Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_cu.cif
_database_code_CSD                  156828

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communicatirons'

loop_
_publ_author_name
'Chan, Albert S. C.'
'Kang, Bei-Sheng'
'Liao, Sen'
'Liu, Jun'
'Liu, Hong-Ke'
'Tan, Hai-Yan'
'Yu, Xiao-Lan'
'Zhang, Hua-Xin'
'Zhou, Zhong-Yuan'

_publ_contact_author_name     	'Dr Hong-Ke Liu'  
_publ_contact_author_address 
;
Dr Hong-Ke Liu
School of Chemistry and Chemical Engineering
Zhongshan University
Guangzhou
510275
CHINA
;

_publ_contact_author_email       'hongke_liu@hotmail.com'

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common      {Cu6(tib)8(OH)4](OH)8.4CH3OH.22H2O
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C37 H54 Cu1.50 N12 O9.50'
_chemical_formula_weight          914.23

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'
'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    P2(1)/c

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                    13.662(2)
_cell_length_b                    23.197(4)
_cell_length_c                    18.914(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  110.074(3)
_cell_angle_gamma                 90.00
_cell_volume                      5630.1(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     859
_cell_measurement_theta_min       4.15
_cell_measurement_theta_max       21.91

_exptl_crystal_description        plate
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.079
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1918
_exptl_absorpt_coefficient_mu     0.623
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   0.9123
_exptl_absorpt_correction_T_max   0.9755
_exptl_absorpt_process_details    'SADABS'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(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   'CCD area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             27562
_diffrn_reflns_av_R_equivalents   0.0702
_diffrn_reflns_av_sigmaI/netI     0.0967
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.83
_diffrn_reflns_theta_max          24.71
_reflns_number_total              9552
_reflns_number_gt                 4316
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SHELXTL'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'

_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.
;

_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^)+(0.2000P)^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      SHELXL
_refine_ls_extinction_coef        0.0007(9)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          9552
_refine_ls_number_parameters      596
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1670
_refine_ls_R_factor_gt            0.0920
_refine_ls_wR_factor_ref          0.3207
_refine_ls_wR_factor_gt           0.2710
_refine_ls_goodness_of_fit_ref    0.961
_refine_ls_restrained_S_all       0.961
_refine_ls_shift/su_max           0.076
_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
Cu1 Cu 0.37282(6) 0.21187(5) 0.99364(5) 0.0716(4) Uani 1 1 d . . .
Cu2 Cu 1.0000 0.5000 1.5000 0.0699(5) Uani 1 2 d S . .
N1 N 0.5575(4) 0.1822(3) 1.2127(3) 0.0650(16) Uani 1 1 d . . .
N2 N 0.4438(4) 0.2080(3) 1.1042(3) 0.0678(17) Uani 1 1 d . . .
N3 N 0.8251(4) 0.3914(3) 1.3324(3) 0.0609(15) Uani 1 1 d . . .
N4 N 0.8931(5) 0.4491(3) 1.4296(4) 0.0675(17) Uani 1 1 d . . .
N5 N 0.5108(4) 0.2277(3) 0.9820(3) 0.0689(17) Uani 1 1 d . . .
N6 N 0.6587(4) 0.2714(3) 0.9988(3) 0.0693(18) Uani 1 1 d . . .
N7 N 0.3018(4) 0.2152(3) 0.8831(3) 0.0733(18) Uani 1 1 d . . .
N8 N 0.1916(5) 0.1949(3) 0.7716(4) 0.0768(19) Uani 1 1 d . . .
N9 N 0.2339(4) 0.2244(3) 1.0051(3) 0.0613(16) Uani 1 1 d . . .
N10 N 0.0835(4) 0.2678(3) 0.9876(3) 0.0610(16) Uani 1 1 d . . .
N11 N 0.9843(5) 0.5528(2) 1.4138(4) 0.0657(16) Uani 1 1 d . . .
N12 N 1.0219(4) 0.6074(3) 1.3315(3) 0.0628(15) Uani 1 1 d . . .
C1 C 0.8239(5) 0.1774(3) 1.3599(4) 0.0530(16) Uani 1 1 d . . .
H1A H 0.8222 0.1306 1.3835 0.050 Uiso 1 1 d . . .
C2 C 0.9086(5) 0.2145(3) 1.3914(4) 0.0529(17) Uani 1 1 d . . .
C3 C 0.9062(5) 0.2697(3) 1.3636(4) 0.0595(19) Uani 1 1 d . . .
H3A H 0.9729 0.2949 1.3826 0.050 Uiso 1 1 d . . .
C4 C 0.8219(5) 0.2888(3) 1.3044(4) 0.0536(17) Uani 1 1 d . . .
C5 C 0.7378(5) 0.2513(3) 1.2714(4) 0.0537(17) Uani 1 1 d . . .
H5A H 0.6786 0.2758 1.2322 0.050 Uiso 1 1 d . . .
C6 C 0.7380(5) 0.1968(3) 1.2993(4) 0.0544(17) Uani 1 1 d . . .
C7 C 0.6492(5) 0.1546(4) 1.2672(4) 0.076(2) Uani 1 1 d . . .
H7A H 0.6722 0.1233 1.2428 0.092 Uiso 1 1 calc R . .
H7B H 0.6300 0.1384 1.3079 0.092 Uiso 1 1 calc R . .
C8 C 0.5256(5) 0.1756(3) 1.1390(4) 0.064(2) Uani 1 1 d . . .
H8A H 0.5570 0.1510 1.1144 0.077 Uiso 1 1 calc R . .
C9 C 0.4234(6) 0.2362(4) 1.1613(5) 0.083(3) Uani 1 1 d . . .
H9A H 0.3687 0.2619 1.1544 0.099 Uiso 1 1 calc R . .
C10 C 0.4925(6) 0.2218(4) 1.2282(5) 0.084(3) Uani 1 1 d . . .
H10A H 0.4960 0.2393 1.2887 0.050 Uiso 1 1 d . . .
C11 C 0.8187(6) 0.3503(3) 1.2746(4) 0.071(2) Uani 1 1 d . . .
H11A H 0.8764 0.3561 1.2566 0.085 Uiso 1 1 calc R . .
H11B H 0.7544 0.3561 1.2327 0.085 Uiso 1 1 calc R . .
C12 C 0.9107(6) 0.4185(3) 1.3761(4) 0.0654(19) Uani 1 1 d . . .
H12A H 0.9751 0.4161 1.3697 0.078 Uiso 1 1 calc R . .
C13 C 0.7884(6) 0.4418(3) 1.4184(5) 0.074(2) Uani 1 1 d . . .
H13A H 0.7524 0.4585 1.4469 0.089 Uiso 1 1 calc R . .
C14 C 0.7472(6) 0.4059(4) 1.3584(5) 0.078(2) Uani 1 1 d . . .
H14A H 0.6783 0.3936 1.3388 0.093 Uiso 1 1 calc R . .
C15 C 0.9978(5) 0.1916(4) 1.4582(4) 0.071(2) Uani 1 1 d . . .
H15A H 0.9713 0.1818 1.4981 0.085 Uiso 1 1 calc R . .
H15B H 1.0242 0.1566 1.4433 0.085 Uiso 1 1 calc R . .
C16 C 0.5752(5) 0.2676(4) 1.0207(4) 0.069(2) Uani 1 1 d . . .
H16A H 0.5645 0.2901 1.0581 0.083 Uiso 1 1 calc R . .
C17 C 0.5567(6) 0.2042(4) 0.9342(4) 0.073(2) Uani 1 1 d . . .
H17A H 0.5166 0.1651 0.8965 0.050 Uiso 1 1 d . . .
C18 C 0.6489(5) 0.2317(4) 0.9454(4) 0.077(2) Uani 1 1 d . . .
H18A H 0.7136 0.2283 0.9238 0.050 Uiso 1 1 d . . .
C19 C 0.7462(5) 0.3105(4) 1.0312(5) 0.079(2) Uani 1 1 d . . .
H19A H 0.7220 0.3443 1.0507 0.095 Uiso 1 1 calc R . .
H19C H 0.7717 0.3232 0.9918 0.095 Uiso 1 1 calc R . .
H19B H 0.668(6) 0.207(3) 0.389(5) 0.095 Uiso 1 1 d . . .
C20 C 0.8364(5) 0.2832(3) 1.0947(4) 0.0558(18) Uani 1 1 d . . .
C21 C 0.8325(5) 0.2278(3) 1.1194(4) 0.0586(18) Uani 1 1 d . . .
H21A H 0.7650 0.2052 1.0957 0.050 Uiso 1 1 d . . .
C22 C 0.9178(5) 0.2050(3) 1.1779(4) 0.0567(18) Uani 1 1 d . . .
C23 C 1.0069(5) 0.2402(3) 1.2100(4) 0.0565(17) Uani 1 1 d . . .
H23A H 1.0783 0.2210 1.2498 0.050 Uiso 1 1 d . . .
C24 C 1.0109(5) 0.2943(3) 1.1838(4) 0.0591(19) Uani 1 1 d . . .
C25 C 0.9245(5) 0.3173(3) 1.1262(4) 0.0599(18) Uani 1 1 d . . .
H25A H 0.9219 0.3670 1.1010 0.050 Uiso 1 1 d . . .
C26 C 1.1050(6) 0.3335(4) 1.2123(5) 0.083(3) Uani 1 1 d . . .
H26A H 1.1278 0.3440 1.1707 0.099 Uiso 1 1 calc R . .
H26B H 1.0859 0.3685 1.2322 0.099 Uiso 1 1 calc R . .
C27 C 0.3171(6) 0.2522(4) 0.8307(5) 0.084(3) Uani 1 1 d . . .
H27A H 0.3673 0.2811 0.8419 0.101 Uiso 1 1 calc R . .
C28 C 0.2502(6) 0.2411(5) 0.7621(5) 0.089(3) Uani 1 1 d . . .
H28A H 0.2281 0.2597 0.6988 0.050 Uiso 1 1 d . . .
C29 C 0.2246(5) 0.1798(4) 0.8446(4) 0.070(2) Uani 1 1 d . . .
H29A H 0.1981 0.1497 0.8651 0.084 Uiso 1 1 calc R . .
C30 C 0.1700(5) 0.2675(4) 0.9708(4) 0.070(2) Uani 1 1 d . . .
H30A H 0.1847 0.2940 0.9390 0.084 Uiso 1 1 calc R . .
C31 C 0.0919(5) 0.2218(4) 1.0356(4) 0.068(2) Uani 1 1 d . . .
H31A H 0.0438 0.2247 1.0554 0.050 Uiso 1 1 d . . .
C32 C 0.1825(5) 0.1964(4) 1.0469(4) 0.065(2) Uani 1 1 d . . .
H32A H 0.2233 0.1580 1.0833 0.050 Uiso 1 1 d . . .
C33 C 0.8936(7) 0.5659(4) 1.3575(5) 0.083(2) Uani 1 1 d . . .
H33A H 0.8067 0.5601 1.3457 0.050 Uiso 1 1 d . . .
C34 C 0.9158(6) 0.6007(4) 1.3060(5) 0.091(3) Uani 1 1 d . . .
H34A H 0.8611 0.6249 1.2606 0.050 Uiso 1 1 d . . .
C35 C 1.0600(5) 0.5787(3) 1.3961(4) 0.0610(18) Uani 1 1 d . . .
H35A H 1.1383 0.5759 1.4206 0.050 Uiso 1 1 d . . .
C36 C 1.0817(6) 0.6434(3) 1.2980(4) 0.069(2) Uani 1 1 d . . .
H36A H 1.0517 0.6410 1.2436 0.083 Uiso 1 1 calc R . .
H36B H 1.1528 0.6293 1.3131 0.083 Uiso 1 1 calc R . .
C37 C 0.1460(16) 0.0360(8) 0.8199(10) 0.202(8) Uani 1 1 d . . .
O1 O 0.2542(10) 0.0115(7) 0.8125(9) 0.250(7) Uani 1 1 d . . .
OW1 O 0.3681(5) 0.1103(3) 0.9900(4) 0.125(3) Uani 1 1 d . . .
OW2 O 1.1473(4) 0.0510(3) 0.9617(5) 0.115(2) Uani 1 1 d . . .
OW3 O 1.3221(7) -0.0915(5) 0.9292(7) 0.205(5) Uani 1 1 d . . .
OW4 O 0.3770(9) 0.1533(7) 0.5065(11) 0.149(7) Uani 0.50 1 d P . .
OW5 O 0.946(2) 0.0395(7) 0.7125(12) 0.194(10) Uani 0.50 1 d P . .
OW6 O 1.2636(18) 0.1289(9) 0.6145(15) 0.208(11) Uani 0.50 1 d P . .
OW7 O 0.5665(11) 0.1272(8) 0.6498(10) 0.160(7) Uani 0.50 1 d P . .
OW8 O 0.4918(19) 0.1267(8) 0.3824(13) 0.192(10) Uani 0.50 1 d P . .
OW9 O 0.633(2) -0.0650(9) 0.8734(16) 0.228(12) Uani 0.50 1 d P . .
OW10 O 0.466(2) 0.3808(10) 0.2647(11) 0.212(10) Uani 0.50 1 d P . .
OW11 O 0.144(3) 0.1038(9) 0.3800(9) 0.281(17) Uani 0.50 1 d P . .
OW12 O 0.894(5) 0.0632(11) 0.517(2) 0.48(4) Uani 0.50 1 d P . .
OW13 O 0.724(3) 0.0075(19) 0.6789(17) 0.38(3) Uani 0.50 1 d P . .
OW14 O 0.6133(19) -0.0696(17) 0.7442(16) 0.305(19) Uani 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
Cu1 0.0338(5) 0.1276(10) 0.0477(6) 0.0014(5) 0.0066(4) -0.0022(5)
Cu2 0.0919(10) 0.0585(8) 0.0566(8) -0.0043(6) 0.0218(7) -0.0198(7)
N1 0.043(3) 0.091(4) 0.053(4) -0.005(3) 0.005(3) -0.010(3)
N2 0.036(3) 0.113(5) 0.052(4) -0.005(3) 0.011(3) 0.004(3)
N3 0.056(4) 0.068(4) 0.053(4) -0.005(3) 0.013(3) -0.007(3)
N4 0.079(4) 0.058(4) 0.066(4) -0.001(3) 0.025(3) -0.011(3)
N5 0.047(3) 0.106(5) 0.051(4) -0.002(3) 0.012(3) 0.000(3)
N6 0.032(3) 0.117(5) 0.053(4) 0.004(4) 0.007(3) -0.002(3)
N7 0.045(3) 0.123(6) 0.050(4) 0.009(4) 0.013(3) -0.001(3)
N8 0.048(3) 0.121(6) 0.051(4) 0.008(4) 0.004(3) 0.012(4)
N9 0.038(3) 0.088(4) 0.049(3) 0.009(3) 0.003(3) 0.002(3)
N10 0.033(3) 0.098(5) 0.046(3) 0.001(3) 0.006(2) 0.002(3)
N11 0.067(4) 0.058(4) 0.068(4) 0.001(3) 0.018(3) -0.007(3)
N12 0.059(4) 0.078(4) 0.049(4) 0.005(3) 0.015(3) -0.007(3)
C1 0.045(4) 0.068(4) 0.043(4) -0.003(3) 0.011(3) 0.002(3)
C2 0.037(3) 0.074(5) 0.042(4) -0.003(3) 0.006(3) -0.001(3)
C3 0.047(4) 0.083(5) 0.042(4) -0.013(4) 0.008(3) -0.020(3)
C4 0.045(4) 0.068(5) 0.043(4) -0.002(3) 0.008(3) -0.006(3)
C5 0.046(4) 0.069(5) 0.039(4) -0.002(3) 0.007(3) -0.002(3)
C6 0.044(4) 0.071(5) 0.044(4) -0.009(3) 0.010(3) -0.007(3)
C7 0.055(4) 0.102(6) 0.052(5) 0.010(4) -0.008(4) -0.021(4)
C8 0.045(4) 0.094(6) 0.047(4) -0.013(4) 0.006(3) -0.008(4)
C9 0.043(4) 0.142(8) 0.062(5) -0.021(5) 0.016(4) 0.005(4)
C10 0.060(5) 0.135(8) 0.054(5) -0.024(5) 0.018(4) -0.004(5)
C11 0.081(5) 0.082(6) 0.042(4) -0.003(4) 0.011(4) -0.013(4)
C12 0.070(5) 0.063(5) 0.061(5) -0.005(4) 0.020(4) -0.006(4)
C13 0.077(5) 0.074(5) 0.077(6) -0.008(4) 0.033(5) -0.010(4)
C14 0.057(5) 0.097(6) 0.073(6) -0.002(5) 0.016(4) -0.009(4)
C15 0.045(4) 0.092(6) 0.060(5) 0.005(4) -0.002(3) -0.005(4)
C16 0.040(4) 0.108(6) 0.053(5) -0.004(4) 0.007(3) 0.005(4)
C17 0.055(4) 0.109(7) 0.052(5) -0.013(4) 0.016(4) 0.001(4)
C18 0.043(4) 0.133(8) 0.054(5) -0.009(5) 0.015(4) 0.006(4)
C19 0.048(4) 0.101(6) 0.078(6) 0.010(5) 0.008(4) -0.006(4)
C20 0.038(3) 0.085(5) 0.040(4) -0.001(4) 0.006(3) -0.003(3)
C21 0.044(4) 0.086(6) 0.044(4) -0.009(4) 0.013(3) -0.001(3)
C22 0.052(4) 0.073(5) 0.049(4) -0.003(4) 0.022(3) 0.006(3)
C23 0.044(4) 0.078(5) 0.042(4) -0.004(4) 0.008(3) 0.000(3)
C24 0.048(4) 0.085(6) 0.037(4) -0.006(4) 0.005(3) -0.012(4)
C25 0.051(4) 0.079(5) 0.047(4) -0.002(4) 0.013(3) -0.001(4)
C26 0.056(4) 0.111(7) 0.057(5) 0.013(5) -0.010(4) -0.017(4)
C27 0.047(4) 0.125(7) 0.079(6) 0.020(6) 0.020(4) -0.001(4)
C28 0.050(4) 0.156(9) 0.054(5) 0.026(5) 0.008(4) -0.002(5)
C29 0.038(4) 0.108(6) 0.050(4) 0.015(4) -0.003(3) 0.002(4)
C30 0.044(4) 0.110(6) 0.051(4) 0.010(4) 0.009(3) -0.010(4)
C31 0.042(4) 0.116(7) 0.050(4) 0.004(4) 0.019(3) -0.001(4)
C32 0.045(4) 0.094(6) 0.050(4) 0.014(4) 0.008(3) 0.004(4)
C33 0.071(5) 0.079(6) 0.096(7) 0.015(5) 0.023(5) -0.010(4)
C34 0.068(5) 0.099(7) 0.095(7) 0.036(5) 0.013(5) -0.001(5)
C35 0.059(4) 0.063(5) 0.061(5) 0.000(4) 0.021(4) -0.005(4)
C36 0.078(5) 0.079(6) 0.057(5) 0.000(4) 0.034(4) -0.010(4)
C37 0.25(2) 0.224(18) 0.162(15) 0.017(13) 0.111(15) -0.088(16)
O1 0.180(10) 0.322(17) 0.287(17) -0.076(13) 0.132(11) -0.032(10)
OW1 0.121(6) 0.109(5) 0.105(6) -0.018(4) -0.014(4) 0.010(4)
OW2 0.073(4) 0.098(5) 0.161(7) -0.010(4) 0.024(4) -0.017(3)
OW3 0.134(7) 0.209(10) 0.275(14) -0.096(10) 0.076(8) -0.006(7)
OW4 0.063(8) 0.137(13) 0.25(2) 0.022(12) 0.050(11) -0.007(7)
OW5 0.36(3) 0.091(11) 0.21(2) 0.014(11) 0.20(2) 0.028(14)
OW6 0.26(2) 0.164(16) 0.30(3) 0.100(17) 0.22(2) 0.097(16)
OW7 0.099(10) 0.186(16) 0.138(14) 0.052(12) -0.033(9) -0.052(10)
OW8 0.30(3) 0.119(13) 0.23(2) -0.049(13) 0.18(2) -0.065(15)
OW9 0.29(3) 0.152(17) 0.29(3) -0.018(17) 0.15(2) -0.125(18)
OW10 0.31(3) 0.19(2) 0.120(16) 0.002(14) 0.058(17) 0.019(19)
OW11 0.55(4) 0.201(19) 0.064(10) -0.033(12) 0.069(18) 0.20(3)
OW12 1.13(12) 0.14(2) 0.34(4) 0.00(2) 0.49(7) 0.11(4)
OW13 0.52(6) 0.48(6) 0.18(3) -0.12(3) 0.15(3) -0.28(5)
OW14 0.18(2) 0.46(5) 0.21(3) 0.07(3) -0.016(19) -0.14(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 N7 1.981(6) . ?
Cu1 N2 1.983(6) . ?
Cu1 N9 2.005(5) . ?
Cu1 N5 2.006(6) . ?
Cu1 OW1 2.357(8) . ?
Cu2 N4 1.991(6) 3_768 ?
Cu2 N4 1.991(6) . ?
Cu2 N11 1.991(6) 3_768 ?
Cu2 N11 1.991(6) . ?
N1 C8 1.319(8) . ?
N1 C10 1.378(10) . ?
N1 C7 1.468(9) . ?
N2 C8 1.319(9) . ?
N2 C9 1.370(10) . ?
N3 C12 1.335(9) . ?
N3 C14 1.359(9) . ?
N3 C11 1.430(9) . ?
N4 C12 1.325(9) . ?
N4 C13 1.382(9) . ?
N5 C16 1.313(10) . ?
N5 C17 1.378(9) . ?
N6 C18 1.339(10) . ?
N6 C16 1.344(9) . ?
N6 C19 1.459(10) . ?
N7 C29 1.337(9) . ?
N7 C27 1.380(10) . ?
N8 C29 1.345(9) . ?
N8 C28 1.385(11) . ?
N8 C26 1.476(10) 4_465 ?
N9 C30 1.339(9) . ?
N9 C32 1.385(9) . ?
N10 C30 1.325(8) . ?
N10 C31 1.381(9) . ?
N10 C15 1.455(9) 4_465 ?
N11 C35 1.334(9) . ?
N11 C33 1.362(10) . ?
N12 C35 1.330(9) . ?
N12 C34 1.370(10) . ?
N12 C36 1.457(9) . ?
C1 C2 1.401(9) . ?
C1 C6 1.403(9) . ?
C2 C3 1.381(9) . ?
C2 C15 1.518(9) . ?
C3 C4 1.376(9) . ?
C4 C5 1.405(9) . ?
C4 C11 1.529(10) . ?
C5 C6 1.370(9) . ?
C6 C7 1.515(9) . ?
C9 C10 1.336(11) . ?
C13 C14 1.364(11) . ?
C15 N10 1.455(9) 4_666 ?
C17 C18 1.362(10) . ?
C19 C20 1.531(10) . ?
C20 C21 1.375(10) . ?
C20 C25 1.392(9) . ?
C21 C22 1.405(9) . ?
C22 C23 1.417(10) . ?
C22 C36 1.501(10) 2_747 ?
C23 C24 1.356(10) . ?
C24 C25 1.407(9) . ?
C24 C26 1.515(10) . ?
C26 N8 1.476(10) 4_666 ?
C27 C28 1.332(11) . ?
C31 C32 1.321(10) . ?
C33 C34 1.377(12) . ?
C36 C22 1.501(10) 2_757 ?
C37 O1 1.64(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Cu1 N2 179.6(3) . . ?
N7 Cu1 N9 88.3(2) . . ?
N2 Cu1 N9 91.8(2) . . ?
N7 Cu1 N5 90.9(2) . . ?
N2 Cu1 N5 89.2(2) . . ?
N9 Cu1 N5 161.1(3) . . ?
N7 Cu1 OW1 90.5(3) . . ?
N2 Cu1 OW1 89.1(3) . . ?
N9 Cu1 OW1 97.5(3) . . ?
N5 Cu1 OW1 101.3(3) . . ?
N4 Cu2 N4 180.0(3) 3_768 . ?
N4 Cu2 N11 88.2(2) 3_768 3_768 ?
N4 Cu2 N11 91.8(2) . 3_768 ?
N4 Cu2 N11 91.8(2) 3_768 . ?
N4 Cu2 N11 88.2(2) . . ?
N11 Cu2 N11 180.000(3) 3_768 . ?
C8 N1 C10 107.4(6) . . ?
C8 N1 C7 125.8(7) . . ?
C10 N1 C7 126.7(7) . . ?
C8 N2 C9 104.2(6) . . ?
C8 N2 Cu1 125.1(5) . . ?
C9 N2 Cu1 130.6(5) . . ?
C12 N3 C14 106.8(6) . . ?
C12 N3 C11 126.7(6) . . ?
C14 N3 C11 126.3(6) . . ?
C12 N4 C13 105.5(6) . . ?
C12 N4 Cu2 123.0(5) . . ?
C13 N4 Cu2 131.1(6) . . ?
C16 N5 C17 106.1(6) . . ?
C16 N5 Cu1 122.9(5) . . ?
C17 N5 Cu1 131.0(5) . . ?
C18 N6 C16 108.2(6) . . ?
C18 N6 C19 126.9(7) . . ?
C16 N6 C19 124.8(7) . . ?
C29 N7 C27 106.1(7) . . ?
C29 N7 Cu1 124.0(5) . . ?
C27 N7 Cu1 129.9(6) . . ?
C29 N8 C28 109.2(7) . . ?
C29 N8 C26 124.3(8) . 4_465 ?
C28 N8 C26 126.5(7) . 4_465 ?
C30 N9 C32 104.7(6) . . ?
C30 N9 Cu1 122.6(5) . . ?
C32 N9 Cu1 132.7(5) . . ?
C30 N10 C31 105.8(6) . . ?
C30 N10 C15 125.4(7) . 4_465 ?
C31 N10 C15 128.7(6) . 4_465 ?
C35 N11 C33 106.2(6) . . ?
C35 N11 Cu2 127.4(5) . . ?
C33 N11 Cu2 126.2(5) . . ?
C35 N12 C34 107.5(6) . . ?
C35 N12 C36 125.8(6) . . ?
C34 N12 C36 126.5(7) . . ?
C2 C1 C6 119.2(6) . . ?
C3 C2 C1 120.0(6) . . ?
C3 C2 C15 123.3(6) . . ?
C1 C2 C15 116.7(6) . . ?
C4 C3 C2 120.9(6) . . ?
C3 C4 C5 119.4(6) . . ?
C3 C4 C11 120.7(6) . . ?
C5 C4 C11 119.9(6) . . ?
C6 C5 C4 120.5(6) . . ?
C5 C6 C1 120.1(6) . . ?
C5 C6 C7 123.1(6) . . ?
C1 C6 C7 116.8(6) . . ?
N1 C7 C6 111.9(6) . . ?
N1 C8 N2 112.1(7) . . ?
C10 C9 N2 111.0(7) . . ?
C9 C10 N1 105.2(7) . . ?
N3 C11 C4 110.8(6) . . ?
N4 C12 N3 112.0(7) . . ?
C14 C13 N4 108.2(7) . . ?
N3 C14 C13 107.5(7) . . ?
N10 C15 C2 113.7(6) 4_666 . ?
N5 C16 N6 110.5(7) . . ?
C18 C17 N5 108.5(7) . . ?
N6 C18 C17 106.7(6) . . ?
N6 C19 C20 113.2(7) . . ?
C21 C20 C25 120.9(6) . . ?
C21 C20 C19 122.7(6) . . ?
C25 C20 C19 116.4(7) . . ?
C20 C21 C22 120.0(6) . . ?
C21 C22 C23 118.6(7) . . ?
C21 C22 C36 120.8(7) . 2_747 ?
C23 C22 C36 120.4(6) . 2_747 ?
C24 C23 C22 120.8(6) . . ?
C23 C24 C25 120.3(6) . . ?
C23 C24 C26 124.1(6) . . ?
C25 C24 C26 115.6(7) . . ?
C20 C25 C24 119.2(7) . . ?
N8 C26 C24 111.3(7) 4_666 . ?
C28 C27 N7 110.9(8) . . ?
C27 C28 N8 104.9(7) . . ?
N7 C29 N8 108.9(7) . . ?
N10 C30 N9 112.0(7) . . ?
C32 C31 N10 108.3(6) . . ?
C31 C32 N9 109.2(7) . . ?
N11 C33 C34 108.8(7) . . ?
N12 C34 C33 106.3(7) . . ?
N12 C35 N11 111.3(6) . . ?
N12 C36 C22 111.0(6) . 2_757 ?

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 N2 C8 48(34) . . . . ?
N9 Cu1 N2 C8 146.5(6) . . . . ?
N5 Cu1 N2 C8 -52.3(6) . . . . ?
OW1 Cu1 N2 C8 49.0(6) . . . . ?
N7 Cu1 N2 C9 -132(34) . . . . ?
N9 Cu1 N2 C9 -33.7(7) . . . . ?
N5 Cu1 N2 C9 127.5(7) . . . . ?
OW1 Cu1 N2 C9 -131.2(7) . . . . ?
N4 Cu2 N4 C12 -108(100) 3_768 . . . ?
N11 Cu2 N4 C12 -109.8(6) 3_768 . . . ?
N11 Cu2 N4 C12 70.2(6) . . . . ?
N4 Cu2 N4 C13 80(100) 3_768 . . . ?
N11 Cu2 N4 C13 78.2(7) 3_768 . . . ?
N11 Cu2 N4 C13 -101.8(7) . . . . ?
N7 Cu1 N5 C16 130.4(6) . . . . ?
N2 Cu1 N5 C16 -50.0(6) . . . . ?
N9 Cu1 N5 C16 43.1(11) . . . . ?
OW1 Cu1 N5 C16 -138.9(6) . . . . ?
N7 Cu1 N5 C17 -46.5(7) . . . . ?
N2 Cu1 N5 C17 133.2(7) . . . . ?
N9 Cu1 N5 C17 -133.7(8) . . . . ?
OW1 Cu1 N5 C17 44.3(7) . . . . ?
N2 Cu1 N7 C29 40(34) . . . . ?
N9 Cu1 N7 C29 -58.4(6) . . . . ?
N5 Cu1 N7 C29 140.5(6) . . . . ?
OW1 Cu1 N7 C29 39.1(6) . . . . ?
N2 Cu1 N7 C27 -141(34) . . . . ?
N9 Cu1 N7 C27 120.5(7) . . . . ?
N5 Cu1 N7 C27 -40.6(7) . . . . ?
OW1 Cu1 N7 C27 -142.0(7) . . . . ?
N7 Cu1 N9 C30 -51.4(6) . . . . ?
N2 Cu1 N9 C30 129.0(6) . . . . ?
N5 Cu1 N9 C30 36.3(10) . . . . ?
OW1 Cu1 N9 C30 -141.7(6) . . . . ?
N7 Cu1 N9 C32 130.8(7) . . . . ?
N2 Cu1 N9 C32 -48.9(7) . . . . ?
N5 Cu1 N9 C32 -141.5(8) . . . . ?
OW1 Cu1 N9 C32 40.5(7) . . . . ?
N4 Cu2 N11 C35 43.9(6) 3_768 . . . ?
N4 Cu2 N11 C35 -136.1(6) . . . . ?
N11 Cu2 N11 C35 113(100) 3_768 . . . ?
N4 Cu2 N11 C33 -141.7(7) 3_768 . . . ?
N4 Cu2 N11 C33 38.3(7) . . . . ?
N11 Cu2 N11 C33 -73(100) 3_768 . . . ?
C6 C1 C2 C3 1.0(10) . . . . ?
C6 C1 C2 C15 178.3(6) . . . . ?
C1 C2 C3 C4 -0.8(10) . . . . ?
C15 C2 C3 C4 -177.9(7) . . . . ?
C2 C3 C4 C5 -0.8(11) . . . . ?
C2 C3 C4 C11 178.9(6) . . . . ?
C3 C4 C5 C6 2.1(10) . . . . ?
C11 C4 C5 C6 -177.5(6) . . . . ?
C4 C5 C6 C1 -1.9(10) . . . . ?
C4 C5 C6 C7 179.0(7) . . . . ?
C2 C1 C6 C5 0.3(10) . . . . ?
C2 C1 C6 C7 179.5(6) . . . . ?
C8 N1 C7 C6 106.1(8) . . . . ?
C10 N1 C7 C6 -70.0(10) . . . . ?
C5 C6 C7 N1 -9.9(10) . . . . ?
C1 C6 C7 N1 170.9(6) . . . . ?
C10 N1 C8 N2 -0.1(9) . . . . ?
C7 N1 C8 N2 -176.8(6) . . . . ?
C9 N2 C8 N1 -0.7(8) . . . . ?
Cu1 N2 C8 N1 179.2(5) . . . . ?
C8 N2 C9 C10 1.3(10) . . . . ?
Cu1 N2 C9 C10 -178.6(6) . . . . ?
N2 C9 C10 N1 -1.3(10) . . . . ?
C8 N1 C10 C9 0.9(9) . . . . ?
C7 N1 C10 C9 177.5(7) . . . . ?
C12 N3 C11 C4 97.0(8) . . . . ?
C14 N3 C11 C4 -75.8(9) . . . . ?
C3 C4 C11 N3 -60.0(9) . . . . ?
C5 C4 C11 N3 119.7(7) . . . . ?
C13 N4 C12 N3 -1.2(9) . . . . ?
Cu2 N4 C12 N3 -174.9(5) . . . . ?
C14 N3 C12 N4 0.9(9) . . . . ?
C11 N3 C12 N4 -173.0(7) . . . . ?
C12 N4 C13 C14 1.0(9) . . . . ?
Cu2 N4 C13 C14 174.0(6) . . . . ?
C12 N3 C14 C13 -0.3(9) . . . . ?
C11 N3 C14 C13 173.7(7) . . . . ?
N4 C13 C14 N3 -0.4(9) . . . . ?
C3 C2 C15 N10 -3.3(11) . . . 4_666 ?
C1 C2 C15 N10 179.4(6) . . . 4_666 ?
C17 N5 C16 N6 1.2(9) . . . . ?
Cu1 N5 C16 N6 -176.3(5) . . . . ?
C18 N6 C16 N5 -1.4(9) . . . . ?
C19 N6 C16 N5 -178.8(7) . . . . ?
C16 N5 C17 C18 -0.5(9) . . . . ?
Cu1 N5 C17 C18 176.7(6) . . . . ?
C16 N6 C18 C17 1.1(9) . . . . ?
C19 N6 C18 C17 178.3(7) . . . . ?
N5 C17 C18 N6 -0.4(10) . . . . ?
C18 N6 C19 C20 -83.4(10) . . . . ?
C16 N6 C19 C20 93.5(9) . . . . ?
N6 C19 C20 C21 -1.9(11) . . . . ?
N6 C19 C20 C25 177.4(6) . . . . ?
C25 C20 C21 C22 0.8(10) . . . . ?
C19 C20 C21 C22 180.0(7) . . . . ?
C20 C21 C22 C23 -0.3(10) . . . . ?
C20 C21 C22 C36 -175.6(6) . . . 2_747 ?
C21 C22 C23 C24 -1.4(10) . . . . ?
C36 C22 C23 C24 173.9(6) 2_747 . . . ?
C22 C23 C24 C25 2.5(11) . . . . ?
C22 C23 C24 C26 -176.8(7) . . . . ?
C21 C20 C25 C24 0.4(10) . . . . ?
C19 C20 C25 C24 -178.9(7) . . . . ?
C23 C24 C25 C20 -2.0(11) . . . . ?
C26 C24 C25 C20 177.4(7) . . . . ?
C23 C24 C26 N8 0.3(11) . . . 4_666 ?
C25 C24 C26 N8 -179.1(7) . . . 4_666 ?
C29 N7 C27 C28 1.2(10) . . . . ?
Cu1 N7 C27 C28 -177.8(6) . . . . ?
N7 C27 C28 N8 -0.7(10) . . . . ?
C29 N8 C28 C27 -0.1(10) . . . . ?
C26 N8 C28 C27 178.9(7) 4_465 . . . ?
C27 N7 C29 N8 -1.3(8) . . . . ?
Cu1 N7 C29 N8 177.8(5) . . . . ?
C28 N8 C29 N7 0.9(9) . . . . ?
C26 N8 C29 N7 -178.2(7) 4_465 . . . ?
C31 N10 C30 N9 -0.2(8) . . . . ?
C15 N10 C30 N9 -178.7(6) 4_465 . . . ?
C32 N9 C30 N10 -0.6(8) . . . . ?
Cu1 N9 C30 N10 -179.0(5) . . . . ?
C30 N10 C31 C32 1.0(8) . . . . ?
C15 N10 C31 C32 179.4(7) 4_465 . . . ?
N10 C31 C32 N9 -1.3(9) . . . . ?
C30 N9 C32 C31 1.2(9) . . . . ?
Cu1 N9 C32 C31 179.3(5) . . . . ?
C35 N11 C33 C34 -0.6(10) . . . . ?
Cu2 N11 C33 C34 -175.9(6) . . . . ?
C35 N12 C34 C33 -1.1(10) . . . . ?
C36 N12 C34 C33 -176.2(7) . . . . ?
N11 C33 C34 N12 1.0(11) . . . . ?
C34 N12 C35 N11 0.8(9) . . . . ?
C36 N12 C35 N11 176.0(6) . . . . ?
C33 N11 C35 N12 -0.1(9) . . . . ?
Cu2 N11 C35 N12 175.2(5) . . . . ?
C35 N12 C36 C22 -92.3(9) . . . 2_757 ?
C34 N12 C36 C22 82.0(9) . . . 2_757 ?

_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              24.71
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.776
_refine_diff_density_min   -0.583
_refine_diff_density_rms    0.110