#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:39:13 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224820 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/79/7057985.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7057985
loop_
_publ_author_name
'Zeisel, Lukas'
'Szimhardt, Norbert'
'Wurzenberger, Maximilian H. H.'
'Klapötke, Thomas M.'
'Stierstorfer, Jörg'
_publ_section_title
;
 2-Methyl-substituted monotetrazoles in copper(ii) perchlorate complexes:
 manipulating coordination chemistry and derived energetic properties
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              609
_journal_paper_doi               10.1039/C8NJ05375H
_journal_volume                  43
_journal_year                    2019
_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
_chemical_name_common
'diaqua tetrakis(2-methyl-5-aminotetrazolyl) copper(II) diperchlorate hydrate'
_chemical_name_systematic
;
diaqua tetrakis(2-methyl-5-aminotetrazolyl) copper(II) diperchlorate hydrate
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2036fs
_audit_creation_date
;
'Fri Oct 14 17:14:15 2016'
;
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-11-20 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.272(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   37.8504(12)
_cell_length_b                   18.5558(5)
_cell_length_c                   18.0159(5)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.7490
_cell_measurement_theta_min      4.2050
_cell_volume                     11346.3(6)
_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_collection
;
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_molecular_graphics    'Diamond 2'
_computing_publication_material  'WINGX Version 2013.3'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_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_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.1941
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         4.107
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98424
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            blue
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             5840
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0556P)²+48.5550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7133
_reflns_number_total             11093
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj05375h2.cif
_cod_data_source_block           lx501
_cod_depositor_comments
'Adding full bibliography for 7057985--7057989.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7057985
_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.
;
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.859
_shelxl_version_number           2013-4
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'
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_
_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_
_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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
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)
