# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

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

data_lx501
_audit_block_doi                 10.5517/ccdc.csd.cc2036fs
_database_code_depnum_ccdc_archive 'CCDC 1850124'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Oct 14 17:14:15 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(2-methyl-5-aminotetrazolyl) copper(II) diperchlorate hydrate
;
_chemical_name_common            
'diaqua tetrakis(2-methyl-5-aminotetrazolyl) copper(II) diperchlorate hydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C8 H24 Cu N20 O2, 2(Cl O4), H2 O'
_chemical_formula_sum            'C8 H26 Cl2 Cu N20 O11'
_chemical_formula_weight         712.93

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


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

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

_cell_length_a                   37.8504(12)
_cell_length_b                   18.5558(5)
_cell_length_c                   18.0159(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.272(3)
_cell_angle_gamma                90
_cell_volume                     11346.3(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5516
_cell_measurement_theta_min      4.2050
_cell_measurement_theta_max      24.7490

_exptl_crystal_description       block
_exptl_crystal_colour            blue

_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.043
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98424
_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    1.669
_exptl_crystal_F_000             5840
_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            46903
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.1941
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.107
_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             11093
_reflns_number_gt                7133
_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    SIR-92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'

_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)+(0.0556P)²+48.5550P] 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         11093
_refine_ls_number_parameters     815
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1680
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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      0.0078219000
_diffrn_orient_matrix_UB_12      0.0151245000
_diffrn_orient_matrix_UB_13      0.0188847000
_diffrn_orient_matrix_UB_21      -0.0027896000
_diffrn_orient_matrix_UB_22      0.0351001000
_diffrn_orient_matrix_UB_23      -0.0081870000
_diffrn_orient_matrix_UB_31      -0.0385117000
_diffrn_orient_matrix_UB_32      0.0005208000
_diffrn_orient_matrix_UB_33      0.0036290000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00   38.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  -60.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega   45.00   92.20   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
  3 omega    0.00  101.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  120.0000 127

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   96.20   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000   30.0000 124

#__ type_ start__ end____ width___ exp.time_
  5 omega   -9.00   19.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   77.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   64.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -150.0000 105

#__ type_ start__ end____ width___ exp.time_
  7 omega   47.00   74.20   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega  -24.00   15.20   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 49

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24835(2) 0.00148(3) 0.04287(4) 0.02370(17) Uani 1 1 d . . . . .
O2 O 0.18470(13) -0.0497(2) -0.0225(3) 0.0360(10) Uani 1 1 d . . . . .
O1 O 0.31454(13) 0.0514(3) 0.1049(3) 0.0336(10) Uani 1 1 d . . . . .
N4 N 0.26695(13) -0.0665(2) 0.1390(3) 0.0251(10) Uani 1 1 d . . . . .
N1 N 0.27444(15) -0.1342(2) 0.2470(3) 0.0349(11) Uani 1 1 d . . . . .
N3 N 0.30473(14) -0.0865(2) 0.1779(3) 0.0295(10) Uani 1 1 d . . . . .
N2 N 0.30789(15) -0.1249(2) 0.2400(3) 0.0341(11) Uani 1 1 d . . . . .
N14 N 0.22974(14) 0.0688(2) 0.1060(3) 0.0279(10) Uani 1 1 d . . . . .
N15 N 0.28672(15) 0.0976(3) 0.2302(3) 0.0405(12) Uani 1 1 d . . . . .
H15A H 0.2967 0.1198 0.2783 0.049 Uiso 1 1 calc R U . . .
H15B H 0.3024 0.0750 0.2135 0.049 Uiso 1 1 calc R U . . .
N11 N 0.22163(15) 0.1312(2) 0.2027(3) 0.0350(11) Uani 1 1 d . . . . .
N12 N 0.18806(14) 0.1183(2) 0.1364(3) 0.0322(11) Uani 1 1 d . . . . .
N13 N 0.19119(14) 0.0827(2) 0.0769(3) 0.0339(11) Uani 1 1 d . . . . .
N9 N 0.26684(13) -0.0658(2) -0.0199(3) 0.0246(9) Uani 1 1 d . . . . .
N10 N 0.30312(14) 0.0079(2) -0.0719(3) 0.0352(12) Uani 1 1 d . . . . .
H10A H 0.3154 0.0112 -0.1033 0.042 Uiso 1 1 calc R U . . .
H10B H 0.3006 0.0463 -0.0460 0.042 Uiso 1 1 calc R U . . .
N19 N 0.23054(13) 0.0703(2) -0.0527(3) 0.0261(10) Uani 1 1 d . . . . .
N7 N 0.26903(13) -0.1614(2) -0.0782(3) 0.0263(10) Uani 1 1 d . . . . .
N8 N 0.25515(13) -0.1339(2) -0.0306(3) 0.0251(10) Uani 1 1 d . . . . .
N18 N 0.24415(13) 0.1377(2) -0.0411(3) 0.0258(10) Uani 1 1 d . . . . .
N17 N 0.22968(13) 0.1661(2) -0.1136(3) 0.0271(10) Uani 1 1 d . . . . .
N5 N 0.21053(16) -0.0901(3) 0.1622(3) 0.0539(15) Uani 1 1 d . . . . .
H5A H 0.2006 -0.1111 0.1927 0.065 Uiso 1 1 calc R U . . .
H5B H 0.1952 -0.0646 0.1186 0.065 Uiso 1 1 calc R U . . .
N6 N 0.29046(14) -0.1163(2) -0.0997(3) 0.0297(10) Uani 1 1 d . . . . .
N20 N 0.19120(15) -0.0002(2) -0.1737(3) 0.0404(12) Uani 1 1 d . . . . .
H20A H 0.1784 -0.0018 -0.2280 0.048 Uiso 1 1 calc R U . . .
H20B H 0.1929 -0.0390 -0.1442 0.048 Uiso 1 1 calc R U . . .
N16 N 0.20686(13) 0.1225(2) -0.1763(3) 0.0284(10) Uani 1 1 d . . . . .
C6 C 0.14986(19) 0.1444(4) 0.1281(4) 0.0514(17) Uani 1 1 d . . . . .
H6A H 0.1460 0.1944 0.1088 0.077 Uiso 1 1 calc R U . . .
H6B H 0.1493 0.1418 0.1820 0.077 Uiso 1 1 calc R U . . .
H6C H 0.1287 0.1143 0.0881 0.077 Uiso 1 1 calc R U . . .
C5 C 0.24803(17) 0.0981(3) 0.1827(3) 0.0273(12) Uani 1 1 d . . . . .
C1 C 0.24869(18) -0.0968(3) 0.1822(3) 0.0297(12) Uani 1 1 d . . . . .
C2 C 0.34488(19) -0.1577(3) 0.2973(4) 0.0457(16) Uani 1 1 d . . . . .
H2A H 0.3439 -0.2097 0.2869 0.069 Uiso 1 1 calc R U . . .
H2B H 0.3490 -0.1492 0.3543 0.069 Uiso 1 1 calc R U . . .
H2C H 0.3666 -0.1364 0.2893 0.069 Uiso 1 1 calc R U . . .
C3 C 0.28815(16) -0.0559(3) -0.0635(3) 0.0268(11) Uani 1 1 d . . . . .
C4 C 0.2622(2) -0.2360(3) -0.1067(4) 0.0420(16) Uani 1 1 d . . . . .
H4A H 0.2478 -0.2612 -0.0808 0.063 Uiso 1 1 calc R U . . .
H4B H 0.2875 -0.2600 -0.0915 0.063 Uiso 1 1 calc R U . . .
H4C H 0.2467 -0.2370 -0.1670 0.063 Uiso 1 1 calc R U . . .
C7 C 0.20824(16) 0.0618(3) -0.1357(3) 0.0282(12) Uani 1 1 d . . . . .
C8 C 0.2382(2) 0.2398(3) -0.1285(4) 0.0395(15) Uani 1 1 d . . . . .
H8A H 0.2565 0.2619 -0.0760 0.059 Uiso 1 1 calc R U . . .
H8B H 0.2137 0.2677 -0.1526 0.059 Uiso 1 1 calc R U . . .
H8C H 0.2502 0.2395 -0.1669 0.059 Uiso 1 1 calc R U . . .
Cu2 Cu 0.0000 0.05620(4) 0.7500 0.0260(2) Uani 1 2 d S T P . .
O3 O 0.05709(14) 0.0577(2) 0.8835(3) 0.0373(10) Uani 1 1 d . . . . .
N22 N 0.07039(13) 0.1960(2) 0.7057(3) 0.0286(10) Uani 1 1 d . . . . .
N21 N 0.03836(14) 0.2339(2) 0.6595(3) 0.0329(11) Uani 1 1 d . . . . .
N25 N -0.02837(15) 0.2103(3) 0.6251(3) 0.0462(14) Uani 1 1 d . . . . .
H25A H -0.0363 0.2497 0.5950 0.055 Uiso 1 1 calc R U . . .
H25B H -0.0457 0.1814 0.6301 0.055 Uiso 1 1 calc R U . . .
N23 N 0.06386(13) 0.1362(2) 0.7357(3) 0.0287(10) Uani 1 1 d . . . . .
N24 N 0.02495(13) 0.1337(2) 0.7092(3) 0.0278(10) Uani 1 1 d . . . . .
N29 N -0.02256(13) -0.0222(2) 0.7944(3) 0.0271(10) Uani 1 1 d . . . . .
N30 N -0.06009(16) -0.0983(2) 0.6792(3) 0.0445(13) Uani 1 1 d . . . . .
H30A H -0.0724 -0.1396 0.6615 0.053 Uiso 1 1 calc R U . . .
H30B H -0.0587 -0.0673 0.6436 0.053 Uiso 1 1 calc R U . . .
N26 N -0.04387(14) -0.1263(2) 0.8191(3) 0.0326(11) Uani 1 1 d . . . . .
N28 N -0.00924(13) -0.0279(2) 0.8763(3) 0.0282(10) Uani 1 1 d . . . . .
N27 N -0.02209(13) -0.0898(2) 0.8880(3) 0.0276(10) Uani 1 1 d . . . . .
C11 C -0.04327(17) -0.0826(3) 0.7608(4) 0.0316(13) Uani 1 1 d . . . . .
C12 C -0.01307(19) -0.1182(3) 0.9695(3) 0.0363(14) Uani 1 1 d . . . . .
H12A H 0.0050 -0.1592 0.9814 0.055 Uiso 1 1 calc R U . . .
H12B H -0.0374 -0.1342 0.9709 0.055 Uiso 1 1 calc R U . . .
H12C H -0.0006 -0.0806 1.0112 0.055 Uiso 1 1 calc R U . . .
C9 C 0.01003(17) 0.1941(3) 0.6632(3) 0.0286(12) Uani 1 1 d . . . . .
C10 C 0.10991(18) 0.2186(3) 0.7207(4) 0.0397(15) Uani 1 1 d . . . . .
H10C H 0.1294 0.1948 0.7707 0.060 Uiso 1 1 calc R U . . .
H10D H 0.1123 0.2710 0.7283 0.060 Uiso 1 1 calc R U . . .
H10E H 0.1146 0.2052 0.6733 0.060 Uiso 1 1 calc R U . . .
Cu3 Cu 0.0000 0.44303(4) 0.2500 0.0227(2) Uani 1 2 d S T P . .
O4 O 0.06212(13) 0.4436(2) 0.2445(3) 0.0372(10) Uani 1 1 d . . . . .
N35 N -0.03624(16) 0.2897(3) 0.3078(4) 0.0524(15) Uani 1 1 d . . . . .
H35A H -0.0458 0.2510 0.3205 0.063 Uiso 1 1 calc R U . . .
H35B H -0.0518 0.3179 0.2671 0.063 Uiso 1 1 calc R U . . .
N34 N 0.01959(13) 0.3655(2) 0.3373(3) 0.0247(9) Uani 1 1 d . . . . .
N33 N 0.05745(14) 0.3626(2) 0.3927(3) 0.0286(10) Uani 1 1 d . . . . .
N32 N 0.06087(14) 0.3041(2) 0.4350(3) 0.0319(11) Uani 1 1 d . . . . .
N31 N 0.02785(15) 0.2667(2) 0.4125(3) 0.0350(11) Uani 1 1 d . . . . .
N40 N -0.05810(15) 0.6004(2) 0.2038(3) 0.0405(13) Uani 1 1 d . . . . .
H40A H -0.0697 0.6425 0.1980 0.049 Uiso 1 1 calc R U . . .
H40B H -0.0584 0.5693 0.2404 0.049 Uiso 1 1 calc R U . . .
N39 N -0.01982(13) 0.5214(2) 0.1632(3) 0.0244(9) Uani 1 1 d . . . . .
N38 N -0.00515(14) 0.5255(2) 0.1084(3) 0.0266(10) Uani 1 1 d . . . . .
N37 N -0.01613(13) 0.5883(2) 0.0734(3) 0.0268(10) Uani 1 1 d . . . . .
N36 N -0.03821(14) 0.6272(2) 0.0999(3) 0.0303(10) Uani 1 1 d . . . . .
C14 C 0.0977(2) 0.2826(4) 0.5051(4) 0.0481(16) Uani 1 1 d . . . . .
H14A H 0.1199 0.3053 0.5003 0.072 Uiso 1 1 calc R U . . .
H14B H 0.1004 0.2300 0.5052 0.072 Uiso 1 1 calc R U . . .
H14C H 0.0973 0.2979 0.5568 0.072 Uiso 1 1 calc R U . . .
C13 C 0.00199(18) 0.3058(3) 0.3502(3) 0.0291(12) Uani 1 1 d . . . . .
C15 C -0.03996(16) 0.5834(3) 0.1566(3) 0.0276(12) Uani 1 1 d . . . . .
C16 C -0.0044(2) 0.6165(3) 0.0116(4) 0.0414(15) Uani 1 1 d . . . . .
H16A H 0.0112 0.5802 -0.0002 0.062 Uiso 1 1 calc R U . . .
H16B H 0.0114 0.6602 0.0330 0.062 Uiso 1 1 calc R U . . .
H16C H -0.0280 0.6280 -0.0394 0.062 Uiso 1 1 calc R U . . .
Cl1 Cl 0.10541(5) 0.52754(10) 0.11442(12) 0.0573(5) Uani 1 1 d . . . . .
O10 O 0.08132(15) 0.4670(3) 0.1105(3) 0.0672(15) Uani 1 1 d . . . . .
O9 O 0.14558(15) 0.5081(3) 0.1605(3) 0.0683(14) Uani 1 1 d . . . . .
O8 O 0.1011(2) 0.5405(4) 0.0328(4) 0.119(3) Uani 1 1 d . . . . .
O7 O 0.0945(2) 0.5853(4) 0.1459(5) 0.119(3) Uani 1 1 d . . . . .
Cl2 Cl 0.10110(4) 0.05066(8) 0.57413(9) 0.0389(3) Uani 1 1 d . . . . .
O14 O 0.07553(14) -0.0100(2) 0.5519(3) 0.0609(13) Uani 1 1 d . . . . .
O13 O 0.1303(2) 0.0447(3) 0.6555(4) 0.105(2) Uani 1 1 d . . . . .
O12 O 0.1178(2) 0.0542(4) 0.5191(4) 0.115(3) Uani 1 1 d . . . . .
O20A O 0.3501(7) 0.1810(7) 0.1166(6) 0.102(5) Uani 0.78(4) 1 d . . P A 1
O21A O 0.3920(3) 0.2510(6) 0.0845(18) 0.126(7) Uani 0.78(4) 1 d . . P A 1
O20B O 0.3652(7) 0.1800(14) 0.1145(16) 0.020(8) Uiso 0.22(4) 1 d . . P A 2
O21B O 0.3877(9) 0.2463(18) 0.0410(18) 0.048(10) Uiso 0.22(4) 1 d . . P A 2
O11 O 0.07969(19) 0.1143(3) 0.5668(4) 0.098(2) Uani 1 1 d . . . . .
Cl3 Cl 0.14839(4) 0.22850(8) 0.37554(10) 0.0414(4) Uani 1 1 d . . . . .
O18 O 0.15412(18) 0.1877(2) 0.4485(4) 0.0759(18) Uani 1 1 d . . . . .
O17 O 0.16353(18) 0.1878(3) 0.3295(3) 0.0785(17) Uani 1 1 d . . . . .
O16 O 0.16871(16) 0.2943(3) 0.4021(3) 0.0729(16) Uani 1 1 d . . . . .
O15 O 0.10754(15) 0.2421(3) 0.3301(4) 0.0867(19) Uani 1 1 d . . . . .
Cl4 Cl 0.35287(5) 0.22532(8) 0.05161(11) 0.0448(4) Uani 1 1 d . . . . .
O22 O 0.3360(2) 0.1870(4) -0.0224(4) 0.106(2) Uani 1 1 d . . . . .
O19 O 0.32905(15) 0.2852(3) 0.0493(4) 0.0792(17) Uani 1 1 d . . . . .
O5 O 0.13091(12) 0.4383(2) 0.3879(3) 0.0448(10) Uani 1 1 d . . . . .
H51 H 0.1272 0.4434 0.4313 0.054 Uiso 1 1 d R U . . .
H52 H 0.1452 0.4027 0.4002 0.054 Uiso 1 1 d R U . . .
O6 O 0.13034(15) 0.0723(3) 0.8935(4) 0.0489(12) Uani 1 1 d . . . . .
H42 H 0.0625(17) 0.452(3) 0.202(4) 0.026(17) Uiso 1 1 d . . . . .
H11 H 0.3246(18) 0.088(3) 0.107(4) 0.034(19) Uiso 1 1 d . . . . .
H21 H 0.1768(17) -0.092(3) -0.032(3) 0.028(16) Uiso 1 1 d . . . . .
H32 H 0.0577(18) 0.043(3) 0.928(4) 0.035(18) Uiso 1 1 d . . . . .
H62 H 0.1384(19) 0.107(3) 0.923(4) 0.03(2) Uiso 1 1 d . . . . .
H12 H 0.329(2) 0.024(4) 0.112(4) 0.04(2) Uiso 1 1 d . . . . .
H31 H 0.079(2) 0.059(4) 0.889(4) 0.06(2) Uiso 1 1 d . . . . .
H61 H 0.120(3) 0.079(5) 0.846(6) 0.11(4) Uiso 1 1 d . . . . .
H41 H 0.085(3) 0.444(4) 0.288(5) 0.08(3) Uiso 1 1 d . . . . .
H22 H 0.163(2) -0.037(4) -0.035(4) 0.06(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
Cu1 N4 2.003(4) . ?
Cu1 N19 2.005(4) . ?
Cu1 N9 2.007(4) . ?
Cu1 N14 2.014(4) . ?
Cu1 O2 2.362(4) . ?
Cu1 O1 2.430(4) . ?
O2 H21 0.84(6) . ?
O2 H22 0.79(8) . ?
O1 H11 0.77(6) . ?
O1 H12 0.70(7) . ?
N4 N3 1.336(6) . ?
N4 C1 1.369(6) . ?
N1 C1 1.337(7) . ?
N1 N2 1.338(6) . ?
N3 N2 1.288(6) . ?
N2 C2 1.455(7) . ?
N14 N13 1.339(6) . ?
N14 C5 1.357(7) . ?
N15 C5 1.329(7) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N11 N12 1.325(6) . ?
N11 C5 1.351(7) . ?
N12 N13 1.308(6) . ?
N12 C6 1.468(7) . ?
N9 N8 1.326(5) . ?
N9 C3 1.364(6) . ?
N10 C3 1.350(6) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N19 N18 1.334(5) . ?
N19 C7 1.362(7) . ?
N7 N8 1.292(5) . ?
N7 N6 1.337(6) . ?
N7 C4 1.460(6) . ?
N18 N17 1.285(6) . ?
N17 N16 1.346(6) . ?
N17 C8 1.457(6) . ?
N5 C1 1.331(7) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 C3 1.318(6) . ?
N20 C7 1.347(7) . ?
N20 H20A 0.8800 . ?
N20 H20B 0.8800 . ?
N16 C7 1.332(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cu2 N29 2.023(4) 2_556 ?
Cu2 N29 2.023(4) . ?
Cu2 N24 2.028(4) . ?
Cu2 N24 2.028(4) 2_556 ?
Cu2 O3 2.419(4) 2_556 ?
Cu2 O3 2.419(4) . ?
O3 H32 0.84(6) . ?
O3 H31 0.81(8) . ?
N22 N23 1.306(6) . ?
N22 N21 1.328(6) . ?
N22 C10 1.459(7) . ?
N21 C9 1.328(7) . ?
N25 C9 1.338(7) . ?
N25 H25A 0.8800 . ?
N25 H25B 0.8800 . ?
N23 N24 1.333(6) . ?
N24 C9 1.361(6) . ?
N29 N28 1.336(6) . ?
N29 C11 1.348(6) . ?
N30 C11 1.351(7) . ?
N30 H30A 0.8800 . ?
N30 H30B 0.8800 . ?
N26 N27 1.331(6) . ?
N26 C11 1.335(7) . ?
N28 N27 1.299(6) . ?
N27 C12 1.452(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
Cu3 N34 2.016(4) 2 ?
Cu3 N34 2.016(4) . ?
Cu3 N39 2.020(4) 2 ?
Cu3 N39 2.020(4) . ?
Cu3 O4 2.397(4) 2 ?
Cu3 O4 2.397(4) . ?
O4 H42 0.78(6) . ?
O4 H41 0.87(9) . ?
N35 C13 1.337(8) . ?
N35 H35A 0.8800 . ?
N35 H35B 0.8800 . ?
N34 N33 1.337(6) . ?
N34 C13 1.364(6) . ?
N33 N32 1.299(6) . ?
N32 N31 1.327(6) . ?
N32 C14 1.462(8) . ?
N31 C13 1.331(7) . ?
N40 C15 1.345(6) . ?
N40 H40A 0.8800 . ?
N40 H40B 0.8800 . ?
N39 N38 1.333(5) . ?
N39 C15 1.356(6) . ?
N38 N37 1.301(5) . ?
N37 N36 1.343(6) . ?
N37 C16 1.465(6) . ?
N36 C15 1.330(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
Cl1 O7 1.358(6) . ?
Cl1 O9 1.419(5) . ?
Cl1 O8 1.426(6) . ?
Cl1 O10 1.428(5) . ?
Cl2 O12 1.393(5) . ?
Cl2 O13 1.396(6) . ?
Cl2 O11 1.405(6) . ?
Cl2 O14 1.422(4) . ?
O20A Cl4 1.473(11) . ?
O21A Cl4 1.412(9) . ?
O20B Cl4 1.32(3) . ?
O21B Cl4 1.47(3) . ?
Cl3 O16 1.408(5) . ?
Cl3 O15 1.416(5) . ?
Cl3 O17 1.417(5) . ?
Cl3 O18 1.447(5) . ?
Cl4 O22 1.391(6) . ?
Cl4 O19 1.420(5) . ?
O5 H51 0.8589 . ?
O5 H52 0.8208 . ?
O6 H62 0.80(6) . ?
O6 H61 0.78(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N19 179.13(18) . . ?
N4 Cu1 N9 91.08(16) . . ?
N19 Cu1 N9 88.89(17) . . ?
N4 Cu1 N14 88.82(16) . . ?
N19 Cu1 N14 91.20(17) . . ?
N9 Cu1 N14 179.87(18) . . ?
N4 Cu1 O2 93.94(17) . . ?
N19 Cu1 O2 86.93(17) . . ?
N9 Cu1 O2 90.13(16) . . ?
N14 Cu1 O2 89.78(17) . . ?
N4 Cu1 O1 86.94(17) . . ?
N19 Cu1 O1 92.19(17) . . ?
N9 Cu1 O1 87.17(17) . . ?
N14 Cu1 O1 92.92(18) . . ?
O2 Cu1 O1 177.18(16) . . ?
Cu1 O2 H21 132(4) . . ?
Cu1 O2 H22 137(5) . . ?
H21 O2 H22 90(6) . . ?
Cu1 O1 H11 138(5) . . ?
Cu1 O1 H12 111(5) . . ?
H11 O1 H12 107(7) . . ?
N3 N4 C1 106.4(4) . . ?
N3 N4 Cu1 120.8(3) . . ?
C1 N4 Cu1 132.6(4) . . ?
C1 N1 N2 101.8(4) . . ?
N2 N3 N4 105.9(4) . . ?
N3 N2 N1 115.2(5) . . ?
N3 N2 C2 122.6(5) . . ?
N1 N2 C2 122.2(4) . . ?
N13 N14 C5 107.3(4) . . ?
N13 N14 Cu1 119.5(3) . . ?
C5 N14 Cu1 132.5(4) . . ?
C5 N15 H15A 120.0 . . ?
C5 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
N12 N11 C5 101.8(4) . . ?
N13 N12 N11 115.6(4) . . ?
N13 N12 C6 121.7(5) . . ?
N11 N12 C6 122.7(5) . . ?
N12 N13 N14 104.8(4) . . ?
N8 N9 C3 106.8(4) . . ?
N8 N9 Cu1 119.9(3) . . ?
C3 N9 Cu1 133.1(3) . . ?
C3 N10 H10A 120.0 . . ?
C3 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
N18 N19 C7 106.8(4) . . ?
N18 N19 Cu1 120.2(3) . . ?
C7 N19 Cu1 132.7(3) . . ?
N8 N7 N6 114.9(4) . . ?
N8 N7 C4 123.2(4) . . ?
N6 N7 C4 121.9(4) . . ?
N7 N8 N9 105.4(4) . . ?
N17 N18 N19 105.3(4) . . ?
N18 N17 N16 115.6(4) . . ?
N18 N17 C8 122.8(5) . . ?
N16 N17 C8 121.5(4) . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C3 N6 N7 102.0(4) . . ?
C7 N20 H20A 120.0 . . ?
C7 N20 H20B 120.0 . . ?
H20A N20 H20B 120.0 . . ?
C7 N16 N17 101.1(4) . . ?
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 C5 N11 124.5(5) . . ?
N15 C5 N14 124.9(5) . . ?
N11 C5 N14 110.5(5) . . ?
N5 C1 N1 124.7(5) . . ?
N5 C1 N4 124.6(5) . . ?
N1 C1 N4 110.7(5) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N6 C3 N10 124.5(5) . . ?
N6 C3 N9 110.9(4) . . ?
N10 C3 N9 124.5(4) . . ?
N7 C4 H4A 109.5 . . ?
N7 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N7 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N16 C7 N20 123.3(5) . . ?
N16 C7 N19 111.1(4) . . ?
N20 C7 N19 125.6(5) . . ?
N17 C8 H8A 109.5 . . ?
N17 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N17 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N29 Cu2 N29 88.0(2) 2_556 . ?
N29 Cu2 N24 91.19(16) 2_556 . ?
N29 Cu2 N24 177.55(19) . . ?
N29 Cu2 N24 177.55(19) 2_556 2_556 ?
N29 Cu2 N24 91.19(16) . 2_556 ?
N24 Cu2 N24 89.7(2) . 2_556 ?
N29 Cu2 O3 87.85(18) 2_556 2_556 ?
N29 Cu2 O3 93.07(17) . 2_556 ?
N24 Cu2 O3 89.20(17) . 2_556 ?
N24 Cu2 O3 89.89(17) 2_556 2_556 ?
N29 Cu2 O3 93.07(17) 2_556 . ?
N29 Cu2 O3 87.86(18) . . ?
N24 Cu2 O3 89.89(17) . . ?
N24 Cu2 O3 89.20(17) 2_556 . ?
O3 Cu2 O3 178.7(2) 2_556 . ?
Cu2 O3 H32 126(4) . . ?
Cu2 O3 H31 123(5) . . ?
H32 O3 H31 108(7) . . ?
N23 N22 N21 115.0(4) . . ?
N23 N22 C10 122.3(5) . . ?
N21 N22 C10 122.8(4) . . ?
C9 N21 N22 102.0(4) . . ?
C9 N25 H25A 120.0 . . ?
C9 N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
N22 N23 N24 105.3(4) . . ?
N23 N24 C9 106.5(4) . . ?
N23 N24 Cu2 120.9(3) . . ?
C9 N24 Cu2 132.2(4) . . ?
N28 N29 C11 106.9(4) . . ?
N28 N29 Cu2 118.4(3) . . ?
C11 N29 Cu2 133.2(4) . . ?
C11 N30 H30A 120.0 . . ?
C11 N30 H30B 120.0 . . ?
H30A N30 H30B 120.0 . . ?
N27 N26 C11 101.9(4) . . ?
N27 N28 N29 105.3(4) . . ?
N28 N27 N26 114.9(4) . . ?
N28 N27 C12 123.2(4) . . ?
N26 N27 C12 121.9(4) . . ?
N26 C11 N29 111.1(5) . . ?
N26 C11 N30 124.2(5) . . ?
N29 C11 N30 124.6(5) . . ?
N27 C12 H12A 109.5 . . ?
N27 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N27 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N21 C9 N25 124.6(5) . . ?
N21 C9 N24 111.2(5) . . ?
N25 C9 N24 124.1(5) . . ?
N22 C10 H10C 109.5 . . ?
N22 C10 H10D 109.5 . . ?
H10C C10 H10D 109.5 . . ?
N22 C10 H10E 109.5 . . ?
H10C C10 H10E 109.5 . . ?
H10D C10 H10E 109.5 . . ?
N34 Cu3 N34 88.9(2) 2 . ?
N34 Cu3 N39 179.40(17) 2 2 ?
N34 Cu3 N39 91.59(16) . 2 ?
N34 Cu3 N39 91.59(16) 2 . ?
N34 Cu3 N39 179.40(17) . . ?
N39 Cu3 N39 88.0(2) 2 . ?
N34 Cu3 O4 90.40(17) 2 2 ?
N34 Cu3 O4 89.98(17) . 2 ?
N39 Cu3 O4 89.98(17) 2 2 ?
N39 Cu3 O4 89.63(16) . 2 ?
N34 Cu3 O4 89.98(17) 2 . ?
N34 Cu3 O4 90.40(17) . . ?
N39 Cu3 O4 89.63(16) 2 . ?
N39 Cu3 O4 89.99(17) . . ?
O4 Cu3 O4 179.5(2) 2 . ?
Cu3 O4 H42 119(4) . . ?
Cu3 O4 H41 125(5) . . ?
H42 O4 H41 116(7) . . ?
C13 N35 H35A 120.0 . . ?
C13 N35 H35B 120.0 . . ?
H35A N35 H35B 120.0 . . ?
N33 N34 C13 106.5(4) . . ?
N33 N34 Cu3 120.9(3) . . ?
C13 N34 Cu3 132.4(4) . . ?
N32 N33 N34 105.5(4) . . ?
N33 N32 N31 115.0(5) . . ?
N33 N32 C14 123.0(5) . . ?
N31 N32 C14 121.9(5) . . ?
N32 N31 C13 102.4(4) . . ?
C15 N40 H40A 120.0 . . ?
C15 N40 H40B 120.0 . . ?
H40A N40 H40B 120.0 . . ?
N38 N39 C15 106.7(4) . . ?
N38 N39 Cu3 118.8(3) . . ?
C15 N39 Cu3 132.9(3) . . ?
N37 N38 N39 105.2(4) . . ?
N38 N37 N36 115.1(4) . . ?
N38 N37 C16 123.3(4) . . ?
N36 N37 C16 121.6(4) . . ?
C15 N36 N37 101.2(4) . . ?
N32 C14 H14A 109.5 . . ?
N32 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N32 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N31 C13 N35 124.5(5) . . ?
N31 C13 N34 110.7(5) . . ?
N35 C13 N34 124.8(5) . . ?
N36 C15 N40 123.7(5) . . ?
N36 C15 N39 111.7(4) . . ?
N40 C15 N39 124.6(5) . . ?
N37 C16 H16A 109.5 . . ?
N37 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N37 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 Cl1 O9 113.6(4) . . ?
O7 Cl1 O8 112.3(5) . . ?
O9 Cl1 O8 104.5(4) . . ?
O7 Cl1 O10 109.6(4) . . ?
O9 Cl1 O10 108.9(3) . . ?
O8 Cl1 O10 107.6(4) . . ?
O12 Cl2 O13 110.7(5) . . ?
O12 Cl2 O11 108.5(5) . . ?
O13 Cl2 O11 108.7(4) . . ?
O12 Cl2 O14 107.6(3) . . ?
O13 Cl2 O14 110.9(3) . . ?
O11 Cl2 O14 110.3(4) . . ?
O16 Cl3 O15 109.5(3) . . ?
O16 Cl3 O17 111.0(4) . . ?
O15 Cl3 O17 112.2(4) . . ?
O16 Cl3 O18 107.7(3) . . ?
O15 Cl3 O18 107.7(4) . . ?
O17 Cl3 O18 108.5(3) . . ?
O20B Cl4 O22 109.6(12) . . ?
O22 Cl4 O21A 121.8(10) . . ?
O20B Cl4 O19 120.2(9) . . ?
O22 Cl4 O19 110.8(4) . . ?
O21A Cl4 O19 106.4(4) . . ?
O20B Cl4 O21B 106.5(15) . . ?
O22 Cl4 O21B 93.9(14) . . ?
O19 Cl4 O21B 112.6(13) . . ?
O22 Cl4 O20A 108.2(5) . . ?
O21A Cl4 O20A 106.5(8) . . ?
O19 Cl4 O20A 101.2(11) . . ?
H51 O5 H52 101.3 . . ?
H62 O6 H61 117(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 -0.8(5) . . . . ?
Cu1 N4 N3 N2 174.9(3) . . . . ?
N4 N3 N2 N1 0.7(6) . . . . ?
N4 N3 N2 C2 179.1(5) . . . . ?
C1 N1 N2 N3 -0.3(6) . . . . ?
C1 N1 N2 C2 -178.7(5) . . . . ?
C5 N11 N12 N13 -2.0(6) . . . . ?
C5 N11 N12 C6 -179.6(5) . . . . ?
N11 N12 N13 N14 1.7(6) . . . . ?
C6 N12 N13 N14 179.3(5) . . . . ?
C5 N14 N13 N12 -0.6(5) . . . . ?
Cu1 N14 N13 N12 170.8(3) . . . . ?
N6 N7 N8 N9 1.3(6) . . . . ?
C4 N7 N8 N9 -178.8(5) . . . . ?
C3 N9 N8 N7 -0.2(5) . . . . ?
Cu1 N9 N8 N7 174.9(3) . . . . ?
C7 N19 N18 N17 1.1(5) . . . . ?
Cu1 N19 N18 N17 175.6(3) . . . . ?
N19 N18 N17 N16 -0.6(6) . . . . ?
N19 N18 N17 C8 -178.6(5) . . . . ?
N8 N7 N6 C3 -1.9(6) . . . . ?
C4 N7 N6 C3 178.3(5) . . . . ?
N18 N17 N16 C7 -0.1(6) . . . . ?
C8 N17 N16 C7 177.9(5) . . . . ?
N12 N11 C5 N15 178.5(5) . . . . ?
N12 N11 C5 N14 1.5(5) . . . . ?
N13 N14 C5 N15 -177.5(5) . . . . ?
Cu1 N14 C5 N15 12.7(8) . . . . ?
N13 N14 C5 N11 -0.6(6) . . . . ?
Cu1 N14 C5 N11 -170.4(3) . . . . ?
N2 N1 C1 N5 179.7(5) . . . . ?
N2 N1 C1 N4 -0.2(5) . . . . ?
N3 N4 C1 N5 -179.2(5) . . . . ?
Cu1 N4 C1 N5 5.9(8) . . . . ?
N3 N4 C1 N1 0.6(6) . . . . ?
Cu1 N4 C1 N1 -174.3(3) . . . . ?
N7 N6 C3 N10 -175.2(5) . . . . ?
N7 N6 C3 N9 1.7(6) . . . . ?
N8 N9 C3 N6 -1.0(6) . . . . ?
Cu1 N9 C3 N6 -175.2(4) . . . . ?
N8 N9 C3 N10 175.8(5) . . . . ?
Cu1 N9 C3 N10 1.6(8) . . . . ?
N17 N16 C7 N20 -176.1(5) . . . . ?
N17 N16 C7 N19 0.8(6) . . . . ?
N18 N19 C7 N16 -1.2(6) . . . . ?
Cu1 N19 C7 N16 -174.8(4) . . . . ?
N18 N19 C7 N20 175.6(5) . . . . ?
Cu1 N19 C7 N20 2.0(9) . . . . ?
N23 N22 N21 C9 1.2(6) . . . . ?
C10 N22 N21 C9 -179.9(5) . . . . ?
N21 N22 N23 N24 -0.9(6) . . . . ?
C10 N22 N23 N24 -179.8(4) . . . . ?
N22 N23 N24 C9 0.2(5) . . . . ?
N22 N23 N24 Cu2 -172.9(3) . . . . ?
C11 N29 N28 N27 0.1(5) . . . . ?
Cu2 N29 N28 N27 -167.3(3) . . . . ?
N29 N28 N27 N26 -1.0(6) . . . . ?
N29 N28 N27 C12 177.9(5) . . . . ?
C11 N26 N27 N28 1.3(6) . . . . ?
C11 N26 N27 C12 -177.6(5) . . . . ?
N27 N26 C11 N29 -1.2(6) . . . . ?
N27 N26 C11 N30 176.6(5) . . . . ?
N28 N29 C11 N26 0.7(6) . . . . ?
Cu2 N29 C11 N26 165.5(4) . . . . ?
N28 N29 C11 N30 -177.1(5) . . . . ?
Cu2 N29 C11 N30 -12.3(9) . . . . ?
N22 N21 C9 N25 -179.6(5) . . . . ?
N22 N21 C9 N24 -1.0(6) . . . . ?
N23 N24 C9 N21 0.6(6) . . . . ?
Cu2 N24 C9 N21 172.5(4) . . . . ?
N23 N24 C9 N25 179.1(5) . . . . ?
Cu2 N24 C9 N25 -8.9(8) . . . . ?
C13 N34 N33 N32 -0.2(5) . . . . ?
Cu3 N34 N33 N32 -175.0(3) . . . . ?
N34 N33 N32 N31 -0.2(5) . . . . ?
N34 N33 N32 C14 -177.0(5) . . . . ?
N33 N32 N31 C13 0.6(6) . . . . ?
C14 N32 N31 C13 177.4(5) . . . . ?
C15 N39 N38 N37 1.1(5) . . . . ?
Cu3 N39 N38 N37 -166.3(3) . . . . ?
N39 N38 N37 N36 -1.2(6) . . . . ?
N39 N38 N37 C16 176.7(5) . . . . ?
N38 N37 N36 C15 0.7(6) . . . . ?
C16 N37 N36 C15 -177.2(5) . . . . ?
N32 N31 C13 N35 -178.9(5) . . . . ?
N32 N31 C13 N34 -0.7(5) . . . . ?
N33 N34 C13 N31 0.6(5) . . . . ?
Cu3 N34 C13 N31 174.6(3) . . . . ?
N33 N34 C13 N35 178.8(5) . . . . ?
Cu3 N34 C13 N35 -7.3(8) . . . . ?
N37 N36 C15 N40 177.3(5) . . . . ?
N37 N36 C15 N39 0.0(6) . . . . ?
N38 N39 C15 N36 -0.7(6) . . . . ?
Cu3 N39 C15 N36 164.2(4) . . . . ?
N38 N39 C15 N40 -178.0(5) . . . . ?
Cu3 N39 C15 N40 -13.1(8) . . . . ?

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

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

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



_refine_diff_density_max         1.238
_refine_diff_density_min         -0.495
_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_mx143
_audit_block_doi                 10.5517/ccdc.csd.cc2036dr
_database_code_depnum_ccdc_archive 'CCDC 1850123'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Mar 24 16:12:05 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(2-methyltetrazolyl) copper(II) diperchlorate
;
_chemical_name_common            
'diaqua tetrakis(2-methyltetrazolyl) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H20 Cl2 Cu N16 O10'
_chemical_formula_weight         634.84

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'




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

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

_cell_length_a                   7.9548(3)
_cell_length_b                   14.4157(6)
_cell_length_c                   10.8494(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.303(3)
_cell_angle_gamma                90
_cell_volume                     1238.82(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2318
_cell_measurement_theta_min      4.7030
_cell_measurement_theta_max      26.9430

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.175
_shelx_estimated_absorpt_T_min   0.712
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91989
_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    1.702
_exptl_crystal_F_000             646
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            9189
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.367
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2417
_reflns_number_gt                1935
_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    SIR-92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'

_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)+(0.0487P)²+1.3324P] 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         2417
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0116235000
_diffrn_orient_matrix_UB_12      0.0239400000
_diffrn_orient_matrix_UB_13      -0.0557110000
_diffrn_orient_matrix_UB_21      0.0041071000
_diffrn_orient_matrix_UB_22      -0.0429806000
_diffrn_orient_matrix_UB_23      -0.0313964000
_diffrn_orient_matrix_UB_31      -0.0886773000
_diffrn_orient_matrix_UB_32      0.0011692000
_diffrn_orient_matrix_UB_33      -0.0149008000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -89.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -19.0000  -30.0000 127

#__ type_ start__ end____ width___ exp.time_
  2 omega  -99.00  -28.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  120.0000 71

#__ type_ start__ end____ width___ exp.time_
  3 omega -109.00  -73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega  -87.00  -11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  131.0000  154.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000    0.0000 51

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.0000 1.0000 0.02329(17) Uani 1 2 d S . P . .
O1 O 0.3542(4) 0.13702(19) 1.0118(3) 0.0342(6) Uani 1 1 d . . . . .
N1 N 0.6507(4) 0.0163(2) 0.6442(3) 0.0337(7) Uani 1 1 d . . . . .
N2 N 0.5670(3) 0.09470(19) 0.6610(2) 0.0294(6) Uani 1 1 d . . . . .
N3 N 0.5265(3) 0.10774(19) 0.7736(2) 0.0305(6) Uani 1 1 d . . . . .
N4 N 0.5856(3) 0.03374(19) 0.8359(2) 0.0261(6) Uani 1 1 d . . . . .
N5 N 0.0401(3) -0.1137(2) 0.8505(3) 0.0343(7) Uani 1 1 d . . . . .
N6 N 0.1247(3) -0.0943(2) 0.7539(2) 0.0317(6) Uani 1 1 d . . . . .
N7 N 0.2739(3) -0.0586(2) 0.7817(2) 0.0323(6) Uani 1 1 d . . . . .
N8 N 0.2922(3) -0.05461(18) 0.9042(2) 0.0252(6) Uani 1 1 d . . . . .
C1 C 0.6605(4) -0.0203(3) 0.7562(3) 0.0317(7) Uani 1 1 d . . . . .
C2 C 0.5231(5) 0.1619(3) 0.5626(3) 0.0460(9) Uani 1 1 d . . . . .
H2A H 0.4080 0.1846 0.5687 0.069 Uiso 1 1 calc R U . . .
H2B H 0.5296 0.1322 0.4820 0.069 Uiso 1 1 calc R U . . .
H2C H 0.6021 0.2142 0.5711 0.069 Uiso 1 1 calc R U . . .
C3 C 0.1491(4) -0.0881(2) 0.9429(3) 0.0344(8) Uani 1 1 d . . . . .
C4 C 0.0535(5) -0.1089(3) 0.6261(3) 0.0530(11) Uani 1 1 d . . . . .
H4A H -0.0424 -0.0669 0.6073 0.079 Uiso 1 1 calc R U . . .
H4B H 0.0151 -0.1733 0.6157 0.079 Uiso 1 1 calc R U . . .
H4C H 0.1400 -0.0963 0.5696 0.079 Uiso 1 1 calc R U . . .
Cl1 Cl 0.52497(10) 0.30685(6) 0.24547(7) 0.0341(2) Uani 1 1 d . . . . .
O2 O 0.5101(4) 0.4006(2) 0.2832(3) 0.0679(9) Uani 1 1 d . . . . .
O3 O 0.6620(4) 0.2645(2) 0.3160(3) 0.0675(9) Uani 1 1 d . . . . .
O4 O 0.5464(6) 0.2968(3) 0.1201(3) 0.1000(14) Uani 1 1 d . . . . .
O5 O 0.3745(4) 0.2586(3) 0.2695(5) 0.1012(14) Uani 1 1 d . . . . .
H3 H 0.127(4) -0.091(3) 1.017(3) 0.033(10) Uiso 1 1 d . . . . .
H1 H 0.709(5) -0.080(3) 0.779(4) 0.055(12) Uiso 1 1 d . . . . .
H11 H 0.298(6) 0.153(3) 0.953(5) 0.057(14) Uiso 1 1 d . . . . .
H12 H 0.395(5) 0.174(3) 1.037(4) 0.037(14) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.024(2) 3_657 ?
Cu1 N4 2.024(3) . ?
Cu1 N8 2.028(2) . ?
Cu1 N8 2.028(2) 3_657 ?
Cu1 O1 2.300(3) . ?
Cu1 O1 2.300(3) 3_657 ?
O1 H11 0.78(5) . ?
O1 H12 0.67(4) . ?
N1 C1 1.320(4) . ?
N1 N2 1.333(4) . ?
N2 N3 1.305(4) . ?
N2 C2 1.460(4) . ?
N3 N4 1.325(4) . ?
N4 C1 1.343(4) . ?
N5 C3 1.316(4) . ?
N5 N6 1.326(4) . ?
N6 N7 1.303(4) . ?
N6 C4 1.465(4) . ?
N7 N8 1.325(3) . ?
N8 C3 1.339(4) . ?
C1 H1 0.97(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.84(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Cl1 O4 1.394(3) . ?
Cl1 O3 1.412(3) . ?
Cl1 O2 1.420(3) . ?
Cl1 O5 1.429(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N4 180.0 3_657 . ?
N4 Cu1 N8 91.88(10) 3_657 . ?
N4 Cu1 N8 88.12(10) . . ?
N4 Cu1 N8 88.12(10) 3_657 3_657 ?
N4 Cu1 N8 91.88(10) . 3_657 ?
N8 Cu1 N8 180.0 . 3_657 ?
N4 Cu1 O1 86.83(10) 3_657 . ?
N4 Cu1 O1 93.17(10) . . ?
N8 Cu1 O1 88.32(11) . . ?
N8 Cu1 O1 91.68(11) 3_657 . ?
N4 Cu1 O1 93.17(10) 3_657 3_657 ?
N4 Cu1 O1 86.83(10) . 3_657 ?
N8 Cu1 O1 91.68(11) . 3_657 ?
N8 Cu1 O1 88.32(11) 3_657 3_657 ?
O1 Cu1 O1 180.00(15) . 3_657 ?
Cu1 O1 H11 117(3) . . ?
Cu1 O1 H12 119(4) . . ?
H11 O1 H12 109(5) . . ?
C1 N1 N2 101.6(3) . . ?
N3 N2 N1 114.8(3) . . ?
N3 N2 C2 121.7(3) . . ?
N1 N2 C2 123.5(3) . . ?
N2 N3 N4 104.7(2) . . ?
N3 N4 C1 107.2(3) . . ?
N3 N4 Cu1 120.6(2) . . ?
C1 N4 Cu1 129.2(2) . . ?
C3 N5 N6 101.3(3) . . ?
N7 N6 N5 114.8(2) . . ?
N7 N6 C4 122.7(3) . . ?
N5 N6 C4 122.5(3) . . ?
N6 N7 N8 105.2(3) . . ?
N7 N8 C3 106.3(3) . . ?
N7 N8 Cu1 122.7(2) . . ?
C3 N8 Cu1 131.0(2) . . ?
N1 C1 N4 111.6(3) . . ?
N1 C1 H1 125(2) . . ?
N4 C1 H1 123(2) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 N8 112.4(3) . . ?
N5 C3 H3 122(2) . . ?
N8 C3 H3 126(2) . . ?
N6 C4 H4A 109.5 . . ?
N6 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N6 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O4 Cl1 O3 109.1(2) . . ?
O4 Cl1 O2 113.7(2) . . ?
O3 Cl1 O2 109.6(2) . . ?
O4 Cl1 O5 107.9(3) . . ?
O3 Cl1 O5 108.0(2) . . ?
O2 Cl1 O5 108.5(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.1(4) . . . . ?
C1 N1 N2 C2 179.9(3) . . . . ?
N1 N2 N3 N4 -0.3(3) . . . . ?
C2 N2 N3 N4 179.9(3) . . . . ?
N2 N3 N4 C1 0.4(3) . . . . ?
N2 N3 N4 Cu1 -161.97(19) . . . . ?
C3 N5 N6 N7 -0.6(4) . . . . ?
C3 N5 N6 C4 -178.5(3) . . . . ?
N5 N6 N7 N8 0.8(4) . . . . ?
C4 N6 N7 N8 178.7(3) . . . . ?
N6 N7 N8 C3 -0.6(3) . . . . ?
N6 N7 N8 Cu1 -177.75(19) . . . . ?
N2 N1 C1 N4 0.2(4) . . . . ?
N3 N4 C1 N1 -0.4(4) . . . . ?
Cu1 N4 C1 N1 160.0(2) . . . . ?
N6 N5 C3 N8 0.2(4) . . . . ?
N7 N8 C3 N5 0.2(4) . . . . ?
Cu1 N8 C3 N5 177.1(2) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H11 O3 0.78(5) 2.12(5) 2.875(4) 163(5) 4_566
O1 H12 O4 0.67(4) 2.27(4) 2.948(5) 177(5) 1_556

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



_refine_diff_density_max         0.788
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.075

_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_lx593
_audit_block_doi                 10.5517/ccdc.csd.cc2036bp
_database_code_depnum_ccdc_archive 'CCDC 1850121'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;

_vrf_PLAT094_lx593               
; 
PROBLEM: Ratio of Maximum / Minimum Residual Density ....    8.66 Report

RESPONSE: Remaining electron density of 3.24 must be caused by crystal defects. 
Potential missing atoms e.g. crystal water can be excluded by
too short distances and impossible H bridges
;

_vrf_PLAT097_lx593               
; 
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.24 eA-3

RESPONSE: Remaining electron density must be caused by crystal defects. 
Potential missing atoms e.g. crystal water can be excluded by
too short distances and impossible H bridges
;
_audit_creation_date             
;
'Wed Dec 07 16:35:59 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(2-methyl-5H-tetrazolyl) copper(II) diperchlorate
;
_chemical_name_common            
'diaqua tetrakis(2-methyl-5H-tetrazolyl) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C8 H24 Cu N20 O2, 2(Cl O4)'
_chemical_formula_sum            'C8 H24 Cl2 Cu N20 O10'
_chemical_formula_weight         694.91

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'




_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'

_cell_length_a                   7.8894(7)
_cell_length_b                   19.9150(15)
_cell_length_c                   8.3691(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.004(8)
_cell_angle_gamma                90
_cell_volume                     1290.75(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3068
_cell_measurement_theta_min      4.8060
_cell_measurement_theta_max      30.1130

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.140
_shelx_estimated_absorpt_T_min   0.553
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83925
_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    1.788
_exptl_crystal_F_000             710
_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            11360
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.446
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.725
_diffrn_reflns_point_group_measured_fraction_full 0.733
_reflns_number_total             4524
_reflns_number_gt                3937
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.416
_reflns_Friedel_fraction_max     0.438
_reflns_Friedel_fraction_full    0.456

_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    SIR-92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'

_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)+(0.0787P)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 
;
 Flack x determined using 993 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;

_refine_ls_abs_structure_Flack   0.025(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4524
_refine_ls_number_parameters     423
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1278
_refine_ls_wR_factor_gt          0.1189
_refine_ls_goodness_of_fit_ref   1.054
_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      0.0277972000
_diffrn_orient_matrix_UB_12      0.0247998000
_diffrn_orient_matrix_UB_13      0.0600505000
_diffrn_orient_matrix_UB_21      -0.0232755000
_diffrn_orient_matrix_UB_22      0.0255386000
_diffrn_orient_matrix_UB_23      -0.0592771000
_diffrn_orient_matrix_UB_31      -0.0841079000
_diffrn_orient_matrix_UB_32      0.0011584000
_diffrn_orient_matrix_UB_33      0.0182990000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -41.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  -57.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega   47.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494  -99.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
  3 omega   39.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494 -179.0000   90.0000 73

#__ type_ start__ end____ width___ exp.time_
  4 omega   49.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   38.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  5 omega   76.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega    6.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       29.9494   57.0000 -180.0000 92

#__ type_ start__ end____ width___ exp.time_
  7 omega  -62.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557 -179.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  8 omega  -81.00    0.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.8557  -77.0000 -120.0000 81

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu01 Cu 0.13544(9) 0.15135(4) 0.38178(8) 0.01489(17) Uani 1 1 d . . . . .
O1 O -0.1613(6) 0.1886(3) 0.3172(6) 0.0211(10) Uani 1 1 d . . . . .
O2 O 0.4300(6) 0.1146(3) 0.4426(7) 0.0220(10) Uani 1 1 d . . . . .
N1 N 0.0964(7) 0.1070(3) 0.1635(6) 0.0182(10) Uani 1 1 d . . . . .
N2 N 0.1607(7) 0.0456(3) 0.1638(6) 0.0193(10) Uani 1 1 d . . . . .
N3 N 0.1098(7) 0.0237(3) 0.0160(6) 0.0204(11) Uani 1 1 d . . . . .
N4 N 0.0134(7) 0.0667(3) -0.0847(6) 0.0250(12) Uani 1 1 d . . . . .
N5 N -0.0804(10) 0.1760(4) -0.0363(8) 0.0365(16) Uani 1 1 d D . . . .
N6 N 0.0516(6) 0.0668(3) 0.4826(6) 0.0178(10) Uani 1 1 d . . . . .
N7 N -0.1049(6) 0.0696(3) 0.5229(6) 0.0187(10) Uani 1 1 d . . . . .
N8 N -0.1351(6) 0.0098(3) 0.5713(6) 0.0188(11) Uani 1 1 d . . . . .
N9 N -0.0074(7) -0.0343(3) 0.5714(6) 0.0194(10) Uani 1 1 d . . . . .
N10 N 0.2670(7) -0.0205(3) 0.5013(8) 0.0253(12) Uani 1 1 d . . . . .
N11 N 0.1765(6) 0.1956(3) 0.6003(6) 0.0183(10) Uani 1 1 d . . . . .
N12 N 0.1120(7) 0.2567(3) 0.6037(6) 0.0193(10) Uani 1 1 d . . . . .
N13 N 0.1724(7) 0.2800(3) 0.7481(6) 0.0206(11) Uani 1 1 d . . . . .
N14 N 0.2749(7) 0.2370(3) 0.8459(6) 0.0258(12) Uani 1 1 d . . . . .
N15 N 0.3657(10) 0.1277(4) 0.7927(8) 0.0344(15) Uani 1 1 d D . . . .
N16 N 0.2160(6) 0.2372(3) 0.2798(6) 0.0166(10) Uani 1 1 d . . . . .
N17 N 0.3699(6) 0.2354(3) 0.2369(6) 0.0191(10) Uani 1 1 d . . . . .
N18 N 0.3964(6) 0.2962(3) 0.1912(6) 0.0180(10) Uani 1 1 d . . . . .
N19 N 0.2684(7) 0.3394(3) 0.1989(6) 0.0203(11) Uani 1 1 d . . . . .
N20 N -0.0022(7) 0.3224(3) 0.2754(7) 0.0244(12) Uani 1 1 d . . . . .
C1 C 0.0039(9) 0.1190(4) 0.0116(8) 0.0218(13) Uani 1 1 d . . . . .
C2 C 0.1457(10) -0.0452(4) -0.0294(8) 0.0306(15) Uani 1 1 d . . . . .
H2A H 0.2141 -0.0682 0.0649 0.046 Uiso 1 1 calc R U . . .
H2B H 0.2104 -0.0443 -0.1183 0.046 Uiso 1 1 calc R U . . .
H2C H 0.0365 -0.0692 -0.0649 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1081(8) 0.0026(3) 0.5132(7) 0.0181(12) Uani 1 1 d . . . . .
C4 C -0.2920(9) -0.0064(4) 0.6305(9) 0.0313(16) Uani 1 1 d . . . . .
H4A H -0.3695 0.0325 0.6155 0.047 Uiso 1 1 calc R U . . .
H4B H -0.2627 -0.0178 0.7464 0.047 Uiso 1 1 calc R U . . .
H4C H -0.3495 -0.0447 0.5695 0.047 Uiso 1 1 calc R U . . .
C5 C 0.2763(9) 0.1844(4) 0.7511(8) 0.0212(14) Uani 1 1 d . . . . .
C6 C 0.1411(10) 0.3487(4) 0.7916(9) 0.0349(17) Uani 1 1 d . . . . .
H6A H 0.2468 0.3751 0.7967 0.052 Uiso 1 1 calc R U . . .
H6B H 0.1067 0.3495 0.8981 0.052 Uiso 1 1 calc R U . . .
H6C H 0.0487 0.3680 0.7095 0.052 Uiso 1 1 calc R U . . .
C7 C 0.1564(8) 0.3009(3) 0.2561(7) 0.0164(12) Uani 1 1 d . . . . .
C8 C 0.5513(8) 0.3160(4) 0.1308(8) 0.0276(15) Uani 1 1 d . . . . .
H8A H 0.6343 0.2788 0.1460 0.041 Uiso 1 1 calc R U . . .
H8B H 0.6034 0.3554 0.1911 0.041 Uiso 1 1 calc R U . . .
H8C H 0.5200 0.3269 0.0147 0.041 Uiso 1 1 calc R U . . .
Cl1 Cl 0.61535(19) 0.01853(7) 0.13220(18) 0.0212(3) Uani 1 1 d . . . . .
O3 O 0.7985(6) 0.0063(3) 0.1614(7) 0.0384(13) Uani 1 1 d . . . . .
O4 O 0.5380(7) 0.0005(3) -0.0297(6) 0.0380(14) Uani 1 1 d . . . . .
O5 O 0.5832(7) 0.0897(3) 0.1540(6) 0.0334(12) Uani 1 1 d . . . . .
O6 O 0.5395(6) -0.0191(3) 0.2468(6) 0.0348(12) Uani 1 1 d . . . . .
Cl2 Cl 0.65263(19) 0.28914(8) 0.62640(18) 0.0227(3) Uani 1 1 d . . . . .
O7 O 0.4718(6) 0.3028(3) 0.5918(7) 0.0414(14) Uani 1 1 d . . . . .
O8 O 0.7264(7) 0.3063(3) 0.7905(6) 0.0402(14) Uani 1 1 d . . . . .
O9 O 0.7373(6) 0.3267(3) 0.5157(6) 0.0315(11) Uani 1 1 d . . . . .
O10 O 0.6803(7) 0.2178(3) 0.6023(6) 0.0328(11) Uani 1 1 d . . . . .
H20A H 0.006(8) 0.358(4) 0.303(8) 0.008(16) Uiso 1 1 d . . . . .
H12 H -0.22(2) 0.226(10) 0.327(17) 0.13(6) Uiso 1 1 d . . . . .
H20B H -0.043(9) 0.296(4) 0.345(8) 0.020(18) Uiso 1 1 d . . . . .
H5B H -0.143(12) 0.181(5) -0.127(11) 0.05(3) Uiso 1 1 d . . . . .
H5A H -0.089(11) 0.206(3) 0.027(8) 0.03(2) Uiso 1 1 d D . . . .
H11 H -0.225(13) 0.163(7) 0.253(12) 0.06(3) Uiso 1 1 d . . . . .
H21 H 0.449(11) 0.104(5) 0.352(11) 0.04(2) Uiso 1 1 d . . . . .
H22 H 0.489(11) 0.146(6) 0.478(10) 0.04(2) Uiso 1 1 d . . . . .
H10B H 0.281(11) -0.059(5) 0.502(10) 0.03(2) Uiso 1 1 d . . . . .
H10A H 0.312(8) -0.006(4) 0.443(8) 0.005(16) Uiso 1 1 d . . . . .
H15B H 0.421(8) 0.129(4) 0.883(4) 0.018(18) Uiso 1 1 d D . . . .
H15A H 0.374(10) 0.097(3) 0.734(8) 0.02(2) Uiso 1 1 d D . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu01 N1 1.999(5) . ?
Cu01 N11 2.000(5) . ?
Cu01 N6 2.048(5) . ?
Cu01 N16 2.065(5) . ?
Cu01 O2 2.396(5) . ?
Cu01 O1 2.417(5) . ?
O1 H12 0.89(18) . ?
O1 H11 0.83(12) . ?
O2 H21 0.83(9) . ?
O2 H22 0.80(11) . ?
N1 N2 1.323(7) . ?
N1 C1 1.361(8) . ?
N2 N3 1.302(7) . ?
N3 N4 1.333(8) . ?
N3 C2 1.465(9) . ?
N4 C1 1.328(9) . ?
N5 C1 1.338(9) . ?
N5 H5B 0.83(9) . ?
N5 H5A 0.80(2) . ?
N6 N7 1.342(7) . ?
N6 C3 1.362(8) . ?
N7 N8 1.296(8) . ?
N8 N9 1.337(7) . ?
N8 C4 1.454(8) . ?
N9 C3 1.333(8) . ?
N10 C3 1.357(8) . ?
N10 H10B 0.77(10) . ?
N10 H10A 0.71(7) . ?
N11 N12 1.322(8) . ?
N11 C5 1.373(8) . ?
N12 N13 1.298(7) . ?
N13 N14 1.344(8) . ?
N13 C6 1.448(9) . ?
N14 C5 1.315(9) . ?
N15 C5 1.342(9) . ?
N15 H15B 0.80(2) . ?
N15 H15A 0.80(2) . ?
N16 N17 1.331(7) . ?
N16 C7 1.353(8) . ?
N17 N18 1.298(8) . ?
N18 N19 1.337(7) . ?
N18 C8 1.463(8) . ?
N19 C7 1.326(8) . ?
N20 C7 1.361(8) . ?
N20 H20A 0.75(8) . ?
N20 H20B 0.88(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Cl1 O4 1.422(5) . ?
Cl1 O6 1.434(5) . ?
Cl1 O3 1.439(5) . ?
Cl1 O5 1.457(6) . ?
Cl2 O7 1.426(5) . ?
Cl2 O8 1.427(5) . ?
Cl2 O9 1.449(5) . ?
Cl2 O10 1.457(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 Cu01 N11 179.6(2) . . ?
N1 Cu01 N6 90.4(2) . . ?
N11 Cu01 N6 89.7(2) . . ?
N1 Cu01 N16 89.7(2) . . ?
N11 Cu01 N16 90.2(2) . . ?
N6 Cu01 N16 179.1(2) . . ?
N1 Cu01 O2 91.9(2) . . ?
N11 Cu01 O2 87.7(2) . . ?
N6 Cu01 O2 92.18(18) . . ?
N16 Cu01 O2 88.75(18) . . ?
N1 Cu01 O1 87.57(19) . . ?
N11 Cu01 O1 92.87(19) . . ?
N6 Cu01 O1 88.24(18) . . ?
N16 Cu01 O1 90.84(18) . . ?
O2 Cu01 O1 179.33(19) . . ?
Cu01 O1 H12 138(10) . . ?
Cu01 O1 H11 113(8) . . ?
H12 O1 H11 108(10) . . ?
Cu01 O2 H21 103(6) . . ?
Cu01 O2 H22 108(7) . . ?
H21 O2 H22 110(9) . . ?
N2 N1 C1 107.5(5) . . ?
N2 N1 Cu01 114.5(4) . . ?
C1 N1 Cu01 137.5(5) . . ?
N3 N2 N1 105.1(5) . . ?
N2 N3 N4 114.8(5) . . ?
N2 N3 C2 121.4(6) . . ?
N4 N3 C2 123.6(5) . . ?
C1 N4 N3 102.3(5) . . ?
C1 N5 H5B 124(7) . . ?
C1 N5 H5A 122(6) . . ?
H5B N5 H5A 113(9) . . ?
N7 N6 C3 105.9(5) . . ?
N7 N6 Cu01 117.0(4) . . ?
C3 N6 Cu01 136.8(4) . . ?
N8 N7 N6 105.9(5) . . ?
N7 N8 N9 114.9(5) . . ?
N7 N8 C4 121.9(6) . . ?
N9 N8 C4 123.1(6) . . ?
C3 N9 N8 101.8(5) . . ?
C3 N10 H10B 118(6) . . ?
C3 N10 H10A 120(5) . . ?
H10B N10 H10A 108(8) . . ?
N12 N11 C5 106.6(5) . . ?
N12 N11 Cu01 115.5(4) . . ?
C5 N11 Cu01 137.2(5) . . ?
N13 N12 N11 106.0(5) . . ?
N12 N13 N14 114.2(5) . . ?
N12 N13 C6 121.5(6) . . ?
N14 N13 C6 124.1(5) . . ?
C5 N14 N13 102.4(5) . . ?
C5 N15 H15B 113(6) . . ?
C5 N15 H15A 126(6) . . ?
H15B N15 H15A 120(8) . . ?
N17 N16 C7 107.1(5) . . ?
N17 N16 Cu01 117.3(4) . . ?
C7 N16 Cu01 135.3(4) . . ?
N18 N17 N16 105.1(5) . . ?
N17 N18 N19 114.8(5) . . ?
N17 N18 C8 123.0(5) . . ?
N19 N18 C8 122.1(5) . . ?
C7 N19 N18 101.9(5) . . ?
C7 N20 H20A 108(5) . . ?
C7 N20 H20B 110(5) . . ?
H20A N20 H20B 112(7) . . ?
N4 C1 N5 124.5(6) . . ?
N4 C1 N1 110.3(6) . . ?
N5 C1 N1 125.1(6) . . ?
N3 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N9 C3 N10 123.0(6) . . ?
N9 C3 N6 111.4(5) . . ?
N10 C3 N6 125.3(6) . . ?
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 . . ?
N14 C5 N15 125.3(6) . . ?
N14 C5 N11 110.9(6) . . ?
N15 C5 N11 123.8(6) . . ?
N13 C6 H6A 109.5 . . ?
N13 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N13 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N19 C7 N16 111.0(5) . . ?
N19 C7 N20 123.5(6) . . ?
N16 C7 N20 125.4(6) . . ?
N18 C8 H8A 109.5 . . ?
N18 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N18 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O4 Cl1 O6 110.3(3) . . ?
O4 Cl1 O3 110.7(4) . . ?
O6 Cl1 O3 109.4(3) . . ?
O4 Cl1 O5 108.2(3) . . ?
O6 Cl1 O5 108.6(3) . . ?
O3 Cl1 O5 109.7(3) . . ?
O7 Cl2 O8 111.0(4) . . ?
O7 Cl2 O9 109.7(3) . . ?
O8 Cl2 O9 109.8(3) . . ?
O7 Cl2 O10 109.1(3) . . ?
O8 Cl2 O10 108.8(3) . . ?
O9 Cl2 O10 108.3(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 1.2(6) . . . . ?
Cu01 N1 N2 N3 174.8(4) . . . . ?
N1 N2 N3 N4 -0.4(7) . . . . ?
N1 N2 N3 C2 -175.6(5) . . . . ?
N2 N3 N4 C1 -0.7(7) . . . . ?
C2 N3 N4 C1 174.4(6) . . . . ?
C3 N6 N7 N8 -0.8(6) . . . . ?
Cu01 N6 N7 N8 175.1(4) . . . . ?
N6 N7 N8 N9 1.6(7) . . . . ?
N6 N7 N8 C4 177.9(5) . . . . ?
N7 N8 N9 C3 -1.7(7) . . . . ?
C4 N8 N9 C3 -177.9(6) . . . . ?
C5 N11 N12 N13 0.6(6) . . . . ?
Cu01 N11 N12 N13 -171.2(4) . . . . ?
N11 N12 N13 N14 -0.7(7) . . . . ?
N11 N12 N13 C6 174.4(6) . . . . ?
N12 N13 N14 C5 0.6(7) . . . . ?
C6 N13 N14 C5 -174.4(6) . . . . ?
C7 N16 N17 N18 0.2(6) . . . . ?
Cu01 N16 N17 N18 -174.3(4) . . . . ?
N16 N17 N18 N19 -0.6(7) . . . . ?
N16 N17 N18 C8 -178.7(5) . . . . ?
N17 N18 N19 C7 0.7(7) . . . . ?
C8 N18 N19 C7 178.8(5) . . . . ?
N3 N4 C1 N5 179.5(7) . . . . ?
N3 N4 C1 N1 1.4(7) . . . . ?
N2 N1 C1 N4 -1.7(7) . . . . ?
Cu01 N1 C1 N4 -173.0(5) . . . . ?
N2 N1 C1 N5 -179.8(7) . . . . ?
Cu01 N1 C1 N5 9.0(11) . . . . ?
N8 N9 C3 N10 175.6(6) . . . . ?
N8 N9 C3 N6 1.1(6) . . . . ?
N7 N6 C3 N9 -0.2(7) . . . . ?
Cu01 N6 C3 N9 -174.9(4) . . . . ?
N7 N6 C3 N10 -174.6(6) . . . . ?
Cu01 N6 C3 N10 10.7(10) . . . . ?
N13 N14 C5 N15 178.2(7) . . . . ?
N13 N14 C5 N11 -0.2(7) . . . . ?
N12 N11 C5 N14 -0.2(7) . . . . ?
Cu01 N11 C5 N14 168.8(5) . . . . ?
N12 N11 C5 N15 -178.7(7) . . . . ?
Cu01 N11 C5 N15 -9.7(11) . . . . ?
N18 N19 C7 N16 -0.5(6) . . . . ?
N18 N19 C7 N20 -175.8(6) . . . . ?
N17 N16 C7 N19 0.2(7) . . . . ?
Cu01 N16 C7 N19 173.3(4) . . . . ?
N17 N16 C7 N20 175.4(6) . . . . ?
Cu01 N16 C7 N20 -11.5(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
N20 H20A N9 0.75(8) 2.39(8) 3.124(9) 170(7) 2_556
O1 H12 O10 0.89(18) 2.57(15) 2.955(7) 107(12) 1_455
O1 H12 O9 0.89(18) 2.61(18) 3.386(8) 146(12) 1_455
N20 H20B O1 0.88(8) 2.34(8) 2.993(8) 132(6) .
N20 H20B N12 0.88(8) 2.41(7) 3.020(8) 127(6) .
N20 H20B O9 0.88(8) 2.53(7) 3.139(7) 127(6) 1_455
N5 H5B O10 0.83(9) 2.53(9) 3.351(8) 171(9) 1_454
N5 H5A O1 0.80(2) 2.62(7) 3.153(9) 125(7) .
O1 H11 O5 0.83(12) 2.15(12) 2.960(8) 163(9) 1_455
O2 H21 O5 0.83(9) 2.15(9) 2.942(7) 160(8) .
O2 H22 O10 0.80(11) 2.19(10) 2.983(8) 169(10) .
N10 H10B O9 0.77(10) 2.29(10) 3.047(9) 168(9) 2_646
N10 H10A O2 0.71(7) 2.58(7) 3.062(9) 127(6) .
N10 H10A N2 0.71(7) 2.63(7) 3.084(8) 124(6) .
N10 H10A O6 0.71(7) 2.67(7) 3.303(8) 150(7) .
N15 H15B O5 0.80(2) 2.51(4) 3.268(8) 161(8) 1_556
N15 H15A O2 0.80(2) 2.58(7) 3.079(9) 121(7) .

_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         3.239
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.119

_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_mx046
_audit_block_doi                 10.5517/ccdc.csd.cc2036cq
_database_code_depnum_ccdc_archive 'CCDC 1850122'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_audit_creation_date             
;
'Tue Jan 31 19:31:47 2017'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua tetrakis(2-methyl--5-aminotetrazolyl) copper(II) diperchlorate
;
_chemical_name_common            
'diaqua tetrakis(2-methyl--5-aminotetrazolyl) copper(II) diperchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Cu N20 O2, C2 H5 N5, 2(Cl O4)'
_chemical_formula_sum            'C10 H29 Cl2 Cu N25 O10'
_chemical_formula_weight         794.02

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



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

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

_cell_length_a                   10.6159(6)
_cell_length_b                   10.7796(5)
_cell_length_c                   13.8295(7)
_cell_angle_alpha                89.498(4)
_cell_angle_beta                 80.568(4)
_cell_angle_gamma                83.990(4)
_cell_volume                     1552.55(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3185
_cell_measurement_theta_min      4.4110
_cell_measurement_theta_max      30.1910

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.964
_shelx_estimated_absorpt_T_min   0.688
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98531
_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    1.699
_exptl_crystal_F_000             814
_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            11962
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.172
_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             6072
_reflns_number_gt                4695
_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    SIR-92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+0.2238P] 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         6072
_refine_ls_number_parameters     494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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      0.0164428000
_diffrn_orient_matrix_UB_12      -0.0641714000
_diffrn_orient_matrix_UB_13      0.0085772000
_diffrn_orient_matrix_UB_21      0.0331174000
_diffrn_orient_matrix_UB_22      -0.0072550000
_diffrn_orient_matrix_UB_23      -0.0488307000
_diffrn_orient_matrix_UB_31      0.0571936000
_diffrn_orient_matrix_UB_32      0.0144012000
_diffrn_orient_matrix_UB_33      0.0156638000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -111.00  -84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -74.00  -29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000  150.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega   21.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000   60.0000 75

#__ type_ start__ end____ width___ exp.time_
  4 omega   34.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000    0.0000 51

#__ type_ start__ end____ width___ exp.time_
  5 omega  -22.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
  6 omega   -2.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
  7 omega   34.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000   30.0000 41

#__ type_ start__ end____ width___ exp.time_
  8 omega   33.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  150.0000 36

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu01 Cu 0.14013(3) 0.76213(3) 0.17295(2) 0.02070(10) Uani 1 1 d . . . . .
O1 O 0.2748(2) 0.8712(2) 0.05378(17) 0.0290(5) Uani 1 1 d . . . . .
O2 O 0.0197(2) 0.6455(2) 0.30887(16) 0.0286(5) Uani 1 1 d . . . . .
N1 N -0.0209(2) 0.8631(2) 0.14802(16) 0.0235(5) Uani 1 1 d . . . . .
N2 N -0.1237(2) 0.8002(2) 0.14797(16) 0.0256(5) Uani 1 1 d . . . . .
N3 N -0.2133(2) 0.8815(2) 0.12816(17) 0.0268(5) Uani 1 1 d . . . . .
N4 N -0.1799(2) 0.9971(2) 0.11558(18) 0.0312(6) Uani 1 1 d . . . . .
N5 N 0.0193(3) 1.0749(3) 0.1170(3) 0.0417(8) Uani 1 1 d . . . . .
N6 N 0.2860(2) 0.8957(2) 0.28910(16) 0.0228(5) Uani 1 1 d . . . . .
N7 N 0.1654(2) 0.8787(2) 0.27853(15) 0.0201(5) Uani 1 1 d . . . . .
N8 N 0.2742(2) 0.9578(2) 0.37032(16) 0.0236(5) Uani 1 1 d . . . . .
N9 N 0.1541(2) 0.9846(2) 0.41669(17) 0.0256(5) Uani 1 1 d . . . . .
N10 N -0.0415(2) 0.9371(3) 0.3727(2) 0.0285(6) Uani 1 1 d . . . . .
N11 N 0.1233(2) 0.6331(2) 0.07204(16) 0.0220(5) Uani 1 1 d . . . . .
N12 N 0.1420(2) 0.6581(2) -0.02374(16) 0.0254(5) Uani 1 1 d . . . . .
N13 N 0.1652(2) 0.5496(2) -0.06685(16) 0.0248(5) Uani 1 1 d . . . . .
N14 N 0.1626(2) 0.4518(2) -0.00801(17) 0.0285(5) Uani 1 1 d . . . . .
N15 N 0.1160(3) 0.4453(3) 0.1651(2) 0.0336(6) Uani 1 1 d . . . . .
N16 N 0.2947(2) 0.6533(2) 0.19994(15) 0.0200(5) Uani 1 1 d . . . . .
N17 N 0.4025(2) 0.5340(2) 0.28195(17) 0.0243(5) Uani 1 1 d . . . . .
N18 N 0.4751(2) 0.5287(2) 0.19378(17) 0.0258(5) Uani 1 1 d . . . . .
N19 N 0.2959(2) 0.6062(2) 0.28951(16) 0.0247(5) Uani 1 1 d . . . . .
N20 N 0.4328(3) 0.6285(3) 0.04645(19) 0.0311(6) Uani 1 1 d . . . . .
C1 C -0.0579(3) 0.9827(3) 0.1281(2) 0.0273(6) Uani 1 1 d . . . . .
C2 C -0.3426(3) 0.8493(3) 0.1226(2) 0.0399(8) Uani 1 1 d . . . . .
H2A H -0.3619 0.8665 0.0566 0.060 Uiso 1 1 calc R U . . .
H2B H -0.4052 0.8993 0.1706 0.060 Uiso 1 1 calc R U . . .
H2C H -0.3471 0.7605 0.1369 0.060 Uiso 1 1 calc R U . . .
C3 C 0.3855(3) 0.9919(3) 0.4094(2) 0.0343(7) Uani 1 1 d . . . . .
H3A H 0.4631 0.9725 0.3606 0.051 Uiso 1 1 calc R U . . .
H3B H 0.3940 0.9448 0.4693 0.051 Uiso 1 1 calc R U . . .
H3C H 0.3743 1.0814 0.4245 0.051 Uiso 1 1 calc R U . . .
C4 C 0.0869(3) 0.9329(2) 0.35729(19) 0.0221(6) Uani 1 1 d . . . . .
C5 C 0.4045(2) 0.6056(2) 0.1433(2) 0.0210(6) Uani 1 1 d . . . . .
C6 C 0.4378(3) 0.4615(3) 0.3650(2) 0.0371(8) Uani 1 1 d . . . . .
H6A H 0.3733 0.4824 0.4233 0.056 Uiso 1 1 calc R U . . .
H6B H 0.5218 0.4813 0.3772 0.056 Uiso 1 1 calc R U . . .
H6C H 0.4419 0.3723 0.3501 0.056 Uiso 1 1 calc R U . . .
C7 C 0.1977(3) 0.5341(3) -0.1732(2) 0.0350(7) Uani 1 1 d . . . . .
H7A H 0.1550 0.6043 -0.2051 0.053 Uiso 1 1 calc R U . . .
H7B H 0.1689 0.4560 -0.1928 0.053 Uiso 1 1 calc R U . . .
H7C H 0.2909 0.5316 -0.1930 0.053 Uiso 1 1 calc R U . . .
C8 C 0.1352(3) 0.5071(3) 0.0804(2) 0.0240(6) Uani 1 1 d . . . . .
N21 N 0.0909(3) 0.6772(3) 0.5054(2) 0.0430(7) Uani 1 1 d . . . . .
N22 N 0.2041(3) 0.7111(3) 0.5190(2) 0.0456(7) Uani 1 1 d . . . . .
N23 N 0.1858(3) 0.7520(2) 0.60934(19) 0.0360(6) Uani 1 1 d . . . . .
N24 N 0.0673(3) 0.7479(2) 0.65843(19) 0.0372(6) Uani 1 1 d . . . . .
N25 N -0.1137(3) 0.6731(3) 0.6058(3) 0.0452(8) Uani 1 1 d . . . . .
C9 C 0.0104(3) 0.7001(3) 0.5899(2) 0.0322(7) Uani 1 1 d . . . . .
C10 C 0.2866(3) 0.8058(4) 0.6509(3) 0.0485(9) Uani 1 1 d . . . . .
H10A H 0.3690 0.7874 0.6074 0.073 Uiso 1 1 calc R U . . .
H10B H 0.2925 0.7695 0.7155 0.073 Uiso 1 1 calc R U . . .
H10C H 0.2657 0.8963 0.6577 0.073 Uiso 1 1 calc R U . . .
Cl1 Cl 0.37251(7) 0.17469(7) 0.16341(5) 0.03044(17) Uani 1 1 d . . . . .
O3 O 0.4164(2) 0.0664(2) 0.10243(17) 0.0435(6) Uani 1 1 d . . . . .
O4 O 0.4510(3) 0.1811(3) 0.2358(2) 0.0794(10) Uani 1 1 d . . . . .
O5 O 0.2425(2) 0.1655(2) 0.2100(2) 0.0534(7) Uani 1 1 d . . . . .
O6 O 0.3753(3) 0.2841(2) 0.10585(19) 0.0574(7) Uani 1 1 d . . . . .
Cl2 Cl 0.33892(6) 0.26923(7) 0.60518(5) 0.02800(17) Uani 1 1 d . . . . .
O7 O 0.2366(3) 0.3645(3) 0.5955(2) 0.0788(9) Uani 1 1 d . . . . .
O8 O 0.4039(3) 0.3075(3) 0.6789(2) 0.0757(10) Uani 1 1 d . . . . .
O9 O 0.2899(2) 0.1536(2) 0.63382(17) 0.0463(6) Uani 1 1 d . . . . .
O10 O 0.4251(2) 0.2567(2) 0.51567(17) 0.0536(7) Uani 1 1 d . . . . .
H15B H 0.101(3) 0.483(3) 0.217(2) 0.027(9) Uiso 1 1 d . . . . .
H102 H -0.077(3) 0.957(3) 0.430(3) 0.031(9) Uiso 1 1 d . . . . .
H5A H 0.077(3) 1.069(3) 0.140(2) 0.020(9) Uiso 1 1 d . . . . .
H11 H 0.251(3) 0.894(3) 0.012(2) 0.014(8) Uiso 1 1 d . . . . .
H101 H -0.072(3) 0.887(3) 0.351(2) 0.022(9) Uiso 1 1 d . . . . .
H22 H 0.049(4) 0.644(4) 0.354(3) 0.057(14) Uiso 1 1 d . . . . .
H15A H 0.147(4) 0.368(4) 0.164(3) 0.053(11) Uiso 1 1 d . . . . .
H12 H 0.310(3) 0.928(3) 0.077(3) 0.049(11) Uiso 1 1 d . . . . .
H5B H -0.017(4) 1.144(4) 0.120(3) 0.063(14) Uiso 1 1 d . . . . .
H21 H -0.053(3) 0.633(3) 0.325(2) 0.031(9) Uiso 1 1 d . . . . .
H20A H 0.506(3) 0.610(3) 0.022(2) 0.024(8) Uiso 1 1 d . . . . .
H20B H 0.405(3) 0.694(3) 0.029(2) 0.027(9) Uiso 1 1 d . . . . .
H25A H -0.140(3) 0.659(3) 0.559(3) 0.041(12) Uiso 1 1 d . . . . .
H25B H -0.156(4) 0.715(3) 0.645(3) 0.042(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
Cu01 N16 2.000(2) . ?
Cu01 N7 2.003(2) . ?
Cu01 N1 2.006(2) . ?
Cu01 N11 2.020(2) . ?
Cu01 O1 2.385(2) . ?
O1 H11 0.71(3) . ?
O1 H12 0.84(4) . ?
O2 H22 0.74(4) . ?
O2 H21 0.79(3) . ?
N1 N2 1.343(3) . ?
N1 C1 1.347(3) . ?
N2 N3 1.286(3) . ?
N3 N4 1.333(3) . ?
N3 C2 1.464(3) . ?
N4 C1 1.328(4) . ?
N5 C1 1.346(4) . ?
N5 H5A 0.73(3) . ?
N5 H5B 0.80(4) . ?
N6 N8 1.294(3) . ?
N6 N7 1.343(3) . ?
N7 C4 1.354(3) . ?
N8 N9 1.333(3) . ?
N8 C3 1.459(3) . ?
N9 C4 1.334(3) . ?
N10 C4 1.340(4) . ?
N10 H102 0.84(3) . ?
N10 H101 0.74(3) . ?
N11 N12 1.336(3) . ?
N11 C8 1.357(3) . ?
N12 N13 1.299(3) . ?
N13 N14 1.326(3) . ?
N13 C7 1.461(3) . ?
N14 C8 1.340(3) . ?
N15 C8 1.340(4) . ?
N15 H15B 0.81(3) . ?
N15 H15A 0.87(4) . ?
N16 N19 1.336(3) . ?
N16 C5 1.349(3) . ?
N17 N19 1.295(3) . ?
N17 N18 1.329(3) . ?
N17 C6 1.460(3) . ?
N18 C5 1.329(3) . ?
N20 C5 1.350(4) . ?
N20 H20A 0.80(3) . ?
N20 H20B 0.79(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N21 N22 1.334(4) . ?
N21 C9 1.339(4) . ?
N22 N23 1.306(4) . ?
N23 N24 1.332(4) . ?
N23 C10 1.467(4) . ?
N24 C9 1.338(4) . ?
N25 C9 1.362(4) . ?
N25 H25A 0.77(4) . ?
N25 H25B 0.77(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Cl1 O4 1.410(3) . ?
Cl1 O6 1.417(2) . ?
Cl1 O5 1.437(2) . ?
Cl1 O3 1.437(2) . ?
Cl2 O8 1.408(2) . ?
Cl2 O10 1.412(2) . ?
Cl2 O9 1.429(2) . ?
Cl2 O7 1.437(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
N16 Cu01 N7 88.70(9) . . ?
N16 Cu01 N1 176.70(9) . . ?
N7 Cu01 N1 92.89(9) . . ?
N16 Cu01 N11 86.82(8) . . ?
N7 Cu01 N11 175.15(9) . . ?
N1 Cu01 N11 91.50(9) . . ?
N16 Cu01 O1 89.49(8) . . ?
N7 Cu01 O1 90.69(9) . . ?
N1 Cu01 O1 93.38(8) . . ?
N11 Cu01 O1 91.12(9) . . ?
Cu01 O1 H11 119(2) . . ?
Cu01 O1 H12 115(3) . . ?
H11 O1 H12 108(3) . . ?
H22 O2 H21 107(4) . . ?
N2 N1 C1 106.5(2) . . ?
N2 N1 Cu01 116.16(17) . . ?
C1 N1 Cu01 137.32(19) . . ?
N3 N2 N1 105.5(2) . . ?
N2 N3 N4 114.7(2) . . ?
N2 N3 C2 122.3(2) . . ?
N4 N3 C2 123.0(2) . . ?
C1 N4 N3 102.2(2) . . ?
C1 N5 H5A 119(2) . . ?
C1 N5 H5B 115(3) . . ?
H5A N5 H5B 114(4) . . ?
N8 N6 N7 105.0(2) . . ?
N6 N7 C4 106.8(2) . . ?
N6 N7 Cu01 118.34(17) . . ?
C4 N7 Cu01 133.73(17) . . ?
N6 N8 N9 115.4(2) . . ?
N6 N8 C3 121.8(2) . . ?
N9 N8 C3 122.8(2) . . ?
N8 N9 C4 101.9(2) . . ?
C4 N10 H102 115(2) . . ?
C4 N10 H101 119(2) . . ?
H102 N10 H101 113(3) . . ?
N12 N11 C8 106.9(2) . . ?
N12 N11 Cu01 121.51(17) . . ?
C8 N11 Cu01 128.20(18) . . ?
N13 N12 N11 104.9(2) . . ?
N12 N13 N14 115.8(2) . . ?
N12 N13 C7 123.0(2) . . ?
N14 N13 C7 121.2(2) . . ?
N13 N14 C8 101.5(2) . . ?
C8 N15 H15B 120(2) . . ?
C8 N15 H15A 117(3) . . ?
H15B N15 H15A 119(3) . . ?
N19 N16 C5 106.9(2) . . ?
N19 N16 Cu01 119.34(17) . . ?
C5 N16 Cu01 133.56(18) . . ?
N19 N17 N18 115.6(2) . . ?
N19 N17 C6 121.5(2) . . ?
N18 N17 C6 122.9(2) . . ?
C5 N18 N17 101.5(2) . . ?
N17 N19 N16 104.7(2) . . ?
C5 N20 H20A 116(2) . . ?
C5 N20 H20B 116(2) . . ?
H20A N20 H20B 112(3) . . ?
N4 C1 N5 123.8(3) . . ?
N4 C1 N1 111.0(2) . . ?
N5 C1 N1 125.0(3) . . ?
N3 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N8 C3 H3A 109.5 . . ?
N8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N9 C4 N10 124.2(3) . . ?
N9 C4 N7 110.9(2) . . ?
N10 C4 N7 124.8(2) . . ?
N18 C5 N16 111.3(2) . . ?
N18 C5 N20 125.4(3) . . ?
N16 C5 N20 123.2(3) . . ?
N17 C6 H6A 109.5 . . ?
N17 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N17 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N13 C7 H7A 109.5 . . ?
N13 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N13 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N15 C8 N14 124.1(3) . . ?
N15 C8 N11 124.9(3) . . ?
N14 C8 N11 110.9(2) . . ?
N22 N21 C9 106.6(3) . . ?
N23 N22 N21 105.2(3) . . ?
N22 N23 N24 115.1(3) . . ?
N22 N23 C10 121.9(3) . . ?
N24 N23 C10 122.8(3) . . ?
N23 N24 C9 100.8(2) . . ?
C9 N25 H25A 114(3) . . ?
C9 N25 H25B 113(3) . . ?
H25A N25 H25B 119(4) . . ?
N24 C9 N21 112.3(3) . . ?
N24 C9 N25 123.7(3) . . ?
N21 C9 N25 123.9(3) . . ?
N23 C10 H10A 109.5 . . ?
N23 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N23 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O4 Cl1 O6 109.95(18) . . ?
O4 Cl1 O5 109.30(18) . . ?
O6 Cl1 O5 108.64(16) . . ?
O4 Cl1 O3 109.76(18) . . ?
O6 Cl1 O3 110.20(15) . . ?
O5 Cl1 O3 108.97(14) . . ?
O8 Cl2 O10 109.10(18) . . ?
O8 Cl2 O9 108.38(15) . . ?
O10 Cl2 O9 111.25(15) . . ?
O8 Cl2 O7 107.9(2) . . ?
O10 Cl2 O7 109.08(17) . . ?
O9 Cl2 O7 111.06(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.5(3) . . . . ?
Cu01 N1 N2 N3 -178.28(16) . . . . ?
N1 N2 N3 N4 -0.8(3) . . . . ?
N1 N2 N3 C2 -179.2(2) . . . . ?
N2 N3 N4 C1 0.7(3) . . . . ?
C2 N3 N4 C1 179.1(3) . . . . ?
N8 N6 N7 C4 -0.4(3) . . . . ?
N8 N6 N7 Cu01 -170.14(16) . . . . ?
N7 N6 N8 N9 0.2(3) . . . . ?
N7 N6 N8 C3 178.2(2) . . . . ?
N6 N8 N9 C4 0.2(3) . . . . ?
C3 N8 N9 C4 -177.8(2) . . . . ?
C8 N11 N12 N13 -0.8(3) . . . . ?
Cu01 N11 N12 N13 159.92(16) . . . . ?
N11 N12 N13 N14 0.6(3) . . . . ?
N11 N12 N13 C7 -176.9(2) . . . . ?
N12 N13 N14 C8 -0.1(3) . . . . ?
C7 N13 N14 C8 177.4(2) . . . . ?
N19 N17 N18 C5 -0.2(3) . . . . ?
C6 N17 N18 C5 178.5(2) . . . . ?
N18 N17 N19 N16 0.5(3) . . . . ?
C6 N17 N19 N16 -178.2(2) . . . . ?
C5 N16 N19 N17 -0.6(3) . . . . ?
Cu01 N16 N19 N17 175.50(15) . . . . ?
N3 N4 C1 N5 176.3(3) . . . . ?
N3 N4 C1 N1 -0.4(3) . . . . ?
N2 N1 C1 N4 0.0(3) . . . . ?
Cu01 N1 C1 N4 178.3(2) . . . . ?
N2 N1 C1 N5 -176.7(3) . . . . ?
Cu01 N1 C1 N5 1.7(5) . . . . ?
N8 N9 C4 N10 -178.9(3) . . . . ?
N8 N9 C4 N7 -0.5(3) . . . . ?
N6 N7 C4 N9 0.6(3) . . . . ?
Cu01 N7 C4 N9 168.01(18) . . . . ?
N6 N7 C4 N10 179.0(3) . . . . ?
Cu01 N7 C4 N10 -13.5(4) . . . . ?
N17 N18 C5 N16 -0.2(3) . . . . ?
N17 N18 C5 N20 -176.4(3) . . . . ?
N19 N16 C5 N18 0.5(3) . . . . ?
Cu01 N16 C5 N18 -174.76(17) . . . . ?
N19 N16 C5 N20 176.8(2) . . . . ?
Cu01 N16 C5 N20 1.5(4) . . . . ?
N13 N14 C8 N15 176.6(3) . . . . ?
N13 N14 C8 N11 -0.4(3) . . . . ?
N12 N11 C8 N15 -176.2(3) . . . . ?
Cu01 N11 C8 N15 24.8(4) . . . . ?
N12 N11 C8 N14 0.8(3) . . . . ?
Cu01 N11 C8 N14 -158.23(18) . . . . ?
C9 N21 N22 N23 -0.1(3) . . . . ?
N21 N22 N23 N24 0.2(4) . . . . ?
N21 N22 N23 C10 -176.1(3) . . . . ?
N22 N23 N24 C9 -0.2(3) . . . . ?
C10 N23 N24 C9 176.1(3) . . . . ?
N23 N24 C9 N21 0.1(3) . . . . ?
N23 N24 C9 N25 177.5(3) . . . . ?
N22 N21 C9 N24 0.0(4) . . . . ?
N22 N21 C9 N25 -177.4(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
N15 H15B O2 0.81(3) 2.19(3) 2.933(4) 152(3) .
N10 H102 N9 0.84(3) 2.22(4) 3.052(4) 175(3) 2_576
N5 H5A O5 0.73(3) 2.47(3) 3.118(4) 150(3) 1_565
O1 H11 N4 0.71(3) 2.29(3) 2.989(3) 170(3) 2_575
N10 H101 O9 0.74(3) 2.38(3) 2.922(3) 131(3) 2_566
O2 H22 N21 0.74(4) 2.25(4) 2.969(4) 164(4) .
N15 H15A O5 0.87(4) 2.43(4) 3.268(4) 164(3) .
N15 H15A O6 0.87(4) 2.50(4) 3.091(4) 126(3) .
N15 H15A Cl1 0.87(4) 3.00(4) 3.774(3) 150(3) .
O1 H12 O3 0.84(4) 2.03(4) 2.855(3) 168(4) 1_565
O2 H21 O7 0.79(3) 2.08(4) 2.837(4) 162(3) 2_566
N20 H20A O6 0.80(3) 2.36(3) 2.905(4) 127(3) 2_665
N20 H20B O1 0.79(3) 2.23(3) 2.950(4) 152(3) .
N25 H25A O7 0.77(4) 2.54(4) 3.307(5) 174(4) 2_566
N25 H25B O5 0.77(4) 2.39(4) 3.135(5) 165(4) 2_566

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



_refine_diff_density_max         0.461
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4


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

data_lx621
_audit_block_doi                 10.5517/ccdc.csd.cc20369n
_database_code_depnum_ccdc_archive 'CCDC 1850120'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_audit_creation_date             
;
'Sat Dec 24 16:51:02 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
diaqua di(methylaminotetrazolyl) copper(II) perchlorate
;
_chemical_name_common            
'diaqua di(methylaminotetrazolyl) copper(II) perchlorate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H14 Cl2 Cu N10 O10'
_chemical_formula_sum            'C4 H14 Cl2 Cu N10 O10'
_chemical_formula_weight         496.69

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'




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

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

_cell_length_a                   7.0476(3)
_cell_length_b                   7.4569(3)
_cell_length_c                   15.8059(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.021(4)
_cell_angle_gamma                90
_cell_volume                     826.07(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2961
_cell_measurement_theta_min      4.5880
_cell_measurement_theta_max      31.8820

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.722
_shelx_estimated_absorpt_T_min   0.703
_shelx_estimated_absorpt_T_max   0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89755
_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    1.997
_exptl_crystal_F_000             502
_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            6210
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.289
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1617
_reflns_number_gt                1480
_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    SIR-92
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'

_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)+(0.0558P)²+1.3414P] 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         1617
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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      -0.0898641000
_diffrn_orient_matrix_UB_12      -0.0074059000
_diffrn_orient_matrix_UB_13      0.0161133000
_diffrn_orient_matrix_UB_21      -0.0459393000
_diffrn_orient_matrix_UB_22      0.0005483000
_diffrn_orient_matrix_UB_23      -0.0421209000
_diffrn_orient_matrix_UB_31      0.0066315000
_diffrn_orient_matrix_UB_32      -0.0948872000
_diffrn_orient_matrix_UB_33      -0.0014786000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -109.00  -37.00   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   90.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega -104.00  -72.80   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
  3 omega  -88.00  -46.40   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   30.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega -101.00    3.00   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000   60.0000 130

#__ type_ start__ end____ width___ exp.time_
  5 omega   18.00   74.80   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 71

#__ type_ start__ end____ width___ exp.time_
  6 omega   25.00   49.80   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
  7 omega  -44.00   92.00   0.8000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000 -120.0000 170

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu01 Cu 1.0000 0.0000 0.0000 0.0257(2) Uani 1 2 d S . P . .
Cl1 Cl 0.67515(10) 0.09043(9) 0.15074(5) 0.0253(2) Uani 1 1 d . . . . .
O2A O 0.5252(6) -0.0277(6) 0.1651(5) 0.064(3) Uani 0.635(15) 1 d . . P A 1
O4A O 0.7417(13) 0.1721(8) 0.2334(4) 0.063(2) Uani 0.635(15) 1 d . . P A 1
O2B O 0.5409(12) -0.005(2) 0.0872(11) 0.106(8) Uani 0.365(15) 1 d . . P A 2
O4B O 0.628(2) 0.098(3) 0.2266(7) 0.088(8) Uani 0.365(15) 1 d . . P A 2
O3 O 0.6296(5) 0.2389(4) 0.0969(2) 0.0601(9) Uani 1 1 d . . . . .
O5 O 0.8440(4) -0.0001(3) 0.13091(15) 0.0394(6) Uani 1 1 d . . . . .
O1 O 0.8018(4) 0.1365(4) -0.06849(15) 0.0278(5) Uani 1 1 d . . . . .
N1 N 1.2687(4) 0.4962(3) 0.04935(17) 0.0285(6) Uani 1 1 d . . . . .
N5 N 1.1667(5) 0.3985(5) -0.09026(18) 0.0331(7) Uani 1 1 d . . . . .
N4 N 1.1359(4) 0.2269(4) 0.03606(15) 0.0260(6) Uani 1 1 d . . . . .
N3 N 1.1795(4) 0.2579(4) 0.11918(16) 0.0290(6) Uani 1 1 d . . . . .
N2 N 1.2561(4) 0.4154(4) 0.12398(16) 0.0283(6) Uani 1 1 d . . . . .
C1 C 1.3228(6) 0.4998(5) 0.2053(2) 0.0411(9) Uani 1 1 d . . . . .
H1A H 1.2326 0.5935 0.2182 0.062 Uiso 1 1 calc R U . . .
H1B H 1.4487 0.5533 0.2017 0.062 Uiso 1 1 calc R U . . .
H1C H 1.3318 0.4092 0.2505 0.062 Uiso 1 1 calc R U . . .
C2 C 1.1927(4) 0.3736(4) -0.00564(19) 0.0259(6) Uani 1 1 d . . . . .
H5B H 1.218(6) 0.482(6) -0.107(3) 0.032(12) Uiso 1 1 d . . . . .
H12 H 0.782(8) 0.231(8) -0.051(3) 0.068(17) Uiso 1 1 d . . . . .
H11 H 0.712(6) 0.085(6) -0.081(3) 0.031(11) Uiso 1 1 d . . . . .
H5A H 1.158(5) 0.322(5) -0.113(2) 0.017(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
Cu01 O1 1.960(2) . ?
Cu01 O1 1.960(2) 3_755 ?
Cu01 N4 1.997(3) . ?
Cu01 N4 1.997(3) 3_755 ?
Cl1 O4B 1.278(8) . ?
Cl1 O2A 1.412(4) . ?
Cl1 O3 1.413(3) . ?
Cl1 O5 1.431(2) . ?
Cl1 O4A 1.473(5) . ?
Cl1 O2B 1.488(9) . ?
O1 H12 0.77(6) . ?
O1 H11 0.75(5) . ?
N1 C2 1.334(4) . ?
N1 N2 1.336(4) . ?
N5 C2 1.344(4) . ?
N5 H5B 0.78(4) . ?
N5 H5A 0.68(4) . ?
N4 N3 1.338(3) . ?
N4 C2 1.359(4) . ?
N3 N2 1.291(4) . ?
N2 C1 1.464(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 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 Cu01 O1 180.0 . 3_755 ?
O1 Cu01 N4 90.58(11) . . ?
O1 Cu01 N4 89.42(11) 3_755 . ?
O1 Cu01 N4 89.42(11) . 3_755 ?
O1 Cu01 N4 90.58(11) 3_755 3_755 ?
N4 Cu01 N4 180.0 . 3_755 ?
O4B Cl1 O3 117.7(7) . . ?
O2A Cl1 O3 117.3(3) . . ?
O4B Cl1 O5 122.0(5) . . ?
O2A Cl1 O5 113.2(3) . . ?
O3 Cl1 O5 112.29(16) . . ?
O2A Cl1 O4A 106.8(4) . . ?
O3 Cl1 O4A 104.0(3) . . ?
O5 Cl1 O4A 101.2(3) . . ?
O4B Cl1 O2B 116.6(10) . . ?
O3 Cl1 O2B 83.1(8) . . ?
O5 Cl1 O2B 96.3(4) . . ?
Cu01 O1 H12 115(4) . . ?
Cu01 O1 H11 115(3) . . ?
H12 O1 H11 113(5) . . ?
C2 N1 N2 101.9(3) . . ?
C2 N5 H5B 116(3) . . ?
C2 N5 H5A 114(3) . . ?
H5B N5 H5A 121(4) . . ?
N3 N4 C2 106.8(3) . . ?
N3 N4 Cu01 118.7(2) . . ?
C2 N4 Cu01 134.5(2) . . ?
N2 N3 N4 105.4(3) . . ?
N3 N2 N1 115.1(3) . . ?
N3 N2 C1 122.4(3) . . ?
N1 N2 C1 122.4(3) . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 N5 123.9(3) . . ?
N1 C2 N4 110.7(3) . . ?
N5 C2 N4 125.3(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
C2 N4 N3 N2 0.4(3) . . . . ?
Cu01 N4 N3 N2 -176.77(18) . . . . ?
N4 N3 N2 N1 0.0(3) . . . . ?
N4 N3 N2 C1 179.5(3) . . . . ?
C2 N1 N2 N3 -0.4(3) . . . . ?
C2 N1 N2 C1 -179.9(3) . . . . ?
N2 N1 C2 N5 177.0(3) . . . . ?
N2 N1 C2 N4 0.6(3) . . . . ?
N3 N4 C2 N1 -0.7(3) . . . . ?
Cu01 N4 C2 N1 175.9(2) . . . . ?
N3 N4 C2 N5 -177.0(3) . . . . ?
Cu01 N4 C2 N5 -0.5(5) . . . . ?

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

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1B O4A 0.98 2.47 3.374(9) 152.3 2_755
N5 H5B O3 0.78(4) 2.34(4) 3.068(6) 155(4) 3_765
O1 H12 N1 0.77(6) 2.07(6) 2.806(4) 160(5) 3_765
O1 H11 O2A 0.75(5) 2.07(5) 2.751(6) 152(4) 3_655
O1 H11 O2B 0.75(5) 1.88(5) 2.594(10) 161(4) 3_655
N5 H5A O4A 0.68(4) 2.56(4) 2.938(7) 118(3) 4_665
N5 H5A O5 0.68(4) 2.41(4) 3.039(5) 154(4) 3_755
C1 H1B O4A 0.98 2.47 3.374(9) 152.3 2_755
N5 H5B O3 0.78(4) 2.34(4) 3.068(6) 155(4) 3_765
O1 H12 N1 0.77(6) 2.07(6) 2.806(4) 160(5) 3_765
O1 H11 O2A 0.75(5) 2.07(5) 2.751(6) 152(4) 3_655
O1 H11 O2B 0.75(5) 1.88(5) 2.594(10) 161(4) 3_655
N5 H5A O4A 0.68(4) 2.56(4) 2.938(7) 118(3) 4_665
N5 H5A O5 0.68(4) 2.41(4) 3.039(5) 154(4) 3_755

_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         0.781
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.085

_shelxl_version_number           2013-4


