# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Vadapalli Chandrasekhar'
_publ_contact_author_email       VC@IITK.AC.IN

_publ_section_title              
;
A Hexadecameric Copper(II) Phosphonate Cage
;
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Loganathan Nagarajan'

# Attachment 'VC16_Revised2.cif'

data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 720270'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'metal phosphonate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H104 Cu16 N18 O34 P6'
_chemical_formula_weight         2824.07

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'
P P 0.1023 0.0942 '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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_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                   13.714(5)
_cell_length_b                   13.929(5)
_cell_length_c                   15.394(5)
_cell_angle_alpha                76.035(5)
_cell_angle_beta                 70.235(5)
_cell_angle_gamma                85.334(5)
_cell_volume                     2685.6(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    2587
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    3.260
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;
# 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 0.500 0.000 1.000 344 84 ' '
2 0.380 0.879 0.507 20 3 ' '
3 0.620 0.121 0.493 21 3 ' '
_platon_squeeze_details          
;
;
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            14442
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.25
_reflns_number_total             9584
_reflns_number_gt                7213
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.0688P)^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_extinction_coef       ?
_refine_ls_number_reflns         9584
_refine_ls_number_parameters     632
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.18819(6) 1.08402(6) 0.37087(5) 0.0188(2) Uani 1 1 d . . .
Cu2 Cu 0.27130(7) 0.95594(6) 0.21693(6) 0.0217(2) Uani 1 1 d . . .
Cu3 Cu 0.42457(7) 0.75585(6) 0.23370(6) 0.0196(2) Uani 1 1 d . . .
Cu4 Cu 0.65128(7) 0.67744(6) 0.26102(6) 0.0213(2) Uani 1 1 d . . .
Cu5 Cu 0.76182(6) 0.71147(6) 0.39773(5) 0.0181(2) Uani 1 1 d . . .
Cu6 Cu 0.62956(6) 0.79037(6) 0.59679(5) 0.01463(19) Uani 1 1 d . . .
Cu7 Cu 0.44246(6) 0.97574(6) 0.67006(5) 0.01487(19) Uani 1 1 d . . .
Cu8 Cu 0.23564(6) 1.05265(6) 0.57771(5) 0.01470(19) Uani 1 1 d . . .
P1 P 0.74393(14) 0.88988(13) 0.24580(11) 0.0159(4) Uani 1 1 d . . .
P2 P 0.59551(14) 0.86939(13) 0.77705(12) 0.0173(4) Uani 1 1 d . . .
P3 P 0.41482(13) 0.88018(12) 0.55261(11) 0.0138(4) Uani 1 1 d . . .
O1 O 0.2980(4) 1.0772(3) 0.2519(3) 0.0196(10) Uani 1 1 d . . .
O2 O 0.0880(4) 1.1068(4) 0.3041(3) 0.0276(12) Uani 1 1 d . . .
O3 O 0.1509(4) 1.0213(4) 0.1891(3) 0.0259(12) Uani 1 1 d . . .
O4 O 0.3848(4) 0.8868(4) 0.2429(4) 0.0310(13) Uani 1 1 d D . .
O5 O 0.5296(4) 0.7540(4) 0.2878(4) 0.0267(12) Uani 1 1 d D . .
O6 O 0.6340(4) 0.9279(3) 0.2663(3) 0.0200(11) Uani 1 1 d . . .
O7 O 0.7404(4) 0.7746(3) 0.2789(3) 0.0189(10) Uani 1 1 d . . .
O8 O 0.7721(4) 0.5917(4) 0.2348(3) 0.0276(12) Uani 1 1 d . . .
O9 O 0.8528(4) 0.6141(3) 0.3358(3) 0.0264(12) Uani 1 1 d . . .
O10 O 0.6627(4) 0.7988(3) 0.4640(3) 0.0151(10) Uani 1 1 d D . .
O11 O 0.6091(4) 0.7847(3) 0.7283(3) 0.0184(10) Uani 1 1 d . . .
O12 O 0.5161(4) 0.9465(3) 0.7574(3) 0.0219(11) Uani 1 1 d . . .
O13 O 0.4983(3) 0.8655(3) 0.6035(3) 0.0169(10) Uani 1 1 d . . .
O14 O 0.5443(3) 1.0968(3) 0.5527(3) 0.0170(10) Uani 1 1 d . . .
O15 O 0.3505(4) 0.9649(3) 0.5962(3) 0.0193(10) Uani 1 1 d . . .
O16 O 0.8082(3) 0.9328(3) 0.2905(3) 0.0165(10) Uani 1 1 d . . .
O17 O 0.2786(4) 1.0511(3) 0.4448(3) 0.0178(10) Uani 1 1 d D . .
N1 N 0.1042(4) 1.1051(4) 0.5649(4) 0.0178(13) Uani 1 1 d . . .
N2 N 0.0847(4) 1.1150(4) 0.4815(4) 0.0202(13) Uani 1 1 d . . .
N3 N 0.2403(5) 0.8336(5) 0.1910(4) 0.0269(14) Uani 1 1 d . . .
N4 N 0.2905(5) 0.7460(4) 0.2178(4) 0.0265(14) Uani 1 1 d . . .
N5 N 0.4890(5) 0.6361(4) 0.1923(4) 0.0216(14) Uani 1 1 d . . .
N6 N 0.5818(5) 0.6036(4) 0.2045(4) 0.0256(14) Uani 1 1 d . . .
N7 N 0.7950(4) 0.6608(4) 0.5131(4) 0.0190(13) Uani 1 1 d . . .
N8 N 0.7379(4) 0.6899(4) 0.5948(4) 0.0171(12) Uani 1 1 d . . .
C1 C 0.0885(6) 1.0792(5) 0.2309(5) 0.0223(16) Uani 1 1 d . . .
C2 C -0.0001(6) 1.1177(6) 0.1966(5) 0.0297(18) Uani 1 1 d . . .
H2A H -0.0545 1.0693 0.2223 0.044 Uiso 1 1 calc R . .
H2B H 0.0229 1.1308 0.1286 0.044 Uiso 1 1 calc R . .
H2C H -0.0255 1.1777 0.2168 0.044 Uiso 1 1 calc R . .
C3 C 0.1535(6) 0.8085(6) 0.1817(6) 0.0345(19) Uani 1 1 d . . .
H3 H 0.1052 0.8535 0.1652 0.041 Uiso 1 1 calc R . .
C4 C 0.1440(7) 0.7068(6) 0.1998(6) 0.043(2) Uani 1 1 d . . .
H4 H 0.0916 0.6704 0.1970 0.052 Uiso 1 1 calc R . .
C5 C 0.2320(7) 0.6724(6) 0.2232(6) 0.039(2) Uani 1 1 d . . .
H5 H 0.2477 0.6058 0.2405 0.047 Uiso 1 1 calc R . .
C6 C 0.4642(7) 0.5732(6) 0.1502(6) 0.037(2) Uani 1 1 d . . .
H6 H 0.4052 0.5774 0.1326 0.045 Uiso 1 1 calc R . .
C7 C 0.5386(8) 0.5013(7) 0.1368(7) 0.054(3) Uani 1 1 d . . .
H7 H 0.5401 0.4488 0.1089 0.065 Uiso 1 1 calc R . .
C8 C 0.6094(8) 0.5229(6) 0.1727(7) 0.049(3) Uani 1 1 d . . .
H8 H 0.6686 0.4861 0.1746 0.059 Uiso 1 1 calc R . .
C9 C 0.8087(5) 0.9183(5) 0.1176(4) 0.0226(16) Uani 1 1 d . . .
C10 C 0.9220(5) 0.8860(6) 0.0967(5) 0.0298(18) Uani 1 1 d . . .
H10A H 0.9558 0.8976 0.0294 0.045 Uiso 1 1 calc R . .
H10B H 0.9252 0.8168 0.1247 0.045 Uiso 1 1 calc R . .
H10C H 0.9562 0.9233 0.1229 0.045 Uiso 1 1 calc R . .
C11 C 0.7545(6) 0.8620(6) 0.0724(5) 0.0328(19) Uani 1 1 d . . .
H11A H 0.7677 0.7924 0.0896 0.049 Uiso 1 1 calc R . .
H11B H 0.7807 0.8846 0.0047 0.049 Uiso 1 1 calc R . .
H11C H 0.6812 0.8738 0.0947 0.049 Uiso 1 1 calc R . .
C12 C 0.8020(6) 1.0309(6) 0.0802(5) 0.034(2) Uani 1 1 d . . .
H12A H 0.8314 1.0470 0.0123 0.051 Uiso 1 1 calc R . .
H12B H 0.8396 1.0646 0.1064 0.051 Uiso 1 1 calc R . .
H12C H 0.7307 1.0512 0.0986 0.051 Uiso 1 1 calc R . .
C13 C 0.8444(6) 0.5765(6) 0.2702(5) 0.0274(17) Uani 1 1 d . . .
C14 C 0.9252(6) 0.5024(6) 0.2364(6) 0.041(2) Uani 1 1 d . . .
H14A H 0.9899 0.5356 0.2000 0.062 Uiso 1 1 calc R . .
H14B H 0.9041 0.4696 0.1975 0.062 Uiso 1 1 calc R . .
H14C H 0.9333 0.4545 0.2900 0.062 Uiso 1 1 calc R . .
C15 C 0.8647(6) 0.5948(5) 0.5322(5) 0.0234(16) Uani 1 1 d . . .
H15 H 0.9128 0.5636 0.4888 0.028 Uiso 1 1 calc R . .
C16 C 0.8547(6) 0.5796(6) 0.6275(5) 0.0295(18) Uani 1 1 d . . .
H16 H 0.8936 0.5376 0.6599 0.035 Uiso 1 1 calc R . .
C17 C 0.7742(6) 0.6405(5) 0.6636(5) 0.0254(17) Uani 1 1 d . . .
H17 H 0.7490 0.6464 0.7262 0.030 Uiso 1 1 calc R . .
C18 C 0.5551(6) 0.8174(5) 0.9032(5) 0.0220(16) Uani 1 1 d . . .
C19 C 0.4496(6) 0.7681(6) 0.9333(5) 0.0342(19) Uani 1 1 d . . .
H19A H 0.4002 0.8164 0.9184 0.051 Uiso 1 1 calc R . .
H19B H 0.4269 0.7401 1.0003 0.051 Uiso 1 1 calc R . .
H19C H 0.4553 0.7166 0.9001 0.051 Uiso 1 1 calc R . .
C20 C 0.5442(6) 0.9005(5) 0.9568(5) 0.0282(18) Uani 1 1 d . . .
H20A H 0.5145 0.8738 1.0237 0.042 Uiso 1 1 calc R . .
H20B H 0.5000 0.9516 0.9366 0.042 Uiso 1 1 calc R . .
H20C H 0.6112 0.9276 0.9433 0.042 Uiso 1 1 calc R . .
C21 C 0.6358(6) 0.7400(6) 0.9262(5) 0.034(2) Uani 1 1 d . . .
H21A H 0.6212 0.7210 0.9935 0.051 Uiso 1 1 calc R . .
H21B H 0.7040 0.7681 0.8963 0.051 Uiso 1 1 calc R . .
H21C H 0.6321 0.6828 0.9029 0.051 Uiso 1 1 calc R . .
C22 C 0.3349(5) 0.7697(5) 0.5996(5) 0.0198(15) Uani 1 1 d . . .
C23 C 0.4017(6) 0.6821(5) 0.5727(6) 0.0340(19) Uani 1 1 d . . .
H23A H 0.3596 0.6236 0.5953 0.051 Uiso 1 1 calc R . .
H23B H 0.4554 0.6728 0.6009 0.051 Uiso 1 1 calc R . .
H23C H 0.4323 0.6943 0.5050 0.051 Uiso 1 1 calc R . .
C24 C 0.2467(6) 0.7845(6) 0.5560(6) 0.038(2) Uani 1 1 d . . .
H24A H 0.2062 0.7251 0.5773 0.056 Uiso 1 1 calc R . .
H24B H 0.2761 0.7993 0.4881 0.056 Uiso 1 1 calc R . .
H24C H 0.2033 0.8383 0.5755 0.056 Uiso 1 1 calc R . .
C25 C 0.2887(6) 0.7520(5) 0.7065(5) 0.0315(19) Uani 1 1 d . . .
H25A H 0.3433 0.7473 0.7332 0.047 Uiso 1 1 calc R . .
H25B H 0.2499 0.6914 0.7309 0.047 Uiso 1 1 calc R . .
H25C H 0.2437 0.8059 0.7231 0.047 Uiso 1 1 calc R . .
C26 C 0.0229(5) 1.1382(5) 0.6244(5) 0.0232(16) Uani 1 1 d . . .
H26 H 0.0172 1.1399 0.6859 0.028 Uiso 1 1 calc R . .
C27 C -0.0533(6) 1.1704(6) 0.5835(5) 0.0323(19) Uani 1 1 d . . .
H27 H -0.1179 1.1973 0.6098 0.039 Uiso 1 1 calc R . .
C28 C -0.0095(6) 1.1527(6) 0.4939(5) 0.0297(19) Uani 1 1 d . . .
H28 H -0.0420 1.1656 0.4482 0.036 Uiso 1 1 calc R . .
H102 H 0.620(4) 0.817(4) 0.440(4) 0.006(17) Uiso 1 1 d D . .
H103 H 0.547(6) 0.808(3) 0.285(6) 0.04(3) Uiso 1 1 d D . .
H105 H 0.421(5) 0.926(5) 0.247(6) 0.04(3) Uiso 1 1 d D . .
H101 H 0.321(4) 1.010(4) 0.431(5) 0.01(2) Uiso 1 1 d D . .
N1S N 0.6124(5) 0.5817(4) 0.4295(4) 0.0243(14) Uani 1 1 d . . .
C51 C 0.6143(6) 0.5343(5) 0.4995(5) 0.0239(16) Uani 1 1 d . . .
C52 C 0.6167(6) 0.4742(6) 0.5907(5) 0.0322(19) Uani 1 1 d . . .
H52A H 0.5785 0.4142 0.6059 0.048 Uiso 1 1 calc R . .
H52B H 0.5860 0.5105 0.6390 0.048 Uiso 1 1 calc R . .
H52C H 0.6872 0.4585 0.5871 0.048 Uiso 1 1 calc 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 0.0226(5) 0.0253(5) 0.0133(4) -0.0068(4) -0.0103(4) -0.0003(4)
Cu2 0.0320(5) 0.0217(5) 0.0162(4) -0.0054(4) -0.0128(4) -0.0026(4)
Cu3 0.0266(5) 0.0181(5) 0.0163(4) -0.0039(3) -0.0084(4) -0.0055(4)
Cu4 0.0243(5) 0.0247(5) 0.0182(5) -0.0095(4) -0.0074(4) -0.0024(4)
Cu5 0.0222(5) 0.0209(5) 0.0128(4) -0.0061(3) -0.0065(4) -0.0001(4)
Cu6 0.0202(5) 0.0166(4) 0.0092(4) -0.0032(3) -0.0071(3) -0.0011(3)
Cu7 0.0186(4) 0.0182(4) 0.0109(4) -0.0050(3) -0.0073(3) -0.0012(3)
Cu8 0.0159(4) 0.0206(4) 0.0093(4) -0.0027(3) -0.0062(3) -0.0025(3)
P1 0.0176(9) 0.0228(10) 0.0084(8) -0.0040(7) -0.0047(7) -0.0017(8)
P2 0.0241(10) 0.0221(10) 0.0095(8) -0.0055(7) -0.0092(8) 0.0000(8)
P3 0.0175(9) 0.0168(9) 0.0098(8) -0.0047(7) -0.0058(7) -0.0032(7)
O1 0.025(3) 0.020(3) 0.016(2) -0.006(2) -0.007(2) -0.002(2)
O2 0.025(3) 0.047(3) 0.019(3) -0.014(2) -0.014(2) 0.003(2)
O3 0.032(3) 0.033(3) 0.021(3) -0.012(2) -0.015(2) -0.002(2)
O4 0.048(4) 0.019(3) 0.044(3) -0.016(2) -0.033(3) 0.000(3)
O5 0.022(3) 0.029(3) 0.037(3) -0.015(3) -0.014(2) 0.001(2)
O6 0.022(3) 0.025(3) 0.022(3) -0.015(2) -0.012(2) 0.000(2)
O7 0.025(3) 0.024(3) 0.013(2) -0.009(2) -0.010(2) 0.001(2)
O8 0.030(3) 0.035(3) 0.023(3) -0.016(2) -0.009(2) -0.001(2)
O9 0.026(3) 0.028(3) 0.030(3) -0.017(2) -0.010(2) 0.009(2)
O10 0.020(3) 0.018(3) 0.010(2) -0.0060(19) -0.008(2) 0.003(2)
O11 0.029(3) 0.019(3) 0.012(2) -0.0023(19) -0.013(2) -0.004(2)
O12 0.032(3) 0.024(3) 0.019(3) -0.012(2) -0.016(2) 0.005(2)
O13 0.016(2) 0.026(3) 0.010(2) -0.0029(19) -0.006(2) -0.004(2)
O14 0.020(3) 0.022(3) 0.009(2) -0.0026(19) -0.005(2) -0.005(2)
O15 0.028(3) 0.017(2) 0.015(2) -0.002(2) -0.010(2) 0.000(2)
O16 0.014(2) 0.028(3) 0.009(2) -0.002(2) -0.0054(19) -0.008(2)
O17 0.024(3) 0.021(3) 0.009(2) -0.005(2) -0.007(2) 0.002(2)
N1 0.017(3) 0.032(3) 0.010(3) -0.006(2) -0.009(2) -0.003(3)
N2 0.017(3) 0.032(4) 0.013(3) -0.006(3) -0.007(3) -0.001(3)
N3 0.027(4) 0.037(4) 0.015(3) -0.008(3) -0.001(3) -0.010(3)
N4 0.035(4) 0.018(3) 0.032(4) -0.005(3) -0.018(3) -0.001(3)
N5 0.037(4) 0.013(3) 0.017(3) -0.002(2) -0.012(3) 0.000(3)
N6 0.031(4) 0.019(3) 0.031(4) -0.011(3) -0.011(3) 0.002(3)
N7 0.020(3) 0.023(3) 0.016(3) -0.007(2) -0.006(3) -0.001(3)
N8 0.018(3) 0.023(3) 0.015(3) -0.008(2) -0.007(2) -0.001(2)
C1 0.030(4) 0.020(4) 0.015(4) 0.000(3) -0.005(3) -0.014(3)
C2 0.032(5) 0.041(5) 0.025(4) -0.012(4) -0.018(4) -0.002(4)
C3 0.033(5) 0.033(5) 0.043(5) -0.008(4) -0.019(4) -0.004(4)
C4 0.036(5) 0.038(5) 0.067(6) -0.014(5) -0.028(5) -0.006(4)
C5 0.058(6) 0.023(4) 0.044(5) -0.002(4) -0.030(5) -0.005(4)
C6 0.056(6) 0.030(5) 0.043(5) -0.016(4) -0.033(5) -0.001(4)
C7 0.073(7) 0.046(6) 0.073(7) -0.040(5) -0.044(6) 0.011(5)
C8 0.059(6) 0.036(5) 0.073(7) -0.021(5) -0.045(6) 0.016(5)
C9 0.024(4) 0.035(4) 0.009(3) -0.005(3) -0.005(3) -0.008(3)
C10 0.024(4) 0.055(5) 0.009(4) -0.011(3) 0.001(3) -0.009(4)
C11 0.034(5) 0.056(6) 0.012(4) -0.012(4) -0.007(3) -0.014(4)
C12 0.043(5) 0.040(5) 0.023(4) 0.003(4) -0.018(4) -0.009(4)
C13 0.024(4) 0.033(5) 0.028(4) -0.017(4) -0.005(4) -0.001(3)
C14 0.040(5) 0.049(6) 0.043(5) -0.023(4) -0.014(4) -0.001(4)
C15 0.023(4) 0.026(4) 0.020(4) -0.004(3) -0.008(3) 0.004(3)
C16 0.026(4) 0.036(5) 0.027(4) -0.002(3) -0.015(4) 0.008(4)
C17 0.030(4) 0.033(4) 0.013(4) -0.001(3) -0.011(3) 0.000(4)
C18 0.033(4) 0.020(4) 0.017(4) -0.007(3) -0.010(3) 0.000(3)
C19 0.045(5) 0.037(5) 0.022(4) -0.005(4) -0.012(4) -0.009(4)
C20 0.039(5) 0.036(5) 0.015(4) -0.007(3) -0.013(4) -0.005(4)
C21 0.043(5) 0.039(5) 0.021(4) 0.001(4) -0.016(4) -0.001(4)
C22 0.023(4) 0.020(4) 0.017(4) -0.005(3) -0.005(3) -0.004(3)
C23 0.041(5) 0.026(4) 0.034(5) -0.002(4) -0.015(4) -0.003(4)
C24 0.036(5) 0.030(5) 0.055(6) -0.005(4) -0.025(4) -0.015(4)
C25 0.033(5) 0.025(4) 0.026(4) 0.001(3) 0.001(4) -0.008(4)
C26 0.019(4) 0.031(4) 0.019(4) -0.003(3) -0.006(3) -0.001(3)
C27 0.026(4) 0.053(5) 0.019(4) -0.010(4) -0.009(3) 0.003(4)
C28 0.027(4) 0.049(5) 0.021(4) -0.007(4) -0.020(4) 0.007(4)
N1S 0.029(4) 0.025(3) 0.015(3) 0.001(3) -0.003(3) -0.009(3)
C51 0.029(4) 0.018(4) 0.018(4) 0.002(3) -0.002(3) -0.011(3)
C52 0.035(5) 0.036(5) 0.029(4) -0.006(4) -0.012(4) -0.013(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 O17 1.911(4) . ?
Cu1 N2 1.929(5) . ?
Cu1 O2 1.943(4) . ?
Cu1 O1 1.956(4) . ?
Cu2 O4 1.871(5) . ?
Cu2 O3 1.945(5) . ?
Cu2 N3 1.951(6) . ?
Cu2 O1 1.987(4) . ?
Cu3 O4 1.886(5) . ?
Cu3 O5 1.887(5) . ?
Cu3 N4 1.955(6) . ?
Cu3 N5 1.966(5) . ?
Cu4 O5 1.884(5) . ?
Cu4 O8 1.948(5) . ?
Cu4 N6 1.969(6) . ?
Cu4 O7 2.019(5) . ?
Cu5 N7 1.935(5) . ?
Cu5 O7 1.936(4) . ?
Cu5 O10 1.939(4) . ?
Cu5 O9 1.962(4) . ?
Cu6 O10 1.914(4) . ?
Cu6 O11 1.930(4) . ?
Cu6 N8 1.954(5) . ?
Cu6 O13 1.992(4) . ?
Cu7 O6 1.891(4) 2_676 ?
Cu7 O12 1.892(4) . ?
Cu7 O15 1.998(4) . ?
Cu7 O13 2.008(4) . ?
Cu7 O14 2.294(5) . ?
Cu7 P3 2.6252(18) . ?
Cu8 O17 1.934(4) . ?
Cu8 N1 1.944(5) . ?
Cu8 O16 1.968(4) 2_676 ?
Cu8 O15 1.969(4) . ?
Cu8 O10 2.420(5) 2_676 ?
P1 O6 1.510(5) . ?
P1 O16 1.517(4) . ?
P1 O7 1.563(5) . ?
P1 C9 1.826(7) . ?
P2 O11 1.512(4) . ?
P2 O12 1.519(5) . ?
P2 O1 1.569(5) 2_676 ?
P2 C18 1.806(7) . ?
P3 O14 1.486(4) 2_676 ?
P3 O15 1.560(5) . ?
P3 O13 1.567(4) . ?
P3 C22 1.814(7) . ?
O1 P2 1.569(5) 2_676 ?
O2 C1 1.273(8) . ?
O3 C1 1.250(8) . ?
O6 Cu7 1.891(4) 2_676 ?
O8 C13 1.266(8) . ?
O9 C13 1.284(8) . ?
O10 Cu8 2.420(5) 2_676 ?
O14 P3 1.486(4) 2_676 ?
O16 Cu8 1.968(4) 2_676 ?
N1 C26 1.313(8) . ?
N1 N2 1.370(7) . ?
N2 C28 1.325(9) . ?
N3 C3 1.330(9) . ?
N3 N4 1.395(8) . ?
N4 C5 1.322(10) . ?
N5 C6 1.332(8) . ?
N5 N6 1.374(8) . ?
N6 C8 1.310(9) . ?
N7 C15 1.329(8) . ?
N7 N8 1.374(7) . ?
N8 C17 1.338(8) . ?
C1 C2 1.494(9) . ?
C3 C4 1.384(11) . ?
C4 C5 1.389(11) . ?
C6 C7 1.370(11) . ?
C7 C8 1.351(11) . ?
C9 C10 1.529(10) . ?
C9 C11 1.536(9) . ?
C9 C12 1.542(10) . ?
C13 C14 1.499(10) . ?
C15 C16 1.390(9) . ?
C16 C17 1.381(10) . ?
C18 C19 1.529(10) . ?
C18 C20 1.546(9) . ?
C18 C21 1.548(10) . ?
C22 C25 1.515(9) . ?
C22 C23 1.519(9) . ?
C22 C24 1.549(10) . ?
C26 C27 1.387(9) . ?
C27 C28 1.378(10) . ?
N1S C51 1.127(8) . ?
C51 C52 1.460(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
O17 Cu1 N2 87.3(2) . . ?
O17 Cu1 O2 174.5(2) . . ?
N2 Cu1 O2 90.4(2) . . ?
O17 Cu1 O1 93.83(19) . . ?
N2 Cu1 O1 170.1(2) . . ?
O2 Cu1 O1 89.34(19) . . ?
O4 Cu2 O3 177.0(2) . . ?
O4 Cu2 N3 85.3(2) . . ?
O3 Cu2 N3 91.7(2) . . ?
O4 Cu2 O1 94.4(2) . . ?
O3 Cu2 O1 88.62(19) . . ?
N3 Cu2 O1 176.4(2) . . ?
O4 Cu3 O5 93.5(2) . . ?
O4 Cu3 N4 85.4(2) . . ?
O5 Cu3 N4 162.7(2) . . ?
O4 Cu3 N5 165.5(2) . . ?
O5 Cu3 N5 87.0(2) . . ?
N4 Cu3 N5 98.3(2) . . ?
O5 Cu4 O8 176.7(2) . . ?
O5 Cu4 N6 86.5(2) . . ?
O8 Cu4 N6 90.8(2) . . ?
O5 Cu4 O7 95.1(2) . . ?
O8 Cu4 O7 87.98(19) . . ?
N6 Cu4 O7 163.2(2) . . ?
N7 Cu5 O7 173.2(2) . . ?
N7 Cu5 O10 87.7(2) . . ?
O7 Cu5 O10 91.61(18) . . ?
N7 Cu5 O9 91.6(2) . . ?
O7 Cu5 O9 89.63(19) . . ?
O10 Cu5 O9 175.0(2) . . ?
O10 Cu6 O11 174.8(2) . . ?
O10 Cu6 N8 87.0(2) . . ?
O11 Cu6 N8 90.1(2) . . ?
O10 Cu6 O13 92.06(18) . . ?
O11 Cu6 O13 91.71(18) . . ?
N8 Cu6 O13 166.4(2) . . ?
O6 Cu7 O12 89.11(19) 2_676 . ?
O6 Cu7 O15 98.19(18) 2_676 . ?
O12 Cu7 O15 162.8(2) . . ?
O6 Cu7 O13 169.50(19) 2_676 . ?
O12 Cu7 O13 98.05(18) . . ?
O15 Cu7 O13 72.87(17) . . ?
O6 Cu7 O14 90.60(18) 2_676 . ?
O12 Cu7 O14 101.58(19) . . ?
O15 Cu7 O14 93.92(17) . . ?
O13 Cu7 O14 95.43(17) . . ?
O6 Cu7 P3 134.44(14) 2_676 . ?
O12 Cu7 P3 133.40(14) . . ?
O15 Cu7 P3 36.34(13) . . ?
O13 Cu7 P3 36.56(12) . . ?
O14 Cu7 P3 94.64(11) . . ?
O17 Cu8 N1 86.8(2) . . ?
O17 Cu8 O16 174.89(19) . 2_676 ?
N1 Cu8 O16 91.24(19) . 2_676 ?
O17 Cu8 O15 91.80(19) . . ?
N1 Cu8 O15 164.3(2) . . ?
O16 Cu8 O15 91.38(18) 2_676 . ?
O17 Cu8 O10 89.06(17) . 2_676 ?
N1 Cu8 O10 102.4(2) . 2_676 ?
O16 Cu8 O10 86.77(16) 2_676 2_676 ?
O15 Cu8 O10 93.21(17) . 2_676 ?
O6 P1 O16 114.6(2) . . ?
O6 P1 O7 108.4(3) . . ?
O16 P1 O7 110.3(2) . . ?
O6 P1 C9 108.7(3) . . ?
O16 P1 C9 108.2(3) . . ?
O7 P1 C9 106.4(3) . . ?
O11 P2 O12 115.1(2) . . ?
O11 P2 O1 109.9(3) . 2_676 ?
O12 P2 O1 108.3(3) . 2_676 ?
O11 P2 C18 107.5(3) . . ?
O12 P2 C18 108.0(3) . . ?
O1 P2 C18 107.7(3) 2_676 . ?
O14 P3 O15 114.8(3) 2_676 . ?
O14 P3 O13 115.7(3) 2_676 . ?
O15 P3 O13 99.1(2) . . ?
O14 P3 C22 111.4(3) 2_676 . ?
O15 P3 C22 107.8(3) . . ?
O13 P3 C22 107.1(3) . . ?
O14 P3 Cu7 129.2(2) 2_676 . ?
O15 P3 Cu7 49.39(16) . . ?
O13 P3 Cu7 49.75(16) . . ?
C22 P3 Cu7 119.4(2) . . ?
P2 O1 Cu1 120.9(2) 2_676 . ?
P2 O1 Cu2 127.6(3) 2_676 . ?
Cu1 O1 Cu2 106.5(2) . . ?
C1 O2 Cu1 130.4(5) . . ?
C1 O3 Cu2 128.8(4) . . ?
Cu2 O4 Cu3 127.1(3) . . ?
Cu4 O5 Cu3 124.5(3) . . ?
P1 O6 Cu7 134.6(3) . 2_676 ?
P1 O7 Cu5 119.7(2) . . ?
P1 O7 Cu4 129.1(3) . . ?
Cu5 O7 Cu4 103.9(2) . . ?
C13 O8 Cu4 130.0(4) . . ?
C13 O9 Cu5 127.9(5) . . ?
Cu6 O10 Cu5 122.7(2) . . ?
Cu6 O10 Cu8 92.22(17) . 2_676 ?
Cu5 O10 Cu8 102.0(2) . 2_676 ?
P2 O11 Cu6 128.5(3) . . ?
P2 O12 Cu7 135.2(3) . . ?
P3 O13 Cu6 137.8(3) . . ?
P3 O13 Cu7 93.7(2) . . ?
Cu6 O13 Cu7 127.7(2) . . ?
P3 O14 Cu7 136.1(3) 2_676 . ?
P3 O15 Cu8 137.0(3) . . ?
P3 O15 Cu7 94.3(2) . . ?
Cu8 O15 Cu7 128.0(2) . . ?
P1 O16 Cu8 126.2(3) . 2_676 ?
Cu1 O17 Cu8 123.2(3) . . ?
C26 N1 N2 107.7(5) . . ?
C26 N1 Cu8 131.4(4) . . ?
N2 N1 Cu8 120.8(4) . . ?
C28 N2 N1 107.1(5) . . ?
C28 N2 Cu1 131.1(5) . . ?
N1 N2 Cu1 121.7(4) . . ?
C3 N3 N4 107.1(6) . . ?
C3 N3 Cu2 128.4(5) . . ?
N4 N3 Cu2 120.1(4) . . ?
C5 N4 N3 106.9(6) . . ?
C5 N4 Cu3 135.1(5) . . ?
N3 N4 Cu3 118.0(4) . . ?
C6 N5 N6 106.1(6) . . ?
C6 N5 Cu3 134.5(5) . . ?
N6 N5 Cu3 119.5(4) . . ?
C8 N6 N5 108.9(6) . . ?
C8 N6 Cu4 130.7(6) . . ?
N5 N6 Cu4 120.4(4) . . ?
C15 N7 N8 108.6(5) . . ?
C15 N7 Cu5 131.2(5) . . ?
N8 N7 Cu5 120.1(4) . . ?
C17 N8 N7 107.4(5) . . ?
C17 N8 Cu6 130.7(5) . . ?
N7 N8 Cu6 121.9(4) . . ?
O3 C1 O2 127.3(7) . . ?
O3 C1 C2 118.3(6) . . ?
O2 C1 C2 114.3(6) . . ?
N3 C3 C4 111.4(7) . . ?
C3 C4 C5 102.9(7) . . ?
N4 C5 C4 111.7(7) . . ?
N5 C6 C7 109.8(7) . . ?
C8 C7 C6 105.6(7) . . ?
N6 C8 C7 109.6(8) . . ?
C10 C9 C11 109.8(6) . . ?
C10 C9 C12 110.2(6) . . ?
C11 C9 C12 110.7(6) . . ?
C10 C9 P1 108.9(5) . . ?
C11 C9 P1 109.0(5) . . ?
C12 C9 P1 108.1(5) . . ?
O8 C13 O9 126.7(7) . . ?
O8 C13 C14 116.6(6) . . ?
O9 C13 C14 116.5(7) . . ?
N7 C15 C16 109.3(6) . . ?
C17 C16 C15 104.9(6) . . ?
N8 C17 C16 109.8(6) . . ?
C19 C18 C20 108.7(6) . . ?
C19 C18 C21 110.0(6) . . ?
C20 C18 C21 110.3(6) . . ?
C19 C18 P2 108.5(5) . . ?
C20 C18 P2 109.9(5) . . ?
C21 C18 P2 109.4(5) . . ?
C25 C22 C23 109.7(6) . . ?
C25 C22 C24 109.5(6) . . ?
C23 C22 C24 110.1(6) . . ?
C25 C22 P3 110.2(5) . . ?
C23 C22 P3 108.8(5) . . ?
C24 C22 P3 108.5(5) . . ?
N1 C26 C27 111.2(6) . . ?
C28 C27 C26 102.7(7) . . ?
N2 C28 C27 111.3(6) . . ?
N1S C51 C52 179.2(8) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.156