# 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_lx565
_database_code_depnum_ccdc_archive 'CCDC 1834841'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Nov 24 22:02:45 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(2-aminotetrazolyl) copper(II) diperchlorate
;
_chemical_name_common            
'diaqua tetrakis(2-aminotetrazolyl) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Cu N20 O2, 2(Cl O4)'
_chemical_formula_sum            'C4 H16 Cl2 Cu N20 O10'
_chemical_formula_weight         638.82

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/n '
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'




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

_cell_length_a                   10.3883(3)
_cell_length_b                   10.3883(3)
_cell_length_c                   10.0967(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1089.60(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1518
_cell_measurement_theta_min      4.3970
_cell_measurement_theta_max      31.3340

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.342
_shelx_estimated_absorpt_T_min   0.616
_shelx_estimated_absorpt_T_max   0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84002
_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    1.947
_exptl_crystal_F_000             646
_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            8313
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.413
_diffrn_reflns_theta_max         25.989
_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             1067
_reflns_number_gt                879
_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)+(0.0528P)²+1.6507P] 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         1067
_refine_ls_number_parameters     113
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1049
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.362
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0112621000
_diffrn_orient_matrix_UB_12      0.0112328000
_diffrn_orient_matrix_UB_13      -0.0682935000
_diffrn_orient_matrix_UB_21      0.0497204000
_diffrn_orient_matrix_UB_22      -0.0440252000
_diffrn_orient_matrix_UB_23      -0.0164358000
_diffrn_orient_matrix_UB_31      -0.0454331000
_diffrn_orient_matrix_UB_32      -0.0509572000
_diffrn_orient_matrix_UB_33      -0.0009596000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -60.00  -34.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega -111.00  -84.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -62.00    6.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000  -60.0000 68

#__ type_ start__ end____ width___ exp.time_
  4 omega  -22.00   42.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000 -150.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega  -92.00   44.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000 -180.0000 136

#__ type_ start__ end____ width___ exp.time_
  6 omega   65.00  109.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -120.0000 44

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00   61.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
  8 omega  -13.00   75.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 88

;



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 0.2500 0.2500 0.2500 0.0132(2) Uani 1 4 d S T P . .
O1 O 0.2500 0.2500 0.0211(4) 0.0247(8) Uani 1 2 d S T P . .
N1 N 0.1162(2) 0.1083(2) 0.2539(3) 0.0148(5) Uani 1 1 d . . . . .
N2 N 0.0220(2) 0.1075(2) 0.1642(3) 0.0173(6) Uani 1 1 d . . . . .
N3 N -0.0513(2) 0.0123(2) 0.2011(3) 0.0197(6) Uani 1 1 d . . . . .
N4 N -0.0130(3) -0.0510(3) 0.3077(3) 0.0302(7) Uani 1 1 d . . . . .
N5 N -0.1614(3) -0.0239(3) 0.1310(4) 0.0260(7) Uani 1 1 d . . . . .
C1 C 0.0923(3) 0.0132(3) 0.3395(4) 0.0223(7) Uani 1 1 d . . . . .
Cl1 Cl 0.2500 0.7500 0.13602(10) 0.0215(3) Uani 1 2 d DS T P . .
O3 O 0.2500 0.7500 0.2783(3) 0.0257(7) Uani 1 2 d DS T P A .
O2 O 0.1245(10) 0.711(3) 0.0881(7) 0.066(7) Uiso 0.155(7) 1 d D . P A -1
O4 O 0.346(2) 0.660(2) 0.0877(7) 0.069(7) Uiso 0.155(7) 1 d D . P A -1
O1A O 0.279(2) 0.8771(7) 0.0867(6) 0.017(2) Uiso 0.155(7) 1 d D U P A -1
O2B O 0.2642(9) 0.6224(4) 0.0853(6) 0.0210(19) Uiso 0.345(7) 1 d D . P A -2
O1B O 0.3379(7) 0.8385(7) 0.0758(6) 0.0223(17) Uiso 0.345(7) 1 d D U P A -2
O4B O 0.1176(4) 0.7942(8) 0.1029(6) 0.0166(17) Uiso 0.345(7) 1 d D . P A -2
H1 H 0.140(4) -0.004(4) 0.405(4) 0.032(11) Uiso 1 1 d . . . . .
H5A H -0.166(4) 0.028(4) 0.072(4) 0.024(11) Uiso 1 1 d . . . . .
H5B H -0.224(5) -0.013(5) 0.187(5) 0.053(14) Uiso 1 1 d . . . . .
H1A H 0.284(4) 0.300(3) -0.018(4) 0.025(11) 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 2.025(2) 3 ?
Cu1 N1 2.025(2) . ?
Cu1 N1 2.025(2) 8_656 ?
Cu1 N1 2.025(2) 6_566 ?
Cu1 O1 2.311(4) . ?
Cu1 O1 2.311(4) 6_566 ?
O1 H1A 0.74(4) . ?
N1 N2 1.334(4) . ?
N1 C1 1.335(4) . ?
N2 N3 1.303(3) . ?
N3 N4 1.323(4) . ?
N3 N5 1.396(4) . ?
N4 C1 1.321(4) . ?
N5 H5A 0.81(4) . ?
N5 H5B 0.87(5) . ?
C1 H1 0.84(4) . ?
Cl1 O1B 1.431(4) . ?
Cl1 O2B 1.429(4) . ?
Cl1 O3 1.436(3) . ?
Cl1 O1A 1.444(4) . ?
Cl1 O4 1.449(4) . ?
Cl1 O2 1.448(4) . ?
Cl1 O4B 1.488(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 177.78(14) 3 . ?
N1 Cu1 N1 90.021(3) 3 8_656 ?
N1 Cu1 N1 90.021(3) . 8_656 ?
N1 Cu1 N1 90.021(3) 3 6_566 ?
N1 Cu1 N1 90.022(3) . 6_566 ?
N1 Cu1 N1 177.78(14) 8_656 6_566 ?
N1 Cu1 O1 91.11(7) 3 . ?
N1 Cu1 O1 91.11(7) . . ?
N1 Cu1 O1 88.89(7) 8_656 . ?
N1 Cu1 O1 88.89(7) 6_566 . ?
N1 Cu1 O1 88.89(7) 3 6_566 ?
N1 Cu1 O1 88.89(7) . 6_566 ?
N1 Cu1 O1 91.11(7) 8_656 6_566 ?
N1 Cu1 O1 91.11(7) 6_566 6_566 ?
O1 Cu1 O1 180.0 . 6_566 ?
Cu1 O1 H1A 122(3) . . ?
N2 N1 C1 107.4(3) . . ?
N2 N1 Cu1 119.66(19) . . ?
C1 N1 Cu1 132.7(2) . . ?
N3 N2 N1 103.8(2) . . ?
N2 N3 N4 115.8(3) . . ?
N2 N3 N5 122.5(3) . . ?
N4 N3 N5 121.7(3) . . ?
C1 N4 N3 101.3(3) . . ?
N3 N5 H5A 104(3) . . ?
N3 N5 H5B 104(3) . . ?
H5A N5 H5B 110(4) . . ?
N4 C1 N1 111.7(3) . . ?
N4 C1 H1 125(3) . . ?
N1 C1 H1 124(3) . . ?
O1B Cl1 O2B 112.2(3) . . ?
O1B Cl1 O3 115.1(3) . . ?
O2B Cl1 O3 111.0(3) . . ?
O3 Cl1 O1A 110.2(3) . . ?
O3 Cl1 O4 109.7(3) . . ?
O1A Cl1 O4 109.1(3) . . ?
O3 Cl1 O2 109.5(3) . . ?
O1A Cl1 O2 109.3(3) . . ?
O4 Cl1 O2 109.1(3) . . ?
O1B Cl1 O4B 107.2(3) . . ?
O2B Cl1 O4B 107.5(3) . . ?
O3 Cl1 O4B 103.0(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 -0.4(3) . . . . ?
Cu1 N1 N2 N3 -174.85(19) . . . . ?
N1 N2 N3 N4 -0.4(4) . . . . ?
N1 N2 N3 N5 -178.5(3) . . . . ?
N2 N3 N4 C1 1.1(4) . . . . ?
N5 N3 N4 C1 179.2(3) . . . . ?
N3 N4 C1 N1 -1.3(4) . . . . ?
N2 N1 C1 N4 1.1(4) . . . . ?
Cu1 N1 C1 N4 174.5(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         0.740
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.085

_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_lx540
_database_code_depnum_ccdc_archive 'CCDC 1834859'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Nov 10 12:30:09 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-aminotetrazolyl)copper(II) perchlorate
;
_chemical_name_common            
'hexakis(1-aminotetrazolyl)copper(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Cu N30, 2(Cl O4)'
_chemical_formula_sum            'C6 H18 Cl2 Cu N30 O8'
_chemical_formula_weight         772.94

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'



_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, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   21.8207(4)
_cell_length_b                   21.8207(4)
_cell_length_c                   6.9043(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2847.00(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    2820
_cell_measurement_theta_min      4.3370
_cell_measurement_theta_max      31.7770

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.049
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82269
_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    1.803
_exptl_crystal_F_000             1564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173
_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            15966
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.314
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4111
_reflns_number_gt                2713
_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)+(0.0838P)²+6.0145P] 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         4111
_refine_ls_number_parameters     347
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1925
_refine_ls_wR_factor_gt          0.1674
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_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      -0.0294083000
_diffrn_orient_matrix_UB_12      0.0023889000
_diffrn_orient_matrix_UB_13      -0.0340592000
_diffrn_orient_matrix_UB_21      -0.0210826000
_diffrn_orient_matrix_UB_22      -0.0374278000
_diffrn_orient_matrix_UB_23      0.0017846000
_diffrn_orient_matrix_UB_31      -0.0099590000
_diffrn_orient_matrix_UB_32      0.0015310000
_diffrn_orient_matrix_UB_33      0.0968776000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000    0.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega  -65.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000   80.0000  250.0000 104

;



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 0.0000 0.0000 0.0000 0.0213(3) Uani 1 6 d S T P . .
N1 N 0.08625(18) 0.07395(18) 0.1722(5) 0.0335(7) Uani 1 1 d . . . . .
N2 N 0.0818(2) 0.1239(2) 0.2800(6) 0.0513(10) Uani 1 1 d . . . . .
N3 N 0.1402(2) 0.1620(2) 0.3730(7) 0.0576(11) Uani 1 1 d . . . . .
N4 N 0.18336(18) 0.13688(18) 0.3267(5) 0.0362(8) Uani 1 1 d . . . . .
N5 N 0.2507(2) 0.1630(2) 0.4045(7) 0.0526(11) Uani 1 1 d D . . . .
C1 C 0.1493(2) 0.0832(2) 0.2062(6) 0.0367(9) Uani 1 1 d . . . . .
H1 H 0.1674 0.0562 0.1538 0.044 Uiso 1 1 calc R U . . .
Cu2 Cu 0.0000 0.5000 0.0000 0.0260(2) Uani 1 2 d S . P . .
N6 N -0.03910(17) 0.40035(18) 0.1940(5) 0.0371(8) Uani 1 1 d . . . . .
N7 N -0.10118(18) 0.37345(19) 0.2918(6) 0.0434(9) Uani 1 1 d . . . . .
N8 N -0.11362(18) 0.3170(2) 0.3849(6) 0.0471(10) Uani 1 1 d . . . . .
N9 N -0.05915(18) 0.30695(18) 0.3481(6) 0.0396(9) Uani 1 1 d . . . . .
N10 N -0.0534(2) 0.2507(2) 0.4245(8) 0.0611(13) Uani 1 1 d D . . . .
N11 N 0.08899(16) 0.55438(17) 0.1648(5) 0.0305(7) Uani 1 1 d . . . . .
N12 N 0.11548(18) 0.51943(19) 0.2667(6) 0.0433(9) Uani 1 1 d . . . . .
N13 N 0.17438(19) 0.5642(2) 0.3469(6) 0.0460(10) Uani 1 1 d . . . . .
N14 N 0.18594(17) 0.62854(19) 0.2979(5) 0.0378(8) Uani 1 1 d . . . . .
N15 N 0.2459(2) 0.6909(2) 0.3522(8) 0.0726(15) Uani 1 1 d . . . . .
H15B H 0.2477 0.6901 0.4780 0.087 Uiso 1 1 d R U . . .
H15A H 0.2806 0.7013 0.2781 0.087 Uiso 1 1 d R U . . .
N16 N 0.05322(17) 0.46395(17) -0.1670(5) 0.0320(7) Uani 1 1 d . . . . .
N17 N 0.01954(19) 0.39763(19) -0.2448(6) 0.0460(10) Uani 1 1 d . . . . .
N18 N 0.0650(2) 0.3861(2) -0.3309(6) 0.0506(10) Uani 1 1 d . . . . .
N19 N 0.12821(19) 0.4451(2) -0.3127(5) 0.0384(8) Uani 1 1 d . . . . .
N20 N 0.1918(2) 0.4530(3) -0.3831(7) 0.0641(13) Uani 1 1 d . . . . .
H20B H 0.2055 0.4305 -0.2920 0.077 Uiso 1 1 d R U . . .
H20A H 0.1798 0.4305 -0.4999 0.077 Uiso 1 1 d R U . . .
C2 C -0.0145(2) 0.3577(2) 0.2332(7) 0.0427(11) Uani 1 1 d . . . . .
H2 H 0.0277 0.3626 0.1869 0.051 Uiso 1 1 calc R U . . .
C3 C 0.1338(2) 0.6224(2) 0.1877(6) 0.0358(9) Uani 1 1 d . . . . .
H3 H 0.1295 0.6593 0.1357 0.043 Uiso 1 1 calc R U . . .
C4 C 0.1204(2) 0.4924(2) -0.2133(6) 0.0344(9) Uani 1 1 d . . . . .
H4 H 0.1561 0.5379 -0.1816 0.041 Uiso 1 1 calc R U . . .
Cl1 Cl 0.17268(9) 0.34710(12) 0.0908(2) 0.0785(5) Uani 1 1 d . . . . .
Cl2 Cl 0.6667 0.3333 0.1179(3) 0.0401(4) Uani 1 3 d S T P . .
O1 O 0.6208(7) 0.3545(9) 0.0396(18) 0.113(6) Uani 0.70(2) 1 d . . P A 1
O2 O 0.6667 0.3333 0.3189(17) 0.130(8) Uani 0.70(2) 3 d S T P A 1
O2A O 0.6463(11) 0.3827(9) 0.167(5) 0.105(11) Uani 0.30(2) 1 d . . P A 2
O1A O 0.6667 0.3333 -0.076(6) 0.17(2) Uani 0.30(2) 3 d S T P A 2
O4 O 0.1670(8) 0.3560(5) 0.2776(11) 0.164(8) Uani 0.629(12) 1 d . . P B 1
O5 O 0.2237(5) 0.3976(11) -0.020(2) 0.183(10) Uani 0.629(12) 1 d . . P B 1
O7 O 0.1091(8) 0.3238(11) 0.000(2) 0.177(8) Uani 0.629(12) 1 d . . P B 1
O8 O 0.1901(7) 0.2918(11) 0.048(2) 0.214(9) Uani 0.629(12) 1 d . . P B 1
O5A O 0.2359(7) 0.3540(6) 0.167(3) 0.090(6) Uani 0.371(12) 1 d . . P B 2
O8A O 0.1131(9) 0.2845(13) 0.127(4) 0.172(13) Uani 0.371(12) 1 d . . P B 2
O7A O 0.173(2) 0.4175(16) 0.079(4) 0.245(18) Uani 0.371(12) 1 d . . P B 2
O4A O 0.172(2) 0.3406(19) -0.086(3) 0.188(17) Uani 0.371(12) 1 d . . P B 2
H5A H 0.278(6) 0.209(2) 0.370(18) 0.226 Uiso 1 1 d D U . . .
H5B H 0.243(6) 0.169(7) 0.529(6) 0.226 Uiso 1 1 d D U . . .
H10A H -0.083(5) 0.212(4) 0.358(16) 0.226 Uiso 1 1 d D U . . .
H10B H -0.071(7) 0.241(7) 0.546(7) 0.226 Uiso 1 1 d D U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.126(3) 4 ?
Cu1 N1 2.126(3) 6 ?
Cu1 N1 2.126(3) 3 ?
Cu1 N1 2.126(3) 2 ?
Cu1 N1 2.126(3) 5 ?
Cu1 N1 2.127(3) . ?
N1 C1 1.309(5) . ?
N1 N2 1.363(5) . ?
N2 N3 1.292(5) . ?
N3 N4 1.344(5) . ?
N4 C1 1.320(5) . ?
N4 N5 1.392(5) . ?
N5 H5A 0.899(10) . ?
N5 H5B 0.899(10) . ?
C1 H1 0.9300 . ?
Cu2 N11 2.042(3) . ?
Cu2 N11 2.042(3) 4_565 ?
Cu2 N16 2.052(3) 4_565 ?
Cu2 N16 2.052(3) . ?
Cu2 N6 2.323(4) 4_565 ?
Cu2 N6 2.323(4) . ?
N6 C2 1.314(5) . ?
N6 N7 1.357(5) . ?
N7 N8 1.292(5) . ?
N8 N9 1.337(5) . ?
N9 C2 1.313(6) . ?
N9 N10 1.398(5) . ?
N10 H10A 0.898(10) . ?
N10 H10B 0.899(10) . ?
N11 C3 1.316(5) . ?
N11 N12 1.361(5) . ?
N12 N13 1.287(5) . ?
N13 N14 1.339(5) . ?
N14 C3 1.318(5) . ?
N14 N15 1.387(5) . ?
N15 H15B 0.8699 . ?
N15 H15A 0.8448 . ?
N16 C4 1.314(5) . ?
N16 N17 1.364(4) . ?
N17 N18 1.285(5) . ?
N18 N19 1.341(5) . ?
N19 C4 1.320(5) . ?
N19 N20 1.396(5) . ?
N20 H20B 0.9353 . ?
N20 H20A 0.9119 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
Cl1 O4A 1.23(2) . ?
Cl1 O4 1.319(8) . ?
Cl1 O5 1.347(10) . ?
Cl1 O8A 1.356(17) . ?
Cl1 O7 1.368(11) . ?
Cl1 O5A 1.411(11) . ?
Cl1 O8 1.47(2) . ?
Cl1 O7A 1.531(16) . ?
Cl2 O1A 1.34(4) . ?
Cl2 O2 1.387(12) . ?
Cl2 O2A 1.397(15) 3_665 ?
Cl2 O2A 1.397(15) 2_655 ?
Cl2 O2A 1.397(15) . ?
Cl2 O1 1.404(7) 2_655 ?
Cl2 O1 1.404(7) 3_665 ?
Cl2 O1 1.404(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 91.79(12) 4 6 ?
N1 Cu1 N1 88.21(12) 4 3 ?
N1 Cu1 N1 180.0(2) 6 3 ?
N1 Cu1 N1 88.21(12) 4 2 ?
N1 Cu1 N1 88.21(12) 6 2 ?
N1 Cu1 N1 91.79(12) 3 2 ?
N1 Cu1 N1 91.79(12) 4 5 ?
N1 Cu1 N1 91.79(12) 6 5 ?
N1 Cu1 N1 88.21(12) 3 5 ?
N1 Cu1 N1 180.00(16) 2 5 ?
N1 Cu1 N1 180.0 4 . ?
N1 Cu1 N1 88.21(12) 6 . ?
N1 Cu1 N1 91.79(12) 3 . ?
N1 Cu1 N1 91.79(12) 2 . ?
N1 Cu1 N1 88.21(12) 5 . ?
C1 N1 N2 105.6(3) . . ?
C1 N1 Cu1 132.9(3) . . ?
N2 N1 Cu1 121.5(3) . . ?
N3 N2 N1 110.1(3) . . ?
N2 N3 N4 106.6(4) . . ?
C1 N4 N3 108.3(4) . . ?
C1 N4 N5 128.1(4) . . ?
N3 N4 N5 123.6(4) . . ?
N4 N5 H5A 110(8) . . ?
N4 N5 H5B 101(8) . . ?
H5A N5 H5B 99(10) . . ?
N1 C1 N4 109.4(4) . . ?
N1 C1 H1 125.3 . . ?
N4 C1 H1 125.3 . . ?
N11 Cu2 N11 180.0 . 4_565 ?
N11 Cu2 N16 91.15(12) . 4_565 ?
N11 Cu2 N16 88.84(12) 4_565 4_565 ?
N11 Cu2 N16 88.84(12) . . ?
N11 Cu2 N16 91.16(12) 4_565 . ?
N16 Cu2 N16 180.0 4_565 . ?
N11 Cu2 N6 88.85(13) . 4_565 ?
N11 Cu2 N6 91.15(13) 4_565 4_565 ?
N16 Cu2 N6 88.76(13) 4_565 4_565 ?
N16 Cu2 N6 91.24(13) . 4_565 ?
N11 Cu2 N6 91.15(13) . . ?
N11 Cu2 N6 88.85(13) 4_565 . ?
N16 Cu2 N6 91.24(13) 4_565 . ?
N16 Cu2 N6 88.76(13) . . ?
N6 Cu2 N6 180.0 4_565 . ?
C2 N6 N7 105.3(4) . . ?
C2 N6 Cu2 133.9(3) . . ?
N7 N6 Cu2 120.8(3) . . ?
N8 N7 N6 110.4(3) . . ?
N7 N8 N9 106.4(3) . . ?
C2 N9 N8 108.8(4) . . ?
C2 N9 N10 127.9(4) . . ?
N8 N9 N10 123.4(4) . . ?
N9 N10 H10A 107(8) . . ?
N9 N10 H10B 111(8) . . ?
H10A N10 H10B 103(10) . . ?
C3 N11 N12 106.6(3) . . ?
C3 N11 Cu2 132.6(3) . . ?
N12 N11 Cu2 120.6(2) . . ?
N13 N12 N11 109.8(3) . . ?
N12 N13 N14 106.3(3) . . ?
C3 N14 N13 109.8(3) . . ?
C3 N14 N15 126.8(4) . . ?
N13 N14 N15 123.4(4) . . ?
N14 N15 H15B 106.3 . . ?
N14 N15 H15A 112.3 . . ?
H15B N15 H15A 124.6 . . ?
C4 N16 N17 106.7(3) . . ?
C4 N16 Cu2 131.8(3) . . ?
N17 N16 Cu2 121.3(2) . . ?
N18 N17 N16 109.3(3) . . ?
N17 N18 N19 107.0(3) . . ?
C4 N19 N18 109.1(3) . . ?
C4 N19 N20 126.4(4) . . ?
N18 N19 N20 124.5(4) . . ?
N19 N20 H20B 105.2 . . ?
N19 N20 H20A 104.1 . . ?
H20B N20 H20A 113.1 . . ?
N9 C2 N6 109.2(4) . . ?
N9 C2 H2 125.4 . . ?
N6 C2 H2 125.4 . . ?
N11 C3 N14 107.5(4) . . ?
N11 C3 H3 126.2 . . ?
N14 C3 H3 126.2 . . ?
N16 C4 N19 107.8(4) . . ?
N16 C4 H4 126.1 . . ?
N19 C4 H4 126.1 . . ?
O4 Cl1 O5 122.4(10) . . ?
O4A Cl1 O8A 96(2) . . ?
O4 Cl1 O7 110.6(9) . . ?
O5 Cl1 O7 108.2(10) . . ?
O4A Cl1 O5A 110.0(18) . . ?
O8A Cl1 O5A 115.6(10) . . ?
O4 Cl1 O8 113.6(9) . . ?
O5 Cl1 O8 96.4(12) . . ?
O7 Cl1 O8 103.5(9) . . ?
O4A Cl1 O7A 93.1(15) . . ?
O8A Cl1 O7A 123.0(19) . . ?
O5A Cl1 O7A 113.2(16) . . ?
O1A Cl2 O2A 104.1(16) . 3_665 ?
O1A Cl2 O2A 104.1(16) . 2_655 ?
O2A Cl2 O2A 114.2(12) 3_665 2_655 ?
O1A Cl2 O2A 104.1(16) . . ?
O2A Cl2 O2A 114.2(12) 3_665 . ?
O2A Cl2 O2A 114.2(12) 2_655 . ?
O2 Cl2 O1 112.7(5) . 2_655 ?
O2 Cl2 O1 112.7(5) . 3_665 ?
O1 Cl2 O1 106.1(6) 2_655 3_665 ?
O2 Cl2 O1 112.7(5) . . ?
O1 Cl2 O1 106.1(6) 2_655 . ?
O1 Cl2 O1 106.1(6) 3_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 0.7(5) . . . . ?
Cu1 N1 N2 N3 179.4(3) . . . . ?
N1 N2 N3 N4 -0.2(5) . . . . ?
N2 N3 N4 C1 -0.4(5) . . . . ?
N2 N3 N4 N5 -177.6(4) . . . . ?
N2 N1 C1 N4 -1.0(5) . . . . ?
Cu1 N1 C1 N4 -179.4(3) . . . . ?
N3 N4 C1 N1 0.9(5) . . . . ?
N5 N4 C1 N1 177.9(4) . . . . ?
C2 N6 N7 N8 -0.3(5) . . . . ?
Cu2 N6 N7 N8 177.9(3) . . . . ?
N6 N7 N8 N9 0.1(5) . . . . ?
N7 N8 N9 C2 0.1(5) . . . . ?
N7 N8 N9 N10 179.8(4) . . . . ?
C3 N11 N12 N13 -0.6(5) . . . . ?
Cu2 N11 N12 N13 174.9(3) . . . . ?
N11 N12 N13 N14 0.4(5) . . . . ?
N12 N13 N14 C3 0.0(5) . . . . ?
N12 N13 N14 N15 -177.8(4) . . . . ?
C4 N16 N17 N18 1.4(5) . . . . ?
Cu2 N16 N17 N18 -175.5(3) . . . . ?
N16 N17 N18 N19 -1.1(5) . . . . ?
N17 N18 N19 C4 0.4(5) . . . . ?
N17 N18 N19 N20 178.3(4) . . . . ?
N8 N9 C2 N6 -0.3(5) . . . . ?
N10 N9 C2 N6 -179.9(4) . . . . ?
N7 N6 C2 N9 0.3(5) . . . . ?
Cu2 N6 C2 N9 -177.5(3) . . . . ?
N12 N11 C3 N14 0.6(4) . . . . ?
Cu2 N11 C3 N14 -174.2(3) . . . . ?
N13 N14 C3 N11 -0.4(5) . . . . ?
N15 N14 C3 N11 177.3(4) . . . . ?
N17 N16 C4 N19 -1.1(5) . . . . ?
Cu2 N16 C4 N19 175.3(3) . . . . ?
N18 N19 C4 N16 0.5(5) . . . . ?
N20 N19 C4 N16 -177.3(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         1.471
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.093

_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_mx202
_database_code_depnum_ccdc_archive 'CCDC 1834854'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed May 10 17:13:18 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetra(2-aminotetrazolyl) manganese(II) diperchlorate
;
_chemical_name_common            
'diaqua tetra(2-aminotetrazolyl) manganese(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Mn N20 O2, 2(Cl O4)'
_chemical_formula_sum            'C4 H16 Cl2 Mn N20 O10'
_chemical_formula_weight         630.21

_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                   7.8980(5)
_cell_length_b                   9.6180(6)
_cell_length_c                   15.7710(7)
_cell_angle_alpha                78.554(4)
_cell_angle_beta                 76.267(4)
_cell_angle_gamma                73.230(5)
_cell_volume                     1103.34(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4126
_cell_measurement_theta_min      4.4940
_cell_measurement_theta_max      32.1210

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.960
_exptl_crystal_size_mid          0.710
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.933
_shelx_estimated_absorpt_T_min   0.468
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65379
_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    1.897
_exptl_crystal_F_000             638
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            8333
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.347
_diffrn_reflns_theta_max         25.997
_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             4311
_reflns_number_gt                3820
_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)+(0.0450P)²+1.6143P] 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         4311
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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      -0.0248245000
_diffrn_orient_matrix_UB_12      0.0079357000
_diffrn_orient_matrix_UB_13      0.0453897000
_diffrn_orient_matrix_UB_21      -0.0541414000
_diffrn_orient_matrix_UB_22      -0.0501657000
_diffrn_orient_matrix_UB_23      0.0070700000
_diffrn_orient_matrix_UB_31      0.0747533000
_diffrn_orient_matrix_UB_32      -0.0589192000
_diffrn_orient_matrix_UB_33      0.0087181000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -43.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057    0.0000   60.0000 132

#__ type_ start__ end____ width___ exp.time_
  2 omega   13.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057 -112.0000  142.0000 69

#__ type_ start__ end____ width___ exp.time_
  3 omega  -36.00   -1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057  -57.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
  4 omega  -86.00  -60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0119 -179.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   -3.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057   77.0000   30.0000 103

#__ type_ start__ end____ width___ exp.time_
  6 omega   59.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       30.1057  179.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
  7 omega -107.00  -59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0119 -179.0000  120.0000 48

;



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
Mn1 Mn 0.0000 0.5000 0.5000 0.01419(13) Uani 1 2 d S . P . .
O1 O 0.1700(3) 0.4454(2) 0.37726(13) 0.0246(4) Uani 1 1 d . . . . .
N1 N 0.4028(3) 0.7450(3) 0.48100(14) 0.0255(5) Uani 1 1 d . . . . .
N2 N 0.3657(3) 0.6950(2) 0.56590(13) 0.0154(4) Uani 1 1 d . . . . .
N3 N 0.2527(3) 0.6126(2) 0.58795(14) 0.0186(4) Uani 1 1 d . . . . .
N4 N 0.2101(3) 0.6061(2) 0.51232(14) 0.0189(4) Uani 1 1 d . . . . .
N5 N 0.4486(3) 0.7250(2) 0.62631(15) 0.0180(4) Uani 1 1 d . . . . .
N6 N -0.3109(3) 0.9435(2) 0.40264(15) 0.0214(5) Uani 1 1 d . . . . .
N7 N -0.3021(3) 0.8582(2) 0.34534(13) 0.0168(4) Uani 1 1 d . . . . .
N8 N -0.2108(3) 0.7230(2) 0.36096(13) 0.0185(4) Uani 1 1 d . . . . .
N9 N -0.1528(3) 0.7164(2) 0.43458(13) 0.0175(4) Uani 1 1 d . . . . .
N10 N -0.3768(3) 0.9141(3) 0.27003(16) 0.0262(5) Uani 1 1 d . . . . .
C1 C 0.3008(4) 0.6872(3) 0.44952(18) 0.0255(6) Uani 1 1 d . . . . .
H1 H 0.2932 0.7019 0.3890 0.031 Uiso 1 1 calc R U . . .
C2 C -0.2163(3) 0.8507(3) 0.45861(18) 0.0217(5) Uani 1 1 d . . . . .
H2 H -0.1958 0.8763 0.5098 0.026 Uiso 1 1 calc R U . . .
Mn2 Mn 0.0000 1.0000 0.0000 0.01763(14) Uani 1 2 d S . P . .
O2 O 0.1656(3) 0.9206(3) -0.12175(17) 0.0349(5) Uani 1 1 d . . . . .
N11 N 0.4568(3) 0.9950(3) 0.11455(15) 0.0284(5) Uani 1 1 d . . . . .
N12 N 0.3775(3) 1.1341(2) 0.09130(15) 0.0235(5) Uani 1 1 d . . . . .
N13 N 0.2382(3) 1.1572(2) 0.05494(15) 0.0234(5) Uani 1 1 d . . . . .
N14 N 0.2238(3) 1.0228(2) 0.05370(14) 0.0197(4) Uani 1 1 d . . . . .
N15 N 0.4463(4) 1.2462(4) 0.1000(3) 0.0468(9) Uani 1 1 d . . . . .
N16 N 0.1038(3) 0.5215(2) 0.08347(14) 0.0237(5) Uani 1 1 d . . . . .
N17 N 0.0168(3) 0.5783(2) 0.15583(13) 0.0170(4) Uani 1 1 d . . . . .
N18 N -0.0243(3) 0.7207(2) 0.14894(14) 0.0202(4) Uani 1 1 d . . . . .
N19 N 0.0402(3) 0.7633(2) 0.06434(14) 0.0202(4) Uani 1 1 d . . . . .
N20 N -0.0166(3) 0.4908(3) 0.23668(15) 0.0194(4) Uani 1 1 d . . . . .
C3 C 0.3537(4) 0.9291(3) 0.09058(18) 0.0254(6) Uani 1 1 d . . . . .
H3 H 0.3711 0.8258 0.0990 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1157(4) 0.6411(3) 0.02668(17) 0.0241(6) Uani 1 1 d . . . . .
H4 H 0.1713 0.6405 -0.0337 0.029 Uiso 1 1 calc R U . . .
Cl1 Cl 0.09834(8) 0.07863(7) 0.31123(4) 0.02183(15) Uani 1 1 d . . . . .
O3 O -0.0189(3) 0.1691(2) 0.25289(14) 0.0345(5) Uani 1 1 d . . . . .
O4 O 0.1481(4) -0.0690(2) 0.29298(16) 0.0484(6) Uani 1 1 d . . . . .
O5 O 0.2576(3) 0.1320(3) 0.29596(16) 0.0445(6) Uani 1 1 d . . . . .
O6 O 0.0078(3) 0.0868(2) 0.40051(12) 0.0310(5) Uani 1 1 d . . . . .
Cl2 Cl 0.55563(8) 0.54070(7) 0.17526(4) 0.02274(15) Uani 1 1 d . . . . .
O7 O 0.5616(3) 0.6132(3) 0.2454(2) 0.0601(8) Uani 1 1 d . . . . .
O8 O 0.6638(3) 0.3921(2) 0.18735(13) 0.0353(5) Uani 1 1 d . . . . .
O9 O 0.3776(3) 0.5434(4) 0.1785(2) 0.0741(10) Uani 1 1 d . . . . .
O10 O 0.6348(5) 0.6101(3) 0.0953(2) 0.0945(14) Uani 1 1 d . . . . .
H20B H -0.115(5) 0.539(4) 0.265(2) 0.027(8) Uiso 1 1 d . . . . .
H5B H 0.426(4) 0.823(4) 0.620(2) 0.034(9) Uiso 1 1 d . . . . .
H5A H 0.401(4) 0.692(3) 0.678(2) 0.026(8) Uiso 1 1 d . . . . .
H20A H -0.028(5) 0.413(4) 0.221(2) 0.041(10) Uiso 1 1 d . . . . .
H11 H 0.259(5) 0.398(4) 0.375(2) 0.037(11) Uiso 1 1 d . . . . .
H12 H 0.135(5) 0.454(4) 0.330(3) 0.047(11) Uiso 1 1 d . . . . .
H10B H -0.499(5) 0.952(4) 0.291(2) 0.039(9) Uiso 1 1 d . . . . .
H10A H -0.352(8) 0.850(6) 0.241(4) 0.10(2) Uiso 1 1 d . . . . .
H15A H 0.382(6) 1.317(5) 0.085(3) 0.042(11) Uiso 1 1 d . . . . .
H15B H 0.435(8) 1.249(7) 0.153(4) 0.11(2) Uiso 1 1 d . . . . .
H21 H 0.122(6) 0.907(4) -0.156(3) 0.048(12) Uiso 1 1 d . . . . .
H22 H 0.246(16) 0.909(12) -0.116(7) 0.24(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
Mn1 O1 2.1420(19) 2_566 ?
Mn1 O1 2.1420(19) . ?
Mn1 N4 2.246(2) 2_566 ?
Mn1 N4 2.246(2) . ?
Mn1 N9 2.267(2) 2_566 ?
Mn1 N9 2.267(2) . ?
O1 H11 0.72(4) . ?
O1 H12 0.84(4) . ?
N1 N2 1.323(3) . ?
N1 C1 1.328(3) . ?
N2 N3 1.302(3) . ?
N2 N5 1.391(3) . ?
N3 N4 1.331(3) . ?
N4 C1 1.334(3) . ?
N5 H5B 0.89(4) . ?
N5 H5A 0.85(3) . ?
N6 N7 1.314(3) . ?
N6 C2 1.323(3) . ?
N7 N8 1.299(3) . ?
N7 N10 1.394(3) . ?
N8 N9 1.329(3) . ?
N9 C2 1.340(3) . ?
N10 H10B 0.93(4) . ?
N10 H10A 0.79(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
Mn2 O2 2.190(2) 2_575 ?
Mn2 O2 2.190(2) . ?
Mn2 N14 2.213(2) . ?
Mn2 N14 2.213(2) 2_575 ?
Mn2 N19 2.266(2) . ?
Mn2 N19 2.266(2) 2_575 ?
O2 H21 0.76(5) . ?
O2 H22 0.64(12) . ?
N11 C3 1.322(4) . ?
N11 N12 1.322(3) . ?
N12 N13 1.302(3) . ?
N12 N15 1.381(4) . ?
N13 N14 1.334(3) . ?
N14 C3 1.321(3) . ?
N15 H15A 0.76(4) . ?
N15 H15B 0.83(6) . ?
N16 N17 1.316(3) . ?
N16 C4 1.323(3) . ?
N17 N18 1.301(3) . ?
N17 N20 1.396(3) . ?
N18 N19 1.337(3) . ?
N19 C4 1.339(3) . ?
N20 H20B 0.85(3) . ?
N20 H20A 0.86(4) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
Cl1 O6 1.4261(19) . ?
Cl1 O4 1.428(2) . ?
Cl1 O3 1.443(2) . ?
Cl1 O5 1.443(2) . ?
Cl2 O9 1.388(2) . ?
Cl2 O10 1.400(3) . ?
Cl2 O7 1.436(3) . ?
Cl2 O8 1.440(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
O1 Mn1 O1 180.00(12) 2_566 . ?
O1 Mn1 N4 85.86(8) 2_566 2_566 ?
O1 Mn1 N4 94.14(8) . 2_566 ?
O1 Mn1 N4 94.14(8) 2_566 . ?
O1 Mn1 N4 85.86(8) . . ?
N4 Mn1 N4 180.0 2_566 . ?
O1 Mn1 N9 92.28(8) 2_566 2_566 ?
O1 Mn1 N9 87.72(8) . 2_566 ?
N4 Mn1 N9 90.33(7) 2_566 2_566 ?
N4 Mn1 N9 89.67(7) . 2_566 ?
O1 Mn1 N9 87.73(8) 2_566 . ?
O1 Mn1 N9 92.27(8) . . ?
N4 Mn1 N9 89.67(7) 2_566 . ?
N4 Mn1 N9 90.33(7) . . ?
N9 Mn1 N9 180.0 2_566 . ?
Mn1 O1 H11 122(3) . . ?
Mn1 O1 H12 126(3) . . ?
H11 O1 H12 110(4) . . ?
N2 N1 C1 100.6(2) . . ?
N3 N2 N1 115.7(2) . . ?
N3 N2 N5 122.9(2) . . ?
N1 N2 N5 121.3(2) . . ?
N2 N3 N4 104.56(19) . . ?
N3 N4 C1 106.6(2) . . ?
N3 N4 Mn1 124.95(15) . . ?
C1 N4 Mn1 128.07(17) . . ?
N2 N5 H5B 106(2) . . ?
N2 N5 H5A 108(2) . . ?
H5B N5 H5A 110(3) . . ?
N7 N6 C2 101.2(2) . . ?
N8 N7 N6 115.7(2) . . ?
N8 N7 N10 123.1(2) . . ?
N6 N7 N10 121.0(2) . . ?
N7 N8 N9 104.68(19) . . ?
N8 N9 C2 106.4(2) . . ?
N8 N9 Mn1 120.69(15) . . ?
C2 N9 Mn1 132.65(17) . . ?
N7 N10 H10B 105(2) . . ?
N7 N10 H10A 108(4) . . ?
H10B N10 H10A 116(5) . . ?
N1 C1 N4 112.5(2) . . ?
N1 C1 H1 123.8 . . ?
N4 C1 H1 123.8 . . ?
N6 C2 N9 112.0(2) . . ?
N6 C2 H2 124.0 . . ?
N9 C2 H2 124.0 . . ?
O2 Mn2 O2 180.0 2_575 . ?
O2 Mn2 N14 83.57(9) 2_575 . ?
O2 Mn2 N14 96.44(9) . . ?
O2 Mn2 N14 96.43(9) 2_575 2_575 ?
O2 Mn2 N14 83.57(9) . 2_575 ?
N14 Mn2 N14 180.0 . 2_575 ?
O2 Mn2 N19 91.86(9) 2_575 . ?
O2 Mn2 N19 88.14(9) . . ?
N14 Mn2 N19 90.79(8) . . ?
N14 Mn2 N19 89.20(8) 2_575 . ?
O2 Mn2 N19 88.14(9) 2_575 2_575 ?
O2 Mn2 N19 91.86(9) . 2_575 ?
N14 Mn2 N19 89.20(8) . 2_575 ?
N14 Mn2 N19 90.80(8) 2_575 2_575 ?
N19 Mn2 N19 180.00(11) . 2_575 ?
Mn2 O2 H21 120(3) . . ?
Mn2 O2 H22 104(10) . . ?
H21 O2 H22 136(10) . . ?
C3 N11 N12 100.7(2) . . ?
N13 N12 N11 115.6(2) . . ?
N13 N12 N15 122.7(3) . . ?
N11 N12 N15 121.6(2) . . ?
N12 N13 N14 104.0(2) . . ?
C3 N14 N13 107.1(2) . . ?
C3 N14 Mn2 134.19(18) . . ?
N13 N14 Mn2 118.68(15) . . ?
N12 N15 H15A 106(3) . . ?
N12 N15 H15B 108(4) . . ?
H15A N15 H15B 103(5) . . ?
N17 N16 C4 101.1(2) . . ?
N18 N17 N16 116.1(2) . . ?
N18 N17 N20 121.9(2) . . ?
N16 N17 N20 121.8(2) . . ?
N17 N18 N19 104.04(19) . . ?
N18 N19 C4 106.7(2) . . ?
N18 N19 Mn2 124.48(15) . . ?
C4 N19 Mn2 128.60(18) . . ?
N17 N20 H20B 105(2) . . ?
N17 N20 H20A 102(2) . . ?
H20B N20 H20A 113(3) . . ?
N14 C3 N11 112.6(2) . . ?
N14 C3 H3 123.7 . . ?
N11 C3 H3 123.7 . . ?
N16 C4 N19 112.1(2) . . ?
N16 C4 H4 124.0 . . ?
N19 C4 H4 124.0 . . ?
O6 Cl1 O4 110.63(14) . . ?
O6 Cl1 O3 109.60(13) . . ?
O4 Cl1 O3 108.95(13) . . ?
O6 Cl1 O5 109.12(13) . . ?
O4 Cl1 O5 109.61(16) . . ?
O3 Cl1 O5 108.91(14) . . ?
O9 Cl2 O10 113.1(2) . . ?
O9 Cl2 O7 108.43(17) . . ?
O10 Cl2 O7 108.7(2) . . ?
O9 Cl2 O8 110.82(18) . . ?
O10 Cl2 O8 107.25(15) . . ?
O7 Cl2 O8 108.40(14) . . ?

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 0.4(3) . . . . ?
C1 N1 N2 N5 178.0(2) . . . . ?
N1 N2 N3 N4 0.0(3) . . . . ?
N5 N2 N3 N4 -177.6(2) . . . . ?
N2 N3 N4 C1 -0.5(3) . . . . ?
N2 N3 N4 Mn1 -173.89(15) . . . . ?
C2 N6 N7 N8 -0.3(3) . . . . ?
C2 N6 N7 N10 -176.2(2) . . . . ?
N6 N7 N8 N9 -0.1(3) . . . . ?
N10 N7 N8 N9 175.6(2) . . . . ?
N7 N8 N9 C2 0.5(3) . . . . ?
N7 N8 N9 Mn1 175.59(14) . . . . ?
N2 N1 C1 N4 -0.7(3) . . . . ?
N3 N4 C1 N1 0.8(3) . . . . ?
Mn1 N4 C1 N1 173.91(18) . . . . ?
N7 N6 C2 N9 0.6(3) . . . . ?
N8 N9 C2 N6 -0.7(3) . . . . ?
Mn1 N9 C2 N6 -175.01(17) . . . . ?
C3 N11 N12 N13 -0.7(3) . . . . ?
C3 N11 N12 N15 -176.6(3) . . . . ?
N11 N12 N13 N14 -0.1(3) . . . . ?
N15 N12 N13 N14 175.7(3) . . . . ?
N12 N13 N14 C3 0.9(3) . . . . ?
N12 N13 N14 Mn2 178.67(15) . . . . ?
C4 N16 N17 N18 -0.5(3) . . . . ?
C4 N16 N17 N20 -175.6(2) . . . . ?
N16 N17 N18 N19 0.3(3) . . . . ?
N20 N17 N18 N19 175.3(2) . . . . ?
N17 N18 N19 C4 0.1(3) . . . . ?
N17 N18 N19 Mn2 175.03(15) . . . . ?
N13 N14 C3 N11 -1.5(3) . . . . ?
Mn2 N14 C3 N11 -178.72(18) . . . . ?
N12 N11 C3 N14 1.3(3) . . . . ?
N17 N16 C4 N19 0.5(3) . . . . ?
N18 N19 C4 N16 -0.4(3) . . . . ?
Mn2 N19 C4 N16 -175.08(17) . . . . ?

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
N20 H20B N8 0.85(3) 2.40(3) 3.085(3) 138(3) .
N20 H20B O7 0.85(3) 2.52(3) 3.176(3) 134(3) 1_455
N20 H20B N3 0.85(3) 2.66(3) 3.106(3) 114(2) 2_566
N5 H5B N6 0.89(4) 2.16(4) 3.035(3) 166(3) 2_576
N5 H5A O8 0.85(3) 2.11(3) 2.953(3) 168(3) 2_666
N5 H5A Cl2 0.85(3) 2.89(3) 3.626(2) 145(3) 2_666
N20 H20A O3 0.86(4) 2.28(4) 3.058(3) 149(3) .
O1 H11 N5 0.72(4) 2.27(4) 2.978(3) 172(4) 2_666
O1 H12 N20 0.84(4) 2.03(4) 2.842(3) 164(4) .
N10 H10B O5 0.93(4) 2.18(4) 3.030(3) 151(3) 1_465
N10 H10A O7 0.79(6) 2.55(6) 3.180(4) 138(5) 1_455
N15 H15A N16 0.76(4) 2.49(4) 3.213(4) 160(4) 1_565
N15 H15B O5 0.83(6) 2.59(6) 3.223(5) 134(6) 1_565
O2 H21 O3 0.76(5) 2.21(5) 2.964(3) 171(4) 2_565
O2 H22 N15 0.64(12) 2.50(12) 3.087(4) 155(12) 2_675

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



_refine_diff_density_max         1.395
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.074

_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_nx013
_database_code_depnum_ccdc_archive 'CCDC 1834855'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             2018-01-18
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
1-amino-5H-tetrazole
;
_chemical_name_common            1-amino-5H-tetrazole
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H3 N5'
_chemical_formula_sum            'C H3 N5'
_chemical_formula_weight         85.08

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19
_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'

_cell_length_a                   5.0889(3)
_cell_length_b                   6.5662(5)
_cell_length_c                   11.1652(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     373.08(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    1454
_cell_measurement_theta_min      5.0830
_cell_measurement_theta_max      32.2070

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.119
_shelx_estimated_absorpt_T_min   0.943
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87247
_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    1.515
_exptl_crystal_F_000             176
_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            2753
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.401
_diffrn_reflns_theta_max         25.992
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             730
_reflns_number_gt                701
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.604
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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)+(0.0218P)²+0.0395P] 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 
;
 Flack x determined using 265 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;

_refine_ls_abs_structure_Flack   -2.3(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         730
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0504
_refine_ls_wR_factor_gt          0.0494
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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      0.0024404000
_diffrn_orient_matrix_UB_12      -0.0543840000
_diffrn_orient_matrix_UB_13      -0.0548468000
_diffrn_orient_matrix_UB_21      0.0365738000
_diffrn_orient_matrix_UB_22      0.0903093000
_diffrn_orient_matrix_UB_23      -0.0306220000
_diffrn_orient_matrix_UB_31      0.1345213000
_diffrn_orient_matrix_UB_32      -0.0236581000
_diffrn_orient_matrix_UB_33      0.0092729000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  44.00   1.00    5.00    --  -28.70  19.00 120.00   96
  2  ω     79.00 110.00   1.00    5.00    --   29.79 179.00  60.00   31
  3  ω    -20.00  72.00   1.00    5.00    --   29.79 -99.00-150.00   92
  4  ω     27.00 109.00   1.00    5.00    --   29.79-163.00-163.00   82
  5  ω    -83.00 -57.00   1.00    5.00    --  -28.70-179.00 -60.00   26
  6  ω    -80.00 -47.00   1.00    5.00    --  -28.70-179.00 150.00   33
  7  ω   -102.00 -13.00   1.00    5.00    --  -28.70 -38.00 -60.00   89
;



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 0.2087(2) 0.97035(17) 0.07911(10) 0.0182(3) Uani 1 1 d . . . . .
N2 N -0.0133(2) 0.8602(2) 0.07149(12) 0.0252(3) Uani 1 1 d . . . . .
N3 N -0.0055(3) 0.7334(2) 0.16068(12) 0.0280(3) Uani 1 1 d . . . . .
N4 N 0.2205(3) 0.7583(2) 0.22568(11) 0.0267(3) Uani 1 1 d . . . . .
N5 N 0.2787(3) 1.1194(2) -0.00468(12) 0.0242(3) Uani 1 1 d . . . . .
C1 C 0.3472(3) 0.9072(2) 0.17255(13) 0.0219(3) Uani 1 1 d . . . . .
H1 H 0.511(4) 0.963(3) 0.1936(15) 0.033(5) Uiso 1 1 d . . . . .
H5A H 0.311(4) 1.056(3) -0.0721(19) 0.047(6) Uiso 1 1 d . . . . .
H5B H 0.135(4) 1.203(3) -0.0097(17) 0.036(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
N1 C1 1.3258(18) . ?
N1 N2 1.3441(16) . ?
N1 N5 1.4002(16) . ?
N2 N3 1.2985(19) . ?
N3 N4 1.3697(18) . ?
N4 C1 1.313(2) . ?
N5 H5A 0.88(2) . ?
N5 H5B 0.92(2) . ?
C1 H1 0.94(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 109.18(12) . . ?
C1 N1 N5 127.52(12) . . ?
N2 N1 N5 123.22(11) . . ?
N3 N2 N1 105.70(12) . . ?
N2 N3 N4 110.85(12) . . ?
C1 N4 N3 105.16(13) . . ?
N1 N5 H5A 106.9(13) . . ?
N1 N5 H5B 104.7(12) . . ?
H5A N5 H5B 112.4(18) . . ?
N4 C1 N1 109.11(13) . . ?
N4 C1 H1 127.8(11) . . ?
N1 C1 H1 123.1(11) . . ?

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 0.34(15) . . . . ?
N5 N1 N2 N3 177.35(12) . . . . ?
N1 N2 N3 N4 -0.64(16) . . . . ?
N2 N3 N4 C1 0.71(17) . . . . ?
N3 N4 C1 N1 -0.48(16) . . . . ?
N2 N1 C1 N4 0.10(16) . . . . ?
N5 N1 C1 N4 -176.75(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
N5 H5A N3 0.88(2) 2.34(2) 3.100(2) 145.5(17) 3_565
N5 H5A N4 0.88(2) 2.57(2) 3.1159(18) 121.3(16) 2_574
N5 H5B N5 0.92(2) 2.16(2) 3.0702(16) 171.4(17) 3_475

_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         0.115
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.029

_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_mx031
_database_code_depnum_ccdc_archive 'CCDC 1834856'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Jan 23 19:07:27 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
aqua pentakis(2-aminotetrazole) iron(II) diperchlorate
;
_chemical_name_common            
'aqua pentakis(2-aminotetrazole) iron(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H17 Fe N25 O, 2(Cl O4)'
_chemical_formula_sum            'C5 H17 Cl2 Fe N25 O9'
_chemical_formula_weight         698.19

_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                   9.4770(6)
_cell_length_b                   9.9109(6)
_cell_length_c                   15.4054(8)
_cell_angle_alpha                75.695(5)
_cell_angle_beta                 89.058(5)
_cell_angle_gamma                63.694(6)
_cell_volume                     1249.66(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3896
_cell_measurement_theta_min      4.2370
_cell_measurement_theta_max      31.9920

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.912
_shelx_estimated_absorpt_T_min   0.593
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91523
_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    1.855
_exptl_crystal_F_000             708
_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            10053
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.144
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_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             4884
_reflns_number_gt                4136
_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)+(0.0762P)²+2.1583P] 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         4884
_refine_ls_number_parameters     484
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1276
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.039
_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      -0.0352270000
_diffrn_orient_matrix_UB_12      0.0628619000
_diffrn_orient_matrix_UB_13      -0.0393751000
_diffrn_orient_matrix_UB_21      -0.0733797000
_diffrn_orient_matrix_UB_22      0.0260882000
_diffrn_orient_matrix_UB_23      0.0185853000
_diffrn_orient_matrix_UB_31      0.0206425000
_diffrn_orient_matrix_UB_32      0.0472531000
_diffrn_orient_matrix_UB_33      0.0197012000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   10.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega   45.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega   72.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -180.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega  -69.00    5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000  120.0000 74

#__ type_ start__ end____ width___ exp.time_
  5 omega  -28.00    3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -90.0000  -82.0000 31

#__ type_ start__ end____ width___ exp.time_
  6 omega  -19.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 87

#__ type_ start__ end____ width___ exp.time_
  7 omega  -75.00  -34.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
  8 omega -101.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  -30.0000 105

;



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
Fe1 Fe -0.03402(5) 0.28728(5) 0.76865(3) 0.01377(15) Uani 1 1 d . . . . .
O1 O -0.2477(3) 0.2777(3) 0.77811(18) 0.0241(5) Uani 1 1 d . . . . .
N1 N 0.4540(3) 0.2088(3) 0.7695(2) 0.0234(6) Uani 1 1 d . . . . .
N2 N 0.3691(3) 0.3586(3) 0.72567(17) 0.0166(5) Uani 1 1 d . . . . .
N3 N 0.2155(3) 0.4098(3) 0.72354(17) 0.0181(5) Uani 1 1 d . . . . .
N4 N 0.1966(3) 0.2872(3) 0.76740(17) 0.0171(5) Uani 1 1 d . . . . .
N5 N 0.4428(3) 0.4493(3) 0.6861(2) 0.0213(6) Uani 1 1 d . . . . .
N6 N 0.0973(3) -0.1717(3) 0.72797(19) 0.0221(6) Uani 1 1 d . . . . .
N7 N 0.2159(3) -0.1976(3) 0.78464(17) 0.0174(5) Uani 1 1 d . . . . .
N8 N 0.2044(3) -0.0762(3) 0.80885(17) 0.0183(5) Uani 1 1 d . . . . .
N9 N 0.0692(3) 0.0402(3) 0.76532(18) 0.0191(5) Uani 1 1 d . . . . .
N10 N 0.3451(4) -0.3445(3) 0.8129(2) 0.0247(6) Uani 1 1 d . . . . .
N11 N -0.1586(4) 0.4536(4) 0.4785(2) 0.0372(8) Uani 1 1 d . . . . .
N12 N -0.0261(3) 0.3229(3) 0.49244(18) 0.0244(6) Uani 1 1 d . . . . .
N13 N 0.0361(3) 0.2563(3) 0.57631(18) 0.0251(6) Uani 1 1 d . . . . .
N14 N -0.0655(3) 0.3505(3) 0.62218(17) 0.0205(6) Uani 1 1 d . . . . .
N15 N 0.0488(4) 0.2659(4) 0.4223(2) 0.0338(7) Uani 1 1 d . . . . .
N16 N -0.2185(3) 0.7748(3) 0.77563(19) 0.0228(6) Uani 1 1 d . . . . .
N17 N -0.3272(3) 0.7657(3) 0.72745(18) 0.0187(5) Uani 1 1 d . . . . .
N18 N -0.2939(3) 0.6261(3) 0.72172(18) 0.0192(6) Uani 1 1 d . . . . .
N19 N -0.1517(3) 0.5338(3) 0.76899(18) 0.0187(5) Uani 1 1 d . . . . .
N20 N -0.4710(4) 0.8942(4) 0.6925(2) 0.0271(7) Uani 1 1 d D . . . .
N21 N -0.0037(3) 0.2085(3) 1.06032(19) 0.0267(7) Uani 1 1 d . . . . .
N22 N 0.1320(3) 0.1057(3) 1.04097(17) 0.0165(5) Uani 1 1 d . . . . .
N23 N 0.1398(3) 0.1062(3) 0.95705(18) 0.0213(6) Uani 1 1 d . . . . .
N24 N 0.0002(3) 0.2179(3) 0.91556(17) 0.0195(6) Uani 1 1 d . . . . .
N25 N 0.2540(3) -0.0031(3) 1.1076(2) 0.0190(6) Uani 1 1 d . . . . .
C1 C 0.3417(4) 0.1678(4) 0.7950(2) 0.0228(7) Uani 1 1 d . . . . .
C2 C 0.0064(4) -0.0212(4) 0.7181(2) 0.0233(7) Uani 1 1 d . . . . .
C3 C -0.1801(5) 0.4663(5) 0.5621(2) 0.0316(8) Uani 1 1 d . . . . .
C4 C -0.1095(4) 0.6269(4) 0.8002(2) 0.0215(7) Uani 1 1 d . . . . .
C5 C -0.0839(4) 0.2774(4) 0.9787(2) 0.0247(7) Uani 1 1 d . . . . .
Cl1 Cl 0.58563(9) 0.68836(8) 0.00511(5) 0.02003(19) Uani 1 1 d . . . . .
O2 O 0.7318(3) 0.5883(3) 0.06309(19) 0.0387(7) Uani 1 1 d . . . . .
O3 O 0.5475(3) 0.8482(3) -0.0051(2) 0.0408(7) Uani 1 1 d . . . . .
O4 O 0.6055(3) 0.6544(4) -0.08097(18) 0.0381(7) Uani 1 1 d . . . . .
O5 O 0.4609(3) 0.6580(3) 0.0443(2) 0.0398(7) Uani 1 1 d . . . . .
Cl2 Cl 0.62628(16) 0.18335(14) 0.50980(7) 0.0512(3) Uani 1 1 d . . . . .
O6A O 0.677(5) 0.261(4) 0.557(2) 0.245(16) Uani 0.408(9) 1 d . . P A 1
O7A O 0.552(5) 0.199(4) 0.5800(18) 0.29(2) Uani 0.408(9) 1 d . . P A 1
O8A O 0.8187(13) 0.1183(14) 0.5163(9) 0.090(5) Uani 0.408(9) 1 d . . P A 1
O9A O 0.6759(17) 0.1721(18) 0.4263(10) 0.077(5) Uani 0.408(9) 1 d . . P A 1
O6B O 0.5707(11) 0.3454(8) 0.5137(5) 0.069(2) Uani 0.592(9) 1 d . . P A 2
O7B O 0.4675(8) 0.1790(9) 0.5083(6) 0.080(3) Uani 0.592(9) 1 d . . P A 2
O8B O 0.7132(9) 0.0615(9) 0.5772(5) 0.087(3) Uani 0.592(9) 1 d . . P A 2
O9B O 0.6034(17) 0.2443(16) 0.4217(7) 0.110(5) Uani 0.592(9) 1 d . . P A 2
H2 H -0.085(5) 0.033(5) 0.679(3) 0.031(11) Uiso 1 1 d . . . . .
H51 H 0.400(6) 0.539(6) 0.703(3) 0.044(13) Uiso 1 1 d . . . . .
H4 H -0.014(4) 0.589(4) 0.838(2) 0.017(9) Uiso 1 1 d . . . . .
H3 H -0.265(5) 0.549(5) 0.579(3) 0.036(11) Uiso 1 1 d . . . . .
H52 H 0.420(5) 0.468(5) 0.628(3) 0.033(11) Uiso 1 1 d . . . . .
H5 H -0.182(5) 0.360(5) 0.967(3) 0.025(10) Uiso 1 1 d . . . . .
H1 H 0.362(5) 0.073(5) 0.827(3) 0.028(10) Uiso 1 1 d . . . . .
H10B H 0.319(5) -0.394(5) 0.846(3) 0.023(11) Uiso 1 1 d . . . . .
H25A H 0.256(5) 0.048(5) 1.143(3) 0.027(11) Uiso 1 1 d . . . . .
H1B H -0.251(5) 0.202(5) 0.813(3) 0.034(12) Uiso 1 1 d . . . . .
H15B H -0.026(6) 0.283(6) 0.383(3) 0.046(14) Uiso 1 1 d . . . . .
H1A H -0.328(6) 0.340(5) 0.741(3) 0.036(12) Uiso 1 1 d . . . . .
H10A H 0.421(5) -0.332(5) 0.841(3) 0.033(11) Uiso 1 1 d . . . . .
H25B H 0.330(6) -0.034(6) 1.081(3) 0.043(14) Uiso 1 1 d . . . . .
H15A H 0.106(6) 0.167(6) 0.448(3) 0.046(14) Uiso 1 1 d . . . . .
H20A H -0.506(6) 0.873(6) 0.657(3) 0.047(15) Uiso 1 1 d . . . . .
H20B H -0.453(5) 0.961(4) 0.662(3) 0.038(13) Uiso 1 1 d 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
Fe1 O1 2.070(2) . ?
Fe1 N14 2.175(3) . ?
Fe1 N24 2.181(3) . ?
Fe1 N4 2.186(3) . ?
Fe1 N19 2.192(3) . ?
Fe1 N9 2.212(3) . ?
O1 H1B 0.82(5) . ?
O1 H1A 0.84(5) . ?
N1 C1 1.320(4) . ?
N1 N2 1.331(4) . ?
N2 N3 1.310(4) . ?
N2 N5 1.392(4) . ?
N3 N4 1.322(4) . ?
N4 C1 1.341(4) . ?
N5 H51 0.90(5) . ?
N5 H52 0.88(5) . ?
N6 C2 1.320(4) . ?
N6 N7 1.326(4) . ?
N7 N8 1.305(4) . ?
N7 N10 1.389(4) . ?
N8 N9 1.326(4) . ?
N9 C2 1.345(4) . ?
N10 H10B 0.74(4) . ?
N10 H10A 0.91(5) . ?
N11 N12 1.315(4) . ?
N11 C3 1.329(5) . ?
N12 N13 1.308(4) . ?
N12 N15 1.383(4) . ?
N13 N14 1.343(4) . ?
N14 C3 1.326(4) . ?
N15 H15B 0.87(5) . ?
N15 H15A 0.87(5) . ?
N16 C4 1.325(4) . ?
N16 N17 1.327(4) . ?
N17 N18 1.302(4) . ?
N17 N20 1.384(4) . ?
N18 N19 1.339(4) . ?
N19 C4 1.339(4) . ?
N20 H20A 0.76(5) . ?
N20 H20B 0.79(2) . ?
N21 N22 1.325(4) . ?
N21 C5 1.331(4) . ?
N22 N23 1.293(4) . ?
N22 N25 1.393(4) . ?
N23 N24 1.329(4) . ?
N24 C5 1.330(4) . ?
N25 H25A 0.83(5) . ?
N25 H25B 0.79(5) . ?
C1 H1 0.88(4) . ?
C2 H2 0.92(4) . ?
C3 H3 0.95(4) . ?
C4 H4 0.95(4) . ?
C5 H5 0.91(4) . ?
Cl1 O3 1.427(3) . ?
Cl1 O5 1.433(3) . ?
Cl1 O4 1.437(3) . ?
Cl1 O2 1.444(3) . ?
Cl2 O7A 1.285(15) . ?
Cl2 O8B 1.320(6) . ?
Cl2 O9B 1.320(10) . ?
Cl2 O9A 1.376(13) . ?
Cl2 O6A 1.40(2) . ?
Cl2 O6B 1.469(7) . ?
Cl2 O7B 1.525(7) . ?
Cl2 O8A 1.639(11) . ?
O6A O7A 1.57(4) . ?
O6A O8A 1.71(4) . ?
O8A O9A 1.760(19) . ?

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
O1 Fe1 N14 92.35(10) . . ?
O1 Fe1 N24 87.59(10) . . ?
N14 Fe1 N24 178.60(10) . . ?
O1 Fe1 N4 176.31(10) . . ?
N14 Fe1 N4 91.03(10) . . ?
N24 Fe1 N4 89.00(10) . . ?
O1 Fe1 N19 90.43(10) . . ?
N14 Fe1 N19 91.22(10) . . ?
N24 Fe1 N19 90.18(10) . . ?
N4 Fe1 N19 90.99(10) . . ?
O1 Fe1 N9 86.02(10) . . ?
N14 Fe1 N9 87.53(10) . . ?
N24 Fe1 N9 91.06(10) . . ?
N4 Fe1 N9 92.64(10) . . ?
N19 Fe1 N9 176.18(10) . . ?
Fe1 O1 H1B 119(3) . . ?
Fe1 O1 H1A 122(3) . . ?
H1B O1 H1A 118(4) . . ?
C1 N1 N2 101.4(3) . . ?
N3 N2 N1 114.7(3) . . ?
N3 N2 N5 124.5(3) . . ?
N1 N2 N5 120.8(3) . . ?
N2 N3 N4 104.9(2) . . ?
N3 N4 C1 107.1(3) . . ?
N3 N4 Fe1 122.46(19) . . ?
C1 N4 Fe1 129.7(2) . . ?
N2 N5 H51 109(3) . . ?
N2 N5 H52 104(3) . . ?
H51 N5 H52 111(4) . . ?
C2 N6 N7 100.8(3) . . ?
N8 N7 N6 115.6(2) . . ?
N8 N7 N10 123.4(3) . . ?
N6 N7 N10 121.0(3) . . ?
N7 N8 N9 104.7(2) . . ?
N8 N9 C2 106.4(3) . . ?
N8 N9 Fe1 127.2(2) . . ?
C2 N9 Fe1 126.4(2) . . ?
N7 N10 H10B 107(3) . . ?
N7 N10 H10A 107(3) . . ?
H10B N10 H10A 109(4) . . ?
N12 N11 C3 101.0(3) . . ?
N13 N12 N11 115.8(3) . . ?
N13 N12 N15 122.0(3) . . ?
N11 N12 N15 122.1(3) . . ?
N12 N13 N14 103.9(3) . . ?
C3 N14 N13 106.7(3) . . ?
C3 N14 Fe1 132.3(2) . . ?
N13 N14 Fe1 120.7(2) . . ?
N12 N15 H15B 106(3) . . ?
N12 N15 H15A 103(3) . . ?
H15B N15 H15A 112(4) . . ?
C4 N16 N17 101.2(3) . . ?
N18 N17 N16 115.3(3) . . ?
N18 N17 N20 122.8(3) . . ?
N16 N17 N20 121.7(3) . . ?
N17 N18 N19 104.8(2) . . ?
C4 N19 N18 106.4(3) . . ?
C4 N19 Fe1 134.8(2) . . ?
N18 N19 Fe1 118.42(19) . . ?
N17 N20 H20A 106(4) . . ?
N17 N20 H20B 108(3) . . ?
H20A N20 H20B 101(5) . . ?
N22 N21 C5 100.5(3) . . ?
N23 N22 N21 115.7(2) . . ?
N23 N22 N25 122.1(3) . . ?
N21 N22 N25 122.1(3) . . ?
N22 N23 N24 104.8(2) . . ?
N23 N24 C5 106.8(3) . . ?
N23 N24 Fe1 118.9(2) . . ?
C5 N24 Fe1 133.7(2) . . ?
N22 N25 H25A 104(3) . . ?
N22 N25 H25B 105(3) . . ?
H25A N25 H25B 116(4) . . ?
N1 C1 N4 111.9(3) . . ?
N1 C1 H1 123(3) . . ?
N4 C1 H1 125(3) . . ?
N6 C2 N9 112.5(3) . . ?
N6 C2 H2 121(3) . . ?
N9 C2 H2 127(3) . . ?
N14 C3 N11 112.5(3) . . ?
N14 C3 H3 122(3) . . ?
N11 C3 H3 126(3) . . ?
N16 C4 N19 112.3(3) . . ?
N16 C4 H4 124(2) . . ?
N19 C4 H4 123(2) . . ?
N24 C5 N21 112.2(3) . . ?
N24 C5 H5 124(2) . . ?
N21 C5 H5 124(2) . . ?
O3 Cl1 O5 109.38(17) . . ?
O3 Cl1 O4 110.13(18) . . ?
O5 Cl1 O4 109.69(18) . . ?
O3 Cl1 O2 109.90(17) . . ?
O5 Cl1 O2 109.28(18) . . ?
O4 Cl1 O2 108.44(17) . . ?
O8B Cl2 O9B 145.9(9) . . ?
O7A Cl2 O9A 168(2) . . ?
O7A Cl2 O6A 71.1(19) . . ?
O9A Cl2 O6A 118.5(19) . . ?
O8B Cl2 O6B 123.1(6) . . ?
O9B Cl2 O6B 84.4(8) . . ?
O8B Cl2 O7B 103.0(5) . . ?
O9B Cl2 O7B 90.7(6) . . ?
O6B Cl2 O7B 99.0(5) . . ?
O7A Cl2 O8A 121(2) . . ?
O9A Cl2 O8A 70.8(8) . . ?
O6A Cl2 O8A 67.8(17) . . ?
Cl2 O6A O7A 51.0(11) . . ?
Cl2 O6A O8A 62.7(12) . . ?
O7A O6A O8A 102.4(18) . . ?
Cl2 O7A O6A 57.9(14) . . ?
Cl2 O8A O6A 49.5(10) . . ?
Cl2 O8A O9A 47.6(5) . . ?
O6A O8A O9A 87.0(10) . . ?
Cl2 O9A O8A 61.6(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.4(4) . . . . ?
C1 N1 N2 N5 -179.5(3) . . . . ?
N1 N2 N3 N4 -0.8(3) . . . . ?
N5 N2 N3 N4 179.1(3) . . . . ?
N2 N3 N4 C1 0.8(3) . . . . ?
N2 N3 N4 Fe1 -169.91(18) . . . . ?
C2 N6 N7 N8 -0.4(4) . . . . ?
C2 N6 N7 N10 -178.4(3) . . . . ?
N6 N7 N8 N9 -0.4(3) . . . . ?
N10 N7 N8 N9 177.6(3) . . . . ?
N7 N8 N9 C2 0.9(3) . . . . ?
N7 N8 N9 Fe1 -178.86(19) . . . . ?
C3 N11 N12 N13 -1.0(4) . . . . ?
C3 N11 N12 N15 -176.3(3) . . . . ?
N11 N12 N13 N14 0.8(4) . . . . ?
N15 N12 N13 N14 176.1(3) . . . . ?
N12 N13 N14 C3 -0.3(4) . . . . ?
N12 N13 N14 Fe1 174.6(2) . . . . ?
C4 N16 N17 N18 0.6(4) . . . . ?
C4 N16 N17 N20 175.4(3) . . . . ?
N16 N17 N18 N19 -0.4(3) . . . . ?
N20 N17 N18 N19 -175.2(3) . . . . ?
N17 N18 N19 C4 0.0(3) . . . . ?
N17 N18 N19 Fe1 -174.36(19) . . . . ?
C5 N21 N22 N23 -0.4(4) . . . . ?
C5 N21 N22 N25 -176.0(3) . . . . ?
N21 N22 N23 N24 0.5(4) . . . . ?
N25 N22 N23 N24 176.1(3) . . . . ?
N22 N23 N24 C5 -0.4(4) . . . . ?
N22 N23 N24 Fe1 171.44(19) . . . . ?
N2 N1 C1 N4 0.2(4) . . . . ?
N3 N4 C1 N1 -0.6(4) . . . . ?
Fe1 N4 C1 N1 169.2(2) . . . . ?
N7 N6 C2 N9 1.0(4) . . . . ?
N8 N9 C2 N6 -1.3(4) . . . . ?
Fe1 N9 C2 N6 178.5(2) . . . . ?
N13 N14 C3 N11 -0.4(5) . . . . ?
Fe1 N14 C3 N11 -174.3(3) . . . . ?
N12 N11 C3 N14 0.8(5) . . . . ?
N17 N16 C4 N19 -0.5(4) . . . . ?
N18 N19 C4 N16 0.3(4) . . . . ?
Fe1 N19 C4 N16 173.4(2) . . . . ?
N23 N24 C5 N21 0.2(4) . . . . ?
Fe1 N24 C5 N21 -169.9(2) . . . . ?
N22 N21 C5 N24 0.1(4) . . . . ?
O8B Cl2 O6A O7A -74(2) . . . . ?
O9B Cl2 O6A O7A 137(2) . . . . ?
O9A Cl2 O6A O7A 172(2) . . . . ?
O6B Cl2 O6A O7A 84(3) . . . . ?
O7B Cl2 O6A O7A 27(3) . . . . ?
O8A Cl2 O6A O7A -137(2) . . . . ?
O7A Cl2 O6A O8A 137(2) . . . . ?
O8B Cl2 O6A O8A 62.9(8) . . . . ?
O9B Cl2 O6A O8A -85.6(14) . . . . ?
O9A Cl2 O6A O8A -51.3(16) . . . . ?
O6B Cl2 O6A O8A -139(2) . . . . ?
O7B Cl2 O6A O8A 163.6(8) . . . . ?
O8B Cl2 O7A O6A 88(2) . . . . ?
O9B Cl2 O7A O6A -104(3) . . . . ?
O9A Cl2 O7A O6A -144(6) . . . . ?
O6B Cl2 O7A O6A -46.3(14) . . . . ?
O7B Cl2 O7A O6A -157(2) . . . . ?
O8A Cl2 O7A O6A 48(2) . . . . ?
O8A O6A O7A Cl2 -38.4(18) . . . . ?
O7A Cl2 O8A O6A -49.1(19) . . . . ?
O8B Cl2 O8A O6A -93.3(17) . . . . ?
O9B Cl2 O8A O6A 113.1(18) . . . . ?
O9A Cl2 O8A O6A 133.5(19) . . . . ?
O6B Cl2 O8A O6A 27.8(16) . . . . ?
O7B Cl2 O8A O6A -143(2) . . . . ?
O7A Cl2 O8A O9A 177.5(14) . . . . ?
O8B Cl2 O8A O9A 133.2(10) . . . . ?
O9B Cl2 O8A O9A -20.4(10) . . . . ?
O6A Cl2 O8A O9A -133.5(19) . . . . ?
O6B Cl2 O8A O9A -105.6(8) . . . . ?
O7B Cl2 O8A O9A 83.8(17) . . . . ?
O7A O6A O8A Cl2 32.9(16) . . . . ?
Cl2 O6A O8A O9A 32.5(12) . . . . ?
O7A O6A O8A O9A 65(2) . . . . ?
O7A Cl2 O9A O8A -170(6) . . . . ?
O8B Cl2 O9A O8A -45.1(8) . . . . ?
O9B Cl2 O9A O8A 138(2) . . . . ?
O6A Cl2 O9A O8A 49.9(18) . . . . ?
O6B Cl2 O9A O8A 96.9(7) . . . . ?
O7B Cl2 O9A O8A -157.8(5) . . . . ?
O6A O8A O9A Cl2 -33.5(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
C2 H2 O8A 0.92(4) 2.48(4) 3.257(11) 142(3) 1_455
C2 H2 O8B 0.92(4) 2.36(4) 3.225(8) 156(3) 1_455
N5 H51 N10 0.90(5) 2.21(5) 3.015(5) 148(4) 1_565
C3 H3 N18 0.95(4) 2.47(4) 3.169(5) 130(3) .
C3 H3 O7B 0.95(4) 2.54(4) 3.268(8) 133(3) 2_566
N5 H52 N11 0.88(5) 2.69(4) 3.366(4) 135(3) 2_566
N5 H52 O6B 0.88(5) 2.46(5) 3.118(8) 132(4) .
N5 H52 O6B 0.88(5) 2.52(5) 3.212(8) 136(3) 2_666
C5 H5 O4 0.91(4) 2.63(4) 3.480(4) 158(3) 1_456
C1 H1 N8 0.88(4) 2.59(4) 3.181(4) 126(3) .
N10 H10B O2 0.74(4) 2.32(4) 3.042(5) 169(4) 2_656
N25 H25A N16 0.83(5) 2.31(5) 3.128(4) 169(4) 2_567
O1 H1B N25 0.82(5) 2.06(5) 2.878(4) 176(4) 2_557
N15 H15B N6 0.87(5) 2.50(5) 3.236(4) 143(4) 2_556
O1 H1A N5 0.84(5) 2.03(5) 2.833(4) 158(4) 1_455
N10 H10A O4 0.91(5) 2.08(5) 2.977(4) 169(4) 1_546
N25 H25B O3 0.79(5) 2.44(5) 3.225(4) 173(5) 1_546
N25 H25B O3 0.79(5) 2.63(5) 3.107(4) 120(4) 2_666
N15 H15A O8A 0.87(5) 2.50(5) 3.316(12) 156(4) 2_656
N15 H15A O8B 0.87(5) 2.28(5) 3.019(9) 143(4) 2_656
N20 H20A O9A 0.76(5) 2.33(6) 3.065(17) 163(5) 2_566
N20 H20A O9B 0.76(5) 2.31(5) 3.057(12) 166(5) 2_566
N20 H20B O7A 0.79(2) 2.41(3) 3.18(2) 168(5) 1_465
N20 H20B O7B 0.79(2) 2.63(3) 3.316(8) 145(4) 1_465
N20 H20B O8B 0.79(2) 2.42(3) 3.157(9) 154(4) 1_465
C2 H2 O8A 0.92(4) 2.48(4) 3.257(11) 142(3) 1_455
C2 H2 O8B 0.92(4) 2.36(4) 3.225(8) 156(3) 1_455
N5 H51 N10 0.90(5) 2.21(5) 3.015(5) 148(4) 1_565
C3 H3 N18 0.95(4) 2.47(4) 3.169(5) 130(3) .
C3 H3 O7B 0.95(4) 2.54(4) 3.268(8) 133(3) 2_566
N5 H52 N11 0.88(5) 2.69(4) 3.366(4) 135(3) 2_566
N5 H52 O6B 0.88(5) 2.46(5) 3.118(8) 132(4) .
N5 H52 O6B 0.88(5) 2.52(5) 3.212(8) 136(3) 2_666
C5 H5 O4 0.91(4) 2.63(4) 3.480(4) 158(3) 1_456
C1 H1 N8 0.88(4) 2.59(4) 3.181(4) 126(3) .
N10 H10B O2 0.74(4) 2.32(4) 3.042(5) 169(4) 2_656
N25 H25A N16 0.83(5) 2.31(5) 3.128(4) 169(4) 2_567
O1 H1B N25 0.82(5) 2.06(5) 2.878(4) 176(4) 2_557
N15 H15B N6 0.87(5) 2.50(5) 3.236(4) 143(4) 2_556
O1 H1A N5 0.84(5) 2.03(5) 2.833(4) 158(4) 1_455
N10 H10A O4 0.91(5) 2.08(5) 2.977(4) 169(4) 1_546
N25 H25B O3 0.79(5) 2.44(5) 3.225(4) 173(5) 1_546
N25 H25B O3 0.79(5) 2.63(5) 3.107(4) 120(4) 2_666
N15 H15A O8A 0.87(5) 2.50(5) 3.316(12) 156(4) 2_656
N15 H15A O8B 0.87(5) 2.28(5) 3.019(9) 143(4) 2_656
N20 H20A O9A 0.76(5) 2.33(6) 3.065(17) 163(5) 2_566
N20 H20A O9B 0.76(5) 2.31(5) 3.057(12) 166(5) 2_566
N20 H20B O7A 0.79(2) 2.41(3) 3.18(2) 168(5) 1_465
N20 H20B O7B 0.79(2) 2.63(3) 3.316(8) 145(4) 1_465
N20 H20B O8B 0.79(2) 2.42(3) 3.157(9) 154(4) 1_465

_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         2.486
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.107

_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_lx582
_database_code_depnum_ccdc_archive 'CCDC 1834842'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Dec 02 12:09:50 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
dichlorido bis(2-aminotetrazolyl) copper(II)
;
_chemical_name_common            'dichlorido bis(2-aminotetrazolyl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 Cl2 Cu N10'
_chemical_formula_sum            'C2 H6 Cl2 Cu N10'
_chemical_formula_weight         304.61

_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                   6.8468(5)
_cell_length_b                   3.6679(2)
_cell_length_c                   18.5122(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.579(6)
_cell_angle_gamma                90
_cell_volume                     464.73(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1367
_cell_measurement_theta_min      5.2430
_cell_measurement_theta_max      32.0220

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.909
_shelx_estimated_absorpt_T_min   0.438
_shelx_estimated_absorpt_T_max   0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92278
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_F_000             302
_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            2907
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.405
_diffrn_reflns_theta_max         25.991
_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             920
_reflns_number_gt                831
_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)+(0.0277P)²+0.1545P] 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         920
_refine_ls_number_parameters     82
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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      0.0753711000
_diffrn_orient_matrix_UB_12      -0.0699876000
_diffrn_orient_matrix_UB_13      -0.0215762000
_diffrn_orient_matrix_UB_21      -0.0572293000
_diffrn_orient_matrix_UB_22      0.0380366000
_diffrn_orient_matrix_UB_23      -0.0316346000
_diffrn_orient_matrix_UB_31      0.0423490000
_diffrn_orient_matrix_UB_32      0.1761106000
_diffrn_orient_matrix_UB_33      -0.0017523000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   20.00   96.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000   60.0000 76

#__ type_ start__ end____ width___ exp.time_
  2 omega   12.00  100.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega  -37.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000 -120.0000 114

#__ type_ start__ end____ width___ exp.time_
  4 omega  -87.00  -12.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  129.0000  -87.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega -111.00  -78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
  6 omega  -97.00  -71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -30.0000 26

;



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'
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
Cu01 Cu 1.0000 1.0000 0.0000 0.01260(15) Uani 1 2 d S . P . .
Cl1 Cl 0.78472(9) 0.40117(16) -0.05385(3) 0.01517(17) Uani 1 1 d . . . . .
N1 N 0.6102(3) 1.1409(6) 0.16959(11) 0.0176(5) Uani 1 1 d . . . . .
N2 N 0.7651(3) 0.9740(5) 0.19901(10) 0.0124(4) Uani 1 1 d . . . . .
N3 N 0.9005(3) 0.8873(6) 0.15386(10) 0.0143(4) Uani 1 1 d . . . . .
N4 N 0.8343(3) 1.0089(5) 0.09004(10) 0.0122(4) Uani 1 1 d . . . . .
N5 N 0.7885(4) 0.8757(7) 0.27150(11) 0.0192(5) Uani 1 1 d . . . . .
C1 C 0.6580(4) 1.1557(7) 0.10084(13) 0.0164(5) Uani 1 1 d . . . . .
H1 H 0.585(4) 1.255(8) 0.0690(14) 0.019(7) Uiso 1 1 d . . . . .
H5B H 0.838(5) 1.041(8) 0.2887(18) 0.027(10) Uiso 1 1 d . . . . .
H5A H 0.668(4) 0.810(8) 0.2901(14) 0.023(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
Cu01 N4 2.0422(19) . ?
Cu01 N4 2.0422(19) 3_775 ?
Cu01 Cl1 2.2915(6) 1_565 ?
Cu01 Cl1 2.2915(6) 3_765 ?
Cl1 Cu01 2.2914(6) 1_545 ?
N1 C1 1.324(3) . ?
N1 N2 1.328(3) . ?
N2 N3 1.305(3) . ?
N2 N5 1.395(3) . ?
N3 N4 1.331(3) . ?
N4 C1 1.342(3) . ?
N5 H5B 0.76(3) . ?
N5 H5A 0.93(3) . ?
C1 H1 0.85(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
N4 Cu01 N4 180.0 . 3_775 ?
N4 Cu01 Cl1 88.83(6) . 1_565 ?
N4 Cu01 Cl1 91.17(6) 3_775 1_565 ?
N4 Cu01 Cl1 91.17(6) . 3_765 ?
N4 Cu01 Cl1 88.83(6) 3_775 3_765 ?
Cl1 Cu01 Cl1 180.00(2) 1_565 3_765 ?
C1 N1 N2 101.39(19) . . ?
N3 N2 N1 115.02(18) . . ?
N3 N2 N5 119.3(2) . . ?
N1 N2 N5 125.7(2) . . ?
N2 N3 N4 104.87(19) . . ?
N3 N4 C1 106.73(19) . . ?
N3 N4 Cu01 122.41(15) . . ?
C1 N4 Cu01 130.58(17) . . ?
N2 N5 H5B 104(2) . . ?
N2 N5 H5A 110.0(17) . . ?
H5B N5 H5A 116(3) . . ?
N1 C1 N4 112.0(2) . . ?
N1 C1 H1 122.1(18) . . ?
N4 C1 H1 125.9(18) . . ?

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(3) . . . . ?
C1 N1 N2 N5 -177.5(2) . . . . ?
N1 N2 N3 N4 1.1(3) . . . . ?
N5 N2 N3 N4 178.6(2) . . . . ?
N2 N3 N4 C1 -1.5(2) . . . . ?
N2 N3 N4 Cu01 173.02(14) . . . . ?
N2 N1 C1 N4 -0.8(3) . . . . ?
N3 N4 C1 N1 1.5(3) . . . . ?
Cu01 N4 C1 N1 -172.39(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
N5 H5B N3 0.76(3) 2.42(3) 3.131(3) 157(3) 2_755
N5 H5B Cl1 0.76(3) 2.96(3) 3.336(2) 114(3) 4_576
N5 H5A N1 0.93(3) 2.16(3) 3.090(3) 178(3) 2_645

_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         0.398
_refine_diff_density_min         -0.435
_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_mx021
_database_code_depnum_ccdc_archive 'CCDC 1834850'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jan 17 07:57:06 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(2-aminotetrazolyl) zinc(II) diperchlorate *2 2-aminotetrazole
;
_chemical_name_common            
'hexakis(2-aminotetrazolyl) zinc(II) diperchlorate *2 2-aminotetrazole'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C6 H18 N30 Zn, 2(C H3 N5), 2(Cl O4)'
_chemical_formula_sum            'C8 H24 Cl2 N40 O8 Zn'
_chemical_formula_weight         944.94

_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                   8.5016(2)
_cell_length_b                   10.8035(3)
_cell_length_c                   19.2662(6)
_cell_angle_alpha                79.175(3)
_cell_angle_beta                 86.100(2)
_cell_angle_gamma                86.315(2)
_cell_volume                     1731.63(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3700
_cell_measurement_theta_min      4.4230
_cell_measurement_theta_max      31.4030

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.966
_shelx_estimated_absorpt_T_min   0.780
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94744
_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    1.812
_exptl_crystal_F_000             960
_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            14327
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.315
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6784
_reflns_number_gt                5317
_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)+(0.0374P)²] 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         6784
_refine_ls_number_parameters     628
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0874
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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      0.0122211000
_diffrn_orient_matrix_UB_12      0.0389470000
_diffrn_orient_matrix_UB_13      0.0247580000
_diffrn_orient_matrix_UB_21      -0.0036427000
_diffrn_orient_matrix_UB_22      0.0539959000
_diffrn_orient_matrix_UB_23      -0.0273351000
_diffrn_orient_matrix_UB_31      -0.0827641000
_diffrn_orient_matrix_UB_32      0.0069334000
_diffrn_orient_matrix_UB_33      0.0070272000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -99.00  -17.10   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -30.0000 117

#__ type_ start__ end____ width___ exp.time_
  2 omega   -6.00   41.60   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  120.0000 68

#__ type_ start__ end____ width___ exp.time_
  3 omega   -2.00   85.50   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000 -150.0000 125

#__ type_ start__ end____ width___ exp.time_
  4 omega   31.00   75.80   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -150.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega  -22.00   74.60   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 138

#__ type_ start__ end____ width___ exp.time_
  6 omega    3.00   95.40   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000   90.0000 132

#__ type_ start__ end____ width___ exp.time_
  7 omega   27.00   69.00   0.7000   37.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 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'
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 0.22840(3) 0.49834(3) 0.25448(2) 0.01600(9) Uani 1 1 d . . . . .
N1 N 0.4690(2) 0.8443(2) 0.17667(11) 0.0217(5) Uani 1 1 d . . . . .
N2 N 0.4484(2) 0.7924(2) 0.12124(11) 0.0179(5) Uani 1 1 d . . . . .
N3 N 0.3845(2) 0.6834(2) 0.13534(11) 0.0211(5) Uani 1 1 d . . . . .
N4 N 0.3602(2) 0.6596(2) 0.20592(11) 0.0187(5) Uani 1 1 d . . . . .
N5 N 0.4781(3) 0.8563(3) 0.05295(12) 0.0248(5) Uani 1 1 d . . . . .
N6 N 0.3643(2) 0.3349(2) 0.06527(11) 0.0204(5) Uani 1 1 d . . . . .
N7 N 0.3892(2) 0.2469(2) 0.12217(11) 0.0170(5) Uani 1 1 d . . . . .
N8 N 0.3574(2) 0.2839(2) 0.18269(11) 0.0186(5) Uani 1 1 d . . . . .
N9 N 0.3075(2) 0.4042(2) 0.16542(10) 0.0168(5) Uani 1 1 d . . . . .
N10 N 0.4500(3) 0.1264(2) 0.11620(13) 0.0230(5) Uani 1 1 d . . . . .
N11 N -0.0474(2) 0.1625(2) 0.30037(11) 0.0223(5) Uani 1 1 d . . . . .
N12 N -0.0246(2) 0.1862(2) 0.36334(11) 0.0186(5) Uani 1 1 d . . . . .
N13 N 0.0570(2) 0.2845(2) 0.36421(11) 0.0197(5) Uani 1 1 d . . . . .
N14 N 0.0925(2) 0.3299(2) 0.29590(10) 0.0176(5) Uani 1 1 d . . . . .
N15 N -0.0810(3) 0.1078(2) 0.42484(13) 0.0254(5) Uani 1 1 d . . . . .
N16 N 0.6872(2) 0.3641(2) 0.32396(11) 0.0231(5) Uani 1 1 d . . . . .
N17 N 0.5958(2) 0.3589(2) 0.38289(11) 0.0185(5) Uani 1 1 d . . . . .
N18 N 0.4470(2) 0.3896(2) 0.37431(11) 0.0184(5) Uani 1 1 d . . . . .
N19 N 0.4367(2) 0.4178(2) 0.30442(10) 0.0179(5) Uani 1 1 d . . . . .
N20 N 0.6565(3) 0.3145(3) 0.44816(13) 0.0268(6) Uani 1 1 d . . . . .
N21 N 0.1030(2) 0.6183(2) 0.45697(11) 0.0197(5) Uani 1 1 d . . . . .
N22 N 0.0846(2) 0.7212(2) 0.40758(10) 0.0176(5) Uani 1 1 d . . . . .
N23 N 0.1127(2) 0.7028(2) 0.34227(11) 0.0192(5) Uani 1 1 d . . . . .
N24 N 0.1523(2) 0.5807(2) 0.34856(10) 0.0174(5) Uani 1 1 d . . . . .
N25 N 0.0379(3) 0.8368(2) 0.42589(13) 0.0259(6) Uani 1 1 d . . . . .
N26 N -0.2153(2) 0.6549(2) 0.17376(11) 0.0245(5) Uani 1 1 d . . . . .
N27 N -0.1125(2) 0.6578(2) 0.11872(11) 0.0187(5) Uani 1 1 d . . . . .
N28 N 0.0311(2) 0.6189(2) 0.13345(11) 0.0205(5) Uani 1 1 d . . . . .
N29 N 0.0254(2) 0.5861(2) 0.20380(10) 0.0182(5) Uani 1 1 d . . . . .
N30 N -0.1555(4) 0.7063(3) 0.05031(13) 0.0288(6) Uani 1 1 d . . . . .
C1 C 0.4141(3) 0.7574(3) 0.22890(14) 0.0199(6) Uani 1 1 d . . . . .
C2 C 0.3121(3) 0.4326(3) 0.09410(14) 0.0196(6) Uani 1 1 d . . . . .
C3 C 0.0263(3) 0.2555(3) 0.25900(14) 0.0213(6) Uani 1 1 d . . . . .
C4 C 0.5830(3) 0.4024(3) 0.27547(14) 0.0218(6) Uani 1 1 d . . . . .
C5 C 0.1452(3) 0.5321(3) 0.41844(14) 0.0200(6) Uani 1 1 d . . . . .
C6 C -0.1234(3) 0.6087(3) 0.22591(15) 0.0228(6) Uani 1 1 d . . . . .
N31 N 0.5388(3) 0.0859(2) 0.37515(12) 0.0332(6) Uani 1 1 d . . . . .
N32 N 0.5144(2) 0.0432(2) 0.31709(11) 0.0223(5) Uani 1 1 d . . . . .
N33 N 0.3749(3) 0.0002(2) 0.31505(13) 0.0319(6) Uani 1 1 d . . . . .
N34 N 0.3005(3) 0.0130(2) 0.37647(14) 0.0356(6) Uani 1 1 d . . . . .
N35 N 0.6225(3) 0.0481(3) 0.25927(13) 0.0260(6) Uani 1 1 d . . . . .
C8 C 0.4009(4) 0.0658(3) 0.41030(18) 0.0398(8) Uani 1 1 d . . . . .
N36 N 0.8940(3) 0.9385(2) 0.17324(12) 0.0325(6) Uani 1 1 d . . . . .
N37 N 0.9052(2) 0.9875(2) 0.10558(12) 0.0235(5) Uani 1 1 d . . . . .
N38 N 1.0466(3) 1.0239(3) 0.08155(13) 0.0356(6) Uani 1 1 d . . . . .
N39 N 1.1359(3) 0.9965(3) 0.13674(13) 0.0401(7) Uani 1 1 d . . . . .
N40 N 0.7775(3) 1.0002(3) 0.06279(14) 0.0276(6) Uani 1 1 d . . . . .
C7 C 1.0404(4) 0.9460(3) 0.19114(17) 0.0369(8) Uani 1 1 d . . . . .
Cl1 Cl 0.34026(8) 0.29422(7) 0.59661(3) 0.02616(16) Uani 1 1 d . . . . .
O1 O 0.5038(2) 0.3116(3) 0.60053(12) 0.0631(8) Uani 1 1 d . . . . .
O2 O 0.2496(3) 0.4104(2) 0.59684(13) 0.0532(6) Uani 1 1 d . . . . .
O3 O 0.2845(3) 0.2050(2) 0.65533(13) 0.0599(7) Uani 1 1 d . . . . .
O4 O 0.3172(3) 0.2525(3) 0.53261(13) 0.0637(8) Uani 1 1 d . . . . .
Cl2 Cl 0.80220(7) 0.33602(6) 0.08634(3) 0.02244(15) Uani 1 1 d . . . . .
O5 O 0.7692(2) 0.2371(2) 0.14533(10) 0.0367(5) Uani 1 1 d . . . . .
O6 O 0.7751(2) 0.2941(2) 0.02200(10) 0.0363(5) Uani 1 1 d . . . . .
O7 O 0.9635(2) 0.3675(2) 0.08540(12) 0.0447(6) Uani 1 1 d . . . . .
O8 O 0.7003(3) 0.4443(2) 0.09324(12) 0.0452(6) Uani 1 1 d . . . . .
H2 H 0.281(3) 0.511(3) 0.0682(13) 0.018(7) Uiso 1 1 d . . . . .
H4 H 0.608(3) 0.410(3) 0.2291(14) 0.024(7) Uiso 1 1 d . . . . .
H1 H 0.409(3) 0.769(2) 0.2753(14) 0.020(7) Uiso 1 1 d . . . . .
H3 H 0.030(3) 0.265(2) 0.2110(14) 0.016(7) Uiso 1 1 d . . . . .
H10B H 0.510(4) 0.096(3) 0.1535(16) 0.039(9) Uiso 1 1 d . . . . .
H10A H 0.370(4) 0.079(3) 0.1229(16) 0.042(10) Uiso 1 1 d . . . . .
H6 H -0.157(3) 0.598(3) 0.2669(15) 0.028(8) Uiso 1 1 d . . . . .
H8 H 0.380(3) 0.089(3) 0.4516(16) 0.034(8) Uiso 1 1 d . . . . .
H20A H 0.584(4) 0.308(3) 0.4767(17) 0.038(10) Uiso 1 1 d . . . . .
H20B H 0.716(4) 0.367(3) 0.4528(15) 0.031(9) Uiso 1 1 d . . . . .
H7 H 1.077(3) 0.921(3) 0.2356(16) 0.039(9) Uiso 1 1 d . . . . .
H35A H 0.657(3) -0.023(3) 0.2569(15) 0.029(9) Uiso 1 1 d . . . . .
H25A H 0.103(3) 0.887(3) 0.4071(15) 0.029(9) Uiso 1 1 d . . . . .
H30B H -0.219(4) 0.661(3) 0.0427(16) 0.040(10) Uiso 1 1 d . . . . .
H5A H 0.481(3) 0.805(3) 0.0275(15) 0.027(9) Uiso 1 1 d . . . . .
H25B H -0.054(4) 0.855(3) 0.4116(15) 0.033(9) Uiso 1 1 d . . . . .
H5B H 0.573(3) 0.885(3) 0.0532(14) 0.029(8) Uiso 1 1 d . . . . .
H40A H 0.740(4) 1.070(3) 0.0619(18) 0.044(11) Uiso 1 1 d . . . . .
H40B H 0.816(4) 0.992(3) 0.0187(19) 0.053(11) Uiso 1 1 d . . . . .
H30A H -0.073(4) 0.702(4) 0.0232(19) 0.057(12) Uiso 1 1 d . . . . .
H35B H 0.694(4) 0.094(4) 0.2647(18) 0.057(11) Uiso 1 1 d . . . . .
H15B H -0.040(3) 0.135(3) 0.4597(17) 0.037(9) Uiso 1 1 d . . . . .
H5 H 0.171(3) 0.451(3) 0.4365(14) 0.028(8) Uiso 1 1 d . . . . .
H15A H -0.176(4) 0.126(4) 0.4280(18) 0.053(12) 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
Zn1 N29 2.122(2) . ?
Zn1 N19 2.130(2) . ?
Zn1 N4 2.159(2) . ?
Zn1 N9 2.200(2) . ?
Zn1 N24 2.206(2) . ?
Zn1 N14 2.209(2) . ?
N1 N2 1.322(3) . ?
N1 C1 1.323(3) . ?
N2 N3 1.304(3) . ?
N2 N5 1.381(3) . ?
N3 N4 1.340(3) . ?
N4 C1 1.337(3) . ?
N5 H5A 0.80(3) . ?
N5 H5B 0.89(3) . ?
N6 C2 1.321(3) . ?
N6 N7 1.329(3) . ?
N7 N8 1.308(3) . ?
N7 N10 1.392(3) . ?
N8 N9 1.329(3) . ?
N9 C2 1.349(3) . ?
N10 H10B 0.91(3) . ?
N10 H10A 0.86(3) . ?
N11 N12 1.315(3) . ?
N11 C3 1.322(3) . ?
N12 N13 1.309(3) . ?
N12 N15 1.396(3) . ?
N13 N14 1.336(3) . ?
N14 C3 1.340(3) . ?
N15 H15B 0.88(3) . ?
N15 H15A 0.82(4) . ?
N16 C4 1.323(3) . ?
N16 N17 1.326(3) . ?
N17 N18 1.301(3) . ?
N17 N20 1.381(3) . ?
N18 N19 1.331(3) . ?
N19 C4 1.342(3) . ?
N20 H20A 0.80(3) . ?
N20 H20B 0.80(3) . ?
N21 C5 1.314(3) . ?
N21 N22 1.329(3) . ?
N22 N23 1.314(3) . ?
N22 N25 1.388(3) . ?
N23 N24 1.325(3) . ?
N24 C5 1.349(3) . ?
N25 H25A 0.82(3) . ?
N25 H25B 0.84(3) . ?
N26 C6 1.318(4) . ?
N26 N27 1.325(3) . ?
N27 N28 1.297(3) . ?
N27 N30 1.388(3) . ?
N28 N29 1.333(3) . ?
N29 C6 1.329(3) . ?
N30 H30B 0.79(3) . ?
N30 H30A 0.85(4) . ?
C1 H1 0.92(3) . ?
C2 H2 0.93(3) . ?
C3 H3 0.91(2) . ?
C4 H4 0.89(3) . ?
C5 H5 0.90(3) . ?
C6 H6 0.81(3) . ?
N31 N32 1.321(3) . ?
N31 C8 1.323(4) . ?
N32 N33 1.308(3) . ?
N32 N35 1.390(3) . ?
N33 N34 1.329(3) . ?
N34 C8 1.325(4) . ?
N35 H35A 0.81(3) . ?
N35 H35B 0.84(3) . ?
C8 H8 0.88(3) . ?
N36 N37 1.311(3) . ?
N36 C7 1.325(4) . ?
N37 N38 1.316(3) . ?
N37 N40 1.392(3) . ?
N38 N39 1.325(3) . ?
N39 C7 1.335(4) . ?
N40 H40A 0.80(4) . ?
N40 H40B 0.91(4) . ?
C7 H7 0.92(3) . ?
Cl1 O3 1.418(2) . ?
Cl1 O4 1.419(2) . ?
Cl1 O1 1.424(2) . ?
Cl1 O2 1.431(3) . ?
Cl2 O8 1.432(2) . ?
Cl2 O7 1.4323(19) . ?
Cl2 O5 1.432(2) . ?
Cl2 O6 1.4348(18) . ?

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
N29 Zn1 N19 177.55(7) . . ?
N29 Zn1 N4 89.30(8) . . ?
N19 Zn1 N4 88.34(8) . . ?
N29 Zn1 N9 93.17(8) . . ?
N19 Zn1 N9 87.49(8) . . ?
N4 Zn1 N9 89.59(7) . . ?
N29 Zn1 N24 89.49(8) . . ?
N19 Zn1 N24 89.97(8) . . ?
N4 Zn1 N24 93.15(8) . . ?
N9 Zn1 N24 176.20(8) . . ?
N29 Zn1 N14 89.03(8) . . ?
N19 Zn1 N14 93.37(8) . . ?
N4 Zn1 N14 175.56(7) . . ?
N9 Zn1 N14 86.40(7) . . ?
N24 Zn1 N14 90.94(7) . . ?
N2 N1 C1 101.04(19) . . ?
N3 N2 N1 115.5(2) . . ?
N3 N2 N5 122.6(2) . . ?
N1 N2 N5 121.5(2) . . ?
N2 N3 N4 104.61(19) . . ?
C1 N4 N3 106.2(2) . . ?
C1 N4 Zn1 134.71(17) . . ?
N3 N4 Zn1 118.61(14) . . ?
N2 N5 H5A 107(2) . . ?
N2 N5 H5B 104.5(18) . . ?
H5A N5 H5B 110(3) . . ?
C2 N6 N7 101.7(2) . . ?
N8 N7 N6 114.9(2) . . ?
N8 N7 N10 123.7(2) . . ?
N6 N7 N10 121.3(2) . . ?
N7 N8 N9 104.8(2) . . ?
N8 N9 C2 106.8(2) . . ?
N8 N9 Zn1 115.82(15) . . ?
C2 N9 Zn1 137.27(18) . . ?
N7 N10 H10B 109(2) . . ?
N7 N10 H10A 106(2) . . ?
H10B N10 H10A 104(3) . . ?
N12 N11 C3 101.10(19) . . ?
N13 N12 N11 115.86(19) . . ?
N13 N12 N15 123.0(2) . . ?
N11 N12 N15 121.1(2) . . ?
N12 N13 N14 104.17(18) . . ?
N13 N14 C3 106.5(2) . . ?
N13 N14 Zn1 125.63(15) . . ?
C3 N14 Zn1 127.90(17) . . ?
N12 N15 H15B 105(2) . . ?
N12 N15 H15A 105(3) . . ?
H15B N15 H15A 106(3) . . ?
C4 N16 N17 101.0(2) . . ?
N18 N17 N16 115.7(2) . . ?
N18 N17 N20 123.5(2) . . ?
N16 N17 N20 120.7(2) . . ?
N17 N18 N19 104.43(18) . . ?
N18 N19 C4 106.8(2) . . ?
N18 N19 Zn1 123.60(15) . . ?
C4 N19 Zn1 128.99(18) . . ?
N17 N20 H20A 107(2) . . ?
N17 N20 H20B 104(2) . . ?
H20A N20 H20B 113(3) . . ?
C5 N21 N22 101.7(2) . . ?
N23 N22 N21 114.7(2) . . ?
N23 N22 N25 124.4(2) . . ?
N21 N22 N25 120.9(2) . . ?
N22 N23 N24 104.8(2) . . ?
N23 N24 C5 106.7(2) . . ?
N23 N24 Zn1 120.65(15) . . ?
C5 N24 Zn1 132.48(18) . . ?
N22 N25 H25A 107(2) . . ?
N22 N25 H25B 106(2) . . ?
H25A N25 H25B 114(3) . . ?
C6 N26 N27 100.4(2) . . ?
N28 N27 N26 115.7(2) . . ?
N28 N27 N30 122.7(2) . . ?
N26 N27 N30 121.4(2) . . ?
N27 N28 N29 104.50(19) . . ?
C6 N29 N28 106.3(2) . . ?
C6 N29 Zn1 133.99(18) . . ?
N28 N29 Zn1 119.39(15) . . ?
N27 N30 H30B 105(2) . . ?
N27 N30 H30A 107(3) . . ?
H30B N30 H30A 111(3) . . ?
N1 C1 N4 112.6(2) . . ?
N1 C1 H1 121.2(16) . . ?
N4 C1 H1 126.0(16) . . ?
N6 C2 N9 111.8(2) . . ?
N6 C2 H2 124.0(16) . . ?
N9 C2 H2 124.2(16) . . ?
N11 C3 N14 112.4(2) . . ?
N11 C3 H3 121.9(15) . . ?
N14 C3 H3 125.7(15) . . ?
N16 C4 N19 112.1(2) . . ?
N16 C4 H4 122.7(17) . . ?
N19 C4 H4 125.0(17) . . ?
N21 C5 N24 112.1(3) . . ?
N21 C5 H5 124.2(18) . . ?
N24 C5 H5 123.7(18) . . ?
N26 C6 N29 113.1(2) . . ?
N26 C6 H6 121(2) . . ?
N29 C6 H6 125(2) . . ?
N32 N31 C8 100.2(2) . . ?
N33 N32 N31 115.3(2) . . ?
N33 N32 N35 120.3(2) . . ?
N31 N32 N35 124.3(2) . . ?
N32 N33 N34 105.0(2) . . ?
C8 N34 N33 105.8(2) . . ?
N32 N35 H35A 109(2) . . ?
N32 N35 H35B 108(2) . . ?
H35A N35 H35B 112(3) . . ?
N31 C8 N34 113.7(3) . . ?
N31 C8 H8 121.2(18) . . ?
N34 C8 H8 125.0(18) . . ?
N37 N36 C7 101.3(2) . . ?
N36 N37 N38 114.6(2) . . ?
N36 N37 N40 122.6(2) . . ?
N38 N37 N40 122.8(2) . . ?
N37 N38 N39 105.5(2) . . ?
N38 N39 C7 105.6(2) . . ?
N37 N40 H40A 106(2) . . ?
N37 N40 H40B 108(2) . . ?
H40A N40 H40B 110(3) . . ?
N36 C7 N39 113.0(3) . . ?
N36 C7 H7 125.9(19) . . ?
N39 C7 H7 121.1(19) . . ?
O3 Cl1 O4 110.07(17) . . ?
O3 Cl1 O1 110.76(16) . . ?
O4 Cl1 O1 109.06(15) . . ?
O3 Cl1 O2 107.90(14) . . ?
O4 Cl1 O2 108.37(17) . . ?
O1 Cl1 O2 110.65(16) . . ?
O8 Cl2 O7 109.68(14) . . ?
O8 Cl2 O5 108.93(13) . . ?
O7 Cl2 O5 109.54(13) . . ?
O8 Cl2 O6 109.93(14) . . ?
O7 Cl2 O6 109.50(13) . . ?
O5 Cl2 O6 109.26(12) . . ?

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 0.9(3) . . . . ?
C1 N1 N2 N5 174.5(2) . . . . ?
N1 N2 N3 N4 -0.1(3) . . . . ?
N5 N2 N3 N4 -173.7(2) . . . . ?
N2 N3 N4 C1 -0.7(3) . . . . ?
N2 N3 N4 Zn1 172.43(16) . . . . ?
C2 N6 N7 N8 -0.5(3) . . . . ?
C2 N6 N7 N10 -178.3(2) . . . . ?
N6 N7 N8 N9 0.2(2) . . . . ?
N10 N7 N8 N9 178.0(2) . . . . ?
N7 N8 N9 C2 0.2(2) . . . . ?
N7 N8 N9 Zn1 176.57(13) . . . . ?
C3 N11 N12 N13 -0.4(3) . . . . ?
C3 N11 N12 N15 -178.6(2) . . . . ?
N11 N12 N13 N14 -0.4(3) . . . . ?
N15 N12 N13 N14 177.8(2) . . . . ?
N12 N13 N14 C3 1.0(3) . . . . ?
N12 N13 N14 Zn1 179.45(16) . . . . ?
C4 N16 N17 N18 0.4(3) . . . . ?
C4 N16 N17 N20 175.9(2) . . . . ?
N16 N17 N18 N19 -0.1(3) . . . . ?
N20 N17 N18 N19 -175.5(2) . . . . ?
N17 N18 N19 C4 -0.3(3) . . . . ?
N17 N18 N19 Zn1 -171.98(15) . . . . ?
C5 N21 N22 N23 0.0(3) . . . . ?
C5 N21 N22 N25 179.5(2) . . . . ?
N21 N22 N23 N24 -0.1(3) . . . . ?
N25 N22 N23 N24 -179.6(2) . . . . ?
N22 N23 N24 C5 0.2(2) . . . . ?
N22 N23 N24 Zn1 -175.86(13) . . . . ?
C6 N26 N27 N28 -0.6(3) . . . . ?
C6 N26 N27 N30 -177.1(2) . . . . ?
N26 N27 N28 N29 0.5(3) . . . . ?
N30 N27 N28 N29 177.0(2) . . . . ?
N27 N28 N29 C6 -0.2(3) . . . . ?
N27 N28 N29 Zn1 173.99(15) . . . . ?
N2 N1 C1 N4 -1.3(3) . . . . ?
N3 N4 C1 N1 1.3(3) . . . . ?
Zn1 N4 C1 N1 -170.19(18) . . . . ?
N7 N6 C2 N9 0.6(3) . . . . ?
N8 N9 C2 N6 -0.5(3) . . . . ?
Zn1 N9 C2 N6 -175.74(16) . . . . ?
N12 N11 C3 N14 1.1(3) . . . . ?
N13 N14 C3 N11 -1.4(3) . . . . ?
Zn1 N14 C3 N11 -179.77(17) . . . . ?
N17 N16 C4 N19 -0.6(3) . . . . ?
N18 N19 C4 N16 0.6(3) . . . . ?
Zn1 N19 C4 N16 171.67(17) . . . . ?
N22 N21 C5 N24 0.1(3) . . . . ?
N23 N24 C5 N21 -0.2(3) . . . . ?
Zn1 N24 C5 N21 175.17(16) . . . . ?
N27 N26 C6 N29 0.5(3) . . . . ?
N28 N29 C6 N26 -0.2(3) . . . . ?
Zn1 N29 C6 N26 -173.13(18) . . . . ?
C8 N31 N32 N33 0.1(3) . . . . ?
C8 N31 N32 N35 176.7(3) . . . . ?
N31 N32 N33 N34 -0.9(3) . . . . ?
N35 N32 N33 N34 -177.7(3) . . . . ?
N32 N33 N34 C8 1.3(3) . . . . ?
N32 N31 C8 N34 0.8(4) . . . . ?
N33 N34 C8 N31 -1.4(4) . . . . ?
C7 N36 N37 N38 -0.1(3) . . . . ?
C7 N36 N37 N40 -179.9(3) . . . . ?
N36 N37 N38 N39 0.5(3) . . . . ?
N40 N37 N38 N39 -179.7(3) . . . . ?
N37 N38 N39 C7 -0.7(3) . . . . ?
N37 N36 C7 N39 -0.3(3) . . . . ?
N38 N39 C7 N36 0.7(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
N10 H10B N35 0.91(3) 2.27(3) 3.159(4) 167(3) .
N10 H10A N39 0.86(3) 2.21(3) 3.064(3) 168(3) 1_445
N20 H20A O1 0.80(3) 2.44(3) 3.124(3) 144(3) .
N20 H20A O4 0.80(3) 2.50(3) 3.258(4) 159(3) .
N20 H20A Cl1 0.80(3) 2.98(3) 3.775(3) 172(3) .
N20 H20B N21 0.80(3) 2.43(3) 3.041(3) 133(3) 2_666
N20 H20B O2 0.80(3) 2.44(3) 3.077(4) 136(3) 2_666
N35 H35A O3 0.81(3) 2.39(3) 3.003(4) 133(3) 2_656
N35 H35A N36 0.81(3) 2.56(3) 3.057(3) 121(2) 1_545
N25 H25A N34 0.82(3) 2.21(3) 3.015(4) 169(3) 1_565
N30 H30B N6 0.79(3) 2.48(3) 3.053(3) 130(3) 2_565
N30 H30B O8 0.79(3) 2.48(3) 3.102(4) 137(3) 1_455
N25 H25B O3 0.84(3) 2.60(3) 3.343(4) 148(3) 2_566
N25 H25B O4 0.84(3) 2.65(3) 3.232(4) 127(3) 2_566
N5 H5B N40 0.89(3) 2.24(3) 3.101(3) 165(3) .
N40 H40A O6 0.80(4) 2.43(4) 3.123(4) 146(3) 1_565
N40 H40A O5 0.80(4) 2.67(3) 3.252(4) 132(3) 1_565
N40 H40A N10 0.80(4) 2.69(3) 3.213(4) 125(3) 1_565
N40 H40B N38 0.91(4) 2.22(4) 3.113(4) 169(3) 2_775
N30 H30A O7 0.85(4) 2.46(4) 3.189(3) 144(3) 2_665
N30 H30A O6 0.85(4) 2.62(4) 3.434(4) 160(3) 2_665
N35 H35B N11 0.84(3) 2.54(3) 3.339(3) 161(3) 1_655
N15 H15B N25 0.88(3) 2.28(3) 3.095(4) 153(2) 2_566
N15 H15A N20 0.82(4) 2.49(4) 3.125(4) 136(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         0.394
_refine_diff_density_min         -0.403
_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_lx623
_database_code_depnum_ccdc_archive 'CCDC 1834847'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sun Dec 25 08:56:57 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-aminotetrazolyl)iron(II) perchlorate
;
_chemical_name_common            
'hexakis(1-aminotetrazolyl)iron(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Fe N30, 2(Cl O4)'
_chemical_formula_sum            'C6 H18 Cl2 Fe N30 O8'
_chemical_formula_weight         765.25

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'




_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, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   18.8934(4)
_cell_length_b                   18.8934(4)
_cell_length_c                   6.9830(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2158.70(13)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5645
_cell_measurement_theta_min      4.3910
_cell_measurement_theta_max      32.1660

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.802
_shelx_estimated_absorpt_T_min   0.690
_shelx_estimated_absorpt_T_max   0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92266
_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    1.766
_exptl_crystal_F_000             1164
_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            16975
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.315
_diffrn_reflns_theta_max         26.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2898
_reflns_number_gt                2492
_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)+(0.1137P)²+3.8766P] 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         2898
_refine_ls_number_parameters     286
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1923
_refine_ls_wR_factor_gt          0.1799
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0387203000
_diffrn_orient_matrix_UB_12      0.0024937000
_diffrn_orient_matrix_UB_13      0.0000490000
_diffrn_orient_matrix_UB_21      -0.0123656000
_diffrn_orient_matrix_UB_22      -0.0275046000
_diffrn_orient_matrix_UB_23      0.0784505000
_diffrn_orient_matrix_UB_31      -0.0150192000
_diffrn_orient_matrix_UB_32      -0.0334027000
_diffrn_orient_matrix_UB_33      -0.0645771000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -109.00  -80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
  2 omega  -81.00  -45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega  -24.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 99

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega    5.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000   60.0000 124

;



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
Fe2 Fe 0.6667 0.3333 0.01628(10) 0.0193(3) Uani 1 3 d S T P . .
N1 N 0.45334(17) 0.17124(17) 0.3398(4) 0.0279(6) Uani 1 1 d . . . . .
N2 N 0.50256(19) 0.14128(18) 0.3799(5) 0.0383(7) Uani 1 1 d . . . . .
N3 N 0.57082(18) 0.18731(18) 0.2913(5) 0.0360(7) Uani 1 1 d . . . . .
N4 N 0.56567(16) 0.24718(16) 0.1942(4) 0.0266(6) Uani 1 1 d . . . . .
N5 N 0.3735(2) 0.1376(2) 0.4090(6) 0.0439(8) Uani 1 1 d D . . . .
N6 N 0.50086(17) 0.37914(19) -0.3065(4) 0.0299(6) Uani 1 1 d D . . . .
N7 N 0.46835(19) 0.2988(2) -0.3312(5) 0.0420(8) Uani 1 1 d . . . . .
N8 N 0.51566(19) 0.27839(18) -0.2443(5) 0.0396(7) Uani 1 1 d . . . . .
N9 N 0.57871(16) 0.34526(16) -0.1609(4) 0.0266(6) Uani 1 1 d . . . . .
N10 N 0.4650(3) 0.4229(3) -0.3765(7) 0.0637(13) Uani 1 1 d D . . . .
C1 C 0.4923(2) 0.2360(2) 0.2284(5) 0.0300(7) Uani 1 1 d . . . . .
C2 C 0.5683(2) 0.4070(2) -0.2032(5) 0.0286(7) Uani 1 1 d . . . . .
Fe1 Fe 0.0000 0.0000 0.0000 0.0208(3) Uani 1 6 d S T P . .
N11 N 0.05711(17) 0.21411(17) 0.3298(4) 0.0286(6) Uani 1 1 d . . . . .
N12 N 0.1198(2) 0.2033(2) 0.3774(5) 0.0472(9) Uani 1 1 d . . . . .
N13 N 0.1097(2) 0.1400(2) 0.2839(5) 0.0444(8) Uani 1 1 d . . . . .
N14 N 0.04028(17) 0.10887(16) 0.1771(4) 0.0281(6) Uani 1 1 d . . . . .
N15 N 0.0451(2) 0.2759(2) 0.4056(6) 0.0445(8) Uani 1 1 d . . . . .
C3 C 0.0095(2) 0.1563(2) 0.2086(5) 0.0322(7) Uani 1 1 d . . . . .
Cl1 Cl 0.34522(10) 0.34740(8) 0.09558(17) 0.0596(4) Uani 1 1 d . . . . .
O1A O 0.4134(17) 0.3501(16) 0.159(6) 0.276(18) Uani 0.448(12) 1 d . . P A 1
O2A O 0.4193(18) 0.4231(12) 0.038(4) 0.234(16) Uani 0.448(12) 1 d . . P A 1
O3A O 0.3187(9) 0.3924(7) 0.196(3) 0.114(6) Uani 0.448(12) 1 d . . P A 1
O4A O 0.2605(16) 0.3225(10) 0.032(2) 0.165(10) Uani 0.448(12) 1 d . . P A 1
O1B O 0.3669(11) 0.2961(9) 0.0207(13) 0.122(5) Uani 0.552(12) 1 d . . P A 2
O2B O 0.3519(8) 0.4034(8) -0.0334(13) 0.106(4) Uani 0.552(12) 1 d . . P A 2
O3B O 0.3454(8) 0.3596(10) 0.2820(11) 0.130(6) Uani 0.552(12) 1 d . . P A 2
O4B O 0.2846(12) 0.2707(8) 0.118(2) 0.216(12) Uani 0.552(12) 1 d . . P A 2
H1 H 0.471(3) 0.266(3) 0.192(6) 0.035(10) Uiso 1 1 d . . . . .
H2 H 0.597(3) 0.457(3) -0.179(6) 0.049(13) Uiso 1 1 d . . . . .
H3 H -0.038(3) 0.151(3) 0.157(6) 0.047(12) Uiso 1 1 d . . . . .
H15A H 0.090(3) 0.320(3) 0.399(8) 0.057(14) Uiso 1 1 d . . . . .
H15B H 0.056(4) 0.276(4) 0.525(9) 0.08(2) Uiso 1 1 d . . . . .
H5A H 0.344(3) 0.0932(17) 0.367(6) 0.056(15) Uiso 1 1 d D . . . .
H10A H 0.424(3) 0.413(5) -0.322(8) 0.13(3) Uiso 1 1 d D . . . .
H5B H 0.371(3) 0.124(3) 0.519(3) 0.055(15) Uiso 1 1 d D . . . .
H10B H 0.447(3) 0.405(3) -0.479(4) 0.08(2) Uiso 1 1 d 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
Fe2 N9 2.172(3) 2_655 ?
Fe2 N9 2.172(3) 3_665 ?
Fe2 N9 2.172(3) . ?
Fe2 N4 2.174(3) . ?
Fe2 N4 2.174(3) 2_655 ?
Fe2 N4 2.174(3) 3_665 ?
N1 C1 1.321(4) . ?
N1 N2 1.338(4) . ?
N1 N5 1.397(4) . ?
N2 N3 1.296(4) . ?
N3 N4 1.364(4) . ?
N4 C1 1.315(4) . ?
N5 H5A 0.795(19) . ?
N5 H5B 0.805(19) . ?
N6 C2 1.323(4) . ?
N6 N7 1.333(5) . ?
N6 N10 1.394(4) . ?
N7 N8 1.289(4) . ?
N8 N9 1.360(4) . ?
N9 C2 1.309(4) . ?
N10 H10A 0.79(2) . ?
N10 H10B 0.789(19) . ?
C1 H1 0.88(4) . ?
C2 H2 0.85(5) . ?
Fe1 N14 2.185(3) 4 ?
Fe1 N14 2.185(3) 6 ?
Fe1 N14 2.185(3) 3 ?
Fe1 N14 2.185(3) 2 ?
Fe1 N14 2.185(3) 5 ?
Fe1 N14 2.185(3) . ?
N11 C3 1.318(4) . ?
N11 N12 1.341(4) . ?
N11 N15 1.400(4) . ?
N12 N13 1.290(4) . ?
N13 N14 1.361(4) . ?
N14 C3 1.308(4) . ?
N15 H15A 0.84(6) . ?
N15 H15B 0.86(6) . ?
C3 H3 0.92(4) . ?
Cl1 O3B 1.322(8) . ?
Cl1 O1B 1.333(9) . ?
Cl1 O4B 1.333(11) . ?
Cl1 O1A 1.340(15) . ?
Cl1 O2B 1.346(7) . ?
Cl1 O3A 1.375(11) . ?
Cl1 O2A 1.471(17) . ?
Cl1 O4A 1.49(3) . ?
O1A O2A 1.57(4) . ?
O3A O4A 1.67(3) . ?
O1B O4B 1.54(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
N9 Fe2 N9 90.77(10) 2_655 3_665 ?
N9 Fe2 N9 90.77(10) 2_655 . ?
N9 Fe2 N9 90.77(10) 3_665 . ?
N9 Fe2 N4 90.23(10) 2_655 . ?
N9 Fe2 N4 178.72(9) 3_665 . ?
N9 Fe2 N4 88.42(10) . . ?
N9 Fe2 N4 88.42(10) 2_655 2_655 ?
N9 Fe2 N4 90.23(10) 3_665 2_655 ?
N9 Fe2 N4 178.72(9) . 2_655 ?
N4 Fe2 N4 90.60(10) . 2_655 ?
N9 Fe2 N4 178.72(9) 2_655 3_665 ?
N9 Fe2 N4 88.42(10) 3_665 3_665 ?
N9 Fe2 N4 90.23(10) . 3_665 ?
N4 Fe2 N4 90.60(10) . 3_665 ?
N4 Fe2 N4 90.60(10) 2_655 3_665 ?
C1 N1 N2 109.4(3) . . ?
C1 N1 N5 126.8(3) . . ?
N2 N1 N5 123.8(3) . . ?
N3 N2 N1 106.6(3) . . ?
N2 N3 N4 109.5(3) . . ?
C1 N4 N3 106.4(3) . . ?
C1 N4 Fe2 133.1(2) . . ?
N3 N4 Fe2 120.4(2) . . ?
N1 N5 H5A 112(4) . . ?
N1 N5 H5B 110(4) . . ?
H5A N5 H5B 97(3) . . ?
C2 N6 N7 109.1(3) . . ?
C2 N6 N10 127.8(4) . . ?
N7 N6 N10 123.1(3) . . ?
N8 N7 N6 106.6(3) . . ?
N7 N8 N9 109.9(3) . . ?
C2 N9 N8 106.2(3) . . ?
C2 N9 Fe2 133.2(2) . . ?
N8 N9 Fe2 120.5(2) . . ?
N6 N10 H10A 113(6) . . ?
N6 N10 H10B 108(2) . . ?
H10A N10 H10B 100(3) . . ?
N4 C1 N1 108.1(3) . . ?
N4 C1 H1 129(3) . . ?
N1 C1 H1 123(3) . . ?
N9 C2 N6 108.2(3) . . ?
N9 C2 H2 131(3) . . ?
N6 C2 H2 121(3) . . ?
N14 Fe1 N14 91.12(10) 4 6 ?
N14 Fe1 N14 88.88(10) 4 3 ?
N14 Fe1 N14 180.00(16) 6 3 ?
N14 Fe1 N14 88.88(10) 4 2 ?
N14 Fe1 N14 88.88(10) 6 2 ?
N14 Fe1 N14 91.12(10) 3 2 ?
N14 Fe1 N14 91.12(10) 4 5 ?
N14 Fe1 N14 91.12(10) 6 5 ?
N14 Fe1 N14 88.88(10) 3 5 ?
N14 Fe1 N14 180.0(3) 2 5 ?
N14 Fe1 N14 180.00(17) 4 . ?
N14 Fe1 N14 88.88(10) 6 . ?
N14 Fe1 N14 91.12(10) 3 . ?
N14 Fe1 N14 91.12(10) 2 . ?
N14 Fe1 N14 88.88(10) 5 . ?
C3 N11 N12 108.8(3) . . ?
C3 N11 N15 127.3(3) . . ?
N12 N11 N15 123.9(3) . . ?
N13 N12 N11 106.4(3) . . ?
N12 N13 N14 110.0(3) . . ?
C3 N14 N13 105.9(3) . . ?
C3 N14 Fe1 132.5(2) . . ?
N13 N14 Fe1 121.6(2) . . ?
N11 N15 H15A 108(4) . . ?
N11 N15 H15B 104(4) . . ?
H15A N15 H15B 86(5) . . ?
N14 C3 N11 108.8(3) . . ?
N14 C3 H3 127(3) . . ?
N11 C3 H3 124(3) . . ?
O3B Cl1 O1B 122.6(9) . . ?
O3B Cl1 O4B 90.0(9) . . ?
O1B Cl1 O4B 70.4(12) . . ?
O3B Cl1 O2B 122.0(10) . . ?
O1B Cl1 O2B 111.5(6) . . ?
O4B Cl1 O2B 128.7(11) . . ?
O1A Cl1 O3A 116.6(16) . . ?
O1A Cl1 O2A 68(2) . . ?
O3A Cl1 O2A 90.1(10) . . ?
O1A Cl1 O4A 166.0(13) . . ?
O3A Cl1 O4A 71.4(10) . . ?
O2A Cl1 O4A 125.1(17) . . ?
Cl1 O1A O2A 60.0(12) . . ?
Cl1 O2A O1A 52.1(12) . . ?
Cl1 O3A O4A 57.6(9) . . ?
Cl1 O4A O3A 51.1(9) . . ?
Cl1 O1B O4B 54.8(7) . . ?
Cl1 O4B O1B 54.8(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 -0.6(4) . . . . ?
N5 N1 N2 N3 179.7(3) . . . . ?
N1 N2 N3 N4 0.1(4) . . . . ?
N2 N3 N4 C1 0.5(4) . . . . ?
N2 N3 N4 Fe2 -177.0(2) . . . . ?
C2 N6 N7 N8 -0.1(4) . . . . ?
N10 N6 N7 N8 -178.2(3) . . . . ?
N6 N7 N8 N9 0.6(4) . . . . ?
N7 N8 N9 C2 -0.9(4) . . . . ?
N7 N8 N9 Fe2 175.6(2) . . . . ?
N3 N4 C1 N1 -0.8(4) . . . . ?
Fe2 N4 C1 N1 176.2(2) . . . . ?
N2 N1 C1 N4 0.9(4) . . . . ?
N5 N1 C1 N4 -179.4(3) . . . . ?
N8 N9 C2 N6 0.8(4) . . . . ?
Fe2 N9 C2 N6 -175.1(2) . . . . ?
N7 N6 C2 N9 -0.5(4) . . . . ?
N10 N6 C2 N9 177.5(3) . . . . ?
C3 N11 N12 N13 0.5(4) . . . . ?
N15 N11 N12 N13 178.4(4) . . . . ?
N11 N12 N13 N14 -0.6(5) . . . . ?
N12 N13 N14 C3 0.5(4) . . . . ?
N12 N13 N14 Fe1 -179.1(3) . . . . ?
N13 N14 C3 N11 -0.2(4) . . . . ?
Fe1 N14 C3 N11 179.4(2) . . . . ?
N12 N11 C3 N14 -0.2(4) . . . . ?
N15 N11 C3 N14 -178.0(3) . . . . ?
O3B Cl1 O1A O2A -107.8(12) . . . . ?
O1B Cl1 O1A O2A 111.1(19) . . . . ?
O4B Cl1 O1A O2A 166.6(12) . . . . ?
O2B Cl1 O1A O2A 11.0(17) . . . . ?
O3A Cl1 O1A O2A -78.3(18) . . . . ?
O4A Cl1 O1A O2A 159(7) . . . . ?
O3B Cl1 O2A O1A 69.5(17) . . . . ?
O1B Cl1 O2A O1A -55.4(16) . . . . ?
O4B Cl1 O2A O1A -70(8) . . . . ?
O2B Cl1 O2A O1A -168(2) . . . . ?
O3A Cl1 O2A O1A 118.9(19) . . . . ?
O4A Cl1 O2A O1A -174.0(18) . . . . ?
O3B Cl1 O3A O4A -129.2(12) . . . . ?
O4B Cl1 O3A O4A -50.6(11) . . . . ?
O1A Cl1 O3A O4A -167(2) . . . . ?
O2B Cl1 O3A O4A 76.5(9) . . . . ?
O2A Cl1 O3A O4A 127.3(18) . . . . ?
O3B Cl1 O4A O3A 38.0(9) . . . . ?
O1B Cl1 O4A O3A 170.9(10) . . . . ?
O4B Cl1 O4A O3A 119.0(13) . . . . ?
O1A Cl1 O4A O3A 127(8) . . . . ?
O2B Cl1 O4A O3A -81.5(10) . . . . ?
O2A Cl1 O4A O3A -76.4(13) . . . . ?
O3B Cl1 O1B O4B 76.9(14) . . . . ?
O1A Cl1 O1B O4B 123(2) . . . . ?
O2B Cl1 O1B O4B -124.9(11) . . . . ?
O2A Cl1 O1B O4B -176.5(19) . . . . ?
O4A Cl1 O1B O4B -45.9(10) . . . . ?
O3B Cl1 O4B O1B -124.8(9) . . . . ?
O1A Cl1 O4B O1B -50.1(18) . . . . ?
O2B Cl1 O4B O1B 102.3(12) . . . . ?
O3A Cl1 O4B O1B -173.7(11) . . . . ?
O2A Cl1 O4B O1B 15(8) . . . . ?
O4A Cl1 O4B O1B 127.9(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
C1 H1 O1A 0.88(4) 2.34(5) 3.211(13) 169(4) .
C1 H1 O1B 0.88(4) 2.60(4) 3.421(12) 156(4) .
C2 H2 O2A 0.85(5) 2.62(5) 3.31(2) 139(4) 4_665
C2 H2 O3A 0.85(5) 2.47(5) 3.292(12) 166(4) 4_665
C3 H3 O4A 0.92(4) 2.68(5) 3.346(19) 130(4) 6
N15 H15A N7 0.84(6) 2.48(6) 3.236(5) 151(5) 6
N15 H15B O4B 0.86(6) 2.64(7) 3.397(18) 147(5) 6_556
N5 H5A N15 0.795(19) 2.43(3) 3.143(5) 150(4) 3
N10 H10A N2 0.79(2) 2.54(7) 3.009(5) 119(7) 6
N10 H10A O2A 0.79(2) 2.53(6) 3.02(2) 122(6) .
N10 H10A O2B 0.79(2) 2.39(3) 3.108(11) 151(6) .
N5 H5B O3A 0.805(19) 2.33(3) 3.103(16) 163(5) 5_556
N5 H5B O3B 0.805(19) 2.42(4) 3.090(13) 142(4) 5_556
N10 H10B O3B 0.789(19) 2.36(3) 3.085(12) 153(4) 1_554
C1 H1 O1A 0.88(4) 2.34(5) 3.211(13) 169(4) .
C1 H1 O1B 0.88(4) 2.60(4) 3.421(12) 156(4) .
C2 H2 O2A 0.85(5) 2.62(5) 3.31(2) 139(4) 4_665
C2 H2 O3A 0.85(5) 2.47(5) 3.292(12) 166(4) 4_665
N15 H15A N7 0.84(6) 2.48(6) 3.236(5) 151(5) 6
N15 H15B O4B 0.86(6) 2.64(7) 3.397(18) 147(5) 6_556
N5 H5A N15 0.795(19) 2.43(3) 3.143(5) 150(4) 3
N10 H10A N2 0.79(2) 2.54(7) 3.009(5) 119(7) 6
N10 H10A O2A 0.79(2) 2.53(6) 3.02(2) 122(6) .
N10 H10A O2B 0.79(2) 2.39(3) 3.108(11) 151(6) .
N5 H5B O3A 0.805(19) 2.33(3) 3.103(16) 163(5) 5_556
N5 H5B O3B 0.805(19) 2.42(4) 3.090(13) 142(4) 5_556
N10 H10B O3B 0.789(19) 2.36(3) 3.085(12) 153(4) 1_554

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



_refine_diff_density_max         1.577
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.108

_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_mx017
_database_code_depnum_ccdc_archive 'CCDC 1834848'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sat Jan 14 18:07:35 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(2-aminotetrazolyl)iron(II) diperchlorate *2 2-aminotetrazole
;
_chemical_name_common            
'hexakis(2-aminotetrazolyl)iron(II) diperchlorate *2 2-aminotetrazole'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Fe N30, 2(C H3 N5), 2(Cl O4)'
_chemical_formula_sum            'C8 H24 Cl2 Fe N40 O8'
_chemical_formula_weight         935.42

_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                   8.5150(3)
_cell_length_b                   10.8300(5)
_cell_length_c                   19.3050(8)
_cell_angle_alpha                79.072(4)
_cell_angle_beta                 86.098(3)
_cell_angle_gamma                86.476(3)
_cell_volume                     1741.78(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5333
_cell_measurement_theta_min      4.5310
_cell_measurement_theta_max      31.7620

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    0.689
_shelx_estimated_absorpt_T_min   0.761
_shelx_estimated_absorpt_T_max   0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94454
_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    1.784
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            13639
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.348
_diffrn_reflns_theta_max         25.999
_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             6835
_reflns_number_gt                5770
_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)+(0.0384P)²+0.5420P] 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         6835
_refine_ls_number_parameters     628
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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      0.0281109000
_diffrn_orient_matrix_UB_12      0.0418548000
_diffrn_orient_matrix_UB_13      0.0199479000
_diffrn_orient_matrix_UB_21      0.0783112000
_diffrn_orient_matrix_UB_22      -0.0233675000
_diffrn_orient_matrix_UB_23      -0.0062465000
_diffrn_orient_matrix_UB_31      0.0080966000
_diffrn_orient_matrix_UB_32      0.0465069000
_diffrn_orient_matrix_UB_33      -0.0311133000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -22.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000  -60.0000 125

#__ type_ start__ end____ width___ exp.time_
  2 omega   26.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -30.0000 69

#__ type_ start__ end____ width___ exp.time_
  3 omega   -9.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 48

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
  6 omega  -83.00  -38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000    0.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega -109.00  -84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  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'
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
Fe1 Fe 0.22619(3) 0.49731(2) 0.25485(2) 0.01464(8) Uani 1 1 d . . . . .
N1 N -0.0492(2) 0.16019(16) 0.30045(9) 0.0237(4) Uani 1 1 d . . . . .
N2 N -0.02689(19) 0.18436(15) 0.36361(8) 0.0184(3) Uani 1 1 d . . . . .
N3 N 0.05381(19) 0.28269(15) 0.36438(8) 0.0192(3) Uani 1 1 d . . . . .
N4 N 0.08984(18) 0.32803(15) 0.29604(8) 0.0189(3) Uani 1 1 d . . . . .
N5 N -0.0842(2) 0.10608(17) 0.42482(10) 0.0247(4) Uani 1 1 d . . . . .
N6 N -0.2188(2) 0.65808(17) 0.17217(9) 0.0251(4) Uani 1 1 d . . . . .
N7 N -0.11480(19) 0.65938(15) 0.11769(8) 0.0190(3) Uani 1 1 d . . . . .
N8 N 0.02737(19) 0.61876(16) 0.13285(8) 0.0210(4) Uani 1 1 d . . . . .
N9 N 0.02049(19) 0.58773(15) 0.20332(8) 0.0189(3) Uani 1 1 d . . . . .
N10 N -0.1562(3) 0.7070(2) 0.04902(10) 0.0301(4) Uani 1 1 d . . . . .
N11 N 0.30755(19) 0.40297(15) 0.16575(8) 0.0176(3) Uani 1 1 d . . . . .
C3 C 0.3131(2) 0.43231(19) 0.09467(10) 0.0204(4) Uani 1 1 d . . . . .
N13 N 0.36493(19) 0.33559(15) 0.06514(8) 0.0207(4) Uani 1 1 d . . . . .
N14 N 0.38934(18) 0.24681(15) 0.12161(8) 0.0176(3) Uani 1 1 d . . . . .
N15 N 0.4499(2) 0.12662(16) 0.11526(10) 0.0236(4) Uani 1 1 d . . . . .
N16 N 0.46757(19) 0.84530(15) 0.17649(8) 0.0211(4) Uani 1 1 d . . . . .
N17 N 0.44684(18) 0.79323(14) 0.12148(8) 0.0171(3) Uani 1 1 d . . . . .
N18 N 0.3838(2) 0.68417(15) 0.13517(8) 0.0207(4) Uani 1 1 d . . . . .
N19 N 0.35985(19) 0.66052(15) 0.20581(8) 0.0189(3) Uani 1 1 d . . . . .
N20 N 0.4771(2) 0.85711(19) 0.05277(9) 0.0255(4) Uani 1 1 d . . . . .
N21 N 0.10283(19) 0.61778(15) 0.45716(8) 0.0201(4) Uani 1 1 d . . . . .
N22 N 0.08429(19) 0.72148(15) 0.40804(8) 0.0175(3) Uani 1 1 d . . . . .
N23 N 0.11141(19) 0.70381(15) 0.34272(8) 0.0190(3) Uani 1 1 d . . . . .
N24 N 0.15057(19) 0.58225(15) 0.34824(8) 0.0178(3) Uani 1 1 d . . . . .
N25 N 0.0384(3) 0.83623(17) 0.42701(10) 0.0254(4) Uani 1 1 d . . . . .
N26 N 0.68902(19) 0.36281(17) 0.32416(9) 0.0239(4) Uani 1 1 d . . . . .
N27 N 0.59766(19) 0.35913(15) 0.38301(8) 0.0184(3) Uani 1 1 d . . . . .
N28 N 0.44953(19) 0.39020(15) 0.37432(8) 0.0196(3) Uani 1 1 d . . . . .
N29 N 0.43899(19) 0.41727(15) 0.30440(8) 0.0188(3) Uani 1 1 d . . . . .
N30 N 0.6577(2) 0.31518(19) 0.44869(9) 0.0266(4) Uani 1 1 d . . . . .
C1 C 0.0252(2) 0.2533(2) 0.25949(11) 0.0219(4) Uani 1 1 d . . . . .
C2 C -0.1284(2) 0.61199(19) 0.22518(11) 0.0217(4) Uani 1 1 d . . . . .
N12 N 0.35701(19) 0.28243(15) 0.18236(8) 0.0188(3) Uani 1 1 d . . . . .
C4 C 0.4127(2) 0.75809(19) 0.22893(10) 0.0202(4) Uani 1 1 d . . . . .
C5 C 0.1435(2) 0.53256(19) 0.41798(10) 0.0200(4) Uani 1 1 d . . . . .
C6 C 0.5850(2) 0.4007(2) 0.27584(11) 0.0226(4) Uani 1 1 d . . . . .
N31 N 0.8925(2) 0.93941(18) 0.17332(9) 0.0334(5) Uani 1 1 d . . . . .
N32 N 0.9052(2) 0.98762(16) 0.10530(9) 0.0231(4) Uani 1 1 d . . . . .
N33 N 1.0465(2) 1.0233(2) 0.08181(10) 0.0354(5) Uani 1 1 d . . . . .
N34 N 1.1354(2) 0.9963(2) 0.13688(10) 0.0398(5) Uani 1 1 d . . . . .
N35 N 0.7776(2) 1.00052(19) 0.06248(11) 0.0271(4) Uani 1 1 d . . . . .
C7 C 1.0388(3) 0.9469(2) 0.19113(13) 0.0363(6) Uani 1 1 d . . . . .
N36 N 0.5381(2) 0.08627(19) 0.37450(10) 0.0338(4) Uani 1 1 d . . . . .
N37 N 0.51292(19) 0.04337(15) 0.31687(9) 0.0219(4) Uani 1 1 d . . . . .
N38 N 0.3731(2) 0.00051(18) 0.31503(10) 0.0320(4) Uani 1 1 d . . . . .
N39 N 0.2993(2) 0.01428(19) 0.37649(11) 0.0364(5) Uani 1 1 d . . . . .
N40 N 0.6208(2) 0.0474(2) 0.25888(10) 0.0262(4) Uani 1 1 d . . . . .
C8 C 0.4001(3) 0.0670(2) 0.41024(14) 0.0394(6) Uani 1 1 d . . . . .
Cl1 Cl 0.34086(6) 0.29306(5) 0.59675(3) 0.02650(12) Uani 1 1 d . . . . .
O1 O 0.2849(2) 0.20361(19) 0.65537(10) 0.0628(6) Uani 1 1 d . . . . .
O2 O 0.5047(2) 0.3098(2) 0.59974(10) 0.0646(6) Uani 1 1 d . . . . .
O3 O 0.3163(3) 0.2529(2) 0.53241(11) 0.0667(6) Uani 1 1 d . . . . .
O4 O 0.2517(2) 0.40838(16) 0.59754(11) 0.0552(5) Uani 1 1 d . . . . .
Cl2 Cl 0.80245(6) 0.33559(5) 0.08648(2) 0.02270(12) Uani 1 1 d . . . . .
O5 O 0.7021(2) 0.44429(16) 0.09353(10) 0.0461(4) Uani 1 1 d . . . . .
O6 O 0.7746(2) 0.29463(15) 0.02193(8) 0.0370(4) Uani 1 1 d . . . . .
O7 O 0.96443(19) 0.36520(18) 0.08547(9) 0.0461(5) Uani 1 1 d . . . . .
O8 O 0.7684(2) 0.23645(15) 0.14531(8) 0.0371(4) Uani 1 1 d . . . . .
H1 H 0.028(2) 0.2653(19) 0.2093(11) 0.020(5) Uiso 1 1 d . . . . .
H6 H 0.612(3) 0.410(2) 0.2285(12) 0.030(6) Uiso 1 1 d . . . . .
H5 H 0.168(2) 0.448(2) 0.4363(10) 0.017(5) Uiso 1 1 d . . . . .
H3 H 0.283(3) 0.512(2) 0.0692(12) 0.031(6) Uiso 1 1 d . . . . .
H4 H 0.410(3) 0.766(2) 0.2769(12) 0.027(6) Uiso 1 1 d . . . . .
H30A H 0.579(3) 0.313(2) 0.4785(13) 0.031(7) Uiso 1 1 d . . . . .
H2 H -0.168(3) 0.602(2) 0.2728(12) 0.027(6) Uiso 1 1 d . . . . .
H25A H 0.104(3) 0.891(3) 0.4052(13) 0.039(7) Uiso 1 1 d . . . . .
H40A H 0.687(3) 0.095(3) 0.2649(14) 0.049(9) Uiso 1 1 d . . . . .
H15B H 0.374(3) 0.082(2) 0.1185(12) 0.026(6) Uiso 1 1 d . . . . .
H30B H 0.722(3) 0.371(2) 0.4546(12) 0.032(7) Uiso 1 1 d . . . . .
H5B H -0.052(3) 0.134(2) 0.4596(13) 0.031(7) Uiso 1 1 d . . . . .
H20A H 0.477(3) 0.802(2) 0.0269(13) 0.037(7) Uiso 1 1 d . . . . .
H20B H 0.573(3) 0.888(2) 0.0517(12) 0.034(7) Uiso 1 1 d . . . . .
H35B H 0.737(3) 1.074(3) 0.0613(14) 0.046(8) Uiso 1 1 d . . . . .
H40B H 0.657(3) -0.028(2) 0.2597(12) 0.030(7) Uiso 1 1 d . . . . .
H25B H -0.052(3) 0.856(2) 0.4136(13) 0.033(7) Uiso 1 1 d . . . . .
H10A H -0.227(4) 0.654(3) 0.0397(14) 0.051(9) Uiso 1 1 d . . . . .
H5A H -0.184(4) 0.121(3) 0.4245(14) 0.048(8) Uiso 1 1 d . . . . .
H7 H 1.071(3) 0.922(3) 0.2372(14) 0.049(8) Uiso 1 1 d . . . . .
H10B H -0.075(3) 0.699(3) 0.0248(14) 0.041(8) Uiso 1 1 d . . . . .
H15A H 0.510(4) 0.098(3) 0.1564(15) 0.061(9) Uiso 1 1 d . . . . .
H35A H 0.820(3) 0.993(3) 0.0197(15) 0.050(8) Uiso 1 1 d . . . . .
H8 H 0.378(3) 0.091(3) 0.4536(14) 0.046(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
Fe1 N9 2.1618(16) . ?
Fe1 N29 2.1629(16) . ?
Fe1 N19 2.1868(15) . ?
Fe1 N11 2.2134(15) . ?
Fe1 N24 2.2158(15) . ?
Fe1 N4 2.2192(16) . ?
N1 N2 1.323(2) . ?
N1 C1 1.323(3) . ?
N2 N3 1.305(2) . ?
N2 N5 1.395(2) . ?
N3 N4 1.339(2) . ?
N4 C1 1.334(3) . ?
N5 H5B 0.86(3) . ?
N5 H5A 0.86(3) . ?
N6 C2 1.325(3) . ?
N6 N7 1.326(2) . ?
N7 N8 1.296(2) . ?
N7 N10 1.389(2) . ?
N8 N9 1.336(2) . ?
N9 C2 1.335(2) . ?
N10 H10A 0.91(3) . ?
N10 H10B 0.81(3) . ?
N11 N12 1.333(2) . ?
N11 C3 1.347(2) . ?
C3 N13 1.324(3) . ?
C3 H3 0.94(2) . ?
N13 N14 1.329(2) . ?
N14 N12 1.309(2) . ?
N14 N15 1.394(2) . ?
N15 H15B 0.83(2) . ?
N15 H15A 0.97(3) . ?
N16 N17 1.320(2) . ?
N16 C4 1.328(2) . ?
N17 N18 1.301(2) . ?
N17 N20 1.390(2) . ?
N18 N19 1.343(2) . ?
N19 C4 1.335(3) . ?
N20 H20A 0.85(3) . ?
N20 H20B 0.90(3) . ?
N21 C5 1.317(2) . ?
N21 N22 1.334(2) . ?
N22 N23 1.314(2) . ?
N22 N25 1.387(2) . ?
N23 N24 1.324(2) . ?
N24 C5 1.351(2) . ?
N25 H25A 0.87(3) . ?
N25 H25B 0.83(3) . ?
N26 C6 1.322(3) . ?
N26 N27 1.328(2) . ?
N27 N28 1.299(2) . ?
N27 N30 1.388(2) . ?
N28 N29 1.334(2) . ?
N29 C6 1.341(3) . ?
N30 H30A 0.85(2) . ?
N30 H30B 0.87(3) . ?
C1 H1 0.95(2) . ?
C2 H2 0.95(2) . ?
C4 H4 0.94(2) . ?
C5 H5 0.94(2) . ?
C6 H6 0.92(2) . ?
N31 N32 1.318(2) . ?
N31 C7 1.326(3) . ?
N32 N33 1.311(2) . ?
N32 N35 1.394(3) . ?
N33 N34 1.324(3) . ?
N34 C7 1.336(3) . ?
N35 H35B 0.84(3) . ?
N35 H35A 0.89(3) . ?
C7 H7 0.93(3) . ?
N36 N37 1.319(2) . ?
N36 C8 1.329(3) . ?
N37 N38 1.309(2) . ?
N37 N40 1.395(2) . ?
N38 N39 1.334(3) . ?
N39 C8 1.328(3) . ?
N40 H40A 0.81(3) . ?
N40 H40B 0.85(3) . ?
C8 H8 0.93(3) . ?
Cl1 O1 1.4191(17) . ?
Cl1 O4 1.4231(18) . ?
Cl1 O3 1.4238(19) . ?
Cl1 O2 1.4240(19) . ?
Cl2 O7 1.4332(16) . ?
Cl2 O5 1.4336(17) . ?
Cl2 O8 1.4344(15) . ?
Cl2 O6 1.4383(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
N9 Fe1 N29 176.58(6) . . ?
N9 Fe1 N19 88.98(6) . . ?
N29 Fe1 N19 87.65(6) . . ?
N9 Fe1 N11 93.83(6) . . ?
N29 Fe1 N11 86.71(6) . . ?
N19 Fe1 N11 89.48(6) . . ?
N9 Fe1 N24 88.96(6) . . ?
N29 Fe1 N24 90.61(6) . . ?
N19 Fe1 N24 92.35(6) . . ?
N11 Fe1 N24 176.69(6) . . ?
N9 Fe1 N4 89.38(6) . . ?
N29 Fe1 N4 94.03(6) . . ?
N19 Fe1 N4 175.41(6) . . ?
N11 Fe1 N4 86.35(6) . . ?
N24 Fe1 N4 91.90(6) . . ?
N2 N1 C1 100.60(16) . . ?
N3 N2 N1 115.92(15) . . ?
N3 N2 N5 123.21(17) . . ?
N1 N2 N5 120.85(17) . . ?
N2 N3 N4 104.19(15) . . ?
C1 N4 N3 106.40(15) . . ?
C1 N4 Fe1 128.18(13) . . ?
N3 N4 Fe1 125.41(12) . . ?
N2 N5 H5B 106.4(16) . . ?
N2 N5 H5A 103.4(18) . . ?
H5B N5 H5A 107(2) . . ?
C2 N6 N7 100.48(16) . . ?
N8 N7 N6 116.04(15) . . ?
N8 N7 N10 122.63(16) . . ?
N6 N7 N10 121.26(17) . . ?
N7 N8 N9 104.39(14) . . ?
C2 N9 N8 106.51(16) . . ?
C2 N9 Fe1 134.36(13) . . ?
N8 N9 Fe1 118.75(12) . . ?
N7 N10 H10A 105.4(17) . . ?
N7 N10 H10B 104(2) . . ?
H10A N10 H10B 109(3) . . ?
N12 N11 C3 106.51(15) . . ?
N12 N11 Fe1 116.60(11) . . ?
C3 N11 Fe1 136.73(13) . . ?
N13 C3 N11 112.11(17) . . ?
N13 C3 H3 124.0(14) . . ?
N11 C3 H3 123.9(14) . . ?
C3 N13 N14 101.48(15) . . ?
N12 N14 N13 114.95(15) . . ?
N12 N14 N15 123.53(16) . . ?
N13 N14 N15 121.49(15) . . ?
N14 N15 H15B 106.6(16) . . ?
N14 N15 H15A 105.6(18) . . ?
H15B N15 H15A 108(2) . . ?
N17 N16 C4 100.85(16) . . ?
N18 N17 N16 116.14(14) . . ?
N18 N17 N20 122.16(16) . . ?
N16 N17 N20 121.43(16) . . ?
N17 N18 N19 104.04(15) . . ?
C4 N19 N18 106.63(15) . . ?
C4 N19 Fe1 134.47(13) . . ?
N18 N19 Fe1 118.34(12) . . ?
N17 N20 H20A 105.4(16) . . ?
N17 N20 H20B 106.1(15) . . ?
H20A N20 H20B 111(2) . . ?
C5 N21 N22 101.50(15) . . ?
N23 N22 N21 114.49(16) . . ?
N23 N22 N25 124.74(16) . . ?
N21 N22 N25 120.77(15) . . ?
N22 N23 N24 105.19(14) . . ?
N23 N24 C5 106.54(15) . . ?
N23 N24 Fe1 122.07(11) . . ?
C5 N24 Fe1 131.25(13) . . ?
N22 N25 H25A 107.4(17) . . ?
N22 N25 H25B 107.8(18) . . ?
H25A N25 H25B 110(2) . . ?
C6 N26 N27 100.77(16) . . ?
N28 N27 N26 115.74(15) . . ?
N28 N27 N30 123.28(16) . . ?
N26 N27 N30 120.79(16) . . ?
N27 N28 N29 104.55(14) . . ?
N28 N29 C6 106.50(16) . . ?
N28 N29 Fe1 122.92(12) . . ?
C6 N29 Fe1 130.02(13) . . ?
N27 N30 H30A 105.8(17) . . ?
N27 N30 H30B 105.6(16) . . ?
H30A N30 H30B 111(2) . . ?
N1 C1 N4 112.88(17) . . ?
N1 C1 H1 122.3(13) . . ?
N4 C1 H1 124.8(13) . . ?
N6 C2 N9 112.56(17) . . ?
N6 C2 H2 121.7(14) . . ?
N9 C2 H2 125.7(14) . . ?
N14 N12 N11 104.96(14) . . ?
N16 C4 N19 112.32(17) . . ?
N16 C4 H4 123.4(14) . . ?
N19 C4 H4 124.3(14) . . ?
N21 C5 N24 112.27(17) . . ?
N21 C5 H5 124.0(12) . . ?
N24 C5 H5 123.7(12) . . ?
N26 C6 N29 112.43(18) . . ?
N26 C6 H6 121.8(14) . . ?
N29 C6 H6 125.7(14) . . ?
N32 N31 C7 100.82(17) . . ?
N33 N32 N31 114.54(18) . . ?
N33 N32 N35 123.18(17) . . ?
N31 N32 N35 122.28(16) . . ?
N32 N33 N34 106.00(17) . . ?
N33 N34 C7 105.3(2) . . ?
N32 N35 H35B 107.4(19) . . ?
N32 N35 H35A 105.1(18) . . ?
H35B N35 H35A 110(2) . . ?
N31 C7 N34 113.3(2) . . ?
N31 C7 H7 123.3(17) . . ?
N34 C7 H7 123.3(17) . . ?
N37 N36 C8 100.49(19) . . ?
N38 N37 N36 115.46(16) . . ?
N38 N37 N40 120.14(17) . . ?
N36 N37 N40 124.32(17) . . ?
N37 N38 N39 104.75(18) . . ?
C8 N39 N38 106.11(18) . . ?
N37 N40 H40A 105(2) . . ?
N37 N40 H40B 106.2(15) . . ?
H40A N40 H40B 114(3) . . ?
N39 C8 N36 113.2(2) . . ?
N39 C8 H8 124.8(16) . . ?
N36 C8 H8 122.0(17) . . ?
O1 Cl1 O4 107.76(11) . . ?
O1 Cl1 O3 110.28(15) . . ?
O4 Cl1 O3 108.14(14) . . ?
O1 Cl1 O2 111.17(13) . . ?
O4 Cl1 O2 110.80(14) . . ?
O3 Cl1 O2 108.65(12) . . ?
O7 Cl2 O5 109.99(12) . . ?
O7 Cl2 O8 109.42(10) . . ?
O5 Cl2 O8 108.99(10) . . ?
O7 Cl2 O6 109.19(10) . . ?
O5 Cl2 O6 109.92(11) . . ?
O8 Cl2 O6 109.31(10) . . ?

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) . . . . ?
C1 N1 N2 N5 -178.63(17) . . . . ?
N1 N2 N3 N4 -0.4(2) . . . . ?
N5 N2 N3 N4 178.00(16) . . . . ?
N2 N3 N4 C1 0.84(19) . . . . ?
N2 N3 N4 Fe1 179.59(12) . . . . ?
C2 N6 N7 N8 0.1(2) . . . . ?
C2 N6 N7 N10 -177.16(18) . . . . ?
N6 N7 N8 N9 -0.3(2) . . . . ?
N10 N7 N8 N9 176.92(17) . . . . ?
N7 N8 N9 C2 0.4(2) . . . . ?
N7 N8 N9 Fe1 174.29(12) . . . . ?
N12 N11 C3 N13 -0.4(2) . . . . ?
Fe1 N11 C3 N13 -175.44(13) . . . . ?
N11 C3 N13 N14 0.4(2) . . . . ?
C3 N13 N14 N12 -0.2(2) . . . . ?
C3 N13 N14 N15 -178.23(17) . . . . ?
C4 N16 N17 N18 0.6(2) . . . . ?
C4 N16 N17 N20 174.77(17) . . . . ?
N16 N17 N18 N19 0.0(2) . . . . ?
N20 N17 N18 N19 -174.11(16) . . . . ?
N17 N18 N19 C4 -0.6(2) . . . . ?
N17 N18 N19 Fe1 172.09(11) . . . . ?
C5 N21 N22 N23 -0.1(2) . . . . ?
C5 N21 N22 N25 179.25(18) . . . . ?
N21 N22 N23 N24 -0.2(2) . . . . ?
N25 N22 N23 N24 -179.55(18) . . . . ?
N22 N23 N24 C5 0.4(2) . . . . ?
N22 N23 N24 Fe1 -175.74(11) . . . . ?
C6 N26 N27 N28 0.5(2) . . . . ?
C6 N26 N27 N30 175.73(18) . . . . ?
N26 N27 N28 N29 -0.1(2) . . . . ?
N30 N27 N28 N29 -175.23(17) . . . . ?
N27 N28 N29 C6 -0.3(2) . . . . ?
N27 N28 N29 Fe1 -172.54(12) . . . . ?
N2 N1 C1 N4 0.7(2) . . . . ?
N3 N4 C1 N1 -1.0(2) . . . . ?
Fe1 N4 C1 N1 -179.73(13) . . . . ?
N7 N6 C2 N9 0.1(2) . . . . ?
N8 N9 C2 N6 -0.3(2) . . . . ?
Fe1 N9 C2 N6 -172.87(14) . . . . ?
N13 N14 N12 N11 0.0(2) . . . . ?
N15 N14 N12 N11 177.97(17) . . . . ?
C3 N11 N12 N14 0.20(19) . . . . ?
Fe1 N11 N12 N14 176.42(11) . . . . ?
N17 N16 C4 N19 -1.0(2) . . . . ?
N18 N19 C4 N16 1.1(2) . . . . ?
Fe1 N19 C4 N16 -169.91(13) . . . . ?
N22 N21 C5 N24 0.4(2) . . . . ?
N23 N24 C5 N21 -0.6(2) . . . . ?
Fe1 N24 C5 N21 175.12(13) . . . . ?
N27 N26 C6 N29 -0.7(2) . . . . ?
N28 N29 C6 N26 0.7(2) . . . . ?
Fe1 N29 C6 N26 172.13(14) . . . . ?
C7 N31 N32 N33 -0.3(2) . . . . ?
C7 N31 N32 N35 -179.6(2) . . . . ?
N31 N32 N33 N34 0.8(3) . . . . ?
N35 N32 N33 N34 -179.92(19) . . . . ?
N32 N33 N34 C7 -0.9(3) . . . . ?
N32 N31 C7 N34 -0.3(3) . . . . ?
N33 N34 C7 N31 0.7(3) . . . . ?
C8 N36 N37 N38 0.0(3) . . . . ?
C8 N36 N37 N40 176.7(2) . . . . ?
N36 N37 N38 N39 -0.8(2) . . . . ?
N40 N37 N38 N39 -177.61(18) . . . . ?
N37 N38 N39 C8 1.1(2) . . . . ?
N38 N39 C8 N36 -1.3(3) . . . . ?
N37 N36 C8 N39 0.8(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
N30 H30A O2 0.85(2) 2.38(3) 3.104(3) 143(2) .
N30 H30A O3 0.85(2) 2.47(3) 3.272(3) 157(2) .
N30 H30A Cl1 0.85(2) 2.93(3) 3.779(2) 172(2) .
N25 H25A N39 0.87(3) 2.17(3) 3.020(3) 165(2) 1_565
N40 H40A N1 0.81(3) 2.57(3) 3.337(3) 158(3) 1_655
N15 H15B N34 0.83(2) 2.26(3) 3.070(3) 167(2) 1_445
N30 H30B N21 0.87(3) 2.37(3) 3.029(3) 134(2) 2_666
N30 H30B O4 0.87(3) 2.43(2) 3.087(3) 133(2) 2_666
N5 H5B N25 0.86(3) 2.28(3) 3.096(3) 159(2) 2_566
N20 H20B N35 0.90(3) 2.23(3) 3.109(3) 165(2) .
N35 H35B O6 0.84(3) 2.41(3) 3.132(3) 145(2) 1_565
N35 H35B O8 0.84(3) 2.65(3) 3.256(3) 130(2) 1_565
N35 H35B N15 0.84(3) 2.66(3) 3.219(3) 125(2) 1_565
N40 H40B O1 0.85(3) 2.32(2) 2.997(3) 137(2) 2_656
N40 H40B N31 0.85(3) 2.57(2) 3.054(3) 116.8(18) 1_545
N25 H25B O1 0.83(3) 2.64(3) 3.361(3) 146(2) 2_566
N25 H25B O3 0.83(3) 2.66(3) 3.228(3) 127(2) 2_566
N10 H10A N13 0.91(3) 2.39(3) 3.041(3) 129(2) 2_565
N10 H10A O5 0.91(3) 2.41(3) 3.105(3) 134(2) 1_455
N5 H5A N30 0.86(3) 2.53(3) 3.133(3) 129(2) 1_455
N5 H5A N36 0.86(3) 2.69(3) 3.452(3) 149(2) 1_455
N10 H10B O7 0.81(3) 2.47(3) 3.171(3) 144(3) 2_665
N10 H10B O6 0.81(3) 2.66(3) 3.439(3) 162(3) 2_665
N15 H15A N40 0.97(3) 2.21(3) 3.168(3) 171(3) .
N35 H35A N33 0.89(3) 2.23(3) 3.119(3) 173(3) 2_775

_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         0.447
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.055

_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_mx149
_database_code_depnum_ccdc_archive 'CCDC 1834852'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Mar 27 21:16:30 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) zinc(II9 dinitrate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) zinc(II9 dinitrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C6 H18 N30 Zn, 2(N O3)'
_chemical_formula_sum            'C6 H18 N32 O6 Zn'
_chemical_formula_weight         699.89

_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                   9.4477(10)
_cell_length_b                   7.9116(9)
_cell_length_c                   17.279(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.610(11)
_cell_angle_gamma                90
_cell_volume                     1291.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1382
_cell_measurement_theta_min      4.8560
_cell_measurement_theta_max      26.5900

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.047
_shelx_estimated_absorpt_T_min   0.679
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62945
_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    1.800
_exptl_crystal_F_000             712
_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            9361
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1570
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.164
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2524
_reflns_number_gt                1856
_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)+(0.0752P)²+1.0337P] 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         2524
_refine_ls_number_parameters     229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1725
_refine_ls_wR_factor_gt          0.1533
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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      0.0296900000
_diffrn_orient_matrix_UB_12      0.0044398000
_diffrn_orient_matrix_UB_13      0.0378254000
_diffrn_orient_matrix_UB_21      -0.0215885000
_diffrn_orient_matrix_UB_22      0.0856045000
_diffrn_orient_matrix_UB_23      0.0028735000
_diffrn_orient_matrix_UB_31      -0.0655116000
_diffrn_orient_matrix_UB_32      -0.0262350000
_diffrn_orient_matrix_UB_33      0.0156809000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -95.00  -66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000 -120.0000 29

#__ type_ start__ end____ width___ exp.time_
  2 omega   -4.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000 -120.0000 48

#__ type_ start__ end____ width___ exp.time_
  3 omega -108.00  -65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  120.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega  -21.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega   -1.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
  6 omega    3.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
  7 omega  -15.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000   60.0000 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'
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 1.0000 0.0000 0.0000 0.0260(3) Uani 1 2 d S . P . .
N1 N 1.1421(4) 0.3785(5) -0.1575(2) 0.0275(9) Uani 1 1 d . . . . .
C1 C 1.0961(5) 0.3347(6) -0.0891(3) 0.0255(10) Uani 1 1 d . . . . .
H1 H 1.0808 0.4093 -0.0469 0.031 Uiso 1 1 calc R U . . .
N4 N 1.0746(4) 0.1715(5) -0.0883(2) 0.0265(9) Uani 1 1 d . . . . .
N5 N 1.1905(6) 0.5371(6) -0.1806(3) 0.0432(12) Uani 1 1 d . . . . .
N9 N 0.8106(4) 0.1518(5) 0.0141(2) 0.0271(9) Uani 1 1 d . . . . .
C2 C 0.6915(5) 0.1332(6) 0.0527(3) 0.0282(11) Uani 1 1 d . . . . .
H2 H 0.6641 0.0364 0.0814 0.034 Uiso 1 1 calc R U . . .
N6 N 0.6178(4) 0.2736(5) 0.0442(2) 0.0293(9) Uani 1 1 d . . . . .
N10 N 0.4833(4) 0.3080(6) 0.0746(3) 0.0355(11) Uani 1 1 d . . . . .
N11 N 1.2264(4) 0.2303(5) 0.1850(2) 0.0295(9) Uani 1 1 d . . . . .
C3 C 1.1829(4) 0.0950(5) 0.1461(3) 0.0261(10) Uani 1 1 d . . . . .
H3 H 1.2031 -0.0196 0.1585 0.031 Uiso 1 1 calc R U . . .
N14 N 1.1083(4) 0.1481(5) 0.0886(2) 0.0282(9) Uani 1 1 d . . . . .
N15 N 1.3114(6) 0.2304(9) 0.2519(4) 0.0532(15) Uani 1 1 d . . . . .
N2 N 1.1499(4) 0.2386(6) -0.2022(2) 0.0357(10) Uani 1 1 d . . . . .
N3 N 1.1086(4) 0.1139(5) -0.1599(2) 0.0329(10) Uani 1 1 d . . . . .
N7 N 0.6880(4) 0.3827(5) -0.0004(3) 0.0339(10) Uani 1 1 d . . . . .
N8 N 0.8054(4) 0.3074(5) -0.0176(3) 0.0327(10) Uani 1 1 d . . . . .
N12 N 1.1775(5) 0.3700(6) 0.1506(3) 0.0425(11) Uani 1 1 d . . . . .
N13 N 1.1034(4) 0.3197(5) 0.0905(2) 0.0303(9) Uani 1 1 d . . . . .
O1 O 0.5853(4) 0.7512(5) 0.0926(2) 0.0485(11) Uani 1 1 d . . . . .
O2 O 0.4836(5) 0.6089(6) 0.1824(2) 0.0573(11) Uani 1 1 d . . . . .
O3 O 0.4824(4) 0.8820(5) 0.1855(3) 0.0582(12) Uani 1 1 d . . . . .
N16 N 0.5148(4) 0.7471(6) 0.1533(3) 0.0377(11) Uani 1 1 d . . . . .
H10B H 0.428(6) 0.337(7) 0.030(3) 0.036(15) Uiso 1 1 d . . . . .
H10A H 0.490(6) 0.405(9) 0.094(3) 0.045(18) Uiso 1 1 d . . . . .
H5B H 1.295(7) 0.526(7) -0.196(4) 0.058(19) Uiso 1 1 d . . . . .
H5A H 1.128(6) 0.546(7) -0.225(4) 0.046(17) Uiso 1 1 d . . . . .
H15B H 1.260(13) 0.251(13) 0.286(7) 0.14(5) Uiso 1 1 d . . . . .
H15A H 1.393(15) 0.188(16) 0.236(8) 0.20(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
Zn1 N4 2.166(4) . ?
Zn1 N4 2.166(4) 3_755 ?
Zn1 N9 2.171(4) . ?
Zn1 N9 2.171(4) 3_755 ?
Zn1 N14 2.175(4) 3_755 ?
Zn1 N14 2.175(4) . ?
N1 C1 1.312(6) . ?
N1 N2 1.352(6) . ?
N1 N5 1.395(6) . ?
C1 N4 1.307(6) . ?
C1 H1 0.9500 . ?
N4 N3 1.359(5) . ?
N5 H5B 1.03(7) . ?
N5 H5A 0.97(6) . ?
N9 C2 1.322(6) . ?
N9 N8 1.348(5) . ?
C2 N6 1.318(6) . ?
C2 H2 0.9500 . ?
N6 N7 1.338(5) . ?
N6 N10 1.407(5) . ?
N10 H10B 0.96(5) . ?
N10 H10A 0.84(6) . ?
N11 C3 1.327(6) . ?
N11 N12 1.335(6) . ?
N11 N15 1.400(6) . ?
C3 N14 1.283(6) . ?
C3 H3 0.9500 . ?
N14 N13 1.359(5) . ?
N15 H15B 0.79(12) . ?
N15 H15A 0.89(14) . ?
N2 N3 1.291(6) . ?
N7 N8 1.297(5) . ?
N12 N13 1.308(6) . ?
O1 N16 1.249(6) . ?
O2 N16 1.241(6) . ?
O3 N16 1.244(6) . ?

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 Zn1 N4 180.0 . 3_755 ?
N4 Zn1 N9 90.42(14) . . ?
N4 Zn1 N9 89.58(14) 3_755 . ?
N4 Zn1 N9 89.58(14) . 3_755 ?
N4 Zn1 N9 90.42(14) 3_755 3_755 ?
N9 Zn1 N9 180.0 . 3_755 ?
N4 Zn1 N14 89.74(14) . 3_755 ?
N4 Zn1 N14 90.26(14) 3_755 3_755 ?
N9 Zn1 N14 89.69(14) . 3_755 ?
N9 Zn1 N14 90.31(14) 3_755 3_755 ?
N4 Zn1 N14 90.26(14) . . ?
N4 Zn1 N14 89.74(14) 3_755 . ?
N9 Zn1 N14 90.30(14) . . ?
N9 Zn1 N14 89.69(14) 3_755 . ?
N14 Zn1 N14 180.0 3_755 . ?
C1 N1 N2 108.6(4) . . ?
C1 N1 N5 127.5(4) . . ?
N2 N1 N5 123.6(4) . . ?
N4 C1 N1 108.8(4) . . ?
N4 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
C1 N4 N3 106.5(4) . . ?
C1 N4 Zn1 132.6(3) . . ?
N3 N4 Zn1 120.9(3) . . ?
N1 N5 H5B 108(3) . . ?
N1 N5 H5A 95(3) . . ?
H5B N5 H5A 112(5) . . ?
C2 N9 N8 106.2(4) . . ?
C2 N9 Zn1 134.6(3) . . ?
N8 N9 Zn1 119.1(3) . . ?
N6 C2 N9 107.5(4) . . ?
N6 C2 H2 126.2 . . ?
N9 C2 H2 126.2 . . ?
C2 N6 N7 110.1(4) . . ?
C2 N6 N10 126.8(4) . . ?
N7 N6 N10 123.0(4) . . ?
N6 N10 H10B 103(3) . . ?
N6 N10 H10A 105(4) . . ?
H10B N10 H10A 98(5) . . ?
C3 N11 N12 109.8(4) . . ?
C3 N11 N15 126.2(4) . . ?
N12 N11 N15 124.0(5) . . ?
N14 C3 N11 107.0(4) . . ?
N14 C3 H3 126.5 . . ?
N11 C3 H3 126.5 . . ?
C3 N14 N13 109.1(4) . . ?
C3 N14 Zn1 128.2(3) . . ?
N13 N14 Zn1 122.7(3) . . ?
N11 N15 H15B 106(8) . . ?
N11 N15 H15A 104(9) . . ?
H15B N15 H15A 149(10) . . ?
N3 N2 N1 106.5(4) . . ?
N2 N3 N4 109.6(4) . . ?
N8 N7 N6 105.4(4) . . ?
N7 N8 N9 110.7(4) . . ?
N13 N12 N11 106.3(4) . . ?
N12 N13 N14 107.8(4) . . ?
O2 N16 O3 120.9(5) . . ?
O2 N16 O1 119.7(5) . . ?
O3 N16 O1 119.4(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 N1 C1 N4 0.2(5) . . . . ?
N5 N1 C1 N4 -173.3(4) . . . . ?
N1 C1 N4 N3 -0.3(5) . . . . ?
N1 C1 N4 Zn1 -179.9(3) . . . . ?
N8 N9 C2 N6 0.0(5) . . . . ?
Zn1 N9 C2 N6 175.5(3) . . . . ?
N9 C2 N6 N7 0.6(6) . . . . ?
N9 C2 N6 N10 179.0(5) . . . . ?
N12 N11 C3 N14 0.0(5) . . . . ?
N15 N11 C3 N14 -179.7(5) . . . . ?
N11 C3 N14 N13 -0.2(5) . . . . ?
N11 C3 N14 Zn1 -179.3(3) . . . . ?
C1 N1 N2 N3 0.0(5) . . . . ?
N5 N1 N2 N3 173.9(4) . . . . ?
N1 N2 N3 N4 -0.2(5) . . . . ?
C1 N4 N3 N2 0.3(5) . . . . ?
Zn1 N4 N3 N2 179.9(3) . . . . ?
C2 N6 N7 N8 -0.9(5) . . . . ?
N10 N6 N7 N8 -179.5(5) . . . . ?
N6 N7 N8 N9 1.0(5) . . . . ?
C2 N9 N8 N7 -0.6(5) . . . . ?
Zn1 N9 N8 N7 -176.9(3) . . . . ?
C3 N11 N12 N13 0.2(5) . . . . ?
N15 N11 N12 N13 179.9(5) . . . . ?
N11 N12 N13 N14 -0.3(5) . . . . ?
C3 N14 N13 N12 0.3(5) . . . . ?
Zn1 N14 N13 N12 179.5(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
N10 H10B O1 0.96(5) 2.23(5) 2.991(7) 136(4) 3_665
N10 H10B N7 0.96(5) 2.52(5) 3.194(6) 127(4) 3_665
N10 H10A O2 0.84(6) 2.23(6) 3.022(7) 159(6) .
N5 H5B O2 1.03(7) 2.36(7) 3.289(7) 150(5) 3_765
N5 H5B N2 1.03(7) 2.49(6) 2.997(6) 110(4) 2_754
N5 H5A O3 0.97(6) 2.13(6) 3.088(7) 168(5) 4_675
N15 H15B O3 0.79(12) 2.56(12) 3.221(9) 141(10) 2_645

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



_refine_diff_density_max         1.123
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.118

_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_mx030
_database_code_depnum_ccdc_archive 'CCDC 1834849'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Jan 23 15:04:34 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
2-aminotetrazolium perchlorate
;
_chemical_name_common            '2-aminotetrazolium perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C H4 N5, Cl O4'
_chemical_formula_sum            'C H4 Cl N5 O4'
_chemical_formula_weight         185.54

_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                   5.5236(4)
_cell_length_b                   8.3025(7)
_cell_length_c                   13.6929(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.247(5)
_cell_angle_gamma                90
_cell_volume                     627.95(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2006
_cell_measurement_theta_min      4.6570
_cell_measurement_theta_max      31.9410

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.586
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89942
_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    1.963
_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            4330
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.432
_diffrn_reflns_theta_max         25.976
_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             1228
_reflns_number_gt                1098
_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)+(0.0342P)²+0.3665P] 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     SHELXL
_refine_ls_extinction_coef       0.087(5)
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1228
_refine_ls_number_parameters     117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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      0.0190779000
_diffrn_orient_matrix_UB_12      0.0780907000
_diffrn_orient_matrix_UB_13      -0.0195061000
_diffrn_orient_matrix_UB_21      0.0064131000
_diffrn_orient_matrix_UB_22      -0.0331282000
_diffrn_orient_matrix_UB_23      -0.0476714000
_diffrn_orient_matrix_UB_31      -0.1268186000
_diffrn_orient_matrix_UB_32      0.0100839000
_diffrn_orient_matrix_UB_33      -0.0055712000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    4.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  2 omega    8.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega  -10.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000    0.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega   79.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -120.0000 30

#__ type_ start__ end____ width___ exp.time_
  5 omega   41.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -180.0000 67

#__ type_ start__ end____ width___ exp.time_
  6 omega  -42.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -38.0000  120.0000 86

#__ type_ start__ end____ width___ exp.time_
  7 omega  -86.00    0.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  121.0000  -70.0000 86

;



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'
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 0.7126(3) 0.06292(19) 0.09473(11) 0.0201(4) Uani 1 1 d . . . . .
N2 N 0.5890(3) 0.19908(19) 0.10780(10) 0.0164(3) Uani 1 1 d . . . . .
N3 N 0.6759(3) 0.29988(19) 0.17038(11) 0.0205(4) Uani 1 1 d . . . . .
N4 N 0.8746(3) 0.2232(2) 0.20002(12) 0.0203(4) Uani 1 1 d . . . . .
N5 N 0.3699(3) 0.2235(2) 0.06302(12) 0.0202(4) Uani 1 1 d . . . . .
C1 C 0.8962(3) 0.0828(2) 0.15534(13) 0.0198(4) Uani 1 1 d . . . . .
Cl1 Cl 0.34903(7) 0.15708(5) 0.37506(3) 0.01690(18) Uani 1 1 d . . . . .
O1 O 0.3538(2) 0.05358(17) 0.29099(10) 0.0270(4) Uani 1 1 d . . . . .
O2 O 0.2526(3) 0.07143(17) 0.45744(10) 0.0279(4) Uani 1 1 d . . . . .
O3 O 0.5873(2) 0.21448(18) 0.39580(10) 0.0279(4) Uani 1 1 d . . . . .
O4 O 0.1933(2) 0.29484(16) 0.35443(10) 0.0265(3) Uani 1 1 d . . . . .
H1 H 1.013(4) 0.015(3) 0.1645(15) 0.020(5) Uiso 1 1 d . . . . .
H4 H 0.967(4) 0.263(3) 0.2421(16) 0.024(6) Uiso 1 1 d . . . . .
H5B H 0.372(4) 0.169(3) 0.0097(19) 0.034(7) Uiso 1 1 d . . . . .
H5A H 0.350(4) 0.327(3) 0.0553(17) 0.028(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 1.318(2) . ?
N1 N2 1.333(2) . ?
N2 N3 1.289(2) . ?
N2 N5 1.370(2) . ?
N3 N4 1.331(2) . ?
N4 C1 1.322(3) . ?
N4 H4 0.84(2) . ?
N5 H5B 0.86(3) . ?
N5 H5A 0.87(3) . ?
C1 H1 0.86(2) . ?
Cl1 O3 1.4272(14) . ?
Cl1 O1 1.4368(13) . ?
Cl1 O2 1.4378(13) . ?
Cl1 O4 1.4581(14) . ?

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 101.68(15) . . ?
N3 N2 N1 116.76(15) . . ?
N3 N2 N5 121.83(16) . . ?
N1 N2 N5 121.17(15) . . ?
N2 N3 N4 101.34(15) . . ?
C1 N4 N3 110.89(16) . . ?
C1 N4 H4 127.7(16) . . ?
N3 N4 H4 121.4(16) . . ?
N2 N5 H5B 106.7(16) . . ?
N2 N5 H5A 108.1(16) . . ?
H5B N5 H5A 115(2) . . ?
N1 C1 N4 109.34(17) . . ?
N1 C1 H1 125.6(14) . . ?
N4 C1 H1 125.1(14) . . ?
O3 Cl1 O1 109.83(8) . . ?
O3 Cl1 O2 110.71(9) . . ?
O1 Cl1 O2 109.93(9) . . ?
O3 Cl1 O4 108.63(8) . . ?
O1 Cl1 O4 109.07(8) . . ?
O2 Cl1 O4 108.64(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.5(2) . . . . ?
C1 N1 N2 N5 -174.98(15) . . . . ?
N1 N2 N3 N4 0.6(2) . . . . ?
N5 N2 N3 N4 175.03(14) . . . . ?
N2 N3 N4 C1 -0.42(19) . . . . ?
N2 N1 C1 N4 0.16(19) . . . . ?
N3 N4 C1 N1 0.2(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
N4 H4 O4 0.84(2) 2.00(2) 2.809(2) 164(2) 1_655
N4 H4 O1 0.84(2) 2.65(2) 3.128(2) 118.1(19) 2_655
N4 H4 Cl1 0.84(2) 2.92(2) 3.5861(17) 138(2) 1_655
N5 H5B N1 0.86(3) 2.44(3) 3.243(2) 155(2) 3_655
N5 H5A O2 0.87(3) 2.12(3) 2.980(2) 171(2) 2

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



_refine_diff_density_max         0.198
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060

_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_lx624
_database_code_depnum_ccdc_archive 'CCDC 1834851'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

_vrf_PLAT094_lx624               
; 
PROBLEM: Ratio of Maximum / Minimum Residual Density ....   4.68 Report 
RESPONSE: Must be caused by crystal defects. Inclusion of 
water or other solvents has been excluded by elemental anaylsis.
Perchlorate anions are strongly disordered!
;

_vrf_PLAT097_lx624               
; 
PROBLEM: Large Reported Max.  (Positive) Residual Density   3.07 eA-3   
RESPONSE: Must be caused by crystal defects. Inclusion of 
water or other solvents has been excluded by elemental anaylsis.
Perchlorate anions are strongly disordered!
;
_audit_creation_date             
;
'Mon Dec 26 08:08:19 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-aminotetrazolyl)zinc(II) perchlorate
;
_chemical_name_common            
'hexakis(1-aminotetrazolyl)zinc(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C6 H18 N30 Zn, 2(Cl O4)'
_chemical_formula_sum            'C6 H18 Cl2 N30 O8 Zn'
_chemical_formula_weight         774.77

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'




_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, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   18.908(5)
_cell_length_b                   18.908(5)
_cell_length_c                   6.992(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2164.8(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5523
_cell_measurement_theta_min      4.3750
_cell_measurement_theta_max      32.1080

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.129
_shelx_estimated_absorpt_T_min   0.674
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74851
_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    1.783
_exptl_crystal_F_000             1176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            17769
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.311
_diffrn_reflns_theta_max         26.490
_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             2987
_reflns_number_gt                2571
_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)+(0.1117P)²+7.9238P] 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         2987
_refine_ls_number_parameters     262
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.2024
_refine_ls_wR_factor_gt          0.1925
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.003


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0423603000
_diffrn_orient_matrix_UB_12      -0.0289821000
_diffrn_orient_matrix_UB_13      0.0012754000
_diffrn_orient_matrix_UB_21      -0.0089783000
_diffrn_orient_matrix_UB_22      0.0322059000
_diffrn_orient_matrix_UB_23      0.0009173000
_diffrn_orient_matrix_UB_31      -0.0006617000
_diffrn_orient_matrix_UB_32      -0.0000675000
_diffrn_orient_matrix_UB_33      -0.1014499000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -108.00  -38.00   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   60.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   74.40   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 142

#__ type_ start__ end____ width___ exp.time_
  3 omega    2.00   97.90   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 137

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   84.30   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   90.0000 119

#__ type_ start__ end____ width___ exp.time_
  5 omega  -31.00   92.20   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000 -150.0000 176

;



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 0.6667 0.3333 0.02111(11) 0.0214(3) Uani 1 3 d S T P . .
N1 N 0.8288(2) 0.5462(2) 0.3429(5) 0.0271(7) Uani 1 1 d . . . . .
N2 N 0.8593(2) 0.4976(2) 0.3784(6) 0.0380(9) Uani 1 1 d . . . . .
N3 N 0.8132(2) 0.4296(2) 0.2896(6) 0.0367(9) Uani 1 1 d . . . . .
N4 N 0.7527(2) 0.4344(2) 0.1967(5) 0.0257(7) Uani 1 1 d . . . . .
N5 N 0.8622(3) 0.6260(2) 0.4131(7) 0.0433(10) Uani 1 1 d . . . . .
H5B H 0.9065 0.6536 0.3444 0.065 Uiso 1 1 d R U . . .
H5A H 0.8760 0.6216 0.5338 0.065 Uiso 1 1 d R U . . .
N6 N 0.5788(2) 0.2336(2) -0.1548(5) 0.0261(7) Uani 1 1 d . . . . .
N7 N 0.5152(2) 0.2377(2) -0.2359(6) 0.0398(9) Uani 1 1 d . . . . .
N8 N 0.4683(2) 0.1702(3) -0.3249(6) 0.0440(10) Uani 1 1 d . . . . .
N9 N 0.5010(2) 0.1226(2) -0.3040(5) 0.0325(8) Uani 1 1 d . . . . .
H10A H 0.4337 0.0118 -0.2916 0.049 Uiso 1 1 d R U . . .
H10B H 0.4687 0.0442 -0.5004 0.049 Uiso 1 1 d R U . . .
N10 N 0.4656(3) 0.0444(3) -0.3776(8) 0.0696(18) Uani 1 1 d . . . . .
C1 C 0.7634(2) 0.5065(3) 0.2315(6) 0.0300(9) Uani 1 1 d . . . . .
H1 H 0.7302 0.5274 0.1854 0.036 Uiso 1 1 calc R U . . .
C2 C 0.5688(2) 0.1619(3) -0.2003(6) 0.0292(9) Uani 1 1 d . . . . .
H2 H 0.6039 0.1415 -0.1653 0.035 Uiso 1 1 calc R U . . .
Zn2 Zn 0.0000 0.0000 0.0000 0.0217(3) Uani 1 6 d S T P . .
N11 N 0.1560(2) 0.2130(2) 0.3296(5) 0.0271(7) Uani 1 1 d . . . . .
N12 N 0.0825(2) 0.2023(2) 0.3755(6) 0.0413(10) Uani 1 1 d . . . . .
N13 N 0.0296(2) 0.1391(2) 0.2817(6) 0.0397(9) Uani 1 1 d . . . . .
N14 N 0.0681(2) 0.1080(2) 0.1751(5) 0.0254(7) Uani 1 1 d . . . . .
N15 N 0.2294(3) 0.2742(3) 0.4063(8) 0.0404(10) Uani 1 1 d . . . . .
C3 C 0.1464(2) 0.1551(2) 0.2078(6) 0.0284(9) Uani 1 1 d . . . . .
H3 H 0.1890 0.1489 0.1536 0.034 Uiso 1 1 calc R U . . .
Cl1A Cl -0.0005(4) 0.3604(5) 0.1046(12) 0.0379(16) Uani 0.425(14) 1 d D . P A 1
O2A O -0.0221(15) 0.4173(14) 0.089(3) 0.24(2) Uani 0.425(14) 1 d D . P A 1
O1A O -0.0531(9) 0.2993(16) 0.216(3) 0.35(3) Uani 0.425(14) 1 d D . P A 1
O3A O 0.0763(8) 0.3933(8) 0.182(2) 0.102(7) Uani 0.425(14) 1 d D . P A 1
O4A O -0.0014(14) 0.3302(15) -0.071(2) 0.165(15) Uani 0.425(14) 1 d D . P A 1
Cl1B Cl 0.0035(4) 0.3439(5) 0.0935(10) 0.059(2) Uani 0.575(14) 1 d D . P A 2
O2B O 0.0516(6) 0.4059(7) -0.0310(14) 0.099(5) Uani 0.575(14) 1 d D . P A 2
O1B O -0.0748(6) 0.3177(14) 0.048(2) 0.264(18) Uani 0.575(14) 1 d D . P A 2
O3B O 0.0201(12) 0.3696(11) 0.2772(13) 0.174(9) Uani 0.575(14) 1 d D . P A 2
O4B O 0.0218(17) 0.2837(12) 0.069(3) 0.292(16) Uiso 0.575(14) 1 d D . P A 2
H15A H 0.236(4) 0.321(4) 0.372(9) 0.057(18) Uiso 1 1 d . . . . .
H15B H 0.217(5) 0.270(5) 0.513(12) 0.09(3) 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
Zn1 N6 2.167(3) 2_655 ?
Zn1 N6 2.167(3) 3_665 ?
Zn1 N6 2.167(3) . ?
Zn1 N4 2.167(3) 3_665 ?
Zn1 N4 2.167(3) . ?
Zn1 N4 2.167(3) 2_655 ?
N1 C1 1.331(5) . ?
N1 N2 1.332(5) . ?
N1 N5 1.401(5) . ?
N2 N3 1.295(5) . ?
N3 N4 1.358(5) . ?
N4 C1 1.297(5) . ?
N5 H5B 0.8755 . ?
N5 H5A 0.8994 . ?
N6 C2 1.311(5) . ?
N6 N7 1.366(5) . ?
N7 N8 1.293(6) . ?
N8 N9 1.330(6) . ?
N9 C2 1.330(6) . ?
N9 N10 1.381(6) . ?
N10 H10A 0.8565 . ?
N10 H10B 0.8612 . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
Zn2 N14 2.167(3) 4 ?
Zn2 N14 2.167(3) . ?
Zn2 N14 2.167(3) 6 ?
Zn2 N14 2.167(3) 2 ?
Zn2 N14 2.167(3) 5 ?
Zn2 N14 2.167(3) 3 ?
N11 C3 1.326(5) . ?
N11 N12 1.338(5) . ?
N11 N15 1.395(5) . ?
N12 N13 1.290(5) . ?
N13 N14 1.364(5) . ?
N14 C3 1.312(5) . ?
N15 H15A 0.86(7) . ?
N15 H15B 0.77(8) . ?
C3 H3 0.9500 . ?
Cl1A O1A 1.332(13) . ?
Cl1A O2A 1.333(13) . ?
Cl1A O4A 1.350(13) . ?
Cl1A O3A 1.373(11) . ?
Cl1B O1B 1.342(10) . ?
Cl1B O3B 1.354(11) . ?
Cl1B O4B 1.356(14) . ?
Cl1B O2B 1.377(10) . ?

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
N6 Zn1 N6 90.96(13) 2_655 3_665 ?
N6 Zn1 N6 90.96(13) 2_655 . ?
N6 Zn1 N6 90.96(13) 3_665 . ?
N6 Zn1 N4 88.03(13) 2_655 3_665 ?
N6 Zn1 N4 178.64(12) 3_665 3_665 ?
N6 Zn1 N4 89.96(13) . 3_665 ?
N6 Zn1 N4 89.96(13) 2_655 . ?
N6 Zn1 N4 88.03(13) 3_665 . ?
N6 Zn1 N4 178.64(12) . . ?
N4 Zn1 N4 91.07(13) 3_665 . ?
N6 Zn1 N4 178.64(12) 2_655 2_655 ?
N6 Zn1 N4 89.96(13) 3_665 2_655 ?
N6 Zn1 N4 88.03(13) . 2_655 ?
N4 Zn1 N4 91.07(13) 3_665 2_655 ?
N4 Zn1 N4 91.07(13) . 2_655 ?
C1 N1 N2 108.7(3) . . ?
C1 N1 N5 127.2(4) . . ?
N2 N1 N5 124.1(3) . . ?
N3 N2 N1 106.7(3) . . ?
N2 N3 N4 109.6(3) . . ?
C1 N4 N3 106.7(3) . . ?
C1 N4 Zn1 133.4(3) . . ?
N3 N4 Zn1 119.9(3) . . ?
N1 N5 H5B 103.4 . . ?
N1 N5 H5A 103.0 . . ?
H5B N5 H5A 109.6 . . ?
C2 N6 N7 106.3(3) . . ?
C2 N6 Zn1 133.6(3) . . ?
N7 N6 Zn1 120.0(3) . . ?
N8 N7 N6 109.4(4) . . ?
N7 N8 N9 107.1(4) . . ?
N8 N9 C2 109.0(4) . . ?
N8 N9 N10 122.9(5) . . ?
C2 N9 N10 128.0(5) . . ?
N9 N10 H10A 107.4 . . ?
N9 N10 H10B 112.3 . . ?
H10A N10 H10B 136.2 . . ?
N4 C1 N1 108.4(4) . . ?
N4 C1 H1 125.8 . . ?
N1 C1 H1 125.8 . . ?
N6 C2 N9 108.1(4) . . ?
N6 C2 H2 126.0 . . ?
N9 C2 H2 126.0 . . ?
N14 Zn2 N14 180.00(14) 4 . ?
N14 Zn2 N14 91.21(13) 4 6 ?
N14 Zn2 N14 88.79(13) . 6 ?
N14 Zn2 N14 88.79(13) 4 2 ?
N14 Zn2 N14 91.21(13) . 2 ?
N14 Zn2 N14 88.79(13) 6 2 ?
N14 Zn2 N14 91.21(13) 4 5 ?
N14 Zn2 N14 88.79(13) . 5 ?
N14 Zn2 N14 91.21(13) 6 5 ?
N14 Zn2 N14 180.00(13) 2 5 ?
N14 Zn2 N14 88.79(13) 4 3 ?
N14 Zn2 N14 91.21(13) . 3 ?
N14 Zn2 N14 180.0(2) 6 3 ?
N14 Zn2 N14 91.21(13) 2 3 ?
N14 Zn2 N14 88.79(13) 5 3 ?
C3 N11 N12 109.1(3) . . ?
C3 N11 N15 126.8(4) . . ?
N12 N11 N15 124.1(4) . . ?
N13 N12 N11 106.5(3) . . ?
N12 N13 N14 110.1(3) . . ?
C3 N14 N13 106.0(3) . . ?
C3 N14 Zn2 132.5(3) . . ?
N13 N14 Zn2 121.5(3) . . ?
N11 N15 H15A 108(4) . . ?
N11 N15 H15B 100(6) . . ?
H15A N15 H15B 105(7) . . ?
N14 C3 N11 108.3(4) . . ?
N14 C3 H3 125.8 . . ?
N11 C3 H3 125.8 . . ?
O1A Cl1A O2A 110.5(11) . . ?
O1A Cl1A O4A 108.5(11) . . ?
O2A Cl1A O4A 108.9(10) . . ?
O1A Cl1A O3A 109.0(9) . . ?
O2A Cl1A O3A 110.3(10) . . ?
O4A Cl1A O3A 109.5(9) . . ?
O1B Cl1B O3B 111.8(10) . . ?
O1B Cl1B O4B 111.0(11) . . ?
O3B Cl1B O4B 108.1(10) . . ?
O1B Cl1B O2B 107.6(8) . . ?
O3B Cl1B O2B 111.0(9) . . ?
O4B Cl1B O2B 107.3(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.1(5) . . . . ?
N5 N1 N2 N3 -179.5(4) . . . . ?
N1 N2 N3 N4 -0.1(5) . . . . ?
N2 N3 N4 C1 0.0(5) . . . . ?
N2 N3 N4 Zn1 177.2(3) . . . . ?
C2 N6 N7 N8 0.7(5) . . . . ?
Zn1 N6 N7 N8 -176.4(3) . . . . ?
N6 N7 N8 N9 -0.5(5) . . . . ?
N7 N8 N9 C2 0.1(5) . . . . ?
N7 N8 N9 N10 178.4(4) . . . . ?
N3 N4 C1 N1 0.1(5) . . . . ?
Zn1 N4 C1 N1 -176.5(3) . . . . ?
N2 N1 C1 N4 -0.2(5) . . . . ?
N5 N1 C1 N4 179.5(4) . . . . ?
N7 N6 C2 N9 -0.6(5) . . . . ?
Zn1 N6 C2 N9 175.9(3) . . . . ?
N8 N9 C2 N6 0.4(5) . . . . ?
N10 N9 C2 N6 -177.8(4) . . . . ?
C3 N11 N12 N13 -0.4(5) . . . . ?
N15 N11 N12 N13 -178.1(4) . . . . ?
N11 N12 N13 N14 0.4(5) . . . . ?
N12 N13 N14 C3 -0.2(5) . . . . ?
N12 N13 N14 Zn2 179.0(3) . . . . ?
N13 N14 C3 N11 0.0(5) . . . . ?
Zn2 N14 C3 N11 -179.1(3) . . . . ?
N12 N11 C3 N14 0.2(5) . . . . ?
N15 N11 C3 N14 177.9(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         3.072
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.133

_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_mx201
_database_code_depnum_ccdc_archive 'CCDC 1834853'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed May 10 14:48:25 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-amino-5H-tetrazolyl)copper(II) chlorate
;
_chemical_name_common            
'hexakis(1-amino-5H-tetrazolyl)copper(II) chlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C6 H18 Cu N30, 2(Cl O3)'
_chemical_formula_sum            'C6 H18 Cl2 Cu N30 O6'
_chemical_formula_weight         740.94

_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                   9.6517(3)
_cell_length_b                   7.8880(3)
_cell_length_c                   17.1904(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.923(2)
_cell_angle_gamma                90
_cell_volume                     1305.68(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4350
_cell_measurement_theta_min      4.7040
_cell_measurement_theta_max      32.1940

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.133
_shelx_estimated_absorpt_T_min   0.713
_shelx_estimated_absorpt_T_max   0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94003
_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    1.885
_exptl_crystal_F_000             750
_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            9613
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.182
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2549
_reflns_number_gt                2372
_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)+9.7701P] 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         2549
_refine_ls_number_parameters     229
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1411
_refine_ls_goodness_of_fit_ref   1.353
_refine_ls_restrained_S_all      1.353
_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      -0.0408196000
_diffrn_orient_matrix_UB_12      -0.0736542000
_diffrn_orient_matrix_UB_13      -0.0076934000
_diffrn_orient_matrix_UB_21      0.0488088000
_diffrn_orient_matrix_UB_22      -0.0487519000
_diffrn_orient_matrix_UB_23      0.0232085000
_diffrn_orient_matrix_UB_31      -0.0371126000
_diffrn_orient_matrix_UB_32      0.0168383000
_diffrn_orient_matrix_UB_33      0.0333604000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00   31.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000   60.0000 56

#__ type_ start__ end____ width___ exp.time_
  2 omega  -23.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -89.00   -1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -97.00  -32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000   60.0000 65

#__ type_ start__ end____ width___ exp.time_
  5 omega -100.00    1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000 -120.0000 101

#__ type_ start__ end____ width___ exp.time_
  6 omega   48.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000   90.0000 62

;



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 0.5000 0.0000 1.0000 0.0144(2) Uani 1 2 d S . P . .
Cl1 Cl 0.98277(13) 0.21778(17) 0.85805(8) 0.0186(3) Uani 1 1 d . . . . .
N3 N 0.6835(5) 0.2995(6) 0.9732(3) 0.0183(10) Uani 1 1 d . . . . .
N4 N 0.6704(4) 0.1551(6) 1.0165(2) 0.0146(9) Uani 1 1 d . . . . .
N8 N 0.4029(5) 0.1110(6) 0.8401(3) 0.0178(10) Uani 1 1 d . . . . .
N6 N 0.3455(4) 0.3700(5) 0.8482(2) 0.0128(9) Uani 1 1 d . . . . .
N7 N 0.3579(5) 0.2376(6) 0.7988(3) 0.0182(10) Uani 1 1 d . . . . .
O1 O 0.9905(4) 0.3824(6) 0.8165(3) 0.0301(10) Uani 1 1 d . . . . .
O2 O 1.0881(4) 0.2238(6) 0.9250(2) 0.0256(9) Uani 1 1 d . . . . .
N9 N 0.4202(4) 0.1590(6) 0.9171(2) 0.0135(9) Uani 1 1 d . . . . .
N2 N 0.8014(5) 0.3702(6) 0.9917(3) 0.0196(10) Uani 1 1 d . . . . .
N1 N 0.8657(4) 0.2721(6) 1.0475(2) 0.0145(9) Uani 1 1 d . . . . .
O3 O 1.0264(5) 0.0846(6) 0.8053(2) 0.0306(10) Uani 1 1 d . . . . .
N5 N 0.9979(5) 0.3094(6) 1.0818(3) 0.0201(10) Uani 1 1 d D . . . .
C1 C 0.7862(5) 0.1421(7) 1.0621(3) 0.0153(11) Uani 1 1 d . . . . .
H1 H 0.8080 0.0545 1.0989 0.018 Uiso 1 1 calc R U . . .
N10 N 0.2892(6) 0.5283(6) 0.8265(3) 0.0196(10) Uani 1 1 d . . . . .
C2 C 0.3837(5) 0.3196(7) 0.9203(3) 0.0135(10) Uani 1 1 d . . . . .
H2 H 0.3845 0.3873 0.9660 0.016 Uiso 1 1 calc R U . . .
N15 N 0.3860(5) 0.1541(6) 1.0979(3) 0.0166(10) Uani 1 1 d . . . . .
N12 N 0.2627(4) 0.2346(6) 1.1884(2) 0.0156(9) Uani 1 1 d . . . . .
N14 N 0.3861(5) 0.3262(6) 1.0994(3) 0.0201(10) Uani 1 1 d . . . . .
C3 C 0.3106(5) 0.0986(7) 1.1520(3) 0.0169(11) Uani 1 1 d . . . . .
H3 H 0.2926 -0.0167 1.1637 0.020 Uiso 1 1 calc R U . . .
N13 N 0.3077(6) 0.3753(7) 1.1550(3) 0.0314(13) Uani 1 1 d . . . . .
N16 N 0.1734(5) 0.2310(7) 1.2492(3) 0.0206(10) Uani 1 1 d . . . . .
H10A H 0.342(6) 0.579(8) 0.788(3) 0.016(15) Uiso 1 1 d . . . . .
H10B H 0.211(8) 0.509(10) 0.807(4) 0.04(2) Uiso 1 1 d . . . . .
H16B H 0.086(9) 0.207(11) 1.224(5) 0.05(2) Uiso 1 1 d . . . . .
H16A H 0.202(9) 0.140(12) 1.276(5) 0.06(3) Uiso 1 1 d . . . . .
H5B H 1.049(5) 0.311(7) 1.044(3) 0.013(15) Uiso 1 1 d D . . . .
H5A H 0.989(6) 0.399(6) 1.107(3) 0.022(17) Uiso 1 1 d 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 N9 2.012(4) 3_657 ?
Cu1 N9 2.012(4) . ?
Cu1 N4 2.054(4) 3_657 ?
Cu1 N4 2.054(4) . ?
Cu1 N15 2.404(4) . ?
Cu1 N15 2.404(4) 3_657 ?
Cl1 O3 1.468(4) . ?
Cl1 O2 1.483(4) . ?
Cl1 O1 1.486(5) . ?
N3 N2 1.288(6) . ?
N3 N4 1.372(6) . ?
N4 C1 1.325(7) . ?
N8 N7 1.284(6) . ?
N8 N9 1.375(6) . ?
N6 C2 1.330(6) . ?
N6 N7 1.356(6) . ?
N6 N10 1.402(6) . ?
N9 C2 1.317(7) . ?
N2 N1 1.350(6) . ?
N1 C1 1.316(7) . ?
N1 N5 1.399(6) . ?
N5 H5B 0.84(4) . ?
N5 H5A 0.84(4) . ?
C1 H1 0.9500 . ?
N10 H10A 0.95(6) . ?
N10 H10B 0.82(7) . ?
C2 H2 0.9500 . ?
N15 C3 1.296(7) . ?
N15 N14 1.358(6) . ?
N12 N13 1.335(7) . ?
N12 C3 1.340(7) . ?
N12 N16 1.400(6) . ?
N14 N13 1.318(7) . ?
C3 H3 0.9500 . ?
N16 H16B 0.94(8) . ?
N16 H16A 0.89(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N9 Cu1 N9 180.0 3_657 . ?
N9 Cu1 N4 89.45(17) 3_657 3_657 ?
N9 Cu1 N4 90.55(17) . 3_657 ?
N9 Cu1 N4 90.55(17) 3_657 . ?
N9 Cu1 N4 89.45(17) . . ?
N4 Cu1 N4 180.0 3_657 . ?
N9 Cu1 N15 89.44(16) 3_657 . ?
N9 Cu1 N15 90.56(16) . . ?
N4 Cu1 N15 89.84(16) 3_657 . ?
N4 Cu1 N15 90.16(16) . . ?
N9 Cu1 N15 90.56(16) 3_657 3_657 ?
N9 Cu1 N15 89.44(16) . 3_657 ?
N4 Cu1 N15 90.16(16) 3_657 3_657 ?
N4 Cu1 N15 89.84(16) . 3_657 ?
N15 Cu1 N15 180.00(18) . 3_657 ?
O3 Cl1 O2 107.0(3) . . ?
O3 Cl1 O1 107.6(3) . . ?
O2 Cl1 O1 106.9(3) . . ?
N2 N3 N4 109.8(4) . . ?
C1 N4 N3 106.3(4) . . ?
C1 N4 Cu1 132.1(4) . . ?
N3 N4 Cu1 121.5(3) . . ?
N7 N8 N9 109.4(4) . . ?
C2 N6 N7 108.8(4) . . ?
C2 N6 N10 126.3(4) . . ?
N7 N6 N10 124.7(4) . . ?
N8 N7 N6 107.1(4) . . ?
C2 N9 N8 106.8(4) . . ?
C2 N9 Cu1 131.3(4) . . ?
N8 N9 Cu1 121.7(3) . . ?
N3 N2 N1 106.4(4) . . ?
C1 N1 N2 109.7(4) . . ?
C1 N1 N5 127.6(5) . . ?
N2 N1 N5 122.7(4) . . ?
N1 N5 H5B 104(4) . . ?
N1 N5 H5A 106(4) . . ?
H5B N5 H5A 119(5) . . ?
N1 C1 N4 107.8(5) . . ?
N1 C1 H1 126.1 . . ?
N4 C1 H1 126.1 . . ?
N6 N10 H10A 110(4) . . ?
N6 N10 H10B 106(6) . . ?
H10A N10 H10B 109(6) . . ?
N9 C2 N6 107.9(5) . . ?
N9 C2 H2 126.1 . . ?
N6 C2 H2 126.1 . . ?
C3 N15 N14 108.9(4) . . ?
C3 N15 Cu1 129.7(4) . . ?
N14 N15 Cu1 121.2(3) . . ?
N13 N12 C3 109.4(4) . . ?
N13 N12 N16 124.9(5) . . ?
C3 N12 N16 125.6(5) . . ?
N13 N14 N15 107.9(4) . . ?
N15 C3 N12 107.0(5) . . ?
N15 C3 H3 126.5 . . ?
N12 C3 H3 126.5 . . ?
N14 N13 N12 106.7(5) . . ?
N12 N16 H16B 104(5) . . ?
N12 N16 H16A 103(6) . . ?
H16B N16 H16A 108(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 N3 N4 C1 0.0(6) . . . . ?
N2 N3 N4 Cu1 -176.9(3) . . . . ?
N9 N8 N7 N6 0.2(6) . . . . ?
C2 N6 N7 N8 -0.3(6) . . . . ?
N10 N6 N7 N8 -174.9(5) . . . . ?
N7 N8 N9 C2 0.0(6) . . . . ?
N7 N8 N9 Cu1 -176.4(3) . . . . ?
N4 N3 N2 N1 -0.2(6) . . . . ?
N3 N2 N1 C1 0.3(6) . . . . ?
N3 N2 N1 N5 179.7(5) . . . . ?
N2 N1 C1 N4 -0.2(6) . . . . ?
N5 N1 C1 N4 -179.7(5) . . . . ?
N3 N4 C1 N1 0.1(6) . . . . ?
Cu1 N4 C1 N1 176.6(4) . . . . ?
N8 N9 C2 N6 -0.2(5) . . . . ?
Cu1 N9 C2 N6 175.8(3) . . . . ?
N7 N6 C2 N9 0.3(6) . . . . ?
N10 N6 C2 N9 174.8(5) . . . . ?
C3 N15 N14 N13 -0.8(7) . . . . ?
Cu1 N15 N14 N13 175.3(4) . . . . ?
N14 N15 C3 N12 -0.2(6) . . . . ?
Cu1 N15 C3 N12 -175.8(3) . . . . ?
N13 N12 C3 N15 1.1(6) . . . . ?
N16 N12 C3 N15 178.0(5) . . . . ?
N15 N14 N13 N12 1.4(6) . . . . ?
C3 N12 N13 N14 -1.5(6) . . . . ?
N16 N12 N13 N14 -178.5(5) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N8 0.95 2.69 3.250(7) 118.3 3_657
C1 H1 O2 0.95 2.46 3.133(7) 127.8 3_757
C1 H1 O3 0.95 2.47 3.332(7) 150.4 3_757
C2 H2 N14 0.95 2.34 3.078(7) 133.9 .
C3 H3 N16 0.95 2.50 3.359(7) 150.6 2_547
N10 H10A O3 0.95(6) 2.11(6) 3.009(7) 156(5) 2_656
N10 H10B O1 0.82(7) 2.36(8) 3.098(7) 150(7) 1_455
N16 H16B N7 0.94(8) 2.66(8) 3.228(7) 119(6) 4_566
N16 H16B O3 0.94(8) 2.58(9) 3.247(7) 129(7) 3_657
N16 H16B N5 0.94(8) 2.66(8) 3.297(7) 125(6) 1_455
N16 H16A N13 0.89(10) 2.40(10) 3.252(8) 160(8) 2_547
N5 H5B O2 0.84(4) 2.21(4) 2.967(7) 149(5) .
N5 H5A O1 0.84(4) 2.17(4) 2.993(7) 168(6) 3_767
C1 H1 N8 0.95 2.69 3.250(7) 118.3 3_657
C1 H1 O2 0.95 2.46 3.133(7) 127.8 3_757
C1 H1 O3 0.95 2.47 3.332(7) 150.4 3_757
C2 H2 N14 0.95 2.34 3.078(7) 133.9 .
C3 H3 N16 0.95 2.50 3.359(7) 150.6 2_547
N10 H10A O3 0.95(6) 2.11(6) 3.009(7) 156(5) 2_656
N10 H10B O1 0.82(7) 2.36(8) 3.098(7) 150(7) 1_455
N16 H16B N7 0.94(8) 2.66(8) 3.228(7) 119(6) 4_566
N16 H16B O3 0.94(8) 2.58(9) 3.247(7) 129(7) 3_657
N16 H16B N5 0.94(8) 2.66(8) 3.297(7) 125(6) 1_455
N16 H16A N13 0.89(10) 2.40(10) 3.252(8) 160(8) 2_547
N5 H5B O2 0.84(4) 2.21(4) 2.967(7) 149(5) .
N5 H5A O1 0.84(4) 2.17(4) 2.993(7) 168(6) 3_767

_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         0.813
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.112

_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_mx
_database_code_depnum_ccdc_archive 'CCDC 1838980'
_audit_update_record             
;
2018-04-23 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             2018-04-07
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(2-aminotetrazolyl)copper(II) perchlorate * 2 2-aminotetrazole
;
_chemical_name_common            
'hexakis(2-aminotetrazolyl)copper(II) perchlorate * 2 2-aminotetrazole'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C6 H18 Cu N30, 2(C H3 N5), 2(Cl O4)'
_chemical_formula_sum            'C8 H24 Cl2 Cu N40 O8'
_chemical_formula_weight         943.11

_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                   10.3015(7)
_cell_length_b                   10.8660(7)
_cell_length_c                   16.4236(11)
_cell_angle_alpha                80.433(6)
_cell_angle_beta                 73.574(6)
_cell_angle_gamma                80.646(5)
_cell_volume                     1725.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    3172
_cell_measurement_theta_min      4.5590
_cell_measurement_theta_max      29.6350

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.891
_shelx_estimated_absorpt_T_min   0.717
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97300
_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    1.815
_exptl_crystal_F_000             958
_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            13551
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0910
_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       20
_diffrn_reflns_theta_min         4.130
_diffrn_reflns_theta_max         26.000
_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             6759
_reflns_number_gt                5061
_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)+(0.0326P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6759
_refine_ls_number_parameters     599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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      0.0143145000
_diffrn_orient_matrix_UB_12      0.0627222000
_diffrn_orient_matrix_UB_13      -0.0149549000
_diffrn_orient_matrix_UB_21      -0.0691290000
_diffrn_orient_matrix_UB_22      0.0223667000
_diffrn_orient_matrix_UB_23      0.0182119000
_diffrn_orient_matrix_UB_31      0.0157234000
_diffrn_orient_matrix_UB_32      0.0037627000
_diffrn_orient_matrix_UB_33      0.0387975000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  11.00   1.00    7.00    --   29.79 -99.00  90.00   26
  2  ω    -22.00  66.00   1.00    7.00    --   29.79 -99.00  30.00   88
  3  ω     49.00  75.00   1.00    7.00    --   29.79 -99.00  90.00   26
  4  ω    -99.00 -58.00   1.00    7.00    --  -28.70-179.00   0.00   41
  5  ω   -100.00   4.00   1.00    7.00    --  -28.70 -77.00-180.00  104
  6  ω   -101.00  36.00   1.00    7.00    --  -28.70   0.00   0.00  137
  7  ω     60.00 110.00   1.00    7.00    --   29.79 179.00  30.00   50
;



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 0.0000 1.0000 0.0000 0.01505(13) Uani 1 2 d S . P . .
N1 N 0.1950(2) 0.6734(2) -0.11250(15) 0.0192(6) Uani 1 1 d . . . . .
N2 N 0.2797(2) 0.6975(2) -0.07095(14) 0.0155(5) Uani 1 1 d . . . . .
N3 N 0.2410(2) 0.7978(2) -0.03128(14) 0.0161(5) Uani 1 1 d . . . . .
N4 N 0.1207(2) 0.8439(2) -0.04750(14) 0.0154(5) Uani 1 1 d . . . . .
N5 N 0.3983(3) 0.6175(2) -0.06814(19) 0.0202(6) Uani 1 1 d . . . . .
N6 N -0.1102(3) 0.8453(2) 0.25637(15) 0.0217(6) Uani 1 1 d . . . . .
N7 N 0.0249(2) 0.8377(2) 0.23333(14) 0.0166(5) Uani 1 1 d . . . . .
N8 N 0.0813(2) 0.8757(2) 0.15329(14) 0.0174(5) Uani 1 1 d . . . . .
N9 N -0.0256(2) 0.9127(2) 0.11975(14) 0.0149(5) Uani 1 1 d . . . . .
N10 N 0.1008(3) 0.7844(3) 0.29121(19) 0.0257(7) Uani 1 1 d . . . . .
N11 N 0.3891(2) 1.1199(2) 0.03413(14) 0.0170(5) Uani 1 1 d . . . . .
N12 N 0.3240(2) 1.2235(2) 0.00121(14) 0.0152(5) Uani 1 1 d . . . . .
N13 N 0.2105(2) 1.2072(2) -0.01591(14) 0.0178(5) Uani 1 1 d . . . . .
N14 N 0.1997(2) 1.0857(2) 0.00697(14) 0.0169(5) Uani 1 1 d . . . . .
N15 N 0.3760(3) 1.3382(2) -0.01349(19) 0.0210(6) Uani 1 1 d . . . . .
C1 C 0.0968(3) 0.7683(3) -0.09706(17) 0.0181(6) Uani 1 1 d . . . . .
H1 H 0.0186 0.7814 -0.1186 0.022 Uiso 1 1 calc R U . . .
C2 C -0.1386(3) 0.8936(3) 0.18288(17) 0.0176(6) Uani 1 1 d . . . . .
H2 H -0.2284 0.9125 0.1758 0.021 Uiso 1 1 calc R U . . .
C3 C 0.3085(3) 1.0356(3) 0.03663(17) 0.0176(6) Uani 1 1 d . . . . .
H3 H 0.3255 0.9491 0.0571 0.021 Uiso 1 1 calc R U . . .
Cu2 Cu 0.5000 0.0000 0.5000 0.01283(12) Uani 1 2 d S . P . .
N16 N 0.1497(2) -0.1799(2) 0.47197(14) 0.0171(5) Uani 1 1 d . . . . .
N17 N 0.2267(2) -0.2638(2) 0.51230(14) 0.0154(5) Uani 1 1 d . . . . .
N18 N 0.3278(2) -0.2203(2) 0.52756(14) 0.0174(5) Uani 1 1 d . . . . .
N19 N 0.3181(2) -0.0993(2) 0.49560(14) 0.0175(5) Uani 1 1 d . . . . .
N20 N 0.1978(3) -0.3869(2) 0.53932(18) 0.0194(6) Uani 1 1 d . . . . .
N21 N 0.2591(3) 0.3386(2) 0.57843(15) 0.0190(6) Uani 1 1 d . . . . .
N22 N 0.1943(2) 0.2907(2) 0.53407(14) 0.0164(5) Uani 1 1 d . . . . .
N23 N 0.2528(2) 0.1834(2) 0.50676(14) 0.0167(5) Uani 1 1 d . . . . .
N24 N 0.3645(2) 0.1575(2) 0.53448(14) 0.0151(5) Uani 1 1 d . . . . .
N25 N 0.0726(3) 0.3534(3) 0.51870(19) 0.0245(6) Uani 1 1 d . . . . .
N26 N 0.6237(2) 0.1338(2) 0.23999(14) 0.0188(5) Uani 1 1 d . . . . .
N27 N 0.4900(2) 0.1348(2) 0.25882(14) 0.0148(5) Uani 1 1 d . . . . .
N28 N 0.4295(2) 0.0973(2) 0.33834(14) 0.0156(5) Uani 1 1 d . . . . .
N29 N 0.5321(2) 0.0687(2) 0.37612(14) 0.0139(5) Uani 1 1 d . . . . .
N30 N 0.4178(3) 0.1819(3) 0.19830(18) 0.0218(6) Uani 1 1 d . . . . .
C4 C 0.2108(3) -0.0781(3) 0.46219(17) 0.0169(6) Uani 1 1 d . . . . .
H4 H 0.1817 0.0013 0.4345 0.020 Uiso 1 1 calc R U . . .
C5 C 0.3664(3) 0.2524(3) 0.57699(17) 0.0179(6) Uani 1 1 d . . . . .
H5 H 0.4365 0.2571 0.6030 0.021 Uiso 1 1 calc R U . . .
C6 C 0.6466(3) 0.0909(3) 0.31584(17) 0.0164(6) Uani 1 1 d . . . . .
H6 H 0.7345 0.0776 0.3260 0.020 Uiso 1 1 calc R U . . .
N31 N 0.4923(3) 0.4206(2) 0.26351(16) 0.0265(6) Uani 1 1 d . . . . .
N32 N 0.5538(2) 0.4551(2) 0.31533(15) 0.0183(5) Uani 1 1 d . . . . .
N33 N 0.4726(3) 0.4883(3) 0.38713(15) 0.0277(6) Uani 1 1 d . . . . .
N34 N 0.3480(3) 0.4765(3) 0.38381(16) 0.0286(6) Uani 1 1 d . . . . .
N35 N 0.6942(3) 0.4582(3) 0.29805(18) 0.0227(6) Uani 1 1 d . . . . .
C7 C 0.3636(3) 0.4338(3) 0.3092(2) 0.0292(8) Uani 1 1 d . . . . .
H7 H 0.2901 0.4150 0.2911 0.035 Uiso 1 1 calc R U . . .
N36 N -0.0513(3) 0.5722(2) 0.18925(16) 0.0273(6) Uani 1 1 d . . . . .
N37 N 0.0479(3) 0.5141(2) 0.22362(16) 0.0222(6) Uani 1 1 d . . . . .
N38 N 0.1565(3) 0.4656(3) 0.16940(17) 0.0330(7) Uani 1 1 d . . . . .
N39 N 0.1296(3) 0.4932(3) 0.09379(17) 0.0337(7) Uani 1 1 d . . . . .
N40 N 0.0424(3) 0.4995(3) 0.31065(18) 0.0271(6) Uani 1 1 d . . . . .
C8 C 0.0041(4) 0.5572(3) 0.1077(2) 0.0293(8) Uani 1 1 d . . . . .
H8 H -0.0403 0.5886 0.0637 0.035 Uiso 1 1 calc R U . . .
Cl1 Cl 0.03582(7) 0.15808(7) 0.29622(4) 0.01989(17) Uani 1 1 d . . . . .
O1 O 0.1198(2) 0.1288(2) 0.21373(13) 0.0356(6) Uani 1 1 d . . . . .
O2 O -0.0239(2) 0.0481(2) 0.34333(14) 0.0354(6) Uani 1 1 d . . . . .
O3 O -0.0715(2) 0.2568(2) 0.28509(14) 0.0305(6) Uani 1 1 d . . . . .
O4 O 0.1181(2) 0.1979(2) 0.34199(14) 0.0302(5) Uani 1 1 d . . . . .
Cl2 Cl 0.48419(8) 0.79632(7) 0.21619(4) 0.02170(18) Uani 1 1 d . . . . .
O5 O 0.3951(3) 0.7630(3) 0.17314(15) 0.0470(7) Uani 1 1 d . . . . .
O6 O 0.5323(3) 0.9123(2) 0.17348(16) 0.0423(6) Uani 1 1 d . . . . .
O7 O 0.4119(3) 0.8079(3) 0.30282(14) 0.0514(8) Uani 1 1 d . . . . .
O8 O 0.5995(3) 0.7022(2) 0.21141(16) 0.0511(7) Uani 1 1 d . . . . .
H21A H 0.233(3) -0.424(3) 0.4954(19) 0.022(9) Uiso 1 1 d . . . . .
H30B H 0.446(3) 0.135(3) 0.1596(19) 0.019(9) Uiso 1 1 d . . . . .
H25A H 0.025(4) 0.295(3) 0.512(2) 0.035(10) Uiso 1 1 d . . . . .
H22B H 0.236(3) -0.419(3) 0.585(2) 0.035(10) Uiso 1 1 d . . . . .
H5B H 0.435(3) 0.643(3) -0.039(2) 0.021(9) Uiso 1 1 d . . . . .
H35A H 0.731(4) 0.401(4) 0.266(2) 0.050(12) Uiso 1 1 d . . . . .
H35B H 0.714(4) 0.532(4) 0.264(2) 0.053(12) Uiso 1 1 d . . . . .
H30A H 0.337(4) 0.181(3) 0.220(2) 0.036(12) Uiso 1 1 d . . . . .
H25B H 0.096(4) 0.397(4) 0.473(2) 0.049(13) Uiso 1 1 d . . . . .
H5A H 0.446(3) 0.617(3) -0.124(2) 0.022(8) Uiso 1 1 d . . . . .
H15B H 0.307(4) 1.393(3) 0.008(2) 0.035(10) Uiso 1 1 d . . . . .
H10B H 0.181(3) 0.772(3) 0.2656(19) 0.021(10) Uiso 1 1 d . . . . .
H40B H 0.026(4) 0.575(4) 0.327(2) 0.052(12) Uiso 1 1 d . . . . .
H15A H 0.406(4) 1.357(3) -0.067(2) 0.040(11) Uiso 1 1 d . . . . .
H10A H 0.083(3) 0.839(3) 0.327(2) 0.034(10) Uiso 1 1 d . . . . .
H40A H -0.023(4) 0.458(4) 0.336(2) 0.044(12) 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 N9 2.001(2) 2_575 ?
Cu1 N9 2.001(2) . ?
Cu1 N4 2.059(2) . ?
Cu1 N4 2.059(2) 2_575 ?
Cu1 N14 2.430(2) . ?
Cu1 N14 2.430(2) 2_575 ?
N1 C1 1.324(3) . ?
N1 N2 1.329(3) . ?
N2 N3 1.311(3) . ?
N2 N5 1.387(3) . ?
N3 N4 1.342(3) . ?
N4 C1 1.341(3) . ?
N5 H5B 0.80(3) . ?
N5 H5A 0.91(3) . ?
N6 C2 1.326(3) . ?
N6 N7 1.327(3) . ?
N7 N8 1.305(3) . ?
N7 N10 1.393(3) . ?
N8 N9 1.343(3) . ?
N9 C2 1.340(4) . ?
N10 H10B 0.81(3) . ?
N10 H10A 0.87(3) . ?
N11 C3 1.321(4) . ?
N11 N12 1.329(3) . ?
N12 N13 1.321(3) . ?
N12 N15 1.394(3) . ?
N13 N14 1.325(3) . ?
N14 C3 1.346(3) . ?
N15 H15B 0.88(3) . ?
N15 H15A 0.85(4) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
Cu2 N29 2.000(2) 2_656 ?
Cu2 N29 2.000(2) . ?
Cu2 N24 2.073(2) . ?
Cu2 N24 2.073(2) 2_656 ?
Cu2 N19 2.332(2) . ?
Cu2 N19 2.332(2) 2_656 ?
N16 C4 1.325(4) . ?
N16 N17 1.326(3) . ?
N17 N18 1.310(3) . ?
N17 N20 1.390(3) . ?
N18 N19 1.331(3) . ?
N19 C4 1.340(3) . ?
N20 H21A 0.84(3) . ?
N20 H22B 0.93(3) . ?
N21 C5 1.324(3) . ?
N21 N22 1.327(3) . ?
N22 N23 1.310(3) . ?
N22 N25 1.394(3) . ?
N23 N24 1.326(3) . ?
N24 C5 1.343(3) . ?
N25 H25A 0.90(4) . ?
N25 H25B 0.81(4) . ?
N26 N27 1.321(3) . ?
N26 C6 1.328(3) . ?
N27 N28 1.306(3) . ?
N27 N30 1.389(3) . ?
N28 N29 1.341(3) . ?
N29 C6 1.336(4) . ?
N30 H30B 0.84(3) . ?
N30 H30A 0.81(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N31 C7 1.324(4) . ?
N31 N32 1.325(3) . ?
N32 N33 1.306(3) . ?
N32 N35 1.397(3) . ?
N33 N34 1.328(4) . ?
N34 C7 1.340(4) . ?
N35 H35A 0.85(4) . ?
N35 H35B 0.91(4) . ?
C7 H7 0.9500 . ?
N36 C8 1.325(4) . ?
N36 N37 1.327(3) . ?
N37 N38 1.313(3) . ?
N37 N40 1.397(3) . ?
N38 N39 1.324(4) . ?
N39 C8 1.342(4) . ?
N40 H40B 0.89(4) . ?
N40 H40A 0.85(4) . ?
C8 H8 0.9500 . ?
Cl1 O4 1.435(2) . ?
Cl1 O2 1.438(2) . ?
Cl1 O3 1.439(2) . ?
Cl1 O1 1.441(2) . ?
Cl2 O7 1.423(2) . ?
Cl2 O5 1.426(2) . ?
Cl2 O6 1.428(2) . ?
Cl2 O8 1.429(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
N9 Cu1 N9 180.0 2_575 . ?
N9 Cu1 N4 89.25(9) 2_575 . ?
N9 Cu1 N4 90.75(9) . . ?
N9 Cu1 N4 90.75(9) 2_575 2_575 ?
N9 Cu1 N4 89.25(9) . 2_575 ?
N4 Cu1 N4 180.0 . 2_575 ?
N9 Cu1 N14 88.39(8) 2_575 . ?
N9 Cu1 N14 91.61(8) . . ?
N4 Cu1 N14 90.66(8) . . ?
N4 Cu1 N14 89.34(8) 2_575 . ?
N9 Cu1 N14 91.61(8) 2_575 2_575 ?
N9 Cu1 N14 88.39(8) . 2_575 ?
N4 Cu1 N14 89.34(8) . 2_575 ?
N4 Cu1 N14 90.66(8) 2_575 2_575 ?
N14 Cu1 N14 180.0 . 2_575 ?
C1 N1 N2 101.1(2) . . ?
N3 N2 N1 115.7(2) . . ?
N3 N2 N5 123.2(2) . . ?
N1 N2 N5 121.0(2) . . ?
N2 N3 N4 103.8(2) . . ?
C1 N4 N3 107.1(2) . . ?
C1 N4 Cu1 128.79(19) . . ?
N3 N4 Cu1 124.14(16) . . ?
N2 N5 H5B 108(2) . . ?
N2 N5 H5A 104.5(19) . . ?
H5B N5 H5A 116(3) . . ?
C2 N6 N7 100.8(2) . . ?
N8 N7 N6 116.4(2) . . ?
N8 N7 N10 122.6(3) . . ?
N6 N7 N10 120.9(2) . . ?
N7 N8 N9 103.4(2) . . ?
C2 N9 N8 107.3(2) . . ?
C2 N9 Cu1 131.43(19) . . ?
N8 N9 Cu1 120.75(19) . . ?
N7 N10 H10B 109(2) . . ?
N7 N10 H10A 104(2) . . ?
H10B N10 H10A 114(3) . . ?
C3 N11 N12 101.1(2) . . ?
N13 N12 N11 114.9(2) . . ?
N13 N12 N15 124.5(2) . . ?
N11 N12 N15 120.6(2) . . ?
N12 N13 N14 104.8(2) . . ?
N13 N14 C3 106.6(2) . . ?
N13 N14 Cu1 120.32(17) . . ?
C3 N14 Cu1 132.93(19) . . ?
N12 N15 H15B 106(2) . . ?
N12 N15 H15A 108(2) . . ?
H15B N15 H15A 111(3) . . ?
N1 C1 N4 112.2(2) . . ?
N1 C1 H1 123.9 . . ?
N4 C1 H1 123.9 . . ?
N6 C2 N9 112.0(3) . . ?
N6 C2 H2 124.0 . . ?
N9 C2 H2 124.0 . . ?
N11 C3 N14 112.7(3) . . ?
N11 C3 H3 123.7 . . ?
N14 C3 H3 123.7 . . ?
N29 Cu2 N29 180.0 2_656 . ?
N29 Cu2 N24 89.09(9) 2_656 . ?
N29 Cu2 N24 90.91(9) . . ?
N29 Cu2 N24 90.91(9) 2_656 2_656 ?
N29 Cu2 N24 89.09(9) . 2_656 ?
N24 Cu2 N24 180.0 . 2_656 ?
N29 Cu2 N19 88.33(9) 2_656 . ?
N29 Cu2 N19 91.67(9) . . ?
N24 Cu2 N19 89.32(8) . . ?
N24 Cu2 N19 90.68(8) 2_656 . ?
N29 Cu2 N19 91.67(9) 2_656 2_656 ?
N29 Cu2 N19 88.33(9) . 2_656 ?
N24 Cu2 N19 90.68(8) . 2_656 ?
N24 Cu2 N19 89.32(8) 2_656 2_656 ?
N19 Cu2 N19 180.0 . 2_656 ?
C4 N16 N17 101.1(2) . . ?
N18 N17 N16 114.9(2) . . ?
N18 N17 N20 122.9(2) . . ?
N16 N17 N20 122.1(2) . . ?
N17 N18 N19 105.0(2) . . ?
N18 N19 C4 106.3(2) . . ?
N18 N19 Cu2 113.12(17) . . ?
C4 N19 Cu2 140.0(2) . . ?
N17 N20 H21A 104(2) . . ?
N17 N20 H22B 109(2) . . ?
H21A N20 H22B 113(3) . . ?
C5 N21 N22 100.9(2) . . ?
N23 N22 N21 115.5(2) . . ?
N23 N22 N25 123.9(2) . . ?
N21 N22 N25 120.7(2) . . ?
N22 N23 N24 104.5(2) . . ?
N23 N24 C5 106.9(2) . . ?
N23 N24 Cu2 119.11(17) . . ?
C5 N24 Cu2 133.83(19) . . ?
N22 N25 H25A 108(2) . . ?
N22 N25 H25B 104(3) . . ?
H25A N25 H25B 108(3) . . ?
N27 N26 C6 100.7(2) . . ?
N28 N27 N26 116.4(2) . . ?
N28 N27 N30 122.2(2) . . ?
N26 N27 N30 121.3(2) . . ?
N27 N28 N29 103.6(2) . . ?
C6 N29 N28 107.1(2) . . ?
C6 N29 Cu2 131.35(19) . . ?
N28 N29 Cu2 121.49(18) . . ?
N27 N30 H30B 106(2) . . ?
N27 N30 H30A 109(2) . . ?
H30B N30 H30A 112(3) . . ?
N16 C4 N19 112.6(3) . . ?
N16 C4 H4 123.7 . . ?
N19 C4 H4 123.7 . . ?
N21 C5 N24 112.2(2) . . ?
N21 C5 H5 123.9 . . ?
N24 C5 H5 123.9 . . ?
N26 C6 N29 112.2(3) . . ?
N26 C6 H6 123.9 . . ?
N29 C6 H6 123.9 . . ?
C7 N31 N32 100.9(2) . . ?
N33 N32 N31 114.9(2) . . ?
N33 N32 N35 120.0(2) . . ?
N31 N32 N35 125.0(2) . . ?
N32 N33 N34 105.5(2) . . ?
N33 N34 C7 105.9(3) . . ?
N32 N35 H35A 105(3) . . ?
N32 N35 H35B 108(2) . . ?
H35A N35 H35B 105(3) . . ?
N31 C7 N34 112.9(3) . . ?
N31 C7 H7 123.6 . . ?
N34 C7 H7 123.6 . . ?
C8 N36 N37 100.7(3) . . ?
N38 N37 N36 115.0(2) . . ?
N38 N37 N40 119.8(3) . . ?
N36 N37 N40 125.1(2) . . ?
N37 N38 N39 105.2(2) . . ?
N38 N39 C8 106.1(3) . . ?
N37 N40 H40B 108(2) . . ?
N37 N40 H40A 106(2) . . ?
H40B N40 H40A 110(4) . . ?
N36 C8 N39 113.0(3) . . ?
N36 C8 H8 123.5 . . ?
N39 C8 H8 123.5 . . ?
O4 Cl1 O2 109.93(14) . . ?
O4 Cl1 O3 109.78(12) . . ?
O2 Cl1 O3 108.95(14) . . ?
O4 Cl1 O1 109.32(14) . . ?
O2 Cl1 O1 109.26(14) . . ?
O3 Cl1 O1 109.58(13) . . ?
O7 Cl2 O5 109.08(16) . . ?
O7 Cl2 O6 110.77(16) . . ?
O5 Cl2 O6 108.77(16) . . ?
O7 Cl2 O8 110.92(16) . . ?
O5 Cl2 O8 109.33(16) . . ?
O6 Cl2 O8 107.93(16) . . ?

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 0.5(3) . . . . ?
C1 N1 N2 N5 178.3(3) . . . . ?
N1 N2 N3 N4 0.2(3) . . . . ?
N5 N2 N3 N4 -177.4(2) . . . . ?
N2 N3 N4 C1 -0.9(3) . . . . ?
N2 N3 N4 Cu1 177.88(17) . . . . ?
C2 N6 N7 N8 -0.4(3) . . . . ?
C2 N6 N7 N10 -176.6(2) . . . . ?
N6 N7 N8 N9 0.3(3) . . . . ?
N10 N7 N8 N9 176.4(2) . . . . ?
N7 N8 N9 C2 -0.1(3) . . . . ?
N7 N8 N9 Cu1 172.59(16) . . . . ?
C3 N11 N12 N13 0.1(3) . . . . ?
C3 N11 N12 N15 -179.5(2) . . . . ?
N11 N12 N13 N14 0.0(3) . . . . ?
N15 N12 N13 N14 179.6(2) . . . . ?
N12 N13 N14 C3 -0.1(3) . . . . ?
N12 N13 N14 Cu1 175.63(15) . . . . ?
N2 N1 C1 N4 -1.1(3) . . . . ?
N3 N4 C1 N1 1.3(3) . . . . ?
Cu1 N4 C1 N1 -177.39(19) . . . . ?
N7 N6 C2 N9 0.4(3) . . . . ?
N8 N9 C2 N6 -0.2(3) . . . . ?
Cu1 N9 C2 N6 -171.77(18) . . . . ?
N12 N11 C3 N14 -0.2(3) . . . . ?
N13 N14 C3 N11 0.2(3) . . . . ?
Cu1 N14 C3 N11 -174.77(16) . . . . ?
C4 N16 N17 N18 0.2(3) . . . . ?
C4 N16 N17 N20 177.6(2) . . . . ?
N16 N17 N18 N19 0.1(3) . . . . ?
N20 N17 N18 N19 -177.2(2) . . . . ?
N17 N18 N19 C4 -0.5(3) . . . . ?
N17 N18 N19 Cu2 -173.79(15) . . . . ?
C5 N21 N22 N23 0.4(3) . . . . ?
C5 N21 N22 N25 -179.4(3) . . . . ?
N21 N22 N23 N24 -0.1(3) . . . . ?
N25 N22 N23 N24 179.7(3) . . . . ?
N22 N23 N24 C5 -0.2(3) . . . . ?
N22 N23 N24 Cu2 -175.97(17) . . . . ?
C6 N26 N27 N28 0.2(3) . . . . ?
C6 N26 N27 N30 175.7(2) . . . . ?
N26 N27 N28 N29 0.0(3) . . . . ?
N30 N27 N28 N29 -175.4(2) . . . . ?
N27 N28 N29 C6 -0.2(3) . . . . ?
N27 N28 N29 Cu2 -178.17(16) . . . . ?
N17 N16 C4 N19 -0.5(3) . . . . ?
N18 N19 C4 N16 0.7(3) . . . . ?
Cu2 N19 C4 N16 171.08(19) . . . . ?
N22 N21 C5 N24 -0.5(3) . . . . ?
N23 N24 C5 N21 0.5(3) . . . . ?
Cu2 N24 C5 N21 175.4(2) . . . . ?
N27 N26 C6 N29 -0.4(3) . . . . ?
N28 N29 C6 N26 0.4(3) . . . . ?
Cu2 N29 C6 N26 178.04(18) . . . . ?
C7 N31 N32 N33 -0.5(3) . . . . ?
C7 N31 N32 N35 179.7(3) . . . . ?
N31 N32 N33 N34 -0.5(3) . . . . ?
N35 N32 N33 N34 179.4(3) . . . . ?
N32 N33 N34 C7 1.2(3) . . . . ?
N32 N31 C7 N34 1.2(4) . . . . ?
N33 N34 C7 N31 -1.6(4) . . . . ?
C8 N36 N37 N38 -0.5(3) . . . . ?
C8 N36 N37 N40 -178.8(3) . . . . ?
N36 N37 N38 N39 0.5(4) . . . . ?
N40 N37 N38 N39 178.9(3) . . . . ?
N37 N38 N39 C8 -0.3(3) . . . . ?
N37 N36 C8 N39 0.3(4) . . . . ?
N38 N39 C8 N36 0.0(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
N20 H21A N34 0.84(3) 2.22(3) 3.066(4) 174(3) 1_545
N30 H30B N11 0.84(3) 2.34(3) 2.988(3) 135(3) 1_545
N30 H30B O6 0.84(3) 2.43(3) 3.023(4) 128(2) 1_545
N25 H25A N16 0.90(4) 2.29(4) 3.152(4) 161(3) 2_556
N25 H25A N20 0.90(4) 2.65(3) 3.140(4) 115(2) 2_556
N20 H22B N35 0.93(3) 2.20(3) 3.112(4) 168(3) 2_656
N5 H5B N15 0.80(3) 2.39(3) 3.127(4) 154(3) 2_675
N35 H35A O3 0.85(4) 2.42(4) 2.967(3) 123(3) 1_655
N35 H35A N1 0.85(4) 2.64(4) 3.403(3) 149(3) 2_665
N35 H35B O8 0.91(4) 2.22(4) 2.949(4) 137(3) .
N35 H35B N36 0.91(4) 2.46(4) 3.045(4) 123(3) 1_655
N30 H30A O1 0.81(4) 2.44(4) 3.148(4) 148(3) .
N30 H30A O4 0.81(4) 2.56(4) 3.312(4) 156(3) .
N5 H5A N31 0.91(3) 2.28(3) 3.159(4) 161(3) 2_665
N15 H15B N39 0.88(3) 2.22(3) 3.074(4) 164(3) 1_565
N10 H10B O5 0.81(3) 2.30(3) 3.099(4) 169(3) .
N40 H40B N10 0.89(4) 2.44(4) 3.196(4) 143(3) .
N40 H40B N25 0.89(4) 2.64(4) 3.288(4) 131(3) 2_566
N15 H15A O8 0.85(4) 2.57(3) 3.286(4) 143(3) 2_675
N15 H15A O5 0.85(4) 2.61(3) 3.204(4) 128(3) 2_675
N10 H10A O2 0.87(3) 2.38(3) 3.097(4) 140(3) 1_565
N10 H10A N16 0.87(3) 2.62(3) 3.242(3) 129(3) 1_565
N40 H40A N20 0.85(4) 2.42(4) 3.198(4) 153(3) 2_556
N40 H40A O3 0.85(4) 2.63(4) 3.187(4) 125(3) .

_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         0.360
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.080

_shelxl_version_number           2013-4


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

data_lx588
_database_code_depnum_ccdc_archive 'CCDC 1834843'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Dec 05 16:19:34 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(2-aminotetrazolyl) dinitrato copper(II)
;
_chemical_name_common            'bis(2-aminotetrazolyl) dinitrato copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 Cu N12 O6'
_chemical_formula_sum            'C2 H6 Cu N12 O6'
_chemical_formula_weight         357.73

_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                   7.9953(8)
_cell_length_b                   8.9746(8)
_cell_length_c                   8.0033(9)
_cell_angle_alpha                90
_cell_angle_beta                 107.469(12)
_cell_angle_gamma                90
_cell_volume                     547.79(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2019
_cell_measurement_theta_min      4.8470
_cell_measurement_theta_max      31.8900

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.058
_shelx_estimated_absorpt_T_min   0.465
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_F_000             358
_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            4198
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.307
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             1121
_reflns_number_gt                1024
_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)+(0.0397P)²+0.0655P] 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         1121
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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      -0.0518532000
_diffrn_orient_matrix_UB_12      0.0463623000
_diffrn_orient_matrix_UB_13      0.0366380000
_diffrn_orient_matrix_UB_21      -0.0205862000
_diffrn_orient_matrix_UB_22      -0.0622835000
_diffrn_orient_matrix_UB_23      0.0447426000
_diffrn_orient_matrix_UB_31      0.0743655000
_diffrn_orient_matrix_UB_32      0.0150844000
_diffrn_orient_matrix_UB_33      0.0726235000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 47

#__ type_ start__ end____ width___ exp.time_
  2 omega   25.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -132.0000    2.0000 69

#__ type_ start__ end____ width___ exp.time_
  3 omega  -42.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000 -180.0000 131

#__ type_ start__ end____ width___ exp.time_
  4 omega   60.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   -3.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
  6 omega -106.00  -61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega -109.00  -64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   90.0000 45

;



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 0.0000 0.0000 0.0000 0.01129(13) Uani 1 2 d S . P . .
O1 O 0.14733(16) 0.18661(13) 0.01126(16) 0.0154(3) Uani 1 1 d . . . . .
O2 O 0.06882(18) 0.22540(14) -0.27114(17) 0.0191(3) Uani 1 1 d . . . . .
O3 O 0.21781(16) 0.39225(14) -0.09258(17) 0.0179(3) Uani 1 1 d . . . . .
N1 N 0.5027(2) -0.17382(16) 0.1789(2) 0.0154(3) Uani 1 1 d . . . . .
N2 N 0.39591(19) -0.29010(16) 0.14808(18) 0.0112(3) Uani 1 1 d . . . . .
N3 N 0.22921(19) -0.26203(17) 0.09068(19) 0.0136(3) Uani 1 1 d . . . . .
N4 N 0.22289(19) -0.11331(16) 0.07874(19) 0.0127(3) Uani 1 1 d . . . . .
N6 N 0.14376(19) 0.26833(16) -0.12150(18) 0.0125(3) Uani 1 1 d . . . . .
C1 C 0.3885(2) -0.0630(2) 0.1328(2) 0.0154(4) Uani 1 1 d . . . . .
N5 N 0.4588(2) -0.43402(17) 0.1970(2) 0.0132(3) Uani 1 1 d . . . . .
H1 H 0.417(3) 0.038(2) 0.140(3) 0.012(5) Uiso 1 1 d . . . . .
H5A H 0.394(3) -0.497(2) 0.132(3) 0.013(6) Uiso 1 1 d . . . . .
H5B H 0.558(3) -0.444(3) 0.177(3) 0.024(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
Cu1 N4 1.9831(14) 3 ?
Cu1 N4 1.9831(14) . ?
Cu1 O1 2.0339(12) . ?
Cu1 O1 2.0339(12) 3 ?
Cu1 N5 2.4206(16) 4 ?
Cu1 N5 2.4206(16) 2 ?
O1 N6 1.2843(18) . ?
O2 N6 1.2292(19) . ?
O3 N6 1.2485(19) . ?
N1 N2 1.324(2) . ?
N1 C1 1.326(2) . ?
N2 N3 1.297(2) . ?
N2 N5 1.399(2) . ?
N3 N4 1.338(2) . ?
N4 C1 1.342(2) . ?
C1 H1 0.93(2) . ?
N5 Cu1 2.4206(16) 2_545 ?
N5 H5A 0.83(2) . ?
N5 H5B 0.86(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
N4 Cu1 N4 180.0 3 . ?
N4 Cu1 O1 92.58(5) 3 . ?
N4 Cu1 O1 87.42(5) . . ?
N4 Cu1 O1 87.42(5) 3 3 ?
N4 Cu1 O1 92.58(5) . 3 ?
O1 Cu1 O1 180.0 . 3 ?
N4 Cu1 N5 88.16(6) 3 4 ?
N4 Cu1 N5 91.84(6) . 4 ?
O1 Cu1 N5 98.56(5) . 4 ?
O1 Cu1 N5 81.44(5) 3 4 ?
N4 Cu1 N5 91.84(6) 3 2 ?
N4 Cu1 N5 88.16(6) . 2 ?
O1 Cu1 N5 81.44(5) . 2 ?
O1 Cu1 N5 98.56(5) 3 2 ?
N5 Cu1 N5 180.00(8) 4 2 ?
N6 O1 Cu1 124.39(10) . . ?
N2 N1 C1 100.81(14) . . ?
N3 N2 N1 116.72(14) . . ?
N3 N2 N5 121.54(15) . . ?
N1 N2 N5 121.22(14) . . ?
N2 N3 N4 103.40(13) . . ?
N3 N4 C1 107.49(14) . . ?
N3 N4 Cu1 123.04(11) . . ?
C1 N4 Cu1 129.44(12) . . ?
O2 N6 O3 121.68(14) . . ?
O2 N6 O1 120.69(14) . . ?
O3 N6 O1 117.63(14) . . ?
N1 C1 N4 111.57(16) . . ?
N1 C1 H1 125.1(13) . . ?
N4 C1 H1 123.3(13) . . ?
N2 N5 Cu1 115.85(11) . 2_545 ?
N2 N5 H5A 110.3(15) . . ?
Cu1 N5 H5A 109.3(17) 2_545 . ?
N2 N5 H5B 108.7(17) . . ?
Cu1 N5 H5B 107.8(15) 2_545 . ?
H5A N5 H5B 104(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 -0.9(2) . . . . ?
C1 N1 N2 N5 -172.72(16) . . . . ?
N1 N2 N3 N4 1.1(2) . . . . ?
N5 N2 N3 N4 172.89(15) . . . . ?
N2 N3 N4 C1 -0.79(19) . . . . ?
N2 N3 N4 Cu1 -179.17(11) . . . . ?
Cu1 O1 N6 O2 -11.3(2) . . . . ?
Cu1 O1 N6 O3 168.29(11) . . . . ?
N2 N1 C1 N4 0.3(2) . . . . ?
N3 N4 C1 N1 0.3(2) . . . . ?
Cu1 N4 C1 N1 178.53(12) . . . . ?
N3 N2 N5 Cu1 -89.31(17) . . . 2_545 ?
N1 N2 N5 Cu1 82.09(18) . . . 2_545 ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5A O3 0.83(2) 2.17(3) 2.972(2) 163(2) 1_545
N5 H5B O3 0.86(3) 2.15(3) 2.971(2) 160(2) 3_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         0.303
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.070

_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_lx543
_database_code_depnum_ccdc_archive 'CCDC 1834844'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Nov 11 16:42:26 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
 tris(1-aminotetrazolyl) dinitrato copper(II)
;
_chemical_name_common            ' tris(1-aminotetrazolyl) dinitrato copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C3 H9 Cu N17 O6'
_chemical_formula_sum            'C3 H9 Cu N17 O6'
_chemical_formula_weight         442.81

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_symmetry_Int_Tables_number      9
_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'

_cell_length_a                   15.301(5)
_cell_length_b                   6.684(5)
_cell_length_c                   15.203(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.027(5)
_cell_angle_gamma                90
_cell_volume                     1494.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1960
_cell_measurement_theta_min      5.0120
_cell_measurement_theta_max      27.8580

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.539
_shelx_estimated_absorpt_T_min   0.623
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97478
_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    1.968
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(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            6665
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.106
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2808
_reflns_number_gt                2567
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.995

_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)+(0.0158P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

_refine_ls_abs_structure_Flack   0.036(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2808
_refine_ls_number_parameters     269
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0545
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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      0.0216472000
_diffrn_orient_matrix_UB_12      -0.0714496000
_diffrn_orient_matrix_UB_13      0.0334278000
_diffrn_orient_matrix_UB_21      0.0316133000
_diffrn_orient_matrix_UB_22      -0.0210943000
_diffrn_orient_matrix_UB_23      -0.0251912000
_diffrn_orient_matrix_UB_31      0.0293005000
_diffrn_orient_matrix_UB_32      0.0755896000
_diffrn_orient_matrix_UB_33      0.0245790000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.00  -32.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -180.0000 47

#__ type_ start__ end____ width___ exp.time_
  2 omega -111.00  -33.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
  3 omega   57.00  100.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  120.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega   28.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 40

#__ type_ start__ end____ width___ exp.time_
  5 omega  -22.00   28.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 50

#__ type_ start__ end____ width___ exp.time_
  6 omega   -2.00  100.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000   90.0000 102

#__ type_ start__ end____ width___ exp.time_
  7 omega  -38.00   15.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega   43.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 32

#__ type_ start__ end____ width___ exp.time_
  9 omega   80.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000   90.0000 28

;



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
Cu Cu 0.85537(3) 0.06452(6) 0.58343(3) 0.01607(12) Uani 1 1 d . . . . .
O1 O 0.7811(2) 0.2526(4) 0.6341(2) 0.0185(7) Uani 1 1 d . . . . .
O2 O 0.7814(2) 0.4002(4) 0.5064(2) 0.0278(8) Uani 1 1 d . . . . .
O3 O 0.6992(3) 0.5204(5) 0.5905(2) 0.0317(9) Uani 1 1 d . . . . .
O4 O 0.9343(2) -0.1359(4) 0.5459(2) 0.0202(7) Uani 1 1 d . . . . .
O5 O 1.0207(2) -0.1721(5) 0.4561(3) 0.0326(8) Uani 1 1 d . . . . .
O6 O 0.9304(3) 0.0839(5) 0.4394(2) 0.0325(8) Uani 1 1 d . . . . .
N1 N 0.6530(3) -0.2475(5) 0.4036(2) 0.0158(8) Uani 1 1 d . . . . .
N2 N 0.6021(3) -0.1274(5) 0.4410(3) 0.0223(9) Uani 1 1 d . . . . .
N3 N 0.6588(3) -0.0134(5) 0.4983(3) 0.0250(9) Uani 1 1 d . . . . .
N4 N 0.7452(3) -0.0582(5) 0.4972(2) 0.0164(7) Uani 1 1 d . . . . .
N5 N 0.6185(3) -0.4047(6) 0.3433(3) 0.0212(8) Uani 1 1 d . . . . .
N6 N 1.0578(3) 0.4789(5) 0.6705(2) 0.0162(8) Uani 1 1 d . . . . .
N7 N 1.0702(3) 0.3689(5) 0.7465(3) 0.0238(9) Uani 1 1 d . . . . .
N8 N 1.0131(3) 0.2214(5) 0.7262(3) 0.0236(9) Uani 1 1 d . . . . .
N9 N 0.9629(3) 0.2391(5) 0.6374(2) 0.0181(8) Uani 1 1 d . . . . .
N10 N 1.1065(3) 0.6567(6) 0.6744(3) 0.0215(9) Uani 1 1 d . . . . .
N11 N 0.8535(3) -0.3842(5) 0.7883(2) 0.0174(8) Uani 1 1 d . . . . .
N12 N 0.8946(3) -0.2972(5) 0.7305(3) 0.0219(9) Uani 1 1 d . . . . .
N13 N 0.8476(3) -0.1370(5) 0.7026(2) 0.0193(8) Uani 1 1 d . . . . .
N14 N 0.7766(3) -0.1193(5) 0.7405(3) 0.0234(9) Uani 1 1 d . . . . .
N15 N 0.8845(4) -0.5625(6) 0.8352(3) 0.0303(10) Uani 1 1 d . . . . .
N16 N 0.7524(3) 0.3979(6) 0.5745(3) 0.0210(10) Uani 1 1 d . . . . .
N17 N 0.9627(3) -0.0719(5) 0.4779(3) 0.0193(8) Uani 1 1 d . . . . .
C1 C 0.7390(3) -0.2044(5) 0.4378(3) 0.0167(9) Uani 1 1 d . . . . .
H1 H 0.7885 -0.2676 0.4225 0.020 Uiso 1 1 calc R U . . .
C2 C 0.9925(3) 0.4002(7) 0.6037(3) 0.0179(10) Uani 1 1 d . . . . .
H2 H 0.9709 0.4498 0.5430 0.022 Uiso 1 1 calc R U . . .
C3 C 0.7820(3) -0.2753(6) 0.7931(3) 0.0203(10) Uani 1 1 d . . . . .
H3 H 0.7418 -0.3062 0.8289 0.024 Uiso 1 1 calc R U . . .
H5A H 0.595(3) -0.349(6) 0.290(4) 0.011(11) Uiso 1 1 d . . . . .
H10A H 1.157(4) 0.618(6) 0.681(3) 0.015(14) Uiso 1 1 d . . . . .
H5B H 0.591(4) -0.480(8) 0.366(4) 0.036(16) Uiso 1 1 d . . . . .
H10B H 1.084(4) 0.735(8) 0.628(4) 0.034(15) Uiso 1 1 d . . . . .
H15B H 0.949(5) -0.544(8) 0.866(4) 0.05(2) Uiso 1 1 d . . . . .
H15A H 0.876(4) -0.651(9) 0.795(4) 0.05(2) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu O1 1.987(3) . ?
Cu O4 1.989(3) . ?
Cu N9 1.999(4) . ?
Cu N4 2.003(4) . ?
Cu N13 2.287(4) . ?
O1 N16 1.318(5) . ?
O2 N16 1.234(5) . ?
O3 N16 1.225(5) . ?
O4 N17 1.300(4) . ?
O5 N17 1.229(4) . ?
O6 N17 1.229(5) . ?
N1 C1 1.307(6) . ?
N1 N2 1.349(5) . ?
N1 N5 1.399(5) . ?
N2 N3 1.295(5) . ?
N3 N4 1.361(5) . ?
N4 C1 1.316(5) . ?
N5 H5A 0.87(5) . ?
N5 H5B 0.80(6) . ?
N6 C2 1.322(6) . ?
N6 N7 1.338(5) . ?
N6 N10 1.395(5) . ?
N7 N8 1.296(5) . ?
N8 N9 1.361(5) . ?
N9 C2 1.325(6) . ?
N10 H10A 0.79(5) . ?
N10 H10B 0.87(6) . ?
N11 C3 1.333(5) . ?
N11 N12 1.345(5) . ?
N11 N15 1.402(5) . ?
N12 N13 1.294(5) . ?
N13 N14 1.370(5) . ?
N14 C3 1.302(5) . ?
N15 H15B 0.98(7) . ?
N15 H15A 0.83(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 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
O1 Cu O4 173.95(13) . . ?
O1 Cu N9 88.03(14) . . ?
O4 Cu N9 90.84(14) . . ?
O1 Cu N4 92.60(13) . . ?
O4 Cu N4 90.22(14) . . ?
N9 Cu N4 162.95(14) . . ?
O1 Cu N13 84.57(12) . . ?
O4 Cu N13 89.92(13) . . ?
N9 Cu N13 103.63(14) . . ?
N4 Cu N13 93.39(14) . . ?
N16 O1 Cu 108.5(3) . . ?
N17 O4 Cu 111.7(2) . . ?
C1 N1 N2 109.7(3) . . ?
C1 N1 N5 125.7(4) . . ?
N2 N1 N5 124.5(4) . . ?
N3 N2 N1 106.0(4) . . ?
N2 N3 N4 109.6(3) . . ?
C1 N4 N3 106.6(4) . . ?
C1 N4 Cu 129.9(3) . . ?
N3 N4 Cu 123.1(3) . . ?
N1 N5 H5A 106(3) . . ?
N1 N5 H5B 110(4) . . ?
H5A N5 H5B 122(5) . . ?
C2 N6 N7 110.0(3) . . ?
C2 N6 N10 130.7(4) . . ?
N7 N6 N10 119.0(4) . . ?
N8 N7 N6 106.7(4) . . ?
N7 N8 N9 109.2(3) . . ?
C2 N9 N8 107.1(4) . . ?
C2 N9 Cu 130.2(3) . . ?
N8 N9 Cu 122.1(3) . . ?
N6 N10 H10A 103(3) . . ?
N6 N10 H10B 113(4) . . ?
H10A N10 H10B 117(5) . . ?
C3 N11 N12 109.8(3) . . ?
C3 N11 N15 127.2(4) . . ?
N12 N11 N15 123.1(4) . . ?
N13 N12 N11 104.8(3) . . ?
N12 N13 N14 111.5(3) . . ?
N12 N13 Cu 127.0(3) . . ?
N14 N13 Cu 120.2(3) . . ?
C3 N14 N13 105.4(4) . . ?
N11 N15 H15B 107(3) . . ?
N11 N15 H15A 106(4) . . ?
H15B N15 H15A 112(6) . . ?
O3 N16 O2 124.8(4) . . ?
O3 N16 O1 118.0(4) . . ?
O2 N16 O1 117.2(4) . . ?
O5 N17 O6 124.0(4) . . ?
O5 N17 O4 117.4(4) . . ?
O6 N17 O4 118.6(3) . . ?
N1 C1 N4 108.1(4) . . ?
N1 C1 H1 125.9 . . ?
N4 C1 H1 125.9 . . ?
N6 C2 N9 107.0(4) . . ?
N6 C2 H2 126.5 . . ?
N9 C2 H2 126.5 . . ?
N14 C3 N11 108.6(4) . . ?
N14 C3 H3 125.7 . . ?
N11 C3 H3 125.7 . . ?

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 -0.4(5) . . . . ?
N5 N1 N2 N3 174.6(4) . . . . ?
N1 N2 N3 N4 0.6(4) . . . . ?
N2 N3 N4 C1 -0.5(5) . . . . ?
N2 N3 N4 Cu -174.3(3) . . . . ?
C2 N6 N7 N8 0.7(5) . . . . ?
N10 N6 N7 N8 175.6(4) . . . . ?
N6 N7 N8 N9 -1.2(5) . . . . ?
N7 N8 N9 C2 1.2(5) . . . . ?
N7 N8 N9 Cu -171.2(3) . . . . ?
C3 N11 N12 N13 0.6(5) . . . . ?
N15 N11 N12 N13 -178.9(4) . . . . ?
N11 N12 N13 N14 -0.5(5) . . . . ?
N11 N12 N13 Cu -167.6(3) . . . . ?
N12 N13 N14 C3 0.1(5) . . . . ?
Cu N13 N14 C3 168.3(3) . . . . ?
Cu O1 N16 O3 174.2(3) . . . . ?
Cu O1 N16 O2 -5.9(4) . . . . ?
Cu O4 N17 O5 171.3(3) . . . . ?
Cu O4 N17 O6 -8.7(5) . . . . ?
N2 N1 C1 N4 0.1(5) . . . . ?
N5 N1 C1 N4 -174.8(4) . . . . ?
N3 N4 C1 N1 0.2(4) . . . . ?
Cu N4 C1 N1 173.5(3) . . . . ?
N7 N6 C2 N9 0.1(5) . . . . ?
N10 N6 C2 N9 -174.0(4) . . . . ?
N8 N9 C2 N6 -0.8(5) . . . . ?
Cu N9 C2 N6 170.9(3) . . . . ?
N13 N14 C3 N11 0.3(5) . . . . ?
N12 N11 C3 N14 -0.6(5) . . . . ?
N15 N11 C3 N14 179.0(5) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 N15 0.95 2.51 3.426(6) 162.6 2_544
N5 H5A N10 0.87(5) 2.23(5) 3.019(6) 151(4) 4_454
N10 H10A O1 0.79(5) 2.38(5) 2.972(5) 132(4) 3
N10 H10A N14 0.79(5) 2.40(5) 3.122(6) 151(4) 3
N5 H5B O5 0.80(6) 2.34(6) 3.129(6) 171(5) 3_445
N10 H10B O4 0.87(6) 2.44(6) 3.137(6) 138(5) 1_565
N10 H10B O5 0.87(6) 2.60(6) 3.411(6) 155(4) 1_565
N15 H15B O5 0.98(7) 2.42(6) 2.959(6) 114(4) 2_545
N15 H15B N2 0.98(7) 2.57(7) 3.510(7) 161(4) 4_545
N15 H15A O1 0.83(6) 2.56(7) 3.272(7) 144(5) 1_545
C1 H1 N15 0.95 2.51 3.426(6) 162.6 2_544
N5 H5A N10 0.87(5) 2.23(5) 3.019(6) 151(4) 4_454
N10 H10A O1 0.79(5) 2.38(5) 2.972(5) 132(4) 3
N10 H10A N14 0.79(5) 2.40(5) 3.122(6) 151(4) 3
N5 H5B O5 0.80(6) 2.34(6) 3.129(6) 171(5) 3_445
N10 H10B O4 0.87(6) 2.44(6) 3.137(6) 138(5) 1_565
N10 H10B O5 0.87(6) 2.60(6) 3.411(6) 155(4) 1_565
N15 H15B O5 0.98(7) 2.42(6) 2.959(6) 114(4) 2_545
N15 H15B N2 0.98(7) 2.57(7) 3.510(7) 161(4) 4_545
N15 H15A O1 0.83(6) 2.56(7) 3.272(7) 144(5) 1_545

_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         0.413
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.070

_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_lx529
_database_code_depnum_ccdc_archive 'CCDC 1834845'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Nov 04 15:42:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis-chlorido bis(1-aminotetrazolyl) copper(II)
;
_chemical_name_common            'bischlorido bis(1-aminotetrazolyl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 Cl2 Cu N10'
_chemical_formula_sum            'C2 H6 Cl2 Cu N10'
_chemical_formula_weight         304.61

_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                   7.4976(2)
_cell_length_b                   12.2023(5)
_cell_length_c                   10.3115(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.719(4)
_cell_angle_gamma                90
_cell_volume                     942.95(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3025
_cell_measurement_theta_min      4.6820
_cell_measurement_theta_max      31.8480

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.867
_shelx_estimated_absorpt_T_min   0.598
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_F_000             604
_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            6823
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.293
_diffrn_reflns_theta_max         25.991
_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             1846
_reflns_number_gt                1625
_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)+(0.0226P)²+0.4773P] 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         1846
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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      -0.0427507000
_diffrn_orient_matrix_UB_12      -0.0173413000
_diffrn_orient_matrix_UB_13      -0.0587857000
_diffrn_orient_matrix_UB_21      0.0171536000
_diffrn_orient_matrix_UB_22      0.0518803000
_diffrn_orient_matrix_UB_23      -0.0280246000
_diffrn_orient_matrix_UB_31      0.0827177000
_diffrn_orient_matrix_UB_32      -0.0196804000
_diffrn_orient_matrix_UB_33      -0.0221549000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -45.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000   90.0000 150

#__ type_ start__ end____ width___ exp.time_
  2 omega   50.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega    8.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 62

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   90.0000 85

#__ type_ start__ end____ width___ exp.time_
  5 omega   60.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -90.0000 37

#__ type_ start__ end____ width___ exp.time_
  6 omega   44.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -90.0000 43

#__ type_ start__ end____ width___ exp.time_
  7 omega -109.00  -60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -120.0000 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'
H H 0.0000 0.0000 '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'


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 0.38321(3) 0.07794(2) 0.13034(3) 0.01614(10) Uani 1 1 d . . . . .
Cl1 Cl 0.11792(7) 0.05452(5) 0.23028(6) 0.02039(14) Uani 1 1 d . . . . .
Cl2 Cl 0.64924(7) 0.10818(4) 0.02835(5) 0.01577(13) Uani 1 1 d . . . . .
N5 N 0.4034(3) 0.26783(19) 0.2691(2) 0.0199(4) Uani 1 1 d . . . . .
N1 N 0.5570(2) 0.28696(15) 0.34742(18) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.7079(3) 0.23120(17) 0.3236(2) 0.0242(5) Uani 1 1 d . . . . .
N3 N 0.8251(3) 0.26266(16) 0.4102(2) 0.0247(5) Uani 1 1 d . . . . .
N9 N 0.5108(2) -0.01032(15) 0.26928(19) 0.0179(4) Uani 1 1 d . . . . .
N8 N 0.4294(3) -0.08208(17) 0.3515(2) 0.0287(5) Uani 1 1 d . . . . .
N7 N 0.5475(3) -0.12709(17) 0.4278(2) 0.0270(5) Uani 1 1 d . . . . .
N6 N 0.7067(2) -0.08516(15) 0.39541(19) 0.0166(4) Uani 1 1 d . . . . .
N10 N 0.8713(3) -0.1156(2) 0.4544(2) 0.0239(5) Uani 1 1 d . . . . .
C1 C 0.5847(3) 0.35026(19) 0.4502(2) 0.0164(5) Uani 1 1 d . . . . .
C2 C 0.6825(3) -0.01493(18) 0.2987(2) 0.0154(5) Uani 1 1 d . . . . .
N4 N 0.7510(2) 0.33732(15) 0.49088(19) 0.0164(4) Uani 1 1 d . . . . .
H1 H 0.508(3) 0.392(2) 0.483(3) 0.023(7) Uiso 1 1 d . . . . .
H2 H 0.763(4) 0.026(2) 0.261(3) 0.025(7) Uiso 1 1 d . . . . .
H10A H 0.866(4) -0.190(2) 0.459(3) 0.035(8) Uiso 1 1 d . . . . .
H10B H 0.882(4) -0.089(3) 0.532(4) 0.049(10) Uiso 1 1 d . . . . .
H5A H 0.318(4) 0.256(3) 0.319(3) 0.048(10) Uiso 1 1 d . . . . .
H5B H 0.380(4) 0.325(2) 0.226(3) 0.032(9) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.0086(19) 4_565 ?
Cu1 N9 2.011(2) . ?
Cu1 Cl1 2.2854(6) . ?
Cu1 Cl2 2.3122(5) . ?
N5 N1 1.407(3) . ?
N5 H5A 0.85(3) . ?
N5 H5B 0.84(3) . ?
N1 C1 1.323(3) . ?
N1 N2 1.349(3) . ?
N2 N3 1.292(3) . ?
N3 N4 1.363(3) . ?
N9 C2 1.315(3) . ?
N9 N8 1.375(3) . ?
N8 N7 1.289(3) . ?
N7 N6 1.350(3) . ?
N6 C2 1.323(3) . ?
N6 N10 1.409(3) . ?
N10 H10A 0.92(3) . ?
N10 H10B 0.86(4) . ?
C1 N4 1.313(3) . ?
C1 H1 0.85(3) . ?
C2 H2 0.88(3) . ?
N4 Cu1 2.0086(19) 4_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N9 178.42(7) 4_565 . ?
N4 Cu1 Cl1 88.26(5) 4_565 . ?
N9 Cu1 Cl1 90.79(5) . . ?
N4 Cu1 Cl2 90.35(5) 4_565 . ?
N9 Cu1 Cl2 90.63(5) . . ?
Cl1 Cu1 Cl2 177.96(2) . . ?
N1 N5 H5A 108(2) . . ?
N1 N5 H5B 109(2) . . ?
H5A N5 H5B 108(3) . . ?
C1 N1 N2 109.15(19) . . ?
C1 N1 N5 131.56(19) . . ?
N2 N1 N5 119.24(18) . . ?
N3 N2 N1 106.33(18) . . ?
N2 N3 N4 109.81(18) . . ?
C2 N9 N8 106.25(19) . . ?
C2 N9 Cu1 128.97(16) . . ?
N8 N9 Cu1 124.75(15) . . ?
N7 N8 N9 109.79(19) . . ?
N8 N7 N6 106.46(18) . . ?
C2 N6 N7 109.26(19) . . ?
C2 N6 N10 126.45(19) . . ?
N7 N6 N10 124.27(18) . . ?
N6 N10 H10A 104.5(18) . . ?
N6 N10 H10B 111(2) . . ?
H10A N10 H10B 109(3) . . ?
N4 C1 N1 108.1(2) . . ?
N4 C1 H1 126.3(18) . . ?
N1 C1 H1 125.6(18) . . ?
N9 C2 N6 108.2(2) . . ?
N9 C2 H2 123.5(17) . . ?
N6 C2 H2 128.2(18) . . ?
C1 N4 N3 106.59(19) . . ?
C1 N4 Cu1 127.63(16) . 4_666 ?
N3 N4 Cu1 125.42(14) . 4_666 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -1.1(3) . . . . ?
N5 N1 N2 N3 -178.8(2) . . . . ?
N1 N2 N3 N4 0.7(3) . . . . ?
C2 N9 N8 N7 0.5(3) . . . . ?
Cu1 N9 N8 N7 178.94(17) . . . . ?
N9 N8 N7 N6 -0.2(3) . . . . ?
N8 N7 N6 C2 -0.2(3) . . . . ?
N8 N7 N6 N10 -178.4(2) . . . . ?
N2 N1 C1 N4 1.0(3) . . . . ?
N5 N1 C1 N4 178.4(2) . . . . ?
N8 N9 C2 N6 -0.6(3) . . . . ?
Cu1 N9 C2 N6 -178.95(15) . . . . ?
N7 N6 C2 N9 0.5(3) . . . . ?
N10 N6 C2 N9 178.7(2) . . . . ?
N1 C1 N4 N3 -0.6(3) . . . . ?
N1 C1 N4 Cu1 172.77(14) . . . 4_666 ?
N2 N3 N4 C1 -0.1(3) . . . . ?
N2 N3 N4 Cu1 -173.64(16) . . . 4_666 ?

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 Cl2 0.85(3) 2.74(3) 3.424(2) 138(2) 4_566
C2 H2 Cl1 0.88(3) 2.71(3) 3.466(2) 144(2) 1_655
C2 H2 Cl2 0.88(3) 2.72(3) 3.170(2) 114(2) .
N10 H10A Cl2 0.92(3) 2.46(3) 3.380(2) 179(3) 2_645
N10 H10B Cl1 0.86(4) 2.49(4) 3.334(3) 167(3) 3_656
N5 H5B Cl1 0.84(3) 2.84(3) 3.502(2) 137(3) 2
N5 H5B N8 0.84(3) 2.69(3) 3.308(3) 132(2) 2
C1 H1 Cl2 0.85(3) 2.74(3) 3.424(2) 138(2) 4_566
C2 H2 Cl1 0.88(3) 2.71(3) 3.466(2) 144(2) 1_655
C2 H2 Cl2 0.88(3) 2.72(3) 3.170(2) 114(2) .
N10 H10A Cl2 0.92(3) 2.46(3) 3.380(2) 179(3) 2_645
N10 H10B Cl1 0.86(4) 2.49(4) 3.334(3) 167(3) 3_656
N5 H5B Cl1 0.84(3) 2.84(3) 3.502(2) 137(3) 2
N5 H5B N8 0.84(3) 2.69(3) 3.308(3) 132(2) 2

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



_refine_diff_density_max         0.342
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.068

_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_lx622
_database_code_depnum_ccdc_archive 'CCDC 1834846'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sat Dec 24 21:14:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
aqua penta(2-aminotetrazolyl)zinc(II) perchlorate
;
_chemical_name_common            
'aqua penta(2-aminotetrazolyl)zinc(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H17 N25 O Zn, 2(Cl O4)'
_chemical_formula_sum            'C5 H17 Cl2 N25 O9 Zn'
_chemical_formula_weight         707.71

_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                   9.4977(6)
_cell_length_b                   9.9017(5)
_cell_length_c                   15.3665(8)
_cell_angle_alpha                75.918(5)
_cell_angle_beta                 89.336(5)
_cell_angle_gamma                63.584(6)
_cell_volume                     1247.54(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3922
_cell_measurement_theta_min      4.4820
_cell_measurement_theta_max      31.8670

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.293
_shelx_estimated_absorpt_T_min   0.460
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81997
_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    1.884
_exptl_crystal_F_000             716
_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            9906
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.251
_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             4875
_reflns_number_gt                4264
_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)+(0.0757P)²+2.4644P] 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         4875
_refine_ls_number_parameters     475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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      -0.0510784000
_diffrn_orient_matrix_UB_12      -0.0230889000
_diffrn_orient_matrix_UB_13      0.0265808000
_diffrn_orient_matrix_UB_21      0.0452580000
_diffrn_orient_matrix_UB_22      -0.0110335000
_diffrn_orient_matrix_UB_23      0.0398316000
_diffrn_orient_matrix_UB_31      -0.0488211000
_diffrn_orient_matrix_UB_32      0.0789292000
_diffrn_orient_matrix_UB_33      -0.0000437000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -54.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   38.0000  -30.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega    7.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   77.0000  -30.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega   14.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   57.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega   11.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   57.0000 -150.0000 89

#__ type_ start__ end____ width___ exp.time_
  5 omega   40.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  -99.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  -21.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  -99.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
  7 omega   53.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   57.0000  120.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega  -60.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557   77.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  9 omega -107.00  -54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557 -179.0000  -90.0000 53

;



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
Zn01 Zn -0.03111(4) 0.78796(4) 0.26868(2) 0.01424(14) Uani 1 1 d . . . . .
O1 O -0.2473(3) 0.7817(3) 0.2766(2) 0.0254(6) Uani 1 1 d . . . . .
N1 N -0.0069(4) 0.7050(4) 0.5591(2) 0.0265(7) Uani 1 1 d . . . . .
N2 N 0.1308(3) 0.6043(3) 0.54028(18) 0.0156(6) Uani 1 1 d . . . . .
N3 N 0.1419(3) 0.6070(3) 0.45585(19) 0.0209(6) Uani 1 1 d . . . . .
N4 N 0.0017(3) 0.7181(3) 0.41350(19) 0.0188(6) Uani 1 1 d . . . . .
N5 N 0.2518(4) 0.4950(4) 0.6076(2) 0.0192(6) Uani 1 1 d . . . . .
N9 N 0.0697(3) 0.5420(3) 0.26572(19) 0.0186(6) Uani 1 1 d . . . . .
N8 N 0.2052(3) 0.4254(3) 0.30859(19) 0.0180(6) Uani 1 1 d . . . . .
N6 N 0.0948(3) 0.3311(3) 0.2281(2) 0.0217(6) Uani 1 1 d . . . . .
N7 N 0.2150(3) 0.3042(3) 0.28433(19) 0.0165(6) Uani 1 1 d . . . . .
N10 N 0.3430(4) 0.1561(4) 0.3124(2) 0.0248(7) Uani 1 1 d . . . . .
N14 N -0.0661(3) 0.8511(3) 0.12387(19) 0.0198(6) Uani 1 1 d . . . . .
N13 N 0.0375(4) 0.7580(4) 0.0780(2) 0.0251(7) Uani 1 1 d . . . . .
N11 N -0.1598(4) 0.9515(4) -0.0202(2) 0.0374(9) Uani 1 1 d . . . . .
N12 N -0.0254(4) 0.8233(4) -0.0059(2) 0.0230(6) Uani 1 1 d . . . . .
N15 N 0.0508(5) 0.7666(5) -0.0765(2) 0.0339(8) Uani 1 1 d . . . . .
N19 N -0.1485(3) 1.0316(3) 0.26987(19) 0.0172(6) Uani 1 1 d . . . . .
N18 N -0.2913(3) 1.1238(3) 0.22278(19) 0.0188(6) Uani 1 1 d . . . . .
N16 N -0.2152(4) 1.2723(4) 0.2770(2) 0.0227(6) Uani 1 1 d . . . . .
N17 N -0.3244(3) 1.2638(3) 0.22883(19) 0.0181(6) Uani 1 1 d . . . . .
N20 N -0.4688(4) 1.3926(4) 0.1935(2) 0.0270(7) Uani 1 1 d . . . . .
N21 N 0.1979(3) 0.7846(3) 0.26758(19) 0.0166(6) Uani 1 1 d . . . . .
N22 N 0.2148(3) 0.9076(3) 0.22322(19) 0.0173(6) Uani 1 1 d . . . . .
N23 N 0.4549(3) 0.7089(3) 0.2697(2) 0.0218(6) Uani 1 1 d . . . . .
N24 N 0.3686(3) 0.8582(3) 0.22556(19) 0.0159(6) Uani 1 1 d . . . . .
N25 N 0.4400(3) 0.9496(4) 0.1848(2) 0.0208(6) Uani 1 1 d . . . . .
C1 C -0.0851(4) 0.7755(4) 0.4764(2) 0.0237(8) Uani 1 1 d . . . . .
C2 C 0.0052(4) 0.4816(4) 0.2188(2) 0.0217(7) Uani 1 1 d . . . . .
C4 C -0.1068(4) 1.1247(4) 0.3014(3) 0.0212(7) Uani 1 1 d . . . . .
C3 C -0.1825(5) 0.9647(5) 0.0636(3) 0.0310(9) Uani 1 1 d . . . . .
C5 C 0.3440(4) 0.6661(4) 0.2959(3) 0.0225(7) Uani 1 1 d . . . . .
Cl1 Cl 0.58732(9) 0.18746(9) 0.50422(5) 0.0196(2) Uani 1 1 d . . . . .
O2 O 0.6070(3) 0.1508(4) 0.41858(19) 0.0364(7) Uani 1 1 d . . . . .
O3 O 0.4621(4) 0.1583(4) 0.5434(2) 0.0397(7) Uani 1 1 d . . . . .
O4 O 0.5496(4) 0.3475(3) 0.4932(2) 0.0418(8) Uani 1 1 d . . . . .
O5 O 0.7328(3) 0.0874(4) 0.5628(2) 0.0384(7) Uani 1 1 d . . . . .
Cl2 Cl 0.62866(19) 0.68067(15) 0.00909(8) 0.0534(4) Uani 1 1 d . . . . .
O6 O 0.5833(13) 0.8360(10) 0.0191(6) 0.165(4) Uani 1 1 d . . . . .
O7A O 0.8183(13) 0.6185(14) 0.0185(9) 0.095(5) Uani 0.452(10) 1 d . . P A 1
O8A O 0.6732(13) 0.6716(16) -0.0770(8) 0.066(4) Uani 0.452(10) 1 d . . P A 1
O9A O 0.576(5) 0.692(3) 0.0862(16) 0.28(2) Uani 0.452(10) 1 d . . P A 1
O7B O 0.7125(9) 0.5618(10) 0.0789(6) 0.074(3) Uani 0.548(10) 1 d . . P A 2
O8B O 0.5928(17) 0.7521(16) -0.0773(7) 0.092(4) Uani 0.548(10) 1 d . . P A 2
O9B O 0.4649(9) 0.6817(10) 0.0075(6) 0.073(3) Uani 0.548(10) 1 d . . P A 2
H25B H 0.403(5) 1.031(6) 0.198(3) 0.025(11) Uiso 1 1 d . . . . .
H5A H 0.257(5) 0.546(5) 0.644(3) 0.023(11) Uiso 1 1 d . . . . .
H25A H 0.419(6) 0.973(6) 0.124(4) 0.043(14) Uiso 1 1 d . . . . .
H5 H 0.360(5) 0.574(5) 0.331(3) 0.022(10) Uiso 1 1 d . . . . .
H2 H -0.084(6) 0.538(5) 0.184(3) 0.034(12) Uiso 1 1 d . . . . .
H10A H 0.319(6) 0.098(6) 0.349(3) 0.034(13) Uiso 1 1 d . . . . .
H3 H -0.266(7) 1.042(6) 0.076(4) 0.052(15) Uiso 1 1 d . . . . .
H10B H 0.415(6) 0.160(6) 0.338(3) 0.035(13) Uiso 1 1 d . . . . .
H5B H 0.337(6) 0.463(6) 0.579(3) 0.036(13) Uiso 1 1 d . . . . .
H1 H -0.185(5) 0.848(5) 0.466(3) 0.027(11) Uiso 1 1 d . . . . .
H20A H -0.510(6) 1.362(6) 0.161(4) 0.041(15) Uiso 1 1 d . . . . .
H4 H -0.019(5) 1.094(5) 0.333(3) 0.024(11) Uiso 1 1 d . . . . .
H20B H -0.449(6) 1.454(7) 0.168(4) 0.041(16) Uiso 1 1 d . . . . .
H1A H -0.247(8) 0.701(9) 0.309(5) 0.08(2) Uiso 1 1 d . . . . .
H1B H -0.320(7) 0.837(7) 0.242(4) 0.051(16) Uiso 1 1 d . . . . .
H15B H 0.102(6) 0.675(6) -0.056(3) 0.035(14) Uiso 1 1 d . . . . .
H15A H -0.027(7) 0.779(6) -0.118(4) 0.054(16) 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
Zn01 O1 2.083(3) . ?
Zn01 N4 2.145(3) . ?
Zn01 N14 2.147(3) . ?
Zn01 N21 2.160(3) . ?
Zn01 N19 2.166(3) . ?
Zn01 N9 2.197(3) . ?
O1 H1A 0.83(8) . ?
O1 H1B 0.77(6) . ?
N1 N2 1.326(4) . ?
N1 C1 1.335(5) . ?
N2 N3 1.295(4) . ?
N2 N5 1.392(4) . ?
N3 N4 1.332(4) . ?
N4 C1 1.331(5) . ?
N5 H5A 0.85(5) . ?
N5 H5B 0.88(5) . ?
N9 N8 1.323(4) . ?
N9 C2 1.341(5) . ?
N8 N7 1.307(4) . ?
N6 C2 1.318(5) . ?
N6 N7 1.327(4) . ?
N7 N10 1.390(4) . ?
N10 H10A 0.81(5) . ?
N10 H10B 0.82(5) . ?
N14 C3 1.325(5) . ?
N14 N13 1.344(4) . ?
N13 N12 1.306(4) . ?
N11 N12 1.311(5) . ?
N11 C3 1.331(5) . ?
N12 N15 1.391(4) . ?
N15 H15B 0.79(5) . ?
N15 H15A 0.93(6) . ?
N19 C4 1.336(5) . ?
N19 N18 1.340(4) . ?
N18 N17 1.306(4) . ?
N16 C4 1.320(5) . ?
N16 N17 1.325(4) . ?
N17 N20 1.388(4) . ?
N20 H20A 0.82(6) . ?
N20 H20B 0.73(6) . ?
N21 N22 1.320(4) . ?
N21 C5 1.345(4) . ?
N22 N24 1.316(4) . ?
N23 C5 1.325(5) . ?
N23 N24 1.328(4) . ?
N24 N25 1.390(4) . ?
N25 H25B 0.80(5) . ?
N25 H25A 0.91(6) . ?
C1 H1 0.89(4) . ?
C2 H2 0.87(5) . ?
C4 H4 0.86(4) . ?
C3 H3 0.89(5) . ?
C5 H5 0.89(4) . ?
Cl1 O4 1.426(3) . ?
Cl1 O2 1.437(3) . ?
Cl1 O3 1.437(3) . ?
Cl1 O5 1.442(3) . ?
Cl2 O9A 1.292(15) . ?
Cl2 O8B 1.311(10) . ?
Cl2 O7B 1.320(7) . ?
Cl2 O8A 1.395(11) . ?
Cl2 O6 1.449(7) . ?
Cl2 O9B 1.551(8) . ?
Cl2 O7A 1.619(11) . ?
O6 O9A 1.57(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
O1 Zn01 N4 87.55(11) . . ?
O1 Zn01 N14 91.09(11) . . ?
N4 Zn01 N14 177.91(11) . . ?
O1 Zn01 N21 176.80(11) . . ?
N4 Zn01 N21 89.62(11) . . ?
N14 Zn01 N21 91.69(11) . . ?
O1 Zn01 N19 89.51(11) . . ?
N4 Zn01 N19 90.30(11) . . ?
N14 Zn01 N19 91.28(11) . . ?
N21 Zn01 N19 92.01(10) . . ?
O1 Zn01 N9 86.13(11) . . ?
N4 Zn01 N9 90.44(11) . . ?
N14 Zn01 N9 87.89(11) . . ?
N21 Zn01 N9 92.39(11) . . ?
N19 Zn01 N9 175.54(10) . . ?
Zn01 O1 H1A 117(5) . . ?
Zn01 O1 H1B 123(4) . . ?
H1A O1 H1B 117(6) . . ?
N2 N1 C1 100.5(3) . . ?
N3 N2 N1 115.8(3) . . ?
N3 N2 N5 121.9(3) . . ?
N1 N2 N5 122.1(3) . . ?
N2 N3 N4 104.7(3) . . ?
C1 N4 N3 106.9(3) . . ?
C1 N4 Zn01 133.4(2) . . ?
N3 N4 Zn01 119.2(2) . . ?
N2 N5 H5A 105(3) . . ?
N2 N5 H5B 104(3) . . ?
H5A N5 H5B 112(4) . . ?
N8 N9 C2 106.7(3) . . ?
N8 N9 Zn01 127.1(2) . . ?
C2 N9 Zn01 126.1(2) . . ?
N7 N8 N9 104.5(3) . . ?
C2 N6 N7 100.6(3) . . ?
N8 N7 N6 115.6(3) . . ?
N8 N7 N10 123.6(3) . . ?
N6 N7 N10 120.8(3) . . ?
N7 N10 H10A 110(3) . . ?
N7 N10 H10B 110(3) . . ?
H10A N10 H10B 106(5) . . ?
C3 N14 N13 106.7(3) . . ?
C3 N14 Zn01 133.0(3) . . ?
N13 N14 Zn01 120.0(2) . . ?
N12 N13 N14 103.9(3) . . ?
N12 N11 C3 101.0(3) . . ?
N13 N12 N11 116.0(3) . . ?
N13 N12 N15 122.1(3) . . ?
N11 N12 N15 121.8(3) . . ?
N12 N15 H15B 106(4) . . ?
N12 N15 H15A 107(3) . . ?
H15B N15 H15A 106(5) . . ?
C4 N19 N18 106.5(3) . . ?
C4 N19 Zn01 134.8(2) . . ?
N18 N19 Zn01 118.4(2) . . ?
N17 N18 N19 104.5(3) . . ?
C4 N16 N17 101.3(3) . . ?
N18 N17 N16 115.2(3) . . ?
N18 N17 N20 122.4(3) . . ?
N16 N17 N20 122.2(3) . . ?
N17 N20 H20A 104(4) . . ?
N17 N20 H20B 105(4) . . ?
H20A N20 H20B 114(6) . . ?
N22 N21 C5 107.0(3) . . ?
N22 N21 Zn01 121.3(2) . . ?
C5 N21 Zn01 131.0(2) . . ?
N24 N22 N21 105.1(3) . . ?
C5 N23 N24 101.7(3) . . ?
N22 N24 N23 114.4(3) . . ?
N22 N24 N25 124.6(3) . . ?
N23 N24 N25 121.0(3) . . ?
N24 N25 H25B 111(3) . . ?
N24 N25 H25A 109(3) . . ?
H25B N25 H25A 107(4) . . ?
N4 C1 N1 112.2(3) . . ?
N4 C1 H1 124(3) . . ?
N1 C1 H1 123(3) . . ?
N6 C2 N9 112.6(3) . . ?
N6 C2 H2 125(3) . . ?
N9 C2 H2 123(3) . . ?
N16 C4 N19 112.5(3) . . ?
N16 C4 H4 122(3) . . ?
N19 C4 H4 125(3) . . ?
N14 C3 N11 112.4(4) . . ?
N14 C3 H3 125(4) . . ?
N11 C3 H3 123(4) . . ?
N23 C5 N21 111.7(3) . . ?
N23 C5 H5 126(3) . . ?
N21 C5 H5 122(3) . . ?
O4 Cl1 O2 110.5(2) . . ?
O4 Cl1 O3 109.42(19) . . ?
O2 Cl1 O3 109.38(19) . . ?
O4 Cl1 O5 110.00(19) . . ?
O2 Cl1 O5 108.41(18) . . ?
O3 Cl1 O5 109.1(2) . . ?
O8B Cl2 O7B 153.7(9) . . ?
O9A Cl2 O8A 175(2) . . ?
O9A Cl2 O6 69.7(10) . . ?
O8B Cl2 O6 84.1(8) . . ?
O7B Cl2 O6 116.9(6) . . ?
O8A Cl2 O6 110.5(7) . . ?
O8B Cl2 O9B 87.3(6) . . ?
O7B Cl2 O9B 103.2(5) . . ?
O6 Cl2 O9B 100.1(5) . . ?
O9A Cl2 O7A 110(2) . . ?
O8A Cl2 O7A 74.5(7) . . ?
O6 Cl2 O7A 97.8(6) . . ?
Cl2 O6 O9A 50.5(6) . . ?
Cl2 O9A O6 59.8(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.5(4) . . . . ?
C1 N1 N2 N5 -176.0(3) . . . . ?
N1 N2 N3 N4 0.3(4) . . . . ?
N5 N2 N3 N4 175.8(3) . . . . ?
N2 N3 N4 C1 0.1(4) . . . . ?
N2 N3 N4 Zn01 172.6(2) . . . . ?
C2 N9 N8 N7 0.8(4) . . . . ?
Zn01 N9 N8 N7 -178.6(2) . . . . ?
N9 N8 N7 N6 -0.2(4) . . . . ?
N9 N8 N7 N10 178.2(3) . . . . ?
C2 N6 N7 N8 -0.5(4) . . . . ?
C2 N6 N7 N10 -178.9(3) . . . . ?
C3 N14 N13 N12 -0.1(4) . . . . ?
Zn01 N14 N13 N12 175.0(2) . . . . ?
N14 N13 N12 N11 0.7(4) . . . . ?
N14 N13 N12 N15 176.3(3) . . . . ?
C3 N11 N12 N13 -1.0(5) . . . . ?
C3 N11 N12 N15 -176.6(4) . . . . ?
C4 N19 N18 N17 0.3(3) . . . . ?
Zn01 N19 N18 N17 -174.0(2) . . . . ?
N19 N18 N17 N16 -0.5(4) . . . . ?
N19 N18 N17 N20 -175.6(3) . . . . ?
C4 N16 N17 N18 0.5(4) . . . . ?
C4 N16 N17 N20 175.6(3) . . . . ?
C5 N21 N22 N24 0.8(3) . . . . ?
Zn01 N21 N22 N24 -170.95(19) . . . . ?
N21 N22 N24 N23 -0.4(4) . . . . ?
N21 N22 N24 N25 178.4(3) . . . . ?
C5 N23 N24 N22 -0.2(4) . . . . ?
C5 N23 N24 N25 -179.0(3) . . . . ?
N3 N4 C1 N1 -0.4(4) . . . . ?
Zn01 N4 C1 N1 -171.4(3) . . . . ?
N2 N1 C1 N4 0.5(4) . . . . ?
N7 N6 C2 N9 1.0(4) . . . . ?
N8 N9 C2 N6 -1.2(4) . . . . ?
Zn01 N9 C2 N6 178.2(2) . . . . ?
N17 N16 C4 N19 -0.2(4) . . . . ?
N18 N19 C4 N16 -0.1(4) . . . . ?
Zn01 N19 C4 N16 173.0(2) . . . . ?
N13 N14 C3 N11 -0.5(5) . . . . ?
Zn01 N14 C3 N11 -174.7(3) . . . . ?
N12 N11 C3 N14 0.9(5) . . . . ?
N24 N23 C5 N21 0.7(4) . . . . ?
N22 N21 C5 N23 -1.0(4) . . . . ?
Zn01 N21 C5 N23 169.7(2) . . . . ?
O8B Cl2 O6 O9A 151(2) . . . . ?
O7B Cl2 O6 O9A -45(2) . . . . ?
O8A Cl2 O6 O9A 175(2) . . . . ?
O9B Cl2 O6 O9A 65(2) . . . . ?
O7A Cl2 O6 O9A -109(2) . . . . ?
O8B Cl2 O9A O6 -50(3) . . . . ?
O7B Cl2 O9A O6 135.3(15) . . . . ?
O9B Cl2 O9A O6 -109.0(12) . . . . ?
O7A Cl2 O9A O6 91.0(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
? ? ? ? ? ? ? ?

_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         2.754
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.120

_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_mx217
_database_code_depnum_ccdc_archive 'CCDC 1834857'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue May 16 15:37:12 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexaaqua manganese(II) di-1-aminotetrazolyl phloroglucinolate
;
_chemical_name_common            
'hexaaqua manganese(II) di-1-aminotetrazolyl phloroglucinolate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C6 H2 N3 O9), H12 Mn O6, 2(C H3 N5)'
_chemical_formula_sum            'C14 H22 Mn N16 O24'
_chemical_formula_weight         853.41

_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                   14.8973(9)
_cell_length_b                   5.0185(2)
_cell_length_c                   20.4159(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.628(5)
_cell_angle_gamma                90
_cell_volume                     1483.36(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    2287
_cell_measurement_theta_min      4.5450
_cell_measurement_theta_max      32.1620

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.578
_shelx_estimated_absorpt_T_min   0.855
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86825
_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    1.911
_exptl_crystal_F_000             870
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            11409
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.189
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3079
_reflns_number_gt                2410
_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)+(0.0253P)²+0.7227P] 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         3079
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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      -0.0064214000
_diffrn_orient_matrix_UB_12      -0.0572837000
_diffrn_orient_matrix_UB_13      0.0303459000
_diffrn_orient_matrix_UB_21      0.0482493000
_diffrn_orient_matrix_UB_22      -0.0216309000
_diffrn_orient_matrix_UB_23      0.0108745000
_diffrn_orient_matrix_UB_31      0.0053159000
_diffrn_orient_matrix_UB_32      0.1273626000
_diffrn_orient_matrix_UB_33      0.0155079000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -98.00  -18.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega -100.00   33.60   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -19.0000   90.0000 167

#__ type_ start__ end____ width___ exp.time_
  3 omega   -4.00   40.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
  4 omega  -15.00   74.60   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 112

#__ type_ start__ end____ width___ exp.time_
  5 omega   66.00  106.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
  6 omega   63.00  110.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -90.0000 59

#__ type_ start__ end____ width___ exp.time_
  7 omega   -2.00   32.40   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   88.0000 -102.0000 43

;



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'
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
O1 O 0.27548(10) 0.4256(3) 0.40275(8) 0.0157(3) Uani 1 1 d . . . . .
O2 O 0.27026(11) 0.7020(3) 0.51440(8) 0.0235(4) Uani 1 1 d . . . . .
O3 O 0.16259(12) 0.9998(3) 0.49266(9) 0.0244(4) Uani 1 1 d . . . . .
O4 O 0.00521(13) 0.7583(3) 0.45967(9) 0.0213(4) Uani 1 1 d . . . . .
O5 O -0.14295(11) 0.5233(3) 0.40624(8) 0.0230(4) Uani 1 1 d . . . . .
O6 O -0.14362(11) 0.1794(3) 0.34180(9) 0.0263(4) Uani 1 1 d . . . . .
O7 O -0.00493(12) 0.0580(3) 0.29472(8) 0.0197(4) Uani 1 1 d . . . . .
O8 O 0.16433(12) 0.2006(3) 0.24307(8) 0.0248(4) Uani 1 1 d . . . . .
O9 O 0.22043(11) -0.0772(3) 0.32297(9) 0.0235(4) Uani 1 1 d . . . . .
N1 N 0.19419(13) 0.7794(4) 0.48283(10) 0.0165(4) Uani 1 1 d . . . . .
N2 N -0.10078(13) 0.3679(4) 0.37544(10) 0.0184(4) Uani 1 1 d . . . . .
N3 N 0.17483(12) 0.1186(4) 0.30115(9) 0.0145(4) Uani 1 1 d . . . . .
C1 C 0.18956(15) 0.4331(4) 0.39579(11) 0.0129(5) Uani 1 1 d . . . . .
C2 C 0.14067(15) 0.6017(4) 0.43249(11) 0.0143(5) Uani 1 1 d . . . . .
C3 C 0.04538(15) 0.5954(4) 0.42371(11) 0.0145(5) Uani 1 1 d . . . . .
C4 C -0.00721(15) 0.4026(4) 0.37882(11) 0.0145(5) Uani 1 1 d . . . . .
C5 C 0.03781(16) 0.2397(4) 0.33874(11) 0.0142(5) Uani 1 1 d . . . . .
C6 C 0.13056(15) 0.2704(4) 0.34626(11) 0.0134(5) Uani 1 1 d . . . . .
Mn Mn 0.5000 0.5000 0.0000 0.01396(13) Uani 1 2 d S . P . .
O10 O 0.40259(12) 0.6740(4) -0.08649(9) 0.0207(4) Uani 1 1 d . . . . .
O11 O 0.39152(12) 0.2489(3) 0.02320(10) 0.0174(4) Uani 1 1 d . . . . .
O12 O 0.47908(13) 0.7831(4) 0.07339(10) 0.0195(4) Uani 1 1 d . . . . .
N4 N 0.35688(13) 0.3356(4) 0.19231(10) 0.0171(4) Uani 1 1 d . . . . .
N5 N 0.39839(14) 0.0970(4) 0.19376(10) 0.0231(5) Uani 1 1 d . . . . .
N6 N 0.42552(14) 0.0353(4) 0.25706(10) 0.0252(5) Uani 1 1 d . . . . .
N7 N 0.40181(14) 0.2298(4) 0.29679(10) 0.0228(5) Uani 1 1 d . . . . .
N8 N 0.32327(17) 0.4600(5) 0.12970(11) 0.0239(5) Uani 1 1 d . . . . .
C7 C 0.35948(17) 0.4119(5) 0.25494(12) 0.0201(5) Uani 1 1 d . . . . .
H4 H -0.047(2) 0.722(7) 0.4520(18) 0.056(12) Uiso 1 1 d . . . . .
H12A H 0.453(2) 0.917(6) 0.0624(15) 0.035(9) Uiso 1 1 d . . . . .
H11A H 0.353(2) 0.195(6) -0.0068(16) 0.033(9) Uiso 1 1 d . . . . .
H10A H 0.378(2) 0.572(6) -0.1120(16) 0.037(10) Uiso 1 1 d . . . . .
H7 H -0.057(2) 0.061(6) 0.2953(15) 0.041(10) Uiso 1 1 d . . . . .
H1 H 0.3329(17) 0.568(5) 0.2673(13) 0.025(7) Uiso 1 1 d . . . . .
H10B H 0.361(2) 0.795(7) -0.0861(17) 0.057(11) Uiso 1 1 d . . . . .
H12B H 0.513(2) 0.794(6) 0.1080(17) 0.043(10) Uiso 1 1 d . . . . .
H8B H 0.349(2) 0.618(7) 0.1300(16) 0.050(10) Uiso 1 1 d . . . . .
H11B H 0.365(2) 0.314(6) 0.0539(17) 0.049(10) Uiso 1 1 d . . . . .
H8A H 0.265(3) 0.475(7) 0.1263(18) 0.065(12) 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
O1 C1 1.255(3) . ?
O2 N1 1.227(2) . ?
O3 N1 1.237(2) . ?
O4 C3 1.331(3) . ?
O4 H4 0.78(3) . ?
O5 N2 1.259(2) . ?
O6 N2 1.252(2) . ?
O7 C5 1.332(3) . ?
O7 H7 0.78(3) . ?
O8 N3 1.230(2) . ?
O9 N3 1.218(2) . ?
N1 C2 1.449(3) . ?
N2 C4 1.390(3) . ?
N3 C6 1.466(3) . ?
C1 C6 1.430(3) . ?
C1 C2 1.437(3) . ?
C2 C3 1.389(3) . ?
C3 C4 1.432(3) . ?
C4 C5 1.431(3) . ?
C5 C6 1.363(3) . ?
Mn O12 2.1402(18) . ?
Mn O12 2.1402(18) 3_665 ?
Mn O10 2.1859(17) 3_665 ?
Mn O10 2.1859(17) . ?
Mn O11 2.1873(17) . ?
Mn O11 2.1873(17) 3_665 ?
O10 H10A 0.76(3) . ?
O10 H10B 0.87(4) . ?
O11 H11A 0.78(3) . ?
O11 H11B 0.88(4) . ?
O12 H12A 0.78(3) . ?
O12 H12B 0.77(3) . ?
N4 C7 1.326(3) . ?
N4 N5 1.345(3) . ?
N4 N8 1.404(3) . ?
N5 N6 1.297(3) . ?
N6 N7 1.368(3) . ?
N7 C7 1.307(3) . ?
N8 H8B 0.88(3) . ?
N8 H8A 0.85(4) . ?
C7 H1 0.94(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
C3 O4 H4 108(3) . . ?
C5 O7 H7 107(2) . . ?
O2 N1 O3 122.51(19) . . ?
O2 N1 C2 117.59(18) . . ?
O3 N1 C2 119.90(19) . . ?
O6 N2 O5 119.49(19) . . ?
O6 N2 C4 119.8(2) . . ?
O5 N2 C4 120.67(19) . . ?
O9 N3 O8 123.8(2) . . ?
O9 N3 C6 118.96(18) . . ?
O8 N3 C6 117.26(18) . . ?
O1 C1 C6 120.2(2) . . ?
O1 C1 C2 126.0(2) . . ?
C6 C1 C2 113.74(19) . . ?
C3 C2 C1 123.2(2) . . ?
C3 C2 N1 118.7(2) . . ?
C1 C2 N1 118.04(19) . . ?
O4 C3 C2 119.6(2) . . ?
O4 C3 C4 121.2(2) . . ?
C2 C3 C4 119.1(2) . . ?
N2 C4 C5 120.0(2) . . ?
N2 C4 C3 120.5(2) . . ?
C5 C4 C3 119.5(2) . . ?
O7 C5 C6 117.7(2) . . ?
O7 C5 C4 124.3(2) . . ?
C6 C5 C4 118.1(2) . . ?
C5 C6 C1 125.6(2) . . ?
C5 C6 N3 117.70(19) . . ?
C1 C6 N3 116.66(19) . . ?
O12 Mn O12 180.00(10) . 3_665 ?
O12 Mn O10 82.99(8) . 3_665 ?
O12 Mn O10 97.01(8) 3_665 3_665 ?
O12 Mn O10 97.01(8) . . ?
O12 Mn O10 82.99(8) 3_665 . ?
O10 Mn O10 180.0 3_665 . ?
O12 Mn O11 89.65(7) . . ?
O12 Mn O11 90.35(7) 3_665 . ?
O10 Mn O11 88.78(7) 3_665 . ?
O10 Mn O11 91.22(7) . . ?
O12 Mn O11 90.35(7) . 3_665 ?
O12 Mn O11 89.65(7) 3_665 3_665 ?
O10 Mn O11 91.22(7) 3_665 3_665 ?
O10 Mn O11 88.78(7) . 3_665 ?
O11 Mn O11 180.0 . 3_665 ?
Mn O10 H10A 114(2) . . ?
Mn O10 H10B 128(2) . . ?
H10A O10 H10B 105(3) . . ?
Mn O11 H11A 118(2) . . ?
Mn O11 H11B 115(2) . . ?
H11A O11 H11B 108(3) . . ?
Mn O12 H12A 121(2) . . ?
Mn O12 H12B 121(2) . . ?
H12A O12 H12B 112(3) . . ?
C7 N4 N5 109.08(19) . . ?
C7 N4 N8 132.2(2) . . ?
N5 N4 N8 118.63(19) . . ?
N6 N5 N4 105.56(19) . . ?
N5 N6 N7 110.90(19) . . ?
C7 N7 N6 105.3(2) . . ?
N4 N8 H8B 109(2) . . ?
N4 N8 H8A 105(2) . . ?
H8B N8 H8A 110(3) . . ?
N7 C7 N4 109.2(2) . . ?
N7 C7 H1 125.2(16) . . ?
N4 C7 H1 125.5(16) . . ?

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
O1 C1 C2 C3 -178.2(2) . . . . ?
C6 C1 C2 C3 3.8(3) . . . . ?
O1 C1 C2 N1 -0.6(3) . . . . ?
C6 C1 C2 N1 -178.55(19) . . . . ?
O2 N1 C2 C3 143.8(2) . . . . ?
O3 N1 C2 C3 -36.1(3) . . . . ?
O2 N1 C2 C1 -33.9(3) . . . . ?
O3 N1 C2 C1 146.2(2) . . . . ?
C1 C2 C3 O4 -180.0(2) . . . . ?
N1 C2 C3 O4 2.4(3) . . . . ?
C1 C2 C3 C4 3.6(3) . . . . ?
N1 C2 C3 C4 -174.05(19) . . . . ?
O6 N2 C4 C5 6.1(3) . . . . ?
O5 N2 C4 C5 -174.3(2) . . . . ?
O6 N2 C4 C3 -172.0(2) . . . . ?
O5 N2 C4 C3 7.5(3) . . . . ?
O4 C3 C4 N2 -4.8(3) . . . . ?
C2 C3 C4 N2 171.7(2) . . . . ?
O4 C3 C4 C5 177.1(2) . . . . ?
C2 C3 C4 C5 -6.5(3) . . . . ?
N2 C4 C5 O7 3.0(3) . . . . ?
C3 C4 C5 O7 -178.8(2) . . . . ?
N2 C4 C5 C6 -176.5(2) . . . . ?
C3 C4 C5 C6 1.6(3) . . . . ?
O7 C5 C6 C1 -172.9(2) . . . . ?
C4 C5 C6 C1 6.7(3) . . . . ?
O7 C5 C6 N3 5.3(3) . . . . ?
C4 C5 C6 N3 -175.11(19) . . . . ?
O1 C1 C6 C5 172.6(2) . . . . ?
C2 C1 C6 C5 -9.3(3) . . . . ?
O1 C1 C6 N3 -5.6(3) . . . . ?
C2 C1 C6 N3 172.51(18) . . . . ?
O9 N3 C6 C5 -104.1(2) . . . . ?
O8 N3 C6 C5 76.9(3) . . . . ?
O9 N3 C6 C1 74.3(3) . . . . ?
O8 N3 C6 C1 -104.8(2) . . . . ?
C7 N4 N5 N6 -0.3(3) . . . . ?
N8 N4 N5 N6 177.5(2) . . . . ?
N4 N5 N6 N7 0.3(3) . . . . ?
N5 N6 N7 C7 -0.2(3) . . . . ?
N6 N7 C7 N4 -0.1(3) . . . . ?
N5 N4 C7 N7 0.3(3) . . . . ?
N8 N4 C7 N7 -177.1(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
O4 H4 O5 0.78(3) 1.81(3) 2.514(2) 149(4) .
O4 H4 N2 0.78(3) 2.38(3) 2.830(3) 118(3) .
O12 H12A O11 0.78(3) 1.98(3) 2.755(3) 172(3) 1_565
O11 H11A O1 0.78(3) 2.03(3) 2.793(2) 167(3) 4_565
O11 H11A O2 0.78(3) 2.43(3) 2.874(2) 117(3) 4_565
O10 H10A O9 0.76(3) 2.42(3) 2.942(2) 128(3) 4_565
O10 H10A N7 0.76(3) 2.49(3) 3.126(3) 143(3) 4_565
O7 H7 O6 0.78(3) 1.87(3) 2.549(2) 145(3) .
O7 H7 O8 0.78(3) 2.42(3) 2.931(2) 124(3) 2_545
O7 H7 N2 0.78(3) 2.45(3) 2.878(3) 117(3) .
O10 H10B O1 0.87(4) 1.87(4) 2.734(2) 171(3) 4_575
O12 H12B N7 0.77(3) 2.08(3) 2.833(3) 166(3) 2_655
N8 H8B O12 0.88(3) 2.61(3) 3.255(3) 131(3) .
O11 H11B N8 0.88(4) 1.94(4) 2.815(3) 172(3) .
N8 H8A O6 0.85(4) 2.30(4) 3.074(3) 150(3) 2
O4 H4 O5 0.78(3) 1.81(3) 2.514(2) 149(4) .
O4 H4 N2 0.78(3) 2.38(3) 2.830(3) 118(3) .
O12 H12A O11 0.78(3) 1.98(3) 2.755(3) 172(3) 1_565
O11 H11A O1 0.78(3) 2.03(3) 2.793(2) 167(3) 4_565
O11 H11A O2 0.78(3) 2.43(3) 2.874(2) 117(3) 4_565
O10 H10A O9 0.76(3) 2.42(3) 2.942(2) 128(3) 4_565
O10 H10A N7 0.76(3) 2.49(3) 3.126(3) 143(3) 4_565
O7 H7 O6 0.78(3) 1.87(3) 2.549(2) 145(3) .
O7 H7 O8 0.78(3) 2.42(3) 2.931(2) 124(3) 2_545
O7 H7 N2 0.78(3) 2.45(3) 2.878(3) 117(3) .
O10 H10B O1 0.87(4) 1.87(4) 2.734(2) 171(3) 4_575
O12 H12B N7 0.77(3) 2.08(3) 2.833(3) 166(3) 2_655
N8 H8B O12 0.88(3) 2.61(3) 3.255(3) 131(3) .
O11 H11B N8 0.88(4) 1.94(4) 2.815(3) 172(3) .
N8 H8A O6 0.85(4) 2.30(4) 3.074(3) 150(3) 2

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



_refine_diff_density_max         0.346
_refine_diff_density_min         -0.299
_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_mx253
_database_code_depnum_ccdc_archive 'CCDC 1834858'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Jun 02 17:16:54 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexaaquamanganese(II) distyphnate bis(1-aminotetrazole)
;
_chemical_name_common            
'hexaaquamanganese(II) distyphnate bis(1-aminotetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	2(C6 H2 N3 O8), H12 Mn O6, 2(C H3 N5)'
_chemical_formula_sum            'C14 H22 Mn N16 O22'
_chemical_formula_weight         821.41

_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                   14.7040(6)
_cell_length_b                   5.0490(2)
_cell_length_c                   20.4680(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.858(4)
_cell_angle_gamma                90
_cell_volume                     1475.32(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    3786
_cell_measurement_theta_min      4.5830
_cell_measurement_theta_max      32.1130

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.573
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96274
_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    1.849
_exptl_crystal_F_000             838
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      143(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            10483
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.164
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2885
_reflns_number_gt                2540
_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)+(0.0343P)²+0.6359P] 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         2885
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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      0.0448413000
_diffrn_orient_matrix_UB_12      0.0440990000
_diffrn_orient_matrix_UB_13      -0.0025580000
_diffrn_orient_matrix_UB_21      -0.0193454000
_diffrn_orient_matrix_UB_22      0.0414305000
_diffrn_orient_matrix_UB_23      -0.0335451000
_diffrn_orient_matrix_UB_31      -0.0092272000
_diffrn_orient_matrix_UB_32      0.1267378000
_diffrn_orient_matrix_UB_33      0.0119148000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega   11.00   65.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -150.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
  4 omega   29.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  5 omega  -36.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -60.0000 116

#__ type_ start__ end____ width___ exp.time_
  6 omega   47.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
  7 omega   43.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -60.0000 26

;



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'
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
O4 O 0.26990(8) 0.0810(2) 0.40928(6) 0.0194(3) Uani 1 1 d . . . . .
O5 O 0.21196(9) 0.5934(2) 0.32808(7) 0.0267(3) Uani 1 1 d . . . . .
O6 O 0.17015(9) 0.2915(2) 0.25204(6) 0.0238(3) Uani 1 1 d . . . . .
O7 O -0.01220(8) 0.4445(2) 0.29201(6) 0.0220(3) Uani 1 1 d . . . . .
H7 H -0.0702 0.4463 0.2889 0.033 Uiso 1 1 calc R U . . .
O8 O -0.16105(9) 0.2989(2) 0.32956(6) 0.0261(3) Uani 1 1 d . . . . .
O9 O -0.15836(9) -0.0380(3) 0.39579(7) 0.0273(3) Uani 1 1 d . . . . .
O10 O 0.12504(10) -0.4372(3) 0.50759(7) 0.0337(3) Uani 1 1 d . . . . .
O11 O 0.25896(10) -0.2638(3) 0.50676(7) 0.0397(4) Uani 1 1 d . . . . .
N6 N 0.17207(9) 0.3871(3) 0.30747(7) 0.0168(3) Uani 1 1 d . . . . .
N7 N -0.11797(10) 0.1212(3) 0.36706(7) 0.0197(3) Uani 1 1 d . . . . .
N8 N 0.17349(11) -0.2747(3) 0.48624(7) 0.0232(3) Uani 1 1 d . . . . .
C2 C 0.18177(11) 0.0767(3) 0.40077(8) 0.0156(3) Uani 1 1 d . . . . .
C3 C 0.12389(11) 0.2395(3) 0.35101(8) 0.0156(3) Uani 1 1 d . . . . .
C4 C 0.02832(11) 0.2685(3) 0.33851(8) 0.0157(3) Uani 1 1 d . . . . .
C5 C -0.01873(11) 0.1063(3) 0.37653(8) 0.0170(3) Uani 1 1 d . . . . .
C6 C 0.03139(12) -0.0718(3) 0.42303(8) 0.0179(3) Uani 1 1 d . . . . .
H6 H -0.0011 -0.1861 0.4465 0.021 Uiso 1 1 calc R U . . .
C7 C 0.12748(12) -0.0856(3) 0.43577(8) 0.0176(3) Uani 1 1 d . . . . .
Mn1 Mn 0.5000 0.0000 0.0000 0.01430(11) Uani 1 2 d S . P . .
O1 O 0.60128(9) 0.1797(3) 0.08465(7) 0.0216(3) Uani 1 1 d . . . . .
O2 O 0.47703(9) -0.2723(2) 0.07426(7) 0.0201(3) Uani 1 1 d . . . . .
O3 O 0.39316(9) 0.2651(2) 0.02360(7) 0.0173(3) Uani 1 1 d . . . . .
N1 N 0.35662(9) 0.1780(3) 0.19180(7) 0.0162(3) Uani 1 1 d . . . . .
N2 N 0.39696(11) 0.4178(3) 0.19483(7) 0.0239(3) Uani 1 1 d . . . . .
N3 N 0.42318(11) 0.4769(3) 0.25799(8) 0.0250(3) Uani 1 1 d . . . . .
N4 N 0.40037(11) 0.2778(3) 0.29651(7) 0.0230(3) Uani 1 1 d . . . . .
N5 N 0.32395(12) 0.0583(3) 0.12872(8) 0.0216(3) Uani 1 1 d . . . . .
C1 C 0.35880(12) 0.0964(3) 0.25389(9) 0.0201(4) Uani 1 1 d . . . . .
H1 H 0.3343 -0.0664 0.2655 0.024 Uiso 1 1 calc R U . . .
H3B H 0.3500(19) 0.317(5) -0.0080(14) 0.047(7) Uiso 1 1 d . . . . .
H5A H 0.2650(17) 0.056(4) 0.1195(11) 0.027(6) Uiso 1 1 d . . . . .
H2A H 0.4506(17) -0.414(5) 0.0620(12) 0.036(6) Uiso 1 1 d . . . . .
H2B H 0.515(2) -0.287(5) 0.1119(15) 0.051(8) Uiso 1 1 d . . . . .
H3A H 0.3696(17) 0.213(5) 0.0542(13) 0.039(7) Uiso 1 1 d . . . . .
H5B H 0.3438(18) -0.098(5) 0.1307(12) 0.046(7) Uiso 1 1 d . . . . .
H1B H 0.649(2) 0.287(6) 0.0842(14) 0.063(9) Uiso 1 1 d . . . . .
H1A H 0.6230(19) 0.084(6) 0.1128(14) 0.051(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
O4 C2 1.266(2) . ?
O5 N6 1.2204(18) . ?
O6 N6 1.2269(18) . ?
O7 C4 1.3337(19) . ?
O7 H7 0.8400 . ?
O8 N7 1.2500(19) . ?
O9 N7 1.2296(19) . ?
O10 N8 1.233(2) . ?
O11 N8 1.227(2) . ?
N6 C3 1.468(2) . ?
N7 C5 1.427(2) . ?
N8 C7 1.450(2) . ?
C2 C3 1.422(2) . ?
C2 C7 1.448(2) . ?
C3 C4 1.375(2) . ?
C4 C5 1.419(2) . ?
C5 C6 1.386(2) . ?
C6 C7 1.376(2) . ?
C6 H6 0.9500 . ?
Mn1 O2 2.1358(12) 3_655 ?
Mn1 O2 2.1358(12) . ?
Mn1 O1 2.1923(12) 3_655 ?
Mn1 O1 2.1923(12) . ?
Mn1 O3 2.2038(12) . ?
Mn1 O3 2.2038(12) 3_655 ?
O1 H1B 0.89(3) . ?
O1 H1A 0.76(3) . ?
O2 H2A 0.82(3) . ?
O2 H2B 0.84(3) . ?
O3 H3B 0.83(3) . ?
O3 H3A 0.83(3) . ?
N1 C1 1.329(2) . ?
N1 N2 1.3430(19) . ?
N1 N5 1.4021(19) . ?
N2 N3 1.292(2) . ?
N3 N4 1.368(2) . ?
N4 C1 1.311(2) . ?
N5 H5A 0.84(2) . ?
N5 H5B 0.84(3) . ?
C1 H1 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
C4 O7 H7 109.5 . . ?
O5 N6 O6 123.92(14) . . ?
O5 N6 C3 119.05(13) . . ?
O6 N6 C3 117.03(13) . . ?
O9 N7 O8 122.08(14) . . ?
O9 N7 C5 119.72(14) . . ?
O8 N7 C5 118.19(14) . . ?
O11 N8 O10 122.66(15) . . ?
O11 N8 C7 118.64(15) . . ?
O10 N8 C7 118.69(15) . . ?
O4 C2 C3 120.40(15) . . ?
O4 C2 C7 127.54(15) . . ?
C3 C2 C7 112.04(14) . . ?
C4 C3 C2 127.22(15) . . ?
C4 C3 N6 116.95(14) . . ?
C2 C3 N6 115.81(14) . . ?
O7 C4 C3 117.78(14) . . ?
O7 C4 C5 125.66(15) . . ?
C3 C4 C5 116.56(15) . . ?
C6 C5 C4 120.15(15) . . ?
C6 C5 N7 119.05(15) . . ?
C4 C5 N7 120.80(15) . . ?
C7 C6 C5 121.06(16) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C2 122.73(15) . . ?
C6 C7 N8 116.83(15) . . ?
C2 C7 N8 120.45(15) . . ?
O2 Mn1 O2 180.00(7) 3_655 . ?
O2 Mn1 O1 84.10(5) 3_655 3_655 ?
O2 Mn1 O1 95.90(5) . 3_655 ?
O2 Mn1 O1 95.90(5) 3_655 . ?
O2 Mn1 O1 84.10(5) . . ?
O1 Mn1 O1 180.0 3_655 . ?
O2 Mn1 O3 90.43(5) 3_655 . ?
O2 Mn1 O3 89.57(5) . . ?
O1 Mn1 O3 92.27(5) 3_655 . ?
O1 Mn1 O3 87.73(5) . . ?
O2 Mn1 O3 89.57(5) 3_655 3_655 ?
O2 Mn1 O3 90.43(5) . 3_655 ?
O1 Mn1 O3 87.73(5) 3_655 3_655 ?
O1 Mn1 O3 92.27(5) . 3_655 ?
O3 Mn1 O3 180.0 . 3_655 ?
Mn1 O1 H1B 129.3(19) . . ?
Mn1 O1 H1A 115(2) . . ?
H1B O1 H1A 102(3) . . ?
Mn1 O2 H2A 119.1(16) . . ?
Mn1 O2 H2B 122.0(18) . . ?
H2A O2 H2B 111(2) . . ?
Mn1 O3 H3B 118.2(17) . . ?
Mn1 O3 H3A 114.8(16) . . ?
H3B O3 H3A 108(2) . . ?
C1 N1 N2 109.03(13) . . ?
C1 N1 N5 132.16(14) . . ?
N2 N1 N5 118.78(13) . . ?
N3 N2 N1 106.09(14) . . ?
N2 N3 N4 110.55(14) . . ?
C1 N4 N3 105.65(14) . . ?
N1 N5 H5A 108.7(15) . . ?
N1 N5 H5B 108.8(17) . . ?
H5A N5 H5B 109(2) . . ?
N4 C1 N1 108.68(15) . . ?
N4 C1 H1 125.7 . . ?
N1 C1 H1 125.7 . . ?

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
O4 C2 C3 C4 -175.85(15) . . . . ?
C7 C2 C3 C4 5.5(2) . . . . ?
O4 C2 C3 N6 5.7(2) . . . . ?
C7 C2 C3 N6 -172.92(13) . . . . ?
O5 N6 C3 C4 100.23(18) . . . . ?
O6 N6 C3 C4 -80.41(18) . . . . ?
O5 N6 C3 C2 -81.15(18) . . . . ?
O6 N6 C3 C2 98.21(17) . . . . ?
C2 C3 C4 O7 175.93(15) . . . . ?
N6 C3 C4 O7 -5.6(2) . . . . ?
C2 C3 C4 C5 -4.2(2) . . . . ?
N6 C3 C4 C5 174.21(13) . . . . ?
O7 C4 C5 C6 179.27(15) . . . . ?
C3 C4 C5 C6 -0.6(2) . . . . ?
O7 C4 C5 N7 0.0(2) . . . . ?
C3 C4 C5 N7 -179.80(14) . . . . ?
O9 N7 C5 C6 -6.1(2) . . . . ?
O8 N7 C5 C6 173.61(15) . . . . ?
O9 N7 C5 C4 173.16(14) . . . . ?
O8 N7 C5 C4 -7.1(2) . . . . ?
C4 C5 C6 C7 3.4(2) . . . . ?
N7 C5 C6 C7 -177.38(15) . . . . ?
C5 C6 C7 C2 -1.8(3) . . . . ?
C5 C6 C7 N8 178.82(14) . . . . ?
O4 C2 C7 C6 179.16(16) . . . . ?
C3 C2 C7 C6 -2.4(2) . . . . ?
O4 C2 C7 N8 -1.4(3) . . . . ?
C3 C2 C7 N8 177.04(14) . . . . ?
O11 N8 C7 C6 -168.46(16) . . . . ?
O10 N8 C7 C6 10.4(2) . . . . ?
O11 N8 C7 C2 12.1(2) . . . . ?
O10 N8 C7 C2 -169.04(15) . . . . ?
C1 N1 N2 N3 0.33(18) . . . . ?
N5 N1 N2 N3 -177.82(15) . . . . ?
N1 N2 N3 N4 0.00(19) . . . . ?
N2 N3 N4 C1 -0.33(19) . . . . ?
N3 N4 C1 N1 0.52(19) . . . . ?
N2 N1 C1 N4 -0.54(19) . . . . ?
N5 N1 C1 N4 177.27(17) . . . . ?

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
O7 H7 O8 0.84 1.89 2.5939(17) 140.8 .
O7 H7 O6 0.84 2.30 2.8763(17) 125.7 2
O7 H7 N7 0.84 2.51 2.9307(18) 112.3 .
O3 H3B O4 0.83(3) 1.89(3) 2.7078(18) 168(3) 4_565
N5 H5A O8 0.84(2) 2.42(2) 3.027(2) 129.1(18) 2_545
N5 H5A O9 0.84(2) 2.55(2) 3.122(2) 125.9(17) 2
O2 H2A O3 0.82(3) 1.91(3) 2.7272(17) 173(2) 1_545
O2 H2B N4 0.84(3) 2.02(3) 2.833(2) 165(2) 2_645
O3 H3A N5 0.83(3) 1.97(3) 2.794(2) 174(2) .
N5 H5B O2 0.84(3) 2.65(3) 3.209(2) 125(2) .
O1 H1B O4 0.89(3) 1.89(3) 2.7560(17) 165(3) 2_655
O1 H1B O11 0.89(3) 2.56(3) 3.1059(19) 120(2) 2_655
O1 H1A O5 0.76(3) 2.44(3) 2.9278(18) 123(2) 2_645
O1 H1A N4 0.76(3) 2.50(3) 3.172(2) 148(3) 2_645

_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         0.302
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.051

_shelxl_version_number           2013-4


