# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_lx316
_database_code_depnum_ccdc_archive 'CCDC 1816626'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Jun 23 14:26:03 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,1-ditetrazolylpropane) copper(II) diperchlorate
;
_chemical_name_common            
'tris(1,1-ditetrazolylpropane) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C5 H8 Cu0.33 N8), 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 Cu N24 O8'
_chemical_formula_weight         803.02

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'



_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'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'

_cell_length_a                   11.061(5)
_cell_length_b                   11.061(5)
_cell_length_c                   14.622(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_volume                     1549.3(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2898
_cell_measurement_theta_min      4.2400
_cell_measurement_theta_max      26.4060

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.177
_exptl_absorpt_coefficient_mu    0.962
_shelx_estimated_absorpt_T_min   0.775
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91350
_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    1.721
_exptl_crystal_F_000             818
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_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            11267
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.621
_diffrn_reflns_theta_max         26.240
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             1037
_reflns_number_gt                828
_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)+(0.0435P)²+0.9818P] 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         1037
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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      0.0140009000
_diffrn_orient_matrix_UB_12      -0.0367170000
_diffrn_orient_matrix_UB_13      -0.0342729000
_diffrn_orient_matrix_UB_21      0.0502542000
_diffrn_orient_matrix_UB_22      0.0642691000
_diffrn_orient_matrix_UB_23      -0.0198404000
_diffrn_orient_matrix_UB_31      0.0525750000
_diffrn_orient_matrix_UB_32      0.0003687000
_diffrn_orient_matrix_UB_33      0.0279699000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -30.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000    0.0000 124

#__ type_ start__ end____ width___ exp.time_
  2 omega    4.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 99

#__ type_ start__ end____ width___ exp.time_
  4 omega    2.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000 -120.0000 83

#__ type_ start__ end____ width___ exp.time_
  5 omega -110.00  -41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -150.0000 69

;



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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 0.0000 0.0000 0.5000 0.0240(2) Uani 1 6 d S T P . .
N4 N 0.0615(2) 0.3573(2) 0.64676(14) 0.0417(5) Uani 1 1 d . . . . .
N1 N 0.0486(2) 0.1768(2) 0.58313(13) 0.0364(5) Uani 1 1 d . . . . .
N2 N 0.1671(2) 0.2424(3) 0.63452(16) 0.0490(6) Uani 1 1 d . . . . .
C1 C -0.0132(3) 0.2509(3) 0.59208(17) 0.0404(6) Uani 1 1 d . . . . .
H1 H -0.0984 0.2311 0.5636 0.048 Uiso 1 1 calc R U . . .
N3 N 0.1752(2) 0.3514(3) 0.67267(16) 0.0523(6) Uani 1 1 d . . . . .
C3 C -0.0616(6) 0.4560(6) 0.7304(3) 0.0451(12) Uani 0.5 1 d . . P . .
H3A H -0.1481 0.3734 0.7083 0.054 Uiso 0.5 1 calc R U P . .
H3B H -0.0764 0.5369 0.7258 0.054 Uiso 0.5 1 calc R U P . .
Cl1A Cl 0.3333 0.6667 0.4587(3) 0.0333(8) Uani 0.694(11) 3 d S T P A 1
O2A O 0.3333 0.6667 0.3628(4) 0.134(4) Uani 0.694(11) 3 d S T P A 1
O1A O 0.2616(12) 0.5352(12) 0.5056(9) 0.061(3) Uani 0.306(11) 1 d . . P A 1
Cl1B Cl 0.3333 0.6667 0.4875(8) 0.039(2) Uani 0.306(11) 3 d S T P A 2
O1B O 0.2271(6) 0.5290(6) 0.4664(4) 0.0650(14) Uani 0.694(11) 1 d . . P A 2
O2B O 0.3333 0.6667 0.5848(7) 0.049(4) Uani 0.306(11) 3 d S T P A 2
C2 C 0.0463(4) 0.4793(3) 0.6686(2) 0.0548(8) Uani 1 1 d . . . . .
H2A H 0.1342 0.5524 0.6931 0.066 Uiso 0.5 1 d R U P B 1
H2B H 0.0295 0.5138 0.6118 0.066 Uiso 0.5 1 d R U P B 1
H2C H 0.102(8) 0.550(7) 0.629(5) 0.066 Uiso 0.5 1 d . U P C 2
H2D H -0.046(8) 0.461(6) 0.647(5) 0.066 Uiso 0.5 1 d . U P D 2


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 2.131(2) . ?
Cu1 N1 2.131(2) 7_556 ?
Cu1 N1 2.131(2) 9_556 ?
Cu1 N1 2.131(2) 3 ?
Cu1 N1 2.131(2) 2 ?
N4 C1 1.317(3) . ?
N4 N3 1.346(3) . ?
N4 C2 1.475(4) . ?
N1 C1 1.310(3) . ?
N1 N2 1.363(3) . ?
N2 N3 1.291(3) . ?
C1 H1 0.9500 . ?
C3 C2 1.414(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H2D 1.23(7) . ?
Cl1A O2A 1.402(8) . ?
Cl1A O1A 1.436(11) . ?
Cl1B O1B 1.416(5) . ?
Cl1B O2B 1.422(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.92(7) . ?
C2 H2D 0.99(7) . ?

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 . 7_556 ?
N1 Cu1 N1 89.32(7) . 9_556 ?
N1 Cu1 N1 90.68(7) 7_556 9_556 ?
N1 Cu1 N1 90.68(7) . 3 ?
N1 Cu1 N1 89.32(7) 7_556 3 ?
N1 Cu1 N1 180.00(8) 9_556 3 ?
N1 Cu1 N1 90.69(7) . 2 ?
N1 Cu1 N1 89.32(7) 7_556 2 ?
N1 Cu1 N1 89.32(7) 9_556 2 ?
N1 Cu1 N1 90.68(7) 3 2 ?
N1 Cu1 N1 89.31(7) . 8_556 ?
N1 Cu1 N1 90.68(7) 7_556 8_556 ?
N1 Cu1 N1 90.68(7) 9_556 8_556 ?
N1 Cu1 N1 89.32(7) 3 8_556 ?
N1 Cu1 N1 180.00(10) 2 8_556 ?
C1 N4 N3 108.1(2) . . ?
C1 N4 C2 129.9(2) . . ?
N3 N4 C2 121.3(2) . . ?
C1 N1 N2 106.0(2) . . ?
C1 N1 Cu1 131.32(17) . . ?
N2 N1 Cu1 122.46(16) . . ?
N3 N2 N1 109.5(2) . . ?
N1 C1 N4 109.2(2) . . ?
N1 C1 H1 125.4 . . ?
N4 C1 H1 125.4 . . ?
N2 N3 N4 107.1(2) . . ?
C2 C3 C2 119.7(4) . 5_556 ?
C2 C3 H3A 107.4 . . ?
C2 C3 H3A 107.4 5_556 . ?
C2 C3 H3B 107.4 . . ?
C2 C3 H3B 107.4 5_556 . ?
H3A C3 H3B 106.9 . . ?
C2 C3 H2D 161(3) 5_556 . ?
H3A C3 H2D 76.6 . . ?
H3B C3 H2D 88.5 . . ?
O2A Cl1A O1A 118.5(5) . 3_565 ?
O2A Cl1A O1A 118.5(5) . . ?
O1A Cl1A O1A 99.1(7) 3_565 . ?
O2A Cl1A O1A 118.5(5) . 2_665 ?
O1A Cl1A O1A 99.1(7) 3_565 2_665 ?
O1A Cl1A O1A 99.1(7) . 2_665 ?
O1B Cl1B O1B 115.4(3) 3_565 . ?
O1B Cl1B O1B 115.4(3) 3_565 2_665 ?
O1B Cl1B O1B 115.4(3) . 2_665 ?
O1B Cl1B O2B 102.6(4) 3_565 . ?
O1B Cl1B O2B 102.6(4) . . ?
O1B Cl1B O2B 102.6(4) 2_665 . ?
C3 C2 N4 116.3(3) . . ?
N4 C2 C3 114.6(3) . 5_556 ?
C3 C2 H2A 108.6 . . ?
N4 C2 H2A 108.5 . . ?
C3 C2 H2B 107.9 . . ?
N4 C2 H2B 107.9 . . ?
C3 C2 H2B 137.5 5_556 . ?
H2A C2 H2B 107.3 . . ?
C3 C2 H2C 135(4) . . ?
N4 C2 H2C 108(4) . . ?
C3 C2 H2C 116(4) 5_556 . ?
C3 C2 H2D 58(4) . . ?
N4 C2 H2D 109(4) . . ?
C3 C2 H2D 109(4) 5_556 . ?
H2C C2 H2D 99(6) . . ?

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(3) . . . . ?
Cu1 N1 N2 N3 175.43(17) . . . . ?
N2 N1 C1 N4 -0.4(3) . . . . ?
Cu1 N1 C1 N4 -175.22(15) . . . . ?
N3 N4 C1 N1 0.6(3) . . . . ?
C2 N4 C1 N1 171.2(2) . . . . ?
N1 N2 N3 N4 0.3(3) . . . . ?
C1 N4 N3 N2 -0.6(3) . . . . ?
C2 N4 N3 N2 -172.1(2) . . . . ?
C2 C3 C2 N4 72.4(5) 5_556 . . . ?
C2 C3 C2 C3 -29.7(5) 5_556 . . 5_556 ?
C1 N4 C2 C3 77.0(4) . . . . ?
N3 N4 C2 C3 -113.5(4) . . . . ?
C1 N4 C2 C3 136.1(4) . . . 5_556 ?
N3 N4 C2 C3 -54.4(4) . . . 5_556 ?

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 O1A 0.95 2.36 3.269(14) 161.3 9_556
C1 H1 O1B 0.95 2.27 3.187(6) 161.4 9_556
C3 H3A O2A 0.99 2.14 2.941(6) 137.2 7_566
C3 H3B N3 0.99 2.51 3.295(6) 135.8 4_566
C2 H2C Cl1B 0.92(7) 3.03(8) 3.848(8) 149(5) .
C2 H2C O2B 0.92(7) 2.31(8) 3.049(6) 137(6) .
C1 H1 O1A 0.95 2.36 3.269(14) 161.3 9_556
C1 H1 O1B 0.95 2.27 3.187(6) 161.4 9_556
C3 H3A O2A 0.99 2.14 2.941(6) 137.2 7_566
C3 H3B N3 0.99 2.51 3.295(6) 135.8 4_566
C2 H2C Cl1B 0.92(7) 3.03(8) 3.848(8) 149(5) .
C2 H2C O2B 0.92(7) 2.31(8) 3.049(6) 137(6) .

_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         0.511
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.057

_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_lx241
_database_code_depnum_ccdc_archive 'CCDC 1816630'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu May 12 14:28:56 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,2-ditetrazolylpropanyl silver(I) perchlorate'
;
_chemical_name_common            
'1,2-ditetrazolylpropanyl silver(I) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H8 Ag N8, Cl O4'
_chemical_formula_sum            'C5 H8 Ag Cl N8 O4'
_chemical_formula_weight         387.51

_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                   9.8070(2)
_cell_length_b                   10.7250(2)
_cell_length_c                   11.1830(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.128(2)
_cell_angle_gamma                90
_cell_volume                     1135.47(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4790
_cell_measurement_theta_min      4.9690
_cell_measurement_theta_max      31.9730

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.039
_shelx_estimated_absorpt_T_min   0.454
_shelx_estimated_absorpt_T_max   0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    2.267
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_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            8392
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.227
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.240
_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             2218
_reflns_number_gt                2071
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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)+(0.0172P)²+1.0918P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_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         2218
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0170
_refine_ls_wR_factor_ref         0.0413
_refine_ls_wR_factor_gt          0.0403
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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      0.0322417000
_diffrn_orient_matrix_UB_12      0.0361008000
_diffrn_orient_matrix_UB_13      0.0529763000
_diffrn_orient_matrix_UB_21      -0.0119342000
_diffrn_orient_matrix_UB_22      0.0548682000
_diffrn_orient_matrix_UB_23      -0.0366859000
_diffrn_orient_matrix_UB_31      -0.0665597000
_diffrn_orient_matrix_UB_32      0.0076350000
_diffrn_orient_matrix_UB_33      0.0129199000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -54.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000  -90.0000 96

#__ type_ start__ end____ width___ exp.time_
  2 omega    2.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega    6.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000 -150.0000 96

#__ type_ start__ end____ width___ exp.time_
  4 omega  -14.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -112.0000   98.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega  -39.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  150.0000 81

;



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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Ag1 Ag -0.35272(2) 0.91295(2) -0.04539(2) 0.01576(6) Uani 1 1 d . . . . .
N1 N -0.15128(17) 0.71528(15) 0.17862(15) 0.0123(3) Uani 1 1 d . . . . .
N2 N -0.27673(17) 0.76260(15) 0.12190(15) 0.0134(3) Uani 1 1 d . . . . .
C1 C -0.3569(2) 0.72178(18) 0.19222(19) 0.0141(4) Uani 1 1 d . . . . .
N4 N -0.28257(17) 0.65328(16) 0.28785(16) 0.0148(3) Uani 1 1 d . . . . .
N5 N 0.31525(18) 0.60352(15) 0.45549(16) 0.0145(4) Uani 1 1 d . . . . .
N6 N 0.19436(17) 0.65877(15) 0.41651(15) 0.0144(3) Uani 1 1 d . . . . .
N7 N 0.22158(17) 0.76883(15) 0.37034(15) 0.0119(3) Uani 1 1 d . . . . .
C5 C 0.3607(2) 0.77773(19) 0.38322(18) 0.0136(4) Uani 1 1 d . . . . .
N9 N 0.42171(17) 0.67528(16) 0.43611(15) 0.0135(3) Uani 1 1 d . . . . .
N10 N -0.15082(17) 0.65022(16) 0.27860(16) 0.0154(3) Uani 1 1 d . . . . .
C2 C -0.0244(2) 0.7324(2) 0.1342(2) 0.0154(4) Uani 1 1 d . . . . .
C3 C 0.0514(2) 0.8533(2) 0.18125(19) 0.0160(4) Uani 1 1 d . . . . .
C4 C 0.1084(2) 0.85934(19) 0.32119(19) 0.0141(4) Uani 1 1 d . . . . .
Cl1 Cl 0.31470(5) 0.51008(4) 0.13513(4) 0.01468(11) Uani 1 1 d . . . . .
O1 O 0.19109(17) 0.45249(17) 0.15637(19) 0.0392(5) Uani 1 1 d . . . . .
O2 O 0.3318(2) 0.47360(16) 0.01627(15) 0.0362(4) Uani 1 1 d . . . . .
O3 O 0.29890(15) 0.64406(13) 0.13774(13) 0.0187(3) Uani 1 1 d . . . . .
O4 O 0.43802(15) 0.47247(14) 0.22980(14) 0.0212(3) Uani 1 1 d . . . . .
H3B H 0.125(3) 0.864(2) 0.142(2) 0.023(6) Uiso 1 1 d . . . . .
H4A H 0.039(2) 0.844(2) 0.364(2) 0.016(6) Uiso 1 1 d . . . . .
H3A H -0.007(3) 0.920(2) 0.156(2) 0.015(6) Uiso 1 1 d . . . . .
H4B H 0.148(3) 0.935(2) 0.346(2) 0.017(6) Uiso 1 1 d . . . . .
H5 H 0.410(3) 0.845(2) 0.361(2) 0.023(6) Uiso 1 1 d . . . . .
H2B H -0.056(3) 0.735(2) 0.052(3) 0.026(7) Uiso 1 1 d . . . . .
H2A H 0.034(2) 0.663(2) 0.162(2) 0.011(5) Uiso 1 1 d . . . . .
H1 H -0.451(3) 0.737(2) 0.175(2) 0.013(5) 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
Ag1 N5 2.2650(17) 2 ?
Ag1 N2 2.4347(16) . ?
N1 N10 1.317(2) . ?
N1 N2 1.329(2) . ?
N1 C2 1.466(2) . ?
N2 C1 1.323(3) . ?
C1 N4 1.345(3) . ?
C1 H1 0.91(2) . ?
N4 N10 1.323(2) . ?
N5 N6 1.295(2) . ?
N5 N9 1.359(2) . ?
N6 N7 1.343(2) . ?
N7 C5 1.338(3) . ?
N7 C4 1.469(2) . ?
C5 N9 1.315(3) . ?
C5 H5 0.94(3) . ?
C2 C3 1.518(3) . ?
C2 H2B 0.90(3) . ?
C2 H2A 0.94(2) . ?
C3 C4 1.520(3) . ?
C3 H3B 0.94(3) . ?
C3 H3A 0.92(2) . ?
C4 H4A 0.95(2) . ?
C4 H4B 0.92(2) . ?
Cl1 O1 1.4345(16) . ?
Cl1 O2 1.4370(17) . ?
Cl1 O4 1.4415(15) . ?
Cl1 O3 1.4464(15) . ?

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 Ag1 N5 126.85(6) 4_575 2 ?
N4 Ag1 N9 106.31(6) 4_575 4_475 ?
N5 Ag1 N9 116.08(6) 2 4_475 ?
N4 Ag1 N2 109.10(6) 4_575 . ?
N5 Ag1 N2 105.96(6) 2 . ?
N9 Ag1 N2 83.91(5) 4_475 . ?
N10 N1 N2 113.90(15) . . ?
N10 N1 C2 122.58(16) . . ?
N2 N1 C2 123.52(16) . . ?
C1 N2 N1 102.11(16) . . ?
C1 N2 Ag1 124.44(13) . . ?
N1 N2 Ag1 132.78(12) . . ?
N2 C1 N4 111.74(17) . . ?
N2 C1 H1 123.1(14) . . ?
N4 C1 H1 125.1(14) . . ?
N10 N4 C1 106.81(16) . . ?
N10 N4 Ag1 124.71(13) . 4_576 ?
C1 N4 Ag1 127.47(13) . 4_576 ?
N6 N5 N9 111.16(15) . . ?
N6 N5 Ag1 126.20(13) . 2_545 ?
N9 N5 Ag1 122.64(12) . 2_545 ?
N5 N6 N7 105.98(15) . . ?
C5 N7 N6 108.71(16) . . ?
C5 N7 C4 130.03(17) . . ?
N6 N7 C4 121.21(16) . . ?
N9 C5 N7 108.68(18) . . ?
N9 C5 H5 124.0(15) . . ?
N7 C5 H5 127.3(15) . . ?
C5 N9 N5 105.46(16) . . ?
C5 N9 Ag1 132.75(14) . 4_676 ?
N5 N9 Ag1 119.96(12) . 4_676 ?
N1 N10 N4 105.43(15) . . ?
N1 C2 C3 111.82(17) . . ?
N1 C2 H2B 104.9(17) . . ?
C3 C2 H2B 109.7(17) . . ?
N1 C2 H2A 106.6(13) . . ?
C3 C2 H2A 111.2(13) . . ?
H2B C2 H2A 112(2) . . ?
C2 C3 C4 114.11(17) . . ?
C2 C3 H3B 108.2(16) . . ?
C4 C3 H3B 110.6(15) . . ?
C2 C3 H3A 110.7(15) . . ?
C4 C3 H3A 108.3(15) . . ?
H3B C3 H3A 105(2) . . ?
N7 C4 C3 113.34(17) . . ?
N7 C4 H4A 105.7(14) . . ?
C3 C4 H4A 113.1(14) . . ?
N7 C4 H4B 104.6(15) . . ?
C3 C4 H4B 111.5(15) . . ?
H4A C4 H4B 108(2) . . ?
O1 Cl1 O2 110.11(12) . . ?
O1 Cl1 O4 109.95(10) . . ?
O2 Cl1 O4 108.96(10) . . ?
O1 Cl1 O3 108.95(10) . . ?
O2 Cl1 O3 109.15(9) . . ?
O4 Cl1 O3 109.69(9) . . ?

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
N10 N1 N2 C1 -0.7(2) . . . . ?
C2 N1 N2 C1 178.83(18) . . . . ?
N10 N1 N2 Ag1 169.91(13) . . . . ?
C2 N1 N2 Ag1 -10.6(3) . . . . ?
N1 N2 C1 N4 0.4(2) . . . . ?
Ag1 N2 C1 N4 -171.28(12) . . . . ?
N2 C1 N4 N10 0.1(2) . . . . ?
N2 C1 N4 Ag1 168.90(13) . . . 4_576 ?
N9 N5 N6 N7 0.1(2) . . . . ?
Ag1 N5 N6 N7 179.99(12) 2_545 . . . ?
N5 N6 N7 C5 -0.2(2) . . . . ?
N5 N6 N7 C4 -177.83(16) . . . . ?
N6 N7 C5 N9 0.3(2) . . . . ?
C4 N7 C5 N9 177.56(18) . . . . ?
N7 C5 N9 N5 -0.2(2) . . . . ?
N7 C5 N9 Ag1 163.83(13) . . . 4_676 ?
N6 N5 N9 C5 0.0(2) . . . . ?
Ag1 N5 N9 C5 -179.85(13) 2_545 . . . ?
N6 N5 N9 Ag1 -166.47(12) . . . 4_676 ?
Ag1 N5 N9 Ag1 13.67(19) 2_545 . . 4_676 ?
N2 N1 N10 N4 0.7(2) . . . . ?
C2 N1 N10 N4 -178.77(17) . . . . ?
C1 N4 N10 N1 -0.5(2) . . . . ?
Ag1 N4 N10 N1 -169.69(12) 4_576 . . . ?
N10 N1 C2 C3 -94.8(2) . . . . ?
N2 N1 C2 C3 85.7(2) . . . . ?
N1 C2 C3 C4 63.5(2) . . . . ?
C5 N7 C4 C3 85.9(3) . . . . ?
N6 N7 C4 C3 -97.1(2) . . . . ?
C2 C3 C4 N7 65.9(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
? ? ? ? ? ? ? ?

_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         0.450
_refine_diff_density_min         -0.394
_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_lx561
_database_code_depnum_ccdc_archive 'CCDC 1816632'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Nov 23 15:53:49 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,2-ditetrazolylpropane
;
_chemical_name_common            1,2-ditetrazolylpropane
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H8 N8'
_chemical_formula_sum            'C5 H8 N8'
_chemical_formula_weight         180.19

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                   10.6063(6)
_cell_length_b                   6.5631(4)
_cell_length_c                   11.7632(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.685(5)
_cell_angle_gamma                90
_cell_volume                     818.78(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2576
_cell_measurement_theta_min      4.9310
_cell_measurement_theta_max      31.8630

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.310
_exptl_absorpt_coefficient_mu    0.107
_shelx_estimated_absorpt_T_min   0.956
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90909
_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    1.462
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            6419
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.654
_diffrn_reflns_theta_max         25.997
_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             1598
_reflns_number_gt                1387
_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)+(0.0457P)²+0.1131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_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         1598
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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      -0.0289123000
_diffrn_orient_matrix_UB_12      0.0703349000
_diffrn_orient_matrix_UB_13      0.0374220000
_diffrn_orient_matrix_UB_21      0.0601563000
_diffrn_orient_matrix_UB_22      0.0371370000
_diffrn_orient_matrix_UB_23      0.0166623000
_diffrn_orient_matrix_UB_31      -0.0027370000
_diffrn_orient_matrix_UB_32      0.0732987000
_diffrn_orient_matrix_UB_33      -0.0442836000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -38.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega   41.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -64.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
  5 omega   34.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
  6 omega  -93.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000    0.0000 137

#__ type_ start__ end____ width___ exp.time_
  7 omega -108.00  -72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  150.0000 36

;



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'
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
N4 N 0.16997(9) 0.79227(16) 0.09600(9) 0.0350(3) Uani 1 1 d . . . . .
N3 N 0.23957(10) 0.80602(15) -0.00025(9) 0.0349(3) Uani 1 1 d . . . . .
N2 N 0.35616(9) 0.84573(14) 0.02435(8) 0.0302(2) Uani 1 1 d . . . . .
N1 N 0.36395(8) 0.85842(13) 0.13836(7) 0.0240(2) Uani 1 1 d . . . . .
N6 N 0.68662(8) 0.62509(14) 0.09789(7) 0.0231(2) Uani 1 1 d . . . . .
N5 N 0.80116(9) 0.66409(15) 0.13885(8) 0.0301(2) Uani 1 1 d . . . . .
N7 N 0.67610(9) 0.65025(14) -0.01295(7) 0.0280(2) Uani 1 1 d . . . . .
N8 N 0.78844(9) 0.70903(15) -0.04823(8) 0.0311(3) Uani 1 1 d . . . . .
C1 C 0.24957(11) 0.82481(18) 0.17971(10) 0.0296(3) Uani 1 1 d . . . . .
C2 C 0.48295(11) 0.90211(18) 0.19836(10) 0.0286(3) Uani 1 1 d . . . . .
C3 C 0.54013(11) 0.71248(19) 0.25240(9) 0.0290(3) Uani 1 1 d . . . . .
C4 C 0.58286(10) 0.55206(17) 0.16825(10) 0.0277(3) Uani 1 1 d . . . . .
C5 C 0.86144(12) 0.71604(18) 0.04520(10) 0.0314(3) Uani 1 1 d . . . . .
H4A H 0.5160(12) 0.513(2) 0.1161(10) 0.031(3) Uiso 1 1 d . . . . .
H4B H 0.6156(12) 0.435(2) 0.2083(11) 0.036(3) Uiso 1 1 d . . . . .
H3A H 0.4782(13) 0.648(2) 0.3029(11) 0.033(3) Uiso 1 1 d . . . . .
H2B H 0.5399(13) 0.963(2) 0.1399(11) 0.035(3) Uiso 1 1 d . . . . .
H3B H 0.6106(13) 0.7537(19) 0.2982(11) 0.033(3) Uiso 1 1 d . . . . .
H2A H 0.4639(12) 1.004(2) 0.2577(11) 0.037(3) Uiso 1 1 d . . . . .
H1 H 0.2340(14) 0.827(2) 0.2576(13) 0.044(4) Uiso 1 1 d . . . . .
H5 H 0.9483(15) 0.754(2) 0.0463(12) 0.047(4) 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
N4 C1 1.3070(15) . ?
N4 N3 1.3620(15) . ?
N3 N2 1.2931(14) . ?
N2 N1 1.3453(12) . ?
N1 C1 1.3308(15) . ?
N1 C2 1.4670(13) . ?
N6 N7 1.3176(12) . ?
N6 N5 1.3266(12) . ?
N6 C4 1.4655(14) . ?
N5 C5 1.3249(16) . ?
N7 N8 1.3239(14) . ?
N8 C5 1.3376(15) . ?
C1 H1 0.934(15) . ?
C2 C3 1.5204(16) . ?
C2 H2B 1.002(14) . ?
C2 H2A 0.989(13) . ?
C3 C4 1.5180(16) . ?
C3 H3A 0.986(14) . ?
C3 H3B 0.955(14) . ?
C4 H4A 0.966(13) . ?
C4 H4B 0.965(14) . ?
C5 H5 0.954(16) . ?

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
C1 N4 N3 105.30(10) . . ?
N2 N3 N4 110.71(9) . . ?
N3 N2 N1 106.42(9) . . ?
C1 N1 N2 107.98(9) . . ?
C1 N1 C2 129.75(10) . . ?
N2 N1 C2 122.27(9) . . ?
N7 N6 N5 113.68(9) . . ?
N7 N6 C4 123.00(9) . . ?
N5 N6 C4 123.27(8) . . ?
C5 N5 N6 101.34(9) . . ?
N6 N7 N8 106.31(8) . . ?
N7 N8 C5 105.47(9) . . ?
N4 C1 N1 109.58(11) . . ?
N4 C1 H1 128.5(9) . . ?
N1 C1 H1 121.9(9) . . ?
N1 C2 C3 112.19(9) . . ?
N1 C2 H2B 105.6(7) . . ?
C3 C2 H2B 111.7(8) . . ?
N1 C2 H2A 106.9(8) . . ?
C3 C2 H2A 110.0(7) . . ?
H2B C2 H2A 110.3(11) . . ?
C4 C3 C2 114.57(9) . . ?
C4 C3 H3A 107.5(7) . . ?
C2 C3 H3A 109.7(8) . . ?
C4 C3 H3B 109.1(8) . . ?
C2 C3 H3B 108.0(8) . . ?
H3A C3 H3B 107.8(10) . . ?
N6 C4 C3 111.93(9) . . ?
N6 C4 H4A 106.2(7) . . ?
C3 C4 H4A 112.0(8) . . ?
N6 C4 H4B 105.6(8) . . ?
C3 C4 H4B 110.1(8) . . ?
H4A C4 H4B 110.9(11) . . ?
N5 C5 N8 113.21(10) . . ?
N5 C5 H5 122.1(9) . . ?
N8 C5 H5 124.7(9) . . ?

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 N3 N2 -0.17(12) . . . . ?
N4 N3 N2 N1 0.01(12) . . . . ?
N3 N2 N1 C1 0.15(12) . . . . ?
N3 N2 N1 C2 -179.98(9) . . . . ?
N7 N6 N5 C5 0.14(12) . . . . ?
C4 N6 N5 C5 177.54(10) . . . . ?
N5 N6 N7 N8 -0.08(12) . . . . ?
C4 N6 N7 N8 -177.49(9) . . . . ?
N6 N7 N8 C5 -0.02(11) . . . . ?
N3 N4 C1 N1 0.26(13) . . . . ?
N2 N1 C1 N4 -0.26(13) . . . . ?
C2 N1 C1 N4 179.89(10) . . . . ?
C1 N1 C2 C3 76.25(14) . . . . ?
N2 N1 C2 C3 -103.59(12) . . . . ?
N1 C2 C3 C4 65.85(13) . . . . ?
N7 N6 C4 C3 -115.30(11) . . . . ?
N5 N6 C4 C3 67.53(13) . . . . ?
C2 C3 C4 N6 64.69(12) . . . . ?
N6 N5 C5 N8 -0.15(12) . . . . ?
N7 N8 C5 N5 0.11(13) . . . . ?

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         0.171
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.043

_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_lx372
_database_code_depnum_ccdc_archive 'CCDC 1816628'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sun Aug 07 07:06:55 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,1-ditetrazolylpropane) manganese(II) diperchlorate
;
_chemical_name_common            
'tris(1,1-ditetrazolylpropane) manganese(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	3(C5 H8 Mn0.33 N8), 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 Mn N24 O8'
_chemical_formula_weight         794.42

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   ' P -3 c 1'
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'



_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'

_cell_length_a                   11.1661(2)
_cell_length_b                   11.1661(2)
_cell_length_c                   14.7523(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1592.92(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5282
_cell_measurement_theta_min      5.0370
_cell_measurement_theta_max      31.9770

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.665
_shelx_estimated_absorpt_T_min   0.668
_shelx_estimated_absorpt_T_max   0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79136
_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    1.656
_exptl_crystal_F_000             810
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            11705
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.215
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             1036
_reflns_number_gt                925
_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)+(0.0433P)²+0.7064P] 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     SHELXL
_refine_ls_extinction_coef       0.0033(11)
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1036
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0825
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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      0.0144877000
_diffrn_orient_matrix_UB_12      0.0510648000
_diffrn_orient_matrix_UB_13      0.0334960000
_diffrn_orient_matrix_UB_21      0.0544462000
_diffrn_orient_matrix_UB_22      0.0500395000
_diffrn_orient_matrix_UB_23      -0.0272059000
_diffrn_orient_matrix_UB_31      -0.0469719000
_diffrn_orient_matrix_UB_32      0.0164323000
_diffrn_orient_matrix_UB_33      -0.0212097000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.00   46.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   19.0000   30.0000 125

#__ type_ start__ end____ width___ exp.time_
  2 omega  -72.00  -47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557 -179.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00    9.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557  -87.0000  -97.0000 40

#__ type_ start__ end____ width___ exp.time_
  4 omega  -99.00  -35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557  -57.0000   60.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega  -15.00   75.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  -99.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   63.00  110.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  179.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
  7 omega   66.00  101.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   77.0000    0.0000 35

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  179.0000  -30.0000 60

;



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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
Mn01 Mn 0.0000 0.0000 0.0000 0.0236(2) Uani 1 6 d S T P . .
N1 N 0.13845(13) 0.18482(13) 0.08625(8) 0.0302(3) Uani 1 1 d . . . . .
N2 N 0.08721(16) 0.24895(16) 0.13808(11) 0.0448(4) Uani 1 1 d . . . . .
N3 N 0.18722(17) 0.35750(17) 0.17522(12) 0.0476(4) Uani 1 1 d . . . . .
N4 N 0.30510(14) 0.36495(13) 0.14795(9) 0.0328(3) Uani 1 1 d . . . . .
C1 C 0.27324(17) 0.25940(16) 0.09380(11) 0.0356(4) Uani 1 1 d . . . . .
H1 H 0.3378 0.2403 0.0648 0.043 Uiso 1 1 calc R U . . .
C2 C 0.4413(2) 0.48642(18) 0.16870(12) 0.0464(5) Uani 1 1 d . . . . .
C3 C 0.5240(3) 0.4649(3) 0.2316(2) 0.0337(7) Uani 0.5 1 d . . P . .
H3A H 0.6184 0.5461 0.2276 0.040 Uiso 0.5 1 calc R U P . .
H3B H 0.5301 0.3842 0.2100 0.040 Uiso 0.5 1 calc R U P . .
Cl1A Cl 0.6667 0.3333 0.0398(3) 0.0343(7) Uani 0.666(8) 3 d S T P A 1
O2A O 0.6667 0.3333 0.1349(3) 0.112(3) Uani 0.666(8) 3 d S T P A 1
O1A O 0.5318(6) 0.2446(7) 0.0098(5) 0.095(2) Uani 0.666(8) 1 d . . P A 1
O1B O 0.5341(13) 0.2226(12) 0.0412(7) 0.065(3) Uani 0.334(8) 1 d . . P A 2
O2B O 0.6667 0.3333 -0.0826(5) 0.065(3) Uani 0.334(8) 3 d S T P A 2
Cl1B Cl 0.6667 0.3333 0.0151(6) 0.0406(17) Uani 0.334(8) 3 d S T P A 2
H2B H 0.4937 0.5197 0.1100 0.049 Uiso 0.5 1 d R U P A 1
H2A H 0.4262 0.5610 0.1907 0.049 Uiso 0.5 1 d R U P A 1
H2C H 0.4575 0.5620 0.1287 0.049 Uiso 0.5 1 d R U P A 2
H2D H 0.5266 0.4625 0.1441 0.049 Uiso 0.5 1 d R U P A 2


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
Mn01 N1 2.2533(12) . ?
Mn01 N1 2.2533(12) 7 ?
Mn01 N1 2.2533(12) 9 ?
Mn01 N1 2.2533(12) 2 ?
Mn01 N1 2.2533(12) 8 ?
Mn01 N1 2.2533(12) 3 ?
N1 C1 1.311(2) . ?
N1 N2 1.354(2) . ?
N2 N3 1.290(2) . ?
N3 N4 1.339(2) . ?
N4 C1 1.317(2) . ?
N4 C2 1.477(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.412(4) . ?
C2 C3 1.516(4) 4 ?
C2 H2B 1.0067 . ?
C2 H2A 0.9832 . ?
C2 H2C 0.9692 . ?
C2 H2D 1.1683 . ?
C3 C2 1.517(4) 4 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H2D 1.2906 . ?
Cl1A O1A 1.397(6) 3_665 ?
Cl1A O1A 1.397(6) . ?
Cl1A O1A 1.397(6) 2_655 ?
Cl1A O2A 1.403(6) . ?
O1B Cl1B 1.428(11) . ?
O2B Cl1B 1.441(11) . ?
Cl1B O1B 1.428(11) 2_655 ?
Cl1B O1B 1.428(11) 3_665 ?

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 Mn01 N1 180.0 . 7 ?
N1 Mn01 N1 88.76(4) . 9 ?
N1 Mn01 N1 91.24(4) 7 9 ?
N1 Mn01 N1 91.24(4) . 2 ?
N1 Mn01 N1 88.76(4) 7 2 ?
N1 Mn01 N1 88.76(4) 9 2 ?
N1 Mn01 N1 88.76(4) . 8 ?
N1 Mn01 N1 91.24(4) 7 8 ?
N1 Mn01 N1 91.24(4) 9 8 ?
N1 Mn01 N1 180.00(7) 2 8 ?
N1 Mn01 N1 91.24(4) . 3 ?
N1 Mn01 N1 88.76(4) 7 3 ?
N1 Mn01 N1 180.00(7) 9 3 ?
N1 Mn01 N1 91.24(4) 2 3 ?
N1 Mn01 N1 88.76(4) 8 3 ?
C1 N1 N2 105.70(13) . . ?
C1 N1 Mn01 132.37(11) . . ?
N2 N1 Mn01 121.69(10) . . ?
N3 N2 N1 109.91(14) . . ?
N2 N3 N4 107.05(14) . . ?
C1 N4 N3 108.03(13) . . ?
C1 N4 C2 129.85(16) . . ?
N3 N4 C2 121.56(15) . . ?
N1 C1 N4 109.31(15) . . ?
N1 C1 H1 125.3 . . ?
N4 C1 H1 125.3 . . ?
C3 C2 N4 116.14(18) . . ?
C3 C2 C3 51.1(3) . 4 ?
N4 C2 C3 114.33(18) . 4 ?
C3 C2 H2B 108.6 . . ?
N4 C2 H2B 107.6 . . ?
C3 C2 H2B 138.1 4 . ?
C3 C2 H2A 109.3 . . ?
N4 C2 H2A 108.2 . . ?
C3 C2 H2A 61.7 4 . ?
H2B C2 H2A 106.6 . . ?
C3 C2 H2C 134.0 . . ?
N4 C2 H2C 109.4 . . ?
C3 C2 H2C 114.7 4 . ?
C3 C2 H2D 59.1 . . ?
N4 C2 H2D 108.0 . . ?
C3 C2 H2D 108.4 4 . ?
H2C C2 H2D 101.1 . . ?
C2 C3 C2 121.3(2) . 4 ?
C2 C3 H3A 107.0 . . ?
C2 C3 H3A 107.0 4 . ?
C2 C3 H3B 107.0 . . ?
C2 C3 H3B 107.0 4 . ?
H3A C3 H3B 106.7 . . ?
C2 C3 H2D 51.0 . . ?
C2 C3 H2D 166.7 4 . ?
H3A C3 H2D 86.3 . . ?
H3B C3 H2D 69.3 . . ?
O1A Cl1A O1A 110.5(4) 3_665 . ?
O1A Cl1A O1A 110.5(4) 3_665 2_655 ?
O1A Cl1A O1A 110.5(4) . 2_655 ?
O1A Cl1A O2A 108.5(4) 3_665 . ?
O1A Cl1A O2A 108.5(4) . . ?
O1A Cl1A O2A 108.5(4) 2_655 . ?
O1B Cl1B O1B 113.0(5) 2_655 3_665 ?
O1B Cl1B O1B 113.0(5) 2_655 . ?
O1B Cl1B O1B 113.0(5) 3_665 . ?
O1B Cl1B O2B 105.7(6) 2_655 . ?
O1B Cl1B O2B 105.7(6) 3_665 . ?
O1B Cl1B O2B 105.7(6) . . ?

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 -0.04(19) . . . . ?
Mn01 N1 N2 N3 -175.00(12) . . . . ?
N1 N2 N3 N4 -0.1(2) . . . . ?
N2 N3 N4 C1 0.2(2) . . . . ?
N2 N3 N4 C2 172.40(15) . . . . ?
N2 N1 C1 N4 0.19(18) . . . . ?
Mn01 N1 C1 N4 174.39(10) . . . . ?
N3 N4 C1 N1 -0.28(19) . . . . ?
C2 N4 C1 N1 -171.56(15) . . . . ?
C1 N4 C2 C3 -79.2(3) . . . . ?
N3 N4 C2 C3 110.5(2) . . . . ?
C1 N4 C2 C3 -136.1(2) . . . 4 ?
N3 N4 C2 C3 53.7(3) . . . 4 ?
N4 C2 C3 C2 -70.5(3) . . . 4 ?
C3 C2 C3 C2 30.6(3) 4 . . 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
? ? ? ? ? ? ? ?

_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         0.399
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.042

_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_lx370
_database_code_depnum_ccdc_archive 'CCDC 1816629'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Aug 05 19:15:44 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,1-ditetrazolylpropane) zinc(II) diperchlorate'
;
_chemical_name_common            
'tris(1,1-ditetrazolylpropane) zinc(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C5 H8 N8 Zn0.33), 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 N24 O8 Zn'
_chemical_formula_weight         804.85

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   ' P-3c1'
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'




_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'

_cell_length_a                   11.0824(3)
_cell_length_b                   11.0824(3)
_cell_length_c                   14.7279(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1566.53(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2167
_cell_measurement_theta_min      5.0490
_cell_measurement_theta_max      27.6970

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    1.038
_shelx_estimated_absorpt_T_min   0.547
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76358
_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    1.706
_exptl_crystal_F_000             820
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            15991
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.247
_diffrn_reflns_theta_max         32.351
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1815
_reflns_number_gt                1210
_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)+(0.0469P)²+0.5751P] 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         1815
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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      -0.0187792000
_diffrn_orient_matrix_UB_12      -0.0083280000
_diffrn_orient_matrix_UB_13      0.0465930000
_diffrn_orient_matrix_UB_21      -0.0709937000
_diffrn_orient_matrix_UB_22      -0.0281504000
_diffrn_orient_matrix_UB_23      -0.0122220000
_diffrn_orient_matrix_UB_31      -0.0084379000
_diffrn_orient_matrix_UB_32      -0.0677576000
_diffrn_orient_matrix_UB_33      -0.0006570000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -93.00  -36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  133.0000   19.0000 57

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00    4.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega -102.00  -67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
  4 omega   44.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -60.0000 66

#__ type_ start__ end____ width___ exp.time_
  5 omega   39.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega  -45.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -60.0000 133

#__ type_ start__ end____ width___ exp.time_
  7 omega  -38.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -38.0000   90.0000 84

;



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'
Cl Cl 0.1484 0.1585 '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'
Zn Zn 0.2839 1.4301 '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
Zn1 Zn 0.0000 0.0000 0.0000 0.02269(14) Uani 1 6 d S T P . .
N1 N 0.04857(16) 0.17928(16) 0.08366(10) 0.0270(3) Uani 1 1 d . . . . .
N2 N 0.16535(19) 0.24324(19) 0.13542(13) 0.0410(4) Uani 1 1 d . . . . .
N3 N 0.17401(19) 0.3524(2) 0.17358(13) 0.0431(4) Uani 1 1 d . . . . .
N4 N 0.06209(17) 0.35962(16) 0.14731(10) 0.0303(3) Uani 1 1 d . . . . .
C1 C -0.0127(2) 0.25375(19) 0.09238(13) 0.0311(4) Uani 1 1 d . . . . .
H1 H -0.0973 0.2346 0.0638 0.037 Uiso 1 1 calc R U . . .
C3 C -0.0614(4) 0.4577(4) 0.2317(2) 0.0318(8) Uani 0.5 1 d . . P . .
H3A H -0.1479 0.3754 0.2098 0.038 Uiso 0.5 1 calc R U P . .
H3B H -0.0763 0.5384 0.2274 0.038 Uiso 0.5 1 calc R U P . .
Cl1A Cl 0.3333 0.6667 -0.0143(5) 0.0341(12) Uani 0.330(9) 3 d S T P A 1
O1A O 0.2225(14) 0.5323(15) -0.0421(9) 0.060(3) Uani 0.330(9) 1 d . . P A 1
O2A O 0.3333 0.6667 0.0826(6) 0.052(3) Uani 0.330(9) 3 d S T P A 1
O2B O 0.3333 0.6667 -0.1366(4) 0.117(4) Uani 0.670(9) 3 d S T P A 2
O1B O 0.2453(8) 0.5307(7) -0.0120(6) 0.096(2) Uani 0.670(9) 1 d . . P A 2
Cl1B Cl 0.3333 0.6667 -0.0411(2) 0.0318(5) Uani 0.670(9) 3 d S T P A 2
C2 C 0.0469(3) 0.4814(2) 0.16900(15) 0.0428(5) Uani 1 1 d . . . . .
H2A H 0.1366 0.5558 0.1937 0.051 Uiso 0.5 1 d R U P B 1
H2B H 0.0295 0.5164 0.1115 0.051 Uiso 0.5 1 d R U P B 1
H2C H 0.0928 0.5418 0.1326 0.051 Uiso 0.5 1 d R U P C 2
H2D H -0.0416 0.4711 0.1541 0.051 Uiso 0.5 1 d R U P C 2


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
Zn1 N1 2.1647(15) 9 ?
Zn1 N1 2.1647(15) 3 ?
Zn1 N1 2.1647(15) . ?
Zn1 N1 2.1647(15) 2 ?
Zn1 N1 2.1647(15) 8 ?
Zn1 N1 2.1648(15) 7 ?
N1 C1 1.311(2) . ?
N1 N2 1.357(2) . ?
N2 N3 1.293(2) . ?
N3 N4 1.340(2) . ?
N4 C1 1.321(2) . ?
N4 C2 1.477(3) . ?
C1 H1 0.9500 . ?
C3 C2 1.430(4) . ?
C3 C2 1.507(4) 5 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H2D 1.1595 . ?
Cl1A O2A 1.428(12) . ?
Cl1A O1A 1.437(12) . ?
Cl1A O1A 1.437(12) 3_565 ?
Cl1A O1A 1.437(12) 2_665 ?
O2B Cl1B 1.406(7) . ?
O1B Cl1B 1.391(6) . ?
Cl1B O1B 1.392(6) 3_565 ?
Cl1B O1B 1.392(6) 2_665 ?
C2 C3 1.507(4) 5 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2C 0.8086 . ?
C2 H2D 0.9546 . ?

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 Zn1 N1 180.00(9) 9 3 ?
N1 Zn1 N1 89.20(6) 9 . ?
N1 Zn1 N1 90.80(6) 3 . ?
N1 Zn1 N1 89.20(6) 9 2 ?
N1 Zn1 N1 90.80(6) 3 2 ?
N1 Zn1 N1 90.80(6) . 2 ?
N1 Zn1 N1 90.80(6) 9 8 ?
N1 Zn1 N1 89.20(6) 3 8 ?
N1 Zn1 N1 89.20(6) . 8 ?
N1 Zn1 N1 180.00(15) 2 8 ?
N1 Zn1 N1 90.80(6) 9 7 ?
N1 Zn1 N1 89.20(6) 3 7 ?
N1 Zn1 N1 180.0 . 7 ?
N1 Zn1 N1 89.20(6) 2 7 ?
N1 Zn1 N1 90.80(6) 8 7 ?
C1 N1 N2 105.96(15) . . ?
C1 N1 Zn1 131.62(13) . . ?
N2 N1 Zn1 122.26(12) . . ?
N3 N2 N1 109.77(17) . . ?
N2 N3 N4 107.02(16) . . ?
C1 N4 N3 108.18(15) . . ?
C1 N4 C2 129.54(18) . . ?
N3 N4 C2 121.66(17) . . ?
N1 C1 N4 109.07(17) . . ?
N1 C1 H1 125.5 . . ?
N4 C1 H1 125.5 . . ?
C2 C3 C2 120.4(3) . 5 ?
C2 C3 H3A 107.2 . . ?
C2 C3 H3A 107.2 5 . ?
C2 C3 H3B 107.2 . . ?
C2 C3 H3B 107.2 5 . ?
H3A C3 H3B 106.9 . . ?
C2 C3 H2D 161.6 5 . ?
H3A C3 H2D 80.3 . . ?
H3B C3 H2D 85.8 . . ?
O2A Cl1A O1A 106.6(7) . . ?
O2A Cl1A O1A 106.6(7) . 3_565 ?
O1A Cl1A O1A 112.2(6) . 3_565 ?
O2A Cl1A O1A 106.6(7) . 2_665 ?
O1A Cl1A O1A 112.2(6) . 2_665 ?
O1A Cl1A O1A 112.2(6) 3_565 2_665 ?
O1B Cl1B O1B 110.9(4) . 3_565 ?
O1B Cl1B O1B 110.9(4) . 2_665 ?
O1B Cl1B O1B 110.9(4) 3_565 2_665 ?
O1B Cl1B O2B 108.0(5) . . ?
O1B Cl1B O2B 108.0(5) 3_565 . ?
O1B Cl1B O2B 108.0(5) 2_665 . ?
C3 C2 N4 116.1(2) . . ?
C3 C2 C3 52.3(3) . 5 ?
N4 C2 C3 114.7(2) . 5 ?
C3 C2 H2A 108.5 . . ?
N4 C2 H2A 108.3 . . ?
C3 C2 H2A 59.3 5 . ?
C3 C2 H2B 108.4 . . ?
N4 C2 H2B 107.8 . . ?
C3 C2 H2B 137.5 5 . ?
H2A C2 H2B 107.3 . . ?
C3 C2 H2C 134.7 . . ?
N4 C2 H2C 107.5 . . ?
C3 C2 H2C 118.6 5 . ?
C3 C2 H2D 53.8 . . ?
N4 C2 H2D 114.9 . . ?
C3 C2 H2D 102.6 5 . ?
H2C C2 H2D 97.5 . . ?

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 N1 N2 N3 -0.2(2) . . . . ?
Zn1 N1 N2 N3 175.68(14) . . . . ?
N1 N2 N3 N4 0.4(2) . . . . ?
N2 N3 N4 C1 -0.5(2) . . . . ?
N2 N3 N4 C2 -172.28(17) . . . . ?
N2 N1 C1 N4 -0.1(2) . . . . ?
Zn1 N1 C1 N4 -175.44(12) . . . . ?
N3 N4 C1 N1 0.4(2) . . . . ?
C2 N4 C1 N1 171.32(17) . . . . ?
C2 C3 C2 N4 72.0(3) 5 . . . ?
C2 C3 C2 C3 -30.1(4) 5 . . 5 ?
C1 N4 C2 C3 78.0(3) . . . . ?
N3 N4 C2 C3 -112.2(3) . . . . ?
C1 N4 C2 C3 136.3(3) . . . 5 ?
N3 N4 C2 C3 -53.8(3) . . . 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         0.536
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.069

_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_lx280
_database_code_depnum_ccdc_archive 'CCDC 1816636'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_lx280               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         56 Note
RESPONSE: low crystal quality due to low solubility in any solvent
;
_vrf_PLAT097_lx280               
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.98 eA-3
RESPONSE: low crystal quality due to low solubility in any solvent
;
_vrf_PLAT971_lx280               
;
PROBLEM: Check Calcd Resid. Dens.  1.36A   From C23             2.72 eA-3
RESPONSE: low crystal quality due to low solubility in any solvent
;
_audit_creation_date             
;
'Thu Jun 02 09:16:08 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,2-ditetrazolylpropane copper(II) perchlorate
;
_chemical_name_common            
'1,2-ditetrazolylpropane copper(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H48 Cu2 N48, 4(Cl O4)'
_chemical_formula_sum            'C30 H48 Cl4 Cu2 N48 O16'
_chemical_formula_weight         1606.04

_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                   13.2260(6)
_cell_length_b                   13.7860(8)
_cell_length_c                   20.2220(8)
_cell_angle_alpha                99.253(4)
_cell_angle_beta                 102.001(4)
_cell_angle_gamma                114.596(5)
_cell_volume                     3150.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5758
_cell_measurement_theta_min      4.3570
_cell_measurement_theta_max      27.7360

_exptl_crystal_description       stab
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.163
_exptl_absorpt_coefficient_mu    0.947
_shelx_estimated_absorpt_T_min   0.802
_shelx_estimated_absorpt_T_max   0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.693
_exptl_crystal_F_000             1636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_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            22717
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.151
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.240
_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             12300
_reflns_number_gt                9173
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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)+(0.0844P)²+10.5040P] 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         12300
_refine_ls_number_parameters     925
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1860
_refine_ls_wR_factor_gt          0.1665
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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      0.0163229000
_diffrn_orient_matrix_UB_12      -0.0407572000
_diffrn_orient_matrix_UB_13      -0.0123698000
_diffrn_orient_matrix_UB_21      0.0490297000
_diffrn_orient_matrix_UB_22      0.0235441000
_diffrn_orient_matrix_UB_23      0.0306577000
_diffrn_orient_matrix_UB_31      -0.0341838000
_diffrn_orient_matrix_UB_32      -0.0354253000
_diffrn_orient_matrix_UB_33      0.0173424000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -62.00   -7.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -57.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
  2 omega  -45.00   20.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931   38.0000 -150.0000 65

#__ type_ start__ end____ width___ exp.time_
  3 omega  -19.00   23.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -99.0000 -180.0000 42

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00    0.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -99.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  5 omega   15.00   66.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   38.0000    0.0000 51

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00   44.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  -57.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
  7 omega    0.00   92.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   57.0000   30.0000 92

;



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'
Cl Cl 0.1484 0.1585 '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 0.74948(5) 0.19787(5) 0.50119(3) 0.01927(15) Uani 1 1 d . . . . .
Cu2 Cu 0.26541(5) 0.25439(4) 0.01769(3) 0.01850(15) Uani 1 1 d . . . . .
N12 N 0.7387(3) 0.0239(3) 0.4699(2) 0.0222(8) Uani 1 1 d . . . . .
N11 N 0.6630(4) -0.0499(3) 0.4078(2) 0.0261(9) Uani 1 1 d . . . . .
N10 N 0.6425(4) -0.1495(3) 0.4097(2) 0.0257(9) Uani 1 1 d . . . . .
N9 N 0.7065(3) -0.1404(3) 0.4740(2) 0.0214(8) Uani 1 1 d . . . . .
N14 N 0.9126(3) -0.2876(3) 0.4093(2) 0.0196(8) Uani 1 1 d . . . . .
N13 N 0.9186(4) -0.3412(3) 0.3506(2) 0.0250(9) Uani 1 1 d . . . . .
N15 N 1.0096(3) -0.2385(3) 0.4612(2) 0.0231(9) Uani 1 1 d . . . . .
N16 N 1.0849(3) -0.2622(3) 0.4366(2) 0.0216(8) Uani 1 1 d . . . . .
N4 N 0.6972(3) 0.1660(3) 0.58698(19) 0.0214(8) Uani 1 1 d . . . . .
N1 N 0.6374(4) 0.1683(4) 0.6804(2) 0.0369(11) Uani 1 1 d . . . . .
N3 N 0.7569(4) 0.1334(3) 0.6311(2) 0.0268(9) Uani 1 1 d . . . . .
N2 N 0.7197(4) 0.1366(4) 0.6855(2) 0.0285(10) Uani 1 1 d . . . . .
N20 N 0.8073(3) 0.2374(3) 0.4189(2) 0.0225(8) Uani 1 1 d . . . . .
N19 N 0.7927(4) 0.3158(3) 0.3950(2) 0.0250(9) Uani 1 1 d . . . . .
N17 N 0.8758(4) 0.2502(4) 0.3279(2) 0.0270(9) Uani 1 1 d . . . . .
N18 N 0.8343(3) 0.3208(3) 0.3413(2) 0.0214(8) Uani 1 1 d . . . . .
N21 N 0.6081(3) 0.3645(3) 0.13396(19) 0.0187(8) Uani 1 1 d . . . . .
N22 N 0.6078(4) 0.3174(4) 0.0700(2) 0.0280(9) Uani 1 1 d . . . . .
N23 N 0.5018(4) 0.2734(4) 0.0288(2) 0.0269(9) Uani 1 1 d . . . . .
N24 N 0.4326(3) 0.2897(3) 0.0656(2) 0.0206(8) Uani 1 1 d . . . . .
N30 N 0.8232(4) 0.8603(3) 0.8167(2) 0.0240(9) Uani 1 1 d . . . . .
N31 N 0.7721(4) 0.8501(3) 0.8649(2) 0.0227(8) Uani 1 1 d . . . . .
N29 N 0.8648(3) 0.7864(3) 0.81342(19) 0.0189(8) Uani 1 1 d . . . . .
N32 N 0.7812(3) 0.7698(3) 0.89371(19) 0.0188(8) Uani 1 1 d . . . . .
N25 N 0.7109(4) 0.5192(4) 0.5606(2) 0.0309(10) Uani 1 1 d . . . . .
N28 N 0.7527(4) 0.3794(3) 0.5411(2) 0.0283(9) Uani 1 1 d . . . . .
N26 N 0.7684(4) 0.5102(3) 0.6194(2) 0.0225(8) Uani 1 1 d . . . . .
N27 N 0.7954(4) 0.4283(4) 0.6095(2) 0.0311(10) Uani 1 1 d . . . . .
N41 N 0.3486(5) 0.6164(4) 0.0865(3) 0.0483(14) Uani 1 1 d . . . . .
N44 N 0.3216(4) 0.4446(3) 0.0629(2) 0.0277(9) Uani 1 1 d . . . . .
N42 N 0.3810(4) 0.5894(4) 0.1435(2) 0.0333(11) Uani 1 1 d . . . . .
N43 N 0.3662(4) 0.4883(3) 0.1321(2) 0.0311(10) Uani 1 1 d . . . . .
N34 N 0.1121(4) -0.1163(4) -0.0682(2) 0.0315(10) Uani 1 1 d . . . . .
N35 N 0.1107(4) -0.0221(3) -0.0625(2) 0.0293(10) Uani 1 1 d . . . . .
N36 N 0.2150(4) 0.0628(3) -0.0195(2) 0.0222(8) Uani 1 1 d . . . . .
N33 N 0.2172(4) -0.0937(3) -0.0280(2) 0.0228(8) Uani 1 1 d . . . . .
C6 C 0.7638(4) -0.0349(4) 0.5095(2) 0.0234(10) Uani 1 1 d . . . . .
H6 H 0.8152 -0.0056 0.5563 0.028 Uiso 1 1 calc R U . . .
C7 C 0.7016(5) -0.2396(4) 0.4952(3) 0.0301(11) Uani 1 1 d . . . . .
H7A H 0.6295 -0.3063 0.4646 0.036 Uiso 1 1 calc R U . . .
H7B H 0.6995 -0.2317 0.5443 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8078(5) -0.2535(4) 0.4891(3) 0.0261(11) Uani 1 1 d . . . . .
H8A H 0.8797 -0.1853 0.5182 0.031 Uiso 1 1 calc R U . . .
H8B H 0.8073 -0.3160 0.5075 0.031 Uiso 1 1 calc R U . . .
C9 C 0.8093(4) -0.2758(4) 0.4137(3) 0.0244(10) Uani 1 1 d . . . . .
H9A H 0.7382 -0.3447 0.3845 0.029 Uiso 1 1 calc R U . . .
H9B H 0.8092 -0.2138 0.3949 0.029 Uiso 1 1 calc R U . . .
C10 C 1.0272(4) -0.3246(4) 0.3694(3) 0.0263(11) Uani 1 1 d . . . . .
H10 H 1.0608 -0.3530 0.3393 0.032 Uiso 1 1 calc R U . . .
C2 C 0.7711(5) 0.1120(5) 0.7491(3) 0.0420(15) Uani 1 1 d . . . . .
H2A H 0.8337 0.0942 0.7415 0.050 Uiso 1 1 calc R U . . .
H2B H 0.8072 0.1792 0.7896 0.050 Uiso 1 1 calc R U . . .
C1 C 0.6247(5) 0.1866(4) 0.6177(3) 0.0289(11) Uani 1 1 d . . . . .
H1 H 0.5715 0.2111 0.5971 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8578(4) 0.1985(4) 0.3777(2) 0.0246(10) Uani 1 1 d . . . . .
H11 H 0.8779 0.1411 0.3835 0.029 Uiso 1 1 calc R U . . .
C12 C 0.8282(4) 0.3967(4) 0.2994(3) 0.0258(11) Uani 1 1 d . . . . .
H12A H 0.9027 0.4322 0.2885 0.031 Uiso 1 1 calc R U . . .
H12B H 0.8178 0.4560 0.3271 0.031 Uiso 1 1 calc R U . . .
C13 C 0.7281(4) 0.3363(4) 0.2313(2) 0.0238(10) Uani 1 1 d . . . . .
H13A H 0.6548 0.2930 0.2414 0.029 Uiso 1 1 calc R U . . .
H13B H 0.7435 0.2840 0.2004 0.029 Uiso 1 1 calc R U . . .
C14 C 0.7152(4) 0.4200(4) 0.1943(3) 0.0247(10) Uani 1 1 d . . . . .
H14A H 0.7121 0.4789 0.2277 0.030 Uiso 1 1 calc R U . . .
H14B H 0.7838 0.4553 0.1778 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5010(4) 0.3467(4) 0.1309(3) 0.0234(10) Uani 1 1 d . . . . .
H15 H 0.4771 0.3706 0.1688 0.028 Uiso 1 1 calc R U . . .
C20 C 0.8377(4) 0.7313(4) 0.8606(2) 0.0189(9) Uani 1 1 d . . . . .
H20 H 0.8562 0.6739 0.8689 0.023 Uiso 1 1 calc R U . . .
C19 C 0.9322(4) 0.7796(4) 0.7652(2) 0.0231(10) Uani 1 1 d . . . . .
H19A H 0.9866 0.7520 0.7850 0.028 Uiso 1 1 calc R U . . .
H19B H 0.9797 0.8552 0.7617 0.028 Uiso 1 1 calc R U . . .
C18 C 0.8560(4) 0.7039(4) 0.6915(2) 0.0229(10) Uani 1 1 d . . . . .
H18A H 0.7941 0.7244 0.6742 0.028 Uiso 1 1 calc R U . . .
H18B H 0.9044 0.7152 0.6593 0.028 Uiso 1 1 calc R U . . .
C17 C 0.8000(5) 0.5825(4) 0.6899(2) 0.0265(11) Uani 1 1 d . . . . .
H17A H 0.8551 0.5688 0.7237 0.032 Uiso 1 1 calc R U . . .
H17B H 0.7291 0.5642 0.7048 0.032 Uiso 1 1 calc R U . . .
C16 C 0.7029(5) 0.4368(4) 0.5132(3) 0.0295(11) Uani 1 1 d . . . . .
H16 H 0.6657 0.4197 0.4643 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3116(6) 0.5240(4) 0.0363(3) 0.0397(14) Uani 1 1 d . . . . .
H26 H 0.2817 0.5153 -0.0124 0.048 Uiso 1 1 calc R U . . .
C27 C 0.4216(6) 0.6638(5) 0.2157(3) 0.0472(17) Uani 1 1 d . . . . .
H27A H 0.3558 0.6750 0.2242 0.057 Uiso 1 1 calc R U . . .
H27B H 0.4419 0.6255 0.2496 0.057 Uiso 1 1 calc R U . . .
C21 C 0.2787(4) 0.0147(4) 0.0011(3) 0.0259(11) Uani 1 1 d . . . . .
H21 H 0.3565 0.0520 0.0320 0.031 Uiso 1 1 calc R U . . .
C22 C 0.2544(5) -0.1801(4) -0.0258(3) 0.0337(12) Uani 1 1 d . . . . .
H22A H 0.2095 -0.2406 -0.0702 0.040 Uiso 1 1 calc R U . . .
H22B H 0.3380 -0.1480 -0.0231 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.57410(13) 0.03194(11) 0.15589(7) 0.0383(3) Uani 1 1 d . . . . .
O1 O 0.6843(6) 0.0515(7) 0.1450(3) 0.100(2) Uani 1 1 d . . . . .
O2 O 0.5968(4) 0.0686(4) 0.2290(2) 0.0540(12) Uani 1 1 d . . . . .
O3 O 0.4973(8) -0.0803(5) 0.1279(4) 0.137(4) Uani 1 1 d . . . . .
O4 O 0.5315(5) 0.0965(4) 0.1222(3) 0.0662(15) Uani 1 1 d . . . . .
Cl2 Cl 0.50444(13) 0.42467(11) 0.32966(7) 0.0388(3) Uani 1 1 d . . . . .
O5 O 0.6054(6) 0.4321(11) 0.3279(5) 0.207(7) Uani 1 1 d . . . . .
O6 O 0.4662(8) 0.3542(6) 0.3786(4) 0.119(3) Uani 1 1 d . . . . .
O7 O 0.5050(5) 0.5186(5) 0.3655(4) 0.103(3) Uani 1 1 d . . . . .
O8 O 0.4106(4) 0.3638(4) 0.2669(2) 0.0478(11) Uani 1 1 d . . . . .
Cl3 Cl 0.04384(11) 0.52319(11) 0.17073(6) 0.0304(3) Uani 1 1 d . . . . .
O9 O 0.1229(4) 0.5038(4) 0.1409(3) 0.0559(12) Uani 1 1 d . . . . .
O10 O 0.1089(7) 0.6150(6) 0.2315(3) 0.106(3) Uani 1 1 d . . . . .
O11 O -0.0199(4) 0.4284(6) 0.1915(3) 0.089(2) Uani 1 1 d . . . . .
O12 O -0.0336(4) 0.5422(5) 0.1202(3) 0.0612(14) Uani 1 1 d . . . . .
Cl4 Cl 0.02192(11) 0.02612(10) 0.67294(7) 0.0340(3) Uani 1 1 d . . . . .
N5 N 0.5585(3) -0.1118(3) 0.64965(19) 0.0225(8) Uani 1 1 d . . . . .
N45 N 0.6574(4) 0.7396(4) 0.1705(2) 0.0279(9) Uani 1 1 d . . . . .
C4 C 0.6361(5) -0.0944(5) 0.7193(3) 0.0309(12) Uani 1 1 d . . . . .
H4A H 0.7014 -0.1084 0.7127 0.037 Uiso 1 1 calc R U . . .
H4B H 0.5918 -0.1492 0.7420 0.037 Uiso 1 1 calc R U . . .
N46 N 0.6552(5) 0.6413(5) 0.1528(3) 0.0482(14) Uani 1 1 d . . . . .
C29 C 0.6396(5) 0.7796(5) 0.2377(3) 0.0393(14) Uani 1 1 d . . . . .
H29A H 0.7003 0.8575 0.2603 0.047 Uiso 1 1 calc R U . . .
H29B H 0.6512 0.7349 0.2694 0.047 Uiso 1 1 calc R U . . .
C3 C 0.6848(6) 0.0187(5) 0.7669(3) 0.0480(16) Uani 1 1 d . . . . .
H3A H 0.6188 0.0342 0.7693 0.058 Uiso 1 1 calc R U . . .
H3B H 0.7218 0.0181 0.8146 0.058 Uiso 1 1 calc R U . . .
N7 N 0.4992(4) -0.1536(4) 0.5383(2) 0.0293(10) Uani 1 1 d . . . . .
N6 N 0.5868(4) -0.1337(4) 0.5907(2) 0.0323(10) Uani 1 1 d . . . . .
N38 N 0.0465(4) -0.2537(3) 0.0429(2) 0.0229(9) Uani 1 1 d . . . . .
N37 N 0.0828(4) -0.1617(4) 0.0934(2) 0.0349(11) Uani 1 1 d . . . . .
C5 C 0.4535(4) -0.1180(4) 0.6313(2) 0.0221(10) Uani 1 1 d . . . . .
H5 H 0.4132 -0.1051 0.6628 0.027 Uiso 1 1 calc R U . . .
C24 C 0.1197(5) -0.3075(5) 0.0325(3) 0.0316(12) Uani 1 1 d . . . . .
H24A H 0.0805 -0.3656 -0.0131 0.038 Uiso 1 1 calc R U . . .
H24B H 0.1273 -0.3443 0.0701 0.038 Uiso 1 1 calc R U . . .
N8 N 0.4141(3) -0.1450(3) 0.56195(19) 0.0203(8) Uani 1 1 d . . . . .
N39 N -0.0619(3) -0.2952(3) 0.0042(2) 0.0235(9) Uani 1 1 d . . . . .
N47 N 0.6784(5) 0.6335(4) 0.0936(3) 0.0429(13) Uani 1 1 d . . . . .
C30 C 0.6821(5) 0.7910(4) 0.1220(3) 0.0291(11) Uani 1 1 d . . . . .
H30 H 0.6890 0.8625 0.1222 0.035 Uiso 1 1 calc R U . . .
C25 C -0.0115(5) -0.1477(5) 0.0833(3) 0.0318(12) Uani 1 1 d . . . . .
H25 H -0.0159 -0.0881 0.1112 0.038 Uiso 1 1 calc R U . . .
N40 N -0.1003(3) -0.2274(3) 0.02905(19) 0.0197(8) Uani 1 1 d . . . . .
N48 N 0.6957(4) 0.7259(3) 0.0730(2) 0.0234(9) Uani 1 1 d . . . . .
O13 O -0.0912(5) -0.0652(5) 0.6533(3) 0.088(2) Uani 1 1 d . . . . .
O14 O 0.0085(8) 0.1190(6) 0.6670(4) 0.070(3) Uani 0.811(11) 1 d . . P A 1
O15 O 0.0872(7) 0.0163(6) 0.6244(5) 0.089(3) Uani 0.811(11) 1 d . . P A 1
O16 O 0.0845(6) 0.0399(8) 0.7424(4) 0.093(4) Uani 0.811(11) 1 d . . P A 1
O15B O 0.0851(16) -0.0198(17) 0.6940(14) 0.029(6) Uani 0.189(11) 1 d . . P A 2
O16B O 0.051(3) 0.119(3) 0.734(2) 0.11(2) Uani 0.189(11) 1 d . . P A 2
O14B O 0.032(3) 0.086(3) 0.6258(17) 0.069(10) Uiso 0.189(11) 1 d . . P A 2
C23 C 0.2388(7) -0.2277(7) 0.0334(5) 0.067(2) Uani 1 1 d . . . . .
H23A H 0.2714 -0.1649 0.0763 0.081 Uiso 1 1 calc R U . . .
H23B H 0.2880 -0.2655 0.0390 0.081 Uiso 1 1 calc R U . . .
C28 C 0.5233(6) 0.7742(6) 0.2308(4) 0.0552(18) Uani 1 1 d . . . . .
H28A H 0.5288 0.8216 0.2751 0.066 Uiso 1 1 calc R U . . .
H28B H 0.5067 0.8078 0.1928 0.066 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 N16 2.012(4) 2_756 ?
Cu1 N8 2.020(4) 2_656 ?
Cu1 N20 2.031(4) . ?
Cu1 N4 2.042(4) . ?
Cu1 N12 2.316(4) . ?
Cu2 N24 2.032(4) . ?
Cu2 N48 2.034(4) 2_665 ?
Cu2 N40 2.038(4) 2 ?
Cu2 N32 2.045(4) 2_666 ?
Cu2 N44 2.364(4) . ?
Cu2 N36 2.382(4) . ?
N12 C6 1.315(6) . ?
N12 N11 1.353(5) . ?
N11 N10 1.293(6) . ?
N10 N9 1.351(6) . ?
N9 C6 1.313(6) . ?
N9 C7 1.478(6) . ?
N14 N15 1.302(5) . ?
N14 N13 1.329(5) . ?
N14 C9 1.460(6) . ?
N13 C10 1.315(6) . ?
N15 N16 1.331(5) . ?
N16 C10 1.347(6) . ?
N16 Cu1 2.012(4) 2_756 ?
N4 N3 1.324(6) . ?
N4 C1 1.343(6) . ?
N1 C1 1.323(7) . ?
N1 N2 1.323(7) . ?
N3 N2 1.297(6) . ?
N2 C2 1.484(7) . ?
N20 N19 1.320(6) . ?
N20 C11 1.346(6) . ?
N19 N18 1.315(5) . ?
N17 N18 1.321(6) . ?
N17 C11 1.330(6) . ?
N18 C12 1.466(6) . ?
N21 C15 1.318(6) . ?
N21 N22 1.350(5) . ?
N21 C14 1.470(6) . ?
N22 N23 1.292(6) . ?
N23 N24 1.357(5) . ?
N24 C15 1.326(6) . ?
N30 N31 1.291(5) . ?
N30 N29 1.344(6) . ?
N31 N32 1.368(5) . ?
N29 C20 1.328(6) . ?
N29 C19 1.469(6) . ?
N32 C20 1.308(6) . ?
N32 Cu2 2.045(4) 2_666 ?
N25 C16 1.315(6) . ?
N25 N26 1.326(6) . ?
N28 N27 1.320(6) . ?
N28 C16 1.342(7) . ?
N26 N27 1.317(6) . ?
N26 C17 1.466(6) . ?
N41 N42 1.311(7) . ?
N41 C26 1.323(7) . ?
N44 N43 1.327(6) . ?
N44 C26 1.336(7) . ?
N42 N43 1.298(6) . ?
N42 C27 1.484(7) . ?
N34 N35 1.294(6) . ?
N34 N33 1.333(6) . ?
N35 N36 1.363(6) . ?
N36 C21 1.315(6) . ?
N33 C21 1.322(6) . ?
N33 C22 1.470(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.521(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.513(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10 0.9500 . ?
C2 C3 1.477(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.516(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.519(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 0.9500 . ?
C20 H20 0.9500 . ?
C19 C18 1.525(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C18 C17 1.514(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C16 H16 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.481(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C21 H21 0.9500 . ?
C22 C23 1.465(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
Cl1 O3 1.385(6) . ?
Cl1 O2 1.406(4) . ?
Cl1 O4 1.424(5) . ?
Cl1 O1 1.439(6) . ?
Cl2 O5 1.304(6) . ?
Cl2 O7 1.375(6) . ?
Cl2 O8 1.411(4) . ?
Cl2 O6 1.513(7) . ?
Cl3 O9 1.404(4) . ?
Cl3 O11 1.415(5) . ?
Cl3 O10 1.416(6) . ?
Cl3 O12 1.426(5) . ?
Cl4 O15B 1.288(18) . ?
Cl4 O14B 1.35(3) . ?
Cl4 O14 1.384(6) . ?
Cl4 O16 1.411(6) . ?
Cl4 O13 1.416(5) . ?
Cl4 O15 1.461(6) . ?
Cl4 O16B 1.48(3) . ?
N5 C5 1.324(6) . ?
N5 N6 1.347(6) . ?
N5 C4 1.476(6) . ?
N45 C30 1.319(6) . ?
N45 N46 1.331(7) . ?
N45 C29 1.484(6) . ?
C4 C3 1.481(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N46 N47 1.295(6) . ?
C29 C28 1.485(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N7 N6 1.293(6) . ?
N7 N8 1.352(5) . ?
N38 N39 1.304(6) . ?
N38 N37 1.323(6) . ?
N38 C24 1.472(6) . ?
N37 C25 1.320(7) . ?
C5 N8 1.321(6) . ?
C5 H5 0.9500 . ?
C24 C23 1.494(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
N8 Cu1 2.020(4) 2_656 ?
N39 N40 1.317(5) . ?
N47 N48 1.348(6) . ?
C30 N48 1.320(6) . ?
C30 H30 0.9500 . ?
C25 N40 1.338(6) . ?
C25 H25 0.9500 . ?
N40 Cu2 2.038(4) 2 ?
N48 Cu2 2.034(4) 2_665 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 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
N16 Cu1 N8 175.64(16) 2_756 2_656 ?
N16 Cu1 N20 90.41(16) 2_756 . ?
N8 Cu1 N20 87.68(16) 2_656 . ?
N16 Cu1 N4 87.67(16) 2_756 . ?
N8 Cu1 N4 94.09(16) 2_656 . ?
N20 Cu1 N4 177.12(16) . . ?
N16 Cu1 N12 91.19(15) 2_756 . ?
N8 Cu1 N12 92.77(15) 2_656 . ?
N20 Cu1 N12 91.23(15) . . ?
N4 Cu1 N12 90.95(15) . . ?
N24 Cu2 N48 90.31(16) . 2_665 ?
N24 Cu2 N40 177.08(15) . 2 ?
N48 Cu2 N40 89.51(16) 2_665 2 ?
N24 Cu2 N32 92.01(15) . 2_666 ?
N48 Cu2 N32 177.47(16) 2_665 2_666 ?
N40 Cu2 N32 88.23(15) 2 2_666 ?
N24 Cu2 N44 87.72(15) . . ?
N48 Cu2 N44 93.66(15) 2_665 . ?
N40 Cu2 N44 89.39(15) 2 . ?
N32 Cu2 N44 87.45(15) 2_666 . ?
N24 Cu2 N36 89.68(15) . . ?
N48 Cu2 N36 89.51(15) 2_665 . ?
N40 Cu2 N36 93.23(15) 2 . ?
N32 Cu2 N36 89.49(14) 2_666 . ?
N44 Cu2 N36 175.91(15) . . ?
C6 N12 N11 105.9(4) . . ?
C6 N12 Cu1 130.2(3) . . ?
N11 N12 Cu1 119.9(3) . . ?
N10 N11 N12 110.1(4) . . ?
N11 N10 N9 106.6(4) . . ?
C6 N9 N10 108.2(4) . . ?
C6 N9 C7 130.6(4) . . ?
N10 N9 C7 121.2(4) . . ?
N15 N14 N13 114.6(4) . . ?
N15 N14 C9 122.2(4) . . ?
N13 N14 C9 123.0(4) . . ?
C10 N13 N14 102.1(4) . . ?
N14 N15 N16 105.1(4) . . ?
N15 N16 C10 106.6(4) . . ?
N15 N16 Cu1 119.0(3) . 2_756 ?
C10 N16 Cu1 134.3(3) . 2_756 ?
N3 N4 C1 107.1(4) . . ?
N3 N4 Cu1 117.4(3) . . ?
C1 N4 Cu1 134.5(4) . . ?
C1 N1 N2 102.3(4) . . ?
N2 N3 N4 105.2(4) . . ?
N3 N2 N1 114.6(4) . . ?
N3 N2 C2 121.7(5) . . ?
N1 N2 C2 123.7(4) . . ?
N19 N20 C11 106.8(4) . . ?
N19 N20 Cu1 118.6(3) . . ?
C11 N20 Cu1 134.5(3) . . ?
N18 N19 N20 105.2(4) . . ?
N18 N17 C11 101.7(4) . . ?
N19 N18 N17 114.7(4) . . ?
N19 N18 C12 120.7(4) . . ?
N17 N18 C12 124.6(4) . . ?
C15 N21 N22 108.9(4) . . ?
C15 N21 C14 129.8(4) . . ?
N22 N21 C14 121.2(4) . . ?
N23 N22 N21 106.8(4) . . ?
N22 N23 N24 109.6(4) . . ?
C15 N24 N23 106.7(4) . . ?
C15 N24 Cu2 130.3(3) . . ?
N23 N24 Cu2 122.1(3) . . ?
N31 N30 N29 107.1(4) . . ?
N30 N31 N32 109.3(4) . . ?
C20 N29 N30 108.6(4) . . ?
C20 N29 C19 130.4(4) . . ?
N30 N29 C19 120.9(4) . . ?
C20 N32 N31 106.7(4) . . ?
C20 N32 Cu2 131.2(3) . 2_666 ?
N31 N32 Cu2 121.3(3) . 2_666 ?
C16 N25 N26 101.5(4) . . ?
N27 N28 C16 105.6(4) . . ?
N27 N26 N25 113.8(4) . . ?
N27 N26 C17 121.6(4) . . ?
N25 N26 C17 124.6(4) . . ?
N26 N27 N28 106.0(4) . . ?
N42 N41 C26 102.3(5) . . ?
N43 N44 C26 106.2(4) . . ?
N43 N44 Cu2 117.8(3) . . ?
C26 N44 Cu2 135.8(4) . . ?
N43 N42 N41 114.3(4) . . ?
N43 N42 C27 122.2(5) . . ?
N41 N42 C27 123.4(5) . . ?
N42 N43 N44 105.7(4) . . ?
N35 N34 N33 106.2(4) . . ?
N34 N35 N36 110.8(4) . . ?
C21 N36 N35 104.9(4) . . ?
C21 N36 Cu2 127.4(3) . . ?
N35 N36 Cu2 127.5(3) . . ?
C21 N33 N34 108.9(4) . . ?
C21 N33 C22 129.0(4) . . ?
N34 N33 C22 121.8(4) . . ?
N9 C6 N12 109.2(4) . . ?
N9 C6 H6 125.4 . . ?
N12 C6 H6 125.4 . . ?
N9 C7 C8 110.1(4) . . ?
N9 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
N9 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
C9 C8 C7 111.7(4) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N14 C9 C8 110.7(4) . . ?
N14 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N14 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N13 C10 N16 111.7(4) . . ?
N13 C10 H10 124.2 . . ?
N16 C10 H10 124.2 . . ?
C3 C2 N2 113.3(5) . . ?
C3 C2 H2A 108.9 . . ?
N2 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
N2 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N1 C1 N4 110.9(5) . . ?
N1 C1 H1 124.6 . . ?
N4 C1 H1 124.6 . . ?
N17 C11 N20 111.7(4) . . ?
N17 C11 H11 124.2 . . ?
N20 C11 H11 124.2 . . ?
N18 C12 C13 111.4(4) . . ?
N18 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
N18 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C12 C13 C14 109.6(4) . . ?
C12 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
C12 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
N21 C14 C13 110.1(4) . . ?
N21 C14 H14A 109.6 . . ?
C13 C14 H14A 109.6 . . ?
N21 C14 H14B 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
N21 C15 N24 108.0(4) . . ?
N21 C15 H15 126.0 . . ?
N24 C15 H15 126.0 . . ?
N32 C20 N29 108.3(4) . . ?
N32 C20 H20 125.9 . . ?
N29 C20 H20 125.9 . . ?
N29 C19 C18 113.3(4) . . ?
N29 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
N29 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C17 C18 C19 112.2(4) . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N26 C17 C18 111.5(4) . . ?
N26 C17 H17A 109.3 . . ?
C18 C17 H17A 109.3 . . ?
N26 C17 H17B 109.3 . . ?
C18 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
N25 C16 N28 113.0(4) . . ?
N25 C16 H16 123.5 . . ?
N28 C16 H16 123.5 . . ?
N41 C26 N44 111.5(6) . . ?
N41 C26 H26 124.3 . . ?
N44 C26 H26 124.3 . . ?
C28 C27 N42 116.1(5) . . ?
C28 C27 H27A 108.3 . . ?
N42 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
N42 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
N36 C21 N33 109.2(4) . . ?
N36 C21 H21 125.4 . . ?
N33 C21 H21 125.4 . . ?
C23 C22 N33 114.1(5) . . ?
C23 C22 H22A 108.7 . . ?
N33 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
N33 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
O3 Cl1 O2 112.8(5) . . ?
O3 Cl1 O4 110.9(4) . . ?
O2 Cl1 O4 109.2(3) . . ?
O3 Cl1 O1 108.3(6) . . ?
O2 Cl1 O1 106.4(3) . . ?
O4 Cl1 O1 109.0(4) . . ?
O5 Cl2 O7 116.8(5) . . ?
O5 Cl2 O8 116.4(4) . . ?
O7 Cl2 O8 114.1(4) . . ?
O5 Cl2 O6 106.1(8) . . ?
O7 Cl2 O6 98.0(5) . . ?
O8 Cl2 O6 101.7(4) . . ?
O9 Cl3 O11 108.1(4) . . ?
O9 Cl3 O10 108.1(4) . . ?
O11 Cl3 O10 108.6(4) . . ?
O9 Cl3 O12 109.8(3) . . ?
O11 Cl3 O12 110.1(3) . . ?
O10 Cl3 O12 112.0(4) . . ?
O15B Cl4 O14B 127.9(18) . . ?
O14 Cl4 O16 111.4(6) . . ?
O15B Cl4 O13 100.5(9) . . ?
O14B Cl4 O13 111.6(13) . . ?
O14 Cl4 O13 107.5(5) . . ?
O16 Cl4 O13 110.0(3) . . ?
O14 Cl4 O15 104.1(4) . . ?
O16 Cl4 O15 110.9(6) . . ?
O13 Cl4 O15 112.9(5) . . ?
O15B Cl4 O16B 105.9(18) . . ?
O14B Cl4 O16B 96(2) . . ?
O13 Cl4 O16B 116.3(18) . . ?
C5 N5 N6 108.4(4) . . ?
C5 N5 C4 130.6(4) . . ?
N6 N5 C4 120.8(4) . . ?
C30 N45 N46 109.3(4) . . ?
C30 N45 C29 129.0(5) . . ?
N46 N45 C29 121.6(4) . . ?
N5 C4 C3 113.7(5) . . ?
N5 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
N5 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N47 N46 N45 106.4(4) . . ?
N45 C29 C28 115.1(5) . . ?
N45 C29 H29A 108.5 . . ?
C28 C29 H29A 108.5 . . ?
N45 C29 H29B 108.5 . . ?
C28 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C2 C3 C4 117.8(6) . . ?
C2 C3 H3A 107.9 . . ?
C4 C3 H3A 107.9 . . ?
C2 C3 H3B 107.9 . . ?
C4 C3 H3B 107.9 . . ?
H3A C3 H3B 107.2 . . ?
N6 N7 N8 110.1(4) . . ?
N7 N6 N5 106.8(4) . . ?
N39 N38 N37 114.2(4) . . ?
N39 N38 C24 122.4(4) . . ?
N37 N38 C24 123.4(4) . . ?
C25 N37 N38 101.6(4) . . ?
N8 C5 N5 108.5(4) . . ?
N8 C5 H5 125.8 . . ?
N5 C5 H5 125.8 . . ?
N38 C24 C23 112.8(5) . . ?
N38 C24 H24A 109.0 . . ?
C23 C24 H24A 109.0 . . ?
N38 C24 H24B 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C5 N8 N7 106.3(4) . . ?
C5 N8 Cu1 129.2(3) . 2_656 ?
N7 N8 Cu1 123.3(3) . 2_656 ?
N38 N39 N40 105.7(4) . . ?
N46 N47 N48 110.1(4) . . ?
N45 C30 N48 108.0(5) . . ?
N45 C30 H30 126.0 . . ?
N48 C30 H30 126.0 . . ?
N37 C25 N40 112.1(4) . . ?
N37 C25 H25 124.0 . . ?
N40 C25 H25 124.0 . . ?
N39 N40 C25 106.4(4) . . ?
N39 N40 Cu2 120.4(3) . 2 ?
C25 N40 Cu2 133.2(3) . 2 ?
C30 N48 N47 106.1(4) . . ?
C30 N48 Cu2 131.8(3) . 2_665 ?
N47 N48 Cu2 122.1(3) . 2_665 ?
C22 C23 C24 120.2(7) . . ?
C22 C23 H23A 107.3 . . ?
C24 C23 H23A 107.3 . . ?
C22 C23 H23B 107.3 . . ?
C24 C23 H23B 107.3 . . ?
H23A C23 H23B 106.9 . . ?
C27 C28 C29 118.0(6) . . ?
C27 C28 H28A 107.8 . . ?
C29 C28 H28A 107.8 . . ?
C27 C28 H28B 107.8 . . ?
C29 C28 H28B 107.8 . . ?
H28A C28 H28B 107.2 . . ?

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
C6 N12 N11 N10 0.2(5) . . . . ?
Cu1 N12 N11 N10 -159.6(3) . . . . ?
N12 N11 N10 N9 -0.3(5) . . . . ?
N11 N10 N9 C6 0.2(5) . . . . ?
N11 N10 N9 C7 178.3(4) . . . . ?
N15 N14 N13 C10 1.1(5) . . . . ?
C9 N14 N13 C10 176.0(4) . . . . ?
N13 N14 N15 N16 -1.1(5) . . . . ?
C9 N14 N15 N16 -176.0(4) . . . . ?
N14 N15 N16 C10 0.7(5) . . . . ?
N14 N15 N16 Cu1 177.7(3) . . . 2_756 ?
C1 N4 N3 N2 -0.6(5) . . . . ?
Cu1 N4 N3 N2 169.8(3) . . . . ?
N4 N3 N2 N1 0.8(6) . . . . ?
N4 N3 N2 C2 -176.3(4) . . . . ?
C1 N1 N2 N3 -0.6(6) . . . . ?
C1 N1 N2 C2 176.4(5) . . . . ?
C11 N20 N19 N18 0.0(5) . . . . ?
Cu1 N20 N19 N18 -178.0(3) . . . . ?
N20 N19 N18 N17 0.0(5) . . . . ?
N20 N19 N18 C12 177.5(4) . . . . ?
C11 N17 N18 N19 0.0(5) . . . . ?
C11 N17 N18 C12 -177.4(4) . . . . ?
C15 N21 N22 N23 1.0(5) . . . . ?
C14 N21 N22 N23 178.4(4) . . . . ?
N21 N22 N23 N24 -1.0(5) . . . . ?
N22 N23 N24 C15 0.7(5) . . . . ?
N22 N23 N24 Cu2 170.5(3) . . . . ?
N29 N30 N31 N32 0.6(5) . . . . ?
N31 N30 N29 C20 0.0(5) . . . . ?
N31 N30 N29 C19 -177.7(4) . . . . ?
N30 N31 N32 C20 -0.9(5) . . . . ?
N30 N31 N32 Cu2 170.1(3) . . . 2_666 ?
C16 N25 N26 N27 0.5(6) . . . . ?
C16 N25 N26 C17 -179.2(5) . . . . ?
N25 N26 N27 N28 -0.9(6) . . . . ?
C17 N26 N27 N28 178.8(4) . . . . ?
C16 N28 N27 N26 0.9(6) . . . . ?
C26 N41 N42 N43 -0.3(6) . . . . ?
C26 N41 N42 C27 -175.3(5) . . . . ?
N41 N42 N43 N44 0.4(6) . . . . ?
C27 N42 N43 N44 175.4(5) . . . . ?
C26 N44 N43 N42 -0.3(5) . . . . ?
Cu2 N44 N43 N42 -175.2(3) . . . . ?
N33 N34 N35 N36 0.8(5) . . . . ?
N34 N35 N36 C21 -0.8(5) . . . . ?
N34 N35 N36 Cu2 -176.2(3) . . . . ?
N35 N34 N33 C21 -0.5(5) . . . . ?
N35 N34 N33 C22 -175.0(4) . . . . ?
N10 N9 C6 N12 -0.1(5) . . . . ?
C7 N9 C6 N12 -177.9(4) . . . . ?
N11 N12 C6 N9 -0.1(5) . . . . ?
Cu1 N12 C6 N9 156.8(3) . . . . ?
C6 N9 C7 C8 -81.4(6) . . . . ?
N10 N9 C7 C8 101.1(5) . . . . ?
N9 C7 C8 C9 -64.2(6) . . . . ?
N15 N14 C9 C8 -28.0(6) . . . . ?
N13 N14 C9 C8 157.5(4) . . . . ?
C7 C8 C9 N14 179.3(4) . . . . ?
N14 N13 C10 N16 -0.6(5) . . . . ?
N15 N16 C10 N13 0.0(6) . . . . ?
Cu1 N16 C10 N13 -176.5(3) 2_756 . . . ?
N3 N2 C2 C3 -121.4(6) . . . . ?
N1 N2 C2 C3 61.8(7) . . . . ?
N2 N1 C1 N4 0.2(6) . . . . ?
N3 N4 C1 N1 0.3(6) . . . . ?
Cu1 N4 C1 N1 -167.8(4) . . . . ?
N18 N17 C11 N20 0.0(5) . . . . ?
N19 N20 C11 N17 0.0(6) . . . . ?
Cu1 N20 C11 N17 177.5(3) . . . . ?
N19 N18 C12 C13 -100.7(5) . . . . ?
N17 N18 C12 C13 76.6(6) . . . . ?
N18 C12 C13 C14 172.6(4) . . . . ?
C15 N21 C14 C13 89.4(6) . . . . ?
N22 N21 C14 C13 -87.4(5) . . . . ?
C12 C13 C14 N21 -171.4(4) . . . . ?
N22 N21 C15 N24 -0.5(5) . . . . ?
C14 N21 C15 N24 -177.6(4) . . . . ?
N23 N24 C15 N21 -0.1(5) . . . . ?
Cu2 N24 C15 N21 -168.7(3) . . . . ?
N31 N32 C20 N29 0.9(5) . . . . ?
Cu2 N32 C20 N29 -168.9(3) 2_666 . . . ?
N30 N29 C20 N32 -0.6(5) . . . . ?
C19 N29 C20 N32 176.8(4) . . . . ?
C20 N29 C19 C18 96.3(6) . . . . ?
N30 N29 C19 C18 -86.6(5) . . . . ?
N29 C19 C18 C17 -70.8(5) . . . . ?
N27 N26 C17 C18 132.2(5) . . . . ?
N25 N26 C17 C18 -48.2(7) . . . . ?
C19 C18 C17 N26 -156.9(4) . . . . ?
N26 N25 C16 N28 0.1(6) . . . . ?
N27 N28 C16 N25 -0.6(6) . . . . ?
N42 N41 C26 N44 0.1(7) . . . . ?
N43 N44 C26 N41 0.1(7) . . . . ?
Cu2 N44 C26 N41 173.6(4) . . . . ?
N43 N42 C27 C28 128.0(6) . . . . ?
N41 N42 C27 C28 -57.4(8) . . . . ?
N35 N36 C21 N33 0.4(5) . . . . ?
Cu2 N36 C21 N33 175.8(3) . . . . ?
N34 N33 C21 N36 0.0(6) . . . . ?
C22 N33 C21 N36 174.0(4) . . . . ?
C21 N33 C22 C23 89.9(7) . . . . ?
N34 N33 C22 C23 -96.8(7) . . . . ?
C5 N5 C4 C3 -69.1(7) . . . . ?
N6 N5 C4 C3 116.4(6) . . . . ?
C30 N45 N46 N47 -0.1(7) . . . . ?
C29 N45 N46 N47 -177.3(5) . . . . ?
C30 N45 C29 C28 78.7(8) . . . . ?
N46 N45 C29 C28 -104.6(7) . . . . ?
N2 C2 C3 C4 69.6(8) . . . . ?
N5 C4 C3 C2 -69.1(7) . . . . ?
N8 N7 N6 N5 0.1(6) . . . . ?
C5 N5 N6 N7 -0.7(6) . . . . ?
C4 N5 N6 N7 175.0(4) . . . . ?
N39 N38 N37 C25 -0.3(6) . . . . ?
C24 N38 N37 C25 -178.2(4) . . . . ?
N6 N5 C5 N8 1.0(5) . . . . ?
C4 N5 C5 N8 -174.1(5) . . . . ?
N39 N38 C24 C23 134.5(6) . . . . ?
N37 N38 C24 C23 -47.8(7) . . . . ?
N5 C5 N8 N7 -0.9(5) . . . . ?
N5 C5 N8 Cu1 166.3(3) . . . 2_656 ?
N6 N7 N8 C5 0.5(6) . . . . ?
N6 N7 N8 Cu1 -167.7(3) . . . 2_656 ?
N37 N38 N39 N40 0.8(5) . . . . ?
C24 N38 N39 N40 178.7(4) . . . . ?
N45 N46 N47 N48 0.1(7) . . . . ?
N46 N45 C30 N48 0.0(6) . . . . ?
C29 N45 C30 N48 177.0(5) . . . . ?
N38 N37 C25 N40 -0.3(6) . . . . ?
N38 N39 N40 C25 -0.9(5) . . . . ?
N38 N39 N40 Cu2 177.4(3) . . . 2 ?
N37 C25 N40 N39 0.8(6) . . . . ?
N37 C25 N40 Cu2 -177.2(4) . . . 2 ?
N45 C30 N48 N47 0.0(6) . . . . ?
N45 C30 N48 Cu2 -180.0(3) . . . 2_665 ?
N46 N47 N48 C30 0.0(7) . . . . ?
N46 N47 N48 Cu2 179.9(4) . . . 2_665 ?
N33 C22 C23 C24 74.9(8) . . . . ?
N38 C24 C23 C22 -72.1(8) . . . . ?
N42 C27 C28 C29 -71.9(8) . . . . ?
N45 C29 C28 C27 73.7(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
? ? ? ? ? ? ? ?

_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         2.982
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.116

_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_mx035
_database_code_depnum_ccdc_archive 'CCDC 1816637'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Jan 25 17:27:59 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,3-di-1,tetrazolyl-propane monohydrate
;
_chemical_name_common            '1,3-di-1,tetrazolyl-propane monohydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H8 N8, H2 O'
_chemical_formula_sum            'C5 H10 N8 O'
_chemical_formula_weight         198.21

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'



_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+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.2283(10)
_cell_length_b                   10.9670(12)
_cell_length_c                   16.3177(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1830.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3992
_cell_measurement_theta_min      4.6890
_cell_measurement_theta_max      31.5420

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.380
_exptl_absorpt_coefficient_mu    0.111
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.39171
_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    1.439
_exptl_crystal_F_000             832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            13404
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.397
_diffrn_reflns_theta_max         25.996
_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             1792
_reflns_number_gt                1485
_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)+(0.0362P)²+0.4291P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_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         1792
_refine_ls_number_parameters     167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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      -0.0286796000
_diffrn_orient_matrix_UB_12      0.0127544000
_diffrn_orient_matrix_UB_13      0.0386540000
_diffrn_orient_matrix_UB_21      0.0582642000
_diffrn_orient_matrix_UB_22      -0.0187701000
_diffrn_orient_matrix_UB_23      0.0199060000
_diffrn_orient_matrix_UB_31      0.0240221000
_diffrn_orient_matrix_UB_32      0.0605873000
_diffrn_orient_matrix_UB_33      -0.0018944000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -37.00   53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057  -57.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -23.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057  -99.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -24.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057  -99.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
  4 omega   57.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057   57.0000  -90.0000 44

#__ type_ start__ end____ width___ exp.time_
  5 omega   -1.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057   77.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega    6.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   77.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  -63.00  -38.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557 -179.0000 -150.0000 25

;



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'
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
N1 N 0.14088(9) 0.41688(9) 0.08104(6) 0.0223(2) Uani 1 1 d . . . . .
N2 N 0.08396(11) 0.49888(9) 0.13143(6) 0.0289(3) Uani 1 1 d . . . . .
N3 N -0.04055(11) 0.48444(10) 0.12332(6) 0.0316(3) Uani 1 1 d . . . . .
N4 N -0.06663(10) 0.39352(10) 0.06837(7) 0.0306(3) Uani 1 1 d . . . . .
N5 N 0.37145(9) 0.22912(8) 0.26834(6) 0.0222(2) Uani 1 1 d . . . . .
N6 N 0.50105(10) 0.21364(10) 0.27476(6) 0.0285(3) Uani 1 1 d . . . . .
N7 N 0.51876(10) 0.11925(10) 0.32133(7) 0.0331(3) Uani 1 1 d . . . . .
N8 N 0.40228(11) 0.07202(10) 0.34536(7) 0.0343(3) Uani 1 1 d . . . . .
C1 C 0.04740(12) 0.35365(12) 0.04367(8) 0.0265(3) Uani 1 1 d . . . . .
C2 C 0.28292(12) 0.40520(13) 0.07481(8) 0.0283(3) Uani 1 1 d . . . . .
C3 C 0.33354(13) 0.30168(12) 0.12788(7) 0.0257(3) Uani 1 1 d . . . . .
C4 C 0.31674(12) 0.32780(11) 0.21865(8) 0.0247(3) Uani 1 1 d . . . . .
C5 C 0.31300(13) 0.14219(12) 0.31145(8) 0.0283(3) Uani 1 1 d . . . . .
O1 O 0.65774(11) 0.34820(10) 0.06723(8) 0.0470(3) Uani 1 1 d . . . . .
H3B H 0.2886(13) 0.2279(13) 0.1133(9) 0.032(4) Uiso 1 1 d . . . . .
H3A H 0.4250(15) 0.2917(13) 0.1173(8) 0.031(4) Uiso 1 1 d . . . . .
H4A H 0.3620(13) 0.4019(13) 0.2335(9) 0.033(4) Uiso 1 1 d . . . . .
H5 H 0.2222(15) 0.1319(13) 0.3156(8) 0.035(4) Uiso 1 1 d . . . . .
H2B H 0.3003(13) 0.3905(13) 0.0175(9) 0.033(4) Uiso 1 1 d . . . . .
H4B H 0.2262(14) 0.3338(12) 0.2333(8) 0.029(4) Uiso 1 1 d . . . . .
H1 H 0.0656(13) 0.2887(13) 0.0069(9) 0.034(4) Uiso 1 1 d . . . . .
H2A H 0.3203(14) 0.4849(14) 0.0922(9) 0.038(4) Uiso 1 1 d . . . . .
H11 H 0.632(2) 0.4156(19) 0.0916(13) 0.072(6) Uiso 1 1 d . . . . .
H12 H 0.741(2) 0.3548(17) 0.0628(11) 0.063(6) 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
N1 C1 1.3293(16) . ?
N1 N2 1.3505(14) . ?
N1 C2 1.4621(16) . ?
N2 N3 1.2902(15) . ?
N3 N4 1.3673(16) . ?
N4 C1 1.3092(17) . ?
N5 C5 1.3271(15) . ?
N5 N6 1.3405(14) . ?
N5 C4 1.4635(15) . ?
N6 N7 1.2969(15) . ?
N7 N8 1.3570(15) . ?
N8 C5 1.3162(17) . ?
C1 H1 0.950(15) . ?
C2 C3 1.5188(18) . ?
C2 H2B 0.966(15) . ?
C2 H2A 0.995(15) . ?
C3 C4 1.5184(17) . ?
C3 H3B 0.961(15) . ?
C3 H3A 0.957(15) . ?
C4 H4A 0.966(14) . ?
C4 H4B 0.959(14) . ?
C5 H5 0.938(15) . ?
O1 H11 0.88(2) . ?
O1 H12 0.86(2) . ?

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
C1 N1 N2 108.46(10) . . ?
C1 N1 C2 129.58(11) . . ?
N2 N1 C2 121.94(10) . . ?
N3 N2 N1 106.34(10) . . ?
N2 N3 N4 110.45(10) . . ?
C1 N4 N3 105.77(10) . . ?
C5 N5 N6 108.24(10) . . ?
C5 N5 C4 130.74(10) . . ?
N6 N5 C4 121.00(9) . . ?
N7 N6 N5 106.56(10) . . ?
N6 N7 N8 110.57(10) . . ?
C5 N8 N7 105.34(10) . . ?
N4 C1 N1 108.98(11) . . ?
N4 C1 H1 128.3(8) . . ?
N1 C1 H1 122.7(8) . . ?
N1 C2 C3 111.38(10) . . ?
N1 C2 H2B 105.3(8) . . ?
C3 C2 H2B 111.4(9) . . ?
N1 C2 H2A 106.6(8) . . ?
C3 C2 H2A 111.3(9) . . ?
H2B C2 H2A 110.7(12) . . ?
C4 C3 C2 112.12(11) . . ?
C4 C3 H3B 110.3(8) . . ?
C2 C3 H3B 109.0(8) . . ?
C4 C3 H3A 107.9(8) . . ?
C2 C3 H3A 108.4(8) . . ?
H3B C3 H3A 109.1(11) . . ?
N5 C4 C3 110.95(10) . . ?
N5 C4 H4A 107.4(8) . . ?
C3 C4 H4A 110.4(8) . . ?
N5 C4 H4B 106.4(8) . . ?
C3 C4 H4B 111.5(8) . . ?
H4A C4 H4B 110.0(11) . . ?
N8 C5 N5 109.29(11) . . ?
N8 C5 H5 125.9(9) . . ?
N5 C5 H5 124.8(9) . . ?
H11 O1 H12 105.3(17) . . ?

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 -0.39(13) . . . . ?
C2 N1 N2 N3 -179.04(10) . . . . ?
N1 N2 N3 N4 0.23(13) . . . . ?
N2 N3 N4 C1 0.02(14) . . . . ?
C5 N5 N6 N7 -0.29(13) . . . . ?
C4 N5 N6 N7 -179.20(10) . . . . ?
N5 N6 N7 N8 0.28(14) . . . . ?
N6 N7 N8 C5 -0.16(14) . . . . ?
N3 N4 C1 N1 -0.27(14) . . . . ?
N2 N1 C1 N4 0.41(14) . . . . ?
C2 N1 C1 N4 178.93(11) . . . . ?
C1 N1 C2 C3 -80.73(16) . . . . ?
N2 N1 C2 C3 97.61(14) . . . . ?
N1 C2 C3 C4 -67.21(14) . . . . ?
C5 N5 C4 C3 -106.35(14) . . . . ?
N6 N5 C4 C3 72.27(14) . . . . ?
C2 C3 C4 N5 -177.51(10) . . . . ?
N7 N8 C5 N5 -0.03(14) . . . . ?
N6 N5 C5 N8 0.20(14) . . . . ?
C4 N5 C5 N8 178.96(11) . . . . ?

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
O1 H11 N8 0.88(2) 2.03(2) 2.9046(16) 172.1(19) 4_655
O1 H12 N4 0.86(2) 2.01(2) 2.8627(16) 169.5(18) 1_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         0.190
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.035

_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_vv797
_database_code_depnum_ccdc_archive 'CCDC 1816634'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_vrf_PLAT112_vv797               
; 
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem        m      100 %Fit 
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem        n      100 %Fit  

RESPONSE: The disorder in both dinitramide anions cannot be solved 
in the probably correct space group Ibam. 
;


_vrf_PLAT113_vv797               
; 
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group     Ibam Check   

RESPONSE: The disorder in both dinitramide anions cannot be solved 
in the probably correct space group Ibam.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,3-ditetrazol-1-ylpropane) copper(II) dinitramide
;
_chemical_name_common            
'tris(1,3-ditetrazol-1-ylpropane) copper(II) dinitramide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Cu N24, 2(N3 O4)'
_chemical_formula_sum            'C15 H24 Cu N30 O8'
_chemical_formula_weight         816.18

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15
_symmetry_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                   27.0187(10)
_cell_length_b                   18.5080(6)
_cell_length_c                   15.4569(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.9100(10)
_cell_angle_gamma                90
_cell_volume                     6338.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.6355
_cell_measurement_theta_max      27.4587

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.784
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.7098
_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    1.711
_exptl_crystal_F_000             3336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      103(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            46253
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.515
_diffrn_reflns_theta_max         26.000
_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             6221
_reflns_number_gt                5166
_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)+(0.0339P)²+9.8138P] 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         6221
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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'
O O 0.0106 0.0060 '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
O300 O -0.24998(8) 0.38360(8) -0.38215(12) 0.0328(4) Uani 1 1 d . . . . .
N300 N -0.24992(11) 0.39739(10) -0.30694(16) 0.0357(5) Uani 1 1 d . . . . .
O301 O -0.19702(13) 0.43589(17) -0.2359(2) 0.0289(7) Uani 0.5 1 d . . P A 1
N301 N -0.28159(15) 0.37281(19) -0.2767(3) 0.0218(7) Uani 0.5 1 d . . P A 1
O304 O -0.2922(2) 0.3435(2) -0.1525(4) 0.0439(11) Uani 0.5 1 d . . P A 1
O306 O -0.19967(17) 0.34684(19) -0.1088(3) 0.0316(8) Uani 0.5 1 d . . P A 1
N302 N -0.21834(15) 0.37278(18) -0.2137(3) 0.0215(7) Uani 0.5 1 d . . P A 2
O302 O -0.30295(13) 0.43565(18) -0.3418(2) 0.0295(7) Uani 0.5 1 d . . P A 2
O303 O -0.30031(17) 0.34670(19) -0.2096(3) 0.0318(8) Uani 0.5 1 d . . P A 2
O305 O -0.2077(2) 0.3437(2) -0.0680(3) 0.0456(12) Uani 0.5 1 d . . P A 2
O201 O -0.24998(7) -0.21421(9) -0.82111(13) 0.0381(4) Uani 1 1 d . . . . .
O202 O -0.25002(8) -0.09397(9) -0.62185(12) 0.0332(4) Uani 1 1 d . . . . .
N200 N -0.24995(10) -0.16157(10) -0.77421(15) 0.0338(5) Uani 1 1 d . . . . .
N202 N -0.28214(14) -0.07998(18) -0.7117(3) 0.0182(7) Uani 0.5 1 d . . P B 1
O205 O -0.31767(12) -0.02849(15) -0.7442(2) 0.0230(6) Uani 0.5 1 d . . P B 1
N209 N -0.2920(3) -0.1256(5) -0.7918(5) 0.0199(13) Uani 0.5 1 d . . P B 1
O217 O -0.1892(2) -0.1393(4) -0.6982(6) 0.0312(14) Uani 0.5 1 d . . P B 1
O211 O -0.3106(2) -0.1391(4) -0.8196(5) 0.0295(13) Uani 0.5 1 d . . P B 2
N218 N -0.2079(3) -0.1257(4) -0.7080(6) 0.0188(12) Uani 0.5 1 d . . P B 2
O207 O -0.18226(12) -0.02839(15) -0.6088(2) 0.0231(6) Uani 0.5 1 d . . P B 2
N203 N -0.21775(14) -0.08014(18) -0.6471(2) 0.0178(7) Uani 0.5 1 d . . P B 2
Cu1 Cu 0.0000 0.0000 0.0000 0.00944(8) Uani 1 2 d S . P . .
Cu2 Cu 0.0000 0.5000 -0.5000 0.00944(8) Uani 1 2 d S . P . .
N12 N 0.05338(7) 0.10886(8) 0.02189(12) 0.0150(3) Uani 1 1 d . . . . .
N24 N -0.06345(7) 0.47498(8) -0.47612(11) 0.0116(3) Uani 1 1 d . . . . .
N4 N -0.06347(7) 0.02505(8) -0.15074(11) 0.0115(3) Uani 1 1 d . . . . .
N13 N 0.09844(7) 0.30919(8) -0.29485(11) 0.0132(3) Uani 1 1 d . . . . .
N9 N 0.09841(7) 0.19080(8) -0.00818(11) 0.0135(3) Uani 1 1 d . . . . .
N16 N 0.05334(7) 0.39112(8) -0.41521(12) 0.0151(3) Uani 1 1 d . . . . .
N17 N -0.09484(7) 0.35999(8) -0.75553(11) 0.0131(3) Uani 1 1 d . . . . .
N2 N -0.11042(7) 0.08513(9) -0.29712(12) 0.0175(3) Uani 1 1 d . . . . .
N5 N -0.09489(7) 0.14005(8) 0.06582(11) 0.0133(3) Uani 1 1 d . . . . .
N22 N -0.11033(7) 0.41485(9) -0.42363(12) 0.0170(3) Uani 1 1 d . . . . .
C7 C 0.09087(8) 0.25005(9) -0.15921(14) 0.0129(4) Uani 1 1 d . . . . .
H7A H 0.0647 0.2089 -0.2016 0.015 Uiso 1 1 calc R U . . .
H7B H 0.0648 0.2914 -0.1690 0.015 Uiso 1 1 calc R U . . .
N21 N -0.13987(7) 0.47691(8) -0.46887(11) 0.0121(3) Uani 1 1 d . . . . .
N1 N -0.13998(7) 0.02307(8) -0.31096(11) 0.0119(3) Uani 1 1 d . . . . .
N8 N -0.04583(7) 0.06032(8) 0.04335(11) 0.0117(3) Uani 1 1 d . . . . .
N20 N -0.04587(7) 0.43970(8) -0.63502(11) 0.0120(3) Uani 1 1 d . . . . .
N6 N -0.08066(7) 0.08627(8) 0.13557(12) 0.0174(3) Uani 1 1 d . . . . .
N19 N -0.05128(7) 0.46169(8) -0.72416(11) 0.0161(3) Uani 1 1 d . . . . .
N7 N -0.05133(7) 0.03836(8) 0.12138(12) 0.0163(3) Uani 1 1 d . . . . .
N10 N 0.08060(8) 0.22205(9) 0.04830(14) 0.0238(4) Uani 1 1 d . . . . .
N18 N -0.08071(8) 0.41375(9) -0.79691(12) 0.0180(3) Uani 1 1 d . . . . .
N14 N 0.08070(8) 0.27792(9) -0.38691(12) 0.0233(4) Uani 1 1 d . . . . .
N3 N -0.06392(7) 0.08625(8) -0.19977(12) 0.0166(3) Uani 1 1 d . . . . .
C11 C -0.12966(8) 0.29765(10) -0.82186(15) 0.0167(4) Uani 1 1 d . . . . .
H11A H -0.1651 0.3148 -0.8904 0.020 Uiso 1 1 calc R U . . .
H11B H -0.1445 0.2691 -0.7869 0.020 Uiso 1 1 calc R U . . .
C4 C -0.12959(8) 0.20235(10) 0.06267(14) 0.0169(4) Uani 1 1 d . . . . .
H4A H -0.1650 0.1852 0.0603 0.020 Uiso 1 1 calc R U . . .
H4B H -0.1444 0.2309 -0.0020 0.020 Uiso 1 1 calc R U . . .
C15 C -0.24991(8) 0.46735(10) -0.57597(14) 0.0144(4) Uani 1 1 d . . . . .
H15A H -0.2499 0.4139 -0.5734 0.017 Uiso 1 1 calc R U . . .
H15B H -0.2499 0.4821 -0.6375 0.017 Uiso 1 1 calc R U . . .
N23 N -0.06396(7) 0.41382(8) -0.42825(12) 0.0163(3) Uani 1 1 d . . . . .
C8 C 0.13163(8) 0.27072(10) -0.19392(14) 0.0150(4) Uani 1 1 d . . . . .
H8A H 0.1648 0.3018 -0.1393 0.018 Uiso 1 1 calc R U . . .
H8B H 0.1498 0.2265 -0.2006 0.018 Uiso 1 1 calc R U . . .
C6 C 0.13168(8) 0.22914(10) -0.04271(14) 0.0153(4) Uani 1 1 d . . . . .
H6A H 0.1648 0.1979 -0.0311 0.018 Uiso 1 1 calc R U . . .
H6B H 0.1500 0.2733 0.0004 0.018 Uiso 1 1 calc R U . . .
N15 N 0.05373(8) 0.32754(9) -0.45876(12) 0.0211(4) Uani 1 1 d . . . . .
C1 C -0.11104(8) -0.01310(10) -0.22097(13) 0.0134(4) Uani 1 1 d . . . . .
H1 H -0.1225 -0.0585 -0.2091 0.016 Uiso 1 1 calc R U . . .
C13 C -0.11109(8) 0.51303(10) -0.50113(14) 0.0130(4) Uani 1 1 d . . . . .
H13 H -0.1227 0.5584 -0.5362 0.016 Uiso 1 1 calc R U . . .
N11 N 0.05363(8) 0.17249(9) 0.06609(13) 0.0221(4) Uani 1 1 d . . . . .
C10 C -0.07331(8) 0.37655(10) -0.65656(14) 0.0136(4) Uani 1 1 d . . . . .
H10 H -0.0770 0.3480 -0.6094 0.016 Uiso 1 1 calc R U . . .
C3 C -0.07322(8) 0.12352(10) 0.00999(14) 0.0138(4) Uani 1 1 d . . . . .
H3 H -0.0768 0.1521 -0.0444 0.017 Uiso 1 1 calc R U . . .
C12 C -0.09034(9) 0.25006(10) -0.84028(16) 0.0196(4) Uani 1 1 d . . . . .
H12A H -0.0641 0.2193 -0.7776 0.024 Uiso 1 1 calc R U . . .
H12B H -0.0641 0.2809 -0.8505 0.024 Uiso 1 1 calc R U . . .
C14 C -0.19446(8) 0.49676(10) -0.47571(14) 0.0145(4) Uani 1 1 d . . . . .
H14A H -0.1973 0.5500 -0.4746 0.017 Uiso 1 1 calc R U . . .
H14B H -0.1922 0.4771 -0.4139 0.017 Uiso 1 1 calc R U . . .
C2 C -0.19447(8) 0.00326(10) -0.41323(14) 0.0146(4) Uani 1 1 d . . . . .
H2A H -0.1973 -0.0500 -0.4201 0.017 Uiso 1 1 calc R U . . .
H2B H -0.1922 0.0229 -0.4704 0.017 Uiso 1 1 calc R U . . .
C5 C 0.08148(9) 0.12224(10) -0.02282(15) 0.0194(4) Uani 1 1 d . . . . .
H5 H 0.0886 0.0879 -0.0602 0.023 Uiso 1 1 calc R U . . .
C9 C 0.08155(9) 0.37780(10) -0.31408(15) 0.0197(4) Uani 1 1 d . . . . .
H9 H 0.0888 0.4122 -0.2624 0.024 Uiso 1 1 calc R U . . .
N303 N -0.25004(11) 0.35494(9) -0.16976(15) 0.0279(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
O300 N300 1.189(2) . ?
N300 N302 1.267(4) . ?
N300 N301 1.271(4) . ?
N300 O301 1.400(3) . ?
N300 O302 1.401(3) . ?
N301 N303 1.399(4) . ?
O304 N303 1.328(4) . ?
O306 N303 1.138(4) . ?
N302 N303 1.403(4) . ?
O303 N303 1.136(4) . ?
O305 N303 1.329(4) . ?
O201 N200 1.214(2) . ?
O202 N203 1.170(4) . ?
O202 N202 1.170(4) . ?
N200 N218 1.203(9) . ?
N200 N209 1.206(9) . ?
N200 O211 1.425(7) . ?
N200 O217 1.427(7) . ?
N202 O205 1.237(4) . ?
N202 N209 1.392(8) . ?
N218 N203 1.397(8) . ?
O207 N203 1.240(4) . ?
Cu1 N4 2.0028(14) . ?
Cu1 N4 2.0028(14) 5 ?
Cu1 N8 2.0439(14) 5 ?
Cu1 N8 2.0439(14) . ?
Cu1 N12 2.3865(15) 5 ?
Cu1 N12 2.3865(15) . ?
Cu2 N24 2.0034(14) 5_564 ?
Cu2 N24 2.0035(14) . ?
Cu2 N20 2.0437(14) 5_564 ?
Cu2 N20 2.0437(14) . ?
Cu2 N16 2.3862(15) 5_564 ?
Cu2 N16 2.3862(15) . ?
N12 C5 1.310(2) . ?
N12 N11 1.360(2) . ?
N24 C13 1.316(2) . ?
N24 N23 1.357(2) . ?
N4 C1 1.316(2) . ?
N4 N3 1.359(2) . ?
N13 C9 1.324(2) . ?
N13 N14 1.345(2) . ?
N13 C8 1.464(2) . ?
N9 C5 1.324(2) . ?
N9 N10 1.345(2) . ?
N9 C6 1.465(2) . ?
N16 C9 1.312(2) . ?
N16 N15 1.359(2) . ?
N17 C10 1.324(2) . ?
N17 N18 1.351(2) . ?
N17 C11 1.471(2) . ?
N2 N3 1.296(2) . ?
N2 N1 1.344(2) . ?
N5 C3 1.326(2) . ?
N5 N6 1.351(2) . ?
N5 C4 1.469(2) . ?
N22 N23 1.295(2) . ?
N22 N21 1.344(2) . ?
C7 C8 1.524(2) . ?
C7 C6 1.528(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N21 C13 1.321(2) . ?
N21 C14 1.464(2) . ?
N1 C1 1.323(2) . ?
N1 C2 1.462(2) . ?
N8 C3 1.321(2) . ?
N8 N7 1.359(2) . ?
N20 C10 1.320(2) . ?
N20 N19 1.362(2) . ?
N6 N7 1.289(2) . ?
N19 N18 1.289(2) . ?
N10 N11 1.295(2) . ?
N14 N15 1.297(2) . ?
C11 C12 1.527(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C4 C12 1.528(3) 1_556 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C15 C14 1.512(2) . ?
C15 C2 1.515(3) 7_454 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C1 H1 0.9500 . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
C12 C4 1.528(3) 1_554 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C2 C15 1.515(3) 7_454 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 H5 0.9500 . ?
C9 H9 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
O300 N300 N302 131.2(3) . . ?
O300 N300 N301 131.1(2) . . ?
O300 N300 O301 107.8(2) . . ?
N301 N300 O301 119.6(2) . . ?
O300 N300 O302 107.7(2) . . ?
N302 N300 O302 119.6(2) . . ?
N300 N301 N303 115.9(3) . . ?
N300 N302 N303 115.8(3) . . ?
N218 N200 O201 128.9(3) . . ?
N209 N200 O201 129.0(3) . . ?
N218 N200 O211 121.1(4) . . ?
O201 N200 O211 109.4(3) . . ?
N209 N200 O217 121.1(4) . . ?
O201 N200 O217 109.3(3) . . ?
O202 N202 O205 121.9(3) . . ?
O202 N202 N209 123.8(5) . . ?
O205 N202 N209 113.4(4) . . ?
N200 N209 N202 117.3(5) . . ?
N200 N218 N203 117.1(5) . . ?
O202 N203 O207 122.0(3) . . ?
O202 N203 N218 123.9(4) . . ?
O207 N203 N218 113.3(4) . . ?
N4 Cu1 N4 180.0 . 5 ?
N4 Cu1 N8 91.20(6) . 5 ?
N4 Cu1 N8 88.80(6) 5 5 ?
N4 Cu1 N8 88.80(6) . . ?
N4 Cu1 N8 91.21(6) 5 . ?
N8 Cu1 N8 180.0 5 . ?
N4 Cu1 N12 89.13(6) . 5 ?
N4 Cu1 N12 90.87(6) 5 5 ?
N8 Cu1 N12 85.57(5) 5 5 ?
N8 Cu1 N12 94.43(5) . 5 ?
N4 Cu1 N12 90.87(6) . . ?
N4 Cu1 N12 89.13(6) 5 . ?
N8 Cu1 N12 94.43(5) 5 . ?
N8 Cu1 N12 85.57(5) . . ?
N12 Cu1 N12 180.00(8) 5 . ?
N24 Cu2 N24 180.0 5_564 . ?
N24 Cu2 N20 88.80(6) 5_564 5_564 ?
N24 Cu2 N20 91.20(6) . 5_564 ?
N24 Cu2 N20 91.20(6) 5_564 . ?
N24 Cu2 N20 88.80(6) . . ?
N20 Cu2 N20 180.00(7) 5_564 . ?
N24 Cu2 N16 90.87(6) 5_564 5_564 ?
N24 Cu2 N16 89.13(6) . 5_564 ?
N20 Cu2 N16 85.55(5) 5_564 5_564 ?
N20 Cu2 N16 94.45(5) . 5_564 ?
N24 Cu2 N16 89.13(6) 5_564 . ?
N24 Cu2 N16 90.87(6) . . ?
N20 Cu2 N16 94.45(5) 5_564 . ?
N20 Cu2 N16 85.55(5) . . ?
N16 Cu2 N16 180.00(9) 5_564 . ?
C5 N12 N11 105.29(15) . . ?
C5 N12 Cu1 124.79(12) . . ?
N11 N12 Cu1 129.15(12) . . ?
C13 N24 N23 107.04(14) . . ?
C13 N24 Cu2 128.19(12) . . ?
N23 N24 Cu2 124.77(11) . . ?
C1 N4 N3 107.11(14) . . ?
C1 N4 Cu1 128.12(12) . . ?
N3 N4 Cu1 124.76(11) . . ?
C9 N13 N14 107.87(15) . . ?
C9 N13 C8 128.88(15) . . ?
N14 N13 C8 123.24(15) . . ?
C5 N9 N10 107.82(15) . . ?
C5 N9 C6 128.77(16) . . ?
N10 N9 C6 123.39(15) . . ?
C9 N16 N15 105.29(15) . . ?
C9 N16 Cu2 124.71(12) . . ?
N15 N16 Cu2 129.26(11) . . ?
C10 N17 N18 108.68(15) . . ?
C10 N17 C11 132.04(16) . . ?
N18 N17 C11 119.28(14) . . ?
N3 N2 N1 106.93(14) . . ?
C3 N5 N6 108.62(15) . . ?
C3 N5 C4 132.09(16) . . ?
N6 N5 C4 119.28(14) . . ?
N23 N22 N21 106.79(14) . . ?
C8 C7 C6 107.39(14) . . ?
C8 C7 H7A 110.2 . . ?
C6 C7 H7A 110.2 . . ?
C8 C7 H7B 110.2 . . ?
C6 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C13 N21 N22 109.06(15) . . ?
C13 N21 C14 129.23(16) . . ?
N22 N21 C14 121.71(15) . . ?
C1 N1 N2 108.98(15) . . ?
C1 N1 C2 129.32(16) . . ?
N2 N1 C2 121.68(14) . . ?
C3 N8 N7 106.83(14) . . ?
C3 N8 Cu1 131.67(12) . . ?
N7 N8 Cu1 121.48(11) . . ?
C10 N20 N19 106.84(14) . . ?
C10 N20 Cu2 131.74(12) . . ?
N19 N20 Cu2 121.40(11) . . ?
N7 N6 N5 107.02(14) . . ?
N18 N19 N20 109.41(14) . . ?
N6 N7 N8 109.61(14) . . ?
N11 N10 N9 106.68(15) . . ?
N19 N18 N17 107.12(14) . . ?
N15 N14 N13 106.66(15) . . ?
N2 N3 N4 109.12(14) . . ?
N17 C11 C12 110.30(15) . . ?
N17 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N17 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N5 C4 C12 110.47(15) . 1_556 ?
N5 C4 H4A 109.6 . . ?
C12 C4 H4A 109.6 1_556 . ?
N5 C4 H4B 109.6 . . ?
C12 C4 H4B 109.6 1_556 . ?
H4A C4 H4B 108.1 . . ?
C14 C15 C2 108.80(14) . 7_454 ?
C14 C15 H15A 109.9 . . ?
C2 C15 H15A 109.9 7_454 . ?
C14 C15 H15B 109.9 . . ?
C2 C15 H15B 109.9 7_454 . ?
H15A C15 H15B 108.3 . . ?
N22 N23 N24 109.27(15) . . ?
N13 C8 C7 111.83(14) . . ?
N13 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
N13 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N9 C6 C7 111.87(14) . . ?
N9 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
N9 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N14 N15 N16 110.42(15) . . ?
N4 C1 N1 107.85(16) . . ?
N4 C1 H1 126.1 . . ?
N1 C1 H1 126.1 . . ?
N24 C13 N21 107.84(16) . . ?
N24 C13 H13 126.1 . . ?
N21 C13 H13 126.1 . . ?
N10 N11 N12 110.39(15) . . ?
N20 C10 N17 107.95(15) . . ?
N20 C10 H10 126.0 . . ?
N17 C10 H10 126.0 . . ?
N8 C3 N5 107.92(15) . . ?
N8 C3 H3 126.0 . . ?
N5 C3 H3 126.0 . . ?
C11 C12 C4 110.52(15) . 1_554 ?
C11 C12 H12A 109.5 . . ?
C4 C12 H12A 109.5 1_554 . ?
C11 C12 H12B 109.5 . . ?
C4 C12 H12B 109.5 1_554 . ?
H12A C12 H12B 108.1 . . ?
N21 C14 C15 110.49(14) . . ?
N21 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
N21 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
N1 C2 C15 110.53(14) . 7_454 ?
N1 C2 H2A 109.5 . . ?
C15 C2 H2A 109.5 7_454 . ?
N1 C2 H2B 109.5 . . ?
C15 C2 H2B 109.5 7_454 . ?
H2A C2 H2B 108.1 . . ?
N12 C5 N9 109.82(16) . . ?
N12 C5 H5 125.1 . . ?
N9 C5 H5 125.1 . . ?
N16 C9 N13 109.76(16) . . ?
N16 C9 H9 125.1 . . ?
N13 C9 H9 125.1 . . ?
O306 N303 O304 124.7(3) . . ?
O303 N303 O305 124.9(3) . . ?
O306 N303 N301 129.9(3) . . ?
O304 N303 N301 105.2(3) . . ?
O303 N303 N302 129.8(3) . . ?
O305 N303 N302 105.1(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
O300 N300 N301 N303 134.7(3) . . . . ?
N302 N300 N301 N303 9.3(3) . . . . ?
O301 N300 N301 N303 -29.6(4) . . . . ?
O302 N300 N301 N303 -133.7(3) . . . . ?
O300 N300 N302 N303 -134.6(3) . . . . ?
N301 N300 N302 N303 -9.3(3) . . . . ?
O301 N300 N302 N303 133.5(3) . . . . ?
O302 N300 N302 N303 29.2(4) . . . . ?
N203 O202 N202 O205 -118.0(4) . . . . ?
N203 O202 N202 N209 74.0(5) . . . . ?
N218 N200 N209 N202 -25.3(8) . . . . ?
O201 N200 N209 N202 163.9(4) . . . . ?
O211 N200 N209 N202 155(3) . . . . ?
O217 N200 N209 N202 -25.2(9) . . . . ?
O202 N202 N209 N200 -34.7(9) . . . . ?
O205 N202 N209 N200 156.3(5) . . . . ?
N209 N200 N218 N203 25.5(8) . . . . ?
O201 N200 N218 N203 -163.7(3) . . . . ?
O211 N200 N218 N203 25.5(9) . . . . ?
O217 N200 N218 N203 -154(3) . . . . ?
N202 O202 N203 O207 117.4(4) . . . . ?
N202 O202 N203 N218 -73.7(5) . . . . ?
N200 N218 N203 O202 34.2(8) . . . . ?
N200 N218 N203 O207 -156.1(5) . . . . ?
N23 N22 N21 C13 0.28(19) . . . . ?
N23 N22 N21 C14 -178.83(15) . . . . ?
N3 N2 N1 C1 0.3(2) . . . . ?
N3 N2 N1 C2 -178.66(15) . . . . ?
C3 N5 N6 N7 -0.3(2) . . . . ?
C4 N5 N6 N7 179.11(15) . . . . ?
C10 N20 N19 N18 -0.1(2) . . . . ?
Cu2 N20 N19 N18 178.41(12) . . . . ?
N5 N6 N7 N8 0.35(19) . . . . ?
C3 N8 N7 N6 -0.3(2) . . . . ?
Cu1 N8 N7 N6 178.37(12) . . . . ?
C5 N9 N10 N11 -0.1(2) . . . . ?
C6 N9 N10 N11 -178.96(16) . . . . ?
N20 N19 N18 N17 0.1(2) . . . . ?
C10 N17 N18 N19 0.0(2) . . . . ?
C11 N17 N18 N19 179.11(15) . . . . ?
C9 N13 N14 N15 -0.2(2) . . . . ?
C8 N13 N14 N15 -178.98(16) . . . . ?
N1 N2 N3 N4 -0.07(19) . . . . ?
C1 N4 N3 N2 -0.2(2) . . . . ?
Cu1 N4 N3 N2 178.87(12) . . . . ?
C10 N17 C11 C12 -108.8(2) . . . . ?
N18 N17 C11 C12 72.3(2) . . . . ?
C3 N5 C4 C12 -108.5(2) . . . 1_556 ?
N6 N5 C4 C12 72.2(2) . . . 1_556 ?
N21 N22 N23 N24 0.08(19) . . . . ?
C13 N24 N23 N22 -0.41(19) . . . . ?
Cu2 N24 N23 N22 178.84(11) . . . . ?
C9 N13 C8 C7 78.9(2) . . . . ?
N14 N13 C8 C7 -102.6(2) . . . . ?
C6 C7 C8 N13 -165.19(15) . . . . ?
C5 N9 C6 C7 79.0(2) . . . . ?
N10 N9 C6 C7 -102.37(19) . . . . ?
C8 C7 C6 N9 -165.19(15) . . . . ?
N13 N14 N15 N16 -0.1(2) . . . . ?
C9 N16 N15 N14 0.4(2) . . . . ?
Cu2 N16 N15 N14 -169.91(13) . . . . ?
N3 N4 C1 N1 0.32(19) . . . . ?
Cu1 N4 C1 N1 -178.66(11) . . . . ?
N2 N1 C1 N4 -0.4(2) . . . . ?
C2 N1 C1 N4 178.45(16) . . . . ?
N23 N24 C13 N21 0.57(19) . . . . ?
Cu2 N24 C13 N21 -178.64(11) . . . . ?
N22 N21 C13 N24 -0.54(19) . . . . ?
C14 N21 C13 N24 178.48(16) . . . . ?
N9 N10 N11 N12 -0.1(2) . . . . ?
C5 N12 N11 N10 0.2(2) . . . . ?
Cu1 N12 N11 N10 -169.91(13) . . . . ?
N19 N20 C10 N17 0.1(2) . . . . ?
Cu2 N20 C10 N17 -178.24(12) . . . . ?
N18 N17 C10 N20 -0.1(2) . . . . ?
C11 N17 C10 N20 -179.06(17) . . . . ?
N7 N8 C3 N5 0.07(19) . . . . ?
Cu1 N8 C3 N5 -178.37(12) . . . . ?
N6 N5 C3 N8 0.1(2) . . . . ?
C4 N5 C3 N8 -179.17(17) . . . . ?
N17 C11 C12 C4 -159.71(15) . . . 1_554 ?
C13 N21 C14 C15 92.0(2) . . . . ?
N22 N21 C14 C15 -89.04(19) . . . . ?
C2 C15 C14 N21 -173.01(14) 7_454 . . . ?
C1 N1 C2 C15 92.2(2) . . . 7_454 ?
N2 N1 C2 C15 -89.14(19) . . . 7_454 ?
N11 N12 C5 N9 -0.3(2) . . . . ?
Cu1 N12 C5 N9 170.40(12) . . . . ?
N10 N9 C5 N12 0.2(2) . . . . ?
C6 N9 C5 N12 179.01(16) . . . . ?
N15 N16 C9 N13 -0.5(2) . . . . ?
Cu2 N16 C9 N13 170.38(12) . . . . ?
N14 N13 C9 N16 0.4(2) . . . . ?
C8 N13 C9 N16 179.15(17) . . . . ?
N300 N301 N303 O303 176.6(4) . . . . ?
N300 N301 N303 O306 -15.4(5) . . . . ?
N300 N301 N303 O304 169.0(3) . . . . ?
N300 N301 N303 O305 -0.5(12) . . . . ?
N300 N301 N303 N302 -8.9(3) . . . . ?
N300 N302 N303 O303 15.8(5) . . . . ?
N300 N302 N303 O306 -176.3(4) . . . . ?
N300 N302 N303 O304 1.2(12) . . . . ?
N300 N302 N303 O305 -168.8(3) . . . . ?
N300 N302 N303 N301 9.0(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
C7 H7A N2 0.99 2.61 3.234(2) 121.3 2_554
C7 H7B N22 0.99 2.60 3.232(2) 121.6 2_554
C11 H11A O305 0.99 2.35 3.234(4) 148.3 1_554
C11 H11B O304 0.99 2.51 3.237(4) 129.9 7_454
C11 H11B O303 0.99 2.59 3.465(4) 146.9 7_454
C4 H4A O304 0.99 2.35 3.235(4) 148.3 7_455
C4 H4B O306 0.99 2.60 3.466(4) 146.8 .
C4 H4B O305 0.99 2.51 3.240(4) 129.9 .
C8 H8A O300 0.99 2.61 3.416(3) 138.3 2_554
C8 H8B O201 0.99 2.54 3.244(2) 127.9 5_554
C6 H6A O300 0.99 2.61 3.414(3) 138.3 8_556
C6 H6B O201 0.99 2.54 3.243(2) 128.2 3_556
C1 H1 O302 0.95 2.55 3.134(3) 120.0 4_444
C1 H1 O303 0.95 2.45 3.268(4) 144.2 4_444
C1 H1 N12 0.95 2.56 3.090(2) 115.6 5
C13 H13 O301 0.95 2.55 3.132(3) 120.1 6_565
C13 H13 O306 0.95 2.45 3.266(4) 144.3 6_565
C13 H13 N16 0.95 2.56 3.092(2) 115.5 5_564
C10 H10 N10 0.95 2.54 3.375(2) 147.0 2_554
C3 H3 N14 0.95 2.54 3.374(2) 147.1 2_554
C14 H14A O305 0.99 2.36 3.209(4) 143.4 6_565
C14 H14B O300 0.99 2.56 3.348(2) 136.5 .
C14 H14B O205 0.99 2.49 3.276(3) 136.0 7_454
C2 H2A O304 0.99 2.36 3.212(4) 143.3 4_444
C2 H2B O300 0.99 2.56 3.348(2) 136.5 7_454
C2 H2B O207 0.99 2.49 3.276(3) 136.0 .
C5 H5 N2 0.95 2.59 3.365(2) 139.1 2_554
C5 H5 N7 0.95 2.51 3.225(2) 132.5 5
C9 H9 N22 0.95 2.59 3.362(2) 139.0 2_554
C9 H9 N19 0.95 2.51 3.224(2) 132.5 5_564
C7 H7A N2 0.99 2.61 3.234(2) 121.3 2_554
C7 H7B N22 0.99 2.60 3.232(2) 121.6 2_554
C11 H11A O305 0.99 2.35 3.234(4) 148.3 1_554
C11 H11B O304 0.99 2.51 3.237(4) 129.9 7_454
C11 H11B O303 0.99 2.59 3.465(4) 146.9 7_454
C4 H4A O304 0.99 2.35 3.235(4) 148.3 7_455
C4 H4B O306 0.99 2.60 3.466(4) 146.8 .
C4 H4B O305 0.99 2.51 3.240(4) 129.9 .
C8 H8A O300 0.99 2.61 3.416(3) 138.3 2_554
C8 H8B O201 0.99 2.54 3.244(2) 127.9 5_554
C6 H6A O300 0.99 2.61 3.414(3) 138.3 8_556
C6 H6B O201 0.99 2.54 3.243(2) 128.2 3_556
C1 H1 O302 0.95 2.55 3.134(3) 120.0 4_444
C1 H1 O303 0.95 2.45 3.268(4) 144.2 4_444
C1 H1 N12 0.95 2.56 3.090(2) 115.6 5
C13 H13 O301 0.95 2.55 3.132(3) 120.1 6_565
C13 H13 O306 0.95 2.45 3.266(4) 144.3 6_565
C13 H13 N16 0.95 2.56 3.092(2) 115.5 5_564
C10 H10 N10 0.95 2.54 3.375(2) 147.0 2_554
C3 H3 N14 0.95 2.54 3.374(2) 147.1 2_554
C14 H14A O305 0.99 2.36 3.209(4) 143.4 6_565
C14 H14B O300 0.99 2.56 3.348(2) 136.5 .
C14 H14B O205 0.99 2.49 3.276(3) 136.0 7_454
C2 H2A O304 0.99 2.36 3.212(4) 143.3 4_444
C2 H2B O300 0.99 2.56 3.348(2) 136.5 7_454
C2 H2B O207 0.99 2.49 3.276(3) 136.0 .
C5 H5 N2 0.95 2.59 3.365(2) 139.1 2_554
C5 H5 N7 0.95 2.51 3.225(2) 132.5 5
C9 H9 N22 0.95 2.59 3.362(2) 139.0 2_554
C9 H9 N19 0.95 2.51 3.224(2) 132.5 5_564

_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         0.353
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.057

_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_lx333
_database_code_depnum_ccdc_archive 'CCDC 1816631'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Jul 07 17:22:40 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua bis(di(5H-tetrazol1-yl)propyl) copper(II) cyanodinitromethanide'
;
_chemical_name_common            
'diaqua bis(di(5H-tetrazol1-yl)propyl) copper(II) cyanodinitromethanide'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H20 Cu N16 O2, 2(C2 N3 O4)'
_chemical_formula_sum            'C14 H20 Cu N22 O10'
_chemical_formula_weight         720.06

_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                   9.4670(5)
_cell_length_b                   10.3140(5)
_cell_length_c                   14.0761(7)
_cell_angle_alpha                90.390(4)
_cell_angle_beta                 92.808(4)
_cell_angle_gamma                98.412(4)
_cell_volume                     1357.87(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4484
_cell_measurement_theta_min      4.2210
_cell_measurement_theta_max      32.1440

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    0.900
_shelx_estimated_absorpt_T_min   0.614
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75503
_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    1.761
_exptl_crystal_F_000             734
_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            11012
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.231
_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             5316
_reflns_number_gt                4536
_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)+(0.0266P)²+1.0037P] 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         5316
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0688
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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      -0.0630605000
_diffrn_orient_matrix_UB_12      0.0292257000
_diffrn_orient_matrix_UB_13      0.0025225000
_diffrn_orient_matrix_UB_21      -0.0355203000
_diffrn_orient_matrix_UB_22      -0.0465062000
_diffrn_orient_matrix_UB_23      -0.0337663000
_diffrn_orient_matrix_UB_31      -0.0226423000
_diffrn_orient_matrix_UB_32      -0.0426239000
_diffrn_orient_matrix_UB_33      0.0374069000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -12.00  105.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000    0.0000 117

#__ type_ start__ end____ width___ exp.time_
  2 omega   19.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega   55.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega   45.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -180.0000 65

#__ type_ start__ end____ width___ exp.time_
  5 omega  -12.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000    0.0000 54

#__ type_ start__ end____ width___ exp.time_
  6 omega   18.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
  7 omega   -8.00   63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 71

#__ type_ start__ end____ width___ exp.time_
  8 omega  -90.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000 -120.0000 76

;



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 0.5000 0.5000 0.5000 0.01140(9) Uani 1 2 d S . P . .
O1 O 0.73326(15) 0.48232(16) 0.55320(11) 0.0162(3) Uani 1 1 d . . . . .
N1 N 0.55760(16) 0.63035(14) 0.39829(11) 0.0132(3) Uani 1 1 d . . . . .
N2 N 0.69538(17) 0.66800(16) 0.37644(12) 0.0186(4) Uani 1 1 d . . . . .
N3 N 0.69972(17) 0.74649(16) 0.30544(12) 0.0192(4) Uani 1 1 d . . . . .
N4 N 0.56432(16) 0.76098(14) 0.28051(11) 0.0119(3) Uani 1 1 d . . . . .
N5 N 0.50480(16) 0.35081(14) 0.40660(11) 0.0126(3) Uani 1 1 d . . . . .
N6 N 0.60213(18) 0.36032(16) 0.33790(12) 0.0195(4) Uani 1 1 d . . . . .
N7 N 0.59607(19) 0.24912(16) 0.29431(13) 0.0210(4) Uani 1 1 d . . . . .
N8 N 0.49403(16) 0.16546(14) 0.33480(11) 0.0129(3) Uani 1 1 d . . . . .
C1 C 0.4784(2) 0.68941(17) 0.33762(14) 0.0145(4) Uani 1 1 d . . . . .
H1 H 0.3770 0.6818 0.3353 0.017 Uiso 1 1 calc R U . . .
C2 C 0.4392(2) 0.22859(18) 0.40302(14) 0.0141(4) Uani 1 1 d . . . . .
H2 H 0.3654 0.1922 0.4425 0.017 Uiso 1 1 calc R U . . .
C3 C 0.4557(2) 0.02798(18) 0.30223(15) 0.0170(4) Uani 1 1 d . . . . .
H3A H 0.3623(15) 0.0162(3) 0.2712(5) 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4534(2) -0.0286(9) 0.3560(9) 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5628(2) -0.00848(18) 0.23398(14) 0.0163(4) Uani 1 1 d . . . . .
H4A H 0.6538(15) 0.0086(3) 0.2631(5) 0.020 Uiso 1 1 calc R U . . .
H4B H 0.5611(2) 0.0439(9) 0.1807(9) 0.020 Uiso 1 1 calc R U . . .
C5 C 0.5336(2) 0.84823(18) 0.20242(13) 0.0143(4) Uani 1 1 d . . . . .
H5A H 0.4371(16) 0.8271(4) 0.1810(4) 0.017 Uiso 1 1 calc R U . . .
H5B H 0.5907(9) 0.8352(3) 0.1512(8) 0.017 Uiso 1 1 calc R U . . .
Cu2 Cu 0.0000 0.0000 0.0000 0.01163(9) Uani 1 2 d S . P . .
O2 O -0.24737(16) -0.08231(16) 0.01531(11) 0.0186(3) Uani 1 1 d . . . . .
N9 N 0.01718(17) 0.32791(14) 0.16903(11) 0.0135(3) Uani 1 1 d . . . . .
N10 N -0.06773(18) 0.23943(15) 0.21902(12) 0.0189(4) Uani 1 1 d . . . . .
N11 N -0.08663(18) 0.13154(16) 0.17024(12) 0.0179(4) Uani 1 1 d . . . . .
N12 N -0.01428(17) 0.14859(15) 0.08893(11) 0.0134(3) Uani 1 1 d . . . . .
N13 N 0.04355(16) -0.11325(14) 0.11153(11) 0.0125(3) Uani 1 1 d . . . . .
N14 N 0.17960(18) -0.11399(17) 0.14525(13) 0.0218(4) Uani 1 1 d . . . . .
N15 N 0.18124(18) -0.19847(17) 0.21239(12) 0.0199(4) Uani 1 1 d . . . . .
N16 N 0.04590(16) -0.25339(14) 0.22268(11) 0.0110(3) Uani 1 1 d . . . . .
C6 C 0.0697(2) 0.45990(18) 0.20731(15) 0.0168(4) Uani 1 1 d . . . . .
H6A H 0.0996(6) 0.5154(9) 0.1573(8) 0.020 Uiso 1 1 calc R U . . .
H6B H 0.1490(13) 0.45633(18) 0.2494(7) 0.020 Uiso 1 1 calc R U . . .
C7 C 0.0489(2) 0.27164(18) 0.09005(14) 0.0144(4) Uani 1 1 d . . . . .
H7 H 0.1069 0.3124 0.0423 0.017 Uiso 1 1 calc R U . . .
C8 C -0.0375(2) -0.19935(18) 0.16098(13) 0.0146(4) Uani 1 1 d . . . . .
H8 H -0.1386 -0.2195 0.1538 0.018 Uiso 1 1 calc R U . . .
C9 C 0.0117(2) -0.34813(17) 0.29868(13) 0.0126(4) Uani 1 1 d . . . . .
H9A H -0.0597(11) -0.3184(5) 0.3378(6) 0.015 Uiso 1 1 calc R U . . .
H9B H 0.0974(13) -0.35218(18) 0.3391(6) 0.015 Uiso 1 1 calc R U . . .
C10 C -0.0448(2) 0.51595(17) 0.25902(14) 0.0138(4) Uani 1 1 d . . . . .
H10A H -0.0759(5) 0.4592(9) 0.3101(8) 0.017 Uiso 1 1 calc R U . . .
H10B H -0.1257(13) 0.52052(18) 0.2159(7) 0.017 Uiso 1 1 calc R U . . .
O3 O 0.80115(17) 0.46742(17) 0.02797(12) 0.0369(4) Uani 1 1 d . . . . .
O4 O 0.6761(2) 0.60776(15) 0.08449(14) 0.0433(5) Uani 1 1 d . . . . .
O5 O 0.37535(17) 0.29267(17) 0.12982(12) 0.0335(4) Uani 1 1 d . . . . .
O6 O 0.4314(2) 0.50401(17) 0.15258(13) 0.0406(4) Uani 1 1 d . . . . .
N17 N 0.6901(2) 0.49357(18) 0.06390(14) 0.0279(4) Uani 1 1 d . . . . .
N18 N 0.4587(2) 0.39830(18) 0.12277(13) 0.0254(4) Uani 1 1 d . . . . .
N19 N 0.6238(2) 0.16091(19) 0.02362(14) 0.0299(4) Uani 1 1 d . . . . .
C11 C 0.5859(2) 0.38814(19) 0.07886(14) 0.0183(4) Uani 1 1 d . . . . .
C12 C 0.6084(2) 0.2632(2) 0.04828(15) 0.0215(4) Uani 1 1 d . . . . .
O7 O 0.95258(15) 0.35719(13) 0.47265(10) 0.0196(3) Uani 1 1 d . . . . .
O8 O 1.11414(15) 0.26107(14) 0.40833(11) 0.0231(3) Uani 1 1 d . . . . .
O9 O 0.72326(15) 0.19765(14) 0.51868(11) 0.0227(3) Uani 1 1 d . . . . .
O10 O 0.70886(16) -0.00189(14) 0.46413(11) 0.0257(3) Uani 1 1 d . . . . .
N20 N 0.99200(17) 0.25719(15) 0.44008(11) 0.0148(3) Uani 1 1 d . . . . .
N21 N 0.77361(18) 0.11230(16) 0.47471(12) 0.0178(4) Uani 1 1 d . . . . .
N22 N 1.0117(2) -0.05148(18) 0.36009(14) 0.0303(5) Uani 1 1 d . . . . .
C13 C 0.9054(2) 0.13690(18) 0.43384(13) 0.0146(4) Uani 1 1 d . . . . .
C14 C 0.9620(2) 0.03224(19) 0.39255(14) 0.0192(4) Uani 1 1 d . . . . .
H1A H 0.771(3) 0.436(2) 0.5216(18) 0.024(7) Uiso 1 1 d . . . . .
H1B H 0.784(3) 0.552(3) 0.5553(18) 0.027(7) Uiso 1 1 d . . . . .
H2A H -0.292(3) -0.132(3) -0.020(2) 0.034(8) Uiso 1 1 d . . . . .
H2B H -0.280(3) -0.019(3) 0.015(2) 0.040(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 N1 2.0106(15) 2_666 ?
Cu1 N1 2.0106(15) . ?
Cu1 N5 2.0241(15) . ?
Cu1 N5 2.0241(15) 2_666 ?
Cu1 O1 2.3298(14) 2_666 ?
Cu1 O1 2.3299(14) . ?
O1 H1A 0.78(3) . ?
O1 H1B 0.81(3) . ?
N1 C1 1.319(2) . ?
N1 N2 1.356(2) . ?
N2 N3 1.289(2) . ?
N3 N4 1.342(2) . ?
N4 C1 1.323(2) . ?
N4 C5 1.470(2) . ?
N5 C2 1.321(2) . ?
N5 N6 1.362(2) . ?
N6 N7 1.290(2) . ?
N7 N8 1.349(2) . ?
N8 C2 1.325(2) . ?
N8 C3 1.475(2) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C4 1.515(3) . ?
C3 H3A 0.957(15) . ?
C3 H3B 0.957(15) . ?
C4 C5 1.522(3) 1_545 ?
C4 H4A 0.928(15) . ?
C4 H4B 0.928(15) . ?
C5 C4 1.522(3) 1_565 ?
C5 H5A 0.942(15) . ?
C5 H5B 0.942(15) . ?
Cu2 N12 1.9962(15) 2 ?
Cu2 N12 1.9963(15) . ?
Cu2 N13 2.0252(15) 2 ?
Cu2 N13 2.0253(15) . ?
Cu2 O2 2.3920(15) . ?
Cu2 O2 2.3920(15) 2 ?
O2 H2A 0.77(3) . ?
O2 H2B 0.77(3) . ?
N9 C7 1.318(2) . ?
N9 N10 1.350(2) . ?
N9 C6 1.468(2) . ?
N10 N11 1.289(2) . ?
N11 N12 1.362(2) . ?
N12 C7 1.321(2) . ?
N13 C8 1.312(2) . ?
N13 N14 1.352(2) . ?
N14 N15 1.291(2) . ?
N15 N16 1.338(2) . ?
N16 C8 1.325(2) . ?
N16 C9 1.470(2) . ?
C6 C10 1.514(3) . ?
C6 H6A 0.939(15) . ?
C6 H6B 0.939(15) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.518(2) 1_545 ?
C9 H9A 0.974(15) . ?
C9 H9B 0.974(15) . ?
C10 C9 1.518(2) 1_565 ?
C10 H10A 0.960(14) . ?
C10 H10B 0.960(14) . ?
O3 N17 1.252(3) . ?
O4 N17 1.238(2) . ?
O5 N18 1.256(2) . ?
O6 N18 1.232(2) . ?
N17 C11 1.382(3) . ?
N18 C11 1.397(3) . ?
N19 C12 1.140(3) . ?
C11 C12 1.405(3) . ?
O7 N20 1.239(2) . ?
O8 N20 1.255(2) . ?
O9 N21 1.237(2) . ?
O10 N21 1.250(2) . ?
N20 C13 1.383(2) . ?
N21 C13 1.390(3) . ?
N22 C14 1.144(3) . ?
C13 C14 1.408(3) . ?

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_666 . ?
N1 Cu1 N5 89.82(6) 2_666 . ?
N1 Cu1 N5 90.18(6) . . ?
N1 Cu1 N5 90.18(6) 2_666 2_666 ?
N1 Cu1 N5 89.82(6) . 2_666 ?
N5 Cu1 N5 180.00(7) . 2_666 ?
N1 Cu1 O1 94.98(6) 2_666 2_666 ?
N1 Cu1 O1 85.02(6) . 2_666 ?
N5 Cu1 O1 90.51(6) . 2_666 ?
N5 Cu1 O1 89.49(6) 2_666 2_666 ?
N1 Cu1 O1 85.02(6) 2_666 . ?
N1 Cu1 O1 94.98(6) . . ?
N5 Cu1 O1 89.49(6) . . ?
N5 Cu1 O1 90.50(6) 2_666 . ?
O1 Cu1 O1 180.0 2_666 . ?
Cu1 O1 H1A 113.8(18) . . ?
Cu1 O1 H1B 112.4(17) . . ?
H1A O1 H1B 106(2) . . ?
C1 N1 N2 106.42(15) . . ?
C1 N1 Cu1 130.29(13) . . ?
N2 N1 Cu1 123.18(12) . . ?
N3 N2 N1 109.63(15) . . ?
N2 N3 N4 107.18(15) . . ?
C1 N4 N3 108.52(15) . . ?
C1 N4 C5 131.10(16) . . ?
N3 N4 C5 120.36(15) . . ?
C2 N5 N6 106.26(15) . . ?
C2 N5 Cu1 132.17(13) . . ?
N6 N5 Cu1 121.02(12) . . ?
N7 N6 N5 110.01(15) . . ?
N6 N7 N8 106.69(15) . . ?
C2 N8 N7 108.82(15) . . ?
C2 N8 C3 129.05(16) . . ?
N7 N8 C3 122.12(15) . . ?
N1 C1 N4 108.25(17) . . ?
N1 C1 H1 125.9 . . ?
N4 C1 H1 125.9 . . ?
N5 C2 N8 108.21(16) . . ?
N5 C2 H2 125.9 . . ?
N8 C2 H2 125.9 . . ?
N8 C3 C4 110.71(16) . . ?
N8 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N8 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C3 C4 C5 113.07(16) . 1_545 ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 1_545 . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 1_545 . ?
H4A C4 H4B 107.8 . . ?
N4 C5 C4 111.42(16) . 1_565 ?
N4 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 1_565 . ?
N4 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 1_565 . ?
H5A C5 H5B 108.0 . . ?
N12 Cu2 N12 180.00(9) 2 . ?
N12 Cu2 N13 90.25(6) 2 2 ?
N12 Cu2 N13 89.75(6) . 2 ?
N12 Cu2 N13 89.75(6) 2 . ?
N12 Cu2 N13 90.25(6) . . ?
N13 Cu2 N13 180.0 2 . ?
N12 Cu2 O2 89.32(6) 2 . ?
N12 Cu2 O2 90.68(6) . . ?
N13 Cu2 O2 92.39(6) 2 . ?
N13 Cu2 O2 87.61(6) . . ?
N12 Cu2 O2 90.68(6) 2 2 ?
N12 Cu2 O2 89.32(6) . 2 ?
N13 Cu2 O2 87.61(6) 2 2 ?
N13 Cu2 O2 92.39(6) . 2 ?
O2 Cu2 O2 180.0 . 2 ?
Cu2 O2 H2A 124(2) . . ?
Cu2 O2 H2B 101(2) . . ?
H2A O2 H2B 109(3) . . ?
C7 N9 N10 109.02(15) . . ?
C7 N9 C6 129.30(16) . . ?
N10 N9 C6 121.47(16) . . ?
N11 N10 N9 106.75(15) . . ?
N10 N11 N12 109.60(15) . . ?
C7 N12 N11 106.64(15) . . ?
C7 N12 Cu2 130.92(13) . . ?
N11 N12 Cu2 122.11(12) . . ?
C8 N13 N14 106.62(15) . . ?
C8 N13 Cu2 132.51(13) . . ?
N14 N13 Cu2 120.77(12) . . ?
N15 N14 N13 109.49(15) . . ?
N14 N15 N16 107.25(15) . . ?
C8 N16 N15 108.27(15) . . ?
C8 N16 C9 131.37(16) . . ?
N15 N16 C9 120.15(14) . . ?
N9 C6 C10 111.56(16) . . ?
N9 C6 H6A 109.3 . . ?
C10 C6 H6A 109.3 . . ?
N9 C6 H6B 109.3 . . ?
C10 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N9 C7 N12 107.98(16) . . ?
N9 C7 H7 126.0 . . ?
N12 C7 H7 126.0 . . ?
N13 C8 N16 108.36(17) . . ?
N13 C8 H8 125.8 . . ?
N16 C8 H8 125.8 . . ?
N16 C9 C10 111.81(15) . 1_545 ?
N16 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 1_545 . ?
N16 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 1_545 . ?
H9A C9 H9B 107.9 . . ?
C6 C10 C9 110.80(16) . 1_565 ?
C6 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 1_565 . ?
C6 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 1_565 . ?
H10A C10 H10B 108.1 . . ?
O4 N17 O3 121.22(19) . . ?
O4 N17 C11 122.7(2) . . ?
O3 N17 C11 116.10(19) . . ?
O6 N18 O5 122.80(19) . . ?
O6 N18 C11 121.84(19) . . ?
O5 N18 C11 115.36(18) . . ?
N17 C11 N18 123.82(19) . . ?
N17 C11 C12 118.39(19) . . ?
N18 C11 C12 117.79(18) . . ?
N19 C12 C11 178.6(2) . . ?
O7 N20 O8 120.88(16) . . ?
O7 N20 C13 123.12(16) . . ?
O8 N20 C13 115.97(16) . . ?
O9 N21 O10 121.99(17) . . ?
O9 N21 C13 122.33(16) . . ?
O10 N21 C13 115.67(17) . . ?
N20 C13 N21 123.20(17) . . ?
N20 C13 C14 117.27(17) . . ?
N21 C13 C14 119.18(17) . . ?
N22 C14 C13 178.1(2) . . ?

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(2) . . . . ?
Cu1 N1 N2 N3 176.51(13) . . . . ?
N1 N2 N3 N4 0.2(2) . . . . ?
N2 N3 N4 C1 -0.2(2) . . . . ?
N2 N3 N4 C5 178.45(16) . . . . ?
C2 N5 N6 N7 0.1(2) . . . . ?
Cu1 N5 N6 N7 172.60(13) . . . . ?
N5 N6 N7 N8 -0.1(2) . . . . ?
N6 N7 N8 C2 0.1(2) . . . . ?
N6 N7 N8 C3 179.24(17) . . . . ?
N2 N1 C1 N4 -0.1(2) . . . . ?
Cu1 N1 C1 N4 -176.31(12) . . . . ?
N3 N4 C1 N1 0.2(2) . . . . ?
C5 N4 C1 N1 -178.29(17) . . . . ?
N6 N5 C2 N8 0.0(2) . . . . ?
Cu1 N5 C2 N8 -171.33(12) . . . . ?
N7 N8 C2 N5 -0.1(2) . . . . ?
C3 N8 C2 N5 -179.10(17) . . . . ?
C2 N8 C3 C4 -170.36(18) . . . . ?
N7 N8 C3 C4 10.7(2) . . . . ?
N8 C3 C4 C5 176.63(16) . . . 1_545 ?
C1 N4 C5 C4 101.0(2) . . . 1_565 ?
N3 N4 C5 C4 -77.3(2) . . . 1_565 ?
C7 N9 N10 N11 -0.1(2) . . . . ?
C6 N9 N10 N11 -175.35(16) . . . . ?
N9 N10 N11 N12 0.3(2) . . . . ?
N10 N11 N12 C7 -0.3(2) . . . . ?
N10 N11 N12 Cu2 173.74(12) . . . . ?
C8 N13 N14 N15 0.5(2) . . . . ?
Cu2 N13 N14 N15 -176.42(13) . . . . ?
N13 N14 N15 N16 0.1(2) . . . . ?
N14 N15 N16 C8 -0.6(2) . . . . ?
N14 N15 N16 C9 -175.93(16) . . . . ?
C7 N9 C6 C10 145.60(19) . . . . ?
N10 N9 C6 C10 -40.2(2) . . . . ?
N10 N9 C7 N12 -0.1(2) . . . . ?
C6 N9 C7 N12 174.66(17) . . . . ?
N11 N12 C7 N9 0.2(2) . . . . ?
Cu2 N12 C7 N9 -173.09(12) . . . . ?
N14 N13 C8 N16 -0.9(2) . . . . ?
Cu2 N13 C8 N16 175.55(12) . . . . ?
N15 N16 C8 N13 0.9(2) . . . . ?
C9 N16 C8 N13 175.54(17) . . . . ?
C8 N16 C9 C10 71.2(2) . . . 1_545 ?
N15 N16 C9 C10 -114.65(18) . . . 1_545 ?
N9 C6 C10 C9 179.59(15) . . . 1_565 ?
O4 N17 C11 N18 -3.5(3) . . . . ?
O3 N17 C11 N18 176.50(19) . . . . ?
O4 N17 C11 C12 176.52(19) . . . . ?
O3 N17 C11 C12 -3.5(3) . . . . ?
O6 N18 C11 N17 -0.9(3) . . . . ?
O5 N18 C11 N17 179.41(18) . . . . ?
O6 N18 C11 C12 179.16(19) . . . . ?
O5 N18 C11 C12 -0.6(3) . . . . ?
O7 N20 C13 N21 -8.9(3) . . . . ?
O8 N20 C13 N21 172.84(17) . . . . ?
O7 N20 C13 C14 178.00(17) . . . . ?
O8 N20 C13 C14 -0.3(2) . . . . ?
O9 N21 C13 N20 1.1(3) . . . . ?
O10 N21 C13 N20 -178.94(17) . . . . ?
O9 N21 C13 C14 174.14(17) . . . . ?
O10 N21 C13 C14 -5.9(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
O1 H1A O7 0.78(3) 2.15(3) 2.873(2) 154(2) .
O1 H1A O9 0.78(3) 2.43(2) 2.960(2) 126(2) .
O1 H1B O8 0.81(3) 2.07(3) 2.858(2) 165(2) 2_766
O1 H1B O7 0.81(3) 2.58(3) 3.224(2) 138(2) 2_766
O1 H1B N20 0.81(3) 2.67(3) 3.452(2) 165(2) 2_766
O2 H2A O5 0.77(3) 2.28(3) 3.046(2) 167(3) 2
O2 H2B N19 0.77(3) 2.18(3) 2.949(2) 176(3) 1_455

_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         0.453
_refine_diff_density_min         -0.375
_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_wv009
_database_code_depnum_ccdc_archive 'CCDC 1816627'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,3-ditetrazol-1-yl)propane cobalt(II) diperchlorate
;
_chemical_name_common            
'tris-1,3(ditetrazol-1-yl)propane cobalt(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C5 H8 Co0.33 N8), 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 Co N24 O8'
_chemical_formula_weight         798.41

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'




_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'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'

_cell_length_a                   11.085(5)
_cell_length_b                   11.085(5)
_cell_length_c                   14.554(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_volume                     1548.8(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.7990
_cell_measurement_theta_max      27.5054

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.811
_shelx_estimated_absorpt_T_min   0.923
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6881
_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    1.712
_exptl_crystal_F_000             814
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71069
_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            13757
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.513
_diffrn_reflns_theta_max         25.971
_diffrn_reflns_theta_full        25.240
_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             1023
_reflns_number_gt                918
_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)+(0.0401P)²+1.1628P] 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         1023
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
Co1 Co 0.0000 0.0000 0.5000 0.01517(18) Uani 1 6 d S T P . .
N2 N 0.16827(16) 0.24437(16) 0.63389(11) 0.0290(4) Uani 1 1 d . . . . .
N4 N 0.06321(16) 0.35917(14) 0.64687(9) 0.0230(3) Uani 1 1 d . . . . .
N1 N 0.04936(14) 0.17808(14) 0.58311(9) 0.0197(3) Uani 1 1 d . . . . .
C2 C 0.0484(2) 0.48160(19) 0.66806(13) 0.0325(5) Uani 1 1 d . . . . .
H2A H 0.1374 0.5554 0.6941 0.039 Uiso 0.5 1 calc R U P . .
H2B H 0.0324 0.5176 0.6098 0.039 Uiso 0.5 1 calc R U P . .
N3 N 0.17684(17) 0.35333(17) 0.67219(11) 0.0322(4) Uani 1 1 d . . . . .
C1 C -0.01332(18) 0.25184(17) 0.59257(12) 0.0231(4) Uani 1 1 d . . . . .
H1 H -0.0992 0.2313 0.5650 0.028 Uiso 1 1 calc R U . . .
C3 C -0.0617(4) 0.4564(4) 0.7308(2) 0.0229(7) Uani 0.5 1 d . . P . .
H3A H -0.1474 0.3737 0.7081 0.028 Uiso 0.5 1 calc R U P . .
H3B H -0.0776 0.5365 0.7261 0.028 Uiso 0.5 1 calc R U P . .
Cl1A Cl 0.3333 0.6667 0.4565(2) 0.0230(6) Uani 0.671(8) 3 d S T P A 1
O2A O 0.3333 0.6667 0.3590(4) 0.108(3) Uani 0.671(8) 3 d S T P A 1
O1A O 0.2452(7) 0.5307(7) 0.4865(5) 0.0738(18) Uani 0.671(8) 1 d . . P A 1
Cl1B Cl 0.3333 0.6667 0.4876(5) 0.0239(11) Uani 0.329(8) 3 d S T P A 2
O2B O 0.3333 0.6667 0.5853(5) 0.035(2) Uani 0.329(8) 3 d S T P A 2
O1B O 0.2209(11) 0.5312(12) 0.4584(6) 0.0335(18) Uani 0.329(8) 1 d . . P A 2
H2C H 0.1299 0.5703 0.6497 0.062(17) Uiso 0.5 1 d R . P . .
H2D H -0.0558 0.4459 0.6641 0.064(17) Uiso 0.5 1 d R . P . .


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
Co1 N1 2.1399(15) 7_556 ?
Co1 N1 2.1399(15) 9_556 ?
Co1 N1 2.1399(15) 3 ?
Co1 N1 2.1399(15) 2 ?
Co1 N1 2.1399(15) 8_556 ?
Co1 N1 2.1399(15) . ?
N2 N3 1.290(2) . ?
N2 N1 1.362(2) . ?
N4 C1 1.323(2) . ?
N4 N3 1.345(2) . ?
N4 C2 1.479(2) . ?
N1 C1 1.318(2) . ?
C2 C3 1.436(4) . ?
C2 C3 1.514(4) 5_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2C 0.9827 . ?
C2 H2D 1.0184 . ?
C1 H1 0.9500 . ?
C3 C2 1.514(4) 5_556 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H2D 0.9831 . ?
Cl1A O1A 1.394(6) 2_665 ?
Cl1A O1A 1.394(6) . ?
Cl1A O1A 1.394(6) 3_565 ?
Cl1A O2A 1.420(6) . ?
Cl1B O2B 1.421(10) . ?
Cl1B O1B 1.455(11) 3_565 ?
Cl1B O1B 1.455(11) . ?
Cl1B O1B 1.455(11) 2_665 ?

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 Co1 N1 91.19(5) 7_556 9_556 ?
N1 Co1 N1 88.81(5) 7_556 3 ?
N1 Co1 N1 180.00(6) 9_556 3 ?
N1 Co1 N1 88.81(5) 7_556 2 ?
N1 Co1 N1 88.81(5) 9_556 2 ?
N1 Co1 N1 91.19(5) 3 2 ?
N1 Co1 N1 91.19(5) 7_556 8_556 ?
N1 Co1 N1 91.19(5) 9_556 8_556 ?
N1 Co1 N1 88.81(5) 3 8_556 ?
N1 Co1 N1 180.00(7) 2 8_556 ?
N1 Co1 N1 180.0 7_556 . ?
N1 Co1 N1 88.81(5) 9_556 . ?
N1 Co1 N1 91.19(5) 3 . ?
N1 Co1 N1 91.19(5) 2 . ?
N1 Co1 N1 88.81(5) 8_556 . ?
N3 N2 N1 109.75(14) . . ?
C1 N4 N3 108.38(14) . . ?
C1 N4 C2 129.37(16) . . ?
N3 N4 C2 121.58(16) . . ?
C1 N1 N2 106.07(13) . . ?
C1 N1 Co1 131.31(12) . . ?
N2 N1 Co1 122.44(11) . . ?
C3 C2 N4 115.35(19) . . ?
N4 C2 C3 114.05(19) . 5_556 ?
C3 C2 H2A 108.4 . . ?
N4 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
N4 C2 H2B 108.4 . . ?
C3 C2 H2B 137.5 5_556 . ?
H2A C2 H2B 107.5 . . ?
C3 C2 H2C 129.4 . . ?
N4 C2 H2C 113.1 . . ?
C3 C2 H2C 94.5 5_556 . ?
N4 C2 H2D 104.9 . . ?
C3 C2 H2D 95.7 5_556 . ?
H2A C2 H2D 144.2 . . ?
H2B C2 H2D 73.2 . . ?
H2C C2 H2D 132.1 . . ?
N2 N3 N4 107.13(15) . . ?
N1 C1 N4 108.68(15) . . ?
N1 C1 H1 125.7 . . ?
N4 C1 H1 125.7 . . ?
C2 C3 C2 120.4(3) . 5_556 ?
C2 C3 H3A 107.2 . . ?
C2 C3 H3A 107.2 5_556 . ?
C2 C3 H3B 107.2 . . ?
C2 C3 H3B 107.2 5_556 . ?
H3A C3 H3B 106.9 . . ?
C2 C3 H2D 157.1 5_556 . ?
H3A C3 H2D 69.6 . . ?
H3B C3 H2D 95.2 . . ?
O1A Cl1A O1A 110.7(4) 2_665 . ?
O1A Cl1A O1A 110.7(4) 2_665 3_565 ?
O1A Cl1A O1A 110.7(4) . 3_565 ?
O1A Cl1A O2A 108.3(4) 2_665 . ?
O1A Cl1A O2A 108.3(4) . . ?
O1A Cl1A O2A 108.3(4) 3_565 . ?
O2B Cl1B O1B 107.0(5) . 3_565 ?
O2B Cl1B O1B 107.0(5) . . ?
O1B Cl1B O1B 111.8(5) 3_565 . ?
O2B Cl1B O1B 107.0(5) . 2_665 ?
O1B Cl1B O1B 111.8(5) 3_565 2_665 ?
O1B Cl1B O1B 111.8(5) . 2_665 ?

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
N3 N2 N1 C1 -0.05(19) . . . . ?
N3 N2 N1 Co1 175.59(12) . . . . ?
C1 N4 C2 C3 76.2(3) . . . . ?
N3 N4 C2 C3 -114.4(2) . . . . ?
C1 N4 C2 C3 134.6(2) . . . 5_556 ?
N3 N4 C2 C3 -56.0(3) . . . 5_556 ?
N1 N2 N3 N4 0.1(2) . . . . ?
C1 N4 N3 N2 -0.13(19) . . . . ?
C2 N4 N3 N2 -171.53(15) . . . . ?
N2 N1 C1 N4 -0.04(18) . . . . ?
Co1 N1 C1 N4 -175.13(11) . . . . ?
N3 N4 C1 N1 0.10(19) . . . . ?
C2 N4 C1 N1 170.62(16) . . . . ?
N4 C2 C3 C2 72.5(3) . . . 5_556 ?
C3 C2 C3 C2 -29.4(3) 5_556 . . 5_556 ?

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 H2C O2B 0.98 2.17 3.026(4) 145.1 .
C1 H1 O1A 0.95 2.27 3.195(7) 163.4 9_556
C1 H1 O1B 0.95 2.31 3.221(12) 160.6 9_556
C3 H3A O2A 0.99 2.12 2.920(4) 136.9 7_566
C3 H3B N3 0.99 2.49 3.277(4) 135.7 4_566
C2 H2C N3 0.98 2.60 3.313(3) 129.1 3_565
C2 H2C O2B 0.98 2.17 3.026(4) 145.1 .
C2 H2C O2B 0.98 2.17 3.026(4) 145.1 .
C1 H1 O1A 0.95 2.27 3.195(7) 163.4 9_556
C1 H1 O1B 0.95 2.31 3.221(12) 160.6 9_556
C3 H3A O2A 0.99 2.12 2.920(4) 136.9 7_566
C3 H3B N3 0.99 2.49 3.277(4) 135.7 4_566
C2 H2C N3 0.98 2.60 3.313(3) 129.1 3_565
C2 H2C O2B 0.98 2.17 3.026(4) 145.1 .

_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         0.536
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.063

_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_lx362
_database_code_depnum_ccdc_archive 'CCDC 1816635'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sat Jul 30 14:59:07 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tris(1,1-ditetrazolylpropane) iron(II) perchlorate
;
_chemical_name_common            
'tris(1,1-ditetrazolylpropane) iron(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	3(C5 H8 Fe0.33 N8), 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 Fe N24 O8'
_chemical_formula_weight         795.33

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'



_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'

_cell_length_a                   10.9450(4)
_cell_length_b                   10.9450(4)
_cell_length_c                   14.5170(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1506.05(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3282
_cell_measurement_theta_min      4.2920
_cell_measurement_theta_max      31.6820

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.765
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97762
_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    1.754
_exptl_crystal_F_000             812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_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            11272
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.300
_diffrn_reflns_theta_max         26.346
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1032
_reflns_number_gt                873
_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)+(0.0401P)²+0.8886P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         1032
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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      -0.0547872000
_diffrn_orient_matrix_UB_12      -0.0105799000
_diffrn_orient_matrix_UB_13      -0.0308044000
_diffrn_orient_matrix_UB_21      0.0425084000
_diffrn_orient_matrix_UB_22      0.0692943000
_diffrn_orient_matrix_UB_23      -0.0174498000
_diffrn_orient_matrix_UB_31      0.0280492000
_diffrn_orient_matrix_UB_32      -0.0261059000
_diffrn_orient_matrix_UB_33      -0.0336928000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -101.00   -5.00   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  -90.0000 120

#__ type_ start__ end____ width___ exp.time_
  2 omega  -88.00    0.00   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  120.0000 110

#__ type_ start__ end____ width___ exp.time_
  3 omega -110.00  -46.80   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega   54.00   87.60   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000   60.0000 42

#__ type_ start__ end____ width___ exp.time_
  5 omega    3.80   75.00   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
  6 omega  -16.00  101.60   0.8000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000 -120.0000 147

;



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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
Fe Fe 0.0000 0.0000 0.0000 0.01430(18) Uani 1 6 d S T P . .
N1 N 0.16848(15) 0.05145(15) 0.07857(9) 0.0182(3) Uani 1 1 d . . . . .
N2 N 0.23421(17) 0.17243(17) 0.12915(11) 0.0278(4) Uani 1 1 d . . . . .
N3 N 0.34402(17) 0.18141(18) 0.16921(11) 0.0299(4) Uani 1 1 d . . . . .
C2 C 0.4730(2) 0.0509(2) 0.16839(13) 0.0302(5) Uani 1 1 d . . . A 1
H2C H 0.5128 0.0375 0.1105 0.036 Uiso 0.5 1 d R U P A 1
H2D H 0.5461 0.1400 0.1968 0.036 Uiso 0.5 1 d R U P A 1
H2A H 0.5559 0.1235 0.1342 0.036 Uiso 0.5 1 d R U P A 1
H2B H 0.4551 -0.0426 0.1470 0.036 Uiso 0.5 1 d R U P A 1
C3 C 0.5086(4) 0.0649(4) 0.2693(2) 0.0222(7) Uani 0.5 1 d . . P A 1
H31 H 0.6020 0.0780 0.2696 0.027 Uiso 0.5 1 d R U P A 1
H32 H 0.5150 0.1457 0.2946 0.027 Uiso 0.5 1 d R U P A 1
N4 N 0.34981(15) 0.06585(16) 0.14519(10) 0.0216(3) Uani 1 1 d . . . . .
C1 C 0.24266(18) -0.01193(19) 0.09003(12) 0.0207(4) Uani 1 1 d . . . . .
Cl1A Cl 0.3333 0.6667 0.0456(3) 0.0249(6) Uani 0.656(8) 3 d S T P B 1
O2A O 0.2819(8) 0.5289(7) 0.0147(6) 0.077(2) Uani 0.656(8) 1 d . . P B 1
O1A O 0.3333 0.6667 0.1425(4) 0.118(4) Uani 0.656(8) 3 d S T P B 1
Cl1B Cl 0.3333 0.6667 0.0141(5) 0.0228(11) Uani 0.344(8) 3 d S T P B 2
O2B O 0.3109(11) 0.5303(12) 0.0432(6) 0.0308(16) Uani 0.344(8) 1 d . . P B 2
O1B O 0.3333 0.6667 -0.0846(5) 0.035(2) Uani 0.344(8) 3 d S T P B 2
H1 H 0.225(2) -0.098(2) 0.0660(14) 0.029(5) Uiso 1 1 d . . . C 2


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
Fe N1 1.9950(14) 7 ?
Fe N1 1.9950(14) 8 ?
Fe N1 1.9950(14) 2 ?
Fe N1 1.9950(14) 9 ?
Fe N1 1.9950(14) 3 ?
Fe N1 1.9950(14) . ?
N1 C1 1.316(2) . ?
N1 N2 1.363(2) . ?
N2 N3 1.294(2) . ?
N3 N4 1.344(2) . ?
C2 C3 1.456(4) 6 ?
C2 N4 1.477(2) . ?
C2 C3 1.503(4) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.456(4) 6 ?
C3 H2D 1.2705 . ?
C3 H31 0.9596 . ?
C3 H32 0.9271 . ?
N4 C1 1.320(2) . ?
C1 H1 0.93(2) . ?
Cl1A O2A 1.394(7) 3_565 ?
Cl1A O2A 1.394(7) . ?
Cl1A O2A 1.394(7) 2_665 ?
Cl1A O1A 1.407(6) . ?
Cl1B O1B 1.434(10) . ?
Cl1B O2B 1.448(10) . ?
Cl1B O2B 1.448(10) 3_565 ?
Cl1B O2B 1.448(10) 2_665 ?

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 Fe N1 90.56(5) 7 8 ?
N1 Fe N1 89.44(5) 7 2 ?
N1 Fe N1 180.00(9) 8 2 ?
N1 Fe N1 90.56(5) 7 9 ?
N1 Fe N1 90.56(5) 8 9 ?
N1 Fe N1 89.44(5) 2 9 ?
N1 Fe N1 89.44(5) 7 3 ?
N1 Fe N1 89.44(5) 8 3 ?
N1 Fe N1 90.56(5) 2 3 ?
N1 Fe N1 180.00(16) 9 3 ?
N1 Fe N1 180.0 7 . ?
N1 Fe N1 89.44(5) 8 . ?
N1 Fe N1 90.56(5) 2 . ?
N1 Fe N1 89.44(5) 9 . ?
N1 Fe N1 90.56(5) 3 . ?
C1 N1 N2 106.20(14) . . ?
C1 N1 Fe 130.57(12) . . ?
N2 N1 Fe 123.14(11) . . ?
N3 N2 N1 109.58(15) . . ?
N2 N3 N4 106.92(14) . . ?
C3 C2 N4 114.93(19) 6 . ?
N4 C2 C3 114.49(19) . . ?
C3 C2 H2C 108.7 6 . ?
N4 C2 H2C 108.5 . . ?
C3 C2 H2C 137.0 . . ?
C3 C2 H2D 108.5 6 . ?
N4 C2 H2D 108.5 . . ?
H2C C2 H2D 107.5 . . ?
C3 C2 H2A 136.6 6 . ?
N4 C2 H2A 108.5 . . ?
C3 C2 H2A 108.7 . . ?
H2C C2 H2A 53.1 . . ?
H2D C2 H2A 56.9 . . ?
C3 C2 H2B 56.8 6 . ?
N4 C2 H2B 108.8 . . ?
C3 C2 H2B 108.6 . . ?
H2C C2 H2B 57.1 . . ?
H2D C2 H2B 142.5 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 C2 119.6(3) 6 . ?
C2 C3 H2D 159.5 6 . ?
C2 C3 H31 107.8 6 . ?
C2 C3 H31 102.9 . . ?
H2D C3 H31 86.1 . . ?
C2 C3 H32 106.9 6 . ?
C2 C3 H32 112.2 . . ?
H2D C3 H32 82.3 . . ?
H31 C3 H32 106.8 . . ?
C1 N4 N3 108.64(14) . . ?
C1 N4 C2 129.27(16) . . ?
N3 N4 C2 121.40(16) . . ?
N1 C1 N4 108.67(16) . . ?
N1 C1 H1 128.0(13) . . ?
N4 C1 H1 123.3(13) . . ?
O2A Cl1A O2A 110.2(4) 3_565 . ?
O2A Cl1A O2A 110.2(4) 3_565 2_665 ?
O2A Cl1A O2A 110.2(4) . 2_665 ?
O2A Cl1A O1A 108.8(4) 3_565 . ?
O2A Cl1A O1A 108.8(4) . . ?
O2A Cl1A O1A 108.8(4) 2_665 . ?
O1B Cl1B O2B 106.9(5) . . ?
O1B Cl1B O2B 106.9(5) . 3_565 ?
O2B Cl1B O2B 111.9(4) . 3_565 ?
O1B Cl1B O2B 106.9(5) . 2_665 ?
O2B Cl1B O2B 111.9(4) . 2_665 ?
O2B Cl1B O2B 111.9(4) 3_565 2_665 ?

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 0.19(19) . . . . ?
Fe N1 N2 N3 -176.67(12) . . . . ?
N1 N2 N3 N4 -0.29(19) . . . . ?
C3 C2 C3 C2 -28.6(3) 6 . . 6 ?
N4 C2 C3 C2 75.5(3) . . . 6 ?
N2 N3 N4 C1 0.27(19) . . . . ?
N2 N3 N4 C2 171.51(15) . . . . ?
C3 C2 N4 C1 -74.3(3) 6 . . . ?
C3 C2 N4 C1 -134.7(2) . . . . ?
C3 C2 N4 N3 116.4(2) 6 . . . ?
C3 C2 N4 N3 56.1(3) . . . . ?
N2 N1 C1 N4 -0.02(19) . . . . ?
Fe N1 C1 N4 176.52(11) . . . . ?
N3 N4 C1 N1 -0.16(19) . . . . ?
C2 N4 C1 N1 -170.49(16) . . . . ?

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         0.561
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.053

_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_lx536
_database_code_depnum_ccdc_archive 'CCDC 1816633'
_audit_update_record             
;
2018-01-12 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Nov 09 04:21:27 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(ditetrazolylpropanyl) copper(II) perchlorate dihydrate
;
_chemical_name_common            
'bis(ditetrazolylpropanyl) copper(II) perchlorate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H20 Cu N16 O2, 2(Cl O4)'
_chemical_formula_sum            'C10 H20 Cl2 Cu N16 O10'
_chemical_formula_weight         658.86

_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                   8.4824(4)
_cell_length_b                   14.4398(5)
_cell_length_c                   10.7195(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.217(5)
_cell_angle_gamma                90
_cell_volume                     1239.81(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    6456
_cell_measurement_theta_min      4.8440
_cell_measurement_theta_max      30.6730

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.178
_shelx_estimated_absorpt_T_min   0.719
_shelx_estimated_absorpt_T_max   0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83957
_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    1.765
_exptl_crystal_F_000             670
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      233(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            18445
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.235
_diffrn_reflns_theta_max         26.222
_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             2490
_reflns_number_gt                2224
_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)+(0.0663P)²+1.2597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_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         2490
_refine_ls_number_parameters     246
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1110
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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      -0.0043910000
_diffrn_orient_matrix_UB_12      -0.0421789000
_diffrn_orient_matrix_UB_13      0.0326303000
_diffrn_orient_matrix_UB_21      -0.0467640000
_diffrn_orient_matrix_UB_22      -0.0202075000
_diffrn_orient_matrix_UB_23      -0.0613274000
_diffrn_orient_matrix_UB_31      0.0750933000
_diffrn_orient_matrix_UB_32      -0.0150463000
_diffrn_orient_matrix_UB_33      -0.0090538000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   94.70   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -60.0000 201

#__ type_ start__ end____ width___ exp.time_
  2 omega  -24.00   69.10   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -100.0000  153.0000 133

#__ type_ start__ end____ width___ exp.time_
  3 omega  -51.00   39.30   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000 -120.0000 129

#__ type_ start__ end____ width___ exp.time_
  4 omega  -32.00   -0.50   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  131.0000  -31.0645 45

#__ type_ start__ end____ width___ exp.time_
  5 omega  -26.00    0.60   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  128.0000   30.9452 38

#__ type_ start__ end____ width___ exp.time_
  6 omega  -70.00   24.50   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  100.0000 -101.0000 135

#__ type_ start__ end____ width___ exp.time_
  7 omega  -84.00    4.20   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000 -150.0000 126

#__ type_ start__ end____ width___ exp.time_
  8 omega -102.00    3.00   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000  -30.0000 150

#__ type_ start__ end____ width___ exp.time_
  9 omega  -98.00   -4.90   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -90.0000 133

#__ type_ start__ end____ width___ exp.time_
 10 omega  -98.00   -4.90   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000   90.0000 133

#__ type_ start__ end____ width___ exp.time_
 11 omega -109.00  -74.70   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -60.0000 49

;



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'
Cl Cl 0.1484 0.1585 '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 0.5000 0.0000 0.5000 0.01914(16) Uani 1 2 d S . P . .
O1 O 0.5058(3) 0.10818(17) 0.6582(2) 0.0377(5) Uani 1 1 d . . . . .
N1 N 0.5878(2) 0.09543(13) 0.4015(2) 0.0228(4) Uani 1 1 d . . . . .
N2 N 0.6907(3) 0.15885(14) 0.4742(2) 0.0255(4) Uani 1 1 d . . . . .
N3 N 0.7103(2) 0.21907(14) 0.38993(19) 0.0219(4) Uani 1 1 d . . . . .
N4 N 0.6266(3) 0.19937(15) 0.2643(2) 0.0260(5) Uani 1 1 d . . . . .
N5 N 0.7380(2) -0.04118(15) 0.5969(2) 0.0248(4) Uani 1 1 d . . . . .
N6 N 0.7996(3) -0.04356(15) 0.7277(2) 0.0273(5) Uani 1 1 d . . . . .
N7 N 0.9498(3) -0.07714(15) 0.7543(2) 0.0277(5) Uani 1 1 d . . . . .
N8 N 0.9929(3) -0.09773(19) 0.6491(2) 0.0386(6) Uani 1 1 d . . . . .
C1 C 0.5513(3) 0.12131(19) 0.2754(3) 0.0270(5) Uani 1 1 d . . . . .
C2 C 0.8090(4) 0.3037(2) 0.4286(3) 0.0361(7) Uani 1 1 d . . . . .
C3 C 0.8569(4) -0.0740(2) 0.5521(3) 0.0345(6) Uani 1 1 d . . . . .
C4 C 1.0595(4) -0.08987(19) 0.8912(3) 0.0330(6) Uani 1 1 d . . . . .
C5 C 0.8966(4) 0.30980(18) 0.5758(3) 0.0284(5) Uani 1 1 d . . . . .
Cl1 Cl 0.27731(10) 0.34665(5) 0.38313(8) 0.0426(2) Uani 1 1 d . . . . .
O2A O 0.4602(13) 0.339(2) 0.4422(17) 0.201(12) Uani 0.452(14) 1 d . . P A 1
O3A O 0.239(3) 0.4038(11) 0.2780(11) 0.171(8) Uani 0.548(14) 1 d . . P A 1
O4A O 0.2266(15) 0.3794(8) 0.4860(11) 0.088(3) Uani 0.548(14) 1 d . . P A 1
O2B O 0.3977(13) 0.4115(6) 0.3865(9) 0.089(3) Uani 0.548(14) 1 d . . P A 2
O3B O 0.1116(11) 0.3755(6) 0.2879(11) 0.082(3) Uani 0.452(14) 1 d . . P A 2
O4B O 0.2496(18) 0.3305(18) 0.5035(13) 0.130(7) Uani 0.452(14) 1 d . . P A 2
O5 O 0.2966(8) 0.2595(3) 0.3399(8) 0.176(3) Uani 1 1 d . . . . .
H1 H 0.484(4) 0.092(2) 0.211(3) 0.032(8) Uiso 1 1 d . . . . .
H5A H 0.818(5) 0.298(3) 0.617(4) 0.052(10) Uiso 1 1 d . . . . .
H11 H 0.464(4) 0.106(2) 0.704(3) 0.020(8) Uiso 1 1 d . . . . .
H3 H 0.853(4) -0.082(2) 0.474(4) 0.044(9) Uiso 1 1 d . . . . .
H4B H 1.154(4) -0.054(2) 0.903(3) 0.037(8) Uiso 1 1 d . . . . .
H4A H 1.006(4) -0.065(2) 0.946(4) 0.043(9) Uiso 1 1 d . . . . .
H5B H 0.989(5) 0.272(3) 0.603(4) 0.053(11) Uiso 1 1 d . . . . .
H2A H 0.888(5) 0.304(3) 0.384(4) 0.054(11) Uiso 1 1 d . . . . .
H12 H 0.514(7) 0.162(4) 0.648(5) 0.088(18) Uiso 1 1 d . . . . .
H2B H 0.720(6) 0.349(3) 0.400(4) 0.069(13) 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 N1 2.021(2) . ?
Cu1 N1 2.022(2) 3_656 ?
Cu1 N5 2.032(2) 3_656 ?
Cu1 N5 2.032(2) . ?
Cu1 O1 2.294(2) 3_656 ?
Cu1 O1 2.294(2) . ?
O1 H11 0.69(3) . ?
O1 H12 0.79(6) . ?
N1 N2 1.327(3) . ?
N1 C1 1.337(3) . ?
N2 N3 1.303(3) . ?
N3 N4 1.330(3) . ?
N3 C2 1.463(3) . ?
N4 C1 1.320(3) . ?
N5 N6 1.326(3) . ?
N5 C3 1.337(3) . ?
N6 N7 1.304(3) . ?
N7 N8 1.329(3) . ?
N7 C4 1.468(3) . ?
N8 C3 1.319(4) . ?
C1 H1 0.85(3) . ?
C2 C5 1.509(4) . ?
C2 H2A 0.94(4) . ?
C2 H2B 0.96(5) . ?
C3 H3 0.83(4) . ?
C4 C5 1.509(4) 2_746 ?
C4 H4B 0.93(3) . ?
C4 H4A 0.93(4) . ?
C5 C4 1.509(4) 2_756 ?
C5 H5A 0.93(4) . ?
C5 H5B 0.92(4) . ?
Cl1 O3A 1.348(8) . ?
Cl1 O5 1.369(5) . ?
Cl1 O2B 1.377(5) . ?
Cl1 O4A 1.392(9) . ?
Cl1 O4B 1.406(13) . ?
Cl1 O2A 1.474(11) . ?
Cl1 O3B 1.499(7) . ?

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 . 3_656 ?
N1 Cu1 N5 90.49(8) . 3_656 ?
N1 Cu1 N5 89.51(8) 3_656 3_656 ?
N1 Cu1 N5 89.51(8) . . ?
N1 Cu1 N5 90.49(8) 3_656 . ?
N5 Cu1 N5 180.00(11) 3_656 . ?
N1 Cu1 O1 89.99(9) . 3_656 ?
N1 Cu1 O1 90.01(9) 3_656 3_656 ?
N5 Cu1 O1 92.62(9) 3_656 3_656 ?
N5 Cu1 O1 87.38(9) . 3_656 ?
N1 Cu1 O1 90.01(9) . . ?
N1 Cu1 O1 89.99(9) 3_656 . ?
N5 Cu1 O1 87.38(9) 3_656 . ?
N5 Cu1 O1 92.62(9) . . ?
O1 Cu1 O1 180.0 3_656 . ?
Cu1 O1 H11 127(3) . . ?
Cu1 O1 H12 123(4) . . ?
H11 O1 H12 104(5) . . ?
N2 N1 C1 106.83(19) . . ?
N2 N1 Cu1 116.61(15) . . ?
C1 N1 Cu1 135.75(17) . . ?
N3 N2 N1 105.24(19) . . ?
N2 N3 N4 114.31(19) . . ?
N2 N3 C2 123.6(2) . . ?
N4 N3 C2 122.0(2) . . ?
C1 N4 N3 101.8(2) . . ?
N6 N5 C3 106.8(2) . . ?
N6 N5 Cu1 121.83(16) . . ?
C3 N5 Cu1 131.29(18) . . ?
N7 N6 N5 104.9(2) . . ?
N6 N7 N8 114.8(2) . . ?
N6 N7 C4 121.2(2) . . ?
N8 N7 C4 124.1(2) . . ?
C3 N8 N7 101.4(2) . . ?
N4 C1 N1 111.8(2) . . ?
N4 C1 H1 125(2) . . ?
N1 C1 H1 123(2) . . ?
N3 C2 C5 112.6(2) . . ?
N3 C2 H2A 107(2) . . ?
C5 C2 H2A 110(2) . . ?
N3 C2 H2B 99(3) . . ?
C5 C2 H2B 111(3) . . ?
H2A C2 H2B 117(4) . . ?
N8 C3 N5 112.1(3) . . ?
N8 C3 H3 119(2) . . ?
N5 C3 H3 128(2) . . ?
N7 C4 C5 112.4(2) . 2_746 ?
N7 C4 H4B 107(2) . . ?
C5 C4 H4B 112(2) 2_746 . ?
N7 C4 H4A 108(2) . . ?
C5 C4 H4A 111(2) 2_746 . ?
H4B C4 H4A 107(3) . . ?
C4 C5 C2 107.4(2) 2_756 . ?
C4 C5 H5A 103(2) 2_756 . ?
C2 C5 H5A 108(2) . . ?
C4 C5 H5B 112(2) 2_756 . ?
C2 C5 H5B 112(2) . . ?
H5A C5 H5B 115(3) . . ?
O3A Cl1 O5 107.6(6) . . ?
O5 Cl1 O2B 117.6(5) . . ?
O3A Cl1 O4A 113.8(5) . . ?
O5 Cl1 O4A 133.1(6) . . ?
O5 Cl1 O4B 103.5(11) . . ?
O2B Cl1 O4B 115.8(8) . . ?
O3A Cl1 O2A 109.5(19) . . ?
O5 Cl1 O2A 81.4(10) . . ?
O4A Cl1 O2A 104.0(7) . . ?
O5 Cl1 O3B 102.4(5) . . ?
O2B Cl1 O3B 110.5(7) . . ?
O4B Cl1 O3B 105.6(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 N1 N2 N3 0.3(3) . . . . ?
Cu1 N1 N2 N3 -171.04(15) . . . . ?
N1 N2 N3 N4 -0.3(3) . . . . ?
N1 N2 N3 C2 177.0(3) . . . . ?
N2 N3 N4 C1 0.1(3) . . . . ?
C2 N3 N4 C1 -177.2(3) . . . . ?
C3 N5 N6 N7 0.0(3) . . . . ?
Cu1 N5 N6 N7 176.96(16) . . . . ?
N5 N6 N7 N8 -0.1(3) . . . . ?
N5 N6 N7 C4 179.6(2) . . . . ?
N6 N7 N8 C3 0.2(3) . . . . ?
C4 N7 N8 C3 -179.5(3) . . . . ?
N3 N4 C1 N1 0.1(3) . . . . ?
N2 N1 C1 N4 -0.2(3) . . . . ?
Cu1 N1 C1 N4 168.64(18) . . . . ?
N2 N3 C2 C5 4.6(4) . . . . ?
N4 N3 C2 C5 -178.4(2) . . . . ?
N7 N8 C3 N5 -0.2(3) . . . . ?
N6 N5 C3 N8 0.1(3) . . . . ?
Cu1 N5 C3 N8 -176.4(2) . . . . ?
N6 N7 C4 C5 117.0(3) . . . 2_746 ?
N8 N7 C4 C5 -63.3(4) . . . 2_746 ?
N3 C2 C5 C4 -160.1(3) . . . 2_756 ?

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         0.832
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.084

_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_nx005
_database_code_depnum_ccdc_archive 'CCDC 1816943'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;
_audit_creation_date             2018-01-13
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1,3-di(tetrazol-2-yl)propane
;
_chemical_name_common            1,3-di(tetrazol-2-yl)propane
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C5 H8 N8'
_chemical_formula_sum            'C5 H8 N8'
_chemical_formula_weight         180.19

_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                   11.6710(6)
_cell_length_b                   4.7586(2)
_cell_length_c                   15.1639(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.362(5)
_cell_angle_gamma                90
_cell_volume                     812.08(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    2227
_cell_measurement_theta_min      4.9940
_cell_measurement_theta_max      31.5240

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.108
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98869
_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    1.474
_exptl_crystal_F_000             376
_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            5707
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.504
_diffrn_reflns_theta_max         25.990
_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             1588
_reflns_number_gt                1370
_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)+(0.0354P)²+0.1888P] 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         1588
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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      0.0296348000
_diffrn_orient_matrix_UB_12      -0.0941715000
_diffrn_orient_matrix_UB_13      0.0348635000
_diffrn_orient_matrix_UB_21      0.0556343000
_diffrn_orient_matrix_UB_22      0.0467549000
_diffrn_orient_matrix_UB_23      -0.0050401000
_diffrn_orient_matrix_UB_31      0.0017835000
_diffrn_orient_matrix_UB_32      0.1055241000
_diffrn_orient_matrix_UB_33      0.0333683000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  75.00   1.00   12.00    --   29.79 -99.00   0.00   99
  2  ω      4.00  69.00   1.00   12.00    --   29.79 -99.00 -90.00   65
  3  ω    -28.00 105.00   1.00   12.00    --   29.79   0.00 -30.00  133
  4  ω     62.00  88.00   1.00   12.00    --   29.79 179.00 150.00   26
  5  ω   -101.00 -24.00   1.00   12.00    --  -28.70 -77.00-180.00   77
  6  ω   -110.00 -56.00   1.00   12.00    --  -28.70 179.00  30.00   54
;



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'
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
N1 N 0.30472(9) 0.4878(2) 0.58659(7) 0.0276(3) Uani 1 1 d . . . . .
N2 N 0.36312(8) 0.6741(2) 0.55012(6) 0.0233(2) Uani 1 1 d . . . . .
N3 N 0.47844(9) 0.6806(2) 0.58938(7) 0.0335(3) Uani 1 1 d . . . . .
N4 N 0.49807(9) 0.4900(2) 0.65527(7) 0.0343(3) Uani 1 1 d . . . . .
N5 N 0.18026(9) 0.5072(2) 0.18830(7) 0.0290(3) Uani 1 1 d . . . . .
N6 N 0.14424(8) 0.7329(2) 0.22481(6) 0.0238(2) Uani 1 1 d . . . . .
N7 N 0.03857(9) 0.8242(2) 0.17942(7) 0.0298(3) Uani 1 1 d . . . . .
N8 N 0.00177(9) 0.6529(2) 0.10887(7) 0.0322(3) Uani 1 1 d . . . . .
C1 C 0.39201(10) 0.3774(3) 0.65182(8) 0.0266(3) Uani 1 1 d . . . . .
H1 H 0.3804 0.2333 0.6919 0.032 Uiso 1 1 calc R U . . .
C2 C 0.30754(11) 0.8526(2) 0.47229(8) 0.0259(3) Uani 1 1 d . . . . .
H2A H 0.3696 0.9658 0.4552 0.031 Uiso 1 1 calc R U . . .
H2B H 0.2518 0.9838 0.4902 0.031 Uiso 1 1 calc R U . . .
C3 C 0.24042(10) 0.6821(2) 0.38994(7) 0.0233(3) Uani 1 1 d . . . . .
H3A H 0.2885 0.5184 0.3811 0.028 Uiso 1 1 calc R U . . .
H3B H 0.1647 0.6123 0.3995 0.028 Uiso 1 1 calc R U . . .
C4 C 0.21599(11) 0.8718(2) 0.30668(8) 0.0261(3) Uani 1 1 d . . . . .
H4A H 0.1741 1.0425 0.3187 0.031 Uiso 1 1 calc R U . . .
H4B H 0.2925 0.9312 0.2959 0.031 Uiso 1 1 calc R U . . .
C5 C 0.08922(11) 0.4643(3) 0.11621(8) 0.0289(3) Uani 1 1 d . . . . .
H5 H 0.0861 0.3152 0.0740 0.035 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
N1 N2 1.3250(13) . ?
N1 C1 1.3260(15) . ?
N2 N3 1.3200(14) . ?
N2 C2 1.4594(14) . ?
N3 N4 1.3239(15) . ?
N4 C1 1.3371(16) . ?
N5 C5 1.3230(15) . ?
N5 N6 1.3267(13) . ?
N6 N7 1.3167(13) . ?
N6 C4 1.4590(14) . ?
N7 N8 1.3227(14) . ?
N8 C5 1.3416(16) . ?
C1 H1 0.9500 . ?
C2 C3 1.5208(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.5162(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5 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
N2 N1 C1 101.41(10) . . ?
N3 N2 N1 113.79(9) . . ?
N3 N2 C2 122.18(9) . . ?
N1 N2 C2 124.01(9) . . ?
N2 N3 N4 106.02(9) . . ?
N3 N4 C1 105.77(10) . . ?
C5 N5 N6 101.30(10) . . ?
N7 N6 N5 113.92(9) . . ?
N7 N6 C4 122.84(10) . . ?
N5 N6 C4 123.22(9) . . ?
N6 N7 N8 106.13(9) . . ?
N7 N8 C5 105.57(10) . . ?
N1 C1 N4 113.01(11) . . ?
N1 C1 H1 123.5 . . ?
N4 C1 H1 123.5 . . ?
N2 C2 C3 112.05(9) . . ?
N2 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 107.97(9) . . ?
C4 C3 H3A 110.1 . . ?
C2 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
C2 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
N6 C4 C3 112.20(9) . . ?
N6 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N6 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N5 C5 N8 113.08(11) . . ?
N5 C5 H5 123.5 . . ?
N8 C5 H5 123.5 . . ?

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 N1 N2 N3 -0.01(13) . . . . ?
C1 N1 N2 C2 178.50(10) . . . . ?
N1 N2 N3 N4 -0.07(13) . . . . ?
C2 N2 N3 N4 -178.61(10) . . . . ?
N2 N3 N4 C1 0.12(13) . . . . ?
C5 N5 N6 N7 0.24(13) . . . . ?
C5 N5 N6 C4 -178.48(10) . . . . ?
N5 N6 N7 N8 -0.23(13) . . . . ?
C4 N6 N7 N8 178.49(10) . . . . ?
N6 N7 N8 C5 0.11(13) . . . . ?
N2 N1 C1 N4 0.09(13) . . . . ?
N3 N4 C1 N1 -0.14(14) . . . . ?
N3 N2 C2 C3 122.80(11) . . . . ?
N1 N2 C2 C3 -55.59(14) . . . . ?
N2 C2 C3 C4 -164.43(10) . . . . ?
N7 N6 C4 C3 118.42(12) . . . . ?
N5 N6 C4 C3 -62.97(14) . . . . ?
C2 C3 C4 N6 -175.93(9) . . . . ?
N6 N5 C5 N8 -0.16(14) . . . . ?
N7 N8 C5 N5 0.04(14) . . . . ?

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         0.147
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.041

_shelxl_version_number           2013-4


