# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_lx162
_database_code_depnum_ccdc_archive 'CCDC 1566359'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Mar 30 14:05:47 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl)manganese(II) perchlorate di(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl)manganese(II) perchlorate di(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C12 H24 Mn N24, 2(C2 H4 N4), 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 Mn N32 O8'
_chemical_formula_weight         926.57

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.9801(4)
_cell_length_b                   11.4163(6)
_cell_length_c                   13.4480(8)
_cell_angle_alpha                111.348(5)
_cell_angle_beta                 100.966(5)
_cell_angle_gamma                94.176(4)
_cell_volume                     967.98(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4189
_cell_measurement_theta_min      4.6260
_cell_measurement_theta_max      31.6590

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.565
_shelx_estimated_absorpt_T_min   0.840
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96243
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             475
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            7471
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.470
_diffrn_reflns_theta_max         25.996
_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             3788
_reflns_number_gt                3273
_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)+(0.0425P)²+0.4282P] 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         3788
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0844
_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      0.0710611000
_diffrn_orient_matrix_UB_12      0.0560593000
_diffrn_orient_matrix_UB_13      0.0265372000
_diffrn_orient_matrix_UB_21      0.0636907000
_diffrn_orient_matrix_UB_22      -0.0288584000
_diffrn_orient_matrix_UB_23      -0.0338999000
_diffrn_orient_matrix_UB_31      -0.0432729000
_diffrn_orient_matrix_UB_32      0.0241773000
_diffrn_orient_matrix_UB_33      -0.0392186000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    3.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega    2.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega  -29.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  120.0000 120

#__ type_ start__ end____ width___ exp.time_
  4 omega  -21.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
  5 omega -109.00  -38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -30.0000 71

;



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 0.0000 0.0000 0.01523(12) Uani 1 2 d S . P . .
N1 N 0.1994(2) -0.11978(15) 0.05779(13) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.3355(3) 0.22739(18) 0.19167(16) 0.0196(4) Uani 1 1 d . . . . .
N2 N 0.3399(3) -0.06270(16) 0.15254(14) 0.0282(4) Uani 1 1 d . . . . .
N3 N 0.4291(3) -0.14691(16) 0.17743(14) 0.0272(4) Uani 1 1 d . . . . .
N4 N 0.3466(2) -0.26066(15) 0.09809(13) 0.0174(3) Uani 1 1 d . . . . .
N5 N 0.2356(2) 0.17366(15) 0.08833(13) 0.0190(3) Uani 1 1 d . . . . .
N6 N 0.2990(3) 0.24672(16) 0.03657(14) 0.0249(4) Uani 1 1 d . . . . .
N8 N 0.4542(2) 0.33003(15) 0.20364(13) 0.0186(3) Uani 1 1 d . . . . .
N9 N -0.1061(2) 0.04955(15) 0.15561(13) 0.0195(4) Uani 1 1 d . . . . .
N10 N -0.1616(3) 0.16436(16) 0.20726(14) 0.0274(4) Uani 1 1 d . . . . .
N11 N -0.2154(3) 0.16652(16) 0.29470(14) 0.0270(4) Uani 1 1 d . . . . .
N12 N -0.1962(2) 0.05276(15) 0.30052(12) 0.0182(3) Uani 1 1 d . . . . .
C1 C 0.2065(3) -0.24237(19) 0.02606(16) 0.0198(4) Uani 1 1 d . . . . .
C2 C 0.4111(4) -0.3767(2) 0.1038(2) 0.0254(5) Uani 1 1 d . . . . .
N7 N 0.4307(3) 0.34077(16) 0.10573(14) 0.0248(4) Uani 1 1 d . . . . .
C4 C 0.5976(3) 0.4210(2) 0.30028(19) 0.0266(5) Uani 1 1 d . . . . .
C5 C -0.1287(3) -0.01728(19) 0.21560(16) 0.0183(4) Uani 1 1 d . . . . .
C6 C -0.2422(4) 0.0223(2) 0.39051(17) 0.0260(5) Uani 1 1 d . . . . .
N13 N 0.0047(3) 0.70778(17) 0.20777(15) 0.0275(4) Uani 1 1 d . . . . .
N14 N -0.0662(3) 0.58396(18) 0.14398(15) 0.0321(4) Uani 1 1 d . . . . .
N15 N -0.0195(3) 0.51195(18) 0.19741(16) 0.0327(4) Uani 1 1 d . . . . .
N16 N 0.0832(2) 0.58966(17) 0.29863(14) 0.0238(4) Uani 1 1 d . . . . .
C7 C 0.0969(3) 0.7080(2) 0.30264(18) 0.0260(5) Uani 1 1 d . . . . .
C8 C 0.1467(4) 0.5416(3) 0.3847(2) 0.0396(6) Uani 1 1 d . . . . .
Cl1 Cl 0.30972(7) 0.23464(5) 0.49261(4) 0.02235(13) Uani 1 1 d . . . . .
O1 O 0.1474(3) 0.2532(2) 0.54265(17) 0.0615(6) Uani 1 1 d . . . . .
O2 O 0.3468(3) 0.33448(19) 0.45573(16) 0.0570(6) Uani 1 1 d . . . . .
O3 O 0.4797(3) 0.23860(18) 0.57250(16) 0.0524(5) Uani 1 1 d . . . . .
O4 O 0.2648(3) 0.11480(18) 0.40294(16) 0.0574(6) Uani 1 1 d . . . . .
H3 H 0.327(3) 0.200(2) 0.2450(18) 0.022(6) Uiso 1 1 d . . . . .
H5 H -0.106(3) -0.098(2) 0.2034(17) 0.017(5) Uiso 1 1 d . . . . .
H1 H 0.132(4) -0.301(2) -0.033(2) 0.037(7) Uiso 1 1 d . . . . .
H7 H 0.163(4) 0.782(3) 0.363(2) 0.055(8) Uiso 1 1 d . . . . .
H22 H 0.538(4) -0.379(2) 0.0930(19) 0.031(6) Uiso 1 1 d . . . . .
H61 H -0.256(4) -0.068(3) 0.369(2) 0.037(7) Uiso 1 1 d . . . . .
H43 H 0.592(4) 0.500(3) 0.303(2) 0.048(8) Uiso 1 1 d . . . . .
H41 H 0.734(4) 0.405(3) 0.291(2) 0.048(8) Uiso 1 1 d . . . . .
H81 H 0.272(5) 0.572(3) 0.414(2) 0.054(9) Uiso 1 1 d . . . . .
H62 H -0.132(4) 0.060(2) 0.454(2) 0.042(7) Uiso 1 1 d . . . . .
H21 H 0.328(4) -0.448(3) 0.045(2) 0.039(7) Uiso 1 1 d . . . . .
H42 H 0.575(4) 0.410(2) 0.366(2) 0.033(6) Uiso 1 1 d . . . . .
H23 H 0.411(4) -0.376(2) 0.174(2) 0.039(7) Uiso 1 1 d . . . . .
H82 H 0.121(5) 0.450(3) 0.352(2) 0.059(9) Uiso 1 1 d . . . . .
H63 H -0.361(5) 0.052(3) 0.406(2) 0.052(8) Uiso 1 1 d . . . . .
H83 H 0.063(4) 0.565(3) 0.437(2) 0.049(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
Mn1 N9 2.2440(16) 2 ?
Mn1 N9 2.2441(16) . ?
Mn1 N1 2.2473(16) 2 ?
Mn1 N1 2.2474(16) . ?
Mn1 N5 2.2612(15) 2 ?
Mn1 N5 2.2612(15) . ?
N1 C1 1.314(3) . ?
N1 N2 1.355(2) . ?
C3 N5 1.320(2) . ?
C3 N8 1.325(2) . ?
C3 H3 0.89(2) . ?
N2 N3 1.291(2) . ?
N3 N4 1.343(2) . ?
N4 C1 1.325(3) . ?
N4 C2 1.453(3) . ?
N5 N6 1.365(2) . ?
N6 N7 1.291(2) . ?
N8 N7 1.347(2) . ?
N8 C4 1.463(3) . ?
N9 C5 1.318(2) . ?
N9 N10 1.365(2) . ?
N10 N11 1.293(2) . ?
N11 N12 1.344(2) . ?
N12 C5 1.327(3) . ?
N12 C6 1.458(2) . ?
C1 H1 0.87(3) . ?
C2 H22 0.92(3) . ?
C2 H21 0.95(3) . ?
C2 H23 0.94(3) . ?
C4 H43 0.90(3) . ?
C4 H41 1.01(3) . ?
C4 H42 0.97(3) . ?
C5 H5 0.91(2) . ?
C6 H61 0.95(3) . ?
C6 H62 0.97(3) . ?
C6 H63 0.95(3) . ?
N13 C7 1.314(3) . ?
N13 N14 1.354(3) . ?
N14 N15 1.296(3) . ?
N15 N16 1.346(2) . ?
N16 C7 1.328(3) . ?
N16 C8 1.463(3) . ?
C7 H7 0.94(3) . ?
C8 H81 0.88(3) . ?
C8 H82 0.96(3) . ?
C8 H83 0.97(3) . ?
Cl1 O1 1.4152(18) . ?
Cl1 O4 1.4201(18) . ?
Cl1 O2 1.4246(18) . ?
Cl1 O3 1.4267(17) . ?

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 Mn1 N9 180.0 2 . ?
N9 Mn1 N1 88.54(6) 2 2 ?
N9 Mn1 N1 91.46(6) . 2 ?
N9 Mn1 N1 91.46(6) 2 . ?
N9 Mn1 N1 88.54(6) . . ?
N1 Mn1 N1 180.0 2 . ?
N9 Mn1 N5 87.89(6) 2 2 ?
N9 Mn1 N5 92.11(6) . 2 ?
N1 Mn1 N5 90.72(6) 2 2 ?
N1 Mn1 N5 89.28(6) . 2 ?
N9 Mn1 N5 92.11(6) 2 . ?
N9 Mn1 N5 87.89(6) . . ?
N1 Mn1 N5 89.28(6) 2 . ?
N1 Mn1 N5 90.72(6) . . ?
N5 Mn1 N5 180.0 2 . ?
C1 N1 N2 106.03(16) . . ?
C1 N1 Mn1 134.96(13) . . ?
N2 N1 Mn1 118.71(12) . . ?
N5 C3 N8 108.49(17) . . ?
N5 C3 H3 126.8(14) . . ?
N8 C3 H3 124.7(14) . . ?
N3 N2 N1 110.16(16) . . ?
N2 N3 N4 106.74(16) . . ?
C1 N4 N3 108.35(16) . . ?
C1 N4 C2 131.22(18) . . ?
N3 N4 C2 120.40(16) . . ?
C3 N5 N6 106.13(15) . . ?
C3 N5 Mn1 131.53(13) . . ?
N6 N5 Mn1 122.33(12) . . ?
N7 N6 N5 109.83(15) . . ?
C3 N8 N7 108.61(16) . . ?
C3 N8 C4 130.39(17) . . ?
N7 N8 C4 120.97(16) . . ?
C5 N9 N10 106.02(16) . . ?
C5 N9 Mn1 130.75(14) . . ?
N10 N9 Mn1 123.23(12) . . ?
N11 N10 N9 109.87(16) . . ?
N10 N11 N12 106.88(16) . . ?
C5 N12 N11 108.64(15) . . ?
C5 N12 C6 129.59(18) . . ?
N11 N12 C6 121.76(17) . . ?
N1 C1 N4 108.73(17) . . ?
N1 C1 H1 125.2(17) . . ?
N4 C1 H1 126.1(17) . . ?
N4 C2 H22 108.8(15) . . ?
N4 C2 H21 108.8(16) . . ?
H22 C2 H21 107(2) . . ?
N4 C2 H23 108.8(16) . . ?
H22 C2 H23 110(2) . . ?
H21 C2 H23 113(2) . . ?
N6 N7 N8 106.94(15) . . ?
N8 C4 H43 109.6(18) . . ?
N8 C4 H41 108.4(16) . . ?
H43 C4 H41 105(2) . . ?
N8 C4 H42 109.4(14) . . ?
H43 C4 H42 114(2) . . ?
H41 C4 H42 110(2) . . ?
N9 C5 N12 108.60(18) . . ?
N9 C5 H5 128.3(13) . . ?
N12 C5 H5 123.1(13) . . ?
N12 C6 H61 108.1(15) . . ?
N12 C6 H62 108.9(15) . . ?
H61 C6 H62 108(2) . . ?
N12 C6 H63 110.0(17) . . ?
H61 C6 H63 110(2) . . ?
H62 C6 H63 112(2) . . ?
C7 N13 N14 105.26(18) . . ?
N15 N14 N13 110.77(17) . . ?
N14 N15 N16 106.57(17) . . ?
C7 N16 N15 107.76(17) . . ?
C7 N16 C8 130.5(2) . . ?
N15 N16 C8 121.6(2) . . ?
N13 C7 N16 109.64(19) . . ?
N13 C7 H7 124.0(17) . . ?
N16 C7 H7 126.3(18) . . ?
N16 C8 H81 107.5(19) . . ?
N16 C8 H82 108.1(18) . . ?
H81 C8 H82 113(3) . . ?
N16 C8 H83 108.9(17) . . ?
H81 C8 H83 114(2) . . ?
H82 C8 H83 105(2) . . ?
O1 Cl1 O4 108.74(13) . . ?
O1 Cl1 O2 109.61(14) . . ?
O4 Cl1 O2 110.47(13) . . ?
O1 Cl1 O3 108.49(14) . . ?
O4 Cl1 O3 110.78(13) . . ?
O2 Cl1 O3 108.71(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 0.1(2) . . . . ?
Mn1 N1 N2 N3 174.80(13) . . . . ?
N1 N2 N3 N4 0.1(2) . . . . ?
N2 N3 N4 C1 -0.3(2) . . . . ?
N2 N3 N4 C2 -178.20(18) . . . . ?
N8 C3 N5 N6 0.6(2) . . . . ?
N8 C3 N5 Mn1 -178.37(13) . . . . ?
C3 N5 N6 N7 -0.3(2) . . . . ?
Mn1 N5 N6 N7 178.79(13) . . . . ?
N5 C3 N8 N7 -0.7(2) . . . . ?
N5 C3 N8 C4 -178.6(2) . . . . ?
C5 N9 N10 N11 0.0(2) . . . . ?
Mn1 N9 N10 N11 -179.87(13) . . . . ?
N9 N10 N11 N12 -0.3(2) . . . . ?
N10 N11 N12 C5 0.4(2) . . . . ?
N10 N11 N12 C6 179.26(18) . . . . ?
N2 N1 C1 N4 -0.3(2) . . . . ?
Mn1 N1 C1 N4 -173.69(13) . . . . ?
N3 N4 C1 N1 0.3(2) . . . . ?
C2 N4 C1 N1 177.97(19) . . . . ?
N5 N6 N7 N8 -0.1(2) . . . . ?
C3 N8 N7 N6 0.5(2) . . . . ?
C4 N8 N7 N6 178.62(19) . . . . ?
N10 N9 C5 N12 0.3(2) . . . . ?
Mn1 N9 C5 N12 -179.88(12) . . . . ?
N11 N12 C5 N9 -0.4(2) . . . . ?
C6 N12 C5 N9 -179.14(19) . . . . ?
C7 N13 N14 N15 0.0(2) . . . . ?
N13 N14 N15 N16 0.4(2) . . . . ?
N14 N15 N16 C7 -0.6(2) . . . . ?
N14 N15 N16 C8 175.0(2) . . . . ?
N14 N13 C7 N16 -0.3(2) . . . . ?
N15 N16 C7 N13 0.6(2) . . . . ?
C8 N16 C7 N13 -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         0.502
_refine_diff_density_min         -0.371
_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_lx352
_database_code_depnum_ccdc_archive 'CCDC 1566378'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jul 19 20:15:10 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakis(1-methyltetrazolyl) bis(cyanodinitromethanido) copper(II)
;
_chemical_name_common            
'tetrakis(1-methyltetrazolyl) bis(cyanodinitromethanido) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Cu N22 O8'
_chemical_formula_sum            'C12 H16 Cu N22 O8'
_chemical_formula_weight         660.01

_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                   8.5663(6)
_cell_length_b                   8.9435(8)
_cell_length_c                   9.9252(9)
_cell_angle_alpha                69.408(9)
_cell_angle_beta                 69.665(7)
_cell_angle_gamma                65.094(8)
_cell_volume                     627.56(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2165
_cell_measurement_theta_min      4.6070
_cell_measurement_theta_max      32.0070

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.959
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86487
_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    1.746
_exptl_crystal_F_000             335
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            4809
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.270
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_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             2459
_reflns_number_gt                2250
_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)+(0.0259P)²+0.3735P] 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         2459
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0710
_refine_ls_wR_factor_gt          0.0681
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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      0.0354018000
_diffrn_orient_matrix_UB_12      0.0528397000
_diffrn_orient_matrix_UB_13      -0.0651801000
_diffrn_orient_matrix_UB_21      -0.0018062000
_diffrn_orient_matrix_UB_22      -0.0472564000
_diffrn_orient_matrix_UB_23      -0.0434424000
_diffrn_orient_matrix_UB_31      -0.0869715000
_diffrn_orient_matrix_UB_32      0.0556254000
_diffrn_orient_matrix_UB_33      -0.0057123000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   27.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
  2 omega   -2.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000   90.0000 41

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega   16.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 80

#__ type_ start__ end____ width___ exp.time_
  5 omega   40.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega   43.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -146.0000    7.0000 58

#__ type_ start__ end____ width___ exp.time_
  7 omega  -99.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -60.0000 91

#__ type_ start__ end____ width___ exp.time_
  8 omega -108.00  -65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -30.0000 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.0000 0.0000 0.01305(11) Uani 1 2 d S . P . .
O1 O -0.10473(18) -0.0131(2) 0.24195(16) 0.0252(3) Uani 1 1 d . . . . .
O2 O -0.30456(17) 0.05186(19) 0.43976(15) 0.0224(3) Uani 1 1 d . . . . .
O3 O -0.24012(17) 0.22817(18) 0.56749(14) 0.0198(3) Uani 1 1 d . . . . .
O4 O -0.00419(18) 0.29687(19) 0.45030(16) 0.0236(3) Uani 1 1 d . . . . .
N1 N 0.6038(2) 0.1589(2) 0.01168(17) 0.0140(3) Uani 1 1 d . . . . .
N2 N 0.5473(2) 0.2316(2) 0.12709(18) 0.0202(4) Uani 1 1 d . . . . .
N3 N 0.6329(2) 0.3314(2) 0.10201(19) 0.0244(4) Uani 1 1 d . . . . .
N4 N 0.7470(2) 0.3239(2) -0.03171(18) 0.0168(3) Uani 1 1 d . . . . .
N5 N -0.1658(2) 0.0584(2) 0.34613(18) 0.0164(3) Uani 1 1 d . . . . .
N6 N -0.1092(2) 0.2278(2) 0.46266(17) 0.0152(3) Uani 1 1 d . . . . .
N7 N 0.2191(2) 0.1359(2) 0.15070(19) 0.0205(4) Uani 1 1 d . . . . .
N8 N 0.41952(19) 0.16976(19) -0.17893(17) 0.0138(3) Uani 1 1 d . . . . .
N9 N 0.3578(2) 0.3400(2) -0.18898(19) 0.0228(4) Uani 1 1 d . . . . .
N11 N 0.3583(2) 0.3054(2) -0.39022(17) 0.0139(3) Uani 1 1 d . . . . .
N10 N 0.3209(2) 0.4223(2) -0.31634(19) 0.0229(4) Uani 1 1 d . . . . .
C1 C 0.7270(3) 0.2186(3) -0.0850(2) 0.0177(4) Uani 1 1 d . . . . .
C2 C 0.8690(3) 0.4202(3) -0.0936(3) 0.0291(5) Uani 1 1 d . . . . .
H2A H 0.9734 0.3573 -0.0515 0.044 Uiso 1 1 calc R U . . .
H2B H 0.8094 0.5312 -0.0692 0.044 Uiso 1 1 calc R U . . .
H2C H 0.9058 0.4364 -0.2014 0.044 Uiso 1 1 calc R U . . .
C3 C -0.0682(2) 0.1473(2) 0.3506(2) 0.0147(4) Uani 1 1 d . . . . .
C4 C 0.0900(2) 0.1432(2) 0.2412(2) 0.0149(4) Uani 1 1 d . . . . .
C5 C 0.4188(2) 0.1519(2) -0.3046(2) 0.0131(4) Uani 1 1 d . . . . .
C6 C 0.3391(3) 0.3555(3) -0.5421(2) 0.0186(4) Uani 1 1 d . . . . .
H6A H 0.4404 0.3878 -0.6105 0.028 Uiso 1 1 calc R U . . .
H6B H 0.2295 0.4524 -0.5521 0.028 Uiso 1 1 calc R U . . .
H6C H 0.3345 0.2601 -0.5657 0.028 Uiso 1 1 calc R U . . .
H5 H 0.456(3) 0.049(3) -0.326(2) 0.015(5) Uiso 1 1 d . . . . .
H1 H 0.787(3) 0.195(3) -0.173(3) 0.025(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 N8 2.0017(16) . ?
Cu1 N8 2.0017(16) 2_655 ?
Cu1 N1 2.0192(16) 2_655 ?
Cu1 N1 2.0192(16) . ?
Cu1 N7 2.4122(16) 2_655 ?
Cu1 N7 2.4122(16) . ?
O1 N5 1.249(2) . ?
O2 N5 1.238(2) . ?
O3 N6 1.236(2) . ?
O4 N6 1.242(2) . ?
N1 C1 1.315(2) . ?
N1 N2 1.357(2) . ?
N2 N3 1.290(2) . ?
N3 N4 1.352(2) . ?
N4 C1 1.322(3) . ?
N4 C2 1.466(2) . ?
N5 C3 1.395(2) . ?
N6 C3 1.399(2) . ?
N7 C4 1.150(2) . ?
N8 C5 1.314(2) . ?
N8 N9 1.364(2) . ?
N9 N10 1.291(2) . ?
N11 C5 1.327(2) . ?
N11 N10 1.352(2) . ?
N11 C6 1.462(2) . ?
C1 H1 0.90(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.407(3) . ?
C5 H5 0.92(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Cu1 N8 180.0 . 2_655 ?
N8 Cu1 N1 91.31(6) . 2_655 ?
N8 Cu1 N1 88.69(6) 2_655 2_655 ?
N8 Cu1 N1 88.69(6) . . ?
N8 Cu1 N1 91.31(6) 2_655 . ?
N1 Cu1 N1 180.00(4) 2_655 . ?
N8 Cu1 N7 91.46(6) . 2_655 ?
N8 Cu1 N7 88.54(6) 2_655 2_655 ?
N1 Cu1 N7 90.72(6) 2_655 2_655 ?
N1 Cu1 N7 89.28(6) . 2_655 ?
N8 Cu1 N7 88.54(6) . . ?
N8 Cu1 N7 91.46(6) 2_655 . ?
N1 Cu1 N7 89.28(6) 2_655 . ?
N1 Cu1 N7 90.72(6) . . ?
N7 Cu1 N7 180.0 2_655 . ?
C1 N1 N2 106.49(16) . . ?
C1 N1 Cu1 129.95(14) . . ?
N2 N1 Cu1 123.51(12) . . ?
N3 N2 N1 109.85(15) . . ?
N2 N3 N4 106.72(16) . . ?
C1 N4 N3 108.44(16) . . ?
C1 N4 C2 130.33(18) . . ?
N3 N4 C2 121.22(17) . . ?
O2 N5 O1 122.48(16) . . ?
O2 N5 C3 121.71(16) . . ?
O1 N5 C3 115.80(15) . . ?
O3 N6 O4 122.52(16) . . ?
O3 N6 C3 122.04(16) . . ?
O4 N6 C3 115.44(15) . . ?
C4 N7 Cu1 156.41(15) . . ?
C5 N8 N9 106.76(15) . . ?
C5 N8 Cu1 131.84(13) . . ?
N9 N8 Cu1 121.33(12) . . ?
N10 N9 N8 109.49(16) . . ?
C5 N11 N10 108.46(16) . . ?
C5 N11 C6 130.05(17) . . ?
N10 N11 C6 121.40(16) . . ?
N9 N10 N11 106.99(16) . . ?
N1 C1 N4 108.49(17) . . ?
N1 C1 H1 126.9(15) . . ?
N4 C1 H1 124.6(15) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N6 124.46(16) . . ?
N5 C3 C4 117.22(17) . . ?
N6 C3 C4 118.11(17) . . ?
N7 C4 C3 178.0(2) . . ?
N8 C5 N11 108.29(17) . . ?
N8 C5 H5 123.8(13) . . ?
N11 C5 H5 127.9(13) . . ?
N11 C6 H6A 109.5 . . ?
N11 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N11 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.1(2) . . . . ?
Cu1 N1 N2 N3 -177.68(13) . . . . ?
N1 N2 N3 N4 0.0(2) . . . . ?
N2 N3 N4 C1 0.1(2) . . . . ?
N2 N3 N4 C2 -178.63(18) . . . . ?
C5 N8 N9 N10 0.0(2) . . . . ?
Cu1 N8 N9 N10 177.55(12) . . . . ?
N8 N9 N10 N11 0.1(2) . . . . ?
C5 N11 N10 N9 -0.3(2) . . . . ?
C6 N11 N10 N9 -177.25(16) . . . . ?
N2 N1 C1 N4 0.2(2) . . . . ?
Cu1 N1 C1 N4 177.53(13) . . . . ?
N3 N4 C1 N1 -0.2(2) . . . . ?
C2 N4 C1 N1 178.38(19) . . . . ?
O2 N5 C3 N6 3.8(3) . . . . ?
O1 N5 C3 N6 -176.36(17) . . . . ?
O2 N5 C3 C4 178.40(17) . . . . ?
O1 N5 C3 C4 -1.8(2) . . . . ?
O3 N6 C3 N5 -1.2(3) . . . . ?
O4 N6 C3 N5 178.08(16) . . . . ?
O3 N6 C3 C4 -175.68(17) . . . . ?
O4 N6 C3 C4 3.6(2) . . . . ?
N9 N8 C5 N11 -0.18(19) . . . . ?
Cu1 N8 C5 N11 -177.35(12) . . . . ?
N10 N11 C5 N8 0.3(2) . . . . ?
C6 N11 C5 N8 176.92(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
? ? ? ? ? ? ? ?

_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         -0.362
_refine_diff_density_rms         0.061

_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_lx166
_database_code_depnum_ccdc_archive 'CCDC 1566370'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Apr 01 07:30:57 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl)manganese(II) perchlorate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl)manganese(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C12 H24 Mn N24, 2(Cl O4)'
_chemical_formula_sum            'C12 H24 Cl2 Mn N24 O8'
_chemical_formula_weight         758.39

_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'"

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_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                   18.0701(11)
_cell_length_b                   10.2773(4)
_cell_length_c                   18.7841(9)
_cell_angle_alpha                90
_cell_angle_beta                 114.147(7)
_cell_angle_gamma                90
_cell_volume                     3183.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5810
_cell_measurement_theta_min      4.5330
_cell_measurement_theta_max      30.7610

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.661
_shelx_estimated_absorpt_T_min   0.778
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78635
_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    1.582
_exptl_crystal_F_000             1548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            26034
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.140
_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             6239
_reflns_number_gt                4638
_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)+(0.0559P)²+1.8485P] 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         6239
_refine_ls_number_parameters     551
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.012
_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      -0.0403906000
_diffrn_orient_matrix_UB_12      -0.0231446000
_diffrn_orient_matrix_UB_13      -0.0125759000
_diffrn_orient_matrix_UB_21      0.0020738000
_diffrn_orient_matrix_UB_22      0.0085885000
_diffrn_orient_matrix_UB_23      0.0382270000
_diffrn_orient_matrix_UB_31      -0.0147644000
_diffrn_orient_matrix_UB_32      0.0644101000
_diffrn_orient_matrix_UB_33      -0.0095946000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -51.00  -20.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   57.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega  -35.00   13.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   57.0000 -180.0000 48

#__ type_ start__ end____ width___ exp.time_
  3 omega  -77.00  -48.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432 -179.0000  150.0000 29

#__ type_ start__ end____ width___ exp.time_
  4 omega  -76.00    5.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432  108.0000  157.0000 81

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   74.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.6369  -99.0000  -30.0000 99

#__ type_ start__ end____ width___ exp.time_
  6 omega    1.00  101.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.6369   77.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
  7 omega  -25.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.6369   19.0000   90.0000 130

;



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 0.5000 0.5000 0.5000 0.04024(18) Uani 1 2 d S . P . .
N1 N 0.56667(16) 0.3708(2) 0.60357(14) 0.0413(6) Uani 1 1 d . . . . .
N2 N 0.61883(18) 0.2772(3) 0.60299(15) 0.0518(7) Uani 1 1 d . . . . .
N3 N 0.64841(19) 0.2173(3) 0.66913(17) 0.0608(8) Uani 1 1 d . . . . .
N4 N 0.61587(15) 0.2731(2) 0.71409(14) 0.0400(6) Uani 1 1 d . . . . .
N5 N 0.42504(17) 0.3271(2) 0.43755(14) 0.0447(6) Uani 1 1 d . . . . .
N6 N 0.3795(2) 0.3233(3) 0.36023(15) 0.0616(8) Uani 1 1 d . . . . .
N7 N 0.3337(2) 0.2218(3) 0.34246(15) 0.0611(8) Uani 1 1 d . . . . .
N8 N 0.34938(16) 0.1575(2) 0.40912(14) 0.0401(6) Uani 1 1 d . . . . .
N9 N 0.41123(17) 0.5425(2) 0.55375(14) 0.0423(6) Uani 1 1 d . . . . .
N10 N 0.35675(18) 0.4535(2) 0.55660(16) 0.0499(7) Uani 1 1 d . . . . .
N11 N 0.31702(17) 0.5004(2) 0.59434(17) 0.0475(7) Uani 1 1 d . . . . .
N12 N 0.34441(14) 0.6217(2) 0.61542(13) 0.0336(5) Uani 1 1 d . . . . .
C1 C 0.5661(2) 0.3648(3) 0.67301(19) 0.0475(8) Uani 1 1 d . . . . .
C2 C 0.6322(3) 0.2228(4) 0.7921(2) 0.0551(9) Uani 1 1 d . . . . .
C3 C 0.4048(2) 0.2229(3) 0.4655(2) 0.0506(8) Uani 1 1 d . . . . .
C4 C 0.3060(3) 0.0376(4) 0.4100(3) 0.0543(9) Uani 1 1 d . . . . .
C5 C 0.4018(2) 0.6448(3) 0.59069(18) 0.0415(7) Uani 1 1 d . . . . .
C6 C 0.3136(2) 0.7022(3) 0.6613(2) 0.0411(7) Uani 1 1 d . . . . .
Mn2 Mn 0.0000 0.5000 0.5000 0.02474(15) Uani 1 2 d S . P . .
N13 N 0.07275(13) 0.62086(19) 0.45422(12) 0.0280(5) Uani 1 1 d . . . . .
N14 N 0.13882(15) 0.6909(2) 0.49985(13) 0.0379(6) Uani 1 1 d . . . . .
N15 N 0.17930(16) 0.7263(2) 0.46030(14) 0.0439(6) Uani 1 1 d . . . . .
N16 N 0.13893(14) 0.6800(2) 0.38762(13) 0.0333(5) Uani 1 1 d . . . . .
N17 N 0.08400(13) 0.55178(19) 0.62539(12) 0.0278(5) Uani 1 1 d . . . . .
N18 N 0.14270(14) 0.4702(2) 0.67358(12) 0.0327(5) Uani 1 1 d . . . . .
N19 N 0.18782(14) 0.5296(2) 0.73686(13) 0.0329(5) Uani 1 1 d . . . . .
N20 N 0.15885(13) 0.65222(19) 0.73043(12) 0.0278(5) Uani 1 1 d . . . . .
N21 N -0.07787(13) 0.67214(19) 0.49813(12) 0.0287(5) Uani 1 1 d . . . . .
N22 N -0.12951(15) 0.6746(2) 0.53447(14) 0.0371(6) Uani 1 1 d . . . . .
N23 N -0.16957(15) 0.7829(2) 0.51910(14) 0.0386(6) Uani 1 1 d . . . . .
N24 N -0.14425(14) 0.8513(2) 0.47199(12) 0.0312(5) Uani 1 1 d . . . . .
C7 C 0.07471(18) 0.6170(3) 0.38538(16) 0.0326(6) Uani 1 1 d . . . . .
C8 C 0.1664(3) 0.7048(5) 0.3259(2) 0.0554(9) Uani 1 1 d . . . . .
C9 C 0.09581(17) 0.6631(2) 0.66275(15) 0.0293(6) Uani 1 1 d . . . . .
C10 C 0.1951(2) 0.7477(3) 0.79351(18) 0.0405(7) Uani 1 1 d . . . . .
C11 C -0.08859(17) 0.7827(2) 0.46018(15) 0.0309(6) Uani 1 1 d . . . . .
C12 C -0.1738(2) 0.9835(3) 0.4466(2) 0.0458(8) Uani 1 1 d . . . . .
Cl1 Cl 0.45381(5) 0.00621(7) 0.64933(5) 0.0444(2) Uani 1 1 d . . . . .
O1A O 0.5100(4) 0.0520(8) 0.6184(4) 0.062(2) Uani 0.421(7) 1 d . . P A 1
O2A O 0.4655(6) -0.0344(9) 0.7197(4) 0.082(3) Uani 0.421(7) 1 d . . P A 1
O3A O 0.4703(4) 0.0825(9) 0.7205(5) 0.088(3) Uani 0.421(7) 1 d . . P A 1
O1B O 0.4946(5) -0.0385(8) 0.6073(5) 0.130(3) Uani 0.579(7) 1 d . . P A 2
O2B O 0.4883(5) -0.1088(9) 0.6942(5) 0.147(4) Uani 0.579(7) 1 d . . P A 2
O3C O 0.4524(3) 0.1459(4) 0.6484(3) 0.0666(18) Uani 0.579(7) 1 d . . P A 2
O4 O 0.37253(19) -0.0226(3) 0.59976(17) 0.0879(10) Uani 1 1 d . . . . .
Cl2 Cl 0.49832(4) 0.48454(6) 0.16608(4) 0.03444(17) Uani 1 1 d . . . . .
O5 O 0.51063(15) 0.5471(2) 0.10373(12) 0.0528(6) Uani 1 1 d . . . . .
O6 O 0.52639(15) 0.3531(2) 0.17311(13) 0.0557(6) Uani 1 1 d . . . . .
O7 O 0.41270(15) 0.4850(2) 0.14906(15) 0.0617(7) Uani 1 1 d . . . . .
O8 O 0.54144(14) 0.5527(2) 0.23741(13) 0.0549(6) Uani 1 1 d . . . . .
H11 H -0.0627(16) 0.810(2) 0.4286(15) 0.026(7) Uiso 1 1 d . . . . .
H9 H 0.0683(17) 0.739(3) 0.6471(16) 0.034(7) Uiso 1 1 d . . . . .
H5 H 0.4345(19) 0.716(3) 0.6005(17) 0.044(9) Uiso 1 1 d . . . . .
H7 H 0.036(2) 0.582(3) 0.342(2) 0.050(9) Uiso 1 1 d . . . . .
H1 H 0.536(2) 0.411(3) 0.690(2) 0.062(11) Uiso 1 1 d . . . . .
H10B H 0.1876(19) 0.719(3) 0.840(2) 0.048(9) Uiso 1 1 d . . . . .
H10A H 0.254(2) 0.756(3) 0.8055(19) 0.050(9) Uiso 1 1 d . . . . .
H10C H 0.170(2) 0.827(3) 0.776(2) 0.057(10) Uiso 1 1 d . . . . .
H6C H 0.323(2) 0.667(4) 0.710(3) 0.079(13) Uiso 1 1 d . . . . .
H6A H 0.259(2) 0.711(3) 0.632(2) 0.057(10) Uiso 1 1 d . . . . .
H6B H 0.339(3) 0.784(4) 0.669(2) 0.079(13) Uiso 1 1 d . . . . .
H12B H -0.160(3) 1.033(4) 0.488(3) 0.077(13) Uiso 1 1 d . . . . .
H12A H -0.170(3) 1.007(4) 0.403(3) 0.106(18) Uiso 1 1 d . . . . .
H2B H 0.680(3) 0.173(4) 0.810(2) 0.078(13) Uiso 1 1 d . . . . .
H12C H -0.233(3) 0.979(4) 0.420(3) 0.094(15) Uiso 1 1 d . . . . .
H2A H 0.584(3) 0.173(4) 0.788(3) 0.104(16) Uiso 1 1 d . . . . .
H2C H 0.637(2) 0.291(4) 0.826(2) 0.072(12) Uiso 1 1 d . . . . .
H4C H 0.333(3) -0.012(4) 0.443(3) 0.092(17) Uiso 1 1 d . . . . .
H4B H 0.292(3) -0.001(4) 0.361(3) 0.083(14) Uiso 1 1 d . . . . .
H8C H 0.166(3) 0.791(4) 0.316(2) 0.080(14) Uiso 1 1 d . . . . .
H3 H 0.428(3) 0.196(4) 0.518(3) 0.098(15) Uiso 1 1 d . . . . .
H8B H 0.135(3) 0.663(4) 0.284(3) 0.090(15) Uiso 1 1 d . . . . .
H8A H 0.224(4) 0.664(6) 0.344(3) 0.15(2) Uiso 1 1 d . . . . .
H4A H 0.253(3) 0.055(4) 0.416(2) 0.083(13) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N5 2.252(3) 3_666 ?
Mn1 N5 2.252(3) . ?
Mn1 N1 2.254(2) 3_666 ?
Mn1 N1 2.254(2) . ?
Mn1 N9 2.260(2) . ?
Mn1 N9 2.260(2) 3_666 ?
N1 C1 1.310(4) . ?
N1 N2 1.350(3) . ?
N2 N3 1.290(4) . ?
N3 N4 1.339(3) . ?
N4 C1 1.313(4) . ?
N4 C2 1.464(4) . ?
N5 C3 1.309(4) . ?
N5 N6 1.345(4) . ?
N6 N7 1.288(4) . ?
N7 N8 1.340(3) . ?
N8 C3 1.307(4) . ?
N8 C4 1.464(4) . ?
N9 C5 1.309(4) . ?
N9 N10 1.361(4) . ?
N10 N11 1.291(4) . ?
N11 N12 1.339(3) . ?
N12 C5 1.320(4) . ?
N12 C6 1.459(4) . ?
C1 H1 0.87(4) . ?
C2 H2B 0.94(4) . ?
C2 H2A 0.99(5) . ?
C2 H2C 0.92(4) . ?
C3 H3 0.94(4) . ?
C4 H4C 0.79(5) . ?
C4 H4B 0.93(5) . ?
C4 H4A 1.02(5) . ?
C5 H5 0.91(3) . ?
C6 H6C 0.94(4) . ?
C6 H6A 0.93(4) . ?
C6 H6B 0.94(4) . ?
Mn2 N13 2.222(2) . ?
Mn2 N13 2.222(2) 3_566 ?
Mn2 N21 2.252(2) 3_566 ?
Mn2 N21 2.252(2) . ?
Mn2 N17 2.282(2) . ?
Mn2 N17 2.282(2) 3_566 ?
N13 C7 1.309(3) . ?
N13 N14 1.357(3) . ?
N14 N15 1.290(3) . ?
N15 N16 1.345(3) . ?
N16 C7 1.314(4) . ?
N16 C8 1.457(4) . ?
N17 C9 1.313(3) . ?
N17 N18 1.365(3) . ?
N18 N19 1.288(3) . ?
N19 N20 1.351(3) . ?
N20 C9 1.320(3) . ?
N20 C10 1.470(3) . ?
N21 C11 1.313(3) . ?
N21 N22 1.363(3) . ?
N22 N23 1.295(3) . ?
N23 N24 1.348(3) . ?
N24 C11 1.319(3) . ?
N24 C12 1.466(4) . ?
C7 H7 0.90(3) . ?
C8 H8C 0.91(4) . ?
C8 H8B 0.88(5) . ?
C8 H8A 1.04(7) . ?
C9 H9 0.91(3) . ?
C10 H10B 0.97(3) . ?
C10 H10A 0.99(4) . ?
C10 H10C 0.92(4) . ?
C11 H11 0.94(3) . ?
C12 H12B 0.88(4) . ?
C12 H12A 0.89(6) . ?
C12 H12C 0.97(5) . ?
Cl1 O2A 1.318(7) . ?
Cl1 O1B 1.360(5) . ?
Cl1 O4 1.412(3) . ?
Cl1 O3C 1.436(4) . ?
Cl1 O2B 1.438(7) . ?
Cl1 O1A 1.439(6) . ?
Cl1 O3A 1.472(6) . ?
O2A O3A 1.204(12) . ?
Cl2 O8 1.428(2) . ?
Cl2 O6 1.430(2) . ?
Cl2 O5 1.431(2) . ?
Cl2 O7 1.446(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
N5 Mn1 N5 180.0 3_666 . ?
N5 Mn1 N1 88.85(9) 3_666 3_666 ?
N5 Mn1 N1 91.15(9) . 3_666 ?
N5 Mn1 N1 91.15(9) 3_666 . ?
N5 Mn1 N1 88.85(9) . . ?
N1 Mn1 N1 180.0 3_666 . ?
N5 Mn1 N9 90.03(9) 3_666 . ?
N5 Mn1 N9 89.97(9) . . ?
N1 Mn1 N9 92.60(9) 3_666 . ?
N1 Mn1 N9 87.40(9) . . ?
N5 Mn1 N9 89.97(9) 3_666 3_666 ?
N5 Mn1 N9 90.03(9) . 3_666 ?
N1 Mn1 N9 87.40(9) 3_666 3_666 ?
N1 Mn1 N9 92.60(9) . 3_666 ?
N9 Mn1 N9 180.00(9) . 3_666 ?
C1 N1 N2 105.3(3) . . ?
C1 N1 Mn1 131.9(2) . . ?
N2 N1 Mn1 122.76(18) . . ?
N3 N2 N1 110.3(2) . . ?
N2 N3 N4 106.7(3) . . ?
C1 N4 N3 107.9(2) . . ?
C1 N4 C2 130.6(3) . . ?
N3 N4 C2 121.3(3) . . ?
C3 N5 N6 105.2(3) . . ?
C3 N5 Mn1 130.1(2) . . ?
N6 N5 Mn1 123.8(2) . . ?
N7 N6 N5 110.3(3) . . ?
N6 N7 N8 106.8(3) . . ?
C3 N8 N7 107.7(3) . . ?
C3 N8 C4 131.2(3) . . ?
N7 N8 C4 121.1(3) . . ?
C5 N9 N10 105.5(2) . . ?
C5 N9 Mn1 131.4(2) . . ?
N10 N9 Mn1 123.02(18) . . ?
N11 N10 N9 110.1(2) . . ?
N10 N11 N12 106.8(2) . . ?
C5 N12 N11 108.2(2) . . ?
C5 N12 C6 130.5(3) . . ?
N11 N12 C6 121.2(2) . . ?
N1 C1 N4 109.7(3) . . ?
N1 C1 H1 127(2) . . ?
N4 C1 H1 124(2) . . ?
N4 C2 H2B 110(2) . . ?
N4 C2 H2A 107(3) . . ?
H2B C2 H2A 113(4) . . ?
N4 C2 H2C 110(2) . . ?
H2B C2 H2C 111(4) . . ?
H2A C2 H2C 106(4) . . ?
N8 C3 N5 110.0(3) . . ?
N8 C3 H3 125(3) . . ?
N5 C3 H3 125(3) . . ?
N8 C4 H4C 113(4) . . ?
N8 C4 H4B 106(3) . . ?
H4C C4 H4B 108(4) . . ?
N8 C4 H4A 113(2) . . ?
H4C C4 H4A 110(4) . . ?
H4B C4 H4A 107(4) . . ?
N9 C5 N12 109.4(3) . . ?
N9 C5 H5 123(2) . . ?
N12 C5 H5 127.6(19) . . ?
N12 C6 H6C 114(2) . . ?
N12 C6 H6A 106(2) . . ?
H6C C6 H6A 110(3) . . ?
N12 C6 H6B 109(2) . . ?
H6C C6 H6B 108(3) . . ?
H6A C6 H6B 110(3) . . ?
N13 Mn2 N13 180.0 . 3_566 ?
N13 Mn2 N21 88.87(7) . 3_566 ?
N13 Mn2 N21 91.13(7) 3_566 3_566 ?
N13 Mn2 N21 91.13(7) . . ?
N13 Mn2 N21 88.87(7) 3_566 . ?
N21 Mn2 N21 180.0 3_566 . ?
N13 Mn2 N17 91.15(7) . . ?
N13 Mn2 N17 88.85(7) 3_566 . ?
N21 Mn2 N17 91.12(7) 3_566 . ?
N21 Mn2 N17 88.88(7) . . ?
N13 Mn2 N17 88.85(7) . 3_566 ?
N13 Mn2 N17 91.15(7) 3_566 3_566 ?
N21 Mn2 N17 88.88(7) 3_566 3_566 ?
N21 Mn2 N17 91.12(7) . 3_566 ?
N17 Mn2 N17 180.0 . 3_566 ?
C7 N13 N14 105.5(2) . . ?
C7 N13 Mn2 128.68(18) . . ?
N14 N13 Mn2 124.00(16) . . ?
N15 N14 N13 110.2(2) . . ?
N14 N15 N16 106.5(2) . . ?
C7 N16 N15 108.2(2) . . ?
C7 N16 C8 130.1(3) . . ?
N15 N16 C8 121.7(3) . . ?
C9 N17 N18 105.6(2) . . ?
C9 N17 Mn2 130.44(17) . . ?
N18 N17 Mn2 123.33(15) . . ?
N19 N18 N17 110.3(2) . . ?
N18 N19 N20 106.5(2) . . ?
C9 N20 N19 108.4(2) . . ?
C9 N20 C10 130.1(2) . . ?
N19 N20 C10 121.5(2) . . ?
C11 N21 N22 106.1(2) . . ?
C11 N21 Mn2 129.86(18) . . ?
N22 N21 Mn2 123.92(15) . . ?
N23 N22 N21 109.8(2) . . ?
N22 N23 N24 106.6(2) . . ?
C11 N24 N23 108.6(2) . . ?
C11 N24 C12 129.9(3) . . ?
N23 N24 C12 121.3(3) . . ?
N13 C7 N16 109.5(2) . . ?
N13 C7 H7 125(2) . . ?
N16 C7 H7 125(2) . . ?
N16 C8 H8C 112(3) . . ?
N16 C8 H8B 109(3) . . ?
H8C C8 H8B 110(4) . . ?
N16 C8 H8A 107(3) . . ?
H8C C8 H8A 112(4) . . ?
H8B C8 H8A 107(4) . . ?
N17 C9 N20 109.2(2) . . ?
N17 C9 H9 129.0(18) . . ?
N20 C9 H9 121.9(18) . . ?
N20 C10 H10B 109.8(19) . . ?
N20 C10 H10A 108.9(19) . . ?
H10B C10 H10A 110(3) . . ?
N20 C10 H10C 108(2) . . ?
H10B C10 H10C 111(3) . . ?
H10A C10 H10C 109(3) . . ?
N21 C11 N24 108.9(2) . . ?
N21 C11 H11 127.1(16) . . ?
N24 C11 H11 124.0(16) . . ?
N24 C12 H12B 109(3) . . ?
N24 C12 H12A 114(3) . . ?
H12B C12 H12A 124(4) . . ?
N24 C12 H12C 108(3) . . ?
H12B C12 H12C 110(4) . . ?
H12A C12 H12C 91(4) . . ?
O2A Cl1 O4 106.9(5) . . ?
O1B Cl1 O4 102.2(4) . . ?
O1B Cl1 O3C 110.0(4) . . ?
O4 Cl1 O3C 101.1(2) . . ?
O1B Cl1 O2B 81.6(7) . . ?
O4 Cl1 O2B 107.4(3) . . ?
O3C Cl1 O2B 146.2(4) . . ?
O2A Cl1 O1A 131.2(5) . . ?
O4 Cl1 O1A 121.2(3) . . ?
O2A Cl1 O3A 50.8(5) . . ?
O4 Cl1 O3A 118.7(3) . . ?
O1A Cl1 O3A 106.1(4) . . ?
O3A O2A Cl1 71.2(5) . . ?
O2A O3A Cl1 58.0(4) . . ?
O8 Cl2 O6 109.87(15) . . ?
O8 Cl2 O5 109.87(14) . . ?
O6 Cl2 O5 109.39(14) . . ?
O8 Cl2 O7 109.26(15) . . ?
O6 Cl2 O7 109.29(15) . . ?
O5 Cl2 O7 109.15(15) . . ?

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 0.0(4) . . . . ?
Mn1 N1 N2 N3 -179.8(2) . . . . ?
N1 N2 N3 N4 -0.6(4) . . . . ?
N2 N3 N4 C1 0.9(4) . . . . ?
N2 N3 N4 C2 175.8(3) . . . . ?
C3 N5 N6 N7 0.3(4) . . . . ?
Mn1 N5 N6 N7 -169.9(2) . . . . ?
N5 N6 N7 N8 -0.1(4) . . . . ?
N6 N7 N8 C3 -0.1(4) . . . . ?
N6 N7 N8 C4 178.8(3) . . . . ?
C5 N9 N10 N11 -0.6(4) . . . . ?
Mn1 N9 N10 N11 176.2(2) . . . . ?
N9 N10 N11 N12 1.0(3) . . . . ?
N10 N11 N12 C5 -1.0(3) . . . . ?
N10 N11 N12 C6 -178.3(3) . . . . ?
N2 N1 C1 N4 0.6(4) . . . . ?
Mn1 N1 C1 N4 -179.7(2) . . . . ?
N3 N4 C1 N1 -0.9(4) . . . . ?
C2 N4 C1 N1 -175.2(3) . . . . ?
N7 N8 C3 N5 0.3(4) . . . . ?
C4 N8 C3 N5 -178.4(3) . . . . ?
N6 N5 C3 N8 -0.3(4) . . . . ?
Mn1 N5 C3 N8 169.0(2) . . . . ?
N10 N9 C5 N12 -0.1(3) . . . . ?
Mn1 N9 C5 N12 -176.48(19) . . . . ?
N11 N12 C5 N9 0.7(4) . . . . ?
C6 N12 C5 N9 177.6(3) . . . . ?
C7 N13 N14 N15 -0.7(3) . . . . ?
Mn2 N13 N14 N15 165.23(18) . . . . ?
N13 N14 N15 N16 0.5(3) . . . . ?
N14 N15 N16 C7 -0.1(3) . . . . ?
N14 N15 N16 C8 178.3(3) . . . . ?
C9 N17 N18 N19 -0.1(3) . . . . ?
Mn2 N17 N18 N19 171.55(17) . . . . ?
N17 N18 N19 N20 -0.2(3) . . . . ?
N18 N19 N20 C9 0.5(3) . . . . ?
N18 N19 N20 C10 178.7(3) . . . . ?
C11 N21 N22 N23 -0.2(3) . . . . ?
Mn2 N21 N22 N23 -176.03(17) . . . . ?
N21 N22 N23 N24 0.4(3) . . . . ?
N22 N23 N24 C11 -0.4(3) . . . . ?
N22 N23 N24 C12 -176.4(3) . . . . ?
N14 N13 C7 N16 0.6(3) . . . . ?
Mn2 N13 C7 N16 -164.43(17) . . . . ?
N15 N16 C7 N13 -0.3(3) . . . . ?
C8 N16 C7 N13 -178.6(3) . . . . ?
N18 N17 C9 N20 0.4(3) . . . . ?
Mn2 N17 C9 N20 -170.44(17) . . . . ?
N19 N20 C9 N17 -0.6(3) . . . . ?
C10 N20 C9 N17 -178.6(3) . . . . ?
N22 N21 C11 N24 -0.1(3) . . . . ?
Mn2 N21 C11 N24 175.42(16) . . . . ?
N23 N24 C11 N21 0.3(3) . . . . ?
C12 N24 C11 N21 175.8(3) . . . . ?
O1B Cl1 O2A O3A 127.7(7) . . . . ?
O4 Cl1 O2A O3A -113.5(5) . . . . ?
O3C Cl1 O2A O3A -5.0(7) . . . . ?
O2B Cl1 O2A O3A 148.5(11) . . . . ?
O1A Cl1 O2A O3A 76.3(10) . . . . ?
O1B Cl1 O3A O2A -101.0(10) . . . . ?
O4 Cl1 O3A O2A 89.0(7) . . . . ?
O3C Cl1 O3A O2A 174.4(8) . . . . ?
O2B Cl1 O3A O2A -21.9(8) . . . . ?
O1A Cl1 O3A O2A -130.4(7) . . . . ?

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         0.611
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4


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

data_lx150
_database_code_depnum_ccdc_archive 'CCDC 1566363'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Mar 22 08:47:49 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl)nickel(II) diperchlorate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl)nickel(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 N24 Ni, 2(Cl O4)'
_chemical_formula_sum            'C12 H24 Cl2 N24 Ni O8'
_chemical_formula_weight         762.16

_symmetry_cell_setting           TRIGONAL
_symmetry_space_group_name_H-M   'R -3'
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 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+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.4382(11)
_cell_length_b                   19.4382(11)
_cell_length_c                   21.3656(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6991.3(9)
_cell_formula_units_Z            9
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1675
_cell_measurement_theta_min      4.4830
_cell_measurement_theta_max      22.4680

_exptl_crystal_description       rod
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.877
_shelx_estimated_absorpt_T_min   0.910
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78888
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_F_000             3510
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            21514
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_av_R_equivalents  0.1234
_diffrn_reflns_av_sigmaI/netI    0.2501
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.194
_diffrn_reflns_theta_max         25.992
_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             3052
_reflns_number_gt                1972
_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)+(0.0284P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3052
_refine_ls_number_parameters     216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_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      -0.0415112000
_diffrn_orient_matrix_UB_12      -0.0156130000
_diffrn_orient_matrix_UB_13      0.0033166000
_diffrn_orient_matrix_UB_21      0.0065210000
_diffrn_orient_matrix_UB_22      0.0202148000
_diffrn_orient_matrix_UB_23      0.0289480000
_diffrn_orient_matrix_UB_31      0.0032019000
_diffrn_orient_matrix_UB_32      0.0334948000
_diffrn_orient_matrix_UB_33      -0.0159086000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   18.00   43.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   38.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega    8.00   34.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   57.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega  -12.00   19.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   19.0000   30.0000 31

#__ type_ start__ end____ width___ exp.time_
  4 omega  -95.00  -20.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   19.0000   30.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega -100.00  -25.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432  -38.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
  6 omega  -91.00  -65.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432 -179.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega -111.00  -32.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432  179.0000  -60.0000 79

#__ type_ start__ end____ width___ exp.time_
  8 omega  -47.00  -21.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   57.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega    6.00   32.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   57.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega  -53.00  -28.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.5432   38.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   17.00   74.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.6369  -99.0000  -90.0000 57

#__ type_ start__ end____ width___ exp.time_
 12 omega  -11.00   74.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.6369  -99.0000  150.0000 85

;



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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'


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
Ni1 Ni 0.3333 0.6667 0.1667 0.0151(3) Uani 1 6 d S T P . .
N1 N 0.24922(14) 0.57347(15) 0.11194(13) 0.0165(6) Uani 1 1 d . . . . .
N2 N 0.18989(15) 0.57756(15) 0.08108(14) 0.0204(7) Uani 1 1 d . . . . .
N3 N 0.14016(15) 0.50896(15) 0.05823(14) 0.0220(7) Uani 1 1 d . . . . .
N4 N 0.16642(14) 0.45907(15) 0.07438(13) 0.0187(7) Uani 1 1 d . . . . .
C1 C 0.23327(17) 0.49934(17) 0.10652(16) 0.0173(8) Uani 1 1 d . . . . .
H1 H 0.2644 0.4784 0.1229 0.021 Uiso 1 1 calc R U . . .
C2 C 0.12285(19) 0.37407(18) 0.05873(19) 0.0293(9) Uani 1 1 d . . . . .
H21 H 0.0738 0.3475 0.0833 0.044 Uiso 1 1 calc R U . . .
H22 H 0.1559 0.3505 0.0684 0.044 Uiso 1 1 calc R U . . .
H23 H 0.1098 0.3676 0.0140 0.044 Uiso 1 1 calc R U . . .
Ni2 Ni 0.0000 0.0000 0.19138(4) 0.0178(2) Uani 1 3 d S T P . .
N5 N 0.08711(15) 0.09037(15) 0.24623(13) 0.0185(6) Uani 1 1 d . . . . .
N6 N 0.14283(15) 0.07937(15) 0.27578(14) 0.0226(7) Uani 1 1 d . . . . .
N7 N 0.19396(15) 0.14417(15) 0.30363(14) 0.0230(7) Uani 1 1 d . . . . .
N8 N 0.17102(14) 0.19826(15) 0.29266(14) 0.0191(7) Uani 1 1 d . . . . .
N9 N -0.00816(14) 0.08402(15) 0.13553(14) 0.0201(7) Uani 1 1 d . . . . .
N10 N 0.05351(16) 0.14227(16) 0.10293(15) 0.0278(8) Uani 1 1 d . . . . .
N11 N 0.02932(16) 0.18133(16) 0.06969(15) 0.0302(8) Uani 1 1 d . . . . .
N12 N -0.04942(16) 0.14808(15) 0.08048(14) 0.0217(7) Uani 1 1 d . . . . .
C4 C 0.21599(19) 0.27803(18) 0.31791(19) 0.0295(9) Uani 1 1 d . . . . .
H41 H 0.1925 0.2808 0.3578 0.044 Uiso 1 1 calc R U . . .
H42 H 0.2147 0.3158 0.2883 0.044 Uiso 1 1 calc R U . . .
H43 H 0.2712 0.2914 0.3247 0.044 Uiso 1 1 calc R U . . .
C3 C 0.10596(18) 0.16460(18) 0.25752(16) 0.0184(8) Uani 1 1 d . . . . .
H3 H 0.0777 0.1897 0.2430 0.022 Uiso 1 1 calc R U . . .
C5 C -0.07074(19) 0.08968(19) 0.12060(17) 0.0204(8) Uani 1 1 d . . . . .
H5 H -0.1230 0.0568 0.1363 0.024 Uiso 1 1 calc R U . . .
C6 C -0.0969(2) 0.1783(2) 0.05112(19) 0.0324(10) Uani 1 1 d . . . . .
H62 H -0.0902 0.2247 0.0744 0.049 Uiso 1 1 calc R U . . .
H61 H -0.1530 0.1369 0.0515 0.049 Uiso 1 1 calc R U . . .
H63 H -0.0793 0.1937 0.0078 0.049 Uiso 1 1 calc R U . . .
Cl1 Cl 0.31588(5) 0.31729(5) 0.12991(5) 0.0303(2) Uani 1 1 d . . . . .
O1 O 0.27556(19) 0.26122(17) 0.17871(14) 0.0614(9) Uani 1 1 d . . . . .
O2 O 0.3042(2) 0.38321(17) 0.13701(16) 0.0693(10) Uani 1 1 d . . . . .
O3 O 0.39837(16) 0.34428(19) 0.13323(17) 0.0672(10) Uani 1 1 d . . . . .
O4 O 0.28562(16) 0.27994(15) 0.07121(13) 0.0474(8) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.088(3) 2_665 ?
Ni1 N1 2.088(3) . ?
Ni1 N1 2.088(3) 15 ?
Ni1 N1 2.088(3) 3_565 ?
Ni1 N1 2.088(3) 13_565 ?
Ni1 N1 2.088(3) 14_455 ?
N1 C1 1.319(4) . ?
N1 N2 1.365(3) . ?
N2 N3 1.289(3) . ?
N3 N4 1.347(3) . ?
N4 C1 1.325(4) . ?
N4 C2 1.470(4) . ?
C1 H1 0.9500 . ?
C2 H21 0.9800 . ?
C2 H22 0.9800 . ?
C2 H23 0.9800 . ?
Ni2 N5 2.086(3) . ?
Ni2 N5 2.086(3) 3 ?
Ni2 N5 2.086(3) 2 ?
Ni2 N9 2.092(3) 2 ?
Ni2 N9 2.092(3) 3 ?
Ni2 N9 2.092(3) . ?
N5 C3 1.321(4) . ?
N5 N6 1.360(3) . ?
N6 N7 1.295(4) . ?
N7 N8 1.352(3) . ?
N8 C3 1.328(4) . ?
N8 C4 1.451(4) . ?
N9 C5 1.314(4) . ?
N9 N10 1.359(4) . ?
N10 N11 1.288(4) . ?
N11 N12 1.351(4) . ?
N12 C5 1.313(4) . ?
N12 C6 1.461(4) . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C6 H62 0.9800 . ?
C6 H61 0.9800 . ?
C6 H63 0.9800 . ?
Cl1 O2 1.417(3) . ?
Cl1 O3 1.418(3) . ?
Cl1 O4 1.421(3) . ?
Cl1 O1 1.427(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 91.70(10) 2_665 . ?
N1 Ni1 N1 88.30(10) 2_665 15 ?
N1 Ni1 N1 88.30(10) . 15 ?
N1 Ni1 N1 91.70(10) 2_665 3_565 ?
N1 Ni1 N1 91.70(10) . 3_565 ?
N1 Ni1 N1 180.0 15 3_565 ?
N1 Ni1 N1 88.30(10) 2_665 13_565 ?
N1 Ni1 N1 180.00(13) . 13_565 ?
N1 Ni1 N1 91.70(10) 15 13_565 ?
N1 Ni1 N1 88.30(10) 3_565 13_565 ?
N1 Ni1 N1 180.0 2_665 14_455 ?
N1 Ni1 N1 88.30(10) . 14_455 ?
N1 Ni1 N1 91.70(10) 15 14_455 ?
N1 Ni1 N1 88.30(10) 3_565 14_455 ?
N1 Ni1 N1 91.70(10) 13_565 14_455 ?
C1 N1 N2 106.1(2) . . ?
C1 N1 Ni1 130.6(2) . . ?
N2 N1 Ni1 122.54(18) . . ?
N3 N2 N1 110.0(2) . . ?
N2 N3 N4 106.8(2) . . ?
C1 N4 N3 108.7(3) . . ?
C1 N4 C2 128.7(3) . . ?
N3 N4 C2 122.6(3) . . ?
N1 C1 N4 108.4(3) . . ?
N1 C1 H1 125.8 . . ?
N4 C1 H1 125.8 . . ?
N4 C2 H21 109.5 . . ?
N4 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
N4 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
N5 Ni2 N5 91.53(11) . 3 ?
N5 Ni2 N5 91.53(11) . 2 ?
N5 Ni2 N5 91.53(11) 3 2 ?
N5 Ni2 N9 177.64(10) . 2 ?
N5 Ni2 N9 87.29(10) 3 2 ?
N5 Ni2 N9 90.54(10) 2 2 ?
N5 Ni2 N9 87.29(10) . 3 ?
N5 Ni2 N9 90.54(10) 3 3 ?
N5 Ni2 N9 177.64(10) 2 3 ?
N9 Ni2 N9 90.68(11) 2 3 ?
N5 Ni2 N9 90.54(10) . . ?
N5 Ni2 N9 177.64(10) 3 . ?
N5 Ni2 N9 87.29(10) 2 . ?
N9 Ni2 N9 90.68(11) 2 . ?
N9 Ni2 N9 90.68(11) 3 . ?
C3 N5 N6 106.2(3) . . ?
C3 N5 Ni2 133.4(2) . . ?
N6 N5 Ni2 120.23(19) . . ?
N7 N6 N5 110.2(2) . . ?
N6 N7 N8 106.6(2) . . ?
C3 N8 N7 108.5(3) . . ?
C3 N8 C4 130.8(3) . . ?
N7 N8 C4 120.7(3) . . ?
C5 N9 N10 105.9(3) . . ?
C5 N9 Ni2 129.7(2) . . ?
N10 N9 Ni2 124.29(19) . . ?
N11 N10 N9 110.1(3) . . ?
N10 N11 N12 106.5(3) . . ?
C5 N12 N11 108.5(3) . . ?
C5 N12 C6 129.7(3) . . ?
N11 N12 C6 121.8(3) . . ?
N8 C4 H41 109.5 . . ?
N8 C4 H42 109.5 . . ?
H41 C4 H42 109.5 . . ?
N8 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
N5 C3 N8 108.5(3) . . ?
N5 C3 H3 125.8 . . ?
N8 C3 H3 125.8 . . ?
N12 C5 N9 109.0(3) . . ?
N12 C5 H5 125.5 . . ?
N9 C5 H5 125.5 . . ?
N12 C6 H62 109.5 . . ?
N12 C6 H61 109.5 . . ?
H62 C6 H61 109.5 . . ?
N12 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
O2 Cl1 O3 108.8(2) . . ?
O2 Cl1 O4 110.12(19) . . ?
O3 Cl1 O4 109.63(19) . . ?
O2 Cl1 O1 109.7(2) . . ?
O3 Cl1 O1 109.5(2) . . ?
O4 Cl1 O1 109.01(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(4) . . . . ?
Ni1 N1 N2 N3 -171.1(2) . . . . ?
N1 N2 N3 N4 0.4(3) . . . . ?
N2 N3 N4 C1 -0.9(4) . . . . ?
N2 N3 N4 C2 177.3(3) . . . . ?
N2 N1 C1 N4 -0.8(3) . . . . ?
Ni1 N1 C1 N4 169.6(2) . . . . ?
N3 N4 C1 N1 1.0(4) . . . . ?
C2 N4 C1 N1 -177.0(3) . . . . ?
C3 N5 N6 N7 -0.4(4) . . . . ?
Ni2 N5 N6 N7 175.7(2) . . . . ?
N5 N6 N7 N8 0.6(4) . . . . ?
N6 N7 N8 C3 -0.5(4) . . . . ?
N6 N7 N8 C4 179.7(3) . . . . ?
C5 N9 N10 N11 -0.1(4) . . . . ?
Ni2 N9 N10 N11 175.7(2) . . . . ?
N9 N10 N11 N12 -0.2(4) . . . . ?
N10 N11 N12 C5 0.4(4) . . . . ?
N10 N11 N12 C6 178.9(3) . . . . ?
N6 N5 C3 N8 0.1(4) . . . . ?
Ni2 N5 C3 N8 -175.3(2) . . . . ?
N7 N8 C3 N5 0.2(4) . . . . ?
C4 N8 C3 N5 180.0(3) . . . . ?
N11 N12 C5 N9 -0.5(4) . . . . ?
C6 N12 C5 N9 -178.8(3) . . . . ?
N10 N9 C5 N12 0.4(4) . . . . ?
Ni2 N9 C5 N12 -175.1(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
? ? ? ? ? ? ? ?

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



_refine_diff_density_max         0.511
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.081

_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_lx139
_database_code_depnum_ccdc_archive 'CCDC 1566360'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Mar 17 04:56:34 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolato) zinc(II) perchlorate bis(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolato) zinc(II) perchlorate bis(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 N24 Zn, 2(C2 H4 N4), 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 N32 O8 Zn'
_chemical_formula_weight         937.00

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'


_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.9713(3)
_cell_length_b                   11.2765(4)
_cell_length_c                   13.4545(5)
_cell_angle_alpha                111.256(3)
_cell_angle_beta                 101.267(3)
_cell_angle_gamma                94.278(3)
_cell_volume                     954.42(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7145
_cell_measurement_theta_min      4.9540
_cell_measurement_theta_max      32.0700

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.870
_shelx_estimated_absorpt_T_min   0.762
_shelx_estimated_absorpt_T_max   0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96461
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_F_000             480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            13753
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.488
_diffrn_reflns_theta_max         25.998
_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             3737
_reflns_number_gt                3428
_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)+(0.0440P)²+0.7838P] 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         3737
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0860
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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      -0.0744837000
_diffrn_orient_matrix_UB_12      0.0008749000
_diffrn_orient_matrix_UB_13      -0.0438527000
_diffrn_orient_matrix_UB_21      0.0739248000
_diffrn_orient_matrix_UB_22      0.0113660000
_diffrn_orient_matrix_UB_23      -0.0264174000
_diffrn_orient_matrix_UB_31      -0.0054582000
_diffrn_orient_matrix_UB_32      -0.0674055000
_diffrn_orient_matrix_UB_33      -0.0278068000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -6.00   41.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000   60.0000 47

#__ type_ start__ end____ width___ exp.time_
  2 omega    7.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -30.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega    2.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 99

#__ type_ start__ end____ width___ exp.time_
  4 omega   -2.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 103

#__ type_ start__ end____ width___ exp.time_
  5 omega  -22.00    3.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -84.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
  6 omega  -43.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -84.0000  150.0000 110

#__ type_ start__ end____ width___ exp.time_
  7 omega  -19.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  8 omega  -57.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   84.0000  -88.0000 101

#__ type_ start__ end____ width___ exp.time_
  9 omega   -6.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   84.0000  -88.0000 29

#__ type_ start__ end____ width___ exp.time_
 10 omega  -93.00   -9.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
 11 omega -102.00   -1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000 -150.0000 101

#__ type_ start__ end____ width___ exp.time_
 12 omega  -65.00  -35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  120.0000 30

;



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 0.5000 0.5000 0.0000 0.01450(10) Uani 1 2 d S . P . .
N1 N 0.3952(2) 0.54951(15) 0.14829(13) 0.0175(3) Uani 1 1 d . . . . .
N2 N 0.3384(3) 0.66528(17) 0.19792(15) 0.0257(4) Uani 1 1 d . . . . .
N3 N 0.2843(3) 0.66885(17) 0.28560(15) 0.0267(4) Uani 1 1 d . . . . .
N4 N 0.3055(2) 0.55466(16) 0.29335(13) 0.0180(3) Uani 1 1 d . . . . .
N5 N 0.2722(2) 0.32969(15) -0.08472(13) 0.0176(3) Uani 1 1 d . . . . .
N6 N 0.2052(3) 0.25825(16) -0.03210(14) 0.0226(4) Uani 1 1 d . . . . .
N7 N 0.0736(3) 0.16216(17) -0.10120(14) 0.0234(4) Uani 1 1 d . . . . .
N8 N 0.0541(2) 0.17004(15) -0.19999(13) 0.0176(3) Uani 1 1 d . . . . .
N9 N 0.6923(2) 0.38526(15) 0.05757(13) 0.0164(3) Uani 1 1 d . . . . .
N10 N 0.8326(3) 0.44262(17) 0.15366(15) 0.0263(4) Uani 1 1 d . . . . .
N11 N 0.9221(3) 0.35707(17) 0.17719(15) 0.0256(4) Uani 1 1 d . . . . .
N12 N 0.8415(2) 0.24253(15) 0.09641(13) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.3738(3) 0.48322(19) 0.20951(15) 0.0171(4) Uani 1 1 d . . . . .
C2 C 0.2604(4) 0.5255(2) 0.38453(18) 0.0267(5) Uani 1 1 d . . . . .
C3 C 0.1757(3) 0.27316(18) -0.18858(16) 0.0181(4) Uani 1 1 d . . . . .
C4 C -0.0882(3) 0.0766(2) -0.29705(19) 0.0258(5) Uani 1 1 d . . . . .
C5 C 0.7014(3) 0.26138(19) 0.02426(16) 0.0182(4) Uani 1 1 d . . . . .
C6 C 0.9066(4) 0.1245(2) 0.1012(2) 0.0244(4) Uani 1 1 d . . . . .
N13 N 0.5053(3) 0.20934(18) 0.20874(15) 0.0270(4) Uani 1 1 d . . . . .
N14 N 0.4369(3) 0.08369(19) 0.14528(15) 0.0313(4) Uani 1 1 d . . . . .
N15 N 0.4833(3) 0.01197(19) 0.19962(16) 0.0321(4) Uani 1 1 d . . . . .
N16 N 0.5833(3) 0.09158(18) 0.30127(15) 0.0238(4) Uani 1 1 d . . . . .
C7 C 0.5953(3) 0.2112(2) 0.30436(18) 0.0265(5) Uani 1 1 d . . . . .
C8 C 0.6451(4) 0.0438(3) 0.3882(3) 0.0400(6) Uani 1 1 d . . . . .
Cl1 Cl 0.18899(7) 0.27000(5) 0.50789(4) 0.02314(13) Uani 1 1 d . . . . .
O1 O 0.0188(3) 0.2654(2) 0.42802(19) 0.0604(6) Uani 1 1 d . . . . .
O2 O 0.3474(3) 0.2455(2) 0.4563(2) 0.0709(8) Uani 1 1 d . . . . .
O3 O 0.1483(4) 0.1712(3) 0.5468(2) 0.0739(8) Uani 1 1 d . . . . .
O4 O 0.2398(3) 0.3930(2) 0.5939(2) 0.0720(8) Uani 1 1 d . . . . .
H3 H 0.184(4) 0.299(2) -0.242(2) 0.022(6) Uiso 1 1 d . . . . .
H1 H 0.396(4) 0.404(3) 0.198(2) 0.024(6) Uiso 1 1 d . . . . .
H5 H 0.627(4) 0.199(3) -0.038(2) 0.036(7) Uiso 1 1 d . . . . .
H6A H 1.036(4) 0.124(2) 0.094(2) 0.025(6) Uiso 1 1 d . . . . .
H2A H 0.240(4) 0.434(3) 0.363(2) 0.038(7) Uiso 1 1 d . . . . .
H6C H 0.897(4) 0.120(2) 0.169(2) 0.025(6) Uiso 1 1 d . . . . .
H7 H 0.658(4) 0.284(3) 0.363(2) 0.044(8) Uiso 1 1 d . . . . .
H4A H -0.070(5) 0.000(3) -0.301(2) 0.044(8) Uiso 1 1 d . . . . .
H4C H -0.069(4) 0.094(3) -0.361(2) 0.044(8) Uiso 1 1 d . . . . .
H4B H -0.222(5) 0.090(3) -0.291(2) 0.048(8) Uiso 1 1 d . . . . .
H6B H 0.824(4) 0.056(3) 0.044(2) 0.039(7) Uiso 1 1 d . . . . .
H8C H 0.631(5) -0.048(4) 0.359(3) 0.069(11) Uiso 1 1 d . . . . .
H2B H 0.374(5) 0.561(3) 0.447(3) 0.043(8) Uiso 1 1 d . . . . .
H2C H 0.143(5) 0.553(3) 0.400(2) 0.046(8) Uiso 1 1 d . . . . .
H8B H 0.566(5) 0.068(3) 0.439(2) 0.043(8) Uiso 1 1 d . . . . .
H8A H 0.774(6) 0.077(4) 0.426(3) 0.072(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
Zn1 N1 2.1561(16) . ?
Zn1 N1 2.1561(16) 2_665 ?
Zn1 N9 2.1564(16) 2_665 ?
Zn1 N9 2.1564(16) . ?
Zn1 N5 2.1819(16) . ?
Zn1 N5 2.1819(16) 2_665 ?
N1 C1 1.318(2) . ?
N1 N2 1.362(2) . ?
N2 N3 1.295(3) . ?
N3 N4 1.346(2) . ?
N4 C1 1.325(3) . ?
N4 C2 1.463(3) . ?
N5 C3 1.317(3) . ?
N5 N6 1.362(2) . ?
N6 N7 1.292(2) . ?
N7 N8 1.345(2) . ?
N8 C3 1.329(3) . ?
N8 C4 1.463(3) . ?
N9 C5 1.314(3) . ?
N9 N10 1.361(2) . ?
N10 N11 1.286(2) . ?
N11 N12 1.342(2) . ?
N12 C5 1.323(3) . ?
N12 C6 1.456(3) . ?
C1 H1 0.88(3) . ?
C2 H2A 0.96(3) . ?
C2 H2B 0.97(3) . ?
C2 H2C 0.93(3) . ?
C3 H3 0.87(2) . ?
C4 H4A 0.86(3) . ?
C4 H4C 0.98(3) . ?
C4 H4B 0.97(3) . ?
C5 H5 0.91(3) . ?
C6 H6A 0.93(3) . ?
C6 H6C 0.95(3) . ?
C6 H6B 0.92(3) . ?
N13 C7 1.309(3) . ?
N13 N14 1.352(3) . ?
N14 N15 1.292(3) . ?
N15 N16 1.344(3) . ?
N16 C7 1.330(3) . ?
N16 C8 1.463(3) . ?
C7 H7 0.91(3) . ?
C8 H8C 0.95(4) . ?
C8 H8B 0.94(3) . ?
C8 H8A 0.92(4) . ?
Cl1 O2 1.409(2) . ?
Cl1 O4 1.412(2) . ?
Cl1 O1 1.420(2) . ?
Cl1 O3 1.424(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
N1 Zn1 N1 180.0 . 2_665 ?
N1 Zn1 N9 91.05(6) . 2_665 ?
N1 Zn1 N9 88.95(6) 2_665 2_665 ?
N1 Zn1 N9 88.95(6) . . ?
N1 Zn1 N9 91.05(6) 2_665 . ?
N9 Zn1 N9 180.0 2_665 . ?
N1 Zn1 N5 91.81(6) . . ?
N1 Zn1 N5 88.20(6) 2_665 . ?
N9 Zn1 N5 90.67(6) 2_665 . ?
N9 Zn1 N5 89.33(6) . . ?
N1 Zn1 N5 88.19(6) . 2_665 ?
N1 Zn1 N5 91.80(6) 2_665 2_665 ?
N9 Zn1 N5 89.33(6) 2_665 2_665 ?
N9 Zn1 N5 90.67(6) . 2_665 ?
N5 Zn1 N5 180.00(7) . 2_665 ?
C1 N1 N2 106.17(16) . . ?
C1 N1 Zn1 130.62(13) . . ?
N2 N1 Zn1 123.21(12) . . ?
N3 N2 N1 109.89(16) . . ?
N2 N3 N4 106.72(16) . . ?
C1 N4 N3 108.69(16) . . ?
C1 N4 C2 129.60(18) . . ?
N3 N4 C2 121.69(17) . . ?
C3 N5 N6 106.30(16) . . ?
C3 N5 Zn1 131.22(13) . . ?
N6 N5 Zn1 122.46(12) . . ?
N7 N6 N5 109.90(16) . . ?
N6 N7 N8 106.86(15) . . ?
C3 N8 N7 108.59(16) . . ?
C3 N8 C4 130.35(18) . . ?
N7 N8 C4 121.03(17) . . ?
C5 N9 N10 105.97(16) . . ?
C5 N9 Zn1 134.37(14) . . ?
N10 N9 Zn1 119.47(12) . . ?
N11 N10 N9 109.90(16) . . ?
N10 N11 N12 107.06(16) . . ?
C5 N12 N11 108.36(16) . . ?
C5 N12 C6 131.10(18) . . ?
N11 N12 C6 120.48(17) . . ?
N1 C1 N4 108.53(17) . . ?
N1 C1 H1 127.8(16) . . ?
N4 C1 H1 123.6(16) . . ?
N4 C2 H2A 108.5(17) . . ?
N4 C2 H2B 108.8(17) . . ?
H2A C2 H2B 108(2) . . ?
N4 C2 H2C 111.6(19) . . ?
H2A C2 H2C 107(3) . . ?
H2B C2 H2C 114(2) . . ?
N5 C3 N8 108.35(17) . . ?
N5 C3 H3 127.2(16) . . ?
N8 C3 H3 124.5(16) . . ?
N8 C4 H4A 108(2) . . ?
N8 C4 H4C 107.9(17) . . ?
H4A C4 H4C 113(3) . . ?
N8 C4 H4B 109.5(18) . . ?
H4A C4 H4B 111(3) . . ?
H4C C4 H4B 107(2) . . ?
N9 C5 N12 108.70(18) . . ?
N9 C5 H5 126.1(17) . . ?
N12 C5 H5 125.2(17) . . ?
N12 C6 H6A 109.4(15) . . ?
N12 C6 H6C 109.3(15) . . ?
H6A C6 H6C 111(2) . . ?
N12 C6 H6B 107.7(18) . . ?
H6A C6 H6B 110(2) . . ?
H6C C6 H6B 110(2) . . ?
C7 N13 N14 105.35(18) . . ?
N15 N14 N13 110.81(18) . . ?
N14 N15 N16 106.63(18) . . ?
C7 N16 N15 107.58(18) . . ?
C7 N16 C8 130.7(2) . . ?
N15 N16 C8 121.5(2) . . ?
N13 C7 N16 109.6(2) . . ?
N13 C7 H7 124.5(19) . . ?
N16 C7 H7 125.8(19) . . ?
N16 C8 H8C 111(2) . . ?
N16 C8 H8B 110.2(18) . . ?
H8C C8 H8B 107(3) . . ?
N16 C8 H8A 111(2) . . ?
H8C C8 H8A 109(3) . . ?
H8B C8 H8A 108(3) . . ?
O2 Cl1 O4 108.77(14) . . ?
O2 Cl1 O1 108.05(17) . . ?
O4 Cl1 O1 110.64(15) . . ?
O2 Cl1 O3 109.27(18) . . ?
O4 Cl1 O3 111.89(17) . . ?
O1 Cl1 O3 108.13(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 -0.1(2) . . . . ?
Zn1 N1 N2 N3 -179.40(14) . . . . ?
N1 N2 N3 N4 -0.1(2) . . . . ?
N2 N3 N4 C1 0.3(2) . . . . ?
N2 N3 N4 C2 179.04(19) . . . . ?
C3 N5 N6 N7 0.1(2) . . . . ?
Zn1 N5 N6 N7 -178.96(13) . . . . ?
N5 N6 N7 N8 0.2(2) . . . . ?
N6 N7 N8 C3 -0.4(2) . . . . ?
N6 N7 N8 C4 -178.49(18) . . . . ?
C5 N9 N10 N11 -0.1(2) . . . . ?
Zn1 N9 N10 N11 175.66(14) . . . . ?
N9 N10 N11 N12 0.2(2) . . . . ?
N10 N11 N12 C5 -0.2(2) . . . . ?
N10 N11 N12 C6 -177.72(18) . . . . ?
N2 N1 C1 N4 0.3(2) . . . . ?
Zn1 N1 C1 N4 179.51(13) . . . . ?
N3 N4 C1 N1 -0.4(2) . . . . ?
C2 N4 C1 N1 -179.00(19) . . . . ?
N6 N5 C3 N8 -0.3(2) . . . . ?
Zn1 N5 C3 N8 178.59(13) . . . . ?
N7 N8 C3 N5 0.4(2) . . . . ?
C4 N8 C3 N5 178.3(2) . . . . ?
N10 N9 C5 N12 -0.1(2) . . . . ?
Zn1 N9 C5 N12 -174.85(13) . . . . ?
N11 N12 C5 N9 0.2(2) . . . . ?
C6 N12 C5 N9 177.32(19) . . . . ?
C7 N13 N14 N15 -0.1(3) . . . . ?
N13 N14 N15 N16 0.4(2) . . . . ?
N14 N15 N16 C7 -0.5(2) . . . . ?
N14 N15 N16 C8 174.9(2) . . . . ?
N14 N13 C7 N16 -0.3(2) . . . . ?
N15 N16 C7 N13 0.5(2) . . . . ?
C8 N16 C7 N13 -174.4(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         0.728
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4


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

data_lx214
_database_code_depnum_ccdc_archive 'CCDC 1566365'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Apr 27 20:17:02 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis-1-methyl-tetrazolyl copper(II) bis-styphnate
;
_chemical_name_common            
'bis-1-methyl-tetrazolyl copper(II) bis-styphnate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 Cu N14 O16'
_chemical_formula_sum            'C16 H12 Cu N14 O16'
_chemical_formula_weight         719.94

_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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_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                   6.0790(3)
_cell_length_b                   20.0450(7)
_cell_length_c                   10.8420(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.129(4)
_cell_angle_gamma                90
_cell_volume                     1319.17(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3271
_cell_measurement_theta_min      4.4260
_cell_measurement_theta_max      30.8520

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.935
_shelx_estimated_absorpt_T_min   0.800
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94330
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            10304
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.273
_diffrn_reflns_theta_max         25.995
_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             2581
_reflns_number_gt                2164
_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)+(0.0367P)²+0.7722P] 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         2581
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0793
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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      0.0791459000
_diffrn_orient_matrix_UB_12      0.0044635000
_diffrn_orient_matrix_UB_13      -0.0450031000
_diffrn_orient_matrix_UB_21      0.0016082000
_diffrn_orient_matrix_UB_22      -0.0349303000
_diffrn_orient_matrix_UB_23      -0.0103128000
_diffrn_orient_matrix_UB_31      -0.0859235000
_diffrn_orient_matrix_UB_32      0.0034270000
_diffrn_orient_matrix_UB_33      -0.0465132000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -87.00   18.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -19.0000    0.0000 105

#__ type_ start__ end____ width___ exp.time_
  2 omega  -80.00  -45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  150.0000 35

#__ type_ start__ end____ width___ exp.time_
  3 omega    7.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
  4 omega -108.00  -44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -180.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega  -98.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  150.0000 93

#__ type_ start__ end____ width___ exp.time_
  6 omega   87.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  -23.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
  8 omega   74.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -180.0000 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
Cu1 Cu 0.0000 0.0000 0.0000 0.01932(13) Uani 1 2 d S . P . .
O1 O 0.4936(3) 0.18013(10) -0.12165(17) 0.0406(5) Uani 1 1 d . . . . .
O2 O 0.2534(3) 0.17893(12) -0.27384(16) 0.0481(6) Uani 1 1 d . . . . .
O3 O -0.2661(3) 0.06302(8) 0.09206(15) 0.0248(4) Uani 1 1 d . . . . .
O4 O -0.3131(3) 0.13717(9) 0.23292(17) 0.0420(5) Uani 1 1 d . . . . .
O5 O -0.2667(4) 0.36396(9) 0.1216(2) 0.0519(6) Uani 1 1 d . . . . .
O6 O -0.0323(3) 0.39746(8) -0.00740(16) 0.0297(4) Uani 1 1 d . . . . .
O7 O 0.0996(3) 0.08888(7) -0.04831(14) 0.0214(3) Uani 1 1 d . . . . .
O8 O 0.1982(3) 0.31319(9) -0.12893(17) 0.0332(4) Uani 1 1 d . . . . .
N1 N 0.2020(3) 0.00385(9) 0.15021(17) 0.0208(4) Uani 1 1 d . . . . .
N2 N 0.1676(3) 0.04620(10) 0.24515(18) 0.0283(5) Uani 1 1 d . . . . .
N3 N 0.3274(3) 0.04029(10) 0.32806(18) 0.0273(5) Uani 1 1 d . . . . .
N4 N 0.4656(3) -0.00553(9) 0.28717(16) 0.0199(4) Uani 1 1 d . . . . .
N5 N -0.1283(3) 0.35244(10) 0.04709(19) 0.0287(5) Uani 1 1 d . . . . .
N6 N 0.3067(3) 0.18685(9) -0.16529(17) 0.0225(4) Uani 1 1 d . . . . .
N7 N -0.2387(3) 0.12037(9) 0.13533(18) 0.0249(4) Uani 1 1 d . . . . .
C1 C 0.3879(4) -0.02741(12) 0.1787(2) 0.0220(5) Uani 1 1 d . . . . .
C2 C 0.6695(4) -0.02384(13) 0.3571(2) 0.0294(6) Uani 1 1 d . . . . .
H2A H 0.6369 -0.0569 0.4201 0.044 Uiso 1 1 calc R U . . .
H2B H 0.7342 0.0159 0.3972 0.044 Uiso 1 1 calc R U . . .
H2C H 0.7738 -0.0428 0.3009 0.044 Uiso 1 1 calc R U . . .
C3 C 0.0379(4) 0.14795(11) -0.02154(19) 0.0182(5) Uani 1 1 d . . . . .
C4 C -0.1185(4) 0.16823(11) 0.0663(2) 0.0195(5) Uani 1 1 d . . . . .
C5 C -0.1680(4) 0.23428(11) 0.0868(2) 0.0221(5) Uani 1 1 d . . . . .
C6 C -0.0717(4) 0.28436(11) 0.0220(2) 0.0210(5) Uani 1 1 d . . . . .
C7 C 0.0885(4) 0.26928(11) -0.0641(2) 0.0202(5) Uani 1 1 d . . . . .
C8 C 0.1351(4) 0.20271(11) -0.07985(19) 0.0177(5) Uani 1 1 d . . . . .
H5 H -0.294(4) 0.2451(12) 0.149(2) 0.021(6) Uiso 1 1 d . . . . .
H8 H 0.152(6) 0.353(2) -0.106(3) 0.069(12) Uiso 1 1 d . . . . .
H1 H 0.448(4) -0.0581(13) 0.132(2) 0.027(7) 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 O7 1.9621(14) . ?
Cu1 O7 1.9622(14) 3 ?
Cu1 N1 1.9868(18) . ?
Cu1 N1 1.9869(18) 3 ?
Cu1 O3 2.3207(16) 3 ?
Cu1 O3 2.3207(16) . ?
O1 N6 1.214(2) . ?
O2 N6 1.214(2) . ?
O3 N7 1.249(2) . ?
O4 N7 1.220(3) . ?
O5 N5 1.220(3) . ?
O6 N5 1.242(3) . ?
O7 C3 1.280(3) . ?
O8 C7 1.328(3) . ?
O8 H8 0.88(4) . ?
N1 C1 1.314(3) . ?
N1 N2 1.359(3) . ?
N2 N3 1.292(3) . ?
N3 N4 1.337(3) . ?
N4 C1 1.318(3) . ?
N4 C2 1.464(3) . ?
N5 C6 1.437(3) . ?
N6 C8 1.467(3) . ?
N7 C4 1.440(3) . ?
C1 H1 0.89(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C8 1.412(3) . ?
C3 C4 1.440(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.374(3) . ?
C5 H5 1.07(2) . ?
C6 C7 1.418(3) . ?
C7 C8 1.377(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
O7 Cu1 O7 180.00(3) . 3 ?
O7 Cu1 N1 89.86(7) . . ?
O7 Cu1 N1 90.14(7) 3 . ?
O7 Cu1 N1 90.14(7) . 3 ?
O7 Cu1 N1 89.86(7) 3 3 ?
N1 Cu1 N1 180.0 . 3 ?
O7 Cu1 O3 98.45(6) . 3 ?
O7 Cu1 O3 81.55(6) 3 3 ?
N1 Cu1 O3 87.68(7) . 3 ?
N1 Cu1 O3 92.32(7) 3 3 ?
O7 Cu1 O3 81.55(6) . . ?
O7 Cu1 O3 98.45(6) 3 . ?
N1 Cu1 O3 92.32(7) . . ?
N1 Cu1 O3 87.68(7) 3 . ?
O3 Cu1 O3 180.00(11) 3 . ?
N7 O3 Cu1 125.48(14) . . ?
C3 O7 Cu1 132.90(15) . . ?
C7 O8 H8 105(2) . . ?
C1 N1 N2 106.57(19) . . ?
C1 N1 Cu1 131.26(16) . . ?
N2 N1 Cu1 122.09(15) . . ?
N3 N2 N1 109.19(19) . . ?
N2 N3 N4 107.12(18) . . ?
C1 N4 N3 108.86(19) . . ?
C1 N4 C2 129.1(2) . . ?
N3 N4 C2 122.01(19) . . ?
O5 N5 O6 122.5(2) . . ?
O5 N5 C6 119.1(2) . . ?
O6 N5 C6 118.5(2) . . ?
O2 N6 O1 123.9(2) . . ?
O2 N6 C8 118.63(19) . . ?
O1 N6 C8 117.41(18) . . ?
O4 N7 O3 122.08(19) . . ?
O4 N7 C4 119.31(19) . . ?
O3 N7 C4 118.61(18) . . ?
N1 C1 N4 108.2(2) . . ?
N1 C1 H1 125.2(16) . . ?
N4 C1 H1 126.6(16) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O7 C3 C8 118.8(2) . . ?
O7 C3 C4 128.5(2) . . ?
C8 C3 C4 112.58(19) . . ?
C5 C4 C3 122.4(2) . . ?
C5 C4 N7 115.8(2) . . ?
C3 C4 N7 121.84(19) . . ?
C6 C5 C4 121.1(2) . . ?
C6 C5 H5 120.8(13) . . ?
C4 C5 H5 117.9(13) . . ?
C5 C6 C7 120.5(2) . . ?
C5 C6 N5 119.0(2) . . ?
C7 C6 N5 120.5(2) . . ?
O8 C7 C8 117.6(2) . . ?
O8 C7 C6 126.2(2) . . ?
C8 C7 C6 116.2(2) . . ?
C7 C8 C3 127.1(2) . . ?
C7 C8 N6 116.52(19) . . ?
C3 C8 N6 116.33(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(2) . . . . ?
Cu1 N1 N2 N3 -177.46(15) . . . . ?
N1 N2 N3 N4 0.2(2) . . . . ?
N2 N3 N4 C1 -0.1(2) . . . . ?
N2 N3 N4 C2 178.6(2) . . . . ?
Cu1 O3 N7 O4 -138.2(2) . . . . ?
Cu1 O3 N7 C4 42.8(3) . . . . ?
N2 N1 C1 N4 0.2(2) . . . . ?
Cu1 N1 C1 N4 177.04(15) . . . . ?
N3 N4 C1 N1 -0.1(3) . . . . ?
C2 N4 C1 N1 -178.6(2) . . . . ?
Cu1 O7 C3 C8 -175.44(14) . . . . ?
Cu1 O7 C3 C4 6.8(3) . . . . ?
O7 C3 C4 C5 179.3(2) . . . . ?
C8 C3 C4 C5 1.4(3) . . . . ?
O7 C3 C4 N7 -2.8(3) . . . . ?
C8 C3 C4 N7 179.34(19) . . . . ?
O4 N7 C4 C5 -25.0(3) . . . . ?
O3 N7 C4 C5 154.0(2) . . . . ?
O4 N7 C4 C3 157.0(2) . . . . ?
O3 N7 C4 C3 -24.1(3) . . . . ?
C3 C4 C5 C6 1.1(3) . . . . ?
N7 C4 C5 C6 -176.9(2) . . . . ?
C4 C5 C6 C7 -2.7(3) . . . . ?
C4 C5 C6 N5 -179.8(2) . . . . ?
O5 N5 C6 C5 -2.8(3) . . . . ?
O6 N5 C6 C5 176.4(2) . . . . ?
O5 N5 C6 C7 180.0(2) . . . . ?
O6 N5 C6 C7 -0.7(3) . . . . ?
C5 C6 C7 O8 -177.6(2) . . . . ?
N5 C6 C7 O8 -0.4(4) . . . . ?
C5 C6 C7 C8 1.5(3) . . . . ?
N5 C6 C7 C8 178.6(2) . . . . ?
O8 C7 C8 C3 -179.5(2) . . . . ?
C6 C7 C8 C3 1.4(3) . . . . ?
O8 C7 C8 N6 1.4(3) . . . . ?
C6 C7 C8 N6 -177.74(18) . . . . ?
O7 C3 C8 C7 179.2(2) . . . . ?
C4 C3 C8 C7 -2.7(3) . . . . ?
O7 C3 C8 N6 -1.7(3) . . . . ?
C4 C3 C8 N6 176.38(18) . . . . ?
O2 N6 C8 C7 -89.0(3) . . . . ?
O1 N6 C8 C7 93.5(3) . . . . ?
O2 N6 C8 C3 91.7(3) . . . . ?
O1 N6 C8 C3 -85.7(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
C2 H2B O6 0.98 2.44 3.402(3) 168.0 4_666
O8 H8 O6 0.88(4) 1.83(4) 2.599(3) 146(4) .
O8 H8 N2 0.88(4) 2.60(4) 3.133(3) 120(3) 4_565
O8 H8 N3 0.88(4) 2.52(4) 3.082(3) 122(3) 4_565
O8 H8 N5 0.88(4) 2.44(4) 2.935(3) 116(3) .
C1 H1 O1 0.89(3) 2.47(3) 3.213(3) 141(2) 3_655
C1 H1 O3 0.89(3) 2.62(2) 3.073(3) 112.6(19) 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         0.345
_refine_diff_density_min         -0.320
_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_lx124
_database_code_depnum_ccdc_archive 'CCDC 1566364'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Mar 09 10:23:26 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) copper(II) perchlorate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) copper(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Cl2 Cu N24 O8'
_chemical_formula_weight         766.99

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_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                   10.4126(6)
_cell_length_b                   17.9765(9)
_cell_length_c                   18.3433(9)
_cell_angle_alpha                64.772(5)
_cell_angle_beta                 87.906(4)
_cell_angle_gamma                85.765(5)
_cell_volume                     3097.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9425
_cell_measurement_theta_min      4.4610
_cell_measurement_theta_max      32.2980

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.958
_shelx_estimated_absorpt_T_min   0.831
_shelx_estimated_absorpt_T_max   0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82725
_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    1.645
_exptl_crystal_F_000             1564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            35144
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.227
_diffrn_reflns_theta_max         32.345
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             19936
_reflns_number_gt                14850
_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)+(0.0495P)²+1.8591P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         19936
_refine_ls_number_parameters     865
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.005
_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      -0.0584779000
_diffrn_orient_matrix_UB_12      -0.0095329000
_diffrn_orient_matrix_UB_13      -0.0117528000
_diffrn_orient_matrix_UB_21      0.0230638000
_diffrn_orient_matrix_UB_22      -0.0418828000
_diffrn_orient_matrix_UB_23      0.0141867000
_diffrn_orient_matrix_UB_31      -0.0267252000
_diffrn_orient_matrix_UB_32      -0.0080846000
_diffrn_orient_matrix_UB_33      0.0385723000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -84.00    9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -73.00   30.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000  -30.0000 103

#__ type_ start__ end____ width___ exp.time_
  3 omega  -90.00  -58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
  4 omega   17.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  150.0000 57

#__ type_ start__ end____ width___ exp.time_
  5 omega  -13.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 81

#__ type_ start__ end____ width___ exp.time_
  6 omega   59.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
  7 omega   -1.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -30.0000 66

;



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'
O O 0.0106 0.0060 '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 0.01412(6) Uani 1 2 d S . P . .
N1 N 0.16102(13) 0.92732(9) 0.00299(8) 0.0161(3) Uani 1 1 d . . . . .
N2 N 0.17324(14) 0.87872(10) -0.03740(9) 0.0209(3) Uani 1 1 d . . . . .
N3 N 0.28439(15) 0.83855(10) -0.02281(9) 0.0216(3) Uani 1 1 d . . . . .
N4 N 0.34522(13) 0.86077(9) 0.02758(8) 0.0172(3) Uani 1 1 d . . . . .
N5 N 0.10513(13) 1.06931(9) 0.03409(8) 0.0157(3) Uani 1 1 d . . . . .
N6 N 0.18842(14) 1.12479(10) -0.01422(9) 0.0208(3) Uani 1 1 d . . . . .
N7 N 0.22498(15) 1.16742(10) 0.02192(10) 0.0231(3) Uani 1 1 d . . . . .
N8 N 0.16521(14) 1.13982(9) 0.09408(9) 0.0193(3) Uani 1 1 d . . . . .
N9 N -0.04514(14) 0.91464(9) 0.13907(8) 0.0191(3) Uani 1 1 d . . . . .
N10 N 0.03387(16) 0.84827(11) 0.18234(9) 0.0276(4) Uani 1 1 d . . . . .
N11 N -0.02279(17) 0.80071(11) 0.24801(10) 0.0307(4) Uani 1 1 d . . . . .
N12 N -0.14095(14) 0.83648(9) 0.24805(9) 0.0192(3) Uani 1 1 d . . . . .
C1 C 0.26928(16) 0.91521(11) 0.04289(10) 0.0181(3) Uani 1 1 d . . . . .
H1 H 0.2893 0.9408 0.0765 0.022 Uiso 1 1 calc R U . . .
C2 C 0.47672(17) 0.82881(12) 0.05421(11) 0.0248(4) Uani 1 1 d . . . . .
H21 H 0.5297 0.8319 0.0079 0.037 Uiso 1 1 calc R U . . .
H22 H 0.4759 0.7713 0.0942 0.037 Uiso 1 1 calc R U . . .
H23 H 0.5127 0.8618 0.0784 0.037 Uiso 1 1 calc R U . . .
C3 C 0.09289(16) 1.07949(11) 0.10103(10) 0.0181(3) Uani 1 1 d . . . . .
H3 H 0.0413 1.0490 0.1463 0.022 Uiso 1 1 calc R U . . .
C4 C 0.1829(2) 1.17514(14) 0.15111(14) 0.0318(4) Uani 1 1 d . . . . .
H41 H 0.1388 1.1430 0.2019 0.048 Uiso 1 1 calc R U . . .
H42 H 0.1467 1.2323 0.1286 0.048 Uiso 1 1 calc R U . . .
H43 H 0.2750 1.1738 0.1612 0.048 Uiso 1 1 calc R U . . .
C5 C -0.15257(17) 0.90586(11) 0.18103(10) 0.0219(3) Uani 1 1 d . . . . .
H5 H -0.2266 0.9432 0.1658 0.026 Uiso 1 1 calc R U . . .
C6 C -0.23082(19) 0.80094(12) 0.31542(11) 0.0267(4) Uani 1 1 d . . . . .
H61 H -0.2234 0.7407 0.3362 0.040 Uiso 1 1 calc R U . . .
H62 H -0.3190 0.8214 0.2969 0.040 Uiso 1 1 calc R U . . .
H63 H -0.2102 0.8169 0.3583 0.040 Uiso 1 1 calc R U . . .
Cu2 Cu 0.5000 0.0000 0.5000 0.01823(7) Uani 1 2 d S . P . .
N13 N 0.34118(14) 0.07022(10) 0.44133(9) 0.0205(3) Uani 1 1 d . . . . .
N14 N 0.32713(16) 0.10164(10) 0.35991(9) 0.0251(3) Uani 1 1 d . . . . .
N15 N 0.21763(16) 0.14330(11) 0.33952(9) 0.0258(3) Uani 1 1 d . . . . .
N16 N 0.16009(15) 0.13952(10) 0.40775(9) 0.0220(3) Uani 1 1 d . . . . .
N17 N 0.53865(15) 0.09351(10) 0.55698(10) 0.0237(3) Uani 1 1 d . . . . .
N18 N 0.45790(17) 0.16031(11) 0.54459(11) 0.0321(4) Uani 1 1 d . . . . .
N19 N 0.50221(17) 0.20327(11) 0.57887(12) 0.0335(4) Uani 1 1 d . . . . .
N20 N 0.61360(14) 0.16453(9) 0.61344(9) 0.0208(3) Uani 1 1 d . . . . .
N21 N 0.38791(14) -0.06225(9) 0.59645(9) 0.0195(3) Uani 1 1 d . . . . .
N22 N 0.29792(17) -0.11267(11) 0.59508(9) 0.0288(4) Uani 1 1 d . . . . .
N23 N 0.24067(17) -0.14354(12) 0.66409(10) 0.0302(4) Uani 1 1 d . . . . .
N24 N 0.29382(14) -0.11405(10) 0.71149(9) 0.0203(3) Uani 1 1 d . . . . .
C7 C 0.23603(17) 0.09439(12) 0.46955(11) 0.0228(3) Uani 1 1 d . . . . .
H7 H 0.2178 0.0817 0.5246 0.027 Uiso 1 1 calc R U . . .
C8 C 0.03228(19) 0.18008(15) 0.40630(14) 0.0342(5) Uani 1 1 d . . . . .
H81 H -0.0150 0.1474 0.4555 0.051 Uiso 1 1 calc R U . . .
H82 H -0.0151 0.1847 0.3592 0.051 Uiso 1 1 calc R U . . .
H83 H 0.0415 0.2352 0.4032 0.051 Uiso 1 1 calc R U . . .
C9 C 0.63369(18) 0.09786(12) 0.60019(12) 0.0263(4) Uani 1 1 d . . . . .
H9 H 0.7056 0.0591 0.6189 0.032 Uiso 1 1 calc R U . . .
C10 C 0.6859(2) 0.19354(13) 0.66209(12) 0.0284(4) Uani 1 1 d . . . . .
H101 H 0.6618 0.2520 0.6467 0.043 Uiso 1 1 calc R U . . .
H102 H 0.7784 0.1864 0.6529 0.043 Uiso 1 1 calc R U . . .
H103 H 0.6660 0.1616 0.7192 0.043 Uiso 1 1 calc R U . . .
C11 C 0.38276(17) -0.06389(12) 0.66910(10) 0.0216(3) Uani 1 1 d . . . . .
H11 H 0.4342 -0.0341 0.6878 0.026 Uiso 1 1 calc R U . . .
C12 C 0.2440(2) -0.13126(13) 0.79205(11) 0.0286(4) Uani 1 1 d . . . . .
H121 H 0.2213 -0.1888 0.8189 0.043 Uiso 1 1 calc R U . . .
H122 H 0.1673 -0.0948 0.7880 0.043 Uiso 1 1 calc R U . . .
H123 H 0.3100 -0.1218 0.8234 0.043 Uiso 1 1 calc R U . . .
Cu3 Cu 0.5000 0.5000 0.5000 0.01315(6) Uani 1 2 d S . P . .
N25 N 0.39709(13) 0.43164(8) 0.46247(8) 0.0148(2) Uani 1 1 d . . . . .
N26 N 0.30765(13) 0.37974(9) 0.50907(9) 0.0182(3) Uani 1 1 d . . . . .
N27 N 0.27200(14) 0.33578(9) 0.47385(9) 0.0199(3) Uani 1 1 d . . . . .
N28 N 0.33875(13) 0.35911(9) 0.40392(8) 0.0168(3) Uani 1 1 d . . . . .
N29 N 0.66219(13) 0.42777(9) 0.50404(8) 0.0148(3) Uani 1 1 d . . . . .
N30 N 0.67676(14) 0.37986(10) 0.46302(9) 0.0202(3) Uani 1 1 d . . . . .
N31 N 0.78903(14) 0.34101(10) 0.47741(9) 0.0207(3) Uani 1 1 d . . . . .
N32 N 0.84819(13) 0.36389(9) 0.52815(8) 0.0162(3) Uani 1 1 d . . . . .
N33 N 0.54976(14) 0.58381(9) 0.36316(8) 0.0176(3) Uani 1 1 d . . . . .
N34 N 0.46181(15) 0.63967(10) 0.31261(9) 0.0237(3) Uani 1 1 d . . . . .
N35 N 0.51557(16) 0.68453(10) 0.24480(9) 0.0263(3) Uani 1 1 d . . . . .
N36 N 0.64103(14) 0.65826(9) 0.25096(8) 0.0186(3) Uani 1 1 d . . . . .
C13 C 0.41367(15) 0.41811(10) 0.39751(10) 0.0164(3) Uani 1 1 d . . . . .
H13 H 0.4697 0.4458 0.3536 0.020 Uiso 1 1 calc R U . . .
C14 C 0.3225(2) 0.32147(13) 0.34859(12) 0.0260(4) Uani 1 1 d . . . . .
H141 H 0.2308 0.3243 0.3365 0.039 Uiso 1 1 calc R U . . .
H142 H 0.3556 0.2637 0.3735 0.039 Uiso 1 1 calc R U . . .
H143 H 0.3700 0.3511 0.2986 0.039 Uiso 1 1 calc R U . . .
C15 C 0.77011(15) 0.41689(10) 0.54390(10) 0.0161(3) Uani 1 1 d . . . . .
H15 H 0.7885 0.4425 0.5778 0.019 Uiso 1 1 calc R U . . .
C16 C 0.97992(17) 0.33367(12) 0.55439(11) 0.0239(4) Uani 1 1 d . . . . .
H161 H 1.0332 0.3376 0.5079 0.036 Uiso 1 1 calc R U . . .
H162 H 0.9808 0.2761 0.5942 0.036 Uiso 1 1 calc R U . . .
H163 H 1.0144 0.3670 0.5787 0.036 Uiso 1 1 calc R U . . .
C17 C 0.65957(16) 0.59637(11) 0.32351(10) 0.0183(3) Uani 1 1 d . . . . .
H17 H 0.7392 0.5662 0.3434 0.022 Uiso 1 1 calc R U . . .
C18 C 0.72965(19) 0.69215(12) 0.18287(11) 0.0264(4) Uani 1 1 d . . . . .
H181 H 0.7074 0.6752 0.1410 0.040 Uiso 1 1 calc R U . . .
H182 H 0.8180 0.6716 0.2010 0.040 Uiso 1 1 calc R U . . .
H183 H 0.7230 0.7524 0.1610 0.040 Uiso 1 1 calc R U . . .
Cu4 Cu 0.0000 0.5000 0.0000 0.01805(7) Uani 1 2 d S . P . .
N37 N 0.02939(14) 0.57995(10) 0.04955(9) 0.0206(3) Uani 1 1 d . . . . .
N38 N -0.04873(17) 0.64850(11) 0.03647(12) 0.0323(4) Uani 1 1 d . . . . .
N39 N 0.00069(18) 0.69134(12) 0.06860(12) 0.0336(4) Uani 1 1 d . . . . .
N40 N 0.11183(14) 0.65104(9) 0.10253(9) 0.0203(3) Uani 1 1 d . . . . .
N41 N -0.10771(14) 0.43211(9) 0.09734(9) 0.0193(3) Uani 1 1 d . . . . .
N42 N -0.17011(18) 0.36642(11) 0.10169(10) 0.0302(4) Uani 1 1 d . . . . .
N43 N -0.21987(18) 0.32966(11) 0.17254(10) 0.0299(4) Uani 1 1 d . . . . .
N44 N -0.19010(14) 0.37127(10) 0.21528(9) 0.0205(3) Uani 1 1 d . . . . .
N45 N 0.18606(15) 0.42018(10) 0.07105(9) 0.0237(3) Uani 1 1 d . . . . .
N46 N 0.18858(16) 0.37288(10) 0.15170(10) 0.0258(3) Uani 1 1 d . . . . .
N47 N 0.29623(17) 0.32862(11) 0.17173(10) 0.0281(3) Uani 1 1 d . . . . .
N48 N 0.36490(15) 0.34661(10) 0.10364(10) 0.0238(3) Uani 1 1 d . . . . .
C19 C 0.12793(18) 0.58334(11) 0.09105(11) 0.0225(3) Uani 1 1 d . . . . .
H19 H 0.1987 0.5436 0.1096 0.027 Uiso 1 1 calc R U . . .
C20 C 0.1903(2) 0.68018(12) 0.14869(12) 0.0266(4) Uani 1 1 d . . . . .
H201 H 0.1822 0.6443 0.2063 0.040 Uiso 1 1 calc R U . . .
H202 H 0.1605 0.7367 0.1385 0.040 Uiso 1 1 calc R U . . .
H203 H 0.2807 0.6789 0.1321 0.040 Uiso 1 1 calc R U . . .
C21 C -0.12181(17) 0.43383(11) 0.16845(10) 0.0210(3) Uani 1 1 d . . . . .
H219 H -0.0887 0.4731 0.1835 0.025 Uiso 1 1 calc R U . . .
C22 C -0.2356(2) 0.34745(13) 0.29793(11) 0.0276(4) Uani 1 1 d . . . . .
H221 H -0.3243 0.3701 0.2974 0.041 Uiso 1 1 calc R U . . .
H222 H -0.1802 0.3690 0.3255 0.041 Uiso 1 1 calc R U . . .
H223 H -0.2330 0.2872 0.3264 0.041 Uiso 1 1 calc R U . . .
C23 C 0.29628(19) 0.40291(13) 0.04306(12) 0.0286(4) Uani 1 1 d . . . . .
H231 H 0.3228 0.4269 -0.0118 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4922(2) 0.30661(15) 0.10368(15) 0.0358(5) Uani 1 1 d . . . . .
H241 H 0.5431 0.3056 0.1480 0.054 Uiso 1 1 calc R U . . .
H242 H 0.5358 0.3374 0.0524 0.054 Uiso 1 1 calc R U . . .
H243 H 0.4831 0.2501 0.1107 0.054 Uiso 1 1 calc R U . . .
Cl1 Cl 0.47980(4) 0.00346(3) 0.16640(2) 0.01842(8) Uani 1 1 d . . . . .
O1 O 0.47949(14) 0.08896(9) 0.15069(9) 0.0314(3) Uani 1 1 d . . . . .
O2 O 0.54421(14) -0.04616(9) 0.24177(8) 0.0292(3) Uani 1 1 d . . . . .
O3 O 0.34961(13) -0.01992(10) 0.17087(9) 0.0314(3) Uani 1 1 d . . . . .
O4 O 0.54770(16) -0.01019(10) 0.10280(9) 0.0350(3) Uani 1 1 d . . . . .
Cl2 Cl 0.50606(4) 0.52268(3) 0.15735(3) 0.02272(9) Uani 1 1 d . . . . .
O5 O 0.56654(18) 0.47370(11) 0.11939(10) 0.0424(4) Uani 1 1 d . . . . .
O6 O 0.38064(16) 0.49515(12) 0.18517(11) 0.0517(5) Uani 1 1 d . . . . .
O7 O 0.58120(17) 0.51079(11) 0.22667(10) 0.0409(4) Uani 1 1 d . . . . .
O8 O 0.49768(17) 0.60813(10) 0.10183(9) 0.0410(4) Uani 1 1 d . . . . .
Cl3 Cl 0.02358(4) 0.49541(3) 0.32958(2) 0.01855(8) Uani 1 1 d . . . . .
O9 O 0.02293(14) 0.40995(9) 0.34550(9) 0.0314(3) Uani 1 1 d . . . . .
O10 O -0.03641(14) 0.54556(9) 0.25255(8) 0.0271(3) Uani 1 1 d . . . . .
O11 O 0.15424(13) 0.51764(9) 0.32801(8) 0.0283(3) Uani 1 1 d . . . . .
O12 O -0.04791(14) 0.51015(9) 0.39165(8) 0.0301(3) Uani 1 1 d . . . . .
Cl4 Cl 0.00250(4) 0.04783(3) 0.64309(3) 0.02653(10) Uani 1 1 d . . . . .
O13 O 0.13891(15) 0.04323(12) 0.65283(11) 0.0465(4) Uani 1 1 d . . . . .
O14 O -0.0250(2) 0.01107(14) 0.59103(13) 0.0669(6) Uani 1 1 d . . . . .
O15 O -0.0630(2) 0.01282(19) 0.71599(12) 0.0873(9) Uani 1 1 d . . . . .
O16 O -0.0378(2) 0.13396(12) 0.60130(13) 0.0627(6) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N5 2.0143(14) . ?
Cu1 N5 2.0143(14) 2_575 ?
Cu1 N1 2.0355(14) . ?
Cu1 N1 2.0356(14) 2_575 ?
Cu1 N9 2.4010(14) . ?
Cu1 N9 2.4010(14) 2_575 ?
N1 C1 1.320(2) . ?
N1 N2 1.3626(19) . ?
N2 N3 1.291(2) . ?
N3 N4 1.345(2) . ?
N4 C1 1.329(2) . ?
N4 C2 1.462(2) . ?
N5 C3 1.317(2) . ?
N5 N6 1.3603(19) . ?
N6 N7 1.291(2) . ?
N7 N8 1.346(2) . ?
N8 C3 1.325(2) . ?
N8 C4 1.459(2) . ?
N9 C5 1.315(2) . ?
N9 N10 1.351(2) . ?
N10 N11 1.294(2) . ?
N11 N12 1.346(2) . ?
N12 C5 1.328(2) . ?
N12 C6 1.463(2) . ?
C1 H1 0.9500 . ?
C2 H21 0.9800 . ?
C2 H22 0.9800 . ?
C2 H23 0.9800 . ?
C3 H3 0.9500 . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 H5 0.9500 . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
Cu2 N21 2.0245(14) 2_656 ?
Cu2 N21 2.0246(14) . ?
Cu2 N13 2.0372(15) 2_656 ?
Cu2 N13 2.0372(15) . ?
Cu2 N17 2.3893(16) . ?
Cu2 N17 2.3893(16) 2_656 ?
N13 C7 1.317(2) . ?
N13 N14 1.362(2) . ?
N14 N15 1.291(2) . ?
N15 N16 1.345(2) . ?
N16 C7 1.325(2) . ?
N16 C8 1.465(2) . ?
N17 C9 1.317(2) . ?
N17 N18 1.354(2) . ?
N18 N19 1.301(2) . ?
N19 N20 1.338(2) . ?
N20 C9 1.322(2) . ?
N20 C10 1.463(2) . ?
N21 C11 1.319(2) . ?
N21 N22 1.359(2) . ?
N22 N23 1.289(2) . ?
N23 N24 1.347(2) . ?
N24 C11 1.322(2) . ?
N24 C12 1.458(2) . ?
C7 H7 0.9500 . ?
C8 H81 0.9800 . ?
C8 H82 0.9800 . ?
C8 H83 0.9800 . ?
C9 H9 0.9500 . ?
C10 H101 0.9800 . ?
C10 H102 0.9800 . ?
C10 H103 0.9800 . ?
C11 H11 0.9500 . ?
C12 H121 0.9800 . ?
C12 H122 0.9800 . ?
C12 H123 0.9800 . ?
Cu3 N25 2.0254(14) . ?
Cu3 N25 2.0254(14) 2_666 ?
Cu3 N29 2.0363(13) . ?
Cu3 N29 2.0364(13) 2_666 ?
Cu3 N33 2.3738(14) 2_666 ?
Cu3 N33 2.3739(14) . ?
N25 C13 1.317(2) . ?
N25 N26 1.3633(18) . ?
N26 N27 1.295(2) . ?
N27 N28 1.3505(19) . ?
N28 C13 1.325(2) . ?
N28 C14 1.460(2) . ?
N29 C15 1.320(2) . ?
N29 N30 1.3624(19) . ?
N30 N31 1.292(2) . ?
N31 N32 1.349(2) . ?
N32 C15 1.325(2) . ?
N32 C16 1.457(2) . ?
N33 C17 1.313(2) . ?
N33 N34 1.356(2) . ?
N34 N35 1.293(2) . ?
N35 N36 1.348(2) . ?
N36 C17 1.331(2) . ?
N36 C18 1.460(2) . ?
C13 H13 0.9500 . ?
C14 H141 0.9800 . ?
C14 H142 0.9800 . ?
C14 H143 0.9800 . ?
C15 H15 0.9500 . ?
C16 H161 0.9800 . ?
C16 H162 0.9800 . ?
C16 H163 0.9800 . ?
C17 H17 0.9500 . ?
C18 H181 0.9800 . ?
C18 H182 0.9800 . ?
C18 H183 0.9800 . ?
Cu4 N41 2.0331(15) 2_565 ?
Cu4 N41 2.0332(15) . ?
Cu4 N37 2.0456(15) . ?
Cu4 N37 2.0457(15) 2_565 ?
Cu4 N45 2.3856(16) . ?
Cu4 N45 2.3856(16) 2_565 ?
N37 C19 1.320(2) . ?
N37 N38 1.361(2) . ?
N38 N39 1.293(2) . ?
N39 N40 1.340(2) . ?
N40 C19 1.319(2) . ?
N40 C20 1.467(2) . ?
N41 C21 1.321(2) . ?
N41 N42 1.361(2) . ?
N42 N43 1.290(2) . ?
N43 N44 1.350(2) . ?
N44 C21 1.326(2) . ?
N44 C22 1.460(2) . ?
N45 C23 1.310(2) . ?
N45 N46 1.356(2) . ?
N46 N47 1.294(2) . ?
N47 N48 1.342(2) . ?
N48 C23 1.327(2) . ?
N48 C24 1.460(3) . ?
C19 H19 0.9500 . ?
C20 H201 0.9800 . ?
C20 H202 0.9800 . ?
C20 H203 0.9800 . ?
C21 H219 0.9500 . ?
C22 H221 0.9800 . ?
C22 H222 0.9800 . ?
C22 H223 0.9800 . ?
C23 H231 0.9500 . ?
C24 H241 0.9800 . ?
C24 H242 0.9800 . ?
C24 H243 0.9800 . ?
Cl1 O1 1.4378(15) . ?
Cl1 O3 1.4379(14) . ?
Cl1 O4 1.4419(14) . ?
Cl1 O2 1.4439(14) . ?
Cl2 O6 1.4291(16) . ?
Cl2 O8 1.4344(16) . ?
Cl2 O5 1.4372(16) . ?
Cl2 O7 1.4460(16) . ?
Cl3 O9 1.4367(15) . ?
Cl3 O11 1.4420(14) . ?
Cl3 O12 1.4446(14) . ?
Cl3 O10 1.4474(13) . ?
Cl4 O15 1.3892(19) . ?
Cl4 O14 1.4200(19) . ?
Cl4 O13 1.4300(17) . ?
Cl4 O16 1.441(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
N5 Cu1 N5 180.0 . 2_575 ?
N5 Cu1 N1 89.83(6) . . ?
N5 Cu1 N1 90.17(6) 2_575 . ?
N5 Cu1 N1 90.17(6) . 2_575 ?
N5 Cu1 N1 89.84(6) 2_575 2_575 ?
N1 Cu1 N1 180.0 . 2_575 ?
N5 Cu1 N9 89.55(5) . . ?
N5 Cu1 N9 90.45(5) 2_575 . ?
N1 Cu1 N9 91.04(5) . . ?
N1 Cu1 N9 88.96(5) 2_575 . ?
N5 Cu1 N9 90.46(5) . 2_575 ?
N5 Cu1 N9 89.54(5) 2_575 2_575 ?
N1 Cu1 N9 88.96(5) . 2_575 ?
N1 Cu1 N9 91.04(5) 2_575 2_575 ?
N9 Cu1 N9 180.0 . 2_575 ?
C1 N1 N2 106.62(14) . . ?
C1 N1 Cu1 129.62(12) . . ?
N2 N1 Cu1 123.74(11) . . ?
N3 N2 N1 109.83(14) . . ?
N2 N3 N4 106.68(14) . . ?
C1 N4 N3 109.11(14) . . ?
C1 N4 C2 129.68(16) . . ?
N3 N4 C2 121.14(15) . . ?
C3 N5 N6 106.81(14) . . ?
C3 N5 Cu1 127.27(11) . . ?
N6 N5 Cu1 125.16(11) . . ?
N7 N6 N5 109.46(14) . . ?
N6 N7 N8 106.96(14) . . ?
C3 N8 N7 108.81(14) . . ?
C3 N8 C4 129.15(16) . . ?
N7 N8 C4 122.04(16) . . ?
C5 N9 N10 105.89(14) . . ?
C5 N9 Cu1 131.01(12) . . ?
N10 N9 Cu1 120.85(10) . . ?
N11 N10 N9 110.35(15) . . ?
N10 N11 N12 106.77(15) . . ?
C5 N12 N11 107.92(14) . . ?
C5 N12 C6 130.23(16) . . ?
N11 N12 C6 121.81(15) . . ?
N1 C1 N4 107.76(15) . . ?
N1 C1 H1 126.1 . . ?
N4 C1 H1 126.1 . . ?
N4 C2 H21 109.5 . . ?
N4 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
N4 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
N5 C3 N8 107.96(15) . . ?
N5 C3 H3 126.0 . . ?
N8 C3 H3 126.0 . . ?
N8 C4 H41 109.5 . . ?
N8 C4 H42 109.5 . . ?
H41 C4 H42 109.5 . . ?
N8 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
N9 C5 N12 109.08(16) . . ?
N9 C5 H5 125.5 . . ?
N12 C5 H5 125.5 . . ?
N12 C6 H61 109.5 . . ?
N12 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
N12 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
N21 Cu2 N21 180.00(7) 2_656 . ?
N21 Cu2 N13 89.37(6) 2_656 2_656 ?
N21 Cu2 N13 90.64(6) . 2_656 ?
N21 Cu2 N13 90.63(6) 2_656 . ?
N21 Cu2 N13 89.37(6) . . ?
N13 Cu2 N13 180.0 2_656 . ?
N21 Cu2 N17 90.84(6) 2_656 . ?
N21 Cu2 N17 89.16(6) . . ?
N13 Cu2 N17 88.55(6) 2_656 . ?
N13 Cu2 N17 91.46(6) . . ?
N21 Cu2 N17 89.16(6) 2_656 2_656 ?
N21 Cu2 N17 90.84(6) . 2_656 ?
N13 Cu2 N17 91.45(6) 2_656 2_656 ?
N13 Cu2 N17 88.55(6) . 2_656 ?
N17 Cu2 N17 180.0 . 2_656 ?
C7 N13 N14 106.60(15) . . ?
C7 N13 Cu2 130.36(12) . . ?
N14 N13 Cu2 123.04(11) . . ?
N15 N14 N13 109.62(15) . . ?
N14 N15 N16 106.84(15) . . ?
C7 N16 N15 108.92(15) . . ?
C7 N16 C8 129.94(16) . . ?
N15 N16 C8 121.13(16) . . ?
C9 N17 N18 105.28(16) . . ?
C9 N17 Cu2 132.72(13) . . ?
N18 N17 Cu2 121.93(13) . . ?
N19 N18 N17 110.38(17) . . ?
N18 N19 N20 106.62(16) . . ?
C9 N20 N19 108.20(16) . . ?
C9 N20 C10 130.39(17) . . ?
N19 N20 C10 121.19(16) . . ?
C11 N21 N22 106.55(14) . . ?
C11 N21 Cu2 130.71(13) . . ?
N22 N21 Cu2 122.73(11) . . ?
N23 N22 N21 109.41(14) . . ?
N22 N23 N24 107.34(15) . . ?
C11 N24 N23 108.32(14) . . ?
C11 N24 C12 129.59(16) . . ?
N23 N24 C12 121.74(15) . . ?
N13 C7 N16 108.02(16) . . ?
N13 C7 H7 126.0 . . ?
N16 C7 H7 126.0 . . ?
N16 C8 H81 109.5 . . ?
N16 C8 H82 109.5 . . ?
H81 C8 H82 109.5 . . ?
N16 C8 H83 109.5 . . ?
H81 C8 H83 109.5 . . ?
H82 C8 H83 109.5 . . ?
N17 C9 N20 109.50(17) . . ?
N17 C9 H9 125.2 . . ?
N20 C9 H9 125.2 . . ?
N20 C10 H101 109.5 . . ?
N20 C10 H102 109.5 . . ?
H101 C10 H102 109.5 . . ?
N20 C10 H103 109.5 . . ?
H101 C10 H103 109.5 . . ?
H102 C10 H103 109.5 . . ?
N21 C11 N24 108.36(16) . . ?
N21 C11 H11 125.8 . . ?
N24 C11 H11 125.8 . . ?
N24 C12 H121 109.5 . . ?
N24 C12 H122 109.5 . . ?
H121 C12 H122 109.5 . . ?
N24 C12 H123 109.5 . . ?
H121 C12 H123 109.5 . . ?
H122 C12 H123 109.5 . . ?
N25 Cu3 N25 180.00(9) . 2_666 ?
N25 Cu3 N29 90.26(5) . . ?
N25 Cu3 N29 89.74(5) 2_666 . ?
N25 Cu3 N29 89.74(5) . 2_666 ?
N25 Cu3 N29 90.26(5) 2_666 2_666 ?
N29 Cu3 N29 180.0 . 2_666 ?
N25 Cu3 N33 91.34(5) . 2_666 ?
N25 Cu3 N33 88.66(5) 2_666 2_666 ?
N29 Cu3 N33 91.83(5) . 2_666 ?
N29 Cu3 N33 88.17(5) 2_666 2_666 ?
N25 Cu3 N33 88.66(5) . . ?
N25 Cu3 N33 91.34(5) 2_666 . ?
N29 Cu3 N33 88.17(5) . . ?
N29 Cu3 N33 91.83(5) 2_666 . ?
N33 Cu3 N33 180.00(4) 2_666 . ?
C13 N25 N26 106.72(13) . . ?
C13 N25 Cu3 128.91(11) . . ?
N26 N25 Cu3 123.66(10) . . ?
N27 N26 N25 109.53(13) . . ?
N26 N27 N28 106.78(13) . . ?
C13 N28 N27 108.77(14) . . ?
C13 N28 C14 129.70(15) . . ?
N27 N28 C14 121.52(14) . . ?
C15 N29 N30 106.72(13) . . ?
C15 N29 Cu3 129.56(11) . . ?
N30 N29 Cu3 123.72(10) . . ?
N31 N30 N29 109.75(14) . . ?
N30 N31 N32 106.56(14) . . ?
C15 N32 N31 109.14(14) . . ?
C15 N32 C16 129.81(15) . . ?
N31 N32 C16 121.00(14) . . ?
C17 N33 N34 106.01(13) . . ?
C17 N33 Cu3 131.53(12) . . ?
N34 N33 Cu3 121.85(10) . . ?
N35 N34 N33 110.32(14) . . ?
N34 N35 N36 106.69(14) . . ?
C17 N36 N35 108.08(14) . . ?
C17 N36 C18 130.22(15) . . ?
N35 N36 C18 121.49(14) . . ?
N25 C13 N28 108.19(14) . . ?
N25 C13 H13 125.9 . . ?
N28 C13 H13 125.9 . . ?
N28 C14 H141 109.5 . . ?
N28 C14 H142 109.5 . . ?
H141 C14 H142 109.5 . . ?
N28 C14 H143 109.5 . . ?
H141 C14 H143 109.5 . . ?
H142 C14 H143 109.5 . . ?
N29 C15 N32 107.82(15) . . ?
N29 C15 H15 126.1 . . ?
N32 C15 H15 126.1 . . ?
N32 C16 H161 109.5 . . ?
N32 C16 H162 109.5 . . ?
H161 C16 H162 109.5 . . ?
N32 C16 H163 109.5 . . ?
H161 C16 H163 109.5 . . ?
H162 C16 H163 109.5 . . ?
N33 C17 N36 108.89(15) . . ?
N33 C17 H17 125.6 . . ?
N36 C17 H17 125.6 . . ?
N36 C18 H181 109.5 . . ?
N36 C18 H182 109.5 . . ?
H181 C18 H182 109.5 . . ?
N36 C18 H183 109.5 . . ?
H181 C18 H183 109.5 . . ?
H182 C18 H183 109.5 . . ?
N41 Cu4 N41 180.0 2_565 . ?
N41 Cu4 N37 89.76(6) 2_565 . ?
N41 Cu4 N37 90.24(6) . . ?
N41 Cu4 N37 90.24(6) 2_565 2_565 ?
N41 Cu4 N37 89.76(6) . 2_565 ?
N37 Cu4 N37 180.0 . 2_565 ?
N41 Cu4 N45 91.80(6) 2_565 . ?
N41 Cu4 N45 88.20(6) . . ?
N37 Cu4 N45 87.54(6) . . ?
N37 Cu4 N45 92.46(6) 2_565 . ?
N41 Cu4 N45 88.20(6) 2_565 2_565 ?
N41 Cu4 N45 91.80(6) . 2_565 ?
N37 Cu4 N45 92.46(6) . 2_565 ?
N37 Cu4 N45 87.54(6) 2_565 2_565 ?
N45 Cu4 N45 180.00(4) . 2_565 ?
C19 N37 N38 105.86(15) . . ?
C19 N37 Cu4 130.03(13) . . ?
N38 N37 Cu4 123.74(12) . . ?
N39 N38 N37 109.87(16) . . ?
N38 N39 N40 106.83(16) . . ?
C19 N40 N39 108.76(15) . . ?
C19 N40 C20 129.60(16) . . ?
N39 N40 C20 121.48(16) . . ?
C21 N41 N42 106.57(14) . . ?
C21 N41 Cu4 130.63(12) . . ?
N42 N41 Cu4 122.41(11) . . ?
N43 N42 N41 109.60(14) . . ?
N42 N43 N44 107.16(15) . . ?
C21 N44 N43 108.43(15) . . ?
C21 N44 C22 130.04(16) . . ?
N43 N44 C22 121.49(16) . . ?
C23 N45 N46 105.88(16) . . ?
C23 N45 Cu4 129.63(13) . . ?
N46 N45 Cu4 123.87(12) . . ?
N47 N46 N45 110.12(15) . . ?
N46 N47 N48 106.84(15) . . ?
C23 N48 N47 108.06(16) . . ?
C23 N48 C24 130.21(18) . . ?
N47 N48 C24 121.73(17) . . ?
N40 C19 N37 108.68(16) . . ?
N40 C19 H19 125.7 . . ?
N37 C19 H19 125.7 . . ?
N40 C20 H201 109.5 . . ?
N40 C20 H202 109.5 . . ?
H201 C20 H202 109.5 . . ?
N40 C20 H203 109.5 . . ?
H201 C20 H203 109.5 . . ?
H202 C20 H203 109.5 . . ?
N41 C21 N44 108.24(16) . . ?
N41 C21 H219 125.9 . . ?
N44 C21 H219 125.9 . . ?
N44 C22 H221 109.5 . . ?
N44 C22 H222 109.5 . . ?
H221 C22 H222 109.5 . . ?
N44 C22 H223 109.5 . . ?
H221 C22 H223 109.5 . . ?
H222 C22 H223 109.5 . . ?
N45 C23 N48 109.10(17) . . ?
N45 C23 H231 125.4 . . ?
N48 C23 H231 125.4 . . ?
N48 C24 H241 109.5 . . ?
N48 C24 H242 109.5 . . ?
H241 C24 H242 109.5 . . ?
N48 C24 H243 109.5 . . ?
H241 C24 H243 109.5 . . ?
H242 C24 H243 109.5 . . ?
O1 Cl1 O3 109.77(9) . . ?
O1 Cl1 O4 109.86(9) . . ?
O3 Cl1 O4 109.38(10) . . ?
O1 Cl1 O2 109.33(9) . . ?
O3 Cl1 O2 109.64(9) . . ?
O4 Cl1 O2 108.85(9) . . ?
O6 Cl2 O8 110.42(11) . . ?
O6 Cl2 O5 109.32(12) . . ?
O8 Cl2 O5 110.32(10) . . ?
O6 Cl2 O7 107.92(11) . . ?
O8 Cl2 O7 110.00(11) . . ?
O5 Cl2 O7 108.80(11) . . ?
O9 Cl3 O11 109.84(9) . . ?
O9 Cl3 O12 109.89(9) . . ?
O11 Cl3 O12 109.26(9) . . ?
O9 Cl3 O10 109.43(9) . . ?
O11 Cl3 O10 109.54(8) . . ?
O12 Cl3 O10 108.87(9) . . ?
O15 Cl4 O14 111.71(16) . . ?
O15 Cl4 O13 112.82(13) . . ?
O14 Cl4 O13 108.92(13) . . ?
O15 Cl4 O16 110.00(16) . . ?
O14 Cl4 O16 106.31(14) . . ?
O13 Cl4 O16 106.76(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.01(19) . . . . ?
Cu1 N1 N2 N3 -178.64(11) . . . . ?
N1 N2 N3 N4 0.17(19) . . . . ?
N2 N3 N4 C1 -0.26(19) . . . . ?
N2 N3 N4 C2 -177.68(15) . . . . ?
C3 N5 N6 N7 -0.30(19) . . . . ?
Cu1 N5 N6 N7 170.31(12) . . . . ?
N5 N6 N7 N8 -0.10(19) . . . . ?
N6 N7 N8 C3 0.5(2) . . . . ?
N6 N7 N8 C4 -179.15(17) . . . . ?
C5 N9 N10 N11 0.1(2) . . . . ?
Cu1 N9 N10 N11 -164.61(13) . . . . ?
N9 N10 N11 N12 -0.1(2) . . . . ?
N10 N11 N12 C5 0.1(2) . . . . ?
N10 N11 N12 C6 -177.60(17) . . . . ?
N2 N1 C1 N4 -0.15(18) . . . . ?
Cu1 N1 C1 N4 178.37(11) . . . . ?
N3 N4 C1 N1 0.25(19) . . . . ?
C2 N4 C1 N1 177.38(16) . . . . ?
N6 N5 C3 N8 0.59(19) . . . . ?
Cu1 N5 C3 N8 -169.76(11) . . . . ?
N7 N8 C3 N5 -0.7(2) . . . . ?
C4 N8 C3 N5 178.93(17) . . . . ?
N10 N9 C5 N12 0.0(2) . . . . ?
Cu1 N9 C5 N12 162.54(12) . . . . ?
N11 N12 C5 N9 -0.1(2) . . . . ?
C6 N12 C5 N9 177.40(18) . . . . ?
C7 N13 N14 N15 0.0(2) . . . . ?
Cu2 N13 N14 N15 179.90(12) . . . . ?
N13 N14 N15 N16 0.3(2) . . . . ?
N14 N15 N16 C7 -0.6(2) . . . . ?
N14 N15 N16 C8 -179.41(18) . . . . ?
C9 N17 N18 N19 0.0(2) . . . . ?
Cu2 N17 N18 N19 -177.36(13) . . . . ?
N17 N18 N19 N20 0.5(2) . . . . ?
N18 N19 N20 C9 -0.8(2) . . . . ?
N18 N19 N20 C10 -176.04(17) . . . . ?
C11 N21 N22 N23 0.0(2) . . . . ?
Cu2 N21 N22 N23 -179.55(13) . . . . ?
N21 N22 N23 N24 -0.6(2) . . . . ?
N22 N23 N24 C11 0.9(2) . . . . ?
N22 N23 N24 C12 174.76(18) . . . . ?
N14 N13 C7 N16 -0.4(2) . . . . ?
Cu2 N13 C7 N16 179.76(12) . . . . ?
N15 N16 C7 N13 0.6(2) . . . . ?
C8 N16 C7 N13 179.29(19) . . . . ?
N18 N17 C9 N20 -0.5(2) . . . . ?
Cu2 N17 C9 N20 176.43(12) . . . . ?
N19 N20 C9 N17 0.8(2) . . . . ?
C10 N20 C9 N17 175.47(17) . . . . ?
N22 N21 C11 N24 0.6(2) . . . . ?
Cu2 N21 C11 N24 -179.91(12) . . . . ?
N23 N24 C11 N21 -0.9(2) . . . . ?
C12 N24 C11 N21 -174.12(18) . . . . ?
C13 N25 N26 N27 0.49(18) . . . . ?
Cu3 N25 N26 N27 -170.59(11) . . . . ?
N25 N26 N27 N28 0.08(18) . . . . ?
N26 N27 N28 C13 -0.63(18) . . . . ?
N26 N27 N28 C14 179.79(15) . . . . ?
C15 N29 N30 N31 0.18(19) . . . . ?
Cu3 N29 N30 N31 -179.81(11) . . . . ?
N29 N30 N31 N32 -0.08(19) . . . . ?
N30 N31 N32 C15 -0.05(18) . . . . ?
N30 N31 N32 C16 -177.54(15) . . . . ?
C17 N33 N34 N35 0.0(2) . . . . ?
Cu3 N33 N34 N35 172.08(12) . . . . ?
N33 N34 N35 N36 -0.5(2) . . . . ?
N34 N35 N36 C17 0.7(2) . . . . ?
N34 N35 N36 C18 176.03(17) . . . . ?
N26 N25 C13 N28 -0.87(18) . . . . ?
Cu3 N25 C13 N28 169.58(11) . . . . ?
N27 N28 C13 N25 0.94(19) . . . . ?
C14 N28 C13 N25 -179.51(17) . . . . ?
N30 N29 C15 N32 -0.20(18) . . . . ?
Cu3 N29 C15 N32 179.78(11) . . . . ?
N31 N32 C15 N29 0.16(18) . . . . ?
C16 N32 C15 N29 177.36(16) . . . . ?
N34 N33 C17 N36 0.41(19) . . . . ?
Cu3 N33 C17 N36 -170.55(11) . . . . ?
N35 N36 C17 N33 -0.7(2) . . . . ?
C18 N36 C17 N33 -175.48(17) . . . . ?
C19 N37 N38 N39 0.1(2) . . . . ?
Cu4 N37 N38 N39 -173.46(14) . . . . ?
N37 N38 N39 N40 0.3(2) . . . . ?
N38 N39 N40 C19 -0.6(2) . . . . ?
N38 N39 N40 C20 -176.50(17) . . . . ?
C21 N41 N42 N43 -0.1(2) . . . . ?
Cu4 N41 N42 N43 173.50(13) . . . . ?
N41 N42 N43 N44 0.0(2) . . . . ?
N42 N43 N44 C21 0.2(2) . . . . ?
N42 N43 N44 C22 177.93(17) . . . . ?
C23 N45 N46 N47 -0.1(2) . . . . ?
Cu4 N45 N46 N47 171.67(12) . . . . ?
N45 N46 N47 N48 -0.3(2) . . . . ?
N46 N47 N48 C23 0.6(2) . . . . ?
N46 N47 N48 C24 -179.11(18) . . . . ?
N39 N40 C19 N37 0.6(2) . . . . ?
C20 N40 C19 N37 176.13(16) . . . . ?
N38 N37 C19 N40 -0.4(2) . . . . ?
Cu4 N37 C19 N40 172.55(12) . . . . ?
N42 N41 C21 N44 0.2(2) . . . . ?
Cu4 N41 C21 N44 -172.67(12) . . . . ?
N43 N44 C21 N41 -0.3(2) . . . . ?
C22 N44 C21 N41 -177.74(18) . . . . ?
N46 N45 C23 N48 0.4(2) . . . . ?
Cu4 N45 C23 N48 -170.66(12) . . . . ?
N47 N48 C23 N45 -0.6(2) . . . . ?
C24 N48 C23 N45 179.03(19) . . . . ?

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         0.790
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.076

_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_lx267
_database_code_depnum_ccdc_archive 'CCDC 1566372'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed May 25 14:07:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(1-methyltetrazolyl) nickel(II) dipicrate
;
_chemical_name_common            
'diaqua tetrakis(1-methyltetrazolyl) nickel(II) dipicrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' 	C8 H20 N16 Ni O2, 2(C6 H2 N3 O7)'
_chemical_formula_sum            'C20 H24 N22 Ni O16'
_chemical_formula_weight         887.32

_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                   13.5772(4)
_cell_length_b                   16.6129(6)
_cell_length_c                   7.5443(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.707(3)
_cell_angle_gamma                90
_cell_volume                     1677.30(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3621
_cell_measurement_theta_min      4.4690
_cell_measurement_theta_max      28.2170

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.688
_shelx_estimated_absorpt_T_min   0.836
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_F_000             908
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            10946
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.154
_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             3283
_reflns_number_gt                2791
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0341P)²+0.7411P] 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         3283
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0738
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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      -0.0181711000
_diffrn_orient_matrix_UB_12      -0.0400887000
_diffrn_orient_matrix_UB_13      -0.0048521000
_diffrn_orient_matrix_UB_21      0.0005166000
_diffrn_orient_matrix_UB_22      -0.0004827000
_diffrn_orient_matrix_UB_23      -0.0938911000
_diffrn_orient_matrix_UB_31      0.0497841000
_diffrn_orient_matrix_UB_32      -0.0146334000
_diffrn_orient_matrix_UB_33      0.0163664000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   57.0000   90.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -99.0000  120.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  -57.0000  -60.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  -99.0000 -120.0000 89

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  -77.0000 -150.0000 33

#__ type_ start__ end____ width___ exp.time_
  6 omega  -81.00  -44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931 -179.0000   30.0000 37

;



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'
Ni Ni 0.3393 1.1124 '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
Ni01 Ni 0.0000 0.5000 0.0000 0.01417(11) Uani 1 2 d S . P . .
O1 O 0.13489(11) 0.47308(9) 0.1607(2) 0.0198(3) Uani 1 1 d . . . . .
N1 N 0.05732(11) 0.60558(10) -0.0929(2) 0.0163(3) Uani 1 1 d . . . . .
N2 N 0.00113(11) 0.67398(10) -0.1176(2) 0.0201(4) Uani 1 1 d . . . . .
N3 N 0.04887(12) 0.72939(10) -0.1886(2) 0.0208(4) Uani 1 1 d . . . . .
N4 N 0.13729(11) 0.69719(10) -0.2109(2) 0.0167(3) Uani 1 1 d . . . . .
N5 N -0.04062(11) 0.56344(10) 0.2127(2) 0.0167(3) Uani 1 1 d . . . . .
N6 N 0.02512(11) 0.57026(10) 0.3697(2) 0.0177(3) Uani 1 1 d . . . . .
N7 N -0.01233(11) 0.61399(10) 0.4822(2) 0.0181(4) Uani 1 1 d . . . . .
N8 N -0.10399(11) 0.63674(10) 0.3987(2) 0.0159(3) Uani 1 1 d . . . . .
C1 C 0.14110(14) 0.62205(12) -0.1521(3) 0.0174(4) Uani 1 1 d . . . . .
C2 C 0.21016(15) 0.74505(13) -0.2865(3) 0.0229(4) Uani 1 1 d . . . . .
H2A H 0.2738 0.7454 -0.2028 0.034 Uiso 1 1 calc R U . . .
H2B H 0.1855 0.8003 -0.3061 0.034 Uiso 1 1 calc R U . . .
H2C H 0.2202 0.7216 -0.4014 0.034 Uiso 1 1 calc R U . . .
C3 C -0.12003(14) 0.60536(12) 0.2349(3) 0.0177(4) Uani 1 1 d . . . . .
C4 C -0.16724(14) 0.68993(12) 0.4864(3) 0.0222(4) Uani 1 1 d . . . . .
H4A H -0.1356 0.7430 0.5057 0.033 Uiso 1 1 calc R U . . .
H4B H -0.1757 0.6669 0.6025 0.033 Uiso 1 1 calc R U . . .
H4C H -0.2327 0.6955 0.4098 0.033 Uiso 1 1 calc R U . . .
O2 O 0.36873(12) -0.16025(10) 0.5110(2) 0.0336(4) Uani 1 1 d . . . . .
O3 O 0.46383(12) -0.19969(9) 0.7554(2) 0.0350(4) Uani 1 1 d . . . . .
O4 O 0.30361(10) -0.00755(9) 0.5440(2) 0.0236(3) Uani 1 1 d . . . . .
O5 O 0.33040(11) 0.15888(10) 0.4950(2) 0.0336(4) Uani 1 1 d . . . . .
O6 O 0.35106(11) 0.19231(10) 0.7771(2) 0.0350(4) Uani 1 1 d . . . . .
O7 O 0.73758(10) -0.02234(9) 0.9782(2) 0.0309(4) Uani 1 1 d . . . . .
O8 O 0.70189(10) 0.10191(9) 1.0209(2) 0.0321(4) Uani 1 1 d . . . . .
N9 N 0.42853(12) -0.14689(11) 0.6498(2) 0.0226(4) Uani 1 1 d . . . . .
N10 N 0.36550(11) 0.14808(11) 0.6545(2) 0.0216(4) Uani 1 1 d . . . . .
N11 N 0.68012(11) 0.03562(10) 0.9555(2) 0.0198(4) Uani 1 1 d . . . . .
C5 C 0.38973(13) 0.00082(12) 0.6333(3) 0.0171(4) Uani 1 1 d . . . . .
C6 C 0.45868(13) -0.06364(12) 0.6922(3) 0.0179(4) Uani 1 1 d . . . . .
C7 C 0.55149(14) -0.05299(13) 0.7946(3) 0.0182(4) Uani 1 1 d . . . . .
C8 C 0.58248(13) 0.02390(12) 0.8483(3) 0.0167(4) Uani 1 1 d . . . . .
C9 C 0.52041(14) 0.09034(12) 0.8055(3) 0.0168(4) Uani 1 1 d . . . . .
C10 C 0.42950(13) 0.07735(12) 0.7000(3) 0.0172(4) Uani 1 1 d . . . . .
H9 H 0.5403(15) 0.1415(14) 0.846(3) 0.019(5) Uiso 1 1 d . . . . .
H1 H 0.1943(14) 0.5901(12) -0.145(3) 0.011(5) Uiso 1 1 d . . . . .
H7 H 0.5889(15) -0.0950(13) 0.831(3) 0.016(5) Uiso 1 1 d . . . . .
H12 H 0.190(2) 0.4830(15) 0.130(3) 0.032(7) Uiso 1 1 d . . . . .
H11 H 0.1432(18) 0.4909(16) 0.263(4) 0.035(8) Uiso 1 1 d . . . . .
H3 H -0.1776(16) 0.6102(13) 0.151(3) 0.022(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
Ni01 O1 2.0678(14) . ?
Ni01 O1 2.0678(14) 3_565 ?
Ni01 N5 2.0707(16) 3_565 ?
Ni01 N5 2.0707(16) . ?
Ni01 N1 2.0874(16) . ?
Ni01 N1 2.0874(16) 3_565 ?
O1 H12 0.84(3) . ?
O1 H11 0.82(3) . ?
N1 C1 1.319(2) . ?
N1 N2 1.364(2) . ?
N2 N3 1.293(2) . ?
N3 N4 1.351(2) . ?
N4 C1 1.323(3) . ?
N4 C2 1.458(2) . ?
N5 C3 1.318(2) . ?
N5 N6 1.363(2) . ?
N6 N7 1.285(2) . ?
N7 N8 1.351(2) . ?
N8 C3 1.325(3) . ?
N8 C4 1.466(2) . ?
C1 H1 0.89(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.92(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
O2 N9 1.232(2) . ?
O3 N9 1.227(2) . ?
O4 C5 1.255(2) . ?
O5 N10 1.230(2) . ?
O6 N10 1.222(2) . ?
O7 N11 1.233(2) . ?
O8 N11 1.223(2) . ?
N9 C6 1.463(2) . ?
N10 C10 1.467(2) . ?
N11 C8 1.445(2) . ?
C5 C10 1.439(3) . ?
C5 C6 1.442(3) . ?
C6 C7 1.374(3) . ?
C7 C8 1.384(3) . ?
C7 H7 0.88(2) . ?
C8 C9 1.393(3) . ?
C9 C10 1.368(3) . ?
C9 H9 0.93(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 Ni01 O1 180.0 . 3_565 ?
O1 Ni01 N5 91.09(6) . 3_565 ?
O1 Ni01 N5 88.91(6) 3_565 3_565 ?
O1 Ni01 N5 88.91(6) . . ?
O1 Ni01 N5 91.09(6) 3_565 . ?
N5 Ni01 N5 180.00(7) 3_565 . ?
O1 Ni01 N1 92.01(6) . . ?
O1 Ni01 N1 87.99(6) 3_565 . ?
N5 Ni01 N1 90.26(6) 3_565 . ?
N5 Ni01 N1 89.75(6) . . ?
O1 Ni01 N1 87.99(6) . 3_565 ?
O1 Ni01 N1 92.01(6) 3_565 3_565 ?
N5 Ni01 N1 89.74(6) 3_565 3_565 ?
N5 Ni01 N1 90.25(6) . 3_565 ?
N1 Ni01 N1 180.0 . 3_565 ?
Ni01 O1 H12 122.5(17) . . ?
Ni01 O1 H11 116.3(18) . . ?
H12 O1 H11 102(2) . . ?
C1 N1 N2 105.98(16) . . ?
C1 N1 Ni01 132.82(13) . . ?
N2 N1 Ni01 120.96(11) . . ?
N3 N2 N1 110.01(15) . . ?
N2 N3 N4 106.72(15) . . ?
C1 N4 N3 108.50(15) . . ?
C1 N4 C2 130.91(16) . . ?
N3 N4 C2 120.58(16) . . ?
C3 N5 N6 105.98(15) . . ?
C3 N5 Ni01 134.28(13) . . ?
N6 N5 Ni01 119.67(11) . . ?
N7 N6 N5 110.30(14) . . ?
N6 N7 N8 106.63(15) . . ?
C3 N8 N7 108.58(15) . . ?
C3 N8 C4 129.92(17) . . ?
N7 N8 C4 121.46(16) . . ?
N1 C1 N4 108.79(17) . . ?
N1 C1 H1 126.3(13) . . ?
N4 C1 H1 124.7(13) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.51(17) . . ?
N5 C3 H3 125.2(14) . . ?
N8 C3 H3 126.3(14) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 N9 O2 123.54(17) . . ?
O3 N9 C6 118.00(17) . . ?
O2 N9 C6 118.45(17) . . ?
O6 N10 O5 124.54(18) . . ?
O6 N10 C10 117.94(17) . . ?
O5 N10 C10 117.51(17) . . ?
O8 N11 O7 122.89(16) . . ?
O8 N11 C8 118.94(16) . . ?
O7 N11 C8 118.17(17) . . ?
O4 C5 C10 123.14(18) . . ?
O4 C5 C6 125.50(18) . . ?
C10 C5 C6 111.25(16) . . ?
C7 C6 C5 124.32(18) . . ?
C7 C6 N9 116.18(17) . . ?
C5 C6 N9 119.44(16) . . ?
C6 C7 C8 119.22(18) . . ?
C6 C7 H7 119.9(14) . . ?
C8 C7 H7 120.8(14) . . ?
C7 C8 C9 121.42(17) . . ?
C7 C8 N11 119.55(17) . . ?
C9 C8 N11 119.01(17) . . ?
C10 C9 C8 117.45(18) . . ?
C10 C9 H9 121.2(13) . . ?
C8 C9 H9 121.3(13) . . ?
C9 C10 C5 126.26(18) . . ?
C9 C10 N10 116.77(17) . . ?
C5 C10 N10 116.95(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 0.0(2) . . . . ?
Ni01 N1 N2 N3 -175.03(12) . . . . ?
N1 N2 N3 N4 0.0(2) . . . . ?
N2 N3 N4 C1 0.0(2) . . . . ?
N2 N3 N4 C2 -179.11(16) . . . . ?
C3 N5 N6 N7 0.1(2) . . . . ?
Ni01 N5 N6 N7 177.68(12) . . . . ?
N5 N6 N7 N8 -0.2(2) . . . . ?
N6 N7 N8 C3 0.2(2) . . . . ?
N6 N7 N8 C4 -177.92(16) . . . . ?
N2 N1 C1 N4 0.0(2) . . . . ?
Ni01 N1 C1 N4 174.18(13) . . . . ?
N3 N4 C1 N1 0.0(2) . . . . ?
C2 N4 C1 N1 178.96(18) . . . . ?
N6 N5 C3 N8 0.0(2) . . . . ?
Ni01 N5 C3 N8 -177.02(13) . . . . ?
N7 N8 C3 N5 -0.1(2) . . . . ?
C4 N8 C3 N5 177.78(18) . . . . ?
O4 C5 C6 C7 -177.95(18) . . . . ?
C10 C5 C6 C7 -1.7(3) . . . . ?
O4 C5 C6 N9 -1.0(3) . . . . ?
C10 C5 C6 N9 175.28(16) . . . . ?
O3 N9 C6 C7 27.8(2) . . . . ?
O2 N9 C6 C7 -152.74(18) . . . . ?
O3 N9 C6 C5 -149.46(18) . . . . ?
O2 N9 C6 C5 30.0(3) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
N9 C6 C7 C8 -176.38(17) . . . . ?
C6 C7 C8 C9 2.0(3) . . . . ?
C6 C7 C8 N11 -179.78(17) . . . . ?
O8 N11 C8 C7 -170.96(18) . . . . ?
O7 N11 C8 C7 8.3(3) . . . . ?
O8 N11 C8 C9 7.3(3) . . . . ?
O7 N11 C8 C9 -173.44(17) . . . . ?
C7 C8 C9 C10 -3.4(3) . . . . ?
N11 C8 C9 C10 178.39(16) . . . . ?
C8 C9 C10 C5 2.3(3) . . . . ?
C8 C9 C10 N10 -179.35(16) . . . . ?
O4 C5 C10 C9 176.50(18) . . . . ?
C6 C5 C10 C9 0.2(3) . . . . ?
O4 C5 C10 N10 -1.8(3) . . . . ?
C6 C5 C10 N10 -178.19(16) . . . . ?
O6 N10 C10 C9 -50.5(2) . . . . ?
O5 N10 C10 C9 129.18(19) . . . . ?
O6 N10 C10 C5 128.01(19) . . . . ?
O5 N10 C10 C5 -52.3(2) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H12 O4 0.84(3) 1.82(3) 2.652(2) 175(3) 4_565
O1 H11 O7 0.82(3) 2.33(3) 2.972(2) 136(2) 2_656
O1 H11 N6 0.82(3) 2.32(3) 2.847(2) 123(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         0.307
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.058

_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_lx269
_database_code_depnum_ccdc_archive 'CCDC 1566375'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu May 26 10:35:15 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(1-methyltetrazolyl) bis(picryl) copper(II)
;
_chemical_name_common            
'bis(1-methyltetrazolyl) bis(picryl) copper(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H12 Cu N14 O14'
_chemical_formula_weight         687.94

_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                   10.9660(6)
_cell_length_b                   5.7912(4)
_cell_length_c                   19.6839(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.344(5)
_cell_angle_gamma                90
_cell_volume                     1249.71(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2309
_cell_measurement_theta_min      4.4530
_cell_measurement_theta_max      29.2100

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.976
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_F_000             694
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            8943
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.123
_diffrn_reflns_theta_max         25.998
_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             2447
_reflns_number_gt                1937
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0825P)²+0.1332P] 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         2447
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1358
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.015
_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      -0.0376013000
_diffrn_orient_matrix_UB_12      0.0602896000
_diffrn_orient_matrix_UB_13      -0.0238326000
_diffrn_orient_matrix_UB_21      -0.0517406000
_diffrn_orient_matrix_UB_22      -0.0241481000
_diffrn_orient_matrix_UB_23      0.0197608000
_diffrn_orient_matrix_UB_31      0.0098195000
_diffrn_orient_matrix_UB_32      0.1038256000
_diffrn_orient_matrix_UB_33      0.0184560000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -21.00   21.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033  -99.0000 -120.0000 42

#__ type_ start__ end____ width___ exp.time_
  2 omega  -37.00   16.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033   57.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   16.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033  -99.0000  120.0000 29

#__ type_ start__ end____ width___ exp.time_
  4 omega -100.00  -47.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033 -179.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega -106.00  -70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033  179.0000  -60.0000 36

#__ type_ start__ end____ width___ exp.time_
  6 omega -102.00  -71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033 -179.0000 -120.0000 31

#__ type_ start__ end____ width___ exp.time_
  7 omega  -92.00   42.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1033  -19.0000  -90.0000 134

#__ type_ start__ end____ width___ exp.time_
  8 omega   16.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.1971   38.0000  -90.0000 82

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.0000 0.0234(2) Uani 1 2 d S . P . .
O1 O 1.1486(2) 0.3971(4) 0.18182(12) 0.0343(6) Uani 1 1 d . . . . .
O2 O 1.0559(2) 0.6689(4) 0.23530(12) 0.0388(6) Uani 1 1 d . . . . .
O3 O 0.6645(2) 0.9194(5) 0.15856(13) 0.0422(7) Uani 1 1 d . . . . .
O4 O 0.58550(19) 0.8077(4) 0.06303(11) 0.0296(5) Uani 1 1 d . . . . .
O5 O 0.8626(2) 0.2081(4) -0.06276(11) 0.0336(6) Uani 1 1 d . . . . .
O6 O 0.8705(2) -0.0655(4) 0.01222(13) 0.0329(6) Uani 1 1 d . . . . .
O7 O 0.66679(19) 0.3972(4) 0.01002(11) 0.0270(5) Uani 1 1 d . . . . .
N1 N 1.0604(2) 0.5217(5) 0.19045(14) 0.0265(6) Uani 1 1 d . . . . .
N2 N 0.6629(2) 0.7907(5) 0.10989(14) 0.0261(6) Uani 1 1 d . . . . .
N3 N 0.8654(2) 0.1388(5) -0.00378(13) 0.0237(6) Uani 1 1 d . . . . .
N4 N 0.4548(2) 0.3334(5) 0.08486(13) 0.0262(6) Uani 1 1 d . . . . .
N5 N 0.4932(3) 0.4033(5) 0.14780(14) 0.0325(7) Uani 1 1 d . . . . .
N6 N 0.4500(3) 0.2669(5) 0.19291(14) 0.0330(7) Uani 1 1 d . . . . .
N7 N 0.3836(2) 0.1067(5) 0.15992(13) 0.0269(6) Uani 1 1 d . . . . .
C1 C 0.8617(3) 0.3102(5) 0.05042(15) 0.0214(6) Uani 1 1 d . . . . .
C2 C 0.9595(3) 0.3270(6) 0.09463(15) 0.0240(7) Uani 1 1 d . . . . .
C3 C 0.9546(3) 0.4958(5) 0.14461(16) 0.0231(7) Uani 1 1 d . . . . .
C4 C 0.8563(3) 0.6412(6) 0.15006(16) 0.0243(7) Uani 1 1 d . . . . .
C5 C 0.7575(3) 0.6157(5) 0.10487(15) 0.0236(7) Uani 1 1 d . . . . .
C6 C 0.7527(3) 0.4447(6) 0.05256(15) 0.0229(7) Uani 1 1 d . . . . .
C7 C 0.3873(3) 0.1492(6) 0.09409(17) 0.0291(7) Uani 1 1 d . . . . .
C8 C 0.3218(3) -0.0762(7) 0.19663(18) 0.0378(8) Uani 1 1 d . . . . .
H8A H 0.2343 -0.0428 0.1977 0.057 Uiso 1 1 calc R U . . .
H8B H 0.3551 -0.0847 0.2432 0.057 Uiso 1 1 calc R U . . .
H8C H 0.3346 -0.2241 0.1737 0.057 Uiso 1 1 calc R U . . .
H4 H 0.852(3) 0.762(6) 0.1811(16) 0.020(8) Uiso 1 1 d . . . . .
H2 H 1.027(3) 0.242(5) 0.0884(15) 0.014(7) Uiso 1 1 d . . . . .
H7 H 0.350(3) 0.059(6) 0.0597(18) 0.021(8) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O7 1.929(2) . ?
Cu1 O7 1.929(2) 3_665 ?
Cu1 N4 2.001(3) . ?
Cu1 N4 2.001(3) 3_665 ?
Cu1 O4 2.354(2) 3_665 ?
Cu1 O4 2.354(2) . ?
O1 N1 1.222(4) . ?
O2 N1 1.229(3) . ?
O3 N2 1.214(3) . ?
O4 N2 1.243(3) . ?
O5 N3 1.228(3) . ?
O6 N3 1.225(4) . ?
O7 C6 1.276(4) . ?
N1 C3 1.460(4) . ?
N2 C5 1.455(4) . ?
N3 C1 1.459(4) . ?
N4 C7 1.314(4) . ?
N4 N5 1.361(4) . ?
N5 N6 1.287(4) . ?
N6 N7 1.338(4) . ?
N7 C7 1.320(4) . ?
N7 C8 1.458(5) . ?
C1 C2 1.369(4) . ?
C1 C6 1.428(4) . ?
C2 C3 1.389(4) . ?
C2 H2 0.90(3) . ?
C3 C4 1.375(4) . ?
C4 C5 1.393(4) . ?
C4 H4 0.93(3) . ?
C5 C6 1.428(4) . ?
C7 H7 0.94(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Cu1 O7 180.0 . 3_665 ?
O7 Cu1 N4 91.07(10) . . ?
O7 Cu1 N4 88.93(10) 3_665 . ?
O7 Cu1 N4 88.93(10) . 3_665 ?
O7 Cu1 N4 91.07(10) 3_665 3_665 ?
N4 Cu1 N4 180.0 . 3_665 ?
O7 Cu1 O4 100.68(8) . 3_665 ?
O7 Cu1 O4 79.32(8) 3_665 3_665 ?
N4 Cu1 O4 88.36(9) . 3_665 ?
N4 Cu1 O4 91.63(9) 3_665 3_665 ?
O7 Cu1 O4 79.32(8) . . ?
O7 Cu1 O4 100.68(8) 3_665 . ?
N4 Cu1 O4 91.64(9) . . ?
N4 Cu1 O4 88.37(9) 3_665 . ?
O4 Cu1 O4 180.00(9) 3_665 . ?
N2 O4 Cu1 126.01(19) . . ?
C6 O7 Cu1 133.2(2) . . ?
O1 N1 O2 123.6(3) . . ?
O1 N1 C3 118.2(3) . . ?
O2 N1 C3 118.1(3) . . ?
O3 N2 O4 122.3(3) . . ?
O3 N2 C5 119.0(2) . . ?
O4 N2 C5 118.7(2) . . ?
O6 N3 O5 124.0(3) . . ?
O6 N3 C1 118.1(2) . . ?
O5 N3 C1 117.9(3) . . ?
C7 N4 N5 106.2(3) . . ?
C7 N4 Cu1 131.2(2) . . ?
N5 N4 Cu1 122.6(2) . . ?
N6 N5 N4 109.5(3) . . ?
N5 N6 N7 107.2(3) . . ?
C7 N7 N6 108.6(3) . . ?
C7 N7 C8 130.3(3) . . ?
N6 N7 C8 121.1(3) . . ?
C2 C1 C6 125.9(3) . . ?
C2 C1 N3 118.6(3) . . ?
C6 C1 N3 115.5(2) . . ?
C1 C2 C3 117.2(3) . . ?
C1 C2 H2 121(2) . . ?
C3 C2 H2 122(2) . . ?
C4 C3 C2 122.0(3) . . ?
C4 C3 N1 120.1(3) . . ?
C2 C3 N1 117.8(3) . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H4 124(2) . . ?
C5 C4 H4 117(2) . . ?
C4 C5 C6 123.3(3) . . ?
C4 C5 N2 115.3(3) . . ?
C6 C5 N2 121.2(3) . . ?
O7 C6 C1 117.9(3) . . ?
O7 C6 C5 129.6(3) . . ?
C1 C6 C5 112.5(3) . . ?
N4 C7 N7 108.5(3) . . ?
N4 C7 H7 126(2) . . ?
N7 C7 H7 125(2) . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O4 N2 O3 -145.7(3) . . . . ?
Cu1 O4 N2 C5 36.5(4) . . . . ?
C7 N4 N5 N6 -0.3(4) . . . . ?
Cu1 N4 N5 N6 179.4(2) . . . . ?
N4 N5 N6 N7 0.3(3) . . . . ?
N5 N6 N7 C7 -0.1(4) . . . . ?
N5 N6 N7 C8 179.8(3) . . . . ?
O6 N3 C1 C2 63.1(4) . . . . ?
O5 N3 C1 C2 -117.3(3) . . . . ?
O6 N3 C1 C6 -116.0(3) . . . . ?
O5 N3 C1 C6 63.6(3) . . . . ?
C6 C1 C2 C3 -2.6(5) . . . . ?
N3 C1 C2 C3 178.4(3) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C1 C2 C3 N1 -177.6(3) . . . . ?
O1 N1 C3 C4 -176.3(3) . . . . ?
O2 N1 C3 C4 3.2(4) . . . . ?
O1 N1 C3 C2 1.4(4) . . . . ?
O2 N1 C3 C2 -179.1(3) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
N1 C3 C4 C5 178.8(3) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C3 C4 C5 N2 -174.2(3) . . . . ?
O3 N2 C5 C4 -12.4(4) . . . . ?
O4 N2 C5 C4 165.4(3) . . . . ?
O3 N2 C5 C6 173.3(3) . . . . ?
O4 N2 C5 C6 -8.9(4) . . . . ?
Cu1 O7 C6 C1 171.3(2) . . . . ?
Cu1 O7 C6 C5 -7.7(5) . . . . ?
C2 C1 C6 O7 -175.6(3) . . . . ?
N3 C1 C6 O7 3.4(4) . . . . ?
C2 C1 C6 C5 3.6(4) . . . . ?
N3 C1 C6 C5 -177.4(2) . . . . ?
C4 C5 C6 O7 176.9(3) . . . . ?
N2 C5 C6 O7 -9.3(5) . . . . ?
C4 C5 C6 C1 -2.2(4) . . . . ?
N2 C5 C6 C1 171.7(3) . . . . ?
N5 N4 C7 N7 0.2(3) . . . . ?
Cu1 N4 C7 N7 -179.4(2) . . . . ?
N6 N7 C7 N4 0.0(4) . . . . ?
C8 N7 C7 N4 -179.9(3) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C8 H8B N5 0.98 2.68 3.635(5) 163.5 2_645
C8 H8B N6 0.98 2.60 3.400(5) 138.8 2_645
C2 H2 O6 0.90(3) 2.52(3) 3.221(4) 136(2) 3_755
C7 H7 O4 0.94(4) 2.65(3) 3.124(4) 112(2) 3_665
C8 H8B N5 0.98 2.68 3.635(5) 163.5 2_645
C8 H8B N6 0.98 2.60 3.400(5) 138.8 2_645
C2 H2 O6 0.90(3) 2.52(3) 3.221(4) 136(2) 3_755
C7 H7 O4 0.94(4) 2.65(3) 3.124(4) 112(2) 3_665

_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         0.955
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.104

_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_lx215
_database_code_depnum_ccdc_archive 'CCDC 1566369'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Apr 28 06:28:41 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(1-methyltetrazolyl) bis(trinitroresorcinoyl) zinc(II)
;
_chemical_name_common            
'bis(1-methyltetrazolyl) bis(trinitroresorcinoyl) zinc(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 N14 O16 Zn'
_chemical_formula_sum            'C16 H12 N14 O16 Zn'
_chemical_formula_weight         721.77

_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                   9.6200(3)
_cell_length_b                   11.4310(4)
_cell_length_c                   12.0220(3)
_cell_angle_alpha                81.920(2)
_cell_angle_beta                 82.467(2)
_cell_angle_gamma                74.196(3)
_cell_volume                     1253.42(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    11185
_cell_measurement_theta_min      4.3220
_cell_measurement_theta_max      32.1220

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    1.092
_shelx_estimated_absorpt_T_min   0.657
_shelx_estimated_absorpt_T_max   0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93702
_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    1.912
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            18110
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.268
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_full        25.240
_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             4898
_reflns_number_gt                4608
_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)+(0.0289P)²+0.6994P] 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         4898
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0594
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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      0.0061111000
_diffrn_orient_matrix_UB_12      -0.0205356000
_diffrn_orient_matrix_UB_13      -0.0538642000
_diffrn_orient_matrix_UB_21      -0.0674779000
_diffrn_orient_matrix_UB_22      0.0417865000
_diffrn_orient_matrix_UB_23      -0.0110671000
_diffrn_orient_matrix_UB_31      0.0365797000
_diffrn_orient_matrix_UB_32      0.0451838000
_diffrn_orient_matrix_UB_33      -0.0236962000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -9.00  104.40   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000   60.0000 162

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00   66.90   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 127

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   72.30   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 139

#__ type_ start__ end____ width___ exp.time_
  4 omega  -35.00   96.60   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000  -90.0000 188

#__ type_ start__ end____ width___ exp.time_
  5 omega  -64.00    3.90   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000    0.0000 97

#__ type_ start__ end____ width___ exp.time_
  6 omega  -60.00    4.40   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  7 omega  -93.00    2.90   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  -90.0000 137

#__ type_ start__ end____ width___ exp.time_
  8 omega -101.00    4.00   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000   90.0000 150

#__ type_ start__ end____ width___ exp.time_
  9 omega -107.00  -51.70   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -90.0000 79

#__ type_ start__ end____ width___ exp.time_
 10 omega -106.00  -57.70   0.7000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   90.0000 69

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 0.12926(2) 0.34921(2) 0.72741(2) 0.01408(6) Uani 1 1 d . . . . .
O1 O 0.00504(12) 0.29126(10) 0.85308(9) 0.0176(2) Uani 1 1 d . . . . .
O2 O 0.02677(13) 0.19910(12) 1.10040(10) 0.0273(3) Uani 1 1 d . . . . .
O3 O -0.17671(13) 0.33835(10) 1.09424(10) 0.0224(3) Uani 1 1 d . . . . .
O4 O -0.24980(14) 0.07927(12) 1.12148(10) 0.0247(3) Uani 1 1 d . . . . .
O5 O -0.35816(13) -0.07898(11) 1.04944(10) 0.0229(3) Uani 1 1 d . . . . .
O6 O -0.35689(13) -0.08912(11) 0.87097(10) 0.0232(3) Uani 1 1 d . . . . .
O7 O -0.13889(13) 0.15121(11) 0.59605(9) 0.0216(2) Uani 1 1 d . . . . .
O8 O -0.02296(12) 0.27588(11) 0.63287(9) 0.0193(2) Uani 1 1 d . . . . .
O9 O 0.25733(12) 0.15512(10) 0.71072(9) 0.0184(2) Uani 1 1 d . . . . .
O10 O 0.45545(13) 0.01455(11) 0.68788(10) 0.0245(3) Uani 1 1 d . . . . .
O11 O 0.82132(13) 0.03375(11) 0.40095(10) 0.0234(3) Uani 1 1 d . . . . .
O12 O 0.83899(12) 0.20747(11) 0.31125(9) 0.0225(3) Uani 1 1 d . . . . .
O13 O 0.60813(13) 0.38810(11) 0.29420(9) 0.0203(2) Uani 1 1 d . . . . .
O14 O 0.31108(13) 0.51977(11) 0.29966(9) 0.0257(3) Uani 1 1 d . . . . .
O15 O 0.31931(14) 0.57420(10) 0.46297(10) 0.0241(3) Uani 1 1 d . . . . .
O20 O 0.22494(11) 0.36935(10) 0.57186(9) 0.0164(2) Uani 1 1 d . . . . .
N1 N 0.28468(14) 0.35375(12) 0.83012(11) 0.0159(3) Uani 1 1 d . . . . .
N2 N 0.42893(15) 0.31688(13) 0.79555(11) 0.0204(3) Uani 1 1 d . . . . .
N3 N 0.50362(15) 0.31752(13) 0.87669(11) 0.0210(3) Uani 1 1 d . . . . .
N4 N 0.40801(14) 0.35513(12) 0.96524(11) 0.0167(3) Uani 1 1 d . . . . .
N5 N 0.00539(14) 0.52692(12) 0.71502(11) 0.0161(3) Uani 1 1 d . . . . .
N6 N -0.09924(15) 0.56816(13) 0.79912(12) 0.0219(3) Uani 1 1 d . . . . .
N7 N -0.16969(16) 0.67835(13) 0.76888(12) 0.0222(3) Uani 1 1 d . . . . .
N8 N -0.11173(14) 0.71057(12) 0.66496(11) 0.0175(3) Uani 1 1 d . . . . .
N9 N -0.09446(14) 0.19927(12) 0.66435(11) 0.0153(3) Uani 1 1 d . . . . .
N10 N -0.32632(14) -0.04517(12) 0.94844(11) 0.0176(3) Uani 1 1 d . . . . .
N11 N -0.09030(14) 0.24452(12) 1.06471(11) 0.0158(3) Uani 1 1 d . . . . .
N12 N 0.34490(14) 0.49780(12) 0.39614(11) 0.0151(3) Uani 1 1 d . . . . .
N13 N 0.77094(14) 0.14296(13) 0.37548(11) 0.0176(3) Uani 1 1 d . . . . .
N14 N 0.37920(14) 0.11688(12) 0.65996(11) 0.0156(3) Uani 1 1 d . . . . .
C1 C -0.00453(17) 0.61692(14) 0.63325(13) 0.0172(3) Uani 1 1 d . . . . .
H1 H 0.0547 0.6154 0.5634 0.021 Uiso 1 1 calc R U . . .
C2 C -0.16221(19) 0.83364(15) 0.60834(15) 0.0238(4) Uani 1 1 d . . . . .
H2A H -0.1035 0.8854 0.6256 0.036 Uiso 1 1 calc R U . . .
H2B H -0.2642 0.8679 0.6347 0.036 Uiso 1 1 calc R U . . .
H2C H -0.1529 0.8304 0.5266 0.036 Uiso 1 1 calc R U . . .
C3 C -0.07773(16) 0.22003(13) 0.86662(13) 0.0139(3) Uani 1 1 d . . . . .
C4 C -0.13133(16) 0.18513(14) 0.97831(12) 0.0145(3) Uani 1 1 d . . . . .
C5 C -0.21257(17) 0.10198(14) 1.01147(13) 0.0164(3) Uani 1 1 d . . . . .
C6 C -0.24888(16) 0.04818(14) 0.92381(13) 0.0153(3) Uani 1 1 d . . . . .
C7 C -0.20899(16) 0.08316(14) 0.81279(13) 0.0155(3) Uani 1 1 d . . . . .
H7 H -0.2386 0.0490 0.7551 0.019 Uiso 1 1 calc R U . . .
C8 C -0.12689(16) 0.16689(14) 0.78297(12) 0.0146(3) Uani 1 1 d . . . . .
C9 C 0.34962(16) 0.31376(14) 0.52992(12) 0.0137(3) Uani 1 1 d . . . . .
C10 C 0.41965(16) 0.37198(14) 0.43509(12) 0.0138(3) Uani 1 1 d . . . . .
C11 C 0.55466(17) 0.32205(14) 0.38055(12) 0.0149(3) Uani 1 1 d . . . . .
C12 C 0.62725(16) 0.20219(14) 0.42259(12) 0.0151(3) Uani 1 1 d . . . . .
C13 C 0.56587(17) 0.13952(14) 0.51291(13) 0.0151(3) Uani 1 1 d . . . . .
H13 H 0.6166 0.0588 0.5393 0.018 Uiso 1 1 calc R U . . .
C14 C 0.27491(17) 0.37600(14) 0.93555(13) 0.0175(3) Uani 1 1 d . . . . .
H14 H 0.1874 0.4025 0.9824 0.021 Uiso 1 1 calc R U . . .
C15 C 0.45836(19) 0.36200(17) 1.07330(14) 0.0239(4) Uani 1 1 d . . . . .
H15A H 0.3948 0.4327 1.1080 0.036 Uiso 1 1 calc R U . . .
H15B H 0.5579 0.3708 1.0607 0.036 Uiso 1 1 calc R U . . .
H15C H 0.4560 0.2871 1.1236 0.036 Uiso 1 1 calc R U . . .
C140 C 0.43158(17) 0.19189(14) 0.56602(12) 0.0142(3) Uani 1 1 d . . . . .
H131 H 0.709(3) 0.339(2) 0.275(2) 0.061(8) Uiso 1 1 d . . . . .
H4 H -0.291(3) 0.031(2) 1.125(2) 0.050(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
Zn1 O1 1.9560(10) . ?
Zn1 O20 1.9851(10) . ?
Zn1 N5 2.0522(13) . ?
Zn1 N1 2.0754(13) . ?
Zn1 O9 2.2477(11) . ?
Zn1 O8 2.3477(11) . ?
O1 C3 1.2670(18) . ?
O2 N11 1.2115(18) . ?
O3 N11 1.2294(17) . ?
O4 C5 1.3322(19) . ?
O4 H4 0.75(3) . ?
O5 N10 1.2461(17) . ?
O6 N10 1.2207(17) . ?
O7 N9 1.2269(17) . ?
O8 N9 1.2449(17) . ?
O9 N14 1.2435(17) . ?
O10 N14 1.2271(17) . ?
O11 N13 1.2203(18) . ?
O12 N13 1.2405(17) . ?
O13 C11 1.3280(18) . ?
O13 H131 1.00(3) . ?
O14 N12 1.2193(17) . ?
O15 N12 1.2236(17) . ?
O20 C9 1.2700(18) . ?
N1 C14 1.314(2) . ?
N1 N2 1.3622(19) . ?
N2 N3 1.2869(19) . ?
N3 N4 1.3493(18) . ?
N4 C14 1.324(2) . ?
N4 C15 1.464(2) . ?
N5 C1 1.312(2) . ?
N5 N6 1.3662(18) . ?
N6 N7 1.284(2) . ?
N7 N8 1.3443(19) . ?
N8 C1 1.329(2) . ?
N8 C2 1.457(2) . ?
N9 C8 1.4373(19) . ?
N10 C6 1.4379(19) . ?
N11 C4 1.4654(19) . ?
N12 C10 1.4630(19) . ?
N13 C12 1.443(2) . ?
N14 C140 1.4418(19) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.417(2) . ?
C3 C8 1.434(2) . ?
C4 C5 1.375(2) . ?
C5 C6 1.416(2) . ?
C6 C7 1.374(2) . ?
C7 C8 1.382(2) . ?
C7 H7 0.9500 . ?
C9 C10 1.423(2) . ?
C9 C140 1.439(2) . ?
C10 C11 1.386(2) . ?
C11 C12 1.413(2) . ?
C12 C13 1.373(2) . ?
C13 C140 1.380(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O20 158.82(5) . . ?
O1 Zn1 N5 95.15(5) . . ?
O20 Zn1 N5 92.54(5) . . ?
O1 Zn1 N1 93.44(5) . . ?
O20 Zn1 N1 104.12(5) . . ?
N5 Zn1 N1 102.48(5) . . ?
O1 Zn1 O9 89.78(4) . . ?
O20 Zn1 O9 80.06(4) . . ?
N5 Zn1 O9 170.32(5) . . ?
N1 Zn1 O9 85.49(5) . . ?
O1 Zn1 O8 78.18(4) . . ?
O20 Zn1 O8 81.51(4) . . ?
N5 Zn1 O8 95.09(5) . . ?
N1 Zn1 O8 161.18(5) . . ?
O9 Zn1 O8 77.74(4) . . ?
C3 O1 Zn1 135.72(10) . . ?
C5 O4 H4 104(2) . . ?
N9 O8 Zn1 131.66(9) . . ?
N14 O9 Zn1 128.89(9) . . ?
C11 O13 H131 105.2(15) . . ?
C9 O20 Zn1 129.76(10) . . ?
C14 N1 N2 106.61(13) . . ?
C14 N1 Zn1 132.06(11) . . ?
N2 N1 Zn1 120.97(10) . . ?
N3 N2 N1 109.63(13) . . ?
N2 N3 N4 106.93(13) . . ?
C14 N4 N3 108.57(13) . . ?
C14 N4 C15 130.63(14) . . ?
N3 N4 C15 120.74(13) . . ?
C1 N5 N6 106.50(13) . . ?
C1 N5 Zn1 132.44(11) . . ?
N6 N5 Zn1 120.83(10) . . ?
N7 N6 N5 109.62(13) . . ?
N6 N7 N8 107.11(13) . . ?
C1 N8 N7 108.59(13) . . ?
C1 N8 C2 130.27(14) . . ?
N7 N8 C2 121.04(13) . . ?
O7 N9 O8 121.31(12) . . ?
O7 N9 C8 119.12(13) . . ?
O8 N9 C8 119.56(12) . . ?
O6 N10 O5 122.54(13) . . ?
O6 N10 C6 119.54(13) . . ?
O5 N10 C6 117.92(13) . . ?
O2 N11 O3 124.79(14) . . ?
O2 N11 C4 117.90(13) . . ?
O3 N11 C4 117.29(13) . . ?
O14 N12 O15 124.15(14) . . ?
O14 N12 C10 118.09(12) . . ?
O15 N12 C10 117.76(12) . . ?
O11 N13 O12 122.82(13) . . ?
O11 N13 C12 119.69(13) . . ?
O12 N13 C12 117.48(13) . . ?
O10 N14 O9 120.67(13) . . ?
O10 N14 C140 119.16(13) . . ?
O9 N14 C140 120.16(13) . . ?
N5 C1 N8 108.18(14) . . ?
N5 C1 H1 125.9 . . ?
N8 C1 H1 125.9 . . ?
N8 C2 H2A 109.5 . . ?
N8 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N8 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 C4 117.93(13) . . ?
O1 C3 C8 128.86(14) . . ?
C4 C3 C8 113.21(13) . . ?
C5 C4 C3 126.91(14) . . ?
C5 C4 N11 118.88(13) . . ?
C3 C4 N11 114.20(13) . . ?
O4 C5 C4 117.88(14) . . ?
O4 C5 C6 126.08(14) . . ?
C4 C5 C6 116.04(13) . . ?
C7 C6 C5 120.52(14) . . ?
C7 C6 N10 118.35(14) . . ?
C5 C6 N10 121.12(13) . . ?
C6 C7 C8 121.59(14) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C3 121.48(13) . . ?
C7 C8 N9 116.95(13) . . ?
C3 C8 N9 121.57(13) . . ?
O20 C9 C10 119.55(14) . . ?
O20 C9 C140 126.86(14) . . ?
C10 C9 C140 113.56(13) . . ?
C11 C10 C9 125.71(14) . . ?
C11 C10 N12 117.62(13) . . ?
C9 C10 N12 116.59(13) . . ?
O13 C11 C10 119.20(14) . . ?
O13 C11 C12 124.23(14) . . ?
C10 C11 C12 116.57(13) . . ?
C13 C12 C11 121.11(14) . . ?
C13 C12 N13 117.43(14) . . ?
C11 C12 N13 121.41(13) . . ?
C12 C13 C140 121.03(14) . . ?
C12 C13 H13 119.5 . . ?
C140 C13 H13 119.5 . . ?
N1 C14 N4 108.25(14) . . ?
N1 C14 H14 125.9 . . ?
N4 C14 H14 125.9 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C140 C9 122.00(13) . . ?
C13 C140 N14 115.70(13) . . ?
C9 C140 N14 122.30(13) . . ?

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
C14 N1 N2 N3 -0.38(17) . . . . ?
Zn1 N1 N2 N3 -174.27(10) . . . . ?
N1 N2 N3 N4 -0.05(17) . . . . ?
N2 N3 N4 C14 0.47(17) . . . . ?
N2 N3 N4 C15 177.92(14) . . . . ?
C1 N5 N6 N7 0.29(18) . . . . ?
Zn1 N5 N6 N7 -174.92(10) . . . . ?
N5 N6 N7 N8 -0.20(17) . . . . ?
N6 N7 N8 C1 0.04(17) . . . . ?
N6 N7 N8 C2 -176.60(14) . . . . ?
Zn1 O8 N9 O7 -161.84(10) . . . . ?
Zn1 O8 N9 C8 18.66(19) . . . . ?
Zn1 O9 N14 O10 155.17(11) . . . . ?
Zn1 O9 N14 C140 -25.88(19) . . . . ?
N6 N5 C1 N8 -0.26(17) . . . . ?
Zn1 N5 C1 N8 174.16(11) . . . . ?
N7 N8 C1 N5 0.14(18) . . . . ?
C2 N8 C1 N5 176.36(15) . . . . ?
Zn1 O1 C3 C4 169.36(11) . . . . ?
Zn1 O1 C3 C8 -10.3(3) . . . . ?
O1 C3 C4 C5 -174.59(15) . . . . ?
C8 C3 C4 C5 5.2(2) . . . . ?
O1 C3 C4 N11 4.0(2) . . . . ?
C8 C3 C4 N11 -176.22(12) . . . . ?
O2 N11 C4 C5 94.09(18) . . . . ?
O3 N11 C4 C5 -87.13(18) . . . . ?
O2 N11 C4 C3 -84.65(17) . . . . ?
O3 N11 C4 C3 94.13(16) . . . . ?
C3 C4 C5 O4 178.38(15) . . . . ?
N11 C4 C5 O4 -0.2(2) . . . . ?
C3 C4 C5 C6 -1.6(2) . . . . ?
N11 C4 C5 C6 179.82(13) . . . . ?
O4 C5 C6 C7 177.25(15) . . . . ?
C4 C5 C6 C7 -2.8(2) . . . . ?
O4 C5 C6 N10 -3.6(2) . . . . ?
C4 C5 C6 N10 176.40(14) . . . . ?
O6 N10 C6 C7 -1.3(2) . . . . ?
O5 N10 C6 C7 177.84(14) . . . . ?
O6 N10 C6 C5 179.49(14) . . . . ?
O5 N10 C6 C5 -1.3(2) . . . . ?
C5 C6 C7 C8 3.1(2) . . . . ?
N10 C6 C7 C8 -176.06(14) . . . . ?
C6 C7 C8 C3 0.9(2) . . . . ?
C6 C7 C8 N9 -178.46(14) . . . . ?
O1 C3 C8 C7 175.08(15) . . . . ?
C4 C3 C8 C7 -4.6(2) . . . . ?
O1 C3 C8 N9 -5.6(2) . . . . ?
C4 C3 C8 N9 174.65(13) . . . . ?
O7 N9 C8 C7 -0.7(2) . . . . ?
O8 N9 C8 C7 178.78(13) . . . . ?
O7 N9 C8 C3 179.96(14) . . . . ?
O8 N9 C8 C3 -0.5(2) . . . . ?
Zn1 O20 C9 C10 -154.72(11) . . . . ?
Zn1 O20 C9 C140 27.2(2) . . . . ?
O20 C9 C10 C11 -179.58(14) . . . . ?
C140 C9 C10 C11 -1.2(2) . . . . ?
O20 C9 C10 N12 3.7(2) . . . . ?
C140 C9 C10 N12 -177.92(12) . . . . ?
O14 N12 C10 C11 62.83(18) . . . . ?
O15 N12 C10 C11 -117.72(15) . . . . ?
O14 N12 C10 C9 -120.21(15) . . . . ?
O15 N12 C10 C9 59.24(18) . . . . ?
C9 C10 C11 O13 -178.62(14) . . . . ?
N12 C10 C11 O13 -2.0(2) . . . . ?
C9 C10 C11 C12 0.9(2) . . . . ?
N12 C10 C11 C12 177.55(13) . . . . ?
O13 C11 C12 C13 179.48(14) . . . . ?
C10 C11 C12 C13 0.0(2) . . . . ?
O13 C11 C12 N13 2.1(2) . . . . ?
C10 C11 C12 N13 -177.39(13) . . . . ?
O11 N13 C12 C13 14.1(2) . . . . ?
O12 N13 C12 C13 -164.84(13) . . . . ?
O11 N13 C12 C11 -168.47(14) . . . . ?
O12 N13 C12 C11 12.6(2) . . . . ?
C11 C12 C13 C140 -0.4(2) . . . . ?
N13 C12 C13 C140 177.08(13) . . . . ?
N2 N1 C14 N4 0.67(17) . . . . ?
Zn1 N1 C14 N4 173.60(11) . . . . ?
N3 N4 C14 N1 -0.71(17) . . . . ?
C15 N4 C14 N1 -177.83(15) . . . . ?
C12 C13 C140 C9 0.0(2) . . . . ?
C12 C13 C140 N14 -179.83(13) . . . . ?
O20 C9 C140 C13 178.97(14) . . . . ?
C10 C9 C140 C13 0.8(2) . . . . ?
O20 C9 C140 N14 -1.2(2) . . . . ?
C10 C9 C140 N14 -179.44(13) . . . . ?
O10 N14 C140 C13 1.1(2) . . . . ?
O9 N14 C140 C13 -177.83(13) . . . . ?
O10 N14 C140 C9 -178.67(13) . . . . ?
O9 N14 C140 C9 2.4(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         0.349
_refine_diff_density_min         -0.338
_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_lx277
_database_code_depnum_ccdc_archive 'CCDC 1566376'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon May 30 20:32:06 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakis-aqua bis(1-methyltetrazolyl) cobalt(II) dipicrate dihydrate
;
_chemical_name_common            
'tetrakis-aqua bis(1-methyltetrazolyl) cobalt(II) dipicrate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C4 H16 Co N8 O4, 2(C6 H2 N3 O7), 2(H2 O)'
_chemical_formula_sum            'C16 H24 Co N14 O20'
_chemical_formula_weight         791.42

_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                   15.5380(5)
_cell_length_b                   5.22980(10)
_cell_length_c                   18.5676(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.713(3)
_cell_angle_gamma                90
_cell_volume                     1471.83(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173
_cell_measurement_reflns_used    3855
_cell_measurement_theta_min      4.4750
_cell_measurement_theta_max      32.2410

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.698
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91042
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             810
_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            10884
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.164
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_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             2893
_reflns_number_gt                2482
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+1.0759P] 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         2893
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0467224000
_diffrn_orient_matrix_UB_12      -0.0068437000
_diffrn_orient_matrix_UB_13      -0.0092838000
_diffrn_orient_matrix_UB_21      0.0008465000
_diffrn_orient_matrix_UB_22      0.0003402000
_diffrn_orient_matrix_UB_23      -0.0380408000
_diffrn_orient_matrix_UB_31      0.0023678000
_diffrn_orient_matrix_UB_32      -0.1354647000
_diffrn_orient_matrix_UB_33      0.0004117000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -79.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -150.0000 40

#__ type_ start__ end____ width___ exp.time_
  2 omega   74.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega   74.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -120.0000 37

#__ type_ start__ end____ width___ exp.time_
  4 omega   29.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 69

#__ type_ start__ end____ width___ exp.time_
  5 omega   -9.00   32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 41

#__ type_ start__ end____ width___ exp.time_
  6 omega   41.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
  7 omega  -24.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
  8 omega  -27.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000    0.0000 123

;



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'
Co Co 0.3494 0.9721 '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
Co1 Co 0.5000 0.0000 0.5000 0.01186(10) Uani 1 2 d S . P . .
O1 O 0.58978(9) 0.2841(3) 0.48546(8) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.54482(10) -0.2268(2) 0.42175(8) 0.0149(3) Uani 1 1 d . . . . .
N1 N 0.39869(10) 0.1724(3) 0.41815(8) 0.0150(3) Uani 1 1 d . . . . .
N2 N 0.41995(11) 0.2920(3) 0.35941(9) 0.0214(4) Uani 1 1 d . . . . .
N3 N 0.35367(11) 0.4242(3) 0.32430(9) 0.0217(4) Uani 1 1 d . . . . .
N4 N 0.28790(10) 0.3916(3) 0.36028(8) 0.0153(3) Uani 1 1 d . . . . .
C1 C 0.31659(13) 0.2377(3) 0.41718(11) 0.0160(4) Uani 1 1 d . . . . .
C2 C 0.20519(12) 0.5314(4) 0.33754(11) 0.0205(4) Uani 1 1 d . . . . .
H2A H 0.1582 0.4345 0.3503 0.031 Uiso 1 1 calc R U . . .
H2B H 0.1928 0.5581 0.2851 0.031 Uiso 1 1 calc R U . . .
H2C H 0.2101 0.6937 0.3622 0.031 Uiso 1 1 calc R U . . .
O3 O 0.28924(8) 0.4734(2) 0.06751(7) 0.0173(3) Uani 1 1 d . . . . .
O4 O 0.22231(9) 0.9167(3) 0.00997(8) 0.0275(3) Uani 1 1 d . . . . .
O5 O 0.08077(9) 0.9104(3) -0.02687(8) 0.0254(3) Uani 1 1 d . . . . .
O6 O -0.08877(9) 0.5420(3) 0.13031(9) 0.0269(3) Uani 1 1 d . . . . .
O7 O -0.02967(9) 0.2670(3) 0.21404(8) 0.0263(3) Uani 1 1 d . . . . .
O8 O 0.25438(11) -0.0546(3) 0.22488(10) 0.0410(5) Uani 1 1 d . . . . .
O9 O 0.34003(10) 0.0863(4) 0.15993(10) 0.0460(5) Uani 1 1 d . . . . .
N5 N 0.14957(10) 0.8286(3) 0.01206(8) 0.0165(3) Uani 1 1 d . . . . .
N6 N -0.02628(11) 0.4107(3) 0.16242(9) 0.0199(4) Uani 1 1 d . . . . .
N7 N 0.27003(10) 0.0913(3) 0.17818(9) 0.0180(3) Uani 1 1 d . . . . .
C3 C 0.21970(12) 0.4597(3) 0.09059(10) 0.0141(4) Uani 1 1 d . . . . .
C4 C 0.14394(12) 0.6256(3) 0.06466(10) 0.0149(4) Uani 1 1 d . . . . .
C5 C 0.06521(13) 0.6080(4) 0.08590(11) 0.0169(4) Uani 1 1 d . . . . .
C6 C 0.05603(12) 0.4252(4) 0.13784(11) 0.0166(4) Uani 1 1 d . . . . .
C7 C 0.12364(12) 0.2578(4) 0.16669(10) 0.0165(4) Uani 1 1 d . . . . .
C8 C 0.20203(12) 0.2736(3) 0.14401(10) 0.0151(4) Uani 1 1 d . . . . .
O10 O 0.52905(11) 0.2786(3) 0.22442(8) 0.0213(3) Uani 1 1 d . . . . .
H5 H 0.0223(14) 0.720(4) 0.0690(11) 0.016(5) Uiso 1 1 d . . . . .
H7 H 0.1171(13) 0.135(4) 0.2016(12) 0.018(5) Uiso 1 1 d . . . . .
H1 H 0.2836(14) 0.193(4) 0.4507(12) 0.018(5) Uiso 1 1 d . . . . .
H11 H 0.5709(18) 0.408(5) 0.4600(14) 0.037(7) Uiso 1 1 d . . . . .
H22 H 0.5949(19) -0.198(5) 0.4189(14) 0.035(7) Uiso 1 1 d . . . . .
H102 H 0.5797(19) 0.271(5) 0.2377(14) 0.036(8) Uiso 1 1 d . . . . .
H101 H 0.515(2) 0.416(6) 0.2427(17) 0.054(9) Uiso 1 1 d . . . . .
H21 H 0.5130(19) -0.223(5) 0.3758(17) 0.047(8) Uiso 1 1 d . . . . .
H12 H 0.632(2) 0.237(5) 0.4690(15) 0.048(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
Co1 O1 2.0956(13) 3_656 ?
Co1 O1 2.0957(13) . ?
Co1 O2 2.1091(13) 3_656 ?
Co1 O2 2.1091(13) . ?
Co1 N1 2.1325(15) 3_656 ?
Co1 N1 2.1325(15) . ?
O1 H11 0.82(3) . ?
O1 H12 0.82(3) . ?
O2 H22 0.81(3) . ?
O2 H21 0.89(3) . ?
N1 C1 1.317(2) . ?
N1 N2 1.360(2) . ?
N2 N3 1.291(2) . ?
N3 N4 1.349(2) . ?
N4 C1 1.325(2) . ?
N4 C2 1.458(2) . ?
C1 H1 0.92(2) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
O3 C3 1.249(2) . ?
O4 N5 1.229(2) . ?
O5 N5 1.228(2) . ?
O6 N6 1.231(2) . ?
O7 N6 1.228(2) . ?
O8 N7 1.219(2) . ?
O9 N7 1.209(2) . ?
N5 C4 1.458(2) . ?
N6 C6 1.451(2) . ?
N7 C8 1.460(2) . ?
C3 C4 1.456(3) . ?
C3 C8 1.458(3) . ?
C4 C5 1.368(3) . ?
C5 C6 1.387(3) . ?
C5 H5 0.89(2) . ?
C6 C7 1.382(3) . ?
C7 C8 1.376(3) . ?
C7 H7 0.93(2) . ?
O10 H102 0.77(3) . ?
O10 H101 0.84(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
O1 Co1 O1 180.0 3_656 . ?
O1 Co1 O2 88.85(5) 3_656 3_656 ?
O1 Co1 O2 91.15(5) . 3_656 ?
O1 Co1 O2 91.15(5) 3_656 . ?
O1 Co1 O2 88.85(5) . . ?
O2 Co1 O2 180.0 3_656 . ?
O1 Co1 N1 90.94(6) 3_656 3_656 ?
O1 Co1 N1 89.06(6) . 3_656 ?
O2 Co1 N1 92.90(6) 3_656 3_656 ?
O2 Co1 N1 87.10(6) . 3_656 ?
O1 Co1 N1 89.06(6) 3_656 . ?
O1 Co1 N1 90.94(6) . . ?
O2 Co1 N1 87.10(6) 3_656 . ?
O2 Co1 N1 92.90(6) . . ?
N1 Co1 N1 180.0 3_656 . ?
Co1 O1 H11 118.1(19) . . ?
Co1 O1 H12 116(2) . . ?
H11 O1 H12 104(3) . . ?
Co1 O2 H22 114.2(18) . . ?
Co1 O2 H21 116.9(18) . . ?
H22 O2 H21 106(2) . . ?
C1 N1 N2 105.98(15) . . ?
C1 N1 Co1 132.87(13) . . ?
N2 N1 Co1 119.64(11) . . ?
N3 N2 N1 110.10(15) . . ?
N2 N3 N4 106.81(15) . . ?
C1 N4 N3 108.24(15) . . ?
C1 N4 C2 131.01(16) . . ?
N3 N4 C2 120.57(15) . . ?
N1 C1 N4 108.87(17) . . ?
N1 C1 H1 127.3(13) . . ?
N4 C1 H1 123.7(13) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 N5 O4 122.56(16) . . ?
O5 N5 C4 118.37(15) . . ?
O4 N5 C4 119.03(15) . . ?
O7 N6 O6 123.70(16) . . ?
O7 N6 C6 118.00(16) . . ?
O6 N6 C6 118.30(16) . . ?
O9 N7 O8 121.23(17) . . ?
O9 N7 C8 120.13(16) . . ?
O8 N7 C8 118.64(16) . . ?
O3 C3 C4 123.36(16) . . ?
O3 C3 C8 125.32(17) . . ?
C4 C3 C8 111.28(15) . . ?
C5 C4 C3 125.00(17) . . ?
C5 C4 N5 115.54(16) . . ?
C3 C4 N5 119.46(16) . . ?
C4 C5 C6 118.81(18) . . ?
C4 C5 H5 120.1(13) . . ?
C6 C5 H5 121.0(13) . . ?
C7 C6 C5 121.35(17) . . ?
C7 C6 N6 119.48(17) . . ?
C5 C6 N6 119.17(17) . . ?
C8 C7 C6 119.46(17) . . ?
C8 C7 H7 119.5(13) . . ?
C6 C7 H7 121.1(13) . . ?
C7 C8 C3 124.06(17) . . ?
C7 C8 N7 115.62(16) . . ?
C3 C8 N7 120.31(16) . . ?
H102 O10 H101 104(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.0(2) . . . . ?
Co1 N1 N2 N3 -167.77(13) . . . . ?
N1 N2 N3 N4 0.0(2) . . . . ?
N2 N3 N4 C1 -0.1(2) . . . . ?
N2 N3 N4 C2 175.52(16) . . . . ?
N2 N1 C1 N4 0.0(2) . . . . ?
Co1 N1 C1 N4 165.42(12) . . . . ?
N3 N4 C1 N1 0.0(2) . . . . ?
C2 N4 C1 N1 -174.90(18) . . . . ?
O3 C3 C4 C5 176.59(18) . . . . ?
C8 C3 C4 C5 -1.3(3) . . . . ?
O3 C3 C4 N5 -3.5(3) . . . . ?
C8 C3 C4 N5 178.59(15) . . . . ?
O5 N5 C4 C5 -23.3(2) . . . . ?
O4 N5 C4 C5 154.41(17) . . . . ?
O5 N5 C4 C3 156.78(16) . . . . ?
O4 N5 C4 C3 -25.5(2) . . . . ?
C3 C4 C5 C6 2.2(3) . . . . ?
N5 C4 C5 C6 -177.73(16) . . . . ?
C4 C5 C6 C7 -1.7(3) . . . . ?
C4 C5 C6 N6 178.06(16) . . . . ?
O7 N6 C6 C7 7.6(3) . . . . ?
O6 N6 C6 C7 -172.20(17) . . . . ?
O7 N6 C6 C5 -172.24(17) . . . . ?
O6 N6 C6 C5 8.0(3) . . . . ?
C5 C6 C7 C8 0.6(3) . . . . ?
N6 C6 C7 C8 -179.25(17) . . . . ?
C6 C7 C8 C3 0.3(3) . . . . ?
C6 C7 C8 N7 179.22(16) . . . . ?
O3 C3 C8 C7 -177.82(18) . . . . ?
C4 C3 C8 C7 0.1(3) . . . . ?
O3 C3 C8 N7 3.3(3) . . . . ?
C4 C3 C8 N7 -178.82(15) . . . . ?
O9 N7 C8 C7 177.77(19) . . . . ?
O8 N7 C8 C7 -2.0(3) . . . . ?
O9 N7 C8 C3 -3.3(3) . . . . ?
O8 N7 C8 C3 177.00(18) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H11 O2 0.82(3) 2.05(3) 2.8403(19) 163(3) 1_565
O2 H22 O3 0.81(3) 1.98(3) 2.7491(19) 160(2) 2_645
O2 H22 O9 0.81(3) 2.26(3) 2.766(2) 122(2) 2_645
O10 H102 N3 0.77(3) 2.49(3) 2.881(2) 113(2) 2_645
O10 H102 O9 0.77(3) 2.62(3) 3.069(2) 119(2) 2_655
O10 H101 O10 0.84(3) 2.15(3) 2.9887(15) 173(3) 2_655
O2 H21 O10 0.89(3) 1.83(3) 2.704(2) 167(3) 2_645
O1 H12 O3 0.82(3) 2.05(3) 2.8205(19) 155(3) 2_645
O1 H12 O4 0.82(3) 2.40(3) 2.984(2) 129(2) 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         0.335
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.054

_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_lx281
_database_code_depnum_ccdc_archive 'CCDC 1566377'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Jun 03 09:34:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakis-aqua bis(1-methyltetrazolyl) manganese(II) dipicrate dihydrate
;
_chemical_name_common            
'tetrakis-aqua bis(1-methyltetrazolyl) manganese(II) dipicrate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Mn N8 O4, 2(C6 H2 N3 O7), 2(H2 O)'
_chemical_formula_sum            'C16 H24 Mn N14 O20'
_chemical_formula_weight         787.43

_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                   15.5640(10)
_cell_length_b                   5.2200(2)
_cell_length_c                   18.5520(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.645(6)
_cell_angle_gamma                90
_cell_volume                     1470.68(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2134
_cell_measurement_theta_min      4.3620
_cell_measurement_theta_max      27.8310

_exptl_crystal_description       block
_exptl_crystal_colour            light-yellow
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.563
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_F_000             806
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            9834
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.128
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2887
_reflns_number_gt                2191
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0414P)²+0.8841P] 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         2887
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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      0.0291889000
_diffrn_orient_matrix_UB_12      -0.0219582000
_diffrn_orient_matrix_UB_13      0.0345977000
_diffrn_orient_matrix_UB_21      0.0319712000
_diffrn_orient_matrix_UB_22      -0.0485686000
_diffrn_orient_matrix_UB_23      -0.0183787000
_diffrn_orient_matrix_UB_31      0.0175833000
_diffrn_orient_matrix_UB_32      0.1249407000
_diffrn_orient_matrix_UB_33      -0.0010610000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00  -57.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -57.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega  -42.00    1.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -57.0000 -120.0000 43

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   25.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -99.0000  150.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega   11.00   47.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931   57.0000 -180.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega  -29.00    3.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -57.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
  6 omega  -44.00   50.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931   57.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  7 omega   39.00   90.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869  179.0000  -30.0000 51

#__ type_ start__ end____ width___ exp.time_
  8 omega    2.00   92.00   1.0000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3869   57.0000  150.0000 90

;



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
Mn1 Mn 0.0000 0.5000 0.0000 0.00877(15) Uani 1 2 d S . P . .
O1 O 0.04508(14) 0.2733(3) -0.07851(11) 0.0190(4) Uani 1 1 d . . . . .
O2 O -0.08986(14) 0.2150(4) 0.01467(10) 0.0215(4) Uani 1 1 d . . . . .
N1 N 0.10126(16) 0.3281(4) 0.08180(12) 0.0197(5) Uani 1 1 d . . . . .
N2 N 0.07992(17) 0.2077(4) 0.14079(13) 0.0256(6) Uani 1 1 d . . . . .
N3 N 0.14598(17) 0.0753(5) 0.17562(13) 0.0265(6) Uani 1 1 d . . . . .
N4 N 0.21167(16) 0.1083(4) 0.13955(12) 0.0191(5) Uani 1 1 d . . . . .
C1 C 0.1835(2) 0.2629(5) 0.08272(15) 0.0214(6) Uani 1 1 d . . . . .
C2 C 0.29464(19) -0.0299(5) 0.16241(16) 0.0256(6) Uani 1 1 d . . . . .
H2A H 0.2903 -0.1956 0.1371 0.038 Uiso 1 1 calc R U . . .
H2B H 0.3071 -0.0576 0.2159 0.038 Uiso 1 1 calc R U . . .
H2C H 0.3423 0.0708 0.1496 0.038 Uiso 1 1 calc R U . . .
O4 O 0.16007(16) 0.4141(5) 0.34013(14) 0.0518(7) Uani 1 1 d . . . . .
O5 O 0.24561(16) 0.5546(4) 0.27505(14) 0.0461(7) Uani 1 1 d . . . . .
O6 O 0.21089(13) 0.0272(3) 0.43233(10) 0.0222(4) Uani 1 1 d . . . . .
O7 O 0.27774(15) -0.4163(4) 0.49026(12) 0.0333(5) Uani 1 1 d . . . . .
O8 O 0.41888(14) -0.4107(4) 0.52654(11) 0.0307(5) Uani 1 1 d . . . . .
O9 O 0.58869(14) -0.0421(4) 0.36973(12) 0.0326(5) Uani 1 1 d . . . . .
O10 O 0.52995(14) 0.2347(4) 0.28626(11) 0.0312(5) Uani 1 1 d . . . . .
N5 N 0.23014(16) 0.4084(4) 0.32187(12) 0.0220(5) Uani 1 1 d . . . . .
N6 N 0.35050(16) -0.3290(4) 0.48784(12) 0.0215(5) Uani 1 1 d . . . . .
N7 N 0.52580(16) 0.0903(4) 0.33767(13) 0.0233(5) Uani 1 1 d . . . . .
C3 C 0.29821(19) 0.2267(5) 0.35598(14) 0.0207(6) Uani 1 1 d . . . . .
C4 C 0.28046(18) 0.0404(5) 0.40941(14) 0.0179(6) Uani 1 1 d . . . . .
C5 C 0.35564(19) -0.1260(5) 0.43518(14) 0.0193(6) Uani 1 1 d . . . . .
C6 C 0.4346(2) -0.1078(5) 0.41395(15) 0.0204(6) Uani 1 1 d . . . . .
C7 C 0.4440(2) 0.0747(5) 0.36217(15) 0.0207(6) Uani 1 1 d . . . . .
C8 C 0.37645(19) 0.2425(5) 0.33350(15) 0.0202(6) Uani 1 1 d . . . . .
O3 O 0.02941(16) 0.7204(4) 0.22452(11) 0.0267(5) Uani 1 1 d . . . . .
H8 H 0.3841(18) 0.368(5) 0.2994(14) 0.013(7) Uiso 1 1 d . . . . .
H6 H 0.481(2) -0.231(5) 0.4309(14) 0.019(7) Uiso 1 1 d . . . . .
H22 H -0.145(3) 0.266(8) 0.031(2) 0.076(14) Uiso 1 1 d . . . . .
H1 H 0.215(2) 0.311(6) 0.0489(17) 0.032(9) Uiso 1 1 d . . . . .
H21 H -0.072(3) 0.061(7) 0.038(2) 0.051(11) Uiso 1 1 d . . . . .
H32 H 0.096(3) 0.733(9) 0.238(2) 0.087(16) Uiso 1 1 d . . . . .
H31 H 0.019(3) 0.570(8) 0.244(2) 0.069(14) Uiso 1 1 d . . . . .
H12 H 0.110(3) 0.330(8) -0.086(2) 0.075(13) Uiso 1 1 d . . . . .
H11 H 0.014(3) 0.294(7) -0.129(2) 0.061(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
Mn1 O2 2.1001(19) . ?
Mn1 O2 2.1001(19) 3_565 ?
Mn1 O1 2.1123(18) . ?
Mn1 O1 2.1123(18) 3_565 ?
Mn1 N1 2.132(2) . ?
Mn1 N1 2.132(2) 3_565 ?
O1 H12 1.09(5) . ?
O1 H11 0.95(4) . ?
O2 H22 1.01(5) . ?
O2 H21 0.93(4) . ?
N1 C1 1.320(4) . ?
N1 N2 1.365(3) . ?
N2 N3 1.289(3) . ?
N3 N4 1.350(3) . ?
N4 C1 1.324(3) . ?
N4 C2 1.459(4) . ?
C1 H1 0.91(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O4 N5 1.211(3) . ?
O5 N5 1.219(3) . ?
O6 C4 1.249(3) . ?
O7 N6 1.231(3) . ?
O8 N6 1.223(3) . ?
O9 N7 1.239(3) . ?
O10 N7 1.228(3) . ?
N5 C3 1.459(3) . ?
N6 C5 1.456(3) . ?
N7 C7 1.445(4) . ?
C3 C8 1.373(4) . ?
C3 C4 1.458(4) . ?
C4 C5 1.452(4) . ?
C5 C6 1.373(4) . ?
C6 C7 1.383(4) . ?
C6 H6 0.97(3) . ?
C7 C8 1.382(4) . ?
C8 H8 0.94(3) . ?
O3 H32 1.02(5) . ?
O3 H31 0.90(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
O2 Mn1 O2 180.0 . 3_565 ?
O2 Mn1 O1 91.35(8) . . ?
O2 Mn1 O1 88.65(8) 3_565 . ?
O2 Mn1 O1 88.65(8) . 3_565 ?
O2 Mn1 O1 91.35(8) 3_565 3_565 ?
O1 Mn1 O1 180.0 . 3_565 ?
O2 Mn1 N1 91.09(8) . . ?
O2 Mn1 N1 88.91(8) 3_565 . ?
O1 Mn1 N1 87.11(8) . . ?
O1 Mn1 N1 92.89(8) 3_565 . ?
O2 Mn1 N1 88.91(8) . 3_565 ?
O2 Mn1 N1 91.09(8) 3_565 3_565 ?
O1 Mn1 N1 92.89(8) . 3_565 ?
O1 Mn1 N1 87.11(8) 3_565 3_565 ?
N1 Mn1 N1 180.0 . 3_565 ?
Mn1 O1 H12 113(2) . . ?
Mn1 O1 H11 116(2) . . ?
H12 O1 H11 98(3) . . ?
Mn1 O2 H22 119(2) . . ?
Mn1 O2 H21 122(2) . . ?
H22 O2 H21 106(3) . . ?
C1 N1 N2 106.0(2) . . ?
C1 N1 Mn1 132.92(18) . . ?
N2 N1 Mn1 119.53(18) . . ?
N3 N2 N1 110.0(2) . . ?
N2 N3 N4 106.9(2) . . ?
C1 N4 N3 108.5(2) . . ?
C1 N4 C2 130.6(2) . . ?
N3 N4 C2 120.7(2) . . ?
N1 C1 N4 108.6(2) . . ?
N1 C1 H1 126(2) . . ?
N4 C1 H1 126(2) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 N5 O5 120.9(2) . . ?
O4 N5 C3 120.5(2) . . ?
O5 N5 C3 118.5(2) . . ?
O8 N6 O7 122.6(2) . . ?
O8 N6 C5 118.6(2) . . ?
O7 N6 C5 118.7(2) . . ?
O10 N7 O9 123.0(2) . . ?
O10 N7 C7 118.6(2) . . ?
O9 N7 C7 118.4(2) . . ?
C8 C3 C4 124.0(3) . . ?
C8 C3 N5 115.9(2) . . ?
C4 C3 N5 120.1(2) . . ?
O6 C4 C5 123.5(2) . . ?
O6 C4 C3 125.2(3) . . ?
C5 C4 C3 111.3(2) . . ?
C6 C5 C4 124.9(3) . . ?
C6 C5 N6 115.3(2) . . ?
C4 C5 N6 119.9(2) . . ?
C5 C6 C7 119.0(3) . . ?
C5 C6 H6 120.7(17) . . ?
C7 C6 H6 120.1(17) . . ?
C8 C7 C6 121.1(3) . . ?
C8 C7 N7 119.4(2) . . ?
C6 C7 N7 119.5(3) . . ?
C3 C8 C7 119.7(3) . . ?
C3 C8 H8 120.0(17) . . ?
C7 C8 H8 120.3(17) . . ?
H32 O3 H31 103(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.2(3) . . . . ?
Mn1 N1 N2 N3 167.53(18) . . . . ?
N1 N2 N3 N4 0.1(3) . . . . ?
N2 N3 N4 C1 0.1(3) . . . . ?
N2 N3 N4 C2 -176.1(2) . . . . ?
N2 N1 C1 N4 0.2(3) . . . . ?
Mn1 N1 C1 N4 -165.15(18) . . . . ?
N3 N4 C1 N1 -0.2(3) . . . . ?
C2 N4 C1 N1 175.5(3) . . . . ?
O4 N5 C3 C8 -177.5(3) . . . . ?
O5 N5 C3 C8 2.1(4) . . . . ?
O4 N5 C3 C4 3.5(4) . . . . ?
O5 N5 C3 C4 -176.9(3) . . . . ?
C8 C3 C4 O6 177.7(3) . . . . ?
N5 C3 C4 O6 -3.4(4) . . . . ?
C8 C3 C4 C5 -0.4(4) . . . . ?
N5 C3 C4 C5 178.5(2) . . . . ?
O6 C4 C5 C6 -176.5(3) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
O6 C4 C5 N6 3.1(4) . . . . ?
C3 C4 C5 N6 -178.8(2) . . . . ?
O8 N6 C5 C6 23.0(3) . . . . ?
O7 N6 C5 C6 -155.1(3) . . . . ?
O8 N6 C5 C4 -156.6(2) . . . . ?
O7 N6 C5 C4 25.3(4) . . . . ?
C4 C5 C6 C7 -2.5(4) . . . . ?
N6 C5 C6 C7 177.9(2) . . . . ?
C5 C6 C7 C8 2.0(4) . . . . ?
C5 C6 C7 N7 -178.1(2) . . . . ?
O10 N7 C7 C8 -7.6(4) . . . . ?
O9 N7 C7 C8 172.2(3) . . . . ?
O10 N7 C7 C6 172.5(2) . . . . ?
O9 N7 C7 C6 -7.7(4) . . . . ?
C4 C3 C8 C7 0.0(4) . . . . ?
N5 C3 C8 C7 -178.9(2) . . . . ?
C6 C7 C8 C3 -0.8(4) . . . . ?
N7 C7 C8 C3 179.3(2) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H22 O6 1.01(5) 1.92(5) 2.825(3) 149(4) 2
O2 H22 O7 1.01(5) 2.23(5) 2.985(3) 130(3) 2
O2 H21 O1 0.93(4) 1.91(4) 2.833(3) 173(3) 3
O3 H32 N3 1.02(5) 2.35(5) 2.875(3) 111(3) 1_565
O3 H32 O5 1.02(5) 2.46(5) 3.401(3) 154(4) .
O3 H31 O4 0.90(4) 2.63(4) 3.063(3) 110(3) .
O3 H31 O3 0.90(4) 2.10(4) 2.987(2) 169(4) 2_545
O1 H12 O6 1.09(5) 1.71(5) 2.749(3) 159(3) 4_565
O1 H12 O4 1.09(5) 2.15(4) 2.761(3) 113(3) 4_565
O1 H11 O3 0.95(4) 1.76(4) 2.703(3) 168(4) 3_565

_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         0.523
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.071

_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_mx333
_database_code_depnum_ccdc_archive 'CCDC 1566386'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jul 18 14:02:46 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) copper(II) perchlorate di(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) copper(II) perchlorate di(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Cu N24, 2(C2 H4 N4), 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 Cu N32 O8'
_chemical_formula_weight         935.17

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




_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.9979(2)
_cell_length_b                   11.2379(4)
_cell_length_c                   13.4606(5)
_cell_angle_alpha                111.450(3)
_cell_angle_beta                 101.356(3)
_cell_angle_gamma                93.102(3)
_cell_volume                     956.69(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    3363
_cell_measurement_theta_min      4.8360
_cell_measurement_theta_max      32.2270

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.429
_exptl_crystal_size_min          0.291
_exptl_absorpt_coefficient_mu    0.797
_shelx_estimated_absorpt_T_min   0.628
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88416
_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    1.623
_exptl_crystal_F_000             479
_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            6934
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.486
_diffrn_reflns_theta_max         25.987
_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             3748
_reflns_number_gt                3361
_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)+(0.0529P)²+0.7625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3748
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0030189000
_diffrn_orient_matrix_UB_12      -0.0328290000
_diffrn_orient_matrix_UB_13      0.0362509000
_diffrn_orient_matrix_UB_21      -0.0444956000
_diffrn_orient_matrix_UB_22      -0.0579692000
_diffrn_orient_matrix_UB_23      -0.0449620000
_diffrn_orient_matrix_UB_31      0.0943780000
_diffrn_orient_matrix_UB_32      -0.0158133000
_diffrn_orient_matrix_UB_33      -0.0073436000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -23.00    6.40   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 42

#__ type_ start__ end____ width___ exp.time_
  2 omega  -24.00   66.30   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 129

#__ type_ start__ end____ width___ exp.time_
  3 omega  -23.00   69.40   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -150.0000 132

#__ type_ start__ end____ width___ exp.time_
  4 omega   -9.00   41.40   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000   30.0000 72

#__ type_ start__ end____ width___ exp.time_
  5 omega  -97.00  -17.90   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000 -120.0000 113

#__ type_ start__ end____ width___ exp.time_
  6 omega   -3.00   94.30   0.7000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  120.0000 139

;



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 1.0000 0.0000 1.0000 0.01662(12) Uani 1 2 d S . P . .
Cl1 Cl 0.69018(8) -0.21894(6) 0.51041(5) 0.02781(15) Uani 1 1 d . . . . .
C5 C 0.8087(3) 0.2340(2) 0.97806(18) 0.0199(4) Uani 1 1 d . . . . .
H5 H 0.8919 0.2991 1.0414 0.024 Uiso 1 1 calc R U . . .
C2 C 0.4004(4) -0.4326(2) 0.6955(2) 0.0316(5) Uani 1 1 d . . . . .
H2A H 0.2661 -0.4158 0.7011 0.047 Uiso 1 1 calc R U . . .
H2B H 0.4143 -0.5211 0.6894 0.047 Uiso 1 1 calc R U . . .
H2C H 0.4268 -0.4216 0.6303 0.047 Uiso 1 1 calc R U . . .
C4 C 1.2367(4) -0.0231(3) 0.62539(19) 0.0299(5) Uani 1 1 d . . . . .
H4A H 1.1311 -0.0666 0.5593 0.045 Uiso 1 1 calc R U . . .
H4B H 1.3612 -0.0535 0.6114 0.045 Uiso 1 1 calc R U . . .
H4C H 1.2485 0.0704 0.6447 0.045 Uiso 1 1 calc R U . . .
N5 N 1.1909(3) -0.05251(18) 0.71619(15) 0.0208(4) Uani 1 1 d . . . . .
N1 N 0.5403(3) -0.34196(17) 0.79335(15) 0.0211(4) Uani 1 1 d . . . . .
N9 N 0.6657(3) 0.25342(17) 0.90788(15) 0.0190(4) Uani 1 1 d . . . . .
N6 N 1.2074(3) -0.1689(2) 0.72139(17) 0.0314(5) Uani 1 1 d . . . . .
N10 N 0.5816(3) 0.13899(19) 0.82930(17) 0.0301(5) Uani 1 1 d . . . . .
N16 N 0.9950(3) 0.2906(2) 0.79257(18) 0.0308(5) Uani 1 1 d . . . . .
N4 N 0.7578(3) -0.18583(17) 0.91019(15) 0.0218(4) Uani 1 1 d . . . . .
N12 N 0.8164(3) 0.10909(17) 0.94522(14) 0.0181(4) Uani 1 1 d . . . . .
N13 N 0.9120(3) 0.4036(2) 0.69516(17) 0.0277(4) Uani 1 1 d . . . . .
C7 C 0.9040(4) 0.2850(2) 0.6957(2) 0.0296(5) Uani 1 1 d . . . . .
H7 H 0.8419 0.2083 0.6351 0.035 Uiso 1 1 calc R U . . .
N2 N 0.5565(3) -0.35119(19) 0.89121(17) 0.0291(5) Uani 1 1 d . . . . .
N3 N 0.6880(3) -0.25716(19) 0.96138(16) 0.0281(4) Uani 1 1 d . . . . .
N7 N 1.1529(3) -0.16596(19) 0.80868(17) 0.0302(5) Uani 1 1 d . . . . .
N8 N 1.1002(3) -0.04795(17) 0.86058(15) 0.0195(4) Uani 1 1 d . . . . .
N15 N 1.0594(3) 0.4172(2) 0.85312(18) 0.0365(5) Uani 1 1 d . . . . .
N11 N 0.6723(3) 0.05191(19) 0.85196(17) 0.0300(5) Uani 1 1 d . . . . .
N14 N 1.0105(3) 0.4860(2) 0.7959(2) 0.0380(5) Uani 1 1 d . . . . .
C1 C 0.6637(3) -0.2404(2) 0.80640(18) 0.0229(5) Uani 1 1 d . . . . .
H1 H 0.6810 -0.2119 0.7500 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5997(4) 0.3729(2) 0.9027(2) 0.0269(5) Uani 1 1 d . . . . .
H6A H 0.6862 0.4472 0.9612 0.040 Uiso 1 1 calc R U . . .
H6B H 0.4645 0.3759 0.9123 0.040 Uiso 1 1 calc R U . . .
H6C H 0.6041 0.3757 0.8313 0.040 Uiso 1 1 calc R U . . .
C3 C 1.1251(3) 0.0205(2) 0.80107(17) 0.0195(4) Uani 1 1 d . . . . .
H3 H 1.1002 0.1070 0.8166 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8475(4) 0.4474(4) 0.6055(3) 0.0467(8) Uani 1 1 d . . . . .
H8A H 0.9310 0.4195 0.5529 0.070 Uiso 1 1 calc R U . . .
H8B H 0.8580 0.5418 0.6352 0.070 Uiso 1 1 calc R U . . .
H8C H 0.7104 0.4101 0.5683 0.070 Uiso 1 1 calc R U . . .
O1 O 0.5204(4) -0.2226(3) 0.4313(2) 0.0748(8) Uani 1 1 d . . . . .
O2 O 0.8452(4) -0.2471(3) 0.4568(3) 0.0798(9) Uani 1 1 d . . . . .
O4 O 0.6494(5) -0.3162(3) 0.5503(2) 0.0896(10) Uani 1 1 d . . . . .
O3 O 0.7425(4) -0.0945(3) 0.5942(2) 0.0855(11) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N8 2.0306(18) . ?
Cu1 N8 2.0307(18) 2_757 ?
Cu1 N12 2.0388(17) 2_757 ?
Cu1 N12 2.0388(17) . ?
Cu1 N4 2.3789(18) . ?
Cu1 N4 2.3789(18) 2_757 ?
Cl1 O2 1.406(2) . ?
Cl1 O3 1.411(2) . ?
Cl1 O1 1.418(2) . ?
Cl1 O4 1.421(3) . ?
C5 N12 1.317(3) . ?
C5 N9 1.321(3) . ?
C5 H5 0.9500 . ?
C2 N1 1.461(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 N5 1.464(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N5 C3 1.324(3) . ?
N5 N6 1.345(3) . ?
N1 C1 1.329(3) . ?
N1 N2 1.342(3) . ?
N9 N10 1.340(3) . ?
N9 C6 1.464(3) . ?
N6 N7 1.295(3) . ?
N10 N11 1.289(3) . ?
N16 C7 1.311(3) . ?
N16 N15 1.352(3) . ?
N4 C1 1.315(3) . ?
N4 N3 1.360(3) . ?
N12 N11 1.359(3) . ?
N13 C7 1.334(3) . ?
N13 N14 1.348(3) . ?
N13 C8 1.465(3) . ?
C7 H7 0.9500 . ?
N2 N3 1.295(3) . ?
N7 N8 1.364(3) . ?
N8 C3 1.325(3) . ?
N15 N14 1.292(3) . ?
C1 H1 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3 H3 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Cu1 N8 180.0 . 2_757 ?
N8 Cu1 N12 90.85(7) . 2_757 ?
N8 Cu1 N12 89.15(7) 2_757 2_757 ?
N8 Cu1 N12 89.15(7) . . ?
N8 Cu1 N12 90.85(7) 2_757 . ?
N12 Cu1 N12 180.0 2_757 . ?
N8 Cu1 N4 88.76(7) . . ?
N8 Cu1 N4 91.24(7) 2_757 . ?
N12 Cu1 N4 88.86(7) 2_757 . ?
N12 Cu1 N4 91.14(7) . . ?
N8 Cu1 N4 91.24(7) . 2_757 ?
N8 Cu1 N4 88.76(7) 2_757 2_757 ?
N12 Cu1 N4 91.14(7) 2_757 2_757 ?
N12 Cu1 N4 88.86(7) . 2_757 ?
N4 Cu1 N4 180.0 . 2_757 ?
O2 Cl1 O3 108.34(17) . . ?
O2 Cl1 O1 107.5(2) . . ?
O3 Cl1 O1 110.51(18) . . ?
O2 Cl1 O4 109.7(2) . . ?
O3 Cl1 O4 113.0(2) . . ?
O1 Cl1 O4 107.64(17) . . ?
N12 C5 N9 108.29(19) . . ?
N12 C5 H5 125.9 . . ?
N9 C5 H5 125.9 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 N5 N6 108.95(18) . . ?
C3 N5 C4 129.5(2) . . ?
N6 N5 C4 121.51(19) . . ?
C1 N1 N2 108.39(18) . . ?
C1 N1 C2 130.4(2) . . ?
N2 N1 C2 121.20(18) . . ?
C5 N9 N10 108.69(18) . . ?
C5 N9 C6 131.00(19) . . ?
N10 N9 C6 120.25(19) . . ?
N7 N6 N5 106.94(18) . . ?
N11 N10 N9 107.10(18) . . ?
C7 N16 N15 105.5(2) . . ?
C1 N4 N3 106.05(18) . . ?
C1 N4 Cu1 129.60(15) . . ?
N3 N4 Cu1 124.35(14) . . ?
C5 N12 N11 106.42(18) . . ?
C5 N12 Cu1 133.56(15) . . ?
N11 N12 Cu1 119.90(14) . . ?
C7 N13 N14 107.4(2) . . ?
C7 N13 C8 130.6(2) . . ?
N14 N13 C8 121.8(2) . . ?
N16 C7 N13 109.5(2) . . ?
N16 C7 H7 125.2 . . ?
N13 C7 H7 125.2 . . ?
N3 N2 N1 106.86(18) . . ?
N2 N3 N4 109.96(19) . . ?
N6 N7 N8 109.61(18) . . ?
C3 N8 N7 106.37(18) . . ?
C3 N8 Cu1 130.08(15) . . ?
N7 N8 Cu1 123.54(14) . . ?
N14 N15 N16 110.8(2) . . ?
N10 N11 N12 109.51(18) . . ?
N15 N14 N13 106.8(2) . . ?
N4 C1 N1 108.74(19) . . ?
N4 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
N9 C6 H6A 109.5 . . ?
N9 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N9 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C3 N8 108.14(19) . . ?
N5 C3 H3 125.9 . . ?
N8 C3 H3 125.9 . . ?
N13 C8 H8A 109.5 . . ?
N13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 C5 N9 N10 -0.1(2) . . . . ?
N12 C5 N9 C6 -177.1(2) . . . . ?
C3 N5 N6 N7 -0.2(3) . . . . ?
C4 N5 N6 N7 -178.5(2) . . . . ?
C5 N9 N10 N11 0.2(3) . . . . ?
C6 N9 N10 N11 177.6(2) . . . . ?
N9 C5 N12 N11 0.0(2) . . . . ?
N9 C5 N12 Cu1 175.84(14) . . . . ?
N15 N16 C7 N13 0.4(3) . . . . ?
N14 N13 C7 N16 -0.5(3) . . . . ?
C8 N13 C7 N16 174.4(2) . . . . ?
C1 N1 N2 N3 -0.3(3) . . . . ?
C2 N1 N2 N3 -178.7(2) . . . . ?
N1 N2 N3 N4 0.2(3) . . . . ?
C1 N4 N3 N2 -0.1(3) . . . . ?
Cu1 N4 N3 N2 179.40(15) . . . . ?
N5 N6 N7 N8 0.1(3) . . . . ?
N6 N7 N8 C3 0.0(3) . . . . ?
N6 N7 N8 Cu1 178.92(16) . . . . ?
C7 N16 N15 N14 -0.1(3) . . . . ?
N9 N10 N11 N12 -0.2(3) . . . . ?
C5 N12 N11 N10 0.1(3) . . . . ?
Cu1 N12 N11 N10 -176.40(16) . . . . ?
N16 N15 N14 N13 -0.2(3) . . . . ?
C7 N13 N14 N15 0.4(3) . . . . ?
C8 N13 N14 N15 -175.0(2) . . . . ?
N3 N4 C1 N1 -0.2(3) . . . . ?
Cu1 N4 C1 N1 -179.58(14) . . . . ?
N2 N1 C1 N4 0.3(3) . . . . ?
C2 N1 C1 N4 178.5(2) . . . . ?
N6 N5 C3 N8 0.2(2) . . . . ?
C4 N5 C3 N8 178.4(2) . . . . ?
N7 N8 C3 N5 -0.1(2) . . . . ?
Cu1 N8 C3 N5 -178.94(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
C5 H5 N14 0.95 2.54 3.436(3) 157.0 2_767
C2 H2C O4 0.98 2.53 3.396(4) 147.8 .
C4 H4A O2 0.98 2.54 3.409(4) 147.8 .
C7 H7 O1 0.95 2.55 3.022(4) 110.8 2_656
C1 H1 O4 0.95 2.47 3.214(4) 135.4 .
C6 H6A N15 0.98 2.63 3.562(3) 159.4 2_767
C3 H3 N16 0.95 2.34 3.251(3) 161.1 .
C8 H8A O2 0.98 2.54 3.201(4) 124.7 2_756
C8 H8B O4 0.98 2.63 3.312(5) 126.9 1_565
C8 H8C O1 0.98 2.59 3.337(4) 133.4 2_656
C8 H8C O4 0.98 2.63 3.602(4) 173.4 2_656
C5 H5 N14 0.95 2.54 3.436(3) 157.0 2_767
C2 H2C O4 0.98 2.53 3.396(4) 147.8 .
C4 H4A O2 0.98 2.54 3.409(4) 147.8 .
C7 H7 O1 0.95 2.55 3.022(4) 110.8 2_656
C1 H1 O4 0.95 2.47 3.214(4) 135.4 .
C6 H6A N15 0.98 2.63 3.562(3) 159.4 2_767
C3 H3 N16 0.95 2.34 3.251(3) 161.1 .
C8 H8A O2 0.98 2.54 3.201(4) 124.7 2_756
C8 H8B O4 0.98 2.63 3.312(5) 126.9 1_565
C8 H8C O1 0.98 2.59 3.337(4) 133.4 2_656
C8 H8C O4 0.98 2.63 3.602(4) 173.4 2_656

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



_refine_diff_density_max         0.758
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.066

_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_lx216
_database_code_depnum_ccdc_archive 'CCDC 1566367'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Apr 28 14:58:17 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetraaqua bis(1-methyltetrazolyl)cbalt(II) distyphnate dihydrate
;
_chemical_name_common            
' tetraaqua bis(1-methyltetrazolyl)cbalt(II) distyphnate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C4 H16 Co N8 O4, 2(C6 H2 N3 O8), 2(H2 O)'
_chemical_formula_sum            'C16 H24 Co N14 O22'
_chemical_formula_weight         823.42

_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                   15.3750(9)
_cell_length_b                   5.8840(2)
_cell_length_c                   18.4840(8)
_cell_angle_alpha                90
_cell_angle_beta                 114.220(6)
_cell_angle_gamma                90
_cell_volume                     1524.99(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4649
_cell_measurement_theta_min      4.8100
_cell_measurement_theta_max      32.0070

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.682
_shelx_estimated_absorpt_T_min   0.767
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83541
_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    1.793
_exptl_crystal_F_000             842
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            11195
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.224
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.240
_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             2978
_reflns_number_gt                2585
_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)+(0.0292P)²+1.0270P] 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         2978
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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      -0.0384228000
_diffrn_orient_matrix_UB_12      -0.0394361000
_diffrn_orient_matrix_UB_13      0.0084450000
_diffrn_orient_matrix_UB_21      0.0296810000
_diffrn_orient_matrix_UB_22      0.0031075000
_diffrn_orient_matrix_UB_23      0.0411939000
_diffrn_orient_matrix_UB_31      -0.0141306000
_diffrn_orient_matrix_UB_32      0.1138729000
_diffrn_orient_matrix_UB_33      0.0017887000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -62.00   39.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000   90.0000 101

#__ type_ start__ end____ width___ exp.time_
  2 omega   50.00  104.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -30.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega  -80.00  -35.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -129.0000 -138.0000 80

#__ type_ start__ end____ width___ exp.time_
  5 omega  -95.00   47.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000   90.0000 142

#__ type_ start__ end____ width___ exp.time_
  6 omega -111.00  -73.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000 -120.0000 38

;



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'
Co Co 0.3494 0.9721 '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
Co1 Co 0.0000 0.5000 0.5000 0.01263(10) Uani 1 2 d S . P . .
O1 O -0.10779(10) 0.6872(2) 0.41814(8) 0.0221(3) Uani 1 1 d . . . . .
O2 O -0.09635(10) 0.2231(2) 0.47392(8) 0.0166(3) Uani 1 1 d . . . . .
N4 N 0.05225(10) 0.4002(2) 0.41438(8) 0.0157(3) Uani 1 1 d . . . . .
N5 N 0.04762(11) 0.5345(2) 0.35330(9) 0.0195(3) Uani 1 1 d . . . . .
N6 N 0.08489(11) 0.4295(3) 0.31136(9) 0.0203(3) Uani 1 1 d . . . . .
N7 N 0.11438(10) 0.2248(2) 0.34508(8) 0.0162(3) Uani 1 1 d . . . . .
C1 C 0.09405(13) 0.2100(3) 0.40815(10) 0.0166(4) Uani 1 1 d . . . . .
C2 C 0.16386(14) 0.0639(3) 0.31443(11) 0.0214(4) Uani 1 1 d . . . . .
H2A H 0.2322 0.0991 0.3371 0.032 Uiso 1 1 calc R U . . .
H2B H 0.1381 0.0762 0.2565 0.032 Uiso 1 1 calc R U . . .
H2C H 0.1544 -0.0911 0.3292 0.032 Uiso 1 1 calc R U . . .
O3 O 0.25237(9) 0.9885(2) 0.06924(8) 0.0219(3) Uani 1 1 d . . . . .
O4 O 0.31651(9) 1.2242(2) 0.21983(8) 0.0232(3) Uani 1 1 d . . . . .
O5 O 0.26606(10) 0.6221(3) -0.00935(9) 0.0351(4) Uani 1 1 d . . . . .
O6 O 0.39716(10) 0.5559(2) -0.02059(9) 0.0335(4) Uani 1 1 d . . . . .
O7 O 0.53343(11) 1.3902(2) 0.20817(8) 0.0242(3) Uani 1 1 d . . . . .
O8 O 0.67812(9) 0.9615(2) 0.11822(8) 0.0242(3) Uani 1 1 d . . . . .
O9 O 0.68446(9) 1.2413(2) 0.19674(7) 0.0236(3) Uani 1 1 d . . . . .
O10 O 0.34199(12) 1.5231(2) 0.16371(9) 0.0334(4) Uani 1 1 d . . . . .
N1 N 0.34960(11) 0.6660(3) 0.00658(8) 0.0191(3) Uani 1 1 d . . . . .
N2 N 0.63888(11) 1.0885(3) 0.14830(9) 0.0188(3) Uani 1 1 d . . . . .
N3 N 0.34844(10) 1.3189(2) 0.17648(8) 0.0179(3) Uani 1 1 d . . . . .
C3 C 0.34017(12) 1.0027(3) 0.08722(10) 0.0156(4) Uani 1 1 d . . . . .
C4 C 0.39483(12) 0.8562(3) 0.05860(10) 0.0159(4) Uani 1 1 d . . . . .
C5 C 0.39672(12) 1.1778(3) 0.13889(10) 0.0156(4) Uani 1 1 d . . . . .
C6 C 0.49048(13) 0.8870(3) 0.07934(10) 0.0163(4) Uani 1 1 d . . . . .
C7 C 0.49203(13) 1.2177(3) 0.15981(10) 0.0164(4) Uani 1 1 d . . . . .
C8 C 0.53966(13) 1.0648(3) 0.12875(10) 0.0166(4) Uani 1 1 d . . . . .
O11 O 0.13475(11) 0.5570(2) 0.18130(8) 0.0206(3) Uani 1 1 d . . . . .
H1 H 0.1050(14) 0.088(3) 0.4406(11) 0.016(5) Uiso 1 1 d . . . . .
H6 H 0.5234(15) 0.781(3) 0.0608(12) 0.021(5) Uiso 1 1 d . . . . .
H1A H -0.161(2) 0.643(5) 0.4130(17) 0.060(9) Uiso 1 1 d . . . . .
H1B H -0.1127(18) 0.780(4) 0.3854(15) 0.037(7) Uiso 1 1 d . . . . .
H22 H -0.1019(18) 0.174(4) 0.4313(16) 0.039(7) Uiso 1 1 d . . . . .
H7 H 0.589(2) 1.389(5) 0.2171(16) 0.048(8) Uiso 1 1 d . . . . .
H11B H 0.191(2) 0.589(5) 0.2071(16) 0.048(8) Uiso 1 1 d . . . . .
H11A H 0.115(2) 0.533(4) 0.2146(17) 0.047(8) Uiso 1 1 d . . . . .
H21 H -0.152(2) 0.270(5) 0.4673(16) 0.055(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
Co1 O1 2.0474(13) . ?
Co1 O1 2.0474(13) 3_566 ?
Co1 O2 2.1201(12) 3_566 ?
Co1 O2 2.1201(12) . ?
Co1 N4 2.1302(14) 3_566 ?
Co1 N4 2.1303(14) . ?
O1 H1A 0.83(3) . ?
O1 H1B 0.79(3) . ?
O2 H22 0.81(3) . ?
O2 H21 0.85(3) . ?
N4 C1 1.319(2) . ?
N4 N5 1.356(2) . ?
N5 N6 1.294(2) . ?
N6 N7 1.347(2) . ?
N7 C1 1.328(2) . ?
N7 C2 1.466(2) . ?
C1 H1 0.91(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C3 1.254(2) . ?
O4 N3 1.2313(19) . ?
O5 N1 1.222(2) . ?
O6 N1 1.228(2) . ?
O7 C7 1.329(2) . ?
O7 H7 0.80(3) . ?
O8 N2 1.228(2) . ?
O9 N2 1.2593(19) . ?
O10 N3 1.220(2) . ?
N1 C4 1.453(2) . ?
N2 C8 1.423(2) . ?
N3 C5 1.465(2) . ?
C3 C5 1.431(2) . ?
C3 C4 1.447(2) . ?
C4 C6 1.371(2) . ?
C5 C7 1.374(2) . ?
C6 C8 1.391(2) . ?
C6 H6 0.95(2) . ?
C7 C8 1.421(2) . ?
O11 H11B 0.82(3) . ?
O11 H11A 0.80(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
O1 Co1 O1 180.0 . 3_566 ?
O1 Co1 O2 91.88(5) . 3_566 ?
O1 Co1 O2 88.12(5) 3_566 3_566 ?
O1 Co1 O2 88.12(5) . . ?
O1 Co1 O2 91.88(5) 3_566 . ?
O2 Co1 O2 180.00(6) 3_566 . ?
O1 Co1 N4 87.88(6) . 3_566 ?
O1 Co1 N4 92.12(6) 3_566 3_566 ?
O2 Co1 N4 93.47(5) 3_566 3_566 ?
O2 Co1 N4 86.53(5) . 3_566 ?
O1 Co1 N4 92.12(6) . . ?
O1 Co1 N4 87.88(6) 3_566 . ?
O2 Co1 N4 86.53(5) 3_566 . ?
O2 Co1 N4 93.47(5) . . ?
N4 Co1 N4 180.0 3_566 . ?
Co1 O1 H1A 112(2) . . ?
Co1 O1 H1B 136.6(18) . . ?
H1A O1 H1B 110(3) . . ?
Co1 O2 H22 106.4(18) . . ?
Co1 O2 H21 110.4(19) . . ?
H22 O2 H21 106(3) . . ?
C1 N4 N5 106.43(14) . . ?
C1 N4 Co1 130.15(12) . . ?
N5 N4 Co1 123.42(11) . . ?
N6 N5 N4 109.59(14) . . ?
N5 N6 N7 107.31(14) . . ?
C1 N7 N6 108.00(14) . . ?
C1 N7 C2 130.04(15) . . ?
N6 N7 C2 121.89(14) . . ?
N4 C1 N7 108.66(15) . . ?
N4 C1 H1 125.4(12) . . ?
N7 C1 H1 125.9(12) . . ?
N7 C2 H2A 109.5 . . ?
N7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C7 O7 H7 108(2) . . ?
O5 N1 O6 122.23(15) . . ?
O5 N1 C4 119.52(14) . . ?
O6 N1 C4 118.24(15) . . ?
O8 N2 O9 121.53(15) . . ?
O8 N2 C8 120.01(15) . . ?
O9 N2 C8 118.46(15) . . ?
O10 N3 O4 123.30(15) . . ?
O10 N3 C5 118.89(15) . . ?
O4 N3 C5 117.82(14) . . ?
O3 C3 C5 121.20(16) . . ?
O3 C3 C4 125.96(16) . . ?
C5 C3 C4 112.82(15) . . ?
C6 C4 C3 122.43(16) . . ?
C6 C4 N1 117.00(15) . . ?
C3 C4 N1 120.56(15) . . ?
C7 C5 C3 126.65(16) . . ?
C7 C5 N3 117.32(15) . . ?
C3 C5 N3 115.93(15) . . ?
C4 C6 C8 120.99(16) . . ?
C4 C6 H6 118.7(12) . . ?
C8 C6 H6 120.2(12) . . ?
O7 C7 C5 118.76(16) . . ?
O7 C7 C8 124.82(16) . . ?
C5 C7 C8 116.41(15) . . ?
C6 C8 C7 120.67(16) . . ?
C6 C8 N2 118.55(16) . . ?
C7 C8 N2 120.77(16) . . ?
H11B O11 H11A 104(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N5 N6 0.2(2) . . . . ?
Co1 N4 N5 N6 179.88(11) . . . . ?
N4 N5 N6 N7 -0.09(19) . . . . ?
N5 N6 N7 C1 -0.09(19) . . . . ?
N5 N6 N7 C2 -177.47(15) . . . . ?
N5 N4 C1 N7 -0.30(19) . . . . ?
Co1 N4 C1 N7 -179.90(11) . . . . ?
N6 N7 C1 N4 0.3(2) . . . . ?
C2 N7 C1 N4 177.34(17) . . . . ?
O3 C3 C4 C6 178.06(17) . . . . ?
C5 C3 C4 C6 -0.4(2) . . . . ?
O3 C3 C4 N1 -2.7(3) . . . . ?
C5 C3 C4 N1 178.82(14) . . . . ?
O5 N1 C4 C6 175.12(16) . . . . ?
O6 N1 C4 C6 -5.6(2) . . . . ?
O5 N1 C4 C3 -4.2(2) . . . . ?
O6 N1 C4 C3 175.08(16) . . . . ?
O3 C3 C5 C7 -176.59(17) . . . . ?
C4 C3 C5 C7 2.0(2) . . . . ?
O3 C3 C5 N3 7.2(2) . . . . ?
C4 C3 C5 N3 -174.18(14) . . . . ?
O10 N3 C5 C7 63.8(2) . . . . ?
O4 N3 C5 C7 -115.97(18) . . . . ?
O10 N3 C5 C3 -119.63(18) . . . . ?
O4 N3 C5 C3 60.6(2) . . . . ?
C3 C4 C6 C8 -0.8(3) . . . . ?
N1 C4 C6 C8 179.88(15) . . . . ?
C3 C5 C7 O7 179.34(16) . . . . ?
N3 C5 C7 O7 -4.5(2) . . . . ?
C3 C5 C7 C8 -2.1(3) . . . . ?
N3 C5 C7 C8 174.03(14) . . . . ?
C4 C6 C8 C7 0.8(3) . . . . ?
C4 C6 C8 N2 180.00(15) . . . . ?
O7 C7 C8 C6 179.07(16) . . . . ?
C5 C7 C8 C6 0.6(2) . . . . ?
O7 C7 C8 N2 -0.1(3) . . . . ?
C5 C7 C8 N2 -178.60(15) . . . . ?
O8 N2 C8 C6 4.0(2) . . . . ?
O9 N2 C8 C6 -175.87(15) . . . . ?
O8 N2 C8 C7 -176.73(15) . . . . ?
O9 N2 C8 C7 3.4(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
O1 H1B O11 0.79(3) 1.99(3) 2.7674(19) 167(2) 2
O2 H22 O11 0.81(3) 2.05(3) 2.8543(19) 172(2) 2_545
O7 H7 O9 0.80(3) 1.87(3) 2.571(2) 145(3) .
O7 H7 O4 0.80(3) 2.44(3) 2.9048(19) 118(2) 2_655
O7 H7 N2 0.80(3) 2.47(3) 2.911(2) 115(2) .
O11 H11A N6 0.80(3) 2.11(3) 2.905(2) 170(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         0.300
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.053

_shelxl_version_number           2013-4


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

data_lx138
_database_code_depnum_ccdc_archive 'CCDC 1566361'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Mar 16 20:08:53 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
'hexakis(1-methyltetrazolato) zinc(II) perchlorate'
;
_chemical_name_common            
'hexakis(1-methyltetrazolato) zinc(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 N24 Zn, 2(Cl O4)'
_chemical_formula_sum            'C12 H24 Cl2 N24 O8 Zn'
_chemical_formula_weight         768.82

_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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_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                   17.9700(18)
_cell_length_b                   10.2320(7)
_cell_length_c                   18.5730(17)
_cell_angle_alpha                90
_cell_angle_beta                 113.811(11)
_cell_angle_gamma                90
_cell_volume                     3124.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1696
_cell_measurement_theta_min      4.2050
_cell_measurement_theta_max      25.5620

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.037
_shelx_estimated_absorpt_T_min   0.713
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87933
_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.
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    1.634
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            15544
_diffrn_reflns_av_unetI/netI     0.1065
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1978
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.112
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_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             6113
_reflns_number_gt                3309
_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)+(0.0714P)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         6113
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1468
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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      0.0413525000
_diffrn_orient_matrix_UB_12      -0.0067340000
_diffrn_orient_matrix_UB_13      0.0059568000
_diffrn_orient_matrix_UB_21      -0.0113879000
_diffrn_orient_matrix_UB_22      0.0035812000
_diffrn_orient_matrix_UB_23      -0.0412531000
_diffrn_orient_matrix_UB_31      0.0046340000
_diffrn_orient_matrix_UB_32      0.0688806000
_diffrn_orient_matrix_UB_33      0.0027525000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00  103.00   1.0000   14.0000
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   14.0000
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   14.0000
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'
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 0.5000 0.5000 0.5000 0.0268(2) Uani 1 2 d S . P . .
N1 N 0.4253(3) 0.3348(4) 0.4994(3) 0.0303(10) Uani 1 1 d . . . . .
N2 N 0.3737(3) 0.3329(4) 0.5372(3) 0.0387(12) Uani 1 1 d . . . . .
N3 N 0.3325(3) 0.2253(5) 0.5214(3) 0.0394(12) Uani 1 1 d . . . . .
N4 N 0.3571(3) 0.1559(4) 0.4726(3) 0.0336(11) Uani 1 1 d . . . . .
N5 N 0.4302(2) 0.6183(4) 0.5441(2) 0.0287(10) Uani 1 1 d . . . . .
N6 N 0.3649(3) 0.6908(5) 0.4979(3) 0.0408(12) Uani 1 1 d . . . . .
N7 N 0.3253(3) 0.7294(5) 0.5377(3) 0.0420(12) Uani 1 1 d . . . . .
N8 N 0.3638(3) 0.6796(4) 0.6110(3) 0.0322(11) Uani 1 1 d . . . . .
N9 N 0.3424(2) 0.6503(4) 0.2729(2) 0.0287(10) Uani 1 1 d . . . . .
N10 N 0.3139(3) 0.5259(4) 0.2662(3) 0.0360(11) Uani 1 1 d . . . . .
N11 N 0.3596(3) 0.4663(4) 0.3300(3) 0.0353(11) Uani 1 1 d . . . . .
N12 N 0.4175(3) 0.5488(4) 0.3776(2) 0.0299(10) Uani 1 1 d . . . . .
C1 C 0.4129(4) 0.2232(6) 0.4608(3) 0.0325(13) Uani 1 1 d . . . . .
C2 C 0.3266(4) 0.0237(5) 0.4467(4) 0.0467(16) Uani 1 1 d . . . . .
H2A H 0.2839 0.0025 0.4649 0.070 Uiso 1 1 calc R U . . .
H2B H 0.3713 -0.0391 0.4688 0.070 Uiso 1 1 calc R U . . .
H2C H 0.3043 0.0195 0.3891 0.070 Uiso 1 1 calc R U . . .
C3 C 0.4262(4) 0.6137(6) 0.6130(3) 0.0343(14) Uani 1 1 d . . . . .
C4 C 0.3347(4) 0.7055(7) 0.6726(4) 0.0544(18) Uani 1 1 d . . . . .
H4A H 0.2856 0.7597 0.6512 0.082 Uiso 1 1 calc R U . . .
H4B H 0.3770 0.7516 0.7163 0.082 Uiso 1 1 calc R U . . .
H4C H 0.3221 0.6226 0.6916 0.082 Uiso 1 1 calc R U . . .
C5 C 0.4054(3) 0.6603(6) 0.3410(3) 0.0314(13) Uani 1 1 d . . . . .
C6 C 0.3050(4) 0.7450(6) 0.2096(3) 0.0455(16) Uani 1 1 d . . . . .
H6A H 0.2585 0.7044 0.1672 0.068 Uiso 1 1 calc R U . . .
H6B H 0.3449 0.7730 0.1893 0.068 Uiso 1 1 calc R U . . .
H6C H 0.2864 0.8209 0.2300 0.068 Uiso 1 1 calc R U . . .
Zn2 Zn 0.0000 0.5000 0.5000 0.0407(3) Uani 1 2 d S . P . .
N13 N 0.0865(3) 0.5392(5) 0.4478(3) 0.0417(12) Uani 1 1 d . . . . .
N14 N 0.1423(3) 0.4513(5) 0.4472(3) 0.0515(14) Uani 1 1 d . . . . .
N15 N 0.1843(3) 0.4982(5) 0.4101(3) 0.0489(14) Uani 1 1 d . . . . .
N16 N 0.1548(3) 0.6205(5) 0.3871(3) 0.0362(11) Uani 1 1 d . . . . .
N17 N -0.0645(3) 0.3733(5) 0.4015(3) 0.0427(12) Uani 1 1 d . . . . .
N18 N -0.1182(3) 0.2804(6) 0.4024(3) 0.0506(14) Uani 1 1 d . . . . .
N19 N -0.1490(3) 0.2218(6) 0.3358(3) 0.0576(15) Uani 1 1 d . . . . .
N20 N -0.1143(3) 0.2741(5) 0.2907(3) 0.0433(13) Uani 1 1 d . . . . .
N21 N 0.0728(3) 0.3349(5) 0.5625(3) 0.0455(13) Uani 1 1 d . . . . .
N22 N 0.1208(4) 0.3361(6) 0.6404(3) 0.0627(17) Uani 1 1 d . . . . .
N23 N 0.1670(4) 0.2349(6) 0.6590(3) 0.0626(17) Uani 1 1 d . . . . .
N24 N 0.1493(3) 0.1656(5) 0.5923(3) 0.0408(12) Uani 1 1 d . . . . .
C7 C 0.0956(4) 0.6416(6) 0.4102(4) 0.0416(15) Uani 1 1 d . . . . .
C8 C 0.1858(4) 0.7006(6) 0.3402(3) 0.0412(15) Uani 1 1 d . . . . .
H8A H 0.2314 0.6556 0.3348 0.062 Uiso 1 1 calc R U . . .
H8B H 0.2044 0.7849 0.3663 0.062 Uiso 1 1 calc R U . . .
H8C H 0.1425 0.7150 0.2879 0.062 Uiso 1 1 calc R U . . .
C9 C -0.0627(4) 0.3645(7) 0.3322(4) 0.0481(17) Uani 1 1 d . . . . .
C10 C -0.1308(4) 0.2224(7) 0.2126(4) 0.0552(18) Uani 1 1 d . . . . .
H10A H -0.1731 0.1553 0.1992 0.083 Uiso 1 1 calc R U . . .
H10B H -0.0810 0.1839 0.2123 0.083 Uiso 1 1 calc R U . . .
H10C H -0.1493 0.2934 0.1740 0.083 Uiso 1 1 calc R U . . .
C11 C 0.0915(4) 0.2279(6) 0.5352(4) 0.0441(16) Uani 1 1 d . . . . .
C12 C 0.1924(4) 0.0437(6) 0.5919(4) 0.0506(17) Uani 1 1 d . . . . .
H12A H 0.2323 0.0250 0.6453 0.076 Uiso 1 1 calc R U . . .
H12B H 0.2203 0.0532 0.5566 0.076 Uiso 1 1 calc R U . . .
H12C H 0.1532 -0.0283 0.5737 0.076 Uiso 1 1 calc R U . . .
Cl1 Cl 0.04599(11) 0.00373(15) 0.35187(10) 0.0476(4) Uani 1 1 d . . . . .
O1A O 0.0493(5) 0.1456(8) 0.3522(6) 0.068(4) Uani 0.558(14) 1 d . . P A 1
O2A O -0.0084(7) 0.0454(17) 0.3857(7) 0.084(4) Uani 0.558(14) 1 d . . P A 1
O4A O 0.0306(8) -0.0484(15) 0.2827(6) 0.097(5) Uani 0.558(14) 1 d . . P A 1
O1B O 0.0296(7) 0.0805(16) 0.2807(9) 0.085(6) Uani 0.442(14) 1 d . . P A 2
O2B O 0.0019(12) -0.0422(18) 0.3901(14) 0.113(8) Uani 0.442(14) 1 d . . P A 2
O4B O 0.0013(10) -0.1225(13) 0.3154(11) 0.107(7) Uani 0.442(14) 1 d . . P A 2
O3 O 0.1267(3) -0.0265(6) 0.4024(3) 0.0856(18) Uani 1 1 d . . . . .
Cl2 Cl 0.50229(9) 0.01386(13) 0.33341(8) 0.0355(4) Uani 1 1 d . . . . .
O5 O 0.5869(3) 0.0110(4) 0.3493(3) 0.0538(12) Uani 1 1 d . . . . .
O6 O 0.4750(3) 0.1471(4) 0.3265(2) 0.0523(11) Uani 1 1 d . . . . .
O7 O 0.4570(3) -0.0537(4) 0.2613(2) 0.0527(12) Uani 1 1 d . . . . .
O8 O 0.4887(3) -0.0476(4) 0.3967(2) 0.0499(11) Uani 1 1 d . . . . .
H5 H 0.437(3) 0.729(5) 0.363(3) 0.026(14) Uiso 1 1 d . . . . .
H3 H 0.463(3) 0.579(5) 0.652(3) 0.031(16) Uiso 1 1 d . . . . .
H1 H 0.440(3) 0.193(6) 0.435(4) 0.048(19) Uiso 1 1 d . . . . .
H9 H -0.038(4) 0.420(7) 0.311(4) 0.07(2) Uiso 1 1 d . . . . .
H7 H 0.060(3) 0.710(5) 0.402(3) 0.029(14) Uiso 1 1 d . . . . .
H11 H 0.064(3) 0.211(6) 0.480(4) 0.053(18) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N5 2.131(4) . ?
Zn1 N5 2.131(4) 3_666 ?
Zn1 N1 2.156(4) 3_666 ?
Zn1 N1 2.156(4) . ?
Zn1 N12 2.212(4) 3_666 ?
Zn1 N12 2.212(4) . ?
N1 C1 1.319(7) . ?
N1 N2 1.370(6) . ?
N2 N3 1.293(6) . ?
N3 N4 1.358(6) . ?
N4 C1 1.306(7) . ?
N4 C2 1.465(7) . ?
N5 C3 1.310(7) . ?
N5 N6 1.361(6) . ?
N6 N7 1.278(6) . ?
N7 N8 1.354(6) . ?
N8 C3 1.297(7) . ?
N8 C4 1.460(7) . ?
N9 C5 1.318(7) . ?
N9 N10 1.359(6) . ?
N9 C6 1.461(7) . ?
N10 N11 1.291(6) . ?
N11 N12 1.355(6) . ?
N12 C5 1.300(7) . ?
C1 H1 0.86(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.83(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 0.89(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Zn2 N17 2.158(5) . ?
Zn2 N17 2.158(5) 3_566 ?
Zn2 N21 2.165(5) 3_566 ?
Zn2 N21 2.165(5) . ?
Zn2 N13 2.176(5) . ?
Zn2 N13 2.176(5) 3_566 ?
N13 C7 1.306(7) . ?
N13 N14 1.350(7) . ?
N14 N15 1.301(6) . ?
N15 N16 1.359(6) . ?
N16 C7 1.316(7) . ?
N16 C8 1.462(7) . ?
N17 C9 1.304(7) . ?
N17 N18 1.359(7) . ?
N18 N19 1.281(7) . ?
N19 N20 1.342(6) . ?
N20 C9 1.316(8) . ?
N20 C10 1.457(7) . ?
N21 C11 1.306(8) . ?
N21 N22 1.353(7) . ?
N22 N23 1.284(7) . ?
N23 N24 1.349(7) . ?
N24 C11 1.311(7) . ?
N24 C12 1.469(7) . ?
C7 H7 0.92(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.90(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.96(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
Cl1 O4A 1.312(10) . ?
Cl1 O2B 1.344(15) . ?
Cl1 O3 1.407(5) . ?
Cl1 O2A 1.423(11) . ?
Cl1 O1A 1.453(8) . ?
Cl1 O1B 1.461(13) . ?
Cl1 O4B 1.527(13) . ?
O1A O2A 1.741(17) . ?
O2B O4B 1.61(3) . ?
Cl2 O5 1.427(4) . ?
Cl2 O7 1.433(4) . ?
Cl2 O6 1.437(4) . ?
Cl2 O8 1.439(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
N5 Zn1 N5 180.0 . 3_666 ?
N5 Zn1 N1 90.85(16) . 3_666 ?
N5 Zn1 N1 89.15(16) 3_666 3_666 ?
N5 Zn1 N1 89.15(16) . . ?
N5 Zn1 N1 90.85(16) 3_666 . ?
N1 Zn1 N1 180.0 3_666 . ?
N5 Zn1 N12 89.28(16) . 3_666 ?
N5 Zn1 N12 90.72(16) 3_666 3_666 ?
N1 Zn1 N12 90.82(16) 3_666 3_666 ?
N1 Zn1 N12 89.18(16) . 3_666 ?
N5 Zn1 N12 90.72(16) . . ?
N5 Zn1 N12 89.28(16) 3_666 . ?
N1 Zn1 N12 89.18(16) 3_666 . ?
N1 Zn1 N12 90.82(16) . . ?
N12 Zn1 N12 180.0 3_666 . ?
C1 N1 N2 105.4(4) . . ?
C1 N1 Zn1 130.5(4) . . ?
N2 N1 Zn1 123.9(3) . . ?
N3 N2 N1 109.9(4) . . ?
N2 N3 N4 106.6(4) . . ?
C1 N4 N3 108.4(5) . . ?
C1 N4 C2 130.0(5) . . ?
N3 N4 C2 121.4(5) . . ?
C3 N5 N6 105.2(5) . . ?
C3 N5 Zn1 128.9(4) . . ?
N6 N5 Zn1 123.9(3) . . ?
N7 N6 N5 110.0(4) . . ?
N6 N7 N8 106.8(4) . . ?
C3 N8 N7 108.0(4) . . ?
C3 N8 C4 130.6(5) . . ?
N7 N8 C4 121.4(5) . . ?
C5 N9 N10 107.9(4) . . ?
C5 N9 C6 131.2(5) . . ?
N10 N9 C6 120.8(4) . . ?
N11 N10 N9 106.3(4) . . ?
N10 N11 N12 109.9(4) . . ?
C5 N12 N11 106.5(4) . . ?
C5 N12 Zn1 129.5(4) . . ?
N11 N12 Zn1 123.3(3) . . ?
N4 C1 N1 109.7(5) . . ?
N4 C1 H1 123(4) . . ?
N1 C1 H1 127(4) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N8 C3 N5 110.0(5) . . ?
N8 C3 H3 128(4) . . ?
N5 C3 H3 122(4) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N12 C5 N9 109.3(5) . . ?
N12 C5 H5 121(3) . . ?
N9 C5 H5 130(3) . . ?
N9 C6 H6A 109.5 . . ?
N9 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N9 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N17 Zn2 N17 180.0(2) . 3_566 ?
N17 Zn2 N21 90.72(19) . 3_566 ?
N17 Zn2 N21 89.28(19) 3_566 3_566 ?
N17 Zn2 N21 89.28(19) . . ?
N17 Zn2 N21 90.72(19) 3_566 . ?
N21 Zn2 N21 180.00(17) 3_566 . ?
N17 Zn2 N13 88.20(18) . . ?
N17 Zn2 N13 91.80(18) 3_566 . ?
N21 Zn2 N13 90.17(18) 3_566 . ?
N21 Zn2 N13 89.83(18) . . ?
N17 Zn2 N13 91.80(18) . 3_566 ?
N17 Zn2 N13 88.20(18) 3_566 3_566 ?
N21 Zn2 N13 89.83(18) 3_566 3_566 ?
N21 Zn2 N13 90.17(18) . 3_566 ?
N13 Zn2 N13 180.0 . 3_566 ?
C7 N13 N14 106.1(5) . . ?
C7 N13 Zn2 130.7(4) . . ?
N14 N13 Zn2 123.2(4) . . ?
N15 N14 N13 110.5(5) . . ?
N14 N15 N16 105.7(5) . . ?
C7 N16 N15 108.2(5) . . ?
C7 N16 C8 131.0(5) . . ?
N15 N16 C8 120.7(5) . . ?
C9 N17 N18 105.3(5) . . ?
C9 N17 Zn2 131.3(4) . . ?
N18 N17 Zn2 123.4(4) . . ?
N19 N18 N17 110.4(5) . . ?
N18 N19 N20 106.7(5) . . ?
C9 N20 N19 108.1(5) . . ?
C9 N20 C10 130.5(5) . . ?
N19 N20 C10 121.2(5) . . ?
C11 N21 N22 105.7(5) . . ?
C11 N21 Zn2 129.8(4) . . ?
N22 N21 Zn2 123.6(4) . . ?
N23 N22 N21 110.1(5) . . ?
N22 N23 N24 106.9(5) . . ?
C11 N24 N23 107.6(5) . . ?
C11 N24 C12 131.0(5) . . ?
N23 N24 C12 121.4(5) . . ?
N13 C7 N16 109.5(6) . . ?
N13 C7 H7 118(3) . . ?
N16 C7 H7 132(3) . . ?
N16 C8 H8A 109.5 . . ?
N16 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N16 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N17 C9 N20 109.5(6) . . ?
N17 C9 H9 126(4) . . ?
N20 C9 H9 123(4) . . ?
N20 C10 H10A 109.5 . . ?
N20 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N20 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N21 C11 N24 109.7(6) . . ?
N21 C11 H11 117(4) . . ?
N24 C11 H11 133(4) . . ?
N24 C12 H12A 109.5 . . ?
N24 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N24 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4A Cl1 O3 108.5(6) . . ?
O2B Cl1 O3 103.8(10) . . ?
O4A Cl1 O2A 129.9(7) . . ?
O3 Cl1 O2A 118.6(6) . . ?
O4A Cl1 O1A 113.7(8) . . ?
O3 Cl1 O1A 100.8(4) . . ?
O2A Cl1 O1A 74.5(9) . . ?
O2B Cl1 O1B 136.0(10) . . ?
O3 Cl1 O1B 119.9(5) . . ?
O2B Cl1 O4B 67.8(14) . . ?
O3 Cl1 O4B 109.0(6) . . ?
O1B Cl1 O4B 100.1(9) . . ?
Cl1 O1A O2A 52.0(6) . . ?
Cl1 O2A O1A 53.5(5) . . ?
Cl1 O2B O4B 61.5(11) . . ?
Cl1 O4B O2B 50.7(7) . . ?
O5 Cl2 O7 109.8(3) . . ?
O5 Cl2 O6 109.6(3) . . ?
O7 Cl2 O6 109.3(3) . . ?
O5 Cl2 O8 109.9(3) . . ?
O7 Cl2 O8 109.5(3) . . ?
O6 Cl2 O8 108.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.3(6) . . . . ?
Zn1 N1 N2 N3 175.0(3) . . . . ?
N1 N2 N3 N4 -0.1(6) . . . . ?
N2 N3 N4 C1 0.4(6) . . . . ?
N2 N3 N4 C2 175.9(5) . . . . ?
C3 N5 N6 N7 1.3(6) . . . . ?
Zn1 N5 N6 N7 166.6(4) . . . . ?
N5 N6 N7 N8 -1.3(6) . . . . ?
N6 N7 N8 C3 0.8(6) . . . . ?
N6 N7 N8 C4 179.6(5) . . . . ?
C5 N9 N10 N11 0.7(6) . . . . ?
C6 N9 N10 N11 179.0(4) . . . . ?
N9 N10 N11 N12 -0.5(6) . . . . ?
N10 N11 N12 C5 0.2(6) . . . . ?
N10 N11 N12 Zn1 171.6(3) . . . . ?
N3 N4 C1 N1 -0.6(6) . . . . ?
C2 N4 C1 N1 -175.6(5) . . . . ?
N2 N1 C1 N4 0.5(6) . . . . ?
Zn1 N1 C1 N4 -174.3(3) . . . . ?
N7 N8 C3 N5 0.0(6) . . . . ?
C4 N8 C3 N5 -178.6(5) . . . . ?
N6 N5 C3 N8 -0.8(6) . . . . ?
Zn1 N5 C3 N8 -165.1(4) . . . . ?
N11 N12 C5 N9 0.2(6) . . . . ?
Zn1 N12 C5 N9 -170.5(3) . . . . ?
N10 N9 C5 N12 -0.5(6) . . . . ?
C6 N9 C5 N12 -178.6(5) . . . . ?
C7 N13 N14 N15 -0.2(7) . . . . ?
Zn2 N13 N14 N15 177.9(4) . . . . ?
N13 N14 N15 N16 0.7(7) . . . . ?
N14 N15 N16 C7 -1.0(7) . . . . ?
N14 N15 N16 C8 -177.2(5) . . . . ?
C9 N17 N18 N19 -2.1(7) . . . . ?
Zn2 N17 N18 N19 178.4(4) . . . . ?
N17 N18 N19 N20 1.4(7) . . . . ?
N18 N19 N20 C9 -0.1(8) . . . . ?
N18 N19 N20 C10 175.0(6) . . . . ?
C11 N21 N22 N23 0.7(8) . . . . ?
Zn2 N21 N22 N23 -169.1(4) . . . . ?
N21 N22 N23 N24 0.0(8) . . . . ?
N22 N23 N24 C11 -0.7(7) . . . . ?
N22 N23 N24 C12 178.9(5) . . . . ?
N14 N13 C7 N16 -0.4(7) . . . . ?
Zn2 N13 C7 N16 -178.3(4) . . . . ?
N15 N16 C7 N13 0.8(7) . . . . ?
C8 N16 C7 N13 176.5(5) . . . . ?
N18 N17 C9 N20 2.0(7) . . . . ?
Zn2 N17 C9 N20 -178.5(4) . . . . ?
N19 N20 C9 N17 -1.2(8) . . . . ?
C10 N20 C9 N17 -175.7(6) . . . . ?
N22 N21 C11 N24 -1.1(7) . . . . ?
Zn2 N21 C11 N24 167.8(4) . . . . ?
N23 N24 C11 N21 1.1(7) . . . . ?
C12 N24 C11 N21 -178.4(6) . . . . ?
O4A Cl1 O1A O2A 127.3(8) . . . . ?
O2B Cl1 O1A O2A -6.9(14) . . . . ?
O3 Cl1 O1A O2A -116.9(6) . . . . ?
O1B Cl1 O1A O2A 124.5(8) . . . . ?
O4B Cl1 O1A O2A 77(2) . . . . ?
O4A Cl1 O2A O1A -108.2(12) . . . . ?
O2B Cl1 O2A O1A 170(2) . . . . ?
O3 Cl1 O2A O1A 94.1(7) . . . . ?
O1B Cl1 O2A O1A -47.0(7) . . . . ?
O4B Cl1 O2A O1A -150.0(7) . . . . ?
O4A Cl1 O2B O4B 13.7(12) . . . . ?
O3 Cl1 O2B O4B -105.1(8) . . . . ?
O2A Cl1 O2B O4B 136(2) . . . . ?
O1A Cl1 O2B O4B 146.8(7) . . . . ?
O1B Cl1 O2B O4B 81.4(15) . . . . ?
O4A Cl1 O4B O2B -163.8(15) . . . . ?
O3 Cl1 O4B O2B 97.6(11) . . . . ?
O2A Cl1 O4B O2B -25.7(12) . . . . ?
O1A Cl1 O4B O2B -96.6(19) . . . . ?
O1B Cl1 O4B O2B -135.8(10) . . . . ?

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         1.111
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.100

_shelxl_version_number           2013-4


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

data_lx198
_database_code_depnum_ccdc_archive 'CCDC 1566362'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Apr 18 19:51:17 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
di(1-methyl-tetrazolyl) manganese(II) dichloride
;
_chemical_name_common            
'di(1-methyl-tetrazolyl) manganese(II) dichloride'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C4 H8 Cl2 Mn N8'
_chemical_formula_sum            'C4 H8 Cl2 Mn N8'
_chemical_formula_weight         294.02

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



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.4607(9)
_cell_length_b                   6.7022(4)
_cell_length_c                   7.0108(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.511(8)
_cell_angle_gamma                90
_cell_volume                     525.73(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2035
_cell_measurement_theta_min      5.1580
_cell_measurement_theta_max      32.1270

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.744
_shelx_estimated_absorpt_T_min   0.722
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37895
_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    1.857
_exptl_crystal_F_000             294
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            3702
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.256
_diffrn_reflns_theta_max         25.991
_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             1028
_reflns_number_gt                951
_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)+(0.1348P)²+5.6821P] 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         1028
_refine_ls_number_parameters     75
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0848
_refine_ls_wR_factor_ref         0.2323
_refine_ls_wR_factor_gt          0.2299
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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      0.0555903000
_diffrn_orient_matrix_UB_12      0.0421070000
_diffrn_orient_matrix_UB_13      0.0467697000
_diffrn_orient_matrix_UB_21      0.0035770000
_diffrn_orient_matrix_UB_22      -0.0676929000
_diffrn_orient_matrix_UB_23      0.0788215000
_diffrn_orient_matrix_UB_31      0.0302917000
_diffrn_orient_matrix_UB_32      -0.0695265000
_diffrn_orient_matrix_UB_33      -0.0483672000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -110.00  -42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -30.0000 68

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00    6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -84.0000  123.0000 38

#__ type_ start__ end____ width___ exp.time_
  3 omega   49.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  120.0000 51

#__ type_ start__ end____ width___ exp.time_
  4 omega  -40.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  5 omega   17.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 57

#__ type_ start__ end____ width___ exp.time_
  6 omega   -4.00   31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   84.0000 -116.0000 35

#__ type_ start__ end____ width___ exp.time_
  7 omega  -41.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  150.0000 133

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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 0.0000 0.0132(5) Uani 1 2 d S . P . .
Cl1 Cl 0.07387(14) 0.7547(2) -0.2203(2) 0.0155(5) Uani 1 1 d . . . . .
N1 N 0.1764(5) 0.3443(8) 0.0575(8) 0.0153(11) Uani 1 1 d . . . . .
N2 N 0.2883(6) 0.4192(9) 0.0632(11) 0.0314(16) Uani 1 1 d . . . . .
N3 N 0.3649(6) 0.2748(10) 0.0776(13) 0.0341(17) Uani 1 1 d . . . . .
N4 N 0.3040(5) 0.1046(8) 0.0872(10) 0.0222(13) Uani 1 1 d . . . . .
C1 C 0.1887(6) 0.1501(10) 0.0695(9) 0.0163(13) Uani 1 1 d . . . . .
C2 C 0.3634(7) -0.0883(11) 0.1087(15) 0.0343(19) Uani 1 1 d . . . . .
H2A H 0.3076 -0.1908 0.1338 0.052 Uiso 1 1 calc R U . . .
H2B H 0.4328 -0.0833 0.2184 0.052 Uiso 1 1 calc R U . . .
H2C H 0.3898 -0.1208 -0.0115 0.052 Uiso 1 1 calc R U . . .
H1 H 0.141(10) 0.057(19) 0.076(18) 0.05(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
Mn1 N1 2.233(5) 3_565 ?
Mn1 N1 2.233(5) . ?
Mn1 Cl1 2.5587(14) 4_576 ?
Mn1 Cl1 2.5587(14) 2_544 ?
Mn1 Cl1 2.5654(14) 3_565 ?
Mn1 Cl1 2.5654(14) . ?
Cl1 Mn1 2.5587(14) 2_554 ?
N1 C1 1.310(9) . ?
N1 N2 1.369(8) . ?
N2 N3 1.296(9) . ?
N3 N4 1.347(8) . ?
N4 C1 1.336(9) . ?
N4 C2 1.453(9) . ?
C1 H1 0.84(13) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mn1 N1 180.0 3_565 . ?
N1 Mn1 Cl1 88.54(14) 3_565 4_576 ?
N1 Mn1 Cl1 91.46(14) . 4_576 ?
N1 Mn1 Cl1 91.46(14) 3_565 2_544 ?
N1 Mn1 Cl1 88.54(14) . 2_544 ?
Cl1 Mn1 Cl1 180.0 4_576 2_544 ?
N1 Mn1 Cl1 90.89(14) 3_565 3_565 ?
N1 Mn1 Cl1 89.11(14) . 3_565 ?
Cl1 Mn1 Cl1 93.65(2) 4_576 3_565 ?
Cl1 Mn1 Cl1 86.35(2) 2_544 3_565 ?
N1 Mn1 Cl1 89.11(14) 3_565 . ?
N1 Mn1 Cl1 90.89(14) . . ?
Cl1 Mn1 Cl1 86.35(2) 4_576 . ?
Cl1 Mn1 Cl1 93.65(2) 2_544 . ?
Cl1 Mn1 Cl1 180.0 3_565 . ?
Mn1 Cl1 Mn1 142.32(7) 2_554 . ?
C1 N1 N2 106.0(5) . . ?
C1 N1 Mn1 123.8(4) . . ?
N2 N1 Mn1 129.8(4) . . ?
N3 N2 N1 110.1(6) . . ?
N2 N3 N4 106.7(6) . . ?
C1 N4 N3 108.4(6) . . ?
C1 N4 C2 130.1(6) . . ?
N3 N4 C2 121.5(6) . . ?
N1 C1 N4 108.9(6) . . ?
N1 C1 H1 133(8) . . ?
N4 C1 H1 118(8) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.1(9) . . . . ?
Mn1 N1 N2 N3 -172.2(5) . . . . ?
N1 N2 N3 N4 -1.7(9) . . . . ?
N2 N3 N4 C1 2.7(9) . . . . ?
N2 N3 N4 C2 -178.6(7) . . . . ?
N2 N1 C1 N4 1.6(7) . . . . ?
Mn1 N1 C1 N4 174.5(4) . . . . ?
N3 N4 C1 N1 -2.7(8) . . . . ?
C2 N4 C1 N1 178.8(7) . . . . ?

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         4.036
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.283

_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_mx179
_database_code_depnum_ccdc_archive 'CCDC 1566383'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sun Apr 16 11:27:16 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakis(1-methyltetrazolyl) bis(picrato) zinc(II)
;
_chemical_name_common            
'tetrakis(1-methyltetrazolyl) bis(picrato) zinc(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H20 N22 O14 Zn'
_chemical_formula_sum            'C20 H20 N22 O14 Zn'
_chemical_formula_weight         857.95

_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                   11.2981(6)
_cell_length_b                   8.9988(5)
_cell_length_c                   16.2583(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.512(6)
_cell_angle_gamma                90
_cell_volume                     1652.40(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2283
_cell_measurement_theta_min      4.3990
_cell_measurement_theta_max      27.1920

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.846
_shelx_estimated_absorpt_T_min   0.774
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97696
_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    1.724
_exptl_crystal_F_000             872
_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            12751
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.215
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_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             3228
_reflns_number_gt                2420
_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)+(0.0371P)²+0.4734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3228
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0933
_refine_ls_wR_factor_gt          0.0828
_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      -0.0512987000
_diffrn_orient_matrix_UB_12      0.0338508000
_diffrn_orient_matrix_UB_13      -0.0178394000
_diffrn_orient_matrix_UB_21      0.0293835000
_diffrn_orient_matrix_UB_22      0.0077677000
_diffrn_orient_matrix_UB_23      -0.0377568000
_diffrn_orient_matrix_UB_31      -0.0212617000
_diffrn_orient_matrix_UB_32      -0.0707779000
_diffrn_orient_matrix_UB_33      -0.0125933000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00   74.20   0.8000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 124

#__ type_ start__ end____ width___ exp.time_
  2 omega    5.00   97.00   0.8000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 115

#__ type_ start__ end____ width___ exp.time_
  3 omega    0.00   82.40   0.8000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 103

#__ type_ start__ end____ width___ exp.time_
  4 omega  -22.00   67.60   0.8000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 112

#__ type_ start__ end____ width___ exp.time_
  5 omega  -30.00   82.00   0.8000   52.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -90.0000 140

;



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'
Zn Zn 0.2839 1.4301 '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 0.5000 0.5000 0.0000 0.02364(14) Uani 1 2 d S . P . .
O1 O 0.32257(15) 0.42595(18) -0.03270(12) 0.0279(4) Uani 1 1 d . . . . .
O2 O 0.30894(19) -0.0158(2) -0.03171(14) 0.0442(5) Uani 1 1 d . . . . .
O3 O 0.32867(19) 0.1645(2) -0.11780(13) 0.0418(5) Uani 1 1 d . . . . .
O4 O 0.18639(17) 0.6715(2) -0.00638(14) 0.0425(6) Uani 1 1 d . . . . .
O5 O 0.1084(2) 0.6597(2) 0.11346(16) 0.0548(7) Uani 1 1 d . . . . .
O6 O -0.10174(19) 0.2195(3) 0.17686(15) 0.0556(7) Uani 1 1 d . . . . .
O7 O -0.0462(2) 0.0053(2) 0.12899(14) 0.0502(6) Uani 1 1 d . . . . .
N1 N 0.34824(18) 0.7785(2) 0.17843(14) 0.0265(5) Uani 1 1 d . . . . .
N2 N 0.3637(2) 0.6526(3) 0.22206(15) 0.0408(6) Uani 1 1 d . . . . .
N3 N 0.4173(2) 0.5595(3) 0.17561(15) 0.0368(6) Uani 1 1 d . . . . .
N4 N 0.43660(18) 0.6223(2) 0.10143(13) 0.0243(5) Uani 1 1 d . . . . .
N5 N 0.41216(18) 0.8055(2) -0.18845(14) 0.0276(5) Uani 1 1 d . . . . .
N6 N 0.5162(2) 0.8618(3) -0.16181(17) 0.0438(7) Uani 1 1 d . . . . .
N7 N 0.5489(2) 0.7873(3) -0.09717(16) 0.0390(6) Uani 1 1 d . . . . .
N8 N 0.46666(18) 0.6821(2) -0.08092(13) 0.0243(5) Uani 1 1 d . . . . .
N9 N 0.28983(19) 0.1126(2) -0.05454(15) 0.0295(5) Uani 1 1 d . . . . .
N10 N 0.1488(2) 0.6009(2) 0.05173(17) 0.0342(6) Uani 1 1 d . . . . .
N11 N -0.0382(2) 0.1413(3) 0.13389(16) 0.0400(6) Uani 1 1 d . . . . .
C1 C 0.3941(2) 0.7581(3) 0.10566(17) 0.0275(6) Uani 1 1 d . . . . .
H1 H 0.3961 0.8301 0.0630 0.033 Uiso 1 1 calc R U . . .
C2 C 0.2800(3) 0.9019(3) 0.2110(2) 0.0370(7) Uani 1 1 d . . . . .
H2A H 0.2034 0.8652 0.2294 0.055 Uiso 1 1 calc R U . . .
H2B H 0.2670 0.9767 0.1679 0.055 Uiso 1 1 calc R U . . .
H2C H 0.3237 0.9468 0.2576 0.055 Uiso 1 1 calc R U . . .
C3 C 0.3831(2) 0.6966(3) -0.13810(17) 0.0262(6) Uani 1 1 d . . . . .
H3 H 0.3131 0.6384 -0.1426 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3523(3) 0.8662(4) -0.2615(2) 0.0462(8) Uani 1 1 d . . . . .
H4A H 0.2692 0.8350 -0.2628 0.069 Uiso 1 1 calc R U . . .
H4B H 0.3910 0.8296 -0.3108 0.069 Uiso 1 1 calc R U . . .
H4C H 0.3566 0.9750 -0.2601 0.069 Uiso 1 1 calc R U . . .
C5 C 0.2351(2) 0.3629(3) -0.00071(16) 0.0225(6) Uani 1 1 d . . . . .
C6 C 0.1477(2) 0.4379(3) 0.04681(17) 0.0257(6) Uani 1 1 d . . . . .
C7 C 0.0618(2) 0.3679(3) 0.09078(17) 0.0295(6) Uani 1 1 d . . . . .
H7 H 0.0093 0.4238 0.1234 0.035 Uiso 1 1 calc R U . . .
C8 C 0.0530(2) 0.2155(3) 0.08671(17) 0.0301(6) Uani 1 1 d . . . . .
C9 C 0.1283(2) 0.1325(3) 0.03910(17) 0.0269(6) Uani 1 1 d . . . . .
H9 H 0.1211 0.0274 0.0366 0.032 Uiso 1 1 calc R U . . .
C10 C 0.2135(2) 0.2043(3) -0.00430(16) 0.0240(6) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N4 2.123(2) 3_665 ?
Zn1 N4 2.123(2) . ?
Zn1 N8 2.129(2) . ?
Zn1 N8 2.129(2) 3_665 ?
Zn1 O1 2.1654(17) . ?
Zn1 O1 2.1654(17) 3_665 ?
O1 C5 1.264(3) . ?
O2 N9 1.231(3) . ?
O3 N9 1.222(3) . ?
O4 N10 1.224(3) . ?
O5 N10 1.233(3) . ?
O6 N11 1.235(3) . ?
O7 N11 1.230(3) . ?
N1 C1 1.317(3) . ?
N1 N2 1.345(3) . ?
N1 C2 1.460(3) . ?
N2 N3 1.290(3) . ?
N3 N4 1.355(3) . ?
N4 C1 1.316(3) . ?
N5 C3 1.324(3) . ?
N5 N6 1.342(3) . ?
N5 C4 1.458(4) . ?
N6 N7 1.292(3) . ?
N7 N8 1.358(3) . ?
N8 C3 1.314(3) . ?
N9 C10 1.459(3) . ?
N10 C6 1.469(3) . ?
N11 C8 1.461(3) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.438(3) . ?
C5 C10 1.449(3) . ?
C6 C7 1.373(3) . ?
C7 C8 1.377(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(4) . ?
C9 C10 1.370(3) . ?
C9 H9 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Zn1 N4 180.0 3_665 . ?
N4 Zn1 N8 88.67(8) 3_665 . ?
N4 Zn1 N8 91.33(8) . . ?
N4 Zn1 N8 91.33(8) 3_665 3_665 ?
N4 Zn1 N8 88.67(8) . 3_665 ?
N8 Zn1 N8 180.0 . 3_665 ?
N4 Zn1 O1 88.79(7) 3_665 . ?
N4 Zn1 O1 91.21(7) . . ?
N8 Zn1 O1 86.42(7) . . ?
N8 Zn1 O1 93.58(7) 3_665 . ?
N4 Zn1 O1 91.21(7) 3_665 3_665 ?
N4 Zn1 O1 88.79(7) . 3_665 ?
N8 Zn1 O1 93.58(7) . 3_665 ?
N8 Zn1 O1 86.42(7) 3_665 3_665 ?
O1 Zn1 O1 180.0 . 3_665 ?
C5 O1 Zn1 140.03(18) . . ?
C1 N1 N2 108.0(2) . . ?
C1 N1 C2 131.0(2) . . ?
N2 N1 C2 120.8(2) . . ?
N3 N2 N1 107.1(2) . . ?
N2 N3 N4 109.8(2) . . ?
C1 N4 N3 105.9(2) . . ?
C1 N4 Zn1 130.80(18) . . ?
N3 N4 Zn1 122.72(16) . . ?
C3 N5 N6 108.0(2) . . ?
C3 N5 C4 131.6(2) . . ?
N6 N5 C4 120.3(2) . . ?
N7 N6 N5 107.2(2) . . ?
N6 N7 N8 109.7(2) . . ?
C3 N8 N7 106.0(2) . . ?
C3 N8 Zn1 128.76(16) . . ?
N7 N8 Zn1 123.11(17) . . ?
O3 N9 O2 123.3(2) . . ?
O3 N9 C10 119.1(2) . . ?
O2 N9 C10 117.6(2) . . ?
O4 N10 O5 123.3(2) . . ?
O4 N10 C6 118.6(2) . . ?
O5 N10 C6 118.1(2) . . ?
O7 N11 O6 124.1(2) . . ?
O7 N11 C8 118.2(3) . . ?
O6 N11 C8 117.7(2) . . ?
N4 C1 N1 109.2(2) . . ?
N4 C1 H1 125.4 . . ?
N1 C1 H1 125.4 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N8 C3 N5 109.0(2) . . ?
N8 C3 H3 125.5 . . ?
N5 C3 H3 125.5 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C5 C6 124.5(2) . . ?
O1 C5 C10 123.9(2) . . ?
C6 C5 C10 111.5(2) . . ?
C7 C6 C5 124.7(2) . . ?
C7 C6 N10 115.7(2) . . ?
C5 C6 N10 119.5(2) . . ?
C6 C7 C8 118.9(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C9 121.3(2) . . ?
C7 C8 N11 118.7(2) . . ?
C9 C8 N11 120.0(2) . . ?
C10 C9 C8 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C5 124.3(2) . . ?
C9 C10 N9 117.1(2) . . ?
C5 C10 N9 118.6(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 -0.2(3) . . . . ?
C2 N1 N2 N3 174.3(2) . . . . ?
N1 N2 N3 N4 -0.5(3) . . . . ?
N2 N3 N4 C1 1.0(3) . . . . ?
N2 N3 N4 Zn1 -171.00(18) . . . . ?
C3 N5 N6 N7 0.4(3) . . . . ?
C4 N5 N6 N7 -179.6(3) . . . . ?
N5 N6 N7 N8 -0.1(3) . . . . ?
N6 N7 N8 C3 -0.3(3) . . . . ?
N6 N7 N8 Zn1 164.46(19) . . . . ?
N3 N4 C1 N1 -1.2(3) . . . . ?
Zn1 N4 C1 N1 169.96(17) . . . . ?
N2 N1 C1 N4 0.9(3) . . . . ?
C2 N1 C1 N4 -172.8(2) . . . . ?
N7 N8 C3 N5 0.5(3) . . . . ?
Zn1 N8 C3 N5 -163.06(16) . . . . ?
N6 N5 C3 N8 -0.6(3) . . . . ?
C4 N5 C3 N8 179.4(3) . . . . ?
Zn1 O1 C5 C6 82.9(3) . . . . ?
Zn1 O1 C5 C10 -94.2(3) . . . . ?
O1 C5 C6 C7 -170.9(3) . . . . ?
C10 C5 C6 C7 6.5(4) . . . . ?
O1 C5 C6 N10 7.8(4) . . . . ?
C10 C5 C6 N10 -174.9(2) . . . . ?
O4 N10 C6 C7 -151.7(3) . . . . ?
O5 N10 C6 C7 26.2(4) . . . . ?
O4 N10 C6 C5 29.5(4) . . . . ?
O5 N10 C6 C5 -152.5(3) . . . . ?
C5 C6 C7 C8 -3.5(4) . . . . ?
N10 C6 C7 C8 177.8(2) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C6 C7 C8 N11 179.7(3) . . . . ?
O7 N11 C8 C7 179.1(3) . . . . ?
O6 N11 C8 C7 -1.5(4) . . . . ?
O7 N11 C8 C9 -0.9(4) . . . . ?
O6 N11 C8 C9 178.5(3) . . . . ?
C7 C8 C9 C10 0.3(4) . . . . ?
N11 C8 C9 C10 -179.7(3) . . . . ?
C8 C9 C10 C5 3.4(4) . . . . ?
C8 C9 C10 N9 -179.1(2) . . . . ?
O1 C5 C10 C9 170.9(3) . . . . ?
C6 C5 C10 C9 -6.4(4) . . . . ?
O1 C5 C10 N9 -6.5(4) . . . . ?
C6 C5 C10 N9 176.2(2) . . . . ?
O3 N9 C10 C9 148.8(3) . . . . ?
O2 N9 C10 C9 -29.2(4) . . . . ?
O3 N9 C10 C5 -33.6(4) . . . . ?
O2 N9 C10 C5 148.4(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         0.364
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.062

_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_mx334
_database_code_depnum_ccdc_archive 'CCDC 1566382'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jul 18 20:46:26 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) cobalt(II) perchlorate di(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) cobalt(II) perchlorate di(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Co N24, 2(Cl O4), 2(C2 H4 N4)'
_chemical_formula_sum            'C16 H32 Cl2 Co N32 O8'
_chemical_formula_weight         930.56

_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                   7.0040(3)
_cell_length_b                   11.2557(4)
_cell_length_c                   13.4811(5)
_cell_angle_alpha                111.269(4)
_cell_angle_beta                 101.299(4)
_cell_angle_gamma                94.311(3)
_cell_volume                     958.68(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    3499
_cell_measurement_theta_min      4.6150
_cell_measurement_theta_max      32.0500

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.143
_exptl_absorpt_coefficient_mu    0.674
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92186
_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    1.612
_exptl_crystal_F_000             477
_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            7437
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.486
_diffrn_reflns_theta_max         25.998
_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             3758
_reflns_number_gt                3287
_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)+(0.0415P)²+0.4508P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3758
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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      -0.0449853000
_diffrn_orient_matrix_UB_12      -0.0638071000
_diffrn_orient_matrix_UB_13      -0.0358429000
_diffrn_orient_matrix_UB_21      -0.0779965000
_diffrn_orient_matrix_UB_22      0.0054796000
_diffrn_orient_matrix_UB_23      0.0271396000
_diffrn_orient_matrix_UB_31      -0.0532776000
_diffrn_orient_matrix_UB_32      0.0243253000
_diffrn_orient_matrix_UB_33      -0.0369002000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00  105.20   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   19.0000    0.0000 186

#__ type_ start__ end____ width___ exp.time_
  2 omega    1.00   82.90   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   90.0000 117

#__ type_ start__ end____ width___ exp.time_
  3 omega    3.00   97.50   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 135

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00   74.40   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 142

#__ type_ start__ end____ width___ exp.time_
  5 omega  -79.00  -46.80   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   60.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega -106.00  -78.00   0.7000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   30.0000 40

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.5000 0.01684(12) Uani 1 2 d S . P . .
Cl1 Cl 0.81233(8) 0.72793(5) 0.99211(4) 0.02880(14) Uani 1 1 d . . . . .
N9 N 0.9404(2) 0.82898(16) 0.69917(14) 0.0221(4) Uani 1 1 d . . . . .
C5 C 0.8184(3) 0.72624(18) 0.68744(17) 0.0218(4) Uani 1 1 d . . . . .
H5 H 0.8029 0.6981 0.7442 0.026 Uiso 1 1 calc R U . . .
N3 N 0.3384(3) 0.66528(17) 0.69555(16) 0.0314(4) Uani 1 1 d . . . . .
N5 N 0.1597(2) 0.75624(16) 0.40412(14) 0.0205(4) Uani 1 1 d . . . . .
N13 N 0.4196(3) 0.90782(19) 1.19698(16) 0.0296(4) Uani 1 1 d . . . . .
N6 N 0.0803(3) 0.64227(17) 0.32305(16) 0.0319(4) Uani 1 1 d . . . . .
C7 C 0.4050(4) 0.7882(2) 1.19475(19) 0.0329(5) Uani 1 1 d . . . . .
H7 H 0.3404 0.7126 1.1330 0.039 Uiso 1 1 calc R U . . .
N1 N 0.3061(2) 0.55520(16) 0.79151(14) 0.0219(4) Uani 1 1 d . . . . .
N15 N 0.5625(3) 0.9160(2) 1.35313(17) 0.0398(5) Uani 1 1 d . . . . .
N12 N 0.7224(2) 0.66995(15) 0.58377(14) 0.0210(4) Uani 1 1 d . . . . .
N2 N 0.2846(3) 0.66897(18) 0.78316(16) 0.0329(4) Uani 1 1 d . . . . .
N10 N 0.9213(3) 0.83706(17) 0.60047(16) 0.0296(4) Uani 1 1 d . . . . .
N11 N 0.7905(3) 0.74103(17) 0.53136(15) 0.0274(4) Uani 1 1 d . . . . .
N16 N 0.4937(3) 0.79077(19) 1.29086(17) 0.0344(5) Uani 1 1 d . . . . .
N8 N 0.3103(2) 0.61340(16) 0.44190(13) 0.0201(4) Uani 1 1 d . . . . .
N4 N 0.3958(2) 0.54958(16) 0.64655(14) 0.0210(4) Uani 1 1 d . . . . .
C2 C 0.2612(4) 0.5264(2) 0.88254(18) 0.0328(5) Uani 1 1 d . . . . .
H2A H 0.2472 0.4330 0.8636 0.049 Uiso 1 1 calc R U . . .
H2B H 0.1378 0.5564 0.8968 0.049 Uiso 1 1 calc R U . . .
H2C H 0.3686 0.5705 0.9483 0.049 Uiso 1 1 calc R U . . .
N7 N 0.1708(3) 0.55623(17) 0.34583(16) 0.0320(4) Uani 1 1 d . . . . .
C4 C 0.0942(3) 0.8749(2) 0.4002(2) 0.0298(5) Uani 1 1 d . . . . .
H4A H 0.1050 0.8813 0.3309 0.045 Uiso 1 1 calc R U . . .
H4B H 0.1772 0.9494 0.4616 0.045 Uiso 1 1 calc R U . . .
H4C H -0.0434 0.8736 0.4056 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3746(3) 0.48379(19) 0.70806(16) 0.0208(4) Uani 1 1 d . . . . .
H1 H 0.4037 0.3991 0.6948 0.025 Uiso 1 1 calc R U . . .
C8 C 0.3600(4) 0.9553(3) 1.1101(3) 0.0506(7) Uani 1 1 d . . . . .
H8A H 0.3745 1.0497 1.1421 0.076 Uiso 1 1 calc R U . . .
H8B H 0.2219 0.9190 1.0719 0.076 Uiso 1 1 calc R U . . .
H8C H 0.4435 0.9290 1.0579 0.076 Uiso 1 1 calc R U . . .
C3 C 0.3007(3) 0.73760(19) 0.47586(17) 0.0219(4) Uani 1 1 d . . . . .
H3 H 0.3811 0.8029 0.5408 0.026 Uiso 1 1 calc R U . . .
C6 C 1.0811(3) 0.9230(2) 0.79606(19) 0.0313(5) Uani 1 1 d . . . . .
H6A H 1.0593 0.9110 0.8617 0.047 Uiso 1 1 calc R U . . .
H6B H 1.0625 1.0105 0.8020 0.047 Uiso 1 1 calc R U . . .
H6C H 1.2157 0.9106 0.7895 0.047 Uiso 1 1 calc R U . . .
N14 N 0.5185(3) 0.9873(2) 1.29853(18) 0.0407(5) Uani 1 1 d . . . . .
O2 O 0.7577(4) 0.6032(2) 0.9098(2) 0.0906(9) Uani 1 1 d . . . . .
O4 O 0.9873(5) 0.7333(3) 1.0696(3) 0.0646(10) Uani 0.870(6) 1 d . . P A 1
O3 O 0.6617(4) 0.7527(3) 1.0487(3) 0.0753(12) Uani 0.870(6) 1 d . . P A 1
O1 O 0.8484(6) 0.8263(4) 0.9519(2) 0.0859(14) Uani 0.870(6) 1 d . . P A 1
O1A O 0.944(3) 0.7584(19) 0.9368(15) 0.060(6) Uiso 0.130(6) 1 d . . P A 2
O4A O 0.900(3) 0.7583(15) 1.1006(13) 0.042(4) Uiso 0.130(6) 1 d . . P A 2
O3A O 0.648(2) 0.7932(17) 0.9988(16) 0.050(5) Uiso 0.130(6) 1 d . . P A 2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 2.1385(16) . ?
Co1 N4 2.1385(16) 2_666 ?
Co1 N8 2.1402(15) 2_666 ?
Co1 N8 2.1402(15) . ?
Co1 N12 2.1579(17) 2_666 ?
Co1 N12 2.1579(17) . ?
Cl1 O4A 1.373(16) . ?
Cl1 O1A 1.391(18) . ?
Cl1 O2 1.404(2) . ?
Cl1 O3 1.407(2) . ?
Cl1 O3A 1.409(16) . ?
Cl1 O1 1.425(3) . ?
Cl1 O4 1.428(2) . ?
N9 C5 1.326(3) . ?
N9 N10 1.348(2) . ?
N9 C6 1.460(3) . ?
C5 N12 1.316(3) . ?
C5 H5 0.9500 . ?
N3 N2 1.296(3) . ?
N3 N4 1.361(2) . ?
N5 C3 1.326(3) . ?
N5 N6 1.337(2) . ?
N5 C4 1.459(2) . ?
N13 C7 1.332(3) . ?
N13 N14 1.342(3) . ?
N13 C8 1.458(3) . ?
N6 N7 1.291(2) . ?
C7 N16 1.311(3) . ?
C7 H7 0.9500 . ?
N1 C1 1.325(3) . ?
N1 N2 1.342(2) . ?
N1 C2 1.461(3) . ?
N15 N14 1.287(3) . ?
N15 N16 1.344(3) . ?
N12 N11 1.361(2) . ?
N10 N11 1.289(3) . ?
N8 C3 1.315(3) . ?
N8 N7 1.361(2) . ?
N4 C1 1.317(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C1 H1 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C3 H3 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Co1 N4 180.0 . 2_666 ?
N4 Co1 N8 88.83(6) . 2_666 ?
N4 Co1 N8 91.17(6) 2_666 2_666 ?
N4 Co1 N8 91.18(6) . . ?
N4 Co1 N8 88.82(6) 2_666 . ?
N8 Co1 N8 180.0 2_666 . ?
N4 Co1 N12 92.00(6) . 2_666 ?
N4 Co1 N12 88.00(6) 2_666 2_666 ?
N8 Co1 N12 88.97(6) 2_666 2_666 ?
N8 Co1 N12 91.03(6) . 2_666 ?
N4 Co1 N12 88.00(6) . . ?
N4 Co1 N12 92.00(6) 2_666 . ?
N8 Co1 N12 91.03(6) 2_666 . ?
N8 Co1 N12 88.97(6) . . ?
N12 Co1 N12 180.0 2_666 . ?
O4A Cl1 O1A 111.8(11) . . ?
O4A Cl1 O2 126.1(7) . . ?
O1A Cl1 O2 89.9(8) . . ?
O2 Cl1 O3 107.98(17) . . ?
O4A Cl1 O3A 102.2(10) . . ?
O1A Cl1 O3A 117.2(11) . . ?
O2 Cl1 O3A 110.5(7) . . ?
O2 Cl1 O1 113.8(2) . . ?
O3 Cl1 O1 110.2(2) . . ?
O2 Cl1 O4 109.82(18) . . ?
O3 Cl1 O4 107.0(2) . . ?
O1 Cl1 O4 107.82(18) . . ?
C5 N9 N10 108.46(17) . . ?
C5 N9 C6 130.62(18) . . ?
N10 N9 C6 120.91(17) . . ?
N12 C5 N9 108.42(17) . . ?
N12 C5 H5 125.8 . . ?
N9 C5 H5 125.8 . . ?
N2 N3 N4 109.81(16) . . ?
C3 N5 N6 108.65(16) . . ?
C3 N5 C4 130.83(18) . . ?
N6 N5 C4 120.44(17) . . ?
C7 N13 N14 107.24(18) . . ?
C7 N13 C8 130.9(2) . . ?
N14 N13 C8 121.7(2) . . ?
N7 N6 N5 106.96(17) . . ?
N16 C7 N13 109.6(2) . . ?
N16 C7 H7 125.2 . . ?
N13 C7 H7 125.2 . . ?
C1 N1 N2 108.46(16) . . ?
C1 N1 C2 129.75(18) . . ?
N2 N1 C2 121.77(17) . . ?
N14 N15 N16 111.0(2) . . ?
C5 N12 N11 106.35(17) . . ?
C5 N12 Co1 130.97(13) . . ?
N11 N12 Co1 122.69(13) . . ?
N3 N2 N1 106.92(16) . . ?
N11 N10 N9 106.91(16) . . ?
N10 N11 N12 109.86(17) . . ?
C7 N16 N15 105.30(19) . . ?
C3 N8 N7 105.99(16) . . ?
C3 N8 Co1 134.00(14) . . ?
N7 N8 Co1 119.88(12) . . ?
C1 N4 N3 106.01(16) . . ?
C1 N4 Co1 130.72(13) . . ?
N3 N4 Co1 123.26(13) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N6 N7 N8 109.91(17) . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C1 N1 108.79(17) . . ?
N4 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
N13 C8 H8A 109.5 . . ?
N13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N8 C3 N5 108.50(18) . . ?
N8 C3 H3 125.8 . . ?
N5 C3 H3 125.8 . . ?
N9 C6 H6A 109.5 . . ?
N9 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N9 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N15 N14 N13 106.87(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 N9 C5 N12 -0.3(2) . . . . ?
C6 N9 C5 N12 -179.05(19) . . . . ?
C3 N5 N6 N7 0.4(2) . . . . ?
C4 N5 N6 N7 177.47(18) . . . . ?
N14 N13 C7 N16 -0.8(3) . . . . ?
C8 N13 C7 N16 174.7(2) . . . . ?
N9 C5 N12 N11 0.5(2) . . . . ?
N9 C5 N12 Co1 -179.75(12) . . . . ?
N4 N3 N2 N1 -0.2(2) . . . . ?
C1 N1 N2 N3 0.4(2) . . . . ?
C2 N1 N2 N3 179.1(2) . . . . ?
C5 N9 N10 N11 0.0(2) . . . . ?
C6 N9 N10 N11 178.90(18) . . . . ?
N9 N10 N11 N12 0.3(2) . . . . ?
C5 N12 N11 N10 -0.5(2) . . . . ?
Co1 N12 N11 N10 179.71(13) . . . . ?
N13 C7 N16 N15 0.5(3) . . . . ?
N14 N15 N16 C7 0.1(3) . . . . ?
N2 N3 N4 C1 0.0(2) . . . . ?
N2 N3 N4 Co1 -179.31(14) . . . . ?
N5 N6 N7 N8 -0.1(2) . . . . ?
C3 N8 N7 N6 -0.2(2) . . . . ?
Co1 N8 N7 N6 -176.56(14) . . . . ?
N3 N4 C1 N1 0.3(2) . . . . ?
Co1 N4 C1 N1 179.47(13) . . . . ?
N2 N1 C1 N4 -0.4(2) . . . . ?
C2 N1 C1 N4 -179.0(2) . . . . ?
N7 N8 C3 N5 0.5(2) . . . . ?
Co1 N8 C3 N5 176.08(13) . . . . ?
N6 N5 C3 N8 -0.6(2) . . . . ?
C4 N5 C3 N8 -177.21(19) . . . . ?
N16 N15 N14 N13 -0.6(3) . . . . ?
C7 N13 N14 N15 0.9(3) . . . . ?
C8 N13 N14 N15 -175.1(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
C5 H5 O1 0.95 2.58 3.284(4) 130.8 .
C2 H2C O3 0.98 2.55 3.420(4) 147.5 .
C4 H4B N15 0.98 2.63 3.566(3) 160.0 2_677
C1 H1 N16 0.95 2.37 3.295(3) 165.8 2_667
C8 H8A O1 0.98 2.61 3.229(4) 121.0 2_677
C8 H8B O4 0.98 2.55 3.291(4) 132.6 1_455
C8 H8C O3 0.98 2.58 3.223(4) 123.5 .
C3 H3 N14 0.95 2.49 3.393(3) 158.6 2_677
C6 H6A O1 0.98 2.43 3.315(4) 150.0 .
C5 H5 O1 0.95 2.58 3.284(4) 130.8 .
C2 H2C O3 0.98 2.55 3.420(4) 147.5 .
C4 H4B N15 0.98 2.63 3.566(3) 160.0 2_677
C1 H1 N16 0.95 2.37 3.295(3) 165.8 2_667
C8 H8A O1 0.98 2.61 3.229(4) 121.0 2_677
C8 H8B O4 0.98 2.55 3.291(4) 132.6 1_455
C8 H8C O3 0.98 2.58 3.223(4) 123.5 .
C3 H3 N14 0.95 2.49 3.393(3) 158.6 2_677
C6 H6A O1 0.98 2.43 3.315(4) 150.0 .

_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         0.582
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-4


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

data_mx128
_database_code_depnum_ccdc_archive 'CCDC 1566380'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Mar 17 17:57:07 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) iron(II) di-perchlorate bis(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) iron(II) di-perchlorate bis(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Fe N24, 2(C2 H4 N4), 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 Fe N32 O8'
_chemical_formula_weight         927.48

_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                   7.0337(4)
_cell_length_b                   11.3122(10)
_cell_length_c                   13.4921(9)
_cell_angle_alpha                111.433(7)
_cell_angle_beta                 101.254(5)
_cell_angle_gamma                94.220(6)
_cell_volume                     967.64(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2462
_cell_measurement_theta_min      4.6010
_cell_measurement_theta_max      30.6000

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.614
_shelx_estimated_absorpt_T_min   0.733
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92777
_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    1.592
_exptl_crystal_F_000             476
_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            7361
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.484
_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             3791
_reflns_number_gt                3162
_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)+(0.0575P)²+0.7388P] 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         3791
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.1095
_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      0.0011419000
_diffrn_orient_matrix_UB_12      0.0517057000
_diffrn_orient_matrix_UB_13      -0.0178430000
_diffrn_orient_matrix_UB_21      -0.0298709000
_diffrn_orient_matrix_UB_22      -0.0444352000
_diffrn_orient_matrix_UB_23      -0.0553309000
_diffrn_orient_matrix_UB_31      -0.0997575000
_diffrn_orient_matrix_UB_32      0.0025927000
_diffrn_orient_matrix_UB_33      0.0018393000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -2.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -90.0000 101

#__ type_ start__ end____ width___ exp.time_
  2 omega   25.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  120.0000 75

#__ type_ start__ end____ width___ exp.time_
  3 omega   61.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
  4 omega -104.00   28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994    0.0000  -60.0000 132

#__ type_ start__ end____ width___ exp.time_
  5 omega   22.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -130.0000   36.0000 71

#__ type_ start__ end____ width___ exp.time_
  6 omega -109.00  -64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   60.0000 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'
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 0.0000 0.0000 0.5000 0.02077(15) Uani 1 2 d S . P . .
N1 N 0.3423(3) -0.2574(2) 0.59652(17) 0.0249(4) Uani 1 1 d . . . . .
N2 N 0.4242(4) -0.1432(2) 0.6759(2) 0.0400(6) Uani 1 1 d . . . . .
N3 N 0.3360(4) -0.0582(2) 0.6521(2) 0.0400(6) Uani 1 1 d . . . . .
N4 N 0.1951(3) -0.1151(2) 0.55743(16) 0.0235(4) Uani 1 1 d . . . . .
N5 N 0.4436(3) 0.3294(2) 0.70104(17) 0.0261(5) Uani 1 1 d . . . . .
N6 N 0.4221(3) 0.3389(2) 0.60301(19) 0.0352(5) Uani 1 1 d . . . . .
N7 N 0.2917(3) 0.2434(2) 0.53376(19) 0.0346(5) Uani 1 1 d . . . . .
N8 N 0.2267(3) 0.17110(19) 0.58541(17) 0.0253(4) Uani 1 1 d . . . . .
N10 N -0.2154(4) 0.1683(2) 0.7868(2) 0.0392(6) Uani 1 1 d . . . . .
N9 N -0.1942(3) 0.0545(2) 0.79392(17) 0.0261(5) Uani 1 1 d . . . . .
C5 C -0.1276(4) -0.0160(3) 0.7100(2) 0.0247(5) Uani 1 1 d . . . . .
N12 N -0.1068(3) 0.0498(2) 0.64921(17) 0.0252(5) Uani 1 1 d . . . . .
C1 C 0.2025(4) -0.2385(3) 0.5251(2) 0.0273(5) Uani 1 1 d . . . . .
C2 C 0.4067(4) -0.3754(3) 0.6010(3) 0.0365(6) Uani 1 1 d . . . . .
H2A H 0.3215 -0.4499 0.5411 0.055 Uiso 1 1 calc R U . . .
H2B H 0.3993 -0.3797 0.6714 0.055 Uiso 1 1 calc R U . . .
H2C H 0.5424 -0.3760 0.5934 0.055 Uiso 1 1 calc R U . . .
C3 C 0.3237(4) 0.2265(2) 0.6886(2) 0.0261(5) Uani 1 1 d . . . . .
C4 C 0.5841(4) 0.4224(3) 0.7982(2) 0.0390(7) Uani 1 1 d . . . . .
H4A H 0.5657 0.4078 0.8633 0.058 Uiso 1 1 calc R U . . .
H4B H 0.5627 0.5098 0.8065 0.058 Uiso 1 1 calc R U . . .
H4C H 0.7180 0.4119 0.7902 0.058 Uiso 1 1 calc R U . . .
N11 N -0.1634(4) 0.1648(2) 0.6993(2) 0.0380(6) Uani 1 1 d . . . . .
C6 C -0.2385(4) 0.0253(3) 0.8845(2) 0.0379(7) Uani 1 1 d . . . . .
H6A H -0.2589 -0.0681 0.8636 0.057 Uiso 1 1 calc R U . . .
H6B H -0.3577 0.0590 0.9015 0.057 Uiso 1 1 calc R U . . .
H6C H -0.1286 0.0654 0.9491 0.057 Uiso 1 1 calc R U . . .
N13 N 0.9204(3) 0.4079(2) 0.1975(2) 0.0347(5) Uani 1 1 d . . . . .
C7 C 0.9048(4) 0.2892(3) 0.1953(2) 0.0389(7) Uani 1 1 d . . . . .
N16 N 0.9940(4) 0.2910(3) 0.2906(2) 0.0396(6) Uani 1 1 d . . . . .
N15 N 1.0637(4) 0.4154(3) 0.3531(2) 0.0478(7) Uani 1 1 d . . . . .
N14 N 1.0207(4) 0.4865(3) 0.2988(2) 0.0496(7) Uani 1 1 d . . . . .
C8 C 0.8605(5) 0.4549(4) 0.1104(3) 0.0596(10) Uani 1 1 d . . . . .
H8A H 0.9454 0.4303 0.0590 0.089 Uiso 1 1 calc R U . . .
H8B H 0.8720 0.5489 0.1425 0.089 Uiso 1 1 calc R U . . .
H8C H 0.7239 0.4172 0.0713 0.089 Uiso 1 1 calc R U . . .
Cl1 Cl 0.68776(9) 0.77054(7) 0.00788(5) 0.03338(18) Uani 1 1 d . . . . .
O1 O 0.8390(5) 0.7456(4) -0.0463(3) 0.1091(14) Uani 1 1 d . . . . .
O2 O 0.5188(5) 0.7634(3) -0.0710(3) 0.0936(11) Uani 1 1 d . . . . .
O3 O 0.6519(6) 0.6748(4) 0.0482(3) 0.1132(14) Uani 1 1 d . . . . .
O4 O 0.7409(4) 0.8944(3) 0.0911(3) 0.0960(12) Uani 1 1 d . . . . .
H3 H 0.315(4) 0.196(3) 0.740(2) 0.024(7) Uiso 1 1 d . . . . .
H1 H 0.125(5) -0.301(4) 0.468(3) 0.051(10) Uiso 1 1 d . . . . .
H5 H -0.105(4) -0.096(3) 0.695(2) 0.033(8) Uiso 1 1 d . . . . .
H7 H 0.837(5) 0.212(4) 0.141(3) 0.055(10) 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 N12 2.181(2) . ?
Fe1 N12 2.181(2) 2_556 ?
Fe1 N4 2.183(2) . ?
Fe1 N4 2.183(2) 2_556 ?
Fe1 N8 2.194(2) 2_556 ?
Fe1 N8 2.194(2) . ?
N1 C1 1.324(3) . ?
N1 N2 1.337(3) . ?
N1 C2 1.459(3) . ?
N2 N3 1.285(3) . ?
N3 N4 1.356(3) . ?
N4 C1 1.310(3) . ?
N5 C3 1.324(3) . ?
N5 N6 1.346(3) . ?
N5 C4 1.461(3) . ?
N6 N7 1.290(3) . ?
N7 N8 1.360(3) . ?
N8 C3 1.314(3) . ?
N10 N11 1.291(3) . ?
N10 N9 1.342(3) . ?
N9 C5 1.319(3) . ?
N9 C6 1.458(3) . ?
C5 N12 1.314(3) . ?
C5 H5 0.89(3) . ?
N12 N11 1.358(3) . ?
C1 H1 0.88(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.89(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N13 C7 1.328(4) . ?
N13 N14 1.342(3) . ?
N13 C8 1.463(4) . ?
C7 N16 1.309(4) . ?
C7 H7 0.93(4) . ?
N16 N15 1.342(4) . ?
N15 N14 1.286(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cl1 O1 1.393(3) . ?
Cl1 O4 1.405(3) . ?
Cl1 O3 1.406(3) . ?
Cl1 O2 1.407(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
N12 Fe1 N12 180.0 . 2_556 ?
N12 Fe1 N4 89.54(8) . . ?
N12 Fe1 N4 90.46(8) 2_556 . ?
N12 Fe1 N4 90.46(8) . 2_556 ?
N12 Fe1 N4 89.54(8) 2_556 2_556 ?
N4 Fe1 N4 180.0 . 2_556 ?
N12 Fe1 N8 91.62(8) . 2_556 ?
N12 Fe1 N8 88.38(8) 2_556 2_556 ?
N4 Fe1 N8 89.63(8) . 2_556 ?
N4 Fe1 N8 90.37(8) 2_556 2_556 ?
N12 Fe1 N8 88.38(8) . . ?
N12 Fe1 N8 91.62(8) 2_556 . ?
N4 Fe1 N8 90.37(8) . . ?
N4 Fe1 N8 89.63(8) 2_556 . ?
N8 Fe1 N8 180.0 2_556 . ?
C1 N1 N2 108.2(2) . . ?
C1 N1 C2 131.1(2) . . ?
N2 N1 C2 120.6(2) . . ?
N3 N2 N1 106.9(2) . . ?
N2 N3 N4 110.3(2) . . ?
C1 N4 N3 105.7(2) . . ?
C1 N4 Fe1 134.20(17) . . ?
N3 N4 Fe1 119.88(16) . . ?
C3 N5 N6 108.3(2) . . ?
C3 N5 C4 130.5(2) . . ?
N6 N5 C4 121.1(2) . . ?
N7 N6 N5 106.9(2) . . ?
N6 N7 N8 109.9(2) . . ?
C3 N8 N7 106.1(2) . . ?
C3 N8 Fe1 131.21(17) . . ?
N7 N8 Fe1 122.66(16) . . ?
N11 N10 N9 106.8(2) . . ?
C5 N9 N10 108.5(2) . . ?
C5 N9 C6 129.9(2) . . ?
N10 N9 C6 121.7(2) . . ?
N12 C5 N9 108.9(2) . . ?
N12 C5 H5 125.4(19) . . ?
N9 C5 H5 125.7(19) . . ?
C5 N12 N11 105.8(2) . . ?
C5 N12 Fe1 130.54(17) . . ?
N11 N12 Fe1 123.63(16) . . ?
N4 C1 N1 108.9(2) . . ?
N4 C1 H1 127(2) . . ?
N1 C1 H1 123(2) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N8 C3 N5 108.7(2) . . ?
N8 C3 H3 124.8(18) . . ?
N5 C3 H3 126.3(18) . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N10 N11 N12 110.0(2) . . ?
N9 C6 H6A 109.5 . . ?
N9 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N9 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N13 N14 107.0(2) . . ?
C7 N13 C8 130.8(3) . . ?
N14 N13 C8 122.0(3) . . ?
N16 C7 N13 109.9(3) . . ?
N16 C7 H7 119(2) . . ?
N13 C7 H7 131(2) . . ?
C7 N16 N15 105.2(3) . . ?
N14 N15 N16 111.0(2) . . ?
N15 N14 N13 107.0(2) . . ?
N13 C8 H8A 109.5 . . ?
N13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 Cl1 O4 108.1(2) . . ?
O1 Cl1 O3 109.8(3) . . ?
O4 Cl1 O3 112.8(2) . . ?
O1 Cl1 O2 106.7(3) . . ?
O4 Cl1 O2 111.1(2) . . ?
O3 Cl1 O2 108.2(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) . . . . ?
C2 N1 N2 N3 -178.3(2) . . . . ?
N1 N2 N3 N4 0.3(3) . . . . ?
N2 N3 N4 C1 -0.1(3) . . . . ?
N2 N3 N4 Fe1 174.86(19) . . . . ?
C3 N5 N6 N7 0.1(3) . . . . ?
C4 N5 N6 N7 179.0(2) . . . . ?
N5 N6 N7 N8 0.1(3) . . . . ?
N6 N7 N8 C3 -0.2(3) . . . . ?
N6 N7 N8 Fe1 179.02(17) . . . . ?
N11 N10 N9 C5 0.5(3) . . . . ?
N11 N10 N9 C6 179.4(2) . . . . ?
N10 N9 C5 N12 -0.3(3) . . . . ?
C6 N9 C5 N12 -179.1(2) . . . . ?
N9 C5 N12 N11 0.1(3) . . . . ?
N9 C5 N12 Fe1 178.77(16) . . . . ?
N3 N4 C1 N1 -0.1(3) . . . . ?
Fe1 N4 C1 N1 -174.03(16) . . . . ?
N2 N1 C1 N4 0.3(3) . . . . ?
C2 N1 C1 N4 178.0(2) . . . . ?
N7 N8 C3 N5 0.3(3) . . . . ?
Fe1 N8 C3 N5 -178.89(16) . . . . ?
N6 N5 C3 N8 -0.2(3) . . . . ?
C4 N5 C3 N8 -179.0(2) . . . . ?
N9 N10 N11 N12 -0.4(3) . . . . ?
C5 N12 N11 N10 0.2(3) . . . . ?
Fe1 N12 N11 N10 -178.58(18) . . . . ?
N14 N13 C7 N16 -1.0(3) . . . . ?
C8 N13 C7 N16 174.4(3) . . . . ?
N13 C7 N16 N15 0.9(3) . . . . ?
C7 N16 N15 N14 -0.4(3) . . . . ?
N16 N15 N14 N13 -0.2(3) . . . . ?
C7 N13 N14 N15 0.7(3) . . . . ?
C8 N13 N14 N15 -175.2(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
? ? ? ? ? ? ? ?

_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         0.631
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.067

_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_lx235
_database_code_depnum_ccdc_archive 'CCDC 1566368'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sun May 08 09:21:21 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl)iron(II) bis(tetrachloridoferrat(III))
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl)iron(II) bis(tetrachloridoferrat(III))'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Cl8 Fe3 N24'
_chemical_formula_weight         955.70

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

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_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                   12.5500(4)
_cell_length_b                   12.5500(4)
_cell_length_c                   6.6590(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     908.29(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3900
_cell_measurement_theta_min      4.8190
_cell_measurement_theta_max      32.3760

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.390
_exptl_absorpt_coefficient_mu    1.819
_shelx_estimated_absorpt_T_min   0.424
_shelx_estimated_absorpt_T_max   0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             478
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            6610
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.463
_diffrn_reflns_theta_max         25.991
_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             1196
_reflns_number_gt                1107
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0291P)²+0.5858P] 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         1196
_refine_ls_number_parameters     77
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0574
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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      0.0627269000
_diffrn_orient_matrix_UB_12      0.0158709000
_diffrn_orient_matrix_UB_13      -0.0030955000
_diffrn_orient_matrix_UB_21      -0.0179309000
_diffrn_orient_matrix_UB_22      -0.0627032000
_diffrn_orient_matrix_UB_23      -0.0154432000
_diffrn_orient_matrix_UB_31      0.0008196000
_diffrn_orient_matrix_UB_32      0.0087065000
_diffrn_orient_matrix_UB_33      -0.1053401000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -9.00   41.40   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  -60.0000 72

#__ type_ start__ end____ width___ exp.time_
  2 omega  -97.00  -16.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  150.0000 115

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00  100.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   30.0000 148

#__ type_ start__ end____ width___ exp.time_
  4 omega  -23.00    3.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega  -25.00   68.10   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 133

#__ type_ start__ end____ width___ exp.time_
  6 omega  -19.00   68.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 125

;



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'
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 0.0000 0.0000 0.5000 0.01092(14) Uani 1 6 d S T P . .
N1 N 0.10937(12) 0.14701(12) 0.32979(19) 0.0157(3) Uani 1 1 d . . . . .
N2 N 0.06789(13) 0.21441(13) 0.2318(2) 0.0209(3) Uani 1 1 d . . . . .
N3 N 0.15861(13) 0.30699(14) 0.1432(2) 0.0225(3) Uani 1 1 d . . . . .
N4 N 0.25991(13) 0.30040(12) 0.1836(2) 0.0173(3) Uani 1 1 d . . . . .
C1 C 0.22889(15) 0.20280(15) 0.2967(2) 0.0171(3) Uani 1 1 d . . . . .
C2 C 0.38058(16) 0.39285(16) 0.1081(3) 0.0238(4) Uani 1 1 d . . . . .
H2A H 0.4083 0.4705 0.1798 0.036 Uiso 1 1 calc R U . . .
H2B H 0.3748 0.4055 -0.0358 0.036 Uiso 1 1 calc R U . . .
H2C H 0.4397 0.3645 0.1297 0.036 Uiso 1 1 calc R U . . .
Fe2 Fe 0.3333 0.6667 0.48315(6) 0.01960(13) Uani 1 3 d S T P . .
Cl1 Cl 0.32324(4) 0.49640(4) 0.59349(7) 0.02763(13) Uani 1 1 d . . . . .
Cl2 Cl 0.3333 0.6667 0.15502(11) 0.03099(19) Uani 1 3 d S T P . .
H1 H 0.283(2) 0.179(2) 0.341(3) 0.027(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
Fe1 N1 2.0100(14) . ?
Fe1 N1 2.0101(14) 5_556 ?
Fe1 N1 2.0101(14) 2 ?
Fe1 N1 2.0101(14) 6_556 ?
Fe1 N1 2.0101(14) 3 ?
Fe1 N1 2.0101(14) 4_556 ?
N1 C1 1.318(2) . ?
N1 N2 1.3611(19) . ?
N2 N3 1.293(2) . ?
N3 N4 1.342(2) . ?
N4 C1 1.320(2) . ?
N4 C2 1.461(2) . ?
C1 H1 0.91(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
Fe2 Cl2 2.1850(9) . ?
Fe2 Cl1 2.2026(5) 3_565 ?
Fe2 Cl1 2.2026(5) 2_665 ?
Fe2 Cl1 2.2026(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 88.68(5) . 5_556 ?
N1 Fe1 N1 91.32(5) . 2 ?
N1 Fe1 N1 180.00(5) 5_556 2 ?
N1 Fe1 N1 88.68(5) . 6_556 ?
N1 Fe1 N1 91.32(5) 5_556 6_556 ?
N1 Fe1 N1 88.68(5) 2 6_556 ?
N1 Fe1 N1 91.32(5) . 3 ?
N1 Fe1 N1 88.68(5) 5_556 3 ?
N1 Fe1 N1 91.32(5) 2 3 ?
N1 Fe1 N1 180.0 6_556 3 ?
N1 Fe1 N1 180.0 . 4_556 ?
N1 Fe1 N1 91.32(5) 5_556 4_556 ?
N1 Fe1 N1 88.68(5) 2 4_556 ?
N1 Fe1 N1 91.32(5) 6_556 4_556 ?
N1 Fe1 N1 88.68(5) 3 4_556 ?
C1 N1 N2 106.08(13) . . ?
C1 N1 Fe1 130.93(11) . . ?
N2 N1 Fe1 122.88(10) . . ?
N3 N2 N1 109.79(13) . . ?
N2 N3 N4 106.80(13) . . ?
C1 N4 N3 108.82(14) . . ?
C1 N4 C2 129.85(15) . . ?
N3 N4 C2 121.33(14) . . ?
N1 C1 N4 108.51(14) . . ?
N1 C1 H1 127.3(13) . . ?
N4 C1 H1 124.2(13) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Cl2 Fe2 Cl1 109.486(16) . 3_565 ?
Cl2 Fe2 Cl1 109.486(16) . 2_665 ?
Cl1 Fe2 Cl1 109.456(16) 3_565 2_665 ?
Cl2 Fe2 Cl1 109.487(16) . . ?
Cl1 Fe2 Cl1 109.456(16) 3_565 . ?
Cl1 Fe2 Cl1 109.456(16) 2_665 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.02(18) . . . . ?
Fe1 N1 N2 N3 176.52(11) . . . . ?
N1 N2 N3 N4 -0.12(18) . . . . ?
N2 N3 N4 C1 0.17(18) . . . . ?
N2 N3 N4 C2 -179.13(14) . . . . ?
N2 N1 C1 N4 0.08(17) . . . . ?
Fe1 N1 C1 N4 -176.03(10) . . . . ?
N3 N4 C1 N1 -0.16(18) . . . . ?
C2 N4 C1 N1 179.06(15) . . . . ?

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         0.307
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.054

_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_lx237
_database_code_depnum_ccdc_archive 'CCDC 1566374'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue May 10 15:39:33 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakisaqua di(1-methyl-5H-tetrazolyl) nickel(II)
 trinitroresorcinate monohydrate
;
_chemical_name_common            
;
tetrakisaqua di(1-methyl-5H-tetrazolyl) nickel(II)
 trinitroresorcinate monohydrate
;
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 N8 Ni O4, 2(C6 H2 N3 O8), 2(H2 O)'
_chemical_formula_sum            'C16 H24 N14 Ni O22'
_chemical_formula_weight         823.20

_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                   15.2670(4)
_cell_length_b                   5.88500(10)
_cell_length_c                   18.4360(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.712(3)
_cell_angle_gamma                90
_cell_volume                     1516.57(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7118
_cell_measurement_theta_min      4.8210
_cell_measurement_theta_max      32.2240

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.470
_exptl_crystal_size_min          0.380
_exptl_absorpt_coefficient_mu    0.759
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92699
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            11713
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.221
_diffrn_reflns_theta_max         25.989
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2963
_reflns_number_gt                2744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+0.8113P] 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         2963
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0601
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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      -0.0261382000
_diffrn_orient_matrix_UB_12      0.0839194000
_diffrn_orient_matrix_UB_13      0.0105000000
_diffrn_orient_matrix_UB_21      -0.0400191000
_diffrn_orient_matrix_UB_22      -0.0739969000
_diffrn_orient_matrix_UB_23      -0.0116628000
_diffrn_orient_matrix_UB_31      0.0171030000
_diffrn_orient_matrix_UB_32      -0.0446843000
_diffrn_orient_matrix_UB_33      0.0389903000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   28.00   99.40   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000    0.0000 102

#__ type_ start__ end____ width___ exp.time_
  2 omega    6.00  101.20   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 136

#__ type_ start__ end____ width___ exp.time_
  3 omega   32.00   69.80   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 54

#__ type_ start__ end____ width___ exp.time_
  4 omega  -18.00   74.40   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 132

#__ type_ start__ end____ width___ exp.time_
  5 omega  -42.00  -15.40   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   38.0000  -30.0000 38

#__ type_ start__ end____ width___ exp.time_
  6 omega  -39.00   26.10   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000 -150.0000 93

#__ type_ start__ end____ width___ exp.time_
  7 omega -101.00    4.00   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  150.0000 150

;



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'
Ni Ni 0.3393 1.1124 '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
Ni1 Ni 0.5000 0.0000 0.0000 0.01168(8) Uani 1 2 d S . P . .
O1 O 0.60592(8) -0.1919(2) 0.08011(7) 0.0217(2) Uani 1 1 d . . . . .
O2 O 0.59428(7) 0.27333(17) 0.02652(6) 0.0156(2) Uani 1 1 d . . . . .
N1 N 0.44939(8) 0.0987(2) 0.08376(7) 0.0147(2) Uani 1 1 d . . . . .
N2 N 0.45514(9) -0.0330(2) 0.14569(7) 0.0195(3) Uani 1 1 d . . . . .
N3 N 0.41719(9) 0.0729(2) 0.18741(7) 0.0208(3) Uani 1 1 d . . . . .
N4 N 0.38671(8) 0.2757(2) 0.15282(7) 0.0161(2) Uani 1 1 d . . . . .
C1 C 0.40667(10) 0.2885(2) 0.08925(8) 0.0158(3) Uani 1 1 d . . . . .
C2 C 0.33660(11) 0.4370(3) 0.18337(9) 0.0212(3) Uani 1 1 d . . . . .
H2A H 0.3477 0.5921 0.1697 0.032 Uiso 1 1 calc R U . . .
H2B H 0.3608 0.4224 0.2411 0.032 Uiso 1 1 calc R U . . .
H2C H 0.2679 0.4043 0.1598 0.032 Uiso 1 1 calc R U . . .
O4 O 0.23376(8) 0.8804(2) 0.50716(7) 0.0346(3) Uani 1 1 d . . . . .
O5 O 0.10276(8) 0.9446(2) 0.52027(8) 0.0338(3) Uani 1 1 d . . . . .
O6 O 0.24759(7) 0.51602(18) 0.42800(7) 0.0226(2) Uani 1 1 d . . . . .
O7 O 0.18453(7) 0.27823(18) 0.27910(6) 0.0230(2) Uani 1 1 d . . . . .
O8 O 0.15760(10) -0.02011(18) 0.33448(8) 0.0326(3) Uani 1 1 d . . . . .
O9 O -0.03404(8) 0.11207(19) 0.29202(6) 0.0236(2) Uani 1 1 d . . . . .
O10 O -0.18572(7) 0.26068(19) 0.30448(6) 0.0232(2) Uani 1 1 d . . . . .
O11 O -0.17934(7) 0.53923(19) 0.38333(7) 0.0239(2) Uani 1 1 d . . . . .
N5 N 0.15176(8) 0.1839(2) 0.32218(7) 0.0176(3) Uani 1 1 d . . . . .
N6 N 0.15001(8) 0.8358(2) 0.49215(7) 0.0185(3) Uani 1 1 d . . . . .
N7 N -0.14000(8) 0.4131(2) 0.35269(7) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.10325(10) 0.3253(2) 0.35986(8) 0.0156(3) Uani 1 1 d . . . . .
C4 C 0.15940(10) 0.5005(2) 0.41096(8) 0.0156(3) Uani 1 1 d . . . . .
C5 C 0.10480(9) 0.6464(2) 0.44029(8) 0.0158(3) Uani 1 1 d . . . . .
C6 C 0.00866(10) 0.6148(2) 0.42041(8) 0.0159(3) Uani 1 1 d . . . . .
C7 C -0.04032(10) 0.4372(3) 0.37143(8) 0.0160(3) Uani 1 1 d . . . . .
C8 C 0.00731(10) 0.2847(2) 0.33990(8) 0.0162(3) Uani 1 1 d . . . . .
O3 O 0.36770(8) 0.9419(2) 0.31842(6) 0.0207(2) Uani 1 1 d . . . . .
H1 H 0.3944(11) 0.408(3) 0.0569(10) 0.016(4) Uiso 1 1 d . . . . .
H6 H -0.0233(12) 0.719(3) 0.4406(10) 0.022(4) Uiso 1 1 d . . . . .
H12 H 0.6590(17) -0.146(4) 0.0884(13) 0.043(6) Uiso 1 1 d . . . . .
H11 H 0.6052(15) -0.281(4) 0.1129(13) 0.039(6) Uiso 1 1 d . . . . .
H22 H 0.5983(13) 0.324(3) 0.0698(12) 0.032(5) Uiso 1 1 d . . . . .
H21 H 0.6480(16) 0.231(4) 0.0336(12) 0.039(6) Uiso 1 1 d . . . . .
H3B H 0.3870(17) 0.964(4) 0.2840(14) 0.044(6) Uiso 1 1 d . . . . .
H9 H -0.0922(17) 0.116(4) 0.2844(13) 0.050(7) Uiso 1 1 d . . . . .
H3A H 0.3105(17) 0.910(4) 0.2934(13) 0.041(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
Ni1 O1 2.0374(10) 3_655 ?
Ni1 O1 2.0375(10) . ?
Ni1 N1 2.0684(11) 3_655 ?
Ni1 N1 2.0685(11) . ?
Ni1 O2 2.0814(10) 3_655 ?
Ni1 O2 2.0814(10) . ?
O1 H12 0.81(2) . ?
O1 H11 0.80(2) . ?
O2 H22 0.83(2) . ?
O2 H21 0.82(2) . ?
N1 C1 1.3176(18) . ?
N1 N2 1.3535(17) . ?
N2 N3 1.2940(18) . ?
N3 N4 1.3449(17) . ?
N4 C1 1.3263(18) . ?
N4 C2 1.4663(18) . ?
C1 H1 0.893(18) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O4 N6 1.2231(16) . ?
O5 N6 1.2246(16) . ?
O6 C4 1.2569(18) . ?
O7 N5 1.2284(16) . ?
O8 N5 1.2184(16) . ?
O9 C8 1.3270(18) . ?
O9 H9 0.84(2) . ?
O10 N7 1.2579(16) . ?
O11 N7 1.2264(17) . ?
N5 C3 1.4621(18) . ?
N6 C5 1.4502(18) . ?
N7 C7 1.4256(18) . ?
C3 C8 1.3801(19) . ?
C3 C4 1.427(2) . ?
C4 C5 1.444(2) . ?
C5 C6 1.3749(19) . ?
C6 C7 1.387(2) . ?
C6 H6 0.949(18) . ?
C7 C8 1.419(2) . ?
O3 H3B 0.81(2) . ?
O3 H3A 0.83(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 Ni1 O1 180.0 3_655 . ?
O1 Ni1 N1 92.32(5) 3_655 3_655 ?
O1 Ni1 N1 87.68(5) . 3_655 ?
O1 Ni1 N1 87.68(5) 3_655 . ?
O1 Ni1 N1 92.32(5) . . ?
N1 Ni1 N1 180.00(6) 3_655 . ?
O1 Ni1 O2 89.19(4) 3_655 3_655 ?
O1 Ni1 O2 90.81(4) . 3_655 ?
N1 Ni1 O2 92.18(4) 3_655 3_655 ?
N1 Ni1 O2 87.82(4) . 3_655 ?
O1 Ni1 O2 90.81(4) 3_655 . ?
O1 Ni1 O2 89.19(4) . . ?
N1 Ni1 O2 87.81(4) 3_655 . ?
N1 Ni1 O2 92.19(4) . . ?
O2 Ni1 O2 180.0 3_655 . ?
Ni1 O1 H12 113.2(16) . . ?
Ni1 O1 H11 131.3(15) . . ?
H12 O1 H11 113(2) . . ?
Ni1 O2 H22 106.4(13) . . ?
Ni1 O2 H21 111.0(15) . . ?
H22 O2 H21 106(2) . . ?
C1 N1 N2 106.67(11) . . ?
C1 N1 Ni1 129.83(10) . . ?
N2 N1 Ni1 123.49(9) . . ?
N3 N2 N1 109.44(12) . . ?
N2 N3 N4 107.33(11) . . ?
C1 N4 N3 108.11(11) . . ?
C1 N4 C2 130.04(13) . . ?
N3 N4 C2 121.78(12) . . ?
N1 C1 N4 108.45(13) . . ?
N1 C1 H1 126.5(11) . . ?
N4 C1 H1 125.0(11) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 O9 H9 106.0(17) . . ?
O8 N5 O7 123.18(13) . . ?
O8 N5 C3 119.06(12) . . ?
O7 N5 C3 117.76(12) . . ?
O4 N6 O5 122.16(13) . . ?
O4 N6 C5 119.43(12) . . ?
O5 N6 C5 118.41(12) . . ?
O11 N7 O10 121.44(12) . . ?
O11 N7 C7 120.06(12) . . ?
O10 N7 C7 118.50(12) . . ?
C8 C3 C4 126.36(13) . . ?
C8 C3 N5 117.42(12) . . ?
C4 C3 N5 116.14(12) . . ?
O6 C4 C3 121.08(13) . . ?
O6 C4 C5 125.78(13) . . ?
C3 C4 C5 113.12(12) . . ?
C6 C5 C4 122.34(13) . . ?
C6 C5 N6 116.97(12) . . ?
C4 C5 N6 120.69(12) . . ?
C5 C6 C7 120.89(13) . . ?
C5 C6 H6 118.1(10) . . ?
C7 C6 H6 121.0(10) . . ?
C6 C7 C8 120.84(13) . . ?
C6 C7 N7 118.45(13) . . ?
C8 C7 N7 120.71(13) . . ?
O9 C8 C3 118.70(13) . . ?
O9 C8 C7 124.87(13) . . ?
C3 C8 C7 116.42(13) . . ?
H3B O3 H3A 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 0.01(16) . . . . ?
Ni1 N1 N2 N3 -179.60(9) . . . . ?
N1 N2 N3 N4 -0.23(16) . . . . ?
N2 N3 N4 C1 0.37(15) . . . . ?
N2 N3 N4 C2 177.72(12) . . . . ?
N2 N1 C1 N4 0.22(15) . . . . ?
Ni1 N1 C1 N4 179.79(9) . . . . ?
N3 N4 C1 N1 -0.37(15) . . . . ?
C2 N4 C1 N1 -177.42(13) . . . . ?
O8 N5 C3 C8 -62.80(18) . . . . ?
O7 N5 C3 C8 116.96(14) . . . . ?
O8 N5 C3 C4 120.27(15) . . . . ?
O7 N5 C3 C4 -59.98(16) . . . . ?
C8 C3 C4 O6 176.75(14) . . . . ?
N5 C3 C4 O6 -6.6(2) . . . . ?
C8 C3 C4 C5 -2.0(2) . . . . ?
N5 C3 C4 C5 174.63(12) . . . . ?
O6 C4 C5 C6 -178.30(14) . . . . ?
C3 C4 C5 C6 0.4(2) . . . . ?
O6 C4 C5 N6 2.2(2) . . . . ?
C3 C4 C5 N6 -179.09(12) . . . . ?
O4 N6 C5 C6 -175.00(14) . . . . ?
O5 N6 C5 C6 5.8(2) . . . . ?
O4 N6 C5 C4 4.5(2) . . . . ?
O5 N6 C5 C4 -174.66(13) . . . . ?
C4 C5 C6 C7 0.8(2) . . . . ?
N6 C5 C6 C7 -179.67(12) . . . . ?
C5 C6 C7 C8 -0.6(2) . . . . ?
C5 C6 C7 N7 -179.87(13) . . . . ?
O11 N7 C7 C6 -4.3(2) . . . . ?
O10 N7 C7 C6 175.74(12) . . . . ?
O11 N7 C7 C8 176.49(13) . . . . ?
O10 N7 C7 C8 -3.5(2) . . . . ?
C4 C3 C8 O9 -179.23(13) . . . . ?
N5 C3 C8 O9 4.18(19) . . . . ?
C4 C3 C8 C7 2.2(2) . . . . ?
N5 C3 C8 C7 -174.36(12) . . . . ?
C6 C7 C8 O9 -179.24(13) . . . . ?
N7 C7 C8 O9 0.0(2) . . . . ?
C6 C7 C8 C3 -0.8(2) . . . . ?
N7 C7 C8 C3 178.42(12) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H12 O6 0.81(2) 1.84(2) 2.6060(15) 158(2) 2_645
O1 H11 O3 0.80(2) 2.00(2) 2.7745(16) 161(2) 2_635
O2 H22 O3 0.83(2) 2.03(2) 2.8564(15) 170.4(18) 2_645
O2 H21 O6 0.82(2) 1.93(2) 2.6826(15) 152(2) 2_645
O2 H21 O4 0.82(2) 2.38(2) 2.9977(15) 132.6(19) 2_645
O3 H3B N3 0.81(2) 2.11(3) 2.9097(17) 169(2) 1_565
O9 H9 O10 0.84(2) 1.82(2) 2.5705(15) 147(2) .
O9 H9 N7 0.84(2) 2.43(2) 2.9087(17) 117(2) .
O9 H9 O7 0.84(2) 2.45(2) 2.9043(15) 115(2) 2_545
O3 H3A O10 0.83(2) 2.21(2) 2.9879(16) 156(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         0.293
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.044

_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_mx337
_database_code_depnum_ccdc_archive 'CCDC 1566385'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Jul 20 16:09:40 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) nickel(II) perchlorate di(1-methyltetrazole)
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) nickel(II) perchlorate di(1-methyltetrazole)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C12 H24 N24 Ni, 2(C2 H4 N4), 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 N32 Ni O8'
_chemical_formula_weight         930.34

_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                   7.0227(6)
_cell_length_b                   11.1679(11)
_cell_length_c                   13.4907(13)
_cell_angle_alpha                111.317(9)
_cell_angle_beta                 101.502(8)
_cell_angle_gamma                94.379(7)
_cell_volume                     952.95(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    1437
_cell_measurement_theta_min      4.5070
_cell_measurement_theta_max      25.9740

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.077
_exptl_absorpt_coefficient_mu    0.736
_shelx_estimated_absorpt_T_min   0.849
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98129
_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    1.621
_exptl_crystal_F_000             478
_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            7547
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.504
_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             3741
_reflns_number_gt                2667
_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)+(0.0522P)²+1.1069P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3741
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1254
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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      -0.0184662000
_diffrn_orient_matrix_UB_12      0.0620674000
_diffrn_orient_matrix_UB_13      0.0013515000
_diffrn_orient_matrix_UB_21      0.0190824000
_diffrn_orient_matrix_UB_22      -0.0157560000
_diffrn_orient_matrix_UB_23      -0.0525943000
_diffrn_orient_matrix_UB_31      -0.1010368000
_diffrn_orient_matrix_UB_32      -0.0259690000
_diffrn_orient_matrix_UB_33      -0.0248978000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -92.00   -5.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  120.0000 87

#__ type_ start__ end____ width___ exp.time_
  2 omega  -57.00   36.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   38.0000  -90.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega  -32.00    2.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -88.0000 -146.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega  -16.00   44.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   38.0000 -180.0000 60

#__ type_ start__ end____ width___ exp.time_
  5 omega   53.00   82.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   74.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
  7 omega   35.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000   30.0000 71

;



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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'


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
Ni Ni 0.5000 0.5000 0.5000 0.0176(2) Uani 1 2 d S . P . .
N1 N 0.1626(5) 0.7549(3) 0.4053(3) 0.0214(7) Uani 1 1 d . . . . .
N2 N 0.0842(5) 0.6399(4) 0.3230(3) 0.0333(9) Uani 1 1 d . . . . .
N3 N 0.1733(5) 0.5530(4) 0.3458(3) 0.0319(9) Uani 1 1 d . . . . .
N4 N 0.3121(5) 0.6106(3) 0.4416(3) 0.0197(7) Uani 1 1 d . . . . .
N5 N 0.0657(5) 0.1711(3) 0.3022(3) 0.0237(8) Uani 1 1 d . . . . .
N6 N 0.0796(5) 0.1647(4) 0.4011(3) 0.0304(9) Uani 1 1 d . . . . .
N7 N 0.2115(5) 0.2626(3) 0.4705(3) 0.0279(8) Uani 1 1 d . . . . .
N8 N 0.2822(5) 0.3329(3) 0.4184(3) 0.0206(7) Uani 1 1 d . . . . .
N9 N 0.6942(5) 0.4435(3) 0.2119(3) 0.0227(8) Uani 1 1 d . . . . .
N10 N 0.7188(6) 0.3301(4) 0.2225(3) 0.0341(9) Uani 1 1 d . . . . .
N11 N 0.6661(6) 0.3348(4) 0.3100(3) 0.0319(9) Uani 1 1 d . . . . .
N12 N 0.6048(5) 0.4506(3) 0.3576(3) 0.0210(7) Uani 1 1 d . . . . .
C1 C 0.3013(6) 0.7358(4) 0.4766(3) 0.0224(9) Uani 1 1 d . . . . .
H1 H 0.3806 0.8013 0.5424 0.027 Uiso 1 1 calc R U . . .
C2 C 0.0967(7) 0.8738(4) 0.4013(4) 0.0308(10) Uani 1 1 d . . . . .
H2A H 0.1758 0.9490 0.4645 0.046 Uiso 1 1 calc R U . . .
H2B H -0.0423 0.8704 0.4034 0.046 Uiso 1 1 calc R U . . .
H2C H 0.1121 0.8820 0.3333 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1882(6) 0.2741(4) 0.3140(3) 0.0228(9) Uani 1 1 d . . . . .
H3 H 0.2056 0.3012 0.2569 0.027 Uiso 1 1 calc R U . . .
C4 C -0.0741(7) 0.0752(4) 0.2043(4) 0.0331(11) Uani 1 1 d . . . . .
H4A H -0.0544 0.0890 0.1391 0.050 Uiso 1 1 calc R U . . .
H4B H -0.2089 0.0853 0.2110 0.050 Uiso 1 1 calc R U . . .
H4C H -0.0524 -0.0128 0.1974 0.050 Uiso 1 1 calc R U . . .
C5 C 0.6238(6) 0.5157(4) 0.2945(3) 0.0203(8) Uani 1 1 d . . . . .
H5 H 0.5923 0.6003 0.3063 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7368(7) 0.4710(5) 0.1202(3) 0.0324(11) Uani 1 1 d . . . . .
H6A H 0.7476 0.5649 0.1377 0.049 Uiso 1 1 calc R U . . .
H6B H 0.6302 0.4242 0.0543 0.049 Uiso 1 1 calc R U . . .
H6C H 0.8612 0.4425 0.1069 0.049 Uiso 1 1 calc R U . . .
N13 N 0.4202(5) 0.9056(4) 0.1943(3) 0.0304(9) Uani 1 1 d . . . . .
N14 N 0.5191(6) 0.9874(4) 0.2957(4) 0.0436(11) Uani 1 1 d . . . . .
N15 N 0.5607(6) 0.9157(4) 0.3514(3) 0.0411(10) Uani 1 1 d . . . . .
N16 N 0.4921(6) 0.7895(4) 0.2894(3) 0.0349(9) Uani 1 1 d . . . . .
C7 C 0.4053(7) 0.7858(5) 0.1928(4) 0.0350(11) Uani 1 1 d . . . . .
H7 H 0.3414 0.7091 0.1311 0.042 Uiso 1 1 calc R U . . .
C8 C 0.3617(8) 0.9519(6) 0.1058(5) 0.0545(16) Uani 1 1 d . . . . .
H8A H 0.4445 0.9237 0.0538 0.082 Uiso 1 1 calc R U . . .
H8B H 0.3781 1.0473 0.1368 0.082 Uiso 1 1 calc R U . . .
H8C H 0.2234 0.9159 0.0677 0.082 Uiso 1 1 calc R U . . .
Cl1 Cl 0.18793(15) 0.27647(11) 0.00870(9) 0.0307(3) Uani 1 1 d . . . . .
O4 O 0.1469(11) 0.1843(7) 0.0522(5) 0.137(3) Uani 1 1 d . . . . .
O1 O 0.0169(7) 0.2670(5) -0.0710(4) 0.0983(19) Uani 1 1 d . . . . .
O2 O 0.2445(6) 0.4048(5) 0.0859(4) 0.0946(19) Uani 1 1 d . . . . .
O3 O 0.3317(8) 0.2447(5) -0.0489(5) 0.116(2) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N12 2.096(3) . ?
Ni N12 2.096(3) 2_666 ?
Ni N4 2.104(3) 2_666 ?
Ni N4 2.105(3) . ?
Ni N8 2.105(3) 2_666 ?
Ni N8 2.105(3) . ?
N1 C1 1.314(5) . ?
N1 N2 1.340(5) . ?
N1 C2 1.455(5) . ?
N2 N3 1.287(5) . ?
N3 N4 1.354(5) . ?
N4 C1 1.316(5) . ?
N5 C3 1.322(5) . ?
N5 N6 1.347(5) . ?
N5 C4 1.466(5) . ?
N6 N7 1.299(5) . ?
N7 N8 1.356(4) . ?
N8 C3 1.319(5) . ?
N9 C5 1.328(5) . ?
N9 N10 1.345(5) . ?
N9 C6 1.458(5) . ?
N10 N11 1.289(5) . ?
N11 N12 1.365(5) . ?
N12 C5 1.323(5) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N13 C7 1.327(6) . ?
N13 N14 1.344(5) . ?
N13 C8 1.465(6) . ?
N14 N15 1.295(5) . ?
N15 N16 1.340(5) . ?
N16 C7 1.308(6) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cl1 O3 1.384(5) . ?
Cl1 O4 1.396(5) . ?
Cl1 O2 1.400(4) . ?
Cl1 O1 1.412(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
N12 Ni N12 180.00(19) . 2_666 ?
N12 Ni N4 90.67(12) . 2_666 ?
N12 Ni N4 89.33(12) 2_666 2_666 ?
N12 Ni N4 89.33(12) . . ?
N12 Ni N4 90.68(12) 2_666 . ?
N4 Ni N4 180.0 2_666 . ?
N12 Ni N8 91.44(13) . 2_666 ?
N12 Ni N8 88.56(13) 2_666 2_666 ?
N4 Ni N8 90.43(12) 2_666 2_666 ?
N4 Ni N8 89.56(12) . 2_666 ?
N12 Ni N8 88.56(13) . . ?
N12 Ni N8 91.44(13) 2_666 . ?
N4 Ni N8 89.56(12) 2_666 . ?
N4 Ni N8 90.44(12) . . ?
N8 Ni N8 180.0 2_666 . ?
C1 N1 N2 108.5(3) . . ?
C1 N1 C2 131.3(4) . . ?
N2 N1 C2 120.1(3) . . ?
N3 N2 N1 107.0(3) . . ?
N2 N3 N4 109.7(3) . . ?
C1 N4 N3 106.1(3) . . ?
C1 N4 Ni 133.4(3) . . ?
N3 N4 Ni 120.4(3) . . ?
C3 N5 N6 108.8(3) . . ?
C3 N5 C4 130.5(4) . . ?
N6 N5 C4 120.6(3) . . ?
N7 N6 N5 106.2(3) . . ?
N6 N7 N8 110.3(3) . . ?
C3 N8 N7 106.0(3) . . ?
C3 N8 Ni 131.0(3) . . ?
N7 N8 Ni 123.0(3) . . ?
C5 N9 N10 108.3(3) . . ?
C5 N9 C6 129.6(4) . . ?
N10 N9 C6 122.1(3) . . ?
N11 N10 N9 107.2(3) . . ?
N10 N11 N12 110.1(3) . . ?
C5 N12 N11 105.7(3) . . ?
C5 N12 Ni 130.8(3) . . ?
N11 N12 Ni 123.6(3) . . ?
N1 C1 N4 108.6(4) . . ?
N1 C1 H1 125.7 . . ?
N4 C1 H1 125.7 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N8 C3 N5 108.7(3) . . ?
N8 C3 H3 125.7 . . ?
N5 C3 H3 125.7 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N12 C5 N9 108.8(4) . . ?
N12 C5 H5 125.6 . . ?
N9 C5 H5 125.6 . . ?
N9 C6 H6A 109.5 . . ?
N9 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N9 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N13 N14 107.7(4) . . ?
C7 N13 C8 130.7(4) . . ?
N14 N13 C8 121.5(4) . . ?
N15 N14 N13 106.2(4) . . ?
N14 N15 N16 111.0(4) . . ?
C7 N16 N15 105.5(4) . . ?
N16 C7 N13 109.5(4) . . ?
N16 C7 H7 125.2 . . ?
N13 C7 H7 125.2 . . ?
N13 C8 H8A 109.5 . . ?
N13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 Cl1 O4 110.9(5) . . ?
O3 Cl1 O2 108.8(3) . . ?
O4 Cl1 O2 114.8(4) . . ?
O3 Cl1 O1 104.9(4) . . ?
O4 Cl1 O1 107.0(3) . . ?
O2 Cl1 O1 110.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.9(5) . . . . ?
C2 N1 N2 N3 177.8(4) . . . . ?
N1 N2 N3 N4 -1.0(5) . . . . ?
N2 N3 N4 C1 0.8(5) . . . . ?
N2 N3 N4 Ni -176.1(3) . . . . ?
C3 N5 N6 N7 -0.8(5) . . . . ?
C4 N5 N6 N7 -179.0(4) . . . . ?
N5 N6 N7 N8 0.5(5) . . . . ?
N6 N7 N8 C3 0.0(5) . . . . ?
N6 N7 N8 Ni -179.8(3) . . . . ?
C5 N9 N10 N11 -0.6(5) . . . . ?
C6 N9 N10 N11 -179.0(4) . . . . ?
N9 N10 N11 N12 0.5(5) . . . . ?
N10 N11 N12 C5 -0.2(5) . . . . ?
N10 N11 N12 Ni 178.7(3) . . . . ?
N2 N1 C1 N4 -0.4(4) . . . . ?
C2 N1 C1 N4 -176.8(4) . . . . ?
N3 N4 C1 N1 -0.3(4) . . . . ?
Ni N4 C1 N1 176.1(3) . . . . ?
N7 N8 C3 N5 -0.5(4) . . . . ?
Ni N8 C3 N5 179.2(3) . . . . ?
N6 N5 C3 N8 0.8(5) . . . . ?
C4 N5 C3 N8 178.7(4) . . . . ?
N11 N12 C5 N9 -0.2(4) . . . . ?
Ni N12 C5 N9 -178.9(3) . . . . ?
N10 N9 C5 N12 0.5(4) . . . . ?
C6 N9 C5 N12 178.7(4) . . . . ?
C7 N13 N14 N15 0.2(5) . . . . ?
C8 N13 N14 N15 -175.4(4) . . . . ?
N13 N14 N15 N16 0.1(5) . . . . ?
N14 N15 N16 C7 -0.3(5) . . . . ?
N15 N16 C7 N13 0.4(5) . . . . ?
N14 N13 C7 N16 -0.3(5) . . . . ?
C8 N13 C7 N16 174.6(4) . . . . ?

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

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

_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         0.913
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.090

_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_lx347
_database_code_depnum_ccdc_archive 'CCDC 1566384'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Jul 15 08:58:50 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl) copper(II) dinitrate dihydrate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl) copper(II) dinitrate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 Cu N24, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C12 H28 Cu N26 O8'
_chemical_formula_weight         728.14

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



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.8722(2)
_cell_length_b                   13.2085(4)
_cell_length_c                   16.9461(5)
_cell_angle_alpha                88.192(3)
_cell_angle_beta                 89.492(3)
_cell_angle_gamma                75.344(3)
_cell_volume                     1487.43(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8470
_cell_measurement_theta_min      4.6890
_cell_measurement_theta_max      31.9180

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.821
_shelx_estimated_absorpt_T_min   0.762
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96748
_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    1.626
_exptl_crystal_F_000             750
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            21999
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.466
_diffrn_reflns_theta_max         26.000
_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             5834
_reflns_number_gt                5065
_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)+(0.0375P)²+0.8826P] 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         5834
_refine_ls_number_parameters     473
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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      0.0249237000
_diffrn_orient_matrix_UB_12      0.0451432000
_diffrn_orient_matrix_UB_13      -0.0164699000
_diffrn_orient_matrix_UB_21      0.0168626000
_diffrn_orient_matrix_UB_22      0.0157797000
_diffrn_orient_matrix_UB_23      0.0384300000
_diffrn_orient_matrix_UB_31      0.1023519000
_diffrn_orient_matrix_UB_32      -0.0282289000
_diffrn_orient_matrix_UB_33      -0.0023607000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -99.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -60.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega  -58.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega  -97.00  -33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  143.0000  -39.0000 64

#__ type_ start__ end____ width___ exp.time_
  4 omega  -98.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000   30.0000 93

#__ type_ start__ end____ width___ exp.time_
  5 omega  -94.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega  -43.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -77.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000 -150.0000 76

#__ type_ start__ end____ width___ exp.time_
  8 omega  -23.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 91

#__ type_ start__ end____ width___ exp.time_
  9 omega  -41.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -38.0000  150.0000 73

#__ type_ start__ end____ width___ exp.time_
 10 omega  -34.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  132.0000  -35.6605 31

#__ type_ start__ end____ width___ exp.time_
 11 omega  -29.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000  -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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.0000 0.01438(8) Uani 1 2 d S . P . .
N1 N 0.5903(2) 0.63543(11) 0.00259(9) 0.0164(3) Uani 1 1 d . . . . .
N2 N 0.6847(3) 0.66118(13) 0.06635(10) 0.0276(4) Uani 1 1 d . . . . .
N3 N 0.7288(3) 0.74925(13) 0.05193(10) 0.0292(4) Uani 1 1 d . . . . .
N4 N 0.6642(2) 0.78140(11) -0.02119(9) 0.0178(3) Uani 1 1 d . . . . .
N5 N 0.3023(2) 0.55350(11) 0.08713(8) 0.0158(3) Uani 1 1 d . . . . .
N6 N 0.2510(2) 0.49075(12) 0.14504(9) 0.0199(3) Uani 1 1 d . . . . .
N7 N 0.1280(2) 0.54757(12) 0.19374(9) 0.0208(3) Uani 1 1 d . . . . .
N8 N 0.0967(2) 0.64786(12) 0.16725(9) 0.0179(3) Uani 1 1 d . . . . .
N9 N 0.7429(2) 0.42085(12) 0.09917(9) 0.0200(3) Uani 1 1 d . . . . .
N10 N 0.9011(2) 0.33498(13) 0.09239(10) 0.0263(4) Uani 1 1 d . . . . .
N11 N 0.9864(2) 0.30808(13) 0.16039(10) 0.0266(4) Uani 1 1 d . . . . .
N12 N 0.8833(2) 0.37673(12) 0.21227(9) 0.0186(3) Uani 1 1 d . . . . .
C1 C 0.5797(3) 0.71135(14) -0.05028(11) 0.0186(4) Uani 1 1 d . . . . .
C2 C 0.6945(3) 0.87865(15) -0.05663(13) 0.0263(4) Uani 1 1 d . . . . .
H2A H 0.8056 0.8623 -0.0946 0.039 Uiso 1 1 calc R U . . .
H2B H 0.7267 0.9219 -0.0152 0.039 Uiso 1 1 calc R U . . .
H2C H 0.5713 0.9169 -0.0839 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2041(3) 0.65040(14) 0.10243(11) 0.0171(4) Uani 1 1 d . . . . .
C4 C -0.0296(3) 0.73316(16) 0.21125(12) 0.0266(4) Uani 1 1 d . . . . .
H4A H 0.0380 0.7413 0.2604 0.040 Uiso 1 1 calc R U . . .
H4B H -0.1586 0.7173 0.2235 0.040 Uiso 1 1 calc R U . . .
H4C H -0.0533 0.7983 0.1793 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7372(3) 0.44514(15) 0.17390(11) 0.0190(4) Uani 1 1 d . . . . .
C6 C 0.9361(3) 0.37072(17) 0.29585(11) 0.0273(4) Uani 1 1 d . . . . .
H6A H 1.0313 0.4133 0.3047 0.041 Uiso 1 1 calc R U . . .
H6B H 0.9981 0.2978 0.3117 0.041 Uiso 1 1 calc R U . . .
H6C H 0.8144 0.3970 0.3273 0.041 Uiso 1 1 calc R U . . .
Cu2 Cu 0.0000 0.0000 0.5000 0.01419(8) Uani 1 2 d S . P . .
N15 N 0.1043(2) 0.11722(11) 0.54238(8) 0.0155(3) Uani 1 1 d . . . . .
N16 N 0.2264(2) 0.10385(12) 0.60691(9) 0.0201(3) Uani 1 1 d . . . . .
N17 N 0.2620(2) 0.19217(12) 0.62317(9) 0.0206(3) Uani 1 1 d . . . . .
N18 N 0.1640(2) 0.26337(11) 0.56929(9) 0.0174(3) Uani 1 1 d . . . . .
N19 N -0.1668(2) 0.00152(11) 0.60066(9) 0.0162(3) Uani 1 1 d . . . . .
N20 N -0.1942(2) -0.08779(12) 0.63679(9) 0.0211(3) Uani 1 1 d . . . . .
N21 N -0.2994(2) -0.06448(12) 0.70019(10) 0.0224(3) Uani 1 1 d . . . . .
N22 N -0.3418(2) 0.04048(11) 0.70552(9) 0.0161(3) Uani 1 1 d . . . . .
N23 N 0.2700(2) -0.12530(12) 0.56284(9) 0.0192(3) Uani 1 1 d . . . . .
N24 N 0.4263(2) -0.19071(12) 0.52573(9) 0.0223(3) Uani 1 1 d . . . . .
N25 N 0.5393(2) -0.25371(12) 0.57648(9) 0.0226(3) Uani 1 1 d . . . . .
N26 N 0.4563(2) -0.22941(11) 0.64781(9) 0.0169(3) Uani 1 1 d . . . . .
C7 C 0.1746(3) 0.37248(15) 0.56941(13) 0.0278(4) Uani 1 1 d . . . . .
H7A H 0.2954 0.3796 0.5409 0.042 Uiso 1 1 calc R U . . .
H7B H 0.1805 0.3940 0.6240 0.042 Uiso 1 1 calc R U . . .
H7C H 0.0551 0.4170 0.5434 0.042 Uiso 1 1 calc R U . . .
C8 C 0.0688(3) 0.21644(14) 0.52012(11) 0.0167(4) Uani 1 1 d . . . . .
C9 C -0.2601(3) 0.07951(14) 0.64479(10) 0.0158(4) Uani 1 1 d . . . . .
C10 C -0.4536(3) 0.09319(15) 0.77295(11) 0.0243(4) Uani 1 1 d . . . . .
H10A H -0.4738 0.1691 0.7657 0.037 Uiso 1 1 calc R U . . .
H10B H -0.3773 0.0693 0.8215 0.037 Uiso 1 1 calc R U . . .
H10C H -0.5845 0.0765 0.7767 0.037 Uiso 1 1 calc R U . . .
C11 C 0.2937(3) -0.15057(14) 0.63852(11) 0.0189(4) Uani 1 1 d . . . . .
C12 C 0.5443(3) -0.28633(15) 0.71941(11) 0.0220(4) Uani 1 1 d . . . . .
H12A H 0.6492 -0.2554 0.7391 0.033 Uiso 1 1 calc R U . . .
H12B H 0.6034 -0.3599 0.7075 0.033 Uiso 1 1 calc R U . . .
H12C H 0.4395 -0.2820 0.7597 0.033 Uiso 1 1 calc R U . . .
O1 O 0.4637(2) 0.64638(11) 0.26509(8) 0.0274(3) Uani 1 1 d . . . . .
O2 O 0.4711(2) 0.51626(10) 0.34716(9) 0.0304(3) Uani 1 1 d . . . . .
O3 O 0.2890(2) 0.67118(10) 0.37308(8) 0.0283(3) Uani 1 1 d . . . . .
N13 N 0.4078(2) 0.61138(12) 0.32814(9) 0.0208(3) Uani 1 1 d . . . . .
O4 O 0.8538(3) 0.00320(14) 0.09549(9) 0.0450(4) Uani 1 1 d . . . . .
O5 O 0.9446(2) 0.00341(13) 0.21667(9) 0.0412(4) Uani 1 1 d . . . . .
O6 O 0.7116(3) 0.12967(13) 0.16894(10) 0.0488(5) Uani 1 1 d . . . . .
N14 N 0.8389(2) 0.04665(12) 0.16089(9) 0.0222(3) Uani 1 1 d . . . . .
O7 O 0.2244(3) 0.87169(12) 0.04629(11) 0.0325(4) Uani 1 1 d . . . . .
O8 O 0.7364(2) 0.41097(12) 0.47091(10) 0.0282(3) Uani 1 1 d . . . . .
H9 H -0.269(3) 0.1484(17) 0.6355(12) 0.016(5) Uiso 1 1 d . . . . .
H3 H 0.209(3) 0.7094(17) 0.0763(13) 0.020(5) Uiso 1 1 d . . . . .
H8 H -0.011(3) 0.2489(17) 0.4778(13) 0.024(5) Uiso 1 1 d . . . . .
H11 H 0.217(3) -0.1200(17) 0.6795(13) 0.026(6) Uiso 1 1 d . . . . .
H5 H 0.657(3) 0.5000(17) 0.1981(13) 0.024(5) Uiso 1 1 d . . . . .
H1 H 0.524(3) 0.7170(16) -0.0985(14) 0.024(6) Uiso 1 1 d . . . . .
H81 H 0.709(4) 0.394(2) 0.5186(17) 0.038(7) Uiso 1 1 d . . . . .
H72 H 0.221(4) 0.900(2) -0.0053(18) 0.046(8) Uiso 1 1 d . . . . .
H82 H 0.639(4) 0.437(2) 0.4498(16) 0.036(8) Uiso 1 1 d . . . . .
H71 H 0.134(4) 0.898(2) 0.0627(17) 0.038(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 N5 2.0174(14) 2_665 ?
Cu1 N5 2.0175(14) . ?
Cu1 N1 2.0381(15) . ?
Cu1 N1 2.0381(15) 2_665 ?
Cu1 N9 2.3999(15) 2_665 ?
Cu1 N9 2.3999(15) . ?
N1 C1 1.312(2) . ?
N1 N2 1.361(2) . ?
N2 N3 1.290(2) . ?
N3 N4 1.339(2) . ?
N4 C1 1.320(2) . ?
N4 C2 1.462(2) . ?
N5 C3 1.320(2) . ?
N5 N6 1.365(2) . ?
N6 N7 1.290(2) . ?
N7 N8 1.350(2) . ?
N8 C3 1.322(2) . ?
N8 C4 1.458(2) . ?
N9 C5 1.314(2) . ?
N9 N10 1.365(2) . ?
N10 N11 1.296(2) . ?
N11 N12 1.346(2) . ?
N12 C5 1.328(2) . ?
N12 C6 1.460(2) . ?
C1 H1 0.90(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.89(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 0.90(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Cu2 N15 2.0166(14) . ?
Cu2 N15 2.0166(14) 2_556 ?
Cu2 N19 2.0443(15) 2_556 ?
Cu2 N19 2.0443(15) . ?
Cu2 N23 2.3843(15) . ?
Cu2 N23 2.3843(15) 2_556 ?
N15 C8 1.315(2) . ?
N15 N16 1.364(2) . ?
N16 N17 1.289(2) . ?
N17 N18 1.344(2) . ?
N18 C8 1.325(2) . ?
N18 C7 1.461(2) . ?
N19 C9 1.318(2) . ?
N19 N20 1.366(2) . ?
N20 N21 1.291(2) . ?
N21 N22 1.348(2) . ?
N22 C9 1.321(2) . ?
N22 C10 1.464(2) . ?
N23 C11 1.316(2) . ?
N23 N24 1.360(2) . ?
N24 N25 1.294(2) . ?
N25 N26 1.345(2) . ?
N26 C11 1.328(2) . ?
N26 C12 1.459(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.93(2) . ?
C9 H9 0.90(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.91(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O1 N13 1.247(2) . ?
O2 N13 1.254(2) . ?
O3 N13 1.253(2) . ?
O4 N14 1.256(2) . ?
O5 N14 1.231(2) . ?
O6 N14 1.228(2) . ?
O7 H72 0.94(3) . ?
O7 H71 0.69(3) . ?
O8 H81 0.86(3) . ?
O8 H82 0.76(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
N5 Cu1 N5 180.0 2_665 . ?
N5 Cu1 N1 91.03(6) 2_665 . ?
N5 Cu1 N1 88.97(6) . . ?
N5 Cu1 N1 88.97(6) 2_665 2_665 ?
N5 Cu1 N1 91.03(6) . 2_665 ?
N1 Cu1 N1 180.0 . 2_665 ?
N5 Cu1 N9 88.55(6) 2_665 2_665 ?
N5 Cu1 N9 91.45(6) . 2_665 ?
N1 Cu1 N9 89.23(6) . 2_665 ?
N1 Cu1 N9 90.77(6) 2_665 2_665 ?
N5 Cu1 N9 91.45(6) 2_665 . ?
N5 Cu1 N9 88.55(6) . . ?
N1 Cu1 N9 90.77(6) . . ?
N1 Cu1 N9 89.23(6) 2_665 . ?
N9 Cu1 N9 180.0 2_665 . ?
C1 N1 N2 106.17(15) . . ?
C1 N1 Cu1 131.73(13) . . ?
N2 N1 Cu1 122.08(12) . . ?
N3 N2 N1 109.43(15) . . ?
N2 N3 N4 107.28(15) . . ?
C1 N4 N3 108.30(15) . . ?
C1 N4 C2 130.39(16) . . ?
N3 N4 C2 121.30(15) . . ?
C3 N5 N6 106.62(14) . . ?
C3 N5 Cu1 129.59(13) . . ?
N6 N5 Cu1 123.75(11) . . ?
N7 N6 N5 109.49(14) . . ?
N6 N7 N8 106.91(14) . . ?
C3 N8 N7 108.87(14) . . ?
C3 N8 C4 130.19(16) . . ?
N7 N8 C4 120.85(15) . . ?
C5 N9 N10 105.74(15) . . ?
C5 N9 Cu1 126.30(12) . . ?
N10 N9 Cu1 127.60(12) . . ?
N11 N10 N9 110.27(15) . . ?
N10 N11 N12 106.45(15) . . ?
C5 N12 N11 108.59(15) . . ?
C5 N12 C6 129.25(16) . . ?
N11 N12 C6 122.16(15) . . ?
N1 C1 N4 108.82(16) . . ?
N1 C1 H1 127.2(14) . . ?
N4 C1 H1 124.0(14) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.11(16) . . ?
N5 C3 H3 128.3(13) . . ?
N8 C3 H3 123.6(13) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C5 N12 108.94(16) . . ?
N9 C5 H5 129.3(14) . . ?
N12 C5 H5 121.7(14) . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N15 Cu2 N15 180.00(4) . 2_556 ?
N15 Cu2 N19 91.07(6) . 2_556 ?
N15 Cu2 N19 88.93(6) 2_556 2_556 ?
N15 Cu2 N19 88.93(6) . . ?
N15 Cu2 N19 91.07(6) 2_556 . ?
N19 Cu2 N19 180.0 2_556 . ?
N15 Cu2 N23 90.10(5) . . ?
N15 Cu2 N23 89.90(5) 2_556 . ?
N19 Cu2 N23 90.88(5) 2_556 . ?
N19 Cu2 N23 89.12(5) . . ?
N15 Cu2 N23 89.90(5) . 2_556 ?
N15 Cu2 N23 90.10(5) 2_556 2_556 ?
N19 Cu2 N23 89.12(5) 2_556 2_556 ?
N19 Cu2 N23 90.88(5) . 2_556 ?
N23 Cu2 N23 180.0 . 2_556 ?
C8 N15 N16 106.75(14) . . ?
C8 N15 Cu2 130.83(13) . . ?
N16 N15 Cu2 122.35(11) . . ?
N17 N16 N15 109.28(14) . . ?
N16 N17 N18 107.16(14) . . ?
C8 N18 N17 108.73(14) . . ?
C8 N18 C7 129.49(16) . . ?
N17 N18 C7 121.77(15) . . ?
C9 N19 N20 106.34(14) . . ?
C9 N19 Cu2 131.00(12) . . ?
N20 N19 Cu2 122.62(11) . . ?
N21 N20 N19 109.62(14) . . ?
N20 N21 N22 106.80(14) . . ?
C9 N22 N21 108.89(14) . . ?
C9 N22 C10 129.93(16) . . ?
N21 N22 C10 121.11(15) . . ?
C11 N23 N24 105.77(15) . . ?
C11 N23 Cu2 128.18(12) . . ?
N24 N23 Cu2 125.92(11) . . ?
N25 N24 N23 110.40(15) . . ?
N24 N25 N26 106.47(14) . . ?
C11 N26 N25 108.53(15) . . ?
C11 N26 C12 130.09(16) . . ?
N25 N26 C12 121.38(15) . . ?
N18 C7 H7A 109.5 . . ?
N18 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N18 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N15 C8 N18 108.08(16) . . ?
N15 C8 H8 126.5(13) . . ?
N18 C8 H8 125.5(13) . . ?
N19 C9 N22 108.34(16) . . ?
N19 C9 H9 126.8(13) . . ?
N22 C9 H9 124.9(13) . . ?
N22 C10 H10A 109.5 . . ?
N22 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N22 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N23 C11 N26 108.81(16) . . ?
N23 C11 H11 127.9(14) . . ?
N26 C11 H11 123.2(14) . . ?
N26 C12 H12A 109.5 . . ?
N26 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N26 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 N13 O3 120.20(15) . . ?
O1 N13 O2 120.16(15) . . ?
O3 N13 O2 119.64(16) . . ?
O6 N14 O5 121.11(17) . . ?
O6 N14 O4 118.97(17) . . ?
O5 N14 O4 119.83(17) . . ?
H72 O7 H71 105(3) . . ?
H81 O8 H82 109(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.0(2) . . . . ?
Cu1 N1 N2 N3 178.70(13) . . . . ?
N1 N2 N3 N4 -0.2(2) . . . . ?
N2 N3 N4 C1 0.3(2) . . . . ?
N2 N3 N4 C2 -178.83(17) . . . . ?
C3 N5 N6 N7 -0.5(2) . . . . ?
Cu1 N5 N6 N7 177.54(11) . . . . ?
N5 N6 N7 N8 0.62(19) . . . . ?
N6 N7 N8 C3 -0.6(2) . . . . ?
N6 N7 N8 C4 -177.32(16) . . . . ?
C5 N9 N10 N11 0.5(2) . . . . ?
Cu1 N9 N10 N11 -172.92(12) . . . . ?
N9 N10 N11 N12 0.1(2) . . . . ?
N10 N11 N12 C5 -0.6(2) . . . . ?
N10 N11 N12 C6 179.75(17) . . . . ?
N2 N1 C1 N4 0.2(2) . . . . ?
Cu1 N1 C1 N4 -178.35(12) . . . . ?
N3 N4 C1 N1 -0.3(2) . . . . ?
C2 N4 C1 N1 178.70(17) . . . . ?
N6 N5 C3 N8 0.1(2) . . . . ?
Cu1 N5 C3 N8 -177.74(12) . . . . ?
N7 N8 C3 N5 0.3(2) . . . . ?
C4 N8 C3 N5 176.63(17) . . . . ?
N10 N9 C5 N12 -0.8(2) . . . . ?
Cu1 N9 C5 N12 172.67(11) . . . . ?
N11 N12 C5 N9 0.9(2) . . . . ?
C6 N12 C5 N9 -179.47(18) . . . . ?
C8 N15 N16 N17 0.43(19) . . . . ?
Cu2 N15 N16 N17 -176.89(11) . . . . ?
N15 N16 N17 N18 -0.22(19) . . . . ?
N16 N17 N18 C8 -0.07(19) . . . . ?
N16 N17 N18 C7 -178.92(16) . . . . ?
C9 N19 N20 N21 -0.14(19) . . . . ?
Cu2 N19 N20 N21 177.86(12) . . . . ?
N19 N20 N21 N22 0.26(19) . . . . ?
N20 N21 N22 C9 -0.3(2) . . . . ?
N20 N21 N22 C10 -177.55(16) . . . . ?
C11 N23 N24 N25 0.6(2) . . . . ?
Cu2 N23 N24 N25 -175.65(12) . . . . ?
N23 N24 N25 N26 -0.03(19) . . . . ?
N24 N25 N26 C11 -0.5(2) . . . . ?
N24 N25 N26 C12 179.32(15) . . . . ?
N16 N15 C8 N18 -0.46(19) . . . . ?
Cu2 N15 C8 N18 176.54(12) . . . . ?
N17 N18 C8 N15 0.3(2) . . . . ?
C7 N18 C8 N15 179.07(17) . . . . ?
N20 N19 C9 N22 -0.04(19) . . . . ?
Cu2 N19 C9 N22 -177.80(12) . . . . ?
N21 N22 C9 N19 0.2(2) . . . . ?
C10 N22 C9 N19 177.14(17) . . . . ?
N24 N23 C11 N26 -0.9(2) . . . . ?
Cu2 N23 C11 N26 175.23(11) . . . . ?
N25 N26 C11 N23 0.9(2) . . . . ?
C12 N26 C11 N23 -178.93(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
O8 H81 O3 0.86(3) 2.00(3) 2.847(2) 166(2) 2_666
O7 H72 O4 0.94(3) 1.95(3) 2.849(2) 160(2) 2_665
O8 H82 O2 0.76(3) 2.18(3) 2.874(2) 152(3) .
O7 H71 O4 0.69(3) 2.15(3) 2.831(3) 168(3) 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         0.339
_refine_diff_density_min         -0.320
_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_lx133
_database_code_depnum_ccdc_archive 'CCDC 1566366'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sun Mar 13 11:25:38 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
 'hexakis-1-methyltetrazolyl cobalt(II) perchlorate'
;
_chemical_name_common            
'hexakis-1-methyltetrazolyl cobalt(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Cl2 Co N24 O8'
_chemical_formula_weight         762.38

_symmetry_cell_setting           TRIGONAL
_symmetry_space_group_name_H-M   'R -3'
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 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+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.5455(3)
_cell_length_b                   19.5455(3)
_cell_length_c                   21.3390(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7059.9(3)
_cell_formula_units_Z            9
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7597
_cell_measurement_theta_min      4.4230
_cell_measurement_theta_max      31.4910

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.797
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87404
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_F_000             3501
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            35040
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.171
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3069
_reflns_number_gt                2547
_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)+(0.0416P)²+14.8394P] 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         3069
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0824
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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      -0.0298600000
_diffrn_orient_matrix_UB_12      -0.0025143000
_diffrn_orient_matrix_UB_13      -0.0203572000
_diffrn_orient_matrix_UB_21      -0.0225992000
_diffrn_orient_matrix_UB_22      -0.0412541000
_diffrn_orient_matrix_UB_23      0.0055209000
_diffrn_orient_matrix_UB_31      -0.0188085000
_diffrn_orient_matrix_UB_32      0.0068766000
_diffrn_orient_matrix_UB_33      0.0256949000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -99.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega -109.00  -59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -90.0000 50

#__ type_ start__ end____ width___ exp.time_
  3 omega  -92.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000  120.0000 96

#__ type_ start__ end____ width___ exp.time_
  4 omega  -92.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
  5 omega  -58.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
  6 omega  -43.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -77.0000  -90.0000 106

#__ type_ start__ end____ width___ exp.time_
  7 omega  -24.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 90

#__ type_ start__ end____ width___ exp.time_
  8 omega  -34.00   -1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  132.0000  -63.4889 33

#__ type_ start__ end____ width___ exp.time_
  9 omega  -41.00   19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  150.0000 60

#__ type_ start__ end____ width___ exp.time_
 10 omega  -24.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 96

#__ type_ start__ end____ width___ exp.time_
 11 omega  -31.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932    0.0000  -90.0000 129

;



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'
Co Co 0.3494 0.9721 '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
Co1 Co 0.0000 0.0000 0.0000 0.01278(15) Uani 1 6 d S T P . .
N1 N 0.00927(9) 0.09538(9) 0.05523(7) 0.0162(3) Uani 1 1 d . . . . .
N2 N -0.05376(10) 0.09111(10) 0.08585(8) 0.0207(4) Uani 1 1 d . . . . .
N3 N -0.03503(10) 0.15961(10) 0.10838(8) 0.0233(4) Uani 1 1 d . . . . .
N4 N 0.04062(10) 0.20908(10) 0.09233(8) 0.0190(4) Uani 1 1 d . . . . .
C1 C 0.06710(13) 0.16897(12) 0.06058(9) 0.0183(4) Uani 1 1 d . . . . .
C2 C 0.08118(16) 0.29313(14) 0.10835(13) 0.0311(5) Uani 1 1 d . . . . .
Co2 Co 0.0000 0.0000 0.30813(2) 0.01816(14) Uani 1 3 d S T P . .
N5 N 0.00845(10) 0.09395(10) 0.36486(8) 0.0225(4) Uani 1 1 d . . . . .
N6 N -0.05332(11) 0.09084(11) 0.39686(10) 0.0301(4) Uani 1 1 d . . . . .
N7 N -0.02895(11) 0.15375(11) 0.43032(10) 0.0316(5) Uani 1 1 d . . . . .
N8 N 0.04955(10) 0.19837(10) 0.42030(8) 0.0233(4) Uani 1 1 d . . . . .
N9 N -0.00346(10) -0.09225(10) 0.25252(8) 0.0202(4) Uani 1 1 d . . . . .
N10 N 0.06345(10) -0.08125(10) 0.22355(9) 0.0241(4) Uani 1 1 d . . . . .
N11 N 0.04954(10) -0.14536(10) 0.19522(8) 0.0235(4) Uani 1 1 d . . . . .
N12 N -0.02662(10) -0.19857(10) 0.20568(8) 0.0198(4) Uani 1 1 d . . . . .
C3 C 0.07105(13) 0.16129(13) 0.38018(10) 0.0229(4) Uani 1 1 d . . . . .
C4 C 0.09657(16) 0.27569(15) 0.44935(13) 0.0336(6) Uani 1 1 d . . . . .
C5 C -0.05813(13) -0.16540(12) 0.24050(10) 0.0209(4) Uani 1 1 d . . . . .
C6 C -0.06146(15) -0.27811(14) 0.17950(13) 0.0310(5) Uani 1 1 d . . . . .
Cl1 Cl 0.33101(3) 0.35081(3) 0.03599(2) 0.03187(16) Uani 1 1 d . . . . .
O1 O 0.34706(15) 0.40648(14) -0.01308(9) 0.0657(7) Uani 1 1 d . . . . .
O2 O 0.38536(15) 0.32299(15) 0.03241(12) 0.0709(7) Uani 1 1 d . . . . .
O3 O 0.25367(12) 0.28596(14) 0.02953(11) 0.0713(7) Uani 1 1 d . . . . .
O4 O 0.33956(13) 0.38909(12) 0.09446(8) 0.0522(5) Uani 1 1 d . . . . .
H5 H -0.1081(14) -0.1896(13) 0.2527(10) 0.020(6) Uiso 1 1 d . . . . .
H1 H 0.1156(16) 0.1895(15) 0.0477(11) 0.028(6) Uiso 1 1 d . . . . .
H2C H 0.0736(15) 0.2988(15) 0.1513(13) 0.035(7) Uiso 1 1 d . . . . .
H6C H -0.0985(17) -0.3132(17) 0.2112(13) 0.041(8) Uiso 1 1 d . . . . .
H2B H 0.0619(16) 0.3187(16) 0.0829(13) 0.043(8) Uiso 1 1 d . . . . .
H2A H 0.1355(18) 0.3132(16) 0.1002(12) 0.040(7) Uiso 1 1 d . . . . .
H4B H 0.0918(16) 0.3146(17) 0.4249(13) 0.041(7) Uiso 1 1 d . . . . .
H3 H 0.1210(16) 0.1800(14) 0.3680(11) 0.027(6) Uiso 1 1 d . . . . .
H4A H 0.149(2) 0.2880(18) 0.4471(15) 0.058(9) Uiso 1 1 d . . . . .
H4C H 0.0801(17) 0.2734(17) 0.4913(14) 0.047(8) Uiso 1 1 d . . . . .
H6A H -0.020(2) -0.2921(19) 0.1751(15) 0.064(10) Uiso 1 1 d . . . . .
H6B H -0.0882(17) -0.2805(16) 0.1405(13) 0.043(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
Co1 N1 2.1352(16) 10 ?
Co1 N1 2.1352(16) 12 ?
Co1 N1 2.1352(16) 3 ?
Co1 N1 2.1352(16) 2 ?
Co1 N1 2.1352(16) 11 ?
Co1 N1 2.1353(16) . ?
N1 C1 1.317(3) . ?
N1 N2 1.360(2) . ?
N2 N3 1.291(2) . ?
N3 N4 1.345(2) . ?
N4 C1 1.322(3) . ?
N4 C2 1.464(3) . ?
C1 H1 0.87(3) . ?
C2 H2C 0.94(3) . ?
C2 H2B 0.94(3) . ?
C2 H2A 0.95(3) . ?
Co2 N9 2.1312(17) . ?
Co2 N9 2.1312(17) 3 ?
Co2 N9 2.1312(17) 2 ?
Co2 N5 2.1357(17) . ?
Co2 N5 2.1358(17) 3 ?
Co2 N5 2.1358(17) 2 ?
N5 C3 1.314(3) . ?
N5 N6 1.362(2) . ?
N6 N7 1.290(3) . ?
N7 N8 1.350(3) . ?
N8 C3 1.319(3) . ?
N8 C4 1.457(3) . ?
N9 C5 1.313(3) . ?
N9 N10 1.363(2) . ?
N10 N11 1.292(2) . ?
N11 N12 1.341(2) . ?
N12 C5 1.323(3) . ?
N12 C6 1.461(3) . ?
C3 H3 0.89(3) . ?
C4 H4B 0.96(3) . ?
C4 H4A 0.93(3) . ?
C4 H4C 0.95(3) . ?
C5 H5 0.88(2) . ?
C6 H6C 0.98(3) . ?
C6 H6A 0.98(3) . ?
C6 H6B 0.97(3) . ?
Cl1 O3 1.412(2) . ?
Cl1 O2 1.417(2) . ?
Cl1 O4 1.4210(18) . ?
Cl1 O1 1.428(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
N1 Co1 N1 92.47(6) 10 12 ?
N1 Co1 N1 87.53(6) 10 3 ?
N1 Co1 N1 180.00(10) 12 3 ?
N1 Co1 N1 87.53(6) 10 2 ?
N1 Co1 N1 87.53(6) 12 2 ?
N1 Co1 N1 92.47(6) 3 2 ?
N1 Co1 N1 92.47(6) 10 11 ?
N1 Co1 N1 92.47(6) 12 11 ?
N1 Co1 N1 87.53(6) 3 11 ?
N1 Co1 N1 180.00(17) 2 11 ?
N1 Co1 N1 180.0 10 . ?
N1 Co1 N1 87.53(6) 12 . ?
N1 Co1 N1 92.47(6) 3 . ?
N1 Co1 N1 92.47(6) 2 . ?
N1 Co1 N1 87.53(6) 11 . ?
C1 N1 N2 106.38(16) . . ?
C1 N1 Co1 130.79(14) . . ?
N2 N1 Co1 122.20(12) . . ?
N3 N2 N1 109.68(16) . . ?
N2 N3 N4 106.88(16) . . ?
C1 N4 N3 108.66(16) . . ?
C1 N4 C2 129.23(19) . . ?
N3 N4 C2 122.10(18) . . ?
N1 C1 N4 108.39(18) . . ?
N1 C1 H1 128.4(16) . . ?
N4 C1 H1 123.2(16) . . ?
N4 C2 H2C 109.2(16) . . ?
N4 C2 H2B 109.1(17) . . ?
H2C C2 H2B 112(2) . . ?
N4 C2 H2A 106.8(17) . . ?
H2C C2 H2A 110(2) . . ?
H2B C2 H2A 110(2) . . ?
N9 Co2 N9 92.00(6) . 3 ?
N9 Co2 N9 92.00(6) . 2 ?
N9 Co2 N9 92.00(6) 3 2 ?
N9 Co2 N5 177.61(6) . . ?
N9 Co2 N5 90.14(6) 3 . ?
N9 Co2 N5 86.86(6) 2 . ?
N9 Co2 N5 86.86(6) . 3 ?
N9 Co2 N5 177.61(6) 3 3 ?
N9 Co2 N5 90.14(6) 2 3 ?
N5 Co2 N5 91.04(7) . 3 ?
N9 Co2 N5 90.14(6) . 2 ?
N9 Co2 N5 86.86(6) 3 2 ?
N9 Co2 N5 177.61(6) 2 2 ?
N5 Co2 N5 91.04(7) . 2 ?
N5 Co2 N5 91.04(7) 3 2 ?
C3 N5 N6 106.31(17) . . ?
C3 N5 Co2 129.45(14) . . ?
N6 N5 Co2 124.06(13) . . ?
N7 N6 N5 109.78(18) . . ?
N6 N7 N8 106.68(17) . . ?
C3 N8 N7 108.62(18) . . ?
C3 N8 C4 129.6(2) . . ?
N7 N8 C4 121.76(19) . . ?
C5 N9 N10 106.11(17) . . ?
C5 N9 Co2 133.97(14) . . ?
N10 N9 Co2 119.81(13) . . ?
N11 N10 N9 109.83(16) . . ?
N10 N11 N12 106.74(16) . . ?
C5 N12 N11 108.75(17) . . ?
C5 N12 C6 130.74(19) . . ?
N11 N12 C6 120.51(18) . . ?
N5 C3 N8 108.60(19) . . ?
N5 C3 H3 128.2(16) . . ?
N8 C3 H3 123.2(16) . . ?
N8 C4 H4B 109.2(16) . . ?
N8 C4 H4A 106.7(19) . . ?
H4B C4 H4A 107(3) . . ?
N8 C4 H4C 109.3(18) . . ?
H4B C4 H4C 113(2) . . ?
H4A C4 H4C 112(3) . . ?
N9 C5 N12 108.57(19) . . ?
N9 C5 H5 127.2(15) . . ?
N12 C5 H5 124.2(15) . . ?
N12 C6 H6C 105.7(16) . . ?
N12 C6 H6A 108.9(19) . . ?
H6C C6 H6A 107(2) . . ?
N12 C6 H6B 109.4(16) . . ?
H6C C6 H6B 112(2) . . ?
H6A C6 H6B 114(3) . . ?
O3 Cl1 O2 108.77(16) . . ?
O3 Cl1 O4 110.47(14) . . ?
O2 Cl1 O4 109.64(14) . . ?
O3 Cl1 O1 109.94(15) . . ?
O2 Cl1 O1 109.38(15) . . ?
O4 Cl1 O1 108.63(13) . . ?

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(2) . . . . ?
Co1 N1 N2 N3 -171.26(12) . . . . ?
N1 N2 N3 N4 0.1(2) . . . . ?
N2 N3 N4 C1 -0.8(2) . . . . ?
N2 N3 N4 C2 177.94(19) . . . . ?
N2 N1 C1 N4 -1.0(2) . . . . ?
Co1 N1 C1 N4 169.83(13) . . . . ?
N3 N4 C1 N1 1.1(2) . . . . ?
C2 N4 C1 N1 -177.5(2) . . . . ?
C3 N5 N6 N7 -0.2(2) . . . . ?
Co2 N5 N6 N7 175.36(15) . . . . ?
N5 N6 N7 N8 -0.2(2) . . . . ?
N6 N7 N8 C3 0.5(2) . . . . ?
N6 N7 N8 C4 178.0(2) . . . . ?
C5 N9 N10 N11 0.0(2) . . . . ?
Co2 N9 N10 N11 176.62(13) . . . . ?
N9 N10 N11 N12 -0.1(2) . . . . ?
N10 N11 N12 C5 0.2(2) . . . . ?
N10 N11 N12 C6 179.76(19) . . . . ?
N6 N5 C3 N8 0.4(2) . . . . ?
Co2 N5 C3 N8 -174.75(14) . . . . ?
N7 N8 C3 N5 -0.6(2) . . . . ?
C4 N8 C3 N5 -177.8(2) . . . . ?
N10 N9 C5 N12 0.1(2) . . . . ?
Co2 N9 C5 N12 -175.84(14) . . . . ?
N11 N12 C5 N9 -0.2(2) . . . . ?
C6 N12 C5 N9 -179.7(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         0.888
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.062

_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_lx217
_database_code_depnum_ccdc_archive 'CCDC 1566371'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;

_vrf_PLAT097_lx217               
; PROBLEM: Large Reported Max.  (Positive) Residual Density   
RESPONSE: Low crystal quality
;
_audit_creation_date             
;
'Fri Apr 29 08:38:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
dichlorido tetrakis(1-methyl-5H-tetrazolyl) cobalt(II) di(1-methyl-5H-tetrazole)
;
_chemical_name_common            
;
dichlorido tetrakis(1-methyl-5H-tetrazolyl) cobalt(II) 
di(1-methyl-5H-tetrazole)
;
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H16 Cl2 Co N16, 2(C2 H4 N4)'
_chemical_formula_sum            'C12 H24 Cl2 Co N24'
_chemical_formula_weight         634.38

_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                   11.9613(6)
_cell_length_b                   6.7360(2)
_cell_length_c                   16.8524(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.389(5)
_cell_angle_gamma                90
_cell_volume                     1302.65(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6235
_cell_measurement_theta_min      4.5520
_cell_measurement_theta_max      32.0160

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.920
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90137
_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    1.617
_exptl_crystal_F_000             650
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            16601
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.565
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             2262
_reflns_number_gt                2054
_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)+(0.0718P)²+25.3702P] 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         2262
_refine_ls_number_parameters     185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0822
_refine_ls_wR_factor_ref         0.2310
_refine_ls_wR_factor_gt          0.2287
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_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      -0.0055812000
_diffrn_orient_matrix_UB_12      -0.1004900000
_diffrn_orient_matrix_UB_13      0.0109034000
_diffrn_orient_matrix_UB_21      0.0495146000
_diffrn_orient_matrix_UB_22      0.0105145000
_diffrn_orient_matrix_UB_23      0.0347492000
_diffrn_orient_matrix_UB_31      -0.0365366000
_diffrn_orient_matrix_UB_32      0.0296922000
_diffrn_orient_matrix_UB_33      0.0244837000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -89.00   40.50   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000   60.0000 185

#__ type_ start__ end____ width___ exp.time_
  2 omega -106.00  -71.70   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000  -90.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega   -2.30  102.00   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   60.0000 149

#__ type_ start__ end____ width___ exp.time_
  4 omega   -2.00   98.10   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -30.0000 143

#__ type_ start__ end____ width___ exp.time_
  5 omega   -3.00  100.60   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000 -120.0000 148

#__ type_ start__ end____ width___ exp.time_
  6 omega   -3.00   92.90   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  150.0000 137

#__ type_ start__ end____ width___ exp.time_
  7 omega  -19.00   74.10   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  120.0000 133

#__ type_ start__ end____ width___ exp.time_
  8 omega  -22.00   72.50   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 135

#__ type_ start__ end____ width___ exp.time_
  9 omega  -30.00   88.30   0.7000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000   90.0000 169

;



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'
Co Co 0.3494 0.9721 '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
Co1 Co 0.0000 0.5000 0.0000 0.0103(4) Uani 1 2 d S . P . .
Cl1 Cl -0.14689(14) 0.2393(3) -0.04194(11) 0.0152(5) Uani 1 1 d . . . . .
N1 N 0.0955(5) 0.3690(9) -0.0768(4) 0.0142(13) Uani 1 1 d . . . . .
N2 N 0.1387(6) 0.4670(10) -0.1319(4) 0.0199(14) Uani 1 1 d . . . . .
N3 N 0.1756(6) 0.3418(10) -0.1768(4) 0.0216(15) Uani 1 1 d . . . . .
N4 N 0.1565(5) 0.1592(9) -0.1507(4) 0.0153(13) Uani 1 1 d . . . . .
N5 N 0.1004(5) 0.3156(9) 0.0997(4) 0.0126(12) Uani 1 1 d . . . . .
N6 N 0.0646(5) 0.2002(10) 0.1533(4) 0.0181(14) Uani 1 1 d . . . . .
N7 N 0.1549(6) 0.1310(10) 0.2093(4) 0.0198(14) Uani 1 1 d . . . . .
N8 N 0.2502(5) 0.1998(9) 0.1913(4) 0.0151(13) Uani 1 1 d . . . . .
C1 C 0.1083(6) 0.1776(11) -0.0888(4) 0.0142(15) Uani 1 1 d . . . . .
H1 H 0.0871 0.0720 -0.0586 0.017 Uiso 1 1 calc R U . . .
C2 C 0.1896(7) -0.0193(12) -0.1877(5) 0.0216(17) Uani 1 1 d . . . . .
H2A H 0.2729 -0.0452 -0.1634 0.032 Uiso 1 1 calc R U . . .
H2B H 0.1737 -0.0001 -0.2475 0.032 Uiso 1 1 calc R U . . .
H2C H 0.1444 -0.1326 -0.1771 0.032 Uiso 1 1 calc R U . . .
C3 C 0.2152(6) 0.3153(11) 0.1247(4) 0.0140(15) Uani 1 1 d . . . . .
C4 C 0.3678(6) 0.1566(12) 0.2424(5) 0.0192(16) Uani 1 1 d . . . . .
H4A H 0.3809 0.0129 0.2440 0.029 Uiso 1 1 calc R U . . .
H4B H 0.3773 0.2057 0.2987 0.029 Uiso 1 1 calc R U . . .
H4C H 0.4244 0.2222 0.2190 0.029 Uiso 1 1 calc R U . . .
N9 N 0.5642(6) 0.7548(11) -0.0530(5) 0.0322(18) Uani 1 1 d . . . . .
N10 N 0.4514(6) 0.7084(11) -0.0897(4) 0.0281(16) Uani 1 1 d . . . . .
N11 N 0.3998(7) 0.7106(12) -0.0300(5) 0.0363(19) Uani 1 1 d . . . . .
N12 N 0.4788(6) 0.7551(10) 0.0400(4) 0.0204(14) Uani 1 1 d . . . . .
C5 C 0.5817(6) 0.7826(11) 0.0252(5) 0.0174(16) Uani 1 1 d . . . . .
H5 H 0.6533 0.8159 0.0645 0.021 Uiso 1 1 calc R U . . .
C6 C 0.4658(8) 0.7689(14) 0.1243(5) 0.029(2) Uani 1 1 d . . . . .
H6A H 0.3838 0.7928 0.1211 0.044 Uiso 1 1 calc R U . . .
H6B H 0.5135 0.8787 0.1539 0.044 Uiso 1 1 calc R U . . .
H6C H 0.4915 0.6443 0.1539 0.044 Uiso 1 1 calc R U . . .
H3 H 0.267(7) 0.381(12) 0.100(5) 0.009(18) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.142(6) 3_565 ?
Co1 N1 2.142(6) . ?
Co1 N5 2.161(6) . ?
Co1 N5 2.161(6) 3_565 ?
Co1 Cl1 2.4435(17) . ?
Co1 Cl1 2.4435(17) 3_565 ?
N1 C1 1.320(10) . ?
N1 N2 1.356(9) . ?
N2 N3 1.291(9) . ?
N3 N4 1.348(9) . ?
N4 C1 1.332(9) . ?
N4 C2 1.461(9) . ?
N5 C3 1.318(9) . ?
N5 N6 1.350(8) . ?
N6 N7 1.304(9) . ?
N7 N8 1.342(9) . ?
N8 C3 1.332(9) . ?
N8 C4 1.457(9) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.95(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N9 C5 1.288(11) . ?
N9 N10 1.353(11) . ?
N10 N11 1.320(11) . ?
N11 N12 1.321(11) . ?
N12 C5 1.336(10) . ?
N12 C6 1.474(10) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 180.0 3_565 . ?
N1 Co1 N5 92.3(2) 3_565 . ?
N1 Co1 N5 87.7(2) . . ?
N1 Co1 N5 87.7(2) 3_565 3_565 ?
N1 Co1 N5 92.3(2) . 3_565 ?
N5 Co1 N5 180.0 . 3_565 ?
N1 Co1 Cl1 90.48(16) 3_565 . ?
N1 Co1 Cl1 89.52(16) . . ?
N5 Co1 Cl1 90.48(16) . . ?
N5 Co1 Cl1 89.52(16) 3_565 . ?
N1 Co1 Cl1 89.52(16) 3_565 3_565 ?
N1 Co1 Cl1 90.48(16) . 3_565 ?
N5 Co1 Cl1 89.52(16) . 3_565 ?
N5 Co1 Cl1 90.48(16) 3_565 3_565 ?
Cl1 Co1 Cl1 180.0 . 3_565 ?
C1 N1 N2 106.7(6) . . ?
C1 N1 Co1 126.8(5) . . ?
N2 N1 Co1 125.8(5) . . ?
N3 N2 N1 110.1(6) . . ?
N2 N3 N4 106.7(6) . . ?
C1 N4 N3 108.8(6) . . ?
C1 N4 C2 129.8(7) . . ?
N3 N4 C2 121.3(6) . . ?
C3 N5 N6 106.5(6) . . ?
C3 N5 Co1 123.3(5) . . ?
N6 N5 Co1 129.8(4) . . ?
N7 N6 N5 109.6(6) . . ?
N6 N7 N8 107.2(6) . . ?
C3 N8 N7 107.9(6) . . ?
C3 N8 C4 129.5(6) . . ?
N7 N8 C4 122.5(6) . . ?
N1 C1 N4 107.8(6) . . ?
N1 C1 H1 126.1 . . ?
N4 C1 H1 126.1 . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.7(6) . . ?
N5 C3 H3 127(5) . . ?
N8 C3 H3 124(5) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 N9 N10 110.8(7) . . ?
N11 N10 N9 105.6(7) . . ?
N10 N11 N12 108.3(7) . . ?
N11 N12 C5 109.2(7) . . ?
N11 N12 C6 129.2(7) . . ?
C5 N12 C6 121.6(7) . . ?
N9 C5 N12 106.2(7) . . ?
N9 C5 H5 126.9 . . ?
N12 C5 H5 126.9 . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.6(8) . . . . ?
Co1 N1 N2 N3 -170.2(5) . . . . ?
N1 N2 N3 N4 0.0(8) . . . . ?
N2 N3 N4 C1 -0.6(8) . . . . ?
N2 N3 N4 C2 -179.2(7) . . . . ?
C3 N5 N6 N7 -0.1(8) . . . . ?
Co1 N5 N6 N7 -173.2(5) . . . . ?
N5 N6 N7 N8 -0.8(8) . . . . ?
N6 N7 N8 C3 1.5(8) . . . . ?
N6 N7 N8 C4 178.3(7) . . . . ?
N2 N1 C1 N4 -1.0(8) . . . . ?
Co1 N1 C1 N4 169.7(4) . . . . ?
N3 N4 C1 N1 1.0(8) . . . . ?
C2 N4 C1 N1 179.5(7) . . . . ?
N6 N5 C3 N8 1.0(8) . . . . ?
Co1 N5 C3 N8 174.7(5) . . . . ?
N7 N8 C3 N5 -1.6(8) . . . . ?
C4 N8 C3 N5 -178.1(7) . . . . ?
C5 N9 N10 N11 0.5(10) . . . . ?
N9 N10 N11 N12 -0.4(9) . . . . ?
N10 N11 N12 C5 0.3(9) . . . . ?
N10 N11 N12 C6 -177.6(8) . . . . ?
N10 N9 C5 N12 -0.3(9) . . . . ?
N11 N12 C5 N9 0.1(9) . . . . ?
C6 N12 C5 N9 178.1(7) . . . . ?

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         3.079
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.182

_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_mx113
_database_code_depnum_ccdc_archive 'CCDC 1566379'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Mar 10 13:55:43 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
bis(1-methyltetrazolyl) silver(I) nitrate
;
_chemical_name_common            'bis(1-methyltetrazolyl) silver(I) nitrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Ag N9 O3'
_chemical_formula_sum            'C4 H8 Ag N9 O3'
_chemical_formula_weight         338.06

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



_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.4897(3)
_cell_length_b                   29.2446(12)
_cell_length_c                   6.8299(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.214(5)
_cell_angle_gamma                90
_cell_volume                     1062.93(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3914
_cell_measurement_theta_min      4.3510
_cell_measurement_theta_max      32.1270

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.914
_shelx_estimated_absorpt_T_min   0.393
_shelx_estimated_absorpt_T_max   0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74554
_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    2.113
_exptl_crystal_F_000             664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            8289
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.181
_diffrn_reflns_theta_max         26.494
_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             2194
_reflns_number_gt                2129
_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)+2.4131P] 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         2194
_refine_ls_number_parameters     164
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0654
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.485
_refine_ls_restrained_S_all      1.485
_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      0.0340869000
_diffrn_orient_matrix_UB_12      -0.0171741000
_diffrn_orient_matrix_UB_13      0.0750670000
_diffrn_orient_matrix_UB_21      0.0236072000
_diffrn_orient_matrix_UB_22      0.0170530000
_diffrn_orient_matrix_UB_23      0.0761871000
_diffrn_orient_matrix_UB_31      -0.1267076000
_diffrn_orient_matrix_UB_32      -0.0014451000
_diffrn_orient_matrix_UB_33      0.0066433000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -40.00   26.40   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000   30.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega  -21.00   69.40   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 113

#__ type_ start__ end____ width___ exp.time_
  3 omega   57.00   98.60   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega   67.00  106.20   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -90.0000 49

#__ type_ start__ end____ width___ exp.time_
  5 omega    7.00  101.40   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000  150.0000 118

#__ type_ start__ end____ width___ exp.time_
  6 omega  -92.00  -58.40   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  143.0000  -17.0000 42

#__ type_ start__ end____ width___ exp.time_
  7 omega  -93.00    0.60   0.8000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000  -90.0000 117

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.20829(6) 0.14192(2) 0.23732(5) 0.02121(10) Uani 1 1 d . . . . .
O1 O -0.0273(5) 0.10082(10) 0.4629(5) 0.0256(7) Uani 1 1 d . . . . .
O2 O -0.2890(5) 0.14672(10) 0.2683(5) 0.0285(7) Uani 1 1 d . . . . .
O3 O -0.4233(5) 0.09962(10) 0.4637(5) 0.0258(7) Uani 1 1 d . . . . .
N1 N 0.1842(6) 0.21779(11) 0.2635(5) 0.0184(7) Uani 1 1 d . . . . .
N2 N 0.3678(6) 0.24786(11) 0.2468(6) 0.0235(8) Uani 1 1 d . . . . .
N3 N 0.2880(6) 0.28936(11) 0.2513(6) 0.0250(8) Uani 1 1 d . . . . .
N4 N 0.0502(6) 0.28660(10) 0.2706(5) 0.0158(7) Uani 1 1 d . . . . .
N5 N 0.1264(6) 0.08875(11) -0.0092(5) 0.0182(7) Uani 1 1 d . . . . .
N6 N 0.3102(6) 0.06481(11) -0.0681(5) 0.0197(7) Uani 1 1 d . . . . .
N7 N 0.2125(6) 0.03112(11) -0.1821(5) 0.0189(7) Uani 1 1 d . . . . .
N8 N -0.0373(6) 0.03254(10) -0.1990(5) 0.0156(7) Uani 1 1 d . . . . .
N9 N -0.2463(6) 0.11561(11) 0.3992(5) 0.0190(7) Uani 1 1 d . . . . .
C1 C -0.0095(7) 0.24284(13) 0.2767(6) 0.0180(8) Uani 1 1 d . . . . .
C2 C -0.0944(8) 0.32783(13) 0.2879(7) 0.0221(9) Uani 1 1 d . . . . .
H2A H -0.2726 0.3199 0.2656 0.033 Uiso 1 1 calc R U . . .
H2B H -0.0734 0.3502 0.1866 0.033 Uiso 1 1 calc R U . . .
H2C H -0.0339 0.3409 0.4233 0.033 Uiso 1 1 calc R U . . .
C3 C -0.0856(7) 0.06798(13) -0.0926(6) 0.0168(8) Uani 1 1 d . . . . .
C4 C -0.2097(8) 0.00141(13) -0.3302(6) 0.0217(9) Uani 1 1 d . . . . .
H4A H -0.3564 -0.0038 -0.2753 0.033 Uiso 1 1 calc R U . . .
H4B H -0.1248 -0.0278 -0.3381 0.033 Uiso 1 1 calc R U . . .
H4C H -0.2641 0.0148 -0.4655 0.033 Uiso 1 1 calc R U . . .
H3 H -0.241(8) 0.0748(13) -0.082(6) 0.015(10) Uiso 1 1 d . . . . .
H1 H -0.154(7) 0.2339(12) 0.283(6) 0.009(10) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.232(3) . ?
Ag1 N5 2.255(3) . ?
Ag1 O1 2.544(3) . ?
Ag1 O3 2.545(3) 1_655 ?
O1 N9 1.251(4) . ?
O2 N9 1.257(4) . ?
O3 N9 1.252(4) . ?
O3 Ag1 2.545(3) 1_455 ?
N1 C1 1.312(5) . ?
N1 N2 1.364(4) . ?
N2 N3 1.293(5) . ?
N3 N4 1.347(5) . ?
N4 C1 1.324(5) . ?
N4 C2 1.464(5) . ?
N5 C3 1.313(5) . ?
N5 N6 1.367(4) . ?
N6 N7 1.288(4) . ?
N7 N8 1.348(4) . ?
N8 C3 1.329(5) . ?
N8 C4 1.453(5) . ?
C1 H1 0.85(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.90(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 N5 137.76(12) . . ?
N1 Ag1 O1 111.85(11) . . ?
N5 Ag1 O1 95.09(11) . . ?
N1 Ag1 O3 119.24(11) . 1_655 ?
N5 Ag1 O3 95.82(11) . 1_655 ?
O1 Ag1 O3 81.30(9) . 1_655 ?
N9 O1 Ag1 102.3(2) . . ?
N9 O3 Ag1 100.0(2) . 1_455 ?
C1 N1 N2 105.9(3) . . ?
C1 N1 Ag1 128.7(3) . . ?
N2 N1 Ag1 125.1(2) . . ?
N3 N2 N1 110.0(3) . . ?
N2 N3 N4 106.8(3) . . ?
C1 N4 N3 108.3(3) . . ?
C1 N4 C2 130.6(3) . . ?
N3 N4 C2 121.1(3) . . ?
C3 N5 N6 106.0(3) . . ?
C3 N5 Ag1 129.5(3) . . ?
N6 N5 Ag1 123.1(2) . . ?
N7 N6 N5 110.0(3) . . ?
N6 N7 N8 107.0(3) . . ?
C3 N8 N7 108.2(3) . . ?
C3 N8 C4 129.7(3) . . ?
N7 N8 C4 121.9(3) . . ?
O1 N9 O3 120.7(3) . . ?
O1 N9 O2 119.6(3) . . ?
O3 N9 O2 119.7(3) . . ?
N1 C1 N4 109.0(3) . . ?
N1 C1 H1 128(3) . . ?
N4 C1 H1 123(3) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.9(3) . . ?
N5 C3 H3 128(3) . . ?
N8 C3 H3 123(3) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.5(5) . . . . ?
Ag1 N1 N2 N3 174.4(3) . . . . ?
N1 N2 N3 N4 -0.2(5) . . . . ?
N2 N3 N4 C1 -0.2(5) . . . . ?
N2 N3 N4 C2 177.8(4) . . . . ?
C3 N5 N6 N7 0.0(4) . . . . ?
Ag1 N5 N6 N7 167.8(2) . . . . ?
N5 N6 N7 N8 -0.1(4) . . . . ?
N6 N7 N8 C3 0.1(4) . . . . ?
N6 N7 N8 C4 175.2(3) . . . . ?
Ag1 O1 N9 O3 173.6(3) . . . . ?
Ag1 O1 N9 O2 -6.1(4) . . . . ?
Ag1 O3 N9 O1 -174.8(3) 1_455 . . . ?
Ag1 O3 N9 O2 4.9(4) 1_455 . . . ?
N2 N1 C1 N4 -0.6(5) . . . . ?
Ag1 N1 C1 N4 -174.2(3) . . . . ?
N3 N4 C1 N1 0.5(5) . . . . ?
C2 N4 C1 N1 -177.2(4) . . . . ?
N6 N5 C3 N8 0.1(4) . . . . ?
Ag1 N5 C3 N8 -166.6(3) . . . . ?
N7 N8 C3 N5 -0.1(4) . . . . ?
C4 N8 C3 N5 -174.7(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
? ? ? ? ? ? ? ?

_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         0.681
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.094

_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_lx311
_database_code_depnum_ccdc_archive 'CCDC 1566381'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Jun 20 22:31:03 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexakis(1-methyltetrazolyl)zinc(II) dinitrate dihydrate
;
_chemical_name_common            
'hexakis(1-methyltetrazolyl)zinc(II) dinitrate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C12 H24 N24 Zn, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C12 H28 N26 O8 Zn'
_chemical_formula_weight         729.97

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




_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.9267(5)
_cell_length_b                   13.2751(5)
_cell_length_c                   16.9711(11)
_cell_angle_alpha                92.342(4)
_cell_angle_beta                 90.442(5)
_cell_angle_gamma                104.792(5)
_cell_volume                     1507.29(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2913
_cell_measurement_theta_min      4.6630
_cell_measurement_theta_max      28.4260

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.900
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93492
_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    1.608
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            12378
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.1307
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.408
_diffrn_reflns_theta_max         26.000
_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             5911
_reflns_number_gt                4537
_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)+(0.0248P)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         5911
_refine_ls_number_parameters     473
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0030984000
_diffrn_orient_matrix_UB_12      0.0538662000
_diffrn_orient_matrix_UB_13      0.0018714000
_diffrn_orient_matrix_UB_21      0.0805196000
_diffrn_orient_matrix_UB_22      0.0094524000
_diffrn_orient_matrix_UB_23      0.0276934000
_diffrn_orient_matrix_UB_31      0.0687606000
_diffrn_orient_matrix_UB_32      0.0083072000
_diffrn_orient_matrix_UB_33      -0.0313032000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -13.00   23.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   38.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega -104.00  -32.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  163.0000   22.0000 89

#__ type_ start__ end____ width___ exp.time_
  3 omega   32.00  101.60   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  -60.0000 87

#__ type_ start__ end____ width___ exp.time_
  4 omega  -37.00   92.60   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000 -120.0000 162

#__ type_ start__ end____ width___ exp.time_
  5 omega  -21.00    5.40   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 33

#__ type_ start__ end____ width___ exp.time_
  6 omega   12.00   72.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega    1.00  101.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   30.0000 125

;



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 1.0000 0.0000 0.01782(12) Uani 1 2 d S . P . .
N1 N 0.7653(3) 0.85689(18) 0.00390(13) 0.0194(5) Uani 1 1 d . . . . .
N2 N 0.6539(4) 0.8294(2) 0.06873(15) 0.0335(7) Uani 1 1 d . . . . .
N3 N 0.5225(4) 0.7432(2) 0.05436(15) 0.0328(6) Uani 1 1 d . . . . .
N4 N 0.5459(3) 0.71252(17) -0.02078(14) 0.0201(5) Uani 1 1 d . . . . .
N5 N 1.1570(3) 0.94490(18) 0.09096(13) 0.0193(5) Uani 1 1 d . . . . .
N6 N 1.2750(4) 1.00808(19) 0.14755(14) 0.0238(6) Uani 1 1 d . . . . .
N7 N 1.3411(4) 0.9516(2) 0.19677(14) 0.0257(6) Uani 1 1 d . . . . .
N8 N 1.2670(3) 0.85150(19) 0.17190(13) 0.0206(5) Uani 1 1 d . . . . .
N9 N 0.8549(3) 1.07252(18) 0.09206(13) 0.0209(5) Uani 1 1 d . . . . .
N10 N 0.7778(4) 1.15615(19) 0.08229(14) 0.0286(6) Uani 1 1 d . . . . .
N11 N 0.7185(4) 1.1863(2) 0.14910(15) 0.0294(6) Uani 1 1 d . . . . .
N12 N 0.7570(3) 1.12211(18) 0.20335(13) 0.0215(5) Uani 1 1 d . . . . .
C1 C 0.6953(5) 0.7831(2) -0.04937(18) 0.0227(7) Uani 1 1 d . . . . .
C2 C 0.4186(5) 0.6174(2) -0.05749(19) 0.0313(7) Uani 1 1 d . . . . .
H2A H 0.3169 0.6349 -0.0909 0.047 Uiso 1 1 calc R U . . .
H2B H 0.3533 0.5714 -0.0165 0.047 Uiso 1 1 calc R U . . .
H2C H 0.4998 0.5818 -0.0898 0.047 Uiso 1 1 calc R U . . .
C3 C 1.1551(4) 0.8489(2) 0.10782(16) 0.0186(6) Uani 1 1 d . . . . .
C4 C 1.3053(5) 0.7670(3) 0.21603(18) 0.0316(8) Uani 1 1 d . . . . .
H4A H 1.2351 0.7630 0.2662 0.047 Uiso 1 1 calc R U . . .
H4B H 1.4492 0.7800 0.2264 0.047 Uiso 1 1 calc R U . . .
H4C H 1.2577 0.7011 0.1853 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8380(4) 1.0528(2) 0.16733(17) 0.0207(6) Uani 1 1 d . . . . .
C6 C 0.7101(5) 1.1333(3) 0.28671(17) 0.0307(8) Uani 1 1 d . . . . .
H6A H 0.5729 1.0932 0.2957 0.046 Uiso 1 1 calc R U . . .
H6B H 0.7233 1.2070 0.3010 0.046 Uiso 1 1 calc R U . . .
H6C H 0.8027 1.1071 0.3192 0.046 Uiso 1 1 calc R U . . .
Zn2 Zn 1.0000 0.5000 0.5000 0.01747(12) Uani 1 2 d S . P . .
N13 N 0.8311(3) 0.50480(17) 0.39214(13) 0.0183(5) Uani 1 1 d . . . . .
N14 N 0.7120(4) 0.41710(18) 0.35520(14) 0.0248(6) Uani 1 1 d . . . . .
N15 N 0.6352(4) 0.44197(18) 0.29116(14) 0.0251(6) Uani 1 1 d . . . . .
N16 N 0.7035(3) 0.54544(17) 0.28648(13) 0.0177(5) Uani 1 1 d . . . . .
N17 N 1.1270(3) 0.38388(17) 0.44124(13) 0.0198(5) Uani 1 1 d . . . . .
N18 N 1.2104(4) 0.31795(18) 0.48135(14) 0.0247(6) Uani 1 1 d . . . . .
N19 N 1.2696(4) 0.25569(19) 0.43246(14) 0.0252(6) Uani 1 1 d . . . . .
N20 N 1.2235(3) 0.28025(17) 0.35950(13) 0.0198(5) Uani 1 1 d . . . . .
N21 N 0.7636(3) 0.37881(17) 0.54310(13) 0.0182(5) Uani 1 1 d . . . . .
N22 N 0.6528(4) 0.39427(18) 0.60699(13) 0.0229(6) Uani 1 1 d . . . . .
N23 N 0.5300(3) 0.30677(18) 0.62324(14) 0.0230(6) Uani 1 1 d . . . . .
N24 N 0.5592(3) 0.23433(17) 0.57021(13) 0.0190(5) Uani 1 1 d . . . . .
C7 C 0.8230(4) 0.5825(2) 0.34792(16) 0.0176(6) Uani 1 1 d . . . . .
C8 C 0.6520(5) 0.6000(2) 0.21942(16) 0.0275(7) Uani 1 1 d . . . . .
H8A H 0.7026 0.6754 0.2294 0.041 Uiso 1 1 calc R U . . .
H8B H 0.5065 0.5825 0.2123 0.041 Uiso 1 1 calc R U . . .
H8C H 0.7124 0.5786 0.1716 0.041 Uiso 1 1 calc R U . . .
C9 C 1.1388(4) 0.3589(2) 0.36591(17) 0.0209(6) Uani 1 1 d . . . . .
C10 C 1.2677(4) 0.2219(2) 0.28951(17) 0.0269(7) Uani 1 1 d . . . . .
H10A H 1.1749 0.2254 0.2464 0.040 Uiso 1 1 calc R U . . .
H10B H 1.2526 0.1489 0.3020 0.040 Uiso 1 1 calc R U . . .
H10C H 1.4050 0.2524 0.2733 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7009(4) 0.2799(2) 0.52200(17) 0.0199(6) Uani 1 1 d . . . . .
C12 C 0.4429(5) 0.1262(2) 0.5707(2) 0.0322(8) Uani 1 1 d . . . . .
H12A H 0.3107 0.1199 0.5469 0.048 Uiso 1 1 calc R U . . .
H12B H 0.4279 0.1040 0.6252 0.048 Uiso 1 1 calc R U . . .
H12C H 0.5117 0.0820 0.5403 0.048 Uiso 1 1 calc R U . . .
O1 O -0.0253(3) 0.01039(16) 0.65243(13) 0.0351(6) Uani 1 1 d . . . . .
O2 O -0.0445(3) 0.16586(15) 0.62540(12) 0.0304(5) Uani 1 1 d . . . . .
O3 O 0.0981(3) 0.14068(16) 0.73463(12) 0.0308(5) Uani 1 1 d . . . . .
N25 N 0.0094(4) 0.10552(19) 0.67102(14) 0.0248(6) Uani 1 1 d . . . . .
O4 O 0.1446(4) 0.3631(2) 0.17093(15) 0.0597(8) Uani 1 1 d . . . . .
O5 O 0.0641(4) 0.49818(19) 0.21753(13) 0.0456(7) Uani 1 1 d . . . . .
O6 O 0.1539(4) 0.49117(19) 0.09681(13) 0.0473(7) Uani 1 1 d . . . . .
N26 N 0.1183(4) 0.4496(2) 0.16209(15) 0.0280(6) Uani 1 1 d . . . . .
O7 O 0.9215(4) 0.62746(19) 0.04857(16) 0.0377(6) Uani 1 1 d . . . . .
O8 O 0.8483(4) 0.09050(19) 0.46762(15) 0.0329(6) Uani 1 1 d . . . . .
H11 H 0.747(4) 0.244(2) 0.4786(16) 0.015(7) Uiso 1 1 d . . . . .
H7 H 0.888(4) 0.650(2) 0.3562(16) 0.017(7) Uiso 1 1 d . . . . .
H5 H 0.864(4) 1.003(2) 0.1917(17) 0.022(8) Uiso 1 1 d . . . . .
H3 H 1.091(4) 0.786(2) 0.0800(17) 0.024(8) Uiso 1 1 d . . . . .
H1 H 0.728(4) 0.778(2) -0.0970(18) 0.029(9) Uiso 1 1 d . . . . .
H9 H 1.106(4) 0.396(2) 0.3227(15) 0.012(7) Uiso 1 1 d . . . . .
H71 H 0.901(5) 0.605(3) 0.002(2) 0.041(11) Uiso 1 1 d . . . . .
H72 H 0.991(5) 0.590(3) 0.068(2) 0.046(12) Uiso 1 1 d . . . . .
H82 H 0.893(6) 0.103(3) 0.512(2) 0.055(13) Uiso 1 1 d . . . . .
H81 H 0.926(6) 0.057(3) 0.442(2) 0.066(13) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N5 2.139(2) . ?
Zn1 N5 2.139(2) 2_775 ?
Zn1 N1 2.166(2) . ?
Zn1 N1 2.166(2) 2_775 ?
Zn1 N9 2.185(2) 2_775 ?
Zn1 N9 2.185(2) . ?
N1 C1 1.301(4) . ?
N1 N2 1.357(3) . ?
N2 N3 1.281(4) . ?
N3 N4 1.346(3) . ?
N4 C1 1.317(4) . ?
N4 C2 1.456(4) . ?
N5 C3 1.314(3) . ?
N5 N6 1.366(3) . ?
N6 N7 1.300(3) . ?
N7 N8 1.345(3) . ?
N8 C3 1.324(4) . ?
N8 C4 1.452(3) . ?
N9 C5 1.314(3) . ?
N9 N10 1.364(3) . ?
N10 N11 1.291(3) . ?
N11 N12 1.349(3) . ?
N12 C5 1.326(3) . ?
N12 C6 1.464(3) . ?
C1 H1 0.85(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.94(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 0.85(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Zn2 N21 2.139(2) . ?
Zn2 N21 2.139(2) 2_766 ?
Zn2 N17 2.174(2) . ?
Zn2 N17 2.174(2) 2_766 ?
Zn2 N13 2.177(2) 2_766 ?
Zn2 N13 2.177(2) . ?
N13 C7 1.312(3) . ?
N13 N14 1.368(3) . ?
N14 N15 1.297(3) . ?
N15 N16 1.340(3) . ?
N16 C7 1.324(4) . ?
N16 C8 1.463(3) . ?
N17 C9 1.316(3) . ?
N17 N18 1.365(3) . ?
N18 N19 1.289(3) . ?
N19 N20 1.349(3) . ?
N20 C9 1.323(3) . ?
N20 C10 1.468(3) . ?
N21 C11 1.308(3) . ?
N21 N22 1.372(3) . ?
N22 N23 1.294(3) . ?
N23 N24 1.344(3) . ?
N24 C11 1.322(3) . ?
N24 C12 1.456(4) . ?
C7 H7 0.91(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.96(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.96(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O1 N25 1.250(3) . ?
O2 N25 1.257(3) . ?
O3 N25 1.250(3) . ?
O4 N26 1.222(3) . ?
O5 N26 1.233(3) . ?
O6 N26 1.256(3) . ?
O7 H71 0.83(4) . ?
O7 H72 0.85(3) . ?
O8 H82 0.80(4) . ?
O8 H81 0.88(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
N5 Zn1 N5 180.0 . 2_775 ?
N5 Zn1 N1 88.91(9) . . ?
N5 Zn1 N1 91.09(9) 2_775 . ?
N5 Zn1 N1 91.09(9) . 2_775 ?
N5 Zn1 N1 88.91(9) 2_775 2_775 ?
N1 Zn1 N1 180.0 . 2_775 ?
N5 Zn1 N9 91.77(8) . 2_775 ?
N5 Zn1 N9 88.23(8) 2_775 2_775 ?
N1 Zn1 N9 89.51(8) . 2_775 ?
N1 Zn1 N9 90.49(8) 2_775 2_775 ?
N5 Zn1 N9 88.23(8) . . ?
N5 Zn1 N9 91.77(8) 2_775 . ?
N1 Zn1 N9 90.49(8) . . ?
N1 Zn1 N9 89.51(8) 2_775 . ?
N9 Zn1 N9 180.0 2_775 . ?
C1 N1 N2 105.5(2) . . ?
C1 N1 Zn1 131.58(19) . . ?
N2 N1 Zn1 122.86(18) . . ?
N3 N2 N1 110.0(2) . . ?
N2 N3 N4 107.2(2) . . ?
C1 N4 N3 107.3(3) . . ?
C1 N4 C2 130.6(2) . . ?
N3 N4 C2 122.1(2) . . ?
C3 N5 N6 106.1(2) . . ?
C3 N5 Zn1 129.8(2) . . ?
N6 N5 Zn1 124.05(17) . . ?
N7 N6 N5 109.7(2) . . ?
N6 N7 N8 106.7(2) . . ?
C3 N8 N7 108.6(2) . . ?
C3 N8 C4 130.3(3) . . ?
N7 N8 C4 121.0(2) . . ?
C5 N9 N10 106.1(2) . . ?
C5 N9 Zn1 128.83(18) . . ?
N10 N9 Zn1 124.85(17) . . ?
N11 N10 N9 109.9(2) . . ?
N10 N11 N12 106.8(2) . . ?
C5 N12 N11 108.4(2) . . ?
C5 N12 C6 129.4(2) . . ?
N11 N12 C6 122.2(2) . . ?
N1 C1 N4 110.0(3) . . ?
N1 C1 H1 129(2) . . ?
N4 C1 H1 121(2) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 108.9(3) . . ?
N5 C3 H3 128.4(17) . . ?
N8 C3 H3 122.7(17) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C5 N12 108.7(3) . . ?
N9 C5 H5 129.3(18) . . ?
N12 C5 H5 121.8(18) . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N21 Zn2 N21 180.0 . 2_766 ?
N21 Zn2 N17 90.12(8) . . ?
N21 Zn2 N17 89.88(8) 2_766 . ?
N21 Zn2 N17 89.88(8) . 2_766 ?
N21 Zn2 N17 90.12(8) 2_766 2_766 ?
N17 Zn2 N17 180.00(10) . 2_766 ?
N21 Zn2 N13 88.55(9) . 2_766 ?
N21 Zn2 N13 91.46(9) 2_766 2_766 ?
N17 Zn2 N13 91.38(8) . 2_766 ?
N17 Zn2 N13 88.62(8) 2_766 2_766 ?
N21 Zn2 N13 91.45(9) . . ?
N21 Zn2 N13 88.54(8) 2_766 . ?
N17 Zn2 N13 88.62(8) . . ?
N17 Zn2 N13 91.38(8) 2_766 . ?
N13 Zn2 N13 180.0 2_766 . ?
C7 N13 N14 106.1(2) . . ?
C7 N13 Zn2 131.3(2) . . ?
N14 N13 Zn2 122.55(17) . . ?
N15 N14 N13 109.6(2) . . ?
N14 N15 N16 106.7(2) . . ?
C7 N16 N15 108.9(2) . . ?
C7 N16 C8 129.5(2) . . ?
N15 N16 C8 121.5(2) . . ?
C9 N17 N18 106.0(2) . . ?
C9 N17 Zn2 131.12(18) . . ?
N18 N17 Zn2 122.85(16) . . ?
N19 N18 N17 110.1(2) . . ?
N18 N19 N20 106.6(2) . . ?
C9 N20 N19 108.7(2) . . ?
C9 N20 C10 130.7(2) . . ?
N19 N20 C10 120.6(2) . . ?
C11 N21 N22 106.1(2) . . ?
C11 N21 Zn2 131.37(18) . . ?
N22 N21 Zn2 122.43(17) . . ?
N23 N22 N21 109.4(2) . . ?
N22 N23 N24 107.0(2) . . ?
C11 N24 N23 108.4(2) . . ?
C11 N24 C12 129.9(2) . . ?
N23 N24 C12 121.7(2) . . ?
N13 C7 N16 108.7(3) . . ?
N13 C7 H7 127.2(18) . . ?
N16 C7 H7 124.1(18) . . ?
N16 C8 H8A 109.5 . . ?
N16 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N16 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N17 C9 N20 108.6(2) . . ?
N17 C9 H9 125.9(15) . . ?
N20 C9 H9 125.1(14) . . ?
N20 C10 H10A 109.5 . . ?
N20 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N20 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N21 C11 N24 109.1(2) . . ?
N21 C11 H11 127.1(16) . . ?
N24 C11 H11 123.8(16) . . ?
N24 C12 H12A 109.5 . . ?
N24 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N24 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 N25 O1 120.2(2) . . ?
O3 N25 O2 120.0(2) . . ?
O1 N25 O2 119.8(3) . . ?
O4 N26 O5 120.6(3) . . ?
O4 N26 O6 119.8(3) . . ?
O5 N26 O6 119.5(3) . . ?
H71 O7 H72 105(3) . . ?
H82 O8 H81 107(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.3(3) . . . . ?
Zn1 N1 N2 N3 178.1(2) . . . . ?
N1 N2 N3 N4 0.0(3) . . . . ?
N2 N3 N4 C1 0.4(3) . . . . ?
N2 N3 N4 C2 -179.1(3) . . . . ?
C3 N5 N6 N7 -0.1(3) . . . . ?
Zn1 N5 N6 N7 176.57(15) . . . . ?
N5 N6 N7 N8 0.4(3) . . . . ?
N6 N7 N8 C3 -0.4(3) . . . . ?
N6 N7 N8 C4 -177.3(2) . . . . ?
C5 N9 N10 N11 0.6(3) . . . . ?
Zn1 N9 N10 N11 -174.3(2) . . . . ?
N9 N10 N11 N12 0.1(3) . . . . ?
N10 N11 N12 C5 -0.7(3) . . . . ?
N10 N11 N12 C6 179.7(3) . . . . ?
N2 N1 C1 N4 0.6(3) . . . . ?
Zn1 N1 C1 N4 -177.63(17) . . . . ?
N3 N4 C1 N1 -0.6(3) . . . . ?
C2 N4 C1 N1 178.8(3) . . . . ?
N6 N5 C3 N8 -0.1(3) . . . . ?
Zn1 N5 C3 N8 -176.59(16) . . . . ?
N7 N8 C3 N5 0.3(3) . . . . ?
C4 N8 C3 N5 176.9(2) . . . . ?
N10 N9 C5 N12 -1.0(3) . . . . ?
Zn1 N9 C5 N12 173.62(19) . . . . ?
N11 N12 C5 N9 1.0(3) . . . . ?
C6 N12 C5 N9 -179.3(3) . . . . ?
C7 N13 N14 N15 -0.2(3) . . . . ?
Zn2 N13 N14 N15 -177.72(16) . . . . ?
N13 N14 N15 N16 -0.2(3) . . . . ?
N14 N15 N16 C7 0.4(3) . . . . ?
N14 N15 N16 C8 177.8(2) . . . . ?
C9 N17 N18 N19 -0.2(3) . . . . ?
Zn2 N17 N18 N19 178.48(18) . . . . ?
N17 N18 N19 N20 -0.4(3) . . . . ?
N18 N19 N20 C9 0.9(3) . . . . ?
N18 N19 N20 C10 -178.7(2) . . . . ?
C11 N21 N22 N23 0.5(3) . . . . ?
Zn2 N21 N22 N23 -175.75(17) . . . . ?
N21 N22 N23 N24 -0.2(3) . . . . ?
N22 N23 N24 C11 -0.1(3) . . . . ?
N22 N23 N24 C12 -179.2(2) . . . . ?
N14 N13 C7 N16 0.4(3) . . . . ?
Zn2 N13 C7 N16 177.69(16) . . . . ?
N15 N16 C7 N13 -0.5(3) . . . . ?
C8 N16 C7 N13 -177.6(2) . . . . ?
N18 N17 C9 N20 0.7(3) . . . . ?
Zn2 N17 C9 N20 -177.79(18) . . . . ?
N19 N20 C9 N17 -1.0(3) . . . . ?
C10 N20 C9 N17 178.6(3) . . . . ?
N22 N21 C11 N24 -0.6(3) . . . . ?
Zn2 N21 C11 N24 175.22(18) . . . . ?
N23 N24 C11 N21 0.4(3) . . . . ?
C12 N24 C11 N21 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
O7 H71 O6 0.83(4) 2.04(4) 2.843(4) 162(3) 2_665
O7 H72 O6 0.85(3) 2.01(4) 2.850(4) 171(3) 1_655
O8 H82 O2 0.80(4) 2.07(4) 2.845(3) 163(4) 1_655
O8 H81 O1 0.88(4) 2.02(4) 2.846(3) 156(4) 2_656

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



_refine_diff_density_max         0.627
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.071

_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_lx236
_database_code_depnum_ccdc_archive 'CCDC 1566373'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue May 10 07:12:30 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrakis(1-methyltetrazolyl) bis(styphnato) manganese(II)
;
_chemical_name_common            
'tetrakis(1-methyltetrazolyl) bis(styphnato) manganese(II)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H20 Mn N22 O16'
_chemical_formula_sum            'C20 H20 Mn N22 O16'
_chemical_formula_weight         879.52

_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                   11.2818(4)
_cell_length_b                   9.0093(3)
_cell_length_c                   16.5990(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.382(4)
_cell_angle_gamma                90
_cell_volume                     1686.65(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3383
_cell_measurement_theta_min      4.5170
_cell_measurement_theta_max      30.4900

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.500
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_F_000             894
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            12905
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.142
_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 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3292
_reflns_number_gt                2692
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+3.4865P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3292
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1646
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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      -0.0552464000
_diffrn_orient_matrix_UB_12      -0.0050979000
_diffrn_orient_matrix_UB_13      0.0192964000
_diffrn_orient_matrix_UB_21      -0.0291614000
_diffrn_orient_matrix_UB_22      -0.0096574000
_diffrn_orient_matrix_UB_23      -0.0379951000
_diffrn_orient_matrix_UB_31      0.0072845000
_diffrn_orient_matrix_UB_32      -0.0779570000
_diffrn_orient_matrix_UB_33      0.0033788000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -111.00  -83.80   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega  -59.00   -7.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   38.0000   60.0000 65

#__ type_ start__ end____ width___ exp.time_
  3 omega   54.00   97.20   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
  4 omega  -16.20   75.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 114

#__ type_ start__ end____ width___ exp.time_
  5 omega  -41.00   41.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  150.0000 103

#__ type_ start__ end____ width___ exp.time_
  6 omega  -44.00   74.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000    0.0000 148

#__ type_ start__ end____ width___ exp.time_
  7 omega   72.00  112.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -180.0000 50

#__ type_ start__ end____ width___ exp.time_
  8 omega   84.00  108.80   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -90.0000 31

;



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
Mn1 Mn 0.0000 1.0000 0.0000 0.0209(2) Uani 1 2 d S . P . .
O1 O 0.3920(3) 1.1319(3) 0.1155(2) 0.0564(10) Uani 1 1 d . . . . .
O2 O 0.3288(2) 1.1505(3) -0.00720(16) 0.0347(6) Uani 1 1 d . . . . .
O3 O 0.1726(2) 0.9228(3) -0.03416(15) 0.0262(5) Uani 1 1 d . . . . .
O4 O 0.1658(3) 0.6606(3) -0.12938(16) 0.0435(7) Uani 1 1 d . . . . .
O5 O 0.1259(3) 0.5138(4) -0.0339(2) 0.0630(11) Uani 1 1 d . . . . .
O6 O 0.3463(3) 0.4622(3) 0.0256(2) 0.0484(8) Uani 1 1 d . . . . .
H6 H 0.3980 0.4234 0.0562 0.073 Uiso 1 1 calc R U . . .
O7 O 0.5196(2) 0.4618(3) 0.12542(17) 0.0392(7) Uani 1 1 d . . . . .
O8 O 0.6040(2) 0.6683(4) 0.16230(18) 0.0449(7) Uani 1 1 d . . . . .
N1 N 0.1816(3) 0.6160(3) -0.06153(18) 0.0266(6) Uani 1 1 d . . . . .
N2 N 0.3572(3) 1.0763(3) 0.05182(19) 0.0288(7) Uani 1 1 d . . . . .
N3 N 0.5248(3) 0.6004(4) 0.12562(18) 0.0316(7) Uani 1 1 d . . . . .
N4 N 0.0746(2) 1.1387(3) 0.10191(16) 0.0229(6) Uani 1 1 d . . . . .
N5 N 0.0682(3) 1.0914(3) 0.17931(18) 0.0332(7) Uani 1 1 d . . . . .
N6 N 0.1185(3) 1.1864(3) 0.22690(18) 0.0352(8) Uani 1 1 d . . . . .
N7 N 0.1575(2) 1.2979(3) 0.18080(16) 0.0226(6) Uani 1 1 d . . . . .
N8 N 0.0276(3) 1.1817(3) -0.08964(17) 0.0245(6) Uani 1 1 d . . . . .
N9 N -0.0646(3) 1.2607(4) -0.12189(19) 0.0327(7) Uani 1 1 d . . . . .
N10 N -0.0316(3) 1.3288(4) -0.18568(19) 0.0360(8) Uani 1 1 d . . . . .
N11 N 0.0830(3) 1.2933(3) -0.19610(17) 0.0265(6) Uani 1 1 d . . . . .
C1 C 0.3506(3) 0.6075(3) 0.03299(19) 0.0215(7) Uani 1 1 d . . . . .
C2 C 0.4351(3) 0.6822(4) 0.0820(2) 0.0235(7) Uani 1 1 d . . . . .
C3 C 0.4351(3) 0.8359(4) 0.0886(2) 0.0245(7) Uani 1 1 d . . . . .
H3 H 0.4923 0.8849 0.1221 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3506(3) 0.9164(4) 0.0459(2) 0.0225(7) Uani 1 1 d . . . . .
C5 C 0.2577(3) 0.8497(4) -0.00277(19) 0.0199(6) Uani 1 1 d . . . . .
C6 C 0.2685(3) 0.6929(4) -0.00964(19) 0.0212(7) Uani 1 1 d . . . . .
C7 C 0.1296(3) 1.2670(4) 0.1049(2) 0.0237(7) Uani 1 1 d . . . . .
H7 H 0.1465 1.3278 0.0599 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2292(3) 1.4181(4) 0.2149(2) 0.0318(8) Uani 1 1 d . . . . .
H8A H 0.3109 1.3836 0.2236 0.048 Uiso 1 1 calc R U . . .
H8B H 0.1965 1.4490 0.2664 0.048 Uiso 1 1 calc R U . . .
H8C H 0.2284 1.5024 0.1776 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1169(3) 1.2038(4) -0.1370(2) 0.0264(7) Uani 1 1 d . . . . .
H9 H 0.1938 1.1620 -0.1301 0.032 Uiso 1 1 calc R U . . .
C10 C 0.1471(4) 1.3544(5) -0.2643(2) 0.0392(9) Uani 1 1 d . . . . .
H10A H 0.2296 1.3203 -0.2616 0.059 Uiso 1 1 calc R U . . .
H10B H 0.1451 1.4630 -0.2621 0.059 Uiso 1 1 calc R U . . .
H10C H 0.1095 1.3206 -0.3149 0.059 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.157(2) . ?
Mn1 O3 2.157(2) 3_575 ?
Mn1 N8 2.239(3) 3_575 ?
Mn1 N8 2.239(3) . ?
Mn1 N4 2.250(3) . ?
Mn1 N4 2.250(3) 3_575 ?
O1 N2 1.226(4) . ?
O2 N2 1.222(4) . ?
O3 C5 1.266(4) . ?
O4 N1 1.205(4) . ?
O5 N1 1.212(4) . ?
O6 C1 1.316(4) . ?
O6 H6 0.8400 . ?
O7 N3 1.250(4) . ?
O8 N3 1.232(4) . ?
N1 C6 1.464(4) . ?
N2 C4 1.446(4) . ?
N3 C2 1.433(4) . ?
N4 C7 1.312(4) . ?
N4 N5 1.357(4) . ?
N5 N6 1.287(4) . ?
N6 N7 1.343(4) . ?
N7 C7 1.320(4) . ?
N7 C8 1.458(4) . ?
N8 C9 1.308(5) . ?
N8 N9 1.360(4) . ?
N9 N10 1.287(4) . ?
N10 N11 1.347(4) . ?
N11 C9 1.319(4) . ?
N11 C10 1.466(5) . ?
C1 C6 1.386(5) . ?
C1 C2 1.410(5) . ?
C2 C3 1.389(5) . ?
C3 C4 1.380(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.439(4) . ?
C5 C6 1.422(4) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O3 180.0 . 3_575 ?
O3 Mn1 N8 94.59(10) . 3_575 ?
O3 Mn1 N8 85.41(10) 3_575 3_575 ?
O3 Mn1 N8 85.41(10) . . ?
O3 Mn1 N8 94.59(10) 3_575 . ?
N8 Mn1 N8 180.0 3_575 . ?
O3 Mn1 N4 93.03(10) . . ?
O3 Mn1 N4 86.97(10) 3_575 . ?
N8 Mn1 N4 87.83(10) 3_575 . ?
N8 Mn1 N4 92.17(10) . . ?
O3 Mn1 N4 86.97(10) . 3_575 ?
O3 Mn1 N4 93.03(10) 3_575 3_575 ?
N8 Mn1 N4 92.17(10) 3_575 3_575 ?
N8 Mn1 N4 87.83(10) . 3_575 ?
N4 Mn1 N4 180.0 . 3_575 ?
C5 O3 Mn1 137.7(2) . . ?
C1 O6 H6 109.5 . . ?
O4 N1 O5 122.8(3) . . ?
O4 N1 C6 118.3(3) . . ?
O5 N1 C6 118.9(3) . . ?
O2 N2 O1 122.7(3) . . ?
O2 N2 C4 118.6(3) . . ?
O1 N2 C4 118.7(3) . . ?
O8 N3 O7 122.0(3) . . ?
O8 N3 C2 119.3(3) . . ?
O7 N3 C2 118.7(3) . . ?
C7 N4 N5 106.1(3) . . ?
C7 N4 Mn1 133.3(2) . . ?
N5 N4 Mn1 120.6(2) . . ?
N6 N5 N4 109.8(3) . . ?
N5 N6 N7 107.1(3) . . ?
C7 N7 N6 108.2(3) . . ?
C7 N7 C8 130.1(3) . . ?
N6 N7 C8 121.4(3) . . ?
C9 N8 N9 106.1(3) . . ?
C9 N8 Mn1 129.2(2) . . ?
N9 N8 Mn1 121.8(2) . . ?
N10 N9 N8 109.8(3) . . ?
N9 N10 N11 106.9(3) . . ?
C9 N11 N10 108.2(3) . . ?
C9 N11 C10 131.6(3) . . ?
N10 N11 C10 120.2(3) . . ?
O6 C1 C6 118.9(3) . . ?
O6 C1 C2 123.5(3) . . ?
C6 C1 C2 117.6(3) . . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 N3 118.3(3) . . ?
C1 C2 N3 120.3(3) . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 123.6(3) . . ?
C3 C4 N2 117.1(3) . . ?
C5 C4 N2 119.3(3) . . ?
O3 C5 C6 123.3(3) . . ?
O3 C5 C4 123.3(3) . . ?
C6 C5 C4 113.4(3) . . ?
C1 C6 C5 124.6(3) . . ?
C1 C6 N1 117.8(3) . . ?
C5 C6 N1 117.4(3) . . ?
N4 C7 N7 108.9(3) . . ?
N4 C7 H7 125.6 . . ?
N7 C7 H7 125.6 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N8 C9 N11 109.0(3) . . ?
N8 C9 H9 125.5 . . ?
N11 C9 H9 125.5 . . ?
N11 C10 H10A 109.5 . . ?
N11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N4 N5 N6 -0.8(4) . . . . ?
Mn1 N4 N5 N6 178.6(2) . . . . ?
N4 N5 N6 N7 0.5(4) . . . . ?
N5 N6 N7 C7 -0.1(4) . . . . ?
N5 N6 N7 C8 -174.0(3) . . . . ?
C9 N8 N9 N10 -0.7(4) . . . . ?
Mn1 N8 N9 N10 -162.9(3) . . . . ?
N8 N9 N10 N11 0.6(4) . . . . ?
N9 N10 N11 C9 -0.3(4) . . . . ?
N9 N10 N11 C10 -179.8(3) . . . . ?
O6 C1 C2 C3 -179.2(3) . . . . ?
C6 C1 C2 C3 1.1(5) . . . . ?
O6 C1 C2 N3 1.7(5) . . . . ?
C6 C1 C2 N3 -178.0(3) . . . . ?
O8 N3 C2 C3 -5.6(5) . . . . ?
O7 N3 C2 C3 174.1(3) . . . . ?
O8 N3 C2 C1 173.6(3) . . . . ?
O7 N3 C2 C1 -6.7(5) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
N3 C2 C3 C4 178.8(3) . . . . ?
C2 C3 C4 C5 3.2(5) . . . . ?
C2 C3 C4 N2 -177.4(3) . . . . ?
O2 N2 C4 C3 145.7(3) . . . . ?
O1 N2 C4 C3 -33.6(5) . . . . ?
O2 N2 C4 C5 -34.8(4) . . . . ?
O1 N2 C4 C5 145.9(4) . . . . ?
Mn1 O3 C5 C6 91.5(4) . . . . ?
Mn1 O3 C5 C4 -86.1(4) . . . . ?
C3 C4 C5 O3 171.4(3) . . . . ?
N2 C4 C5 O3 -8.0(5) . . . . ?
C3 C4 C5 C6 -6.4(5) . . . . ?
N2 C4 C5 C6 174.2(3) . . . . ?
O6 C1 C6 C5 175.3(3) . . . . ?
C2 C1 C6 C5 -5.0(5) . . . . ?
O6 C1 C6 N1 -0.6(5) . . . . ?
C2 C1 C6 N1 179.1(3) . . . . ?
O3 C5 C6 C1 -170.5(3) . . . . ?
C4 C5 C6 C1 7.3(5) . . . . ?
O3 C5 C6 N1 5.4(5) . . . . ?
C4 C5 C6 N1 -176.8(3) . . . . ?
O4 N1 C6 C1 -132.2(3) . . . . ?
O5 N1 C6 C1 50.3(5) . . . . ?
O4 N1 C6 C5 51.6(4) . . . . ?
O5 N1 C6 C5 -125.9(4) . . . . ?
N5 N4 C7 N7 0.7(4) . . . . ?
Mn1 N4 C7 N7 -178.6(2) . . . . ?
N6 N7 C7 N4 -0.4(4) . . . . ?
C8 N7 C7 N4 172.8(3) . . . . ?
N9 N8 C9 N11 0.5(4) . . . . ?
Mn1 N8 C9 N11 160.9(2) . . . . ?
N10 N11 C9 N8 -0.1(4) . . . . ?
C10 N11 C9 N8 179.3(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         2.482
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.088

_shelxl_version_number           2013-4


