# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- Adamantane_CIF.cif'

# 1. SUBMISSION DETAILS

_publ_contact_author             
;
Konstantin V. Domasevitch
Inorganic Chemistry Department
Kiev Shevchenko University
Volodimirska Str. 64
01033 Kiev
Ukraine
;
_publ_contact_author_phone       ?
_publ_contact_author_fax         +380(44)296-2467
_publ_contact_author_email       dk@univ.kiev.ua
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
?
;

#------------------ TITLE AND AUTHOR LIST------------------------------------#

_publ_section_title              
;
1,2,4-Triazole functionalized adamantanes: A new library of polydentate
tectons for the designing structures of coordination polymers
;

loop_
_publ_author_name
_publ_author_address

'Senchyk, Ganna A.'
;
Inorganic Chemistry Department
National Taras Shevchenko University of Kyiv
Volodimirska Str. 64
Kyiv 01033
Ukraine
;
'Lysenko, Andrey B.'
;
Inorganic Chemistry Department
National Taras Shevchenko University of Kyiv
Volodimirska Str. 64
Kyiv 01033
Ukraine
;
'Boldog, Ishtvan'
;
Inorganic Chemistry Department
National Taras Shevchenko University of Kyiv
Volodimirska Str. 64
Kyiv 01033
Ukraine
;
'Rusanov, Eduard B.'
;
Istitute of Organic Chemistry
Murmans'ka Str. 4
Kyiv 253660
Ukraine
;
'Chernega, Alexander N.'
;
Istitute of Organic Chemistry
Murmans'ka Str. 4
Kyiv 253660
Ukraine
;
'Krautscheid, Harald'
;
Institute of Inorganic Chemistry
Leipzig University
Johannisallee 29
D-04103 Leipzig
Germany
;
'Domasevitch, Konstantin V.'
;
Inorganic Chemistry Department
National Taras Shevchenko University of Kyiv
Volodimirska Str. 64
Kyiv 01033
Ukraine
;

#------------------ TEXT ----------------------------------------------------#

_publ_section_abstract           
;

;

_publ_section_comment            
;

;

_publ_section_exptl_prep         
;

;

_publ_section_exptl_refinement   
;

;

_publ_section_references         
;

Farrugia, L. J. (1999). <i>WinGX</i>. <i>J. Appl. Cryst.</i> <b>32</b>,
837--838.

Sheldrick, G. M. (2008). <i>Acta Cryst.</i> A<b>64</b>, 112---122.

Stoe & Cie (1999). <i>X-SHAPE</i>. Revision 1.06. Stoe & Cie GmbH,
Darmstadt, Germany.

Stoe & Cie (2000). <i>IPDS Software</i>. Stoe & Cie GmbH, Darmstadt,
Germany.

Stoe & Cie (2001). <i>X-RED</i>. Version 1.22. Stoe & Cie GmbH,
Darmstadt,Germany.

;

_publ_section_figure_captions    
;

;

_publ_section_acknowledgements   
;

;

_publ_section_table_legends      
;

;

#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_(1)
_database_code_depnum_ccdc_archive 'CCDC 867224'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[1,3-di(1,2,4-triazol-4-yl)adamantane]diaquacadmium(II)
Tetrabromocadmate(II) Dihydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H80 Cd2 N24 O4, 2(Br4 Cd), 2(H2 O)'
_chemical_formula_sum            'C56 H84 Br8 Cd4 N24 O6'
_chemical_formula_weight         2278.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_symmetry_equiv_pos_as_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                   14.7635(12)
_cell_length_b                   29.457(3)
_cell_length_c                   17.5708(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.031(8)
_cell_angle_gamma                90.00
_cell_volume                     7641.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    31673
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      26.02

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4432
_exptl_absorpt_coefficient_mu    5.344
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3371
_exptl_absorpt_correction_T_max  0.4300
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31673
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.1434
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         26.02
_reflns_number_total             14439
_reflns_number_gt                8284
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Monoclinic crystals of (1), with beta nearly 90, exhibit common type of
pseudomerohedral twinning emulating orthorhombic P lattice.
In the latter case R(int) = 0.105, however no solution was possible in any
of the reasonable orthorhombic space groups (for example, Pmmn, Pmn21,
P212121, etc). The structure was successfully solved in the monoclinic
space group P21/n and refined as twin (the twin law 1 0 0 0 -1 0 0 0 -1)
with actually equal contributions of the twin components
(the refined BASF parameter was 0.565).

All non-hydrogen atoms were refined anisotropically. The CH-hydrogen atoms
were constrained with U(iso) = 1.2U(eq) of the parent C-atom and with C-H
distances 0.95 A (triazole), 0.99 A (CH2 adamantane) and 1.00
(CH adamantane). The OH-hydrogen atoms were located and then constrained
with O-H distances set to 0.85 A and Uiso = 1.5Ueq of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         14439
_refine_ls_number_parameters     885
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1132
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.77223(5) 0.03496(2) 0.73841(4) 0.02910(18) Uani 1 1 d . . .
Cd2 Cd 0.26569(5) 0.21301(2) 0.76682(4) 0.02681(17) Uani 1 1 d . . .
Cd3 Cd 0.79382(6) 0.23898(3) 0.74199(5) 0.0448(2) Uani 1 1 d . . .
Cd4 Cd 0.27986(6) 0.01364(3) 0.73394(5) 0.0412(2) Uani 1 1 d . . .
Br1 Br 0.73407(12) 0.19609(5) 0.86317(6) 0.0688(4) Uani 1 1 d . . .
Br2 Br 0.75680(11) 0.18779(5) 0.62751(7) 0.0689(5) Uani 1 1 d . . .
Br3 Br 0.96286(9) 0.25643(6) 0.76253(12) 0.1002(6) Uani 1 1 d . . .
Br4 Br 0.71693(8) 0.31514(4) 0.71241(6) 0.0442(3) Uani 1 1 d . . .
Br5 Br 0.25922(10) 0.05850(4) 0.86115(6) 0.0610(4) Uani 1 1 d . . .
Br6 Br 0.21984(10) 0.06213(4) 0.62002(6) 0.0566(4) Uani 1 1 d . . .
Br7 Br 0.18886(9) -0.05994(4) 0.74638(8) 0.0660(4) Uani 1 1 d . . .
Br8 Br 0.44888(9) 0.00021(6) 0.70793(9) 0.0779(5) Uani 1 1 d . . .
O1 O 0.8298(6) 0.1085(3) 0.7661(4) 0.076(3) Uani 1 1 d . . .
H1W H 0.8104 0.1255 0.8016 0.114 Uiso 1 1 d R . .
H2W H 0.8189 0.1216 0.7241 0.114 Uiso 1 1 d R . .
O2 O 0.6350(6) 0.0735(3) 0.7083(5) 0.099(4) Uani 1 1 d . . .
H3W H 0.5925 0.0540 0.7064 0.148 Uiso 1 1 d R . .
H4W H 0.6144 0.0975 0.7288 0.148 Uiso 1 1 d R . .
O3 O 0.3165(5) 0.1389(2) 0.7364(4) 0.053(2) Uani 1 1 d . . .
H5W H 0.3078 0.1229 0.7761 0.080 Uiso 1 1 d R . .
H6W H 0.2954 0.1243 0.6986 0.080 Uiso 1 1 d R . .
O4 O 0.1220(5) 0.1797(2) 0.7993(4) 0.045(2) Uani 1 1 d . . .
H7W H 0.1028 0.1550 0.7800 0.068 Uiso 1 1 d R . .
H8W H 0.0829 0.2002 0.7909 0.068 Uiso 1 1 d R . .
N1 N 0.8275(6) 0.0509(3) 0.6180(4) 0.035(2) Uani 1 1 d . . .
N2 N 0.7899(7) 0.0343(3) 0.5523(5) 0.061(3) Uani 1 1 d . . .
N3 N 0.8942(6) 0.0838(3) 0.5219(5) 0.035(2) Uani 1 1 d . . .
N4 N 1.2432(7) 0.2407(3) 0.5861(5) 0.057(3) Uani 1 1 d . . .
N5 N 1.2082(6) 0.2150(3) 0.6438(4) 0.036(2) Uani 1 1 d . . .
N6 N 1.1329(6) 0.1973(3) 0.5421(4) 0.030(2) Uani 1 1 d . . .
N7 N 0.7137(6) 0.0357(3) 0.8623(5) 0.043(2) Uani 1 1 d . . .
N8 N 0.7462(7) 0.0108(3) 0.9212(5) 0.051(3) Uani 1 1 d . . .
N9 N 0.6402(6) 0.0571(3) 0.9653(5) 0.039(2) Uani 1 1 d . . .
N10 N 0.3142(6) 0.1941(3) 0.8861(4) 0.035(2) Uani 1 1 d . . .
N11 N 0.2702(6) 0.2080(3) 0.9513(4) 0.041(2) Uani 1 1 d . . .
N12 N 0.3877(6) 0.1648(3) 0.9814(4) 0.028(2) Uani 1 1 d . . .
N13 N 0.3956(5) 0.2471(3) 0.7189(4) 0.028(2) Uani 1 1 d . . .
N14 N 0.4780(6) 0.2281(3) 0.7001(5) 0.033(2) Uani 1 1 d . . .
N15 N 0.4626(5) 0.2922(3) 0.6370(4) 0.0216(19) Uani 1 1 d . . .
N16 N 0.6025(5) 0.4996(3) 0.7106(5) 0.036(2) Uani 1 1 d . . .
N17 N 0.5241(6) 0.5226(3) 0.6878(5) 0.035(2) Uani 1 1 d . . .
N18 N 0.5305(5) 0.4557(3) 0.6313(4) 0.025(2) Uani 1 1 d . . .
N19 N 0.2109(6) 0.2787(3) 0.8166(5) 0.036(2) Uani 1 1 d . . .
N20 N 0.2256(6) 0.3205(3) 0.7819(4) 0.036(2) Uani 1 1 d . . .
N21 N 0.1339(5) 0.3305(3) 0.8806(4) 0.026(2) Uani 1 1 d . . .
N22 N -0.2108(6) 0.4702(3) 0.8083(4) 0.035(2) Uani 1 1 d . . .
N23 N -0.2242(6) 0.4286(3) 0.7733(5) 0.045(2) Uani 1 1 d . . .
N24 N -0.1392(5) 0.4200(3) 0.8755(4) 0.028(2) Uani 1 1 d . . .
C1 C 0.8848(8) 0.0809(4) 0.5987(6) 0.042(3) Uani 1 1 d . . .
H1 H 0.9172 0.0993 0.6339 0.051 Uiso 1 1 calc R . .
C2 C 0.8359(10) 0.0525(4) 0.4962(7) 0.077(5) Uani 1 1 d . . .
H2 H 0.8288 0.0445 0.4442 0.092 Uiso 1 1 calc R . .
C3 C 1.1974(8) 0.2303(4) 0.5268(6) 0.057(4) Uani 1 1 d . . .
H3 H 1.2065 0.2435 0.4781 0.068 Uiso 1 1 calc R . .
C4 C 1.1422(8) 0.1896(4) 0.6170(6) 0.042(3) Uani 1 1 d . . .
H4 H 1.1067 0.1690 0.6460 0.050 Uiso 1 1 calc R . .
C5 C 0.9502(7) 0.1164(4) 0.4765(5) 0.029(3) Uani 1 1 d . . .
C6 C 1.0137(7) 0.1404(3) 0.5305(5) 0.030(3) Uani 1 1 d . . .
H6A H 1.0541 0.1180 0.5553 0.036 Uiso 1 1 calc R . .
H6B H 0.9784 0.1559 0.5707 0.036 Uiso 1 1 calc R . .
C7 C 1.0706(7) 0.1753(4) 0.4868(5) 0.035(3) Uani 1 1 d . . .
C8 C 1.0084(6) 0.2107(3) 0.4515(6) 0.031(3) Uani 1 1 d . . .
H8A H 1.0446 0.2336 0.4235 0.037 Uiso 1 1 calc R . .
H8B H 0.9736 0.2265 0.4917 0.037 Uiso 1 1 calc R . .
C9 C 0.9439(7) 0.1865(4) 0.3970(6) 0.041(3) Uani 1 1 d . . .
H9 H 0.9032 0.2094 0.3727 0.050 Uiso 1 1 calc R . .
C10 C 0.8850(7) 0.1510(4) 0.4399(6) 0.039(3) Uani 1 1 d . . .
H10A H 0.8483 0.1662 0.4797 0.047 Uiso 1 1 calc R . .
H10B H 0.8435 0.1356 0.4041 0.047 Uiso 1 1 calc R . .
C11 C 1.0055(7) 0.0915(4) 0.4145(6) 0.040(3) Uani 1 1 d . . .
H11A H 1.0465 0.0690 0.4381 0.048 Uiso 1 1 calc R . .
H11B H 0.9642 0.0754 0.3792 0.048 Uiso 1 1 calc R . .
C12 C 1.0605(7) 0.1271(4) 0.3709(5) 0.042(3) Uani 1 1 d . . .
H12 H 1.0957 0.1119 0.3296 0.050 Uiso 1 1 calc R . .
C13 C 1.1266(7) 0.1509(4) 0.4259(6) 0.035(3) Uani 1 1 d . . .
H13A H 1.1671 0.1283 0.4499 0.042 Uiso 1 1 calc R . .
H13B H 1.1644 0.1730 0.3978 0.042 Uiso 1 1 calc R . .
C14 C 0.9966(8) 0.1621(4) 0.3357(6) 0.047(3) Uani 1 1 d . . .
H14A H 1.0321 0.1844 0.3059 0.056 Uiso 1 1 calc R . .
H14B H 0.9541 0.1467 0.3006 0.056 Uiso 1 1 calc R . .
C15 C 0.6518(8) 0.0633(4) 0.8887(5) 0.043(3) Uani 1 1 d . . .
H15 H 0.6195 0.0848 0.8588 0.051 Uiso 1 1 calc R . .
C16 C 0.7010(8) 0.0242(4) 0.9810(6) 0.052(4) Uani 1 1 d . . .
H16 H 0.7100 0.0120 1.0304 0.063 Uiso 1 1 calc R . .
C17 C 0.3846(8) 0.1689(4) 0.9045(5) 0.034(3) Uani 1 1 d . . .
H17 H 0.4262 0.1557 0.8698 0.041 Uiso 1 1 calc R . .
C18 C 0.3160(8) 0.1893(4) 1.0075(5) 0.049(4) Uani 1 1 d . . .
H18 H 0.3007 0.1924 1.0598 0.059 Uiso 1 1 calc R . .
C19 C 0.5825(7) 0.0837(4) 1.0192(5) 0.032(3) Uani 1 1 d . . .
C20 C 0.5132(7) 0.1112(4) 0.9724(5) 0.032(3) Uani 1 1 d . . .
H20A H 0.5453 0.1321 0.9375 0.038 Uiso 1 1 calc R . .
H20B H 0.4757 0.0903 0.9414 0.038 Uiso 1 1 calc R . .
C21 C 0.4526(7) 0.1383(4) 1.0262(5) 0.026(3) Uani 1 1 d . . .
C22 C 0.5112(8) 0.1715(4) 1.0709(6) 0.040(3) Uani 1 1 d . . .
H22A H 0.4729 0.1898 1.1054 0.048 Uiso 1 1 calc R . .
H22B H 0.5427 0.1923 1.0356 0.048 Uiso 1 1 calc R . .
C23 C 0.5814(8) 0.1443(4) 1.1177(6) 0.050(4) Uani 1 1 d . . .
H23 H 0.6202 0.1657 1.1476 0.060 Uiso 1 1 calc R . .
C24 C 0.6415(7) 0.1161(4) 1.0629(6) 0.040(3) Uani 1 1 d . . .
H24A H 0.6735 0.1366 1.0272 0.048 Uiso 1 1 calc R . .
H24B H 0.6874 0.0990 1.0923 0.048 Uiso 1 1 calc R . .
C25 C 0.5331(7) 0.0515(4) 1.0726(5) 0.038(3) Uani 1 1 d . . .
H25A H 0.5774 0.0336 1.1025 0.045 Uiso 1 1 calc R . .
H25B H 0.4952 0.0301 1.0430 0.045 Uiso 1 1 calc R . .
C26 C 0.4734(8) 0.0798(4) 1.1261(6) 0.043(3) Uani 1 1 d . . .
H26 H 0.4409 0.0590 1.1619 0.052 Uiso 1 1 calc R . .
C27 C 0.4051(8) 0.1071(4) 1.0823(6) 0.043(3) Uani 1 1 d . . .
H27A H 0.3683 0.1254 1.1180 0.051 Uiso 1 1 calc R . .
H27B H 0.3640 0.0864 1.0544 0.051 Uiso 1 1 calc R . .
C28 C 0.5311(9) 0.1127(4) 1.1718(6) 0.060(4) Uani 1 1 d . . .
H28A H 0.5752 0.0956 1.2033 0.072 Uiso 1 1 calc R . .
H28B H 0.4921 0.1307 1.2063 0.072 Uiso 1 1 calc R . .
C29 C 0.3907(7) 0.2847(3) 0.6822(5) 0.027(2) Uani 1 1 d . . .
H29 H 0.3412 0.3052 0.6866 0.032 Uiso 1 1 calc R . .
C30 C 0.5162(7) 0.2572(4) 0.6508(5) 0.033(3) Uani 1 1 d . . .
H30 H 0.5743 0.2531 0.6287 0.040 Uiso 1 1 calc R . .
C31 C 0.6049(7) 0.4611(3) 0.6758(5) 0.028(3) Uani 1 1 d . . .
H31 H 0.6522 0.4394 0.6807 0.033 Uiso 1 1 calc R . .
C32 C 0.4826(7) 0.4951(3) 0.6409(6) 0.033(3) Uani 1 1 d . . .
H32 H 0.4266 0.5015 0.6166 0.039 Uiso 1 1 calc R . .
C33 C 0.4768(6) 0.3324(3) 0.5874(5) 0.022(2) Uani 1 1 d . . .
C34 C 0.4959(8) 0.3744(3) 0.6350(5) 0.025(2) Uani 1 1 d . . .
H34A H 0.5506 0.3694 0.6665 0.030 Uiso 1 1 calc R . .
H34B H 0.4443 0.3803 0.6696 0.030 Uiso 1 1 calc R . .
C35 C 0.5105(7) 0.4158(3) 0.5825(5) 0.026(3) Uani 1 1 d . . .
C36 C 0.4249(7) 0.4235(4) 0.5380(6) 0.039(3) Uani 1 1 d . . .
H36A H 0.3740 0.4292 0.5734 0.047 Uiso 1 1 calc R . .
H36B H 0.4320 0.4505 0.5050 0.047 Uiso 1 1 calc R . .
C37 C 0.4046(8) 0.3826(4) 0.4901(6) 0.036(3) Uani 1 1 d . . .
H37 H 0.3482 0.3882 0.4600 0.043 Uiso 1 1 calc R . .
C38 C 0.3906(7) 0.3396(3) 0.5417(5) 0.029(3) Uani 1 1 d . . .
H38A H 0.3386 0.3442 0.5763 0.035 Uiso 1 1 calc R . .
H38B H 0.3782 0.3126 0.5098 0.035 Uiso 1 1 calc R . .
C39 C 0.5573(7) 0.3223(4) 0.5323(5) 0.029(3) Uani 1 1 d . . .
H39A H 0.6134 0.3165 0.5616 0.035 Uiso 1 1 calc R . .
H39B H 0.5439 0.2952 0.5009 0.035 Uiso 1 1 calc R . .
C40 C 0.5692(8) 0.3646(4) 0.4808(6) 0.035(3) Uani 1 1 d . . .
H40 H 0.6208 0.3591 0.4451 0.042 Uiso 1 1 calc R . .
C41 C 0.5907(7) 0.4064(3) 0.5293(5) 0.032(3) Uani 1 1 d . . .
H41A H 0.6013 0.4330 0.4960 0.039 Uiso 1 1 calc R . .
H41B H 0.6462 0.4010 0.5596 0.039 Uiso 1 1 calc R . .
C42 C 0.4839(9) 0.3721(4) 0.4347(5) 0.047(4) Uani 1 1 d . . .
H42A H 0.4700 0.3446 0.4044 0.057 Uiso 1 1 calc R . .
H42B H 0.4926 0.3979 0.3992 0.057 Uiso 1 1 calc R . .
C43 C 0.1556(7) 0.2864(4) 0.8732(6) 0.038(3) Uani 1 1 d . . .
H43 H 0.1331 0.2632 0.9057 0.046 Uiso 1 1 calc R . .
C44 C 0.1793(7) 0.3495(4) 0.8230(6) 0.038(3) Uani 1 1 d . . .
H44 H 0.1780 0.3811 0.8127 0.045 Uiso 1 1 calc R . .
C45 C -0.1622(8) 0.4634(4) 0.8683(6) 0.049(3) Uani 1 1 d . . .
H45 H -0.1450 0.4865 0.9031 0.059 Uiso 1 1 calc R . .
C46 C -0.1786(8) 0.4004(4) 0.8152(6) 0.049(3) Uani 1 1 d . . .
H46 H -0.1738 0.3689 0.8042 0.059 Uiso 1 1 calc R . .
C47 C 0.0670(7) 0.3514(4) 0.9315(5) 0.025(3) Uani 1 1 d . . .
C48 C -0.0037(6) 0.3753(4) 0.8797(5) 0.024(2) Uani 1 1 d . . .
H48A H 0.0268 0.3985 0.8479 0.028 Uiso 1 1 calc R . .
H48B H -0.0320 0.3527 0.8454 0.028 Uiso 1 1 calc R . .
C49 C -0.0765(7) 0.3978(4) 0.9286(5) 0.030(3) Uani 1 1 d . . .
C50 C -0.0313(7) 0.4337(3) 0.9799(5) 0.036(3) Uani 1 1 d . . .
H50A H -0.0009 0.4569 0.9480 0.043 Uiso 1 1 calc R . .
H50B H -0.0778 0.4491 1.0112 0.043 Uiso 1 1 calc R . .
C51 C 0.0383(7) 0.4106(4) 1.0317(6) 0.035(3) Uani 1 1 d . . .
H51 H 0.0674 0.4336 1.0656 0.042 Uiso 1 1 calc R . .
C52 C 0.1110(7) 0.3876(4) 0.9816(6) 0.036(3) Uani 1 1 d . . .
H52A H 0.1410 0.4106 0.9492 0.043 Uiso 1 1 calc R . .
H52B H 0.1577 0.3734 1.0143 0.043 Uiso 1 1 calc R . .
C53 C 0.0201(7) 0.3160(4) 0.9798(5) 0.033(3) Uani 1 1 d . . .
H53A H 0.0648 0.3006 1.0129 0.039 Uiso 1 1 calc R . .
H53B H -0.0085 0.2929 0.9467 0.039 Uiso 1 1 calc R . .
C54 C -0.0543(7) 0.3399(4) 1.0302(6) 0.040(3) Uani 1 1 d . . .
H54 H -0.0856 0.3167 1.0623 0.048 Uiso 1 1 calc R . .
C55 C -0.1231(7) 0.3627(4) 0.9774(5) 0.031(3) Uani 1 1 d . . .
H55A H -0.1518 0.3395 0.9446 0.037 Uiso 1 1 calc R . .
H55B H -0.1711 0.3773 1.0081 0.037 Uiso 1 1 calc R . .
C56 C -0.0094(8) 0.3741(4) 1.0803(5) 0.046(3) Uani 1 1 d . . .
H56A H 0.0356 0.3588 1.1133 0.055 Uiso 1 1 calc R . .
H56B H -0.0552 0.3887 1.1134 0.055 Uiso 1 1 calc R . .
O1W O 0.5497(6) 0.1479(3) 0.7771(5) 0.097(4) Uani 1 1 d . . .
H9W H 0.5964 0.1579 0.7999 0.145 Uiso 1 1 d R . .
H10W H 0.5254 0.1698 0.7532 0.145 Uiso 1 1 d R . .
O2W O 0.0502(5) 0.1007(2) 0.7335(4) 0.060(2) Uani 1 1 d . . .
H11W H 0.0929 0.0914 0.7050 0.090 Uiso 1 1 d R . .
H12W H 0.0281 0.0780 0.7569 0.090 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0376(4) 0.0242(4) 0.0255(3) 0.0017(3) 0.0011(4) 0.0009(4)
Cd2 0.0331(4) 0.0249(4) 0.0224(3) 0.0018(3) 0.0003(4) -0.0020(3)
Cd3 0.0525(6) 0.0395(5) 0.0425(5) -0.0033(4) -0.0049(5) 0.0055(4)
Cd4 0.0504(5) 0.0311(4) 0.0422(4) 0.0020(4) 0.0072(5) -0.0009(4)
Br1 0.1163(13) 0.0568(9) 0.0332(6) 0.0001(6) 0.0083(8) 0.0103(9)
Br2 0.1064(13) 0.0564(9) 0.0440(7) -0.0194(7) 0.0012(8) 0.0030(9)
Br3 0.0557(9) 0.0850(13) 0.1598(18) 0.0149(12) -0.0348(12) 0.0017(8)
Br4 0.0478(7) 0.0380(7) 0.0467(6) -0.0064(5) -0.0063(6) 0.0061(6)
Br5 0.1045(12) 0.0443(8) 0.0340(6) 0.0010(6) 0.0076(7) -0.0011(8)
Br6 0.0757(9) 0.0558(8) 0.0381(6) 0.0056(6) -0.0033(7) 0.0023(8)
Br7 0.0696(9) 0.0370(7) 0.0915(10) -0.0092(7) 0.0311(9) -0.0113(6)
Br8 0.0540(9) 0.0844(12) 0.0953(11) 0.0230(9) 0.0209(8) 0.0103(8)
O1 0.122(7) 0.053(6) 0.053(5) -0.008(4) 0.022(6) -0.012(5)
O2 0.118(8) 0.127(10) 0.051(6) -0.016(6) -0.033(6) 0.079(7)
O3 0.087(6) 0.029(4) 0.044(4) -0.005(4) -0.008(5) -0.008(4)
O4 0.042(5) 0.043(5) 0.051(5) 0.014(4) 0.001(4) -0.010(4)
N1 0.055(6) 0.029(6) 0.022(5) 0.001(4) -0.008(4) -0.015(5)
N2 0.083(8) 0.070(8) 0.031(5) -0.008(5) 0.007(6) -0.039(7)
N3 0.048(6) 0.034(6) 0.023(5) -0.001(4) 0.000(5) -0.023(5)
N4 0.074(8) 0.064(8) 0.033(5) 0.009(5) -0.020(5) -0.048(6)
N5 0.045(6) 0.047(6) 0.017(4) 0.009(4) -0.010(4) -0.021(5)
N6 0.036(6) 0.035(6) 0.020(4) 0.010(4) 0.000(4) -0.005(4)
N7 0.046(6) 0.049(6) 0.033(5) 0.005(5) -0.002(5) 0.011(5)
N8 0.073(8) 0.039(6) 0.040(5) 0.009(5) 0.005(5) 0.020(5)
N9 0.045(6) 0.036(6) 0.035(5) 0.016(5) 0.009(5) 0.006(5)
N10 0.044(6) 0.037(6) 0.025(5) -0.005(4) 0.005(4) 0.002(5)
N11 0.033(5) 0.065(7) 0.024(4) 0.006(4) 0.002(4) 0.016(5)
N12 0.036(6) 0.037(6) 0.012(4) 0.001(4) 0.004(4) 0.009(5)
N13 0.024(5) 0.030(5) 0.029(5) 0.005(4) -0.009(4) -0.006(4)
N14 0.031(6) 0.029(5) 0.040(5) 0.001(4) 0.004(4) 0.001(4)
N15 0.026(5) 0.017(5) 0.022(4) 0.003(4) 0.004(4) 0.006(4)
N16 0.036(5) 0.023(5) 0.048(6) -0.005(4) -0.002(4) 0.009(4)
N17 0.040(6) 0.026(5) 0.040(5) -0.001(4) -0.001(5) 0.002(4)
N18 0.027(5) 0.017(5) 0.030(5) 0.001(4) 0.001(4) -0.003(4)
N19 0.031(5) 0.022(5) 0.055(6) 0.001(4) 0.006(5) 0.000(4)
N20 0.031(5) 0.039(6) 0.037(5) 0.002(4) 0.008(5) 0.012(5)
N21 0.025(5) 0.027(5) 0.027(5) 0.008(4) 0.003(4) 0.004(4)
N22 0.044(6) 0.021(5) 0.039(5) 0.004(4) -0.010(5) 0.008(5)
N23 0.057(6) 0.019(5) 0.058(6) -0.003(4) -0.017(6) 0.010(5)
N24 0.023(5) 0.036(6) 0.025(5) -0.005(4) 0.003(4) 0.012(4)
C1 0.065(9) 0.040(8) 0.022(6) 0.005(5) 0.008(6) -0.021(7)
C2 0.124(14) 0.059(10) 0.047(8) -0.010(7) 0.018(9) -0.059(10)
C3 0.069(10) 0.068(9) 0.034(6) 0.017(6) -0.014(7) -0.042(8)
C4 0.052(8) 0.039(8) 0.035(6) 0.014(6) -0.013(6) -0.027(6)
C5 0.034(7) 0.041(8) 0.013(5) -0.004(5) 0.008(5) -0.007(6)
C6 0.037(8) 0.037(7) 0.015(5) 0.005(5) 0.002(5) -0.003(6)
C7 0.040(7) 0.050(9) 0.014(5) -0.003(5) 0.000(5) -0.005(6)
C8 0.019(6) 0.036(7) 0.037(6) 0.009(5) -0.009(5) -0.001(5)
C9 0.023(7) 0.047(8) 0.055(7) 0.026(6) 0.001(6) 0.003(6)
C10 0.028(7) 0.067(9) 0.023(6) 0.007(6) -0.005(5) 0.000(6)
C11 0.031(7) 0.043(8) 0.048(7) -0.001(6) -0.002(6) -0.013(6)
C12 0.040(7) 0.074(10) 0.011(5) -0.002(6) 0.007(5) 0.001(7)
C13 0.026(6) 0.045(8) 0.033(6) 0.008(5) 0.003(5) -0.010(6)
C14 0.049(8) 0.073(9) 0.020(6) -0.001(6) 0.010(5) -0.016(7)
C15 0.065(9) 0.045(8) 0.019(5) 0.008(5) 0.006(6) 0.023(7)
C16 0.065(10) 0.055(9) 0.037(6) 0.016(6) 0.008(7) 0.027(7)
C17 0.053(8) 0.036(7) 0.015(5) 0.001(5) 0.004(5) 0.010(6)
C18 0.060(9) 0.078(10) 0.009(5) 0.011(6) 0.004(5) 0.029(7)
C19 0.029(7) 0.051(8) 0.015(5) 0.007(5) 0.011(5) 0.015(6)
C20 0.041(8) 0.036(8) 0.018(6) 0.008(5) 0.001(5) 0.015(6)
C21 0.030(7) 0.037(7) 0.013(5) 0.004(5) -0.015(5) 0.005(5)
C22 0.057(8) 0.040(8) 0.024(6) 0.011(5) 0.003(6) 0.006(6)
C23 0.059(9) 0.048(9) 0.043(7) -0.017(7) -0.024(7) 0.012(7)
C24 0.044(8) 0.039(8) 0.038(7) 0.009(6) -0.015(6) 0.002(6)
C25 0.049(8) 0.039(8) 0.025(6) 0.005(5) 0.008(6) 0.006(6)
C26 0.062(8) 0.038(7) 0.031(6) 0.012(6) 0.020(6) 0.017(6)
C27 0.046(8) 0.052(9) 0.030(6) 0.006(6) 0.011(6) 0.013(7)
C28 0.090(11) 0.058(10) 0.033(7) 0.000(6) -0.007(7) 0.045(8)
C29 0.024(6) 0.019(6) 0.039(6) 0.008(5) 0.001(5) -0.001(5)
C30 0.034(7) 0.033(7) 0.033(6) -0.003(5) 0.007(5) -0.015(6)
C31 0.019(6) 0.026(7) 0.039(6) 0.003(5) -0.008(5) 0.002(5)
C32 0.033(7) 0.025(6) 0.039(6) 0.000(5) -0.005(6) 0.005(5)
C33 0.023(6) 0.023(6) 0.021(5) 0.008(4) 0.007(5) 0.001(5)
C34 0.034(6) 0.018(5) 0.022(5) -0.006(5) 0.000(5) 0.008(5)
C35 0.035(7) 0.016(6) 0.028(6) -0.004(5) 0.005(5) -0.005(5)
C36 0.045(8) 0.037(8) 0.035(7) 0.015(6) -0.006(6) -0.003(6)
C37 0.047(8) 0.040(8) 0.021(6) -0.002(5) -0.001(6) 0.008(6)
C38 0.038(7) 0.023(6) 0.027(6) -0.005(5) -0.002(5) 0.005(5)
C39 0.034(7) 0.040(7) 0.014(5) -0.011(5) 0.001(5) 0.013(6)
C40 0.052(8) 0.030(7) 0.024(6) 0.007(5) 0.011(6) 0.006(6)
C41 0.043(7) 0.026(7) 0.028(6) 0.009(5) 0.002(5) -0.006(5)
C42 0.107(11) 0.026(7) 0.009(5) 0.004(5) -0.009(7) -0.014(7)
C43 0.029(7) 0.037(7) 0.047(7) 0.025(6) 0.004(6) 0.007(6)
C44 0.041(7) 0.020(6) 0.053(7) -0.002(5) 0.007(6) 0.000(5)
C45 0.066(9) 0.039(8) 0.042(7) -0.019(6) -0.016(7) 0.036(7)
C46 0.060(9) 0.033(7) 0.054(8) -0.007(6) -0.031(7) 0.010(6)
C47 0.025(6) 0.027(7) 0.024(5) -0.004(5) -0.001(5) 0.012(5)
C48 0.011(5) 0.044(6) 0.016(5) -0.001(5) -0.009(5) 0.006(5)
C49 0.036(7) 0.033(7) 0.022(6) 0.000(5) -0.011(5) 0.009(6)
C50 0.056(8) 0.024(7) 0.028(6) -0.007(5) 0.001(6) 0.011(6)
C51 0.028(7) 0.040(8) 0.037(7) -0.018(6) -0.001(5) -0.003(6)
C52 0.037(7) 0.036(8) 0.035(7) 0.004(6) 0.004(6) -0.011(6)
C53 0.032(7) 0.038(7) 0.029(6) 0.020(5) -0.005(5) 0.003(6)
C54 0.039(8) 0.054(9) 0.027(6) 0.020(6) 0.004(5) -0.007(7)
C55 0.038(7) 0.041(7) 0.014(5) 0.008(5) 0.009(5) 0.006(6)
C56 0.048(8) 0.069(9) 0.019(6) 0.002(6) -0.002(6) 0.007(7)
O1W 0.139(9) 0.102(8) 0.049(6) 0.020(5) 0.017(6) 0.077(7)
O2W 0.080(6) 0.041(5) 0.058(5) 0.011(4) 0.005(5) -0.002(4)

_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.
;

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
Cd1 N22 2.265(8) 2_546 ?
Cd1 N16 2.303(8) 2_646 ?
Cd1 N1 2.317(8) . ?
Cd1 N7 2.343(8) . ?
Cd1 O1 2.377(8) . ?
Cd1 O2 2.382(8) . ?
Cd2 N19 2.272(8) . ?
Cd2 N10 2.284(8) . ?
Cd2 N5 2.323(7) 1_455 ?
Cd2 N13 2.323(8) . ?
Cd2 O3 2.370(6) . ?
Cd2 O4 2.406(7) . ?
Cd3 Br4 2.5673(14) . ?
Cd3 Br2 2.5725(14) . ?
Cd3 Br3 2.5733(16) . ?
Cd3 Br1 2.6286(15) . ?
Cd4 Br7 2.5595(14) . ?
Cd4 Br8 2.5678(16) . ?
Cd4 Br6 2.6134(15) . ?
Cd4 Br5 2.6145(14) . ?
O1 H1W 0.8500 . ?
O1 H2W 0.8500 . ?
O2 H3W 0.8502 . ?
O2 H4W 0.8500 . ?
O3 H5W 0.8499 . ?
O3 H6W 0.8499 . ?
O4 H7W 0.8501 . ?
O4 H8W 0.8500 . ?
N1 C1 1.269(12) . ?
N1 N2 1.371(11) . ?
N2 C2 1.312(13) . ?
N3 C2 1.340(14) . ?
N3 C1 1.360(11) . ?
N3 C5 1.497(13) . ?
N4 C3 1.279(12) . ?
N4 N5 1.368(11) . ?
N5 C4 1.316(12) . ?
N5 Cd2 2.323(7) 1_655 ?
N6 C4 1.342(12) . ?
N6 C3 1.386(13) . ?
N6 C7 1.487(13) . ?
N7 C15 1.308(12) . ?
N7 N8 1.355(11) . ?
N8 C16 1.305(13) . ?
N9 C16 1.348(13) . ?
N9 C15 1.370(11) . ?
N9 C19 1.497(12) . ?
N10 C17 1.319(12) . ?
N10 N11 1.378(10) . ?
N11 C18 1.319(12) . ?
N12 C17 1.357(11) . ?
N12 C18 1.360(12) . ?
N12 C21 1.465(12) . ?
N13 C29 1.285(11) . ?
N13 N14 1.378(10) . ?
N14 C30 1.343(12) . ?
N15 C30 1.323(12) . ?
N15 C29 1.345(11) . ?
N15 C33 1.485(11) . ?
N16 C31 1.291(11) . ?
N16 N17 1.399(11) . ?
N16 Cd1 2.303(8) 2_656 ?
N17 C32 1.308(12) . ?
N18 C31 1.358(12) . ?
N18 C32 1.367(11) . ?
N18 C35 1.485(12) . ?
N19 C43 1.307(12) . ?
N19 N20 1.390(10) . ?
N20 C44 1.311(11) . ?
N21 C44 1.337(12) . ?
N21 C43 1.344(12) . ?
N21 C47 1.469(11) . ?
N22 C45 1.291(12) . ?
N22 N23 1.387(10) . ?
N22 Cd1 2.265(8) 2_556 ?
N23 C46 1.297(12) . ?
N24 C45 1.330(12) . ?
N24 C46 1.338(12) . ?
N24 C49 1.467(12) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.510(14) . ?
C5 C10 1.543(14) . ?
C5 C11 1.545(13) . ?
C6 C7 1.533(13) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.522(14) . ?
C7 C13 1.532(14) . ?
C8 C9 1.527(14) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.511(14) . ?
C9 C10 1.554(14) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.532(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.527(15) . ?
C12 C13 1.540(14) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.503(14) . ?
C19 C25 1.522(13) . ?
C19 C20 1.542(13) . ?
C20 C21 1.527(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.520(14) . ?
C21 C22 1.524(14) . ?
C22 C23 1.546(14) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C28 1.523(16) . ?
C23 C24 1.551(14) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.535(13) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.502(14) . ?
C26 C28 1.521(16) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.519(13) . ?
C33 C34 1.520(13) . ?
C33 C39 1.563(12) . ?
C34 C35 1.544(13) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.503(14) . ?
C35 C41 1.534(13) . ?
C36 C37 1.501(14) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C42 1.555(15) . ?
C37 C38 1.572(14) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.552(13) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C42 1.513(15) . ?
C40 C41 1.530(14) . ?
C40 H40 1.0000 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C53 1.513(13) . ?
C47 C52 1.526(14) . ?
C47 C48 1.552(13) . ?
C48 C49 1.528(13) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C55 1.510(13) . ?
C49 C50 1.542(14) . ?
C50 C51 1.532(14) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C56 1.542(15) . ?
C51 C52 1.545(13) . ?
C51 H51 1.0000 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.577(14) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C56 1.492(15) . ?
C54 C55 1.529(14) . ?
C54 H54 1.0000 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
O1W H9W 0.8500 . ?
O1W H10W 0.8500 . ?
O2W H11W 0.8500 . ?
O2W H12W 0.8501 . ?

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
N22 Cd1 N16 94.7(3) 2_546 2_646 ?
N22 Cd1 N1 88.9(3) 2_546 . ?
N16 Cd1 N1 99.4(3) 2_646 . ?
N22 Cd1 N7 101.4(3) 2_546 . ?
N16 Cd1 N7 86.5(3) 2_646 . ?
N1 Cd1 N7 167.7(3) . . ?
N22 Cd1 O1 169.8(3) 2_546 . ?
N16 Cd1 O1 92.6(3) 2_646 . ?
N1 Cd1 O1 82.9(3) . . ?
N7 Cd1 O1 86.2(3) . . ?
N22 Cd1 O2 88.9(3) 2_546 . ?
N16 Cd1 O2 169.9(3) 2_646 . ?
N1 Cd1 O2 90.0(3) . . ?
N7 Cd1 O2 83.6(3) . . ?
O1 Cd1 O2 85.2(3) . . ?
N19 Cd2 N10 88.0(3) . . ?
N19 Cd2 N5 101.9(3) . 1_455 ?
N10 Cd2 N5 167.1(3) . 1_455 ?
N19 Cd2 N13 93.8(3) . . ?
N10 Cd2 N13 100.3(3) . . ?
N5 Cd2 N13 87.3(3) 1_455 . ?
N19 Cd2 O3 169.8(3) . . ?
N10 Cd2 O3 83.3(3) . . ?
N5 Cd2 O3 85.9(3) 1_455 . ?
N13 Cd2 O3 93.2(3) . . ?
N19 Cd2 O4 86.7(3) . . ?
N10 Cd2 O4 87.7(3) . . ?
N5 Cd2 O4 84.8(3) 1_455 . ?
N13 Cd2 O4 172.0(3) . . ?
O3 Cd2 O4 87.5(2) . . ?
Br4 Cd3 Br2 105.08(5) . . ?
Br4 Cd3 Br3 106.41(6) . . ?
Br2 Cd3 Br3 115.62(7) . . ?
Br4 Cd3 Br1 115.82(5) . . ?
Br2 Cd3 Br1 106.28(5) . . ?
Br3 Cd3 Br1 107.95(6) . . ?
Br7 Cd4 Br8 113.26(6) . . ?
Br7 Cd4 Br6 110.52(6) . . ?
Br8 Cd4 Br6 106.08(5) . . ?
Br7 Cd4 Br5 107.07(5) . . ?
Br8 Cd4 Br5 110.11(6) . . ?
Br6 Cd4 Br5 109.82(5) . . ?
Cd1 O1 H1W 124.5 . . ?
Cd1 O1 H2W 99.8 . . ?
H1W O1 H2W 107.8 . . ?
Cd1 O2 H3W 108.4 . . ?
Cd1 O2 H4W 127.4 . . ?
H3W O2 H4W 108.2 . . ?
Cd2 O3 H5W 106.1 . . ?
Cd2 O3 H6W 121.6 . . ?
H5W O3 H6W 107.9 . . ?
Cd2 O4 H7W 123.3 . . ?
Cd2 O4 H8W 105.5 . . ?
H7W O4 H8W 108.3 . . ?
C1 N1 N2 107.1(8) . . ?
C1 N1 Cd1 128.3(7) . . ?
N2 N1 Cd1 123.6(7) . . ?
C2 N2 N1 106.1(10) . . ?
C2 N3 C1 103.0(9) . . ?
C2 N3 C5 128.1(9) . . ?
C1 N3 C5 128.8(9) . . ?
C3 N4 N5 105.7(8) . . ?
C4 N5 N4 109.2(8) . . ?
C4 N5 Cd2 126.1(7) . 1_655 ?
N4 N5 Cd2 124.5(6) . 1_655 ?
C4 N6 C3 103.8(9) . . ?
C4 N6 C7 129.0(9) . . ?
C3 N6 C7 127.1(8) . . ?
C15 N7 N8 108.3(8) . . ?
C15 N7 Cd1 126.3(7) . . ?
N8 N7 Cd1 125.0(7) . . ?
C16 N8 N7 105.6(9) . . ?
C16 N9 C15 102.4(9) . . ?
C16 N9 C19 128.8(9) . . ?
C15 N9 C19 128.5(9) . . ?
C17 N10 N11 109.6(8) . . ?
C17 N10 Cd2 127.5(6) . . ?
N11 N10 Cd2 122.9(6) . . ?
C18 N11 N10 104.9(8) . . ?
C17 N12 C18 105.3(8) . . ?
C17 N12 C21 127.0(8) . . ?
C18 N12 C21 127.6(7) . . ?
C29 N13 N14 106.2(8) . . ?
C29 N13 Cd2 120.5(7) . . ?
N14 N13 Cd2 129.8(6) . . ?
C30 N14 N13 105.5(8) . . ?
C30 N15 C29 103.6(8) . . ?
C30 N15 C33 130.2(8) . . ?
C29 N15 C33 126.1(8) . . ?
C31 N16 N17 108.3(8) . . ?
C31 N16 Cd1 124.0(7) . 2_656 ?
N17 N16 Cd1 123.8(6) . 2_656 ?
C32 N17 N16 105.5(8) . . ?
C31 N18 C32 104.4(8) . . ?
C31 N18 C35 125.7(8) . . ?
C32 N18 C35 129.8(9) . . ?
C43 N19 N20 106.1(8) . . ?
C43 N19 Cd2 131.5(7) . . ?
N20 N19 Cd2 122.0(6) . . ?
C44 N20 N19 104.7(8) . . ?
C44 N21 C43 102.3(8) . . ?
C44 N21 C47 128.4(9) . . ?
C43 N21 C47 128.7(9) . . ?
C45 N22 N23 107.6(8) . . ?
C45 N22 Cd1 130.5(7) . 2_556 ?
N23 N22 Cd1 121.8(6) . 2_556 ?
C46 N23 N22 103.9(9) . . ?
C45 N24 C46 103.2(9) . . ?
C45 N24 C49 130.5(9) . . ?
C46 N24 C49 125.8(9) . . ?
N1 C1 N3 112.1(10) . . ?
N1 C1 H1 123.9 . . ?
N3 C1 H1 123.9 . . ?
N2 C2 N3 111.2(11) . . ?
N2 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
N4 C3 N6 111.9(9) . . ?
N4 C3 H3 124.0 . . ?
N6 C3 H3 124.0 . . ?
N5 C4 N6 109.3(9) . . ?
N5 C4 H4 125.4 . . ?
N6 C4 H4 125.4 . . ?
N3 C5 C6 107.9(7) . . ?
N3 C5 C10 107.5(8) . . ?
C6 C5 C10 109.8(9) . . ?
N3 C5 C11 111.4(9) . . ?
C6 C5 C11 109.7(9) . . ?
C10 C5 C11 110.5(8) . . ?
C5 C6 C7 109.7(8) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N6 C7 C8 109.8(9) . . ?
N6 C7 C13 109.1(8) . . ?
C8 C7 C13 111.2(8) . . ?
N6 C7 C6 107.7(8) . . ?
C8 C7 C6 109.5(9) . . ?
C13 C7 C6 109.4(9) . . ?
C7 C8 C9 108.1(9) . . ?
C7 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C14 C9 C8 110.3(9) . . ?
C14 C9 C10 108.4(10) . . ?
C8 C9 C10 111.0(9) . . ?
C14 C9 H9 109.0 . . ?
C8 C9 H9 109.0 . . ?
C10 C9 H9 109.0 . . ?
C5 C10 C9 107.3(8) . . ?
C5 C10 H10A 110.3 . . ?
C9 C10 H10A 110.3 . . ?
C5 C10 H10B 110.3 . . ?
C9 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
C12 C11 C5 108.0(9) . . ?
C12 C11 H11A 110.1 . . ?
C5 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
C5 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C14 C12 C11 109.6(9) . . ?
C14 C12 C13 109.8(10) . . ?
C11 C12 C13 109.5(8) . . ?
C14 C12 H12 109.3 . . ?
C11 C12 H12 109.3 . . ?
C13 C12 H12 109.3 . . ?
C7 C13 C12 108.0(8) . . ?
C7 C13 H13A 110.1 . . ?
C12 C13 H13A 110.1 . . ?
C7 C13 H13B 110.1 . . ?
C12 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
C9 C14 C12 110.5(9) . . ?
C9 C14 H14A 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N7 C15 N9 110.6(10) . . ?
N7 C15 H15 124.7 . . ?
N9 C15 H15 124.7 . . ?
N8 C16 N9 113.1(10) . . ?
N8 C16 H16 123.4 . . ?
N9 C16 H16 123.4 . . ?
N10 C17 N12 108.6(9) . . ?
N10 C17 H17 125.7 . . ?
N12 C17 H17 125.7 . . ?
N11 C18 N12 111.6(8) . . ?
N11 C18 H18 124.2 . . ?
N12 C18 H18 124.2 . . ?
N9 C19 C24 109.0(8) . . ?
N9 C19 C25 109.7(9) . . ?
C24 C19 C25 111.0(9) . . ?
N9 C19 C20 108.4(8) . . ?
C24 C19 C20 108.9(9) . . ?
C25 C19 C20 109.8(9) . . ?
C21 C20 C19 109.5(8) . . ?
C21 C20 H20A 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
N12 C21 C27 111.6(8) . . ?
N12 C21 C22 107.9(9) . . ?
C27 C21 C22 108.4(8) . . ?
N12 C21 C20 109.3(7) . . ?
C27 C21 C20 110.8(9) . . ?
C22 C21 C20 108.8(9) . . ?
C21 C22 C23 108.8(9) . . ?
C21 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
C21 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C28 C23 C22 108.8(10) . . ?
C28 C23 C24 109.8(10) . . ?
C22 C23 C24 109.3(9) . . ?
C28 C23 H23 109.6 . . ?
C22 C23 H23 109.6 . . ?
C24 C23 H23 109.6 . . ?
C19 C24 C23 109.0(9) . . ?
C19 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
C19 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C19 C25 C26 108.3(9) . . ?
C19 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
C19 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C27 C26 C28 107.8(9) . . ?
C27 C26 C25 111.2(9) . . ?
C28 C26 C25 110.3(10) . . ?
C27 C26 H26 109.2 . . ?
C28 C26 H26 109.2 . . ?
C25 C26 H26 109.2 . . ?
C26 C27 C21 110.3(9) . . ?
C26 C27 H27A 109.6 . . ?
C21 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C21 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C26 C28 C23 109.5(9) . . ?
C26 C28 H28A 109.8 . . ?
C23 C28 H28A 109.8 . . ?
C26 C28 H28B 109.8 . . ?
C23 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
N13 C29 N15 113.2(9) . . ?
N13 C29 H29 123.4 . . ?
N15 C29 H29 123.4 . . ?
N15 C30 N14 111.4(9) . . ?
N15 C30 H30 124.3 . . ?
N14 C30 H30 124.3 . . ?
N16 C31 N18 110.6(9) . . ?
N16 C31 H31 124.7 . . ?
N18 C31 H31 124.7 . . ?
N17 C32 N18 111.2(9) . . ?
N17 C32 H32 124.4 . . ?
N18 C32 H32 124.4 . . ?
N15 C33 C38 107.6(8) . . ?
N15 C33 C34 110.6(7) . . ?
C38 C33 C34 109.5(8) . . ?
N15 C33 C39 108.6(8) . . ?
C38 C33 C39 109.6(7) . . ?
C34 C33 C39 110.8(8) . . ?
C33 C34 C35 109.8(7) . . ?
C33 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
C35 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
N18 C35 C36 110.3(9) . . ?
N18 C35 C41 110.0(8) . . ?
C36 C35 C41 111.0(8) . . ?
N18 C35 C34 107.9(7) . . ?
C36 C35 C34 108.2(8) . . ?
C41 C35 C34 109.3(8) . . ?
C37 C36 C35 109.8(9) . . ?
C37 C36 H36A 109.7 . . ?
C35 C36 H36A 109.7 . . ?
C37 C36 H36B 109.7 . . ?
C35 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C36 C37 C42 111.1(10) . . ?
C36 C37 C38 110.5(8) . . ?
C42 C37 C38 107.5(9) . . ?
C36 C37 H37 109.2 . . ?
C42 C37 H37 109.2 . . ?
C38 C37 H37 109.2 . . ?
C33 C38 C37 107.9(8) . . ?
C33 C38 H38A 110.1 . . ?
C37 C38 H38A 110.1 . . ?
C33 C38 H38B 110.1 . . ?
C37 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
C40 C39 C33 107.1(8) . . ?
C40 C39 H39A 110.3 . . ?
C33 C39 H39A 110.3 . . ?
C40 C39 H39B 110.3 . . ?
C33 C39 H39B 110.3 . . ?
H39A C39 H39B 108.5 . . ?
C42 C40 C41 110.7(9) . . ?
C42 C40 C39 109.6(9) . . ?
C41 C40 C39 110.2(8) . . ?
C42 C40 H40 108.8 . . ?
C41 C40 H40 108.8 . . ?
C39 C40 H40 108.8 . . ?
C40 C41 C35 109.0(8) . . ?
C40 C41 H41A 109.9 . . ?
C35 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 . . ?
C35 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C40 C42 C37 108.7(8) . . ?
C40 C42 H42A 109.9 . . ?
C37 C42 H42A 109.9 . . ?
C40 C42 H42B 109.9 . . ?
C37 C42 H42B 109.9 . . ?
H42A C42 H42B 108.3 . . ?
N19 C43 N21 112.9(9) . . ?
N19 C43 H43 123.5 . . ?
N21 C43 H43 123.5 . . ?
N20 C44 N21 113.9(9) . . ?
N20 C44 H44 123.0 . . ?
N21 C44 H44 123.0 . . ?
N22 C45 N24 111.7(10) . . ?
N22 C45 H45 124.2 . . ?
N24 C45 H45 124.2 . . ?
N23 C46 N24 113.6(10) . . ?
N23 C46 H46 123.2 . . ?
N24 C46 H46 123.2 . . ?
N21 C47 C53 111.1(9) . . ?
N21 C47 C52 111.0(8) . . ?
C53 C47 C52 110.6(8) . . ?
N21 C47 C48 106.6(7) . . ?
C53 C47 C48 109.4(8) . . ?
C52 C47 C48 108.0(9) . . ?
C49 C48 C47 109.8(7) . . ?
C49 C48 H48A 109.7 . . ?
C47 C48 H48A 109.7 . . ?
C49 C48 H48B 109.7 . . ?
C47 C48 H48B 109.7 . . ?
H48A C48 H48B 108.2 . . ?
N24 C49 C55 112.3(9) . . ?
N24 C49 C48 106.2(7) . . ?
C55 C49 C48 110.1(9) . . ?
N24 C49 C50 109.8(9) . . ?
C55 C49 C50 109.6(8) . . ?
C48 C49 C50 108.8(9) . . ?
C51 C50 C49 109.3(8) . . ?
C51 C50 H50A 109.8 . . ?
C49 C50 H50A 109.8 . . ?
C51 C50 H50B 109.8 . . ?
C49 C50 H50B 109.8 . . ?
H50A C50 H50B 108.3 . . ?
C50 C51 C56 109.4(9) . . ?
C50 C51 C52 108.8(8) . . ?
C56 C51 C52 109.1(9) . . ?
C50 C51 H51 109.8 . . ?
C56 C51 H51 109.8 . . ?
C52 C51 H51 109.8 . . ?
C47 C52 C51 109.8(8) . . ?
C47 C52 H52A 109.7 . . ?
C51 C52 H52A 109.7 . . ?
C47 C52 H52B 109.7 . . ?
C51 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
C47 C53 C54 109.1(9) . . ?
C47 C53 H53A 109.9 . . ?
C54 C53 H53A 109.9 . . ?
C47 C53 H53B 109.9 . . ?
C54 C53 H53B 109.9 . . ?
H53A C53 H53B 108.3 . . ?
C56 C54 C55 110.9(10) . . ?
C56 C54 C53 108.9(9) . . ?
C55 C54 C53 108.5(8) . . ?
C56 C54 H54 109.5 . . ?
C55 C54 H54 109.5 . . ?
C53 C54 H54 109.5 . . ?
C49 C55 C54 110.0(9) . . ?
C49 C55 H55A 109.7 . . ?
C54 C55 H55A 109.7 . . ?
C49 C55 H55B 109.7 . . ?
C54 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C54 C56 C51 110.3(8) . . ?
C54 C56 H56A 109.6 . . ?
C51 C56 H56A 109.6 . . ?
C54 C56 H56B 109.6 . . ?
C51 C56 H56B 109.6 . . ?
H56A C56 H56B 108.1 . . ?
H9W O1W H10W 108.2 . . ?
H11W O2W H12W 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N22 Cd1 N1 C1 -168.3(10) 2_546 . . . ?
N16 Cd1 N1 C1 -73.7(10) 2_646 . . . ?
N7 Cd1 N1 C1 45(2) . . . . ?
O1 Cd1 N1 C1 17.8(10) . . . . ?
O2 Cd1 N1 C1 102.9(10) . . . . ?
N22 Cd1 N1 N2 24.6(9) 2_546 . . . ?
N16 Cd1 N1 N2 119.1(9) 2_646 . . . ?
N7 Cd1 N1 N2 -122.5(15) . . . . ?
O1 Cd1 N1 N2 -149.4(9) . . . . ?
O2 Cd1 N1 N2 -64.3(9) . . . . ?
C1 N1 N2 C2 7.1(14) . . . . ?
Cd1 N1 N2 C2 176.6(9) . . . . ?
C3 N4 N5 C4 0.3(14) . . . . ?
C3 N4 N5 Cd2 175.7(8) . . . 1_655 ?
N22 Cd1 N7 C15 -108.9(10) 2_546 . . . ?
N16 Cd1 N7 C15 157.0(10) 2_646 . . . ?
N1 Cd1 N7 C15 37(2) . . . . ?
O1 Cd1 N7 C15 64.2(10) . . . . ?
O2 Cd1 N7 C15 -21.4(10) . . . . ?
N22 Cd1 N7 N8 79.2(9) 2_546 . . . ?
N16 Cd1 N7 N8 -14.9(9) 2_646 . . . ?
N1 Cd1 N7 N8 -134.4(14) . . . . ?
O1 Cd1 N7 N8 -107.7(9) . . . . ?
O2 Cd1 N7 N8 166.7(9) . . . . ?
C15 N7 N8 C16 1.0(13) . . . . ?
Cd1 N7 N8 C16 174.1(8) . . . . ?
N19 Cd2 N10 C17 -150.3(9) . . . . ?
N5 Cd2 N10 C17 68.9(18) 1_455 . . . ?
N13 Cd2 N10 C17 -56.8(9) . . . . ?
O3 Cd2 N10 C17 35.2(9) . . . . ?
O4 Cd2 N10 C17 123.0(9) . . . . ?
N19 Cd2 N10 N11 30.8(8) . . . . ?
N5 Cd2 N10 N11 -110.0(14) 1_455 . . . ?
N13 Cd2 N10 N11 124.3(8) . . . . ?
O3 Cd2 N10 N11 -143.7(8) . . . . ?
O4 Cd2 N10 N11 -56.0(8) . . . . ?
C17 N10 N11 C18 -1.3(13) . . . . ?
Cd2 N10 N11 C18 177.8(8) . . . . ?
N19 Cd2 N13 C29 -46.2(8) . . . . ?
N10 Cd2 N13 C29 -134.8(7) . . . . ?
N5 Cd2 N13 C29 55.6(8) 1_455 . . . ?
O3 Cd2 N13 C29 141.4(7) . . . . ?
N19 Cd2 N13 N14 157.8(7) . . . . ?
N10 Cd2 N13 N14 69.1(8) . . . . ?
N5 Cd2 N13 N14 -100.4(7) 1_455 . . . ?
O3 Cd2 N13 N14 -14.6(7) . . . . ?
C29 N13 N14 C30 -0.8(10) . . . . ?
Cd2 N13 N14 C30 157.9(7) . . . . ?
C31 N16 N17 C32 1.4(11) . . . . ?
Cd1 N16 N17 C32 160.0(7) 2_656 . . . ?
N10 Cd2 N19 C43 -54.1(9) . . . . ?
N5 Cd2 N19 C43 117.6(9) 1_455 . . . ?
N13 Cd2 N19 C43 -154.4(9) . . . . ?
O3 Cd2 N19 C43 -22(2) . . . . ?
O4 Cd2 N19 C43 33.6(9) . . . . ?
N10 Cd2 N19 N20 133.8(8) . . . . ?
N5 Cd2 N19 N20 -54.5(8) 1_455 . . . ?
N13 Cd2 N19 N20 33.6(8) . . . . ?
O3 Cd2 N19 N20 166.0(12) . . . . ?
O4 Cd2 N19 N20 -138.4(8) . . . . ?
C43 N19 N20 C44 1.8(11) . . . . ?
Cd2 N19 N20 C44 175.6(7) . . . . ?
C45 N22 N23 C46 -2.1(12) . . . . ?
Cd1 N22 N23 C46 179.3(7) 2_556 . . . ?
N2 N1 C1 N3 -4.7(14) . . . . ?
Cd1 N1 C1 N3 -173.5(7) . . . . ?
C2 N3 C1 N1 0.5(14) . . . . ?
C5 N3 C1 N1 176.1(11) . . . . ?
N1 N2 C2 N3 -7.0(17) . . . . ?
C1 N3 C2 N2 4.2(16) . . . . ?
C5 N3 C2 N2 -171.5(11) . . . . ?
N5 N4 C3 N6 -1.2(15) . . . . ?
C4 N6 C3 N4 1.6(14) . . . . ?
C7 N6 C3 N4 -176.7(10) . . . . ?
N4 N5 C4 N6 0.7(13) . . . . ?
Cd2 N5 C4 N6 -174.6(7) 1_655 . . . ?
C3 N6 C4 N5 -1.4(13) . . . . ?
C7 N6 C4 N5 176.9(10) . . . . ?
C2 N3 C5 C6 -172.7(12) . . . . ?
C1 N3 C5 C6 12.7(16) . . . . ?
C2 N3 C5 C10 68.9(16) . . . . ?
C1 N3 C5 C10 -105.7(12) . . . . ?
C2 N3 C5 C11 -52.2(16) . . . . ?
C1 N3 C5 C11 133.2(12) . . . . ?
N3 C5 C6 C7 -178.2(9) . . . . ?
C10 C5 C6 C7 -61.3(11) . . . . ?
C11 C5 C6 C7 60.3(12) . . . . ?
C4 N6 C7 C8 119.9(12) . . . . ?
C3 N6 C7 C8 -62.2(13) . . . . ?
C4 N6 C7 C13 -117.9(12) . . . . ?
C3 N6 C7 C13 60.0(14) . . . . ?
C4 N6 C7 C6 0.7(15) . . . . ?
C3 N6 C7 C6 178.6(10) . . . . ?
C5 C6 C7 N6 -179.0(8) . . . . ?
C5 C6 C7 C8 61.6(11) . . . . ?
C5 C6 C7 C13 -60.6(11) . . . . ?
N6 C7 C8 C9 -178.3(8) . . . . ?
C13 C7 C8 C9 60.8(11) . . . . ?
C6 C7 C8 C9 -60.3(11) . . . . ?
C7 C8 C9 C14 -59.3(11) . . . . ?
C7 C8 C9 C10 60.8(11) . . . . ?
N3 C5 C10 C9 176.5(8) . . . . ?
C6 C5 C10 C9 59.4(11) . . . . ?
C11 C5 C10 C9 -61.7(12) . . . . ?
C14 C9 C10 C5 61.4(11) . . . . ?
C8 C9 C10 C5 -59.9(12) . . . . ?
N3 C5 C11 C12 -180.0(8) . . . . ?
C6 C5 C11 C12 -60.6(11) . . . . ?
C10 C5 C11 C12 60.6(11) . . . . ?
C5 C11 C12 C14 -58.9(11) . . . . ?
C5 C11 C12 C13 61.6(11) . . . . ?
N6 C7 C13 C12 178.3(8) . . . . ?
C8 C7 C13 C12 -60.4(12) . . . . ?
C6 C7 C13 C12 60.7(11) . . . . ?
C14 C12 C13 C7 58.2(11) . . . . ?
C11 C12 C13 C7 -62.2(12) . . . . ?
C8 C9 C14 C12 59.5(12) . . . . ?
C10 C9 C14 C12 -62.2(12) . . . . ?
C11 C12 C14 C9 61.4(12) . . . . ?
C13 C12 C14 C9 -58.9(11) . . . . ?
N8 N7 C15 N9 -1.1(13) . . . . ?
Cd1 N7 C15 N9 -174.1(7) . . . . ?
C16 N9 C15 N7 0.8(13) . . . . ?
C19 N9 C15 N7 174.5(10) . . . . ?
N7 N8 C16 N9 -0.5(14) . . . . ?
C15 N9 C16 N8 -0.2(14) . . . . ?
C19 N9 C16 N8 -173.9(10) . . . . ?
N11 N10 C17 N12 1.0(12) . . . . ?
Cd2 N10 C17 N12 -178.0(7) . . . . ?
C18 N12 C17 N10 -0.4(12) . . . . ?
C21 N12 C17 N10 177.5(10) . . . . ?
N10 N11 C18 N12 1.0(13) . . . . ?
C17 N12 C18 N11 -0.4(13) . . . . ?
C21 N12 C18 N11 -178.3(10) . . . . ?
C16 N9 C19 C24 71.1(15) . . . . ?
C15 N9 C19 C24 -101.0(13) . . . . ?
C16 N9 C19 C25 -50.6(15) . . . . ?
C15 N9 C19 C25 137.3(11) . . . . ?
C16 N9 C19 C20 -170.4(11) . . . . ?
C15 N9 C19 C20 17.5(16) . . . . ?
N9 C19 C20 C21 179.4(9) . . . . ?
C24 C19 C20 C21 -62.1(11) . . . . ?
C25 C19 C20 C21 59.6(12) . . . . ?
C17 N12 C21 C27 -128.4(11) . . . . ?
C18 N12 C21 C27 49.0(15) . . . . ?
C17 N12 C21 C22 112.6(11) . . . . ?
C18 N12 C21 C22 -70.0(13) . . . . ?
C17 N12 C21 C20 -5.5(15) . . . . ?
C18 N12 C21 C20 171.9(10) . . . . ?
C19 C20 C21 N12 179.2(8) . . . . ?
C19 C20 C21 C27 -57.4(12) . . . . ?
C19 C20 C21 C22 61.7(11) . . . . ?
N12 C21 C22 C23 -179.1(8) . . . . ?
C27 C21 C22 C23 59.8(11) . . . . ?
C20 C21 C22 C23 -60.7(11) . . . . ?
C21 C22 C23 C28 -59.8(12) . . . . ?
C21 C22 C23 C24 60.1(12) . . . . ?
N9 C19 C24 C23 179.0(9) . . . . ?
C25 C19 C24 C23 -60.1(12) . . . . ?
C20 C19 C24 C23 60.9(11) . . . . ?
C28 C23 C24 C19 58.7(12) . . . . ?
C22 C23 C24 C19 -60.6(12) . . . . ?
N9 C19 C25 C26 -179.0(9) . . . . ?
C24 C19 C25 C26 60.4(11) . . . . ?
C20 C19 C25 C26 -60.1(12) . . . . ?
C19 C25 C26 C27 60.0(13) . . . . ?
C19 C25 C26 C28 -59.6(12) . . . . ?
C28 C26 C27 C21 62.8(12) . . . . ?
C25 C26 C27 C21 -58.3(13) . . . . ?
N12 C21 C27 C26 178.9(9) . . . . ?
C22 C21 C27 C26 -62.4(12) . . . . ?
C20 C21 C27 C26 56.9(12) . . . . ?
C27 C26 C28 C23 -61.9(11) . . . . ?
C25 C26 C28 C23 59.7(12) . . . . ?
C22 C23 C28 C26 61.0(12) . . . . ?
C24 C23 C28 C26 -58.6(12) . . . . ?
N14 N13 C29 N15 2.4(11) . . . . ?
Cd2 N13 C29 N15 -158.6(6) . . . . ?
C30 N15 C29 N13 -3.0(11) . . . . ?
C33 N15 C29 N13 179.8(8) . . . . ?
C29 N15 C30 N14 2.4(11) . . . . ?
C33 N15 C30 N14 179.4(9) . . . . ?
N13 N14 C30 N15 -1.1(11) . . . . ?
N17 N16 C31 N18 -1.5(11) . . . . ?
Cd1 N16 C31 N18 -160.0(6) 2_656 . . . ?
C32 N18 C31 N16 1.0(11) . . . . ?
C35 N18 C31 N16 179.5(9) . . . . ?
N16 N17 C32 N18 -0.8(11) . . . . ?
C31 N18 C32 N17 -0.1(11) . . . . ?
C35 N18 C32 N17 -178.4(9) . . . . ?
C30 N15 C33 C38 134.5(10) . . . . ?
C29 N15 C33 C38 -49.1(12) . . . . ?
C30 N15 C33 C34 -105.9(11) . . . . ?
C29 N15 C33 C34 70.5(12) . . . . ?
C30 N15 C33 C39 16.0(13) . . . . ?
C29 N15 C33 C39 -167.7(8) . . . . ?
N15 C33 C34 C35 180.0(8) . . . . ?
C38 C33 C34 C35 -61.6(11) . . . . ?
C39 C33 C34 C35 59.4(11) . . . . ?
C31 N18 C35 C36 -176.4(9) . . . . ?
C32 N18 C35 C36 1.6(13) . . . . ?
C31 N18 C35 C41 -53.6(12) . . . . ?
C32 N18 C35 C41 124.4(10) . . . . ?
C31 N18 C35 C34 65.5(12) . . . . ?
C32 N18 C35 C34 -116.5(11) . . . . ?
C33 C34 C35 N18 -179.0(8) . . . . ?
C33 C34 C35 C36 61.6(11) . . . . ?
C33 C34 C35 C41 -59.5(11) . . . . ?
N18 C35 C36 C37 -178.9(8) . . . . ?
C41 C35 C36 C37 58.9(11) . . . . ?
C34 C35 C36 C37 -61.1(11) . . . . ?
C35 C36 C37 C42 -58.4(11) . . . . ?
C35 C36 C37 C38 60.8(11) . . . . ?
N15 C33 C38 C37 179.1(8) . . . . ?
C34 C33 C38 C37 58.8(10) . . . . ?
C39 C33 C38 C37 -63.0(10) . . . . ?
C36 C37 C38 C33 -58.9(11) . . . . ?
C42 C37 C38 C33 62.4(11) . . . . ?
N15 C33 C39 C40 179.2(8) . . . . ?
C38 C33 C39 C40 61.9(10) . . . . ?
C34 C33 C39 C40 -59.0(10) . . . . ?
C33 C39 C40 C42 -61.6(10) . . . . ?
C33 C39 C40 C41 60.3(11) . . . . ?
C42 C40 C41 C35 58.9(11) . . . . ?
C39 C40 C41 C35 -62.4(11) . . . . ?
N18 C35 C41 C40 178.9(8) . . . . ?
C36 C35 C41 C40 -58.7(11) . . . . ?
C34 C35 C41 C40 60.6(10) . . . . ?
C41 C40 C42 C37 -58.3(11) . . . . ?
C39 C40 C42 C37 63.4(11) . . . . ?
C36 C37 C42 C40 58.3(12) . . . . ?
C38 C37 C42 C40 -62.7(11) . . . . ?
N20 N19 C43 N21 -1.8(12) . . . . ?
Cd2 N19 C43 N21 -174.8(7) . . . . ?
C44 N21 C43 N19 1.0(12) . . . . ?
C47 N21 C43 N19 172.7(9) . . . . ?
N19 N20 C44 N21 -1.3(12) . . . . ?
C43 N21 C44 N20 0.3(12) . . . . ?
C47 N21 C44 N20 -171.5(9) . . . . ?
N23 N22 C45 N24 1.8(13) . . . . ?
Cd1 N22 C45 N24 -179.8(7) 2_556 . . . ?
C46 N24 C45 N22 -0.7(13) . . . . ?
C49 N24 C45 N22 171.7(9) . . . . ?
N22 N23 C46 N24 1.8(13) . . . . ?
C45 N24 C46 N23 -0.8(13) . . . . ?
C49 N24 C46 N23 -173.7(9) . . . . ?
C44 N21 C47 C53 169.9(10) . . . . ?
C43 N21 C47 C53 0.2(14) . . . . ?
C44 N21 C47 C52 -66.6(13) . . . . ?
C43 N21 C47 C52 123.7(11) . . . . ?
C44 N21 C47 C48 50.8(14) . . . . ?
C43 N21 C47 C48 -118.9(11) . . . . ?
N21 C47 C48 C49 179.6(8) . . . . ?
C53 C47 C48 C49 59.4(12) . . . . ?
C52 C47 C48 C49 -61.1(11) . . . . ?
C45 N24 C49 C55 119.8(12) . . . . ?
C46 N24 C49 C55 -69.3(13) . . . . ?
C45 N24 C49 C48 -119.8(12) . . . . ?
C46 N24 C49 C48 51.1(14) . . . . ?
C45 N24 C49 C50 -2.3(15) . . . . ?
C46 N24 C49 C50 168.5(10) . . . . ?
C47 C48 C49 N24 179.1(8) . . . . ?
C47 C48 C49 C55 -59.1(11) . . . . ?
C47 C48 C49 C50 61.0(12) . . . . ?
N24 C49 C50 C51 -176.5(8) . . . . ?
C55 C49 C50 C51 59.7(11) . . . . ?
C48 C49 C50 C51 -60.7(11) . . . . ?
C49 C50 C51 C56 -58.7(11) . . . . ?
C49 C50 C51 C52 60.5(11) . . . . ?
N21 C47 C52 C51 177.4(8) . . . . ?
C53 C47 C52 C51 -58.9(12) . . . . ?
C48 C47 C52 C51 60.8(11) . . . . ?
C50 C51 C52 C47 -61.4(12) . . . . ?
C56 C51 C52 C47 58.0(12) . . . . ?
N21 C47 C53 C54 -177.2(8) . . . . ?
C52 C47 C53 C54 59.1(11) . . . . ?
C48 C47 C53 C54 -59.7(10) . . . . ?
C47 C53 C54 C56 -60.3(11) . . . . ?
C47 C53 C54 C55 60.5(11) . . . . ?
N24 C49 C55 C54 178.7(8) . . . . ?
C48 C49 C55 C54 60.6(11) . . . . ?
C50 C49 C55 C54 -59.0(11) . . . . ?
C56 C54 C55 C49 59.1(11) . . . . ?
C53 C54 C55 C49 -60.5(12) . . . . ?
C55 C54 C56 C51 -58.3(12) . . . . ?
C53 C54 C56 C51 61.0(12) . . . . ?
C50 C51 C56 C54 58.5(13) . . . . ?
C52 C51 C56 C54 -60.5(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.203

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk2010_12 in P2(1)/n
CELL 0.71073 14.7635 29.4568 17.5708 90.000 90.031 90.000
ZERR 4.00 0.0012 0.0033 0.0016 0.000 0.008 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H N O BR CD
UNIT 224 336 96 24 32 16
MERG 2
OMIT 0.00 180.00
OMIT 0 1 1
OMIT 0 2 0
OMIT 0 2 1
OMIT -8 11 12
TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2
SHEL 0.81 6
FMAP 2
PLAN 20
SIZE 0.19 0.22 0.26
ACTA
BOND
BOND $H
CONF
LIST 4
L.S. 4
TEMP -100.00
WGHT 0.000000
EXTI 0.000257
BASF 0.56494
FVAR 0.10299
CD1 6 0.772230 0.034955 0.738414 11.00000 0.03758 0.02422 =
0.02551 0.00169 0.00108 0.00094
CD2 6 0.265694 0.213011 0.766823 11.00000 0.03314 0.02490 =
0.02240 0.00182 0.00029 -0.00201
CD3 6 0.793816 0.238979 0.741993 11.00000 0.05250 0.03947 =
0.04248 -0.00331 -0.00487 0.00547
CD4 6 0.279860 0.013644 0.733938 11.00000 0.05037 0.03108 =
0.04217 0.00203 0.00719 -0.00090
BR1 5 0.734073 0.196089 0.863172 11.00000 0.11634 0.05683 =
0.03324 0.00007 0.00825 0.01032
BR2 5 0.756796 0.187787 0.627510 11.00000 0.10636 0.05636 =
0.04404 -0.01943 0.00124 0.00301
BR3 5 0.962856 0.256431 0.762527 11.00000 0.05570 0.08503 =
0.15982 0.01492 -0.03483 0.00166
BR4 5 0.716931 0.315140 0.712408 11.00000 0.04781 0.03795 =
0.04671 -0.00637 -0.00635 0.00606
BR5 5 0.259218 0.058497 0.861152 11.00000 0.10452 0.04430 =
0.03404 0.00098 0.00765 -0.00112
BR6 5 0.219842 0.062131 0.620019 11.00000 0.07570 0.05585 =
0.03810 0.00560 -0.00328 0.00228
BR7 5 0.188864 -0.059941 0.746381 11.00000 0.06957 0.03704 =
0.09152 -0.00922 0.03113 -0.01131
BR8 5 0.448881 0.000210 0.707931 11.00000 0.05397 0.08445 =
0.09526 0.02297 0.02088 0.01032
O1 4 0.829830 0.108463 0.766111 11.00000 0.12205 0.05269 =
0.05253 -0.00771 0.02211 -0.01239
AFIX 3
H1W 2 0.810370 0.125453 0.801621 11.00000 -1.50000
H2W 2 0.818921 0.121643 0.724061 11.00000 -1.50000
AFIX 0
O2 4 0.634971 0.073466 0.708299 11.00000 0.11775 0.12725 =
0.05147 -0.01623 -0.03326 0.07868
AFIX 3
H3W 2 0.592481 0.054016 0.706429 11.00000 -1.50000
H4W 2 0.614351 0.097476 0.728779 11.00000 -1.50000
AFIX 0
O3 4 0.316510 0.138873 0.736450 11.00000 0.08734 0.02918 =
0.04396 -0.00528 -0.00786 -0.00832
AFIX 3
H5W 2 0.307790 0.122923 0.776080 11.00000 -1.50000
H6W 2 0.295400 0.124333 0.698610 11.00000 -1.50000
AFIX 0
O4 4 0.122022 0.179669 0.799274 11.00000 0.04210 0.04278 =
0.05082 0.01431 0.00097 -0.00965
AFIX 3
H7W 2 0.102802 0.155009 0.780003 11.00000 -1.50000
H8W 2 0.082882 0.200239 0.790934 11.00000 -1.50000
AFIX 0
N1 3 0.827538 0.050927 0.617976 11.00000 0.05491 0.02851 =
0.02249 0.00075 -0.00819 -0.01491
N2 3 0.789909 0.034286 0.552334 11.00000 0.08277 0.07030 =
0.03100 -0.00827 0.00660 -0.03901
N3 3 0.894225 0.083822 0.521893 11.00000 0.04847 0.03416 =
0.02256 -0.00052 -0.00050 -0.02328
N4 3 1.243184 0.240727 0.586062 11.00000 0.07448 0.06421 =
0.03297 0.00865 -0.01967 -0.04832
N5 3 1.208177 0.215004 0.643802 11.00000 0.04524 0.04729 =
0.01684 0.00876 -0.01029 -0.02082
N6 3 1.132853 0.197333 0.542102 11.00000 0.03648 0.03461 =
0.02034 0.01003 -0.00040 -0.00510
N7 3 0.713669 0.035695 0.862325 11.00000 0.04649 0.04941 =
0.03304 0.00481 -0.00155 0.01123
N8 3 0.746164 0.010796 0.921172 11.00000 0.07318 0.03902 =
0.03998 0.00925 0.00535 0.02014
N9 3 0.640216 0.057052 0.965297 11.00000 0.04508 0.03634 =
0.03488 0.01567 0.00889 0.00622
N10 3 0.314181 0.194147 0.886143 11.00000 0.04367 0.03676 =
0.02482 -0.00549 0.00550 0.00177
N11 3 0.270171 0.207992 0.951250 11.00000 0.03336 0.06546 =
0.02440 0.00593 0.00168 0.01604
N12 3 0.387670 0.164846 0.981432 11.00000 0.03602 0.03749 =
0.01199 0.00116 0.00424 0.00940
N13 3 0.395614 0.247084 0.718921 11.00000 0.02431 0.03027 =
0.02906 0.00519 -0.00851 -0.00582
N14 3 0.477952 0.228119 0.700108 11.00000 0.03050 0.02913 =
0.04029 0.00104 0.00434 0.00068
N15 3 0.462584 0.292235 0.636996 11.00000 0.02619 0.01669 =
0.02195 0.00282 0.00379 0.00616
N16 3 0.602508 0.499627 0.710578 11.00000 0.03592 0.02321 =
0.04761 -0.00520 -0.00242 0.00920
N17 3 0.524104 0.522606 0.687776 11.00000 0.04003 0.02591 =
0.03963 -0.00056 -0.00097 0.00207
N18 3 0.530460 0.455741 0.631295 11.00000 0.02737 0.01674 =
0.03040 0.00122 0.00096 -0.00286
N19 3 0.210889 0.278685 0.816566 11.00000 0.03090 0.02152 =
0.05496 0.00068 0.00553 -0.00039
N20 3 0.225558 0.320470 0.781922 11.00000 0.03076 0.03940 =
0.03697 0.00210 0.00810 0.01185
N21 3 0.133948 0.330454 0.880604 11.00000 0.02509 0.02707 =
0.02660 0.00842 0.00297 0.00415
N22 3 -0.210838 0.470233 0.808306 11.00000 0.04384 0.02089 =
0.03921 0.00404 -0.01048 0.00773
N23 3 -0.224159 0.428556 0.773279 11.00000 0.05711 0.01884 =
0.05825 -0.00319 -0.01670 0.01032
N24 3 -0.139180 0.419952 0.875466 11.00000 0.02328 0.03563 =
0.02465 -0.00472 0.00322 0.01166
C1 1 0.884767 0.080949 0.598706 11.00000 0.06468 0.03963 =
0.02247 0.00522 0.00831 -0.02140
AFIX 43
H1 2 0.917219 0.099282 0.633866 11.00000 -1.20000
AFIX 0
C2 1 0.835882 0.052483 0.496241 11.00000 0.12433 0.05852 =
0.04731 -0.01020 0.01781 -0.05892
AFIX 43
H2 2 0.828761 0.044492 0.444199 11.00000 -1.20000
AFIX 0
C3 1 1.197375 0.230273 0.526788 11.00000 0.06861 0.06767 =
0.03442 0.01672 -0.01429 -0.04155
AFIX 43
H3 2 1.206484 0.243505 0.478083 11.00000 -1.20000
AFIX 0
C4 1 1.142187 0.189595 0.616992 11.00000 0.05178 0.03870 =
0.03483 0.01379 -0.01308 -0.02652
AFIX 43
H4 2 1.106729 0.169014 0.646048 11.00000 -1.20000
AFIX 0
C5 1 0.950249 0.116378 0.476450 11.00000 0.03376 0.04146 =
0.01260 -0.00378 0.00760 -0.00670
C6 1 1.013743 0.140386 0.530529 11.00000 0.03744 0.03710 =
0.01524 0.00489 0.00176 -0.00268
AFIX 23
H6A 2 1.054131 0.117971 0.555264 11.00000 -1.20000
H6B 2 0.978380 0.155890 0.570714 11.00000 -1.20000
AFIX 0
C7 1 1.070559 0.175256 0.486782 11.00000 0.03963 0.04981 =
0.01411 -0.00300 -0.00018 -0.00539
C8 1 1.008398 0.210709 0.451464 11.00000 0.01881 0.03648 =
0.03706 0.00903 -0.00920 -0.00135
AFIX 23
H8A 2 1.044586 0.233557 0.423500 11.00000 -1.20000
H8B 2 0.973622 0.226476 0.491723 11.00000 -1.20000
AFIX 0
C9 1 0.943864 0.186493 0.397006 11.00000 0.02295 0.04669 =
0.05460 0.02626 0.00138 0.00278
AFIX 13
H9 2 0.903212 0.209446 0.372665 11.00000 -1.20000
AFIX 0
C10 1 0.885002 0.151045 0.439948 11.00000 0.02817 0.06681 =
0.02285 0.00681 -0.00470 0.00012
AFIX 23
H10A 2 0.848326 0.166175 0.479699 11.00000 -1.20000
H10B 2 0.843486 0.135579 0.404075 11.00000 -1.20000
AFIX 0
C11 1 1.005452 0.091547 0.414451 11.00000 0.03068 0.04261 =
0.04754 -0.00074 -0.00227 -0.01251
AFIX 23
H11A 2 1.046473 0.069017 0.438135 11.00000 -1.20000
H11B 2 0.964197 0.075379 0.379242 11.00000 -1.20000
AFIX 0
C12 1 1.060547 0.127133 0.370914 11.00000 0.04020 0.07411 =
0.01094 -0.00239 0.00701 0.00091
AFIX 13
H12 2 1.095738 0.111852 0.329596 11.00000 -1.20000
AFIX 0
C13 1 1.126579 0.150884 0.425870 11.00000 0.02605 0.04536 =
0.03303 0.00769 0.00332 -0.00958
AFIX 23
H13A 2 1.167077 0.128253 0.449914 11.00000 -1.20000
H13B 2 1.164350 0.173033 0.397806 11.00000 -1.20000
AFIX 0
C14 1 0.996637 0.162099 0.335727 11.00000 0.04878 0.07253 =
0.01966 -0.00146 0.01038 -0.01639
AFIX 23
H14A 2 1.032119 0.184394 0.305933 11.00000 -1.20000
H14B 2 0.954092 0.146690 0.300644 11.00000 -1.20000
AFIX 0
C15 1 0.651822 0.063337 0.888689 11.00000 0.06499 0.04488 =
0.01880 0.00767 0.00605 0.02284
AFIX 43
H15 2 0.619458 0.084790 0.858837 11.00000 -1.20000
AFIX 0
C16 1 0.700986 0.024171 0.980950 11.00000 0.06504 0.05486 =
0.03710 0.01565 0.00849 0.02721
AFIX 43
H16 2 0.710000 0.011983 1.030435 11.00000 -1.20000
AFIX 0
C17 1 0.384614 0.168860 0.904531 11.00000 0.05251 0.03555 =
0.01499 0.00142 0.00366 0.00958
AFIX 43
H17 2 0.426239 0.155665 0.869755 11.00000 -1.20000
AFIX 0
C18 1 0.315964 0.189254 1.007522 11.00000 0.06010 0.07849 =
0.00940 0.01063 0.00393 0.02915
AFIX 43
H18 2 0.300747 0.192415 1.059780 11.00000 -1.20000
AFIX 0
C19 1 0.582485 0.083705 1.019200 11.00000 0.02926 0.05132 =
0.01462 0.00717 0.01100 0.01502
C20 1 0.513159 0.111169 0.972403 11.00000 0.04131 0.03648 =
0.01800 0.00793 0.00142 0.01488
AFIX 23
H20A 2 0.545289 0.132066 0.937510 11.00000 -1.20000
H20B 2 0.475688 0.090309 0.941397 11.00000 -1.20000
AFIX 0
C21 1 0.452603 0.138320 1.026178 11.00000 0.02976 0.03654 =
0.01308 0.00360 -0.01529 0.00482
C22 1 0.511247 0.171478 1.070941 11.00000 0.05693 0.03972 =
0.02411 0.01087 0.00311 0.00637
AFIX 23
H22A 2 0.472885 0.189826 1.105412 11.00000 -1.20000
H22B 2 0.542740 0.192333 1.035573 11.00000 -1.20000
AFIX 0
C23 1 0.581393 0.144297 1.117743 11.00000 0.05891 0.04834 =
0.04330 -0.01704 -0.02419 0.01246
AFIX 13
H23 2 0.620164 0.165686 1.147626 11.00000 -1.20000
AFIX 0
C24 1 0.641495 0.116093 1.062900 11.00000 0.04380 0.03944 =
0.03796 0.00878 -0.01484 0.00170
AFIX 23
H24A 2 0.673485 0.136573 1.027232 11.00000 -1.20000
H24B 2 0.687407 0.098982 1.092308 11.00000 -1.20000
AFIX 0
C25 1 0.533084 0.051480 1.072628 11.00000 0.04902 0.03915 =
0.02530 0.00473 0.00750 0.00620
AFIX 23
H25A 2 0.577369 0.033623 1.102547 11.00000 -1.20000
H25B 2 0.495158 0.030138 1.042962 11.00000 -1.20000
AFIX 0
C26 1 0.473376 0.079775 1.126143 11.00000 0.06176 0.03784 =
0.03074 0.01175 0.02044 0.01656
AFIX 13
H26 2 0.440871 0.058991 1.161891 11.00000 -1.20000
AFIX 0
C27 1 0.405118 0.107089 1.082272 11.00000 0.04588 0.05226 =
0.03021 0.00625 0.01079 0.01263
AFIX 23
H27A 2 0.368262 0.125381 1.117965 11.00000 -1.20000
H27B 2 0.363967 0.086393 1.054411 11.00000 -1.20000
AFIX 0
C28 1 0.531146 0.112710 1.171828 11.00000 0.09010 0.05781 =
0.03258 -0.00022 -0.00716 0.04504
AFIX 23
H28A 2 0.575186 0.095638 1.203252 11.00000 -1.20000
H28B 2 0.492134 0.130707 1.206303 11.00000 -1.20000
AFIX 0
C29 1 0.390653 0.284723 0.682224 11.00000 0.02352 0.01892 =
0.03864 0.00755 0.00147 -0.00064
AFIX 43
H29 2 0.341184 0.305182 0.686589 11.00000 -1.20000
AFIX 0
C30 1 0.516203 0.257198 0.650832 11.00000 0.03378 0.03285 =
0.03289 -0.00344 0.00713 -0.01481
AFIX 43
H30 2 0.574348 0.253135 0.628722 11.00000 -1.20000
AFIX 0
C31 1 0.604915 0.461050 0.675793 11.00000 0.01861 0.02569 =
0.03932 0.00271 -0.00786 0.00206
AFIX 43
H31 2 0.652223 0.439380 0.680655 11.00000 -1.20000
AFIX 0
C32 1 0.482637 0.495065 0.640884 11.00000 0.03327 0.02550 =
0.03910 -0.00010 -0.00494 0.00477
AFIX 43
H32 2 0.426577 0.501549 0.616644 11.00000 -1.20000
AFIX 0
C33 1 0.476770 0.332429 0.587414 11.00000 0.02275 0.02315 =
0.02074 0.00835 0.00688 0.00062
C34 1 0.495890 0.374436 0.635028 11.00000 0.03379 0.01835 =
0.02175 -0.00571 0.00014 0.00821
AFIX 23
H34A 2 0.550648 0.369423 0.666471 11.00000 -1.20000
H34B 2 0.444276 0.380301 0.669606 11.00000 -1.20000
AFIX 0
C35 1 0.510502 0.415799 0.582497 11.00000 0.03549 0.01606 =
0.02784 -0.00374 0.00459 -0.00538
C36 1 0.424905 0.423497 0.538013 11.00000 0.04491 0.03704 =
0.03484 0.01505 -0.00626 -0.00314
AFIX 23
H36A 2 0.374009 0.429206 0.573404 11.00000 -1.20000
H36B 2 0.431978 0.450488 0.504974 11.00000 -1.20000
AFIX 0
C37 1 0.404563 0.382556 0.490071 11.00000 0.04747 0.03967 =
0.02070 -0.00246 -0.00059 0.00755
AFIX 13
H37 2 0.348158 0.388192 0.459984 11.00000 -1.20000
AFIX 0
C38 1 0.390612 0.339554 0.541696 11.00000 0.03816 0.02276 =
0.02689 -0.00538 -0.00205 0.00543
AFIX 23
H38A 2 0.338575 0.344247 0.576327 11.00000 -1.20000
H38B 2 0.378152 0.312577 0.509760 11.00000 -1.20000
AFIX 0
C39 1 0.557309 0.322281 0.532274 11.00000 0.03361 0.04042 =
0.01391 -0.01139 0.00096 0.01299
AFIX 23
H39A 2 0.613412 0.316498 0.561599 11.00000 -1.20000
H39B 2 0.543873 0.295174 0.500931 11.00000 -1.20000
AFIX 0
C40 1 0.569241 0.364639 0.480753 11.00000 0.05222 0.02977 =
0.02390 0.00703 0.01098 0.00645
AFIX 13
H40 2 0.620841 0.359142 0.445078 11.00000 -1.20000
AFIX 0
C41 1 0.590663 0.406415 0.529280 11.00000 0.04261 0.02552 =
0.02843 0.00860 0.00162 -0.00580
AFIX 23
H41A 2 0.601306 0.433008 0.496011 11.00000 -1.20000
H41B 2 0.646170 0.400973 0.559572 11.00000 -1.20000
AFIX 0
C42 1 0.483937 0.372125 0.434666 11.00000 0.10659 0.02644 =
0.00899 0.00401 -0.00879 -0.01408
AFIX 23
H42A 2 0.469981 0.344644 0.404419 11.00000 -1.20000
H42B 2 0.492602 0.397853 0.399156 11.00000 -1.20000
AFIX 0
C43 1 0.155598 0.286363 0.873208 11.00000 0.02930 0.03749 =
0.04725 0.02543 0.00365 0.00740
AFIX 43
H43 2 0.133086 0.263205 0.905728 11.00000 -1.20000
AFIX 0
C44 1 0.179257 0.349463 0.822993 11.00000 0.04105 0.01963 =
0.05303 -0.00172 0.00654 0.00036
AFIX 43
H44 2 0.178015 0.381122 0.812741 11.00000 -1.20000
AFIX 0
C45 1 -0.162227 0.463393 0.868311 11.00000 0.06648 0.03866 =
0.04173 -0.01897 -0.01581 0.03575
AFIX 43
H45 2 -0.145031 0.486540 0.903083 11.00000 -1.20000
AFIX 0
C46 1 -0.178633 0.400410 0.815226 11.00000 0.06003 0.03284 =
0.05430 -0.00716 -0.03136 0.00968
AFIX 43
H46 2 -0.173760 0.368928 0.804233 11.00000 -1.20000
AFIX 0
C47 1 0.067018 0.351445 0.931468 11.00000 0.02550 0.02738 =
0.02354 -0.00363 -0.00057 0.01239
C48 1 -0.003671 0.375258 0.879670 11.00000 0.01052 0.04430 =
0.01640 -0.00096 -0.00870 0.00642
AFIX 23
H48A 2 0.026765 0.398453 0.847928 11.00000 -1.20000
H48B 2 -0.031978 0.352682 0.845358 11.00000 -1.20000
AFIX 0
C49 1 -0.076491 0.397766 0.928575 11.00000 0.03602 0.03306 =
0.02181 0.00026 -0.01148 0.00903
C50 1 -0.031293 0.433724 0.979874 11.00000 0.05646 0.02407 =
0.02766 -0.00662 0.00100 0.01056
AFIX 23
H50A 2 -0.000914 0.456885 0.948024 11.00000 -1.20000
H50B 2 -0.077822 0.449109 1.011172 11.00000 -1.20000
AFIX 0
C51 1 0.038287 0.410564 1.031688 11.00000 0.02785 0.03959 =
0.03678 -0.01820 -0.00122 -0.00270
AFIX 13
H51 2 0.067351 0.433614 1.065603 11.00000 -1.20000
AFIX 0
C52 1 0.111024 0.387571 0.981580 11.00000 0.03669 0.03620 =
0.03550 0.00435 0.00414 -0.01055
AFIX 23
H52A 2 0.140980 0.410625 0.949233 11.00000 -1.20000
H52B 2 0.157693 0.373393 1.014342 11.00000 -1.20000
AFIX 0
C53 1 0.020087 0.316040 0.979796 11.00000 0.03184 0.03817 =
0.02871 0.02025 -0.00480 0.00268
AFIX 23
H53A 2 0.064845 0.300624 1.012867 11.00000 -1.20000
H53B 2 -0.008535 0.292924 0.946701 11.00000 -1.20000
AFIX 0
C54 1 -0.054276 0.339939 1.030194 11.00000 0.03902 0.05418 =
0.02674 0.01966 0.00439 -0.00742
AFIX 13
H54 2 -0.085608 0.316727 1.062300 11.00000 -1.20000
AFIX 0
C55 1 -0.123060 0.362651 0.977430 11.00000 0.03751 0.04060 =
0.01449 0.00792 0.00914 0.00604
AFIX 23
H55A 2 -0.151840 0.339464 0.944572 11.00000 -1.20000
H55B 2 -0.171060 0.377333 1.008102 11.00000 -1.20000
AFIX 0
C56 1 -0.009391 0.374094 1.080260 11.00000 0.04845 0.06935 =
0.01932 0.00207 -0.00239 0.00702
AFIX 23
H56A 2 0.035574 0.358774 1.113260 11.00000 -1.20000
H56B 2 -0.055189 0.388654 1.113375 11.00000 -1.20000
AFIX 0
O1W 4 0.549690 0.147905 0.777101 11.00000 0.13938 0.10223 =
0.04860 0.02045 0.01658 0.07651
AFIX 3
H9W 2 0.596450 0.157865 0.799871 11.00000 -1.50000
H10W 2 0.525410 0.169835 0.753161 11.00000 -1.50000
AFIX 0
O2W 4 0.050224 0.100710 0.733478 11.00000 0.07988 0.04147 =
0.05798 0.01103 0.00486 -0.00230
AFIX 3
H11W 2 0.092874 0.091350 0.705038 11.00000 -1.50000
H12W 2 0.028074 0.078031 0.756888 11.00000 -1.50000
HKLF 4

REM dk2010_12 in P2(1)/n
REM R1 = 0.0540 for 8284 Fo > 4sig(Fo) and 0.1274 for all 14439 data
REM 885 parameters refined using 0 restraints

END

WGHT 0.0000 0.0000
REM Highest difference peak 1.572, deepest hole -1.257, 1-sigma level 0.203
Q1 1 0.2783 0.2142 0.8037 11.00000 0.05 1.57
Q2 1 0.2007 0.2141 0.7780 11.00000 0.05 1.43
Q3 1 0.8374 0.0348 0.7237 11.00000 0.05 1.28
Q4 1 0.7819 0.0351 0.7777 11.00000 0.05 1.25
Q5 1 0.9594 0.2258 0.7383 11.00000 0.05 1.17
Q6 1 0.1826 -0.0807 0.7393 11.00000 0.05 1.16
Q7 1 0.2155 0.0155 0.7409 11.00000 0.05 1.11
Q8 1 0.3273 0.2161 0.7535 11.00000 0.05 1.11
Q9 1 0.2427 0.1922 0.7574 11.00000 0.05 1.07
Q10 1 0.2580 0.2140 0.7219 11.00000 0.05 1.07

;

#---------------------------------------------------------

data_(2)
_database_code_depnum_ccdc_archive 'CCDC 867225'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetrakis-[1,3-di(1,2,4-triazol-4-yl)adamantane]cadmium(II)
bis-triiodocadmate(II) Tetrahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H72 Cd3 I6 N24, 4(H2 O)'
_chemical_formula_sum            'C56 H80 Cd3 I6 N24 O4'
_chemical_formula_weight         2252.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3397(2)
_cell_length_b                   11.3871(2)
_cell_length_c                   17.8908(5)
_cell_angle_alpha                95.6320(10)
_cell_angle_beta                 102.9610(10)
_cell_angle_gamma                115.4300(10)
_cell_volume                     1808.07(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    26667
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      29.57

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1078
_exptl_absorpt_coefficient_mu    3.496
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2738
_exptl_absorpt_correction_T_max  0.5415
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            26667
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         29.57
_reflns_number_total             10023
_reflns_number_gt                8815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The refinement was standard. All non-hydrogen atoms were refined
anisotropically. The CH-hydrogen atoms were constrained with U(iso) =
1.2U(eq) of the parent C-atom and with C-H distances 0.93 A (triazole),
0.97 A (CH2 adamantane) and 0.98 (CH adamantane). The OH-hydrogen atoms
were located and then constrained with O-H distances set to 0.85 A and
U(iso) = 1.5U(eq) of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+3.2317P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10023
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0604
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.0000 0.5000 0.5000 0.01530(5) Uani 1 2 d S . .
Cd2 Cd 0.83966(2) -0.088048(19) -0.168246(12) 0.02081(5) Uani 1 1 d . . .
I1 I 0.70059(2) -0.10117(2) -0.320986(12) 0.03060(5) Uani 1 1 d . . .
I2 I 0.78677(2) -0.332303(18) -0.135481(12) 0.02430(5) Uani 1 1 d . . .
I3 I 1.14433(2) 0.07744(2) -0.124909(16) 0.03978(6) Uani 1 1 d . . .
N1 N 0.7855(3) 0.5165(2) 0.44643(14) 0.0225(5) Uani 1 1 d . . .
N2 N 0.6696(3) 0.4137(2) 0.38743(17) 0.0329(6) Uani 1 1 d . . .
N3 N 0.6340(2) 0.5914(2) 0.39172(14) 0.0200(4) Uani 1 1 d . . .
N4 N 0.8471(3) 1.2683(2) 0.49479(14) 0.0210(4) Uani 1 1 d . . .
N5 N 0.9051(3) 1.2089(2) 0.54672(14) 0.0237(5) Uani 1 1 d . . .
N6 N 0.7224(2) 1.0520(2) 0.44882(13) 0.0176(4) Uani 1 1 d . . .
N7 N 0.9857(3) 0.4295(2) 0.36861(14) 0.0229(5) Uani 1 1 d . . .
N8 N 0.9776(3) 0.3082(3) 0.34073(14) 0.0273(5) Uani 1 1 d . . .
N9 N 0.8871(3) 0.3765(2) 0.24076(13) 0.0189(4) Uani 1 1 d . . .
N10 N 0.7332(3) 0.0147(2) -0.10615(14) 0.0229(5) Uani 1 1 d . . .
N11 N 0.5835(3) -0.0201(2) -0.13780(14) 0.0243(5) Uani 1 1 d . . .
N12 N 0.6861(2) 0.1529(2) -0.03776(13) 0.0170(4) Uani 1 1 d . . .
C1 C 0.7617(3) 0.6206(3) 0.44793(16) 0.0204(5) Uani 1 1 d . . .
H1 H 0.8237 0.7028 0.4827 0.025 Uiso 1 1 calc R . .
C2 C 0.5810(3) 0.4614(3) 0.3559(2) 0.0308(7) Uani 1 1 d . . .
H2 H 0.4933 0.4131 0.3144 0.037 Uiso 1 1 calc R . .
C3 C 0.7383(3) 1.1729(3) 0.43745(16) 0.0205(5) Uani 1 1 d . . .
H3 H 0.6798 1.1862 0.3948 0.025 Uiso 1 1 calc R . .
C4 C 0.8296(3) 1.0812(3) 0.51715(16) 0.0236(6) Uani 1 1 d . . .
H4 H 0.8472 1.0176 0.5402 0.028 Uiso 1 1 calc R . .
C5 C 0.5697(3) 0.6816(2) 0.36972(16) 0.0177(5) Uani 1 1 d . . .
C6 C 0.6779(3) 0.8215(2) 0.42036(15) 0.0166(5) Uani 1 1 d . . .
H6A H 0.7752 0.8514 0.4115 0.020 Uiso 1 1 calc R . .
H6B H 0.6904 0.8198 0.4756 0.020 Uiso 1 1 calc R . .
C7 C 0.6149(3) 0.9173(2) 0.39871(15) 0.0174(5) Uani 1 1 d . . .
C8 C 0.5973(4) 0.9211(3) 0.31159(16) 0.0269(6) Uani 1 1 d . . .
H8A H 0.5580 0.9821 0.2976 0.032 Uiso 1 1 calc R . .
H8B H 0.6940 0.9518 0.3018 0.032 Uiso 1 1 calc R . .
C9 C 0.4892(4) 0.7801(3) 0.26213(18) 0.0312(7) Uani 1 1 d . . .
H9 H 0.4771 0.7815 0.2064 0.037 Uiso 1 1 calc R . .
C10 C 0.5535(3) 0.6845(3) 0.28316(17) 0.0248(6) Uani 1 1 d . . .
H10A H 0.4869 0.5958 0.2507 0.030 Uiso 1 1 calc R . .
H10B H 0.6505 0.7147 0.2739 0.030 Uiso 1 1 calc R . .
C11 C 0.4169(3) 0.6326(3) 0.3850(2) 0.0267(6) Uani 1 1 d . . .
H11A H 0.4279 0.6296 0.4400 0.032 Uiso 1 1 calc R . .
H11B H 0.3486 0.5436 0.3534 0.032 Uiso 1 1 calc R . .
C12 C 0.3543(3) 0.7295(3) 0.3634(2) 0.0311(7) Uani 1 1 d . . .
H12 H 0.2563 0.6993 0.3727 0.037 Uiso 1 1 calc R . .
C13 C 0.4628(3) 0.8696(3) 0.41474(19) 0.0261(6) Uani 1 1 d . . .
H13A H 0.4226 0.9307 0.4026 0.031 Uiso 1 1 calc R . .
H13B H 0.4748 0.8675 0.4699 0.031 Uiso 1 1 calc R . .
C14 C 0.3370(4) 0.7328(3) 0.2764(2) 0.0409(9) Uani 1 1 d . . .
H14A H 0.2682 0.6445 0.2440 0.049 Uiso 1 1 calc R . .
H14B H 0.2962 0.7928 0.2622 0.049 Uiso 1 1 calc R . .
C15 C 0.9312(3) 0.4673(3) 0.30810(16) 0.0226(5) Uani 1 1 d . . .
H15 H 0.9236 0.5461 0.3108 0.027 Uiso 1 1 calc R . .
C16 C 0.9189(4) 0.2805(3) 0.26426(17) 0.0269(6) Uani 1 1 d . . .
H16 H 0.9015 0.2043 0.2305 0.032 Uiso 1 1 calc R . .
C17 C 0.7915(3) 0.1169(3) -0.04719(16) 0.0222(5) Uani 1 1 d . . .
H17 H 0.8910 0.1591 -0.0161 0.027 Uiso 1 1 calc R . .
C18 C 0.5596(3) 0.0641(3) -0.09555(16) 0.0210(5) Uani 1 1 d . . .
H18 H 0.4673 0.0636 -0.1038 0.025 Uiso 1 1 calc R . .
C19 C 0.8125(3) 0.3830(3) 0.16114(15) 0.0159(5) Uani 1 1 d . . .
C20 C 0.7841(3) 0.2625(2) 0.10206(14) 0.0160(5) Uani 1 1 d . . .
H20A H 0.7201 0.1812 0.1154 0.019 Uiso 1 1 calc R . .
H20B H 0.8782 0.2622 0.1034 0.019 Uiso 1 1 calc R . .
C21 C 0.7082(3) 0.2690(2) 0.01954(14) 0.0146(4) Uani 1 1 d . . .
C22 C 0.8072(3) 0.3972(3) -0.00219(15) 0.0181(5) Uani 1 1 d . . .
H22A H 0.7584 0.4003 -0.0545 0.022 Uiso 1 1 calc R . .
H22B H 0.9022 0.3997 -0.0022 0.022 Uiso 1 1 calc R . .
C23 C 0.8344(3) 0.5179(3) 0.05833(16) 0.0190(5) Uani 1 1 d . . .
H23 H 0.8979 0.6006 0.0449 0.023 Uiso 1 1 calc R . .
C24 C 0.9135(3) 0.5118(3) 0.14043(15) 0.0185(5) Uani 1 1 d . . .
H24A H 1.0084 0.5138 0.1409 0.022 Uiso 1 1 calc R . .
H24B H 0.9334 0.5883 0.1790 0.022 Uiso 1 1 calc R . .
C25 C 0.6618(3) 0.3792(3) 0.16056(15) 0.0189(5) Uani 1 1 d . . .
H25A H 0.5987 0.2982 0.1746 0.023 Uiso 1 1 calc R . .
H25B H 0.6784 0.4549 0.1986 0.023 Uiso 1 1 calc R . .
C26 C 0.5846(3) 0.3838(3) 0.07758(16) 0.0209(5) Uani 1 1 d . . .
H26 H 0.4882 0.3812 0.0765 0.025 Uiso 1 1 calc R . .
C27 C 0.5571(3) 0.2637(3) 0.01702(16) 0.0194(5) Uani 1 1 d . . .
H27A H 0.4927 0.1814 0.0293 0.023 Uiso 1 1 calc R . .
H27B H 0.5079 0.2669 -0.0352 0.023 Uiso 1 1 calc R . .
C28 C 0.6842(3) 0.5135(3) 0.05706(17) 0.0223(5) Uani 1 1 d . . .
H28A H 0.6351 0.5182 0.0053 0.027 Uiso 1 1 calc R . .
H28B H 0.7004 0.5894 0.0949 0.027 Uiso 1 1 calc R . .
O1 O 1.0194(3) 0.1024(3) 0.40293(15) 0.0420(6) Uani 1 1 d . . .
H1C H 0.9979 0.1643 0.3926 0.063 Uiso 1 1 d R . .
H1D H 1.0585 0.0857 0.3689 0.063 Uiso 1 1 d R . .
O2 O 0.9133(3) 0.7396(3) 0.29263(16) 0.0476(7) Uani 1 1 d . . .
H2C H 0.9750 0.7594 0.3379 0.071 Uiso 1 1 d R . .
H2D H 0.9364 0.8099 0.2747 0.071 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.01751(12) 0.00989(11) 0.01529(12) 0.00016(9) -0.00090(9) 0.00689(9)
Cd2 0.02019(9) 0.01745(9) 0.02324(10) 0.00302(7) 0.00441(7) 0.00869(8)
I1 0.03082(10) 0.03760(12) 0.02589(10) 0.01275(8) 0.00639(8) 0.01793(9)
I2 0.02056(9) 0.02035(9) 0.03337(10) 0.01050(7) 0.00848(7) 0.00956(7)
I3 0.01961(9) 0.02486(11) 0.05987(15) 0.00567(10) -0.00018(9) 0.00365(8)
N1 0.0212(11) 0.0160(11) 0.0262(12) 0.0012(9) -0.0009(9) 0.0095(9)
N2 0.0235(12) 0.0163(12) 0.0468(16) -0.0027(11) -0.0090(11) 0.0101(10)
N3 0.0176(10) 0.0111(10) 0.0267(12) -0.0001(8) -0.0006(9) 0.0069(8)
N4 0.0255(12) 0.0132(10) 0.0232(11) 0.0051(9) 0.0046(9) 0.0092(9)
N5 0.0268(12) 0.0175(11) 0.0210(11) 0.0054(9) 0.0017(9) 0.0074(10)
N6 0.0209(11) 0.0121(10) 0.0194(11) 0.0040(8) 0.0048(9) 0.0078(8)
N7 0.0294(12) 0.0198(11) 0.0185(11) 0.0010(9) 0.0025(9) 0.0134(10)
N8 0.0413(15) 0.0267(13) 0.0192(11) 0.0030(10) 0.0034(10) 0.0237(12)
N9 0.0225(11) 0.0180(11) 0.0158(10) 0.0026(8) 0.0021(8) 0.0112(9)
N10 0.0227(11) 0.0210(12) 0.0222(12) 0.0027(9) 0.0046(9) 0.0090(10)
N11 0.0212(11) 0.0212(12) 0.0243(12) 0.0013(9) 0.0031(9) 0.0071(10)
N12 0.0159(10) 0.0167(10) 0.0151(10) 0.0027(8) 0.0020(8) 0.0060(8)
C1 0.0202(12) 0.0146(12) 0.0225(13) -0.0003(10) -0.0007(10) 0.0088(10)
C2 0.0241(14) 0.0124(12) 0.0417(18) -0.0046(12) -0.0089(13) 0.0072(11)
C3 0.0244(13) 0.0132(12) 0.0239(13) 0.0049(10) 0.0041(11) 0.0101(10)
C4 0.0282(14) 0.0153(12) 0.0209(13) 0.0057(10) 0.0002(11) 0.0077(11)
C5 0.0156(11) 0.0110(11) 0.0231(13) 0.0015(9) 0.0003(10) 0.0062(9)
C6 0.0149(11) 0.0129(11) 0.0202(12) 0.0018(9) 0.0018(9) 0.0069(9)
C7 0.0179(12) 0.0117(11) 0.0195(12) 0.0011(9) 0.0010(9) 0.0067(9)
C8 0.0370(16) 0.0190(13) 0.0203(13) 0.0035(10) -0.0014(12) 0.0142(12)
C9 0.0436(18) 0.0218(14) 0.0206(14) 0.0000(11) -0.0061(13) 0.0172(14)
C10 0.0293(14) 0.0179(13) 0.0223(13) -0.0019(10) -0.0005(11) 0.0120(11)
C11 0.0162(12) 0.0146(12) 0.0435(18) 0.0026(12) 0.0058(12) 0.0043(10)
C12 0.0143(12) 0.0193(14) 0.055(2) -0.0027(13) 0.0046(13) 0.0088(11)
C13 0.0176(12) 0.0181(13) 0.0410(17) -0.0008(12) 0.0048(12) 0.0102(11)
C14 0.0295(16) 0.0244(16) 0.053(2) -0.0085(14) -0.0183(15) 0.0164(14)
C15 0.0305(14) 0.0175(13) 0.0186(13) 0.0014(10) 0.0034(11) 0.0125(11)
C16 0.0420(17) 0.0266(15) 0.0181(13) 0.0026(11) 0.0055(12) 0.0234(14)
C17 0.0186(12) 0.0235(13) 0.0223(13) -0.0003(10) 0.0037(10) 0.0101(11)
C18 0.0180(12) 0.0169(12) 0.0212(13) 0.0022(10) 0.0006(10) 0.0050(10)
C19 0.0166(11) 0.0163(12) 0.0150(11) 0.0040(9) 0.0028(9) 0.0086(10)
C20 0.0160(11) 0.0149(11) 0.0161(11) 0.0025(9) 0.0033(9) 0.0073(9)
C21 0.0135(11) 0.0152(11) 0.0139(11) 0.0026(9) 0.0029(9) 0.0063(9)
C22 0.0178(12) 0.0187(12) 0.0200(12) 0.0072(10) 0.0082(10) 0.0087(10)
C23 0.0207(12) 0.0160(12) 0.0218(13) 0.0083(10) 0.0084(10) 0.0079(10)
C24 0.0168(12) 0.0144(12) 0.0202(12) 0.0013(9) 0.0035(10) 0.0051(10)
C25 0.0191(12) 0.0219(13) 0.0184(12) 0.0059(10) 0.0080(10) 0.0106(10)
C26 0.0184(12) 0.0283(14) 0.0228(13) 0.0093(11) 0.0088(10) 0.0148(11)
C27 0.0119(11) 0.0232(13) 0.0216(13) 0.0072(10) 0.0040(9) 0.0069(10)
C28 0.0251(13) 0.0241(14) 0.0251(14) 0.0102(11) 0.0077(11) 0.0168(12)
O1 0.0562(16) 0.0514(16) 0.0435(14) 0.0246(12) 0.0242(13) 0.0397(14)
O2 0.0560(17) 0.0399(15) 0.0427(15) 0.0046(12) 0.0004(13) 0.0264(13)

_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.
;

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
Cd1 N1 2.305(2) . ?
Cd1 N1 2.305(2) 2_766 ?
Cd1 N7 2.359(2) 2_766 ?
Cd1 N7 2.359(2) . ?
Cd1 N4 2.403(2) 1_545 ?
Cd1 N4 2.403(2) 2_776 ?
Cd2 N10 2.283(2) . ?
Cd2 I1 2.7441(3) . ?
Cd2 I2 2.7452(3) . ?
Cd2 I3 2.7560(3) . ?
N1 C1 1.309(3) . ?
N1 N2 1.381(3) . ?
N2 C2 1.307(4) . ?
N3 C1 1.352(3) . ?
N3 C2 1.365(3) . ?
N3 C5 1.483(3) . ?
N4 C3 1.308(4) . ?
N4 N5 1.379(3) . ?
N4 Cd1 2.403(2) 1_565 ?
N5 C4 1.302(4) . ?
N6 C4 1.353(3) . ?
N6 C3 1.357(3) . ?
N6 C7 1.487(3) . ?
N7 C15 1.304(4) . ?
N7 N8 1.382(3) . ?
N8 C16 1.311(4) . ?
N9 C16 1.348(3) . ?
N9 C15 1.354(3) . ?
N9 C19 1.485(3) . ?
N10 C17 1.305(4) . ?
N10 N11 1.383(3) . ?
N11 C18 1.302(4) . ?
N12 C17 1.355(3) . ?
N12 C18 1.362(3) . ?
N12 C21 1.490(3) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C10 1.525(4) . ?
C5 C6 1.530(3) . ?
C5 C11 1.533(4) . ?
C6 C7 1.531(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C13 1.533(4) . ?
C7 C8 1.535(4) . ?
C8 C9 1.533(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.520(5) . ?
C9 C10 1.535(4) . ?
C9 H9 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.539(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C14 1.533(5) . ?
C12 C13 1.536(4) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.522(3) . ?
C19 C24 1.531(4) . ?
C19 C25 1.538(3) . ?
C20 C21 1.533(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.529(3) . ?
C21 C27 1.529(3) . ?
C22 C23 1.543(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.528(4) . ?
C23 C24 1.536(4) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.537(4) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C28 1.532(4) . ?
C26 C27 1.536(4) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
O1 H1C 0.8499 . ?
O1 H1D 0.8500 . ?
O2 H2C 0.8500 . ?
O2 H2D 0.8499 . ?

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 Cd1 N1 180.000(1) . 2_766 ?
N1 Cd1 N7 94.69(8) . 2_766 ?
N1 Cd1 N7 85.31(8) 2_766 2_766 ?
N1 Cd1 N7 85.31(8) . . ?
N1 Cd1 N7 94.69(8) 2_766 . ?
N7 Cd1 N7 180.000(1) 2_766 . ?
N1 Cd1 N4 89.15(8) . 1_545 ?
N1 Cd1 N4 90.85(8) 2_766 1_545 ?
N7 Cd1 N4 94.10(8) 2_766 1_545 ?
N7 Cd1 N4 85.90(8) . 1_545 ?
N1 Cd1 N4 90.85(8) . 2_776 ?
N1 Cd1 N4 89.15(8) 2_766 2_776 ?
N7 Cd1 N4 85.90(8) 2_766 2_776 ?
N7 Cd1 N4 94.10(8) . 2_776 ?
N4 Cd1 N4 180.0 1_545 2_776 ?
N10 Cd2 I1 98.84(6) . . ?
N10 Cd2 I2 113.75(6) . . ?
I1 Cd2 I2 113.766(9) . . ?
N10 Cd2 I3 108.34(6) . . ?
I1 Cd2 I3 112.277(10) . . ?
I2 Cd2 I3 109.457(9) . . ?
C1 N1 N2 108.0(2) . . ?
C1 N1 Cd1 130.59(19) . . ?
N2 N1 Cd1 119.32(17) . . ?
C2 N2 N1 106.0(2) . . ?
C1 N3 C2 104.5(2) . . ?
C1 N3 C5 128.3(2) . . ?
C2 N3 C5 127.1(2) . . ?
C3 N4 N5 107.4(2) . . ?
C3 N4 Cd1 131.05(18) . 1_565 ?
N5 N4 Cd1 117.78(17) . 1_565 ?
C4 N5 N4 106.3(2) . . ?
C4 N6 C3 103.9(2) . . ?
C4 N6 C7 126.9(2) . . ?
C3 N6 C7 129.2(2) . . ?
C15 N7 N8 107.3(2) . . ?
C15 N7 Cd1 125.73(18) . . ?
N8 N7 Cd1 122.63(17) . . ?
C16 N8 N7 106.1(2) . . ?
C16 N9 C15 104.3(2) . . ?
C16 N9 C19 129.9(2) . . ?
C15 N9 C19 125.7(2) . . ?
C17 N10 N11 108.3(2) . . ?
C17 N10 Cd2 131.67(19) . . ?
N11 N10 Cd2 119.53(17) . . ?
C18 N11 N10 105.6(2) . . ?
C17 N12 C18 104.1(2) . . ?
C17 N12 C21 127.2(2) . . ?
C18 N12 C21 128.6(2) . . ?
N1 C1 N3 110.2(2) . . ?
N1 C1 H1 124.9 . . ?
N3 C1 H1 124.9 . . ?
N2 C2 N3 111.2(3) . . ?
N2 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
N4 C3 N6 110.6(2) . . ?
N4 C3 H3 124.7 . . ?
N6 C3 H3 124.7 . . ?
N5 C4 N6 111.8(2) . . ?
N5 C4 H4 124.1 . . ?
N6 C4 H4 124.1 . . ?
N3 C5 C10 109.4(2) . . ?
N3 C5 C6 108.0(2) . . ?
C10 C5 C6 109.5(2) . . ?
N3 C5 C11 109.5(2) . . ?
C10 C5 C11 110.5(2) . . ?
C6 C5 C11 109.9(2) . . ?
C5 C6 C7 109.3(2) . . ?
C5 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
N6 C7 C6 107.9(2) . . ?
N6 C7 C13 110.0(2) . . ?
C6 C7 C13 108.9(2) . . ?
N6 C7 C8 109.9(2) . . ?
C6 C7 C8 109.7(2) . . ?
C13 C7 C8 110.4(2) . . ?
C9 C8 C7 108.3(2) . . ?
C9 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C14 C9 C8 110.1(3) . . ?
C14 C9 C10 110.2(3) . . ?
C8 C9 C10 109.8(2) . . ?
C14 C9 H9 108.9 . . ?
C8 C9 H9 108.9 . . ?
C10 C9 H9 108.9 . . ?
C5 C10 C9 108.4(2) . . ?
C5 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C5 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C5 C11 C12 108.5(2) . . ?
C5 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
C5 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C14 C12 C13 109.8(3) . . ?
C14 C12 C11 109.3(3) . . ?
C13 C12 C11 109.4(2) . . ?
C14 C12 H12 109.5 . . ?
C13 C12 H12 109.5 . . ?
C11 C12 H12 109.5 . . ?
C7 C13 C12 109.1(2) . . ?
C7 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
C7 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C9 C14 C12 109.4(2) . . ?
C9 C14 H14A 109.8 . . ?
C12 C14 H14A 109.8 . . ?
C9 C14 H14B 109.8 . . ?
C12 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
N7 C15 N9 110.8(2) . . ?
N7 C15 H15 124.6 . . ?
N9 C15 H15 124.6 . . ?
N8 C16 N9 111.4(2) . . ?
N8 C16 H16 124.3 . . ?
N9 C16 H16 124.3 . . ?
N10 C17 N12 110.2(2) . . ?
N10 C17 H17 124.9 . . ?
N12 C17 H17 124.9 . . ?
N11 C18 N12 111.9(2) . . ?
N11 C18 H18 124.1 . . ?
N12 C18 H18 124.1 . . ?
N9 C19 C20 108.7(2) . . ?
N9 C19 C24 109.5(2) . . ?
C20 C19 C24 110.1(2) . . ?
N9 C19 C25 109.0(2) . . ?
C20 C19 C25 109.2(2) . . ?
C24 C19 C25 110.2(2) . . ?
C19 C20 C21 109.1(2) . . ?
C19 C20 H20A 109.9 . . ?
C21 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
C21 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N12 C21 C22 108.69(19) . . ?
N12 C21 C27 110.1(2) . . ?
C22 C21 C27 109.6(2) . . ?
N12 C21 C20 108.32(19) . . ?
C22 C21 C20 110.5(2) . . ?
C27 C21 C20 109.5(2) . . ?
C21 C22 C23 109.0(2) . . ?
C21 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
C21 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C28 C23 C24 110.1(2) . . ?
C28 C23 C22 109.3(2) . . ?
C24 C23 C22 108.9(2) . . ?
C28 C23 H23 109.5 . . ?
C24 C23 H23 109.5 . . ?
C22 C23 H23 109.5 . . ?
C19 C24 C23 109.0(2) . . ?
C19 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
C19 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C26 C25 C19 108.5(2) . . ?
C26 C25 H25A 110.0 . . ?
C19 C25 H25A 110.0 . . ?
C26 C25 H25B 110.0 . . ?
C19 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C28 C26 C27 109.7(2) . . ?
C28 C26 C25 109.3(2) . . ?
C27 C26 C25 110.3(2) . . ?
C28 C26 H26 109.2 . . ?
C27 C26 H26 109.2 . . ?
C25 C26 H26 109.2 . . ?
C21 C27 C26 108.5(2) . . ?
C21 C27 H27A 110.0 . . ?
C26 C27 H27A 110.0 . . ?
C21 C27 H27B 110.0 . . ?
C26 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
C23 C28 C26 109.4(2) . . ?
C23 C28 H28A 109.8 . . ?
C26 C28 H28A 109.8 . . ?
C23 C28 H28B 109.8 . . ?
C26 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
H1C O1 H1D 108.2 . . ?
H2C O2 H2D 108.0 . . ?

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
N7 Cd1 N1 C1 64.5(3) 2_766 . . . ?
N7 Cd1 N1 C1 -115.5(3) . . . . ?
N4 Cd1 N1 C1 158.6(3) 1_545 . . . ?
N4 Cd1 N1 C1 -21.4(3) 2_776 . . . ?
N7 Cd1 N1 N2 -133.8(2) 2_766 . . . ?
N7 Cd1 N1 N2 46.2(2) . . . . ?
N4 Cd1 N1 N2 -39.8(2) 1_545 . . . ?
N4 Cd1 N1 N2 140.2(2) 2_776 . . . ?
C1 N1 N2 C2 0.2(4) . . . . ?
Cd1 N1 N2 C2 -165.3(2) . . . . ?
C3 N4 N5 C4 1.0(3) . . . . ?
Cd1 N4 N5 C4 -159.48(19) 1_565 . . . ?
N1 Cd1 N7 C15 31.1(2) . . . . ?
N1 Cd1 N7 C15 -148.9(2) 2_766 . . . ?
N4 Cd1 N7 C15 120.6(2) 1_545 . . . ?
N4 Cd1 N7 C15 -59.4(2) 2_776 . . . ?
N1 Cd1 N7 N8 -122.4(2) . . . . ?
N1 Cd1 N7 N8 57.6(2) 2_766 . . . ?
N4 Cd1 N7 N8 -32.9(2) 1_545 . . . ?
N4 Cd1 N7 N8 147.1(2) 2_776 . . . ?
C15 N7 N8 C16 0.4(3) . . . . ?
Cd1 N7 N8 C16 158.1(2) . . . . ?
I1 Cd2 N10 C17 -131.8(3) . . . . ?
I2 Cd2 N10 C17 107.2(3) . . . . ?
I3 Cd2 N10 C17 -14.7(3) . . . . ?
I1 Cd2 N10 N11 39.1(2) . . . . ?
I2 Cd2 N10 N11 -81.8(2) . . . . ?
I3 Cd2 N10 N11 156.24(18) . . . . ?
C17 N10 N11 C18 -0.1(3) . . . . ?
Cd2 N10 N11 C18 -172.96(18) . . . . ?
N2 N1 C1 N3 -0.3(3) . . . . ?
Cd1 N1 C1 N3 162.95(19) . . . . ?
C2 N3 C1 N1 0.3(3) . . . . ?
C5 N3 C1 N1 -176.1(3) . . . . ?
N1 N2 C2 N3 0.0(4) . . . . ?
C1 N3 C2 N2 -0.2(4) . . . . ?
C5 N3 C2 N2 176.3(3) . . . . ?
N5 N4 C3 N6 -0.6(3) . . . . ?
Cd1 N4 C3 N6 156.31(18) 1_565 . . . ?
C4 N6 C3 N4 0.0(3) . . . . ?
C7 N6 C3 N4 -179.5(2) . . . . ?
N4 N5 C4 N6 -1.0(3) . . . . ?
C3 N6 C4 N5 0.7(3) . . . . ?
C7 N6 C4 N5 -179.9(2) . . . . ?
C1 N3 C5 C10 121.4(3) . . . . ?
C2 N3 C5 C10 -54.2(4) . . . . ?
C1 N3 C5 C6 2.4(4) . . . . ?
C2 N3 C5 C6 -173.2(3) . . . . ?
C1 N3 C5 C11 -117.4(3) . . . . ?
C2 N3 C5 C11 67.1(4) . . . . ?
N3 C5 C6 C7 179.7(2) . . . . ?
C10 C5 C6 C7 60.7(3) . . . . ?
C11 C5 C6 C7 -60.8(3) . . . . ?
C4 N6 C7 C6 -19.5(3) . . . . ?
C3 N6 C7 C6 159.8(3) . . . . ?
C4 N6 C7 C13 99.2(3) . . . . ?
C3 N6 C7 C13 -81.5(3) . . . . ?
C4 N6 C7 C8 -139.1(3) . . . . ?
C3 N6 C7 C8 40.2(4) . . . . ?
C5 C6 C7 N6 -180.0(2) . . . . ?
C5 C6 C7 C13 60.6(3) . . . . ?
C5 C6 C7 C8 -60.3(3) . . . . ?
N6 C7 C8 C9 178.5(2) . . . . ?
C6 C7 C8 C9 60.0(3) . . . . ?
C13 C7 C8 C9 -60.0(3) . . . . ?
C7 C8 C9 C14 60.6(3) . . . . ?
C7 C8 C9 C10 -60.9(3) . . . . ?
N3 C5 C10 C9 -179.1(2) . . . . ?
C6 C5 C10 C9 -61.0(3) . . . . ?
C11 C5 C10 C9 60.2(3) . . . . ?
C14 C9 C10 C5 -59.8(3) . . . . ?
C8 C9 C10 C5 61.6(3) . . . . ?
N3 C5 C11 C12 178.8(2) . . . . ?
C10 C5 C11 C12 -60.7(3) . . . . ?
C6 C5 C11 C12 60.3(3) . . . . ?
C5 C11 C12 C14 59.9(3) . . . . ?
C5 C11 C12 C13 -60.3(3) . . . . ?
N6 C7 C13 C12 -179.1(2) . . . . ?
C6 C7 C13 C12 -61.0(3) . . . . ?
C8 C7 C13 C12 59.5(3) . . . . ?
C14 C12 C13 C7 -58.8(3) . . . . ?
C11 C12 C13 C7 61.2(3) . . . . ?
C8 C9 C14 C12 -60.9(3) . . . . ?
C10 C9 C14 C12 60.4(3) . . . . ?
C13 C12 C14 C9 59.7(3) . . . . ?
C11 C12 C14 C9 -60.3(3) . . . . ?
N8 N7 C15 N9 -0.1(3) . . . . ?
Cd1 N7 C15 N9 -156.96(19) . . . . ?
C16 N9 C15 N7 -0.2(3) . . . . ?
C19 N9 C15 N7 176.5(2) . . . . ?
N7 N8 C16 N9 -0.5(4) . . . . ?
C15 N9 C16 N8 0.5(4) . . . . ?
C19 N9 C16 N8 -176.1(3) . . . . ?
N11 N10 C17 N12 0.0(3) . . . . ?
Cd2 N10 C17 N12 171.66(18) . . . . ?
C18 N12 C17 N10 0.1(3) . . . . ?
C21 N12 C17 N10 -176.1(2) . . . . ?
N10 N11 C18 N12 0.2(3) . . . . ?
C17 N12 C18 N11 -0.2(3) . . . . ?
C21 N12 C18 N11 176.0(2) . . . . ?
C16 N9 C19 C20 -4.9(4) . . . . ?
C15 N9 C19 C20 179.2(2) . . . . ?
C16 N9 C19 C24 -125.3(3) . . . . ?
C15 N9 C19 C24 58.9(3) . . . . ?
C16 N9 C19 C25 114.1(3) . . . . ?
C15 N9 C19 C25 -61.8(3) . . . . ?
N9 C19 C20 C21 -179.5(2) . . . . ?
C24 C19 C20 C21 -59.5(3) . . . . ?
C25 C19 C20 C21 61.7(3) . . . . ?
C17 N12 C21 C22 66.4(3) . . . . ?
C18 N12 C21 C22 -108.9(3) . . . . ?
C17 N12 C21 C27 -173.5(2) . . . . ?
C18 N12 C21 C27 11.2(3) . . . . ?
C17 N12 C21 C20 -53.7(3) . . . . ?
C18 N12 C21 C20 130.9(3) . . . . ?
C19 C20 C21 N12 178.10(19) . . . . ?
C19 C20 C21 C22 59.1(3) . . . . ?
C19 C20 C21 C27 -61.8(3) . . . . ?
N12 C21 C22 C23 -178.4(2) . . . . ?
C27 C21 C22 C23 61.2(3) . . . . ?
C20 C21 C22 C23 -59.6(3) . . . . ?
C21 C22 C23 C28 -60.1(3) . . . . ?
C21 C22 C23 C24 60.2(3) . . . . ?
N9 C19 C24 C23 -179.5(2) . . . . ?
C20 C19 C24 C23 61.0(3) . . . . ?
C25 C19 C24 C23 -59.6(3) . . . . ?
C28 C23 C24 C19 59.0(3) . . . . ?
C22 C23 C24 C19 -60.9(3) . . . . ?
N9 C19 C25 C26 -179.1(2) . . . . ?
C20 C19 C25 C26 -60.5(3) . . . . ?
C24 C19 C25 C26 60.6(3) . . . . ?
C19 C25 C26 C28 -60.8(3) . . . . ?
C19 C25 C26 C27 60.0(3) . . . . ?
N12 C21 C27 C26 179.2(2) . . . . ?
C22 C21 C27 C26 -61.2(3) . . . . ?
C20 C21 C27 C26 60.2(3) . . . . ?
C28 C26 C27 C21 60.6(3) . . . . ?
C25 C26 C27 C21 -59.9(3) . . . . ?
C24 C23 C28 C26 -60.0(3) . . . . ?
C22 C23 C28 C26 59.7(3) . . . . ?
C27 C26 C28 C23 -60.2(3) . . . . ?
C25 C26 C28 C23 60.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        29.57
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.242
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.106

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk7 in P-1
CELL 0.71073 10.3397 11.3871 17.8908 95.632 102.961 115.430
ZERR 1.00 0.0002 0.0002 0.0005 0.001 0.001 0.001
LATT 1
SFAC C H N O CD I
UNIT 56 80 24 4 3 6

MERG 2
OMIT 0.00 180.00
OMIT -1 1 0
OMIT -2 -1 3
OMIT 7 -9 2
OMIT -2 3 5
SHEL 0.72 7
FMAP 2
PLAN 20
SIZE 0.20 0.35 0.50
ACTA
BOND
BOND $H
CONF
L.S. 4
TEMP 23.00
WGHT 0.019700 3.231700
FVAR 0.25886
CD1 5 1.000000 0.500000 0.500000 10.50000 0.01751 0.00989 =
0.01529 0.00016 -0.00090 0.00689
CD2 5 0.839658 -0.088048 -0.168246 11.00000 0.02019 0.01745 =
0.02324 0.00302 0.00441 0.00869
I1 6 0.700589 -0.101168 -0.320986 11.00000 0.03082 0.03760 =
0.02589 0.01275 0.00639 0.01793
I2 6 0.786774 -0.332303 -0.135481 11.00000 0.02056 0.02035 =
0.03337 0.01050 0.00848 0.00956
I3 6 1.144328 0.077436 -0.124909 11.00000 0.01961 0.02486 =
0.05987 0.00567 -0.00018 0.00365
N1 3 0.785515 0.516504 0.446433 11.00000 0.02123 0.01595 =
0.02619 0.00120 -0.00088 0.00951
N2 3 0.669554 0.413659 0.387429 11.00000 0.02351 0.01632 =
0.04679 -0.00269 -0.00904 0.01010
N3 3 0.633998 0.591445 0.391719 11.00000 0.01760 0.01115 =
0.02671 -0.00007 -0.00060 0.00694
N4 3 0.847058 1.268254 0.494785 11.00000 0.02550 0.01315 =
0.02325 0.00514 0.00455 0.00919
N5 3 0.905130 1.208933 0.546717 11.00000 0.02679 0.01746 =
0.02100 0.00541 0.00174 0.00740
N6 3 0.722450 1.051981 0.448815 11.00000 0.02091 0.01212 =
0.01942 0.00403 0.00481 0.00783
N7 3 0.985712 0.429543 0.368606 11.00000 0.02938 0.01983 =
0.01846 0.00099 0.00252 0.01345
N8 3 0.977615 0.308231 0.340732 11.00000 0.04126 0.02671 =
0.01924 0.00300 0.00335 0.02370
N9 3 0.887080 0.376538 0.240755 11.00000 0.02255 0.01795 =
0.01582 0.00257 0.00208 0.01119
N10 3 0.733246 0.014707 -0.106150 11.00000 0.02269 0.02100 =
0.02225 0.00267 0.00458 0.00904
N11 3 0.583467 -0.020115 -0.137804 11.00000 0.02122 0.02123 =
0.02430 0.00134 0.00307 0.00707
N12 3 0.686079 0.152884 -0.037758 11.00000 0.01586 0.01669 =
0.01512 0.00268 0.00198 0.00597
C1 1 0.761701 0.620583 0.447932 11.00000 0.02022 0.01457 =
0.02247 -0.00028 -0.00067 0.00879
AFIX 43
H1 2 0.823716 0.702762 0.482673 11.00000 -1.20000
AFIX 0
C2 1 0.581034 0.461415 0.355896 11.00000 0.02411 0.01245 =
0.04170 -0.00455 -0.00892 0.00722
AFIX 43
H2 2 0.493341 0.413081 0.314433 11.00000 -1.20000
AFIX 0
C3 1 0.738261 1.172942 0.437455 11.00000 0.02437 0.01317 =
0.02391 0.00493 0.00413 0.01006
AFIX 43
H3 2 0.679810 1.186231 0.394797 11.00000 -1.20000
AFIX 0
C4 1 0.829622 1.081153 0.517146 11.00000 0.02819 0.01531 =
0.02093 0.00566 0.00018 0.00769
AFIX 43
H4 2 0.847237 1.017620 0.540212 11.00000 -1.20000
AFIX 0
C5 1 0.569746 0.681611 0.369724 11.00000 0.01563 0.01101 =
0.02309 0.00152 0.00035 0.00624
C6 1 0.677888 0.821469 0.420356 11.00000 0.01494 0.01295 =
0.02016 0.00181 0.00175 0.00693
AFIX 23
H6A 2 0.775213 0.851443 0.411535 11.00000 -1.20000
H6B 2 0.690376 0.819822 0.475558 11.00000 -1.20000
AFIX 0
C7 1 0.614904 0.917283 0.398714 11.00000 0.01795 0.01167 =
0.01948 0.00106 0.00102 0.00671
C8 1 0.597344 0.921137 0.311595 11.00000 0.03705 0.01903 =
0.02027 0.00351 -0.00137 0.01420
AFIX 23
H8A 2 0.558030 0.982129 0.297638 11.00000 -1.20000
H8B 2 0.693963 0.951772 0.301849 11.00000 -1.20000
AFIX 0
C9 1 0.489179 0.780062 0.262127 11.00000 0.04363 0.02179 =
0.02063 -0.00004 -0.00613 0.01723
AFIX 13
H9 2 0.477101 0.781533 0.206363 11.00000 -1.20000
AFIX 0
C10 1 0.553509 0.684527 0.283160 11.00000 0.02928 0.01795 =
0.02227 -0.00189 -0.00051 0.01203
AFIX 23
H10A 2 0.486891 0.595773 0.250676 11.00000 -1.20000
H10B 2 0.650461 0.714742 0.273855 11.00000 -1.20000
AFIX 0
C11 1 0.416914 0.632646 0.385015 11.00000 0.01618 0.01463 =
0.04349 0.00260 0.00580 0.00434
AFIX 23
H11A 2 0.427908 0.629551 0.439969 11.00000 -1.20000
H11B 2 0.348582 0.543582 0.353358 11.00000 -1.20000
AFIX 0
C12 1 0.354311 0.729538 0.363448 11.00000 0.01434 0.01932 =
0.05493 -0.00269 0.00459 0.00879
AFIX 13
H12 2 0.256279 0.699324 0.372717 11.00000 -1.20000
AFIX 0
C13 1 0.462762 0.869628 0.414741 11.00000 0.01762 0.01807 =
0.04101 -0.00082 0.00477 0.01020
AFIX 23
H13A 2 0.422629 0.930741 0.402598 11.00000 -1.20000
H13B 2 0.474848 0.867451 0.469862 11.00000 -1.20000
AFIX 0
C14 1 0.337008 0.732846 0.276399 11.00000 0.02950 0.02437 =
0.05262 -0.00845 -0.01834 0.01645
AFIX 23
H14A 2 0.268166 0.644474 0.243970 11.00000 -1.20000
H14B 2 0.296242 0.792777 0.262206 11.00000 -1.20000
AFIX 0
C15 1 0.931187 0.467349 0.308100 11.00000 0.03054 0.01747 =
0.01864 0.00139 0.00338 0.01248
AFIX 43
H15 2 0.923627 0.546051 0.310847 11.00000 -1.20000
AFIX 0
C16 1 0.918945 0.280531 0.264259 11.00000 0.04200 0.02664 =
0.01811 0.00260 0.00545 0.02344
AFIX 43
H16 2 0.901501 0.204299 0.230484 11.00000 -1.20000
AFIX 0
C17 1 0.791522 0.116936 -0.047195 11.00000 0.01860 0.02349 =
0.02232 -0.00027 0.00368 0.01005
AFIX 43
H17 2 0.891034 0.159054 -0.016134 11.00000 -1.20000
AFIX 0
C18 1 0.559624 0.064074 -0.095548 11.00000 0.01802 0.01687 =
0.02117 0.00215 0.00059 0.00500
AFIX 43
H18 2 0.467315 0.063600 -0.103845 11.00000 -1.20000
AFIX 0
C19 1 0.812479 0.382999 0.161138 11.00000 0.01657 0.01631 =
0.01504 0.00399 0.00280 0.00860
C20 1 0.784075 0.262540 0.102057 11.00000 0.01605 0.01495 =
0.01614 0.00251 0.00329 0.00732
AFIX 23
H20A 2 0.720073 0.181169 0.115386 11.00000 -1.20000
H20B 2 0.878246 0.262246 0.103414 11.00000 -1.20000
AFIX 0
C21 1 0.708237 0.268967 0.019537 11.00000 0.01353 0.01520 =
0.01395 0.00255 0.00288 0.00630
C22 1 0.807244 0.397220 -0.002187 11.00000 0.01784 0.01870 =
0.02003 0.00720 0.00819 0.00871
AFIX 23
H22A 2 0.758375 0.400259 -0.054472 11.00000 -1.20000
H22B 2 0.902214 0.399710 -0.002156 11.00000 -1.20000
AFIX 0
C23 1 0.834403 0.517887 0.058330 11.00000 0.02073 0.01600 =
0.02176 0.00831 0.00844 0.00786
AFIX 13
H23 2 0.897945 0.600569 0.044864 11.00000 -1.20000
AFIX 0
C24 1 0.913482 0.511850 0.140432 11.00000 0.01683 0.01444 =
0.02022 0.00135 0.00348 0.00510
AFIX 23
H24A 2 1.008401 0.513824 0.140928 11.00000 -1.20000
H24B 2 0.933435 0.588340 0.178986 11.00000 -1.20000
AFIX 0
C25 1 0.661751 0.379197 0.160561 11.00000 0.01915 0.02190 =
0.01840 0.00592 0.00801 0.01061
AFIX 23
H25A 2 0.598723 0.298216 0.174600 11.00000 -1.20000
H25B 2 0.678355 0.454890 0.198600 11.00000 -1.20000
AFIX 0
C26 1 0.584565 0.383766 0.077581 11.00000 0.01835 0.02825 =
0.02277 0.00928 0.00881 0.01476
AFIX 13
H26 2 0.488223 0.381231 0.076543 11.00000 -1.20000
AFIX 0
C27 1 0.557051 0.263750 0.017017 11.00000 0.01195 0.02325 =
0.02164 0.00716 0.00400 0.00688
AFIX 23
H27A 2 0.492697 0.181397 0.029318 11.00000 -1.20000
H27B 2 0.507929 0.266885 -0.035188 11.00000 -1.20000
AFIX 0
C28 1 0.684153 0.513544 0.057063 11.00000 0.02510 0.02412 =
0.02509 0.01025 0.00768 0.01684
AFIX 23
H28A 2 0.635067 0.518232 0.005276 11.00000 -1.20000
H28B 2 0.700429 0.589383 0.094861 11.00000 -1.20000
AFIX 0
O1 4 1.019392 0.102354 0.402926 11.00000 0.05624 0.05137 =
0.04346 0.02456 0.02420 0.03974
AFIX 3
H1C 2 0.997913 0.164264 0.392556 11.00000 -1.50000
H1D 2 1.058462 0.085734 0.368916 11.00000 -1.50000
AFIX 0
O2 4 0.913312 0.739568 0.292628 11.00000 0.05600 0.03989 =
0.04271 0.00457 0.00040 0.02636
AFIX 3
H2C 2 0.974982 0.759398 0.337908 11.00000 -1.50000
H2D 2 0.936382 0.809888 0.274658 11.00000 -1.50000
HKLF 4

REM dk7 in P-1
REM R1 = 0.0267 for 8815 Fo > 4sig(Fo) and 0.0327 for all 10023 data
REM 421 parameters refined using 0 restraints

END

WGHT 0.0190 3.2869
REM Highest difference peak 2.242, deepest hole -1.839, 1-sigma level 0.106
Q1 1 0.7538 -0.1264 -0.3287 11.00000 0.05 2.24
Q2 1 1.1174 0.1046 -0.0886 11.00000 0.05 1.35
Q3 1 0.7880 -0.3454 -0.1802 11.00000 0.05 0.75
Q4 1 0.7212 -0.3080 -0.1341 11.00000 0.05 0.54
Q5 1 0.8146 -0.2869 -0.0967 11.00000 0.05 0.53
Q6 1 0.9009 -0.1109 -0.1706 11.00000 0.05 0.51
Q7 1 1.0781 0.0414 -0.1599 11.00000 0.05 0.50
Q8 1 0.8176 -0.1159 -0.2177 11.00000 0.05 0.49
Q9 1 0.6165 -0.0638 -0.3206 11.00000 0.05 0.49
Q10 1 0.7287 0.6756 0.5510 11.00000 0.05 0.48

;

#---------------------------------------------------------

data_(3)
_database_code_depnum_ccdc_archive 'CCDC 867226'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[1,3-di(1,2,4-triazol-4-yl)adamantane]disilver(I)
dinitrate Dihydrate
;
_chemical_name_common            
;bis-(1,3-di(1,2,4-triazol-4-yl)adamantane)disilver(i)
dinitrate Dihydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H36 Ag2 N12, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C28 H40 Ag2 N14 O8'
_chemical_formula_weight         916.48

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

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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5192(6)
_cell_length_b                   15.4818(11)
_cell_length_c                   16.9913(12)
_cell_angle_alpha                89.230(9)
_cell_angle_beta                 84.607(10)
_cell_angle_gamma                85.574(9)
_cell_volume                     1702.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      26.02

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7417
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
Crystals of the compound are non-merohedral twins exhibiting typical set
of problems with the structure refinement. In spite of the reasonable
Rint value (0.0537), the overall convergence was very poor, with very
heavy residual electron density peaks in the region of silver-triazole
chain and with systematically Fo^2^ larger of Fc^2^.
Then the data frames were indexed and integrated
(with a soft tolerance for the reflection overlap at 5 pixels)
as a two-domain system using RECIPE/TWIN facilities implemented in a
Stoe IPDS software. The data were scaled and merged yielding a single
dataset of about 84% completeness (for the coverage 26.0 deg.) due to a
partial overlap of the reflections, which correspond to the different
domains of the crystal.
;

_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8222
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         26.02
_reflns_number_total             5659
_reflns_number_gt                3473
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

For one of two unique non-coordinated NO3- ions, the O-atoms are equally
disordered over two positions. All non-hydrogen atoms were refined
anisotropically, including the disordered O-atoms. In order to improve
the refinement stabilty, the disordered nitrate was refined with soft
restraints in geometry for N-O bonds (0.01 A) [N-O = 1.22 A] and
with SIMU restrained refinement of the anisotropic thermal parameters
for the 0.50/0.50 disordered O-atoms, giving a
total number of the restraints used during the refinement 48.

The CH-hydrogen atoms were constrained with U(iso) = 1.2U(eq) of the
parent C-atom and with C-H distances 0.94 A (triazole), 0.98 A
(CH2 adamantane) and 0.99 A (CH adamantane). The OH-hydrogen atoms were
located and then constrained with O-H distances set to 0.85 A and
U(iso) = 1.5U(eq) of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5659
_refine_ls_number_parameters     496
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.920
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.72880(8) 0.02035(4) 0.05761(2) 0.03483(17) Uani 1 1 d . . .
Ag2 Ag 0.74721(8) 0.53013(4) 0.43691(2) 0.03202(16) Uani 1 1 d . . .
N1 N 0.4399(9) 0.1034(4) 0.0728(3) 0.0316(13) Uani 1 1 d . . .
N2 N 0.3047(9) 0.1097(4) 0.0146(3) 0.0344(14) Uani 1 1 d . . .
N3 N 0.2371(8) 0.2213(3) 0.0946(2) 0.0254(12) Uani 1 1 d . . .
N4 N 0.4837(8) 0.4864(4) 0.3821(2) 0.0276(13) Uani 1 1 d . . .
N5 N 0.3736(9) 0.4228(4) 0.4234(3) 0.0324(14) Uani 1 1 d . . .
N6 N 0.2755(8) 0.4340(3) 0.3039(2) 0.0230(12) Uani 1 1 d . . .
N7 N 0.8551(9) 0.3950(4) 0.5066(3) 0.0305(13) Uani 1 1 d . . .
N8 N 0.9764(9) 0.3967(4) 0.5709(2) 0.0305(13) Uani 1 1 d . . .
N9 N 0.7865(8) 0.2862(3) 0.5860(2) 0.0253(12) Uani 1 1 d . . .
N10 N 0.8420(10) 0.0797(4) 0.9242(3) 0.0383(15) Uani 1 1 d . . .
N11 N 0.9925(9) 0.0221(4) 0.8861(3) 0.0336(14) Uani 1 1 d . . .
N12 N 0.7842(8) 0.0707(3) 0.7998(2) 0.0239(12) Uani 1 1 d . . .
C1 C 0.3947(11) 0.1696(4) 0.1195(3) 0.0328(16) Uani 1 1 d . . .
H1 H 0.4627 0.1799 0.1645 0.039 Uiso 1 1 calc R . .
C2 C 0.1857(11) 0.1813(4) 0.0291(3) 0.0296(16) Uani 1 1 d . . .
H2 H 0.0794 0.2020 -0.0016 0.036 Uiso 1 1 calc R . .
C3 C 0.4170(10) 0.4915(4) 0.3110(3) 0.0283(15) Uani 1 1 d . . .
H3 H 0.4620 0.5300 0.2710 0.034 Uiso 1 1 calc R . .
C4 C 0.2538(11) 0.3931(4) 0.3756(3) 0.0317(16) Uani 1 1 d . . .
H4 H 0.1638 0.3494 0.3884 0.038 Uiso 1 1 calc R . .
C5 C 0.1457(10) 0.3062(4) 0.1269(3) 0.0236(14) Uani 1 1 d . . .
C6 C 0.2568(10) 0.3260(4) 0.2005(3) 0.0221(14) Uani 1 1 d . . .
H6A H 0.2353 0.2809 0.2409 0.027 Uiso 1 1 calc R . .
H6B H 0.4057 0.3272 0.1860 0.027 Uiso 1 1 calc R . .
C7 C 0.1673(10) 0.4144(4) 0.2329(3) 0.0253(15) Uani 1 1 d . . .
C8 C 0.2022(11) 0.4849(4) 0.1702(3) 0.0320(16) Uani 1 1 d . . .
H8A H 0.3503 0.4869 0.1546 0.038 Uiso 1 1 calc R . .
H8B H 0.1490 0.5416 0.1917 0.038 Uiso 1 1 calc R . .
C9 C 0.0891(13) 0.4644(5) 0.0981(3) 0.042(2) Uani 1 1 d . . .
H9 H 0.1085 0.5103 0.0575 0.051 Uiso 1 1 calc R . .
C10 C 0.1845(11) 0.3764(4) 0.0642(3) 0.0294(16) Uani 1 1 d . . .
H10A H 0.1209 0.3631 0.0162 0.035 Uiso 1 1 calc R . .
H10B H 0.3333 0.3791 0.0505 0.035 Uiso 1 1 calc R . .
C11 C -0.0829(10) 0.3003(5) 0.1506(4) 0.0356(18) Uani 1 1 d . . .
H11A H -0.1032 0.2556 0.1913 0.043 Uiso 1 1 calc R . .
H11B H -0.1532 0.2852 0.1047 0.043 Uiso 1 1 calc R . .
C12 C -0.1719(12) 0.3901(6) 0.1830(4) 0.048(2) Uani 1 1 d . . .
H12 H -0.3218 0.3884 0.1984 0.058 Uiso 1 1 calc R . .
C13 C -0.0598(11) 0.4108(5) 0.2570(4) 0.042(2) Uani 1 1 d . . .
H13A H -0.1170 0.4665 0.2794 0.050 Uiso 1 1 calc R . .
H13B H -0.0810 0.3658 0.2975 0.050 Uiso 1 1 calc R . .
C14 C -0.1379(13) 0.4589(5) 0.1213(4) 0.053(2) Uani 1 1 d . . .
H14A H -0.1984 0.5150 0.1420 0.064 Uiso 1 1 calc R . .
H14B H -0.2072 0.4457 0.0747 0.064 Uiso 1 1 calc R . .
C15 C 0.7477(11) 0.3281(4) 0.5176(3) 0.0290(15) Uani 1 1 d . . .
H15 H 0.6550 0.3109 0.4828 0.035 Uiso 1 1 calc R . .
C16 C 0.9300(10) 0.3306(4) 0.6168(3) 0.0276(15) Uani 1 1 d . . .
H16 H 0.9883 0.3164 0.6643 0.033 Uiso 1 1 calc R . .
C17 C 0.7212(10) 0.1072(4) 0.8705(3) 0.0293(15) Uani 1 1 d . . .
H17 H 0.6056 0.1471 0.8799 0.035 Uiso 1 1 calc R . .
C18 C 0.9519(10) 0.0173(4) 0.8123(3) 0.0282(15) Uani 1 1 d . . .
H18 H 1.0282 -0.0180 0.7737 0.034 Uiso 1 1 calc R . .
C19 C 0.7053(10) 0.2031(4) 0.6138(3) 0.0235(14) Uani 1 1 d . . .
C20 C 0.7783(10) 0.1802(4) 0.6956(3) 0.0246(14) Uani 1 1 d . . .
H20A H 0.9295 0.1770 0.6927 0.029 Uiso 1 1 calc R . .
H20B H 0.7236 0.2250 0.7338 0.029 Uiso 1 1 calc R . .
C21 C 0.7003(10) 0.0926(4) 0.7220(3) 0.0229(14) Uani 1 1 d . . .
C22 C 0.7843(10) 0.0218(4) 0.6629(3) 0.0271(15) Uani 1 1 d . . .
H22A H 0.9356 0.0170 0.6588 0.033 Uiso 1 1 calc R . .
H22B H 0.7358 -0.0341 0.6811 0.033 Uiso 1 1 calc R . .
C23 C 0.7088(11) 0.0449(4) 0.5823(3) 0.0285(15) Uani 1 1 d . . .
H23 H 0.7618 -0.0007 0.5437 0.034 Uiso 1 1 calc R . .
C24 C 0.7901(11) 0.1324(4) 0.5545(3) 0.0270(15) Uani 1 1 d . . .
H24A H 0.9415 0.1278 0.5505 0.032 Uiso 1 1 calc R . .
H24B H 0.7460 0.1473 0.5021 0.032 Uiso 1 1 calc R . .
C25 C 0.4686(10) 0.2108(4) 0.6210(3) 0.0302(16) Uani 1 1 d . . .
H25A H 0.4188 0.2267 0.5697 0.036 Uiso 1 1 calc R . .
H25B H 0.4156 0.2559 0.6591 0.036 Uiso 1 1 calc R . .
C26 C 0.3917(11) 0.1227(5) 0.6488(3) 0.0333(16) Uani 1 1 d . . .
H26 H 0.2388 0.1266 0.6532 0.040 Uiso 1 1 calc R . .
C27 C 0.4674(10) 0.0977(5) 0.7295(3) 0.0303(16) Uani 1 1 d . . .
H27A H 0.4125 0.1412 0.7689 0.036 Uiso 1 1 calc R . .
H27B H 0.4187 0.0416 0.7467 0.036 Uiso 1 1 calc R . .
C28 C 0.4757(11) 0.0530(4) 0.5884(3) 0.0339(17) Uani 1 1 d . . .
H28A H 0.4230 -0.0027 0.6048 0.041 Uiso 1 1 calc R . .
H28B H 0.4283 0.0684 0.5367 0.041 Uiso 1 1 calc R . .
N13 N 0.7092(13) 0.1698(5) 0.3194(3) 0.0497(18) Uani 1 1 d . . .
O1 O 0.8892(14) 0.1475(7) 0.3213(4) 0.125(4) Uani 1 1 d . . .
O2 O 0.6247(13) 0.2244(6) 0.3628(4) 0.112(3) Uani 1 1 d . . .
O3 O 0.6150(15) 0.1326(5) 0.2732(4) 0.112(3) Uani 1 1 d . . .
O1W O 0.1901(12) 0.1947(4) 0.4283(3) 0.086(2) Uani 1 1 d . . .
H1W H 0.1119 0.1812 0.3938 0.129 Uiso 1 1 d R . .
H2W H 0.3089 0.2022 0.4052 0.129 Uiso 1 1 d R . .
O2W O 0.7744(13) 0.3151(5) 0.9352(4) 0.101(3) Uani 1 1 d . . .
H3W H 0.8845 0.3062 0.9045 0.152 Uiso 1 1 d R . .
H4W H 0.6716 0.3131 0.9082 0.152 Uiso 1 1 d R . .
N14 N 0.7144(12) 0.6843(4) 0.1847(3) 0.063(2) Uani 1 1 d D . .
O4 O 0.606(2) 0.6461(9) 0.2297(7) 0.092(4) Uani 0.50 1 d PDU A -1
O5 O 0.8903(16) 0.6997(11) 0.1991(7) 0.091(4) Uani 0.50 1 d PDU A -1
O6 O 0.655(2) 0.7189(9) 0.1249(6) 0.076(3) Uani 0.50 1 d PDU A -1
O4A O 0.800(2) 0.6480(8) 0.2390(6) 0.075(3) Uani 0.50 1 d PDU A -2
O5A O 0.793(2) 0.7292(10) 0.1377(8) 0.103(4) Uani 0.50 1 d PDU A -2
O6A O 0.5319(16) 0.6657(10) 0.1837(7) 0.081(3) Uani 0.50 1 d PDU A -2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0378(4) 0.0365(3) 0.0298(3) -0.0060(2) -0.0111(2) 0.0106(3)
Ag2 0.0349(4) 0.0364(3) 0.0269(2) 0.0016(2) -0.0084(2) -0.0105(3)
N1 0.031(4) 0.031(3) 0.034(3) -0.008(2) -0.013(2) 0.001(3)
N2 0.040(4) 0.035(3) 0.030(2) -0.012(2) -0.016(2) 0.006(3)
N3 0.032(4) 0.016(3) 0.028(2) -0.0054(19) -0.005(2) 0.001(2)
N4 0.027(4) 0.030(3) 0.027(2) 0.001(2) -0.007(2) -0.007(3)
N5 0.040(4) 0.029(3) 0.028(2) -0.004(2) -0.005(2) 0.003(3)
N6 0.022(3) 0.025(3) 0.021(2) -0.0048(19) -0.0011(19) 0.001(3)
N7 0.035(4) 0.029(3) 0.029(2) 0.006(2) -0.015(2) -0.003(3)
N8 0.032(4) 0.034(3) 0.028(2) 0.005(2) -0.007(2) -0.015(3)
N9 0.029(3) 0.023(3) 0.024(2) 0.0004(19) -0.006(2) 0.002(2)
N10 0.044(4) 0.045(4) 0.025(2) 0.000(2) -0.006(2) 0.010(3)
N11 0.042(4) 0.031(3) 0.028(3) -0.001(2) -0.009(2) 0.006(3)
N12 0.027(3) 0.022(3) 0.022(2) 0.0042(19) -0.008(2) 0.004(2)
C1 0.039(5) 0.031(4) 0.029(3) -0.009(3) -0.009(3) 0.002(3)
C2 0.034(4) 0.020(4) 0.035(3) -0.007(2) -0.016(3) 0.005(3)
C3 0.033(5) 0.028(4) 0.024(3) -0.008(2) -0.001(2) -0.007(3)
C4 0.040(5) 0.035(4) 0.022(3) -0.004(2) -0.001(3) -0.012(3)
C5 0.022(4) 0.024(4) 0.024(3) -0.007(2) -0.003(2) 0.006(3)
C6 0.024(4) 0.016(3) 0.027(3) -0.002(2) -0.005(2) -0.001(3)
C7 0.030(4) 0.025(4) 0.022(3) -0.006(2) -0.010(2) -0.002(3)
C8 0.040(5) 0.027(4) 0.031(3) -0.003(3) -0.014(3) -0.003(3)
C9 0.072(7) 0.026(4) 0.033(3) 0.000(3) -0.028(3) 0.001(4)
C10 0.038(5) 0.028(4) 0.024(3) -0.005(2) -0.012(2) 0.001(3)
C11 0.025(4) 0.045(5) 0.037(3) -0.021(3) -0.004(3) -0.003(4)
C12 0.028(5) 0.056(6) 0.058(4) -0.035(4) -0.005(3) 0.012(4)
C13 0.031(5) 0.052(5) 0.043(4) -0.027(3) 0.002(3) -0.011(4)
C14 0.046(6) 0.047(5) 0.070(5) -0.024(4) -0.039(4) 0.026(4)
C15 0.033(4) 0.028(4) 0.026(3) 0.004(2) -0.009(2) 0.000(3)
C16 0.032(4) 0.027(4) 0.026(3) 0.005(2) -0.008(2) -0.006(3)
C17 0.027(4) 0.035(4) 0.025(3) 0.000(2) -0.001(2) 0.002(3)
C18 0.028(4) 0.030(4) 0.026(3) 0.000(2) -0.009(2) 0.008(3)
C19 0.028(4) 0.015(3) 0.028(3) 0.001(2) -0.008(2) -0.001(3)
C20 0.026(4) 0.025(4) 0.023(3) -0.003(2) -0.005(2) 0.001(3)
C21 0.030(4) 0.020(3) 0.019(2) 0.004(2) -0.009(2) 0.000(3)
C22 0.029(4) 0.023(4) 0.030(3) 0.001(2) -0.008(2) 0.002(3)
C23 0.032(5) 0.024(4) 0.030(3) -0.008(2) -0.007(3) 0.000(3)
C24 0.030(4) 0.026(4) 0.026(3) -0.002(2) -0.004(2) -0.004(3)
C25 0.027(5) 0.034(4) 0.031(3) 0.001(3) -0.009(3) -0.002(3)
C26 0.029(5) 0.037(4) 0.036(3) 0.002(3) -0.010(3) -0.007(3)
C27 0.024(4) 0.035(4) 0.033(3) 0.000(3) 0.001(3) -0.010(3)
C28 0.039(5) 0.028(4) 0.037(3) 0.003(3) -0.018(3) -0.006(4)
N13 0.073(6) 0.041(4) 0.034(3) 0.004(3) -0.011(3) 0.006(4)
O1 0.087(7) 0.169(10) 0.109(6) 0.001(5) -0.027(5) 0.070(7)
O2 0.090(7) 0.126(8) 0.116(6) -0.065(5) -0.008(5) 0.022(6)
O3 0.184(10) 0.090(6) 0.079(4) 0.015(4) -0.076(5) -0.043(6)
O1W 0.104(6) 0.064(5) 0.088(4) -0.011(3) 0.020(4) -0.029(4)
O2W 0.155(8) 0.079(5) 0.082(4) 0.005(4) -0.061(4) -0.028(5)
N14 0.094(7) 0.042(5) 0.048(4) -0.013(3) 0.025(4) -0.011(5)
O4 0.120(9) 0.079(7) 0.073(6) -0.008(6) 0.015(6) -0.009(7)
O5 0.107(10) 0.095(8) 0.072(7) -0.006(6) -0.027(6) 0.010(8)
O6 0.082(9) 0.090(8) 0.056(5) 0.005(5) -0.029(5) 0.011(7)
O4A 0.106(9) 0.076(7) 0.044(5) -0.012(5) -0.026(6) 0.019(7)
O5A 0.120(10) 0.099(8) 0.086(7) 0.016(6) 0.003(7) -0.002(8)
O6A 0.090(9) 0.089(8) 0.066(6) -0.008(6) -0.029(6) 0.012(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.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N11 2.185(5) 2_756 ?
Ag1 N1 2.194(5) . ?
Ag1 N2 2.407(5) 2_655 ?
Ag1 N10 2.502(5) 1_554 ?
Ag2 N4 2.185(5) . ?
Ag2 N8 2.194(5) 2_766 ?
Ag2 N7 2.477(5) . ?
Ag2 N5 2.529(4) 2_666 ?
N1 C1 1.303(8) . ?
N1 N2 1.383(7) . ?
N2 C2 1.315(8) . ?
N2 Ag1 2.407(5) 2_655 ?
N3 C1 1.350(8) . ?
N3 C2 1.363(7) . ?
N3 C5 1.489(7) . ?
N4 C3 1.320(7) . ?
N4 N5 1.405(7) . ?
N5 C4 1.290(8) . ?
N5 Ag2 2.529(4) 2_666 ?
N6 C3 1.345(8) . ?
N6 C4 1.366(7) . ?
N6 C7 1.500(7) . ?
N7 C15 1.295(8) . ?
N7 N8 1.409(6) . ?
N8 C16 1.315(8) . ?
N8 Ag2 2.194(5) 2_766 ?
N9 C16 1.351(8) . ?
N9 C15 1.358(7) . ?
N9 C19 1.483(8) . ?
N10 C17 1.307(8) . ?
N10 N11 1.392(7) . ?
N10 Ag1 2.502(5) 1_556 ?
N11 C18 1.310(7) . ?
N11 Ag1 2.185(5) 2_756 ?
N12 C17 1.349(7) . ?
N12 C18 1.351(8) . ?
N12 C21 1.503(6) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 H3 0.9400 . ?
C4 H4 0.9400 . ?
C5 C11 1.516(9) . ?
C5 C10 1.531(8) . ?
C5 C6 1.549(7) . ?
C6 C7 1.534(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C13 1.503(9) . ?
C7 C8 1.530(9) . ?
C8 C9 1.537(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C14 1.504(11) . ?
C9 C10 1.549(9) . ?
C9 H9 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.552(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C14 1.498(12) . ?
C12 C13 1.562(9) . ?
C12 H12 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
C18 H18 0.9400 . ?
C19 C25 1.532(9) . ?
C19 C24 1.533(8) . ?
C19 C20 1.540(7) . ?
C20 C21 1.532(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 C27 1.507(9) . ?
C21 C22 1.530(8) . ?
C22 C23 1.528(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C28 1.509(10) . ?
C23 C24 1.543(9) . ?
C23 H23 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 C26 1.542(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 C28 1.533(9) . ?
C26 C27 1.535(8) . ?
C26 H26 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
N13 O2 1.196(9) . ?
N13 O1 1.200(10) . ?
N13 O3 1.217(9) . ?
O1W H1W 0.8503 . ?
O1W H2W 0.8496 . ?
O2W H3W 0.8500 . ?
O2W H4W 0.8500 . ?
N14 O5A 1.162(8) . ?
N14 O4 1.177(8) . ?
N14 O6 1.225(8) . ?
N14 O4A 1.231(8) . ?
N14 O5 1.236(8) . ?
N14 O6A 1.248(8) . ?

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
N11 Ag1 N1 143.54(17) 2_756 . ?
N11 Ag1 N2 98.34(19) 2_756 2_655 ?
N1 Ag1 N2 112.75(19) . 2_655 ?
N11 Ag1 N10 107.33(19) 2_756 1_554 ?
N1 Ag1 N10 94.93(18) . 1_554 ?
N2 Ag1 N10 83.83(19) 2_655 1_554 ?
N4 Ag2 N8 149.55(17) . 2_766 ?
N4 Ag2 N7 99.46(19) . . ?
N8 Ag2 N7 103.6(2) 2_766 . ?
N4 Ag2 N5 108.50(18) . 2_666 ?
N8 Ag2 N5 94.42(17) 2_766 2_666 ?
N7 Ag2 N5 81.64(16) . 2_666 ?
C1 N1 N2 107.7(5) . . ?
C1 N1 Ag1 128.3(4) . . ?
N2 N1 Ag1 121.0(3) . . ?
C2 N2 N1 106.1(4) . . ?
C2 N2 Ag1 134.1(4) . 2_655 ?
N1 N2 Ag1 116.6(4) . 2_655 ?
C1 N3 C2 104.4(5) . . ?
C1 N3 C5 128.9(5) . . ?
C2 N3 C5 126.6(5) . . ?
C3 N4 N5 106.1(5) . . ?
C3 N4 Ag2 135.9(4) . . ?
N5 N4 Ag2 116.5(3) . . ?
C4 N5 N4 107.2(5) . . ?
C4 N5 Ag2 123.5(5) . 2_666 ?
N4 N5 Ag2 111.4(3) . 2_666 ?
C3 N6 C4 105.3(5) . . ?
C3 N6 C7 128.9(5) . . ?
C4 N6 C7 125.8(5) . . ?
C15 N7 N8 106.4(5) . . ?
C15 N7 Ag2 125.5(4) . . ?
N8 N7 Ag2 121.0(4) . . ?
C16 N8 N7 106.8(5) . . ?
C16 N8 Ag2 129.3(4) . 2_766 ?
N7 N8 Ag2 120.6(4) . 2_766 ?
C16 N9 C15 105.3(5) . . ?
C16 N9 C19 128.3(5) . . ?
C15 N9 C19 125.9(5) . . ?
C17 N10 N11 106.0(5) . . ?
C17 N10 Ag1 126.1(5) . 1_556 ?
N11 N10 Ag1 109.4(4) . 1_556 ?
C18 N11 N10 107.5(5) . . ?
C18 N11 Ag1 130.4(4) . 2_756 ?
N10 N11 Ag1 120.5(4) . 2_756 ?
C17 N12 C18 105.4(5) . . ?
C17 N12 C21 127.1(5) . . ?
C18 N12 C21 127.2(4) . . ?
N1 C1 N3 110.9(5) . . ?
N1 C1 H1 124.6 . . ?
N3 C1 H1 124.6 . . ?
N2 C2 N3 110.9(5) . . ?
N2 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
N4 C3 N6 110.6(5) . . ?
N4 C3 H3 124.7 . . ?
N6 C3 H3 124.7 . . ?
N5 C4 N6 110.7(6) . . ?
N5 C4 H4 124.6 . . ?
N6 C4 H4 124.6 . . ?
N3 C5 C11 109.4(5) . . ?
N3 C5 C10 108.7(4) . . ?
C11 C5 C10 111.9(6) . . ?
N3 C5 C6 107.9(5) . . ?
C11 C5 C6 109.7(4) . . ?
C10 C5 C6 109.2(5) . . ?
C7 C6 C5 108.2(5) . . ?
C7 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C7 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
N6 C7 C13 109.3(4) . . ?
N6 C7 C8 109.3(5) . . ?
C13 C7 C8 110.3(6) . . ?
N6 C7 C6 108.3(5) . . ?
C13 C7 C6 109.5(5) . . ?
C8 C7 C6 110.2(5) . . ?
C7 C8 C9 108.8(6) . . ?
C7 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C14 C9 C8 110.7(5) . . ?
C14 C9 C10 109.7(6) . . ?
C8 C9 C10 108.0(5) . . ?
C14 C9 H9 109.5 . . ?
C8 C9 H9 109.5 . . ?
C10 C9 H9 109.5 . . ?
C5 C10 C9 108.5(5) . . ?
C5 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C5 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C5 C11 C12 107.6(6) . . ?
C5 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
C5 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C14 C12 C11 110.3(6) . . ?
C14 C12 C13 109.5(7) . . ?
C11 C12 C13 108.6(6) . . ?
C14 C12 H12 109.5 . . ?
C11 C12 H12 109.5 . . ?
C13 C12 H12 109.5 . . ?
C7 C13 C12 109.1(5) . . ?
C7 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
C7 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C12 C14 C9 110.6(6) . . ?
C12 C14 H14A 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N7 C15 N9 111.3(5) . . ?
N7 C15 H15 124.4 . . ?
N9 C15 H15 124.4 . . ?
N8 C16 N9 110.2(5) . . ?
N8 C16 H16 124.9 . . ?
N9 C16 H16 124.9 . . ?
N10 C17 N12 111.1(6) . . ?
N10 C17 H17 124.4 . . ?
N12 C17 H17 124.4 . . ?
N11 C18 N12 110.0(5) . . ?
N11 C18 H18 125.0 . . ?
N12 C18 H18 125.0 . . ?
N9 C19 C25 110.4(5) . . ?
N9 C19 C24 108.3(5) . . ?
C25 C19 C24 110.5(5) . . ?
N9 C19 C20 109.3(5) . . ?
C25 C19 C20 108.6(5) . . ?
C24 C19 C20 109.7(5) . . ?
C21 C20 C19 108.6(5) . . ?
C21 C20 H20A 110.0 . . ?
C19 C20 H20A 110.0 . . ?
C21 C20 H20B 110.0 . . ?
C19 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
N12 C21 C27 111.4(4) . . ?
N12 C21 C22 108.1(5) . . ?
C27 C21 C22 109.4(5) . . ?
N12 C21 C20 106.7(4) . . ?
C27 C21 C20 110.4(5) . . ?
C22 C21 C20 110.7(5) . . ?
C23 C22 C21 109.0(5) . . ?
C23 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C28 C23 C22 110.1(5) . . ?
C28 C23 C24 109.2(6) . . ?
C22 C23 C24 108.8(5) . . ?
C28 C23 H23 109.6 . . ?
C22 C23 H23 109.6 . . ?
C24 C23 H23 109.6 . . ?
C19 C24 C23 109.4(5) . . ?
C19 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
C19 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
C19 C25 C26 108.6(5) . . ?
C19 C25 H25A 110.0 . . ?
C26 C25 H25A 110.0 . . ?
C19 C25 H25B 110.0 . . ?
C26 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
C28 C26 C27 109.0(6) . . ?
C28 C26 C25 109.3(5) . . ?
C27 C26 C25 110.3(5) . . ?
C28 C26 H26 109.4 . . ?
C27 C26 H26 109.4 . . ?
C25 C26 H26 109.4 . . ?
C21 C27 C26 108.8(5) . . ?
C21 C27 H27A 109.9 . . ?
C26 C27 H27A 109.9 . . ?
C21 C27 H27B 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C23 C28 C26 110.0(5) . . ?
C23 C28 H28A 109.7 . . ?
C26 C28 H28A 109.7 . . ?
C23 C28 H28B 109.7 . . ?
C26 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
O2 N13 O1 121.3(8) . . ?
O2 N13 O3 121.4(10) . . ?
O1 N13 O3 117.3(9) . . ?
H1W O1W H2W 108.6 . . ?
H3W O2W H4W 108.4 . . ?
O4 N14 O6 122.6(9) . . ?
O5A N14 O4A 124.7(9) . . ?
O4 N14 O5 121.7(9) . . ?
O6 N14 O5 115.3(8) . . ?
O5A N14 O6A 122.7(9) . . ?
O4A N14 O6A 112.6(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Ag1 N1 C1 20.8(8) 2_756 . . . ?
N2 Ag1 N1 C1 167.1(5) 2_655 . . . ?
N10 Ag1 N1 C1 -107.5(6) 1_554 . . . ?
N11 Ag1 N1 N2 178.7(4) 2_756 . . . ?
N2 Ag1 N1 N2 -34.9(6) 2_655 . . . ?
N10 Ag1 N1 N2 50.4(5) 1_554 . . . ?
C1 N1 N2 C2 0.9(7) . . . . ?
Ag1 N1 N2 C2 -161.0(5) . . . . ?
C1 N1 N2 Ag1 -161.8(4) . . . 2_655 ?
Ag1 N1 N2 Ag1 36.2(6) . . . 2_655 ?
N8 Ag2 N4 C3 5.8(9) 2_766 . . . ?
N7 Ag2 N4 C3 -133.1(6) . . . . ?
N5 Ag2 N4 C3 142.6(6) 2_666 . . . ?
N8 Ag2 N4 N5 169.8(4) 2_766 . . . ?
N7 Ag2 N4 N5 30.9(4) . . . . ?
N5 Ag2 N4 N5 -53.4(5) 2_666 . . . ?
C3 N4 N5 C4 1.2(7) . . . . ?
Ag2 N4 N5 C4 -167.3(4) . . . . ?
C3 N4 N5 Ag2 -136.7(4) . . . 2_666 ?
Ag2 N4 N5 Ag2 54.8(4) . . . 2_666 ?
N4 Ag2 N7 C15 -12.9(5) . . . . ?
N8 Ag2 N7 C15 -172.8(5) 2_766 . . . ?
N5 Ag2 N7 C15 94.6(5) 2_666 . . . ?
N4 Ag2 N7 N8 -159.2(4) . . . . ?
N8 Ag2 N7 N8 40.8(5) 2_766 . . . ?
N5 Ag2 N7 N8 -51.7(4) 2_666 . . . ?
C15 N7 N8 C16 -0.9(7) . . . . ?
Ag2 N7 N8 C16 151.1(4) . . . . ?
C15 N7 N8 Ag2 160.4(4) . . . 2_766 ?
Ag2 N7 N8 Ag2 -47.6(6) . . . 2_766 ?
C17 N10 N11 C18 -0.9(7) . . . . ?
Ag1 N10 N11 C18 137.8(4) 1_556 . . . ?
C17 N10 N11 Ag1 166.3(4) . . . 2_756 ?
Ag1 N10 N11 Ag1 -54.9(5) 1_556 . . 2_756 ?
N2 N1 C1 N3 -1.1(8) . . . . ?
Ag1 N1 C1 N3 159.1(4) . . . . ?
C2 N3 C1 N1 0.8(8) . . . . ?
C5 N3 C1 N1 -175.5(6) . . . . ?
N1 N2 C2 N3 -0.4(8) . . . . ?
Ag1 N2 C2 N3 157.9(4) 2_655 . . . ?
C1 N3 C2 N2 -0.2(8) . . . . ?
C5 N3 C2 N2 176.2(6) . . . . ?
N5 N4 C3 N6 -1.5(7) . . . . ?
Ag2 N4 C3 N6 163.7(5) . . . . ?
C4 N6 C3 N4 1.2(7) . . . . ?
C7 N6 C3 N4 -176.7(6) . . . . ?
N4 N5 C4 N6 -0.5(7) . . . . ?
Ag2 N5 C4 N6 131.0(4) 2_666 . . . ?
C3 N6 C4 N5 -0.4(7) . . . . ?
C7 N6 C4 N5 177.6(6) . . . . ?
C1 N3 C5 C11 -122.3(7) . . . . ?
C2 N3 C5 C11 62.1(8) . . . . ?
C1 N3 C5 C10 115.3(7) . . . . ?
C2 N3 C5 C10 -60.3(8) . . . . ?
C1 N3 C5 C6 -3.0(8) . . . . ?
C2 N3 C5 C6 -178.6(6) . . . . ?
N3 C5 C6 C7 178.6(5) . . . . ?
C11 C5 C6 C7 -62.3(7) . . . . ?
C10 C5 C6 C7 60.6(6) . . . . ?
C3 N6 C7 C13 -133.7(7) . . . . ?
C4 N6 C7 C13 48.8(8) . . . . ?
C3 N6 C7 C8 -13.0(9) . . . . ?
C4 N6 C7 C8 169.5(6) . . . . ?
C3 N6 C7 C6 107.1(7) . . . . ?
C4 N6 C7 C6 -70.4(7) . . . . ?
C5 C6 C7 N6 -179.6(5) . . . . ?
C5 C6 C7 C13 61.3(6) . . . . ?
C5 C6 C7 C8 -60.1(7) . . . . ?
N6 C7 C8 C9 -179.6(5) . . . . ?
C13 C7 C8 C9 -59.4(7) . . . . ?
C6 C7 C8 C9 61.5(7) . . . . ?
C7 C8 C9 C14 58.2(7) . . . . ?
C7 C8 C9 C10 -61.9(7) . . . . ?
N3 C5 C10 C9 180.0(5) . . . . ?
C11 C5 C10 C9 59.1(6) . . . . ?
C6 C5 C10 C9 -62.6(7) . . . . ?
C14 C9 C10 C5 -57.9(7) . . . . ?
C8 C9 C10 C5 62.9(7) . . . . ?
N3 C5 C11 C12 -179.5(5) . . . . ?
C10 C5 C11 C12 -58.9(6) . . . . ?
C6 C5 C11 C12 62.4(7) . . . . ?
C5 C11 C12 C14 58.9(7) . . . . ?
C5 C11 C12 C13 -61.2(8) . . . . ?
N6 C7 C13 C12 -179.9(6) . . . . ?
C8 C7 C13 C12 60.0(7) . . . . ?
C6 C7 C13 C12 -61.4(7) . . . . ?
C14 C12 C13 C7 -59.3(8) . . . . ?
C11 C12 C13 C7 61.3(8) . . . . ?
C11 C12 C14 C9 -60.9(8) . . . . ?
C13 C12 C14 C9 58.6(8) . . . . ?
C8 C9 C14 C12 -59.0(8) . . . . ?
C10 C9 C14 C12 60.1(7) . . . . ?
N8 N7 C15 N9 1.3(7) . . . . ?
Ag2 N7 C15 N9 -149.1(4) . . . . ?
C16 N9 C15 N7 -1.2(7) . . . . ?
C19 N9 C15 N7 -174.3(6) . . . . ?
N7 N8 C16 N9 0.2(7) . . . . ?
Ag2 N8 C16 N9 -158.9(4) 2_766 . . . ?
C15 N9 C16 N8 0.6(7) . . . . ?
C19 N9 C16 N8 173.5(6) . . . . ?
N11 N10 C17 N12 0.1(8) . . . . ?
Ag1 N10 C17 N12 -129.6(5) 1_556 . . . ?
C18 N12 C17 N10 0.7(7) . . . . ?
C21 N12 C17 N10 -173.0(6) . . . . ?
N10 N11 C18 N12 1.4(7) . . . . ?
Ag1 N11 C18 N12 -164.1(5) 2_756 . . . ?
C17 N12 C18 N11 -1.3(7) . . . . ?
C21 N12 C18 N11 172.4(5) . . . . ?
C16 N9 C19 C25 130.4(6) . . . . ?
C15 N9 C19 C25 -58.0(7) . . . . ?
C16 N9 C19 C24 -108.5(6) . . . . ?
C15 N9 C19 C24 63.1(8) . . . . ?
C16 N9 C19 C20 11.0(8) . . . . ?
C15 N9 C19 C20 -177.5(6) . . . . ?
N9 C19 C20 C21 -177.8(5) . . . . ?
C25 C19 C20 C21 61.6(6) . . . . ?
C24 C19 C20 C21 -59.2(7) . . . . ?
C17 N12 C21 C27 -47.2(8) . . . . ?
C18 N12 C21 C27 140.4(7) . . . . ?
C17 N12 C21 C22 -167.4(6) . . . . ?
C18 N12 C21 C22 20.2(9) . . . . ?
C17 N12 C21 C20 73.4(7) . . . . ?
C18 N12 C21 C20 -99.0(7) . . . . ?
C19 C20 C21 N12 177.1(5) . . . . ?
C19 C20 C21 C27 -61.7(6) . . . . ?
C19 C20 C21 C22 59.6(6) . . . . ?
N12 C21 C22 C23 -177.4(5) . . . . ?
C27 C21 C22 C23 61.1(6) . . . . ?
C20 C21 C22 C23 -60.8(7) . . . . ?
C21 C22 C23 C28 -59.2(7) . . . . ?
C21 C22 C23 C24 60.5(7) . . . . ?
N9 C19 C24 C23 179.7(5) . . . . ?
C25 C19 C24 C23 -59.2(6) . . . . ?
C20 C19 C24 C23 60.5(7) . . . . ?
C28 C23 C24 C19 59.2(6) . . . . ?
C22 C23 C24 C19 -61.0(7) . . . . ?
N9 C19 C25 C26 179.2(4) . . . . ?
C24 C19 C25 C26 59.3(6) . . . . ?
C20 C19 C25 C26 -61.0(6) . . . . ?
C19 C25 C26 C28 -59.7(6) . . . . ?
C19 C25 C26 C27 60.2(6) . . . . ?
N12 C21 C27 C26 178.4(5) . . . . ?
C22 C21 C27 C26 -62.1(7) . . . . ?
C20 C21 C27 C26 60.0(6) . . . . ?
C28 C26 C27 C21 60.7(7) . . . . ?
C25 C26 C27 C21 -59.3(7) . . . . ?
C22 C23 C28 C26 58.7(7) . . . . ?
C24 C23 C28 C26 -60.7(6) . . . . ?
C27 C26 C28 C23 -59.2(7) . . . . ?
C25 C26 C28 C23 61.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.846
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.846
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.091

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL IP1-1146 in P-1
CELL 0.71073 6.5192 15.4818 16.9913 89.230 84.607 85.574
ZERR 2.00 0.0006 0.0011 0.0012 0.009 0.010 0.009
LATT 1
SFAC C H N O AG
UNIT 56 80 28 16 4
MERG 2
OMIT -2 5 0
OMIT 3 -1 3
OMIT 1 8 0
OMIT 3 -2 4
OMIT -3 1 1
OMIT -3 -2 1

SHEL 0.81 8

DFIX 1.22 0.01 N14 O4 N14 O5 N14 O6
DFIX 2.09 0.01 O4 O5 O4 o6 O5 O6
DFIX 1.22 0.01 N14 O4a N14 O5a N14 O6a
DFIX 2.09 0.01 O4a O5a O4a o6a O5a O6a

SIMU 0.005 O4 > O6a

EQIV $1 -1+X, Y, Z
EQIV $2 2-X, 1-Y, 1-Z
EQIV $3 1-X, 1-Y, 1-Z

RTAB H..O H1W O1_$1
RTAB H..O H2W O2
RTAB H..O H3W O5_$2
RTAB H..O H3W O5A_$2
RTAB H..O H4W O6_$3
RTAB H..O H4W O6A_$3

RTAB O..O O1W O1_$1
RTAB O..O O1W O2
RTAB O..O O2W O5_$2
RTAB O..O O2W O5A_$2
RTAB O..O O2W O6_$3
RTAB O..O O2W O6A_$3

RTAB XHY O1W H1W O1_$1
RTAB XHY O1W H2W O2
RTAB XHY O2W H3W O5_$2
RTAB XHY O2W H3W O5A_$2
RTAB XHY O2W H4W O6_$3
RTAB XHY O2W H4W O6A_$3

FMAP 2
PLAN 25
SIZE 0.18 0.22 0.26
ACTA
BOND $H
CONF
LIST 4
L.S. 6
TEMP -60.00
WGHT 0.042400
FVAR 0.99760
AG1 5 0.728804 0.020353 0.057610 11.00000 0.03783 0.03648 =
0.02976 -0.00601 -0.01115 0.01061
AG2 5 0.747212 0.530127 0.436911 11.00000 0.03495 0.03639 =
0.02692 0.00159 -0.00842 -0.01045
N1 3 0.439915 0.103431 0.072837 11.00000 0.03109 0.03136 =
0.03390 -0.00751 -0.01334 0.00131
N2 3 0.304668 0.109722 0.014604 11.00000 0.03978 0.03465 =
0.03026 -0.01219 -0.01607 0.00607
N3 3 0.237075 0.221348 0.094643 11.00000 0.03220 0.01569 =
0.02849 -0.00536 -0.00509 0.00084
N4 3 0.483702 0.486362 0.382066 11.00000 0.02739 0.03031 =
0.02650 0.00063 -0.00653 -0.00653
N5 3 0.373643 0.422763 0.423373 11.00000 0.03954 0.02946 =
0.02765 -0.00390 -0.00471 0.00328
N6 3 0.275546 0.433969 0.303889 11.00000 0.02248 0.02509 =
0.02093 -0.00482 -0.00111 0.00101
N7 3 0.855071 0.394982 0.506573 11.00000 0.03545 0.02873 =
0.02947 0.00648 -0.01506 -0.00332
N8 3 0.976421 0.396684 0.570858 11.00000 0.03236 0.03408 =
0.02780 0.00521 -0.00731 -0.01511
N9 3 0.786459 0.286184 0.585961 11.00000 0.02868 0.02338 =
0.02399 0.00036 -0.00628 0.00174
N10 3 0.841980 0.079682 0.924243 11.00000 0.04362 0.04488 =
0.02498 0.00039 -0.00614 0.00968
N11 3 0.992450 0.022089 0.886092 11.00000 0.04204 0.03061 =
0.02783 -0.00052 -0.00919 0.00578
N12 3 0.784155 0.070748 0.799816 11.00000 0.02749 0.02240 =
0.02199 0.00417 -0.00810 0.00410
C1 1 0.394697 0.169602 0.119509 11.00000 0.03930 0.03097 =
0.02886 -0.00884 -0.00920 0.00185
AFIX 43
H1 2 0.462705 0.179930 0.164468 11.00000 -1.20000
AFIX 0
C2 1 0.185671 0.181259 0.029123 11.00000 0.03431 0.02041 =
0.03548 -0.00670 -0.01569 0.00537
AFIX 43
H2 2 0.079413 0.201979 -0.001557 11.00000 -1.20000
AFIX 0
C3 1 0.416953 0.491495 0.311034 11.00000 0.03313 0.02813 =
0.02444 -0.00807 -0.00079 -0.00747
AFIX 43
H3 2 0.462035 0.530027 0.270997 11.00000 -1.20000
AFIX 0
C4 1 0.253782 0.393112 0.375595 11.00000 0.03992 0.03463 =
0.02177 -0.00423 -0.00085 -0.01237
AFIX 43
H4 2 0.163780 0.349367 0.388393 11.00000 -1.20000
AFIX 0
C5 1 0.145728 0.306153 0.126890 11.00000 0.02181 0.02406 =
0.02418 -0.00713 -0.00282 0.00591
C6 1 0.256849 0.325970 0.200500 11.00000 0.02413 0.01587 =
0.02684 -0.00151 -0.00494 -0.00095
AFIX 23
H6A 2 0.235253 0.280926 0.240853 11.00000 -1.20000
H6B 2 0.405681 0.327195 0.185973 11.00000 -1.20000
AFIX 0
C7 1 0.167260 0.414356 0.232887 11.00000 0.03025 0.02509 =
0.02204 -0.00628 -0.00953 -0.00189
C8 1 0.202176 0.484944 0.170203 11.00000 0.04041 0.02706 =
0.03074 -0.00309 -0.01362 -0.00276
AFIX 23
H8A 2 0.350325 0.486901 0.154561 11.00000 -1.20000
H8B 2 0.149003 0.541574 0.191721 11.00000 -1.20000
AFIX 0
C9 1 0.089085 0.464442 0.098083 11.00000 0.07186 0.02624 =
0.03257 0.00034 -0.02800 0.00095
AFIX 13
H9 2 0.108456 0.510322 0.057508 11.00000 -1.20000
AFIX 0
C10 1 0.184462 0.376441 0.064162 11.00000 0.03752 0.02836 =
0.02371 -0.00455 -0.01204 0.00112
AFIX 23
H10A 2 0.120891 0.363071 0.016186 11.00000 -1.20000
H10B 2 0.333268 0.379094 0.050464 11.00000 -1.20000
AFIX 0
C11 1 -0.082858 0.300303 0.150557 11.00000 0.02529 0.04548 =
0.03698 -0.02094 -0.00391 -0.00313
AFIX 23
H11A 2 -0.103183 0.255556 0.191285 11.00000 -1.20000
H11B 2 -0.153171 0.285188 0.104707 11.00000 -1.20000
AFIX 0
C12 1 -0.171903 0.390120 0.182997 11.00000 0.02792 0.05619 =
0.05837 -0.03489 -0.00465 0.01226
AFIX 13
H12 2 -0.321804 0.388442 0.198448 11.00000 -1.20000
AFIX 0
C13 1 -0.059763 0.410775 0.257021 11.00000 0.03105 0.05170 =
0.04270 -0.02668 0.00174 -0.01057
AFIX 23
H13A 2 -0.116954 0.466491 0.279420 11.00000 -1.20000
H13B 2 -0.081015 0.365800 0.297465 11.00000 -1.20000
AFIX 0
C14 1 -0.137943 0.458944 0.121321 11.00000 0.04554 0.04656 =
0.06983 -0.02432 -0.03894 0.02631
AFIX 23
H14A 2 -0.198420 0.514974 0.141971 11.00000 -1.20000
H14B 2 -0.207199 0.445669 0.074669 11.00000 -1.20000
AFIX 0
C15 1 0.747726 0.328139 0.517595 11.00000 0.03339 0.02787 =
0.02645 0.00428 -0.00905 -0.00001
AFIX 43
H15 2 0.654970 0.310890 0.482767 11.00000 -1.20000
AFIX 0
C16 1 0.929995 0.330620 0.616805 11.00000 0.03151 0.02705 =
0.02573 0.00467 -0.00845 -0.00553
AFIX 43
H16 2 0.988291 0.316368 0.664276 11.00000 -1.20000
AFIX 0
C17 1 0.721193 0.107170 0.870511 11.00000 0.02686 0.03486 =
0.02512 -0.00044 -0.00081 0.00156
AFIX 43
H17 2 0.605587 0.147091 0.879900 11.00000 -1.20000
AFIX 0
C18 1 0.951894 0.017326 0.812288 11.00000 0.02812 0.03007 =
0.02606 0.00011 -0.00878 0.00822
AFIX 43
H18 2 1.028249 -0.018045 0.773708 11.00000 -1.20000
AFIX 0
C19 1 0.705335 0.203088 0.613775 11.00000 0.02765 0.01546 =
0.02833 0.00082 -0.00781 -0.00122
C20 1 0.778253 0.180230 0.695619 11.00000 0.02569 0.02517 =
0.02295 -0.00321 -0.00474 0.00095
AFIX 23
H20A 2 0.929490 0.177034 0.692743 11.00000 -1.20000
H20B 2 0.723577 0.225042 0.733833 11.00000 -1.20000
AFIX 0
C21 1 0.700274 0.092621 0.721954 11.00000 0.02992 0.02003 =
0.01946 0.00405 -0.00883 0.00032
C22 1 0.784252 0.021793 0.662935 11.00000 0.02941 0.02283 =
0.02960 0.00117 -0.00841 0.00158
AFIX 23
H22A 2 0.935647 0.016999 0.658845 11.00000 -1.20000
H22B 2 0.735849 -0.034114 0.681071 11.00000 -1.20000
AFIX 0
C23 1 0.708830 0.044944 0.582287 11.00000 0.03166 0.02450 =
0.02994 -0.00782 -0.00671 0.00035
AFIX 13
H23 2 0.761847 -0.000690 0.543725 11.00000 -1.20000
AFIX 0
C24 1 0.790108 0.132361 0.554497 11.00000 0.03018 0.02591 =
0.02550 -0.00179 -0.00356 -0.00382
AFIX 23
H24A 2 0.941493 0.127830 0.550530 11.00000 -1.20000
H24B 2 0.746047 0.147339 0.502124 11.00000 -1.20000
AFIX 0
C25 1 0.468640 0.210753 0.620965 11.00000 0.02663 0.03415 =
0.03084 0.00084 -0.00862 -0.00209
AFIX 23
H25A 2 0.418848 0.226673 0.569683 11.00000 -1.20000
H25B 2 0.415649 0.255857 0.659135 11.00000 -1.20000
AFIX 0
C26 1 0.391739 0.122698 0.648779 11.00000 0.02903 0.03662 =
0.03646 0.00239 -0.01048 -0.00745
AFIX 13
H26 2 0.238803 0.126592 0.653197 11.00000 -1.20000
AFIX 0
C27 1 0.467435 0.097745 0.729468 11.00000 0.02394 0.03486 =
0.03261 -0.00046 0.00107 -0.00999
AFIX 23
H27A 2 0.412500 0.141208 0.768929 11.00000 -1.20000
H27B 2 0.418731 0.041608 0.746731 11.00000 -1.20000
AFIX 0
C28 1 0.475659 0.052975 0.588437 11.00000 0.03921 0.02843 =
0.03705 0.00263 -0.01761 -0.00559
AFIX 23
H28A 2 0.423016 -0.002733 0.604822 11.00000 -1.20000
H28B 2 0.428309 0.068400 0.536657 11.00000 -1.20000
AFIX 0
N13 3 0.709195 0.169784 0.319373 11.00000 0.07327 0.04133 =
0.03400 0.00376 -0.01101 0.00561
O1 4 0.889157 0.147533 0.321282 11.00000 0.08728 0.16904 =
0.10890 0.00127 -0.02692 0.06954
O2 4 0.624706 0.224375 0.362816 11.00000 0.08966 0.12617 =
0.11608 -0.06483 -0.00800 0.02184
O3 4 0.614963 0.132633 0.273225 11.00000 0.18431 0.08978 =
0.07942 0.01463 -0.07647 -0.04294
O1W 4 0.190094 0.194744 0.428255 11.00000 0.10446 0.06382 =
0.08801 -0.01143 0.01984 -0.02934
AFIX 3
H1W 2 0.111944 0.181164 0.393775 11.00000 -1.50000
H2W 2 0.308894 0.202164 0.405215 11.00000 -1.50000
AFIX 0
O2W 4 0.774394 0.315095 0.935234 11.00000 0.15493 0.07929 =
0.08165 0.00510 -0.06084 -0.02843
AFIX 3
H3W 2 0.884454 0.306195 0.904514 11.00000 -1.50000
H4W 2 0.671594 0.313075 0.908204 11.00000 -1.50000
AFIX 0
MOLE 1
N14 3 0.714391 0.684299 0.184729 11.00000 0.09385 0.04229 =
0.04751 -0.01340 0.02488 -0.01087
PART -1
O4 4 0.605872 0.646081 0.229700 10.50000 0.12025 0.07929 =
0.07259 -0.00780 0.01475 -0.00851
O5 4 0.890255 0.699715 0.199142 10.50000 0.10701 0.09522 =
0.07186 -0.00589 -0.02698 0.01031
O6 4 0.654523 0.718929 0.124891 10.50000 0.08197 0.09043 =
0.05610 0.00489 -0.02867 0.01114
PART -2
O4A 4 0.800329 0.648048 0.239022 10.50000 0.10589 0.07636 =
0.04364 -0.01218 -0.02600 0.01935
O5A 4 0.793430 0.729213 0.137733 10.50000 0.11969 0.09888 =
0.08600 0.01609 0.00329 -0.00167
O6A 4 0.531864 0.665653 0.183697 10.50000 0.08962 0.08870 =
0.06579 -0.00846 -0.02860 0.01209
HKLF 4

REM IP1-1146 in P-1
REM R1 = 0.0409 for 3473 Fo > 4sig(Fo) and 0.0673 for all 5659 data
REM 496 parameters refined using 48 restraints

END

WGHT 0.0424 0.0000
REM Highest difference peak 0.458, deepest hole -0.572, 1-sigma level 0.091
Q1 1 0.9833 -0.0147 0.9608 11.00000 0.05 0.46
Q2 1 0.9659 0.5046 0.4461 11.00000 0.05 0.46
Q3 1 0.8614 0.5193 0.5192 11.00000 0.05 0.44
Q4 1 0.4749 0.4249 0.4751 11.00000 0.05 0.41
Q5 1 0.6919 0.7376 0.1255 11.00000 0.05 0.41
Q6 1 0.6485 -0.0215 0.0208 11.00000 0.05 0.38
Q7 1 0.5259 0.2003 0.2985 11.00000 0.05 0.38
Q8 1 1.0539 -0.0144 0.9165 11.00000 0.05 0.36
Q9 1 0.7245 0.6286 0.2382 11.00000 0.05 0.35
Q10 1 0.7607 0.1068 0.2839 11.00000 0.05 0.31

;

#---------------------------------------------------------

data_(4)
_database_code_depnum_ccdc_archive 'CCDC 867227'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[1,3,5-tri(1,2,4-triazol-4-yl)adamantane]cadmium(II)
Nitrate Hexahydrate
;
_chemical_name_common            
;bis-(1,3,5-tri(1,2,4-triazol-4-yl)adamantane)cadmium(ii)
Nitrate Hexahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C32 H38 Cd N18), 2(N O3), 6(H2 O)'
_chemical_formula_sum            'C32 H50 Cd N20 O12'
_chemical_formula_weight         1019.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.5603(2)
_cell_length_b                   11.5603(2)
_cell_length_c                   53.0233(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6136.7(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11430
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.41

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3156
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8753
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11430
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.41
_reflns_number_total             1408
_reflns_number_gt                1190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Refinement of Cd-organic framework atoms was standard. The CH-hydrogen
atoms were constrained with U(iso) = 1.2U(eq) of the parent C-atom and
with C-H distances 0.93 A (triazole), 0.97 A (CH2 adamantane) and 0.98 A
(CH adamantane).

Some minor problems were associated with the disorder in the region of
non-coordinated anions and water molecules. One water molecule is
equally disordered by symmetry over three positions (1/3O...1/3O 1.11 A),
related by a 3-fold axis. These positions overlap with the additional
water molecule, which adopt two closely separated positions
(O...O 1.29 A) disordered over the 3-fold axis. The nitrate anions are
also disordered by symmetry and overlap with water molecules (third
equivalent). Two anions adopt three positions, related by 3-fold axis
thus the occuppancy factors for the entire NO3- sites were 0.66.
In addition, NO3- group possesses two orientations ad therefore partial
occupancies for NO3- site were set at 0.33, amounting Cd/NO3 1:2
proportion.
It was possible to resolve this disorder with the restrained molecular
geometry for NO3- [N-O 1.222(5); O...O 2.105(5) A] and with restraints
for coplanarity of the atoms (FLAT) and the thermal motion (SIMU) for
the entire NO3- moiety. All the disordered atoms were refined
anisotropically, but the H-atoms were not added for water molecules.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+12.1670P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1408
_refine_ls_number_parameters     141
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.01670(15) Uani 1 6 d S . .
N1 N 0.1440(2) 0.1891(2) 0.02383(4) 0.0235(4) Uani 1 1 d . . .
N2 N 0.2693(2) 0.2127(2) 0.03025(4) 0.0300(5) Uani 1 1 d . . .
N3 N 0.25643(19) 0.39234(19) 0.03835(3) 0.0203(4) Uani 1 1 d . . .
C1 C 0.1387(2) 0.2966(3) 0.02900(5) 0.0246(5) Uani 1 1 d . . .
H1 H 0.0641 0.3059 0.0266 0.030 Uiso 1 1 calc R . .
C2 C 0.3331(3) 0.3339(3) 0.03903(6) 0.0321(6) Uani 1 1 d . . .
H2 H 0.4204 0.3754 0.0450 0.039 Uiso 1 1 calc R . .
C3 C 0.2937(2) 0.5276(2) 0.04769(4) 0.0196(5) Uani 1 1 d . . .
C4 C 0.4337(2) 0.6269(2) 0.03785(4) 0.0209(5) Uani 1 1 d . . .
H4A H 0.4975 0.6016 0.0437 0.025 Uiso 1 1 calc R . .
H4B H 0.4340 0.6269 0.0196 0.025 Uiso 1 1 calc R . .
C5 C 0.2933(3) 0.5266(2) 0.07664(4) 0.0235(5) Uani 1 1 d . . .
H5A H 0.2050 0.4628 0.0828 0.028 Uiso 1 1 calc R . .
H5B H 0.3558 0.5004 0.0828 0.028 Uiso 1 1 calc R . .
C6 C 0.3333 0.6667 0.08621(7) 0.0236(8) Uani 1 3 d S . .
H6 H 0.3333 0.6667 0.1047 0.028 Uiso 1 3 calc SR . .
N4 N -0.1481(7) 0.3036(7) 0.07557(16) 0.0742(17) Uani 0.3333 1 d PDU . 1
O1 O -0.0513(8) 0.3455(12) 0.08899(17) 0.078(2) Uani 0.3333 1 d PDU . 1
O2 O -0.1305(9) 0.3475(9) 0.05370(15) 0.077(2) Uani 0.3333 1 d PDU . 1
O3 O -0.2600(7) 0.2218(8) 0.08216(16) 0.0706(18) Uani 0.3333 1 d PDU . 1
O1W O -0.1336(5) 0.3317(5) 0.02889(12) 0.0687(14) Uani 0.50 1 d PU A 2
O2W O -0.2791(8) 0.3329(11) 0.02556(17) 0.077(2) Uani 0.3333 1 d PU . 2
O3W O -0.0939(12) 0.3398(14) 0.0636(3) 0.038(3) Uani 0.1667 1 d P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.01543(17) 0.01543(17) 0.0192(2) 0.000 0.000 0.00772(8)
N1 0.0211(10) 0.0229(11) 0.0271(10) -0.0026(8) -0.0018(8) 0.0114(9)
N2 0.0256(11) 0.0267(11) 0.0410(13) -0.0056(10) -0.0059(10) 0.0155(9)
N3 0.0198(10) 0.0186(10) 0.0223(10) -0.0008(8) -0.0017(8) 0.0095(8)
C1 0.0217(12) 0.0243(12) 0.0287(12) -0.0055(10) -0.0041(10) 0.0122(10)
C2 0.0249(13) 0.0250(13) 0.0474(15) -0.0090(12) -0.0093(12) 0.0131(11)
C3 0.0203(11) 0.0166(11) 0.0214(11) -0.0008(9) 0.0007(9) 0.0089(9)
C4 0.0203(11) 0.0199(11) 0.0237(11) -0.0004(9) -0.0005(9) 0.0110(10)
C5 0.0252(12) 0.0252(13) 0.0203(11) 0.0039(10) 0.0006(9) 0.0127(10)
C6 0.0275(13) 0.0275(13) 0.0157(17) 0.000 0.000 0.0138(7)
N4 0.058(3) 0.061(3) 0.094(5) 0.006(3) 0.009(3) 0.023(3)
O1 0.059(3) 0.068(3) 0.094(5) 0.004(3) 0.007(3) 0.022(3)
O2 0.061(3) 0.061(3) 0.096(5) 0.008(3) 0.010(3) 0.020(3)
O3 0.059(3) 0.056(3) 0.089(5) 0.009(3) 0.011(3) 0.024(3)
O1W 0.060(3) 0.036(2) 0.099(4) -0.003(2) 0.002(3) 0.016(2)
O2W 0.067(4) 0.049(3) 0.089(4) -0.002(4) 0.005(3) 0.011(4)
O3W 0.023(6) 0.049(8) 0.043(8) 0.014(6) -0.014(5) 0.018(6)

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

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
Cd1 N1 2.347(2) 19 ?
Cd1 N1 2.347(2) 2 ?
Cd1 N1 2.347(2) . ?
Cd1 N1 2.347(2) 20 ?
Cd1 N1 2.347(2) 21 ?
Cd1 N1 2.347(2) 3 ?
N1 C1 1.302(3) . ?
N1 N2 1.376(3) . ?
N2 C2 1.300(3) . ?
N3 C1 1.348(3) . ?
N3 C2 1.357(3) . ?
N3 C3 1.484(3) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.530(3) 3_565 ?
C3 C4 1.534(3) . ?
C3 C5 1.535(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.531(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C5 1.531(3) 3_565 ?
C6 C5 1.531(3) 2_665 ?
C6 H6 0.9800 . ?
N4 O1 1.205(6) . ?
N4 O3 1.211(6) . ?
N4 O2 1.241(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 86.27(7) 19 2 ?
N1 Cd1 N1 180.00(12) 19 . ?
N1 Cd1 N1 93.73(7) 2 . ?
N1 Cd1 N1 93.73(7) 19 20 ?
N1 Cd1 N1 180.00(8) 2 20 ?
N1 Cd1 N1 86.27(7) . 20 ?
N1 Cd1 N1 93.73(7) 19 21 ?
N1 Cd1 N1 86.27(7) 2 21 ?
N1 Cd1 N1 86.27(7) . 21 ?
N1 Cd1 N1 93.73(7) 20 21 ?
N1 Cd1 N1 86.27(7) 19 3 ?
N1 Cd1 N1 93.73(7) 2 3 ?
N1 Cd1 N1 93.73(7) . 3 ?
N1 Cd1 N1 86.27(7) 20 3 ?
N1 Cd1 N1 180.00(11) 21 3 ?
C1 N1 N2 107.8(2) . . ?
C1 N1 Cd1 130.71(17) . . ?
N2 N1 Cd1 120.23(14) . . ?
C2 N2 N1 106.0(2) . . ?
C1 N3 C2 104.1(2) . . ?
C1 N3 C3 129.1(2) . . ?
C2 N3 C3 126.72(19) . . ?
N1 C1 N3 110.6(2) . . ?
N1 C1 H1 124.7 . . ?
N3 C1 H1 124.7 . . ?
N2 C2 N3 111.5(2) . . ?
N2 C2 H2 124.2 . . ?
N3 C2 H2 124.2 . . ?
N3 C3 C4 109.37(18) . 3_565 ?
N3 C3 C4 108.48(19) . . ?
C4 C3 C4 109.7(2) 3_565 . ?
N3 C3 C5 109.14(18) . . ?
C4 C3 C5 110.08(19) 3_565 . ?
C4 C3 C5 110.09(19) . . ?
C3 C4 C3 108.4(2) 2_665 . ?
C3 C4 H4A 110.0 2_665 . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 2_665 . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 C3 109.0(2) . . ?
C6 C5 H5A 109.9 . . ?
C3 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
C3 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C5 C6 C5 109.59(17) 3_565 2_665 ?
C5 C6 C5 109.59(17) 3_565 . ?
C5 C6 C5 109.59(16) 2_665 . ?
C5 C6 H6 109.4 3_565 . ?
C5 C6 H6 109.4 2_665 . ?
C5 C6 H6 109.4 . . ?
O1 N4 O3 123.9(7) . . ?
O1 N4 O2 117.2(7) . . ?
O3 N4 O2 118.8(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cd1 N1 C1 -55.7(3) 2 . . . ?
N1 Cd1 N1 C1 124.3(3) 20 . . . ?
N1 Cd1 N1 C1 30.3(2) 21 . . . ?
N1 Cd1 N1 C1 -149.7(2) 3 . . . ?
N1 Cd1 N1 N2 138.89(15) 2 . . . ?
N1 Cd1 N1 N2 -41.11(15) 20 . . . ?
N1 Cd1 N1 N2 -135.1(2) 21 . . . ?
N1 Cd1 N1 N2 44.9(2) 3 . . . ?
C1 N1 N2 C2 0.1(3) . . . . ?
Cd1 N1 N2 C2 168.50(18) . . . . ?
N2 N1 C1 N3 0.8(3) . . . . ?
Cd1 N1 C1 N3 -165.94(15) . . . . ?
C2 N3 C1 N1 -1.3(3) . . . . ?
C3 N3 C1 N1 -177.2(2) . . . . ?
N1 N2 C2 N3 -1.0(3) . . . . ?
C1 N3 C2 N2 1.4(3) . . . . ?
C3 N3 C2 N2 177.4(2) . . . . ?
C1 N3 C3 C4 -18.1(3) . . . 3_565 ?
C2 N3 C3 C4 166.9(2) . . . 3_565 ?
C1 N3 C3 C4 -137.7(2) . . . . ?
C2 N3 C3 C4 47.3(3) . . . . ?
C1 N3 C3 C5 102.4(3) . . . . ?
C2 N3 C3 C5 -72.6(3) . . . . ?
N3 C3 C4 C3 -179.50(15) . . . 2_665 ?
C4 C3 C4 C3 61.1(3) 3_565 . . 2_665 ?
C5 C3 C4 C3 -60.1(2) . . . 2_665 ?
N3 C3 C5 C6 179.34(15) . . . . ?
C4 C3 C5 C6 -60.6(2) 3_565 . . . ?
C4 C3 C5 C6 60.4(2) . . . . ?
C3 C5 C6 C5 60.2(2) . . . 3_565 ?
C3 C5 C6 C5 -60.1(2) . . . 2_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.41
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.075

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk2010_01 in R-3c
CELL 0.71073 11.5603 11.5603 53.0233 90.000 90.000 120.000
ZERR 6.00 0.0002 0.0002 0.0019 0.000 0.000 0.000
LATT 3
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SYMM Y, X, 1/2 - Z
SYMM X - Y, - Y, 1/2 - Z
SYMM - X, - X + Y, 1/2 - Z
SFAC C H N O CD
UNIT 192 300 120 72 6
MERG 2
OMIT 0.00 180.00
OMIT -1 1 4
OMIT 0 0 48
OMIT -4 7 1
OMIT -4 5 15
DFIX 1.222 0.007 N4 O1 N4 O2 N4 O3
DFIX 2.105 0.007 O1 O2 O1 O3 O2 O3
FLAT 0.008 N4 O1 O2 O3
SIMU 0.002 N4 > O3
SIMU 0.002 O1W > O3W
FMAP 2
PLAN 7
SIZE 0.07 0.13 0.22
ACTA
BOND
BOND $H
CONF
L.S. 6
TEMP 23.00
WGHT 0.046200 12.167001
FVAR 0.13017
CD1 5 0.000000 0.000000 0.000000 10.16667 0.01543 0.01543 =
0.01925 0.00000 0.00000 0.00772
N1 3 0.143960 0.189140 0.023835 11.00000 0.02111 0.02292 =
0.02710 -0.00264 -0.00179 0.01144
N2 3 0.269296 0.212737 0.030246 11.00000 0.02556 0.02675 =
0.04099 -0.00558 -0.00593 0.01549
N3 3 0.256427 0.392336 0.038350 11.00000 0.01983 0.01860 =
0.02229 -0.00078 -0.00170 0.00948
C1 1 0.138711 0.296556 0.029003 11.00000 0.02169 0.02432 =
0.02869 -0.00547 -0.00405 0.01217
AFIX 43
H1 2 0.064106 0.305880 0.026581 11.00000 -1.20000
AFIX 0
C2 1 0.333107 0.333933 0.039028 11.00000 0.02487 0.02500 =
0.04735 -0.00900 -0.00932 0.01312
AFIX 43
H2 2 0.420370 0.375403 0.045022 11.00000 -1.20000
AFIX 0
C3 1 0.293661 0.527581 0.047685 11.00000 0.02035 0.01661 =
0.02141 -0.00077 0.00074 0.00886
C4 1 0.433728 0.626929 0.037846 11.00000 0.02027 0.01991 =
0.02372 -0.00044 -0.00046 0.01101
AFIX 23
H4A 2 0.497478 0.601560 0.043678 11.00000 -1.20000
H4B 2 0.434018 0.626885 0.019552 11.00000 -1.20000
AFIX 0
C5 1 0.293303 0.526643 0.076643 11.00000 0.02524 0.02525 =
0.02027 0.00386 0.00056 0.01273
AFIX 23
H5A 2 0.204953 0.462762 0.082802 11.00000 -1.20000
H5B 2 0.355837 0.500424 0.082821 11.00000 -1.20000
AFIX 0
C6 1 0.333333 0.666667 0.086209 10.33333 0.02753 0.02753 =
0.01567 0.00000 0.00000 0.01376
AFIX 13
H6 2 0.333333 0.666667 0.104691 10.33333 -1.20000
AFIX 0
PART 1
N4 3 -0.148127 0.303629 0.075569 10.33333 0.05837 0.06126 =
0.09351 0.00647 0.00934 0.02290
O1 4 -0.051255 0.345484 0.088991 10.33333 0.05949 0.06758 =
0.09421 0.00366 0.00703 0.02200
O2 4 -0.130492 0.347534 0.053697 10.33333 0.06087 0.06087 =
0.09617 0.00817 0.01005 0.02040
O3 4 -0.260050 0.221820 0.082159 10.33333 0.05936 0.05648 =
0.08907 0.00860 0.01142 0.02374
PART 2
O1W 4 -0.133641 0.331663 0.028892 10.50000 0.05975 0.03641 =
0.09912 -0.00265 0.00203 0.01588
O2W 4 -0.279146 0.332945 0.025562 10.33333 0.06748 0.04912 =
0.08888 -0.00204 0.00536 0.01103
O3W 4 -0.093942 0.339840 0.063641 10.16667 0.02260 0.04879 =
0.04336 0.01406 -0.01420 0.01757
HKLF 4

REM dk2010_01 in R-3c
REM R1 = 0.0304 for 1190 Fo > 4sig(Fo) and 0.0390 for all 1408 data
REM 141 parameters refined using 31 restraints

END

WGHT 0.0462 12.1553
REM Highest difference peak 0.657, deepest hole -0.313, 1-sigma level 0.075
Q1 1 -0.0324 0.3953 0.0805 11.00000 0.05 0.56
Q2 1 0.4597 0.6986 0.0416 11.00000 0.05 0.36
Q3 1 -0.0784 -0.0354 0.0104 11.00000 0.05 0.36
Q4 1 -0.1998 0.3601 0.0277 11.00000 0.05 0.35
Q5 1 0.3627 0.5808 0.0408 11.00000 0.05 0.34
Q6 1 0.3144 0.6001 0.0792 11.00000 0.05 0.32
Q7 1 -0.2230 0.3389 0.0469 11.00000 0.05 0.31

;

#---------------------------------------------------------

data_(5)
_database_code_depnum_ccdc_archive 'CCDC 867228'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[1,3,5-tri(1,2,4-triazol-4-yl)adamantane]cadmium(II)
Tetrachlorocadmate(II) Trihydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C32 H38 Cd N18), (Cd Cl4), 3(H2 O)'
_chemical_formula_sum            'C32 H44 Cd2 Cl4 N18 O3'
_chemical_formula_weight         1095.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.3552(11)
_cell_length_b                   11.3552(11)
_cell_length_c                   54.979(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6139.3(9)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8109
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.45

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3300
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7540
_exptl_absorpt_correction_T_max  0.8430
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8109
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         26.45
_reflns_number_total             1419
_reflns_number_gt                944
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Refinement of Cd-organic framework atoms was standard. The CH-hydrogen
atoms were constrained with U(iso) = 1.2U(eq) of the parent C-atom and
with C-H distances 0.95 A (triazole), 0.99 A (CH2 adamantane) and 1.00 A
(CH adamantane). The OH-hydrogen atoms were located and then fixed
with U(iso) = 1.5U(eq) of the parent O-atom.

There is disorder in the region of guest anion/water, which is similar
to that in the structure of (7). The CdCl4^2-^ anion is equally
disordered by symmetry (the same was observed for the refinement in the
acentric space group R3c) in such a way that three Cl-atoms are ordered
and are common for two orientations, while Cd-Cl fragment is equally
disordered from two axial sides of the Cl-Cl-Cl triangle. Positions of
this disordered fragment are overlapped with the solvate water
molecule (O1), which thus was also refined with a partial occupancy
factor 0.50. The disorder was trated without any restraints in geometry
and thermal parameters and all corresponding atoms were refined
anisotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+9.8369P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1419
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.0243(2) Uani 1 6 d S . .
Cl1 Cl 0.4616(2) 0.1282(2) 0.0833 0.0928(8) Uani 1 2 d S . .
Cd2 Cd 0.6667 0.3333 0.09540(2) 0.0546(4) Uani 0.50 3 d SP . .
Cl2 Cl 0.6667 0.3333 0.13987(13) 0.152(4) Uani 0.50 3 d SP . .
N1 N 0.1478(3) 0.1873(3) 0.02365(6) 0.0349(9) Uani 1 1 d . . .
N2 N 0.2717(4) 0.2091(4) 0.03056(8) 0.0456(10) Uani 1 1 d . . .
N3 N 0.2574(3) 0.3890(3) 0.03978(6) 0.0291(8) Uani 1 1 d . . .
C1 C 0.1405(4) 0.2947(4) 0.02933(8) 0.0366(10) Uani 1 1 d . . .
H1 H 0.0637 0.3052 0.0265 0.044 Uiso 1 1 calc R . .
C2 C 0.3336(4) 0.3290(5) 0.04013(10) 0.0475(12) Uani 1 1 d . . .
H2 H 0.4229 0.3701 0.0467 0.057 Uiso 1 1 calc R . .
C3 C 0.2946(4) 0.5254(4) 0.04890(7) 0.0273(9) Uani 1 1 d . . .
C4 C 0.4364(4) 0.6278(4) 0.03964(7) 0.0282(9) Uani 1 1 d . . .
H4A H 0.5033 0.6026 0.0455 0.034 Uiso 1 1 calc R . .
H4B H 0.4374 0.6275 0.0216 0.034 Uiso 1 1 calc R . .
C5 C 0.2931(4) 0.5244(4) 0.07685(7) 0.0332(10) Uani 1 1 d . . .
H5A H 0.2010 0.4581 0.0828 0.040 Uiso 1 1 calc R . .
H5B H 0.3578 0.4973 0.0831 0.040 Uiso 1 1 calc R . .
C6 C 0.3333 0.6667 0.08590(12) 0.0306(15) Uani 1 3 d S . .
H6 H 0.3333 0.6667 0.1041 0.037 Uiso 1 3 calc SR . .
O1 O 0.4853(15) 0.1492(15) 0.0189(2) 0.163(6) Uani 0.50 1 d P . .
H1W H 0.4223 0.1701 0.0184 0.245 Uiso 0.50 1 d P . .
H2W H 0.4973 0.1403 0.0343 0.245 Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0218(3) 0.0218(3) 0.0292(4) 0.000 0.000 0.01089(14)
Cl1 0.0647(11) 0.0647(11) 0.135(2) -0.0016(8) 0.0016(8) 0.0217(12)
Cd2 0.0543(5) 0.0543(5) 0.0552(8) 0.000 0.000 0.0272(3)
Cl2 0.202(6) 0.202(6) 0.050(4) 0.000 0.000 0.101(3)
N1 0.031(2) 0.031(2) 0.043(2) -0.0112(17) -0.0099(17) 0.0164(17)
N2 0.041(2) 0.033(2) 0.068(3) -0.011(2) -0.010(2) 0.0227(19)
N3 0.0264(19) 0.0248(19) 0.0351(19) -0.0033(15) -0.0048(16) 0.0119(16)
C1 0.029(2) 0.030(2) 0.052(3) -0.013(2) -0.009(2) 0.015(2)
C2 0.033(3) 0.036(3) 0.078(3) -0.009(3) -0.011(3) 0.021(2)
C3 0.028(2) 0.022(2) 0.032(2) -0.0020(17) -0.0020(17) 0.0124(17)
C4 0.030(2) 0.026(2) 0.030(2) -0.0018(17) -0.0012(17) 0.0157(19)
C5 0.034(2) 0.030(2) 0.033(2) 0.0054(19) 0.0008(19) 0.0147(19)
C6 0.035(2) 0.035(2) 0.022(3) 0.000 0.000 0.0175(12)
O1 0.210(13) 0.244(15) 0.151(11) 0.083(10) 0.072(10) 0.201(13)

_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.
;

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
Cd1 N1 2.337(3) . ?
Cd1 N1 2.337(3) 3 ?
Cd1 N1 2.337(3) 2 ?
Cd1 N1 2.337(3) 19 ?
Cd1 N1 2.337(3) 21 ?
Cd1 N1 2.337(3) 20 ?
Cd2 Cl1 2.422(2) 2_655 ?
Cd2 Cl1 2.422(2) 3_665 ?
Cd2 Cl2 2.444(7) . ?
N1 C1 1.302(5) . ?
N1 N2 1.355(5) . ?
N2 C2 1.292(6) . ?
N3 C2 1.342(5) . ?
N3 C1 1.348(5) . ?
N3 C3 1.475(5) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C4 1.526(5) 3_565 ?
C3 C4 1.527(5) . ?
C3 C5 1.536(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.525(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C5 1.525(5) 3_565 ?
C6 C5 1.525(5) 2_665 ?
C6 H6 1.0000 . ?
O1 H1W 0.8594 . ?
O1 H2W 0.8684 . ?

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 Cd1 N1 92.04(12) . 3 ?
N1 Cd1 N1 92.04(12) . 2 ?
N1 Cd1 N1 92.04(12) 3 2 ?
N1 Cd1 N1 180.0(2) . 19 ?
N1 Cd1 N1 87.96(12) 3 19 ?
N1 Cd1 N1 87.96(12) 2 19 ?
N1 Cd1 N1 87.96(12) . 21 ?
N1 Cd1 N1 180.00(14) 3 21 ?
N1 Cd1 N1 87.96(12) 2 21 ?
N1 Cd1 N1 92.04(12) 19 21 ?
N1 Cd1 N1 87.96(12) . 20 ?
N1 Cd1 N1 87.96(12) 3 20 ?
N1 Cd1 N1 180.00(14) 2 20 ?
N1 Cd1 N1 92.04(12) 19 20 ?
N1 Cd1 N1 92.04(12) 21 20 ?
Cl1 Cd2 Cl1 112.79(3) 2_655 . ?
Cl1 Cd2 Cl1 112.79(3) 2_655 3_665 ?
Cl1 Cd2 Cl1 112.79(3) . 3_665 ?
Cl1 Cd2 Cl2 105.91(3) 2_655 . ?
Cl1 Cd2 Cl2 105.91(3) . . ?
Cl1 Cd2 Cl2 105.91(3) 3_665 . ?
C1 N1 N2 107.9(3) . . ?
C1 N1 Cd1 129.3(3) . . ?
N2 N1 Cd1 122.0(3) . . ?
C2 N2 N1 106.0(4) . . ?
C2 N3 C1 103.4(3) . . ?
C2 N3 C3 127.5(3) . . ?
C1 N3 C3 129.1(3) . . ?
N1 C1 N3 110.3(4) . . ?
N1 C1 H1 124.8 . . ?
N3 C1 H1 124.8 . . ?
N2 C2 N3 112.3(4) . . ?
N2 C2 H2 123.8 . . ?
N3 C2 H2 123.8 . . ?
N3 C3 C4 109.1(3) . 3_565 ?
N3 C3 C4 109.0(3) . . ?
C4 C3 C4 109.9(4) 3_565 . ?
N3 C3 C5 109.7(3) . . ?
C4 C3 C5 109.2(3) 3_565 . ?
C4 C3 C5 110.0(3) . . ?
C3 C4 C3 109.1(4) 2_665 . ?
C3 C4 H4A 109.9 2_665 . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 2_665 . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
C6 C5 C3 108.8(4) . . ?
C6 C5 H5A 109.9 . . ?
C3 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
C3 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C5 C6 C5 109.9(3) 3_565 2_665 ?
C5 C6 C5 109.9(3) 3_565 . ?
C5 C6 C5 109.9(3) 2_665 . ?
C5 C6 H6 109.1 3_565 . ?
C5 C6 H6 109.1 2_665 . ?
C5 C6 H6 109.1 . . ?
Cl2 O1 H1W 105.5 16_544 . ?
Cl2 O1 H2W 77.6 16_544 . ?
H1W O1 H2W 105.3 . . ?

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
N1 Cd1 N1 C1 -146.1(4) 3 . . . ?
N1 Cd1 N1 C1 -54.0(5) 2 . . . ?
N1 Cd1 N1 C1 33.9(4) 21 . . . ?
N1 Cd1 N1 C1 126.0(5) 20 . . . ?
N1 Cd1 N1 N2 45.2(4) 3 . . . ?
N1 Cd1 N1 N2 137.3(3) 2 . . . ?
N1 Cd1 N1 N2 -134.8(4) 21 . . . ?
N1 Cd1 N1 N2 -42.7(3) 20 . . . ?
C1 N1 N2 C2 0.1(5) . . . . ?
Cd1 N1 N2 C2 170.9(3) . . . . ?
N2 N1 C1 N3 0.4(5) . . . . ?
Cd1 N1 C1 N3 -169.5(3) . . . . ?
C2 N3 C1 N1 -0.7(5) . . . . ?
C3 N3 C1 N1 179.7(4) . . . . ?
N1 N2 C2 N3 -0.5(6) . . . . ?
C1 N3 C2 N2 0.8(5) . . . . ?
C3 N3 C2 N2 -179.6(4) . . . . ?
C2 N3 C3 C4 167.2(4) . . . 3_565 ?
C1 N3 C3 C4 -13.2(5) . . . 3_565 ?
C2 N3 C3 C4 47.3(5) . . . . ?
C1 N3 C3 C4 -133.2(4) . . . . ?
C2 N3 C3 C5 -73.2(5) . . . . ?
C1 N3 C3 C5 106.3(5) . . . . ?
N3 C3 C4 C3 179.6(3) . . . 2_665 ?
C4 C3 C4 C3 60.0(5) 3_565 . . 2_665 ?
C5 C3 C4 C3 -60.2(4) . . . 2_665 ?
N3 C3 C5 C6 179.4(3) . . . . ?
C4 C3 C5 C6 -61.1(4) 3_565 . . . ?
C4 C3 C5 C6 59.5(4) . . . . ?
C3 C5 C6 C5 61.1(4) . . . 3_565 ?
C3 C5 C6 C5 -60.0(4) . . . 2_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.101

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL r-3c in R-3c
CELL 0.71073 11.3552 11.3552 54.9788 90.000 90.000 120.000
ZERR 6.00 0.0011 0.0011 0.0034 0.000 0.000 0.000
LATT 3
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SYMM Y, X, 1/2 - Z
SYMM X - Y, - Y, 1/2 - Z
SYMM - X, - X + Y, 1/2 - Z
SFAC C H N O CL CD
UNIT 192 264 108 18 24 12
MERG 2
OMIT 0.00 180.00
OMIT 0 0 6
OMIT -1 2 6
OMIT -1 5 6
FMAP 2
PLAN 20
SIZE 0.13 0.15 0.22
ACTA
BOND
BOND $H
CONF
L.S. 6
TEMP -100.00
WGHT 0.060900 9.836900
FVAR 0.12534
CD1 6 0.000000 0.000000 0.000000 10.16667 0.02179 0.02179 =
0.02919 0.00000 0.00000 0.01089
CL1 5 0.461560 0.128227 0.083333 10.50000 0.06465 0.06465 =
0.13493 -0.00158 0.00158 0.02169
CD2 6 0.666667 0.333333 0.095405 10.16667 0.05434 0.05434 =
0.05520 0.00000 0.00000 0.02717
CL2 5 0.666667 0.333333 0.139866 10.16667 0.20233 0.20233 =
0.05014 0.00000 0.00000 0.10117
N1 3 0.147830 0.187260 0.023652 11.00000 0.03090 0.03149 =
0.04321 -0.01118 -0.00990 0.01637
N2 3 0.271697 0.209123 0.030555 11.00000 0.04100 0.03334 =
0.06791 -0.01078 -0.00962 0.02266
N3 3 0.257397 0.388994 0.039777 11.00000 0.02636 0.02479 =
0.03509 -0.00331 -0.00478 0.01189
C1 1 0.140514 0.294749 0.029329 11.00000 0.02867 0.03040 =
0.05153 -0.01345 -0.00890 0.01535
AFIX 43
H1 2 0.063724 0.305245 0.026508 11.00000 -1.20000
AFIX 0
C2 1 0.333562 0.329031 0.040133 11.00000 0.03287 0.03642 =
0.07759 -0.00896 -0.01114 0.02055
AFIX 43
H2 2 0.422855 0.370119 0.046686 11.00000 -1.20000
AFIX 0
C3 1 0.294587 0.525392 0.048903 11.00000 0.02762 0.02227 =
0.03187 -0.00204 -0.00203 0.01243
C4 1 0.436436 0.627797 0.039641 11.00000 0.03009 0.02620 =
0.03037 -0.00178 -0.00119 0.01570
AFIX 23
H4A 2 0.503267 0.602562 0.045524 11.00000 -1.20000
H4B 2 0.437408 0.627451 0.021636 11.00000 -1.20000
AFIX 0
C5 1 0.293076 0.524433 0.076847 11.00000 0.03438 0.03007 =
0.03324 0.00542 0.00080 0.01470
AFIX 23
H5A 2 0.201042 0.458103 0.082818 11.00000 -1.20000
H5B 2 0.357849 0.497283 0.083077 11.00000 -1.20000
AFIX 0
C6 1 0.333333 0.666667 0.085904 10.33333 0.03494 0.03494 =
0.02178 0.00000 0.00000 0.01747
AFIX 13
H6 2 0.333333 0.666667 0.104092 10.33333 -1.20000
AFIX 0
O1 4 0.485337 0.149208 0.018942 10.50000 0.21036 0.24424 =
0.15112 0.08280 0.07157 0.20070
AFIX 1
H1W 2 0.422340 0.170100 0.018420 10.50000 -1.50000
H2W 2 0.497270 0.140350 0.034290 10.50000 -1.50000
HKLF 4

REM r-3c in R-3c
REM R1 = 0.0440 for 944 Fo > 4sig(Fo) and 0.0773 for all 1419 data
REM 98 parameters refined using 0 restraints

END

WGHT 0.0599 10.3867
REM Highest difference peak 0.499, deepest hole -0.970, 1-sigma level 0.101
Q1 1 0.5804 0.2415 0.1394 11.00000 0.05 0.50
Q2 1 0.6667 0.2401 0.0833 10.50000 0.05 0.41
Q3 1 0.4404 0.3333 0.0833 10.50000 0.05 0.37
Q4 1 0.5042 0.1675 0.0669 11.00000 0.05 0.36
Q5 1 0.4551 0.0752 0.0114 11.00000 0.05 0.36
Q6 1 0.2742 0.4559 0.0443 11.00000 0.05 0.35
Q7 1 0.6870 0.3132 0.1170 11.00000 0.05 0.34
Q8 1 0.5837 0.2504 0.0833 10.50000 0.05 0.34
Q9 1 0.3001 0.6967 0.0827 11.00000 0.05 0.32
Q10 1 0.3689 0.5736 0.0445 11.00000 0.05 0.32

;

#---------------------------------------------------------

data_(6)
_database_code_depnum_ccdc_archive 'CCDC 867229'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris-[1,3,5-tri(1,2,4-triazol-4-yl)-adamantane]-
di(mu3-hydroxido)-pentasulfato triaqua hexacopper(II)
Hexacosahydrate
;
_chemical_name_common            
;
tris-(1,3,5-tri(1,2,4-triazol-4-yl)-adamantane)-di(mu3-
hydroxido)-pentasulfato triaqua hexacopper(ii) Hexacosahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H65 Cu6 N27 O25 S5, 26(H2 O)'
_chemical_formula_sum            'C48 H117 Cu6 N27 O51 S5'
_chemical_formula_weight         2430.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

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

loop_
_symmetry_equiv_pos_as_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                   38.1357(13)
_cell_length_b                   22.2267(4)
_cell_length_c                   27.8475(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.357(6)
_cell_angle_gamma                90.00
_cell_volume                     20573.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    59257
_cell_measurement_theta_min      5.10
_cell_measurement_theta_max      27.10

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10048
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_T_max  0.7740
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            59257
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_sigmaI/netI    0.2303
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         27.10
_reflns_number_total             22268
_reflns_number_gt                10206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The refinement was somewhat complicated by the problems arising from the
disorder of part of the solvate water molecules, SO4^2-^ anions and
triazole rings:

1) In the anionic cluster, [Cu3(mu3-OH)(mu3-SO4)(mu2-tr)3(SO4)3(H2O)]3-,
at least two out of three present monodentate equatorial sulfate ligands
show "rotational" disorder of three non-coordinated O-atoms. This disorder
was resolved with restrained tetrahedral geometry of the SO4^2-^ groups
[S-O 1.480(5) A] and with equal anisotropic thermal parameters for the
disordered O-atoms (EADP). Partial occupancies of the disorder components
were refined as additional free variable parameters giving almost equal
contributions at 0.57/0.43 and 0.54/0.46.
Relatively high parameters for the thermal motion of O-atoms
corresponding to the third monodentate sulfate, and also for mu3-SO4-cap
of the cationic cluster were also indicative of the disorder. However,
it was not possible to resolve it. The corresponding atoms were refined
anisotropically for the sake of overall convergence.

2) Very high anisotropy for the thermal motion of one of the singly
coordinated triazole groups (N27-C37-N25-N26-C38; N26 is coordinated to
Cu) suggests the disorder as "rotation" around N27...N26 axis. The
disorder was resolved with equal 0.50 partial contributions for C37, N25
and C38 atoms, restraints in the triazole bond lengths, FLAT 0.01
restraints for the coplanarity of the ring atoms and EADP constraints
for the anisotropic thermal values for atoms of two components:
N25, C37, C38 and N25A, C37A, C38A.

3) It was possible to locate 3 coordinated water molecules (long axial
Cu-O bonds at 2.29-2.57 A) and 16 solvate water molecules, one of which
is 0.65/0.35 disordered over two closely separated positions. The
coordinated water molecules and 7 solvate water molecules were refined
anisotropically, while other 9 solvate water were left isotropic in
view of the relatively large thermal parameters [U(iso) = 0.137-0.174
A^2^], for two components of the disordered water molecule U(iso) =
0.102 and 0.111 A^2^].

4) The remaining solvate water molecules are badly disordered and
it was impossible to found a stable refinement model. This electron
density was modelled using SQUEEZE routine, as it implemented in
PLATON: 850 e / unit cell are found, which were attributed to 80
additional water molecules, 10 per the formula unit. This gives
total density of 1.569 g cm^-3^.

5) With the exception of 9 isotropic solvate water molecules,
all non-hydrogen atoms were refined anisotropically. The CH-hydrogen
atoms were constrained with U(iso) = 1.2U(eq) of the parent C-atom and
with C-H distances 0.95 A (triazole), 0.99 A (CH2 adamantane) and
1.00 A (CH adamantane). The OH-hydrogen atoms were located for mu3-OH
groups and for two coordinated water molecules. These H-atoms were
then constrained with O-H distances set to 0.85 A (H2O) and 1.00 A
(mu3-OH) and U(iso) = 1.5U(eq) of the parent O-atom. For the remaining
water molecules, the H-atoms were not added considering the disorder
in the solvent region.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         22268
_refine_ls_number_parameters     1102
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1571
_refine_ls_wR_factor_gt          0.1457
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_restrained_S_all      0.798
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74607(2) 0.20116(3) 0.36313(4) 0.0217(2) Uani 1 1 d . . .
Cu2 Cu 0.67021(2) 0.21309(3) 0.39149(4) 0.0212(2) Uani 1 1 d . . .
Cu3 Cu 0.70833(2) 0.33731(3) 0.36519(4) 0.0216(2) Uani 1 1 d . . .
Cu4 Cu 0.42947(2) 0.21326(3) 0.41962(4) 0.0264(2) Uani 1 1 d . . .
Cu5 Cu 0.37952(2) 0.33762(3) 0.40105(4) 0.0212(2) Uani 1 1 d . . .
Cu6 Cu 0.33824(2) 0.20160(3) 0.39605(4) 0.0192(2) Uani 1 1 d . . .
S1 S 0.65338(5) 0.23770(7) 0.26548(8) 0.0204(4) Uani 1 1 d . . .
S2 S 0.81199(8) 0.11993(11) 0.36094(15) 0.0768(10) Uani 1 1 d D . .
S3 S 0.62774(7) 0.16239(9) 0.45380(11) 0.0445(6) Uani 1 1 d . . .
S4 S 0.71353(8) 0.47842(10) 0.35954(15) 0.0744(10) Uani 1 1 d D . .
S5 S 0.42698(6) 0.24710(8) 0.52987(10) 0.0323(5) Uani 1 1 d . . .
O1 O 0.71784(11) 0.25268(16) 0.39306(19) 0.0149(10) Uani 1 1 d . . .
H1W H 0.7377 0.2566 0.4332 0.022 Uiso 1 1 calc R . .
O2 O 0.37605(10) 0.25126(16) 0.38338(19) 0.0134(10) Uani 1 1 d . . .
H2W H 0.3664 0.2490 0.3429 0.020 Uiso 1 1 calc R . .
O3 O 0.69159(12) 0.20769(18) 0.2770(2) 0.0273(12) Uani 1 1 d . . .
O4 O 0.63863(12) 0.21005(19) 0.3007(2) 0.0292(13) Uani 1 1 d . . .
O5 O 0.66242(12) 0.30191(17) 0.2792(2) 0.0276(13) Uani 1 1 d . . .
O6 O 0.62294(12) 0.2307(2) 0.2073(2) 0.0287(12) Uani 1 1 d . . .
O7 O 0.77396(15) 0.1528(2) 0.3344(3) 0.0495(18) Uani 1 1 d . A .
O8 O 0.8091(4) 0.0594(3) 0.3812(5) 0.088(2) Uani 0.532(6) 1 d PD A 1
O9 O 0.8485(2) 0.1476(4) 0.4061(4) 0.088(2) Uani 0.532(6) 1 d PD A 1
O10 O 0.8229(3) 0.1076(5) 0.3172(3) 0.088(2) Uani 0.532(6) 1 d PD A 1
O8A O 0.8256(4) 0.1278(6) 0.4194(3) 0.088(2) Uani 0.468(6) 1 d PD A 2
O9A O 0.8418(3) 0.1441(5) 0.3487(6) 0.088(2) Uani 0.468(6) 1 d PD A 2
O10A O 0.8052(4) 0.0567(3) 0.3475(6) 0.088(2) Uani 0.468(6) 1 d PD A 2
O11 O 0.62860(12) 0.17294(18) 0.4013(2) 0.0258(12) Uani 1 1 d . . .
O12 O 0.6671(2) 0.1742(5) 0.4997(4) 0.145(4) Uani 1 1 d . . .
O13 O 0.6152(2) 0.1012(3) 0.4538(3) 0.083(2) Uani 1 1 d . . .
O14 O 0.59880(19) 0.2042(3) 0.4558(3) 0.067(2) Uani 1 1 d . . .
O15 O 0.69923(16) 0.42034(19) 0.3377(3) 0.0552(19) Uani 1 1 d . B .
O16 O 0.7017(3) 0.4981(4) 0.4006(3) 0.088(2) Uani 0.565(5) 1 d PD B 3
O17 O 0.6981(3) 0.5246(4) 0.3164(3) 0.088(2) Uani 0.565(5) 1 d PD B 3
O18 O 0.75781(14) 0.4827(4) 0.3885(4) 0.088(2) Uani 0.565(5) 1 d PD B 3
O16A O 0.6819(3) 0.5210(4) 0.3509(6) 0.088(2) Uani 0.435(5) 1 d PD B 4
O17A O 0.7429(3) 0.5073(5) 0.3486(6) 0.088(2) Uani 0.435(5) 1 d PD B 4
O18A O 0.7336(3) 0.4603(5) 0.4175(3) 0.088(2) Uani 0.435(5) 1 d PD B 4
O19 O 0.41551(19) 0.1973(2) 0.4873(3) 0.069(2) Uani 1 1 d . . .
O20 O 0.4219(3) 0.3016(3) 0.5037(4) 0.132(4) Uani 1 1 d . . .
O21 O 0.46728(19) 0.2366(4) 0.5753(4) 0.105(3) Uani 1 1 d . . .
O22 O 0.3997(3) 0.2425(5) 0.5536(4) 0.134(4) Uani 1 1 d . . .
O23 O 0.7525(3) 0.3772(6) 0.4648(4) 0.178(5) Uani 1 1 d . . .
O24 O 0.34053(16) 0.3669(2) 0.3096(2) 0.0487(16) Uani 1 1 d . . .
H3W H 0.3391 0.3489 0.2818 0.073 Uiso 1 1 d R . .
H4W H 0.3314 0.4023 0.3000 0.073 Uiso 1 1 d R . .
O25 O 0.28993(12) 0.1951(2) 0.3052(2) 0.0337(13) Uani 1 1 d . . .
H5W H 0.2775 0.1617 0.2976 0.051 Uiso 1 1 d R . .
H6W H 0.2727 0.2233 0.2948 0.051 Uiso 1 1 d R . .
N1 N 0.77446(14) 0.2746(2) 0.3609(2) 0.0172(13) Uani 1 1 d . . .
N2 N 0.75769(14) 0.3305(2) 0.3589(2) 0.0168(13) Uani 1 1 d . . .
N3 N 0.81490(13) 0.3447(2) 0.3611(2) 0.0158(13) Uani 1 1 d . . .
N4 N 0.90235(14) 0.6317(2) 0.3928(2) 0.0163(13) Uani 1 1 d . . .
N5 N 0.86448(15) 0.6277(2) 0.3868(3) 0.0235(15) Uani 1 1 d . . .
N6 N 0.88379(14) 0.5381(2) 0.3799(2) 0.0185(14) Uani 1 1 d . . .
N7 N 1.01708(16) 0.3234(2) 0.5414(3) 0.0306(17) Uani 1 1 d . . .
N8 N 0.99896(17) 0.3457(3) 0.5703(3) 0.0401(18) Uani 1 1 d . . .
N9 N 0.96019(15) 0.3611(2) 0.4793(3) 0.0230(15) Uani 1 1 d . . .
N10 N 0.72432(15) 0.1279(2) 0.3806(2) 0.0189(14) Uani 1 1 d . . .
N11 N 0.69435(15) 0.1339(2) 0.3945(3) 0.0211(15) Uani 1 1 d . . .
N12 N 0.70612(14) 0.0390(2) 0.3922(3) 0.0216(15) Uani 1 1 d . . .
N13 N 0.82843(14) -0.1685(2) 0.4031(3) 0.0214(15) Uani 1 1 d . . .
N14 N 0.81254(14) -0.2236(2) 0.4036(3) 0.0211(15) Uani 1 1 d . . .
N15 N 0.77145(14) -0.1538(2) 0.4016(2) 0.0203(14) Uani 1 1 d . . .
N16 N 0.72153(19) -0.1243(3) 0.5962(3) 0.0397(18) Uani 1 1 d . . .
N17 N 0.68638(16) -0.1563(2) 0.5674(3) 0.0226(15) Uani 1 1 d . . .
N18 N 0.70150(15) -0.1233(2) 0.5064(3) 0.0196(14) Uani 1 1 d . . .
N19 N 0.64723(15) 0.2928(2) 0.3896(3) 0.0253(16) Uani 1 1 d . . .
N20 N 0.66296(14) 0.3435(2) 0.3809(2) 0.0173(13) Uani 1 1 d . . .
N21 N 0.61053(14) 0.3681(2) 0.3877(2) 0.0136(13) Uani 1 1 d . . .
N22 N 0.45172(14) 0.2896(2) 0.4038(3) 0.0315(17) Uani 1 1 d . . .
N23 N 0.43016(14) 0.3409(2) 0.3984(3) 0.0230(15) Uani 1 1 d . . .
N24 N 0.48389(14) 0.3649(2) 0.3937(3) 0.0220(15) Uani 1 1 d . . .
N26 N 0.60922(14) 0.5823(2) 0.5633(3) 0.0281(17) Uani 1 1 d D . .
N27 N 0.58773(14) 0.5115(2) 0.5016(3) 0.0219(15) Uani 1 1 d D . .
N25 N 0.6297(3) 0.5306(3) 0.5900(5) 0.034(3) Uani 0.50 1 d PD C 5
C37 C 0.6157(2) 0.4898(5) 0.5515(3) 0.034(3) Uani 0.50 1 d PD C 5
H37A H 0.6244 0.4486 0.5576 0.041 Uiso 0.50 1 d PR C 5
C38 C 0.5850(3) 0.5706(3) 0.5111(3) 0.034(3) Uani 0.50 1 d PD C 5
H38A H 0.5674 0.5990 0.4840 0.041 Uiso 0.50 1 d PR C 5
N25A N 0.6111(3) 0.5301(3) 0.5922(4) 0.038(3) Uani 0.50 1 d PD C 6
C37A C 0.5978(3) 0.4899(5) 0.5526(3) 0.038(3) Uani 0.50 1 d PD C 6
H37B H 0.5954 0.4481 0.5591 0.046 Uiso 0.50 1 d PR C 6
C38A C 0.5956(3) 0.5708(3) 0.5110(3) 0.038(3) Uani 0.50 1 d PD C 6
H38B H 0.5917 0.6000 0.4835 0.046 Uiso 0.50 1 d PR C 6
C1 C 0.80817(18) 0.2845(3) 0.3614(3) 0.0214(17) Uani 1 1 d . . .
H1 H 0.8257 0.2539 0.3618 0.026 Uiso 1 1 calc R . .
C2 C 0.78272(18) 0.3704(3) 0.3600(3) 0.0189(16) Uani 1 1 d . . .
H2 H 0.7788 0.4126 0.3599 0.023 Uiso 1 1 calc R . .
C3 C 0.91260(18) 0.5773(3) 0.3890(3) 0.0238(19) Uani 1 1 d . . .
H3 H 0.9378 0.5667 0.3923 0.029 Uiso 1 1 calc R . .
C4 C 0.85424(18) 0.5711(2) 0.3795(3) 0.0225(18) Uani 1 1 d . . .
H4 H 0.8295 0.5556 0.3747 0.027 Uiso 1 1 calc R . .
C5 C 0.99439(19) 0.3319(3) 0.4886(4) 0.030(2) Uani 1 1 d . . .
H5 H 1.0007 0.3198 0.4610 0.036 Uiso 1 1 calc R . .
C6 C 0.9651(2) 0.3682(3) 0.5305(4) 0.036(2) Uani 1 1 d . . .
H6 H 0.9458 0.3878 0.5372 0.043 Uiso 1 1 calc R . .
C7 C 0.85149(17) 0.3734(2) 0.3650(3) 0.0171(17) Uani 1 1 d . . .
C8 C 0.84771(17) 0.4418(2) 0.3687(3) 0.0193(17) Uani 1 1 d . . .
H8A H 0.8246 0.4570 0.3343 0.023 Uiso 1 1 calc R . .
H8B H 0.8432 0.4518 0.3999 0.023 Uiso 1 1 calc R . .
C9 C 0.88659(17) 0.4710(2) 0.3771(3) 0.0154(16) Uani 1 1 d . . .
C10 C 0.92197(17) 0.4497(2) 0.4296(3) 0.0189(17) Uani 1 1 d . . .
H10A H 0.9182 0.4605 0.4613 0.023 Uiso 1 1 calc R . .
H10B H 0.9468 0.4695 0.4346 0.023 Uiso 1 1 calc R . .
C11 C 0.92577(17) 0.3811(2) 0.4270(3) 0.0192(17) Uani 1 1 d . . .
C12 C 0.88776(16) 0.3510(2) 0.4202(3) 0.0155(16) Uani 1 1 d . . .
H12A H 0.8835 0.3616 0.4515 0.019 Uiso 1 1 calc R . .
H12B H 0.8903 0.3067 0.4194 0.019 Uiso 1 1 calc R . .
C13 C 0.8574(2) 0.3577(3) 0.3172(3) 0.0255(19) Uani 1 1 d . . .
H13A H 0.8344 0.3726 0.2826 0.031 Uiso 1 1 calc R . .
H13B H 0.8590 0.3135 0.3144 0.031 Uiso 1 1 calc R . .
C14 C 0.89667(17) 0.3871(3) 0.3259(3) 0.0189(16) Uani 1 1 d . . .
H14 H 0.9009 0.3763 0.2942 0.023 Uiso 1 1 calc R . .
C15 C 0.89281(19) 0.4556(3) 0.3277(3) 0.0249(19) Uani 1 1 d . . .
H15A H 0.8696 0.4701 0.2931 0.030 Uiso 1 1 calc R . .
H15B H 0.9175 0.4754 0.3321 0.030 Uiso 1 1 calc R . .
C16 C 0.93292(19) 0.3649(3) 0.3797(3) 0.0257(19) Uani 1 1 d . . .
H16A H 0.9359 0.3208 0.3782 0.031 Uiso 1 1 calc R . .
H16B H 0.9579 0.3842 0.3848 0.031 Uiso 1 1 calc R . .
C17 C 0.73097(17) 0.0715(2) 0.3808(3) 0.0172(16) Uani 1 1 d . . .
H17 H 0.7509 0.0547 0.3738 0.021 Uiso 1 1 calc R . .
C18 C 0.68419(19) 0.0800(3) 0.4013(3) 0.0214(18) Uani 1 1 d . . .
H18 H 0.6642 0.0710 0.4112 0.026 Uiso 1 1 calc R . .
C19 C 0.80492(17) -0.1271(2) 0.4041(3) 0.0196(17) Uani 1 1 d . . .
H19 H 0.8100 -0.0850 0.4063 0.023 Uiso 1 1 calc R . .
C20 C 0.77841(19) -0.2143(3) 0.4021(3) 0.0219(17) Uani 1 1 d . . .
H20 H 0.7609 -0.2450 0.4015 0.026 Uiso 1 1 calc R . .
C21 C 0.7287(3) -0.1060(4) 0.5562(4) 0.053(3) Uani 1 1 d . . .
H21 H 0.7516 -0.0826 0.5630 0.064 Uiso 1 1 calc R . .
C22 C 0.6747(2) -0.1555(3) 0.5150(4) 0.0270(19) Uani 1 1 d . . .
H22 H 0.6512 -0.1744 0.4871 0.032 Uiso 1 1 calc R . .
C23 C 0.70288(18) -0.0268(2) 0.3962(3) 0.0186(17) Uani 1 1 d . . .
C24 C 0.73931(17) -0.0563(2) 0.3958(3) 0.0169(16) Uani 1 1 d . . .
H24A H 0.7392 -0.0465 0.3610 0.020 Uiso 1 1 calc R . .
H24B H 0.7646 -0.0410 0.4269 0.020 Uiso 1 1 calc R . .
C25 C 0.73655(17) -0.1250(2) 0.4009(3) 0.0175(17) Uani 1 1 d . . .
C26 C 0.73688(18) -0.1398(2) 0.4549(3) 0.0183(17) Uani 1 1 d . . .
H26A H 0.7353 -0.1839 0.4585 0.022 Uiso 1 1 calc R . .
H26B H 0.7622 -0.1253 0.4866 0.022 Uiso 1 1 calc R . .
C27 C 0.70111(18) -0.1096(3) 0.4551(3) 0.0195(16) Uani 1 1 d . . .
C28 C 0.70287(18) -0.0411(2) 0.4488(3) 0.0155(16) Uani 1 1 d . . .
H28A H 0.6793 -0.0219 0.4485 0.019 Uiso 1 1 calc R . .
H28B H 0.7276 -0.0247 0.4804 0.019 Uiso 1 1 calc R . .
C29 C 0.66392(18) -0.0493(3) 0.3449(3) 0.0276(19) Uani 1 1 d . . .
H29A H 0.6650 -0.0408 0.3108 0.033 Uiso 1 1 calc R . .
H29B H 0.6400 -0.0291 0.3425 0.033 Uiso 1 1 calc R . .
C30 C 0.66185(18) -0.1188(3) 0.3527(3) 0.0227(18) Uani 1 1 d . . .
H30 H 0.6366 -0.1350 0.3211 0.027 Uiso 1 1 calc R . .
C31 C 0.69808(17) -0.1480(3) 0.3523(3) 0.0225(18) Uani 1 1 d . . .
H31A H 0.6966 -0.1923 0.3546 0.027 Uiso 1 1 calc R . .
H31B H 0.6979 -0.1381 0.3175 0.027 Uiso 1 1 calc R . .
C32 C 0.66186(19) -0.1329(3) 0.4059(3) 0.0228(18) Uani 1 1 d . . .
H32A H 0.6596 -0.1769 0.4093 0.027 Uiso 1 1 calc R . .
H32B H 0.6385 -0.1134 0.4057 0.027 Uiso 1 1 calc R . .
C33 C 0.61579(17) 0.3082(3) 0.3939(3) 0.0224(18) Uani 1 1 d . . .
H33 H 0.5992 0.2812 0.4004 0.027 Uiso 1 1 calc R . .
C34 C 0.64043(18) 0.3881(3) 0.3788(3) 0.0187(17) Uani 1 1 d . . .
H34 H 0.6443 0.4288 0.3720 0.022 Uiso 1 1 calc R . .
C35 C 0.48331(17) 0.3047(3) 0.4014(3) 0.027(2) Uani 1 1 d . . .
H35 H 0.5035 0.2775 0.4045 0.033 Uiso 1 1 calc R . .
C36 C 0.45012(19) 0.3854(3) 0.3928(3) 0.028(2) Uani 1 1 d . . .
H36 H 0.4421 0.4264 0.3886 0.033 Uiso 1 1 calc R . .
C39 C 0.57877(17) 0.4057(2) 0.3899(3) 0.0167(16) Uani 1 1 d . C .
C40 C 0.54641(16) 0.3645(2) 0.3888(3) 0.0163(16) Uani 1 1 d . . .
H40A H 0.5335 0.3413 0.3541 0.020 Uiso 1 1 calc R . .
H40B H 0.5586 0.3358 0.4200 0.020 Uiso 1 1 calc R . .
C41 C 0.51531(18) 0.4035(2) 0.3934(3) 0.0206(18) Uani 1 1 d . C .
C42 C 0.53548(18) 0.4380(3) 0.4472(3) 0.0217(18) Uani 1 1 d . . .
H42A H 0.5152 0.4624 0.4509 0.026 Uiso 1 1 calc R C .
H42B H 0.5477 0.4095 0.4784 0.026 Uiso 1 1 calc R . .
C43 C 0.56757(18) 0.4785(3) 0.4483(3) 0.0212(17) Uani 1 1 d . C .
C44 C 0.60009(18) 0.4398(3) 0.4451(3) 0.0256(19) Uani 1 1 d . . .
H44A H 0.6217 0.4656 0.4465 0.031 Uiso 1 1 calc R C .
H44B H 0.6121 0.4111 0.4762 0.031 Uiso 1 1 calc R . .
C45 C 0.56045(19) 0.4494(3) 0.3409(3) 0.0255(19) Uani 1 1 d . . .
H45A H 0.5817 0.4755 0.3416 0.031 Uiso 1 1 calc R C .
H45B H 0.5478 0.4266 0.3059 0.031 Uiso 1 1 calc R . .
C46 C 0.52879(18) 0.4879(3) 0.3453(3) 0.0246(19) Uani 1 1 d . C .
H46 H 0.5165 0.5170 0.3139 0.030 Uiso 1 1 calc R . .
C47 C 0.49599(18) 0.4468(3) 0.3448(3) 0.0261(19) Uani 1 1 d . . .
H47A H 0.4754 0.4714 0.3474 0.031 Uiso 1 1 calc R C .
H47B H 0.4826 0.4238 0.3099 0.031 Uiso 1 1 calc R . .
C48 C 0.54994(19) 0.5231(3) 0.4017(3) 0.0250(19) Uani 1 1 d . . .
H48A H 0.5715 0.5492 0.4031 0.030 Uiso 1 1 calc R C .
H48B H 0.5301 0.5489 0.4050 0.030 Uiso 1 1 calc R . .
O1W O 0.5925(2) 0.3802(3) 0.2441(3) 0.096(3) Uani 1 1 d . . .
O2W O 0.7914(2) -0.2122(3) 0.5816(4) 0.103(3) Uani 1 1 d . . .
O3W O 0.2498(2) 0.0890(4) 0.2808(4) 0.116(3) Uani 1 1 d . . .
O4W O 0.6403(3) 0.0803(3) 0.2621(4) 0.144(4) Uani 1 1 d . . .
O5W O 0.5358(3) 0.3160(3) 0.2520(4) 0.111(3) Uani 1 1 d . . .
O6W O 0.8121(2) -0.0201(3) 0.2846(4) 0.110(3) Uani 1 1 d . . .
O7W O 0.4191(3) 0.0744(3) 0.5165(4) 0.116(3) Uani 1 1 d . . .
O8W O 0.6554(3) -0.0002(4) 0.5229(5) 0.134(3) Uiso 1 1 d . . .
O9W O 0.2318(3) 0.2890(4) 0.2705(5) 0.143(3) Uiso 1 1 d . . .
O10W O 0.6713(3) 0.6373(4) 0.3266(5) 0.149(4) Uiso 1 1 d . . .
O11W O 0.4968(3) 0.0063(4) 0.5741(4) 0.133(3) Uiso 1 1 d . . .
O12W O 0.5386(3) 0.4635(5) 0.5762(5) 0.155(4) Uiso 1 1 d . . .
O13W O 0.2417(3) 0.4118(5) 0.2695(5) 0.169(4) Uiso 1 1 d . . .
O14W O 0.7034(3) 0.0235(4) 0.2540(5) 0.153(4) Uiso 1 1 d . . .
O15W O 0.3380(3) 0.3225(5) 0.5313(5) 0.170(4) Uiso 1 1 d . . .
O16W O 0.5578(4) 0.1939(6) 0.2804(7) 0.118(4) Uiso 0.65 1 d P . .
O17W O 0.5502(6) 0.2018(9) 0.2130(11) 0.098(7) Uiso 0.35 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0224(4) 0.0155(4) 0.0380(7) -0.0016(4) 0.0231(4) -0.0010(3)
Cu2 0.0242(4) 0.0137(4) 0.0383(7) 0.0028(4) 0.0252(4) 0.0036(3)
Cu3 0.0195(4) 0.0155(4) 0.0382(7) 0.0016(4) 0.0207(4) 0.0017(3)
Cu4 0.0154(4) 0.0169(4) 0.0428(8) 0.0061(4) 0.0111(4) 0.0016(3)
Cu5 0.0211(4) 0.0148(4) 0.0366(7) -0.0081(4) 0.0209(4) -0.0045(3)
Cu6 0.0232(4) 0.0133(4) 0.0325(7) 0.0041(4) 0.0227(4) 0.0029(3)
S1 0.0224(8) 0.0259(8) 0.0160(14) -0.0010(8) 0.0118(9) -0.0031(7)
S2 0.0621(16) 0.0503(14) 0.141(4) -0.0088(17) 0.067(2) 0.0008(13)
S3 0.0507(13) 0.0501(12) 0.044(2) 0.0059(11) 0.0320(13) 0.0039(11)
S4 0.0796(18) 0.0375(12) 0.135(3) -0.0055(15) 0.075(2) -0.0006(12)
S5 0.0351(10) 0.0339(10) 0.0264(17) -0.0017(9) 0.0140(11) -0.0004(8)
O1 0.017(2) 0.018(2) 0.012(3) -0.0046(19) 0.009(2) -0.0006(17)
O2 0.014(2) 0.018(2) 0.010(3) 0.0023(18) 0.008(2) 0.0008(17)
O3 0.024(2) 0.031(2) 0.030(4) -0.006(2) 0.016(2) 0.007(2)
O4 0.025(2) 0.036(3) 0.040(4) 0.004(2) 0.026(3) -0.004(2)
O5 0.026(2) 0.018(2) 0.036(4) 0.004(2) 0.013(3) 0.0048(19)
O6 0.025(2) 0.051(3) 0.008(4) 0.002(2) 0.007(2) -0.007(2)
O7 0.053(3) 0.034(3) 0.097(6) -0.002(3) 0.064(4) 0.008(3)
O8 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O9 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O10 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O8A 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O9A 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O10A 0.062(4) 0.102(4) 0.111(8) -0.036(4) 0.049(5) 0.003(3)
O11 0.031(2) 0.027(2) 0.032(4) 0.001(2) 0.025(3) 0.001(2)
O12 0.062(5) 0.287(13) 0.051(9) -0.003(7) 0.001(5) 0.002(6)
O13 0.142(6) 0.047(4) 0.106(8) 0.022(4) 0.096(6) 0.006(4)
O14 0.093(5) 0.067(4) 0.080(7) 0.005(4) 0.073(5) 0.018(4)
O15 0.067(4) 0.013(2) 0.115(7) 0.002(3) 0.067(4) 0.001(2)
O16 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O17 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O18 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O16A 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O17A 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O18A 0.104(5) 0.030(3) 0.166(9) 0.017(3) 0.093(5) 0.012(3)
O19 0.089(4) 0.046(4) 0.052(6) 0.007(3) 0.018(4) -0.002(3)
O20 0.197(9) 0.051(4) 0.103(10) 0.009(5) 0.038(7) -0.022(5)
O21 0.054(4) 0.144(7) 0.078(8) -0.038(5) 0.003(4) 0.022(4)
O22 0.130(7) 0.189(9) 0.126(11) -0.040(7) 0.097(8) -0.043(7)
O23 0.091(6) 0.358(17) 0.062(11) -0.023(9) 0.020(6) -0.051(8)
O24 0.080(4) 0.034(3) 0.038(5) -0.001(3) 0.033(4) 0.009(3)
O25 0.027(2) 0.044(3) 0.030(4) -0.001(2) 0.013(3) 0.005(2)
N1 0.019(3) 0.018(3) 0.016(4) 0.001(2) 0.010(3) -0.004(2)
N2 0.015(2) 0.018(3) 0.021(4) -0.001(2) 0.011(3) -0.001(2)
N3 0.009(2) 0.018(3) 0.023(4) 0.001(2) 0.009(3) -0.003(2)
N4 0.015(3) 0.021(3) 0.017(4) 0.003(2) 0.012(3) -0.001(2)
N5 0.020(3) 0.014(3) 0.043(5) 0.002(3) 0.020(3) 0.006(2)
N6 0.016(3) 0.015(3) 0.030(5) 0.010(2) 0.016(3) 0.005(2)
N7 0.024(3) 0.020(3) 0.041(6) 0.011(3) 0.010(3) 0.007(2)
N8 0.028(3) 0.045(4) 0.041(6) 0.001(3) 0.012(4) 0.007(3)
N9 0.014(3) 0.021(3) 0.028(5) 0.007(3) 0.005(3) 0.003(2)
N10 0.022(3) 0.016(3) 0.029(5) 0.001(2) 0.021(3) 0.000(2)
N11 0.025(3) 0.017(3) 0.030(5) 0.005(2) 0.020(3) 0.008(2)
N12 0.019(3) 0.016(3) 0.031(5) 0.010(3) 0.013(3) 0.009(2)
N13 0.018(3) 0.018(3) 0.037(5) -0.004(3) 0.020(3) -0.001(2)
N14 0.018(3) 0.013(3) 0.039(5) 0.005(2) 0.020(3) 0.004(2)
N15 0.022(3) 0.011(2) 0.036(5) 0.001(2) 0.020(3) 0.004(2)
N16 0.054(4) 0.052(4) 0.005(5) -0.004(3) 0.008(4) -0.027(3)
N17 0.030(3) 0.012(3) 0.040(5) -0.002(3) 0.028(3) -0.002(2)
N18 0.025(3) 0.017(3) 0.027(5) -0.003(3) 0.021(3) -0.001(2)
N19 0.023(3) 0.018(3) 0.047(5) 0.003(3) 0.027(3) 0.001(2)
N20 0.015(2) 0.020(3) 0.020(4) 0.003(2) 0.010(3) 0.005(2)
N21 0.018(3) 0.014(2) 0.015(4) -0.004(2) 0.013(3) 0.000(2)
N22 0.017(3) 0.017(3) 0.063(6) 0.006(3) 0.021(3) 0.001(2)
N23 0.020(3) 0.010(2) 0.043(5) 0.000(3) 0.018(3) 0.002(2)
N24 0.015(3) 0.013(2) 0.042(5) -0.008(3) 0.017(3) -0.004(2)
N26 0.019(3) 0.018(3) 0.056(6) -0.006(3) 0.024(3) -0.009(2)
N27 0.018(3) 0.022(3) 0.028(5) -0.008(3) 0.013(3) -0.003(2)
N25 0.023(5) 0.018(4) 0.060(9) -0.006(4) 0.019(5) 0.002(3)
C37 0.023(5) 0.018(4) 0.060(9) -0.006(4) 0.019(5) 0.002(3)
C38 0.023(5) 0.018(4) 0.060(9) -0.006(4) 0.019(5) 0.002(3)
N25A 0.037(5) 0.036(5) 0.038(9) -0.023(5) 0.015(5) -0.008(4)
C37A 0.037(5) 0.036(5) 0.038(9) -0.023(5) 0.015(5) -0.008(4)
C38A 0.037(5) 0.036(5) 0.038(9) -0.023(5) 0.015(5) -0.008(4)
C1 0.022(3) 0.015(3) 0.031(6) -0.007(3) 0.016(4) -0.001(3)
C2 0.024(3) 0.023(3) 0.011(5) -0.001(3) 0.010(3) 0.001(3)
C3 0.017(3) 0.017(3) 0.044(6) 0.001(3) 0.020(4) -0.006(3)
C4 0.021(3) 0.015(3) 0.038(6) 0.001(3) 0.019(4) 0.001(3)
C5 0.023(3) 0.023(3) 0.045(7) -0.003(4) 0.018(4) -0.004(3)
C6 0.024(4) 0.040(4) 0.041(8) 0.005(4) 0.014(4) 0.003(3)
C7 0.019(3) 0.011(3) 0.026(6) -0.001(3) 0.015(4) -0.004(3)
C8 0.017(3) 0.012(3) 0.033(6) 0.005(3) 0.016(3) 0.003(2)
C9 0.015(3) 0.011(3) 0.028(6) -0.001(3) 0.017(3) -0.001(2)
C10 0.013(3) 0.013(3) 0.035(6) 0.000(3) 0.016(3) 0.000(2)
C11 0.014(3) 0.010(3) 0.032(6) 0.004(3) 0.010(3) 0.002(2)
C12 0.016(3) 0.014(3) 0.020(5) 0.006(3) 0.011(3) 0.003(2)
C13 0.030(4) 0.020(3) 0.036(6) -0.002(3) 0.024(4) 0.001(3)
C14 0.017(3) 0.022(3) 0.017(6) 0.002(3) 0.008(3) -0.001(3)
C15 0.020(3) 0.022(3) 0.035(6) 0.004(3) 0.015(4) 0.000(3)
C16 0.026(4) 0.015(3) 0.047(7) 0.002(3) 0.026(4) -0.001(3)
C17 0.013(3) 0.018(3) 0.025(6) 0.007(3) 0.013(3) 0.005(3)
C18 0.029(4) 0.020(3) 0.032(6) -0.002(3) 0.029(4) -0.002(3)
C19 0.022(3) 0.010(3) 0.037(6) -0.003(3) 0.023(4) -0.003(3)
C20 0.026(3) 0.019(3) 0.034(6) 0.002(3) 0.026(4) 0.000(3)
C21 0.059(5) 0.069(6) 0.042(9) -0.009(5) 0.033(6) -0.042(5)
C22 0.024(4) 0.030(4) 0.034(7) 0.004(4) 0.020(4) -0.001(3)
C23 0.025(3) 0.011(3) 0.021(6) -0.001(3) 0.013(4) -0.001(3)
C24 0.016(3) 0.012(3) 0.023(5) 0.005(3) 0.010(3) 0.002(2)
C25 0.015(3) 0.012(3) 0.026(6) -0.007(3) 0.010(3) -0.002(2)
C26 0.020(3) 0.013(3) 0.028(6) 0.004(3) 0.017(4) 0.004(3)
C27 0.017(3) 0.026(3) 0.014(5) 0.006(3) 0.007(3) 0.008(3)
C28 0.017(3) 0.014(3) 0.026(5) -0.002(3) 0.019(3) 0.003(2)
C29 0.023(3) 0.026(4) 0.029(6) 0.006(3) 0.009(4) 0.008(3)
C30 0.018(3) 0.016(3) 0.034(6) -0.004(3) 0.013(4) 0.002(3)
C31 0.021(3) 0.021(3) 0.031(6) -0.004(3) 0.017(4) -0.001(3)
C32 0.025(3) 0.016(3) 0.035(6) 0.003(3) 0.021(4) 0.000(3)
C33 0.013(3) 0.021(3) 0.037(6) 0.004(3) 0.016(3) 0.005(3)
C34 0.026(3) 0.015(3) 0.020(6) 0.001(3) 0.015(4) -0.003(3)
C35 0.013(3) 0.016(3) 0.055(7) -0.002(3) 0.019(4) -0.002(3)
C36 0.026(3) 0.012(3) 0.059(7) 0.000(3) 0.032(4) 0.005(3)
C39 0.018(3) 0.010(3) 0.030(6) -0.001(3) 0.019(3) 0.003(2)
C40 0.011(3) 0.013(3) 0.024(5) -0.009(3) 0.008(3) -0.001(2)
C41 0.019(3) 0.012(3) 0.042(6) -0.007(3) 0.024(4) -0.001(3)
C42 0.020(3) 0.014(3) 0.041(6) -0.005(3) 0.023(4) -0.004(3)
C43 0.026(3) 0.021(3) 0.025(6) -0.006(3) 0.019(4) -0.001(3)
C44 0.021(3) 0.020(3) 0.049(7) 0.006(3) 0.027(4) 0.000(3)
C45 0.026(3) 0.020(3) 0.036(6) -0.001(3) 0.019(4) 0.005(3)
C46 0.024(3) 0.012(3) 0.044(6) 0.000(3) 0.022(4) 0.003(3)
C47 0.018(3) 0.016(3) 0.050(7) -0.004(3) 0.021(4) -0.002(3)
C48 0.027(3) 0.018(3) 0.036(6) 0.003(3) 0.021(4) -0.002(3)
O1W 0.072(4) 0.118(6) 0.091(8) 0.019(5) 0.035(5) 0.047(4)
O2W 0.139(6) 0.045(4) 0.115(9) 0.002(4) 0.054(6) -0.015(4)
O3W 0.114(6) 0.150(7) 0.084(9) -0.032(6) 0.049(6) -0.050(6)
O4W 0.187(8) 0.038(4) 0.105(9) 0.001(4) -0.008(7) -0.013(5)
O5W 0.136(7) 0.081(5) 0.134(10) 0.008(5) 0.078(7) 0.020(5)
O6W 0.142(7) 0.089(5) 0.090(9) 0.021(5) 0.051(6) 0.045(5)
O7W 0.160(7) 0.069(5) 0.126(10) 0.030(5) 0.074(7) 0.022(5)

_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.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O7 1.939(4) . ?
Cu1 N1 1.976(4) . ?
Cu1 N10 1.994(5) . ?
Cu1 O1 2.011(4) . ?
Cu1 O3 2.282(5) . ?
Cu2 O11 1.953(4) . ?
Cu2 N19 1.966(5) . ?
Cu2 N11 1.968(5) . ?
Cu2 O1 1.999(4) . ?
Cu2 O4 2.204(5) . ?
Cu3 O15 1.963(5) . ?
Cu3 N2 1.980(4) . ?
Cu3 N20 1.987(5) . ?
Cu3 O1 1.999(4) . ?
Cu3 O5 2.304(5) . ?
Cu3 O23 2.595(11) . ?
Cu4 N7 1.956(5) 7_656 ?
Cu4 O2 1.966(4) . ?
Cu4 N4 2.039(5) 3_445 ?
Cu4 N22 2.039(5) . ?
Cu4 O19 2.224(7) . ?
Cu5 N23 1.969(5) . ?
Cu5 O2 1.970(4) . ?
Cu5 N26 1.980(5) 5_666 ?
Cu5 N13 1.981(5) 3_455 ?
Cu5 O24 2.325(6) . ?
Cu5 O20 2.625(10) . ?
Cu6 N17 1.966(5) 5_656 ?
Cu6 O2 1.980(4) . ?
Cu6 N14 1.993(5) 3_455 ?
Cu6 N5 2.006(5) 3_445 ?
Cu6 O25 2.289(5) . ?
S1 O6 1.468(5) . ?
S1 O5 1.474(4) . ?
S1 O4 1.483(5) . ?
S1 O3 1.488(4) . ?
S2 O9A 1.442(4) . ?
S2 O10A 1.445(4) . ?
S2 O8A 1.457(5) . ?
S2 O7 1.460(5) . ?
S2 O9 1.477(4) . ?
S2 O8 1.483(5) . ?
S2 O10 1.493(4) . ?
S3 O12 1.441(8) . ?
S3 O13 1.441(6) . ?
S3 O14 1.464(5) . ?
S3 O11 1.497(5) . ?
S4 O15 1.417(5) . ?
S4 O17A 1.448(4) . ?
S4 O16A 1.457(4) . ?
S4 O18A 1.465(5) . ?
S4 O17 1.465(4) . ?
S4 O18 1.475(4) . ?
S4 O16 1.488(4) . ?
S5 O20 1.377(7) . ?
S5 O21 1.453(7) . ?
S5 O22 1.486(8) . ?
S5 O19 1.521(7) . ?
O1 H1W 1.0000 . ?
O2 H2W 1.0000 . ?
O24 H3W 0.8502 . ?
O24 H4W 0.8500 . ?
O25 H5W 0.8500 . ?
O25 H6W 0.8501 . ?
N1 C1 1.299(7) . ?
N1 N2 1.385(6) . ?
N2 C2 1.293(7) . ?
N3 C2 1.340(7) . ?
N3 C1 1.363(7) . ?
N3 C7 1.489(7) . ?
N4 C3 1.290(7) . ?
N4 N5 1.372(6) . ?
N4 Cu4 2.039(5) 3 ?
N5 C4 1.302(7) . ?
N5 Cu6 2.006(5) 3 ?
N6 C3 1.326(7) . ?
N6 C4 1.341(7) . ?
N6 C9 1.499(7) . ?
N7 C5 1.303(9) . ?
N7 N8 1.385(9) . ?
N7 Cu4 1.956(5) 7_656 ?
N8 C6 1.319(9) . ?
N9 C6 1.352(10) . ?
N9 C5 1.362(8) . ?
N9 C11 1.473(9) . ?
N10 C17 1.277(7) . ?
N10 N11 1.382(6) . ?
N11 C18 1.302(7) . ?
N12 C18 1.342(7) . ?
N12 C17 1.348(7) . ?
N12 C23 1.477(7) . ?
N13 C19 1.295(7) . ?
N13 N14 1.370(6) . ?
N13 Cu5 1.981(5) 3_545 ?
N14 C20 1.299(7) . ?
N14 Cu6 1.993(5) 3_545 ?
N15 C20 1.369(7) . ?
N15 C19 1.378(7) . ?
N15 C25 1.468(7) . ?
N16 C21 1.337(10) . ?
N16 N17 1.376(7) . ?
N17 C22 1.301(9) . ?
N17 Cu6 1.966(5) 5_656 ?
N18 C21 1.318(10) . ?
N18 C22 1.361(7) . ?
N18 C27 1.452(9) . ?
N19 C33 1.308(7) . ?
N19 N20 1.351(6) . ?
N20 C34 1.294(7) . ?
N21 C33 1.346(7) . ?
N21 C34 1.356(7) . ?
N21 C39 1.498(6) . ?
N22 C35 1.284(7) . ?
N22 N23 1.371(6) . ?
N23 C36 1.304(7) . ?
N24 C36 1.354(7) . ?
N24 C35 1.357(7) . ?
N24 C41 1.477(7) . ?
N26 C38A 1.308(5) . ?
N26 C38 1.312(5) . ?
N26 N25 1.382(5) . ?
N26 N25A 1.394(5) . ?
N26 Cu5 1.980(5) 5_666 ?
N27 C38A 1.350(5) . ?
N27 C38 1.354(5) . ?
N27 C37 1.359(5) . ?
N27 C37A 1.365(5) . ?
N27 C43 1.487(8) . ?
N25 C37 1.304(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 1.2898 . ?
C38 H38A 0.9600 . ?
C38 H38B 1.1313 . ?
N25A C37A 1.312(5) . ?
C37A H37B 0.9600 . ?
C38A H38B 0.9600 . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C13 1.495(9) . ?
C7 C8 1.537(7) . ?
C7 C12 1.562(9) . ?
C8 C9 1.527(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.498(9) . ?
C9 C15 1.544(10) . ?
C10 C11 1.538(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C16 1.513(10) . ?
C11 C12 1.522(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.540(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.534(8) . ?
C14 C16 1.538(9) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.497(9) . ?
C23 C24 1.542(8) . ?
C23 C29 1.555(9) . ?
C24 C25 1.542(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C31 1.516(9) . ?
C25 C26 1.534(9) . ?
C26 C27 1.523(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.539(8) . ?
C27 C32 1.541(9) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.567(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C32 1.514(10) . ?
C30 C31 1.532(8) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C39 C40 1.525(7) . ?
C39 C45 1.536(9) . ?
C39 C44 1.539(10) . ?
C40 C41 1.525(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.513(9) . ?
C41 C47 1.524(10) . ?
C42 C43 1.508(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C48 1.504(9) . ?
C43 C44 1.548(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.533(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.544(8) . ?
C46 C48 1.575(10) . ?
C46 H46 1.0000 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
O16W O17W 1.76(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Cu1 N1 91.5(2) . . ?
O7 Cu1 N10 91.5(2) . . ?
N1 Cu1 N10 169.2(2) . . ?
O7 Cu1 O1 178.89(17) . . ?
N1 Cu1 O1 87.43(18) . . ?
N10 Cu1 O1 89.59(18) . . ?
O7 Cu1 O3 90.1(2) . . ?
N1 Cu1 O3 98.3(2) . . ?
N10 Cu1 O3 92.0(2) . . ?
O1 Cu1 O3 90.17(16) . . ?
O11 Cu2 N19 91.93(18) . . ?
O11 Cu2 N11 88.87(18) . . ?
N19 Cu2 N11 178.8(3) . . ?
O11 Cu2 O1 171.8(2) . . ?
N19 Cu2 O1 89.54(17) . . ?
N11 Cu2 O1 89.54(17) . . ?
O11 Cu2 O4 96.98(18) . . ?
N19 Cu2 O4 90.6(2) . . ?
N11 Cu2 O4 90.2(2) . . ?
O1 Cu2 O4 91.06(17) . . ?
O15 Cu3 N2 91.8(2) . . ?
O15 Cu3 N20 90.9(2) . . ?
N2 Cu3 N20 173.3(2) . . ?
O15 Cu3 O1 179.7(2) . . ?
N2 Cu3 O1 87.85(17) . . ?
N20 Cu3 O1 89.47(17) . . ?
O15 Cu3 O5 90.9(2) . . ?
N2 Cu3 O5 98.8(2) . . ?
N20 Cu3 O5 87.3(2) . . ?
O1 Cu3 O5 89.02(16) . . ?
O15 Cu3 O23 89.7(4) . . ?
N2 Cu3 O23 88.4(3) . . ?
N20 Cu3 O23 85.4(3) . . ?
O1 Cu3 O23 90.4(3) . . ?
O5 Cu3 O23 172.7(2) . . ?
N7 Cu4 O2 177.6(3) 7_656 . ?
N7 Cu4 N4 92.1(2) 7_656 3_445 ?
O2 Cu4 N4 88.98(17) . 3_445 ?
N7 Cu4 N22 92.1(2) 7_656 . ?
O2 Cu4 N22 88.16(17) . . ?
N4 Cu4 N22 148.3(3) 3_445 . ?
N7 Cu4 O19 94.6(3) 7_656 . ?
O2 Cu4 O19 83.4(2) . . ?
N4 Cu4 O19 83.0(2) 3_445 . ?
N22 Cu4 O19 127.8(2) . . ?
N23 Cu5 O2 88.53(17) . . ?
N23 Cu5 N26 90.53(19) . 5_666 ?
O2 Cu5 N26 166.6(2) . 5_666 ?
N23 Cu5 N13 178.2(2) . 3_455 ?
O2 Cu5 N13 89.64(17) . 3_455 ?
N26 Cu5 N13 91.25(19) 5_666 3_455 ?
N23 Cu5 O24 93.5(2) . . ?
O2 Cu5 O24 94.05(18) . . ?
N26 Cu5 O24 99.3(2) 5_666 . ?
N13 Cu5 O24 86.6(2) 3_455 . ?
N23 Cu5 O20 87.7(3) . . ?
O2 Cu5 O20 84.5(2) . . ?
N26 Cu5 O20 82.1(2) 5_666 . ?
N13 Cu5 O20 92.1(3) 3_455 . ?
O24 Cu5 O20 178.1(2) . . ?
N17 Cu6 O2 162.1(2) 5_656 . ?
N17 Cu6 N14 89.3(2) 5_656 3_455 ?
O2 Cu6 N14 89.56(17) . 3_455 ?
N17 Cu6 N5 92.4(2) 5_656 3_445 ?
O2 Cu6 N5 88.91(18) . 3_445 ?
N14 Cu6 N5 178.2(2) 3_455 3_445 ?
N17 Cu6 O25 102.1(2) 5_656 . ?
O2 Cu6 O25 95.75(18) . . ?
N14 Cu6 O25 89.9(2) 3_455 . ?
N5 Cu6 O25 89.3(2) 3_445 . ?
O6 S1 O5 110.2(3) . . ?
O6 S1 O4 109.7(3) . . ?
O5 S1 O4 110.3(3) . . ?
O6 S1 O3 110.6(3) . . ?
O5 S1 O3 107.4(2) . . ?
O4 S1 O3 108.7(3) . . ?
O9A S2 O10A 111.3(4) . . ?
O9A S2 O8A 109.3(4) . . ?
O10A S2 O8A 109.1(4) . . ?
O9A S2 O7 113.3(6) . . ?
O10A S2 O7 110.3(6) . . ?
O8A S2 O7 103.1(6) . . ?
O7 S2 O9 120.7(5) . . ?
O7 S2 O8 113.9(5) . . ?
O9 S2 O8 105.5(4) . . ?
O7 S2 O10 106.5(5) . . ?
O9 S2 O10 104.4(4) . . ?
O8 S2 O10 104.2(4) . . ?
O12 S3 O13 111.9(6) . . ?
O12 S3 O14 109.2(5) . . ?
O13 S3 O14 110.1(4) . . ?
O12 S3 O11 109.0(5) . . ?
O13 S3 O11 108.3(4) . . ?
O14 S3 O11 108.3(3) . . ?
O15 S4 O17A 119.2(6) . . ?
O15 S4 O16A 114.1(6) . . ?
O17A S4 O16A 109.9(4) . . ?
O17A S4 O18A 108.4(4) . . ?
O16A S4 O18A 107.6(4) . . ?
O15 S4 O17 111.7(5) . . ?
O15 S4 O18 113.0(4) . . ?
O17 S4 O18 107.2(4) . . ?
O15 S4 O16 113.6(5) . . ?
O17 S4 O16 105.9(4) . . ?
O18 S4 O16 105.0(4) . . ?
O20 S5 O21 114.7(6) . . ?
O20 S5 O22 110.4(6) . . ?
O21 S5 O22 105.9(6) . . ?
O20 S5 O19 108.3(5) . . ?
O21 S5 O19 109.8(4) . . ?
O22 S5 O19 107.5(4) . . ?
Cu3 O1 Cu2 114.58(17) . . ?
Cu3 O1 Cu1 114.0(2) . . ?
Cu2 O1 Cu1 113.92(18) . . ?
Cu3 O1 H1W 104.2 . . ?
Cu2 O1 H1W 104.2 . . ?
Cu1 O1 H1W 104.2 . . ?
Cu4 O2 Cu5 111.38(18) . . ?
Cu4 O2 Cu6 109.32(18) . . ?
Cu5 O2 Cu6 117.67(18) . . ?
Cu4 O2 H2W 105.9 . . ?
Cu5 O2 H2W 105.9 . . ?
Cu6 O2 H2W 105.9 . . ?
S1 O3 Cu1 123.1(3) . . ?
S1 O4 Cu2 125.1(3) . . ?
S1 O5 Cu3 124.2(3) . . ?
S2 O7 Cu1 132.7(4) . . ?
S3 O11 Cu2 128.1(3) . . ?
S4 O15 Cu3 137.0(5) . . ?
S5 O19 Cu4 116.6(3) . . ?
S5 O20 Cu5 134.2(5) . . ?
Cu5 O24 H3W 125.9 . . ?
Cu5 O24 H4W 123.2 . . ?
H3W O24 H4W 108.5 . . ?
Cu6 O25 H5W 112.2 . . ?
Cu6 O25 H6W 113.5 . . ?
H5W O25 H6W 108.4 . . ?
C1 N1 N2 106.5(4) . . ?
C1 N1 Cu1 134.0(4) . . ?
N2 N1 Cu1 119.5(3) . . ?
C2 N2 N1 107.0(4) . . ?
C2 N2 Cu3 132.0(4) . . ?
N1 N2 Cu3 120.4(3) . . ?
C2 N3 C1 104.2(5) . . ?
C2 N3 C7 129.4(5) . . ?
C1 N3 C7 126.3(4) . . ?
C3 N4 N5 105.8(4) . . ?
C3 N4 Cu4 138.0(4) . 3 ?
N5 N4 Cu4 114.7(3) . 3 ?
C4 N5 N4 107.4(5) . . ?
C4 N5 Cu6 132.9(4) . 3 ?
N4 N5 Cu6 119.5(3) . 3 ?
C3 N6 C4 104.8(5) . . ?
C3 N6 C9 126.2(5) . . ?
C4 N6 C9 128.7(5) . . ?
C5 N7 N8 111.0(6) . . ?
C5 N7 Cu4 128.4(5) . 7_656 ?
N8 N7 Cu4 120.5(6) . 7_656 ?
C6 N8 N7 101.9(7) . . ?
C6 N9 C5 103.2(6) . . ?
C6 N9 C11 127.2(6) . . ?
C5 N9 C11 129.6(7) . . ?
C17 N10 N11 106.5(4) . . ?
C17 N10 Cu1 134.2(4) . . ?
N11 N10 Cu1 119.3(3) . . ?
C18 N11 N10 107.2(4) . . ?
C18 N11 Cu2 131.6(4) . . ?
N10 N11 Cu2 120.6(4) . . ?
C18 N12 C17 104.8(5) . . ?
C18 N12 C23 125.1(5) . . ?
C17 N12 C23 130.1(5) . . ?
C19 N13 N14 108.7(4) . . ?
C19 N13 Cu5 130.8(4) . 3_545 ?
N14 N13 Cu5 120.5(3) . 3_545 ?
C20 N14 N13 107.4(4) . . ?
C20 N14 Cu6 131.8(4) . 3_545 ?
N13 N14 Cu6 120.2(3) . 3_545 ?
C20 N15 C19 104.7(4) . . ?
C20 N15 C25 126.7(5) . . ?
C19 N15 C25 128.6(4) . . ?
C21 N16 N17 102.2(7) . . ?
C22 N17 N16 110.3(5) . . ?
C22 N17 Cu6 126.9(4) . 5_656 ?
N16 N17 Cu6 122.6(5) . 5_656 ?
C21 N18 C22 103.8(7) . . ?
C21 N18 C27 126.6(6) . . ?
C22 N18 C27 129.6(6) . . ?
C33 N19 N20 107.8(5) . . ?
C33 N19 Cu2 130.5(4) . . ?
N20 N19 Cu2 121.7(3) . . ?
C34 N20 N19 107.7(4) . . ?
C34 N20 Cu3 132.2(4) . . ?
N19 N20 Cu3 119.5(3) . . ?
C33 N21 C34 105.2(5) . . ?
C33 N21 C39 128.3(5) . . ?
C34 N21 C39 126.5(5) . . ?
C35 N22 N23 107.7(5) . . ?
C35 N22 Cu4 136.9(4) . . ?
N23 N22 Cu4 115.2(3) . . ?
C36 N23 N22 106.9(4) . . ?
C36 N23 Cu5 132.4(4) . . ?
N22 N23 Cu5 120.7(4) . . ?
C36 N24 C35 104.3(5) . . ?
C36 N24 C41 124.8(5) . . ?
C35 N24 C41 130.5(5) . . ?
C38 N26 N25 109.7(7) . . ?
C38A N26 N25A 111.2(7) . . ?
C38A N26 Cu5 127.1(4) . 5_666 ?
C38 N26 Cu5 126.6(4) . 5_666 ?
N25 N26 Cu5 123.4(6) . 5_666 ?
N25A N26 Cu5 121.4(6) . 5_666 ?
C38 N27 C37 104.0(8) . . ?
C38A N27 C37A 102.5(8) . . ?
C38A N27 C43 129.3(6) . . ?
C38 N27 C43 128.4(6) . . ?
C37 N27 C43 127.5(7) . . ?
C37A N27 C43 127.7(7) . . ?
C37 N25 N26 103.9(9) . . ?
N25 C37 N27 113.2(10) . . ?
N25 C37 H37A 123.4 . . ?
N27 C37 H37A 123.4 . . ?
N26 C38 H38A 125.6 . . ?
N27 C38 H38A 125.2 . . ?
C37A N25A N26 101.0(9) . . ?
N25A C37A N27 115.7(10) . . ?
N25A C37A H37B 122.2 . . ?
N27 C37A H37B 122.2 . . ?
N26 C38A N27 109.7(7) . . ?
N26 C38A H38B 125.5 . . ?
N27 C38A H38B 124.9 . . ?
N1 C1 N3 110.7(5) . . ?
N1 C1 H1 124.6 . . ?
N3 C1 H1 124.6 . . ?
N2 C2 N3 111.5(5) . . ?
N2 C2 H2 124.3 . . ?
N3 C2 H2 124.3 . . ?
N4 C3 N6 112.1(5) . . ?
N4 C3 H3 124.0 . . ?
N6 C3 H3 124.0 . . ?
N5 C4 N6 109.9(5) . . ?
N5 C4 H4 125.0 . . ?
N6 C4 H4 125.0 . . ?
N7 C5 N9 109.2(7) . . ?
N7 C5 H5 125.4 . . ?
N9 C5 H5 125.4 . . ?
N8 C6 N9 114.6(7) . . ?
N8 C6 H6 122.7 . . ?
N9 C6 H6 122.7 . . ?
N3 C7 C13 112.4(5) . . ?
N3 C7 C8 108.3(4) . . ?
C13 C7 C8 110.5(5) . . ?
N3 C7 C12 106.3(5) . . ?
C13 C7 C12 110.8(5) . . ?
C8 C7 C12 108.4(5) . . ?
C9 C8 C7 108.4(4) . . ?
C9 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 N6 108.4(5) . . ?
C10 C9 C8 111.0(5) . . ?
N6 C9 C8 110.0(4) . . ?
C10 C9 C15 109.9(5) . . ?
N6 C9 C15 108.1(5) . . ?
C8 C9 C15 109.3(5) . . ?
C9 C10 C11 109.1(5) . . ?
C9 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
N9 C11 C16 109.6(5) . . ?
N9 C11 C12 108.8(5) . . ?
C16 C11 C12 110.8(6) . . ?
N9 C11 C10 108.2(5) . . ?
C16 C11 C10 109.8(5) . . ?
C12 C11 C10 109.6(4) . . ?
C11 C12 C7 108.2(5) . . ?
C11 C12 H12A 110.1 . . ?
C7 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
C7 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
C7 C13 C14 108.7(6) . . ?
C7 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C7 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C15 C14 C16 109.9(5) . . ?
C15 C14 C13 108.9(5) . . ?
C16 C14 C13 111.0(5) . . ?
C15 C14 H14 109.0 . . ?
C16 C14 H14 109.0 . . ?
C13 C14 H14 109.0 . . ?
C14 C15 C9 108.0(5) . . ?
C14 C15 H15A 110.1 . . ?
C9 C15 H15A 110.1 . . ?
C14 C15 H15B 110.1 . . ?
C9 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
C11 C16 C14 108.2(5) . . ?
C11 C16 H16A 110.1 . . ?
C14 C16 H16A 110.1 . . ?
C11 C16 H16B 110.1 . . ?
C14 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
N10 C17 N12 111.5(5) . . ?
N10 C17 H17 124.3 . . ?
N12 C17 H17 124.3 . . ?
N11 C18 N12 110.0(5) . . ?
N11 C18 H18 125.0 . . ?
N12 C18 H18 125.0 . . ?
N13 C19 N15 109.0(5) . . ?
N13 C19 H19 125.5 . . ?
N15 C19 H19 125.5 . . ?
N14 C20 N15 110.0(5) . . ?
N14 C20 H20 125.0 . . ?
N15 C20 H20 125.0 . . ?
N18 C21 N16 114.3(7) . . ?
N18 C21 H21 122.9 . . ?
N16 C21 H21 122.9 . . ?
N17 C22 N18 109.5(6) . . ?
N17 C22 H22 125.3 . . ?
N18 C22 H22 125.3 . . ?
N12 C23 C28 108.9(5) . . ?
N12 C23 C24 108.1(4) . . ?
C28 C23 C24 110.5(5) . . ?
N12 C23 C29 109.0(5) . . ?
C28 C23 C29 111.9(5) . . ?
C24 C23 C29 108.3(5) . . ?
C25 C24 C23 108.5(4) . . ?
C25 C24 H24A 110.0 . . ?
C23 C24 H24A 110.0 . . ?
C25 C24 H24B 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
N15 C25 C31 109.8(5) . . ?
N15 C25 C26 108.8(5) . . ?
C31 C25 C26 110.0(5) . . ?
N15 C25 C24 109.3(4) . . ?
C31 C25 C24 109.4(5) . . ?
C26 C25 C24 109.5(5) . . ?
C27 C26 C25 109.4(5) . . ?
C27 C26 H26A 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
N18 C27 C26 109.5(5) . . ?
N18 C27 C28 109.9(5) . . ?
C26 C27 C28 110.3(5) . . ?
N18 C27 C32 110.0(5) . . ?
C26 C27 C32 109.2(5) . . ?
C28 C27 C32 107.9(5) . . ?
C23 C28 C27 110.0(5) . . ?
C23 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
C23 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C23 C29 C30 106.3(5) . . ?
C23 C29 H29A 110.5 . . ?
C30 C29 H29A 110.5 . . ?
C23 C29 H29B 110.5 . . ?
C30 C29 H29B 110.5 . . ?
H29A C29 H29B 108.7 . . ?
C32 C30 C31 110.6(6) . . ?
C32 C30 C29 111.3(5) . . ?
C31 C30 C29 108.1(5) . . ?
C32 C30 H30 108.9 . . ?
C31 C30 H30 108.9 . . ?
C29 C30 H30 108.9 . . ?
C25 C31 C30 109.4(5) . . ?
C25 C31 H31A 109.8 . . ?
C30 C31 H31A 109.8 . . ?
C25 C31 H31B 109.8 . . ?
C30 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
C30 C32 C27 109.6(5) . . ?
C30 C32 H32A 109.7 . . ?
C27 C32 H32A 109.7 . . ?
C30 C32 H32B 109.7 . . ?
C27 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
N19 C33 N21 109.4(5) . . ?
N19 C33 H33 125.3 . . ?
N21 C33 H33 125.3 . . ?
N20 C34 N21 109.8(5) . . ?
N20 C34 H34 125.1 . . ?
N21 C34 H34 125.1 . . ?
N22 C35 N24 110.8(5) . . ?
N22 C35 H35 124.6 . . ?
N24 C35 H35 124.6 . . ?
N23 C36 N24 110.4(5) . . ?
N23 C36 H36 124.8 . . ?
N24 C36 H36 124.8 . . ?
N21 C39 C40 109.1(4) . . ?
N21 C39 C45 110.0(5) . . ?
C40 C39 C45 110.6(5) . . ?
N21 C39 C44 105.9(5) . . ?
C40 C39 C44 110.0(5) . . ?
C45 C39 C44 111.3(5) . . ?
C41 C40 C39 108.2(4) . . ?
C41 C40 H40A 110.1 . . ?
C39 C40 H40A 110.1 . . ?
C41 C40 H40B 110.1 . . ?
C39 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?
N24 C41 C42 108.0(5) . . ?
N24 C41 C47 109.3(5) . . ?
C42 C41 C47 110.4(5) . . ?
N24 C41 C40 109.7(4) . . ?
C42 C41 C40 109.4(5) . . ?
C47 C41 C40 110.0(6) . . ?
C43 C42 C41 109.7(5) . . ?
C43 C42 H42A 109.7 . . ?
C41 C42 H42A 109.7 . . ?
C43 C42 H42B 109.7 . . ?
C41 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
N27 C43 C48 109.3(5) . . ?
N27 C43 C42 109.4(5) . . ?
C48 C43 C42 111.1(5) . . ?
N27 C43 C44 107.1(5) . . ?
C48 C43 C44 110.4(6) . . ?
C42 C43 C44 109.3(5) . . ?
C39 C44 C43 106.6(5) . . ?
C39 C44 H44A 110.4 . . ?
C43 C44 H44A 110.4 . . ?
C39 C44 H44B 110.4 . . ?
C43 C44 H44B 110.4 . . ?
H44A C44 H44B 108.6 . . ?
C46 C45 C39 108.4(6) . . ?
C46 C45 H45A 110.0 . . ?
C39 C45 H45A 110.0 . . ?
C46 C45 H45B 110.0 . . ?
C39 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
C45 C46 C47 109.5(5) . . ?
C45 C46 C48 108.5(5) . . ?
C47 C46 C48 108.7(6) . . ?
C45 C46 H46 110.0 . . ?
C47 C46 H46 110.0 . . ?
C48 C46 H46 110.0 . . ?
C41 C47 C46 109.2(5) . . ?
C41 C47 H47A 109.8 . . ?
C46 C47 H47A 109.8 . . ?
C41 C47 H47B 109.8 . . ?
C46 C47 H47B 109.8 . . ?
H47A C47 H47B 108.3 . . ?
C43 C48 C46 109.1(5) . . ?
C43 C48 H48A 109.9 . . ?
C46 C48 H48A 109.9 . . ?
C43 C48 H48B 109.9 . . ?
C46 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?

loop_
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_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Cu3 O1 Cu2 -163.8(3) . . . . ?
N20 Cu3 O1 Cu2 22.4(3) . . . . ?
O5 Cu3 O1 Cu2 -64.9(2) . . . . ?
O23 Cu3 O1 Cu2 107.8(3) . . . . ?
N2 Cu3 O1 Cu1 -30.0(2) . . . . ?
N20 Cu3 O1 Cu1 156.1(2) . . . . ?
O5 Cu3 O1 Cu1 68.8(2) . . . . ?
O23 Cu3 O1 Cu1 -118.4(3) . . . . ?
N19 Cu2 O1 Cu3 -21.0(3) . . . . ?
N11 Cu2 O1 Cu3 159.8(3) . . . . ?
O4 Cu2 O1 Cu3 69.6(2) . . . . ?
N19 Cu2 O1 Cu1 -154.8(3) . . . . ?
N11 Cu2 O1 Cu1 25.9(3) . . . . ?
O4 Cu2 O1 Cu1 -64.2(2) . . . . ?
N1 Cu1 O1 Cu3 32.1(2) . . . . ?
N10 Cu1 O1 Cu3 -158.3(2) . . . . ?
O3 Cu1 O1 Cu3 -66.3(2) . . . . ?
N1 Cu1 O1 Cu2 166.2(3) . . . . ?
N10 Cu1 O1 Cu2 -24.2(3) . . . . ?
O3 Cu1 O1 Cu2 67.8(2) . . . . ?
N4 Cu4 O2 Cu5 173.1(2) 3_445 . . . ?
N22 Cu4 O2 Cu5 -38.4(3) . . . . ?
O19 Cu4 O2 Cu5 90.0(2) . . . . ?
N4 Cu4 O2 Cu6 41.4(2) 3_445 . . . ?
N22 Cu4 O2 Cu6 -170.2(3) . . . . ?
O19 Cu4 O2 Cu6 -41.7(2) . . . . ?
N23 Cu5 O2 Cu4 37.0(3) . . . . ?
N26 Cu5 O2 Cu4 -49.1(8) 5_666 . . . ?
N13 Cu5 O2 Cu4 -143.0(3) 3_455 . . . ?
O24 Cu5 O2 Cu4 130.4(2) . . . . ?
O20 Cu5 O2 Cu4 -50.9(3) . . . . ?
N23 Cu5 O2 Cu6 164.3(3) . . . . ?
N26 Cu5 O2 Cu6 78.2(7) 5_666 . . . ?
N13 Cu5 O2 Cu6 -15.7(3) 3_455 . . . ?
O24 Cu5 O2 Cu6 -102.3(2) . . . . ?
O20 Cu5 O2 Cu6 76.4(3) . . . . ?
N17 Cu6 O2 Cu4 55.8(6) 5_656 . . . ?
N14 Cu6 O2 Cu4 142.3(3) 3_455 . . . ?
N5 Cu6 O2 Cu4 -38.7(3) 3_445 . . . ?
O25 Cu6 O2 Cu4 -127.9(2) . . . . ?
N17 Cu6 O2 Cu5 -72.5(6) 5_656 . . . ?
N14 Cu6 O2 Cu5 13.9(3) 3_455 . . . ?
N5 Cu6 O2 Cu5 -167.0(3) 3_445 . . . ?
O25 Cu6 O2 Cu5 103.8(2) . . . . ?
O6 S1 O3 Cu1 -175.7(3) . . . . ?
O5 S1 O3 Cu1 64.0(4) . . . . ?
O4 S1 O3 Cu1 -55.2(4) . . . . ?
O7 Cu1 O3 S1 175.9(3) . . . . ?
N1 Cu1 O3 S1 -92.6(3) . . . . ?
N10 Cu1 O3 S1 84.4(3) . . . . ?
O1 Cu1 O3 S1 -5.2(3) . . . . ?
O6 S1 O4 Cu2 -175.4(3) . . . . ?
O5 S1 O4 Cu2 -53.9(4) . . . . ?
O3 S1 O4 Cu2 63.6(4) . . . . ?
O11 Cu2 O4 S1 175.8(3) . . . . ?
N19 Cu2 O4 S1 83.8(3) . . . . ?
N11 Cu2 O4 S1 -95.3(3) . . . . ?
O1 Cu2 O4 S1 -5.8(3) . . . . ?
O6 S1 O5 Cu3 -179.8(3) . . . . ?
O4 S1 O5 Cu3 59.0(3) . . . . ?
O3 S1 O5 Cu3 -59.3(4) . . . . ?
O15 Cu3 O5 S1 177.0(3) . . . . ?
N2 Cu3 O5 S1 85.0(3) . . . . ?
N20 Cu3 O5 S1 -92.2(3) . . . . ?
O1 Cu3 O5 S1 -2.7(3) . . . . ?
O9A S2 O7 Cu1 -114.3(7) . . . . ?
O10A S2 O7 Cu1 120.1(6) . . . . ?
O8A S2 O7 Cu1 3.7(7) . . . . ?
O9 S2 O7 Cu1 -44.6(7) . . . . ?
O8 S2 O7 Cu1 82.5(6) . . . . ?
O10 S2 O7 Cu1 -163.2(5) . . . . ?
N1 Cu1 O7 S2 89.1(4) . . . . ?
N10 Cu1 O7 S2 -80.5(4) . . . . ?
O3 Cu1 O7 S2 -172.5(4) . . . . ?
O12 S3 O11 Cu2 -13.2(6) . . . . ?
O13 S3 O11 Cu2 -135.1(4) . . . . ?
O14 S3 O11 Cu2 105.5(4) . . . . ?
N19 Cu2 O11 S3 -84.4(4) . . . . ?
N11 Cu2 O11 S3 94.6(3) . . . . ?
O4 Cu2 O11 S3 -175.3(3) . . . . ?
O17A S4 O15 Cu3 103.2(7) . . . . ?
O16A S4 O15 Cu3 -124.2(7) . . . . ?
O18A S4 O15 Cu3 -11.8(7) . . . . ?
O17 S4 O15 Cu3 174.4(5) . . . . ?
O18 S4 O15 Cu3 53.5(7) . . . . ?
O16 S4 O15 Cu3 -66.0(6) . . . . ?
N2 Cu3 O15 S4 -81.8(5) . . . . ?
N20 Cu3 O15 S4 92.1(5) . . . . ?
O5 Cu3 O15 S4 179.4(5) . . . . ?
O23 Cu3 O15 S4 6.6(5) . . . . ?
O20 S5 O19 Cu4 34.4(6) . . . . ?
O21 S5 O19 Cu4 -91.5(5) . . . . ?
O22 S5 O19 Cu4 153.8(5) . . . . ?
N7 Cu4 O19 S5 90.8(4) 7_656 . . . ?
O2 Cu4 O19 S5 -87.9(4) . . . . ?
N4 Cu4 O19 S5 -177.7(4) 3_445 . . . ?
N22 Cu4 O19 S5 -5.4(5) . . . . ?
O21 S5 O20 Cu5 144.4(7) . . . . ?
O22 S5 O20 Cu5 -96.1(9) . . . . ?
O19 S5 O20 Cu5 21.4(10) . . . . ?
N23 Cu5 O20 S5 -105.7(9) . . . . ?
O2 Cu5 O20 S5 -16.9(9) . . . . ?
N26 Cu5 O20 S5 163.5(9) 5_666 . . . ?
N13 Cu5 O20 S5 72.5(9) 3_455 . . . ?
O7 Cu1 N1 C1 -23.2(7) . . . . ?
N10 Cu1 N1 C1 82.5(13) . . . . ?
O1 Cu1 N1 C1 156.6(7) . . . . ?
O3 Cu1 N1 C1 -113.6(7) . . . . ?
O7 Cu1 N1 N2 157.4(5) . . . . ?
N10 Cu1 N1 N2 -96.8(11) . . . . ?
O1 Cu1 N1 N2 -22.7(5) . . . . ?
O3 Cu1 N1 N2 67.1(5) . . . . ?
C1 N1 N2 C2 -1.9(7) . . . . ?
Cu1 N1 N2 C2 177.6(5) . . . . ?
C1 N1 N2 Cu3 -173.8(5) . . . . ?
Cu1 N1 N2 Cu3 5.7(6) . . . . ?
O15 Cu3 N2 C2 25.6(7) . . . . ?
O1 Cu3 N2 C2 -154.5(6) . . . . ?
O5 Cu3 N2 C2 116.8(6) . . . . ?
O23 Cu3 N2 C2 -64.0(7) . . . . ?
O15 Cu3 N2 N1 -164.8(5) . . . . ?
O1 Cu3 N2 N1 15.1(5) . . . . ?
O5 Cu3 N2 N1 -73.6(5) . . . . ?
O23 Cu3 N2 N1 105.5(5) . . . . ?
C3 N4 N5 C4 -0.2(8) . . . . ?
Cu4 N4 N5 C4 -168.6(5) 3 . . . ?
C3 N4 N5 Cu6 175.1(5) . . . 3 ?
Cu4 N4 N5 Cu6 6.6(6) 3 . . 3 ?
C5 N7 N8 C6 -1.2(7) . . . . ?
Cu4 N7 N8 C6 177.5(4) 7_656 . . . ?
O7 Cu1 N10 C17 9.4(7) . . . . ?
N1 Cu1 N10 C17 -96.4(12) . . . . ?
O1 Cu1 N10 C17 -170.3(7) . . . . ?
O3 Cu1 N10 C17 99.6(7) . . . . ?
O7 Cu1 N10 N11 -168.3(5) . . . . ?
N1 Cu1 N10 N11 85.9(11) . . . . ?
O1 Cu1 N10 N11 12.1(5) . . . . ?
O3 Cu1 N10 N11 -78.1(5) . . . . ?
C17 N10 N11 C18 -1.3(7) . . . . ?
Cu1 N10 N11 C18 177.0(5) . . . . ?
C17 N10 N11 Cu2 -173.3(5) . . . . ?
Cu1 N10 N11 Cu2 4.9(7) . . . . ?
O11 Cu2 N11 C18 -0.8(7) . . . . ?
O1 Cu2 N11 C18 171.2(7) . . . . ?
O4 Cu2 N11 C18 -97.7(7) . . . . ?
O11 Cu2 N11 N10 169.1(5) . . . . ?
O1 Cu2 N11 N10 -19.0(5) . . . . ?
O4 Cu2 N11 N10 72.1(5) . . . . ?
C19 N13 N14 C20 3.2(8) . . . . ?
Cu5 N13 N14 C20 -176.8(5) 3_545 . . . ?
C19 N13 N14 Cu6 175.0(5) . . . 3_545 ?
Cu5 N13 N14 Cu6 -5.0(7) 3_545 . . 3_545 ?
C21 N16 N17 C22 -0.5(8) . . . . ?
C21 N16 N17 Cu6 174.6(5) . . . 5_656 ?
O11 Cu2 N19 C33 0.3(7) . . . . ?
O1 Cu2 N19 C33 -171.7(7) . . . . ?
O4 Cu2 N19 C33 97.3(7) . . . . ?
O11 Cu2 N19 N20 -177.3(5) . . . . ?
O1 Cu2 N19 N20 10.8(5) . . . . ?
O4 Cu2 N19 N20 -80.3(5) . . . . ?
C33 N19 N20 C34 -1.6(8) . . . . ?
Cu2 N19 N20 C34 176.5(5) . . . . ?
C33 N19 N20 Cu3 -174.3(5) . . . . ?
Cu2 N19 N20 Cu3 3.8(7) . . . . ?
O15 Cu3 N20 C34 -6.6(6) . . . . ?
O1 Cu3 N20 C34 173.5(6) . . . . ?
O5 Cu3 N20 C34 -97.5(6) . . . . ?
O23 Cu3 N20 C34 83.0(7) . . . . ?
O15 Cu3 N20 N19 163.9(5) . . . . ?
O1 Cu3 N20 N19 -16.0(5) . . . . ?
O5 Cu3 N20 N19 73.1(5) . . . . ?
O23 Cu3 N20 N19 -106.4(6) . . . . ?
N7 Cu4 N22 C35 21.2(8) 7_656 . . . ?
O2 Cu4 N22 C35 -161.1(8) . . . . ?
N4 Cu4 N22 C35 -76.1(9) 3_445 . . . ?
O19 Cu4 N22 C35 118.7(8) . . . . ?
N7 Cu4 N22 N23 -151.9(5) 7_656 . . . ?
O2 Cu4 N22 N23 25.7(5) . . . . ?
N4 Cu4 N22 N23 110.8(5) 3_445 . . . ?
O19 Cu4 N22 N23 -54.5(6) . . . . ?
C35 N22 N23 C36 0.2(8) . . . . ?
Cu4 N22 N23 C36 175.2(5) . . . . ?
C35 N22 N23 Cu5 -179.1(5) . . . . ?
Cu4 N22 N23 Cu5 -4.0(7) . . . . ?
O2 Cu5 N23 C36 161.0(7) . . . . ?
N26 Cu5 N23 C36 -32.4(7) 5_666 . . . ?
O24 Cu5 N23 C36 67.0(7) . . . . ?
O20 Cu5 N23 C36 -114.5(7) . . . . ?
O2 Cu5 N23 N22 -20.0(5) . . . . ?
N26 Cu5 N23 N22 146.6(5) 5_666 . . . ?
O24 Cu5 N23 N22 -114.0(5) . . . . ?
O20 Cu5 N23 N22 64.6(5) . . . . ?
C38A N26 N25 C37 -18.8(5) . . . . ?
C38 N26 N25 C37 -1.0(5) . . . . ?
Cu5 N26 N25 C37 -174.9(4) 5_666 . . . ?
N26 N25 C37 N27 0.3(3) . . . . ?
C38A N27 C37 N25 17.3(5) . . . . ?
C38 N27 C37 N25 0.4(3) . . . . ?
C37A N27 C37 N25 -81.9(16) . . . . ?
C43 N27 C37 N25 176.0(5) . . . . ?
C38A N26 C38 N27 76.8(12) . . . . ?
N25 N26 C38 N27 1.3(6) . . . . ?
N25A N26 C38 N27 -31.2(7) . . . . ?
Cu5 N26 C38 N27 175.0(4) 5_666 . . . ?
C38A N27 C38 N26 -76.6(12) . . . . ?
C37 N27 C38 N26 -1.0(5) . . . . ?
C37A N27 C38 N26 28.7(7) . . . . ?
C43 N27 C38 N26 -176.5(6) . . . . ?
C38A N26 N25A C37A 0.2(5) . . . . ?
C38 N26 N25A C37A 18.3(5) . . . . ?
N25 N26 N25A C37A -82.5(14) . . . . ?
Cu5 N26 N25A C37A 173.8(4) 5_666 . . . ?
N26 N25A C37A N27 0.0(3) . . . . ?
C38A N27 C37A N25A -0.1(3) . . . . ?
C38 N27 C37A N25A -17.2(5) . . . . ?
C37 N27 C37A N25A 86.4(16) . . . . ?
C43 N27 C37A N25A -172.2(5) . . . . ?
C38 N26 C38A N27 -78.2(12) . . . . ?
N25 N26 C38A N27 31.5(7) . . . . ?
N25A N26 C38A N27 -0.3(6) . . . . ?
Cu5 N26 C38A N27 -173.5(4) 5_666 . . . ?
C38 N27 C38A N26 78.0(12) . . . . ?
C37 N27 C38A N26 -29.8(7) . . . . ?
C37A N27 C38A N26 0.2(5) . . . . ?
C43 N27 C38A N26 172.1(5) . . . . ?
N2 N1 C1 N3 1.5(7) . . . . ?
Cu1 N1 C1 N3 -177.9(5) . . . . ?
C2 N3 C1 N1 -0.6(7) . . . . ?
C7 N3 C1 N1 175.9(6) . . . . ?
N1 N2 C2 N3 1.6(8) . . . . ?
Cu3 N2 C2 N3 172.2(5) . . . . ?
C1 N3 C2 N2 -0.7(8) . . . . ?
C7 N3 C2 N2 -177.0(6) . . . . ?
N5 N4 C3 N6 1.1(8) . . . . ?
Cu4 N4 C3 N6 165.3(5) 3 . . . ?
C4 N6 C3 N4 -1.6(8) . . . . ?
C9 N6 C3 N4 -175.5(6) . . . . ?
N4 N5 C4 N6 -0.8(8) . . . . ?
Cu6 N5 C4 N6 -175.2(5) 3 . . . ?
C3 N6 C4 N5 1.4(8) . . . . ?
C9 N6 C4 N5 175.1(6) . . . . ?
N8 N7 C5 N9 0.9(7) . . . . ?
Cu4 N7 C5 N9 -177.7(4) 7_656 . . . ?
C6 N9 C5 N7 -0.2(7) . . . . ?
C11 N9 C5 N7 179.3(5) . . . . ?
N7 N8 C6 N9 1.1(7) . . . . ?
C5 N9 C6 N8 -0.6(7) . . . . ?
C11 N9 C6 N8 179.9(5) . . . . ?
C2 N3 C7 C13 -121.4(7) . . . . ?
C1 N3 C7 C13 63.0(8) . . . . ?
C2 N3 C7 C8 0.9(9) . . . . ?
C1 N3 C7 C8 -174.7(6) . . . . ?
C2 N3 C7 C12 117.2(7) . . . . ?
C1 N3 C7 C12 -58.4(8) . . . . ?
N3 C7 C8 C9 175.7(6) . . . . ?
C13 C7 C8 C9 -60.9(7) . . . . ?
C12 C7 C8 C9 60.7(7) . . . . ?
C3 N6 C9 C10 55.6(8) . . . . ?
C4 N6 C9 C10 -116.8(7) . . . . ?
C3 N6 C9 C8 177.2(7) . . . . ?
C4 N6 C9 C8 4.8(10) . . . . ?
C3 N6 C9 C15 -63.5(8) . . . . ?
C4 N6 C9 C15 124.1(7) . . . . ?
C7 C8 C9 C10 -61.1(7) . . . . ?
C7 C8 C9 N6 178.9(5) . . . . ?
C7 C8 C9 C15 60.4(7) . . . . ?
N6 C9 C10 C11 -178.9(4) . . . . ?
C8 C9 C10 C11 60.2(6) . . . . ?
C15 C9 C10 C11 -60.9(6) . . . . ?
C6 N9 C11 C16 179.0(6) . . . . ?
C5 N9 C11 C16 -0.4(8) . . . . ?
C6 N9 C11 C12 -59.7(8) . . . . ?
C5 N9 C11 C12 120.9(6) . . . . ?
C6 N9 C11 C10 59.3(7) . . . . ?
C5 N9 C11 C10 -120.1(6) . . . . ?
C9 C10 C11 N9 -178.9(5) . . . . ?
C9 C10 C11 C16 61.5(6) . . . . ?
C9 C10 C11 C12 -60.4(7) . . . . ?
N9 C11 C12 C7 179.2(5) . . . . ?
C16 C11 C12 C7 -60.2(6) . . . . ?
C10 C11 C12 C7 61.1(7) . . . . ?
N3 C7 C12 C11 -177.9(5) . . . . ?
C13 C7 C12 C11 59.7(6) . . . . ?
C8 C7 C12 C11 -61.7(6) . . . . ?
N3 C7 C13 C14 -177.7(5) . . . . ?
C8 C7 C13 C14 61.3(7) . . . . ?
C12 C7 C13 C14 -58.9(6) . . . . ?
C7 C13 C14 C15 -61.8(7) . . . . ?
C7 C13 C14 C16 59.3(7) . . . . ?
C16 C14 C15 C9 -60.2(6) . . . . ?
C13 C14 C15 C9 61.6(7) . . . . ?
C10 C9 C15 C14 60.5(6) . . . . ?
N6 C9 C15 C14 178.7(4) . . . . ?
C8 C9 C15 C14 -61.6(6) . . . . ?
N9 C11 C16 C14 -179.4(4) . . . . ?
C12 C11 C16 C14 60.5(6) . . . . ?
C10 C11 C16 C14 -60.7(6) . . . . ?
C15 C14 C16 C11 61.0(6) . . . . ?
C13 C14 C16 C11 -59.5(6) . . . . ?
N11 N10 C17 N12 2.2(8) . . . . ?
Cu1 N10 C17 N12 -175.6(5) . . . . ?
C18 N12 C17 N10 -2.3(8) . . . . ?
C23 N12 C17 N10 179.4(6) . . . . ?
N10 N11 C18 N12 -0.2(8) . . . . ?
Cu2 N11 C18 N12 170.7(5) . . . . ?
C17 N12 C18 N11 1.5(8) . . . . ?
C23 N12 C18 N11 179.8(6) . . . . ?
N14 N13 C19 N15 -4.0(8) . . . . ?
Cu5 N13 C19 N15 176.0(5) 3_545 . . . ?
C20 N15 C19 N13 3.3(8) . . . . ?
C25 N15 C19 N13 -179.2(7) . . . . ?
N13 N14 C20 N15 -1.0(8) . . . . ?
Cu6 N14 C20 N15 -171.5(5) 3_545 . . . ?
C19 N15 C20 N14 -1.4(8) . . . . ?
C25 N15 C20 N14 -178.9(6) . . . . ?
C22 N18 C21 N16 -0.3(9) . . . . ?
C27 N18 C21 N16 179.1(6) . . . . ?
N17 N16 C21 N18 0.5(9) . . . . ?
N16 N17 C22 N18 0.3(7) . . . . ?
Cu6 N17 C22 N18 -174.5(4) 5_656 . . . ?
C21 N18 C22 N17 0.0(7) . . . . ?
C27 N18 C22 N17 -179.4(5) . . . . ?
C18 N12 C23 C28 -47.2(8) . . . . ?
C17 N12 C23 C28 130.7(7) . . . . ?
C18 N12 C23 C24 -167.3(6) . . . . ?
C17 N12 C23 C24 10.6(10) . . . . ?
C18 N12 C23 C29 75.1(8) . . . . ?
C17 N12 C23 C29 -107.0(8) . . . . ?
N12 C23 C24 C25 179.1(5) . . . . ?
C28 C23 C24 C25 60.1(7) . . . . ?
C29 C23 C24 C25 -62.8(7) . . . . ?
C20 N15 C25 C31 -55.6(9) . . . . ?
C19 N15 C25 C31 127.4(7) . . . . ?
C20 N15 C25 C26 64.9(8) . . . . ?
C19 N15 C25 C26 -112.1(7) . . . . ?
C20 N15 C25 C24 -175.6(6) . . . . ?
C19 N15 C25 C24 7.5(9) . . . . ?
C23 C24 C25 N15 -179.0(6) . . . . ?
C23 C24 C25 C31 60.8(7) . . . . ?
C23 C24 C25 C26 -59.8(7) . . . . ?
N15 C25 C26 C27 179.3(4) . . . . ?
C31 C25 C26 C27 -60.4(6) . . . . ?
C24 C25 C26 C27 59.9(6) . . . . ?
C21 N18 C27 C26 65.7(8) . . . . ?
C22 N18 C27 C26 -115.0(6) . . . . ?
C21 N18 C27 C28 -55.6(8) . . . . ?
C22 N18 C27 C28 123.7(6) . . . . ?
C21 N18 C27 C32 -174.3(6) . . . . ?
C22 N18 C27 C32 5.0(8) . . . . ?
C25 C26 C27 N18 -179.7(5) . . . . ?
C25 C26 C27 C28 -58.6(7) . . . . ?
C25 C26 C27 C32 59.8(6) . . . . ?
N12 C23 C28 C27 -177.9(4) . . . . ?
C24 C23 C28 C27 -59.3(6) . . . . ?
C29 C23 C28 C27 61.5(6) . . . . ?
N18 C27 C28 C23 179.5(5) . . . . ?
C26 C27 C28 C23 58.7(7) . . . . ?
C32 C27 C28 C23 -60.6(6) . . . . ?
N12 C23 C29 C30 -178.5(5) . . . . ?
C28 C23 C29 C30 -58.0(6) . . . . ?
C24 C23 C29 C30 64.0(7) . . . . ?
C23 C29 C30 C32 57.8(7) . . . . ?
C23 C29 C30 C31 -63.8(7) . . . . ?
N15 C25 C31 C30 178.8(5) . . . . ?
C26 C25 C31 C30 59.0(6) . . . . ?
C24 C25 C31 C30 -61.4(7) . . . . ?
C32 C30 C31 C25 -58.8(7) . . . . ?
C29 C30 C31 C25 63.2(7) . . . . ?
C31 C30 C32 C27 58.9(6) . . . . ?
C29 C30 C32 C27 -61.2(6) . . . . ?
N18 C27 C32 C30 -179.6(4) . . . . ?
C26 C27 C32 C30 -59.4(6) . . . . ?
C28 C27 C32 C30 60.5(6) . . . . ?
N20 N19 C33 N21 0.6(8) . . . . ?
Cu2 N19 C33 N21 -177.3(5) . . . . ?
C34 N21 C33 N19 0.6(8) . . . . ?
C39 N21 C33 N19 -179.5(6) . . . . ?
N19 N20 C34 N21 2.0(8) . . . . ?
Cu3 N20 C34 N21 173.4(5) . . . . ?
C33 N21 C34 N20 -1.6(8) . . . . ?
C39 N21 C34 N20 178.4(6) . . . . ?
N23 N22 C35 N24 -0.9(8) . . . . ?
Cu4 N22 C35 N24 -174.4(6) . . . . ?
C36 N24 C35 N22 1.2(9) . . . . ?
C41 N24 C35 N22 173.7(7) . . . . ?
N22 N23 C36 N24 0.6(8) . . . . ?
Cu5 N23 C36 N24 179.7(5) . . . . ?
C35 N24 C36 N23 -1.1(8) . . . . ?
C41 N24 C36 N23 -174.2(6) . . . . ?
C33 N21 C39 C40 -11.6(9) . . . . ?
C34 N21 C39 C40 168.3(6) . . . . ?
C33 N21 C39 C45 -133.0(7) . . . . ?
C34 N21 C39 C45 46.9(8) . . . . ?
C33 N21 C39 C44 106.7(7) . . . . ?
C34 N21 C39 C44 -73.4(8) . . . . ?
N21 C39 C40 C41 177.8(6) . . . . ?
C45 C39 C40 C41 -61.2(7) . . . . ?
C44 C39 C40 C41 62.1(7) . . . . ?
C36 N24 C41 C42 66.6(8) . . . . ?
C35 N24 C41 C42 -104.6(8) . . . . ?
C36 N24 C41 C47 -53.7(9) . . . . ?
C35 N24 C41 C47 135.2(7) . . . . ?
C36 N24 C41 C40 -174.3(7) . . . . ?
C35 N24 C41 C40 14.5(10) . . . . ?
C39 C40 C41 N24 -178.8(6) . . . . ?
C39 C40 C41 C42 -60.5(7) . . . . ?
C39 C40 C41 C47 60.9(7) . . . . ?
N24 C41 C42 C43 -179.4(5) . . . . ?
C47 C41 C42 C43 -59.9(6) . . . . ?
C40 C41 C42 C43 61.3(7) . . . . ?
C38A N27 C43 C48 -9.0(8) . . . . ?
C38 N27 C43 C48 13.2(8) . . . . ?
C37 N27 C43 C48 -161.3(6) . . . . ?
C37A N27 C43 C48 161.0(6) . . . . ?
C38A N27 C43 C42 -130.9(7) . . . . ?
C38 N27 C43 C42 -108.7(7) . . . . ?
C37 N27 C43 C42 76.8(7) . . . . ?
C37A N27 C43 C42 39.1(8) . . . . ?
C38A N27 C43 C44 110.7(7) . . . . ?
C38 N27 C43 C44 132.9(6) . . . . ?
C37 N27 C43 C44 -41.6(8) . . . . ?
C37A N27 C43 C44 -79.3(7) . . . . ?
C41 C42 C43 N27 -179.0(5) . . . . ?
C41 C42 C43 C48 60.2(7) . . . . ?
C41 C42 C43 C44 -62.0(7) . . . . ?
N21 C39 C44 C43 -179.5(5) . . . . ?
C40 C39 C44 C43 -61.9(6) . . . . ?
C45 C39 C44 C43 61.0(6) . . . . ?
N27 C43 C44 C39 179.7(5) . . . . ?
C48 C43 C44 C39 -61.3(6) . . . . ?
C42 C43 C44 C39 61.3(7) . . . . ?
N21 C39 C45 C46 -178.8(5) . . . . ?
C40 C39 C45 C46 60.7(7) . . . . ?
C44 C39 C45 C46 -61.8(6) . . . . ?
C39 C45 C46 C47 -59.2(7) . . . . ?
C39 C45 C46 C48 59.3(6) . . . . ?
N24 C41 C47 C46 178.8(5) . . . . ?
C42 C41 C47 C46 60.1(6) . . . . ?
C40 C41 C47 C46 -60.7(7) . . . . ?
C45 C46 C47 C41 59.8(8) . . . . ?
C48 C46 C47 C41 -58.6(6) . . . . ?
N27 C43 C48 C46 179.8(4) . . . . ?
C42 C43 C48 C46 -59.4(6) . . . . ?
C44 C43 C48 C46 62.1(6) . . . . ?
C45 C46 C48 C43 -60.6(6) . . . . ?
C47 C46 C48 C43 58.4(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.118

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.287 0.250 812 212 ' '
2 0.500 0.787 0.250 812 212 ' '
3 0.000 0.713 0.750 813 213 ' '
4 0.500 0.213 0.750 813 213 ' '
_platon_squeeze_details          
;
;

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL C2c in C2/c
CELL 0.71073 38.1357 22.2267 27.8475 90.000 119.357 90.000
ZERR 8.00 0.0013 0.0004 0.0011 0.000 0.006 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H N O S CU
UNIT 384 936 216 408 40 48
MERG 2
OMIT 0.00 180.00
OMIT 0 8 0
OMIT -8 2 8
OMIT -3 5 6
OMIT -4 6 2
OMIT -4 6 5
OMIT -13 1 8
OMIT -10 0 2
OMIT 8 2 0
OMIT 2 0 6
OMIT -12 0 6
OMIT -3 7 7
OMIT -10 2 4
OMIT 9 3 0
OMIT -12 4 4
OMIT -3 9 5
OMIT -10 2 6
OMIT -11 3 1
OMIT -11 3 9
OMIT -20 2 4
OMIT -11 3 7
OMIT -3 7 1
OMIT -13 1 4
SHEL 0.78 4
EADP O16 > O18A
DFIX 1.480 0.005 S4 O16 S4 O17 S4 O18
DFIX 1.480 0.005 S4 O16A S4 O17A S4 O18A
DFIX 2.350 0.005 O16 O17 O17 O18 O16 O18
DFIX 2.350 0.005 O16A O17A O17A O18A O16A O18A
EADP O8 > O10A
DFIX 1.480 0.005 S2 O8 S2 O9 S2 O10
DFIX 1.480 0.005 S2 O8A S2 O9A S2 O10A
DFIX 2.350 0.005 O8 O9 O8 O10 O9 O10
DFIX 2.350 0.005 O8A O9A O8A O10A O9A O10A

EADP N25 C37 C38
EADP N25A C37A C38A

FLAT 0.01 N27 C37 N25 N26 C38
DFIX 1.363 0.005 N27 C37 N27 C38
DFIX 1.307 0.005 C37 N25 C38 N26
DFIX 1.389 0.005 N25 N26 N25A N26
FLAT 0.01 N27 C37A N25A N26 C38A
DFIX 1.363 0.005 N27 C37A N27 C38A
DFIX 1.307 0.005 C37A N25A C38A N26
BIND Cu3 O23
BIND Cu5 O20
EQIV $1 1-X, Y, 0.5-Z
EQIV $2 -0.5+X, 0.5+Y, Z
RTAB H..O H2W O6_$1
RTAB H..O H3W O5_$1
RTAB H..O H4W O6W_$2
RTAB H..O H5W O3W
RTAB H..O H6W O9W
RTAB O..O O2 O6_$1
RTAB O..O O24 O5_$1
RTAB O..O O24 O6W_$2
RTAB O..O O25 O3W
RTAB O..O O25 O9W
RTAB XHY O2 H2W O6_$1
RTAB XHY O24 H3W O5_$1
RTAB XHY O24 H4W O6W_$2
RTAB XHY O25 H5W O3W
RTAB XHY O25 H6W O9W
FMAP 2
PLAN 25
SIZE 0.19 0.25 0.26
ACTA
BOND
BOND $H
CONF
LIST 4
L.S. 5
TEMP -100.00
WGHT 0.073900
FVAR 0.31849 0.56472 0.53203
CU1 6 0.746074 0.201164 0.363132 11.00000 0.02237 0.01554 =
0.03798 -0.00165 0.02310 -0.00096
CU2 6 0.670211 0.213088 0.391489 11.00000 0.02422 0.01375 =
0.03834 0.00284 0.02524 0.00355
CU3 6 0.708333 0.337310 0.365189 11.00000 0.01950 0.01550 =
0.03818 0.00158 0.02074 0.00168
CU4 6 0.429470 0.213257 0.419615 11.00000 0.01537 0.01690 =
0.04282 0.00610 0.01111 0.00159
CU5 6 0.379522 0.337624 0.401050 11.00000 0.02109 0.01479 =
0.03660 -0.00810 0.02091 -0.00454
CU6 6 0.338240 0.201602 0.396048 11.00000 0.02325 0.01334 =
0.03251 0.00414 0.02265 0.00293
S1 5 0.653376 0.237697 0.265479 11.00000 0.02241 0.02587 =
0.01605 -0.00104 0.01179 -0.00306
S2 5 0.811987 0.119934 0.360944 11.00000 0.06208 0.05025 =
0.14068 -0.00879 0.06733 0.00078
S3 5 0.627737 0.162393 0.453801 11.00000 0.05075 0.05007 =
0.04402 0.00589 0.03203 0.00393
S4 5 0.713527 0.478417 0.359535 11.00000 0.07961 0.03751 =
0.13452 -0.00555 0.07462 -0.00061
S5 5 0.426975 0.247097 0.529872 11.00000 0.03515 0.03388 =
0.02643 -0.00165 0.01399 -0.00041
O1 4 0.717835 0.252684 0.393056 11.00000 0.01720 0.01762 =
0.01231 -0.00456 0.00907 -0.00061
AFIX 13
H1W 2 0.737715 0.256598 0.433174 11.00000 -1.50000
AFIX 0
O2 4 0.376052 0.251262 0.383381 11.00000 0.01409 0.01764 =
0.01046 0.00231 0.00759 0.00078
AFIX 13
H2W 2 0.366377 0.248970 0.342933 11.00000 -1.50000
AFIX 0
O3 4 0.691592 0.207689 0.276979 11.00000 0.02387 0.03081 =
0.03021 -0.00595 0.01554 0.00692
O4 4 0.638629 0.210048 0.300746 11.00000 0.02495 0.03641 =
0.03951 0.00387 0.02606 -0.00381
O5 4 0.662416 0.301908 0.279181 11.00000 0.02580 0.01827 =
0.03578 0.00424 0.01283 0.00483
O6 4 0.622939 0.230742 0.207266 11.00000 0.02524 0.05104 =
0.00802 0.00163 0.00666 -0.00674
O7 4 0.773957 0.152813 0.334403 11.00000 0.05309 0.03398 =
0.09650 -0.00199 0.06395 0.00836
PART 1
O8 4 0.809081 0.059446 0.381171 31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
O9 4 0.848499 0.147557 0.406148 31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
O10 4 0.822895 0.107561 0.317195 31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
PART 2
O8A 4 0.825564 0.127816 0.419402 -31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
O9A 4 0.841801 0.144120 0.348680 -31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
O10A 4 0.805170 0.056722 0.347461 -31.00000 0.06187 0.10168 =
0.11065 -0.03559 0.04950 0.00280
PART 0
O11 4 0.628602 0.172937 0.401293 11.00000 0.03083 0.02732 =
0.03152 0.00111 0.02470 0.00126
O12 4 0.667131 0.174194 0.499720 11.00000 0.06184 0.28717 =
0.05085 -0.00277 0.00125 0.00233
O13 4 0.615213 0.101216 0.453839 11.00000 0.14194 0.04652 =
0.10553 0.02192 0.09561 0.00595
O14 4 0.598804 0.204244 0.455754 11.00000 0.09345 0.06698 =
0.08005 0.00457 0.07323 0.01813
O15 4 0.699231 0.420343 0.337659 11.00000 0.06670 0.01263 =
0.11534 0.00214 0.06708 0.00123
PART 3
O16 4 0.701661 0.498064 0.400635 21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
O17 4 0.698088 0.524564 0.316409 21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
O18 4 0.757812 0.482715 0.388510 21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
PART 4
O16A 4 0.681917 0.520991 0.350924 -21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
O17A 4 0.742923 0.507285 0.348579 -21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
O18A 4 0.733554 0.460257 0.417530 -21.00000 0.10428 0.02977 =
0.16571 0.01743 0.09317 0.01239
PART 0
O19 4 0.415515 0.197281 0.487312 11.00000 0.08871 0.04587 =
0.05184 0.00734 0.01788 -0.00219
O20 4 0.421863 0.301557 0.503654 11.00000 0.19736 0.05115 =
0.10255 0.00888 0.03843 -0.02217
O21 4 0.467283 0.236559 0.575323 11.00000 0.05444 0.14413 =
0.07844 -0.03845 0.00322 0.02235
O22 4 0.399691 0.242465 0.553649 11.00000 0.13029 0.18919 =
0.12590 -0.03983 0.09671 -0.04268
O23 4 0.752549 0.377154 0.464777 11.00000 0.09076 0.35819 =
0.06186 -0.02342 0.01984 -0.05138
O24 4 0.340525 0.366901 0.309595 11.00000 0.07953 0.03364 =
0.03835 -0.00148 0.03306 0.00888
AFIX 3
H3W 2 0.339105 0.348859 0.281774 11.00000 -1.50000
H4W 2 0.331364 0.402339 0.299975 11.00000 -1.50000
AFIX 0
O25 4 0.289927 0.195143 0.305239 11.00000 0.02705 0.04395 =
0.02952 -0.00121 0.01340 0.00481
AFIX 3
H5W 2 0.277497 0.161733 0.297640 11.00000 -1.50000
H6W 2 0.272677 0.223343 0.294832 11.00000 -1.50000
AFIX 0
N1 3 0.774458 0.274618 0.360938 11.00000 0.01866 0.01844 =
0.01630 0.00083 0.01002 -0.00424
N2 3 0.757691 0.330451 0.358924 11.00000 0.01450 0.01826 =
0.02111 -0.00059 0.01144 -0.00065
N3 3 0.814903 0.344677 0.361118 11.00000 0.00939 0.01761 =
0.02259 0.00063 0.00943 -0.00294
N4 3 0.902353 0.631683 0.392845 11.00000 0.01506 0.02133 =
0.01740 0.00252 0.01180 -0.00059
N5 3 0.864477 0.627660 0.386766 11.00000 0.01996 0.01403 =
0.04276 0.00239 0.02024 0.00599
N6 3 0.883787 0.538055 0.379863 11.00000 0.01645 0.01508 =
0.02957 0.00990 0.01563 0.00542
N7 3 1.017085 0.323412 0.541396 11.00000 0.02364 0.01977 =
0.04052 0.01119 0.00972 0.00698
N8 3 0.998957 0.345698 0.570329 11.00000 0.02751 0.04479 =
0.04133 0.00115 0.01175 0.00678
N9 3 0.960187 0.361058 0.479310 11.00000 0.01356 0.02110 =
0.02756 0.00661 0.00492 0.00260
N10 3 0.724316 0.127859 0.380586 11.00000 0.02201 0.01621 =
0.02936 0.00101 0.02099 0.00040
N11 3 0.694348 0.133925 0.394540 11.00000 0.02453 0.01695 =
0.03024 0.00534 0.02003 0.00767
N12 3 0.706115 0.038971 0.392177 11.00000 0.01853 0.01608 =
0.03117 0.01004 0.01288 0.00920
N13 3 0.828431 -0.168485 0.403083 11.00000 0.01791 0.01777 =
0.03654 -0.00389 0.01953 -0.00056
N14 3 0.812543 -0.223596 0.403582 11.00000 0.01837 0.01311 =
0.03932 0.00493 0.01988 0.00398
N15 3 0.771450 -0.153806 0.401558 11.00000 0.02193 0.01051 =
0.03604 0.00136 0.02006 0.00429
N16 3 0.721525 -0.124320 0.596247 11.00000 0.05363 0.05198 =
0.00488 -0.00442 0.00779 -0.02743
N17 3 0.686382 -0.156338 0.567426 11.00000 0.03039 0.01173 =
0.03961 -0.00250 0.02799 -0.00152
N18 3 0.701500 -0.123326 0.506364 11.00000 0.02490 0.01720 =
0.02744 -0.00322 0.02114 -0.00119
N19 3 0.647229 0.292813 0.389574 11.00000 0.02341 0.01783 =
0.04687 0.00270 0.02669 0.00127
N20 3 0.662955 0.343461 0.380932 11.00000 0.01497 0.01979 =
0.01956 0.00257 0.01043 0.00491
N21 3 0.610529 0.368088 0.387715 11.00000 0.01780 0.01371 =
0.01548 -0.00429 0.01294 -0.00043
N22 3 0.451720 0.289596 0.403807 11.00000 0.01703 0.01665 =
0.06286 0.00558 0.02128 0.00070
N23 3 0.430159 0.340943 0.398438 11.00000 0.01962 0.01029 =
0.04295 -0.00016 0.01834 0.00202
N24 3 0.483890 0.364913 0.393714 11.00000 0.01525 0.01291 =
0.04232 -0.00801 0.01750 -0.00417
N26 3 0.609222 0.582275 0.563306 11.00000 0.01864 0.01761 =
0.05569 -0.00579 0.02408 -0.00878
N27 3 0.587731 0.511466 0.501556 11.00000 0.01797 0.02197 =
0.02803 -0.00796 0.01308 -0.00271
PART 5
N25 3 0.629667 0.530650 0.589996 10.50000 0.02345 0.01839 =
0.05966 -0.00581 0.01885 0.00239
C37 1 0.615692 0.489769 0.551454 10.50000 0.02345 0.01839 =
0.05966 -0.00581 0.01885 0.00239
AFIX 3
H37A 2 0.624392 0.448588 0.557625 10.50000 -1.20000
AFIX 0
C38 1 0.584970 0.570556 0.511064 10.50000 0.02345 0.01839 =
0.05966 -0.00581 0.01885 0.00239
AFIX 3
H38A 2 0.567440 0.599006 0.483954 10.50000 -1.20000
AFIX 0
PART 6
N25A 3 0.611102 0.530074 0.592242 10.50000 0.03652 0.03565 =
0.03790 -0.02277 0.01479 -0.00778
C37A 1 0.597824 0.489937 0.552625 10.50000 0.03652 0.03565 =
0.03790 -0.02277 0.01479 -0.00778
AFIX 3
H37B 2 0.595412 0.448116 0.559145 10.50000 -1.20000
AFIX 0
C38A 1 0.595595 0.570840 0.511041 10.50000 0.03652 0.03565 =
0.03790 -0.02277 0.01479 -0.00778
AFIX 3
H38B 2 0.591695 0.600040 0.483451 10.50000 -1.20000
AFIX 0
PART 0
C1 1 0.808169 0.284499 0.361359 11.00000 0.02202 0.01454 =
0.03144 -0.00668 0.01614 -0.00099
AFIX 43
H1 2 0.825736 0.253946 0.361777 11.00000 -1.20000
AFIX 0
C2 1 0.782720 0.370363 0.359964 11.00000 0.02447 0.02346 =
0.01084 -0.00148 0.01017 0.00117
AFIX 43
H2 2 0.778784 0.412572 0.359916 11.00000 -1.20000
AFIX 0
C3 1 0.912598 0.577317 0.389002 11.00000 0.01689 0.01717 =
0.04362 0.00075 0.01973 -0.00585
AFIX 43
H3 2 0.937820 0.566662 0.392329 11.00000 -1.20000
AFIX 0
C4 1 0.854239 0.571110 0.379499 11.00000 0.02080 0.01467 =
0.03812 0.00055 0.01921 0.00145
AFIX 43
H4 2 0.829504 0.555574 0.374657 11.00000 -1.20000
AFIX 0
C5 1 0.994388 0.331935 0.488617 11.00000 0.02307 0.02286 =
0.04514 -0.00335 0.01837 -0.00417
AFIX 43
H5 2 1.000689 0.319775 0.461019 11.00000 -1.20000
AFIX 0
C6 1 0.965142 0.368171 0.530475 11.00000 0.02380 0.04036 =
0.04124 0.00457 0.01409 0.00268
AFIX 43
H6 2 0.945831 0.387774 0.537201 11.00000 -1.20000
AFIX 0
C7 1 0.851489 0.373361 0.364979 11.00000 0.01939 0.01108 =
0.02612 -0.00137 0.01524 -0.00400
C8 1 0.847707 0.441815 0.368671 11.00000 0.01675 0.01216 =
0.03341 0.00490 0.01566 0.00293
AFIX 23
H8A 2 0.824563 0.457044 0.334344 11.00000 -1.20000
H8B 2 0.843217 0.451772 0.399891 11.00000 -1.20000
AFIX 0
C9 1 0.886592 0.470986 0.377137 11.00000 0.01545 0.01072 =
0.02769 -0.00124 0.01650 -0.00141
C10 1 0.921966 0.449743 0.429614 11.00000 0.01345 0.01338 =
0.03503 -0.00044 0.01593 0.00047
AFIX 23
H10A 2 0.918243 0.460479 0.461330 11.00000 -1.20000
H10B 2 0.946817 0.469461 0.434620 11.00000 -1.20000
AFIX 0
C11 1 0.925770 0.381072 0.426981 11.00000 0.01372 0.01038 =
0.03212 0.00403 0.01028 0.00177
C12 1 0.887759 0.350990 0.420219 11.00000 0.01573 0.01379 =
0.01996 0.00604 0.01116 0.00284
AFIX 23
H12A 2 0.883518 0.361617 0.451522 11.00000 -1.20000
H12B 2 0.890264 0.306715 0.419434 11.00000 -1.20000
AFIX 0
C13 1 0.857390 0.357734 0.317205 11.00000 0.03009 0.02037 =
0.03620 -0.00207 0.02407 0.00114
AFIX 23
H13A 2 0.834376 0.372619 0.282566 11.00000 -1.20000
H13B 2 0.858963 0.313514 0.314441 11.00000 -1.20000
AFIX 0
C14 1 0.896672 0.387064 0.325906 11.00000 0.01684 0.02247 =
0.01715 0.00158 0.00812 -0.00116
AFIX 13
H14 2 0.900910 0.376345 0.294244 11.00000 -1.20000
AFIX 0
C15 1 0.892809 0.455624 0.327738 11.00000 0.01988 0.02156 =
0.03550 0.00440 0.01533 -0.00014
AFIX 23
H15A 2 0.869630 0.470060 0.293054 11.00000 -1.20000
H15B 2 0.917473 0.475385 0.332111 11.00000 -1.20000
AFIX 0
C16 1 0.932917 0.364900 0.379685 11.00000 0.02634 0.01509 =
0.04666 0.00218 0.02631 -0.00092
AFIX 23
H16A 2 0.935853 0.320784 0.378233 11.00000 -1.20000
H16B 2 0.957904 0.384240 0.384797 11.00000 -1.20000
AFIX 0
C17 1 0.730970 0.071530 0.380790 11.00000 0.01330 0.01768 =
0.02527 0.00720 0.01314 0.00504
AFIX 43
H17 2 0.750925 0.054686 0.373797 11.00000 -1.20000
AFIX 0
C18 1 0.684191 0.079973 0.401273 11.00000 0.02935 0.02032 =
0.03219 -0.00206 0.02865 -0.00154
AFIX 43
H18 2 0.664210 0.070951 0.411165 11.00000 -1.20000
AFIX 0
C19 1 0.804923 -0.127066 0.404125 11.00000 0.02224 0.00989 =
0.03711 -0.00263 0.02272 -0.00313
AFIX 43
H19 2 0.809951 -0.085017 0.406308 11.00000 -1.20000
AFIX 0
C20 1 0.778415 -0.214296 0.402114 11.00000 0.02643 0.01947 =
0.03417 0.00192 0.02590 -0.00024
AFIX 43
H20 2 0.760854 -0.244967 0.401513 11.00000 -1.20000
AFIX 0
C21 1 0.728739 -0.106049 0.556180 11.00000 0.05862 0.06879 =
0.04234 -0.00871 0.03291 -0.04194
AFIX 43
H21 2 0.751556 -0.082604 0.563018 11.00000 -1.20000
AFIX 0
C22 1 0.674735 -0.155487 0.515012 11.00000 0.02444 0.02981 =
0.03421 0.00438 0.02023 -0.00086
AFIX 43
H22 2 0.651193 -0.174389 0.487099 11.00000 -1.20000
AFIX 0
C23 1 0.702877 -0.026842 0.396204 11.00000 0.02521 0.01095 =
0.02123 -0.00136 0.01266 -0.00130
C24 1 0.739315 -0.056340 0.395765 11.00000 0.01559 0.01235 =
0.02335 0.00456 0.00992 0.00207
AFIX 23
H24A 2 0.739218 -0.046474 0.361032 11.00000 -1.20000
H24B 2 0.764630 -0.040987 0.426927 11.00000 -1.20000
AFIX 0
C25 1 0.736553 -0.125035 0.400876 11.00000 0.01469 0.01237 =
0.02575 -0.00735 0.01006 -0.00152
C26 1 0.736876 -0.139825 0.454914 11.00000 0.01965 0.01315 =
0.02835 0.00389 0.01656 0.00354
AFIX 23
H26A 2 0.735322 -0.183928 0.458487 11.00000 -1.20000
H26B 2 0.762229 -0.125335 0.486578 11.00000 -1.20000
AFIX 0
C27 1 0.701112 -0.109603 0.455118 11.00000 0.01721 0.02588 =
0.01426 0.00562 0.00680 0.00837
C28 1 0.702872 -0.041067 0.448756 11.00000 0.01742 0.01376 =
0.02564 -0.00196 0.01854 0.00251
AFIX 23
H28A 2 0.679348 -0.021897 0.448499 11.00000 -1.20000
H28B 2 0.727551 -0.024749 0.480377 11.00000 -1.20000
AFIX 0
C29 1 0.663920 -0.049327 0.344883 11.00000 0.02280 0.02619 =
0.02911 0.00554 0.00916 0.00840
AFIX 23
H29A 2 0.665024 -0.040820 0.310752 11.00000 -1.20000
H29B 2 0.639986 -0.029085 0.342478 11.00000 -1.20000
AFIX 0
C30 1 0.661845 -0.118808 0.352667 11.00000 0.01821 0.01630 =
0.03408 -0.00444 0.01331 0.00215
AFIX 13
H30 2 0.636585 -0.134976 0.321082 11.00000 -1.20000
AFIX 0
C31 1 0.698085 -0.148031 0.352268 11.00000 0.02063 0.02137 =
0.03119 -0.00445 0.01714 -0.00070
AFIX 23
H31A 2 0.696560 -0.192314 0.354613 11.00000 -1.20000
H31B 2 0.697884 -0.138127 0.317473 11.00000 -1.20000
AFIX 0
C32 1 0.661865 -0.132871 0.405887 11.00000 0.02548 0.01584 =
0.03481 0.00341 0.02077 0.00004
AFIX 23
H32A 2 0.659646 -0.176867 0.409267 11.00000 -1.20000
H32B 2 0.638452 -0.113429 0.405730 11.00000 -1.20000
AFIX 0
C33 1 0.615787 0.308156 0.393917 11.00000 0.01298 0.02147 =
0.03695 0.00411 0.01551 0.00520
AFIX 43
H33 2 0.599242 0.281191 0.400434 11.00000 -1.20000
AFIX 0
C34 1 0.640429 0.388107 0.378774 11.00000 0.02564 0.01545 =
0.02013 0.00125 0.01516 -0.00275
AFIX 43
H34 2 0.644269 0.428790 0.371951 11.00000 -1.20000
AFIX 0
C35 1 0.483307 0.304721 0.401386 11.00000 0.01331 0.01610 =
0.05516 -0.00165 0.01866 -0.00221
AFIX 43
H35 2 0.503522 0.277472 0.404538 11.00000 -1.20000
AFIX 0
C36 1 0.450120 0.385429 0.392784 11.00000 0.02579 0.01244 =
0.05934 -0.00046 0.03197 0.00466
AFIX 43
H36 2 0.442113 0.426432 0.388604 11.00000 -1.20000
AFIX 0
C39 1 0.578770 0.405703 0.389919 11.00000 0.01836 0.00991 =
0.03028 -0.00106 0.01851 0.00294
C40 1 0.546412 0.364480 0.388848 11.00000 0.01055 0.01345 =
0.02401 -0.00865 0.00779 -0.00079
AFIX 23
H40A 2 0.533454 0.341257 0.354051 11.00000 -1.20000
H40B 2 0.558570 0.335761 0.419985 11.00000 -1.20000
AFIX 0
C41 1 0.515310 0.403512 0.393431 11.00000 0.01924 0.01196 =
0.04221 -0.00747 0.02409 -0.00125
C42 1 0.535482 0.437999 0.447155 11.00000 0.01994 0.01439 =
0.04087 -0.00550 0.02265 -0.00413
AFIX 23
H42A 2 0.515249 0.462401 0.450928 11.00000 -1.20000
H42B 2 0.547701 0.409477 0.478443 11.00000 -1.20000
AFIX 0
C43 1 0.567575 0.478535 0.448254 11.00000 0.02588 0.02094 =
0.02498 -0.00640 0.01878 -0.00138
C44 1 0.600091 0.439758 0.445067 11.00000 0.02076 0.01964 =
0.04901 0.00645 0.02694 0.00032
AFIX 23
H44A 2 0.621722 0.465640 0.446532 11.00000 -1.20000
H44B 2 0.612130 0.411056 0.476227 11.00000 -1.20000
AFIX 0
C45 1 0.560447 0.449411 0.340937 11.00000 0.02621 0.01995 =
0.03552 -0.00071 0.01920 0.00503
AFIX 23
H45A 2 0.581724 0.475470 0.341573 11.00000 -1.20000
H45B 2 0.547805 0.426647 0.305877 11.00000 -1.20000
AFIX 0
C46 1 0.528793 0.487940 0.345311 11.00000 0.02444 0.01193 =
0.04405 -0.00005 0.02191 0.00328
AFIX 13
H46 2 0.516450 0.516995 0.313900 11.00000 -1.20000
AFIX 0
C47 1 0.495987 0.446761 0.344777 11.00000 0.01847 0.01576 =
0.04953 -0.00352 0.02082 -0.00214
AFIX 23
H47A 2 0.475379 0.471446 0.347392 11.00000 -1.20000
H47B 2 0.482634 0.423783 0.309861 11.00000 -1.20000
AFIX 0
C48 1 0.549938 0.523082 0.401657 11.00000 0.02738 0.01776 =
0.03635 0.00344 0.02068 -0.00151
AFIX 23
H48A 2 0.571470 0.549169 0.403081 11.00000 -1.20000
H48B 2 0.530098 0.548915 0.405008 11.00000 -1.20000
AFIX 0
O1W 4 0.592501 0.380174 0.244067 11.00000 0.07247 0.11786 =
0.09055 0.01914 0.03459 0.04665
O2W 4 0.791404 -0.212226 0.581631 11.00000 0.13862 0.04480 =
0.11455 0.00180 0.05441 -0.01534
O3W 4 0.249801 0.089006 0.280819 11.00000 0.11393 0.14959 =
0.08443 -0.03157 0.04912 -0.04965
O4W 4 0.640321 0.080300 0.262087 11.00000 0.18661 0.03848 =
0.10502 0.00098 -0.00805 -0.01291
O5W 4 0.535765 0.315984 0.252037 11.00000 0.13589 0.08060 =
0.13361 0.00760 0.07828 0.02033
O6W 4 0.812083 -0.020081 0.284630 11.00000 0.14218 0.08864 =
0.09018 0.02119 0.05051 0.04525
O7W 4 0.419062 0.074401 0.516458 11.00000 0.16000 0.06868 =
0.12559 0.03034 0.07407 0.02209
O8W 4 0.655363 -0.000172 0.522897 11.00000 0.13408
O9W 4 0.231789 0.288954 0.270485 11.00000 0.14341
O10W 4 0.671279 0.637326 0.326571 11.00000 0.14862
O11W 4 0.496817 0.006268 0.574112 11.00000 0.13296
O12W 4 0.538614 0.463549 0.576178 11.00000 0.15459
O13W 4 0.241748 0.411782 0.269545 11.00000 0.16867
O14W 4 0.703434 0.023495 0.253976 11.00000 0.15334
O15W 4 0.338023 0.322488 0.531299 11.00000 0.17026
O16W 4 0.557833 0.193851 0.280370 10.65000 0.11805
O17W 4 0.550151 0.201793 0.212967 10.35000 0.09810
HKLF 4

REM C2c in C2/c
REM R1 = 0.0635 for 10206 Fo > 4sig(Fo) and 0.1265 for all 22268 data
REM 1102 parameters refined using 38 restraints

END

WGHT 0.0740 0.0000
REM Highest difference peak 1.426, deepest hole -0.981, 1-sigma level 0.118
Q1 1 0.4445 0.2707 0.4913 11.00000 0.05 1.18
Q2 1 0.2507 0.3296 0.2702 11.00000 0.05 1.12
Q3 1 0.5561 0.1570 0.2996 11.00000 0.05 0.95
Q4 1 0.4258 0.2101 0.3781 11.00000 0.05 0.91
Q5 1 0.3272 0.3033 0.5243 11.00000 0.05 0.77
Q6 1 0.5192 0.4282 0.5697 11.00000 0.05 0.76
Q7 1 0.6721 0.5191 0.3009 11.00000 0.05 0.73
Q8 1 0.3635 0.3489 0.5564 11.00000 0.05 0.68
Q9 1 0.4156 0.3004 0.5528 11.00000 0.05 0.68
Q10 1 0.6715 0.4998 0.3598 11.00000 0.05 0.65

;

#---------------------------------------------------------

data_(7)
_database_code_depnum_ccdc_archive 'CCDC 867230'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[3,5,7-tri(1,2,4-triazol-4-yl)-1-azaadamantane]cadmium(II)
Tetraiodocadmate(II) Trihydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C30 H36 Cd N20), (Cd I4), 3(H2 O)'
_chemical_formula_sum            'C30 H42 Cd2 I4 N20 O3'
_chemical_formula_weight         1463.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   11.4936(8)
_cell_length_b                   11.4936(8)
_cell_length_c                   57.216(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6545.7(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      27.87

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4164
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2052
_exptl_absorpt_correction_T_max  0.5121
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11820
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         27.87
_reflns_number_total             1733
_reflns_number_gt                1305
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The CdI4^2-^ anion is equally disordered by symmetry in such a way that
three iodine atoms are ordered and are common for two orientations,
while Cd-I fragment is equally disordered from two axial sides of the
I-I-I triangle. Positions of this disordered fragment are overlapped
with the solvate water molecule (O1W), which thus was also refined with
a partial occupancy factor 0.50. The disorder was trated without any
restraints in geometry and thermal parameters and all corresponding
atoms were refined anisotropically.

Refinement of Cd-organic framework atoms was standard. The CH-hydrogen
atoms were constrained with U(iso) = 1.2U(eq) of the parent C-atom and
with C-H distances 0.94 A (triazole), 0.98 A (CH2 azaadamantane).
The OH-hydrogen atoms were constrained with O-H distances set to 0.85 A
and U(iso) = 1.5U(eq) of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+36.5985P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1733
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1245
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.0157(2) Uani 1 6 d S . .
Cd2 Cd 0.6667 0.3333 0.07113(2) 0.0277(3) Uani 0.50 3 d SP . .
I1 I 0.6667 0.55790(5) 0.0833 0.0654(3) Uani 1 2 d S . .
I2 I 0.6667 0.3333 0.02365(3) 0.0885(8) Uani 0.50 3 d SP . .
N1 N 0.1421(4) 0.1897(4) 0.02285(7) 0.0256(9) Uani 1 1 d . . .
N2 N 0.2617(5) 0.2065(5) 0.03113(9) 0.0373(11) Uani 1 1 d . . .
N3 N 0.2506(4) 0.3881(4) 0.03928(7) 0.0216(8) Uani 1 1 d . . .
N4 N 0.3333 0.6667 0.08287(12) 0.0216(13) Uani 1 3 d S . .
C1 C 0.1375(5) 0.2974(5) 0.02804(10) 0.0284(10) Uani 1 1 d . . .
H1 H 0.0651 0.3107 0.0245 0.034 Uiso 1 1 calc R . .
C2 C 0.3231(6) 0.3251(6) 0.04099(12) 0.0400(14) Uani 1 1 d . . .
H2 H 0.4072 0.3620 0.0484 0.048 Uiso 1 1 calc R . .
C3 C 0.2915(4) 0.5257(4) 0.04766(8) 0.0184(8) Uani 1 1 d . . .
C4 C 0.1907(4) 0.5663(4) 0.03847(8) 0.0194(9) Uani 1 1 d . . .
H4A H 0.0999 0.5025 0.0440 0.023 Uiso 1 1 calc R . .
H4B H 0.1901 0.5659 0.0213 0.023 Uiso 1 1 calc R . .
C5 C 0.2930(4) 0.5305(4) 0.07450(8) 0.0209(9) Uani 1 1 d . . .
H5A H 0.2032 0.4669 0.0805 0.025 Uiso 1 1 calc R . .
H5B H 0.3558 0.5034 0.0805 0.025 Uiso 1 1 calc R . .
O1W O 0.485(3) 0.161(3) 0.0170(4) 0.205(15) Uani 0.50 1 d P . .
H1W H 0.4950 0.1446 0.0312 0.307 Uiso 0.50 1 d PR . .
H2W H 0.4210 0.1781 0.0167 0.307 Uiso 0.50 1 d PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0104(2) 0.0104(2) 0.0264(4) 0.000 0.000 0.00521(12)
Cd2 0.0274(4) 0.0274(4) 0.0284(6) 0.000 0.000 0.01369(19)
I1 0.0346(3) 0.0232(2) 0.1420(8) -0.01544(18) -0.0309(4) 0.01731(17)
I2 0.1186(12) 0.1186(12) 0.0282(8) 0.000 0.000 0.0593(6)
N1 0.0177(19) 0.0205(19) 0.039(2) -0.0076(17) -0.0086(16) 0.0097(16)
N2 0.028(2) 0.029(2) 0.060(3) -0.018(2) -0.021(2) 0.018(2)
N3 0.0189(18) 0.0159(18) 0.031(2) -0.0044(15) -0.0054(15) 0.0092(15)
N4 0.0198(19) 0.0198(19) 0.025(3) 0.000 0.000 0.0099(9)
C1 0.019(2) 0.022(2) 0.045(3) -0.009(2) -0.010(2) 0.0110(19)
C2 0.029(3) 0.030(3) 0.068(4) -0.021(3) -0.021(3) 0.019(2)
C3 0.0171(19) 0.0115(18) 0.027(2) 0.0003(16) -0.0024(16) 0.0071(16)
C4 0.016(2) 0.0154(19) 0.027(2) 0.0013(17) -0.0029(17) 0.0083(16)
C5 0.020(2) 0.018(2) 0.025(2) 0.0026(17) -0.0015(16) 0.0099(16)
O1W 0.30(3) 0.31(3) 0.166(18) 0.18(2) 0.18(2) 0.28(3)

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

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
Cd1 N1 2.360(4) 19 ?
Cd1 N1 2.360(4) 21 ?
Cd1 N1 2.360(4) 20 ?
Cd1 N1 2.360(4) . ?
Cd1 N1 2.360(4) 3 ?
Cd1 N1 2.360(4) 2 ?
Cd2 I1 2.6739(6) 3_665 ?
Cd2 I1 2.6739(6) 2_655 ?
Cd2 I1 2.6739(6) . ?
Cd2 I2 2.716(2) . ?
N1 C1 1.299(6) . ?
N1 N2 1.373(6) . ?
N2 C2 1.308(7) . ?
N3 C2 1.353(7) . ?
N3 C1 1.355(6) . ?
N3 C3 1.487(5) . ?
N4 C5 1.472(5) 3_565 ?
N4 C5 1.472(5) 2_665 ?
N4 C5 1.472(5) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 C5 1.537(6) . ?
C3 C4 1.542(6) . ?
C3 C4 1.542(6) 2_665 ?
C4 C3 1.542(6) 3_565 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
O1W H1W 0.8500 . ?
O1W H2W 0.8500 . ?

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 Cd1 N1 92.27(15) 19 21 ?
N1 Cd1 N1 92.27(15) 19 20 ?
N1 Cd1 N1 92.27(15) 21 20 ?
N1 Cd1 N1 180.00(17) 19 . ?
N1 Cd1 N1 87.73(15) 21 . ?
N1 Cd1 N1 87.73(15) 20 . ?
N1 Cd1 N1 87.73(15) 19 3 ?
N1 Cd1 N1 180.00(17) 21 3 ?
N1 Cd1 N1 87.73(15) 20 3 ?
N1 Cd1 N1 92.27(15) . 3 ?
N1 Cd1 N1 87.73(15) 19 2 ?
N1 Cd1 N1 87.73(15) 21 2 ?
N1 Cd1 N1 180.00(17) 20 2 ?
N1 Cd1 N1 92.27(15) . 2 ?
N1 Cd1 N1 92.27(15) 3 2 ?
I1 Cd2 I1 113.44(2) 3_665 2_655 ?
I1 Cd2 I1 113.44(2) 3_665 . ?
I1 Cd2 I1 113.44(2) 2_655 . ?
I1 Cd2 I2 105.14(3) 3_665 . ?
I1 Cd2 I2 105.14(3) 2_655 . ?
I1 Cd2 I2 105.14(3) . . ?
C1 N1 N2 107.6(4) . . ?
C1 N1 Cd1 131.9(3) . . ?
N2 N1 Cd1 120.2(3) . . ?
C2 N2 N1 106.0(4) . . ?
C2 N3 C1 103.5(4) . . ?
C2 N3 C3 126.4(4) . . ?
C1 N3 C3 130.1(4) . . ?
C5 N4 C5 110.0(3) 3_565 2_665 ?
C5 N4 C5 110.0(3) 3_565 . ?
C5 N4 C5 110.0(3) 2_665 . ?
N1 C1 N3 111.2(4) . . ?
N1 C1 H1 124.4 . . ?
N3 C1 H1 124.4 . . ?
N2 C2 N3 111.7(5) . . ?
N2 C2 H2 124.1 . . ?
N3 C2 H2 124.1 . . ?
N3 C3 C5 110.6(3) . . ?
N3 C3 C4 109.0(3) . . ?
C5 C3 C4 109.0(4) . . ?
N3 C3 C4 109.1(4) . 2_665 ?
C5 C3 C4 109.0(3) . 2_665 ?
C4 C3 C4 110.0(4) . 2_665 ?
C3 C4 C3 108.0(4) . 3_565 ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 3_565 . ?
C3 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 3_565 . ?
H4A C4 H4B 108.4 . . ?
N4 C5 C3 110.8(4) . . ?
N4 C5 H5A 109.5 . . ?
C3 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
H1W O1W H2W 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cd1 N1 C1 30.6(5) 21 . . . ?
N1 Cd1 N1 C1 123.0(6) 20 . . . ?
N1 Cd1 N1 C1 -149.4(5) 3 . . . ?
N1 Cd1 N1 C1 -57.0(6) 2 . . . ?
N1 Cd1 N1 N2 -141.5(4) 21 . . . ?
N1 Cd1 N1 N2 -49.1(3) 20 . . . ?
N1 Cd1 N1 N2 38.5(4) 3 . . . ?
N1 Cd1 N1 N2 130.9(3) 2 . . . ?
C1 N1 N2 C2 0.1(7) . . . . ?
Cd1 N1 N2 C2 173.9(4) . . . . ?
N2 N1 C1 N3 0.9(6) . . . . ?
Cd1 N1 C1 N3 -172.0(3) . . . . ?
C2 N3 C1 N1 -1.4(6) . . . . ?
C3 N3 C1 N1 177.5(5) . . . . ?
N1 N2 C2 N3 -1.0(7) . . . . ?
C1 N3 C2 N2 1.5(7) . . . . ?
C3 N3 C2 N2 -177.5(5) . . . . ?
C2 N3 C3 C5 -69.7(6) . . . . ?
C1 N3 C3 C5 111.7(5) . . . . ?
C2 N3 C3 C4 170.4(5) . . . . ?
C1 N3 C3 C4 -8.2(7) . . . . ?
C2 N3 C3 C4 50.2(6) . . . 2_665 ?
C1 N3 C3 C4 -128.4(5) . . . 2_665 ?
N3 C3 C4 C3 179.3(3) . . . 3_565 ?
C5 C3 C4 C3 58.4(5) . . . 3_565 ?
C4 C3 C4 C3 -61.1(6) 2_665 . . 3_565 ?
C5 N4 C5 C3 60.6(5) 3_565 . . . ?
C5 N4 C5 C3 -60.6(5) 2_665 . . . ?
N3 C3 C5 N4 -179.9(3) . . . . ?
C4 C3 C5 N4 -60.0(4) . . . . ?
C4 C3 C5 N4 60.1(4) 2_665 . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.986
_refine_diff_density_rms         0.162

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL IP1-1134 in R-3c
CELL 0.71073 11.4936 11.4936 57.2157 90.000 90.000 120.000
ZERR 6.00 0.0008 0.0008 0.0021 0.000 0.000 0.000
LATT 3
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SYMM Y, X, 1/2 - Z
SYMM X - Y, - Y, 1/2 - Z
SYMM - X, - X + Y, 1/2 - Z
SFAC C H N O CD I
UNIT 180 252 120 18 12 24
MERG 2
OMIT -1 2 0
OMIT -1 3 2
OMIT -2 5 8
OMIT -1 2 24
OMIT -1 3 68
OMIT -2 7 9
SHEL 0.76 7
FMAP 2
PLAN 20
SIZE 0.20 0.21 0.60
ACTA
BOND
BOND $H
CONF
LIST 4
L.S. 4
TEMP -60.00
WGHT 0.074500 36.598499
FVAR 0.08833
CD1 5 0.000000 0.000000 0.000000 10.16667 0.01041 0.01041 =
0.02641 0.00000 0.00000 0.00521
CD2 5 0.666667 0.333333 0.071130 10.16667 0.02739 0.02739 =
0.02838 0.00000 0.00000 0.01369
I1 6 0.666667 0.557904 0.083333 10.50000 0.03461 0.02324 =
0.14204 -0.01544 -0.03088 0.01731
I2 6 0.666667 0.333333 0.023653 10.16667 0.11860 0.11860 =
0.02821 0.00000 0.00000 0.05930
N1 3 0.142091 0.189737 0.022853 11.00000 0.01770 0.02054 =
0.03889 -0.00764 -0.00862 0.00970
N2 3 0.261653 0.206506 0.031126 11.00000 0.02775 0.02941 =
0.06006 -0.01822 -0.02071 0.01836
N3 3 0.250572 0.388093 0.039278 11.00000 0.01891 0.01593 =
0.03059 -0.00440 -0.00535 0.00921
N4 3 0.333333 0.666667 0.082868 10.33333 0.01977 0.01977 =
0.02520 0.00000 0.00000 0.00988
C1 1 0.137484 0.297414 0.028037 11.00000 0.01919 0.02203 =
0.04485 -0.00935 -0.00965 0.01101
AFIX 43
H1 2 0.065120 0.310661 0.024454 11.00000 -1.20000
AFIX 0
C2 1 0.323062 0.325078 0.040987 11.00000 0.02850 0.03012 =
0.06750 -0.02052 -0.02063 0.01932
AFIX 43
H2 2 0.407247 0.361989 0.048359 11.00000 -1.20000
AFIX 0
C3 1 0.291539 0.525743 0.047660 11.00000 0.01708 0.01147 =
0.02650 0.00034 -0.00238 0.00709
C4 1 0.190682 0.566299 0.038472 11.00000 0.01601 0.01545 =
0.02729 0.00133 -0.00288 0.00833
AFIX 23
H4A 2 0.099926 0.502454 0.043979 11.00000 -1.20000
H4B 2 0.190131 0.565906 0.021344 11.00000 -1.20000
AFIX 0
C5 1 0.292963 0.530481 0.074503 11.00000 0.02026 0.01765 =
0.02546 0.00260 -0.00153 0.00989
AFIX 23
H5A 2 0.203245 0.466948 0.080477 11.00000 -1.20000
H5B 2 0.355838 0.503422 0.080474 11.00000 -1.20000
AFIX 0
O1W 4 0.484637 0.160591 0.017044 10.50000 0.30414 0.31193 =
0.16574 0.17857 0.17906 0.27962
AFIX 3
H1W 2 0.494987 0.144581 0.031164 10.50000 -1.50000
H2W 2 0.421027 0.178091 0.016674 10.50000 -1.50000
HKLF 4

REM IP1-1134 in R-3c
REM R1 = 0.0455 for 1305 Fo > 4sig(Fo) and 0.0608 for all 1733 data
REM 98 parameters refined using 0 restraints

END

WGHT 0.0747 36.5038
REM Highest difference peak 1.908, deepest hole -1.986, 1-sigma level 0.162
Q1 1 0.6813 0.5381 0.0730 11.00000 0.05 1.91
Q2 1 0.7251 0.5662 0.0590 11.00000 0.05 1.35
Q3 1 0.6667 0.3781 0.0833 10.50000 0.05 1.34
Q4 1 0.5867 0.2327 0.0271 11.00000 0.05 1.22
Q5 1 0.0000 0.0000 0.0131 10.33333 0.05 1.17
Q6 1 0.5511 0.2649 0.0200 11.00000 0.05 0.85
Q7 1 0.6667 0.3333 0.0547 10.33333 0.05 0.55
Q8 1 0.2788 0.5219 0.0601 11.00000 0.05 0.51
Q9 1 0.5057 0.2216 0.0324 11.00000 0.05 0.45
Q10 1 0.3333 0.6667 0.0940 10.33333 0.05 0.43

;

#---------------------------------------------------------

data_(8)
_database_code_depnum_ccdc_archive 'CCDC 867231'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[3,5,7-tri(1,2,4-triazol-4-yl)-1-azaadamantane]-dihydroxy-tetraaqua-
tricopper(II) Perchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 Cl2 Cu3 N20 O14, 2(Cl O4)'
_chemical_formula_sum            'C30 H46 Cl4 Cu3 N20 O22'
_chemical_formula_weight         1371.29

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

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

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

_cell_length_a                   12.1931(7)
_cell_length_b                   17.2484(12)
_cell_length_c                   22.1135(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4650.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      4.09
_cell_measurement_theta_max      27.03

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2788
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6862
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28242
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.09
_diffrn_reflns_theta_max         27.03
_reflns_number_total             5038
_reflns_number_gt                3458
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

One of two unique ClO4^-^ anions displays disorder by two overlapping
positions, with the refined partial occupancy factors 0.80/0.20. The
major contribution of the disorder was freely refined anisotropically.
For the minor component, the Cl atom was anisotropic, while O-atoms
were left isotropic. This minor component was refined with restrained
geometry [Cl-O 1.42(1) A; O...O 2.30(1) A] and with SIMU restraint for
the isotropic thermal parameters of O-atoms.

This minor 0.2 component of the ClO4^-^ generates short contact with
distal aqua-ligand O11 indicating that the latter possibly adopts a
partial occupancy. However, site of O11 was refined with the occupancy
factor 1.00. All the H-atoms were located and then constrained. The
CH-hydrogen atoms were constrained with U(iso) = 1.2U(eq) of the parent
C-atom and with C-H distances allowed to refine giving C-H 0.94-1.00 A
(triazole) and 0.88-0.97 A (CH2 azaadamantane). The same approach was
used for the OH-hydrogen atoms constrained with U(iso) = 1.5U(eq) of
the parent O-atom (O-H distances 0.85-0.86 A).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5038
_refine_ls_number_parameters     395
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.914
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.0000 0.5000 0.01792(14) Uani 1 2 d S . .
Cu2 Cu 0.48972(3) 0.19300(2) 0.474193(18) 0.02221(12) Uani 1 1 d . . .
O1 O 0.4829(2) 0.10369(12) 0.52422(10) 0.0279(5) Uani 1 1 d . . .
H1W H 0.4444 0.1129 0.5559 0.042 Uiso 1 1 d . . .
O2 O 0.6763(3) 0.19196(18) 0.47758(17) 0.0551(9) Uani 1 1 d . . .
H2W H 0.6998 0.1479 0.4902 0.083 Uiso 1 1 d . . .
H3W H 0.7001 0.2265 0.5020 0.083 Uiso 1 1 d . . .
O11 O 0.2706(3) 0.2015(2) 0.45104(18) 0.0673(10) Uani 1 1 d . . .
H4W H 0.2453 0.2043 0.4147 0.101 Uiso 1 1 d . . .
H5W H 0.2398 0.1620 0.4674 0.101 Uiso 1 1 d . . .
N1 N 0.4890(2) 0.03741(14) 0.41397(12) 0.0178(5) Uani 1 1 d . A .
N2 N 0.4841(2) 0.11565(15) 0.40230(12) 0.0203(6) Uani 1 1 d . A .
N3 N 0.4420(2) 0.05279(13) 0.31941(11) 0.0171(5) Uani 1 1 d . . .
N4 N 0.5957(3) -0.2026(2) 0.1184(2) 0.0552(11) Uani 1 1 d . . .
N5 N 0.5055(3) -0.21610(16) 0.08217(13) 0.0273(6) Uani 1 1 d . . .
N6 N 0.4724(2) -0.11497(15) 0.13859(12) 0.0226(6) Uani 1 1 d . . .
N7 N 0.3793(3) 0.28633(17) 0.09054(14) 0.0350(8) Uani 1 1 d . . .
N8 N 0.4379(3) 0.24560(15) 0.04711(13) 0.0252(6) Uani 1 1 d . . .
N9 N 0.3913(2) 0.16394(14) 0.11745(12) 0.0221(6) Uani 1 1 d . . .
N10 N 0.2365(2) 0.00469(16) 0.19731(13) 0.0233(6) Uani 1 1 d . . .
C1 C 0.4632(3) 0.00132(18) 0.36395(14) 0.0191(6) Uani 1 1 d . . .
H1 H 0.4600(3) -0.049(2) 0.3599(2) 0.023 Uiso 1 1 calc R A .
C2 C 0.4560(3) 0.12312(18) 0.34569(15) 0.0237(7) Uani 1 1 d . . .
H2 H 0.4475(5) 0.167(2) 0.3274(9) 0.028 Uiso 1 1 calc R A .
C3 C 0.5715(4) -0.1432(2) 0.1508(2) 0.0515(12) Uani 1 1 d . . .
H3 H 0.622(3) -0.1206(12) 0.1820(17) 0.062 Uiso 1 1 calc R . .
C4 C 0.4320(3) -0.16466(19) 0.09683(17) 0.0299(8) Uani 1 1 d . . .
H4 H 0.356(3) -0.1622(2) 0.0796(8) 0.036 Uiso 1 1 calc R . .
C5 C 0.3533(4) 0.2356(2) 0.13184(18) 0.0353(9) Uani 1 1 d . . .
H5 H 0.312(2) 0.2477(6) 0.1686(18) 0.042 Uiso 1 1 calc R . .
C6 C 0.4443(3) 0.17386(18) 0.06440(15) 0.0233(7) Uani 1 1 d . . .
H6 H 0.4805(17) 0.1346(18) 0.0431(10) 0.028 Uiso 1 1 calc R . .
C7 C 0.4014(3) 0.03666(16) 0.25712(13) 0.0157(6) Uani 1 1 d . . .
C8 C 0.4636(3) -0.03250(17) 0.22969(14) 0.0182(6) Uani 1 1 d . . .
H8A H 0.4544(4) -0.0739(12) 0.2522(7) 0.022 Uiso 1 1 calc R . .
H8B H 0.534(2) -0.0222(3) 0.22774(14) 0.022 Uiso 1 1 calc R . .
C9 C 0.4173(3) -0.04664(16) 0.16570(14) 0.0180(6) Uani 1 1 d . . .
C10 C 0.4381(3) 0.02507(17) 0.12595(14) 0.0195(6) Uani 1 1 d . . .
H10A H 0.516(2) 0.0364(3) 0.12428(16) 0.023 Uiso 1 1 calc R . .
H10B H 0.4122(7) 0.0159(3) 0.0853(11) 0.023 Uiso 1 1 calc R . .
C11 C 0.3758(3) 0.09307(16) 0.15437(14) 0.0188(6) Uani 1 1 d . . .
C12 C 0.4205(3) 0.10935(17) 0.21811(13) 0.0180(6) Uani 1 1 d . . .
H12A H 0.3840(10) 0.1520(11) 0.2351(5) 0.022 Uiso 1 1 calc R . .
H12B H 0.496(2) 0.1208(4) 0.21621(14) 0.022 Uiso 1 1 calc R . .
C13 C 0.2782(3) 0.01829(18) 0.25890(15) 0.0221(7) Uani 1 1 d . . .
H13A H 0.2664(4) -0.0250(12) 0.2822(7) 0.027 Uiso 1 1 calc R . .
H13B H 0.2410(11) 0.0590(11) 0.2761(5) 0.027 Uiso 1 1 calc R . .
C14 C 0.2931(3) -0.06211(19) 0.17004(16) 0.0246(7) Uani 1 1 d . . .
H14A H 0.2652(9) -0.0712(3) 0.1319(11) 0.030 Uiso 1 1 calc R . .
H14B H 0.2809(5) -0.1058(13) 0.1933(7) 0.030 Uiso 1 1 calc R . .
C15 C 0.2527(3) 0.07344(19) 0.15913(16) 0.0247(7) Uani 1 1 d . . .
H15A H 0.2139(12) 0.1167(12) 0.1762(5) 0.030 Uiso 1 1 calc R . .
H15B H 0.2236(9) 0.0638(3) 0.1195(11) 0.030 Uiso 1 1 calc R . .
Cl2 Cl 0.66007(9) 0.26241(5) 0.20952(5) 0.0390(2) Uani 1 1 d . . .
O7 O 0.6640(4) 0.19395(19) 0.17389(19) 0.0717(12) Uani 1 1 d . . .
O8 O 0.5828(5) 0.2562(3) 0.2567(2) 0.121(2) Uani 1 1 d . . .
O9 O 0.7656(4) 0.2750(3) 0.2349(2) 0.0940(14) Uani 1 1 d . . .
O10 O 0.6413(4) 0.3284(2) 0.1723(2) 0.0885(14) Uani 1 1 d . . .
Cl1 Cl 0.80053(11) 0.00207(8) 0.53549(6) 0.0285(3) Uani 0.80 1 d P A -1
O3 O 0.8853(4) 0.0577(3) 0.53318(19) 0.0593(12) Uani 0.80 1 d P A -1
O4 O 0.7687(5) -0.0170(6) 0.59548(19) 0.063(3) Uani 0.80 1 d P A -1
O5 O 0.7094(4) 0.0252(5) 0.4997(3) 0.059(3) Uani 0.80 1 d P A -1
O6 O 0.8447(5) -0.0671(3) 0.5082(2) 0.0718(14) Uani 0.80 1 d P A -1
Cl1A Cl 0.7836(5) -0.0398(5) 0.5302(3) 0.0515(17) Uani 0.20 1 d PD B -2
O3A O 0.8945(9) -0.0254(11) 0.5157(9) 0.072(6) Uiso 0.20 1 d PD B -2
O4A O 0.768(2) -0.0299(18) 0.5930(6) 0.086(15) Uiso 0.20 1 d PD B -2
O5A O 0.7166(18) 0.0132(13) 0.4986(14) 0.089(17) Uiso 0.20 1 d PD B -2
O6A O 0.7552(15) -0.1161(8) 0.5137(9) 0.079(6) Uiso 0.20 1 d PD . -2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0308(3) 0.0114(2) 0.0115(3) 0.00133(18) -0.0008(2) 0.0017(2)
Cu2 0.0410(3) 0.01168(18) 0.0139(2) -0.00017(14) 0.00263(17) -0.00094(16)
O1 0.0551(16) 0.0124(10) 0.0161(12) 0.0012(9) 0.0069(11) 0.0050(10)
O2 0.0408(17) 0.0491(18) 0.076(3) 0.0128(16) -0.0002(16) -0.0034(14)
O11 0.079(3) 0.061(2) 0.062(2) 0.0009(18) 0.001(2) -0.0016(19)
N1 0.0272(14) 0.0137(11) 0.0126(13) 0.0013(10) -0.0009(10) 0.0017(10)
N2 0.0356(16) 0.0115(11) 0.0138(13) 0.0001(10) -0.0012(11) -0.0009(10)
N3 0.0280(14) 0.0125(11) 0.0110(13) 0.0004(9) -0.0005(11) 0.0007(10)
N4 0.045(2) 0.049(2) 0.072(3) -0.033(2) -0.017(2) 0.0146(17)
N5 0.0445(18) 0.0177(13) 0.0197(15) -0.0014(11) -0.0014(13) 0.0019(12)
N6 0.0318(16) 0.0166(12) 0.0195(15) -0.0040(11) -0.0012(11) 0.0021(11)
N7 0.058(2) 0.0221(14) 0.0246(17) 0.0013(12) 0.0101(15) 0.0068(14)
N8 0.0400(17) 0.0179(13) 0.0179(15) 0.0016(11) 0.0031(12) 0.0012(12)
N9 0.0370(16) 0.0145(12) 0.0149(14) 0.0039(10) 0.0004(12) 0.0023(11)
N10 0.0232(14) 0.0271(14) 0.0196(15) 0.0005(11) -0.0011(11) -0.0046(11)
C1 0.0316(17) 0.0126(14) 0.0132(16) -0.0005(11) -0.0003(12) 0.0019(12)
C2 0.043(2) 0.0138(14) 0.0144(17) 0.0012(12) 0.0003(14) -0.0016(14)
C3 0.045(3) 0.040(2) 0.070(3) -0.027(2) -0.015(2) 0.0063(19)
C4 0.039(2) 0.0224(17) 0.028(2) -0.0076(14) 0.0008(16) 0.0002(14)
C5 0.056(3) 0.0228(17) 0.027(2) 0.0035(15) 0.0108(18) 0.0103(17)
C6 0.0337(19) 0.0188(15) 0.0173(17) 0.0006(13) 0.0035(14) 0.0010(13)
C7 0.0241(16) 0.0165(13) 0.0064(15) 0.0001(11) -0.0017(11) 0.0007(11)
C8 0.0273(17) 0.0140(13) 0.0133(15) 0.0000(11) -0.0013(12) -0.0007(12)
C9 0.0287(17) 0.0113(13) 0.0140(16) -0.0026(11) 0.0015(13) 0.0003(11)
C10 0.0306(18) 0.0153(14) 0.0126(16) -0.0002(12) 0.0013(13) -0.0004(12)
C11 0.0286(17) 0.0145(14) 0.0132(16) 0.0028(11) 0.0006(13) 0.0013(12)
C12 0.0271(17) 0.0124(13) 0.0144(16) -0.0007(12) 0.0004(12) -0.0008(11)
C13 0.0259(17) 0.0214(15) 0.0191(18) -0.0004(12) 0.0017(13) -0.0013(12)
C14 0.0313(18) 0.0222(16) 0.0205(18) -0.0006(13) -0.0044(14) -0.0064(13)
C15 0.0259(17) 0.0281(16) 0.0201(18) -0.0003(14) -0.0046(14) 0.0023(14)
Cl2 0.0527(6) 0.0242(4) 0.0403(6) -0.0066(4) -0.0007(4) 0.0007(4)
O7 0.100(3) 0.0397(18) 0.076(3) -0.0289(17) 0.033(2) -0.0151(19)
O8 0.165(5) 0.084(3) 0.112(4) -0.058(3) 0.100(4) -0.061(3)
O9 0.087(3) 0.114(4) 0.081(3) -0.012(3) -0.031(3) 0.000(3)
O10 0.129(4) 0.062(2) 0.075(3) 0.010(2) -0.004(3) 0.049(3)
Cl1 0.0274(6) 0.0349(7) 0.0231(6) 0.0061(6) 0.0015(4) 0.0010(5)
O3 0.056(3) 0.075(3) 0.047(3) 0.013(2) -0.008(2) -0.032(2)
O4 0.041(3) 0.130(6) 0.019(2) 0.023(2) 0.0109(17) -0.001(3)
O5 0.025(2) 0.098(5) 0.053(4) 0.041(3) -0.0104(18) -0.001(2)
O6 0.098(4) 0.040(2) 0.078(4) -0.006(2) 0.024(3) 0.018(3)
Cl1A 0.032(3) 0.092(6) 0.031(3) -0.002(4) 0.001(2) 0.022(4)

_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.
;

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 O1 1.879(2) 5_656 ?
Cu1 O1 1.879(2) . ?
Cu1 N1 2.013(3) . ?
Cu1 N1 2.013(3) 5_656 ?
Cu1 O5 2.590(5) . ?
Cu2 O1 1.898(2) . ?
Cu2 N5 2.004(3) 4_655 ?
Cu2 N8 2.030(3) 8_566 ?
Cu2 N2 2.077(3) . ?
Cu2 O2 2.277(3) . ?
Cu2 O11 2.725(4) . ?
O1 H1W 0.8583 . ?
O2 H2W 0.8594 . ?
O2 H3W 0.8548 . ?
O11 H4W 0.8626 . ?
O11 H5W 0.8582 . ?
N1 C1 1.308(4) . ?
N1 N2 1.375(3) . ?
N2 C2 1.304(4) . ?
N3 C1 1.351(4) . ?
N3 C2 1.356(4) . ?
N3 C7 1.490(4) . ?
N4 C3 1.284(5) . ?
N4 N5 1.381(5) . ?
N5 C4 1.302(5) . ?
N6 C3 1.330(5) . ?
N6 C4 1.353(4) . ?
N6 C9 1.483(4) . ?
N7 C5 1.303(5) . ?
N7 N8 1.388(4) . ?
N8 C6 1.297(4) . ?
N9 C6 1.351(4) . ?
N9 C5 1.358(4) . ?
N9 C11 1.482(4) . ?
N10 C15 1.469(4) . ?
N10 C14 1.472(4) . ?
N10 C13 1.472(4) . ?
C1 H1 0.8734 . ?
C2 H2 0.8629 . ?
C3 H3 1.0018 . ?
C4 H4 1.0015 . ?
C5 H5 0.9810 . ?
C6 H6 0.9352 . ?
C7 C13 1.537(4) . ?
C7 C8 1.538(4) . ?
C7 C12 1.539(4) . ?
C8 C9 1.543(4) . ?
C8 H8A 0.8772 . ?
C8 H8B 0.8772 . ?
C9 C10 1.539(4) . ?
C9 C14 1.541(5) . ?
C10 C11 1.532(4) . ?
C10 H10A 0.9667 . ?
C10 H10B 0.9667 . ?
C11 C12 1.537(4) . ?
C11 C15 1.542(5) . ?
C12 H12A 0.9381 . ?
C12 H12B 0.9381 . ?
C13 H13A 0.9177 . ?
C13 H13B 0.9177 . ?
C14 H14A 0.9234 . ?
C14 H14B 0.9234 . ?
C15 H15A 0.9610 . ?
C15 H15B 0.9610 . ?
Cl2 O8 1.410(4) . ?
Cl2 O7 1.420(3) . ?
Cl2 O9 1.421(5) . ?
Cl2 O10 1.423(4) . ?
Cl1 O3 1.412(4) . ?
Cl1 O4 1.421(4) . ?
Cl1 O5 1.421(5) . ?
Cl1 O6 1.441(4) . ?
Cl1A O6A 1.410(9) . ?
Cl1A O4A 1.411(9) . ?
Cl1A O3A 1.412(8) . ?
Cl1A O5A 1.412(9) . ?

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 Cu1 O1 180.0 5_656 . ?
O1 Cu1 N1 92.47(10) 5_656 . ?
O1 Cu1 N1 87.53(10) . . ?
O1 Cu1 N1 87.53(10) 5_656 5_656 ?
O1 Cu1 N1 92.47(10) . 5_656 ?
N1 Cu1 N1 180.0 . 5_656 ?
O1 Cu1 O5 92.9(2) 5_656 . ?
O1 Cu1 O5 87.1(2) . . ?
N1 Cu1 O5 90.53(14) . . ?
N1 Cu1 O5 89.47(14) 5_656 . ?
O1 Cu2 N5 177.08(11) . 4_655 ?
O1 Cu2 N8 86.96(10) . 8_566 ?
N5 Cu2 N8 95.45(11) 4_655 8_566 ?
O1 Cu2 N2 85.60(10) . . ?
N5 Cu2 N2 91.58(11) 4_655 . ?
N8 Cu2 N2 158.90(12) 8_566 . ?
O1 Cu2 O2 91.03(11) . . ?
N5 Cu2 O2 89.86(12) 4_655 . ?
N8 Cu2 O2 106.81(13) 8_566 . ?
N2 Cu2 O2 93.05(12) . . ?
O1 Cu2 O11 96.35(11) . . ?
N5 Cu2 O11 82.50(12) 4_655 . ?
N8 Cu2 O11 79.38(12) 8_566 . ?
N2 Cu2 O11 81.86(11) . . ?
O2 Cu2 O11 170.66(13) . . ?
Cu1 O1 Cu2 126.98(12) . . ?
Cu1 O1 H1W 118.0 . . ?
Cu2 O1 H1W 110.4 . . ?
Cu2 O2 H2W 110.5 . . ?
Cu2 O2 H3W 110.7 . . ?
H2W O2 H3W 107.3 . . ?
Cu2 O11 H4W 121.9 . . ?
Cu2 O11 H5W 107.9 . . ?
H4W O11 H5W 106.2 . . ?
C1 N1 N2 107.3(2) . . ?
C1 N1 Cu1 131.5(2) . . ?
N2 N1 Cu1 119.65(19) . . ?
C2 N2 N1 106.8(2) . . ?
C2 N2 Cu2 132.8(2) . . ?
N1 N2 Cu2 119.04(19) . . ?
C1 N3 C2 104.6(3) . . ?
C1 N3 C7 127.9(2) . . ?
C2 N3 C7 127.3(2) . . ?
C3 N4 N5 106.0(3) . . ?
C4 N5 N4 106.8(3) . . ?
C4 N5 Cu2 135.1(3) . 4_645 ?
N4 N5 Cu2 118.0(2) . 4_645 ?
C3 N6 C4 103.8(3) . . ?
C3 N6 C9 128.3(3) . . ?
C4 N6 C9 127.9(3) . . ?
C5 N7 N8 105.7(3) . . ?
C6 N8 N7 108.1(3) . . ?
C6 N8 Cu2 135.5(2) . 8_565 ?
N7 N8 Cu2 116.5(2) . 8_565 ?
C6 N9 C5 104.5(3) . . ?
C6 N9 C11 130.1(3) . . ?
C5 N9 C11 125.4(3) . . ?
C15 N10 C14 109.5(3) . . ?
C15 N10 C13 110.9(3) . . ?
C14 N10 C13 110.0(3) . . ?
N1 C1 N3 110.5(3) . . ?
N1 C1 H1 124.8 . . ?
N3 C1 H1 124.8 . . ?
N2 C2 N3 110.9(3) . . ?
N2 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
N4 C3 N6 112.8(4) . . ?
N4 C3 H3 123.6 . . ?
N6 C3 H3 123.6 . . ?
N5 C4 N6 110.5(3) . . ?
N5 C4 H4 124.7 . . ?
N6 C4 H4 124.7 . . ?
N7 C5 N9 111.3(3) . . ?
N7 C5 H5 124.3 . . ?
N9 C5 H5 124.3 . . ?
N8 C6 N9 110.4(3) . . ?
N8 C6 H6 124.8 . . ?
N9 C6 H6 124.8 . . ?
N3 C7 C13 109.8(2) . . ?
N3 C7 C8 110.2(2) . . ?
C13 C7 C8 109.4(2) . . ?
N3 C7 C12 108.4(2) . . ?
C13 C7 C12 109.2(3) . . ?
C8 C7 C12 109.7(2) . . ?
C7 C8 C9 107.7(3) . . ?
C7 C8 H8A 110.2 . . ?
C9 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
C9 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N6 C9 C10 109.5(2) . . ?
N6 C9 C14 109.4(2) . . ?
C10 C9 C14 109.7(3) . . ?
N6 C9 C8 109.3(3) . . ?
C10 C9 C8 109.7(2) . . ?
C14 C9 C8 109.3(3) . . ?
C11 C10 C9 107.4(2) . . ?
C11 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C11 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N9 C11 C10 110.0(3) . . ?
N9 C11 C12 108.0(2) . . ?
C10 C11 C12 109.9(3) . . ?
N9 C11 C15 110.0(3) . . ?
C10 C11 C15 110.0(3) . . ?
C12 C11 C15 108.8(3) . . ?
C11 C12 C7 108.2(2) . . ?
C11 C12 H12A 110.1 . . ?
C7 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
C7 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N10 C13 C7 110.3(3) . . ?
N10 C13 H13A 109.6 . . ?
C7 C13 H13A 109.6 . . ?
N10 C13 H13B 109.6 . . ?
C7 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
N10 C14 C9 110.5(3) . . ?
N10 C14 H14A 109.5 . . ?
C9 C14 H14A 109.5 . . ?
N10 C14 H14B 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N10 C15 C11 110.3(3) . . ?
N10 C15 H15A 109.6 . . ?
C11 C15 H15A 109.6 . . ?
N10 C15 H15B 109.6 . . ?
C11 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
O8 Cl2 O7 111.7(2) . . ?
O8 Cl2 O9 108.9(4) . . ?
O7 Cl2 O9 108.4(3) . . ?
O8 Cl2 O10 112.4(3) . . ?
O7 Cl2 O10 110.5(3) . . ?
O9 Cl2 O10 104.6(3) . . ?
O3 Cl1 O4 113.0(4) . . ?
O3 Cl1 O5 111.2(3) . . ?
O4 Cl1 O5 111.8(3) . . ?
O3 Cl1 O6 105.9(3) . . ?
O4 Cl1 O6 107.5(5) . . ?
O5 Cl1 O6 106.9(5) . . ?
Cl1 O5 Cu1 136.2(3) . . ?
O6A Cl1A O4A 109.6(8) . . ?
O6A Cl1A O3A 109.9(8) . . ?
O4A Cl1A O3A 109.3(8) . . ?
O6A Cl1A O5A 109.5(8) . . ?
O4A Cl1A O5A 109.4(8) . . ?
O3A Cl1A O5A 109.1(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cu1 O1 Cu2 -11.55(17) . . . . ?
N1 Cu1 O1 Cu2 168.45(17) 5_656 . . . ?
O5 Cu1 O1 Cu2 79.1(2) . . . . ?
N8 Cu2 O1 Cu1 171.84(19) 8_566 . . . ?
N2 Cu2 O1 Cu1 11.60(18) . . . . ?
O2 Cu2 O1 Cu1 -81.38(19) . . . . ?
O11 Cu2 O1 Cu1 92.89(18) . . . . ?
O1 Cu2 O11 O6A -6.6(6) . . . 5_656 ?
N5 Cu2 O11 O6A 170.7(6) 4_655 . . 5_656 ?
N8 Cu2 O11 O6A -92.3(6) 8_566 . . 5_656 ?
N2 Cu2 O11 O6A 78.0(6) . . . 5_656 ?
O1 Cu1 N1 C1 21.5(3) 5_656 . . . ?
O1 Cu1 N1 C1 -158.5(3) . . . . ?
O5 Cu1 N1 C1 114.4(4) . . . . ?
O1 Cu1 N1 N2 -174.5(2) 5_656 . . . ?
O1 Cu1 N1 N2 5.5(2) . . . . ?
O5 Cu1 N1 N2 -81.6(3) . . . . ?
C1 N1 N2 C2 -0.3(4) . . . . ?
Cu1 N1 N2 C2 -167.8(2) . . . . ?
C1 N1 N2 Cu2 168.1(2) . . . . ?
Cu1 N1 N2 Cu2 0.6(3) . . . . ?
O1 Cu2 N2 C2 158.5(3) . . . . ?
N5 Cu2 N2 C2 -20.7(3) 4_655 . . . ?
N8 Cu2 N2 C2 88.9(4) 8_566 . . . ?
O2 Cu2 N2 C2 -110.7(3) . . . . ?
O11 Cu2 N2 C2 61.5(3) . . . . ?
O1 Cu2 N2 N1 -6.3(2) . . . . ?
N5 Cu2 N2 N1 174.4(2) 4_655 . . . ?
N8 Cu2 N2 N1 -76.0(4) 8_566 . . . ?
O2 Cu2 N2 N1 84.5(2) . . . . ?
O11 Cu2 N2 N1 -103.4(2) . . . . ?
C3 N4 N5 C4 -1.7(5) . . . . ?
C3 N4 N5 Cu2 -178.5(3) . . . 4_645 ?
C5 N7 N8 C6 -0.2(4) . . . . ?
C5 N7 N8 Cu2 178.9(3) . . . 8_565 ?
N2 N1 C1 N3 0.4(4) . . . . ?
Cu1 N1 C1 N3 165.9(2) . . . . ?
C2 N3 C1 N1 -0.4(4) . . . . ?
C7 N3 C1 N1 -174.8(3) . . . . ?
N1 N2 C2 N3 0.1(4) . . . . ?
Cu2 N2 C2 N3 -166.1(2) . . . . ?
C1 N3 C2 N2 0.2(4) . . . . ?
C7 N3 C2 N2 174.7(3) . . . . ?
N5 N4 C3 N6 -0.9(6) . . . . ?
C4 N6 C3 N4 3.1(6) . . . . ?
C9 N6 C3 N4 -178.8(4) . . . . ?
N4 N5 C4 N6 3.7(4) . . . . ?
Cu2 N5 C4 N6 179.7(2) 4_645 . . . ?
C3 N6 C4 N5 -4.1(4) . . . . ?
C9 N6 C4 N5 177.7(3) . . . . ?
N8 N7 C5 N9 -0.4(5) . . . . ?
C6 N9 C5 N7 0.8(4) . . . . ?
C11 N9 C5 N7 -179.7(3) . . . . ?
N7 N8 C6 N9 0.8(4) . . . . ?
Cu2 N8 C6 N9 -178.1(3) 8_565 . . . ?
C5 N9 C6 N8 -1.0(4) . . . . ?
C11 N9 C6 N8 179.6(3) . . . . ?
C1 N3 C7 C13 76.3(4) . . . . ?
C2 N3 C7 C13 -97.0(4) . . . . ?
C1 N3 C7 C8 -44.4(4) . . . . ?
C2 N3 C7 C8 142.4(3) . . . . ?
C1 N3 C7 C12 -164.4(3) . . . . ?
C2 N3 C7 C12 22.3(4) . . . . ?
N3 C7 C8 C9 179.5(2) . . . . ?
C13 C7 C8 C9 58.6(3) . . . . ?
C12 C7 C8 C9 -61.2(3) . . . . ?
C3 N6 C9 C10 94.2(5) . . . . ?
C4 N6 C9 C10 -88.1(4) . . . . ?
C3 N6 C9 C14 -145.5(4) . . . . ?
C4 N6 C9 C14 32.2(4) . . . . ?
C3 N6 C9 C8 -25.9(5) . . . . ?
C4 N6 C9 C8 151.8(3) . . . . ?
C7 C8 C9 N6 -177.9(2) . . . . ?
C7 C8 C9 C10 62.1(3) . . . . ?
C7 C8 C9 C14 -58.1(3) . . . . ?
N6 C9 C10 C11 177.7(3) . . . . ?
C14 C9 C10 C11 57.6(3) . . . . ?
C8 C9 C10 C11 -62.4(3) . . . . ?
C6 N9 C11 C10 3.8(5) . . . . ?
C5 N9 C11 C10 -175.4(3) . . . . ?
C6 N9 C11 C12 123.8(4) . . . . ?
C5 N9 C11 C12 -55.5(4) . . . . ?
C6 N9 C11 C15 -117.6(4) . . . . ?
C5 N9 C11 C15 63.2(4) . . . . ?
C9 C10 C11 N9 -179.1(3) . . . . ?
C9 C10 C11 C12 62.0(3) . . . . ?
C9 C10 C11 C15 -57.8(3) . . . . ?
N9 C11 C12 C7 178.4(2) . . . . ?
C10 C11 C12 C7 -61.6(3) . . . . ?
C15 C11 C12 C7 58.9(3) . . . . ?
N3 C7 C12 C11 -178.6(2) . . . . ?
C13 C7 C12 C11 -58.9(3) . . . . ?
C8 C7 C12 C11 61.0(3) . . . . ?
C15 N10 C13 C7 -60.1(3) . . . . ?
C14 N10 C13 C7 61.1(3) . . . . ?
N3 C7 C13 N10 178.2(2) . . . . ?
C8 C7 C13 N10 -60.7(3) . . . . ?
C12 C7 C13 N10 59.4(3) . . . . ?
C15 N10 C14 C9 61.3(3) . . . . ?
C13 N10 C14 C9 -60.8(3) . . . . ?
N6 C9 C14 N10 179.5(3) . . . . ?
C10 C9 C14 N10 -60.4(3) . . . . ?
C8 C9 C14 N10 59.9(3) . . . . ?
C14 N10 C15 C11 -61.0(3) . . . . ?
C13 N10 C15 C11 60.5(3) . . . . ?
N9 C11 C15 N10 -178.2(2) . . . . ?
C10 C11 C15 N10 60.5(3) . . . . ?
C12 C11 C15 N10 -60.0(3) . . . . ?
O3 Cl1 O5 Cu1 -153.1(6) . . . . ?
O4 Cl1 O5 Cu1 -25.7(9) . . . . ?
O6 Cl1 O5 Cu1 91.8(7) . . . . ?
O1 Cu1 O5 Cl1 -70.4(8) 5_656 . . . ?
O1 Cu1 O5 Cl1 109.6(8) . . . . ?
N1 Cu1 O5 Cl1 -162.9(8) . . . . ?
N1 Cu1 O5 Cl1 17.1(8) 5_656 . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.098

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL IP699 in Pbca
CELL 0.71073 12.1931 17.2484 22.1135 90.000 90.000 90.000
ZERR 4.00 0.0007 0.0012 0.0011 0.000 0.000 0.000
LATT 1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM 1/2 + X, 1/2 - Y, - Z
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O CL CU
UNIT 120 184 80 88 16 12
MERG 2
OMIT 0.00 180.00
OMIT 0 8 3
OMIT 2 3 0
OMIT 3 6 6
SHEL 0.76 5
DFIX 1.42 0.01 Cl1A O3A Cl1A O4A Cl1A O5A Cl1A O6A
DFIX 2.30 0.01 O3A O4A O3A O5A O3A O6A O4A O5A O4A O6A O5A O6A
SIMU 0.005 O3A > O6A
FMAP 2
PLAN 25
ACTA
CONF
BOND $H

BIND Cu1 O5
BIND Cu2 O11

SIZE 0.13 0.16 0.24

L.S. 6
TEMP -60.00
WGHT 0.071800
FVAR 0.22536
CU1 6 0.500000 0.000000 0.500000 10.50000 0.03085 0.01143 =
0.01147 0.00133 -0.00082 0.00174
CU2 6 0.489716 0.193001 0.474193 11.00000 0.04104 0.01168 =
0.01392 -0.00017 0.00263 -0.00094
O1 4 0.482932 0.103688 0.524222 11.00000 0.05510 0.01236 =
0.01614 0.00119 0.00694 0.00498
AFIX 1
H1W 2 0.444400 0.112900 0.555900 11.00000 -1.50000
AFIX 0
O2 4 0.676321 0.191955 0.477577 11.00000 0.04077 0.04907 =
0.07553 0.01279 -0.00018 -0.00342
AFIX 1
H2W 2 0.699770 0.147860 0.490240 11.00000 -1.50000
H3W 2 0.700100 0.226460 0.502030 11.00000 -1.50000
AFIX 0
O11 4 0.270569 0.201546 0.451042 11.00000 0.07872 0.06110 =
0.06206 0.00089 0.00147 -0.00158
AFIX 1
H4W 2 0.245340 0.204260 0.414660 11.00000 -1.50000
H5W 2 0.239780 0.162000 0.467370 11.00000 -1.50000
AFIX 0
N1 3 0.489017 0.037414 0.413965 11.00000 0.02719 0.01366 =
0.01256 0.00129 -0.00093 0.00174
N2 3 0.484063 0.115648 0.402303 11.00000 0.03559 0.01146 =
0.01384 0.00005 -0.00122 -0.00094
N3 3 0.441984 0.052792 0.319408 11.00000 0.02797 0.01247 =
0.01096 0.00039 -0.00046 0.00072
N4 3 0.595733 -0.202571 0.118429 11.00000 0.04529 0.04851 =
0.07172 -0.03279 -0.01738 0.01463
N5 3 0.505491 -0.216099 0.082170 11.00000 0.04447 0.01766 =
0.01968 -0.00137 -0.00136 0.00195
N6 3 0.472447 -0.114971 0.138586 11.00000 0.03177 0.01658 =
0.01946 -0.00397 -0.00117 0.00207
N7 3 0.379314 0.286330 0.090540 11.00000 0.05817 0.02213 =
0.02461 0.00128 0.01009 0.00683
N8 3 0.437894 0.245601 0.047110 11.00000 0.03998 0.01787 =
0.01787 0.00163 0.00314 0.00116
N9 3 0.391279 0.163937 0.117454 11.00000 0.03696 0.01451 =
0.01494 0.00389 0.00044 0.00228
N10 3 0.236505 0.004693 0.197313 11.00000 0.02317 0.02710 =
0.01965 0.00051 -0.00111 -0.00464
C1 1 0.463158 0.001317 0.363951 11.00000 0.03159 0.01261 =
0.01317 -0.00046 -0.00033 0.00193
AFIX 44
H1 2 0.460018 -0.049004 0.359913 11.00000 -1.20000
AFIX 0
C2 1 0.455990 0.123124 0.345695 11.00000 0.04312 0.01375 =
0.01436 0.00119 0.00032 -0.00161
AFIX 44
H2 2 0.447477 0.166920 0.327431 11.00000 -1.20000
AFIX 0
C3 1 0.571468 -0.143215 0.150827 11.00000 0.04509 0.03987 =
0.06969 -0.02685 -0.01486 0.00634
AFIX 44
H3 2 0.621772 -0.120598 0.182001 11.00000 -1.20000
AFIX 0
C4 1 0.431983 -0.164664 0.096825 11.00000 0.03898 0.02235 =
0.02845 -0.00757 0.00084 0.00017
AFIX 44
H4 2 0.356100 -0.162224 0.079596 11.00000 -1.20000
AFIX 0
C5 1 0.353338 0.235637 0.131843 11.00000 0.05629 0.02276 =
0.02690 0.00348 0.01081 0.01027
AFIX 44
H5 2 0.311709 0.247726 0.168617 11.00000 -1.20000
AFIX 0
C6 1 0.444322 0.173864 0.064403 11.00000 0.03372 0.01881 =
0.01733 0.00065 0.00347 0.00097
AFIX 44
H6 2 0.480546 0.134601 0.043148 11.00000 -1.20000
AFIX 0
C7 1 0.401436 0.036657 0.257120 11.00000 0.02414 0.01649 =
0.00636 0.00014 -0.00169 0.00066
C8 1 0.463586 -0.032501 0.229686 11.00000 0.02734 0.01396 =
0.01333 -0.00001 -0.00129 -0.00072
AFIX 24
H8A 2 0.454414 -0.073889 0.252176 11.00000 -1.20000
H8B 2 0.533959 -0.022234 0.227742 11.00000 -1.20000
AFIX 0
C9 1 0.417313 -0.046639 0.165704 11.00000 0.02868 0.01126 =
0.01400 -0.00262 0.00155 0.00034
C10 1 0.438100 0.025074 0.125948 11.00000 0.03057 0.01528 =
0.01264 -0.00023 0.00131 -0.00037
AFIX 24
H10A 2 0.515684 0.036425 0.124282 11.00000 -1.20000
H10B 2 0.412205 0.015855 0.085259 11.00000 -1.20000
AFIX 0
C11 1 0.375798 0.093066 0.154370 11.00000 0.02863 0.01454 =
0.01319 0.00275 0.00063 0.00126
C12 1 0.420454 0.109350 0.218115 11.00000 0.02709 0.01239 =
0.01440 -0.00071 0.00040 -0.00083
AFIX 24
H12A 2 0.384037 0.152013 0.235111 11.00000 -1.20000
H12B 2 0.495597 0.120757 0.216209 11.00000 -1.20000
AFIX 0
C13 1 0.278166 0.018289 0.258899 11.00000 0.02586 0.02138 =
0.01909 -0.00042 0.00175 -0.00128
AFIX 24
H13A 2 0.266357 -0.024951 0.282183 11.00000 -1.20000
H13B 2 0.241047 0.058965 0.276118 11.00000 -1.20000
AFIX 0
C14 1 0.293089 -0.062109 0.170038 11.00000 0.03128 0.02218 =
0.02046 -0.00061 -0.00442 -0.00644
AFIX 24
H14A 2 0.265194 -0.071184 0.131867 11.00000 -1.20000
H14B 2 0.280855 -0.105755 0.193259 11.00000 -1.20000
AFIX 0
C15 1 0.252715 0.073438 0.159131 11.00000 0.02590 0.02813 =
0.02013 -0.00029 -0.00456 0.00232
AFIX 24
H15A 2 0.213919 0.116727 0.176190 11.00000 -1.20000
H15B 2 0.223595 0.063790 0.119454 11.00000 -1.20000
AFIX 0
CL2 5 0.660069 0.262414 0.209519 11.00000 0.05267 0.02419 =
0.04028 -0.00664 -0.00066 0.00068
O7 4 0.664027 0.193945 0.173892 11.00000 0.09984 0.03972 =
0.07559 -0.02888 0.03322 -0.01515
O8 4 0.582751 0.256214 0.256662 11.00000 0.16517 0.08429 =
0.11237 -0.05833 0.09960 -0.06073
O9 4 0.765573 0.275007 0.234933 11.00000 0.08685 0.11366 =
0.08140 -0.01217 -0.03060 0.00003
O10 4 0.641347 0.328421 0.172305 11.00000 0.12851 0.06182 =
0.07512 0.00953 -0.00382 0.04924
PART -1
CL1 5 0.800532 0.002075 0.535489 10.80000 0.02744 0.03488 =
0.02306 0.00614 0.00151 0.00098
O3 4 0.885346 0.057720 0.533181 10.80000 0.05604 0.07454 =
0.04739 0.01315 -0.00840 -0.03166
O4 4 0.768745 -0.017028 0.595482 10.80000 0.04098 0.13006 =
0.01892 0.02337 0.01093 -0.00101
O5 4 0.709418 0.025220 0.499696 10.80000 0.02473 0.09803 =
0.05288 0.04111 -0.01038 -0.00126
O6 4 0.844702 -0.067067 0.508166 10.80000 0.09785 0.03960 =
0.07792 -0.00603 0.02378 0.01776
PART -2
CL1A 5 0.783644 -0.039775 0.530241 10.20000 0.03210 0.09189 =
0.03051 -0.00236 0.00116 0.02194
O3A 4 0.894504 -0.025400 0.515651 10.20000 0.07208
O4A 4 0.768233 -0.029924 0.593016 10.20000 0.08561
O5A 4 0.716587 0.013229 0.498583 10.20000 0.08871
O6A 4 0.755195 -0.116091 0.513681 10.20000 0.07944
HKLF 4

REM IP699 in Pbca
REM R1 = 0.0432 for 3458 Fo > 4sig(Fo) and 0.0625 for all 5038 data
REM 395 parameters refined using 10 restraints

END

WGHT 0.0718 0.0000
REM Highest difference peak 0.790, deepest hole -0.594, 1-sigma level 0.098
Q1 1 0.5744 0.3012 0.1895 11.00000 0.05 0.79
Q2 1 0.6122 -0.1673 0.0824 11.00000 0.05 0.77
Q3 1 0.5886 -0.1097 0.1170 11.00000 0.05 0.76
Q4 1 0.6795 0.2189 0.5175 11.00000 0.05 0.64
Q5 1 0.7190 0.2778 0.1980 11.00000 0.05 0.58
Q6 1 0.8981 0.0103 0.5246 11.00000 0.05 0.58
Q7 1 0.7207 0.3188 0.2116 11.00000 0.05 0.57
Q8 1 0.4204 -0.2212 0.0648 11.00000 0.05 0.46
Q9 1 0.7699 -0.0564 0.4886 11.00000 0.05 0.46
Q10 1 0.4942 0.1310 0.4967 11.00000 0.05 0.43

;

#---------------------------------------------------------

data_(9)
_database_code_depnum_ccdc_archive 'CCDC 867232'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[3,5,7-tri(1,2,4-triazol-4-yl)-1-azaadamantane]-triaqua-
dicopper(II) Sulfate Heptahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Cu2 N20 O3, 2(O4 S), 7(H2 O)'
_chemical_formula_sum            'C30 H56 Cu2 N20 O18 S2'
_chemical_formula_weight         1176.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

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

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

_cell_length_a                   21.8567(15)
_cell_length_b                   11.5525(9)
_cell_length_c                   21.4604(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.611(4)
_cell_angle_gamma                90.00
_cell_volume                     4801.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      4.11
_cell_measurement_theta_max      25.87

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2440
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_T_max  0.8397
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19844
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.11
_diffrn_reflns_theta_max         25.87
_reflns_number_total             9003
_reflns_number_gt                6283
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The refinement was standard. All non-hydrogen atoms were refined
anisotropically. The CH-hydrogen atoms were constrained with U(iso) =
1.2U(eq) of the parent C-atom and with C-H distances 0.94 A (triazole),
0.97 A (CH2 azaadamantane). All the OH-hydrogen atoms were located and
then constrained with O-H distances set to 0.85 A and U(iso) = 1.5U(eq) of
the parent O-atom. The O-atoms for one of the SO4^2-^ anions and one of 7
solvate water molecules have slightly higher thermal parameters
[up to U(eq) = 0.123 A^2^], however there are no any signs of the
disorder.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9003
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.879
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.744931(19) 0.32630(2) 0.419404(19) 0.01914(9) Uani 1 1 d . . .
Cu2 Cu 0.756774(18) 0.30125(3) 0.602473(19) 0.01885(9) Uani 1 1 d . . .
S1 S 0.55444(4) 0.24923(6) 0.17969(4) 0.02802(17) Uani 1 1 d . . .
S2 S 0.86735(5) 0.52906(7) 0.29735(5) 0.0392(2) Uani 1 1 d . . .
O1 O 0.70961(12) 0.20357(16) 0.34650(12) 0.0297(5) Uani 1 1 d . . .
H1W H 0.6995 0.1361 0.3546 0.045 Uiso 1 1 d R . .
H2W H 0.6836 0.2197 0.3035 0.045 Uiso 1 1 d R . .
O2 O 0.84929(13) 0.31764(18) 0.40978(13) 0.0371(5) Uani 1 1 d . . .
H3W H 0.8495 0.3555 0.3759 0.056 Uiso 1 1 d R . .
H4W H 0.8840 0.3386 0.4476 0.056 Uiso 1 1 d R . .
O3 O 0.72845(12) 0.16619(16) 0.66363(12) 0.0306(5) Uani 1 1 d . . .
H5W H 0.6973 0.1881 0.6742 0.046 Uiso 1 1 d R . .
H6W H 0.7619 0.1390 0.7004 0.046 Uiso 1 1 d R . .
O4 O 0.51965(17) 0.3632(2) 0.16707(18) 0.0585(8) Uani 1 1 d . . .
O5 O 0.53869(15) 0.1807(2) 0.22832(14) 0.0461(6) Uani 1 1 d . . .
O6 O 0.53120(16) 0.1883(2) 0.11164(15) 0.0519(7) Uani 1 1 d . . .
O7 O 0.63078(13) 0.2657(2) 0.21155(13) 0.0398(6) Uani 1 1 d . . .
O8 O 0.8409(2) 0.6119(2) 0.33122(18) 0.0650(9) Uani 1 1 d . . .
O9 O 0.83058(15) 0.4174(2) 0.28849(14) 0.0450(6) Uani 1 1 d . . .
O10 O 0.8523(3) 0.5711(3) 0.2268(2) 0.0871(14) Uani 1 1 d . . .
O11 O 0.9413(2) 0.5084(3) 0.3433(3) 0.1093(17) Uani 1 1 d . . .
N1 N 0.79112(14) 0.45610(18) 0.48675(13) 0.0235(5) Uani 1 1 d . . .
N2 N 0.78699(15) 0.46706(19) 0.54803(14) 0.0284(6) Uani 1 1 d . . .
N3 N 0.84907(14) 0.61079(18) 0.53973(14) 0.0235(5) Uani 1 1 d . . .
N4 N 0.79626(13) 1.20053(18) 0.49529(13) 0.0215(5) Uani 1 1 d . . .
N5 N 0.78872(13) 1.18071(17) 0.55490(13) 0.0208(5) Uani 1 1 d . . .
N6 N 0.84942(13) 1.03911(17) 0.54394(13) 0.0199(5) Uani 1 1 d . . .
N7 N 1.14259(13) 0.81029(19) 0.82263(14) 0.0247(5) Uani 1 1 d . . .
N8 N 1.09019(15) 0.8199(3) 0.84177(16) 0.0389(7) Uani 1 1 d . . .
N9 N 1.04440(13) 0.82214(19) 0.72592(14) 0.0242(5) Uani 1 1 d . . .
N10 N 0.97355(14) 0.82778(19) 0.52902(14) 0.0243(5) Uani 1 1 d . . .
N11 N 0.65948(13) 0.29143(19) 0.45152(13) 0.0230(5) Uani 1 1 d . . .
N12 N 0.66216(13) 0.29370(18) 0.51753(13) 0.0209(5) Uani 1 1 d . . .
N13 N 0.55565(13) 0.25648(17) 0.43952(13) 0.0196(5) Uani 1 1 d . . .
N14 N 0.31238(14) -0.05281(18) 0.15110(14) 0.0240(5) Uani 1 1 d . . .
N15 N 0.36167(18) 0.0056(2) 0.14051(18) 0.0436(8) Uani 1 1 d . . .
N16 N 0.36462(13) 0.06625(18) 0.23905(13) 0.0227(5) Uani 1 1 d . . .
N17 N 0.27328(14) 0.57805(19) 0.35149(13) 0.0235(5) Uani 1 1 d . . .
N18 N 0.24677(15) 0.5636(2) 0.27962(14) 0.0314(6) Uani 1 1 d . . .
N19 N 0.32019(14) 0.42311(19) 0.33558(14) 0.0240(5) Uani 1 1 d . . .
N20 N 0.38853(14) 0.13222(19) 0.42148(14) 0.0243(6) Uani 1 1 d . . .
C1 C 0.82733(17) 0.5422(2) 0.48172(17) 0.0265(7) Uani 1 1 d . . .
H1 H 0.8369 0.5549 0.4439 0.032 Uiso 1 1 calc R . .
C2 C 0.82225(19) 0.5606(2) 0.57948(19) 0.0314(7) Uani 1 1 d . . .
H2 H 0.8282 0.5888 0.6230 0.038 Uiso 1 1 calc R . .
C3 C 0.89245(16) 0.7169(2) 0.55734(16) 0.0226(6) Uani 1 1 d . . .
C4 C 0.84571(15) 0.8248(2) 0.54238(16) 0.0208(6) Uani 1 1 d . . .
H4A H 0.8106 0.8259 0.4929 0.025 Uiso 1 1 calc R . .
H4B H 0.8223 0.8236 0.5718 0.025 Uiso 1 1 calc R . .
C5 C 0.89246(16) 0.9326(2) 0.55935(16) 0.0200(6) Uani 1 1 d . . .
C6 C 0.94637(15) 0.9331(2) 0.63702(16) 0.0197(6) Uani 1 1 d . . .
H6A H 0.9234 0.9326 0.6669 0.024 Uiso 1 1 calc R . .
H6B H 0.9750 1.0029 0.6477 0.024 Uiso 1 1 calc R . .
C7 C 0.99190(15) 0.8238(2) 0.65130(16) 0.0213(6) Uani 1 1 d . . .
C8 C 0.94693(16) 0.7136(2) 0.63556(16) 0.0231(6) Uani 1 1 d . . .
H8A H 0.9758 0.6443 0.6450 0.028 Uiso 1 1 calc R . .
H8B H 0.9241 0.7113 0.6655 0.028 Uiso 1 1 calc R . .
C9 C 0.93025(17) 0.7226(2) 0.51170(17) 0.0240(6) Uani 1 1 d . . .
H9A H 0.9593 0.6538 0.5203 0.029 Uiso 1 1 calc R . .
H9B H 0.8963 0.7237 0.4618 0.029 Uiso 1 1 calc R . .
C10 C 0.92880(17) 0.9314(2) 0.51279(17) 0.0235(6) Uani 1 1 d . . .
H10A H 0.8943 0.9303 0.4631 0.028 Uiso 1 1 calc R . .
H10B H 0.9568 1.0015 0.5213 0.028 Uiso 1 1 calc R . .
C11 C 1.02636(16) 0.8271(2) 0.60304(17) 0.0265(6) Uani 1 1 d . . .
H11A H 1.0551 0.8967 0.6131 0.032 Uiso 1 1 calc R . .
H11B H 1.0562 0.7593 0.6121 0.032 Uiso 1 1 calc R . .
C12 C 0.82089(16) 1.0838(2) 0.58321(16) 0.0218(6) Uani 1 1 d . . .
H12 H 0.8238 1.0503 0.6244 0.026 Uiso 1 1 calc R . .
C13 C 0.83244(16) 1.1153(2) 0.48987(16) 0.0232(6) Uani 1 1 d . . .
H13 H 0.8451 1.1073 0.4538 0.028 Uiso 1 1 calc R . .
C14 C 1.11368(16) 0.8115(2) 0.75369(17) 0.0244(6) Uani 1 1 d . . .
H14 H 1.1379 0.8058 0.7272 0.029 Uiso 1 1 calc R . .
C15 C 1.03266(19) 0.8267(3) 0.78314(19) 0.0403(8) Uani 1 1 d . . .
H15 H 0.9887 0.8338 0.7806 0.048 Uiso 1 1 calc R . .
C16 C 0.59554(16) 0.2688(2) 0.40606(17) 0.0231(6) Uani 1 1 d . . .
H16 H 0.5792 0.2619 0.3573 0.028 Uiso 1 1 calc R . .
C17 C 0.59944(16) 0.2734(2) 0.50877(16) 0.0225(6) Uani 1 1 d . . .
H17 H 0.5868 0.2710 0.5451 0.027 Uiso 1 1 calc R . .
C18 C 0.48039(15) 0.2321(2) 0.40544(15) 0.0194(6) Uani 1 1 d . . .
C19 C 0.46091(15) 0.1627(2) 0.33755(16) 0.0208(6) Uani 1 1 d . . .
H19A H 0.4706 0.2085 0.3047 0.025 Uiso 1 1 calc R . .
H19B H 0.4881 0.0913 0.3484 0.025 Uiso 1 1 calc R . .
C20 C 0.38378(15) 0.1340(2) 0.30450(16) 0.0205(6) Uani 1 1 d . . .
C21 C 0.34073(16) 0.2460(2) 0.28464(16) 0.0221(6) Uani 1 1 d . . .
H21A H 0.2914 0.2276 0.2628 0.027 Uiso 1 1 calc R . .
H21B H 0.3498 0.2913 0.2512 0.027 Uiso 1 1 calc R . .
C22 C 0.36200(16) 0.3152(2) 0.35307(16) 0.0222(6) Uani 1 1 d . . .
C23 C 0.43916(16) 0.3463(2) 0.38785(16) 0.0208(6) Uani 1 1 d . . .
H23A H 0.4517 0.3911 0.4309 0.025 Uiso 1 1 calc R . .
H23B H 0.4494 0.3930 0.3557 0.025 Uiso 1 1 calc R . .
C24 C 0.46286(16) 0.1592(2) 0.45544(16) 0.0233(6) Uani 1 1 d . . .
H24A H 0.4896 0.0872 0.4675 0.028 Uiso 1 1 calc R . .
H24B H 0.4754 0.2024 0.4990 0.028 Uiso 1 1 calc R . .
C25 C 0.36852(17) 0.0637(2) 0.35641(17) 0.0252(7) Uani 1 1 d . . .
H25A H 0.3192 0.0450 0.3350 0.030 Uiso 1 1 calc R . .
H25B H 0.3945 -0.0090 0.3678 0.030 Uiso 1 1 calc R . .
C26 C 0.34738(16) 0.2405(2) 0.40444(17) 0.0247(6) Uani 1 1 d . . .
H26A H 0.3593 0.2842 0.4477 0.030 Uiso 1 1 calc R . .
H26B H 0.2981 0.2216 0.3830 0.030 Uiso 1 1 calc R . .
C27 C 0.31495(16) -0.0151(2) 0.20956(16) 0.0237(6) Uani 1 1 d . . .
H27 H 0.2863 -0.0410 0.2285 0.028 Uiso 1 1 calc R . .
C28 C 0.3918(2) 0.0762(3) 0.1939(2) 0.0441(10) Uani 1 1 d . . .
H28 H 0.4277 0.1272 0.2002 0.053 Uiso 1 1 calc R . .
C29 C 0.31715(16) 0.4951(2) 0.38386(17) 0.0239(6) Uani 1 1 d . . .
H29 H 0.3426 0.4867 0.4329 0.029 Uiso 1 1 calc R . .
C30 C 0.27617(19) 0.4696(3) 0.27235(18) 0.0326(7) Uani 1 1 d . . .
H30 H 0.2678 0.4380 0.2287 0.039 Uiso 1 1 calc R . .
O1W O 0.55759(18) 0.9397(2) 0.26155(17) 0.0610(9) Uani 1 1 d . . .
H7W H 0.5317 0.9180 0.2791 0.091 Uiso 1 1 d R . .
H8W H 0.5480 1.0097 0.2485 0.091 Uiso 1 1 d R . .
O2W O 0.68297(19) 0.9879(2) 0.38001(19) 0.0691(9) Uani 1 1 d . . .
H9W H 0.6510 0.9592 0.3426 0.104 Uiso 1 1 d R . .
H10W H 0.6678 0.9957 0.4098 0.104 Uiso 1 1 d R . .
O3W O 0.6006(2) 0.9614(3) 0.44721(18) 0.0769(10) Uani 1 1 d . . .
H11W H 0.5676 0.9186 0.4193 0.115 Uiso 1 1 d R . .
H12W H 0.6072 0.9487 0.4889 0.115 Uiso 1 1 d R . .
O4W O 0.8374(2) 0.8060(3) 0.21069(19) 0.0723(10) Uani 1 1 d . . .
H13W H 0.8401 0.7326 0.2128 0.108 Uiso 1 1 d R . .
H14W H 0.8583 0.8326 0.2523 0.108 Uiso 1 1 d R . .
O5W O 0.41709(16) 0.0485(2) 0.04195(14) 0.0503(7) Uani 1 1 d . . .
H15W H 0.4005 0.0262 0.0688 0.075 Uiso 1 1 d R . .
H16W H 0.4545 0.0847 0.0667 0.075 Uiso 1 1 d R . .
O6W O 1.04413(19) 0.6337(3) 0.44978(18) 0.0794(11) Uani 1 1 d . . .
H17W H 1.0692 0.6508 0.4304 0.119 Uiso 1 1 d R . .
H18W H 1.0087 0.5977 0.4200 0.119 Uiso 1 1 d R . .
O7W O 0.9289(3) 0.8266(3) 0.3645(2) 0.123(2) Uani 1 1 d . . .
H19W H 0.9138 0.7582 0.3627 0.185 Uiso 1 1 d R . .
H20W H 0.9493 0.8478 0.4072 0.185 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.02084(19) 0.01532(14) 0.0189(2) 0.00163(12) 0.00725(16) 0.00261(12)
Cu2 0.01649(18) 0.01918(15) 0.0193(2) -0.00222(12) 0.00689(16) 0.00304(13)
S1 0.0281(4) 0.0312(3) 0.0254(5) -0.0008(3) 0.0130(4) -0.0076(3)
S2 0.0376(5) 0.0424(4) 0.0450(6) -0.0065(4) 0.0252(5) -0.0074(4)
O1 0.0373(13) 0.0246(9) 0.0212(12) -0.0019(8) 0.0085(11) -0.0023(9)
O2 0.0378(14) 0.0409(12) 0.0376(15) 0.0008(10) 0.0216(13) 0.0002(10)
O3 0.0323(13) 0.0298(10) 0.0348(14) 0.0051(9) 0.0199(12) 0.0013(9)
O4 0.059(2) 0.0465(14) 0.074(2) 0.0117(14) 0.0344(19) 0.0096(13)
O5 0.0490(17) 0.0535(14) 0.0457(17) 0.0051(12) 0.0302(15) -0.0106(12)
O6 0.0514(18) 0.0671(16) 0.0373(16) -0.0165(13) 0.0205(15) -0.0251(14)
O7 0.0302(14) 0.0573(14) 0.0323(15) 0.0004(11) 0.0147(12) -0.0125(11)
O8 0.093(3) 0.0534(16) 0.066(2) -0.0088(14) 0.052(2) 0.0001(16)
O9 0.0518(18) 0.0442(13) 0.0408(17) -0.0055(11) 0.0229(15) -0.0130(12)
O10 0.165(4) 0.0587(18) 0.076(3) -0.0062(16) 0.088(3) -0.017(2)
O11 0.039(2) 0.080(2) 0.175(5) -0.025(3) 0.020(3) -0.0045(17)
N1 0.0250(14) 0.0208(10) 0.0235(15) -0.0002(9) 0.0103(12) 0.0001(10)
N2 0.0358(17) 0.0245(11) 0.0279(16) -0.0045(10) 0.0174(14) -0.0068(11)
N3 0.0293(15) 0.0167(10) 0.0262(15) -0.0012(9) 0.0143(13) -0.0007(9)
N4 0.0250(14) 0.0186(10) 0.0216(14) 0.0005(9) 0.0116(12) 0.0031(9)
N5 0.0229(13) 0.0180(10) 0.0230(14) 0.0009(9) 0.0120(12) 0.0029(9)
N6 0.0224(14) 0.0159(10) 0.0237(14) 0.0016(9) 0.0125(12) 0.0033(9)
N7 0.0187(13) 0.0285(12) 0.0273(16) 0.0033(10) 0.0110(12) 0.0012(10)
N8 0.0208(15) 0.0690(19) 0.0281(17) 0.0029(14) 0.0124(14) 0.0037(14)
N9 0.0184(13) 0.0268(11) 0.0254(15) 0.0004(10) 0.0085(12) 0.0028(10)
N10 0.0260(14) 0.0226(10) 0.0292(15) -0.0007(10) 0.0171(13) 0.0037(10)
N11 0.0207(13) 0.0277(11) 0.0202(14) 0.0008(9) 0.0092(12) -0.0017(10)
N12 0.0211(13) 0.0205(10) 0.0201(14) -0.0001(9) 0.0086(11) 0.0024(9)
N13 0.0177(13) 0.0199(10) 0.0212(15) -0.0021(9) 0.0090(12) 0.0000(9)
N14 0.0248(14) 0.0219(11) 0.0246(15) -0.0026(9) 0.0109(13) -0.0041(10)
N15 0.050(2) 0.0489(16) 0.046(2) -0.0241(14) 0.0337(18) -0.0288(14)
N16 0.0218(14) 0.0217(11) 0.0251(15) -0.0079(9) 0.0113(12) -0.0041(9)
N17 0.0239(14) 0.0249(11) 0.0218(15) -0.0023(9) 0.0107(12) 0.0035(10)
N18 0.0338(16) 0.0350(13) 0.0230(16) -0.0011(10) 0.0112(14) 0.0115(11)
N19 0.0236(14) 0.0236(11) 0.0249(15) -0.0027(10) 0.0112(12) 0.0050(10)
N20 0.0268(15) 0.0222(11) 0.0268(16) -0.0029(9) 0.0149(13) -0.0037(10)
C1 0.0324(18) 0.0224(13) 0.0265(18) 0.0004(11) 0.0152(16) -0.0010(12)
C2 0.040(2) 0.0274(14) 0.033(2) -0.0040(12) 0.0229(18) -0.0061(13)
C3 0.0263(16) 0.0144(11) 0.0277(18) -0.0001(10) 0.0130(15) 0.0005(11)
C4 0.0183(14) 0.0198(12) 0.0226(16) -0.0004(10) 0.0082(13) 0.0024(11)
C5 0.0230(16) 0.0144(11) 0.0252(17) 0.0020(10) 0.0134(14) 0.0051(10)
C6 0.0162(15) 0.0191(12) 0.0241(17) -0.0010(10) 0.0097(13) 0.0008(10)
C7 0.0185(15) 0.0205(12) 0.0228(16) 0.0019(11) 0.0078(13) 0.0038(11)
C8 0.0224(16) 0.0185(12) 0.0270(18) 0.0025(11) 0.0104(14) 0.0039(11)
C9 0.0293(17) 0.0182(12) 0.0278(18) -0.0022(11) 0.0159(15) 0.0005(11)
C10 0.0280(17) 0.0195(12) 0.0274(18) 0.0011(11) 0.0165(15) 0.0032(11)
C11 0.0223(16) 0.0284(13) 0.0296(19) 0.0002(12) 0.0128(15) 0.0035(12)
C12 0.0240(17) 0.0207(12) 0.0223(17) 0.0024(10) 0.0121(15) 0.0044(11)
C13 0.0267(17) 0.0218(12) 0.0235(17) 0.0024(11) 0.0138(15) 0.0046(11)
C14 0.0191(15) 0.0252(13) 0.0287(19) 0.0005(11) 0.0110(14) 0.0005(11)
C15 0.0212(18) 0.071(2) 0.031(2) 0.0026(17) 0.0142(17) 0.0040(16)
C16 0.0212(16) 0.0282(13) 0.0185(17) 0.0014(11) 0.0079(14) -0.0011(11)
C17 0.0215(16) 0.0245(13) 0.0212(17) -0.0029(11) 0.0098(14) 0.0006(11)
C18 0.0170(15) 0.0196(12) 0.0196(17) -0.0030(10) 0.0066(13) -0.0005(10)
C19 0.0222(16) 0.0180(11) 0.0225(17) -0.0040(10) 0.0106(14) 0.0008(10)
C20 0.0200(16) 0.0200(12) 0.0217(17) -0.0086(10) 0.0097(14) -0.0031(10)
C21 0.0180(15) 0.0234(12) 0.0233(17) -0.0041(11) 0.0082(14) -0.0001(11)
C22 0.0216(15) 0.0193(12) 0.0262(17) -0.0046(11) 0.0114(14) 0.0029(11)
C23 0.0222(16) 0.0170(12) 0.0230(17) -0.0039(10) 0.0102(14) 0.0004(10)
C24 0.0242(16) 0.0223(12) 0.0254(18) -0.0019(11) 0.0133(15) -0.0014(11)
C25 0.0299(18) 0.0206(12) 0.0284(19) -0.0047(11) 0.0163(16) -0.0063(11)
C26 0.0217(16) 0.0281(13) 0.0265(18) -0.0057(11) 0.0131(15) -0.0023(11)
C27 0.0237(17) 0.0228(13) 0.0262(18) -0.0033(11) 0.0130(15) -0.0034(11)
C28 0.051(3) 0.0494(19) 0.048(2) -0.0289(17) 0.037(2) -0.0314(17)
C29 0.0234(17) 0.0241(13) 0.0219(18) -0.0042(11) 0.0085(15) 0.0037(11)
C30 0.035(2) 0.0354(15) 0.0224(19) -0.0028(13) 0.0090(16) 0.0109(14)
O1W 0.083(3) 0.0527(15) 0.069(2) -0.0078(14) 0.053(2) -0.0031(15)
O2W 0.078(3) 0.0587(17) 0.076(2) 0.0072(15) 0.040(2) -0.0139(16)
O3W 0.083(3) 0.097(2) 0.049(2) 0.0138(17) 0.029(2) -0.024(2)
O4W 0.085(3) 0.075(2) 0.065(2) 0.0295(17) 0.041(2) 0.0167(18)
O5W 0.0520(18) 0.0651(16) 0.0294(16) -0.0041(12) 0.0152(14) -0.0256(13)
O6W 0.050(2) 0.144(3) 0.047(2) -0.014(2) 0.0239(19) -0.019(2)
O7W 0.232(7) 0.081(3) 0.075(3) 0.001(2) 0.087(4) 0.004(3)

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

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 O1 1.984(2) . ?
Cu1 N1 2.001(2) . ?
Cu1 N14 2.013(2) 2_655 ?
Cu1 N4 2.080(2) 1_545 ?
Cu1 N11 2.306(2) . ?
Cu1 O2 2.386(2) . ?
Cu2 N17 1.988(2) 3_666 ?
Cu2 N12 2.028(3) . ?
Cu2 N5 2.032(2) 1_545 ?
Cu2 N7 2.038(3) 2_746 ?
Cu2 O3 2.301(2) . ?
Cu2 N2 2.487(2) . ?
S1 O5 1.472(2) . ?
S1 O4 1.481(3) . ?
S1 O6 1.483(3) . ?
S1 O7 1.493(3) . ?
S2 O11 1.470(4) . ?
S2 O8 1.473(3) . ?
S2 O10 1.475(3) . ?
S2 O9 1.485(2) . ?
O1 H1W 0.8500 . ?
O1 H2W 0.8499 . ?
O2 H3W 0.8499 . ?
O2 H4W 0.8500 . ?
O3 H5W 0.8501 . ?
O3 H6W 0.8499 . ?
N1 C1 1.306(4) . ?
N1 N2 1.365(3) . ?
N2 C2 1.317(4) . ?
N3 C1 1.362(4) . ?
N3 C2 1.368(4) . ?
N3 C3 1.488(3) . ?
N4 C13 1.302(3) . ?
N4 N5 1.383(3) . ?
N4 Cu1 2.080(2) 1_565 ?
N5 C12 1.312(3) . ?
N5 Cu2 2.032(2) 1_565 ?
N6 C12 1.361(4) . ?
N6 C13 1.364(4) . ?
N6 C5 1.490(3) . ?
N7 C14 1.312(4) . ?
N7 N8 1.389(4) . ?
N7 Cu2 2.038(3) 2_756 ?
N8 C15 1.305(5) . ?
N9 C14 1.352(4) . ?
N9 C15 1.367(4) . ?
N9 C7 1.476(4) . ?
N10 C11 1.468(4) . ?
N10 C9 1.478(4) . ?
N10 C10 1.481(3) . ?
N11 C16 1.307(4) . ?
N11 N12 1.391(3) . ?
N12 C17 1.315(4) . ?
N13 C17 1.358(4) . ?
N13 C16 1.370(4) . ?
N13 C18 1.485(4) . ?
N14 C27 1.304(4) . ?
N14 N15 1.376(4) . ?
N14 Cu1 2.013(2) 2_645 ?
N15 C28 1.308(4) . ?
N16 C27 1.351(4) . ?
N16 C28 1.356(4) . ?
N16 C20 1.488(3) . ?
N17 C29 1.305(4) . ?
N17 N18 1.384(4) . ?
N17 Cu2 1.988(2) 3_666 ?
N18 C30 1.308(4) . ?
N19 C29 1.354(4) . ?
N19 C30 1.358(4) . ?
N19 C22 1.487(3) . ?
N20 C24 1.473(4) . ?
N20 C25 1.484(4) . ?
N20 C26 1.484(4) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 C8 1.544(4) . ?
C3 C4 1.548(4) . ?
C3 C9 1.548(4) . ?
C4 C5 1.543(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.532(4) . ?
C5 C10 1.538(4) . ?
C6 C7 1.548(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C11 1.538(4) . ?
C7 C8 1.547(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12 0.9400 . ?
C13 H13 0.9400 . ?
C14 H14 0.9400 . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
C18 C19 1.540(4) . ?
C18 C23 1.543(3) . ?
C18 C24 1.545(4) . ?
C19 C20 1.532(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 C25 1.535(4) . ?
C20 C21 1.540(4) . ?
C21 C22 1.542(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 C23 1.537(4) . ?
C22 C26 1.545(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27 0.9400 . ?
C28 H28 0.9400 . ?
C29 H29 0.9400 . ?
C30 H30 0.9400 . ?
O1W H7W 0.8500 . ?
O1W H8W 0.8499 . ?
O2W H9W 0.8501 . ?
O2W H10W 0.8501 . ?
O3W H11W 0.8501 . ?
O3W H12W 0.8500 . ?
O4W H13W 0.8500 . ?
O4W H14W 0.8500 . ?
O5W H15W 0.8500 . ?
O5W H16W 0.8501 . ?
O6W H17W 0.8501 . ?
O6W H18W 0.8500 . ?
O7W H19W 0.8499 . ?
O7W H20W 0.8500 . ?

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 Cu1 N1 170.75(10) . . ?
O1 Cu1 N14 91.37(10) . 2_655 ?
N1 Cu1 N14 87.30(10) . 2_655 ?
O1 Cu1 N4 89.42(9) . 1_545 ?
N1 Cu1 N4 92.83(10) . 1_545 ?
N14 Cu1 N4 174.19(10) 2_655 1_545 ?
O1 Cu1 N11 92.17(9) . . ?
N1 Cu1 N11 97.03(9) . . ?
N14 Cu1 N11 92.16(10) 2_655 . ?
N4 Cu1 N11 82.05(9) 1_545 . ?
O1 Cu1 O2 86.56(9) . . ?
N1 Cu1 O2 84.92(9) . . ?
N14 Cu1 O2 104.53(9) 2_655 . ?
N4 Cu1 O2 81.27(9) 1_545 . ?
N11 Cu1 O2 163.28(8) . . ?
N17 Cu2 N12 92.45(10) 3_666 . ?
N17 Cu2 N5 178.69(10) 3_666 1_545 ?
N12 Cu2 N5 87.91(10) . 1_545 ?
N17 Cu2 N7 93.24(10) 3_666 2_746 ?
N12 Cu2 N7 171.53(10) . 2_746 ?
N5 Cu2 N7 86.26(10) 1_545 2_746 ?
N17 Cu2 O3 87.36(9) 3_666 . ?
N12 Cu2 O3 92.97(9) . . ?
N5 Cu2 O3 93.88(8) 1_545 . ?
N7 Cu2 O3 93.57(9) 2_746 . ?
N17 Cu2 N2 85.07(9) 3_666 . ?
N12 Cu2 N2 89.60(9) . . ?
N5 Cu2 N2 93.66(8) 1_545 . ?
N7 Cu2 N2 84.64(10) 2_746 . ?
O3 Cu2 N2 172.11(8) . . ?
O5 S1 O4 109.80(16) . . ?
O5 S1 O6 110.92(15) . . ?
O4 S1 O6 109.22(19) . . ?
O5 S1 O7 108.84(16) . . ?
O4 S1 O7 109.88(16) . . ?
O6 S1 O7 108.15(16) . . ?
O11 S2 O8 109.6(2) . . ?
O11 S2 O10 113.3(3) . . ?
O8 S2 O10 109.9(2) . . ?
O11 S2 O9 107.8(2) . . ?
O8 S2 O9 108.35(17) . . ?
O10 S2 O9 107.75(19) . . ?
Cu1 O1 H1W 122.4 . . ?
Cu1 O1 H2W 121.3 . . ?
H1W O1 H2W 108.5 . . ?
Cu1 O2 H3W 115.8 . . ?
Cu1 O2 H4W 111.7 . . ?
H3W O2 H4W 108.4 . . ?
Cu2 O3 H5W 114.2 . . ?
Cu2 O3 H6W 116.0 . . ?
H5W O3 H6W 108.2 . . ?
C1 N1 N2 108.8(2) . . ?
C1 N1 Cu1 129.3(2) . . ?
N2 N1 Cu1 121.93(17) . . ?
C2 N2 N1 106.6(2) . . ?
C2 N2 Cu2 127.6(2) . . ?
N1 N2 Cu2 122.11(16) . . ?
C1 N3 C2 104.7(2) . . ?
C1 N3 C3 128.5(2) . . ?
C2 N3 C3 126.7(2) . . ?
C13 N4 N5 107.2(2) . . ?
C13 N4 Cu1 126.0(2) . 1_565 ?
N5 N4 Cu1 126.00(16) . 1_565 ?
C12 N5 N4 107.6(2) . . ?
C12 N5 Cu2 126.0(2) . 1_565 ?
N4 N5 Cu2 124.56(15) . 1_565 ?
C12 N6 C13 105.1(2) . . ?
C12 N6 C5 126.8(2) . . ?
C13 N6 C5 128.1(2) . . ?
C14 N7 N8 107.5(3) . . ?
C14 N7 Cu2 132.0(2) . 2_756 ?
N8 N7 Cu2 120.5(2) . 2_756 ?
C15 N8 N7 106.1(3) . . ?
C14 N9 C15 104.2(3) . . ?
C14 N9 C7 128.9(2) . . ?
C15 N9 C7 126.8(3) . . ?
C11 N10 C9 111.0(2) . . ?
C11 N10 C10 111.1(2) . . ?
C9 N10 C10 109.2(2) . . ?
C16 N11 N12 106.8(2) . . ?
C16 N11 Cu1 123.1(2) . . ?
N12 N11 Cu1 130.06(18) . . ?
C17 N12 N11 107.6(2) . . ?
C17 N12 Cu2 134.2(2) . . ?
N11 N12 Cu2 117.42(18) . . ?
C17 N13 C16 105.2(2) . . ?
C17 N13 C18 128.6(2) . . ?
C16 N13 C18 126.2(3) . . ?
C27 N14 N15 107.9(2) . . ?
C27 N14 Cu1 133.5(2) . 2_645 ?
N15 N14 Cu1 118.56(19) . 2_645 ?
C28 N15 N14 106.0(3) . . ?
C27 N16 C28 104.3(2) . . ?
C27 N16 C20 128.4(2) . . ?
C28 N16 C20 127.2(2) . . ?
C29 N17 N18 109.3(2) . . ?
C29 N17 Cu2 125.5(2) . 3_666 ?
N18 N17 Cu2 125.04(19) . 3_666 ?
C30 N18 N17 104.9(3) . . ?
C29 N19 C30 105.0(2) . . ?
C29 N19 C22 124.3(3) . . ?
C30 N19 C22 130.6(2) . . ?
C24 N20 C25 110.8(2) . . ?
C24 N20 C26 110.3(2) . . ?
C25 N20 C26 109.7(2) . . ?
N1 C1 N3 109.6(3) . . ?
N1 C1 H1 125.2 . . ?
N3 C1 H1 125.2 . . ?
N2 C2 N3 110.3(3) . . ?
N2 C2 H2 124.9 . . ?
N3 C2 H2 124.9 . . ?
N3 C3 C8 109.6(2) . . ?
N3 C3 C4 109.2(2) . . ?
C8 C3 C4 110.4(2) . . ?
N3 C3 C9 109.8(2) . . ?
C8 C3 C9 108.7(3) . . ?
C4 C3 C9 109.2(2) . . ?
C5 C4 C3 107.4(2) . . ?
C5 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
C5 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
N6 C5 C6 109.0(2) . . ?
N6 C5 C10 109.0(2) . . ?
C6 C5 C10 109.8(2) . . ?
N6 C5 C4 109.5(2) . . ?
C6 C5 C4 110.6(2) . . ?
C10 C5 C4 108.9(2) . . ?
C5 C6 C7 108.2(2) . . ?
C5 C6 H6A 110.1 . . ?
C7 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
C7 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
N9 C7 C11 110.7(2) . . ?
N9 C7 C8 108.8(2) . . ?
C11 C7 C8 109.5(2) . . ?
N9 C7 C6 109.3(2) . . ?
C11 C7 C6 108.5(2) . . ?
C8 C7 C6 110.1(2) . . ?
C3 C8 C7 108.0(2) . . ?
C3 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
C3 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
N10 C9 C3 110.1(2) . . ?
N10 C9 H9A 109.6 . . ?
C3 C9 H9A 109.6 . . ?
N10 C9 H9B 109.6 . . ?
C3 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
N10 C10 C5 109.7(2) . . ?
N10 C10 H10A 109.7 . . ?
C5 C10 H10A 109.7 . . ?
N10 C10 H10B 109.7 . . ?
C5 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N10 C11 C7 110.1(2) . . ?
N10 C11 H11A 109.6 . . ?
C7 C11 H11A 109.6 . . ?
N10 C11 H11B 109.6 . . ?
C7 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
N5 C12 N6 109.8(2) . . ?
N5 C12 H12 125.1 . . ?
N6 C12 H12 125.1 . . ?
N4 C13 N6 110.4(2) . . ?
N4 C13 H13 124.8 . . ?
N6 C13 H13 124.8 . . ?
N7 C14 N9 110.7(3) . . ?
N7 C14 H14 124.6 . . ?
N9 C14 H14 124.6 . . ?
N8 C15 N9 111.4(3) . . ?
N8 C15 H15 124.3 . . ?
N9 C15 H15 124.3 . . ?
N11 C16 N13 110.5(3) . . ?
N11 C16 H16 124.8 . . ?
N13 C16 H16 124.8 . . ?
N12 C17 N13 110.0(3) . . ?
N12 C17 H17 125.0 . . ?
N13 C17 H17 125.0 . . ?
N13 C18 C19 108.8(2) . . ?
N13 C18 C23 110.3(2) . . ?
C19 C18 C23 109.8(2) . . ?
N13 C18 C24 109.6(2) . . ?
C19 C18 C24 109.0(2) . . ?
C23 C18 C24 109.3(2) . . ?
C20 C19 C18 108.3(2) . . ?
C20 C19 H19A 110.0 . . ?
C18 C19 H19A 110.0 . . ?
C20 C19 H19B 110.0 . . ?
C18 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
N16 C20 C19 108.6(2) . . ?
N16 C20 C25 110.3(2) . . ?
C19 C20 C25 110.0(3) . . ?
N16 C20 C21 108.2(2) . . ?
C19 C20 C21 110.2(2) . . ?
C25 C20 C21 109.6(2) . . ?
C20 C21 C22 107.2(2) . . ?
C20 C21 H21A 110.3 . . ?
C22 C21 H21A 110.3 . . ?
C20 C21 H21B 110.3 . . ?
C22 C21 H21B 110.3 . . ?
H21A C21 H21B 108.5 . . ?
N19 C22 C23 109.5(2) . . ?
N19 C22 C21 108.4(2) . . ?
C23 C22 C21 111.2(2) . . ?
N19 C22 C26 110.0(2) . . ?
C23 C22 C26 109.1(2) . . ?
C21 C22 C26 108.6(2) . . ?
C22 C23 C18 107.7(2) . . ?
C22 C23 H23A 110.2 . . ?
C18 C23 H23A 110.2 . . ?
C22 C23 H23B 110.2 . . ?
C18 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
N20 C24 C18 110.1(2) . . ?
N20 C24 H24A 109.6 . . ?
C18 C24 H24A 109.6 . . ?
N20 C24 H24B 109.6 . . ?
C18 C24 H24B 109.6 . . ?
H24A C24 H24B 108.2 . . ?
N20 C25 C20 109.4(2) . . ?
N20 C25 H25A 109.8 . . ?
C20 C25 H25A 109.8 . . ?
N20 C25 H25B 109.8 . . ?
C20 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
N20 C26 C22 110.1(2) . . ?
N20 C26 H26A 109.6 . . ?
C22 C26 H26A 109.6 . . ?
N20 C26 H26B 109.6 . . ?
C22 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
N14 C27 N16 110.5(3) . . ?
N14 C27 H27 124.8 . . ?
N16 C27 H27 124.8 . . ?
N15 C28 N16 111.3(3) . . ?
N15 C28 H28 124.3 . . ?
N16 C28 H28 124.3 . . ?
N17 C29 N19 109.2(3) . . ?
N17 C29 H29 125.4 . . ?
N19 C29 H29 125.4 . . ?
N18 C30 N19 111.6(3) . . ?
N18 C30 H30 124.2 . . ?
N19 C30 H30 124.2 . . ?
H7W O1W H8W 108.2 . . ?
H9W O2W H10W 108.4 . . ?
H11W O3W H12W 108.4 . . ?
H13W O4W H14W 108.3 . . ?
H15W O5W H16W 108.4 . . ?
H17W O6W H18W 108.3 . . ?
H19W O7W H20W 108.3 . . ?

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
N14 Cu1 N1 C1 -61.3(3) 2_655 . . . ?
N4 Cu1 N1 C1 124.5(3) 1_545 . . . ?
N11 Cu1 N1 C1 -153.2(3) . . . . ?
O2 Cu1 N1 C1 43.5(3) . . . . ?
N14 Cu1 N1 N2 117.3(2) 2_655 . . . ?
N4 Cu1 N1 N2 -56.9(2) 1_545 . . . ?
N11 Cu1 N1 N2 25.4(2) . . . . ?
O2 Cu1 N1 N2 -137.9(2) . . . . ?
C1 N1 N2 C2 -0.8(3) . . . . ?
Cu1 N1 N2 C2 -179.7(2) . . . . ?
C1 N1 N2 Cu2 -160.7(2) . . . . ?
Cu1 N1 N2 Cu2 20.4(3) . . . . ?
N17 Cu2 N2 C2 48.0(3) 3_666 . . . ?
N12 Cu2 N2 C2 140.5(3) . . . . ?
N5 Cu2 N2 C2 -131.6(3) 1_545 . . . ?
N7 Cu2 N2 C2 -45.7(3) 2_746 . . . ?
N17 Cu2 N2 N1 -156.5(2) 3_666 . . . ?
N12 Cu2 N2 N1 -64.0(2) . . . . ?
N5 Cu2 N2 N1 23.9(2) 1_545 . . . ?
N7 Cu2 N2 N1 109.8(2) 2_746 . . . ?
C13 N4 N5 C12 0.1(3) . . . . ?
Cu1 N4 N5 C12 170.2(2) 1_565 . . . ?
C13 N4 N5 Cu2 165.1(2) . . . 1_565 ?
Cu1 N4 N5 Cu2 -24.8(3) 1_565 . . 1_565 ?
C14 N7 N8 C15 -0.2(3) . . . . ?
Cu2 N7 N8 C15 178.4(2) 2_756 . . . ?
O1 Cu1 N11 C16 -39.8(2) . . . . ?
N1 Cu1 N11 C16 139.1(2) . . . . ?
N14 Cu1 N11 C16 51.6(2) 2_655 . . . ?
N4 Cu1 N11 C16 -129.0(2) 1_545 . . . ?
O2 Cu1 N11 C16 -125.1(3) . . . . ?
O1 Cu1 N11 N12 142.9(2) . . . . ?
N1 Cu1 N11 N12 -38.1(2) . . . . ?
N14 Cu1 N11 N12 -125.7(2) 2_655 . . . ?
N4 Cu1 N11 N12 53.8(2) 1_545 . . . ?
O2 Cu1 N11 N12 57.6(4) . . . . ?
C16 N11 N12 C17 -0.6(3) . . . . ?
Cu1 N11 N12 C17 176.99(18) . . . . ?
C16 N11 N12 Cu2 170.47(17) . . . . ?
Cu1 N11 N12 Cu2 -11.9(3) . . . . ?
N17 Cu2 N12 C17 -56.4(3) 3_666 . . . ?
N5 Cu2 N12 C17 124.9(2) 1_545 . . . ?
O3 Cu2 N12 C17 31.1(2) . . . . ?
N2 Cu2 N12 C17 -141.5(2) . . . . ?
N17 Cu2 N12 N11 135.45(18) 3_666 . . . ?
N5 Cu2 N12 N11 -43.28(18) 1_545 . . . ?
O3 Cu2 N12 N11 -137.06(17) . . . . ?
N2 Cu2 N12 N11 50.40(17) . . . . ?
C27 N14 N15 C28 0.1(4) . . . . ?
Cu1 N14 N15 C28 -178.7(3) 2_645 . . . ?
C29 N17 N18 C30 0.8(3) . . . . ?
Cu2 N17 N18 C30 -174.6(2) 3_666 . . . ?
N2 N1 C1 N3 1.1(3) . . . . ?
Cu1 N1 C1 N3 179.9(2) . . . . ?
C2 N3 C1 N1 -1.0(4) . . . . ?
C3 N3 C1 N1 178.9(3) . . . . ?
N1 N2 C2 N3 0.2(4) . . . . ?
Cu2 N2 C2 N3 158.7(2) . . . . ?
C1 N3 C2 N2 0.5(4) . . . . ?
C3 N3 C2 N2 -179.4(3) . . . . ?
C1 N3 C3 C8 -136.7(3) . . . . ?
C2 N3 C3 C8 43.1(4) . . . . ?
C1 N3 C3 C4 102.2(3) . . . . ?
C2 N3 C3 C4 -77.9(4) . . . . ?
C1 N3 C3 C9 -17.5(4) . . . . ?
C2 N3 C3 C9 162.4(3) . . . . ?
N3 C3 C4 C5 -178.4(2) . . . . ?
C8 C3 C4 C5 61.0(3) . . . . ?
C9 C3 C4 C5 -58.4(3) . . . . ?
C12 N6 C5 C6 -45.7(4) . . . . ?
C13 N6 C5 C6 131.3(3) . . . . ?
C12 N6 C5 C10 -165.6(3) . . . . ?
C13 N6 C5 C10 11.4(4) . . . . ?
C12 N6 C5 C4 75.4(4) . . . . ?
C13 N6 C5 C4 -107.6(3) . . . . ?
C3 C4 C5 N6 178.5(2) . . . . ?
C3 C4 C5 C6 -61.3(3) . . . . ?
C3 C4 C5 C10 59.4(3) . . . . ?
N6 C5 C6 C7 -178.2(2) . . . . ?
C10 C5 C6 C7 -58.9(3) . . . . ?
C4 C5 C6 C7 61.4(3) . . . . ?
C14 N9 C7 C11 -7.3(4) . . . . ?
C15 N9 C7 C11 175.4(3) . . . . ?
C14 N9 C7 C8 113.0(3) . . . . ?
C15 N9 C7 C8 -64.2(4) . . . . ?
C14 N9 C7 C6 -126.8(3) . . . . ?
C15 N9 C7 C6 56.0(4) . . . . ?
C5 C6 C7 N9 180.0(2) . . . . ?
C5 C6 C7 C11 59.2(3) . . . . ?
C5 C6 C7 C8 -60.6(3) . . . . ?
N3 C3 C8 C7 178.8(2) . . . . ?
C4 C3 C8 C7 -60.9(3) . . . . ?
C9 C3 C8 C7 58.8(3) . . . . ?
N9 C7 C8 C3 -179.9(2) . . . . ?
C11 C7 C8 C3 -58.9(3) . . . . ?
C6 C7 C8 C3 60.3(3) . . . . ?
C11 N10 C9 C3 61.0(3) . . . . ?
C10 N10 C9 C3 -61.9(3) . . . . ?
N3 C3 C9 N10 -179.9(2) . . . . ?
C8 C3 C9 N10 -60.1(3) . . . . ?
C4 C3 C9 N10 60.4(3) . . . . ?
C11 N10 C10 C5 -59.8(3) . . . . ?
C9 N10 C10 C5 63.0(3) . . . . ?
N6 C5 C10 N10 178.3(2) . . . . ?
C6 C5 C10 N10 58.9(3) . . . . ?
C4 C5 C10 N10 -62.4(3) . . . . ?
C9 N10 C11 C7 -60.6(3) . . . . ?
C10 N10 C11 C7 61.2(3) . . . . ?
N9 C7 C11 N10 179.5(2) . . . . ?
C8 C7 C11 N10 59.6(3) . . . . ?
C6 C7 C11 N10 -60.5(3) . . . . ?
N4 N5 C12 N6 0.0(3) . . . . ?
Cu2 N5 C12 N6 -164.81(19) 1_565 . . . ?
C13 N6 C12 N5 0.0(3) . . . . ?
C5 N6 C12 N5 177.5(3) . . . . ?
N5 N4 C13 N6 -0.1(3) . . . . ?
Cu1 N4 C13 N6 -170.18(19) 1_565 . . . ?
C12 N6 C13 N4 0.1(3) . . . . ?
C5 N6 C13 N4 -177.5(3) . . . . ?
N8 N7 C14 N9 0.3(3) . . . . ?
Cu2 N7 C14 N9 -178.06(18) 2_756 . . . ?
C15 N9 C14 N7 -0.3(3) . . . . ?
C7 N9 C14 N7 -178.1(2) . . . . ?
N7 N8 C15 N9 -0.1(4) . . . . ?
C14 N9 C15 N8 0.2(4) . . . . ?
C7 N9 C15 N8 178.0(3) . . . . ?
N12 N11 C16 N13 0.3(3) . . . . ?
Cu1 N11 C16 N13 -177.53(16) . . . . ?
C17 N13 C16 N11 0.1(3) . . . . ?
C18 N13 C16 N11 179.1(2) . . . . ?
N11 N12 C17 N13 0.7(3) . . . . ?
Cu2 N12 C17 N13 -168.22(18) . . . . ?
C16 N13 C17 N12 -0.6(3) . . . . ?
C18 N13 C17 N12 -179.5(2) . . . . ?
C17 N13 C18 C19 -152.3(2) . . . . ?
C16 N13 C18 C19 29.0(3) . . . . ?
C17 N13 C18 C23 87.2(3) . . . . ?
C16 N13 C18 C23 -91.5(3) . . . . ?
C17 N13 C18 C24 -33.3(3) . . . . ?
C16 N13 C18 C24 148.1(2) . . . . ?
N13 C18 C19 C20 177.8(2) . . . . ?
C23 C18 C19 C20 -61.5(3) . . . . ?
C24 C18 C19 C20 58.3(3) . . . . ?
C27 N16 C20 C19 149.9(3) . . . . ?
C28 N16 C20 C19 -32.9(4) . . . . ?
C27 N16 C20 C25 29.3(4) . . . . ?
C28 N16 C20 C25 -153.5(3) . . . . ?
C27 N16 C20 C21 -90.5(3) . . . . ?
C28 N16 C20 C21 86.7(4) . . . . ?
C18 C19 C20 N16 -179.6(2) . . . . ?
C18 C19 C20 C25 -58.9(3) . . . . ?
C18 C19 C20 C21 62.0(3) . . . . ?
N16 C20 C21 C22 -179.4(2) . . . . ?
C19 C20 C21 C22 -60.8(3) . . . . ?
C25 C20 C21 C22 60.3(3) . . . . ?
C29 N19 C22 C23 -69.6(3) . . . . ?
C30 N19 C22 C23 113.5(4) . . . . ?
C29 N19 C22 C21 168.9(3) . . . . ?
C30 N19 C22 C21 -8.0(4) . . . . ?
C29 N19 C22 C26 50.3(4) . . . . ?
C30 N19 C22 C26 -126.6(3) . . . . ?
C20 C21 C22 N19 -179.0(2) . . . . ?
C20 C21 C22 C23 60.6(3) . . . . ?
C20 C21 C22 C26 -59.5(3) . . . . ?
N19 C22 C23 C18 179.6(2) . . . . ?
C21 C22 C23 C18 -60.6(3) . . . . ?
C26 C22 C23 C18 59.2(3) . . . . ?
N13 C18 C23 C22 -179.8(2) . . . . ?
C19 C18 C23 C22 60.3(3) . . . . ?
C24 C18 C23 C22 -59.2(3) . . . . ?
C25 N20 C24 C18 61.1(3) . . . . ?
C26 N20 C24 C18 -60.6(3) . . . . ?
N13 C18 C24 N20 -178.7(2) . . . . ?
C19 C18 C24 N20 -59.7(3) . . . . ?
C23 C18 C24 N20 60.3(3) . . . . ?
C24 N20 C25 C20 -60.7(3) . . . . ?
C26 N20 C25 C20 61.3(3) . . . . ?
N16 C20 C25 N20 179.5(2) . . . . ?
C19 C20 C25 N20 59.8(3) . . . . ?
C21 C20 C25 N20 -61.5(3) . . . . ?
C24 N20 C26 C22 60.8(3) . . . . ?
C25 N20 C26 C22 -61.5(3) . . . . ?
N19 C22 C26 N20 179.5(2) . . . . ?
C23 C22 C26 N20 -60.4(3) . . . . ?
C21 C22 C26 N20 61.0(3) . . . . ?
N15 N14 C27 N16 -0.4(4) . . . . ?
Cu1 N14 C27 N16 178.2(2) 2_645 . . . ?
C28 N16 C27 N14 0.5(4) . . . . ?
C20 N16 C27 N14 178.2(3) . . . . ?
N14 N15 C28 N16 0.2(5) . . . . ?
C27 N16 C28 N15 -0.4(4) . . . . ?
C20 N16 C28 N15 -178.2(3) . . . . ?
N18 N17 C29 N19 -1.1(3) . . . . ?
Cu2 N17 C29 N19 174.22(19) 3_666 . . . ?
C30 N19 C29 N17 1.0(3) . . . . ?
C22 N19 C29 N17 -176.6(3) . . . . ?
N17 N18 C30 N19 -0.2(4) . . . . ?
C29 N19 C30 N18 -0.5(4) . . . . ?
C22 N19 C30 N18 176.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.87
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.069

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL ip1-819 in P 21/c
CELL 0.71073 21.8567 11.5525 21.4604 90.000 117.611 90.000
ZERR 4.00 0.0015 0.0009 0.0014 0.000 0.004 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O S CU
UNIT 120 224 80 72 8 8
MERG 2
OMIT 0.00 180.00
OMIT 1 1 0
OMIT 2 2 21
OMIT -10 2 2
OMIT -6 2 6
OMIT -5 1 6
OMIT 3 1 4
OMIT 2 2 4
OMIT 5 5 1
OMIT -5 4 6
SHEL 0.78 5
FMAP 2
PLAN 28
SIZE 0.17 0.26 0.39
ACTA
CONF
BOND $H
BIND Cu2 N2

LIST 4
L.S. 4
TEMP -60.00
WGHT 0.047500
FVAR 0.99405
CU1 6 0.744931 0.326296 0.419404 11.00000 0.02084 0.01532 =
0.01893 0.00163 0.00725 0.00261
CU2 6 0.756774 0.301251 0.602473 11.00000 0.01649 0.01918 =
0.01925 -0.00222 0.00689 0.00304
S1 5 0.554440 0.249226 0.179689 11.00000 0.02812 0.03118 =
0.02545 -0.00080 0.01300 -0.00762
S2 5 0.867355 0.529065 0.297350 11.00000 0.03757 0.04236 =
0.04496 -0.00649 0.02518 -0.00740
O1 4 0.709610 0.203570 0.346498 11.00000 0.03727 0.02458 =
0.02124 -0.00186 0.00848 -0.00230
AFIX 3
H1W 2 0.699470 0.136140 0.354648 11.00000 -1.50000
H2W 2 0.683610 0.219720 0.303528 11.00000 -1.50000
AFIX 0
O2 4 0.849286 0.317644 0.409776 11.00000 0.03778 0.04092 =
0.03757 0.00078 0.02160 0.00017
AFIX 3
H3W 2 0.849456 0.355484 0.375896 11.00000 -1.50000
H4W 2 0.883956 0.338634 0.447636 11.00000 -1.50000
AFIX 0
O3 4 0.728455 0.166189 0.663625 11.00000 0.03229 0.02979 =
0.03484 0.00512 0.01985 0.00135
AFIX 3
H5W 2 0.697315 0.188149 0.674214 11.00000 -1.50000
H6W 2 0.761914 0.138969 0.700444 11.00000 -1.50000
AFIX 0
O4 4 0.519651 0.363197 0.167073 11.00000 0.05887 0.04649 =
0.07437 0.01167 0.03445 0.00961
O5 4 0.538686 0.180667 0.228320 11.00000 0.04898 0.05350 =
0.04571 0.00506 0.03023 -0.01056
O6 4 0.531203 0.188337 0.111635 11.00000 0.05145 0.06709 =
0.03725 -0.01645 0.02053 -0.02505
O7 4 0.630778 0.265743 0.211548 11.00000 0.03019 0.05728 =
0.03227 0.00036 0.01468 -0.01255
O8 4 0.840901 0.611942 0.331225 11.00000 0.09345 0.05341 =
0.06607 -0.00879 0.05222 0.00006
O9 4 0.830577 0.417427 0.288490 11.00000 0.05179 0.04416 =
0.04076 -0.00549 0.02286 -0.01299
O10 4 0.852318 0.571121 0.226812 11.00000 0.16503 0.05868 =
0.07590 -0.00624 0.08841 -0.01717
O11 4 0.941260 0.508355 0.343286 11.00000 0.03882 0.07972 =
0.17489 -0.02457 0.02036 -0.00451
N1 3 0.791123 0.456099 0.486754 11.00000 0.02505 0.02084 =
0.02353 -0.00021 0.01035 0.00013
N2 3 0.786993 0.467061 0.548029 11.00000 0.03582 0.02448 =
0.02793 -0.00446 0.01736 -0.00678
N3 3 0.849069 0.610794 0.539732 11.00000 0.02930 0.01666 =
0.02622 -0.00119 0.01434 -0.00074
N4 3 0.796256 1.200533 0.495290 11.00000 0.02504 0.01863 =
0.02163 0.00052 0.01156 0.00314
N5 3 0.788719 1.180705 0.554904 11.00000 0.02294 0.01801 =
0.02299 0.00093 0.01203 0.00293
N6 3 0.849424 1.039109 0.543941 11.00000 0.02237 0.01586 =
0.02371 0.00163 0.01251 0.00330
N7 3 1.142591 0.810289 0.822628 11.00000 0.01869 0.02850 =
0.02733 0.00326 0.01098 0.00115
N8 3 1.090194 0.819917 0.841771 11.00000 0.02080 0.06904 =
0.02812 0.00287 0.01238 0.00366
N9 3 1.044402 0.822142 0.725918 11.00000 0.01844 0.02677 =
0.02542 0.00037 0.00852 0.00277
N10 3 0.973549 0.827776 0.529019 11.00000 0.02598 0.02255 =
0.02924 -0.00067 0.01705 0.00373
N11 3 0.659481 0.291433 0.451520 11.00000 0.02073 0.02766 =
0.02017 0.00079 0.00921 -0.00166
N12 3 0.662161 0.293704 0.517531 11.00000 0.02112 0.02045 =
0.02010 -0.00007 0.00861 0.00244
N13 3 0.555653 0.256482 0.439516 11.00000 0.01771 0.01989 =
0.02122 -0.00212 0.00904 -0.00002
N14 3 0.312383 -0.052815 0.151100 11.00000 0.02481 0.02193 =
0.02459 -0.00258 0.01092 -0.00410
N15 3 0.361674 0.005590 0.140510 11.00000 0.05004 0.04890 =
0.04559 -0.02414 0.03374 -0.02884
N16 3 0.364618 0.066249 0.239047 11.00000 0.02184 0.02170 =
0.02511 -0.00789 0.01128 -0.00406
N17 3 0.273284 0.578049 0.351491 11.00000 0.02390 0.02489 =
0.02183 -0.00229 0.01066 0.00351
N18 3 0.246773 0.563646 0.279616 11.00000 0.03382 0.03503 =
0.02303 -0.00112 0.01123 0.01151
N19 3 0.320194 0.423114 0.335576 11.00000 0.02356 0.02357 =
0.02489 -0.00268 0.01118 0.00502
N20 3 0.388534 0.132224 0.421476 11.00000 0.02682 0.02217 =
0.02682 -0.00291 0.01487 -0.00368
C1 1 0.827332 0.542198 0.481718 11.00000 0.03240 0.02239 =
0.02652 0.00036 0.01519 -0.00102
AFIX 43
H1 2 0.836920 0.554874 0.443851 11.00000 -1.20000
AFIX 0
C2 1 0.822254 0.560573 0.579479 11.00000 0.04020 0.02740 =
0.03343 -0.00402 0.02288 -0.00610
AFIX 43
H2 2 0.828151 0.588768 0.623005 11.00000 -1.20000
AFIX 0
C3 1 0.892451 0.716921 0.557340 11.00000 0.02629 0.01440 =
0.02769 -0.00012 0.01298 0.00052
C4 1 0.845710 0.824811 0.542379 11.00000 0.01833 0.01985 =
0.02258 -0.00040 0.00819 0.00236
AFIX 23
H4A 2 0.810578 0.825927 0.492936 11.00000 -1.20000
H4B 2 0.822330 0.823576 0.571835 11.00000 -1.20000
AFIX 0
C5 1 0.892463 0.932554 0.559347 11.00000 0.02300 0.01445 =
0.02519 0.00201 0.01339 0.00515
C6 1 0.946370 0.933101 0.637022 11.00000 0.01623 0.01908 =
0.02409 -0.00100 0.00970 0.00083
AFIX 23
H6A 2 0.923427 0.932643 0.666893 11.00000 -1.20000
H6B 2 0.974953 1.002903 0.647686 11.00000 -1.20000
AFIX 0
C7 1 0.991902 0.823834 0.651302 11.00000 0.01855 0.02050 =
0.02282 0.00186 0.00776 0.00381
C8 1 0.946934 0.713582 0.635556 11.00000 0.02242 0.01850 =
0.02705 0.00249 0.01040 0.00395
AFIX 23
H8A 2 0.975803 0.644343 0.645022 11.00000 -1.20000
H8B 2 0.924133 0.711275 0.665541 11.00000 -1.20000
AFIX 0
C9 1 0.930250 0.722604 0.511699 11.00000 0.02935 0.01815 =
0.02779 -0.00223 0.01595 0.00046
AFIX 23
H9A 2 0.959283 0.653789 0.520253 11.00000 -1.20000
H9B 2 0.896320 0.723706 0.461811 11.00000 -1.20000
AFIX 0
C10 1 0.928804 0.931390 0.512787 11.00000 0.02800 0.01951 =
0.02736 0.00107 0.01649 0.00316
AFIX 23
H10A 2 0.894267 0.930331 0.463115 11.00000 -1.20000
H10B 2 0.956778 1.001535 0.521284 11.00000 -1.20000
AFIX 0
C11 1 1.026359 0.827128 0.603039 11.00000 0.02233 0.02840 =
0.02963 0.00020 0.01278 0.00352
AFIX 23
H11A 2 1.055086 0.896654 0.613083 11.00000 -1.20000
H11B 2 1.056235 0.759309 0.612093 11.00000 -1.20000
AFIX 0
C12 1 0.820885 1.083803 0.583212 11.00000 0.02403 0.02067 =
0.02233 0.00244 0.01210 0.00440
AFIX 43
H12 2 0.823792 1.050275 0.624408 11.00000 -1.20000
AFIX 0
C13 1 0.832436 1.115268 0.489866 11.00000 0.02672 0.02182 =
0.02350 0.00245 0.01375 0.00465
AFIX 43
H13 2 0.845073 1.107319 0.453756 11.00000 -1.20000
AFIX 0
C14 1 1.113684 0.811518 0.753686 11.00000 0.01905 0.02520 =
0.02875 0.00047 0.01101 0.00047
AFIX 43
H14 2 1.137852 0.805794 0.727234 11.00000 -1.20000
AFIX 0
C15 1 1.032658 0.826704 0.783140 11.00000 0.02116 0.07149 =
0.03073 0.00261 0.01415 0.00395
AFIX 43
H15 2 0.988713 0.833826 0.780590 11.00000 -1.20000
AFIX 0
C16 1 0.595544 0.268776 0.406064 11.00000 0.02124 0.02818 =
0.01846 0.00142 0.00794 -0.00112
AFIX 43
H16 2 0.579243 0.261892 0.357279 11.00000 -1.20000
AFIX 0
C17 1 0.599440 0.273434 0.508769 11.00000 0.02152 0.02454 =
0.02123 -0.00295 0.00982 0.00056
AFIX 43
H17 2 0.586797 0.271037 0.545070 11.00000 -1.20000
AFIX 0
C18 1 0.480394 0.232076 0.405439 11.00000 0.01699 0.01958 =
0.01956 -0.00303 0.00662 -0.00051
C19 1 0.460915 0.162739 0.337548 11.00000 0.02222 0.01804 =
0.02246 -0.00404 0.01058 0.00081
AFIX 23
H19A 2 0.470619 0.208528 0.304698 11.00000 -1.20000
H19B 2 0.488087 0.091275 0.348359 11.00000 -1.20000
AFIX 0
C20 1 0.383785 0.133951 0.304505 11.00000 0.01998 0.01995 =
0.02172 -0.00857 0.00969 -0.00310
C21 1 0.340728 0.246011 0.284639 11.00000 0.01803 0.02337 =
0.02328 -0.00407 0.00817 -0.00012
AFIX 23
H21A 2 0.291357 0.227634 0.262823 11.00000 -1.20000
H21B 2 0.349815 0.291315 0.251200 11.00000 -1.20000
AFIX 0
C22 1 0.362002 0.315202 0.353068 11.00000 0.02158 0.01932 =
0.02622 -0.00464 0.01143 0.00286
C23 1 0.439165 0.346306 0.387851 11.00000 0.02220 0.01698 =
0.02301 -0.00391 0.01024 0.00039
AFIX 23
H23A 2 0.451661 0.391086 0.430858 11.00000 -1.20000
H23B 2 0.449449 0.393033 0.355739 11.00000 -1.20000
AFIX 0
C24 1 0.462861 0.159226 0.455435 11.00000 0.02421 0.02231 =
0.02545 -0.00191 0.01329 -0.00136
AFIX 23
H24A 2 0.489569 0.087184 0.467456 11.00000 -1.20000
H24B 2 0.475393 0.202351 0.499014 11.00000 -1.20000
AFIX 0
C25 1 0.368518 0.063701 0.356414 11.00000 0.02988 0.02057 =
0.02837 -0.00471 0.01632 -0.00629
AFIX 23
H25A 2 0.319204 0.045027 0.335038 11.00000 -1.20000
H25B 2 0.394531 -0.009042 0.367819 11.00000 -1.20000
AFIX 0
C26 1 0.347383 0.240526 0.404436 11.00000 0.02167 0.02808 =
0.02655 -0.00572 0.01307 -0.00227
AFIX 23
H26A 2 0.359321 0.284226 0.447699 11.00000 -1.20000
H26B 2 0.298105 0.221571 0.383027 11.00000 -1.20000
AFIX 0
C27 1 0.314951 -0.015135 0.209557 11.00000 0.02374 0.02280 =
0.02618 -0.00334 0.01301 -0.00335
AFIX 43
H27 2 0.286278 -0.040966 0.228512 11.00000 -1.20000
AFIX 0
C28 1 0.391798 0.076157 0.193903 11.00000 0.05106 0.04936 =
0.04811 -0.02886 0.03685 -0.03140
AFIX 43
H28 2 0.427694 0.127199 0.200163 11.00000 -1.20000
AFIX 0
C29 1 0.317148 0.495116 0.383862 11.00000 0.02336 0.02407 =
0.02186 -0.00420 0.00847 0.00370
AFIX 43
H29 2 0.342587 0.486684 0.432896 11.00000 -1.20000
AFIX 0
C30 1 0.276168 0.469566 0.272346 11.00000 0.03483 0.03544 =
0.02238 -0.00283 0.00898 0.01087
AFIX 43
H30 2 0.267850 0.438009 0.228750 11.00000 -1.20000
AFIX 0
O1W 4 0.557587 0.939702 0.261550 11.00000 0.08270 0.05269 =
0.06853 -0.00778 0.05278 -0.00307
AFIX 3
H7W 2 0.531677 0.918002 0.279080 11.00000 -1.50000
H8W 2 0.547977 1.009722 0.248510 11.00000 -1.50000
AFIX 0
O2W 4 0.682973 0.987936 0.380007 11.00000 0.07762 0.05867 =
0.07604 0.00724 0.03984 -0.01389
AFIX 3
H9W 2 0.651023 0.959216 0.342597 11.00000 -1.50000
H10W 2 0.667813 0.995717 0.409787 11.00000 -1.50000
AFIX 0
O3W 4 0.600608 0.961436 0.447208 11.00000 0.08277 0.09703 =
0.04921 0.01375 0.02917 -0.02429
AFIX 3
H11W 2 0.567648 0.918566 0.419328 11.00000 -1.50000
H12W 2 0.607208 0.948716 0.488878 11.00000 -1.50000
AFIX 0
O4W 4 0.837438 0.806050 0.210689 11.00000 0.08457 0.07494 =
0.06531 0.02946 0.04145 0.01665
AFIX 3
H13W 2 0.840108 0.732629 0.212819 11.00000 -1.50000
H14W 2 0.858268 0.832590 0.252319 11.00000 -1.50000
AFIX 0
O5W 4 0.417092 0.048480 0.041946 11.00000 0.05203 0.06508 =
0.02936 -0.00408 0.01521 -0.02560
AFIX 3
H15W 2 0.400512 0.026150 0.068766 11.00000 -1.50000
H16W 2 0.454493 0.084680 0.066666 11.00000 -1.50000
AFIX 0
O6W 4 1.044126 0.633715 0.449778 11.00000 0.04959 0.14405 =
0.04664 -0.01399 0.02395 -0.01939
AFIX 3
H17W 2 1.069176 0.650835 0.430408 11.00000 -1.50000
H18W 2 1.008696 0.597715 0.419978 11.00000 -1.50000
AFIX 0
O7W 4 0.928917 0.826578 0.364463 11.00000 0.23234 0.08147 =
0.07505 0.00076 0.08742 0.00374
AFIX 3
H19W 2 0.913837 0.758209 0.362713 11.00000 -1.50000
H20W 2 0.949307 0.847839 0.407243 11.00000 -1.50000
HKLF 4

REM ip1-819 in P 21/c
REM R1 = 0.0355 for 6283 Fo > 4sig(Fo) and 0.0569 for all 9003 data
REM 649 parameters refined using 0 restraints

END

WGHT 0.0475 0.0000
REM Highest difference peak 1.453, deepest hole -0.379, 1-sigma level 0.069
Q1 1 0.2168 0.2996 0.1325 11.00000 0.05 1.45
Q2 1 0.6916 0.7338 0.4370 11.00000 0.05 1.06
Q3 1 0.9118 0.5308 0.3760 11.00000 0.05 0.58
Q4 1 0.9175 0.4844 0.2706 11.00000 0.05 0.53
Q5 1 0.5199 0.3151 0.1211 11.00000 0.05 0.52
Q6 1 0.5410 0.3035 0.2363 11.00000 0.05 0.46
Q7 1 1.0169 0.8172 0.4221 11.00000 0.05 0.46
Q8 1 0.6627 1.0178 0.5127 11.00000 0.05 0.38
Q9 1 0.8565 0.8317 0.3429 11.00000 0.05 0.37
Q10 1 0.5265 0.1275 0.1729 11.00000 0.05 0.37

;

#---------------------------------------------------------

data_(10)
_database_code_depnum_ccdc_archive 'CCDC 867233'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris-[3,5,7-tri(1,2,4-triazol-4-yl)-1-azaadamantane]-
dicadmium(II) Chloride Octacosahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H54 Cd2 N30, 28(H2 O), Cl4'
_chemical_formula_sum            'C45 H110 Cd2 Cl4 N30 O28'
_chemical_formula_weight         1886.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_space_group_name_Hall           '-P 6c'
_symmetry_Int_Tables_number      176

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

_cell_length_a                   18.5633(17)
_cell_length_b                   18.5633(17)
_cell_length_c                   14.3967(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4296.4(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    20410
_cell_measurement_theta_min      3.58
_cell_measurement_theta_max      25.68

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8776
_exptl_absorpt_correction_T_max  0.9264
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20410
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_sigmaI/netI    0.1402
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2842
_reflns_number_gt                1394
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The problems were associated with a relatively weak diffraction from
the crystals (nearly 10 of which were tested in order to select a more
satisfactory one) and with disorder in the region of large crystal
channels.
Refinement of Cd-organic framework atoms was standard. The CH-hydrogen
atoms were constrained with U(iso) = 1.2U(eq) of the parent C-atom and
with C-H distances 0.95 A (triazole), 0.99 A (CH2 azaadamantane).
One chloride anion (0.5 equivalents per Cd) appears to be entrapped
into the pocket of the structure, with 6 symmetry related directional
CH(tr)...Cl hydrogen bonds. This chloride was refined anisotropically
giving good thermal parameters. One water molecule, which lie in the
proximity to the Cd-organic framework and forms H-bond to triazole
N-atom (N...O ca. 2.80 A) was also located. This molecule is equally
disordered over two closely separated positions (1/2O...1/2O 0.97 A),
which were refined anisotropically, but without H-atoms.
Other anions are badly disordered in the channels of the structure,
also overlapping with the solvate water molecules, most of which are
totally disordered. This electron density was modelled using SQUEEZE
routine implemented in PLATON -- 634 e / unit cell, corresponding to
electron density of 3Cl and 25(H2O) per formula unit (Cd2).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2842
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1566
_refine_ls_wR_factor_gt          0.1426
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_restrained_S_all      0.820
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.6667 0.3333 0.60354(4) 0.0403(3) Uani 1 3 d S . .
Cl1 Cl 0.6667 0.3333 0.2500 0.0637(11) Uani 1 6 d S . .
N1 N 0.5546(3) 0.2353(3) 0.5188(3) 0.0556(15) Uani 1 1 d . . .
N2 N 0.4862(4) 0.1756(3) 0.5705(3) 0.0692(19) Uani 1 1 d . . .
N3 N 0.4581(3) 0.1473(3) 0.4204(3) 0.0519(14) Uani 1 1 d . . .
N4 N 0.3440(3) -0.2275(3) 0.2974(3) 0.0455(13) Uani 1 1 d . . .
N5 N 0.3590(5) -0.1102(4) 0.2500 0.053(2) Uani 1 2 d S . .
N6 N 0.2869(6) 0.0466(6) 0.2500 0.082(3) Uani 1 2 d S . .
C1 C 0.5360(5) 0.2182(4) 0.4312(4) 0.059(2) Uani 1 1 d . . .
H1 H 0.5710 0.2499 0.3813 0.071 Uiso 1 1 calc R . .
C2 C 0.4326(5) 0.1266(5) 0.5098(4) 0.088(3) Uani 1 1 d . . .
H2 H 0.3802 0.0804 0.5262 0.106 Uiso 1 1 calc R . .
C3 C 0.3519(4) -0.1571(4) 0.3221(4) 0.063(2) Uani 1 1 d . . .
H3 H 0.3525 -0.1410 0.3849 0.076 Uiso 1 1 calc R . .
C4 C 0.4169(4) 0.1035(4) 0.3362(4) 0.0564(19) Uani 1 1 d . . .
C5 C 0.4123(4) 0.0205(3) 0.3362(3) 0.0536(18) Uani 1 1 d . . .
H5A H 0.3830 -0.0111 0.3926 0.064 Uiso 1 1 calc R . .
H5B H 0.4690 0.0282 0.3362 0.064 Uiso 1 1 calc R . .
C6 C 0.3656(6) -0.0268(5) 0.2500 0.054(3) Uani 1 2 d S . .
C7 C 0.3299(5) 0.0932(5) 0.3338(4) 0.070(2) Uani 1 1 d . . .
H7A H 0.2983 0.0628 0.3898 0.084 Uiso 1 1 calc R . .
H7B H 0.3340 0.1485 0.3332 0.084 Uiso 1 1 calc R . .
C8 C 0.4680(6) 0.1579(5) 0.2500 0.060(3) Uani 1 2 d S . .
H8A H 0.4705 0.2125 0.2500 0.072 Uiso 1 2 calc SR . .
H8B H 0.5254 0.1672 0.2500 0.072 Uiso 1 2 calc SR . .
C9 C 0.2790(6) -0.0368(6) 0.2500 0.060(3) Uani 1 2 d S . .
H9 H 0.2480 -0.0682 0.1942 0.072 Uiso 1 1 d R . .
O1A O 0.442(3) 0.112(3) 0.7500 0.167(19) Uani 0.50 2 d SP . .
O1B O 0.416(2) 0.147(2) 0.7500 0.122(13) Uani 0.50 2 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0530(4) 0.0530(4) 0.0151(3) 0.000 0.000 0.02648(18)
Cl1 0.0694(17) 0.0694(17) 0.052(2) 0.000 0.000 0.0347(9)
N1 0.069(4) 0.048(3) 0.030(3) -0.013(2) -0.007(3) 0.014(3)
N2 0.080(4) 0.050(4) 0.025(2) 0.002(3) 0.009(3) -0.007(3)
N3 0.058(4) 0.040(3) 0.029(3) -0.008(2) -0.004(2) 0.003(3)
N4 0.068(4) 0.051(3) 0.020(2) -0.002(2) 0.006(2) 0.032(3)
N5 0.094(6) 0.037(4) 0.021(3) 0.000 0.000 0.028(4)
N6 0.105(8) 0.087(7) 0.043(5) 0.000 0.000 0.041(6)
C1 0.091(6) 0.077(5) 0.014(2) 0.004(3) 0.008(3) 0.047(5)
C2 0.095(6) 0.081(5) 0.019(3) 0.012(4) 0.013(4) -0.009(5)
C3 0.109(6) 0.060(5) 0.017(3) 0.003(3) 0.001(3) 0.040(5)
C4 0.077(5) 0.045(4) 0.025(3) 0.001(3) 0.005(3) 0.014(4)
C5 0.083(5) 0.039(4) 0.020(3) 0.001(3) 0.004(3) 0.016(4)
C6 0.081(7) 0.038(5) 0.024(4) 0.000 0.000 0.016(5)
C7 0.101(6) 0.082(5) 0.028(3) -0.004(3) 0.001(4) 0.047(5)
C8 0.101(8) 0.045(6) 0.026(4) 0.000 0.000 0.031(6)
C9 0.054(7) 0.070(8) 0.048(5) 0.000 0.000 0.024(6)
O1A 0.21(4) 0.17(4) 0.042(11) 0.000 0.000 0.03(2)
O1B 0.103(19) 0.13(3) 0.045(10) 0.000 0.000 -0.011(16)

_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.
;

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
Cd1 N1 2.311(5) 3_655 ?
Cd1 N1 2.311(5) . ?
Cd1 N1 2.311(5) 4_665 ?
Cd1 N4 2.354(5) 7_656 ?
Cd1 N4 2.354(5) 9_666 ?
Cd1 N4 2.354(5) 10_556 ?
N1 C1 1.305(7) . ?
N1 N2 1.409(7) . ?
N2 C2 1.295(8) . ?
N3 C2 1.359(7) . ?
N3 C1 1.394(8) . ?
N3 C4 1.447(7) . ?
N4 C3 1.290(7) . ?
N4 N4 1.366(8) 8_556 ?
N4 Cd1 2.354(5) 7_656 ?
N5 C3 1.319(7) 8_556 ?
N5 C3 1.319(7) . ?
N5 C6 1.491(10) . ?
N6 C7 1.466(8) . ?
N6 C7 1.466(8) 8_556 ?
N6 C9 1.480(12) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.498(8) . ?
C4 C7 1.530(9) . ?
C4 C8 1.582(8) . ?
C5 C6 1.517(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C5 1.517(7) 8_556 ?
C6 C9 1.524(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C4 1.582(8) 8_556 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 94.73(16) 3_655 . ?
N1 Cd1 N1 94.73(16) 3_655 4_665 ?
N1 Cd1 N1 94.73(16) . 4_665 ?
N1 Cd1 N4 88.17(17) 3_655 7_656 ?
N1 Cd1 N4 89.73(17) . 7_656 ?
N1 Cd1 N4 174.45(17) 4_665 7_656 ?
N1 Cd1 N4 89.73(17) 3_655 9_666 ?
N1 Cd1 N4 174.45(17) . 9_666 ?
N1 Cd1 N4 88.17(17) 4_665 9_666 ?
N4 Cd1 N4 87.12(15) 7_656 9_666 ?
N1 Cd1 N4 174.45(17) 3_655 10_556 ?
N1 Cd1 N4 88.17(17) . 10_556 ?
N1 Cd1 N4 89.73(17) 4_665 10_556 ?
N4 Cd1 N4 87.12(15) 7_656 10_556 ?
N4 Cd1 N4 87.12(15) 9_666 10_556 ?
C1 N1 N2 107.1(5) . . ?
C1 N1 Cd1 136.6(5) . . ?
N2 N1 Cd1 116.3(3) . . ?
C2 N2 N1 105.7(5) . . ?
C2 N3 C1 102.2(5) . . ?
C2 N3 C4 128.5(5) . . ?
C1 N3 C4 129.1(5) . . ?
C3 N4 N4 106.0(3) . 8_556 ?
C3 N4 Cd1 126.7(3) . 7_656 ?
N4 N4 Cd1 127.28(11) 8_556 7_656 ?
C3 N5 C3 103.9(7) 8_556 . ?
C3 N5 C6 127.9(4) 8_556 . ?
C3 N5 C6 127.9(4) . . ?
C7 N6 C7 110.8(8) . 8_556 ?
C7 N6 C9 110.9(6) . . ?
C7 N6 C9 110.9(6) 8_556 . ?
N1 C1 N3 111.2(6) . . ?
N1 C1 H1 124.4 . . ?
N3 C1 H1 124.4 . . ?
N2 C2 N3 113.8(6) . . ?
N2 C2 H2 123.1 . . ?
N3 C2 H2 123.1 . . ?
N4 C3 N5 112.0(5) . . ?
N4 C3 H3 124.0 . . ?
N5 C3 H3 124.0 . . ?
N3 C4 C5 108.6(5) . . ?
N3 C4 C7 108.5(5) . . ?
C5 C4 C7 110.9(5) . . ?
N3 C4 C8 108.6(5) . . ?
C5 C4 C8 111.4(6) . . ?
C7 C4 C8 108.7(6) . . ?
C4 C5 C6 108.5(6) . . ?
C4 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
C4 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N5 C6 C5 109.2(5) . . ?
N5 C6 C5 109.2(5) . 8_556 ?
C5 C6 C5 109.8(7) . 8_556 ?
N5 C6 C9 109.8(8) . . ?
C5 C6 C9 109.4(5) . . ?
C5 C6 C9 109.4(5) 8_556 . ?
N6 C7 C4 108.7(6) . . ?
N6 C7 H7A 109.9 . . ?
C4 C7 H7A 109.9 . . ?
N6 C7 H7B 109.9 . . ?
C4 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C4 C8 C4 103.3(7) 8_556 . ?
C4 C8 H8A 111.1 8_556 . ?
C4 C8 H8A 111.1 . . ?
C4 C8 H8B 111.1 8_556 . ?
C4 C8 H8B 111.1 . . ?
H8A C8 H8B 109.1 . . ?
N6 C9 C6 109.0(8) . . ?
N6 C9 H9 109.9 . . ?
C6 C9 H9 109.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cd1 N1 C1 -46.7(6) 3_655 . . . ?
N1 Cd1 N1 C1 48.5(6) 4_665 . . . ?
N4 Cd1 N1 C1 -134.8(7) 7_656 . . . ?
N4 Cd1 N1 C1 138.1(7) 10_556 . . . ?
N1 Cd1 N1 N2 132.5(5) 3_655 . . . ?
N1 Cd1 N1 N2 -132.3(5) 4_665 . . . ?
N4 Cd1 N1 N2 44.4(4) 7_656 . . . ?
N4 Cd1 N1 N2 -42.8(4) 10_556 . . . ?
C1 N1 N2 C2 1.0(8) . . . . ?
Cd1 N1 N2 C2 -178.4(5) . . . . ?
N2 N1 C1 N3 -1.7(8) . . . . ?
Cd1 N1 C1 N3 177.5(4) . . . . ?
C2 N3 C1 N1 1.7(8) . . . . ?
C4 N3 C1 N1 -174.8(6) . . . . ?
N1 N2 C2 N3 0.1(10) . . . . ?
C1 N3 C2 N2 -1.1(9) . . . . ?
C4 N3 C2 N2 175.4(7) . . . . ?
N4 N4 C3 N5 -1.5(7) 8_556 . . . ?
Cd1 N4 C3 N5 178.0(5) 7_656 . . . ?
C3 N5 C3 N4 2.3(11) 8_556 . . . ?
C6 N5 C3 N4 177.3(8) . . . . ?
C2 N3 C4 C5 -64.2(10) . . . . ?
C1 N3 C4 C5 111.4(7) . . . . ?
C2 N3 C4 C7 56.5(9) . . . . ?
C1 N3 C4 C7 -127.9(7) . . . . ?
C2 N3 C4 C8 174.5(8) . . . . ?
C1 N3 C4 C8 -9.9(10) . . . . ?
N3 C4 C5 C6 177.5(6) . . . . ?
C7 C4 C5 C6 58.3(7) . . . . ?
C8 C4 C5 C6 -63.0(8) . . . . ?
C3 N5 C6 C5 -153.1(8) 8_556 . . . ?
C3 N5 C6 C5 33.1(12) . . . . ?
C3 N5 C6 C5 -33.1(12) 8_556 . . 8_556 ?
C3 N5 C6 C5 153.1(8) . . . 8_556 ?
C3 N5 C6 C9 86.9(9) 8_556 . . . ?
C3 N5 C6 C9 -86.9(9) . . . . ?
C4 C5 C6 N5 -178.9(6) . . . . ?
C4 C5 C6 C5 61.5(9) . . . 8_556 ?
C4 C5 C6 C9 -58.6(8) . . . . ?
C7 N6 C7 C4 -63.3(10) 8_556 . . . ?
C9 N6 C7 C4 60.3(8) . . . . ?
N3 C4 C7 N6 -178.3(6) . . . . ?
C5 C4 C7 N6 -59.0(7) . . . . ?
C8 C4 C7 N6 63.8(7) . . . . ?
N3 C4 C8 C4 179.9(4) . . . 8_556 ?
C5 C4 C8 C4 60.3(9) . . . 8_556 ?
C7 C4 C8 C4 -62.2(8) . . . 8_556 ?
C7 N6 C9 C6 -61.8(6) . . . . ?
C7 N6 C9 C6 61.8(6) 8_556 . . . ?
N5 C6 C9 N6 180.0 . . . . ?
C5 C6 C9 N6 60.2(5) . . . . ?
C5 C6 C9 N6 -60.2(5) 8_556 . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.098

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.019 2194 634 ' '
_platon_squeeze_details          
;
;

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk13 in P6(3)/m
CELL 0.71073 18.5633 18.5633 14.3967 90.000 90.000 120.000
ZERR 2.00 0.0017 0.0017 0.0013 0.000 0.000 0.000
LATT 1
SYMM - X, - Y, 1/2 + Z
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SYMM X - Y, X, 1/2 + Z
SYMM Y, - X + Y, 1/2 + Z
SFAC C H N O CL CD
UNIT 90 220 60 56 8 4
MERG 2
OMIT 0.00 180.00
OMIT 0 2 2
OMIT -1 12 4
OMIT -3 6 3
OMIT -1 2 2
SHEL 0.82 6
FMAP 2
PLAN 25
SIZE 0.11 0.17 0.19
ACTA
BOND
BOND $H
CONF
LIST 4
L.S. 4
TEMP -100.00
WGHT 0.083000
FVAR 2.76845
CD1 6 0.666667 0.333333 0.603537 10.33333 0.05295 0.05295 =
0.01512 0.00000 0.00000 0.02648
CL1 5 0.666667 0.333333 0.250000 10.16667 0.06944 0.06944 =
0.05214 0.00000 0.00000 0.03472
N1 3 0.554591 0.235280 0.518843 11.00000 0.06868 0.04822 =
0.03029 -0.01327 -0.00662 0.01445
N2 3 0.486231 0.175584 0.570496 11.00000 0.08027 0.04978 =
0.02538 0.00169 0.00857 -0.00657
N3 3 0.458139 0.147273 0.420377 11.00000 0.05771 0.03965 =
0.02927 -0.00784 -0.00411 0.00263
N4 3 0.344020 -0.227521 0.297435 11.00000 0.06786 0.05135 =
0.02042 -0.00242 0.00629 0.03204
N5 3 0.358950 -0.110245 0.250000 10.50000 0.09417 0.03709 =
0.02061 0.00000 0.00000 0.02795
N6 3 0.286902 0.046643 0.250000 10.50000 0.10525 0.08691 =
0.04309 0.00000 0.00000 0.04108
C1 1 0.535999 0.218172 0.431188 11.00000 0.09109 0.07730 =
0.01448 0.00419 0.00802 0.04685
AFIX 43
H1 2 0.570963 0.249896 0.381260 11.00000 -1.20000
AFIX 0
C2 1 0.432577 0.126570 0.509798 11.00000 0.09511 0.08069 =
0.01898 0.01188 0.01330 -0.00875
AFIX 43
H2 2 0.380198 0.080416 0.526246 11.00000 -1.20000
AFIX 0
C3 1 0.351870 -0.157145 0.322139 11.00000 0.10903 0.06025 =
0.01663 0.00287 0.00132 0.04015
AFIX 43
H3 2 0.352480 -0.141006 0.384884 11.00000 -1.20000
AFIX 0
C4 1 0.416938 0.103470 0.336176 11.00000 0.07672 0.04532 =
0.02514 0.00125 0.00480 0.01402
C5 1 0.412292 0.020545 0.336225 11.00000 0.08269 0.03857 =
0.01985 0.00131 0.00435 0.01565
AFIX 23
H5A 2 0.382979 -0.011079 0.392604 11.00000 -1.20000
H5B 2 0.469042 0.028212 0.336233 11.00000 -1.20000
AFIX 0
C6 1 0.365609 -0.026794 0.250000 10.50000 0.08149 0.03775 =
0.02399 0.00000 0.00000 0.01591
C7 1 0.329867 0.093200 0.333814 11.00000 0.10056 0.08230 =
0.02841 -0.00423 0.00053 0.04660
AFIX 23
H7A 2 0.298264 0.062826 0.389763 11.00000 -1.20000
H7B 2 0.334021 0.148484 0.333195 11.00000 -1.20000
AFIX 0
C8 1 0.468034 0.157926 0.250000 10.50000 0.10071 0.04533 =
0.02556 0.00000 0.00000 0.03091
AFIX 23
H8A 2 0.470521 0.212457 0.250000 10.50000 -1.20000
H8B 2 0.525380 0.167162 0.250000 10.50000 -1.20000
AFIX 0
C9 1 0.278989 -0.036766 0.250000 10.50000 0.05406 0.06968 =
0.04763 0.00000 0.00000 0.02442
AFIX 3
H9 2 0.248013 -0.068166 0.194220 11.00000 -1.20000
AFIX 0
O1A 4 0.441824 0.112031 0.750000 10.25000 0.21028 0.16748 =
0.04190 0.00000 0.00000 0.03341
O1B 4 0.416320 0.146528 0.750000 10.25000 0.10260 0.12633 =
0.04487 0.00000 0.00000 -0.01110
HKLF 4

REM dk13 in P6(3)/m
REM R1 = 0.0655 for 1365 Fo > 4sig(Fo) and 0.1148 for all 2841 data
REM 138 parameters refined using 0 restraints

END

WGHT 0.0831 0.0000
REM Highest difference peak 1.184, deepest hole -0.858, 1-sigma level 0.098
Q1 1 0.6667 0.3333 0.3239 10.33333 0.05 1.18
Q2 1 0.6309 0.3622 0.6027 11.00000 0.05 1.17
Q3 1 0.6667 0.3333 0.5565 10.33333 0.05 0.93
Q4 1 0.6021 0.2994 0.6031 11.00000 0.05 0.90
Q5 1 0.6667 0.3333 0.4114 10.33333 0.05 0.57
Q6 1 0.0000 0.0000 0.4457 10.33333 0.05 0.56
Q7 1 0.5996 0.3269 0.2500 10.50000 0.05 0.56
Q8 1 0.3333 -0.3333 0.2500 10.16667 0.05 0.52
Q9 1 0.7488 0.3637 0.2500 10.50000 0.05 0.46
Q10 1 0.5671 0.3453 0.5072 11.00000 0.05 0.46

;

#---------------------------------------------------------

data_(11)
_database_code_depnum_ccdc_archive 'CCDC 867234'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[1,3,5,7-tetrakis(1,2,4-triazol-4-yl)adamantane]silver(I)
Nitrate, Solvate with 3.5 Water
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C18 H20 Ag N12), (N O3), 3.5(H2 O)'
_chemical_formula_sum            'C18 H27 Ag N13 O6.50'
_chemical_formula_weight         637.40

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
_symmetry_Int_Tables_number      60

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

_cell_length_a                   11.9308(12)
_cell_length_b                   18.9239(12)
_cell_length_c                   22.4189(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5061.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    24142
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      26.02

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2600
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8889
_exptl_absorpt_correction_T_max  0.9188
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24142
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         26.02
_reflns_number_total             4831
_reflns_number_gt                2835
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Non-coordinated NO3^-^ anion is unequally disordered over two closely
separated positions (situated almost parallel at ca. 0.8-1.3 A). The
refined contributios were 0.60/0.40. The disorder was resolved with the
restrained geometry [N-O 1.25(1) A; O...O 2.17(1) A] and FLAT [0.01 A]
restraint for the planarity of NO3^-^ atoms. Only the N-atoms of both
components were refined anisotropically, while O-atoms were left
isotropic. In all other aspects, the refinement was standard. All
non-hydrogen atoms of the Ag-organic linkage were refined
anisotropically. The CH-hydrogen atoms were constrained with
U(iso) = 1.2U(eq) of the parent C-atom and with C-H distances 0.93 A
(triazole) and 0.97 A (CH2 adamantane). The OH-hydrogen atoms were
located and then constrained with O-H distances set to 0.85 A and
U(iso) = 1.5U(eq) of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4831
_refine_ls_number_parameters     354
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1534
_refine_ls_wR_factor_gt          0.1325
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.27978(4) 0.19757(2) 0.698250(18) 0.03903(19) Uani 1 1 d . . .
N1 N 0.3934(4) 0.2914(2) 0.6784(2) 0.0440(13) Uani 1 1 d . . .
N2 N 0.3694(5) 0.3601(3) 0.6834(3) 0.0737(19) Uani 1 1 d . . .
N3 N 0.5429(4) 0.3507(2) 0.65378(18) 0.0299(10) Uani 1 1 d . . .
N4 N 1.0148(4) 0.1746(2) 0.6681(3) 0.0587(15) Uani 1 1 d . . .
N5 N 1.0917(4) 0.2267(3) 0.6830(2) 0.0437(12) Uani 1 1 d . . .
N6 N 0.9374(3) 0.2791(2) 0.65630(18) 0.0283(10) Uani 1 1 d . . .
N7 N 0.9088(7) 0.6335(3) 0.6871(3) 0.099(3) Uani 1 1 d . . .
N8 N 0.8224(4) 0.6264(2) 0.7243(2) 0.0389(12) Uani 1 1 d . . .
N9 N 0.8325(4) 0.5305(2) 0.67067(19) 0.0317(10) Uani 1 1 d . . .
N10 N 0.7895(4) 0.3730(3) 0.3887(2) 0.0490(13) Uani 1 1 d . . .
N11 N 0.8180(5) 0.4433(3) 0.3926(2) 0.0523(14) Uani 1 1 d . . .
N12 N 0.7887(4) 0.4025(2) 0.48274(17) 0.0330(11) Uani 1 1 d . . .
C1 C 0.4975(5) 0.2865(3) 0.6624(3) 0.0532(18) Uani 1 1 d . . .
H1 H 0.5358 0.2441 0.6574 0.064 Uiso 1 1 calc R . .
C2 C 0.4594(6) 0.3931(3) 0.6689(4) 0.096(3) Uani 1 1 d . . .
H2 H 0.4653 0.4421 0.6691 0.116 Uiso 1 1 calc R . .
C3 C 0.9253(6) 0.2085(3) 0.6523(3) 0.0588(19) Uani 1 1 d . . .
H3 H 0.8599 0.1865 0.6395 0.071 Uiso 1 1 calc R . .
C4 C 1.0438(5) 0.2864(3) 0.6744(3) 0.0406(14) Uani 1 1 d . . .
H4 H 1.0788 0.3298 0.6801 0.049 Uiso 1 1 calc R . .
C5 C 0.9137(7) 0.5760(4) 0.6564(4) 0.108(4) Uani 1 1 d . . .
H5 H 0.9678 0.5672 0.6275 0.129 Uiso 1 1 calc R . .
C6 C 0.7773(5) 0.5658(3) 0.7134(3) 0.0473(17) Uani 1 1 d . . .
H6 H 0.7141 0.5487 0.7329 0.057 Uiso 1 1 calc R . .
C7 C 0.7731(5) 0.3504(3) 0.4430(2) 0.0488(16) Uani 1 1 d . . .
H7 H 0.7532 0.3043 0.4528 0.059 Uiso 1 1 calc R . .
C8 C 0.8179(5) 0.4592(3) 0.4495(3) 0.0463(16) Uani 1 1 d . . .
H8 H 0.8355 0.5035 0.4649 0.056 Uiso 1 1 calc R . .
C9 C 0.6572(4) 0.3698(2) 0.6346(2) 0.0240(11) Uani 1 1 d . . .
C10 C 0.7390(4) 0.3128(2) 0.6564(2) 0.0276(12) Uani 1 1 d . . .
H10A H 0.7355 0.3089 0.6995 0.033 Uiso 1 1 calc R . .
H10B H 0.7193 0.2674 0.6393 0.033 Uiso 1 1 calc R . .
C11 C 0.8564(4) 0.3339(3) 0.6371(2) 0.0268(12) Uani 1 1 d . . .
C12 C 0.8885(4) 0.4057(2) 0.6654(2) 0.0285(12) Uani 1 1 d . . .
H12A H 0.8864 0.4021 0.7085 0.034 Uiso 1 1 calc R . .
H12B H 0.9640 0.4187 0.6536 0.034 Uiso 1 1 calc R . .
C13 C 0.8066(4) 0.4609(3) 0.6445(2) 0.0266(12) Uani 1 1 d . . .
C14 C 0.6870(4) 0.4412(3) 0.6630(2) 0.0278(12) Uani 1 1 d . . .
H14A H 0.6349 0.4772 0.6497 0.033 Uiso 1 1 calc R . .
H14B H 0.6821 0.4378 0.7061 0.033 Uiso 1 1 calc R . .
C15 C 0.6623(4) 0.3758(3) 0.5664(2) 0.0283(12) Uani 1 1 d . . .
H15A H 0.6427 0.3309 0.5483 0.034 Uiso 1 1 calc R . .
H15B H 0.6096 0.4112 0.5526 0.034 Uiso 1 1 calc R . .
C16 C 0.7817(4) 0.3967(3) 0.5487(2) 0.0268(12) Uani 1 1 d . . .
C17 C 0.8629(4) 0.3396(3) 0.5683(2) 0.0282(12) Uani 1 1 d . . .
H17A H 0.9385 0.3517 0.5561 0.034 Uiso 1 1 calc R . .
H17B H 0.8430 0.2948 0.5502 0.034 Uiso 1 1 calc R . .
C18 C 0.8122(4) 0.4675(3) 0.5764(2) 0.0296(12) Uani 1 1 d . . .
H18A H 0.7603 0.5036 0.5629 0.036 Uiso 1 1 calc R . .
H18B H 0.8872 0.4812 0.5643 0.036 Uiso 1 1 calc R . .
O4 O 0.1660(4) 0.4385(2) 0.68867(17) 0.0541(12) Uani 1 1 d . . .
H1W H 0.2255 0.4144 0.6841 0.081 Uiso 1 1 d R . .
H2W H 0.1685 0.4738 0.6653 0.081 Uiso 1 1 d R . .
O5 O 1.0000 0.0495(3) 0.7500 0.071(2) Uani 1 2 d S . .
H3W H 1.0181 0.0757 0.7208 0.107 Uiso 1 1 d R . .
O6 O 1.0251(5) 0.0422(3) 0.5874(3) 0.113(2) Uani 1 1 d . . .
H4W H 1.0640 0.0685 0.6101 0.170 Uiso 1 1 d R . .
H5W H 1.0196 0.0620 0.5535 0.170 Uiso 1 1 d R . .
O7 O 0.8928(5) 0.0665(4) 0.4907(4) 0.162(3) Uani 1 1 d . . .
H6W H 0.8774 0.0332 0.4665 0.243 Uiso 1 1 d R . .
H7W H 0.8422 0.0979 0.4879 0.243 Uiso 1 1 d R . .
N13 N 0.8655(9) 0.6645(5) 0.5256(3) 0.088(5) Uani 0.60 1 d PD A -1
O1 O 0.9035(8) 0.6093(4) 0.5053(4) 0.077(3) Uiso 0.60 1 d PD A -1
O2 O 0.7667(9) 0.6733(7) 0.5398(7) 0.141(5) Uiso 0.60 1 d PD A -1
O3 O 0.9335(10) 0.7145(6) 0.5328(6) 0.163(5) Uiso 0.60 1 d PD A -1
N13A N 0.8310(12) 0.6720(7) 0.4919(5) 0.104(9) Uani 0.40 1 d PD B -2
O1A O 0.8655(12) 0.6117(6) 0.4826(6) 0.076(4) Uiso 0.40 1 d PD B -2
O2A O 0.7303(12) 0.6825(10) 0.5041(12) 0.173(10) Uiso 0.40 1 d PD B -2
O3A O 0.8967(14) 0.7234(7) 0.4891(8) 0.133(6) Uiso 0.40 1 d PD B -2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0406(3) 0.0347(3) 0.0417(3) 0.0062(2) -0.0029(2) -0.0062(2)
N1 0.033(3) 0.032(3) 0.067(3) 0.008(2) 0.009(3) -0.008(2)
N2 0.044(4) 0.032(3) 0.145(6) -0.011(3) 0.039(4) 0.003(3)
N3 0.025(3) 0.023(2) 0.042(2) -0.002(2) 0.007(2) 0.001(2)
N4 0.035(3) 0.030(3) 0.111(5) 0.004(3) -0.018(3) 0.003(3)
N5 0.032(3) 0.036(3) 0.063(3) 0.002(2) -0.009(2) 0.000(2)
N6 0.025(3) 0.018(2) 0.042(2) 0.0021(19) -0.005(2) 0.0016(19)
N7 0.127(6) 0.054(4) 0.116(5) -0.045(4) 0.077(5) -0.054(4)
N8 0.042(3) 0.026(3) 0.048(3) -0.010(2) 0.011(3) -0.002(2)
N9 0.034(3) 0.020(2) 0.041(2) -0.010(2) 0.012(2) -0.001(2)
N10 0.062(4) 0.044(3) 0.040(3) -0.004(2) 0.008(3) -0.007(3)
N11 0.068(4) 0.047(4) 0.041(3) 0.009(2) 0.008(3) -0.005(3)
N12 0.038(3) 0.033(3) 0.028(2) 0.003(2) 0.004(2) -0.002(2)
C1 0.026(4) 0.036(4) 0.098(5) 0.002(3) 0.010(4) -0.001(3)
C2 0.041(4) 0.022(4) 0.226(10) -0.003(5) 0.048(6) -0.005(3)
C3 0.046(4) 0.032(4) 0.099(5) 0.001(4) -0.011(4) -0.001(3)
C4 0.033(4) 0.023(3) 0.065(4) 0.004(3) -0.010(3) -0.001(3)
C5 0.122(8) 0.063(5) 0.138(8) -0.059(5) 0.098(7) -0.061(5)
C6 0.056(4) 0.042(4) 0.044(3) -0.014(3) 0.019(3) -0.014(3)
C7 0.074(5) 0.037(4) 0.036(3) 0.000(3) 0.003(3) -0.010(3)
C8 0.057(4) 0.035(4) 0.047(4) 0.007(3) 0.010(3) -0.003(3)
C9 0.015(3) 0.018(3) 0.038(3) 0.002(2) 0.007(2) -0.004(2)
C10 0.030(3) 0.018(3) 0.035(3) 0.001(2) 0.006(2) -0.001(2)
C11 0.026(3) 0.024(3) 0.030(3) 0.004(2) -0.002(2) 0.005(2)
C12 0.029(3) 0.024(3) 0.032(3) -0.001(2) 0.005(2) -0.004(2)
C13 0.030(3) 0.020(3) 0.030(3) -0.003(2) 0.004(2) 0.001(2)
C14 0.023(3) 0.026(3) 0.034(3) -0.002(2) 0.005(2) 0.000(2)
C15 0.023(3) 0.028(3) 0.033(3) -0.003(2) -0.003(2) 0.001(2)
C16 0.027(3) 0.027(3) 0.026(2) -0.001(2) 0.000(2) -0.007(2)
C17 0.031(3) 0.022(3) 0.031(3) 0.000(2) 0.001(2) 0.002(2)
C18 0.027(3) 0.026(3) 0.036(3) -0.002(2) 0.010(2) -0.004(2)
O4 0.049(3) 0.051(3) 0.062(3) 0.012(2) 0.011(2) 0.002(2)
O5 0.078(5) 0.045(4) 0.091(5) 0.000 -0.025(4) 0.000
O6 0.125(5) 0.088(4) 0.127(5) -0.016(4) 0.020(4) -0.026(4)
O7 0.089(5) 0.178(7) 0.219(8) -0.023(6) 0.021(6) -0.019(5)
N13 0.060(8) 0.062(9) 0.144(13) 0.014(8) 0.037(9) 0.018(6)
N13A 0.107(19) 0.052(13) 0.15(2) 0.032(13) 0.066(17) -0.017(13)

_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.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N8 2.256(4) 6_557 ?
Ag1 N1 2.277(4) . ?
Ag1 N5 2.335(5) 1_455 ?
Ag1 N10 2.366(5) 4_456 ?
N1 C1 1.297(7) . ?
N1 N2 1.335(6) . ?
N2 C2 1.283(8) . ?
N3 C2 1.323(7) . ?
N3 C1 1.344(7) . ?
N3 C9 1.475(6) . ?
N4 C3 1.295(8) . ?
N4 N5 1.387(7) . ?
N5 C4 1.282(7) . ?
N5 Ag1 2.335(5) 1_655 ?
N6 C4 1.339(7) . ?
N6 C3 1.348(7) . ?
N6 C11 1.481(6) . ?
N7 C5 1.288(8) . ?
N7 N8 1.334(7) . ?
N8 C6 1.289(7) . ?
N8 Ag1 2.256(4) 6_667 ?
N9 C5 1.336(8) . ?
N9 C6 1.341(7) . ?
N9 C13 1.474(6) . ?
N10 C7 1.306(7) . ?
N10 N11 1.376(7) . ?
N10 Ag1 2.366(5) 4_556 ?
N11 C8 1.311(7) . ?
N12 C7 1.341(7) . ?
N12 C8 1.353(7) . ?
N12 C16 1.484(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C15 1.533(6) . ?
C9 C14 1.535(6) . ?
C9 C10 1.536(7) . ?
C10 C11 1.520(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.547(7) . ?
C11 C17 1.548(6) . ?
C12 C13 1.506(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.532(7) . ?
C13 C18 1.535(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.530(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.517(7) . ?
C16 C18 1.522(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
O4 H1W 0.8500 . ?
O4 H2W 0.8500 . ?
O5 H3W 0.8500 . ?
O6 H4W 0.8500 . ?
O6 H5W 0.8500 . ?
O7 H6W 0.8500 . ?
O7 H7W 0.8500 . ?
N13 O1 1.227(8) . ?
N13 O2 1.231(8) . ?
N13 O3 1.257(8) . ?
N13A O1A 1.230(8) . ?
N13A O2A 1.248(9) . ?
N13A O3A 1.251(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Ag1 N1 118.81(18) 6_557 . ?
N8 Ag1 N5 118.04(18) 6_557 1_455 ?
N1 Ag1 N5 111.04(17) . 1_455 ?
N8 Ag1 N10 106.61(18) 6_557 4_456 ?
N1 Ag1 N10 104.50(18) . 4_456 ?
N5 Ag1 N10 93.43(17) 1_455 4_456 ?
C1 N1 N2 107.3(5) . . ?
C1 N1 Ag1 124.7(4) . . ?
N2 N1 Ag1 128.0(4) . . ?
C2 N2 N1 105.9(5) . . ?
C2 N3 C1 101.9(5) . . ?
C2 N3 C9 128.5(4) . . ?
C1 N3 C9 129.5(4) . . ?
C3 N4 N5 105.1(5) . . ?
C4 N5 N4 107.2(5) . . ?
C4 N5 Ag1 131.2(4) . 1_655 ?
N4 N5 Ag1 120.2(3) . 1_655 ?
C4 N6 C3 103.0(5) . . ?
C4 N6 C11 129.3(4) . . ?
C3 N6 C11 127.2(5) . . ?
C5 N7 N8 106.5(5) . . ?
C6 N8 N7 107.1(5) . . ?
C6 N8 Ag1 125.7(4) . 6_667 ?
N7 N8 Ag1 126.6(4) . 6_667 ?
C5 N9 C6 101.8(5) . . ?
C5 N9 C13 129.3(5) . . ?
C6 N9 C13 128.8(5) . . ?
C7 N10 N11 107.2(5) . . ?
C7 N10 Ag1 125.1(4) . 4_556 ?
N11 N10 Ag1 127.6(4) . 4_556 ?
C8 N11 N10 106.4(5) . . ?
C7 N12 C8 104.6(5) . . ?
C7 N12 C16 126.8(4) . . ?
C8 N12 C16 128.5(5) . . ?
N1 C1 N3 111.2(5) . . ?
N1 C1 H1 124.4 . . ?
N3 C1 H1 124.4 . . ?
N2 C2 N3 113.6(5) . . ?
N2 C2 H2 123.2 . . ?
N3 C2 H2 123.2 . . ?
N4 C3 N6 112.6(6) . . ?
N4 C3 H3 123.7 . . ?
N6 C3 H3 123.7 . . ?
N5 C4 N6 112.2(5) . . ?
N5 C4 H4 123.9 . . ?
N6 C4 H4 123.9 . . ?
N7 C5 N9 112.6(6) . . ?
N7 C5 H5 123.7 . . ?
N9 C5 H5 123.7 . . ?
N8 C6 N9 112.0(5) . . ?
N8 C6 H6 124.0 . . ?
N9 C6 H6 124.0 . . ?
N10 C7 N12 110.9(5) . . ?
N10 C7 H7 124.5 . . ?
N12 C7 H7 124.5 . . ?
N11 C8 N12 110.8(5) . . ?
N11 C8 H8 124.6 . . ?
N12 C8 H8 124.6 . . ?
N3 C9 C15 110.2(4) . . ?
N3 C9 C14 108.0(4) . . ?
C15 C9 C14 109.9(4) . . ?
N3 C9 C10 108.8(4) . . ?
C15 C9 C10 110.1(4) . . ?
C14 C9 C10 109.8(4) . . ?
C11 C10 C9 108.1(4) . . ?
C11 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N6 C11 C10 109.6(4) . . ?
N6 C11 C12 109.5(4) . . ?
C10 C11 C12 110.0(4) . . ?
N6 C11 C17 107.8(4) . . ?
C10 C11 C17 110.4(4) . . ?
C12 C11 C17 109.6(4) . . ?
C13 C12 C11 108.8(4) . . ?
C13 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C13 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N9 C13 C12 111.1(4) . . ?
N9 C13 C14 107.8(4) . . ?
C12 C13 C14 110.6(4) . . ?
N9 C13 C18 108.3(4) . . ?
C12 C13 C18 109.7(4) . . ?
C14 C13 C18 109.3(4) . . ?
C13 C14 C9 108.5(4) . . ?
C13 C14 H14A 110.0 . . ?
C9 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
C9 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
C16 C15 C9 108.4(4) . . ?
C16 C15 H15A 110.0 . . ?
C9 C15 H15A 110.0 . . ?
C16 C15 H15B 110.0 . . ?
C9 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
N12 C16 C17 107.8(4) . . ?
N12 C16 C18 109.1(4) . . ?
C17 C16 C18 110.9(4) . . ?
N12 C16 C15 109.3(4) . . ?
C17 C16 C15 109.6(4) . . ?
C18 C16 C15 110.1(4) . . ?
C16 C17 C11 107.9(4) . . ?
C16 C17 H17A 110.1 . . ?
C11 C17 H17A 110.1 . . ?
C16 C17 H17B 110.1 . . ?
C11 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C16 C18 C13 108.9(4) . . ?
C16 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
C16 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
H1W O4 H2W 108.5 . . ?
H4W O6 H5W 108.5 . . ?
H6W O7 H7W 108.5 . . ?
O1 N13 O2 124.4(9) . . ?
O1 N13 O3 116.7(8) . . ?
O2 N13 O3 118.8(9) . . ?
O1A N13A O2A 120.5(9) . . ?
O1A N13A O3A 120.2(9) . . ?
O2A N13A O3A 119.3(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
N8 Ag1 N1 C1 63.8(6) 6_557 . . . ?
N5 Ag1 N1 C1 -154.4(5) 1_455 . . . ?
N10 Ag1 N1 C1 -54.8(6) 4_456 . . . ?
N8 Ag1 N1 N2 -112.9(5) 6_557 . . . ?
N5 Ag1 N1 N2 28.9(6) 1_455 . . . ?
N10 Ag1 N1 N2 128.5(5) 4_456 . . . ?
C1 N1 N2 C2 1.2(9) . . . . ?
Ag1 N1 N2 C2 178.4(6) . . . . ?
C3 N4 N5 C4 -0.8(7) . . . . ?
C3 N4 N5 Ag1 -168.7(4) . . . 1_655 ?
C5 N7 N8 C6 -1.6(9) . . . . ?
C5 N7 N8 Ag1 169.1(6) . . . 6_667 ?
C7 N10 N11 C8 0.4(7) . . . . ?
Ag1 N10 N11 C8 -176.8(4) 4_556 . . . ?
N2 N1 C1 N3 -2.8(8) . . . . ?
Ag1 N1 C1 N3 180.0(4) . . . . ?
C2 N3 C1 N1 3.0(8) . . . . ?
C9 N3 C1 N1 -178.9(5) . . . . ?
N1 N2 C2 N3 0.7(11) . . . . ?
C1 N3 C2 N2 -2.3(10) . . . . ?
C9 N3 C2 N2 179.7(6) . . . . ?
N5 N4 C3 N6 -0.6(8) . . . . ?
C4 N6 C3 N4 1.7(8) . . . . ?
C11 N6 C3 N4 174.3(5) . . . . ?
N4 N5 C4 N6 1.9(7) . . . . ?
Ag1 N5 C4 N6 168.1(4) 1_655 . . . ?
C3 N6 C4 N5 -2.2(7) . . . . ?
C11 N6 C4 N5 -174.6(5) . . . . ?
N8 N7 C5 N9 1.1(11) . . . . ?
C6 N9 C5 N7 -0.1(10) . . . . ?
C13 N9 C5 N7 177.3(7) . . . . ?
N7 N8 C6 N9 1.6(8) . . . . ?
Ag1 N8 C6 N9 -169.2(4) 6_667 . . . ?
C5 N9 C6 N8 -0.9(8) . . . . ?
C13 N9 C6 N8 -178.4(5) . . . . ?
N11 N10 C7 N12 0.3(7) . . . . ?
Ag1 N10 C7 N12 177.6(4) 4_556 . . . ?
C8 N12 C7 N10 -0.9(7) . . . . ?
C16 N12 C7 N10 -177.7(5) . . . . ?
N10 N11 C8 N12 -1.0(7) . . . . ?
C7 N12 C8 N11 1.2(7) . . . . ?
C16 N12 C8 N11 177.9(5) . . . . ?
C2 N3 C9 C15 -92.0(8) . . . . ?
C1 N3 C9 C15 90.4(6) . . . . ?
C2 N3 C9 C14 28.0(8) . . . . ?
C1 N3 C9 C14 -149.5(6) . . . . ?
C2 N3 C9 C10 147.1(7) . . . . ?
C1 N3 C9 C10 -30.5(7) . . . . ?
N3 C9 C10 C11 -179.1(4) . . . . ?
C15 C9 C10 C11 60.0(5) . . . . ?
C14 C9 C10 C11 -61.2(5) . . . . ?
C4 N6 C11 C10 -145.6(5) . . . . ?
C3 N6 C11 C10 43.7(7) . . . . ?
C4 N6 C11 C12 -24.9(7) . . . . ?
C3 N6 C11 C12 164.4(5) . . . . ?
C4 N6 C11 C17 94.2(6) . . . . ?
C3 N6 C11 C17 -76.5(7) . . . . ?
C9 C10 C11 N6 -178.7(4) . . . . ?
C9 C10 C11 C12 60.8(5) . . . . ?
C9 C10 C11 C17 -60.2(5) . . . . ?
N6 C11 C12 C13 179.0(4) . . . . ?
C10 C11 C12 C13 -60.5(5) . . . . ?
C17 C11 C12 C13 61.0(5) . . . . ?
C5 N9 C13 C12 75.8(9) . . . . ?
C6 N9 C13 C12 -107.4(6) . . . . ?
C5 N9 C13 C14 -162.9(7) . . . . ?
C6 N9 C13 C14 13.9(7) . . . . ?
C5 N9 C13 C18 -44.8(9) . . . . ?
C6 N9 C13 C18 132.0(6) . . . . ?
C11 C12 C13 N9 179.4(4) . . . . ?
C11 C12 C13 C14 59.7(5) . . . . ?
C11 C12 C13 C18 -60.9(5) . . . . ?
N9 C13 C14 C9 178.3(4) . . . . ?
C12 C13 C14 C9 -60.1(5) . . . . ?
C18 C13 C14 C9 60.8(5) . . . . ?
N3 C9 C14 C13 178.8(4) . . . . ?
C15 C9 C14 C13 -60.9(5) . . . . ?
C10 C9 C14 C13 60.3(5) . . . . ?
N3 C9 C15 C16 179.2(4) . . . . ?
C14 C9 C15 C16 60.3(5) . . . . ?
C10 C9 C15 C16 -60.8(5) . . . . ?
C7 N12 C16 C17 56.2(7) . . . . ?
C8 N12 C16 C17 -119.9(6) . . . . ?
C7 N12 C16 C18 176.7(5) . . . . ?
C8 N12 C16 C18 0.6(7) . . . . ?
C7 N12 C16 C15 -62.8(7) . . . . ?
C8 N12 C16 C15 121.1(6) . . . . ?
C9 C15 C16 N12 179.8(4) . . . . ?
C9 C15 C16 C17 61.9(5) . . . . ?
C9 C15 C16 C18 -60.4(5) . . . . ?
N12 C16 C17 C11 179.5(4) . . . . ?
C18 C16 C17 C11 60.2(5) . . . . ?
C15 C16 C17 C11 -61.6(5) . . . . ?
N6 C11 C17 C16 -178.9(4) . . . . ?
C10 C11 C17 C16 61.5(5) . . . . ?
C12 C11 C17 C16 -59.8(5) . . . . ?
N12 C16 C18 C13 -179.1(4) . . . . ?
C17 C16 C18 C13 -60.5(5) . . . . ?
C15 C16 C18 C13 60.9(5) . . . . ?
N9 C13 C18 C16 -178.1(4) . . . . ?
C12 C13 C18 C16 60.5(5) . . . . ?
C14 C13 C18 C16 -60.9(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.108

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk21 in Pbcn
CELL 0.71073 11.9308 18.9239 22.4189 90.000 90.000 90.000
ZERR 8.00 0.0012 0.0012 0.0015 0.000 0.000 0.000
LATT 1
SYMM 1/2 - X, 1/2 - Y, 1/2 + Z
SYMM - X, Y, 1/2 - Z
SYMM 1/2 + X, 1/2 - Y, - Z
SFAC C H N O AG
UNIT 144 216 104 52 8
MERG 2
OMIT 0.00 180.00
OMIT 1 22 5
SHEL 0.81 7
DFIX 1.25 0.01 N13 O1 N13 O2 N13 O3
DFIX 1.25 0.01 N13a O1a N13a O2a N13a O3a
DFIX 2.17 0.01 O1 O2 O1 O3 O2 O3
DFIX 2.17 0.01 O1a O2a O1a O3a O2a O3a
FLAT 0.01 N13 O1 O2 O3
FLAT 0.01 N13A O1A O2A O3A
EQIV $1 1-X, 1-Y, 1-Z
EQIV $2 2-X, -Y, 1-Z
EQIV $3 1.5-X, -0.5+Y, Z
RTAB XHY O4 H1W N2
RTAB XHY O4 H2W N11_$1
RTAB XHY O5 H3W N4
RTAB XHY O6 H4W N4
RTAB XHY O6 H5W O7
RTAB XHY O7 H6W O6_$2
RTAB XHY O7 H7W O2A_$3
RTAB XHY O7 H7W O2_$3
RTAB H..O H1W N2
RTAB H..O H2W N11_$1
RTAB H..O H3W N4
RTAB H..O H4W N4
RTAB H..O H5W O7
RTAB H..O H6W O6_$2
RTAB H..O H7W O2A_$3
RTAB H..O H7W O2_$3
RTAB O..O O4 N2
RTAB O..O O4 N11_$1
RTAB O..O O5 N4
RTAB O..O O6 N4
RTAB O..O O6 O7
RTAB O..O O7 O6_$2
RTAB O..O O7 O2A_$3
RTAB O..O O7 O2_$3
FMAP 2
PLAN 20
SIZE 0.10 0.11 0.14
ACTA
BOND
CONF
BOND $H
L.S. 4
TEMP 23.00
WGHT 0.076500
FVAR 0.04846
AG1 5 0.279783 0.197571 0.698250 11.00000 0.04060 0.03474 =
0.04175 0.00616 -0.00292 -0.00621
N1 3 0.393357 0.291403 0.678427 11.00000 0.03320 0.03172 =
0.06713 0.00784 0.00887 -0.00789
N2 3 0.369400 0.360053 0.683386 11.00000 0.04404 0.03183 =
0.14516 -0.01101 0.03889 0.00294
N3 3 0.542884 0.350736 0.653778 11.00000 0.02481 0.02301 =
0.04186 -0.00247 0.00740 0.00146
N4 3 1.014828 0.174611 0.668059 11.00000 0.03496 0.02977 =
0.11124 0.00436 -0.01810 0.00318
N5 3 1.091732 0.226687 0.682981 11.00000 0.03226 0.03566 =
0.06313 0.00244 -0.00944 0.00000
N6 3 0.937443 0.279109 0.656295 11.00000 0.02496 0.01801 =
0.04188 0.00208 -0.00451 0.00158
N7 3 0.908842 0.633504 0.687067 11.00000 0.12712 0.05371 =
0.11610 -0.04501 0.07698 -0.05350
N8 3 0.822361 0.626392 0.724295 11.00000 0.04236 0.02609 =
0.04823 -0.00970 0.01059 -0.00159
N9 3 0.832521 0.530493 0.670672 11.00000 0.03405 0.01999 =
0.04111 -0.01009 0.01167 -0.00139
N10 3 0.789538 0.373034 0.388679 11.00000 0.06245 0.04439 =
0.04021 -0.00393 0.00785 -0.00707
N11 3 0.818011 0.443329 0.392571 11.00000 0.06823 0.04735 =
0.04143 0.00881 0.00763 -0.00452
N12 3 0.788739 0.402458 0.482741 11.00000 0.03831 0.03268 =
0.02811 0.00264 0.00374 -0.00181
C1 1 0.497476 0.286543 0.662354 11.00000 0.02591 0.03592 =
0.09764 0.00164 0.00984 -0.00126
AFIX 43
H1 2 0.535760 0.244138 0.657403 11.00000 -1.20000
AFIX 0
C2 1 0.459363 0.393061 0.668944 11.00000 0.04085 0.02178 =
0.22617 -0.00261 0.04813 -0.00512
AFIX 43
H2 2 0.465277 0.442063 0.669124 11.00000 -1.20000
AFIX 0
C3 1 0.925320 0.208466 0.652253 11.00000 0.04593 0.03176 =
0.09870 0.00126 -0.01125 -0.00115
AFIX 43
H3 2 0.859866 0.186457 0.639512 11.00000 -1.20000
AFIX 0
C4 1 1.043779 0.286429 0.674417 11.00000 0.03336 0.02345 =
0.06499 0.00410 -0.01035 -0.00121
AFIX 43
H4 2 1.078754 0.329825 0.680124 11.00000 -1.20000
AFIX 0
C5 1 0.913715 0.576048 0.656401 11.00000 0.12224 0.06270 =
0.13824 -0.05897 0.09817 -0.06109
AFIX 43
H5 2 0.967836 0.567239 0.627488 11.00000 -1.20000
AFIX 0
C6 1 0.777329 0.565840 0.713401 11.00000 0.05628 0.04186 =
0.04371 -0.01436 0.01936 -0.01425
AFIX 43
H6 2 0.714082 0.548698 0.732857 11.00000 -1.20000
AFIX 0
C7 1 0.773079 0.350397 0.443006 11.00000 0.07353 0.03698 =
0.03587 -0.00024 0.00328 -0.01005
AFIX 43
H7 2 0.753159 0.304332 0.452830 11.00000 -1.20000
AFIX 0
C8 1 0.817889 0.459197 0.449471 11.00000 0.05669 0.03534 =
0.04697 0.00670 0.01019 -0.00343
AFIX 43
H8 2 0.835457 0.503457 0.464888 11.00000 -1.20000
AFIX 0
C9 1 0.657200 0.369839 0.634568 11.00000 0.01536 0.01814 =
0.03847 0.00193 0.00664 -0.00374
C10 1 0.739006 0.312795 0.656421 11.00000 0.02996 0.01751 =
0.03541 0.00089 0.00627 -0.00069
AFIX 23
H10A 2 0.735503 0.308932 0.699525 11.00000 -1.20000
H10B 2 0.719337 0.267360 0.639344 11.00000 -1.20000
AFIX 0
C11 1 0.856416 0.333896 0.637103 11.00000 0.02645 0.02369 =
0.03031 0.00375 -0.00232 0.00459
C12 1 0.888532 0.405658 0.665379 11.00000 0.02940 0.02390 =
0.03207 -0.00110 0.00531 -0.00440
AFIX 23
H12A 2 0.886410 0.402085 0.708526 11.00000 -1.20000
H12B 2 0.963956 0.418692 0.653553 11.00000 -1.20000
AFIX 0
C13 1 0.806578 0.460902 0.644529 11.00000 0.02983 0.02036 =
0.02955 -0.00252 0.00406 0.00111
C14 1 0.687008 0.441154 0.663029 11.00000 0.02329 0.02613 =
0.03394 -0.00222 0.00521 -0.00035
AFIX 23
H14A 2 0.634908 0.477198 0.649702 11.00000 -1.20000
H14B 2 0.682123 0.437751 0.706123 11.00000 -1.20000
AFIX 0
C15 1 0.662307 0.375791 0.566420 11.00000 0.02349 0.02845 =
0.03292 -0.00345 -0.00254 0.00133
AFIX 23
H15A 2 0.642662 0.330898 0.548343 11.00000 -1.20000
H15B 2 0.609551 0.411211 0.552639 11.00000 -1.20000
AFIX 0
C16 1 0.781653 0.396681 0.548665 11.00000 0.02717 0.02730 =
0.02594 -0.00117 0.00045 -0.00729
C17 1 0.862916 0.339599 0.568297 11.00000 0.03079 0.02237 =
0.03135 -0.00014 0.00119 0.00246
AFIX 23
H17A 2 0.938512 0.351709 0.556088 11.00000 -1.20000
H17B 2 0.842968 0.294788 0.550170 11.00000 -1.20000
AFIX 0
C18 1 0.812169 0.467542 0.576370 11.00000 0.02651 0.02635 =
0.03607 -0.00241 0.01013 -0.00401
AFIX 23
H18A 2 0.760308 0.503634 0.562874 11.00000 -1.20000
H18B 2 0.887177 0.481156 0.564261 11.00000 -1.20000
AFIX 0
O4 4 0.166004 0.438507 0.688666 11.00000 0.04927 0.05101 =
0.06213 0.01176 0.01133 0.00227
AFIX 3
H1W 2 0.225545 0.414431 0.684135 11.00000 -1.50000
H2W 2 0.168550 0.473825 0.665280 11.00000 -1.50000
AFIX 0
O5 4 1.000000 0.049496 0.750000 10.50000 0.07807 0.04521 =
0.09064 0.00000 -0.02495 0.00000
AFIX 3
H3W 2 1.018143 0.075732 0.720777 11.00000 -1.50000
AFIX 0
O6 4 1.025051 0.042198 0.587378 11.00000 0.12469 0.08762 =
0.12744 -0.01641 0.02046 -0.02639
AFIX 3
H4W 2 1.063981 0.068502 0.610081 11.00000 -1.50000
H5W 2 1.019649 0.062043 0.553487 11.00000 -1.50000
AFIX 0
O7 4 0.892834 0.066453 0.490657 11.00000 0.08933 0.17788 =
0.21858 -0.02325 0.02108 -0.01883
AFIX 3
H6W 2 0.877411 0.033199 0.466517 11.00000 -1.50000
H7W 2 0.842154 0.097862 0.487907 11.00000 -1.50000
AFIX 0
PART -1
N13 3 0.865480 0.664501 0.525645 10.60000 0.05962 0.06171 =
0.14392 0.01361 0.03705 0.01792
O1 4 0.903511 0.609325 0.505267 10.60000 0.07680
O2 4 0.766735 0.673324 0.539776 10.60000 0.14072
O3 4 0.933473 0.714539 0.532785 10.60000 0.16268
PART -2
N13A 3 0.830987 0.671951 0.491936 10.40000 0.10700 0.05188 =
0.15256 0.03166 0.06648 -0.01745
O1A 4 0.865475 0.611717 0.482644 10.40000 0.07586
O2A 4 0.730332 0.682516 0.504111 10.40000 0.17341
O3A 4 0.896674 0.723370 0.489120 10.40000 0.13328
HKLF 4

REM dk21 in Pbcn
REM R1 = 0.0541 for 2835 Fo > 4sig(Fo) and 0.1094 for all 4831 data
REM 354 parameters refined using 14 restraints

END

WGHT 0.0765 0.0000
REM Highest difference peak 0.763, deepest hole -0.792, 1-sigma level 0.108
Q1 1 0.8517 0.6657 0.5070 11.00000 0.05 0.76
Q2 1 0.3550 0.1826 0.6973 11.00000 0.05 0.76
Q3 1 0.7662 0.6997 0.5146 11.00000 0.05 0.65
Q4 1 0.8154 0.7090 0.5490 11.00000 0.05 0.59
Q5 1 0.4884 0.2258 0.6797 11.00000 0.05 0.57
Q6 1 0.7775 0.6470 0.5792 11.00000 0.05 0.55
Q7 1 0.9422 0.1709 0.5043 11.00000 0.05 0.55
Q8 1 0.9255 0.6203 0.5357 11.00000 0.05 0.49
Q9 1 0.9638 0.6705 0.5526 11.00000 0.05 0.46
Q10 1 0.8345 0.6472 0.6662 11.00000 0.05 0.40

;

#---------------------------------------------------------

data_(12)
_database_code_depnum_ccdc_archive 'CCDC 867235'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[1,3,5,7-tetrakis(1,2,4-triazol-4-yl)adamantane]aquacopper(II)
Perchlorate Trihydrate
;
_chemical_name_common            
;
(1,3,5,7-tetrakis(1,2,4-triazol-4-
yl)adamantane)aquacopper(ii) Perchlorate Trihydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H22 Cu N12 O, 2(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C18 H28 Cl2 Cu N12 O12'
_chemical_formula_weight         738.96

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_symmetry_Int_Tables_number      62

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

_cell_length_a                   17.1623(13)
_cell_length_b                   13.1560(8)
_cell_length_c                   12.8631(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2904.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      6.83
_cell_measurement_theta_max      26.37

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1516
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7779
_exptl_absorpt_correction_T_max  0.8381
_exptl_absorpt_process_details   
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11791
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         6.83
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3041
_reflns_number_gt                1910
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The non-coordinated ClO4^-^ anion is unequally disordered by two
overlapping positions (one O-atom, referred O5, is common for both
contributions). The partial occupancy factors were set 0.70/0.30, as
was suggested by refinement of the isotropic thermal parameters. Soft
restraints in the ClO4^-^ geometry [Cl-O 1.42(1) A; O...O 2.30(1) A]
were applied and the disordered atoms were refined anisotropically with
SIMU restraints for two pairs of very closely separated O-atoms
(Total number of restraints in the structure is 37).

Two present solvate water molecules are also disordered over two close
positions (0.99 and 1.29 A). They were refined anisotropically with
partial occupancies 0.50/0.50 and 0.55/0.45, and the corresponding
H-atoms were not added.

The CH-hydrogen atoms were constrained with U(iso) = 1.2U(eq) of
the parent C-atom and with C-H distances 0.94 A (triazole), 0.98 A
(CH2 adamantane). The OH-hydrogen atom for the coordinated water
molecule O1 (mirror plane) was located and then constrained with O-H
distance set to 0.85 A and U(iso) = 1.5U(eq) of the parent O-atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+2.3289P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3041
_refine_ls_number_parameters     280
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2135
_refine_ls_wR_factor_gt          0.1985
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.06616(5) 0.7500 0.83615(6) 0.0289(3) Uani 1 2 d S . .
O1 O -0.0533(5) 0.7500 0.8985(6) 0.082(3) Uani 1 2 d S . .
H1W H -0.0822 0.8023 0.8944 0.123 Uiso 1 1 d R . .
N1 N 0.0752(3) 0.5975(4) 0.8310(3) 0.0351(11) Uani 1 1 d . . .
N2 N 0.0513(5) 0.5415(5) 0.9129(4) 0.073(2) Uani 1 1 d . . .
N3 N 0.0845(3) 0.4385(4) 0.7870(3) 0.0299(11) Uani 1 1 d . . .
N4 N -0.0438(4) 0.2500 0.3162(4) 0.0377(17) Uani 1 2 d S . .
N5 N -0.1059(5) 0.2500 0.3835(5) 0.052(2) Uani 1 2 d S . .
N6 N 0.0024(4) 0.2500 0.4746(4) 0.0295(14) Uani 1 2 d S . .
N7 N 0.3774(4) 0.2500 0.4719(4) 0.0305(14) Uani 1 2 d S . .
N8 N 0.4061(4) 0.2500 0.5722(5) 0.046(2) Uani 1 2 d S . .
N9 N 0.2775(4) 0.2500 0.5774(4) 0.0277(13) Uani 1 2 d S . .
C1 C 0.0932(3) 0.5344(5) 0.7563(3) 0.0327(12) Uani 1 1 d . . .
H1 H 0.1100 0.5541 0.6898 0.039 Uiso 1 1 calc R . .
C2 C 0.0572(6) 0.4458(6) 0.8850(5) 0.068(3) Uani 1 1 d . . .
H2 H 0.0442 0.3901 0.9275 0.082 Uiso 1 1 calc R . .
C3 C 0.0216(5) 0.2500 0.3718(5) 0.0364(19) Uani 1 2 d S . .
H3 H 0.0725 0.2500 0.3447 0.044 Uiso 1 2 calc SR . .
C4 C -0.0768(5) 0.2500 0.4743(6) 0.054(3) Uani 1 2 d S . .
H4 H -0.1071 0.2500 0.5352 0.065 Uiso 1 2 calc SR . .
C5 C 0.3014(5) 0.2500 0.4775(5) 0.042(2) Uani 1 2 d S . .
H5 H 0.2679 0.2500 0.4197 0.050 Uiso 1 2 calc SR . .
C6 C 0.3439(5) 0.2500 0.6328(5) 0.045(2) Uani 1 2 d S . .
H6 H 0.3458 0.2500 0.7058 0.054 Uiso 1 2 calc SR . .
C7 C 0.0989(3) 0.3450(4) 0.7235(3) 0.0272(11) Uani 1 1 d . . .
C8 C 0.0414(3) 0.3458(4) 0.6310(3) 0.0264(11) Uani 1 1 d . . .
H8A H -0.0124 0.3458 0.6564 0.032 Uiso 1 1 calc R . .
H8B H 0.0493 0.4069 0.5887 0.032 Uiso 1 1 calc R . .
C9 C 0.0570(4) 0.2500 0.5658(5) 0.0300(16) Uani 1 2 d S . .
C10 C 0.1402(4) 0.2500 0.5246(4) 0.0246(15) Uani 1 2 d S . .
H10 H 0.1491 0.3104 0.4817 0.029 Uiso 1 1 d R . .
C11 C 0.1968(4) 0.2500 0.6182(5) 0.0242(15) Uani 1 2 d S . .
C12 C 0.1835(3) 0.3462(4) 0.6837(3) 0.0275(11) Uani 1 1 d . . .
H12A H 0.1926 0.4069 0.6412 0.033 Uiso 1 1 calc R . .
H12B H 0.2198 0.3475 0.7425 0.033 Uiso 1 1 calc R . .
C13 C 0.0858(4) 0.2500 0.7898(5) 0.0270(16) Uani 1 2 d S . .
H13A H 0.1220 0.2500 0.8487 0.032 Uiso 1 2 calc SR . .
H13B H 0.0325 0.2500 0.8173 0.032 Uiso 1 2 calc SR . .
O1W O 0.2541(14) 0.2500 0.2341(16) 0.090(6) Uani 0.50 2 d SP . .
O2W O 0.2036(16) 0.2500 0.2720(13) 0.098(7) Uani 0.50 2 d SP . .
O3W O -0.1643(16) 0.904(2) 0.8816(16) 0.146(8) Uani 0.55 1 d PU . .
O4W O -0.123(2) 0.983(2) 0.871(2) 0.169(11) Uani 0.45 1 d PU . .
O5 O 0.1365(7) -0.0282(7) 0.4940(6) 0.157(5) Uani 1 1 d D . .
Cl1 Cl 0.1648(5) -0.0263(6) 0.3902(6) 0.106(3) Uani 0.70 1 d PD A 1
O2 O 0.1117(11) 0.0328(13) 0.3320(13) 0.256(15) Uani 0.70 1 d PD A 1
O4 O 0.1672(8) -0.1255(7) 0.3509(9) 0.104(5) Uani 0.70 1 d PDU A 1
O3 O 0.2390(8) 0.0185(13) 0.3870(14) 0.164(8) Uani 0.70 1 d PDU A 1
Cl2 Cl 0.1831(8) -0.0375(11) 0.4064(7) 0.069(4) Uani 0.30 1 d PD A 2
O2A O 0.2357(16) -0.113(2) 0.440(2) 0.18(2) Uani 0.30 1 d PD A 2
O3A O 0.2225(18) 0.0534(17) 0.384(2) 0.152(15) Uani 0.30 1 d PDU A 2
O4A O 0.1412(14) -0.071(3) 0.3200(11) 0.123(14) Uani 0.30 1 d PDU A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0266(5) 0.0328(6) 0.0272(4) 0.000 -0.0037(3) 0.000
O1 0.034(4) 0.135(9) 0.077(5) 0.000 0.004(3) 0.000
N1 0.041(3) 0.032(3) 0.0324(18) -0.0008(18) 0.0022(17) -0.003(2)
N2 0.131(7) 0.049(4) 0.040(2) -0.008(2) 0.037(3) -0.023(4)
N3 0.034(3) 0.029(3) 0.0266(17) -0.0035(16) 0.0058(15) -0.007(2)
N4 0.039(4) 0.045(5) 0.029(3) 0.000 -0.009(2) 0.000
N5 0.039(5) 0.073(7) 0.043(3) 0.000 -0.001(3) 0.000
N6 0.025(3) 0.031(4) 0.033(3) 0.000 -0.003(2) 0.000
N7 0.030(3) 0.036(4) 0.025(2) 0.000 0.004(2) 0.000
N8 0.022(3) 0.082(7) 0.034(3) 0.000 -0.001(2) 0.000
N9 0.022(3) 0.028(4) 0.033(3) 0.000 0.002(2) 0.000
C1 0.039(3) 0.031(4) 0.028(2) -0.001(2) 0.0036(18) -0.004(2)
C2 0.119(8) 0.041(5) 0.044(3) -0.010(3) 0.035(4) -0.022(5)
C3 0.039(5) 0.038(5) 0.031(3) 0.000 -0.002(3) 0.000
C4 0.037(5) 0.098(9) 0.029(3) 0.000 0.000(3) 0.000
C5 0.031(4) 0.064(7) 0.030(3) 0.000 -0.001(3) 0.000
C6 0.027(4) 0.080(8) 0.029(3) 0.000 -0.001(3) 0.000
C7 0.022(2) 0.033(3) 0.027(2) -0.0043(18) 0.0015(16) -0.001(2)
C8 0.024(2) 0.027(3) 0.0286(19) -0.0010(17) -0.0004(16) 0.002(2)
C9 0.024(4) 0.038(5) 0.028(3) 0.000 -0.005(2) 0.000
C10 0.023(4) 0.025(4) 0.026(3) 0.000 0.000(2) 0.000
C11 0.017(3) 0.027(4) 0.029(3) 0.000 -0.001(2) 0.000
C12 0.025(3) 0.032(3) 0.0251(19) -0.0035(17) 0.0011(15) -0.006(2)
C13 0.022(4) 0.033(5) 0.026(3) 0.000 0.003(2) 0.000
O1W 0.074(15) 0.114(19) 0.082(12) 0.000 0.000(10) 0.000
O2W 0.091(17) 0.15(2) 0.056(9) 0.000 -0.003(9) 0.000
O3W 0.15(2) 0.125(19) 0.160(14) -0.037(13) -0.033(13) 0.037(15)
O4W 0.25(3) 0.12(2) 0.143(15) 0.008(15) -0.080(18) 0.00(2)
O5 0.206(13) 0.128(9) 0.138(7) -0.068(6) 0.084(8) 0.007(8)
Cl1 0.078(4) 0.071(4) 0.168(7) -0.048(4) 0.025(3) -0.020(3)
O2 0.27(4) 0.096(17) 0.41(4) 0.046(19) -0.10(3) 0.002(19)
O4 0.106(10) 0.073(9) 0.135(8) -0.067(7) 0.082(8) -0.027(7)
O3 0.105(12) 0.081(13) 0.304(18) -0.073(12) 0.058(12) -0.042(11)
Cl2 0.083(8) 0.082(9) 0.041(3) -0.018(3) 0.028(4) -0.035(6)
O2A 0.14(3) 0.30(6) 0.101(19) 0.09(3) -0.01(2) -0.06(4)
O3A 0.15(3) 0.06(2) 0.25(3) -0.040(19) 0.12(2) -0.05(2)
O4A 0.08(2) 0.11(3) 0.17(2) -0.10(2) 0.017(16) -0.06(2)

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

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 N7 1.996(5) 2_565 ?
Cu1 N4 1.997(5) 5_566 ?
Cu1 N1 2.014(5) . ?
Cu1 N1 2.014(5) 8_575 ?
Cu1 O1 2.202(8) . ?
O1 H1W 0.8498 . ?
N1 C1 1.307(7) . ?
N1 N2 1.348(7) . ?
N2 C2 1.314(10) . ?
N3 C1 1.329(8) . ?
N3 C2 1.349(7) . ?
N3 C7 1.498(7) . ?
N4 C3 1.331(11) . ?
N4 N5 1.373(11) . ?
N4 Cu1 1.997(5) 5_566 ?
N5 C4 1.271(10) . ?
N6 C4 1.360(11) . ?
N6 C3 1.363(9) . ?
N6 C9 1.501(8) . ?
N7 C5 1.306(11) . ?
N7 N8 1.381(8) . ?
N7 Cu1 1.996(5) 2_564 ?
N8 C6 1.321(11) . ?
N9 C6 1.344(10) . ?
N9 C5 1.349(9) . ?
N9 C11 1.481(9) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 H3 0.9400 . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
C7 C13 1.530(6) . ?
C7 C12 1.540(7) . ?
C7 C8 1.545(6) . ?
C8 C9 1.538(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.523(10) . ?
C9 C8 1.538(6) 8_565 ?
C10 C11 1.547(8) . ?
C10 H10 0.9795 . ?
C11 C12 1.537(6) 8_565 ?
C11 C12 1.537(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 C7 1.530(6) 8_565 ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
O5 Cl2 1.389(8) . ?
O5 Cl1 1.421(7) . ?
Cl1 O4 1.400(7) . ?
Cl1 O3 1.404(8) . ?
Cl1 O2 1.413(8) . ?
Cl2 O4A 1.398(9) . ?
Cl2 O3A 1.405(9) . ?
Cl2 O2A 1.405(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
N7 Cu1 N4 162.1(3) 2_565 5_566 ?
N7 Cu1 N1 89.49(12) 2_565 . ?
N4 Cu1 N1 89.02(11) 5_566 . ?
N7 Cu1 N1 89.49(12) 2_565 8_575 ?
N4 Cu1 N1 89.02(11) 5_566 8_575 ?
N1 Cu1 N1 170.4(3) . 8_575 ?
N7 Cu1 O1 97.6(3) 2_565 . ?
N4 Cu1 O1 100.3(3) 5_566 . ?
N1 Cu1 O1 94.81(14) . . ?
N1 Cu1 O1 94.81(14) 8_575 . ?
Cu1 O1 H1W 121.4 . . ?
C1 N1 N2 107.4(5) . . ?
C1 N1 Cu1 132.5(4) . . ?
N2 N1 Cu1 119.7(4) . . ?
C2 N2 N1 106.7(5) . . ?
C1 N3 C2 104.5(5) . . ?
C1 N3 C7 126.8(4) . . ?
C2 N3 C7 128.7(5) . . ?
C3 N4 N5 108.4(6) . . ?
C3 N4 Cu1 133.6(6) . 5_566 ?
N5 N4 Cu1 118.0(5) . 5_566 ?
C4 N5 N4 105.9(8) . . ?
C4 N6 C3 103.9(6) . . ?
C4 N6 C9 128.7(6) . . ?
C3 N6 C9 127.4(7) . . ?
C5 N7 N8 107.6(5) . . ?
C5 N7 Cu1 122.2(5) . 2_564 ?
N8 N7 Cu1 130.2(5) . 2_564 ?
C6 N8 N7 105.3(6) . . ?
C6 N9 C5 104.3(6) . . ?
C6 N9 C11 127.2(6) . . ?
C5 N9 C11 128.5(6) . . ?
N1 C1 N3 111.0(4) . . ?
N1 C1 H1 124.5 . . ?
N3 C1 H1 124.5 . . ?
N2 C2 N3 110.4(6) . . ?
N2 C2 H2 124.8 . . ?
N3 C2 H2 124.8 . . ?
N4 C3 N6 108.5(7) . . ?
N4 C3 H3 125.8 . . ?
N6 C3 H3 125.8 . . ?
N5 C4 N6 113.3(7) . . ?
N5 C4 H4 123.4 . . ?
N6 C4 H4 123.4 . . ?
N7 C5 N9 110.9(6) . . ?
N7 C5 H5 124.5 . . ?
N9 C5 H5 124.5 . . ?
N8 C6 N9 111.9(6) . . ?
N8 C6 H6 124.1 . . ?
N9 C6 H6 124.1 . . ?
N3 C7 C13 110.0(3) . . ?
N3 C7 C12 109.1(4) . . ?
C13 C7 C12 109.4(5) . . ?
N3 C7 C8 108.0(4) . . ?
C13 C7 C8 110.0(5) . . ?
C12 C7 C8 110.2(3) . . ?
C9 C8 C7 107.6(5) . . ?
C9 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
C9 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N6 C9 C10 108.3(5) . . ?
N6 C9 C8 108.5(4) . 8_565 ?
C10 C9 C8 110.6(4) . 8_565 ?
N6 C9 C8 108.5(4) . . ?
C10 C9 C8 110.6(4) . . ?
C8 C9 C8 110.2(5) 8_565 . ?
C9 C10 C11 108.6(5) . . ?
C9 C10 H10 110.0 . . ?
C11 C10 H10 109.9 . . ?
N9 C11 C12 109.4(4) . 8_565 ?
N9 C11 C12 109.4(4) . . ?
C12 C11 C12 110.9(5) 8_565 . ?
N9 C11 C10 108.1(5) . . ?
C12 C11 C10 109.5(4) 8_565 . ?
C12 C11 C10 109.5(4) . . ?
C11 C12 C7 108.3(4) . . ?
C11 C12 H12A 110.0 . . ?
C7 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C7 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C7 C13 C7 109.5(5) 8_565 . ?
C7 C13 H13A 109.8 8_565 . ?
C7 C13 H13A 109.8 . . ?
C7 C13 H13B 109.8 8_565 . ?
C7 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
O4 Cl1 O3 110.7(7) . . ?
O4 Cl1 O2 109.9(7) . . ?
O3 Cl1 O2 109.8(8) . . ?
O4 Cl1 O5 109.5(6) . . ?
O3 Cl1 O5 110.2(7) . . ?
O2 Cl1 O5 106.6(8) . . ?
O5 Cl2 O4A 112.1(9) . . ?
O5 Cl2 O3A 111.8(9) . . ?
O4A Cl2 O3A 110.8(8) . . ?
O5 Cl2 O2A 100.5(14) . . ?
O4A Cl2 O2A 110.6(9) . . ?
O3A Cl2 O2A 110.7(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N7 Cu1 N1 C1 -136.5(6) 2_565 . . . ?
N4 Cu1 N1 C1 25.7(6) 5_566 . . . ?
O1 Cu1 N1 C1 125.9(6) . . . . ?
N7 Cu1 N1 N2 52.4(6) 2_565 . . . ?
N4 Cu1 N1 N2 -145.5(6) 5_566 . . . ?
O1 Cu1 N1 N2 -45.3(6) . . . . ?
C1 N1 N2 C2 1.2(9) . . . . ?
Cu1 N1 N2 C2 174.4(6) . . . . ?
N2 N1 C1 N3 -2.1(7) . . . . ?
Cu1 N1 C1 N3 -174.1(4) . . . . ?
C2 N3 C1 N1 2.1(7) . . . . ?
C7 N3 C1 N1 179.6(5) . . . . ?
N1 N2 C2 N3 0.1(11) . . . . ?
C1 N3 C2 N2 -1.3(10) . . . . ?
C7 N3 C2 N2 -178.8(7) . . . . ?
C1 N3 C7 C13 177.2(5) . . . . ?
C2 N3 C7 C13 -5.9(9) . . . . ?
C1 N3 C7 C12 57.2(6) . . . . ?
C2 N3 C7 C12 -126.0(7) . . . . ?
C1 N3 C7 C8 -62.7(7) . . . . ?
C2 N3 C7 C8 114.2(7) . . . . ?
N3 C7 C8 C9 179.6(4) . . . . ?
C13 C7 C8 C9 -60.3(5) . . . . ?
C12 C7 C8 C9 60.4(6) . . . . ?
C4 N6 C9 C8 59.9(4) . . . 8_565 ?
C3 N6 C9 C8 -120.1(4) . . . 8_565 ?
C4 N6 C9 C8 -59.9(4) . . . . ?
C3 N6 C9 C8 120.1(4) . . . . ?
C7 C8 C9 N6 -179.2(4) . . . . ?
C7 C8 C9 C10 -60.6(5) . . . . ?
C7 C8 C9 C8 62.1(7) . . . 8_565 ?
N6 C9 C10 C11 180.0 . . . . ?
C8 C9 C10 C11 -61.2(4) 8_565 . . . ?
C8 C9 C10 C11 61.2(4) . . . . ?
C6 N9 C11 C12 -60.8(3) . . . 8_565 ?
C5 N9 C11 C12 119.2(3) . . . 8_565 ?
C6 N9 C11 C12 60.8(3) . . . . ?
C5 N9 C11 C12 -119.2(3) . . . . ?
C9 C10 C11 C12 60.8(4) . . . 8_565 ?
C9 C10 C11 C12 -60.8(4) . . . . ?
N9 C11 C12 C7 179.0(4) . . . . ?
C12 C11 C12 C7 -60.1(6) 8_565 . . . ?
C10 C11 C12 C7 60.7(5) . . . . ?
N3 C7 C12 C11 -179.7(4) . . . . ?
C13 C7 C12 C11 59.9(5) . . . . ?
C8 C7 C12 C11 -61.2(5) . . . . ?
N3 C7 C13 C7 178.8(3) . . . 8_565 ?
C12 C7 C13 C7 -61.3(6) . . . 8_565 ?
C8 C7 C13 C7 59.9(7) . . . 8_565 ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.103

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL ip1123 in Pnma
CELL 0.71073 17.1623 13.1560 12.8631 90.000 90.000 90.000
ZERR 4.00 0.0013 0.0008 0.0008 0.000 0.000 0.000
LATT 1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM 1/2 + X, 1/2 - Y, 1/2 - Z
SYMM - X, 1/2 + Y, - Z
SFAC C H N O CL CU
UNIT 72 112 48 48 8 4
MERG 2
OMIT 0.00 180.00
OMIT 1 7 6
OMIT 0 8 8
OMIT 3 8 6
OMIT 0 12 8
OMIT 4 5 8
OMIT 3 6 6
OMIT 7 8 5
SHEL 0.8 3
DFIX 1.415 0.01 Cl1 O2 Cl1 O3 Cl1 O4 Cl1 O5
DFIX 2.303 0.01 O2 O3 O2 O4 O2 O5 O3 O4 O3 O5 O4 O5
DFIX 1.415 0.01 Cl2 O4a Cl2 O3a Cl2 O5 Cl2 O2a
DFIX 2.303 0.01 O4a O3a O4a O5 O3a O5 O2a O3a O2a O4a
SIMU 0.02 O3 O3A
SIMU 0.02 O4 O4A
SIMU 0.02 O3W O4W
FMAP 2
PLAN 15
SIZE 0.18 0.23 0.26
ACTA
BOND $H
CONF
LIST 4
L.S. 6
TEMP -60.00
WGHT 0.115100 2.328900
FVAR 1.00733
CU1 6 0.066158 0.750000 0.836150 10.50000 0.02662 0.03278 =
0.02718 0.00000 -0.00368 0.00000
O1 4 -0.053341 0.750000 0.898516 10.50000 0.03426 0.13469 =
0.07678 0.00000 0.00356 0.00000
AFIX 3
H1W 2 -0.082241 0.802300 0.894396 11.00000 -1.50000
AFIX 0
N1 3 0.075231 0.597467 0.831041 11.00000 0.04102 0.03171 =
0.03243 -0.00079 0.00220 -0.00347
N2 3 0.051324 0.541514 0.912855 11.00000 0.13054 0.04893 =
0.04017 -0.00826 0.03693 -0.02267
N3 3 0.084528 0.438536 0.786990 11.00000 0.03361 0.02940 =
0.02657 -0.00348 0.00580 -0.00670
N4 3 -0.043782 0.250000 0.316182 10.50000 0.03882 0.04540 =
0.02876 0.00000 -0.00887 0.00000
N5 3 -0.105904 0.250000 0.383457 10.50000 0.03867 0.07344 =
0.04339 0.00000 -0.00125 0.00000
N6 3 0.002439 0.250000 0.474575 10.50000 0.02485 0.03070 =
0.03309 0.00000 -0.00324 0.00000
N7 3 0.377437 0.250000 0.471876 10.50000 0.02986 0.03642 =
0.02525 0.00000 0.00358 0.00000
N8 3 0.406061 0.250000 0.572249 10.50000 0.02167 0.08245 =
0.03359 0.00000 -0.00058 0.00000
N9 3 0.277468 0.250000 0.577368 10.50000 0.02159 0.02841 =
0.03314 0.00000 0.00159 0.00000
C1 1 0.093192 0.534358 0.756327 11.00000 0.03930 0.03129 =
0.02756 -0.00074 0.00358 -0.00435
AFIX 43
H1 2 0.110000 0.554098 0.689771 11.00000 -1.20000
AFIX 0
C2 1 0.057181 0.445755 0.885031 11.00000 0.11933 0.04065 =
0.04442 -0.00958 0.03464 -0.02238
AFIX 43
H2 2 0.044155 0.390111 0.927450 11.00000 -1.20000
AFIX 0
C3 1 0.021650 0.250000 0.371793 10.50000 0.03946 0.03832 =
0.03135 0.00000 -0.00217 0.00000
AFIX 43
H3 2 0.072522 0.250000 0.344714 10.50000 -1.20000
AFIX 0
C4 1 -0.076819 0.250000 0.474315 10.50000 0.03683 0.09755 =
0.02900 0.00000 -0.00028 0.00000
AFIX 43
H4 2 -0.107054 0.250000 0.535249 10.50000 -1.20000
AFIX 0
C5 1 0.301433 0.250000 0.477521 10.50000 0.03093 0.06381 =
0.03030 0.00000 -0.00112 0.00000
AFIX 43
H5 2 0.267927 0.250000 0.419712 10.50000 -1.20000
AFIX 0
C6 1 0.343866 0.250000 0.632757 10.50000 0.02680 0.08000 =
0.02919 0.00000 -0.00091 0.00000
AFIX 43
H6 2 0.345818 0.250000 0.705788 10.50000 -1.20000
AFIX 0
C7 1 0.098874 0.345004 0.723454 11.00000 0.02223 0.03262 =
0.02668 -0.00426 0.00154 -0.00070
C8 1 0.041414 0.345848 0.630998 11.00000 0.02358 0.02697 =
0.02865 -0.00102 -0.00037 0.00225
AFIX 23
H8A 2 -0.012418 0.345770 0.656407 11.00000 -1.20000
H8B 2 0.049337 0.406916 0.588670 11.00000 -1.20000
AFIX 0
C9 1 0.056999 0.250000 0.565784 10.50000 0.02441 0.03761 =
0.02793 0.00000 -0.00457 0.00000
C10 1 0.140200 0.250000 0.524637 10.50000 0.02251 0.02504 =
0.02613 0.00000 -0.00008 0.00000
AFIX 3
H10 2 0.149070 0.310400 0.481717 11.00000 -1.20000
AFIX 0
C11 1 0.196803 0.250000 0.618222 10.50000 0.01694 0.02655 =
0.02902 0.00000 -0.00074 0.00000
C12 1 0.183523 0.346207 0.683655 11.00000 0.02505 0.03244 =
0.02510 -0.00345 0.00106 -0.00595
AFIX 23
H12A 2 0.192558 0.406932 0.641209 11.00000 -1.20000
H12B 2 0.219801 0.347490 0.742476 11.00000 -1.20000
AFIX 0
C13 1 0.085796 0.250000 0.789806 10.50000 0.02237 0.03294 =
0.02580 0.00000 0.00250 0.00000
AFIX 23
H13A 2 0.122024 0.250000 0.848696 10.50000 -1.20000
H13B 2 0.032542 0.250000 0.817299 10.50000 -1.20000
AFIX 0
O1W 4 0.254064 0.250000 0.234098 10.25000 0.07417 0.11352 =
0.08219 0.00000 -0.00007 0.00000
O2W 4 0.203560 0.250000 0.271984 10.25000 0.09127 0.14574 =
0.05569 0.00000 -0.00283 0.00000
O3W 4 -0.164331 0.903599 0.881616 10.55000 0.15377 0.12477 =
0.16035 -0.03701 -0.03300 0.03672
O4W 4 -0.123433 0.983199 0.871322 10.45000 0.24644 0.11592 =
0.14341 0.00754 -0.08020 0.00163
O5 4 0.136461 -0.028228 0.494029 11.00000 0.20587 0.12835 =
0.13764 -0.06770 0.08359 0.00736
PART 1
CL1 5 0.164813 -0.026330 0.390227 10.70000 0.07769 0.07086 =
0.16840 -0.04820 0.02495 -0.01977
O2 4 0.111667 0.032827 0.332039 10.70000 0.26711 0.09645 =
0.40588 0.04580 -0.10192 0.00192
O4 4 0.167236 -0.125499 0.350857 10.70000 0.10599 0.07257 =
0.13462 -0.06749 0.08225 -0.02657
O3 4 0.238983 0.018534 0.387017 10.70000 0.10510 0.08148 =
0.30420 -0.07288 0.05817 -0.04159
PART 2
CL2 5 0.183146 -0.037537 0.406381 10.30000 0.08346 0.08202 =
0.04088 -0.01804 0.02826 -0.03463
O2A 4 0.235658 -0.112574 0.439947 10.30000 0.14092 0.29660 =
0.10068 0.08576 -0.00691 -0.06141
O3A 4 0.222519 0.053418 0.383748 10.30000 0.14839 0.06011 =
0.24815 -0.03992 0.11656 -0.05376
O4A 4 0.141157 -0.071394 0.319972 10.30000 0.08471 0.11392 =
0.16933 -0.09593 0.01710 -0.06116
HKLF 4

REM ip1123 in Pnma
REM R1 = 0.0802 for 1910 Fo > 4sig(Fo) and 0.1106 for all 3041 data
REM 280 parameters refined using 37 restraints

END

WGHT 0.1152 2.3313
REM Highest difference peak 0.722, deepest hole -0.836, 1-sigma level 0.103
Q1 1 0.1027 0.7998 0.8417 11.00000 0.05 0.72
Q2 1 0.0630 0.8185 0.7671 11.00000 0.05 0.71
Q3 1 0.0630 0.8227 0.9154 11.00000 0.05 0.65
Q4 1 -0.0725 0.2011 0.5218 11.00000 0.05 0.62
Q5 1 0.0304 0.8022 0.8417 11.00000 0.05 0.60
Q6 1 0.0970 0.0158 0.4096 11.00000 0.05 0.60
Q7 1 -0.0673 0.2500 0.5871 10.50000 0.05 0.52
Q8 1 0.2225 0.2500 0.3647 10.50000 0.05 0.42
Q9 1 0.1619 -0.0906 0.3183 11.00000 0.05 0.38
Q10 1 0.2911 -0.2500 0.4821 10.50000 0.05 0.38

;

#---------------------------------------------------------

data_(13)
_database_code_depnum_ccdc_archive 'CCDC 867236'
#TrackingRef '- Adamantane_CIF.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis-[1,3,5,7-tetra(1,2,4-triazol-4-yl)adamantane]-hexachloro-
tricadmium(II) Nonahydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H40 Cd3 Cl6 N24, 9(H2 O)'
_chemical_formula_sum            'C36 H58 Cd3 Cl6 N24 O9'
_chemical_formula_weight         1520.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n m'
_space_group_name_Hall           '-P 2 2n'
_symmetry_Int_Tables_number      58

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

_cell_length_a                   28.2333(5)
_cell_length_b                   8.7809(2)
_cell_length_c                   11.3833(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2822.08(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    18819
_cell_measurement_theta_min      5.12
_cell_measurement_theta_max      26.34

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7771
_exptl_absorpt_correction_T_max  0.8911
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18819
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         5.12
_diffrn_reflns_theta_max         26.34
_reflns_number_total             2973
_reflns_number_gt                2606
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'

#------------------------------- Refinement data-----------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Refinement of the Cd-organic framework atoms was standard.
The CH-hydrogen atoms were constrained with U(iso) = 1.2U(eq) of the
parent C-atom and with C-H distances 0.95 A (triazole), 0.99 A
(CH2 adamantane). Very high anisotropy for thermal motion of the
coordinated Cl-ligands led us to refinement of two-component disordering
model, with equal 0.5 contributions of two closely separated chlorine
atoms (Cl1...Cl1 0.715 A; Cl2...Cl2 0.707 A). Actually the same problem
was connected with ring atoms of the non-coordinated triazole group
(N8-C5-N7-N7a-C5a). In this case we were not able to resolve the
possible disordering scheme. Corresponding atoms were refined
anisotropically without restraints in the geometry. The solvate water
molecules are also disordered (some of them are in special positions);
they were refined with partial occupancy factors 0.5 and left isotropic.
No H-atoms were added to these solvate water molecules.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+19.5694P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2973
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.11742(2) 0.22730(7) 0.0000 0.03520(19) Uani 1 2 d S . .
Cd2 Cd 0.0000 0.0000 0.0000 0.0282(2) Uani 1 4 d S . .
Cl1 Cl 0.02695(10) 0.2830(3) 0.0314(3) 0.0497(12) Uani 0.50 1 d P . .
Cl2A Cl 0.1486(4) 0.403(2) 0.1696(12) 0.120(4) Uani 0.50 1 d P . .
Cl2B Cl 0.1267(4) 0.4252(18) 0.1444(12) 0.114(3) Uani 0.50 1 d P . .
N1 N 0.1950(2) 0.1416(7) 0.0000 0.0338(15) Uani 1 2 d S . .
N2 N 0.2038(3) -0.0093(10) 0.0000 0.069(3) Uani 1 2 d S . .
N3 N 0.2712(2) 0.1144(8) 0.0000 0.0310(14) Uani 1 2 d S . .
N4 N 0.39996(15) 0.5369(6) 0.3571(4) 0.0352(11) Uani 1 1 d . . .
N5 N 0.44239(17) 0.4636(8) 0.3580(5) 0.0590(18) Uani 1 1 d . . .
N6 N 0.40066(14) 0.3697(6) 0.2145(4) 0.0304(10) Uani 1 1 d . . .
N7 N 0.4674(2) -0.3079(7) 0.0612(8) 0.087(3) Uani 1 1 d . . .
N8 N 0.4303(2) -0.1038(8) 0.0000 0.0413(18) Uani 1 2 d S . .
C1 C 0.2350(3) 0.2111(10) 0.0000 0.0362(18) Uani 1 2 d S . .
H1 H 0.2383 0.3188 0.0000 0.043 Uiso 1 2 calc SR . .
C2 C 0.2503(3) -0.0229(13) 0.0000 0.076(4) Uani 1 2 d S . .
H2 H 0.2669 -0.1171 0.0000 0.091 Uiso 1 2 calc SR . .
C3 C 0.37620(19) 0.4776(7) 0.2693(5) 0.0393(14) Uani 1 1 d . . .
H3 H 0.3451 0.5082 0.2476 0.047 Uiso 1 1 calc R . .
C4 C 0.4422(2) 0.3652(11) 0.2735(7) 0.074(3) Uani 1 1 d . . .
H4 H 0.4678 0.2989 0.2553 0.089 Uiso 1 1 calc R . .
C5 C 0.4447(3) -0.1872(8) 0.0930(9) 0.071(2) Uani 1 1 d . . .
H5 H 0.4388 -0.1603 0.1725 0.086 Uiso 1 1 calc R . .
C6 C 0.3227(2) 0.1514(9) 0.0000 0.0277(15) Uani 1 2 d S . .
C7 C 0.33464(16) 0.2433(6) 0.1111(4) 0.0267(11) Uani 1 1 d . . .
H7A H 0.3269 0.1830 0.1821 0.032 Uiso 1 1 calc R . .
H7B H 0.3159 0.3385 0.1130 0.032 Uiso 1 1 calc R . .
C8 C 0.38804(16) 0.2808(6) 0.1089(4) 0.0257(10) Uani 1 1 d . . .
C9 C 0.41592(17) 0.1319(6) 0.1092(5) 0.0294(11) Uani 1 1 d . . .
H9A H 0.4503 0.1538 0.1097 0.035 Uiso 1 1 calc R . .
H9B H 0.4082 0.0725 0.1806 0.035 Uiso 1 1 calc R . .
C10 C 0.4032(2) 0.0400(9) 0.0000 0.0294(16) Uani 1 2 d S . .
C11 C 0.3503(3) 0.0003(9) 0.0000 0.0341(17) Uani 1 2 d S . .
H11A H 0.3423 -0.0604 0.0705 0.041 Uiso 1 1 d R . .
C12 C 0.4002(2) 0.3762(9) 0.0000 0.0262(15) Uani 1 2 d S . .
H12A H 0.3816 0.4718 0.0000 0.031 Uiso 1 2 calc SR . .
H12B H 0.4343 0.4025 0.0000 0.031 Uiso 1 2 calc SR . .
O1 O 0.2130(4) 0.5162(15) 0.0000 0.046(3) Uiso 0.50 2 d SP . .
O2A O 0.2830(3) 0.6106(11) 0.0771(9) 0.055(2) Uiso 0.50 1 d P . .
O2B O 0.2661(5) 0.6150(15) 0.1636(12) 0.085(4) Uiso 0.50 1 d P . .
O3 O 0.5000 0.0000 0.3019(14) 0.063(4) Uiso 0.50 2 d SP . .
O4 O 0.2207(6) 0.403(2) 0.2486(15) 0.116(5) Uiso 0.50 1 d P . .
O6 O 0.1485(11) 0.712(3) 0.0000 0.141(9) Uiso 0.50 2 d SP . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0261(3) 0.0380(3) 0.0414(3) 0.000 0.000 -0.0026(2)
Cd2 0.0171(3) 0.0466(5) 0.0210(4) 0.000 0.000 0.0016(3)
Cl1 0.0326(13) 0.0399(14) 0.077(4) -0.0014(14) -0.0025(13) 0.0082(11)
Cl2A 0.118(8) 0.148(9) 0.093(6) -0.052(6) 0.016(6) -0.044(8)
Cl2B 0.119(8) 0.115(6) 0.107(7) -0.060(5) 0.019(6) -0.015(7)
N1 0.025(3) 0.028(3) 0.049(4) 0.000 0.000 -0.002(3)
N2 0.029(4) 0.046(5) 0.131(9) 0.000 0.000 -0.007(4)
N3 0.021(3) 0.033(3) 0.038(4) 0.000 0.000 -0.005(3)
N4 0.023(2) 0.050(3) 0.032(2) -0.010(2) -0.0033(18) 0.006(2)
N5 0.028(3) 0.108(5) 0.041(3) -0.037(3) -0.015(2) 0.019(3)
N6 0.022(2) 0.048(3) 0.022(2) -0.004(2) -0.0024(17) 0.0015(19)
N7 0.060(4) 0.043(3) 0.157(8) -0.002(4) -0.031(4) 0.008(3)
N8 0.027(3) 0.027(4) 0.070(5) 0.000 0.000 0.003(3)
C1 0.024(4) 0.039(4) 0.045(5) 0.000 0.000 0.004(3)
C2 0.023(4) 0.052(6) 0.154(13) 0.000 0.000 -0.001(4)
C3 0.025(3) 0.047(3) 0.046(3) -0.011(3) -0.011(2) 0.011(2)
C4 0.032(3) 0.132(8) 0.058(4) -0.060(5) -0.019(3) 0.029(4)
C5 0.072(5) 0.042(4) 0.101(7) 0.002(4) -0.029(5) 0.015(4)
C6 0.017(3) 0.034(4) 0.031(4) 0.000 0.000 -0.007(3)
C7 0.018(2) 0.036(3) 0.026(2) 0.001(2) 0.0023(19) 0.000(2)
C8 0.020(2) 0.037(3) 0.020(2) 0.000(2) -0.0027(18) -0.002(2)
C9 0.020(2) 0.036(3) 0.032(3) 0.007(2) -0.002(2) 0.000(2)
C10 0.020(3) 0.025(4) 0.043(4) 0.000 0.000 0.001(3)
C11 0.026(4) 0.031(4) 0.045(4) 0.000 0.000 -0.002(3)
C12 0.020(3) 0.034(4) 0.025(3) 0.000 0.000 0.000(3)

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

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
Cd1 N1 2.317(6) . ?
Cd1 N4 2.384(5) 8_655 ?
Cd1 N4 2.384(5) 3_545 ?
Cd1 Cl2B 2.406(11) . ?
Cd1 Cl2B 2.406(11) 6 ?
Cd1 Cl2A 2.624(12) . ?
Cd1 Cl2A 2.624(12) 6 ?
Cd1 Cl1 2.625(3) 6 ?
Cd1 Cl1 2.625(3) . ?
Cd2 N5 2.315(5) 3_545 ?
Cd2 N5 2.315(5) 7_565 ?
Cd2 N5 2.315(5) 8_655 ?
Cd2 N5 2.315(5) 4_455 ?
Cd2 Cl1 2.623(3) 5 ?
Cd2 Cl1 2.623(3) 2 ?
Cd2 Cl1 2.623(3) . ?
Cd2 Cl1 2.623(3) 6 ?
N1 C1 1.283(10) . ?
N1 N2 1.348(11) . ?
N2 C2 1.320(12) . ?
N3 C1 1.328(10) . ?
N3 C2 1.341(12) . ?
N3 C6 1.490(9) . ?
N4 C3 1.311(7) . ?
N4 N5 1.360(6) . ?
N4 Cd1 2.384(5) 3 ?
N5 C4 1.293(8) . ?
N5 Cd2 2.315(5) 3 ?
N6 C3 1.328(7) . ?
N6 C4 1.353(7) . ?
N6 C8 1.477(6) . ?
N7 C5 1.290(10) . ?
N7 N7 1.393(17) 6 ?
N8 C5 1.350(9) 6 ?
N8 C5 1.350(9) . ?
N8 C10 1.477(10) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.538(6) . ?
C6 C7 1.538(6) 6 ?
C6 C11 1.539(11) . ?
C7 C8 1.543(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.527(7) . ?
C8 C12 1.535(7) . ?
C9 C10 1.525(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C9 1.525(7) 6 ?
C10 C11 1.534(10) . ?
C11 H11A 0.9900 . ?
C12 C8 1.535(7) 6 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N4 88.10(16) . 8_655 ?
N1 Cd1 N4 88.10(16) . 3_545 ?
N4 Cd1 N4 86.1(2) 8_655 3_545 ?
N1 Cd1 Cl2B 97.6(3) . . ?
N4 Cd1 Cl2B 174.3(3) 8_655 . ?
N4 Cd1 Cl2B 93.6(4) 3_545 . ?
N1 Cd1 Cl2B 97.6(3) . 6 ?
N4 Cd1 Cl2B 93.6(4) 8_655 6 ?
N4 Cd1 Cl2B 174.3(3) 3_545 6 ?
Cl2B Cd1 Cl2B 86.2(8) . 6 ?
N1 Cd1 Cl2A 82.8(3) . . ?
N4 Cd1 Cl2A 169.7(3) 8_655 . ?
N4 Cd1 Cl2A 88.8(4) 3_545 . ?
Cl2B Cd1 Cl2A 92.3(2) 6 . ?
N1 Cd1 Cl2A 82.8(3) . 6 ?
N4 Cd1 Cl2A 88.8(4) 8_655 6 ?
N4 Cd1 Cl2A 169.7(3) 3_545 6 ?
Cl2B Cd1 Cl2A 92.3(2) . 6 ?
Cl2A Cd1 Cl2A 94.7(8) . 6 ?
N1 Cd1 Cl1 168.74(14) . 6 ?
N4 Cd1 Cl1 80.64(13) 8_655 6 ?
N4 Cd1 Cl1 91.33(13) 3_545 6 ?
Cl2B Cd1 Cl1 93.7(3) . 6 ?
Cl2B Cd1 Cl1 83.0(3) 6 6 ?
Cl2A Cd1 Cl1 108.4(3) . 6 ?
Cl2A Cd1 Cl1 96.7(3) 6 6 ?
N1 Cd1 Cl1 168.74(14) . . ?
N4 Cd1 Cl1 91.33(13) 8_655 . ?
N4 Cd1 Cl1 80.64(13) 3_545 . ?
Cl2B Cd1 Cl1 83.0(3) . . ?
Cl2B Cd1 Cl1 93.7(3) 6 . ?
Cl2A Cd1 Cl1 96.7(3) . . ?
Cl2A Cd1 Cl1 108.4(3) 6 . ?
N5 Cd2 N5 180.0(2) 3_545 7_565 ?
N5 Cd2 N5 88.6(3) 3_545 8_655 ?
N5 Cd2 N5 91.4(3) 7_565 8_655 ?
N5 Cd2 N5 91.4(3) 3_545 4_455 ?
N5 Cd2 N5 88.6(3) 7_565 4_455 ?
N5 Cd2 N5 180.0(2) 8_655 4_455 ?
N5 Cd2 Cl1 99.69(19) 3_545 5 ?
N5 Cd2 Cl1 80.31(19) 7_565 5 ?
N5 Cd2 Cl1 88.74(18) 8_655 5 ?
N5 Cd2 Cl1 91.26(18) 4_455 5 ?
N5 Cd2 Cl1 88.74(18) 3_545 2 ?
N5 Cd2 Cl1 91.26(18) 7_565 2 ?
N5 Cd2 Cl1 99.69(19) 8_655 2 ?
N5 Cd2 Cl1 80.31(19) 4_455 2 ?
N5 Cd2 Cl1 80.31(19) 3_545 . ?
N5 Cd2 Cl1 99.69(19) 7_565 . ?
N5 Cd2 Cl1 91.26(18) 8_655 . ?
N5 Cd2 Cl1 88.74(18) 4_455 . ?
Cl1 Cd2 Cl1 180.00(13) 5 . ?
Cl1 Cd2 Cl1 164.33(15) 2 . ?
N5 Cd2 Cl1 91.26(18) 3_545 6 ?
N5 Cd2 Cl1 88.74(18) 7_565 6 ?
N5 Cd2 Cl1 80.31(19) 8_655 6 ?
N5 Cd2 Cl1 99.69(19) 4_455 6 ?
Cl1 Cd2 Cl1 164.33(15) 5 6 ?
Cl1 Cd2 Cl1 180.00(12) 2 6 ?
Cl1 Cd2 Cl1 15.67(15) . 6 ?
Cd2 Cl1 Cd1 95.00(9) . . ?
C1 N1 N2 107.9(7) . . ?
C1 N1 Cd1 132.6(6) . . ?
N2 N1 Cd1 119.5(5) . . ?
C2 N2 N1 105.7(8) . . ?
C1 N3 C2 103.8(7) . . ?
C1 N3 C6 127.6(7) . . ?
C2 N3 C6 128.6(7) . . ?
C3 N4 N5 105.6(5) . . ?
C3 N4 Cd1 133.9(4) . 3 ?
N5 N4 Cd1 120.5(3) . 3 ?
C4 N5 N4 107.9(5) . . ?
C4 N5 Cd2 127.9(4) . 3 ?
N4 N5 Cd2 124.0(4) . 3 ?
C3 N6 C4 103.8(5) . . ?
C3 N6 C8 129.3(4) . . ?
C4 N6 C8 126.7(5) . . ?
C5 N7 N7 106.3(6) . 6 ?
C5 N8 C5 103.3(9) 6 . ?
C5 N8 C10 128.3(5) 6 . ?
C5 N8 C10 128.3(5) . . ?
N1 C1 N3 111.8(8) . . ?
N1 C1 H1 124.1 . . ?
N3 C1 H1 124.1 . . ?
N2 C2 N3 110.8(9) . . ?
N2 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
N4 C3 N6 112.0(5) . . ?
N4 C3 H3 124.0 . . ?
N6 C3 H3 124.0 . . ?
N5 C4 N6 110.6(6) . . ?
N5 C4 H4 124.7 . . ?
N6 C4 H4 124.7 . . ?
N7 C5 N8 112.0(9) . . ?
N7 C5 H5 124.0 . . ?
N8 C5 H5 124.0 . . ?
N3 C6 C7 109.2(4) . . ?
N3 C6 C7 109.2(4) . 6 ?
C7 C6 C7 110.7(6) . 6 ?
N3 C6 C11 107.8(6) . . ?
C7 C6 C11 109.9(4) . . ?
C7 C6 C11 109.9(4) 6 . ?
C6 C7 C8 108.3(4) . . ?
C6 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N6 C8 C9 109.1(4) . . ?
N6 C8 C12 108.4(4) . . ?
C9 C8 C12 110.7(4) . . ?
N6 C8 C7 109.6(4) . . ?
C9 C8 C7 108.7(4) . . ?
C12 C8 C7 110.4(4) . . ?
C10 C9 C8 109.2(4) . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
N8 C10 C9 109.3(4) . . ?
N8 C10 C9 109.3(4) . 6 ?
C9 C10 C9 109.2(6) . 6 ?
N8 C10 C11 108.1(6) . . ?
C9 C10 C11 110.5(4) . . ?
C9 C10 C11 110.5(4) 6 . ?
C10 C11 C6 107.3(6) . . ?
C10 C11 H11A 110.1 . . ?
C6 C11 H11A 110.5 . . ?
C8 C12 C8 107.8(6) 6 . ?
C8 C12 H12A 110.2 6 . ?
C8 C12 H12A 110.2 . . ?
C8 C12 H12B 110.2 6 . ?
C8 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N5 Cd2 Cl1 Cd1 52.38(16) 3_545 . . . ?
N5 Cd2 Cl1 Cd1 -127.62(16) 7_565 . . . ?
N5 Cd2 Cl1 Cd1 -35.96(18) 8_655 . . . ?
N5 Cd2 Cl1 Cd1 144.04(18) 4_455 . . . ?
Cl1 Cd2 Cl1 Cd1 98.63(8) 2 . . . ?
Cl1 Cd2 Cl1 Cd1 -81.37(8) 6 . . . ?
N1 Cd1 Cl1 Cd2 -52.3(7) . . . . ?
N4 Cd1 Cl1 Cd2 34.68(15) 8_655 . . . ?
N4 Cd1 Cl1 Cd2 -51.14(14) 3_545 . . . ?
Cl2B Cd1 Cl1 Cd2 -146.0(4) . . . . ?
Cl2B Cd1 Cl1 Cd2 128.4(4) 6 . . . ?
Cl2A Cd1 Cl1 Cd2 -138.8(4) . . . . ?
Cl2A Cd1 Cl1 Cd2 123.9(4) 6 . . . ?
Cl1 Cd1 Cl1 Cd2 81.37(8) 6 . . . ?
N4 Cd1 N1 C1 136.93(12) 8_655 . . . ?
N4 Cd1 N1 C1 -136.93(12) 3_545 . . . ?
Cl2B Cd1 N1 C1 -43.6(4) . . . . ?
Cl2B Cd1 N1 C1 43.6(4) 6 . . . ?
Cl2A Cd1 N1 C1 -47.9(4) . . . . ?
Cl2A Cd1 N1 C1 47.9(4) 6 . . . ?
Cl1 Cd1 N1 C1 135.8(7) 6 . . . ?
Cl1 Cd1 N1 C1 -135.8(7) . . . . ?
N4 Cd1 N1 N2 -43.07(12) 8_655 . . . ?
N4 Cd1 N1 N2 43.07(12) 3_545 . . . ?
Cl2B Cd1 N1 N2 136.4(4) . . . . ?
Cl2B Cd1 N1 N2 -136.4(4) 6 . . . ?
Cl2A Cd1 N1 N2 132.1(4) . . . . ?
Cl2A Cd1 N1 N2 -132.1(4) 6 . . . ?
Cl1 Cd1 N1 N2 -44.2(7) 6 . . . ?
Cl1 Cd1 N1 N2 44.2(7) . . . . ?
C1 N1 N2 C2 0.0 . . . . ?
Cd1 N1 N2 C2 180.0 . . . . ?
C3 N4 N5 C4 -0.4(9) . . . . ?
Cd1 N4 N5 C4 178.8(6) 3 . . . ?
C3 N4 N5 Cd2 -175.2(5) . . . 3 ?
Cd1 N4 N5 Cd2 4.0(7) 3 . . 3 ?
N2 N1 C1 N3 0.0 . . . . ?
Cd1 N1 C1 N3 180.0 . . . . ?
C2 N3 C1 N1 0.0 . . . . ?
C6 N3 C1 N1 180.0 . . . . ?
N1 N2 C2 N3 0.0 . . . . ?
C1 N3 C2 N2 0.0 . . . . ?
C6 N3 C2 N2 180.0 . . . . ?
N5 N4 C3 N6 0.6(7) . . . . ?
Cd1 N4 C3 N6 -178.5(4) 3 . . . ?
C4 N6 C3 N4 -0.5(8) . . . . ?
C8 N6 C3 N4 -176.6(5) . . . . ?
N4 N5 C4 N6 0.1(10) . . . . ?
Cd2 N5 C4 N6 174.7(5) 3 . . . ?
C3 N6 C4 N5 0.2(10) . . . . ?
C8 N6 C4 N5 176.4(6) . . . . ?
N7 N7 C5 N8 -1.5(7) 6 . . . ?
C5 N8 C5 N7 2.3(12) 6 . . . ?
C10 N8 C5 N7 179.4(7) . . . . ?
C1 N3 C6 C7 60.6(4) . . . . ?
C2 N3 C6 C7 -119.4(4) . . . . ?
C1 N3 C6 C7 -60.6(4) . . . 6 ?
C2 N3 C6 C7 119.4(4) . . . 6 ?
C1 N3 C6 C11 180.0 . . . . ?
C2 N3 C6 C11 0.0 . . . . ?
N3 C6 C7 C8 -179.8(5) . . . . ?
C7 C6 C7 C8 -59.5(7) 6 . . . ?
C11 C6 C7 C8 62.1(6) . . . . ?
C3 N6 C8 C9 -156.7(6) . . . . ?
C4 N6 C8 C9 28.1(8) . . . . ?
C3 N6 C8 C12 82.7(7) . . . . ?
C4 N6 C8 C12 -92.6(8) . . . . ?
C3 N6 C8 C7 -37.8(7) . . . . ?
C4 N6 C8 C7 146.9(7) . . . . ?
C6 C7 C8 N6 179.8(4) . . . . ?
C6 C7 C8 C9 -61.1(5) . . . . ?
C6 C7 C8 C12 60.5(6) . . . . ?
N6 C8 C9 C10 -179.7(4) . . . . ?
C12 C8 C9 C10 -60.5(6) . . . . ?
C7 C8 C9 C10 60.8(5) . . . . ?
C5 N8 C10 C9 -151.5(7) 6 . . . ?
C5 N8 C10 C9 32.1(10) . . . . ?
C5 N8 C10 C9 -32.1(10) 6 . . 6 ?
C5 N8 C10 C9 151.5(7) . . . 6 ?
C5 N8 C10 C11 88.2(8) 6 . . . ?
C5 N8 C10 C11 -88.2(8) . . . . ?
C8 C9 C10 N8 179.8(4) . . . . ?
C8 C9 C10 C9 60.3(7) . . . 6 ?
C8 C9 C10 C11 -61.4(6) . . . . ?
N8 C10 C11 C6 180.0 . . . . ?
C9 C10 C11 C6 60.5(4) . . . . ?
C9 C10 C11 C6 -60.5(4) 6 . . . ?
N3 C6 C11 C10 180.0 . . . . ?
C7 C6 C11 C10 -61.0(4) . . . . ?
C7 C6 C11 C10 61.0(4) 6 . . . ?
N6 C8 C12 C8 178.6(3) . . . 6 ?
C9 C8 C12 C8 59.0(6) . . . 6 ?
C7 C8 C12 C8 -61.4(7) . . . 6 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        26.34
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.125

_iucr_refine_instruction_details 
;
#---------------------------------------------------------

TITL dk57 in Pnnm
CELL 0.71073 28.2333 8.7809 11.3833 90.000 90.000 90.000
ZERR 2.00 0.0005 0.0002 0.0002 0.000 0.000 0.000
LATT 1
SYMM - X, - Y, Z
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SYMM 1/2 + X, 1/2 - Y, 1/2 - Z
SFAC C H N O CL CD
UNIT 72 116 48 18 12 6
MERG 2
OMIT 0.00 180.00
OMIT 6 0 2
OMIT 27 1 9
OMIT 5 7 3
OMIT 0 3 1
OMIT 4 1 3
OMIT 4 2 0
OMIT 6 2 1
SHEL 0.80 4
FMAP 2
PLAN 20
SIZE 0.08 0.14 0.18
ACTA
BOND
BOND $H
CONF
LIST 4
L.S. 4
TEMP -100.00
WGHT 0.036000 19.569401
FVAR 0.24614
CD1 6 0.117424 0.227305 0.000000 10.50000 0.02614 0.03805 =
0.04141 0.00000 0.00000 -0.00257
CD2 6 0.000000 0.000000 0.000000 10.25000 0.01714 0.04656 =
0.02098 0.00000 0.00000 0.00157
CL1 5 0.026949 0.283008 0.031412 10.50000 0.03263 0.03986 =
0.07652 -0.00137 -0.00252 0.00822
CL2A 5 0.148559 0.403230 0.169589 10.50000 0.11819 0.14782 =
0.09297 -0.05194 0.01609 -0.04372
CL2B 5 0.126707 0.425205 0.144417 10.50000 0.11857 0.11533 =
0.10664 -0.05970 0.01945 -0.01546
N1 3 0.195029 0.141570 0.000000 10.50000 0.02521 0.02774 =
0.04858 0.00000 0.00000 -0.00184
N2 3 0.203787 -0.009328 0.000000 10.50000 0.02909 0.04624 =
0.13057 0.00000 0.00000 -0.00708
N3 3 0.271162 0.114361 0.000000 10.50000 0.02144 0.03306 =
0.03845 0.00000 0.00000 -0.00476
N4 3 0.399960 0.536917 0.357053 11.00000 0.02310 0.05000 =
0.03242 -0.00962 -0.00334 0.00636
N5 3 0.442393 0.463646 0.357964 11.00000 0.02830 0.10790 =
0.04076 -0.03689 -0.01493 0.01903
N6 3 0.400656 0.369739 0.214542 11.00000 0.02152 0.04777 =
0.02185 -0.00405 -0.00243 0.00149
N7 3 0.467355 -0.307859 0.061168 11.00000 0.05972 0.04259 =
0.15734 -0.00161 -0.03112 0.00842
N8 3 0.430322 -0.103788 0.000000 10.50000 0.02735 0.02696 =
0.06968 0.00000 0.00000 0.00259
C1 1 0.235000 0.211127 0.000000 10.50000 0.02423 0.03901 =
0.04542 0.00000 0.00000 0.00412
AFIX 43
H1 2 0.238326 0.318787 0.000000 10.50000 -1.20000
AFIX 0
C2 1 0.250349 -0.022896 0.000000 10.50000 0.02269 0.05191 =
0.15412 0.00000 0.00000 -0.00107
AFIX 43
H2 2 0.266875 -0.117138 0.000000 10.50000 -1.20000
AFIX 0
C3 1 0.376196 0.477639 0.269348 11.00000 0.02527 0.04666 =
0.04591 -0.01146 -0.01058 0.01066
AFIX 43
H3 2 0.345141 0.508243 0.247554 11.00000 -1.20000
AFIX 0
C4 1 0.442234 0.365246 0.273484 11.00000 0.03168 0.13217 =
0.05831 -0.06013 -0.01892 0.02855
AFIX 43
H4 2 0.467790 0.298933 0.255310 11.00000 -1.20000
AFIX 0
C5 1 0.444679 -0.187210 0.093004 11.00000 0.07155 0.04186 =
0.10067 0.00194 -0.02881 0.01525
AFIX 43
H5 2 0.438782 -0.160256 0.172493 11.00000 -1.20000
AFIX 0
C6 1 0.322665 0.151397 0.000000 10.50000 0.01743 0.03419 =
0.03137 0.00000 0.00000 -0.00650
C7 1 0.334644 0.243256 0.111123 11.00000 0.01769 0.03649 =
0.02580 0.00089 0.00230 -0.00018
AFIX 23
H7A 2 0.326920 0.183035 0.182107 11.00000 -1.20000
H7B 2 0.315871 0.338451 0.112988 11.00000 -1.20000
AFIX 0
C8 1 0.388039 0.280838 0.108900 11.00000 0.02025 0.03658 =
0.02039 -0.00033 -0.00269 -0.00223
C9 1 0.415925 0.131867 0.109197 11.00000 0.01957 0.03642 =
0.03227 0.00676 -0.00186 -0.00035
AFIX 23
H9A 2 0.450320 0.153794 0.109730 11.00000 -1.20000
H9B 2 0.408201 0.072522 0.180618 11.00000 -1.20000
AFIX 0
C10 1 0.403187 0.040042 0.000000 10.50000 0.01975 0.02512 =
0.04325 0.00000 0.00000 0.00130
C11 1 0.350267 0.000314 0.000000 10.50000 0.02593 0.03137 =
0.04510 0.00000 0.00000 -0.00238
AFIX 3
H11A 2 0.342299 -0.060437 0.070548 11.00000 -1.20000
AFIX 0
C12 1 0.400180 0.376154 0.000000 10.50000 0.01996 0.03369 =
0.02499 0.00000 0.00000 0.00037
AFIX 23
H12A 2 0.381620 0.471810 0.000000 10.50000 -1.20000
H12B 2 0.434277 0.402469 0.000000 10.50000 -1.20000
AFIX 0
O1 4 0.213015 0.516226 0.000000 10.25000 0.04610
O2A 4 0.283040 0.610647 0.077099 10.50000 0.05548
O2B 4 0.266097 0.615001 0.163580 10.50000 0.08548
O3 4 0.500000 0.000000 0.301933 10.25000 0.06314
O4 4 0.220650 0.403009 0.248559 10.50000 0.11561
O6 4 0.148472 0.712007 0.000000 10.25000 0.14092
HKLF 4

REM dk57 in Pnnm
REM R1 = 0.0556 for 2606 Fo > 4sig(Fo) and 0.0643 for all 2973 data
REM 208 parameters refined using 0 restraints

END

WGHT 0.0359 19.5975
REM Highest difference peak 1.380, deepest hole -1.335, 1-sigma level 0.125
Q1 1 0.1279 0.1487 0.0000 10.50000 0.05 1.38
Q2 1 0.2305 0.4595 0.0000 10.50000 0.05 1.35
Q3 1 0.2926 0.6034 0.0000 10.50000 0.05 1.05
Q4 1 0.1450 0.7185 0.0558 11.00000 0.05 1.01
Q5 1 0.2984 0.6162 0.0351 11.00000 0.05 0.97
Q6 1 0.2691 0.6005 0.1119 11.00000 0.05 0.96
Q7 1 0.1193 0.2724 0.0579 11.00000 0.05 0.70
Q8 1 0.0815 0.6437 0.0870 11.00000 0.05 0.68
Q9 1 0.2818 0.6565 0.2172 11.00000 0.05 0.57
Q10 1 0.2429 0.4595 0.2416 11.00000 0.05 0.56

;

# ------------- END of CIF -----------------#