.105(6) 0.485(6) 0.784(4) 0.027(8) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.0046(18) . ?
Cu1 N4 2.0046(18) 2 ?
Cu1 N1 2.0052(19) . ?
Cu1 N1 2.0052(19) 2 ?
N1 N2 1.192(3) . ?
N2 N3 1.160(3) . ?
N4 C1 1.314(3) . ?
N4 N5 1.388(3) . ?
N5 C2 1.309(3) . ?
N6 C1 1.344(3) . ?
N6 C2 1.361(3) . ?
N6 N7 1.412(3) . ?
N7 H7A 0.81(3) . ?
N7 H7B 0.79(3) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?

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
_geom_angle_publ_flag
N4 Cu1 N4 180.00(5) . 2 ?
N4 Cu1 N1 92.29(8) . . ?
N4 Cu1 N1 87.71(8) 2 . ?
N4 Cu1 N1 87.71(8) . 2 ?
N4 Cu1 N1 92.29(8) 2 2 ?
N1 Cu1 N1 180.0 . 2 ?
N2 N1 Cu1 124.28(16) . . ?
N3 N2 N1 177.2(2) . . ?
C1 N4 N5 108.18(18) . . ?
C1 N4 Cu1 124.40(16) . . ?
N5 N4 Cu1 127.40(15) . . ?
C2 N5 N4 105.9(2) . . ?
C1 N6 C2 105.82(19) . . ?
C1 N6 N7 123.06(19) . . ?
C2 N6 N7 131.12(19) . . ?
N6 N7 H7A 108(2) . . ?
N6 N7 H7B 109(2) . . ?
H7A N7 H7B 110(3) . . ?
N4 C1 N6 109.4(2) . . ?
N4 C1 H1 125.3 . . ?
N6 C1 H1 125.3 . . ?
N5 C2 N6 110.6(2) . . ?
N5 C2 H2 124.7 . . ?
N6 C2 H2 124.7 . . ?

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
_geom_torsion_publ_flag
C1 N4 N5 C2 0.3(3) . . . . ?
Cu1 N4 N5 C2 178.87(17) . . . . ?
N5 N4 C1 N6 0.1(3) . . . . ?
Cu1 N4 C1 N6 -178.58(14) . . . . ?
C2 N6 C1 N4 -0.4(3) . . . . ?
N7 N6 C1 N4 -179.8(2) . . . . ?
N4 N5 C2 N6 -0.5(3) . . . . ?
C1 N6 C2 N5 0.6(3) . . . . ?
N7 N6 C2 N5 179.9(2) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7A N1 0.81(3) 2.50(3) 3.210(3) 147(3) 1_556
N7 H7A N3 0.81(3) 2.53(3) 3.105(3) 129(3) 1_456
N7 H7B N1 0.79(3) 2.42(3) 3.071(3) 141(3) 2_566

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.531
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.080

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_vv678
_database_code_depnum_ccdc_archive 'CCDC 2081736'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
4,4-bi(triazolyl) diazido copper(II)
;
_chemical_name_common            '4,4-bi(triazolyl) diazido copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H4 Cu N12'
_chemical_formula_sum            'C4 H4 Cu N12'
_chemical_formula_weight         283.73

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.4279(5)
_cell_length_b                   6.3343(2)
_cell_length_c                   10.7437(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.6450(10)
_cell_angle_gamma                90
_cell_volume                     912.85(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9218
_cell_measurement_theta_min      3.0373
_cell_measurement_theta_max      27.3986

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.394
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            15502
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.037
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1797
_reflns_number_gt                1632
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0198P)²+0.9875P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1797
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0510
_refine_ls_wR_factor_gt          0.0493
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu1 Cu 0.04312(2) 0.46031(4) 0.13579(2) 0.01149(8) Uani 1 1 d . . . . .
N1 N 0.17724(12) 0.4685(3) 0.22164(15) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.26148(12) 0.5554(3) 0.17094(16) 0.0175(4) Uani 1 1 d . . . . .
N3 N 0.29937(12) 0.4293(3) 0.35547(15) 0.0128(3) Uani 1 1 d . . . . .
N4 N 0.35478(12) 0.3746(3) 0.46213(15) 0.0143(3) Uani 1 1 d . . . . .
N5 N 0.42675(14) 0.3920(3) 0.64701(16) 0.0230(4) Uani 1 1 d . . . . .
N6 N 0.46925(13) 0.2251(3) 0.58100(16) 0.0214(4) Uani 1 1 d . . . . .
N7 N -0.01490(12) 0.3297(3) 0.28585(14) 0.0134(3) Uani 1 1 d . . . . .
N8 N -0.06240(12) 0.4460(3) 0.34894(15) 0.0148(4) Uani 1 1 d . . . . .
N10 N -0.08453(12) 0.4478(3) 0.03309(15) 0.0145(3) Uani 1 1 d . . . . .
N11 N -0.16574(13) 0.4202(3) 0.07602(15) 0.0150(4) Uani 1 1 d . . . . .
N12 N -0.24156(13) 0.3987(3) 0.11858(17) 0.0259(4) Uani 1 1 d . . . . .
C1 C 0.33367(15) 0.5302(3) 0.25410(18) 0.0176(4) Uani 1 1 d . . . . .
H1 H 0.4005 0.5754 0.2455 0.021 Uiso 1 1 calc R U . . .
C2 C 0.20109(14) 0.3935(3) 0.33169(17) 0.0130(4) Uani 1 1 d . . . . .
H2 H 0.1572 0.3256 0.3858 0.016 Uiso 1 1 calc R U . . .
C3 C 0.35930(16) 0.4792(3) 0.57300(19) 0.0197(4) Uani 1 1 d . . . . .
H3 H 0.3195 0.5973 0.5931 0.024 Uiso 1 1 calc R U . . .
C4 C 0.42449(15) 0.2184(3) 0.47137(19) 0.0179(4) Uani 1 1 d . . . . .
H4 H 0.4382 0.1200 0.4076 0.021 Uiso 1 1 calc R U . . .
N9 N -0.10812(15) 0.5533(3) 0.41157(18) 0.0270(4) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.9858(16) . ?
Cu1 N10 1.9968(16) . ?
Cu1 N7 2.0016(16) . ?
Cu1 N10 2.0082(16) 3_565 ?
N1 C2 1.300(2) . ?
N1 N2 1.391(2) . ?
N2 C1 1.298(3) . ?
N3 C2 1.352(2) . ?
N3 C1 1.361(3) . ?
N3 N4 1.381(2) . ?
N4 C3 1.362(3) . ?
N4 C4 1.363(3) . ?
N5 C3 1.301(3) . ?
N5 N6 1.408(3) . ?
N6 C4 1.298(3) . ?
N7 N8 1.204(2) . ?
N8 N9 1.153(2) . ?
N10 N11 1.216(2) . ?
N10 Cu1 2.0082(16) 3_565 ?
N11 N12 1.143(2) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?

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
_geom_angle_publ_flag
N1 Cu1 N10 174.07(6) . . ?
N1 Cu1 N7 90.87(7) . . ?
N10 Cu1 N7 94.16(6) . . ?
N1 Cu1 N10 97.42(6) . 3_565 ?
N10 Cu1 N10 77.21(7) . 3_565 ?
N7 Cu1 N10 169.04(7) . 3_565 ?
C2 N1 N2 109.26(16) . . ?
C2 N1 Cu1 126.35(14) . . ?
N2 N1 Cu1 124.39(12) . . ?
C1 N2 N1 106.07(16) . . ?
C2 N3 C1 106.91(16) . . ?
C2 N3 N4 126.76(16) . . ?
C1 N3 N4 126.32(16) . . ?
C3 N4 C4 106.68(17) . . ?
C3 N4 N3 127.13(17) . . ?
C4 N4 N3 125.79(16) . . ?
C3 N5 N6 107.34(17) . . ?
C4 N6 N5 107.48(16) . . ?
N8 N7 Cu1 115.90(13) . . ?
N9 N8 N7 178.2(2) . . ?
N11 N10 Cu1 123.92(13) . . ?
N11 N10 Cu1 132.44(13) . 3_565 ?
Cu1 N10 Cu1 102.79(7) . 3_565 ?
N12 N11 N10 178.1(2) . . ?
N2 C1 N3 109.82(17) . . ?
N2 C1 H1 125.1 . . ?
N3 C1 H1 125.1 . . ?
N1 C2 N3 107.93(17) . . ?
N1 C2 H2 126.0 . . ?
N3 C2 H2 126.0 . . ?
N5 C3 N4 109.23(19) . . ?
N5 C3 H3 125.4 . . ?
N4 C3 H3 125.4 . . ?
N6 C4 N4 109.26(18) . . ?
N6 C4 H4 125.4 . . ?
N4 C4 H4 125.4 . . ?

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
_geom_torsion_publ_flag
C2 N1 N2 C1 -0.4(2) . . . . ?
Cu1 N1 N2 C1 -179.80(14) . . . . ?
C2 N3 N4 C3 -80.0(3) . . . . ?
C1 N3 N4 C3 99.9(3) . . . . ?
C2 N3 N4 C4 108.2(2) . . . . ?
C1 N3 N4 C4 -71.8(3) . . . . ?
C3 N5 N6 C4 -0.8(2) . . . . ?
N1 N2 C1 N3 0.5(2) . . . . ?
C2 N3 C1 N2 -0.4(2) . . . . ?
N4 N3 C1 N2 179.67(17) . . . . ?
N2 N1 C2 N3 0.2(2) . . . . ?
Cu1 N1 C2 N3 179.56(12) . . . . ?
C1 N3 C2 N1 0.1(2) . . . . ?
N4 N3 C2 N1 -179.97(17) . . . . ?
N6 N5 C3 N4 0.9(2) . . . . ?
C4 N4 C3 N5 -0.7(2) . . . . ?
N3 N4 C3 N5 -173.72(18) . . . . ?
N5 N6 C4 N4 0.4(2) . . . . ?
C3 N4 C4 N6 0.2(2) . . . . ?
N3 N4 C4 N6 173.29(18) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N5 0.95 2.55 3.377(3) 145.4 3_666
C2 H2 N11 0.95 2.60 3.200(3) 121.3 2_545
C2 H2 N9 0.95 2.43 3.098(3) 127.4 3_566
C3 H3 N2 0.95 2.49 3.413(3) 163.6 4_576
C4 H4 N6 0.95 2.52 3.212(3) 130.3 3_656
C1 H1 N5 0.95 2.55 3.377(3) 145.4 3_666
C2 H2 N11 0.95 2.60 3.200(3) 121.3 2_545
C2 H2 N9 0.95 2.43 3.098(3) 127.4 3_566
C3 H3 N2 0.95 2.49 3.413(3) 163.6 4_576
C4 H4 N6 0.95 2.52 3.212(3) 130.3 3_656

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.266
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_vv369
_database_code_depnum_ccdc_archive 'CCDC 2081740'
loop_
_audit_author_name
_audit_author_address
'Joerg Stierstorfer'
;University of Munich (LMU)
Germany
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;

_vrf_PLAT213_vv369               
; 
PROBLEM: Atom N7      has ADP max/min Ratio .....        5.7 prolat

RESPONSE: mono-coordinating azides are strongly vibrating at the
 non-coordinating end and show therefore a large thermal ellipsoid

;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1-amino-1,2,3-triazole copper(II) azide
;
_chemical_name_common            ' 1-amino-1,2,3-triazole copper(II) azide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C2 H4 Cu N10'
_chemical_formula_sum            'C2 H4 Cu N10'
_chemical_formula_weight         231.69

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   3.42640(10)
_cell_length_b                   14.7560(5)
_cell_length_c                   14.5974(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.0290(10)
_cell_angle_gamma                90
_cell_volume                     735.20(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7354
_cell_measurement_theta_min      2.7607
_cell_measurement_theta_max      26.3408

_exptl_crystal_description       rod
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.939
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            1517
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.761
_diffrn_reflns_theta_max         26.342
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1517
_reflns_number_gt                1456
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+1.1957P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1517
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0938
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_restrained_S_all      1.274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
Cu1 Cu 0.22733(14) 0.06235(3) 0.57116(3) 0.00984(17) Uani 1 1 d . . . . .
N9 N 0.7764(11) 0.1263(2) 0.4047(2) 0.0117(7) Uani 1 1 d . . . . .
N5 N 0.6642(10) 0.0375(2) 0.6718(2) 0.0128(7) Uani 1 1 d . . . . .
N3 N 0.2159(10) 0.1944(2) 0.5955(2) 0.0110(7) Uani 1 1 d . . . . .
C1 C 0.1166(15) 0.3308(3) 0.6472(3) 0.0221(10) Uani 1 1 d . . . . .
H1 H 0.0586 0.3809 0.6846 0.026 Uiso 1 1 calc R U . . .
N8 N 0.7507(12) 0.1773(3) 0.3474(3) 0.0213(9) Uani 1 1 d . . . . .
N1 N 0.2121(13) 0.3319(2) 0.5597(2) 0.0190(8) Uani 1 1 d . . . . .
N2 N 0.2732(11) 0.2503(3) 0.5267(2) 0.0157(8) Uani 1 1 d . . . . .
C2 C 0.1225(14) 0.2418(3) 0.6697(3) 0.0142(9) Uani 1 1 d . . . . .
H2 H 0.0702 0.2171 0.7274 0.017 Uiso 1 1 calc R U . . .
N10 N 0.7963(11) 0.0692(2) 0.4667(2) 0.0112(7) Uani 1 1 d . . . . .
N6 N 0.6097(13) 0.0478(3) 0.7450(3) 0.0296(10) Uani 1 1 d . . . . .
N7 N 0.564(2) 0.0563(6) 0.8230(3) 0.082(3) Uani 1 1 d . . . . .
N4 N 0.251(2) 0.4081(3) 0.5042(3) 0.0526(18) Uani 1 1 d . . . . .
H4A H 0.3167 0.4015 0.4476 0.063 Uiso 1 1 calc R U . . .
H4B H 0.2111 0.4626 0.5259 0.063 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 1.981(4) . ?
Cu1 N10 2.018(3) 3_656 ?
Cu1 N10 2.031(4) 1_455 ?
Cu1 N5 2.037(4) . ?
N9 N8 1.123(5) . ?
N9 N10 1.234(5) . ?
N5 N6 1.111(6) . ?
N3 N2 1.328(5) . ?
N3 C2 1.352(5) . ?
C1 N1 1.346(6) . ?
C1 C2 1.353(7) . ?
C1 H1 0.9500 . ?
N1 N2 1.320(5) . ?
N1 N4 1.399(5) . ?
C2 H2 0.9500 . ?
N10 Cu1 2.018(3) 3_656 ?
N10 Cu1 2.031(3) 1_655 ?
N6 N7 1.169(7) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?

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
_geom_angle_publ_flag
N3 Cu1 N10 173.73(14) . 3_656 ?
N3 Cu1 N10 93.51(14) . 1_455 ?
N10 Cu1 N10 80.40(15) 3_656 1_455 ?
N3 Cu1 N5 94.15(14) . . ?
N10 Cu1 N5 91.93(14) 3_656 . ?
N10 Cu1 N5 172.33(14) 1_455 . ?
N8 N9 N10 178.4(5) . . ?
N6 N5 Cu1 119.6(3) . . ?
N2 N3 C2 110.2(3) . . ?
N2 N3 Cu1 118.0(3) . . ?
C2 N3 Cu1 131.5(3) . . ?
N1 C1 C2 104.0(4) . . ?
N1 C1 H1 128.0 . . ?
C2 C1 H1 128.0 . . ?
N2 N1 C1 113.3(4) . . ?
N2 N1 N4 119.6(4) . . ?
C1 N1 N4 127.0(4) . . ?
N1 N2 N3 104.6(3) . . ?
N3 C2 C1 107.9(4) . . ?
N3 C2 H2 126.0 . . ?
C1 C2 H2 126.0 . . ?
N9 N10 Cu1 117.3(3) . 3_656 ?
N9 N10 Cu1 125.1(3) . 1_655 ?
Cu1 N10 Cu1 99.60(15) 3_656 1_655 ?
N5 N6 N7 177.4(6) . . ?
N1 N4 H4A 120.0 . . ?
N1 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?

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
_geom_torsion_publ_flag
C2 C1 N1 N2 0.5(6) . . . . ?
C2 C1 N1 N4 -179.2(6) . . . . ?
C1 N1 N2 N3 -0.1(5) . . . . ?
N4 N1 N2 N3 179.6(5) . . . . ?
C2 N3 N2 N1 -0.3(5) . . . . ?
Cu1 N3 N2 N1 174.1(3) . . . . ?
N2 N3 C2 C1 0.5(5) . . . . ?
Cu1 N3 C2 C1 -172.8(3) . . . . ?
N1 C1 C2 N3 -0.6(5) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.462
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.117

_shelxl_version_number           2013-4


